#------------------------------------------------------------------------------ #$Date: 2016-03-24 14:04:12 +0200 (Thu, 24 Mar 2016) $ #$Revision: 179650 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/03/4510357.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_4510357 loop_ _publ_author_name 'Chun, Hyungphil' 'Bak, Woojeong' 'Hong, Keunil' 'Moon, Dohyun' _publ_section_title ; A Simple and Rational Approach for Binodal Metal--Organic Frameworks with Tetrahedral Nodes and Unexpected Multimodal Porosities from Nonstoichiometric Defects ; _journal_issue 4 _journal_name_full 'Crystal Growth & Design' _journal_page_first 1998 _journal_paper_doi 10.1021/cg500116f _journal_volume 14 _journal_year 2014 _chemical_formula_moiety '[H2NMe2]2[Zn5(hbdc)6(dabco)2]' _chemical_formula_sum 'C64 H64 N6 O30 Zn5' _chemical_formula_weight 1724.06 _chemical_name_systematic ; ? ; _space_group_IT_number 205 _symmetry_cell_setting cubic _symmetry_space_group_name_Hall '-P 2ac 2ab 3' _symmetry_space_group_name_H-M 'P a -3' _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 24.942(3) _cell_length_b 24.942(3) _cell_length_c 24.942(3) _cell_measurement_temperature 100(2) _cell_volume 15517(3) _computing_cell_refinement HKL3000 _computing_data_collection 'PAL ADSC Quantum-210 ADX Program' _computing_data_reduction HKL3000 _computing_molecular_graphics 'Diamond 3' _computing_structure_refinement 'Bruker SHELXTL-XL' _computing_structure_solution 'Bruker SHELXTL-XS' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'ADSC Q210 CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_radiation_monochromator 'Si(111) double crystal monochromator' _diffrn_radiation_source 'PLSII 2D bending magnet' _diffrn_radiation_type Synchrotron _diffrn_radiation_wavelength 0.74999 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 119407 _diffrn_reflns_theta_full 29.99 _diffrn_reflns_theta_max 29.99 _diffrn_reflns_theta_min 1.72 _exptl_absorpt_coefficient_mu 0.922 _exptl_absorpt_correction_T_max 0.8974 _exptl_absorpt_correction_T_min 0.8665 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_process_details 'HKL3000 Scalepack' _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 0.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Octahedral _exptl_crystal_F_000 3520 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _platon_squeeze_details ' ?' _refine_diff_density_max 0.840 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.101 _refine_ls_extinction_coef 0.0046(6) _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 1.059 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 187 _refine_ls_number_reflns 6354 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all 0.0967 _refine_ls_R_factor_gt 0.0709 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1636P)^2^+1.1104P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2181 _refine_ls_wR_factor_ref 0.2343 _reflns_number_gt 4496 _reflns_number_total 6354 _reflns_threshold_expression >2sigma(I) _cod_data_source_file cg500116f_si_002.cif _cod_data_source_block 1 _cod_original_sg_symbol_H-M Pa-3 _cod_database_code 4510357 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.078855(13) 0.078855(13) 0.078855(13) 0.0424(2) Uani 1 3 d S . . Zn2 Zn 0.0000 0.0000 0.0000 0.0427(3) Uani 1 6 d S . . Zn3 Zn 0.231833(13) 0.231833(13) 0.231833(13) 0.0448(2) Uani 1 3 d S . . O1 O 0.00958(9) 0.10986(9) 0.09296(10) 0.0552(6) Uani 1 1 d . . . O2 O -0.03105(9) 0.03320(9) 0.07079(9) 0.0528(5) Uani 1 1 d . . . O3 O 0.26289(10) 0.29179(10) 0.19374(10) 0.0630(7) Uani 1 1 d . . . O4 O 0.30007(11) 0.23898(10) 0.13203(12) 0.0725(7) Uani 1 1 d . . . O5A O -0.21953(15) 0.06184(18) 0.13716(19) 0.1004(14) Uani 0.80 1 d P A 1 O5B O -0.1315(6) 0.0214(7) 0.0920(9) 0.111(7) Uani 0.20 1 d P B 2 N1 N 0.12591(9) 0.12591(9) 0.12591(9) 0.0423(9) Uani 1 3 d S . . N2 N 0.18471(9) 0.18471(9) 0.18471(9) 0.0417(9) Uani 1 3 d S . . C1 C -0.03092(13) 0.07813(12) 0.09209(13) 0.0495(7) Uani 1 1 d . . . C2 C -0.07948(12) 0.09769(13) 0.12063(13) 0.0496(7) Uani 1 1 d . . . C3 C -0.07622(14) 0.14352(17) 0.15205(18) 0.0705(11) Uani 1 1 d . . . H3 H -0.0436 0.1631 0.1540 0.085 Uiso 1 1 calc R . . C4 C -0.12058(14) 0.16036(16) 0.18028(18) 0.0718(11) Uani 1 1 d . . . H4 H -0.1180 0.1909 0.2028 0.086 Uiso 1 1 calc R . . C5 C 0.32373(14) 0.33141(13) 0.13353(14) 0.0562(8) Uani 1 1 d . . . C6 C 0.29391(15) 0.28372(14) 0.15425(15) 0.0594(8) Uani 1 1 d . . . C7 C -0.17184(14) 0.08835(16) 0.14449(16) 0.0644(10) Uani 1 1 d . . . C8 C -0.12771(14) 0.07005(15) 0.11694(15) 0.0595(9) Uani 1 1 d . A . H8 H -0.1302 0.0387 0.0955 0.071 Uiso 1 1 calc R . . C9 C 0.10875(12) 0.12173(12) 0.18271(12) 0.0462(7) Uani 1 1 d . . . H9A H 0.1164 0.0853 0.1964 0.055 Uiso 1 1 calc R . . H9B H 0.0697 0.1281 0.1854 0.055 Uiso 1 1 calc R . . C10 C 0.13910(12) 0.16360(12) 0.21661(12) 0.0444(6) Uani 1 1 d . . . H10A H 0.1147 0.1933 0.2265 0.053 Uiso 1 1 calc R . . H10B H 0.1525 0.1468 0.2500 0.053 Uiso 1 1 calc R . . N1C N -0.2608(3) 0.0024(4) 0.0148(4) 0.069(3) Uani 0.33 1 d P . . H1C1 H -0.2878 -0.0074 -0.0083 0.082 Uiso 0.33 1 calc PR . . H1C2 H -0.2753 0.0256 0.0397 0.082 Uiso 0.33 1 calc PR . . C1C C -0.2414(6) -0.0459(5) 0.0429(7) 0.088(4) Uani 0.33 1 d P . . H1C3 H -0.2544 -0.0780 0.0244 0.133 Uiso 0.33 1 calc PR . . H1C4 H -0.2548 -0.0459 0.0799 0.133 Uiso 0.33 1 calc PR . . H1C5 H -0.2021 -0.0460 0.0432 0.133 Uiso 0.33 1 calc PR . . C2C C -0.2212(7) 0.0296(9) -0.0142(6) 0.123(7) Uani 0.33 1 d P . . H2C1 H -0.1858 0.0200 -0.0002 0.185 Uiso 0.33 1 calc PR . . H2C2 H -0.2266 0.0684 -0.0105 0.185 Uiso 0.33 1 calc PR . . H2C3 H -0.2235 0.0196 -0.0521 0.185 Uiso 0.33 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0424(2) 0.0424(2) 0.0424(2) 0.00015(13) 0.00015(13) 0.00015(13) Zn2 0.0427(3) 0.0427(3) 0.0427(3) -0.00037(18) -0.00037(18) -0.00037(18) Zn3 0.0448(2) 0.0448(2) 0.0448(2) -0.00094(14) -0.00094(14) -0.00094(14) O1 0.0437(12) 0.0514(12) 0.0704(15) -0.0032(11) 0.0053(10) -0.0016(9) O2 0.0542(13) 0.0527(13) 0.0517(12) -0.0063(10) 0.0095(10) -0.0009(10) O3 0.0666(16) 0.0512(13) 0.0712(16) 0.0044(11) 0.0130(12) -0.0062(11) O4 0.0755(17) 0.0469(14) 0.095(2) -0.0064(13) 0.0174(14) -0.0108(11) O5A 0.056(2) 0.117(3) 0.127(3) -0.040(3) 0.015(2) -0.017(2) O5B 0.057(8) 0.083(11) 0.192(19) -0.064(11) 0.040(10) -0.030(8) N1 0.0423(9) 0.0423(9) 0.0423(9) -0.0020(9) -0.0020(9) -0.0020(9) N2 0.0417(9) 0.0417(9) 0.0417(9) 0.0013(10) 0.0013(10) 0.0013(10) C1 0.0489(17) 0.0507(18) 0.0487(16) -0.0008(13) 0.0018(13) 0.0028(13) C2 0.0441(16) 0.0551(18) 0.0498(17) -0.0049(14) 0.0030(12) 0.0009(13) C3 0.0472(19) 0.072(2) 0.093(3) -0.026(2) 0.0148(18) -0.0081(16) C4 0.051(2) 0.067(2) 0.097(3) -0.029(2) 0.0120(19) -0.0014(16) C5 0.0571(19) 0.0420(16) 0.069(2) -0.0010(14) 0.0048(16) -0.0076(14) C6 0.060(2) 0.0490(19) 0.069(2) 0.0025(16) 0.0022(17) -0.0056(15) C7 0.0455(18) 0.076(2) 0.071(2) -0.0151(18) 0.0100(16) -0.0122(16) C8 0.0502(18) 0.066(2) 0.062(2) -0.0172(17) 0.0035(15) -0.0055(15) C9 0.0488(16) 0.0464(16) 0.0435(16) 0.0017(12) 0.0019(12) -0.0026(12) C10 0.0408(15) 0.0520(17) 0.0404(15) 0.0009(12) 0.0008(11) -0.0027(12) N1C 0.041(5) 0.107(8) 0.058(5) -0.017(5) 0.010(4) 0.010(4) C1C 0.084(9) 0.062(7) 0.119(11) -0.011(7) -0.028(8) 0.012(6) C2C 0.094(11) 0.21(2) 0.062(8) 0.001(10) 0.021(7) -0.072(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0036 0.0018 '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' N N 0.0070 0.0037 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0123 0.0068 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2523 1.5758 '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 Zn1 O1 116.81(4) 9 5 O1 Zn1 O1 116.81(4) 9 . O1 Zn1 O1 116.81(4) 5 . O1 Zn1 N1 100.42(7) 9 . O1 Zn1 N1 100.42(7) 5 . O1 Zn1 N1 100.41(7) . . O2 Zn2 O2 180.00(16) 21 9 O2 Zn2 O2 97.14(8) 21 13 O2 Zn2 O2 82.86(8) 9 13 O2 Zn2 O2 82.86(8) 21 5 O2 Zn2 O2 97.14(8) 9 5 O2 Zn2 O2 82.86(8) 13 5 O2 Zn2 O2 97.14(8) 21 17 O2 Zn2 O2 82.86(8) 9 17 O2 Zn2 O2 97.14(8) 13 17 O2 Zn2 O2 180.00(16) 5 17 O2 Zn2 O2 82.86(8) 21 . O2 Zn2 O2 97.14(8) 9 . O2 Zn2 O2 180.0 13 . O2 Zn2 O2 97.14(8) 5 . O2 Zn2 O2 82.86(8) 17 . O3 Zn3 O3 105.49(9) . 9 O3 Zn3 O3 105.49(9) . 5 O3 Zn3 O3 105.49(9) 9 5 O3 Zn3 N2 113.21(8) . . O3 Zn3 N2 113.21(8) 9 . O3 Zn3 N2 113.21(8) 5 . C1 O1 Zn1 117.1(2) . . C1 O2 Zn2 135.7(2) . . C6 O3 Zn3 120.2(2) . . C9 N1 C9 108.80(19) . 9 C9 N1 C9 108.80(19) . 5 C9 N1 C9 108.80(19) 9 5 C9 N1 Zn1 110.13(18) . . C9 N1 Zn1 110.13(18) 9 . C9 N1 Zn1 110.13(18) 5 . C10 N2 C10 109.20(19) . 9 C10 N2 C10 109.20(19) . 5 C10 N2 C10 109.20(19) 9 5 C10 N2 Zn3 109.74(18) . . C10 N2 Zn3 109.74(18) 9 . C10 N2 Zn3 109.74(18) 5 . O2 C1 O1 124.5(3) . . O2 C1 C2 119.9(3) . . O1 C1 C2 115.5(3) . . C3 C2 C8 119.8(3) . . C3 C2 C1 119.5(3) . . C8 C2 C1 120.7(3) . . C4 C3 C2 119.5(3) . . C5 C4 C3 120.9(4) 24_556 . C4 C5 C7 119.4(3) 18_665 18_665 C4 C5 C6 119.2(3) 18_665 . C7 C5 C6 121.4(3) 18_665 . O4 C6 O3 123.9(3) . . O4 C6 C5 119.6(3) . . O3 C6 C5 116.5(3) . . O5A C7 C8 117.8(3) . . O5A C7 C5 121.4(3) . 24_556 C8 C7 C5 120.7(3) . 24_556 C7 C8 C2 119.7(3) . . N1 C9 C10 109.5(3) . . N2 C10 C9 108.8(3) . . C2C N1C C1C 114.2(13) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Zn1 O1 1.925(2) 9 Zn1 O1 1.925(2) 5 Zn1 O1 1.926(2) . Zn1 N1 2.033(4) . Zn2 O2 2.098(2) 21 Zn2 O2 2.098(2) 9 Zn2 O2 2.098(2) 13 Zn2 O2 2.098(2) 5 Zn2 O2 2.098(2) 17 Zn2 O2 2.098(2) . Zn3 O3 1.934(2) . Zn3 O3 1.934(2) 9 Zn3 O3 1.934(2) 5 Zn3 N2 2.036(4) . O1 C1 1.283(4) . O2 C1 1.240(4) . O3 C6 1.268(4) . O4 C6 1.256(4) . O5A C7 1.373(5) . N1 C9 1.484(3) . N1 C9 1.484(3) 9 N1 C9 1.484(3) 5 N2 C10 1.485(3) . N2 C10 1.485(3) 9 N2 C10 1.485(3) 5 C1 C2 1.487(4) . C2 C3 1.388(5) . C2 C8 1.389(5) . C3 C4 1.377(5) . C4 C5 1.376(5) 24_556 C5 C4 1.376(5) 18_665 C5 C7 1.380(5) 18_665 C5 C6 1.495(5) . C7 C8 1.376(5) . C7 C5 1.380(5) 24_556 C9 C10 1.542(4) . N1C C2C 1.400(16) . N1C C1C 1.477(17) . loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.008 -0.005 0.410 8284.0 619.3