Chemistry of Vanadaboranes: Synthesis, Structures, and Characterization of Organovanadium Sulfide Clusters with Disulfido Linkage
Shubhankar Kumar Bose; K. Geetharani; V. Ramkumar; Babu Varghese; Sundargopal Ghosh; Inorganic Chemistry 49 (2010) 2881–2888; doi:10.1021/ic9023597

data_4315165
_publ_section_title
;
 Chemistry of Vanadaboranes: Synthesis, Structures, and Characterization
 of Organovanadium Sulfide Clusters with Disulfido Linkage
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2881
_journal_page_last               2888
_journal_paper_doi               10.1021/ic9023597
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         '0.5(C10 H10 S6 V2) . 0.5(C10 H10 S4 V2)'
_chemical_formula_sum            'C10 H10 S5 V2'
_chemical_formula_weight         392.36
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.75(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.885(3)
_cell_length_b                   7.0801(14)
_cell_length_c                   13.914(3)
_cell_measurement_reflns_used    2783
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.8
_cell_volume                     1367.2(5)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altornare et al., 1993)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9108
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         1.46
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.101
_exptl_absorpt_correction_T_max  0.722
_exptl_absorpt_correction_T_min  0.523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.535
_refine_diff_density_min         -1.351
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0684
_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^)+(0.0318P)^2^+13.3918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1523
_refine_ls_wR_factor_ref         0.1661
_reflns_number_gt                2481
_reflns_number_total             3046
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9023597_si_001_1.cif
_cod_data_source_block           mono
_cod_database_code               4315165