A Germanium Isocyanide Complex Featuring (n → π*) Back-Bonding and Its Conversion to a Hydride/Cyanide Product via C-H Bond Activation under Mild Conditions
Zachary D. Brown; Petra Vasko; James C. Fettinger; Heikki M. Tuononen; Philip P. Power; Journal of the American Chemical Society 134 (2012) 4045–4048; doi:10.1021/ja211874u

data_4117598
_publ_section_title
;
 A Germanium Isocyanide Complex Featuring (n \\rightarrow \p*)
 Back-Bonding and Its Conversion to a Hydride/Cyanide Product via C-H Bond
 Activation under Mild Conditions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4045
_journal_page_last               4048
_journal_paper_doi               10.1021/ja211874u
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C49 H51 Ge N'
_chemical_formula_weight         726.50
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.1260(10)
_cell_angle_beta                 89.7840(10)
_cell_angle_gamma                67.8890(10)
_cell_formula_units_Z            2
_cell_length_a                   8.9615(4)
_cell_length_b                   10.0990(5)
_cell_length_c                   23.3680(11)
_cell_measurement_reflns_used    9045
_cell_measurement_temperature    90
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.46
_cell_volume                     1926.01(16)
_computing_cell_refinement       'SAINT (7.68A) (Bruker, 2009)'
_computing_data_collection       'SMART (Version 5.054) (Bruker, 2002)'
_computing_data_reduction        'SAINT (7.68A) (Bruker, 2009)'
_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
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 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  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            18218
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         0.89
_exptl_absorpt_coefficient_mu    0.830
_exptl_absorpt_correction_T_max  0.9186
_exptl_absorpt_correction_T_min  0.7378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description       Block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         7068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0617P)^2^+2.3630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1126
_reflns_number_gt                6308
_reflns_number_total             7068
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja211874u_si_003.cif
_cod_data_source_block           zb99_0m
_cod_database_code               4117598