Tetrabutylammonium bis[4,4'-dimethyl-2,2'-(3,7-dimethyl-1<i>H</i>-4,2,1-benzothiazasiline-1,1-diyl)dibenzenethiolato]vanadium(III) acetonitrile tetrasolvate
Tsai, Yi-Fang; Hsu, Hua-Fen; Hsu, Kuei-Fang; Wang, Ju-Chun; Acta Crystallographica Section E 66 (2010) m844–; doi:10.1107/S1600536810022014

data_2226455
_publ_section_title
;
 Tetrabutylammonium
 bis[4,4'-dimethyl-2,2'-(3,7-dimethyl-1<i>H</i>-4,2,1-benzothiazasiline-1,1-diyl)dibenzenethiolato]vanadium(III)
 acetonitrile tetrasolvate
;
_journal_coeditor_code           HB5425
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m844
_journal_paper_doi               10.1107/S1600536810022014
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'(C16 H36 N) [V (C23 H21 N1 S3 Si1)2], 4C2 H3 N'
_chemical_formula_moiety
'C16 H36 N +, C46 H42 N2 S6 Si2 V -, 4(C2 H3 N)'
_chemical_formula_sum            'C70 H90 N7 S6 Si2 V'
_chemical_formula_weight         1328.97
_chemical_name_systematic
;
Tetrabutylammonium bis[4,4'-dimethyl-2,2'-(3,7-dimethyl-1<i>H</i>-
4,2,1-benzothiazasiline-1,1-diyl)dibenzenethiolato]vanadium(III)
acetonitrile tetrasolvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 126.3590(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.0867(16)
_cell_length_b                   14.6525(9)
_cell_length_c                   22.0590(13)
_cell_measurement_reflns_used    5232
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.14
_cell_measurement_theta_min      2.32
_cell_volume                     7050.5(7)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_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  0.0628
_diffrn_reflns_av_sigmaI/netI    0.0747
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26980
_diffrn_reflns_theta_full        28.41
_diffrn_reflns_theta_max         28.41
_diffrn_reflns_theta_min         1.67
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2004)'
_exptl_crystal_colour            'deep purple'
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2824
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.439
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     396
_refine_ls_number_reflns         8840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0702P)^2^+1.1431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1437
_reflns_number_gt                5635
_reflns_number_total             8840
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb5425.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2226455
_cod_database_fobs_code          2226455