#------------------------------------------------------------------------------ #$Date: 2015-01-23 14:30:19 +0200 (Fri, 23 Jan 2015) $ #$Revision: 130086 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/33/98/4339875.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_4339875 loop_ _publ_author_name 'Dybtsev, Danil N.' 'Yutkin, Maxim P.' 'Peresypkina, Eugenia V.' 'Virovets, Alexander V.' 'Serre, Christian' 'F\'erey, G\'erard' 'Fedin, Vladimir P.' _publ_section_title ; Isoreticular homochiral porous metal-organic structures with tunable pore sizes. ; _journal_issue 17 _journal_name_full 'Inorganic chemistry' _journal_page_first 6843 _journal_page_last 6845 _journal_paper_doi 10.1021/ic7009226 _journal_volume 46 _journal_year 2007 _chemical_formula_sum 'C30 H36 N2 O8 Zn2' _chemical_formula_weight 683.35 _chemical_name_systematic ; ? ; _space_group_IT_number 120 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'I -4 -2c' _symmetry_space_group_name_H-M 'I -4 c 2' _atom_sites_solution_hydrogens none _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 13.3433(3) _cell_length_b 13.3433(3) _cell_length_c 27.8994(12) _cell_measurement_reflns_used 2525 _cell_measurement_temperature 90.0(2) _cell_measurement_theta_max 25.6862 _cell_measurement_theta_min 2.6062 _cell_volume 4967.3(3) _computing_cell_refinement 'Apex2 V.1.27 (Bruker, 2005)' _computing_data_collection 'Apex2 V.1.27 (Bruker, 2005)' _computing_data_reduction 'Apex2 V.1.27 (Bruker, 2005)' _computing_molecular_graphics 'SHELXTL V6.22 (Bruker, 2000-2005)' _computing_publication_material 'local programs' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 90.0(2) _diffrn_detector_area_resol_mean 25 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker X8Apex CCD detector' _diffrn_measurement_method 'combined omega- and phi-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 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 8447 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 1.46 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.997 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.625873 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'based on intensities (SADABS, Bruker, 2005)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 0.914 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1416 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.870 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.170 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.26(7) _refine_ls_extinction_coef 0.0016(4) _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 1.190 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 119 _refine_ls_number_reflns 2830 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.190 _refine_ls_R_factor_all 0.1194 _refine_ls_R_factor_gt 0.0755 _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^)+(0.1400P)^2^+14.7949P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2269 _refine_ls_wR_factor_ref 0.2740 _reflns_number_gt 1770 _reflns_number_total 2830 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic7009226-file002.cif _[local]_cod_data_source_block 2_I _[local]_cod_cif_authors_sg_H-M I-4c2 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'none' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_database_code 4339875 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x, -y, z+1/2' '-x, y, z+1/2' 'y, x, -z+1/2' '-y, -x, -z+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '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' '-x+1/2, y+1/2, z+1' 'y+1/2, x+1/2, -z+1' '-y+1/2, -x+1/2, -z+1' 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 0.0000 0.0000 0.05120(3) 0.0312(4) Uani 1 2 d S . . N1 N 0.0000 0.0000 0.1237(3) 0.053(3) Uani 1 2 d S . . C9 C 0.0000 0.0000 0.2230(3) 0.070(4) Uani 1 2 d S . . C10A C 0.089(2) 0.006(2) 0.1979(8) 0.062(6) Uiso 0.45 1 d P A 1 C11A C 0.0803(16) 0.0189(15) 0.1476(7) 0.046(4) Uiso 0.45 1 d P A 1 C10B C 0.069(3) -0.060(3) 0.1982(9) 0.103(9) Uiso 0.55 1 d P A 2 C11B C 0.0765(14) -0.0426(16) 0.1481(6) 0.059(4) Uiso 0.55 1 d P A 2 O1 O 0.1493(5) -0.0366(6) 0.0387(3) 0.0496(17) Uani 1 1 d . . . O2 O 0.1417(5) -0.0368(8) -0.0398(4) 0.069(2) Uani 1 1 d . . . C1 C 0.2967(4) -0.0749(4) 0.0002(6) 0.056(2) Uani 1 1 d . . . C2 C 0.1863(5) -0.0457(5) 0.0038(6) 0.0390(18) Uani 1 1 d . A . C3 C 0.3455(13) -0.0682(15) -0.0488(10) 0.054(6) Uani 0.50 1 d P A . C4 C 0.4347(15) -0.138(2) -0.0370(11) 0.055(7) Uani 0.50 1 d P . . C5 C 0.3158(12) -0.1907(15) 0.0207(5) 0.040(3) Uani 0.50 1 d P A . C6 C 0.3527(18) -0.014(2) 0.0412(12) 0.073(7) Uani 0.50 1 d P A . C7 C 0.2435(5) -0.2565(5) 0.0000 0.098(6) Uani 1 2 d S . . C8 C 0.2946(19) -0.2166(18) 0.0713(7) 0.075(6) Uani 0.50 1 d P . . 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 0.0350(11) 0.0308(10) 0.0277(5) 0.000 0.000 -0.0070(5) N1 0.044(11) 0.089(16) 0.027(3) 0.000 0.000 -0.003(7) C9 0.08(2) 0.11(3) 0.024(5) 0.000 0.000 -0.009(12) O1 0.029(3) 0.059(4) 0.060(5) 0.002(5) -0.003(4) -0.006(3) O2 0.038(4) 0.097(6) 0.072(6) 0.021(6) 0.002(4) 0.039(4) C1 0.020(3) 0.024(3) 0.123(7) -0.024(7) -0.015(8) 0.002(2) C2 0.027(3) 0.025(3) 0.065(5) 0.005(6) -0.006(6) 0.000(2) C3 0.032(8) 0.049(12) 0.082(16) 0.017(12) 0.020(11) 0.013(7) C4 0.018(8) 0.072(15) 0.074(14) -0.019(11) 0.023(10) -0.008(9) C5 0.008(8) 0.044(12) 0.068(7) -0.014(11) 0.013(9) -0.010(4) C6 0.046(12) 0.061(14) 0.11(2) -0.026(18) -0.037(13) 0.005(11) C7 0.024(3) 0.024(3) 0.245(19) -0.002(9) 0.002(9) -0.007(4) C8 0.077(17) 0.067(16) 0.081(11) 0.033(12) 0.030(12) 0.037(10) 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 N1 Zn1 Zn1 180.0 . 3 N1 Zn1 O1 99.6(2) . 2 N1 Zn1 O1 99.6(2) . . O1 Zn1 Zn1 80.4(2) 2 3 O1 Zn1 Zn1 80.4(2) . 3 O1 Zn1 O1 160.7(5) 2 . O2 Zn1 Zn1 80.8(3) 3 3 O2 Zn1 Zn1 80.8(3) 4 3 O2 Zn1 N1 99.2(3) 3 . O2 Zn1 N1 99.2(3) 4 . O2 Zn1 O1 87.7(5) 3 2 O2 Zn1 O1 89.3(5) 4 2 O2 Zn1 O1 89.3(5) 3 . O2 Zn1 O1 87.7(5) 4 . O2 Zn1 O2 161.5(6) 3 4 C11A N1 Zn1 121.2(9) 2 . C11A N1 Zn1 121.2(9) . . C11A N1 C11A 117.6(18) 2 . C11A N1 C11B 106.6(11) 2 . C11A N1 C11B 36.2(10) . . C11A N1 C11B 36.2(10) 2 2 C11A N1 C11B 106.6(11) . 2 C11B N1 Zn1 120.2(8) . . C11B N1 Zn1 120.2(8) 2 . C11B N1 C11B 119.6(16) . 2 C10A C9 C9 120.4(10) 2 7 C10A C9 C9 120.4(10) . 7 C10A C9 C10A 119(2) 2 . C10A C9 C10B 106.3(12) 2 . C10A C9 C10B 38.9(12) . . C10A C9 C10B 38.9(12) 2 2 C10A C9 C10B 106.3(12) . 2 C10B C9 C9 119.5(12) . 7 C10B C9 C9 119.5(12) 2 7 C10B C9 C10B 121(2) . 2 C9 C10A C11A 116(2) . . N1 C11A C10A 124.1(19) . . C9 C10B C11B 116(2) . . N1 C11B C10B 121(2) . . C2 O1 Zn1 127.3(7) . . C2 O2 Zn1 125.7(7) . 3 C2 C1 C3 117.3(14) . . C2 C1 C5 111.3(9) . 15_544 C2 C1 C5 111.2(9) . . C2 C1 C6 105.9(13) . . C3 C1 C5 107.4(10) . . C4 C1 C2 123.1(16) 15_544 . C4 C1 C3 113.8(14) 15_544 . C4 C1 C5 107.5(12) 15_544 15_544 C4 C1 C5 74.2(11) 15_544 . C4 C1 C6 26.1(10) 15_544 . C5 C1 C3 71.1(11) 15_544 . C5 C1 C5 41.9(9) 15_544 . C6 C1 C3 114.7(15) . . C6 C1 C5 133.4(13) . 15_544 C6 C1 C5 98.9(13) . . O1 C2 O2 125.9(7) . . O1 C2 C1 121.4(13) . . O2 C2 C1 112.6(13) . . C1 C3 C5 56.1(9) . 15_544 C4 C3 C1 95.9(19) . . C4 C3 C5 66.1(15) . 15_544 C1 C4 C3 118.5(18) 15_544 . C1 C4 C5 60.8(11) 15_544 15_544 C3 C4 C5 63.5(13) . 15_544 C6 C4 C1 96(4) 15_544 15_544 C6 C4 C3 145(4) 15_544 . C6 C4 C5 150(4) 15_544 15_544 C1 C5 C1 96.5(7) 15_544 . C1 C5 C3 52.8(10) 15_544 15_544 C1 C5 C3 91.9(9) . 15_544 C1 C5 C4 83.1(10) 15_544 15_544 C1 C5 C4 45.0(11) . 15_544 C3 C5 C4 50.3(10) 15_544 15_544 C5 C5 C1 73.1(17) 15_544 15_544 C5 C5 C1 65.0(17) 15_544 . C5 C5 C3 118.5(13) 15_544 15_544 C5 C5 C4 101.6(16) 15_544 15_544 C5 C5 C7 65.9(5) 15_544 . C5 C5 C8 162.0(12) 15_544 . C7 C5 C1 114.2(13) . 15_544 C7 C5 C1 109.1(11) . . C7 C5 C3 157.3(17) . 15_544 C7 C5 C4 152.3(18) . 15_544 C7 C5 C8 96.5(12) . . C8 C5 C1 120.3(18) . 15_544 C8 C5 C1 121.0(18) . . C8 C5 C3 79.2(14) . 15_544 C8 C5 C4 92.4(15) . 15_544 C4 C6 C1 58(3) 15_544 . C5 C7 C5 48.1(11) . 15_544 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Zn1 Zn1 2.8567(16) 3 Zn1 N1 2.023(8) . Zn1 O1 2.080(7) 2 Zn1 O1 2.080(7) . Zn1 O2 1.979(6) 3 Zn1 O2 1.979(6) 4 N1 C11A 1.29(2) 2 N1 C11A 1.29(2) . N1 C11B 1.351(19) . N1 C11B 1.351(19) 2 C9 C9 1.506(18) 7 C9 C10A 1.39(3) 2 C9 C10A 1.39(3) . C9 C10B 1.41(3) . C9 C10B 1.41(3) 2 C10A C11A 1.42(3) . C10B C11B 1.42(3) . O1 C2 1.098(15) . O2 Zn1 1.979(6) 3 O2 C2 1.361(16) . C1 C2 1.527(9) . C1 C3 1.52(3) . C1 C4 1.35(3) 15_544 C1 C5 1.579(17) 15_544 C1 C5 1.67(2) . C1 C6 1.59(3) . C3 C4 1.55(3) . C3 C5 1.80(2) 15_544 C4 C1 1.35(3) 15_544 C4 C5 1.84(3) 15_544 C4 C6 0.70(2) 15_544 C5 C1 1.579(17) 15_544 C5 C3 1.80(2) 15_544 C5 C4 1.84(3) 15_544 C5 C5 1.16(3) 15_544 C5 C7 1.427(13) . C5 C8 1.48(2) . C6 C4 0.70(2) 15_544 C7 C5 1.427(13) 15_544