#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/53/2005342.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_2005342 loop_ _publ_author_name 'Tian, Y.-P.' 'Duan, C.-Y.' 'Lu, Z.-L.' 'You, X.-Z.' 'Fun, H.-K.' 'Sivakumar, K.' _publ_section_title ; Bis[methyl N^{\b^}-(4-dimethylaminophenylmethylene)dithiocarbazato]nickel(II) ; _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 2150 _journal_page_last 2153 _journal_paper_doi 10.1107/S010827019600385X _journal_volume 52 _journal_year 1996 _chemical_formula_iupac '[Ni (C11 H14 N3 S2)2]' _chemical_formula_sum 'C22 H28 N6 Ni S4' _chemical_formula_weight 563.45 _chemical_name_systematic ; Bis[S-Methyl-\b-N-(4-dimethylaminophenyl)methylenedithiocarbazido]- nickel(II). ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method SHELXL _cell_angle_alpha 94.09(1) _cell_angle_beta 90.114(6) _cell_angle_gamma 105.871(6) _cell_formula_units_Z 2 _cell_length_a 5.7712(3) _cell_length_b 10.513(1) _cell_length_c 21.633(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 8 _cell_volume 1258.97(18) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Siemens, 1994)' _computing_data_reduction XSCANS _computing_molecular_graphics 'SHELXTL/PC. Molecular geometry: PARST (Nardelli, 1983)' _computing_publication_material SHELXL93 _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXTL/PC (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Siemens P4 diffractometer' _diffrn_measurement_method '\q/2\q 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 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 5837 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 1.89 _diffrn_standards_decay_% <3 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.126 _exptl_absorpt_correction_type none _exptl_crystal_colour Black _exptl_crystal_density_diffrn 1.486 _exptl_crystal_description Prism _exptl_crystal_F_000 588 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.407 _refine_diff_density_min -0.572 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 0.938 _refine_ls_goodness_of_fit_obs 1.032 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 413 _refine_ls_number_reflns 4419 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.938 _refine_ls_restrained_S_obs 1.032 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_obs 0.0388 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0614P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1002 _refine_ls_wR_factor_obs 0.0944 _reflns_number_observed 3337 _reflns_number_total 4419 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file cf1065.cif _[local]_cod_data_source_block tnl5 _[local]_cod_cif_authors_sg_H-M P-1 _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. '_exptl_absorpt_correction_type' value 'None' changed to 'none' 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 The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0614P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0614P)^2^] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 1259.0(2) _cod_database_code 2005342 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 0.0650(4) 0.0413(3) 0.0277(3) 0.0128(3) -0.0035(2) 0.0035(2) S1a 0.1241(9) 0.0728(6) 0.0327(4) 0.0539(6) 0.0025(5) 0.0093(4) S2a 0.0814(6) 0.0691(5) 0.0458(5) 0.0358(5) 0.0009(4) 0.0059(4) N1a 0.060(2) 0.0542(14) 0.0325(12) 0.0179(13) -0.0008(11) 0.0058(11) N2a 0.063(2) 0.0436(13) 0.0316(12) 0.0129(12) -0.0034(11) 0.0036(10) N3a 0.076(2) 0.066(2) 0.0291(12) 0.0361(14) -0.0011(12) 0.0050(11) C1a 0.061(2) 0.045(2) 0.0333(15) 0.0095(14) -0.0021(13) 0.0031(12) C2a 0.061(2) 0.048(2) 0.0341(15) 0.017(2) -0.0043(14) 0.0003(13) C3a 0.059(2) 0.045(2) 0.0303(14) 0.0132(14) -0.0049(13) 0.0012(12) C4a 0.072(2) 0.055(2) 0.035(2) 0.030(2) 0.0011(15) -0.0021(13) C5a 0.069(2) 0.058(2) 0.040(2) 0.034(2) -0.0032(15) 0.0030(14) C6a 0.051(2) 0.044(2) 0.0352(15) 0.0140(13) -0.0008(13) 0.0037(12) C7a 0.068(2) 0.068(2) 0.035(2) 0.035(2) 0.005(2) 0.0035(15) C8a 0.066(2) 0.065(2) 0.036(2) 0.032(2) -0.0002(15) 0.0080(14) C9a 0.089(3) 0.096(3) 0.038(2) 0.053(3) 0.001(2) 0.014(2) C10a 0.073(3) 0.073(2) 0.033(2) 0.031(2) 0.004(2) 0.007(2) C11a 0.097(3) 0.058(2) 0.042(2) 0.023(2) 0.011(2) 0.001(2) Ni2 0.0519(3) 0.0380(3) 0.0290(3) 0.0122(2) 0.0018(2) 0.0036(2) S1b 0.0642(5) 0.0627(5) 0.0349(4) -0.0036(4) -0.0033(4) 0.0126(3) S2b 0.0546(5) 0.0626(5) 0.0429(4) 0.0038(4) -0.0020(4) 0.0121(4) N1b 0.0499(14) 0.0460(13) 0.0335(12) 0.0107(11) 0.0011(11) 0.0053(10) N2b 0.0547(15) 0.0381(12) 0.0329(12) 0.0136(11) 0.0034(11) 0.0038(9) N3b 0.058(2) 0.068(2) 0.0337(13) 0.0106(13) 0.0015(12) 0.0136(12) C1b 0.053(2) 0.0405(15) 0.0321(14) 0.0143(13) 0.0001(13) 0.0002(11) C2b 0.049(2) 0.044(2) 0.035(2) 0.0091(14) 0.0009(13) 0.0018(12) C3b 0.048(2) 0.045(2) 0.0301(14) 0.0124(13) 0.0052(12) 0.0046(11) C4b 0.045(2) 0.052(2) 0.039(2) 0.0089(14) -0.0002(13) 0.0023(13) C5b 0.050(2) 0.054(2) 0.041(2) 0.0088(15) 0.0103(15) 0.0090(14) C6b 0.053(2) 0.046(2) 0.0349(15) 0.0183(14) 0.0045(13) 0.0072(12) C7b 0.048(2) 0.068(2) 0.040(2) 0.004(2) -0.0068(15) 0.0116(15) C8b 0.047(2) 0.070(2) 0.039(2) 0.006(2) 0.0069(14) 0.0155(15) C9b 0.064(3) 0.131(4) 0.047(2) 0.023(3) 0.014(2) 0.036(2) C10b 0.076(3) 0.104(4) 0.045(2) 0.013(3) -0.009(2) 0.022(2) C11b 0.075(3) 0.064(2) 0.043(2) 0.015(2) -0.009(2) 0.009(2) loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_type_symbol Ni1 1 0.5000 0.5000 0.0000 0.0450(2) Uani d S Ni S1a 1 0.3287(2) 0.66026(9) 0.00613(4) 0.0709(3) Uani d . S S2a 1 0.1115(2) 0.76503(9) 0.11273(4) 0.0624(2) Uani d . S N1a 1 0.3600(5) 0.5886(2) 0.12095(11) 0.0485(6) Uani d . N N2a 1 0.4964(5) 0.5138(2) 0.08897(11) 0.0463(6) Uani d . N N3a 1 0.7709(5) 0.4256(3) 0.38027(11) 0.0535(7) Uani d . N C1a 1 0.2788(6) 0.6579(3) 0.08464(13) 0.0474(7) Uani d . C C2a 1 0.6188(6) 0.4599(3) 0.12454(14) 0.0475(7) Uani d . C C3a 1 0.6393(6) 0.4563(3) 0.19089(12) 0.0451(7) Uani d . C C4a 1 0.7911(6) 0.3843(3) 0.21127(14) 0.0516(8) Uani d . C C5a 1 0.8340(7) 0.3712(3) 0.27244(14) 0.0526(8) Uani d . C C6a 1 0.7243(5) 0.4329(3) 0.31897(13) 0.0429(7) Uani d . C C7a 1 0.5687(6) 0.5035(3) 0.29920(14) 0.0537(8) Uani d . C C8a 1 0.5248(6) 0.5148(3) 0.23760(14) 0.0526(8) Uani d . C C9a 1 0.9170(9) 0.3442(5) 0.3999(2) 0.0686(12) Uani d . C C10a 1 0.6619(8) 0.4902(4) 0.4281(2) 0.0573(9) Uani d . C C11a 1 0.1228(9) 0.7513(4) 0.1949(2) 0.0654(10) Uani d . C Ni2 1 0.0000 0.0000 0.5000 0.0396(2) Uani d S Ni S1b 1 -0.3322(2) -0.15275(8) 0.51329(4) 0.0576(2) Uani d . S S2b 1 -0.7378(2) -0.26366(8) 0.42787(4) 0.0554(2) Uani d . S N1b 1 -0.3343(4) -0.0945(2) 0.39488(10) 0.0435(6) Uani d . N N2b 1 -0.1012(4) -0.0167(2) 0.41388(10) 0.0417(5) Uani d . N N3b 1 -0.0760(5) 0.0920(3) 0.11335(11) 0.0541(7) Uani d . N C1b 1 -0.4466(5) -0.1584(3) 0.43960(12) 0.0418(6) Uani d . C C2b 1 0.0295(6) 0.0376(3) 0.36920(13) 0.0432(7) Uani d . C C3b 1 -0.0146(5) 0.0405(3) 0.30361(12) 0.0407(6) Uani d . C C4b 1 0.1792(6) 0.1117(3) 0.27022(13) 0.0462(7) Uani d . C C5b 1 0.1627(6) 0.1273(3) 0.20794(14) 0.0490(7) Uani d . C C6b 1 -0.0547(5) 0.0727(3) 0.17443(13) 0.0437(7) Uani d . C C7b 1 -0.2474(6) 0.0001(3) 0.20747(14) 0.0537(8) Uani d . C C8b 1 -0.2301(6) -0.0162(4) 0.26950(15) 0.0537(8) Uani d . C C9b 1 0.1193(9) 0.1718(6) 0.0801(2) 0.0799(14) Uani d . C C10b 1 -0.2877(9) 0.0211(6) 0.0769(2) 0.0764(12) Uani d . C C11b 1 -0.7985(8) -0.2521(4) 0.3474(2) 0.0610(9) Uani d . C H2a 1 0.7197(54) 0.4185(28) 0.1062(13) 0.046(8) Uiso d . H H4a 1 0.8660(63) 0.3442(32) 0.1807(16) 0.068(10) Uiso d . H H5a 1 0.9461(56) 0.3290(30) 0.2808(14) 0.050(9) Uiso d . H H7a 1 0.4900(64) 0.5440(33) 0.3274(16) 0.070(11) Uiso d . H H8a 1 0.4226(65) 0.5663(34) 0.2280(16) 0.070(11) Uiso d . H H9a 1 0.8368(80) 0.2606(44) 0.3915(21) 0.094(17) Uiso d . H H9b 1 0.9205(82) 0.3382(43) 0.4355(22) 0.094(15) Uiso d . H H9C 1 1.0706(95) 0.3593(46) 0.3753(23) 0.124(18) Uiso d . H H10a 1 0.6766(63) 0.5769(37) 0.4202(16) 0.066(11) Uiso d . H H10b 1 0.5067(82) 0.4610(40) 0.4309(20) 0.089(15) Uiso d . H H10C 1 0.7195(80) 0.4727(41) 0.4706(22) 0.106(15) Uiso d . H H11a 1 0.0681(79) 0.6613(46) 0.2033(19) 0.096(14) Uiso d . H H11b 1 0.0723(82) 0.8114(44) 0.2136(20) 0.095(15) Uiso d . H H11C 1 0.3012(105) 0.7672(50) 0.2098(25) 0.135(20) Uiso d . H H2b 1 0.1813(56) 0.0843(28) 0.3798(13) 0.044(8) Uiso d . H H4b 1 0.3364(59) 0.1523(29) 0.2901(14) 0.055(9) Uiso d . H H5b 1 0.2931(57) 0.1699(30) 0.1918(14) 0.049(9) Uiso d . H H7b 1 -0.3834(54) -0.0402(27) 0.1859(13) 0.042(8) Uiso d . H H8b 1 -0.3506(65) -0.0631(35) 0.2859(16) 0.068(11) Uiso d . H H9D 1 0.2233(85) 0.1408(41) 0.0751(21) 0.082(16) Uiso d . H H9E 1 0.0615(78) 0.1924(41) 0.0428(22) 0.101(15) Uiso d . H H9F 1 0.2079(111) 0.2693(59) 0.1094(28) 0.165(24) Uiso d . H H10D 1 -0.2772(70) 0.0570(37) 0.0335(19) 0.088(13) Uiso d . H H10E 1 -0.3068(81) -0.0636(45) 0.0757(21) 0.090(16) Uiso d . H H10F 1 -0.4165(90) 0.0321(46) 0.0955(22) 0.107(18) Uiso d . H H11D 1 -0.7838(63) -0.1736(37) 0.3377(16) 0.062(11) Uiso d . H H11E 1 -0.9682(95) -0.2854(42) 0.3420(21) 0.106(16) Uiso d . H H11F 1 -0.7059(113) -0.2966(60) 0.3250(27) 0.157(25) Uiso d . H 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' 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_3 _geom_angle N2a Ni1 S1a 2_665 94.69(8) N2a Ni1 S1a . 85.31(8) C1a S1a Ni1 . 96.04(11) C1a S2a C11a . 102.2(2) C1a N1a N2a . 111.6(2) C2a N2a N1a . 114.5(2) C2a N2a Ni1 . 124.6(2) N1a N2a Ni1 . 120.9(2) C6a N3a C10a . 121.7(3) C6a N3a C9a . 121.2(3) C10a N3a C9a . 116.9(3) N1a C1a S1a . 124.6(3) N1a C1a S2a . 121.3(2) S1a C1a S2a . 114.1(2) N2a C2a C3a . 133.5(3) C4a C3a C8a . 115.7(3) C4a C3a C2a . 115.8(3) C8a C3a C2a . 128.5(3) C5a C4a C3a . 123.8(3) C4a C5a C6a . 120.2(3) N3a C6a C7a . 122.0(3) N3a C6a C5a . 121.4(3) C7a C6a C5a . 116.6(3) C8a C7a C6a . 122.7(3) C7a C8a C3a . 120.9(3) N2b Ni2 S1b 2_556 94.11(7) N2b Ni2 S1b . 85.89(7) C1b S1b Ni2 . 96.09(10) C1b S2b C11b . 103.0(2) C1b N1b N2b . 111.6(2) C2b N2b N1b . 114.1(2) C2b N2b Ni2 . 125.5(2) N1b N2b Ni2 . 120.4(2) C6b N3b C9b . 122.1(3) C6b N3b C10b . 121.3(3) C9b N3b C10b . 116.2(3) N1b C1b S1b . 125.3(2) N1b C1b S2b . 120.6(2) S1b C1b S2b . 114.0(2) N2b C2b C3b . 133.7(3) C4b C3b C8b . 115.9(3) C4b C3b C2b . 116.0(3) C8b C3b C2b . 128.1(3) C5b C4b C3b . 122.8(3) C4b C5b C6b . 121.0(3) N3b C6b C7b . 122.2(3) N3b C6b C5b . 121.5(3) C7b C6b C5b . 116.3(3) C8b C7b C6b . 122.6(3) C7b C8b C3b . 121.3(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ni1 N2a 1.920(2) Ni1 S1a 2.1710(9) S1a C1a 1.724(3) S2a C1a 1.752(3) S2a C11a 1.795(4) N1a C1a 1.279(4) N1a N2a 1.407(4) N2a C2a 1.300(4) N3a C6a 1.364(4) N3a C10a 1.436(4) N3a C9a 1.438(5) C2a C3a 1.444(4) C3a C4a 1.394(4) C3a C8a 1.405(4) C4a C5a 1.369(4) C5a C6a 1.403(4) C6a C7a 1.396(4) C7a C8a 1.376(4) Ni2 N2b 1.933(2) Ni2 S1b 2.1727(8) S1b C1b 1.715(3) S2b C1b 1.748(3) S2b C11b 1.794(3) N1b C1b 1.290(4) N1b N2b 1.413(3) N2b C2b 1.294(4) N3b C6b 1.361(3) N3b C9b 1.437(5) N3b C10b 1.444(5) C2b C3b 1.445(4) C3b C4b 1.399(4) C3b C8b 1.405(4) C4b C5b 1.375(4) C5b C6b 1.404(4) C6b C7b 1.395(4) C7b C8b 1.372(4)