A non-oxo methanolate-bridged divanadium(IV) complex with tris(2-sulfanidylphenyl)phosphane ligands: synthesis, structural characterization and magnetic investigation
Wu, Hong-Ming; Chang, Ya-Ho; Su, Chia-Lin; Lee, Gene-Hsiang; Hsu, Hua-Fen; Acta Crystallographica Section C 72 (2016) 416–420; doi:10.1107/S2053229616005222

data_2020487
_publ_section_title
;
 A non-oxo methanolate-bridged divanadium(IV) complex with
 tris(2-sulfanidylphenyl)phosphane ligands: synthesis, structural
 characterization and magnetic investigation
;
_journal_coeditor_code           YO3020
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              416
_journal_page_last               420
_journal_paper_doi               10.1107/S2053229616005222
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac
'(C24 H20 P) [V2 (C H3 O)3 (C27 H36 P S3)2], 2CH4 O'
_chemical_formula_moiety
'C24 H20 P +, C57 H81 O3 P2 S6 Si6 V2 -, 2(CH4 O) '
_chemical_formula_sum            'C83 H109 O5 P3 S6 Si6 V2'
_chemical_formula_weight         1742.39
_chemical_name_common            (PPh4)[V2(PS3'')2(mu-OMe)3]
_chemical_name_systematic
;Tetraphenylphosphonium
tri-\m-methanolato-\k^6^<i>O</i>:<i>O</i>-bis({tris[2-sulfanidyl-3-(trimethylsilyl)phenyl]phosphane-\k^4^<i>P</i>,<i>S</i>,<i>S</i>',<i>S</i>''}vanadium(IV)) methanol disolvate
;
_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
_audit_creation_method           ' SHELXL-97'
_cell_angle_alpha                90.00
_cell_angle_beta                 100.036(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.4740(12)
_cell_length_b                   25.4633(18)
_cell_length_c                   19.3663(13)
_cell_measurement_reflns_used    1430
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.60
_cell_measurement_theta_min      2.24
_cell_volume                     8970.7(11)
_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      150(2)
_diffrn_measurement_device_type  'BRUKER SMART APEXCCD area detector'
_diffrn_measurement_method       'omega 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  0.0996
_diffrn_reflns_av_sigmaI/netI    0.1176
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20475
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_T_max  0.9740
_exptl_absorpt_correction_T_min  0.7596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2004)
;
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3672
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.472
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         7880
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1369
_refine_ls_R_factor_gt           0.0877
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+20.3783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1712
_refine_ls_wR_factor_ref         0.1912
_reflns_number_gt                5218
_reflns_number_total             7880
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            yo3020sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2020487.cif.'
_cod_original_sg_symbol_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               2020487
_cod_database_fobs_code          2020487
_shelx_hkl_checksum              7894
_shelx_res_checksum              65761