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_7024280
_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            'C35 H45 F3 Ge N2 O S'
_chemical_formula_weight         671.38
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 98.61(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.142(2)
_cell_length_b                   8.7405(17)
_cell_length_c                   32.073(6)
_cell_measurement_reflns_used    26340
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      51.8
_cell_measurement_theta_min      2.6
_cell_volume                     3365.5(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            25583
_diffrn_reflns_theta_full        25.91
_diffrn_reflns_theta_max         25.91
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_T_max  0.7366
_exptl_absorpt_correction_T_min  0.6550
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.37
_refine_diff_density_max         1.115
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0566P)^2^+5.7562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1385
_reflns_number_gt                6047
_reflns_number_total             6486
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b914164b.txt
_cod_data_source_block           ja54
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7024280