Preparation of Half-Sandwich Osmium-Allyl Complexes by Consecutive C−C Bond Formation and C−H Bond Activation Reactions
Esteruelas, Miguel A.; González, Ana I.; López, Ana M.; Oliván, Montserrat; Oñate, Enrique; Organometallics 25 (2006) 693–; doi:10.1021/om050907b

data_4074811
_publ_section_title
;
 Preparation of Half-Sandwich Osmium-Allyl Complexes by Consecutive
 C&#x2212;C Bond Formation and C&#x2212;H Bond Activation Reactions
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              693
_journal_paper_doi               10.1021/om050907b
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C23 H35 Os P'
_chemical_formula_weight         532.68
_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                99.221(2)
_cell_angle_beta                 95.381(2)
_cell_angle_gamma                105.264(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0672(14)
_cell_length_b                   10.3723(16)
_cell_length_c                   11.6987(18)
_cell_measurement_reflns_used    954
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     1037.0(3)
_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 0.990
_diffrn_measured_fraction_theta_max 0.922
_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  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13064
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.80
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    6.229
_exptl_absorpt_correction_T_max  0.4002
_exptl_absorpt_correction_T_min  0.3411
_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            yellow
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.191
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0174
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0207P)^2^+0.2244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0418
_refine_ls_wR_factor_ref         0.0421
_reflns_number_gt                4841
_reflns_number_total             4967
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050907bsi20051121_063054.cif
_cod_data_source_block           mae1601s
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4074811