#------------------------------------------------------------------------------ #$Date: 2011-06-22 00:01:30 +0300 (Wed, 22 Jun 2011) $ #$Revision: 21243 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/7052627.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_7052627 loop_ _publ_author_name 'Kostakis, George E.' 'Casella, Luigi' 'Boudalis, Athanassios K.' 'Monzani, Enrico' 'Plakatouras, John C.' _publ_section_title ; Structural variation from 1D chains to 3D networks: a systematic study of coordination number effect on the construction of coordination polymers using the terepthaloylbisglycinate ligand ; _journal_issue 5 _journal_name_full 'New Journal of Chemistry' _journal_page_first 1060 _journal_volume 35 _journal_year 2011 _chemical_compound_source 'synthesis as described' _chemical_formula_moiety 'C12 H16 Cd1 N2 O9, 2(H2 O)' _chemical_formula_sum 'C12 H20 Cd N2 O11' _chemical_formula_weight 480.7 _chemical_name_common 'Compound X' _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_creation_date 2005-02-28T17:09:07-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90.00 _cell_angle_beta 93.8408(14) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 6.9224(2) _cell_length_b 7.9698(2) _cell_length_c 30.1896(8) _cell_measurement_reflns_used 15322 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 27.485 _cell_measurement_theta_min 1 _cell_measurement_wavelength 0.71073 _cell_volume 1661.82(8) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD; rotation images' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_UB_11 -0.11874 _diffrn_orient_matrix_UB_12 0.14927E-2 _diffrn_orient_matrix_UB_13 0.171256E-1 _diffrn_orient_matrix_UB_21 -0.799206E-1 _diffrn_orient_matrix_UB_22 -0.35099E-1 _diffrn_orient_matrix_UB_23 -0.272472E-1 _diffrn_orient_matrix_UB_31 0.218163E-1 _diffrn_orient_matrix_UB_32 -0.120455 _diffrn_orient_matrix_UB_33 0.81517E-2 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_unetI/netI 0.0271 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 7402 _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; _diffrn_reflns_theta_full 27.46 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_min 3.9 _exptl_absorpt_coefficient_mu 1.379 _exptl_absorpt_correction_T_max 0.8216 _exptl_absorpt_correction_T_min 0.7776 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.921 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 968 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.59 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.076 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 159 _refine_ls_number_reflns 1865 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.093 _refine_ls_R_factor_all 0.0246 _refine_ls_R_factor_gt 0.0212 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0160P)^2^+2.8586P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.046 _refine_ls_wR_factor_ref 0.047 _reflns_number_gt 1754 _reflns_number_total 1865 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c0nj01009j.txt _[local]_cod_data_source_block km0405 _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_database_code 7052627 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-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 Cd1 Cd 0.5 0.17901(2) 0.25 0.01335(7) Uani 1 2 d S . . O1 O 0.37740(19) 0.36786(17) 0.20081(4) 0.0153(3) Uani 1 1 d . . . O2 O 0.2693(2) 0.12189(17) 0.17507(5) 0.0188(3) Uani 1 1 d . . . O3 O 0.3736(2) 0.19895(17) 0.07460(5) 0.0174(3) Uani 1 1 d . . . O4 O 0.7642(2) 0.18372(18) 0.20634(5) 0.0142(3) Uani 1 1 d . . . O5 O 0.5 -0.0946(3) 0.25 0.0206(5) Uani 1 2 d S . . O6 O 0.1916(2) -0.1740(2) 0.12444(5) 0.0168(3) Uani 1 1 d . . . N1 N 0.0858(3) 0.2755(2) 0.09943(5) 0.0158(4) Uani 1 1 d . . . C1 C 0.2795(3) 0.2771(2) 0.17236(6) 0.0128(4) Uani 1 1 d . . . C2 C 0.1745(3) 0.3765(3) 0.13490(6) 0.0151(4) Uani 1 1 d . . . C3 C 0.1946(3) 0.1941(2) 0.07117(6) 0.0135(4) Uani 1 1 d . . . C4 C 0.0888(3) 0.0951(2) 0.03470(6) 0.0129(4) Uani 1 1 d . . . C5 C -0.1129(3) 0.0925(3) 0.02751(7) 0.0170(4) Uani 1 1 d . . . C6 C -0.1992(3) -0.0013(3) -0.00695(6) 0.0161(4) Uani 1 1 d . . . H2A H 0.075(3) 0.435(3) 0.1472(7) 0.015(5) Uiso 1 1 d . . . H2B H 0.267(3) 0.456(3) 0.1233(7) 0.017(6) Uiso 1 1 d . . . H5 H -0.189(3) 0.150(3) 0.0457(8) 0.018(6) Uiso 1 1 d . . . H6 H -0.331(4) -0.001(3) -0.0113(8) 0.025(6) Uiso 1 1 d . . . H1W H 0.743(3) 0.218(3) 0.1807(9) 0.020(6) Uiso 1 1 d . . . H2W H 0.812(4) 0.092(4) 0.2027(10) 0.040(8) Uiso 1 1 d . . . H3W H 0.185(4) -0.082(4) 0.1332(10) 0.039(9) Uiso 1 1 d . . . H4W H 0.102(4) -0.203(4) 0.1111(10) 0.037(9) Uiso 1 1 d . . . H5W H 0.576(4) -0.155(3) 0.2644(9) 0.033(8) Uiso 1 1 d . . . H1N H -0.034(4) 0.274(3) 0.0971(8) 0.023(6) 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 Cd1 0.01508(11) 0.01081(11) 0.01395(11) 0 -0.00065(7) 0 O1 0.0160(7) 0.0145(7) 0.0148(6) -0.0017(5) -0.0042(5) 0.0019(5) O2 0.0232(8) 0.0124(7) 0.0204(7) 0.0002(6) -0.0013(6) 0.0000(6) O3 0.0148(7) 0.0194(7) 0.0175(7) -0.0035(6) -0.0022(6) -0.0019(5) O4 0.0165(7) 0.0110(7) 0.0149(7) -0.0010(6) 0.0004(6) 0.0022(6) O5 0.0169(10) 0.0087(10) 0.0347(12) 0 -0.0099(9) 0 O6 0.0166(7) 0.0151(8) 0.0181(7) -0.0016(6) -0.0023(6) 0.0002(6) N1 0.0132(9) 0.0177(9) 0.0159(8) -0.0050(7) -0.0041(7) 0.0006(7) C1 0.0113(9) 0.0157(10) 0.0116(8) -0.0019(7) 0.0026(7) 0.0021(7) C2 0.0155(10) 0.0149(10) 0.0144(9) -0.0030(8) -0.0019(8) 0.0016(8) C3 0.0152(9) 0.0114(9) 0.0136(9) 0.0024(7) -0.0019(7) -0.0004(7) C4 0.0166(9) 0.0096(9) 0.0124(9) 0.0013(7) -0.0014(7) -0.0006(7) C5 0.0181(10) 0.0174(10) 0.0155(9) -0.0036(8) 0.0012(8) 0.0022(8) C6 0.0120(9) 0.0182(10) 0.0177(9) -0.0013(8) -0.0013(8) -0.0002(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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.11 -1 0 0 0.07 0 1 0 0.1 0 -1 0 0.1 0 0 1 0.02 0 0 -1 0.07 1 1 0 0.11 -1 -1 0 0.07 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 O5 Cd1 O1 132.19(4) . 2_655 ? O5 Cd1 O1 132.19(4) . . ? O1 Cd1 O1 95.62(8) 2_655 . ? O5 Cd1 O4 90.92(4) . . ? O1 Cd1 O4 95.02(6) 2_655 . ? O1 Cd1 O4 83.73(6) . . ? O5 Cd1 O4 90.92(4) . 2_655 ? O1 Cd1 O4 83.73(6) 2_655 2_655 ? O1 Cd1 O4 95.02(6) . 2_655 ? O4 Cd1 O4 178.15(7) . 2_655 ? C1 O1 Cd1 102.98(12) . . ? Cd1 O4 H1W 116.2(17) . . ? Cd1 O4 H2W 114(2) . . ? H1W O4 H2W 103(3) . . ? Cd1 O5 H5W 126.1(19) . . ? H3W O6 H4W 114(3) . . ? C3 N1 C2 120.83(18) . . ? C3 N1 H1N 122.7(18) . . ? C2 N1 H1N 116.4(18) . . ? O2 C1 O1 123.25(17) . . ? O2 C1 C2 122.67(17) . . ? O1 C1 C2 114.08(17) . . ? N1 C2 C1 114.73(17) . . ? N1 C2 H2A 106.6(14) . . ? C1 C2 H2A 107.1(14) . . ? N1 C2 H2B 110.6(13) . . ? C1 C2 H2B 108.1(13) . . ? H2A C2 H2B 109.6(19) . . ? O3 C3 N1 122.21(18) . . ? O3 C3 C4 120.88(17) . . ? N1 C3 C4 116.91(17) . . ? C6 C4 C5 118.82(17) 5 . ? C6 C4 C3 117.59(17) 5 . ? C5 C4 C3 123.59(17) . . ? C6 C5 C4 120.08(19) . . ? C6 C5 H5 119.1(15) . . ? C4 C5 H5 120.8(15) . . ? C5 C6 C4 121.10(19) . 5 ? C5 C6 H6 119.1(15) . . ? C4 C6 H6 119.8(15) 5 . ? 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 Cd1 O5 2.181(2) . ? Cd1 O1 2.2411(15) 2_655 ? Cd1 O1 2.2411(15) . ? Cd1 O2 2.719(2) . ? Cd1 O2 2.719(2) 2_655 ? Cd1 O4 2.3249(18) . ? Cd1 O4 2.3249(18) 2_655 ? O1 C1 1.281(2) . ? O2 C1 1.242(3) . ? O3 C3 1.237(3) . ? O4 H1W 0.82(3) . ? O4 H2W 0.81(3) . ? O5 H5W 0.82(3) . ? O6 H3W 0.78(3) . ? O6 H4W 0.75(3) . ? N1 C3 1.342(3) . ? N1 C2 1.443(3) . ? N1 H1N 0.83(3) . ? C1 C2 1.525(3) . ? C2 H2A 0.93(2) . ? C2 H2B 0.98(2) . ? C3 C4 1.504(3) . ? C4 C6 1.389(3) 5 ? C4 C5 1.398(3) . ? C5 C6 1.384(3) . ? C5 H5 0.91(2) . ? C6 C4 1.389(3) 5 ? C6 H6 0.91(2) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H1W O6 0.82(3) 1.92(3) 2.736(2) 172(2) 3 O4 H2W O1 0.81(3) 1.84(3) 2.645(3) 168(3) 3_545 O6 H3W O2 0.78(3) 2.12(3) 2.842(3) 154(3) . O6 H4W O3 0.75(3) 2.02(3) 2.774(2) 175(3) 3_445 O5 H5W O4 0.82(3) 1.88(3) 2.690(2) 173(3) 4_645 N1 H1N O6 0.83(3) 2.16(3) 2.908(3) 150(2) 3_455 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Cd1 O1 C1 7.67(13) . . . . ? O1 Cd1 O1 C1 -172.33(13) 2_655 . . . ? O4 Cd1 O1 C1 93.21(12) . . . . ? O4 Cd1 O1 C1 -88.16(12) 2_655 . . . ? Cd1 O1 C1 O2 -0.8(2) . . . . ? Cd1 O1 C1 C2 178.63(13) . . . . ? C3 N1 C2 C1 -71.0(2) . . . . ? O2 C1 C2 N1 -8.7(3) . . . . ? O1 C1 C2 N1 171.84(16) . . . . ? C2 N1 C3 O3 1.4(3) . . . . ? C2 N1 C3 C4 -178.71(17) . . . . ? O3 C3 C4 C6 4.0(3) . . . 5 ? N1 C3 C4 C6 -175.91(17) . . . 5 ? O3 C3 C4 C5 -176.15(18) . . . . ? N1 C3 C4 C5 3.9(3) . . . . ? C6 C4 C5 C6 -0.5(3) 5 . . . ? C3 C4 C5 C6 179.70(18) . . . . ? C4 C5 C6 C4 0.5(3) . . . 5 ?