Reactivity of germanium(II) hydride with nitrous oxide, trimethylsilyl azide, ketones, and alkynes and the reaction of a methyl analogue with trimethylsilyl diazomethane.
Jana, Anukul; Roesky, Herbert W.; Schulzke, Carola; Dalton transactions (Cambridge, England : 2003) 39 (2010) 132–138; doi:10.1039/b914164b

data_7024279
_publ_section_title
;
 Reactivity of germanium(II) hydride with nitrous oxide, trimethylsilyl
 azide, ketones, and alkynes and the reaction of a methyl analogue with
 trimethylsilyl diazomethane.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              132
_journal_page_last               138
_journal_paper_doi               10.1039/b914164b
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C37 H47 F3 Ge N2 O'
_chemical_formula_weight         665.36
_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                79.54(3)
_cell_angle_beta                 83.10(3)
_cell_angle_gamma                69.63(3)
_cell_formula_units_Z            2
_cell_length_a                   10.833(2)
_cell_length_b                   11.879(2)
_cell_length_c                   14.500(3)
_cell_measurement_reflns_used    15959
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      54.2
_cell_measurement_theta_min      3.7
_cell_volume                     1716.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  IPDSII
_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  0.1029
_diffrn_reflns_av_sigmaI/netI    0.0849
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15959
_diffrn_reflns_theta_full        27.09
_diffrn_reflns_theta_max         27.09
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.939
_exptl_absorpt_correction_T_max  0.9051
_exptl_absorpt_correction_T_min  0.7846
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.873
_refine_diff_density_min         -1.444
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         7458
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0724
_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^)+(0.1187P)^2^+0.3561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1880
_refine_ls_wR_factor_ref         0.2109
_reflns_number_gt                5519
_reflns_number_total             7458
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b914164b.txt
_cod_data_source_block           ja50
_cod_original_cell_volume        1717.0(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7024279