#------------------------------------------------------------------------------ #$Date: 2019-12-06 12:26:14 +0200 (Fri, 06 Dec 2019) $ #$Revision: 244939 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/64/1556442.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1556442 loop_ _publ_author_name 'Muller, I.' 'Schneider, C.' 'Pietzonka, C.' 'Kraus, F.' 'Werncke, C.G.' _publ_section_title ; Reduction of 2,2'-Bipyridine by Quasi-Linear 3d-Metal(I) Silylamides-A Structural and Spectroscopic Study ; _journal_name_full Inorganics _journal_page_first 117 _journal_paper_doi 10.3390/inorganics7100117 _journal_volume 7 _journal_year 2019 _chemical_formula_moiety 'C22 H44 N4 Si4 Zn, C16 H34 K O7' _chemical_formula_sum 'C38 H78 K N4 O7 Si4 Zn' _chemical_formula_weight 919.87 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _cell_angle_alpha 90 _cell_angle_beta 95.423(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.1899(7) _cell_length_b 18.4365(10) _cell_length_c 22.8273(13) _cell_measurement_reflns_used 9929 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 26.43 _cell_measurement_theta_min 2.26 _cell_volume 5107.2(5) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_temperature 100.0 _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker Quest D8' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0946 _diffrn_reflns_av_unetI/netI 0.0427 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 96672 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 2.134 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.700 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6647 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1330 before and 0.0638 after correction. The Ratio of minimum to maximum transmission is 0.8917. The \l/2 correction factor is Not present.' _exptl_crystal_colour 'clear dark pink' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary pink _exptl_crystal_density_diffrn 1.196 _exptl_crystal_description block _exptl_crystal_F_000 1980 _exptl_crystal_size_max 0.492 _exptl_crystal_size_mid 0.383 _exptl_crystal_size_min 0.15 _refine_diff_density_max 1.777 _refine_diff_density_min -1.895 _refine_diff_density_rms 0.151 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 693 _refine_ls_number_reflns 8987 _refine_ls_number_restraints 1954 _refine_ls_restrained_S_all 1.015 _refine_ls_R_factor_all 0.1506 _refine_ls_R_factor_gt 0.1281 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0002P)^2^+100.8345P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2499 _refine_ls_wR_factor_ref 0.2596 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 7347 _reflns_number_total 8987 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file K_18c6_Zn10.cif _cod_data_source_block k(18c6)zn10 _cod_database_code 1556442 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.902 _shelx_estimated_absorpt_t_min 0.724 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances Si6-C28 1.8 with sigma of 0.02 O14-C59 \\sim O14-C60 \\sim O12-C41 \\sim O12-C45 \\sim O10-C46 \\sim O10-C47 \\sim O8-C48 \\sim O8-C49 ~ O6-C50 \\sim O6-C67 \\sim O3-C65 \\sim O3-C62 with sigma of 0.02 C59-C41 \\sim C45-C46 \\sim C47-C48 \\sim C49-C50 \\sim C67-C65 \\sim C62-C60 with sigma of 0.02 C41-C45 \\sim C46-C47 \\sim C48-C49 \\sim C50-C67 \\sim C65-C62 \\sim C60-C59 with sigma of 0.04 O14-C41 \\sim O12-C46 \\sim O10-C48 \\sim O8-C50 \\sim O6-C65 \\sim O3-C60 \\sim O12-C59 \\sim O10-C45 ~ O8-C47 \\sim O6-C49 \\sim O3-C67 \\sim O14-C62 with sigma of 0.04 O4-C63 \\sim O4-C39 \\sim O5-C64 \\sim O5-C68 \\sim O7-C69 \\sim O7-C51 \\sim O9-C52 \\sim O9-C53 \\sim O11- C55 \\sim O11-C56 \\sim O13-C57 \\sim O13-C40 with sigma of 0.02 C63-C64 \\sim C68-C69 \\sim C51-C52 \\sim C53-C55 \\sim C56-C57 \\sim C40-C39 with sigma of 0.02 C64-C68 \\sim C69-C51 \\sim C52-C53 \\sim C55-C56 \\sim C57-C40 \\sim C39-C63 with sigma of 0.04 O4-C64 \\sim O5-C69 \\sim O7-C52 \\sim O9-C55 \\sim O11-C57 \\sim O13-C39 \\sim O5-C63 \\sim O7-C68 \\sim O9- C51 \\sim O11-C53 \\sim O13-C56 \\sim O4-C40 with sigma of 0.04 Si1-C20 \\sim Si1-C19 with sigma of 0.02 C37-C38 \\sim C35-C36 with sigma of 0.02 O2-C38 \\sim O2-C35 with sigma of 0.02 C37-O2 \\sim O2-C36 with sigma of 0.04 C34-C33 \\sim C32-C31 with sigma of 0.02 O1-C33 \\sim O1-C32 with sigma of 0.02 C34-O1 \\sim O1-C31 with sigma of 0.04 Si3-N4 \\sim Si3A-N4 with sigma of 0.02 Si3-C23 \\sim Si3A-C23A with sigma of 0.02 Si3-C24 \\sim Si3A-C24A with sigma of 0.02 Si3-C25 \\sim Si3A-C25A with sigma of 0.02 N4-C23 \\sim N4-C23A with sigma of 0.04 N4-C24 \\sim N4-C24A with sigma of 0.04 N4-C25 \\sim N4-C25A with sigma of 0.04 C23-C24 \\sim C23A-C24A with sigma of 0.04 C23-C25 \\sim C23A-C25A with sigma of 0.04 C24-C25 \\sim C24A-C25A with sigma of 0.04 N4-Si6 \\sim N4-Si6A with sigma of 0.02 C28-Si6 \\sim C28A-Si6A with sigma of 0.02 Si6-C27 \\sim Si6A-C27A with sigma of 0.02 Si6-C30 \\sim Si6A-C30A with sigma of 0.02 N4-C28 \\sim N4-C28A with sigma of 0.04 N4-C27 \\sim N4-C27A with sigma of 0.04 N4-C30 \\sim N4-C30A with sigma of 0.04 C28-C27 \\sim C28A-C27A with sigma of 0.04 C28-C30 \\sim C28A-C30A with sigma of 0.04 C27-C30 \\sim C27A-C30A with sigma of 0.04 Zn1-N1 \\sim Zn1-N1A with sigma of 0.02 Zn1-N2 \\sim Zn1-N2A with sigma of 0.02 N1-C1 \\sim N1A-C1A with sigma of 0.02 N1-C5 \\sim N1A-C5A with sigma of 0.02 N2-C6 \\sim N2A-C6A with sigma of 0.02 N2-C10 \\sim N2A-C10A with sigma of 0.02 C1-C2 \\sim C1A-C2A with sigma of 0.02 C2-C3 \\sim C2A-C3A with sigma of 0.02 C3-C4 \\sim C3A-C4A with sigma of 0.02 C4-C5 \\sim C4A-C5A with sigma of 0.02 C5-C6 \\sim C5A-C6A with sigma of 0.02 C6-C7 \\sim C6A-C7A with sigma of 0.02 C7-C8 \\sim C7A-C8A with sigma of 0.02 C8-C9 \\sim C8A-C9A with sigma of 0.02 C9-C10 \\sim C9A-C10A with sigma of 0.02 Zn1-C1 \\sim Zn1-C1A with sigma of 0.04 Zn1-C5 \\sim Zn1-C5A with sigma of 0.04 Zn1-C6 \\sim Zn1-C6A with sigma of 0.04 Zn1-C10 \\sim Zn1-C10A with sigma of 0.04 N1-C2 \\sim N1A-C2A with sigma of 0.04 N1-C4 \\sim N1A-C4A with sigma of 0.04 N1-C6 \\sim N1A-C6A with sigma of 0.04 N2-C5 \\sim N2A-C5A with sigma of 0.04 N2-C7 \\sim N2A-C7A with sigma of 0.04 N2-C9 \\sim N2A-C9A with sigma of 0.04 C1-C3 \\sim C1A-C3A with sigma of 0.04 C1-C5 \\sim C1A-C5A with sigma of 0.04 C2-C4 \\sim C2A-C4A with sigma of 0.04 C3-C5 \\sim C3A-C5A with sigma of 0.04 C4-C6 \\sim C4A-C6A with sigma of 0.04 C5-C7 \\sim C5A-C7A with sigma of 0.04 C6-C8 \\sim C6A-C8A with sigma of 0.04 C6-C10 \\sim C6A-C10A with sigma of 0.04 C7-C9 \\sim C7A-C9A with sigma of 0.04 C8-C10 \\sim C8A-C10A with sigma of 0.04 3. Uiso/Uaniso restraints and constraints O3 \\sim O6 \\sim O8 \\sim O10 \\sim O12 \\sim O14 \\sim C41 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C59 \\sim C60 \\sim C62 \\sim C65 \\sim C67: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 O4 \\sim O5 \\sim O7 \\sim O9 \\sim O11 \\sim O13 \\sim C39 \\sim C40 \\sim C51 \\sim C52 \\sim C53 \\sim C55 \\sim C56 \\sim C57 \\sim C63 \\sim C64 \\sim C68 \\sim C69: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 O1 \\sim C31 \\sim C32 \\sim C33 \\sim C34: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 O2 \\sim C35 \\sim C36 \\sim C37 \\sim C38: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 C23 \\sim C24 \\sim Si3 \\sim C25 \\sim N4 \\sim C30 \\sim Si6 \\sim C27: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 C23 \\sim C24 \\sim Si3 \\sim C25: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 N4 \\sim C27 \\sim Si6 \\sim C28 \\sim C30: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 N1 \\sim N2 \\sim C1 \\sim H1 \\sim C2 \\sim H2 \\sim C3 \\sim H3 \\sim C4 \\sim H4 \\sim C5 \\sim C6 \\sim C7 \\sim H7 \\sim C8 \\sim H8 \\sim C9 \\sim H9 \\sim C10 \\sim H10: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 N1A \\sim N2A \\sim C1A \\sim C2A \\sim H2A \\sim C3A \\sim H3A \\sim C4A \\sim H4A \\sim C5A \\sim C6A \\sim C7A \\sim H7A \\sim C8A \\sim H8A \\sim C9A \\sim H9A \\sim C10A \\sim H10A \\sim H1A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 Uanis(O14) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C60) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(O1) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(Si3) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(Si6) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(Si3) \\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(N4) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(Si6) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(Si6) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.0002 Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, : with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(N1A) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C10A) \\sim Ueq, : with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C6) = Uanis(C2) Uanis(C10) = Uanis(C1) Uanis(C34) = Uanis(C31) = Uanis(C32) = Uanis(C33) Uanis(O14) = Uanis(O4) = Uanis(O3) = Uanis(O5) = Uanis(O6) = Uanis(O7) = Uanis(O8) = Uanis(O9) = Uanis(O10) = Uanis(O11) = Uanis(O12) = Uanis(O13) Uanis(C40) = Uanis(C59) = Uanis(C41) = Uanis(C50) = Uanis(C39) Uanis(C25) = Uanis(C24) = Uanis(C23) Uanis(C35) = Uanis(C38) Uanis(C24) = Uanis(C25A) Uanis(C24A) = Uanis(C23) Uanis(C23A) = Uanis(C25) Uanis(Si3) = Uanis(Si1) = Uanis(Si3A) Uanis(C1) = Uanis(C7) Uanis(C22) = Uanis(C21) Uanis(Si6A) = Uanis(Si6) Uanis(C27A) = Uanis(C27) Uanis(C30A) = Uanis(C30) Uanis(N1A) = Uanis(N4) Uanis(N1) = Uanis(N3) Uanis(C3) = Uanis(C3A) Uanis(C2A) = Uanis(C2) 4. Rigid body (RIGU) restrains O3, O6, O8, O10, O12, O14, C41, C45, C46, C47, C48, C49, C50, C59, C60, C62, C65, C67 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O4, O5, O7, O9, O11, O13, C39, C40, C51, C52, C53, C55, C56, C57, C63, C64, C68, C69 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O1, C31, C32, C33, C34 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O2, C35, C36, C37, C38 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C23, C24, Si3, C25, N4, C30, Si6, C27 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C23, C24, Si3, C25 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 N4, C27, Si6, C28, C30 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 N1, N2, C1, H1, C2, H2, C3, H3, C4, H4, C5, C6, C7, H7, C8, H8, C9, H9, C10, H10 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 N1A, N2A, C1A, C2A, H2A, C3A, H3A, C4A, H4A, C5A, C6A, C7A, H7A, C8A, H8A, C9A, H9A, C10A, H10A, H1A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Fixed Sof: Si3(0.5) N1(0.5) N2(0.5) C1(0.5) H1(0.5) C2(0.5) H2(0.5) C3(0.5) H3(0.5) C4(0.5) H4(0.5) C5(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5) C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) Si6(0.5) C6(0.5) C7(0.5) H7(0.5) C8(0.5) H8(0.5) C9(0.5) H9(0.5) C10(0.5) H10(0.5) C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) O1(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) C32(0.5) H32A(0.5) H32B(0.5) C33(0.5) H33A(0.5) H33B(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5) O2(0.5) C35(0.5) H35A(0.5) H35B(0.5) C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5) C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5) C38(0.5) H38A(0.5) H38B(0.5) O3(0.5) O6(0.5) O8(0.5) O10(0.5) O12(0.5) O14(0.5) C41(0.5) H41A(0.5) H41B(0.5) C45(0.5) H45A(0.5) H45B(0.5) C46(0.5) H46A(0.5) H46B(0.5) C47(0.5) H47A(0.5) H47B(0.5) C48(0.5) H48A(0.5) H48B(0.5) C49(0.5) H49A(0.5) H49B(0.5) C50(0.5) H50A(0.5) H50B(0.5) C59(0.5) H59A(0.5) H59B(0.5) C60(0.5) H60A(0.5) H60B(0.5) C62(0.5) H62A(0.5) H62B(0.5) C65(0.5) H65A(0.5) H65B(0.5) C67(0.5) H67A(0.5) H67B(0.5) O4(0.5) O5(0.5) O7(0.5) O9(0.5) O11(0.5) O13(0.5) C39(0.5) H39A(0.5) H39B(0.5) C40(0.5) H40A(0.5) H40B(0.5) C51(0.5) H51A(0.5) H51B(0.5) C52(0.5) H52A(0.5) H52B(0.5) C53(0.5) H53A(0.5) H53B(0.5) C55(0.5) H55A(0.5) H55B(0.5) C56(0.5) H56A(0.5) H56B(0.5) C57(0.5) H57A(0.5) H57B(0.5) C63(0.5) H63A(0.5) H63B(0.5) C64(0.5) H64A(0.5) H64B(0.5) C68(0.5) H68A(0.5) H68B(0.5) C69(0.5) H69A(0.5) H69B(0.5) C23A(0.5) H23D(0.5) H23E(0.5) H23F(0.5) C24A(0.5) H24D(0.5) H24E(0.5) H24F(0.5) Si3A(0.5) C25A(0.5) H25D(0.5) H25E(0.5) H25F(0.5) C27A(0.5) H27D(0.5) H27E(0.5) H27F(0.5) Si6A(0.5) C28A(0.5) H28D(0.5) H28E(0.5) H28F(0.5) C30A(0.5) H30D(0.5) H30E(0.5) H30F(0.5) N1A(0.5) N2A(0.5) C1A(0.5) H1A(0.5) C2A(0.5) H2A(0.5) C3A(0.5) H3A(0.5) C4A(0.5) H4A(0.5) C5A(0.5) C6A(0.5) C7A(0.5) H7A(0.5) C8A(0.5) H8A(0.5) C9A(0.5) H9A(0.5) C10A(0.5) H10A(0.5) 6.a Secondary CH2 refined with riding coordinates: C32(H32A,H32B), C33(H33A,H33B), C35(H35A,H35B), C38(H38A,H38B), C41(H41A, H41B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C59(H59A,H59B), C60(H60A,H60B), C62(H62A,H62B), C65(H65A,H65B), C67(H67A,H67B), C39(H39A,H39B), C40(H40A,H40B), C51(H51A, H51B), C52(H52A,H52B), C53(H53A,H53B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C63(H63A,H63B), C64(H64A,H64B), C68(H68A,H68B), C69(H69A,H69B) 6.b Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C7A(H7A), C8A(H8A), C9A(H9A), C10A(H10A) 6.c Idealised Me refined as rotating group: C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C21(H21A,H21B, H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A, H25B,H25C), C28(H28A,H28B,H28C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C19(H19A,H19B,H19C), C31(H31A,H31B,H31C), C34(H34A,H34B, H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F), C25A(H25D,H25E,H25F), C27A(H27D,H27E,H27F), C28A(H28D, H28E,H28F), C30A(H30D,H30E,H30F) ; _shelx_res_file ; TITL gwx052a_0m_a.res in P2(1)/c k{18c6}zn10.res created by SHELXL-2018/3 at 09:59:21 on 05-Jun-2019 REM Old TITL GWX052a_0m in P2/c REM SHELXT solution in P2(1)/c REM R1 0.282, Rweak 0.058, Alpha 0.119, Orientation as input REM Formula found by SHELXT: C42 N7 O11 Si5 K2 Zn CELL 0.71073 12.1899 18.4365 22.8273 90 95.423 90 ZERR 4 0.0007 0.001 0.0013 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H K N O Si Zn UNIT 152 312 4 16 28 16 4 DFIX 1.8 Si6 C28 SADI O14 C59 O14 C60 O12 C41 O12 C45 O10 C46 O10 C47 O8 C48 O8 C49 O6 C50 = O6 C67 O3 C65 O3 C62 SADI C59 C41 C45 C46 C47 C48 C49 C50 C67 C65 C62 C60 SADI 0.04 C41 C45 C46 C47 C48 C49 C50 C67 C65 C62 C60 C59 SADI 0.04 O14 C41 O12 C46 O10 C48 O8 C50 O6 C65 O3 C60 O12 C59 O10 C45 O8 = C47 O6 C49 O3 C67 O14 C62 SADI O4 C63 O4 C39 O5 C64 O5 C68 O7 C69 O7 C51 O9 C52 O9 C53 O11 C55 O11 = C56 O13 C57 O13 C40 SADI C63 C64 C68 C69 C51 C52 C53 C55 C56 C57 C40 C39 SADI 0.04 C64 C68 C69 C51 C52 C53 C55 C56 C57 C40 C39 C63 SADI 0.04 O4 C64 O5 C69 O7 C52 O9 C55 O11 C57 O13 C39 O5 C63 O7 C68 O9 C51 = O11 C53 O13 C56 O4 C40 SADI Si1 C20 Si1 C19 SADI C37 C38 C35 C36 SADI O2 C38 O2 C35 SADI 0.04 C37 O2 O2 C36 SADI C34 C33 C32 C31 SADI O1 C33 O1 C32 SADI 0.04 C34 O1 O1 C31 SADI Si3 N4 Si3A N4 SADI Si3 C23 Si3A C23A SADI Si3 C24 Si3A C24A SADI Si3 C25 Si3A C25A SADI 0.04 N4 C23 N4 C23A SADI 0.04 N4 C24 N4 C24A SADI 0.04 N4 C25 N4 C25A SADI 0.04 C23 C24 C23A C24A SADI 0.04 C23 C25 C23A C25A SADI 0.04 C24 C25 C24A C25A SADI N4 Si6 N4 Si6A SADI C28 Si6 C28A Si6A SADI Si6 C27 Si6A C27A SADI Si6 C30 Si6A C30A SADI 0.04 N4 C28 N4 C28A SADI 0.04 N4 C27 N4 C27A SADI 0.04 N4 C30 N4 C30A SADI 0.04 C28 C27 C28A C27A SADI 0.04 C28 C30 C28A C30A SADI 0.04 C27 C30 C27A C30A SADI Zn1 N1 Zn1 N1A SADI Zn1 N2 Zn1 N2A SADI N1 C1 N1A C1A SADI N1 C5 N1A C5A SADI N2 C6 N2A C6A SADI N2 C10 N2A C10A SADI C1 C2 C1A C2A SADI C2 C3 C2A C3A SADI C3 C4 C3A C4A SADI C4 C5 C4A C5A SADI C5 C6 C5A C6A SADI C6 C7 C6A C7A SADI C7 C8 C7A C8A SADI C8 C9 C8A C9A SADI C9 C10 C9A C10A SADI 0.04 Zn1 C1 Zn1 C1A SADI 0.04 Zn1 C5 Zn1 C5A SADI 0.04 Zn1 C6 Zn1 C6A SADI 0.04 Zn1 C10 Zn1 C10A SADI 0.04 N1 C2 N1A C2A SADI 0.04 N1 C4 N1A C4A SADI 0.04 N1 C6 N1A C6A SADI 0.04 N2 C5 N2A C5A SADI 0.04 N2 C7 N2A C7A SADI 0.04 N2 C9 N2A C9A SADI 0.04 C1 C3 C1A C3A SADI 0.04 C1 C5 C1A C5A SADI 0.04 C2 C4 C2A C4A SADI 0.04 C3 C5 C3A C5A SADI 0.04 C4 C6 C4A C6A SADI 0.04 C5 C7 C5A C7A SADI 0.04 C6 C8 C6A C8A SADI 0.04 C6 C10 C6A C10A SADI 0.04 C7 C9 C7A C9A SADI 0.04 C8 C10 C8A C10A SIMU O3 > C67 SIMU O4 > C69 SIMU O1 > C34 SIMU O2 > C38 SIMU C23 C24 Si3 C25 N4 C30 Si6 C27 SIMU C23 C24 Si3 C25 SIMU N4 C27 Si6 C28 C30 SIMU N1 N2 C1 H1 C2 H2 C3 H3 C4 H4 C5 C6 C7 H7 C8 H8 C9 H9 C10 H10 SIMU N1A N2A C1A C2A H2A C3A H3A C4A H4A C5A C6A C7A H7A C8A H8A C9A H9A = C10A H10A H1A RIGU O3 > C67 RIGU O4 > C69 RIGU O1 > C34 RIGU O2 > C38 RIGU C23 C24 Si3 C25 N4 C30 Si6 C27 RIGU C23 C24 Si3 C25 RIGU N4 C27 Si6 C28 C30 RIGU N1 N2 C1 H1 C2 H2 C3 H3 C4 H4 C5 C6 C7 H7 C8 H8 C9 H9 C10 H10 RIGU N1A N2A C1A C2A H2A C3A H3A C4A H4A C5A C6A C7A H7A C8A H8A C9A H9A = C10A H10A H1A ISOR O14 O12 O10 O8 O6 O3 C59 C41 C45 C46 C47 C48 C49 C50 C67 C65 C62 C60 ISOR O4 O5 O7 O9 O11 O13 C63 C64 C68 C69 C51 C52 C53 C55 C56 C57 C40 C39 ISOR O1 C34 C33 C32 C31 ISOR C36 C35 O2 C38 C37 ISOR C23 C24 Si3 C25 N4 C30 Si6 C27 ISOR C23 C24 Si3 C25 ISOR N4 C27 Si6 C28 C30 ISOR 0.01 0.0002 Si6 C27 ISOR 0.01 0.02 C27 C28 C30 ISOR N1 N2 C1 H1 C2 H2 C3 H3 C4 H4 C5 C6 C7 H7 C8 H8 C9 H9 C10 H10 ISOR N1A N2A C1A C2A H2A C3A H3A C4A H4A C5A C6A C7A H7A C8A H8A C9A H9A = C10A H10A H1A EADP C6 C2 EADP C10 C1 EADP C34 C31 C32 C33 EADP O14 O4 O3 O5 O6 O7 O8 O9 O10 O11 O12 O13 EADP C40 C59 C41 C50 C39 EADP C25 C24 C23 EADP C35 C38 EADP C24 C25A EADP C24A C23 EADP C23A C25 EADP Si3 Si1 Si3A EADP C1 C7 EADP C22 C21 EADP Si6A Si6 EADP C27A C27 EADP C30A C30 EADP N1A N4 EADP N1 N3 EADP C3 C3A EADP C2A C2 L.S. 20 PLAN 20 SIZE 0.15 0.383 0.492 TEMP -173.15 FREE K1 C21 FREE K1 H34a FREE C62 C8 BOND $H LIST 6 fmap 2 acta OMIT 0 50 OMIT 2 14 4 REM REM REM WGHT 0.000200 100.834503 FVAR 0.31166 ZN1 7 0.522916 0.743432 0.551876 11.00000 0.02548 0.01086 = 0.02036 -0.00231 0.01103 -0.00280 SI1 6 0.777408 0.716455 0.556144 11.00000 0.02849 0.04101 = 0.03352 -0.01753 0.00520 -0.00490 SI2 6 0.630338 0.637136 0.465319 11.00000 0.02635 0.01770 = 0.02172 -0.00863 0.00485 -0.00277 PART 1 SI3 6 0.447433 0.852071 0.454778 10.50000 0.02849 0.04101 = 0.03352 -0.01753 0.00520 -0.00490 N1 4 0.546496 0.811718 0.625064 10.50000 0.02267 0.02485 = 0.03650 -0.01839 0.01692 -0.01103 N2 4 0.481626 0.674175 0.619148 10.50000 0.02584 0.02191 = 0.01960 -0.00187 0.00327 0.00165 PART 0 N3 4 0.652649 0.701261 0.518395 11.00000 0.02267 0.02485 = 0.03650 -0.01839 0.01692 -0.01103 N4 4 0.397300 0.785292 0.502670 11.00000 0.05228 0.03220 = 0.02759 0.00219 0.01362 0.01750 PART 1 C1 1 0.552045 0.886088 0.619419 10.50000 0.02873 0.02596 = 0.01919 -0.00717 0.00569 -0.00072 AFIX 43 H1 2 0.548878 0.906297 0.581014 10.50000 -1.20000 AFIX 0 C2 1 0.561951 0.932217 0.666888 10.50000 0.02361 0.02211 = 0.02617 -0.00586 -0.00003 0.00846 AFIX 43 H2 2 0.567923 0.983286 0.662644 10.50000 -1.20000 AFIX 0 C3 1 0.562626 0.898837 0.721735 10.50000 0.04427 0.02774 = 0.01987 -0.01216 -0.00719 0.00759 AFIX 43 H3 2 0.584123 0.926196 0.756183 10.50000 -1.20000 AFIX 0 C4 1 0.532711 0.826663 0.727347 10.50000 0.04297 0.02477 = 0.02049 -0.00128 -0.00798 0.01823 AFIX 43 H4 2 0.521117 0.807822 0.765003 10.50000 -1.20000 AFIX 0 C5 1 0.519171 0.780279 0.676564 10.50000 0.02271 0.02228 = 0.03082 -0.00850 0.00757 0.00690 PART 0 C16 1 0.481785 0.623896 0.441148 11.00000 0.02891 0.02810 = 0.04513 -0.00937 -0.01509 0.00124 AFIX 137 H16A 2 0.443879 0.605753 0.474197 11.00000 -1.50000 H16B 2 0.473941 0.588689 0.408859 11.00000 -1.50000 H16C 2 0.449204 0.670263 0.427644 11.00000 -1.50000 AFIX 0 C17 1 0.694753 0.659541 0.395663 11.00000 0.07084 0.03880 = 0.03482 -0.00551 0.02221 -0.00502 AFIX 137 H17A 2 0.657565 0.701752 0.376758 11.00000 -1.50000 H17B 2 0.687131 0.617966 0.368836 11.00000 -1.50000 H17C 2 0.773062 0.670556 0.405172 11.00000 -1.50000 AFIX 0 C18 1 0.681386 0.545098 0.488937 11.00000 0.04132 0.02763 = 0.03485 -0.00760 -0.00071 0.01004 AFIX 137 H18A 2 0.760299 0.547656 0.501801 11.00000 -1.50000 H18B 2 0.669311 0.511288 0.455827 11.00000 -1.50000 H18C 2 0.641312 0.528094 0.521564 11.00000 -1.50000 AFIX 0 C21 1 0.787042 0.679766 0.631811 11.00000 0.05272 0.07219 = 0.07699 -0.01467 -0.01937 -0.02499 AFIX 137 H21A 2 0.736290 0.706212 0.654919 11.00000 -1.50000 H21B 2 0.862582 0.685419 0.650100 11.00000 -1.50000 H21C 2 0.767362 0.628214 0.630532 11.00000 -1.50000 AFIX 0 C22 1 0.814758 0.814613 0.562062 11.00000 0.05272 0.07219 = 0.07699 -0.01467 -0.01937 -0.02499 AFIX 137 H22A 2 0.810682 0.836044 0.522629 11.00000 -1.50000 H22B 2 0.889898 0.819555 0.581071 11.00000 -1.50000 H22C 2 0.763292 0.839740 0.585592 11.00000 -1.50000 AFIX 0 PART 1 C23 1 0.597709 0.862904 0.456738 10.50000 0.10966 0.03303 = 0.03629 0.01925 0.03289 0.02533 AFIX 137 H23A 2 0.626139 0.884116 0.494521 10.50000 -1.50000 H23B 2 0.615156 0.894963 0.424655 10.50000 -1.50000 H23C 2 0.631912 0.815404 0.452084 10.50000 -1.50000 AFIX 0 C24 1 0.399666 0.815774 0.376091 10.50000 0.10966 0.03303 = 0.03629 0.01925 0.03289 0.02533 AFIX 137 H24A 2 0.454304 0.781343 0.363812 10.50000 -1.50000 H24B 2 0.392354 0.856432 0.348342 10.50000 -1.50000 H24C 2 0.328376 0.791337 0.376641 10.50000 -1.50000 AFIX 0 C25 1 0.379801 0.941249 0.457277 10.50000 0.10966 0.03303 = 0.03629 0.01925 0.03289 0.02533 AFIX 137 H25A 2 0.303252 0.937305 0.440114 10.50000 -1.50000 H25B 2 0.419042 0.976485 0.434804 10.50000 -1.50000 H25C 2 0.381136 0.957388 0.498243 10.50000 -1.50000 AFIX 0 PART 0 PART -2 C28 1 0.232570 0.797590 0.588483 10.50000 0.02603 0.04037 = 0.05204 0.00143 0.00575 -0.00986 AFIX 137 H28A 2 0.283004 0.776864 0.620080 10.50000 -1.50000 H28B 2 0.156511 0.785225 0.595059 10.50000 -1.50000 H28C 2 0.240987 0.850450 0.588230 10.50000 -1.50000 AFIX 0 SI6 6 0.265370 0.759908 0.516198 10.50000 0.04170 0.07844 = 0.02656 -0.00063 0.00562 0.03498 PART 0 PART 1 C6 1 0.478236 0.708194 0.674398 10.50000 0.02361 0.02211 = 0.02617 -0.00586 -0.00003 0.00846 C7 1 0.435345 0.666781 0.718960 10.50000 0.02873 0.02596 = 0.01919 -0.00717 0.00569 -0.00072 AFIX 43 H7 2 0.428774 0.689217 0.755930 10.50000 -1.20000 AFIX 0 C8 1 0.402757 0.596171 0.711819 10.50000 0.03369 0.02593 = 0.01900 0.00492 0.00942 -0.00020 AFIX 43 H8 2 0.372854 0.570490 0.742699 10.50000 -1.20000 AFIX 0 C9 1 0.414739 0.562507 0.657377 10.50000 0.03749 0.02137 = 0.02559 -0.00333 0.00566 -0.00822 AFIX 43 H9 2 0.399333 0.512427 0.651221 10.50000 -1.20000 AFIX 0 C10 1 0.449385 0.605019 0.614037 10.50000 0.02873 0.02596 = 0.01919 -0.00717 0.00569 -0.00072 AFIX 43 H10 2 0.450797 0.583362 0.576354 10.50000 -1.20000 AFIX 0 C20 1 0.897598 0.656119 0.536140 10.50000 0.01743 0.04728 = 0.08430 -0.01945 0.00057 0.00749 AFIX 137 H20A 2 0.964930 0.669554 0.560611 10.50000 -1.50000 H20B 2 0.908818 0.663004 0.494557 10.50000 -1.50000 H20C 2 0.880125 0.605136 0.543087 10.50000 -1.50000 AFIX 0 PART 0 PART -2 C27 1 0.241503 0.659018 0.517880 10.50000 0.05547 0.05550 = 0.05549 -0.00003 0.00526 0.00000 AFIX 137 H27A 2 0.270060 0.636576 0.483487 10.50000 -1.50000 H27B 2 0.162338 0.649332 0.517156 10.50000 -1.50000 H27C 2 0.279694 0.638654 0.553872 10.50000 -1.50000 AFIX 0 C30 1 0.149735 0.788786 0.462169 10.50000 0.06838 0.09664 = 0.05797 -0.00813 -0.00241 0.03951 AFIX 137 H30A 2 0.148840 0.841819 0.459253 10.50000 -1.50000 H30B 2 0.079822 0.771893 0.475240 10.50000 -1.50000 H30C 2 0.159646 0.767853 0.423561 10.50000 -1.50000 AFIX 0 PART 0 PART 2 C19 1 0.896114 0.695410 0.509273 10.50000 0.02467 0.07453 = 0.03365 -0.01873 0.00953 0.00044 AFIX 137 H19A 2 0.904742 0.642747 0.506105 10.50000 -1.50000 H19B 2 0.964501 0.716559 0.527877 10.50000 -1.50000 H19C 2 0.879727 0.716175 0.469899 10.50000 -1.50000 AFIX 0 PART 0 K1 3 0.926749 0.555321 0.728552 11.00000 0.04736 0.03729 = 0.03934 -0.00794 0.01403 0.00587 PART 1 O1 5 1.022188 0.491162 0.835111 10.50000 0.04608 0.18501 = 0.12685 0.05424 0.01226 0.00094 C31 1 0.922792 0.511434 0.922596 10.50000 0.06047 0.16498 = 0.12765 0.04834 0.02375 -0.00390 AFIX 137 H31A 2 0.883298 0.540135 0.891193 10.50000 -1.50000 H31B 2 0.945968 0.543064 0.955994 10.50000 -1.50000 H31C 2 0.874096 0.473418 0.935309 10.50000 -1.50000 AFIX 0 C32 1 1.011287 0.481062 0.902575 10.50000 0.06047 0.16498 = 0.12765 0.04834 0.02375 -0.00390 AFIX 23 H32A 2 1.010028 0.428452 0.911173 10.50000 -1.20000 H32B 2 1.077874 0.501548 0.924751 10.50000 -1.20000 AFIX 0 C33 1 1.133262 0.459645 0.817613 10.50000 0.06047 0.16498 = 0.12765 0.04834 0.02375 -0.00390 AFIX 23 H33A 2 1.187892 0.499401 0.817831 10.50000 -1.20000 H33B 2 1.161262 0.423739 0.847633 10.50000 -1.20000 AFIX 0 C34 1 1.124876 0.427235 0.763807 10.50000 0.06047 0.16498 = 0.12765 0.04834 0.02375 -0.00390 AFIX 137 H34A 2 1.054356 0.440342 0.742206 10.50000 -1.50000 H34B 2 1.128773 0.374467 0.768745 10.50000 -1.50000 H34C 2 1.185461 0.443560 0.741727 10.50000 -1.50000 AFIX 0 PART 0 PART 2 O2 5 1.054330 0.466971 0.797622 10.50000 0.05554 0.05047 = 0.06159 0.00854 -0.00872 0.00333 C35 1 1.115417 0.484223 0.852307 10.50000 0.10020 0.05650 = 0.06961 0.01090 -0.02072 0.01261 AFIX 23 H35A 2 1.163892 0.442610 0.864095 10.50000 -1.20000 H35B 2 1.163537 0.526203 0.845966 10.50000 -1.20000 AFIX 0 C36 1 1.058758 0.499183 0.894803 10.50000 0.07797 0.12432 = 0.08960 -0.06062 -0.02625 -0.03325 AFIX 137 H36A 2 1.035667 0.550085 0.892130 10.50000 -1.50000 H36B 2 1.103493 0.491068 0.932196 10.50000 -1.50000 H36C 2 0.993499 0.467912 0.892794 10.50000 -1.50000 AFIX 0 C37 1 1.138472 0.357231 0.765572 10.50000 0.06233 0.04146 = 0.06862 0.02001 -0.01565 -0.00803 AFIX 137 H37A 2 1.205398 0.344102 0.790508 10.50000 -1.50000 H37B 2 1.158291 0.386458 0.732296 10.50000 -1.50000 H37C 2 1.100618 0.313048 0.750824 10.50000 -1.50000 AFIX 0 C38 1 1.078177 0.391863 0.794042 10.50000 0.10020 0.05650 = 0.06961 0.01090 -0.02072 0.01261 AFIX 23 H38A 2 1.101308 0.377906 0.835242 10.50000 -1.20000 H38B 2 1.005055 0.369132 0.784628 10.50000 -1.20000 AFIX 0 PART 0 PART 3 O3 5 0.737826 0.482734 0.729304 10.50000 0.07423 0.07751 = 0.07767 -0.02548 0.02950 -0.00875 O6 5 0.890214 0.426676 0.661739 10.50000 0.07423 0.07751 = 0.07767 -0.02548 0.02950 -0.00875 O8 5 1.068319 0.521151 0.645099 10.50000 0.07423 0.07751 = 0.07767 -0.02548 0.02950 -0.00875 O10 5 1.124963 0.629847 0.723251 10.50000 0.07423 0.07751 = 0.07767 -0.02548 0.02950 -0.00875 O12 5 0.966459 0.687211 0.788222 10.50000 0.07423 0.07751 = 0.07767 -0.02548 0.02950 -0.00875 O14 5 0.784343 0.600281 0.804662 10.50000 0.07423 0.07751 = 0.07767 -0.02548 0.02950 -0.00875 C41 1 0.914165 0.694984 0.840286 10.50000 0.09897 0.08612 = 0.08176 -0.03861 0.04460 -0.01320 AFIX 23 H41A 2 0.918088 0.746056 0.853717 10.50000 -1.20000 H41B 2 0.950740 0.664068 0.871786 10.50000 -1.20000 AFIX 0 C45 1 1.076167 0.711532 0.796839 10.50000 0.07495 0.04913 = 0.04721 -0.01060 0.00144 -0.03506 AFIX 23 H45A 2 1.115883 0.683899 0.829454 10.50000 -1.20000 H45B 2 1.077130 0.763406 0.808083 10.50000 -1.20000 AFIX 0 C46 1 1.133907 0.702162 0.742153 10.50000 0.05278 0.06499 = 0.04782 -0.00874 -0.01380 -0.00365 AFIX 23 H46A 2 1.100456 0.734615 0.710839 10.50000 -1.20000 H46B 2 1.212583 0.715383 0.750305 10.50000 -1.20000 AFIX 0 C47 1 1.189842 0.617215 0.677268 10.50000 0.06409 0.05168 = 0.11185 0.00319 0.05889 0.00166 AFIX 23 H47A 2 1.267577 0.629064 0.690220 10.50000 -1.20000 H47B 2 1.165367 0.649113 0.643662 10.50000 -1.20000 AFIX 0 C48 1 1.181496 0.538060 0.657665 10.50000 0.05724 0.04866 = 0.05711 0.01731 0.03811 0.00840 AFIX 23 H48A 2 1.221002 0.530839 0.622165 10.50000 -1.20000 H48B 2 1.215099 0.506070 0.689265 10.50000 -1.20000 AFIX 0 C49 1 1.060936 0.450044 0.621535 10.50000 0.09842 0.07694 = 0.08342 -0.02877 0.04516 -0.00651 AFIX 23 H49A 2 1.095695 0.414867 0.650349 10.50000 -1.20000 H49B 2 1.099194 0.447360 0.585223 10.50000 -1.20000 AFIX 0 C50 1 0.939531 0.432756 0.607959 10.50000 0.09897 0.08612 = 0.08176 -0.03861 0.04460 -0.01320 AFIX 23 H50A 2 0.903032 0.471759 0.583487 10.50000 -1.20000 H50B 2 0.930812 0.386653 0.585771 10.50000 -1.20000 AFIX 0 C59 1 0.793473 0.671786 0.826467 10.50000 0.09897 0.08612 = 0.08176 -0.03861 0.04460 -0.01320 AFIX 23 H59A 2 0.755108 0.675335 0.862697 10.50000 -1.20000 H59B 2 0.756697 0.705356 0.796979 10.50000 -1.20000 AFIX 0 C60 1 0.675694 0.582036 0.785771 10.50000 0.07012 0.09896 = 0.08320 -0.02182 0.02661 -0.00810 AFIX 23 H60A 2 0.650284 0.611080 0.750605 10.50000 -1.20000 H60B 2 0.627589 0.593374 0.817152 10.50000 -1.20000 AFIX 0 C62 1 0.667199 0.501546 0.770804 10.50000 0.06808 0.11257 = 0.11005 -0.04691 0.04501 -0.04143 AFIX 23 H62A 2 0.685414 0.472670 0.806983 10.50000 -1.20000 H62B 2 0.590525 0.489950 0.755460 10.50000 -1.20000 AFIX 0 C65 1 0.724986 0.411053 0.709403 10.50000 0.05727 0.06934 = 0.07511 -0.00516 -0.00205 -0.01008 AFIX 23 H65A 2 0.645725 0.399034 0.702060 10.50000 -1.20000 H65B 2 0.759135 0.377186 0.739466 10.50000 -1.20000 AFIX 0 C67 1 0.780669 0.403999 0.652708 10.50000 0.08713 0.05246 = 0.06949 -0.02172 0.00750 -0.01997 AFIX 23 H67A 2 0.777847 0.352845 0.639460 10.50000 -1.20000 H67B 2 0.740913 0.433941 0.621557 10.50000 -1.20000 AFIX 0 PART 0 PART 4 O4 5 0.748065 0.502273 0.783862 10.50000 0.07423 0.07751 = 0.07767 -0.02548 0.02950 -0.00875 O5 5 0.821134 0.421275 0.689527 10.50000 0.07423 0.07751 = 0.07767 -0.02548 0.02950 -0.00875 O7 5 0.966469 0.480794 0.618626 10.50000 0.07423 0.07751 = 0.07767 -0.02548 0.02950 -0.00875 O9 5 1.107268 0.591784 0.661780 10.50000 0.07423 0.07751 = 0.07767 -0.02548 0.02950 -0.00875 O11 5 1.032610 0.683855 0.746578 10.50000 0.07423 0.07751 = 0.07767 -0.02548 0.02950 -0.00875 O13 5 0.868332 0.624937 0.820759 10.50000 0.07423 0.07751 = 0.07767 -0.02548 0.02950 -0.00875 C39 1 0.738521 0.534470 0.836689 10.50000 0.09897 0.08612 = 0.08176 -0.03861 0.04460 -0.01320 AFIX 23 H39A 2 0.781761 0.505932 0.867528 10.50000 -1.20000 H39B 2 0.660310 0.532133 0.844931 10.50000 -1.20000 AFIX 0 C40 1 0.773954 0.608687 0.841647 10.50000 0.09897 0.08612 = 0.08176 -0.03861 0.04460 -0.01320 AFIX 23 H40A 2 0.715711 0.639353 0.821136 10.50000 -1.20000 H40B 2 0.779666 0.622233 0.883791 10.50000 -1.20000 AFIX 0 C51 1 1.067590 0.488594 0.601211 10.50000 0.08921 0.08321 = 0.07706 -0.02885 0.04747 -0.00745 AFIX 23 H51A 2 1.067217 0.474112 0.559431 10.50000 -1.20000 H51B 2 1.119862 0.456728 0.624974 10.50000 -1.20000 AFIX 0 C52 1 1.102468 0.562845 0.608109 10.50000 0.07032 0.08332 = 0.08281 -0.02833 0.04226 -0.00550 AFIX 23 H52A 2 1.176590 0.566907 0.594034 10.50000 -1.20000 H52B 2 1.051908 0.592921 0.581716 10.50000 -1.20000 AFIX 0 C53 1 1.135904 0.660846 0.667518 10.50000 0.10062 0.07978 = 0.08328 -0.01640 0.03616 -0.02180 AFIX 23 H53A 2 1.088721 0.689307 0.638242 10.50000 -1.20000 H53B 2 1.212824 0.665772 0.657511 10.50000 -1.20000 AFIX 0 C55 1 1.128520 0.693110 0.725143 10.50000 0.06911 0.05665 = 0.07700 -0.01237 0.02274 -0.01550 AFIX 23 H55A 2 1.187002 0.672011 0.753073 10.50000 -1.20000 H55B 2 1.143093 0.745779 0.722509 10.50000 -1.20000 AFIX 0 C56 1 1.004385 0.704862 0.797506 10.50000 0.10364 0.07206 = 0.07186 0.01076 0.04783 0.03082 AFIX 23 H56A 2 1.020600 0.757387 0.800966 10.50000 -1.20000 H56B 2 1.054187 0.680171 0.827989 10.50000 -1.20000 AFIX 0 C57 1 0.893790 0.694561 0.812888 10.50000 0.11292 0.07226 = 0.13118 0.01226 0.07123 0.02170 AFIX 23 H57A 2 0.884522 0.721650 0.849541 10.50000 -1.20000 H57B 2 0.841634 0.715132 0.781341 10.50000 -1.20000 AFIX 0 C63 1 0.737170 0.432164 0.778542 10.50000 0.04777 0.09113 = 0.09326 -0.02633 0.01379 -0.00524 AFIX 23 H63A 2 0.668133 0.417517 0.794906 10.50000 -1.20000 H63B 2 0.799025 0.408593 0.802572 10.50000 -1.20000 AFIX 0 C64 1 0.734644 0.405311 0.719126 10.50000 0.05751 0.06850 = 0.10174 -0.02679 0.01282 -0.03265 AFIX 23 H64A 2 0.727294 0.351866 0.720300 10.50000 -1.20000 H64B 2 0.667540 0.424491 0.696547 10.50000 -1.20000 AFIX 0 C68 1 0.815493 0.406966 0.632910 10.50000 0.09036 0.06856 = 0.08731 -0.02825 0.01651 -0.00439 AFIX 23 H68A 2 0.758425 0.438383 0.612238 10.50000 -1.20000 H68B 2 0.791630 0.356004 0.626623 10.50000 -1.20000 AFIX 0 C69 1 0.917638 0.417425 0.606867 10.50000 0.08476 0.06538 = 0.03930 -0.01898 -0.00329 0.00293 AFIX 23 H69A 2 0.969264 0.378272 0.620773 10.50000 -1.20000 H69B 2 0.903055 0.412470 0.563648 10.50000 -1.20000 AFIX 0 PART 0 PART 2 C23A 1 0.346958 0.937632 0.474741 10.50000 0.10966 0.03303 = 0.03629 0.01925 0.03289 0.02533 AFIX 137 H23D 2 0.267849 0.932980 0.478513 10.50000 -1.50000 H23E 2 0.358994 0.974975 0.445474 10.50000 -1.50000 H23F 2 0.385121 0.951426 0.512824 10.50000 -1.50000 AFIX 0 C24A 1 0.557890 0.868937 0.444205 10.50000 0.10966 0.03303 = 0.03629 0.01925 0.03289 0.02533 AFIX 137 H24D 2 0.592734 0.883638 0.482828 10.50000 -1.50000 H24E 2 0.563964 0.908422 0.415952 10.50000 -1.50000 H24F 2 0.594908 0.825657 0.430778 10.50000 -1.50000 AFIX 0 SI3A 6 0.403148 0.847281 0.450275 10.50000 0.02849 0.04101 = 0.03352 -0.01753 0.00520 -0.00490 C25A 1 0.346247 0.832847 0.373559 10.50000 0.10966 0.03303 = 0.03629 0.01925 0.03289 0.02533 AFIX 137 H25D 2 0.377255 0.788338 0.358418 10.50000 -1.50000 H25E 2 0.365285 0.874163 0.349477 10.50000 -1.50000 H25F 2 0.265911 0.828355 0.371943 10.50000 -1.50000 AFIX 0 PART 0 PART -1 C27A 1 0.241809 0.672695 0.534450 10.50000 0.05547 0.05550 = 0.05549 -0.00003 0.00526 0.00000 AFIX 137 H27D 2 0.250706 0.648640 0.496909 10.50000 -1.50000 H27E 2 0.166234 0.665731 0.544682 10.50000 -1.50000 H27F 2 0.293610 0.651742 0.565319 10.50000 -1.50000 AFIX 0 SI6A 6 0.270552 0.773122 0.527573 10.50000 0.04170 0.07844 = 0.02656 -0.00063 0.00562 0.03498 C28A 1 0.264440 0.817755 0.601794 10.50000 0.03449 0.03703 = 0.04518 0.00385 0.02625 0.00827 AFIX 137 H28D 2 0.318564 0.795025 0.630568 10.50000 -1.50000 H28E 2 0.190436 0.811834 0.614566 10.50000 -1.50000 H28F 2 0.281153 0.869531 0.598708 10.50000 -1.50000 AFIX 0 C30A 1 0.147468 0.803250 0.479901 10.50000 0.06838 0.09664 = 0.05797 -0.00813 -0.00241 0.03951 AFIX 137 H30D 2 0.153581 0.855188 0.471675 10.50000 -1.50000 H30E 2 0.081144 0.794400 0.499981 10.50000 -1.50000 H30F 2 0.142598 0.776090 0.442842 10.50000 -1.50000 AFIX 0 PART 0 PART 2 N1A 4 0.544026 0.812204 0.624994 10.50000 0.05228 0.03220 = 0.02759 0.00219 0.01362 0.01750 N2A 4 0.499165 0.671333 0.619582 10.50000 0.02565 0.01834 = 0.01024 -0.00230 0.00457 -0.00461 C1A 1 0.580022 0.881813 0.630626 10.50000 0.02191 0.03408 = 0.03046 -0.00851 0.01229 0.00255 AFIX 43 H1A 2 0.601739 0.904766 0.596296 10.50000 -1.20000 AFIX 0 C2A 1 0.587831 0.922033 0.681618 10.50000 0.02361 0.02211 = 0.02617 -0.00586 -0.00003 0.00846 AFIX 43 H2A 2 0.606328 0.972056 0.680815 10.50000 -1.20000 AFIX 0 C3A 1 0.568428 0.888847 0.734285 10.50000 0.04427 0.02774 = 0.01987 -0.01216 -0.00719 0.00759 AFIX 43 H3A 2 0.569120 0.915775 0.769800 10.50000 -1.20000 AFIX 0 C4A 1 0.548094 0.815163 0.732965 10.50000 0.04898 0.02412 = 0.02092 -0.00809 -0.00753 0.01442 AFIX 43 H4A 2 0.542443 0.789212 0.768508 10.50000 -1.20000 AFIX 0 C5A 1 0.535600 0.778202 0.677586 10.50000 0.02405 0.02188 = 0.01938 -0.00755 -0.00497 0.00900 C6A 1 0.513719 0.703505 0.675236 10.50000 0.03519 0.02369 = 0.01248 -0.00683 0.00455 0.00794 C7A 1 0.511775 0.661780 0.726085 10.50000 0.04967 0.02509 = 0.01665 -0.00505 0.00057 -0.00679 AFIX 43 H7A 2 0.517537 0.684368 0.763655 10.50000 -1.20000 AFIX 0 C8A 1 0.501564 0.588492 0.721463 10.50000 0.03733 0.02506 = 0.02241 -0.00184 0.00734 -0.00529 AFIX 43 H8A 2 0.500799 0.559256 0.755692 10.50000 -1.20000 AFIX 0 C9A 1 0.492184 0.556756 0.665383 10.50000 0.03258 0.01629 = 0.02359 -0.00022 0.00907 -0.00291 AFIX 43 H9A 2 0.485169 0.505643 0.661303 10.50000 -1.20000 AFIX 0 C10A 1 0.493171 0.599291 0.617068 10.50000 0.02079 0.01869 = 0.01863 -0.00371 0.00877 0.00052 AFIX 43 H10A 2 0.489403 0.576615 0.579562 10.50000 -1.20000 AFIX 0 HKLF 4 REM gwx052a_0m_a.res in P2(1)/c REM wR2 = 0.2596, GooF = S = 1.086, Restrained GooF = 1.015 for all data REM R1 = 0.1281 for 7347 Fo > 4sig(Fo) and 0.1506 for all 8987 data REM 693 parameters refined using 1954 restraints END WGHT 0.0002 100.6596 REM Highest difference peak 1.777, deepest hole -1.895, 1-sigma level 0.151 Q1 1 0.7662 0.7426 0.5377 11.00000 0.05 1.78 Q2 1 0.4738 0.8592 0.4554 11.00000 0.05 1.76 Q3 1 0.7818 0.6968 0.5800 11.00000 0.05 1.71 Q4 1 0.8370 0.5812 0.8380 11.00000 0.05 1.70 Q5 1 0.2908 0.8109 0.5260 11.00000 0.05 1.63 Q6 1 0.9947 0.5228 0.6258 11.00000 0.05 1.51 Q7 1 1.0964 0.6814 0.7738 11.00000 0.05 1.34 Q8 1 0.8647 0.4216 0.6667 11.00000 0.05 1.33 Q9 1 0.7455 0.5557 0.7713 11.00000 0.05 1.25 Q10 1 1.0912 0.6220 0.6981 11.00000 0.05 1.21 Q11 1 0.7387 0.4745 0.8333 11.00000 0.05 1.19 Q12 1 0.7431 0.4719 0.7708 11.00000 0.05 1.15 Q13 1 0.2331 0.6965 0.5126 11.00000 0.05 1.10 Q14 1 0.1857 0.8606 0.4788 11.00000 0.05 1.06 Q15 1 1.1367 0.6336 0.7365 11.00000 0.05 1.04 Q16 1 0.7834 0.4664 0.6780 11.00000 0.05 1.03 Q17 1 1.1218 0.6224 0.6323 11.00000 0.05 0.96 Q18 1 0.8362 0.6618 0.8549 11.00000 0.05 0.95 Q19 1 0.9638 0.7006 0.8421 11.00000 0.05 0.94 Q20 1 0.7383 0.5578 0.8524 11.00000 0.05 0.90 ; _shelx_res_checksum 94340 _shelx_hkl_file ; 2 0 0 3135.29 91.59 -2 0 0 3178.08 90.99 -2 0 0 3076.79 91.49 -2 0 0 3218.08 91.19 -2 0 0 3277.07 91.69 2 0 0 3171.98 90.99 2 0 0 3338.47 91.79 2 0 0 3149.19 91.29 -3 0 0 4884.31 139.19 3 0 0 4880.21 139.79 -3 0 0 4790.92 139.79 -3 0 0 4726.53 139.39 -3 0 0 4990.40 139.99 3 0 0 4946.10 138.99 3 0 0 4921.01 140.09 4 0 0 1317.77 39.50 4 0 0 1268.17 38.00 4 0 0 1232.58 39.10 -4 0 0 1294.27 37.90 -4 0 0 1222.88 39.20 -4 0 0 1266.67 38.20 -4 0 0 1271.87 39.50 -5 0 0 1246.18 37.50 5 0 0 1218.98 37.30 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-5 27 21.60 30.00 2 -5 27 -20.80 25.60 -2 -5 -27 -23.50 25.40 2 5 27 12.50 29.50 2 5 27 52.39 39.10 -2 5 -27 38.10 29.50 3 -5 27 39.90 31.40 3 5 27 32.40 30.10 3 5 27 22.30 40.00 -3 5 -27 -28.30 32.40 -5 -6 27 3.20 32.40 -5 -6 27 -36.30 29.40 -5 -6 27 -29.70 25.90 5 -6 -27 10.20 27.20 5 -6 -27 14.20 26.50 -5 6 27 -3.10 39.70 -5 6 27 -12.80 24.40 5 6 -27 18.50 29.80 5 6 -27 -6.50 21.10 4 -6 -27 1.90 25.50 -4 -6 27 31.30 37.70 4 -6 -27 35.40 24.90 -4 -6 27 3.10 24.70 -4 -6 27 76.49 31.80 -4 6 27 -0.20 24.30 4 6 -27 45.10 20.30 4 6 -27 48.10 28.50 -4 6 27 68.19 39.30 3 -6 -27 -24.50 23.10 3 -6 -27 60.39 25.80 -3 -6 27 44.50 30.10 -3 -6 27 -24.50 23.90 -3 6 27 4.00 23.60 -3 6 27 129.59 37.50 3 6 -27 44.90 28.00 -3 6 27 19.70 24.20 2 -6 -27 6.50 24.50 -2 -6 27 36.00 29.80 2 -6 -27 -12.60 23.50 -2 -6 27 36.40 25.20 -2 6 27 6.50 22.60 -2 6 27 75.09 38.00 -2 6 27 -6.90 24.20 2 6 -27 77.59 27.90 1 -6 -27 -28.90 23.60 -1 -6 27 12.00 28.70 1 -6 -27 53.59 39.70 -1 -6 27 -2.10 24.10 -1 6 27 -1.00 24.40 1 6 -27 -12.40 26.50 -1 6 27 11.60 21.30 -1 6 27 20.80 38.40 0 -6 27 -34.70 28.20 0 -6 -27 4.00 25.10 0 -6 27 -13.60 24.30 0 6 27 9.70 24.70 0 6 -27 -59.89 26.10 0 6 27 48.30 38.10 -1 -6 -27 58.29 26.60 1 -6 27 67.19 30.80 1 -6 27 7.10 26.30 1 6 27 104.29 41.90 1 6 27 74.99 27.70 -1 6 -27 97.49 30.60 2 -6 27 16.70 30.90 -2 -6 -27 -35.30 25.60 2 -6 27 56.59 28.90 2 6 27 80.79 44.00 -2 6 -27 -43.40 31.20 2 6 27 19.90 29.60 4 -7 -27 89.39 28.40 -4 -7 27 7.00 31.40 -4 -7 27 30.70 27.50 4 -7 -27 44.20 25.70 -4 7 27 18.60 43.30 4 7 -27 35.70 20.80 4 7 -27 43.30 28.50 -4 7 27 25.80 26.00 -3 -7 27 57.59 26.50 3 -7 -27 80.79 27.20 -3 -7 27 40.60 30.60 3 -7 -27 34.70 24.10 -3 7 27 86.79 40.80 3 7 -27 59.49 29.50 -3 7 27 59.89 25.60 -3 7 27 60.49 23.50 -2 -7 27 -15.90 28.90 2 -7 -27 -1.30 25.70 2 -7 -27 -30.70 23.70 -2 -7 27 2.00 25.00 -2 7 27 -19.70 24.20 2 7 -27 1.00 27.40 -2 7 27 71.39 42.30 -2 7 27 -9.30 25.90 -1 -7 27 49.30 25.40 1 -7 -27 59.69 26.80 -1 -7 27 59.89 29.30 1 -7 -27 43.20 26.10 -1 7 27 143.19 42.90 1 7 -27 99.59 29.80 -1 7 27 57.79 26.40 -1 7 27 6.00 23.80 0 -7 -27 -1.60 43.10 0 -7 -27 43.10 26.30 0 -7 27 62.59 29.90 0 -7 27 17.30 25.30 0 7 -27 28.80 29.70 0 7 27 74.59 27.10 0 7 27 103.19 42.60 1 -7 27 49.10 28.70 -1 -7 -27 64.69 27.80 1 -7 27 77.99 28.60 1 7 27 26.10 28.80 -1 7 -27 64.89 32.20 1 7 27 141.69 45.90 -3 -8 27 -39.20 29.40 -3 8 27 80.89 42.30 2 -8 -27 45.50 28.20 2 -8 -27 14.30 25.60 -2 -8 27 15.40 26.70 -2 -8 27 29.30 29.00 2 8 -27 58.69 30.50 -2 8 27 47.80 40.90 -2 8 27 2.80 25.20 -2 8 27 20.90 24.10 1 -8 -27 27.60 25.40 1 -8 -27 59.19 29.20 -1 -8 27 6.20 29.10 -1 -8 27 26.60 26.40 -1 8 27 51.39 26.70 -1 8 27 104.69 44.50 -1 8 27 5.70 26.20 1 8 -27 14.30 29.20 0 -8 -27 -68.49 24.80 0 -8 27 8.10 28.40 0 -8 -27 -61.69 26.70 0 -8 27 9.70 26.40 0 8 27 80.09 29.20 0 8 27 40.00 44.80 0 8 27 -51.79 27.10 0 8 -27 14.70 30.80 -5 0 28 3.00 26.90 -5 0 28 39.40 35.30 -5 0 28 43.90 26.30 5 0 -28 42.60 28.10 5 0 -28 35.20 24.80 -4 0 28 90.79 27.60 4 0 -28 83.09 23.90 -4 0 28 128.89 38.20 -4 0 28 41.10 25.80 4 0 -28 122.79 29.90 -3 0 28 51.39 25.70 -3 0 28 113.69 35.20 3 0 -28 99.39 29.60 -3 0 28 66.49 22.80 -2 0 28 35.90 26.20 -2 0 28 2.80 35.00 2 0 -28 43.70 27.50 -1 0 28 42.20 34.60 1 0 -28 -3.60 27.20 -1 0 28 72.29 26.80 0 0 28 276.87 39.30 0 0 -28 211.28 32.80 -1 0 -28 87.09 27.50 1 0 28 51.79 27.50 1 0 28 131.69 36.40 2 0 28 59.39 28.40 -2 0 -28 66.39 31.60 2 0 28 94.99 38.40 5 -1 -28 171.28 32.30 -5 -1 28 178.28 32.10 -5 -1 28 168.38 31.20 5 -1 -28 158.78 29.00 -5 -1 28 131.99 38.10 -5 1 28 144.29 28.80 -5 1 28 152.28 40.10 5 1 -28 167.48 26.80 -5 1 28 208.88 31.20 5 1 -28 142.09 31.60 -4 -1 28 46.20 27.00 4 -1 -28 98.59 24.80 4 -1 -28 37.60 27.70 -4 -1 28 61.99 36.10 -4 -1 28 55.39 26.20 -4 1 28 17.00 24.30 4 1 -28 2.20 26.50 4 1 -28 92.09 24.20 -4 1 28 72.49 36.90 -4 1 28 79.49 26.10 3 -1 -28 -36.50 26.20 -3 -1 28 41.00 34.80 -3 -1 28 67.19 26.50 3 -1 -28 66.79 23.30 -3 1 28 45.70 26.50 3 1 -28 32.30 28.40 -3 1 28 141.09 37.30 -3 1 28 41.60 23.00 -2 -1 28 15.20 27.30 -2 -1 28 42.90 34.40 2 -1 -28 32.10 27.20 2 1 -28 -15.40 25.70 -2 1 28 -45.10 24.60 -2 1 28 51.49 36.20 -1 -1 28 37.00 25.90 -1 -1 28 -17.80 33.80 1 -1 -28 8.40 26.90 -1 1 28 73.89 36.20 1 1 -28 -1.30 28.30 -1 1 28 21.90 26.70 0 -1 -28 -30.10 26.90 0 -1 28 -0.40 26.30 0 -1 28 58.09 35.10 0 1 -28 -36.60 27.00 0 1 28 41.70 35.70 0 1 28 -12.70 26.20 1 -1 28 34.10 36.10 1 -1 28 24.80 25.60 -1 -1 -28 13.70 26.70 1 1 28 26.90 26.60 -1 1 -28 -35.10 29.30 1 1 28 1.30 36.40 2 -1 28 -19.50 26.50 2 -1 28 75.79 37.40 -2 -1 -28 14.30 27.70 -2 1 -28 1.30 28.30 2 1 28 51.59 38.90 2 1 28 66.09 30.40 -5 -2 28 -20.40 36.10 5 2 -28 28.50 23.90 -5 2 28 52.39 37.20 5 2 -28 29.90 29.50 -4 -2 28 40.60 27.00 4 -2 -28 52.79 25.50 -4 -2 28 63.99 25.80 4 -2 -28 44.70 28.60 -4 -2 28 137.59 37.60 -4 2 28 90.59 27.00 -4 2 28 1.80 37.50 4 2 -28 74.19 29.10 -4 2 28 45.60 28.10 -3 -2 28 133.79 35.00 -3 -2 28 63.39 27.10 3 -2 -28 126.09 30.60 3 2 -28 121.99 28.50 -3 2 28 79.09 26.20 -3 2 28 109.59 26.70 -3 2 28 133.09 38.60 -2 -2 28 20.50 34.80 2 -2 -28 -12.10 26.30 -2 -2 28 -18.90 25.00 2 2 -28 38.70 28.10 -2 2 28 -28.90 24.30 -2 2 28 23.60 37.50 1 -2 -28 -3.50 27.30 -1 -2 28 117.79 35.40 -1 -2 28 31.20 26.40 1 2 -28 34.30 27.40 -1 2 28 3.70 25.80 -1 2 28 110.09 39.30 0 -2 -28 8.10 26.20 0 -2 28 68.79 34.80 0 -2 28 72.99 26.80 0 2 28 55.89 26.70 0 2 28 40.80 37.90 0 2 -28 92.29 29.30 -1 -2 -28 45.30 27.70 1 -2 28 114.29 29.40 1 -2 28 78.29 35.50 1 2 28 115.39 31.00 1 2 28 94.29 40.50 -1 2 -28 38.80 30.10 -2 -2 -28 69.59 30.20 2 -2 28 74.19 35.90 2 -2 28 -24.10 28.80 -2 2 -28 46.20 30.10 2 2 28 22.90 29.50 2 2 28 3.90 39.60 -4 -3 28 35.00 27.80 -4 -3 28 73.79 33.70 4 -3 -28 51.09 25.40 4 -3 -28 49.70 29.20 -4 3 28 83.59 28.70 -4 3 28 39.70 26.20 -4 3 28 85.89 39.70 4 3 -28 110.39 29.60 -3 -3 28 24.00 25.70 3 -3 -28 -22.90 26.20 3 -3 -28 55.69 24.80 -3 -3 28 24.70 33.40 -3 3 28 41.60 37.40 3 3 -28 14.70 27.80 -3 3 28 29.20 25.80 -3 3 28 3.50 24.20 -2 -3 28 44.40 26.30 -2 -3 28 92.09 34.60 2 -3 -28 26.30 27.10 -2 3 28 12.90 37.60 2 3 -28 11.70 26.80 -2 3 28 30.90 26.50 -1 -3 28 93.29 33.70 -1 -3 28 -11.50 27.40 1 -3 -28 -12.30 25.60 1 3 -28 42.40 28.70 -1 3 28 7.10 24.60 -1 3 28 -44.50 36.60 0 -3 -28 -38.90 25.40 0 -3 28 -3.20 25.50 0 -3 28 14.80 32.40 0 3 28 -29.70 37.10 0 3 -28 -14.10 28.40 0 3 28 9.70 27.00 1 -3 28 32.40 27.70 -1 -3 -28 39.40 27.80 1 -3 28 -82.69 32.20 1 3 28 -4.30 29.20 -1 3 -28 22.30 29.20 1 3 28 48.40 40.00 2 -3 28 10.60 34.10 2 3 28 107.69 40.70 -4 -4 28 13.90 34.60 -4 -4 28 20.20 26.80 4 -4 -28 36.30 27.70 4 -4 -28 45.10 26.20 -4 4 28 18.60 26.40 -4 4 28 61.39 26.50 4 4 -28 51.09 24.50 4 4 -28 31.50 29.20 -4 4 28 -56.89 39.50 3 -4 -28 -39.30 26.00 -3 -4 28 21.10 26.70 -3 -4 28 7.50 33.70 3 -4 -28 -8.80 24.20 -3 4 28 37.60 24.70 3 4 -28 -20.00 28.90 -3 4 28 51.99 26.40 -3 4 28 19.40 39.20 -2 -4 28 19.00 33.70 -2 -4 28 22.00 26.10 2 -4 -28 -0.20 25.10 -2 4 28 82.89 41.10 -2 4 28 21.30 22.10 2 4 -28 31.90 27.00 -2 4 28 94.89 27.30 -1 -4 28 114.19 35.50 -1 -4 28 39.70 26.80 1 -4 -28 17.70 26.20 1 4 -28 117.89 29.60 -1 4 28 132.09 41.80 -1 4 28 63.09 27.20 0 -4 28 116.99 33.90 0 -4 28 111.19 28.90 0 -4 -28 52.29 26.90 0 4 -28 73.89 30.40 0 4 28 96.19 28.00 0 4 28 56.09 40.90 1 -4 28 18.90 29.00 -1 -4 -28 46.60 28.00 1 -4 28 15.60 34.20 -1 4 -28 -0.40 32.20 1 4 28 29.50 40.70 1 4 28 22.70 29.10 -3 -5 28 140.89 36.40 3 -5 -28 104.09 27.80 -3 -5 28 96.39 28.40 3 -5 -28 145.79 28.10 -3 5 28 165.28 42.20 -3 5 28 41.40 26.30 3 5 -28 53.29 29.40 -3 5 28 108.69 29.30 -2 -5 28 110.79 27.40 2 -5 -28 56.09 27.30 -2 -5 28 71.49 33.60 2 -5 -28 116.89 27.20 -2 5 28 42.20 42.60 -2 5 28 95.59 27.30 2 5 -28 81.09 29.40 -2 5 28 32.70 24.30 -1 -5 28 65.29 33.40 -1 -5 28 88.39 27.90 1 -5 -28 11.80 27.00 1 5 -28 85.09 29.90 -1 5 28 155.88 43.60 -1 5 28 -1.20 26.30 0 -5 28 -23.00 27.40 0 -5 -28 7.90 27.10 0 -5 28 -20.10 32.40 0 5 28 49.10 41.70 0 5 -28 12.20 30.40 0 5 28 -45.10 26.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 8677 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.52292(7) 0.74343(4) 0.55188(4) 0.0183(2) Uani 1 1 d D . . . . Si1 Si 0.7774(2) 0.71645(15) 0.55614(11) 0.0342(5) Uani 1 1 d D . . . . Si2 Si 0.63034(18) 0.63714(12) 0.46532(10) 0.0218(5) Uani 1 1 d . . . . . Si3 Si 0.4474(5) 0.8521(3) 0.4548(3) 0.0342(5) Uani 0.5 1 d D U P A 1 N1 N 0.546(4) 0.8117(11) 0.6251(7) 0.0271(14) Uani 0.5 1 d D U P B 1 N2 N 0.482(5) 0.6742(10) 0.6191(7) 0.022(6) Uani 0.5 1 d D U P B 1 N3 N 0.6526(5) 0.7013(4) 0.5184(3) 0.0271(14) Uani 1 1 d . . . . . N4 N 0.3973(7) 0.7853(4) 0.5027(3) 0.0367(15) Uani 1 1 d D U . . . C1 C 0.552(2) 0.8861(9) 0.6194(8) 0.024(2) Uani 0.5 1 d D U P B 1 H1 H 0.548878 0.906297 0.581014 0.029 Uiso 0.5 1 calc R U P B 1 C2 C 0.5620(17) 0.9322(9) 0.6669(7) 0.024(3) Uani 0.5 1 d D U P B 1 H2 H 0.567923 0.983286 0.662644 0.029 Uiso 0.5 1 calc R U P B 1 C3 C 0.563(3) 0.8988(11) 0.7217(8) 0.031(3) Uani 0.5 1 d D U P B 1 H3 H 0.584123 0.926196 0.756183 0.038 Uiso 0.5 1 calc R U P B 1 C4 C 0.533(4) 0.8267(11) 0.7273(8) 0.030(6) Uani 0.5 1 d D U P B 1 H4 H 0.521117 0.807822 0.765003 0.036 Uiso 0.5 1 calc R U P B 1 C5 C 0.519(6) 0.7803(13) 0.6766(9) 0.025(7) Uani 0.5 1 d D U P B 1 C16 C 0.4818(7) 0.6239(5) 0.4411(4) 0.035(2) Uani 1 1 d . . . . . H16A H 0.443879 0.605753 0.474197 0.053 Uiso 1 1 calc GR . . . . H16B H 0.473941 0.588689 0.408859 0.053 Uiso 1 1 calc GR . . . . H16C H 0.449204 0.670263 0.427644 0.053 Uiso 1 1 calc GR . . . . C17 C 0.6948(10) 0.6595(6) 0.3957(4) 0.047(3) Uani 1 1 d . . . . . H17A H 0.657565 0.701752 0.376758 0.071 Uiso 1 1 calc GR . . . . H17B H 0.687131 0.617966 0.368836 0.071 Uiso 1 1 calc GR . . . . H17C H 0.773062 0.670556 0.405172 0.071 Uiso 1 1 calc GR . . . . C18 C 0.6814(8) 0.5451(5) 0.4889(4) 0.035(2) Uani 1 1 d . . . . . H18A H 0.760299 0.547656 0.501801 0.052 Uiso 1 1 calc GR . . . . H18B H 0.669311 0.511288 0.455827 0.052 Uiso 1 1 calc GR . . . . H18C H 0.641312 0.528094 0.521564 0.052 Uiso 1 1 calc GR . . . . C21 C 0.7870(10) 0.6798(7) 0.6318(6) 0.069(3) Uani 1 1 d . . . . . H21A H 0.736290 0.706212 0.654919 0.103 Uiso 1 1 calc GR . . . . H21B H 0.862582 0.685419 0.650100 0.103 Uiso 1 1 calc GR . . . . H21C H 0.767362 0.628214 0.630532 0.103 Uiso 1 1 calc GR . . . . C22 C 0.8148(10) 0.8146(7) 0.5621(6) 0.069(3) Uani 1 1 d . . . . . H22A H 0.810682 0.836044 0.522629 0.103 Uiso 1 1 calc GR . . . . H22B H 0.889898 0.819555 0.581071 0.103 Uiso 1 1 calc GR . . . . H22C H 0.763292 0.839740 0.585592 0.103 Uiso 1 1 calc GR . . . . C23 C 0.5977(17) 0.8629(14) 0.4567(11) 0.058(3) Uani 0.5 1 d D U P A 1 H23A H 0.626139 0.884116 0.494521 0.087 Uiso 0.5 1 calc GR . P A 1 H23B H 0.615156 0.894963 0.424655 0.087 Uiso 0.5 1 calc GR . P A 1 H23C H 0.631912 0.815404 0.452084 0.087 Uiso 0.5 1 calc GR . P A 1 C24 C 0.400(2) 0.8158(11) 0.3761(8) 0.058(3) Uani 0.5 1 d D U P A 1 H24A H 0.454304 0.781343 0.363812 0.087 Uiso 0.5 1 calc GR . P A 1 H24B H 0.392354 0.856432 0.348342 0.087 Uiso 0.5 1 calc GR . P A 1 H24C H 0.328376 0.791337 0.376641 0.087 Uiso 0.5 1 calc GR . P A 1 C25 C 0.380(2) 0.9412(11) 0.4573(10) 0.058(3) Uani 0.5 1 d D U P A 1 H25A H 0.303252 0.937305 0.440114 0.087 Uiso 0.5 1 calc GR . P A 1 H25B H 0.419042 0.976485 0.434804 0.087 Uiso 0.5 1 calc GR . P A 1 H25C H 0.381136 0.957388 0.498243 0.087 Uiso 0.5 1 calc GR . P A 1 C28 C 0.2326(19) 0.7976(14) 0.5885(9) 0.039(6) Uani 0.5 1 d D U P A -2 H28A H 0.283004 0.776864 0.620080 0.059 Uiso 0.5 1 calc GR . P A -2 H28B H 0.156511 0.785225 0.595059 0.059 Uiso 0.5 1 calc GR . P A -2 H28C H 0.240987 0.850450 0.588230 0.059 Uiso 0.5 1 calc GR . P A -2 Si6 Si 0.2654(9) 0.7599(8) 0.5162(6) 0.049(2) Uani 0.5 1 d D U P A -2 C6 C 0.4782(19) 0.7082(9) 0.6744(7) 0.024(3) Uani 0.5 1 d D U P B 1 C7 C 0.4353(15) 0.6668(8) 0.7190(7) 0.024(2) Uani 0.5 1 d D U P B 1 H7 H 0.428774 0.689217 0.755930 0.029 Uiso 0.5 1 calc R U P B 1 C8 C 0.4028(14) 0.5962(8) 0.7118(6) 0.026(3) Uani 0.5 1 d D U P B 1 H8 H 0.372854 0.570490 0.742699 0.031 Uiso 0.5 1 calc R U P B 1 C9 C 0.4147(16) 0.5625(8) 0.6574(6) 0.028(3) Uani 0.5 1 d D U P B 1 H9 H 0.399333 0.512427 0.651221 0.034 Uiso 0.5 1 calc R U P B 1 C10 C 0.4494(16) 0.6050(9) 0.6140(7) 0.024(2) Uani 0.5 1 d D U P B 1 H10 H 0.450797 0.583362 0.576354 0.029 Uiso 0.5 1 calc R U P B 1 C20 C 0.8976(15) 0.6561(13) 0.5361(13) 0.050(6) Uani 0.5 1 d D . P C 1 H20A H 0.964930 0.669554 0.560611 0.075 Uiso 0.5 1 calc GR . P C 1 H20B H 0.908818 0.663004 0.494557 0.075 Uiso 0.5 1 calc GR . P C 1 H20C H 0.880125 0.605136 0.543087 0.075 Uiso 0.5 1 calc GR . P C 1 C27 C 0.242(2) 0.6590(11) 0.5179(11) 0.055(3) Uani 0.5 1 d D U P A -2 H27A H 0.270060 0.636576 0.483487 0.083 Uiso 0.5 1 calc GR . P A -2 H27B H 0.162338 0.649332 0.517156 0.083 Uiso 0.5 1 calc GR . P A -2 H27C H 0.279694 0.638654 0.553872 0.083 Uiso 0.5 1 calc GR . P A -2 C30 C 0.150(2) 0.7888(19) 0.4622(12) 0.075(7) Uani 0.5 1 d D U P A -2 H30A H 0.148840 0.841819 0.459253 0.112 Uiso 0.5 1 calc GR . P A -2 H30B H 0.079822 0.771893 0.475240 0.112 Uiso 0.5 1 calc GR . P A -2 H30C H 0.159646 0.767853 0.423561 0.112 Uiso 0.5 1 calc GR . P A -2 C19 C 0.8961(15) 0.6954(15) 0.5093(9) 0.044(6) Uani 0.5 1 d D . P C 2 H19A H 0.904742 0.642747 0.506105 0.066 Uiso 0.5 1 calc GR . P C 2 H19B H 0.964501 0.716559 0.527877 0.066 Uiso 0.5 1 calc GR . P C 2 H19C H 0.879727 0.716175 0.469899 0.066 Uiso 0.5 1 calc GR . P C 2 K1 K 0.92675(19) 0.55532(12) 0.72855(10) 0.0407(5) Uani 1 1 d . . . . . O1 O 1.0222(17) 0.4912(16) 0.8351(10) 0.119(8) Uani 0.5 1 d D U P D 1 C31 C 0.923(2) 0.511(2) 0.9226(16) 0.117(6) Uani 0.5 1 d D U P D 1 H31A H 0.883298 0.540135 0.891193 0.175 Uiso 0.5 1 calc GR . P D 1 H31B H 0.945968 0.543064 0.955994 0.175 Uiso 0.5 1 calc GR . P D 1 H31C H 0.874096 0.473418 0.935309 0.175 Uiso 0.5 1 calc GR . P D 1 C32 C 1.011(3) 0.481(3) 0.9026(15) 0.117(6) Uani 0.5 1 d D U P D 1 H32A H 1.010028 0.428452 0.911173 0.140 Uiso 0.5 1 calc R . P D 1 H32B H 1.077874 0.501548 0.924751 0.140 Uiso 0.5 1 calc R . P D 1 C33 C 1.133(3) 0.460(2) 0.8176(18) 0.117(6) Uani 0.5 1 d D U P D 1 H33A H 1.187892 0.499401 0.817831 0.140 Uiso 0.5 1 calc R . P D 1 H33B H 1.161262 0.423739 0.847633 0.140 Uiso 0.5 1 calc R . P D 1 C34 C 1.125(3) 0.427(2) 0.7638(16) 0.117(6) Uani 0.5 1 d D U P D 1 H34A H 1.054356 0.440342 0.742206 0.175 Uiso 0.5 1 calc GR . P D 1 H34B H 1.128773 0.374467 0.768745 0.175 Uiso 0.5 1 calc GR . P D 1 H34C H 1.185461 0.443560 0.741727 0.175 Uiso 0.5 1 calc GR . P D 1 O2 O 1.0543(15) 0.4670(8) 0.7976(7) 0.057(4) Uani 0.5 1 d D U P D 2 C35 C 1.115(3) 0.4842(16) 0.8523(12) 0.077(5) Uani 0.5 1 d D U P D 2 H35A H 1.163892 0.442610 0.864095 0.093 Uiso 0.5 1 calc R . P D 2 H35B H 1.163537 0.526203 0.845966 0.093 Uiso 0.5 1 calc R . P D 2 C36 C 1.059(3) 0.499(2) 0.8948(13) 0.099(11) Uani 0.5 1 d D U P D 2 H36A H 1.035667 0.550085 0.892130 0.149 Uiso 0.5 1 calc GR . P D 2 H36B H 1.103493 0.491068 0.932196 0.149 Uiso 0.5 1 calc GR . P D 2 H36C H 0.993499 0.467912 0.892794 0.149 Uiso 0.5 1 calc GR . P D 2 C37 C 1.138(2) 0.3572(12) 0.7656(11) 0.059(5) Uani 0.5 1 d D U P D 2 H37A H 1.205398 0.344102 0.790508 0.088 Uiso 0.5 1 calc GR . P D 2 H37B H 1.158291 0.386458 0.732296 0.088 Uiso 0.5 1 calc GR . P D 2 H37C H 1.100618 0.313048 0.750824 0.088 Uiso 0.5 1 calc GR . P D 2 C38 C 1.078(3) 0.3919(13) 0.7940(12) 0.077(5) Uani 0.5 1 d D U P D 2 H38A H 1.101308 0.377906 0.835242 0.093 Uiso 0.5 1 calc R . P D 2 H38B H 1.005055 0.369132 0.784628 0.093 Uiso 0.5 1 calc R . P D 2 O3 O 0.7378(15) 0.4827(9) 0.7293(8) 0.0751(14) Uani 0.5 1 d D U P D 3 O6 O 0.8902(13) 0.4267(10) 0.6617(8) 0.0751(14) Uani 0.5 1 d D U P D 3 O8 O 1.0683(13) 0.5212(9) 0.6451(8) 0.0751(14) Uani 0.5 1 d D U P D 3 O10 O 1.1250(15) 0.6298(9) 0.7233(8) 0.0751(14) Uani 0.5 1 d D U P D 3 O12 O 0.9665(14) 0.6872(13) 0.7882(9) 0.0751(14) Uani 0.5 1 d D U P D 3 O14 O 0.7843(14) 0.6003(9) 0.8047(8) 0.0751(14) Uani 0.5 1 d D U P D 3 C41 C 0.914(2) 0.6950(19) 0.8403(11) 0.087(3) Uani 0.5 1 d D U P D 3 H41A H 0.918088 0.746056 0.853717 0.104 Uiso 0.5 1 calc R . P D 3 H41B H 0.950740 0.664068 0.871786 0.104 Uiso 0.5 1 calc R . P D 3 C45 C 1.0762(15) 0.7115(13) 0.7968(9) 0.057(5) Uani 0.5 1 d D U P D 3 H45A H 1.115883 0.683899 0.829454 0.069 Uiso 0.5 1 calc R . P D 3 H45B H 1.077130 0.763406 0.808083 0.069 Uiso 0.5 1 calc R . P D 3 C46 C 1.134(2) 0.7022(12) 0.7422(11) 0.056(5) Uani 0.5 1 d D U P D 3 H46A H 1.100456 0.734615 0.710839 0.068 Uiso 0.5 1 calc R . P D 3 H46B H 1.212583 0.715383 0.750305 0.068 Uiso 0.5 1 calc R . P D 3 C47 C 1.190(2) 0.6172(11) 0.6773(11) 0.073(6) Uani 0.5 1 d D U P D 3 H47A H 1.267577 0.629064 0.690220 0.087 Uiso 0.5 1 calc R . P D 3 H47B H 1.165367 0.649113 0.643662 0.087 Uiso 0.5 1 calc R . P D 3 C48 C 1.1815(14) 0.5381(9) 0.6577(9) 0.052(4) Uani 0.5 1 d D U P D 3 H48A H 1.221002 0.530839 0.622165 0.063 Uiso 0.5 1 calc R . P D 3 H48B H 1.215099 0.506070 0.689265 0.063 Uiso 0.5 1 calc R . P D 3 C49 C 1.0609(18) 0.4500(12) 0.6215(13) 0.084(7) Uani 0.5 1 d D U P D 3 H49A H 1.095695 0.414867 0.650349 0.101 Uiso 0.5 1 calc R . P D 3 H49B H 1.099194 0.447360 0.585223 0.101 Uiso 0.5 1 calc R . P D 3 C50 C 0.940(2) 0.433(2) 0.6080(11) 0.087(3) Uani 0.5 1 d D U P D 3 H50A H 0.903032 0.471759 0.583487 0.104 Uiso 0.5 1 calc R . P D 3 H50B H 0.930812 0.386653 0.585771 0.104 Uiso 0.5 1 calc R . P D 3 C59 C 0.7935(17) 0.6718(12) 0.8265(13) 0.087(3) Uani 0.5 1 d D U P D 3 H59A H 0.755108 0.675335 0.862697 0.104 Uiso 0.5 1 calc R . P D 3 H59B H 0.756697 0.705356 0.796979 0.104 Uiso 0.5 1 calc R . P D 3 C60 C 0.6757(16) 0.5820(12) 0.7858(13) 0.083(7) Uani 0.5 1 d D U P D 3 H60A H 0.650284 0.611080 0.750605 0.099 Uiso 0.5 1 calc R . P D 3 H60B H 0.627589 0.593374 0.817152 0.099 Uiso 0.5 1 calc R . P D 3 C62 C 0.667(2) 0.5015(13) 0.7708(13) 0.095(8) Uani 0.5 1 d D U P D 3 H62A H 0.685414 0.472670 0.806983 0.113 Uiso 0.5 1 calc R . P D 3 H62B H 0.590525 0.489950 0.755460 0.113 Uiso 0.5 1 calc R . P D 3 C65 C 0.725(3) 0.4111(14) 0.7094(14) 0.068(7) Uani 0.5 1 d D U P D 3 H65A H 0.645725 0.399034 0.702060 0.081 Uiso 0.5 1 calc R . P D 3 H65B H 0.759135 0.377186 0.739466 0.081 Uiso 0.5 1 calc R . P D 3 C67 C 0.7807(17) 0.4040(16) 0.6527(10) 0.070(6) Uani 0.5 1 d D U P D 3 H67A H 0.777847 0.352845 0.639460 0.084 Uiso 0.5 1 calc R . P D 3 H67B H 0.740913 0.433941 0.621557 0.084 Uiso 0.5 1 calc R . P D 3 O4 O 0.7481(16) 0.5023(9) 0.7839(7) 0.0751(14) Uani 0.5 1 d D U P D 4 O5 O 0.8211(14) 0.4213(11) 0.6895(7) 0.0751(14) Uani 0.5 1 d D U P D 4 O7 O 0.9665(13) 0.4808(9) 0.6186(8) 0.0751(14) Uani 0.5 1 d D U P D 4 O9 O 1.1073(16) 0.5918(9) 0.6618(7) 0.0751(14) Uani 0.5 1 d D U P D 4 O11 O 1.0326(14) 0.6839(10) 0.7466(7) 0.0751(14) Uani 0.5 1 d D U P D 4 O13 O 0.8683(14) 0.6249(9) 0.8208(8) 0.0751(14) Uani 0.5 1 d D U P D 4 C39 C 0.739(3) 0.5345(12) 0.8367(10) 0.087(3) Uani 0.5 1 d D U P D 4 H39A H 0.781761 0.505932 0.867528 0.104 Uiso 0.5 1 calc R . P D 4 H39B H 0.660310 0.532133 0.844931 0.104 Uiso 0.5 1 calc R . P D 4 C40 C 0.774(2) 0.6087(12) 0.8416(13) 0.087(3) Uani 0.5 1 d D U P D 4 H40A H 0.715711 0.639353 0.821136 0.104 Uiso 0.5 1 calc R . P D 4 H40B H 0.779666 0.622233 0.883791 0.104 Uiso 0.5 1 calc R . P D 4 C51 C 1.0676(19) 0.4886(12) 0.6012(13) 0.081(7) Uani 0.5 1 d D U P D 4 H51A H 1.067217 0.474112 0.559431 0.097 Uiso 0.5 1 calc R . P D 4 H51B H 1.119862 0.456728 0.624974 0.097 Uiso 0.5 1 calc R . P D 4 C52 C 1.102(2) 0.5628(12) 0.6081(9) 0.077(6) Uani 0.5 1 d D U P D 4 H52A H 1.176590 0.566907 0.594034 0.092 Uiso 0.5 1 calc R . P D 4 H52B H 1.051908 0.592921 0.581716 0.092 Uiso 0.5 1 calc R . P D 4 C53 C 1.136(3) 0.6608(12) 0.6675(10) 0.086(7) Uani 0.5 1 d D U P D 4 H53A H 1.088721 0.689307 0.638242 0.103 Uiso 0.5 1 calc R . P D 4 H53B H 1.212824 0.665772 0.657511 0.103 Uiso 0.5 1 calc R . P D 4 C55 C 1.129(2) 0.6931(16) 0.7251(12) 0.067(7) Uani 0.5 1 d D U P D 4 H55A H 1.187002 0.672011 0.753073 0.080 Uiso 0.5 1 calc R . P D 4 H55B H 1.143093 0.745779 0.722509 0.080 Uiso 0.5 1 calc R . P D 4 C56 C 1.004(2) 0.7049(17) 0.7975(11) 0.080(7) Uani 0.5 1 d D U P D 4 H56A H 1.020600 0.757387 0.800966 0.096 Uiso 0.5 1 calc R . P D 4 H56B H 1.054187 0.680171 0.827989 0.096 Uiso 0.5 1 calc R . P D 4 C57 C 0.894(2) 0.6946(12) 0.8129(16) 0.102(8) Uani 0.5 1 d D U P D 4 H57A H 0.884522 0.721650 0.849541 0.122 Uiso 0.5 1 calc R . P D 4 H57B H 0.841634 0.715132 0.781341 0.122 Uiso 0.5 1 calc R . P D 4 C63 C 0.737(2) 0.4322(11) 0.7785(10) 0.077(6) Uani 0.5 1 d D U P D 4 H63A H 0.668133 0.417517 0.794906 0.092 Uiso 0.5 1 calc R . P D 4 H63B H 0.799025 0.408593 0.802572 0.092 Uiso 0.5 1 calc R . P D 4 C64 C 0.735(3) 0.4053(19) 0.7191(13) 0.076(8) Uani 0.5 1 d D U P D 4 H64A H 0.727294 0.351866 0.720300 0.091 Uiso 0.5 1 calc R . P D 4 H64B H 0.667540 0.424491 0.696547 0.091 Uiso 0.5 1 calc R . P D 4 C68 C 0.815(2) 0.4070(18) 0.6329(9) 0.082(7) Uani 0.5 1 d D U P D 4 H68A H 0.758425 0.438383 0.612238 0.098 Uiso 0.5 1 calc R . P D 4 H68B H 0.791630 0.356004 0.626623 0.098 Uiso 0.5 1 calc R . P D 4 C69 C 0.918(2) 0.4174(13) 0.6069(10) 0.064(5) Uani 0.5 1 d D U P D 4 H69A H 0.969264 0.378272 0.620773 0.076 Uiso 0.5 1 calc R . P D 4 H69B H 0.903055 0.412470 0.563648 0.076 Uiso 0.5 1 calc R . P D 4 C23A C 0.347(2) 0.9376(11) 0.4747(10) 0.058(3) Uani 0.5 1 d D . P A 2 H23D H 0.267849 0.932980 0.478513 0.087 Uiso 0.5 1 calc GR . P A 2 H23E H 0.358994 0.974975 0.445474 0.087 Uiso 0.5 1 calc GR . P A 2 H23F H 0.385121 0.951426 0.512824 0.087 Uiso 0.5 1 calc GR . P A 2 C24A C 0.5579(18) 0.8689(14) 0.4442(11) 0.058(3) Uani 0.5 1 d D . P A 2 H24D H 0.592734 0.883638 0.482828 0.087 Uiso 0.5 1 calc GR . P A 2 H24E H 0.563964 0.908422 0.415952 0.087 Uiso 0.5 1 calc GR . P A 2 H24F H 0.594908 0.825657 0.430778 0.087 Uiso 0.5 1 calc GR . P A 2 Si3A Si 0.4031(4) 0.8473(3) 0.4503(3) 0.0342(5) Uani 0.5 1 d D . P A 2 C25A C 0.346(2) 0.8328(12) 0.3736(8) 0.058(3) Uani 0.5 1 d D . P A 2 H25D H 0.377255 0.788338 0.358418 0.087 Uiso 0.5 1 calc GR . P A 2 H25E H 0.365285 0.874163 0.349477 0.087 Uiso 0.5 1 calc GR . P A 2 H25F H 0.265911 0.828355 0.371943 0.087 Uiso 0.5 1 calc GR . P A 2 C27A C 0.242(2) 0.6727(11) 0.5345(11) 0.055(3) Uani 0.5 1 d D . P A -1 H27D H 0.250706 0.648640 0.496909 0.083 Uiso 0.5 1 calc GR . P A -1 H27E H 0.166234 0.665731 0.544682 0.083 Uiso 0.5 1 calc GR . P A -1 H27F H 0.293610 0.651742 0.565319 0.083 Uiso 0.5 1 calc GR . P A -1 Si6A Si 0.2706(9) 0.7731(9) 0.5276(6) 0.049(2) Uani 0.5 1 d D . P A -1 C28A C 0.2644(19) 0.8178(13) 0.6018(9) 0.037(6) Uani 0.5 1 d D . P A -1 H28D H 0.318564 0.795025 0.630568 0.056 Uiso 0.5 1 calc GR . P A -1 H28E H 0.190436 0.811834 0.614566 0.056 Uiso 0.5 1 calc GR . P A -1 H28F H 0.281153 0.869531 0.598708 0.056 Uiso 0.5 1 calc GR . P A -1 C30A C 0.147(2) 0.8032(19) 0.4799(12) 0.075(7) Uani 0.5 1 d D . P A -1 H30D H 0.153581 0.855188 0.471675 0.112 Uiso 0.5 1 calc GR . P A -1 H30E H 0.081144 0.794400 0.499981 0.112 Uiso 0.5 1 calc GR . P A -1 H30F H 0.142598 0.776090 0.442842 0.112 Uiso 0.5 1 calc GR . P A -1 N1A N 0.544(5) 0.8122(10) 0.6250(6) 0.0367(15) Uani 0.5 1 d D U P B 2 N2A N 0.499(5) 0.6713(10) 0.6196(7) 0.018(6) Uani 0.5 1 d D U P B 2 C1A C 0.5800(16) 0.8818(9) 0.6306(8) 0.028(4) Uani 0.5 1 d D U P B 2 H1A H 0.601739 0.904766 0.596296 0.034 Uiso 0.5 1 calc R U P B 2 C2A C 0.5878(17) 0.9220(9) 0.6816(7) 0.024(3) Uani 0.5 1 d D U P B 2 H2A H 0.606328 0.972056 0.680815 0.029 Uiso 0.5 1 calc R U P B 2 C3A C 0.568(4) 0.8888(11) 0.7343(8) 0.031(3) Uani 0.5 1 d D U P B 2 H3A H 0.569120 0.915775 0.769800 0.038 Uiso 0.5 1 calc R U P B 2 C4A C 0.548(4) 0.8152(12) 0.7330(8) 0.032(6) Uani 0.5 1 d D U P B 2 H4A H 0.542443 0.789212 0.768508 0.038 Uiso 0.5 1 calc R U P B 2 C5A C 0.536(6) 0.7782(12) 0.6776(7) 0.022(6) Uani 0.5 1 d D U P B 2 C6A C 0.5137(16) 0.7035(8) 0.6752(6) 0.024(5) Uani 0.5 1 d D U P B 2 C7A C 0.5118(17) 0.6618(8) 0.7261(6) 0.031(4) Uani 0.5 1 d D U P B 2 H7A H 0.517537 0.684368 0.763655 0.037 Uiso 0.5 1 calc R U P B 2 C8A C 0.5016(15) 0.5885(8) 0.7215(6) 0.028(3) Uani 0.5 1 d D U P B 2 H8A H 0.500799 0.559256 0.755692 0.034 Uiso 0.5 1 calc R U P B 2 C9A C 0.4922(15) 0.5568(8) 0.6654(6) 0.024(3) Uani 0.5 1 d D U P B 2 H9A H 0.485169 0.505643 0.661303 0.028 Uiso 0.5 1 calc R U P B 2 C10A C 0.4932(14) 0.5993(7) 0.6171(6) 0.019(4) Uani 0.5 1 d D U P B 2 H10A H 0.489403 0.576615 0.579562 0.023 Uiso 0.5 1 calc R U P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0255(5) 0.0109(4) 0.0204(4) -0.0023(4) 0.0110(3) -0.0028(4) Si1 0.0285(13) 0.0410(12) 0.0335(11) -0.0175(9) 0.0052(10) -0.0049(11) Si2 0.0263(12) 0.0177(11) 0.0217(11) -0.0086(9) 0.0048(9) -0.0028(9) Si3 0.0285(13) 0.0410(12) 0.0335(11) -0.0175(9) 0.0052(10) -0.0049(11) N1 0.023(3) 0.025(3) 0.037(4) -0.018(3) 0.017(3) -0.011(3) N2 0.026(16) 0.022(6) 0.020(7) -0.002(5) 0.003(7) 0.002(7) N3 0.023(3) 0.025(3) 0.037(4) -0.018(3) 0.017(3) -0.011(3) N4 0.052(4) 0.032(3) 0.028(3) 0.002(3) 0.014(3) 0.018(3) C1 0.029(6) 0.026(3) 0.019(4) -0.007(3) 0.006(4) -0.001(4) C2 0.024(7) 0.022(4) 0.026(5) -0.006(3) 0.000(4) 0.008(4) C3 0.044(6) 0.028(5) 0.020(5) -0.012(4) -0.007(6) 0.008(5) C4 0.043(14) 0.025(7) 0.020(7) -0.001(5) -0.008(8) 0.018(8) C5 0.023(17) 0.022(6) 0.031(7) -0.008(5) 0.008(8) 0.007(7) C16 0.029(5) 0.028(5) 0.045(6) -0.009(4) -0.015(4) 0.001(4) C17 0.071(8) 0.039(6) 0.035(6) -0.006(5) 0.022(5) -0.005(5) C18 0.041(5) 0.028(5) 0.035(5) -0.008(4) -0.001(4) 0.010(4) C21 0.053(5) 0.072(6) 0.077(6) -0.015(5) -0.019(5) -0.025(5) C22 0.053(5) 0.072(6) 0.077(6) -0.015(5) -0.019(5) -0.025(5) C23 0.110(10) 0.033(4) 0.036(5) 0.019(4) 0.033(6) 0.025(5) C24 0.110(10) 0.033(4) 0.036(5) 0.019(4) 0.033(6) 0.025(5) C25 0.110(10) 0.033(4) 0.036(5) 0.019(4) 0.033(6) 0.025(5) C28 0.026(11) 0.040(12) 0.052(11) 0.001(9) 0.006(8) -0.010(9) Si6 0.0417(18) 0.078(5) 0.027(5) -0.001(3) 0.006(2) 0.035(2) C6 0.024(7) 0.022(4) 0.026(5) -0.006(3) 0.000(4) 0.008(4) C7 0.029(6) 0.026(3) 0.019(4) -0.007(3) 0.006(4) -0.001(4) C8 0.034(9) 0.026(6) 0.019(6) 0.005(5) 0.009(6) 0.000(6) C9 0.037(9) 0.021(7) 0.026(6) -0.003(5) 0.006(6) -0.008(7) C10 0.029(6) 0.026(3) 0.019(4) -0.007(3) 0.006(4) -0.001(4) C20 0.017(10) 0.047(14) 0.08(2) -0.019(13) 0.001(11) 0.007(10) C27 0.055(3) 0.056(3) 0.055(3) 0.0000(2) 0.0053(4) 0.0000(2) C30 0.068(8) 0.097(13) 0.058(13) -0.008(11) -0.002(9) 0.040(9) C19 0.025(11) 0.075(18) 0.034(12) -0.019(11) 0.010(9) 0.000(11) K1 0.0474(13) 0.0373(12) 0.0393(12) -0.0079(9) 0.0140(10) 0.0059(10) O1 0.046(10) 0.19(2) 0.127(14) 0.054(16) 0.012(11) 0.001(12) C31 0.060(9) 0.165(16) 0.128(13) 0.048(13) 0.024(10) -0.004(10) C32 0.060(9) 0.165(16) 0.128(13) 0.048(13) 0.024(10) -0.004(10) C33 0.060(9) 0.165(16) 0.128(13) 0.048(13) 0.024(10) -0.004(10) C34 0.060(9) 0.165(16) 0.128(13) 0.048(13) 0.024(10) -0.004(10) O2 0.056(10) 0.050(8) 0.062(8) 0.009(7) -0.009(7) 0.003(7) C35 0.100(13) 0.056(8) 0.070(9) 0.011(8) -0.021(8) 0.013(8) C36 0.078(18) 0.12(3) 0.090(14) -0.061(17) -0.026(12) -0.033(16) C37 0.062(14) 0.041(11) 0.069(14) 0.020(10) -0.016(10) -0.008(9) C38 0.100(13) 0.056(8) 0.070(9) 0.011(8) -0.021(8) 0.013(8) O3 0.074(3) 0.078(3) 0.078(3) -0.025(3) 0.030(3) -0.009(3) O6 0.074(3) 0.078(3) 0.078(3) -0.025(3) 0.030(3) -0.009(3) O8 0.074(3) 0.078(3) 0.078(3) -0.025(3) 0.030(3) -0.009(3) O10 0.074(3) 0.078(3) 0.078(3) -0.025(3) 0.030(3) -0.009(3) O12 0.074(3) 0.078(3) 0.078(3) -0.025(3) 0.030(3) -0.009(3) O14 0.074(3) 0.078(3) 0.078(3) -0.025(3) 0.030(3) -0.009(3) C41 0.099(6) 0.086(7) 0.082(6) -0.039(6) 0.045(5) -0.013(6) C45 0.075(9) 0.049(11) 0.047(10) -0.011(8) 0.001(8) -0.035(9) C46 0.053(11) 0.065(9) 0.048(11) -0.009(9) -0.014(8) -0.004(10) C47 0.064(13) 0.052(10) 0.112(14) 0.003(10) 0.059(11) 0.002(9) C48 0.057(7) 0.049(9) 0.057(11) 0.017(8) 0.038(8) 0.008(7) C49 0.098(10) 0.077(11) 0.083(16) -0.029(12) 0.045(11) -0.007(10) C50 0.099(6) 0.086(7) 0.082(6) -0.039(6) 0.045(5) -0.013(6) C59 0.099(6) 0.086(7) 0.082(6) -0.039(6) 0.045(5) -0.013(6) C60 0.070(9) 0.099(13) 0.083(16) -0.022(12) 0.027(10) -0.008(10) C62 0.068(14) 0.113(14) 0.110(16) -0.047(13) 0.045(12) -0.041(11) C65 0.057(14) 0.069(10) 0.075(14) -0.005(11) -0.002(11) -0.010(11) C67 0.087(9) 0.052(13) 0.069(13) -0.022(11) 0.007(9) -0.020(10) O4 0.074(3) 0.078(3) 0.078(3) -0.025(3) 0.030(3) -0.009(3) O5 0.074(3) 0.078(3) 0.078(3) -0.025(3) 0.030(3) -0.009(3) O7 0.074(3) 0.078(3) 0.078(3) -0.025(3) 0.030(3) -0.009(3) O9 0.074(3) 0.078(3) 0.078(3) -0.025(3) 0.030(3) -0.009(3) O11 0.074(3) 0.078(3) 0.078(3) -0.025(3) 0.030(3) -0.009(3) O13 0.074(3) 0.078(3) 0.078(3) -0.025(3) 0.030(3) -0.009(3) C39 0.099(6) 0.086(7) 0.082(6) -0.039(6) 0.045(5) -0.013(6) C40 0.099(6) 0.086(7) 0.082(6) -0.039(6) 0.045(5) -0.013(6) C51 0.089(10) 0.083(13) 0.077(16) -0.029(12) 0.047(12) -0.007(10) C52 0.070(14) 0.083(12) 0.083(10) -0.028(10) 0.042(11) -0.005(10) C53 0.101(17) 0.080(9) 0.083(14) -0.016(10) 0.036(12) -0.022(11) C55 0.069(11) 0.057(14) 0.077(15) -0.012(10) 0.023(12) -0.015(11) C56 0.104(15) 0.072(15) 0.072(11) 0.011(11) 0.048(13) 0.031(11) C57 0.113(16) 0.072(9) 0.13(2) 0.012(15) 0.071(15) 0.022(10) C63 0.048(13) 0.091(8) 0.093(12) -0.026(10) 0.014(11) -0.005(10) C64 0.058(13) 0.068(15) 0.102(13) -0.027(11) 0.013(12) -0.033(13) C68 0.090(14) 0.069(15) 0.087(8) -0.028(11) 0.017(10) -0.004(11) C69 0.085(12) 0.065(10) 0.039(10) -0.019(10) -0.003(9) 0.003(9) C23A 0.110(10) 0.033(4) 0.036(5) 0.019(4) 0.033(6) 0.025(5) C24A 0.110(10) 0.033(4) 0.036(5) 0.019(4) 0.033(6) 0.025(5) Si3A 0.0285(13) 0.0410(12) 0.0335(11) -0.0175(9) 0.0052(10) -0.0049(11) C25A 0.110(10) 0.033(4) 0.036(5) 0.019(4) 0.033(6) 0.025(5) C27A 0.055(3) 0.056(3) 0.055(3) 0.0000(2) 0.0053(4) 0.0000(2) Si6A 0.0417(18) 0.078(5) 0.027(5) -0.001(3) 0.006(2) 0.035(2) C28A 0.034(15) 0.037(14) 0.045(14) 0.004(10) 0.026(12) 0.008(11) C30A 0.068(8) 0.097(13) 0.058(13) -0.008(11) -0.002(9) 0.040(9) N1A 0.052(4) 0.032(3) 0.028(3) 0.002(3) 0.014(3) 0.018(3) N2A 0.026(17) 0.018(6) 0.010(6) -0.002(5) 0.005(7) -0.005(7) C1A 0.022(11) 0.034(6) 0.030(7) -0.009(5) 0.012(7) 0.003(6) C2A 0.024(7) 0.022(4) 0.026(5) -0.006(3) 0.000(4) 0.008(4) C3A 0.044(6) 0.028(5) 0.020(5) -0.012(4) -0.007(6) 0.008(5) C4A 0.049(16) 0.024(7) 0.021(7) -0.008(6) -0.008(9) 0.014(9) C5A 0.024(18) 0.022(6) 0.019(6) -0.008(4) -0.005(6) 0.009(7) C6A 0.035(13) 0.024(5) 0.012(6) -0.007(4) 0.005(6) 0.008(6) C7A 0.050(10) 0.025(6) 0.017(6) -0.005(5) 0.001(7) -0.007(7) C8A 0.037(9) 0.025(6) 0.022(6) -0.002(5) 0.007(6) -0.005(6) C9A 0.033(9) 0.016(6) 0.024(6) 0.000(4) 0.009(6) -0.003(6) C10A 0.021(9) 0.019(6) 0.019(6) -0.004(5) 0.009(6) 0.001(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 N1 Zn1 N2 78.8(6) . . N3 Zn1 N1 119.4(14) . . N3 Zn1 N2 107.4(15) . . N3 Zn1 N1A 120.2(17) . . N3 Zn1 N2A 102.0(15) . . N4 Zn1 N1 105.1(13) . . N4 Zn1 N2 115.4(18) . . N4 Zn1 N3 122.7(3) . . N4 Zn1 N1A 104.4(14) . . N4 Zn1 N2A 121.3(17) . . N2A Zn1 N1A 79.0(6) . . N3 Si1 C21 112.9(5) . . N3 Si1 C22 113.4(5) . . N3 Si1 C20 116.6(8) . . N3 Si1 C19 111.7(7) . . C21 Si1 C22 107.1(6) . . C21 Si1 C20 91.6(10) . . C21 Si1 C19 117.5(9) . . C22 Si1 C20 113.0(9) . . C22 Si1 C19 92.6(10) . . N3 Si2 C16 112.9(4) . . N3 Si2 C17 113.5(4) . . N3 Si2 C18 113.6(4) . . C16 Si2 C17 104.5(5) . . C16 Si2 C18 104.8(4) . . C18 Si2 C17 106.8(5) . . N4 Si3 C23 117.1(8) . . N4 Si3 C24 103.7(7) . . N4 Si3 C25 114.5(7) . . C23 Si3 C24 105.6(12) . . C23 Si3 C25 110.5(12) . . C25 Si3 C24 103.8(10) . . C1 N1 Zn1 121.9(13) . . C1 N1 C5 121.0(18) . . C5 N1 Zn1 113.7(10) . . C6 N2 Zn1 114.4(9) . . C10 N2 Zn1 127.4(11) . . C10 N2 C6 117.9(14) . . Si1 N3 Zn1 116.7(4) . . Si2 N3 Zn1 118.0(4) . . Si2 N3 Si1 123.5(4) . . Si3 N4 Zn1 109.0(4) . . Si6 N4 Zn1 118.6(7) . . Si3A N4 Zn1 126.6(5) . . Si3A N4 Si6 114.7(7) . . Si6A N4 Zn1 115.9(7) . . Si6A N4 Si3 131.6(7) . . N1 C1 H1 118.6 . . C2 C1 N1 122.9(15) . . C2 C1 H1 118.6 . . C1 C2 H2 122.3 . . C1 C2 C3 115.3(14) . . C3 C2 H2 122.3 . . C2 C3 H3 119.1 . . C4 C3 C2 121.8(15) . . C4 C3 H3 119.1 . . C3 C4 H4 119.8 . . C3 C4 C5 120.4(15) . . C5 C4 H4 119.8 . . N1 C5 C4 114.8(13) . . N1 C5 C6 118.4(12) . . C6 C5 C4 126.8(15) . . Si2 C16 H16A 109.5 . . Si2 C16 H16B 109.5 . . Si2 C16 H16C 109.5 . . H16A C16 H16B 109.5 . . H16A C16 H16C 109.5 . . H16B C16 H16C 109.5 . . Si2 C17 H17A 109.5 . . Si2 C17 H17B 109.5 . . Si2 C17 H17C 109.5 . . H17A C17 H17B 109.5 . . H17A C17 H17C 109.5 . . H17B C17 H17C 109.5 . . Si2 C18 H18A 109.5 . . Si2 C18 H18B 109.5 . . Si2 C18 H18C 109.5 . . H18A C18 H18B 109.5 . . H18A C18 H18C 109.5 . . H18B C18 H18C 109.5 . . Si1 C21 H21A 109.5 . . Si1 C21 H21B 109.5 . . Si1 C21 H21C 109.5 . . H21A C21 H21B 109.5 . . H21A C21 H21C 109.5 . . H21B C21 H21C 109.5 . . Si1 C22 H22A 109.5 . . Si1 C22 H22B 109.5 . . Si1 C22 H22C 109.5 . . H22A C22 H22B 109.5 . . H22A C22 H22C 109.5 . . H22B C22 H22C 109.5 . . Si3 C23 H23A 109.5 . . Si3 C23 H23B 109.5 . . Si3 C23 H23C 109.5 . . H23A C23 H23B 109.5 . . H23A C23 H23C 109.5 . . H23B C23 H23C 109.5 . . Si3 C24 H24A 109.5 . . Si3 C24 H24B 109.5 . . Si3 C24 H24C 109.5 . . H24A C24 H24B 109.5 . . H24A C24 H24C 109.5 . . H24B C24 H24C 109.5 . . Si3 C25 H25A 109.5 . . Si3 C25 H25B 109.5 . . Si3 C25 H25C 109.5 . . H25A C25 H25B 109.5 . . H25A C25 H25C 109.5 . . H25B C25 H25C 109.5 . . H28A C28 H28B 109.5 . . H28A C28 H28C 109.5 . . H28B C28 H28C 109.5 . . Si6 C28 H28A 109.5 . . Si6 C28 H28B 109.5 . . Si6 C28 H28C 109.5 . . N4 Si6 C28 109.7(10) . . N4 Si6 C27 114.7(10) . . N4 Si6 C30 117.6(12) . . C28 Si6 C27 107.6(11) . . C30 Si6 C28 105.5(12) . . C30 Si6 C27 100.8(12) . . N2 C6 C5 114.0(14) . . C7 C6 N2 116.6(13) . . C7 C6 C5 129.4(14) . . C6 C7 H7 118.2 . . C8 C7 C6 123.6(13) . . C8 C7 H7 118.2 . . C7 C8 H8 120.9 . . C7 C8 C9 118.1(13) . . C9 C8 H8 120.9 . . C8 C9 H9 121.5 . . C10 C9 C8 116.9(14) . . C10 C9 H9 121.5 . . N2 C10 C9 126.5(14) . . N2 C10 H10 116.7 . . C9 C10 H10 116.7 . . Si1 C20 H20A 109.5 . . Si1 C20 H20B 109.5 . . Si1 C20 H20C 109.5 . . H20A C20 H20B 109.5 . . H20A C20 H20C 109.5 . . H20B C20 H20C 109.5 . . Si6 C27 H27A 109.5 . . Si6 C27 H27B 109.5 . . Si6 C27 H27C 109.5 . . H27A C27 H27B 109.5 . . H27A C27 H27C 109.5 . . H27B C27 H27C 109.5 . . Si6 C30 H30A 109.5 . . Si6 C30 H30B 109.5 . . Si6 C30 H30C 109.5 . . H30A C30 H30B 109.5 . . H30A C30 H30C 109.5 . . H30B C30 H30C 109.5 . . Si1 C19 H19A 109.5 . . Si1 C19 H19B 109.5 . . Si1 C19 H19C 109.5 . . H19A C19 H19B 109.5 . . H19A C19 H19C 109.5 . . H19B C19 H19C 109.5 . . O3 K1 O6 59.4(4) . . O3 K1 O8 119.1(4) . . O3 K1 O10 177.8(5) . . O3 K1 O12 122.8(4) . . O3 K1 O14 62.7(4) . . O8 K1 O6 60.9(4) . . O8 K1 O10 58.8(4) . . O8 K1 O12 116.2(4) . . O10 K1 O6 118.8(4) . . O10 K1 O12 59.0(4) . . O12 K1 O6 176.4(6) . . O14 K1 O6 121.7(4) . . O14 K1 O8 174.7(6) . . O14 K1 O10 119.2(4) . . O14 K1 O12 60.9(4) . . O4 K1 O9 172.0(4) . . O11 K1 O4 128.1(4) . . O11 K1 O9 59.9(4) . . O13 K1 O4 61.7(4) . . O13 K1 O9 126.3(4) . . O13 K1 O11 67.1(4) . . C32 O1 K1 145.1(18) . . C33 O1 K1 103.3(18) . . C33 O1 C32 111(3) . . H31A C31 H31B 109.5 . . H31A C31 H31C 109.5 . . H31B C31 H31C 109.5 . . C32 C31 H31A 109.5 . . C32 C31 H31B 109.5 . . C32 C31 H31C 109.5 . . O1 C32 H32A 108.4 . . O1 C32 H32B 108.4 . . C31 C32 O1 116(3) . . C31 C32 H32A 108.4 . . C31 C32 H32B 108.4 . . H32A C32 H32B 107.4 . . O1 C33 H33A 108.8 . . O1 C33 H33B 108.8 . . H33A C33 H33B 107.7 . . C34 C33 O1 114(3) . . C34 C33 H33A 108.8 . . C34 C33 H33B 108.8 . . K1 C34 H34A 31.2 . . K1 C34 H34B 137.6 . . K1 C34 H34C 102.5 . . C33 C34 K1 84(2) . . C33 C34 H34A 109.5 . . C33 C34 H34B 109.5 . . C33 C34 H34C 109.5 . . H34A C34 H34B 109.5 . . H34A C34 H34C 109.5 . . H34B C34 H34C 109.5 . . C35 O2 K1 127.5(14) . . C38 O2 K1 132.4(14) . . C38 O2 C35 100(2) . . O2 C35 H35A 108.3 . . O2 C35 H35B 108.3 . . H35A C35 H35B 107.4 . . C36 C35 O2 116(2) . . C36 C35 H35A 108.3 . . C36 C35 H35B 108.3 . . C35 C36 H36A 109.5 . . C35 C36 H36B 109.5 . . C35 C36 H36C 109.5 . . H36A C36 H36B 109.5 . . H36A C36 H36C 109.5 . . H36B C36 H36C 109.5 . . H37A C37 H37B 109.5 . . H37A C37 H37C 109.5 . . H37B C37 H37C 109.5 . . C38 C37 H37A 109.5 . . C38 C37 H37B 109.5 . . C38 C37 H37C 109.5 . . O2 C38 H38A 103.9 . . O2 C38 H38B 103.9 . . C37 C38 O2 133(3) . . C37 C38 H38A 103.9 . . C37 C38 H38B 103.9 . . H38A C38 H38B 105.4 . . C62 O3 K1 118.2(12) . . C62 O3 C65 113.6(16) . . C65 O3 K1 122.8(14) . . C50 O6 K1 110.0(14) . . C67 O6 K1 115.5(13) . . C67 O6 C50 111.9(17) . . C48 O8 K1 118.0(11) . . C49 O8 K1 116.8(13) . . C49 O8 C48 107.8(15) . . C46 O10 K1 119.8(13) . . C47 O10 K1 120.4(12) . . C47 O10 C46 111.0(16) . . C41 O12 K1 115.3(15) . . C45 O12 K1 117.5(13) . . C45 O12 C41 110.5(16) . . C59 O14 K1 118.7(12) . . C60 O14 K1 112.1(13) . . C60 O14 C59 112.1(16) . . O12 C41 H41A 110.2 . . O12 C41 H41B 110.2 . . O12 C41 C59 107.4(16) . . H41A C41 H41B 108.5 . . C59 C41 H41A 110.2 . . C59 C41 H41B 110.2 . . O12 C45 H45A 109.4 . . O12 C45 H45B 109.4 . . O12 C45 C46 111.2(15) . . H45A C45 H45B 108.0 . . C46 C45 H45A 109.4 . . C46 C45 H45B 109.4 . . O10 C46 C45 109.7(16) . . O10 C46 H46A 109.7 . . O10 C46 H46B 109.7 . . C45 C46 H46A 109.7 . . C45 C46 H46B 109.7 . . H46A C46 H46B 108.2 . . O10 C47 H47A 109.5 . . O10 C47 H47B 109.5 . . O10 C47 C48 110.7(14) . . H47A C47 H47B 108.1 . . C48 C47 H47A 109.5 . . C48 C47 H47B 109.5 . . O8 C48 C47 107.8(14) . . O8 C48 H48A 110.1 . . O8 C48 H48B 110.1 . . C47 C48 H48A 110.1 . . C47 C48 H48B 110.1 . . H48A C48 H48B 108.5 . . O8 C49 H49A 110.2 . . O8 C49 H49B 110.2 . . O8 C49 C50 107.3(17) . . H49A C49 H49B 108.5 . . C50 C49 H49A 110.2 . . C50 C49 H49B 110.2 . . O6 C50 C49 108.9(18) . . O6 C50 H50A 109.9 . . O6 C50 H50B 109.9 . . C49 C50 H50A 109.9 . . C49 C50 H50B 109.9 . . H50A C50 H50B 108.3 . . O14 C59 C41 112.0(17) . . O14 C59 H59A 109.2 . . O14 C59 H59B 109.2 . . C41 C59 H59A 109.2 . . C41 C59 H59B 109.2 . . H59A C59 H59B 107.9 . . K1 C60 H60A 89.5 . . K1 C60 H60B 154.8 . . O14 C60 K1 46.0(10) . . O14 C60 H60A 109.6 . . O14 C60 H60B 109.6 . . O14 C60 C62 110.3(17) . . H60A C60 H60B 108.1 . . C62 C60 K1 79.7(10) . . C62 C60 H60A 109.6 . . C62 C60 H60B 109.6 . . K1 C62 H62A 104.0 . . K1 C62 H62B 143.4 . . O3 C62 K1 41.6(9) . . O3 C62 C60 111.4(16) . . O3 C62 H62A 109.4 . . O3 C62 H62B 109.4 . . C60 C62 K1 75.2(10) . . C60 C62 H62A 109.4 . . C60 C62 H62B 109.4 . . H62A C62 H62B 108.0 . . O3 C65 H65A 110.1 . . O3 C65 H65B 110.1 . . O3 C65 C67 108.1(17) . . H65A C65 H65B 108.4 . . C67 C65 H65A 110.1 . . C67 C65 H65B 110.1 . . O6 C67 C65 110.2(17) . . O6 C67 H67A 109.6 . . O6 C67 H67B 109.6 . . C65 C67 H67A 109.6 . . C65 C67 H67B 109.6 . . H67A C67 H67B 108.1 . . C39 O4 K1 112.6(13) . . C63 O4 K1 112.4(14) . . C63 O4 C39 119.9(18) . . C64 O5 K1 112.5(13) . . C68 O5 K1 117.1(15) . . C68 O5 C64 119(2) . . C51 O7 K1 115.7(13) . . C69 O7 K1 118.5(12) . . C69 O7 C51 116.3(17) . . C52 O9 K1 115.1(13) . . C53 O9 K1 112.4(13) . . C53 O9 C52 117.7(18) . . C55 O11 K1 118.8(14) . . C56 O11 K1 103.5(14) . . C56 O11 C55 127.6(19) . . C40 O13 K1 119.4(14) . . C40 O13 C57 119.2(18) . . C57 O13 K1 106.2(16) . . O4 C39 H39A 108.3 . . O4 C39 H39B 108.3 . . O4 C39 C40 115.8(18) . . H39A C39 H39B 107.4 . . C40 C39 H39A 108.3 . . C40 C39 H39B 108.3 . . K1 C40 H40A 102.8 . . K1 C40 H40B 143.3 . . O13 C40 K1 41.2(10) . . O13 C40 C39 117.0(18) . . O13 C40 H40A 108.1 . . O13 C40 H40B 108.1 . . C39 C40 K1 81.4(10) . . C39 C40 H40A 108.1 . . C39 C40 H40B 108.1 . . H40A C40 H40B 107.3 . . O7 C51 H51A 109.7 . . O7 C51 H51B 109.7 . . O7 C51 C52 109.9(17) . . H51A C51 H51B 108.2 . . C52 C51 H51A 109.7 . . C52 C51 H51B 109.7 . . O9 C52 C51 118.0(19) . . O9 C52 H52A 107.8 . . O9 C52 H52B 107.8 . . C51 C52 H52A 107.8 . . C51 C52 H52B 107.8 . . H52A C52 H52B 107.2 . . O9 C53 H53A 108.2 . . O9 C53 H53B 108.2 . . O9 C53 C55 116.4(18) . . H53A C53 H53B 107.3 . . C55 C53 H53A 108.2 . . C55 C53 H53B 108.2 . . O11 C55 C53 114.5(19) . . O11 C55 H55A 108.6 . . O11 C55 H55B 108.6 . . C53 C55 H55A 108.6 . . C53 C55 H55B 108.6 . . H55A C55 H55B 107.6 . . K1 C56 H56A 155.5 . . K1 C56 H56B 94.6 . . O11 C56 K1 53.7(12) . . O11 C56 H56A 107.1 . . O11 C56 H56B 107.1 . . O11 C56 C57 121(2) . . H56A C56 H56B 106.8 . . C57 C56 K1 76.7(13) . . C57 C56 H56A 107.1 . . C57 C56 H56B 107.1 . . K1 C57 H57A 158.1 . . K1 C57 H57B 88.8 . . O13 C57 K1 50.6(12) . . O13 C57 C56 113.2(19) . . O13 C57 H57A 108.9 . . O13 C57 H57B 108.9 . . C56 C57 K1 77.8(13) . . C56 C57 H57A 108.9 . . C56 C57 H57B 108.9 . . H57A C57 H57B 107.7 . . K1 C63 H63A 155.4 . . K1 C63 H63B 88.5 . . O4 C63 K1 47.5(11) . . O4 C63 H63A 108.5 . . O4 C63 H63B 108.5 . . O4 C63 C64 115(2) . . H63A C63 H63B 107.5 . . C64 C63 K1 82.7(11) . . C64 C63 H63A 108.5 . . C64 C63 H63B 108.5 . . O5 C64 C63 117(2) . . O5 C64 H64A 108.1 . . O5 C64 H64B 108.1 . . C63 C64 H64A 108.1 . . C63 C64 H64B 108.1 . . H64A C64 H64B 107.3 . . O5 C68 H68A 108.7 . . O5 C68 H68B 108.7 . . O5 C68 C69 114.3(18) . . H68A C68 H68B 107.6 . . C69 C68 H68A 108.7 . . C69 C68 H68B 108.7 . . O7 C69 C68 115.0(18) . . O7 C69 H69A 108.5 . . O7 C69 H69B 108.5 . . C68 C69 H69A 108.5 . . C68 C69 H69B 108.5 . . H69A C69 H69B 107.5 . . H23D C23A H23E 109.5 . . H23D C23A H23F 109.5 . . H23E C23A H23F 109.5 . . Si3A C23A H23D 109.5 . . Si3A C23A H23E 109.5 . . Si3A C23A H23F 109.5 . . H24D C24A H24E 109.5 . . H24D C24A H24F 109.5 . . H24E C24A H24F 109.5 . . Si3A C24A H24D 109.5 . . Si3A C24A H24E 109.5 . . Si3A C24A H24F 109.5 . . N4 Si3A C23A 110.5(7) . . N4 Si3A C24A 107.5(7) . . N4 Si3A C25A 123.2(8) . . C23A Si3A C24A 102.7(12) . . C25A Si3A C23A 107.0(11) . . C25A Si3A C24A 104.0(11) . . Si3A C25A H25D 109.5 . . Si3A C25A H25E 109.5 . . Si3A C25A H25F 109.5 . . H25D C25A H25E 109.5 . . H25D C25A H25F 109.5 . . H25E C25A H25F 109.5 . . H27D C27A H27E 109.5 . . H27D C27A H27F 109.5 . . H27E C27A H27F 109.5 . . Si6A C27A H27D 109.5 . . Si6A C27A H27E 109.5 . . Si6A C27A H27F 109.5 . . N4 Si6A C27A 109.6(10) . . N4 Si6A C28A 110.7(10) . . N4 Si6A C30A 118.2(12) . . C28A Si6A C27A 109.1(11) . . C30A Si6A C27A 101.3(12) . . C30A Si6A C28A 107.3(11) . . Si6A C28A H28D 109.5 . . Si6A C28A H28E 109.5 . . Si6A C28A H28F 109.5 . . H28D C28A H28E 109.5 . . H28D C28A H28F 109.5 . . H28E C28A H28F 109.5 . . Si6A C30A H30D 109.5 . . Si6A C30A H30E 109.5 . . Si6A C30A H30F 109.5 . . H30D C30A H30E 109.5 . . H30D C30A H30F 109.5 . . H30E C30A H30F 109.5 . . C1A N1A Zn1 131.5(12) . . C1A N1A C5A 113.6(14) . . C5A N1A Zn1 114.1(10) . . C6A N2A Zn1 112.9(9) . . C10A N2A Zn1 128.1(11) . . C10A N2A C6A 117.7(15) . . N1A C1A H1A 117.1 . . N1A C1A C2A 125.8(16) . . C2A C1A H1A 117.1 . . C1A C2A H2A 120.3 . . C1A C2A C3A 119.4(14) . . C3A C2A H2A 120.3 . . C2A C3A H3A 121.3 . . C4A C3A C2A 117.3(15) . . C4A C3A H3A 121.3 . . C3A C4A H4A 120.3 . . C3A C4A C5A 119.4(15) . . C5A C4A H4A 120.3 . . N1A C5A C4A 123.1(13) . . N1A C5A C6A 116.5(12) . . C6A C5A C4A 120.3(13) . . N2A C6A C5A 117.3(12) . . C7A C6A N2A 120.8(12) . . C7A C6A C5A 121.9(13) . . C6A C7A H7A 120.3 . . C8A C7A C6A 119.5(13) . . C8A C7A H7A 120.3 . . C7A C8A H8A 120.5 . . C7A C8A C9A 119.0(14) . . C9A C8A H8A 120.5 . . C8A C9A H9A 120.1 . . C10A C9A C8A 119.7(13) . . C10A C9A H9A 120.1 . . N2A C10A C9A 123.2(13) . . N2A C10A H10A 118.4 . . C9A C10A H10A 118.4 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Zn1 N1 2.090(11) . Zn1 N2 2.095(12) . Zn1 N3 1.979(6) . Zn1 N4 1.969(8) . Zn1 N1A 2.092(12) . Zn1 N2A 2.079(11) . Si1 N3 1.699(7) . Si1 C21 1.848(14) . Si1 C22 1.868(13) . Si1 C20 1.928(15) . Si1 C19 1.919(15) . Si2 N3 1.696(7) . Si2 C16 1.859(9) . Si2 C17 1.885(9) . Si2 C18 1.869(9) . Si3 N4 1.792(10) . Si3 C23 1.84(2) . Si3 C24 1.95(2) . Si3 C25 1.843(19) . N1 C1 1.379(19) . N1 C5 1.379(15) . N2 C6 1.413(15) . N2 C10 1.336(17) . N4 Si6 1.730(13) . N4 Si3A 1.661(9) . N4 Si6A 1.711(13) . C1 H1 0.9500 . C1 C2 1.374(16) . C2 H2 0.9500 . C2 C3 1.394(18) . C3 H3 0.9500 . C3 C4 1.389(18) . C4 H4 0.9500 . C4 C5 1.437(15) . C5 C6 1.419(17) . C16 H16A 0.9800 . C16 H16B 0.9800 . C16 H16C 0.9800 . C17 H17A 0.9800 . C17 H17B 0.9800 . C17 H17C 0.9800 . C18 H18A 0.9800 . C18 H18B 0.9800 . C18 H18C 0.9800 . C21 H21A 0.9800 . C21 H21B 0.9800 . C21 H21C 0.9800 . C22 H22A 0.9800 . C22 H22B 0.9800 . C22 H22C 0.9800 . C23 H23A 0.9800 . C23 H23B 0.9800 . C23 H23C 0.9800 . C24 H24A 0.9800 . C24 H24B 0.9800 . C24 H24C 0.9800 . C25 H25A 0.9800 . C25 H25B 0.9800 . C25 H25C 0.9800 . C28 H28A 0.9800 . C28 H28B 0.9800 . C28 H28C 0.9800 . C28 Si6 1.868(14) . Si6 C27 1.884(17) . Si6 C30 1.861(17) . C6 C7 1.411(17) . C7 H7 0.9500 . C7 C8 1.366(18) . C8 H8 0.9500 . C8 C9 1.409(17) . C9 H9 0.9500 . C9 C10 1.360(17) . C10 H10 0.9500 . C20 H20A 0.9800 . C20 H20B 0.9800 . C20 H20C 0.9800 . C27 H27A 0.9800 . C27 H27B 0.9800 . C27 H27C 0.9800 . C30 H30A 0.9800 . C30 H30B 0.9800 . C30 H30C 0.9800 . C19 H19A 0.9800 . C19 H19B 0.9800 . C19 H19C 0.9800 . K1 O1 2.85(2) . K1 O2 2.664(16) . K1 O3 2.665(17) . K1 O6 2.832(18) . K1 O8 2.761(16) . K1 O10 2.792(17) . K1 O12 2.81(2) . K1 O14 2.700(17) . K1 O4 2.795(18) . K1 O9 2.873(17) . K1 O11 2.711(18) . K1 O13 2.621(16) . O1 C32 1.57(3) . O1 C33 1.56(3) . C31 H31A 0.9800 . C31 H31B 0.9800 . C31 H31C 0.9800 . C31 C32 1.33(4) . C32 H32A 0.9900 . C32 H32B 0.9900 . C33 H33A 0.9900 . C33 H33B 0.9900 . C33 C34 1.36(4) . C34 H34A 0.9800 . C34 H34B 0.9800 . C34 H34C 0.9800 . O2 C35 1.43(2) . O2 C38 1.42(2) . C35 H35A 0.9900 . C35 H35B 0.9900 . C35 C36 1.27(3) . C36 H36A 0.9800 . C36 H36B 0.9800 . C36 H36C 0.9800 . C37 H37A 0.9800 . C37 H37B 0.9800 . C37 H37C 0.9800 . C37 C38 1.21(3) . C38 H38A 0.9900 . C38 H38B 0.9900 . O3 C62 1.383(15) . O3 C65 1.401(16) . O6 C50 1.421(16) . O6 C67 1.396(16) . O8 C48 1.417(15) . O8 C49 1.417(16) . O10 C46 1.402(16) . O10 C47 1.392(15) . O12 C41 1.408(16) . O12 C45 1.407(15) . O14 C59 1.410(15) . O14 C60 1.395(16) . C41 H41A 0.9900 . C41 H41B 0.9900 . C41 C59 1.54(2) . C45 H45A 0.9900 . C45 H45B 0.9900 . C45 C46 1.50(2) . C46 H46A 0.9900 . C46 H46B 0.9900 . C47 H47A 0.9900 . C47 H47B 0.9900 . C47 C48 1.53(2) . C48 H48A 0.9900 . C48 H48B 0.9900 . C49 H49A 0.9900 . C49 H49B 0.9900 . C49 C50 1.52(2) . C50 H50A 0.9900 . C50 H50B 0.9900 . C59 H59A 0.9900 . C59 H59B 0.9900 . C60 H60A 0.9900 . C60 H60B 0.9900 . C60 C62 1.52(2) . C62 H62A 0.9900 . C62 H62B 0.9900 . C65 H65A 0.9900 . C65 H65B 0.9900 . C65 C67 1.52(2) . C67 H67A 0.9900 . C67 H67B 0.9900 . O4 C39 1.359(15) . O4 C63 1.304(16) . O5 C64 1.338(16) . O5 C68 1.314(16) . O7 C51 1.338(15) . O7 C69 1.327(15) . O9 C52 1.332(15) . O9 C53 1.323(16) . O11 C55 1.320(16) . O11 C56 1.302(15) . O13 C40 1.321(15) . O13 C57 1.337(16) . C39 H39A 0.9900 . C39 H39B 0.9900 . C39 C40 1.44(2) . C40 H40A 0.9900 . C40 H40B 0.9900 . C51 H51A 0.9900 . C51 H51B 0.9900 . C51 C52 1.44(2) . C52 H52A 0.9900 . C52 H52B 0.9900 . C53 H53A 0.9900 . C53 H53B 0.9900 . C53 C55 1.45(2) . C55 H55A 0.9900 . C55 H55B 0.9900 . C56 H56A 0.9900 . C56 H56B 0.9900 . C56 C57 1.44(2) . C57 H57A 0.9900 . C57 H57B 0.9900 . C63 H63A 0.9900 . C63 H63B 0.9900 . C63 C64 1.44(2) . C64 H64A 0.9900 . C64 H64B 0.9900 . C68 H68A 0.9900 . C68 H68B 0.9900 . C68 C69 1.44(2) . C69 H69A 0.9900 . C69 H69B 0.9900 . C23A H23D 0.9800 . C23A H23E 0.9800 . C23A H23F 0.9800 . C23A Si3A 1.90(2) . C24A H24D 0.9800 . C24A H24E 0.9800 . C24A H24F 0.9800 . C24A Si3A 1.95(2) . Si3A C25A 1.841(19) . C25A H25D 0.9800 . C25A H25E 0.9800 . C25A H25F 0.9800 . C27A H27D 0.9800 . C27A H27E 0.9800 . C27A H27F 0.9800 . C27A Si6A 1.894(17) . Si6A C28A 1.891(17) . Si6A C30A 1.853(17) . C28A H28D 0.9800 . C28A H28E 0.9800 . C28A H28F 0.9800 . C30A H30D 0.9800 . C30A H30E 0.9800 . C30A H30F 0.9800 . N1A C1A 1.358(18) . N1A C5A 1.367(15) . N2A C6A 1.398(15) . N2A C10A 1.331(17) . C1A H1A 0.9500 . C1A C2A 1.376(16) . C2A H2A 0.9500 . C2A C3A 1.389(18) . C3A H3A 0.9500 . C3A C4A 1.381(18) . C4A H4A 0.9500 . C4A C5A 1.432(15) . C5A C6A 1.403(16) . C6A C7A 1.395(17) . C7A H7A 0.9500 . C7A C8A 1.360(18) . C8A H8A 0.9500 . C8A C9A 1.402(17) . C9A H9A 0.9500 . C9A C10A 1.354(16) . C10A H10A 0.9500 .