A Germanium(II) Hydride as an Effective Reagent for Hydrogermylation Reactions
Anukul Jana; Debajyoti Ghoshal; Herbert W. Roesky; Ina Objartel; Gerald Schwab; Dietmar Stalke; Journal of the American Chemical Society 131 (2009) 1288–1293; doi:10.1021/ja808656t

data_4103827
_publ_contact_author             'Prof. Dr. H. W. Roesky'
_publ_contact_author_email
'hroesky@gwdg.de, dstalke@chemie.uni-goettingen.de'
_publ_section_title
;
 A Germanium(II) Hydride as an Effective Reagent for Hydrogermylation
 Reactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1288
_journal_page_last               1293
_journal_paper_doi               10.1021/ja808656t
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C30 H42 Ge N2 O2'
_chemical_formula_weight         535.25
_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                98.446(2)
_cell_angle_beta                 96.896(2)
_cell_angle_gamma                109.595(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7449(12)
_cell_length_b                   11.7058(16)
_cell_length_c                   14.970(2)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.715
_cell_measurement_theta_min      2.543
_cell_volume                     1404.2(3)
_computing_cell_refinement       'SAINT V7.46A'
_computing_data_collection       'APEX2 v2.2-0'
_computing_data_reduction        'SAINT V7.46A'
_computing_molecular_graphics    'XSHELL ver. 4.01'
_computing_publication_material  'XSHELL ver. 4.01'
_computing_structure_refinement  'SHELXL in SHELXTL Ver. 6.10'
_computing_structure_solution    'SHELXS in SHELXTL Ver. 6.10'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Smart Apex II with D8-Goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC quazar mirrior optics'
_diffrn_radiation_source         'INCOATEC Mo micro source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            26322
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    1.119
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS2008/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         5494
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0000P)^2^+2.4506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0876
_reflns_number_gt                5286
_reflns_number_total             5494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808656t_si_002_1.cif
_cod_data_source_block           3
_cod_database_code               4103827