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_4081787
_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            'C33 H58 Al F Ge N'
_chemical_formula_weight         587.37
_chemical_name_systematic
; 
 ? 
;
_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                90.675(5)
_cell_angle_beta                 97.831(5)
_cell_angle_gamma                98.747(5)
_cell_formula_units_Z            2
_cell_length_a                   9.7221(18)
_cell_length_b                   10.986(2)
_cell_length_c                   17.117(3)
_cell_measurement_reflns_used    9833
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.15
_cell_measurement_theta_min      2.62
_cell_volume                     1789.1(6)
_computing_cell_refinement       'SAINT V8.18C (Bruker AXS Inc.)'
_computing_data_collection       'APEX2 v2012.2-0'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc.)'
_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      153(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Photon 100 CMOS-detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'Venture Mo multilayer optic'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28551
_diffrn_reflns_theta_full        30.16
_diffrn_reflns_theta_max         30.16
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_T_max  0.7605
_exptl_absorpt_correction_T_min  0.6705
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             634
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         10433
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0447P)^2^+0.4321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0771
_reflns_number_gt                9745
_reflns_number_total             10433
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400543v_si_002.cif
_cod_data_source_block           sad
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4081787