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_4331718
_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_sum            'C28.5 H32.5 B Cl1.5 N6 O P S3 W'
_chemical_formula_weight         850.10
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      43
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   32.242(6)
_cell_length_b                   41.145(6)
_cell_length_c                   10.352(4)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293
_cell_measurement_theta_max      38.1
_cell_measurement_theta_min      33.1
_cell_volume                     13733(6)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       AFC6R
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.02386
_diffrn_orient_matrix_UB_12      0.01527
_diffrn_orient_matrix_UB_13      -0.01123
_diffrn_orient_matrix_UB_21      0.00881
_diffrn_orient_matrix_UB_22      0.00421
_diffrn_orient_matrix_UB_23      -0.09109
_diffrn_orient_matrix_UB_31      -0.01775
_diffrn_orient_matrix_UB_32      -0.01844
_diffrn_orient_matrix_UB_33      -0.03012
_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  0.000
_diffrn_reflns_av_sigmaI/netI    0.050
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3342
_diffrn_reflns_theta_full        25.1
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        -1.9
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.747
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.683
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   Walker&Stuart_DIFABS
_exptl_crystal_colour            pale-green
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       plate
_exptl_crystal_F_000             6736
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.65
_refine_diff_density_min         -0.93
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         3227
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.055
_refine_ls_R_factor_gt           0.037
_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^)+(0.0502P)^2^+51.0763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.086
_refine_ls_wR_factor_ref         0.092
_reflns_number_observed          2559
_reflns_number_total             3227
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic051456qsup2.cif
_cod_data_source_block           '[Tp*WS(S2PPh2)(CO)].0.5CHCl3'
_cod_original_cell_volume        13733(5)
_cod_original_sg_symbol_H-M      'F d d 2    '
_cod_original_formula_sum        'C28.50 H32.50 B Cl1.50 N6 O P S3 W '
_cod_database_code               4331718