Syntheses, Characterization, and Computational Study of WSF4 and WSF4.CH3CN
Jared Nieboer; William Hillary; Xin Yu; Hélène P. A. Mercier; Michael Gerken; Inorganic Chemistry 48 (2009) 11251–11258; doi:10.1021/ic901752w

data_4303743
_publ_section_title
;
Syntheses, Characterization, and Computational Study of WSF4 and WSF4.CH3CN
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11251
_journal_page_last               11258
_journal_paper_doi               10.1021/ic901752w
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'F4 S W'
_chemical_formula_weight         291.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.886(3)
_cell_length_b                   5.3754(8)
_cell_length_c                   9.4435(14)
_cell_measurement_temperature    153(2)
_cell_volume                     857.2(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8767
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    27.381
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2665
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    4.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.331
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.207
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.024(13)
_refine_ls_extinction_coef       0.00027(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1953
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0201
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0177P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0412
_refine_ls_wR_factor_ref         0.0422
_reflns_number_gt                1856
_reflns_number_total             1953
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901752w_si_002_1.cif
_cod_data_source_block           mg07006_0ma
_cod_database_code               4303743