Chloridotris(pentafluorobenzenethiolato-κ<i>S</i>)[tris(4-fluorophenyl)phosphine-κ<i>P</i>]osmium(IV)
Arias, Asdrúbal; Meléndez, Lidia; Bernès, Sylvain; Arroyo, Maribel; Acta Crystallographica Section E 66 (2010) m477–m478; doi:10.1107/S1600536810011281

data_2225628
_publ_section_title
;
 Chloridotris(pentafluorobenzenethiolato-\k<i>S</i>)[tris(4-fluorophenyl)phosphine-\k<i>P</i>]osmium(IV)
;
_journal_coeditor_code           KP2255
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m477
_journal_page_last               m478
_journal_paper_doi               10.1107/S1600536810011281
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Os (C6 F5 S)3 Cl (C18 H12 F3 P)]'
_chemical_formula_moiety         'C36 H12 Cl F18 Os P S3'
_chemical_formula_sum            'C36 H12 Cl F18 Os P S3'
_chemical_formula_weight         1139.26
_chemical_name_systematic
;
Chloridotris(pentafluorobenzenethiolato-\k<i>S</i>)[tris(4-
fluorophenyl)phosphine-\k<i>P</i>]osmium(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL-Plus
_cell_angle_alpha                90.00
_cell_angle_beta                 107.62(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.983(7)
_cell_length_b                   10.446(5)
_cell_length_c                   21.521(8)
_cell_measurement_pressure       101(2)
_cell_measurement_reflns_used    84
_cell_measurement_temperature    298.0(10)
_cell_measurement_theta_max      12.47
_cell_measurement_theta_min      5.21
_cell_volume                     3853(3)
_computing_cell_refinement       'XSCANS (Siemens, 1996)'
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        'XSCANS (Siemens, 1996)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>,  2008)'
_computing_publication_material  'SHELXTL-Plus (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL-Plus (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.0(10)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0516
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13694
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.699
_exptl_absorpt_correction_T_max  0.330
_exptl_absorpt_correction_T_min  0.215
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(XSCANS; Siemens, 1996)'
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.964
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.956
_refine_diff_density_min         -2.106
_refine_ls_extinction_coef       0.00165(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXTL-Plus (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.325
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     542
_refine_ls_number_reflns         6749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.325
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+24.9505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1349
_reflns_number_gt                5120
_reflns_number_total             6749
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            kp2255.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2225628
_cod_database_fobs_code          2225628