Preparation of Capped Octahedral OsHC6Complexes by Sequential Carbon-Directed C‒H Bond Activation Reactions
Esteruelas, Miguel A.; Oñate, Enrique; Palacios, Adrián; Tsai, Jui-Yi; Xia, Chuanjun; Organometallics 35 (2016) 2532–; doi:10.1021/acs.organomet.6b00436

data_4086682
_publ_section_title
;
 Preparation of Capped Octahedral OsHC6Complexes by Sequential
 Carbon-Directed C--H Bond Activation Reactions
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              2532
_journal_paper_doi               10.1021/acs.organomet.6b00436
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C34 H32 N7 Os, C F3 O3 S '
_chemical_formula_sum            'C35 H32 F3 N7 O3 Os S'
_chemical_formula_weight         877.94
_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                73.721(2)
_cell_angle_beta                 83.081(2)
_cell_angle_gamma                76.522(2)
_cell_formula_units_Z            4
_cell_length_a                   12.3099(14)
_cell_length_b                   14.2086(16)
_cell_length_c                   21.270(2)
_cell_measurement_reflns_used    4388
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     3466.7(6)
_computing_cell_refinement       'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_data_collection       'apex2 v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_sigmaI/netI    0.1163
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31879
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    3.801
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 7.56a (2008).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.122
_refine_diff_density_min         -1.716
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     882
_refine_ls_number_reflns         12823
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1158
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1299
_reflns_number_gt                7994
_reflns_number_total             12823
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00436_si_001.cif
_cod_data_source_block           10c-enrique198
_cod_original_cell_volume        3466.7(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4086682