#------------------------------------------------------------------------------ #$Date: 2014-07-12 07:06:18 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/20/60/7206024.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_7206024 loop_ _publ_author_name 'Yang, Ming' 'Jiang, Feilong' 'Chen, Qihui' 'Zhou, Youfu' 'Feng, Rui' 'Xiong, Kecai' 'Hong, Maochun' _publ_section_title ; Solvent and temperature influence structural variation from nonporous 2D \\rightarrow 3D parallel polycatenation to 3D microporous metal--organic framework ; _journal_issue 12 _journal_name_full CrystEngComm _journal_page_first 3971 _journal_volume 13 _journal_year 2011 _chemical_formula_sum 'C13 H9 N2 O6.5 Zn' _chemical_formula_weight 362.59 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 97.510(3) _cell_angle_beta 103.711(5) _cell_angle_gamma 112.582(6) _cell_formula_units_Z 2 _cell_length_a 8.2330(16) _cell_length_b 9.1285(16) _cell_length_c 10.7920(16) _cell_measurement_temperature 293(2) _cell_volume 705.0(2) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _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 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 6044 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 2.49 _exptl_absorpt_coefficient_mu 1.778 _exptl_absorpt_correction_T_max 0.7176 _exptl_absorpt_correction_T_min 0.7176 _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 366 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 1.031 _refine_diff_density_min -0.700 _refine_diff_density_rms 0.102 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 214 _refine_ls_number_reflns 3197 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.088 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0503 _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^)+(0.0792P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1412 _refine_ls_wR_factor_ref 0.1492 _reflns_number_gt 2598 _reflns_number_total 3197 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c1ce05263b.txt _[local]_cod_data_source_block 2 _[local]_cod_chemical_formula_sum_orig 'C13 H9 N2 O6.50 Zn' _cod_database_code 7206024 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -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 _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 1.07382(6) 0.84002(5) -0.00289(4) 0.03365(18) Uani 1 1 d . . . O1 O 0.8890(4) 0.6746(3) 0.0501(3) 0.0377(6) Uani 1 1 d . . . N1 N 1.0404(4) 0.7233(4) -0.1896(3) 0.0336(7) Uani 1 1 d . . . C1 C 0.8754(5) 0.7155(4) 0.1636(4) 0.0337(8) Uani 1 1 d . . . O2 O 0.9805(4) 0.8458(4) 0.2453(3) 0.0590(9) Uani 1 1 d . . . N2 N 0.5317(5) 0.5555(4) 0.4730(3) 0.0429(8) Uani 1 1 d . . . C2 C 0.7214(5) 0.5903(4) 0.1959(3) 0.0270(7) Uani 1 1 d . . . O3 O 0.3883(4) 0.1047(4) -0.0413(3) 0.0451(7) Uani 1 1 d . . . C3 C 0.6091(5) 0.4371(4) 0.1095(3) 0.0273(7) Uani 1 1 d . . . H3 H 0.6294 0.4113 0.0300 0.033 Uiso 1 1 calc R . . O4 O 0.1883(3) 0.0774(3) 0.0700(3) 0.0345(6) Uani 1 1 d . . . C4 C 0.4666(5) 0.3223(4) 0.1416(3) 0.0257(7) Uani 1 1 d . . . O5 O 0.5712(15) 0.7212(9) 0.5082(7) 0.087(3) Uani 0.50 1 d P . . C5 C 0.3425(5) 0.1583(4) 0.0478(3) 0.0291(7) Uani 1 1 d . . . O6 O 1.2960(4) 0.8036(4) 0.1039(3) 0.0455(8) Uani 1 1 d . . . C6 C 0.4379(5) 0.3572(4) 0.2605(3) 0.0308(8) Uani 1 1 d . . . H6 H 0.3432 0.2804 0.2823 0.037 Uiso 1 1 calc R . . O7 O 1.3556(8) 0.9590(7) 0.3672(5) 0.133(2) Uani 1 1 d . . . C7 C 0.5533(5) 0.5095(5) 0.3474(4) 0.0360(9) Uani 1 1 d . . . C8 C 0.6911(5) 0.6274(5) 0.3144(4) 0.0359(9) Uani 1 1 d . . . H8 H 0.7625 0.7306 0.3715 0.043 Uiso 1 1 calc R . . C9 C 1.1231(7) 0.7987(5) -0.2701(4) 0.0589(14) Uani 1 1 d . . . H9 H 1.1925 0.9116 -0.2438 0.071 Uiso 1 1 calc R . . C10 C 1.1098(8) 0.7155(5) -0.3914(4) 0.0621(15) Uani 1 1 d . . . H10 H 1.1714 0.7728 -0.4440 0.075 Uiso 1 1 calc R . . C11 C 1.0056(5) 0.5475(4) -0.4353(3) 0.0330(8) Uani 1 1 d . . . C12 C 0.9146(5) 0.4703(5) -0.3533(4) 0.0362(9) Uani 1 1 d . . . H12 H 0.8390 0.3583 -0.3796 0.043 Uiso 1 1 calc R . . C13 C 0.9366(5) 0.5608(4) -0.2315(4) 0.0338(8) Uani 1 1 d . . . H13 H 0.8768 0.5065 -0.1767 0.041 Uiso 1 1 calc R . . H6A H 1.390(7) 0.842(5) 0.077(4) 0.041 Uiso 1 1 d . . . H6B H 1.324(7) 0.852(6) 0.168(5) 0.041 Uiso 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 Zn1 0.0377(3) 0.0218(2) 0.0297(3) -0.00171(17) 0.0186(2) -0.00129(19) O1 0.0353(14) 0.0334(14) 0.0409(15) 0.0099(12) 0.0216(12) 0.0054(11) N1 0.0355(17) 0.0271(15) 0.0278(14) -0.0037(12) 0.0133(13) 0.0043(13) C1 0.0276(18) 0.0244(17) 0.042(2) 0.0080(15) 0.0126(16) 0.0026(14) O2 0.0509(19) 0.0333(16) 0.0582(19) -0.0058(14) 0.0194(16) -0.0130(14) N2 0.0424(19) 0.0392(19) 0.0299(17) -0.0058(14) 0.0180(14) 0.0007(15) C2 0.0232(16) 0.0264(17) 0.0257(16) 0.0041(13) 0.0086(13) 0.0050(13) O3 0.0372(15) 0.0353(15) 0.0441(15) -0.0124(12) 0.0202(13) -0.0009(12) C3 0.0267(17) 0.0268(17) 0.0240(15) 0.0020(13) 0.0111(13) 0.0066(14) O4 0.0280(13) 0.0228(12) 0.0420(14) -0.0001(11) 0.0172(11) -0.0010(10) C4 0.0217(16) 0.0234(16) 0.0252(15) 0.0021(13) 0.0087(13) 0.0032(13) O5 0.185(9) 0.048(4) 0.051(4) 0.017(3) 0.063(5) 0.057(5) C5 0.0251(17) 0.0230(17) 0.0329(17) 0.0024(14) 0.0110(14) 0.0041(14) O6 0.0394(17) 0.0444(18) 0.0503(18) 0.0075(15) 0.0232(15) 0.0117(14) C6 0.0264(18) 0.0296(18) 0.0278(16) 0.0038(14) 0.0114(14) 0.0026(14) O7 0.139(5) 0.128(5) 0.076(3) 0.017(3) -0.008(3) 0.026(4) C7 0.033(2) 0.038(2) 0.0264(17) -0.0045(15) 0.0135(15) 0.0069(16) C8 0.031(2) 0.0320(19) 0.0319(18) -0.0041(15) 0.0101(15) 0.0049(16) C9 0.076(3) 0.031(2) 0.040(2) -0.0099(18) 0.036(2) -0.011(2) C10 0.083(4) 0.033(2) 0.041(2) -0.0076(18) 0.038(2) -0.011(2) C11 0.0342(19) 0.0305(18) 0.0244(17) -0.0022(14) 0.0076(15) 0.0076(15) C12 0.041(2) 0.0262(18) 0.0325(18) -0.0022(15) 0.0149(16) 0.0060(16) C13 0.040(2) 0.0285(18) 0.0315(18) 0.0019(15) 0.0186(16) 0.0110(16) 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' 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' H H 0.0000 0.0000 '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 _geom_angle_publ_flag O1 Zn1 O4 126.95(12) . 1_665 ? O1 Zn1 N1 103.22(12) . . ? O4 Zn1 N1 125.84(12) 1_665 . ? O1 Zn1 O6 94.73(12) . . ? O4 Zn1 O6 95.38(12) 1_665 . ? N1 Zn1 O6 99.88(13) . . ? C1 O1 Zn1 117.1(2) . . ? C9 N1 C13 117.6(3) . . ? C9 N1 Zn1 123.6(3) . . ? C13 N1 Zn1 118.8(3) . . ? O2 C1 O1 124.6(4) . . ? O2 C1 C2 120.0(4) . . ? O1 C1 C2 115.4(3) . . ? N2 N2 O5 130.1(5) 2_666 . ? N2 N2 C7 117.1(4) 2_666 . ? O5 N2 C7 112.4(4) . . ? C8 C2 C3 119.5(3) . . ? C8 C2 C1 119.3(3) . . ? C3 C2 C1 121.2(3) . . ? C2 C3 C4 120.3(3) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 O4 Zn1 115.5(2) . 1_445 ? C6 C4 C3 120.5(3) . . ? C6 C4 C5 118.9(3) . . ? C3 C4 C5 120.6(3) . . ? O3 C5 O4 123.1(3) . . ? O3 C5 C4 121.2(3) . . ? O4 C5 C4 115.7(3) . . ? Zn1 O6 H6A 112(3) . . ? Zn1 O6 H6B 106(4) . . ? H6A O6 H6B 105(5) . . ? C4 C6 C7 118.7(3) . . ? C4 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? C8 C7 C6 121.3(3) . . ? C8 C7 N2 116.5(3) . . ? C6 C7 N2 122.1(3) . . ? C2 C8 C7 119.5(3) . . ? C2 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? N1 C9 C10 122.5(4) . . ? N1 C9 H9 118.8 . . ? C10 C9 H9 118.8 . . ? C9 C10 C11 120.7(4) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 116.7(3) . . ? C12 C11 C11 121.4(4) . 2_764 ? C10 C11 C11 121.9(4) . 2_764 ? C11 C12 C13 119.7(3) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? N1 C13 C12 122.8(4) . . ? N1 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.948(3) . ? Zn1 O4 1.959(2) 1_665 ? Zn1 N1 2.055(3) . ? Zn1 O6 2.086(3) . ? O1 C1 1.276(5) . ? N1 C9 1.330(5) . ? N1 C13 1.343(5) . ? C1 O2 1.231(4) . ? C1 C2 1.496(5) . ? N2 N2 1.238(7) 2_666 ? N2 O5 1.396(8) . ? N2 C7 1.439(5) . ? C2 C8 1.384(5) . ? C2 C3 1.392(5) . ? O3 C5 1.224(5) . ? C3 C4 1.392(5) . ? C3 H3 0.9300 . ? O4 C5 1.298(4) . ? O4 Zn1 1.959(2) 1_445 ? C4 C6 1.378(5) . ? C4 C5 1.499(5) . ? O6 H6A 0.85(5) . ? O6 H6B 0.70(5) . ? C6 C7 1.392(5) . ? C6 H6 0.9300 . ? C7 C8 1.387(5) . ? C8 H8 0.9300 . ? C9 C10 1.382(6) . ? C9 H9 0.9300 . ? C10 C11 1.385(6) . ? C10 H10 0.9300 . ? C11 C12 1.383(5) . ? C11 C11 1.507(7) 2_764 ? C12 C13 1.390(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? _journal_paper_doi 10.1039/c1ce05263b