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_4110551
_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            'C21 H29 F3 N O5 Os P S'
_chemical_formula_weight         685.68
_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                 103.695(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   18.377(2)
_cell_length_b                   15.1715(17)
_cell_length_c                   36.589(4)
_cell_measurement_reflns_used    1021
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     9911.2(19)
_computing_cell_refinement       'SAINT+ v. 6.02 (Bruker AXS, 1999)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.02 (Bruker AXS, 1999)'
_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      173(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Bruker SMART 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  0.0579
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            123210
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.15
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    5.350
_exptl_absorpt_correction_T_max  0.516
_exptl_absorpt_correction_T_min  0.363
_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.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.838
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             5376
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.625
_refine_diff_density_min         -1.287
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1209
_refine_ls_number_reflns         24738
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.866
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.199
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+3.6931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0912
_reflns_number_gt                19318
_reflns_number_total             24738
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja060901tsi20060308_121721_1.cif
_cod_data_source_block           mae181as
_cod_original_cell_volume        9911.1(19)
_cod_database_code               4110551