# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1059012'
_audit_update_record             
;
2015-04-11 deposited with the CCDC.
2016-01-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        PKU-15
_chemical_name_common            germanate
_chemical_melting_point          1000
_chemical_formula_moiety         'Ge14.27 O31 Si0.73, C6 H16 N, C6 H13 N'
_chemical_formula_sum            'C12 H32 Ge13.75 N2 O31 Si1.25'
_chemical_formula_weight         1733.62

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'
Si Si 0.0817 0.0704 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

_cell_length_a                   16.8108(5)
_cell_length_b                   19.7138(7)
_cell_length_c                   23.9394(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7933.6(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    100.00(10)
_cell_measurement_reflns_used    6177
_cell_measurement_theta_min      2.9326
_cell_measurement_theta_max      28.2923

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.903
_exptl_crystal_F_000             6588
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    10.393
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.77823
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.00(10)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 10.3914
_diffrn_reflns_number            21706
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.939
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             7987
_reflns_number_gt                6038
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0480P)²+84.7570P] 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         7987
_refine_ls_number_parameters     494
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_ref         0.1346
_refine_ls_wR_factor_gt          0.1222
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.104
_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 0.51802(5) 0.06230(4) 0.26921(4) 0.0080(2) Uani 1 1 d . . . . .
Ge2 Ge 0.51718(5) -0.07037(4) 0.21911(4) 0.0078(2) Uani 1 1 d . . . . .
Ge3 Ge 0.44325(5) 0.05984(4) 0.12795(4) 0.0098(2) Uani 1 1 d . . . . .
Ge4 Ge 0.34374(5) 0.06674(4) 0.01432(4) 0.0101(2) Uani 1 1 d . . . . .
Ge5 Ge 0.65860(5) 0.06946(5) 0.50183(4) 0.0133(2) Uani 1 1 d . . . . .
Ge6 Ge 0.57716(5) 0.03390(4) 0.39204(4) 0.0080(3) Uani 0.982(7) 1 d . . P . .
Si6 Si 0.57716(5) 0.03390(4) 0.39204(4) 0.0080(3) Uani 0.018(7) 1 d . . P . .
Ge7 Ge 0.55561(5) 0.16652(5) 0.18006(4) 0.0089(4) Uani 0.879(8) 1 d . . P . .
Si7 Si 0.55561(5) 0.16652(5) 0.18006(4) 0.0089(4) Uani 0.121(8) 1 d . . P . .
Ge8 Ge 0.53811(5) -0.16625(5) 0.31839(4) 0.0082(4) Uani 0.887(8) 1 d . . P . .
Si8 Si 0.53811(5) -0.16625(5) 0.31839(4) 0.0082(4) Uani 0.113(8) 1 d . . P . .
Ge9 Ge 0.74729(5) -0.06831(5) 0.49711(4) 0.0108(2) Uani 1 1 d . . . . .
Ge10 Ge 0.57011(6) 0.06452(5) 0.61424(5) 0.0119(4) Uani 0.845(7) 1 d . . P . .
Si10 Si 0.57011(6) 0.06452(5) 0.61424(5) 0.0119(4) Uani 0.155(7) 1 d . . P . .
Ge11 Ge 0.33613(5) -0.04241(4) 0.19637(4) 0.0080(3) Uani 0.973(7) 1 d . . P . .
Si11 Si 0.33613(5) -0.04241(4) 0.19637(4) 0.0080(3) Uani 0.027(7) 1 d . . P . .
Ge12 Ge 0.70260(5) 0.09643(5) 0.11913(4) 0.0087(4) Uani 0.910(8) 1 d . . P . .
Si12 Si 0.70260(5) 0.09643(5) 0.11913(4) 0.0087(4) Uani 0.090(8) 1 d . . P . .
Ge13 Ge 0.58798(5) -0.03392(4) 0.10355(4) 0.0081(2) Uani 1 1 d . . . . .
Ge14 Ge 0.33930(5) 0.04402(5) 0.30434(4) 0.0074(3) Uani 0.894(7) 1 d . . P . .
Si14 Si 0.33930(5) 0.04402(5) 0.30434(4) 0.0074(3) Uani 0.106(7) 1 d . . P . .
Ge15 Ge 0.69186(5) -0.09207(5) 0.37585(4) 0.0077(3) Uani 0.899(8) 1 d . . P . .
Si15 Si 0.69186(5) -0.09207(5) 0.37585(4) 0.0077(3) Uani 0.101(8) 1 d . . P . .
O1 O 0.5949(3) 0.0884(3) 0.4484(3) 0.0127(13) Uani 1 1 d . . . . .
O2 O 0.7609(3) -0.1209(3) 0.5539(3) 0.0122(13) Uani 1 1 d . . . . .
O3 O 0.6170(3) -0.1478(3) 0.3622(3) 0.0124(13) Uani 1 1 d . . . . .
O4 O 0.7274(3) -0.1194(3) 0.4401(2) 0.0103(12) Uani 1 1 d . . . . .
O5 O 0.6671(3) -0.0075(3) 0.3805(2) 0.0084(12) Uani 1 1 d . . . . .
O6 O 0.6102(3) -0.0876(3) 0.0484(2) 0.0127(8) Uani 1 1 d . . . . .
O7 O 0.2924(3) -0.0046(3) 0.2552(3) 0.0172(14) Uani 1 1 d . . . . .
O8 O 0.4668(3) 0.1422(3) 0.1524(3) 0.0127(8) Uani 1 1 d . . . . .
O9 O 0.3935(3) 0.1012(3) 0.0684(3) 0.0108(13) Uani 1 1 d . . . . .
O10 O 0.6739(3) 0.0128(3) 0.1176(3) 0.0103(13) Uani 1 1 d . . . . .
O11 O 0.7660(3) -0.1008(3) 0.3276(3) 0.0123(13) Uani 1 1 d . . . . .
O12 O 0.5465(4) 0.0862(3) 0.3403(3) 0.0127(8) Uani 1 1 d . . . . .
O13 O 0.6656(3) -0.0175(3) 0.5108(2) 0.0089(12) Uani 1 1 d . . . . .
O14 O 0.4164(3) 0.0878(3) 0.2751(3) 0.0124(13) Uani 1 1 d . . . . .
O15 O 0.6206(3) 0.1050(3) 0.5614(3) 0.0124(13) Uani 1 1 d . . . . .
O16 O 0.4154(3) -0.0931(3) 0.2142(3) 0.0121(13) Uani 1 1 d . . . . .
O17 O 0.2754(3) 0.1045(3) 0.3306(3) 0.0133(13) Uani 1 1 d . . . . .
O18 O 0.5715(4) -0.0893(3) 0.1572(3) 0.0144(13) Uani 1 1 d . . . . .
O19 O 0.4895(3) 0.0267(3) 0.5840(2) 0.0095(12) Uani 1 1 d . . . . .
O20 O 0.5205(6) -0.2500 0.3301(4) 0.022(2) Uani 1 2 d S T P . .
O21 O 0.6348(3) 0.0078(3) 0.6406(3) 0.0165(14) Uani 1 1 d . . . . .
O22 O 0.3545(3) 0.0166(3) 0.1456(3) 0.0133(13) Uani 1 1 d . . . . .
O23 O 0.8319(3) -0.0216(3) 0.4844(2) 0.0084(12) Uani 1 1 d . . . . .
O24 O 0.5432(4) -0.0252(3) 0.2801(3) 0.0164(14) Uani 1 1 d . . . . .
O25 O 0.5790(3) 0.1260(3) 0.2408(3) 0.0189(15) Uani 1 1 d . . . . .
O26 O 0.4983(3) 0.0224(3) 0.1933(3) 0.0127(13) Uani 1 1 d . . . . .
O27 O 0.5114(3) 0.0183(3) 0.0836(3) 0.0119(13) Uani 1 1 d . . . . .
O28 O 0.6301(3) 0.1551(3) 0.1309(3) 0.0127(13) Uani 1 1 d . . . . .
O29 O 0.5518(3) -0.1501(3) 0.2494(3) 0.0168(14) Uani 1 1 d . . . . .
O30 O 0.5522(5) 0.2500 0.1962(4) 0.022(2) Uani 1 2 d S T P . .
O31 O 0.2492(3) 0.1047(3) 0.0122(3) 0.0175(15) Uani 1 1 d . . . . .
O32 O 0.5487(3) 0.1310(3) 0.6570(3) 0.0142(13) Uani 1 1 d . . . . .
N1 N 0.4609(8) 0.2500 0.4780(7) 0.051(4) Uani 1 2 d DS T P . .
C11 C 0.4952(13) 0.2500 0.4190(7) 0.081(7) Uiso 1 2 d DS . P . .
H11A H 0.5279 0.2900 0.4132 0.097 Uiso 0.5 1 calc R U P . .
H11B H 0.5279 0.2100 0.4132 0.097 Uiso 0.5 1 calc R U P . .
C12 C 0.5313(12) 0.2500 0.5182(9) 0.081(8) Uiso 1 2 d DS . P . .
H12A H 0.5764 0.2705 0.5003 0.121 Uiso 0.5 1 calc R U P . .
H12B H 0.5440 0.2042 0.5284 0.121 Uiso 0.5 1 calc R U P . .
H12C H 0.5177 0.2753 0.5511 0.121 Uiso 0.5 1 calc R U P . .
C13 C 0.4138(11) 0.1867(5) 0.4866(11) 0.162(12) Uiso 1 1 d D . . . .
H13A H 0.3599 0.1983 0.4956 0.243 Uiso 1 1 calc R U . . .
H13B H 0.4367 0.1610 0.5166 0.243 Uiso 1 1 calc R U . . .
H13C H 0.4147 0.1601 0.4530 0.243 Uiso 1 1 calc R U . . .
C14 C 0.4251(16) 0.2500 0.3788(13) 0.162(17) Uiso 1 2 d DS . P . .
H14A H 0.3925 0.2899 0.3850 0.195 Uiso 0.5 1 calc R U P . .
H14B H 0.3925 0.2101 0.3850 0.195 Uiso 0.5 1 calc R U P . .
C15 C 0.458(2) 0.2500 0.3188(10) 0.140(14) Uiso 1 2 d DS . P . .
H15A H 0.4898 0.2897 0.3131 0.211 Uiso 0.5 1 calc R U P . .
H15B H 0.4142 0.2502 0.2928 0.211 Uiso 1 2 calc R U P . .
H15C H 0.4895 0.2102 0.3130 0.211 Uiso 0.5 1 calc R U P . .
N2 N 0.5375(10) 0.2500 -0.0228(7) 0.055(4) Uani 1 2 d DS T P . .
C21 C 0.5033(18) 0.2500 -0.0830(10) 0.22(2) Uiso 1 2 d DS . P . .
H21A H 0.4712 0.2901 -0.0897 0.263 Uiso 0.5 1 calc R U P . .
H21B H 0.4712 0.2099 -0.0897 0.263 Uiso 0.5 1 calc R U P . .
C22 C 0.471(2) 0.2500 0.0196(14) 0.25(3) Uiso 1 2 d DS . P . .
H22A H 0.4931 0.2556 0.0563 0.372 Uiso 0.5 1 calc R U P . .
H22B H 0.4430 0.2077 0.0177 0.372 Uiso 0.5 1 calc R U P . .
H22C H 0.4353 0.2867 0.0117 0.372 Uiso 0.5 1 calc R U P . .
C23 C 0.5843(14) 0.1862(5) -0.0170(13) 0.203(16) Uiso 1 1 d D . . . .
H23A H 0.5811 0.1607 -0.0511 0.304 Uiso 1 1 calc R U . . .
H23B H 0.5631 0.1597 0.0132 0.304 Uiso 1 1 calc R U . . .
H23C H 0.6389 0.1971 -0.0093 0.304 Uiso 1 1 calc R U . . .
C24 C 0.580(2) 0.2500 -0.1207(12) 0.27(3) Uiso 1 2 d DS . P . .
H24A H 0.6123 0.2899 -0.1128 0.329 Uiso 0.5 1 calc R U P . .
H24B H 0.6123 0.2101 -0.1128 0.329 Uiso 0.5 1 calc R U P . .
C25 C 0.555(4) 0.2500 -0.1817(12) 0.51(8) Uiso 1 2 d DS . P . .
H25A H 0.5864 0.2826 -0.2019 0.765 Uiso 0.5 1 calc R U P . .
H25B H 0.5000 0.2617 -0.1843 0.765 Uiso 0.5 1 calc R U P . .
H25C H 0.5636 0.2057 -0.1973 0.765 Uiso 0.5 1 calc R U P . .
N3 N 0.2611(8) 0.2500 0.1689(7) 0.065(5) Uani 1 2 d DS T P . .
C31 C 0.3131(16) 0.2500 0.1175(9) 0.195(9) Uiso 1 2 d DS . P . .
H31A H 0.3470 0.2102 0.1178 0.234 Uiso 0.5 1 calc R U P . .
H31B H 0.3470 0.2898 0.1178 0.234 Uiso 0.5 1 calc R U P . .
C32 C 0.3156(19) 0.2500 0.2206(11) 0.195(9) Uiso 1 2 d DS . P . .
H32A H 0.2836 0.2490 0.2538 0.292 Uiso 1 2 calc R U P . .
H32B H 0.3477 0.2902 0.2206 0.292 Uiso 0.5 1 calc R U P . .
H32C H 0.3493 0.2107 0.2197 0.292 Uiso 0.5 1 calc R U P . .
C33 C 0.2113(13) 0.1863(5) 0.1702(13) 0.195(9) Uiso 1 1 d D . . . .
H33A H 0.1700 0.1911 0.1976 0.292 Uiso 1 1 calc R U . . .
H33B H 0.2444 0.1483 0.1798 0.292 Uiso 1 1 calc R U . . .
H33C H 0.1880 0.1790 0.1341 0.292 Uiso 1 1 calc R U . . .
C34 C 0.263(2) 0.2500 0.0644(10) 0.195(9) Uiso 1 2 d DS . P . .
H34A H 0.2291 0.2899 0.0633 0.234 Uiso 0.5 1 calc R U P . .
H34B H 0.2291 0.2101 0.0633 0.234 Uiso 0.5 1 calc R U P . .
C35 C 0.322(3) 0.2500 0.0132(11) 0.195(9) Uiso 1 2 d DS . P . .
N4 N 0.7467(10) 0.2500 0.6848(11) 0.098(9) Uani 1 2 d DS T P . .
C41 C 0.698(3) 0.2500 0.6313(15) 0.320(17) Uiso 1 2 d DS . P . .
H41A H 0.6647 0.2900 0.6292 0.384 Uiso 0.5 1 calc R U P . .
H41B H 0.6647 0.2100 0.6292 0.384 Uiso 0.5 1 calc R U P . .
C42 C 0.687(3) 0.2500 0.7339(17) 0.320(17) Uiso 1 2 d DS . P . .
H42A H 0.7151 0.2496 0.7687 0.480 Uiso 1 2 calc R U P . .
H42B H 0.6535 0.2104 0.7316 0.480 Uiso 0.5 1 calc R U P . .
H42C H 0.6541 0.2899 0.7319 0.480 Uiso 0.5 1 calc R U P . .
C43 C 0.7952(16) 0.1865(5) 0.6880(19) 0.320(17) Uiso 1 1 d D . . . .
H43A H 0.8498 0.1980 0.6950 0.480 Uiso 1 1 calc R U . . .
H43B H 0.7913 0.1623 0.6533 0.480 Uiso 1 1 calc R U . . .
H43C H 0.7757 0.1585 0.7178 0.480 Uiso 1 1 calc R U . . .
C44 C 0.760(3) 0.2500 0.584(3) 0.320(17) Uiso 1 2 d DS . P . .
H44A H 0.7937 0.2101 0.5871 0.384 Uiso 0.5 1 calc R U P . .
H44B H 0.7937 0.2899 0.5871 0.384 Uiso 0.5 1 calc R U P . .
C45 C 0.715(4) 0.2500 0.5280(19) 0.320(17) Uiso 1 2 d DS . P . .


_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 O25 1.758(6) . ?
Ge1 O14 1.786(5) . ?
Ge1 O24 1.796(6) . ?
Ge1 O12 1.831(6) . ?
Ge1 O26 2.007(6) . ?
Ge1 Ge2 2.8772(13) . ?
Ge2 O24 1.765(6) . ?
Ge2 O16 1.773(5) . ?
Ge2 O18 1.781(6) . ?
Ge2 O29 1.827(6) . ?
Ge2 O26 1.957(6) . ?
Ge3 O27 1.764(6) . ?
Ge3 O22 1.768(6) . ?
Ge3 O8 1.770(6) . ?
Ge3 O9 1.842(6) . ?
Ge3 O26 1.962(6) . ?
Ge4 O9 1.685(6) . ?
Ge4 O6 1.739(6) 5_655 ?
Ge4 O23 1.754(5) 6_556 ?
Ge4 O31 1.757(6) . ?
Ge5 O31 1.708(6) 6_656 ?
Ge5 O1 1.709(6) . ?
Ge5 O15 1.713(6) . ?
Ge5 O13 1.732(5) . ?
Ge6 O12 1.691(6) . ?
Ge6 O19 1.736(5) 5_656 ?
Ge6 O5 1.740(5) . ?
Ge6 O1 1.750(6) . ?
Ge7 O30 1.691(3) . ?
Ge7 O8 1.702(6) . ?
Ge7 O25 1.706(6) . ?
Ge7 O28 1.733(6) . ?
Ge8 O29 1.697(6) . ?
Ge8 O20 1.701(3) . ?
Ge8 O32 1.720(6) 5_656 ?
Ge8 O3 1.728(6) . ?
Ge9 O23 1.721(5) . ?
Ge9 O2 1.724(6) . ?
Ge9 O4 1.729(6) . ?
Ge9 O13 1.730(5) . ?
Ge10 O21 1.682(6) . ?
Ge10 O32 1.702(6) . ?
Ge10 O19 1.707(5) . ?
Ge10 O15 1.720(6) . ?
Ge11 O22 1.712(6) . ?
Ge11 O16 1.720(5) . ?
Ge11 O11 1.744(6) 6_556 ?
Ge11 O7 1.756(6) . ?
Ge12 O28 1.704(5) . ?
Ge12 O10 1.719(6) . ?
Ge12 O17 1.723(6) 6_656 ?
Ge12 O2 1.746(6) 2_654 ?
Ge13 O18 1.708(6) . ?
Ge13 O27 1.717(5) . ?
Ge13 O6 1.733(6) . ?
Ge13 O10 1.745(5) . ?
Ge14 O14 1.707(6) . ?
Ge14 O7 1.709(6) . ?
Ge14 O21 1.724(6) 5_656 ?
Ge14 O17 1.724(6) . ?
Ge15 O3 1.703(5) . ?
Ge15 O11 1.709(6) . ?
Ge15 O5 1.722(5) . ?
Ge15 O4 1.735(6) . ?
O2 Si12 1.746(6) 2_655 ?
O2 Ge12 1.746(6) 2_655 ?
O6 Ge4 1.739(6) 5_655 ?
O11 Si11 1.744(6) 6_656 ?
O11 Ge11 1.744(6) 6_656 ?
O17 Si12 1.724(6) 6_556 ?
O17 Ge12 1.724(6) 6_556 ?
O19 Si6 1.736(5) 5_656 ?
O19 Ge6 1.736(5) 5_656 ?
O20 Si8 1.701(3) 7 ?
O20 Ge8 1.701(3) 7 ?
O21 Si14 1.724(6) 5_656 ?
O21 Ge14 1.724(6) 5_656 ?
O23 Ge4 1.754(5) 6_656 ?
O30 Si7 1.691(3) 7_565 ?
O30 Ge7 1.691(3) 7_565 ?
O31 Ge5 1.708(6) 6_556 ?
O32 Si8 1.719(6) 5_656 ?
O32 Ge8 1.719(6) 5_656 ?
N1 C13 1.491(11) . ?
N1 C13 1.491(11) 7_565 ?
N1 C12 1.525(15) . ?
N1 C11 1.525(15) . ?
C11 C14 1.522(18) . ?
C14 C15 1.538(19) . ?
N2 C23 1.490(12) 7_565 ?
N2 C23 1.490(12) . ?
N2 C22 1.507(17) . ?
N2 C21 1.551(17) . ?
C21 C24 1.581(19) . ?
C24 C25 1.52(2) . ?
N3 C33 1.509(11) . ?
N3 C33 1.509(11) 7_565 ?
N3 C31 1.510(16) . ?
N3 C32 1.539(16) . ?
C31 C34 1.526(19) . ?
C34 C35 1.574(19) . ?
N4 C43 1.496(13) 7_565 ?
N4 C43 1.496(13) . ?
N4 C41 1.517(18) . ?
N4 C42 1.551(18) . ?
C41 C44 1.53(2) . ?
C44 C45 1.55(2) . ?

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
O25 Ge1 O14 112.8(3) . . ?
O25 Ge1 O24 127.2(3) . . ?
O14 Ge1 O24 119.0(3) . . ?
O25 Ge1 O12 91.3(3) . . ?
O14 Ge1 O12 96.0(3) . . ?
O24 Ge1 O12 92.9(3) . . ?
O25 Ge1 O26 91.5(3) . . ?
O14 Ge1 O26 91.4(3) . . ?
O24 Ge1 O26 78.1(3) . . ?
O12 Ge1 O26 170.4(2) . . ?
O25 Ge1 Ge2 119.4(2) . . ?
O14 Ge1 Ge2 106.5(2) . . ?
O24 Ge1 Ge2 35.7(2) . . ?
O12 Ge1 Ge2 128.53(18) . . ?
O26 Ge1 Ge2 42.78(17) . . ?
O24 Ge2 O16 114.9(3) . . ?
O24 Ge2 O18 131.8(3) . . ?
O16 Ge2 O18 112.8(3) . . ?
O24 Ge2 O29 91.5(3) . . ?
O16 Ge2 O29 96.6(3) . . ?
O18 Ge2 O29 89.2(3) . . ?
O24 Ge2 O26 80.2(3) . . ?
O16 Ge2 O26 93.4(2) . . ?
O18 Ge2 O26 90.9(3) . . ?
O29 Ge2 O26 169.0(3) . . ?
O24 Ge2 Ge1 36.5(2) . . ?
O16 Ge2 Ge1 105.20(19) . . ?
O18 Ge2 Ge1 122.35(19) . . ?
O29 Ge2 Ge1 128.0(2) . . ?
O26 Ge2 Ge1 44.15(18) . . ?
O27 Ge3 O22 117.9(3) . . ?
O27 Ge3 O8 118.6(3) . . ?
O22 Ge3 O8 123.5(3) . . ?
O27 Ge3 O9 92.0(3) . . ?
O22 Ge3 O9 90.9(3) . . ?
O8 Ge3 O9 87.2(3) . . ?
O27 Ge3 O26 90.0(3) . . ?
O22 Ge3 O26 91.5(3) . . ?
O8 Ge3 O26 88.6(3) . . ?
O9 Ge3 O26 175.8(3) . . ?
O9 Ge4 O6 110.3(3) . 5_655 ?
O9 Ge4 O23 116.3(3) . 6_556 ?
O6 Ge4 O23 107.5(3) 5_655 6_556 ?
O9 Ge4 O31 107.4(3) . . ?
O6 Ge4 O31 106.1(3) 5_655 . ?
O23 Ge4 O31 108.8(3) 6_556 . ?
O31 Ge5 O1 108.8(3) 6_656 . ?
O31 Ge5 O15 109.2(3) 6_656 . ?
O1 Ge5 O15 107.5(3) . . ?
O31 Ge5 O13 111.5(3) 6_656 . ?
O1 Ge5 O13 110.6(3) . . ?
O15 Ge5 O13 109.1(3) . . ?
O12 Ge6 O19 117.7(3) . 5_656 ?
O12 Ge6 O5 115.7(3) . . ?
O19 Ge6 O5 106.9(3) 5_656 . ?
O12 Ge6 O1 104.0(3) . . ?
O19 Ge6 O1 106.1(3) 5_656 . ?
O5 Ge6 O1 105.2(3) . . ?
O30 Ge7 O8 109.5(4) . . ?
O30 Ge7 O25 105.6(4) . . ?
O8 Ge7 O25 113.7(3) . . ?
O30 Ge7 O28 107.8(4) . . ?
O8 Ge7 O28 109.4(3) . . ?
O25 Ge7 O28 110.6(3) . . ?
O29 Ge8 O20 111.4(4) . . ?
O29 Ge8 O32 111.8(3) . 5_656 ?
O20 Ge8 O32 100.9(4) . 5_656 ?
O29 Ge8 O3 116.5(3) . . ?
O20 Ge8 O3 103.8(4) . . ?
O32 Ge8 O3 111.0(3) 5_656 . ?
O23 Ge9 O2 110.6(3) . . ?
O23 Ge9 O4 109.4(3) . . ?
O2 Ge9 O4 107.3(3) . . ?
O23 Ge9 O13 112.3(3) . . ?
O2 Ge9 O13 107.7(3) . . ?
O4 Ge9 O13 109.4(3) . . ?
O21 Ge10 O32 115.0(3) . . ?
O21 Ge10 O19 112.5(3) . . ?
O32 Ge10 O19 115.0(3) . . ?
O21 Ge10 O15 105.4(3) . . ?
O32 Ge10 O15 100.9(3) . . ?
O19 Ge10 O15 106.5(3) . . ?
O22 Ge11 O16 115.6(3) . . ?
O22 Ge11 O11 109.7(3) . 6_556 ?
O16 Ge11 O11 102.8(3) . 6_556 ?
O22 Ge11 O7 110.9(3) . . ?
O16 Ge11 O7 111.8(3) . . ?
O11 Ge11 O7 105.1(3) 6_556 . ?
O28 Ge12 O10 117.0(3) . . ?
O28 Ge12 O17 109.3(3) . 6_656 ?
O10 Ge12 O17 107.7(3) . 6_656 ?
O28 Ge12 O2 102.2(3) . 2_654 ?
O10 Ge12 O2 110.1(3) . 2_654 ?
O17 Ge12 O2 110.5(3) 6_656 2_654 ?
O18 Ge13 O27 118.1(3) . . ?
O18 Ge13 O6 102.5(3) . . ?
O27 Ge13 O6 108.4(3) . . ?
O18 Ge13 O10 109.1(3) . . ?
O27 Ge13 O10 111.0(3) . . ?
O6 Ge13 O10 106.9(3) . . ?
O14 Ge14 O7 110.6(3) . . ?
O14 Ge14 O21 114.9(3) . 5_656 ?
O7 Ge14 O21 108.0(3) . 5_656 ?
O14 Ge14 O17 105.9(3) . . ?
O7 Ge14 O17 110.6(3) . . ?
O21 Ge14 O17 106.8(3) 5_656 . ?
O3 Ge15 O11 110.1(3) . . ?
O3 Ge15 O5 117.3(3) . . ?
O11 Ge15 O5 108.5(3) . . ?
O3 Ge15 O4 103.0(3) . . ?
O11 Ge15 O4 108.5(3) . . ?
O5 Ge15 O4 109.0(3) . . ?
Ge5 O1 Ge6 123.4(3) . . ?
Ge9 O2 Si12 125.9(3) . 2_655 ?
Ge9 O2 Ge12 125.9(3) . 2_655 ?
Si12 O2 Ge12 0.0 2_655 2_655 ?
Ge15 O3 Ge8 145.0(4) . . ?
Ge9 O4 Ge15 125.8(3) . . ?
Ge15 O5 Ge6 132.4(3) . . ?
Ge13 O6 Ge4 127.5(3) . 5_655 ?
Ge14 O7 Ge11 126.7(3) . . ?
Ge7 O8 Ge3 125.7(3) . . ?
Ge4 O9 Ge3 129.9(3) . . ?
Ge12 O10 Ge13 138.0(3) . . ?
Ge15 O11 Si11 130.5(3) . 6_656 ?
Ge15 O11 Ge11 130.5(3) . 6_656 ?
Si11 O11 Ge11 0.0 6_656 6_656 ?
Ge6 O12 Ge1 127.1(3) . . ?
Ge9 O13 Ge5 127.1(3) . . ?
Ge14 O14 Ge1 128.1(3) . . ?
Ge5 O15 Ge10 127.3(3) . . ?
Ge11 O16 Ge2 128.1(3) . . ?
Si12 O17 Ge12 0.0 6_556 6_556 ?
Si12 O17 Ge14 129.3(3) 6_556 . ?
Ge12 O17 Ge14 129.3(3) 6_556 . ?
Ge13 O18 Ge2 125.1(3) . . ?
Ge10 O19 Si6 132.3(4) . 5_656 ?
Ge10 O19 Ge6 132.3(4) . 5_656 ?
Si6 O19 Ge6 0.0 5_656 5_656 ?
Ge8 O20 Si8 152.3 . 7 ?
Ge8 O20 Ge8 152.3(7) . 7 ?
Si8 O20 Ge8 0.0 7 7 ?
Ge10 O21 Si14 147.6(4) . 5_656 ?
Ge10 O21 Ge14 147.6(4) . 5_656 ?
Si14 O21 Ge14 0.0 5_656 5_656 ?
Ge11 O22 Ge3 130.5(3) . . ?
Ge9 O23 Ge4 128.4(3) . 6_656 ?
Ge2 O24 Ge1 107.8(3) . . ?
Ge7 O25 Ge1 122.0(3) . . ?
Ge2 O26 Ge3 132.8(3) . . ?
Ge2 O26 Ge1 93.1(3) . . ?
Ge3 O26 Ge1 130.8(3) . . ?
Ge13 O27 Ge3 126.7(4) . . ?
Ge12 O28 Ge7 135.8(4) . . ?
Ge8 O29 Ge2 120.3(3) . . ?
Si7 O30 Ge7 0.0 7_565 7_565 ?
Si7 O30 Ge7 153.3 7_565 . ?
Ge7 O30 Ge7 153.3(7) 7_565 . ?
Ge5 O31 Ge4 129.7(4) 6_556 . ?
Ge10 O32 Si8 134.2(4) . 5_656 ?
Ge10 O32 Ge8 134.2(4) . 5_656 ?
Si8 O32 Ge8 0.0 5_656 5_656 ?
C13 N1 C13 113.6(15) . 7_565 ?
C13 N1 C12 108.9(10) . . ?
C13 N1 C12 108.9(10) 7_565 . ?
C13 N1 C11 109.2(10) . . ?
C13 N1 C11 109.2(10) 7_565 . ?
C12 N1 C11 106.8(12) . . ?
C14 C11 N1 106.9(18) . . ?
C11 C14 C15 108.3(17) . . ?
C23 N2 C23 115.1(16) 7_565 . ?
C23 N2 C22 109.1(10) 7_565 . ?
C23 N2 C22 109.1(10) . . ?
C23 N2 C21 106.4(10) 7_565 . ?
C23 N2 C21 106.4(10) . . ?
C22 N2 C21 110.5(15) . . ?
N2 C21 C24 103.1(16) . . ?
C25 C24 C21 108.7(19) . . ?
C33 N3 C33 112.6(15) . 7_565 ?
C33 N3 C31 109.7(10) . . ?
C33 N3 C31 109.7(10) 7_565 . ?
C33 N3 C32 108.2(10) . . ?
C33 N3 C32 108.2(10) 7_565 . ?
C31 N3 C32 108.2(14) . . ?
N3 C31 C34 111.0(17) . . ?
C31 C34 C35 107.5(17) . . ?
C43 N4 C43 113.5(17) 7_565 . ?
C43 N4 C41 109.7(12) 7_565 . ?
C43 N4 C41 109.7(12) . . ?
C43 N4 C42 108.4(12) 7_565 . ?
C43 N4 C42 108.4(12) . . ?
C41 N4 C42 106.9(16) . . ?
N4 C41 C44 105(4) . . ?
C41 C44 C45 107.6(19) . . ?

_refine_diff_density_max         3.453
_refine_diff_density_min         -1.388
_refine_diff_density_rms         0.263





_exptl_crystal_recrystallization_method 'Hydrothermal Synthesis'
_chemical_compound_source        GeO2
_exptl_crystal_preparation       'CO2 adsorption'
