Cooperative Ge‒N Bond Activation in Hydrogallation Products of Alkynyl(diethylamino)germanes (Et2N)nGe(C≡CtBu)4‒n
Uhl, Werner; Tannert, Jens; Layh, Marcus; Hepp, Alexander; Grimme, Stefan; Risthaus, Tobias; Organometallics 32 (2013) 6770–; doi:10.1021/om400543v

data_4081791
_publ_section_title
;
 Cooperative Ge--N Bond Activation in Hydrogallation Products of
 Alkynyl(diethylamino)germanes (Et2N)nGe(C\\tb CtBu)4--n
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6770
_journal_paper_doi               10.1021/om400543v
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C38 H75 Ga2 Ge N'
_chemical_formula_weight         758.02
_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                 98.98(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.564(3)
_cell_length_b                   17.419(4)
_cell_length_c                   17.269(4)
_cell_measurement_reflns_used    43969
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      1.68
_cell_volume                     4327.3(17)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'imaginng plate detector'
_diffrn_measurement_method       'omega 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  0.0669
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            59540
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    1.949
_exptl_absorpt_correction_T_max  0.7587
_exptl_absorpt_correction_T_min  0.5744
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.648
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         10353
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+0.6553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                8105
_reflns_number_total             10353
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400543v_si_002.cif
_cod_data_source_block           sad
_cod_original_cell_volume        4327.3(15)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4081791