Triple Benzylic Dehydrogenation by Osmium in an Amide Ligand Environment
Lee, Joo-Ho; Pink, Maren; Caulton, Kenneth G.; Organometallics 25 (2006) 802–; doi:10.1021/om050916k

data_4074820
_publ_section_title
;
 Triple Benzylic Dehydrogenation by Osmium in an Amide Ligand Environment
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              802
_journal_paper_doi               10.1021/om050916k
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C32 H65 N Os P2 Si2'
_chemical_formula_sum            'C32 H65 N Os P2 Si2'
_chemical_formula_weight         772.17
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.6920(10)
_cell_angle_beta                 96.4360(10)
_cell_angle_gamma                98.4400(10)
_cell_formula_units_Z            2
_cell_length_a                   11.1319(4)
_cell_length_b                   12.8735(5)
_cell_length_c                   13.5173(5)
_cell_measurement_reflns_used    8099
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      36.3
_cell_measurement_theta_min      2.17
_cell_volume                     1903.26(12)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2003), XTEL (loc. libr.)'
_computing_publication_material  'SHELXTL (Bruker, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
'0.30 degree frames measured for 3 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       \w-scans
_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  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50566
_diffrn_reflns_theta_full        36.39
_diffrn_reflns_theta_max         36.39
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    3.517
_exptl_absorpt_correction_T_max  0.8438
_exptl_absorpt_correction_T_min  0.5398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.682
_refine_diff_density_min         -2.097
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         18183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0111P)^2^+1.5695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0771
_reflns_number_gt                14540
_reflns_number_total             18183
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050916ksi20051219_040532.cif
_cod_data_source_block           05198
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4074820