Efficient Concatenation of C═C Reduction, C−H Bond Activation, and C−C and C−N Coupling Reactions on Osmium: Assembly of Two Allylamines and an Allene
Baya, Miguel; Esteruelas, Miguel A.; Oñate, Enrique; Organometallics 29 (2010) 6298–; doi:10.1021/om100715k

data_4066927
_publ_section_title
;
 Efficient Concatenation of C&#x2550;C Reduction, C&#x2212;H Bond
 Activation, and C&#x2212;C and C&#x2212;N Coupling Reactions on Osmium:
 Assembly of Two Allylamines and an Allene
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6298
_journal_paper_doi               10.1021/om100715k
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C21 H41 F6 N O2 Os P2 Si'
_chemical_formula_weight         733.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.440(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.456(5)
_cell_length_b                   12.727(2)
_cell_length_c                   14.731(3)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2.2
_cell_volume                     5709.8(17)
_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 0.993
_diffrn_measured_fraction_theta_max 0.931
_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  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            53080
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.84
_diffrn_reflns_theta_min         1.34
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.678
_exptl_absorpt_correction_T_max  0.56
_exptl_absorpt_correction_T_min  0.40
_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            colorless
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         8.101
_refine_diff_density_min         -3.462
_refine_diff_density_rms         0.286
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         13933
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0809
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+342.3118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2048
_refine_ls_wR_factor_ref         0.2213
_reflns_number_gt                11894
_reflns_number_total             13933
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100715k_si_001.cif
_cod_data_source_block           enrique11bs
_cod_original_cell_volume        5709.7(18)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4066927