Aromatic C−H Bond Activation of 2-Methylpyridine Promoted by an Osmium(VI) Complex: Formation of an η2(N,C)-Pyridyl Derivative
Esteruelas, Miguel A.; Forcén, Elena; Oliván, Montserrat; Oñate, Enrique; Organometallics 27 (2008) 6188–; doi:10.1021/om800706g

data_4072254
_publ_section_title
;
 Aromatic C&#x2212;H Bond Activation of 2-Methylpyridine Promoted by an
 Osmium(VI) Complex: Formation of an \h2(N,C)-Pyridyl Derivative
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6188
_journal_paper_doi               10.1021/om800706g
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C24 H50 Cl N Os P2'
_chemical_formula_sum            'C24 H50 Cl N Os P2'
_chemical_formula_weight         640.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.762(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.867(5)
_cell_length_b                   15.319(7)
_cell_length_c                   17.315(7)
_cell_measurement_reflns_used    3931
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     2774(2)
_computing_cell_refinement       'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Bruker SMART 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  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25973
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.91
_diffrn_reflns_theta_min         1.81
_diffrn_standards_number         'no decay'
_exptl_absorpt_coefficient_mu    4.820
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.714
_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. 6.1 (2000).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.365
_refine_diff_density_min         -2.111
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         6790
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1045
_reflns_number_gt                4597
_reflns_number_total             6790
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800706g_si_001.cif
_cod_data_source_block           mae327as
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4072254