A crystallographic and spectroscopic study on the reactions of WCl6 with carbonyl compounds.
Dolci, Sara; Marchetti, Fabio; Pampaloni, Guido; Zacchini, Stefano; Dalton transactions (Cambridge, England : 2003) 42 (2013) 5635–5648; doi:10.1039/c2dt32771f

data_7021113
_publ_section_title
;
 A crystallographic and spectroscopic study on the reactions of WCl6 with
 carbonyl compounds.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5635
_journal_page_last               5648
_journal_paper_doi               10.1039/c2dt32771f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C3 H5 Cl4 O3 W'
_chemical_formula_weight         414.72
_chemical_name_systematic
;
?
;
_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                 120.147(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.305(4)
_cell_length_b                   9.7756(19)
_cell_length_c                   12.088(2)
_cell_measurement_reflns_used    5026
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.407
_cell_measurement_theta_min      2.4485
_cell_volume                     1870.5(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7541
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    13.450
_exptl_absorpt_correction_T_max  0.2547
_exptl_absorpt_correction_T_min  0.2221
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.945
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.291
_refine_diff_density_min         -2.059
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.244
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.244
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0111P)^2^+34.1802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0616
_reflns_number_gt                1979
_reflns_number_total             2039
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32771f.txt
_cod_data_source_block           fm2605b9_C2C
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7021113