#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:53:39 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179602 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/66/4506688.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4506688
loop_
_publ_author_name
'Inge, A. Ken'
'Huang, Shiliang'
'Chen, Hong'
'Moraga, Francisca'
'Sun, Junliang'
'Zou, Xiaodong'
_publ_section_title
;
 The Structure of a Complex Open-Framework Germanate Obtained by
 Combining Powder Charge-Flipping and Simulated Annealing
;
_journal_issue                   10
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4853
_journal_paper_doi               10.1021/cg300647s
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         Ge12H2O27,C6H17N3,2(H4N)
_chemical_formula_sum            'C6 H27 Ge12 N5 O27'
_chemical_formula_weight         1472.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.870(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6277(10)
_cell_length_b                   17.3845(11)
_cell_length_c                   16.305(2)
_cell_measurement_reflns_used    10202
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.2557
_cell_measurement_theta_min      1.6698
_cell_volume                     3220.7(6)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET)
        (compiled Dec  8 2009,17:31:18)
;
_computing_data_collection
;                                                    
        CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009) 
;
_computing_data_reduction
;
         CrysAlisPro, Oxford Diffraction Ltd., 
         Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) 
         (compiled Dec  8 2009,17:31:18) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Diamond Light Source Beamline I19'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.1873
_diffrn_reflns_av_sigmaI/netI    0.1869
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21060
_diffrn_reflns_theta_full        24.21
_diffrn_reflns_theta_max         24.21
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    9.994
_exptl_absorpt_correction_T_max  0.9425
_exptl_absorpt_correction_T_min  0.8895
_exptl_absorpt_process_details
;                                                          
CrysAlis RED, Oxford Diffraction Ltd.,                     
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)  
(compiled Jan 10 2008,16:37:18)                            
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm.          
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.037
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blcok
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.012
_refine_diff_density_max         3.205
_refine_diff_density_min         -2.184
_refine_diff_density_rms         0.363
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         5497
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0780
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0719P)²+7.8956P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2010
_refine_ls_wR_factor_ref         0.2201
_reflns_number_gt                4204
_reflns_number_total             5497
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg300647s_si_002.cif
_cod_data_source_block           1760
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        3220.7(5)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4506688
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge2 Ge 0.80371(11) 0.41696(8) 0.88421(9) 0.0172(3) Uani 1 1 d . . .
Ge3 Ge 0.94098(11) 0.40478(8) 0.65241(9) 0.0156(3) Uani 1 1 d . . .
Ge4 Ge 0.94523(11) 0.50558(7) 0.80361(9) 0.0155(3) Uani 1 1 d . . .
Ge5 Ge 0.61868(11) 0.38309(8) 0.67615(9) 0.0184(3) Uani 1 1 d . . .
Ge6 Ge 1.16759(12) 0.42913(8) 0.62472(9) 0.0200(3) Uani 1 1 d D . .
Ge7 Ge 0.79825(11) 0.26301(8) 0.65519(9) 0.0197(3) Uani 1 1 d . . .
Ge8 Ge 1.18408(11) 0.58818(7) 0.91277(9) 0.0150(3) Uani 1 1 d . . .
Ge9 Ge 0.65764(12) 0.64891(8) 0.45148(9) 0.0210(3) Uani 1 1 d D . .
Ge10 Ge 0.98083(11) 0.33605(7) 0.83161(9) 0.0169(3) Uani 1 1 d . A .
Ge11 Ge 0.73922(12) 0.51885(8) 0.61283(9) 0.0217(3) Uani 1 1 d . . .
Ge12 Ge 1.16656(11) 0.43200(7) 0.81603(9) 0.0142(3) Uani 1 1 d . A .
Ge1A Ge 1.23622(15) 0.31730(10) 0.97515(12) 0.0213(4) Uani 0.819(3) 1 d PD A 1
Ge1B Ge 1.2269(7) 0.2707(4) 0.8991(5) 0.0213(4) Uani 0.181(3) 1 d PD A 2
O1 O 0.6620(8) 0.2995(5) 0.6421(7) 0.024(2) Uani 1 1 d . . .
O2 O 0.6257(8) 0.4664(5) 0.6188(6) 0.022(2) Uani 1 1 d . . .
O3 O 0.4677(8) 0.3712(6) 0.6450(6) 0.027(2) Uani 1 1 d . . .
O4 O 1.3438(9) 0.2436(6) 1.0159(7) 0.031(2) Uani 1 1 d . . .
O5 O 0.6612(10) 0.5900(7) 0.5378(7) 0.042(3) Uani 1 1 d D . .
O6 O 0.8334(8) 0.5653(5) 0.7140(6) 0.024(2) Uani 1 1 d . . .
O7 O 0.8262(7) 0.4680(5) 0.5726(6) 0.0208(19) Uani 1 1 d . . .
O8 O 0.8612(8) 0.3168(5) 0.5976(6) 0.0192(18) Uani 1 1 d . . .
O9 O 0.8955(8) 0.2521(5) 0.7688(6) 0.022(2) Uani 1 1 d . . .
O10 O 0.7540(9) 0.1752(6) 0.5992(8) 0.032(2) Uani 1 1 d . . .
O11 O 1.2425(8) 0.5195(5) 0.8691(7) 0.023(2) Uani 1 1 d . . .
O12 O 1.0309(8) 0.5899(5) 0.8586(6) 0.0224(19) Uani 1 1 d . . .
O13 O 0.8644(8) 0.5040(5) 0.8728(6) 0.024(2) Uani 1 1 d . . .
O14 O 0.6681(8) 0.3953(6) 0.7924(6) 0.025(2) Uani 1 1 d . . .
O15 O 0.7574(8) 0.4242(5) 0.9696(6) 0.024(2) Uani 1 1 d . . .
O16 O 1.0298(7) 0.4889(4) 0.7261(6) 0.0160(18) Uani 1 1 d . . .
O17 O 0.8703(8) 0.4066(5) 0.7395(6) 0.0194(11) Uani 1 1 d . . .
O18 O 0.9016(8) 0.3425(5) 0.9023(6) 0.0194(11) Uani 1 1 d . . .
O19 O 1.0216(8) 0.4035(5) 0.5839(6) 0.0194(11) Uani 1 1 d . . .
O20 O 1.0649(7) 0.4330(5) 0.8786(6) 0.0160(18) Uani 1 1 d . . .
O21 O 1.0610(7) 0.3467(5) 0.7535(6) 0.0192(19) Uani 1 1 d . . .
O22 O 1.1898(11) 0.5228(6) 0.5945(7) 0.037(3) Uani 1 1 d D . .
H22 H 1.190(10) 0.523(2) 0.539(4) 0.056 Uiso 1 1 d D . .
O23 O 1.2192(9) 0.3638(7) 0.5695(8) 0.035(2) Uani 1 1 d . . .
O24 O 1.2425(7) 0.4239(5) 0.7434(6) 0.0181(19) Uani 1 1 d . . .
O25 O 1.2749(8) 0.3687(5) 0.9030(6) 0.0207(19) Uani 1 1 d . . .
O26 O 1.0971(8) 0.2762(5) 0.9149(6) 0.0218(19) Uani 1 1 d . . .
O27A O 1.2458(11) 0.3647(7) 1.0726(8) 0.033(3) Uani 0.819(3) 1 d PD A 1
H27A H 1.291(9) 0.407(5) 1.095(5) 0.050 Uiso 0.819(3) 1 d PD A 1
O27B O 1.216(5) 0.221(3) 0.799(2) 0.033(3) Uani 0.181(3) 1 d PD A 2
H27B H 1.21(2) 0.249(5) 0.750(6) 0.050 Uiso 0.181(3) 1 d PD A 2
N4 N 0.0433(15) 0.2761(10) 0.0757(12) 0.059(4) Uiso 1 1 d D . .
H4B H 0.052(6) 0.283(5) 0.132(2) 0.071 Uiso 1 1 d D . .
H4A H 0.020(7) 0.320(2) 0.044(5) 0.071 Uiso 1 1 d D . .
H4C H 0.112(4) 0.262(5) 0.077(5) 0.071 Uiso 1 1 d D . .
H4D H -0.010(5) 0.240(3) 0.047(5) 0.071 Uiso 1 1 d D . .
N5 N 0.9822(11) 0.1211(7) 0.8783(9) 0.033(3) Uiso 1 1 d D . .
H5A H 1.053(3) 0.141(3) 0.912(4) 0.040 Uiso 1 1 d D . .
H5B H 0.956(5) 0.097(4) 0.914(4) 0.040 Uiso 1 1 d D . .
H5C H 0.932(4) 0.159(3) 0.848(5) 0.040 Uiso 1 1 d D . .
H5D H 0.986(7) 0.088(4) 0.838(4) 0.040 Uiso 1 1 d D . .
C1A C 0.653(3) 0.184(2) 0.805(4) 0.210(15) Uiso 0.819(3) 1 d PD A 1
H1A1 H 0.7172 0.1608 0.8570 0.252 Uiso 0.819(3) 1 calc PR A 1
H1A2 H 0.6740 0.2371 0.8010 0.252 Uiso 0.819(3) 1 calc PR A 1
C2A C 0.637(4) 0.143(3) 0.723(3) 0.210(15) Uiso 0.819(3) 1 d PD A 1
H2A1 H 0.7129 0.1372 0.7226 0.252 Uiso 0.819(3) 1 calc PR A 1
H2A2 H 0.5886 0.1749 0.6705 0.252 Uiso 0.819(3) 1 calc PR A 1
C3A C 0.485(4) 0.062(2) 0.736(4) 0.210(15) Uiso 0.819(3) 1 d PD A 1
H3A1 H 0.4762 0.0089 0.7485 0.252 Uiso 0.819(3) 1 calc PR A 1
H3A2 H 0.4140 0.0780 0.6840 0.252 Uiso 0.819(3) 1 calc PR A 1
C4A C 0.495(4) 0.108(2) 0.814(4) 0.210(15) Uiso 0.819(3) 1 d PD A 1
H4A1 H 0.4174 0.1138 0.8114 0.252 Uiso 0.819(3) 1 calc PR A 1
H4A2 H 0.5424 0.0790 0.8694 0.252 Uiso 0.819(3) 1 calc PR A 1
C5A C 0.526(3) 0.242(2) 0.868(3) 0.210(15) Uiso 0.819(3) 1 d PD A 1
H5A1 H 0.5979 0.2720 0.8973 0.252 Uiso 0.819(3) 1 calc PR A 1
H5A2 H 0.5094 0.2201 0.9154 0.252 Uiso 0.819(3) 1 calc PR A 1
C6A C 0.431(3) 0.2961(19) 0.817(5) 0.210(15) Uiso 0.819(3) 1 d PD A 1
H6A1 H 0.4237 0.3327 0.8587 0.252 Uiso 0.819(3) 1 calc PR A 1
H6A2 H 0.4513 0.3245 0.7743 0.252 Uiso 0.819(3) 1 calc PR A 1
N1A N 0.582(6) 0.068(3) 0.712(5) 0.38(4) Uiso 0.819(3) 1 d PD A 1
H1A3 H 0.5557 0.0537 0.6533 0.451 Uiso 0.819(3) 1 calc PR A 1
H1A4 H 0.6375 0.0342 0.7460 0.451 Uiso 0.819(3) 1 calc PR A 1
N2A N 0.548(4) 0.184(2) 0.822(4) 0.38(4) Uiso 0.819(3) 1 d PD A 1
N3A N 0.326(3) 0.261(2) 0.770(5) 0.38(4) Uiso 0.819(3) 1 d PD A 1
H3A3 H 0.2754 0.2939 0.7310 0.564 Uiso 0.819(3) 1 calc PR A 1
H3A4 H 0.2991 0.2441 0.8086 0.564 Uiso 0.819(3) 1 calc PR A 1
H3A5 H 0.3357 0.2210 0.7392 0.564 Uiso 0.819(3) 1 calc PR A 1
C1B C 0.358(3) 0.097(2) 0.714(5) 0.210(15) Uiso 0.181(3) 1 d PRD A 2
H1B1 H 0.2914 0.1046 0.6548 0.252 Uiso 0.181(3) 1 calc PR A 2
H1B2 H 0.3370 0.0563 0.7444 0.252 Uiso 0.181(3) 1 calc PR A 2
C2B C 0.374(5) 0.167(3) 0.766(7) 0.210(5) Uiso 0.181(3) 1 d PD A 2
H2B1 H 0.3978 0.1524 0.8290 0.252 Uiso 0.181(3) 1 calc PR A 2
H2B2 H 0.2981 0.1920 0.7448 0.252 Uiso 0.181(3) 1 calc PR A 2
C3B C 0.553(5) 0.198(3) 0.743(8) 0.210(5) Uiso 0.181(3) 1 d PD A 2
H3B1 H 0.5694 0.2389 0.7106 0.252 Uiso 0.181(3) 1 calc PR A 2
H3B2 H 0.6224 0.1913 0.8007 0.252 Uiso 0.181(3) 1 calc PR A 2
C4B C 0.537(5) 0.128(3) 0.691(7) 0.210(5) Uiso 0.181(3) 1 d PD A 2
H4B1 H 0.5091 0.1420 0.6277 0.252 Uiso 0.181(3) 1 calc PR A 2
H4B2 H 0.6134 0.1040 0.7103 0.252 Uiso 0.181(3) 1 calc PR A 2
C5B C 0.448(6) -0.001(2) 0.656(5) 0.210(5) Uiso 0.181(3) 1 d PD A 2
H5B1 H 0.5272 -0.0209 0.6753 0.252 Uiso 0.181(3) 1 calc PR A 2
H5B2 H 0.4073 -0.0359 0.6789 0.252 Uiso 0.181(3) 1 calc PR A 2
C6B C 0.389(8) -0.004(4) 0.557(5) 0.210(5) Uiso 0.181(3) 1 d PD A 2
H6B1 H 0.3875 -0.0561 0.5364 0.252 Uiso 0.181(3) 1 calc PR A 2
H6B2 H 0.3083 0.0137 0.5359 0.252 Uiso 0.181(3) 1 calc PR A 2
N1B N 0.458(8) 0.224(3) 0.765(11) 0.38(4) Uiso 0.181(3) 1 d PD A 2
H1B3 H 0.4909 0.2466 0.8198 0.451 Uiso 0.181(3) 1 calc PR A 2
H1B4 H 0.4174 0.2602 0.7239 0.451 Uiso 0.181(3) 1 calc PR A 2
N2B N 0.456(6) 0.069(2) 0.697(6) 0.38(4) Uiso 0.181(3) 1 d PD A 2
N3B N 0.445(6) 0.042(2) 0.520(6) 0.38(4) Uiso 0.181(3) 1 d PRD A 2
H3B3 H 0.3907 0.0728 0.4807 0.564 Uiso 0.181(3) 1 d PR A 2
H3B4 H 0.4776 0.0139 0.4918 0.564 Uiso 0.181(3) 1 d PR A 2
H3B5 H 0.5001 0.0697 0.5638 0.564 Uiso 0.181(3) 1 d PR A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0029 0.0015 '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 0.1924 1.7125 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0057 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0101 0.0057 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O18 Ge2 O15 112.7(4) . .
O18 Ge2 O13 110.7(4) . .
O15 Ge2 O13 109.9(4) . .
O18 Ge2 O14 110.2(5) . .
O15 Ge2 O14 99.0(4) . .
O13 Ge2 O14 113.9(5) . .
O19 Ge3 O7 93.0(4) . .
O19 Ge3 O8 91.5(4) . .
O7 Ge3 O8 93.4(4) . .
O19 Ge3 O16 93.6(4) . .
O7 Ge3 O16 93.0(4) . .
O8 Ge3 O16 171.6(4) . .
O19 Ge3 O21 94.3(4) . .
O7 Ge3 O21 170.7(4) . .
O8 Ge3 O21 92.2(4) . .
O16 Ge3 O21 80.8(4) . .
O19 Ge3 O17 173.6(4) . .
O7 Ge3 O17 92.0(4) . .
O8 Ge3 O17 92.2(4) . .
O16 Ge3 O17 82.1(4) . .
O21 Ge3 O17 80.3(4) . .
O12 Ge4 O13 94.6(4) . .
O12 Ge4 O6 91.2(4) . .
O13 Ge4 O6 93.2(4) . .
O12 Ge4 O20 94.7(4) . .
O13 Ge4 O20 95.3(4) . .
O6 Ge4 O20 169.1(4) . .
O12 Ge4 O16 93.6(4) . .
O13 Ge4 O16 170.7(4) . .
O6 Ge4 O16 90.9(4) . .
O20 Ge4 O16 79.6(3) . .
O12 Ge4 O17 171.6(4) . .
O13 Ge4 O17 92.6(4) . .
O6 Ge4 O17 92.6(4) . .
O20 Ge4 O17 80.3(4) . .
O16 Ge4 O17 78.9(3) . .
O1 Ge5 O14 116.2(5) . .
O1 Ge5 O2 115.4(5) . .
O14 Ge5 O2 113.9(5) . .
O1 Ge5 O3 105.3(5) . .
O14 Ge5 O3 99.1(4) . .
O2 Ge5 O3 104.2(4) . .
O19 Ge6 O24 112.7(4) . .
O19 Ge6 O23 102.2(5) . .
O24 Ge6 O23 113.3(5) . .
O19 Ge6 O22 113.9(5) . .
O24 Ge6 O22 106.5(5) . .
O23 Ge6 O22 108.5(5) . .
O9 Ge7 O10 112.4(5) . .
O9 Ge7 O8 111.0(4) . .
O10 Ge7 O8 107.8(5) . .
O9 Ge7 O1 111.7(5) . .
O10 Ge7 O1 100.4(4) . .
O8 Ge7 O1 113.2(4) . .
O11 Ge8 O12 112.7(4) . .
O11 Ge8 O15 108.6(5) . 3_767
O12 Ge8 O15 113.9(4) . 3_767
O11 Ge8 O10 105.2(5) . 2_756
O12 Ge8 O10 112.3(4) . 2_756
O15 Ge8 O10 103.5(5) 3_767 2_756
O3 Ge9 O5 108.2(5) 3_666 .
O3 Ge9 O4 110.3(5) 3_666 2_756
O5 Ge9 O4 108.3(6) . 2_756
O3 Ge9 O23 109.9(5) 3_666 3_766
O5 Ge9 O23 112.1(5) . 3_766
O4 Ge9 O23 108.1(5) 2_756 3_766
O18 Ge10 O26 92.8(4) . .
O18 Ge10 O9 92.9(4) . .
O26 Ge10 O9 92.7(4) . .
O18 Ge10 O21 170.9(4) . .
O26 Ge10 O21 93.5(4) . .
O9 Ge10 O21 93.3(4) . .
O18 Ge10 O20 93.0(4) . .
O26 Ge10 O20 94.4(4) . .
O9 Ge10 O20 170.5(4) . .
O21 Ge10 O20 80.1(4) . .
O18 Ge10 O17 92.4(4) . .
O26 Ge10 O17 173.2(4) . .
O9 Ge10 O17 91.2(4) . .
O21 Ge10 O17 80.8(4) . .
O20 Ge10 O17 81.1(4) . .
O5 Ge11 O2 100.8(5) . .
O5 Ge11 O7 110.9(5) . .
O2 Ge11 O7 115.2(4) . .
O5 Ge11 O6 106.4(5) . .
O2 Ge11 O6 115.2(4) . .
O7 Ge11 O6 107.9(4) . .
O11 Ge12 O24 93.3(4) . .
O11 Ge12 O25 94.3(4) . .
O24 Ge12 O25 91.7(4) . .
O11 Ge12 O21 170.7(4) . .
O24 Ge12 O21 91.9(4) . .
O25 Ge12 O21 93.2(4) . .
O11 Ge12 O20 94.3(4) . .
O24 Ge12 O20 171.2(4) . .
O25 Ge12 O20 92.3(4) . .
O21 Ge12 O20 80.0(4) . .
O11 Ge12 O16 92.5(4) . .
O24 Ge12 O16 95.4(4) . .
O25 Ge12 O16 169.9(4) . .
O21 Ge12 O16 79.4(3) . .
O20 Ge12 O16 79.8(3) . .
O25 Ge1A O27A 116.9(5) . .
O25 Ge1A O26 110.2(4) . .
O27A Ge1A O26 110.9(5) . .
O25 Ge1A O4 103.5(5) . .
O27A Ge1A O4 105.2(5) . .
O26 Ge1A O4 109.5(4) . .
O27B Ge1B O26 116.7(19) . .
O27B Ge1B O25 112.5(18) . .
O26 Ge1B O25 105.2(6) . .
O27B Ge1B O4 120.5(18) . .
O26 Ge1B O4 103.4(6) . .
O25 Ge1B O4 95.6(5) . .
Ge5 O1 Ge7 134.1(6) . .
Ge11 O2 Ge5 134.5(5) . .
Ge9 O3 Ge5 137.8(6) 3_666 .
Ge9 O4 Ge1A 133.9(6) 2_746 .
Ge9 O4 Ge1B 116.0(6) 2_746 .
Ge1A O4 Ge1B 46.2(3) . .
Ge11 O5 Ge9 144.3(7) . .
Ge11 O6 Ge4 117.2(5) . .
Ge11 O7 Ge3 118.0(5) . .
Ge7 O8 Ge3 117.9(4) . .
Ge7 O9 Ge10 118.6(5) . .
Ge7 O10 Ge8 139.4(6) . 2_746
Ge8 O11 Ge12 123.5(5) . .
Ge8 O12 Ge4 121.9(5) . .
Ge2 O13 Ge4 118.0(5) . .
Ge5 O14 Ge2 135.4(5) . .
Ge2 O15 Ge8 138.2(6) . 3_767
Ge3 O16 Ge12 99.6(4) . .
Ge3 O16 Ge4 100.3(4) . .
Ge12 O16 Ge4 98.0(4) . .
Ge10 O17 Ge3 98.4(4) . .
Ge10 O17 Ge4 96.8(4) . .
Ge3 O17 Ge4 97.4(4) . .
Ge2 O18 Ge10 119.2(5) . .
Ge6 O19 Ge3 123.6(5) . .
Ge4 O20 Ge12 100.6(4) . .
Ge4 O20 Ge10 100.0(4) . .
Ge12 O20 Ge10 98.9(4) . .
Ge12 O21 Ge10 99.2(4) . .
Ge12 O21 Ge3 98.5(4) . .
Ge10 O21 Ge3 99.6(4) . .
Ge9 O23 Ge6 138.6(7) 3_766 .
Ge6 O24 Ge12 122.1(5) . .
Ge1A O25 Ge1B 48.5(3) . .
Ge1A O25 Ge12 120.1(5) . .
Ge1B O25 Ge12 114.4(5) . .
Ge1A O26 Ge1B 48.4(4) . .
Ge1A O26 Ge10 118.0(5) . .
Ge1B O26 Ge10 114.7(5) . .
H4B N4 H4A 110.13 . .
H4B N4 H4C 109.48 . .
H4A N4 H4C 108.57 . .
H4B N4 H4D 111.40 . .
H4A N4 H4D 108.34 . .
H4C N4 H4D 108.86 . .
H5B N5 H5D 109.49 . .
N2A C1A C2A 113.4(19) . .
N2A C1A H1A1 108.9 . .
C2A C1A H1A1 109.75 . .
N2A C1A H1A2 108.9 . .
C2A C1A H1A2 109.75 . .
H1A1 C1A H1A2 107.7 . .
C1A C2A N1A 115(2) . .
C1A C2A H2A1 108.6 . .
N1A C2A H2A1 108.6 . .
C1A C2A H2A2 108.6 . .
N1A C2A H2A2 108.6 . .
H2A1 C2A H2A2 107.6 . .
N1A C3A C4A 116(2) . .
N1A C3A H3A1 108.2 . .
C4A C3A H3A1 108.2 . .
N1A C3A H3A2 108.2 . .
C4A C3A H3A2 107.49 . .
H3A1 C3A H3A2 107.3 . .
N2A C4A C3A 115(2) . .
N2A C4A H4A1 108.5 . .
C3A C4A H4A1 108.5 . .
N2A C4A H4A2 108.5 . .
C3A C4A H4A2 108.5 . .
H4A1 C4A H4A2 107.5 . .
N2A C5A C6A 119(2) . .
N2A C5A H5A1 107.6 . .
C6A C5A H5A1 107.6 . .
N2A C5A H5A2 108.59 . .
C6A C5A H5A2 107.6 . .
H5A1 C5A H5A2 107.1 . .
N3A C6A C5A 113(2) . .
N3A C6A H6A1 109.0 . .
C5A C6A H6A1 109.0 . .
N3A C6A H6A2 109.0 . .
C5A C6A H6A2 109.0 . .
H6A1 C6A H6A2 107.8 . .
C3A N1A C2A 116(2) . .
C3A N1A H1A3 108.2 . .
C2A N1A H1A3 108.2 . .
C3A N1A H1A4 108.2 . .
C2A N1A H1A4 108.2 . .
H1A3 N1A H1A4 107.4 . .
C3A N1A H3B5 105.0 . .
C2A N1A H3B5 95.4 . .
H1A4 N1A H3B5 123.9 . .
C5A N2A C1A 120.8(18) . .
C5A N2A C4A 122.4(19) . .
C1A N2A C4A 113.7(17) . .
C6A N3A H3A3 109.5 . .
C6A N3A H3A4 109.5 . .
H3A3 N3A H3A4 109.5 . .
C6A N3A H3A5 109.5 . .
H3A3 N3A H3A5 109.5 . .
H3A4 N3A H3A5 109.5 . .
C2B C1B N2B 118.5(18) . .
C2B C1B H1B1 107.7 . .
N2B C1B H1B1 107.7 . .
C2B C1B H1B2 107.7 . .
N2B C1B H1B2 107.7 . .
H1B1 C1B H1B2 107.1 . .
C1B C2B N1B 118(2) . .
C1B C2B H2B1 107.7 . .
N1B C2B H2B1 107.7 . .
C1B C2B H2B2 107.7 . .
N1B C2B H2B2 107.7 . .
H2B1 C2B H2B2 107.1 . .
C4B C3B N1B 119(2) . .
C4B C3B H3B1 107.6 . .
N1B C3B H3B1 107.6 . .
C4B C3B H3B2 107.6 . .
N1B C3B H3B2 107.6 . .
H3B1 C3B H3B2 107.0 . .
N2B C4B C3B 118(2) . .
N2B C4B H4B1 107.8 . .
C3B C4B H4B1 107.8 . .
N2B C4B H4B2 107.8 . .
C3B C4B H4B2 107.8 . .
H4B1 C4B H4B2 107.2 . .
C6B C5B N2B 117(2) . .
C6B C5B H5B1 108.0 . .
N2B C5B H5B1 108.0 . .
C6B C5B H5B2 108.0 . .
N2B C5B H5B2 108.0 . .
H5B1 C5B H5B2 107.2 . .
N3B C6B C5B 111(4) . .
N3B C6B H6B1 109.5 . .
C5B C6B H6B1 109.5 . .
N3B C6B H6B2 109.5 . .
C5B C6B H6B2 109.5 . .
H6B1 C6B H6B2 108.1 . .
C2B N1B C3B 118(2) . .
C2B N1B H1B3 107.8 . .
C3B N1B H1B3 107.8 . .
C2B N1B H1B4 107.8 . .
C3B N1B H1B4 107.8 . .
H1B3 N1B H1B4 107.1 . .
C4B N2B C1B 117(2) . .
C4B N2B C5B 120(2) . .
C1B N2B C5B 120(2) . .
C6B N3B H3B3 106.8 . .
C6B N3B H3B4 111.3 . .
H3B3 N3B H3B4 109.5 . .
C6B N3B H3B5 110.2 . .
H3B3 N3B H3B5 109.5 . .
H3B4 N3B H3B5 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge2 O18 1.724(9) .
Ge2 O15 1.734(9) .
Ge2 O13 1.742(10) .
Ge2 O14 1.754(9) .
Ge3 O19 1.810(8) .
Ge3 O7 1.833(9) .
Ge3 O8 1.836(9) .
Ge3 O16 1.913(8) .
Ge3 O21 1.963(9) .
Ge3 O17 1.979(8) .
Ge4 O12 1.810(9) .
Ge4 O13 1.823(8) .
Ge4 O6 1.845(9) .
Ge4 O20 1.939(8) .
Ge4 O16 2.000(8) .
Ge4 O17 2.022(9) .
Ge5 O1 1.727(9) .
Ge5 O14 1.730(9) .
Ge5 O2 1.747(9) .
Ge5 O3 1.758(9) .
Ge6 O19 1.724(9) .
Ge6 O24 1.747(9) .
Ge6 O23 1.743(10) .
Ge6 O22 1.759(10) .
Ge7 O9 1.730(9) .
Ge7 O10 1.741(9) .
Ge7 O8 1.743(8) .
Ge7 O1 1.758(9) .
Ge8 O11 1.712(8) .
Ge8 O12 1.742(10) .
Ge8 O15 1.742(9) 3_767
Ge8 O10 1.752(10) 2_756
Ge9 O3 1.711(9) 3_666
Ge9 O5 1.725(7) .
Ge9 O4 1.733(10) 2_756
Ge9 O23 1.746(9) 3_766
Ge10 O18 1.829(8) .
Ge10 O26 1.828(9) .
Ge10 O9 1.838(9) .
Ge10 O21 1.952(8) .
Ge10 O20 1.960(9) .
Ge10 O17 1.970(9) .
Ge11 O5 1.716(9) .
Ge11 O2 1.737(9) .
Ge11 O7 1.745(8) .
Ge11 O6 1.754(9) .
Ge12 O11 1.806(9) .
Ge12 O24 1.825(8) .
Ge12 O25 1.844(9) .
Ge12 O21 1.957(9) .
Ge12 O20 1.958(8) .
Ge12 O16 1.975(9) .
Ge1A O25 1.710(8) .
Ge1A O27A 1.747(11) .
Ge1A O26 1.748(9) .
Ge1A O4 1.772(10) .
Ge1B O27B 1.80(2) .
Ge1B O26 1.769(11) .
Ge1B O25 1.799(12) .
Ge1B O4 1.891(13) .
O3 Ge9 1.711(9) 3_666
O4 Ge9 1.733(10) 2_746
O10 Ge8 1.752(9) 2_746
O15 Ge8 1.742(9) 3_767
O23 Ge9 1.746(9) 3_766
N4 H4B 0.879(18) .
N4 H4A 0.895(18) .
N4 H4C 0.891(18) .
N4 H4D 0.886(18) .
N5 H5B 0.885(18) .
N5 H5D 0.890(18) .
C1A N2A 1.464(18) .
C1A C2A 1.456(19) .
C1A H1A1 0.9700 .
C1A H1A2 0.9700 .
C2A N1A 1.46(2) .
C2A H2A1 0.9700 .
C2A H2A2 0.9700 .
C3A N1A 1.440(19) .
C3A C4A 1.454(19) .
C3A H3A1 0.9700 .
C3A H3A2 0.9700 .
C4A N2A 1.458(18) .
C4A H4A1 0.9700 .
C4A H4A2 0.9700 .
C5A N2A 1.360(16) .
C5A C6A 1.46(2) .
C5A H5A1 0.9700 .
C5A H5A2 0.9700 .
C6A N3A 1.35(2) .
C6A H6A1 0.9700 .
C6A H6A2 0.9700 .
N1A H1A3 0.9000 .
N1A H1A4 0.9000 .
N3A H3A3 0.8900 .
N3A H3A4 0.8900 .
N3A H3A5 0.8900 .
C1B C2B 1.451(18) .
C1B N2B 1.462(19) .
C1B H1B1 0.9700 .
C1B H1B2 0.9700 .
C2B N1B 1.46(2) .
C2B H2B1 0.9700 .
C2B H2B2 0.9700 .
C3B C4B 1.449(19) .
C3B N1B 1.454(19) .
C3B H3B1 0.9700 .
C3B H3B2 0.9700 .
C4B N2B 1.470(19) .
C4B H4B1 0.9700 .
C4B H4B2 0.9700 .
C5B C6B 1.45(2) .
C5B N2B 1.372(16) .
C5B H5B1 0.9700 .
C5B H5B2 0.9700 .
C6B N3B 1.35(2) .
C6B H6B1 0.9700 .
C6B H6B2 0.9700 .
N1B H1B3 0.9000 .
N1B H1B4 0.9000 .
N3B H3B3 0.8900 .
N3B H3B4 0.8900 .
N3B H3B5 0.8900 .
