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_4075661
_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            'C34 H59 Cl O Os P2 Sn'
_chemical_formula_weight         890.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 94.7080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5516(8)
_cell_length_b                   19.3519(14)
_cell_length_c                   17.6856(13)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.7
_cell_measurement_theta_min      2.1
_cell_volume                     3599.1(5)
_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, SHELTX v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELTX 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 0.26
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.915
_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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44897
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.03
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.409
_exptl_absorpt_correction_T_max  0.545
_exptl_absorpt_correction_T_min  0.449
_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
 whithin SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0185
_refine_ls_shift/su_max          0.056
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0165P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0373
_refine_ls_wR_factor_ref         0.0380
_reflns_number_gt                7789
_reflns_number_total             8779
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049064zsi20060522_040723.cif
_cod_data_source_block           mae146as
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4075661