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_4315764
_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 N3 Pb'
_chemical_formula_weight         668.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 99.12(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9507(18)
_cell_length_b                   22.604(5)
_cell_length_c                   14.904(3)
_cell_measurement_reflns_used    48574
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      51.8
_cell_measurement_theta_min      2.8
_cell_volume                     2977.3(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1014
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12107
_diffrn_reflns_theta_full        25.92
_diffrn_reflns_theta_max         25.92
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    5.689
_exptl_absorpt_correction_T_max  0.2704
_exptl_absorpt_correction_T_min  0.0711
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         9.439
_refine_diff_density_min         -4.106
_refine_diff_density_rms         0.366
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0667
_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^)+(0.1181P)^2^+35.2464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.1766
_reflns_number_gt                2851
_reflns_number_total             2956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1003808_si_001_2.cif
_cod_data_source_block           ja45
_cod_original_cell_volume        2977.2(10)
_cod_database_code               4315764