#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100974.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 _chemical_name_common '[ZnCl4][H2Me2biim]' _chemical_formula_sum 'C8 H12 Cl4 N4 Zn' _chemical_formula_weight 371.39 _space_group_IT_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _[local]_cod_cif_authors_sg_H-M C2/c 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' _symmetry_cell_setting ? 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' _cell_length_a 15.816(3) _cell_length_b 8.9899(17) _cell_length_c 11.474(2) _cell_angle_alpha 90.00 _cell_angle_beta 117.899(3) _cell_angle_gamma 90.00 _cell_volume 1441.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 1202 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 2.428 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.6891 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2179 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 25.04 _reflns_number_total 1268 _reflns_number_gt 1030 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1268 _refine_ls_number_parameters 78 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1384 _refine_ls_wR_factor_gt 0.1299 _refine_ls_goodness_of_fit_ref 1.633 _refine_ls_restrained_S_all 1.633 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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) . ? 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) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.458 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.124 _cod_database_code 1100974