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_4315763
_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            'C31 H47 Ge N3'
_chemical_formula_weight         534.31
_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                66.98(3)
_cell_angle_beta                 80.50(3)
_cell_angle_gamma                72.40(3)
_cell_formula_units_Z            2
_cell_length_a                   10.453(2)
_cell_length_b                   12.286(3)
_cell_length_c                   13.016(3)
_cell_measurement_reflns_used    13048
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      54.0
_cell_measurement_theta_min      3.4
_cell_volume                     1464.4(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13048
_diffrn_reflns_theta_full        27.02
_diffrn_reflns_theta_max         27.02
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    1.069
_exptl_absorpt_correction_T_max  0.9178
_exptl_absorpt_correction_T_min  0.7922
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         6309
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0335
_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^)+(0.0317P)^2^+0.4886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0657
_reflns_number_gt                5701
_reflns_number_total             6309
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1003808_si_001_1.cif
_cod_data_source_block           ja46
_cod_original_cell_volume        1464.4(6)
_cod_database_code               4315763