Reaction of Hydrogen or Ammonia with Unsaturated Germanium or Tin Molecules under Ambient Conditions: Oxidative Addition versus Arene Elimination
Yang Peng; Jing-Dong Guo; Bobby D. Ellis; Zhongliang Zhu; James C. Fettinger; Shigeru Nagase; Philip P. Power; Journal of the American Chemical Society 131 (2009) 16272–16282; doi:10.1021/ja9068408

data_4105323
_publ_section_title
;
 Reaction of Hydrogen or Ammonia with Unsaturated Germanium or Tin
 Molecules under Ambient Conditions: Oxidative Addition versus Arene
 Elimination
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16272
_journal_page_last               16282
_journal_paper_doi               10.1021/ja9068408
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C48 H53 Ge N, C7 H8'
_chemical_formula_sum            'C55 H61 Ge N'
_chemical_formula_weight         808.66
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 89.973(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5642(10)
_cell_length_b                   21.275(3)
_cell_length_c                   23.860(3)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.70
_cell_volume                     4347.4(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            47138
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs, 2008'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       needle
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.524
_exptl_crystal_size_mid          0.289
_exptl_crystal_size_min          0.172
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         9945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+0.9489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                9369
_reflns_number_total             9945
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9068408_si_002_2.cif
_cod_data_source_block           py36f1
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               4105323