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_4071878
_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         'C40 H64 N O Os P2, B F4'
_chemical_formula_sum            'C40 H64 B F4 N O Os P2'
_chemical_formula_weight         913.87
_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                92.738(4)
_cell_angle_beta                 94.386(4)
_cell_angle_gamma                107.905(4)
_cell_formula_units_Z            2
_cell_length_a                   10.258(2)
_cell_length_b                   14.422(3)
_cell_length_c                   14.825(3)
_cell_measurement_reflns_used    3033
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21
_cell_measurement_theta_min      2.5
_cell_volume                     2075.0(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      173(2)
_diffrn_detector_area_resol_mean 16.3990
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.908
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_sigmaI/netI    0.0829
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25911
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.81
_diffrn_reflns_theta_min         1.38
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.198
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.706
_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    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.514
_refine_diff_density_min         -1.256
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         9835
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1012
_reflns_number_gt                8194
_reflns_number_total             9835
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800439g_si_001.cif
_cod_data_source_block           mae253as
_cod_original_cell_volume        2075.1(8)
_cod_database_code               4071878