#------------------------------------------------------------------------------ #$Date: 2011-01-03 14:48:23 +0200 (Mon, 03 Jan 2011) $ #$Revision: 5312 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100775.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_1100775 loop_ _publ_author_name 'Qiong Ye' 'Yong-Hua Li' 'Yu-Mei Song' 'Xue-Feng Huang' 'Ren-Gen Xiong' 'Ziling Xue' _publ_section_title ; A Second-Order Nonlinear Optical Material Prepared through In Situ Hydrothermal Ligand Synthesis ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3618 _journal_page_last 3625 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C12 H10 Cl0 N12 Zn' _chemical_formula_weight 387.69 _chemical_name_systematic ; ? ; _space_group_IT_number 122 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'I -4 2bw' _symmetry_space_group_name_H-M 'I -4 2 d' _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 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.4850(16) _cell_length_b 10.4850(16) _cell_length_c 13.088(3) _cell_measurement_temperature 293(2) _cell_volume 1438.8(5) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega 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 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 4184 _diffrn_reflns_theta_full 28.18 _diffrn_reflns_theta_max 28.18 _diffrn_reflns_theta_min 2.49 _exptl_absorpt_coefficient_mu 1.735 _exptl_absorpt_correction_type none _exptl_crystal_density_diffrn 1.790 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _refine_diff_density_max 0.832 _refine_diff_density_min -0.587 _refine_diff_density_rms 0.107 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 67 _refine_ls_number_reflns 878 _refine_ls_number_restraints 45 _refine_ls_restrained_S_all 1.179 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0449 _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^)+(0.0709P)^2^+1.8741P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1179 _refine_ls_wR_factor_ref 0.1196 _reflns_number_gt 809 _reflns_number_total 878 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic0500098si20050104_032035_2.cif _[local]_cod_data_source_block 2 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 1438.9(4) _cod_database_code 1100775 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' '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, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' 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 0.5000 0.5000 0.0000 0.01824(12) Uani 1 4 d S . . N1 N 0.4725(2) 0.3428(2) 0.08684(18) 0.0226(6) Uani 1 1 d . . . N2 N 0.3500(2) 0.3041(2) 0.1031(2) 0.0262(6) Uani 1 1 d . . . C1 C 0.5481(4) 0.2500 0.1250 0.0227(9) Uani 1 2 d S . . C2 C 0.6864(4) 0.2500 0.1250 0.0281(10) Uani 1 2 d SDU . . C3 C 0.7521(3) 0.1363(4) 0.1133(3) 0.0494(9) Uani 1 1 d DU . . H3A H 0.7001 0.0616 0.1051 0.059 Uiso 1 1 d R . . C4 C 0.8807(4) 0.1313(5) 0.1130(4) 0.0815(12) Uani 0.50 1 d PDU . . H4A H 0.9174 0.0489 0.1006 0.098 Uiso 0.50 1 d PR . . N3 N 0.8807(4) 0.1313(5) 0.1130(4) 0.0815(12) Uani 0.50 1 d PU . . C5 C 0.9437(6) 0.2417(9) 0.1317(13) 0.0781(17) Uani 0.50 1 d PDU . . N4 N 1.0692(5) 0.1792(7) 0.1233(6) 0.0514(17) Uani 0.50 1 d PU . . H4B H 1.0954 0.0987 0.1119 0.062 Uiso 0.50 1 d PR . . H4C H 1.1269 0.2414 0.1338 0.062 Uiso 0.50 1 d PR . . 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 0.01614(14) 0.01614(14) 0.0224(2) 0.000 0.000 0.000 N1 0.0222(15) 0.0200(10) 0.0255(10) 0.0051(9) 0.0014(8) -0.0009(8) N2 0.0189(11) 0.0288(12) 0.0309(13) 0.0074(10) 0.0017(10) 0.0051(10) C1 0.0177(15) 0.034(2) 0.0170(16) -0.0006(18) 0.000 0.000 C2 0.0186(17) 0.039(2) 0.0269(18) 0.0133(19) 0.000 0.000 C3 0.0372(15) 0.070(2) 0.0413(17) 0.0121(17) 0.0092(16) 0.0259(17) C4 0.0592(18) 0.132(3) 0.053(2) 0.012(2) 0.0123(18) 0.048(2) N3 0.0592(18) 0.132(3) 0.053(2) 0.012(2) 0.0123(18) 0.048(2) C5 0.038(2) 0.151(4) 0.045(3) -0.002(3) 0.012(4) 0.031(4) N4 0.013(2) 0.087(4) 0.054(3) -0.018(4) 0.000(3) 0.028(2) 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' Cl Cl 0.1484 0.1585 '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 N1 Zn1 N1 108.40(7) 2_665 4_655 ? N1 Zn1 N1 108.40(7) 2_665 3_565 ? N1 Zn1 N1 111.64(14) 4_655 3_565 ? N1 Zn1 N1 111.64(14) 2_665 . ? N1 Zn1 N1 108.40(7) 4_655 . ? N1 Zn1 N1 108.40(7) 3_565 . ? C1 N1 N2 106.3(2) . . ? C1 N1 Zn1 135.29(19) . . ? N2 N1 Zn1 117.69(18) . . ? N2 N2 N1 109.64(15) 14_454 . ? N1 C1 N1 108.1(3) 14_454 . ? N1 C1 C2 125.95(16) 14_454 . ? N1 C1 C2 125.95(16) . . ? C3 C2 C3 120.4(4) 14_454 . ? C3 C2 C1 119.8(2) 14_454 . ? C3 C2 C1 119.8(2) . . ? C4 C3 C2 122.0(4) . . ? C4 C3 H3A 122.4 . . ? C2 C3 H3A 115.6 . . ? C3 C4 C5 117.0(5) . . ? C3 C4 C5 114.1(5) . 14_454 ? C5 C4 C5 8.4(13) . 14_454 ? C3 C4 H4A 115.8 . . ? C5 C4 H4A 127.2 . . ? C5 C4 H4A 129.5 14_454 . ? C5 C5 C4 118(5) 14_454 . ? C5 C5 N4 105(3) 14_454 . ? C4 C5 N4 92.4(6) . . ? C5 C5 C4 53(4) 14_454 14_454 ? C4 C5 C4 123.8(6) . 14_454 ? N4 C5 C4 142.9(7) . 14_454 ? C5 C5 N3 53(4) 14_454 14_454 ? C4 C5 N3 123.8(6) . 14_454 ? N4 C5 N3 142.9(7) . 14_454 ? C4 C5 N3 0.0(5) 14_454 14_454 ? C5 C5 N4 66(2) 14_454 14_454 ? C4 C5 N4 149.3(8) . 14_454 ? N4 C5 N4 58.6(6) . 14_454 ? C4 C5 N4 84.3(5) 14_454 14_454 ? N3 C5 N4 84.3(5) 14_454 14_454 ? C5 N4 N4 63.5(4) . 14_454 ? C5 N4 C5 8.8(11) . 14_454 ? N4 N4 C5 57.9(4) 14_454 14_454 ? C5 N4 H4B 134.6 . . ? N4 N4 H4B 160.4 14_454 . ? C5 N4 H4B 138.6 14_454 . ? C5 N4 H4C 105.4 . . ? N4 N4 H4C 43.2 14_454 . ? C5 N4 H4C 100.8 14_454 . ? H4B N4 H4C 120.0 . . ? 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 N1 2.023(2) 2_665 ? Zn1 N1 2.023(2) 4_655 ? Zn1 N1 2.023(2) 3_565 ? Zn1 N1 2.023(2) . ? N1 C1 1.351(3) . ? N1 N2 1.363(3) . ? N2 N2 1.271(5) 14_454 ? C1 N1 1.351(3) 14_454 ? C1 C2 1.450(6) . ? C2 C3 1.386(4) 14_454 ? C2 C3 1.386(4) . ? C3 C4 1.350(5) . ? C3 H3A 0.9600 . ? C4 C5 1.355(8) . ? C4 C5 1.488(11) 14_454 ? C4 H4A 0.9600 . ? C5 C5 0.25(3) 14_454 ? C5 N4 1.474(9) . ? C5 C4 1.488(11) 14_454 ? C5 N3 1.488(11) 14_454 ? C5 N4 1.557(9) 14_454 ? N4 N4 1.485(16) 14_454 ? N4 C5 1.557(9) 14_454 ? N4 H4B 0.9000 . ? N4 H4C 0.9000 . ?