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_4303744
_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            'C2 H3 F4 N S W'
_chemical_formula_weight         332.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.995(3)
_cell_length_b                   7.874(2)
_cell_length_c                   8.046(2)
_cell_measurement_temperature    153(2)
_cell_volume                     696.6(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0141
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7627
_diffrn_reflns_theta_full        28.78
_diffrn_reflns_theta_max         28.78
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    16.873
_exptl_absorpt_correction_T_max  0.4112
_exptl_absorpt_correction_T_min  0.1925
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.944
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.00319(17)
_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   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         930
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0127
_refine_ls_R_factor_gt           0.0123
_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^)+(0.0115P)^2^+0.8001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0301
_refine_ls_wR_factor_ref         0.0303
_reflns_number_gt                912
_reflns_number_total             930
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901752w_si_002_2.cif
_cod_data_source_block           mg08001_0ma
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'contr' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        696.5(3)
_cod_database_code               4303744