Synthesis and Characterization of the κ2-acac-O,OComplex OsIV(acac)2PhCl and Study of CH Activation with Benzene
Young, Kenneth J. H.; Mironov, Oleg A.; Nielsen, Robert J.; Cheng, Mu-Jeng; Stewart, Timothy; Goddard, William A.; Periana, Roy A.; Organometallics 30 (2011) 5088–; doi:10.1021/om1010512

data_4063938
_publ_section_title
;
 Synthesis and Characterization of the \k2-acac-O,OComplex OsIV(acac)2PhCl
 and Study of CH Activation with Benzene
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5088
_journal_paper_doi               10.1021/om1010512
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C17 H19 F3 O7 Os S'
_chemical_formula_weight         614.58
_chemical_name_systematic
; 
 ? 
;
_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           SHELXL-97
_cell_angle_alpha                86.170(2)
_cell_angle_beta                 88.963(3)
_cell_angle_gamma                85.364(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5774(6)
_cell_length_b                   9.3032(5)
_cell_length_c                   13.0773(7)
_cell_measurement_reflns_used    4455
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.78
_cell_volume                     1037.71(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6338
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    6.306
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing,R.H.,Acta Crystallogr.1995,A51,33'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_density_meas      1.962
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.532
_refine_diff_density_min         -1.138
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4455
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0771
_reflns_number_gt                3905
_reflns_number_total             4455
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1010512_si_002.cif
_cod_data_source_block           osphotfm
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4063938