#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/21/2202124.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2202124 loop_ _publ_author_name 'Sheng-Li Li' 'Anwar Usman' 'Ibrahim A. Razak' 'Azhar A. Rahman' 'Hoong-Kun Fun' 'Jie-Ying Wu' 'Yu-Peng Tian' 'Min-Hua Jiang' 'Zu-Yao Chen' _publ_section_title ; Bis(thiosemicarbazido-\k^2^N,S)nickel(II)--succinate--succinic acid (1/1/1) ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m199 _journal_page_last m201 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Ni (C1 H5 N3 S1)2] (C4 H4 O4), C4 H6 O4' _chemical_formula_moiety 'C2 H10 N6 Ni S2 2+, C4 H4 O4 2-, C4 H6 O4' _chemical_formula_sum 'C10 H20 N6 Ni O8 S2' _chemical_formula_weight 475.15 _chemical_name_systematic ; Bis(thiosemicarbazido-\k^2^N,S)nickel(II)--succinate--succinic acid (1/1/1) ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _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 102.6880(10) _cell_angle_beta 107.0560(10) _cell_angle_gamma 98.9260(10) _cell_formula_units_Z 1 _cell_length_a 6.3886(3) _cell_length_b 8.4876(3) _cell_length_c 8.9485(3) _cell_measurement_reflns_used 2847 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.53 _cell_measurement_theta_min 2.48 _cell_volume 439.83(3) _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_collection 'SMART (Siemens, 1996)' _computing_data_reduction SAINT _computing_molecular_graphics SHELXTL _computing_publication_material ; SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 2003) ; _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 8.33 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measurement_device_type 'Siemens SMART CCD area-detector' _diffrn_measurement_method \w _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 0.0640 _diffrn_reflns_av_sigmaI/netI 0.1047 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 2494 _diffrn_reflns_theta_full 24.99 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_min 2.48 _diffrn_standards_decay_% negligible _diffrn_standards_interval_count none _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.396 _exptl_absorpt_correction_T_max 0.658 _exptl_absorpt_correction_T_min 0.525 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 246 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.792 _refine_diff_density_min -1.737 _refine_ls_extinction_coef 0.055(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXTL _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 148 _refine_ls_number_reflns 1521 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.010 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_gt 0.0652 _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^)+(0.1198P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1676 _refine_ls_wR_factor_ref 0.1737 _reflns_number_gt 1350 _reflns_number_total 1521 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ob6227.cif _[local]_cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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 The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2202124 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Ni1 0.5000 0.0000 0.5000 0.0133(4) Uani d S 1 . . Ni S1 0.22033(16) 0.04027(14) 0.31535(12) 0.0229(4) Uani d . 1 . . S N1 0.6822(5) 0.0406(4) 0.3709(4) 0.0160(7) Uani d D 1 . . N N2 0.5869(6) 0.1083(4) 0.2407(4) 0.0188(8) Uani d D 1 . . N N3 0.2731(7) 0.1672(5) 0.0804(4) 0.0236(9) Uani d . 1 . . N C1 0.3721(6) 0.1104(5) 0.2029(5) 0.0154(8) Uani d . 1 . . C H1A 0.810(4) 0.101(6) 0.430(5) 0.039(15) Uiso d D 1 . . H H1B 0.711(7) -0.050(3) 0.333(5) 0.016(11) Uiso d D 1 . . H H2A 0.667(7) 0.122(6) 0.183(5) 0.035(14) Uiso d D 1 . . H H3A 0.339(11) 0.197(8) 0.013(8) 0.055(18) Uiso d . 1 . . H H3B 0.157(10) 0.197(7) 0.077(7) 0.044(17) Uiso d . 1 . . H O1 1.4048(6) 0.4552(4) 0.7096(4) 0.0418(10) Uani d D 1 . . O O2 1.0943(5) 0.2523(3) 0.6148(3) 0.0240(7) Uani d . 1 . . O C2 1.1066(7) 0.4751(5) 0.4895(5) 0.0233(10) Uani d . 1 . . C H2B 1.0707 0.4050 0.3797 0.028 Uiso calc R 1 . . H H2C 1.2191 0.5740 0.5055 0.028 Uiso calc R 1 . . H C3 1.2001(7) 0.3833(5) 0.6102(5) 0.0189(9) Uani d . 1 . . C H1O 1.457(10) 0.398(6) 0.778(6) 0.050 Uiso d D 1 . . H O3 0.8412(5) 0.2489(4) 0.0805(4) 0.0231(7) Uani d . 1 . . O O4 0.5431(5) 0.2944(4) -0.0915(4) 0.0246(8) Uani d . 1 . . O C4 0.9086(7) 0.4377(5) -0.0716(5) 0.0272(10) Uani d . 1 . . C H4A 0.9778 0.3732 -0.1387 0.033 Uiso calc R 1 . . H H4B 0.8194 0.4967 -0.1371 0.033 Uiso calc R 1 . . H C5 0.7538(7) 0.3200(5) -0.0231(4) 0.0161(8) Uani d . 1 . . C loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni1 0.0109(5) 0.0200(5) 0.0119(5) 0.0039(3) 0.0041(3) 0.0094(3) S1 0.0143(6) 0.0424(8) 0.0204(6) 0.0096(5) 0.0074(5) 0.0212(5) N1 0.0131(17) 0.0196(18) 0.0194(18) 0.0080(14) 0.0045(14) 0.0121(15) N2 0.0184(18) 0.0276(19) 0.0158(17) 0.0027(14) 0.0068(14) 0.0173(15) N3 0.0200(19) 0.033(2) 0.0219(19) 0.0071(16) 0.0062(16) 0.0173(16) C1 0.0146(19) 0.0166(19) 0.0134(18) 0.0023(15) 0.0028(15) 0.0043(15) O1 0.0278(18) 0.0397(19) 0.043(2) -0.0096(15) -0.0138(15) 0.0291(17) O2 0.0209(15) 0.0277(16) 0.0220(15) 0.0014(12) 0.0037(12) 0.0121(13) C2 0.023(2) 0.029(2) 0.020(2) 0.0092(18) 0.0054(17) 0.0138(18) C3 0.0181(19) 0.023(2) 0.0148(19) 0.0049(16) 0.0043(16) 0.0066(17) O3 0.0199(16) 0.0302(16) 0.0247(16) 0.0051(13) 0.0061(13) 0.0210(13) O4 0.0162(16) 0.0318(17) 0.0290(18) 0.0033(13) 0.0045(14) 0.0210(14) C4 0.027(2) 0.033(2) 0.018(2) -0.0066(19) 0.0037(18) 0.0158(19) C5 0.0187(19) 0.0171(18) 0.0116(18) 0.0013(15) 0.0043(15) 0.0052(15) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 N1 . 1.910(3) yes Ni1 N1 2_656 1.910(3) ? Ni1 S1 . 2.1784(9) yes Ni1 S1 2_656 2.1784(9) ? S1 C1 . 1.722(4) yes N1 N2 . 1.430(4) y N1 H1A . 0.84(4) ? N1 H1B . 0.84(4) ? N2 C1 . 1.318(5) y N2 H2A . 0.84(5) ? N3 C1 . 1.325(5) y N3 H3A . 0.88(7) ? N3 H3B . 0.82(6) ? O1 C3 . 1.306(5) yes O1 H1O . 0.88(5) ? O2 C3 . 1.223(5) yes C2 C3 . 1.506(5) ? C2 C2 2_766 1.536(9) ? C2 H2B . 0.9700 ? C2 H2C . 0.9700 ? O3 C5 . 1.257(5) yes O4 C5 . 1.266(5) yes C4 C4 2_765 1.506(8) ? C4 C5 . 1.517(5) ? C4 H4A . 0.9700 ? C4 H4B . 0.9700 ? 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 Ni1 N1 . 2_656 180.0000(10) ? N1 Ni1 S1 . . 87.92(10) yes N1 Ni1 S1 2_656 . 92.08(10) yes N1 Ni1 S1 . 2_656 92.08(10) ? N1 Ni1 S1 2_656 2_656 87.92(10) ? S1 Ni1 S1 . 2_656 180.0 ? C1 S1 Ni1 . . 97.37(13) ? N2 N1 Ni1 . . 115.8(2) ? N2 N1 H1A . . 110(4) ? Ni1 N1 H1A . . 111(4) ? N2 N1 H1B . . 109(3) ? Ni1 N1 H1B . . 107(3) ? H1A N1 H1B . . 103(5) ? C1 N2 N1 . . 117.9(3) ? C1 N2 H2A . . 126(4) ? N1 N2 H2A . . 115(4) ? C1 N3 H3A . . 124(4) ? C1 N3 H3B . . 119(4) ? H3A N3 H3B . . 116(6) ? N2 C1 N3 . . 120.6(4) ? N2 C1 S1 . . 119.5(3) ? N3 C1 S1 . . 119.9(3) ? C3 O1 H1O . . 113(4) ? C3 C2 C2 . 2_766 110.6(4) ? C3 C2 H2B . . 109.5 ? C2 C2 H2B 2_766 . 109.5 ? C3 C2 H2C . . 109.5 ? C2 C2 H2C 2_766 . 109.5 ? H2B C2 H2C . . 108.1 ? O2 C3 O1 . . 122.8(4) ? O2 C3 C2 . . 123.1(4) ? O1 C3 C2 . . 114.2(4) ? C4 C4 C5 2_765 . 113.4(4) ? C4 C4 H4A 2_765 . 108.9 ? C5 C4 H4A . . 108.9 ? C4 C4 H4B 2_765 . 108.9 ? C5 C4 H4B . . 108.9 ? H4A C4 H4B . . 107.7 ? O3 C5 O4 . . 123.0(4) ? O3 C5 C4 . . 118.4(4) ? O4 C5 C4 . . 118.7(3) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1A O2 1_555 0.84(4) 2.06(4) 2.892(4) 168(4) yes N1 H1B O2 2_756 0.84(4) 2.32(4) 3.061(4) 147(4) yes N1 H1B O4 2_655 0.84(4) 2.56(4) 3.147(5) 128(4) yes O1 H1O O4 1_656 0.88(5) 1.63(5) 2.516(5) 177(6) yes N2 H2A O3 1_555 0.84(5) 1.98(5) 2.763(5) 156(5) yes N3 H3A O4 1_555 0.89(7) 1.99(7) 2.866(5) 167(6) yes N3 H3B O3 1_455 0.81(7) 2.14(7) 2.948(6) 173(6) yes C2 H2B O3 1_555 0.97 2.57 3.496(5) 159 yes C4 H4A O2 1_554 0.97 2.58 3.514(5) 161 yes C4 H4B O1 1_454 0.97 2.53 3.285(6) 135 yes 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_site_symmetry_1 _geom_torsion N1 Ni1 S1 C1 . -8.69(16) N1 Ni1 S1 C1 2_656 171.31(16) S1 Ni1 N1 N2 . 11.9(3) S1 Ni1 N1 N2 2_656 -168.1(3) Ni1 N1 N2 C1 . -11.3(5) N1 N2 C1 N3 . -178.1(3) N1 N2 C1 S1 . 2.5(5) Ni1 S1 C1 N2 . 5.7(3) Ni1 S1 C1 N3 . -173.7(3) C2 C2 C3 O2 2_766 60.6(6) C2 C2 C3 O1 2_766 -119.7(5) C4 C4 C5 O3 2_765 -49.0(7) C4 C4 C5 O4 2_765 132.8(5)