#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:05:56 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242467 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/24/4132494.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_4132494 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 Hf3 O16' _chemical_formula_weight 1342.09 _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 20.5524(17) _cell_length_b 34.409(2) _cell_length_c 21.0160(16) _cell_measurement_reflns_used 512 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 34.316 _cell_measurement_theta_min 4.574 _cell_volume 14862.3(19) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source synchrotron _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.41328 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 79381 _diffrn_reflns_theta_full 12.98 _diffrn_reflns_theta_max 12.98 _diffrn_reflns_theta_min 0.56 _exptl_absorpt_coefficient_mu 1.139 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour 'Light yellow' _exptl_crystal_density_diffrn 0.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2520 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _refine_diff_density_max 3.791 _refine_diff_density_min -2.069 _refine_diff_density_rms 0.171 _refine_ls_extinction_coef 0.0008(2) _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 1.183 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 155 _refine_ls_number_reflns 5348 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.183 _refine_ls_R_factor_all 0.0808 _refine_ls_R_factor_gt 0.0723 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1910P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2391 _refine_ls_wR_factor_ref 0.2524 _reflns_number_gt 4221 _reflns_number_total 5348 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ja8b04277_si_004.cif _cod_data_source_block NPF-300-Hf _cod_original_cell_volume 14862.1(19) _cod_original_sg_symbol_H-M Cmmm _cod_database_code 4132494 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 Hf1 Hf 0.0000 0.070626(17) 0.5000 0.0605(4) Uani 1 4 d S Hf2 Hf 0.08551(3) 0.0000 0.41616(2) 0.0632(4) Uani 1 2 d S O1 O 0.0867(5) 0.0344(3) 0.5000 0.089(3) Uani 1 2 d S O3 O 0.0643(3) 0.10376(15) 0.4380(3) 0.0646(15) Uani 1 1 d . O2 O 0.0000 0.0348(3) 0.4147(5) 0.084(3) Uani 1 2 d S O5 O 0.0787(5) 0.0000 0.3140(4) 0.090(3) Uani 1 2 d S O4 O 0.1191(4) 0.05878(17) 0.3817(3) 0.087(2) Uani 1 1 d . O6 O 0.1920(5) 0.0000 0.4218(5) 0.093(3) Uani 1 2 d S C1 C 0.1027(7) 0.0932(3) 0.3960(5) 0.087(3) Uani 1 1 d . C13 C 0.1397(6) 0.1249(3) 0.3588(5) 0.086(3) Uani 1 1 d . C12 C 0.1748(6) 0.1171(3) 0.3073(4) 0.087(3) Uani 1 1 d . H12A H 0.1816 0.0910 0.2939 0.104 Uiso 1 1 calc R C11 C 0.2500 0.2500 0.2868(5) 0.092(5) Uani 1 2 d S H11A H 0.2500 0.2500 0.3320 0.111 Uiso 1 2 calc SR C10 C 0.1970(6) 0.1853(3) 0.2920(4) 0.096(4) Uani 1 1 d . C9 C 0.2243(7) 0.2188(3) 0.1894(4) 0.110(4) Uani 1 1 d . H9A H 0.2085 0.1972 0.1659 0.132 Uiso 1 1 calc R C8 C 0.2015(7) 0.1481(3) 0.2733(5) 0.107(4) Uani 1 1 d . H8A H 0.2241 0.1426 0.2349 0.128 Uiso 1 1 calc R C7 C 0.2211(6) 0.2184(3) 0.2557(4) 0.104(4) Uani 1 1 d . C6 C 0.1293(7) 0.1633(2) 0.3790(4) 0.097(4) Uani 1 1 d . H6B H 0.1032 0.1689 0.4152 0.117 Uiso 1 1 calc R C5 C 0.1575(7) 0.1919(3) 0.3456(5) 0.112(4) Uani 1 1 d . H5B H 0.1505 0.2179 0.3588 0.134 Uiso 1 1 calc R C4 C 0.2500 0.2500 0.1579(5) 0.105(6) Uani 1 2 d S C3 C 0.2500 0.2500 0.0873(7) 0.170(13) Uani 1 2 d S C2 C 0.2500 0.2500 0.0336(7) 0.151(10) 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 Hf1 0.1193(7) 0.0199(5) 0.0424(5) 0.000 0.000 0.000 Hf2 0.1175(7) 0.0242(4) 0.0478(5) 0.000 0.0044(2) 0.000 O1 0.153(9) 0.062(6) 0.051(5) 0.000 0.000 0.057(6) O3 0.124(4) 0.027(3) 0.043(3) 0.004(2) 0.014(3) -0.002(3) O2 0.076(6) 0.036(5) 0.140(9) -0.040(5) 0.000 0.000 O5 0.165(9) 0.045(5) 0.058(5) 0.000 0.029(5) 0.000 O4 0.160(6) 0.025(3) 0.075(4) -0.006(3) 0.035(4) -0.005(4) O6 0.087(6) 0.081(8) 0.111(8) 0.000 0.020(5) 0.000 C1 0.175(10) 0.034(6) 0.053(5) -0.001(5) 0.018(6) -0.019(6) C13 0.154(9) 0.040(5) 0.065(6) 0.001(4) 0.007(6) -0.016(6) C12 0.150(9) 0.042(5) 0.069(6) -0.006(4) 0.023(6) -0.046(6) C11 0.181(14) 0.053(8) 0.042(6) 0.000 0.000 -0.050(9) C10 0.202(12) 0.037(5) 0.051(5) -0.011(4) 0.011(6) -0.049(6) C9 0.202(13) 0.069(7) 0.058(5) -0.004(5) 0.009(7) -0.063(8) C8 0.195(12) 0.061(7) 0.064(5) -0.012(5) 0.031(7) -0.034(7) C7 0.189(11) 0.068(7) 0.055(5) -0.004(5) 0.018(6) -0.073(7) C6 0.208(12) 0.025(5) 0.060(5) -0.013(4) 0.032(6) -0.029(6) C5 0.212(13) 0.036(6) 0.088(7) -0.021(5) 0.048(8) -0.016(7) C4 0.212(17) 0.071(9) 0.032(6) 0.000 0.000 -0.065(11) C3 0.34(3) 0.111(16) 0.059(10) 0.000 0.000 -0.15(2) C2 0.28(3) 0.126(15) 0.047(7) 0.000 0.000 -0.145(17) 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' Hf Hf -0.3548 4.1643 '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 O2 Hf1 O2 111.0(6) . 10_556 O2 Hf1 O1 71.05(19) . . O2 Hf1 O1 71.05(19) 10_556 . O2 Hf1 O1 71.05(19) . 3_556 O2 Hf1 O1 71.05(19) 10_556 3_556 O1 Hf1 O1 110.0(6) . 3_556 O2 Hf1 O3 142.16(18) . 10_556 O2 Hf1 O3 78.6(3) 10_556 10_556 O1 Hf1 O3 78.7(3) . 10_556 O1 Hf1 O3 142.84(16) 3_556 10_556 O2 Hf1 O3 78.6(3) . . O2 Hf1 O3 142.16(18) 10_556 . O1 Hf1 O3 78.7(3) . . O1 Hf1 O3 142.84(16) 3_556 . O3 Hf1 O3 73.5(3) 10_556 . O2 Hf1 O3 142.16(18) . 3_556 O2 Hf1 O3 78.6(3) 10_556 3_556 O1 Hf1 O3 142.84(16) . 3_556 O1 Hf1 O3 78.7(3) 3_556 3_556 O3 Hf1 O3 74.7(3) 10_556 3_556 O3 Hf1 O3 116.9(3) . 3_556 O2 Hf1 O3 78.6(3) . 12 O2 Hf1 O3 142.16(18) 10_556 12 O1 Hf1 O3 142.84(16) . 12 O1 Hf1 O3 78.7(3) 3_556 12 O3 Hf1 O3 116.9(3) 10_556 12 O3 Hf1 O3 74.7(3) . 12 O3 Hf1 O3 73.5(3) 3_556 12 O2 Hf1 Hf2 35.59(14) . 2 O2 Hf1 Hf2 91.3(2) 10_556 2 O1 Hf1 Hf2 90.8(3) . 2 O1 Hf1 Hf2 35.45(15) 3_556 2 O3 Hf1 Hf2 167.24(15) 10_556 2 O3 Hf1 Hf2 111.65(15) . 2 O3 Hf1 Hf2 111.25(17) 3_556 2 O3 Hf1 Hf2 75.88(14) 12 2 O2 Hf1 Hf2 35.59(14) . . O2 Hf1 Hf2 91.3(2) 10_556 . O1 Hf1 Hf2 35.45(16) . . O1 Hf1 Hf2 90.8(3) 3_556 . O3 Hf1 Hf2 111.25(17) 10_556 . O3 Hf1 Hf2 75.88(14) . . O3 Hf1 Hf2 167.24(14) 3_556 . O3 Hf1 Hf2 111.65(15) 12 . Hf2 Hf1 Hf2 60.698(19) 2 . O2 Hf1 Hf2 91.3(2) . 10_556 O2 Hf1 Hf2 35.59(14) 10_556 10_556 O1 Hf1 Hf2 35.45(16) . 10_556 O1 Hf1 Hf2 90.8(3) 3_556 10_556 O3 Hf1 Hf2 75.88(14) 10_556 10_556 O3 Hf1 Hf2 111.25(17) . 10_556 O3 Hf1 Hf2 111.65(15) 3_556 10_556 O3 Hf1 Hf2 167.24(14) 12 10_556 Hf2 Hf1 Hf2 91.363(18) 2 10_556 Hf2 Hf1 Hf2 60.869(16) . 10_556 O2 Hf1 Hf2 91.3(2) . 9_556 O2 Hf1 Hf2 35.59(14) 10_556 9_556 O1 Hf1 Hf2 90.8(3) . 9_556 O1 Hf1 Hf2 35.45(15) 3_556 9_556 O3 Hf1 Hf2 111.65(15) 10_556 9_556 O3 Hf1 Hf2 167.24(15) . 9_556 O3 Hf1 Hf2 75.88(14) 3_556 9_556 O3 Hf1 Hf2 111.25(17) 12 9_556 Hf2 Hf1 Hf2 60.869(16) 2 9_556 Hf2 Hf1 Hf2 91.363(19) . 9_556 Hf2 Hf1 Hf2 60.698(19) 10_556 9_556 O1 Hf2 O1 67.8(5) . 11 O1 Hf2 O2 109.6(4) . 2 O1 Hf2 O2 73.0(3) 11 2 O1 Hf2 O2 73.0(3) . . O1 Hf2 O2 109.6(4) 11 . O2 Hf2 O2 68.6(4) 2 . O1 Hf2 O5 146.0(2) . . O1 Hf2 O5 146.0(2) 11 . O2 Hf2 O5 86.1(4) 2 . O2 Hf2 O5 86.1(4) . . O1 Hf2 O6 86.8(4) . . O1 Hf2 O6 86.8(4) 11 . O2 Hf2 O6 145.6(2) 2 . O2 Hf2 O6 145.6(2) . . O5 Hf2 O6 96.8(4) . . O1 Hf2 O4 76.3(3) . . O1 Hf2 O4 139.7(3) 11 . O2 Hf2 O4 138.9(3) 2 . O2 Hf2 O4 75.1(3) . . O5 Hf2 O4 72.5(2) . . O6 Hf2 O4 73.2(2) . . O1 Hf2 O4 139.7(3) . 11 O1 Hf2 O4 76.3(3) 11 11 O2 Hf2 O4 75.1(3) 2 11 O2 Hf2 O4 138.9(3) . 11 O5 Hf2 O4 72.5(2) . 11 O6 Hf2 O4 73.2(2) . 11 O4 Hf2 O4 127.3(3) . 11 O1 Hf2 Hf1 88.5(3) . 9_556 O1 Hf2 Hf1 36.5(2) 11 9_556 O2 Hf2 Hf1 36.5(2) 2 9_556 O2 Hf2 Hf1 89.0(3) . 9_556 O5 Hf2 Hf1 118.21(18) . 9_556 O6 Hf2 Hf1 118.50(16) . 9_556 O4 Hf2 Hf1 160.64(16) . 9_556 O4 Hf2 Hf1 72.02(16) 11 9_556 O1 Hf2 Hf1 36.5(2) . . O1 Hf2 Hf1 88.5(3) 11 . O2 Hf2 Hf1 89.0(3) 2 . O2 Hf2 Hf1 36.5(2) . . O5 Hf2 Hf1 118.21(18) . . O6 Hf2 Hf1 118.50(16) . . O4 Hf2 Hf1 72.02(16) . . O4 Hf2 Hf1 160.64(16) 11 . Hf1 Hf2 Hf1 88.637(18) 9_556 . O1 Hf2 Hf2 90.6(3) . 2 O1 Hf2 Hf2 90.6(3) 11 2 O2 Hf2 Hf2 34.3(2) 2 2 O2 Hf2 Hf2 34.3(2) . 2 O5 Hf2 Hf2 86.3(3) . 2 O6 Hf2 Hf2 176.9(3) . 2 O4 Hf2 Hf2 107.8(2) . 2 O4 Hf2 Hf2 107.8(2) 11 2 Hf1 Hf2 Hf2 59.651(10) 9_556 2 Hf1 Hf2 Hf2 59.651(10) . 2 O1 Hf2 Hf2 33.9(2) . 10_556 O1 Hf2 Hf2 33.9(2) 11 10_556 O2 Hf2 Hf2 90.8(3) 2 10_556 O2 Hf2 Hf2 90.8(3) . 10_556 O5 Hf2 Hf2 176.3(3) . 10_556 O6 Hf2 Hf2 86.9(3) . 10_556 O4 Hf2 Hf2 108.73(16) . 10_556 O4 Hf2 Hf2 108.73(16) 11 10_556 Hf1 Hf2 Hf2 59.565(8) 9_556 10_556 Hf1 Hf2 Hf2 59.565(8) . 10_556 Hf2 Hf2 Hf2 90.0 2 10_556 Hf2 O1 Hf2 112.2(5) . 10_556 Hf2 O1 Hf1 108.1(3) . . Hf2 O1 Hf1 108.1(3) 10_556 . C1 O3 Hf1 131.3(5) . . Hf2 O2 Hf2 111.4(4) . 2 Hf2 O2 Hf1 107.9(3) . . Hf2 O2 Hf1 107.9(3) 2 . C1 O4 Hf2 132.8(6) . . O3 C1 O4 127.7(8) . . O3 C1 C13 118.0(8) . . O4 C1 C13 114.1(9) . . C12 C13 C6 121.3(9) . . C12 C13 C1 122.5(8) . . C6 C13 C1 116.0(9) . . C13 C12 C8 118.4(9) . . C7 C11 C7 124.5(11) . 6 C8 C10 C5 115.3(9) . . C8 C10 C7 124.7(9) . . C5 C10 C7 119.2(9) . . C4 C9 C7 120.6(9) . . C10 C8 C12 123.6(9) . . C9 C7 C11 115.9(8) . . C9 C7 C10 123.1(8) . . C11 C7 C10 120.5(8) . . C5 C6 C13 117.8(9) . . C6 C5 C10 123.4(9) . . C9 C4 C9 122.1(11) 6 . C9 C4 C3 118.9(6) 6 . C9 C4 C3 118.9(6) . . C2 C3 C4 180.000(2) . . C3 C2 C2 180.000(2) . 13 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Hf1 O2 2.174(8) . Hf1 O2 2.174(8) 10_556 Hf1 O1 2.175(8) . Hf1 O1 2.175(8) 3_556 Hf1 O3 2.178(5) 10_556 Hf1 O3 2.178(5) . Hf1 O3 2.178(5) 3_556 Hf1 O3 2.178(5) 12 Hf1 Hf2 3.4784(6) 2 Hf1 Hf2 3.4784(6) . Hf1 Hf2 3.4784(6) 10_556 Hf1 Hf2 3.4784(6) 9_556 Hf2 O1 2.122(6) . Hf2 O1 2.122(6) 11 Hf2 O2 2.128(5) 2 Hf2 O2 2.128(5) . Hf2 O5 2.152(9) . Hf2 O6 2.191(10) . Hf2 O4 2.257(6) . Hf2 O4 2.257(6) 11 Hf2 Hf1 3.4784(6) 9_556 Hf2 Hf2 3.5150(12) 2 Hf2 Hf2 3.5240(9) 10_556 O1 Hf2 2.122(6) 10_556 O3 C1 1.238(12) . O2 Hf2 2.128(5) 2 O4 C1 1.269(11) . C1 C13 1.541(13) . C13 C12 1.330(13) . C13 C6 1.404(12) . C12 C8 1.395(13) . C11 C7 1.401(10) . C11 C7 1.401(10) 6 C10 C8 1.341(14) . C10 C5 1.408(14) . C10 C7 1.457(12) . C9 C4 1.368(11) . C9 C7 1.396(13) . C6 C5 1.339(13) . C4 C9 1.368(11) 6 C4 C3 1.485(18) . C3 C2 1.128(17) . C2 C2 1.41(3) 13