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_4325069
_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_moiety         'C33 H44 B N6 O3 W'
_chemical_formula_sum            'C33 H44 B N6 O3 W'
_chemical_formula_weight         767.40
_chemical_name_systematic
; 
 {hydrotris(3,5-dimethylpyrazol-1-yl)borato}bis(2-isopropylphenolato)
 oxotungsten(V)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 106.996(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.825(7)
_cell_length_b                   13.277(2)
_cell_length_c                   17.841(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.8
_cell_measurement_theta_min      9.5
_cell_volume                     6983(3)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'PROCESS_DATA (Gable et al., 1993)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4MachS diffractometer'
_diffrn_measurement_method       \w:2\q
_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  0.0154
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            8194
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  160
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.349
_exptl_absorpt_correction_T_max  0.4592
_exptl_absorpt_correction_T_min  0.2318
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SHELX76, corrected for I (Sheldrick, 1976)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3096
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6837
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+11.2641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0926
_reflns_number_gt                5209
_reflns_number_total             6837
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic200161m_si_002_2.cif
_cod_data_source_block           cy_21new_Tp*WO(PP)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        6983(2)
_cod_original_sg_symbol_Hall     '-C 2yc '
_cod_database_code               4325069