Osmium-Catalyzed Allylic Alkylation
Esteruelas, Miguel A.; García-Yebra, Cristina; Oliván, Montserrat; Oñate, Enrique; Valencia, Marta; Organometallics 27 (2008) 4892–; doi:10.1021/om800460h

data_4071903
_publ_section_title
;
 Osmium-Catalyzed Allylic Alkylation
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4892
_journal_paper_doi               10.1021/om800460h
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C29 H35 Cl N O6 Os P'
_chemical_formula_weight         750.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   17.820(3)
_cell_length_b                   16.545(2)
_cell_length_c                   19.229(3)
_cell_measurement_reflns_used    5937
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      2.5
_cell_volume                     5669.3(15)
_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  0.0846
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            67418
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.90
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.693
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.444
_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            yellow
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.660
_refine_diff_density_min         -2.261
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         7148
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+15.5373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1039
_reflns_number_gt                5765
_reflns_number_total             7148
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800460h_si_001.cif
_cod_data_source_block           mae2911b
_cod_original_cell_volume        5669.5(14)
_cod_original_sg_symbol_H-M      'P bca'
_cod_database_code               4071903