#------------------------------------------------------------------------------ #$Date: 2012-11-19 11:53:29 +0200 (Mon, 19 Nov 2012) $ #$Revision: 68671 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/10/86/7108645.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_7108645 loop_ _publ_author_name 'Yun-Nan Gong' 'Miao Meng' 'Di-Chang Zhong' 'Yong-Liang Huang' 'Long Jiang' 'Tong-Bu Lu' _publ_section_title ; Counter-cation modulation of hydrogen and methane storage in a sodalite-type porous metal-organic framework ; _journal_name_full Chem.Commun. _journal_page_first 12002 _journal_volume 48 _journal_year 2012 _chemical_formula_sum 'C56 H24 Cl Cu4 O16' _chemical_formula_weight 1242.40 _chemical_name_systematic ; ? ; _space_group_IT_number 226 _symmetry_cell_setting cubic _symmetry_space_group_name_Hall '-F 4a 2 3' _symmetry_space_group_name_H-M 'F m -3 c' _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 24 _cell_length_a 41.4543(15) _cell_length_b 41.4543(15) _cell_length_c 41.4543(15) _cell_measurement_temperature 173(2) _cell_volume 71238(4) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_molecular_graphics 'Bruker SMART' _computing_publication_material 'Bruker SMART' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 0.0735 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_k_max 52 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_number 90314 _diffrn_reflns_theta_full 27.00 _diffrn_reflns_theta_max 27.00 _diffrn_reflns_theta_min 1.70 _exptl_absorpt_coefficient_mu 0.761 _exptl_absorpt_correction_T_max 0.8210 _exptl_absorpt_correction_T_min 0.8039 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (SHELDRICK,1996)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 0.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 14901 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.27 _platon_squeeze_details ; ; _refine_diff_density_max 0.353 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.046 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 90 _refine_ls_number_reflns 3405 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.068 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0353 _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^)+(0.0514P)^2^+65.2132P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0878 _refine_ls_wR_factor_ref 0.0923 _reflns_number_gt 2920 _reflns_number_total 3405 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c2cc35461f.txt _[local]_cod_data_source_block l10231m _cod_database_code 7108645 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z+1/2' '-x, -y, z' 'y, -x, z+1/2' 'x, -y, -z' 'y, x, -z+1/2' '-x, y, -z' '-y, -x, -z+1/2' 'z, x, y' '-x, z, y+1/2' '-z, -x, y' 'x, -z, y+1/2' 'z, -x, -y' 'x, z, -y+1/2' '-z, x, -y' '-x, -z, -y+1/2' 'y, z, x' '-z+1/2, -y, -x' '-z+1/2, y, x' 'z+1/2, y, -x' 'z+1/2, -y, x' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'x, y+1/2, z+1/2' '-y, x+1/2, z+1' '-x, -y+1/2, z+1/2' 'y, -x+1/2, z+1' 'x, -y+1/2, -z+1/2' 'y, x+1/2, -z+1' '-x, y+1/2, -z+1/2' '-y, -x+1/2, -z+1' 'z, x+1/2, y+1/2' '-x, z+1/2, y+1' '-z, -x+1/2, y+1/2' 'x, -z+1/2, y+1' 'z, -x+1/2, -y+1/2' 'x, z+1/2, -y+1' '-z, x+1/2, -y+1/2' '-x, -z+1/2, -y+1' 'y, z+1/2, x+1/2' '-z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, x+1/2' 'z+1/2, y+1/2, -x+1/2' 'z+1/2, -y+1/2, x+1/2' 'y, -z+1, -x+1' '-y, -z+1, x+1' '-y, z+1, -x+1' 'x+1/2, y, z+1/2' '-y+1/2, x, z+1' '-x+1/2, -y, z+1/2' 'y+1/2, -x, z+1' 'x+1/2, -y, -z+1/2' 'y+1/2, x, -z+1' '-x+1/2, y, -z+1/2' '-y+1/2, -x, -z+1' 'z+1/2, x, y+1/2' '-x+1/2, z, y+1' '-z+1/2, -x, y+1/2' 'x+1/2, -z, y+1' 'z+1/2, -x, -y+1/2' 'x+1/2, z, -y+1' '-z+1/2, x, -y+1/2' '-x+1/2, -z, -y+1' 'y+1/2, z, x+1/2' '-z+1, -y, -x+1/2' '-z+1, y, x+1/2' 'z+1, y, -x+1/2' 'z+1, -y, x+1/2' 'y+1/2, -z+1/2, -x+1' '-y+1/2, -z+1/2, x+1' '-y+1/2, z+1/2, -x+1' 'x+1/2, y+1/2, z' '-y+1/2, x+1/2, z+1/2' '-x+1/2, -y+1/2, z' 'y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, -z' 'y+1/2, x+1/2, -z+1/2' '-x+1/2, y+1/2, -z' '-y+1/2, -x+1/2, -z+1/2' 'z+1/2, x+1/2, y' '-x+1/2, z+1/2, y+1/2' '-z+1/2, -x+1/2, y' 'x+1/2, -z+1/2, y+1/2' 'z+1/2, -x+1/2, -y' 'x+1/2, z+1/2, -y+1/2' '-z+1/2, x+1/2, -y' '-x+1/2, -z+1/2, -y+1/2' 'y+1/2, z+1/2, x' '-z+1, -y+1/2, -x' '-z+1, y+1/2, x' 'z+1, y+1/2, -x' 'z+1, -y+1/2, x' 'y+1/2, -z+1, -x+1/2' '-y+1/2, -z+1, x+1/2' '-y+1/2, z+1, -x+1/2' '-x, -y, -z' 'y, -x, -z-1/2' 'x, y, -z' '-y, x, -z-1/2' '-x, y, z' '-y, -x, z-1/2' 'x, -y, z' 'y, x, z-1/2' '-z, -x, -y' 'x, -z, -y-1/2' 'z, x, -y' '-x, z, -y-1/2' '-z, x, y' '-x, -z, y-1/2' 'z, -x, y' 'x, z, y-1/2' '-y, -z, -x' 'z-1/2, y, x' 'z-1/2, -y, -x' '-z-1/2, -y, x' '-z-1/2, y, -x' '-y, z-1/2, x-1/2' 'y, z-1/2, -x-1/2' 'y, -z-1/2, x-1/2' '-x, -y+1/2, -z+1/2' 'y, -x+1/2, -z' 'x, y+1/2, -z+1/2' '-y, x+1/2, -z' '-x, y+1/2, z+1/2' '-y, -x+1/2, z' 'x, -y+1/2, z+1/2' 'y, x+1/2, z' '-z, -x+1/2, -y+1/2' 'x, -z+1/2, -y' 'z, x+1/2, -y+1/2' '-x, z+1/2, -y' '-z, x+1/2, y+1/2' '-x, -z+1/2, y' 'z, -x+1/2, y+1/2' 'x, z+1/2, y' '-y, -z+1/2, -x+1/2' 'z-1/2, y+1/2, x+1/2' 'z-1/2, -y+1/2, -x+1/2' '-z-1/2, -y+1/2, x+1/2' '-z-1/2, y+1/2, -x+1/2' '-y, z, x' 'y, z, -x' 'y, -z, x' '-x+1/2, -y, -z+1/2' 'y+1/2, -x, -z' 'x+1/2, y, -z+1/2' '-y+1/2, x, -z' '-x+1/2, y, z+1/2' '-y+1/2, -x, z' 'x+1/2, -y, z+1/2' 'y+1/2, x, z' '-z+1/2, -x, -y+1/2' 'x+1/2, -z, -y' 'z+1/2, x, -y+1/2' '-x+1/2, z, -y' '-z+1/2, x, y+1/2' '-x+1/2, -z, y' 'z+1/2, -x, y+1/2' 'x+1/2, z, y' '-y+1/2, -z, -x+1/2' 'z, y, x+1/2' 'z, -y, -x+1/2' '-z, -y, x+1/2' '-z, y, -x+1/2' '-y+1/2, z-1/2, x' 'y+1/2, z-1/2, -x' 'y+1/2, -z-1/2, x' '-x+1/2, -y+1/2, -z' 'y+1/2, -x+1/2, -z-1/2' 'x+1/2, y+1/2, -z' '-y+1/2, x+1/2, -z-1/2' '-x+1/2, y+1/2, z' '-y+1/2, -x+1/2, z-1/2' 'x+1/2, -y+1/2, z' 'y+1/2, x+1/2, z-1/2' '-z+1/2, -x+1/2, -y' 'x+1/2, -z+1/2, -y-1/2' 'z+1/2, x+1/2, -y' '-x+1/2, z+1/2, -y-1/2' '-z+1/2, x+1/2, y' '-x+1/2, -z+1/2, y-1/2' 'z+1/2, -x+1/2, y' 'x+1/2, z+1/2, y-1/2' '-y+1/2, -z+1/2, -x' 'z, y+1/2, x' 'z, -y+1/2, -x' '-z, -y+1/2, x' '-z, y+1/2, -x' '-y+1/2, z, x-1/2' 'y+1/2, z, -x-1/2' '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 Cu1 Cu 0.262905(6) 0.190603(6) 0.0000 0.01762(10) Uani 1 2 d S Cl1 Cl 0.2500 0.2500 0.0000 0.0400(3) Uani 1 8 d S O1 O 0.23442(3) 0.17463(4) 0.03324(3) 0.0465(4) Uani 1 1 d . C1 C 0.20807(4) 0.18324(4) 0.04406(4) 0.0283(4) Uani 1 1 d . C2 C 0.19621(4) 0.16588(5) 0.07350(4) 0.0357(5) Uani 1 1 d . C7 C 0.16920(4) 0.17675(5) 0.08944(4) 0.0387(5) Uani 1 1 d . H7 H 0.1584 0.1947 0.0815 0.046 Uiso 1 1 calc R C6 C 0.15746(5) 0.16165(5) 0.11729(5) 0.0402(5) Uani 1 1 d . C5 C 0.17366(5) 0.13404(5) 0.12892(5) 0.0418(5) Uani 1 1 d . C4 C 0.20130(6) 0.12362(6) 0.11241(6) 0.0619(8) Uani 1 1 d . H4 H 0.2124 0.1057 0.1200 0.074 Uiso 1 1 calc R C3 C 0.21242(5) 0.13914(6) 0.08546(5) 0.0553(7) Uani 1 1 d . H3 H 0.2309 0.1317 0.0751 0.066 Uiso 1 1 calc R O2 O 0.19033(3) 0.20463(4) 0.03349(4) 0.0528(4) Uani 1 1 d . 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 Cu1 0.01611(15) 0.02312(16) 0.01362(15) 0.000 0.000 -0.00116(10) Cl1 0.0184(3) 0.0184(3) 0.0831(10) 0.000 0.000 0.000 O1 0.0413(8) 0.0510(9) 0.0472(9) 0.0250(7) 0.0279(7) 0.0169(6) C1 0.0304(9) 0.0301(9) 0.0243(9) 0.0085(7) 0.0076(7) 0.0021(7) C2 0.0339(10) 0.0401(11) 0.0331(10) 0.0170(8) 0.0183(8) 0.0140(8) C7 0.0368(11) 0.0402(11) 0.0391(10) 0.0223(9) 0.0193(8) 0.0206(8) C6 0.0381(11) 0.0440(11) 0.0383(10) 0.0238(9) 0.0204(9) 0.0212(9) C5 0.0413(11) 0.0434(12) 0.0406(11) 0.0242(9) 0.0241(9) 0.0232(9) C4 0.0574(14) 0.0659(15) 0.0624(14) 0.0437(12) 0.0410(12) 0.0443(12) C3 0.0476(13) 0.0645(15) 0.0537(13) 0.0344(11) 0.0357(11) 0.0369(11) O2 0.0409(8) 0.0667(10) 0.0510(9) 0.0418(8) 0.0219(7) 0.0216(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' 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 Cu1 O1 91.01(10) 99 . O1 Cu1 O2 159.33(6) 99 50_554 O1 Cu1 O2 84.91(7) . 50_554 O1 Cu1 O2 84.91(7) 99 148 O1 Cu1 O2 159.33(6) . 148 O2 Cu1 O2 91.78(11) 50_554 148 O1 Cu1 Cl1 101.84(4) 99 . O1 Cu1 Cl1 101.84(4) . . O2 Cu1 Cl1 98.83(5) 50_554 . O2 Cu1 Cl1 98.83(5) 148 . Cu1 Cl1 Cu1 90.0 122 169 Cu1 Cl1 Cu1 90.0 122 . Cu1 Cl1 Cu1 180.0 169 . Cu1 Cl1 Cu1 180.000(11) 122 50_554 Cu1 Cl1 Cu1 90.0 169 50_554 Cu1 Cl1 Cu1 90.0 . 50_554 C1 O1 Cu1 134.54(13) . . O2 C1 O1 127.38(16) . . O2 C1 C2 116.05(15) . . O1 C1 C2 116.57(16) . . C7 C2 C3 118.96(16) . . C7 C2 C1 120.03(16) . . C3 C2 C1 121.01(16) . . C2 C7 C6 122.15(17) . . C2 C7 H7 118.9 . . C6 C7 H7 118.9 . . C7 C6 C5 118.61(17) . . C7 C6 C5 121.43(17) . 9 C5 C6 C5 119.96(17) . 9 C4 C5 C6 118.13(17) . . C4 C5 C6 121.84(17) . 17 C6 C5 C6 120.04(17) . 17 C3 C4 C5 121.89(18) . . C3 C4 H4 119.1 . . C5 C4 H4 119.1 . . C4 C3 C2 120.24(17) . . C4 C3 H3 119.9 . . C2 C3 H3 119.9 . . C1 O2 Cu1 138.82(12) . 122 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cu1 O1 1.9320(12) 99 Cu1 O1 1.9320(12) . Cu1 O2 1.9334(13) 50_554 Cu1 O2 1.9334(13) 148 Cu1 Cl1 2.5197(3) . Cl1 Cu1 2.5197(3) 122 Cl1 Cu1 2.5197(3) 169 Cl1 Cu1 2.5197(3) 50_554 O1 C1 1.234(2) . C1 O2 1.233(2) . C1 C2 1.500(2) . C2 C7 1.376(2) . C2 C3 1.388(3) . C7 C6 1.400(2) . C7 H7 0.9300 . C6 C5 1.412(3) . C6 C5 1.460(3) 9 C5 C4 1.403(3) . C5 C6 1.460(3) 17 C4 C3 1.369(3) . C4 H4 0.9300 . C3 H3 0.9300 . O2 Cu1 1.9334(13) 122 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 O1 Cu1 Cl1 Cu1 46.79(5) 99 122 O1 Cu1 Cl1 Cu1 -46.79(5) . 122 O2 Cu1 Cl1 Cu1 -133.40(5) 50_554 122 O2 Cu1 Cl1 Cu1 133.40(5) 148 122 O1 Cu1 Cl1 Cu1 -133.21(5) 99 169 O1 Cu1 Cl1 Cu1 133.21(5) . 169 O2 Cu1 Cl1 Cu1 46.60(5) 50_554 169 O2 Cu1 Cl1 Cu1 -46.60(5) 148 169 O1 Cu1 Cl1 Cu1 -133.21(5) 99 50_554 O1 Cu1 Cl1 Cu1 133.21(5) . 50_554 O2 Cu1 Cl1 Cu1 46.60(5) 50_554 50_554 O2 Cu1 Cl1 Cu1 -46.60(5) 148 50_554 O1 Cu1 O1 C1 -74.1(2) 99 . O2 Cu1 O1 C1 126.2(2) 50_554 . O2 Cu1 O1 C1 -152.3(2) 148 . Cl1 Cu1 O1 C1 28.2(2) . . Cu1 O1 C1 O2 7.5(4) . . Cu1 O1 C1 C2 -172.24(15) . . O2 C1 C2 C7 -8.2(3) . . O1 C1 C2 C7 171.6(2) . . O2 C1 C2 C3 173.0(2) . . O1 C1 C2 C3 -7.2(3) . . C3 C2 C7 C6 -0.2(4) . . C1 C2 C7 C6 -179.1(2) . . C2 C7 C6 C5 -1.1(3) . . C2 C7 C6 C5 179.5(2) . 9 C7 C6 C5 C4 1.7(4) . . C5 C6 C5 C4 -178.96(18) 9 . C7 C6 C5 C6 -178.63(15) . 17 C5 C6 C5 C6 0.8(5) 9 17 C6 C5 C4 C3 -0.9(4) . . C6 C5 C4 C3 179.4(3) 17 . C5 C4 C3 C2 -0.4(4) . . C7 C2 C3 C4 1.0(4) . . C1 C2 C3 C4 179.9(2) . . O1 C1 O2 Cu1 -4.2(4) . 122 C2 C1 O2 Cu1 175.49(17) . 122 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 _platon_squeeze_void_content 1 -0.020 -0.039 -0.023 37580 5727 ' ' 2 0.250 0.250 0.250 1437 251 ' ' 3 0.750 0.250 0.250 1437 251 ' ' 4 0.250 0.250 0.750 1437 251 ' ' 5 0.750 0.250 0.750 1437 251 ' ' 6 0.250 0.750 0.250 1437 251 ' ' 7 0.750 0.750 0.250 1437 251 ' ' 8 0.250 0.750 0.750 1437 251 ' ' 9 0.750 0.750 0.750 1437 251 ' '