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_4067664
_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 (1:4)'
_chemical_formula_moiety         'C30 H5 F19 Os S4'
_chemical_formula_sum            'C30 H5 F19 Os S4'
_chemical_formula_weight         1044.78
_chemical_melting_point          493
_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                74.697(7)
_cell_angle_beta                 82.010(10)
_cell_angle_gamma                83.771(9)
_cell_formula_units_Z            2
_cell_length_a                   10.7829(13)
_cell_length_b                   12.2538(13)
_cell_length_c                   12.7859(15)
_cell_measurement_pressure       101(2)
_cell_measurement_reflns_used    87
_cell_measurement_temperature    293(1)
_cell_measurement_theta_max      13.78
_cell_measurement_theta_min      4.61
_cell_volume                     1609.1(3)
_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      293(1)
_diffrn_detector                 'Scintillation counter'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14865
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.66
_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    4.357
_exptl_absorpt_correction_T_max  0.147
_exptl_absorpt_correction_T_min  0.096
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'XSCANS (Siemens, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.00140(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL-Plus
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     488
_refine_ls_number_reflns         9286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0263
_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^)+(0.0250P)^2^+0.9375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0628
_reflns_number_gt                8408
_reflns_number_total             9286
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om901065g_si_001.cif
_cod_data_source_block           4b
_cod_database_code               4067664