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_4349422
_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            'C27 H32 B N6 O2 S W'
_chemical_formula_weight         699.30
_chemical_name_systematic
;
{hydrotris(3,5-dimethylpyrazol-1-yl)borato}bis(phenolato)sulfidotungsten(V)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                76.8880(10)
_cell_angle_beta                 85.3830(10)
_cell_angle_gamma                65.5180(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9067(7)
_cell_length_b                   11.0138(7)
_cell_length_c                   14.2504(9)
_cell_measurement_reflns_used    4238
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.26
_cell_volume                     1378.02(16)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0195
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7277
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.467
_exptl_absorpt_coefficient_mu    4.304
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_description       block
_exptl_crystal_F_000             694
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.046
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4780
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+0.2621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0621
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4489
_reflns_number_total             4780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00331_si_002.cif
_cod_data_source_block           jmwspr11_Tp*WS(OPh)2
_cod_database_code               4349422
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              42701
_shelx_hkl_checksum              74310