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_4066924
_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            'C15 H36 Cl N2 Os P'
_chemical_formula_weight         501.08
_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                 99.836(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.0286(19)
_cell_length_b                   15.1283(17)
_cell_length_c                   14.5231(16)
_cell_measurement_reflns_used    975
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     3686.4(7)
_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 0.996
_diffrn_measured_fraction_theta_max 0.945
_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  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            45297
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.89
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    7.145
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_correction_T_min  0.43
_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            'light yellow'
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.285
_refine_diff_density_min         -1.905
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         9156
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.224
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+34.4297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0888
_reflns_number_gt                8152
_reflns_number_total             9156
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100715k_si_001.cif
_cod_data_source_block           mae304as
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4066924