π-Acid/π-Base Carbonyloxo, Carbonylsulfido, and Mixed-Valence Complexes of Tungsten
Thomas, Simon; Tiekink, Edward R. T.; Young, Charles G.; Inorganic Chemistry 45 (2006) 352–361; doi:10.1021/ic051456q

data_4331716
_publ_section_title
;
 \p-Acid/\p-Base Carbonyloxo, Carbonylsulfido, and Mixed-Valence Complexes
 of Tungsten
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              352
_journal_page_last               361
_journal_paper_doi               10.1021/ic051456q
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C28 H32 B N6 O2 P S2 W '
_chemical_formula_sum            'C28 H32 B N6 O2 P S2 W'
_chemical_formula_weight         774.35
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                96.33(2)
_cell_angle_beta                 107.34(2)
_cell_angle_gamma                73.03(2)
_cell_formula_units_Z            2
_cell_length_a                   11.281(2)
_cell_length_b                   16.228(6)
_cell_length_c                   9.338(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      44.3
_cell_measurement_theta_min      41.5
_cell_volume                     1560.2(8)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan for Windows (MSC, 1997)'
_computing_publication_material  'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
'SIR92 (Burla, 1989)'
;
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       AFC6R
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.01090
_diffrn_orient_matrix_UB_12      -0.01941
_diffrn_orient_matrix_UB_13      -0.10185
_diffrn_orient_matrix_UB_21      0.00018
_diffrn_orient_matrix_UB_22      -0.05950
_diffrn_orient_matrix_UB_23      0.01897
_diffrn_orient_matrix_UB_31      -0.09591
_diffrn_orient_matrix_UB_32      0.01540
_diffrn_orient_matrix_UB_33      -0.04313
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_av_sigmaI/netI    0.062
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7536
_diffrn_reflns_theta_full        27.6
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        -0.3
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.927
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.536
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   Walker&Stuart_DIFABS
_exptl_crystal_colour            dark-pink
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.93
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         7173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.072
_refine_ls_R_factor_gt           0.035
_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^)+(0.0322P)^2^+0.4985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.074
_refine_ls_wR_factor_ref         0.083
_reflns_number_observed          5439
_reflns_number_total             7173
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic051456qsup1.cif
_cod_data_source_block           '[Tp*WO(S2PPh2)(CO)]'
_cod_original_cell_volume        1560.3(8)
_cod_original_sg_symbol_H-M      'P -1       '
_cod_original_formula_sum        'C28 H32 B N6 O2 P S2 W '
_cod_database_code               4331716