Synthesis and oxidation of d6 tungsten pincer complexes: a complete series of tungsten(II) hydridocarbonyl and halocarbonyl pincer complexes.
Wingard, Leah A.; White, Peter S.; Templeton, Joseph L.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 11438–11448; doi:10.1039/c2dt30848g

data_7030219
_publ_section_title
;
 Synthesis and oxidation of d6 tungsten pincer complexes: a complete
 series of tungsten(II) hydridocarbonyl and halocarbonyl pincer complexes.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11438
_journal_page_last               11448
_journal_paper_doi               10.1039/c2dt30848g
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C33 H38 N O3 P2 Si2 W, B F4, C H2 Cl2'
_chemical_formula_sum            'C34 H40 B Cl2 F4 N O3 P2 Si2 W'
_chemical_formula_weight         970.35
_chemical_name_systematic
;
?
;
_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                 90.665(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1944(5)
_cell_length_b                   18.9951(8)
_cell_length_c                   15.4344(6)
_cell_measurement_reflns_used    8257
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.07
_cell_measurement_theta_min      3.69
_cell_volume                     3868.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            31454
_diffrn_reflns_theta_full        67.96
_diffrn_reflns_theta_max         67.96
_diffrn_reflns_theta_min         3.35
_exptl_absorpt_coefficient_mu    8.654
_exptl_absorpt_correction_T_max  0.7345
_exptl_absorpt_correction_T_min  0.2018
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   Apex2
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.416
_refine_diff_density_min         -2.251
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         6614
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0623
_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^)+(0.0661P)^2^+38.6559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1649
_reflns_number_gt                4823
_reflns_number_total             6614
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30848g.txt
_cod_data_source_block           x0911002
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7030219