#------------------------------------------------------------------------------ #$Date: 2014-07-11 17:35:18 +0300 (Fri, 11 Jul 2014) $ #$Revision: 120071 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100974.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_1100974 loop_ _publ_author_name 'Ruili Sang' 'Li Xu' _publ_contact_author_address ; Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian, 350002, China ; _publ_contact_author_email ' xuli65@hotmail.com ' _publ_contact_author_fax ' (86)591-83705045 ' _publ_contact_author_name ' Li Xu' _publ_contact_author_phone ' (86)591-83705045 ' _publ_section_title ; A Series of Single, Double, and Triple Me2biim-Bridged Dinuclear, Trinuclear, and Polymeric Complexes: Syntheses, Crystal Structures, and Luminescent Properties ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3731 _journal_page_last 3737 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C8 H12 Cl4 N4 Zn' _chemical_formula_weight 371.39 _chemical_name_common '[ZnCl4][H2Me2biim]' _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_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 117.899(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 15.816(3) _cell_length_b 8.9899(17) _cell_length_c 11.474(2) _cell_measurement_reflns_used 1202 _cell_measurement_temperature 273(2) _cell_volume 1441.8(5) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 273(2) _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _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 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 2179 _diffrn_reflns_theta_full 25.04 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_theta_min 2.69 _exptl_absorpt_coefficient_mu 2.428 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.6891 _exptl_absorpt_correction_type SADABS _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 744 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.458 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.124 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.633 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 78 _refine_ls_number_reflns 1268 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.633 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0613 _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^)+(0.0460P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1299 _refine_ls_wR_factor_ref 0.1384 _reflns_number_gt 1030 _reflns_number_total 1268 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic048280xsi20041208_095610_1.cif _[local]_cod_data_source_block '[ZnCl4][H2Me2biim]' _cod_database_code 1100974 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 Zn Zn 0.5000 0.35216(10) 0.7500 0.0296(3) Uani 1 2 d S . . Cl1 Cl 0.60069(11) 0.49552(17) 0.92496(15) 0.0443(5) Uani 1 1 d . . . Cl2 Cl 0.41400(11) 0.2104(2) 0.81893(15) 0.0464(5) Uani 1 1 d . . . N1 N 0.4387(3) 0.7449(6) 0.8450(5) 0.0391(12) Uani 1 1 d . . . N2 N 0.3729(3) 0.8743(5) 0.6648(4) 0.0274(10) Uani 1 1 d . . . C1 C 0.4546(3) 0.8119(6) 0.7526(5) 0.0277(12) Uani 1 1 d . . . C2 C 0.3442(4) 0.7631(7) 0.8139(6) 0.0415(15) Uani 1 1 d . . . H2 H 0.3139 0.7269 0.8607 0.050 Uiso 1 1 calc R . . C3 C 0.3039(4) 0.8445(7) 0.7014(6) 0.0378(14) Uani 1 1 d . . . H3 H 0.2404 0.8747 0.6569 0.045 Uiso 1 1 calc R . . C4 C 0.3596(4) 0.9653(7) 0.5505(6) 0.0424(16) Uani 1 1 d . . . H4C H 0.4184 0.9689 0.5455 0.064 Uiso 1 1 calc R . . H4B H 0.3411 1.0643 0.5605 0.064 Uiso 1 1 calc R . . H4A H 0.3105 0.9219 0.4712 0.064 Uiso 1 1 calc R . . 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 Zn 0.0271(5) 0.0347(6) 0.0276(5) 0.000 0.0133(4) 0.000 Cl1 0.0374(8) 0.0436(9) 0.0342(8) -0.0039(7) 0.0022(7) -0.0003(7) Cl2 0.0499(10) 0.0539(11) 0.0501(10) -0.0022(8) 0.0356(8) -0.0091(8) N1 0.033(3) 0.046(3) 0.039(3) 0.006(2) 0.018(2) 0.000(2) N2 0.026(2) 0.030(3) 0.028(2) 0.001(2) 0.013(2) 0.0006(19) C1 0.017(3) 0.029(3) 0.032(3) -0.001(2) 0.008(2) -0.005(2) C2 0.034(3) 0.045(4) 0.047(4) 0.005(3) 0.020(3) 0.000(3) C3 0.027(3) 0.048(4) 0.038(3) 0.000(3) 0.016(3) -0.001(3) C4 0.039(3) 0.054(4) 0.040(3) 0.013(3) 0.024(3) 0.008(3) 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' Cl Cl 0.1484 0.1585 '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 _geom_angle_publ_flag Cl2 Zn Cl2 111.35(10) 2_656 . ? Cl2 Zn Cl1 109.81(6) 2_656 . ? Cl2 Zn Cl1 107.24(6) . . ? Cl2 Zn Cl1 107.24(6) 2_656 2_656 ? Cl2 Zn Cl1 109.81(6) . 2_656 ? Cl1 Zn Cl1 111.43(9) . 2_656 ? C1 N1 C2 109.0(5) . . ? C1 N2 C3 108.5(5) . . ? C1 N2 C4 126.1(5) . . ? C3 N2 C4 125.4(5) . . ? N2 C1 N1 108.1(4) . . ? N2 C1 C1 126.3(6) . 2_656 ? N1 C1 C1 125.6(5) . 2_656 ? C3 C2 N1 106.3(5) . . ? C2 C3 N2 108.1(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 Zn Cl2 2.2597(16) 2_656 ? Zn Cl2 2.2597(16) . ? Zn Cl1 2.2881(16) . ? Zn Cl1 2.2881(15) 2_656 ? N1 C1 1.342(7) . ? N1 C2 1.374(8) . ? N2 C1 1.335(7) . ? N2 C3 1.367(7) . ? N2 C4 1.475(7) . ? C1 C1 1.463(10) 2_656 ? C2 C3 1.355(8) . ? _journal_paper_doi 10.1021/ic048280x