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_4105322
_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 H52 Ge'
_chemical_formula_sum            'C48 H52 Ge'
_chemical_formula_weight         701.49
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.701(5)
_cell_length_b                   43.699(11)
_cell_length_c                   8.231(2)
_cell_measurement_reflns_used    2901
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      23.78
_cell_measurement_theta_min      3.01
_cell_volume                     7446(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1156
_diffrn_reflns_av_sigmaI/netI    0.0916
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            20228
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.002(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4253
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1118
_reflns_number_gt                3451
_reflns_number_total             4253
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9068408_si_002_1.cif
_cod_data_source_block           fdd2
_cod_original_cell_volume        7445(3)
_cod_database_code               4105322