# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jcm11621a
_database_code_depnum_ccdc_archive 'CCDC 2403134'
loop_
_audit_author_name
_audit_author_address
'Jesus Campos'
;CSIC
Spain
;
_audit_update_record             
;
2024-11-15 deposited with the CCDC.	2025-01-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H20 Cl Ge N5'
_chemical_formula_weight         462.47

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   7.9741(3)
_cell_length_b                   10.8973(5)
_cell_length_c                   12.7245(5)
_cell_angle_alpha                73.962(2)
_cell_angle_beta                 73.7630(10)
_cell_angle_gamma                78.4580(10)
_cell_volume                     1011.21(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    9916
_cell_measurement_theta_min      2.82
_cell_measurement_theta_max      28.64

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_F_000             472
_exptl_transmission_factor_min   .
_exptl_transmission_factor_max   .
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    1.666
_shelx_estimated_absorpt_T_min   .
_shelx_estimated_absorpt_T_max   .
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6646
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   ' Apex3 v2016.9-0 (Bruker, 2016)'
_exptl_absorpt_special_details   .
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'IuS 3.0 Microfocus Source'
_diffrn_measurement_device_type  'Bruker D8Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean .
_diffrn_reflns_number            36358
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.820
_diffrn_reflns_theta_max         28.736
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             5222
_reflns_number_gt                4186
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker APEX3'
_computing_data_reduction        'Bruker APEX3'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0519P)²+0.7452P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5222
_refine_ls_number_parameters     264
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.1117
_refine_ls_wR_factor_gt          0.0905
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_restrained_S_all      1.141
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.54652(3) 0.63347(2) 0.26674(2) 0.02892(9) Uani 1 1 d . . . . .
Cl1 Cl 0.38929(9) 0.66506(6) 0.13006(5) 0.03677(15) Uani 1 1 d . . . . .
C1 C 0.6628(3) 0.3442(3) 0.2463(2) 0.0329(5) Uani 1 1 d . . . . .
C2 C 0.7085(4) 0.2131(3) 0.2843(3) 0.0405(6) Uani 1 1 d . . . . .
H2 H 0.7906 0.1653 0.2353 0.049 Uiso 1 1 calc R U . . .
C3 C 0.6349(4) 0.1513(3) 0.3938(3) 0.0417(6) Uani 1 1 d . . . . .
H3 H 0.6677 0.0617 0.4209 0.050 Uiso 1 1 calc R U . . .
C4 C 0.5138(4) 0.2217(2) 0.4622(2) 0.0350(6) Uani 1 1 d . . . . .
H4 H 0.4609 0.1812 0.5373 0.042 Uiso 1 1 calc R U . . .
C5 C 0.4689(3) 0.3537(2) 0.4204(2) 0.0284(5) Uani 1 1 d . . . . .
C6 C 0.2769(3) 0.5357(2) 0.4748(2) 0.0266(5) Uani 1 1 d . . . . .
C7 C 0.1206(3) 0.5823(2) 0.5548(2) 0.0293(5) Uani 1 1 d . . . . .
C8 C 0.0196(4) 0.5179(3) 0.6547(2) 0.0348(5) Uani 1 1 d . . . . .
H8 H 0.0480 0.4282 0.6839 0.042 Uiso 1 1 calc R U . . .
C9 C -0.1250(4) 0.5894(3) 0.7104(2) 0.0384(6) Uani 1 1 d . . . . .
H9 H -0.1968 0.5482 0.7793 0.046 Uiso 1 1 calc R U . . .
C10 C -0.1660(4) 0.7206(3) 0.6668(3) 0.0402(6) Uani 1 1 d . . . . .
H10 H -0.2663 0.7671 0.7063 0.048 Uiso 1 1 calc R U . . .
C11 C -0.0640(3) 0.7853(3) 0.5672(2) 0.0368(6) Uani 1 1 d . . . . .
H11 H -0.0914 0.8751 0.5382 0.044 Uiso 1 1 calc R U . . .
C12 C 0.0798(3) 0.7129(2) 0.5119(2) 0.0308(5) Uani 1 1 d . . . . .
C13 C 0.2132(3) 0.7506(2) 0.4068(2) 0.0285(5) Uani 1 1 d . . . . .
C14 C 0.3310(3) 0.9211(2) 0.2587(2) 0.0299(5) Uani 1 1 d . . . . .
C15 C 0.2793(4) 1.0418(2) 0.1938(2) 0.0359(6) Uani 1 1 d . . . . .
H15 H 0.1593 1.0793 0.2080 0.043 Uiso 1 1 calc R U . . .
C16 C 0.4030(4) 1.1057(3) 0.1096(2) 0.0386(6) Uani 1 1 d . . . . .
H16 H 0.3697 1.1877 0.0648 0.046 Uiso 1 1 calc R U . . .
C17 C 0.5768(4) 1.0493(3) 0.0906(2) 0.0371(6) Uani 1 1 d . . . . .
H17 H 0.6651 1.0937 0.0345 0.044 Uiso 1 1 calc R U . . .
C18 C 0.6205(4) 0.9279(3) 0.1539(2) 0.0347(5) Uani 1 1 d . . . . .
C19 C 0.7393(4) 0.4157(3) 0.1283(3) 0.0466(7) Uani 1 1 d . . . . .
H19A H 0.7790 0.4944 0.1324 0.056 Uiso 1 1 calc R U . . .
H19B H 0.6443 0.4437 0.0872 0.056 Uiso 1 1 calc R U . . .
C20 C 0.8929(4) 0.3411(3) 0.0598(3) 0.0491(8) Uani 1 1 d . . . . .
H20A H 0.9901 0.3156 0.0977 0.074 Uiso 1 1 calc R U . . .
H20B H 0.9324 0.3958 -0.0154 0.074 Uiso 1 1 calc R U . . .
H20C H 0.8550 0.2641 0.0530 0.074 Uiso 1 1 calc R U . . .
C21 C 0.8085(4) 0.8629(3) 0.1329(3) 0.0470(7) Uani 1 1 d . . . . .
H21A H 0.8112 0.7767 0.1204 0.056 Uiso 1 1 calc R U . . .
H21B H 0.8787 0.9140 0.0635 0.056 Uiso 1 1 calc R U . . .
C22 C 0.8921(5) 0.8480(4) 0.2292(4) 0.0610(10) Uani 1 1 d . . . . .
H22A H 0.8910 0.9331 0.2414 0.092 Uiso 1 1 calc R U . . .
H22B H 1.0140 0.8063 0.2110 0.092 Uiso 1 1 calc R U . . .
H22C H 0.8255 0.7950 0.2976 0.092 Uiso 1 1 calc R U . . .
N1 N 0.5433(3) 0.4142(2) 0.31437(18) 0.0285(4) Uani 1 1 d . . . . .
N2 N 0.3388(3) 0.4148(2) 0.49396(18) 0.0289(4) Uani 1 1 d . . . . .
N3 N 0.3300(3) 0.6402(2) 0.38708(17) 0.0277(4) Uani 1 1 d . . . . .
N4 N 0.2056(3) 0.8688(2) 0.35049(19) 0.0322(5) Uani 1 1 d . . . . .
N5 N 0.4995(3) 0.8634(2) 0.23717(19) 0.0328(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N3 1.966(2) . ?
Ge1 N1 2.301(2) . ?
Ge1 Cl1 2.3305(7) . ?
Ge1 N5 2.396(2) . ?
C1 N1 1.362(3) . ?
C1 C2 1.385(4) . ?
C1 C19 1.505(4) . ?
C2 C3 1.386(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.372(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.399(3) . ?
C4 H4 0.9500 . ?
C5 N1 1.351(3) . ?
C5 N2 1.386(3) . ?
C6 N2 1.291(3) . ?
C6 N3 1.396(3) . ?
C6 C7 1.474(3) . ?
C7 C12 1.384(4) . ?
C7 C8 1.385(4) . ?
C8 C9 1.388(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.391(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.387(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.388(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.472(4) . ?
C13 N4 1.288(3) . ?
C13 N3 1.401(3) . ?
C14 N5 1.352(3) . ?
C14 N4 1.377(3) . ?
C14 C15 1.399(3) . ?
C15 C16 1.370(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.382(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.381(4) . ?
C17 H17 0.9500 . ?
C18 N5 1.355(3) . ?
C18 C21 1.509(4) . ?
C19 C20 1.522(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.508(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

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
N3 Ge1 N1 85.94(8) . . ?
N3 Ge1 Cl1 92.46(6) . . ?
N1 Ge1 Cl1 92.58(5) . . ?
N3 Ge1 N5 84.43(8) . . ?
N1 Ge1 N5 170.16(8) . . ?
Cl1 Ge1 N5 85.82(6) . . ?
N1 C1 C2 121.0(3) . . ?
N1 C1 C19 116.8(2) . . ?
C2 C1 C19 122.2(2) . . ?
C1 C2 C3 120.1(3) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C4 C3 C2 118.9(3) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
C3 C4 C5 119.4(3) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
N1 C5 N2 123.3(2) . . ?
N1 C5 C4 121.6(2) . . ?
N2 C5 C4 115.0(2) . . ?
N2 C6 N3 132.0(2) . . ?
N2 C6 C7 119.5(2) . . ?
N3 C6 C7 108.5(2) . . ?
C12 C7 C8 121.5(2) . . ?
C12 C7 C6 107.3(2) . . ?
C8 C7 C6 131.2(2) . . ?
C7 C8 C9 117.4(3) . . ?
C7 C8 H8 121.3 . . ?
C9 C8 H8 121.3 . . ?
C8 C9 C10 120.9(3) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C11 C10 C9 121.7(3) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C10 C11 C12 117.1(3) . . ?
C10 C11 H11 121.5 . . ?
C12 C11 H11 121.5 . . ?
C7 C12 C11 121.4(3) . . ?
C7 C12 C13 107.6(2) . . ?
C11 C12 C13 130.9(2) . . ?
N4 C13 N3 131.9(2) . . ?
N4 C13 C12 119.8(2) . . ?
N3 C13 C12 108.3(2) . . ?
N5 C14 N4 121.7(2) . . ?
N5 C14 C15 121.4(2) . . ?
N4 C14 C15 116.8(2) . . ?
C16 C15 C14 119.5(3) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.2 . . ?
C15 C16 C17 119.2(3) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?
C18 C17 C16 119.2(3) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
N5 C18 C17 122.2(3) . . ?
N5 C18 C21 117.5(2) . . ?
C17 C18 C21 120.3(3) . . ?
C1 C19 C20 115.9(3) . . ?
C1 C19 H19A 108.3 . . ?
C20 C19 H19A 108.3 . . ?
C1 C19 H19B 108.3 . . ?
C20 C19 H19B 108.3 . . ?
H19A C19 H19B 107.4 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C18 112.7(3) . . ?
C22 C21 H21A 109.1 . . ?
C18 C21 H21A 109.1 . . ?
C22 C21 H21B 109.1 . . ?
C18 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C5 N1 C1 118.9(2) . . ?
C5 N1 Ge1 120.66(16) . . ?
C1 N1 Ge1 117.24(17) . . ?
C6 N2 C5 126.3(2) . . ?
C6 N3 C13 108.3(2) . . ?
C6 N3 Ge1 124.74(16) . . ?
C13 N3 Ge1 126.65(17) . . ?
C13 N4 C14 126.4(2) . . ?
C14 N5 C18 118.4(2) . . ?
C14 N5 Ge1 117.45(17) . . ?
C18 N5 Ge1 116.20(17) . . ?

_refine_diff_density_max         0.915
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.078

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jcm06421a_sq
_database_code_depnum_ccdc_archive 'CCDC 2403143'
loop_
_audit_author_name
_audit_author_address
'Jesus Campos'
;CSIC
Spain
;
_audit_update_record             
;
2024-11-15 deposited with the CCDC.	2025-01-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H12 Cl Ge N5'
_chemical_formula_weight         406.37

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           78
_space_group_name_H-M_alt        'P 43'
_space_group_name_Hall           'P 4cw'

_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, z+1/2'
'-y, x, z+3/4'
'y, -x, z+1/4'

_cell_length_a                   18.5687(15)
_cell_length_b                   18.5687(15)
_cell_length_c                   5.0359(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1736.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    3503
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      28.27

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_F_000             816
_exptl_transmission_factor_min   .
_exptl_transmission_factor_max   .
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    1.928
_shelx_estimated_absorpt_T_min   .
_shelx_estimated_absorpt_T_max   .
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6237
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   ' Apex3 v2016.9-0 (Bruker, 2016)'
_exptl_absorpt_special_details   .
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'IuS 3.0 Microfocus Source'
_diffrn_measurement_device_type  'Bruker D8Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean .
_diffrn_reflns_number            15125
_diffrn_reflns_av_unetI/netI     0.0931
_diffrn_reflns_av_R_equivalents  0.0896
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         2.194
_diffrn_reflns_theta_max         28.267
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4145
_reflns_number_gt                3371
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.757
_reflns_Friedel_fraction_max     0.931
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker APEX3'
_computing_data_reduction        'Bruker APEX3'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.032 137 38 ' '
2 0.500 0.500 -0.025 28 2 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The unit cell contains 1 pentane molecules which have
 been treated as a diffuse contribution to the overall scattering
 without specific atom positions by SQUEEZE/PLATON.'
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0392P)²+2.7491P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1079 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.036(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4145
_refine_ls_number_parameters     226
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0728
_refine_ls_wR_factor_ref         0.1362
_refine_ls_wR_factor_gt          0.1305
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_restrained_S_all      1.181
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.32872(5) 0.83969(5) 0.08984(18) 0.0223(2) Uani 1 1 d . . . . .
Cl1 Cl 0.30123(12) 0.93736(11) 0.3647(7) 0.0364(6) Uani 1 1 d . . . . .
C1 C 0.4700(5) 0.9131(5) -0.032(2) 0.028(2) Uani 1 1 d . . . . .
H1 H 0.4382 0.9284 -0.1689 0.033 Uiso 1 1 calc R U . . .
C2 C 0.5380(5) 0.9419(5) -0.026(2) 0.031(2) Uani 1 1 d . . . . .
H2 H 0.5528 0.9768 -0.1525 0.037 Uiso 1 1 calc R U . . .
C3 C 0.5845(5) 0.9182(5) 0.171(2) 0.032(3) Uani 1 1 d . . . . .
H3 H 0.6322 0.9366 0.1792 0.039 Uiso 1 1 calc R U . . .
C4 C 0.5619(4) 0.8683(4) 0.353(2) 0.0266(19) Uani 1 1 d . . . . .
H4 H 0.5929 0.8528 0.4916 0.032 Uiso 1 1 calc R U . . .
C5 C 0.4919(4) 0.8408(4) 0.329(2) 0.0200(16) Uani 1 1 d . . . . .
C6 C 0.4087(4) 0.7587(4) 0.5247(16) 0.0189(18) Uani 1 1 d . . . . .
C7 C 0.3976(4) 0.7019(4) 0.7219(17) 0.0170(17) Uani 1 1 d . . . . .
C8 C 0.4439(5) 0.6709(5) 0.9004(18) 0.026(2) Uani 1 1 d . . . . .
H8 H 0.4933 0.6841 0.9060 0.031 Uiso 1 1 calc R U . . .
C9 C 0.4164(5) 0.6201(4) 1.071(2) 0.029(2) Uani 1 1 d . . . . .
H9 H 0.4474 0.5973 1.1951 0.034 Uiso 1 1 calc R U . . .
C10 C 0.3437(5) 0.6016(5) 1.064(2) 0.029(2) Uani 1 1 d . . . . .
H10 H 0.3261 0.5661 1.1835 0.035 Uiso 1 1 calc R U . . .
C11 C 0.2970(5) 0.6338(4) 0.8883(19) 0.027(2) Uani 1 1 d . . . . .
H11 H 0.2472 0.6222 0.8864 0.032 Uiso 1 1 calc R U . . .
C12 C 0.3258(5) 0.6840(4) 0.7136(18) 0.0216(19) Uani 1 1 d . . . . .
C13 C 0.2904(4) 0.7280(4) 0.5109(17) 0.0203(19) Uani 1 1 d . . . . .
C14 C 0.1826(5) 0.7601(5) 0.294(2) 0.029(2) Uani 1 1 d . . . . .
C15 C 0.1078(5) 0.7495(6) 0.288(2) 0.036(3) Uani 1 1 d . . . . .
H15 H 0.0862 0.7181 0.4146 0.044 Uiso 1 1 calc R U . . .
C16 C 0.0657(5) 0.7830(6) 0.106(3) 0.046(3) Uani 1 1 d . . . . .
H16 H 0.0149 0.7764 0.1064 0.055 Uiso 1 1 calc R U . . .
C17 C 0.0983(6) 0.8267(6) -0.078(2) 0.046(3) Uani 1 1 d . . . . .
H17 H 0.0709 0.8492 -0.2139 0.055 Uiso 1 1 calc R U . . .
C18 C 0.1712(6) 0.8372(6) -0.062(2) 0.040(3) Uani 1 1 d . . . . .
H18 H 0.1933 0.8688 -0.1852 0.048 Uiso 1 1 calc R U . . .
N1 N 0.4462(4) 0.8648(3) 0.1437(16) 0.0221(17) Uani 1 1 d . . . . .
N2 N 0.4722(4) 0.7872(3) 0.5073(14) 0.0183(15) Uani 1 1 d . . . . .
N3 N 0.3436(3) 0.7724(3) 0.3921(14) 0.0184(15) Uani 1 1 d . . . . .
N4 N 0.2225(4) 0.7228(4) 0.4765(16) 0.0272(17) Uani 1 1 d . . . . .
N5 N 0.2127(4) 0.8050(4) 0.120(2) 0.0327(19) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N3 1.989(7) . ?
Ge1 N1 2.248(7) . ?
Ge1 N5 2.254(8) . ?
Ge1 Cl1 2.338(3) . ?
C1 N1 1.336(12) . ?
C1 C2 1.371(13) . ?
C1 H1 0.9500 . ?
C2 C3 1.385(14) . ?
C2 H2 0.9500 . ?
C3 C4 1.369(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.403(11) . ?
C4 H4 0.9500 . ?
C5 N1 1.338(12) . ?
C5 N2 1.388(11) . ?
C6 N2 1.294(10) . ?
C6 N3 1.405(10) . ?
C6 C7 1.464(12) . ?
C7 C8 1.371(12) . ?
C7 C12 1.374(11) . ?
C8 C9 1.374(13) . ?
C8 H8 0.9500 . ?
C9 C10 1.393(12) . ?
C9 H9 0.9500 . ?
C10 C11 1.377(13) . ?
C10 H10 0.9500 . ?
C11 C12 1.390(12) . ?
C11 H11 0.9500 . ?
C12 C13 1.462(12) . ?
C13 N4 1.277(11) . ?
C13 N3 1.419(10) . ?
C14 N5 1.330(13) . ?
C14 N4 1.370(13) . ?
C14 C15 1.403(12) . ?
C15 C16 1.356(16) . ?
C15 H15 0.9500 . ?
C16 C17 1.374(17) . ?
C16 H16 0.9500 . ?
C17 C18 1.370(14) . ?
C17 H17 0.9500 . ?
C18 N5 1.338(13) . ?
C18 H18 0.9500 . ?

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
N3 Ge1 N1 84.5(3) . . ?
N3 Ge1 N5 84.3(3) . . ?
N1 Ge1 N5 168.2(3) . . ?
N3 Ge1 Cl1 93.7(2) . . ?
N1 Ge1 Cl1 88.82(19) . . ?
N5 Ge1 Cl1 88.4(2) . . ?
N1 C1 C2 123.4(9) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C1 C2 C3 117.8(9) . . ?
C1 C2 H2 121.1 . . ?
C3 C2 H2 121.1 . . ?
C4 C3 C2 120.2(9) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 118.3(10) . . ?
C3 C4 H4 120.9 . . ?
C5 C4 H4 120.9 . . ?
N1 C5 N2 121.6(7) . . ?
N1 C5 C4 121.6(8) . . ?
N2 C5 C4 116.8(9) . . ?
N2 C6 N3 132.7(8) . . ?
N2 C6 C7 118.0(7) . . ?
N3 C6 C7 109.3(7) . . ?
C8 C7 C12 121.8(8) . . ?
C8 C7 C6 131.2(8) . . ?
C12 C7 C6 106.9(7) . . ?
C7 C8 C9 117.7(8) . . ?
C7 C8 H8 121.2 . . ?
C9 C8 H8 121.2 . . ?
C8 C9 C10 121.0(9) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C11 C10 C9 121.2(9) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C11 C12 117.2(8) . . ?
C10 C11 H11 121.4 . . ?
C12 C11 H11 121.4 . . ?
C7 C12 C11 121.1(8) . . ?
C7 C12 C13 108.8(7) . . ?
C11 C12 C13 130.1(8) . . ?
N4 C13 N3 132.4(8) . . ?
N4 C13 C12 119.8(8) . . ?
N3 C13 C12 107.8(7) . . ?
N5 C14 N4 122.0(8) . . ?
N5 C14 C15 119.5(10) . . ?
N4 C14 C15 118.5(9) . . ?
C16 C15 C14 121.3(11) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C15 C16 C17 118.2(9) . . ?
C15 C16 H16 120.9 . . ?
C17 C16 H16 120.9 . . ?
C18 C17 C16 118.7(11) . . ?
C18 C17 H17 120.7 . . ?
C16 C17 H17 120.7 . . ?
N5 C18 C17 123.1(11) . . ?
N5 C18 H18 118.4 . . ?
C17 C18 H18 118.4 . . ?
C5 N1 C1 118.6(7) . . ?
C5 N1 Ge1 129.0(5) . . ?
C1 N1 Ge1 112.4(6) . . ?
C6 N2 C5 125.2(7) . . ?
C6 N3 C13 107.1(7) . . ?
C6 N3 Ge1 126.6(5) . . ?
C13 N3 Ge1 126.3(5) . . ?
C13 N4 C14 126.0(8) . . ?
C14 N5 C18 119.2(9) . . ?
C14 N5 Ge1 128.7(7) . . ?
C18 N5 Ge1 112.1(7) . . ?

_refine_diff_density_max         1.016
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.116



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jcm09823a
_database_code_depnum_ccdc_archive 'CCDC 2403138'
loop_
_audit_author_name
_audit_author_address
'Jesus Campos'
;CSIC
Spain
;
_audit_update_record             
;
2024-11-15 deposited with the CCDC.	2025-01-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H42 Ge2 N10 O'
_chemical_formula_weight         872.05

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'
Ge Ge 0.1547 1.8001 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   9.5726(5)
_cell_length_b                   12.0978(6)
_cell_length_c                   17.3933(10)
_cell_angle_alpha                91.942(2)
_cell_angle_beta                 94.075(2)
_cell_angle_gamma                107.720(2)
_cell_volume                     1910.58(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    9954
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      27.14

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_F_000             896
_exptl_transmission_factor_min   .
_exptl_transmission_factor_max   .
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    1.625
_shelx_estimated_absorpt_T_min   .
_shelx_estimated_absorpt_T_max   .
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6419
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   ' Apex3 v2016.9-0 (Bruker, 2016)'
_exptl_absorpt_special_details   .
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'IuS 3.0 Microfocus Source'
_diffrn_measurement_device_type  'Bruker D8Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean .
_diffrn_reflns_number            66814
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_av_R_equivalents  0.0934
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.067
_diffrn_reflns_theta_max         27.158
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             8180
_reflns_number_gt                6473
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker APEX3'
_computing_data_reduction        'Bruker APEX3'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+6.7837P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8180
_refine_ls_number_parameters     516
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0669
_refine_ls_wR_factor_ref         0.1164
_refine_ls_wR_factor_gt          0.1093
_refine_ls_goodness_of_fit_ref   1.258
_refine_ls_restrained_S_all      1.269
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.85790(5) 0.27931(4) 0.86444(3) 0.01896(12) Uani 1 1 d . . . . .
Ge2 Ge 0.76230(5) 0.16900(4) 0.64388(3) 0.01975(12) Uani 1 1 d . . . . .
N1 N 0.7853(4) 0.3966(3) 0.81878(19) 0.0174(7) Uani 1 1 d . . . . .
N9 N 0.6660(4) 0.1826(3) 0.81632(19) 0.0174(7) Uani 1 1 d . . . . .
N8 N 0.6532(4) 0.1534(3) 0.5294(2) 0.0224(8) Uani 1 1 d . . . . .
N4 N 0.8106(4) 0.3300(3) 0.6870(2) 0.0182(8) Uani 1 1 d . . . . .
N5 N 0.9910(4) 0.3781(3) 0.6047(2) 0.0216(8) Uani 1 1 d . . . . .
H5 H 0.9588 0.3049 0.5872 0.026 Uiso 1 1 calc DR U . . .
N3 N 0.8315(4) 0.3581(3) 0.9726(2) 0.0226(8) Uani 1 1 d . . . . .
N6 N 0.5740(4) 0.1665(3) 0.6794(2) 0.0178(8) Uani 1 1 d . . . . .
N10 N 0.6739(4) 0.0494(3) 0.9042(2) 0.0231(8) Uani 1 1 d . . . . .
H10 H 0.7549 0.1011 0.9252 0.028 Uiso 1 1 calc DR U . . .
N7 N 0.4199(4) 0.1712(3) 0.5650(2) 0.0240(8) Uani 1 1 d . . . . .
N2 N 0.7111(4) 0.4944(3) 0.9234(2) 0.0259(9) Uani 1 1 d . . . . .
C35 C 0.6009(5) 0.0744(4) 0.8420(2) 0.0190(9) Uani 1 1 d . . . . .
C22 C 0.4448(5) 0.2395(4) 0.7658(2) 0.0180(9) Uani 1 1 d . . . . .
C23 C 0.3855(5) 0.2697(4) 0.8298(3) 0.0226(10) Uani 1 1 d . . . . .
H23 H 0.4400 0.2860 0.8788 0.027 Uiso 1 1 calc R U . . .
C15 C 0.9267(5) 0.4148(4) 0.6620(2) 0.0192(9) Uani 1 1 d . . . . .
C2 C 0.6418(5) 0.4461(4) 0.7208(3) 0.0192(9) Uani 1 1 d . . . . .
C7 C 0.6387(5) 0.5096(4) 0.7883(3) 0.0229(10) Uani 1 1 d . . . . .
C27 C 0.3638(5) 0.2139(4) 0.6946(2) 0.0197(9) Uani 1 1 d . . . . .
C16 C 0.9767(5) 0.5299(4) 0.6915(3) 0.0242(10) Uani 1 1 d . . . . .
H16 H 0.9323 0.5548 0.7331 0.029 Uiso 1 1 calc R U . . .
C21 C 0.5961(5) 0.2299(4) 0.7555(2) 0.0172(9) Uani 1 1 d . . . . .
C8 C 0.7182(5) 0.4673(4) 0.8507(3) 0.0207(9) Uani 1 1 d . . . . .
C1 C 0.7149(5) 0.3555(4) 0.7408(2) 0.0172(9) Uani 1 1 d . . . . .
C28 C 0.4558(5) 0.1803(4) 0.6394(2) 0.0194(9) Uani 1 1 d . . . . .
C26 C 0.2242(5) 0.2242(4) 0.6840(3) 0.0267(10) Uani 1 1 d . . . . .
H26 H 0.1712 0.2102 0.6345 0.032 Uiso 1 1 calc R U . . .
C9 C 0.7659(5) 0.4424(4) 0.9819(3) 0.0255(10) Uani 1 1 d . . . . .
C38 C 0.4965(6) -0.1365(4) 0.9046(3) 0.0337(12) Uani 1 1 d . . . . .
H38 H 0.4625 -0.2093 0.9272 0.040 Uiso 1 1 calc R U . . .
C39 C 0.6234(6) -0.0543(4) 0.9344(3) 0.0302(11) Uani 1 1 d . . . . .
C37 C 0.4190(6) -0.1113(4) 0.8411(3) 0.0299(11) Uani 1 1 d . . . . .
H37 H 0.3302 -0.1667 0.8197 0.036 Uiso 1 1 calc R U . . .
C29 C 0.5130(5) 0.1560(4) 0.5123(2) 0.0213(9) Uani 1 1 d . . . . .
C19 C 1.1041(5) 0.4526(4) 0.5740(3) 0.0261(10) Uani 1 1 d . . . . .
C3 C 0.5792(5) 0.4689(4) 0.6514(3) 0.0255(10) Uani 1 1 d . . . . .
H3 H 0.5820 0.4265 0.6049 0.031 Uiso 1 1 calc R U . . .
C18 C 1.1556(5) 0.5679(4) 0.5991(3) 0.0309(11) Uani 1 1 d . . . . .
H18 H 1.2341 0.6203 0.5758 0.037 Uiso 1 1 calc R U . . .
C25 C 0.1643(5) 0.2557(4) 0.7482(3) 0.0283(11) Uani 1 1 d . . . . .
H25 H 0.0685 0.2637 0.7429 0.034 Uiso 1 1 calc R U . . .
O1 O 1.0395(5) 0.8433(4) 0.7487(3) 0.0654(14) Uani 1 1 d . . . . .
C33 C 0.7305(6) 0.1306(4) 0.4709(3) 0.0274(11) Uani 1 1 d . . . . .
C17 C 1.0913(5) 0.6066(4) 0.6590(3) 0.0298(11) Uani 1 1 d . . . . .
H17 H 1.1263 0.6857 0.6777 0.036 Uiso 1 1 calc R U . . .
C6 C 0.5675(5) 0.5932(4) 0.7903(3) 0.0303(11) Uani 1 1 d . . . . .
H6 H 0.5619 0.6335 0.8372 0.036 Uiso 1 1 calc R U . . .
C24 C 0.2426(5) 0.2756(4) 0.8201(3) 0.0280(11) Uani 1 1 d . . . . .
H24 H 0.1976 0.2937 0.8637 0.034 Uiso 1 1 calc R U . . .
C31 C 0.5342(6) 0.1242(4) 0.3778(3) 0.0332(12) Uani 1 1 d . . . . .
H31 H 0.4941 0.1160 0.3256 0.040 Uiso 1 1 calc R U . . .
C36 C 0.4706(5) -0.0057(4) 0.8089(3) 0.0237(10) Uani 1 1 d . . . . .
H36 H 0.4186 0.0124 0.7650 0.028 Uiso 1 1 calc R U . . .
C5 C 0.5047(6) 0.6155(5) 0.7206(3) 0.0376(13) Uani 1 1 d . . . . .
H5A H 0.4555 0.6728 0.7197 0.045 Uiso 1 1 calc R U . . .
C13 C 0.8901(6) 0.3197(4) 1.0366(3) 0.0300(11) Uani 1 1 d . . . . .
C32 C 0.6722(6) 0.1165(4) 0.3953(3) 0.0317(12) Uani 1 1 d . . . . .
H32 H 0.7278 0.1015 0.3554 0.038 Uiso 1 1 calc R U . . .
C30 C 0.4545(6) 0.1437(4) 0.4355(3) 0.0295(11) Uani 1 1 d . . . . .
H30 H 0.3585 0.1491 0.4236 0.035 Uiso 1 1 calc R U . . .
C20 C 1.1738(6) 0.4049(5) 0.5116(3) 0.0371(13) Uani 1 1 d . . . . .
H20A H 1.2269 0.3544 0.5339 0.056 Uiso 1 1 calc R U . . .
H20B H 1.2428 0.4692 0.4878 0.056 Uiso 1 1 calc R U . . .
H20C H 1.0973 0.3600 0.4723 0.056 Uiso 1 1 calc R U . . .
C11 C 0.8038(7) 0.4399(5) 1.1195(3) 0.0419(14) Uani 1 1 d . . . . .
H11 H 0.7925 0.4666 1.1699 0.050 Uiso 1 1 calc R U . . .
C34 C 0.8786(6) 0.1154(5) 0.4901(3) 0.0449(15) Uani 1 1 d . . . . .
H34A H 0.9197 0.0997 0.4423 0.067 Uiso 1 1 calc R U . . .
H34B H 0.9447 0.1866 0.5171 0.067 Uiso 1 1 calc DR U . . .
H34C H 0.8683 0.0501 0.5233 0.067 Uiso 1 1 calc R U . . .
C12 C 0.8778(6) 0.3606(5) 1.1096(3) 0.0362(13) Uani 1 1 d . . . . .
H12 H 0.9206 0.3338 1.1533 0.043 Uiso 1 1 calc R U . . .
C10 C 0.7464(6) 0.4804(5) 1.0564(3) 0.0370(13) Uani 1 1 d . . . . .
H10A H 0.6932 0.5344 1.0629 0.044 Uiso 1 1 calc R U . . .
C4 C 0.5121(6) 0.5558(4) 0.6521(3) 0.0345(12) Uani 1 1 d . . . . .
H4 H 0.4706 0.5748 0.6050 0.041 Uiso 1 1 calc R U . . .
C14 C 0.9756(7) 0.2359(5) 1.0259(3) 0.0450(15) Uani 1 1 d . . . . .
H14A H 1.0103 0.2165 1.0765 0.068 Uiso 1 1 calc R U . . .
H14B H 0.9122 0.1650 0.9975 0.068 Uiso 1 1 calc DR U . . .
H14C H 1.0602 0.2715 0.9967 0.068 Uiso 1 1 calc R U . . .
C40 C 0.7125(7) -0.0762(5) 1.0037(3) 0.0484(15) Uani 1 1 d . . . . .
H40A H 0.8175 -0.0467 0.9959 0.073 Uiso 1 1 calc R U . . .
H40B H 0.6852 -0.1599 1.0107 0.073 Uiso 1 1 calc R U . . .
H40C H 0.6928 -0.0364 1.0498 0.073 Uiso 1 1 calc R U . . .
C43 C 0.9403(7) 0.9755(5) 0.8072(4) 0.0538(17) Uani 1 1 d . . . . .
H43A H 0.9344 0.9724 0.8638 0.065 Uiso 1 1 calc R U . . .
H43B H 0.9370 1.0526 0.7915 0.065 Uiso 1 1 calc R U . . .
C44 C 1.0776(7) 0.9532(6) 0.7846(5) 0.063(2) Uani 1 1 d . . . . .
H44A H 1.1273 1.0119 0.7490 0.075 Uiso 1 1 calc R U . . .
H44B H 1.1462 0.9586 0.8309 0.075 Uiso 1 1 calc R U . . .
C42 C 0.8202(8) 0.8825(7) 0.7662(6) 0.085(3) Uani 1 1 d . . . . .
H42A H 0.7561 0.8357 0.8031 0.102 Uiso 1 1 calc R U . . .
H42B H 0.7597 0.9153 0.7306 0.102 Uiso 1 1 calc R U . . .
C41 C 0.8899(8) 0.8111(8) 0.7230(6) 0.093(3) Uani 1 1 d . . . . .
H41A H 0.8425 0.7279 0.7312 0.112 Uiso 1 1 calc R U . . .
H41B H 0.8784 0.8227 0.6671 0.112 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 1.930(3) . ?
Ge1 N9 1.962(4) . ?
Ge1 N3 2.146(4) . ?
Ge2 N6 1.939(3) . ?
Ge2 N4 1.969(3) . ?
Ge2 N8 2.157(4) . ?
N1 C8 1.344(5) . ?
N1 C1 1.471(5) . ?
N9 C35 1.373(5) . ?
N9 C21 1.438(5) . ?
N8 C29 1.364(6) . ?
N8 C33 1.368(6) . ?
N4 C15 1.372(6) . ?
N4 C1 1.442(5) . ?
N5 C19 1.338(6) . ?
N5 C15 1.339(5) . ?
N5 H5 0.8800 . ?
N3 C9 1.361(6) . ?
N3 C13 1.369(6) . ?
N6 C28 1.342(5) . ?
N6 C21 1.476(5) . ?
N10 C39 1.340(6) . ?
N10 C35 1.339(5) . ?
N10 H10 0.8800 . ?
N7 C28 1.308(5) . ?
N7 C29 1.368(6) . ?
N2 C8 1.307(6) . ?
N2 C9 1.369(6) . ?
C35 C36 1.396(6) . ?
C22 C23 1.371(6) . ?
C22 C27 1.387(6) . ?
C22 C21 1.510(6) . ?
C23 C24 1.390(6) . ?
C23 H23 0.9500 . ?
C15 C16 1.393(6) . ?
C2 C3 1.383(6) . ?
C2 C7 1.388(6) . ?
C2 C1 1.506(6) . ?
C7 C6 1.381(6) . ?
C7 C8 1.475(6) . ?
C27 C26 1.379(6) . ?
C27 C28 1.475(6) . ?
C16 C17 1.374(7) . ?
C16 H16 0.9500 . ?
C21 C1 1.638(6) . ?
C26 C25 1.383(7) . ?
C26 H26 0.9500 . ?
C9 C10 1.405(6) . ?
C38 C39 1.369(7) . ?
C38 C37 1.381(7) . ?
C38 H38 0.9500 . ?
C39 C40 1.505(7) . ?
C37 C36 1.376(7) . ?
C37 H37 0.9500 . ?
C29 C30 1.396(6) . ?
C19 C18 1.374(7) . ?
C19 C20 1.501(6) . ?
C3 C4 1.390(7) . ?
C3 H3 0.9500 . ?
C18 C17 1.384(7) . ?
C18 H18 0.9500 . ?
C25 C24 1.386(7) . ?
C25 H25 0.9500 . ?
O1 C44 1.381(7) . ?
O1 C41 1.400(8) . ?
C33 C32 1.374(7) . ?
C33 C34 1.501(7) . ?
C17 H17 0.9500 . ?
C6 C5 1.386(7) . ?
C6 H6 0.9500 . ?
C24 H24 0.9500 . ?
C31 C30 1.359(7) . ?
C31 C32 1.367(7) . ?
C31 H31 0.9500 . ?
C36 H36 0.9500 . ?
C5 C4 1.389(8) . ?
C5 H5A 0.9500 . ?
C13 C12 1.374(7) . ?
C13 C14 1.498(7) . ?
C32 H32 0.9500 . ?
C30 H30 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C11 C10 1.364(7) . ?
C11 C12 1.368(8) . ?
C11 H11 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C12 H12 0.9500 . ?
C10 H10A 0.9500 . ?
C4 H4 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C43 C42 1.462(9) . ?
C43 C44 1.496(8) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C42 C41 1.461(10) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?

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 N9 79.49(15) . . ?
N1 Ge1 N3 85.03(14) . . ?
N9 Ge1 N3 110.16(14) . . ?
N6 Ge2 N4 79.74(15) . . ?
N6 Ge2 N8 85.37(14) . . ?
N4 Ge2 N8 109.87(14) . . ?
C8 N1 C1 109.3(3) . . ?
C8 N1 Ge1 129.9(3) . . ?
C1 N1 Ge1 110.0(3) . . ?
C35 N9 C21 121.9(4) . . ?
C35 N9 Ge1 120.1(3) . . ?
C21 N9 Ge1 118.0(3) . . ?
C29 N8 C33 118.9(4) . . ?
C29 N8 Ge2 125.5(3) . . ?
C33 N8 Ge2 115.4(3) . . ?
C15 N4 C1 122.3(4) . . ?
C15 N4 Ge2 119.7(3) . . ?
C1 N4 Ge2 117.8(3) . . ?
C19 N5 C15 120.1(4) . . ?
C19 N5 H5 119.9 . . ?
C15 N5 H5 119.9 . . ?
C9 N3 C13 119.0(4) . . ?
C9 N3 Ge1 125.9(3) . . ?
C13 N3 Ge1 115.2(3) . . ?
C28 N6 C21 109.2(3) . . ?
C28 N6 Ge2 129.1(3) . . ?
C21 N6 Ge2 110.0(3) . . ?
C39 N10 C35 119.9(4) . . ?
C39 N10 H10 120.1 . . ?
C35 N10 H10 120.1 . . ?
C28 N7 C29 122.4(4) . . ?
C8 N2 C9 122.1(4) . . ?
N10 C35 N9 113.8(4) . . ?
N10 C35 C36 120.8(4) . . ?
N9 C35 C36 125.4(4) . . ?
C23 C22 C27 121.0(4) . . ?
C23 C22 C21 131.1(4) . . ?
C27 C22 C21 107.9(4) . . ?
C22 C23 C24 117.5(4) . . ?
C22 C23 H23 121.3 . . ?
C24 C23 H23 121.3 . . ?
N5 C15 N4 114.0(4) . . ?
N5 C15 C16 121.1(4) . . ?
N4 C15 C16 124.9(4) . . ?
C3 C2 C7 120.6(4) . . ?
C3 C2 C1 131.2(4) . . ?
C7 C2 C1 108.2(4) . . ?
C6 C7 C2 122.1(4) . . ?
C6 C7 C8 130.6(4) . . ?
C2 C7 C8 107.2(4) . . ?
C26 C27 C22 121.7(4) . . ?
C26 C27 C28 130.7(4) . . ?
C22 C27 C28 107.5(4) . . ?
C17 C16 C15 118.6(4) . . ?
C17 C16 H16 120.7 . . ?
C15 C16 H16 120.7 . . ?
N9 C21 N6 115.2(3) . . ?
N9 C21 C22 118.1(4) . . ?
N6 C21 C22 102.3(3) . . ?
N9 C21 C1 105.3(3) . . ?
N6 C21 C1 102.9(3) . . ?
C22 C21 C1 112.2(3) . . ?
N2 C8 N1 129.9(4) . . ?
N2 C8 C7 121.7(4) . . ?
N1 C8 C7 108.4(4) . . ?
N4 C1 N1 114.9(3) . . ?
N4 C1 C2 118.0(4) . . ?
N1 C1 C2 102.4(3) . . ?
N4 C1 C21 105.6(3) . . ?
N1 C1 C21 102.6(3) . . ?
C2 C1 C21 112.5(3) . . ?
N7 C28 N6 130.2(4) . . ?
N7 C28 C27 121.5(4) . . ?
N6 C28 C27 108.3(4) . . ?
C27 C26 C25 117.5(4) . . ?
C27 C26 H26 121.3 . . ?
C25 C26 H26 121.3 . . ?
N3 C9 N2 125.5(4) . . ?
N3 C9 C10 119.9(4) . . ?
N2 C9 C10 114.5(4) . . ?
C39 C38 C37 118.5(5) . . ?
C39 C38 H38 120.7 . . ?
C37 C38 H38 120.7 . . ?
N10 C39 C38 122.2(4) . . ?
N10 C39 C40 116.8(5) . . ?
C38 C39 C40 121.1(5) . . ?
C36 C37 C38 119.9(5) . . ?
C36 C37 H37 120.0 . . ?
C38 C37 H37 120.0 . . ?
N8 C29 N7 125.5(4) . . ?
N8 C29 C30 119.9(4) . . ?
N7 C29 C30 114.6(4) . . ?
N5 C19 C18 121.4(4) . . ?
N5 C19 C20 117.3(4) . . ?
C18 C19 C20 121.3(4) . . ?
C2 C3 C4 117.7(5) . . ?
C2 C3 H3 121.1 . . ?
C4 C3 H3 121.1 . . ?
C19 C18 C17 119.0(5) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C26 C25 C24 120.7(4) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C44 O1 C41 107.9(5) . . ?
N8 C33 C32 121.2(5) . . ?
N8 C33 C34 119.2(4) . . ?
C32 C33 C34 119.5(4) . . ?
C16 C17 C18 119.7(5) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C7 C6 C5 116.9(5) . . ?
C7 C6 H6 121.5 . . ?
C5 C6 H6 121.5 . . ?
C25 C24 C23 121.5(4) . . ?
C25 C24 H24 119.3 . . ?
C23 C24 H24 119.3 . . ?
C30 C31 C32 119.6(5) . . ?
C30 C31 H31 120.2 . . ?
C32 C31 H31 120.2 . . ?
C37 C36 C35 118.7(4) . . ?
C37 C36 H36 120.6 . . ?
C35 C36 H36 120.6 . . ?
C6 C5 C4 121.5(4) . . ?
C6 C5 H5A 119.3 . . ?
C4 C5 H5A 119.3 . . ?
N3 C13 C12 121.3(5) . . ?
N3 C13 C14 118.9(4) . . ?
C12 C13 C14 119.7(5) . . ?
C31 C32 C33 119.9(5) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C31 C30 C29 120.4(5) . . ?
C31 C30 H30 119.8 . . ?
C29 C30 H30 119.8 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C10 C11 C12 119.6(5) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C11 C12 C13 119.9(5) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C11 C10 C9 120.0(5) . . ?
C11 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
C5 C4 C3 121.0(5) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C43 C44 104.8(5) . . ?
C42 C43 H43A 110.8 . . ?
C44 C43 H43A 110.8 . . ?
C42 C43 H43B 110.8 . . ?
C44 C43 H43B 110.8 . . ?
H43A C43 H43B 108.9 . . ?
O1 C44 C43 108.3(5) . . ?
O1 C44 H44A 110.0 . . ?
C43 C44 H44A 110.0 . . ?
O1 C44 H44B 110.0 . . ?
C43 C44 H44B 110.0 . . ?
H44A C44 H44B 108.4 . . ?
C41 C42 C43 106.0(6) . . ?
C41 C42 H42A 110.5 . . ?
C43 C42 H42A 110.5 . . ?
C41 C42 H42B 110.5 . . ?
C43 C42 H42B 110.5 . . ?
H42A C42 H42B 108.7 . . ?
O1 C41 C42 108.8(6) . . ?
O1 C41 H41A 109.9 . . ?
C42 C41 H41A 109.9 . . ?
O1 C41 H41B 109.9 . . ?
C42 C41 H41B 109.9 . . ?
H41A C41 H41B 108.3 . . ?

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
C39 N10 C35 N9 -178.9(4) . . . . ?
C39 N10 C35 C36 1.3(6) . . . . ?
C21 N9 C35 N10 -173.2(4) . . . . ?
Ge1 N9 C35 N10 5.3(5) . . . . ?
C21 N9 C35 C36 6.5(6) . . . . ?
Ge1 N9 C35 C36 -175.0(3) . . . . ?
C27 C22 C23 C24 -1.1(7) . . . . ?
C21 C22 C23 C24 177.2(4) . . . . ?
C19 N5 C15 N4 178.8(4) . . . . ?
C19 N5 C15 C16 -0.8(6) . . . . ?
C1 N4 C15 N5 -171.4(4) . . . . ?
Ge2 N4 C15 N5 4.5(5) . . . . ?
C1 N4 C15 C16 8.1(6) . . . . ?
Ge2 N4 C15 C16 -176.0(3) . . . . ?
C3 C2 C7 C6 3.4(7) . . . . ?
C1 C2 C7 C6 -174.5(4) . . . . ?
C3 C2 C7 C8 -178.0(4) . . . . ?
C1 C2 C7 C8 4.1(5) . . . . ?
C23 C22 C27 C26 3.8(7) . . . . ?
C21 C22 C27 C26 -174.8(4) . . . . ?
C23 C22 C27 C28 -177.6(4) . . . . ?
C21 C22 C27 C28 3.7(5) . . . . ?
N5 C15 C16 C17 1.7(6) . . . . ?
N4 C15 C16 C17 -177.8(4) . . . . ?
C35 N9 C21 N6 -64.4(5) . . . . ?
Ge1 N9 C21 N6 117.0(3) . . . . ?
C35 N9 C21 C22 56.7(5) . . . . ?
Ge1 N9 C21 C22 -121.8(3) . . . . ?
C35 N9 C21 C1 -177.0(3) . . . . ?
Ge1 N9 C21 C1 4.4(4) . . . . ?
C28 N6 C21 N9 151.6(4) . . . . ?
Ge2 N6 C21 N9 -61.5(4) . . . . ?
C28 N6 C21 C22 22.2(4) . . . . ?
Ge2 N6 C21 C22 169.1(3) . . . . ?
C28 N6 C21 C1 -94.4(4) . . . . ?
Ge2 N6 C21 C1 52.5(3) . . . . ?
C23 C22 C21 N9 38.8(7) . . . . ?
C27 C22 C21 N9 -142.7(4) . . . . ?
C23 C22 C21 N6 166.4(5) . . . . ?
C27 C22 C21 N6 -15.1(4) . . . . ?
C23 C22 C21 C1 -84.0(6) . . . . ?
C27 C22 C21 C1 94.5(4) . . . . ?
C9 N2 C8 N1 -5.9(8) . . . . ?
C9 N2 C8 C7 170.1(4) . . . . ?
C1 N1 C8 N2 156.6(5) . . . . ?
Ge1 N1 C8 N2 16.4(7) . . . . ?
C1 N1 C8 C7 -19.9(5) . . . . ?
Ge1 N1 C8 C7 -160.0(3) . . . . ?
C6 C7 C8 N2 11.4(8) . . . . ?
C2 C7 C8 N2 -167.1(4) . . . . ?
C6 C7 C8 N1 -171.8(5) . . . . ?
C2 C7 C8 N1 9.7(5) . . . . ?
C15 N4 C1 N1 -66.4(5) . . . . ?
Ge2 N4 C1 N1 117.7(3) . . . . ?
C15 N4 C1 C2 54.5(5) . . . . ?
Ge2 N4 C1 C2 -121.4(4) . . . . ?
C15 N4 C1 C21 -178.8(3) . . . . ?
Ge2 N4 C1 C21 5.3(4) . . . . ?
C8 N1 C1 N4 150.6(4) . . . . ?
Ge1 N1 C1 N4 -61.0(4) . . . . ?
C8 N1 C1 C2 21.4(4) . . . . ?
Ge1 N1 C1 C2 169.9(3) . . . . ?
C8 N1 C1 C21 -95.4(4) . . . . ?
Ge1 N1 C1 C21 53.1(3) . . . . ?
C3 C2 C1 N4 40.3(7) . . . . ?
C7 C2 C1 N4 -142.1(4) . . . . ?
C3 C2 C1 N1 167.5(5) . . . . ?
C7 C2 C1 N1 -14.9(5) . . . . ?
C3 C2 C1 C21 -83.0(6) . . . . ?
C7 C2 C1 C21 94.6(4) . . . . ?
N9 C21 C1 N4 85.9(4) . . . . ?
N6 C21 C1 N4 -35.2(4) . . . . ?
C22 C21 C1 N4 -144.4(3) . . . . ?
N9 C21 C1 N1 -34.8(4) . . . . ?
N6 C21 C1 N1 -155.8(3) . . . . ?
C22 C21 C1 N1 94.9(4) . . . . ?
N9 C21 C1 C2 -144.2(3) . . . . ?
N6 C21 C1 C2 94.8(4) . . . . ?
C22 C21 C1 C2 -14.4(5) . . . . ?
C29 N7 C28 N6 -7.0(7) . . . . ?
C29 N7 C28 C27 170.8(4) . . . . ?
C21 N6 C28 N7 157.2(5) . . . . ?
Ge2 N6 C28 N7 18.6(7) . . . . ?
C21 N6 C28 C27 -20.8(5) . . . . ?
Ge2 N6 C28 C27 -159.5(3) . . . . ?
C26 C27 C28 N7 10.7(8) . . . . ?
C22 C27 C28 N7 -167.7(4) . . . . ?
C26 C27 C28 N6 -171.0(5) . . . . ?
C22 C27 C28 N6 10.6(5) . . . . ?
C22 C27 C26 C25 -3.1(7) . . . . ?
C28 C27 C26 C25 178.7(5) . . . . ?
C13 N3 C9 N2 175.6(5) . . . . ?
Ge1 N3 C9 N2 -2.9(7) . . . . ?
C13 N3 C9 C10 -6.2(7) . . . . ?
Ge1 N3 C9 C10 175.3(4) . . . . ?
C8 N2 C9 N3 -0.5(8) . . . . ?
C8 N2 C9 C10 -178.8(5) . . . . ?
C35 N10 C39 C38 -1.2(7) . . . . ?
C35 N10 C39 C40 179.4(4) . . . . ?
C37 C38 C39 N10 0.3(8) . . . . ?
C37 C38 C39 C40 179.7(5) . . . . ?
C39 C38 C37 C36 0.5(7) . . . . ?
C33 N8 C29 N7 176.2(4) . . . . ?
Ge2 N8 C29 N7 1.4(6) . . . . ?
C33 N8 C29 C30 -4.5(6) . . . . ?
Ge2 N8 C29 C30 -179.4(3) . . . . ?
C28 N7 C29 N8 -3.0(7) . . . . ?
C28 N7 C29 C30 177.7(4) . . . . ?
C15 N5 C19 C18 -1.0(7) . . . . ?
C15 N5 C19 C20 178.2(4) . . . . ?
C7 C2 C3 C4 -0.9(7) . . . . ?
C1 C2 C3 C4 176.5(5) . . . . ?
N5 C19 C18 C17 1.8(7) . . . . ?
C20 C19 C18 C17 -177.4(5) . . . . ?
C27 C26 C25 C24 -0.1(7) . . . . ?
C29 N8 C33 C32 3.5(7) . . . . ?
Ge2 N8 C33 C32 178.8(4) . . . . ?
C29 N8 C33 C34 -173.8(4) . . . . ?
Ge2 N8 C33 C34 1.6(6) . . . . ?
C15 C16 C17 C18 -0.9(7) . . . . ?
C19 C18 C17 C16 -0.8(7) . . . . ?
C2 C7 C6 C5 -3.1(7) . . . . ?
C8 C7 C6 C5 178.7(5) . . . . ?
C26 C25 C24 C23 2.8(8) . . . . ?
C22 C23 C24 C25 -2.2(7) . . . . ?
C38 C37 C36 C35 -0.5(7) . . . . ?
N10 C35 C36 C37 -0.4(6) . . . . ?
N9 C35 C36 C37 179.8(4) . . . . ?
C7 C6 C5 C4 0.5(8) . . . . ?
C9 N3 C13 C12 3.0(7) . . . . ?
Ge1 N3 C13 C12 -178.3(4) . . . . ?
C9 N3 C13 C14 -173.8(5) . . . . ?
Ge1 N3 C13 C14 4.8(6) . . . . ?
C30 C31 C32 C33 -1.2(8) . . . . ?
N8 C33 C32 C31 -0.6(7) . . . . ?
C34 C33 C32 C31 176.6(5) . . . . ?
C32 C31 C30 C29 0.1(8) . . . . ?
N8 C29 C30 C31 2.8(7) . . . . ?
N7 C29 C30 C31 -177.8(4) . . . . ?
C10 C11 C12 C13 -1.9(9) . . . . ?
N3 C13 C12 C11 1.1(8) . . . . ?
C14 C13 C12 C11 177.9(5) . . . . ?
C12 C11 C10 C9 -1.3(9) . . . . ?
N3 C9 C10 C11 5.4(8) . . . . ?
N2 C9 C10 C11 -176.2(5) . . . . ?
C6 C5 C4 C3 2.0(8) . . . . ?
C2 C3 C4 C5 -1.7(7) . . . . ?
C41 O1 C44 C43 20.4(9) . . . . ?
C42 C43 C44 O1 -12.7(9) . . . . ?
C44 C43 C42 C41 0.5(10) . . . . ?
C44 O1 C41 C42 -20.2(10) . . . . ?
C43 C42 C41 O1 11.7(11) . . . . ?

_refine_diff_density_max         0.690
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.103

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jcm13021a
_database_code_depnum_ccdc_archive 'CCDC 2403137'
loop_
_audit_author_name
_audit_author_address
'Jesus Campos'
;CSIC
Spain
;
_audit_update_record             
;
2024-11-15 deposited with the CCDC.	2025-01-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H16 Cl Ge N5'
_chemical_formula_weight         434.42

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.5131(8)
_cell_length_b                   13.2092(8)
_cell_length_c                   16.4883(9)
_cell_angle_alpha                90
_cell_angle_beta                 98.056(2)
_cell_angle_gamma                90
_cell_volume                     3561.0(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    8778
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      27.20

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_F_000             1760
_exptl_transmission_factor_min   .
_exptl_transmission_factor_max   .
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    1.886
_shelx_estimated_absorpt_T_min   .
_shelx_estimated_absorpt_T_max   .
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6505
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   ' Apex3 v2016.9-0 (Bruker, 2016)'
_exptl_absorpt_special_details   .
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'IuS 3.0 Microfocus Source'
_diffrn_measurement_device_type  'Bruker D8Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean .
_diffrn_reflns_number            172562
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_av_R_equivalents  0.1549
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.982
_diffrn_reflns_theta_max         28.316
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8840
_reflns_number_gt                6804
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker APEX3'
_computing_data_reduction        'Bruker APEX3'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0092P)²+116.3593P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8840
_refine_ls_number_parameters     491
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1614
_refine_ls_R_factor_gt           0.1327
_refine_ls_wR_factor_ref         0.2818
_refine_ls_wR_factor_gt          0.2692
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_restrained_S_all      1.206
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 1.00865(7) 0.60825(9) 0.64300(7) 0.0219(3) Uani 1 1 d . . . . .
Ge2 Ge 0.39665(7) 0.88041(9) 0.48866(7) 0.0204(3) Uani 1 1 d . . . . .
Cl2 Cl 0.38015(17) 0.7042(2) 0.48480(17) 0.0290(6) Uani 1 1 d . . . . .
Cl1 Cl 1.01619(17) 0.7861(2) 0.65579(18) 0.0300(6) Uani 1 1 d . . . . .
C1 C 1.1207(6) 0.6370(8) 0.5087(7) 0.020(2) Uani 1 1 d . . . . .
C2 C 1.1495(7) 0.6462(9) 0.4341(7) 0.027(2) Uani 1 1 d . . . . .
H2 H 1.2065 0.6498 0.4313 0.032 Uiso 1 1 calc R U . . .
C3 C 1.0933(7) 0.6502(9) 0.3641(7) 0.029(2) Uani 1 1 d . . . . .
H3 H 1.1115 0.6588 0.3124 0.035 Uiso 1 1 calc R U . . .
C4 C 1.0119(7) 0.6418(9) 0.3684(7) 0.030(3) Uani 1 1 d . . . . .
H4 H 0.9735 0.6428 0.3198 0.036 Uiso 1 1 calc R U . . .
C5 C 0.9849(7) 0.6317(8) 0.4447(7) 0.026(2) Uani 1 1 d . . . . .
C6 C 0.8643(6) 0.6129(8) 0.5096(6) 0.023(2) Uani 1 1 d . . . . .
C7 C 0.7764(7) 0.6054(8) 0.4978(6) 0.021(2) Uani 1 1 d . . . . .
C8 C 0.7205(7) 0.6072(11) 0.4263(7) 0.036(3) Uani 1 1 d . . . . .
H8 H 0.7385 0.6130 0.3742 0.043 Uiso 1 1 calc R U . . .
C9 C 0.6370(8) 0.6003(11) 0.4329(7) 0.035(3) Uani 1 1 d . . . . .
H9 H 0.5978 0.6015 0.3849 0.042 Uiso 1 1 calc R U . . .
C10 C 0.6107(7) 0.5917(9) 0.5106(7) 0.030(3) Uani 1 1 d . . . . .
H10 H 0.5541 0.5868 0.5149 0.036 Uiso 1 1 calc R U . . .
C11 C 0.6687(6) 0.5903(9) 0.5812(7) 0.028(2) Uani 1 1 d . . . . .
H11 H 0.6520 0.5847 0.6338 0.034 Uiso 1 1 calc R U . . .
C12 C 0.7498(6) 0.5973(8) 0.5729(7) 0.022(2) Uani 1 1 d . . . . .
C13 C 0.8232(6) 0.5994(8) 0.6339(6) 0.0181(19) Uani 1 1 d . . . . .
C14 C 0.8759(6) 0.6038(8) 0.7765(6) 0.021(2) Uani 1 1 d . . . . .
C15 C 0.8515(8) 0.6186(11) 0.8544(7) 0.037(3) Uani 1 1 d . . . . .
H15 H 0.7952 0.6266 0.8590 0.044 Uiso 1 1 calc R U . . .
C16 C 0.9070(7) 0.6213(11) 0.9217(7) 0.037(3) Uani 1 1 d . . . . .
H16 H 0.8908 0.6324 0.9740 0.045 Uiso 1 1 calc R U . . .
C17 C 0.9875(8) 0.6077(11) 0.9137(7) 0.037(3) Uani 1 1 d . . . . .
H17 H 1.0275 0.6067 0.9611 0.044 Uiso 1 1 calc R U . . .
C18 C 1.0114(7) 0.5953(9) 0.8360(7) 0.026(2) Uani 1 1 d . . . . .
C19 C 1.1789(7) 0.6355(10) 0.5866(7) 0.032(3) Uani 1 1 d . . . . .
H19A H 1.1739 0.6986 0.6166 0.048 Uiso 1 1 calc R U . . .
H19B H 1.2349 0.6287 0.5740 0.048 Uiso 1 1 calc R U . . .
H19C H 1.1661 0.5780 0.6202 0.048 Uiso 1 1 calc R U . . .
C20 C 1.0986(7) 0.5817(13) 0.8275(8) 0.044(4) Uani 1 1 d . . . . .
H20A H 1.1064 0.5152 0.8033 0.065 Uiso 1 1 calc R U . . .
H20B H 1.1317 0.5860 0.8815 0.065 Uiso 1 1 calc R U . . .
H20C H 1.1155 0.6348 0.7919 0.065 Uiso 1 1 calc R U . . .
C21 C 0.2830(7) 0.8848(9) 0.6269(7) 0.028(2) Uani 1 1 d . . . . .
C22 C 0.2552(7) 0.8895(9) 0.7022(7) 0.031(3) Uani 1 1 d . . . . .
H22 H 0.1984 0.8961 0.7052 0.037 Uiso 1 1 calc R U . . .
C23 C 0.3112(7) 0.8846(9) 0.7735(7) 0.029(2) Uani 1 1 d . . . . .
H23 H 0.2933 0.8867 0.8258 0.035 Uiso 1 1 calc R U . . .
C24 C 0.3924(7) 0.8767(9) 0.7666(7) 0.028(2) Uani 1 1 d . . . . .
H24 H 0.4321 0.8734 0.8142 0.033 Uiso 1 1 calc R U . . .
C25 C 0.4158(6) 0.8734(8) 0.6898(6) 0.020(2) Uani 1 1 d . . . . .
C26 C 0.5371(6) 0.8669(8) 0.6253(6) 0.021(2) Uani 1 1 d . . . . .
C27 C 0.6277(6) 0.8561(8) 0.6368(6) 0.020(2) Uani 1 1 d . . . . .
C28 C 0.6824(7) 0.8457(9) 0.7075(7) 0.029(2) Uani 1 1 d . . . . .
H28 H 0.6646 0.8427 0.7598 0.035 Uiso 1 1 calc R U . . .
C29 C 0.7653(7) 0.8399(9) 0.6989(7) 0.030(3) Uani 1 1 d . . . . .
H29 H 0.8052 0.8339 0.7461 0.036 Uiso 1 1 calc R U . . .
C30 C 0.7899(7) 0.8427(10) 0.6210(8) 0.032(3) Uani 1 1 d . . . . .
H30 H 0.8465 0.8378 0.6166 0.038 Uiso 1 1 calc R U . . .
C31 C 0.7358(7) 0.8522(8) 0.5521(8) 0.028(2) Uani 1 1 d . . . . .
H31 H 0.7533 0.8548 0.4997 0.033 Uiso 1 1 calc R U . . .
C32 C 0.6536(7) 0.8579(8) 0.5611(7) 0.025(2) Uani 1 1 d . . . . .
C33 C 0.5798(6) 0.8660(7) 0.4984(6) 0.019(2) Uani 1 1 d . . . . .
C34 C 0.5280(6) 0.8712(8) 0.3563(7) 0.021(2) Uani 1 1 d . . . . .
C35 C 0.5548(7) 0.8737(9) 0.2801(7) 0.028(2) Uani 1 1 d . . . . .
H35 H 0.6115 0.8718 0.2756 0.034 Uiso 1 1 calc R U . . .
C36 C 0.4959(9) 0.8791(10) 0.2097(8) 0.039(3) Uani 1 1 d . . . . .
H36 H 0.5127 0.8809 0.1569 0.047 Uiso 1 1 calc R U . . .
C37 C 0.4137(8) 0.8817(10) 0.2173(7) 0.032(3) Uani 1 1 d . . . . .
H37 H 0.3735 0.8861 0.1702 0.039 Uiso 1 1 calc R U . . .
C38 C 0.3906(7) 0.8777(8) 0.2967(7) 0.024(2) Uani 1 1 d . . . . .
C39 C 0.2238(7) 0.8899(11) 0.5479(8) 0.036(3) Uani 1 1 d . . . . .
H39A H 0.2295 0.9553 0.5213 0.055 Uiso 1 1 calc R U . . .
H39B H 0.1677 0.8823 0.5600 0.055 Uiso 1 1 calc R U . . .
H39C H 0.2360 0.8352 0.5113 0.055 Uiso 1 1 calc R U . . .
C40 C 0.3043(7) 0.8774(11) 0.3076(7) 0.034(3) Uani 1 1 d . . . . .
H40A H 0.2941 0.8218 0.3443 0.051 Uiso 1 1 calc R U . . .
H40B H 0.2704 0.8682 0.2544 0.051 Uiso 1 1 calc R U . . .
H40C H 0.2905 0.9419 0.3316 0.051 Uiso 1 1 calc R U . . .
N1 N 1.0388(5) 0.6307(7) 0.5145(5) 0.0220(18) Uani 1 1 d . . . . .
N2 N 0.9009(6) 0.6223(8) 0.4455(5) 0.028(2) Uani 1 1 d . . . . .
N3 N 0.8918(5) 0.6102(8) 0.5926(5) 0.0244(19) Uani 1 1 d . . . . .
N4 N 0.8152(5) 0.5988(8) 0.7109(5) 0.0248(19) Uani 1 1 d . . . . .
N5 N 0.9555(6) 0.5958(8) 0.7704(6) 0.027(2) Uani 1 1 d . . . . .
N6 N 0.3625(6) 0.8772(7) 0.6201(5) 0.0250(19) Uani 1 1 d . . . . .
N7 N 0.5013(5) 0.8660(7) 0.6877(6) 0.0247(19) Uani 1 1 d . . . . .
N8 N 0.5112(5) 0.8740(7) 0.5402(5) 0.0227(19) Uani 1 1 d . . . . .
N9 N 0.5892(6) 0.8677(7) 0.4225(6) 0.026(2) Uani 1 1 d . . . . .
N10 N 0.4482(5) 0.8731(7) 0.3650(5) 0.0232(19) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N3 1.991(9) . ?
Ge1 N1 2.263(9) . ?
Ge1 Cl1 2.361(3) . ?
Ge1 N5 2.393(9) . ?
Ge2 N8 1.964(8) . ?
Ge2 N6 2.316(9) . ?
Ge2 N10 2.320(9) . ?
Ge2 Cl2 2.343(3) . ?
C1 N1 1.372(13) . ?
C1 C2 1.384(15) . ?
C1 C19 1.492(15) . ?
C2 C3 1.377(16) . ?
C3 C4 1.361(16) . ?
C4 C5 1.397(16) . ?
C5 N1 1.352(14) . ?
C5 N2 1.394(14) . ?
C6 N2 1.295(14) . ?
C6 N3 1.381(13) . ?
C6 C7 1.442(15) . ?
C7 C12 1.376(14) . ?
C7 C8 1.392(15) . ?
C8 C9 1.401(17) . ?
C9 C10 1.414(17) . ?
C10 C11 1.399(15) . ?
C11 C12 1.368(14) . ?
C12 C13 1.462(13) . ?
C13 N4 1.295(13) . ?
C13 N3 1.409(13) . ?
C14 N5 1.336(13) . ?
C14 N4 1.370(13) . ?
C14 C15 1.412(15) . ?
C15 C16 1.337(16) . ?
C16 C17 1.366(17) . ?
C17 C18 1.403(16) . ?
C18 N5 1.320(14) . ?
C18 C20 1.476(15) . ?
C21 N6 1.337(15) . ?
C21 C22 1.383(16) . ?
C21 C39 1.517(16) . ?
C22 C23 1.391(17) . ?
C23 C24 1.366(16) . ?
C24 C25 1.376(15) . ?
C25 N6 1.346(13) . ?
C25 N7 1.422(13) . ?
C26 N7 1.256(14) . ?
C26 N8 1.412(13) . ?
C26 C27 1.489(14) . ?
C27 C28 1.378(14) . ?
C27 C32 1.376(15) . ?
C28 C29 1.398(16) . ?
C29 C30 1.400(17) . ?
C30 C31 1.349(17) . ?
C31 C32 1.388(15) . ?
C32 C33 1.487(14) . ?
C33 N9 1.282(13) . ?
C33 N8 1.409(13) . ?
C34 N10 1.345(13) . ?
C34 N9 1.381(14) . ?
C34 C35 1.390(15) . ?
C35 C36 1.408(18) . ?
C36 C37 1.381(18) . ?
C37 C38 1.415(16) . ?
C38 N10 1.370(13) . ?
C38 C40 1.461(16) . ?

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
N3 Ge1 N1 86.2(3) . . ?
N3 Ge1 Cl1 93.5(3) . . ?
N1 Ge1 Cl1 86.4(2) . . ?
N3 Ge1 N5 85.1(3) . . ?
N1 Ge1 N5 170.7(3) . . ?
Cl1 Ge1 N5 90.6(3) . . ?
N8 Ge2 N6 86.6(3) . . ?
N8 Ge2 N10 85.9(3) . . ?
N6 Ge2 N10 171.9(3) . . ?
N8 Ge2 Cl2 94.0(3) . . ?
N6 Ge2 Cl2 88.0(3) . . ?
N10 Ge2 Cl2 89.5(3) . . ?
N1 C1 C2 122.1(10) . . ?
N1 C1 C19 117.5(9) . . ?
C2 C1 C19 120.4(9) . . ?
C3 C2 C1 118.3(10) . . ?
C4 C3 C2 120.5(11) . . ?
C3 C4 C5 119.8(11) . . ?
N1 C5 C4 120.8(10) . . ?
N1 C5 N2 121.8(10) . . ?
C4 C5 N2 117.4(10) . . ?
N2 C6 N3 133.3(10) . . ?
N2 C6 C7 118.2(9) . . ?
N3 C6 C7 108.5(9) . . ?
C12 C7 C8 120.5(10) . . ?
C12 C7 C6 109.0(9) . . ?
C8 C7 C6 130.5(10) . . ?
C7 C8 C9 118.4(11) . . ?
C8 C9 C10 120.4(11) . . ?
C11 C10 C9 119.6(10) . . ?
C12 C11 C10 118.8(11) . . ?
C11 C12 C7 122.3(10) . . ?
C11 C12 C13 131.4(10) . . ?
C7 C12 C13 106.3(8) . . ?
N4 C13 N3 132.4(9) . . ?
N4 C13 C12 119.0(9) . . ?
N3 C13 C12 108.3(8) . . ?
N5 C14 N4 123.7(10) . . ?
N5 C14 C15 119.3(10) . . ?
N4 C14 C15 117.0(10) . . ?
C16 C15 C14 120.6(11) . . ?
C15 C16 C17 118.6(12) . . ?
C16 C17 C18 120.4(11) . . ?
N5 C18 C17 119.5(10) . . ?
N5 C18 C20 120.1(10) . . ?
C17 C18 C20 120.3(11) . . ?
N6 C21 C22 122.1(11) . . ?
N6 C21 C39 116.9(10) . . ?
C22 C21 C39 121.0(11) . . ?
C21 C22 C23 119.5(11) . . ?
C24 C23 C22 118.5(10) . . ?
C23 C24 C25 119.0(10) . . ?
N6 C25 C24 123.4(10) . . ?
N6 C25 N7 121.0(9) . . ?
C24 C25 N7 115.6(9) . . ?
N7 C26 N8 134.8(10) . . ?
N7 C26 C27 118.3(9) . . ?
N8 C26 C27 106.9(9) . . ?
C28 C27 C32 121.3(10) . . ?
C28 C27 C26 130.2(10) . . ?
C32 C27 C26 108.5(9) . . ?
C27 C28 C29 117.1(11) . . ?
C28 C29 C30 120.3(10) . . ?
C31 C30 C29 122.2(11) . . ?
C30 C31 C32 117.2(11) . . ?
C27 C32 C31 121.9(10) . . ?
C27 C32 C33 107.7(9) . . ?
C31 C32 C33 130.4(11) . . ?
N9 C33 N8 133.8(10) . . ?
N9 C33 C32 118.6(10) . . ?
N8 C33 C32 107.6(9) . . ?
N10 C34 N9 122.5(10) . . ?
N10 C34 C35 122.4(10) . . ?
N9 C34 C35 115.1(10) . . ?
C34 C35 C36 118.4(11) . . ?
C37 C36 C35 120.0(11) . . ?
C36 C37 C38 118.6(11) . . ?
N10 C38 C37 121.1(10) . . ?
N10 C38 C40 118.4(10) . . ?
C37 C38 C40 120.6(10) . . ?
C5 N1 C1 118.6(9) . . ?
C5 N1 Ge1 126.4(7) . . ?
C1 N1 Ge1 114.9(7) . . ?
C6 N2 C5 126.5(9) . . ?
C6 N3 C13 107.9(8) . . ?
C6 N3 Ge1 125.4(7) . . ?
C13 N3 Ge1 126.5(7) . . ?
C13 N4 C14 127.6(9) . . ?
C18 N5 C14 121.4(10) . . ?
C18 N5 Ge1 114.8(7) . . ?
C14 N5 Ge1 123.2(7) . . ?
C21 N6 C25 117.6(9) . . ?
C21 N6 Ge2 116.7(7) . . ?
C25 N6 Ge2 125.7(7) . . ?
C26 N7 C25 127.0(9) . . ?
C26 N8 C33 109.3(8) . . ?
C26 N8 Ge2 124.8(7) . . ?
C33 N8 Ge2 125.7(7) . . ?
C33 N9 C34 126.6(10) . . ?
C34 N10 C38 119.5(9) . . ?
C34 N10 Ge2 125.4(7) . . ?
C38 N10 Ge2 115.0(7) . . ?

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
N1 C1 C2 C3 0.6(17) . . . . ?
C19 C1 C2 C3 -178.2(11) . . . . ?
C1 C2 C3 C4 -2.1(18) . . . . ?
C2 C3 C4 C5 1.7(19) . . . . ?
C3 C4 C5 N1 0.3(18) . . . . ?
C3 C4 C5 N2 -179.3(11) . . . . ?
N2 C6 C7 C12 -179.2(11) . . . . ?
N3 C6 C7 C12 -0.5(13) . . . . ?
N2 C6 C7 C8 -0.6(19) . . . . ?
N3 C6 C7 C8 178.2(12) . . . . ?
C12 C7 C8 C9 -0.2(19) . . . . ?
C6 C7 C8 C9 -178.7(12) . . . . ?
C7 C8 C9 C10 0(2) . . . . ?
C8 C9 C10 C11 0(2) . . . . ?
C9 C10 C11 C12 -0.2(19) . . . . ?
C10 C11 C12 C7 -0.1(18) . . . . ?
C10 C11 C12 C13 179.0(12) . . . . ?
C8 C7 C12 C11 0.3(18) . . . . ?
C6 C7 C12 C11 179.1(11) . . . . ?
C8 C7 C12 C13 -179.0(11) . . . . ?
C6 C7 C12 C13 -0.2(12) . . . . ?
C11 C12 C13 N4 -3.1(19) . . . . ?
C7 C12 C13 N4 176.0(10) . . . . ?
C11 C12 C13 N3 -178.4(12) . . . . ?
C7 C12 C13 N3 0.8(12) . . . . ?
N5 C14 C15 C16 -2(2) . . . . ?
N4 C14 C15 C16 178.0(13) . . . . ?
C14 C15 C16 C17 -1(2) . . . . ?
C15 C16 C17 C18 3(2) . . . . ?
C16 C17 C18 N5 -1(2) . . . . ?
C16 C17 C18 C20 179.4(14) . . . . ?
N6 C21 C22 C23 -1.2(18) . . . . ?
C39 C21 C22 C23 180.0(12) . . . . ?
C21 C22 C23 C24 1.0(18) . . . . ?
C22 C23 C24 C25 -0.3(18) . . . . ?
C23 C24 C25 N6 -0.3(18) . . . . ?
C23 C24 C25 N7 179.5(11) . . . . ?
N7 C26 C27 C28 -0.8(18) . . . . ?
N8 C26 C27 C28 -179.5(11) . . . . ?
N7 C26 C27 C32 179.3(10) . . . . ?
N8 C26 C27 C32 0.6(12) . . . . ?
C32 C27 C28 C29 1.7(17) . . . . ?
C26 C27 C28 C29 -178.3(11) . . . . ?
C27 C28 C29 C30 -1.2(18) . . . . ?
C28 C29 C30 C31 1(2) . . . . ?
C29 C30 C31 C32 -0.7(18) . . . . ?
C28 C27 C32 C31 -1.7(17) . . . . ?
C26 C27 C32 C31 178.2(10) . . . . ?
C28 C27 C32 C33 177.9(10) . . . . ?
C26 C27 C32 C33 -2.1(12) . . . . ?
C30 C31 C32 C27 1.2(17) . . . . ?
C30 C31 C32 C33 -178.4(11) . . . . ?
C27 C32 C33 N9 -179.2(10) . . . . ?
C31 C32 C33 N9 0.5(18) . . . . ?
C27 C32 C33 N8 3.0(12) . . . . ?
C31 C32 C33 N8 -177.4(11) . . . . ?
N10 C34 C35 C36 0.4(17) . . . . ?
N9 C34 C35 C36 -178.9(11) . . . . ?
C34 C35 C36 C37 0.0(19) . . . . ?
C35 C36 C37 C38 -1(2) . . . . ?
C36 C37 C38 N10 1.1(18) . . . . ?
C36 C37 C38 C40 -178.2(12) . . . . ?
C4 C5 N1 C1 -1.8(16) . . . . ?
N2 C5 N1 C1 177.8(10) . . . . ?
C4 C5 N1 Ge1 -177.0(8) . . . . ?
N2 C5 N1 Ge1 2.6(15) . . . . ?
C2 C1 N1 C5 1.3(16) . . . . ?
C19 C1 N1 C5 -179.9(10) . . . . ?
C2 C1 N1 Ge1 177.1(9) . . . . ?
C19 C1 N1 Ge1 -4.1(12) . . . . ?
N3 C6 N2 C5 1(2) . . . . ?
C7 C6 N2 C5 179.2(11) . . . . ?
N1 C5 N2 C6 0.8(18) . . . . ?
C4 C5 N2 C6 -179.6(12) . . . . ?
N2 C6 N3 C13 179.4(13) . . . . ?
C7 C6 N3 C13 0.9(12) . . . . ?
N2 C6 N3 Ge1 -6.0(19) . . . . ?
C7 C6 N3 Ge1 175.5(7) . . . . ?
N4 C13 N3 C6 -175.5(12) . . . . ?
C12 C13 N3 C6 -1.1(12) . . . . ?
N4 C13 N3 Ge1 10.1(18) . . . . ?
C12 C13 N3 Ge1 -175.5(7) . . . . ?
N3 C13 N4 C14 -4(2) . . . . ?
C12 C13 N4 C14 -177.7(11) . . . . ?
N5 C14 N4 C13 -9.9(19) . . . . ?
C15 C14 N4 C13 169.9(12) . . . . ?
C17 C18 N5 C14 -2.7(18) . . . . ?
C20 C18 N5 C14 177.2(12) . . . . ?
C17 C18 N5 Ge1 167.9(10) . . . . ?
C20 C18 N5 Ge1 -12.2(15) . . . . ?
N4 C14 N5 C18 -176.1(11) . . . . ?
C15 C14 N5 C18 4.1(17) . . . . ?
N4 C14 N5 Ge1 14.1(15) . . . . ?
C15 C14 N5 Ge1 -165.7(9) . . . . ?
C22 C21 N6 C25 0.6(17) . . . . ?
C39 C21 N6 C25 179.5(11) . . . . ?
C22 C21 N6 Ge2 -176.3(9) . . . . ?
C39 C21 N6 Ge2 2.6(14) . . . . ?
C24 C25 N6 C21 0.1(17) . . . . ?
N7 C25 N6 C21 -179.6(10) . . . . ?
C24 C25 N6 Ge2 176.7(8) . . . . ?
N7 C25 N6 Ge2 -3.1(15) . . . . ?
N8 C26 N7 C25 -1(2) . . . . ?
C27 C26 N7 C25 -178.8(10) . . . . ?
N6 C25 N7 C26 3.5(17) . . . . ?
C24 C25 N7 C26 -176.2(11) . . . . ?
N7 C26 N8 C33 -177.1(13) . . . . ?
C27 C26 N8 C33 1.3(12) . . . . ?
N7 C26 N8 Ge2 -2.7(19) . . . . ?
C27 C26 N8 Ge2 175.7(7) . . . . ?
N9 C33 N8 C26 180.0(11) . . . . ?
C32 C33 N8 C26 -2.6(11) . . . . ?
N9 C33 N8 Ge2 5.6(17) . . . . ?
C32 C33 N8 Ge2 -177.0(7) . . . . ?
N8 C33 N9 C34 -5.4(19) . . . . ?
C32 C33 N9 C34 177.5(10) . . . . ?
N10 C34 N9 C33 -0.1(17) . . . . ?
C35 C34 N9 C33 179.2(11) . . . . ?
N9 C34 N10 C38 179.3(10) . . . . ?
C35 C34 N10 C38 0.0(16) . . . . ?
N9 C34 N10 Ge2 3.7(15) . . . . ?
C35 C34 N10 Ge2 -175.6(8) . . . . ?
C37 C38 N10 C34 -0.8(17) . . . . ?
C40 C38 N10 C34 178.6(11) . . . . ?
C37 C38 N10 Ge2 175.2(9) . . . . ?
C40 C38 N10 Ge2 -5.4(14) . . . . ?

_refine_diff_density_max         1.369
_refine_diff_density_min         -1.869
_refine_diff_density_rms         0.204

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jcm09021a
_database_code_depnum_ccdc_archive 'CCDC 2403136'
loop_
_audit_author_name
_audit_author_address
'Jesus Campos'
;CSIC
Spain
;
_audit_update_record             
;
2024-11-15 deposited with the CCDC.	2025-01-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H34 Ge N6 Si2'
_chemical_formula_weight         559.36

_vrf_PLAT411_jcm09021a           
;
PROBLEM: Short Inter H...H Contact  H8       ..H8
RESPONSE: All hydrogen atoms are located at calculated positions.
The contact in this case is due to two symmetry equivalent 
hydrogens that are highly close in space due to the strong
pi-pi packing between two 'planar' molecules.
;


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'
Si Si 0.0817 0.0704 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.1498(3)
_cell_length_b                   29.6775(9)
_cell_length_c                   8.7878(2)
_cell_angle_alpha                90
_cell_angle_beta                 103.0370(10)
_cell_angle_gamma                90
_cell_volume                     2832.92(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    9865
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      28.08

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_F_000             1168
_exptl_transmission_factor_min   .
_exptl_transmission_factor_max   .
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    1.191
_shelx_estimated_absorpt_T_min   .
_shelx_estimated_absorpt_T_max   .
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6401
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   ' Apex3 v2016.9-0 (Bruker, 2016)'
_exptl_absorpt_special_details   .
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'IuS 3.0 Microfocus Source'
_diffrn_measurement_device_type  'Bruker D8Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean .
_diffrn_reflns_number            61649
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.996
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6513
_reflns_number_gt                5459
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker APEX3'
_computing_data_reduction        'Bruker APEX3'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²+0.8218P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6513
_refine_ls_number_parameters     324
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.1543
_refine_ls_wR_factor_gt          0.1356
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.65450(2) 0.57970(2) 0.72724(3) 0.03108(12) Uani 1 1 d . . . . .
Si2 Si 0.82179(7) 0.65559(3) 0.87989(10) 0.0390(2) Uani 1 1 d . . . . .
Si1 Si 0.90026(8) 0.61020(3) 0.61155(10) 0.0443(2) Uani 1 1 d . . . . .
N3 N 0.5921(2) 0.58325(7) 0.4998(3) 0.0303(4) Uani 1 1 d . . . . .
N6 N 0.8051(2) 0.61274(7) 0.7415(3) 0.0333(5) Uani 1 1 d . . . . .
N1 N 0.7185(2) 0.51368(7) 0.6807(3) 0.0337(5) Uani 1 1 d . . . . .
N2 N 0.6133(2) 0.50802(7) 0.4074(3) 0.0345(5) Uani 1 1 d . . . . .
N4 N 0.5241(2) 0.65617(7) 0.5203(3) 0.0371(5) Uani 1 1 d . . . . .
N5 N 0.3364(2) 0.69416(8) 0.4507(3) 0.0407(5) Uani 1 1 d . . . . .
C13 C 0.5290(2) 0.62184(8) 0.4342(3) 0.0302(5) Uani 1 1 d . . . . .
C12 C 0.4763(2) 0.61232(8) 0.2666(3) 0.0319(5) Uani 1 1 d . . . . .
C6 C 0.5763(2) 0.54955(8) 0.3928(3) 0.0306(5) Uani 1 1 d . . . . .
C7 C 0.5044(3) 0.56761(9) 0.2445(3) 0.0341(5) Uani 1 1 d . . . . .
C5 C 0.6831(2) 0.49045(8) 0.5440(3) 0.0332(5) Uani 1 1 d . . . . .
C4 C 0.7173(3) 0.44515(9) 0.5344(4) 0.0402(6) Uani 1 1 d . . . . .
H4 H 0.6916 0.4292 0.4389 0.048 Uiso 1 1 calc R U . . .
C14 C 0.4556(3) 0.69404(9) 0.4509(3) 0.0366(6) Uani 1 1 d . . . . .
C11 C 0.4097(3) 0.63753(9) 0.1427(3) 0.0375(6) Uani 1 1 d . . . . .
H11 H 0.3904 0.6683 0.1557 0.045 Uiso 1 1 calc R U . . .
C10 C 0.3724(3) 0.61611(11) -0.0011(3) 0.0447(7) Uani 1 1 d . . . . .
H10 H 0.3277 0.6328 -0.0878 0.054 Uiso 1 1 calc R U . . .
C18 C 0.2693(3) 0.73012(10) 0.3883(4) 0.0474(7) Uani 1 1 d . . . . .
C1 C 0.7883(3) 0.49233(10) 0.8079(4) 0.0416(6) Uani 1 1 d . . . . .
C8 C 0.4638(3) 0.54609(10) 0.1027(3) 0.0458(7) Uani 1 1 d . . . . .
H8 H 0.4802 0.5150 0.0907 0.055 Uiso 1 1 calc R U . . .
C2 C 0.8238(3) 0.44812(11) 0.8006(4) 0.0478(7) Uani 1 1 d . . . . .
H2 H 0.8732 0.4341 0.8904 0.057 Uiso 1 1 calc R U . . .
C3 C 0.7877(3) 0.42392(10) 0.6624(5) 0.0485(8) Uani 1 1 d . . . . .
H3 H 0.8113 0.3933 0.6568 0.058 Uiso 1 1 calc R U . . .
C17 C 0.3203(4) 0.76530(10) 0.3223(4) 0.0574(9) Uani 1 1 d . . . . .
H17 H 0.2702 0.7898 0.2758 0.069 Uiso 1 1 calc R U . . .
C15 C 0.5146(3) 0.72897(10) 0.3925(4) 0.0474(7) Uani 1 1 d . . . . .
H15 H 0.6009 0.7282 0.3995 0.057 Uiso 1 1 calc R U . . .
C22 C 0.6997(4) 0.65328(12) 0.9945(4) 0.0561(8) Uani 1 1 d . . . . .
H22A H 0.6186 0.6559 0.9234 0.084 Uiso 1 1 calc R U . . .
H22B H 0.7114 0.6782 1.0696 0.084 Uiso 1 1 calc R U . . .
H22C H 0.7052 0.6246 1.0508 0.084 Uiso 1 1 calc R U . . .
C9 C 0.3984(3) 0.57133(12) -0.0216(4) 0.0493(8) Uani 1 1 d . . . . .
H9 H 0.3713 0.5577 -0.1212 0.059 Uiso 1 1 calc R U . . .
C16 C 0.4444(4) 0.76488(11) 0.3241(4) 0.0585(9) Uani 1 1 d . . . . .
H16 H 0.4808 0.7889 0.2790 0.070 Uiso 1 1 calc R U . . .
C19 C 0.8230(4) 0.51817(12) 0.9589(4) 0.0574(9) Uani 1 1 d . . . . .
H19A H 0.8715 0.5447 0.9443 0.086 Uiso 1 1 calc R U . . .
H19B H 0.8718 0.4988 1.0401 0.086 Uiso 1 1 calc R U . . .
H19C H 0.7481 0.5278 0.9906 0.086 Uiso 1 1 calc R U . . .
C21 C 0.8117(4) 0.71262(11) 0.7854(5) 0.0564(8) Uani 1 1 d . . . . .
H21A H 0.8771 0.7157 0.7279 0.085 Uiso 1 1 calc R U . . .
H21B H 0.8214 0.7360 0.8660 0.085 Uiso 1 1 calc R U . . .
H21C H 0.7314 0.7160 0.7130 0.085 Uiso 1 1 calc R U . . .
C23 C 0.9690(4) 0.65160(14) 1.0332(5) 0.0698(11) Uani 1 1 d . . . . .
H23A H 0.9746 0.6218 1.0826 0.105 Uiso 1 1 calc R U . . .
H23B H 0.9700 0.6749 1.1124 0.105 Uiso 1 1 calc R U . . .
H23C H 1.0391 0.6560 0.9847 0.105 Uiso 1 1 calc R U . . .
C20 C 0.1363(4) 0.72968(15) 0.3944(5) 0.0733(12) Uani 1 1 d . . . . .
H20A H 0.1016 0.6998 0.3645 0.110 Uiso 1 1 calc R U . . .
H20B H 0.0916 0.7523 0.3219 0.110 Uiso 1 1 calc R U . . .
H20C H 0.1286 0.7367 0.5007 0.110 Uiso 1 1 calc R U . . .
C24 C 1.0568(4) 0.63259(16) 0.6985(6) 0.0738(12) Uani 1 1 d . . . . .
H24A H 1.0499 0.6634 0.7356 0.111 Uiso 1 1 calc R U . . .
H24B H 1.1062 0.6326 0.6193 0.111 Uiso 1 1 calc R U . . .
H24C H 1.0966 0.6135 0.7864 0.111 Uiso 1 1 calc R U . . .
C25 C 0.9198(6) 0.55623(19) 0.5295(9) 0.125(3) Uani 1 1 d . . . . .
H25A H 0.9270 0.5330 0.6105 0.187 Uiso 1 1 calc R U . . .
H25B H 0.9946 0.5564 0.4887 0.187 Uiso 1 1 calc R U . . .
H25C H 0.8485 0.5497 0.4445 0.187 Uiso 1 1 calc R U . . .
C26 C 0.8379(4) 0.6497(2) 0.4399(5) 0.0880(15) Uani 1 1 d . . . . .
H26A H 0.7524 0.6417 0.3924 0.132 Uiso 1 1 calc R U . . .
H26B H 0.8879 0.6468 0.3620 0.132 Uiso 1 1 calc R U . . .
H26C H 0.8415 0.6809 0.4775 0.132 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N6 1.924(2) . ?
Ge1 N3 1.965(2) . ?
Ge1 N1 2.156(2) . ?
Si2 N6 1.740(2) . ?
Si2 C22 1.868(4) . ?
Si2 C23 1.877(4) . ?
Si2 C21 1.877(3) . ?
Si1 N6 1.727(2) . ?
Si1 C25 1.790(5) . ?
Si1 C24 1.863(4) . ?
Si1 C26 1.913(5) . ?
N3 C6 1.357(3) . ?
N3 C13 1.399(3) . ?
N1 C5 1.363(4) . ?
N1 C1 1.366(3) . ?
N2 C6 1.297(3) . ?
N2 C5 1.378(4) . ?
N4 C13 1.277(3) . ?
N4 C14 1.418(3) . ?
N5 C14 1.328(4) . ?
N5 C18 1.347(4) . ?
C13 C12 1.484(4) . ?
C12 C7 1.387(4) . ?
C12 C11 1.390(4) . ?
C6 C7 1.469(4) . ?
C7 C8 1.382(4) . ?
C5 C4 1.405(4) . ?
C4 C3 1.371(5) . ?
C14 C15 1.387(4) . ?
C11 C10 1.392(4) . ?
C10 C9 1.381(5) . ?
C18 C17 1.378(5) . ?
C18 C20 1.496(6) . ?
C1 C2 1.376(4) . ?
C1 C19 1.506(5) . ?
C8 C9 1.388(5) . ?
C2 C3 1.390(5) . ?
C17 C16 1.381(6) . ?
C15 C16 1.378(5) . ?

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
N6 Ge1 N3 98.19(9) . . ?
N6 Ge1 N1 98.88(9) . . ?
N3 Ge1 N1 84.95(8) . . ?
N6 Si2 C22 111.95(14) . . ?
N6 Si2 C23 113.20(15) . . ?
C22 Si2 C23 103.6(2) . . ?
N6 Si2 C21 111.32(14) . . ?
C22 Si2 C21 107.06(17) . . ?
C23 Si2 C21 109.24(19) . . ?
N6 Si1 C25 117.00(18) . . ?
N6 Si1 C24 111.82(16) . . ?
C25 Si1 C24 107.3(3) . . ?
N6 Si1 C26 109.05(18) . . ?
C25 Si1 C26 106.7(3) . . ?
C24 Si1 C26 104.2(2) . . ?
C6 N3 C13 110.0(2) . . ?
C6 N3 Ge1 128.77(17) . . ?
C13 N3 Ge1 119.55(16) . . ?
Si1 N6 Si2 120.59(13) . . ?
Si1 N6 Ge1 126.30(13) . . ?
Si2 N6 Ge1 111.87(12) . . ?
C5 N1 C1 119.0(2) . . ?
C5 N1 Ge1 125.76(17) . . ?
C1 N1 Ge1 114.71(19) . . ?
C6 N2 C5 123.4(2) . . ?
C13 N4 C14 117.9(2) . . ?
C14 N5 C18 117.8(3) . . ?
N4 C13 N3 119.5(2) . . ?
N4 C13 C12 132.8(2) . . ?
N3 C13 C12 107.7(2) . . ?
C7 C12 C11 120.2(2) . . ?
C7 C12 C13 105.6(2) . . ?
C11 C12 C13 134.2(2) . . ?
N2 C6 N3 130.1(2) . . ?
N2 C6 C7 122.1(2) . . ?
N3 C6 C7 107.8(2) . . ?
C8 C7 C12 122.0(3) . . ?
C8 C7 C6 129.3(3) . . ?
C12 C7 C6 108.7(2) . . ?
N1 C5 N2 124.8(2) . . ?
N1 C5 C4 120.5(3) . . ?
N2 C5 C4 114.7(3) . . ?
C3 C4 C5 120.2(3) . . ?
N5 C14 C15 123.8(3) . . ?
N5 C14 N4 116.4(3) . . ?
C15 C14 N4 119.8(3) . . ?
C12 C11 C10 117.6(3) . . ?
C9 C10 C11 122.0(3) . . ?
N5 C18 C17 121.9(3) . . ?
N5 C18 C20 116.3(3) . . ?
C17 C18 C20 121.9(3) . . ?
N1 C1 C2 121.4(3) . . ?
N1 C1 C19 118.1(3) . . ?
C2 C1 C19 120.5(3) . . ?
C7 C8 C9 117.8(3) . . ?
C1 C2 C3 120.2(3) . . ?
C4 C3 C2 118.6(3) . . ?
C18 C17 C16 119.7(3) . . ?
C16 C15 C14 118.0(3) . . ?
C10 C9 C8 120.4(3) . . ?
C15 C16 C17 118.8(3) . . ?

_refine_diff_density_max         1.481
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.073

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jcm12123a
_database_code_depnum_ccdc_archive 'CCDC 2403135'
loop_
_audit_author_name
_audit_author_address
'Jesus Campos'
;CSIC
Spain
;
_audit_update_record             
;
2024-11-15 deposited with the CCDC.	2025-01-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H48 Ge2 N10 O'
_chemical_formula_weight         926.14

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'
Ge Ge 0.1547 1.8001 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/n'
_space_group_name_Hall           '-P 2yac'

_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+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   13.3849(5)
_cell_length_b                   8.7408(3)
_cell_length_c                   18.0043(6)
_cell_angle_alpha                90
_cell_angle_beta                 95.1690(10)
_cell_angle_gamma                90
_cell_volume                     2097.84(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    9803
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      29.15

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_F_000             956
_exptl_transmission_factor_min   .
_exptl_transmission_factor_max   .
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    1.484
_shelx_estimated_absorpt_T_min   .
_shelx_estimated_absorpt_T_max   .
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6219
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   ' Apex3 v2016.9-0 (Bruker, 2016)'
_exptl_absorpt_special_details   .
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'IuS 3.0 Microfocus Source'
_diffrn_measurement_device_type  'Bruker D8Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean .
_diffrn_reflns_number            53015
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.272
_diffrn_reflns_theta_max         29.135
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5647
_reflns_number_gt                4589
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker APEX3'
_computing_data_reduction        'Bruker APEX3'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0487P)²+2.3204P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5647
_refine_ls_number_parameters     278
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0408
_refine_ls_wR_factor_ref         0.1092
_refine_ls_wR_factor_gt          0.0995
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.70989(2) 0.57691(3) 0.64139(2) 0.02822(9) Uani 1 1 d . . . . .
C1 C 0.6780(2) 0.5789(3) 0.47182(16) 0.0417(6) Uani 1 1 d . . . . .
C2 C 0.6385(2) 0.5445(4) 0.40086(16) 0.0474(7) Uani 1 1 d . . . . .
H2 H 0.6482 0.6125 0.3610 0.057 Uiso 1 1 calc R U . . .
C3 C 0.5846(3) 0.4111(4) 0.38724(17) 0.0540(8) Uani 1 1 d . . . . .
H3 H 0.5580 0.3856 0.3381 0.065 Uiso 1 1 calc R U . . .
C4 C 0.5704(2) 0.3171(4) 0.44536(17) 0.0495(7) Uani 1 1 d . . . . .
H4 H 0.5337 0.2249 0.4365 0.059 Uiso 1 1 calc R U . . .
C5 C 0.60888(18) 0.3533(3) 0.51827(14) 0.0356(5) Uani 1 1 d . . . . .
C6 C 0.61204(17) 0.2698(3) 0.64242(14) 0.0310(5) Uani 1 1 d . . . . .
C7 C 0.60622(18) 0.1451(3) 0.69701(15) 0.0334(5) Uani 1 1 d . . . . .
C8 C 0.5704(2) -0.0035(3) 0.68842(18) 0.0441(7) Uani 1 1 d . . . . .
H8 H 0.5405 -0.0389 0.6417 0.053 Uiso 1 1 calc R U . . .
C9 C 0.5798(2) -0.0981(3) 0.7502(2) 0.0509(8) Uani 1 1 d . . . . .
H9 H 0.5556 -0.2002 0.7459 0.061 Uiso 1 1 calc R U . . .
C10 C 0.6239(2) -0.0469(3) 0.8183(2) 0.0466(7) Uani 1 1 d . . . . .
H10 H 0.6294 -0.1142 0.8599 0.056 Uiso 1 1 calc R U . . .
C11 C 0.6602(2) 0.1022(3) 0.82654(17) 0.0386(6) Uani 1 1 d . . . . .
H11 H 0.6904 0.1377 0.8731 0.046 Uiso 1 1 calc R U . . .
C12 C 0.65089(17) 0.1962(3) 0.76495(14) 0.0312(5) Uani 1 1 d . . . . .
C13 C 0.68983(16) 0.3566(3) 0.75406(13) 0.0260(4) Uani 1 1 d . . . . .
C14 C 0.57731(18) 0.4986(3) 0.83014(13) 0.0284(5) Uani 1 1 d . . . . .
C15 C 0.48874(19) 0.4355(3) 0.79501(15) 0.0345(5) Uani 1 1 d . . . . .
H15 H 0.4912 0.3672 0.7542 0.041 Uiso 1 1 calc R U . . .
C16 C 0.3987(2) 0.4742(3) 0.82065(18) 0.0431(6) Uani 1 1 d . . . . .
H16 H 0.3383 0.4306 0.7983 0.052 Uiso 1 1 calc R U . . .
C17 C 0.3955(2) 0.5764(4) 0.87894(19) 0.0482(7) Uani 1 1 d . . . . .
H17 H 0.3333 0.6063 0.8961 0.058 Uiso 1 1 calc R U . . .
C18 C 0.4852(2) 0.6340(3) 0.91168(17) 0.0421(6) Uani 1 1 d . . . . .
C19 C 0.7381(2) 0.7238(4) 0.48432(18) 0.0525(8) Uani 1 1 d . . . . .
H19A H 0.7854 0.7113 0.5295 0.063 Uiso 1 1 calc R U . . .
H19B H 0.7784 0.7398 0.4415 0.063 Uiso 1 1 calc R U . . .
C20 C 0.6751(3) 0.8629(5) 0.4935(3) 0.0721(11) Uani 1 1 d . . . . .
H20A H 0.6281 0.8764 0.4491 0.108 Uiso 1 1 calc R U . . .
H20B H 0.7185 0.9531 0.5002 0.108 Uiso 1 1 calc R U . . .
H20C H 0.6375 0.8504 0.5374 0.108 Uiso 1 1 calc R U . . .
C21 C 0.4873(3) 0.7430(4) 0.9771(2) 0.0625(9) Uani 1 1 d . . . . .
H21A H 0.4945 0.6821 1.0237 0.075 Uiso 1 1 calc R U . . .
H21B H 0.5477 0.8083 0.9767 0.075 Uiso 1 1 calc R U . . .
C22 C 0.4007(4) 0.8414(8) 0.9793(4) 0.148(3) Uani 1 1 d . . . . .
H22A H 0.3905 0.8991 0.9326 0.222 Uiso 1 1 calc R U . . .
H22B H 0.4118 0.9128 1.0213 0.222 Uiso 1 1 calc R U . . .
H22C H 0.3412 0.7790 0.9856 0.222 Uiso 1 1 calc R U . . .
C23 C 0.1976(3) -0.0776(5) 0.7576(4) 0.1029(19) Uani 1 1 d . . . . .
H23A H 0.1903 -0.1031 0.8104 0.124 Uiso 1 1 calc R U . . .
H23B H 0.1583 -0.1516 0.7251 0.124 Uiso 1 1 calc R U . . .
O1 O 0.2500 0.1755(4) 0.7500 0.1011(17) Uani 1 2 d S T P . .
N1 N 0.66374(15) 0.4840(3) 0.53087(12) 0.0342(5) Uani 1 1 d . . . . .
N2 N 0.58949(16) 0.2478(3) 0.57114(13) 0.0375(5) Uani 1 1 d . . . . .
N3 N 0.64501(14) 0.3977(2) 0.67907(11) 0.0275(4) Uani 1 1 d . . . . .
N4 N 0.67284(14) 0.4677(2) 0.81115(11) 0.0277(4) Uani 1 1 d . . . . .
N5 N 0.57442(16) 0.5966(2) 0.88769(12) 0.0344(5) Uani 1 1 d . . . . .
C24 C 0.1648(3) 0.0839(5) 0.7401(4) 0.114(2) Uani 1 1 d . . . . .
H24A H 0.1343 0.0913 0.6881 0.137 Uiso 1 1 calc R U . . .
H24B H 0.1146 0.1169 0.7739 0.137 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N3 1.943(2) . ?
Ge1 N4 1.9656(19) 2_656 ?
Ge1 N1 2.186(2) . ?
C1 C2 1.371(4) . ?
C1 N1 1.376(4) . ?
C1 C19 1.507(4) . ?
C2 C3 1.381(5) . ?
C3 C4 1.357(5) . ?
C4 C5 1.402(4) . ?
C5 N1 1.366(3) . ?
C5 N2 1.367(4) . ?
C6 N2 1.306(3) . ?
C6 N3 1.351(3) . ?
C6 C7 1.475(4) . ?
C7 C12 1.386(4) . ?
C7 C8 1.388(3) . ?
C8 C9 1.383(5) . ?
C9 C10 1.387(5) . ?
C10 C11 1.394(4) . ?
C11 C12 1.377(4) . ?
C12 C13 1.515(3) . ?
C13 N4 1.447(3) . ?
C13 N3 1.472(3) . ?
C13 C13 1.630(4) 2_656 ?
C14 N5 1.347(3) . ?
C14 N4 1.380(3) . ?
C14 C15 1.405(3) . ?
C15 C16 1.371(4) . ?
C16 C17 1.382(4) . ?
C17 C18 1.384(4) . ?
C18 N5 1.346(3) . ?
C18 C21 1.514(4) . ?
C19 C20 1.497(5) . ?
C21 C22 1.447(6) . ?
C23 C23 1.453(9) 2_556 ?
C23 C24 1.503(6) . ?
O1 C24 1.391(5) 2_556 ?
O1 C24 1.391(5) . ?
N4 Ge1 1.9656(19) 2_656 ?

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
N3 Ge1 N4 79.70(8) . 2_656 ?
N3 Ge1 N1 85.39(8) . . ?
N4 Ge1 N1 111.36(8) 2_656 . ?
C2 C1 N1 121.3(3) . . ?
C2 C1 C19 118.7(3) . . ?
N1 C1 C19 120.1(2) . . ?
C1 C2 C3 120.1(3) . . ?
C4 C3 C2 118.8(3) . . ?
C3 C4 C5 121.3(3) . . ?
N1 C5 N2 125.6(2) . . ?
N1 C5 C4 119.4(3) . . ?
N2 C5 C4 115.0(3) . . ?
N2 C6 N3 129.7(2) . . ?
N2 C6 C7 121.6(2) . . ?
N3 C6 C7 108.7(2) . . ?
C12 C7 C8 121.1(3) . . ?
C12 C7 C6 107.8(2) . . ?
C8 C7 C6 131.0(3) . . ?
C9 C8 C7 117.7(3) . . ?
C8 C9 C10 121.2(3) . . ?
C9 C10 C11 120.8(3) . . ?
C12 C11 C10 117.8(3) . . ?
C11 C12 C7 121.3(2) . . ?
C11 C12 C13 130.5(2) . . ?
C7 C12 C13 108.1(2) . . ?
N4 C13 N3 114.26(18) . . ?
N4 C13 C12 116.8(2) . . ?
N3 C13 C12 103.17(18) . . ?
N4 C13 C13 106.47(17) . 2_656 ?
N3 C13 C13 104.0(2) . 2_656 ?
C12 C13 C13 111.45(12) . 2_656 ?
N5 C14 N4 114.0(2) . . ?
N5 C14 C15 120.9(2) . . ?
N4 C14 C15 125.1(2) . . ?
C16 C15 C14 118.9(2) . . ?
C15 C16 C17 120.2(3) . . ?
C16 C17 C18 118.2(3) . . ?
N5 C18 C17 122.4(3) . . ?
N5 C18 C21 116.6(3) . . ?
C17 C18 C21 121.0(3) . . ?
C20 C19 C1 113.6(3) . . ?
C22 C21 C18 115.9(4) . . ?
C23 C23 C24 103.2(3) 2_556 . ?
C24 O1 C24 109.7(5) 2_556 . ?
C5 N1 C1 119.1(2) . . ?
C5 N1 Ge1 124.45(17) . . ?
C1 N1 Ge1 115.58(18) . . ?
C6 N2 C5 122.9(2) . . ?
C6 N3 C13 109.54(19) . . ?
C6 N3 Ge1 129.26(17) . . ?
C13 N3 Ge1 111.03(14) . . ?
C14 N4 C13 121.06(19) . . ?
C14 N4 Ge1 121.26(16) . 2_656 ?
C13 N4 Ge1 117.66(14) . 2_656 ?
C18 N5 C14 119.3(2) . . ?
O1 C24 C23 107.1(4) . . ?

_refine_diff_density_max         0.840
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.069

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jcm09723a_sq
_database_code_depnum_ccdc_archive 'CCDC 2403140'
loop_
_audit_author_name
_audit_author_address
'Jesus Campos'
;CSIC
Spain
;
_audit_update_record             
;
2024-11-15 deposited with the CCDC.	2025-01-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H24 Ge2 N10'
_chemical_formula_weight         741.83

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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.1482(17)
_cell_length_b                   8.6859(6)
_cell_length_c                   22.075(2)
_cell_angle_alpha                90
_cell_angle_beta                 93.619(3)
_cell_angle_gamma                90
_cell_volume                     4047.0(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    9507
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      27.49

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_F_000             1496
_exptl_transmission_factor_min   .
_exptl_transmission_factor_max   .
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    1.521
_shelx_estimated_absorpt_T_min   .
_shelx_estimated_absorpt_T_max   .
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6503
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   ' Apex3 v2016.9-0 (Bruker, 2016)'
_exptl_absorpt_special_details   .
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'IuS 3.0 Microfocus Source'
_diffrn_measurement_device_type  'Bruker D8Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean .
_diffrn_reflns_number            27806
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_av_R_equivalents  0.1129
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.930
_diffrn_reflns_theta_max         25.247
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3669
_reflns_number_gt                2859
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker APEX3'
_computing_data_reduction        'Bruker APEX3'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 -0.024 0.500 321 156 ' '
2 0.250 -0.027 1.000 321 155 ' '
3 0.750 -0.041 0.000 321 155 ' '
4 0.750 -0.019 0.500 321 156 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The unit cell contains 16 pentane molecules which have
 been treated as a diffuse contribution to the overall scattering
 without specific atom positions by SQUEEZE/PLATON.'
;




_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1161P)²+261.4418P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0070(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3669
_refine_ls_number_parameters     218
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1428
_refine_ls_R_factor_gt           0.1224
_refine_ls_wR_factor_ref         0.3440
_refine_ls_wR_factor_gt          0.3304
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.50021(6) 0.08129(14) 0.84513(6) 0.0289(6) Uani 1 1 d . . . . .
N3 N 0.6323(4) 0.0588(11) 0.8532(4) 0.025(2) Uani 1 1 d . . . . .
N2 N 0.5601(4) 0.1801(11) 0.7937(4) 0.026(2) Uani 1 1 d . . . . .
N5 N 0.4947(5) 0.2081(11) 0.5731(4) 0.031(2) Uani 1 1 d . . . . .
N1 N 0.5508(5) 0.2519(12) 0.6868(4) 0.030(2) Uani 1 1 d . . . . .
N4 N 0.5711(6) 0.4023(13) 0.5978(5) 0.037(3) Uani 1 1 d . . . . .
C7 C 0.5814(5) 0.5060(14) 0.7021(6) 0.029(3) Uani 1 1 d . . . . .
C13 C 0.6892(6) 0.0040(19) 0.8715(7) 0.043(3) Uani 1 1 d . . . . .
H13 H 0.6937 -0.0555 0.9076 0.052 Uiso 1 1 calc R U . . .
C2 C 0.5669(6) 0.4526(13) 0.7581(6) 0.028(3) Uani 1 1 d . . . . .
C3 C 0.5733(6) 0.5412(15) 0.8090(6) 0.034(3) Uani 1 1 d . . . . .
H3 H 0.5630 0.5018 0.8473 0.041 Uiso 1 1 calc R U . . .
C1 C 0.5384(6) 0.2920(13) 0.7489(5) 0.027(3) Uani 1 1 d . . . . .
C10 C 0.6741(6) 0.1768(17) 0.7681(7) 0.045(4) Uani 1 1 d . . . . .
H10 H 0.6672 0.2394 0.7330 0.054 Uiso 1 1 calc R U . . .
C14 C 0.5360(7) 0.3152(14) 0.5579(6) 0.036(3) Uani 1 1 d . . . . .
C9 C 0.6237(6) 0.1339(15) 0.8055(6) 0.034(3) Uani 1 1 d . . . . .
C6 C 0.6041(6) 0.6558(16) 0.6958(7) 0.039(3) Uani 1 1 d . . . . .
H6 H 0.6161 0.6926 0.6576 0.046 Uiso 1 1 calc R U . . .
C4 C 0.5951(6) 0.6898(15) 0.8035(6) 0.037(3) Uani 1 1 d . . . . .
H4 H 0.6010 0.7532 0.8384 0.045 Uiso 1 1 calc R U . . .
C8 C 0.5672(6) 0.3823(14) 0.6575(6) 0.031(3) Uani 1 1 d . . . . .
C18 C 0.4529(6) 0.1446(16) 0.5292(6) 0.037(3) Uani 1 1 d . . . . .
H18 H 0.4209 0.0767 0.5414 0.045 Uiso 1 1 calc R U . . .
C5 C 0.6086(6) 0.7478(15) 0.7461(7) 0.042(3) Uani 1 1 d . . . . .
H5 H 0.6209 0.8524 0.7424 0.051 Uiso 1 1 calc R U . . .
C12 C 0.7437(7) 0.0329(19) 0.8377(8) 0.052(4) Uani 1 1 d . . . . .
H12 H 0.7846 -0.0060 0.8497 0.062 Uiso 1 1 calc R U . . .
C15 C 0.5441(7) 0.3471(17) 0.4959(6) 0.044(3) Uani 1 1 d . . . . .
H15 H 0.5767 0.4141 0.4844 0.053 Uiso 1 1 calc R U . . .
C17 C 0.4560(7) 0.1754(17) 0.4703(6) 0.041(3) Uani 1 1 d . . . . .
H17 H 0.4272 0.1296 0.4408 0.049 Uiso 1 1 calc R U . . .
C16 C 0.5038(9) 0.2790(18) 0.4528(6) 0.055(5) Uani 1 1 d . . . . .
H16 H 0.5077 0.3010 0.4111 0.066 Uiso 1 1 calc R U . . .
C11 C 0.7321(8) 0.122(2) 0.7865(8) 0.061(5) Uani 1 1 d . . . . .
H11 H 0.7667 0.1458 0.7628 0.073 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 1.940(10) 2_656 ?
Ge1 N2 1.952(10) . ?
Ge1 N5 2.111(10) 2_656 ?
N3 C9 1.241(17) . ?
N3 C13 1.333(16) . ?
N2 C9 1.413(16) . ?
N2 C1 1.441(14) . ?
N5 C14 1.333(17) . ?
N5 C18 1.386(17) . ?
N5 Ge1 2.111(10) 2_656 ?
N1 C8 1.359(16) . ?
N1 C1 1.454(15) . ?
N1 Ge1 1.940(10) 2_656 ?
N4 C8 1.339(16) . ?
N4 C14 1.348(17) . ?
C7 C2 1.374(17) . ?
C7 C6 1.397(18) . ?
C7 C8 1.475(18) . ?
C13 C12 1.43(2) . ?
C13 H13 0.9500 . ?
C2 C3 1.361(17) . ?
C2 C1 1.528(16) . ?
C3 C4 1.378(18) . ?
C3 H3 0.9500 . ?
C1 C1 1.63(2) 2_656 ?
C10 C11 1.35(2) . ?
C10 C9 1.438(19) . ?
C10 H10 0.9500 . ?
C14 C15 1.418(18) . ?
C6 C5 1.37(2) . ?
C6 H6 0.9500 . ?
C4 C5 1.41(2) . ?
C4 H4 0.9500 . ?
C18 C17 1.333(19) . ?
C18 H18 0.9500 . ?
C5 H5 0.9500 . ?
C12 C11 1.38(2) . ?
C12 H12 0.9500 . ?
C15 C16 1.37(2) . ?
C15 H15 0.9500 . ?
C17 C16 1.42(2) . ?
C17 H17 0.9500 . ?
C16 H16 0.9500 . ?
C11 H11 0.9500 . ?

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 N2 79.6(4) 2_656 . ?
N1 Ge1 N5 84.7(4) 2_656 2_656 ?
N2 Ge1 N5 105.6(4) . 2_656 ?
C9 N3 C13 121.7(12) . . ?
C9 N2 C1 125.2(10) . . ?
C9 N2 Ge1 114.4(8) . . ?
C1 N2 Ge1 120.4(7) . . ?
C14 N5 C18 120.0(11) . . ?
C14 N5 Ge1 125.5(9) . 2_656 ?
C18 N5 Ge1 112.7(8) . 2_656 ?
C8 N1 C1 108.3(10) . . ?
C8 N1 Ge1 128.1(9) . 2_656 ?
C1 N1 Ge1 113.3(7) . 2_656 ?
C8 N4 C14 120.3(11) . . ?
C2 C7 C6 120.1(12) . . ?
C2 C7 C8 107.9(10) . . ?
C6 C7 C8 132.0(12) . . ?
N3 C13 C12 121.3(13) . . ?
N3 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
C3 C2 C7 122.4(11) . . ?
C3 C2 C1 130.2(11) . . ?
C7 C2 C1 107.2(10) . . ?
C2 C3 C4 118.2(13) . . ?
C2 C3 H3 120.9 . . ?
C4 C3 H3 120.9 . . ?
N2 C1 N1 114.7(10) . . ?
N2 C1 C2 114.7(10) . . ?
N1 C1 C2 104.6(9) . . ?
N2 C1 C1 104.7(9) . 2_656 ?
N1 C1 C1 105.6(11) . 2_656 ?
C2 C1 C1 112.4(7) . 2_656 ?
C11 C10 C9 115.2(14) . . ?
C11 C10 H10 122.4 . . ?
C9 C10 H10 122.4 . . ?
N5 C14 N4 124.7(12) . . ?
N5 C14 C15 120.0(12) . . ?
N4 C14 C15 115.2(12) . . ?
N3 C9 N2 113.1(11) . . ?
N3 C9 C10 123.3(12) . . ?
N2 C9 C10 123.5(12) . . ?
C5 C6 C7 118.0(13) . . ?
C5 C6 H6 121.0 . . ?
C7 C6 H6 121.0 . . ?
C3 C4 C5 120.2(12) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
N4 C8 N1 127.6(12) . . ?
N4 C8 C7 122.7(11) . . ?
N1 C8 C7 109.8(10) . . ?
C17 C18 N5 122.3(13) . . ?
C17 C18 H18 118.9 . . ?
N5 C18 H18 118.9 . . ?
C6 C5 C4 120.9(12) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C11 C12 C13 114.6(13) . . ?
C11 C12 H12 122.7 . . ?
C13 C12 H12 122.7 . . ?
C16 C15 C14 118.5(13) . . ?
C16 C15 H15 120.7 . . ?
C14 C15 H15 120.7 . . ?
C18 C17 C16 118.1(13) . . ?
C18 C17 H17 120.9 . . ?
C16 C17 H17 120.9 . . ?
C15 C16 C17 120.4(13) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C10 C11 C12 123.7(15) . . ?
C10 C11 H11 118.1 . . ?
C12 C11 H11 118.1 . . ?

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
C9 N3 C13 C12 2(2) . . . . ?
C6 C7 C2 C3 0.6(19) . . . . ?
C8 C7 C2 C3 -178.3(12) . . . . ?
C6 C7 C2 C1 175.3(11) . . . . ?
C8 C7 C2 C1 -3.6(13) . . . . ?
C7 C2 C3 C4 0.1(19) . . . . ?
C1 C2 C3 C4 -173.4(12) . . . . ?
C9 N2 C1 N1 60.9(15) . . . . ?
Ge1 N2 C1 N1 -120.3(9) . . . . ?
C9 N2 C1 C2 -60.1(15) . . . . ?
Ge1 N2 C1 C2 118.7(9) . . . . ?
C9 N2 C1 C1 176.2(10) . . . 2_656 ?
Ge1 N2 C1 C1 -5.0(11) . . . 2_656 ?
C8 N1 C1 N2 -141.8(10) . . . . ?
Ge1 N1 C1 N2 70.0(11) 2_656 . . . ?
C8 N1 C1 C2 -15.3(13) . . . . ?
Ge1 N1 C1 C2 -163.5(7) 2_656 . . . ?
C8 N1 C1 C1 103.5(8) . . . 2_656 ?
Ge1 N1 C1 C1 -44.7(8) 2_656 . . 2_656 ?
C3 C2 C1 N2 -48.0(18) . . . . ?
C7 C2 C1 N2 137.8(11) . . . . ?
C3 C2 C1 N1 -174.4(13) . . . . ?
C7 C2 C1 N1 11.4(13) . . . . ?
C3 C2 C1 C1 71.5(18) . . . 2_656 ?
C7 C2 C1 C1 -102.7(13) . . . 2_656 ?
C18 N5 C14 N4 168.3(12) . . . . ?
Ge1 N5 C14 N4 -27.8(18) 2_656 . . . ?
C18 N5 C14 C15 -9.8(19) . . . . ?
Ge1 N5 C14 C15 154.1(11) 2_656 . . . ?
C8 N4 C14 N5 2(2) . . . . ?
C8 N4 C14 C15 179.9(13) . . . . ?
C13 N3 C9 N2 179.3(12) . . . . ?
C13 N3 C9 C10 -4(2) . . . . ?
C1 N2 C9 N3 167.3(11) . . . . ?
Ge1 N2 C9 N3 -11.5(13) . . . . ?
C1 N2 C9 C10 -9.4(19) . . . . ?
Ge1 N2 C9 C10 171.8(11) . . . . ?
C11 C10 C9 N3 4(2) . . . . ?
C11 C10 C9 N2 -180.0(14) . . . . ?
C2 C7 C6 C5 -2.9(19) . . . . ?
C8 C7 C6 C5 175.7(13) . . . . ?
C2 C3 C4 C5 2(2) . . . . ?
C14 N4 C8 N1 27(2) . . . . ?
C14 N4 C8 C7 -154.0(12) . . . . ?
C1 N1 C8 N4 -166.8(12) . . . . ?
Ge1 N1 C8 N4 -24.7(19) 2_656 . . . ?
C1 N1 C8 C7 13.7(13) . . . . ?
Ge1 N1 C8 C7 155.8(8) 2_656 . . . ?
C2 C7 C8 N4 174.3(12) . . . . ?
C6 C7 C8 N4 -4(2) . . . . ?
C2 C7 C8 N1 -6.2(14) . . . . ?
C6 C7 C8 N1 175.0(13) . . . . ?
C14 N5 C18 C17 6.6(19) . . . . ?
Ge1 N5 C18 C17 -159.2(11) 2_656 . . . ?
C7 C6 C5 C4 5(2) . . . . ?
C3 C4 C5 C6 -4(2) . . . . ?
N3 C13 C12 C11 1(2) . . . . ?
N5 C14 C15 C16 7(2) . . . . ?
N4 C14 C15 C16 -170.9(14) . . . . ?
N5 C18 C17 C16 -1(2) . . . . ?
C14 C15 C16 C17 -2(2) . . . . ?
C18 C17 C16 C15 -1(2) . . . . ?
C9 C10 C11 C12 -1(3) . . . . ?
C13 C12 C11 C10 -1(3) . . . . ?

_refine_diff_density_max         1.869
_refine_diff_density_min         -1.594
_refine_diff_density_rms         0.251



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jcm07021a
_database_code_depnum_ccdc_archive 'CCDC 2403141'
loop_
_audit_author_name
_audit_author_address
'Jesus Campos'
;CSIC
Spain
;
_audit_update_record             
;
2024-11-15 deposited with the CCDC.	2025-01-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H72 Ge2 K2 N10 O6'
_chemical_formula_weight         1252.65


_vrf_RINTA01_jcm07021a           
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.188
RESPONSE: This was a small crystal of average quality. Nevertheless,
the model perfectly fits the expected structure and other spectroscopic
data that corroborate the validity of the model.
;

_vrf_PLAT020_jcm07021a           
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.188
RESPONSE: SAME as RINTA01.
;

_vrf_PLAT220_jcm07021a           
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        9.7 Ratio
RESPONSE: This is due to the disordered THF molecules, which are both
bound to the complex and as free solvent molecules.
;

_vrf_PLAT341_jcm07021a           
;
PROBLEM: Low Bond Precision on  C-C Bonds
RESPONSE: SAME as PLAT220 and RINTA01.
;


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'
K K 0.2009 0.2494 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   10.6413(11)
_cell_length_b                   15.2209(19)
_cell_length_c                   20.466(2)
_cell_angle_alpha                106.010(5)
_cell_angle_beta                 99.137(5)
_cell_angle_gamma                95.273(5)
_cell_volume                     3113.5(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    9682
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      28.71

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_F_000             1304
_exptl_transmission_factor_min   .
_exptl_transmission_factor_max   .
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    1.155
_shelx_estimated_absorpt_T_min   .
_shelx_estimated_absorpt_T_max   .
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4872
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   ' Apex3 v2016.9-0 (Bruker, 2016)'
_exptl_absorpt_special_details   .
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'IuS 3.0 Microfocus Source'
_diffrn_measurement_device_type  'Bruker D8Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean .
_diffrn_reflns_number            95283
_diffrn_reflns_av_unetI/netI     0.1156
_diffrn_reflns_av_R_equivalents  0.2319
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.958
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11291
_reflns_number_gt                6649
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker APEX3'
_computing_data_reduction        'Bruker APEX3'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0900P)²+8.8395P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11291
_refine_ls_number_parameters     721
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.1579
_refine_ls_R_factor_gt           0.0853
_refine_ls_wR_factor_ref         0.2228
_refine_ls_wR_factor_gt          0.1787
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.07472(7) 0.23395(5) 0.27708(4) 0.0355(2) Uani 1 1 d . . . . .
Ge2 Ge 0.33284(7) 0.35343(5) 0.19702(4) 0.0364(2) Uani 1 1 d . . . . .
K2 K 0.84266(17) 0.37876(13) 0.29491(11) 0.0593(6) Uani 1 1 d . . . . .
K1 K 0.5645(2) 0.07025(13) 0.22466(11) 0.0635(6) Uani 1 1 d . . . . .
N8 N 0.4101(5) 0.3030(4) 0.2707(3) 0.0325(13) Uani 1 1 d . . . . .
N7 N 0.2287(5) 0.3262(4) 0.3290(3) 0.0326(13) Uani 1 1 d . . . . .
N3 N 0.1754(5) 0.1470(4) 0.2283(3) 0.0343(14) Uani 1 1 d . . . . .
N1 N 0.0783(6) 0.1625(4) 0.3468(3) 0.0408(15) Uani 1 1 d . . . . .
N4 N 0.2104(5) 0.2385(4) 0.1509(3) 0.0334(14) Uani 1 1 d . . . . .
N9 N 0.6128(5) 0.2595(4) 0.2342(3) 0.0380(14) Uani 1 1 d . . . . .
C22 C 0.0897(5) 0.4210(4) 0.3813(3) 0.0241(14) Uani 1 1 d . . . . .
H22 H 0.0189 0.3792 0.3509 0.029 Uiso 1 1 calc R U . . .
N5 N 0.1414(6) 0.3065(5) 0.0650(3) 0.0452(16) Uani 1 1 d . . . . .
C31 C 0.5293(6) 0.2743(5) 0.2810(4) 0.0342(17) Uani 1 1 d . . . . .
N10 N 0.4785(6) 0.3076(4) 0.1468(3) 0.0399(15) Uani 1 1 d . . . . .
N2 N 0.1825(6) 0.0332(5) 0.2948(3) 0.0471(16) Uani 1 1 d . . . . .
O6 O 0.7451(6) 0.5283(4) 0.3593(4) 0.0737(19) Uani 1 1 d . . . . .
C6 C 0.2021(7) 0.0647(5) 0.2400(4) 0.0353(17) Uani 1 1 d . . . . .
C23 C 0.2129(7) 0.4055(5) 0.3788(3) 0.0341(16) Uani 1 1 d . . . . .
C13 C 0.2204(6) 0.1572(5) 0.1697(3) 0.0298(15) Uani 1 1 d . . . . .
N6 N 0.3192(7) 0.4674(5) 0.4243(4) 0.063(2) Uani 1 1 d . . . . .
C7 C 0.2634(7) 0.0183(5) 0.1852(4) 0.0370(17) Uani 1 1 d . . . . .
C11 C 0.3424(7) 0.0526(5) 0.0846(4) 0.0439(19) Uani 1 1 d . . . . .
H11 H 0.3552 0.0922 0.0569 0.053 Uiso 1 1 calc R U . . .
C26 C 0.4270(8) 0.2530(5) 0.4382(4) 0.0445(19) Uani 1 1 d . . . . .
H26 H 0.3520 0.2623 0.4575 0.053 Uiso 1 1 calc R U . . .
C14 C 0.1242(7) 0.2330(5) 0.0893(4) 0.0355(17) Uani 1 1 d . . . . .
C12 C 0.2764(7) 0.0793(5) 0.1424(4) 0.0370(17) Uani 1 1 d . . . . .
C24 C 0.3548(6) 0.3026(5) 0.3287(3) 0.0315(16) Uani 1 1 d . . . . .
C19 C 0.2930(8) 0.5454(6) 0.4730(4) 0.049(2) Uani 1 1 d . . . . .
H19 H 0.3617 0.5874 0.5050 0.059 Uiso 1 1 calc R U . . .
C30 C 0.5502(6) 0.2536(5) 0.3448(4) 0.0352(17) Uani 1 1 d . . . . .
O3 O 0.8880(8) 0.4769(6) 0.2102(4) 0.092(2) Uani 1 1 d . . . . .
C34 C 0.6555(9) 0.2573(6) 0.0607(5) 0.060(2) Uani 1 1 d . . . . .
H34 H 0.7171 0.2417 0.0321 0.072 Uiso 1 1 calc R U . . .
C25 C 0.4362(7) 0.2709(5) 0.3738(4) 0.0368(17) Uani 1 1 d . . . . .
C29 C 0.6525(7) 0.2223(5) 0.3813(4) 0.0440(19) Uani 1 1 d . . . . .
H29 H 0.7281 0.2115 0.3629 0.053 Uiso 1 1 calc R U . . .
C15 C 0.0291(7) 0.1573(6) 0.0562(4) 0.048(2) Uani 1 1 d . . . . .
H15 H 0.0196 0.1063 0.0742 0.058 Uiso 1 1 calc R U . . .
C21 C 0.0718(8) 0.4987(6) 0.4289(4) 0.053(2) Uani 1 1 d . . . . .
H21 H -0.0141 0.5101 0.4302 0.064 Uiso 1 1 calc R U . . .
C27 C 0.5284(9) 0.2223(6) 0.4715(4) 0.054(2) Uani 1 1 d . . . . .
H27 H 0.5229 0.2104 0.5143 0.064 Uiso 1 1 calc R U . . .
C5 C 0.1300(7) 0.0805(6) 0.3448(4) 0.046(2) Uani 1 1 d . . . . .
C28 C 0.6411(8) 0.2078(6) 0.4437(5) 0.055(2) Uani 1 1 d . . . . .
H28 H 0.7102 0.1876 0.4686 0.066 Uiso 1 1 calc R U . . .
C1 C 0.0238(7) 0.2051(6) 0.4021(4) 0.048(2) Uani 1 1 d . . . . .
H1 H -0.0122 0.2597 0.4013 0.058 Uiso 1 1 calc R U . . .
C8 C 0.3079(7) -0.0692(5) 0.1679(4) 0.046(2) Uani 1 1 d . . . . .
H8 H 0.2956 -0.1110 0.1940 0.055 Uiso 1 1 calc R U . . .
O1 O 0.5917(10) -0.0311(6) 0.3135(4) 0.102(3) Uani 1 1 d . . . . .
C20 C 0.1670(8) 0.5609(6) 0.4745(4) 0.053(2) Uani 1 1 d . . . . .
H20 H 0.1479 0.6138 0.5066 0.063 Uiso 1 1 calc R U . . .
C32 C 0.5850(7) 0.2721(5) 0.1708(4) 0.0398(18) Uani 1 1 d . . . . .
C10 C 0.3859(8) -0.0318(6) 0.0712(4) 0.053(2) Uani 1 1 d . . . . .
H10 H 0.4285 -0.0504 0.0333 0.063 Uiso 1 1 calc R U . . .
C9 C 0.3692(8) -0.0916(6) 0.1120(4) 0.051(2) Uani 1 1 d . . . . .
H9 H 0.4011 -0.1491 0.1008 0.061 Uiso 1 1 calc R U . . .
C3 C 0.0710(9) 0.0907(7) 0.4591(5) 0.063(3) Uani 1 1 d . . . . .
H3 H 0.0699 0.0670 0.4974 0.075 Uiso 1 1 calc R U . . .
C33 C 0.6752(8) 0.2480(6) 0.1253(5) 0.053(2) Uani 1 1 d . . . . .
H33 H 0.7506 0.2249 0.1411 0.064 Uiso 1 1 calc R U . . .
C35 C 0.5439(9) 0.2901(7) 0.0361(5) 0.063(3) Uani 1 1 d . . . . .
H35 H 0.5269 0.2943 -0.0099 0.076 Uiso 1 1 calc R U . . .
C2 C 0.0189(9) 0.1726(7) 0.4582(5) 0.063(3) Uani 1 1 d . . . . .
H2 H -0.0185 0.2045 0.4954 0.076 Uiso 1 1 calc R U . . .
C16 C -0.0515(8) 0.1587(7) -0.0040(5) 0.062(3) Uani 1 1 d . . . . .
H16 H -0.1169 0.1081 -0.0277 0.075 Uiso 1 1 calc R U . . .
C18 C 0.0593(9) 0.3034(7) 0.0063(4) 0.058(2) Uani 1 1 d . . . . .
H18 H 0.0698 0.3545 -0.0115 0.070 Uiso 1 1 calc R U . . .
C4 C 0.1235(9) 0.0455(7) 0.4040(5) 0.060(2) Uani 1 1 d . . . . .
H4 H 0.1565 -0.0103 0.4045 0.072 Uiso 1 1 calc R U . . .
C36 C 0.4593(8) 0.3159(6) 0.0802(4) 0.054(2) Uani 1 1 d . . . . .
H36 H 0.3853 0.3404 0.0644 0.065 Uiso 1 1 calc R U . . .
C17 C -0.0370(9) 0.2330(7) -0.0295(4) 0.061(2) Uani 1 1 d . . . . .
H17 H -0.0918 0.2353 -0.0703 0.073 Uiso 1 1 calc R U . . .
C44 C 0.7888(13) 0.5178(9) 0.1795(7) 0.100(4) Uani 1 1 d . . . . .
H44A H 0.7723 0.5729 0.2144 0.120 Uiso 1 1 calc R U . . .
H44B H 0.7085 0.4733 0.1629 0.120 Uiso 1 1 calc R U . . .
O2 O 0.7629(13) 0.0045(9) 0.1745(7) 0.179(5) Uani 1 1 d . U . . .
C47 C 0.5719(12) 0.6100(8) 0.3669(8) 0.109(5) Uani 1 1 d . . . . .
H47A H 0.5313 0.6189 0.4081 0.131 Uiso 1 1 calc R U . . .
H47B H 0.5092 0.6172 0.3281 0.131 Uiso 1 1 calc R U . . .
C48 C 0.6918(13) 0.6780(8) 0.3822(8) 0.101(4) Uani 1 1 d . . . . .
H48A H 0.6918 0.7321 0.4223 0.122 Uiso 1 1 calc R U . . .
H48B H 0.7023 0.6993 0.3416 0.122 Uiso 1 1 calc R U . . .
C46 C 0.6123(11) 0.5206(8) 0.3486(9) 0.113(5) Uani 1 1 d . . . . .
H46A H 0.5795 0.4837 0.3769 0.135 Uiso 1 1 calc R U . . .
H46B H 0.5759 0.4880 0.2992 0.135 Uiso 1 1 calc R U . . .
C49 C 0.7945(11) 0.6214(8) 0.3983(8) 0.115(5) Uani 1 1 d . . . . .
H49A H 0.8748 0.6417 0.3846 0.138 Uiso 1 1 calc R U . . .
H49B H 0.8129 0.6278 0.4484 0.138 Uiso 1 1 calc R U . . .
C41 C 0.9703(14) 0.4552(11) 0.1602(8) 0.123(5) Uani 1 1 d . . . . .
H41A H 0.9567 0.3878 0.1369 0.147 Uiso 1 1 calc R U . . .
H41B H 1.0616 0.4739 0.1836 0.147 Uiso 1 1 calc R U . . .
C42 C 0.9391(19) 0.5053(13) 0.1086(9) 0.155(8) Uani 1 1 d . . . . .
H42A H 1.0113 0.5539 0.1134 0.186 Uiso 1 1 calc R U . . .
H42B H 0.9242 0.4621 0.0611 0.186 Uiso 1 1 calc R U . . .
C40 C 0.6949(17) -0.0479(13) 0.3610(9) 0.145(6) Uani 1 1 d . U . . .
H40A H 0.7694 0.0011 0.3719 0.174 Uiso 1 1 calc R U . . .
H40B H 0.7226 -0.1081 0.3405 0.174 Uiso 1 1 calc R U . . .
C37 C 0.4819(16) -0.0427(15) 0.3404(8) 0.148(7) Uani 1 1 d . . . . .
H37A H 0.4383 0.0126 0.3436 0.178 Uiso 1 1 calc R U . . .
H37B H 0.4225 -0.0963 0.3079 0.178 Uiso 1 1 calc R U . . .
C39 C 0.6454(18) -0.0483(13) 0.4249(10) 0.149(6) Uani 1 1 d . U . . .
H39A H 0.6697 -0.1012 0.4409 0.179 Uiso 1 1 calc R U . . .
H39B H 0.6798 0.0096 0.4625 0.179 Uiso 1 1 calc R U . . .
C43 C 0.8272(18) 0.5452(13) 0.1204(9) 0.149(7) Uani 1 1 d . . . . .
H43A H 0.7580 0.5219 0.0788 0.179 Uiso 1 1 calc R U . . .
H43B H 0.8452 0.6133 0.1320 0.179 Uiso 1 1 calc R U . . .
C38 C 0.5054(18) -0.0564(15) 0.4047(9) 0.172(9) Uani 1 1 d . . . . .
H38A H 0.4640 -0.1184 0.4026 0.207 Uiso 1 1 calc R U . . .
H38B H 0.4711 -0.0093 0.4385 0.207 Uiso 1 1 calc R U . . .
C50 C 0.853(3) -0.0385(18) 0.1983(11) 0.238(10) Uani 1 1 d . U . . .
H50A H 0.8501 -0.0354 0.2470 0.286 Uiso 1 1 calc R U . . .
H50B H 0.9389 -0.0080 0.1972 0.286 Uiso 1 1 calc R U . . .
O5 O 0.5265(16) 0.6554(14) 0.1412(13) 0.234(8) Uani 1 1 d . . . . .
C57 C 0.327(2) 0.5623(14) 0.0921(12) 0.162(7) Uani 1 1 d . . . . .
H57A H 0.2963 0.5537 0.0422 0.195 Uiso 1 1 calc R U . . .
H57B H 0.2803 0.5134 0.1061 0.195 Uiso 1 1 calc R U . . .
C55 C 0.468(2) 0.5641(14) 0.1086(16) 0.212(12) Uani 1 1 d . . . . .
H55A H 0.4887 0.5255 0.1395 0.255 Uiso 1 1 calc R U . . .
H55B H 0.5005 0.5387 0.0655 0.255 Uiso 1 1 calc R U . . .
C56 C 0.437(3) 0.6909(19) 0.1719(16) 0.230(15) Uani 1 1 d . . . . .
H56A H 0.4468 0.7583 0.1784 0.276 Uiso 1 1 calc R U . . .
H56B H 0.4448 0.6811 0.2181 0.276 Uiso 1 1 calc R U . . .
C58 C 0.316(3) 0.650(3) 0.133(2) 0.269(19) Uani 1 1 d . . . . .
H58A H 0.2844 0.6880 0.1026 0.323 Uiso 1 1 calc R U . . .
H58B H 0.2539 0.6462 0.1633 0.323 Uiso 1 1 calc R U . . .
C59 C 0.772(3) -0.0171(18) 0.1143(12) 0.218(9) Uani 1 1 d . U . . .
H59A H 0.8570 0.0075 0.1083 0.261 Uiso 1 1 calc R U . . .
H59B H 0.7040 0.0052 0.0864 0.261 Uiso 1 1 calc R U . . .
C60 C 0.753(3) -0.1194(16) 0.0948(11) 0.229(10) Uani 1 1 d . U . . .
H60A H 0.7851 -0.1466 0.0518 0.275 Uiso 1 1 calc R U . . .
H60B H 0.6622 -0.1453 0.0892 0.275 Uiso 1 1 calc R U . . .
C61 C 0.834(3) -0.1342(17) 0.1562(11) 0.233(10) Uani 1 1 d . U . . .
H61A H 0.7875 -0.1760 0.1765 0.279 Uiso 1 1 calc R U . . .
H61B H 0.9157 -0.1563 0.1461 0.279 Uiso 1 1 calc R U . . .
C63 C 0.104(3) 0.7765(15) 0.2733(11) 0.162(7) Uani 1 1 d . . . . .
H63A H 0.1436 0.8389 0.2751 0.194 Uiso 1 1 calc R U . . .
H63B H 0.0662 0.7417 0.2246 0.194 Uiso 1 1 calc R U . . .
C62 C 0.140(4) 0.693(3) 0.351(2) 0.33(3) Uani 1 1 d D . . . .
H62A H 0.0708 0.6404 0.3281 0.392 Uiso 1 1 calc R U . . .
H62B H 0.2035 0.6789 0.3856 0.392 Uiso 1 1 calc R U . . .
C67 C 0.011(2) 0.7820(17) 0.3154(17) 0.195(10) Uani 1 1 d . . . . .
H67A H -0.0592 0.7289 0.2975 0.234 Uiso 1 1 calc R U . . .
H67B H -0.0260 0.8407 0.3225 0.234 Uiso 1 1 calc R U . . .
O7 O 0.094(4) 0.7783(17) 0.3755(9) 0.339(18) Uani 1 1 d . . . . .
C65 C 0.197(3) 0.729(3) 0.3025(17) 0.278(17) Uani 1 1 d D . . . .
H65A H 0.2767 0.7716 0.3266 0.333 Uiso 1 1 calc R U . . .
H65B H 0.2175 0.6779 0.2658 0.333 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N3 1.941(6) . ?
Ge1 N7 1.997(5) . ?
Ge1 N1 2.016(6) . ?
Ge1 K2 3.454(2) 1_455 ?
Ge2 N8 1.975(6) . ?
Ge2 N4 1.983(6) . ?
Ge2 N10 2.062(6) . ?
K2 O3 2.651(8) . ?
K2 O6 2.685(6) . ?
K2 N9 2.791(6) . ?
K2 C22 2.834(6) 1_655 ?
K2 C21 3.331(9) 1_655 ?
K2 C32 3.361(8) . ?
K2 Ge1 3.454(2) 1_655 ?
K2 C31 3.493(7) . ?
K2 C46 3.521(11) . ?
K2 K1 5.025(3) . ?
K1 O2 2.650(12) . ?
K1 O1 2.689(8) . ?
K1 N9 2.826(6) . ?
K1 C31 3.081(7) . ?
K1 C8 3.143(8) . ?
K1 C7 3.147(7) . ?
K1 C9 3.179(8) . ?
K1 C30 3.205(7) . ?
K1 C10 3.280(8) . ?
K1 C12 3.289(7) . ?
K1 C29 3.327(8) . ?
K1 C11 3.343(8) . ?
N8 C31 1.382(9) . ?
N8 C24 1.407(9) . ?
N7 C23 1.392(8) . ?
N7 C24 1.420(8) . ?
N3 C6 1.384(9) . ?
N3 C13 1.401(9) . ?
N1 C1 1.382(9) . ?
N1 C5 1.403(10) . ?
N4 C13 1.402(9) . ?
N4 C14 1.413(9) . ?
N9 C32 1.355(9) . ?
N9 C31 1.395(9) . ?
C22 C21 1.360(10) . ?
C22 C23 1.360(9) . ?
C22 K2 2.834(6) 1_455 ?
N5 C14 1.353(9) . ?
N5 C18 1.356(10) . ?
C31 C30 1.414(10) . ?
N10 C32 1.378(10) . ?
N10 C36 1.389(10) . ?
N2 C5 1.315(10) . ?
N2 C6 1.373(9) . ?
O6 C46 1.384(13) . ?
O6 C49 1.424(13) . ?
C6 C7 1.435(10) . ?
C23 N6 1.421(10) . ?
C13 C12 1.395(9) . ?
N6 C19 1.406(10) . ?
C7 C8 1.426(10) . ?
C7 C12 1.453(10) . ?
C11 C10 1.376(11) . ?
C11 C12 1.452(10) . ?
C26 C27 1.373(11) . ?
C26 C25 1.433(10) . ?
C14 C15 1.397(10) . ?
C24 C25 1.380(10) . ?
C19 C20 1.387(11) . ?
C30 C29 1.416(10) . ?
C30 C25 1.447(10) . ?
O3 C44 1.423(14) . ?
O3 C41 1.442(14) . ?
C34 C33 1.353(12) . ?
C34 C35 1.404(13) . ?
C29 C28 1.376(11) . ?
C15 C16 1.392(11) . ?
C21 C20 1.352(11) . ?
C21 K2 3.331(8) 1_455 ?
C27 C28 1.417(12) . ?
C5 C4 1.460(11) . ?
C1 C2 1.375(12) . ?
C8 C9 1.382(11) . ?
O1 C37 1.385(16) . ?
O1 C40 1.438(16) . ?
C32 C33 1.444(10) . ?
C10 C9 1.414(12) . ?
C3 C4 1.378(12) . ?
C3 C2 1.415(13) . ?
C35 C36 1.381(11) . ?
C16 C17 1.376(13) . ?
C18 C17 1.364(13) . ?
C44 C43 1.485(17) . ?
O2 C59 1.21(2) . ?
O2 C50 1.32(2) . ?
C47 C46 1.433(15) . ?
C47 C48 1.500(16) . ?
C48 C49 1.503(16) . ?
C41 C42 1.479(19) . ?
C42 C43 1.411(19) . ?
C40 C39 1.49(2) . ?
C37 C38 1.377(18) . ?
C39 C38 1.47(2) . ?
C50 C61 1.45(3) . ?
O5 C56 1.30(2) . ?
O5 C55 1.40(2) . ?
C57 C58 1.40(3) . ?
C57 C55 1.48(2) . ?
C56 C58 1.39(4) . ?
C59 C60 1.48(3) . ?
C60 C61 1.49(2) . ?
C63 C67 1.41(2) . ?
C63 C65 1.43(3) . ?
C62 O7 1.42(4) . ?
C62 C65 1.429(18) . ?
C67 O7 1.42(3) . ?

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
N3 Ge1 N7 93.7(2) . . ?
N3 Ge1 N1 87.7(2) . . ?
N7 Ge1 N1 95.7(2) . . ?
N3 Ge1 K2 156.72(17) . 1_455 ?
N7 Ge1 K2 98.71(16) . 1_455 ?
N1 Ge1 K2 110.39(18) . 1_455 ?
N8 Ge2 N4 92.2(2) . . ?
N8 Ge2 N10 86.4(2) . . ?
N4 Ge2 N10 94.5(2) . . ?
O3 K2 O6 83.4(2) . . ?
O3 K2 N9 107.8(2) . . ?
O6 K2 N9 98.76(19) . . ?
O3 K2 C22 98.1(2) . 1_655 ?
O6 K2 C22 97.8(2) . 1_655 ?
N9 K2 C22 150.7(2) . 1_655 ?
O3 K2 C21 96.9(2) . 1_655 ?
O6 K2 C21 74.0(2) . 1_655 ?
N9 K2 C21 153.5(2) . 1_655 ?
C22 K2 C21 23.77(18) 1_655 1_655 ?
O3 K2 C32 84.8(2) . . ?
O6 K2 C32 99.2(2) . . ?
N9 K2 C32 23.15(17) . . ?
C22 K2 C32 163.06(18) 1_655 . ?
C21 K2 C32 172.71(18) 1_655 . ?
O3 K2 Ge1 102.02(17) . 1_655 ?
O6 K2 Ge1 153.97(17) . 1_655 ?
N9 K2 Ge1 103.57(13) . 1_655 ?
C22 K2 Ge1 56.43(12) 1_655 1_655 ?
C21 K2 Ge1 80.02(14) 1_655 1_655 ?
C32 K2 Ge1 106.64(13) . 1_655 ?
O3 K2 C31 119.1(2) . . ?
O6 K2 C31 81.26(18) . . ?
N9 K2 C31 22.25(16) . . ?
C22 K2 C31 142.27(19) 1_655 . ?
C21 K2 C31 133.38(19) 1_655 . ?
C32 K2 C31 41.17(17) . . ?
Ge1 K2 C31 116.36(13) 1_655 . ?
O3 K2 C46 88.8(3) . . ?
O6 K2 C46 20.7(2) . . ?
N9 K2 C46 78.1(2) . . ?
C22 K2 C46 116.9(3) 1_655 . ?
C21 K2 C46 93.1(3) 1_655 . ?
C32 K2 C46 79.8(3) . . ?
Ge1 K2 C46 167.8(3) 1_655 . ?
C31 K2 C46 61.6(2) . . ?
O3 K2 K1 125.3(2) . . ?
O6 K2 K1 118.05(15) . . ?
N9 K2 K1 26.74(13) . . ?
C22 K2 K1 124.45(14) 1_655 . ?
C21 K2 K1 136.11(17) 1_655 . ?
C32 K2 K1 44.68(14) . . ?
Ge1 K2 K1 79.79(5) 1_655 . ?
C31 K2 K1 37.22(11) . . ?
C46 K2 K1 98.8(2) . . ?
O2 K1 O1 89.1(4) . . ?
O2 K1 N9 102.5(4) . . ?
O1 K1 N9 135.9(2) . . ?
O2 K1 C31 127.5(4) . . ?
O1 K1 C31 118.5(2) . . ?
N9 K1 C31 26.87(17) . . ?
O2 K1 C8 113.1(4) . . ?
O1 K1 C8 80.1(3) . . ?
N9 K1 C8 130.0(2) . . ?
C31 K1 C8 115.1(2) . . ?
O2 K1 C7 135.9(3) . . ?
O1 K1 C7 94.0(3) . . ?
N9 K1 C7 105.31(19) . . ?
C31 K1 C7 88.91(19) . . ?
C8 K1 C7 26.20(19) . . ?
O2 K1 C9 91.1(4) . . ?
O1 K1 C9 91.7(3) . . ?
N9 K1 C9 129.7(2) . . ?
C31 K1 C9 127.9(2) . . ?
C8 K1 C9 25.3(2) . . ?
C7 K1 C9 44.79(19) . . ?
O2 K1 C30 131.0(3) . . ?
O1 K1 C30 92.7(2) . . ?
N9 K1 C30 48.06(18) . . ?
C31 K1 C30 25.91(18) . . ?
C8 K1 C30 115.4(2) . . ?
C7 K1 C30 92.86(18) . . ?
C9 K1 C30 137.6(2) . . ?
O2 K1 C10 87.8(3) . . ?
O1 K1 C10 116.6(3) . . ?
N9 K1 C10 106.3(2) . . ?
C31 K1 C10 112.7(2) . . ?
C8 K1 C10 44.7(2) . . ?
C7 K1 C10 51.8(2) . . ?
C9 K1 C10 25.2(2) . . ?
C30 K1 C10 133.0(2) . . ?
O2 K1 C12 129.6(3) . . ?
O1 K1 C12 120.0(3) . . ?
N9 K1 C12 84.71(18) . . ?
C31 K1 C12 76.45(18) . . ?
C8 K1 C12 45.6(2) . . ?
C7 K1 C12 25.97(18) . . ?
C9 K1 C12 51.49(19) . . ?
C30 K1 C12 90.77(18) . . ?
C10 K1 C12 43.33(18) . . ?
O2 K1 C29 112.5(3) . . ?
O1 K1 C29 74.5(2) . . ?
N9 K1 C29 61.69(19) . . ?
C31 K1 C29 47.81(19) . . ?
C8 K1 C29 126.7(2) . . ?
C7 K1 C29 110.7(2) . . ?
C9 K1 C29 151.9(2) . . ?
C30 K1 C29 24.95(18) . . ?
C10 K1 C29 157.7(2) . . ?
C12 K1 C29 114.55(18) . . ?
O2 K1 C11 104.6(3) . . ?
O1 K1 C11 132.5(3) . . ?
N9 K1 C11 85.84(19) . . ?
C31 K1 C11 88.81(19) . . ?
C8 K1 C11 52.6(2) . . ?
C7 K1 C11 45.29(19) . . ?
C9 K1 C11 43.9(2) . . ?
C30 K1 C11 109.59(18) . . ?
C10 K1 C11 23.96(19) . . ?
C12 K1 C11 25.27(17) . . ?
C29 K1 C11 134.54(19) . . ?
C31 N8 C24 107.8(6) . . ?
C31 N8 Ge2 128.9(5) . . ?
C24 N8 Ge2 122.9(4) . . ?
C23 N7 C24 118.2(5) . . ?
C23 N7 Ge1 119.2(4) . . ?
C24 N7 Ge1 120.8(4) . . ?
C6 N3 C13 110.6(6) . . ?
C6 N3 Ge1 127.4(5) . . ?
C13 N3 Ge1 121.7(5) . . ?
C1 N1 C5 120.3(7) . . ?
C1 N1 Ge1 111.8(5) . . ?
C5 N1 Ge1 127.9(5) . . ?
C13 N4 C14 118.0(6) . . ?
C13 N4 Ge2 122.4(4) . . ?
C14 N4 Ge2 118.7(5) . . ?
C32 N9 C31 122.7(6) . . ?
C32 N9 K2 102.8(4) . . ?
C31 N9 K2 108.5(4) . . ?
C32 N9 K1 110.7(4) . . ?
C31 N9 K1 86.8(4) . . ?
K2 N9 K1 126.9(2) . . ?
C21 C22 C23 117.3(6) . . ?
C21 C22 K2 99.1(5) . 1_455 ?
C23 C22 K2 140.2(4) . 1_455 ?
C14 N5 C18 116.1(7) . . ?
N8 C31 N9 126.5(6) . . ?
N8 C31 C30 109.3(6) . . ?
N9 C31 C30 124.0(6) . . ?
N8 C31 K1 121.5(4) . . ?
N9 C31 K1 66.3(4) . . ?
C30 C31 K1 81.9(4) . . ?
N8 C31 K2 133.4(4) . . ?
N9 C31 K2 49.3(3) . . ?
C30 C31 K2 96.7(4) . . ?
K1 C31 K2 99.49(19) . . ?
C32 N10 C36 119.8(6) . . ?
C32 N10 Ge2 128.9(5) . . ?
C36 N10 Ge2 111.3(5) . . ?
C5 N2 C6 122.0(7) . . ?
C46 O6 C49 107.3(8) . . ?
C46 O6 K2 116.1(6) . . ?
C49 O6 K2 136.3(6) . . ?
N2 C6 N3 128.1(7) . . ?
N2 C6 C7 124.8(7) . . ?
N3 C6 C7 107.0(6) . . ?
C22 C23 N7 116.3(6) . . ?
C22 C23 N6 121.6(6) . . ?
N7 C23 N6 122.1(6) . . ?
C12 C13 N3 108.0(6) . . ?
C12 C13 N4 131.7(6) . . ?
N3 C13 N4 120.2(6) . . ?
C19 N6 C23 117.8(7) . . ?
C8 C7 C6 133.0(7) . . ?
C8 C7 C12 120.2(7) . . ?
C6 C7 C12 106.8(6) . . ?
C8 C7 K1 76.8(4) . . ?
C6 C7 K1 111.8(4) . . ?
C12 C7 K1 82.5(4) . . ?
C10 C11 C12 118.1(8) . . ?
C10 C11 K1 75.4(5) . . ?
C12 C11 K1 75.3(4) . . ?
C27 C26 C25 118.8(8) . . ?
N5 C14 C15 122.8(7) . . ?
N5 C14 N4 114.8(6) . . ?
C15 C14 N4 122.3(7) . . ?
C13 C12 C11 133.2(7) . . ?
C13 C12 C7 107.6(6) . . ?
C11 C12 C7 119.2(6) . . ?
C13 C12 K1 116.3(4) . . ?
C11 C12 K1 79.5(4) . . ?
C7 C12 K1 71.6(4) . . ?
C25 C24 N8 109.4(6) . . ?
C25 C24 N7 132.0(6) . . ?
N8 C24 N7 118.4(6) . . ?
C20 C19 N6 120.0(7) . . ?
C31 C30 C29 134.1(7) . . ?
C31 C30 C25 106.2(6) . . ?
C29 C30 C25 119.7(7) . . ?
C31 C30 K1 72.2(4) . . ?
C29 C30 K1 82.3(4) . . ?
C25 C30 K1 123.3(4) . . ?
C44 O3 C41 105.1(9) . . ?
C44 O3 K2 121.1(7) . . ?
C41 O3 K2 124.8(8) . . ?
C33 C34 C35 119.9(8) . . ?
C24 C25 C26 133.4(7) . . ?
C24 C25 C30 107.4(6) . . ?
C26 C25 C30 119.3(7) . . ?
C28 C29 C30 119.2(7) . . ?
C28 C29 K1 127.1(5) . . ?
C30 C29 K1 72.7(4) . . ?
C16 C15 C14 117.9(8) . . ?
C20 C21 C22 125.1(7) . . ?
C20 C21 K2 166.8(7) . 1_455 ?
C22 C21 K2 57.2(4) . 1_455 ?
C26 C27 C28 121.6(8) . . ?
N2 C5 N1 125.8(7) . . ?
N2 C5 C4 118.0(8) . . ?
N1 C5 C4 116.2(8) . . ?
C29 C28 C27 121.3(8) . . ?
C2 C1 N1 123.5(8) . . ?
C9 C8 C7 118.3(8) . . ?
C9 C8 K1 78.8(5) . . ?
C7 C8 K1 77.0(4) . . ?
C37 O1 C40 105.8(12) . . ?
C37 O1 K1 112.2(8) . . ?
C40 O1 K1 136.9(10) . . ?
C21 C20 C19 118.2(7) . . ?
N9 C32 N10 125.1(6) . . ?
N9 C32 C33 117.4(7) . . ?
N10 C32 C33 117.5(7) . . ?
N9 C32 K2 54.1(4) . . ?
N10 C32 K2 129.3(5) . . ?
C33 C32 K2 86.3(5) . . ?
N9 C32 K1 48.3(4) . . ?
N10 C32 K1 123.0(5) . . ?
C33 C32 K1 98.1(5) . . ?
K2 C32 K1 93.4(2) . . ?
C11 C10 C9 122.1(8) . . ?
C11 C10 K1 80.6(5) . . ?
C9 C10 K1 73.4(5) . . ?
C8 C9 C10 122.1(8) . . ?
C8 C9 K1 75.9(5) . . ?
C10 C9 K1 81.4(5) . . ?
C4 C3 C2 119.4(8) . . ?
C34 C33 C32 121.8(8) . . ?
C36 C35 C34 118.4(8) . . ?
C1 C2 C3 118.4(8) . . ?
C17 C16 C15 120.5(9) . . ?
N5 C18 C17 125.5(9) . . ?
C3 C4 C5 122.2(9) . . ?
C35 C36 N10 122.4(8) . . ?
C18 C17 C16 117.2(8) . . ?
O3 C44 C43 110.1(11) . . ?
C59 O2 C50 99.4(16) . . ?
C59 O2 K1 125.5(15) . . ?
C50 O2 K1 132.2(15) . . ?
C46 C47 C48 105.6(10) . . ?
C47 C48 C49 101.8(10) . . ?
O6 C46 C47 110.8(10) . . ?
O6 C46 K2 43.2(5) . . ?
C47 C46 K2 150.3(9) . . ?
O6 C49 C48 106.0(10) . . ?
O3 C41 C42 108.5(11) . . ?
C43 C42 C41 108.0(12) . . ?
O1 C40 C39 107.2(14) . . ?
C38 C37 O1 113.8(14) . . ?
C38 C37 K1 150.1(13) . . ?
O1 C37 K1 46.0(6) . . ?
C38 C39 C40 104.8(15) . . ?
C42 C43 C44 105.8(13) . . ?
C37 C38 C39 106.3(16) . . ?
O2 C50 C61 110(2) . . ?
C56 O5 C55 102(2) . . ?
C58 C57 C55 100(2) . . ?
O5 C55 C57 109.1(16) . . ?
O5 C56 C58 110(3) . . ?
C56 C58 C57 108(2) . . ?
O2 C59 C60 103(2) . . ?
O2 C59 K1 38.2(11) . . ?
C60 C59 K1 110.2(18) . . ?
C59 C60 C61 101(2) . . ?
C50 C61 C60 95.6(18) . . ?
C67 C63 C65 104(2) . . ?
O7 C62 C65 90(2) . . ?
C63 C67 O7 96(2) . . ?
C62 O7 C67 101(2) . . ?
C63 C65 C62 107(2) . . ?

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
C24 N8 C31 N9 175.8(6) . . . . ?
Ge2 N8 C31 N9 -12.2(10) . . . . ?
C24 N8 C31 C30 1.1(7) . . . . ?
Ge2 N8 C31 C30 173.1(4) . . . . ?
C24 N8 C31 K1 93.4(6) . . . . ?
Ge2 N8 C31 K1 -94.6(6) . . . . ?
C24 N8 C31 K2 -118.8(6) . . . . ?
Ge2 N8 C31 K2 53.1(8) . . . . ?
C32 N9 C31 N8 -0.1(11) . . . . ?
K2 N9 C31 N8 119.4(6) . . . . ?
K1 N9 C31 N8 -112.7(6) . . . . ?
C32 N9 C31 C30 173.9(7) . . . . ?
K2 N9 C31 C30 -66.7(7) . . . . ?
K1 N9 C31 C30 61.3(6) . . . . ?
C32 N9 C31 K1 112.6(7) . . . . ?
K2 N9 C31 K1 -128.0(3) . . . . ?
C32 N9 C31 K2 -119.4(7) . . . . ?
K1 N9 C31 K2 128.0(3) . . . . ?
C5 N2 C6 N3 1.6(12) . . . . ?
C5 N2 C6 C7 177.4(7) . . . . ?
C13 N3 C6 N2 174.6(7) . . . . ?
Ge1 N3 C6 N2 -11.7(10) . . . . ?
C13 N3 C6 C7 -1.9(7) . . . . ?
Ge1 N3 C6 C7 171.8(4) . . . . ?
C21 C22 C23 N7 -179.2(7) . . . . ?
K2 C22 C23 N7 -25.4(11) 1_455 . . . ?
C21 C22 C23 N6 0.4(11) . . . . ?
K2 C22 C23 N6 154.3(6) 1_455 . . . ?
C24 N7 C23 C22 -174.3(6) . . . . ?
Ge1 N7 C23 C22 -9.4(8) . . . . ?
C24 N7 C23 N6 6.1(10) . . . . ?
Ge1 N7 C23 N6 171.0(5) . . . . ?
C6 N3 C13 C12 0.6(7) . . . . ?
Ge1 N3 C13 C12 -173.6(4) . . . . ?
C6 N3 C13 N4 -176.1(6) . . . . ?
Ge1 N3 C13 N4 9.8(8) . . . . ?
C14 N4 C13 C12 72.6(9) . . . . ?
Ge2 N4 C13 C12 -96.2(8) . . . . ?
C14 N4 C13 N3 -111.6(7) . . . . ?
Ge2 N4 C13 N3 79.6(7) . . . . ?
C22 C23 N6 C19 0.7(11) . . . . ?
N7 C23 N6 C19 -179.7(7) . . . . ?
N2 C6 C7 C8 6.3(13) . . . . ?
N3 C6 C7 C8 -177.1(7) . . . . ?
N2 C6 C7 C12 -174.2(7) . . . . ?
N3 C6 C7 C12 2.4(7) . . . . ?
N2 C6 C7 K1 -85.7(7) . . . . ?
N3 C6 C7 K1 90.9(5) . . . . ?
C18 N5 C14 C15 0.7(10) . . . . ?
C18 N5 C14 N4 -179.6(6) . . . . ?
C13 N4 C14 N5 -164.4(6) . . . . ?
Ge2 N4 C14 N5 4.8(8) . . . . ?
C13 N4 C14 C15 15.3(10) . . . . ?
Ge2 N4 C14 C15 -175.4(5) . . . . ?
N3 C13 C12 C11 -177.3(7) . . . . ?
N4 C13 C12 C11 -1.2(13) . . . . ?
N3 C13 C12 C7 1.0(7) . . . . ?
N4 C13 C12 C7 177.1(6) . . . . ?
N3 C13 C12 K1 -76.7(6) . . . . ?
N4 C13 C12 K1 99.5(7) . . . . ?
C10 C11 C12 C13 -179.4(8) . . . . ?
K1 C11 C12 C13 116.3(8) . . . . ?
C10 C11 C12 C7 2.5(10) . . . . ?
K1 C11 C12 C7 -61.8(6) . . . . ?
C10 C11 C12 K1 64.2(7) . . . . ?
C8 C7 C12 C13 177.5(6) . . . . ?
C6 C7 C12 C13 -2.1(8) . . . . ?
K1 C7 C12 C13 -112.6(5) . . . . ?
C8 C7 C12 C11 -3.9(10) . . . . ?
C6 C7 C12 C11 176.5(6) . . . . ?
K1 C7 C12 C11 66.0(6) . . . . ?
C8 C7 C12 K1 -69.9(6) . . . . ?
C6 C7 C12 K1 110.5(5) . . . . ?
C31 N8 C24 C25 -2.1(7) . . . . ?
Ge2 N8 C24 C25 -174.6(5) . . . . ?
C31 N8 C24 N7 -177.5(6) . . . . ?
Ge2 N8 C24 N7 10.0(8) . . . . ?
C23 N7 C24 C25 70.1(10) . . . . ?
Ge1 N7 C24 C25 -94.5(8) . . . . ?
C23 N7 C24 N8 -115.7(7) . . . . ?
Ge1 N7 C24 N8 79.7(7) . . . . ?
C23 N6 C19 C20 -1.4(12) . . . . ?
N8 C31 C30 C29 -179.8(7) . . . . ?
N9 C31 C30 C29 5.4(13) . . . . ?
K1 C31 C30 C29 59.6(8) . . . . ?
K2 C31 C30 C29 -39.1(9) . . . . ?
N8 C31 C30 C25 0.2(8) . . . . ?
N9 C31 C30 C25 -174.7(6) . . . . ?
K1 C31 C30 C25 -120.5(5) . . . . ?
K2 C31 C30 C25 140.8(5) . . . . ?
N8 C31 C30 K1 120.7(5) . . . . ?
N9 C31 C30 K1 -54.2(6) . . . . ?
K2 C31 C30 K1 -98.69(19) . . . . ?
N8 C24 C25 C26 -177.1(8) . . . . ?
N7 C24 C25 C26 -2.6(14) . . . . ?
N8 C24 C25 C30 2.2(8) . . . . ?
N7 C24 C25 C30 176.7(7) . . . . ?
C27 C26 C25 C24 -179.0(8) . . . . ?
C27 C26 C25 C30 1.7(11) . . . . ?
C31 C30 C25 C24 -1.5(8) . . . . ?
C29 C30 C25 C24 178.5(6) . . . . ?
K1 C30 C25 C24 -80.5(7) . . . . ?
C31 C30 C25 C26 178.0(6) . . . . ?
C29 C30 C25 C26 -2.0(10) . . . . ?
K1 C30 C25 C26 99.0(7) . . . . ?
C31 C30 C29 C28 -179.3(8) . . . . ?
C25 C30 C29 C28 0.7(11) . . . . ?
K1 C30 C29 C28 -123.4(7) . . . . ?
C31 C30 C29 K1 -55.9(8) . . . . ?
C25 C30 C29 K1 124.1(6) . . . . ?
N5 C14 C15 C16 -0.5(11) . . . . ?
N4 C14 C15 C16 179.8(7) . . . . ?
C23 C22 C21 C20 -0.9(13) . . . . ?
K2 C22 C21 C20 -164.3(8) 1_455 . . . ?
C23 C22 C21 K2 163.4(8) . . . 1_455 ?
C25 C26 C27 C28 -0.1(12) . . . . ?
C6 N2 C5 N1 5.6(12) . . . . ?
C6 N2 C5 C4 -174.6(7) . . . . ?
C1 N1 C5 N2 179.0(7) . . . . ?
Ge1 N1 C5 N2 -2.5(11) . . . . ?
C1 N1 C5 C4 -0.7(10) . . . . ?
Ge1 N1 C5 C4 177.8(6) . . . . ?
C30 C29 C28 C27 0.9(12) . . . . ?
K1 C29 C28 C27 -88.9(9) . . . . ?
C26 C27 C28 C29 -1.2(13) . . . . ?
C5 N1 C1 C2 1.5(12) . . . . ?
Ge1 N1 C1 C2 -177.2(7) . . . . ?
C6 C7 C8 C9 -177.1(8) . . . . ?
C12 C7 C8 C9 3.4(10) . . . . ?
K1 C7 C8 C9 -69.6(7) . . . . ?
C6 C7 C8 K1 -107.5(8) . . . . ?
C12 C7 C8 K1 73.0(6) . . . . ?
C22 C21 C20 C19 0.2(14) . . . . ?
K2 C21 C20 C19 -95(3) 1_455 . . . ?
N6 C19 C20 C21 1.0(13) . . . . ?
C31 N9 C32 N10 5.6(11) . . . . ?
K2 N9 C32 N10 -116.6(7) . . . . ?
K1 N9 C32 N10 105.5(7) . . . . ?
C31 N9 C32 C33 -175.5(7) . . . . ?
K2 N9 C32 C33 62.3(7) . . . . ?
K1 N9 C32 C33 -75.7(7) . . . . ?
C31 N9 C32 K2 122.1(7) . . . . ?
K1 N9 C32 K2 -138.0(4) . . . . ?
C31 N9 C32 K1 -99.9(7) . . . . ?
K2 N9 C32 K1 138.0(4) . . . . ?
C36 N10 C32 N9 -179.0(7) . . . . ?
Ge2 N10 C32 N9 1.0(11) . . . . ?
C36 N10 C32 C33 2.1(10) . . . . ?
Ge2 N10 C32 C33 -177.9(5) . . . . ?
C36 N10 C32 K2 111.5(7) . . . . ?
Ge2 N10 C32 K2 -68.4(8) . . . . ?
C36 N10 C32 K1 -119.8(6) . . . . ?
Ge2 N10 C32 K1 60.2(7) . . . . ?
C12 C11 C10 C9 -0.6(12) . . . . ?
K1 C11 C10 C9 63.5(7) . . . . ?
C12 C11 C10 K1 -64.1(6) . . . . ?
C7 C8 C9 C10 -1.6(12) . . . . ?
K1 C8 C9 C10 -70.1(7) . . . . ?
C7 C8 C9 K1 68.6(6) . . . . ?
C11 C10 C9 C8 0.2(13) . . . . ?
K1 C10 C9 C8 67.3(7) . . . . ?
C11 C10 C9 K1 -67.2(7) . . . . ?
C35 C34 C33 C32 -0.9(13) . . . . ?
N9 C32 C33 C34 179.4(7) . . . . ?
N10 C32 C33 C34 -1.6(12) . . . . ?
K2 C32 C33 C34 -134.6(8) . . . . ?
K1 C32 C33 C34 132.4(8) . . . . ?
C33 C34 C35 C36 2.9(14) . . . . ?
N1 C1 C2 C3 -0.8(13) . . . . ?
C4 C3 C2 C1 -0.7(14) . . . . ?
C14 C15 C16 C17 -0.2(13) . . . . ?
C14 N5 C18 C17 -0.2(12) . . . . ?
C2 C3 C4 C5 1.5(14) . . . . ?
N2 C5 C4 C3 179.5(8) . . . . ?
N1 C5 C4 C3 -0.7(12) . . . . ?
C34 C35 C36 N10 -2.4(14) . . . . ?
C32 N10 C36 C35 -0.1(12) . . . . ?
Ge2 N10 C36 C35 179.8(7) . . . . ?
N5 C18 C17 C16 -0.5(14) . . . . ?
C15 C16 C17 C18 0.7(13) . . . . ?
C41 O3 C44 C43 -15.6(16) . . . . ?
K2 O3 C44 C43 -164.0(10) . . . . ?
C46 C47 C48 C49 -21.8(16) . . . . ?
C49 O6 C46 C47 11.9(17) . . . . ?
K2 O6 C46 C47 -162.3(10) . . . . ?
C49 O6 C46 K2 174.2(12) . . . . ?
C48 C47 C46 O6 7.1(18) . . . . ?
C48 C47 C46 K2 -18(3) . . . . ?
C46 O6 C49 C48 -26.0(15) . . . . ?
K2 O6 C49 C48 146.4(8) . . . . ?
C47 C48 C49 O6 29.1(15) . . . . ?
C44 O3 C41 C42 14.8(17) . . . . ?
K2 O3 C41 C42 161.7(11) . . . . ?
O3 C41 C42 C43 -9(2) . . . . ?
C37 O1 C40 C39 -13.0(19) . . . . ?
K1 O1 C40 C39 138.3(12) . . . . ?
C40 O1 C37 C38 6(2) . . . . ?
K1 O1 C37 C38 -153.0(15) . . . . ?
C40 O1 C37 K1 159.2(13) . . . . ?
O1 C40 C39 C38 15(2) . . . . ?
C41 C42 C43 C44 -1(2) . . . . ?
O3 C44 C43 C42 10(2) . . . . ?
O1 C37 C38 C39 3(3) . . . . ?
K1 C37 C38 C39 -38(4) . . . . ?
C40 C39 C38 C37 -11(2) . . . . ?
C59 O2 C50 C61 -51(3) . . . . ?
K1 O2 C50 C61 110(2) . . . . ?
C56 O5 C55 C57 29(3) . . . . ?
C58 C57 C55 O5 -14(3) . . . . ?
C55 O5 C56 C58 -33(4) . . . . ?
O5 C56 C58 C57 26(5) . . . . ?
C55 C57 C58 C56 -5(4) . . . . ?
C50 O2 C59 C60 56(3) . . . . ?
K1 O2 C59 C60 -106.6(19) . . . . ?
C50 O2 C59 K1 163(3) . . . . ?
O2 C59 C60 C61 -43(3) . . . . ?
K1 C59 C60 C61 -82(2) . . . . ?
O2 C50 C61 C60 20(3) . . . . ?
C59 C60 C61 C50 11(3) . . . . ?
C65 C63 C67 O7 26(3) . . . . ?
C65 C62 O7 C67 62(3) . . . . ?
C63 C67 O7 C62 -58(3) . . . . ?
C67 C63 C65 C62 11(4) . . . . ?
O7 C62 C65 C63 -43(4) . . . . ?

_refine_diff_density_max         1.370
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.104

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jcm01024a_sq
_database_code_depnum_ccdc_archive 'CCDC 2403142'
loop_
_audit_author_name
_audit_author_address
'Jesus Campos'
;CSIC
Spain
;
_audit_update_record             
;
2024-11-15 deposited with the CCDC.	2025-01-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H55 Ge2 K2 N10 O3'
_chemical_formula_weight         1091.44

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'
K K 0.2009 0.2494 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.1680(5)
_cell_length_b                   16.0363(7)
_cell_length_c                   23.4696(9)
_cell_angle_alpha                90
_cell_angle_beta                 94.6980(10)
_cell_angle_gamma                90
_cell_volume                     5314.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    9867
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      26.97

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_F_000             2252
_exptl_transmission_factor_min   .
_exptl_transmission_factor_max   .
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    1.339
_shelx_estimated_absorpt_T_min   .
_shelx_estimated_absorpt_T_max   .
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6181
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   ' Apex3 v2016.9-0 (Bruker, 2016)'
_exptl_absorpt_special_details   .
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'IuS 3.0 Microfocus Source'
_diffrn_measurement_device_type  'Bruker D8Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean .
_diffrn_reflns_number            108974
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_av_R_equivalents  0.1251
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.922
_diffrn_reflns_theta_max         27.126
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11737
_reflns_number_gt                8243
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker APEX3'
_computing_data_reduction        'Bruker APEX3'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    .
_computing_publication_material  .
_refine_special_details          SQUEEZE

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.000 213 90 ' '
2 0.500 1.000 0.500 213 90 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The unit cell contains 4 pentane molecules which have
 been treated as a diffuse contribution to the overall scattering
 without specific atom positions by SQUEEZE/PLATON.'
;




_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0940P)²+3.6549P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11737
_refine_ls_number_parameters     626
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0478
_refine_ls_wR_factor_ref         0.1652
_refine_ls_wR_factor_gt          0.1344
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge2 Ge 0.45437(3) 0.79549(2) 0.83590(2) 0.03031(12) Uani 1 1 d . . . . .
Ge1 Ge 0.64334(3) 0.74121(2) 0.72093(2) 0.03051(12) Uani 1 1 d . . . . .
K003 K 0.40392(7) 0.46851(6) 0.80835(4) 0.0432(2) Uani 1 1 d . . . . .
K004 K 0.79697(8) 0.42360(6) 0.70460(4) 0.0485(2) Uani 1 1 d . . . . .
N8 N 0.4119(2) 0.7163(2) 0.77695(13) 0.0294(6) Uani 1 1 d . . . . .
N10 N 0.3776(2) 0.7296(2) 0.89104(13) 0.0330(7) Uani 1 1 d . . . . .
N5 N 0.6313(2) 0.8428(2) 0.90669(13) 0.0327(7) Uani 1 1 d . . . . .
N7 N 0.5120(2) 0.78042(19) 0.71136(13) 0.0289(6) Uani 1 1 d . . . . .
N3 N 0.6135(2) 0.64707(19) 0.76815(13) 0.0283(6) Uani 1 1 d . . . . .
N4 N 0.5772(2) 0.73525(19) 0.84780(13) 0.0304(7) Uani 1 1 d . . . . .
N9 N 0.3162(2) 0.6192(2) 0.82838(13) 0.0339(7) Uani 1 1 d . . . . .
N6 N 0.5628(2) 0.9150(2) 0.69491(15) 0.0358(7) Uani 1 1 d . . . . .
N1 N 0.6340(2) 0.6628(2) 0.65240(14) 0.0348(7) Uani 1 1 d . . . . .
O1 O 0.3313(3) 0.3704(2) 0.88611(15) 0.0582(9) Uani 1 1 d . . . . .
N2 N 0.6366(2) 0.5310(2) 0.70311(14) 0.0359(7) Uani 1 1 d . . . . .
O2 O 0.4072(3) 0.3524(3) 0.72481(16) 0.0667(10) Uani 1 1 d . . . . .
C28 C 0.3501(2) 0.6515(2) 0.77955(15) 0.0302(8) Uani 1 1 d . . . . .
C15 C 0.6513(3) 0.7704(2) 0.88052(15) 0.0293(8) Uani 1 1 d . . . . .
C27 C 0.3341(2) 0.6171(2) 0.72432(15) 0.0292(7) Uani 1 1 d . . . . .
C22 C 0.3924(2) 0.6636(2) 0.68779(15) 0.0287(7) Uani 1 1 d . . . . .
C29 C 0.4894(3) 0.8625(2) 0.69867(15) 0.0298(8) Uani 1 1 d . . . . .
C21 C 0.4385(2) 0.7239(2) 0.72162(15) 0.0272(7) Uani 1 1 d . . . . .
O3 O 0.8986(3) 0.5493(3) 0.6703(2) 0.0760(12) Uani 1 1 d . U . . .
C1 C 0.6244(2) 0.5643(2) 0.75591(16) 0.0290(7) Uani 1 1 d . . . . .
C2 C 0.6135(3) 0.5185(2) 0.80573(16) 0.0327(8) Uani 1 1 d . . . . .
C35 C 0.3309(3) 0.6544(3) 0.87896(16) 0.0333(8) Uani 1 1 d . . . . .
C23 C 0.3932(3) 0.6407(3) 0.62964(16) 0.0377(9) Uani 1 1 d . . . . .
H23 H 0.4319 0.6699 0.6050 0.045 Uiso 1 1 calc R U . . .
C39 C 0.3743(3) 0.7638(3) 0.94534(17) 0.0409(10) Uani 1 1 d . . . . .
C26 C 0.2753(3) 0.5523(3) 0.70149(17) 0.0368(9) Uani 1 1 d . . . . .
H26 H 0.2349 0.5231 0.7250 0.044 Uiso 1 1 calc R U . . .
C38 C 0.3338(3) 0.7229(3) 0.98803(18) 0.0504(12) Uani 1 1 d . . . . .
H38 H 0.3330 0.7480 1.0247 0.060 Uiso 1 1 calc R U . . .
C3 C 0.6194(3) 0.4324(3) 0.81954(19) 0.0412(9) Uani 1 1 d . . . . .
H3 H 0.6357 0.3924 0.7921 0.049 Uiso 1 1 calc R U . . .
C4 C 0.6008(4) 0.4081(3) 0.8742(2) 0.0515(12) Uani 1 1 d . . . . .
H4 H 0.6052 0.3506 0.8839 0.062 Uiso 1 1 calc R U . . .
C19 C 0.6992(3) 0.8794(3) 0.94188(16) 0.0364(9) Uani 1 1 d . . . . .
C30 C 0.3951(3) 0.8902(3) 0.68969(17) 0.0371(9) Uani 1 1 d . . . . .
H30 H 0.3438 0.8538 0.6954 0.044 Uiso 1 1 calc R U . . .
C36 C 0.2917(3) 0.6111(3) 0.92591(18) 0.0446(10) Uani 1 1 d . . . . .
H36 H 0.2640 0.5576 0.9192 0.054 Uiso 1 1 calc R U . . .
C9 C 0.6314(3) 0.5767(3) 0.65575(17) 0.0369(9) Uani 1 1 d . . . . .
C7 C 0.5904(3) 0.5779(2) 0.84904(16) 0.0320(8) Uani 1 1 d . . . . .
C37 C 0.2933(3) 0.6438(3) 0.97794(18) 0.0494(11) Uani 1 1 d . . . . .
H37 H 0.2673 0.6141 1.0080 0.059 Uiso 1 1 calc R U . . .
C25 C 0.2774(3) 0.5320(3) 0.64492(18) 0.0444(10) Uani 1 1 d . . . . .
H25 H 0.2384 0.4882 0.6293 0.053 Uiso 1 1 calc R U . . .
C31 C 0.3788(3) 0.9705(3) 0.6727(2) 0.0451(10) Uani 1 1 d . . . . .
H31 H 0.3157 0.9903 0.6659 0.054 Uiso 1 1 calc R U . . .
C16 C 0.7426(3) 0.7353(3) 0.88762(19) 0.0414(10) Uani 1 1 d . . . . .
H16 H 0.7567 0.6854 0.8683 0.050 Uiso 1 1 calc R U . . .
C24 C 0.3371(3) 0.5756(3) 0.60938(17) 0.0454(10) Uani 1 1 d . . . . .
H24 H 0.3382 0.5592 0.5705 0.054 Uiso 1 1 calc R U . . .
C5 C 0.5755(4) 0.4654(3) 0.9158(2) 0.0517(12) Uani 1 1 d . . . . .
H5 H 0.5618 0.4458 0.9524 0.062 Uiso 1 1 calc R U . . .
C8 C 0.5923(3) 0.6557(2) 0.82403(16) 0.0306(8) Uani 1 1 d . . . . .
C33 C 0.5445(3) 0.9937(3) 0.6773(2) 0.0432(10) Uani 1 1 d . . . . .
C32 C 0.4547(3) 1.0237(3) 0.6651(2) 0.0491(11) Uani 1 1 d . . . . .
H32 H 0.4444 1.0792 0.6519 0.059 Uiso 1 1 calc R U . . .
C10 C 0.6212(3) 0.5308(3) 0.60260(19) 0.0505(11) Uani 1 1 d . . . . .
H10 H 0.6179 0.4717 0.6036 0.061 Uiso 1 1 calc R U . . .
C13 C 0.6336(3) 0.7007(3) 0.59929(19) 0.0454(10) Uani 1 1 d . . . . .
C6 C 0.5705(3) 0.5492(3) 0.90412(18) 0.0429(10) Uani 1 1 d . . . . .
H6 H 0.5539 0.5875 0.9325 0.051 Uiso 1 1 calc R U . . .
C11 C 0.6162(4) 0.5697(4) 0.5518(2) 0.0570(13) Uani 1 1 d . . . . .
H11 H 0.6064 0.5386 0.5174 0.068 Uiso 1 1 calc R U . . .
C20 C 0.6680(3) 0.9581(3) 0.9699(2) 0.0501(11) Uani 1 1 d . . . . .
H20A H 0.7216 0.9820 0.9935 0.075 Uiso 1 1 calc R U . . .
H20B H 0.6167 0.9452 0.9941 0.075 Uiso 1 1 calc R U . . .
H20C H 0.6455 0.9983 0.9405 0.075 Uiso 1 1 calc R U . . .
C18 C 0.7886(3) 0.8469(3) 0.9514(2) 0.0488(11) Uani 1 1 d . . . . .
H18 H 0.8346 0.8733 0.9770 0.059 Uiso 1 1 calc R U . . .
C12 C 0.6256(4) 0.6563(3) 0.5500(2) 0.0547(13) Uani 1 1 d . . . . .
H12 H 0.6263 0.6841 0.5143 0.066 Uiso 1 1 calc R U . . .
C17 C 0.8105(3) 0.7743(3) 0.9228(2) 0.0528(12) Uani 1 1 d . . . . .
H17 H 0.8727 0.7519 0.9278 0.063 Uiso 1 1 calc R U . . .
C40 C 0.4158(4) 0.8491(3) 0.9556(2) 0.0555(13) Uani 1 1 d . . . . .
H40A H 0.4824 0.8487 0.9471 0.083 Uiso 1 1 calc R U . . .
H40B H 0.4114 0.8648 0.9956 0.083 Uiso 1 1 calc R U . . .
H40C H 0.3807 0.8894 0.9306 0.083 Uiso 1 1 calc R U . . .
C14 C 0.6442(5) 0.7926(3) 0.5976(2) 0.0746(18) Uani 1 1 d . . . . .
H14A H 0.6474 0.8107 0.5579 0.112 Uiso 1 1 calc R U . . .
H14B H 0.7024 0.8089 0.6203 0.112 Uiso 1 1 calc R U . . .
H14C H 0.5896 0.8189 0.6135 0.112 Uiso 1 1 calc R U . . .
C45 C 0.3363(5) 0.3008(4) 0.6966(3) 0.0771(18) Uani 1 1 d . . . . .
H45A H 0.2743 0.3295 0.6941 0.093 Uiso 1 1 calc R U . . .
H45B H 0.3306 0.2480 0.7178 0.093 Uiso 1 1 calc R U . . .
C34 C 0.6300(4) 1.0477(3) 0.6704(3) 0.0649(15) Uani 1 1 d . . . . .
H34A H 0.6108 1.0974 0.6481 0.097 Uiso 1 1 calc R U . . .
H34B H 0.6766 1.0161 0.6505 0.097 Uiso 1 1 calc R U . . .
H34C H 0.6583 1.0646 0.7082 0.097 Uiso 1 1 calc R U . . .
C46 C 0.3657(6) 0.2838(5) 0.6386(3) 0.103(3) Uani 1 1 d . . . . .
H46A H 0.3912 0.2265 0.6363 0.123 Uiso 1 1 calc R U . . .
H46B H 0.3112 0.2898 0.6096 0.123 Uiso 1 1 calc R U . . .
C47 C 0.4384(5) 0.3449(5) 0.6289(3) 0.095(2) Uani 1 1 d . . . . .
H47A H 0.4899 0.3193 0.6088 0.114 Uiso 1 1 calc R U . . .
H47B H 0.4114 0.3921 0.6057 0.114 Uiso 1 1 calc R U . . .
C52 C 0.9993(5) 0.5433(4) 0.6694(4) 0.094(2) Uani 1 1 d . U . . .
H52A H 1.0171 0.5376 0.6297 0.112 Uiso 1 1 calc R U . . .
H52B H 1.0237 0.4944 0.6918 0.112 Uiso 1 1 calc R U . . .
C44 C 0.3263(6) 0.2845(4) 0.8750(3) 0.092(2) Uani 1 1 d . . . . .
H44 H 0.3008 0.2591 0.8406 0.111 Uiso 1 1 calc R U . . .
C51 C 1.0387(5) 0.6226(5) 0.6957(4) 0.102(2) Uani 1 1 d . U . . .
H51A H 1.0633 0.6135 0.7359 0.122 Uiso 1 1 calc R U . . .
H51B H 1.0904 0.6446 0.6740 0.122 Uiso 1 1 calc R U . . .
C49 C 0.8754(5) 0.6348(4) 0.6660(4) 0.101(2) Uani 1 1 d . U . . .
H49A H 0.8185 0.6469 0.6864 0.122 Uiso 1 1 calc R U . . .
H49B H 0.8626 0.6512 0.6255 0.122 Uiso 1 1 calc R U . . .
C41 C 0.3332(7) 0.3797(4) 0.9465(3) 0.096(2) Uani 1 1 d . . . . .
H41A H 0.2682 0.3833 0.9589 0.115 Uiso 1 1 calc R U . . .
H41B H 0.3686 0.4305 0.9593 0.115 Uiso 1 1 calc R U . . .
C43 C 0.3680(7) 0.2406(4) 0.9265(3) 0.100(3) Uani 1 1 d . . . . .
H43A H 0.3243 0.1968 0.9382 0.120 Uiso 1 1 calc R U . . .
H43B H 0.4286 0.2139 0.9186 0.120 Uiso 1 1 calc R U . . .
C48 C 0.4733(5) 0.3729(6) 0.6852(3) 0.112(3) Uani 1 1 d . . . . .
H48A H 0.5349 0.3459 0.6965 0.135 Uiso 1 1 calc R U . . .
H48B H 0.4832 0.4340 0.6848 0.135 Uiso 1 1 calc R U . . .
C42 C 0.3836(7) 0.3011(4) 0.9705(3) 0.095(2) Uani 1 1 d . . . . .
H42A H 0.4521 0.3116 0.9791 0.115 Uiso 1 1 calc R U . . .
H42B H 0.3563 0.2824 1.0059 0.115 Uiso 1 1 calc R U . . .
C50 C 0.9572(6) 0.6803(6) 0.6922(6) 0.149(4) Uani 1 1 d . U . . .
H50A H 0.9446 0.6997 0.7309 0.179 Uiso 1 1 calc R U . . .
H50B H 0.9706 0.7296 0.6687 0.179 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Ge2 N8 1.938(3) . ?
Ge2 N4 1.990(3) . ?
Ge2 N10 2.051(3) . ?
Ge1 N3 1.940(3) . ?
Ge1 N7 1.960(3) . ?
Ge1 N1 2.038(3) . ?
Ge1 K004 3.4760(11) 2_656 ?
K003 O1 2.678(3) . ?
K003 O2 2.708(4) . ?
K003 N9 2.775(4) . ?
K003 C2 3.081(4) . ?
K003 C28 3.093(4) . ?
K003 C3 3.097(4) . ?
K003 C27 3.198(4) . ?
K003 C4 3.225(5) . ?
K003 C7 3.249(4) . ?
K003 C26 3.266(4) . ?
K003 C5 3.356(5) . ?
K003 C6 3.380(4) . ?
K004 O3 2.640(4) . ?
K004 N2 2.848(3) . ?
K004 N6 2.960(4) 2_646 ?
K004 N5 3.157(3) 2_646 ?
K004 C15 3.287(4) 2_646 ?
K004 Ge1 3.4760(11) 2_646 ?
K004 C19 3.515(4) 2_646 ?
K004 C9 3.522(4) . ?
N8 C28 1.363(5) . ?
N8 C21 1.387(4) . ?
N10 C39 1.392(5) . ?
N10 C35 1.394(5) . ?
N5 C19 1.350(5) . ?
N5 C15 1.355(5) . ?
N5 K004 3.157(3) 2_656 ?
N7 C29 1.381(5) . ?
N7 C21 1.416(4) . ?
N3 C1 1.369(5) . ?
N3 C8 1.376(5) . ?
N4 C15 1.370(5) . ?
N4 C8 1.416(5) . ?
N9 C35 1.315(5) . ?
N9 C28 1.379(5) . ?
N6 C29 1.347(5) . ?
N6 C33 1.346(5) . ?
N6 K004 2.960(4) 2_656 ?
N1 C9 1.384(5) . ?
N1 C13 1.387(5) . ?
O1 C44 1.402(7) . ?
O1 C41 1.423(7) . ?
N2 C9 1.329(5) . ?
N2 C1 1.374(5) . ?
O2 C48 1.412(7) . ?
O2 C45 1.422(6) . ?
C28 C27 1.410(5) . ?
C15 C16 1.408(5) . ?
C15 K004 3.287(4) 2_656 ?
C27 C26 1.409(5) . ?
C27 C22 1.446(5) . ?
C22 C21 1.380(5) . ?
C22 C23 1.414(5) . ?
C29 C30 1.409(5) . ?
O3 C49 1.412(8) . ?
O3 C52 1.432(7) . ?
C1 C2 1.400(5) . ?
C2 C3 1.421(6) . ?
C2 C7 1.449(5) . ?
C35 C36 1.451(5) . ?
C23 C24 1.375(6) . ?
C23 H23 0.9500 . ?
C39 C38 1.363(6) . ?
C39 C40 1.499(7) . ?
C26 C25 1.370(6) . ?
C26 H26 0.9500 . ?
C38 C37 1.405(7) . ?
C38 H38 0.9500 . ?
C3 C4 1.385(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.408(7) . ?
C4 H4 0.9500 . ?
C19 C18 1.371(6) . ?
C19 C20 1.506(6) . ?
C19 K004 3.515(4) 2_656 ?
C30 C31 1.361(6) . ?
C30 H30 0.9500 . ?
C36 C37 1.328(6) . ?
C36 H36 0.9500 . ?
C9 C10 1.445(6) . ?
C7 C8 1.380(5) . ?
C7 C6 1.422(6) . ?
C37 H37 0.9500 . ?
C25 C24 1.418(6) . ?
C25 H25 0.9500 . ?
C31 C32 1.396(6) . ?
C31 H31 0.9500 . ?
C16 C17 1.368(6) . ?
C16 H16 0.9500 . ?
C24 H24 0.9500 . ?
C5 C6 1.372(6) . ?
C5 H5 0.9500 . ?
C33 C32 1.368(6) . ?
C33 C34 1.508(6) . ?
C32 H32 0.9500 . ?
C10 C11 1.342(7) . ?
C10 H10 0.9500 . ?
C13 C12 1.355(7) . ?
C13 C14 1.482(7) . ?
C6 H6 0.9500 . ?
C11 C12 1.396(8) . ?
C11 H11 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C18 C17 1.390(7) . ?
C18 H18 0.9500 . ?
C12 H12 0.9500 . ?
C17 H17 0.9500 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C45 C46 1.481(9) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C46 C47 1.453(9) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.443(9) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C52 C51 1.501(11) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C44 C43 1.480(9) . ?
C44 H44 0.9500 . ?
C51 C50 1.477(10) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C49 C50 1.462(12) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C41 C42 1.533(10) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C43 C42 1.421(9) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?

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
N8 Ge2 N4 89.94(13) . . ?
N8 Ge2 N10 87.87(13) . . ?
N4 Ge2 N10 99.44(13) . . ?
N3 Ge1 N7 93.78(12) . . ?
N3 Ge1 N1 88.14(13) . . ?
N7 Ge1 N1 96.20(13) . . ?
N3 Ge1 K004 115.03(9) . 2_656 ?
N7 Ge1 K004 88.70(9) . 2_656 ?
N1 Ge1 K004 156.02(9) . 2_656 ?
O1 K003 O2 96.87(12) . . ?
O1 K003 N9 101.19(10) . . ?
O2 K003 N9 139.13(12) . . ?
O1 K003 C2 126.25(11) . . ?
O2 K003 C2 95.23(11) . . ?
N9 K003 C2 102.82(10) . . ?
O1 K003 C28 127.22(11) . . ?
O2 K003 C28 120.86(12) . . ?
N9 K003 C28 26.48(9) . . ?
C2 K003 C28 88.23(10) . . ?
O1 K003 C3 105.27(11) . . ?
O2 K003 C3 81.81(12) . . ?
N9 K003 C3 126.90(11) . . ?
C2 K003 C3 26.59(10) . . ?
C28 K003 C3 114.81(10) . . ?
O1 K003 C27 137.83(11) . . ?
O2 K003 C27 95.09(11) . . ?
N9 K003 C27 48.34(9) . . ?
C2 K003 C27 92.50(10) . . ?
C28 K003 C27 25.84(9) . . ?
C3 K003 C27 116.41(10) . . ?
O1 K003 C4 82.11(12) . . ?
O2 K003 C4 94.29(13) . . ?
N9 K003 C4 124.20(12) . . ?
C2 K003 C4 44.82(11) . . ?
C28 K003 C4 125.29(11) . . ?
C3 K003 C4 25.21(12) . . ?
C27 K003 C4 136.98(11) . . ?
O1 K003 C7 117.75(11) . . ?
O2 K003 C7 121.51(11) . . ?
N9 K003 C7 81.05(10) . . ?
C2 K003 C7 26.30(10) . . ?
C28 K003 C7 74.44(10) . . ?
C3 K003 C7 45.90(10) . . ?
C27 K003 C7 88.97(10) . . ?
C4 K003 C7 51.01(11) . . ?
O1 K003 C26 122.93(11) . . ?
O2 K003 C26 76.61(12) . . ?
N9 K003 C26 62.77(10) . . ?
C2 K003 C26 110.81(10) . . ?
C28 K003 C26 47.92(10) . . ?
C3 K003 C26 128.76(11) . . ?
C27 K003 C26 25.16(9) . . ?
C4 K003 C26 153.85(12) . . ?
C7 K003 C26 113.12(10) . . ?
O1 K003 C5 76.97(12) . . ?
O2 K003 C5 118.65(13) . . ?
N9 K003 C5 101.10(11) . . ?
C2 K003 C5 51.60(11) . . ?
C28 K003 C5 109.19(11) . . ?
C3 K003 C5 44.37(12) . . ?
C27 K003 C5 130.00(11) . . ?
C4 K003 C5 24.61(12) . . ?
C7 K003 C5 42.75(11) . . ?
C26 K003 C5 155.11(11) . . ?
O1 K003 C6 93.33(11) . . ?
O2 K003 C6 133.82(12) . . ?
N9 K003 C6 81.48(11) . . ?
C2 K003 C6 44.94(10) . . ?
C28 K003 C6 85.88(11) . . ?
C3 K003 C6 52.10(12) . . ?
C27 K003 C6 106.79(10) . . ?
C4 K003 C6 42.87(12) . . ?
C7 K003 C6 24.67(10) . . ?
C26 K003 C6 131.94(11) . . ?
C5 K003 C6 23.50(11) . . ?
O3 K004 N2 89.38(11) . . ?
O3 K004 N6 86.05(12) . 2_646 ?
N2 K004 N6 121.36(10) . 2_646 ?
O3 K004 N5 80.82(12) . 2_646 ?
N2 K004 N5 123.25(9) . 2_646 ?
N6 K004 N5 113.55(9) 2_646 2_646 ?
O3 K004 C15 103.35(12) . 2_646 ?
N2 K004 C15 131.43(10) . 2_646 ?
N6 K004 C15 106.32(9) 2_646 2_646 ?
N5 K004 C15 24.16(9) 2_646 2_646 ?
O3 K004 Ge1 132.78(10) . 2_646 ?
N2 K004 Ge1 132.51(8) . 2_646 ?
N6 K004 Ge1 55.98(7) 2_646 2_646 ?
N5 K004 Ge1 89.37(6) 2_646 2_646 ?
C15 K004 Ge1 67.63(7) 2_646 2_646 ?
O3 K004 C19 78.64(13) . 2_646 ?
N2 K004 C19 100.73(10) . 2_646 ?
N6 K004 C19 134.97(10) 2_646 2_646 ?
N5 K004 C19 22.53(8) 2_646 2_646 ?
C15 K004 C19 39.90(9) 2_646 2_646 ?
Ge1 K004 C19 107.43(7) 2_646 2_646 ?
O3 K004 C9 74.58(11) . . ?
N2 K004 C9 20.83(9) . . ?
N6 K004 C9 132.65(10) 2_646 . ?
N5 K004 C9 105.52(9) 2_646 . ?
C15 K004 C9 119.93(10) 2_646 . ?
Ge1 K004 C9 151.44(7) 2_646 . ?
C19 K004 C9 83.42(9) 2_646 . ?
C28 N8 C21 109.5(3) . . ?
C28 N8 Ge2 129.1(2) . . ?
C21 N8 Ge2 121.2(2) . . ?
C39 N10 C35 118.5(3) . . ?
C39 N10 Ge2 115.7(3) . . ?
C35 N10 Ge2 125.8(2) . . ?
C19 N5 C15 119.1(3) . . ?
C19 N5 K004 93.8(2) . 2_656 ?
C15 N5 K004 83.3(2) . 2_656 ?
C29 N7 C21 119.1(3) . . ?
C29 N7 Ge1 122.1(2) . . ?
C21 N7 Ge1 118.7(2) . . ?
C1 N3 C8 109.5(3) . . ?
C1 N3 Ge1 126.9(2) . . ?
C8 N3 Ge1 122.8(2) . . ?
C15 N4 C8 117.3(3) . . ?
C15 N4 Ge2 120.0(2) . . ?
C8 N4 Ge2 122.7(2) . . ?
C35 N9 C28 123.3(3) . . ?
C35 N9 K003 119.1(3) . . ?
C28 N9 K003 89.7(2) . . ?
C29 N6 C33 118.5(3) . . ?
C29 N6 K004 116.6(2) . 2_656 ?
C33 N6 K004 107.5(3) . 2_656 ?
C9 N1 C13 119.4(4) . . ?
C9 N1 Ge1 124.8(3) . . ?
C13 N1 Ge1 115.7(3) . . ?
C44 O1 C41 106.6(5) . . ?
C44 O1 K003 117.8(4) . . ?
C41 O1 K003 129.8(4) . . ?
C9 N2 C1 122.5(3) . . ?
C9 N2 K004 109.5(2) . . ?
C1 N2 K004 112.6(2) . . ?
C48 O2 C45 108.1(4) . . ?
C48 O2 K003 111.6(4) . . ?
C45 O2 K003 133.2(4) . . ?
N8 C28 N9 126.3(3) . . ?
N8 C28 C27 108.2(3) . . ?
N9 C28 C27 125.2(3) . . ?
N8 C28 K003 125.8(2) . . ?
N9 C28 K003 63.8(2) . . ?
C27 C28 K003 81.3(2) . . ?
N5 C15 N4 115.3(3) . . ?
N5 C15 C16 120.9(3) . . ?
N4 C15 C16 123.8(3) . . ?
N5 C15 K004 72.5(2) . 2_656 ?
N4 C15 K004 99.5(2) . 2_656 ?
C16 C15 K004 97.0(2) . 2_656 ?
C26 C27 C28 133.2(3) . . ?
C26 C27 C22 120.2(3) . . ?
C28 C27 C22 106.6(3) . . ?
C26 C27 K003 80.1(2) . . ?
C28 C27 K003 72.9(2) . . ?
C22 C27 K003 126.0(2) . . ?
C21 C22 C23 134.1(3) . . ?
C21 C22 C27 106.7(3) . . ?
C23 C22 C27 119.3(3) . . ?
N6 C29 N7 116.4(3) . . ?
N6 C29 C30 121.4(3) . . ?
N7 C29 C30 122.3(3) . . ?
C22 C21 N8 109.0(3) . . ?
C22 C21 N7 132.1(3) . . ?
N8 C21 N7 118.4(3) . . ?
C49 O3 C52 106.8(5) . . ?
C49 O3 K004 129.3(4) . . ?
C52 O3 K004 121.5(4) . . ?
N3 C1 N2 126.3(3) . . ?
N3 C1 C2 108.1(3) . . ?
N2 C1 C2 125.5(3) . . ?
C1 C2 C3 133.8(4) . . ?
C1 C2 C7 106.7(3) . . ?
C3 C2 C7 119.4(4) . . ?
C1 C2 K003 109.0(2) . . ?
C3 C2 K003 77.4(2) . . ?
C7 C2 K003 83.4(2) . . ?
N9 C35 N10 126.3(3) . . ?
N9 C35 C36 116.0(4) . . ?
N10 C35 C36 117.7(4) . . ?
C24 C23 C22 118.7(4) . . ?
C24 C23 H23 120.6 . . ?
C22 C23 H23 120.6 . . ?
C38 C39 N10 122.0(4) . . ?
C38 C39 C40 120.3(4) . . ?
N10 C39 C40 117.7(4) . . ?
C25 C26 C27 119.0(4) . . ?
C25 C26 K003 126.3(3) . . ?
C27 C26 K003 74.7(2) . . ?
C25 C26 H26 120.5 . . ?
C27 C26 H26 120.5 . . ?
K003 C26 H26 71.1 . . ?
C39 C38 C37 120.1(4) . . ?
C39 C38 H38 119.9 . . ?
C37 C38 H38 119.9 . . ?
C4 C3 C2 118.2(4) . . ?
C4 C3 K003 82.5(3) . . ?
C2 C3 K003 76.1(2) . . ?
C4 C3 H3 120.9 . . ?
C2 C3 H3 120.9 . . ?
K003 C3 H3 111.2 . . ?
C3 C4 C5 122.5(4) . . ?
C3 C4 K003 72.2(3) . . ?
C5 C4 K003 82.9(3) . . ?
C3 C4 H4 118.8 . . ?
C5 C4 H4 118.8 . . ?
K003 C4 H4 116.4 . . ?
N5 C19 C18 122.4(4) . . ?
N5 C19 C20 114.4(4) . . ?
C18 C19 C20 123.2(4) . . ?
N5 C19 K004 63.7(2) . 2_656 ?
C18 C19 K004 98.5(3) . 2_656 ?
C20 C19 K004 106.7(3) . 2_656 ?
C31 C30 C29 118.6(4) . . ?
C31 C30 H30 120.7 . . ?
C29 C30 H30 120.7 . . ?
C37 C36 C35 122.0(5) . . ?
C37 C36 H36 119.0 . . ?
C35 C36 H36 119.0 . . ?
N2 C9 N1 126.7(4) . . ?
N2 C9 C10 115.9(4) . . ?
N1 C9 C10 117.4(4) . . ?
N2 C9 K004 49.7(2) . . ?
N1 C9 K004 133.9(3) . . ?
C10 C9 K004 86.8(3) . . ?
C8 C7 C6 133.8(4) . . ?
C8 C7 C2 106.4(3) . . ?
C6 C7 C2 119.8(4) . . ?
C8 C7 K003 114.0(2) . . ?
C6 C7 K003 82.8(2) . . ?
C2 C7 K003 70.3(2) . . ?
C36 C37 C38 119.2(4) . . ?
C36 C37 H37 120.4 . . ?
C38 C37 H37 120.4 . . ?
C26 C25 C24 121.0(4) . . ?
C26 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
C30 C31 C32 120.1(4) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C17 C16 C15 118.9(4) . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
C23 C24 C25 121.8(4) . . ?
C23 C24 H24 119.1 . . ?
C25 C24 H24 119.1 . . ?
C6 C5 C4 120.9(4) . . ?
C6 C5 K003 79.2(3) . . ?
C4 C5 K003 72.5(3) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
K003 C5 H5 119.7 . . ?
N3 C8 C7 109.1(3) . . ?
N3 C8 N4 121.2(3) . . ?
C7 C8 N4 129.7(3) . . ?
N6 C33 C32 123.1(4) . . ?
N6 C33 C34 115.7(4) . . ?
C32 C33 C34 121.1(4) . . ?
C33 C32 C31 118.1(4) . . ?
C33 C32 H32 120.9 . . ?
C31 C32 H32 120.9 . . ?
C11 C10 C9 121.7(5) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C12 C13 N1 122.1(4) . . ?
C12 C13 C14 120.1(4) . . ?
N1 C13 C14 117.9(4) . . ?
C5 C6 C7 119.2(4) . . ?
C5 C6 K003 77.3(3) . . ?
C7 C6 K003 72.5(2) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
K003 C6 H6 121.0 . . ?
C10 C11 C12 119.4(5) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C18 C17 118.7(4) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
C13 C12 C11 119.9(4) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C16 C17 C18 120.0(4) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O2 C45 C46 107.1(5) . . ?
O2 C45 H45A 110.3 . . ?
C46 C45 H45A 110.3 . . ?
O2 C45 H45B 110.3 . . ?
C46 C45 H45B 110.3 . . ?
H45A C45 H45B 108.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C47 C46 C45 106.0(5) . . ?
C47 C46 H46A 110.5 . . ?
C45 C46 H46A 110.5 . . ?
C47 C46 H46B 110.5 . . ?
C45 C46 H46B 110.5 . . ?
H46A C46 H46B 108.7 . . ?
C48 C47 C46 105.2(6) . . ?
C48 C47 H47A 110.7 . . ?
C46 C47 H47A 110.7 . . ?
C48 C47 H47B 110.7 . . ?
C46 C47 H47B 110.7 . . ?
H47A C47 H47B 108.8 . . ?
O3 C52 C51 106.0(5) . . ?
O3 C52 H52A 110.5 . . ?
C51 C52 H52A 110.5 . . ?
O3 C52 H52B 110.5 . . ?
C51 C52 H52B 110.5 . . ?
H52A C52 H52B 108.7 . . ?
O1 C44 C43 107.8(5) . . ?
O1 C44 H44 126.1 . . ?
C43 C44 H44 126.1 . . ?
C50 C51 C52 104.2(6) . . ?
C50 C51 H51A 110.9 . . ?
C52 C51 H51A 110.9 . . ?
C50 C51 H51B 110.9 . . ?
C52 C51 H51B 110.9 . . ?
H51A C51 H51B 108.9 . . ?
O3 C49 C50 106.5(6) . . ?
O3 C49 H49A 110.4 . . ?
C50 C49 H49A 110.4 . . ?
O3 C49 H49B 110.4 . . ?
C50 C49 H49B 110.4 . . ?
H49A C49 H49B 108.6 . . ?
O1 C41 C42 104.5(5) . . ?
O1 C41 H41A 110.9 . . ?
C42 C41 H41A 110.9 . . ?
O1 C41 H41B 110.9 . . ?
C42 C41 H41B 110.9 . . ?
H41A C41 H41B 108.9 . . ?
C42 C43 C44 107.2(6) . . ?
C42 C43 H43A 110.3 . . ?
C44 C43 H43A 110.3 . . ?
C42 C43 H43B 110.3 . . ?
C44 C43 H43B 110.3 . . ?
H43A C43 H43B 108.5 . . ?
O2 C48 C47 109.5(5) . . ?
O2 C48 K003 46.3(3) . . ?
C47 C48 K003 142.8(6) . . ?
O2 C48 H48A 109.8 . . ?
C47 C48 H48A 109.8 . . ?
K003 C48 H48A 105.8 . . ?
O2 C48 H48B 109.8 . . ?
C47 C48 H48B 109.8 . . ?
K003 C48 H48B 67.7 . . ?
H48A C48 H48B 108.2 . . ?
C43 C42 C41 104.8(6) . . ?
C43 C42 H42A 110.8 . . ?
C41 C42 H42A 110.8 . . ?
C43 C42 H42B 110.8 . . ?
C41 C42 H42B 110.8 . . ?
H42A C42 H42B 108.9 . . ?
C49 C50 C51 107.4(7) . . ?
C49 C50 H50A 110.2 . . ?
C51 C50 H50A 110.2 . . ?
C49 C50 H50B 110.2 . . ?
C51 C50 H50B 110.2 . . ?
H50A C50 H50B 108.5 . . ?

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
C21 N8 C28 N9 172.5(4) . . . . ?
Ge2 N8 C28 N9 -12.0(6) . . . . ?
C21 N8 C28 C27 -1.5(4) . . . . ?
Ge2 N8 C28 C27 174.0(3) . . . . ?
C21 N8 C28 K003 90.9(3) . . . . ?
Ge2 N8 C28 K003 -93.7(3) . . . . ?
C35 N9 C28 N8 8.7(6) . . . . ?
K003 N9 C28 N8 -116.7(4) . . . . ?
C35 N9 C28 C27 -178.3(4) . . . . ?
K003 N9 C28 C27 56.4(4) . . . . ?
C35 N9 C28 K003 125.3(4) . . . . ?
C19 N5 C15 N4 176.9(3) . . . . ?
K004 N5 C15 N4 -92.5(3) 2_656 . . . ?
C19 N5 C15 C16 -2.9(6) . . . . ?
K004 N5 C15 C16 87.8(3) 2_656 . . . ?
C19 N5 C15 K004 -90.6(3) . . . 2_656 ?
C8 N4 C15 N5 -174.2(3) . . . . ?
Ge2 N4 C15 N5 5.3(4) . . . . ?
C8 N4 C15 C16 5.6(5) . . . . ?
Ge2 N4 C15 C16 -174.9(3) . . . . ?
C8 N4 C15 K004 110.7(3) . . . 2_656 ?
Ge2 N4 C15 K004 -69.8(2) . . . 2_656 ?
N8 C28 C27 C26 -177.3(4) . . . . ?
N9 C28 C27 C26 8.6(7) . . . . ?
K003 C28 C27 C26 57.7(4) . . . . ?
N8 C28 C27 C22 1.7(4) . . . . ?
N9 C28 C27 C22 -172.4(4) . . . . ?
K003 C28 C27 C22 -123.3(3) . . . . ?
N8 C28 C27 K003 125.0(3) . . . . ?
N9 C28 C27 K003 -49.1(3) . . . . ?
C26 C27 C22 C21 177.9(3) . . . . ?
C28 C27 C22 C21 -1.2(4) . . . . ?
K003 C27 C22 C21 -81.9(4) . . . . ?
C26 C27 C22 C23 -3.0(6) . . . . ?
C28 C27 C22 C23 177.8(3) . . . . ?
K003 C27 C22 C23 97.2(4) . . . . ?
C33 N6 C29 N7 173.8(4) . . . . ?
K004 N6 C29 N7 -55.4(4) 2_656 . . . ?
C33 N6 C29 C30 -5.8(6) . . . . ?
K004 N6 C29 C30 125.0(3) 2_656 . . . ?
C21 N7 C29 N6 173.7(3) . . . . ?
Ge1 N7 C29 N6 -2.0(5) . . . . ?
C21 N7 C29 C30 -6.7(5) . . . . ?
Ge1 N7 C29 C30 177.6(3) . . . . ?
C23 C22 C21 N8 -178.5(4) . . . . ?
C27 C22 C21 N8 0.4(4) . . . . ?
C23 C22 C21 N7 -7.5(7) . . . . ?
C27 C22 C21 N7 171.4(4) . . . . ?
C28 N8 C21 C22 0.7(4) . . . . ?
Ge2 N8 C21 C22 -175.2(2) . . . . ?
C28 N8 C21 N7 -171.8(3) . . . . ?
Ge2 N8 C21 N7 12.3(4) . . . . ?
C29 N7 C21 C22 101.3(5) . . . . ?
Ge1 N7 C21 C22 -82.9(5) . . . . ?
C29 N7 C21 N8 -88.4(4) . . . . ?
Ge1 N7 C21 N8 87.4(3) . . . . ?
C8 N3 C1 N2 173.2(3) . . . . ?
Ge1 N3 C1 N2 -16.8(5) . . . . ?
C8 N3 C1 C2 -2.2(4) . . . . ?
Ge1 N3 C1 C2 167.9(2) . . . . ?
C9 N2 C1 N3 -5.7(6) . . . . ?
K004 N2 C1 N3 128.1(3) . . . . ?
C9 N2 C1 C2 168.9(4) . . . . ?
K004 N2 C1 C2 -57.3(4) . . . . ?
N3 C1 C2 C3 -178.1(4) . . . . ?
N2 C1 C2 C3 6.5(7) . . . . ?
N3 C1 C2 C7 2.7(4) . . . . ?
N2 C1 C2 C7 -172.7(3) . . . . ?
N3 C1 C2 K003 91.4(3) . . . . ?
N2 C1 C2 K003 -84.1(4) . . . . ?
C28 N9 C35 N10 3.2(6) . . . . ?
K003 N9 C35 N10 114.2(4) . . . . ?
C28 N9 C35 C36 -178.8(4) . . . . ?
K003 N9 C35 C36 -67.8(4) . . . . ?
C39 N10 C35 N9 170.4(4) . . . . ?
Ge2 N10 C35 N9 -10.7(6) . . . . ?
C39 N10 C35 C36 -7.6(5) . . . . ?
Ge2 N10 C35 C36 171.4(3) . . . . ?
C21 C22 C23 C24 179.9(4) . . . . ?
C27 C22 C23 C24 1.1(6) . . . . ?
C35 N10 C39 C38 5.5(6) . . . . ?
Ge2 N10 C39 C38 -173.5(3) . . . . ?
C35 N10 C39 C40 -173.4(4) . . . . ?
Ge2 N10 C39 C40 7.5(5) . . . . ?
C28 C27 C26 C25 -178.5(4) . . . . ?
C22 C27 C26 C25 2.7(6) . . . . ?
K003 C27 C26 C25 -123.4(4) . . . . ?
C28 C27 C26 K003 -55.1(4) . . . . ?
C22 C27 C26 K003 126.0(3) . . . . ?
N10 C39 C38 C37 -0.3(7) . . . . ?
C40 C39 C38 C37 178.7(5) . . . . ?
C1 C2 C3 C4 -177.8(4) . . . . ?
C7 C2 C3 C4 1.3(6) . . . . ?
K003 C2 C3 C4 -73.5(4) . . . . ?
C1 C2 C3 K003 -104.4(5) . . . . ?
C7 C2 C3 K003 74.8(3) . . . . ?
C2 C3 C4 C5 0.7(7) . . . . ?
K003 C3 C4 C5 -69.1(5) . . . . ?
C2 C3 C4 K003 69.8(4) . . . . ?
C15 N5 C19 C18 1.3(6) . . . . ?
K004 N5 C19 C18 -83.2(4) 2_656 . . . ?
C15 N5 C19 C20 -178.2(4) . . . . ?
K004 N5 C19 C20 97.3(3) 2_656 . . . ?
C15 N5 C19 K004 84.5(3) . . . 2_656 ?
N6 C29 C30 C31 5.0(6) . . . . ?
N7 C29 C30 C31 -174.6(4) . . . . ?
N9 C35 C36 C37 -173.2(4) . . . . ?
N10 C35 C36 C37 5.0(6) . . . . ?
C1 N2 C9 N1 14.9(6) . . . . ?
K004 N2 C9 N1 -120.1(4) . . . . ?
C1 N2 C9 C10 -164.5(4) . . . . ?
K004 N2 C9 C10 60.4(4) . . . . ?
C1 N2 C9 K004 135.1(4) . . . . ?
C13 N1 C9 N2 176.0(4) . . . . ?
Ge1 N1 C9 N2 -1.7(6) . . . . ?
C13 N1 C9 C10 -4.5(6) . . . . ?
Ge1 N1 C9 C10 177.8(3) . . . . ?
C13 N1 C9 K004 109.7(4) . . . . ?
Ge1 N1 C9 K004 -68.0(4) . . . . ?
C1 C2 C7 C8 -2.3(4) . . . . ?
C3 C2 C7 C8 178.4(4) . . . . ?
K003 C2 C7 C8 -110.2(3) . . . . ?
C1 C2 C7 C6 177.0(3) . . . . ?
C3 C2 C7 C6 -2.4(6) . . . . ?
K003 C2 C7 C6 69.0(3) . . . . ?
C1 C2 C7 K003 107.9(3) . . . . ?
C3 C2 C7 K003 -71.4(3) . . . . ?
C35 C36 C37 C38 0.2(7) . . . . ?
C39 C38 C37 C36 -2.6(7) . . . . ?
C27 C26 C25 C24 -0.4(7) . . . . ?
K003 C26 C25 C24 -92.3(5) . . . . ?
C29 C30 C31 C32 -0.8(7) . . . . ?
N5 C15 C16 C17 1.9(6) . . . . ?
N4 C15 C16 C17 -177.9(4) . . . . ?
K004 C15 C16 C17 75.7(5) 2_656 . . . ?
C22 C23 C24 C25 1.2(7) . . . . ?
C26 C25 C24 C23 -1.5(7) . . . . ?
C3 C4 C5 C6 -1.6(8) . . . . ?
K003 C4 C5 C6 -65.3(5) . . . . ?
C3 C4 C5 K003 63.7(4) . . . . ?
C1 N3 C8 C7 0.8(4) . . . . ?
Ge1 N3 C8 C7 -169.8(3) . . . . ?
C1 N3 C8 N4 -179.9(3) . . . . ?
Ge1 N3 C8 N4 9.6(5) . . . . ?
C6 C7 C8 N3 -178.1(4) . . . . ?
C2 C7 C8 N3 1.0(4) . . . . ?
K003 C7 C8 N3 -74.4(3) . . . . ?
C6 C7 C8 N4 2.6(8) . . . . ?
C2 C7 C8 N4 -178.3(4) . . . . ?
K003 C7 C8 N4 106.3(4) . . . . ?
C15 N4 C8 N3 -99.2(4) . . . . ?
Ge2 N4 C8 N3 81.3(4) . . . . ?
C15 N4 C8 C7 80.0(5) . . . . ?
Ge2 N4 C8 C7 -99.4(4) . . . . ?
C29 N6 C33 C32 2.5(7) . . . . ?
K004 N6 C33 C32 -132.4(4) 2_656 . . . ?
C29 N6 C33 C34 -176.2(4) . . . . ?
K004 N6 C33 C34 49.0(5) 2_656 . . . ?
N6 C33 C32 C31 1.6(8) . . . . ?
C34 C33 C32 C31 -179.8(5) . . . . ?
C30 C31 C32 C33 -2.3(7) . . . . ?
N2 C9 C10 C11 -179.2(4) . . . . ?
N1 C9 C10 C11 1.3(7) . . . . ?
K004 C9 C10 C11 -137.6(5) . . . . ?
C9 N1 C13 C12 3.7(6) . . . . ?
Ge1 N1 C13 C12 -178.5(4) . . . . ?
C9 N1 C13 C14 -175.3(5) . . . . ?
Ge1 N1 C13 C14 2.6(6) . . . . ?
C4 C5 C6 C7 0.5(7) . . . . ?
K003 C5 C6 C7 -61.4(4) . . . . ?
C4 C5 C6 K003 61.9(5) . . . . ?
C8 C7 C6 C5 -179.6(5) . . . . ?
C2 C7 C6 C5 1.5(6) . . . . ?
K003 C7 C6 C5 63.9(4) . . . . ?
C8 C7 C6 K003 116.6(5) . . . . ?
C2 C7 C6 K003 -62.4(3) . . . . ?
C9 C10 C11 C12 3.0(8) . . . . ?
N5 C19 C18 C17 1.3(7) . . . . ?
C20 C19 C18 C17 -179.3(5) . . . . ?
K004 C19 C18 C17 -62.8(5) 2_656 . . . ?
N1 C13 C12 C11 0.7(8) . . . . ?
C14 C13 C12 C11 179.6(5) . . . . ?
C10 C11 C12 C13 -4.1(8) . . . . ?
C15 C16 C17 C18 0.7(8) . . . . ?
C19 C18 C17 C16 -2.3(8) . . . . ?
C48 O2 C45 C46 4.9(9) . . . . ?
K003 O2 C45 C46 151.7(5) . . . . ?
O2 C45 C46 C47 -16.0(9) . . . . ?
C45 C46 C47 C48 20.5(10) . . . . ?
C49 O3 C52 C51 30.0(9) . . . . ?
K004 O3 C52 C51 -134.2(5) . . . . ?
C41 O1 C44 C43 -25.5(9) . . . . ?
K003 O1 C44 C43 130.2(6) . . . . ?
O3 C52 C51 C50 -18.5(10) . . . . ?
C52 O3 C49 C50 -29.4(10) . . . . ?
K004 O3 C49 C50 133.1(7) . . . . ?
C44 O1 C41 C42 31.0(8) . . . . ?
K003 O1 C41 C42 -120.7(5) . . . . ?
O1 C44 C43 C42 8.9(10) . . . . ?
C45 O2 C48 C47 8.3(10) . . . . ?
K003 O2 C48 C47 -146.2(6) . . . . ?
C45 O2 C48 K003 154.6(6) . . . . ?
C46 C47 C48 O2 -18.2(11) . . . . ?
C46 C47 C48 K003 -59.8(13) . . . . ?
C44 C43 C42 C41 9.9(10) . . . . ?
O1 C41 C42 C43 -25.1(9) . . . . ?
O3 C49 C50 C51 17.2(12) . . . . ?
C52 C51 C50 C49 0.9(12) . . . . ?

_refine_diff_density_max         0.537
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.092



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jcm05321a
_database_code_depnum_ccdc_archive 'CCDC 2403139'
loop_
_audit_author_name
_audit_author_address
'Jesus Campos'
;CSIC
Spain
;
_audit_update_record             
;
2024-11-15 deposited with the CCDC.	2025-01-03 downloaded from the CCDC.
;
_audit_creation_date             2024-06-14

_vrf_PLAT331_jcm05321a           
;
PROBLEM: Small Aver Phenyl C-C Dist C53      --C58      .       1.35 Ang.  
RESPONSE: It refers to a disorder benzene solvent molecule that
has been constrained to be an hexagon with AFIX 66, so there is nothing
problematic.
;




_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_chemical_formula_moiety         
'C48 H60 Ag2 Ge2 N12 Si4, 2(C2 F6 N O4 S2), 2(C6 H6)'
_chemical_formula_sum            'C64 H72 Ag2 F12 Ge2 N14 O8 S4 Si4'
_chemical_formula_weight         1994.923
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
Ag -0.87490 1.10631 19.28080 16.68850 4.80450 1.04630 0.64460 7.47260 24.66050
99.81560 5.17900 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
C 0.00313 0.00162 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.21560 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
F 0.01756 0.01033 3.53920 2.64120 1.51700 1.02430 10.28250 4.29440 0.26150
26.14760 0.27760 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
Ge 0.15877 1.81111 16.08160 6.37470 3.70680 3.68300 2.85090 0.25160 11.44680
54.76250 2.13130 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.00304 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
N 0.00612 0.00332 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.52900 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
O 0.01085 0.00610 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.25080 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
S 0.12485 0.12449 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360
56.17200 0.86690 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
Si 0.08275 0.07119 6.29150 3.03530 1.98910 1.54100 2.43860 32.33370 0.67850
81.69370 1.14070 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z

_symmetry_Int_Tables_number      2
_cell_length_a                   15.8097(14)
_cell_length_b                   16.6796(15)
_cell_length_c                   17.6314(15)
_cell_angle_alpha                99.488(4)
_cell_angle_beta                 102.293(4)
_cell_angle_gamma                109.977(4)
_cell_volume                     4124.1(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.45
_exptl_absorpt_coefficient_mu    1.435
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1311 before and 0.0982 after correction.
The Ratio of minimum to maximum transmission is 0.7703.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             2008.379
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_Laue_measured_fraction_full 0.9985
_diffrn_reflns_Laue_measured_fraction_max 0.9934
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            20453
_diffrn_reflns_point_group_measured_fraction_full 0.9985
_diffrn_reflns_point_group_measured_fraction_max 0.9934
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.92
_diffrn_ambient_temperature      193.00
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9934
_diffrn_measurement_device_type  'Apex3 v2016.9-0 (Bruker, 2016)'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              20
_reflns_limit_h_min              -21
_reflns_limit_k_max              21
_reflns_limit_k_min              -22
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                12262
_reflns_number_total             20453
_reflns_threshold_expression     I>=2u(I)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.4037
_refine_diff_density_min         -1.9845
_refine_diff_density_rms         0.2755
_refine_ls_d_res_high            0.7487
_refine_ls_d_res_low             10.6082
_refine_ls_goodness_of_fit_ref   1.1917
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    121
_refine_ls_number_parameters     992
_refine_ls_number_reflns         20453
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1665
_refine_ls_R_factor_gt           0.0926
_refine_ls_restrained_S_all      1.1906
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2515
_refine_ls_wR_factor_ref         0.3394
_refine_special_details          ?
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.743(2)
 0.257(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 C59, C60, C61, C62, C63, C64
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C15(H15),
 C16(H16), C17(H17), C18(H18), C25(H25), C26(H26), C27(H27), C28(H28), C32(H32),
  C33(H33), C34(H34), C35(H35), C39(H39), C40(H40), C41(H41), C42(H42),
 C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C59(H59),
  C64(H64), C63(H63), C62(H62), C61(H61)
4.b Fitted hexagon refined as free rotating group:
 C60(C59,C64,C63,C62,C61)
4.c Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C21(H21a,H21b,H21c), C22(H22a,H22b,
 H22c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C43(H43a,H43b,H43c), C44(H44a,
 H44b,H44c), C45(H45a,H45b,H45c), C46(H46a,H46b,H46c), C47(H47a,H47b,H47c),
 C48(H48a,H48b,H48c)
;
_atom_sites_solution_primary     dual
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_refinement_flags_posn
_atom_site_refinement_flags_adp
Ag1 Ag 0.79050(6) 0.79489(5) 0.41262(5) 0.0443(2) Uani 1.000000 . .
Ag2 Ag 0.94604(5) 0.80661(5) 0.21276(5) 0.0453(2) Uani 1.000000 . .
Ge1 Ge 0.89406(7) 0.73024(6) 0.47172(6) 0.0331(2) Uani 1.000000 . .
Ge2 Ge 0.79000(7) 0.72573(7) 0.12300(6) 0.0361(2) Uani 1.000000 . .
S1 S 0.6094(2) 0.75823(18) 0.56489(17) 0.0454(6) Uani 1.000000 . .
S2 S 0.4676(2) 0.82200(18) 0.55533(17) 0.0476(6) Uani 1.000000 . .
Si1 Si 1.0602(2) 0.7227(2) 0.60419(18) 0.0488(7) Uani 1.000000 . .
Si2 Si 0.9979(2) 0.87629(19) 0.62927(18) 0.0474(7) Uani 1.000000 . .
Si3 Si 0.6087(2) 0.6878(2) -0.01668(18) 0.0495(7) Uani 1.000000 . .
Si4 Si 0.7775(2) 0.8625(2) 0.02839(18) 0.0494(7) Uani 1.000000 . .
F1 F 0.6818(8) 0.7044(6) 0.6810(5) 0.096(3) Uani 1.000000 . .
F2 F 0.5799(8) 0.7512(9) 0.7031(6) 0.108(4) Uani 1.000000 . .
F3 F 0.7118(8) 0.8393(7) 0.7134(6) 0.108(4) Uani 1.000000 . .
F4 F 0.3249(6) 0.7780(7) 0.4287(6) 0.097(3) Uani 1.000000 . .
F5 F 0.4507(7) 0.8772(8) 0.4268(6) 0.108(3) Uani 1.000000 . .
F6 F 0.4352(7) 0.7414(8) 0.4057(5) 0.101(3) Uani 1.000000 . .
O1 O 0.5403(6) 0.6703(5) 0.5307(6) 0.065(2) Uani 1.000000 . .
O2 O 0.6942(6) 0.7828(7) 0.5420(6) 0.070(3) Uani 1.000000 . .
O3 O 0.4093(6) 0.7433(6) 0.5714(6) 0.061(2) Uani 1.000000 . .
O4 O 0.4649(8) 0.9030(6) 0.5902(7) 0.080(3) Uani 1.000000 . .
N1 N 0.8110(6) 0.6105(5) 0.4798(5) 0.0394(17) Uani 1.000000 . .
N2 N 0.8323(6) 0.5189(5) 0.3695(5) 0.0411(18) Uani 1.000000 . .
N3 N 0.9400(6) 0.6705(5) 0.3979(5) 0.0361(16) Uani 1.000000 . .
N4 N 1.0455(6) 0.8014(5) 0.3913(5) 0.0381(17) Uani 1.000000 . .
N5 N 1.0882(5) 0.8746(5) 0.2925(4) 0.0342(16) Uani 1.000000 . .
N6 N 0.7889(6) 0.6088(5) 0.0671(5) 0.0379(17) Uani 1.000000 . .
N7 N 0.7022(6) 0.5156(5) 0.1392(5) 0.0405(18) Uani 1.000000 . .
N8 N 0.6998(6) 0.6607(5) 0.1701(5) 0.0390(17) Uani 1.000000 . .
N9 N 0.6884(6) 0.7881(5) 0.2279(5) 0.0417(18) Uani 1.000000 . .
N10 N 0.7011(5) 0.8581(5) 0.3607(4) 0.0328(15) Uani 1.000000 . .
N11 N 0.9834(6) 0.7734(6) 0.5703(5) 0.0412(18) Uani 1.000000 . .
N12 N 0.7267(6) 0.7552(6) 0.0392(5) 0.0421(18) Uani 1.000000 . .
N13 N 0.5716(6) 0.8336(6) 0.5632(6) 0.046(2) Uani 1.000000 . .
C1 C 0.7681(7) 0.6158(7) 0.5382(6) 0.042(2) Uani 1.000000 . .
H1 H 0.7806(7) 0.6725(7) 0.5703(6) 0.051(3) Uiso 1.000000 R .
C2 C 0.7080(8) 0.5434(8) 0.5526(6) 0.052(3) Uani 1.000000 . .
H2 H 0.6781(8) 0.5497(8) 0.5933(6) 0.063(3) Uiso 1.000000 R .
C3 C 0.6907(8) 0.4606(7) 0.5073(7) 0.051(3) Uani 1.000000 . .
H3 H 0.6508(8) 0.4091(7) 0.5177(7) 0.061(3) Uiso 1.000000 R .
C4 C 0.7330(8) 0.4539(7) 0.4460(6) 0.047(2) Uani 1.000000 . .
H4 H 0.7206(8) 0.3975(7) 0.4135(6) 0.056(3) Uiso 1.000000 R .
C5 C 0.7940(7) 0.5309(6) 0.4322(6) 0.038(2) Uani 1.000000 . .
C6 C 0.8962(6) 0.5826(6) 0.3571(5) 0.0344(19) Uani 1.000000 . .
C7 C 0.9363(7) 0.5718(6) 0.2901(5) 0.0368(19) Uani 1.000000 . .
C8 C 0.9160(8) 0.4960(7) 0.2310(6) 0.049(3) Uani 1.000000 . .
H8 H 0.8730(8) 0.4399(7) 0.2309(6) 0.058(3) Uiso 1.000000 R .
C9 C 0.9620(8) 0.5064(7) 0.1716(6) 0.050(2) Uani 1.000000 . .
H9 H 0.9481(8) 0.4562(7) 0.1293(6) 0.060(3) Uiso 1.000000 R .
C10 C 1.0255(9) 0.5854(7) 0.1719(7) 0.051(3) Uani 1.000000 . .
H10 H 1.0543(9) 0.5897(7) 0.1299(7) 0.061(3) Uiso 1.000000 R .
C11 C 1.0494(7) 0.6615(7) 0.2341(6) 0.042(2) Uani 1.000000 . .
H11 H 1.0968(7) 0.7163(7) 0.2367(6) 0.050(3) Uiso 1.000000 R .
C12 C 1.0011(7) 0.6533(6) 0.2915(6) 0.038(2) Uani 1.000000 . .
C13 C 1.0041(6) 0.7178(6) 0.3618(5) 0.0340(18) Uani 1.000000 . .
C14 C 1.1142(6) 0.8561(6) 0.3626(5) 0.0328(18) Uani 1.000000 . .
C15 C 1.2071(7) 0.8955(7) 0.4096(7) 0.045(2) Uani 1.000000 . .
H15 H 1.2246(7) 0.8838(7) 0.4603(7) 0.054(3) Uiso 1.000000 R .
C16 C 1.2726(8) 0.9503(7) 0.3834(7) 0.053(3) Uani 1.000000 . .
H16 H 1.3368(8) 0.9755(7) 0.4146(7) 0.063(3) Uiso 1.000000 R .
C17 C 1.2459(8) 0.9697(7) 0.3106(7) 0.051(3) Uani 1.000000 . .
H17 H 1.2906(8) 1.0089(7) 0.2914(7) 0.062(3) Uiso 1.000000 R .
C18 C 1.1521(8) 0.9300(7) 0.2674(7) 0.048(2) Uani 1.000000 . .
H18 H 1.1325(8) 0.9427(7) 0.2176(7) 0.057(3) Uiso 1.000000 R .
C19 C 1.0035(10) 0.6014(8) 0.5695(8) 0.064(4) Uani 1.000000 . .
H19a H 0.947(4) 0.5806(9) 0.587(5) 0.096(5) Uiso 1.000000 GR .
H19b H 0.986(6) 0.5832(9) 0.5107(9) 0.096(5) Uiso 1.000000 GR .
H19c H 1.047(3) 0.5759(8) 0.592(5) 0.096(5) Uiso 1.000000 GR .
C20 C 1.1025(11) 0.7518(14) 0.7187(9) 0.090(5) Uani 1.000000 . .
H20a H 1.122(8) 0.8154(19) 0.7402(9) 0.135(8) Uiso 1.000000 GR .
H20b H 1.051(3) 0.719(7) 0.7390(9) 0.135(8) Uiso 1.000000 GR .
H20c H 1.156(6) 0.736(8) 0.7358(9) 0.135(8) Uiso 1.000000 GR .
C21 C 1.1641(9) 0.7582(11) 0.5668(9) 0.071(4) Uani 1.000000 . .
H21a H 1.1436(10) 0.744(7) 0.5080(9) 0.107(6) Uiso 1.000000 GR .
H21b H 1.199(4) 0.8220(16) 0.589(5) 0.107(6) Uiso 1.000000 GR .
H21c H 1.204(4) 0.727(6) 0.584(6) 0.107(6) Uiso 1.000000 GR .
C22 C 0.9304(12) 0.9344(9) 0.5730(9) 0.073(4) Uani 1.000000 . .
H22a H 0.947(6) 0.939(7) 0.523(3) 0.110(6) Uiso 1.000000 GR .
H22b H 0.8627(12) 0.901(4) 0.561(6) 0.110(6) Uiso 1.000000 GR .
H22c H 0.947(6) 0.994(3) 0.606(3) 0.110(6) Uiso 1.000000 GR .
C23 C 1.1231(9) 0.9544(10) 0.6624(10) 0.079(4) Uani 1.000000 . .
H23a H 1.1602(17) 0.934(4) 0.700(5) 0.118(7) Uiso 1.000000 GR .
H23b H 1.147(3) 0.958(6) 0.6156(13) 0.118(7) Uiso 1.000000 GR .
H23c H 1.1282(13) 1.013(2) 0.689(6) 0.118(7) Uiso 1.000000 GR .
C24 C 0.9522(11) 0.8620(9) 0.7176(8) 0.073(4) Uani 1.000000 . .
H24a H 0.895(4) 0.808(4) 0.7015(17) 0.109(6) Uiso 1.000000 GR .
H24b H 1.000(3) 0.857(7) 0.760(2) 0.109(6) Uiso 1.000000 GR .
H24c H 0.938(7) 0.913(3) 0.737(4) 0.109(6) Uiso 1.000000 GR .
C25 C 0.8380(8) 0.6168(8) 0.0117(6) 0.047(2) Uani 1.000000 . .
H25 H 0.8683(8) 0.6735(8) 0.0040(6) 0.057(3) Uiso 1.000000 R .
C26 C 0.8445(9) 0.5442(8) -0.0334(7) 0.054(3) Uani 1.000000 . .
H26 H 0.8795(9) 0.5511(8) -0.0713(7) 0.064(3) Uiso 1.000000 R .
C27 C 0.7999(9) 0.4620(8) -0.0229(7) 0.057(3) Uani 1.000000 . .
H27 H 0.8002(9) 0.4108(8) -0.0556(7) 0.068(3) Uiso 1.000000 R .
C28 C 0.7551(8) 0.4553(7) 0.0354(6) 0.048(2) Uani 1.000000 . .
H28 H 0.7270(8) 0.3991(7) 0.0450(6) 0.058(3) Uiso 1.000000 R .
C29 C 0.7497(7) 0.5294(7) 0.0817(6) 0.041(2) Uani 1.000000 . .
C30 C 0.6821(7) 0.5759(6) 0.1775(5) 0.0353(19) Uani 1.000000 . .
C31 C 0.6332(7) 0.5644(6) 0.2397(5) 0.0373(19) Uani 1.000000 . .
C32 C 0.6008(8) 0.4918(7) 0.2697(6) 0.050(2) Uani 1.000000 . .
H32 H 0.6097(8) 0.4393(7) 0.2511(6) 0.059(3) Uiso 1.000000 R .
C33 C 0.5553(8) 0.4980(7) 0.3276(6) 0.050(3) Uani 1.000000 . .
H33 H 0.5317(8) 0.4483(7) 0.3481(6) 0.060(3) Uiso 1.000000 R .
C34 C 0.5427(8) 0.5745(8) 0.3572(7) 0.056(3) Uani 1.000000 . .
H34 H 0.5106(8) 0.5767(8) 0.3969(7) 0.067(3) Uiso 1.000000 R .
C35 C 0.5777(8) 0.6478(7) 0.3277(7) 0.049(2) Uani 1.000000 . .
H35 H 0.5707(8) 0.7009(7) 0.3478(7) 0.059(3) Uiso 1.000000 R .
C36 C 0.6235(7) 0.6431(6) 0.2682(6) 0.0376(19) Uani 1.000000 . .
C37 C 0.6698(6) 0.7059(6) 0.2257(5) 0.0357(19) Uani 1.000000 . .
C38 C 0.6661(7) 0.8439(6) 0.2823(5) 0.038(2) Uani 1.000000 . .
C39 C 0.6131(8) 0.8882(8) 0.2525(7) 0.050(3) Uani 1.000000 . .
H39 H 0.5891(8) 0.8782(8) 0.1961(7) 0.060(3) Uiso 1.000000 R .
C40 C 0.5949(8) 0.9469(8) 0.3045(8) 0.057(3) Uani 1.000000 . .
H40 H 0.5565(8) 0.9765(8) 0.2849(8) 0.068(3) Uiso 1.000000 R .
C41 C 0.6328(8) 0.9613(7) 0.3837(7) 0.052(3) Uani 1.000000 . .
H41 H 0.6217(8) 1.0018(7) 0.4209(7) 0.063(3) Uiso 1.000000 R .
C42 C 0.6874(8) 0.9177(7) 0.4109(6) 0.046(2) Uani 1.000000 . .
H42 H 0.7160(8) 0.9304(7) 0.4670(6) 0.055(3) Uiso 1.000000 R .
C43 C 0.8920(12) 0.9287(9) 0.1069(9) 0.086(5) Uani 1.000000 . .
H43a H 0.884(2) 0.925(7) 0.1600(11) 0.129(8) Uiso 1.000000 GR .
H43b H 0.939(3) 0.906(5) 0.097(4) 0.129(8) Uiso 1.000000 GR .
H43c H 0.913(4) 0.9906(18) 0.105(5) 0.129(8) Uiso 1.000000 GR .
C44 C 0.7002(11) 0.9219(10) 0.0390(10) 0.082(4) Uani 1.000000 . .
H44a H 0.645(4) 0.898(5) -0.009(3) 0.123(7) Uiso 1.000000 GR .
H44b H 0.679(7) 0.915(7) 0.087(4) 0.123(7) Uiso 1.000000 GR .
H44c H 0.735(3) 0.9848(16) 0.044(7) 0.123(7) Uiso 1.000000 GR .
C45 C 0.8050(13) 0.8610(11) -0.0693(8) 0.089(5) Uani 1.000000 . .
H45a H 0.837(8) 0.821(7) -0.078(4) 0.133(8) Uiso 1.000000 GR .
H45b H 0.7464(15) 0.841(8) -0.1130(11) 0.133(8) Uiso 1.000000 GR .
H45c H 0.846(8) 0.921(2) -0.068(3) 0.133(8) Uiso 1.000000 GR .
C46 C 0.5232(10) 0.6982(12) 0.0380(9) 0.080(4) Uani 1.000000 . .
H46a H 0.538(5) 0.683(8) 0.089(3) 0.120(7) Uiso 1.000000 GR .
H46b H 0.527(6) 0.759(2) 0.048(6) 0.120(7) Uiso 1.000000 GR .
H46c H 0.4595(13) 0.658(6) 0.005(3) 0.120(7) Uiso 1.000000 GR .
C47 C 0.5780(11) 0.7128(10) -0.1157(8) 0.078(4) Uani 1.000000 . .
H47a H 0.600(7) 0.7769(10) -0.1081(12) 0.117(7) Uiso 1.000000 GR .
H47b H 0.608(7) 0.689(7) -0.152(2) 0.117(7) Uiso 1.000000 GR .
H47c H 0.5096(12) 0.686(7) -0.140(3) 0.117(7) Uiso 1.000000 GR .
C48 C 0.5885(7) 0.5689(7) -0.0435(6) 0.050(3) Uani 1.000000 . .
H48a H 0.640(3) 0.5620(9) -0.063(5) 0.075(4) Uiso 1.000000 GR .
H48b H 0.586(6) 0.5459(15) 0.0041(14) 0.075(4) Uiso 1.000000 GR .
H48c H 0.529(3) 0.5360(11) -0.086(4) 0.075(4) Uiso 1.000000 GR .
C49 C 0.6473(10) 0.7634(9) 0.6707(7) 0.058(3) Uani 1.000000 . .
C50 C 0.4170(9) 0.8022(12) 0.4482(9) 0.072(4) Uani 1.000000 . .
S3 S 0.3032(3) 0.8205(3) 0.1097(2) 0.0694(9) Uani 1.000000 . .
S4 S 0.1083(2) 0.7708(2) 0.05419(18) 0.0558(7) Uani 1.000000 . .
F7 F 0.2476(7) 0.7082(10) 0.1910(7) 0.123(4) Uani 1.000000 . .
F8 F 0.3949(7) 0.7548(9) 0.2022(8) 0.115(4) Uani 1.000000 . .
F9 F 0.3423(14) 0.8390(12) 0.2627(6) 0.185(8) Uani 1.000000 . .
F10 F 0.0062(9) 0.7714(10) -0.0803(6) 0.139(5) Uani 1.000000 . .
F11 F 0.1058(11) 0.8992(9) -0.0105(9) 0.142(5) Uani 1.000000 . .
F12 F 0.1526(11) 0.8121(11) -0.0713(7) 0.148(5) Uani 1.000000 . .
O5 O 0.2915(9) 0.7491(8) 0.0459(6) 0.093(3) Uani 1.000000 . .
O6 O 0.3799(9) 0.9001(9) 0.1261(11) 0.142(6) Uani 1.000000 . .
O7 O 0.0891(8) 0.6811(6) 0.0221(7) 0.083(3) Uani 1.000000 . .
O8 O 0.0429(8) 0.7899(8) 0.0918(6) 0.084(3) Uani 1.000000 . .
N14 N 0.2113(9) 0.8363(8) 0.1089(7) 0.072(3) Uani 1.000000 . .
C51 C 0.3220(11) 0.7795(12) 0.1959(9) 0.077(4) Uani 1.000000 . .
C52 C 0.0935(12) 0.8147(12) -0.0334(9) 0.079(4) Uani 1.000000 . .
C53 C 0.4440(17) 0.8553(16) 0.7881(14) 0.117(7) Uani 1.000000 . .
H53 H 0.4825(17) 0.8851(16) 0.7585(14) 0.140(9) Uiso 1.000000 R .
C54 C 0.3872(12) 0.7698(14) 0.7583(10) 0.085(5) Uani 1.000000 . .
H54 H 0.3841(12) 0.7398(14) 0.7064(10) 0.102(6) Uiso 1.000000 R .
C55 C 0.3361(11) 0.7268(11) 0.7993(12) 0.088(5) Uani 1.000000 . .
H55 H 0.2981(11) 0.6657(11) 0.7770(12) 0.105(6) Uiso 1.000000 R .
C56 C 0.3357(14) 0.7680(13) 0.8745(11) 0.092(5) Uani 1.000000 . .
H56 H 0.2988(14) 0.7364(13) 0.9042(11) 0.110(6) Uiso 1.000000 R .
C57 C 0.3898(16) 0.8541(15) 0.9032(12) 0.115(7) Uani 1.000000 . .
H57 H 0.3893(16) 0.8845(15) 0.9535(12) 0.138(9) Uiso 1.000000 R .
C58 C 0.4459(18) 0.9001(13) 0.8625(15) 0.122(8) Uani 1.000000 . .
H58 H 0.4851(18) 0.9609(13) 0.8847(15) 0.147(9) Uiso 1.000000 R .
C60 C 0.8462(10) 0.6140(10) 0.7660(9) 0.137(6) Uani 1.000000 . U
H60 H 0.8969(10) 0.6688(10) 0.7745(9) 0.165(7) Uiso 1.000000 R .
C59 C 0.7669(13) 0.6124(9) 0.7889(7) 0.128(6) Uani 1.000000 G U
H59 H 0.7634(13) 0.6660(9) 0.8131(7) 0.154(7) Uiso 1.000000 R .
C64 C 0.6926(9) 0.5323(13) 0.7764(7) 0.119(5) Uani 1.000000 G U
H64 H 0.6384(9) 0.5312(13) 0.7920(7) 0.142(6) Uiso 1.000000 R .
C63 C 0.6977(9) 0.4539(9) 0.7410(8) 0.112(5) Uani 1.000000 G U
H63 H 0.6469(9) 0.3991(9) 0.7324(8) 0.135(6) Uiso 1.000000 R .
C62 C 0.7770(12) 0.4555(10) 0.7181(7) 0.121(6) Uani 1.000000 G U
H62 H 0.7805(12) 0.4019(10) 0.6939(7) 0.145(7) Uiso 1.000000 R .
C61 C 0.8513(9) 0.5356(13) 0.7306(8) 0.127(6) Uani 1.000000 G U
H61 H 0.9055(9) 0.5367(13) 0.7149(8) 0.153(7) Uiso 1.000000 R .


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
Ag1 Ge1 2.4041(11) . ?
Ag1 N10 2.175(7) . ?
Ag2 Ge2 2.4020(12) . ?
Ag2 N5 2.169(7) . ?
Ge1 N1 2.029(8) . ?
Ge1 N3 1.919(8) . ?
Ge1 N11 1.839(9) . ?
Ge2 N6 2.028(8) . ?
Ge2 N8 1.910(8) . ?
Ge2 N12 1.837(9) . ?
S1 O1 1.429(9) . ?
S1 O2 1.428(8) . ?
S1 N13 1.567(9) . ?
S1 C49 1.813(12) . ?
S2 O3 1.436(8) . ?
S2 O4 1.408(9) . ?
S2 N13 1.560(9) . ?
S2 C50 1.814(14) . ?
Si1 N11 1.762(9) . ?
Si1 C19 1.841(13) . ?
Si1 C20 1.908(14) . ?
Si1 C21 1.847(14) . ?
Si2 N11 1.766(9) . ?
Si2 C22 1.907(15) . ?
Si2 C23 1.859(13) . ?
Si2 C24 1.867(12) . ?
Si3 N12 1.770(9) . ?
Si3 C46 1.855(15) . ?
Si3 C47 1.865(12) . ?
Si3 C48 1.859(12) . ?
Si4 N12 1.755(9) . ?
Si4 C43 1.864(15) . ?
Si4 C44 1.838(15) . ?
Si4 C45 1.862(13) . ?
F1 C49 1.297(14) . ?
F2 C49 1.286(15) . ?
F3 C49 1.299(16) . ?
F4 C50 1.318(14) . ?
F5 C50 1.332(18) . ?
F6 C50 1.309(18) . ?
N1 C1 1.355(12) . ?
N1 C5 1.353(12) . ?
N2 C5 1.388(12) . ?
N2 C6 1.278(12) . ?
N3 C6 1.376(11) . ?
N3 C13 1.397(12) . ?
N4 C13 1.280(12) . ?
N4 C14 1.407(12) . ?
N5 C14 1.336(11) . ?
N5 C18 1.326(13) . ?
N6 C25 1.367(13) . ?
N6 C29 1.350(13) . ?
N7 C29 1.387(13) . ?
N7 C30 1.286(12) . ?
N8 C30 1.379(12) . ?
N8 C37 1.399(12) . ?
N9 C37 1.292(12) . ?
N9 C38 1.408(12) . ?
N10 C38 1.323(11) . ?
N10 C42 1.327(12) . ?
C1 H1 0.9500 . ?
C1 C2 1.360(15) . ?
C2 H2 0.9500 . ?
C2 C3 1.380(15) . ?
C3 H3 0.9500 . ?
C3 C4 1.394(15) . ?
C4 H4 0.9500 . ?
C4 C5 1.412(14) . ?
C6 C7 1.469(13) . ?
C7 C8 1.391(13) . ?
C7 C12 1.387(14) . ?
C8 H8 0.9500 . ?
C8 C9 1.397(15) . ?
C9 H9 0.9500 . ?
C9 C10 1.355(16) . ?
C10 H10 0.9500 . ?
C10 C11 1.412(14) . ?
C11 H11 0.9500 . ?
C11 C12 1.389(13) . ?
C12 C13 1.481(13) . ?
C14 C15 1.384(13) . ?
C15 H15 0.9500 . ?
C15 C16 1.348(16) . ?
C16 H16 0.9500 . ?
C16 C17 1.389(16) . ?
C17 H17 0.9500 . ?
C17 C18 1.378(15) . ?
C18 H18 0.9500 . ?
C19 H19a 0.9800 . ?
C19 H19b 0.9800 . ?
C19 H19c 0.9800 . ?
C20 H20a 0.9800 . ?
C20 H20b 0.9800 . ?
C20 H20c 0.9800 . ?
C21 H21a 0.9800 . ?
C21 H21b 0.9800 . ?
C21 H21c 0.9800 . ?
C22 H22a 0.9800 . ?
C22 H22b 0.9800 . ?
C22 H22c 0.9800 . ?
C23 H23a 0.9800 . ?
C23 H23b 0.9800 . ?
C23 H23c 0.9800 . ?
C24 H24a 0.9800 . ?
C24 H24b 0.9800 . ?
C24 H24c 0.9800 . ?
C25 H25 0.9500 . ?
C25 C26 1.383(15) . ?
C26 H26 0.9500 . ?
C26 C27 1.376(17) . ?
C27 H27 0.9500 . ?
C27 C28 1.365(16) . ?
C28 H28 0.9500 . ?
C28 C29 1.405(14) . ?
C30 C31 1.471(13) . ?
C31 C32 1.384(14) . ?
C31 C36 1.398(13) . ?
C32 H32 0.9500 . ?
C32 C33 1.378(15) . ?
C33 H33 0.9500 . ?
C33 C34 1.392(17) . ?
C34 H34 0.9500 . ?
C34 C35 1.394(16) . ?
C35 H35 0.9500 . ?
C35 C36 1.400(14) . ?
C36 C37 1.470(13) . ?
C38 C39 1.373(13) . ?
C39 H39 0.9500 . ?
C39 C40 1.376(16) . ?
C40 H40 0.9500 . ?
C40 C41 1.342(16) . ?
C41 H41 0.9500 . ?
C41 C42 1.367(15) . ?
C42 H42 0.9500 . ?
C43 H43a 0.9800 . ?
C43 H43b 0.9800 . ?
C43 H43c 0.9800 . ?
C44 H44a 0.9800 . ?
C44 H44b 0.9800 . ?
C44 H44c 0.9800 . ?
C45 H45a 0.9800 . ?
C45 H45b 0.9800 . ?
C45 H45c 0.9800 . ?
C46 H46a 0.9800 . ?
C46 H46b 0.9800 . ?
C46 H46c 0.9800 . ?
C47 H47a 0.9800 . ?
C47 H47b 0.9800 . ?
C47 H47c 0.9800 . ?
C48 H48a 0.9800 . ?
C48 H48b 0.9800 . ?
C48 H48c 0.9800 . ?
S3 O5 1.428(11) . ?
S3 O6 1.393(12) . ?
S3 N14 1.561(13) . ?
S3 C51 1.777(15) . ?
S4 O7 1.409(10) . ?
S4 O8 1.435(10) . ?
S4 N14 1.594(12) . ?
S4 C52 1.819(16) . ?
F7 C51 1.33(2) . ?
F8 C51 1.340(16) . ?
F9 C51 1.307(19) . ?
F10 C52 1.322(19) . ?
F11 C52 1.33(2) . ?
F12 C52 1.267(18) . ?
C53 H53 0.9500 . ?
C53 C54 1.34(3) . ?
C53 C58 1.39(3) . ?
C54 H54 0.9500 . ?
C54 C55 1.31(2) . ?
C55 H55 0.9500 . ?
C55 C56 1.39(2) . ?
C56 H56 0.9500 . ?
C56 C57 1.34(3) . ?
C57 H57 0.9500 . ?
C57 C58 1.37(3) . ?
C58 H58 0.9500 . ?
C60 H60 0.9500 . ?
C60 C59 1.3900 . ?
C60 C61 1.3900 . ?
C59 H59 0.9500 . ?
C59 C64 1.3900 . ?
C64 H64 0.9500 . ?
C64 C63 1.3900 . ?
C63 H63 0.9500 . ?
C63 C62 1.3900 . ?
C62 H62 0.9500 . ?
C62 C61 1.3900 . ?
C61 H61 0.9500 . ?

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
N10 Ag1 Ge1 177.9(2) . . ?
N5 Ag2 Ge2 177.5(2) . . ?
N1 Ge1 Ag1 106.7(2) . . ?
N3 Ge1 Ag1 115.2(2) . . ?
N3 Ge1 N1 88.4(3) . . ?
N11 Ge1 Ag1 128.2(3) . . ?
N11 Ge1 N1 101.7(4) . . ?
N11 Ge1 N3 108.0(3) . . ?
N6 Ge2 Ag2 105.9(2) . . ?
N8 Ge2 Ag2 115.2(3) . . ?
N8 Ge2 N6 87.6(3) . . ?
N12 Ge2 Ag2 129.1(3) . . ?
N12 Ge2 N6 101.8(3) . . ?
N12 Ge2 N8 107.7(4) . . ?
O2 S1 O1 118.6(6) . . ?
N13 S1 O1 115.7(5) . . ?
N13 S1 O2 108.9(5) . . ?
C49 S1 O1 103.5(6) . . ?
C49 S1 O2 104.3(6) . . ?
C49 S1 N13 104.1(5) . . ?
O4 S2 O3 118.3(6) . . ?
N13 S2 O3 116.0(5) . . ?
N13 S2 O4 109.8(6) . . ?
C50 S2 O3 102.1(7) . . ?
C50 S2 O4 105.1(7) . . ?
C50 S2 N13 103.3(6) . . ?
C19 Si1 N11 112.2(5) . . ?
C20 Si1 N11 111.4(6) . . ?
C20 Si1 C19 106.8(7) . . ?
C21 Si1 N11 110.5(5) . . ?
C21 Si1 C19 107.5(7) . . ?
C21 Si1 C20 108.3(7) . . ?
C22 Si2 N11 113.4(5) . . ?
C23 Si2 N11 111.0(6) . . ?
C23 Si2 C22 105.4(7) . . ?
C24 Si2 N11 110.8(5) . . ?
C24 Si2 C22 105.4(7) . . ?
C24 Si2 C23 110.7(7) . . ?
C46 Si3 N12 112.8(5) . . ?
C47 Si3 N12 111.0(6) . . ?
C47 Si3 C46 109.5(7) . . ?
C48 Si3 N12 112.1(5) . . ?
C48 Si3 C46 107.0(7) . . ?
C48 Si3 C47 104.0(6) . . ?
C43 Si4 N12 111.9(5) . . ?
C44 Si4 N12 110.4(6) . . ?
C44 Si4 C43 106.7(8) . . ?
C45 Si4 N12 111.4(6) . . ?
C45 Si4 C43 105.3(8) . . ?
C45 Si4 C44 110.9(8) . . ?
C1 N1 Ge1 113.1(6) . . ?
C5 N1 Ge1 126.6(6) . . ?
C5 N1 C1 120.2(8) . . ?
C6 N2 C5 122.1(8) . . ?
C6 N3 Ge1 124.9(6) . . ?
C13 N3 Ge1 120.8(6) . . ?
C13 N3 C6 111.5(7) . . ?
C14 N4 C13 123.2(8) . . ?
C14 N5 Ag2 121.5(6) . . ?
C18 N5 Ag2 118.5(7) . . ?
C18 N5 C14 119.7(8) . . ?
C25 N6 Ge2 112.8(7) . . ?
C29 N6 Ge2 127.2(7) . . ?
C29 N6 C25 120.0(9) . . ?
C30 N7 C29 122.5(9) . . ?
C30 N8 Ge2 126.2(6) . . ?
C37 N8 Ge2 119.6(6) . . ?
C37 N8 C30 110.7(8) . . ?
C38 N9 C37 123.3(9) . . ?
C38 N10 Ag1 122.9(6) . . ?
C42 N10 Ag1 117.3(6) . . ?
C42 N10 C38 119.6(8) . . ?
Si1 N11 Ge1 123.7(5) . . ?
Si2 N11 Ge1 116.9(5) . . ?
Si2 N11 Si1 119.3(5) . . ?
Si3 N12 Ge2 121.7(5) . . ?
Si4 N12 Ge2 117.7(5) . . ?
Si4 N12 Si3 119.4(5) . . ?
S2 N13 S1 125.2(6) . . ?
H1 C1 N1 118.7(6) . . ?
C2 C1 N1 122.7(10) . . ?
C2 C1 H1 118.7(6) . . ?
H2 C2 C1 120.4(6) . . ?
C3 C2 C1 119.2(10) . . ?
C3 C2 H2 120.4(6) . . ?
H3 C3 C2 120.6(6) . . ?
C4 C3 C2 118.9(10) . . ?
C4 C3 H3 120.6(6) . . ?
H4 C4 C3 119.9(6) . . ?
C5 C4 C3 120.1(10) . . ?
C5 C4 H4 119.9(6) . . ?
N2 C5 N1 124.4(8) . . ?
C4 C5 N1 118.9(9) . . ?
C4 C5 N2 116.7(9) . . ?
N3 C6 N2 130.7(9) . . ?
C7 C6 N2 123.0(8) . . ?
C7 C6 N3 106.3(8) . . ?
C8 C7 C6 129.3(9) . . ?
C12 C7 C6 109.0(8) . . ?
C12 C7 C8 121.7(9) . . ?
H8 C8 C7 121.6(6) . . ?
C9 C8 C7 116.8(10) . . ?
C9 C8 H8 121.6(6) . . ?
H9 C9 C8 118.8(6) . . ?
C10 C9 C8 122.4(10) . . ?
C10 C9 H9 118.8(6) . . ?
H10 C10 C9 119.6(6) . . ?
C11 C10 C9 120.8(10) . . ?
C11 C10 H10 119.6(6) . . ?
H11 C11 C10 121.2(6) . . ?
C12 C11 C10 117.5(10) . . ?
C12 C11 H11 121.2(6) . . ?
C11 C12 C7 120.7(9) . . ?
C13 C12 C7 106.7(8) . . ?
C13 C12 C11 132.6(9) . . ?
N4 C13 N3 117.6(8) . . ?
C12 C13 N3 106.5(8) . . ?
C12 C13 N4 135.8(9) . . ?
N5 C14 N4 119.5(8) . . ?
C15 C14 N4 119.9(8) . . ?
C15 C14 N5 120.4(9) . . ?
H15 C15 C14 120.0(6) . . ?
C16 C15 C14 120.0(10) . . ?
C16 C15 H15 120.0(7) . . ?
H16 C16 C15 120.2(7) . . ?
C17 C16 C15 119.7(10) . . ?
C17 C16 H16 120.2(6) . . ?
H17 C17 C16 121.2(6) . . ?
C18 C17 C16 117.6(10) . . ?
C18 C17 H17 121.2(7) . . ?
C17 C18 N5 122.5(10) . . ?
H18 C18 N5 118.7(6) . . ?
H18 C18 C17 118.7(7) . . ?
H19a C19 Si1 109.5 . . ?
H19b C19 Si1 109.5 . . ?
H19b C19 H19a 109.5 . . ?
H19c C19 Si1 109.5 . . ?
H19c C19 H19a 109.5 . . ?
H19c C19 H19b 109.5 . . ?
H20a C20 Si1 109.5 . . ?
H20b C20 Si1 109.5 . . ?
H20b C20 H20a 109.5 . . ?
H20c C20 Si1 109.5 . . ?
H20c C20 H20a 109.5 . . ?
H20c C20 H20b 109.5 . . ?
H21a C21 Si1 109.5 . . ?
H21b C21 Si1 109.5 . . ?
H21b C21 H21a 109.5 . . ?
H21c C21 Si1 109.5 . . ?
H21c C21 H21a 109.5 . . ?
H21c C21 H21b 109.5 . . ?
H22a C22 Si2 109.5 . . ?
H22b C22 Si2 109.5 . . ?
H22b C22 H22a 109.5 . . ?
H22c C22 Si2 109.5 . . ?
H22c C22 H22a 109.5 . . ?
H22c C22 H22b 109.5 . . ?
H23a C23 Si2 109.5 . . ?
H23b C23 Si2 109.5 . . ?
H23b C23 H23a 109.5 . . ?
H23c C23 Si2 109.5 . . ?
H23c C23 H23a 109.5 . . ?
H23c C23 H23b 109.5 . . ?
H24a C24 Si2 109.5 . . ?
H24b C24 Si2 109.5 . . ?
H24b C24 H24a 109.5 . . ?
H24c C24 Si2 109.5 . . ?
H24c C24 H24a 109.5 . . ?
H24c C24 H24b 109.5 . . ?
H25 C25 N6 119.3(6) . . ?
C26 C25 N6 121.5(10) . . ?
C26 C25 H25 119.3(7) . . ?
H26 C26 C25 120.4(7) . . ?
C27 C26 C25 119.3(11) . . ?
C27 C26 H26 120.4(7) . . ?
H27 C27 C26 120.6(7) . . ?
C28 C27 C26 118.7(11) . . ?
C28 C27 H27 120.6(7) . . ?
H28 C28 C27 119.2(7) . . ?
C29 C28 C27 121.6(11) . . ?
C29 C28 H28 119.2(6) . . ?
N7 C29 N6 124.1(9) . . ?
C28 C29 N6 118.7(9) . . ?
C28 C29 N7 117.2(9) . . ?
N8 C30 N7 129.0(9) . . ?
C31 C30 N7 124.2(8) . . ?
C31 C30 N8 106.7(8) . . ?
C32 C31 C30 129.6(9) . . ?
C36 C31 C30 108.6(8) . . ?
C36 C31 C32 121.8(9) . . ?
H32 C32 C31 121.0(6) . . ?
C33 C32 C31 117.9(11) . . ?
C33 C32 H32 121.0(7) . . ?
H33 C33 C32 118.8(7) . . ?
C34 C33 C32 122.4(10) . . ?
C34 C33 H33 118.8(7) . . ?
H34 C34 C33 120.5(7) . . ?
C35 C34 C33 119.0(10) . . ?
C35 C34 H34 120.5(7) . . ?
H35 C35 C34 120.1(7) . . ?
C36 C35 C34 119.9(10) . . ?
C36 C35 H35 120.1(6) . . ?
C35 C36 C31 119.0(9) . . ?
C37 C36 C31 106.5(8) . . ?
C37 C36 C35 134.5(9) . . ?
N9 C37 N8 116.1(8) . . ?
C36 C37 N8 107.4(8) . . ?
C36 C37 N9 136.5(9) . . ?
N10 C38 N9 120.5(8) . . ?
C39 C38 N9 118.7(9) . . ?
C39 C38 N10 120.6(9) . . ?
H39 C39 C38 120.1(6) . . ?
C40 C39 C38 119.9(10) . . ?
C40 C39 H39 120.1(7) . . ?
H40 C40 C39 120.9(7) . . ?
C41 C40 C39 118.2(10) . . ?
C41 C40 H40 120.9(7) . . ?
H41 C41 C40 119.9(7) . . ?
C42 C41 C40 120.1(10) . . ?
C42 C41 H41 119.9(7) . . ?
C41 C42 N10 121.4(10) . . ?
H42 C42 N10 119.3(6) . . ?
H42 C42 C41 119.3(7) . . ?
H43a C43 Si4 109.5 . . ?
H43b C43 Si4 109.5 . . ?
H43b C43 H43a 109.5 . . ?
H43c C43 Si4 109.5 . . ?
H43c C43 H43a 109.5 . . ?
H43c C43 H43b 109.5 . . ?
H44a C44 Si4 109.5 . . ?
H44b C44 Si4 109.5 . . ?
H44b C44 H44a 109.5 . . ?
H44c C44 Si4 109.5 . . ?
H44c C44 H44a 109.5 . . ?
H44c C44 H44b 109.5 . . ?
H45a C45 Si4 109.5 . . ?
H45b C45 Si4 109.5 . . ?
H45b C45 H45a 109.5 . . ?
H45c C45 Si4 109.5 . . ?
H45c C45 H45a 109.5 . . ?
H45c C45 H45b 109.5 . . ?
H46a C46 Si3 109.5 . . ?
H46b C46 Si3 109.5 . . ?
H46b C46 H46a 109.5 . . ?
H46c C46 Si3 109.5 . . ?
H46c C46 H46a 109.5 . . ?
H46c C46 H46b 109.5 . . ?
H47a C47 Si3 109.5 . . ?
H47b C47 Si3 109.5 . . ?
H47b C47 H47a 109.5 . . ?
H47c C47 Si3 109.5 . . ?
H47c C47 H47a 109.5 . . ?
H47c C47 H47b 109.5 . . ?
H48a C48 Si3 109.5 . . ?
H48b C48 Si3 109.5 . . ?
H48b C48 H48a 109.5 . . ?
H48c C48 Si3 109.5 . . ?
H48c C48 H48a 109.5 . . ?
H48c C48 H48b 109.5 . . ?
F1 C49 S1 110.6(9) . . ?
F2 C49 S1 112.4(9) . . ?
F2 C49 F1 108.4(12) . . ?
F3 C49 S1 113.3(9) . . ?
F3 C49 F1 106.9(12) . . ?
F3 C49 F2 104.9(12) . . ?
F4 C50 S2 111.7(11) . . ?
F5 C50 S2 109.1(11) . . ?
F5 C50 F4 106.1(11) . . ?
F6 C50 S2 112.4(9) . . ?
F6 C50 F4 108.1(14) . . ?
F6 C50 F5 109.2(13) . . ?
O6 S3 O5 118.5(10) . . ?
N14 S3 O5 114.0(7) . . ?
N14 S3 O6 111.1(9) . . ?
C51 S3 O5 103.0(8) . . ?
C51 S3 O6 105.7(9) . . ?
C51 S3 N14 102.4(7) . . ?
O8 S4 O7 117.1(7) . . ?
N14 S4 O7 120.2(7) . . ?
N14 S4 O8 107.1(6) . . ?
C52 S4 O7 104.3(8) . . ?
C52 S4 O8 102.6(7) . . ?
C52 S4 N14 102.9(7) . . ?
S4 N14 S3 125.1(7) . . ?
F7 C51 S3 111.1(10) . . ?
F8 C51 S3 110.6(11) . . ?
F8 C51 F7 106.5(15) . . ?
F9 C51 S3 112.5(14) . . ?
F9 C51 F7 109.6(16) . . ?
F9 C51 F8 106.2(14) . . ?
F10 C52 S4 109.0(12) . . ?
F11 C52 S4 109.8(11) . . ?
F11 C52 F10 106.9(15) . . ?
F12 C52 S4 112.7(12) . . ?
F12 C52 F10 111.5(15) . . ?
F12 C52 F11 106.9(16) . . ?
C54 C53 H53 120.3(12) . . ?
C58 C53 H53 120.3(13) . . ?
C58 C53 C54 119.4(18) . . ?
H54 C54 C53 119.4(12) . . ?
C55 C54 C53 121.3(18) . . ?
C55 C54 H54 119.4(11) . . ?
H55 C55 C54 119.1(11) . . ?
C56 C55 C54 121.9(16) . . ?
C56 C55 H55 119.1(11) . . ?
H56 C56 C55 121.5(11) . . ?
C57 C56 C55 116.9(16) . . ?
C57 C56 H56 121.5(11) . . ?
H57 C57 C56 118.8(11) . . ?
C58 C57 C56 122.3(19) . . ?
C58 C57 H57 118.8(13) . . ?
C57 C58 C53 118(2) . . ?
H58 C58 C53 120.9(13) . . ?
H58 C58 C57 120.9(13) . . ?
C59 C60 H60 120.0 . . ?
C61 C60 H60 120.0 . . ?
C61 C60 C59 120.0 . . ?
H59 C59 C60 120.0(6) . . ?
C64 C59 C60 120.0 . . ?
C64 C59 H59 120.0(6) . . ?
H64 C64 C59 120.0(6) . . ?
C63 C64 C59 120.0 . . ?
C63 C64 H64 120.0(6) . . ?
H63 C63 C64 120.0(6) . . ?
C62 C63 C64 120.000000000(17) . . ?
C62 C63 H63 120.0(6) . . ?
H62 C62 C63 120.0(6) . . ?
C61 C62 C63 120.0 . . ?
C61 C62 H62 120.0(6) . . ?
C62 C61 C60 120.0 . . ?
H61 C61 C60 120.0(6) . . ?
H61 C61 C62 120.0(6) . . ?

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
Ag1 N10 C38 N9 -2.1(8) . . . . ?
Ag1 N10 C38 C39 -177.4(8) . . . . ?
Ag1 N10 C42 C41 179.5(8) . . . . ?
Ag2 N5 C14 N4 -9.7(7) . . . . ?
Ag2 N5 C14 C15 175.0(7) . . . . ?
Ag2 N5 C18 C17 -173.8(8) . . . . ?
Ge1 N1 C1 C2 178.6(8) . . . . ?
Ge1 N1 C5 N2 0.4(9) . . . . ?
Ge1 N1 C5 C4 -179.2(8) . . . . ?
Ge1 N3 C6 N2 -16.9(9) . . . . ?
Ge1 N3 C6 C7 162.1(7) . . . . ?
Ge1 N3 C13 N4 14.0(7) . . . . ?
Ge1 N3 C13 C12 -162.3(7) . . . . ?
Ge2 N6 C25 C26 -179.2(8) . . . . ?
Ge2 N6 C29 N7 0.3(9) . . . . ?
Ge2 N6 C29 C28 179.1(8) . . . . ?
Ge2 N8 C30 N7 -19.0(10) . . . . ?
Ge2 N8 C30 C31 161.1(8) . . . . ?
Ge2 N8 C37 N9 15.7(8) . . . . ?
Ge2 N8 C37 C36 -164.1(7) . . . . ?
S1 N13 S2 O3 16.6(9) . . . . ?
S1 N13 S2 O4 154.1(8) . . . . ?
S1 N13 S2 C50 -94.2(9) . . . . ?
N1 C1 C2 C3 1.3(13) . . . . ?
N1 C5 N2 C6 8.3(12) . . . . ?
N1 C5 C4 C3 0.5(11) . . . . ?
N2 C5 C4 C3 -179.1(9) . . . . ?
N2 C6 N3 C13 -178.0(10) . . . . ?
N2 C6 C7 C8 -0.7(12) . . . . ?
N2 C6 C7 C12 177.8(10) . . . . ?
N3 C6 C7 C8 -179.9(8) . . . . ?
N3 C6 C7 C12 -1.3(8) . . . . ?
N3 C13 N4 C14 177.4(7) . . . . ?
N3 C13 C12 C7 -0.4(8) . . . . ?
N3 C13 C12 C11 -179.3(7) . . . . ?
N4 C13 C12 C7 -175.8(12) . . . . ?
N4 C13 C12 C11 5.3(15) . . . . ?
N4 C14 N5 C18 176.4(8) . . . . ?
N4 C14 C15 C16 -177.8(10) . . . . ?
N5 C14 C15 C16 -2.5(11) . . . . ?
N5 C18 C17 C16 -0.3(13) . . . . ?
N6 C25 C26 C27 0.6(13) . . . . ?
N6 C29 N7 C30 8.2(12) . . . . ?
N6 C29 C28 C27 0.8(12) . . . . ?
N7 C29 C28 C27 179.6(10) . . . . ?
N7 C30 N8 C37 -177.4(11) . . . . ?
N7 C30 C31 C32 0.6(13) . . . . ?
N7 C30 C31 C36 179.9(10) . . . . ?
N8 C30 C31 C32 -179.5(8) . . . . ?
N8 C30 C31 C36 -0.3(8) . . . . ?
N8 C37 N9 C38 -177.7(8) . . . . ?
N8 C37 C36 C31 3.7(8) . . . . ?
N8 C37 C36 C35 -177.9(8) . . . . ?
N9 C37 C36 C31 -175.9(13) . . . . ?
N9 C37 C36 C35 2.4(16) . . . . ?
N9 C38 N10 C42 173.1(9) . . . . ?
N9 C38 C39 C40 -176.3(11) . . . . ?
N10 C38 C39 C40 -0.9(12) . . . . ?
N10 C42 C41 C40 -2.7(14) . . . . ?
C1 C2 C3 C4 -2.4(13) . . . . ?
C2 C3 C4 C5 1.5(14) . . . . ?
C6 C7 C8 C9 176.5(11) . . . . ?
C6 C7 C12 C11 -179.9(7) . . . . ?
C6 C7 C12 C13 1.1(8) . . . . ?
C7 C8 C9 C10 1.9(12) . . . . ?
C7 C12 C11 C10 4.1(11) . . . . ?
C8 C9 C10 C11 1.0(14) . . . . ?
C9 C10 C11 C12 -4.1(13) . . . . ?
C10 C11 C12 C13 -177.1(8) . . . . ?
C14 C15 C16 C17 2.5(12) . . . . ?
C15 C16 C17 C18 -1.1(13) . . . . ?
C25 C26 C27 C28 -4.0(14) . . . . ?
C26 C27 C28 C29 3.3(15) . . . . ?
C30 C31 C32 C33 -178.8(12) . . . . ?
C30 C31 C36 C35 179.3(8) . . . . ?
C30 C31 C36 C37 -2.1(8) . . . . ?
C31 C32 C33 C34 -1.1(13) . . . . ?
C31 C36 C35 C34 -0.2(11) . . . . ?
C32 C33 C34 C35 -0.4(13) . . . . ?
C33 C34 C35 C36 1.1(13) . . . . ?
C34 C35 C36 C37 -178.3(9) . . . . ?
C38 C39 C40 C41 2.2(14) . . . . ?
C39 C40 C41 C42 -0.4(15) . . . . ?
S3 N14 S4 O7 21.0(13) . . . . ?
S3 N14 S4 O8 158.0(10) . . . . ?
S3 N14 S4 C52 -94.2(11) . . . . ?
C53 C54 C55 C56 2(2) . . . . ?
C53 C58 C57 C56 2(3) . . . . ?
C54 C55 C56 C57 0(2) . . . . ?
C55 C56 C57 C58 -2(2) . . . . ?
C60 C59 C64 C63 0.0(10) . . . . ?
C60 C61 C62 C63 -0.0(10) . . . . ?
C59 C64 C63 C62 -0.0(10) . . . . ?
C64 C63 C62 C61 0.0(10) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
loop_
_restr_RIGU_atom_site_label_1
_restr_RIGU_atom_site_label_2
_restr_RIGU_target_weight_param
_restr_RIGU_U13_diff
_restr_RIGU_U23_diff
_restr_RIGU_U33_diff
C60 C59 0.004000 -0.008315 -0.001572 0.002849
C60 C64 0.004000 -0.013595 -0.002698 0.016979
C60 C62 0.004000 0.004986 -0.004329 0.016636
C60 C61 0.004000 0.005965 -0.006744 -0.001050
C59 C64 0.004000 -0.011078 0.000800 -0.003730
C59 C63 0.004000 -0.007926 -0.004355 0.005947
C59 C61 0.004000 -0.013921 -0.031505 0.001049
C64 C63 0.004000 -0.004195 0.003632 0.000406
C64 C62 0.004000 -0.004117 -0.011968 0.000332
C63 C62 0.004000 0.003080 0.003389 -0.001343
C63 C61 0.004000 0.003605 -0.001378 -0.005346
C62 C61 0.004000 0.013468 -0.001274 0.000994

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.743(2)
2 0.257(2)

