# 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 
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data_k1p21c
_database_code_depnum_ccdc_archive 'CCDC 1418081'
_audit_update_record             
;
2015-12-01 deposited with the CCDC.
2015-12-14 downloaded from the CCDC.
;
_audit_creation_date             2015-11-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H81 Ge9 Si12, C21 H23 K, C7 H8'
_chemical_formula_sum            'C55 H112 Ge9 K Si12'
_chemical_formula_weight         1802.93
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.8387(9)
_cell_length_b                   20.2949(13)
_cell_length_c                   27.3283(16)
_cell_angle_alpha                90
_cell_angle_beta                 91.2930(10)
_cell_angle_gamma                90
_cell_volume                     8782.3(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9770
_cell_measurement_temperature    150
_cell_measurement_theta_max      22.991
_cell_measurement_theta_min      2.384
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.274
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1020 before and 0.0413 after correction.
The Ratio of minimum to maximum transmission is 0.6955.
The λ/2 correction factor is 0.0000.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3668
_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.136
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            48652
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        23.301
_diffrn_reflns_theta_max         23.301
_diffrn_reflns_theta_min         1.286
_diffrn_ambient_temperature      150.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9218
_reflns_number_total             12586
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.000
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         12586
_refine_ls_number_restraints     130
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0620
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0597P)²+53.4644P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1638
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C201-C200
 1.52 with sigma of 0.02
 Si30-C30A \\sim Si30-C30B \\sim Si30-C30C \\sim Si31-C31A \\sim Si31-C31B
\\sim Si31-C31C
 with sigma of 0.02
 Si32-C32A \\sim Si32-C32B \\sim Si32-C32C \\sim Si33-C33A \\sim Si33-C33B
\\sim Si33-C33C
 with sigma of 0.02
 Si34-C34A \\sim Si34-C34B \\sim Si34-C34C \\sim Si35-C35A \\sim Si35-C35B
\\sim Si35-C35C
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C204 \\sim C203 \\sim C202 \\sim C206 \\sim C201 \\sim C205 \\sim C200: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C204) \\sim Ueq, Uanis(C205) \\sim Ueq, Uanis(C206) \\sim Ueq,
Uanis(C201) \\sim Ueq, Uanis(C202) \\sim Ueq, Uanis(C203) \\sim Ueq,
Uanis(C200) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: Si3(0.5) Si30(0.5) Si31(0.5) Si32(0.5) Si3A(0.5) Si33(0.5)
 Si34(0.5) Si35(0.5) C10A(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C10B(0.5)
 H10D(0.5) H10E(0.5) H10F(0.5) C10C(0.5) H10G(0.5) H10H(0.5) H10I(0.5)
 C20B(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C20A(0.5) H20D(0.5) H20E(0.5)
 H20F(0.5) C20C(0.5) H20G(0.5) H20H(0.5) H20I(0.5) C30B(0.5) H30A(0.5)
 H30B(0.5) H30C(0.5) C30A(0.5) H30D(0.5) H30E(0.5) H30F(0.5) C30C(0.5)
 H30G(0.5) H30H(0.5) H30I(0.5) C31A(0.5) H31A(0.5) H31B(0.5) H31C(0.5)
 C31B(0.5) H31D(0.5) H31E(0.5) H31F(0.5) C31C(0.5) H31G(0.5) H31H(0.5)
 H31I(0.5) C32C(0.5) H32A(0.5) H32B(0.5) H32C(0.5) C32B(0.5) H32D(0.5)
 H32E(0.5) H32F(0.5) C32A(0.5) H32G(0.5) H32H(0.5) H32I(0.5) C33C(0.5)
 H33A(0.5) H33B(0.5) H33C(0.5) C33B(0.5) H33D(0.5) H33E(0.5) H33F(0.5)
 C33A(0.5) H33G(0.5) H33H(0.5) H33I(0.5) C34B(0.5) H34A(0.5) H34B(0.5)
 H34C(0.5) C34A(0.5) H34D(0.5) H34E(0.5) H34F(0.5) C34C(0.5) H34G(0.5)
 H34H(0.5) H34I(0.5) C35B(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C35A(0.5)
 H35D(0.5) H35E(0.5) H35F(0.5) C35C(0.5) H35G(0.5) H35H(0.5) H35I(0.5)
 C100(0.5) H100(0.5) C102(0.5) H102(0.5) C101(0.5) H101(0.5) C105(0.5)
 H105(0.5) C104(0.5) H104(0.5) C103(0.5) C106(0.5) H10J(0.5) H10K(0.5)
 H10L(0.5) C1AA(0.5) H1AA(0.5) C19(0.5) H19(0.5) C2(0.5) H2(0.5) C2AA(0.5)
 H2AA(0.5) C9(0.5) C5(0.5) H5(0.5) C0AA(0.5) H0AA(0.5) H0AB(0.5) H0AC(0.5)
 C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C8(0.5)
 H8A(0.5) H8B(0.5) H8C(0.5) C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C7(0.5) H7A(0.5)
 H7B(0.5) H7C(0.5) C11(0.5) H11J(0.5) H11K(0.5) H11L(0.5)
5.a Ternary CH refined with riding coordinates:
 C112(H112), C111(H111), C110(H110), C121(H121)
5.b Me refined with riding coordinates:
 C10A(H10A,H10B,H10C), C10B(H10D,H10E,H10F), C10C(H10G,H10H,H10I), C11B(H11A,
 H11B,H11C), C11A(H11D,H11E,H11F), C11C(H11G,H11H,H11I), C12B(H12A,H12B,H12C),
 C12A(H12D,H12E,H12F), C12C(H12G,H12H,H12I), C20B(H20A,H20B,H20C), C20A(H20D,
 H20E,H20F), C20C(H20G,H20H,H20I), C21B(H21A,H21B,H21C), C21A(H21D,H21E,H21F),
 C21C(H21G,H21H,H21I), C22C(H22A,H22B,H22C), C22B(H22D,H22E,H22F), C22A(H22G,
 H22H,H22I), C30B(H30A,H30B,H30C), C30A(H30D,H30E,H30F), C30C(H30G,H30H,H30I),
 C31A(H31A,H31B,H31C), C31B(H31D,H31E,H31F), C31C(H31G,H31H,H31I), C32C(H32A,
 H32B,H32C), C32B(H32D,H32E,H32F), C32A(H32G,H32H,H32I), C33C(H33A,H33B,H33C),
 C33B(H33D,H33E,H33F), C33A(H33G,H33H,H33I), C34B(H34A,H34B,H34C), C34A(H34D,
 H34E,H34F), C34C(H34G,H34H,H34I), C35B(H35A,H35B,H35C), C35A(H35D,H35E,H35F),
 C35C(H35G,H35H,H35I), C116(H11M,H11N,H11O), C126(H12J,H12K,H12L), C200(H20J,
 H20K,H20L), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C1(H1A,H1B,H1C),
  C7(H7A,H7B,H7C), C11(H11J,H11K,H11L)
5.c Aromatic/amide H refined with riding coordinates:
 C100(H100), C102(H102), C101(H101), C105(H105), C104(H104), C115(H115),
 C123(H123), C122(H122), C120(H120), C125(H125), C202(H202), C203(H203),
 C204(H204), C205(H205), C206(H206), C1AA(H1AA), C19(H19), C2(H2), C2AA(H2AA),
 C5(H5)
5.d Fitted hexagon refined as free rotating group:
 C100(C102,C101,C105,C104,C103), C114(C113,C112,C111,C110,C115), C124(C123,
 C122,C121,C120,C125), C201(C202,C203,C204,C205,C206), C1AA(C19,C2,C2AA,C9,C5)
5.e Idealised Me refined as rotating group:
 C106(H10J,H10K,H10L), C0AA(H0AA,H0AB,H0AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.43229(5) 0.74029(5) 0.37775(3) 0.0489(3) Uani 1 1 d . . . . .
Ge2 Ge 0.22418(6) 0.66633(4) 0.37495(3) 0.0461(2) Uani 1 1 d . . . . .
Ge3 Ge 0.25288(6) 0.84602(4) 0.38285(3) 0.0483(3) Uani 1 1 d . . . . .
Ge4 Ge 0.20159(6) 0.76395(5) 0.31832(3) 0.0522(3) Uani 1 1 d . . . . .
Ge5 Ge 0.35628(6) 0.81515(5) 0.31696(3) 0.0529(3) Uani 1 1 d . . . . .
Ge6 Ge 0.33809(5) 0.68560(5) 0.31351(3) 0.0448(2) Uani 1 1 d . . . . .
Ge7 Ge 0.20675(5) 0.75433(4) 0.43901(3) 0.0436(2) Uani 1 1 d . . . . .
Ge8 Ge 0.36267(6) 0.80553(5) 0.44427(3) 0.0479(2) Uani 1 1 d . . . . .
Ge9 Ge 0.34403(6) 0.67552(5) 0.43684(3) 0.0480(3) Uani 1 1 d . . . . .
Si1 Si 0.58048(15) 0.72702(18) 0.37636(10) 0.0707(9) Uani 1 1 d . . . . .
Si2 Si 0.13328(15) 0.57383(13) 0.36996(10) 0.0560(7) Uani 1 1 d . . . . .
Si10 Si 0.6422(2) 0.8286(3) 0.37604(14) 0.1133(15) Uani 1 1 d . . . . .
Si11 Si 0.6117(2) 0.6658(3) 0.30634(13) 0.1136(17) Uani 1 1 d . . . . .
Si12 Si 0.61999(19) 0.6658(2) 0.44700(12) 0.0964(13) Uani 1 1 d . . . . .
Si20 Si -0.00510(19) 0.61105(19) 0.3751(2) 0.1139(16) Uani 1 1 d . . . . .
Si21 Si 0.1600(3) 0.52045(18) 0.29512(12) 0.0898(11) Uani 1 1 d . . . . .
Si22 Si 0.16861(19) 0.50511(14) 0.43566(11) 0.0665(8) Uani 1 1 d . . . . .
Si3 Si 0.2090(5) 0.9553(3) 0.3927(2) 0.0445(15) Uani 0.5 1 d . . P A 1
Si30 Si 0.2633(5) 0.9965(3) 0.4670(2) 0.0551(14) Uani 0.5 1 d D . P A 1
Si31 Si 0.0629(5) 0.9523(4) 0.3908(3) 0.080(2) Uani 0.5 1 d D . P A 1
Si32 Si 0.2677(9) 1.0183(3) 0.3285(2) 0.102(3) Uani 0.5 1 d D . P A 1
Si3A Si 0.1625(4) 0.9436(3) 0.3852(3) 0.0494(17) Uani 0.5 1 d . . P A 2
Si33 Si 0.1917(5) 1.0003(4) 0.3128(3) 0.078(2) Uani 0.5 1 d D . P A 2
Si34 Si 0.0213(4) 0.9166(3) 0.3922(2) 0.0551(16) Uani 0.5 1 d D . P A 2
Si35 Si 0.2169(5) 1.0034(4) 0.4526(3) 0.072(2) Uiso 0.5 1 d D . P A 2
K1 K 0.29913(18) 0.74329(14) 0.56609(9) 0.0855(8) Uani 1 1 d . . . . .
C10A C 0.5946(18) 0.8803(14) 0.4180(10) 0.088(8) Uiso 0.5 1 d . U P B 1
H10A H 0.6019 0.8619 0.4509 0.132 Uiso 0.5 1 calc R . P B 1
H10B H 0.6209 0.9240 0.4168 0.132 Uiso 0.5 1 calc R . P B 1
H10C H 0.5342 0.8841 0.4098 0.132 Uiso 0.5 1 calc R . P B 1
C10B C 0.6329(17) 0.8570(13) 0.3153(9) 0.096(8) Uiso 0.5 1 d . U P B 1
H10D H 0.6609 0.8259 0.2935 0.145 Uiso 0.5 1 calc R . P B 1
H10E H 0.5731 0.8605 0.3058 0.145 Uiso 0.5 1 calc R . P B 1
H10F H 0.6597 0.9004 0.3128 0.145 Uiso 0.5 1 calc R . P B 1
C10C C 0.7594(15) 0.8150(13) 0.3959(10) 0.097(8) Uiso 0.5 1 d . U P B 1
H10G H 0.7866 0.7858 0.3724 0.145 Uiso 0.5 1 calc R . P B 1
H10H H 0.7889 0.8575 0.3969 0.145 Uiso 0.5 1 calc R . P B 1
H10I H 0.7620 0.7948 0.4285 0.145 Uiso 0.5 1 calc R . P B 1
C11B C 0.5777(9) 0.7115(11) 0.2506(4) 0.161(8) Uani 1 1 d . . . . .
H11A H 0.5164 0.7180 0.2508 0.241 Uiso 1 1 calc R . . . .
H11B H 0.6060 0.7544 0.2501 0.241 Uiso 1 1 calc R . . . .
H11C H 0.5928 0.6862 0.2215 0.241 Uiso 1 1 calc R . . . .
C11A C 0.7292(7) 0.6547(10) 0.3042(5) 0.168(9) Uani 1 1 d . . . . .
H11D H 0.7489 0.6305 0.3334 0.252 Uiso 1 1 calc R . . . .
H11E H 0.7434 0.6297 0.2748 0.252 Uiso 1 1 calc R . . . .
H11F H 0.7566 0.6979 0.3034 0.252 Uiso 1 1 calc R . . . .
C11C C 0.5536(10) 0.5832(8) 0.3062(7) 0.164(8) Uani 1 1 d . . . . .
H11G H 0.5705 0.5580 0.3354 0.246 Uiso 1 1 calc R . . . .
H11H H 0.4925 0.5910 0.3063 0.246 Uiso 1 1 calc R . . . .
H11I H 0.5679 0.5583 0.2768 0.246 Uiso 1 1 calc R . . . .
C12B C 0.5878(8) 0.7103(8) 0.5014(4) 0.109(5) Uani 1 1 d . . . . .
H12A H 0.6134 0.7542 0.5017 0.164 Uiso 1 1 calc R . . . .
H12B H 0.5261 0.7144 0.5012 0.164 Uiso 1 1 calc R . . . .
H12C H 0.6066 0.6861 0.5307 0.164 Uiso 1 1 calc R . . . .
C12A C 0.5694(10) 0.5816(7) 0.4481(6) 0.141(6) Uani 1 1 d . . . . .
H12D H 0.5858 0.5567 0.4191 0.211 Uiso 1 1 calc R . . . .
H12E H 0.5883 0.5580 0.4777 0.211 Uiso 1 1 calc R . . . .
H12F H 0.5078 0.5864 0.4481 0.211 Uiso 1 1 calc R . . . .
C12C C 0.7389(8) 0.6559(13) 0.4494(6) 0.218(13) Uani 1 1 d . . . . .
H12G H 0.7570 0.6320 0.4203 0.327 Uiso 1 1 calc R . . . .
H12H H 0.7656 0.6994 0.4503 0.327 Uiso 1 1 calc R . . . .
H12I H 0.7556 0.6310 0.4788 0.327 Uiso 1 1 calc R . . . .
C20B C -0.0788(17) 0.5396(13) 0.3872(10) 0.081(8) Uiso 0.5 1 d . . P C 1
H20A H -0.0675 0.5038 0.3642 0.122 Uiso 0.5 1 calc R . P C 1
H20B H -0.0695 0.5239 0.4208 0.122 Uiso 0.5 1 calc R . P C 1
H20C H -0.1374 0.5542 0.3829 0.122 Uiso 0.5 1 calc R . P C 1
C20A C -0.0245(19) 0.6631(15) 0.4103(11) 0.115(10) Uiso 0.5 1 d . . P C 1
H20D H 0.0126 0.7010 0.4050 0.172 Uiso 0.5 1 calc R . P C 1
H20E H -0.0835 0.6768 0.4057 0.172 Uiso 0.5 1 calc R . P C 1
H20F H -0.0156 0.6465 0.4437 0.172 Uiso 0.5 1 calc R . P C 1
C20C C -0.028(2) 0.6489(18) 0.3076(12) 0.140(12) Uiso 0.5 1 d . . P C 1
H20G H -0.0154 0.6155 0.2828 0.210 Uiso 0.5 1 calc R . P C 1
H20H H -0.0870 0.6622 0.3044 0.210 Uiso 0.5 1 calc R . P C 1
H20I H 0.0086 0.6874 0.3027 0.210 Uiso 0.5 1 calc R . P C 1
C21B C 0.2692(8) 0.4869(7) 0.2949(5) 0.106(4) Uani 1 1 d . . . . .
H21A H 0.3097 0.5230 0.2993 0.159 Uiso 1 1 calc R . . . .
H21B H 0.2765 0.4552 0.3217 0.159 Uiso 1 1 calc R . . . .
H21C H 0.2789 0.4649 0.2637 0.159 Uiso 1 1 calc R . . . .
C21A C 0.1466(12) 0.5814(8) 0.2429(5) 0.157(8) Uani 1 1 d . . . . .
H21D H 0.0891 0.5993 0.2428 0.235 Uiso 1 1 calc R . . . .
H21E H 0.1873 0.6174 0.2472 0.235 Uiso 1 1 calc R . . . .
H21F H 0.1563 0.5590 0.2118 0.235 Uiso 1 1 calc R . . . .
C21C C 0.0810(10) 0.4522(7) 0.2867(5) 0.139(6) Uani 1 1 d . . . . .
H21G H 0.0238 0.4705 0.2869 0.208 Uiso 1 1 calc R . . . .
H21H H 0.0902 0.4300 0.2554 0.208 Uiso 1 1 calc R . . . .
H21I H 0.0878 0.4203 0.3135 0.208 Uiso 1 1 calc R . . . .
C22C C 0.2803(7) 0.4805(6) 0.4340(5) 0.094(4) Uani 1 1 d . . . . .
H22A H 0.2908 0.4573 0.4033 0.141 Uiso 1 1 calc R . . . .
H22B H 0.3161 0.5198 0.4362 0.141 Uiso 1 1 calc R . . . .
H22C H 0.2934 0.4513 0.4617 0.141 Uiso 1 1 calc R . . . .
C22B C 0.1519(9) 0.5489(7) 0.4946(4) 0.107(4) Uani 1 1 d . . . . .
H22D H 0.0927 0.5626 0.4964 0.160 Uiso 1 1 calc R . . . .
H22E H 0.1657 0.5193 0.5220 0.160 Uiso 1 1 calc R . . . .
H22F H 0.1884 0.5878 0.4965 0.160 Uiso 1 1 calc R . . . .
C22A C 0.0992(9) 0.4292(6) 0.4348(5) 0.115(5) Uani 1 1 d . . . . .
H22G H 0.0398 0.4425 0.4357 0.173 Uiso 1 1 calc R . . . .
H22H H 0.1090 0.4039 0.4049 0.173 Uiso 1 1 calc R . . . .
H22I H 0.1130 0.4018 0.4634 0.173 Uiso 1 1 calc R . . . .
C30B C 0.218(2) 1.0792(11) 0.4793(10) 0.111(11) Uani 0.5 1 d D . P A 1
H30A H 0.2324 1.1094 0.4527 0.167 Uiso 0.5 1 calc R . P A 1
H30B H 0.1564 1.0757 0.4812 0.167 Uiso 0.5 1 calc R . P A 1
H30C H 0.2412 1.0961 0.5104 0.167 Uiso 0.5 1 calc R . P A 1
C30A C 0.3811(11) 1.0009(14) 0.4673(8) 0.080(7) Uani 0.5 1 d D . P A 1
H30D H 0.4042 0.9570 0.4609 0.121 Uiso 0.5 1 calc R . P A 1
H30E H 0.3991 1.0316 0.4419 0.121 Uiso 0.5 1 calc R . P A 1
H30F H 0.4018 1.0163 0.4994 0.121 Uiso 0.5 1 calc R . P A 1
C30C C 0.2332(17) 0.9420(19) 0.5189(10) 0.087(12) Uani 0.5 1 d D . P A 1
H30G H 0.2561 0.8978 0.5137 0.131 Uiso 0.5 1 calc R . P A 1
H30H H 0.2563 0.9601 0.5496 0.131 Uiso 0.5 1 calc R . P A 1
H30I H 0.1716 0.9397 0.5204 0.131 Uiso 0.5 1 calc R . P A 1
C31A C 0.0252(18) 0.9211(16) 0.4503(8) 0.116(11) Uani 0.5 1 d D . P A 1
H31A H 0.0471 0.9492 0.4768 0.175 Uiso 0.5 1 calc R . P A 1
H31B H -0.0366 0.9215 0.4501 0.175 Uiso 0.5 1 calc R . P A 1
H31C H 0.0454 0.8759 0.4553 0.175 Uiso 0.5 1 calc R . P A 1
C31B C 0.014(2) 1.0359(12) 0.3847(17) 0.182(18) Uani 0.5 1 d D . P A 1
H31D H 0.0360 1.0647 0.4108 0.272 Uiso 0.5 1 calc R . P A 1
H31E H 0.0272 1.0547 0.3528 0.272 Uiso 0.5 1 calc R . P A 1
H31F H -0.0476 1.0321 0.3874 0.272 Uiso 0.5 1 calc R . P A 1
C31C C 0.0206(15) 0.8981(15) 0.3414(11) 0.110(12) Uani 0.5 1 d D . P A 1
H31G H 0.0399 0.9139 0.3097 0.165 Uiso 0.5 1 calc R . P A 1
H31H H 0.0408 0.8529 0.3468 0.165 Uiso 0.5 1 calc R . P A 1
H31I H -0.0413 0.8986 0.3416 0.165 Uiso 0.5 1 calc R . P A 1
C32C C 0.226(2) 0.9852(15) 0.2696(8) 0.114(11) Uani 0.5 1 d D . P A 1
H32A H 0.2419 0.9386 0.2668 0.171 Uiso 0.5 1 calc R . P A 1
H32B H 0.1648 0.9895 0.2682 0.171 Uiso 0.5 1 calc R . P A 1
H32C H 0.2507 1.0099 0.2425 0.171 Uiso 0.5 1 calc R . P A 1
C32B C 0.3845(12) 1.0053(15) 0.3280(10) 0.118(9) Uiso 0.5 1 d D . P A 1
H32D H 0.3965 0.9584 0.3231 0.177 Uiso 0.5 1 calc R . P A 1
H32E H 0.4087 1.0309 0.3014 0.177 Uiso 0.5 1 calc R . P A 1
H32F H 0.4095 1.0196 0.3594 0.177 Uiso 0.5 1 calc R . P A 1
C32A C 0.242(3) 1.1061(9) 0.3378(11) 0.21(2) Uani 0.5 1 d D . P A 1
H32G H 0.2658 1.1206 0.3694 0.313 Uiso 0.5 1 calc R . P A 1
H32H H 0.2669 1.1323 0.3116 0.313 Uiso 0.5 1 calc R . P A 1
H32I H 0.1809 1.1119 0.3372 0.313 Uiso 0.5 1 calc R . P A 1
C33C C 0.1700(16) 0.9472(13) 0.2588(6) 0.100(10) Uani 0.5 1 d D . P A 2
H33A H 0.1107 0.9334 0.2585 0.150 Uiso 0.5 1 calc R . P A 2
H33B H 0.1812 0.9720 0.2288 0.150 Uiso 0.5 1 calc R . P A 2
H33C H 0.2065 0.9083 0.2604 0.150 Uiso 0.5 1 calc R . P A 2
C33B C 0.1226(18) 1.0733(12) 0.3065(10) 0.127(12) Uani 0.5 1 d D . P A 2
H33D H 0.0635 1.0599 0.3096 0.191 Uiso 0.5 1 calc R . P A 2
H33E H 0.1372 1.1052 0.3323 0.191 Uiso 0.5 1 calc R . P A 2
H33F H 0.1304 1.0936 0.2744 0.191 Uiso 0.5 1 calc R . P A 2
C33A C 0.3039(13) 1.0214(17) 0.3075(13) 0.124(13) Uiso 0.5 1 d D . P A 2
H33G H 0.3382 0.9814 0.3110 0.186 Uiso 0.5 1 calc R . P A 2
H33H H 0.3133 1.0413 0.2754 0.186 Uiso 0.5 1 calc R . P A 2
H33I H 0.3201 1.0528 0.3332 0.186 Uiso 0.5 1 calc R . P A 2
C34B C 0.0010(16) 0.8708(11) 0.4496(8) 0.078(8) Uani 0.5 1 d D . P A 2
H34A H 0.0189 0.8976 0.4778 0.118 Uiso 0.5 1 calc R . P A 2
H34B H -0.0595 0.8612 0.4516 0.118 Uiso 0.5 1 calc R . P A 2
H34C H 0.0328 0.8294 0.4498 0.118 Uiso 0.5 1 calc R . P A 2
C34A C -0.0459(16) 0.9926(12) 0.3911(13) 0.119(11) Uani 0.5 1 d D . P A 2
H34D H -0.0358 1.0174 0.3610 0.178 Uiso 0.5 1 calc R . P A 2
H34E H -0.1055 0.9801 0.3922 0.178 Uiso 0.5 1 calc R . P A 2
H34F H -0.0313 1.0202 0.4195 0.178 Uiso 0.5 1 calc R . P A 2
C34C C -0.0139(16) 0.8634(18) 0.3401(10) 0.111(13) Uani 0.5 1 d D . P A 2
H34G H -0.0040 0.8863 0.3092 0.167 Uiso 0.5 1 calc R . P A 2
H34H H 0.0180 0.8221 0.3410 0.167 Uiso 0.5 1 calc R . P A 2
H34I H -0.0743 0.8539 0.3428 0.167 Uiso 0.5 1 calc R . P A 2
C35B C 0.164(2) 1.0856(10) 0.4560(11) 0.126(13) Uani 0.5 1 d D . P A 2
H35A H 0.1030 1.0795 0.4582 0.189 Uiso 0.5 1 calc R . P A 2
H35B H 0.1853 1.1093 0.4851 0.189 Uiso 0.5 1 calc R . P A 2
H35C H 0.1766 1.1112 0.4266 0.189 Uiso 0.5 1 calc R . P A 2
C35A C 0.3340(12) 1.0128(16) 0.4485(11) 0.114(12) Uani 0.5 1 d D . P A 2
H35D H 0.3603 0.9692 0.4467 0.171 Uiso 0.5 1 calc R . P A 2
H35E H 0.3472 1.0381 0.4190 0.171 Uiso 0.5 1 calc R . P A 2
H35F H 0.3559 1.0362 0.4775 0.171 Uiso 0.5 1 calc R . P A 2
C35C C 0.194(2) 0.9585(19) 0.5106(10) 0.106(13) Uani 0.5 1 d D . P A 2
H35G H 0.2205 0.9150 0.5100 0.159 Uiso 0.5 1 calc R . P A 2
H35H H 0.2160 0.9837 0.5386 0.159 Uiso 0.5 1 calc R . P A 2
H35I H 0.1325 0.9533 0.5134 0.159 Uiso 0.5 1 calc R . P A 2
C100 C 0.3979(13) 0.8303(10) 0.6687(6) 0.092(8) Uiso 0.5 1 d . U P D 1
H100 H 0.3722 0.8257 0.6995 0.110 Uiso 0.5 1 calc R . P D 1
C102 C 0.4430(15) 0.7781(8) 0.6492(7) 0.116(10) Uiso 0.5 1 d G U P D 1
H102 H 0.4480 0.7378 0.6668 0.139 Uiso 0.5 1 calc R . P D 1
C101 C 0.4807(13) 0.7847(8) 0.6040(7) 0.091(7) Uiso 0.5 1 d G U P D 1
H101 H 0.5115 0.7490 0.5907 0.110 Uiso 0.5 1 calc R . P D 1
C105 C 0.4734(12) 0.8436(10) 0.5783(6) 0.078(7) Uiso 0.5 1 d G U P D 1
H105 H 0.4992 0.8482 0.5474 0.094 Uiso 0.5 1 calc R . P D 1
C104 C 0.4283(14) 0.8958(8) 0.5978(7) 0.117(15) Uiso 0.5 1 d G U P D 1
H104 H 0.4233 0.9361 0.5802 0.140 Uiso 0.5 1 calc R . P D 1
C103 C 0.3906(13) 0.8892(8) 0.6429(8) 0.087(8) Uiso 0.5 1 d G U P D 1
C106 C 0.340(2) 0.9423(16) 0.6619(12) 0.142(12) Uiso 0.5 1 d . U P D 1
H10J H 0.2911 0.9497 0.6402 0.213 Uiso 0.5 1 calc GR . P D 1
H10K H 0.3742 0.9826 0.6639 0.213 Uiso 0.5 1 calc GR . P D 1
H10L H 0.3210 0.9307 0.6947 0.213 Uiso 0.5 1 calc GR . P D 1
C114 C 0.1336(6) 0.7016(5) 0.6462(3) 0.100(4) Uani 1 1 d . . . . .
C113 C 0.1532(6) 0.7668(6) 0.6571(3) 0.114(5) Uani 1 1 d G . . . .
C112 C 0.1410(6) 0.8153(4) 0.6217(4) 0.116(5) Uani 1 1 d G . . . .
H112 H 0.1457 0.8628 0.6312 0.140 Uiso 1 1 calc R . . . .
C111 C 0.1092(6) 0.7986(5) 0.5755(4) 0.131(6) Uani 1 1 d G . . . .
H111 H 0.0889 0.8342 0.5529 0.157 Uiso 1 1 calc R . . . .
C110 C 0.0896(6) 0.7334(6) 0.5647(3) 0.139(7) Uani 1 1 d G . . . .
H110 H 0.0586 0.7225 0.5335 0.166 Uiso 1 1 calc R . . . .
C115 C 0.1018(6) 0.6848(4) 0.6001(4) 0.105(4) Uani 1 1 d G . . . .
H115 H 0.0885 0.6403 0.5927 0.126 Uiso 1 1 calc R . . . .
C116 C 0.143(2) 0.6546(15) 0.6858(8) 0.34(2) Uani 1 1 d . . . . .
H11M H 0.1277 0.6105 0.6740 0.504 Uiso 1 1 calc R . . . .
H11N H 0.2020 0.6543 0.6977 0.504 Uiso 1 1 calc R . . . .
H11O H 0.1063 0.6670 0.7126 0.504 Uiso 1 1 calc R . . . .
C124 C 0.4441(8) 0.5925(5) 0.6557(4) 0.104(4) Uani 1 1 d . . . . .
C123 C 0.3565(8) 0.5883(5) 0.6560(4) 0.112(5) Uani 1 1 d G . . . .
H123 H 0.3279 0.5875 0.6862 0.135 Uiso 1 1 calc R . . . .
C122 C 0.3107(6) 0.5851(5) 0.6121(5) 0.126(5) Uani 1 1 d G . . . .
H122 H 0.2508 0.5822 0.6122 0.151 Uiso 1 1 calc R . . . .
C121 C 0.3525(11) 0.5862(5) 0.5679(4) 0.137(7) Uani 1 1 d G . . . .
H121 H 0.3264 0.5587 0.5412 0.164 Uiso 1 1 calc R . . . .
C120 C 0.4401(11) 0.5905(5) 0.5676(4) 0.150(7) Uani 1 1 d G . . . .
H120 H 0.4686 0.5912 0.5375 0.180 Uiso 1 1 calc R . . . .
C125 C 0.4858(6) 0.5936(5) 0.6116(6) 0.149(7) Uani 1 1 d G . . . .
H125 H 0.5457 0.5966 0.6114 0.179 Uiso 1 1 calc R . . . .
C126 C 0.4979(14) 0.5917(11) 0.7003(8) 0.216(11) Uani 1 1 d . . . . .
H12J H 0.5573 0.5953 0.6913 0.324 Uiso 1 1 calc R . . . .
H12K H 0.4831 0.6289 0.7213 0.324 Uiso 1 1 calc R . . . .
H12L H 0.4893 0.5503 0.7180 0.324 Uiso 1 1 calc R . . . .
C200 C -0.0645(17) 0.7401(11) 0.7177(9) 0.268(16) Uani 1 1 d D U . . .
H20J H -0.0850 0.7267 0.7497 0.402 Uiso 1 1 calc R . . . .
H20K H -0.0162 0.7126 0.7091 0.402 Uiso 1 1 calc R . . . .
H20L H -0.0471 0.7864 0.7190 0.402 Uiso 1 1 calc R . . . .
C201 C -0.1299(11) 0.7323(6) 0.6820(6) 0.152(7) Uani 1 1 d D U . . .
C202 C -0.1076(9) 0.7499(5) 0.6348(7) 0.148(7) Uani 1 1 d G U . . .
H202 H -0.0521 0.7653 0.6288 0.178 Uiso 1 1 calc R . . . .
C203 C -0.1665(14) 0.7451(6) 0.5965(5) 0.206(10) Uani 1 1 d G U . . .
H203 H -0.1513 0.7572 0.5643 0.247 Uiso 1 1 calc R . . . .
C204 C -0.2476(12) 0.7226(7) 0.6053(7) 0.225(11) Uani 1 1 d G U . . .
H204 H -0.2879 0.7193 0.5791 0.270 Uiso 1 1 calc R . . . .
C205 C -0.2699(9) 0.7050(7) 0.6524(9) 0.253(12) Uani 1 1 d G U . . .
H205 H -0.3254 0.6896 0.6585 0.303 Uiso 1 1 calc R . . . .
C206 C -0.2110(13) 0.7098(6) 0.6908(6) 0.185(8) Uani 1 1 d G U . . .
H206 H -0.2262 0.6977 0.7230 0.222 Uiso 1 1 calc R . . . .
C1AA C 0.4656(15) 0.7702(10) 0.6261(10) 0.142(12) Uiso 0.5 1 d . . P D 2
H1AA H 0.4991 0.7315 0.6237 0.170 Uiso 0.5 1 calc R . P D 2
C19 C 0.4049(14) 0.7750(9) 0.6618(8) 0.099(8) Uiso 0.5 1 d G . P D 2
H19 H 0.3969 0.7395 0.6840 0.119 Uiso 0.5 1 calc R . P D 2
C2 C 0.3560(12) 0.8316(11) 0.6652(7) 0.114(10) Uiso 0.5 1 d G . P D 2
H2 H 0.3145 0.8348 0.6897 0.137 Uiso 0.5 1 calc R . P D 2
C2AA C 0.3678(13) 0.8834(9) 0.6328(9) 0.135(15) Uiso 0.5 1 d G . P D 2
H2AA H 0.3344 0.9221 0.6351 0.162 Uiso 0.5 1 calc R . P D 2
C9 C 0.4285(14) 0.8786(11) 0.5971(7) 0.083(10) Uiso 0.5 1 d G . P D 2
C5 C 0.4774(13) 0.8220(13) 0.5937(8) 0.107(9) Uiso 0.5 1 d G . P D 2
H5 H 0.5189 0.8187 0.5692 0.128 Uiso 0.5 1 calc R . P D 2
C0AA C 0.443(3) 0.923(2) 0.5609(18) 0.24(2) Uiso 0.5 1 d . . P D 2
H0AA H 0.3909 0.9286 0.5411 0.359 Uiso 0.5 1 calc GR . P D 2
H0AB H 0.4878 0.9064 0.5402 0.359 Uiso 0.5 1 calc GR . P D 2
H0AC H 0.4595 0.9650 0.5754 0.359 Uiso 0.5 1 calc GR . P D 2
C3 C -0.0826(17) 0.5428(13) 0.3657(10) 0.080(8) Uiso 0.5 1 d . . P C 2
H3A H -0.0678 0.5061 0.3876 0.120 Uiso 0.5 1 calc R . P C 2
H3B H -0.1394 0.5586 0.3730 0.120 Uiso 0.5 1 calc R . P C 2
H3C H -0.0813 0.5279 0.3317 0.120 Uiso 0.5 1 calc R . P C 2
C4 C -0.0357(18) 0.6732(14) 0.3354(10) 0.102(9) Uiso 0.5 1 d . . P C 2
H4A H 0.0033 0.7105 0.3390 0.153 Uiso 0.5 1 calc R . P C 2
H4B H -0.0349 0.6569 0.3017 0.153 Uiso 0.5 1 calc R . P C 2
H4C H -0.0930 0.6877 0.3431 0.153 Uiso 0.5 1 calc R . P C 2
C8 C -0.0152(14) 0.6579(11) 0.4436(8) 0.075(6) Uiso 0.5 1 d . . P C 2
H8A H 0.0009 0.6270 0.4697 0.113 Uiso 0.5 1 calc R . P C 2
H8B H 0.0224 0.6963 0.4449 0.113 Uiso 0.5 1 calc R . P C 2
H8C H -0.0736 0.6724 0.4479 0.113 Uiso 0.5 1 calc R . P C 2
C1 C 0.581(3) 0.896(2) 0.3281(14) 0.178(16) Uiso 0.5 1 d . . P B 2
H1A H 0.5201 0.8930 0.3322 0.267 Uiso 0.5 1 calc R . P B 2
H1B H 0.6007 0.9404 0.3355 0.267 Uiso 0.5 1 calc R . P B 2
H1C H 0.5949 0.8846 0.2942 0.267 Uiso 0.5 1 calc R . P B 2
C7 C 0.748(2) 0.8467(19) 0.3589(14) 0.167(15) Uiso 0.5 1 d . . P B 2
H7A H 0.7603 0.8244 0.3280 0.251 Uiso 0.5 1 calc R . P B 2
H7B H 0.7546 0.8944 0.3547 0.251 Uiso 0.5 1 calc R . P B 2
H7C H 0.7876 0.8312 0.3845 0.251 Uiso 0.5 1 calc R . P B 2
C11 C 0.617(3) 0.874(2) 0.4383(14) 0.160(17) Uiso 0.5 1 d . . P B 2
H11J H 0.5595 0.8637 0.4477 0.240 Uiso 0.5 1 calc R . P B 2
H11K H 0.6569 0.8582 0.4640 0.240 Uiso 0.5 1 calc R . P B 2
H11L H 0.6238 0.9213 0.4342 0.240 Uiso 0.5 1 calc R . P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 Ge5 2.5351(13) . ?
Ge1 Ge6 2.5342(12) . ?
Ge1 Ge8 2.5226(12) . ?
Ge1 Ge9 2.5280(13) . ?
Ge1 Si1 2.364(3) . ?
Ge2 Ge4 2.5345(13) . ?
Ge2 Ge6 2.5229(12) . ?
Ge2 Ge7 2.5204(13) . ?
Ge2 Ge9 2.5206(12) . ?
Ge2 Si2 2.368(3) . ?
Ge3 Ge4 2.5454(14) . ?
Ge3 Ge5 2.5397(13) . ?
Ge3 Ge7 2.5301(12) . ?
Ge3 Ge8 2.5267(13) . ?
Ge3 Si3 2.341(6) . ?
Ge3 Si3A 2.446(7) . ?
Ge4 Ge5 2.6623(14) . ?
Ge4 Ge6 2.6894(12) . ?
Ge5 Ge6 2.6463(14) . ?
Ge7 Ge8 2.6801(13) . ?
Ge7 Ge9 2.7010(12) . ?
Ge7 K1 3.745(3) . ?
Ge8 Ge9 2.6622(14) . ?
Ge8 K1 3.721(3) . ?
Ge9 K1 3.871(3) . ?
Si1 Si10 2.282(5) . ?
Si1 Si11 2.344(4) . ?
Si1 Si12 2.368(5) . ?
Si2 Si20 2.325(4) . ?
Si2 Si21 2.361(4) . ?
Si2 Si22 2.332(4) . ?
Si10 C10A 1.74(3) . ?
Si10 C10B 1.76(2) . ?
Si10 C10C 1.94(2) . ?
Si10 C1 2.11(4) . ?
Si10 C7 1.79(4) . ?
Si10 C11 1.98(4) . ?
Si11 C11B 1.852(15) . ?
Si11 C11A 1.877(11) . ?
Si11 C11C 1.913(17) . ?
Si12 C12B 1.822(13) . ?
Si12 C12A 1.888(16) . ?
Si12 C12C 1.894(12) . ?
Si20 C20B 1.90(3) . ?
Si20 C20A 1.47(3) . ?
Si20 C20C 2.02(3) . ?
Si20 C3 1.86(3) . ?
Si20 C4 1.73(3) . ?
Si20 C8 2.11(2) . ?
Si21 C21B 1.858(13) . ?
Si21 C21A 1.896(14) . ?
Si21 C21C 1.878(13) . ?
Si22 C22C 1.839(12) . ?
Si22 C22B 1.864(12) . ?
Si22 C22A 1.893(11) . ?
Si3 Si30 2.343(9) . ?
Si3 Si31 2.314(11) . ?
Si3 Si32 2.378(11) . ?
Si30 C30B 1.858(16) . ?
Si30 C30A 1.868(16) . ?
Si30 C30C 1.867(17) . ?
Si31 C31A 1.857(17) . ?
Si31 C31B 1.872(16) . ?
Si31 C31C 1.855(17) . ?
Si32 C32C 1.851(16) . ?
Si32 C32B 1.868(17) . ?
Si32 C32A 1.845(16) . ?
Si3A Si33 2.344(9) . ?
Si3A Si34 2.315(10) . ?
Si3A Si35 2.353(11) . ?
Si33 C33C 1.852(17) . ?
Si33 C33B 1.848(14) . ?
Si33 C33A 1.838(17) . ?
Si34 C34B 1.858(16) . ?
Si34 C34A 1.873(16) . ?
Si34 C34C 1.862(17) . ?
Si35 C35B 1.869(17) . ?
Si35 C35A 1.871(17) . ?
Si35 C35C 1.871(17) . ?
K1 C102 3.26(2) . ?
K1 C101 3.15(2) . ?
K1 C105 3.44(2) . ?
K1 C112 3.300(9) . ?
K1 C111 3.226(10) . ?
K1 C110 3.323(10) . ?
K1 C122 3.451(11) . ?
K1 C121 3.298(10) . ?
K1 C1AA 3.12(3) . ?
K1 C19 3.14(2) . ?
K1 C2 3.35(2) . ?
K1 C5 3.32(2) . ?
C100 C102 1.3900 . ?
C100 C103 1.3900 . ?
C102 C101 1.3900 . ?
C101 C105 1.3900 . ?
C105 C104 1.3900 . ?
C104 C103 1.3900 . ?
C103 C106 1.45(3) . ?
C114 C113 1.3900 . ?
C114 C115 1.3900 . ?
C114 C116 1.45(2) . ?
C113 C112 1.3900 . ?
C112 C111 1.3900 . ?
C111 C110 1.3900 . ?
C110 C115 1.3900 . ?
C124 C123 1.3900 . ?
C124 C125 1.3900 . ?
C124 C126 1.471(18) . ?
C123 C122 1.3900 . ?
C122 C121 1.3900 . ?
C121 C120 1.3900 . ?
C120 C125 1.3900 . ?
C200 C201 1.416(15) . ?
C201 C202 1.3900 . ?
C201 C206 1.3900 . ?
C202 C203 1.3900 . ?
C203 C204 1.3900 . ?
C204 C205 1.3900 . ?
C205 C206 1.3900 . ?
C1AA C19 1.3900 . ?
C1AA C5 1.3900 . ?
C19 C2 1.3900 . ?
C2 C2AA 1.3900 . ?
C2AA C9 1.3900 . ?
C9 C5 1.3900 . ?
C9 C0AA 1.35(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Ge6 Ge1 Ge5 62.94(4) . . ?
Ge8 Ge1 Ge5 87.07(4) . . ?
Ge8 Ge1 Ge6 117.97(4) . . ?
Ge8 Ge1 Ge9 63.62(4) . . ?
Ge9 Ge1 Ge5 117.96(4) . . ?
Ge9 Ge1 Ge6 83.65(4) . . ?
Si1 Ge1 Ge5 120.99(9) . . ?
Si1 Ge1 Ge6 120.55(8) . . ?
Si1 Ge1 Ge8 121.45(8) . . ?
Si1 Ge1 Ge9 120.97(9) . . ?
Ge6 Ge2 Ge4 64.25(4) . . ?
Ge7 Ge2 Ge4 81.60(4) . . ?
Ge7 Ge2 Ge6 116.33(4) . . ?
Ge7 Ge2 Ge9 64.80(4) . . ?
Ge9 Ge2 Ge4 116.46(4) . . ?
Ge9 Ge2 Ge6 84.03(4) . . ?
Si2 Ge2 Ge4 120.49(8) . . ?
Si2 Ge2 Ge6 121.85(8) . . ?
Si2 Ge2 Ge7 121.72(8) . . ?
Si2 Ge2 Ge9 123.03(8) . . ?
Ge5 Ge3 Ge4 63.14(4) . . ?
Ge7 Ge3 Ge4 81.20(4) . . ?
Ge7 Ge3 Ge5 116.63(4) . . ?
Ge8 Ge3 Ge4 116.84(4) . . ?
Ge8 Ge3 Ge5 86.88(4) . . ?
Ge8 Ge3 Ge7 64.01(4) . . ?
Si3 Ge3 Ge4 127.48(17) . . ?
Si3 Ge3 Ge5 120.89(17) . . ?
Si3 Ge3 Ge7 122.41(16) . . ?
Si3 Ge3 Ge8 115.67(17) . . ?
Si3A Ge3 Ge4 111.73(18) . . ?
Si3A Ge3 Ge5 127.27(16) . . ?
Si3A Ge3 Ge7 113.74(16) . . ?
Si3A Ge3 Ge8 129.83(18) . . ?
Ge2 Ge4 Ge3 92.86(4) . . ?
Ge2 Ge4 Ge5 101.32(4) . . ?
Ge2 Ge4 Ge6 57.66(3) . . ?
Ge3 Ge4 Ge5 58.33(4) . . ?
Ge3 Ge4 Ge6 100.16(4) . . ?
Ge5 Ge4 Ge6 59.27(3) . . ?
Ge1 Ge5 Ge3 89.28(4) . . ?
Ge1 Ge5 Ge4 100.40(4) . . ?
Ge1 Ge5 Ge6 58.51(4) . . ?
Ge3 Ge5 Ge4 58.53(4) . . ?
Ge3 Ge5 Ge6 101.48(4) . . ?
Ge6 Ge5 Ge4 60.88(3) . . ?
Ge1 Ge6 Ge4 99.70(4) . . ?
Ge1 Ge6 Ge5 58.55(4) . . ?
Ge2 Ge6 Ge1 91.46(4) . . ?
Ge2 Ge6 Ge4 58.09(3) . . ?
Ge2 Ge6 Ge5 102.08(4) . . ?
Ge5 Ge6 Ge4 59.86(4) . . ?
Ge2 Ge7 Ge3 93.57(4) . . ?
Ge2 Ge7 Ge8 101.35(4) . . ?
Ge2 Ge7 Ge9 57.61(3) . . ?
Ge2 Ge7 K1 123.72(6) . . ?
Ge3 Ge7 Ge8 57.93(3) . . ?
Ge3 Ge7 Ge9 100.28(4) . . ?
Ge3 Ge7 K1 119.63(6) . . ?
Ge8 Ge7 Ge9 59.30(3) . . ?
Ge8 Ge7 K1 68.48(5) . . ?
Ge9 Ge7 K1 71.76(5) . . ?
Ge1 Ge8 Ge3 89.86(4) . . ?
Ge1 Ge8 Ge7 100.08(4) . . ?
Ge1 Ge8 Ge9 58.29(4) . . ?
Ge1 Ge8 K1 126.73(6) . . ?
Ge3 Ge8 Ge7 58.06(3) . . ?
Ge3 Ge8 Ge9 101.43(4) . . ?
Ge3 Ge8 K1 120.58(6) . . ?
Ge7 Ge8 K1 69.44(5) . . ?
Ge9 Ge8 Ge7 60.74(3) . . ?
Ge9 Ge8 K1 72.54(5) . . ?
Ge1 Ge9 Ge7 99.39(4) . . ?
Ge1 Ge9 Ge8 58.09(4) . . ?
Ge1 Ge9 K1 120.91(5) . . ?
Ge2 Ge9 Ge1 91.66(4) . . ?
Ge2 Ge9 Ge7 57.60(3) . . ?
Ge2 Ge9 Ge8 101.84(4) . . ?
Ge2 Ge9 K1 119.17(6) . . ?
Ge7 Ge9 K1 66.74(5) . . ?
Ge8 Ge9 Ge7 59.96(3) . . ?
Ge8 Ge9 K1 66.46(5) . . ?
Ge1 Si1 Si12 106.92(14) . . ?
Si10 Si1 Ge1 108.82(18) . . ?
Si10 Si1 Si11 112.2(2) . . ?
Si10 Si1 Si12 111.82(18) . . ?
Si11 Si1 Ge1 107.54(13) . . ?
Si11 Si1 Si12 109.3(2) . . ?
Si20 Si2 Ge2 108.16(14) . . ?
Si20 Si2 Si21 112.89(19) . . ?
Si20 Si2 Si22 110.98(18) . . ?
Si21 Si2 Ge2 107.03(13) . . ?
Si22 Si2 Ge2 107.15(13) . . ?
Si22 Si2 Si21 110.36(16) . . ?
C10A Si10 Si1 110.5(10) . . ?
C10A Si10 C10B 113.3(13) . . ?
C10A Si10 C10C 109.1(13) . . ?
C10B Si10 Si1 105.8(9) . . ?
C10B Si10 C10C 111.7(12) . . ?
C10C Si10 Si1 106.1(8) . . ?
C1 Si10 Si1 113.3(11) . . ?
C7 Si10 Si1 126.2(13) . . ?
C7 Si10 C1 97.1(17) . . ?
C7 Si10 C11 109.6(18) . . ?
C11 Si10 Si1 108.7(13) . . ?
C11 Si10 C1 98.1(17) . . ?
C11B Si11 Si1 110.0(6) . . ?
C11B Si11 C11A 107.7(7) . . ?
C11B Si11 C11C 107.9(8) . . ?
C11A Si11 Si1 108.4(5) . . ?
C11A Si11 C11C 111.8(8) . . ?
C11C Si11 Si1 110.9(5) . . ?
C12B Si12 Si1 109.4(5) . . ?
C12B Si12 C12A 108.0(7) . . ?
C12B Si12 C12C 108.7(8) . . ?
C12A Si12 Si1 112.5(5) . . ?
C12A Si12 C12C 109.0(9) . . ?
C12C Si12 Si1 109.2(5) . . ?
C20B Si20 Si2 110.3(8) . . ?
C20B Si20 C20C 110.7(13) . . ?
C20A Si20 Si2 119.0(12) . . ?
C20A Si20 C20B 107.3(15) . . ?
C20A Si20 C20C 106.8(16) . . ?
C20C Si20 Si2 102.4(10) . . ?
C3 Si20 Si2 111.6(8) . . ?
C3 Si20 C8 113.2(11) . . ?
C4 Si20 Si2 116.8(10) . . ?
C4 Si20 C3 106.4(13) . . ?
C4 Si20 C8 101.6(12) . . ?
C8 Si20 Si2 106.9(6) . . ?
C21B Si21 Si2 110.8(4) . . ?
C21B Si21 C21A 109.0(7) . . ?
C21B Si21 C21C 110.3(7) . . ?
C21A Si21 Si2 109.4(6) . . ?
C21C Si21 Si2 108.2(5) . . ?
C21C Si21 C21A 109.0(7) . . ?
C22C Si22 Si2 111.0(4) . . ?
C22C Si22 C22B 107.8(6) . . ?
C22C Si22 C22A 109.7(6) . . ?
C22B Si22 Si2 110.1(4) . . ?
C22B Si22 C22A 107.8(6) . . ?
C22A Si22 Si2 110.4(5) . . ?
Ge3 Si3 Si30 109.5(3) . . ?
Ge3 Si3 Si32 107.6(3) . . ?
Si30 Si3 Si32 107.8(4) . . ?
Si31 Si3 Ge3 105.8(4) . . ?
Si31 Si3 Si30 112.1(4) . . ?
Si31 Si3 Si32 113.8(4) . . ?
C30B Si30 Si3 110.1(9) . . ?
C30B Si30 C30A 110.3(14) . . ?
C30B Si30 C30C 107.0(16) . . ?
C30A Si30 Si3 111.6(7) . . ?
C30C Si30 Si3 110.5(13) . . ?
C30C Si30 C30A 107.2(12) . . ?
C31A Si31 Si3 109.2(10) . . ?
C31A Si31 C31B 104.2(18) . . ?
C31B Si31 Si3 113.1(13) . . ?
C31C Si31 Si3 112.1(9) . . ?
C31C Si31 C31A 108.4(17) . . ?
C31C Si31 C31B 109.4(17) . . ?
C32C Si32 Si3 108.1(12) . . ?
C32C Si32 C32B 105.9(15) . . ?
C32B Si32 Si3 109.4(10) . . ?
C32A Si32 Si3 109.1(10) . . ?
C32A Si32 C32C 113.3(17) . . ?
C32A Si32 C32B 111(2) . . ?
Si33 Si3A Ge3 104.4(3) . . ?
Si33 Si3A Si35 109.4(4) . . ?
Si34 Si3A Ge3 112.2(3) . . ?
Si34 Si3A Si33 113.3(4) . . ?
Si34 Si3A Si35 113.2(4) . . ?
Si35 Si3A Ge3 103.5(3) . . ?
C33C Si33 Si3A 110.5(8) . . ?
C33B Si33 Si3A 110.1(8) . . ?
C33B Si33 C33C 107.1(14) . . ?
C33A Si33 Si3A 113.0(12) . . ?
C33A Si33 C33C 103.6(15) . . ?
C33A Si33 C33B 112.2(16) . . ?
C34B Si34 Si3A 112.0(9) . . ?
C34B Si34 C34A 108.5(13) . . ?
C34B Si34 C34C 107.5(15) . . ?
C34A Si34 Si3A 110.7(10) . . ?
C34C Si34 Si3A 110.3(8) . . ?
C34C Si34 C34A 107.8(17) . . ?
C35B Si35 Si3A 110.1(10) . . ?
C35B Si35 C35A 110.9(16) . . ?
C35B Si35 C35C 107.2(17) . . ?
C35A Si35 Si3A 110.6(10) . . ?
C35A Si35 C35C 108.4(15) . . ?
C35C Si35 Si3A 109.6(13) . . ?
C102 K1 C105 42.0(2) . . ?
C102 K1 C112 96.3(4) . . ?
C102 K1 C110 134.7(4) . . ?
C102 K1 C122 85.3(3) . . ?
C102 K1 C121 91.4(3) . . ?
C101 K1 C102 24.98(16) . . ?
C101 K1 C105 23.83(15) . . ?
C101 K1 C112 115.3(3) . . ?
C101 K1 C111 136.6(4) . . ?
C101 K1 C110 157.5(3) . . ?
C101 K1 C122 95.1(4) . . ?
C101 K1 C121 91.2(4) . . ?
C105 K1 C122 118.7(4) . . ?
C112 K1 C105 108.0(3) . . ?
C112 K1 C110 42.63(10) . . ?
C112 K1 C122 106.2(3) . . ?
C112 K1 C2 65.4(4) . . ?
C112 K1 C5 109.5(4) . . ?
C111 K1 C102 120.5(4) . . ?
C111 K1 C105 122.3(4) . . ?
C111 K1 C112 24.56(7) . . ?
C111 K1 C110 24.45(7) . . ?
C111 K1 C122 109.7(3) . . ?
C111 K1 C121 125.0(4) . . ?
C111 K1 C2 89.1(4) . . ?
C111 K1 C5 127.2(5) . . ?
C110 K1 C105 146.7(4) . . ?
C110 K1 C122 89.6(3) . . ?
C110 K1 C2 106.9(4) . . ?
C121 K1 C105 111.5(4) . . ?
C121 K1 C112 128.2(4) . . ?
C121 K1 C110 101.4(4) . . ?
C121 K1 C122 23.63(7) . . ?
C121 K1 C2 116.1(4) . . ?
C121 K1 C5 104.2(5) . . ?
C1AA K1 C112 108.8(4) . . ?
C1AA K1 C111 132.5(4) . . ?
C1AA K1 C110 148.0(5) . . ?
C1AA K1 C122 86.2(4) . . ?
C1AA K1 C121 87.0(4) . . ?
C1AA K1 C19 25.64(19) . . ?
C1AA K1 C2 43.5(2) . . ?
C1AA K1 C5 24.70(19) . . ?
C19 K1 C112 85.5(5) . . ?
C19 K1 C111 110.1(5) . . ?
C19 K1 C110 122.4(5) . . ?
C19 K1 C122 82.2(4) . . ?
C19 K1 C121 93.1(4) . . ?
C19 K1 C2 24.43(14) . . ?
C19 K1 C5 43.7(3) . . ?
C2 K1 C122 101.1(4) . . ?
C5 K1 C110 151.2(4) . . ?
C5 K1 C122 109.1(5) . . ?
C5 K1 C2 49.3(2) . . ?
C102 C100 C103 120.0 . . ?
C100 C102 K1 94.3(8) . . ?
C101 C102 K1 73.1(7) . . ?
C101 C102 C100 120.0 . . ?
C102 C101 K1 81.9(7) . . ?
C102 C101 C105 120.0 . . ?
C105 C101 K1 89.9(8) . . ?
C101 C105 K1 66.3(8) . . ?
C104 C105 K1 94.1(7) . . ?
C104 C105 C101 120.0 . . ?
C105 C104 C103 120.0 . . ?
C100 C103 C106 120.0(19) . . ?
C104 C103 C100 120.0 . . ?
C104 C103 C106 119.9(19) . . ?
C113 C114 C115 120.0 . . ?
C113 C114 C116 116.7(15) . . ?
C115 C114 C116 123.2(16) . . ?
C114 C113 K1 82.3(3) . . ?
C114 C113 C112 120.0 . . ?
C112 C113 K1 71.5(3) . . ?
C113 C112 K1 84.9(3) . . ?
C111 C112 K1 74.7(3) . . ?
C111 C112 C113 120.0 . . ?
C112 C111 K1 80.7(3) . . ?
C110 C111 K1 81.7(3) . . ?
C110 C111 C112 120.0 . . ?
C111 C110 K1 73.9(3) . . ?
C111 C110 C115 120.0 . . ?
C115 C110 K1 84.9(3) . . ?
C114 C115 K1 81.4(3) . . ?
C110 C115 K1 71.7(3) . . ?
C110 C115 C114 120.0 . . ?
C123 C124 C125 120.0 . . ?
C123 C124 C126 123.8(14) . . ?
C125 C124 C126 116.1(14) . . ?
C124 C123 C122 120.0 . . ?
C123 C122 K1 107.1(4) . . ?
C123 C122 C121 120.0 . . ?
C121 C122 K1 72.0(5) . . ?
C122 C121 K1 84.4(5) . . ?
C120 C121 K1 101.2(5) . . ?
C120 C121 C122 120.0 . . ?
C121 C120 C125 120.0 . . ?
C120 C125 C124 120.0 . . ?
C202 C201 C200 114(2) . . ?
C202 C201 C206 120.0 . . ?
C206 C201 C200 126(2) . . ?
C201 C202 C203 120.0 . . ?
C204 C203 C202 120.0 . . ?
C205 C204 C203 120.0 . . ?
C204 C205 C206 120.0 . . ?
C205 C206 C201 120.0 . . ?
C19 C1AA K1 78.0(8) . . ?
C19 C1AA C5 120.0 . . ?
C5 C1AA K1 85.5(8) . . ?
C1AA C19 K1 76.4(8) . . ?
C1AA C19 C2 120.0 . . ?
C2 C19 K1 86.4(9) . . ?
C19 C2 K1 69.2(9) . . ?
C2AA C2 K1 85.8(8) . . ?
C2AA C2 C19 120.0 . . ?
C2 C2AA K1 71.1(7) . . ?
C2 C2AA C9 120.0 . . ?
C9 C2AA K1 77.9(7) . . ?
C2AA C9 K1 79.4(7) . . ?
C2AA C9 C5 120.0 . . ?
C5 C9 K1 70.2(8) . . ?
C0AA C9 K1 116(2) . . ?
C0AA C9 C2AA 127(3) . . ?
C0AA C9 C5 113(3) . . ?
C1AA C5 K1 69.8(8) . . ?
C9 C5 K1 86.6(9) . . ?
C9 C5 C1AA 120.0 . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_k9p21n
_database_code_depnum_ccdc_archive 'CCDC 1418082'
_audit_update_record             
;
2015-12-01 deposited with the CCDC.
2015-12-14 downloaded from the CCDC.
;
_audit_creation_date             2015-12-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C18 H54 Ge9 Si8, 2(C18 H36 K N2 O6), 3(C4 H8 O)'
_chemical_formula_sum            'C66 H150 Ge9 K2 N4 O15 Si8'
_chemical_formula_weight         2196.12
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   28.3009(18)
_cell_length_b                   14.6104(9)
_cell_length_c                   28.7838(17)
_cell_angle_alpha                90
_cell_angle_beta                 119.3980(10)
_cell_angle_gamma                90
_cell_volume                     10369.2(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9780
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.281
_cell_measurement_theta_min      2.565
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.794
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0863 before and 0.0362 after correction.
The Ratio of minimum to maximum transmission is 0.7886.
The λ/2 correction factor is 0.0000.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             4528
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.136
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            85281
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.362
_diffrn_reflns_theta_min         1.414
_diffrn_ambient_temperature      150.02
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                16228
_reflns_number_total             21134
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     934
_refine_ls_number_reflns         21134
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0360
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0434P)²+6.2082P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0899
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C301-C300
 1.6 with sigma of 0.01
 C301-C302
 1.54 with sigma of 0.02
 C310-C311
 1.54 with sigma of 0.02
 C322-C321 = C321-C320 = O320-C320 = O320-C323 = C323-C322
 1.54 with sigma of 0.02
 C123-C122 \\sim C121-C120 \\sim C125-C124
 with sigma of 0.02
3. Others
 Fixed Sof: O320(0.5) C320(0.5) H32A(0.5) H32B(0.5) C321(0.5) H32C(0.5)
 H32D(0.5) O330(0.5) C330(0.5) H33A(0.5) H33B(0.5) C331(0.5) H33C(0.5)
 H33D(0.5) H32E(0.5) H32F(0.5) H32G(0.5) H32H(0.5) H32K(0.5) H32L(0.5)
 H32I(0.5) H32J(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C100(H10J,H10K), C101(H10L,H10M), C102(H10N,H10O), C103(H10P,H10Q), C104(H10R,
 H10S), C105(H10T,H10U), C110(H11J,H11K), C111(H11L,H11M), C112(H11N,H11O),
 C113(H11P,H11Q), C114(H11R,H11S), C115(H11T,H11U), C120(H12J,H12K), C121(H12L,
 H12M), C122(H12N,H12O), C123(H12P,H12Q), C124(H12R,H12S), C125(H12T,H12U),
 C200(H20J,H20K), C201(H20L,H20M), C202(H20N,H20O), C203(H20P,H20Q), C204(H20R,
 H20S), C205(H20T,H20U), C210(H21J,H21K), C211(H21L,H21M), C212(H21N,H21O),
 C213(H21P,H21Q), C214(H21R,H21S), C215(H21T,H21U), C220(H22J,H22K), C221(H22L,
 H22M), C222(H22N,H22O), C223(H22P,H22Q), C224(H22R,H22S), C225(H22T,H22U),
 C300(H30A,H30B), C301(H30C,H30D), C302(H30E,H30F), C303(H30G,H30H), C310(H31A,
 H31B), C311(H31C,H31D), C312(H31E,H31F), C313(H31G,H31H), C320(H32A,H32B),
 C321(H32C,H32D), C330(H33A,H33B), C331(H33C,H33D), C322(H32E,H32F), C322(H32G,
 H32H), C323(H32K,H32L), C323(H32I,H32J)
4.b Me refined with riding coordinates:
 C10A(H10A,H10B,H10C), C10C(H10D,H10E,H10F), C10B(H10G,H10H,H10I), C11A(H11A,
 H11B,H11C), C11C(H11D,H11E,H11F), C11B(H11G,H11H,H11I), C12A(H12A,H12B,H12C),
 C12C(H12D,H12E,H12F), C12B(H12G,H12H,H12I), C20A(H20A,H20B,H20C), C20C(H20D,
 H20E,H20F), C20B(H20G,H20H,H20I), C21B(H21A,H21B,H21C), C21A(H21D,H21E,H21F),
 C21C(H21G,H21H,H21I), C22A(H22A,H22B,H22C), C22C(H22D,H22E,H22F), C22B(H22G,
 H22H,H22I)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.67579(2) 0.13622(2) -0.02380(2) 0.02607(8) Uani 1 1 d . . . . .
Ge2 Ge 0.79797(2) 0.06968(2) 0.02858(2) 0.02449(8) Uani 1 1 d . . . . .
Ge3 Ge 0.74025(2) 0.09278(2) 0.07293(2) 0.02531(8) Uani 1 1 d . . . . .
Ge4 Ge 0.73471(2) 0.11916(2) -0.06752(2) 0.03008(9) Uani 1 1 d . . . . .
Ge5 Ge 0.65976(2) -0.01859(2) 0.01199(2) 0.02689(8) Uani 1 1 d . . . . .
Ge6 Ge 0.76410(2) -0.07455(2) 0.05650(2) 0.02620(8) Uani 1 1 d . . . . .
Ge7 Ge 0.75991(2) -0.05537(2) -0.04509(2) 0.02839(8) Uani 1 1 d . . . . .
Ge8 Ge 0.65553(2) 0.00105(3) -0.08968(2) 0.02994(9) Uani 1 1 d . . . . .
Ge9 Ge 0.68910(2) -0.14454(2) -0.03156(2) 0.03460(9) Uani 1 1 d . . . . .
Si1 Si 0.59035(4) 0.21566(6) -0.05987(3) 0.02489(19) Uani 1 1 d . . . . .
Si2 Si 0.89468(3) 0.04839(6) 0.07154(3) 0.02215(18) Uani 1 1 d . . . . .
Si10 Si 0.56584(4) 0.27563(7) -0.14417(4) 0.0363(2) Uani 1 1 d . . . . .
Si11 Si 0.51698(4) 0.13048(7) -0.06687(4) 0.0358(2) Uani 1 1 d . . . . .
Si12 Si 0.60557(4) 0.33826(7) -0.00145(4) 0.0354(2) Uani 1 1 d . . . . .
Si20 Si 0.93260(4) 0.04853(7) 0.16448(3) 0.0314(2) Uani 1 1 d . . . . .
Si21 Si 0.92520(4) -0.08321(6) 0.04780(3) 0.02571(19) Uani 1 1 d . . . . .
Si22 Si 0.92455(4) 0.17826(7) 0.04596(4) 0.0362(2) Uani 1 1 d . . . . .
C10A C 0.53389(19) 0.1861(3) -0.19692(14) 0.0589(12) Uani 1 1 d . . . . .
H10A H 0.5024 0.1602 -0.1961 0.088 Uiso 1 1 calc R . . . .
H10B H 0.5222 0.2136 -0.2319 0.088 Uiso 1 1 calc R . . . .
H10C H 0.5603 0.1375 -0.1904 0.088 Uiso 1 1 calc R . . . .
C10C C 0.51602(18) 0.3728(3) -0.16042(15) 0.0570(12) Uani 1 1 d . . . . .
H10D H 0.5323 0.4203 -0.1330 0.085 Uiso 1 1 calc R . . . .
H10E H 0.5069 0.3987 -0.1952 0.085 Uiso 1 1 calc R . . . .
H10F H 0.4830 0.3497 -0.1615 0.085 Uiso 1 1 calc R . . . .
C10B C 0.62557(17) 0.3230(3) -0.14724(17) 0.0618(13) Uani 1 1 d . . . . .
H10G H 0.6430 0.3702 -0.1198 0.093 Uiso 1 1 calc R . . . .
H10H H 0.6515 0.2737 -0.1410 0.093 Uiso 1 1 calc R . . . .
H10I H 0.6135 0.3498 -0.1825 0.093 Uiso 1 1 calc R . . . .
C11A C 0.51059(16) 0.0166(3) -0.09887(15) 0.0436(9) Uani 1 1 d . . . . .
H11A H 0.5076 0.0251 -0.1340 0.065 Uiso 1 1 calc R . . . .
H11B H 0.5427 -0.0205 -0.0764 0.065 Uiso 1 1 calc R . . . .
H11C H 0.4781 -0.0147 -0.1030 0.065 Uiso 1 1 calc R . . . .
C11C C 0.52281(19) 0.1171(3) 0.00033(16) 0.0555(11) Uani 1 1 d . . . . .
H11D H 0.5261 0.1776 0.0164 0.083 Uiso 1 1 calc R . . . .
H11E H 0.4904 0.0862 -0.0034 0.083 Uiso 1 1 calc R . . . .
H11F H 0.5550 0.0805 0.0232 0.083 Uiso 1 1 calc R . . . .
C11B C 0.45142(16) 0.1929(3) -0.1096(2) 0.0674(13) Uani 1 1 d . . . . .
H11G H 0.4529 0.2535 -0.0943 0.101 Uiso 1 1 calc R . . . .
H11H H 0.4461 0.1999 -0.1458 0.101 Uiso 1 1 calc R . . . .
H11I H 0.4212 0.1579 -0.1110 0.101 Uiso 1 1 calc R . . . .
C12A C 0.54234(17) 0.4021(3) -0.01615(15) 0.0539(11) Uani 1 1 d . . . . .
H12A H 0.5164 0.3599 -0.0142 0.081 Uiso 1 1 calc R . . . .
H12B H 0.5513 0.4511 0.0101 0.081 Uiso 1 1 calc R . . . .
H12C H 0.5262 0.4286 -0.0520 0.081 Uiso 1 1 calc R . . . .
C12C C 0.63599(16) 0.2963(3) 0.06904(13) 0.0464(10) Uani 1 1 d . . . . .
H12D H 0.6694 0.2624 0.0785 0.070 Uiso 1 1 calc R . . . .
H12E H 0.6444 0.3487 0.0931 0.070 Uiso 1 1 calc R . . . .
H12F H 0.6101 0.2560 0.0724 0.070 Uiso 1 1 calc R . . . .
C12B C 0.65372(18) 0.4217(3) -0.00561(17) 0.0548(11) Uani 1 1 d . . . . .
H12G H 0.6873 0.3899 0.0019 0.082 Uiso 1 1 calc R . . . .
H12H H 0.6370 0.4480 -0.0415 0.082 Uiso 1 1 calc R . . . .
H12I H 0.6620 0.4706 0.0206 0.082 Uiso 1 1 calc R . . . .
C20A C 0.89677(15) 0.1312(3) 0.18602(13) 0.0456(10) Uani 1 1 d . . . . .
H20A H 0.8986 0.1927 0.1734 0.068 Uiso 1 1 calc R . . . .
H20B H 0.8587 0.1128 0.1710 0.068 Uiso 1 1 calc R . . . .
H20C H 0.9142 0.1315 0.2250 0.068 Uiso 1 1 calc R . . . .
C20C C 0.92784(19) -0.0670(3) 0.18959(14) 0.0572(12) Uani 1 1 d . . . . .
H20D H 0.9463 -0.1120 0.1789 0.086 Uiso 1 1 calc R . . . .
H20E H 0.9451 -0.0656 0.2286 0.086 Uiso 1 1 calc R . . . .
H20F H 0.8896 -0.0842 0.1745 0.086 Uiso 1 1 calc R . . . .
C20B C 1.00593(16) 0.0824(4) 0.19801(15) 0.0617(13) Uani 1 1 d . . . . .
H20G H 1.0093 0.1430 0.1854 0.092 Uiso 1 1 calc R . . . .
H20H H 1.0205 0.0843 0.2367 0.092 Uiso 1 1 calc R . . . .
H20I H 1.0263 0.0376 0.1895 0.092 Uiso 1 1 calc R . . . .
C21B C 1.00063(14) -0.0977(3) 0.09241(15) 0.0433(9) Uani 1 1 d . . . . .
H21A H 1.0195 -0.0434 0.0897 0.065 Uiso 1 1 calc R . . . .
H21B H 1.0087 -0.1052 0.1294 0.065 Uiso 1 1 calc R . . . .
H21C H 1.0129 -0.1519 0.0813 0.065 Uiso 1 1 calc R . . . .
C21A C 0.89223(14) -0.1886(2) 0.05515(13) 0.0353(8) Uani 1 1 d . . . . .
H21D H 0.8982 -0.1922 0.0916 0.053 Uiso 1 1 calc R . . . .
H21E H 0.8532 -0.1863 0.0300 0.053 Uiso 1 1 calc R . . . .
H21F H 0.9080 -0.2426 0.0477 0.053 Uiso 1 1 calc R . . . .
C21C C 0.91412(16) -0.0754(3) -0.02157(13) 0.0415(9) Uani 1 1 d . . . . .
H21G H 0.9315 -0.0199 -0.0251 0.062 Uiso 1 1 calc R . . . .
H21H H 0.9299 -0.1292 -0.0292 0.062 Uiso 1 1 calc R . . . .
H21I H 0.8751 -0.0730 -0.0469 0.062 Uiso 1 1 calc R . . . .
C22A C 0.89633(18) 0.2826(3) 0.06157(18) 0.0559(11) Uani 1 1 d . . . . .
H22A H 0.9088 0.2846 0.0999 0.084 Uiso 1 1 calc R . . . .
H22B H 0.9088 0.3375 0.0512 0.084 Uiso 1 1 calc R . . . .
H22C H 0.8566 0.2803 0.0417 0.084 Uiso 1 1 calc R . . . .
C22C C 1.00017(17) 0.1921(3) 0.0796(2) 0.0679(13) Uani 1 1 d . . . . .
H22D H 1.0150 0.1940 0.1184 0.102 Uiso 1 1 calc R . . . .
H22E H 1.0160 0.1403 0.0704 0.102 Uiso 1 1 calc R . . . .
H22F H 1.0090 0.2492 0.0678 0.102 Uiso 1 1 calc R . . . .
C22B C 0.9004(2) 0.1754(3) -0.02724(17) 0.0643(13) Uani 1 1 d . . . . .
H22G H 0.9150 0.1210 -0.0357 0.096 Uiso 1 1 calc R . . . .
H22H H 0.8607 0.1732 -0.0469 0.096 Uiso 1 1 calc R . . . .
H22I H 0.9129 0.2305 -0.0374 0.096 Uiso 1 1 calc R . . . .
K1 K 0.76825(3) 0.53394(5) -0.18528(3) 0.03030(16) Uani 1 1 d . . . . .
N1 N 0.75720(15) 0.5964(2) -0.09126(13) 0.0543(9) Uani 1 1 d . . . . .
N2 N 0.77649(18) 0.4743(3) -0.28069(14) 0.0647(11) Uani 1 1 d . . . . .
O10 O 0.66554(12) 0.5761(2) -0.19444(12) 0.0623(8) Uani 1 1 d . . . . .
O11 O 0.67737(12) 0.5498(2) -0.28559(10) 0.0657(9) Uani 1 1 d . . . . .
O12 O 0.81927(11) 0.69640(18) -0.13332(10) 0.0497(7) Uani 1 1 d . . . . .
O13 O 0.84311(10) 0.62106(17) -0.20993(9) 0.0420(6) Uani 1 1 d . . . . .
O14 O 0.79640(13) 0.4145(2) -0.10060(12) 0.0646(9) Uani 1 1 d . . . . .
O15 O 0.78459(15) 0.3481(2) -0.19964(15) 0.0757(10) Uani 1 1 d . . . . .
C100 C 0.7016(2) 0.5940(4) -0.1018(2) 0.0739(16) Uani 1 1 d . . . . .
H10J H 0.6987 0.6303 -0.0742 0.089 Uiso 1 1 calc R . . . .
H10K H 0.6916 0.5300 -0.0992 0.089 Uiso 1 1 calc R . . . .
C101 C 0.6622(2) 0.6313(4) -0.1560(2) 0.0822(16) Uani 1 1 d . . . . .
H10L H 0.6248 0.6299 -0.1613 0.099 Uiso 1 1 calc R . . . .
H10M H 0.6714 0.6955 -0.1592 0.099 Uiso 1 1 calc R . . . .
C102 C 0.62451(19) 0.5964(4) -0.2468(2) 0.0846(17) Uani 1 1 d . . . . .
H10N H 0.6286 0.6602 -0.2559 0.101 Uiso 1 1 calc R . . . .
H10O H 0.5885 0.5903 -0.2493 0.101 Uiso 1 1 calc R . . . .
C103 C 0.62861(19) 0.5334(5) -0.2839(2) 0.0840(18) Uani 1 1 d . . . . .
H10P H 0.6283 0.4696 -0.2725 0.101 Uiso 1 1 calc R . . . .
H10Q H 0.5970 0.5417 -0.3199 0.101 Uiso 1 1 calc R . . . .
C104 C 0.6771(2) 0.5007(5) -0.32760(17) 0.104(2) Uani 1 1 d . . . . .
H10R H 0.6466 0.5219 -0.3620 0.124 Uiso 1 1 calc R . . . .
H10S H 0.6718 0.4348 -0.3237 0.124 Uiso 1 1 calc R . . . .
C105 C 0.7290(2) 0.5141(4) -0.32758(17) 0.092(2) Uani 1 1 d . . . . .
H10T H 0.7260 0.4862 -0.3603 0.111 Uiso 1 1 calc R . . . .
H10U H 0.7352 0.5806 -0.3288 0.111 Uiso 1 1 calc R . . . .
C110 C 0.7779(2) 0.6904(4) -0.0778(2) 0.0783(16) Uani 1 1 d . . . . .
H11J H 0.7848 0.7045 -0.0413 0.094 Uiso 1 1 calc R . . . .
H11K H 0.7495 0.7331 -0.1026 0.094 Uiso 1 1 calc R . . . .
C111 C 0.8287(2) 0.7075(4) -0.08023(18) 0.0824(18) Uani 1 1 d . . . . .
H11L H 0.8417 0.7704 -0.0678 0.099 Uiso 1 1 calc R . . . .
H11M H 0.8572 0.6642 -0.0563 0.099 Uiso 1 1 calc R . . . .
C112 C 0.86568(17) 0.7210(3) -0.13696(16) 0.0526(11) Uani 1 1 d . . . . .
H11N H 0.8962 0.6800 -0.1141 0.063 Uiso 1 1 calc R . . . .
H11O H 0.8764 0.7845 -0.1242 0.063 Uiso 1 1 calc R . . . .
C113 C 0.85388(17) 0.7135(3) -0.19342(16) 0.0491(10) Uani 1 1 d . . . . .
H11P H 0.8221 0.7519 -0.2167 0.059 Uiso 1 1 calc R . . . .
H11Q H 0.8854 0.7357 -0.1963 0.059 Uiso 1 1 calc R . . . .
C114 C 0.8380(2) 0.6084(3) -0.26121(17) 0.0602(12) Uani 1 1 d . . . . .
H11R H 0.8717 0.6280 -0.2607 0.072 Uiso 1 1 calc R . . . .
H11S H 0.8076 0.6459 -0.2879 0.072 Uiso 1 1 calc R . . . .
C115 C 0.8275(2) 0.5087(3) -0.27585(19) 0.0698(15) Uani 1 1 d . . . . .
H11T H 0.8269 0.4990 -0.3102 0.084 Uiso 1 1 calc R . . . .
H11U H 0.8579 0.4723 -0.2484 0.084 Uiso 1 1 calc R . . . .
C120 C 0.7898(2) 0.5352(4) -0.04792(17) 0.0809(17) Uani 1 1 d D . . . .
H12J H 0.7826 0.5476 -0.0181 0.097 Uiso 1 1 calc R . . . .
H12K H 0.8286 0.5488 -0.0351 0.097 Uiso 1 1 calc R . . . .
C121 C 0.7800(2) 0.4353(4) -0.06190(19) 0.0854(18) Uani 1 1 d D . . . .
H12L H 0.8010 0.3977 -0.0295 0.102 Uiso 1 1 calc R . . . .
H12M H 0.7410 0.4210 -0.0766 0.102 Uiso 1 1 calc R . . . .
C122 C 0.7837(2) 0.3234(4) -0.1186(2) 0.0901(19) Uani 1 1 d D . . . .
H12N H 0.7439 0.3166 -0.1406 0.108 Uiso 1 1 calc R . . . .
H12O H 0.7963 0.2818 -0.0876 0.108 Uiso 1 1 calc R . . . .
C123 C 0.8098(3) 0.2981(3) -0.1505(3) 0.105(2) Uani 1 1 d D . . . .
H12P H 0.8490 0.3128 -0.1304 0.126 Uiso 1 1 calc R . . . .
H12Q H 0.8059 0.2316 -0.1579 0.126 Uiso 1 1 calc R . . . .
C124 C 0.8086(3) 0.3280(4) -0.2316(3) 0.110(3) Uani 1 1 d D . . . .
H12R H 0.8090 0.2610 -0.2367 0.133 Uiso 1 1 calc R . . . .
H12S H 0.8465 0.3503 -0.2140 0.133 Uiso 1 1 calc R . . . .
C125 C 0.7760(3) 0.3744(4) -0.2847(3) 0.109(3) Uani 1 1 d D . . . .
H12T H 0.7908 0.3567 -0.3083 0.131 Uiso 1 1 calc R . . . .
H12U H 0.7381 0.3525 -0.3014 0.131 Uiso 1 1 calc R . . . .
K2 K 0.72442(3) 0.02440(4) 0.30127(2) 0.02400(14) Uani 1 1 d . . . . .
N3 N 0.75396(11) -0.07153(19) 0.22653(10) 0.0306(6) Uani 1 1 d . . . . .
N4 N 0.69580(11) 0.12236(17) 0.37579(9) 0.0263(6) Uani 1 1 d . . . . .
O20 O 0.65882(9) 0.04861(15) 0.19050(8) 0.0300(5) Uani 1 1 d . . . . .
O21 O 0.64493(9) 0.16379(15) 0.26135(8) 0.0301(5) Uani 1 1 d . . . . .
O22 O 0.72905(9) -0.16677(14) 0.30116(8) 0.0315(5) Uani 1 1 d . . . . .
O23 O 0.68217(10) -0.07623(15) 0.35650(8) 0.0320(5) Uani 1 1 d . . . . .
O24 O 0.82873(9) 0.05364(16) 0.31113(9) 0.0343(5) Uani 1 1 d . . . . .
O25 O 0.80666(9) 0.11508(15) 0.39224(8) 0.0330(5) Uani 1 1 d . . . . .
C200 C 0.70760(15) -0.0651(2) 0.17164(13) 0.0375(9) Uani 1 1 d . . . . .
H20J H 0.6799 -0.1107 0.1674 0.045 Uiso 1 1 calc R . . . .
H20K H 0.7203 -0.0811 0.1462 0.045 Uiso 1 1 calc R . . . .
C201 C 0.68152(16) 0.0274(3) 0.15742(13) 0.0378(9) Uani 1 1 d . . . . .
H20L H 0.7089 0.0742 0.1622 0.045 Uiso 1 1 calc R . . . .
H20M H 0.6527 0.0280 0.1196 0.045 Uiso 1 1 calc R . . . .
C202 C 0.62887(14) 0.1313(2) 0.17385(12) 0.0346(8) Uani 1 1 d . . . . .
H20N H 0.6004 0.1264 0.1360 0.042 Uiso 1 1 calc R . . . .
H20O H 0.6532 0.1825 0.1772 0.042 Uiso 1 1 calc R . . . .
C203 C 0.60350(15) 0.1491(3) 0.20761(12) 0.0403(9) Uani 1 1 d . . . . .
H20P H 0.5798 0.2037 0.1943 0.048 Uiso 1 1 calc R . . . .
H20Q H 0.5809 0.0961 0.2059 0.048 Uiso 1 1 calc R . . . .
C204 C 0.62179(15) 0.1927(3) 0.29295(13) 0.0406(9) Uani 1 1 d . . . . .
H20R H 0.5959 0.1460 0.2917 0.049 Uiso 1 1 calc R . . . .
H20S H 0.6018 0.2508 0.2787 0.049 Uiso 1 1 calc R . . . .
C205 C 0.66595(15) 0.2064(2) 0.34952(12) 0.0369(9) Uani 1 1 d . . . . .
H20T H 0.6920 0.2522 0.3499 0.044 Uiso 1 1 calc R . . . .
H20U H 0.6497 0.2318 0.3704 0.044 Uiso 1 1 calc R . . . .
C210 C 0.76557(16) -0.1682(2) 0.24224(15) 0.0411(9) Uani 1 1 d . . . . .
H21J H 0.8024 -0.1729 0.2734 0.049 Uiso 1 1 calc R . . . .
H21K H 0.7654 -0.2030 0.2126 0.049 Uiso 1 1 calc R . . . .
C211 C 0.72613(16) -0.2114(2) 0.25597(14) 0.0393(9) Uani 1 1 d . . . . .
H21L H 0.6889 -0.2062 0.2253 0.047 Uiso 1 1 calc R . . . .
H21M H 0.7347 -0.2771 0.2638 0.047 Uiso 1 1 calc R . . . .
C212 C 0.69555(16) -0.2113(2) 0.31809(13) 0.0373(8) Uani 1 1 d . . . . .
H21N H 0.7054 -0.2769 0.3248 0.045 Uiso 1 1 calc R . . . .
H21O H 0.6571 -0.2070 0.2898 0.045 Uiso 1 1 calc R . . . .
C213 C 0.70282(16) -0.1669(2) 0.36806(13) 0.0367(8) Uani 1 1 d . . . . .
H21P H 0.6833 -0.2025 0.3827 0.044 Uiso 1 1 calc R . . . .
H21Q H 0.7418 -0.1656 0.3951 0.044 Uiso 1 1 calc R . . . .
C214 C 0.68260(16) -0.0347(2) 0.40149(13) 0.0372(9) Uani 1 1 d . . . . .
H21R H 0.7200 -0.0341 0.4320 0.045 Uiso 1 1 calc R . . . .
H21S H 0.6595 -0.0703 0.4119 0.045 Uiso 1 1 calc R . . . .
C215 C 0.66157(15) 0.0619(2) 0.38753(13) 0.0347(8) Uani 1 1 d . . . . .
H21T H 0.6247 0.0602 0.3561 0.042 Uiso 1 1 calc R . . . .
H21U H 0.6584 0.0880 0.4176 0.042 Uiso 1 1 calc R . . . .
C220 C 0.80154(15) -0.0266(3) 0.22904(14) 0.0410(9) Uani 1 1 d . . . . .
H22J H 0.7902 0.0325 0.2098 0.049 Uiso 1 1 calc R . . . .
H22K H 0.8158 -0.0654 0.2105 0.049 Uiso 1 1 calc R . . . .
C221 C 0.84665(16) -0.0091(3) 0.28548(16) 0.0456(10) Uani 1 1 d . . . . .
H22L H 0.8574 -0.0674 0.3056 0.055 Uiso 1 1 calc R . . . .
H22M H 0.8787 0.0162 0.2847 0.055 Uiso 1 1 calc R . . . .
C222 C 0.86978(14) 0.0698(3) 0.36481(14) 0.0418(9) Uani 1 1 d . . . . .
H22N H 0.9040 0.0873 0.3657 0.050 Uiso 1 1 calc R . . . .
H22O H 0.8764 0.0132 0.3860 0.050 Uiso 1 1 calc R . . . .
C223 C 0.85221(15) 0.1447(3) 0.38830(14) 0.0389(9) Uani 1 1 d . . . . .
H22P H 0.8822 0.1608 0.4241 0.047 Uiso 1 1 calc R . . . .
H22Q H 0.8426 0.1999 0.3654 0.047 Uiso 1 1 calc R . . . .
C224 C 0.78992(15) 0.1835(2) 0.41694(13) 0.0382(9) Uani 1 1 d . . . . .
H22R H 0.7768 0.2384 0.3939 0.046 Uiso 1 1 calc R . . . .
H22S H 0.8211 0.2017 0.4516 0.046 Uiso 1 1 calc R . . . .
C225 C 0.74557(14) 0.1458(2) 0.42535(12) 0.0326(8) Uani 1 1 d . . . . .
H22T H 0.7591 0.0901 0.4477 0.039 Uiso 1 1 calc R . . . .
H22U H 0.7365 0.1913 0.4452 0.039 Uiso 1 1 calc R . . . .
O300 O 0.4691(3) 0.0863(7) 0.2305(4) 0.242(5) Uani 1 1 d . . . . .
C300 C 0.4917(5) 0.0293(8) 0.2784(5) 0.254(9) Uani 1 1 d D . . . .
H30A H 0.4647 -0.0129 0.2791 0.305 Uiso 1 1 calc R . . . .
H30B H 0.5243 -0.0052 0.2841 0.305 Uiso 1 1 calc R . . . .
C301 C 0.5045(5) 0.1048(7) 0.3144(3) 0.177(5) Uani 1 1 d D . . . .
H30C H 0.4992 0.0847 0.3443 0.213 Uiso 1 1 calc R . . . .
H30D H 0.5435 0.1190 0.3294 0.213 Uiso 1 1 calc R . . . .
C302 C 0.4760(5) 0.1839(6) 0.2943(4) 0.166(4) Uani 1 1 d D . . . .
H30E H 0.5010 0.2368 0.3047 0.199 Uiso 1 1 calc R . . . .
H30F H 0.4506 0.1936 0.3082 0.199 Uiso 1 1 calc R . . . .
C303 C 0.4470(4) 0.1752(7) 0.2383(4) 0.181(4) Uani 1 1 d . . . . .
H30G H 0.4547 0.2266 0.2207 0.217 Uiso 1 1 calc R . . . .
H30H H 0.4074 0.1715 0.2248 0.217 Uiso 1 1 calc R . . . .
O310 O 1.0367(7) -0.3937(9) 0.0679(6) 0.357(8) Uani 1 1 d . . . . .
C310 C 0.9792(8) -0.3861(10) 0.0365(7) 0.292(13) Uani 1 1 d D . . . .
H31A H 0.9659 -0.3276 0.0432 0.350 Uiso 1 1 calc R . . . .
H31B H 0.9667 -0.3921 -0.0020 0.350 Uiso 1 1 calc R . . . .
C311 C 0.9632(5) -0.4607(8) 0.0558(5) 0.197(5) Uani 1 1 d D . . . .
H31C H 0.9320 -0.4918 0.0260 0.237 Uiso 1 1 calc R . . . .
H31D H 0.9521 -0.4396 0.0817 0.237 Uiso 1 1 calc R . . . .
C312 C 1.0085(4) -0.5236(6) 0.0815(5) 0.187(5) Uani 1 1 d . . . . .
H31E H 1.0122 -0.5449 0.1158 0.225 Uiso 1 1 calc R . . . .
H31F H 1.0023 -0.5776 0.0585 0.225 Uiso 1 1 calc R . . . .
C313 C 1.0563(5) -0.4774(10) 0.0906(6) 0.247(7) Uani 1 1 d . . . . .
H31G H 1.0822 -0.4716 0.1292 0.296 Uiso 1 1 calc R . . . .
H31H H 1.0742 -0.5092 0.0731 0.296 Uiso 1 1 calc R . . . .
O320 O 0.4461(5) 0.2842(9) 0.0554(5) 0.144(4) Uiso 0.5 1 d D . P A 1
C320 C 0.4252(6) 0.3507(10) 0.0763(5) 0.112(4) Uiso 0.5 1 d D . P A 1
H32A H 0.4173 0.4066 0.0542 0.135 Uiso 0.5 1 calc R . P A 1
H32B H 0.3902 0.3276 0.0714 0.135 Uiso 0.5 1 calc R . P A 1
C321 C 0.4546(7) 0.3750(13) 0.1261(6) 0.139(6) Uiso 0.5 1 d D . P A 1
H32C H 0.4439 0.3385 0.1485 0.167 Uiso 0.5 1 calc R . P A 1
H32D H 0.4482 0.4404 0.1301 0.167 Uiso 0.5 1 calc R . P A 1
O330 O 0.4853(4) 0.3026(6) 0.1593(3) 0.103(3) Uiso 0.5 1 d . . P A 2
C330 C 0.4547(6) 0.2396(10) 0.1193(5) 0.107(4) Uiso 0.5 1 d . . P A 2
H33A H 0.4596 0.1765 0.1335 0.129 Uiso 0.5 1 calc R . P A 2
H33B H 0.4157 0.2555 0.1006 0.129 Uiso 0.5 1 calc R . P A 2
C331 C 0.4735(9) 0.2485(14) 0.0923(8) 0.163(7) Uiso 0.5 1 d . . P A 2
H33C H 0.4456 0.2313 0.0556 0.196 Uiso 0.5 1 calc R . P A 2
H33D H 0.5034 0.2039 0.1038 0.196 Uiso 0.5 1 calc R . P A 2
C322 C 0.5094(5) 0.3612(7) 0.1432(4) 0.173(4) Uani 1 1 d D . . . .
H32E H 0.5257 0.3094 0.1683 0.207 Uiso 0.5 1 calc R . P A 1
H32F H 0.5319 0.4170 0.1570 0.207 Uiso 0.5 1 calc R . P A 1
H32G H 0.5493 0.3572 0.1663 0.207 Uiso 0.5 1 calc R . P A 2
H32H H 0.4979 0.4243 0.1451 0.207 Uiso 0.5 1 calc R . P A 2
C323 C 0.4949(7) 0.3394(9) 0.0894(5) 0.324(11) Uani 1 1 d D . . . .
H32K H 0.5265 0.3359 0.0835 0.389 Uiso 0.5 1 calc R . P A 2
H32L H 0.4669 0.3807 0.0629 0.389 Uiso 0.5 1 calc R . P A 2
H32I H 0.5262 0.3073 0.0905 0.389 Uiso 0.5 1 calc R . P A 1
H32J H 0.4910 0.3981 0.0706 0.389 Uiso 0.5 1 calc R . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 Ge3 2.5486(5) . ?
Ge1 Ge4 2.5469(5) . ?
Ge1 Ge5 2.6155(5) . ?
Ge1 Ge8 2.5995(5) . ?
Ge1 Si1 2.4098(9) . ?
Ge2 Ge3 2.5415(5) . ?
Ge2 Ge4 2.5528(5) . ?
Ge2 Ge6 2.6005(5) . ?
Ge2 Ge7 2.5986(5) . ?
Ge2 Si2 2.4071(9) . ?
Ge3 Ge5 2.6439(5) . ?
Ge3 Ge6 2.6399(5) . ?
Ge4 Ge7 2.6411(5) . ?
Ge4 Ge8 2.6463(5) . ?
Ge5 Ge6 2.7046(5) . ?
Ge5 Ge8 2.8837(5) . ?
Ge5 Ge9 2.5824(5) . ?
Ge6 Ge7 2.8816(5) . ?
Ge6 Ge9 2.5872(5) . ?
Ge7 Ge8 2.7076(5) . ?
Ge7 Ge9 2.5752(5) . ?
Ge8 Ge9 2.5819(5) . ?
Si1 Si10 2.3420(12) . ?
Si1 Si11 2.3430(13) . ?
Si1 Si12 2.3473(13) . ?
Si2 Si20 2.3431(12) . ?
Si2 Si21 2.3429(12) . ?
Si2 Si22 2.3383(13) . ?
Si10 C10A 1.867(4) . ?
Si10 C10C 1.890(4) . ?
Si10 C10B 1.868(4) . ?
Si11 C11A 1.868(4) . ?
Si11 C11C 1.869(4) . ?
Si11 C11B 1.884(4) . ?
Si12 C12A 1.873(4) . ?
Si12 C12C 1.876(4) . ?
Si12 C12B 1.875(4) . ?
Si20 C20A 1.868(3) . ?
Si20 C20C 1.867(4) . ?
Si20 C20B 1.875(4) . ?
Si21 C21B 1.887(4) . ?
Si21 C21A 1.865(3) . ?
Si21 C21C 1.866(3) . ?
Si22 C22A 1.875(4) . ?
Si22 C22C 1.877(4) . ?
Si22 C22B 1.869(4) . ?
K1 N1 3.014(3) . ?
K1 N2 2.997(3) . ?
K1 O10 2.854(3) . ?
K1 O11 2.777(3) . ?
K1 O12 2.799(3) . ?
K1 O13 2.844(2) . ?
K1 O14 2.777(3) . ?
K1 O15 2.819(3) . ?
K1 C122 3.537(5) . ?
N1 C100 1.451(6) . ?
N1 C110 1.468(5) . ?
N1 C120 1.441(6) . ?
N2 C105 1.478(7) . ?
N2 C115 1.469(6) . ?
N2 C125 1.464(6) . ?
O10 C101 1.411(6) . ?
O10 C102 1.410(6) . ?
O11 C103 1.425(6) . ?
O11 C104 1.402(6) . ?
O12 C111 1.426(5) . ?
O12 C112 1.414(4) . ?
O13 C113 1.415(4) . ?
O13 C114 1.423(4) . ?
O14 C121 1.434(5) . ?
O14 C122 1.410(6) . ?
O15 C123 1.432(6) . ?
O15 C124 1.419(6) . ?
C100 C101 1.505(7) . ?
C102 C103 1.457(8) . ?
C104 C105 1.483(7) . ?
C110 C111 1.495(6) . ?
C112 C113 1.494(5) . ?
C114 C115 1.506(6) . ?
C120 C121 1.505(7) . ?
C122 C123 1.482(7) . ?
C124 C125 1.504(8) . ?
K2 N3 3.009(3) . ?
K2 N4 3.002(3) . ?
K2 O20 2.815(2) . ?
K2 O21 2.827(2) . ?
K2 O22 2.796(2) . ?
K2 O23 2.826(2) . ?
K2 O24 2.856(2) . ?
K2 O25 2.837(2) . ?
N3 C200 1.480(4) . ?
N3 C210 1.470(4) . ?
N3 C220 1.468(4) . ?
N4 C205 1.472(4) . ?
N4 C215 1.468(4) . ?
N4 C225 1.471(4) . ?
O20 C201 1.420(4) . ?
O20 C202 1.417(4) . ?
O21 C203 1.426(4) . ?
O21 C204 1.421(4) . ?
O22 C211 1.420(4) . ?
O22 C212 1.419(4) . ?
O23 C213 1.420(4) . ?
O23 C214 1.425(4) . ?
O24 C221 1.417(4) . ?
O24 C222 1.425(4) . ?
O25 C223 1.416(4) . ?
O25 C224 1.435(4) . ?
C200 C201 1.497(5) . ?
C202 C203 1.487(5) . ?
C204 C205 1.502(5) . ?
C210 C211 1.494(5) . ?
C212 C213 1.497(4) . ?
C214 C215 1.507(5) . ?
C220 C221 1.516(5) . ?
C222 C223 1.495(5) . ?
C224 C225 1.495(5) . ?
O300 C300 1.462(14) . ?
O300 C303 1.504(11) . ?
C300 C301 1.432(8) . ?
C301 C302 1.366(10) . ?
C302 C303 1.409(11) . ?
O310 C310 1.428(19) . ?
O310 C313 1.368(14) . ?
C310 C311 1.394(13) . ?
C311 C312 1.450(12) . ?
C312 C313 1.416(13) . ?
O320 C320 1.416(14) . ?
O320 C323 1.479(14) . ?
C320 C321 1.306(14) . ?
C321 C322 1.394(13) . ?
O330 C330 1.394(14) . ?
O330 C322 1.314(12) . ?
C330 C331 1.14(2) . ?
C331 C323 1.48(2) . ?
C322 C323 1.429(11) . ?

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
Ge3 Ge1 Ge5 61.575(13) . . ?
Ge3 Ge1 Ge8 113.017(16) . . ?
Ge4 Ge1 Ge3 102.957(16) . . ?
Ge4 Ge1 Ge5 113.089(16) . . ?
Ge4 Ge1 Ge8 61.880(14) . . ?
Ge8 Ge1 Ge5 67.141(14) . . ?
Si1 Ge1 Ge3 128.27(2) . . ?
Si1 Ge1 Ge4 126.59(2) . . ?
Si1 Ge1 Ge5 104.77(3) . . ?
Si1 Ge1 Ge8 103.66(2) . . ?
Ge3 Ge2 Ge4 102.988(16) . . ?
Ge3 Ge2 Ge6 61.767(13) . . ?
Ge3 Ge2 Ge7 113.077(16) . . ?
Ge4 Ge2 Ge6 113.293(16) . . ?
Ge4 Ge2 Ge7 61.679(14) . . ?
Ge7 Ge2 Ge6 67.318(14) . . ?
Si2 Ge2 Ge3 127.46(2) . . ?
Si2 Ge2 Ge4 127.52(2) . . ?
Si2 Ge2 Ge6 103.61(2) . . ?
Si2 Ge2 Ge7 103.87(2) . . ?
Ge1 Ge3 Ge5 60.458(13) . . ?
Ge1 Ge3 Ge6 98.269(14) . . ?
Ge2 Ge3 Ge1 77.074(14) . . ?
Ge2 Ge3 Ge5 98.163(15) . . ?
Ge2 Ge3 Ge6 60.215(13) . . ?
Ge6 Ge3 Ge5 61.577(13) . . ?
Ge1 Ge4 Ge2 76.903(14) . . ?
Ge1 Ge4 Ge7 97.899(15) . . ?
Ge1 Ge4 Ge8 60.037(14) . . ?
Ge2 Ge4 Ge7 60.012(13) . . ?
Ge2 Ge4 Ge8 97.878(15) . . ?
Ge7 Ge4 Ge8 61.606(14) . . ?
Ge1 Ge5 Ge3 57.966(13) . . ?
Ge1 Ge5 Ge6 95.042(15) . . ?
Ge1 Ge5 Ge8 56.164(12) . . ?
Ge3 Ge5 Ge6 59.137(13) . . ?
Ge3 Ge5 Ge8 101.834(15) . . ?
Ge6 Ge5 Ge8 90.153(14) . . ?
Ge9 Ge5 Ge1 105.418(16) . . ?
Ge9 Ge5 Ge3 112.517(17) . . ?
Ge9 Ge5 Ge6 58.541(13) . . ?
Ge9 Ge5 Ge8 56.046(13) . . ?
Ge2 Ge6 Ge3 58.018(13) . . ?
Ge2 Ge6 Ge5 95.223(15) . . ?
Ge2 Ge6 Ge7 56.309(12) . . ?
Ge3 Ge6 Ge5 59.286(12) . . ?
Ge3 Ge6 Ge7 101.823(14) . . ?
Ge5 Ge6 Ge7 89.906(13) . . ?
Ge9 Ge6 Ge2 105.494(15) . . ?
Ge9 Ge6 Ge3 112.494(16) . . ?
Ge9 Ge6 Ge5 58.367(13) . . ?
Ge9 Ge6 Ge7 55.872(13) . . ?
Ge2 Ge7 Ge4 58.309(13) . . ?
Ge2 Ge7 Ge6 56.373(12) . . ?
Ge2 Ge7 Ge8 95.253(15) . . ?
Ge4 Ge7 Ge6 102.334(14) . . ?
Ge4 Ge7 Ge8 59.292(13) . . ?
Ge8 Ge7 Ge6 90.139(14) . . ?
Ge9 Ge7 Ge2 105.900(16) . . ?
Ge9 Ge7 Ge4 112.870(17) . . ?
Ge9 Ge7 Ge6 56.267(12) . . ?
Ge9 Ge7 Ge8 58.450(14) . . ?
Ge1 Ge8 Ge4 58.084(13) . . ?
Ge1 Ge8 Ge5 56.696(12) . . ?
Ge1 Ge8 Ge7 94.982(15) . . ?
Ge4 Ge8 Ge5 102.231(14) . . ?
Ge4 Ge8 Ge7 59.102(14) . . ?
Ge7 Ge8 Ge5 89.802(13) . . ?
Ge9 Ge8 Ge1 105.902(16) . . ?
Ge9 Ge8 Ge4 112.477(17) . . ?
Ge9 Ge8 Ge5 56.063(13) . . ?
Ge9 Ge8 Ge7 58.209(14) . . ?
Ge5 Ge9 Ge6 63.092(14) . . ?
Ge7 Ge9 Ge5 99.926(16) . . ?
Ge7 Ge9 Ge6 67.861(14) . . ?
Ge7 Ge9 Ge8 63.341(14) . . ?
Ge8 Ge9 Ge5 67.891(14) . . ?
Ge8 Ge9 Ge6 99.970(16) . . ?
Si10 Si1 Ge1 110.54(4) . . ?
Si10 Si1 Si11 108.08(5) . . ?
Si10 Si1 Si12 108.28(5) . . ?
Si11 Si1 Ge1 116.14(4) . . ?
Si11 Si1 Si12 108.07(5) . . ?
Si12 Si1 Ge1 105.45(4) . . ?
Si20 Si2 Ge2 110.76(4) . . ?
Si21 Si2 Ge2 116.44(4) . . ?
Si21 Si2 Si20 107.81(5) . . ?
Si22 Si2 Ge2 103.24(4) . . ?
Si22 Si2 Si20 108.97(5) . . ?
Si22 Si2 Si21 109.40(5) . . ?
C10A Si10 Si1 111.06(14) . . ?
C10A Si10 C10C 108.7(2) . . ?
C10A Si10 C10B 108.0(2) . . ?
C10C Si10 Si1 110.05(13) . . ?
C10B Si10 Si1 111.89(13) . . ?
C10B Si10 C10C 107.0(2) . . ?
C11A Si11 Si1 112.53(13) . . ?
C11A Si11 C11C 110.79(19) . . ?
C11A Si11 C11B 106.5(2) . . ?
C11C Si11 Si1 110.02(14) . . ?
C11C Si11 C11B 106.6(2) . . ?
C11B Si11 Si1 110.24(15) . . ?
C12A Si12 Si1 113.51(14) . . ?
C12A Si12 C12C 106.69(18) . . ?
C12A Si12 C12B 107.8(2) . . ?
C12C Si12 Si1 110.55(13) . . ?
C12B Si12 Si1 109.50(14) . . ?
C12B Si12 C12C 108.62(19) . . ?
C20A Si20 Si2 111.13(12) . . ?
C20A Si20 C20B 107.60(19) . . ?
C20C Si20 Si2 111.19(13) . . ?
C20C Si20 C20A 107.59(19) . . ?
C20C Si20 C20B 108.1(2) . . ?
C20B Si20 Si2 111.02(14) . . ?
C21B Si21 Si2 110.45(12) . . ?
C21A Si21 Si2 111.58(11) . . ?
C21A Si21 C21B 106.99(17) . . ?
C21A Si21 C21C 109.94(16) . . ?
C21C Si21 Si2 111.68(13) . . ?
C21C Si21 C21B 105.95(18) . . ?
C22A Si22 Si2 108.79(13) . . ?
C22A Si22 C22C 107.5(2) . . ?
C22C Si22 Si2 114.92(15) . . ?
C22B Si22 Si2 110.37(15) . . ?
C22B Si22 C22A 109.0(2) . . ?
C22B Si22 C22C 106.2(2) . . ?
N1 K1 C122 79.39(12) . . ?
N2 K1 N1 178.50(12) . . ?
N2 K1 C122 101.53(12) . . ?
O10 K1 N1 57.85(9) . . ?
O10 K1 N2 120.79(11) . . ?
O10 K1 C122 94.96(11) . . ?
O11 K1 N1 117.18(11) . . ?
O11 K1 N2 61.36(11) . . ?
O11 K1 O10 60.30(9) . . ?
O11 K1 O12 117.15(9) . . ?
O11 K1 O13 97.27(8) . . ?
O11 K1 O15 93.59(11) . . ?
O11 K1 C122 116.17(13) . . ?
O12 K1 N1 61.12(8) . . ?
O12 K1 N2 118.97(9) . . ?
O12 K1 O10 95.82(9) . . ?
O12 K1 O13 60.11(7) . . ?
O12 K1 O15 144.73(10) . . ?
O12 K1 C122 123.61(13) . . ?
O13 K1 N1 120.44(8) . . ?
O13 K1 N2 59.94(9) . . ?
O13 K1 O10 136.89(9) . . ?
O13 K1 C122 128.02(10) . . ?
O14 K1 N1 60.91(10) . . ?
O14 K1 N2 120.24(11) . . ?
O14 K1 O10 93.27(9) . . ?
O14 K1 O11 133.23(10) . . ?
O14 K1 O12 102.31(9) . . ?
O14 K1 O13 124.90(9) . . ?
O14 K1 O15 61.74(10) . . ?
O14 K1 C122 21.83(12) . . ?
O15 K1 N1 121.35(10) . . ?
O15 K1 N2 59.56(10) . . ?
O15 K1 O10 115.29(10) . . ?
O15 K1 O13 101.46(8) . . ?
O15 K1 C122 41.97(11) . . ?
C100 N1 K1 112.7(2) . . ?
C100 N1 C110 109.2(4) . . ?
C110 N1 K1 108.5(2) . . ?
C120 N1 K1 106.5(3) . . ?
C120 N1 C100 109.5(4) . . ?
C120 N1 C110 110.4(4) . . ?
C105 N2 K1 106.1(3) . . ?
C115 N2 K1 109.2(2) . . ?
C115 N2 C105 111.2(4) . . ?
C125 N2 K1 111.2(3) . . ?
C125 N2 C105 110.6(4) . . ?
C125 N2 C115 108.5(4) . . ?
C101 O10 K1 120.6(3) . . ?
C102 O10 K1 114.3(3) . . ?
C102 O10 C101 112.4(4) . . ?
C103 O11 K1 111.6(2) . . ?
C104 O11 K1 117.6(3) . . ?
C104 O11 C103 110.4(4) . . ?
C111 O12 K1 116.4(2) . . ?
C112 O12 K1 115.5(2) . . ?
C112 O12 C111 111.0(3) . . ?
C113 O13 K1 114.1(2) . . ?
C113 O13 C114 111.6(3) . . ?
C114 O13 K1 119.5(2) . . ?
C121 O14 K1 119.1(3) . . ?
C122 O14 K1 111.0(3) . . ?
C122 O14 C121 111.3(4) . . ?
C123 O15 K1 112.6(3) . . ?
C124 O15 K1 117.4(3) . . ?
C124 O15 C123 111.7(4) . . ?
N1 C100 C101 112.6(4) . . ?
O10 C101 C100 107.8(4) . . ?
O10 C102 C103 109.3(4) . . ?
O11 C103 C102 110.3(4) . . ?
O11 C104 C105 110.3(4) . . ?
N2 C105 C104 113.8(4) . . ?
N1 C110 C111 114.3(4) . . ?
O12 C111 C110 110.7(4) . . ?
O12 C112 C113 110.0(3) . . ?
O13 C113 C112 109.3(3) . . ?
O13 C114 C115 108.8(3) . . ?
N2 C115 C114 114.0(4) . . ?
N1 C120 C121 114.5(4) . . ?
O14 C121 C120 109.0(4) . . ?
O14 C122 K1 47.1(2) . . ?
O14 C122 C123 110.4(4) . . ?
C123 C122 K1 81.2(3) . . ?
O15 C123 C122 109.0(4) . . ?
O15 C124 C125 108.4(5) . . ?
N2 C125 C124 113.1(4) . . ?
N4 K2 N3 179.22(8) . . ?
O20 K2 N3 60.60(7) . . ?
O20 K2 N4 119.34(7) . . ?
O20 K2 O21 59.89(6) . . ?
O20 K2 O23 118.46(7) . . ?
O20 K2 O24 99.71(7) . . ?
O20 K2 O25 140.62(7) . . ?
O21 K2 N3 119.33(7) . . ?
O21 K2 N4 60.45(6) . . ?
O21 K2 O24 120.68(7) . . ?
O21 K2 O25 99.64(7) . . ?
O22 K2 N3 60.29(7) . . ?
O22 K2 N4 120.42(7) . . ?
O22 K2 O20 97.43(7) . . ?
O22 K2 O21 138.37(7) . . ?
O22 K2 O23 60.92(6) . . ?
O22 K2 O24 95.90(7) . . ?
O22 K2 O25 116.74(7) . . ?
O23 K2 N3 120.17(7) . . ?
O23 K2 N4 60.59(7) . . ?
O23 K2 O21 97.55(7) . . ?
O23 K2 O24 136.40(7) . . ?
O23 K2 O25 96.07(6) . . ?
O24 K2 N3 60.29(7) . . ?
O24 K2 N4 119.08(7) . . ?
O25 K2 N3 119.18(7) . . ?
O25 K2 N4 60.30(7) . . ?
O25 K2 O24 59.91(6) . . ?
C200 N3 K2 108.75(19) . . ?
C210 N3 K2 109.04(18) . . ?
C210 N3 C200 109.7(3) . . ?
C220 N3 K2 109.05(19) . . ?
C220 N3 C200 109.6(3) . . ?
C220 N3 C210 110.7(3) . . ?
C205 N4 K2 108.60(17) . . ?
C215 N4 K2 108.51(18) . . ?
C215 N4 C205 110.1(3) . . ?
C215 N4 C225 110.0(2) . . ?
C225 N4 K2 109.76(19) . . ?
C225 N4 C205 109.8(3) . . ?
C201 O20 K2 117.92(19) . . ?
C202 O20 K2 116.27(17) . . ?
C202 O20 C201 110.6(2) . . ?
C203 O21 K2 113.51(18) . . ?
C204 O21 K2 118.63(18) . . ?
C204 O21 C203 110.3(3) . . ?
C211 O22 K2 118.52(18) . . ?
C212 O22 K2 114.71(18) . . ?
C212 O22 C211 110.9(2) . . ?
C213 O23 K2 112.21(18) . . ?
C213 O23 C214 111.4(2) . . ?
C214 O23 K2 118.20(18) . . ?
C221 O24 K2 117.9(2) . . ?
C221 O24 C222 111.2(3) . . ?
C222 O24 K2 112.67(19) . . ?
C223 O25 K2 115.82(18) . . ?
C223 O25 C224 111.2(2) . . ?
C224 O25 K2 117.51(19) . . ?
N3 C200 C201 114.2(3) . . ?
O20 C201 C200 109.7(3) . . ?
O20 C202 C203 109.2(3) . . ?
O21 C203 C202 109.4(3) . . ?
O21 C204 C205 109.5(3) . . ?
N4 C205 C204 114.1(3) . . ?
N3 C210 C211 113.8(3) . . ?
O22 C211 C210 109.5(3) . . ?
O22 C212 C213 109.4(3) . . ?
O23 C213 C212 109.4(3) . . ?
O23 C214 C215 109.3(3) . . ?
N4 C215 C214 114.0(3) . . ?
N3 C220 C221 113.4(3) . . ?
O24 C221 C220 109.8(3) . . ?
O24 C222 C223 109.7(3) . . ?
O25 C223 C222 109.3(3) . . ?
O25 C224 C225 109.3(3) . . ?
N4 C225 C224 114.1(3) . . ?
C300 O300 C303 112.0(9) . . ?
C301 C300 O300 94.6(8) . . ?
C302 C301 C300 117.3(9) . . ?
C301 C302 C303 107.4(8) . . ?
C302 C303 O300 101.4(8) . . ?
C313 O310 C310 116.1(12) . . ?
C311 C310 O310 100.3(10) . . ?
C310 C311 C312 108.8(10) . . ?
C313 C312 C311 108.4(9) . . ?
O310 C313 C312 102.3(11) . . ?
C320 O320 C323 78.1(10) . . ?
C321 C320 O320 118.6(13) . . ?
C320 C321 C322 110.3(14) . . ?
C322 O330 C330 110.9(9) . . ?
C331 C330 O330 100.3(16) . . ?
C330 C331 C323 118.7(18) . . ?
C321 C322 C323 88.4(11) . . ?
O330 C322 C323 108.4(9) . . ?
C322 C323 O320 121.1(11) . . ?
C322 C323 C331 92.7(11) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_k30p-1
_database_code_depnum_ccdc_archive 'CCDC 1418083'
_audit_update_record             
;
2015-12-01 deposited with the CCDC.
2015-12-14 downloaded from the CCDC.
;
_audit_creation_date             2015-12-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C54 H111 Ge9 K O3 Si12'
_chemical_formula_sum            'C54 H111 Ge9 K O3 Si12'
_chemical_formula_weight         1837.91
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   12.1599(11)
_cell_length_b                   15.0580(14)
_cell_length_c                   27.802(3)
_cell_angle_alpha                97.312(2)
_cell_angle_beta                 94.153(2)
_cell_angle_gamma                108.939(2)
_cell_volume                     4740.7(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6416
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.458
_cell_measurement_theta_min      2.389
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.037
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1097 before and 0.0434 after correction.
The Ratio of minimum to maximum transmission is 0.7921.
The λ/2 correction factor is 0.0000.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1868
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.056
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0844
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            39721
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.406
_diffrn_reflns_theta_min         1.448
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12225
_reflns_number_total             19284
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v.2014.1-1 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         19284
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0469
_refine_ls_restrained_S_all      0.935
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0433P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1031
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C122-C121 = C123-C122 = C132-C131 = C133-C132 = C131-C130 = C121-C120
 1.54 with sigma of 0.02
3. Others
 Fixed Sof: C10A(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C10C(0.5) H10D(0.5)
 H10E(0.5) H10F(0.5) C10B(0.5) H10G(0.5) H10H(0.5) H10I(0.5) C30C(0.5)
 H30A(0.5) H30B(0.5) H30C(0.5) C30B(0.5) H30D(0.5) H30E(0.5) H30F(0.5)
 C30A(0.5) H30G(0.5) H30H(0.5) H30I(0.5) C30F(0.5) H30J(0.5) H30K(0.5)
 H30L(0.5) C30E(0.5) H30M(0.5) H30N(0.5) H30O(0.5) C30D(0.5) H30P(0.5)
 H30Q(0.5) H30R(0.5) O110(0.5) C110(0.5) H11J(0.5) H11K(0.5) C111(0.5)
 H11L(0.5) H11M(0.5) C112(0.5) H11N(0.5) H11O(0.5) C113(0.5) H11P(0.5)
 H11Q(0.5) C120(0.5) H12J(0.5) H12K(0.5) C121(0.5) H12L(0.5) H12M(0.5)
 C122(0.5) H12N(0.5) H12O(0.5) C123(0.5) H12P(0.5) H12Q(0.5) C130(0.5)
 H13A(0.5) H13B(0.5) C131(0.5) H13C(0.5) H13D(0.5) C132(0.5) H13E(0.5)
 H13F(0.5) C133(0.5) H13G(0.5) H13H(0.5) C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5)
 C0AA(0.5) H0AA(0.5) H0AB(0.5) H0AC(0.5) C1AA(0.5) H1AA(0.5) H1AB(0.5)
 H1AC(0.5) O121(0.5) C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5)
 C5(0.5) H5A(0.5) H5B(0.5) C7(0.5) H7A(0.5) H7B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C100(H10J,H10K), C101(H10L,H10M), C102(H10N,H10O), C103(H10P,H10Q), C110(H11J,
 H11K), C111(H11L,H11M), C112(H11N,H11O), C113(H11P,H11Q), C120(H12J,H12K),
 C121(H12L,H12M), C122(H12N,H12O), C123(H12P,H12Q), C130(H13A,H13B), C131(H13C,
 H13D), C132(H13E,H13F), C133(H13G,H13H), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B),
  C7(H7A,H7B)
4.b Me refined with riding coordinates:
 C10A(H10A,H10B,H10C), C10C(H10D,H10E,H10F), C10B(H10G,H10H,H10I), C1(H1A,H1B,
 H1C), C0AA(H0AA,H0AB,H0AC), C1AA(H1AA,H1AB,H1AC)
4.c Aromatic/amide H refined with riding coordinates:
 C22H(H22H), C22N(H22N), C22F(H22F), C22R(H22R), C22Q(H22Q), C22P(H22P),
 C22O(H22O), C22L(H22L), C22B(H22B), C22E(H22E), C22K(H22K), C22I(H22I),
 C22D(H22D), C22J(H22J), C22C(H22C)
4.d Idealised Me refined as rotating group:
 C11C(H11A,H11B,H11C), C11B(H11D,H11E,H11F), C11A(H11G,H11H,H11I), C12B(H12A,
 H12B,H12C), C12A(H12D,H12E,H12F), C12C(H12G,H12H,H12I), C20C(H20A,H20B,H20C),
 C20B(H20D,H20E,H20F), C20A(H20G,H20H,H20I), C21C(H21A,H21B,H21C), C21B(H21D,
 H21E,H21F), C21A(H21G,H21H,H21I), C30C(H30A,H30B,H30C), C30B(H30D,H30E,H30F),
 C30A(H30G,H30H,H30I), C30F(H30J,H30K,H30L), C30E(H30M,H30N,H30O), C30D(H30P,
 H30Q,H30R), C31C(H31A,H31B,H31C), C31B(H31D,H31E,H31F), C31A(H31G,H31H,H31I),
 C32C(H32A,H32B,H32C), C32B(H32D,H32E,H32F), C32A(H32G,H32H,H32I)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.29996(5) 1.18111(4) 0.84709(2) 0.03648(13) Uani 1 1 d . . . . .
Ge2 Ge 0.20777(4) 1.07519(3) 0.71843(2) 0.02747(11) Uani 1 1 d . . . . .
Ge3 Ge 0.34554(4) 1.32394(3) 0.74842(2) 0.03441(13) Uani 1 1 d . . . . .
Ge4 Ge 0.13516(4) 1.21544(3) 0.72315(2) 0.03396(13) Uani 1 1 d . . . . .
Ge5 Ge 0.21330(5) 1.29684(4) 0.81538(2) 0.03863(14) Uani 1 1 d . . . . .
Ge6 Ge 0.10694(4) 1.10718(4) 0.79231(2) 0.03472(13) Uani 1 1 d . . . . .
Ge7 Ge 0.36852(4) 1.08209(3) 0.78420(2) 0.03076(12) Uani 1 1 d . . . . .
Ge8 Ge 0.41047(4) 1.18884(3) 0.71349(2) 0.03026(12) Uani 1 1 d . . . . .
Ge9 Ge 0.47366(4) 1.27191(3) 0.80715(2) 0.03523(13) Uani 1 1 d . . . . .
Si1 Si 0.30830(13) 1.15668(10) 0.92980(4) 0.0373(3) Uani 1 1 d . . . . .
Si2 Si 0.10899(10) 0.93271(8) 0.66219(4) 0.0210(2) Uani 1 1 d . . . . .
Si3 Si 0.41439(12) 1.48218(9) 0.73199(4) 0.0326(3) Uani 1 1 d . . . . .
Si10 Si 0.24572(14) 0.99141(10) 0.92843(5) 0.0442(4) Uani 1 1 d . . . . .
Si11 Si 0.18296(16) 1.22368(12) 0.96860(5) 0.0580(4) Uani 1 1 d . . . . .
Si12 Si 0.50132(14) 1.23499(11) 0.96659(5) 0.0482(4) Uani 1 1 d . . . . .
Si20 Si 0.05353(11) 0.80469(9) 0.70691(4) 0.0313(3) Uani 1 1 d . . . . .
Si21 Si -0.06402(11) 0.94632(9) 0.62472(4) 0.0296(3) Uani 1 1 d . . . . .
Si22 Si 0.22567(10) 0.91058(8) 0.60094(4) 0.0211(2) Uani 1 1 d . . . . .
Si30 Si 0.47285(18) 1.58955(12) 0.80551(6) 0.0684(5) Uani 1 1 d . . . . .
Si31 Si 0.57187(13) 1.49479(10) 0.68615(6) 0.0467(4) Uani 1 1 d . . . . .
Si32 Si 0.25661(13) 1.49832(10) 0.68510(5) 0.0462(4) Uani 1 1 d . . . . .
C10A C 0.3332(11) 0.9305(9) 0.8900(4) 0.047(3) Uiso 0.5 1 d . . P A 1
H10A H 0.4166 0.9587 0.9025 0.070 Uiso 0.5 1 calc R . P A 1
H10B H 0.3063 0.8624 0.8921 0.070 Uiso 0.5 1 calc R . P A 1
H10C H 0.3216 0.9391 0.8559 0.070 Uiso 0.5 1 calc R . P A 1
C10C C 0.0884(12) 0.9381(10) 0.9050(5) 0.070(4) Uiso 0.5 1 d . . P A 1
H10D H 0.0754 0.9532 0.8722 0.106 Uiso 0.5 1 calc R . P A 1
H10E H 0.0637 0.8689 0.9034 0.106 Uiso 0.5 1 calc R . P A 1
H10F H 0.0426 0.9638 0.9269 0.106 Uiso 0.5 1 calc R . P A 1
C10B C 0.2717(10) 0.9626(8) 0.9917(3) 0.047(3) Uiso 0.5 1 d . . P A 1
H10G H 0.3552 0.9910 1.0040 0.070 Uiso 0.5 1 calc R . P A 1
H10H H 0.2262 0.9884 1.0137 0.070 Uiso 0.5 1 calc R . P A 1
H10I H 0.2473 0.8934 0.9902 0.070 Uiso 0.5 1 calc R . P A 1
C11C C 0.0313(6) 1.1672(6) 0.9372(3) 0.112(3) Uani 1 1 d . . . . .
H11A H 0.0317 1.1694 0.9021 0.167 Uiso 1 1 calc GR . . . .
H11B H -0.0186 1.2016 0.9505 0.167 Uiso 1 1 calc GR . . . .
H11C H 0.0009 1.1008 0.9423 0.167 Uiso 1 1 calc GR . . . .
C11B C 0.1845(8) 1.2044(6) 1.0335(2) 0.118(3) Uani 1 1 d . . . . .
H11D H 0.1545 1.1361 1.0347 0.176 Uiso 1 1 calc GR . . . .
H11E H 0.1349 1.2355 1.0500 0.176 Uiso 1 1 calc GR . . . .
H11F H 0.2649 1.2316 1.0499 0.176 Uiso 1 1 calc GR . . . .
C11A C 0.2279(7) 1.3529(5) 0.9669(3) 0.107(3) Uani 1 1 d . . . . .
H11G H 0.3040 1.3853 0.9866 0.161 Uiso 1 1 calc GR . . . .
H11H H 0.1693 1.3780 0.9800 0.161 Uiso 1 1 calc GR . . . .
H11I H 0.2342 1.3640 0.9330 0.161 Uiso 1 1 calc GR . . . .
C12B C 0.5113(6) 1.2178(5) 1.03194(19) 0.102(3) Uani 1 1 d . . . . .
H12A H 0.4554 1.2413 1.0485 0.152 Uiso 1 1 calc GR . . . .
H12B H 0.5909 1.2530 1.0480 0.152 Uiso 1 1 calc GR . . . .
H12C H 0.4929 1.1499 1.0336 0.152 Uiso 1 1 calc GR . . . .
C12A C 0.5473(6) 1.3648(4) 0.9641(3) 0.111(3) Uani 1 1 d . . . . .
H12D H 0.5488 1.3748 0.9299 0.167 Uiso 1 1 calc GR . . . .
H12E H 0.6257 1.3966 0.9820 0.167 Uiso 1 1 calc GR . . . .
H12F H 0.4918 1.3913 0.9790 0.167 Uiso 1 1 calc GR . . . .
C12C C 0.6034(5) 1.1875(5) 0.9341(2) 0.094(2) Uani 1 1 d . . . . .
H12G H 0.5876 1.1210 0.9382 0.141 Uiso 1 1 calc GR . . . .
H12H H 0.6843 1.2250 0.9477 0.141 Uiso 1 1 calc GR . . . .
H12I H 0.5923 1.1914 0.8993 0.141 Uiso 1 1 calc GR . . . .
C20C C -0.0638(4) 0.8206(4) 0.74346(17) 0.0468(13) Uani 1 1 d . . . . .
H20A H -0.0357 0.8840 0.7633 0.070 Uiso 1 1 calc GR . . . .
H20B H -0.0836 0.7722 0.7649 0.070 Uiso 1 1 calc GR . . . .
H20C H -0.1335 0.8140 0.7213 0.070 Uiso 1 1 calc GR . . . .
C20B C -0.0077(4) 0.6863(3) 0.66678(18) 0.0468(13) Uani 1 1 d . . . . .
H20D H -0.0685 0.6877 0.6420 0.070 Uiso 1 1 calc GR . . . .
H20E H -0.0419 0.6372 0.6866 0.070 Uiso 1 1 calc GR . . . .
H20F H 0.0550 0.6720 0.6507 0.070 Uiso 1 1 calc GR . . . .
C20A C 0.1772(4) 0.8031(4) 0.75058(17) 0.0488(14) Uani 1 1 d . . . . .
H20G H 0.2384 0.7916 0.7323 0.073 Uiso 1 1 calc GR . . . .
H20H H 0.1483 0.7524 0.7701 0.073 Uiso 1 1 calc GR . . . .
H20I H 0.2095 0.8645 0.7722 0.073 Uiso 1 1 calc GR . . . .
C21C C -0.1431(4) 0.9960(3) 0.67035(16) 0.0400(12) Uani 1 1 d . . . . .
H21A H -0.1572 0.9575 0.6966 0.060 Uiso 1 1 calc GR . . . .
H21B H -0.2182 0.9947 0.6543 0.060 Uiso 1 1 calc GR . . . .
H21C H -0.0954 1.0617 0.6841 0.060 Uiso 1 1 calc GR . . . .
C21B C -0.1646(4) 0.8257(3) 0.59571(16) 0.0411(12) Uani 1 1 d . . . . .
H21D H -0.1226 0.7948 0.5743 0.062 Uiso 1 1 calc GR . . . .
H21E H -0.2318 0.8318 0.5765 0.062 Uiso 1 1 calc GR . . . .
H21F H -0.1921 0.7873 0.6212 0.062 Uiso 1 1 calc GR . . . .
C21A C -0.0375(4) 1.0256(4) 0.57710(16) 0.0477(14) Uani 1 1 d . . . . .
H21G H 0.0097 1.0906 0.5924 0.072 Uiso 1 1 calc GR . . . .
H21H H -0.1126 1.0254 0.5617 0.072 Uiso 1 1 calc GR . . . .
H21I H 0.0044 1.0025 0.5523 0.072 Uiso 1 1 calc GR . . . .
C22G C 0.2795(4) 1.0151(3) 0.56771(14) 0.0243(9) Uani 1 1 d . . . . .
C22A C 0.1366(4) 0.8061(3) 0.55398(14) 0.0251(9) Uani 1 1 d . . . . .
C22M C 0.3571(3) 0.8828(3) 0.62635(14) 0.0236(9) Uani 1 1 d . . . . .
C22H C 0.2709(4) 1.1035(3) 0.58241(15) 0.0319(11) Uani 1 1 d . . . . .
H22H H 0.2341 1.1132 0.6107 0.038 Uiso 1 1 calc R . . . .
C22N C 0.3963(4) 0.9036(3) 0.67597(15) 0.0318(11) Uani 1 1 d . . . . .
H22N H 0.3563 0.9327 0.6976 0.038 Uiso 1 1 calc R . . . .
C22F C 0.0646(4) 0.8158(3) 0.51523(15) 0.0338(11) Uani 1 1 d . . . . .
H22F H 0.0658 0.8777 0.5109 0.041 Uiso 1 1 calc R . . . .
C22R C 0.4195(4) 0.8417(3) 0.59662(15) 0.0323(11) Uani 1 1 d . . . . .
H22R H 0.3951 0.8265 0.5625 0.039 Uiso 1 1 calc R . . . .
C22Q C 0.5165(4) 0.8220(3) 0.61486(17) 0.0404(12) Uani 1 1 d . . . . .
H22Q H 0.5577 0.7942 0.5933 0.048 Uiso 1 1 calc R . . . .
C22P C 0.5531(4) 0.8426(3) 0.66399(18) 0.0393(12) Uani 1 1 d . . . . .
H22P H 0.6196 0.8290 0.6766 0.047 Uiso 1 1 calc R . . . .
C22O C 0.4932(4) 0.8828(3) 0.69487(17) 0.0419(13) Uani 1 1 d . . . . .
H22O H 0.5174 0.8964 0.7290 0.050 Uiso 1 1 calc R . . . .
C22L C 0.3331(4) 1.0045(3) 0.52585(16) 0.0388(12) Uani 1 1 d . . . . .
H22L H 0.3386 0.9442 0.5142 0.047 Uiso 1 1 calc R . . . .
C22B C 0.1331(5) 0.7141(3) 0.55806(16) 0.0449(13) Uani 1 1 d . . . . .
H22B H 0.1819 0.7046 0.5838 0.054 Uiso 1 1 calc R . . . .
C22E C -0.0091(4) 0.7378(3) 0.48271(15) 0.0437(13) Uani 1 1 d . . . . .
H22E H -0.0576 0.7464 0.4566 0.052 Uiso 1 1 calc R . . . .
C22K C 0.3785(4) 1.0791(4) 0.50073(17) 0.0479(13) Uani 1 1 d . . . . .
H22K H 0.4159 1.0702 0.4725 0.057 Uiso 1 1 calc R . . . .
C22I C 0.3146(4) 1.1787(3) 0.55694(16) 0.0415(12) Uani 1 1 d . . . . .
H22I H 0.3065 1.2386 0.5674 0.050 Uiso 1 1 calc R . . . .
C22D C -0.0112(5) 0.6484(4) 0.48858(18) 0.0578(16) Uani 1 1 d . . . . .
H22D H -0.0626 0.5948 0.4668 0.069 Uiso 1 1 calc R . . . .
C22J C 0.3693(4) 1.1656(4) 0.51672(17) 0.0476(14) Uani 1 1 d . . . . .
H22J H 0.4013 1.2172 0.4997 0.057 Uiso 1 1 calc R . . . .
C22C C 0.0601(5) 0.6357(4) 0.52547(19) 0.0649(18) Uani 1 1 d . . . . .
H22C H 0.0597 0.5736 0.5288 0.078 Uiso 1 1 calc R . . . .
C30C C 0.3450(18) 1.6181(15) 0.8236(7) 0.161(8) Uiso 0.5 1 d . . P B 1
H30A H 0.3083 1.6375 0.7961 0.242 Uiso 0.5 1 calc GR . P B 1
H30B H 0.3696 1.6702 0.8514 0.242 Uiso 0.5 1 calc GR . P B 1
H30C H 0.2886 1.5619 0.8330 0.242 Uiso 0.5 1 calc GR . P B 1
C30B C 0.5196(13) 1.5399(10) 0.8557(5) 0.081(4) Uiso 0.5 1 d . . P B 1
H30D H 0.4528 1.4888 0.8635 0.122 Uiso 0.5 1 calc GR . P B 1
H30E H 0.5505 1.5897 0.8844 0.122 Uiso 0.5 1 calc GR . P B 1
H30F H 0.5809 1.5142 0.8465 0.122 Uiso 0.5 1 calc GR . P B 1
C30A C 0.6100(14) 1.6957(11) 0.7991(6) 0.110(5) Uiso 0.5 1 d . . P B 1
H30G H 0.6714 1.6718 0.7880 0.165 Uiso 0.5 1 calc GR . P B 1
H30H H 0.6387 1.7370 0.8308 0.165 Uiso 0.5 1 calc GR . P B 1
H30I H 0.5894 1.7321 0.7752 0.165 Uiso 0.5 1 calc GR . P B 1
C30F C 0.4500(13) 1.7014(10) 0.8015(5) 0.095(5) Uiso 0.5 1 d . . P B 2
H30J H 0.4762 1.7234 0.7712 0.143 Uiso 0.5 1 calc GR . P B 2
H30K H 0.4948 1.7487 0.8296 0.143 Uiso 0.5 1 calc GR . P B 2
H30L H 0.3665 1.6925 0.8015 0.143 Uiso 0.5 1 calc GR . P B 2
C30E C 0.4133(15) 1.5402(11) 0.8586(5) 0.114(5) Uiso 0.5 1 d . . P B 2
H30M H 0.3281 1.5253 0.8549 0.171 Uiso 0.5 1 calc GR . P B 2
H30N H 0.4484 1.5867 0.8882 0.171 Uiso 0.5 1 calc GR . P B 2
H30O H 0.4313 1.4820 0.8612 0.171 Uiso 0.5 1 calc GR . P B 2
C30D C 0.634(2) 1.6095(16) 0.8276(8) 0.185(9) Uiso 0.5 1 d . . P B 2
H30P H 0.6523 1.5522 0.8164 0.277 Uiso 0.5 1 calc GR . P B 2
H30Q H 0.6465 1.6232 0.8634 0.277 Uiso 0.5 1 calc GR . P B 2
H30R H 0.6847 1.6634 0.8143 0.277 Uiso 0.5 1 calc GR . P B 2
C31C C 0.6343(5) 1.6187(4) 0.6718(2) 0.0709(18) Uani 1 1 d . . . . .
H31A H 0.5748 1.6328 0.6514 0.106 Uiso 1 1 calc GR . . . .
H31B H 0.7025 1.6237 0.6542 0.106 Uiso 1 1 calc GR . . . .
H31C H 0.6582 1.6643 0.7023 0.106 Uiso 1 1 calc GR . . . .
C31B C 0.6903(5) 1.4655(5) 0.7206(3) 0.086(2) Uani 1 1 d . . . . .
H31D H 0.7193 1.5104 0.7512 0.129 Uiso 1 1 calc GR . . . .
H31E H 0.7548 1.4703 0.7007 0.129 Uiso 1 1 calc GR . . . .
H31F H 0.6589 1.4007 0.7278 0.129 Uiso 1 1 calc GR . . . .
C31A C 0.5236(6) 1.4110(4) 0.6277(2) 0.0756(19) Uani 1 1 d . . . . .
H31G H 0.4874 1.3462 0.6344 0.113 Uiso 1 1 calc GR . . . .
H31H H 0.5914 1.4142 0.6101 0.113 Uiso 1 1 calc GR . . . .
H31I H 0.4664 1.4285 0.6077 0.113 Uiso 1 1 calc GR . . . .
C32C C 0.3007(5) 1.6140(4) 0.6608(2) 0.0722(19) Uani 1 1 d . . . . .
H32A H 0.3392 1.6664 0.6877 0.108 Uiso 1 1 calc GR . . . .
H32B H 0.2309 1.6233 0.6455 0.108 Uiso 1 1 calc GR . . . .
H32C H 0.3549 1.6128 0.6365 0.108 Uiso 1 1 calc GR . . . .
C32B C 0.2022(6) 1.4019(5) 0.6318(2) 0.089(2) Uani 1 1 d . . . . .
H32D H 0.2556 1.4152 0.6068 0.134 Uiso 1 1 calc GR . . . .
H32E H 0.1239 1.3984 0.6182 0.134 Uiso 1 1 calc GR . . . .
H32F H 0.1982 1.3412 0.6420 0.134 Uiso 1 1 calc GR . . . .
C32A C 0.1343(5) 1.4919(5) 0.7219(2) 0.082(2) Uani 1 1 d . . . . .
H32G H 0.1136 1.4330 0.7360 0.124 Uiso 1 1 calc GR . . . .
H32H H 0.0662 1.4927 0.7010 0.124 Uiso 1 1 calc GR . . . .
H32I H 0.1581 1.5467 0.7483 0.124 Uiso 1 1 calc GR . . . .
K1 K 0.65693(12) 1.10818(11) 0.72935(5) 0.0748(4) Uani 1 1 d . . . . .
O100 O 0.6799(3) 1.0008(2) 0.79630(11) 0.0465(9) Uani 1 1 d . . . . .
C100 C 0.7669(5) 0.9581(5) 0.8009(2) 0.0664(17) Uani 1 1 d . . . . .
H10J H 0.8421 1.0005 0.7929 0.080 Uiso 1 1 calc R . . . .
H10K H 0.7437 0.8972 0.7781 0.080 Uiso 1 1 calc R . . . .
C101 C 0.7799(6) 0.9411(5) 0.8520(2) 0.090(2) Uani 1 1 d . . . . .
H10L H 0.7754 0.8745 0.8529 0.107 Uiso 1 1 calc R . . . .
H10M H 0.8560 0.9841 0.8696 0.107 Uiso 1 1 calc R . . . .
C102 C 0.6833(7) 0.9604(6) 0.8739(2) 0.090(3) Uani 1 1 d . . . . .
H10N H 0.7129 1.0175 0.8994 0.109 Uiso 1 1 calc R . . . .
H10O H 0.6382 0.9057 0.8889 0.109 Uiso 1 1 calc R . . . .
C103 C 0.6085(5) 0.9764(4) 0.83350(18) 0.0584(16) Uani 1 1 d . . . . .
H10P H 0.5407 0.9179 0.8214 0.070 Uiso 1 1 calc R . . . .
H10Q H 0.5789 1.0284 0.8449 0.070 Uiso 1 1 calc R . . . .
O110 O 0.7198(8) 1.1846(7) 0.6544(3) 0.061(3) Uiso 0.5 1 d . . P C 1
C110 C 0.637(2) 1.1706(16) 0.6034(8) 0.075(7) Uiso 0.5 1 d . . P C 1
H11J H 0.6140 1.1049 0.5854 0.090 Uiso 0.5 1 calc R . P C 1
H11K H 0.5650 1.1861 0.6091 0.090 Uiso 0.5 1 calc R . P C 1
C111 C 0.716(2) 1.2404(16) 0.5768(8) 0.093(8) Uiso 0.5 1 d . . P C 1
H11L H 0.7487 1.2073 0.5517 0.112 Uiso 0.5 1 calc R . P C 1
H11M H 0.6718 1.2756 0.5604 0.112 Uiso 0.5 1 calc R . P C 1
C112 C 0.8084(17) 1.3054(13) 0.6127(7) 0.063(5) Uiso 0.5 1 d . . P C 1
H11N H 0.8810 1.3309 0.5975 0.075 Uiso 0.5 1 calc R . P C 1
H11O H 0.7852 1.3593 0.6271 0.075 Uiso 0.5 1 calc R . P C 1
C113 C 0.8258(15) 1.2527(12) 0.6483(6) 0.091(6) Uiso 0.5 1 d . . P C 1
H11P H 0.8595 1.2958 0.6797 0.109 Uiso 0.5 1 calc R . P C 1
H11Q H 0.8820 1.2207 0.6387 0.109 Uiso 0.5 1 calc R . P C 1
O120 O 0.8083(4) 1.2444(4) 0.7906(2) 0.1064(17) Uani 1 1 d . . . . .
C120 C 0.8610(13) 1.2320(9) 0.8394(5) 0.071(4) Uiso 0.5 1 d D . P C 1
H12J H 0.8002 1.1884 0.8553 0.085 Uiso 0.5 1 calc R . P C 1
H12K H 0.9238 1.2044 0.8345 0.085 Uiso 0.5 1 calc R . P C 1
C121 C 0.9105(12) 1.3283(8) 0.8710(4) 0.073(4) Uiso 0.5 1 d D . P C 1
H12L H 0.8495 1.3475 0.8868 0.087 Uiso 0.5 1 calc R . P C 1
H12M H 0.9747 1.3320 0.8961 0.087 Uiso 0.5 1 calc R . P C 1
C122 C 0.9531(17) 1.3831(16) 0.8322(7) 0.158(10) Uiso 0.5 1 d D . P C 1
H12N H 1.0094 1.3612 0.8142 0.189 Uiso 0.5 1 calc R . P C 1
H12O H 0.9855 1.4526 0.8436 0.189 Uiso 0.5 1 calc R . P C 1
C123 C 0.8302(18) 1.350(2) 0.8040(9) 0.168(10) Uiso 0.5 1 d D . P C 1
H12P H 0.7724 1.3630 0.8248 0.202 Uiso 0.5 1 calc R . P C 1
H12Q H 0.8291 1.3811 0.7746 0.202 Uiso 0.5 1 calc R . P C 1
C130 C 0.811(2) 1.2551(16) 0.8380(10) 0.177(11) Uiso 0.5 1 d D . P C 2
H13A H 0.8714 1.2309 0.8512 0.212 Uiso 0.5 1 calc R . P C 2
H13B H 0.7345 1.2142 0.8457 0.212 Uiso 0.5 1 calc R . P C 2
C131 C 0.8357(19) 1.3579(14) 0.8658(7) 0.148(7) Uiso 0.5 1 d D . P C 2
H13C H 0.7649 1.3757 0.8696 0.177 Uiso 0.5 1 calc R . P C 2
H13D H 0.8877 1.3737 0.8970 0.177 Uiso 0.5 1 calc R . P C 2
C132 C 0.899(3) 1.391(2) 0.8214(8) 0.212(13) Uiso 0.5 1 d D . P C 2
H13E H 0.8782 1.4465 0.8140 0.254 Uiso 0.5 1 calc R . P C 2
H13F H 0.9841 1.4149 0.8327 0.254 Uiso 0.5 1 calc R . P C 2
C133 C 0.8822(12) 1.3268(9) 0.7743(4) 0.073(4) Uiso 0.5 1 d D . P C 2
H13G H 0.8421 1.3462 0.7473 0.088 Uiso 0.5 1 calc R . P C 2
H13H H 0.9562 1.3197 0.7649 0.088 Uiso 0.5 1 calc R . P C 2
C1 C 0.2077(12) 0.9605(9) 0.9907(4) 0.071(4) Uiso 0.5 1 d . . P A 2
H1A H 0.1468 0.9862 1.0007 0.106 Uiso 0.5 1 calc R . P A 2
H1B H 0.1789 0.8913 0.9889 0.106 Uiso 0.5 1 calc R . P A 2
H1C H 0.2777 0.9883 1.0147 0.106 Uiso 0.5 1 calc R . P A 2
C0AA C 0.3600(13) 0.9460(11) 0.9065(5) 0.066(4) Uiso 0.5 1 d . . P A 2
H0AA H 0.4327 0.9758 0.9289 0.100 Uiso 0.5 1 calc R . P A 2
H0AB H 0.3342 0.8769 0.9052 0.100 Uiso 0.5 1 calc R . P A 2
H0AC H 0.3738 0.9613 0.8738 0.100 Uiso 0.5 1 calc R . P A 2
C1AA C 0.1070(10) 0.9325(8) 0.8845(4) 0.049(3) Uiso 0.5 1 d . . P A 2
H1AA H 0.0451 0.9558 0.8955 0.074 Uiso 0.5 1 calc R . P A 2
H1AB H 0.1219 0.9479 0.8518 0.074 Uiso 0.5 1 calc R . P A 2
H1AC H 0.0822 0.8634 0.8833 0.074 Uiso 0.5 1 calc R . P A 2
O121 O 0.7078(8) 1.1524(6) 0.6394(3) 0.052(2) Uiso 0.5 1 d . . P C 2
C3 C 0.782(2) 1.2907(19) 0.6037(9) 0.104(9) Uiso 0.5 1 d . . P C 2
H3A H 0.7690 1.3419 0.6263 0.125 Uiso 0.5 1 calc R . P C 2
H3B H 0.8420 1.3193 0.5829 0.125 Uiso 0.5 1 calc R . P C 2
C4 C 0.6773(16) 1.2318(12) 0.5757(7) 0.066(5) Uiso 0.5 1 d . . P C 2
H4A H 0.6919 1.2089 0.5426 0.080 Uiso 0.5 1 calc R . P C 2
H4B H 0.6204 1.2658 0.5727 0.080 Uiso 0.5 1 calc R . P C 2
C5 C 0.8168(12) 1.2184(10) 0.6324(5) 0.064(4) Uiso 0.5 1 d . . P C 2
H5A H 0.8625 1.1863 0.6132 0.077 Uiso 0.5 1 calc R . P C 2
H5B H 0.8637 1.2511 0.6642 0.077 Uiso 0.5 1 calc R . P C 2
C7 C 0.631(2) 1.1460(17) 0.6051(9) 0.100(10) Uiso 0.5 1 d . . P C 2
H7A H 0.5580 1.1478 0.6185 0.120 Uiso 0.5 1 calc R . P C 2
H7B H 0.6121 1.0848 0.5829 0.120 Uiso 0.5 1 calc R . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 Ge5 2.5244(7) . ?
Ge1 Ge6 2.5342(7) . ?
Ge1 Ge7 2.5159(7) . ?
Ge1 Ge9 2.5327(8) . ?
Ge1 Si1 2.3749(12) . ?
Ge2 Ge4 2.5323(6) . ?
Ge2 Ge6 2.5397(7) . ?
Ge2 Ge7 2.5450(6) . ?
Ge2 Ge8 2.5286(7) . ?
Ge2 Si2 2.3858(12) . ?
Ge3 Ge4 2.5380(7) . ?
Ge3 Ge5 2.5334(7) . ?
Ge3 Ge8 2.5210(7) . ?
Ge3 Ge9 2.5408(6) . ?
Ge3 Si3 2.3717(13) . ?
Ge4 Ge5 2.6591(7) . ?
Ge4 Ge6 2.6461(7) . ?
Ge5 Ge6 2.6937(8) . ?
Ge7 Ge8 2.6692(7) . ?
Ge7 Ge9 2.6939(7) . ?
Ge7 K1 3.8486(15) . ?
Ge8 Ge9 2.6819(7) . ?
Ge8 K1 3.5998(14) . ?
Si1 Si10 2.349(2) . ?
Si1 Si11 2.337(2) . ?
Si1 Si12 2.344(2) . ?
Si2 Si20 2.3674(16) . ?
Si2 Si21 2.3601(15) . ?
Si2 Si22 2.3530(15) . ?
Si3 Si30 2.3451(19) . ?
Si3 Si31 2.347(2) . ?
Si3 Si32 2.3368(18) . ?
Si10 C10A 1.914(12) . ?
Si10 C10C 1.849(14) . ?
Si10 C10B 1.894(10) . ?
Si10 C1 1.900(12) . ?
Si10 C0AA 1.844(14) . ?
Si10 C1AA 1.892(12) . ?
Si11 C11C 1.856(7) . ?
Si11 C11B 1.862(6) . ?
Si11 C11A 1.851(7) . ?
Si12 C12B 1.868(5) . ?
Si12 C12A 1.863(6) . ?
Si12 C12C 1.855(6) . ?
Si20 C20C 1.869(5) . ?
Si20 C20B 1.868(5) . ?
Si20 C20A 1.871(5) . ?
Si21 C21C 1.870(4) . ?
Si21 C21B 1.867(5) . ?
Si21 C21A 1.870(4) . ?
Si22 C22G 1.884(4) . ?
Si22 C22A 1.876(4) . ?
Si22 C22M 1.891(4) . ?
Si30 C30C 1.830(19) . ?
Si30 C30B 1.804(12) . ?
Si30 C30A 1.938(16) . ?
Si30 C30F 1.809(13) . ?
Si30 C30E 1.828(16) . ?
Si30 C30D 1.92(2) . ?
Si31 C31C 1.879(5) . ?
Si31 C31B 1.872(5) . ?
Si31 C31A 1.854(6) . ?
Si32 C32C 1.878(5) . ?
Si32 C32B 1.852(6) . ?
Si32 C32A 1.850(6) . ?
C22G C22H 1.382(6) . ?
C22G C22L 1.391(6) . ?
C22A C22F 1.391(5) . ?
C22A C22B 1.392(6) . ?
C22M C22N 1.388(5) . ?
C22M C22R 1.381(5) . ?
C22H C22I 1.391(6) . ?
C22N C22O 1.398(6) . ?
C22F C22E 1.389(6) . ?
C22R C22Q 1.383(6) . ?
C22Q C22P 1.369(6) . ?
C22P C22O 1.371(6) . ?
C22O K1 3.303(5) . ?
C22L C22K 1.381(6) . ?
C22B C22C 1.391(6) . ?
C22E C22D 1.368(6) . ?
C22K C22J 1.364(7) . ?
C22I C22J 1.367(7) . ?
C22D C22C 1.367(6) . ?
K1 O100 2.673(3) . ?
K1 O110 2.553(9) . ?
K1 O120 2.589(6) . ?
K1 C133 3.536(14) . ?
K1 O121 2.732(9) . ?
O100 C100 1.411(6) . ?
O100 C103 1.406(5) . ?
C100 C101 1.481(7) . ?
C101 C102 1.454(8) . ?
C102 C103 1.486(7) . ?
O110 C110 1.63(2) . ?
O110 C113 1.400(19) . ?
C110 C111 1.49(3) . ?
C111 C112 1.45(3) . ?
C112 C113 1.39(2) . ?
O120 C120 1.518(14) . ?
O120 C123 1.52(3) . ?
O120 C130 1.30(2) . ?
O120 C133 1.426(14) . ?
C120 C121 1.507(13) . ?
C121 C122 1.465(15) . ?
C122 C123 1.532(18) . ?
C130 C131 1.563(17) . ?
C131 C132 1.552(17) . ?
C132 C133 1.484(17) . ?
O121 C5 1.419(16) . ?
O121 C7 1.26(3) . ?
C3 C4 1.40(3) . ?
C3 C5 1.57(3) . ?
C4 C7 1.59(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Ge5 Ge1 Ge6 64.35(2) . . ?
Ge5 Ge1 Ge9 82.28(2) . . ?
Ge7 Ge1 Ge5 115.93(2) . . ?
Ge7 Ge1 Ge6 82.89(2) . . ?
Ge7 Ge1 Ge9 64.50(2) . . ?
Ge9 Ge1 Ge6 116.18(2) . . ?
Si1 Ge1 Ge5 123.72(4) . . ?
Si1 Ge1 Ge6 119.00(4) . . ?
Si1 Ge1 Ge7 120.26(4) . . ?
Si1 Ge1 Ge9 124.77(4) . . ?
Ge4 Ge2 Ge6 62.893(19) . . ?
Ge4 Ge2 Ge7 117.45(2) . . ?
Ge6 Ge2 Ge7 82.21(2) . . ?
Ge8 Ge2 Ge4 88.24(2) . . ?
Ge8 Ge2 Ge6 117.87(2) . . ?
Ge8 Ge2 Ge7 63.485(19) . . ?
Si2 Ge2 Ge4 120.87(3) . . ?
Si2 Ge2 Ge6 116.91(4) . . ?
Si2 Ge2 Ge7 121.01(3) . . ?
Si2 Ge2 Ge8 125.04(3) . . ?
Ge4 Ge3 Ge9 117.98(2) . . ?
Ge5 Ge3 Ge4 63.25(2) . . ?
Ge5 Ge3 Ge9 81.95(2) . . ?
Ge8 Ge3 Ge4 88.28(2) . . ?
Ge8 Ge3 Ge5 117.94(2) . . ?
Ge8 Ge3 Ge9 63.987(19) . . ?
Si3 Ge3 Ge4 122.29(4) . . ?
Si3 Ge3 Ge5 115.31(4) . . ?
Si3 Ge3 Ge8 126.29(4) . . ?
Si3 Ge3 Ge9 118.64(4) . . ?
Ge2 Ge4 Ge3 88.24(2) . . ?
Ge2 Ge4 Ge5 100.54(2) . . ?
Ge2 Ge4 Ge6 58.689(18) . . ?
Ge3 Ge4 Ge5 58.292(19) . . ?
Ge3 Ge4 Ge6 100.71(2) . . ?
Ge6 Ge4 Ge5 61.028(19) . . ?
Ge1 Ge5 Ge3 92.75(2) . . ?
Ge1 Ge5 Ge4 102.20(2) . . ?
Ge1 Ge5 Ge6 58.00(2) . . ?
Ge3 Ge5 Ge4 58.46(2) . . ?
Ge3 Ge5 Ge6 99.55(2) . . ?
Ge4 Ge5 Ge6 59.247(18) . . ?
Ge1 Ge6 Ge2 92.35(2) . . ?
Ge1 Ge6 Ge4 102.30(2) . . ?
Ge1 Ge6 Ge5 57.649(19) . . ?
Ge2 Ge6 Ge4 58.418(18) . . ?
Ge2 Ge6 Ge5 99.43(2) . . ?
Ge4 Ge6 Ge5 59.726(19) . . ?
Ge1 Ge7 Ge2 92.66(2) . . ?
Ge1 Ge7 Ge8 102.43(2) . . ?
Ge1 Ge7 Ge9 58.05(2) . . ?
Ge1 Ge7 K1 135.70(3) . . ?
Ge2 Ge7 Ge8 57.959(18) . . ?
Ge2 Ge7 Ge9 99.85(2) . . ?
Ge2 Ge7 K1 110.44(3) . . ?
Ge8 Ge7 Ge9 60.006(18) . . ?
Ge8 Ge7 K1 64.09(2) . . ?
Ge9 Ge7 K1 80.46(3) . . ?
Ge2 Ge8 Ge7 58.556(18) . . ?
Ge2 Ge8 Ge9 100.60(2) . . ?
Ge2 Ge8 K1 118.83(3) . . ?
Ge3 Ge8 Ge2 88.70(2) . . ?
Ge3 Ge8 Ge7 100.23(2) . . ?
Ge3 Ge8 Ge9 58.366(17) . . ?
Ge3 Ge8 K1 138.99(3) . . ?
Ge7 Ge8 Ge9 60.453(18) . . ?
Ge7 Ge8 K1 74.08(3) . . ?
Ge9 Ge8 K1 85.49(3) . . ?
Ge1 Ge9 Ge3 92.38(2) . . ?
Ge1 Ge9 Ge7 57.450(19) . . ?
Ge1 Ge9 Ge8 101.63(2) . . ?
Ge3 Ge9 Ge7 99.07(2) . . ?
Ge3 Ge9 Ge8 57.647(18) . . ?
Ge8 Ge9 Ge7 59.540(17) . . ?
Si10 Si1 Ge1 106.62(6) . . ?
Si11 Si1 Ge1 108.27(6) . . ?
Si11 Si1 Si10 111.05(8) . . ?
Si11 Si1 Si12 109.55(8) . . ?
Si12 Si1 Ge1 107.81(7) . . ?
Si12 Si1 Si10 113.33(7) . . ?
Si20 Si2 Ge2 108.24(5) . . ?
Si21 Si2 Ge2 108.20(5) . . ?
Si21 Si2 Si20 107.63(6) . . ?
Si22 Si2 Ge2 111.01(6) . . ?
Si22 Si2 Si20 113.19(6) . . ?
Si22 Si2 Si21 108.40(6) . . ?
Si30 Si3 Ge3 109.96(7) . . ?
Si30 Si3 Si31 111.21(8) . . ?
Si31 Si3 Ge3 107.18(6) . . ?
Si32 Si3 Ge3 104.75(6) . . ?
Si32 Si3 Si30 112.86(8) . . ?
Si32 Si3 Si31 110.54(7) . . ?
C10A Si10 Si1 112.9(4) . . ?
C10C Si10 Si1 110.0(4) . . ?
C10C Si10 C10A 109.4(6) . . ?
C10C Si10 C10B 109.8(6) . . ?
C10B Si10 Si1 110.7(3) . . ?
C10B Si10 C10A 103.8(5) . . ?
C1 Si10 Si1 110.9(4) . . ?
C0AA Si10 Si1 108.8(5) . . ?
C0AA Si10 C1 112.7(6) . . ?
C0AA Si10 C1AA 108.2(6) . . ?
C1AA Si10 Si1 109.6(4) . . ?
C1AA Si10 C1 106.5(6) . . ?
C11C Si11 Si1 109.8(2) . . ?
C11C Si11 C11B 109.0(4) . . ?
C11B Si11 Si1 109.9(2) . . ?
C11A Si11 Si1 111.0(2) . . ?
C11A Si11 C11C 108.1(4) . . ?
C11A Si11 C11B 109.0(4) . . ?
C12B Si12 Si1 109.1(2) . . ?
C12A Si12 Si1 111.1(2) . . ?
C12A Si12 C12B 108.8(3) . . ?
C12C Si12 Si1 110.3(2) . . ?
C12C Si12 C12B 110.1(3) . . ?
C12C Si12 C12A 107.5(4) . . ?
C20C Si20 Si2 107.24(15) . . ?
C20C Si20 C20A 107.7(2) . . ?
C20B Si20 Si2 112.83(16) . . ?
C20B Si20 C20C 107.7(2) . . ?
C20B Si20 C20A 108.5(2) . . ?
C20A Si20 Si2 112.61(17) . . ?
C21C Si21 Si2 111.48(15) . . ?
C21C Si21 C21A 106.5(2) . . ?
C21B Si21 Si2 109.16(15) . . ?
C21B Si21 C21C 107.5(2) . . ?
C21B Si21 C21A 108.6(2) . . ?
C21A Si21 Si2 113.42(16) . . ?
C22G Si22 Si2 113.99(13) . . ?
C22G Si22 C22M 108.16(18) . . ?
C22A Si22 Si2 108.79(14) . . ?
C22A Si22 C22G 106.88(17) . . ?
C22A Si22 C22M 107.18(18) . . ?
C22M Si22 Si2 111.54(13) . . ?
C30C Si30 Si3 108.0(6) . . ?
C30C Si30 C30A 116.7(8) . . ?
C30B Si30 Si3 113.3(4) . . ?
C30B Si30 C30C 104.9(8) . . ?
C30B Si30 C30A 104.0(7) . . ?
C30A Si30 Si3 109.9(5) . . ?
C30F Si30 Si3 113.4(5) . . ?
C30F Si30 C30E 111.1(7) . . ?
C30F Si30 C30D 111.0(9) . . ?
C30E Si30 Si3 114.4(5) . . ?
C30E Si30 C30D 96.0(8) . . ?
C30D Si30 Si3 109.6(6) . . ?
C31C Si31 Si3 110.5(2) . . ?
C31B Si31 Si3 110.6(2) . . ?
C31B Si31 C31C 108.8(3) . . ?
C31A Si31 Si3 110.6(2) . . ?
C31A Si31 C31C 108.2(3) . . ?
C31A Si31 C31B 107.9(3) . . ?
C32C Si32 Si3 111.19(19) . . ?
C32B Si32 Si3 110.8(2) . . ?
C32B Si32 C32C 107.2(3) . . ?
C32A Si32 Si3 110.4(2) . . ?
C32A Si32 C32C 109.2(3) . . ?
C32A Si32 C32B 107.9(3) . . ?
C22H C22G Si22 124.3(3) . . ?
C22H C22G C22L 116.8(4) . . ?
C22L C22G Si22 118.9(3) . . ?
C22F C22A Si22 121.7(3) . . ?
C22F C22A C22B 116.6(4) . . ?
C22B C22A Si22 121.6(3) . . ?
C22N C22M Si22 121.4(3) . . ?
C22R C22M Si22 121.9(3) . . ?
C22R C22M C22N 116.7(4) . . ?
C22G C22H C22I 121.8(4) . . ?
C22M C22N C22O 121.5(4) . . ?
C22E C22F C22A 122.0(4) . . ?
C22M C22R C22Q 122.3(4) . . ?
C22P C22Q C22R 120.1(4) . . ?
C22Q C22P C22O 119.6(4) . . ?
C22N C22O K1 94.3(3) . . ?
C22P C22O C22N 119.9(4) . . ?
C22P C22O K1 106.9(3) . . ?
C22K C22L C22G 121.9(4) . . ?
C22C C22B C22A 121.7(4) . . ?
C22D C22E C22F 119.4(4) . . ?
C22J C22K C22L 119.5(5) . . ?
C22J C22I C22H 119.3(4) . . ?
C22C C22D C22E 120.6(5) . . ?
C22K C22J C22I 120.7(4) . . ?
C22D C22C C22B 119.7(5) . . ?
Ge8 K1 Ge7 41.833(18) . . ?
C22O K1 Ge7 74.84(9) . . ?
C22O K1 Ge8 92.71(9) . . ?
C22O K1 C133 166.7(2) . . ?
O100 K1 Ge7 81.40(8) . . ?
O100 K1 Ge8 123.21(8) . . ?
O100 K1 C22O 68.00(11) . . ?
O100 K1 C133 102.3(2) . . ?
O100 K1 O121 145.28(19) . . ?
O110 K1 Ge7 126.5(2) . . ?
O110 K1 Ge8 85.0(2) . . ?
O110 K1 C22O 109.8(2) . . ?
O110 K1 O100 151.4(2) . . ?
O110 K1 O120 94.3(3) . . ?
O120 K1 Ge7 102.62(14) . . ?
O120 K1 Ge8 103.81(12) . . ?
O120 K1 C22O 151.94(15) . . ?
O120 K1 O100 83.95(14) . . ?
O120 K1 C133 20.3(2) . . ?
O120 K1 O121 104.8(2) . . ?
C133 K1 Ge7 113.6(2) . . ?
C133 K1 Ge8 100.3(2) . . ?
O121 K1 Ge7 127.26(18) . . ?
O121 K1 Ge8 87.89(18) . . ?
O121 K1 C22O 98.3(2) . . ?
O121 K1 C133 84.7(3) . . ?
C100 O100 K1 126.0(3) . . ?
C103 O100 K1 126.8(3) . . ?
C103 O100 C100 107.2(4) . . ?
O100 C100 C101 107.9(5) . . ?
C102 C101 C100 105.4(5) . . ?
C101 C102 C103 106.1(4) . . ?
O100 C103 C102 106.3(4) . . ?
C110 O110 K1 126.0(10) . . ?
C113 O110 K1 129.7(9) . . ?
C113 O110 C110 104.1(12) . . ?
C111 C110 O110 101.4(16) . . ?
C112 C111 C110 107.1(18) . . ?
C113 C112 C111 106.0(16) . . ?
C112 C113 O110 110.5(14) . . ?
C120 O120 K1 124.4(5) . . ?
C120 O120 C123 96.3(10) . . ?
C123 O120 K1 134.0(8) . . ?
C130 O120 K1 125.4(12) . . ?
C130 O120 C133 112.6(13) . . ?
C133 O120 K1 120.7(6) . . ?
C121 C120 O120 108.1(9) . . ?
C122 C121 C120 97.2(13) . . ?
C121 C122 C123 92.0(15) . . ?
O120 C123 C122 100.3(17) . . ?
O120 C130 C131 117.5(19) . . ?
C132 C131 C130 85.1(17) . . ?
C133 C132 C131 123(2) . . ?
O120 C133 K1 39.0(5) . . ?
O120 C133 C132 95.3(14) . . ?
C132 C133 K1 129.2(15) . . ?
C5 O121 K1 122.1(8) . . ?
C7 O121 K1 123.2(14) . . ?
C7 O121 C5 110.1(15) . . ?
C4 C3 C5 101.7(18) . . ?
C3 C4 C7 104.1(17) . . ?
O121 C5 C3 103.9(13) . . ?
O121 C7 C4 109.4(19) . . ?

# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.000 399 94 ' '
2 0.500 0.500 0.500 289 67 ' '
_platon_squeeze_details          ?


_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_mo_kysliak_20_0m
_database_code_depnum_ccdc_archive 'CCDC 1418084'
_audit_update_record             
;
2015-12-01 deposited with the CCDC.
2015-12-14 downloaded from the CCDC.
;
_audit_creation_date             2015-12-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C39 H105 Ge9 K O3 Si12, C5 H7'
_chemical_formula_sum            'C44 H117 Ge9 K O3 Si12'
_chemical_formula_weight         1723.86
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   26.448(4)
_cell_length_b                   11.2469(18)
_cell_length_c                   30.221(4)
_cell_angle_alpha                90
_cell_angle_beta                 112.221(4)
_cell_angle_gamma                90
_cell_volume                     8322(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4943
_cell_measurement_temperature    150
_cell_measurement_theta_max      22.355
_cell_measurement_theta_min      2.322
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.454
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.5166
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0771 before and 0.0422 after correction.
The Ratio of minimum to maximum transmission is 0.6935.
The λ/2 correction factor is 0.0000.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3520
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.1044
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            30163
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        23.210
_diffrn_reflns_theta_max         23.210
_diffrn_reflns_theta_min         1.377
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7249
_reflns_number_total             11828
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         11828
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0562
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0606P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1339
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C201-C202
 1.54 with sigma of 0.02
 C202-C203
 1.54 with sigma of 0.02
 C203-C204
 1.54 with sigma of 0.02
 C204-C205
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C111 \\sim C112 \\sim C110 \\sim C109: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4.a Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C102(H10C,H10D), C103(H10E,H10F), C104(H10G,H10H), C105(H10I,
 H10J), C106(H10K,H10L), C107(H10M,H10N), C108(H10O,H10P), C109(H10Q,H10R),
 C110(H11D,H11E), C111(H11F,H11G), C112(H11H,H11I), C202(H20A,H20B), C204(H20C,
 H20D)
4.b Me refined with riding coordinates:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C),
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C),
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C205(H20E,H20F,H20G)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.35822(3) 0.21497(8) 0.06645(3) 0.0320(2) Uani 1 1 d . . . . .
Ge2 Ge 0.21430(4) 0.23495(8) 0.03198(3) 0.0352(3) Uani 1 1 d . . . . .
Ge3 Ge 0.26597(4) 0.19687(8) -0.06111(3) 0.0338(3) Uani 1 1 d . . . . .
Ge4 Ge 0.33479(4) 0.34234(8) -0.00758(3) 0.0332(3) Uani 1 1 d . . . . .
Ge5 Ge 0.29210(4) 0.38413(9) 0.05890(3) 0.0351(3) Uani 1 1 d . . . . .
Ge6 Ge 0.22671(4) 0.36972(9) -0.03069(3) 0.0382(3) Uani 1 1 d . . . . .
Ge7 Ge 0.32840(4) 0.05700(9) 0.00162(3) 0.0339(3) Uani 1 1 d . . . . .
Ge8 Ge 0.28497(3) 0.07446(8) 0.06914(3) 0.0328(3) Uani 1 1 d . . . . .
Ge9 Ge 0.21852(4) 0.06526(9) -0.02159(3) 0.0338(3) Uani 1 1 d . . . . .
Si1 Si 0.44581(9) 0.2133(2) 0.12868(8) 0.0267(6) Uani 1 1 d . . . . .
Si2 Si 0.13534(9) 0.2576(2) 0.05028(8) 0.0276(6) Uani 1 1 d . . . . .
Si3 Si 0.25032(10) 0.1863(2) -0.14355(8) 0.0335(6) Uani 1 1 d . . . . .
Si11 Si 0.48978(10) 0.0368(2) 0.12346(9) 0.0384(7) Uani 1 1 d . . . . .
Si12 Si 0.49673(10) 0.3794(2) 0.12276(9) 0.0397(7) Uani 1 1 d . . . . .
Si13 Si 0.43068(10) 0.2225(2) 0.20019(8) 0.0347(6) Uani 1 1 d . . . . .
Si21 Si 0.13351(10) 0.0976(2) 0.09930(9) 0.0378(7) Uani 1 1 d . . . . .
Si22 Si 0.05833(10) 0.2609(2) -0.02101(9) 0.0397(7) Uani 1 1 d . . . . .
Si23 Si 0.14578(10) 0.4374(2) 0.09212(9) 0.0379(7) Uani 1 1 d . . . . .
Si31 Si 0.31115(12) 0.3153(3) -0.15878(10) 0.0583(9) Uani 1 1 d . . . . .
Si32 Si 0.15910(10) 0.2428(3) -0.18395(9) 0.0468(8) Uani 1 1 d . . . . .
Si33 Si 0.26397(13) -0.0121(3) -0.16041(9) 0.0545(8) Uani 1 1 d . . . . .
C11 C 0.4450(4) -0.0938(8) 0.1196(3) 0.062(3) Uani 1 1 d . . . . .
H11A H 0.4352 -0.0956 0.1478 0.092 Uiso 1 1 calc R . . . .
H11B H 0.4118 -0.0876 0.0907 0.092 Uiso 1 1 calc R . . . .
H11C H 0.4645 -0.1670 0.1184 0.092 Uiso 1 1 calc R . . . .
C12 C 0.5536(3) 0.0159(8) 0.1790(3) 0.048(3) Uani 1 1 d . . . . .
H12A H 0.5784 0.0830 0.1824 0.071 Uiso 1 1 calc R . . . .
H12B H 0.5437 0.0119 0.2071 0.071 Uiso 1 1 calc R . . . .
H12C H 0.5718 -0.0581 0.1764 0.071 Uiso 1 1 calc R . . . .
C13 C 0.5084(4) 0.0397(9) 0.0695(3) 0.060(3) Uani 1 1 d . . . . .
H13A H 0.5320 0.1083 0.0714 0.090 Uiso 1 1 calc R . . . .
H13B H 0.5279 -0.0337 0.0682 0.090 Uiso 1 1 calc R . . . .
H13C H 0.4751 0.0458 0.0406 0.090 Uiso 1 1 calc R . . . .
C14 C 0.4940(3) 0.3988(8) 0.0612(3) 0.054(3) Uani 1 1 d . . . . .
H14A H 0.5080 0.3271 0.0513 0.081 Uiso 1 1 calc R . . . .
H14B H 0.4561 0.4125 0.0395 0.081 Uiso 1 1 calc R . . . .
H14C H 0.5164 0.4672 0.0601 0.081 Uiso 1 1 calc R . . . .
C15 C 0.4700(4) 0.5165(8) 0.1417(3) 0.064(3) Uani 1 1 d . . . . .
H15A H 0.4715 0.5061 0.1744 0.096 Uiso 1 1 calc R . . . .
H15B H 0.4925 0.5850 0.1406 0.096 Uiso 1 1 calc R . . . .
H15C H 0.4321 0.5302 0.1200 0.096 Uiso 1 1 calc R . . . .
C16 C 0.5703(3) 0.3572(9) 0.1630(3) 0.066(3) Uani 1 1 d . . . . .
H16A H 0.5730 0.3466 0.1960 0.099 Uiso 1 1 calc R . . . .
H16B H 0.5846 0.2864 0.1528 0.099 Uiso 1 1 calc R . . . .
H16C H 0.5916 0.4270 0.1612 0.099 Uiso 1 1 calc R . . . .
C17 C 0.4037(4) 0.0778(8) 0.2122(3) 0.055(3) Uani 1 1 d . . . . .
H17A H 0.3694 0.0588 0.1856 0.082 Uiso 1 1 calc R . . . .
H17B H 0.4305 0.0149 0.2154 0.082 Uiso 1 1 calc R . . . .
H17C H 0.3969 0.0837 0.2418 0.082 Uiso 1 1 calc R . . . .
C18 C 0.3795(4) 0.3413(9) 0.1959(3) 0.061(3) Uani 1 1 d . . . . .
H18A H 0.3453 0.3241 0.1690 0.091 Uiso 1 1 calc R . . . .
H18B H 0.3727 0.3435 0.2256 0.091 Uiso 1 1 calc R . . . .
H18C H 0.3937 0.4184 0.1909 0.091 Uiso 1 1 calc R . . . .
C19 C 0.4956(4) 0.2555(8) 0.2514(3) 0.055(3) Uani 1 1 d . . . . .
H19A H 0.5105 0.3313 0.2458 0.082 Uiso 1 1 calc R . . . .
H19B H 0.4885 0.2607 0.2809 0.082 Uiso 1 1 calc R . . . .
H19C H 0.5220 0.1919 0.2545 0.082 Uiso 1 1 calc R . . . .
C21 C 0.0709(4) 0.1065(9) 0.1147(4) 0.068(3) Uani 1 1 d . . . . .
H21A H 0.0381 0.1052 0.0853 0.102 Uiso 1 1 calc R . . . .
H21B H 0.0703 0.0384 0.1348 0.102 Uiso 1 1 calc R . . . .
H21C H 0.0718 0.1805 0.1322 0.102 Uiso 1 1 calc R . . . .
C22 C 0.1948(4) 0.1002(9) 0.1553(3) 0.055(3) Uani 1 1 d . . . . .
H22A H 0.1960 0.1753 0.1722 0.083 Uiso 1 1 calc R . . . .
H22B H 0.1933 0.0337 0.1757 0.083 Uiso 1 1 calc R . . . .
H22C H 0.2276 0.0931 0.1478 0.083 Uiso 1 1 calc R . . . .
C23 C 0.1319(4) -0.0453(8) 0.0679(3) 0.060(3) Uani 1 1 d . . . . .
H23A H 0.0995 -0.0474 0.0381 0.090 Uiso 1 1 calc R . . . .
H23B H 0.1648 -0.0522 0.0605 0.090 Uiso 1 1 calc R . . . .
H23C H 0.1305 -0.1116 0.0884 0.090 Uiso 1 1 calc R . . . .
C24 C -0.0052(4) 0.2839(10) -0.0090(4) 0.068(3) Uani 1 1 d . . . . .
H24A H -0.0025 0.3589 0.0083 0.102 Uiso 1 1 calc R . . . .
H24B H -0.0368 0.2871 -0.0394 0.102 Uiso 1 1 calc R . . . .
H24C H -0.0098 0.2180 0.0103 0.102 Uiso 1 1 calc R . . . .
C25 C 0.0512(4) 0.1170(9) -0.0541(3) 0.067(3) Uani 1 1 d . . . . .
H25A H 0.0842 0.1028 -0.0608 0.101 Uiso 1 1 calc R . . . .
H25B H 0.0464 0.0518 -0.0345 0.101 Uiso 1 1 calc R . . . .
H25C H 0.0194 0.1210 -0.0842 0.101 Uiso 1 1 calc R . . . .
C26 C 0.0638(4) 0.3839(9) -0.0611(3) 0.060(3) Uani 1 1 d . . . . .
H26A H 0.0970 0.3731 -0.0677 0.090 Uiso 1 1 calc R . . . .
H26B H 0.0319 0.3822 -0.0912 0.090 Uiso 1 1 calc R . . . .
H26C H 0.0654 0.4607 -0.0452 0.090 Uiso 1 1 calc R . . . .
C27 C 0.0858(4) 0.4674(9) 0.1087(4) 0.070(3) Uani 1 1 d . . . . .
H27A H 0.0818 0.4025 0.1288 0.105 Uiso 1 1 calc R . . . .
H27B H 0.0914 0.5424 0.1264 0.105 Uiso 1 1 calc R . . . .
H27C H 0.0527 0.4730 0.0797 0.105 Uiso 1 1 calc R . . . .
C28 C 0.1530(4) 0.5615(7) 0.0539(3) 0.049(3) Uani 1 1 d . . . . .
H28A H 0.1845 0.5463 0.0451 0.073 Uiso 1 1 calc R . . . .
H28B H 0.1198 0.5670 0.0249 0.073 Uiso 1 1 calc R . . . .
H28C H 0.1586 0.6365 0.0717 0.073 Uiso 1 1 calc R . . . .
C29 C 0.2088(4) 0.4357(9) 0.1482(3) 0.060(3) Uani 1 1 d . . . . .
H29A H 0.2408 0.4200 0.1402 0.090 Uiso 1 1 calc R . . . .
H29B H 0.2131 0.5129 0.1642 0.090 Uiso 1 1 calc R . . . .
H29C H 0.2056 0.3731 0.1696 0.090 Uiso 1 1 calc R . . . .
C31 C 0.3051(6) 0.3015(15) -0.2215(4) 0.158(8) Uani 1 1 d . . . A 1
H31A H 0.2674 0.3188 -0.2429 0.237 Uiso 1 1 calc R . . A 1
H31B H 0.3299 0.3579 -0.2276 0.237 Uiso 1 1 calc R . . A 1
H31C H 0.3146 0.2203 -0.2273 0.237 Uiso 1 1 calc R . . A 1
C32 C 0.3826(4) 0.2816(10) -0.1206(4) 0.079(4) Uani 1 1 d . . . B 1
H32A H 0.3874 0.2881 -0.0869 0.118 Uiso 1 1 calc R . . B 1
H32B H 0.3916 0.2006 -0.1271 0.118 Uiso 1 1 calc R . . B 1
H32C H 0.4069 0.3382 -0.1274 0.118 Uiso 1 1 calc R . . B 1
C33 C 0.2959(5) 0.4731(10) -0.1487(5) 0.115(5) Uani 1 1 d . . . C 1
H33A H 0.2579 0.4915 -0.1690 0.173 Uiso 1 1 calc R . . C 1
H33B H 0.3013 0.4841 -0.1151 0.173 Uiso 1 1 calc R . . C 1
H33C H 0.3204 0.5262 -0.1569 0.173 Uiso 1 1 calc R . . C 1
C34 C 0.1510(4) 0.4041(9) -0.1764(4) 0.087(4) Uani 1 1 d . . . . .
H34A H 0.1740 0.4487 -0.1895 0.131 Uiso 1 1 calc R . . . .
H34B H 0.1127 0.4266 -0.1933 0.131 Uiso 1 1 calc R . . . .
H34C H 0.1621 0.4224 -0.1423 0.131 Uiso 1 1 calc R . . . .
C35 C 0.1354(4) 0.2105(11) -0.2490(3) 0.083(4) Uani 1 1 d . . . . .
H35A H 0.1394 0.1253 -0.2537 0.124 Uiso 1 1 calc R . . . .
H35B H 0.0970 0.2332 -0.2647 0.124 Uiso 1 1 calc R . . . .
H35C H 0.1574 0.2558 -0.2629 0.124 Uiso 1 1 calc R . . . .
C36 C 0.1151(4) 0.1611(11) -0.1588(4) 0.089(4) Uani 1 1 d . . . . .
H36A H 0.1189 0.0754 -0.1625 0.133 Uiso 1 1 calc R . . . .
H36B H 0.1263 0.1803 -0.1248 0.133 Uiso 1 1 calc R . . . .
H36C H 0.0770 0.1845 -0.1758 0.133 Uiso 1 1 calc R . . . .
C37 C 0.3363(4) -0.0580(9) -0.1246(4) 0.074(4) Uani 1 1 d . . . . .
H37A H 0.3615 -0.0053 -0.1322 0.111 Uiso 1 1 calc R . . . .
H37B H 0.3433 -0.0526 -0.0905 0.111 Uiso 1 1 calc R . . . .
H37C H 0.3420 -0.1401 -0.1327 0.111 Uiso 1 1 calc R . . . .
C38 C 0.2521(6) -0.0315(11) -0.2257(3) 0.124(6) Uani 1 1 d . . . . .
H38A H 0.2770 0.0206 -0.2339 0.186 Uiso 1 1 calc R . . . .
H38B H 0.2590 -0.1144 -0.2317 0.186 Uiso 1 1 calc R . . . .
H38C H 0.2142 -0.0106 -0.2454 0.186 Uiso 1 1 calc R . . . .
C39 C 0.2159(4) -0.1126(9) -0.1461(4) 0.072(3) Uani 1 1 d . . . . .
H39A H 0.1782 -0.0886 -0.1648 0.108 Uiso 1 1 calc R . . . .
H39B H 0.2215 -0.1947 -0.1542 0.108 Uiso 1 1 calc R . . . .
H39C H 0.2229 -0.1072 -0.1120 0.108 Uiso 1 1 calc R . . . .
C101 C 0.3187(5) -0.3073(12) -0.0464(4) 0.094(5) Uani 1 1 d . . . . .
H10A H 0.3044 -0.2334 -0.0646 0.113 Uiso 1 1 calc R . . . .
H10B H 0.2955 -0.3748 -0.0635 0.113 Uiso 1 1 calc R . . . .
C102 C 0.3773(5) -0.3275(14) -0.0402(5) 0.121(6) Uani 1 1 d . . . . .
H10C H 0.3837 -0.4123 -0.0452 0.145 Uiso 1 1 calc R . . . .
H10D H 0.3868 -0.2789 -0.0633 0.145 Uiso 1 1 calc R . . . .
C103 C 0.4091(5) -0.2922(11) 0.0076(5) 0.087(4) Uani 1 1 d . . . . .
H10E H 0.4169 -0.2058 0.0096 0.105 Uiso 1 1 calc R . . . .
H10F H 0.4441 -0.3365 0.0205 0.105 Uiso 1 1 calc R . . . .
C104 C 0.3726(5) -0.3243(11) 0.0332(4) 0.079(4) Uani 1 1 d . . . . .
H10G H 0.3761 -0.4097 0.0419 0.095 Uiso 1 1 calc R . . . .
H10H H 0.3814 -0.2764 0.0627 0.095 Uiso 1 1 calc R . . . .
C105 C 0.3315(4) -0.3244(10) 0.1483(4) 0.068(3) Uani 1 1 d . . . . .
H10I H 0.3628 -0.2853 0.1439 0.082 Uiso 1 1 calc R . . . .
H10J H 0.3296 -0.4078 0.1372 0.082 Uiso 1 1 calc R . . . .
C106 C 0.3386(5) -0.3213(13) 0.1980(4) 0.100(4) Uani 1 1 d . . . . .
H10K H 0.3776 -0.3131 0.2190 0.120 Uiso 1 1 calc R . . . .
H10L H 0.3236 -0.3937 0.2071 0.120 Uiso 1 1 calc R . . . .
C107 C 0.3072(6) -0.2148(11) 0.2005(4) 0.089(4) Uani 1 1 d . . . . .
H10M H 0.2900 -0.2267 0.2241 0.106 Uiso 1 1 calc R . . . .
H10N H 0.3316 -0.1446 0.2102 0.106 Uiso 1 1 calc R . . . .
C108 C 0.2663(5) -0.1973(10) 0.1537(4) 0.079(4) Uani 1 1 d . . . . .
H10O H 0.2303 -0.2250 0.1526 0.094 Uiso 1 1 calc R . . . .
H10P H 0.2635 -0.1120 0.1451 0.094 Uiso 1 1 calc R . . . .
C109 C 0.1460(5) -0.3431(10) -0.0925(4) 0.074(3) Uani 1 1 d . U . . .
H10Q H 0.1482 -0.4278 -0.0830 0.089 Uiso 1 1 calc R . . . .
H10R H 0.1757 -0.3264 -0.1040 0.089 Uiso 1 1 calc R . . . .
C110 C 0.0924(6) -0.3170(13) -0.1302(4) 0.112(5) Uani 1 1 d . U . . .
H11D H 0.0968 -0.2928 -0.1601 0.135 Uiso 1 1 calc R . . . .
H11E H 0.0686 -0.3882 -0.1370 0.135 Uiso 1 1 calc R . . . .
C111 C 0.0693(6) -0.2236(16) -0.1130(6) 0.167(7) Uani 1 1 d . U . . .
H11F H 0.0326 -0.2467 -0.1145 0.201 Uiso 1 1 calc R . . . .
H11G H 0.0655 -0.1517 -0.1329 0.201 Uiso 1 1 calc R . . . .
C112 C 0.1047(5) -0.1995(12) -0.0643(5) 0.102(5) Uani 1 1 d . U . . .
H11H H 0.1148 -0.1142 -0.0607 0.122 Uiso 1 1 calc R . . . .
H11I H 0.0857 -0.2183 -0.0426 0.122 Uiso 1 1 calc R . . . .
C201 C 0.0084(10) 0.966(2) 0.7442(8) 0.252(12) Uiso 1 1 d D . . . .
C202 C 0.0292(10) 0.861(2) 0.7312(9) 0.256(12) Uiso 1 1 d D . . . .
H20A H 0.0325 0.8031 0.7568 0.307 Uiso 1 1 calc R . . . .
H20B H -0.0008 0.8313 0.7023 0.307 Uiso 1 1 calc R . . . .
C203 C 0.0766(10) 0.847(2) 0.7218(9) 0.242(11) Uiso 1 1 d D . . . .
C204 C 0.0837(9) 0.726(2) 0.7137(9) 0.263(13) Uiso 1 1 d D . . . .
H20C H 0.0539 0.7016 0.6835 0.315 Uiso 1 1 calc R . . . .
H20D H 0.0795 0.6788 0.7398 0.315 Uiso 1 1 calc R . . . .
C205 C 0.1368(8) 0.6926(17) 0.7103(7) 0.219(10) Uiso 1 1 d D . . . .
H20E H 0.1373 0.6069 0.7047 0.329 Uiso 1 1 calc R . . . .
H20F H 0.1411 0.7360 0.6839 0.329 Uiso 1 1 calc R . . . .
H20G H 0.1668 0.7131 0.7403 0.329 Uiso 1 1 calc R . . . .
K K 0.23959(9) -0.2447(2) 0.02617(8) 0.0587(7) Uani 1 1 d . . . . .
O1 O 0.3198(3) -0.2982(6) 0.0001(3) 0.080(2) Uani 1 1 d . . . . .
O2 O 0.2828(3) -0.2643(6) 0.1217(2) 0.063(2) Uani 1 1 d . . . . .
O3 O 0.1509(3) -0.2681(6) -0.0530(2) 0.067(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 Ge4 2.5284(13) . ?
Ge1 Ge5 2.5353(13) . ?
Ge1 Ge7 2.5394(13) . ?
Ge1 Ge8 2.5252(12) . ?
Ge1 Si1 2.368(2) . ?
Ge2 Ge5 2.5387(13) . ?
Ge2 Ge6 2.5422(13) . ?
Ge2 Ge8 2.5348(13) . ?
Ge2 Ge9 2.5323(13) . ?
Ge2 Si2 2.367(2) . ?
Ge3 Ge4 2.5258(13) . ?
Ge3 Ge6 2.5347(13) . ?
Ge3 Ge7 2.5352(13) . ?
Ge3 Ge9 2.5152(12) . ?
Ge3 Si3 2.369(2) . ?
Ge4 Ge5 2.6923(12) . ?
Ge4 Ge6 2.6913(13) . ?
Ge5 Ge6 2.6090(13) . ?
Ge7 Ge8 2.7010(12) . ?
Ge7 Ge9 2.7210(13) . ?
Ge8 Ge9 2.6406(13) . ?
Ge8 K 3.852(3) . ?
Ge9 K 3.734(3) . ?
Si1 Si11 2.336(3) . ?
Si1 Si12 2.349(3) . ?
Si1 Si13 2.344(3) . ?
Si2 Si21 2.343(3) . ?
Si2 Si22 2.339(3) . ?
Si2 Si23 2.346(3) . ?
Si3 Si31 2.337(4) . ?
Si3 Si32 2.343(3) . ?
Si3 Si33 2.347(4) . ?
Si11 C11 1.863(9) . ?
Si11 C12 1.893(8) . ?
Si11 C13 1.875(8) . ?
Si12 C14 1.848(8) . ?
Si12 C15 1.874(9) . ?
Si12 C16 1.881(9) . ?
Si13 C17 1.867(9) . ?
Si13 C18 1.871(9) . ?
Si13 C19 1.863(9) . ?
Si21 C21 1.885(8) . ?
Si21 C22 1.850(9) . ?
Si21 C23 1.859(9) . ?
Si22 C24 1.867(8) . ?
Si22 C25 1.874(9) . ?
Si22 C26 1.880(9) . ?
Si23 C27 1.866(8) . ?
Si23 C28 1.867(8) . ?
Si23 C29 1.875(9) . ?
Si31 C31 1.847(10) . ?
Si31 C32 1.844(10) . ?
Si31 C33 1.871(12) . ?
Si32 C34 1.850(11) . ?
Si32 C35 1.859(9) . ?
Si32 C36 1.855(10) . ?
Si33 C37 1.880(10) . ?
Si33 C38 1.890(9) . ?
Si33 C39 1.868(10) . ?
C101 C102 1.506(14) . ?
C101 O1 1.398(12) . ?
C102 C103 1.427(16) . ?
C103 C104 1.493(14) . ?
C104 O1 1.409(13) . ?
C105 C106 1.444(13) . ?
C105 O2 1.408(11) . ?
C106 C107 1.475(15) . ?
C107 C108 1.432(14) . ?
C108 O2 1.418(11) . ?
C109 C110 1.475(15) . ?
C109 O3 1.427(11) . ?
C110 C111 1.410(16) . ?
C111 C112 1.441(16) . ?
C112 O3 1.374(13) . ?
C201 C202 1.420(16) . ?
C202 C203 1.396(17) . ?
C203 C204 1.407(17) . ?
C204 C205 1.493(16) . ?
K C28 3.485(9) 1_545 ?
K O1 2.598(7) . ?
K O2 2.683(7) . ?
K O3 2.654(7) . ?

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
Ge4 Ge1 Ge5 64.24(4) . . ?
Ge4 Ge1 Ge7 79.22(4) . . ?
Ge5 Ge1 Ge7 116.95(4) . . ?
Ge8 Ge1 Ge4 116.67(4) . . ?
Ge8 Ge1 Ge5 87.77(4) . . ?
Ge8 Ge1 Ge7 64.46(4) . . ?
Si1 Ge1 Ge4 123.09(7) . . ?
Si1 Ge1 Ge5 120.77(7) . . ?
Si1 Ge1 Ge7 122.16(7) . . ?
Si1 Ge1 Ge8 120.10(7) . . ?
Ge5 Ge2 Ge6 61.79(4) . . ?
Ge8 Ge2 Ge5 87.49(4) . . ?
Ge8 Ge2 Ge6 118.25(4) . . ?
Ge9 Ge2 Ge5 118.47(4) . . ?
Ge9 Ge2 Ge6 85.63(4) . . ?
Ge9 Ge2 Ge8 62.82(4) . . ?
Si2 Ge2 Ge5 122.25(7) . . ?
Si2 Ge2 Ge6 118.93(7) . . ?
Si2 Ge2 Ge8 122.74(7) . . ?
Si2 Ge2 Ge9 119.11(7) . . ?
Ge4 Ge3 Ge6 64.26(4) . . ?
Ge4 Ge3 Ge7 79.35(4) . . ?
Ge6 Ge3 Ge7 116.42(4) . . ?
Ge9 Ge3 Ge4 116.43(4) . . ?
Ge9 Ge3 Ge6 86.14(4) . . ?
Ge9 Ge3 Ge7 65.20(4) . . ?
Si3 Ge3 Ge4 120.20(7) . . ?
Si3 Ge3 Ge6 119.16(7) . . ?
Si3 Ge3 Ge7 124.11(7) . . ?
Si3 Ge3 Ge9 123.35(7) . . ?
Ge1 Ge4 Ge5 58.01(3) . . ?
Ge1 Ge4 Ge6 100.10(4) . . ?
Ge3 Ge4 Ge1 94.35(4) . . ?
Ge3 Ge4 Ge5 100.79(4) . . ?
Ge3 Ge4 Ge6 58.03(4) . . ?
Ge6 Ge4 Ge5 57.98(3) . . ?
Ge1 Ge5 Ge2 88.90(4) . . ?
Ge1 Ge5 Ge4 57.76(3) . . ?
Ge1 Ge5 Ge6 102.16(4) . . ?
Ge2 Ge5 Ge4 99.40(4) . . ?
Ge2 Ge5 Ge6 59.17(4) . . ?
Ge6 Ge5 Ge4 60.99(3) . . ?
Ge2 Ge6 Ge4 99.33(4) . . ?
Ge2 Ge6 Ge5 59.04(4) . . ?
Ge3 Ge6 Ge2 89.94(4) . . ?
Ge3 Ge6 Ge4 57.71(3) . . ?
Ge3 Ge6 Ge5 102.85(4) . . ?
Ge5 Ge6 Ge4 61.03(3) . . ?
Ge1 Ge7 Ge8 57.52(3) . . ?
Ge1 Ge7 Ge9 99.48(4) . . ?
Ge3 Ge7 Ge1 93.85(4) . . ?
Ge3 Ge7 Ge8 100.20(4) . . ?
Ge3 Ge7 Ge9 57.05(3) . . ?
Ge8 Ge7 Ge9 58.29(3) . . ?
Ge1 Ge8 Ge2 89.21(4) . . ?
Ge1 Ge8 Ge7 58.02(3) . . ?
Ge1 Ge8 Ge9 102.03(4) . . ?
Ge1 Ge8 K 135.85(5) . . ?
Ge2 Ge8 Ge7 99.79(4) . . ?
Ge2 Ge8 Ge9 58.55(4) . . ?
Ge2 Ge8 K 115.52(5) . . ?
Ge7 Ge8 K 81.07(4) . . ?
Ge9 Ge8 Ge7 61.24(3) . . ?
Ge9 Ge8 K 67.25(4) . . ?
Ge2 Ge9 Ge7 99.32(4) . . ?
Ge2 Ge9 Ge8 58.64(4) . . ?
Ge2 Ge9 K 119.53(5) . . ?
Ge3 Ge9 Ge2 90.61(4) . . ?
Ge3 Ge9 Ge7 57.76(3) . . ?
Ge3 Ge9 Ge8 102.38(4) . . ?
Ge3 Ge9 K 134.81(5) . . ?
Ge7 Ge9 K 83.10(5) . . ?
Ge8 Ge9 Ge7 60.48(3) . . ?
Ge8 Ge9 K 72.05(5) . . ?
Si11 Si1 Ge1 108.39(11) . . ?
Si11 Si1 Si12 110.88(12) . . ?
Si11 Si1 Si13 111.26(13) . . ?
Si12 Si1 Ge1 110.49(11) . . ?
Si13 Si1 Ge1 105.96(10) . . ?
Si13 Si1 Si12 109.75(13) . . ?
Si21 Si2 Ge2 107.22(11) . . ?
Si21 Si2 Si23 110.34(12) . . ?
Si22 Si2 Ge2 108.92(11) . . ?
Si22 Si2 Si21 112.06(13) . . ?
Si22 Si2 Si23 111.52(13) . . ?
Si23 Si2 Ge2 106.52(11) . . ?
Si31 Si3 Ge3 108.45(12) . . ?
Si31 Si3 Si32 112.26(14) . . ?
Si31 Si3 Si33 111.92(14) . . ?
Si32 Si3 Ge3 105.70(11) . . ?
Si32 Si3 Si33 110.94(15) . . ?
Si33 Si3 Ge3 107.21(12) . . ?
C11 Si11 Si1 110.7(3) . . ?
C11 Si11 C12 106.9(4) . . ?
C11 Si11 C13 109.2(4) . . ?
C12 Si11 Si1 110.2(3) . . ?
C13 Si11 Si1 110.2(3) . . ?
C13 Si11 C12 109.5(4) . . ?
C14 Si12 Si1 111.4(3) . . ?
C14 Si12 C15 109.5(4) . . ?
C14 Si12 C16 107.7(4) . . ?
C15 Si12 Si1 109.8(3) . . ?
C15 Si12 C16 109.2(5) . . ?
C16 Si12 Si1 109.1(3) . . ?
C17 Si13 Si1 110.6(3) . . ?
C17 Si13 C18 108.4(4) . . ?
C18 Si13 Si1 109.8(3) . . ?
C19 Si13 Si1 110.5(3) . . ?
C19 Si13 C17 108.2(4) . . ?
C19 Si13 C18 109.3(4) . . ?
C21 Si21 Si2 110.2(3) . . ?
C22 Si21 Si2 110.3(3) . . ?
C22 Si21 C21 108.7(4) . . ?
C22 Si21 C23 108.9(4) . . ?
C23 Si21 Si2 110.1(3) . . ?
C23 Si21 C21 108.6(5) . . ?
C24 Si22 Si2 111.0(3) . . ?
C24 Si22 C25 107.9(5) . . ?
C24 Si22 C26 108.5(4) . . ?
C25 Si22 Si2 110.8(3) . . ?
C25 Si22 C26 108.0(5) . . ?
C26 Si22 Si2 110.6(3) . . ?
C27 Si23 Si2 111.2(3) . . ?
C27 Si23 C28 109.1(4) . . ?
C27 Si23 C29 108.3(4) . . ?
C28 Si23 Si2 109.3(3) . . ?
C28 Si23 C29 107.6(4) . . ?
C29 Si23 Si2 111.2(3) . . ?
C31 Si31 Si3 110.5(4) . . ?
C31 Si31 C33 107.8(7) . . ?
C32 Si31 Si3 111.6(4) . . ?
C32 Si31 C31 107.2(6) . . ?
C32 Si31 C33 109.1(6) . . ?
C33 Si31 Si3 110.5(3) . . ?
C34 Si32 Si3 110.2(3) . . ?
C34 Si32 C35 108.3(5) . . ?
C34 Si32 C36 108.4(5) . . ?
C35 Si32 Si3 111.5(3) . . ?
C36 Si32 Si3 109.5(4) . . ?
C36 Si32 C35 108.9(5) . . ?
C37 Si33 Si3 110.1(4) . . ?
C37 Si33 C38 107.4(5) . . ?
C38 Si33 Si3 111.0(4) . . ?
C39 Si33 Si3 110.6(3) . . ?
C39 Si33 C37 109.5(5) . . ?
C39 Si33 C38 108.2(6) . . ?
O1 C101 C102 104.9(10) . . ?
C103 C102 C101 105.6(11) . . ?
C102 C103 C104 102.1(10) . . ?
O1 C104 C103 104.0(10) . . ?
O2 C105 C106 108.1(9) . . ?
C105 C106 C107 102.6(10) . . ?
C108 C107 C106 106.9(10) . . ?
O2 C108 C107 106.7(9) . . ?
O3 C109 C110 106.6(9) . . ?
C111 C110 C109 106.7(11) . . ?
C110 C111 C112 108.1(12) . . ?
O3 C112 C111 108.9(10) . . ?
C203 C202 C201 129(3) . . ?
C202 C203 C204 110(2) . . ?
C203 C204 C205 116(2) . . ?
Ge9 K Ge8 40.71(3) . . ?
C28 K Ge8 130.62(15) 1_545 . ?
C28 K Ge9 131.39(16) 1_545 . ?
O1 K Ge8 97.59(18) . . ?
O1 K Ge9 96.80(17) . . ?
O1 K C28 127.9(2) . 1_545 ?
O1 K O2 104.1(3) . . ?
O1 K O3 104.4(3) . . ?
O2 K Ge8 76.24(16) . . ?
O2 K Ge9 115.68(17) . . ?
O2 K C28 75.0(2) . 1_545 ?
O3 K Ge8 116.91(17) . . ?
O3 K Ge9 78.02(16) . . ?
O3 K C28 73.6(2) . 1_545 ?
O3 K O2 146.4(2) . . ?
C101 O1 C104 109.7(8) . . ?
C101 O1 K 127.9(7) . . ?
C104 O1 K 122.4(7) . . ?
C105 O2 C108 108.6(8) . . ?
C105 O2 K 125.3(6) . . ?
C108 O2 K 125.1(6) . . ?
C109 O3 K 125.6(6) . . ?
C112 O3 C109 109.4(8) . . ?
C112 O3 K 124.7(7) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
