#------------------------------------------------------------------------------
#$Date: 2025-08-22 10:56:18 +0200 (Fri 22 de Aug de 2025) $
#$Revision: 301860 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/41/7124165.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_7124165
loop_
_publ_author_name
'Mayer, Kerstin'
'Klein, Wilhelm'
'Fässler, Thomas F'
_publ_section_title
;
 Zinc as a Versatile Connecting Atom for Zintl Cluster Oligomers
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC06388A
_journal_year                    2019
_chemical_formula_moiety         'Ge9 H18 N6 Zn2, 11(H3 N)'
_chemical_formula_sum            'Ge9 H51 N17 Zn2'
_chemical_formula_weight         1073.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-08-12 deposited with the CCDC.    2019-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.42(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.355(2)
_cell_length_b                   17.830(4)
_cell_length_c                   10.478(2)
_cell_measurement_reflns_used    15925
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      63.11
_cell_measurement_theta_min      2.05
_cell_volume                     1775.2(7)
_computing_cell_refinement       'STOE X-AREA 1.76'
_computing_data_collection       'STOE X-AREA 1.76'
_computing_data_reduction        'STOE X-AREA 1.76'
_computing_molecular_graphics    'DIAMOND 3.2k'
_computing_structure_refinement  SHELXL-2014/7
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15020
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.284
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    8.845
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'STOE X-AREA 1.76'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.009
_exptl_crystal_description       block
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         3595
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0704P)²+8.1196P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1624
_refine_ls_wR_factor_ref         0.1751
_reflns_number_gt                2901
_reflns_number_total             3595
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc06388a2.cif
_cod_data_source_block           KM-442
_cod_database_code               7124165
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ge1 Ge -0.03502(16) 0.2500 0.15829(16) 0.0809(4) Uani 1 2 d S T P
Ge2 Ge 0.18531(11) 0.16508(7) 0.21891(11) 0.0773(3) Uani 1 1 d . . .
Ge3 Ge 0.03776(11) 0.16642(6) 0.37886(11) 0.0767(3) Uani 1 1 d . . .
Ge4 Ge 0.19867(16) 0.2500 0.58000(15) 0.0763(4) Uani 1 2 d S T P
Ge5 Ge 0.31217(11) 0.14707(6) 0.49065(11) 0.0778(3) Uani 1 1 d . . .
Ge6 Ge 0.39138(15) 0.2500 0.36911(16) 0.0761(4) Uani 1 2 d S T P
Zn1 Zn 0.60406(16) 0.2500 0.32509(16) 0.0737(4) Uani 1 2 d S T P
N1 N 0.7835(12) 0.2500 0.5132(12) 0.088(3) Uani 1 2 d S T P
H1A H 0.7564 0.2500 0.5859 0.133 Uiso 1 2 d R U P
H1B H 0.8358 0.2083 0.5176 0.133 Uiso 1 1 d R U .
N2 N 0.6450(8) 0.1592(5) 0.2257(8) 0.078(2) Uani 1 1 d . . .
H2A H 0.6048 0.1666 0.1321 0.117 Uiso 1 1 calc R U .
H2B H 0.6085 0.1170 0.2475 0.117 Uiso 1 1 calc R U .
H2C H 0.7396 0.1538 0.2536 0.117 Uiso 1 1 calc R U .
Zn2 Zn 0.14384(17) 0.2500 0.78609(16) 0.0755(4) Uani 1 2 d S T P
N3 N 0.3283(13) 0.2500 0.9620(11) 0.087(3) Uani 1 2 d S T P
H3A H 0.4028 0.2500 0.9368 0.130 Uiso 1 2 d R U P
H3B H 0.3319 0.2083 1.0135 0.130 Uiso 1 1 d R U .
N4 N 0.0435(10) 0.1590(5) 0.8273(8) 0.094(3) Uani 1 1 d . . .
H4A H 0.0915 0.1164 0.8264 0.141 Uiso 1 1 calc R U .
H4B H -0.0457 0.1558 0.7612 0.141 Uiso 1 1 calc R U .
H4C H 0.0406 0.1647 0.9124 0.141 Uiso 1 1 calc R U .
N5 N 0.5027(9) 0.0285(5) 0.3032(9) 0.092(2) Uani 1 1 d . . .
H5A H 0.5692 -0.0020 0.3639 0.138 Uiso 1 1 calc R U .
H5B H 0.4505 0.0023 0.2253 0.138 Uiso 1 1 calc R U .
H5C H 0.4456 0.0462 0.3438 0.138 Uiso 1 1 calc R U .
N6 N 0.7721(15) 0.0770(9) 0.6189(15) 0.157(5) Uani 1 1 d . U .
H6A H 0.7668 0.0303 0.6518 0.235 Uiso 1 1 calc R U .
H6B H 0.7767 0.0730 0.5343 0.235 Uiso 1 1 calc R U .
H6C H 0.6944 0.1038 0.6106 0.235 Uiso 1 1 calc R U .
N7 N 0.1561(12) 0.0249(6) 0.6988(10) 0.112(3) Uani 1 1 d . . .
H7A H 0.1756 -0.0154 0.7566 0.169 Uiso 1 1 calc R U .
H7B H 0.2357 0.0396 0.6887 0.169 Uiso 1 1 calc R U .
H7C H 0.0892 0.0122 0.6142 0.169 Uiso 1 1 calc R U .
N8 N 0.4850(14) 0.1171(7) 0.9101(13) 0.137(4) Uani 1 1 d . U .
H8A H 0.4210 0.0805 0.9024 0.205 Uiso 1 1 d R U .
H8B H 0.5710 0.0959 0.9309 0.205 Uiso 1 1 d R U .
H8C H 0.4582 0.1423 0.8281 0.205 Uiso 1 1 d R U .
N9 N 0.7990(10) 0.0406(6) -0.0217(11) 0.114(3) Uani 1 1 d . . .
H9A H 0.7664 0.0126 -0.1009 0.171 Uiso 1 1 d R U .
H9B H 0.8528 0.0114 0.0513 0.171 Uiso 1 1 d R U .
H9C H 0.8518 0.0792 -0.0315 0.171 Uiso 1 1 d R U .
N10 N 0.700(3) 0.2500 0.762(3) 0.189(10) Uani 1 2 d S TU P
H10A H 0.7789 0.2500 0.8424 0.283 Uiso 1 2 d R U P
H10B H 0.6484 0.2083 0.7612 0.283 Uiso 1 1 d R U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 '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'
Zn Zn 0.2839 1.4301 '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
Ge3 Ge1 Ge3 70.03(6) 4_565 .
Ge3 Ge1 Ge2 62.10(5) 4_565 4_565
Ge3 Ge1 Ge2 101.59(7) . 4_565
Ge3 Ge1 Ge2 101.58(7) 4_565 .
Ge3 Ge1 Ge2 62.10(5) . .
Ge2 Ge1 Ge2 71.30(7) 4_565 .
Ge6 Ge2 Ge1 103.90(5) . .
Ge6 Ge2 Ge5 58.45(5) . .
Ge1 Ge2 Ge5 110.30(6) . .
Ge6 Ge2 Ge3 98.76(5) . .
Ge1 Ge2 Ge3 58.94(5) . .
Ge5 Ge2 Ge3 59.29(4) . .
Ge4 Ge3 Ge1 105.09(5) . .
Ge4 Ge3 Ge5 58.60(5) . .
Ge1 Ge3 Ge5 110.58(6) . .
Ge4 Ge3 Ge2 99.93(5) . .
Ge1 Ge3 Ge2 58.96(5) . .
Ge5 Ge3 Ge2 59.59(4) . .
Zn2 Ge4 Ge5 128.90(4) . 4_565
Zn2 Ge4 Ge5 128.90(4) . .
Ge5 Ge4 Ge5 92.08(7) 4_565 .
Zn2 Ge4 Ge3 114.90(6) . 4_565
Ge5 Ge4 Ge3 61.72(4) 4_565 4_565
Ge5 Ge4 Ge3 111.00(6) . 4_565
Zn2 Ge4 Ge3 114.90(6) . .
Ge5 Ge4 Ge3 111.00(6) 4_565 .
Ge5 Ge4 Ge3 61.72(4) . .
Ge3 Ge4 Ge3 70.62(7) 4_565 .
Ge6 Ge5 Ge4 87.25(5) . .
Ge6 Ge5 Ge3 100.85(6) . .
Ge4 Ge5 Ge3 59.67(5) . .
Ge6 Ge5 Ge2 59.61(5) . .
Ge4 Ge5 Ge2 101.78(6) . .
Ge3 Ge5 Ge2 61.13(5) . .
Zn1 Ge6 Ge5 126.34(5) . .
Zn1 Ge6 Ge5 126.34(5) . 4_565
Ge5 Ge6 Ge5 92.15(7) . 4_565
Zn1 Ge6 Ge2 118.55(6) . 4_565
Ge5 Ge6 Ge2 112.03(6) . 4_565
Ge5 Ge6 Ge2 61.94(4) 4_565 4_565
Zn1 Ge6 Ge2 118.55(6) . .
Ge5 Ge6 Ge2 61.94(4) . .
Ge5 Ge6 Ge2 112.03(6) 4_565 .
Ge2 Ge6 Ge2 71.89(7) 4_565 .
N2 Zn1 N2 103.8(5) . 4_565
N2 Zn1 N1 101.0(3) . .
N2 Zn1 N1 101.0(3) 4_565 .
N2 Zn1 Ge6 118.8(2) . .
N2 Zn1 Ge6 118.8(2) 4_565 .
N1 Zn1 Ge6 110.6(3) . .
Zn1 N1 H1A 109.5 . .
Zn1 N1 H1B 109.5 . .
H1A N1 H1B 109.5 . .
Zn1 N2 N5 104.4(3) . .
Zn1 N2 H2A 109.5 . .
N5 N2 H2A 109.8 . .
Zn1 N2 H2B 109.5 . .
N5 N2 H2B 5.6 . .
H2A N2 H2B 109.5 . .
Zn1 N2 H2C 109.5 . .
N5 N2 H2C 114.1 . .
H2A N2 H2C 109.5 . .
H2B N2 H2C 109.5 . .
N3 Zn2 N4 100.2(3) . 4_565
N3 Zn2 N4 100.2(3) . .
N4 Zn2 N4 103.7(6) 4_565 .
N3 Zn2 Ge4 109.4(3) . .
N4 Zn2 Ge4 119.9(3) 4_565 .
N4 Zn2 Ge4 119.9(3) . .
Zn2 N3 H3A 109.4 . .
Zn2 N3 H3B 109.6 . .
H3A N3 H3B 109.4 . .
Zn2 N4 N7 101.7(4) . .
Zn2 N4 H4A 109.5 . .
N7 N4 H4A 22.4 . .
Zn2 N4 H4B 109.5 . .
N7 N4 H4B 93.6 . .
H4A N4 H4B 109.5 . .
Zn2 N4 H4C 109.5 . .
N7 N4 H4C 131.2 . .
H4A N4 H4C 109.5 . .
H4B N4 H4C 109.5 . .
N2 N5 H5A 109.5 . .
N2 N5 H5B 109.5 . .
H5A N5 H5B 109.5 . .
N2 N5 H5C 109.5 . .
H5A N5 H5C 109.5 . .
H5B N5 H5C 109.5 . .
N4 N6 H6A 109.5 1_655 .
N4 N6 H6B 109.5 1_655 .
H6A N6 H6B 109.5 . .
N4 N6 H6C 109.5 1_655 .
H6A N6 H6C 109.5 . .
H6B N6 H6C 109.5 . .
N4 N7 H7A 109.5 . .
N4 N7 H7B 109.5 . .
H7A N7 H7B 109.5 . .
N4 N7 H7C 109.5 . .
H7A N7 H7C 109.5 . .
H7B N7 H7C 109.5 . .
H8A N8 H8B 109.5 . .
H8A N8 H8C 109.5 . .
H8B N8 H8C 109.5 . .
H9A N9 H9B 109.5 . .
H9A N9 H9C 109.5 . .
H9B N9 H9C 109.5 . .
H10A N10 H10B 108.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 Ge3 2.5973(17) 4_565
Ge1 Ge3 2.5973(17) .
Ge1 Ge2 2.5979(17) 4_565
Ge1 Ge2 2.5979(17) .
Ge2 Ge6 2.5793(17) .
Ge2 Ge5 2.6387(17) .
Ge2 Ge3 2.6794(16) .
Ge3 Ge4 2.5783(18) .
Ge3 Ge5 2.6305(17) .
Ge4 Zn2 2.441(2) .
Ge4 Ge5 2.5496(15) 4_565
Ge4 Ge5 2.5497(15) .
Ge4 Ge3 2.5782(18) 4_565
Ge5 Ge6 2.5481(15) .
Ge6 Zn1 2.423(2) .
Ge6 Ge5 2.5481(15) 4_565
Ge6 Ge2 2.5793(17) 4_565
Zn1 N2 2.058(8) .
Zn1 N2 2.058(8) 4_565
Zn1 N1 2.104(11) .
N1 H1A 0.9100 .
N1 H1B 0.9100 .
N2 N5 3.034(12) .
N2 H2A 0.9100 .
N2 H2B 0.9100 .
N2 H2C 0.9100 .
Zn2 N3 2.061(12) .
Zn2 N4 2.062(9) 4_565
Zn2 N4 2.062(9) .
N3 H3A 0.9100 .
N3 H3B 0.9100 .
N4 N7 3.184(15) .
N4 H4A 0.9100 .
N4 H4B 0.9100 .
N4 H4C 0.9100 .
N5 H5A 0.9100 .
N5 H5B 0.9100 .
N5 H5C 0.9100 .
N6 N4 3.151(17) 1_655
N6 H6A 0.9100 .
N6 H6B 0.9100 .
N6 H6C 0.9100 .
N7 H7A 0.9100 .
N7 H7B 0.9100 .
N7 H7C 0.9100 .
N8 H8A 0.9100 .
N8 H8B 0.9100 .
N8 H8C 0.9100 .
N9 H9A 0.9100 .
N9 H9B 0.9100 .
N9 H9C 0.9100 .
N10 H10A 0.9100 .
N10 H10B 0.9100 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168350966
