Cβ(sp2)−H Bond Activation of α,β-Unsaturated Ketones Promoted by a Hydride-Elongated Dihydrogen Complex: Formation of Osmafuran Derivatives with Carbene, Carbyne, and NH-Tautomerized α-Substituted Pyridine Ligands
Buil, María L.; Esteruelas, Miguel A.; Garcés, Karin; Oliván, Montserrat; Oñate, Enrique; Organometallics 27 (2008) 4680–; doi:10.1021/om800439g

data_4071876
_publ_section_title
;
 C\b(sp2)&#x2212;H Bond Activation of \a,\b-Unsaturated Ketones Promoted
 by a Hydride-Elongated Dihydrogen Complex: Formation of Osmafuran
 Derivatives with Carbene, Carbyne, and NH-Tautomerized \a-Substituted
 Pyridine Ligands
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4680
_journal_paper_doi               10.1021/om800439g
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C26 H53 O2 Os P2, B F4'
_chemical_formula_sum            'C26 H53 B F4 O2 Os P2'
_chemical_formula_weight         736.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           59
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2a'
_symmetry_space_group_name_H-M   'P m m n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.041(4)
_cell_length_b                   14.089(4)
_cell_length_c                   8.462(2)
_cell_measurement_reflns_used    3567
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.3
_cell_measurement_theta_min      2.5
_cell_volume                     1554.8(7)
_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      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.957
_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  0.0712
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            18234
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.83
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.249
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.606
_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            red
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.270
_refine_diff_density_min         -5.166
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2106
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+19.4476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1361
_reflns_number_gt                1977
_reflns_number_total             2106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800439g_si_001.cif
_cod_data_source_block           mae229bs
_cod_original_cell_volume        1554.9(7)
_cod_original_sg_symbol_H-M      Pmmn
_cod_database_code               4071876