Mononuclear Sulfido-Tungsten(V) Complexes: Completing the Tp*MEXY (M = Mo, W; E = O, S) Series.
Sproules, Stephen; Eagle, Aston A.; George, Graham N.; White, Jonathan M.; Young, Charles G.; Inorganic chemistry 56 (2017) 5189–5202; doi:10.1021/acs.inorgchem.7b00331

data_4349424
_publ_section_title
;
 Mononuclear Sulfido-Tungsten(V) Complexes: Completing the Tp*MEXY (M =
 Mo, W; E = O, S) Series.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5189
_journal_page_last               5202
_journal_paper_doi               10.1021/acs.inorgchem.7b00331
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C26 H36 B N6 O S3 W'
_chemical_formula_weight         739.45
_chemical_name_systematic
;
{hydrotris(3,5-dimethylpyrazol-1-yl)borato}sulfido(toluene-3,4-dithiolato)tungsten(V)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 103.156(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.771(4)
_cell_length_b                   10.380(3)
_cell_length_c                   21.227(6)
_cell_measurement_reflns_used    1626
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.13
_cell_measurement_theta_min      2.20
_cell_volume                     2954.6(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_unetI/netI     0.1390
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14462
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.519
_exptl_absorpt_coefficient_mu    4.153
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       rod
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.755
_refine_diff_density_min         -1.274
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.791
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.791
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0146P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0863
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3001
_reflns_number_total             5211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00331_si_002.cif
_cod_data_source_block           jmwspr10_Tp*WS(tdt)
_cod_original_cell_volume        2954.7(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4349424
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              21682
_shelx_hkl_checksum              69573