Paramagnetic Oxotungsten(V) Complexes Containing the Hydrotris(3,5-dimethylpyrazol-1-yl)borate Ligand
Stephen Sproules; Aston A. Eagle; Michelle K. Taylor; Robert W. Gable; Jonathan M. White; Charles G. Young; Inorganic Chemistry 50 (2011) 4503–4514; doi:10.1021/ic200161m

data_4325070
_publ_section_title
;
 Paramagnetic Oxotungsten(V) Complexes Containing the
 Hydrotris(3,5-dimethylpyrazol-1-yl)borate Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4503
_journal_page_last               4514
_journal_paper_doi               10.1021/ic200161m
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C58 H72 B2 N12 O3 S4 W2'
_chemical_formula_weight         1502.84
_chemical_name_systematic
;
 {hydrotris(3,5-dimethylpyrazol-1-yl)borato}oxobis(thiophenolato)tungsten(V)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 102.883(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5168(13)
_cell_length_b                   27.827(4)
_cell_length_c                   21.446(3)
_cell_measurement_reflns_used    5742
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      26.78
_cell_measurement_theta_min      2.40
_cell_volume                     6118.2(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_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         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_sigmaI/netI    0.0899
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31021
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    3.948
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       plate
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.987
_refine_diff_density_min         -2.362
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         10773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+12.3118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1374
_reflns_number_gt                8259
_reflns_number_total             10773
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200161m_si_002_3.cif
_cod_data_source_block           jmwspr15_Tp*WO(SPh)2
_cod_original_cell_volume        6118.1(13)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4325070