# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1440864'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-02-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'8(C24 H24 Ge O6), C2 H4 Cl4, 15(C H2 Cl2), 16(C2 H8 N)'

_chemical_formula_sum            'C241 H354 Cl34 Ge8 N16 O48'
_chemical_formula_weight         6029.40

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'
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'
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'
H H 0.0000 0.0000 '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                   13.5662(3)
_cell_length_b                   23.6439(6)
_cell_length_c                   24.7100(6)
_cell_angle_alpha                69.244(2)
_cell_angle_beta                 79.577(2)
_cell_angle_gamma                79.064(2)
_cell_volume                     7220.9(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    110
_cell_measurement_reflns_used    23692
_cell_measurement_theta_min      3.2880
_cell_measurement_theta_max      28.3550

_exptl_crystal_description       block
_exptl_crystal_colour            colorless

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_F_000             3130
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_exptl_absorpt_coefficient_mu    1.204
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.98036
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            60418
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.968
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             25388
_reflns_number_gt                20742
_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 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'

_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_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)+(0.0606P)²+17.9385P] 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         25388
_refine_ls_number_parameters     1633
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1349
_refine_ls_wR_factor_gt          0.1280
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.021
_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
C49 C 0.6395(3) -0.25357(15) 0.82932(16) 0.0200(8) Uani 1 1 d . . . . .
C1C C 1.1183(5) 0.2900(2) 0.4548(2) 0.0594(15) Uani 1 1 d . . . . .
H1C1 H 1.1740 0.3140 0.4399 0.071 Uiso 1 1 calc R U . . .
H1C2 H 1.0568 0.3168 0.4431 0.071 Uiso 1 1 calc R U . . .
C7N C 0.6231(3) -0.13586(18) 0.67448(17) 0.0264(8) Uani 1 1 d . . . . .
H1N1 H 0.5591 -0.1228 0.6934 0.040 Uiso 1 1 calc R U . . .
H1N2 H 0.6385 -0.1795 0.6902 0.040 Uiso 1 1 calc R U . . .
H1N3 H 0.6199 -0.1239 0.6334 0.040 Uiso 1 1 calc R U . . .
C50 C 0.5806(3) -0.29144(16) 0.82059(17) 0.0237(8) Uani 1 1 d . . . . .
H2 H 0.5164 -0.2958 0.8412 0.028 Uiso 1 1 calc R U . . .
C2C C 0.6885(3) 0.10220(19) 0.39258(19) 0.0335(10) Uani 1 1 d . . . . .
H2C1 H 0.7188 0.0719 0.4255 0.040 Uiso 1 1 calc R U . . .
H2C2 H 0.7360 0.1309 0.3718 0.040 Uiso 1 1 calc R U . . .
C8N C 0.8042(3) -0.12446(17) 0.65554(17) 0.0265(9) Uani 1 1 d . . . . .
H2N1 H 0.8535 -0.1049 0.6632 0.040 Uiso 1 1 calc R U . . .
H2N2 H 0.8023 -0.1118 0.6142 0.040 Uiso 1 1 calc R U . . .
H2N3 H 0.8221 -0.1680 0.6704 0.040 Uiso 1 1 calc R U . . .
C51 C 0.6174(3) -0.32231(17) 0.78155(18) 0.0269(9) Uani 1 1 d . . . . .
H3 H 0.5773 -0.3472 0.7761 0.032 Uiso 1 1 calc R U . . .
C3C C 0.5197(3) 0.33748(19) 0.59549(19) 0.0319(9) Uani 1 1 d . . . . .
H3C1 H 0.5347 0.2937 0.6141 0.038 Uiso 1 1 calc R U . . .
H3C2 H 0.5038 0.3448 0.5566 0.038 Uiso 1 1 calc R U . . .
C3N C 0.4355(3) 0.02547(17) 0.71682(17) 0.0247(8) Uani 1 1 d . . . . .
H3N1 H 0.4648 0.0079 0.6870 0.037 Uiso 1 1 calc R U . . .
H3N2 H 0.4150 0.0684 0.6991 0.037 Uiso 1 1 calc R U . . .
H3N3 H 0.3776 0.0062 0.7385 0.037 Uiso 1 1 calc R U . . .
C52 C 0.7136(3) -0.31710(17) 0.74989(17) 0.0260(8) Uani 1 1 d . . . . .
C4N C 0.4704(3) 0.04222(17) 0.80388(17) 0.0277(9) Uani 1 1 d . . . . .
H4N1 H 0.5211 0.0341 0.8292 0.042 Uiso 1 1 calc R U . . .
H4N2 H 0.4117 0.0240 0.8258 0.042 Uiso 1 1 calc R U . . .
H4N3 H 0.4521 0.0855 0.7872 0.042 Uiso 1 1 calc R U . . .
C53 C 0.7712(3) -0.27979(16) 0.75961(17) 0.0240(8) Uani 1 1 d . . . . .
H5 H 0.8359 -0.2762 0.7395 0.029 Uiso 1 1 calc R U . . .
C5N C 0.9065(3) -0.06752(17) 0.79805(18) 0.0263(8) Uani 1 1 d . . . . .
H5N1 H 0.9005 -0.1026 0.7884 0.039 Uiso 1 1 calc R U . . .
H5N2 H 0.9116 -0.0796 0.8390 0.039 Uiso 1 1 calc R U . . .
H5N3 H 0.9659 -0.0503 0.7760 0.039 Uiso 1 1 calc R U . . .
C54 C 0.7360(3) -0.24779(16) 0.79815(16) 0.0212(8) Uani 1 1 d . . . . .
C6N C 0.8208(3) 0.03379(17) 0.79796(17) 0.0263(8) Uani 1 1 d . . . . .
H6N1 H 0.7604 0.0621 0.7888 0.040 Uiso 1 1 calc R U . . .
H6N2 H 0.8787 0.0525 0.7755 0.040 Uiso 1 1 calc R U . . .
H6N3 H 0.8261 0.0226 0.8388 0.040 Uiso 1 1 calc R U . . .
C55 C 0.7955(3) -0.20552(16) 0.80841(17) 0.0230(8) Uani 1 1 d . . . . .
H7A1 H 0.8141 -0.2228 0.8477 0.028 Uiso 1 1 calc R U . . .
H7A2 H 0.8573 -0.2016 0.7814 0.028 Uiso 1 1 calc R U . . .
C7C C 0.2942(4) 0.1601(2) 0.8984(2) 0.0395(11) Uani 1 1 d . . . . .
H7C1 H 0.2556 0.1996 0.8966 0.047 Uiso 1 1 calc R U . . .
H7C2 H 0.2944 0.1351 0.9392 0.047 Uiso 1 1 calc R U . . .
C1N C 0.7383(4) 0.25712(18) 0.53263(18) 0.0343(10) Uani 1 1 d . . . . .
H7N1 H 0.6660 0.2673 0.5377 0.051 Uiso 1 1 calc R U . . .
H7N2 H 0.7688 0.2938 0.5133 0.051 Uiso 1 1 calc R U . . .
H7N3 H 0.7617 0.2367 0.5701 0.051 Uiso 1 1 calc R U . . .
C56 C 0.7519(4) -0.3514(2) 0.7076(2) 0.0393(11) Uani 1 1 d . . . . .
H8PP H 0.7012 -0.3746 0.7073 0.059 Uiso 0.5 1 calc R U P . .
H8PO H 0.8124 -0.3784 0.7192 0.059 Uiso 0.5 1 calc R U P . .
H8IU H 0.7663 -0.3229 0.6692 0.059 Uiso 0.5 1 calc R U P . .
H8D H 0.8187 -0.3426 0.6898 0.059 Uiso 0.5 1 calc R U P . .
H8E H 0.7076 -0.3389 0.6780 0.059 Uiso 0.5 1 calc R U P . .
H8F H 0.7536 -0.3944 0.7280 0.059 Uiso 0.5 1 calc R U P . .
C8C C -0.2184(4) 0.2121(2) 1.0499(2) 0.0508(13) Uani 1 1 d . . . . .
H8C1 H -0.1565 0.1899 1.0658 0.061 Uiso 1 1 calc R U . . .
H8C2 H -0.2686 0.1843 1.0628 0.061 Uiso 1 1 calc R U . . .
C2N C 0.8762(4) 0.1996(2) 0.4858(2) 0.0503(14) Uani 1 1 d . . . . .
H8N1 H 0.8892 0.1728 0.4631 0.075 Uiso 1 1 calc R U . . .
H8N2 H 0.9035 0.1792 0.5221 0.075 Uiso 1 1 calc R U . . .
H8N3 H 0.9076 0.2357 0.4647 0.075 Uiso 1 1 calc R U . . .
C57 C 0.7610(3) -0.15286(17) 0.93615(16) 0.0241(8) Uani 1 1 d . . . . .
C9C C -0.1821(3) 0.60056(19) 0.89183(18) 0.0310(9) Uani 1 1 d . . . . .
H9C1 H -0.2127 0.5699 0.9251 0.037 Uiso 1 1 calc R U . . .
H9C2 H -0.2361 0.6287 0.8716 0.037 Uiso 1 1 calc R U . . .
C9N C 0.4972(4) 0.2983(2) 1.01461(19) 0.0404(11) Uani 1 1 d . . . . .
H9N1 H 0.4758 0.3266 1.0358 0.061 Uiso 1 1 calc R U . . .
H9N2 H 0.5380 0.3172 0.9789 0.061 Uiso 1 1 calc R U . . .
H9N3 H 0.5361 0.2625 1.0378 0.061 Uiso 1 1 calc R U . . .
C58 C 0.8490(3) -0.18574(19) 0.95937(18) 0.0313(9) Uani 1 1 d . . . . .
H10 H 0.8674 -0.2262 0.9611 0.038 Uiso 1 1 calc R U . . .
C10N C 0.4326(3) 0.24014(18) 0.96606(17) 0.0316(9) Uani 1 1 d . . . . .
H10A H 0.3713 0.2319 0.9579 0.047 Uiso 1 1 calc R U . . .
H10B H 0.4704 0.2025 0.9873 0.047 Uiso 1 1 calc R U . . .
H10C H 0.4724 0.2594 0.9301 0.047 Uiso 1 1 calc R U . . .
C59 C 0.9097(3) -0.1587(2) 0.98010(19) 0.0377(11) Uani 1 1 d . . . . .
H11 H 0.9678 -0.1816 0.9958 0.045 Uiso 1 1 calc R U . . .
C11N C 0.0987(3) 0.47266(18) 0.77891(17) 0.0244(8) Uani 1 1 d . . . . .
H11A H 0.0965 0.4902 0.8088 0.037 Uiso 1 1 calc R U . . .
H11B H 0.0939 0.4298 0.7965 0.037 Uiso 1 1 calc R U . . .
H11C H 0.0432 0.4924 0.7567 0.037 Uiso 1 1 calc R U . . .
C60 C 0.8854(3) -0.0979(2) 0.97784(18) 0.0358(10) Uani 1 1 d . . . . .
C12N C 0.2034(3) 0.45540(17) 0.69245(17) 0.0258(8) Uani 1 1 d . . . . .
H12A H 0.2664 0.4627 0.6679 0.039 Uiso 1 1 calc R U . . .
H12B H 0.1483 0.4745 0.6697 0.039 Uiso 1 1 calc R U . . .
H12C H 0.2009 0.4122 0.7090 0.039 Uiso 1 1 calc R U . . .
C61 C 0.7984(3) -0.0652(2) 0.95306(17) 0.0313(9) Uani 1 1 d . . . . .
H13 H 0.7810 -0.0244 0.9505 0.038 Uiso 1 1 calc R U . . .
C13N C 0.5464(3) 0.45764(17) 0.70232(17) 0.0252(8) Uani 1 1 d . . . . .
H13A H 0.4983 0.4296 0.7112 0.038 Uiso 1 1 calc R U . . .
H13B H 0.6005 0.4390 0.7259 0.038 Uiso 1 1 calc R U . . .
H13C H 0.5732 0.4680 0.6618 0.038 Uiso 1 1 calc R U . . .
C62 C 0.7365(3) -0.09120(17) 0.93199(16) 0.0247(8) Uani 1 1 d . . . . .
C14N C 0.5650(3) 0.55992(17) 0.70008(17) 0.0250(8) Uani 1 1 d . . . . .
H14A H 0.5290 0.5957 0.7082 0.037 Uiso 1 1 calc R U . . .
H14B H 0.5908 0.5706 0.6594 0.037 Uiso 1 1 calc R U . . .
H14C H 0.6202 0.5434 0.7231 0.037 Uiso 1 1 calc R U . . .
C64 C 0.9487(4) -0.0694(2) 1.0026(2) 0.0460(12) Uani 1 1 d . . . . .
H15= H 0.9201 -0.0277 0.9973 0.069 Uiso 1 1 calc R U . . .
H15' H 1.0164 -0.0708 0.9828 0.069 Uiso 1 1 calc R U . . .
H15Y H 0.9500 -0.0916 1.0434 0.069 Uiso 1 1 calc R U . . .
C15N C 0.1494(3) 0.63267(17) 0.82143(17) 0.0254(8) Uani 1 1 d . . . . .
H15A H 0.1076 0.6188 0.8025 0.038 Uiso 1 1 calc R U . . .
H15B H 0.1459 0.6763 0.8049 0.038 Uiso 1 1 calc R U . . .
H15C H 0.1258 0.6215 0.8624 0.038 Uiso 1 1 calc R U . . .
C63 C 0.6448(3) -0.05576(17) 0.90375(16) 0.0240(8) Uani 1 1 d . . . . .
H1JS H 0.5845 -0.0683 0.9299 0.029 Uiso 1 1 calc R U . . .
H1GF H 0.6442 -0.0126 0.8966 0.029 Uiso 1 1 calc R U . . .
C16N C 0.3238(3) 0.62195(17) 0.84252(17) 0.0258(8) Uani 1 1 d . . . . .
H16A H 0.3912 0.6017 0.8367 0.039 Uiso 1 1 calc R U . . .
H16B H 0.3004 0.6105 0.8835 0.039 Uiso 1 1 calc R U . . .
H16C H 0.3238 0.6653 0.8267 0.039 Uiso 1 1 calc R U . . .
C65 C 0.4187(3) -0.11131(16) 0.90153(16) 0.0204(8) Uani 1 1 d . . . . .
C66 C 0.3582(3) -0.08682(17) 0.94222(17) 0.0256(8) Uani 1 1 d . . . . .
H18 H 0.3827 -0.0912 0.9765 0.031 Uiso 1 1 calc R U . . .
C67 C 0.2618(3) -0.05601(19) 0.93200(18) 0.0310(9) Uani 1 1 d . . . . .
H19 H 0.2227 -0.0407 0.9600 0.037 Uiso 1 1 calc R U . . .
C68 C 0.2222(3) -0.04745(18) 0.88106(18) 0.0280(9) Uani 1 1 d . . . . .
C69 C 0.2844(3) -0.07083(17) 0.84028(16) 0.0228(8) Uani 1 1 d . . . . .
H21 H 0.2604 -0.0650 0.8055 0.027 Uiso 1 1 calc R U . . .
C70 C 0.3808(3) -0.10251(16) 0.84932(16) 0.0206(8) Uani 1 1 d . . . . .
C72 C 0.1172(3) -0.0149(2) 0.8702(2) 0.0413(11) Uani 1 1 d . . . . .
H23A H 0.1041 -0.0137 0.8329 0.062 Uiso 0.5 1 calc R U P . .
H23B H 0.1120 0.0260 0.8706 0.062 Uiso 0.5 1 calc R U P . .
H23C H 0.0687 -0.0363 0.9002 0.062 Uiso 0.5 1 calc R U P . .
H23D H 0.0858 -0.0023 0.9029 0.062 Uiso 0.5 1 calc R U P . .
H23E H 0.0778 -0.0420 0.8652 0.062 Uiso 0.5 1 calc R U P . .
H23F H 0.1212 0.0203 0.8356 0.062 Uiso 0.5 1 calc R U P . .
C71 C 0.4474(3) -0.12803(17) 0.80555(16) 0.0209(8) Uani 1 1 d . . . . .
H24A H 0.4527 -0.1722 0.8202 0.025 Uiso 1 1 calc R U . . .
H24B H 0.4172 -0.1134 0.7695 0.025 Uiso 1 1 calc R U . . .
C25 C 0.7745(3) 0.02366(16) 0.53208(15) 0.0196(8) Uani 1 1 d . . . . .
C26 C 0.8522(3) 0.00273(18) 0.49550(16) 0.0260(8) Uani 1 1 d . . . . .
H26 H 0.9144 0.0170 0.4877 0.031 Uiso 1 1 calc R U . . .
C27 C 0.8386(3) -0.03873(19) 0.47067(18) 0.0308(9) Uani 1 1 d . . . . .
H27 H 0.8923 -0.0524 0.4471 0.037 Uiso 1 1 calc R U . . .
C28 C 0.7466(3) -0.06042(18) 0.48005(17) 0.0289(9) Uani 1 1 d . . . . .
C29 C 0.6695(3) -0.04026(16) 0.51736(16) 0.0231(8) Uani 1 1 d . . . . .
H29 H 0.6076 -0.0548 0.5250 0.028 Uiso 1 1 calc R U . . .
C30 C 0.6816(3) 0.00053(16) 0.54349(15) 0.0193(7) Uani 1 1 d . . . . .
C31 C 0.5999(3) 0.02076(16) 0.58493(15) 0.0195(7) Uani 1 1 d . . . . .
H31A H 0.5720 0.0628 0.5662 0.023 Uiso 1 1 calc R U . . .
H31B H 0.5459 -0.0042 0.5949 0.023 Uiso 1 1 calc R U . . .
C32 C 0.7289(4) -0.1034(2) 0.4511(2) 0.0405(11) Uani 1 1 d . . . . .
H32A H 0.6611 -0.1130 0.4632 0.061 Uiso 0.5 1 calc R U P . .
H32B H 0.7759 -0.1402 0.4621 0.061 Uiso 0.5 1 calc R U P . .
H32C H 0.7387 -0.0843 0.4095 0.061 Uiso 0.5 1 calc R U P . .
H32D H 0.7894 -0.1120 0.4267 0.061 Uiso 0.5 1 calc R U P . .
H32E H 0.6745 -0.0848 0.4278 0.061 Uiso 0.5 1 calc R U P . .
H32F H 0.7118 -0.1407 0.4804 0.061 Uiso 0.5 1 calc R U P . .
C33 C 0.5533(3) 0.16022(15) 0.61060(16) 0.0196(8) Uani 1 1 d . . . . .
C34 C 0.4705(3) 0.17904(16) 0.57977(17) 0.0229(8) Uani 1 1 d . . . . .
H34 H 0.4764 0.1756 0.5429 0.028 Uiso 1 1 calc R U . . .
C35 C 0.3786(3) 0.20303(16) 0.60378(18) 0.0258(8) Uani 1 1 d . . . . .
H35 H 0.3237 0.2156 0.5826 0.031 Uiso 1 1 calc R U . . .
C36 C 0.3670(3) 0.20870(17) 0.65843(18) 0.0263(9) Uani 1 1 d . . . . .
C37 C 0.4511(3) 0.18888(16) 0.68940(17) 0.0231(8) Uani 1 1 d . . . . .
H37 H 0.4448 0.1923 0.7263 0.028 Uiso 1 1 calc R U . . .
C38 C 0.5435(3) 0.16425(15) 0.66658(16) 0.0198(8) Uani 1 1 d . . . . .
C39 C 0.2673(3) 0.2352(2) 0.6841(2) 0.0363(10) Uani 1 1 d . . . . .
H39A H 0.2736 0.2354 0.7221 0.054 Uiso 0.5 1 calc R U P . .
H39B H 0.2161 0.2108 0.6873 0.054 Uiso 0.5 1 calc R U P . .
H39C H 0.2488 0.2762 0.6593 0.054 Uiso 0.5 1 calc R U P . .
H39D H 0.2188 0.2462 0.6570 0.054 Uiso 0.5 1 calc R U P . .
H39E H 0.2763 0.2708 0.6918 0.054 Uiso 0.5 1 calc R U P . .
H39F H 0.2435 0.2054 0.7198 0.054 Uiso 0.5 1 calc R U P . .
C40 C 0.6340(3) 0.13844(16) 0.69970(16) 0.0205(8) Uani 1 1 d . . . . .
H40A H 0.6870 0.1641 0.6817 0.025 Uiso 1 1 calc R U . . .
H40B H 0.6150 0.1384 0.7395 0.025 Uiso 1 1 calc R U . . .
C41 C 0.9020(3) 0.11374(17) 0.64372(16) 0.0238(8) Uani 1 1 d . . . . .
C42 C 0.9321(3) 0.15961(18) 0.6576(2) 0.0344(10) Uani 1 1 d . . . . .
H42 H 0.8922 0.1975 0.6505 0.041 Uiso 1 1 calc R U . . .
C43 C 1.0204(3) 0.1492(2) 0.6819(2) 0.0433(12) Uani 1 1 d . . . . .
H43 H 1.0389 0.1802 0.6913 0.052 Uiso 1 1 calc R U . . .
C44 C 1.0822(3) 0.0935(2) 0.6927(2) 0.0409(12) Uani 1 1 d . . . . .
C45 C 1.0508(3) 0.04777(19) 0.68051(18) 0.0308(9) Uani 1 1 d . . . . .
H45 H 1.0905 0.0098 0.6885 0.037 Uiso 1 1 calc R U . . .
C46 C 0.9614(3) 0.05638(17) 0.65658(16) 0.0226(8) Uani 1 1 d . . . . .
C47 C 0.9250(3) 0.00639(17) 0.64423(17) 0.0234(8) Uani 1 1 d . . . . .
H47A H 0.9342 0.0142 0.6025 0.028 Uiso 1 1 calc R U . . .
H47B H 0.9650 -0.0324 0.6623 0.028 Uiso 1 1 calc R U . . .
C48 C 1.1822(4) 0.0843(2) 0.7165(3) 0.0558(16) Uani 1 1 d . . . . .
H48A H 1.1909 0.1210 0.7222 0.084 Uiso 0.5 1 calc R U P . .
H48B H 1.2368 0.0744 0.6892 0.084 Uiso 0.5 1 calc R U P . .
H48C H 1.1821 0.0514 0.7531 0.084 Uiso 0.5 1 calc R U P . .
H48D H 1.2156 0.0436 0.7208 0.084 Uiso 0.5 1 calc R U P . .
H48E H 1.1697 0.0902 0.7538 0.084 Uiso 0.5 1 calc R U P . .
H48F H 1.2245 0.1132 0.6899 0.084 Uiso 0.5 1 calc R U P . .
C9 C 0.8007(3) 0.25080(16) 0.33335(16) 0.0213(8) Uani 1 1 d . . . . .
C10 C 0.8916(3) 0.21394(16) 0.32487(17) 0.0237(8) Uani 1 1 d . . . . .
H50 H 0.9440 0.2098 0.3462 0.028 Uiso 1 1 calc R U . . .
C11 C 0.9039(3) 0.18359(18) 0.28487(18) 0.0280(9) Uani 1 1 d . . . . .
H51 H 0.9648 0.1592 0.2796 0.034 Uiso 1 1 calc R U . . .
C12 C 0.8271(3) 0.18891(17) 0.25244(18) 0.0275(9) Uani 1 1 d . . . . .
C13 C 0.7371(3) 0.22535(16) 0.26150(17) 0.0236(8) Uani 1 1 d . . . . .
H53 H 0.6846 0.2288 0.2405 0.028 Uiso 1 1 calc R U . . .
C14 C 0.7227(3) 0.25686(16) 0.30092(16) 0.0216(8) Uani 1 1 d . . . . .
C15 C 0.6281(3) 0.29903(16) 0.31048(17) 0.0225(8) Uani 1 1 d . . . . .
H55A H 0.5825 0.3032 0.2828 0.027 Uiso 1 1 calc R U . . .
H55B H 0.5940 0.2817 0.3495 0.027 Uiso 1 1 calc R U . . .
C16 C 0.8422(4) 0.1553(2) 0.2091(2) 0.0385(11) Uani 1 1 d . . . . .
H56A H 0.7824 0.1645 0.1902 0.058 Uiso 1 1 calc R U . . .
H56B H 0.8547 0.1122 0.2291 0.058 Uiso 1 1 calc R U . . .
H56C H 0.8989 0.1679 0.1805 0.058 Uiso 1 1 calc R U . . .
C17 C 0.8788(3) 0.39093(16) 0.40715(16) 0.0228(8) Uani 1 1 d . . . . .
C18 C 0.8969(3) 0.41425(18) 0.44838(18) 0.0290(9) Uani 1 1 d . . . . .
H58 H 0.8524 0.4098 0.4825 0.035 Uiso 1 1 calc R U . . .
C19 C 0.9802(3) 0.4440(2) 0.4392(2) 0.0367(10) Uani 1 1 d . . . . .
H59 H 0.9908 0.4588 0.4676 0.044 Uiso 1 1 calc R U . . .
C20 C 1.0481(3) 0.45226(19) 0.3888(2) 0.0358(10) Uani 1 1 d . . . . .
C21 C 1.0283(3) 0.43012(18) 0.34762(18) 0.0271(9) Uani 1 1 d . . . . .
H61 H 1.0716 0.4363 0.3129 0.033 Uiso 1 1 calc R U . . .
C22 C 0.9471(3) 0.39924(16) 0.35563(16) 0.0227(8) Uani 1 1 d . . . . .
C23 C 0.9265(3) 0.37441(17) 0.31118(16) 0.0219(8) Uani 1 1 d . . . . .
H63A H 0.9716 0.3890 0.2755 0.026 Uiso 1 1 calc R U . . .
H63B H 0.9403 0.3302 0.3256 0.026 Uiso 1 1 calc R U . . .
C24 C 1.1418(4) 0.4829(2) 0.3792(2) 0.0488(12) Uani 1 1 d . . . . .
H64A H 1.1792 0.4841 0.3420 0.073 Uiso 1 1 calc R U . . .
H64B H 1.1835 0.4603 0.4095 0.073 Uiso 1 1 calc R U . . .
H64C H 1.1217 0.5238 0.3800 0.073 Uiso 1 1 calc R U . . .
C1 C 0.5395(3) 0.35588(17) 0.43870(15) 0.0236(8) Uani 1 1 d . . . . .
C2 C 0.4553(3) 0.32518(19) 0.46337(18) 0.0320(9) Uani 1 1 d . . . . .
H66 H 0.4585 0.2850 0.4650 0.038 Uiso 1 1 calc R U . . .
C3 C 0.3663(3) 0.3545(2) 0.48551(19) 0.0395(11) Uani 1 1 d . . . . .
H67 H 0.3114 0.3331 0.5020 0.047 Uiso 1 1 calc R U . . .
C4 C 0.3574(3) 0.4145(2) 0.48363(18) 0.0370(11) Uani 1 1 d . . . . .
C5 C 0.4411(3) 0.4452(2) 0.45690(17) 0.0318(9) Uani 1 1 d . . . . .
H69 H 0.4366 0.4859 0.4539 0.038 Uiso 1 1 calc R U . . .
C6 C 0.5309(3) 0.41718(17) 0.43458(15) 0.0243(8) Uani 1 1 d . . . . .
C7 C 0.6195(3) 0.45120(17) 0.40532(16) 0.0253(8) Uani 1 1 d . . . . .
H71A H 0.5982 0.4946 0.3975 0.030 Uiso 1 1 calc R U . . .
H71B H 0.6715 0.4383 0.4312 0.030 Uiso 1 1 calc R U . . .
C8 C 0.2628(4) 0.4450(3) 0.5099(2) 0.0506(14) Uani 1 1 d . . . . .
H72A H 0.2712 0.4862 0.5044 0.076 Uiso 0.5 1 calc R U P . .
H72B H 0.2506 0.4230 0.5509 0.076 Uiso 0.5 1 calc R U P . .
H72C H 0.2064 0.4454 0.4912 0.076 Uiso 0.5 1 calc R U P . .
H72D H 0.2143 0.4168 0.5266 0.076 Uiso 0.5 1 calc R U P . .
H72E H 0.2349 0.4801 0.4801 0.076 Uiso 0.5 1 calc R U P . .
H72F H 0.2791 0.4577 0.5397 0.076 Uiso 0.5 1 calc R U P . .
C73 C 0.3079(3) 0.47492(16) 0.96613(15) 0.0197(8) Uani 1 1 d . . . . .
C74 C 0.3488(3) 0.49675(18) 1.00171(16) 0.0247(8) Uani 1 1 d . . . . .
H74 H 0.4156 0.4831 1.0091 0.030 Uiso 1 1 calc R U . . .
C75 C 0.2903(3) 0.53886(19) 1.02625(17) 0.0295(9) Uani 1 1 d . . . . .
H75 H 0.3189 0.5529 1.0497 0.035 Uiso 1 1 calc R U . . .
C76 C 0.1907(3) 0.56020(17) 1.01647(17) 0.0264(9) Uani 1 1 d . . . . .
C77 C 0.1519(3) 0.53939(17) 0.97974(16) 0.0232(8) Uani 1 1 d . . . . .
H77 H 0.0854 0.5538 0.9720 0.028 Uiso 1 1 calc R U . . .
C78 C 0.2084(3) 0.49785(16) 0.95415(15) 0.0188(7) Uani 1 1 d . . . . .
C79 C 0.1671(3) 0.47660(17) 0.91328(15) 0.0192(7) Uani 1 1 d . . . . .
H79A H 0.1552 0.4345 0.9324 0.023 Uiso 1 1 calc R U . . .
H79B H 0.1031 0.5013 0.9031 0.023 Uiso 1 1 calc R U . . .
C80 C 0.1262(3) 0.6040(2) 1.0447(2) 0.0368(10) Uani 1 1 d . . . . .
H80A H 0.0602 0.6142 1.0322 0.055 Uiso 1 1 calc R U . . .
H80B H 0.1571 0.6405 1.0336 0.055 Uiso 1 1 calc R U . . .
H80C H 0.1204 0.5853 1.0864 0.055 Uiso 1 1 calc R U . . .
C81 C 0.2309(3) 0.33831(15) 0.88649(16) 0.0188(7) Uani 1 1 d . . . . .
C82 C 0.1381(3) 0.32009(16) 0.91525(17) 0.0241(8) Uani 1 1 d . . . . .
H82 H 0.1149 0.3238 0.9518 0.029 Uiso 1 1 calc R U . . .
C83 C 0.0800(3) 0.29647(17) 0.88996(19) 0.0283(9) Uani 1 1 d . . . . .
H83 H 0.0183 0.2845 0.9100 0.034 Uiso 1 1 calc R U . . .
C84 C 0.1111(3) 0.29014(17) 0.83548(19) 0.0280(9) Uani 1 1 d . . . . .
C85 C 0.2037(3) 0.30919(16) 0.80679(17) 0.0232(8) Uani 1 1 d . . . . .
H85 H 0.2262 0.3056 0.7702 0.028 Uiso 1 1 calc R U . . .
C86 C 0.2633(3) 0.33331(15) 0.83095(16) 0.0200(8) Uani 1 1 d . . . . .
C87 C 0.3599(3) 0.35801(16) 0.79942(16) 0.0197(7) Uani 1 1 d . . . . .
H87A H 0.4167 0.3324 0.8188 0.024 Uiso 1 1 calc R U . . .
H87B H 0.3697 0.3573 0.7598 0.024 Uiso 1 1 calc R U . . .
C88 C 0.0476(3) 0.2639(2) 0.8084(2) 0.0391(11) Uani 1 1 d . . . . .
H88A H -0.0129 0.2535 0.8344 0.059 Uiso 1 1 calc R U . . .
H88B H 0.0854 0.2280 0.8015 0.059 Uiso 1 1 calc R U . . .
H88C H 0.0299 0.2936 0.7721 0.059 Uiso 1 1 calc R U . . .
C89 C 0.5721(3) 0.38598(16) 0.85892(15) 0.0192(7) Uani 1 1 d . . . . .
C90 C 0.6459(3) 0.33941(17) 0.84900(17) 0.0252(8) Uani 1 1 d . . . . .
H90 H 0.6289 0.3006 0.8573 0.030 Uiso 1 1 calc R U . . .
C91 C 0.7441(3) 0.35088(18) 0.82686(19) 0.0312(9) Uani 1 1 d . . . . .
H91 H 0.7923 0.3194 0.8206 0.037 Uiso 1 1 calc R U . . .
C92 C 0.7726(3) 0.40823(18) 0.81372(18) 0.0269(9) Uani 1 1 d . . . . .
C93 C 0.6984(3) 0.45376(17) 0.82341(16) 0.0215(8) Uani 1 1 d . . . . .
H93 H 0.7157 0.4925 0.8148 0.026 Uiso 1 1 calc R U . . .
C94 C 0.5991(3) 0.44396(16) 0.84548(15) 0.0185(7) Uani 1 1 d . . . . .
C95 C 0.5188(3) 0.49403(16) 0.85508(16) 0.0206(8) Uani 1 1 d . . . . .
H95A H 0.5032 0.4877 0.8965 0.025 Uiso 1 1 calc R U . . .
H95B H 0.5440 0.5330 0.8364 0.025 Uiso 1 1 calc R U . . .
C96 C 0.8803(3) 0.4204(2) 0.7908(2) 0.0378(11) Uani 1 1 d . . . . .
H96A H 0.8850 0.4624 0.7844 0.057 Uiso 1 1 calc R U . . .
H96B H 0.9000 0.4122 0.7547 0.057 Uiso 1 1 calc R U . . .
H96C H 0.9244 0.3945 0.8188 0.057 Uiso 1 1 calc R U . . .
N4 N 0.7033(2) -0.10707(14) 0.68445(13) 0.0214(7) Uani 1 1 d . . . . .
H4B H 0.6861 -0.0630 0.6698 0.026 Uiso 1 1 calc R U . . .
H4A H 0.7061 -0.1192 0.7260 0.026 Uiso 1 1 calc R U . . .
N2 N 0.5111(2) 0.01608(13) 0.75662(13) 0.0214(7) Uani 1 1 d . . . . .
H2A H 0.5699 0.0349 0.7344 0.026 Uiso 1 1 calc R U . . .
H2B H 0.5326 -0.0273 0.7738 0.026 Uiso 1 1 calc R U . . .
N3 N 0.8163(2) -0.02158(13) 0.78383(13) 0.0205(6) Uani 1 1 d . . . . .
H3A H 0.7563 -0.0395 0.8055 0.025 Uiso 1 1 calc R U . . .
H3B H 0.8108 -0.0100 0.7426 0.025 Uiso 1 1 calc R U . . .
N1 N 0.7663(3) 0.21682(15) 0.49727(14) 0.0293(8) Uani 1 1 d . . . . .
H1B H 0.7394 0.2371 0.4603 0.035 Uiso 1 1 calc R U . . .
H1A H 0.7350 0.1800 0.5171 0.035 Uiso 1 1 calc R U . . .
N5 N 0.4076(2) 0.28111(14) 1.00134(14) 0.0265(7) Uani 1 1 d . . . . .
H5A H 0.3661 0.3179 0.9806 0.032 Uiso 1 1 calc R U . . .
H5B H 0.3680 0.2611 1.0377 0.032 Uiso 1 1 calc R U . . .
N6 N 0.1951(2) 0.48126(13) 0.73998(13) 0.0200(6) Uani 1 1 d . . . . .
H6A H 0.2509 0.4618 0.7627 0.024 Uiso 1 1 calc R U . . .
H6B H 0.2003 0.5245 0.7230 0.024 Uiso 1 1 calc R U . . .
N7 N 0.4956(2) 0.51386(13) 0.71482(13) 0.0202(6) Uani 1 1 d . . . . .
H7A H 0.4387 0.5313 0.6926 0.024 Uiso 1 1 calc R U . . .
H7B H 0.4696 0.5033 0.7559 0.024 Uiso 1 1 calc R U . . .
N8 N 0.2560(2) 0.60391(13) 0.81284(13) 0.0207(6) Uani 1 1 d . . . . .
H8A H 0.2585 0.5599 0.8278 0.025 Uiso 1 1 calc R U . . .
H8B H 0.2797 0.6157 0.7714 0.025 Uiso 1 1 calc R U . . .
O13 O 0.60315(19) -0.22504(11) 0.86844(11) 0.0208(5) Uani 1 1 d . . . . .
O14 O 0.73813(18) -0.14663(10) 0.80083(10) 0.0188(5) Uani 1 1 d . . . . .
O15 O 0.70162(19) -0.18170(11) 0.91938(11) 0.0228(6) Uani 1 1 d . . . . .
O16 O 0.64388(19) -0.06528(11) 0.84981(10) 0.0200(5) Uani 1 1 d . . . . .
O17 O 0.50954(19) -0.14311(11) 0.91321(10) 0.0215(5) Uani 1 1 d . . . . .
O18 O 0.54587(18) -0.11034(11) 0.79431(10) 0.0185(5) Uani 1 1 d . . . . .
O7 O 0.78835(18) 0.06606(11) 0.55323(10) 0.0211(5) Uani 1 1 d . . . . .
O8 O 0.63789(18) 0.01589(11) 0.63687(10) 0.0184(5) Uani 1 1 d . . . . .
O9 O 0.64285(17) 0.13849(10) 0.58578(10) 0.0185(5) Uani 1 1 d . . . . .
O10 O 0.67127(18) 0.07770(10) 0.70007(10) 0.0189(5) Uani 1 1 d . . . . .
O11 O 0.81844(18) 0.12637(11) 0.61719(11) 0.0202(5) Uani 1 1 d . . . . .
O12 O 0.82025(18) 0.00289(11) 0.66632(10) 0.0197(5) Uani 1 1 d . . . . .
O3 O 0.78865(19) 0.27862(11) 0.37350(11) 0.0226(6) Uani 1 1 d . . . . .
O4 O 0.65170(18) 0.35777(10) 0.30346(10) 0.0197(5) Uani 1 1 d . . . . .
O5 O 0.79976(19) 0.36051(11) 0.41783(11) 0.0236(6) Uani 1 1 d . . . . .
O6 O 0.82420(18) 0.39246(11) 0.29893(10) 0.0199(5) Uani 1 1 d . . . . .
O1 O 0.62677(19) 0.32485(11) 0.42188(11) 0.0236(6) Uani 1 1 d . . . . .
O2 O 0.66022(18) 0.44016(11) 0.35195(10) 0.0204(5) Uani 1 1 d . . . . .
O19 O 0.36442(18) 0.43162(11) 0.94553(10) 0.0203(5) Uani 1 1 d . . . . .
O20 O 0.23723(17) 0.48144(10) 0.86116(10) 0.0172(5) Uani 1 1 d . . . . .
O21 O 0.28888(17) 0.35897(10) 0.91229(10) 0.0180(5) Uani 1 1 d . . . . .
O22 O 0.35629(17) 0.41934(10) 0.79849(10) 0.0168(5) Uani 1 1 d . . . . .
O23 O 0.47879(17) 0.37224(10) 0.88277(10) 0.0186(5) Uani 1 1 d . . . . .
O24 O 0.42899(17) 0.49532(10) 0.83194(10) 0.0174(5) Uani 1 1 d . . . . .
Cl1 Cl 1.10864(14) 0.26214(8) 0.52960(7) 0.0821(5) Uani 1 1 d . . . . .
Cl2 Cl 1.13851(13) 0.23144(7) 0.42395(7) 0.0660(4) Uani 1 1 d . . . . .
Cl3 Cl 0.57644(11) 0.14108(6) 0.41807(6) 0.0587(4) Uani 1 1 d . . . . .
Cl4 Cl 0.66553(10) 0.06580(6) 0.34580(5) 0.0463(3) Uani 1 1 d . . . . .
Cl5 Cl 0.41353(9) 0.36585(5) 0.63578(5) 0.0396(3) Uani 1 1 d . . . . .
Cl6 Cl 0.62588(12) 0.37131(10) 0.59000(12) 0.1062(8) Uani 1 1 d . . . . .
C5C C 0.7075(7) 0.2848(5) 0.7219(4) 0.051(3) Uani 0.5 1 d D . P . .
H5C3 H 0.7127 0.3247 0.7232 0.061 Uiso 0.5 1 calc R U P . .
H5C4 H 0.7160 0.2877 0.6812 0.061 Uiso 0.5 1 calc R U P . .
Cl9 Cl 0.5906(2) 0.26696(13) 0.75241(14) 0.0594(7) Uani 0.5 1 d D . P . .
Cl10 Cl 0.8060(2) 0.23215(12) 0.75581(11) 0.0525(6) Uani 0.5 1 d D . P . .
Ge3 Ge 0.62398(3) -0.14417(2) 0.85641(2) 0.01740(9) Uani 1 1 d . . . . .
C6C C 0.7612(8) 0.1473(5) 0.9044(4) 0.056(3) Uani 0.5 1 d D . P A 1
H6C1 H 0.7555 0.1433 0.9452 0.067 Uiso 0.5 1 calc R U P A 1
H6C2 H 0.7523 0.1905 0.8821 0.067 Uiso 0.5 1 calc R U P A 1
Cl11 Cl 0.6644(3) 0.11409(19) 0.89444(16) 0.0652(9) Uani 0.5 1 d D . P A 1
Cl12 Cl 0.8847(5) 0.1147(2) 0.8830(2) 0.0631(13) Uani 0.5 1 d D . P A 1
C6C' C 0.8034(11) 0.1736(7) 0.8337(10) 0.147(10) Uani 0.5 1 d D . P B 2
H6C3 H 0.8151 0.1738 0.7937 0.176 Uiso 0.5 1 calc R U P B 2
H6C4 H 0.8066 0.2143 0.8334 0.176 Uiso 0.5 1 calc R U P B 2
Cl1A Cl 0.6838(5) 0.1512(3) 0.8671(4) 0.152(3) Uani 0.5 1 d D . P B 2
Cl1B Cl 0.8933(10) 0.1216(5) 0.8736(6) 0.185(6) Uani 0.5 1 d D . P B 2
Cl13 Cl 0.41817(13) 0.16952(10) 0.86595(9) 0.0888(6) Uani 1 1 d . . . . .
Cl14 Cl 0.23734(10) 0.12505(6) 0.86220(6) 0.0497(3) Uani 1 1 d . . . . .
Cl15 Cl -0.19587(13) 0.23701(7) 0.97425(6) 0.0673(4) Uani 1 1 d . . . . .
Cl16 Cl -0.26122(12) 0.27286(6) 1.07694(7) 0.0639(4) Uani 1 1 d . . . . .
Cl17 Cl -0.10433(9) 0.56492(5) 0.84464(5) 0.0433(3) Uani 1 1 d . . . . .
Cl18 Cl -0.11274(11) 0.64060(6) 0.91654(6) 0.0564(3) Uani 1 1 d . . . . .
C4C C 0.9478(16) 0.3360(10) 0.6240(8) 0.20(2) Uani 0.430(5) 1 d D . P C 1
H4C3 H 0.9186 0.3588 0.5881 0.244 Uiso 0.430(5) 1 calc R U P C 1
H4C4 H 0.9755 0.2955 0.6227 0.244 Uiso 0.430(5) 1 calc R U P C 1
Cl7 Cl 0.8561(3) 0.3302(2) 0.6814(2) 0.0808(16) Uani 0.430(5) 1 d D . P C 1
Cl8 Cl 1.0438(9) 0.3719(6) 0.6287(7) 0.155(6) Uani 0.430(5) 1 d D . P C 1
C4C' C 0.9931(10) 0.3226(6) 0.6430(6) 0.072(4) Uani 0.570(5) 1 d D . P C 2
H4C5 H 1.0394 0.2950 0.6258 0.086 Uiso 0.570(5) 1 calc R U P C 2
H4C6 H 0.9730 0.2998 0.6835 0.086 Uiso 0.570(5) 1 calc R U P C 2
Cl7' Cl 0.8880(3) 0.34908(17) 0.60672(16) 0.0837(13) Uani 0.570(5) 1 d D . P C
2
Cl8' Cl 1.0539(4) 0.3824(2) 0.6392(3) 0.0728(13) Uani 0.570(5) 1 d D . P C 2
Ge2 Ge 0.72997(3) 0.06974(2) 0.62749(2) 0.01623(9) Uani 1 1 d . . . . .
Ge1 Ge 0.72452(3) 0.36023(2) 0.36003(2) 0.01821(9) Uani 1 1 d . . . . .
Ge4 Ge 0.35869(3) 0.42794(2) 0.87129(2) 0.01487(9) 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
C49 O13 1.340(4) . ?
C49 C50 1.399(5) . ?
C49 C54 1.399(5) . ?
C1C Cl1 1.717(6) . ?
C1C Cl2 1.761(5) . ?
C1C H1C1 0.9700 . ?
C1C H1C2 0.9700 . ?
C7N N4 1.485(5) . ?
C7N H1N1 0.9600 . ?
C7N H1N2 0.9600 . ?
C7N H1N3 0.9600 . ?
C50 C51 1.378(5) . ?
C50 H2 0.9300 . ?
C2C Cl3 1.757(5) . ?
C2C Cl4 1.764(4) . ?
C2C H2C1 0.9700 . ?
C2C H2C2 0.9700 . ?
C8N N4 1.481(5) . ?
C8N H2N1 0.9600 . ?
C8N H2N2 0.9600 . ?
C8N H2N3 0.9600 . ?
C51 C52 1.397(5) . ?
C51 H3 0.9300 . ?
C3C Cl6 1.739(5) . ?
C3C Cl5 1.761(4) . ?
C3C H3C1 0.9700 . ?
C3C H3C2 0.9700 . ?
C3N N2 1.481(5) . ?
C3N H3N1 0.9600 . ?
C3N H3N2 0.9600 . ?
C3N H3N3 0.9600 . ?
C52 C53 1.388(5) . ?
C52 C56 1.504(5) . ?
C4N N2 1.483(5) . ?
C4N H4N1 0.9600 . ?
C4N H4N2 0.9600 . ?
C4N H4N3 0.9600 . ?
C53 C54 1.384(5) . ?
C53 H5 0.9300 . ?
C5N N3 1.477(5) . ?
C5N H5N1 0.9600 . ?
C5N H5N2 0.9600 . ?
C5N H5N3 0.9600 . ?
C54 C55 1.508(5) . ?
C6N N3 1.484(5) . ?
C6N H6N1 0.9600 . ?
C6N H6N2 0.9600 . ?
C6N H6N3 0.9600 . ?
C55 O14 1.427(4) . ?
C55 H7A1 0.9700 . ?
C55 H7A2 0.9700 . ?
C7C Cl13 1.746(5) . ?
C7C Cl14 1.762(5) . ?
C7C H7C1 0.9700 . ?
C7C H7C2 0.9700 . ?
C1N N1 1.466(5) . ?
C1N H7N1 0.9600 . ?
C1N H7N2 0.9600 . ?
C1N H7N3 0.9600 . ?
C56 H8PP 0.9600 . ?
C56 H8PO 0.9600 . ?
C56 H8IU 0.9600 . ?
C56 H8D 0.9600 . ?
C56 H8E 0.9600 . ?
C56 H8F 0.9600 . ?
C8C Cl15 1.738(5) . ?
C8C Cl16 1.752(5) . ?
C8C H8C1 0.9700 . ?
C8C H8C2 0.9700 . ?
C2N N1 1.473(5) . ?
C2N H8N1 0.9600 . ?
C2N H8N2 0.9600 . ?
C2N H8N3 0.9600 . ?
C57 O15 1.348(5) . ?
C57 C58 1.392(6) . ?
C57 C62 1.403(5) . ?
C9C Cl17 1.760(4) . ?
C9C Cl18 1.764(4) . ?
C9C H9C1 0.9700 . ?
C9C H9C2 0.9700 . ?
C9N N5 1.475(5) . ?
C9N H9N1 0.9600 . ?
C9N H9N2 0.9600 . ?
C9N H9N3 0.9600 . ?
C58 C59 1.391(6) . ?
C58 H10 0.9300 . ?
C10N N5 1.477(5) . ?
C10N H10A 0.9600 . ?
C10N H10B 0.9600 . ?
C10N H10C 0.9600 . ?
C59 C60 1.395(7) . ?
C59 H11 0.9300 . ?
C11N N6 1.477(5) . ?
C11N H11A 0.9600 . ?
C11N H11B 0.9600 . ?
C11N H11C 0.9600 . ?
C60 C61 1.396(6) . ?
C60 C64 1.506(6) . ?
C12N N6 1.483(5) . ?
C12N H12A 0.9600 . ?
C12N H12B 0.9600 . ?
C12N H12C 0.9600 . ?
C61 C62 1.392(6) . ?
C61 H13 0.9300 . ?
C13N N7 1.484(5) . ?
C13N H13A 0.9600 . ?
C13N H13B 0.9600 . ?
C13N H13C 0.9600 . ?
C62 C63 1.496(5) . ?
C14N N7 1.480(5) . ?
C14N H14A 0.9600 . ?
C14N H14B 0.9600 . ?
C14N H14C 0.9600 . ?
C64 H15= 0.9600 . ?
C64 H15' 0.9600 . ?
C64 H15Y 0.9600 . ?
C15N N8 1.489(5) . ?
C15N H15A 0.9600 . ?
C15N H15B 0.9600 . ?
C15N H15C 0.9600 . ?
C63 O16 1.431(4) . ?
C63 H1JS 0.9700 . ?
C63 H1GF 0.9700 . ?
C16N N8 1.477(5) . ?
C16N H16A 0.9600 . ?
C16N H16B 0.9600 . ?
C16N H16C 0.9600 . ?
C65 O17 1.338(4) . ?
C65 C66 1.398(5) . ?
C65 C70 1.408(5) . ?
C66 C67 1.390(6) . ?
C66 H18 0.9300 . ?
C67 C68 1.392(6) . ?
C67 H19 0.9300 . ?
C68 C69 1.394(5) . ?
C68 C72 1.506(6) . ?
C69 C70 1.391(5) . ?
C69 H21 0.9300 . ?
C70 C71 1.501(5) . ?
C72 H23A 0.9600 . ?
C72 H23B 0.9600 . ?
C72 H23C 0.9600 . ?
C72 H23D 0.9600 . ?
C72 H23E 0.9600 . ?
C72 H23F 0.9600 . ?
C71 O18 1.426(4) . ?
C71 H24A 0.9700 . ?
C71 H24B 0.9700 . ?
C25 O7 1.339(4) . ?
C25 C26 1.396(5) . ?
C25 C30 1.411(5) . ?
C26 C27 1.381(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.389(6) . ?
C27 H27 0.9300 . ?
C28 C29 1.394(5) . ?
C28 C32 1.507(6) . ?
C29 C30 1.383(5) . ?
C29 H29 0.9300 . ?
C30 C31 1.497(5) . ?
C31 O8 1.428(4) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C32 H32D 0.9600 . ?
C32 H32E 0.9600 . ?
C32 H32F 0.9600 . ?
C33 O9 1.353(4) . ?
C33 C34 1.386(5) . ?
C33 C38 1.401(5) . ?
C34 C35 1.389(5) . ?
C34 H34 0.9300 . ?
C35 C36 1.382(6) . ?
C35 H35 0.9300 . ?
C36 C37 1.401(5) . ?
C36 C39 1.508(5) . ?
C37 C38 1.389(5) . ?
C37 H37 0.9300 . ?
C38 C40 1.508(5) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C39 H39D 0.9600 . ?
C39 H39E 0.9600 . ?
C39 H39F 0.9600 . ?
C40 O10 1.427(4) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 O11 1.344(4) . ?
C41 C42 1.394(6) . ?
C41 C46 1.401(5) . ?
C42 C43 1.379(6) . ?
C42 H42 0.9300 . ?
C43 C44 1.386(7) . ?
C43 H43 0.9300 . ?
C44 C45 1.377(6) . ?
C44 C48 1.522(6) . ?
C45 C46 1.393(5) . ?
C45 H45 0.9300 . ?
C46 C47 1.505(5) . ?
C47 O12 1.434(4) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C48 H48D 0.9600 . ?
C48 H48E 0.9600 . ?
C48 H48F 0.9600 . ?
C9 O3 1.344(4) . ?
C9 C10 1.397(5) . ?
C9 C14 1.397(5) . ?
C10 C11 1.384(5) . ?
C10 H50 0.9300 . ?
C11 C12 1.388(6) . ?
C11 H51 0.9300 . ?
C12 C13 1.386(5) . ?
C12 C16 1.510(5) . ?
C13 C14 1.390(5) . ?
C13 H53 0.9300 . ?
C14 C15 1.506(5) . ?
C15 O4 1.428(4) . ?
C15 H55A 0.9700 . ?
C15 H55B 0.9700 . ?
C16 H56A 0.9600 . ?
C16 H56B 0.9600 . ?
C16 H56C 0.9600 . ?
C17 O5 1.339(5) . ?
C17 C18 1.394(5) . ?
C17 C22 1.408(5) . ?
C18 C19 1.385(6) . ?
C18 H58 0.9300 . ?
C19 C20 1.385(6) . ?
C19 H59 0.9300 . ?
C20 C21 1.383(6) . ?
C20 C24 1.522(6) . ?
C21 C22 1.382(5) . ?
C21 H61 0.9300 . ?
C22 C23 1.503(5) . ?
C23 O6 1.427(4) . ?
C23 H63A 0.9700 . ?
C23 H63B 0.9700 . ?
C24 H64A 0.9600 . ?
C24 H64B 0.9600 . ?
C24 H64C 0.9600 . ?
C1 O1 1.349(4) . ?
C1 C2 1.398(6) . ?
C1 C6 1.400(5) . ?
C2 C3 1.395(6) . ?
C2 H66 0.9300 . ?
C3 C4 1.385(7) . ?
C3 H67 0.9300 . ?
C4 C5 1.398(6) . ?
C4 C8 1.507(6) . ?
C5 C6 1.392(5) . ?
C5 H69 0.9300 . ?
C6 C7 1.502(5) . ?
C7 O2 1.427(4) . ?
C7 H71A 0.9700 . ?
C7 H71B 0.9700 . ?
C8 H72A 0.9600 . ?
C8 H72B 0.9600 . ?
C8 H72C 0.9600 . ?
C8 H72D 0.9600 . ?
C8 H72E 0.9600 . ?
C8 H72F 0.9600 . ?
C73 O19 1.351(4) . ?
C73 C74 1.398(5) . ?
C73 C78 1.398(5) . ?
C74 C75 1.394(6) . ?
C74 H74 0.9300 . ?
C75 C76 1.383(6) . ?
C75 H75 0.9300 . ?
C76 C77 1.390(6) . ?
C76 C80 1.508(5) . ?
C77 C78 1.390(5) . ?
C77 H77 0.9300 . ?
C78 C79 1.503(5) . ?
C79 O20 1.439(4) . ?
C79 H79A 0.9700 . ?
C79 H79B 0.9700 . ?
C80 H80A 0.9600 . ?
C80 H80B 0.9600 . ?
C80 H80C 0.9600 . ?
C81 O21 1.346(4) . ?
C81 C82 1.393(5) . ?
C81 C86 1.403(5) . ?
C82 C83 1.385(6) . ?
C82 H82 0.9300 . ?
C83 C84 1.388(6) . ?
C83 H83 0.9300 . ?
C84 C85 1.396(5) . ?
C84 C88 1.510(6) . ?
C85 C86 1.388(5) . ?
C85 H85 0.9300 . ?
C86 C87 1.505(5) . ?
C87 O22 1.434(4) . ?
C87 H87A 0.9700 . ?
C87 H87B 0.9700 . ?
C88 H88A 0.9600 . ?
C88 H88B 0.9600 . ?
C88 H88C 0.9600 . ?
C89 O23 1.344(4) . ?
C89 C94 1.395(5) . ?
C89 C90 1.400(5) . ?
C90 C91 1.385(5) . ?
C90 H90 0.9300 . ?
C91 C92 1.391(6) . ?
C91 H91 0.9300 . ?
C92 C93 1.383(5) . ?
C92 C96 1.512(5) . ?
C93 C94 1.389(5) . ?
C93 H93 0.9300 . ?
C94 C95 1.503(5) . ?
C95 O24 1.428(4) . ?
C95 H95A 0.9700 . ?
C95 H95B 0.9700 . ?
C96 H96A 0.9600 . ?
C96 H96B 0.9600 . ?
C96 H96C 0.9600 . ?
N4 H4B 0.9700 . ?
N4 H4A 0.9700 . ?
N2 H2A 0.9700 . ?
N2 H2B 0.9700 . ?
N3 H3A 0.9700 . ?
N3 H3B 0.9700 . ?
N1 H1B 0.9700 . ?
N1 H1A 0.9700 . ?
N5 H5A 0.9700 . ?
N5 H5B 0.9700 . ?
N6 H6A 0.9700 . ?
N6 H6B 0.9700 . ?
N7 H7A 0.9700 . ?
N7 H7B 0.9700 . ?
N8 H8A 0.9700 . ?
N8 H8B 0.9700 . ?
O13 Ge3 1.896(2) . ?
O14 Ge3 1.882(2) . ?
O15 Ge3 1.891(2) . ?
O16 Ge3 1.881(2) . ?
O17 Ge3 1.898(2) . ?
O18 Ge3 1.875(2) . ?
O7 Ge2 1.888(2) . ?
O8 Ge2 1.877(2) . ?
O9 Ge2 1.904(2) . ?
O10 Ge2 1.885(2) . ?
O11 Ge2 1.886(2) . ?
O12 Ge2 1.880(2) . ?
O3 Ge1 1.898(2) . ?
O4 Ge1 1.874(2) . ?
O5 Ge1 1.902(3) . ?
O6 Ge1 1.878(2) . ?
O1 Ge1 1.891(2) . ?
O2 Ge1 1.882(2) . ?
O19 Ge4 1.883(2) . ?
O20 Ge4 1.874(2) . ?
O21 Ge4 1.911(2) . ?
O22 Ge4 1.887(2) . ?
O23 Ge4 1.886(2) . ?
O24 Ge4 1.881(2) . ?
C5C Cl9 1.690(9) . ?
C5C Cl10 1.753(9) . ?
C5C H5C3 0.9700 . ?
C5C H5C4 0.9700 . ?
C6C Cl11 1.746(10) . ?
C6C Cl12 1.777(12) . ?
C6C H6C1 0.9700 . ?
C6C H6C2 0.9700 . ?
C6C' Cl1B 1.726(15) . ?
C6C' Cl1A 1.768(15) . ?
C6C' H6C3 0.9700 . ?
C6C' H6C4 0.9700 . ?
C4C Cl7 1.693(17) . ?
C4C Cl8 1.725(17) . ?
C4C H4C3 0.9700 . ?
C4C H4C4 0.9700 . ?
C4C' Cl7' 1.718(12) . ?
C4C' Cl8' 1.736(12) . ?
C4C' H4C5 0.9700 . ?
C4C' H4C6 0.9700 . ?

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
O13 C49 C50 119.3(3) . . ?
O13 C49 C54 121.6(3) . . ?
C50 C49 C54 119.1(3) . . ?
Cl1 C1C Cl2 112.4(3) . . ?
Cl1 C1C H1C1 109.1 . . ?
Cl2 C1C H1C1 109.1 . . ?
Cl1 C1C H1C2 109.1 . . ?
Cl2 C1C H1C2 109.1 . . ?
H1C1 C1C H1C2 107.9 . . ?
N4 C7N H1N1 109.5 . . ?
N4 C7N H1N2 109.5 . . ?
H1N1 C7N H1N2 109.5 . . ?
N4 C7N H1N3 109.5 . . ?
H1N1 C7N H1N3 109.5 . . ?
H1N2 C7N H1N3 109.5 . . ?
C51 C50 C49 120.2(4) . . ?
C51 C50 H2 119.9 . . ?
C49 C50 H2 119.9 . . ?
Cl3 C2C Cl4 111.6(2) . . ?
Cl3 C2C H2C1 109.3 . . ?
Cl4 C2C H2C1 109.3 . . ?
Cl3 C2C H2C2 109.3 . . ?
Cl4 C2C H2C2 109.3 . . ?
H2C1 C2C H2C2 108.0 . . ?
N4 C8N H2N1 109.5 . . ?
N4 C8N H2N2 109.5 . . ?
H2N1 C8N H2N2 109.5 . . ?
N4 C8N H2N3 109.5 . . ?
H2N1 C8N H2N3 109.5 . . ?
H2N2 C8N H2N3 109.5 . . ?
C50 C51 C52 121.6(4) . . ?
C50 C51 H3 119.2 . . ?
C52 C51 H3 119.2 . . ?
Cl6 C3C Cl5 112.3(2) . . ?
Cl6 C3C H3C1 109.1 . . ?
Cl5 C3C H3C1 109.1 . . ?
Cl6 C3C H3C2 109.1 . . ?
Cl5 C3C H3C2 109.1 . . ?
H3C1 C3C H3C2 107.9 . . ?
N2 C3N H3N1 109.5 . . ?
N2 C3N H3N2 109.5 . . ?
H3N1 C3N H3N2 109.5 . . ?
N2 C3N H3N3 109.5 . . ?
H3N1 C3N H3N3 109.5 . . ?
H3N2 C3N H3N3 109.5 . . ?
C53 C52 C51 117.3(4) . . ?
C53 C52 C56 122.2(4) . . ?
C51 C52 C56 120.5(4) . . ?
N2 C4N H4N1 109.5 . . ?
N2 C4N H4N2 109.5 . . ?
H4N1 C4N H4N2 109.5 . . ?
N2 C4N H4N3 109.5 . . ?
H4N1 C4N H4N3 109.5 . . ?
H4N2 C4N H4N3 109.5 . . ?
C54 C53 C52 122.5(4) . . ?
C54 C53 H5 118.8 . . ?
C52 C53 H5 118.8 . . ?
N3 C5N H5N1 109.5 . . ?
N3 C5N H5N2 109.5 . . ?
H5N1 C5N H5N2 109.5 . . ?
N3 C5N H5N3 109.5 . . ?
H5N1 C5N H5N3 109.5 . . ?
H5N2 C5N H5N3 109.5 . . ?
C53 C54 C49 119.3(3) . . ?
C53 C54 C55 123.8(3) . . ?
C49 C54 C55 116.9(3) . . ?
N3 C6N H6N1 109.5 . . ?
N3 C6N H6N2 109.5 . . ?
H6N1 C6N H6N2 109.5 . . ?
N3 C6N H6N3 109.5 . . ?
H6N1 C6N H6N3 109.5 . . ?
H6N2 C6N H6N3 109.5 . . ?
O14 C55 C54 111.2(3) . . ?
O14 C55 H7A1 109.4 . . ?
C54 C55 H7A1 109.4 . . ?
O14 C55 H7A2 109.4 . . ?
C54 C55 H7A2 109.4 . . ?
H7A1 C55 H7A2 108.0 . . ?
Cl13 C7C Cl14 110.0(2) . . ?
Cl13 C7C H7C1 109.7 . . ?
Cl14 C7C H7C1 109.7 . . ?
Cl13 C7C H7C2 109.7 . . ?
Cl14 C7C H7C2 109.7 . . ?
H7C1 C7C H7C2 108.2 . . ?
N1 C1N H7N1 109.5 . . ?
N1 C1N H7N2 109.5 . . ?
H7N1 C1N H7N2 109.5 . . ?
N1 C1N H7N3 109.5 . . ?
H7N1 C1N H7N3 109.5 . . ?
H7N2 C1N H7N3 109.5 . . ?
C52 C56 H8PP 109.5 . . ?
C52 C56 H8PO 109.5 . . ?
H8PP C56 H8PO 109.5 . . ?
C52 C56 H8IU 109.5 . . ?
H8PP C56 H8IU 109.5 . . ?
H8PO C56 H8IU 109.5 . . ?
C52 C56 H8D 109.5 . . ?
H8PP C56 H8D 141.1 . . ?
H8PO C56 H8D 56.3 . . ?
H8IU C56 H8D 56.3 . . ?
C52 C56 H8E 109.5 . . ?
H8PP C56 H8E 56.3 . . ?
H8PO C56 H8E 141.1 . . ?
H8IU C56 H8E 56.3 . . ?
H8D C56 H8E 109.5 . . ?
C52 C56 H8F 109.5 . . ?
H8PP C56 H8F 56.3 . . ?
H8PO C56 H8F 56.3 . . ?
H8IU C56 H8F 141.1 . . ?
H8D C56 H8F 109.5 . . ?
H8E C56 H8F 109.5 . . ?
Cl15 C8C Cl16 112.0(3) . . ?
Cl15 C8C H8C1 109.2 . . ?
Cl16 C8C H8C1 109.2 . . ?
Cl15 C8C H8C2 109.2 . . ?
Cl16 C8C H8C2 109.2 . . ?
H8C1 C8C H8C2 107.9 . . ?
N1 C2N H8N1 109.5 . . ?
N1 C2N H8N2 109.5 . . ?
H8N1 C2N H8N2 109.5 . . ?
N1 C2N H8N3 109.5 . . ?
H8N1 C2N H8N3 109.5 . . ?
H8N2 C2N H8N3 109.5 . . ?
O15 C57 C58 118.8(4) . . ?
O15 C57 C62 122.4(3) . . ?
C58 C57 C62 118.9(4) . . ?
Cl17 C9C Cl18 111.4(2) . . ?
Cl17 C9C H9C1 109.3 . . ?
Cl18 C9C H9C1 109.3 . . ?
Cl17 C9C H9C2 109.3 . . ?
Cl18 C9C H9C2 109.3 . . ?
H9C1 C9C H9C2 108.0 . . ?
N5 C9N H9N1 109.5 . . ?
N5 C9N H9N2 109.5 . . ?
H9N1 C9N H9N2 109.5 . . ?
N5 C9N H9N3 109.5 . . ?
H9N1 C9N H9N3 109.5 . . ?
H9N2 C9N H9N3 109.5 . . ?
C59 C58 C57 120.7(4) . . ?
C59 C58 H10 119.7 . . ?
C57 C58 H10 119.7 . . ?
N5 C10N H10A 109.5 . . ?
N5 C10N H10B 109.5 . . ?
H10A C10N H10B 109.5 . . ?
N5 C10N H10C 109.5 . . ?
H10A C10N H10C 109.5 . . ?
H10B C10N H10C 109.5 . . ?
C58 C59 C60 121.5(4) . . ?
C58 C59 H11 119.3 . . ?
C60 C59 H11 119.3 . . ?
N6 C11N H11A 109.5 . . ?
N6 C11N H11B 109.5 . . ?
H11A C11N H11B 109.5 . . ?
N6 C11N H11C 109.5 . . ?
H11A C11N H11C 109.5 . . ?
H11B C11N H11C 109.5 . . ?
C59 C60 C61 117.1(4) . . ?
C59 C60 C64 121.4(4) . . ?
C61 C60 C64 121.4(4) . . ?
N6 C12N H12A 109.5 . . ?
N6 C12N H12B 109.5 . . ?
H12A C12N H12B 109.5 . . ?
N6 C12N H12C 109.5 . . ?
H12A C12N H12C 109.5 . . ?
H12B C12N H12C 109.5 . . ?
C62 C61 C60 122.5(4) . . ?
C62 C61 H13 118.8 . . ?
C60 C61 H13 118.8 . . ?
N7 C13N H13A 109.5 . . ?
N7 C13N H13B 109.5 . . ?
H13A C13N H13B 109.5 . . ?
N7 C13N H13C 109.5 . . ?
H13A C13N H13C 109.5 . . ?
H13B C13N H13C 109.5 . . ?
C61 C62 C57 119.4(4) . . ?
C61 C62 C63 122.7(4) . . ?
C57 C62 C63 118.0(3) . . ?
N7 C14N H14A 109.5 . . ?
N7 C14N H14B 109.5 . . ?
H14A C14N H14B 109.5 . . ?
N7 C14N H14C 109.5 . . ?
H14A C14N H14C 109.5 . . ?
H14B C14N H14C 109.5 . . ?
C60 C64 H15= 109.5 . . ?
C60 C64 H15' 109.5 . . ?
H15= C64 H15' 109.5 . . ?
C60 C64 H15Y 109.5 . . ?
H15= C64 H15Y 109.5 . . ?
H15' C64 H15Y 109.5 . . ?
N8 C15N H15A 109.5 . . ?
N8 C15N H15B 109.5 . . ?
H15A C15N H15B 109.5 . . ?
N8 C15N H15C 109.5 . . ?
H15A C15N H15C 109.5 . . ?
H15B C15N H15C 109.5 . . ?
O16 C63 C62 111.1(3) . . ?
O16 C63 H1JS 109.4 . . ?
C62 C63 H1JS 109.4 . . ?
O16 C63 H1GF 109.4 . . ?
C62 C63 H1GF 109.4 . . ?
H1JS C63 H1GF 108.0 . . ?
N8 C16N H16A 109.5 . . ?
N8 C16N H16B 109.5 . . ?
H16A C16N H16B 109.5 . . ?
N8 C16N H16C 109.5 . . ?
H16A C16N H16C 109.5 . . ?
H16B C16N H16C 109.5 . . ?
O17 C65 C66 119.9(3) . . ?
O17 C65 C70 121.7(3) . . ?
C66 C65 C70 118.4(3) . . ?
C67 C66 C65 120.7(4) . . ?
C67 C66 H18 119.7 . . ?
C65 C66 H18 119.7 . . ?
C66 C67 C68 121.9(4) . . ?
C66 C67 H19 119.0 . . ?
C68 C67 H19 119.0 . . ?
C67 C68 C69 116.7(4) . . ?
C67 C68 C72 122.1(4) . . ?
C69 C68 C72 121.2(4) . . ?
C70 C69 C68 122.9(4) . . ?
C70 C69 H21 118.5 . . ?
C68 C69 H21 118.5 . . ?
C69 C70 C65 119.3(3) . . ?
C69 C70 C71 122.9(3) . . ?
C65 C70 C71 117.8(3) . . ?
C68 C72 H23A 109.5 . . ?
C68 C72 H23B 109.5 . . ?
H23A C72 H23B 109.5 . . ?
C68 C72 H23C 109.5 . . ?
H23A C72 H23C 109.5 . . ?
H23B C72 H23C 109.5 . . ?
C68 C72 H23D 109.5 . . ?
H23A C72 H23D 141.1 . . ?
H23B C72 H23D 56.3 . . ?
H23C C72 H23D 56.3 . . ?
C68 C72 H23E 109.5 . . ?
H23A C72 H23E 56.3 . . ?
H23B C72 H23E 141.1 . . ?
H23C C72 H23E 56.3 . . ?
H23D C72 H23E 109.5 . . ?
C68 C72 H23F 109.5 . . ?
H23A C72 H23F 56.3 . . ?
H23B C72 H23F 56.3 . . ?
H23C C72 H23F 141.1 . . ?
H23D C72 H23F 109.5 . . ?
H23E C72 H23F 109.5 . . ?
O18 C71 C70 111.0(3) . . ?
O18 C71 H24A 109.4 . . ?
C70 C71 H24A 109.4 . . ?
O18 C71 H24B 109.4 . . ?
C70 C71 H24B 109.4 . . ?
H24A C71 H24B 108.0 . . ?
O7 C25 C26 119.9(3) . . ?
O7 C25 C30 122.2(3) . . ?
C26 C25 C30 117.8(3) . . ?
C27 C26 C25 121.3(4) . . ?
C27 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
C26 C27 C28 121.5(4) . . ?
C26 C27 H27 119.2 . . ?
C28 C27 H27 119.2 . . ?
C27 C28 C29 117.1(4) . . ?
C27 C28 C32 122.2(4) . . ?
C29 C28 C32 120.7(4) . . ?
C30 C29 C28 122.5(4) . . ?
C30 C29 H29 118.7 . . ?
C28 C29 H29 118.7 . . ?
C29 C30 C25 119.7(3) . . ?
C29 C30 C31 122.5(3) . . ?
C25 C30 C31 117.8(3) . . ?
O8 C31 C30 111.2(3) . . ?
O8 C31 H31A 109.4 . . ?
C30 C31 H31A 109.4 . . ?
O8 C31 H31B 109.4 . . ?
C30 C31 H31B 109.4 . . ?
H31A C31 H31B 108.0 . . ?
C28 C32 H32A 109.5 . . ?
C28 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C28 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C28 C32 H32D 109.5 . . ?
H32A C32 H32D 141.1 . . ?
H32B C32 H32D 56.3 . . ?
H32C C32 H32D 56.3 . . ?
C28 C32 H32E 109.5 . . ?
H32A C32 H32E 56.3 . . ?
H32B C32 H32E 141.1 . . ?
H32C C32 H32E 56.3 . . ?
H32D C32 H32E 109.5 . . ?
C28 C32 H32F 109.5 . . ?
H32A C32 H32F 56.3 . . ?
H32B C32 H32F 56.3 . . ?
H32C C32 H32F 141.1 . . ?
H32D C32 H32F 109.5 . . ?
H32E C32 H32F 109.5 . . ?
O9 C33 C34 119.2(3) . . ?
O9 C33 C38 121.1(3) . . ?
C34 C33 C38 119.7(3) . . ?
C33 C34 C35 120.1(4) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C36 C35 C34 121.5(4) . . ?
C36 C35 H35 119.2 . . ?
C34 C35 H35 119.2 . . ?
C35 C36 C37 117.8(3) . . ?
C35 C36 C39 121.3(4) . . ?
C37 C36 C39 120.9(4) . . ?
C38 C37 C36 121.8(4) . . ?
C38 C37 H37 119.1 . . ?
C36 C37 H37 119.1 . . ?
C37 C38 C33 119.0(3) . . ?
C37 C38 C40 123.8(3) . . ?
C33 C38 C40 117.1(3) . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C36 C39 H39D 109.5 . . ?
H39A C39 H39D 141.1 . . ?
H39B C39 H39D 56.3 . . ?
H39C C39 H39D 56.3 . . ?
C36 C39 H39E 109.5 . . ?
H39A C39 H39E 56.3 . . ?
H39B C39 H39E 141.1 . . ?
H39C C39 H39E 56.3 . . ?
H39D C39 H39E 109.5 . . ?
C36 C39 H39F 109.5 . . ?
H39A C39 H39F 56.3 . . ?
H39B C39 H39F 56.3 . . ?
H39C C39 H39F 141.1 . . ?
H39D C39 H39F 109.5 . . ?
H39E C39 H39F 109.5 . . ?
O10 C40 C38 111.0(3) . . ?
O10 C40 H40A 109.4 . . ?
C38 C40 H40A 109.4 . . ?
O10 C40 H40B 109.4 . . ?
C38 C40 H40B 109.4 . . ?
H40A C40 H40B 108.0 . . ?
O11 C41 C42 119.0(3) . . ?
O11 C41 C46 122.1(3) . . ?
C42 C41 C46 118.8(4) . . ?
C43 C42 C41 120.5(4) . . ?
C43 C42 H42 119.8 . . ?
C41 C42 H42 119.8 . . ?
C42 C43 C44 121.4(4) . . ?
C42 C43 H43 119.3 . . ?
C44 C43 H43 119.3 . . ?
C45 C44 C43 117.9(4) . . ?
C45 C44 C48 121.7(4) . . ?
C43 C44 C48 120.4(4) . . ?
C44 C45 C46 122.3(4) . . ?
C44 C45 H45 118.9 . . ?
C46 C45 H45 118.9 . . ?
C45 C46 C41 119.0(4) . . ?
C45 C46 C47 122.8(3) . . ?
C41 C46 C47 118.2(3) . . ?
O12 C47 C46 110.9(3) . . ?
O12 C47 H47A 109.5 . . ?
C46 C47 H47A 109.5 . . ?
O12 C47 H47B 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 108.1 . . ?
C44 C48 H48A 109.5 . . ?
C44 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C44 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C44 C48 H48D 109.5 . . ?
H48A C48 H48D 141.1 . . ?
H48B C48 H48D 56.3 . . ?
H48C C48 H48D 56.3 . . ?
C44 C48 H48E 109.5 . . ?
H48A C48 H48E 56.3 . . ?
H48B C48 H48E 141.1 . . ?
H48C C48 H48E 56.3 . . ?
H48D C48 H48E 109.5 . . ?
C44 C48 H48F 109.5 . . ?
H48A C48 H48F 56.3 . . ?
H48B C48 H48F 56.3 . . ?
H48C C48 H48F 141.1 . . ?
H48D C48 H48F 109.5 . . ?
H48E C48 H48F 109.5 . . ?
O3 C9 C10 119.7(3) . . ?
O3 C9 C14 121.0(3) . . ?
C10 C9 C14 119.3(3) . . ?
C11 C10 C9 120.3(4) . . ?
C11 C10 H50 119.8 . . ?
C9 C10 H50 119.8 . . ?
C10 C11 C12 121.2(4) . . ?
C10 C11 H51 119.4 . . ?
C12 C11 H51 119.4 . . ?
C13 C12 C11 118.0(4) . . ?
C13 C12 C16 121.7(4) . . ?
C11 C12 C16 120.3(4) . . ?
C12 C13 C14 122.3(4) . . ?
C12 C13 H53 118.9 . . ?
C14 C13 H53 118.9 . . ?
C13 C14 C9 119.0(3) . . ?
C13 C14 C15 124.2(3) . . ?
C9 C14 C15 116.7(3) . . ?
O4 C15 C14 110.8(3) . . ?
O4 C15 H55A 109.5 . . ?
C14 C15 H55A 109.5 . . ?
O4 C15 H55B 109.5 . . ?
C14 C15 H55B 109.5 . . ?
H55A C15 H55B 108.1 . . ?
C12 C16 H56A 109.5 . . ?
C12 C16 H56B 109.5 . . ?
H56A C16 H56B 109.5 . . ?
C12 C16 H56C 109.5 . . ?
H56A C16 H56C 109.5 . . ?
H56B C16 H56C 109.5 . . ?
O5 C17 C18 119.9(3) . . ?
O5 C17 C22 122.1(3) . . ?
C18 C17 C22 117.9(4) . . ?
C19 C18 C17 120.9(4) . . ?
C19 C18 H58 119.5 . . ?
C17 C18 H58 119.5 . . ?
C18 C19 C20 121.7(4) . . ?
C18 C19 H59 119.1 . . ?
C20 C19 H59 119.1 . . ?
C21 C20 C19 116.9(4) . . ?
C21 C20 C24 121.0(4) . . ?
C19 C20 C24 122.1(4) . . ?
C22 C21 C20 123.1(4) . . ?
C22 C21 H61 118.4 . . ?
C20 C21 H61 118.4 . . ?
C21 C22 C17 119.4(4) . . ?
C21 C22 C23 123.0(3) . . ?
C17 C22 C23 117.6(3) . . ?
O6 C23 C22 111.6(3) . . ?
O6 C23 H63A 109.3 . . ?
C22 C23 H63A 109.3 . . ?
O6 C23 H63B 109.3 . . ?
C22 C23 H63B 109.3 . . ?
H63A C23 H63B 108.0 . . ?
C20 C24 H64A 109.5 . . ?
C20 C24 H64B 109.5 . . ?
H64A C24 H64B 109.5 . . ?
C20 C24 H64C 109.5 . . ?
H64A C24 H64C 109.5 . . ?
H64B C24 H64C 109.5 . . ?
O1 C1 C2 118.9(3) . . ?
O1 C1 C6 122.6(3) . . ?
C2 C1 C6 118.4(4) . . ?
C3 C2 C1 120.4(4) . . ?
C3 C2 H66 119.8 . . ?
C1 C2 H66 119.8 . . ?
C4 C3 C2 122.0(4) . . ?
C4 C3 H67 119.0 . . ?
C2 C3 H67 119.0 . . ?
C3 C4 C5 116.8(4) . . ?
C3 C4 C8 121.8(4) . . ?
C5 C4 C8 121.4(4) . . ?
C6 C5 C4 122.5(4) . . ?
C6 C5 H69 118.8 . . ?
C4 C5 H69 118.8 . . ?
C5 C6 C1 119.8(4) . . ?
C5 C6 C7 121.7(4) . . ?
C1 C6 C7 118.5(3) . . ?
O2 C7 C6 110.9(3) . . ?
O2 C7 H71A 109.5 . . ?
C6 C7 H71A 109.5 . . ?
O2 C7 H71B 109.5 . . ?
C6 C7 H71B 109.5 . . ?
H71A C7 H71B 108.1 . . ?
C4 C8 H72A 109.5 . . ?
C4 C8 H72B 109.5 . . ?
H72A C8 H72B 109.5 . . ?
C4 C8 H72C 109.5 . . ?
H72A C8 H72C 109.5 . . ?
H72B C8 H72C 109.5 . . ?
C4 C8 H72D 109.5 . . ?
H72A C8 H72D 141.1 . . ?
H72B C8 H72D 56.3 . . ?
H72C C8 H72D 56.3 . . ?
C4 C8 H72E 109.5 . . ?
H72A C8 H72E 56.3 . . ?
H72B C8 H72E 141.1 . . ?
H72C C8 H72E 56.3 . . ?
H72D C8 H72E 109.5 . . ?
C4 C8 H72F 109.5 . . ?
H72A C8 H72F 56.3 . . ?
H72B C8 H72F 56.3 . . ?
H72C C8 H72F 141.1 . . ?
H72D C8 H72F 109.5 . . ?
H72E C8 H72F 109.5 . . ?
O19 C73 C74 119.3(3) . . ?
O19 C73 C78 122.2(3) . . ?
C74 C73 C78 118.5(3) . . ?
C75 C74 C73 120.5(4) . . ?
C75 C74 H74 119.7 . . ?
C73 C74 H74 119.7 . . ?
C76 C75 C74 121.5(4) . . ?
C76 C75 H75 119.3 . . ?
C74 C75 H75 119.3 . . ?
C75 C76 C77 117.4(4) . . ?
C75 C76 C80 121.5(4) . . ?
C77 C76 C80 121.1(4) . . ?
C78 C77 C76 122.6(4) . . ?
C78 C77 H77 118.7 . . ?
C76 C77 H77 118.7 . . ?
C77 C78 C73 119.5(3) . . ?
C77 C78 C79 122.5(3) . . ?
C73 C78 C79 118.1(3) . . ?
O20 C79 C78 110.4(3) . . ?
O20 C79 H79A 109.6 . . ?
C78 C79 H79A 109.6 . . ?
O20 C79 H79B 109.6 . . ?
C78 C79 H79B 109.6 . . ?
H79A C79 H79B 108.1 . . ?
C76 C80 H80A 109.5 . . ?
C76 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
C76 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
O21 C81 C82 120.3(3) . . ?
O21 C81 C86 121.0(3) . . ?
C82 C81 C86 118.7(3) . . ?
C83 C82 C81 120.6(4) . . ?
C83 C82 H82 119.7 . . ?
C81 C82 H82 119.7 . . ?
C82 C83 C84 121.8(4) . . ?
C82 C83 H83 119.1 . . ?
C84 C83 H83 119.1 . . ?
C83 C84 C85 117.1(4) . . ?
C83 C84 C88 121.5(4) . . ?
C85 C84 C88 121.5(4) . . ?
C86 C85 C84 122.4(4) . . ?
C86 C85 H85 118.8 . . ?
C84 C85 H85 118.8 . . ?
C85 C86 C81 119.5(3) . . ?
C85 C86 C87 123.5(3) . . ?
C81 C86 C87 117.0(3) . . ?
O22 C87 C86 110.4(3) . . ?
O22 C87 H87A 109.6 . . ?
C86 C87 H87A 109.6 . . ?
O22 C87 H87B 109.6 . . ?
C86 C87 H87B 109.6 . . ?
H87A C87 H87B 108.1 . . ?
C84 C88 H88A 109.5 . . ?
C84 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C84 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
O23 C89 C94 122.8(3) . . ?
O23 C89 C90 118.2(3) . . ?
C94 C89 C90 118.9(3) . . ?
C91 C90 C89 120.2(4) . . ?
C91 C90 H90 119.9 . . ?
C89 C90 H90 119.9 . . ?
C90 C91 C92 121.7(4) . . ?
C90 C91 H91 119.2 . . ?
C92 C91 H91 119.2 . . ?
C93 C92 C91 117.2(3) . . ?
C93 C92 C96 121.0(4) . . ?
C91 C92 C96 121.7(4) . . ?
C92 C93 C94 122.7(3) . . ?
C92 C93 H93 118.7 . . ?
C94 C93 H93 118.7 . . ?
C93 C94 C89 119.3(3) . . ?
C93 C94 C95 122.2(3) . . ?
C89 C94 C95 118.5(3) . . ?
O24 C95 C94 111.0(3) . . ?
O24 C95 H95A 109.4 . . ?
C94 C95 H95A 109.4 . . ?
O24 C95 H95B 109.4 . . ?
C94 C95 H95B 109.4 . . ?
H95A C95 H95B 108.0 . . ?
C92 C96 H96A 109.5 . . ?
C92 C96 H96B 109.5 . . ?
H96A C96 H96B 109.5 . . ?
C92 C96 H96C 109.5 . . ?
H96A C96 H96C 109.5 . . ?
H96B C96 H96C 109.5 . . ?
C8N N4 C7N 112.4(3) . . ?
C8N N4 H4B 109.1 . . ?
C7N N4 H4B 109.1 . . ?
C8N N4 H4A 109.1 . . ?
C7N N4 H4A 109.1 . . ?
H4B N4 H4A 107.9 . . ?
C3N N2 C4N 112.2(3) . . ?
C3N N2 H2A 109.2 . . ?
C4N N2 H2A 109.2 . . ?
C3N N2 H2B 109.2 . . ?
C4N N2 H2B 109.2 . . ?
H2A N2 H2B 107.9 . . ?
C5N N3 C6N 112.1(3) . . ?
C5N N3 H3A 109.2 . . ?
C6N N3 H3A 109.2 . . ?
C5N N3 H3B 109.2 . . ?
C6N N3 H3B 109.2 . . ?
H3A N3 H3B 107.9 . . ?
C1N N1 C2N 113.8(4) . . ?
C1N N1 H1B 108.8 . . ?
C2N N1 H1B 108.8 . . ?
C1N N1 H1A 108.8 . . ?
C2N N1 H1A 108.8 . . ?
H1B N1 H1A 107.7 . . ?
C9N N5 C10N 113.7(3) . . ?
C9N N5 H5A 108.8 . . ?
C10N N5 H5A 108.8 . . ?
C9N N5 H5B 108.8 . . ?
C10N N5 H5B 108.8 . . ?
H5A N5 H5B 107.7 . . ?
C11N N6 C12N 112.3(3) . . ?
C11N N6 H6A 109.1 . . ?
C12N N6 H6A 109.1 . . ?
C11N N6 H6B 109.1 . . ?
C12N N6 H6B 109.1 . . ?
H6A N6 H6B 107.9 . . ?
C14N N7 C13N 112.1(3) . . ?
C14N N7 H7A 109.2 . . ?
C13N N7 H7A 109.2 . . ?
C14N N7 H7B 109.2 . . ?
C13N N7 H7B 109.2 . . ?
H7A N7 H7B 107.9 . . ?
C16N N8 C15N 112.2(3) . . ?
C16N N8 H8A 109.2 . . ?
C15N N8 H8A 109.2 . . ?
C16N N8 H8B 109.2 . . ?
C15N N8 H8B 109.2 . . ?
H8A N8 H8B 107.9 . . ?
C49 O13 Ge3 122.9(2) . . ?
C55 O14 Ge3 115.2(2) . . ?
C57 O15 Ge3 124.4(2) . . ?
C63 O16 Ge3 115.4(2) . . ?
C65 O17 Ge3 124.5(2) . . ?
C71 O18 Ge3 115.7(2) . . ?
C25 O7 Ge2 123.8(2) . . ?
C31 O8 Ge2 115.5(2) . . ?
C33 O9 Ge2 123.2(2) . . ?
C40 O10 Ge2 115.8(2) . . ?
C41 O11 Ge2 124.7(2) . . ?
C47 O12 Ge2 115.0(2) . . ?
C9 O3 Ge1 122.4(2) . . ?
C15 O4 Ge1 115.5(2) . . ?
C17 O5 Ge1 124.8(2) . . ?
C23 O6 Ge1 116.4(2) . . ?
C1 O1 Ge1 124.4(2) . . ?
C7 O2 Ge1 115.3(2) . . ?
C73 O19 Ge4 123.4(2) . . ?
C79 O20 Ge4 115.4(2) . . ?
C81 O21 Ge4 122.6(2) . . ?
C87 O22 Ge4 115.5(2) . . ?
C89 O23 Ge4 124.9(2) . . ?
C95 O24 Ge4 115.1(2) . . ?
Cl9 C5C Cl10 114.1(6) . . ?
Cl9 C5C H5C3 108.7 . . ?
Cl10 C5C H5C3 108.7 . . ?
Cl9 C5C H5C4 108.7 . . ?
Cl10 C5C H5C4 108.7 . . ?
H5C3 C5C H5C4 107.6 . . ?
O18 Ge3 O16 89.70(10) . . ?
O18 Ge3 O14 87.68(10) . . ?
O16 Ge3 O14 89.01(10) . . ?
O18 Ge3 O15 177.52(10) . . ?
O16 Ge3 O15 92.78(11) . . ?
O14 Ge3 O15 92.46(11) . . ?
O18 Ge3 O13 93.21(11) . . ?
O16 Ge3 O13 176.26(11) . . ?
O14 Ge3 O13 93.46(10) . . ?
O15 Ge3 O13 84.31(11) . . ?
O18 Ge3 O17 92.94(10) . . ?
O16 Ge3 O17 91.74(11) . . ?
O14 Ge3 O17 179.02(11) . . ?
O15 Ge3 O17 86.88(11) . . ?
O13 Ge3 O17 85.76(10) . . ?
Cl11 C6C Cl12 113.9(6) . . ?
Cl11 C6C H6C1 108.8 . . ?
Cl12 C6C H6C1 108.8 . . ?
Cl11 C6C H6C2 108.8 . . ?
Cl12 C6C H6C2 108.8 . . ?
H6C1 C6C H6C2 107.7 . . ?
Cl1B C6C' Cl1A 107.3(11) . . ?
Cl1B C6C' H6C3 110.3 . . ?
Cl1A C6C' H6C3 110.3 . . ?
Cl1B C6C' H6C4 110.2 . . ?
Cl1A C6C' H6C4 110.2 . . ?
H6C3 C6C' H6C4 108.5 . . ?
Cl7 C4C Cl8 111.7(11) . . ?
Cl7 C4C H4C3 109.3 . . ?
Cl8 C4C H4C3 109.3 . . ?
Cl7 C4C H4C4 109.3 . . ?
Cl8 C4C H4C4 109.3 . . ?
H4C3 C4C H4C4 107.9 . . ?
Cl7' C4C' Cl8' 111.0(7) . . ?
Cl7' C4C' H4C5 109.4 . . ?
Cl8' C4C' H4C5 109.4 . . ?
Cl7' C4C' H4C6 109.4 . . ?
Cl8' C4C' H4C6 109.4 . . ?
H4C5 C4C' H4C6 108.0 . . ?
O8 Ge2 O12 89.10(10) . . ?
O8 Ge2 O10 88.61(10) . . ?
O12 Ge2 O10 89.21(10) . . ?
O8 Ge2 O11 177.79(10) . . ?
O12 Ge2 O11 93.07(10) . . ?
O10 Ge2 O11 90.96(11) . . ?
O8 Ge2 O7 93.33(10) . . ?
O12 Ge2 O7 92.93(11) . . ?
O10 Ge2 O7 177.13(10) . . ?
O11 Ge2 O7 87.02(11) . . ?
O8 Ge2 O9 92.40(10) . . ?
O12 Ge2 O9 177.71(10) . . ?
O10 Ge2 O9 92.56(10) . . ?
O11 Ge2 O9 85.45(10) . . ?
O7 Ge2 O9 85.26(10) . . ?
O4 Ge1 O6 87.49(11) . . ?
O4 Ge1 O2 89.83(11) . . ?
O6 Ge1 O2 89.27(10) . . ?
O4 Ge1 O1 92.60(11) . . ?
O6 Ge1 O1 177.88(10) . . ?
O2 Ge1 O1 92.85(10) . . ?
O4 Ge1 O3 93.07(11) . . ?
O6 Ge1 O3 93.21(10) . . ?
O2 Ge1 O3 176.26(11) . . ?
O1 Ge1 O3 84.67(11) . . ?
O4 Ge1 O5 178.49(10) . . ?
O6 Ge1 O5 92.71(11) . . ?
O2 Ge1 O5 91.67(11) . . ?
O1 Ge1 O5 87.14(11) . . ?
O3 Ge1 O5 85.42(11) . . ?
O20 Ge4 O24 88.58(10) . . ?
O20 Ge4 O19 93.59(10) . . ?
O24 Ge4 O19 93.60(11) . . ?
O20 Ge4 O23 178.35(10) . . ?
O24 Ge4 O23 93.06(10) . . ?
O19 Ge4 O23 86.17(10) . . ?
O20 Ge4 O22 89.17(10) . . ?
O24 Ge4 O22 88.43(10) . . ?
O19 Ge4 O22 176.61(10) . . ?
O23 Ge4 O22 91.02(10) . . ?
O20 Ge4 O21 92.14(10) . . ?
O24 Ge4 O21 178.98(10) . . ?
O19 Ge4 O21 85.63(11) . . ?
O23 Ge4 O21 86.22(10) . . ?
O22 Ge4 O21 92.30(10) . . ?

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
O13 C49 C50 C51 -178.5(3) . . . . ?
C54 C49 C50 C51 -0.3(5) . . . . ?
C49 C50 C51 C52 0.2(6) . . . . ?
C50 C51 C52 C53 0.4(6) . . . . ?
C50 C51 C52 C56 180.0(4) . . . . ?
C51 C52 C53 C54 -1.0(6) . . . . ?
C56 C52 C53 C54 179.5(4) . . . . ?
C52 C53 C54 C49 0.9(6) . . . . ?
C52 C53 C54 C55 -178.2(3) . . . . ?
O13 C49 C54 C53 177.9(3) . . . . ?
C50 C49 C54 C53 -0.2(5) . . . . ?
O13 C49 C54 C55 -2.9(5) . . . . ?
C50 C49 C54 C55 178.9(3) . . . . ?
C53 C54 C55 O14 126.6(4) . . . . ?
C49 C54 C55 O14 -52.5(4) . . . . ?
O15 C57 C58 C59 -176.5(4) . . . . ?
C62 C57 C58 C59 2.3(6) . . . . ?
C57 C58 C59 C60 -0.7(6) . . . . ?
C58 C59 C60 C61 -0.9(6) . . . . ?
C58 C59 C60 C64 177.4(4) . . . . ?
C59 C60 C61 C62 0.9(6) . . . . ?
C64 C60 C61 C62 -177.4(4) . . . . ?
C60 C61 C62 C57 0.8(6) . . . . ?
C60 C61 C62 C63 -178.1(4) . . . . ?
O15 C57 C62 C61 176.5(3) . . . . ?
C58 C57 C62 C61 -2.4(5) . . . . ?
O15 C57 C62 C63 -4.6(5) . . . . ?
C58 C57 C62 C63 176.5(3) . . . . ?
C61 C62 C63 O16 131.2(4) . . . . ?
C57 C62 C63 O16 -47.6(4) . . . . ?
O17 C65 C66 C67 -177.1(3) . . . . ?
C70 C65 C66 C67 1.8(5) . . . . ?
C65 C66 C67 C68 -1.0(6) . . . . ?
C66 C67 C68 C69 -0.6(6) . . . . ?
C66 C67 C68 C72 179.1(4) . . . . ?
C67 C68 C69 C70 1.4(6) . . . . ?
C72 C68 C69 C70 -178.3(4) . . . . ?
C68 C69 C70 C65 -0.6(5) . . . . ?
C68 C69 C70 C71 179.6(3) . . . . ?
O17 C65 C70 C69 177.8(3) . . . . ?
C66 C65 C70 C69 -1.0(5) . . . . ?
O17 C65 C70 C71 -2.3(5) . . . . ?
C66 C65 C70 C71 178.8(3) . . . . ?
C69 C70 C71 O18 129.7(3) . . . . ?
C65 C70 C71 O18 -50.1(4) . . . . ?
O7 C25 C26 C27 -176.8(3) . . . . ?
C30 C25 C26 C27 0.7(5) . . . . ?
C25 C26 C27 C28 1.3(6) . . . . ?
C26 C27 C28 C29 -2.3(6) . . . . ?
C26 C27 C28 C32 177.1(4) . . . . ?
C27 C28 C29 C30 1.3(6) . . . . ?
C32 C28 C29 C30 -178.1(4) . . . . ?
C28 C29 C30 C25 0.7(6) . . . . ?
C28 C29 C30 C31 -178.1(3) . . . . ?
O7 C25 C30 C29 175.8(3) . . . . ?
C26 C25 C30 C29 -1.7(5) . . . . ?
O7 C25 C30 C31 -5.4(5) . . . . ?
C26 C25 C30 C31 177.2(3) . . . . ?
C29 C30 C31 O8 131.0(3) . . . . ?
C25 C30 C31 O8 -47.8(4) . . . . ?
O9 C33 C34 C35 -178.2(3) . . . . ?
C38 C33 C34 C35 1.4(5) . . . . ?
C33 C34 C35 C36 -0.1(6) . . . . ?
C34 C35 C36 C37 -0.6(5) . . . . ?
C34 C35 C36 C39 179.5(4) . . . . ?
C35 C36 C37 C38 0.0(5) . . . . ?
C39 C36 C37 C38 179.9(3) . . . . ?
C36 C37 C38 C33 1.2(5) . . . . ?
C36 C37 C38 C40 -175.7(3) . . . . ?
O9 C33 C38 C37 177.7(3) . . . . ?
C34 C33 C38 C37 -1.9(5) . . . . ?
O9 C33 C38 C40 -5.1(5) . . . . ?
C34 C33 C38 C40 175.2(3) . . . . ?
C37 C38 C40 O10 126.2(4) . . . . ?
C33 C38 C40 O10 -50.8(4) . . . . ?
O11 C41 C42 C43 -176.4(4) . . . . ?
C46 C41 C42 C43 2.0(6) . . . . ?
C41 C42 C43 C44 0.6(7) . . . . ?
C42 C43 C44 C45 -2.5(7) . . . . ?
C42 C43 C44 C48 176.6(5) . . . . ?
C43 C44 C45 C46 1.7(7) . . . . ?
C48 C44 C45 C46 -177.4(4) . . . . ?
C44 C45 C46 C41 0.9(6) . . . . ?
C44 C45 C46 C47 -178.6(4) . . . . ?
O11 C41 C46 C45 175.7(3) . . . . ?
C42 C41 C46 C45 -2.7(6) . . . . ?
O11 C41 C46 C47 -4.8(5) . . . . ?
C42 C41 C46 C47 176.8(4) . . . . ?
C45 C46 C47 O12 132.0(4) . . . . ?
C41 C46 C47 O12 -47.5(4) . . . . ?
O3 C9 C10 C11 178.1(3) . . . . ?
C14 C9 C10 C11 -0.2(5) . . . . ?
C9 C10 C11 C12 0.0(6) . . . . ?
C10 C11 C12 C13 -0.3(6) . . . . ?
C10 C11 C12 C16 -179.9(4) . . . . ?
C11 C12 C13 C14 1.0(6) . . . . ?
C16 C12 C13 C14 -179.5(4) . . . . ?
C12 C13 C14 C9 -1.2(6) . . . . ?
C12 C13 C14 C15 177.3(3) . . . . ?
O3 C9 C14 C13 -177.5(3) . . . . ?
C10 C9 C14 C13 0.8(5) . . . . ?
O3 C9 C14 C15 3.9(5) . . . . ?
C10 C9 C14 C15 -177.8(3) . . . . ?
C13 C14 C15 O4 -125.7(4) . . . . ?
C9 C14 C15 O4 52.8(4) . . . . ?
O5 C17 C18 C19 177.7(4) . . . . ?
C22 C17 C18 C19 -0.8(6) . . . . ?
C17 C18 C19 C20 0.6(6) . . . . ?
C18 C19 C20 C21 0.8(6) . . . . ?
C18 C19 C20 C24 -177.9(4) . . . . ?
C19 C20 C21 C22 -2.0(6) . . . . ?
C24 C20 C21 C22 176.6(4) . . . . ?
C20 C21 C22 C17 1.9(6) . . . . ?
C20 C21 C22 C23 -179.1(4) . . . . ?
O5 C17 C22 C21 -178.8(3) . . . . ?
C18 C17 C22 C21 -0.4(5) . . . . ?
O5 C17 C22 C23 2.1(5) . . . . ?
C18 C17 C22 C23 -179.5(3) . . . . ?
C21 C22 C23 O6 -129.8(4) . . . . ?
C17 C22 C23 O6 49.3(4) . . . . ?
O1 C1 C2 C3 174.8(4) . . . . ?
C6 C1 C2 C3 -2.7(6) . . . . ?
C1 C2 C3 C4 0.5(7) . . . . ?
C2 C3 C4 C5 1.8(7) . . . . ?
C2 C3 C4 C8 -177.3(4) . . . . ?
C3 C4 C5 C6 -2.0(6) . . . . ?
C8 C4 C5 C6 177.1(4) . . . . ?
C4 C5 C6 C1 -0.2(6) . . . . ?
C4 C5 C6 C7 179.2(4) . . . . ?
O1 C1 C6 C5 -174.9(3) . . . . ?
C2 C1 C6 C5 2.5(6) . . . . ?
O1 C1 C6 C7 5.7(5) . . . . ?
C2 C1 C6 C7 -176.9(4) . . . . ?
C5 C6 C7 O2 -133.4(4) . . . . ?
C1 C6 C7 O2 45.9(5) . . . . ?
O19 C73 C74 C75 -176.4(3) . . . . ?
C78 C73 C74 C75 2.2(5) . . . . ?
C73 C74 C75 C76 0.1(6) . . . . ?
C74 C75 C76 C77 -1.8(6) . . . . ?
C74 C75 C76 C80 177.8(4) . . . . ?
C75 C76 C77 C78 1.3(6) . . . . ?
C80 C76 C77 C78 -178.4(4) . . . . ?
C76 C77 C78 C73 1.1(5) . . . . ?
C76 C77 C78 C79 -178.4(3) . . . . ?
O19 C73 C78 C77 175.8(3) . . . . ?
C74 C73 C78 C77 -2.8(5) . . . . ?
O19 C73 C78 C79 -4.7(5) . . . . ?
C74 C73 C78 C79 176.8(3) . . . . ?
C77 C78 C79 O20 130.8(3) . . . . ?
C73 C78 C79 O20 -48.7(4) . . . . ?
O21 C81 C82 C83 -177.4(3) . . . . ?
C86 C81 C82 C83 1.2(5) . . . . ?
C81 C82 C83 C84 -0.2(6) . . . . ?
C82 C83 C84 C85 -0.5(6) . . . . ?
C82 C83 C84 C88 179.6(4) . . . . ?
C83 C84 C85 C86 0.2(5) . . . . ?
C88 C84 C85 C86 -179.9(4) . . . . ?
C84 C85 C86 C81 0.8(5) . . . . ?
C84 C85 C86 C87 -175.8(3) . . . . ?
O21 C81 C86 C85 177.0(3) . . . . ?
C82 C81 C86 C85 -1.5(5) . . . . ?
O21 C81 C86 C87 -6.1(5) . . . . ?
C82 C81 C86 C87 175.3(3) . . . . ?
C85 C86 C87 O22 125.4(3) . . . . ?
C81 C86 C87 O22 -51.3(4) . . . . ?
O23 C89 C90 C91 -177.2(4) . . . . ?
C94 C89 C90 C91 0.8(6) . . . . ?
C89 C90 C91 C92 -0.2(6) . . . . ?
C90 C91 C92 C93 -0.3(6) . . . . ?
C90 C91 C92 C96 178.6(4) . . . . ?
C91 C92 C93 C94 0.2(6) . . . . ?
C96 C92 C93 C94 -178.7(4) . . . . ?
C92 C93 C94 C89 0.4(6) . . . . ?
C92 C93 C94 C95 -179.2(4) . . . . ?
O23 C89 C94 C93 177.0(3) . . . . ?
C90 C89 C94 C93 -0.9(5) . . . . ?
O23 C89 C94 C95 -3.4(5) . . . . ?
C90 C89 C94 C95 178.7(3) . . . . ?
C93 C94 C95 O24 132.7(3) . . . . ?
C89 C94 C95 O24 -46.9(4) . . . . ?
C50 C49 O13 Ge3 -141.8(3) . . . . ?
C54 C49 O13 Ge3 40.1(4) . . . . ?
C54 C55 O14 Ge3 66.8(3) . . . . ?
C58 C57 O15 Ge3 -147.4(3) . . . . ?
C62 C57 O15 Ge3 33.8(5) . . . . ?
C62 C63 O16 Ge3 68.4(3) . . . . ?
C66 C65 O17 Ge3 -146.6(3) . . . . ?
C70 C65 O17 Ge3 34.6(4) . . . . ?
C70 C71 O18 Ge3 67.8(3) . . . . ?
C26 C25 O7 Ge2 -146.6(3) . . . . ?
C30 C25 O7 Ge2 36.0(4) . . . . ?
C30 C31 O8 Ge2 67.5(3) . . . . ?
C34 C33 O9 Ge2 -139.1(3) . . . . ?
C38 C33 O9 Ge2 41.3(4) . . . . ?
C38 C40 O10 Ge2 67.8(3) . . . . ?
C42 C41 O11 Ge2 -147.8(3) . . . . ?
C46 C41 O11 Ge2 33.8(5) . . . . ?
C46 C47 O12 Ge2 68.3(3) . . . . ?
C10 C9 O3 Ge1 139.0(3) . . . . ?
C14 C9 O3 Ge1 -42.7(4) . . . . ?
C14 C15 O4 Ge1 -67.2(3) . . . . ?
C18 C17 O5 Ge1 147.7(3) . . . . ?
C22 C17 O5 Ge1 -33.9(4) . . . . ?
C22 C23 O6 Ge1 -66.7(3) . . . . ?
C2 C1 O1 Ge1 150.4(3) . . . . ?
C6 C1 O1 Ge1 -32.2(5) . . . . ?
C6 C7 O2 Ge1 -68.6(3) . . . . ?
C74 C73 O19 Ge4 -144.9(3) . . . . ?
C78 C73 O19 Ge4 36.6(4) . . . . ?
C78 C79 O20 Ge4 67.8(3) . . . . ?
C82 C81 O21 Ge4 -138.1(3) . . . . ?
C86 C81 O21 Ge4 43.4(4) . . . . ?
C86 C87 O22 Ge4 68.6(3) . . . . ?
C94 C89 O23 Ge4 29.8(5) . . . . ?
C90 C89 O23 Ge4 -152.3(3) . . . . ?
C94 C95 O24 Ge4 68.1(3) . . . . ?
C71 O18 Ge3 O16 -126.2(2) . . . . ?
C71 O18 Ge3 O14 144.8(2) . . . . ?
C71 O18 Ge3 O13 51.5(2) . . . . ?
C71 O18 Ge3 O17 -34.4(2) . . . . ?
C63 O16 Ge3 O18 142.9(2) . . . . ?
C63 O16 Ge3 O14 -129.4(2) . . . . ?
C63 O16 Ge3 O15 -37.0(2) . . . . ?
C63 O16 Ge3 O17 49.9(2) . . . . ?
C55 O14 Ge3 O18 -123.0(2) . . . . ?
C55 O14 Ge3 O16 147.3(2) . . . . ?
C55 O14 Ge3 O15 54.5(2) . . . . ?
C55 O14 Ge3 O13 -29.9(2) . . . . ?
C57 O15 Ge3 O16 -12.1(3) . . . . ?
C57 O15 Ge3 O14 77.1(3) . . . . ?
C57 O15 Ge3 O13 170.3(3) . . . . ?
C57 O15 Ge3 O17 -103.7(3) . . . . ?
C49 O13 Ge3 O18 66.2(3) . . . . ?
C49 O13 Ge3 O14 -21.7(3) . . . . ?
C49 O13 Ge3 O15 -113.8(3) . . . . ?
C49 O13 Ge3 O17 158.9(3) . . . . ?
C65 O17 Ge3 O18 -15.2(3) . . . . ?
C65 O17 Ge3 O16 74.6(3) . . . . ?
C65 O17 Ge3 O15 167.3(3) . . . . ?
C65 O17 Ge3 O13 -108.2(3) . . . . ?
C31 O8 Ge2 O12 -128.2(2) . . . . ?
C31 O8 Ge2 O10 142.6(2) . . . . ?
C31 O8 Ge2 O7 -35.3(2) . . . . ?
C31 O8 Ge2 O9 50.1(2) . . . . ?
C47 O12 Ge2 O8 143.1(2) . . . . ?
C47 O12 Ge2 O10 -128.3(2) . . . . ?
C47 O12 Ge2 O11 -37.3(2) . . . . ?
C47 O12 Ge2 O7 49.8(2) . . . . ?
C40 O10 Ge2 O8 -123.8(2) . . . . ?
C40 O10 Ge2 O12 147.1(2) . . . . ?
C40 O10 Ge2 O11 54.0(2) . . . . ?
C40 O10 Ge2 O9 -31.5(2) . . . . ?
C41 O11 Ge2 O12 -11.8(3) . . . . ?
C41 O11 Ge2 O10 77.4(3) . . . . ?
C41 O11 Ge2 O7 -104.6(3) . . . . ?
C41 O11 Ge2 O9 169.9(3) . . . . ?
C25 O7 Ge2 O8 -14.6(3) . . . . ?
C25 O7 Ge2 O12 74.7(3) . . . . ?
C25 O7 Ge2 O11 167.6(3) . . . . ?
C25 O7 Ge2 O9 -106.7(3) . . . . ?
C15 O4 Ge1 O6 122.2(2) . . . . ?
C15 O4 Ge1 O2 -148.6(2) . . . . ?
C15 O4 Ge1 O1 -55.7(2) . . . . ?
C15 O4 Ge1 O3 29.1(2) . . . . ?
C23 O6 Ge1 O4 -144.8(2) . . . . ?
C23 O6 Ge1 O2 125.3(2) . . . . ?
C23 O6 Ge1 O3 -51.9(2) . . . . ?
C23 O6 Ge1 O5 33.7(2) . . . . ?
C7 O2 Ge1 O4 131.8(2) . . . . ?
C7 O2 Ge1 O6 -140.7(2) . . . . ?
C7 O2 Ge1 O1 39.2(3) . . . . ?
C7 O2 Ge1 O5 -48.0(3) . . . . ?
C1 O1 Ge1 O4 -80.6(3) . . . . ?
C1 O1 Ge1 O2 9.3(3) . . . . ?
C1 O1 Ge1 O3 -173.5(3) . . . . ?
C1 O1 Ge1 O5 100.9(3) . . . . ?
C9 O3 Ge1 O4 24.0(3) . . . . ?
C9 O3 Ge1 O6 -63.6(3) . . . . ?
C9 O3 Ge1 O1 116.4(3) . . . . ?
C9 O3 Ge1 O5 -156.1(3) . . . . ?
C79 O20 Ge4 O24 -128.5(2) . . . . ?
C79 O20 Ge4 O19 -35.0(2) . . . . ?
C79 O20 Ge4 O22 143.0(2) . . . . ?
C79 O20 Ge4 O21 50.8(2) . . . . ?
C95 O24 Ge4 O20 141.0(2) . . . . ?
C95 O24 Ge4 O19 47.5(2) . . . . ?
C95 O24 Ge4 O23 -38.9(2) . . . . ?
C95 O24 Ge4 O22 -129.8(2) . . . . ?
C73 O19 Ge4 O20 -15.3(3) . . . . ?
C73 O19 Ge4 O24 73.4(3) . . . . ?
C73 O19 Ge4 O23 166.3(3) . . . . ?
C73 O19 Ge4 O21 -107.2(3) . . . . ?
C89 O23 Ge4 O24 -8.3(3) . . . . ?
C89 O23 Ge4 O19 -101.7(3) . . . . ?
C89 O23 Ge4 O22 80.2(3) . . . . ?
C89 O23 Ge4 O21 172.4(3) . . . . ?
C87 O22 Ge4 O20 -123.6(2) . . . . ?
C87 O22 Ge4 O24 147.8(2) . . . . ?
C87 O22 Ge4 O23 54.7(2) . . . . ?
C87 O22 Ge4 O21 -31.5(2) . . . . ?

_refine_diff_density_max         3.319
_refine_diff_density_min         -2.328
_refine_diff_density_rms         0.085

_shelxl_version_number           2013-4


# start Validation Reply Form
_vrf_DIFMX01_shelx               
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00
RESPONSE: cf. below
;
_vrf_PLAT097_shelx               
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       3.32 eA-3  
RESPONSE: The two highest unrefined electron density peaks are located
1.58 A away from Cl1 (3.3 e/A3) and 1.09 A away from Cl6 (3.1 e/A3).
They indicate a disorder of the respective CH2Cl2 molecules as packing 
solvents, to which these Cl atoms belong. It is verifyed, that trials
to introduce disorder here gave non-reliable results only.
;
_vrf_PLAT413_shelx               
;
PROBLEM: Short Inter XH3 .. XHn     H64B   ..  H72C    ..       1.99 Ang.  
RESPONSE: This contact refers to interactions of hydrogen atoms, of which
at least one belongs to a disordered fragment. 
;
_vrf_PLAT910_shelx               
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         45 Report
RESPONSE: 
;
_vrf_PLAT971_shelx               
;
PROBLEM: Check Calcd Residual Density  1.62A From    Cl13       3.28 eA-3  
RESPONSE: cf. above
;
# end Validation Reply Form

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1440865'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2016-02-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H49 Ge O6, C2 H8 N'
_chemical_formula_sum            'C38 H57 Ge N O6'
_chemical_formula_weight         696.43

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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                   10.5372(5)
_cell_length_b                   14.2260(8)
_cell_length_c                   14.3811(8)
_cell_angle_alpha                118.392(6)
_cell_angle_beta                 92.482(4)
_cell_angle_gamma                93.965(4)
_cell_volume                     1884.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    110
_cell_measurement_reflns_used    6425
_cell_measurement_theta_min      3.5930
_cell_measurement_theta_max      28.3720

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_F_000             744
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_absorpt_coefficient_mu    0.856
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.94206
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       '/w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12164
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.228
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6621
_reflns_number_gt                6069
_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 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_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)+(0.0325P)²+0.7995P] 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         6621
_refine_ls_number_parameters     416
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_ref         0.0709
_refine_ls_wR_factor_gt          0.0693
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_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
C1 C 0.75107(16) -0.08048(14) 0.42755(13) 0.0156(4) Uani 1 1 d . . . . .
H1A H 0.7870 -0.1112 0.3595 0.019 Uiso 1 1 calc R U . . .
H1B H 0.6922 -0.0304 0.4289 0.019 Uiso 1 1 calc R U . . .
C1N C 1.04058(17) 0.25421(15) 0.53297(16) 0.0233(4) Uani 1 1 d . . . . .
H1N1 H 1.0712 0.2626 0.6006 0.035 Uiso 1 1 calc R U . . .
H1N2 H 0.9889 0.3109 0.5434 0.035 Uiso 1 1 calc R U . . .
H1N3 H 1.1118 0.2572 0.4947 0.035 Uiso 1 1 calc R U . . .
C2 C 0.68094(15) -0.16803(14) 0.44140(14) 0.0139(4) Uani 1 1 d . . . . .
C2N C 0.91295(19) 0.13038(16) 0.36651(15) 0.0255(4) Uani 1 1 d . . . . .
H2N1 H 0.8638 0.0615 0.3301 0.038 Uiso 1 1 calc R U . . .
H2N2 H 0.9826 0.1318 0.3261 0.038 Uiso 1 1 calc R U . . .
H2N3 H 0.8595 0.1853 0.3747 0.038 Uiso 1 1 calc R U . . .
C3 C 0.65227(15) -0.27035(14) 0.35641(14) 0.0153(4) Uani 1 1 d . . . . .
H3 H 0.6690 -0.2829 0.2887 0.018 Uiso 1 1 calc R U . . .
C4 C 0.59945(16) -0.35393(14) 0.36999(14) 0.0160(4) Uani 1 1 d . . . . .
C5 C 0.58406(16) -0.33297(14) 0.47346(14) 0.0165(4) Uani 1 1 d . . . . .
H5 H 0.5527 -0.3896 0.4841 0.020 Uiso 1 1 calc R U . . .
C6 C 0.61279(15) -0.23220(14) 0.56220(14) 0.0150(4) Uani 1 1 d . . . . .
C7 C 0.65518(15) -0.14709(13) 0.54345(14) 0.0139(4) Uani 1 1 d . . . . .
C8 C 0.56025(19) -0.46335(15) 0.27708(15) 0.0236(4) Uani 1 1 d . . . . .
H8A H 0.5257 -0.5106 0.3021 0.035 Uiso 0.5 1 calc R U P . .
H8B H 0.6334 -0.4915 0.2393 0.035 Uiso 0.5 1 calc R U P . .
H8C H 0.4967 -0.4578 0.2306 0.035 Uiso 0.5 1 calc R U P . .
H8D H 0.5781 -0.4627 0.2125 0.035 Uiso 0.5 1 calc R U P . .
H8E H 0.4705 -0.4817 0.2754 0.035 Uiso 0.5 1 calc R U P . .
H8F H 0.6072 -0.5155 0.2841 0.035 Uiso 0.5 1 calc R U P . .
C9 C 0.60222(18) -0.21640(15) 0.67476(15) 0.0205(4) Uani 1 1 d . . . . .
C10 C 0.5581(2) -0.32106(16) 0.67454(16) 0.0267(4) Uani 1 1 d . . . . .
H10A H 0.6166 -0.3733 0.6390 0.040 Uiso 1 1 calc R U . . .
H10B H 0.4744 -0.3476 0.6381 0.040 Uiso 1 1 calc R U . . .
H10C H 0.5558 -0.3081 0.7463 0.040 Uiso 1 1 calc R U . . .
C11 C 0.5069(2) -0.13611(16) 0.73153(17) 0.0296(5) Uani 1 1 d . . . . .
H11A H 0.5324 -0.0693 0.7329 0.044 Uiso 1 1 calc R U . . .
H11B H 0.5047 -0.1244 0.8029 0.044 Uiso 1 1 calc R U . . .
H11C H 0.4236 -0.1640 0.6946 0.044 Uiso 1 1 calc R U . . .
C12 C 0.73357(19) -0.17584(16) 0.73703(16) 0.0272(4) Uani 1 1 d . . . . .
H12A H 0.7933 -0.2266 0.7009 0.041 Uiso 1 1 calc R U . . .
H12B H 0.7277 -0.1677 0.8069 0.041 Uiso 1 1 calc R U . . .
H12C H 0.7621 -0.1078 0.7423 0.041 Uiso 1 1 calc R U . . .
C13 C 0.96876(16) 0.12582(15) 0.80966(14) 0.0182(4) Uani 1 1 d . . . . .
H13A H 0.9866 0.2001 0.8260 0.022 Uiso 1 1 calc R U . . .
H13B H 1.0455 0.1042 0.8306 0.022 Uiso 1 1 calc R U . . .
C14 C 0.86362(16) 0.11843(14) 0.87396(14) 0.0165(4) Uani 1 1 d . . . . .
C15 C 0.88392(17) 0.09352(14) 0.95493(14) 0.0194(4) Uani 1 1 d . . . . .
H15 H 0.9634 0.0750 0.9674 0.023 Uiso 1 1 calc R U . . .
C16 C 0.78682(18) 0.09595(15) 1.01766(15) 0.0217(4) Uani 1 1 d . . . . .
C17 C 0.67235(17) 0.12881(15) 0.99989(14) 0.0208(4) Uani 1 1 d . . . . .
H17 H 0.6083 0.1331 1.0438 0.025 Uiso 1 1 calc R U . . .
C18 C 0.64662(16) 0.15605(14) 0.92017(14) 0.0173(4) Uani 1 1 d . . . . .
C19 C 0.74438(16) 0.14390(13) 0.85293(13) 0.0152(4) Uani 1 1 d . . . . .
C20 C 0.8074(2) 0.0691(2) 1.10628(17) 0.0339(5) Uani 1 1 d . . . . .
H20A H 0.8919 0.0479 1.1068 0.051 Uiso 0.5 1 calc R U P . .
H20B H 0.7457 0.0113 1.0957 0.051 Uiso 0.5 1 calc R U P . .
H20C H 0.7979 0.1311 1.1728 0.051 Uiso 0.5 1 calc R U P . .
H20D H 0.7318 0.0790 1.1434 0.051 Uiso 0.5 1 calc R U P . .
H20E H 0.8780 0.1156 1.1545 0.051 Uiso 0.5 1 calc R U P . .
H20F H 0.8257 -0.0042 1.0774 0.051 Uiso 0.5 1 calc R U P . .
C21 C 0.52413(17) 0.20514(15) 0.91290(15) 0.0208(4) Uani 1 1 d . . . . .
C22 C 0.44418(18) 0.13687(16) 0.80728(15) 0.0234(4) Uani 1 1 d . . . . .
H22A H 0.4219 0.0663 0.7984 0.035 Uiso 1 1 calc R U . . .
H22B H 0.4926 0.1316 0.7503 0.035 Uiso 1 1 calc R U . . .
H22C H 0.3678 0.1698 0.8068 0.035 Uiso 1 1 calc R U . . .
C23 C 0.55995(19) 0.31756(15) 0.92742(16) 0.0277(5) Uani 1 1 d . . . . .
H23A H 0.6101 0.3603 0.9939 0.042 Uiso 1 1 calc R U . . .
H23B H 0.4837 0.3506 0.9269 0.042 Uiso 1 1 calc R U . . .
H23C H 0.6086 0.3124 0.8706 0.042 Uiso 1 1 calc R U . . .
C24 C 0.43875(19) 0.2184(2) 1.00160(17) 0.0333(5) Uani 1 1 d . . . . .
H24A H 0.4863 0.2610 1.0693 0.050 Uiso 1 1 calc R U . . .
H24B H 0.4110 0.1490 0.9935 0.050 Uiso 1 1 calc R U . . .
H24C H 0.3657 0.2533 0.9973 0.050 Uiso 1 1 calc R U . . .
C25 C 0.67354(16) 0.23170(13) 0.61653(14) 0.0158(4) Uani 1 1 d . . . . .
H25A H 0.6363 0.2424 0.6809 0.019 Uiso 1 1 calc R U . . .
H25B H 0.6049 0.2113 0.5612 0.019 Uiso 1 1 calc R U . . .
C26 C 0.74888(16) 0.33352(14) 0.63506(14) 0.0163(4) Uani 1 1 d . . . . .
C27 C 0.74042(16) 0.36628(15) 0.55882(15) 0.0192(4) Uani 1 1 d . . . . .
H27 H 0.6845 0.3267 0.4984 0.023 Uiso 1 1 calc R U . . .
C28 C 0.81322(17) 0.45658(15) 0.57027(16) 0.0226(4) Uani 1 1 d . . . . .
C29 C 0.89567(18) 0.51321(15) 0.66199(16) 0.0240(4) Uani 1 1 d . . . . .
H29 H 0.9437 0.5749 0.6714 0.029 Uiso 1 1 calc R U . . .
C30 C 0.91053(18) 0.48311(14) 0.74019(15) 0.0228(4) Uani 1 1 d . . . . .
C31 C 0.83377(17) 0.39143(14) 0.72523(14) 0.0190(4) Uani 1 1 d . . . . .
C32 C 0.8075(2) 0.49041(18) 0.48624(18) 0.0319(5) Uani 1 1 d . . . . .
H32A H 0.8644 0.5544 0.5086 0.048 Uiso 0.5 1 calc R U P . .
H32B H 0.7219 0.5044 0.4750 0.048 Uiso 0.5 1 calc R U P . .
H32C H 0.8325 0.4341 0.4213 0.048 Uiso 0.5 1 calc R U P . .
H32D H 0.7481 0.4409 0.4280 0.048 Uiso 0.5 1 calc R U P . .
H32E H 0.8906 0.4909 0.4616 0.048 Uiso 0.5 1 calc R U P . .
H32F H 0.7801 0.5612 0.5153 0.048 Uiso 0.5 1 calc R U P . .
C33 C 1.0092(2) 0.54487(16) 0.83613(16) 0.0326(5) Uani 1 1 d . . . . .
C34 C 1.1073(2) 0.47035(19) 0.83617(18) 0.0382(6) Uani 1 1 d . . . . .
H34A H 1.1479 0.4426 0.7711 0.057 Uiso 1 1 calc R U . . .
H34B H 1.0651 0.4119 0.8425 0.057 Uiso 1 1 calc R U . . .
H34C H 1.1705 0.5098 0.8950 0.057 Uiso 1 1 calc R U . . .
C35 C 0.9430(2) 0.59020(18) 0.93906(17) 0.0432(6) Uani 1 1 d . . . . .
H35A H 0.8819 0.6366 0.9377 0.065 Uiso 1 1 calc R U . . .
H35B H 1.0055 0.6302 0.9983 0.065 Uiso 1 1 calc R U . . .
H35C H 0.9001 0.5322 0.9458 0.065 Uiso 1 1 calc R U . . .
C36 C 1.0834(3) 0.63969(19) 0.8332(2) 0.0489(7) Uani 1 1 d . . . . .
H36A H 1.1262 0.6140 0.7693 0.073 Uiso 1 1 calc R U . . .
H36B H 1.1452 0.6751 0.8936 0.073 Uiso 1 1 calc R U . . .
H36C H 1.0252 0.6894 0.8349 0.073 Uiso 1 1 calc R U . . .
N1 N 0.96352(13) 0.14960(11) 0.47175(11) 0.0161(3) Uani 1 1 d . . . . .
H1C H 1.0157 0.0929 0.4630 0.019 Uiso 1 1 calc R U . . .
H1D H 0.8928 0.1465 0.5115 0.019 Uiso 1 1 calc R U . . .
O1 O 0.85054(10) -0.02538(9) 0.51063(9) 0.0132(2) Uani 1 1 d . . . . .
O2 O 0.66943(11) -0.04367(9) 0.62616(9) 0.0151(3) Uani 1 1 d . . . . .
O3 O 0.93985(11) 0.06105(10) 0.69775(9) 0.0169(3) Uani 1 1 d . . . . .
O4 O 0.72852(11) 0.16045(9) 0.76718(9) 0.0148(3) Uani 1 1 d . . . . .
O5 O 0.75792(11) 0.14884(9) 0.58535(9) 0.0148(3) Uani 1 1 d . . . . .
O6 O 0.84695(12) 0.35974(10) 0.80073(10) 0.0229(3) Uani 1 1 d . . . . .
H6 H 0.8046 0.3018 0.7805 0.034 Uiso 1 1 calc R U . . .
Ge1 Ge 0.78786(2) 0.06034(2) 0.63877(2) 0.01188(6) 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
C1 O1 1.424(2) . ?
C1 C2 1.503(2) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1N N1 1.475(2) . ?
C1N H1N1 0.9600 . ?
C1N H1N2 0.9600 . ?
C1N H1N3 0.9600 . ?
C2 C3 1.385(2) . ?
C2 C7 1.395(2) . ?
C2N N1 1.472(2) . ?
C2N H2N1 0.9600 . ?
C2N H2N2 0.9600 . ?
C2N H2N3 0.9600 . ?
C3 C4 1.379(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.391(3) . ?
C4 C8 1.505(2) . ?
C5 C6 1.394(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.409(2) . ?
C6 C9 1.535(2) . ?
C7 O2 1.375(2) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C8 H8D 0.9600 . ?
C8 H8E 0.9600 . ?
C8 H8F 0.9600 . ?
C9 C11 1.524(3) . ?
C9 C10 1.527(2) . ?
C9 C12 1.530(3) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 O3 1.428(2) . ?
C13 C14 1.503(2) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.382(3) . ?
C14 C19 1.391(3) . ?
C15 C16 1.385(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.380(3) . ?
C16 C20 1.506(3) . ?
C17 C18 1.396(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.406(2) . ?
C18 C21 1.532(3) . ?
C19 O4 1.367(2) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C20 H20D 0.9600 . ?
C20 H20E 0.9600 . ?
C20 H20F 0.9600 . ?
C21 C22 1.527(3) . ?
C21 C23 1.528(3) . ?
C21 C24 1.538(3) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 O5 1.434(2) . ?
C25 C26 1.502(2) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.382(3) . ?
C26 C31 1.394(3) . ?
C27 C28 1.385(3) . ?
C27 H27 0.9300 . ?
C28 C29 1.392(3) . ?
C28 C32 1.499(3) . ?
C29 C30 1.387(3) . ?
C29 H29 0.9300 . ?
C30 C31 1.405(3) . ?
C30 C33 1.534(3) . ?
C31 O6 1.365(2) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C32 H32D 0.9600 . ?
C32 H32E 0.9600 . ?
C32 H32F 0.9600 . ?
C33 C35 1.529(3) . ?
C33 C36 1.531(3) . ?
C33 C34 1.531(3) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
N1 H1C 0.9700 . ?
N1 H1D 0.9700 . ?
O1 Ge1 1.8435(11) . ?
O2 Ge1 1.8025(11) . ?
O3 Ge1 1.7766(12) . ?
O4 Ge1 1.8846(11) . ?
O5 Ge1 1.7969(12) . ?
O6 H6 0.8200 . ?

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
O1 C1 C2 109.65(14) . . ?
O1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
O1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N1 C1N H1N1 109.5 . . ?
N1 C1N H1N2 109.5 . . ?
H1N1 C1N H1N2 109.5 . . ?
N1 C1N H1N3 109.5 . . ?
H1N1 C1N H1N3 109.5 . . ?
H1N2 C1N H1N3 109.5 . . ?
C3 C2 C7 120.22(16) . . ?
C3 C2 C1 120.92(15) . . ?
C7 C2 C1 118.62(15) . . ?
N1 C2N H2N1 109.5 . . ?
N1 C2N H2N2 109.5 . . ?
H2N1 C2N H2N2 109.5 . . ?
N1 C2N H2N3 109.5 . . ?
H2N1 C2N H2N3 109.5 . . ?
H2N2 C2N H2N3 109.5 . . ?
C4 C3 C2 121.45(16) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 117.16(16) . . ?
C3 C4 C8 121.58(16) . . ?
C5 C4 C8 121.26(16) . . ?
C4 C5 C6 123.90(16) . . ?
C4 C5 H5 118.0 . . ?
C6 C5 H5 118.1 . . ?
C5 C6 C7 116.81(16) . . ?
C5 C6 C9 121.12(15) . . ?
C7 C6 C9 122.05(15) . . ?
O2 C7 C2 120.60(15) . . ?
O2 C7 C6 119.44(15) . . ?
C2 C7 C6 119.95(15) . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C8 H8D 109.5 . . ?
H8A C8 H8D 141.1 . . ?
H8B C8 H8D 56.3 . . ?
H8C C8 H8D 56.3 . . ?
C4 C8 H8E 109.5 . . ?
H8A C8 H8E 56.3 . . ?
H8B C8 H8E 141.1 . . ?
H8C C8 H8E 56.3 . . ?
H8D C8 H8E 109.5 . . ?
C4 C8 H8F 109.5 . . ?
H8A C8 H8F 56.3 . . ?
H8B C8 H8F 56.3 . . ?
H8C C8 H8F 141.1 . . ?
H8D C8 H8F 109.5 . . ?
H8E C8 H8F 109.5 . . ?
C11 C9 C10 107.70(15) . . ?
C11 C9 C12 109.79(16) . . ?
C10 C9 C12 107.19(16) . . ?
C11 C9 C6 110.58(16) . . ?
C10 C9 C6 112.22(15) . . ?
C12 C9 C6 109.28(14) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O3 C13 C14 113.82(14) . . ?
O3 C13 H13A 108.8 . . ?
C14 C13 H13A 108.8 . . ?
O3 C13 H13B 108.8 . . ?
C14 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
C15 C14 C19 120.34(16) . . ?
C15 C14 C13 122.41(16) . . ?
C19 C14 C13 117.16(16) . . ?
C14 C15 C16 120.47(17) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C17 C16 C15 117.95(17) . . ?
C17 C16 C20 120.86(17) . . ?
C15 C16 C20 121.12(17) . . ?
C16 C17 C18 124.15(17) . . ?
C16 C17 H17 117.9 . . ?
C18 C17 H17 117.9 . . ?
C17 C18 C19 115.83(17) . . ?
C17 C18 C21 121.68(15) . . ?
C19 C18 C21 122.29(16) . . ?
O4 C19 C14 117.23(15) . . ?
O4 C19 C18 121.90(16) . . ?
C14 C19 C18 120.82(16) . . ?
C16 C20 H20A 109.5 . . ?
C16 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C16 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C16 C20 H20D 109.5 . . ?
H20A C20 H20D 141.1 . . ?
H20B C20 H20D 56.3 . . ?
H20C C20 H20D 56.3 . . ?
C16 C20 H20E 109.5 . . ?
H20A C20 H20E 56.3 . . ?
H20B C20 H20E 141.1 . . ?
H20C C20 H20E 56.3 . . ?
H20D C20 H20E 109.5 . . ?
C16 C20 H20F 109.5 . . ?
H20A C20 H20F 56.3 . . ?
H20B C20 H20F 56.3 . . ?
H20C C20 H20F 141.1 . . ?
H20D C20 H20F 109.5 . . ?
H20E C20 H20F 109.5 . . ?
C22 C21 C23 109.67(16) . . ?
C22 C21 C18 112.34(15) . . ?
C23 C21 C18 108.84(15) . . ?
C22 C21 C24 107.32(15) . . ?
C23 C21 C24 106.79(16) . . ?
C18 C21 C24 111.72(16) . . ?
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 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O5 C25 C26 108.46(13) . . ?
O5 C25 H25A 110.0 . . ?
C26 C25 H25A 110.0 . . ?
O5 C25 H25B 110.0 . . ?
C26 C25 H25B 110.0 . . ?
H25A C25 H25B 108.4 . . ?
C27 C26 C31 119.61(16) . . ?
C27 C26 C25 119.76(16) . . ?
C31 C26 C25 120.48(16) . . ?
C26 C27 C28 121.61(18) . . ?
C26 C27 H27 119.2 . . ?
C28 C27 H27 119.2 . . ?
C27 C28 C29 117.16(17) . . ?
C27 C28 C32 121.81(18) . . ?
C29 C28 C32 121.00(17) . . ?
C30 C29 C28 123.94(17) . . ?
C30 C29 H29 118.0 . . ?
C28 C29 H29 118.0 . . ?
C29 C30 C31 116.66(18) . . ?
C29 C30 C33 121.46(17) . . ?
C31 C30 C33 121.85(18) . . ?
O6 C31 C26 121.14(15) . . ?
O6 C31 C30 117.86(16) . . ?
C26 C31 C30 120.98(17) . . ?
C28 C32 H32A 109.5 . . ?
C28 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C28 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C28 C32 H32D 109.5 . . ?
H32A C32 H32D 141.1 . . ?
H32B C32 H32D 56.3 . . ?
H32C C32 H32D 56.3 . . ?
C28 C32 H32E 109.5 . . ?
H32A C32 H32E 56.3 . . ?
H32B C32 H32E 141.1 . . ?
H32C C32 H32E 56.3 . . ?
H32D C32 H32E 109.5 . . ?
C28 C32 H32F 109.5 . . ?
H32A C32 H32F 56.3 . . ?
H32B C32 H32F 56.3 . . ?
H32C C32 H32F 141.1 . . ?
H32D C32 H32F 109.5 . . ?
H32E C32 H32F 109.5 . . ?
C35 C33 C36 107.28(18) . . ?
C35 C33 C34 110.5(2) . . ?
C36 C33 C34 106.89(19) . . ?
C35 C33 C30 110.29(18) . . ?
C36 C33 C30 112.09(19) . . ?
C34 C33 C30 109.69(16) . . ?
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 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C2N N1 C1N 112.85(15) . . ?
C2N N1 H1C 109.0 . . ?
C1N N1 H1C 109.0 . . ?
C2N N1 H1D 109.0 . . ?
C1N N1 H1D 109.0 . . ?
H1C N1 H1D 107.8 . . ?
C1 O1 Ge1 112.01(10) . . ?
C7 O2 Ge1 124.62(10) . . ?
C13 O3 Ge1 119.71(10) . . ?
C19 O4 Ge1 117.83(10) . . ?
C25 O5 Ge1 130.14(10) . . ?
C31 O6 H6 109.5 . . ?
O3 Ge1 O5 122.65(5) . . ?
O3 Ge1 O2 114.87(6) . . ?
O5 Ge1 O2 122.27(5) . . ?
O3 Ge1 O1 86.13(5) . . ?
O5 Ge1 O1 85.80(5) . . ?
O2 Ge1 O1 93.79(5) . . ?
O3 Ge1 O4 94.56(5) . . ?
O5 Ge1 O4 88.71(5) . . ?
O2 Ge1 O4 91.45(5) . . ?
O1 Ge1 O4 173.87(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
O1 C1 C2 C3 -133.72(16) . . . . ?
O1 C1 C2 C7 40.6(2) . . . . ?
C7 C2 C3 C4 -0.8(3) . . . . ?
C1 C2 C3 C4 173.47(16) . . . . ?
C2 C3 C4 C5 -4.2(2) . . . . ?
C2 C3 C4 C8 175.93(16) . . . . ?
C3 C4 C5 C6 3.3(3) . . . . ?
C8 C4 C5 C6 -176.81(16) . . . . ?
C4 C5 C6 C7 2.5(3) . . . . ?
C4 C5 C6 C9 -175.75(16) . . . . ?
C3 C2 C7 O2 -172.44(15) . . . . ?
C1 C2 C7 O2 13.2(2) . . . . ?
C3 C2 C7 C6 6.8(2) . . . . ?
C1 C2 C7 C6 -167.52(15) . . . . ?
C5 C6 C7 O2 171.78(15) . . . . ?
C9 C6 C7 O2 -10.0(2) . . . . ?
C5 C6 C7 C2 -7.5(2) . . . . ?
C9 C6 C7 C2 170.70(15) . . . . ?
C5 C6 C9 C11 -120.36(18) . . . . ?
C7 C6 C9 C11 61.5(2) . . . . ?
C5 C6 C9 C10 -0.1(2) . . . . ?
C7 C6 C9 C10 -178.21(16) . . . . ?
C5 C6 C9 C12 118.69(18) . . . . ?
C7 C6 C9 C12 -59.4(2) . . . . ?
O3 C13 C14 C15 126.67(18) . . . . ?
O3 C13 C14 C19 -56.9(2) . . . . ?
C19 C14 C15 C16 -1.5(3) . . . . ?
C13 C14 C15 C16 174.82(17) . . . . ?
C14 C15 C16 C17 -3.0(3) . . . . ?
C14 C15 C16 C20 -179.93(18) . . . . ?
C15 C16 C17 C18 2.4(3) . . . . ?
C20 C16 C17 C18 179.32(18) . . . . ?
C16 C17 C18 C19 2.6(3) . . . . ?
C16 C17 C18 C21 -172.31(17) . . . . ?
C15 C14 C19 O4 -175.60(15) . . . . ?
C13 C14 C19 O4 7.9(2) . . . . ?
C15 C14 C19 C18 6.9(3) . . . . ?
C13 C14 C19 C18 -169.64(16) . . . . ?
C17 C18 C19 O4 175.35(15) . . . . ?
C21 C18 C19 O4 -9.7(3) . . . . ?
C17 C18 C19 C14 -7.2(2) . . . . ?
C21 C18 C19 C14 167.70(16) . . . . ?
C17 C18 C21 C22 -120.95(18) . . . . ?
C19 C18 C21 C22 64.4(2) . . . . ?
C17 C18 C21 C23 117.40(19) . . . . ?
C19 C18 C21 C23 -57.2(2) . . . . ?
C17 C18 C21 C24 -0.3(2) . . . . ?
C19 C18 C21 C24 -174.91(17) . . . . ?
O5 C25 C26 C27 101.87(18) . . . . ?
O5 C25 C26 C31 -73.80(19) . . . . ?
C31 C26 C27 C28 -0.9(3) . . . . ?
C25 C26 C27 C28 -176.61(16) . . . . ?
C26 C27 C28 C29 0.1(3) . . . . ?
C26 C27 C28 C32 178.00(17) . . . . ?
C27 C28 C29 C30 1.4(3) . . . . ?
C32 C28 C29 C30 -176.54(18) . . . . ?
C28 C29 C30 C31 -1.9(3) . . . . ?
C28 C29 C30 C33 176.05(18) . . . . ?
C27 C26 C31 O6 -178.28(16) . . . . ?
C25 C26 C31 O6 -2.6(2) . . . . ?
C27 C26 C31 C30 0.4(3) . . . . ?
C25 C26 C31 C30 176.03(16) . . . . ?
C29 C30 C31 O6 179.67(16) . . . . ?
C33 C30 C31 O6 1.7(3) . . . . ?
C29 C30 C31 C26 1.0(3) . . . . ?
C33 C30 C31 C26 -176.99(17) . . . . ?
C29 C30 C33 C35 120.0(2) . . . . ?
C31 C30 C33 C35 -62.1(3) . . . . ?
C29 C30 C33 C36 0.5(3) . . . . ?
C31 C30 C33 C36 178.41(19) . . . . ?
C29 C30 C33 C34 -118.0(2) . . . . ?
C31 C30 C33 C34 59.8(2) . . . . ?
C2 C1 O1 Ge1 -72.40(14) . . . . ?
C2 C7 O2 Ge1 -33.1(2) . . . . ?
C6 C7 O2 Ge1 147.63(12) . . . . ?
C14 C13 O3 Ge1 45.05(19) . . . . ?
C14 C19 O4 Ge1 46.42(18) . . . . ?
C18 C19 O4 Ge1 -136.07(14) . . . . ?
C26 C25 O5 Ge1 127.09(13) . . . . ?
C13 O3 Ge1 O5 92.66(12) . . . . ?
C13 O3 Ge1 O2 -92.45(12) . . . . ?
C13 O3 Ge1 O1 175.16(12) . . . . ?
C13 O3 Ge1 O4 1.27(12) . . . . ?
C25 O5 Ge1 O3 -117.24(13) . . . . ?
C25 O5 Ge1 O2 68.25(14) . . . . ?
C25 O5 Ge1 O1 160.08(13) . . . . ?
C25 O5 Ge1 O4 -22.65(13) . . . . ?
C7 O2 Ge1 O3 -84.66(13) . . . . ?
C7 O2 Ge1 O5 90.24(13) . . . . ?
C7 O2 Ge1 O1 2.82(13) . . . . ?
C7 O2 Ge1 O4 179.63(13) . . . . ?
C1 O1 Ge1 O3 162.60(11) . . . . ?
C1 O1 Ge1 O5 -74.22(10) . . . . ?
C1 O1 Ge1 O2 47.90(11) . . . . ?
C19 O4 Ge1 O3 -48.27(11) . . . . ?
C19 O4 Ge1 O5 -170.93(11) . . . . ?
C19 O4 Ge1 O2 66.82(11) . . . . ?

_refine_diff_density_max         0.363
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.048

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1440866'
_audit_update_record             
;
2016-02-04 deposited with the CCDC.
2016-02-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C21 H18 Ge O6), C H2 Cl2, 4(C2 H8 N)'
_chemical_formula_sum            'C25.50 H35 Cl Ge N2 O6'
_chemical_formula_weight         573.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

_cell_length_a                   25.226(5)
_cell_length_b                   20.080(3)
_cell_length_c                   24.170(6)
_cell_angle_alpha                90
_cell_angle_beta                 120.32(3)
_cell_angle_gamma                90
_cell_volume                     10568(4)
_cell_formula_units_Z            16
_cell_measurement_temperature    110
_cell_measurement_reflns_used    3964
_cell_measurement_theta_min      4.1200
_cell_measurement_theta_max      66.5750

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_F_000             4784
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    2.864
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.87637
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17583
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.054
_diffrn_reflns_theta_max         63.747
_diffrn_reflns_theta_full        63.750
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             8596
_reflns_number_gt                6286
_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 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'

_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_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)+(0.0410P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8596
_refine_ls_number_parameters     673
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_ref         0.0985
_refine_ls_wR_factor_gt          0.0903
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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
C1 C 0.10231(16) 0.01610(18) 0.37274(16) 0.0296(9) Uani 1 1 d . . . . .
H1A H 0.1217 -0.0033 0.3506 0.036 Uiso 1 1 calc R U . . .
H1B H 0.0658 0.0395 0.3414 0.036 Uiso 1 1 calc R U . . .
C1C C -0.00336(18) 0.3157(2) 0.42953(19) 0.0452(11) Uani 1 1 d . . . . .
H1C1 H 0.0149 0.3275 0.4039 0.054 Uiso 1 1 calc R U . . .
H1C2 H 0.0110 0.2716 0.4471 0.054 Uiso 1 1 calc R U . . .
C7N C -0.34331(17) -0.06277(17) -0.01859(17) 0.0331(9) Uani 1 1 d . . . . .
H1N1 H -0.3154 -0.0749 -0.0330 0.050 Uiso 1 1 calc R U . . .
H1N2 H -0.3848 -0.0666 -0.0535 0.050 Uiso 1 1 calc R U . . .
H1N3 H -0.3375 -0.0919 0.0155 0.050 Uiso 1 1 calc R U . . .
C2 C 0.08424(15) -0.03854(18) 0.40255(16) 0.0285(9) Uani 1 1 d . . . . .
C9N C -0.37262(15) 0.02878(19) 0.02842(17) 0.0324(9) Uani 1 1 d . . . . .
H2N1 H -0.3631 0.0739 0.0433 0.049 Uiso 1 1 calc R U . . .
H2N2 H -0.3670 0.0005 0.0630 0.049 Uiso 1 1 calc R U . . .
H2N3 H -0.4145 0.0262 -0.0058 0.049 Uiso 1 1 calc R U . . .
C3 C 0.08593(16) -0.10560(19) 0.38954(18) 0.0353(9) Uani 1 1 d . . . . .
H3 H 0.1000 -0.1183 0.3622 0.042 Uiso 1 1 calc R U . . .
C3N C -0.10339(18) 0.1364(2) 0.33937(19) 0.0443(11) Uani 1 1 d . . . . .
H3N1 H -0.0936 0.1785 0.3279 0.066 Uiso 1 1 calc R U . . .
H3N2 H -0.0917 0.1369 0.3838 0.066 Uiso 1 1 calc R U . . .
H3N3 H -0.1467 0.1284 0.3136 0.066 Uiso 1 1 calc R U . . .
C4 C 0.06683(16) -0.1542(2) 0.41685(18) 0.0373(10) Uani 1 1 d . . . . .
H4 H 0.0678 -0.1989 0.4073 0.045 Uiso 1 1 calc R U . . .
C4N C -0.08207(17) 0.0161(2) 0.34452(17) 0.0394(10) Uani 1 1 d . . . . .
H4N1 H -0.0589 -0.0162 0.3363 0.059 Uiso 1 1 calc R U . . .
H4N2 H -0.1251 0.0062 0.3188 0.059 Uiso 1 1 calc R U . . .
H4N3 H -0.0701 0.0147 0.3890 0.059 Uiso 1 1 calc R U . . .
C5 C 0.04651(16) -0.1362(2) 0.45806(18) 0.0369(10) Uani 1 1 d . . . . .
H5 H 0.0342 -0.1687 0.4766 0.044 Uiso 1 1 calc R U . . .
C5N C 0.25505(15) 0.23405(18) 0.60841(17) 0.0315(9) Uani 1 1 d . . . . .
H5N1 H 0.2301 0.2524 0.5663 0.047 Uiso 1 1 calc R U . . .
H5N2 H 0.2901 0.2621 0.6328 0.047 Uiso 1 1 calc R U . . .
H5N3 H 0.2314 0.2314 0.6294 0.047 Uiso 1 1 calc R U . . .
C6 C 0.04446(16) -0.06912(18) 0.47191(17) 0.0321(9) Uani 1 1 d . . . . .
H6 H 0.0304 -0.0571 0.4994 0.039 Uiso 1 1 calc R U . . .
C6N C 0.31448(16) 0.1360(2) 0.66716(16) 0.0333(9) Uani 1 1 d . . . . .
H6N1 H 0.3269 0.0923 0.6621 0.050 Uiso 1 1 calc R U . . .
H6N2 H 0.2914 0.1328 0.6888 0.050 Uiso 1 1 calc R U . . .
H6N3 H 0.3502 0.1630 0.6920 0.050 Uiso 1 1 calc R U . . .
C7 C 0.06325(15) -0.02024(18) 0.44484(16) 0.0269(8) Uani 1 1 d . . . . .
C1N C 0.24661(17) -0.05249(19) 0.54888(18) 0.0379(10) Uani 1 1 d . . . . .
H7N1 H 0.2445 -0.0241 0.5796 0.057 Uiso 1 1 calc R U . . .
H7N2 H 0.2825 -0.0801 0.5702 0.057 Uiso 1 1 calc R U . . .
H7N3 H 0.2106 -0.0801 0.5285 0.057 Uiso 1 1 calc R U . . .
C8 C 0.16309(16) 0.06040(18) 0.58726(16) 0.0285(8) Uani 1 1 d . . . . .
H8A H 0.1975 0.0370 0.6219 0.034 Uiso 1 1 calc R U . . .
H8B H 0.1282 0.0304 0.5684 0.034 Uiso 1 1 calc R U . . .
C8N C -0.19360(17) 0.2458(2) 0.02648(19) 0.0422(11) Uani 1 1 d . . . . .
H8N1 H -0.1584 0.2171 0.0430 0.063 Uiso 1 1 calc R U . . .
H8N2 H -0.1906 0.2734 0.0604 0.063 Uiso 1 1 calc R U . . .
H8N3 H -0.1952 0.2735 -0.0067 0.063 Uiso 1 1 calc R U . . .
C9 C 0.14781(15) 0.12017(18) 0.61354(16) 0.0272(8) Uani 1 1 d . . . . .
C10 C 0.17334(16) 0.1294(2) 0.67921(17) 0.0323(9) Uani 1 1 d . . . . .
H10 H 0.2006 0.0979 0.7074 0.039 Uiso 1 1 calc R U . . .
C11 C 0.15894(17) 0.1847(2) 0.70343(17) 0.0371(10) Uani 1 1 d . . . . .
H11 H 0.1762 0.1901 0.7474 0.045 Uiso 1 1 calc R U . . .
C12 C 0.11893(18) 0.2312(2) 0.66179(18) 0.0384(10) Uani 1 1 d . . . . .
H12 H 0.1085 0.2680 0.6778 0.046 Uiso 1 1 calc R U . . .
C13 C 0.09376(16) 0.22414(19) 0.59603(17) 0.0316(9) Uani 1 1 d . . . . .
H13 H 0.0674 0.2567 0.5685 0.038 Uiso 1 1 calc R U . . .
C14 C 0.10758(15) 0.16849(18) 0.57068(16) 0.0247(8) Uani 1 1 d . . . . .
C15 C 0.13585(15) 0.24592(17) 0.44660(15) 0.0254(8) Uani 1 1 d . . . . .
H15A H 0.1671 0.2798 0.4579 0.030 Uiso 1 1 calc R U . . .
H15B H 0.1131 0.2566 0.4680 0.030 Uiso 1 1 calc R U . . .
C16 C 0.09259(14) 0.24626(17) 0.37479(16) 0.0239(8) Uani 1 1 d . . . . .
C17 C 0.09420(15) 0.29422(18) 0.33516(16) 0.0271(8) Uani 1 1 d . . . . .
H17 H 0.1205 0.3303 0.3533 0.033 Uiso 1 1 calc R U . . .
C18 C 0.05792(15) 0.29058(19) 0.26921(17) 0.0304(9) Uani 1 1 d . . . . .
H18 H 0.0595 0.3237 0.2431 0.037 Uiso 1 1 calc R U . . .
C19 C 0.01939(16) 0.23663(19) 0.24316(17) 0.0322(9) Uani 1 1 d . . . . .
H19 H -0.0046 0.2328 0.1988 0.039 Uiso 1 1 calc R U . . .
C20 C 0.01559(15) 0.18813(18) 0.28147(16) 0.0287(8) Uani 1 1 d . . . . .
H20 H -0.0111 0.1524 0.2628 0.034 Uiso 1 1 calc R U . . .
C21 C 0.05177(14) 0.19252(18) 0.34830(15) 0.0244(8) Uani 1 1 d . . . . .
C22 C -0.20443(15) -0.05668(18) 0.13767(16) 0.0280(8) Uani 1 1 d . . . . .
H22A H -0.1629 -0.0619 0.1735 0.034 Uiso 1 1 calc R U . . .
H22B H -0.2150 -0.0966 0.1116 0.034 Uiso 1 1 calc R U . . .
C23 C -0.24771(15) -0.04879(19) 0.16255(16) 0.0278(8) Uani 1 1 d . . . . .
C24 C -0.29114(16) -0.0963(2) 0.15448(17) 0.0333(9) Uani 1 1 d . . . . .
H24 H -0.2938 -0.1357 0.1330 0.040 Uiso 1 1 calc R U . . .
C25 C -0.33071(18) -0.0861(2) 0.17800(18) 0.0421(10) Uani 1 1 d . . . . .
H25 H -0.3596 -0.1184 0.1721 0.051 Uiso 1 1 calc R U . . .
C26 C -0.32694(17) -0.0278(2) 0.21021(18) 0.0392(10) Uani 1 1 d . . . . .
H26 H -0.3528 -0.0210 0.2267 0.047 Uiso 1 1 calc R U . . .
C27 C -0.28437(16) 0.0209(2) 0.21795(17) 0.0356(9) Uani 1 1 d . . . . .
H27 H -0.2826 0.0605 0.2387 0.043 Uiso 1 1 calc R U . . .
C28 C -0.24430(15) 0.01073(19) 0.19480(16) 0.0292(9) Uani 1 1 d . . . . .
C29 C -0.27952(15) 0.16128(19) 0.11542(18) 0.0341(9) Uani 1 1 d . . . . .
H29A H -0.2836 0.1361 0.1473 0.041 Uiso 1 1 calc R U . . .
H29B H -0.3203 0.1748 0.0823 0.041 Uiso 1 1 calc R U . . .
C30 C -0.24130(15) 0.22253(18) 0.14649(16) 0.0293(9) Uani 1 1 d . . . . .
C31 C -0.26975(17) 0.28398(19) 0.13896(17) 0.0340(9) Uani 1 1 d . . . . .
H31 H -0.3123 0.2867 0.1146 0.041 Uiso 1 1 calc R U . . .
C32 C -0.23623(17) 0.3408(2) 0.16679(18) 0.0362(9) Uani 1 1 d . . . . .
H32 H -0.2557 0.3815 0.1620 0.043 Uiso 1 1 calc R U . . .
C33 C -0.17255(17) 0.3359(2) 0.20227(18) 0.0358(9) Uani 1 1 d . . . . .
H33 H -0.1493 0.3739 0.2215 0.043 Uiso 1 1 calc R U . . .
C34 C -0.14352(16) 0.27609(19) 0.20940(17) 0.0322(9) Uani 1 1 d . . . . .
H34 H -0.1008 0.2743 0.2327 0.039 Uiso 1 1 calc R U . . .
C35 C -0.17703(15) 0.21758(19) 0.18215(16) 0.0289(9) Uani 1 1 d . . . . .
C36 C -0.08615(15) 0.11622(19) 0.11522(16) 0.0311(9) Uani 1 1 d . . . . .
H36A H -0.0747 0.1505 0.1476 0.037 Uiso 1 1 calc R U . . .
H36B H -0.0780 0.1331 0.0826 0.037 Uiso 1 1 calc R U . . .
C37 C -0.04825(15) 0.05495(19) 0.14519(16) 0.0288(9) Uani 1 1 d . . . . .
C38 C -0.00432(16) 0.0308(2) 0.13126(18) 0.0362(10) Uani 1 1 d . . . . .
H38 H 0.0042 0.0547 0.1037 0.043 Uiso 1 1 calc R U . . .
C39 C 0.02681(16) -0.0285(2) 0.15790(19) 0.0410(11) Uani 1 1 d . . . . .
H39 H 0.0555 -0.0446 0.1478 0.049 Uiso 1 1 calc R U . . .
C40 C 0.01449(16) -0.0630(2) 0.19959(18) 0.0388(10) Uani 1 1 d . . . . .
H40 H 0.0348 -0.1028 0.2172 0.047 Uiso 1 1 calc R U . . .
C41 C -0.02783(15) -0.03906(19) 0.21581(17) 0.0331(9) Uani 1 1 d . . . . .
H41 H -0.0351 -0.0624 0.2446 0.040 Uiso 1 1 calc R U . . .
C42 C -0.05919(15) 0.02001(18) 0.18865(16) 0.0282(9) Uani 1 1 d . . . . .
O1 O 0.14376(9) 0.06246(11) 0.41977(10) 0.0239(5) Uani 1 1 d . . . . .
O2 O 0.05647(10) 0.04470(12) 0.45513(11) 0.0255(5) Uani 1 1 d . . . . .
O3 O 0.17839(9) 0.07888(12) 0.53984(10) 0.0244(5) Uani 1 1 d . . . . .
O4 O 0.08060(10) 0.16287(11) 0.50639(10) 0.0244(5) Uani 1 1 d . . . . .
O5 O 0.16447(9) 0.18284(11) 0.46789(10) 0.0232(5) Uani 1 1 d . . . . .
O6 O 0.04564(9) 0.14611(12) 0.38528(10) 0.0244(5) Uani 1 1 d . . . . .
O7 O -0.20664(10) -0.00077(11) 0.10028(10) 0.0250(5) Uani 1 1 d . . . . .
O8 O -0.20201(10) 0.05760(12) 0.20499(11) 0.0291(6) Uani 1 1 d . . . . .
O9 O -0.25323(10) 0.11943(12) 0.08760(11) 0.0300(6) Uani 1 1 d . . . . .
O10 O -0.14583(10) 0.16036(12) 0.19160(11) 0.0304(6) Uani 1 1 d . . . . .
O11 O -0.15037(10) 0.10175(12) 0.08688(10) 0.0271(6) Uani 1 1 d . . . . .
O12 O -0.09985(9) 0.04339(12) 0.20509(10) 0.0258(6) Uani 1 1 d . . . . .
Ge1 Ge 0.11251(2) 0.11230(2) 0.46331(2) 0.02256(11) Uani 1 1 d . . . . .
Ge2 Ge -0.17754(2) 0.08051(2) 0.14461(2) 0.02541(11) Uani 1 1 d . . . . .
Cl1 Cl -0.08379(5) 0.31462(6) 0.38068(6) 0.0637(4) Uani 1 1 d . . . . .
Cl2 Cl 0.02018(6) 0.37334(6) 0.49270(5) 0.0620(3) Uani 1 1 d . . . . .
N4 N -0.33134(13) 0.00674(16) 0.00484(14) 0.0288(7) Uani 1 1 d D . . . .
N2 N -0.07000(13) 0.08327(17) 0.32830(14) 0.0306(7) Uani 1 1 d D . . . .
N3 N 0.27576(13) 0.16668(16) 0.60326(13) 0.0265(7) Uani 1 1 d D . . . .
N1 N 0.2500 -0.0112(2) 0.5000 0.0316(11) Uani 1 2 d DS T P . .
N5 N -0.2500 0.2051(2) 0.0000 0.0339(11) Uani 1 2 d DS T P . .
H9N H -0.2911(9) 0.0099(17) 0.0362(13) 0.028(10) Uiso 1 1 d D . . . .
H10N H -0.3327(19) 0.0346(18) -0.0256(16) 0.054(14) Uiso 1 1 d D . . . .
H3N H -0.0820(15) 0.0812(18) 0.2867(10) 0.028(10) Uiso 1 1 d D . . . .
H4N H -0.0287(9) 0.0935(19) 0.3509(16) 0.044(12) Uiso 1 1 d D . . . .
H5N H 0.2433(11) 0.1386(13) 0.5808(13) 0.012(8) Uiso 1 1 d D . . . .
H6N H 0.2971(14) 0.1704(18) 0.5817(15) 0.032(11) Uiso 1 1 d D . . . .
H1N H 0.2850(13) 0.0128(19) 0.521(2) 0.068(16) Uiso 1 1 d D . . . .
H8N H -0.2514(16) 0.1753(14) -0.0289(13) 0.029(10) Uiso 1 1 d 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
C1 O1 1.432(4) . ?
C1 C2 1.504(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1C Cl1 1.758(4) . ?
C1C Cl2 1.763(4) . ?
C1C H1C1 0.9700 . ?
C1C H1C2 0.9700 . ?
C7N N4 1.479(5) . ?
C7N H1N1 0.9600 . ?
C7N H1N2 0.9600 . ?
C7N H1N3 0.9600 . ?
C2 C3 1.388(5) . ?
C2 C7 1.416(5) . ?
C9N N4 1.485(5) . ?
C9N H2N1 0.9600 . ?
C9N H2N2 0.9600 . ?
C9N H2N3 0.9600 . ?
C3 C4 1.393(5) . ?
C3 H3 0.9300 . ?
C3N N2 1.464(5) . ?
C3N H3N1 0.9600 . ?
C3N H3N2 0.9600 . ?
C3N H3N3 0.9600 . ?
C4 C5 1.379(6) . ?
C4 H4 0.9300 . ?
C4N N2 1.478(5) . ?
C4N H4N1 0.9600 . ?
C4N H4N2 0.9600 . ?
C4N H4N3 0.9600 . ?
C5 C6 1.394(5) . ?
C5 H5 0.9300 . ?
C5N N3 1.478(5) . ?
C5N H5N1 0.9600 . ?
C5N H5N2 0.9600 . ?
C5N H5N3 0.9600 . ?
C6 C7 1.389(5) . ?
C6 H6 0.9300 . ?
C6N N3 1.482(4) . ?
C6N H6N1 0.9600 . ?
C6N H6N2 0.9600 . ?
C6N H6N3 0.9600 . ?
C7 O2 1.354(4) . ?
C1N N1 1.480(4) . ?
C1N H7N1 0.9600 . ?
C1N H7N2 0.9600 . ?
C1N H7N3 0.9600 . ?
C8 O3 1.431(4) . ?
C8 C9 1.497(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8N N5 1.478(4) . ?
C8N H8N1 0.9600 . ?
C8N H8N2 0.9600 . ?
C8N H8N3 0.9600 . ?
C9 C10 1.392(5) . ?
C9 C14 1.408(5) . ?
C10 C11 1.385(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.371(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.390(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.401(5) . ?
C13 H13 0.9300 . ?
C14 O4 1.350(4) . ?
C15 O5 1.420(4) . ?
C15 C16 1.514(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.373(5) . ?
C16 C21 1.403(5) . ?
C17 C18 1.382(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.377(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.380(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.400(4) . ?
C20 H20 0.9300 . ?
C21 O6 1.353(4) . ?
C22 O7 1.424(4) . ?
C22 C23 1.498(5) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.391(5) . ?
C23 C28 1.406(5) . ?
C24 C25 1.391(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.383(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.393(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.395(5) . ?
C27 H27 0.9300 . ?
C28 O8 1.349(4) . ?
C29 O9 1.431(4) . ?
C29 C30 1.508(5) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.392(5) . ?
C30 C35 1.404(5) . ?
C31 C32 1.376(5) . ?
C31 H31 0.9300 . ?
C32 C33 1.391(5) . ?
C32 H32 0.9300 . ?
C33 C34 1.372(5) . ?
C33 H33 0.9300 . ?
C34 C35 1.402(5) . ?
C34 H34 0.9300 . ?
C35 O10 1.345(4) . ?
C36 O11 1.434(4) . ?
C36 C37 1.501(5) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 C38 1.398(5) . ?
C37 C42 1.402(5) . ?
C38 C39 1.392(6) . ?
C38 H38 0.9300 . ?
C39 C40 1.381(6) . ?
C39 H39 0.9300 . ?
C40 C41 1.395(5) . ?
C40 H40 0.9300 . ?
C41 C42 1.392(5) . ?
C41 H41 0.9300 . ?
C42 O12 1.357(4) . ?
O1 Ge1 1.889(2) . ?
O2 Ge1 1.897(2) . ?
O3 Ge1 1.879(2) . ?
O4 Ge1 1.900(2) . ?
O5 Ge1 1.895(2) . ?
O6 Ge1 1.911(2) . ?
O7 Ge2 1.886(2) . ?
O8 Ge2 1.906(2) . ?
O9 Ge2 1.870(2) . ?
O10 Ge2 1.893(2) . ?
O11 Ge2 1.888(2) . ?
O12 Ge2 1.908(2) . ?
N4 H9N 0.913(18) . ?
N4 H10N 0.910(19) . ?
N2 H3N 0.892(18) . ?
N2 H4N 0.922(19) . ?
N3 H5N 0.914(17) . ?
N3 H6N 0.922(18) . ?
N1 C1N 1.481(4) 2_556 ?
N1 H1N 0.905(19) . ?
N5 C8N 1.478(4) 2_455 ?
N5 H8N 0.906(17) . ?

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
O1 C1 C2 111.7(3) . . ?
O1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
O1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?
Cl1 C1C Cl2 111.1(2) . . ?
Cl1 C1C H1C1 109.4 . . ?
Cl2 C1C H1C1 109.4 . . ?
Cl1 C1C H1C2 109.4 . . ?
Cl2 C1C H1C2 109.4 . . ?
H1C1 C1C H1C2 108.0 . . ?
N4 C7N H1N1 109.5 . . ?
N4 C7N H1N2 109.5 . . ?
H1N1 C7N H1N2 109.5 . . ?
N4 C7N H1N3 109.5 . . ?
H1N1 C7N H1N3 109.5 . . ?
H1N2 C7N H1N3 109.5 . . ?
C3 C2 C7 118.7(4) . . ?
C3 C2 C1 123.2(3) . . ?
C7 C2 C1 118.1(3) . . ?
N4 C9N H2N1 109.5 . . ?
N4 C9N H2N2 109.5 . . ?
H2N1 C9N H2N2 109.5 . . ?
N4 C9N H2N3 109.5 . . ?
H2N1 C9N H2N3 109.5 . . ?
H2N2 C9N H2N3 109.5 . . ?
C2 C3 C4 121.0(4) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
N2 C3N H3N1 109.5 . . ?
N2 C3N H3N2 109.5 . . ?
H3N1 C3N H3N2 109.5 . . ?
N2 C3N H3N3 109.5 . . ?
H3N1 C3N H3N3 109.5 . . ?
H3N2 C3N H3N3 109.5 . . ?
C5 C4 C3 120.1(4) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
N2 C4N H4N1 109.5 . . ?
N2 C4N H4N2 109.5 . . ?
H4N1 C4N H4N2 109.5 . . ?
N2 C4N H4N3 109.5 . . ?
H4N1 C4N H4N3 109.5 . . ?
H4N2 C4N H4N3 109.5 . . ?
C4 C5 C6 120.0(4) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
N3 C5N H5N1 109.5 . . ?
N3 C5N H5N2 109.5 . . ?
H5N1 C5N H5N2 109.5 . . ?
N3 C5N H5N3 109.5 . . ?
H5N1 C5N H5N3 109.5 . . ?
H5N2 C5N H5N3 109.5 . . ?
C7 C6 C5 120.4(4) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
N3 C6N H6N1 109.5 . . ?
N3 C6N H6N2 109.5 . . ?
H6N1 C6N H6N2 109.5 . . ?
N3 C6N H6N3 109.5 . . ?
H6N1 C6N H6N3 109.5 . . ?
H6N2 C6N H6N3 109.5 . . ?
O2 C7 C6 119.3(3) . . ?
O2 C7 C2 120.7(3) . . ?
C6 C7 C2 119.8(3) . . ?
N1 C1N H7N1 109.5 . . ?
N1 C1N H7N2 109.5 . . ?
H7N1 C1N H7N2 109.5 . . ?
N1 C1N H7N3 109.5 . . ?
H7N1 C1N H7N3 109.5 . . ?
H7N2 C1N H7N3 109.5 . . ?
O3 C8 C9 111.3(3) . . ?
O3 C8 H8A 109.4 . . ?
C9 C8 H8A 109.4 . . ?
O3 C8 H8B 109.4 . . ?
C9 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
N5 C8N H8N1 109.5 . . ?
N5 C8N H8N2 109.5 . . ?
H8N1 C8N H8N2 109.5 . . ?
N5 C8N H8N3 109.5 . . ?
H8N1 C8N H8N3 109.5 . . ?
H8N2 C8N H8N3 109.5 . . ?
C10 C9 C14 119.6(3) . . ?
C10 C9 C8 121.4(3) . . ?
C14 C9 C8 119.0(3) . . ?
C11 C10 C9 121.3(4) . . ?
C11 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
C12 C11 C10 119.2(3) . . ?
C12 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
C11 C12 C13 120.8(4) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C12 C13 C14 120.7(4) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
O4 C14 C13 118.6(3) . . ?
O4 C14 C9 123.1(3) . . ?
C13 C14 C9 118.3(3) . . ?
O5 C15 C16 111.1(3) . . ?
O5 C15 H15A 109.4 . . ?
C16 C15 H15A 109.4 . . ?
O5 C15 H15B 109.4 . . ?
C16 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C17 C16 C21 119.6(3) . . ?
C17 C16 C15 123.0(3) . . ?
C21 C16 C15 117.3(3) . . ?
C16 C17 C18 122.1(3) . . ?
C16 C17 H17 118.9 . . ?
C18 C17 H17 118.9 . . ?
C19 C18 C17 118.2(3) . . ?
C19 C18 H18 120.9 . . ?
C17 C18 H18 120.9 . . ?
C18 C19 C20 121.4(3) . . ?
C18 C19 H19 119.3 . . ?
C20 C19 H19 119.3 . . ?
C19 C20 C21 120.3(3) . . ?
C19 C20 H20 119.9 . . ?
C21 C20 H20 119.9 . . ?
O6 C21 C20 119.6(3) . . ?
O6 C21 C16 122.0(3) . . ?
C20 C21 C16 118.4(3) . . ?
O7 C22 C23 111.6(3) . . ?
O7 C22 H22A 109.3 . . ?
C23 C22 H22A 109.3 . . ?
O7 C22 H22B 109.3 . . ?
C23 C22 H22B 109.3 . . ?
H22A C22 H22B 108.0 . . ?
C24 C23 C28 119.0(4) . . ?
C24 C23 C22 123.6(4) . . ?
C28 C23 C22 117.4(3) . . ?
C23 C24 C25 121.2(4) . . ?
C23 C24 H24 119.4 . . ?
C25 C24 H24 119.4 . . ?
C26 C25 C24 119.7(4) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C25 C26 C27 119.9(4) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C26 C27 C28 120.6(4) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
O8 C28 C27 119.4(3) . . ?
O8 C28 C23 121.1(3) . . ?
C27 C28 C23 119.5(4) . . ?
O9 C29 C30 112.4(3) . . ?
O9 C29 H29A 109.1 . . ?
C30 C29 H29A 109.1 . . ?
O9 C29 H29B 109.1 . . ?
C30 C29 H29B 109.1 . . ?
H29A C29 H29B 107.9 . . ?
C31 C30 C35 120.2(3) . . ?
C31 C30 C29 120.0(3) . . ?
C35 C30 C29 119.9(3) . . ?
C32 C31 C30 121.4(3) . . ?
C32 C31 H31 119.3 . . ?
C30 C31 H31 119.3 . . ?
C31 C32 C33 118.5(4) . . ?
C31 C32 H32 120.8 . . ?
C33 C32 H32 120.8 . . ?
C34 C33 C32 121.0(4) . . ?
C34 C33 H33 119.5 . . ?
C32 C33 H33 119.5 . . ?
C33 C34 C35 121.2(3) . . ?
C33 C34 H34 119.4 . . ?
C35 C34 H34 119.4 . . ?
O10 C35 C34 118.3(3) . . ?
O10 C35 C30 124.1(3) . . ?
C34 C35 C30 117.7(3) . . ?
O11 C36 C37 110.8(3) . . ?
O11 C36 H36A 109.5 . . ?
C37 C36 H36A 109.5 . . ?
O11 C36 H36B 109.5 . . ?
C37 C36 H36B 109.5 . . ?
H36A C36 H36B 108.1 . . ?
C38 C37 C42 119.1(3) . . ?
C38 C37 C36 123.9(4) . . ?
C42 C37 C36 117.0(3) . . ?
C39 C38 C37 121.1(4) . . ?
C39 C38 H38 119.5 . . ?
C37 C38 H38 119.5 . . ?
C40 C39 C38 119.0(4) . . ?
C40 C39 H39 120.5 . . ?
C38 C39 H39 120.5 . . ?
C39 C40 C41 121.2(4) . . ?
C39 C40 H40 119.4 . . ?
C41 C40 H40 119.4 . . ?
C42 C41 C40 119.6(4) . . ?
C42 C41 H41 120.2 . . ?
C40 C41 H41 120.2 . . ?
O12 C42 C41 119.3(3) . . ?
O12 C42 C37 120.7(3) . . ?
C41 C42 C37 120.0(3) . . ?
C1 O1 Ge1 116.3(2) . . ?
C7 O2 Ge1 123.5(2) . . ?
C8 O3 Ge1 114.78(19) . . ?
C14 O4 Ge1 124.7(2) . . ?
C15 O5 Ge1 115.83(19) . . ?
C21 O6 Ge1 123.94(19) . . ?
C22 O7 Ge2 116.25(19) . . ?
C28 O8 Ge2 124.1(2) . . ?
C29 O9 Ge2 116.2(2) . . ?
C35 O10 Ge2 126.0(2) . . ?
C36 O11 Ge2 115.9(2) . . ?
C42 O12 Ge2 123.1(2) . . ?
O3 Ge1 O1 87.07(10) . . ?
O3 Ge1 O5 88.14(10) . . ?
O1 Ge1 O5 87.57(10) . . ?
O3 Ge1 O2 95.12(10) . . ?
O1 Ge1 O2 93.53(10) . . ?
O5 Ge1 O2 176.60(10) . . ?
O3 Ge1 O4 93.45(10) . . ?
O1 Ge1 O4 179.47(10) . . ?
O5 Ge1 O4 92.31(10) . . ?
O2 Ge1 O4 86.55(10) . . ?
O3 Ge1 O6 179.77(11) . . ?
O1 Ge1 O6 92.70(10) . . ?
O5 Ge1 O6 91.83(10) . . ?
O2 Ge1 O6 84.91(10) . . ?
O4 Ge1 O6 86.78(10) . . ?
O9 Ge2 O7 89.04(10) . . ?
O9 Ge2 O11 88.72(11) . . ?
O7 Ge2 O11 87.59(10) . . ?
O9 Ge2 O10 93.05(10) . . ?
O7 Ge2 O10 177.86(10) . . ?
O11 Ge2 O10 92.93(11) . . ?
O9 Ge2 O8 93.45(11) . . ?
O7 Ge2 O8 92.43(10) . . ?
O11 Ge2 O8 177.83(10) . . ?
O10 Ge2 O8 86.97(11) . . ?
O9 Ge2 O12 177.82(10) . . ?
O7 Ge2 O12 92.97(10) . . ?
O11 Ge2 O12 92.22(10) . . ?
O10 Ge2 O12 84.94(10) . . ?
O8 Ge2 O12 85.61(10) . . ?
C7N N4 C9N 112.4(3) . . ?
C7N N4 H9N 108(2) . . ?
C9N N4 H9N 111(2) . . ?
C7N N4 H10N 111(3) . . ?
C9N N4 H10N 112(3) . . ?
H9N N4 H10N 102(3) . . ?
C3N N2 C4N 113.7(3) . . ?
C3N N2 H3N 110(2) . . ?
C4N N2 H3N 105(2) . . ?
C3N N2 H4N 108(2) . . ?
C4N N2 H4N 112(2) . . ?
H3N N2 H4N 109(3) . . ?
C5N N3 C6N 111.6(3) . . ?
C5N N3 H5N 111.4(19) . . ?
C6N N3 H5N 106.5(19) . . ?
C5N N3 H6N 108(2) . . ?
C6N N3 H6N 111(2) . . ?
H5N N3 H6N 108(3) . . ?
C1N N1 C1N 111.9(4) . 2_556 ?
C1N N1 H1N 106(3) . . ?
C1N N1 H1N 109(3) 2_556 . ?
C8N N5 C8N 112.7(4) . 2_455 ?
C8N N5 H8N 111(2) . . ?
C8N N5 H8N 112(2) 2_455 . ?

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
O1 C1 C2 C3 -131.4(3) . . . . ?
O1 C1 C2 C7 50.0(4) . . . . ?
C7 C2 C3 C4 0.7(5) . . . . ?
C1 C2 C3 C4 -177.9(3) . . . . ?
C2 C3 C4 C5 -0.8(5) . . . . ?
C3 C4 C5 C6 0.7(5) . . . . ?
C4 C5 C6 C7 -0.5(5) . . . . ?
C5 C6 C7 O2 175.0(3) . . . . ?
C5 C6 C7 C2 0.4(5) . . . . ?
C3 C2 C7 O2 -175.0(3) . . . . ?
C1 C2 C7 O2 3.6(4) . . . . ?
C3 C2 C7 C6 -0.5(5) . . . . ?
C1 C2 C7 C6 178.2(3) . . . . ?
O3 C8 C9 C10 -132.1(3) . . . . ?
O3 C8 C9 C14 46.7(4) . . . . ?
C14 C9 C10 C11 1.4(5) . . . . ?
C8 C9 C10 C11 -179.7(3) . . . . ?
C9 C10 C11 C12 -0.3(6) . . . . ?
C10 C11 C12 C13 -1.2(6) . . . . ?
C11 C12 C13 C14 1.5(6) . . . . ?
C12 C13 C14 O4 178.1(3) . . . . ?
C12 C13 C14 C9 -0.3(5) . . . . ?
C10 C9 C14 O4 -179.5(3) . . . . ?
C8 C9 C14 O4 1.7(5) . . . . ?
C10 C9 C14 C13 -1.1(5) . . . . ?
C8 C9 C14 C13 -180.0(3) . . . . ?
O5 C15 C16 C17 -129.1(3) . . . . ?
O5 C15 C16 C21 47.2(4) . . . . ?
C21 C16 C17 C18 -1.9(5) . . . . ?
C15 C16 C17 C18 174.3(3) . . . . ?
C16 C17 C18 C19 -0.3(5) . . . . ?
C17 C18 C19 C20 1.6(6) . . . . ?
C18 C19 C20 C21 -0.7(6) . . . . ?
C19 C20 C21 O6 177.2(3) . . . . ?
C19 C20 C21 C16 -1.5(5) . . . . ?
C17 C16 C21 O6 -175.9(3) . . . . ?
C15 C16 C21 O6 7.7(5) . . . . ?
C17 C16 C21 C20 2.7(5) . . . . ?
C15 C16 C21 C20 -173.7(3) . . . . ?
O7 C22 C23 C24 127.6(3) . . . . ?
O7 C22 C23 C28 -51.3(4) . . . . ?
C28 C23 C24 C25 -0.4(5) . . . . ?
C22 C23 C24 C25 -179.3(3) . . . . ?
C23 C24 C25 C26 -0.2(5) . . . . ?
C24 C25 C26 C27 1.1(6) . . . . ?
C25 C26 C27 C28 -1.5(5) . . . . ?
C26 C27 C28 O8 -177.6(3) . . . . ?
C26 C27 C28 C23 1.0(5) . . . . ?
C24 C23 C28 O8 178.5(3) . . . . ?
C22 C23 C28 O8 -2.5(5) . . . . ?
C24 C23 C28 C27 0.0(5) . . . . ?
C22 C23 C28 C27 178.9(3) . . . . ?
O9 C29 C30 C31 138.4(3) . . . . ?
O9 C29 C30 C35 -40.6(5) . . . . ?
C35 C30 C31 C32 -1.1(6) . . . . ?
C29 C30 C31 C32 179.8(4) . . . . ?
C30 C31 C32 C33 0.9(6) . . . . ?
C31 C32 C33 C34 0.2(6) . . . . ?
C32 C33 C34 C35 -1.2(6) . . . . ?
C33 C34 C35 O10 -179.2(3) . . . . ?
C33 C34 C35 C30 1.0(6) . . . . ?
C31 C30 C35 O10 -179.7(3) . . . . ?
C29 C30 C35 O10 -0.7(6) . . . . ?
C31 C30 C35 C34 0.1(5) . . . . ?
C29 C30 C35 C34 179.2(3) . . . . ?
O11 C36 C37 C38 126.2(3) . . . . ?
O11 C36 C37 C42 -52.5(4) . . . . ?
C42 C37 C38 C39 2.5(5) . . . . ?
C36 C37 C38 C39 -176.2(3) . . . . ?
C37 C38 C39 C40 -1.1(5) . . . . ?
C38 C39 C40 C41 -0.7(5) . . . . ?
C39 C40 C41 C42 1.2(5) . . . . ?
C40 C41 C42 O12 -179.3(3) . . . . ?
C40 C41 C42 C37 0.2(5) . . . . ?
C38 C37 C42 O12 177.5(3) . . . . ?
C36 C37 C42 O12 -3.7(5) . . . . ?
C38 C37 C42 C41 -2.0(5) . . . . ?
C36 C37 C42 C41 176.8(3) . . . . ?
C2 C1 O1 Ge1 -64.6(3) . . . . ?
C6 C7 O2 Ge1 145.6(2) . . . . ?
C2 C7 O2 Ge1 -39.8(4) . . . . ?
C9 C8 O3 Ge1 -68.5(3) . . . . ?
C13 C14 O4 Ge1 156.5(2) . . . . ?
C9 C14 O4 Ge1 -25.2(4) . . . . ?
C16 C15 O5 Ge1 -69.3(3) . . . . ?
C20 C21 O6 Ge1 143.1(3) . . . . ?
C16 C21 O6 Ge1 -38.3(4) . . . . ?
C23 C22 O7 Ge2 66.8(3) . . . . ?
C27 C28 O8 Ge2 -143.1(3) . . . . ?
C23 C28 O8 Ge2 38.4(4) . . . . ?
C30 C29 O9 Ge2 64.8(4) . . . . ?
C34 C35 O10 Ge2 -164.0(3) . . . . ?
C30 C35 O10 Ge2 15.9(5) . . . . ?
C37 C36 O11 Ge2 67.9(3) . . . . ?
C41 C42 O12 Ge2 -138.4(3) . . . . ?
C37 C42 O12 Ge2 42.2(4) . . . . ?
C8 O3 Ge1 O1 -139.3(2) . . . . ?
C8 O3 Ge1 O5 133.0(2) . . . . ?
C8 O3 Ge1 O2 -46.0(2) . . . . ?
C8 O3 Ge1 O4 40.8(2) . . . . ?
C1 O1 Ge1 O3 124.0(2) . . . . ?
C1 O1 Ge1 O5 -147.7(2) . . . . ?
C1 O1 Ge1 O2 29.0(2) . . . . ?
C1 O1 Ge1 O6 -56.0(2) . . . . ?
C15 O5 Ge1 O3 -143.7(2) . . . . ?
C15 O5 Ge1 O1 129.2(2) . . . . ?
C15 O5 Ge1 O4 -50.3(2) . . . . ?
C15 O5 Ge1 O6 36.6(2) . . . . ?
C7 O2 Ge1 O3 -65.6(2) . . . . ?
C7 O2 Ge1 O1 21.8(2) . . . . ?
C7 O2 Ge1 O4 -158.8(2) . . . . ?
C7 O2 Ge1 O6 114.2(2) . . . . ?
C14 O4 Ge1 O3 4.2(3) . . . . ?
C14 O4 Ge1 O5 -84.1(3) . . . . ?
C14 O4 Ge1 O2 99.1(3) . . . . ?
C14 O4 Ge1 O6 -175.8(3) . . . . ?
C29 O9 Ge2 O7 135.8(2) . . . . ?
C29 O9 Ge2 O11 -136.6(2) . . . . ?
C29 O9 Ge2 O10 -43.7(2) . . . . ?
C29 O9 Ge2 O8 43.4(2) . . . . ?
C22 O7 Ge2 O9 -124.1(2) . . . . ?
C22 O7 Ge2 O11 147.2(2) . . . . ?
C22 O7 Ge2 O8 -30.7(2) . . . . ?
C22 O7 Ge2 O12 55.1(2) . . . . ?
C36 O11 Ge2 O9 148.1(2) . . . . ?
C36 O11 Ge2 O7 -122.8(2) . . . . ?
C36 O11 Ge2 O10 55.1(2) . . . . ?
C36 O11 Ge2 O12 -29.9(2) . . . . ?
C35 O10 Ge2 O9 4.8(3) . . . . ?
C35 O10 Ge2 O11 93.6(3) . . . . ?
C35 O10 Ge2 O8 -88.5(3) . . . . ?
C35 O10 Ge2 O12 -174.4(3) . . . . ?

_refine_diff_density_max         0.583
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.068

_shelxl_version_number           2013-4

