One-Pot Dehydrogenative Addition of Isopropyl to Alkynes Promoted by Osmium: Formation of γ-(η3-Allyl)-α-Alkenylphosphine Derivatives Starting from a Dihydride−Dihydrogen−Triisopropylphosphine Complex
Esteruelas, Miguel A.; Hernández, Yohar A.; López, Ana M.; Oliván, Montserrat; Oñate, Enrique; Organometallics 26 (2007) 2193–; doi:10.1021/om070004d

data_4072999
_publ_section_title
;
 One-Pot Dehydrogenative Addition of Isopropyl to Alkynes Promoted by
 Osmium:&#x00A0; Formation of \g-(\h3-Allyl)-\a-Alkenylphosphine
 Derivatives Starting from a
 Dihydride&#x2212;Dihydrogen&#x2212;Triisopropylphosphine Complex
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2193
_journal_paper_doi               10.1021/om070004d
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C47 H56 B Os P'
_chemical_formula_weight         852.90
_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                87.048(2)
_cell_angle_beta                 89.732(2)
_cell_angle_gamma                87.597(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2407(16)
_cell_length_b                   12.5147(18)
_cell_length_c                   13.4682(19)
_cell_measurement_reflns_used    891
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     1890.4(5)
_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 0.990
_diffrn_measured_fraction_theta_max 0.906
_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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0800
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23924
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.94
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.448
_exptl_absorpt_correction_T_max  0.813
_exptl_absorpt_correction_T_min  0.724
_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    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.194
_refine_diff_density_min         -1.266
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.856
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         9077
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.856
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0130P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0517
_refine_ls_wR_factor_ref         0.0535
_reflns_number_gt                7540
_reflns_number_total             9077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om070004dsi20070214_020603.cif
_cod_data_source_block           mae213as
_cod_database_code               4072999