#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:32:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179250 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/70/4317004.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4317004
loop_
_publ_author_name
'Anukul Jana'
'Herbert W. Roesky'
'Carola Schulzke'
'Prinson P. Samuel'
'Alexander Döring'
_publ_section_title
;
 Correction to Synthesis and Reaction of Monomeric Germanium(II) and
 Lead(II) Dimethylamide and the Synthesis of Germanium(II) Hydrazide by
 Cleavage of One N-H Bond of Hydrazine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10208
_journal_page_last               10209
_journal_paper_doi               10.1021/ic101845t
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C29 H43.31 Cl0.23 Ge N3.54'
_chemical_formula_weight         522.29
_chemical_name_systematic
;
 ?
;
_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=20
_cell_volume                     1397.8(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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    1.140
_exptl_absorpt_correction_T_max  0.9758
_exptl_absorpt_correction_T_min  0.8214=20
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.241
_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         0.916
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6002
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0410
_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/[σ²(Fo²)+(0.0593P)²+0.4676P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1024
_reflns_number_gt                5142
_reflns_number_total             6002
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic101845t_si_001.cif
_cod_data_source_block           ja56
_cod_original_cell_volume        1397.8(5)
_cod_database_code               4317004
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.51167(3) 0.44745(2) 0.278760(18) 0.02774(9) Uani 1 1 d . . .
Cl1 Cl 0.6044(4) 0.3964(3) 0.1389(3) 0.0421(6) Uani 0.23 1 d P A 2
N1 N 0.6242(4) 0.4135(3) 0.1914(3) 0.0421(6) Uani 0.77 1 d P A 1
N2 N 0.5779(5) 0.3937(4) 0.0955(3) 0.0421(6) Uani 0.77 1 d P A 1
N3 N 0.4343(2) 0.57952(16) 0.22851(12) 0.0226(4) Uani 1 1 d . A .
N4 N 0.2859(2) 0.32590(16) 0.22427(13) 0.0241(4) Uani 1 1 d . A .
C1 C 0.5312(3) 0.70317(19) 0.27374(15) 0.0250(4) Uani 1 1 d . . .
C2 C 0.6620(3) 0.7705(2) 0.23760(16) 0.0278(5) Uani 1 1 d . A .
C3 C 0.7548(3) 0.8881(2) 0.28522(18) 0.0349(5) Uani 1 1 d . . .
H3 H 0.8451 0.9344 0.2625 0.042 Uiso 1 1 calc R A .
C4 C 0.7170(4) 0.9374(2) 0.36445(19) 0.0403(6) Uani 1 1 d . A .
H4 H 0.7796 1.0178 0.3952 0.048 Uiso 1 1 calc R . .
C5 C 0.5883(4) 0.8702(2) 0.39935(17) 0.0360(5) Uani 1 1 d . . .
H5 H 0.5630 0.9054 0.4538 0.043 Uiso 1 1 calc R A .
C6 C 0.4948(3) 0.7515(2) 0.35592(16) 0.0281(5) Uani 1 1 d . A .
C7 C 0.7093(3) 0.7220(2) 0.15032(17) 0.0306(5) Uani 1 1 d . . .
H7 H 0.6218 0.6437 0.1204 0.037 Uiso 1 1 calc R A .
C8 C 0.8726(3) 0.6943(3) 0.1707(2) 0.0445(6) Uani 1 1 d . A .
H8A H 0.9004 0.6632 0.1134 0.067 Uiso 1 1 calc R . .
H8B H 0.8628 0.6324 0.2100 0.067 Uiso 1 1 calc R . .
H8C H 0.9597 0.7694 0.2018 0.067 Uiso 1 1 calc R . .
C9 C 0.7198(4) 0.8115(3) 0.0832(2) 0.0437(6) Uani 1 1 d . A .
H9A H 0.7500 0.7770 0.0277 0.066 Uiso 1 1 calc R . .
H9B H 0.8036 0.8896 0.1115 0.066 Uiso 1 1 calc R . .
H9C H 0.6125 0.8253 0.0673 0.066 Uiso 1 1 calc R . .
C10 C 0.3587(3) 0.6777(2) 0.39871(17) 0.0312(5) Uani 1 1 d . . .
H10 H 0.3668 0.5925 0.3931 0.037 Uiso 1 1 calc R A .
C11 C 0.3819(4) 0.7277(3) 0.5013(2) 0.0519(8) Uani 1 1 d . A .
H11A H 0.4927 0.7324 0.5322 0.078 Uiso 1 1 calc R . .
H11B H 0.2994 0.6729 0.5276 0.078 Uiso 1 1 calc R . .
H11C H 0.3684 0.8096 0.5094 0.078 Uiso 1 1 calc R . .
C12 C 0.1889(4) 0.6686(3) 0.3492(2) 0.0471(7) Uani 1 1 d . A .
H12A H 0.1058 0.6206 0.3790 0.071 Uiso 1 1 calc R . .
H12B H 0.1725 0.6284 0.2856 0.071 Uiso 1 1 calc R . .
H12C H 0.1780 0.7510 0.3507 0.071 Uiso 1 1 calc R . .
C13 C 0.2842(3) 0.6679(2) 0.11657(17) 0.0319(5) Uani 1 1 d . A .
H13A H 0.3121 0.7400 0.1649 0.048 Uiso 1 1 calc R . .
H13B H 0.1683 0.6476 0.0865 0.048 Uiso 1 1 calc R . .
H13C H 0.3548 0.6856 0.0716 0.048 Uiso 1 1 calc R . .
C14 C 0.3108(3) 0.5609(2) 0.15764(15) 0.0253(4) Uani 1 1 d . . .
C15 C 0.1985(3) 0.4454(2) 0.11961(16) 0.0280(5) Uani 1 1 d . A .
H15 H 0.1283 0.4396 0.0630 0.034 Uiso 1 1 calc R . .
C16 C 0.1779(3) 0.3377(2) 0.15561(15) 0.0261(4) Uani 1 1 d . . .
C17 C 0.0227(3) 0.2332(2) 0.11421(18) 0.0355(5) Uani 1 1 d . A .
H17A H 0.0453 0.1785 0.0658 0.053 Uiso 1 1 calc R . .
H17B H -0.0641 0.2660 0.0884 0.053 Uiso 1 1 calc R . .
H17C H -0.0139 0.1873 0.1616 0.053 Uiso 1 1 calc R . .
C18 C 0.2486(3) 0.22043(19) 0.26889(15) 0.0245(4) Uani 1 1 d . . .
C19 C 0.2913(3) 0.1156(2) 0.23697(15) 0.0268(4) Uani 1 1 d . A .
C20 C 0.2638(3) 0.0197(2) 0.28642(17) 0.0344(5) Uani 1 1 d . . .
H20 H 0.2937 -0.0512 0.2668 0.041 Uiso 1 1 calc R A .
C21 C 0.1945(4) 0.0258(2) 0.36301(18) 0.0406(6) Uani 1 1 d . A .
H21 H 0.1757 -0.0407 0.3952 0.049 Uiso 1 1 calc R . .
C22 C 0.1525(3) 0.1294(2) 0.39266(18) 0.0381(6) Uani 1 1 d . . .
H22 H 0.1042 0.1330 0.4453 0.046 Uiso 1 1 calc R A .
C23 C 0.1791(3) 0.2278(2) 0.34735(16) 0.0304(5) Uani 1 1 d . A .
C24 C 0.3638(3) 0.1021(2) 0.15183(17) 0.0314(5) Uani 1 1 d . . .
H24 H 0.3720 0.1777 0.1248 0.038 Uiso 1 1 calc R A .
C25 C 0.5372(4) 0.0906(3) 0.1750(2) 0.0480(7) Uani 1 1 d . A .
H25A H 0.5813 0.0823 0.1189 0.072 Uiso 1 1 calc R . .
H25B H 0.5326 0.0182 0.2031 0.072 Uiso 1 1 calc R . .
H25C H 0.6089 0.1640 0.2176 0.072 Uiso 1 1 calc R . .
C26 C 0.2518(4) -0.0080(2) 0.08044(18) 0.0419(6) Uani 1 1 d . A .
H26A H 0.3009 -0.0144 0.0261 0.063 Uiso 1 1 calc R . .
H26B H 0.1431 0.0032 0.0636 0.063 Uiso 1 1 calc R . .
H26C H 0.2398 -0.0831 0.1060 0.063 Uiso 1 1 calc R . .
C27 C 0.1310(3) 0.3403(2) 0.38222(19) 0.0373(6) Uani 1 1 d . . .
H27 H 0.1919 0.4093 0.3546 0.045 Uiso 1 1 calc R A .
C28 C -0.0519(4) 0.3201(3) 0.3500(3) 0.0643(10) Uani 1 1 d . A .
H28A H -0.0807 0.2946 0.2834 0.096 Uiso 1 1 calc R . .
H28B H -0.0774 0.3966 0.3670 0.096 Uiso 1 1 calc R . .
H28C H -0.1157 0.2562 0.3786 0.096 Uiso 1 1 calc R . .
C29 C 0.1800(6) 0.3795(4) 0.4840(3) 0.0832(14) Uani 1 1 d . A .
H29A H 0.1466 0.4520 0.5025 0.125 Uiso 1 1 calc R . .
H29B H 0.2999 0.3992 0.5024 0.125 Uiso 1 1 calc R . .
H29C H 0.1254 0.3128 0.5134 0.125 Uiso 1 1 calc R . .
H1 H 0.713(5) 0.381(4) 0.218(3) 0.0441(12) Uiso 0.77 1 d P B 1
H2A H 0.591(5) 0.473(3) 0.072(3) 0.0441(12) Uiso 0.77 1 d PD C 1
H2B H 0.471(5) 0.363(3) 0.073(3) 0.0441(12) Uiso 0.77 1 d PD D 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 N3 98.42(13) . . ?
N1 Ge1 N4 99.87(13) . . ?
N3 Ge1 N4 89.17(8) . . ?
N1 Ge1 Cl1 12.90(14) . . ?
N3 Ge1 Cl1 90.57(10) . . ?
N4 Ge1 Cl1 89.58(11) . . ?
N2 N1 Ge1 129.9(3) . . ?
C14 N3 C1 120.57(18) . . ?
C14 N3 Ge1 125.43(15) . . ?
C1 N3 Ge1 113.94(14) . . ?
C16 N4 C18 121.14(18) . . ?
C16 N4 Ge1 125.90(16) . . ?
C18 N4 Ge1 112.96(14) . . ?
C2 C1 C6 121.1(2) . . ?
C2 C1 N3 120.5(2) . . ?
C6 C1 N3 118.4(2) . . ?
C3 C2 C1 118.3(2) . . ?
C3 C2 C7 118.3(2) . . ?
C1 C2 C7 123.4(2) . . ?
C4 C3 C2 121.0(2) . . ?
C3 C4 C5 120.2(2) . . ?
C4 C5 C6 121.1(2) . . ?
C5 C6 C1 118.3(2) . . ?
C5 C6 C10 119.7(2) . . ?
C1 C6 C10 121.9(2) . . ?
C2 C7 C8 111.1(2) . . ?
C2 C7 C9 111.8(2) . . ?
C8 C7 C9 109.7(2) . . ?
C12 C10 C6 112.4(2) . . ?
C12 C10 C11 110.9(2) . . ?
C6 C10 C11 112.0(2) . . ?
N3 C14 C15 123.2(2) . . ?
N3 C14 C13 120.0(2) . . ?
C15 C14 C13 116.7(2) . . ?
C16 C15 C14 127.3(2) . . ?
N4 C16 C15 122.8(2) . . ?
N4 C16 C17 120.3(2) . . ?
C15 C16 C17 116.8(2) . . ?
C23 C18 C19 121.0(2) . . ?
C23 C18 N4 118.8(2) . . ?
C19 C18 N4 120.0(2) . . ?
C20 C19 C18 117.9(2) . . ?
C20 C19 C24 119.0(2) . . ?
C18 C19 C24 123.1(2) . . ?
C21 C20 C19 121.5(2) . . ?
C20 C21 C22 119.6(2) . . ?
C23 C22 C21 121.5(2) . . ?
C22 C23 C18 118.6(2) . . ?
C22 C23 C27 119.9(2) . . ?
C18 C23 C27 121.6(2) . . ?
C19 C24 C25 111.1(2) . . ?
C19 C24 C26 111.1(2) . . ?
C25 C24 C26 110.5(2) . . ?
C29 C27 C28 111.1(3) . . ?
C29 C27 C23 112.9(3) . . ?
C28 C27 C23 111.0(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.812(4) . ?
Ge1 N3 2.0144(18) . ?
Ge1 N4 2.030(2) . ?
Ge1 Cl1 2.422(4) . ?
N1 N2 1.410(5) . ?
N3 C14 1.337(3) . ?
N3 C1 1.453(3) . ?
N4 C16 1.330(3) . ?
N4 C18 1.448(3) . ?
C1 C2 1.404(3) . ?
C1 C6 1.406(3) . ?
C2 C3 1.402(3) . ?
C2 C7 1.518(3) . ?
C3 C4 1.378(4) . ?
C4 C5 1.380(4) . ?
C5 C6 1.397(3) . ?
C6 C10 1.525(3) . ?
C7 C8 1.523(3) . ?
C7 C9 1.531(4) . ?
C10 C12 1.506(4) . ?
C10 C11 1.540(4) . ?
C13 C14 1.509(3) . ?
C14 C15 1.399(3) . ?
C15 C16 1.399(3) . ?
C16 C17 1.512(3) . ?
C18 C23 1.405(3) . ?
C18 C19 1.408(3) . ?
C19 C20 1.400(3) . ?
C19 C24 1.516(3) . ?
C20 C21 1.378(4) . ?
C21 C22 1.384(4) . ?
C22 C23 1.384(4) . ?
C23 C27 1.525(3) . ?
C24 C25 1.527(4) . ?
C24 C26 1.534(4) . ?
C27 C29 1.500(4) . ?
C27 C28 1.518(4) . ?
