C-H Bond Activation and Subsequent C-C Bond Formation Promoted by Osmium: 2-Vinylpyridine-Acetylene Couplings
Miguel A. Esteruelas; Francisco J. Fernández-Alvarez; Montserrat Oliván; Enrique Oñate; Journal of the American Chemical Society 128 (2006) 4596–4597; doi:10.1021/ja060901t

data_4110553
_publ_contact_author
;
  Dr. Enrique O\~nate
  Departamento de Qu\'imica Inorg\'anica - I.C.M.A.
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       enriqueo@unizar.es
_publ_section_title
;
 C-H Bond Activation and Subsequent C-C Bond Formation Promoted by Osmium:
 2-Vinylpyridine-Acetylene Couplings
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4596
_journal_page_last               4597
_journal_paper_doi               10.1021/ja060901t
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C52.5 H61 B Cl3 N2 Os P'
_chemical_formula_weight         1058.36
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.093(3)
_cell_angle_beta                 108.341(2)
_cell_angle_gamma                109.829(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4068(18)
_cell_length_b                   14.961(2)
_cell_length_c                   15.509(3)
_cell_measurement_reflns_used    979
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      3
_cell_volume                     2339.7(7)
_computing_cell_refinement       'SAINT+ v. 6.1 (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 0.990
_diffrn_measured_fraction_theta_max 0.905
_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  0.0351
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_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29659
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.40
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    2.969
_exptl_absorpt_correction_T_max  0.6480
_exptl_absorpt_correction_T_min  0.5882
_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            brown
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1074
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.261
_refine_diff_density_min         -1.420
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         11267
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0638
_reflns_number_gt                9764
_reflns_number_total             11267
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja060901tsi20060308_121721_3.cif
_cod_data_source_block           mae184as
_cod_original_cell_volume        2339.8(6)
_cod_original_formula_sum        'C52.50 H61 B Cl3 N2 Os P'
_cod_database_code               4110553