Tetrakis(2,3,5,6-tetrafluorobenzenethiolato-κ<i>S</i>)(triphenylphosphine-κ<i>P</i>)osmium(IV) <i>n</i>-hexane hemisolvate
Cerón, Margarita; Arroyo, Maribel; Bernès, Sylvain; Acta Crystallographica Section E 62 (2006) m2167–m2169; doi:10.1107/S1600536806029230

data_2210312
_publ_section_title
;Tetrakis(2,3,5,6-tetrafluorobenzenethiolato-\k<i>S</i>)(triphenylphosphine-\k<i>P</i>)osmium(IV)
 <i>n</i>-hexane hemisolvate
;
_journal_coeditor_code           KP2044
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2167
_journal_page_last               m2169
_journal_paper_doi               10.1107/S1600536806029230
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Os (C6 H F4 S)4 (C18 H15 P1)] , 0.5C6 H14'
_chemical_formula_moiety         'C42 H19 F16 Os P S4 , 0.5C6 H14'
_chemical_formula_sum            'C45 H26 F16 Os P S4'
_chemical_formula_weight         1220.07
_chemical_name_systematic
;
Tetrakis(2,3,5,6-tetrafluorobenzenethiolato-\kS)(triphenylphosphine-
\kP)osmium(IV) n-hexane hemisolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXTL-Plus
_cell_angle_alpha                89.20(2)
_cell_angle_beta                 87.40(2)
_cell_angle_gamma                86.454(15)
_cell_formula_units_Z            2
_cell_length_a                   12.209(3)
_cell_length_b                   13.513(3)
_cell_length_c                   13.865(3)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    296.0(10)
_cell_measurement_theta_max      12.17
_cell_measurement_theta_min      3.79
_cell_volume                     2280.6(9)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics
;
SHELXTL-Plus and MERCURY (Version 1.4.1; Macrae <i>et al.</i>,  2006)
;
_computing_publication_material  SHELXTL-Plus
_computing_structure_refinement  SHELXTL-Plus
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1998)'
_diffrn_ambient_temperature      296.0(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8756
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        28.1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.113
_exptl_absorpt_correction_T_max  0.778
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(XSCANS; Siemens, 1996)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1190
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.475
_refine_diff_density_min         -2.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         8033
_refine_ls_number_restraints     336
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0645
_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^)+(0.1011P)^2^+7.7358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1608
_refine_ls_wR_factor_ref         0.1740
_reflns_number_gt                6378
_reflns_number_total             8033
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            kp2044.cif
_cod_data_source_block           I
_cod_original_cell_volume        2280.5(9)
_cod_database_code               2210312
_cod_database_fobs_code          2210312