Bis[bis(triphenylphosphoranylidene)ammonium] μ-tetrathiaoxalato-bis[(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(II)]
Geiser, Urs; Mercuri, Maria Laura; Parakka, James P.; Acta Crystallographica Section C 55 (1999) 1253–1255; doi:10.1107/S0108270199004692

data_2008780
_publ_section_title
;
 Bis[bis(triphenylphosphoranylidene)ammonium]
 \m-tetrathiaoxalato-bis[(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(II)]
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1253
_journal_page_last               1255
_journal_paper_doi               10.1107/S0108270199004692
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '(C36 H30 N P2)2 [Ni2 (C2 S4) (C3 S5)2]'
_chemical_formula_moiety         '(((C6 H5)3 P)2 N)2 (((C3 S5) Ni)2 (C2 S4))'
_chemical_formula_sum            'C80 H60 N2 Ni2 P4 S14'
_chemical_formula_weight         1739.44
_chemical_melting_point          264.0(10)
_chemical_name_systematic
;
Bis [bis(triphenylphosphoranylidene)ammonium]
\m-tetrathiaoxalato-bis[(1,3-dithiol-2-thione-4,5-dithiolato)nickelate(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'
_cell_angle_alpha                75.1700(10)
_cell_angle_beta                 82.0670(10)
_cell_angle_gamma                83.3580(10)
_cell_formula_units_Z            1
_cell_length_a                   9.6507(2)
_cell_length_b                   14.2770(3)
_cell_length_c                   15.0369(4)
_cell_measurement_reflns_used    5332
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.00
_cell_volume                     1976.65(8)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.857
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       'area-detector \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  0.034
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12762
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  690
_diffrn_standards_number         167
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Sheldrick, 1997)'
_exptl_crystal_colour            'dark red--brown'
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'elongated plate'
_exptl_crystal_F_000             894
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         8379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.095
_refine_ls_R_factor_gt           0.059
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0179P)^2^+3.5853P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.122
_reflns_number_gt                6033
_reflns_number_total             8379
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fr1185.cif
_cod_data_source_block           fr1185
_cod_original_formula_sum        'C80 H60 N2  Ni2 P4 S14'
_cod_database_code               2008780