#------------------------------------------------------------------------------ #$Date: 2015-03-02 10:35:10 +0200 (Mon, 02 Mar 2015) $ #$Revision: 132589 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/00/16/4001670.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_4001670 loop_ _publ_author_name 'Zhai, Quan-Guo' 'Lin, Qipu' 'Wu, Tao' 'Wang, Le' 'Zheng, Shou-Tian' 'Bu, Xianhui' 'Feng, Pingyun' _publ_section_title ; High CO2and H2Uptake in an Anionic Porous Framework with Amino-Decorated Polyhedral Cages ; _journal_issue 14 _journal_name_full 'Chemistry of Materials' _journal_page_first 2624 _journal_paper_doi 10.1021/cm301322b _journal_volume 24 _journal_year 2012 _chemical_formula_sum 'C26 H16 N5 O12 Zn3' _chemical_formula_weight 786.55 _chemical_name_systematic ? _space_group_IT_number 136 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-P 4n 2n' _symmetry_space_group_name_H-M 'P 42/m n 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 20.1749(2) _cell_length_b 20.1749(2) _cell_length_c 16.3257(3) _cell_measurement_reflns_used 5832 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 25.02 _cell_measurement_theta_min 2.50 _cell_volume 6644.99(15) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 24093 _diffrn_reflns_theta_full 25.10 _diffrn_reflns_theta_max 25.10 _diffrn_reflns_theta_min 1.43 _exptl_absorpt_coefficient_mu 1.106 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 0.786 _exptl_crystal_density_method 'not measured' _exptl_crystal_description octahedron _exptl_crystal_F_000 1572 _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.28 _platon_squeeze_details ? _refine_diff_density_max 0.918 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.071 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 141 _refine_ls_number_reflns 3193 _refine_ls_number_restraints 10 _refine_ls_restrained_S_all 1.163 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0468 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1071P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1441 _refine_ls_wR_factor_ref 0.1489 _reflns_number_gt 2620 _reflns_number_total 3193 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file cm301322b_si_002.cif _[local]_cod_data_source_block cpf-13 _[local]_cod_cif_authors_sg_H-M P4(2)/mnm _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius ; _cod_database_code 4001670 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y, x, -z' '-y, -x, -z' '-x, -y, -z' 'x, y, -z' 'y-1/2, -x-1/2, -z-1/2' '-y-1/2, x-1/2, -z-1/2' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' '-y, -x, z' 'y, x, 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 Zn1 Zn 0.05178(2) 0.94822(2) 0.0000 0.0329(2) Uani 1 4 d S Zn2 Zn 0.31390(2) 0.80437(2) 0.0000 0.0353(2) Uani 1 2 d S C1 C 0.1873(2) 0.8857(2) 0.0000 0.0409(10) Uani 1 2 d S C2 C -0.06315(15) 0.93685(15) -0.1117(3) 0.0445(11) Uani 1 2 d S C3 C -0.09863(16) 0.90137(16) -0.1798(3) 0.0464(11) Uani 1 2 d S C4 C -0.0734(2) 0.8434(2) -0.2124(3) 0.0739(13) Uani 1 1 d . H4A H -0.0349 0.8252 -0.1906 0.089 Uiso 1 1 calc R C5 C -0.1041(2) 0.81264(19) -0.2755(3) 0.0798(14) Uani 1 1 d . H5A H -0.0861 0.7740 -0.2972 0.096 Uiso 1 1 calc R C6 C -0.16200(17) 0.83800(17) -0.3079(3) 0.0517(12) Uani 1 2 d S C7 C -0.19506(18) 0.80494(18) -0.3784(3) 0.0592(14) Uani 1 2 d S C8 C 0.3907(3) 0.9103(3) 0.0000 0.164(6) Uani 1 2 d SD C9 C 0.4477(3) 0.9565(3) 0.0000 0.076(2) Uani 1 2 d SD C10 C 0.4943(4) 0.9469(4) 0.0559(6) 0.093(3) Uani 0.50 1 d PD C11 C 0.4540(5) 1.0066(5) -0.0594(5) 0.094(3) Uani 0.50 1 d PD N1 N 0.21961(17) 0.82951(16) 0.0000 0.0388(8) Uani 1 2 d S N2 N 0.12107(15) 0.87893(15) 0.0000 0.0339(10) Uani 1 4 d S N3 N 0.2171(2) 0.9458(2) 0.0000 0.104(2) Uani 1 2 d S H3A H 0.2597 0.9485 0.0000 0.124 Uiso 1 2 calc SR H3B H 0.1935 0.9813 0.0000 0.124 Uiso 1 2 calc SR O1 O -0.01151(12) 0.91185(15) -0.08529(18) 0.0776(9) Uani 1 1 d . O2 O -0.16918(16) 0.75277(13) -0.40578(17) 0.0746(8) Uani 1 1 d . O3 O 0.3834(3) 0.8606(3) 0.0352(4) 0.100(3) Uani 0.50 1 d PD O4 O 0.3529(3) 0.9136(4) -0.0620(4) 0.128(3) Uani 0.50 1 d PD 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 0.0315(3) 0.0315(3) 0.0359(4) 0.000 0.000 0.0044(3) Zn2 0.0296(3) 0.0290(3) 0.0472(4) 0.000 0.000 -0.00031(18) C1 0.033(2) 0.024(2) 0.066(3) 0.000 0.000 -0.0008(16) C2 0.0441(16) 0.0441(16) 0.045(2) -0.0093(14) -0.0093(14) 0.000(2) C3 0.0435(15) 0.0435(15) 0.052(3) -0.0113(15) -0.0113(15) 0.006(2) C4 0.074(3) 0.060(2) 0.088(3) -0.031(2) -0.044(2) 0.026(2) C5 0.090(3) 0.057(2) 0.093(3) -0.033(2) -0.040(3) 0.030(2) C6 0.0486(17) 0.0486(17) 0.058(3) -0.0159(17) -0.0159(17) -0.002(2) C7 0.061(2) 0.061(2) 0.056(3) -0.0084(17) -0.0084(17) -0.017(3) C8 0.018(3) 0.097(7) 0.376(19) 0.000 0.000 -0.021(4) C9 0.054(4) 0.037(3) 0.136(6) 0.000 0.000 -0.022(3) C10 0.072(6) 0.073(6) 0.134(8) 0.045(6) -0.042(6) -0.037(5) C11 0.086(7) 0.108(8) 0.089(7) 0.014(6) -0.021(5) -0.041(6) N1 0.0295(19) 0.0259(17) 0.061(2) 0.000 0.000 -0.0030(14) N2 0.0299(15) 0.0299(15) 0.042(3) 0.000 0.000 0.0046(19) N3 0.027(2) 0.029(2) 0.255(8) 0.000 0.000 -0.0050(17) O1 0.0524(16) 0.0836(19) 0.097(2) -0.0475(17) -0.0422(15) 0.0336(14) O2 0.100(2) 0.0484(16) 0.0752(18) -0.0212(14) -0.0310(16) -0.0010(14) O3 0.076(4) 0.039(3) 0.185(9) 0.005(3) -0.032(4) -0.032(3) O4 0.058(4) 0.098(6) 0.227(9) -0.044(6) 0.042(5) -0.047(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 N2 Zn1 O1 100.92(7) . 8_665 N2 Zn1 O1 100.92(7) . . O1 Zn1 O1 158.15(15) 8_665 . N2 Zn1 O1 100.92(7) . 15_665 O1 Zn1 O1 86.79(19) 8_665 15_665 O1 Zn1 O1 89.1(2) . 15_665 N2 Zn1 O1 100.92(7) . 10 O1 Zn1 O1 89.1(2) 8_665 10 O1 Zn1 O1 86.79(19) . 10 O1 Zn1 O1 158.15(15) 15_665 10 N2 Zn1 Zn1 180.00(3) . 9_575 O1 Zn1 Zn1 79.08(7) 8_665 9_575 O1 Zn1 Zn1 79.08(7) . 9_575 O1 Zn1 Zn1 79.08(7) 15_665 9_575 O1 Zn1 Zn1 79.08(7) 10 9_575 O3 Zn2 O3 35.4(4) . 10 O3 Zn2 O2 117.6(2) . 6_564 O3 Zn2 O2 89.1(2) 10 6_564 O3 Zn2 O2 89.1(2) . 13_676 O3 Zn2 O2 117.6(2) 10 13_676 O2 Zn2 O2 103.98(18) 6_564 13_676 O3 Zn2 N1 124.2(2) . . O3 Zn2 N1 124.2(2) 10 . O2 Zn2 N1 108.72(11) 6_564 . O2 Zn2 N1 108.72(11) 13_676 . N1 C1 N2 114.1(4) . . N1 C1 N3 123.7(4) . . N2 C1 N3 122.2(4) . . O1 C2 O1 124.5(4) 16_465 . O1 C2 C3 117.7(2) 16_465 . O1 C2 C3 117.7(2) . . C4 C3 C4 118.3(4) 16_465 . C4 C3 C2 120.8(2) 16_465 . C4 C3 C2 120.8(2) . . C5 C4 C3 120.9(4) . . C4 C5 C6 120.6(4) . . C5 C6 C5 118.7(4) 16_465 . C5 C6 C7 120.6(2) 16_465 . C5 C6 C7 120.6(2) . . O2 C7 O2 124.7(5) . 16_465 O2 C7 C6 117.7(2) . . O2 C7 C6 117.7(2) 16_465 . O3 C8 O3 59.2(8) . 10 O3 C8 O4 111.4(6) . . O3 C8 O4 64.9(5) 10 . O3 C8 O4 64.9(5) . 10 O3 C8 O4 111.4(6) 10 10 O4 C8 O4 105.9(7) . 10 O3 C8 C9 129.8(6) . . O3 C8 C9 129.8(6) 10 . O4 C8 C9 115.6(4) . . O4 C8 C9 115.6(4) 10 . C10 C9 C10 87.1(11) 10 . C10 C9 C11 121.1(6) 10 10 C10 C9 C11 64.3(6) . 10 C10 C9 C11 64.3(6) 10 . C10 C9 C11 121.1(6) . . C11 C9 C11 87.2(9) 10 . C10 C9 C8 117.3(5) 10 . C10 C9 C8 117.3(5) . . C11 C9 C8 121.5(5) 10 . C11 C9 C8 121.5(5) . . C9 C10 C11 117.2(7) . 9_675 C9 C10 C11 60.5(5) . 10 C11 C10 C11 82.0(9) 9_675 10 C9 C10 C10 46.5(5) . 10 C11 C10 C10 92.3(6) 9_675 10 C11 C10 C10 92.2(6) 10 10 C10 C11 C9 121.3(7) 9_675 . C10 C11 C10 97.8(8) 9_675 10 C9 C11 C10 55.1(5) . 10 C10 C11 C11 50.2(6) 9_675 2_675 C9 C11 C11 89.3(7) . 2_675 C10 C11 C11 47.8(6) 10 2_675 C10 C11 C11 87.7(6) 9_675 10 C9 C11 C11 46.4(5) . 10 C10 C11 C11 87.8(6) 10 10 C11 C11 C11 90.000(2) 2_675 10 C1 N1 N1 105.1(2) . 15_665 C1 N1 Zn2 134.8(3) . . N1 N1 Zn2 120.07(9) 15_665 . C1 N2 C1 101.6(5) . 15_665 C1 N2 Zn1 129.2(2) . . C1 N2 Zn1 129.2(2) 15_665 . C2 O1 Zn1 128.6(2) . . C7 O2 Zn2 134.6(3) . 13_575 O3 O3 C8 60.4(4) 10 . O3 O3 O4 109.5(4) 10 10 C8 O3 O4 61.3(3) . 10 O3 O3 Zn2 72.3(2) 10 . C8 O3 Zn2 117.3(5) . . O4 O3 Zn2 104.1(5) 10 . C8 O4 O3 53.7(4) . 10 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Zn1 N2 1.977(4) . Zn1 O1 2.027(2) 8_665 Zn1 O1 2.027(2) . Zn1 O1 2.027(2) 15_665 Zn1 O1 2.027(2) 10 Zn1 Zn1 2.9546(12) 9_575 Zn2 O3 1.892(5) . Zn2 O3 1.892(5) 10 Zn2 O2 1.952(2) 6_564 Zn2 O2 1.952(2) 13_676 Zn2 N1 1.969(3) . C1 N1 1.307(5) . C1 N2 1.343(5) . C1 N3 1.354(6) . C2 O1 1.235(3) 16_465 C2 O1 1.235(3) . C2 C3 1.503(6) . C3 C4 1.383(4) 16_465 C3 C4 1.383(4) . C4 C5 1.352(6) . C5 C6 1.380(5) . C6 C5 1.380(5) 16_465 C6 C7 1.488(7) . C7 O2 1.257(3) . C7 O2 1.257(3) 16_465 C8 O3 1.165(5) . C8 O3 1.165(5) 10 C8 O4 1.268(5) . C8 O4 1.268(5) 10 C8 C9 1.482(7) . C9 C10 1.325(7) 10 C9 C10 1.325(7) . C9 C11 1.406(7) 10 C9 C11 1.406(7) . C10 C11 1.405(11) 9_675 C10 C11 1.455(14) 10 C10 C10 1.825(19) 10 C11 C10 1.405(11) 9_675 C11 C10 1.455(15) 10 C11 C11 1.88(2) 2_675 C11 C11 1.939(18) 10 N1 N1 1.401(6) 15_665 N2 C1 1.343(5) 15_665 O2 Zn2 1.952(2) 13_575 O3 O3 1.150(14) 10 O3 O4 1.309(9) 10 O4 O3 1.309(9) 10 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 0.095 0.328 -0.018 4358.9 1011.7