Carbon−Fluorine Bond Activation in Thermolysis Reactions of the Osmium(IV) Perfluorothiolate Compounds [Os(SC6F5)4(P(C6H4X-4)3)] (X = CF3, Cl, F, H, CH3, and OCH3)
Mendoza, Consuelo; Bernès, Sylvain; Torrens, Hugo; Arroyo, Maribel; Organometallics 29 (2010) 2646–; doi:10.1021/om901065g

data_4067661
_publ_section_title
;
 Carbon&#x2212;Fluorine Bond Activation in Thermolysis Reactions of the
 Osmium(IV) Perfluorothiolate Compounds [Os(SC6F5)4(P(C6H4X-4)3)] (X =
 CF3, Cl, F, H, CH3, and OCH3)
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2646
_journal_paper_doi               10.1021/om901065g
_journal_volume                  29
_journal_year                    2010
_chemical_compound_source        'CH2Cl2/hexane (9:1)'
_chemical_formula_moiety         'C45 H21 F20 Os P S4, 0.5(H2 O)'
_chemical_formula_sum            'C45 H22 F20 O0.5 Os P S4'
_chemical_formula_weight         1300.04
_chemical_melting_point          423
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2009-03-11
_audit_creation_method           SHELXTL-Plus
_cell_angle_alpha                77.420(8)
_cell_angle_beta                 72.116(8)
_cell_angle_gamma                67.338(9)
_cell_formula_units_Z            2
_cell_length_a                   11.6506(13)
_cell_length_b                   12.6198(14)
_cell_length_c                   18.777(2)
_cell_measurement_pressure       101(2)
_cell_measurement_reflns_used    52
_cell_measurement_temperature    296(1)
_cell_measurement_theta_max      12.45
_cell_measurement_theta_min      4.77
_cell_volume                     2408.9(5)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXTL-Plus
_computing_structure_refinement  SHELXTL-Plus
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1998)'
_diffrn_ambient_pressure         101(2)
_diffrn_ambient_temperature      296(1)
_diffrn_detector                 'Scintillation counter'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0583
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9725
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.96
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30
_diffrn_source_power             1.5
_diffrn_source_type              FN4
_diffrn_source_voltage           50
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.965
_exptl_absorpt_correction_T_max  0.554
_exptl_absorpt_correction_T_min  0.486
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'XSCAnS (Siemens, 1996)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1262
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.395
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     658
_refine_ls_number_reflns         8365
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0430P)^2^+3.9509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0994
_reflns_number_gt                6790
_reflns_number_total             8365
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om901065g_si_001.cif
_cod_data_source_block           5a
_cod_original_formula_sum        'C45 H22 F20 O0.50 Os P S4'
_cod_database_code               4067661