#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/49/2004905.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_2004905 loop_ _publ_author_name 'Shan, B.-Z.' 'Zhang, X.-M.' 'You, X.-Z.' 'Fun, H.-K.' 'Sivakumar, K.' _publ_section_title ; Bis(1,4-dimethylpyridinium) Bis(maleonitriledithiolato)nickelate(II) ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1148 _journal_page_last 1150 _journal_paper_doi 10.1107/S0108270195014429 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac '(C7 H10 N)2 [Ni(C4 N2 S2)2]' _chemical_formula_moiety '(C7 H10 N) + , [Ni(C4 N2 S2)2] 2-' _chemical_formula_sum 'C22 H20 N6 Ni S4' _chemical_formula_weight 555.39 _chemical_name_systematic ; Bis(1-methyl-4-methylpyridinium) bis(maleonitriledithiolate) 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 87.560(10) _cell_angle_beta 64.890(10) _cell_angle_gamma 72.260(10) _cell_formula_units_Z 1 _cell_length_a 8.5340(10) _cell_length_b 8.7650(10) _cell_length_c 9.9750(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 8 _cell_volume 640.23(14) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Siemens, 1994)' _computing_data_reduction XSCANS _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990b)' _computing_publication_material SHELXL93 _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990a)' _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 0.0127 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 3509 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 2.27 _diffrn_standards_decay_% <3 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.106 _exptl_absorpt_correction_type none _exptl_crystal_colour brown-red _exptl_crystal_density_diffrn 1.440 _exptl_crystal_description Prism _exptl_crystal_F_000 286 _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.36 _refine_diff_density_max 0.34 _refine_diff_density_min -0.60 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.077 _refine_ls_goodness_of_fit_obs 1.112 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 191 _refine_ls_number_reflns 2913 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.077 _refine_ls_restrained_S_obs 1.112 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_obs 0.0327 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0677P)^2^+0.0513P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0984 _refine_ls_wR_factor_obs 0.0971 _reflns_number_observed 2678 _reflns_number_total 2913 _reflns_observed_criterion >2sigma(I) _cod_data_source_file mu1222.cif _cod_data_source_block sbz4 _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. '_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (17 times). '_geom_angle_publ_flag' value 'Yes' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (5 times). 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^)+(0.0677P)^2^+0.0513P] 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^)+(0.0677P)^2^+0.0513P] 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 640.23(12) _cod_database_code 2004905 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 Ni 0.0308(2) 0.0381(2) 0.0342(2) -0.00581(12) -0.01169(13) 0.00213(11) S1 0.0380(2) 0.0434(2) 0.0444(2) -0.0050(2) -0.0068(2) 0.0079(2) S2 0.0363(2) 0.0446(2) 0.0468(2) -0.0069(2) -0.0064(2) 0.0074(2) N1 0.0658(12) 0.0451(9) 0.0704(12) -0.0056(8) -0.0230(9) 0.0073(8) N2 0.0457(10) 0.0637(11) 0.0645(11) -0.0040(8) -0.0032(8) -0.0109(9) N3 0.0450(8) 0.0574(9) 0.0450(8) -0.0188(7) -0.0162(7) -0.0021(7) C1 0.0362(8) 0.0412(8) 0.0408(8) -0.0049(6) -0.0165(7) 0.0018(6) C2 0.0334(8) 0.0420(8) 0.0398(8) -0.0044(6) -0.0132(7) -0.0006(6) C3 0.0422(9) 0.0468(9) 0.0450(9) -0.0064(7) -0.0157(7) 0.0032(7) C4 0.0404(9) 0.0482(9) 0.0471(9) -0.0088(7) -0.0142(8) 0.0007(7) C5 0.0542(11) 0.0646(11) 0.0390(9) -0.0222(9) -0.0171(8) -0.0018(8) C6 0.0544(11) 0.0586(11) 0.0450(9) -0.0166(9) -0.0127(9) -0.0054(8) C7 0.0527(11) 0.0542(10) 0.0519(10) -0.0232(8) -0.0194(8) 0.0053(8) C8 0.0671(13) 0.0659(12) 0.0420(9) -0.0268(10) -0.0231(9) 0.0032(8) C9 0.0529(11) 0.0634(11) 0.0416(9) -0.0209(9) -0.0126(8) -0.0063(8) C10 0.0542(13) 0.0752(15) 0.0609(13) -0.0080(11) -0.0238(11) -0.0016(11) C11 0.081(2) 0.0631(14) 0.071(2) -0.0153(12) -0.0318(15) 0.0107(12) 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 Ni 1 1.0000 .0000 .5000 .03644(12) Uani d S Ni S1 1 .97031(6) .23678(5) .41892(5) .04808(14) Uani d . S S2 1 .72190(6) .07596(5) .67155(5) .04832(14) Uani d . S N1 1 .6415(3) .6505(2) .5154(2) .0659(5) Uani d . N N2 1 .3210(3) .4437(2) .8404(2) .0682(5) Uani d . N N3 1 .9320(2) .7717(2) .1689(2) .0494(4) Uani d . N C1 1 .7515(2) .3483(2) .5421(2) .0412(3) Uani d . C C2 1 .6434(2) .2793(2) .6528(2) .0410(3) Uani d . C C3 1 .6897(3) .5163(2) .5272(2) .0477(4) Uani d . C C4 1 .4637(2) .3708(2) .7567(2) .0481(4) Uani d . C C5 1 .8114(3) .8859(3) .2822(2) .0526(4) Uani d . C C6 1 .6943(3) 1.0181(3) .2604(2) .0559(5) Uani d . C C7 1 .6958(3) 1.0387(2) .1214(2) .0526(4) Uani d . C C8 1 .8225(3) .9194(3) .0066(2) .0570(5) Uani d . C C9 1 .9379(3) .7887(3) .0324(2) .0545(5) Uani d . C C10 1 1.0538(4) .6269(4) .1965(3) .0666(6) Uani d . C C11 1 .5653(4) 1.1819(3) .0969(4) .0740(7) Uani d . C H5 1 .817(3) .867(3) .363(3) .061(6) Uiso d . H H6 1 .609(3) 1.099(3) .337(3) .060(6) Uiso d . H H8 1 .833(4) .933(3) -.087(3) .071(7) Uiso d . H H9 1 1.018(4) .700(3) -.035(3) .082(8) Uiso d . H H10A 1 1.161(5) .573(4) .107(4) .111(11) Uiso d . H H10B 1 1.096(5) .657(4) .252(4) .102(11) Uiso d . H H10C 1 1.002(6) .560(5) .220(5) .137(17) Uiso d . H H11A 1 .567(5) 1.173(4) .011(4) .107(12) Uiso d . H H11B 1 .454(6) 1.197(5) .178(5) .139(16) Uiso d . H H11C 1 .579(6) 1.283(5) .120(5) .132(14) 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 _geom_angle_publ_flag S2 Ni S1 92.36(2) yes C1 S1 Ni 102.81(7) yes C2 S2 Ni 103.21(6) yes C9 N3 C5 119.9(2) ? C9 N3 C10 120.4(2) ? C5 N3 C10 119.7(2) ? C2 C1 C3 120.9(2) ? C2 C1 S1 121.06(13) yes C3 C1 S1 117.99(14) ? C1 C2 C4 121.5(2) ? C1 C2 S2 120.39(13) yes C4 C2 S2 118.10(14) ? N1 C3 C1 179.5(2) ? N2 C4 C2 179.5(2) ? N3 C5 C6 120.8(2) ? C5 C6 C7 120.8(2) ? C6 C7 C8 117.1(2) ? C6 C7 C11 121.3(2) ? C8 C7 C11 121.6(2) ? C9 C8 C7 120.5(2) ? N3 C9 C8 120.9(2) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ni S2 2.1659(6) yes Ni S1 2.1762(5) yes S1 C1 1.730(2) yes S2 C2 1.735(2) yes N1 C3 1.140(3) yes N2 C4 1.139(2) yes N3 C9 1.344(3) yes N3 C5 1.349(2) yes N3 C10 1.475(3) yes C1 C2 1.362(3) yes C1 C3 1.430(2) yes C2 C4 1.429(2) yes C5 C6 1.359(3) yes C6 C7 1.385(3) yes C7 C8 1.392(3) yes C7 C11 1.493(3) yes C8 C9 1.360(3) yes