Divalent complexes of 3-hydroxy-4-methyl-2(3H)-thiazolethione with Co–Zn: synthesis, X-ray crystal structures and the structure-directing influence of C–H⋯S interactions
Bond, Andrew D.; Jones, William; Journal of the Chemical Society, Dalton Transactions  (2001) 3045–3051; doi:10.1039/b104203n

data_7010828
_publ_section_title
;
 Divalent complexes of 3-hydroxy-4-methyl-2(3H)-thiazolethione with Co--Zn:
 synthesis, X-ray crystal structures and the structure-directing influence
 of C--H&#x22EF;S interactions
;
_journal_coden_ASTM              JCSDAA
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3045
_journal_page_last               3051
_journal_paper_doi               10.1039/b104203n
_journal_year                    2001
_chemical_formula_moiety         'Ni3,6(C4 H4 N1 O1 S2)'
_chemical_formula_sum            'C24 H24 N6 Ni3 O6 S12'
_chemical_formula_weight         1053.34
_chemical_name_common            Ni(MTT)2
_chemical_name_systematic
; 
bis(3-hydroxy-4-methyl-2(3H)-thiazolethiolato-S,O)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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 plus manual editing'
_cell_angle_alpha                92.71(6)
_cell_angle_beta                 114.00(4)
_cell_angle_gamma                112.92(5)
_cell_formula_units_Z            1
_cell_length_a                   10.067(5)
_cell_length_b                   10.167(8)
_cell_length_c                   11.184(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      12.5
_cell_volume                     934.0(11)
_computing_cell_refinement       'MSC/AFC Diffractomer Control (1998)'
_computing_data_collection       'MSC/AFC Diffractomer Control (1998)'
_computing_data_reduction        'TeXsan (MSC, 1995)'
_computing_molecular_graphics    'XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku AFC7R 4-circle diffractometer'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_sigmaI/netI    0.1080
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4505
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.216
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North, Phillips and Mathews (1968)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             534
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1317
_reflns_number_gt                2796
_reflns_number_total             4266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104203n.txt
_cod_data_source_block           5
_cod_original_cell_volume        933.9(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7010828