A Hydrogen-Substituted Osmium Stannylene Complex: Isomerization to a Metallostannylene Complex via an Unusual α-Hydrogen Migration from Tin to Osmium
Paul G. Hayes; Christopher W. Gribble; Rory Waterman; T. Don Tilley; Journal of the American Chemical Society 131 (2009) 4606–4607; doi:10.1021/ja901050m

data_4104149
_publ_section_title
;
 A Hydrogen-Substituted Osmium Stannylene Complex: Isomerization to a
 Metallostannylene Complex via an Unusual \a-Hydrogen Migration from Tin
 to Osmium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4606
_journal_page_last               4607
_journal_paper_doi               10.1021/ja901050m
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C34 H60 Os P Sn'
_chemical_formula_weight         808.68
_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                 99.027(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0526(10)
_cell_length_b                   14.0417(16)
_cell_length_c                   28.238(3)
_cell_measurement_temperature    173(2)
_cell_volume                     3545.0(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0674
_diffrn_reflns_av_sigmaI/netI    0.0788
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            19919
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    4.350
_exptl_absorpt_correction_T_max  0.6462
_exptl_absorpt_correction_T_min  0.6017
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.975
_refine_diff_density_min         -1.268
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         7176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          14.996
_refine_ls_shift/su_mean         0.067
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1165
_reflns_number_gt                5308
_reflns_number_total             7176
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja901050m_si_001.cif
_cod_data_source_block           ph09m
_cod_original_cell_volume        3544.9(7)
_cod_database_code               4104149