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_4325068
_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            'C27 H32 B N6 O3 W'
_chemical_formula_weight         683.25
_chemical_name_systematic
;
 {hydrotris(3,5-dimethylpyrazol-1-yl)borato}oxobis(phenolato)tungsten(V)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 107.513(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3243(17)
_cell_length_b                   10.3973(10)
_cell_length_c                   16.8989(18)
_cell_measurement_reflns_used    2599
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.08
_cell_measurement_theta_min      2.48
_cell_volume                     2735.3(5)
_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 0.996
_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  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0830
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14143
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    4.263
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_description       block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.189
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.792
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         4798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.792
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0091P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0505
_refine_ls_wR_factor_ref         0.0537
_reflns_number_gt                3597
_reflns_number_total             4798
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200161m_si_002_1.cif
_cod_data_source_block           jmwspr3a_Tp*WO(OPh)2
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4325068