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_4067668
_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        'See text'
_chemical_formula_moiety         'C36 H12 Cl3 F16 Os P S3, 1.38(C H2 Cl2)'
_chemical_formula_sum            'C37.38 H14.76 Cl5.76 F16 Os P S3'
_chemical_formula_weight         1289.35
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-01-30
_audit_creation_method           SHELXTL-Plus
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   15.3769(13)
_cell_length_b                   15.3769(13)
_cell_length_c                   34.068(4)
_cell_measurement_pressure       101(2)
_cell_measurement_reflns_used    55
_cell_measurement_temperature    298(1)
_cell_measurement_theta_max      12.09
_cell_measurement_theta_min      4.68
_cell_volume                     6976.1(12)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics
;
SHELXTL-Plus and MERCURY (Macrae et al., 2008)
;
_computing_publication_material  SHELXTL-Plus
_computing_structure_refinement  SHELXTL-Plus
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 2008)'
_diffrn_ambient_pressure         101(2)
_diffrn_ambient_temperature      298(1)
_diffrn_detector                 'Scintillation counter'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         X-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0707
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            3841
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.12
_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_%        2
_diffrn_standards_interval_count 48
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.335
_exptl_absorpt_correction_T_max  0.73823
_exptl_absorpt_correction_T_min  0.49692
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   ' XSCANS (Siemens, 1996)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3720
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2727
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0560P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1238
_reflns_number_gt                1704
_reflns_number_total             2727
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om901065g_si_001.cif
_cod_data_source_block           2e
_cod_original_cell_volume        6976.2(11)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4067668