#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:05:06 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242465 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/24/4132492.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_4132492 loop_ _publ_author_name 'Zhang, Xin' 'Frey, Brandon L.' 'Chen, Yu-Sheng' 'Zhang, Jian' _publ_section_title ; Topology-Guided Stepwise Insertion of Three Secondary Linkers in Zirconium Metal-Organic Frameworks. ; _journal_issue 24 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 7710 _journal_page_last 7715 _journal_paper_doi 10.1021/jacs.8b04277 _journal_volume 140 _journal_year 2018 _chemical_formula_moiety 'C60 H30 O24 Zr3' _chemical_formula_sum 'C60 H30 O24 Zr3' _chemical_formula_weight 1280.50 _space_group_crystal_system orthorhombic _space_group_IT_number 65 _space_group_name_Hall '-C 2 2' _space_group_name_H-M_alt 'C m m m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2017-07-27 _audit_creation_method ; Olex2 1.2 (compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370) ; _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 21.1374(11) _cell_length_b 33.1766(18) _cell_length_c 21.4671(10) _cell_measurement_reflns_used 9683 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 12.809 _cell_measurement_theta_min 2.212 _cell_volume 15054.2(13) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 273.15 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.41328 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_unetI/netI 0.0254 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 9978 _diffrn_reflns_theta_full 12.86 _diffrn_reflns_theta_max 12.86 _diffrn_reflns_theta_min 0.86 _diffrn_source synchrotron _exptl_absorpt_coefficient_mu 0.313 _exptl_absorpt_correction_T_max 0.7437 _exptl_absorpt_correction_T_min 0.7064 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0961 before and 0.0537 after correction. The Ratio of minimum to maximum transmission is 0.9498. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'light yellow' _exptl_crystal_density_diffrn 0.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 12540 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _refine_diff_density_max 2.278 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.182 _refine_ls_extinction_coef 0.020(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.483 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 211 _refine_ls_number_reflns 5324 _refine_ls_number_restraints 245 _refine_ls_restrained_S_all 1.493 _refine_ls_R_factor_all 0.1176 _refine_ls_R_factor_gt 0.1027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3260 _refine_ls_wR_factor_ref 0.3457 _reflns_number_gt 4175 _reflns_number_total 5324 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ja8b04277_si_009.cif _cod_data_source_block NPF-300-5 _cod_database_code 4132492 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Restrained distances C15-C16 = C17-C18 1.38 with sigma of 0.02 C16-C17 1.38 with sigma of 0.02 3. Rigid bond restraints C19, C18, C17, C16, C15, C14, O3 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C13, C12, C10, C9, C11, C8, C5, C4, C3, C2, C7, C6, C1, O4, O006 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C25, C24, C23, C22, C21, C20, O5 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 4. Uiso/Uaniso restraints and constraints C19 \\sim C18 \\sim C17 \\sim C16 \\sim C15 \\sim C14 \\sim O3: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 C13 \\sim C12 \\sim C10 \\sim C9 \\sim C8 \\sim C11 \\sim C5 \\sim C4 \\sim C3 \\sim C2 \\sim C7 \\sim C6 \\sim C1 \\sim O4 \\sim O006: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 C25 \\sim C24 \\sim C23 \\sim C22 \\sim C21 \\sim C20 \\sim O5: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 5.a Aromatic/amide H refined with riding coordinates: C22(H22), C23(H23), C7(H7), C3(H3), C6(H6), C4(H4), C16(H16), C11(H11), C9(H9), C17(H17) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, z' 3 '-x, y, -z' 4 'x, -y, -z' 5 'x+1/2, y+1/2, z' 6 '-x+1/2, -y+1/2, z' 7 '-x+1/2, y+1/2, -z' 8 'x+1/2, -y+1/2, -z' 9 '-x, -y, -z' 10 'x, y, -z' 11 'x, -y, z' 12 '-x, y, z' 13 '-x+1/2, -y+1/2, -z' 14 'x+1/2, y+1/2, -z' 15 'x+1/2, -y+1/2, z' 16 '-x+1/2, 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_calc_flag _atom_site_site_symmetry_order _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Zr1 Zr 0.58186(4) 0.5000 0.41823(3) 0.0728(5) Uani 1 d 2 S T P Zr2 Zr 0.5000 0.57391(3) 0.5000 0.0828(6) Uani 1 d 4 S T P O5 O 0.5551(4) 0.5000 0.3192(3) 0.0839(19) Uani 1 d 2 S TU P O2 O 0.5000 0.4636(2) 0.4201(4) 0.099(2) Uani 1 d 2 S T P O4 O 0.6166(4) 0.4416(2) 0.3814(3) 0.122(2) Uani 1 d 1 . U . O006 O 0.5623(4) 0.39271(18) 0.4372(3) 0.134(2) Uani 1 d 1 . U . O1 O 0.5811(5) 0.5363(4) 0.5000 0.138(4) Uani 1 d 2 S T P C20 C 0.5000 0.5000 0.2919(7) 0.086(4) Uani 1 d 4 S TU P O3 O 0.6838(5) 0.5000 0.4435(6) 0.175(5) Uani 1 d 2 S TU P C21 C 0.5000 0.5000 0.2232(7) 0.101(4) Uani 1 d 4 S TU P C1 C 0.6017(7) 0.4052(4) 0.3942(5) 0.139(4) Uani 1 d 1 . U . C22 C 0.4442(8) 0.5000 0.1898(6) 0.143(5) Uani 1 d 2 S TU P H22 H 0.4062 0.5000 0.2116 0.172 Uiso 1 calc 2 RS T P C2 C 0.6343(8) 0.3740(4) 0.3564(4) 0.182(5) Uani 1 d 1 . U . C23 C 0.4423(10) 0.5000 0.1285(7) 0.178(7) Uani 1 d 2 S TU P H23 H 0.4035 0.5000 0.1081 0.214 Uiso 1 calc 2 RS T P C7 C 0.6306(10) 0.3337(4) 0.3741(5) 0.231(7) Uani 1 d 1 . U . H7 H 0.6094 0.3269 0.4105 0.278 Uiso 1 calc 1 R . . C3 C 0.6618(9) 0.3824(5) 0.3027(5) 0.239(7) Uani 1 d 1 . U . H3 H 0.6627 0.4089 0.2886 0.286 Uiso 1 calc 1 R . . C14 C 0.7090(12) 0.5000 0.5000 0.186(9) Uani 1 d 4 S TU P C24 C 0.5000 0.5000 0.0926(9) 0.179(9) Uani 1 d 4 S TU P C6 C 0.6567(11) 0.3050(4) 0.3402(6) 0.275(8) Uani 1 d 1 . U . H6 H 0.6530 0.2784 0.3531 0.330 Uiso 1 calc 1 R . . C5 C 0.6894(12) 0.3134(5) 0.2859(5) 0.302(8) Uani 1 d 1 . U . C4 C 0.6895(11) 0.3522(5) 0.2670(6) 0.284(8) Uani 1 d 1 . U . H4 H 0.7084 0.3589 0.2293 0.341 Uiso 1 calc 1 R . . C25 C 0.5000 0.5000 0.0259(8) 0.176(10) Uani 1 d 4 S TU P C15 C 0.7735(13) 0.5000 0.5000 0.225(10) Uani 1 d 4 DS TU P C16 C 0.8070(9) 0.5000 0.5552(11) 0.286(11) Uani 1 d 2 DS TU P H16 H 0.7863 0.5000 0.5934 0.343 Uiso 1 calc 2 RS T P C8 C 0.7178(14) 0.2810(6) 0.2494(6) 0.357(10) Uani 1 d 1 . U . C11 C 0.7500 0.2500 0.2804(8) 0.368(15) Uani 1 d 2 S TU P H11 H 0.7500 0.2500 0.3237 0.442 Uiso 1 calc 2 RS T P C12 C 0.7500 0.2500 0.0835(8) 0.387(15) Uani 1 d 2 S TU P C9 C 0.7246(14) 0.2823(6) 0.1832(6) 0.378(12) Uani 1 d 1 . U . H9 H 0.7119 0.3048 0.1605 0.453 Uiso 1 calc 1 R . . C13 C 0.7500 0.2500 0.0313(8) 0.383(17) Uani 1 d 2 S TU P C10 C 0.7500 0.2500 0.1551(8) 0.381(13) Uani 1 d 2 S TU P C17 C 0.8709(10) 0.5000 0.5522(16) 0.332(13) Uani 1 d 2 DS TU P H17 H 0.8922 0.5000 0.5901 0.399 Uiso 1 calc 2 RS T P C18 C 0.908(2) 0.5000 0.5000 0.368(17) Uani 1 d 4 DS TU P C19 C 0.9699(18) 0.5000 0.5000 0.39(2) Uani 1 d 4 S TU P 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 Zr1 0.0986(8) 0.0864(8) 0.0333(7) 0.000 0.0043(3) 0.000 Zr2 0.1627(14) 0.0558(8) 0.0300(7) 0.000 0.000 0.000 O5 0.135(6) 0.081(4) 0.036(3) 0.000 0.004(3) 0.000 O2 0.120(6) 0.065(4) 0.114(7) 0.024(4) 0.000 0.000 O4 0.178(6) 0.131(4) 0.056(3) -0.003(3) 0.014(3) 0.069(4) O006 0.264(8) 0.091(4) 0.048(4) -0.011(3) 0.000(4) 0.063(4) O1 0.201(11) 0.166(9) 0.046(5) 0.000 0.000 0.062(7) C20 0.149(10) 0.066(7) 0.043(6) 0.000 0.000 0.000 O3 0.110(7) 0.275(15) 0.142(10) 0.000 -0.024(6) 0.000 C21 0.153(11) 0.114(11) 0.038(6) 0.000 0.000 0.000 C1 0.245(11) 0.116(6) 0.056(6) -0.001(5) 0.003(6) 0.089(7) C22 0.166(10) 0.224(15) 0.040(5) 0.000 0.000(5) 0.000 C2 0.334(14) 0.160(6) 0.054(5) 0.009(5) 0.017(6) 0.150(9) C23 0.177(12) 0.31(2) 0.046(6) 0.000 -0.019(6) 0.000 C7 0.46(2) 0.161(7) 0.074(7) 0.009(6) 0.020(9) 0.196(11) C3 0.428(18) 0.225(9) 0.063(6) 0.028(6) 0.053(8) 0.231(12) C14 0.108(10) 0.32(3) 0.127(12) 0.000 0.000 0.000 C24 0.209(16) 0.29(2) 0.037(7) 0.000 0.000 0.000 C6 0.57(2) 0.182(9) 0.073(7) 0.003(6) 0.010(9) 0.240(12) C5 0.59(2) 0.256(10) 0.059(6) 0.024(6) 0.027(9) 0.316(13) C4 0.53(2) 0.250(10) 0.077(7) 0.029(7) 0.058(10) 0.280(13) C25 0.20(2) 0.29(3) 0.042(7) 0.000 0.000 0.000 C15 0.107(10) 0.42(3) 0.150(16) 0.000 0.000 0.000 C16 0.123(10) 0.53(3) 0.200(17) 0.000 -0.040(9) 0.000 C8 0.72(2) 0.294(12) 0.058(5) -0.008(7) -0.012(10) 0.384(16) C11 0.78(4) 0.259(19) 0.061(8) 0.000 0.000 0.38(2) C12 0.76(3) 0.34(2) 0.065(7) 0.000 0.000 0.42(2) C9 0.75(3) 0.323(15) 0.060(5) -0.004(8) -0.010(12) 0.418(18) C13 0.75(4) 0.34(2) 0.064(7) 0.000 0.000 0.43(3) C10 0.74(3) 0.338(19) 0.063(6) 0.000 0.000 0.42(2) C17 0.124(10) 0.62(4) 0.25(2) 0.000 -0.031(10) 0.000 C18 0.137(16) 0.68(5) 0.28(3) 0.000 0.000 0.000 C19 0.137(16) 0.73(6) 0.31(4) 0.000 0.000 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 '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' O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -0.5364 2.6141 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.8919 1.1868 '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 Zr1 Zr1 Zr1 90.0 2_665 10_556 Zr1 Zr1 Zr2 60.155(15) 2_665 9_666 Zr1 Zr1 Zr2 60.155(15) 2_665 . Zr2 Zr1 Zr1 59.675(13) 9_666 10_556 Zr2 Zr1 Zr1 59.675(13) . 10_556 Zr2 Zr1 Zr2 89.70(3) . 9_666 O5 Zr1 Zr1 165.1(2) . 10_556 O5 Zr1 Zr1 75.1(2) . 2_665 O5 Zr1 Zr2 111.11(14) . . O5 Zr1 Zr2 111.11(14) . 9_666 O5 Zr1 O4 74.98(18) . 11_565 O5 Zr1 O4 74.98(18) . . O5 Zr1 O3 119.0(4) . . O2 Zr1 Zr1 34.90(17) 2_665 2_665 O2 Zr1 Zr1 88.9(2) 2_665 10_556 O2 Zr1 Zr1 34.90(17) . 2_665 O2 Zr1 Zr1 88.9(2) . 10_556 O2 Zr1 Zr2 34.8(2) . 9_666 O2 Zr1 Zr2 89.2(2) 2_665 9_666 O2 Zr1 Zr2 89.2(2) . . O2 Zr1 Zr2 34.8(2) 2_665 . O2 Zr1 O5 78.9(3) 2_665 . O2 Zr1 O5 78.9(3) . . O2 Zr1 O2 69.8(3) . 2_665 O2 Zr1 O4 77.2(3) 2_665 11_565 O2 Zr1 O4 141.1(3) . 11_565 O2 Zr1 O4 77.2(3) . . O2 Zr1 O4 141.1(3) 2_665 . O2 Zr1 O1 107.5(4) 2_665 11_565 O2 Zr1 O1 107.5(4) . . O2 Zr1 O1 69.8(3) 2_665 . O2 Zr1 O1 69.8(3) . 11_565 O2 Zr1 O3 142.2(2) . . O2 Zr1 O3 142.2(2) 2_665 . O4 Zr1 Zr1 110.87(15) 11_565 10_556 O4 Zr1 Zr1 110.87(15) . 10_556 O4 Zr1 Zr1 109.4(2) . 2_665 O4 Zr1 Zr1 109.4(2) 11_565 2_665 O4 Zr1 Zr2 74.26(19) . 9_666 O4 Zr1 Zr2 163.9(2) . . O4 Zr1 Zr2 163.9(2) 11_565 9_666 O4 Zr1 Zr2 74.26(19) 11_565 . O4 Zr1 O4 121.8(4) . 11_565 O4 Zr1 O3 76.4(3) . . O4 Zr1 O3 76.4(3) 11_565 . O1 Zr1 Zr1 89.5(3) 11_565 2_665 O1 Zr1 Zr1 89.5(3) . 2_665 O1 Zr1 Zr1 34.5(3) 11_565 10_556 O1 Zr1 Zr1 34.5(3) . 10_556 O1 Zr1 Zr2 88.8(3) . 9_666 O1 Zr1 Zr2 35.0(2) . . O1 Zr1 Zr2 35.0(3) 11_565 9_666 O1 Zr1 Zr2 88.8(3) 11_565 . O1 Zr1 O5 142.6(3) 11_565 . O1 Zr1 O5 142.6(3) . . O1 Zr1 O4 142.3(3) . . O1 Zr1 O4 78.6(3) 11_565 . O1 Zr1 O4 142.3(3) 11_565 11_565 O1 Zr1 O4 78.6(3) . 11_565 O1 Zr1 O1 69.0(6) . 11_565 O1 Zr1 O3 78.8(4) 11_565 . O1 Zr1 O3 78.8(4) . . O3 Zr1 Zr1 75.8(4) . 10_556 O3 Zr1 Zr1 165.8(4) . 2_665 O3 Zr1 Zr2 111.0(2) . . O3 Zr1 Zr2 111.0(2) . 9_666 Zr1 Zr2 Zr1 60.65(3) 2_665 9_666 Zr1 Zr2 Zr1 59.69(3) 2_665 . Zr1 Zr2 Zr1 59.69(3) 10_556 9_666 Zr1 Zr2 Zr1 60.65(3) 10_556 . Zr1 Zr2 Zr1 90.30(3) 10_556 2_665 Zr1 Zr2 Zr1 90.30(3) . 9_666 O2 Zr2 Zr1 89.7(2) 2_665 10_556 O2 Zr2 Zr1 34.62(11) 9_666 10_556 O2 Zr2 Zr1 34.62(11) 2_665 . O2 Zr2 Zr1 34.62(11) 2_665 2_665 O2 Zr2 Zr1 89.7(2) 9_666 . O2 Zr2 Zr1 34.62(11) 9_666 9_666 O2 Zr2 Zr1 89.7(2) 2_665 9_666 O2 Zr2 Zr1 89.7(2) 9_666 2_665 O2 Zr2 O2 108.0(5) 9_666 2_665 O2 Zr2 O006 142.8(2) 9_666 11_565 O2 Zr2 O006 78.4(2) 9_666 9_666 O2 Zr2 O006 142.8(2) 2_665 9_666 O2 Zr2 O006 78.4(2) 9_666 4_566 O2 Zr2 O006 78.4(2) 2_665 11_565 O2 Zr2 O006 142.8(2) 9_666 2_665 O2 Zr2 O006 78.4(2) 2_665 2_665 O2 Zr2 O006 142.8(2) 2_665 4_566 O006 Zr2 Zr1 111.7(2) 11_565 10_556 O006 Zr2 Zr1 110.21(16) 2_665 . O006 Zr2 Zr1 75.3(2) 11_565 . O006 Zr2 Zr1 110.21(16) 4_566 9_666 O006 Zr2 Zr1 111.7(2) 4_566 . O006 Zr2 Zr1 75.3(2) 9_666 9_666 O006 Zr2 Zr1 165.6(2) 9_666 . O006 Zr2 Zr1 110.21(16) 9_666 10_556 O006 Zr2 Zr1 75.3(2) 4_566 10_556 O006 Zr2 Zr1 165.6(2) 2_665 10_556 O006 Zr2 Zr1 110.20(16) 11_565 2_665 O006 Zr2 Zr1 165.6(2) 11_565 9_666 O006 Zr2 Zr1 111.7(2) 9_666 2_665 O006 Zr2 Zr1 111.7(2) 2_665 9_666 O006 Zr2 Zr1 75.3(2) 2_665 2_665 O006 Zr2 Zr1 165.6(2) 4_566 2_665 O006 Zr2 O006 74.0(5) 4_566 9_666 O006 Zr2 O006 119.1(4) 11_565 9_666 O006 Zr2 O006 76.2(3) 9_666 2_665 O006 Zr2 O006 119.1(4) 4_566 2_665 O006 Zr2 O006 76.2(3) 4_566 11_565 O006 Zr2 O006 74.0(5) 11_565 2_665 O1 Zr2 Zr1 89.3(3) . 2_665 O1 Zr2 Zr1 35.18(18) . . O1 Zr2 Zr1 35.18(18) 3_656 9_666 O1 Zr2 Zr1 35.18(18) 3_656 2_665 O1 Zr2 Zr1 89.3(3) . 9_666 O1 Zr2 Zr1 35.18(18) . 10_556 O1 Zr2 Zr1 89.3(3) 3_656 10_556 O1 Zr2 Zr1 89.3(3) 3_656 . O1 Zr2 O2 69.8(2) . 2_665 O1 Zr2 O2 69.8(2) 3_656 2_665 O1 Zr2 O2 69.8(2) . 9_666 O1 Zr2 O2 69.8(2) 3_656 9_666 O1 Zr2 O006 141.72(18) 3_656 11_565 O1 Zr2 O006 79.1(4) . 11_565 O1 Zr2 O006 79.1(4) 3_656 9_666 O1 Zr2 O006 141.72(18) . 2_665 O1 Zr2 O006 141.72(18) 3_656 4_566 O1 Zr2 O006 141.72(18) . 9_666 O1 Zr2 O006 79.1(4) . 4_566 O1 Zr2 O006 79.1(4) 3_656 2_665 O1 Zr2 O1 107.9(7) . 3_656 C20 O5 Zr1 131.6(8) . . Zr1 O2 Zr1 110.2(3) . 2_665 Zr1 O2 Zr2 110.6(3) . 9_666 Zr1 O2 Zr2 110.6(3) 2_665 9_666 C1 O4 Zr1 131.9(7) . . C1 O006 Zr2 131.1(6) . 9_666 Zr1 O1 Zr1 111.0(6) . 10_556 Zr2 O1 Zr1 109.8(3) . . Zr2 O1 Zr1 109.8(3) . 10_556 O5 C20 O5 126.6(13) . 2_665 O5 C20 C21 116.7(7) . . O5 C20 C21 116.7(7) 2_665 . C14 O3 Zr1 127.9(14) . . C22 C21 C20 121.3(8) . . C22 C21 C20 121.3(8) 2_665 . C22 C21 C22 117.5(16) 2_665 . O4 C1 O006 127.3(8) . . O4 C1 C2 115.3(12) . . O006 C1 C2 117.4(11) . . C21 C22 H22 118.5 . . C23 C22 C21 123.0(17) . . C23 C22 H22 118.5 . . C7 C2 C1 119.6(12) . . C3 C2 C1 122.3(11) . . C3 C2 C7 117.7(11) . . C22 C23 H23 119.7 . . C22 C23 C24 120.6(18) . . C24 C23 H23 119.7 . . C2 C7 H7 119.3 . . C6 C7 C2 121.3(15) . . C6 C7 H7 119.3 . . C2 C3 H3 119.6 . . C2 C3 C4 120.9(14) . . C4 C3 H3 119.6 . . O3 C14 O3 132(2) 10_556 . O3 C14 C15 113.8(12) . . O3 C14 C15 113.8(12) 10_556 . C23 C24 C23 115.4(18) 2_665 . C25 C24 C23 122.3(9) . . C25 C24 C23 122.3(9) . 2_665 C7 C6 H6 119.0 . . C7 C6 C5 121.9(15) . . C5 C6 H6 119.0 . . C6 C5 C8 120.7(16) . . C4 C5 C6 116.4(11) . . C4 C5 C8 122.7(15) . . C3 C4 H4 119.3 . . C5 C4 C3 121.4(14) . . C5 C4 H4 119.3 . . C25 C25 C24 180.000(4) 9_665 . C14 C15 C16 120.9(15) . . C14 C15 C16 120.9(15) . 10_556 C16 C15 C16 118(3) . 10_556 C15 C16 H16 120.9 . . C17 C16 C15 118(3) . . C17 C16 H16 120.9 . . C11 C8 C5 119.1(11) . . C11 C8 C9 116.4(12) . . C9 C8 C5 123.5(11) . . C8 C11 C8 123.4(16) 6_655 . C8 C11 H11 118.3 6_655 . C8 C11 H11 118.3 . . C13 C12 C10 180.000(2) . . C8 C9 H9 121.2 . . C10 C9 C8 117.6(13) . . C10 C9 H9 121.2 . . C12 C13 C13 180.000(2) . 13_655 C9 C10 C12 116.7(8) 6_655 . C9 C10 C12 116.7(8) . . C9 C10 C9 126.5(17) 6_655 . C16 C17 H17 116.2 . . C16 C17 C18 128(4) . . C18 C17 H17 116.2 . . C17 C18 C17 110(5) . 10_556 C19 C18 C17 125(2) . . C19 C18 C17 125(2) . 10_556 C19 C19 C18 180.000(7) 9_766 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Zr1 Zr1 3.4605(18) 2_665 Zr1 Zr1 3.5109(14) 10_556 Zr1 Zr2 3.4769(9) 9_666 Zr1 Zr2 3.4769(9) . Zr1 O5 2.200(6) . Zr1 O2 2.110(4) . Zr1 O2 2.110(4) 2_665 Zr1 O4 2.217(6) . Zr1 O4 2.217(6) 11_565 Zr1 O1 2.130(7) 11_565 Zr1 O1 2.130(7) . Zr1 O3 2.221(11) . Zr2 Zr1 3.4769(9) 10_556 Zr2 Zr1 3.4769(9) 2_665 Zr2 Zr1 3.4769(9) 9_666 Zr2 O2 2.120(7) 2_665 Zr2 O2 2.120(7) 9_666 Zr2 O006 2.186(6) 2_665 Zr2 O006 2.186(7) 4_566 Zr2 O006 2.186(6) 9_666 Zr2 O006 2.186(7) 11_565 Zr2 O1 2.119(10) 3_656 Zr2 O1 2.119(10) . O5 C20 1.304(9) . O2 Zr1 2.110(4) 2_665 O2 Zr2 2.120(7) 9_666 O4 C1 1.279(14) . O006 Zr2 2.186(6) 9_666 O006 C1 1.310(15) . O1 Zr1 2.130(7) 10_556 C20 O5 1.304(9) 2_665 C20 C21 1.47(2) . O3 C14 1.325(15) . C21 C22 1.380(17) . C21 C22 1.380(17) 2_665 C1 C2 1.484(13) . C22 H22 0.9300 . C22 C23 1.318(19) . C2 C7 1.392(19) . C2 C3 1.320(17) . C23 H23 0.9300 . C23 C24 1.44(2) . C7 H7 0.9300 . C7 C6 1.319(15) . C3 H3 0.9300 . C3 C4 1.391(15) . C14 O3 1.325(15) 10_556 C14 C15 1.36(3) . C24 C23 1.44(2) 2_665 C24 C25 1.43(3) . C6 H6 0.9300 . C6 C5 1.38(2) . C5 C4 1.35(2) . C5 C8 1.459(16) . C4 H4 0.9300 . C25 C25 1.11(4) 9_665 C15 C16 1.380(16) . C15 C16 1.380(16) 10_556 C16 H16 0.9300 . C16 C17 1.352(17) . C8 C11 1.401(14) . C8 C9 1.430(17) . C11 C8 1.401(14) 6_655 C11 H11 0.9300 . C12 C13 1.12(2) . C12 C10 1.54(2) . C9 H9 0.9300 . C9 C10 1.344(14) . C13 C13 1.34(3) 13_655 C10 C9 1.344(14) 6_655 C17 H17 0.9300 . C17 C18 1.364(18) . C18 C17 1.364(18) 10_556 C18 C19 1.31(4) . C19 C19 1.27(8) 9_766