Bis[(2-chloro-4-fluorobenzyl)triphenylphosphonium] bis(1,2,5-thiadiazole-3,4-dithiolato)nickelate(II)
Zeng, Zhou-Hua; Yang, Shui-Bin; Acta Crystallographica Section E 68 (2012) m239–m240; doi:10.1107/S1600536812003625

data_2234030
_publ_section_title
;
 Bis[(2-chloro-4-fluorobenzyl)triphenylphosphonium]
 bis(1,2,5-thiadiazole-3,4-dithiolato)nickelate(II)
;
_journal_coeditor_code           WM2587
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m239
_journal_page_last               m240
_journal_paper_doi               10.1107/S1600536812003625
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '(C25 H20 Cl F P)2 [Ni (C2 N2 S3)2]'
_chemical_formula_moiety         '2(C25 H20 Cl F P +), C4 N4 Ni S6 2-'
_chemical_formula_sum            'C54 H40 Cl2 F2 N4 Ni P2 S6'
_chemical_formula_weight         1166.81
_chemical_name_systematic
;
Bis[(2-chloro-4-fluorobenzyl)triphenylphosphonium]
bis(1,2,5-thiadiazole-3,4-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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2000
_cell_angle_alpha                71.4470(10)
_cell_angle_beta                 83.601(2)
_cell_angle_gamma                68.691(2)
_cell_formula_units_Z            1
_cell_length_a                   9.4447(11)
_cell_length_b                   12.1385(15)
_cell_length_c                   13.1309(16)
_cell_measurement_reflns_used    3884
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.32
_cell_volume                     1329.6(3)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\f and \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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9694
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.64
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  0.9162
_exptl_absorpt_correction_T_min  0.8614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2004)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             598
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.388
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0368P)^2^+1.9880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1183
_reflns_number_gt                3807
_reflns_number_total             4652
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2587.cif
_cod_data_source_block           I
_cod_database_code               2234030
_cod_database_fobs_code          2234030