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_4086681
_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         'C22 H23 N6 Os, C F3 O3 S, C H2 Cl2'
_chemical_formula_sum            'C24 H25 Cl2 F3 N6 O3 Os S'
_chemical_formula_weight         795.66
_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                69.4460(10)
_cell_angle_beta                 80.3970(10)
_cell_angle_gamma                78.8170(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7097(4)
_cell_length_b                   13.2661(7)
_cell_length_c                   13.7956(7)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     1455.70(13)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.899
_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  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15454
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.51
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    4.692
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.676
_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    1.815
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.199
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         6653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0232
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+2.5142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0583
_reflns_number_gt                6279
_reflns_number_total             6653
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00436_si_001.cif
_cod_data_source_block           8-enrique184
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4086681