A Convenient Route To Synthesize the Fully Conjugated Bimetallic Complex (Bu4N)2{tto[Ni(dmit)2]} (tto = Tetrathiooxalate, C2S42-, and dmit = 1,3-dithiole-2-thione-4,5-dithiolate, C3S52-) and the Crystal Structure of a New Crystal Form
Jun-Feng Bai; Jing-Lin Zuo; Zhen Shen; Xiao-Zeng You; Hoong-Kun Fun; Kandasamy Chinnakali; Inorganic Chemistry 39 (2000) 1322–1324; doi:10.1021/ic9902875

data_4300011
_publ_section_title
;
A Convenient Route To Synthesize the Fully Conjugated Bimetallic Complex
(Bu4N)2{tto[Ni(dmit)2]} (tto = Tetrathiooxalate, C2S42-, and dmit =
1,3-dithiole-2-thione-4,5-dithiolate, C3S52-) and the Crystal Structure of
a New Crystal Form
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1322
_journal_page_last               1324
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C20 H36 N Ni S7'
_chemical_formula_weight         573.63
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.8125(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9740(2)
_cell_length_b                   15.2622(3)
_cell_length_c                   17.9482(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      1.75
_cell_volume                     2731.89(10)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material
; SHELXTL (Sheldrick, 1997)
  PLATON (Spek, 1990) 
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measurement_device
;
Siemens SMART CCD area detector diffractometer 
;
_diffrn_measurement_method       '\w 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  0.083
_diffrn_reflns_av_sigmaI/netI    0.113
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17252
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    1.254
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_type   'empirical using SADABS(Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.42
_refine_diff_density_min         -0.57
_refine_diff_density_rms         0.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         6513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.129
_refine_ls_R_factor_gt           0.052
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.097
_refine_ls_wR_factor_ref         0.117
_reflns_number_gt                3194
_reflns_number_total             6513
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               4300011
_journal_paper_doi 10.1021/ic9902875