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_4074813
_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            'C48.5 H59 B Cl Os P'
_chemical_formula_weight         909.39
_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                85.988(4)
_cell_angle_beta                 75.399(5)
_cell_angle_gamma                78.292(5)
_cell_formula_units_Z            2
_cell_length_a                   9.615(2)
_cell_length_b                   13.811(3)
_cell_length_c                   17.423(4)
_cell_measurement_reflns_used    772
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      2
_cell_volume                     2191.9(8)
_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 0.982
_diffrn_measured_fraction_theta_max 0.903
_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  0.1627
_diffrn_reflns_av_sigmaI/netI    0.5133
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25962
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.73
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.038
_exptl_absorpt_correction_T_max  0.740
_exptl_absorpt_correction_T_min  0.538
_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    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             926
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.022
_refine_diff_density_min         -2.525
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.664
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         10249
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      0.666
_refine_ls_R_factor_all          0.1884
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1464
_reflns_number_gt                3381
_reflns_number_total             10249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050907bsi20051121_063054.cif
_cod_data_source_block           mae176as
_cod_original_cell_volume        2191.8(8)
_cod_original_formula_sum        'C48.50 H59 B Cl Os P'
_cod_database_code               4074813