#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:24:52 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180077 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/23/7052392.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7052392
loop_
_publ_author_name
'Suchentrunk, Christof'
'Korber, Nikolaus'
_publ_section_title
;
 Ge52? Zintl anions: synthesis and crystal structures of
 [K([2.2.2]-crypt)]2Ge5?4NH3 and [Rb([2.2.2]-crypt)]2Ge5?4NH3
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1737
_journal_paper_doi               10.1039/b610547e
_journal_volume                  30
_journal_year                    2006
_chemical_formula_moiety         'C36 H84 Ge5 N8 O12 K2'
_chemical_formula_sum            'C36 H84 Ge5 K2 N8 O12'
_chemical_formula_weight         1262.26
_chemical_name_common
;
Bis(potassium-(4,7,13,1621,24-Hexaoxa-1,10-
diazabicyclo(8.8.8)hexacosane))-nonagermanid - ammonia(1/4)
;
_chemical_name_systematic
;
Bis[potassium-(4,7,13,1621,24-Hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)]-
nonagermanid - ammonia(1/4)
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                117.911(8)
_cell_angle_beta                 98.650(9)
_cell_angle_gamma                91.797(9)
_cell_formula_units_Z            1
_cell_length_a                   11.2887(9)
_cell_length_b                   11.8949(9)
_cell_length_c                   11.9433(9)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      51.86
_cell_measurement_theta_min      3.90
_cell_volume                     1391.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       Phi
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10669
_diffrn_reflns_theta_full        25.93
_diffrn_reflns_theta_max         25.93
_diffrn_reflns_theta_min         1.95
_diffrn_standards_interval_time  6.0
_diffrn_standards_number         8934
_exptl_absorpt_coefficient_mu    2.876
_exptl_absorpt_correction_T_max  0.649
_exptl_absorpt_correction_T_min  0.178
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(A.L.Spek, Platon 2004'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             650
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.313
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.668(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         8934
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0866P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1205
_reflns_number_gt                8001
_reflns_number_total             8934
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b610547e.txt
_cod_data_source_block           K-Crypt_Ge5
_cod_original_cell_volume        1391.51(19)
_cod_database_code               7052392
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.57784(5) 0.39973(6) 0.87466(7) 0.03746(17) Uani 1 1 d . . .
Ge2 Ge 0.39963(6) 0.51811(6) 0.87003(7) 0.04148(18) Uani 1 1 d . . .
Ge3 Ge 0.40687(7) 0.34805(8) 0.96081(7) 0.0463(2) Uani 1 1 d . . .
Ge4 Ge 0.39579(6) 0.26700(7) 0.70766(7) 0.04020(17) Uani 1 1 d . . .
Ge5 Ge 0.22418(6) 0.35681(7) 0.81855(7) 0.03962(18) Uani 1 1 d . . .
K1 K 0.94281(12) 0.95998(11) 1.05721(12) 0.0290(3) Uani 1 1 d . . .
K2 K 0.10364(10) -0.33330(11) 0.43643(12) 0.0246(2) Uani 1 1 d . . .
O11 O 0.2319(4) -0.5334(5) 0.4356(5) 0.0422(12) Uani 1 1 d . . .
O8 O -0.0114(4) -0.1249(4) 0.5835(4) 0.0350(10) Uani 1 1 d . . .
O5 O 1.0356(4) 1.1623(4) 1.0270(4) 0.0331(9) Uani 1 1 d . . .
O12 O -0.0057(4) -0.5099(4) 0.4897(4) 0.0340(10) Uani 1 1 d . . .
O2 O 0.8138(4) 0.9410(4) 1.2389(4) 0.0379(10) Uani 1 1 d . . .
O9 O 0.2055(5) -0.2856(8) 0.2560(7) 0.068(2) Uani 1 1 d . . .
O10 O -0.0345(6) -0.4036(6) 0.2002(5) 0.0544(15) Uani 1 1 d . . .
O1 O 1.0544(4) 1.0620(4) 1.3178(4) 0.0364(10) Uani 1 1 d . . .
O6 O 0.7815(4) 1.1142(5) 1.0010(6) 0.0470(13) Uani 1 1 d . . .
O3 O 1.1040(6) 0.7859(5) 0.9348(5) 0.0545(15) Uani 1 1 d . . .
O7 O 0.2370(5) -0.1280(5) 0.6595(6) 0.0629(18) Uani 1 1 d . . .
O4 O 0.8580(6) 0.7164(5) 0.8279(5) 0.0506(13) Uani 1 1 d . . .
N1 N 1.2088(5) 1.0423(6) 1.1359(5) 0.0369(12) Uani 1 1 d . . .
N3 N 0.3690(5) -0.3040(5) 0.4639(7) 0.0411(14) Uani 1 1 d . . .
N4 N -0.1651(5) -0.3652(5) 0.4035(6) 0.0373(13) Uani 1 1 d . . .
N2 N 0.6788(6) 0.8691(7) 0.9762(7) 0.0492(15) Uani 1 1 d . . .
N5 N 0.6372(6) 0.0514(7) 0.5817(9) 0.062(2) Uani 1 1 d . . .
H5C H 0.5985 0.1203 0.6157 0.093 Uiso 1 1 calc R . .
H5D H 0.5842 -0.0169 0.5291 0.093 Uiso 1 1 calc R . .
H5E H 0.6887 0.0629 0.5373 0.093 Uiso 1 1 calc R . .
N6 N 0.6194(8) 0.2994(14) 0.5020(12) 0.104(4) Uani 1 1 d . . .
H6C H 0.6585 0.3158 0.5795 0.156 Uiso 1 1 calc R . .
H6D H 0.5480 0.2549 0.4846 0.156 Uiso 1 1 calc R . .
H6E H 0.6084 0.3728 0.5011 0.156 Uiso 1 1 calc R . .
N7 N 0.8606(6) 0.2882(7) 0.6926(7) 0.0551(16) Uani 1 1 d . . .
H7C H 0.9304 0.3313 0.7436 0.083 Uiso 1 1 calc R . .
H7D H 0.8344 0.2326 0.7162 0.083 Uiso 1 1 calc R . .
H7E H 0.8065 0.3428 0.6993 0.083 Uiso 1 1 calc R . .
N8 N 0.5865(9) 0.2780(12) 0.2156(10) 0.104(4) Uani 1 1 d . . .
H8C H 0.6109 0.3378 0.2974 0.156 Uiso 1 1 calc R . .
H8D H 0.5194 0.2321 0.2087 0.156 Uiso 1 1 calc R . .
H8E H 0.5719 0.3153 0.1662 0.156 Uiso 1 1 calc R . .
C1 C -0.2171(7) -0.4345(7) 0.2652(8) 0.049(2) Uani 1 1 d . . .
H1A H -0.3025 -0.4251 0.2536 0.059 Uiso 1 1 calc R . .
H1B H -0.2095 -0.5250 0.2330 0.059 Uiso 1 1 calc R . .
C2 C 0.8356(7) 1.1878(7) 0.9513(8) 0.0454(17) Uani 1 1 d . . .
H2A H 0.7831 1.2502 0.9496 0.055 Uiso 1 1 calc R . .
H2B H 0.8457 1.1317 0.8637 0.055 Uiso 1 1 calc R . .
C3 C -0.1302(6) -0.5537(6) 0.4401(7) 0.0356(14) Uani 1 1 d . . .
H3A H -0.1591 -0.6012 0.4801 0.043 Uiso 1 1 calc R . .
H3B H -0.1428 -0.6102 0.3477 0.043 Uiso 1 1 calc R . .
C4 C 1.2439(6) 1.1172(7) 1.2784(6) 0.0404(15) Uani 1 1 d . . .
H4A H 1.2239 1.2039 1.3064 0.049 Uiso 1 1 calc R . .
H4B H 1.3305 1.1217 1.3027 0.049 Uiso 1 1 calc R . .
C5 C 0.9542(7) 1.2545(6) 1.0324(8) 0.0436(16) Uani 1 1 d . . .
H5A H 0.9870 1.3093 1.0021 0.052 Uiso 1 1 calc R . .
H5B H 0.9447 1.3078 1.1209 0.052 Uiso 1 1 calc R . .
C6 C 1.2382(7) 1.1240(8) 1.0785(8) 0.0482(18) Uani 1 1 d . . .
H6A H 1.2373 1.0695 0.9873 0.058 Uiso 1 1 calc R . .
H6B H 1.3195 1.1670 1.1183 0.058 Uiso 1 1 calc R . .
C7 C 0.0610(6) -0.6129(7) 0.4826(8) 0.0407(16) Uani 1 1 d . . .
H7A H 0.0454 -0.6828 0.3948 0.049 Uiso 1 1 calc R . .
H7B H 0.0355 -0.6445 0.5378 0.049 Uiso 1 1 calc R . .
C8 C -0.1996(6) -0.4373(6) 0.4688(8) 0.0397(15) Uani 1 1 d . . .
H8A H -0.2854 -0.4660 0.4413 0.048 Uiso 1 1 calc R . .
H8B H -0.1844 -0.3806 0.5612 0.048 Uiso 1 1 calc R . .
C9 C 0.6668(7) 1.0452(10) 0.9179(10) 0.062(2) Uani 1 1 d . . .
H9A H 0.6797 0.9861 0.8322 0.075 Uiso 1 1 calc R . .
H9B H 0.6136 1.1051 0.9110 0.075 Uiso 1 1 calc R . .
C10 C 0.9454(11) 0.6247(7) 0.8013(7) 0.063(3) Uani 1 1 d . . .
H10A H 0.9517 0.5937 0.8637 0.076 Uiso 1 1 calc R . .
H10B H 0.9184 0.5522 0.7161 0.076 Uiso 1 1 calc R . .
C11 C 1.2731(8) 0.9289(9) 1.0882(8) 0.055(2) Uani 1 1 d . . .
H11A H 1.2677 0.8884 1.1416 0.066 Uiso 1 1 calc R . .
H11B H 1.3577 0.9563 1.0983 0.066 Uiso 1 1 calc R . .
C12 C 0.9937(8) 1.0322(7) 1.3996(6) 0.0426(17) Uani 1 1 d . . .
H12A H 1.0249 1.0931 1.4893 0.051 Uiso 1 1 calc R . .
H12B H 1.0075 0.9471 1.3863 0.051 Uiso 1 1 calc R . .
C13 C 0.0590(6) -0.0288(6) 0.7026(7) 0.0384(15) Uani 1 1 d . . .
H13A H 0.0571 -0.0533 0.7692 0.046 Uiso 1 1 calc R . .
H13B H 0.0252 0.0518 0.7289 0.046 Uiso 1 1 calc R . .
C14 C 0.1840(7) -0.0132(7) 0.6873(7) 0.0399(15) Uani 1 1 d . . .
H14A H 0.1855 0.0071 0.6177 0.048 Uiso 1 1 calc R . .
H14B H 0.2299 0.0571 0.7660 0.048 Uiso 1 1 calc R . .
C15 C 0.4182(7) -0.2012(10) 0.5908(8) 0.059(2) Uani 1 1 d . . .
H15A H 0.4260 -0.2376 0.6488 0.071 Uiso 1 1 calc R . .
H15B H 0.4993 -0.1739 0.5888 0.071 Uiso 1 1 calc R . .
C16 C 0.8627(8) 1.0382(7) 1.3678(7) 0.0459(17) Uani 1 1 d . . .
H16A H 0.8215 1.0263 1.4279 0.055 Uiso 1 1 calc R . .
H16B H 0.8498 1.1218 1.3761 0.055 Uiso 1 1 calc R . .
C17 C -0.2063(6) -0.2365(6) 0.4647(8) 0.0460(18) Uani 1 1 d . . .
H17A H -0.2898 -0.2461 0.4725 0.055 Uiso 1 1 calc R . .
H17B H -0.2033 -0.1990 0.4083 0.055 Uiso 1 1 calc R . .
C18 C 0.1931(7) -0.5665(8) 0.5246(7) 0.0470(17) Uani 1 1 d . . .
H18A H 0.2080 -0.4924 0.6099 0.056 Uiso 1 1 calc R . .
H18B H 0.2379 -0.6332 0.5288 0.056 Uiso 1 1 calc R . .
C19 C 0.4134(8) -0.4234(11) 0.448(2) 0.148(9) Uani 1 1 d . . .
H19A H 0.4290 -0.4667 0.3605 0.178 Uiso 1 1 calc R . .
H19B H 0.4917 -0.3988 0.5043 0.178 Uiso 1 1 calc R . .
C20 C -0.1335(6) -0.1447(7) 0.5966(8) 0.0465(18) Uani 1 1 d . . .
H20A H -0.1673 -0.0638 0.6318 0.056 Uiso 1 1 calc R . .
H20B H -0.1357 -0.1801 0.6549 0.056 Uiso 1 1 calc R . .
C21 C 0.7450(9) 0.6574(8) 0.8193(8) 0.062(3) Uani 1 1 d . . .
H21A H 0.7497 0.6278 0.8828 0.075 Uiso 1 1 calc R . .
H21B H 0.7194 0.5842 0.7343 0.075 Uiso 1 1 calc R . .
C22 C 1.1540(7) 1.2232(7) 1.0933(7) 0.0424(16) Uani 1 1 d . . .
H22A H 1.1532 1.2780 1.1840 0.051 Uiso 1 1 calc R . .
H22B H 1.1816 1.2762 1.0584 0.051 Uiso 1 1 calc R . .
C23 C 0.4018(8) -0.2752(11) 0.3659(9) 0.073(3) Uani 1 1 d . . .
H23A H 0.4401 -0.1875 0.4119 0.088 Uiso 1 1 calc R . .
H23B H 0.4644 -0.3285 0.3318 0.088 Uiso 1 1 calc R . .
C24 C 1.2276(8) 0.8303(9) 0.9490(8) 0.060(2) Uani 1 1 d . . .
H24A H 1.2343 0.8681 0.8934 0.071 Uiso 1 1 calc R . .
H24B H 1.2757 0.7591 0.9246 0.071 Uiso 1 1 calc R . .
C25 C 0.6561(9) 0.7547(10) 0.8438(8) 0.066(3) Uani 1 1 d . . .
H25A H 0.6558 0.7851 0.7812 0.080 Uiso 1 1 calc R . .
H25B H 0.5762 0.7119 0.8283 0.080 Uiso 1 1 calc R . .
C26 C 0.3636(9) -0.0955(10) 0.6455(12) 0.079(3) Uani 1 1 d . . .
H26A H 0.3590 -0.0529 0.5929 0.095 Uiso 1 1 calc R . .
H26B H 0.4107 -0.0371 0.7298 0.095 Uiso 1 1 calc R . .
C27 C 0.3288(12) -0.285(3) 0.267(2) 0.240(17) Uani 1 1 d . . .
H27A H 0.3424 -0.3627 0.1942 0.288 Uiso 1 1 calc R . .
H27B H 0.3569 -0.2146 0.2540 0.288 Uiso 1 1 calc R . .
C28 C 1.0622(10) 0.6830(7) 0.8077(7) 0.060(3) Uani 1 1 d . . .
H28A H 1.1190 0.6197 0.7861 0.072 Uiso 1 1 calc R . .
H28B H 1.0562 0.7149 0.7460 0.072 Uiso 1 1 calc R . .
C29 C 1.1819(7) 1.0600(7) 1.3468(6) 0.0414(16) Uani 1 1 d . . .
H29A H 1.1998 0.9726 1.3184 0.050 Uiso 1 1 calc R . .
H29B H 1.2107 1.1091 1.4391 0.050 Uiso 1 1 calc R . .
C30 C 0.6100(7) 0.9721(11) 0.9757(12) 0.068(3) Uani 1 1 d . . .
H30A H 0.6033 1.0317 1.0636 0.081 Uiso 1 1 calc R . .
H30B H 0.5291 0.9352 0.9271 0.081 Uiso 1 1 calc R . .
C31 C 0.3601(7) -0.5103(10) 0.4638(18) 0.107(6) Uani 1 1 d . . .
H31A H 0.3859 -0.4896 0.5532 0.128 Uiso 1 1 calc R . .
H31B H 0.3904 -0.5904 0.4116 0.128 Uiso 1 1 calc R . .
C32 C 0.6864(7) 0.9294(8) 1.2101(9) 0.0500(18) Uani 1 1 d . . .
H32A H 0.6605 1.0120 1.2273 0.060 Uiso 1 1 calc R . .
H32B H 0.6530 0.9024 1.2650 0.060 Uiso 1 1 calc R . .
C33 C -0.1582(9) -0.3886(8) 0.1859(8) 0.065(3) Uani 1 1 d . . .
H33A H -0.1963 -0.4378 0.0958 0.078 Uiso 1 1 calc R . .
H33B H -0.1683 -0.2992 0.2144 0.078 Uiso 1 1 calc R . .
C34 C 0.6396(7) 0.8324(8) 1.0693(8) 0.0505(19) Uani 1 1 d . . .
H34A H 0.6671 0.7506 1.0530 0.061 Uiso 1 1 calc R . .
H34B H 0.5522 0.8212 1.0542 0.061 Uiso 1 1 calc R . .
C35 C 0.145(2) -0.3805(13) 0.1317(16) 0.135(8) Uani 1 1 d . . .
H35A H 0.1759 -0.3685 0.0660 0.162 Uiso 1 1 calc R . .
H35B H 0.1601 -0.4649 0.1197 0.162 Uiso 1 1 calc R . .
C36 C 0.0227(17) -0.3712(15) 0.1198(9) 0.118(7) Uani 1 1 d . . .
H36A H -0.0156 -0.4270 0.0308 0.142 Uiso 1 1 calc R . .
H36B H 0.0099 -0.2841 0.1396 0.142 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Ge2 Ge1 Ge3 65.39(3) . . ?
Ge2 Ge1 Ge4 64.88(3) . . ?
Ge3 Ge1 Ge4 64.84(3) . . ?
Ge2 Ge1 Ge5 146.06(3) . 1_655 ?
Ge3 Ge1 Ge5 146.94(2) . 1_655 ?
Ge4 Ge1 Ge5 128.04(3) . 1_655 ?
Ge1 Ge2 Ge5 103.26(3) . . ?
Ge1 Ge2 Ge4 57.77(3) . . ?
Ge5 Ge2 Ge4 57.30(3) . . ?
Ge1 Ge2 Ge3 57.40(3) . . ?
Ge5 Ge2 Ge3 57.34(3) . . ?
Ge4 Ge2 Ge3 59.85(3) . . ?
Ge5 Ge3 Ge1 103.09(3) . . ?
Ge5 Ge3 Ge4 57.27(3) . . ?
Ge1 Ge3 Ge4 57.70(3) . . ?
Ge5 Ge3 Ge2 57.33(3) . . ?
Ge1 Ge3 Ge2 57.21(3) . . ?
Ge4 Ge3 Ge2 59.79(3) . . ?
Ge5 Ge4 Ge1 103.19(4) . . ?
Ge5 Ge4 Ge2 57.64(3) . . ?
Ge1 Ge4 Ge2 57.35(3) . . ?
Ge5 Ge4 Ge3 57.64(3) . . ?
Ge1 Ge4 Ge3 57.46(3) . . ?
Ge2 Ge4 Ge3 60.36(3) . . ?
Ge4 Ge5 Ge2 65.06(3) . . ?
Ge4 Ge5 Ge3 65.09(3) . . ?
Ge2 Ge5 Ge3 65.33(3) . . ?
O5 K1 O1 95.42(13) . . ?
O5 K1 O3 97.25(17) . . ?
O1 K1 O3 100.80(15) . . ?
O5 K1 O6 60.65(14) . . ?
O1 K1 O6 115.62(16) . . ?
O3 K1 O6 137.96(16) . . ?
O5 K1 O2 134.63(14) . . ?
O1 K1 O2 59.78(14) . . ?
O3 K1 O2 122.92(16) . . ?
O6 K1 O2 94.43(15) . . ?
O5 K1 O4 118.33(14) . . ?
O1 K1 O4 141.00(14) . . ?
O3 K1 O4 58.56(18) . . ?
O6 K1 O4 98.66(17) . . ?
O2 K1 O4 101.54(15) . . ?
O5 K1 N2 120.35(15) . . ?
O1 K1 N2 120.05(17) . . ?
O3 K1 N2 118.1(2) . . ?
O6 K1 N2 61.02(16) . . ?
O2 K1 N2 60.97(16) . . ?
O4 K1 N2 60.5(2) . . ?
O5 K1 N1 61.21(14) . . ?
O1 K1 N1 60.15(15) . . ?
O3 K1 N1 60.24(17) . . ?
O6 K1 N1 120.73(15) . . ?
O2 K1 N1 118.88(15) . . ?
O4 K1 N1 118.02(18) . . ?
N2 K1 N1 178.14(18) . . ?
O10 K2 O12 98.73(14) . . ?
O10 K2 O8 98.27(17) . . ?
O12 K2 O8 97.72(14) . . ?
O10 K2 O7 144.47(18) . . ?
O12 K2 O7 111.67(19) . . ?
O8 K2 O7 60.83(14) . . ?
O10 K2 O11 111.72(19) . . ?
O12 K2 O11 61.15(13) . . ?
O8 K2 O11 144.96(15) . . ?
O7 K2 O11 99.18(15) . . ?
O10 K2 O9 61.20(18) . . ?
O12 K2 O9 147.8(2) . . ?
O8 K2 O9 109.38(18) . . ?
O7 K2 O9 96.9(2) . . ?
O11 K2 O9 100.97(18) . . ?
O10 K2 N3 118.51(19) . . ?
O12 K2 N3 119.41(14) . . ?
O8 K2 N3 119.64(15) . . ?
O7 K2 N3 61.77(18) . . ?
O11 K2 N3 61.25(14) . . ?
O9 K2 N3 61.30(17) . . ?
O10 K2 N4 60.49(18) . . ?
O12 K2 N4 60.93(13) . . ?
O8 K2 N4 61.04(14) . . ?
O7 K2 N4 119.12(17) . . ?
O11 K2 N4 118.73(14) . . ?
O9 K2 N4 117.86(16) . . ?
N3 K2 N4 178.98(19) . . ?
O10 K2 C35 41.9(4) . . ?
O12 K2 C35 126.8(3) . . ?
O8 K2 C35 118.1(3) . . ?
O7 K2 C35 119.7(4) . . ?
O11 K2 C35 96.7(3) . . ?
O9 K2 C35 22.8(3) . . ?
N3 K2 C35 76.9(4) . . ?
N4 K2 C35 102.1(4) . . ?
O10 K2 C18 120.67(18) . . ?
O12 K2 C18 42.70(15) . . ?
O8 K2 C18 124.37(16) . . ?
O7 K2 C18 94.55(19) . . ?
O11 K2 C18 22.43(17) . . ?
O9 K2 C18 123.39(19) . . ?
N3 K2 C18 76.77(17) . . ?
N4 K2 C18 103.52(17) . . ?
C35 K2 C18 117.4(3) . . ?
C18 O11 C31 108.7(8) . . ?
C18 O11 K2 107.9(4) . . ?
C31 O11 K2 117.2(4) . . ?
C13 O8 C20 111.1(5) . . ?
C13 O8 K2 116.3(4) . . ?
C20 O8 K2 119.9(4) . . ?
C22 O5 C5 111.2(5) . . ?
C22 O5 K1 118.8(3) . . ?
C5 O5 K1 115.7(4) . . ?
C3 O12 C7 110.8(5) . . ?
C3 O12 K2 119.5(3) . . ?
C7 O12 K2 116.7(4) . . ?
C32 O2 C16 112.7(6) . . ?
C32 O2 K1 117.2(4) . . ?
C16 O2 K1 111.1(4) . . ?
C27 O9 C35 111.2(16) . . ?
C27 O9 K2 115.6(5) . . ?
C35 O9 K2 106.0(6) . . ?
C33 O10 C36 111.5(9) . . ?
C33 O10 K2 121.6(5) . . ?
C36 O10 K2 114.4(6) . . ?
C29 O1 C12 110.8(5) . . ?
C29 O1 K1 118.2(4) . . ?
C12 O1 K1 117.8(4) . . ?
C2 O6 C9 110.0(5) . . ?
C2 O6 K1 112.9(4) . . ?
C9 O6 K1 114.8(4) . . ?
C28 O3 C24 110.0(7) . . ?
C28 O3 K1 118.8(5) . . ?
C24 O3 K1 120.4(4) . . ?
C14 O7 C26 102.7(7) . . ?
C14 O7 K2 110.4(4) . . ?
C26 O7 K2 113.5(5) . . ?
C21 O4 C10 109.6(7) . . ?
C21 O4 K1 116.6(5) . . ?
C10 O4 K1 113.4(4) . . ?
C11 N1 C6 110.5(6) . . ?
C11 N1 C4 109.6(5) . . ?
C6 N1 C4 109.2(6) . . ?
C11 N1 K1 109.2(5) . . ?
C6 N1 K1 107.7(4) . . ?
C4 N1 K1 110.6(4) . . ?
C15 N3 C23 110.4(7) . . ?
C15 N3 C19 110.2(10) . . ?
C23 N3 C19 109.6(10) . . ?
C15 N3 K2 108.1(5) . . ?
C23 N3 K2 109.8(5) . . ?
C19 N3 K2 108.7(4) . . ?
C1 N4 C8 110.7(5) . . ?
C1 N4 C17 110.6(5) . . ?
C8 N4 C17 109.3(6) . . ?
C1 N4 K2 109.0(5) . . ?
C8 N4 K2 108.8(3) . . ?
C17 N4 K2 108.4(4) . . ?
C30 N2 C34 108.7(7) . . ?
C30 N2 C25 110.2(7) . . ?
C34 N2 C25 109.7(6) . . ?
C30 N2 K1 110.2(5) . . ?
C34 N2 K1 109.1(4) . . ?
C25 N2 K1 109.0(5) . . ?
K1 N5 H5C 109.5 1_545 . ?
K1 N5 H5D 109.5 1_545 . ?
H5C N5 H5D 109.5 . . ?
K1 N5 H5E 109.5 1_545 . ?
H5C N5 H5E 109.5 . . ?
H5D N5 H5E 109.5 . . ?
K1 N6 H6C 109.5 1_544 . ?
K1 N6 H6D 109.5 1_544 . ?
H6C N6 H6D 109.5 . . ?
K1 N6 H6E 109.5 1_544 . ?
H6C N6 H6E 109.5 . . ?
H6D N6 H6E 109.5 . . ?
K1 N7 H7C 109.5 1_544 . ?
K1 N7 H7D 109.5 1_544 . ?
H7C N7 H7D 109.5 . . ?
K1 N7 H7E 109.5 1_544 . ?
H7C N7 H7E 109.5 . . ?
H7D N7 H7E 109.5 . . ?
K1 N8 H8C 109.5 1_544 . ?
K1 N8 H8D 109.5 1_544 . ?
H8C N8 H8D 109.5 . . ?
K1 N8 H8E 109.5 1_544 . ?
H8C N8 H8E 109.5 . . ?
H8D N8 H8E 109.5 . . ?
N4 C1 C33 113.6(6) . . ?
N4 C1 H1A 108.8 . . ?
C33 C1 H1A 108.8 . . ?
N4 C1 H1B 108.8 . . ?
C33 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
O6 C2 C5 110.4(5) . . ?
O6 C2 H2A 109.6 . . ?
C5 C2 H2A 109.6 . . ?
O6 C2 H2B 109.6 . . ?
C5 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
O12 C3 C8 108.6(5) . . ?
O12 C3 H3A 110.0 . . ?
C8 C3 H3A 110.0 . . ?
O12 C3 H3B 110.0 . . ?
C8 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
N1 C4 C29 112.7(6) . . ?
N1 C4 H4A 109.0 . . ?
C29 C4 H4A 109.0 . . ?
N1 C4 H4B 109.0 . . ?
C29 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
O5 C5 C2 109.9(5) . . ?
O5 C5 H5A 109.7 . . ?
C2 C5 H5A 109.7 . . ?
O5 C5 H5B 109.7 . . ?
C2 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
N1 C6 C22 114.4(6) . . ?
N1 C6 H6A 108.7 . . ?
C22 C6 H6A 108.7 . . ?
N1 C6 H6B 108.7 . . ?
C22 C6 H6B 108.7 . . ?
H6A C6 H6B 107.6 . . ?
O12 C7 C18 109.6(6) . . ?
O12 C7 H7A 109.8 . . ?
C18 C7 H7A 109.8 . . ?
O12 C7 H7B 109.8 . . ?
C18 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
N4 C8 C3 112.7(6) . . ?
N4 C8 H8A 109.1 . . ?
C3 C8 H8A 109.1 . . ?
N4 C8 H8B 109.1 . . ?
C3 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
O6 C9 C30 108.6(7) . . ?
O6 C9 H9A 110.0 . . ?
C30 C9 H9A 110.0 . . ?
O6 C9 H9B 110.0 . . ?
C30 C9 H9B 110.0 . . ?
H9A C9 H9B 108.3 . . ?
C28 C10 O4 110.6(6) . . ?
C28 C10 H10A 109.5 . . ?
O4 C10 H10A 109.5 . . ?
C28 C10 H10B 109.5 . . ?
O4 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
N1 C11 C24 115.1(6) . . ?
N1 C11 H11A 108.5 . . ?
C24 C11 H11A 108.5 . . ?
N1 C11 H11B 108.5 . . ?
C24 C11 H11B 108.5 . . ?
H11A C11 H11B 107.5 . . ?
O1 C12 C16 108.8(5) . . ?
O1 C12 H12A 109.9 . . ?
C16 C12 H12A 109.9 . . ?
O1 C12 H12B 109.9 . . ?
C16 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
O8 C13 C14 109.9(6) . . ?
O8 C13 H13A 109.7 . . ?
C14 C13 H13A 109.7 . . ?
O8 C13 H13B 109.7 . . ?
C14 C13 H13B 109.7 . . ?
H13A C13 H13B 108.2 . . ?
O7 C14 C13 109.8(5) . . ?
O7 C14 H14A 109.7 . . ?
C13 C14 H14A 109.7 . . ?
O7 C14 H14B 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
C26 C15 N3 121.5(7) . . ?
C26 C15 H15A 106.9 . . ?
N3 C15 H15A 106.9 . . ?
C26 C15 H15B 106.9 . . ?
N3 C15 H15B 106.9 . . ?
H15A C15 H15B 106.7 . . ?
O2 C16 C12 110.3(6) . . ?
O2 C16 H16A 109.6 . . ?
C12 C16 H16A 109.6 . . ?
O2 C16 H16B 109.6 . . ?
C12 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
N4 C17 C20 114.6(5) . . ?
N4 C17 H17A 108.6 . . ?
C20 C17 H17A 108.6 . . ?
N4 C17 H17B 108.6 . . ?
C20 C17 H17B 108.6 . . ?
H17A C17 H17B 107.6 . . ?
O11 C18 C7 109.2(5) . . ?
O11 C18 K2 49.6(3) . . ?
C7 C18 K2 82.6(3) . . ?
O11 C18 H18A 109.8 . . ?
C7 C18 H18A 109.8 . . ?
K2 C18 H18A 81.4 . . ?
O11 C18 H18B 109.8 . . ?
C7 C18 H18B 109.8 . . ?
K2 C18 H18B 159.4 . . ?
H18A C18 H18B 108.3 . . ?
C31 C19 N3 126.8(9) . . ?
C31 C19 H19A 105.6 . . ?
N3 C19 H19A 105.6 . . ?
C31 C19 H19B 105.6 . . ?
N3 C19 H19B 105.6 . . ?
H19A C19 H19B 106.1 . . ?
O8 C20 C17 108.5(7) . . ?
O8 C20 H20A 110.0 . . ?
C17 C20 H20A 110.0 . . ?
O8 C20 H20B 110.0 . . ?
C17 C20 H20B 110.0 . . ?
H20A C20 H20B 108.4 . . ?
O4 C21 C25 107.9(6) . . ?
O4 C21 H21A 110.1 . . ?
C25 C21 H21A 110.1 . . ?
O4 C21 H21B 110.1 . . ?
C25 C21 H21B 110.1 . . ?
H21A C21 H21B 108.4 . . ?
O5 C22 C6 109.8(6) . . ?
O5 C22 H22A 109.7 . . ?
C6 C22 H22A 109.7 . . ?
O5 C22 H22B 109.7 . . ?
C6 C22 H22B 109.7 . . ?
H22A C22 H22B 108.2 . . ?
C27 C23 N3 125.7(8) . . ?
C27 C23 H23A 105.9 . . ?
N3 C23 H23A 105.9 . . ?
C27 C23 H23B 105.9 . . ?
N3 C23 H23B 105.9 . . ?
H23A C23 H23B 106.2 . . ?
O3 C24 C11 108.7(7) . . ?
O3 C24 H24A 110.0 . . ?
C11 C24 H24A 110.0 . . ?
O3 C24 H24B 110.0 . . ?
C11 C24 H24B 110.0 . . ?
H24A C24 H24B 108.3 . . ?
N2 C25 C21 116.1(7) . . ?
N2 C25 H25A 108.3 . . ?
C21 C25 H25A 108.3 . . ?
N2 C25 H25B 108.3 . . ?
C21 C25 H25B 108.3 . . ?
H25A C25 H25B 107.4 . . ?
C15 C26 O7 111.0(8) . . ?
C15 C26 H26A 109.4 . . ?
O7 C26 H26A 109.4 . . ?
C15 C26 H26B 109.4 . . ?
O7 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
C23 C27 O9 125.3(11) . . ?
C23 C27 H27A 106.0 . . ?
O9 C27 H27A 106.0 . . ?
C23 C27 H27B 106.0 . . ?
O9 C27 H27B 106.0 . . ?
H27A C27 H27B 106.3 . . ?
O3 C28 C10 109.3(8) . . ?
O3 C28 H28A 109.8 . . ?
C10 C28 H28A 109.8 . . ?
O3 C28 H28B 109.8 . . ?
C10 C28 H28B 109.8 . . ?
H28A C28 H28B 108.3 . . ?
O1 C29 C4 108.9(5) . . ?
O1 C29 H29A 109.9 . . ?
C4 C29 H29A 109.9 . . ?
O1 C29 H29B 109.9 . . ?
C4 C29 H29B 109.9 . . ?
H29A C29 H29B 108.3 . . ?
N2 C30 C9 113.4(8) . . ?
N2 C30 H30A 108.9 . . ?
C9 C30 H30A 108.9 . . ?
N2 C30 H30B 108.9 . . ?
C9 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
C19 C31 O11 119.9(9) . . ?
C19 C31 H31A 107.3 . . ?
O11 C31 H31A 107.3 . . ?
C19 C31 H31B 107.3 . . ?
O11 C31 H31B 107.3 . . ?
H31A C31 H31B 106.9 . . ?
O2 C32 C34 110.6(7) . . ?
O2 C32 H32A 109.5 . . ?
C34 C32 H32A 109.5 . . ?
O2 C32 H32B 109.5 . . ?
C34 C32 H32B 109.5 . . ?
H32A C32 H32B 108.1 . . ?
O10 C33 C1 109.5(5) . . ?
O10 C33 H33A 109.8 . . ?
C1 C33 H33A 109.8 . . ?
O10 C33 H33B 109.8 . . ?
C1 C33 H33B 109.8 . . ?
H33A C33 H33B 108.2 . . ?
N2 C34 C32 114.0(6) . . ?
N2 C34 H34A 108.7 . . ?
C32 C34 H34A 108.7 . . ?
N2 C34 H34B 108.7 . . ?
C32 C34 H34B 108.7 . . ?
H34A C34 H34B 107.6 . . ?
C36 C35 O9 109.7(11) . . ?
C36 C35 K2 80.4(6) . . ?
O9 C35 K2 51.1(4) . . ?
C36 C35 H35A 109.7 . . ?
O9 C35 H35A 109.7 . . ?
K2 C35 H35A 160.9 . . ?
C36 C35 H35B 109.7 . . ?
O9 C35 H35B 109.7 . . ?
K2 C35 H35B 82.2 . . ?
H35A C35 H35B 108.2 . . ?
C35 C36 O10 114.5(12) . . ?
C35 C36 H36A 108.6 . . ?
O10 C36 H36A 108.6 . . ?
C35 C36 H36B 108.6 . . ?
O10 C36 H36B 108.6 . . ?
H36A C36 H36B 107.6 . . ?
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 Ge2 2.5000(9) . ?
Ge1 Ge3 2.5053(11) . ?
Ge1 Ge4 2.5119(10) . ?
Ge1 Ge5 7.4385(11) 1_655 ?
Ge2 Ge5 2.5046(10) . ?
Ge2 Ge4 2.6885(11) . ?
Ge2 Ge3 2.7039(9) . ?
Ge3 Ge5 2.5051(9) . ?
Ge3 Ge4 2.6899(11) . ?
Ge4 Ge5 2.4950(11) . ?
K1 O5 2.791(4) . ?
K1 O1 2.817(4) . ?
K1 O3 2.818(6) . ?
K1 O6 2.851(4) . ?
K1 O2 2.875(5) . ?
K1 O4 2.902(5) . ?
K1 N2 2.990(7) . ?
K1 N1 2.994(6) . ?
K2 O10 2.735(5) . ?
K2 O12 2.769(4) . ?
K2 O8 2.780(5) . ?
K2 O7 2.793(5) . ?
K2 O11 2.821(4) . ?
K2 O9 2.852(6) . ?
K2 N3 2.955(6) . ?
K2 N4 2.988(6) . ?
K2 C35 3.521(13) . ?
K2 C18 3.523(7) . ?
O11 C18 1.413(9) . ?
O11 C31 1.424(9) . ?
O8 C13 1.429(8) . ?
O8 C20 1.434(9) . ?
O5 C22 1.422(8) . ?
O5 C5 1.437(8) . ?
O12 C3 1.419(8) . ?
O12 C7 1.434(7) . ?
O2 C32 1.414(9) . ?
O2 C16 1.432(9) . ?
O9 C27 1.377(13) . ?
O9 C35 1.42(2) . ?
O10 C33 1.408(12) . ?
O10 C36 1.415(12) . ?
O1 C29 1.432(9) . ?
O1 C12 1.435(8) . ?
O6 C2 1.434(8) . ?
O6 C9 1.456(11) . ?
O3 C28 1.426(9) . ?
O3 C24 1.433(12) . ?
O7 C14 1.421(9) . ?
O7 C26 1.523(13) . ?
O4 C21 1.403(11) . ?
O4 C10 1.450(11) . ?
N1 C11 1.461(10) . ?
N1 C6 1.483(9) . ?
N1 C4 1.484(8) . ?
N3 C15 1.438(11) . ?
N3 C23 1.457(11) . ?
N3 C19 1.458(9) . ?
N4 C1 1.469(9) . ?
N4 C8 1.481(9) . ?
N4 C17 1.481(9) . ?
N2 C30 1.473(11) . ?
N2 C34 1.488(9) . ?
N2 C25 1.503(12) . ?
N5 K1 6.743(8) 1_545 ?
N5 H5C 0.8900 . ?
N5 H5D 0.8900 . ?
N5 H5E 0.8900 . ?
N6 K1 6.673(12) 1_544 ?
N6 H6C 0.8900 . ?
N6 H6D 0.8900 . ?
N6 H6E 0.8900 . ?
N7 K1 6.950(8) 1_544 ?
N7 H7C 0.8900 . ?
N7 H7D 0.8900 . ?
N7 H7E 0.8900 . ?
N8 K1 5.533(13) 1_544 ?
N8 H8C 0.8900 . ?
N8 H8D 0.8900 . ?
N8 H8E 0.8900 . ?
C1 C33 1.512(13) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C5 1.478(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C8 1.533(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C29 1.511(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C22 1.502(11) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C18 1.498(10) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C30 1.518(11) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C28 1.446(15) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C24 1.511(12) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C16 1.484(12) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.467(10) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C26 1.338(15) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C20 1.514(10) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C31 1.283(14) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C25 1.509(15) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C27 1.287(18) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C34 1.521(12) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.38(3) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
