#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:05:32 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242466 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/24/4132493.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_4132493 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_sum 'C44 H22 O16 Zr3' _chemical_formula_weight 1080.28 _space_group_IT_number 65 _space_group_name_Hall '-C 2 2' _space_group_name_H-M_alt 'C m m m' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m m m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 20.2175(9) _cell_length_b 34.4927(15) _cell_length_c 21.0753(9) _cell_measurement_reflns_used 9919 _cell_measurement_temperature 110(2) _cell_measurement_theta_max 32.961 _cell_measurement_theta_min 4.447 _cell_volume 14697.0(11) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 110(2) _diffrn_measured_fraction_theta_full 0.932 _diffrn_measured_fraction_theta_max 0.932 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source Synchrotron _diffrn_radiation_type Synchrotron _diffrn_radiation_wavelength 0.51500 _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 57492 _diffrn_reflns_theta_full 17.01 _diffrn_reflns_theta_max 17.01 _diffrn_reflns_theta_min 0.85 _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour 'light yellow' _exptl_crystal_density_diffrn 0.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2136 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.566 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.060 _refine_ls_extinction_coef 0.00059(12) _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 1.006 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 155 _refine_ls_number_reflns 5699 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.006 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0513 _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^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1522 _refine_ls_wR_factor_ref 0.1568 _reflns_number_gt 3277 _reflns_number_total 5699 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ja8b04277_si_003.cif _cod_data_source_block NPF-300-LT _cod_original_sg_symbol_H-M cmmm _cod_database_code 4132493 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z' '-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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags Zr1 Zr 0.0000 0.429315(15) 0.5000 0.0744(3) Uani 1 4 d S Zr2 Zr 0.08716(3) 0.5000 0.41604(2) 0.0780(3) Uani 1 2 d S O1 O 0.0000 0.46452(11) 0.4156(2) 0.1126(17) Uani 1 2 d S O2 O 0.0877(3) 0.46576(13) 0.5000 0.1183(18) Uani 1 2 d S O3 O 0.12194(19) 0.44115(7) 0.38169(15) 0.1071(11) Uani 1 1 d . O4 O 0.06644(16) 0.39666(6) 0.43757(14) 0.0830(9) Uani 1 1 d . O5 O 0.1961(3) 0.5000 0.4210(2) 0.1153(16) Uani 1 2 d S O6 O 0.0784(2) 0.5000 0.31291(19) 0.1049(15) Uani 1 2 d S C1 C 0.1056(3) 0.40639(11) 0.3947(2) 0.0879(15) Uani 1 1 d . C2 C 0.1376(3) 0.37515(10) 0.3585(2) 0.0889(14) Uani 1 1 d . C3 C 0.1286(3) 0.33722(11) 0.3775(2) 0.1109(18) Uani 1 1 d . H3A H 0.1021 0.3316 0.4124 0.133 Uiso 1 1 calc R C4 C 0.1591(3) 0.30760(12) 0.3444(2) 0.125(2) Uani 1 1 d . H4A H 0.1559 0.2823 0.3594 0.150 Uiso 1 1 calc R C5 C 0.1942(3) 0.31479(11) 0.2897(2) 0.1062(17) Uani 1 1 d . C6 C 0.2034(3) 0.35262(11) 0.2716(2) 0.115(2) Uani 1 1 d . H6B H 0.2293 0.3582 0.2363 0.137 Uiso 1 1 calc R C7 C 0.1748(3) 0.38211(11) 0.3050(2) 0.1092(17) Uani 1 1 d . H7A H 0.1806 0.4075 0.2913 0.131 Uiso 1 1 calc R C8 C 0.2247(3) 0.28149(13) 0.2540(2) 0.1222(19) Uani 1 1 d . C9 C 0.2500 0.2500 0.2861(3) 0.112(3) Uani 1 2 d S H9A H 0.2500 0.2500 0.3302 0.134 Uiso 1 2 calc SR C10 C 0.2227(3) 0.28160(13) 0.1880(2) 0.138(2) Uani 1 1 d . H10A H 0.2037 0.3021 0.1660 0.165 Uiso 1 1 calc R C11 C 0.2500 0.2500 0.1558(3) 0.147(4) Uani 1 2 d S C13 C 0.2500 0.2500 0.0890(4) 0.177(6) Uani 1 2 d S C14 C 0.2500 0.2500 0.0322(4) 0.167(5) Uani 1 2 d S 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 0.1570(8) 0.0231(3) 0.0433(4) 0.000 0.000 0.000 Zr2 0.1569(6) 0.0269(2) 0.0502(3) 0.000 0.0065(3) 0.000 O1 0.138(4) 0.054(2) 0.146(5) 0.047(3) 0.000 0.000 O2 0.234(6) 0.072(3) 0.049(2) 0.000 0.000 -0.049(3) O3 0.203(3) 0.0394(15) 0.079(2) 0.0025(14) 0.035(2) 0.0129(17) O4 0.160(3) 0.0328(13) 0.0560(17) -0.0009(12) 0.0078(18) 0.0069(14) O5 0.174(5) 0.073(3) 0.099(4) 0.000 0.011(3) 0.000 O6 0.204(5) 0.052(2) 0.059(3) 0.000 0.014(3) 0.000 C1 0.170(5) 0.038(2) 0.056(3) -0.003(2) 0.011(3) 0.013(2) C2 0.163(4) 0.042(2) 0.062(3) 0.0046(19) 0.002(3) 0.016(2) C3 0.220(6) 0.040(2) 0.072(3) -0.002(2) 0.022(3) 0.014(3) C4 0.253(6) 0.045(2) 0.077(3) 0.003(2) 0.035(4) 0.032(3) C5 0.212(6) 0.052(2) 0.055(3) 0.003(2) 0.011(3) 0.039(3) C6 0.231(6) 0.052(2) 0.060(3) 0.012(2) 0.029(3) 0.042(3) C7 0.213(5) 0.045(2) 0.070(3) 0.012(2) 0.026(3) 0.024(3) C8 0.256(6) 0.064(3) 0.047(3) -0.002(2) 0.010(3) 0.051(3) C9 0.230(9) 0.047(3) 0.058(4) 0.000 0.000 0.054(4) C10 0.290(7) 0.067(3) 0.055(3) 0.005(2) 0.010(4) 0.070(4) C11 0.303(12) 0.096(5) 0.044(4) 0.000 0.000 0.090(6) C13 0.373(18) 0.101(6) 0.057(7) 0.000 0.000 0.114(8) C14 0.346(15) 0.104(5) 0.052(5) 0.000 0.000 0.092(7) 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' 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 O1 Zr1 O1 111.3(3) 10_556 . O1 Zr1 O2 70.97(9) 10_556 3_556 O1 Zr1 O2 70.97(9) . 3_556 O1 Zr1 O2 70.97(9) 10_556 . O1 Zr1 O2 70.97(9) . . O2 Zr1 O2 109.4(3) 3_556 . O1 Zr1 O4 78.11(12) 10_556 10_556 O1 Zr1 O4 141.77(8) . 10_556 O2 Zr1 O4 142.86(8) 3_556 10_556 O2 Zr1 O4 78.29(13) . 10_556 O1 Zr1 O4 141.77(8) 10_556 12 O1 Zr1 O4 78.11(12) . 12 O2 Zr1 O4 78.29(13) 3_556 12 O2 Zr1 O4 142.86(8) . 12 O4 Zr1 O4 118.16(14) 10_556 12 O1 Zr1 O4 141.77(8) 10_556 . O1 Zr1 O4 78.11(12) . . O2 Zr1 O4 142.86(8) 3_556 . O2 Zr1 O4 78.29(13) . . O4 Zr1 O4 73.78(15) 10_556 . O4 Zr1 O4 75.59(16) 12 . O1 Zr1 O4 78.11(12) 10_556 3_556 O1 Zr1 O4 141.77(8) . 3_556 O2 Zr1 O4 78.29(13) 3_556 3_556 O2 Zr1 O4 142.86(8) . 3_556 O4 Zr1 O4 75.59(16) 10_556 3_556 O4 Zr1 O4 73.78(15) 12 3_556 O4 Zr1 O4 118.16(14) . 3_556 O1 Zr1 Zr2 35.65(7) 10_556 10_556 O1 Zr1 Zr2 91.42(11) . 10_556 O2 Zr1 Zr2 90.46(12) 3_556 10_556 O2 Zr1 Zr2 35.33(7) . 10_556 O4 Zr1 Zr2 75.24(7) 10_556 10_556 O4 Zr1 Zr2 166.60(7) 12 10_556 O4 Zr1 Zr2 110.73(8) . 10_556 O4 Zr1 Zr2 111.35(7) 3_556 10_556 O1 Zr1 Zr2 35.65(7) 10_556 9_566 O1 Zr1 Zr2 91.42(11) . 9_566 O2 Zr1 Zr2 35.33(7) 3_556 9_566 O2 Zr1 Zr2 90.46(12) . 9_566 O4 Zr1 Zr2 111.35(7) 10_556 9_566 O4 Zr1 Zr2 110.73(8) 12 9_566 O4 Zr1 Zr2 166.60(7) . 9_566 O4 Zr1 Zr2 75.24(7) 3_556 9_566 Zr2 Zr1 Zr2 60.65(2) 10_556 9_566 O1 Zr1 Zr2 91.42(11) 10_556 . O1 Zr1 Zr2 35.65(6) . . O2 Zr1 Zr2 90.46(12) 3_556 . O2 Zr1 Zr2 35.33(7) . . O4 Zr1 Zr2 110.73(8) 10_556 . O4 Zr1 Zr2 111.35(7) 12 . O4 Zr1 Zr2 75.24(7) . . O4 Zr1 Zr2 166.60(7) 3_556 . Zr2 Zr1 Zr2 60.929(16) 10_556 . Zr2 Zr1 Zr2 91.375(17) 9_566 . O1 Zr1 Zr2 91.42(11) 10_556 2_565 O1 Zr1 Zr2 35.65(7) . 2_565 O2 Zr1 Zr2 35.33(7) 3_556 2_565 O2 Zr1 Zr2 90.46(12) . 2_565 O4 Zr1 Zr2 166.60(7) 10_556 2_565 O4 Zr1 Zr2 75.24(7) 12 2_565 O4 Zr1 Zr2 111.35(7) . 2_565 O4 Zr1 Zr2 110.73(8) 3_556 2_565 Zr2 Zr1 Zr2 91.375(17) 10_556 2_565 Zr2 Zr1 Zr2 60.929(16) 9_566 2_565 Zr2 Zr1 Zr2 60.65(2) . 2_565 O2 Zr2 O2 67.4(2) 11_565 . O2 Zr2 O1 108.9(2) 11_565 . O2 Zr2 O1 72.01(17) . . O2 Zr2 O1 72.01(17) 11_565 2_565 O2 Zr2 O1 108.9(2) . 2_565 O1 Zr2 O1 69.56(17) . 2_565 O2 Zr2 O6 146.05(10) 11_565 . O2 Zr2 O6 146.05(10) . . O1 Zr2 O6 85.97(17) . . O1 Zr2 O6 85.97(17) 2_565 . O2 Zr2 O5 87.42(18) 11_565 . O2 Zr2 O5 87.42(18) . . O1 Zr2 O5 145.14(9) . . O1 Zr2 O5 145.14(9) 2_565 . O6 Zr2 O5 97.35(18) . . O2 Zr2 O3 76.51(13) 11_565 11_565 O2 Zr2 O3 139.55(14) . 11_565 O1 Zr2 O3 139.84(14) . 11_565 O1 Zr2 O3 75.08(13) 2_565 11_565 O6 Zr2 O3 72.95(10) . 11_565 O5 Zr2 O3 72.87(11) . 11_565 O2 Zr2 O3 139.55(14) 11_565 . O2 Zr2 O3 76.51(13) . . O1 Zr2 O3 75.08(13) . . O1 Zr2 O3 139.84(14) 2_565 . O6 Zr2 O3 72.95(10) . . O5 Zr2 O3 72.87(11) . . O3 Zr2 O3 127.14(15) 11_565 . O2 Zr2 Zr1 88.22(13) 11_565 . O2 Zr2 Zr1 36.23(12) . . O1 Zr2 Zr1 35.79(11) . . O1 Zr2 Zr1 89.19(11) 2_565 . O6 Zr2 Zr1 117.68(8) . . O5 Zr2 Zr1 118.70(7) . . O3 Zr2 Zr1 160.74(8) 11_565 . O3 Zr2 Zr1 72.12(8) . . O2 Zr2 Zr1 36.23(12) 11_565 9_566 O2 Zr2 Zr1 88.22(13) . 9_566 O1 Zr2 Zr1 89.19(11) . 9_566 O1 Zr2 Zr1 35.79(11) 2_565 9_566 O6 Zr2 Zr1 117.68(8) . 9_566 O5 Zr2 Zr1 118.70(7) . 9_566 O3 Zr2 Zr1 72.12(8) 11_565 9_566 O3 Zr2 Zr1 160.74(8) . 9_566 Zr1 Zr2 Zr1 88.625(17) . 9_566 O2 Zr2 Zr2 90.32(15) 11_565 2_565 O2 Zr2 Zr2 90.32(15) . 2_565 O1 Zr2 Zr2 34.78(9) . 2_565 O1 Zr2 Zr2 34.78(9) 2_565 2_565 O6 Zr2 Zr2 85.37(13) . 2_565 O5 Zr2 Zr2 177.28(11) . 2_565 O3 Zr2 Zr2 108.07(10) 11_565 2_565 O3 Zr2 Zr2 108.07(10) . 2_565 Zr1 Zr2 Zr2 59.674(10) . 2_565 Zr1 Zr2 Zr2 59.674(10) 9_566 2_565 O2 Zr2 Zr2 33.72(10) 11_565 10_556 O2 Zr2 Zr2 33.72(10) . 10_556 O1 Zr2 Zr2 90.23(13) . 10_556 O1 Zr2 Zr2 90.23(13) 2_565 10_556 O6 Zr2 Zr2 175.37(13) . 10_556 O5 Zr2 Zr2 87.28(11) . 10_556 O3 Zr2 Zr2 108.62(8) 11_565 10_556 O3 Zr2 Zr2 108.62(8) . 10_556 Zr1 Zr2 Zr2 59.535(8) . 10_556 Zr1 Zr2 Zr2 59.535(8) 9_566 10_556 Zr2 Zr2 Zr2 90.0 2_565 10_556 Zr2 O1 Zr2 110.44(18) . 2_565 Zr2 O1 Zr1 108.57(15) . . Zr2 O1 Zr1 108.57(15) 2_565 . Zr2 O2 Zr2 112.6(2) 10_556 . Zr2 O2 Zr1 108.45(16) 10_556 . Zr2 O2 Zr1 108.45(16) . . C1 O3 Zr2 134.0(3) . . C1 O4 Zr1 133.3(2) . . O4 C1 O3 125.0(4) . . O4 C1 C2 117.3(4) . . O3 C1 C2 117.7(4) . . C7 C2 C3 118.4(4) . . C7 C2 C1 122.5(4) . . C3 C2 C1 119.1(4) . . C2 C3 C4 119.7(5) . . C5 C4 C3 121.3(4) . . C6 C5 C4 118.3(4) . . C6 C5 C8 122.0(4) . . C4 C5 C8 119.5(4) . . C7 C6 C5 120.5(4) . . C6 C7 C2 121.6(4) . . C9 C8 C10 120.2(4) . . C9 C8 C5 120.5(4) . . C10 C8 C5 119.1(4) . . C8 C9 C8 121.2(6) 6 . C8 C10 C11 118.2(4) . . C10 C11 C10 121.8(6) . 6 C10 C11 C13 119.1(3) . . C10 C11 C13 119.1(3) 6 . C14 C13 C11 180.000(1) . . C13 C14 C14 180.000(1) . 13 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Zr1 O1 2.153(4) 10_556 Zr1 O1 2.153(4) . Zr1 O2 2.174(5) 3_556 Zr1 O2 2.174(5) . Zr1 O4 2.192(3) 10_556 Zr1 O4 2.192(3) 12 Zr1 O4 2.192(3) . Zr1 O4 2.192(3) 3_556 Zr1 Zr2 3.4901(5) 10_556 Zr1 Zr2 3.4901(5) 9_566 Zr1 Zr2 3.4901(5) . Zr1 Zr2 3.4901(5) 2_565 Zr2 O2 2.127(2) 11_565 Zr2 O2 2.127(2) . Zr2 O1 2.146(2) . Zr2 O1 2.146(2) 2_565 Zr2 O6 2.181(4) . Zr2 O5 2.204(6) . Zr2 O3 2.267(3) 11_565 Zr2 O3 2.267(3) . Zr2 Zr1 3.4901(5) 9_566 Zr2 Zr2 3.5244(13) 2_565 Zr2 Zr2 3.5390(9) 10_556 O1 Zr2 2.146(2) 2_565 O2 Zr2 2.127(2) 10_556 O3 C1 1.273(5) . O4 C1 1.248(5) . C1 C2 1.470(5) . C2 C7 1.375(6) . C2 C3 1.380(5) . C3 C4 1.383(6) . C4 C5 1.374(6) . C5 C6 1.373(5) . C5 C8 1.506(6) . C6 C7 1.366(5) . C8 C9 1.378(5) . C8 C10 1.391(6) . C9 C8 1.378(5) 6 C10 C11 1.398(5) . C11 C10 1.398(5) 6 C11 C13 1.407(11) . C13 C14 1.197(10) . C14 C14 1.357(18) 13