#------------------------------------------------------------------------------ #$Date: 2020-07-06 05:32:24 +0300 (Mon, 06 Jul 2020) $ #$Revision: 253844 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/79/1557969.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_1557969 loop_ _publ_author_name 'Fairley, Michael' 'Bole, Leonie J.' 'Mulks, Florian F.' 'Main, Laura' 'Kennedy, Alan R.' 'O'Hara, Charles T.' 'Garc\'ia-Alvarez, Joaqu\'in' 'Hevia, Eva' _publ_section_title ; Ultrafast amidation of esters using lithium amides under aerobic ambient temperature conditions in sustainable solvents ; _journal_issue 25 _journal_name_full 'Chemical Science' _journal_page_first 6500 _journal_paper_doi 10.1039/D0SC01349H _journal_volume 11 _journal_year 2020 _chemical_formula_moiety 'C39 H50 Li2 N2 O3, 0.72(C5 H10 O), 0.28(C5 H7 O)' _chemical_formula_sum 'C44 H60 Li2 N2 O4' _chemical_formula_weight 694.82 _chemical_properties_physical Air-sensitive,Moisture-sensitive,Oxygen-sensitive _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2019-06-13 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-12-20 deposited with the CCDC. 2020-04-30 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.453(4) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.2268(4) _cell_length_b 19.0435(7) _cell_length_c 10.7658(5) _cell_measurement_reflns_used 7467 _cell_measurement_temperature 123.35(10) _cell_measurement_theta_max 72.9960 _cell_measurement_theta_min 4.2000 _cell_volume 2047.36(15) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _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 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 123.35(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0268 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -21.00 69.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 57.0000 -180.0000 90 #__ type_ start__ end____ width___ exp.time_ 2 omega -4.00 42.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -99.0000 -150.0000 46 #__ type_ start__ end____ width___ exp.time_ 3 omega -4.00 42.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -99.0000 30.0000 46 #__ type_ start__ end____ width___ exp.time_ 4 omega 18.00 113.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 -125.0000 -120.0000 95 #__ type_ start__ end____ width___ exp.time_ 5 omega -14.00 86.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 -77.0000 90.0000 100 #__ type_ start__ end____ width___ exp.time_ 6 omega 30.00 128.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 37.0000 -120.0000 98 #__ type_ start__ end____ width___ exp.time_ 7 omega -13.00 77.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 -57.0000 -30.0000 90 #__ type_ start__ end____ width___ exp.time_ 8 omega -16.00 82.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 -37.0000 -150.0000 98 #__ type_ start__ end____ width___ exp.time_ 9 omega 30.00 128.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 37.0000 150.0000 98 #__ type_ start__ end____ width___ exp.time_ 10 omega 100.00 178.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 111.0000 -150.0000 78 #__ type_ start__ end____ width___ exp.time_ 11 omega 100.00 178.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 111.0000 -180.0000 78 #__ type_ start__ end____ width___ exp.time_ 12 omega 40.00 116.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -111.0000 -60.0000 76 #__ type_ start__ end____ width___ exp.time_ 13 omega 100.00 178.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 111.0000 120.0000 78 #__ type_ start__ end____ width___ exp.time_ 14 omega 39.00 94.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -25.0000 -30.0000 55 #__ type_ start__ end____ width___ exp.time_ 15 omega 40.00 116.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -111.0000 -180.0000 76 #__ type_ start__ end____ width___ exp.time_ 16 omega 44.00 134.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -63.0000 -180.0000 90 #__ type_ start__ end____ width___ exp.time_ 17 omega 40.00 92.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -37.0000 90.0000 52 #__ type_ start__ end____ width___ exp.time_ 18 omega 44.00 134.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -63.0000 90.0000 90 #__ type_ start__ end____ width___ exp.time_ 19 omega 39.00 94.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -25.0000 -150.0000 55 #__ type_ start__ end____ width___ exp.time_ 20 omega 39.00 94.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -25.0000 -60.0000 55 #__ type_ start__ end____ width___ exp.time_ 21 omega 40.00 150.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -91.0000 -150.0000 110 #__ type_ start__ end____ width___ exp.time_ 22 omega 90.00 178.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 63.0000 -180.0000 88 #__ type_ start__ end____ width___ exp.time_ 23 omega 40.00 150.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -91.0000 30.0000 110 #__ type_ start__ end____ width___ exp.time_ 24 omega 78.00 178.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 25.0000 -60.0000 100 #__ type_ start__ end____ width___ exp.time_ 25 omega 39.00 94.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -25.0000 150.0000 55 #__ type_ start__ end____ width___ exp.time_ 26 omega 39.00 94.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -25.0000 30.0000 55 #__ type_ start__ end____ width___ exp.time_ 27 omega 40.00 116.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -111.0000 30.0000 76 #__ type_ start__ end____ width___ exp.time_ 28 omega 90.00 178.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 50.0000 -30.0000 88 #__ type_ start__ end____ width___ exp.time_ 29 omega -21.00 69.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 57.0000 60.0000 90 #__ type_ start__ end____ width___ exp.time_ 30 omega -73.00 44.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -19.0000 -90.0000 117 #__ type_ start__ end____ width___ exp.time_ 31 omega 35.00 125.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 57.0000 0.0000 90 #__ type_ start__ end____ width___ exp.time_ 32 omega 35.00 125.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 57.0000 60.0000 90 #__ type_ start__ end____ width___ exp.time_ 33 omega 26.00 126.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 77.0000 -90.0000 100 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0790191000 _diffrn_orient_matrix_UB_12 -0.0110342000 _diffrn_orient_matrix_UB_13 0.1374912000 _diffrn_orient_matrix_UB_21 0.0678254000 _diffrn_orient_matrix_UB_22 0.0719356000 _diffrn_orient_matrix_UB_23 -0.0035685000 _diffrn_orient_matrix_UB_31 -0.1138959000 _diffrn_orient_matrix_UB_32 0.0352776000 _diffrn_orient_matrix_UB_33 0.0505109000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0775 _diffrn_reflns_av_unetI/netI 0.0562 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 23108 _diffrn_reflns_point_group_measured_fraction_full 0.921 _diffrn_reflns_point_group_measured_fraction_max 0.914 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 69.996 _diffrn_reflns_theta_min 4.205 _diffrn_source 'Enhance (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.544 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.33981 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.127 _exptl_crystal_description block _exptl_crystal_F_000 752 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _refine_diff_density_max 0.723 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.069 _refine_ls_abs_structure_details ; Flack x determined using 2150 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.3(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.225 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 542 _refine_ls_number_reflns 7090 _refine_ls_number_restraints 252 _refine_ls_restrained_S_all 1.254 _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_gt 0.0987 _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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2735 _refine_ls_wR_factor_ref 0.2948 _reflns_Friedel_coverage 0.772 _reflns_Friedel_fraction_full 0.837 _reflns_Friedel_fraction_max 0.823 _reflns_number_gt 6096 _reflns_number_total 7090 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01349h2.cif _cod_data_source_block mf7 _cod_depositor_comments 'Adding full bibliography for 1557967--1557970.cif.' _cod_original_cell_volume 2047.35(15) _cod_database_code 1557969 _shelx_shelxl_version_number 2017/1 _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. ; _reflns_odcompleteness_completeness 99.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 71.98 _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 O1-C28 = O1-C25 = O4-C40 = O4-C43 = O2-C33 = O2-C30 = O3-C35 = O3-C38 1.43 with sigma of 0.01 O2-C33A = O2-C30A = O1-C25A = O1-C28A = O3-C35A = O3-C38A 1.43 with sigma of 0.01 O4A-C40A = O4A-C43A 1.43 with sigma of 0.01 C40-C41 = C41-C42 = C42-C43 = C43-C44 1.53 with sigma of 0.01 C28-C27 = C27-C26 = C26-C25 = C25-C29 1.53 with sigma of 0.01 C35-C36 = C36-C37 = C37-C38 = C38-C39 1.53 with sigma of 0.01 C33-C32 = C32-C31 = C31-C30 = C30-C34 1.53 with sigma of 0.01 C33A-C32A = C32A-C31A = C31A-C30A = C30A-C34A 1.53 with sigma of 0.01 C28A-C27A = C27A-C26A = C26A-C25A = C25A-C29A 1.53 with sigma of 0.01 C30A-C33A = C33A-C31A 2.3 with sigma of 0.02 C35A-C36A = C36A-C37A = C37A-C38A = C38A-C39A 1.53 with sigma of 0.01 C40A-C41A = C41A-C42A = C42A-C43A = C43A-C44A 1.53 with sigma of 0.01 C25A-C27A 2.3 with sigma of 0.02 C35A-C37A 2.3 with sigma of 0.02 C35A-C38A 2.3 with sigma of 0.02 O4A-C42A 2.35 with sigma of 0.02 C26A-C28A 2.3 with sigma of 0.02 3. Rigid bond restraints O4, C40, C41, C42, C43, C44 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 O3, C35, C36, C37, C38, C39 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 O2, C30, C31, C32, C33, C34 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 O1, C25, C26, C27, C28, C29 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 4. Uiso/Uaniso restraints and constraints O4 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02 O3 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02 O2 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02 O1 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02 Uanis(C33) = Uanis(C33A) Uanis(C32) = Uanis(C32A) Uanis(C31) = Uanis(C31A) Uanis(C30) = Uanis(C30A) Uanis(C34) = Uanis(C34A) Uanis(C28) = Uanis(C28A) Uanis(C27) = Uanis(C27A) Uanis(C26) = Uanis(C26A) Uanis(C25) = Uanis(C25A) Uanis(C29) = Uanis(C29A) Uanis(C35) = Uanis(C35A) Uanis(C36) = Uanis(C36A) Uanis(C37) = Uanis(C37A) Uanis(C38) = Uanis(C38A) Uanis(C39) = Uanis(C39A) Uanis(O4) = Uanis(O4A) Uanis(C44) = Uanis(C44A) Uanis(C43) = Uanis(C43A) Uanis(C42) = Uanis(C42A) Uanis(C40) = Uanis(C40A) Uanis(C41) = Uanis(C41A) 5. Others Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)= Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C25A)=Sof(H25A)=Sof(C27A)=Sof(H27C)= Sof(H27D)=1-FVAR(1) Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)= Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(1) Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(H31C)=Sof(H31D)=Sof(C32A)=Sof(H32C)= Sof(H32D)=Sof(C33A)=Sof(H33C)=Sof(H33D)=Sof(C34A)=Sof(H34D)=Sof(H34E)= Sof(H34F)=1-FVAR(2) Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)= Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(2) Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C37A)= Sof(H37C)=Sof(H37D)=Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(H39D)=Sof(H39E)= Sof(H39F)=1-FVAR(3) Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)= Sof(H37B)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(3) Sof(O4A)=Sof(C40A)=Sof(H40C)=Sof(H40D)=Sof(C41A)=Sof(C42A)=Sof(H42C)= Sof(H42D)=Sof(C44A)=Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(C43A)=1-FVAR(4) Sof(O4)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)= Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)= FVAR(4) 6.a Ternary CH refined with riding coordinates: C25(H25), C30(H30), C38(H38), C43(H43), C30A(H30A), C25A(H25A), C38A(H38A) 6.b Secondary CH2 refined with riding coordinates: C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C31(H31A,H31B), C32(H32A, H32B), C33(H33A,H33B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C31A(H31C,H31D), C32A(H32C, H32D), C33A(H33C,H33D), C28A(H28C,H28D), C26A(H26C,H26D), C27A(H27C,H27D), C35A(H35C,H35D), C36A(H36C,H36D), C37A(H37C,H37D), C40A(H40C,H40D), C42A(H42C, H42D) 6.c Me refined with riding coordinates: C34A(H34D,H34E,H34F), C44A(H44D,H44E,H44F) 6.d Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24) 6.e Idealised Me refined as rotating group: C29(H29A,H29B,H29C), C34(H34A,H34B,H34C), C39(H39A,H39B,H39C), C44(H44A,H44B, H44C), C29A(H29D,H29E,H29F), C39A(H39D,H39E,H39F) ; _shelx_res_file ; TITL mf7_a.res in P2(1) mf7.res created by SHELXL-2017/1 at 10:14:43 on 13-Jun-2019 CELL 1.54184 10.2268 19.0435 10.7658 90 102.453 90 ZERR 2 0.0004 0.0007 0.0005 0 0.004 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC Li O N C H UNIT 4 8 4 88 120 DFIX 1.43 0.01 O1 C28 O1 C25 O4 C40 O4 C43 O2 C33 O2 C30 O3 C35 O3 C38 DFIX 1.43 0.01 O2 C33A O2 C30A O1 C25A O1 C28A O3 C35A O3 C38A DFIX 1.43 0.01 O4A C40A O4A C43A DFIX 1.53 0.01 C40 C41 C41 C42 C42 C43 C43 C44 DFIX 1.53 0.01 C28 C27 C27 C26 C26 C25 C25 C29 DFIX 1.53 0.01 C35 C36 C36 C37 C37 C38 C38 C39 DFIX 1.53 0.01 C33 C32 C32 C31 C31 C30 C30 C34 DFIX 1.53 0.01 C33A C32A C32A C31A C31A C30A C30A C34A DFIX 1.53 0.01 C28A C27A C27A C26A C26A C25A C25A C29A DFIX 2.3 C30A C33A C33A C31A DFIX 1.53 0.01 C35A C36A C36A C37A C37A C38A C38A C39A DFIX 1.53 0.01 C40A C41A C41A C42A C42A C43A C43A C44A DFIX 2.3 C25A C27A DFIX 2.3 C35A C37A DFIX 2.3 C35A C38A DFIX 2.35 O4A C42A DFIX 2.3 C26A C28A DELU O4 C40 C41 C42 C43 C44 DELU O3 C35 C36 C37 C38 C39 DELU O2 C30 C31 C32 C33 C34 DELU O1 C25 C26 C27 C28 C29 SIMU 0.02 0.02 1.7 O4 C40 C41 C42 C43 C44 SIMU 0.02 0.02 1.7 O3 C35 C36 C37 C38 C39 SIMU 0.02 0.02 1.7 O2 C30 C31 C32 C33 C34 SIMU 0.02 0.02 1.7 O1 C25 C26 C27 C28 C29 EADP C33 C33A EADP C32 C32A EADP C31 C31A EADP C30 C30A EADP C34 C34A EADP C28 C28A EADP C27 C27A EADP C26 C26A EADP C25 C25A EADP C29 C29A EADP C35 C35A EADP C36 C36A EADP C37 C37A EADP C38 C38A EADP C39 C39A EADP O4 O4A EADP C44 C44A EADP C43 C43A EADP C42 C42A EADP C40 C40A EADP C41 C41A L.S. 12 PLAN 20 TEMP -150 FREE C12 Li2 BOND $H CONF LIST 4 fmap 2 ACTA MERG 2 OMIT -3 140 REM REM REM WGHT 0.200000 FVAR 0.72199 0.72162 0.43830 0.65429 0.71526 LI1 1 -0.602314 -0.426957 -0.761602 11.00000 0.04119 0.04442 = 0.04059 0.00114 0.01078 -0.00041 LI2 1 -0.764362 -0.531100 -0.795067 11.00000 0.04147 0.05011 = 0.06857 -0.00395 0.02593 0.00170 O1 2 -0.886553 -0.604349 -0.799461 11.00000 0.05450 0.05406 = 0.11259 0.01297 0.02929 -0.00549 O2 2 -0.577215 -0.354520 -0.886024 11.00000 0.06970 0.05334 = 0.05630 0.01873 0.00146 -0.00968 O3 2 -0.474735 -0.397774 -0.602949 11.00000 0.06320 0.06256 = 0.05957 0.00817 -0.01819 -0.00935 N1 3 -0.810226 -0.432045 -0.748975 11.00000 0.04023 0.04657 = 0.04014 0.00152 0.01212 0.00851 N2 3 -0.573104 -0.534162 -0.812933 11.00000 0.03687 0.04200 = 0.04542 -0.00196 0.01352 0.00542 C1 4 -0.832595 -0.407653 -0.633192 11.00000 0.03671 0.04314 = 0.04549 -0.00006 0.01284 0.00198 C2 4 -0.857954 -0.336314 -0.612346 11.00000 0.05651 0.04736 = 0.04832 -0.00011 0.01736 0.00357 AFIX 43 H2 5 -0.865777 -0.304114 -0.680955 11.00000 -1.20000 AFIX 0 C3 4 -0.871776 -0.311857 -0.494778 11.00000 0.06232 0.04836 = 0.05748 -0.00938 0.01979 0.00157 AFIX 43 H3 5 -0.889964 -0.263573 -0.484105 11.00000 -1.20000 AFIX 0 C4 4 -0.859146 -0.357702 -0.392016 11.00000 0.07569 0.06343 = 0.05045 -0.01091 0.02304 0.00780 AFIX 43 H4 5 -0.866209 -0.340996 -0.310574 11.00000 -1.20000 AFIX 0 C5 4 -0.836348 -0.427316 -0.410874 11.00000 0.08876 0.07051 = 0.04904 0.01013 0.03417 0.01942 AFIX 43 H5 5 -0.827897 -0.459096 -0.341577 11.00000 -1.20000 AFIX 0 C6 4 -0.825262 -0.452561 -0.530011 11.00000 0.06289 0.05013 = 0.04885 0.00240 0.02714 0.01221 AFIX 43 H6 5 -0.812449 -0.501409 -0.540781 11.00000 -1.20000 AFIX 0 C7 4 -0.904849 -0.416618 -0.858711 11.00000 0.03704 0.03922 = 0.04573 0.00481 0.01086 -0.00210 C8 4 -1.034093 -0.389466 -0.863372 11.00000 0.04513 0.05360 = 0.06080 -0.00245 0.00734 0.00480 AFIX 43 H8 5 -1.060080 -0.377405 -0.786534 11.00000 -1.20000 AFIX 0 C9 4 -1.122180 -0.380312 -0.976712 11.00000 0.04899 0.07283 = 0.08562 0.00303 -0.00468 0.01557 AFIX 43 H9 5 -1.208744 -0.362200 -0.976755 11.00000 -1.20000 AFIX 0 C10 4 -1.089473 -0.396684 -1.093082 11.00000 0.06937 0.07834 = 0.05596 0.00843 -0.01522 -0.00214 AFIX 43 H10 5 -1.152197 -0.389664 -1.171104 11.00000 -1.20000 AFIX 0 C11 4 -0.964890 -0.423028 -1.091340 11.00000 0.07588 0.06312 = 0.04536 0.00530 0.00546 -0.01168 AFIX 43 H11 5 -0.941050 -0.435383 -1.169041 11.00000 -1.20000 AFIX 0 C12 4 -0.873508 -0.431868 -0.978210 11.00000 0.04990 0.05056 = 0.04565 -0.00052 0.01075 -0.00273 AFIX 43 H12 5 -0.786526 -0.448735 -0.980058 11.00000 -1.20000 AFIX 0 C13 4 -0.521052 -0.579394 -0.715794 11.00000 0.03661 0.04265 = 0.04410 -0.00650 0.00658 -0.00231 C14 4 -0.549823 -0.569466 -0.595149 11.00000 0.05333 0.04679 = 0.04099 -0.00271 0.00722 -0.00138 AFIX 43 H14 5 -0.598232 -0.528718 -0.581084 11.00000 -1.20000 AFIX 0 C15 4 -0.510426 -0.616848 -0.494874 11.00000 0.08690 0.06494 = 0.04577 0.00282 0.00283 -0.01357 AFIX 43 H15 5 -0.534086 -0.608281 -0.415604 11.00000 -1.20000 AFIX 0 C16 4 -0.437446 -0.675959 -0.510122 11.00000 0.09210 0.05869 = 0.06958 0.01633 -0.01113 -0.00058 AFIX 43 H16 5 -0.408632 -0.708039 -0.442153 11.00000 -1.20000 AFIX 0 C17 4 -0.407410 -0.686894 -0.629760 11.00000 0.07472 0.05189 = 0.08642 -0.00150 0.00106 0.01021 AFIX 43 H17 5 -0.358792 -0.727706 -0.643065 11.00000 -1.20000 AFIX 0 C18 4 -0.445972 -0.640631 -0.727611 11.00000 0.04998 0.04631 = 0.06284 -0.01109 0.00917 0.00694 AFIX 43 H18 5 -0.421638 -0.649798 -0.806378 11.00000 -1.20000 AFIX 0 C19 4 -0.525891 -0.538690 -0.924981 11.00000 0.04415 0.04284 = 0.04804 -0.00760 0.01410 -0.00354 C20 4 -0.388008 -0.531463 -0.925856 11.00000 0.04784 0.07308 = 0.05487 -0.00993 0.02091 -0.00725 AFIX 43 H20 5 -0.325017 -0.525970 -0.847544 11.00000 -1.20000 AFIX 0 C21 4 -0.343183 -0.532249 -1.038818 11.00000 0.06884 0.09179 = 0.07554 -0.01937 0.04010 -0.01817 AFIX 43 H21 5 -0.250060 -0.528868 -1.036760 11.00000 -1.20000 AFIX 0 C22 4 -0.434416 -0.537991 -1.155587 11.00000 0.09395 0.08777 = 0.06121 -0.01459 0.04131 -0.01794 AFIX 43 H22 5 -0.404550 -0.536454 -1.233206 11.00000 -1.20000 AFIX 0 C23 4 -0.568539 -0.545926 -1.155905 11.00000 0.08116 0.08334 = 0.04670 -0.01589 0.01943 -0.00880 AFIX 43 H23 5 -0.631465 -0.549953 -1.234591 11.00000 -1.20000 AFIX 0 C24 4 -0.612765 -0.548106 -1.043025 11.00000 0.05369 0.06159 = 0.04542 -0.01072 0.01207 -0.00579 AFIX 43 H24 5 -0.705043 -0.556259 -1.046045 11.00000 -1.20000 AFIX 0 PART 1 C25 4 -0.842135 -0.675132 -0.767548 21.00000 0.07550 0.05715 = 0.08464 0.01192 0.02177 -0.00425 AFIX 13 H25 5 -0.769911 -0.674527 -0.688421 21.00000 -1.20000 AFIX 0 C26 4 -0.965385 -0.711111 -0.739835 21.00000 0.11043 0.06371 = 0.12880 0.01405 0.05552 -0.02170 AFIX 23 H26A 5 -0.985306 -0.754314 -0.791608 21.00000 -1.20000 H26B 5 -0.949521 -0.724323 -0.648873 21.00000 -1.20000 AFIX 0 C27 4 -1.081480 -0.660718 -0.772140 21.00000 0.08400 0.08938 = 0.18344 0.01341 0.04991 -0.02372 AFIX 23 H27A 5 -1.142446 -0.674485 -0.852931 21.00000 -1.20000 H27B 5 -1.132717 -0.660374 -0.703914 21.00000 -1.20000 AFIX 0 C28 4 -1.022554 -0.590018 -0.784656 21.00000 0.05258 0.08244 = 0.17549 0.02040 0.03426 -0.00216 AFIX 23 H28A 5 -1.074303 -0.564858 -0.859841 21.00000 -1.20000 H28B 5 -1.021448 -0.561277 -0.707810 21.00000 -1.20000 AFIX 0 C29 4 -0.785987 -0.700842 -0.874967 21.00000 0.08133 0.07247 = 0.08989 -0.00502 0.02188 -0.01040 AFIX 137 H29A 5 -0.853819 -0.696797 -0.954254 21.00000 -1.50000 H29B 5 -0.759454 -0.750124 -0.860514 21.00000 -1.50000 H29C 5 -0.707533 -0.672620 -0.881216 21.00000 -1.50000 AFIX 0 C30 4 -0.649889 -0.290823 -0.885827 31.00000 0.09972 0.04820 = 0.11524 0.01029 0.02449 -0.00454 AFIX 13 H30 5 -0.732653 -0.292235 -0.850551 31.00000 -1.20000 AFIX 0 C31 4 -0.665933 -0.271276 -1.026916 31.00000 0.10754 0.08537 = 0.09896 0.02025 0.02602 -0.00048 AFIX 23 H31A 5 -0.622207 -0.225435 -1.033320 31.00000 -1.20000 H31B 5 -0.762348 -0.266176 -1.066070 31.00000 -1.20000 AFIX 0 C32 4 -0.604309 -0.326820 -1.100890 31.00000 0.11452 0.11022 = 0.07329 0.02750 0.03920 -0.00385 AFIX 23 H32A 5 -0.665875 -0.365844 -1.134238 31.00000 -1.20000 H32B 5 -0.562949 -0.306983 -1.168266 31.00000 -1.20000 AFIX 0 C33 4 -0.505747 -0.344238 -0.980527 31.00000 0.04811 0.08581 = 0.10111 0.03933 0.02898 -0.01947 AFIX 23 H33A 5 -0.455527 -0.387316 -0.992141 31.00000 -1.20000 H33B 5 -0.441028 -0.305302 -0.956826 31.00000 -1.20000 AFIX 0 C34 4 -0.555040 -0.229709 -0.847666 31.00000 0.16249 0.09410 = 0.17283 -0.04787 0.06237 -0.03460 AFIX 137 H34A 5 -0.546849 -0.219601 -0.757057 31.00000 -1.50000 H34B 5 -0.590040 -0.188241 -0.897868 31.00000 -1.50000 H34C 5 -0.466838 -0.241727 -0.863373 31.00000 -1.50000 AFIX 0 C35 4 -0.500942 -0.380728 -0.475487 41.00000 0.08188 0.08813 = 0.06771 -0.01913 -0.03284 0.04881 AFIX 23 H35A 5 -0.528558 -0.424059 -0.437267 41.00000 -1.20000 H35B 5 -0.576108 -0.346943 -0.486044 41.00000 -1.20000 AFIX 0 C36 4 -0.381728 -0.350087 -0.386612 41.00000 0.09645 0.15727 = 0.08040 -0.03860 -0.01891 0.02033 AFIX 23 H36A 5 -0.385253 -0.354407 -0.295752 41.00000 -1.20000 H36B 5 -0.361694 -0.301186 -0.407580 41.00000 -1.20000 AFIX 0 C37 4 -0.291197 -0.404994 -0.430717 41.00000 0.07196 0.18650 = 0.07402 -0.01713 0.00091 0.02494 AFIX 23 H37A 5 -0.199795 -0.385478 -0.420724 41.00000 -1.20000 H37B 5 -0.285553 -0.447110 -0.375906 41.00000 -1.20000 AFIX 0 C38 4 -0.342717 -0.426286 -0.568022 41.00000 0.05566 0.09863 = 0.09677 -0.01171 0.00408 0.00232 AFIX 13 H38 5 -0.340012 -0.478176 -0.581490 41.00000 -1.20000 AFIX 0 C39 4 -0.273374 -0.385832 -0.652739 41.00000 0.11837 0.14301 = 0.10014 0.00014 0.04745 0.01552 AFIX 137 H39A 5 -0.325815 -0.388082 -0.740319 41.00000 -1.50000 H39B 5 -0.184417 -0.405970 -0.648962 41.00000 -1.50000 H39C 5 -0.264146 -0.336758 -0.624817 41.00000 -1.50000 AFIX 0 O4 2 -0.001696 -0.631129 -0.434132 51.00000 0.10441 0.11327 = 0.13515 -0.00256 0.02748 0.00669 C40 4 -0.106217 -0.582499 -0.427686 51.00000 0.08175 0.08814 = 0.13345 -0.01813 0.01345 -0.00359 AFIX 23 H40A 5 -0.188470 -0.593739 -0.491862 51.00000 -1.20000 H40B 5 -0.078476 -0.533823 -0.441507 51.00000 -1.20000 AFIX 0 C41 4 -0.128631 -0.591783 -0.293481 51.00000 0.08903 0.13374 = 0.13299 -0.03346 0.01768 -0.02317 AFIX 23 H41A 5 -0.213555 -0.617211 -0.295784 51.00000 -1.20000 H41B 5 -0.134032 -0.545386 -0.253412 51.00000 -1.20000 AFIX 0 C42 4 -0.010566 -0.633773 -0.217211 51.00000 0.12118 0.13153 = 0.10826 -0.03186 -0.00136 -0.03340 AFIX 23 H42A 5 0.028930 -0.611312 -0.134720 51.00000 -1.20000 H42B 5 -0.035401 -0.682909 -0.203034 51.00000 -1.20000 AFIX 0 C43 4 0.080148 -0.628753 -0.310096 51.00000 0.08681 0.10869 = 0.16829 -0.00632 0.00769 0.00018 AFIX 13 H43 5 0.137005 -0.585546 -0.296175 51.00000 -1.20000 AFIX 0 C44 4 0.163114 -0.695368 -0.279002 51.00000 0.13821 0.09821 = 0.21802 -0.03009 -0.02053 0.02049 AFIX 137 H44A 5 0.198038 -0.709499 -0.353163 51.00000 -1.50000 H44B 5 0.106776 -0.732980 -0.256943 51.00000 -1.50000 H44C 5 0.237922 -0.686498 -0.206889 51.00000 -1.50000 AFIX 0 PART 0 PART 2 C30A 4 -0.554540 -0.282044 -0.854609 -31.00000 0.09972 0.04820 = 0.11524 0.01029 0.02449 -0.00454 AFIX 13 H30A 5 -0.500373 -0.279182 -0.765552 -31.00000 -1.20000 AFIX 0 C31A 4 -0.469109 -0.255711 -0.942497 -31.00000 0.10754 0.08537 = 0.09896 0.02025 0.02602 -0.00048 AFIX 23 H31C 5 -0.373387 -0.266516 -0.908493 -31.00000 -1.20000 H31D 5 -0.479625 -0.204404 -0.955793 -31.00000 -1.20000 AFIX 0 C32A 4 -0.523166 -0.295951 -1.066311 -31.00000 0.11452 0.11022 = 0.07329 0.02750 0.03920 -0.00385 AFIX 23 H32C 5 -0.607046 -0.275003 -1.115579 -31.00000 -1.20000 H32D 5 -0.456328 -0.298761 -1.120352 -31.00000 -1.20000 AFIX 0 C33A 4 -0.547178 -0.366362 -1.011743 -31.00000 0.04811 0.08581 = 0.10111 0.03933 0.02898 -0.01947 AFIX 23 H33C 5 -0.623274 -0.390353 -1.068235 -31.00000 -1.20000 H33D 5 -0.466655 -0.396301 -1.003787 -31.00000 -1.20000 AFIX 0 C34A 4 -0.693261 -0.259658 -0.853243 -31.00000 0.16249 0.09410 = 0.17283 -0.04787 0.06237 -0.03460 AFIX 33 H34D 5 -0.693708 -0.209569 -0.832453 -31.00000 -1.50000 H34E 5 -0.751095 -0.267816 -0.937201 -31.00000 -1.50000 H34F 5 -0.726559 -0.286809 -0.789171 -31.00000 -1.50000 AFIX 0 C28A 4 -1.006362 -0.593939 -0.750780 -21.00000 0.05258 0.08244 = 0.17549 0.02040 0.03426 -0.00216 AFIX 23 H28C 5 -1.036214 -0.544380 -0.758979 -21.00000 -1.20000 H28D 5 -0.993003 -0.608633 -0.660710 -21.00000 -1.20000 AFIX 0 C29A 4 -0.762091 -0.708460 -0.808430 -21.00000 0.08133 0.07247 = 0.08989 -0.00502 0.02188 -0.01040 AFIX 137 H29D 5 -0.693102 -0.671966 -0.789404 -21.00000 -1.50000 H29E 5 -0.744014 -0.738989 -0.876062 -21.00000 -1.50000 H29F 5 -0.761105 -0.736435 -0.731831 -21.00000 -1.50000 AFIX 0 C26A 4 -1.017526 -0.708147 -0.810546 -21.00000 0.11043 0.06371 = 0.12880 0.01405 0.05552 -0.02170 AFIX 23 H26C 5 -0.997703 -0.721562 -0.719566 -21.00000 -1.20000 H26D 5 -1.054893 -0.748643 -0.864285 -21.00000 -1.20000 AFIX 0 C25A 4 -0.898286 -0.674414 -0.851727 -21.00000 0.07550 0.05715 = 0.08464 0.01192 0.02177 -0.00425 AFIX 13 H25A 5 -0.918859 -0.670966 -0.946642 -21.00000 -1.20000 AFIX 0 C27A 4 -1.104895 -0.642071 -0.838215 -21.00000 0.08400 0.08938 = 0.18344 0.01341 0.04991 -0.02372 AFIX 23 H27C 5 -1.120916 -0.627570 -0.928545 -21.00000 -1.20000 H27D 5 -1.191094 -0.646863 -0.811247 -21.00000 -1.20000 AFIX 0 C35A 4 -0.525751 -0.363155 -0.503008 -41.00000 0.08188 0.08813 = 0.06771 -0.01913 -0.03284 0.04881 AFIX 23 H35C 5 -0.598038 -0.390372 -0.477290 -41.00000 -1.20000 H35D 5 -0.557041 -0.314807 -0.526739 -41.00000 -1.20000 AFIX 0 C36A 4 -0.397084 -0.364140 -0.402218 -41.00000 0.09645 0.15727 = 0.08040 -0.03860 -0.01891 0.02033 AFIX 23 H36C 5 -0.364844 -0.412474 -0.379740 -41.00000 -1.20000 H36D 5 -0.405536 -0.338358 -0.324482 -41.00000 -1.20000 AFIX 0 C37A 4 -0.308634 -0.324868 -0.478614 -41.00000 0.07196 0.18650 = 0.07402 -0.01713 0.00091 0.02494 AFIX 23 H37C 5 -0.335449 -0.275156 -0.494358 -41.00000 -1.20000 H37D 5 -0.212167 -0.327824 -0.438310 -41.00000 -1.20000 AFIX 0 C38A 4 -0.345350 -0.369074 -0.596229 -41.00000 0.05566 0.09863 = 0.09677 -0.01171 0.00408 0.00232 AFIX 13 H38A 5 -0.359766 -0.333944 -0.666915 -41.00000 -1.20000 AFIX 0 C39A 4 -0.282578 -0.430125 -0.648914 -41.00000 0.11837 0.14301 = 0.10014 0.00014 0.04745 0.01552 AFIX 137 H39D 5 -0.345638 -0.449056 -0.723015 -41.00000 -1.50000 H39E 5 -0.260126 -0.466669 -0.583702 -41.00000 -1.50000 H39F 5 -0.200892 -0.414603 -0.674504 -41.00000 -1.50000 AFIX 0 O4A 2 0.096777 -0.620933 -0.387932 -51.00000 0.10441 0.11327 = 0.13515 -0.00256 0.02748 0.00669 C40A 4 0.162521 -0.686106 -0.352526 -51.00000 0.08175 0.08814 = 0.13345 -0.01813 0.01345 -0.00359 AFIX 23 H40C 5 0.261391 -0.683119 -0.328092 -51.00000 -1.20000 H40D 5 0.132615 -0.725111 -0.412746 -51.00000 -1.20000 AFIX 0 C41A 4 0.091213 -0.682274 -0.240194 -51.00000 0.08903 0.13374 = 0.13299 -0.03346 0.01768 -0.02317 C42A 4 -0.049953 -0.651509 -0.255686 -51.00000 0.12118 0.13153 = 0.10826 -0.03186 -0.00136 -0.03340 AFIX 23 H42C 5 -0.120324 -0.675697 -0.318730 -51.00000 -1.20000 H42D 5 -0.078609 -0.641890 -0.175183 -51.00000 -1.20000 AFIX 0 C44A 4 -0.106469 -0.547125 -0.367189 -51.00000 0.13821 0.09821 = 0.21802 -0.03009 -0.02053 0.02049 AFIX 33 H44D 5 -0.149268 -0.529907 -0.299913 -51.00000 -1.50000 H44E 5 -0.079902 -0.507157 -0.413520 -51.00000 -1.50000 H44F 5 -0.169668 -0.576694 -0.426113 -51.00000 -1.50000 AFIX 0 C43A 4 0.017860 -0.590354 -0.307742 -51.00000 0.08681 0.10869 = 0.16829 -0.00632 0.00769 0.00018 HKLF 4 REM mf7_a.res in P2(1) REM R1 = 0.0987 for 6096 Fo > 4sig(Fo) and 0.1080 for all 7090 data REM 542 parameters refined using 252 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.723, deepest hole -0.335, 1-sigma level 0.069 Q1 1 -0.4572 -0.4066 -0.3965 11.00000 0.05 0.72 Q2 1 -0.6048 -0.2529 -0.7918 11.00000 0.05 0.56 Q3 1 -0.2440 -0.4443 -0.5672 11.00000 0.05 0.50 Q4 1 -0.2292 -0.3729 -0.5417 11.00000 0.05 0.47 Q5 1 -0.6348 -0.2799 -0.8299 11.00000 0.05 0.46 Q6 1 -0.4379 -0.3600 -0.5142 11.00000 0.05 0.42 Q7 1 -0.5512 -0.3625 -1.0470 11.00000 0.05 0.39 Q8 1 -0.3238 -0.4077 -0.6428 11.00000 0.05 0.39 Q9 1 -0.3097 -0.3231 -0.5175 11.00000 0.05 0.37 Q10 1 -1.1169 -0.3992 -1.0528 11.00000 0.05 0.31 Q11 1 -0.8977 -0.4105 -0.8879 11.00000 0.05 0.31 Q12 1 -1.0183 -0.7029 -0.8846 11.00000 0.05 0.30 Q13 1 -0.4191 -0.4093 -0.5010 11.00000 0.05 0.29 Q14 1 -0.8444 -0.6204 -0.8399 11.00000 0.05 0.28 Q15 1 -0.0681 -0.6298 -0.3535 11.00000 0.05 0.28 Q16 1 -0.3900 -0.5142 -1.1028 11.00000 0.05 0.28 Q17 1 -0.8775 -0.4518 -0.4875 11.00000 0.05 0.26 Q18 1 -0.5817 -0.5883 -0.6561 11.00000 0.05 0.26 Q19 1 -0.4021 -0.6809 -0.5908 11.00000 0.05 0.26 Q20 1 -1.0221 -0.6493 -0.6862 11.00000 0.05 0.25 ; _shelx_res_checksum 89118 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' 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 Li1 Li -0.6023(7) -0.4270(4) -0.7616(7) 0.0418(15) Uani 1 1 d . . . . . Li2 Li -0.7644(8) -0.5311(5) -0.7951(9) 0.0513(18) Uani 1 1 d . . . . . O1 O -0.8866(4) -0.6043(2) -0.7995(6) 0.0720(13) Uani 1 1 d D U . . . O2 O -0.5772(4) -0.3545(2) -0.8860(4) 0.0616(10) Uani 1 1 d D U . . . O3 O -0.4747(4) -0.3978(2) -0.6029(4) 0.0665(11) Uani 1 1 d D U . . . N1 N -0.8102(4) -0.4320(2) -0.7490(4) 0.0418(8) Uani 1 1 d . . . . . N2 N -0.5731(3) -0.5342(2) -0.8129(4) 0.0407(8) Uani 1 1 d . . . . . C1 C -0.8326(4) -0.4077(3) -0.6332(4) 0.0412(9) Uani 1 1 d . . . . . C2 C -0.8580(5) -0.3363(3) -0.6123(5) 0.0498(11) Uani 1 1 d . . . . . H2 H -0.865777 -0.304114 -0.680955 0.060 Uiso 1 1 calc R . . . . C3 C -0.8718(6) -0.3119(3) -0.4948(6) 0.0550(12) Uani 1 1 d . . . . . H3 H -0.889964 -0.263573 -0.484105 0.066 Uiso 1 1 calc R . . . . C4 C -0.8591(7) -0.3577(4) -0.3920(6) 0.0618(14) Uani 1 1 d . . . . . H4 H -0.866209 -0.340996 -0.310574 0.074 Uiso 1 1 calc R . . . . C5 C -0.8363(7) -0.4273(4) -0.4109(6) 0.0665(16) Uani 1 1 d . . . . . H5 H -0.827897 -0.459096 -0.341577 0.080 Uiso 1 1 calc R . . . . C6 C -0.8253(5) -0.4526(3) -0.5300(5) 0.0517(12) Uani 1 1 d . . . . . H6 H -0.812449 -0.501409 -0.540781 0.062 Uiso 1 1 calc R . . . . C7 C -0.9048(4) -0.4166(2) -0.8587(4) 0.0404(9) Uani 1 1 d . . . . . C8 C -1.0341(5) -0.3895(3) -0.8634(6) 0.0538(12) Uani 1 1 d . . . . . H8 H -1.060080 -0.377405 -0.786534 0.065 Uiso 1 1 calc R . . . . C9 C -1.1222(6) -0.3803(4) -0.9767(7) 0.0720(18) Uani 1 1 d . . . . . H9 H -1.208744 -0.362200 -0.976755 0.086 Uiso 1 1 calc R . . . . C10 C -1.0895(7) -0.3967(4) -1.0931(6) 0.0722(18) Uani 1 1 d . . . . . H10 H -1.152197 -0.389664 -1.171104 0.087 Uiso 1 1 calc R . . . . C11 C -0.9649(7) -0.4230(4) -1.0913(5) 0.0626(14) Uani 1 1 d . . . . . H11 H -0.941050 -0.435383 -1.169041 0.075 Uiso 1 1 calc R . . . . C12 C -0.8735(5) -0.4319(3) -0.9782(5) 0.0486(10) Uani 1 1 d . . . . . H12 H -0.786526 -0.448735 -0.980058 0.058 Uiso 1 1 calc R . . . . C13 C -0.5211(4) -0.5794(3) -0.7158(4) 0.0414(9) Uani 1 1 d . . . . . C14 C -0.5498(5) -0.5695(3) -0.5951(5) 0.0475(10) Uani 1 1 d . . . . . H14 H -0.598232 -0.528718 -0.581084 0.057 Uiso 1 1 calc R . . . . C15 C -0.5104(8) -0.6168(4) -0.4949(6) 0.0676(16) Uani 1 1 d . . . . . H15 H -0.534086 -0.608281 -0.415604 0.081 Uiso 1 1 calc R . . . . C16 C -0.4374(8) -0.6760(4) -0.5101(7) 0.078(2) Uani 1 1 d . . . . . H16 H -0.408632 -0.708039 -0.442153 0.093 Uiso 1 1 calc R . . . . C17 C -0.4074(7) -0.6869(4) -0.6298(8) 0.0735(17) Uani 1 1 d . . . . . H17 H -0.358792 -0.727706 -0.643065 0.088 Uiso 1 1 calc R . . . . C18 C -0.4460(5) -0.6406(3) -0.7276(6) 0.0535(12) Uani 1 1 d . . . . . H18 H -0.421638 -0.649798 -0.806378 0.064 Uiso 1 1 calc R . . . . C19 C -0.5259(5) -0.5387(3) -0.9250(5) 0.0444(10) Uani 1 1 d . . . . . C20 C -0.3880(5) -0.5315(4) -0.9259(5) 0.0571(13) Uani 1 1 d . . . . . H20 H -0.325017 -0.525970 -0.847544 0.069 Uiso 1 1 calc R . . . . C21 C -0.3432(7) -0.5322(5) -1.0388(7) 0.0750(19) Uani 1 1 d . . . . . H21 H -0.250060 -0.528868 -1.036760 0.090 Uiso 1 1 calc R . . . . C22 C -0.4344(8) -0.5380(5) -1.1556(7) 0.0773(19) Uani 1 1 d . . . . . H22 H -0.404550 -0.536454 -1.233206 0.093 Uiso 1 1 calc R . . . . C23 C -0.5685(7) -0.5459(4) -1.1559(6) 0.0695(16) Uani 1 1 d . . . . . H23 H -0.631465 -0.549953 -1.234591 0.083 Uiso 1 1 calc R . . . . C24 C -0.6128(5) -0.5481(3) -1.0430(5) 0.0534(12) Uani 1 1 d . . . . . H24 H -0.705043 -0.556259 -1.046045 0.064 Uiso 1 1 calc R . . . . C25 C -0.8421(10) -0.6751(4) -0.7675(10) 0.072(2) Uani 0.722(11) 1 d D U P A 1 H25 H -0.769911 -0.674527 -0.688421 0.086 Uiso 0.722(11) 1 calc R . P A 1 C26 C -0.9654(13) -0.7111(6) -0.7398(17) 0.096(4) Uani 0.722(11) 1 d D U P A 1 H26A H -0.985306 -0.754314 -0.791608 0.116 Uiso 0.722(11) 1 calc R . P A 1 H26B H -0.949521 -0.724323 -0.648873 0.116 Uiso 0.722(11) 1 calc R . P A 1 C27 C -1.0815(13) -0.6607(7) -0.772(2) 0.116(5) Uani 0.722(11) 1 d D U P A 1 H27A H -1.142446 -0.674485 -0.852931 0.139 Uiso 0.722(11) 1 calc R . P A 1 H27B H -1.132717 -0.660374 -0.703914 0.139 Uiso 0.722(11) 1 calc R . P A 1 C28 C -1.0226(12) -0.5900(8) -0.785(2) 0.102(5) Uani 0.722(11) 1 d D U P A 1 H28A H -1.074303 -0.564858 -0.859841 0.122 Uiso 0.722(11) 1 calc R . P A 1 H28B H -1.021448 -0.561277 -0.707810 0.122 Uiso 0.722(11) 1 calc R . P A 1 C29 C -0.7860(13) -0.7008(7) -0.8750(12) 0.081(3) Uani 0.722(11) 1 d D U P A 1 H29A H -0.853819 -0.696797 -0.954254 0.121 Uiso 0.722(11) 1 calc GR . P A 1 H29B H -0.759454 -0.750124 -0.860514 0.121 Uiso 0.722(11) 1 calc GR . P A 1 H29C H -0.707533 -0.672620 -0.881216 0.121 Uiso 0.722(11) 1 calc GR . P A 1 C30 C -0.6499(19) -0.2908(7) -0.8858(18) 0.088(3) Uani 0.438(8) 1 d D U P B 1 H30 H -0.732653 -0.292235 -0.850551 0.105 Uiso 0.438(8) 1 calc R . P B 1 C31 C -0.666(3) -0.2713(11) -1.0269(17) 0.097(3) Uani 0.438(8) 1 d D U P B 1 H31A H -0.622207 -0.225435 -1.033320 0.116 Uiso 0.438(8) 1 calc R . P B 1 H31B H -0.762348 -0.266176 -1.066070 0.116 Uiso 0.438(8) 1 calc R . P B 1 C32 C -0.604(2) -0.3268(12) -1.1009(15) 0.096(4) Uani 0.438(8) 1 d D U P B 1 H32A H -0.665875 -0.365844 -1.134238 0.116 Uiso 0.438(8) 1 calc R . P B 1 H32B H -0.562949 -0.306983 -1.168266 0.116 Uiso 0.438(8) 1 calc R . P B 1 C33 C -0.5057(14) -0.3442(12) -0.9805(15) 0.076(3) Uani 0.438(8) 1 d D U P B 1 H33A H -0.455527 -0.387316 -0.992141 0.092 Uiso 0.438(8) 1 calc R . P B 1 H33B H -0.441028 -0.305302 -0.956826 0.092 Uiso 0.438(8) 1 calc R . P B 1 C34 C -0.555(4) -0.2297(16) -0.848(4) 0.139(6) Uani 0.438(8) 1 d D U P B 1 H34A H -0.546849 -0.219601 -0.757057 0.209 Uiso 0.438(8) 1 calc GR . P B 1 H34B H -0.590040 -0.188241 -0.897868 0.209 Uiso 0.438(8) 1 calc GR . P B 1 H34C H -0.466838 -0.241727 -0.863373 0.209 Uiso 0.438(8) 1 calc GR . P B 1 C35 C -0.5009(12) -0.3807(8) -0.4755(9) 0.087(4) Uani 0.654(11) 1 d D U P C 1 H35A H -0.528558 -0.424059 -0.437267 0.104 Uiso 0.654(11) 1 calc R . P C 1 H35B H -0.576108 -0.346943 -0.486044 0.104 Uiso 0.654(11) 1 calc R . P C 1 C36 C -0.3817(17) -0.3501(13) -0.3866(18) 0.117(5) Uani 0.654(11) 1 d D U P C 1 H36A H -0.385253 -0.354407 -0.295752 0.141 Uiso 0.654(11) 1 calc R . P C 1 H36B H -0.361694 -0.301186 -0.407580 0.141 Uiso 0.654(11) 1 calc R . P C 1 C37 C -0.2912(14) -0.4050(13) -0.4307(12) 0.113(4) Uani 0.654(11) 1 d D U P C 1 H37A H -0.199795 -0.385478 -0.420724 0.136 Uiso 0.654(11) 1 calc R . P C 1 H37B H -0.285553 -0.447110 -0.375906 0.136 Uiso 0.654(11) 1 calc R . P C 1 C38 C -0.3427(9) -0.4263(8) -0.5680(11) 0.086(3) Uani 0.654(11) 1 d D U P C 1 H38 H -0.340012 -0.478176 -0.581490 0.103 Uiso 0.654(11) 1 calc R . P C 1 C39 C -0.273(2) -0.3858(12) -0.653(2) 0.117(5) Uani 0.654(11) 1 d D U P C 1 H39A H -0.325815 -0.388082 -0.740319 0.175 Uiso 0.654(11) 1 calc GR . P C 1 H39B H -0.184417 -0.405970 -0.648962 0.175 Uiso 0.654(11) 1 calc GR . P C 1 H39C H -0.264146 -0.336758 -0.624817 0.175 Uiso 0.654(11) 1 calc GR . P C 1 O4 O -0.0017(11) -0.6311(6) -0.4341(12) 0.117(3) Uani 0.715(10) 1 d D U P D 1 C40 C -0.1062(13) -0.5825(8) -0.4277(14) 0.103(3) Uani 0.715(10) 1 d D U P D 1 H40A H -0.188470 -0.593739 -0.491862 0.123 Uiso 0.715(10) 1 calc R . P D 1 H40B H -0.078476 -0.533823 -0.441507 0.123 Uiso 0.715(10) 1 calc R . P D 1 C41 C -0.1286(14) -0.5918(10) -0.2935(14) 0.120(4) Uani 0.715(10) 1 d D U P D 1 H41A H -0.213555 -0.617211 -0.295784 0.143 Uiso 0.715(10) 1 calc R . P D 1 H41B H -0.134032 -0.545386 -0.253412 0.143 Uiso 0.715(10) 1 calc R . P D 1 C42 C -0.0106(16) -0.6338(11) -0.2172(15) 0.124(4) Uani 0.715(10) 1 d D U P D 1 H42A H 0.028930 -0.611312 -0.134720 0.149 Uiso 0.715(10) 1 calc R . P D 1 H42B H -0.035401 -0.682909 -0.203034 0.149 Uiso 0.715(10) 1 calc R . P D 1 C43 C 0.0801(14) -0.6288(10) -0.3101(15) 0.124(4) Uani 0.715(10) 1 d D U P D 1 H43 H 0.137005 -0.585546 -0.296175 0.149 Uiso 0.715(10) 1 calc R . P D 1 C44 C 0.163(3) -0.6954(11) -0.279(3) 0.160(8) Uani 0.715(10) 1 d D U P D 1 H44A H 0.198038 -0.709499 -0.353163 0.241 Uiso 0.715(10) 1 calc GR . P D 1 H44B H 0.106776 -0.732980 -0.256943 0.241 Uiso 0.715(10) 1 calc GR . P D 1 H44C H 0.237922 -0.686498 -0.206889 0.241 Uiso 0.715(10) 1 calc GR . P D 1 C30A C -0.5545(16) -0.2820(5) -0.8546(15) 0.088(3) Uani 0.562(8) 1 d D . P B 2 H30A H -0.500373 -0.279182 -0.765552 0.105 Uiso 0.562(8) 1 calc R . P B 2 C31A C -0.4691(18) -0.2557(8) -0.9425(14) 0.097(3) Uani 0.562(8) 1 d D . P B 2 H31C H -0.373387 -0.266516 -0.908493 0.116 Uiso 0.562(8) 1 calc R . P B 2 H31D H -0.479625 -0.204404 -0.955793 0.116 Uiso 0.562(8) 1 calc R . P B 2 C32A C -0.523(2) -0.2960(8) -1.0663(13) 0.096(4) Uani 0.562(8) 1 d D . P B 2 H32C H -0.607046 -0.275003 -1.115579 0.116 Uiso 0.562(8) 1 calc R . P B 2 H32D H -0.456328 -0.298761 -1.120352 0.116 Uiso 0.562(8) 1 calc R . P B 2 C33A C -0.5472(14) -0.3664(6) -1.0117(11) 0.076(3) Uani 0.562(8) 1 d D . P B 2 H33C H -0.623274 -0.390353 -1.068235 0.092 Uiso 0.562(8) 1 calc R . P B 2 H33D H -0.466655 -0.396301 -1.003787 0.092 Uiso 0.562(8) 1 calc R . P B 2 C34A C -0.6933(19) -0.2597(12) -0.853(3) 0.139(6) Uani 0.562(8) 1 d D . P B 2 H34D H -0.693708 -0.209569 -0.832453 0.209 Uiso 0.562(8) 1 calc R . P B 2 H34E H -0.751095 -0.267816 -0.937201 0.209 Uiso 0.562(8) 1 calc R . P B 2 H34F H -0.726559 -0.286809 -0.789171 0.209 Uiso 0.562(8) 1 calc R . P B 2 C28A C -1.006(3) -0.594(2) -0.751(5) 0.102(5) Uani 0.278(11) 1 d D . P A 2 H28C H -1.036214 -0.544380 -0.758979 0.122 Uiso 0.278(11) 1 calc R . P A 2 H28D H -0.993003 -0.608633 -0.660710 0.122 Uiso 0.278(11) 1 calc R . P A 2 C29A C -0.762(3) -0.7085(18) -0.808(4) 0.081(3) Uani 0.278(11) 1 d D . P A 2 H29D H -0.693102 -0.671966 -0.789404 0.121 Uiso 0.278(11) 1 calc GR . P A 2 H29E H -0.744014 -0.738989 -0.876062 0.121 Uiso 0.278(11) 1 calc GR . P A 2 H29F H -0.761105 -0.736435 -0.731831 0.121 Uiso 0.278(11) 1 calc GR . P A 2 C26A C -1.018(3) -0.7081(13) -0.811(4) 0.096(4) Uani 0.278(11) 1 d D . P A 2 H26C H -0.997703 -0.721562 -0.719566 0.116 Uiso 0.278(11) 1 calc R . P A 2 H26D H -1.054893 -0.748643 -0.864285 0.116 Uiso 0.278(11) 1 calc R . P A 2 C25A C -0.898(2) -0.6744(8) -0.852(3) 0.072(2) Uani 0.278(11) 1 d D . P A 2 H25A H -0.918859 -0.670966 -0.946642 0.086 Uiso 0.278(11) 1 calc R . P A 2 C27A C -1.105(3) -0.6421(18) -0.838(5) 0.116(5) Uani 0.278(11) 1 d D . P A 2 H27C H -1.120916 -0.627570 -0.928545 0.139 Uiso 0.278(11) 1 calc R . P A 2 H27D H -1.191094 -0.646863 -0.811247 0.139 Uiso 0.278(11) 1 calc R . P A 2 C35A C -0.526(2) -0.3632(15) -0.5030(18) 0.087(4) Uani 0.346(11) 1 d D . P C 2 H35C H -0.598038 -0.390372 -0.477290 0.104 Uiso 0.346(11) 1 calc R . P C 2 H35D H -0.557041 -0.314807 -0.526739 0.104 Uiso 0.346(11) 1 calc R . P C 2 C36A C -0.397(3) -0.364(3) -0.402(3) 0.117(5) Uani 0.346(11) 1 d D . P C 2 H36C H -0.364844 -0.412474 -0.379740 0.141 Uiso 0.346(11) 1 calc R . P C 2 H36D H -0.405536 -0.338358 -0.324482 0.141 Uiso 0.346(11) 1 calc R . P C 2 C37A C -0.309(2) -0.3249(19) -0.479(2) 0.113(4) Uani 0.346(11) 1 d D . P C 2 H37C H -0.335449 -0.275156 -0.494358 0.136 Uiso 0.346(11) 1 calc R . P C 2 H37D H -0.212167 -0.327824 -0.438310 0.136 Uiso 0.346(11) 1 calc R . P C 2 C38A C -0.3454(14) -0.3691(13) -0.596(2) 0.086(3) Uani 0.346(11) 1 d D . P C 2 H38A H -0.359766 -0.333944 -0.666915 0.103 Uiso 0.346(11) 1 calc R . P C 2 C39A C -0.283(5) -0.4301(19) -0.649(4) 0.117(5) Uani 0.346(11) 1 d D . P C 2 H39D H -0.345638 -0.449056 -0.723015 0.175 Uiso 0.346(11) 1 calc GR . P C 2 H39E H -0.260126 -0.466669 -0.583702 0.175 Uiso 0.346(11) 1 calc GR . P C 2 H39F H -0.200892 -0.414603 -0.674504 0.175 Uiso 0.346(11) 1 calc GR . P C 2 O4A O 0.097(3) -0.6209(16) -0.388(3) 0.117(3) Uani 0.285(10) 1 d D . P D 2 C40A C 0.163(4) -0.6861(19) -0.353(4) 0.103(3) Uani 0.285(10) 1 d D . P D 2 H40C H 0.261391 -0.683119 -0.328092 0.123 Uiso 0.285(10) 1 calc R . P D 2 H40D H 0.132615 -0.725111 -0.412746 0.123 Uiso 0.285(10) 1 calc R . P D 2 C41A C 0.091(3) -0.682(3) -0.240(4) 0.120(4) Uani 0.285(10) 1 d D . P D 2 C42A C -0.050(4) -0.652(2) -0.256(4) 0.124(4) Uani 0.285(10) 1 d D . P D 2 H42C H -0.120324 -0.675697 -0.318730 0.149 Uiso 0.285(10) 1 calc R . P D 2 H42D H -0.078609 -0.641890 -0.175183 0.149 Uiso 0.285(10) 1 calc R . P D 2 C44A C -0.106(5) -0.547(3) -0.367(7) 0.160(8) Uani 0.285(10) 1 d D . P D 2 H44D H -0.149268 -0.529907 -0.299913 0.241 Uiso 0.285(10) 1 calc R . P D 2 H44E H -0.079902 -0.507157 -0.413520 0.241 Uiso 0.285(10) 1 calc R . P D 2 H44F H -0.169668 -0.576694 -0.426113 0.241 Uiso 0.285(10) 1 calc R . P D 2 C43A C 0.018(3) -0.5904(17) -0.308(4) 0.124(4) Uani 0.285(10) 1 d D . P D 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 Li1 0.041(3) 0.044(4) 0.041(3) 0.001(3) 0.011(3) 0.000(3) Li2 0.041(3) 0.050(4) 0.069(5) -0.004(4) 0.026(3) 0.002(3) O1 0.054(2) 0.054(2) 0.113(4) 0.013(2) 0.029(2) -0.0055(17) O2 0.070(2) 0.053(2) 0.056(2) 0.0187(17) 0.0015(17) -0.0097(18) O3 0.063(2) 0.063(2) 0.060(2) 0.0082(19) -0.0182(17) -0.0093(19) N1 0.0402(16) 0.047(2) 0.0401(17) 0.0015(15) 0.0121(14) 0.0085(15) N2 0.0369(16) 0.0420(19) 0.0454(19) -0.0020(16) 0.0135(14) 0.0054(14) C1 0.0367(18) 0.043(2) 0.045(2) -0.0001(18) 0.0128(16) 0.0020(16) C2 0.057(3) 0.047(3) 0.048(2) 0.000(2) 0.017(2) 0.004(2) C3 0.062(3) 0.048(3) 0.057(3) -0.009(2) 0.020(2) 0.002(2) C4 0.076(3) 0.063(3) 0.050(3) -0.011(2) 0.023(2) 0.008(3) C5 0.089(4) 0.071(4) 0.049(3) 0.010(3) 0.034(3) 0.019(3) C6 0.063(3) 0.050(3) 0.049(3) 0.002(2) 0.027(2) 0.012(2) C7 0.0370(19) 0.039(2) 0.046(2) 0.0048(17) 0.0109(16) -0.0021(16) C8 0.045(2) 0.054(3) 0.061(3) -0.002(2) 0.007(2) 0.005(2) C9 0.049(3) 0.073(4) 0.086(4) 0.003(3) -0.005(3) 0.016(3) C10 0.069(3) 0.078(4) 0.056(3) 0.008(3) -0.015(3) -0.002(3) C11 0.076(3) 0.063(4) 0.045(2) 0.005(2) 0.005(2) -0.012(3) C12 0.050(2) 0.051(3) 0.046(2) -0.001(2) 0.0107(19) -0.003(2) C13 0.0366(19) 0.043(2) 0.044(2) -0.0065(18) 0.0066(16) -0.0023(17) C14 0.053(2) 0.047(3) 0.041(2) -0.0027(19) 0.0072(18) -0.0014(19) C15 0.087(4) 0.065(4) 0.046(3) 0.003(3) 0.003(3) -0.014(3) C16 0.092(5) 0.059(4) 0.070(4) 0.016(3) -0.011(3) -0.001(3) C17 0.075(4) 0.052(3) 0.086(5) -0.002(3) 0.001(3) 0.010(3) C18 0.050(2) 0.046(3) 0.063(3) -0.011(2) 0.009(2) 0.007(2) C19 0.044(2) 0.043(2) 0.048(2) -0.0076(19) 0.0141(18) -0.0035(18) C20 0.048(2) 0.073(4) 0.055(3) -0.010(3) 0.021(2) -0.007(2) C21 0.069(3) 0.092(5) 0.076(4) -0.019(4) 0.040(3) -0.018(3) C22 0.094(5) 0.088(5) 0.061(3) -0.015(3) 0.041(3) -0.018(4) C23 0.081(4) 0.083(5) 0.047(3) -0.016(3) 0.019(3) -0.009(3) C24 0.054(3) 0.062(3) 0.045(2) -0.011(2) 0.012(2) -0.006(2) C25 0.076(5) 0.057(4) 0.085(6) 0.012(4) 0.022(4) -0.004(4) C26 0.110(9) 0.064(5) 0.129(11) 0.014(7) 0.056(8) -0.022(5) C27 0.084(6) 0.089(8) 0.183(15) 0.013(9) 0.050(9) -0.024(5) C28 0.053(4) 0.082(5) 0.175(13) 0.020(7) 0.034(7) -0.002(4) C29 0.081(6) 0.072(6) 0.090(8) -0.005(7) 0.022(6) -0.010(5) C30 0.100(7) 0.048(5) 0.115(7) 0.010(5) 0.024(7) -0.005(5) C31 0.108(8) 0.085(7) 0.099(7) 0.020(6) 0.026(6) 0.000(6) C32 0.115(9) 0.110(10) 0.073(6) 0.027(6) 0.039(6) -0.004(7) C33 0.048(7) 0.086(9) 0.101(7) 0.039(6) 0.029(5) -0.019(5) C34 0.162(15) 0.094(9) 0.173(14) -0.048(11) 0.062(11) -0.035(10) C35 0.082(6) 0.088(8) 0.068(6) -0.019(6) -0.033(5) 0.049(5) C36 0.096(7) 0.157(12) 0.080(6) -0.039(7) -0.019(5) 0.020(7) C37 0.072(5) 0.186(13) 0.074(6) -0.017(7) 0.001(5) 0.025(7) C38 0.056(4) 0.099(7) 0.097(6) -0.012(6) 0.004(4) 0.002(5) C39 0.118(8) 0.143(15) 0.100(7) 0.000(12) 0.047(7) 0.016(13) O4 0.104(6) 0.113(7) 0.135(7) -0.003(6) 0.027(5) 0.007(6) C40 0.082(6) 0.088(7) 0.133(8) -0.018(7) 0.013(6) -0.004(5) C41 0.089(7) 0.134(11) 0.133(9) -0.033(9) 0.018(6) -0.023(7) C42 0.121(10) 0.132(12) 0.108(8) -0.032(8) -0.001(7) -0.033(8) C43 0.087(7) 0.109(9) 0.168(11) -0.006(10) 0.008(7) 0.000(6) C44 0.138(13) 0.098(10) 0.218(19) -0.030(13) -0.021(13) 0.020(9) C30A 0.100(7) 0.048(5) 0.115(7) 0.010(5) 0.024(7) -0.005(5) C31A 0.108(8) 0.085(7) 0.099(7) 0.020(6) 0.026(6) 0.000(6) C32A 0.115(9) 0.110(10) 0.073(6) 0.027(6) 0.039(6) -0.004(7) C33A 0.048(7) 0.086(9) 0.101(7) 0.039(6) 0.029(5) -0.019(5) C34A 0.162(15) 0.094(9) 0.173(14) -0.048(11) 0.062(11) -0.035(10) C28A 0.053(4) 0.082(5) 0.175(13) 0.020(7) 0.034(7) -0.002(4) C29A 0.081(6) 0.072(6) 0.090(8) -0.005(7) 0.022(6) -0.010(5) C26A 0.110(9) 0.064(5) 0.129(11) 0.014(7) 0.056(8) -0.022(5) C25A 0.076(5) 0.057(4) 0.085(6) 0.012(4) 0.022(4) -0.004(4) C27A 0.084(6) 0.089(8) 0.183(15) 0.013(9) 0.050(9) -0.024(5) C35A 0.082(6) 0.088(8) 0.068(6) -0.019(6) -0.033(5) 0.049(5) C36A 0.096(7) 0.157(12) 0.080(6) -0.039(7) -0.019(5) 0.020(7) C37A 0.072(5) 0.186(13) 0.074(6) -0.017(7) 0.001(5) 0.025(7) C38A 0.056(4) 0.099(7) 0.097(6) -0.012(6) 0.004(4) 0.002(5) C39A 0.118(8) 0.143(15) 0.100(7) 0.000(12) 0.047(7) 0.016(13) O4A 0.104(6) 0.113(7) 0.135(7) -0.003(6) 0.027(5) 0.007(6) C40A 0.082(6) 0.088(7) 0.133(8) -0.018(7) 0.013(6) -0.004(5) C41A 0.089(7) 0.134(11) 0.133(9) -0.033(9) 0.018(6) -0.023(7) C42A 0.121(10) 0.132(12) 0.108(8) -0.032(8) -0.001(7) -0.033(8) C44A 0.138(13) 0.098(10) 0.218(19) -0.030(13) -0.021(13) 0.020(9) C43A 0.087(7) 0.109(9) 0.168(11) -0.006(10) 0.008(7) 0.000(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 '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' 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 _geom_angle_publ_flag O2 Li1 Li2 128.3(4) . . ? O2 Li1 O3 103.3(4) . . ? O2 Li1 N1 110.3(4) . . ? O2 Li1 N2 116.2(4) . . ? O3 Li1 Li2 128.4(4) . . ? O3 Li1 N1 115.5(4) . . ? O3 Li1 N2 112.5(4) . . ? N1 Li1 Li2 50.1(3) . . ? N2 Li1 Li2 49.5(3) . . ? N2 Li1 N1 99.6(3) . . ? Li1 Li2 C7 72.2(3) . . ? Li1 Li2 C13 71.7(3) . . ? O1 Li2 Li1 172.8(5) . . ? O1 Li2 N1 120.8(4) . . ? O1 Li2 N2 129.6(5) . . ? O1 Li2 C7 106.8(4) . . ? O1 Li2 C13 109.3(4) . . ? N1 Li2 Li1 54.7(3) . . ? N1 Li2 C7 31.6(2) . . ? N1 Li2 C13 120.0(4) . . ? N2 Li2 Li1 54.6(3) . . ? N2 Li2 N1 109.4(5) . . ? N2 Li2 C7 119.3(4) . . ? N2 Li2 C13 31.1(2) . . ? C13 Li2 C7 143.8(4) . . ? C25 O1 Li2 121.2(5) . . ? C25 O1 C28 114.1(8) . . ? C28 O1 Li2 120.4(7) . . ? C28A O1 Li2 120.2(14) . . ? C25A O1 Li2 134.4(9) . . ? C25A O1 C28A 105.2(16) . . ? C30 O2 Li1 116.7(8) . . ? C33 O2 Li1 139.5(10) . . ? C33 O2 C30 103.8(12) . . ? C30A O2 Li1 123.5(7) . . ? C30A O2 C33A 108.1(7) . . ? C33A O2 Li1 126.9(6) . . ? C35 O3 Li1 129.5(6) . . ? C38 O3 Li1 121.8(6) . . ? C38 O3 C35 100.8(7) . . ? C35A O3 Li1 119.3(9) . . ? C38A O3 Li1 125.6(10) . . ? C38A O3 C35A 105.5(12) . . ? Li2 N1 Li1 75.2(3) . . ? C1 N1 Li1 113.2(3) . . ? C1 N1 Li2 128.2(4) . . ? C7 N1 Li1 116.9(3) . . ? C7 N1 Li2 98.3(4) . . ? C7 N1 C1 118.1(4) . . ? Li2 N2 Li1 75.9(4) . . ? C13 N2 Li1 116.9(4) . . ? C13 N2 Li2 99.9(4) . . ? C13 N2 C19 118.1(4) . . ? C19 N2 Li1 111.9(4) . . ? C19 N2 Li2 127.6(4) . . ? N1 C1 C2 122.3(4) . . ? C6 C1 N1 121.2(4) . . ? C6 C1 C2 116.4(4) . . ? C1 C2 H2 119.1 . . ? C3 C2 C1 121.9(5) . . ? C3 C2 H2 119.1 . . ? C2 C3 H3 119.8 . . ? C2 C3 C4 120.3(5) . . ? C4 C3 H3 119.8 . . ? C3 C4 H4 120.7 . . ? C5 C4 C3 118.6(5) . . ? C5 C4 H4 120.7 . . ? C4 C5 H5 119.3 . . ? C4 C5 C6 121.3(6) . . ? C6 C5 H5 119.3 . . ? C1 C6 C5 121.4(5) . . ? C1 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? N1 C7 Li2 50.1(3) . . ? N1 C7 C8 125.7(4) . . ? N1 C7 C12 118.4(4) . . ? C8 C7 Li2 140.5(4) . . ? C8 C7 C12 115.8(4) . . ? C12 C7 Li2 81.3(4) . . ? C7 C8 H8 119.6 . . ? C9 C8 C7 120.8(6) . . ? C9 C8 H8 119.6 . . ? C8 C9 H9 118.9 . . ? C8 C9 C10 122.2(6) . . ? C10 C9 H9 118.9 . . ? C9 C10 H10 120.9 . . ? C11 C10 C9 118.2(5) . . ? C11 C10 H10 120.9 . . ? C10 C11 H11 119.7 . . ? C10 C11 C12 120.7(6) . . ? C12 C11 H11 119.7 . . ? C7 C12 H12 118.9 . . ? C11 C12 C7 122.2(5) . . ? C11 C12 H12 118.9 . . ? N2 C13 Li2 49.1(3) . . ? N2 C13 C14 119.8(4) . . ? N2 C13 C18 125.3(4) . . ? C14 C13 Li2 83.1(3) . . ? C14 C13 C18 114.8(5) . . ? C18 C13 Li2 139.1(4) . . ? C13 C14 H14 118.5 . . ? C15 C14 C13 123.0(5) . . ? C15 C14 H14 118.5 . . ? C14 C15 H15 119.7 . . ? C16 C15 C14 120.5(6) . . ? C16 C15 H15 119.7 . . ? C15 C16 H16 121.3 . . ? C15 C16 C17 117.5(6) . . ? C17 C16 H16 121.3 . . ? C16 C17 H17 119.0 . . ? C18 C17 C16 121.9(6) . . ? C18 C17 H17 119.0 . . ? C13 C18 H18 118.9 . . ? C17 C18 C13 122.3(6) . . ? C17 C18 H18 118.9 . . ? N2 C19 C20 122.0(4) . . ? N2 C19 C24 121.6(4) . . ? C24 C19 C20 116.4(5) . . ? C19 C20 H20 119.3 . . ? C21 C20 C19 121.4(5) . . ? C21 C20 H20 119.3 . . ? C20 C21 H21 119.8 . . ? C20 C21 C22 120.4(6) . . ? C22 C21 H21 119.8 . . ? C21 C22 H22 120.6 . . ? C23 C22 C21 118.8(6) . . ? C23 C22 H22 120.6 . . ? C22 C23 H23 119.5 . . ? C22 C23 C24 120.9(6) . . ? C24 C23 H23 119.5 . . ? C19 C24 H24 119.0 . . ? C23 C24 C19 122.0(5) . . ? C23 C24 H24 119.0 . . ? O1 C25 H25 109.2 . . ? O1 C25 C26 103.7(8) . . ? O1 C25 C29 106.2(8) . . ? C26 C25 H25 109.2 . . ? C29 C25 H25 109.2 . . ? C29 C25 C26 118.8(10) . . ? C25 C26 H26A 110.1 . . ? C25 C26 H26B 110.1 . . ? H26A C26 H26B 108.4 . . ? C27 C26 C25 108.2(9) . . ? C27 C26 H26A 110.1 . . ? C27 C26 H26B 110.1 . . ? C26 C27 H27A 110.5 . . ? C26 C27 H27B 110.5 . . ? H27A C27 H27B 108.6 . . ? C28 C27 C26 106.4(10) . . ? C28 C27 H27A 110.5 . . ? C28 C27 H27B 110.5 . . ? O1 C28 C27 104.7(10) . . ? O1 C28 H28A 110.8 . . ? O1 C28 H28B 110.8 . . ? C27 C28 H28A 110.8 . . ? C27 C28 H28B 110.8 . . ? H28A C28 H28B 108.9 . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O2 C30 H30 117.6 . . ? O2 C30 C31 98.6(13) . . ? O2 C30 C34 110.6(19) . . ? C31 C30 H30 117.6 . . ? C34 C30 H30 117.6 . . ? C34 C30 C31 90(2) . . ? C30 C31 H31A 109.2 . . ? C30 C31 H31B 109.2 . . ? C30 C31 C32 112.1(14) . . ? H31A C31 H31B 107.9 . . ? C32 C31 H31A 109.2 . . ? C32 C31 H31B 109.2 . . ? C31 C32 H32A 113.9 . . ? C31 C32 H32B 113.9 . . ? H32A C32 H32B 111.1 . . ? C33 C32 C31 88.8(16) . . ? C33 C32 H32A 113.9 . . ? C33 C32 H32B 113.9 . . ? O2 C33 C32 107.6(11) . . ? O2 C33 H33A 110.2 . . ? O2 C33 H33B 110.2 . . ? C32 C33 H33A 110.2 . . ? C32 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? C30 C34 H34A 109.5 . . ? C30 C34 H34B 109.5 . . ? C30 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O3 C35 H35A 109.0 . . ? O3 C35 H35B 109.0 . . ? O3 C35 C36 113.0(12) . . ? H35A C35 H35B 107.8 . . ? C36 C35 H35A 109.0 . . ? C36 C35 H35B 109.0 . . ? C35 C36 H36A 113.6 . . ? C35 C36 H36B 113.6 . . ? C35 C36 C37 90.0(11) . . ? H36A C36 H36B 110.9 . . ? C37 C36 H36A 113.6 . . ? C37 C36 H36B 113.6 . . ? C36 C37 H37A 109.2 . . ? C36 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? C38 C37 C36 112.2(11) . . ? C38 C37 H37A 109.2 . . ? C38 C37 H37B 109.2 . . ? O3 C38 C37 105.4(9) . . ? O3 C38 H38 113.1 . . ? O3 C38 C39 101.0(12) . . ? C37 C38 H38 113.1 . . ? C39 C38 C37 110.4(15) . . ? C39 C38 H38 113.1 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C43 O4 C40 103.3(11) . . ? O4 C40 H40A 111.0 . . ? O4 C40 H40B 111.0 . . ? O4 C40 C41 103.8(12) . . ? H40A C40 H40B 109.0 . . ? C41 C40 H40A 111.0 . . ? C41 C40 H40B 111.0 . . ? C40 C41 H41A 110.1 . . ? C40 C41 H41B 110.1 . . ? C40 C41 C42 107.9(13) . . ? H41A C41 H41B 108.4 . . ? C42 C41 H41A 110.1 . . ? C42 C41 H41B 110.1 . . ? C41 C42 H42A 112.2 . . ? C41 C42 H42B 112.2 . . ? H42A C42 H42B 109.8 . . ? C43 C42 C41 97.9(13) . . ? C43 C42 H42A 112.2 . . ? C43 C42 H42B 112.2 . . ? O4 C43 C42 107.5(12) . . ? O4 C43 H43 112.0 . . ? O4 C43 C44 111.6(16) . . ? C42 C43 H43 112.0 . . ? C42 C43 C44 101.2(19) . . ? C44 C43 H43 112.0 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O2 C30A H30A 107.9 . . ? O2 C30A C31A 105.1(10) . . ? O2 C30A C34A 100.0(12) . . ? C31A C30A H30A 107.9 . . ? C34A C30A H30A 107.9 . . ? C34A C30A C31A 126.6(17) . . ? C30A C31A H31C 111.1 . . ? C30A C31A H31D 111.1 . . ? C30A C31A C32A 103.3(12) . . ? H31C C31A H31D 109.1 . . ? C32A C31A H31C 111.1 . . ? C32A C31A H31D 111.1 . . ? C31A C32A H32C 111.9 . . ? C31A C32A H32D 111.9 . . ? H32C C32A H32D 109.6 . . ? C33A C32A C31A 99.5(10) . . ? C33A C32A H32C 111.9 . . ? C33A C32A H32D 111.9 . . ? O2 C33A C32A 107.9(9) . . ? O2 C33A H33C 110.1 . . ? O2 C33A H33D 110.1 . . ? C32A C33A H33C 110.1 . . ? C32A C33A H33D 110.1 . . ? H33C C33A H33D 108.4 . . ? C30A C34A H34D 109.5 . . ? C30A C34A H34E 109.5 . . ? C30A C34A H34F 109.5 . . ? H34D C34A H34E 109.5 . . ? H34D C34A H34F 109.5 . . ? H34E C34A H34F 109.5 . . ? O1 C28A H28C 111.6 . . ? O1 C28A H28D 111.6 . . ? O1 C28A C27A 101.1(19) . . ? H28C C28A H28D 109.4 . . ? C27A C28A H28C 111.6 . . ? C27A C28A H28D 111.6 . . ? H29D C29A H29E 109.5 . . ? H29D C29A H29F 109.5 . . ? H29E C29A H29F 109.5 . . ? C25A C29A H29D 109.5 . . ? C25A C29A H29E 109.5 . . ? C25A C29A H29F 109.5 . . ? H26C C26A H26D 110.4 . . ? C25A C26A H26C 113.0 . . ? C25A C26A H26D 113.0 . . ? C25A C26A C27A 93.8(14) . . ? C27A C26A H26C 113.0 . . ? C27A C26A H26D 113.0 . . ? O1 C25A C29A 106.4(19) . . ? O1 C25A C26A 106.3(16) . . ? O1 C25A H25A 108.6 . . ? C29A C25A C26A 118(2) . . ? C29A C25A H25A 108.6 . . ? C26A C25A H25A 108.6 . . ? C28A C27A C26A 95.4(16) . . ? C28A C27A H27C 112.7 . . ? C28A C27A H27D 112.7 . . ? C26A C27A H27C 112.7 . . ? C26A C27A H27D 112.7 . . ? H27C C27A H27D 110.2 . . ? O3 C35A H35C 112.3 . . ? O3 C35A H35D 112.3 . . ? O3 C35A C36A 97.5(19) . . ? H35C C35A H35D 109.9 . . ? C36A C35A H35C 112.3 . . ? C36A C35A H35D 112.3 . . ? C35A C36A H36C 112.3 . . ? C35A C36A H36D 112.3 . . ? C35A C36A C37A 97.5(16) . . ? H36C C36A H36D 109.9 . . ? C37A C36A H36C 112.3 . . ? C37A C36A H36D 112.3 . . ? C36A C37A H37C 112.5 . . ? C36A C37A H37D 112.5 . . ? H37C C37A H37D 110.0 . . ? C38A C37A C36A 96(2) . . ? C38A C37A H37C 112.5 . . ? C38A C37A H37D 112.5 . . ? O3 C38A C37A 108.7(14) . . ? O3 C38A H38A 103.7 . . ? O3 C38A C39A 99(2) . . ? C37A C38A H38A 103.7 . . ? C39A C38A C37A 135(3) . . ? C39A C38A H38A 103.7 . . ? C38A C39A H39D 109.5 . . ? C38A C39A H39E 109.5 . . ? C38A C39A H39F 109.5 . . ? H39D C39A H39E 109.5 . . ? H39D C39A H39F 109.5 . . ? H39E C39A H39F 109.5 . . ? C40A O4A C43A 119(3) . . ? O4A C40A H40C 114.7 . . ? O4A C40A H40D 114.7 . . ? O4A C40A C41A 84(3) . . ? H40C C40A H40D 111.8 . . ? C41A C40A H40C 114.7 . . ? C41A C40A H40D 114.7 . . ? C40A C41A C43A 88(3) . . ? C42A C41A C40A 122(3) . . ? C42A C41A C43A 49.4(15) . . ? C41A C42A H42C 115.1 . . ? C41A C42A H42D 115.1 . . ? H42C C42A H42D 112.2 . . ? C43A C42A C41A 81(3) . . ? C43A C42A H42C 115.1 . . ? C43A C42A H42D 115.1 . . ? H44D C44A H44E 109.5 . . ? H44D C44A H44F 109.5 . . ? H44E C44A H44F 109.5 . . ? C43A C44A H44D 109.5 . . ? C43A C44A H44E 109.5 . . ? C43A C44A H44F 109.5 . . ? O4A C43A C41A 69.1(18) . . ? O4A C43A C42A 105.8(18) . . ? O4A C43A C44A 120(4) . . ? C42A C43A C41A 49.9(15) . . ? C42A C43A C44A 99(4) . . ? C44A C43A C41A 147(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 Li2 2.560(12) . ? Li1 O2 1.978(9) . ? Li1 O3 1.992(8) . ? Li1 N1 2.162(8) . ? Li1 N2 2.153(9) . ? Li2 O1 1.867(10) . ? Li2 N1 2.031(10) . ? Li2 N2 2.007(9) . ? Li2 C7 2.620(10) . ? Li2 C13 2.617(10) . ? O1 C25 1.440(9) . ? O1 C28 1.459(10) . ? O1 C28A 1.446(14) . ? O1 C25A 1.443(13) . ? O2 C30 1.423(12) . ? O2 C33 1.389(12) . ? O2 C30A 1.428(10) . ? O2 C33A 1.468(10) . ? O3 C35 1.490(10) . ? O3 C38 1.428(9) . ? O3 C35A 1.451(13) . ? O3 C38A 1.419(12) . ? N1 C1 1.395(6) . ? N1 C7 1.388(6) . ? N2 C13 1.371(6) . ? N2 C19 1.395(6) . ? C1 C2 1.410(7) . ? C1 C6 1.391(7) . ? C2 H2 0.9500 . ? C2 C3 1.384(7) . ? C3 H3 0.9500 . ? C3 C4 1.393(9) . ? C4 H4 0.9500 . ? C4 C5 1.369(10) . ? C5 H5 0.9500 . ? C5 C6 1.397(7) . ? C6 H6 0.9500 . ? C7 C8 1.410(7) . ? C7 C12 1.421(7) . ? C8 H8 0.9500 . ? C8 C9 1.363(9) . ? C9 H9 0.9500 . ? C9 C10 1.400(11) . ? C10 H10 0.9500 . ? C10 C11 1.366(11) . ? C11 H11 0.9500 . ? C11 C12 1.376(8) . ? C12 H12 0.9500 . ? C13 C14 1.405(6) . ? C13 C18 1.417(7) . ? C14 H14 0.9500 . ? C14 C15 1.398(8) . ? C15 H15 0.9500 . ? C15 C16 1.380(12) . ? C16 H16 0.9500 . ? C16 C17 1.403(12) . ? C17 H17 0.9500 . ? C17 C18 1.365(10) . ? C18 H18 0.9500 . ? C19 C20 1.419(7) . ? C19 C24 1.396(7) . ? C20 H20 0.9500 . ? C20 C21 1.389(8) . ? C21 H21 0.9500 . ? C21 C22 1.399(11) . ? C22 H22 0.9500 . ? C22 C23 1.379(11) . ? C23 H23 0.9500 . ? C23 C24 1.386(8) . ? C24 H24 0.9500 . ? C25 H25 1.0000 . ? C25 C26 1.520(10) . ? C25 C29 1.481(11) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26 C27 1.508(12) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27 C28 1.493(12) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30 1.0000 . ? C30 C31 1.538(13) . ? C30 C34 1.514(13) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C31 C32 1.538(13) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32 C33 1.497(13) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C35 C36 1.496(12) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C36 C37 1.538(13) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C37 C38 1.514(11) . ? C38 H38 1.0000 . ? C38 C39 1.486(12) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? O4 C40 1.427(11) . ? O4 C43 1.416(12) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C40 C41 1.521(13) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C41 C42 1.531(13) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C42 C43 1.507(13) . ? C43 H43 1.0000 . ? C43 C44 1.523(13) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C30A H30A 1.0000 . ? C30A C31A 1.506(12) . ? C30A C34A 1.484(13) . ? C31A H31C 0.9900 . ? C31A H31D 0.9900 . ? C31A C32A 1.534(12) . ? C32A H32C 0.9900 . ? C32A H32D 0.9900 . ? C32A C33A 1.505(12) . ? C33A H33C 0.9900 . ? C33A H33D 0.9900 . ? C34A H34D 0.9800 . ? C34A H34E 0.9800 . ? C34A H34F 0.9800 . ? C28A H28C 0.9900 . ? C28A H28D 0.9900 . ? C28A C27A 1.527(14) . ? C29A H29D 0.9800 . ? C29A H29E 0.9800 . ? C29A H29F 0.9800 . ? C29A C25A 1.516(14) . ? C26A H26C 0.9900 . ? C26A H26D 0.9900 . ? C26A C25A 1.526(13) . ? C26A C27A 1.535(14) . ? C25A H25A 1.0000 . ? C27A H27C 0.9900 . ? C27A H27D 0.9900 . ? C35A H35C 0.9900 . ? C35A H35D 0.9900 . ? C35A C36A 1.514(14) . ? C36A H36C 0.9900 . ? C36A H36D 0.9900 . ? C36A C37A 1.541(14) . ? C37A H37C 0.9900 . ? C37A H37D 0.9900 . ? C37A C38A 1.499(13) . ? C38A H38A 1.0000 . ? C38A C39A 1.498(14) . ? C39A H39D 0.9800 . ? C39A H39E 0.9800 . ? C39A H39F 0.9800 . ? O4A C40A 1.424(14) . ? O4A C43A 1.427(14) . ? C40A H40C 0.9900 . ? C40A H40D 0.9900 . ? C40A C41A 1.543(14) . ? C41A C42A 1.533(14) . ? C41A C43A 1.98(6) . ? C42A H42C 0.9900 . ? C42A H42D 0.9900 . ? C42A C43A 1.523(14) . ? C44A H44D 0.9800 . ? C44A H44E 0.9800 . ? C44A H44F 0.9800 . ? C44A C43A 1.534(14) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Li1 O2 C30 C31 -150.5(12) . . . . ? Li1 O2 C30 C34 115.8(19) . . . . ? Li1 O2 C33 C32 124.3(15) . . . . ? Li1 O2 C30A C31A 149.3(10) . . . . ? Li1 O2 C30A C34A -78.3(16) . . . . ? Li1 O2 C33A C32A -174.3(9) . . . . ? Li1 O3 C35 C36 -170.9(12) . . . . ? Li1 O3 C38 C37 -166.9(11) . . . . ? Li1 O3 C38 C39 78.2(13) . . . . ? Li1 O3 C35A C36A 171.2(16) . . . . ? Li1 O3 C38A C37A 154.1(18) . . . . ? Li1 O3 C38A C39A -62(3) . . . . ? Li1 N1 C1 C2 88.0(5) . . . . ? Li1 N1 C1 C6 -89.2(5) . . . . ? Li1 N1 C7 Li2 77.5(4) . . . . ? Li1 N1 C7 C8 -152.9(5) . . . . ? Li1 N1 C7 C12 30.0(6) . . . . ? Li1 N2 C13 Li2 79.1(4) . . . . ? Li1 N2 C13 C14 31.8(6) . . . . ? Li1 N2 C13 C18 -153.2(4) . . . . ? Li1 N2 C19 C20 83.1(6) . . . . ? Li1 N2 C19 C24 -94.6(6) . . . . ? Li2 O1 C25 C26 161.6(9) . . . . ? Li2 O1 C25 C29 -72.4(10) . . . . ? Li2 O1 C28 C27 -171.1(12) . . . . ? Li2 O1 C28A C27A 148(2) . . . . ? Li2 O1 C25A C29A 49(3) . . . . ? Li2 O1 C25A C26A 175.4(19) . . . . ? Li2 N1 C1 C2 177.1(5) . . . . ? Li2 N1 C1 C6 -0.1(7) . . . . ? Li2 N1 C7 C8 129.6(5) . . . . ? Li2 N1 C7 C12 -47.5(5) . . . . ? Li2 N2 C13 C14 -47.3(5) . . . . ? Li2 N2 C13 C18 127.7(5) . . . . ? Li2 N2 C19 C20 171.8(6) . . . . ? Li2 N2 C19 C24 -5.9(8) . . . . ? Li2 C7 C8 C9 -107.6(8) . . . . ? Li2 C7 C12 C11 140.3(6) . . . . ? Li2 C13 C14 C15 140.1(6) . . . . ? Li2 C13 C18 C17 -108.0(7) . . . . ? O1 C25 C26 C27 6.5(16) . . . . ? O1 C28A C27A C26A 55(3) . . . . ? O2 C30 C31 C32 2(2) . . . . ? O2 C30A C31A C32A 36.2(16) . . . . ? O3 C35 C36 C37 -43.1(18) . . . . ? O3 C35A C36A C37A 57(3) . . . . ? N1 Li2 O1 C25 -148.0(7) . . . . ? N1 Li2 O1 C28 7.3(14) . . . . ? N1 Li2 O1 C28A -10(3) . . . . ? N1 Li2 O1 C25A 164.7(16) . . . . ? N1 C1 C2 C3 -175.9(5) . . . . ? N1 C1 C6 C5 174.5(5) . . . . ? N1 C7 C8 C9 -175.9(6) . . . . ? N1 C7 C12 C11 175.2(5) . . . . ? N2 Li2 O1 C25 24.9(11) . . . . ? N2 Li2 O1 C28 -179.8(12) . . . . ? N2 Li2 O1 C28A 163(3) . . . . ? N2 Li2 O1 C25A -22.4(19) . . . . ? N2 C13 C14 C15 174.1(5) . . . . ? N2 C13 C18 C17 -173.9(5) . . . . ? N2 C19 C20 C21 -176.4(6) . . . . ? N2 C19 C24 C23 173.7(6) . . . . ? C1 N1 C7 Li2 -141.9(5) . . . . ? C1 N1 C7 C8 -12.3(7) . . . . ? C1 N1 C7 C12 170.6(4) . . . . ? C1 C2 C3 C4 0.8(9) . . . . ? C2 C1 C6 C5 -2.9(8) . . . . ? C2 C3 C4 C5 -1.7(10) . . . . ? C3 C4 C5 C6 0.2(11) . . . . ? C4 C5 C6 C1 2.1(10) . . . . ? C6 C1 C2 C3 1.4(8) . . . . ? C7 Li2 O1 C25 -179.2(6) . . . . ? C7 Li2 O1 C28 -23.9(13) . . . . ? C7 Li2 O1 C28A -41(3) . . . . ? C7 Li2 O1 C25A 133.5(16) . . . . ? C7 N1 C1 C2 -53.9(6) . . . . ? C7 N1 C1 C6 128.9(5) . . . . ? C7 C8 C9 C10 -0.4(11) . . . . ? C8 C7 C12 C11 -2.1(8) . . . . ? C8 C9 C10 C11 0.4(11) . . . . ? C9 C10 C11 C12 -1.2(10) . . . . ? C10 C11 C12 C7 2.2(9) . . . . ? C12 C7 C8 C9 1.2(8) . . . . ? C13 Li2 O1 C25 -2.5(8) . . . . ? C13 Li2 O1 C28 152.9(11) . . . . ? C13 Li2 O1 C28A 136(3) . . . . ? C13 Li2 O1 C25A -49.8(17) . . . . ? C13 N2 C19 C20 -57.1(7) . . . . ? C13 N2 C19 C24 125.2(5) . . . . ? C13 C14 C15 C16 1.4(9) . . . . ? C14 C13 C18 C17 1.3(8) . . . . ? C14 C15 C16 C17 -1.2(10) . . . . ? C15 C16 C17 C18 1.2(11) . . . . ? C16 C17 C18 C13 -1.3(10) . . . . ? C18 C13 C14 C15 -1.4(7) . . . . ? C19 N2 C13 Li2 -142.7(5) . . . . ? C19 N2 C13 C14 170.0(4) . . . . ? C19 N2 C13 C18 -15.0(7) . . . . ? C19 C20 C21 C22 2.1(12) . . . . ? C20 C19 C24 C23 -4.1(9) . . . . ? C20 C21 C22 C23 -2.8(13) . . . . ? C21 C22 C23 C24 0.1(13) . . . . ? C22 C23 C24 C19 3.5(11) . . . . ? C24 C19 C20 C21 1.4(9) . . . . ? C25 O1 C28 C27 -14(2) . . . . ? C25 C26 C27 C28 -15(2) . . . . ? C26 C27 C28 O1 17(2) . . . . ? C28 O1 C25 C26 4.8(16) . . . . ? C28 O1 C25 C29 130.8(13) . . . . ? C29 C25 C26 C27 -111.0(15) . . . . ? C30 O2 C33 C32 -56.3(19) . . . . ? C30 C31 C32 C33 -29(2) . . . . ? C31 C32 C33 O2 49.8(19) . . . . ? C33 O2 C30 C31 29.9(16) . . . . ? C33 O2 C30 C34 -64(2) . . . . ? C34 C30 C31 C32 113(2) . . . . ? C35 O3 C38 C37 -15.2(15) . . . . ? C35 O3 C38 C39 -130.1(13) . . . . ? C35 C36 C37 C38 31(2) . . . . ? C36 C37 C38 O3 -11(2) . . . . ? C36 C37 C38 C39 97(2) . . . . ? C38 O3 C35 C36 40.6(16) . . . . ? O4 C40 C41 C42 13.6(17) . . . . ? C40 O4 C43 C42 46.8(17) . . . . ? C40 O4 C43 C44 157.0(19) . . . . ? C40 C41 C42 C43 12.4(18) . . . . ? C41 C42 C43 O4 -35.6(17) . . . . ? C41 C42 C43 C44 -152.8(15) . . . . ? C43 O4 C40 C41 -35.7(15) . . . . ? C30A O2 C33A C32A -7.9(14) . . . . ? C30A C31A C32A C33A -39.0(16) . . . . ? C31A C32A C33A O2 29.1(16) . . . . ? C33A O2 C30A C31A -17.8(14) . . . . ? C33A O2 C30A C34A 114.6(15) . . . . ? C34A C30A C31A C32A -78.8(19) . . . . ? C28A O1 C25A C29A -136(3) . . . . ? C28A O1 C25A C26A -10(4) . . . . ? C25A O1 C28A C27A -28(4) . . . . ? C25A C26A C27A C28A -57(2) . . . . ? C27A C26A C25A O1 43(3) . . . . ? C27A C26A C25A C29A 162(3) . . . . ? C35A O3 C38A C37A 9(3) . . . . ? C35A O3 C38A C39A 152(2) . . . . ? C35A C36A C37A C38A -50(3) . . . . ? C36A C37A C38A O3 26(3) . . . . ? C36A C37A C38A C39A -98(4) . . . . ? C38A O3 C35A C36A -41(2) . . . . ? O4A C40A C41A C42A 36(4) . . . . ? O4A C40A C41A C43A -2(3) . . . . ? C40A O4A C43A C41A -2(3) . . . . ? C40A O4A C43A C42A -37(5) . . . . ? C40A O4A C43A C44A -147(5) . . . . ? C40A C41A C42A C43A -54(4) . . . . ? C41A C42A C43A O4A 44(3) . . . . ? C41A C42A C43A C44A 168(4) . . . . ? C43A O4A C40A C41A 3(4) . . . . ?