C(sp2)−H Activation of RCHE−py (E = CH, N) and RCHCHC(O)R‘ Substrates Promoted by a Highly Unsaturated Osmium−Monohydride Complex
Eguillor, Beatriz; Esteruelas, Miguel A.; Oliván, Montserrat; Oñate, Enrique; Organometallics 24 (2005) 1428–; doi:10.1021/om049064z

data_4075660
_publ_section_title
;
 C(sp2)&#x2212;H Activation of RCHE&#x2212;py (E = CH, N) and
 RCHCHC(O)R&#x2018; Substrates Promoted by a Highly Unsaturated
 Osmium&#x2212;Monohydride Complex
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1428
_journal_paper_doi               10.1021/om049064z
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C37 H60 Cl N Os P2 Sn'
_chemical_formula_weight         925.14
_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                102.092(2)
_cell_angle_beta                 91.235(2)
_cell_angle_gamma                117.825(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0322(12)
_cell_length_b                   11.7494(13)
_cell_length_c                   16.8982(18)
_cell_measurement_reflns_used    5447
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     1876.0(4)
_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 0.979
_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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18845
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.77
_diffrn_reflns_theta_min         1.24
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.231
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.627
_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    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.209
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.782
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         8787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.782
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0036P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0403
_refine_ls_wR_factor_ref         0.0417
_reflns_number_gt                7162
_reflns_number_total             8787
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049064zsi20060522_040723.cif
_cod_data_source_block           mae114s
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4075660