Synthesis of a Vanadium(III) Tris(arylthiolato) Complex and Its Reactions with Azide and Azo Compounds: Formation of a Sulfenamide Complex via Cleavage of an Azo NN Bond
Komuro, Takashi; Matsuo, Tsukasa; Kawaguchi, Hiroyuki; Tatsumi, Kazuyuki; Inorganic Chemistry 44 (2005) 175–177; doi:10.1021/ic048721c

data_4308374
_publ_section_title
;
 Synthesis of a Vanadium(III) Tris(arylthiolato) Complex and Its Reactions
 with Azide and Azo Compounds: Formation of a Sulfenamide Complex via
 Cleavage of an Azo NN Bond
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              175
_journal_page_last               177
_journal_paper_doi               10.1021/ic048721c
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C30 H57 N2 S2 Si4 V '
_chemical_formula_sum            'C30 H57 N2 S2 Si4 V'
_chemical_formula_weight         673.20
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             2004-06-19
_audit_creation_method           'by CrystalStructure v3.5.1'
_cell_angle_alpha                90
_cell_angle_beta                 106.141(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.338(4)
_cell_length_b                   19.654(7)
_cell_length_c                   21.400(9)
_cell_measurement_reflns_used    12092
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3773(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure Ver. 3.5.1'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    'DIRDIF99 (PATTY)'
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.9919
_diffrn_measured_fraction_theta_max 0.9934
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
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_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            reddish-brown
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1448.00
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.31
_refine_diff_density_min         -1.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     392
_refine_ls_number_reflns         8602
_refine_ls_R_factor_gt           0.0820
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0071Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2450
_reflns_number_gt                6399
_reflns_number_total             8863
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic048721csi20041021_032116_2.cif
_cod_data_source_block
'_V{SC6H3(CH2SiMe2)(SiMe3)}{SC6H3(SiMe3)2}(tmeda)'
_cod_original_cell_volume        3772.7(26)
_cod_original_formula_sum        'C30 H57 N2 S2 Si4 V '
_cod_database_code               4308374