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_4349423
_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 S Se2 W'
_chemical_formula_weight         825.22
_chemical_name_systematic
;
{hydrotris(3,5-dimethylpyrazol-1-yl)borato}bis(selenophenolato)sulfidotungsten(V)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.0462(14)
_cell_length_b                   26.833(3)
_cell_length_c                   14.4646(14)
_cell_measurement_reflns_used    1611
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      19.55
_cell_measurement_theta_min      2.47
_cell_volume                     5839.9(10)
_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 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.1274
_diffrn_reflns_av_unetI/netI     0.1048
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34672
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.524
_diffrn_reflns_theta_min         1.518
_exptl_absorpt_coefficient_mu    6.549
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_description       plate
_exptl_crystal_F_000             3192
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.232
_refine_diff_density_min         -2.102
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         6701
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.0643
_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^)+(0.0436P)^2^+13.4262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1271
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4205
_reflns_number_total             6701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00331_si_002.cif
_cod_data_source_block           jmwspr13_Tp*WS(SePh)2
_cod_database_code               4349423
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              40264
_shelx_hkl_checksum              72317