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#$Date: 2025-08-21 14:21:36 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301847 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/15/7011555.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_7011555
loop_
_publ_author_name
'Mitzel, Norbert W.'
'Vojinović, Krunoslav'
_publ_section_title
;
 (4+4)-Coordinate germanium atoms in tetrakis(dialkylaminoxy)germanes
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2341
_journal_paper_doi               10.1039/b201472f
_journal_year                    2002
_chemical_formula_sum            'C8 H24 Ge N4 O4'
_chemical_formula_weight         313.08
_chemical_name_systematic
; 
Tetrakis(N,N-dimethylaminoxy)germane
;
_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                96.516(3)
_cell_angle_beta                 96.585(2)
_cell_angle_gamma                91.3672(16)
_cell_formula_units_Z            2
_cell_length_a                   8.9412(4)
_cell_length_b                   9.1281(4)
_cell_length_c                   9.2285(4)
_cell_measurement_reflns_used    31651
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      27.31
_cell_measurement_theta_min      2.98
_cell_volume                     742.87(6)
_computing_cell_refinement       SCALEPACK
_computing_data_collection       'Nonius-DIP 2020 Software'
_computing_data_reduction        'SCALEPACK, DIPSHEL'
_computing_molecular_graphics    'SHELXTL 5.01'
_computing_publication_material  'SHELXTL 5.01'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_detector_area_resol_mean '8 - 0.78'
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'Nonius DIP 2020'
_diffrn_measurement_method       'phi scans 2.0°'
_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  0.0880
_diffrn_reflns_av_sigmaI/netI    0.0742
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            31651
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         2.98
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.072
_exptl_absorpt_correction_type   'Intensity corrections by SCALEPACK'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.244
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3104
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0779
_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/[σ²(Fo²)+(0.0329P)²+6.8542P] where P==(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1754
_refine_ls_wR_factor_ref         0.1838
_reflns_number_gt                2783
_reflns_number_total             3104
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b201472f.txt
_cod_data_source_block           kruno8
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

2018-01-21
Z value changed to be consistent with given formula
                 miguel
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_units_Z    4
_cod_database_code               7011555
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
Ge Ge 0.32435(8) 0.30437(8) -0.34528(8) 0.0213(2) Uani 1 1 d . . .
O1 O 0.2798(5) 0.4853(5) -0.2817(5) 0.0270(10) Uani 1 1 d . . .
O2 O 0.5189(5) 0.2861(5) -0.3010(6) 0.0292(11) Uani 1 1 d . . .
O3 O 0.2193(6) 0.1629(6) -0.2822(5) 0.0336(12) Uani 1 1 d . . .
O4 O 0.2798(5) 0.2769(5) -0.5382(5) 0.0243(10) Uani 1 1 d . . .
N1 N 0.3746(6) 0.5231(6) -0.1405(6) 0.0247(12) Uani 1 1 d . . .
N2 N 0.5440(6) 0.1423(6) -0.3847(6) 0.0256(12) Uani 1 1 d . . .
N3 N 0.1222(6) 0.3229(6) -0.5533(6) 0.0253(12) Uani 1 1 d . . .
N4 N 0.1936(7) 0.2079(7) -0.1304(6) 0.0283(13) Uani 1 1 d . . .
C1 C 0.4814(9) 0.6379(9) -0.1648(9) 0.0368(18) Uani 1 1 d . . .
H1A H 0.556(5) 0.665(4) -0.070(5) 0.05(3) Uiso 1 1 calc R . .
H1B H 0.424(3) 0.730(5) -0.191(6) 0.05(3) Uiso 1 1 calc R . .
H1C H 0.541(5) 0.600(3) -0.251(5) 0.03(2) Uiso 1 1 calc R . .
C2 C 0.2744(9) 0.5829(9) -0.0399(9) 0.0346(17) Uani 1 1 d . . .
H2A H 0.329(3) 0.617(5) 0.048(4) 0.03(2) Uiso 1 1 calc R . .
H2B H 0.207(5) 0.511(4) -0.026(4) 0.07(3) Uiso 1 1 calc R . .
H2C H 0.224(5) 0.659(5) -0.078(3) 0.016(17) Uiso 1 1 calc R . .
C3 C 0.6002(8) 0.0492(8) -0.2750(9) 0.0329(17) Uani 1 1 d . . .
H3A H 0.519(5) 0.023(6) -0.221(6) 0.06(3) Uiso 1 1 calc R . .
H3B H 0.680(6) 0.102(4) -0.208(5) 0.08(4) Uiso 1 1 calc R . .
H3C H 0.639(7) -0.039(6) -0.323(3) 0.07(3) Uiso 1 1 calc R . .
C4 C 0.6610(9) 0.1743(8) -0.4743(8) 0.0330(16) Uani 1 1 d . . .
H4A H 0.684(4) 0.082(4) -0.535(5) 0.05(3) Uiso 1 1 calc R . .
H4B H 0.753(5) 0.213(5) -0.410(3) 0.03(2) Uiso 1 1 calc R . .
H4C H 0.626(3) 0.249(5) -0.539(5) 0.03(2) Uiso 1 1 calc R . .
C5 C 0.0337(9) 0.1938(10) -0.6258(9) 0.0389(19) Uani 1 1 d . . .
H5A H -0.075(5) 0.222(2) -0.651(5) 0.07(3) Uiso 1 1 calc R . .
H5B H 0.037(5) 0.113(4) -0.557(4) 0.05(2) Uiso 1 1 calc R . .
H5C H 0.078(4) 0.155(4) -0.720(5) 0.03(2) Uiso 1 1 calc R . .
C6 C 0.1192(9) 0.4406(9) -0.6465(9) 0.0392(19) Uani 1 1 d . . .
H6A H 0.187(6) 0.526(5) -0.596(3) 0.05(3) Uiso 1 1 calc R . .
H6B H 0.012(5) 0.475(4) -0.665(5) 0.07(3) Uiso 1 1 calc R . .
H6C H 0.156(6) 0.403(2) -0.743(5) 0.03(2) Uiso 1 1 calc R . .
C7 C 0.0347(9) 0.2244(11) -0.1356(12) 0.049(2) Uani 1 1 d . . .
H7A H 0.010(2) 0.251(7) -0.039(6) 0.06(3) Uiso 1 1 calc R . .
H7B H -0.016(3) 0.134(6) -0.175(7) 0.09(4) Uiso 1 1 calc R . .
H7C H 0.005(2) 0.299(7) -0.196(7) 0.07(3) Uiso 1 1 calc R . .
C8 C 0.2357(9) 0.0812(10) -0.0535(9) 0.0373(18) Uani 1 1 d . . .
H8A H 0.228(5) 0.105(2) 0.051(5) 0.04(2) Uiso 1 1 calc R . .
H8B H 0.339(5) 0.057(3) -0.067(4) 0.020(18) Uiso 1 1 calc R . .
H8C H 0.168(4) -0.003(4) -0.093(4) 0.05(3) Uiso 1 1 calc R . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
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
O2 Ge O1 108.1(2) . . ?
O2 Ge O4 109.1(2) . . ?
O1 Ge O4 108.6(2) . . ?
O2 Ge O3 111.4(2) . . ?
O1 Ge O3 115.2(2) . . ?
O4 Ge O3 104.2(2) . . ?
N1 O1 Ge 105.7(3) . . ?
N2 O2 Ge 102.0(3) . . ?
N4 O3 Ge 109.2(4) . . ?
N3 O4 Ge 100.8(3) . . ?
C2 N1 C1 109.7(6) . . ?
C2 N1 O1 105.4(5) . . ?
C1 N1 O1 105.8(5) . . ?
C4 N2 C3 110.3(6) . . ?
C4 N2 O2 104.5(5) . . ?
C3 N2 O2 105.2(5) . . ?
C6 N3 C5 111.2(6) . . ?
C6 N3 O4 105.3(5) . . ?
C5 N3 O4 105.5(5) . . ?
C7 N4 C8 109.2(6) . . ?
C7 N4 O3 105.1(6) . . ?
C8 N4 O3 104.5(6) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N4 C8 H8A 109.5 . . ?
N4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
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
Ge O2 1.757(5) . ?
Ge O1 1.759(5) . ?
Ge O4 1.767(4) . ?
Ge O3 1.768(5) . ?
O1 N1 1.471(7) . ?
O2 N2 1.481(7) . ?
O3 N4 1.459(8) . ?
O4 N3 1.476(7) . ?
N1 C2 1.436(9) . ?
N1 C1 1.454(9) . ?
N2 C4 1.449(9) . ?
N2 C3 1.449(9) . ?
N3 C6 1.449(9) . ?
N3 C5 1.456(10) . ?
N4 C7 1.428(10) . ?
N4 C8 1.459(9) . ?
C1 H1A 1.0385 . ?
C1 H1B 1.0385 . ?
C1 H1C 1.0385 . ?
C2 H2A 0.9163 . ?
C2 H2B 0.9163 . ?
C2 H2C 0.9163 . ?
C3 H3A 0.9640 . ?
C3 H3B 0.9640 . ?
C3 H3C 0.9640 . ?
C4 H4A 0.9939 . ?
C4 H4B 0.9939 . ?
C4 H4C 0.9939 . ?
C5 H5A 1.0230 . ?
C5 H5B 1.0230 . ?
C5 H5C 1.0230 . ?
C6 H6A 1.0132 . ?
C6 H6B 1.0132 . ?
C6 H6C 1.0132 . ?
C7 H7A 0.9492 . ?
C7 H7B 0.9492 . ?
C7 H7C 0.9492 . ?
C8 H8A 0.9748 . ?
C8 H8B 0.9748 . ?
C8 H8C 0.9748 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Ge O1 N1 -37.9(4) . . . . ?
O4 Ge O1 N1 -156.2(3) . . . . ?
O3 Ge O1 N1 87.4(4) . . . . ?
O1 Ge O2 N2 -169.5(3) . . . . ?
O4 Ge O2 N2 -51.5(4) . . . . ?
O3 Ge O2 N2 63.0(4) . . . . ?
O2 Ge O3 N4 86.7(4) . . . . ?
O1 Ge O3 N4 -37.0(5) . . . . ?
O4 Ge O3 N4 -155.8(4) . . . . ?
O2 Ge O4 N3 -170.1(3) . . . . ?
O1 Ge O4 N3 -52.4(4) . . . . ?
O3 Ge O4 N3 70.8(4) . . . . ?
Ge O1 N1 C2 -131.5(5) . . . . ?
Ge O1 N1 C1 112.3(5) . . . . ?
Ge O2 N2 C4 124.9(4) . . . . ?
Ge O2 N2 C3 -118.9(5) . . . . ?
Ge O4 N3 C6 122.5(5) . . . . ?
Ge O4 N3 C5 -119.7(5) . . . . ?
Ge O3 N4 C7 113.8(5) . . . . ?
Ge O3 N4 C8 -131.3(5) . . . . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139154651
