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_4086680
_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         'C24 H25 Cl N2 Os, 0.225(C H2 Cl2)'
_chemical_formula_sum            'C24.23 H25.45 Cl1.45 N2 Os'
_chemical_formula_weight         586.22
_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                76.540(2)
_cell_angle_beta                 83.6930(10)
_cell_angle_gamma                76.701(2)
_cell_formula_units_Z            8
_cell_length_a                   12.9012(14)
_cell_length_b                   15.4777(17)
_cell_length_c                   22.973(3)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     4333.9(9)
_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 0.997
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'Bruker APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            48199
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.61
_diffrn_reflns_theta_min         0.91
_exptl_absorpt_coefficient_mu    6.076
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.677
_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            yellow
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2284
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.013
_refine_diff_density_min         -1.385
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1078
_refine_ls_number_reflns         22007
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+5.9635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0725
_reflns_number_gt                18912
_reflns_number_total             22007
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00436_si_001.cif
_cod_data_source_block           4-enriquen51
_cod_original_cell_volume        4334.0(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4086680