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_4331720
_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            'C31.5 H45 B2 Cl I2 N12 O3 W2'
_chemical_formula_weight         1318.36
_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                93.97(1)
_cell_angle_beta                 97.55(1)
_cell_angle_gamma                97.30(1)
_cell_formula_units_Z            2
_cell_length_a                   13.348(1)
_cell_length_b                   13.962(2)
_cell_length_c                   12.275(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      14.7
_cell_volume                     2240.8(5)
_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 0.856
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device       'Rigaku AFC6R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.07579
_diffrn_orient_matrix_UB_12      0.01472
_diffrn_orient_matrix_UB_13      0.00436
_diffrn_orient_matrix_UB_21      0.00700
_diffrn_orient_matrix_UB_22      0.00316
_diffrn_orient_matrix_UB_23      0.08233
_diffrn_orient_matrix_UB_31      0.00530
_diffrn_orient_matrix_UB_32      -0.07090
_diffrn_orient_matrix_UB_33      -0.00279
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.071
_diffrn_reflns_av_sigmaI/netI    0.093
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7200
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.1
_diffrn_reflns_theta_max         25.1
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        -1.8
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.618
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.500
_exptl_absorpt_correction_type
;
\DF (DIFABS; Walker & Stuart, 1983)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1246
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.90
_refine_diff_density_min         -1.60
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         6831
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.120
_refine_ls_R_factor_gt           0.053
_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^)+(0.0933P)^2^+3.2449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.142
_refine_ls_wR_factor_ref         0.167
_reflns_number_gt                4331
_reflns_number_total             6831
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic051456qsup3.cif
_cod_data_source_block           '[Tp*WI(CO)(mu-O)WOITp*]0.5CH2Cl2'
_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_sg_symbol_H-M      'P -1       '
_cod_original_formula_sum        'C31.50 H45 B2 Cl I2 N12 O3 W2 '
_cod_database_code               4331720