Synthesis and Reaction of Monomeric Germanium(II) and Lead(II) Dimethylamide and the Synthesis of Germanium(II) Hydrazide by Clevage of one N-H bond of Hydrazine
Anukul Jana; Herbert W. Roesky; Carola Schulzke; Prinson P. Samuel; Alexander Döring; Inorganic Chemistry 49 (2010) 5554–5559; doi:10.1021/ic1003808

data_4315765
_publ_section_title
;
 Synthesis and Reaction of Monomeric Germanium(II) and Lead(II)
 Dimethylamide and the Synthesis of Germanium(II) Hydrazide by Clevage of
 one N-H bond of Hydrazine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5554
_journal_page_last               5559
_journal_paper_doi               10.1021/ic1003808
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C29 H44 Ge N4'
_chemical_formula_weight         521.27
_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                97.44(3)
_cell_angle_beta                 98.64(3)
_cell_angle_gamma                106.20(3)
_cell_formula_units_Z            2
_cell_length_a                   8.6062(17)
_cell_length_b                   11.553(2)
_cell_length_c                   15.055(3)
_cell_measurement_reflns_used    12150
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      54.1
_cell_measurement_theta_min      3.7
_cell_volume                     1397.8(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0376
_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       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12150
_diffrn_reflns_theta_full        27.04
_diffrn_reflns_theta_max         27.04
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    1.119
_exptl_absorpt_correction_T_max  0.9758
_exptl_absorpt_correction_T_min  0.8214
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         6002
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.7006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1051
_reflns_number_gt                5142
_reflns_number_total             6002
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1003808_si_001_3.cif
_cod_data_source_block           ja56
_cod_original_cell_volume        1397.8(5)
_cod_database_code               4315765