# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_KM-667
_database_code_depnum_ccdc_archive 'CCDC 1982121'
loop_
_audit_author_name
_audit_author_address
'Wilhelm Klein'
;Technische Universitaet Muenchen
Germany
;
_audit_update_record             
;
2020-02-05 deposited with the CCDC.	2020-04-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         '2(C18 H36 K N2 O6), C4 H10 Ge4 Zn2, 2(H3 N)'
_chemical_formula_sum            'C40 H88 Ge4 K2 N6 O12 Zn2'
_chemical_formula_weight         1344.46

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.8593(6)
_cell_length_b                   14.5737(7)
_cell_length_c                   18.8970(10)
_cell_angle_alpha                80.335(4)
_cell_angle_beta                 74.598(4)
_cell_angle_gamma                69.591(4)
_cell_volume                     2940.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    79638
_cell_measurement_theta_min      1.61
_cell_measurement_theta_max      38.46

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    3.017
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            85499
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.940
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11531
_reflns_number_gt                9084
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_computing_data_collection       'STOE X-AREA 1.76'
_computing_cell_refinement       'STOE X-AREA 1.76'
_computing_data_reduction        'STOE X-AREA 1.76'
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  SHELXL-2014/7
_computing_molecular_graphics    'DIAMOND 3.2k'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0328P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11531
_refine_ls_number_parameters     616
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0259
_refine_ls_wR_factor_ref         0.0571
_refine_ls_wR_factor_gt          0.0527
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_restrained_S_all      0.965
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.64135(2) 0.11771(2) 0.29571(2) 0.01819(6) Uani 1 1 d . . . . .
Ge2 Ge 0.56443(2) 0.30385(2) 0.20677(2) 0.01993(6) Uani 1 1 d . . . . .
Ge3 Ge 0.79159(2) 0.19066(2) 0.19672(2) 0.01863(6) Uani 1 1 d . . . . .
Ge4 Ge 0.68369(2) 0.27606(2) 0.31015(2) 0.02175(6) Uani 1 1 d . . . . .
Zn1 Zn 0.61523(3) 0.13556(2) 0.16571(2) 0.02118(7) Uani 1 1 d . . . . .
C1 C 0.5923(2) 0.06614(17) 0.08994(14) 0.0217(5) Uani 1 1 d . . . . .
H1A H 0.6706 0.0469 0.0523 0.026 Uiso 1 1 calc R U . . .
H1B H 0.5754 0.0051 0.1142 0.026 Uiso 1 1 calc R U . . .
C2 C 0.4883(2) 0.1265(2) 0.05106(15) 0.0284(6) Uani 1 1 d . . . . .
H2A H 0.5057 0.1858 0.0250 0.043 Uiso 1 1 calc R U . . .
H2B H 0.4099 0.1452 0.0876 0.043 Uiso 1 1 calc R U . . .
H2C H 0.4826 0.0871 0.0157 0.043 Uiso 1 1 calc R U . . .
Zn2 Zn 0.45526(3) 0.26459(2) 0.33577(2) 0.02315(7) Uani 1 1 d . . . . .
C3 C 0.2876(3) 0.2938(2) 0.40353(17) 0.0366(7) Uani 1 1 d . . . . .
H3A H 0.2502 0.3661 0.4036 0.044 Uiso 1 1 calc R U . . .
H3B H 0.2358 0.2700 0.3825 0.044 Uiso 1 1 calc R U . . .
C4 C 0.2800(4) 0.2509(4) 0.48337(19) 0.0787(16) Uani 1 1 d . . . . .
H4A H 0.3180 0.2824 0.5080 0.118 Uiso 1 1 calc R U . . .
H4B H 0.3239 0.1800 0.4846 0.118 Uiso 1 1 calc R U . . .
H4C H 0.1933 0.2625 0.5087 0.118 Uiso 1 1 calc R U . . .
K1 K 0.01917(4) 0.62237(3) 0.14064(3) 0.01504(10) Uani 1 1 d . . . . .
N1 N 0.06737(18) 0.41040(14) 0.19521(11) 0.0208(4) Uani 1 1 d . . . . .
N2 N -0.02677(18) 0.83162(14) 0.08645(11) 0.0196(4) Uani 1 1 d . . . . .
O1 O 0.24273(14) 0.48354(11) 0.07982(9) 0.0185(3) Uani 1 1 d . . . . .
O2 O 0.22151(15) 0.68410(12) 0.05500(9) 0.0198(3) Uani 1 1 d . . . . .
O3 O -0.15080(15) 0.70924(11) 0.04761(9) 0.0207(4) Uani 1 1 d . . . . .
O4 O -0.14330(15) 0.52741(11) 0.13141(9) 0.0214(4) Uani 1 1 d . . . . .
O5 O 0.00413(16) 0.56722(12) 0.29316(9) 0.0254(4) Uani 1 1 d . . . . .
O6 O -0.09355(17) 0.76590(12) 0.24237(10) 0.0254(4) Uani 1 1 d . . . . .
C5 C 0.1731(2) 0.35020(17) 0.14342(15) 0.0266(6) Uani 1 1 d . . . . .
H5A H 0.1452 0.3460 0.0995 0.032 Uiso 1 1 calc R U . . .
H5B H 0.2012 0.2828 0.1671 0.032 Uiso 1 1 calc R U . . .
C6 C 0.2811(2) 0.38893(18) 0.11873(15) 0.0257(6) Uani 1 1 d . . . . .
H6A H 0.3099 0.3943 0.1620 0.031 Uiso 1 1 calc R U . . .
H6B H 0.3502 0.3434 0.0862 0.031 Uiso 1 1 calc R U . . .
C7 C 0.3463(2) 0.51556(18) 0.04562(14) 0.0226(5) Uani 1 1 d . . . . .
H7A H 0.4063 0.4676 0.0111 0.027 Uiso 1 1 calc R U . . .
H7B H 0.3876 0.5199 0.0835 0.027 Uiso 1 1 calc R U . . .
C8 C 0.3044(2) 0.61467(19) 0.00436(14) 0.0234(5) Uani 1 1 d . . . . .
H8A H 0.3767 0.6361 -0.0210 0.028 Uiso 1 1 calc R U . . .
H8B H 0.2625 0.6105 -0.0333 0.028 Uiso 1 1 calc R U . . .
C9 C 0.1950(2) 0.78091(18) 0.01826(15) 0.0254(6) Uani 1 1 d . . . . .
H9A H 0.1709 0.7811 -0.0281 0.030 Uiso 1 1 calc R U . . .
H9B H 0.2696 0.8016 0.0058 0.030 Uiso 1 1 calc R U . . .
C10 C 0.0912(2) 0.85164(17) 0.06793(15) 0.0243(5) Uani 1 1 d . . . . .
H10A H 0.1165 0.8497 0.1142 0.029 Uiso 1 1 calc R U . . .
H10B H 0.0786 0.9190 0.0436 0.029 Uiso 1 1 calc R U . . .
C11 C -0.0780(2) 0.84883(18) 0.02083(15) 0.0253(6) Uani 1 1 d . . . . .
H11A H -0.0122 0.8153 -0.0199 0.030 Uiso 1 1 calc R U . . .
H11B H -0.1031 0.9201 0.0057 0.030 Uiso 1 1 calc R U . . .
C12 C -0.1874(2) 0.81374(17) 0.03146(16) 0.0270(6) Uani 1 1 d . . . . .
H12A H -0.2537 0.8459 0.0725 0.032 Uiso 1 1 calc R U . . .
H12B H -0.2200 0.8316 -0.0138 0.032 Uiso 1 1 calc R U . . .
C13 C -0.2560(2) 0.67657(18) 0.07226(16) 0.0263(6) Uani 1 1 d . . . . .
H13A H -0.3112 0.7039 0.0374 0.032 Uiso 1 1 calc R U . . .
H13B H -0.3026 0.7001 0.1212 0.032 Uiso 1 1 calc R U . . .
C14 C -0.2152(3) 0.56648(19) 0.07731(16) 0.0278(6) Uani 1 1 d . . . . .
H14A H -0.2883 0.5438 0.0908 0.033 Uiso 1 1 calc R U . . .
H14B H -0.1656 0.5428 0.0289 0.033 Uiso 1 1 calc R U . . .
C15 C -0.1024(2) 0.42197(17) 0.13608(16) 0.0268(6) Uani 1 1 d . . . . .
H15A H -0.0423 0.3983 0.0902 0.032 Uiso 1 1 calc R U . . .
H15B H -0.1735 0.3984 0.1422 0.032 Uiso 1 1 calc R U . . .
C16 C -0.0430(2) 0.38238(18) 0.20058(16) 0.0270(6) Uani 1 1 d . . . . .
H16A H -0.1044 0.4064 0.2460 0.032 Uiso 1 1 calc R U . . .
H16B H -0.0194 0.3098 0.2051 0.032 Uiso 1 1 calc R U . . .
C17 C 0.0961(2) 0.39728(18) 0.26810(14) 0.0262(6) Uani 1 1 d . . . . .
H17A H 0.1790 0.4032 0.2616 0.031 Uiso 1 1 calc R U . . .
H17B H 0.0996 0.3300 0.2901 0.031 Uiso 1 1 calc R U . . .
C18 C 0.0048(3) 0.46964(19) 0.32089(15) 0.0292(6) Uani 1 1 d . . . . .
H18A H -0.0787 0.4648 0.3277 0.035 Uiso 1 1 calc R U . . .
H18B H 0.0272 0.4540 0.3694 0.035 Uiso 1 1 calc R U . . .
C19 C -0.0906(3) 0.6371(2) 0.33906(15) 0.0344(7) Uani 1 1 d . . . . .
H19A H -0.0845 0.6183 0.3911 0.041 Uiso 1 1 calc R U . . .
H19B H -0.1725 0.6382 0.3350 0.041 Uiso 1 1 calc R U . . .
C20 C -0.0773(3) 0.7373(2) 0.31595(15) 0.0364(7) Uani 1 1 d . . . . .
H20A H -0.1399 0.7853 0.3495 0.044 Uiso 1 1 calc R U . . .
H20B H 0.0056 0.7359 0.3186 0.044 Uiso 1 1 calc R U . . .
C21 C -0.0852(3) 0.86287(18) 0.21955(15) 0.0280(6) Uani 1 1 d . . . . .
H21A H -0.0011 0.8630 0.2179 0.034 Uiso 1 1 calc R U . . .
H21B H -0.1447 0.9095 0.2552 0.034 Uiso 1 1 calc R U . . .
C22 C -0.1134(2) 0.89417(17) 0.14440(15) 0.0279(6) Uani 1 1 d . . . . .
H22A H -0.1978 0.8939 0.1472 0.033 Uiso 1 1 calc R U . . .
H22B H -0.1123 0.9625 0.1302 0.033 Uiso 1 1 calc R U . . .
K2 K 0.24912(4) 0.82036(4) 0.35149(3) 0.01732(10) Uani 1 1 d . . . . .
N3 N 0.21751(19) 1.01536(14) 0.26097(12) 0.0220(4) Uani 1 1 d . . . . .
N4 N 0.28249(19) 0.62715(15) 0.44621(12) 0.0240(5) Uani 1 1 d . . . . .
O7 O 0.28677(16) 0.82518(12) 0.19576(9) 0.0239(4) Uani 1 1 d . . . . .
O8 O 0.34593(16) 0.64392(12) 0.28499(9) 0.0248(4) Uani 1 1 d . . . . .
O9 O 0.04309(16) 0.78694(12) 0.45891(9) 0.0256(4) Uani 1 1 d . . . . .
O10 O 0.02687(14) 0.97520(12) 0.38478(10) 0.0231(4) Uani 1 1 d . . . . .
O11 O 0.3647(2) 0.94323(14) 0.37093(13) 0.0453(6) Uani 1 1 d . . . . .
C23 C 0.2188(3) 1.0016(2) 0.18556(15) 0.0303(6) Uani 1 1 d . . . . .
H23A H 0.2326 1.0592 0.1528 0.036 Uiso 1 1 calc R U . . .
H23B H 0.1367 0.9997 0.1844 0.036 Uiso 1 1 calc R U . . .
C24 C 0.3159(3) 0.9097(2) 0.15534(14) 0.0308(6) Uani 1 1 d . . . . .
H24A H 0.3185 0.9096 0.1025 0.037 Uiso 1 1 calc R U . . .
H24B H 0.3980 0.9077 0.1598 0.037 Uiso 1 1 calc R U . . .
C25 C 0.3766(3) 0.7362(2) 0.16916(14) 0.0297(6) Uani 1 1 d . . . . .
H25A H 0.4583 0.7311 0.1764 0.036 Uiso 1 1 calc R U . . .
H25B H 0.3833 0.7361 0.1158 0.036 Uiso 1 1 calc R U . . .
C26 C 0.3388(3) 0.6503(2) 0.21022(14) 0.0310(6) Uani 1 1 d . . . . .
H26A H 0.2533 0.6590 0.2077 0.037 Uiso 1 1 calc R U . . .
H26B H 0.3940 0.5891 0.1877 0.037 Uiso 1 1 calc R U . . .
C27 C 0.3173(3) 0.55984(18) 0.32636(15) 0.0267(6) Uani 1 1 d . . . . .
H27A H 0.3637 0.5008 0.2989 0.032 Uiso 1 1 calc R U . . .
H27B H 0.2280 0.5701 0.3343 0.032 Uiso 1 1 calc R U . . .
C28 C 0.3525(2) 0.54552(18) 0.39934(15) 0.0266(6) Uani 1 1 d . . . . .
H28A H 0.3395 0.4843 0.4262 0.032 Uiso 1 1 calc R U . . .
H28B H 0.4416 0.5371 0.3902 0.032 Uiso 1 1 calc R U . . .
C29 C 0.1600(3) 0.61861(19) 0.48240(17) 0.0352(7) Uani 1 1 d . . . . .
H29A H 0.1694 0.5635 0.5213 0.042 Uiso 1 1 calc R U . . .
H29B H 0.1252 0.6025 0.4457 0.042 Uiso 1 1 calc R U . . .
C30 C 0.0698(3) 0.7113(2) 0.51657(16) 0.0392(7) Uani 1 1 d . . . . .
H30A H -0.0071 0.6988 0.5454 0.047 Uiso 1 1 calc R U . . .
H30B H 0.1063 0.7317 0.5502 0.047 Uiso 1 1 calc R U . . .
C31 C -0.0415(2) 0.87577(19) 0.48854(15) 0.0286(6) Uani 1 1 d . . . . .
H31A H -0.0024 0.9011 0.5177 0.034 Uiso 1 1 calc R U . . .
H31B H -0.1156 0.8629 0.5215 0.034 Uiso 1 1 calc R U . . .
C32 C -0.0781(2) 0.95010(19) 0.42716(16) 0.0297(6) Uani 1 1 d . . . . .
H32A H -0.1113 0.9229 0.3956 0.036 Uiso 1 1 calc R U . . .
H32B H -0.1433 1.0095 0.4474 0.036 Uiso 1 1 calc R U . . .
C33 C -0.0038(2) 1.04579(18) 0.32451(16) 0.0276(6) Uani 1 1 d . . . . .
H33A H -0.0815 1.0987 0.3419 0.033 Uiso 1 1 calc R U . . .
H33B H -0.0160 1.0138 0.2861 0.033 Uiso 1 1 calc R U . . .
C34 C 0.0994(2) 1.08816(18) 0.29308(16) 0.0273(6) Uani 1 1 d . . . . .
H34A H 0.0750 1.1412 0.2545 0.033 Uiso 1 1 calc R U . . .
H34B H 0.1120 1.1180 0.3325 0.033 Uiso 1 1 calc R U . . .
C35 C 0.3227(2) 1.04595(19) 0.26265(15) 0.0271(6) Uani 1 1 d . . . . .
H35A H 0.3089 1.1143 0.2402 0.033 Uiso 1 1 calc R U . . .
H35B H 0.3984 1.0037 0.2319 0.033 Uiso 1 1 calc R U . . .
C36 C 0.3439(2) 1.04081(18) 0.33824(15) 0.0254(6) Uani 1 1 d . . . . .
H36A H 0.4164 1.0616 0.3349 0.030 Uiso 1 1 calc R U . . .
H36B H 0.2710 1.0857 0.3690 0.030 Uiso 1 1 calc R U . . .
C37A C 0.4081(3) 0.9272(2) 0.43621(15) 0.0279(6) Uani 0.559(10) 1 d . . P A 1
H37A H 0.3625 0.9835 0.4667 0.033 Uiso 0.559(10) 1 calc R U P A 1
H37B H 0.4970 0.9204 0.4240 0.033 Uiso 0.559(10) 1 calc R U P A 1
C38A C 0.3873(5) 0.8314(4) 0.4792(3) 0.0214(15) Uani 0.559(10) 1 d . . P A 1
H38A H 0.4240 0.8141 0.5230 0.026 Uiso 0.559(10) 1 calc R U P A 1
H38B H 0.2980 0.8400 0.4958 0.026 Uiso 0.559(10) 1 calc R U P A 1
O12A O 0.4455(5) 0.7575(3) 0.4300(3) 0.0222(11) Uani 0.559(10) 1 d . . P A 1
C37B C 0.4081(3) 0.9272(2) 0.43621(15) 0.0279(6) Uani 0.441(10) 1 d . . P A 2
H37C H 0.3374 0.9524 0.4775 0.033 Uiso 0.441(10) 1 calc R U P A 2
H37D H 0.4657 0.9648 0.4304 0.033 Uiso 0.441(10) 1 calc R U P A 2
C38B C 0.4723(7) 0.8215(5) 0.4548(4) 0.032(2) Uani 0.441(10) 1 d . . P A 2
H38C H 0.5480 0.7965 0.4164 0.038 Uiso 0.441(10) 1 calc R U P A 2
H38D H 0.4956 0.8125 0.5027 0.038 Uiso 0.441(10) 1 calc R U P A 2
O12B O 0.3863(7) 0.7700(4) 0.4586(4) 0.0282(16) Uani 0.441(10) 1 d . . P A 2
C39 C 0.4596(3) 0.6627(2) 0.47107(19) 0.0450(9) Uani 1 1 d . . . . .
H39A H 0.4949 0.6627 0.5130 0.054 Uiso 1 1 calc R U . A 1
H39B H 0.5226 0.6132 0.4388 0.054 Uiso 1 1 calc R U . A 1
C40 C 0.3507(3) 0.6260(2) 0.50176(16) 0.0355(7) Uani 1 1 d . . . . .
H40A H 0.3800 0.5580 0.5241 0.043 Uiso 1 1 calc R U . . .
H40B H 0.2931 0.6673 0.5414 0.043 Uiso 1 1 calc R U . . .
N5 N 0.6510(2) 0.55733(19) 0.28661(15) 0.0435(7) Uani 1 1 d . . . . .
H5C H 0.6501 0.4942 0.2942 0.065 Uiso 1 1 d R U . . .
H5D H 0.7067 0.5645 0.2442 0.065 Uiso 1 1 d R U . . .
H5E H 0.5746 0.5988 0.2830 0.065 Uiso 1 1 d R U . . .
N6 N 0.6040(3) 0.8069(3) 0.25359(18) 0.0661(9) Uani 1 1 d . . . . .
H6C H 0.5793 0.8737 0.2478 0.099 Uiso 1 1 d R U . . .
H6D H 0.6839 0.7835 0.2580 0.099 Uiso 1 1 d R U . . .
H6E H 0.5553 0.7871 0.2949 0.099 Uiso 1 1 d R U . . .


_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 Zn1 2.5164(4) . ?
Ge1 Zn2 2.5273(4) . ?
Ge1 Ge3 2.5859(4) . ?
Ge1 Ge4 2.5971(4) . ?
Ge1 Ge2 2.9281(4) . ?
Ge2 Zn2 2.5135(4) . ?
Ge2 Zn1 2.5180(4) . ?
Ge2 Ge3 2.5978(4) . ?
Ge2 Ge4 2.6045(4) . ?
Ge3 Ge4 2.4717(4) . ?
Ge3 Zn1 2.7097(4) . ?
Ge4 Zn2 2.6820(4) . ?
Zn1 C1 2.008(2) . ?
C1 C2 1.531(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
Zn2 C3 2.004(3) . ?
C3 C4 1.525(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
K1 O4 2.7889(17) . ?
K1 O1 2.8044(16) . ?
K1 O6 2.8094(18) . ?
K1 O5 2.8344(18) . ?
K1 O3 2.8482(17) . ?
K1 O2 2.8532(16) . ?
K1 N2 2.9554(19) . ?
K1 N1 2.9909(19) . ?
N1 C17 1.472(3) . ?
N1 C5 1.473(3) . ?
N1 C16 1.476(3) . ?
N2 C10 1.468(3) . ?
N2 C11 1.469(3) . ?
N2 C22 1.473(3) . ?
O1 C7 1.421(3) . ?
O1 C6 1.431(3) . ?
O2 C8 1.428(3) . ?
O2 C9 1.431(3) . ?
O3 C13 1.425(3) . ?
O3 C12 1.433(3) . ?
O4 C14 1.423(3) . ?
O4 C15 1.436(3) . ?
O5 C19 1.426(3) . ?
O5 C18 1.429(3) . ?
O6 C20 1.427(3) . ?
O6 C21 1.437(3) . ?
C5 C6 1.509(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.506(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.512(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.509(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.500(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.500(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.504(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.502(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.505(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
K2 O11 2.724(2) . ?
K2 O12B 2.776(5) . ?
K2 O8 2.7873(18) . ?
K2 O10 2.8076(17) . ?
K2 O7 2.8495(18) . ?
K2 O9 2.8620(17) . ?
K2 O12A 2.890(4) . ?
K2 N3 3.018(2) . ?
K2 N4 3.032(2) . ?
K2 C38A 3.310(5) . ?
N3 C23 1.467(3) . ?
N3 C35 1.473(3) . ?
N3 C34 1.478(3) . ?
N4 C28 1.471(3) . ?
N4 C29 1.471(3) . ?
N4 C40 1.480(4) . ?
O7 C25 1.429(3) . ?
O7 C24 1.435(3) . ?
O8 C26 1.423(3) . ?
O8 C27 1.433(3) . ?
O9 C31 1.427(3) . ?
O9 C30 1.429(3) . ?
O10 C32 1.419(3) . ?
O10 C33 1.433(3) . ?
O11 C37B 1.414(3) . ?
O11 C37A 1.414(3) . ?
O11 C36 1.416(3) . ?
C23 C24 1.510(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.499(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.506(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.517(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.491(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.500(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.500(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37A C38A 1.557(5) . ?
C37A H37A 0.9900 . ?
C37A H37B 0.9900 . ?
C38A O12A 1.407(8) . ?
C38A H38A 0.9900 . ?
C38A H38B 0.9900 . ?
O12A C39 1.445(4) . ?
C37B C38B 1.490(7) . ?
C37B H37C 0.9900 . ?
C37B H37D 0.9900 . ?
C38B O12B 1.444(10) . ?
C38B H38C 0.9900 . ?
C38B H38D 0.9900 . ?
O12B C39 1.515(6) . ?
C39 C40 1.507(5) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
N5 H5C 0.9100 . ?
N5 H5D 0.9100 . ?
N5 H5E 0.9100 . ?
N6 H6C 0.9100 . ?
N6 H6D 0.9100 . ?
N6 H6E 0.9100 . ?

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
Zn1 Ge1 Zn2 94.714(13) . . ?
Zn1 Ge1 Ge3 64.140(11) . . ?
Zn2 Ge1 Ge3 104.558(13) . . ?
Zn1 Ge1 Ge4 105.251(13) . . ?
Zn2 Ge1 Ge4 63.100(11) . . ?
Ge3 Ge1 Ge4 56.962(11) . . ?
Zn1 Ge1 Ge2 54.461(10) . . ?
Zn2 Ge1 Ge2 54.267(10) . . ?
Ge3 Ge1 Ge2 55.800(10) . . ?
Ge4 Ge1 Ge2 55.862(10) . . ?
Zn2 Ge2 Zn1 95.017(13) . . ?
Zn2 Ge2 Ge3 104.609(13) . . ?
Zn1 Ge2 Ge3 63.945(11) . . ?
Zn2 Ge2 Ge4 63.176(11) . . ?
Zn1 Ge2 Ge4 104.984(13) . . ?
Ge3 Ge2 Ge4 56.732(11) . . ?
Zn2 Ge2 Ge1 54.709(10) . . ?
Zn1 Ge2 Ge1 54.409(10) . . ?
Ge3 Ge2 Ge1 55.415(9) . . ?
Ge4 Ge2 Ge1 55.622(10) . . ?
Ge4 Ge3 Ge1 61.747(11) . . ?
Ge4 Ge3 Ge2 61.771(11) . . ?
Ge1 Ge3 Ge2 68.785(11) . . ?
Ge4 Ge3 Zn1 103.221(13) . . ?
Ge1 Ge3 Zn1 56.684(10) . . ?
Ge2 Ge3 Zn1 56.595(10) . . ?
Ge3 Ge4 Ge1 61.291(11) . . ?
Ge3 Ge4 Ge2 61.497(11) . . ?
Ge1 Ge4 Ge2 68.515(11) . . ?
Ge3 Ge4 Zn2 103.335(13) . . ?
Ge1 Ge4 Zn2 57.179(11) . . ?
Ge2 Ge4 Zn2 56.754(11) . . ?
C1 Zn1 Ge1 143.71(7) . . ?
C1 Zn1 Ge2 142.22(7) . . ?
Ge1 Zn1 Ge2 71.130(12) . . ?
C1 Zn1 Ge3 139.92(7) . . ?
Ge1 Zn1 Ge3 59.176(10) . . ?
Ge2 Zn1 Ge3 59.460(11) . . ?
C2 C1 Zn1 114.70(17) . . ?
C2 C1 H1A 108.6 . . ?
Zn1 C1 H1A 108.6 . . ?
C2 C1 H1B 108.6 . . ?
Zn1 C1 H1B 108.6 . . ?
H1A C1 H1B 107.6 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 Zn2 Ge2 142.21(10) . . ?
C3 Zn2 Ge1 139.00(9) . . ?
Ge2 Zn2 Ge1 71.024(11) . . ?
C3 Zn2 Ge4 146.29(9) . . ?
Ge2 Zn2 Ge4 60.070(11) . . ?
Ge1 Zn2 Ge4 59.721(11) . . ?
C4 C3 Zn2 117.5(3) . . ?
C4 C3 H3A 107.9 . . ?
Zn2 C3 H3A 107.9 . . ?
C4 C3 H3B 107.9 . . ?
Zn2 C3 H3B 107.9 . . ?
H3A C3 H3B 107.2 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O4 K1 O1 99.09(5) . . ?
O4 K1 O6 111.29(5) . . ?
O1 K1 O6 144.37(5) . . ?
O4 K1 O5 93.87(5) . . ?
O1 K1 O5 101.00(5) . . ?
O6 K1 O5 60.01(5) . . ?
O4 K1 O3 60.39(5) . . ?
O1 K1 O3 116.48(5) . . ?
O6 K1 O3 95.10(5) . . ?
O5 K1 O3 136.43(5) . . ?
O4 K1 O2 142.14(5) . . ?
O1 K1 O2 59.64(5) . . ?
O6 K1 O2 101.40(5) . . ?
O5 K1 O2 119.46(5) . . ?
O3 K1 O2 99.13(5) . . ?
O4 K1 N2 119.67(5) . . ?
O1 K1 N2 119.09(5) . . ?
O6 K1 N2 60.96(5) . . ?
O5 K1 N2 119.28(6) . . ?
O3 K1 N2 61.16(5) . . ?
O2 K1 N2 61.12(5) . . ?
O4 K1 N1 60.63(5) . . ?
O1 K1 N1 60.59(5) . . ?
O6 K1 N1 119.17(6) . . ?
O5 K1 N1 60.77(6) . . ?
O3 K1 N1 119.08(5) . . ?
O2 K1 N1 118.53(5) . . ?
N2 K1 N1 179.64(6) . . ?
C17 N1 C5 110.02(19) . . ?
C17 N1 C16 110.41(19) . . ?
C5 N1 C16 109.7(2) . . ?
C17 N1 K1 107.93(14) . . ?
C5 N1 K1 109.12(13) . . ?
C16 N1 K1 109.59(13) . . ?
C10 N2 C11 110.68(19) . . ?
C10 N2 C22 109.2(2) . . ?
C11 N2 C22 110.86(19) . . ?
C10 N2 K1 108.25(13) . . ?
C11 N2 K1 107.95(14) . . ?
C22 N2 K1 109.84(14) . . ?
C7 O1 C6 110.32(17) . . ?
C7 O1 K1 118.78(13) . . ?
C6 O1 K1 119.08(13) . . ?
C8 O2 C9 109.67(18) . . ?
C8 O2 K1 112.49(13) . . ?
C9 O2 K1 118.12(13) . . ?
C13 O3 C12 110.79(18) . . ?
C13 O3 K1 110.93(13) . . ?
C12 O3 K1 118.20(14) . . ?
C14 O4 C15 110.19(19) . . ?
C14 O4 K1 117.72(13) . . ?
C15 O4 K1 118.83(13) . . ?
C19 O5 C18 110.57(19) . . ?
C19 O5 K1 113.44(14) . . ?
C18 O5 K1 118.96(15) . . ?
C20 O6 C21 110.4(2) . . ?
C20 O6 K1 117.28(15) . . ?
C21 O6 K1 118.35(14) . . ?
N1 C5 C6 114.2(2) . . ?
N1 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N1 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
O1 C6 C5 108.71(19) . . ?
O1 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
O1 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
O1 C7 C8 109.63(19) . . ?
O1 C7 H7A 109.7 . . ?
C8 C7 H7A 109.7 . . ?
O1 C7 H7B 109.7 . . ?
C8 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
O2 C8 C7 109.3(2) . . ?
O2 C8 H8A 109.8 . . ?
C7 C8 H8A 109.8 . . ?
O2 C8 H8B 109.8 . . ?
C7 C8 H8B 109.8 . . ?
H8A C8 H8B 108.3 . . ?
O2 C9 C10 109.49(19) . . ?
O2 C9 H9A 109.8 . . ?
C10 C9 H9A 109.8 . . ?
O2 C9 H9B 109.8 . . ?
C10 C9 H9B 109.8 . . ?
H9A C9 H9B 108.2 . . ?
N2 C10 C9 114.6(2) . . ?
N2 C10 H10A 108.6 . . ?
C9 C10 H10A 108.6 . . ?
N2 C10 H10B 108.6 . . ?
C9 C10 H10B 108.6 . . ?
H10A C10 H10B 107.6 . . ?
N2 C11 C12 114.4(2) . . ?
N2 C11 H11A 108.7 . . ?
C12 C11 H11A 108.7 . . ?
N2 C11 H11B 108.7 . . ?
C12 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
O3 C12 C11 109.70(19) . . ?
O3 C12 H12A 109.7 . . ?
C11 C12 H12A 109.7 . . ?
O3 C12 H12B 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
O3 C13 C14 109.6(2) . . ?
O3 C13 H13A 109.7 . . ?
C14 C13 H13A 109.7 . . ?
O3 C13 H13B 109.7 . . ?
C14 C13 H13B 109.7 . . ?
H13A C13 H13B 108.2 . . ?
O4 C14 C13 109.7(2) . . ?
O4 C14 H14A 109.7 . . ?
C13 C14 H14A 109.7 . . ?
O4 C14 H14B 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
O4 C15 C16 109.3(2) . . ?
O4 C15 H15A 109.8 . . ?
C16 C15 H15A 109.8 . . ?
O4 C15 H15B 109.8 . . ?
C16 C15 H15B 109.8 . . ?
H15A C15 H15B 108.3 . . ?
N1 C16 C15 113.9(2) . . ?
N1 C16 H16A 108.8 . . ?
C15 C16 H16A 108.8 . . ?
N1 C16 H16B 108.8 . . ?
C15 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
N1 C17 C18 114.2(2) . . ?
N1 C17 H17A 108.7 . . ?
C18 C17 H17A 108.7 . . ?
N1 C17 H17B 108.7 . . ?
C18 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
O5 C18 C17 110.1(2) . . ?
O5 C18 H18A 109.6 . . ?
C17 C18 H18A 109.6 . . ?
O5 C18 H18B 109.6 . . ?
C17 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
O5 C19 C20 109.7(2) . . ?
O5 C19 H19A 109.7 . . ?
C20 C19 H19A 109.7 . . ?
O5 C19 H19B 109.7 . . ?
C20 C19 H19B 109.7 . . ?
H19A C19 H19B 108.2 . . ?
O6 C20 C19 109.1(2) . . ?
O6 C20 H20A 109.9 . . ?
C19 C20 H20A 109.9 . . ?
O6 C20 H20B 109.9 . . ?
C19 C20 H20B 109.9 . . ?
H20A C20 H20B 108.3 . . ?
O6 C21 C22 109.0(2) . . ?
O6 C21 H21A 109.9 . . ?
C22 C21 H21A 109.9 . . ?
O6 C21 H21B 109.9 . . ?
C22 C21 H21B 109.9 . . ?
H21A C21 H21B 108.3 . . ?
N2 C22 C21 114.2(2) . . ?
N2 C22 H22A 108.7 . . ?
C21 C22 H22A 108.7 . . ?
N2 C22 H22B 108.7 . . ?
C21 C22 H22B 108.7 . . ?
H22A C22 H22B 107.6 . . ?
O11 K2 O12B 59.97(13) . . ?
O11 K2 O8 130.07(7) . . ?
O12B K2 O8 98.82(15) . . ?
O11 K2 O10 87.05(6) . . ?
O12B K2 O10 114.02(17) . . ?
O8 K2 O10 140.38(5) . . ?
O11 K2 O7 104.46(6) . . ?
O12B K2 O7 139.38(18) . . ?
O8 K2 O7 60.86(5) . . ?
O10 K2 O7 101.21(5) . . ?
O11 K2 O9 122.19(7) . . ?
O12B K2 O9 90.09(18) . . ?
O8 K2 O9 100.45(5) . . ?
O10 K2 O9 59.89(5) . . ?
O7 K2 O9 126.23(5) . . ?
O11 K2 O12A 57.18(9) . . ?
O8 K2 O12A 90.43(10) . . ?
O10 K2 O12A 126.11(11) . . ?
O7 K2 O12A 124.37(13) . . ?
O9 K2 O12A 103.91(12) . . ?
O11 K2 N3 60.30(6) . . ?
O12B K2 N3 120.21(13) . . ?
O8 K2 N3 121.31(6) . . ?
O10 K2 N3 60.25(5) . . ?
O7 K2 N3 61.03(5) . . ?
O9 K2 N3 119.72(5) . . ?
O12A K2 N3 115.99(9) . . ?
O11 K2 N4 118.07(6) . . ?
O12B K2 N4 58.13(13) . . ?
O8 K2 N4 60.22(5) . . ?
O10 K2 N4 119.39(5) . . ?
O7 K2 N4 120.63(6) . . ?
O9 K2 N4 60.18(5) . . ?
O12A K2 N4 62.62(9) . . ?
N3 K2 N4 178.19(6) . . ?
O11 K2 C38A 45.71(9) . . ?
O8 K2 C38A 114.72(10) . . ?
O10 K2 C38A 101.05(10) . . ?
O7 K2 C38A 141.11(10) . . ?
O9 K2 C38A 92.57(10) . . ?
O12A K2 C38A 25.08(15) . . ?
N3 K2 C38A 104.86(9) . . ?
N4 K2 C38A 73.39(9) . . ?
C23 N3 C35 111.1(2) . . ?
C23 N3 C34 109.9(2) . . ?
C35 N3 C34 110.7(2) . . ?
C23 N3 K2 108.67(14) . . ?
C35 N3 K2 106.20(14) . . ?
C34 N3 K2 110.16(14) . . ?
C28 N4 C29 109.5(2) . . ?
C28 N4 C40 110.0(2) . . ?
C29 N4 C40 110.5(2) . . ?
C28 N4 K2 109.33(14) . . ?
C29 N4 K2 108.69(14) . . ?
C40 N4 K2 108.74(15) . . ?
C25 O7 C24 111.28(19) . . ?
C25 O7 K2 110.57(14) . . ?
C24 O7 K2 114.74(15) . . ?
C26 O8 C27 111.7(2) . . ?
C26 O8 K2 115.99(14) . . ?
C27 O8 K2 117.83(14) . . ?
C31 O9 C30 110.6(2) . . ?
C31 O9 K2 111.80(13) . . ?
C30 O9 K2 117.05(15) . . ?
C32 O10 C33 110.98(19) . . ?
C32 O10 K2 117.05(13) . . ?
C33 O10 K2 115.72(14) . . ?
C37B O11 C36 113.3(2) . . ?
C37A O11 C36 113.3(2) . . ?
C37B O11 K2 117.99(15) . . ?
C37A O11 K2 117.99(15) . . ?
C36 O11 K2 124.09(15) . . ?
N3 C23 C24 114.4(2) . . ?
N3 C23 H23A 108.7 . . ?
C24 C23 H23A 108.7 . . ?
N3 C23 H23B 108.7 . . ?
C24 C23 H23B 108.7 . . ?
H23A C23 H23B 107.6 . . ?
O7 C24 C23 109.3(2) . . ?
O7 C24 H24A 109.8 . . ?
C23 C24 H24A 109.8 . . ?
O7 C24 H24B 109.8 . . ?
C23 C24 H24B 109.8 . . ?
H24A C24 H24B 108.3 . . ?
O7 C25 C26 109.3(2) . . ?
O7 C25 H25A 109.8 . . ?
C26 C25 H25A 109.8 . . ?
O7 C25 H25B 109.8 . . ?
C26 C25 H25B 109.8 . . ?
H25A C25 H25B 108.3 . . ?
O8 C26 C25 109.0(2) . . ?
O8 C26 H26A 109.9 . . ?
C25 C26 H26A 109.9 . . ?
O8 C26 H26B 109.9 . . ?
C25 C26 H26B 109.9 . . ?
H26A C26 H26B 108.3 . . ?
O8 C27 C28 108.6(2) . . ?
O8 C27 H27A 110.0 . . ?
C28 C27 H27A 110.0 . . ?
O8 C27 H27B 110.0 . . ?
C28 C27 H27B 110.0 . . ?
H27A C27 H27B 108.3 . . ?
N4 C28 C27 113.9(2) . . ?
N4 C28 H28A 108.8 . . ?
C27 C28 H28A 108.8 . . ?
N4 C28 H28B 108.8 . . ?
C27 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
N4 C29 C30 113.4(2) . . ?
N4 C29 H29A 108.9 . . ?
C30 C29 H29A 108.9 . . ?
N4 C29 H29B 108.9 . . ?
C30 C29 H29B 108.9 . . ?
H29A C29 H29B 107.7 . . ?
O9 C30 C29 108.6(2) . . ?
O9 C30 H30A 110.0 . . ?
C29 C30 H30A 110.0 . . ?
O9 C30 H30B 110.0 . . ?
C29 C30 H30B 110.0 . . ?
H30A C30 H30B 108.3 . . ?
O9 C31 C32 109.4(2) . . ?
O9 C31 H31A 109.8 . . ?
C32 C31 H31A 109.8 . . ?
O9 C31 H31B 109.8 . . ?
C32 C31 H31B 109.8 . . ?
H31A C31 H31B 108.2 . . ?
O10 C32 C31 109.1(2) . . ?
O10 C32 H32A 109.9 . . ?
C31 C32 H32A 109.9 . . ?
O10 C32 H32B 109.9 . . ?
C31 C32 H32B 109.9 . . ?
H32A C32 H32B 108.3 . . ?
O10 C33 C34 108.8(2) . . ?
O10 C33 H33A 109.9 . . ?
C34 C33 H33A 109.9 . . ?
O10 C33 H33B 109.9 . . ?
C34 C33 H33B 109.9 . . ?
H33A C33 H33B 108.3 . . ?
N3 C34 C33 113.8(2) . . ?
N3 C34 H34A 108.8 . . ?
C33 C34 H34A 108.8 . . ?
N3 C34 H34B 108.8 . . ?
C33 C34 H34B 108.8 . . ?
H34A C34 H34B 107.7 . . ?
N3 C35 C36 114.4(2) . . ?
N3 C35 H35A 108.7 . . ?
C36 C35 H35A 108.7 . . ?
N3 C35 H35B 108.7 . . ?
C36 C35 H35B 108.7 . . ?
H35A C35 H35B 107.6 . . ?
O11 C36 C35 109.4(2) . . ?
O11 C36 H36A 109.8 . . ?
C35 C36 H36A 109.8 . . ?
O11 C36 H36B 109.8 . . ?
C35 C36 H36B 109.8 . . ?
H36A C36 H36B 108.2 . . ?
O11 C37A C38A 108.0(3) . . ?
O11 C37A H37A 110.1 . . ?
C38A C37A H37A 110.1 . . ?
O11 C37A H37B 110.1 . . ?
C38A C37A H37B 110.1 . . ?
H37A C37A H37B 108.4 . . ?
O12A C38A C37A 106.3(4) . . ?
O12A C38A K2 60.5(3) . . ?
C37A C38A K2 88.1(2) . . ?
O12A C38A H38A 110.5 . . ?
C37A C38A H38A 110.5 . . ?
K2 C38A H38A 161.4 . . ?
O12A C38A H38B 110.5 . . ?
C37A C38A H38B 110.5 . . ?
K2 C38A H38B 64.1 . . ?
H38A C38A H38B 108.7 . . ?
C38A O12A C39 109.0(4) . . ?
C38A O12A K2 94.4(3) . . ?
C39 O12A K2 114.2(3) . . ?
O11 C37B C38B 112.7(3) . . ?
O11 C37B H37C 109.1 . . ?
C38B C37B H37C 109.1 . . ?
O11 C37B H37D 109.1 . . ?
C38B C37B H37D 109.1 . . ?
H37C C37B H37D 107.8 . . ?
O12B C38B C37B 106.5(6) . . ?
O12B C38B H38C 110.4 . . ?
C37B C38B H38C 110.4 . . ?
O12B C38B H38D 110.4 . . ?
C37B C38B H38D 110.4 . . ?
H38C C38B H38D 108.6 . . ?
C38B O12B C39 104.3(5) . . ?
C38B O12B K2 118.4(4) . . ?
C39 O12B K2 117.4(3) . . ?
O12A C39 C40 120.9(3) . . ?
C40 C39 O12B 96.8(4) . . ?
O12A C39 H39A 107.1 . . ?
C40 C39 H39A 107.1 . . ?
O12A C39 H39B 107.1 . . ?
C40 C39 H39B 107.1 . . ?
H39A C39 H39B 106.8 . . ?
N4 C40 C39 113.8(2) . . ?
N4 C40 H40A 108.8 . . ?
C39 C40 H40A 108.8 . . ?
N4 C40 H40B 108.8 . . ?
C39 C40 H40B 108.8 . . ?
H40A C40 H40B 107.7 . . ?
H5C N5 H5D 109.5 . . ?
H5C N5 H5E 109.5 . . ?
H5D N5 H5E 109.5 . . ?
H6C N6 H6D 109.5 . . ?
H6C N6 H6E 109.5 . . ?
H6D N6 H6E 109.5 . . ?

_refine_diff_density_max         0.727
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.069


#============================================================================== 
# END of CIF  
#============================================================================== 
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ammonia'
####################################################################### 
# 
# 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_KM-151
_database_code_depnum_ccdc_archive 'CCDC 1982122'
loop_
_audit_author_name
_audit_author_address
'Wilhelm Klein'
;Technische Universitaet Muenchen
Germany
;
_audit_update_record             
;
2020-02-05 deposited with the CCDC.	2020-04-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'Sn8 Zn, 6(H3 N), 6(K)'
_chemical_formula_sum            'H48 K6 N16 Sn8 Zn'
_chemical_formula_weight         1522.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6916(6)
_cell_length_b                   12.2418(7)
_cell_length_c                   18.6684(8)
_cell_angle_alpha                99.120(4)
_cell_angle_beta                 90.067(4)
_cell_angle_gamma                94.894(5)
_cell_volume                     2178.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    18457
_cell_measurement_theta_min      2.7172
_cell_measurement_theta_max      29.0250

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.320
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    5.635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.61536
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d 
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Xcalibur 3'
_diffrn_measurement_method       'ω and π scans'
_diffrn_detector_area_resol_mean 16.0238
_diffrn_reflns_number            50041
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_av_R_equivalents  0.0912
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.718
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             8378
_reflns_number_gt                6048
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_computing_data_collection       
; 
 CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.34d 
;
_computing_cell_refinement       
; 
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d 
;
_computing_data_reduction        
; 
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d 
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0302P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00020(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8378
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0694
_refine_ls_wR_factor_gt          0.0667
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_restrained_S_all      0.919
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.28559(4) 0.23389(3) 0.19683(2) 0.02274(11) Uani 1 1 d . . . . .
Sn2 Sn 0.10857(4) 0.39363(3) 0.13330(2) 0.02201(11) Uani 1 1 d . . . . .
Sn3 Sn 0.22335(4) 0.20833(3) 0.04259(2) 0.02313(11) Uani 1 1 d . . . . .
Sn4 Sn 0.00199(4) 0.16991(3) 0.14629(2) 0.02501(11) Uani 1 1 d . . . . .
Zn Zn 0.29291(7) 0.45722(5) 0.24820(4) 0.02115(16) Uani 1 1 d . . . . .
Sn5 Sn 0.50124(4) 0.62663(3) 0.27260(2) 0.02208(11) Uani 1 1 d . . . . .
Sn6 Sn 0.26327(4) 0.59157(3) 0.37741(2) 0.02593(11) Uani 1 1 d . . . . .
Sn7 Sn 0.36741(4) 0.81086(3) 0.35152(2) 0.02612(11) Uani 1 1 d . . . . .
Sn8 Sn 0.53754(4) 0.67827(3) 0.42906(2) 0.02647(11) Uani 1 1 d . . . . .
K1 K 0.48767(14) 0.43836(12) 0.08638(7) 0.0318(3) Uani 1 1 d . . . . .
K2 K -0.04857(14) 0.35141(13) 0.31902(8) 0.0352(4) Uani 1 1 d . . . . .
K3 K 0.57897(15) 0.37891(12) 0.38406(8) 0.0381(4) Uani 1 1 d . . . . .
K4 K 0.16422(14) 0.71618(11) 0.19079(7) 0.0311(3) Uani 1 1 d . . . . .
K5 K 0.12868(14) -0.09691(11) 0.05166(8) 0.0299(3) Uani 1 1 d . . . . .
K6 K 0.77669(16) 0.87870(13) 0.33472(9) 0.0415(4) Uani 1 1 d . . . . .
N1 N 0.4726(5) 0.6733(4) 0.0641(3) 0.0346(13) Uani 1 1 d . . . . .
H1A H 0.5445 0.7217 0.0548 0.052 Uiso 1 1 d R U . . .
H1B H 0.4710 0.6698 0.1124 0.052 Uiso 1 1 d R U . . .
H1C H 0.3916 0.6970 0.0503 0.052 Uiso 1 1 d R U . . .
N2 N 0.7594(5) 0.5443(4) 0.0938(3) 0.0329(13) Uani 1 1 d . . . . .
H2A H 0.7781 0.5713 0.0519 0.049 Uiso 1 1 calc R U . . .
H2B H 0.8211 0.4945 0.1002 0.049 Uiso 1 1 calc R U . . .
H2C H 0.7666 0.6012 0.1318 0.049 Uiso 1 1 calc R U . . .
N3 N 0.1696(5) 0.2807(5) 0.4070(3) 0.0401(15) Uani 1 1 d . . . . .
H3A H 0.2177 0.2298 0.3787 0.060 Uiso 1 1 calc R U . . .
H3B H 0.1303 0.2497 0.4441 0.060 Uiso 1 1 calc R U . . .
H3C H 0.2284 0.3406 0.4253 0.060 Uiso 1 1 calc R U . . .
N4 N 0.8648(5) 0.5182(4) 0.4310(3) 0.0334(13) Uani 1 1 d . . . . .
H4A H 0.8021 0.5660 0.4223 0.050 Uiso 1 1 d R U . . .
H4B H 0.9502 0.5432 0.4172 0.050 Uiso 1 1 d R U . . .
H4C H 0.8667 0.5139 0.4792 0.050 Uiso 1 1 d R U . . .
N5 N 0.7981(6) 0.2323(5) 0.4187(3) 0.0454(16) Uani 1 1 d . . . . .
H5A H 0.7684 0.1621 0.3974 0.068 Uiso 1 1 d R U . . .
H5B H 0.7457 0.2528 0.4581 0.068 Uiso 1 1 d R U . . .
H5C H 0.8884 0.2345 0.4327 0.068 Uiso 1 1 d R U . . .
N6 N 0.6933(5) 0.3472(5) 0.2347(3) 0.0357(14) Uani 1 1 d . . . . .
H6A H 0.6225 0.2928 0.2259 0.054 Uiso 1 1 d R U . . .
H6B H 0.7605 0.3336 0.2013 0.054 Uiso 1 1 d R U . . .
H6C H 0.6611 0.4141 0.2318 0.054 Uiso 1 1 d R U . . .
N7 N 0.4670(5) 0.1424(4) 0.3720(3) 0.0383(14) Uani 1 1 d . . . . .
H7A H 0.5379 0.0978 0.3649 0.057 Uiso 1 1 calc R U . . .
H7B H 0.4063 0.1253 0.3339 0.057 Uiso 1 1 calc R U . . .
H7C H 0.4227 0.1318 0.4136 0.057 Uiso 1 1 calc R U . . .
N8 N 0.3466(5) 0.9137(4) 0.1615(3) 0.0381(14) Uani 1 1 d . . . . .
H8A H 0.4195 0.9057 0.1310 0.057 Uiso 1 1 d R U . . .
H8B H 0.3621 0.8815 0.2011 0.057 Uiso 1 1 d R U . . .
H8C H 0.3370 0.9872 0.1757 0.057 Uiso 1 1 d R U . . .
N9 N 0.1312(5) 0.6582(4) 0.0338(3) 0.0309(13) Uani 1 1 d . . . . .
H9A H 0.0450 0.6470 0.0132 0.046 Uiso 1 1 d R U . . .
H9B H 0.1503 0.5971 0.0527 0.046 Uiso 1 1 d R U . . .
H9C H 0.1947 0.6708 -0.0005 0.046 Uiso 1 1 d R U . . .
N10 N -0.0736(5) 0.8356(4) 0.1596(3) 0.0341(13) Uani 1 1 d . . . . .
H10A H -0.1316 0.8291 0.1205 0.051 Uiso 1 1 d R U . . .
H10B H -0.0610 0.9081 0.1806 0.051 Uiso 1 1 d R U . . .
H10C H -0.1114 0.7943 0.1922 0.051 Uiso 1 1 d R U . . .
N11 N -0.0859(5) 0.6409(4) 0.2698(3) 0.0372(14) Uani 1 1 d . . . . .
H11A H -0.1726 0.6278 0.2870 0.056 Uiso 1 1 d R U . . .
H11B H -0.0259 0.6024 0.2913 0.056 Uiso 1 1 d R U . . .
H11C H -0.0862 0.6186 0.2209 0.056 Uiso 1 1 d R U . . .
N12 N 0.3662(5) -0.1039(5) -0.0436(3) 0.0481(17) Uani 1 1 d . . . . .
H12A H 0.3405 -0.1433 -0.0878 0.072 Uiso 1 1 calc R U . . .
H12B H 0.4344 -0.1371 -0.0240 0.072 Uiso 1 1 calc R U . . .
H12C H 0.3979 -0.0335 -0.0487 0.072 Uiso 1 1 calc R U . . .
N13 N 0.6913(6) 1.0381(5) 0.2510(3) 0.0503(17) Uani 1 1 d . . . . .
H13A H 0.7665 1.0688 0.2300 0.075 Uiso 1 1 calc R U . . .
H13B H 0.6504 1.0922 0.2805 0.075 Uiso 1 1 calc R U . . .
H13C H 0.6298 1.0039 0.2160 0.075 Uiso 1 1 calc R U . . .
N14 N 1.0464(5) 1.0025(5) 0.3197(3) 0.0472(16) Uani 1 1 d . . . . .
H14A H 1.0625 1.0567 0.3589 0.071 Uiso 1 1 calc R U . . .
H14B H 1.0456 1.0337 0.2786 0.071 Uiso 1 1 calc R U . . .
H14C H 1.1145 0.9552 0.3170 0.071 Uiso 1 1 calc R U . . .
N15 N 0.9750(6) 0.8282(5) 0.4393(3) 0.0543(18) Uani 1 1 d . . . . .
H15A H 1.0134 0.8925 0.4657 0.081 Uiso 1 1 calc R U . . .
H15B H 1.0426 0.7905 0.4154 0.081 Uiso 1 1 calc R U . . .
H15C H 0.9309 0.7857 0.4696 0.081 Uiso 1 1 calc R U . . .
N16 N 0.6973(6) 0.9898(5) 0.4718(3) 0.0496(17) Uani 1 1 d . . . . .
H16A H 0.7261 1.0633 0.4762 0.074 Uiso 1 1 calc R U . . .
H16B H 0.7370 0.9602 0.5077 0.074 Uiso 1 1 calc R U . . .
H16C H 0.6035 0.9814 0.4755 0.074 Uiso 1 1 calc R U . . .


_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
Sn1 Zn 2.7450(8) . ?
Sn1 Sn3 2.9038(6) . ?
Sn1 Sn4 2.9071(6) . ?
Sn1 Sn2 3.0785(6) . ?
Sn1 K1 3.8938(14) . ?
Sn2 Zn 2.7611(8) . ?
Sn2 Sn4 2.8904(6) . ?
Sn2 Sn3 2.9100(6) . ?
Sn2 K1 3.7924(14) . ?
Sn2 K2 3.8799(15) . ?
Sn2 K4 3.9149(15) . ?
Sn3 Sn4 2.9492(6) . ?
Sn3 K1 3.6325(14) . ?
Sn3 K5 3.8012(14) . ?
Sn3 K5 3.8764(14) 2 ?
Sn4 K2 3.6734(16) . ?
Sn4 K5 3.7626(15) . ?
Sn4 K5 3.8479(15) 2 ?
Zn Sn6 2.7258(8) . ?
Zn Sn5 2.7512(8) . ?
Zn K1 3.5509(15) . ?
Zn K2 3.7683(16) . ?
Zn K4 3.8083(15) . ?
Zn K3 4.0305(16) . ?
Sn5 Sn7 2.8964(6) . ?
Sn5 Sn8 2.9033(6) . ?
Sn5 Sn6 3.0723(6) . ?
Sn5 K1 3.8500(15) . ?
Sn5 K4 3.9158(14) . ?
Sn5 K6 3.9302(16) . ?
Sn5 K3 4.0595(15) . ?
Sn6 Sn8 2.8827(6) . ?
Sn6 Sn7 2.8998(6) . ?
Sn6 K2 4.0529(15) . ?
Sn6 K4 4.1610(13) . ?
Sn7 Sn8 2.9402(6) . ?
Sn7 K4 3.5664(14) . ?
Sn7 K6 4.0057(16) . ?
Sn8 K3 3.6841(16) . ?
Sn8 K3 3.8190(15) 2_666 ?
Sn8 K6 3.8606(15) . ?
K1 N2 2.828(5) . ?
K1 N1 2.963(5) 2_665 ?
K1 N1 2.987(5) . ?
K1 K1 3.771(3) 2_665 ?
K1 K4 4.992(2) . ?
K1 H1B 2.8159 . ?
K2 N4 2.861(5) 1_455 ?
K2 N5 2.879(5) 1_455 ?
K2 N3 2.945(5) . ?
K2 N6 2.946(5) 1_455 ?
K2 K3 3.835(2) 1_455 ?
K3 N7 2.978(5) . ?
K3 N6 2.981(5) . ?
K3 N5 3.027(5) . ?
K3 N4 3.172(5) . ?
K3 Sn8 3.8190(15) 2_666 ?
K3 K2 3.835(2) 1_655 ?
K3 H4A 3.0103 . ?
K3 H5B 2.8288 . ?
K3 H6A 3.0171 . ?
K3 H6C 3.0375 . ?
K4 N9 2.915(5) . ?
K4 N10 2.938(5) . ?
K4 N11 2.993(5) . ?
K4 N8 2.994(5) . ?
K4 K5 3.7571(18) 1_565 ?
K4 K6 4.989(2) 1_455 ?
K4 H8B 2.6497 . ?
K4 H9B 2.7497 . ?
K4 H10C 2.9113 . ?
K4 H11B 3.0421 . ?
K4 H11C 2.7124 . ?
K5 N12 2.908(6) . ?
K5 N8 2.922(5) 1_545 ?
K5 N9 2.965(5) 1_545 ?
K5 N10 2.974(5) 1_545 ?
K5 K4 3.7572(18) 1_545 ?
K5 Sn4 3.8479(15) 2 ?
K5 Sn3 3.8765(14) 2 ?
K5 K5 4.245(3) 2 ?
K6 N16 2.841(6) . ?
K6 N13 2.859(6) . ?
K6 N15 2.910(6) . ?
K6 N14 2.944(5) . ?
K6 N11 3.356(6) 1_655 ?
K6 K4 4.989(2) 1_655 ?
N1 K1 2.963(5) 2_665 ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
N4 K2 2.861(5) 1_655 ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N4 H4C 0.9100 . ?
N5 K2 2.879(5) 1_655 ?
N5 H5A 0.9100 . ?
N5 H5B 0.9100 . ?
N5 H5C 0.9100 . ?
N6 K2 2.946(5) 1_655 ?
N6 H6A 0.9100 . ?
N6 H6B 0.9100 . ?
N6 H6C 0.9100 . ?
N7 H7A 0.9100 . ?
N7 H7B 0.9100 . ?
N7 H7C 0.9100 . ?
N8 K5 2.922(5) 1_565 ?
N8 H8A 0.9100 . ?
N8 H8B 0.9100 . ?
N8 H8C 0.9100 . ?
N9 K5 2.965(5) 1_565 ?
N9 H9A 0.9100 . ?
N9 H9B 0.9100 . ?
N9 H9C 0.9100 . ?
N10 K5 2.974(5) 1_565 ?
N10 H10A 0.9100 . ?
N10 H10B 0.9100 . ?
N10 H10C 0.9100 . ?
N11 K6 3.356(6) 1_455 ?
N11 H11A 0.9100 . ?
N11 H11B 0.9100 . ?
N11 H11C 0.9100 . ?
N12 H12A 0.9100 . ?
N12 H12B 0.9100 . ?
N12 H12C 0.9100 . ?
N13 H13A 0.9100 . ?
N13 H13B 0.9100 . ?
N13 H13C 0.9100 . ?
N14 H14A 0.9100 . ?
N14 H14B 0.9100 . ?
N14 H14C 0.9100 . ?
N15 H15A 0.9100 . ?
N15 H15B 0.9100 . ?
N15 H15C 0.9100 . ?
N16 H16A 0.9100 . ?
N16 H16B 0.9100 . ?
N16 H16C 0.9100 . ?

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
Zn Sn1 Sn3 106.18(2) . . ?
Zn Sn1 Sn4 104.99(2) . . ?
Sn3 Sn1 Sn4 60.999(14) . . ?
Zn Sn1 Sn2 56.254(18) . . ?
Sn3 Sn1 Sn2 58.125(14) . . ?
Sn4 Sn1 Sn2 57.665(14) . . ?
Zn Sn1 K1 61.84(3) . . ?
Sn3 Sn1 K1 62.62(2) . . ?
Sn4 Sn1 K1 113.79(2) . . ?
Sn2 Sn1 K1 64.67(2) . . ?
Zn Sn2 Sn4 105.02(2) . . ?
Zn Sn2 Sn3 105.58(2) . . ?
Sn4 Sn2 Sn3 61.120(14) . . ?
Zn Sn2 Sn1 55.758(17) . . ?
Sn4 Sn2 Sn1 58.190(14) . . ?
Sn3 Sn2 Sn1 57.929(14) . . ?
Zn Sn2 K1 63.34(3) . . ?
Sn4 Sn2 K1 117.16(3) . . ?
Sn3 Sn2 K1 64.06(3) . . ?
Sn1 Sn2 K1 68.13(2) . . ?
Zn Sn2 K2 66.69(3) . . ?
Sn4 Sn2 K2 63.77(3) . . ?
Sn3 Sn2 K2 119.38(3) . . ?
Sn1 Sn2 K2 72.97(2) . . ?
K1 Sn2 K2 128.06(3) . . ?
Zn Sn2 K4 67.00(2) . . ?
Sn4 Sn2 K4 155.81(3) . . ?
Sn3 Sn2 K4 142.18(3) . . ?
Sn1 Sn2 K4 122.21(2) . . ?
K1 Sn2 K4 80.73(3) . . ?
K2 Sn2 K4 92.59(3) . . ?
Sn1 Sn3 Sn2 63.946(15) . . ?
Sn1 Sn3 Sn4 59.556(15) . . ?
Sn2 Sn3 Sn4 59.113(14) . . ?
Sn1 Sn3 K1 72.15(2) . . ?
Sn2 Sn3 K1 69.86(3) . . ?
Sn4 Sn3 K1 120.43(3) . . ?
Sn1 Sn3 K5 86.46(2) . . ?
Sn2 Sn3 K5 125.36(3) . . ?
Sn4 Sn3 K5 66.36(2) . . ?
K1 Sn3 K5 144.84(3) . . ?
Sn1 Sn3 K5 126.32(3) . 2 ?
Sn2 Sn3 K5 93.78(2) . 2 ?
Sn4 Sn3 K5 67.04(2) . 2 ?
K1 Sn3 K5 147.92(3) . 2 ?
K5 Sn3 K5 67.12(3) . 2 ?
Sn2 Sn4 Sn1 64.146(14) . . ?
Sn2 Sn4 Sn3 59.767(14) . . ?
Sn1 Sn4 Sn3 59.445(14) . . ?
Sn2 Sn4 K2 71.34(3) . . ?
Sn1 Sn4 K2 78.08(3) . . ?
Sn3 Sn4 K2 124.93(3) . . ?
Sn2 Sn4 K5 127.39(3) . . ?
Sn1 Sn4 K5 87.14(3) . . ?
Sn3 Sn4 K5 67.74(2) . . ?
K2 Sn4 K5 147.36(3) . . ?
Sn2 Sn4 K5 94.70(2) . 2 ?
Sn1 Sn4 K5 127.23(3) . 2 ?
Sn3 Sn4 K5 68.07(2) . 2 ?
K2 Sn4 K5 143.20(3) . 2 ?
K5 Sn4 K5 67.79(3) . 2 ?
Sn6 Zn Sn1 137.89(3) . . ?
Sn6 Zn Sn5 68.24(2) . . ?
Sn1 Zn Sn5 134.06(3) . . ?
Sn6 Zn Sn2 130.11(3) . . ?
Sn1 Zn Sn2 67.99(2) . . ?
Sn5 Zn Sn2 130.98(3) . . ?
Sn6 Zn K1 141.83(3) . . ?
Sn1 Zn K1 75.19(3) . . ?
Sn5 Zn K1 74.09(3) . . ?
Sn2 Zn K1 72.64(3) . . ?
Sn6 Zn K2 75.33(3) . . ?
Sn1 Zn K2 78.28(3) . . ?
Sn5 Zn K2 143.19(3) . . ?
Sn2 Zn K2 71.01(3) . . ?
K1 Zn K2 140.90(4) . . ?
Sn6 Zn K4 77.14(3) . . ?
Sn1 Zn K4 138.31(3) . . ?
Sn5 Zn K4 71.24(3) . . ?
Sn2 Zn K4 71.13(3) . . ?
K1 Zn K4 85.36(3) . . ?
K2 Zn K4 96.10(3) . . ?
Sn6 Zn K3 73.99(3) . . ?
Sn1 Zn K3 81.74(3) . . ?
Sn5 Zn K3 70.69(3) . . ?
Sn2 Zn K3 149.71(3) . . ?
K1 Zn K3 99.49(3) . . ?
K2 Zn K3 104.56(3) . . ?
K4 Zn K3 138.51(4) . . ?
Zn Sn5 Sn7 103.95(2) . . ?
Zn Sn5 Sn8 105.75(2) . . ?
Sn7 Sn5 Sn8 60.924(15) . . ?
Zn Sn5 Sn6 55.487(18) . . ?
Sn7 Sn5 Sn6 58.045(14) . . ?
Sn8 Sn5 Sn6 57.603(14) . . ?
Zn Sn5 K1 62.50(3) . . ?
Sn7 Sn5 K1 140.49(3) . . ?
Sn8 Sn5 K1 155.41(3) . . ?
Sn6 Sn5 K1 117.70(2) . . ?
Zn Sn5 K4 67.06(3) . . ?
Sn7 Sn5 K4 60.98(2) . . ?
Sn8 Sn5 K4 116.75(3) . . ?
Sn6 Sn5 K4 71.94(2) . . ?
K1 Sn5 K4 80.01(3) . . ?
Zn Sn5 K6 171.94(3) . . ?
Sn7 Sn5 K6 69.99(3) . . ?
Sn8 Sn5 K6 66.85(3) . . ?
Sn6 Sn5 K6 116.51(3) . . ?
K1 Sn5 K6 125.56(3) . . ?
K4 Sn5 K6 112.72(3) . . ?
Zn Sn5 K3 69.55(3) . . ?
Sn7 Sn5 K3 116.60(3) . . ?
Sn8 Sn5 K3 61.26(3) . . ?
Sn6 Sn5 K3 70.55(2) . . ?
K1 Sn5 K3 94.17(3) . . ?
K4 Sn5 K3 133.61(3) . . ?
K6 Sn5 K3 107.92(3) . . ?
Zn Sn6 Sn8 107.00(2) . . ?
Zn Sn6 Sn7 104.51(2) . . ?
Sn8 Sn6 Sn7 61.123(15) . . ?
Zn Sn6 Sn5 56.272(18) . . ?
Sn8 Sn6 Sn5 58.254(14) . . ?
Sn7 Sn6 Sn5 57.936(14) . . ?
Zn Sn6 K2 64.09(3) . . ?
Sn8 Sn6 K2 155.43(3) . . ?
Sn7 Sn6 K2 141.77(3) . . ?
Sn5 Sn6 K2 120.14(3) . . ?
Zn Sn6 K4 63.16(3) . . ?
Sn8 Sn6 K4 110.43(2) . . ?
Sn7 Sn6 K4 57.39(2) . . ?
Sn5 Sn6 K4 63.47(2) . . ?
K2 Sn6 K4 86.62(3) . . ?
Sn5 Sn7 Sn6 64.019(15) . . ?
Sn5 Sn7 Sn8 59.654(14) . . ?
Sn6 Sn7 Sn8 59.151(14) . . ?
Sn5 Sn7 K4 73.77(3) . . ?
Sn6 Sn7 K4 79.37(2) . . ?
Sn8 Sn7 K4 127.04(3) . . ?
Sn5 Sn7 K6 67.21(3) . . ?
Sn6 Sn7 K6 118.85(3) . . ?
Sn8 Sn7 K6 65.45(3) . . ?
K4 Sn7 K6 119.11(3) . . ?
Sn6 Sn8 Sn5 64.144(15) . . ?
Sn6 Sn8 Sn7 59.726(14) . . ?
Sn5 Sn8 Sn7 59.422(15) . . ?
Sn6 Sn8 K3 78.41(3) . . ?
Sn5 Sn8 K3 75.04(3) . . ?
Sn7 Sn8 K3 127.48(3) . . ?
Sn6 Sn8 K3 86.83(3) . 2_666 ?
Sn5 Sn8 K3 148.06(3) . 2_666 ?
Sn7 Sn8 K3 118.28(3) . 2_666 ?
K3 Sn8 K3 86.82(4) . 2_666 ?
Sn6 Sn8 K6 124.01(3) . . ?
Sn5 Sn8 K6 69.40(3) . . ?
Sn7 Sn8 K6 70.70(3) . . ?
K3 Sn8 K6 117.80(4) . . ?
K3 Sn8 K6 142.32(4) 2_666 . ?
N2 K1 N1 91.84(15) . 2_665 ?
N2 K1 N1 71.49(14) . . ?
N1 K1 N1 101.33(14) 2_665 . ?
N2 K1 Zn 118.10(12) . . ?
N1 K1 Zn 148.85(11) 2_665 . ?
N1 K1 Zn 96.58(11) . . ?
N2 K1 Sn3 155.71(11) . . ?
N1 K1 Sn3 70.94(10) 2_665 . ?
N1 K1 Sn3 127.51(11) . . ?
Zn K1 Sn3 77.93(3) . . ?
N2 K1 K1 76.92(11) . 2_665 ?
N1 K1 K1 50.94(10) 2_665 2_665 ?
N1 K1 K1 50.39(10) . 2_665 ?
Zn K1 K1 139.75(7) . 2_665 ?
Sn3 K1 K1 103.04(5) . 2_665 ?
N2 K1 Sn2 157.46(12) . . ?
N1 K1 Sn2 108.70(10) 2_665 . ?
N1 K1 Sn2 94.79(10) . . ?
Zn K1 Sn2 44.02(2) . . ?
Sn3 K1 Sn2 46.086(18) . . ?
K1 K1 Sn2 108.55(5) 2_665 . ?
N2 K1 Sn5 76.67(11) . . ?
N1 K1 Sn5 167.70(11) 2_665 . ?
N1 K1 Sn5 71.10(10) . . ?
Zn K1 Sn5 43.41(2) . . ?
Sn3 K1 Sn5 121.34(4) . . ?
K1 K1 Sn5 120.74(6) 2_665 . ?
Sn2 K1 Sn5 82.03(3) . . ?
N2 K1 Sn1 134.47(11) . . ?
N1 K1 Sn1 109.99(11) 2_665 . ?
N1 K1 Sn1 136.46(11) . . ?
Zn K1 Sn1 42.966(19) . . ?
Sn3 K1 Sn1 45.224(18) . . ?
K1 K1 Sn1 147.43(6) 2_665 . ?
Sn2 K1 Sn1 47.199(18) . . ?
Sn5 K1 Sn1 81.61(3) . . ?
N2 K1 K4 108.47(11) . . ?
N1 K1 K4 131.91(10) 2_665 . ?
N1 K1 K4 50.05(10) . . ?
Zn K1 K4 49.49(3) . . ?
Sn3 K1 K4 95.81(3) . . ?
K1 K1 K4 90.94(5) 2_665 . ?
Sn2 K1 K4 50.71(2) . . ?
Sn5 K1 K4 50.57(2) . . ?
Sn1 K1 K4 86.41(3) . . ?
N2 K1 H1B 71.5 . . ?
N1 K1 H1B 119.0 2_665 . ?
N1 K1 H1B 17.7 . . ?
Zn K1 H1B 81.3 . . ?
Sn3 K1 H1B 131.6 . . ?
K1 K1 H1B 68.1 2_665 . ?
Sn2 K1 H1B 90.0 . . ?
Sn5 K1 H1B 53.4 . . ?
Sn1 K1 H1B 123.6 . . ?
K4 K1 H1B 40.1 . . ?
N4 K2 N5 74.51(16) 1_455 1_455 ?
N4 K2 N3 95.38(15) 1_455 . ?
N5 K2 N3 76.63(15) 1_455 . ?
N4 K2 N6 92.25(15) 1_455 1_455 ?
N5 K2 N6 88.63(15) 1_455 1_455 ?
N3 K2 N6 160.89(16) . 1_455 ?
N4 K2 Sn4 165.11(11) 1_455 . ?
N5 K2 Sn4 111.09(13) 1_455 . ?
N3 K2 Sn4 99.34(12) . . ?
N6 K2 Sn4 74.45(11) 1_455 . ?
N4 K2 Zn 108.34(11) 1_455 . ?
N5 K2 Zn 149.90(12) 1_455 . ?
N3 K2 Zn 73.27(10) . . ?
N6 K2 Zn 120.65(11) 1_455 . ?
Sn4 K2 Zn 74.11(3) . . ?
N4 K2 K3 54.22(11) 1_455 1_455 ?
N5 K2 K3 51.21(11) 1_455 1_455 ?
N3 K2 K3 123.15(11) . 1_455 ?
N6 K2 K3 50.08(10) 1_455 1_455 ?
Sn4 K2 K3 117.68(4) . 1_455 ?
Zn K2 K3 154.11(5) . 1_455 ?
N4 K2 Sn2 127.48(11) 1_455 . ?
N5 K2 Sn2 155.61(13) 1_455 . ?
N3 K2 Sn2 107.87(11) . . ?
N6 K2 Sn2 80.79(10) 1_455 . ?
Sn4 K2 Sn2 44.895(19) . . ?
Zn K2 Sn2 42.294(19) . . ?
K3 K2 Sn2 128.93(4) 1_455 . ?
N4 K2 Sn6 69.33(10) 1_455 . ?
N5 K2 Sn6 124.56(13) 1_455 . ?
N3 K2 Sn6 66.79(11) . . ?
N6 K2 Sn6 132.30(11) 1_455 . ?
Sn4 K2 Sn6 114.69(4) . . ?
Zn K2 Sn6 40.588(19) . . ?
K3 K2 Sn6 122.72(5) 1_455 . ?
Sn2 K2 Sn6 77.65(3) . . ?
N7 K3 N6 93.30(16) . . ?
N7 K3 N5 68.27(15) . . ?
N6 K3 N5 85.28(14) . . ?
N7 K3 N4 136.32(14) . . ?
N6 K3 N4 85.69(14) . . ?
N5 K3 N4 68.14(15) . . ?
N7 K3 Sn8 151.12(11) . . ?
N6 K3 Sn8 105.32(11) . . ?
N5 K3 Sn8 134.02(12) . . ?
N4 K3 Sn8 68.27(9) . . ?
N7 K3 Sn8 70.99(11) . 2_666 ?
N6 K3 Sn8 161.22(11) . 2_666 ?
N5 K3 Sn8 79.43(11) . 2_666 ?
N4 K3 Sn8 98.50(10) . 2_666 ?
Sn8 K3 Sn8 93.19(4) . 2_666 ?
N7 K3 K2 102.02(11) . 1_655 ?
N6 K3 K2 49.29(10) . 1_655 ?
N5 K3 K2 47.85(11) . 1_655 ?
N4 K3 K2 47.04(10) . 1_655 ?
Sn8 K3 K2 106.86(4) . 1_655 ?
Sn8 K3 K2 122.45(4) 2_666 1_655 ?
N7 K3 Zn 94.44(11) . . ?
N6 K3 Zn 72.04(10) . . ?
N5 K3 Zn 150.86(12) . . ?
N4 K3 Zn 126.06(10) . . ?
Sn8 K3 Zn 71.38(3) . . ?
Sn8 K3 Zn 118.16(4) 2_666 . ?
K2 K3 Zn 119.33(4) 1_655 . ?
N7 K3 Sn5 133.04(11) . . ?
N6 K3 Sn5 67.21(10) . . ?
N5 K3 Sn5 144.04(11) . . ?
N4 K3 Sn5 86.43(9) . . ?
Sn8 K3 Sn5 43.705(18) . . ?
Sn8 K3 Sn5 131.10(4) 2_666 . ?
K2 K3 Sn5 96.23(4) 1_655 . ?
Zn K3 Sn5 39.760(18) . . ?
N7 K3 H4A 152.9 . . ?
N6 K3 H4A 87.2 . . ?
N5 K3 H4A 84.8 . . ?
N4 K3 H4A 16.7 . . ?
Sn8 K3 H4A 52.2 . . ?
Sn8 K3 H4A 102.1 2_666 . ?
K2 K3 H4A 58.7 1_655 . ?
Zn K3 H4A 111.4 . . ?
Sn5 K3 H4A 71.7 . . ?
N7 K3 H5B 67.4 . . ?
N6 K3 H5B 102.7 . . ?
N5 K3 H5B 17.5 . . ?
N4 K3 H5B 70.3 . . ?
Sn8 K3 H5B 127.2 . . ?
Sn8 K3 H5B 62.3 2_666 . ?
K2 K3 H5B 62.7 1_655 . ?
Zn K3 H5B 161.1 . . ?
Sn5 K3 H5B 155.6 . . ?
H4A K3 H5B 86.1 . . ?
N7 K3 H6A 78.0 . . ?
N6 K3 H6A 17.4 . . ?
N5 K3 H6A 87.4 . . ?
N4 K3 H6A 102.5 . . ?
Sn8 K3 H6A 115.7 . . ?
Sn8 K3 H6A 148.9 2_666 . ?
K2 K3 H6A 61.9 1_655 . ?
Zn K3 H6A 65.5 . . ?
Sn5 K3 H6A 73.3 . . ?
H4A K3 H6A 104.6 . . ?
H5B K3 H6A 104.0 . . ?
N7 K3 H6C 106.2 . . ?
N6 K3 H6C 17.4 . . ?
N5 K3 H6C 100.8 . . ?
N4 K3 H6C 84.4 . . ?
Sn8 K3 H6C 88.8 . . ?
Sn8 K3 H6C 177.0 2_666 . ?
K2 K3 H6C 58.9 1_655 . ?
Zn K3 H6C 60.4 . . ?
Sn5 K3 H6C 49.9 . . ?
H4A K3 H6C 81.0 . . ?
H5B K3 H6C 118.1 . . ?
H6A K3 H6C 28.4 . . ?
N9 K4 N10 77.09(14) . . ?
N9 K4 N11 112.48(15) . . ?
N10 K4 N11 69.52(14) . . ?
N9 K4 N8 86.30(14) . . ?
N10 K4 N8 87.49(14) . . ?
N11 K4 N8 144.90(16) . . ?
N9 K4 Sn7 152.40(11) . . ?
N10 K4 Sn7 119.68(11) . . ?
N11 K4 Sn7 94.56(11) . . ?
N8 K4 Sn7 73.65(10) . . ?
N9 K4 K5 50.88(10) . 1_565 ?
N10 K4 K5 50.97(10) . 1_565 ?
N11 K4 K5 119.75(10) . 1_565 ?
N8 K4 K5 49.74(10) . 1_565 ?
Sn7 K4 K5 120.37(4) . 1_565 ?
N9 K4 Zn 103.81(10) . . ?
N10 K4 Zn 147.64(10) . . ?
N11 K4 Zn 80.81(10) . . ?
N8 K4 Zn 124.84(11) . . ?
Sn7 K4 Zn 74.14(3) . . ?
K5 K4 Zn 150.83(5) 1_565 . ?
N9 K4 Sn2 69.37(10) . . ?
N10 K4 Sn2 114.30(11) . . ?
N11 K4 Sn2 73.80(11) . . ?
N8 K4 Sn2 141.22(12) . . ?
Sn7 K4 Sn2 115.73(3) . . ?
K5 K4 Sn2 119.81(4) 1_565 . ?
Zn K4 Sn2 41.866(19) . . ?
N9 K4 Sn5 115.43(11) . . ?
N10 K4 Sn5 164.63(11) . . ?
N11 K4 Sn5 110.72(10) . . ?
N8 K4 Sn5 84.63(10) . . ?
Sn7 K4 Sn5 45.250(18) . . ?
K5 K4 Sn5 129.03(4) 1_565 . ?
Zn K4 Sn5 41.703(18) . . ?
Sn2 K4 Sn5 79.66(3) . . ?
N9 K4 Sn6 143.36(10) . . ?
N10 K4 Sn6 129.84(11) . . ?
N11 K4 Sn6 67.07(10) . . ?
N8 K4 Sn6 115.38(10) . . ?
Sn7 K4 Sn6 43.232(17) . . ?
K5 K4 Sn6 163.50(5) 1_565 . ?
Zn K4 Sn6 39.692(17) . . ?
Sn2 K4 Sn6 75.99(2) . . ?
Sn5 K4 Sn6 44.587(16) . . ?
N9 K4 K6 118.98(10) . 1_455 ?
N10 K4 K6 44.66(10) . 1_455 ?
N11 K4 K6 40.87(11) . 1_455 ?
N8 K4 K6 104.30(11) . 1_455 ?
Sn7 K4 K6 84.91(3) . 1_455 ?
K5 K4 K6 91.55(4) 1_565 1_455 ?
Zn K4 K6 115.99(4) . 1_455 ?
Sn2 K4 K6 113.76(3) . 1_455 ?
Sn5 K4 K6 125.23(4) . 1_455 ?
Sn6 K4 K6 85.49(3) . 1_455 ?
N9 K4 K1 68.09(10) . . ?
N10 K4 K1 144.82(11) . . ?
N11 K4 K1 119.23(11) . . ?
N8 K4 K1 94.96(11) . . ?
Sn7 K4 K1 94.47(3) . . ?
K5 K4 K1 106.08(4) 1_565 . ?
Zn K4 K1 45.15(2) . . ?
Sn2 K4 K1 48.56(2) . . ?
Sn5 K4 K1 49.42(2) . . ?
Sn6 K4 K1 80.33(3) . . ?
K6 K4 K1 159.66(4) 1_455 . ?
N9 K4 H8B 101.0 . . ?
N10 K4 H8B 99.4 . . ?
N11 K4 H8B 140.4 . . ?
N8 K4 H8B 17.2 . . ?
Sn7 K4 H8B 56.9 . . ?
K5 K4 H8B 66.8 1_565 . ?
Zn K4 H8B 111.9 . . ?
Sn2 K4 H8B 140.7 . . ?
Sn5 K4 H8B 70.3 . . ?
Sn6 K4 H8B 98.2 . . ?
K6 K4 H8B 104.3 1_455 . ?
K1 K4 H8B 92.2 . . ?
N9 K4 H9B 18.2 . . ?
N10 K4 H9B 91.0 . . ?
N11 K4 H9B 107.6 . . ?
N8 K4 H9B 98.7 . . ?
Sn7 K4 H9B 147.4 . . ?
K5 K4 H9B 68.9 1_565 . ?
Zn K4 H9B 85.8 . . ?
Sn2 K4 H9B 52.0 . . ?
Sn5 K4 H9B 103.3 . . ?
Sn6 K4 H9B 125.2 . . ?
K6 K4 H9B 127.5 1_455 . ?
K1 K4 H9B 53.9 . . ?
H8B K4 H9B 110.6 . . ?
N9 K4 H10C 87.3 . . ?
N10 K4 H10C 17.9 . . ?
N11 K4 H10C 51.7 . . ?
N8 K4 H10C 102.9 . . ?
Sn7 K4 H10C 115.2 . . ?
K5 K4 H10C 68.8 1_565 . ?
Zn K4 H10C 131.2 . . ?
Sn2 K4 H10C 105.5 . . ?
Sn5 K4 H10C 156.7 . . ?
Sn6 K4 H10C 113.7 . . ?
K6 K4 H10C 31.7 1_455 . ?
K1 K4 H10C 148.6 . . ?
H8B K4 H10C 112.2 . . ?
H9B K4 H10C 97.4 . . ?
N9 K4 H11B 120.6 . . ?
N10 K4 H11B 86.7 . . ?
N11 K4 H11B 17.3 . . ?
N8 K4 H11B 150.2 . . ?
Sn7 K4 H11B 84.0 . . ?
K5 K4 H11B 137.1 1_565 . ?
Zn K4 H11B 64.7 . . ?
Sn2 K4 H11B 66.6 . . ?
Sn5 K4 H11B 93.6 . . ?
Sn6 K4 H11B 50.8 . . ?
K6 K4 H11B 53.3 1_455 . ?
K1 K4 H11B 106.4 . . ?
H8B K4 H11B 138.2 . . ?
H9B K4 H11B 110.6 . . ?
H10C K4 H11B 68.8 . . ?
N9 K4 H11C 95.1 . . ?
N10 K4 H11C 65.2 . . ?
N11 K4 H11C 17.5 . . ?
N8 K4 H11C 151.4 . . ?
Sn7 K4 H11C 111.6 . . ?
K5 K4 H11C 110.8 1_565 . ?
Zn K4 H11C 82.6 . . ?
Sn2 K4 H11C 63.7 . . ?
Sn5 K4 H11C 119.7 . . ?
Sn6 K4 H11C 79.6 . . ?
K6 K4 H11C 50.4 1_455 . ?
K1 K4 H11C 112.1 . . ?
H8B K4 H11C 154.6 . . ?
H9B K4 H11C 90.5 . . ?
H10C K4 H11C 48.8 . . ?
H11B K4 H11C 29.2 . . ?
N12 K5 N8 81.48(16) . 1_545 ?
N12 K5 N9 85.70(16) . 1_545 ?
N8 K5 N9 86.70(14) 1_545 1_545 ?
N12 K5 N10 159.28(15) . 1_545 ?
N8 K5 N10 88.16(14) 1_545 1_545 ?
N9 K5 N10 75.78(14) 1_545 1_545 ?
N12 K5 K4 110.31(11) . 1_545 ?
N8 K5 K4 51.42(10) 1_545 1_545 ?
N9 K5 K4 49.70(10) 1_545 1_545 ?
N10 K5 K4 50.13(10) 1_545 1_545 ?
N12 K5 Sn4 122.99(13) . . ?
N8 K5 Sn4 91.15(11) 1_545 . ?
N9 K5 Sn4 150.60(11) 1_545 . ?
N10 K5 Sn4 74.85(10) 1_545 . ?
K4 K5 Sn4 107.90(4) 1_545 . ?
N12 K5 Sn3 77.36(12) . . ?
N8 K5 Sn3 89.07(10) 1_545 . ?
N9 K5 Sn3 162.97(11) 1_545 . ?
N10 K5 Sn3 120.59(11) 1_545 . ?
K4 K5 Sn3 135.62(4) 1_545 . ?
Sn4 K5 Sn3 45.894(19) . . ?
N12 K5 Sn4 71.22(12) . 2 ?
N8 K5 Sn4 150.77(12) 1_545 2 ?
N9 K5 Sn4 81.15(10) 1_545 2 ?
N10 K5 Sn4 114.06(11) 1_545 2 ?
K4 K5 Sn4 129.40(4) 1_545 2 ?
Sn4 K5 Sn4 112.21(3) . 2 ?
Sn3 K5 Sn4 94.84(3) . 2 ?
N12 K5 Sn3 115.06(12) . 2 ?
N8 K5 Sn3 154.39(11) 1_545 2 ?
N9 K5 Sn3 75.83(9) 1_545 2 ?
N10 K5 Sn3 69.64(10) 1_545 2 ?
K4 K5 Sn3 103.16(4) 1_545 2 ?
Sn4 K5 Sn3 94.99(3) . 2 ?
Sn3 K5 Sn3 112.88(3) . 2 ?
Sn4 K5 Sn3 44.889(18) 2 2 ?
N12 K5 K5 101.00(11) . 2 ?
N8 K5 K5 143.99(12) 1_545 2 ?
N9 K5 K5 129.25(11) 1_545 2 ?
N10 K5 K5 97.93(11) 1_545 2 ?
K4 K5 K5 147.98(6) 1_545 2 ?
Sn4 K5 K5 57.06(3) . 2 ?
Sn3 K5 K5 57.28(3) . 2 ?
Sn4 K5 K5 55.15(3) 2 2 ?
Sn3 K5 K5 55.59(3) 2 2 ?
N16 K6 N13 96.64(18) . . ?
N16 K6 N15 74.27(18) . . ?
N13 K6 N15 146.86(18) . . ?
N16 K6 N14 99.87(17) . . ?
N13 K6 N14 80.65(15) . . ?
N15 K6 N14 70.02(16) . . ?
N16 K6 N11 137.18(16) . 1_655 ?
N13 K6 N11 126.15(16) . 1_655 ?
N15 K6 N11 70.11(16) . 1_655 ?
N14 K6 N11 89.69(15) . 1_655 ?
N16 K6 Sn8 70.36(11) . . ?
N13 K6 Sn8 126.49(12) . . ?
N15 K6 Sn8 81.21(12) . . ?
N14 K6 Sn8 151.21(12) . . ?
N11 K6 Sn8 81.30(9) 1_655 . ?
N16 K6 Sn5 108.24(12) . . ?
N13 K6 Sn5 101.20(13) . . ?
N15 K6 Sn5 111.93(13) . . ?
N14 K6 Sn5 151.32(13) . . ?
N11 K6 Sn5 65.88(9) 1_655 . ?
Sn8 K6 Sn5 43.748(18) . . ?
N16 K6 Sn7 72.56(12) . . ?
N13 K6 Sn7 82.65(11) . . ?
N15 K6 Sn7 122.56(12) . . ?
N14 K6 Sn7 160.72(12) . . ?
N11 K6 Sn7 108.01(9) 1_655 . ?
Sn8 K6 Sn7 43.849(18) . . ?
Sn5 K6 Sn7 42.798(18) . . ?
N16 K6 K4 145.39(13) . 1_655 ?
N13 K6 K4 103.03(12) . 1_655 ?
N15 K6 K4 73.70(12) . 1_655 ?
N14 K6 K4 56.62(12) . 1_655 ?
N11 K6 K4 35.70(8) 1_655 1_655 ?
Sn8 K6 K4 116.75(4) . 1_655 ?
Sn5 K6 K4 95.62(4) . 1_655 ?
Sn7 K6 K4 137.63(4) . 1_655 ?
K1 N1 K1 78.66(14) 2_665 . ?
K1 N1 H1A 85.0 2_665 . ?
K1 N1 H1A 126.8 . . ?
K1 N1 H1B 148.7 2_665 . ?
K1 N1 H1B 70.5 . . ?
H1A N1 H1B 109.5 . . ?
K1 N1 H1C 90.2 2_665 . ?
K1 N1 H1C 120.7 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
K1 N2 H2A 109.5 . . ?
K1 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
K1 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
K2 N3 H3A 109.5 . . ?
K2 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
K2 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
K2 N4 K3 78.74(13) 1_655 . ?
K2 N4 H4A 121.8 1_655 . ?
K3 N4 H4A 71.5 . . ?
K2 N4 H4B 73.2 1_655 . ?
K3 N4 H4B 147.1 . . ?
H4A N4 H4B 109.5 . . ?
K2 N4 H4C 124.6 1_655 . ?
K3 N4 H4C 100.4 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
K2 N5 K3 80.94(13) 1_655 . ?
K2 N5 H5A 111.5 1_655 . ?
K3 N5 H5A 106.1 . . ?
K2 N5 H5B 134.2 1_655 . ?
K3 N5 H5B 68.8 . . ?
H5A N5 H5B 109.5 . . ?
K2 N5 H5C 74.8 1_655 . ?
K3 N5 H5C 142.3 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
K2 N6 K3 80.63(13) 1_655 . ?
K2 N6 H6A 129.3 1_655 . ?
K3 N6 H6A 83.5 . . ?
K2 N6 H6B 74.5 1_655 . ?
K3 N6 H6B 154.8 . . ?
H6A N6 H6B 109.5 . . ?
K2 N6 H6C 116.6 1_655 . ?
K3 N6 H6C 84.8 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
K3 N7 H7A 109.5 . . ?
K3 N7 H7B 109.5 . . ?
H7A N7 H7B 109.5 . . ?
K3 N7 H7C 109.5 . . ?
H7A N7 H7C 109.5 . . ?
H7B N7 H7C 109.5 . . ?
K5 N8 K4 78.84(12) 1_565 . ?
K5 N8 H8A 97.9 1_565 . ?
K4 N8 H8A 121.0 . . ?
K5 N8 H8B 137.5 1_565 . ?
K4 N8 H8B 59.4 . . ?
H8A N8 H8B 109.5 . . ?
K5 N8 H8C 90.1 1_565 . ?
K4 N8 H8C 129.3 . . ?
H8A N8 H8C 109.5 . . ?
H8B N8 H8C 109.5 . . ?
K4 N9 K5 79.42(13) . 1_565 ?
K4 N9 H9A 120.0 . . ?
K5 N9 H9A 92.5 1_565 . ?
K4 N9 H9B 70.6 . . ?
K5 N9 H9B 148.8 1_565 . ?
H9A N9 H9B 109.5 . . ?
K4 N9 H9C 127.5 . . ?
K5 N9 H9C 82.1 1_565 . ?
H9A N9 H9C 109.5 . . ?
H9B N9 H9C 109.5 . . ?
K4 N10 K5 78.91(13) . 1_565 ?
K4 N10 H10A 132.8 . . ?
K5 N10 H10A 80.9 1_565 . ?
K4 N10 H10B 110.5 . . ?
K5 N10 H10B 84.6 1_565 . ?
H10A N10 H10B 109.5 . . ?
K4 N10 H10C 79.4 . . ?
K5 N10 H10C 157.2 1_565 . ?
H10A N10 H10C 109.5 . . ?
H10B N10 H10C 109.5 . . ?
K4 N11 K6 103.43(15) . 1_455 ?
K4 N11 H11A 166.1 . . ?
K6 N11 H11A 68.6 1_455 . ?
K4 N11 H11B 84.4 . . ?
K6 N11 H11B 129.8 1_455 . ?
H11A N11 H11B 109.5 . . ?
K4 N11 H11C 63.5 . . ?
K6 N11 H11C 118.5 1_455 . ?
H11A N11 H11C 109.5 . . ?
H11B N11 H11C 109.5 . . ?
K5 N12 H12A 109.5 . . ?
K5 N12 H12B 109.5 . . ?
H12A N12 H12B 109.5 . . ?
K5 N12 H12C 109.5 . . ?
H12A N12 H12C 109.5 . . ?
H12B N12 H12C 109.5 . . ?
K6 N13 H13A 109.5 . . ?
K6 N13 H13B 109.5 . . ?
H13A N13 H13B 109.5 . . ?
K6 N13 H13C 109.5 . . ?
H13A N13 H13C 109.5 . . ?
H13B N13 H13C 109.5 . . ?
K6 N14 H14A 109.5 . . ?
K6 N14 H14B 109.5 . . ?
H14A N14 H14B 109.5 . . ?
K6 N14 H14C 109.5 . . ?
H14A N14 H14C 109.5 . . ?
H14B N14 H14C 109.5 . . ?
K6 N15 H15A 109.5 . . ?
K6 N15 H15B 109.5 . . ?
H15A N15 H15B 109.5 . . ?
K6 N15 H15C 109.5 . . ?
H15A N15 H15C 109.5 . . ?
H15B N15 H15C 109.5 . . ?
K6 N16 H16A 109.5 . . ?
K6 N16 H16B 109.5 . . ?
H16A N16 H16B 109.5 . . ?
K6 N16 H16C 109.5 . . ?
H16A N16 H16C 109.5 . . ?
H16B N16 H16C 109.5 . . ?

_refine_diff_density_max         1.311
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.194


#============================================================================== 
# END of CIF  
#============================================================================== 
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ammonia'
####################################################################### 
# 
# 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_TH223
_database_code_depnum_ccdc_archive 'CCDC 1982125'
loop_
_audit_author_name
_audit_author_address
'Wilhelm Klein'
;Technische Universitaet Muenchen
Germany
;
_audit_update_record             
;
2020-02-05 deposited with the CCDC.	2020-04-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C24 H24 N2 Zn2, 2(C12 H30 K N2 O6), 4 (H3 N)'
_chemical_formula_sum            'C48 H96 K2 N10 O12 Zn2'
_chemical_formula_weight         1214.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.963(5)
_cell_length_b                   12.328(5)
_cell_length_c                   12.683(6)
_cell_angle_alpha                107.43(4)
_cell_angle_beta                 106.66(4)
_cell_angle_gamma                104.16(3)
_cell_volume                     1594.0(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    10446
_cell_measurement_theta_min      2.752
_cell_measurement_theta_max      32.939

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98132
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d 
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Xcalibur 3'
_diffrn_measurement_method       'ω and π scans'
_diffrn_detector_area_resol_mean 16.0238
_diffrn_reflns_number            16857
_diffrn_reflns_av_unetI/netI     0.1765
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.752
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6272
_reflns_number_gt                3177
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_computing_data_collection       
; 
 CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.34d 
;
_computing_cell_refinement       
; 
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d 
;
_computing_data_reduction        
; 
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d 
;
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  SHELXL-2014/7
_computing_molecular_graphics    'DIAMOND 3.2k'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0476P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6272
_refine_ls_number_parameters     344
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0510
_refine_ls_wR_factor_ref         0.1106
_refine_ls_wR_factor_gt          0.1003
_refine_ls_goodness_of_fit_ref   0.768
_refine_ls_restrained_S_all      0.768
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K K 0.01071(9) 0.20026(9) 0.79208(9) 0.0454(3) Uani 1 1 d . . . . .
O1 O 0.2051(2) 0.4008(2) 0.8191(3) 0.0335(7) Uani 1 1 d . . . . .
O2 O 0.0096(2) 0.2545(3) 0.5899(3) 0.0386(8) Uani 1 1 d . . . . .
O3 O -0.1521(3) 0.0328(3) 0.5646(3) 0.0467(9) Uani 1 1 d . . . . .
O4 O -0.1945(3) 0.0154(3) 0.7665(3) 0.0491(9) Uani 1 1 d . . . . .
O5 O -0.0088(3) 0.1666(3) 0.9979(3) 0.0663(11) Uani 1 1 d . . . . .
O6 O 0.1596(2) 0.3827(3) 1.0210(3) 0.0413(8) Uani 1 1 d . . . . .
C1 C 0.1822(4) 0.4371(4) 0.7218(4) 0.0387(12) Uani 1 1 d . . . . .
H1A H 0.2612 0.4939 0.7291 0.046 Uiso 1 1 calc R U . . .
H1B H 0.1225 0.4803 0.7231 0.046 Uiso 1 1 calc R U . . .
C2 C 0.1294(4) 0.3284(4) 0.6065(4) 0.0421(12) Uani 1 1 d . . . . .
H2A H 0.1227 0.3547 0.5392 0.050 Uiso 1 1 calc R U . . .
H2B H 0.1855 0.2811 0.6078 0.050 Uiso 1 1 calc R U . . .
C3 C -0.0439(4) 0.1487(5) 0.4822(4) 0.0620(16) Uani 1 1 d . . . . .
H3A H 0.0109 0.1002 0.4831 0.074 Uiso 1 1 calc R U . . .
H3B H -0.0533 0.1719 0.4127 0.074 Uiso 1 1 calc R U . . .
C4 C -0.1687(4) 0.0755(5) 0.4721(5) 0.0658(17) Uani 1 1 d . . . . .
H4A H -0.2208 0.1266 0.4785 0.079 Uiso 1 1 calc R U . . .
H4B H -0.2122 0.0057 0.3931 0.079 Uiso 1 1 calc R U . . .
C5 C -0.2661(4) -0.0452(4) 0.5565(5) 0.0542(15) Uani 1 1 d . . . . .
H5A H -0.3059 -0.1163 0.4785 0.065 Uiso 1 1 calc R U . . .
H5B H -0.3243 -0.0008 0.5617 0.065 Uiso 1 1 calc R U . . .
C6 C -0.2394(5) -0.0868(4) 0.6563(6) 0.0631(17) Uani 1 1 d . . . . .
H6A H -0.3165 -0.1481 0.6471 0.076 Uiso 1 1 calc R U . . .
H6B H -0.1758 -0.1252 0.6552 0.076 Uiso 1 1 calc R U . . .
C7 C -0.1798(6) -0.0168(6) 0.8664(6) 0.107(3) Uani 1 1 d . . . . .
H7A H -0.1202 -0.0601 0.8726 0.129 Uiso 1 1 calc R U . . .
H7B H -0.2612 -0.0720 0.8564 0.129 Uiso 1 1 calc R U . . .
C8 C -0.1322(5) 0.0957(7) 0.9770(5) 0.112(3) Uani 1 1 d . . . . .
H8A H -0.1873 0.1433 0.9676 0.135 Uiso 1 1 calc R U . . .
H8B H -0.1317 0.0740 1.0462 0.135 Uiso 1 1 calc R U . . .
C9 C 0.0439(5) 0.2745(5) 1.1038(5) 0.0618(16) Uani 1 1 d . . . . .
H9A H 0.0490 0.2537 1.1741 0.074 Uiso 1 1 calc R U . . .
H9B H -0.0093 0.3244 1.0987 0.074 Uiso 1 1 calc R U . . .
C10 C 0.1719(4) 0.3449(5) 1.1175(4) 0.0507(13) Uani 1 1 d . . . . .
H10A H 0.2135 0.4169 1.1949 0.061 Uiso 1 1 calc R U . . .
H10B H 0.2235 0.2931 1.1164 0.061 Uiso 1 1 calc R U . . .
C11 C 0.2762(4) 0.4568(4) 1.0298(4) 0.0452(13) Uani 1 1 d . . . . .
H11A H 0.3314 0.4090 1.0239 0.054 Uiso 1 1 calc R U . . .
H11B H 0.3179 0.5272 1.1083 0.054 Uiso 1 1 calc R U . . .
C12 C 0.2544(4) 0.5004(4) 0.9316(4) 0.0427(12) Uani 1 1 d . . . . .
H12A H 0.1949 0.5436 0.9347 0.051 Uiso 1 1 calc R U . . .
H12B H 0.3341 0.5585 0.9418 0.051 Uiso 1 1 calc R U . . .
N2 N 0.1946(4) 0.0819(4) 0.8349(3) 0.0602(12) Uani 1 1 d . . . . .
H2C H 0.2307 0.1007 0.9148 0.090 Uiso 1 1 calc R U . . .
H2D H 0.2545 0.1086 0.8081 0.090 Uiso 1 1 calc R U . . .
H2E H 0.1555 -0.0004 0.7949 0.090 Uiso 1 1 calc R U . . .
N3 N -0.1029(3) 0.3781(4) 0.8243(4) 0.0717(14) Uani 1 1 d . . . . .
H3C H -0.0685 0.4304 0.9028 0.107 Uiso 1 1 calc R U . . .
H3D H -0.1866 0.3405 0.8021 0.107 Uiso 1 1 calc R U . . .
H3E H -0.0902 0.4203 0.7783 0.107 Uiso 1 1 calc R U . . .
Zn Zn 0.52347(4) 0.38583(4) 0.49345(5) 0.02552(15) Uani 1 1 d . . . . .
N1 N 0.3658(3) 0.4364(3) 0.4515(4) 0.0266(9) Uani 1 1 d . . . . .
H1C H 0.335(3) 0.417(3) 0.492(3) 0.004(11) Uiso 1 1 d . . . . .
H1D H 0.328(3) 0.393(3) 0.379(3) 0.016(11) Uiso 1 1 d . . . . .
C13 C 0.5228(3) 0.2831(3) 0.3331(4) 0.0280(10) Uani 1 1 d . . . . .
C14 C 0.4985(3) 0.3190(4) 0.2367(4) 0.0297(10) Uani 1 1 d . . . . .
H14 H 0.4868 0.3948 0.2503 0.036 Uiso 1 1 calc R U . . .
C15 C 0.4901(4) 0.2535(4) 0.1240(4) 0.0423(12) Uani 1 1 d . . . . .
H15 H 0.4712 0.2828 0.0623 0.051 Uiso 1 1 calc R U . . .
C16 C 0.5093(7) 0.1456(5) 0.1024(5) 0.084(2) Uani 1 1 d . . . . .
H16 H 0.5064 0.0996 0.0261 0.101 Uiso 1 1 calc R U . . .
C17 C 0.5329(7) 0.1048(5) 0.1935(5) 0.093(2) Uani 1 1 d . . . . .
H17 H 0.5444 0.0289 0.1785 0.112 Uiso 1 1 calc R U . . .
C18 C 0.5404(5) 0.1715(4) 0.3058(4) 0.0518(14) Uani 1 1 d . . . . .
H18 H 0.5580 0.1407 0.3665 0.062 Uiso 1 1 calc R U . . .
C19 C 0.5267(3) 0.3196(3) 0.6227(4) 0.0267(10) Uani 1 1 d . . . . .
C20 C 0.5855(4) 0.2386(4) 0.6450(4) 0.0282(10) Uani 1 1 d . . . . .
H20 H 0.6344 0.2177 0.6005 0.034 Uiso 1 1 calc R U . . .
C21 C 0.5778(4) 0.1871(4) 0.7266(4) 0.0372(11) Uani 1 1 d . . . . .
H21 H 0.6203 0.1328 0.7365 0.045 Uiso 1 1 calc R U . . .
C22 C 0.5081(4) 0.2148(4) 0.7940(4) 0.0358(11) Uani 1 1 d . . . . .
H22 H 0.5025 0.1802 0.8508 0.043 Uiso 1 1 calc R U . . .
C23 C 0.4466(4) 0.2939(4) 0.7771(4) 0.0305(10) Uani 1 1 d . . . . .
H23 H 0.3977 0.3137 0.8219 0.037 Uiso 1 1 calc R U . . .
C24 C 0.4569(3) 0.3434(3) 0.6947(4) 0.0266(10) Uani 1 1 d . . . . .
H24 H 0.4140 0.3976 0.6855 0.032 Uiso 1 1 calc R U . . .
N4 N 0.1212(4) 0.5403(4) 0.4299(5) 0.104(2) Uani 1 1 d . . . . .
H4C H 0.1023 0.6045 0.4244 0.156 Uiso 1 1 d R U . . .
H4D H 0.1024 0.5238 0.4881 0.156 Uiso 1 1 d R U . . .
H4E H 0.0772 0.4763 0.3601 0.156 Uiso 1 1 d R U . . .
N5 N 0.1582(6) 0.7456(6) 0.7354(7) 0.149(3) Uani 1 1 d . . . . .
H5C H 0.1825 0.7131 0.7882 0.224 Uiso 1 1 d R U . . .
H5D H 0.2155 0.8186 0.7586 0.224 Uiso 1 1 d R U . . .
H5E H 0.0850 0.7532 0.7320 0.224 Uiso 1 1 d R U . . .


_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
K O3 2.761(4) . ?
K O4 2.773(3) . ?
K O6 2.797(4) . ?
K O1 2.803(3) . ?
K O5 2.827(4) . ?
K O2 2.834(3) . ?
K N3 2.839(4) . ?
K N2 2.937(4) . ?
O1 C1 1.414(5) . ?
O1 C12 1.416(5) . ?
O2 C3 1.414(5) . ?
O2 C2 1.414(5) . ?
O3 C4 1.407(6) . ?
O3 C5 1.419(5) . ?
O4 C7 1.415(6) . ?
O4 C6 1.419(6) . ?
O5 C9 1.416(6) . ?
O5 C8 1.420(6) . ?
O6 C10 1.417(5) . ?
O6 C11 1.421(5) . ?
C1 C2 1.489(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.491(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.486(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.486(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.495(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.480(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
N2 H2C 0.9100 . ?
N2 H2D 0.9100 . ?
N2 H2E 0.9100 . ?
N3 H3C 0.9100 . ?
N3 H3D 0.9100 . ?
N3 H3E 0.9100 . ?
Zn C19 2.034(4) . ?
Zn N1 2.045(4) 2_666 ?
Zn C13 2.046(4) . ?
Zn N1 2.104(4) . ?
Zn Zn 2.9686(15) 2_666 ?
N1 Zn 2.045(4) 2_666 ?
N1 H1C 0.78(3) . ?
N1 H1D 0.83(4) . ?
C13 C18 1.398(6) . ?
C13 C14 1.399(5) . ?
C14 C15 1.376(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.365(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.378(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.380(6) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.404(5) . ?
C19 C24 1.419(5) . ?
C20 C21 1.380(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.384(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.387(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.378(5) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
N4 H4C 0.8913 . ?
N4 H4D 0.8941 . ?
N4 H4E 0.8913 . ?
N5 H5C 0.8943 . ?
N5 H5D 0.8894 . ?
N5 H5E 0.8931 . ?

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
O3 K O4 60.97(11) . . ?
O3 K O6 174.33(10) . . ?
O4 K O6 118.38(11) . . ?
O3 K O1 119.47(11) . . ?
O4 K O1 174.78(9) . . ?
O6 K O1 60.59(10) . . ?
O3 K O5 120.97(11) . . ?
O4 K O5 60.58(11) . . ?
O6 K O5 59.59(10) . . ?
O1 K O5 119.50(11) . . ?
O3 K O2 60.06(10) . . ?
O4 K O2 118.56(11) . . ?
O6 K O2 118.50(10) . . ?
O1 K O2 60.52(10) . . ?
O5 K O2 171.96(11) . . ?
O3 K N3 100.64(11) . . ?
O4 K N3 94.23(12) . . ?
O6 K N3 73.71(11) . . ?
O1 K N3 80.56(11) . . ?
O5 K N3 91.12(13) . . ?
O2 K N3 80.93(12) . . ?
O3 K N2 98.70(11) . . ?
O4 K N2 97.65(11) . . ?
O6 K N2 86.97(11) . . ?
O1 K N2 87.46(11) . . ?
O5 K N2 81.36(12) . . ?
O2 K N2 106.55(10) . . ?
N3 K N2 160.45(12) . . ?
C1 O1 C12 112.7(3) . . ?
C1 O1 K 115.0(2) . . ?
C12 O1 K 114.5(2) . . ?
C3 O2 C2 111.6(3) . . ?
C3 O2 K 112.5(3) . . ?
C2 O2 K 112.5(2) . . ?
C4 O3 C5 112.7(4) . . ?
C4 O3 K 116.7(3) . . ?
C5 O3 K 115.9(3) . . ?
C7 O4 C6 113.0(4) . . ?
C7 O4 K 115.0(3) . . ?
C6 O4 K 112.1(3) . . ?
C9 O5 C8 112.2(5) . . ?
C9 O5 K 115.0(3) . . ?
C8 O5 K 112.8(3) . . ?
C10 O6 C11 112.5(3) . . ?
C10 O6 K 115.8(3) . . ?
C11 O6 K 113.9(3) . . ?
O1 C1 C2 110.0(4) . . ?
O1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
O1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
O2 C2 C1 109.4(3) . . ?
O2 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
O2 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
O2 C3 C4 108.3(4) . . ?
O2 C3 H3A 110.0 . . ?
C4 C3 H3A 110.0 . . ?
O2 C3 H3B 110.0 . . ?
C4 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
O3 C4 C3 109.1(4) . . ?
O3 C4 H4A 109.9 . . ?
C3 C4 H4A 109.9 . . ?
O3 C4 H4B 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
O3 C5 C6 109.0(4) . . ?
O3 C5 H5A 109.9 . . ?
C6 C5 H5A 109.9 . . ?
O3 C5 H5B 109.9 . . ?
C6 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
O4 C6 C5 108.7(4) . . ?
O4 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
O4 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
O4 C7 C8 109.0(5) . . ?
O4 C7 H7A 109.9 . . ?
C8 C7 H7A 109.9 . . ?
O4 C7 H7B 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
O5 C8 C7 109.0(6) . . ?
O5 C8 H8A 109.9 . . ?
C7 C8 H8A 109.9 . . ?
O5 C8 H8B 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
O5 C9 C10 108.8(4) . . ?
O5 C9 H9A 109.9 . . ?
C10 C9 H9A 109.9 . . ?
O5 C9 H9B 109.9 . . ?
C10 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
O6 C10 C9 108.1(4) . . ?
O6 C10 H10A 110.1 . . ?
C9 C10 H10A 110.1 . . ?
O6 C10 H10B 110.1 . . ?
C9 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
O6 C11 C12 109.2(4) . . ?
O6 C11 H11A 109.8 . . ?
C12 C11 H11A 109.8 . . ?
O6 C11 H11B 109.8 . . ?
C12 C11 H11B 109.8 . . ?
H11A C11 H11B 108.3 . . ?
O1 C12 C11 110.2(4) . . ?
O1 C12 H12A 109.6 . . ?
C11 C12 H12A 109.6 . . ?
O1 C12 H12B 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
K N2 H2C 109.5 . . ?
K N2 H2D 109.5 . . ?
H2C N2 H2D 109.5 . . ?
K N2 H2E 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?
K N3 H3C 109.5 . . ?
K N3 H3D 109.5 . . ?
H3C N3 H3D 109.5 . . ?
K N3 H3E 109.5 . . ?
H3C N3 H3E 109.5 . . ?
H3D N3 H3E 109.5 . . ?
C19 Zn N1 116.97(17) . 2_666 ?
C19 Zn C13 120.96(16) . . ?
N1 Zn C13 109.82(17) 2_666 . ?
C19 Zn N1 108.79(17) . . ?
N1 Zn N1 88.64(15) 2_666 . ?
C13 Zn N1 106.18(17) . . ?
C19 Zn Zn 122.73(11) . 2_666 ?
N1 Zn Zn 45.13(10) 2_666 2_666 ?
C13 Zn Zn 115.53(12) . 2_666 ?
N1 Zn Zn 43.51(11) . 2_666 ?
Zn N1 Zn 91.36(15) 2_666 . ?
Zn N1 H1C 120(3) 2_666 . ?
Zn N1 H1C 101(3) . . ?
Zn N1 H1D 120(3) 2_666 . ?
Zn N1 H1D 101(2) . . ?
H1C N1 H1D 115(4) . . ?
C18 C13 C14 113.6(4) . . ?
C18 C13 Zn 125.5(3) . . ?
C14 C13 Zn 120.9(3) . . ?
C15 C14 C13 125.3(4) . . ?
C15 C14 H14 117.4 . . ?
C13 C14 H14 117.4 . . ?
C16 C15 C14 118.9(5) . . ?
C16 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
C15 C16 C17 118.7(5) . . ?
C15 C16 H16 120.7 . . ?
C17 C16 H16 120.7 . . ?
C16 C17 C18 121.6(5) . . ?
C16 C17 H17 119.2 . . ?
C18 C17 H17 119.2 . . ?
C17 C18 C13 122.0(4) . . ?
C17 C18 H18 119.0 . . ?
C13 C18 H18 119.0 . . ?
C20 C19 C24 112.0(4) . . ?
C20 C19 Zn 126.0(3) . . ?
C24 C19 Zn 121.7(3) . . ?
C21 C20 C19 125.0(4) . . ?
C21 C20 H20 117.5 . . ?
C19 C20 H20 117.5 . . ?
C20 C21 C22 119.9(4) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
C21 C22 C23 118.8(4) . . ?
C21 C22 H22 120.6 . . ?
C23 C22 H22 120.6 . . ?
C24 C23 C22 119.5(4) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C23 C24 C19 124.9(4) . . ?
C23 C24 H24 117.6 . . ?
C19 C24 H24 117.6 . . ?
H4C N4 H4D 109.5 . . ?
H4C N4 H4E 109.1 . . ?
H4D N4 H4E 109.7 . . ?
H5C N5 H5D 109.3 . . ?
H5C N5 H5E 109.5 . . ?
H5D N5 H5E 109.5 . . ?

_refine_diff_density_max         0.913
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.080


#============================================================================== 
# END of CIF 
#============================================================================== 
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ammonia'
####################################################################### 
# 
# 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_TH270
_database_code_depnum_ccdc_archive 'CCDC 1982126'
loop_
_audit_author_name
_audit_author_address
'Wilhelm Klein'
;Technische Universitaet Muenchen
Germany
;
_audit_update_record             
;
2020-02-05 deposited with the CCDC.	2020-04-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

# start Validation Reply Form
_vrf_RINTA01_TH270               
;
PROBLEM: The value of Rint is greater than 0.18 
RESPONSE: Unfortunately, all measured crystals showed weak reflection
 intensities at high 2Theta angles. The enlarged Rint should be a
 manifestation of this. 
;
_vrf_PLAT026_TH270               
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        32% Check 
RESPONSE:  Unfortunately, all measured crystals showed weak reflection
 intensities at high 2Theta angles. Therefore, the amount of observed
 reflections is low. 
;
_vrf_PLAT341_TH270               
;
PROBLEM: Low Bond Precision on C-C Bonds ...............      0.02242 Ang. 
RESPONSE:  The low precision is a result of the weak reflection intensities
 at high 2Theta angles. 
;
# end Validation Reply Form

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C12 H24 K0.84 O6 Rb0.16, C18 H15 Zn'
_chemical_formula_sum            'C30 H39 K0.84 O6 Rb0.16 Zn'
_chemical_formula_weight         607.38

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'
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'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z'

_cell_length_a                   21.842(2)
_cell_length_b                   7.2588(15)
_cell_length_c                   18.322(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2904.9(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    1926
_cell_measurement_theta_min      2.7849
_cell_measurement_theta_max      32.9746

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_F_000             1275
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    1.269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.54108
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d 
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Xcalibur 3'
_diffrn_measurement_method       'ω and π scans'
_diffrn_detector_area_resol_mean 16.0238
_diffrn_reflns_number            30260
_diffrn_reflns_av_unetI/netI     0.3101
_diffrn_reflns_av_R_equivalents  0.1990
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.902
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5705
_reflns_number_gt                1847
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
; 
 CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.34d 
;
_computing_cell_refinement       
; 
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d 
;
_computing_data_reduction        
; 
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d 
;
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  SHELXL-2014/7
_computing_molecular_graphics    'DIAMOND 3.2k'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0328P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 570 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5705
_refine_ls_number_parameters     343
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.1647
_refine_ls_R_factor_gt           0.0540
_refine_ls_wR_factor_ref         0.1059
_refine_ls_wR_factor_gt          0.0902
_refine_ls_goodness_of_fit_ref   0.655
_refine_ls_restrained_S_all      0.680
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K K 0.37656(10) 0.5763(4) 0.5000 0.0583(12) Uani 0.843(7) 1 d . . P . .
Rb Rb 0.37656(10) 0.5763(4) 0.5000 0.0583(12) Uani 0.157(7) 1 d . . P . .
O1 O 0.2912(7) 0.5501(16) 0.6190(7) 0.083(4) Uani 1 1 d . . . . .
O2 O 0.4130(6) 0.6549(14) 0.6406(6) 0.084(4) Uani 1 1 d . U . . .
O3 O 0.5018(4) 0.5906(15) 0.5304(8) 0.077(4) Uani 1 1 d . . . . .
O4 O 0.4578(5) 0.6039(12) 0.3813(6) 0.073(3) Uani 1 1 d . . . . .
O5 O 0.3333(6) 0.4833(14) 0.3615(6) 0.076(4) Uani 1 1 d . . . . .
O6 O 0.2502(4) 0.5450(14) 0.4749(7) 0.072(4) Uani 1 1 d . . . . .
C1 C 0.3105(9) 0.662(2) 0.6757(10) 0.104(7) Uani 1 1 d . U . . .
H1A H 0.2827 0.6466 0.7179 0.125 Uiso 1 1 calc R U . . .
H1B H 0.3086 0.7925 0.6600 0.125 Uiso 1 1 calc R U . . .
C2 C 0.3726(9) 0.618(2) 0.6977(11) 0.104(7) Uani 1 1 d . U . . .
H2A H 0.3840 0.6926 0.7409 0.124 Uiso 1 1 calc R U . . .
H2B H 0.3752 0.4864 0.7112 0.124 Uiso 1 1 calc R U . . .
C3 C 0.4735(11) 0.636(3) 0.6526(12) 0.123(9) Uani 1 1 d . U . . .
H3A H 0.4818 0.5058 0.6646 0.148 Uiso 1 1 calc R U . . .
H3B H 0.4844 0.7106 0.6961 0.148 Uiso 1 1 calc R U . . .
C4 C 0.5151(7) 0.692(2) 0.5910(15) 0.103(7) Uani 1 1 d . U . . .
H4A H 0.5097 0.8248 0.5803 0.124 Uiso 1 1 calc R U . . .
H4B H 0.5583 0.6717 0.6053 0.124 Uiso 1 1 calc R U . . .
C5 C 0.5352(6) 0.652(2) 0.4688(10) 0.083(6) Uani 1 1 d . U . . .
H5A H 0.5793 0.6283 0.4769 0.100 Uiso 1 1 calc R U . . .
H5B H 0.5295 0.7863 0.4632 0.100 Uiso 1 1 calc R U . . .
C6 C 0.5154(7) 0.558(2) 0.4002(9) 0.089(6) Uani 1 1 d . U . . .
H6A H 0.5437 0.5915 0.3601 0.107 Uiso 1 1 calc R U . . .
H6B H 0.5179 0.4225 0.4071 0.107 Uiso 1 1 calc R U . . .
C7 C 0.4343(8) 0.517(3) 0.3169(8) 0.079(6) Uani 1 1 d . U . . .
H7A H 0.4427 0.3829 0.3198 0.094 Uiso 1 1 calc R U . . .
H7B H 0.4563 0.5657 0.2739 0.094 Uiso 1 1 calc R U . . .
C8 C 0.3675(9) 0.544(2) 0.3058(10) 0.094(7) Uani 1 1 d . U . . .
H8A H 0.3594 0.6770 0.2986 0.112 Uiso 1 1 calc R U . . .
H8B H 0.3548 0.4790 0.2608 0.112 Uiso 1 1 calc R U . . .
C9 C 0.2686(8) 0.505(3) 0.3522(11) 0.089(6) Uani 1 1 d . U . . .
H9A H 0.2587 0.6369 0.3451 0.107 Uiso 1 1 calc R U . . .
H9B H 0.2550 0.4365 0.3085 0.107 Uiso 1 1 calc R U . . .
C10 C 0.2379(8) 0.437(2) 0.4149(12) 0.102(7) Uani 1 1 d . . . . .
H10A H 0.1932 0.4359 0.4058 0.123 Uiso 1 1 calc R U . . .
H10B H 0.2511 0.3091 0.4247 0.123 Uiso 1 1 calc R U . . .
C11 C 0.2156(7) 0.494(3) 0.5371(12) 0.090(8) Uani 1 1 d . U . . .
H11A H 0.2212 0.3614 0.5468 0.108 Uiso 1 1 calc R U . . .
H11B H 0.1716 0.5160 0.5272 0.108 Uiso 1 1 calc R U . . .
C12 C 0.2333(10) 0.597(3) 0.6001(13) 0.105(7) Uani 1 1 d . U . . .
H12A H 0.2311 0.7304 0.5895 0.127 Uiso 1 1 calc R U . . .
H12B H 0.2050 0.5697 0.6409 0.127 Uiso 1 1 calc R U . . .
Zn Zn 0.46561(5) 0.0014(3) 0.33874(17) 0.0398(3) Uani 1 1 d . . . . .
C13 C 0.4172(6) -0.006(2) 0.2453(8) 0.033(4) Uani 1 1 d . . . . .
C14 C 0.4333(6) -0.1002(19) 0.1801(9) 0.035(4) Uani 1 1 d . . . . .
H14 H 0.4695 -0.1729 0.1804 0.041 Uiso 1 1 calc R U . . .
C15 C 0.3993(7) -0.093(2) 0.1159(8) 0.046(4) Uani 1 1 d . . . . .
H15 H 0.4118 -0.1603 0.0741 0.055 Uiso 1 1 calc R U . . .
C16 C 0.3479(7) 0.013(2) 0.1141(8) 0.043(4) Uani 1 1 d . . . . .
H16 H 0.3255 0.0229 0.0697 0.051 Uiso 1 1 calc R U . . .
C17 C 0.3280(6) 0.1041(19) 0.1733(9) 0.041(4) Uani 1 1 d . . . . .
H17 H 0.2916 0.1756 0.1713 0.049 Uiso 1 1 calc R U . . .
C18 C 0.3615(6) 0.092(2) 0.2377(8) 0.039(4) Uani 1 1 d . . . . .
H18 H 0.3459 0.1531 0.2795 0.047 Uiso 1 1 calc R U . . .
C19 C 0.4168(7) 0.043(2) 0.4308(9) 0.038(5) Uani 1 1 d . . . . .
C20 C 0.3555(6) -0.005(2) 0.4332(7) 0.037(4) Uani 1 1 d . . . . .
H20 H 0.3376 -0.0534 0.3913 0.045 Uiso 1 1 d R U . . .
C21 C 0.3185(5) 0.0193(17) 0.4945(8) 0.044(4) Uani 1 1 d . . . . .
H21 H 0.2782 -0.0216 0.4933 0.052 Uiso 1 1 d R U . . .
C22 C 0.3408(7) 0.100(2) 0.5573(8) 0.040(4) Uani 1 1 d . . . . .
H22 H 0.3162 0.1188 0.5982 0.048 Uiso 1 1 d R U . . .
C23 C 0.4013(8) 0.156(2) 0.5555(8) 0.052(5) Uani 1 1 d . . . . .
H23 H 0.4184 0.2115 0.5965 0.063 Uiso 1 1 d R U . . .
C24 C 0.4362(6) 0.1259(19) 0.4932(9) 0.043(4) Uani 1 1 d . . . . .
H24 H 0.4766 0.1667 0.4938 0.052 Uiso 1 1 d R U . . .
C25 C 0.5585(4) 0.001(2) 0.3357(11) 0.031(2) Uani 1 1 d . . . . .
C26 C 0.5952(7) 0.0826(19) 0.3895(9) 0.039(4) Uani 1 1 d . . . . .
H26 H 0.5760 0.1406 0.4300 0.047 Uiso 1 1 calc R U . . .
C27 C 0.6589(7) 0.081(2) 0.3858(9) 0.042(4) Uani 1 1 d . . . . .
H27 H 0.6818 0.1425 0.4226 0.050 Uiso 1 1 calc R U . . .
C28 C 0.6887(5) -0.005(2) 0.3310(13) 0.047(4) Uani 1 1 d . . . . .
H28 H 0.7322 -0.0070 0.3302 0.057 Uiso 1 1 calc R U . . .
C29 C 0.6553(7) -0.092(2) 0.2753(9) 0.037(4) Uani 1 1 d . . . . .
H29 H 0.6749 -0.1549 0.2362 0.044 Uiso 1 1 calc R U . . .
C30 C 0.5921(7) -0.082(2) 0.2805(8) 0.038(4) Uani 1 1 d . . . . .
H30 H 0.5693 -0.1375 0.2422 0.045 Uiso 1 1 calc R U . . .


_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
K O2 2.756(10) . ?
K O5 2.790(10) . ?
K O3 2.793(10) . ?
K O6 2.808(9) . ?
K O4 2.814(10) . ?
K O1 2.876(12) . ?
K C23 3.262(15) . ?
K C20 3.311(15) 1_565 ?
K C21 3.458(13) 1_565 ?
K C24 3.522(14) . ?
K C3 3.53(2) . ?
O1 C12 1.35(2) . ?
O1 C1 1.384(19) . ?
O2 C3 1.35(2) . ?
O2 C2 1.394(17) . ?
O3 C4 1.36(2) . ?
O3 C5 1.415(16) . ?
O4 C6 1.347(16) . ?
O4 C7 1.435(16) . ?
O5 C8 1.339(17) . ?
O5 C9 1.432(15) . ?
O6 C10 1.376(17) . ?
O6 C11 1.415(18) . ?
C1 C2 1.450(19) . ?
C3 C4 1.50(3) . ?
C5 C6 1.50(2) . ?
C7 C8 1.49(2) . ?
C9 C10 1.42(2) . ?
C11 C12 1.43(2) . ?
Zn C13 2.013(14) . ?
Zn C19 2.018(17) . ?
Zn C25 2.030(8) . ?
C13 C18 1.414(18) . ?
C13 C14 1.420(19) . ?
C14 C15 1.392(18) . ?
C15 C16 1.362(17) . ?
C16 C17 1.343(19) . ?
C17 C18 1.391(17) . ?
C19 C24 1.361(19) . ?
C19 C20 1.383(19) . ?
C19 Rb 3.720(15) 1_545 ?
C20 C21 1.393(16) . ?
C20 Rb 3.311(15) 1_545 ?
C20 K 3.311(15) 1_545 ?
C21 C22 1.382(17) . ?
C21 Rb 3.458(13) 1_545 ?
C21 K 3.458(13) 1_545 ?
C22 C23 1.381(18) . ?
C23 C24 1.392(18) . ?
C25 C30 1.387(19) . ?
C25 C26 1.401(19) . ?
C26 C27 1.392(17) . ?
C27 C28 1.35(2) . ?
C28 C29 1.41(2) . ?
C29 C30 1.386(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 K O5 176.2(4) . . ?
O2 K O3 61.5(4) . . ?
O5 K O3 121.4(4) . . ?
O2 K O6 117.0(4) . . ?
O5 K O6 59.9(4) . . ?
O3 K O6 176.7(3) . . ?
O2 K O4 121.7(4) . . ?
O5 K O4 61.8(4) . . ?
O3 K O4 62.2(4) . . ?
O6 K O4 120.0(4) . . ?
O2 K O1 59.5(4) . . ?
O5 K O1 117.0(4) . . ?
O3 K O1 119.1(4) . . ?
O6 K O1 58.7(4) . . ?
O4 K O1 178.7(4) . . ?
O2 K C23 81.6(3) . . ?
O5 K C23 96.5(3) . . ?
O3 K C23 79.1(4) . . ?
O6 K C23 97.9(4) . . ?
O4 K C23 101.7(3) . . ?
O1 K C23 79.0(4) . . ?
O2 K C20 101.3(3) . 1_565 ?
O5 K C20 80.7(3) . 1_565 ?
O3 K C20 100.1(3) . 1_565 ?
O6 K C20 82.9(3) . 1_565 ?
O4 K C20 74.7(3) . 1_565 ?
O1 K C20 104.5(3) . 1_565 ?
C23 K C20 176.2(4) . 1_565 ?
O2 K C21 86.6(3) . 1_565 ?
O5 K C21 94.3(3) . 1_565 ?
O3 K C21 109.3(3) . 1_565 ?
O6 K C21 73.2(3) . 1_565 ?
O4 K C21 98.2(3) . 1_565 ?
O1 K C21 81.1(3) . 1_565 ?
C23 K C21 160.0(4) . 1_565 ?
C20 K C21 23.6(3) 1_565 1_565 ?
O2 K C24 96.8(4) . . ?
O5 K C24 82.4(3) . . ?
O3 K C24 71.3(3) . . ?
O6 K C24 106.4(3) . . ?
O4 K C24 78.8(3) . . ?
O1 K C24 101.9(3) . . ?
C23 K C24 23.3(3) . . ?
C20 K C24 153.0(3) 1_565 . ?
C21 K C24 176.3(4) 1_565 . ?
O2 K C3 20.3(4) . . ?
O5 K C3 162.2(5) . . ?
O3 K C3 41.5(4) . . ?
O6 K C3 136.8(5) . . ?
O4 K C3 103.0(5) . . ?
O1 K C3 78.3(5) . . ?
C23 K C3 76.7(5) . . ?
C20 K C3 105.2(5) 1_565 . ?
C21 K C3 97.4(4) 1_565 . ?
C24 K C3 85.5(5) . . ?
C12 O1 C1 109.3(17) . . ?
C12 O1 K 113.3(11) . . ?
C1 O1 K 109.3(11) . . ?
C3 O2 C2 118.7(16) . . ?
C3 O2 K 114.6(12) . . ?
C2 O2 K 118.6(10) . . ?
C4 O3 C5 111.7(15) . . ?
C4 O3 K 113.0(10) . . ?
C5 O3 K 110.9(8) . . ?
C6 O4 C7 115.8(14) . . ?
C6 O4 K 111.9(9) . . ?
C7 O4 K 112.2(8) . . ?
C8 O5 C9 115.0(13) . . ?
C8 O5 K 115.2(9) . . ?
C9 O5 K 114.5(10) . . ?
C10 O6 C11 113.0(14) . . ?
C10 O6 K 111.7(10) . . ?
C11 O6 K 114.5(9) . . ?
O1 C1 C2 111.4(17) . . ?
O2 C2 C1 110.0(17) . . ?
O2 C3 C4 116.4(18) . . ?
O2 C3 K 45.2(9) . . ?
C4 C3 K 78.6(12) . . ?
O3 C4 C3 109.7(15) . . ?
O3 C5 C6 112.2(12) . . ?
O4 C6 C5 111.8(13) . . ?
O4 C7 C8 113.9(13) . . ?
O5 C8 C7 113.5(16) . . ?
C10 C9 O5 109.4(14) . . ?
O6 C10 C9 110.9(17) . . ?
O6 C11 C12 111.8(16) . . ?
O1 C12 C11 109.3(16) . . ?
C13 Zn C19 115.9(4) . . ?
C13 Zn C25 120.1(7) . . ?
C19 Zn C25 123.5(7) . . ?
C18 C13 C14 111.8(13) . . ?
C18 C13 Zn 121.5(12) . . ?
C14 C13 Zn 126.6(11) . . ?
C15 C14 C13 124.0(13) . . ?
C16 C15 C14 118.9(14) . . ?
C17 C16 C15 121.6(14) . . ?
C16 C17 C18 118.9(14) . . ?
C17 C18 C13 124.7(14) . . ?
C24 C19 C20 112.7(15) . . ?
C24 C19 Zn 127.1(12) . . ?
C20 C19 Zn 120.1(11) . . ?
C24 C19 Rb 101.0(10) . 1_545 ?
C20 C19 Rb 62.2(8) . 1_545 ?
Zn C19 Rb 105.9(5) . 1_545 ?
C19 C20 C21 123.7(13) . . ?
C19 C20 Rb 96.1(9) . 1_545 ?
C21 C20 Rb 84.1(8) . 1_545 ?
C19 C20 K 96.1(9) . 1_545 ?
C21 C20 K 84.1(8) . 1_545 ?
C22 C21 C20 121.4(12) . . ?
C22 C21 Rb 104.1(9) . 1_545 ?
C20 C21 Rb 72.3(8) . 1_545 ?
C22 C21 K 104.1(9) . 1_545 ?
C20 C21 K 72.3(8) . 1_545 ?
C23 C22 C21 116.2(13) . . ?
C22 C23 C24 119.9(13) . . ?
C22 C23 K 97.0(10) . . ?
C24 C23 K 88.9(9) . . ?
C19 C24 C23 126.0(13) . . ?
C19 C24 K 109.0(9) . . ?
C23 C24 K 67.8(9) . . ?
C30 C25 C26 113.1(8) . . ?
C30 C25 Zn 123.3(12) . . ?
C26 C25 Zn 123.5(12) . . ?
C27 C26 C25 122.3(13) . . ?
C28 C27 C26 121.3(14) . . ?
C27 C28 C29 120.0(10) . . ?
C30 C29 C28 116.2(14) . . ?
C29 C30 C25 127.0(14) . . ?

_refine_diff_density_max         0.826
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.070


#============================================================================== 
# END of CIF 
#============================================================================== 
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ammonia'
####################################################################### 
# 
# 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_TH464
_database_code_depnum_ccdc_archive 'CCDC 1982127'
loop_
_audit_author_name
_audit_author_address
'Wilhelm Klein'
;Technische Universitaet Muenchen
Germany
;
_audit_update_record             
;
2020-02-05 deposited with the CCDC.	2020-04-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

# start Validation Reply Form
_vrf_PLAT410_TH464               
;
PROBLEM: Short Intra H...H contact       H44B ..H47D          1.78 Ang. 
RESPONSE: These H atoms are part of a disordered THF solvent molecule.
 Therefore, the H-H distances may appear too short. 
;
_vrf_PLAT411_TH464               
;
PROBLEM: Short Inter H...H contact       H1A ..H46A           1.69 Ang. 
RESPONSE:  These H atoms are part of a disordered THF solvent molecule.
 Therefore, the H-H distances may appear too short. 
;
# end Validation Reply Form

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C27 H33 Zn, C16 H35 K N O7, C4 H8 O'
_chemical_formula_sum            'C47 H76 K N O8 Zn'
_chemical_formula_weight         887.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.7570(5)
_cell_length_b                   13.1722(5)
_cell_length_c                   23.6712(8)
_cell_angle_alpha                90
_cell_angle_beta                 94.486(3)
_cell_angle_gamma                90
_cell_volume                     4898.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    11308
_cell_measurement_theta_min      2.6645
_cell_measurement_theta_max      28.9070

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.82228
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d 
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Xcalibur 3'
_diffrn_measurement_method       'ω and π scans'
_diffrn_detector_area_resol_mean 16.0238
_diffrn_reflns_number            55312
_diffrn_reflns_av_unetI/netI     0.1068
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.721
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             9472
_reflns_number_gt                4880
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_computing_data_collection       
; 
 CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.34d 
;
_computing_cell_refinement       
; 
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d 
;
_computing_data_reduction        
; 
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d 
;
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  SHELXL-2014/7
_computing_molecular_graphics    'DIAMOND 3.2k'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0555P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9472
_refine_ls_number_parameters     552
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0455
_refine_ls_wR_factor_ref         0.1107
_refine_ls_wR_factor_gt          0.1018
_refine_ls_goodness_of_fit_ref   0.840
_refine_ls_restrained_S_all      0.840
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn 0.27541(2) 0.51710(3) 0.79455(2) 0.03435(12) Uani 1 1 d . . . . .
C13 C 0.28822(19) 0.3765(2) 0.76001(12) 0.0329(8) Uani 1 1 d . . . . .
C14 C 0.21801(19) 0.3193(2) 0.73933(12) 0.0344(8) Uani 1 1 d . . . . .
C15 C 0.2272(2) 0.2226(3) 0.71584(12) 0.0405(8) Uani 1 1 d . . . . .
H15 H 0.1778 0.1855 0.7027 0.049 Uiso 1 1 calc R U . . .
C16 C 0.3069(2) 0.1798(3) 0.71131(13) 0.0400(8) Uani 1 1 d . . . . .
C17 C 0.3768(2) 0.2362(3) 0.73098(12) 0.0397(8) Uani 1 1 d . . . . .
H17 H 0.4322 0.2093 0.7278 0.048 Uiso 1 1 calc R U . . .
C18 C 0.36818(19) 0.3318(2) 0.75542(12) 0.0348(8) Uani 1 1 d . . . . .
C19 C 0.12888(18) 0.3621(3) 0.74119(14) 0.0439(9) Uani 1 1 d . . . . .
H19A H 0.1276 0.4319 0.7269 0.066 Uiso 1 1 calc R U . . .
H19B H 0.1128 0.3615 0.7804 0.066 Uiso 1 1 calc R U . . .
H19C H 0.0887 0.3204 0.7175 0.066 Uiso 1 1 calc R U . . .
C20 C 0.3148(2) 0.0754(3) 0.68520(14) 0.0543(10) Uani 1 1 d . . . . .
H20A H 0.2880 0.0758 0.6464 0.081 Uiso 1 1 calc R U . . .
H20B H 0.2863 0.0253 0.7078 0.081 Uiso 1 1 calc R U . . .
H20C H 0.3751 0.0576 0.6846 0.081 Uiso 1 1 calc R U . . .
C21 C 0.44891(18) 0.3875(3) 0.77658(14) 0.0446(9) Uani 1 1 d . . . . .
H21A H 0.4585 0.4445 0.7513 0.067 Uiso 1 1 calc R U . . .
H21B H 0.4974 0.3408 0.7772 0.067 Uiso 1 1 calc R U . . .
H21C H 0.4430 0.4131 0.8149 0.067 Uiso 1 1 calc R U . . .
C22 C 0.31155(18) 0.5376(2) 0.87852(12) 0.0311(7) Uani 1 1 d . . . . .
C23 C 0.26637(19) 0.4952(2) 0.92149(13) 0.0350(8) Uani 1 1 d . . . . .
C24 C 0.2918(2) 0.5092(2) 0.97883(13) 0.0388(8) Uani 1 1 d . . . . .
H24 H 0.2581 0.4813 1.0065 0.047 Uiso 1 1 calc R U . . .
C25 C 0.3648(2) 0.5626(2) 0.99650(13) 0.0395(8) Uani 1 1 d . . . . .
C26 C 0.41103(19) 0.6044(2) 0.95435(13) 0.0390(8) Uani 1 1 d . . . . .
H26 H 0.4617 0.6411 0.9650 0.047 Uiso 1 1 calc R U . . .
C27 C 0.38501(19) 0.5939(2) 0.89695(13) 0.0350(8) Uani 1 1 d . . . . .
C28 C 0.18780(19) 0.4327(3) 0.90605(14) 0.0471(9) Uani 1 1 d . . . . .
H28A H 0.1389 0.4779 0.8981 0.071 Uiso 1 1 calc R U . . .
H28B H 0.1770 0.3877 0.9377 0.071 Uiso 1 1 calc R U . . .
H28C H 0.1964 0.3919 0.8724 0.071 Uiso 1 1 calc R U . . .
C29 C 0.3939(2) 0.5765(3) 1.05879(13) 0.0520(10) Uani 1 1 d . . . . .
H29A H 0.3999 0.6491 1.0673 0.078 Uiso 1 1 calc R U . . .
H29B H 0.4489 0.5427 1.0670 0.078 Uiso 1 1 calc R U . . .
H29C H 0.3518 0.5466 1.0822 0.078 Uiso 1 1 calc R U . . .
C30 C 0.43681(19) 0.6454(3) 0.85416(13) 0.0455(9) Uani 1 1 d . . . . .
H30A H 0.3992 0.6865 0.8284 0.068 Uiso 1 1 calc R U . . .
H30B H 0.4652 0.5939 0.8324 0.068 Uiso 1 1 calc R U . . .
H30C H 0.4797 0.6893 0.8739 0.068 Uiso 1 1 calc R U . . .
C31 C 0.22619(18) 0.6362(2) 0.74703(12) 0.0333(8) Uani 1 1 d . . . . .
C32 C 0.27189(19) 0.6853(3) 0.70648(13) 0.0370(8) Uani 1 1 d . . . . .
C33 C 0.2385(2) 0.7697(3) 0.67639(13) 0.0451(9) Uani 1 1 d . . . . .
H33 H 0.2720 0.8023 0.6501 0.054 Uiso 1 1 calc R U . . .
C34 C 0.1581(2) 0.8068(3) 0.68386(14) 0.0476(9) Uani 1 1 d . . . . .
C35 C 0.1118(2) 0.7584(3) 0.72372(14) 0.0423(9) Uani 1 1 d . . . . .
H35 H 0.0565 0.7825 0.7299 0.051 Uiso 1 1 calc R U . . .
C36 C 0.14466(19) 0.6755(3) 0.75470(13) 0.0376(8) Uani 1 1 d . . . . .
C37 C 0.35913(18) 0.6489(3) 0.69380(13) 0.0462(9) Uani 1 1 d . . . . .
H37A H 0.3702 0.6688 0.6552 0.069 Uiso 1 1 calc R U . . .
H37B H 0.3618 0.5748 0.6972 0.069 Uiso 1 1 calc R U . . .
H37C H 0.4021 0.6795 0.7208 0.069 Uiso 1 1 calc R U . . .
C38 C 0.1206(2) 0.8958(3) 0.64999(16) 0.0684(12) Uani 1 1 d . . . . .
H38A H 0.0684 0.8742 0.6280 0.103 Uiso 1 1 calc R U . . .
H38B H 0.1618 0.9201 0.6241 0.103 Uiso 1 1 calc R U . . .
H38C H 0.1073 0.9506 0.6758 0.103 Uiso 1 1 calc R U . . .
C39 C 0.09152(19) 0.6289(3) 0.79844(13) 0.0460(9) Uani 1 1 d . . . . .
H39A H 0.0670 0.5648 0.7839 0.069 Uiso 1 1 calc R U . . .
H39B H 0.0456 0.6757 0.8064 0.069 Uiso 1 1 calc R U . . .
H39C H 0.1275 0.6161 0.8334 0.069 Uiso 1 1 calc R U . . .
K K 0.28899(4) 0.48528(5) 0.46274(3) 0.03282(17) Uani 1 1 d . . . . .
O1 O 0.19136(13) 0.66063(17) 0.47153(10) 0.0486(6) Uani 1 1 d . . . . .
O2 O 0.23636(14) 0.54360(18) 0.56823(9) 0.0471(6) Uani 1 1 d . . . . .
O3 O 0.29983(14) 0.34658(19) 0.55118(10) 0.0546(7) Uani 1 1 d . . . . .
O4 O 0.39306(14) 0.3127(2) 0.45561(11) 0.0586(7) Uani 1 1 d . . . . .
O5 O 0.36567(15) 0.4450(2) 0.36241(10) 0.0611(7) Uani 1 1 d . . . . .
O6 O 0.29583(16) 0.63602(19) 0.38026(9) 0.0562(7) Uani 1 1 d . . . . .
C1 C 0.1806(2) 0.6951(3) 0.52732(17) 0.0632(11) Uani 1 1 d . . . . .
H1A H 0.1325 0.7434 0.5268 0.076 Uiso 1 1 calc R U . . .
H1B H 0.2328 0.7306 0.5428 0.076 Uiso 1 1 calc R U . . .
C2 C 0.1634(2) 0.6056(3) 0.56381(16) 0.0597(11) Uani 1 1 d . . . . .
H2A H 0.1501 0.6289 0.6019 0.072 Uiso 1 1 calc R U . . .
H2B H 0.1140 0.5669 0.5468 0.072 Uiso 1 1 calc R U . . .
C3 C 0.2293(3) 0.4624(3) 0.60756(15) 0.0656(12) Uani 1 1 d . . . . .
H3A H 0.1761 0.4241 0.5979 0.079 Uiso 1 1 calc R U . . .
H3B H 0.2272 0.4900 0.6463 0.079 Uiso 1 1 calc R U . . .
C4 C 0.3034(3) 0.3939(3) 0.60549(15) 0.0689(12) Uani 1 1 d . . . . .
H4A H 0.3569 0.4331 0.6120 0.083 Uiso 1 1 calc R U . . .
H4B H 0.3022 0.3416 0.6355 0.083 Uiso 1 1 calc R U . . .
C5 C 0.3616(3) 0.2686(3) 0.5479(2) 0.0768(14) Uani 1 1 d . . . . .
H5A H 0.3484 0.2113 0.5729 0.092 Uiso 1 1 calc R U . . .
H5B H 0.4188 0.2948 0.5606 0.092 Uiso 1 1 calc R U . . .
C6 C 0.3602(3) 0.2338(3) 0.4889(2) 0.0784(14) Uani 1 1 d . . . . .
H6A H 0.3954 0.1719 0.4866 0.094 Uiso 1 1 calc R U . . .
H6B H 0.3012 0.2173 0.4744 0.094 Uiso 1 1 calc R U . . .
C7 C 0.4026(3) 0.2825(4) 0.3983(2) 0.0823(16) Uani 1 1 d . . . . .
H7A H 0.3477 0.2571 0.3805 0.099 Uiso 1 1 calc R U . . .
H7B H 0.4453 0.2275 0.3974 0.099 Uiso 1 1 calc R U . . .
C8 C 0.4307(3) 0.3721(5) 0.36719(18) 0.0911(18) Uani 1 1 d . . . . .
H8A H 0.4822 0.4016 0.3876 0.109 Uiso 1 1 calc R U . . .
H8B H 0.4455 0.3515 0.3290 0.109 Uiso 1 1 calc R U . . .
C9 C 0.3862(3) 0.5319(4) 0.33072(17) 0.0872(17) Uani 1 1 d . . . . .
H9A H 0.4019 0.5113 0.2927 0.105 Uiso 1 1 calc R U . . .
H9B H 0.4352 0.5681 0.3502 0.105 Uiso 1 1 calc R U . . .
C10 C 0.3107(3) 0.5995(4) 0.32536(16) 0.0819(15) Uani 1 1 d . . . . .
H10A H 0.3210 0.6571 0.2999 0.098 Uiso 1 1 calc R U . . .
H10B H 0.2603 0.5615 0.3091 0.098 Uiso 1 1 calc R U . . .
C11 C 0.2247(3) 0.7023(3) 0.37807(17) 0.0676(13) Uani 1 1 d . . . . .
H11A H 0.1729 0.6653 0.3635 0.081 Uiso 1 1 calc R U . . .
H11B H 0.2338 0.7594 0.3520 0.081 Uiso 1 1 calc R U . . .
C12 C 0.2134(2) 0.7418(3) 0.43556(17) 0.0615(11) Uani 1 1 d . . . . .
H12A H 0.2669 0.7741 0.4513 0.074 Uiso 1 1 calc R U . . .
H12B H 0.1679 0.7937 0.4335 0.074 Uiso 1 1 calc R U . . .
N1 N 0.4170(2) 0.6221(3) 0.49985(19) 0.134(2) Uani 1 1 d . . . . .
H1C H 0.4041 0.6848 0.4855 0.201 Uiso 1 1 calc R U . . .
H1D H 0.4675 0.6011 0.4878 0.201 Uiso 1 1 calc R U . . .
H1E H 0.4210 0.6249 0.5384 0.201 Uiso 1 1 calc R U . . .
O7 O 0.15099(13) 0.4129(2) 0.40196(9) 0.0535(7) Uani 1 1 d . . . . .
C40 C 0.0658(2) 0.4481(3) 0.40442(16) 0.0652(12) Uani 1 1 d . . . . .
H40A H 0.0647 0.5099 0.4281 0.078 Uiso 1 1 calc R U . . .
H40B H 0.0305 0.3953 0.4210 0.078 Uiso 1 1 calc R U . . .
C41 C 0.0322(2) 0.4711(3) 0.34433(16) 0.0643(11) Uani 1 1 d . . . . .
H41A H 0.0339 0.5449 0.3366 0.077 Uiso 1 1 calc R U . . .
H41B H -0.0270 0.4467 0.3369 0.077 Uiso 1 1 calc R U . . .
C42 C 0.0921(2) 0.4139(3) 0.30847(16) 0.0653(11) Uani 1 1 d . . . . .
H42A H 0.0601 0.3662 0.2824 0.078 Uiso 1 1 calc R U . . .
H42B H 0.1244 0.4615 0.2859 0.078 Uiso 1 1 calc R U . . .
C43 C 0.1506(2) 0.3577(3) 0.35012(16) 0.0626(11) Uani 1 1 d . . . . .
H43A H 0.1299 0.2876 0.3552 0.075 Uiso 1 1 calc R U . . .
H43B H 0.2087 0.3545 0.3370 0.075 Uiso 1 1 calc R U . . .
O8 O 0.0511(5) 0.1351(6) 0.5743(4) 0.260(3) Uani 1 1 d . . . . .
C44 C 0.0376(5) 0.2572(6) 0.5850(3) 0.176(4) Uani 1 1 d . . . . .
H44A H -0.0198 0.2707 0.5976 0.211 Uiso 1 1 calc R U . A 2
H44B H 0.0808 0.2833 0.6140 0.211 Uiso 1 1 calc R U . A 2
C45 C 0.0470(3) 0.3026(4) 0.53190(19) 0.0812(15) Uani 1 1 d . . . . .
H45A H 0.1062 0.3264 0.5293 0.097 Uiso 1 1 calc R U . B 1
H45B H 0.0079 0.3611 0.5257 0.097 Uiso 1 1 calc R U . B 1
C46A C 0.0228(5) 0.2115(6) 0.4850(3) 0.037(2) Uani 0.487(7) 1 d . . P C 1
H46A H -0.0302 0.2304 0.4622 0.044 Uiso 0.487(7) 1 calc R U P C 1
H46B H 0.0688 0.2065 0.4590 0.044 Uiso 0.487(7) 1 calc R U P C 1
C47A C 0.0123(6) 0.1228(9) 0.5079(4) 0.083(4) Uani 0.487(7) 1 d . . P C 1
H47A H 0.0435 0.0697 0.4884 0.100 Uiso 0.487(7) 1 calc R U P C 1
H47B H -0.0488 0.1044 0.5060 0.100 Uiso 0.487(7) 1 calc R U P C 1
C46B C 0.0851(6) 0.2422(6) 0.5077(4) 0.056(3) Uani 0.513(7) 1 d . . P C 2
H46C H 0.1328 0.2743 0.4895 0.068 Uiso 0.513(7) 1 calc R U P C 2
H46D H 0.0475 0.2074 0.4783 0.068 Uiso 0.513(7) 1 calc R U P C 2
C47B C 0.1169(5) 0.1705(8) 0.5520(4) 0.071(3) Uani 0.513(7) 1 d . . P C 2
H47C H 0.1491 0.1149 0.5354 0.086 Uiso 0.513(7) 1 calc R U P C 2
H47D H 0.1550 0.2057 0.5810 0.086 Uiso 0.513(7) 1 calc R U 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
Zn C13 2.041(3) . ?
Zn C22 2.042(3) . ?
Zn C31 2.047(3) . ?
C13 C14 1.395(4) . ?
C13 C18 1.402(4) . ?
C14 C15 1.402(4) . ?
C14 C19 1.517(4) . ?
C15 C16 1.388(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.378(4) . ?
C16 C20 1.517(4) . ?
C17 C18 1.397(4) . ?
C17 H17 0.9500 . ?
C18 C21 1.519(4) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.402(4) . ?
C22 C27 1.415(4) . ?
C23 C24 1.397(4) . ?
C23 C28 1.508(4) . ?
C24 C25 1.385(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.393(4) . ?
C25 C29 1.521(4) . ?
C26 C27 1.395(4) . ?
C26 H26 0.9500 . ?
C27 C30 1.510(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.402(4) . ?
C31 C36 1.410(4) . ?
C32 C33 1.401(4) . ?
C32 C37 1.508(4) . ?
C33 C34 1.382(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.392(4) . ?
C34 C38 1.513(5) . ?
C35 C36 1.393(4) . ?
C35 H35 0.9500 . ?
C36 C39 1.512(4) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
K O7 2.687(2) . ?
K O3 2.774(2) . ?
K O1 2.792(2) . ?
K O6 2.793(2) . ?
K N1 2.794(3) . ?
K O5 2.798(2) . ?
K O2 2.799(2) . ?
K O4 2.816(2) . ?
K C6 3.536(4) . ?
O1 C1 1.419(4) . ?
O1 C12 1.426(4) . ?
O2 C2 1.407(4) . ?
O2 C3 1.428(4) . ?
O3 C5 1.422(4) . ?
O3 C4 1.426(4) . ?
O4 C6 1.424(5) . ?
O4 C7 1.434(5) . ?
O5 C8 1.403(5) . ?
O5 C9 1.420(5) . ?
O6 C11 1.418(4) . ?
O6 C10 1.422(4) . ?
C1 C2 1.498(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.479(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.470(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.477(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.484(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.481(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
N1 H1C 0.9100 . ?
N1 H1D 0.9100 . ?
N1 H1E 0.9100 . ?
O7 C40 1.426(4) . ?
O7 C43 1.426(4) . ?
C40 C41 1.509(5) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.518(5) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.492(5) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
O8 C47B 1.287(8) . ?
O8 C44 1.644(9) . ?
O8 C47A 1.649(10) . ?
C44 C45 1.410(6) . ?
C44 C46B 2.040(10) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46B 1.173(7) . ?
C45 C46A 1.659(9) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46A C47A 1.304(12) . ?
C46A H46A 0.9900 . ?
C46A H46B 0.9900 . ?
C47A H47A 0.9900 . ?
C47A H47B 0.9900 . ?
C46B C47B 1.470(11) . ?
C46B H46C 0.9900 . ?
C46B H46D 0.9900 . ?
C47B H47C 0.9900 . ?
C47B H47D 0.9900 . ?

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
C13 Zn C22 118.75(11) . . ?
C13 Zn C31 121.34(11) . . ?
C22 Zn C31 119.90(12) . . ?
C14 C13 C18 116.0(3) . . ?
C14 C13 Zn 122.0(2) . . ?
C18 C13 Zn 122.0(2) . . ?
C13 C14 C15 121.7(3) . . ?
C13 C14 C19 120.0(3) . . ?
C15 C14 C19 118.3(3) . . ?
C16 C15 C14 121.4(3) . . ?
C16 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
C17 C16 C15 117.3(3) . . ?
C17 C16 C20 122.5(3) . . ?
C15 C16 C20 120.2(3) . . ?
C16 C17 C18 121.7(3) . . ?
C16 C17 H17 119.2 . . ?
C18 C17 H17 119.2 . . ?
C17 C18 C13 121.8(3) . . ?
C17 C18 C21 117.8(3) . . ?
C13 C18 C21 120.4(3) . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C20 H20A 109.5 . . ?
C16 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C16 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C27 115.8(3) . . ?
C23 C22 Zn 122.3(2) . . ?
C27 C22 Zn 121.9(2) . . ?
C24 C23 C22 121.9(3) . . ?
C24 C23 C28 118.4(3) . . ?
C22 C23 C28 119.7(3) . . ?
C25 C24 C23 122.0(3) . . ?
C25 C24 H24 119.0 . . ?
C23 C24 H24 119.0 . . ?
C24 C25 C26 116.9(3) . . ?
C24 C25 C29 122.3(3) . . ?
C26 C25 C29 120.8(3) . . ?
C25 C26 C27 121.9(3) . . ?
C25 C26 H26 119.1 . . ?
C27 C26 H26 119.1 . . ?
C26 C27 C22 121.5(3) . . ?
C26 C27 C30 118.4(3) . . ?
C22 C27 C30 120.1(3) . . ?
C23 C28 H28A 109.5 . . ?
C23 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C23 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C29 H29A 109.5 . . ?
C25 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C25 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C36 116.1(3) . . ?
C32 C31 Zn 122.5(2) . . ?
C36 C31 Zn 121.4(2) . . ?
C33 C32 C31 121.4(3) . . ?
C33 C32 C37 117.6(3) . . ?
C31 C32 C37 121.0(3) . . ?
C34 C33 C32 121.9(3) . . ?
C34 C33 H33 119.1 . . ?
C32 C33 H33 119.1 . . ?
C33 C34 C35 117.3(3) . . ?
C33 C34 C38 122.0(3) . . ?
C35 C34 C38 120.7(3) . . ?
C34 C35 C36 121.6(3) . . ?
C34 C35 H35 119.2 . . ?
C36 C35 H35 119.2 . . ?
C35 C36 C31 121.7(3) . . ?
C35 C36 C39 118.4(3) . . ?
C31 C36 C39 119.9(3) . . ?
C32 C37 H37A 109.5 . . ?
C32 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C32 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38A 109.5 . . ?
C34 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C34 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O7 K O3 99.78(7) . . ?
O7 K O1 84.60(7) . . ?
O3 K O1 119.37(8) . . ?
O7 K O6 87.24(7) . . ?
O3 K O6 172.98(7) . . ?
O1 K O6 61.02(8) . . ?
O7 K N1 158.61(9) . . ?
O3 K N1 100.79(9) . . ?
O1 K N1 80.29(11) . . ?
O6 K N1 72.24(9) . . ?
O7 K O5 82.15(7) . . ?
O3 K O5 120.70(9) . . ?
O1 K O5 119.81(8) . . ?
O6 K O5 59.90(9) . . ?
N1 K O5 92.30(12) . . ?
O7 K O2 106.93(7) . . ?
O3 K O2 60.83(8) . . ?
O1 K O2 60.20(7) . . ?
O6 K O2 117.31(8) . . ?
N1 K O2 78.43(12) . . ?
O5 K O2 170.66(7) . . ?
O7 K O4 97.59(7) . . ?
O3 K O4 60.76(8) . . ?
O1 K O4 177.77(7) . . ?
O6 K O4 118.53(9) . . ?
N1 K O4 97.49(11) . . ?
O5 K O4 60.27(9) . . ?
O2 K O4 119.31(8) . . ?
O7 K C6 89.65(9) . . ?
O3 K C6 41.50(10) . . ?
O1 K C6 158.61(10) . . ?
O6 K C6 139.38(11) . . ?
N1 K C6 109.73(10) . . ?
O5 K C6 79.55(11) . . ?
O2 K C6 102.31(10) . . ?
O4 K C6 22.46(9) . . ?
C1 O1 C12 111.6(3) . . ?
C1 O1 K 116.1(2) . . ?
C12 O1 K 114.5(2) . . ?
C2 O2 C3 112.2(3) . . ?
C2 O2 K 112.98(19) . . ?
C3 O2 K 114.8(2) . . ?
C5 O3 C4 112.7(3) . . ?
C5 O3 K 115.9(2) . . ?
C4 O3 K 112.9(2) . . ?
C6 O4 C7 113.0(3) . . ?
C6 O4 K 108.5(2) . . ?
C7 O4 K 112.7(2) . . ?
C8 O5 C9 113.5(4) . . ?
C8 O5 K 115.0(2) . . ?
C9 O5 K 115.3(2) . . ?
C11 O6 C10 111.1(3) . . ?
C11 O6 K 112.9(2) . . ?
C10 O6 K 114.6(2) . . ?
O1 C1 C2 109.0(3) . . ?
O1 C1 H1A 109.9 . . ?
C2 C1 H1A 109.9 . . ?
O1 C1 H1B 109.9 . . ?
C2 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
O2 C2 C1 108.4(3) . . ?
O2 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
O2 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
O2 C3 C4 109.5(3) . . ?
O2 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 . . ?
O2 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.2 . . ?
O3 C4 C3 108.7(3) . . ?
O3 C4 H4A 109.9 . . ?
C3 C4 H4A 109.9 . . ?
O3 C4 H4B 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
O3 C5 C6 108.5(3) . . ?
O3 C5 H5A 110.0 . . ?
C6 C5 H5A 110.0 . . ?
O3 C5 H5B 110.0 . . ?
C6 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
O4 C6 C5 108.7(3) . . ?
O4 C6 K 49.06(16) . . ?
C5 C6 K 81.7(2) . . ?
O4 C6 H6A 110.0 . . ?
C5 C6 H6A 110.0 . . ?
K C6 H6A 159.0 . . ?
O4 C6 H6B 110.0 . . ?
C5 C6 H6B 110.0 . . ?
K C6 H6B 82.5 . . ?
H6A C6 H6B 108.3 . . ?
O4 C7 C8 107.9(4) . . ?
O4 C7 H7A 110.1 . . ?
C8 C7 H7A 110.1 . . ?
O4 C7 H7B 110.1 . . ?
C8 C7 H7B 110.1 . . ?
H7A C7 H7B 108.4 . . ?
O5 C8 C7 110.0(4) . . ?
O5 C8 H8A 109.7 . . ?
C7 C8 H8A 109.7 . . ?
O5 C8 H8B 109.7 . . ?
C7 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
O5 C9 C10 108.3(3) . . ?
O5 C9 H9A 110.0 . . ?
C10 C9 H9A 110.0 . . ?
O5 C9 H9B 110.0 . . ?
C10 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
O6 C10 C9 108.2(3) . . ?
O6 C10 H10A 110.1 . . ?
C9 C10 H10A 110.1 . . ?
O6 C10 H10B 110.1 . . ?
C9 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
O6 C11 C12 109.5(3) . . ?
O6 C11 H11A 109.8 . . ?
C12 C11 H11A 109.8 . . ?
O6 C11 H11B 109.8 . . ?
C12 C11 H11B 109.8 . . ?
H11A C11 H11B 108.2 . . ?
O1 C12 C11 109.7(3) . . ?
O1 C12 H12A 109.7 . . ?
C11 C12 H12A 109.7 . . ?
O1 C12 H12B 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
K N1 H1C 109.5 . . ?
K N1 H1D 109.5 . . ?
H1C N1 H1D 109.5 . . ?
K N1 H1E 109.5 . . ?
H1C N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
C40 O7 C43 105.1(3) . . ?
C40 O7 K 126.0(2) . . ?
C43 O7 K 126.19(19) . . ?
O7 C40 C41 106.8(3) . . ?
O7 C40 H40A 110.4 . . ?
C41 C40 H40A 110.4 . . ?
O7 C40 H40B 110.4 . . ?
C41 C40 H40B 110.4 . . ?
H40A C40 H40B 108.6 . . ?
C40 C41 C42 103.9(3) . . ?
C40 C41 H41A 111.0 . . ?
C42 C41 H41A 111.0 . . ?
C40 C41 H41B 111.0 . . ?
C42 C41 H41B 111.0 . . ?
H41A C41 H41B 109.0 . . ?
C43 C42 C41 104.8(3) . . ?
C43 C42 H42A 110.8 . . ?
C41 C42 H42A 110.8 . . ?
C43 C42 H42B 110.8 . . ?
C41 C42 H42B 110.8 . . ?
H42A C42 H42B 108.9 . . ?
O7 C43 C42 106.0(3) . . ?
O7 C43 H43A 110.5 . . ?
C42 C43 H43A 110.5 . . ?
O7 C43 H43B 110.5 . . ?
C42 C43 H43B 110.5 . . ?
H43A C43 H43B 108.7 . . ?
C47B O8 C44 80.0(6) . . ?
C44 O8 C47A 101.5(6) . . ?
C45 C44 O8 104.7(6) . . ?
O8 C44 C46B 72.9(5) . . ?
C45 C44 H44A 110.8 . . ?
O8 C44 H44A 110.8 . . ?
C46B C44 H44A 134.1 . . ?
C45 C44 H44B 110.8 . . ?
O8 C44 H44B 110.8 . . ?
C46B C44 H44B 112.0 . . ?
H44A C44 H44B 108.9 . . ?
C46B C45 C44 103.9(7) . . ?
C44 C45 C46A 104.7(5) . . ?
C44 C45 H45A 110.8 . . ?
C46A C45 H45A 110.8 . . ?
C44 C45 H45B 110.8 . . ?
C46A C45 H45B 110.8 . . ?
H45A C45 H45B 108.9 . . ?
C47A C46A C45 113.6(6) . . ?
C47A C46A H46A 108.8 . . ?
C45 C46A H46A 108.8 . . ?
C47A C46A H46B 108.8 . . ?
C45 C46A H46B 108.8 . . ?
H46A C46A H46B 107.7 . . ?
C46A C47A O8 105.0(8) . . ?
C46A C47A H47A 110.7 . . ?
O8 C47A H47A 110.7 . . ?
C46A C47A H47B 110.7 . . ?
O8 C47A H47B 110.7 . . ?
H47A C47A H47B 108.8 . . ?
C45 C46B C47B 104.3(7) . . ?
C47B C46B C44 63.3(5) . . ?
C45 C46B H46C 110.9 . . ?
C47B C46B H46C 110.9 . . ?
C44 C46B H46C 133.9 . . ?
C45 C46B H46D 110.9 . . ?
C47B C46B H46D 110.9 . . ?
C44 C46B H46D 115.7 . . ?
H46C C46B H46D 108.9 . . ?
O8 C47B C46B 106.5(7) . . ?
O8 C47B H47C 110.4 . . ?
C46B C47B H47C 110.4 . . ?
O8 C47B H47D 110.4 . . ?
C46B C47B H47D 110.4 . . ?
H47C C47B H47D 108.6 . . ?

_refine_diff_density_max         0.659
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.056


#============================================================================== 
# END of CIF 
#============================================================================== 
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ammonia'
####################################################################### 
# 
# 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_KM-547
_database_code_depnum_ccdc_archive 'CCDC 1982123'
loop_
_audit_author_name
_audit_author_address
'Wilhelm Klein'
;Technische Universitaet Muenchen
Germany
;
_audit_update_record             
;
2020-02-05 deposited with the CCDC.	2020-04-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         '3(C18 H36 K N2 O6), C2 H5 Ge9 Zn, 7.4(H3 N)'
_chemical_formula_sum            'C56 H135.22 Ge9 K3 N13.40 O18 Zn'
_chemical_formula_weight         2120.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.6139(7)
_cell_length_b                   14.9181(6)
_cell_length_c                   23.6002(8)
_cell_angle_alpha                97.552(3)
_cell_angle_beta                 91.645(3)
_cell_angle_gamma                117.312(3)
_cell_volume                     4508.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    116757
_cell_measurement_theta_min      2.145
_cell_measurement_theta_max      30.84

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    3.416
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            93046
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_av_R_equivalents  0.0891
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.145
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             17700
_reflns_number_gt                12811
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_computing_data_collection       'STOE X-AREA 1.76'
_computing_cell_refinement       'STOE X-AREA 1.76'
_computing_data_reduction        'STOE X-AREA 1.76'
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  SHELXL-2014/7
_computing_molecular_graphics    'DIAMOND 3.2k'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0713P)²+5.8522P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         17700
_refine_ls_number_parameters     913
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0509
_refine_ls_wR_factor_ref         0.1374
_refine_ls_wR_factor_gt          0.1210
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.44112(4) 0.25973(4) 0.22815(2) 0.03376(14) Uani 1 1 d . . . . .
Ge2 Ge 0.26510(5) 0.28455(4) 0.23209(2) 0.03222(13) Uani 1 1 d . . . . .
Ge3 Ge 0.14437(4) 0.07993(4) 0.18197(2) 0.03291(13) Uani 1 1 d . . . . .
Ge4 Ge 0.32395(5) 0.05867(4) 0.17824(2) 0.03274(13) Uani 1 1 d . . . . .
Ge5 Ge 0.40276(5) 0.11214(4) 0.28369(2) 0.03396(14) Uani 1 1 d . . . . .
Ge6 Ge 0.36037(4) 0.27392(4) 0.32214(2) 0.03205(13) Uani 1 1 d . . . . .
Ge7 Ge 0.14824(4) 0.14705(4) 0.28800(2) 0.03369(14) Uani 1 1 d . . . . .
Ge8 Ge 0.18904(5) -0.01944(4) 0.24813(2) 0.03380(14) Uani 1 1 d . . . . .
Ge9 Ge 0.25675(5) 0.09182(5) 0.34802(2) 0.03891(15) Uani 1 1 d . . . . .
Zn Zn 0.30514(5) 0.20452(5) 0.13756(2) 0.03902(16) Uani 1 1 d . . . . .
C1 C 0.3211(5) 0.2591(4) 0.0627(2) 0.0392(13) Uani 1 1 d . . . . .
H1A H 0.3689 0.2409 0.0411 0.047 Uiso 1 1 calc R U . . .
H1B H 0.2530 0.2253 0.0396 0.047 Uiso 1 1 calc R U . . .
C2 C 0.3620(5) 0.3738(4) 0.0702(2) 0.0537(17) Uani 1 1 d . . . . .
H2A H 0.3693 0.3955 0.0324 0.081 Uiso 1 1 calc R U . . .
H2B H 0.4296 0.4080 0.0930 0.081 Uiso 1 1 calc R U . . .
H2C H 0.3135 0.3922 0.0900 0.081 Uiso 1 1 calc R U . . .
K1 K 0.63467(9) 0.76811(8) 0.25239(4) 0.0309(2) Uani 1 1 d . . . . .
N1 N 0.4277(3) 0.7028(3) 0.19031(17) 0.0328(10) Uani 1 1 d . . . . .
N2 N 0.8390(4) 0.8313(3) 0.31535(19) 0.0382(10) Uani 1 1 d . . . . .
O1 O 0.4591(3) 0.6082(3) 0.28533(14) 0.0353(8) Uani 1 1 d . . . . .
O2 O 0.6439(3) 0.6891(3) 0.35806(15) 0.0368(8) Uani 1 1 d . . . . .
O3 O 0.5483(3) 0.9046(2) 0.26191(15) 0.0349(8) Uani 1 1 d . . . . .
O4 O 0.7594(3) 0.9752(2) 0.29970(14) 0.0339(8) Uani 1 1 d . . . . .
O5 O 0.6135(3) 0.7360(3) 0.12952(14) 0.0376(8) Uani 1 1 d . . . . .
O6 O 0.7912(3) 0.7500(3) 0.19140(15) 0.0417(9) Uani 1 1 d . . . . .
C3 C 0.3584(5) 0.5986(4) 0.2007(2) 0.0419(13) Uani 1 1 d . . . . .
H3A H 0.3790 0.5508 0.1786 0.050 Uiso 1 1 calc R U . . .
H3B H 0.2871 0.5799 0.1853 0.050 Uiso 1 1 calc R U . . .
C4 C 0.3568(4) 0.5831(4) 0.2620(2) 0.0379(12) Uani 1 1 d . . . . .
H4A H 0.3321 0.6271 0.2845 0.045 Uiso 1 1 calc R U . . .
H4B H 0.3086 0.5110 0.2645 0.045 Uiso 1 1 calc R U . . .
C5 C 0.4600(4) 0.5866(4) 0.3427(2) 0.0407(13) Uani 1 1 d . . . . .
H5A H 0.4022 0.5183 0.3448 0.049 Uiso 1 1 calc R U . . .
H5B H 0.4510 0.6381 0.3696 0.049 Uiso 1 1 calc R U . . .
C6 C 0.5593(4) 0.5891(4) 0.3588(2) 0.0387(13) Uani 1 1 d . . . . .
H6A H 0.5593 0.5712 0.3977 0.046 Uiso 1 1 calc R U . . .
H6B H 0.5682 0.5380 0.3315 0.046 Uiso 1 1 calc R U . . .
C7 C 0.7407(5) 0.6932(5) 0.3731(3) 0.0472(15) Uani 1 1 d . . . . .
H7A H 0.7511 0.6437 0.3453 0.057 Uiso 1 1 calc R U . . .
H7B H 0.7420 0.6750 0.4118 0.057 Uiso 1 1 calc R U . . .
C8 C 0.8261(5) 0.8007(5) 0.3723(2) 0.0464(14) Uani 1 1 d . . . . .
H8A H 0.8113 0.8494 0.3981 0.056 Uiso 1 1 calc R U . . .
H8B H 0.8922 0.8061 0.3881 0.056 Uiso 1 1 calc R U . . .
C9 C 0.3877(4) 0.7733(4) 0.2139(2) 0.0364(12) Uani 1 1 d . . . . .
H9A H 0.3648 0.7581 0.2522 0.044 Uiso 1 1 calc R U . . .
H9B H 0.3263 0.7605 0.1885 0.044 Uiso 1 1 calc R U . . .
C10 C 0.4653(4) 0.8841(4) 0.2197(2) 0.0373(12) Uani 1 1 d . . . . .
H10A H 0.4926 0.8997 0.1823 0.045 Uiso 1 1 calc R U . . .
H10B H 0.4323 0.9274 0.2318 0.045 Uiso 1 1 calc R U . . .
C11 C 0.6239(4) 1.0103(4) 0.2685(2) 0.0401(13) Uani 1 1 d . . . . .
H11A H 0.5904 1.0541 0.2783 0.048 Uiso 1 1 calc R U . . .
H11B H 0.6553 1.0255 0.2321 0.048 Uiso 1 1 calc R U . . .
C12 C 0.7058(5) 1.0319(4) 0.3154(2) 0.0411(13) Uani 1 1 d . . . . .
H12A H 0.7551 1.1058 0.3225 0.049 Uiso 1 1 calc R U . . .
H12B H 0.6736 1.0132 0.3513 0.049 Uiso 1 1 calc R U . . .
C13 C 0.8443(4) 1.0008(4) 0.3419(2) 0.0404(13) Uani 1 1 d . . . . .
H13A H 0.8177 0.9825 0.3790 0.048 Uiso 1 1 calc R U . . .
H13B H 0.8912 1.0753 0.3476 0.048 Uiso 1 1 calc R U . . .
C14 C 0.9033(4) 0.9438(4) 0.3222(2) 0.0429(13) Uani 1 1 d . . . . .
H14A H 0.9296 0.9624 0.2850 0.051 Uiso 1 1 calc R U . . .
H14B H 0.9638 0.9652 0.3505 0.051 Uiso 1 1 calc R U . . .
C15 C 0.4360(5) 0.7033(4) 0.1288(2) 0.0394(13) Uani 1 1 d . . . . .
H15A H 0.4588 0.7738 0.1212 0.047 Uiso 1 1 calc R U . . .
H15B H 0.3665 0.6594 0.1079 0.047 Uiso 1 1 calc R U . . .
C16 C 0.5103(5) 0.6664(4) 0.1054(2) 0.0424(13) Uani 1 1 d . . . . .
H16A H 0.4910 0.5977 0.1149 0.051 Uiso 1 1 calc R U . . .
H16B H 0.5060 0.6611 0.0630 0.051 Uiso 1 1 calc R U . . .
C17 C 0.6854(5) 0.7077(5) 0.1038(2) 0.0442(14) Uani 1 1 d . . . . .
H17A H 0.6865 0.7164 0.0629 0.053 Uiso 1 1 calc R U . . .
H17B H 0.6639 0.6349 0.1055 0.053 Uiso 1 1 calc R U . . .
C18 C 0.7899(5) 0.7720(5) 0.1342(2) 0.0451(14) Uani 1 1 d . . . . .
H18A H 0.8411 0.7582 0.1134 0.054 Uiso 1 1 calc R U . . .
H18B H 0.8089 0.8452 0.1356 0.054 Uiso 1 1 calc R U . . .
C19 C 0.8944(4) 0.7944(5) 0.2192(2) 0.0453(14) Uani 1 1 d . . . . .
H19A H 0.9313 0.8682 0.2165 0.054 Uiso 1 1 calc R U . . .
H19B H 0.9327 0.7611 0.1997 0.054 Uiso 1 1 calc R U . . .
C20 C 0.8905(5) 0.7808(4) 0.2807(2) 0.0449(14) Uani 1 1 d . . . . .
H20A H 0.8538 0.7067 0.2824 0.054 Uiso 1 1 calc R U . . .
H20B H 0.9622 0.8077 0.2985 0.054 Uiso 1 1 calc R U . . .
N7 N 0.5798(5) 0.5322(4) 0.2015(2) 0.0682(17) Uani 1 1 d . . . . .
H7C H 0.5875 0.5266 0.1633 0.102 Uiso 1 1 calc R U . . .
H7D H 0.5133 0.4895 0.2070 0.102 Uiso 1 1 calc R U . . .
H7E H 0.6234 0.5151 0.2201 0.102 Uiso 1 1 calc R U . . .
K2 K 0.83368(8) 0.26846(8) 0.04831(4) 0.0284(2) Uani 1 1 d . . . . .
N3 N 0.7485(3) 0.4206(3) 0.07938(16) 0.0299(9) Uani 1 1 d . . . . .
N4 N 0.9147(3) 0.1192(3) 0.01611(16) 0.0314(9) Uani 1 1 d . . . . .
O7 O 0.8118(3) 0.3821(3) -0.03541(14) 0.0335(8) Uani 1 1 d . . . . .
O8 O 0.9241(3) 0.2692(3) -0.05837(13) 0.0321(8) Uani 1 1 d . . . . .
O9 O 0.9368(3) 0.4368(3) 0.13887(13) 0.0316(8) Uani 1 1 d . . . . .
O10 O 0.9928(3) 0.2768(2) 0.12003(13) 0.0310(8) Uani 1 1 d . . . . .
O11 O 0.6415(3) 0.2030(3) 0.09283(15) 0.0364(8) Uani 1 1 d . . . . .
O12 O 0.7031(3) 0.0568(3) 0.04803(14) 0.0375(9) Uani 1 1 d . . . . .
C21 C 0.7226(4) 0.4492(4) 0.0261(2) 0.0369(12) Uani 1 1 d . . . . .
H21A H 0.7118 0.5100 0.0362 0.044 Uiso 1 1 calc R U . . .
H21B H 0.6565 0.3926 0.0067 0.044 Uiso 1 1 calc R U . . .
C22 C 0.8043(4) 0.4728(4) -0.0155(2) 0.0346(12) Uani 1 1 d . . . . .
H22A H 0.7855 0.4980 -0.0484 0.041 Uiso 1 1 calc R U . . .
H22B H 0.8719 0.5268 0.0038 0.041 Uiso 1 1 calc R U . . .
C23 C 0.8823(4) 0.3999(4) -0.0783(2) 0.0377(13) Uani 1 1 d . . . . .
H23A H 0.9527 0.4515 -0.0613 0.045 Uiso 1 1 calc R U . . .
H23B H 0.8612 0.4270 -0.1095 0.045 Uiso 1 1 calc R U . . .
C24 C 0.8835(4) 0.3015(4) -0.1026(2) 0.0354(12) Uani 1 1 d . . . . .
H24A H 0.8123 0.2482 -0.1172 0.042 Uiso 1 1 calc R U . . .
H24B H 0.9270 0.3125 -0.1350 0.042 Uiso 1 1 calc R U . . .
C25 C 0.9203(4) 0.1724(4) -0.0799(2) 0.0355(12) Uani 1 1 d . . . . .
H25A H 0.9561 0.1778 -0.1153 0.043 Uiso 1 1 calc R U . . .
H25B H 0.8474 0.1192 -0.0897 0.043 Uiso 1 1 calc R U . . .
C26 C 0.9716(5) 0.1433(4) -0.0353(2) 0.0378(12) Uani 1 1 d . . . . .
H26A H 0.9787 0.0830 -0.0526 0.045 Uiso 1 1 calc R U . . .
H26B H 1.0420 0.2003 -0.0233 0.045 Uiso 1 1 calc R U . . .
C27 C 0.8278(4) 0.5116(4) 0.1178(2) 0.0343(12) Uani 1 1 d . . . . .
H27A H 0.7948 0.5516 0.1359 0.041 Uiso 1 1 calc R U . . .
H27B H 0.8808 0.5552 0.0946 0.041 Uiso 1 1 calc R U . . .
C28 C 0.8802(4) 0.4856(4) 0.1643(2) 0.0366(12) Uani 1 1 d . . . . .
H28A H 0.9279 0.5487 0.1907 0.044 Uiso 1 1 calc R U . . .
H28B H 0.8277 0.4395 0.1868 0.044 Uiso 1 1 calc R U . . .
C29 C 0.9924(4) 0.4169(4) 0.1818(2) 0.0349(12) Uani 1 1 d . . . . .
H29A H 0.9428 0.3686 0.2047 0.042 Uiso 1 1 calc R U . . .
H29B H 1.0373 0.4813 0.2081 0.042 Uiso 1 1 calc R U . . .
C30 C 1.0574(4) 0.3724(4) 0.1555(2) 0.0335(12) Uani 1 1 d . . . . .
H30A H 1.1066 0.4200 0.1322 0.040 Uiso 1 1 calc R U . . .
H30B H 1.0979 0.3624 0.1862 0.040 Uiso 1 1 calc R U . . .
C31 C 1.0555(4) 0.2357(4) 0.0933(2) 0.0389(13) Uani 1 1 d . . . . .
H31A H 1.1059 0.2365 0.1225 0.047 Uiso 1 1 calc R U . . .
H31B H 1.0943 0.2778 0.0646 0.047 Uiso 1 1 calc R U . . .
C32 C 0.9857(5) 0.1277(4) 0.0643(2) 0.0401(13) Uani 1 1 d . . . . .
H32A H 1.0291 0.0963 0.0499 0.048 Uiso 1 1 calc R U . . .
H32B H 0.9444 0.0880 0.0931 0.048 Uiso 1 1 calc R U . . .
C33 C 0.6530(4) 0.3698(4) 0.1079(2) 0.0351(12) Uani 1 1 d . . . . .
H33A H 0.6119 0.4067 0.1051 0.042 Uiso 1 1 calc R U . . .
H33B H 0.6724 0.3747 0.1491 0.042 Uiso 1 1 calc R U . . .
C34 C 0.5870(4) 0.2596(4) 0.0827(2) 0.0378(12) Uani 1 1 d . . . . .
H34A H 0.5211 0.2319 0.1006 0.045 Uiso 1 1 calc R U . . .
H34B H 0.5706 0.2530 0.0409 0.045 Uiso 1 1 calc R U . . .
C35 C 0.5718(4) 0.0951(4) 0.0838(2) 0.0436(14) Uani 1 1 d . . . . .
H35A H 0.5352 0.0732 0.0447 0.052 Uiso 1 1 calc R U . . .
H35B H 0.5196 0.0797 0.1119 0.052 Uiso 1 1 calc R U . . .
C36 C 0.6327(5) 0.0390(4) 0.0913(2) 0.0430(14) Uani 1 1 d . . . . .
H36A H 0.6717 0.0632 0.1299 0.052 Uiso 1 1 calc R U . . .
H36B H 0.5853 -0.0351 0.0879 0.052 Uiso 1 1 calc R U . . .
C37 C 0.7505(5) -0.0078(4) 0.0476(2) 0.0456(14) Uani 1 1 d . . . . .
H37A H 0.6970 -0.0803 0.0386 0.055 Uiso 1 1 calc R U . . .
H37B H 0.7866 0.0033 0.0860 0.055 Uiso 1 1 calc R U . . .
C38 C 0.8269(4) 0.0154(4) 0.0033(2) 0.0370(12) Uani 1 1 d . . . . .
H38A H 0.8539 -0.0348 0.0007 0.044 Uiso 1 1 calc R U . . .
H38B H 0.7905 0.0069 -0.0346 0.044 Uiso 1 1 calc R U . . .
N8 N 0.6310(4) 0.1296(3) -0.0619(2) 0.0453(12) Uani 1 1 d . . . . .
H8C H 0.6468 0.1048 -0.0319 0.068 Uiso 1 1 d R U . . .
H8D H 0.6756 0.1974 -0.0589 0.068 Uiso 1 1 d R U . . .
H8E H 0.6366 0.0957 -0.0955 0.068 Uiso 1 1 d R U . . .
K3 K 0.24054(9) 0.65845(8) 0.44593(4) 0.0320(2) Uani 1 1 d . . . . .
N5 N 0.0698(3) 0.6207(3) 0.35713(17) 0.0340(10) Uani 1 1 d . . . . .
N6 N 0.4070(4) 0.6956(4) 0.53453(18) 0.0439(11) Uani 1 1 d . . . . .
O13 O 0.0688(3) 0.6871(3) 0.47864(14) 0.0385(9) Uani 1 1 d . . . . .
O14 O 0.2064(3) 0.6804(3) 0.56417(14) 0.0411(9) Uani 1 1 d . . . . .
O15 O 0.1233(3) 0.4604(3) 0.38200(13) 0.0330(8) Uani 1 1 d . . . . .
O16 O 0.3077(3) 0.5089(3) 0.44903(14) 0.0354(8) Uani 1 1 d . . . . .
O17 O 0.2869(3) 0.7781(3) 0.35631(15) 0.0415(9) Uani 1 1 d . . . . .
O18 O 0.4324(3) 0.8367(3) 0.45327(17) 0.0541(11) Uani 1 1 d . . . . .
C39 C 0.0043(5) 0.6645(5) 0.3813(2) 0.0404(13) Uani 1 1 d . . . . .
H39A H -0.0603 0.6368 0.3553 0.048 Uiso 1 1 calc R U . . .
H39B H 0.0410 0.7395 0.3823 0.048 Uiso 1 1 calc R U . . .
C40 C -0.0235(5) 0.6433(5) 0.4406(2) 0.0420(13) Uani 1 1 d . . . . .
H40A H -0.0689 0.6733 0.4536 0.050 Uiso 1 1 calc R U . . .
H40B H -0.0614 0.5686 0.4404 0.050 Uiso 1 1 calc R U . . .
C41 C 0.0457(5) 0.6742(5) 0.5360(2) 0.0462(14) Uani 1 1 d . . . . .
H41A H 0.0109 0.6005 0.5387 0.055 Uiso 1 1 calc R U . . .
H41B H -0.0019 0.7024 0.5471 0.055 Uiso 1 1 calc R U . . .
C42 C 0.1425(5) 0.7275(5) 0.5759(2) 0.0449(14) Uani 1 1 d . . . . .
H42A H 0.1799 0.8002 0.5713 0.054 Uiso 1 1 calc R U . . .
H42B H 0.1251 0.7245 0.6161 0.054 Uiso 1 1 calc R U . . .
C43 C 0.2955(5) 0.7255(5) 0.6046(2) 0.0536(17) Uani 1 1 d . . . . .
H43A H 0.2744 0.7158 0.6437 0.064 Uiso 1 1 calc R U . . .
H43B H 0.3341 0.7998 0.6038 0.064 Uiso 1 1 calc R U . . .
C44 C 0.3638(5) 0.6765(5) 0.5900(2) 0.0517(16) Uani 1 1 d . . . . .
H44A H 0.4215 0.7028 0.6208 0.062 Uiso 1 1 calc R U . . .
H44B H 0.3231 0.6018 0.5889 0.062 Uiso 1 1 calc R U . . .
C45 C 0.0064(4) 0.5102(4) 0.3388(2) 0.0378(12) Uani 1 1 d . . . . .
H45A H -0.0366 0.4985 0.3028 0.045 Uiso 1 1 calc R U . . .
H45B H -0.0410 0.4824 0.3684 0.045 Uiso 1 1 calc R U . . .
C46 C 0.0670(4) 0.4515(4) 0.3291(2) 0.0383(12) Uani 1 1 d . . . . .
H46A H 0.0192 0.3787 0.3144 0.046 Uiso 1 1 calc R U . . .
H46B H 0.1158 0.4791 0.3000 0.046 Uiso 1 1 calc R U . . .
C47 C 0.1722(4) 0.3967(4) 0.3744(2) 0.0327(11) Uani 1 1 d . . . . .
H47A H 0.2203 0.4175 0.3444 0.039 Uiso 1 1 calc R U . . .
H47B H 0.1193 0.3248 0.3617 0.039 Uiso 1 1 calc R U . . .
C48 C 0.2306(4) 0.4053(4) 0.4295(2) 0.0368(12) Uani 1 1 d . . . . .
H48A H 0.1819 0.3815 0.4590 0.044 Uiso 1 1 calc R U . . .
H48B H 0.2643 0.3608 0.4238 0.044 Uiso 1 1 calc R U . . .
C49 C 0.3700(5) 0.5163(5) 0.4984(2) 0.0456(14) Uani 1 1 d . . . . .
H49A H 0.4042 0.4729 0.4894 0.055 Uiso 1 1 calc R U . . .
H49B H 0.3259 0.4913 0.5298 0.055 Uiso 1 1 calc R U . . .
C50 C 0.4496(5) 0.6238(5) 0.5176(2) 0.0493(15) Uani 1 1 d . . . . .
H50A H 0.4938 0.6475 0.4861 0.059 Uiso 1 1 calc R U . . .
H50B H 0.4944 0.6263 0.5507 0.059 Uiso 1 1 calc R U . . .
C51 C 0.1181(4) 0.6702(4) 0.3081(2) 0.0384(13) Uani 1 1 d . . . . .
H51A H 0.0638 0.6697 0.2818 0.046 Uiso 1 1 calc R U . . .
H51B H 0.1474 0.6293 0.2867 0.046 Uiso 1 1 calc R U . . .
C52 C 0.2021(5) 0.7782(5) 0.3246(2) 0.0472(15) Uani 1 1 d . . . . .
H52A H 0.2254 0.8091 0.2897 0.057 Uiso 1 1 calc R U . . .
H52B H 0.1756 0.8193 0.3483 0.057 Uiso 1 1 calc R U . . .
C53 C 0.3684(5) 0.8802(4) 0.3734(3) 0.0493(15) Uani 1 1 d . . . . .
H53A H 0.3441 0.9195 0.4004 0.059 Uiso 1 1 calc R U . . .
H53B H 0.3884 0.9146 0.3393 0.059 Uiso 1 1 calc R U . . .
C54 C 0.4587(5) 0.8782(5) 0.4014(3) 0.0559(17) Uani 1 1 d . . . . .
H54A H 0.4808 0.8359 0.3752 0.067 Uiso 1 1 calc R U . . .
H54B H 0.5171 0.9484 0.4101 0.067 Uiso 1 1 calc R U . . .
C55 C 0.5204(5) 0.8371(5) 0.4832(3) 0.0640(19) Uani 1 1 d . . . . .
H55A H 0.5795 0.9070 0.4896 0.077 Uiso 1 1 calc R U . . .
H55B H 0.5416 0.7910 0.4598 0.077 Uiso 1 1 calc R U . . .
C56 C 0.4908(6) 0.8019(5) 0.5397(3) 0.0609(18) Uani 1 1 d . . . . .
H56A H 0.5527 0.8075 0.5615 0.073 Uiso 1 1 calc R U . . .
H56B H 0.4687 0.8481 0.5622 0.073 Uiso 1 1 calc R U . . .
N9 N 0.7307(4) 0.4637(4) 0.2904(2) 0.0612(15) Uani 1 1 d . . . . .
H9C H 0.6985 0.4441 0.3224 0.092 Uiso 1 1 d R U . . .
H9D H 0.7943 0.5183 0.3008 0.092 Uiso 1 1 d R U . . .
H9E H 0.7378 0.4109 0.2706 0.092 Uiso 1 1 d R U . . .
N10 N 0.7292(4) 0.2594(4) 0.2301(2) 0.0563(14) Uani 1 1 d . . . . .
H10C H 0.7842 0.2546 0.2457 0.084 Uiso 1 1 d R U . . .
H10D H 0.7337 0.2606 0.1918 0.084 Uiso 1 1 d R U . . .
H10E H 0.6694 0.2045 0.2355 0.084 Uiso 1 1 d R U . . .
N11 N 0.9029(4) 0.1652(4) 0.2328(2) 0.0562(14) Uani 1 1 d . . . . .
H11C H 0.9470 0.1950 0.2655 0.084 Uiso 1 1 d R U . . .
H11D H 0.9396 0.1792 0.2017 0.084 Uiso 1 1 d R U . . .
H11E H 0.8684 0.0963 0.2318 0.084 Uiso 1 1 d R U . . .
N12 N 0.0735(7) 0.1502(6) 0.4612(3) 0.120(3) Uani 1 1 d . . . . .
H12C H 0.0173 0.1270 0.4815 0.181 Uiso 1 1 d R U . . .
H12D H 0.1252 0.1429 0.4792 0.181 Uiso 1 1 d R U . . .
H12E H 0.0561 0.1134 0.4251 0.181 Uiso 1 1 d R U . . .
N13 N 0.2710(13) 0.2082(16) 0.5035(6) 0.096(8) Uani 0.388(15) 1 d . . P . .
H13C H 0.2817 0.2042 0.4656 0.143 Uiso 0.388(15) 1 d R U P . .
H13D H 0.2742 0.1557 0.5176 0.143 Uiso 0.388(15) 1 d R U P . .
H13E H 0.3206 0.2688 0.5233 0.143 Uiso 0.388(15) 1 d R U P . .
N14 N 0.1665(7) 0.9501(6) 0.4844(3) 0.130(4) Uani 1 1 d . . . . .
H14C H 0.1404 0.8809 0.4781 0.195 Uiso 1 1 d R U . . .
H14D H 0.2254 0.9787 0.5090 0.195 Uiso 1 1 d R U . . .
H14E H 0.1812 0.9738 0.4505 0.195 Uiso 1 1 d R U . . .


_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 2.5590(7) . ?
Ge1 Ge6 2.5717(7) . ?
Ge1 Zn 2.6437(9) . ?
Ge1 Ge4 2.7493(8) . ?
Ge1 Ge2 2.7643(8) . ?
Ge2 Ge7 2.5478(7) . ?
Ge2 Ge6 2.5692(7) . ?
Ge2 Zn 2.6001(8) . ?
Ge2 Ge3 2.7962(8) . ?
Ge3 Ge8 2.5494(7) . ?
Ge3 Ge7 2.5591(7) . ?
Ge3 Zn 2.5921(9) . ?
Ge3 Ge4 2.7868(8) . ?
Ge4 Ge8 2.5590(8) . ?
Ge4 Ge5 2.5742(7) . ?
Ge4 Zn 2.6105(8) . ?
Ge5 Ge9 2.5813(8) . ?
Ge5 Ge6 2.8036(8) . ?
Ge5 Ge8 2.8465(8) . ?
Ge6 Ge9 2.6001(8) . ?
Ge6 Ge7 2.8131(8) . ?
Ge7 Ge9 2.5645(8) . ?
Ge7 Ge8 2.8612(8) . ?
Ge8 Ge9 2.5733(8) . ?
Zn C1 2.015(5) . ?
C1 C2 1.515(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
K1 O1 2.804(4) . ?
K1 O4 2.814(3) . ?
K1 O6 2.834(4) . ?
K1 O3 2.836(4) . ?
K1 O5 2.860(3) . ?
K1 O2 2.920(3) . ?
K1 N2 2.967(5) . ?
K1 N1 2.985(5) . ?
K1 N7 3.273(5) . ?
N1 C15 1.460(6) . ?
N1 C3 1.474(6) . ?
N1 C9 1.478(6) . ?
N2 C8 1.466(6) . ?
N2 C14 1.482(7) . ?
N2 C20 1.483(7) . ?
O1 C5 1.433(6) . ?
O1 C4 1.437(6) . ?
O2 C7 1.420(7) . ?
O2 C6 1.439(6) . ?
O3 C11 1.434(6) . ?
O3 C10 1.437(6) . ?
O4 C12 1.417(6) . ?
O4 C13 1.440(6) . ?
O5 C17 1.424(6) . ?
O5 C16 1.427(7) . ?
O6 C18 1.432(6) . ?
O6 C19 1.434(7) . ?
C3 C4 1.494(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.472(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.517(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.500(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.495(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.508(8) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.514(8) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.475(8) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.493(8) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
N7 H7C 0.9100 . ?
N7 H7D 0.9100 . ?
N7 H7E 0.9100 . ?
K2 O10 2.783(3) . ?
K2 O11 2.805(4) . ?
K2 O12 2.841(4) . ?
K2 O9 2.842(3) . ?
K2 O7 2.867(3) . ?
K2 O8 2.876(3) . ?
K2 N4 2.994(4) . ?
K2 N3 3.073(4) . ?
K2 H8C 3.0614 . ?
N3 C21 1.472(6) . ?
N3 C27 1.476(6) . ?
N3 C33 1.480(6) . ?
N4 C32 1.469(7) . ?
N4 C38 1.472(6) . ?
N4 C26 1.481(6) . ?
O7 C23 1.427(6) . ?
O7 C22 1.428(6) . ?
O8 C24 1.427(6) . ?
O8 C25 1.441(6) . ?
O9 C29 1.425(6) . ?
O9 C28 1.427(6) . ?
O10 C30 1.425(6) . ?
O10 C31 1.435(6) . ?
O11 C34 1.436(6) . ?
O11 C35 1.438(6) . ?
O12 C37 1.422(6) . ?
O12 C36 1.432(6) . ?
C21 C22 1.513(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.513(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.494(7) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.509(7) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.494(7) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.506(7) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.497(7) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.496(8) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.504(7) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
N8 H8C 0.9100 . ?
N8 H8D 0.9100 . ?
N8 H8E 0.9100 . ?
K3 O18 2.824(4) . ?
K3 O15 2.824(4) . ?
K3 O16 2.828(4) . ?
K3 O17 2.843(3) . ?
K3 O13 2.844(4) . ?
K3 O14 2.852(3) . ?
K3 N6 2.960(5) . ?
K3 N5 3.005(4) . ?
N5 C45 1.467(7) . ?
N5 C39 1.475(6) . ?
N5 C51 1.475(6) . ?
N6 C44 1.474(7) . ?
N6 C56 1.479(8) . ?
N6 C50 1.487(7) . ?
O13 C40 1.421(7) . ?
O13 C41 1.421(6) . ?
O14 C42 1.417(7) . ?
O14 C43 1.418(7) . ?
O15 C47 1.426(6) . ?
O15 C46 1.433(6) . ?
O16 C49 1.419(6) . ?
O16 C48 1.434(6) . ?
O17 C52 1.430(7) . ?
O17 C53 1.431(7) . ?
O18 C54 1.427(7) . ?
O18 C55 1.446(8) . ?
C39 C40 1.503(7) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.487(8) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.507(8) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.508(7) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.492(7) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.482(8) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.499(8) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.474(9) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.502(9) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
N9 H9C 0.9100 . ?
N9 H9D 0.9100 . ?
N9 H9E 0.9100 . ?
N10 H10C 0.9100 . ?
N10 H10D 0.9100 . ?
N10 H10E 0.9100 . ?
N11 H11C 0.9100 . ?
N11 H11D 0.9100 . ?
N11 H11E 0.9100 . ?
N12 H12C 0.9100 . ?
N12 H12D 0.9100 . ?
N12 H12E 0.9100 . ?
N13 H13C 0.9100 . ?
N13 H13D 0.9100 . ?
N13 H13E 0.9100 . ?
N14 H14C 0.9100 . ?
N14 H14D 0.9100 . ?
N14 H14E 0.9100 . ?

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 66.24(2) . . ?
Ge5 Ge1 Zn 111.97(3) . . ?
Ge6 Ge1 Zn 111.31(3) . . ?
Ge5 Ge1 Ge4 57.88(2) . . ?
Ge6 Ge1 Ge4 103.98(2) . . ?
Zn Ge1 Ge4 57.86(2) . . ?
Ge5 Ge1 Ge2 103.84(2) . . ?
Ge6 Ge1 Ge2 57.43(2) . . ?
Zn Ge1 Ge2 57.42(2) . . ?
Ge4 Ge1 Ge2 90.40(2) . . ?
Ge7 Ge2 Ge6 66.70(2) . . ?
Ge7 Ge2 Zn 111.29(3) . . ?
Ge6 Ge2 Zn 112.83(3) . . ?
Ge7 Ge2 Ge1 103.87(2) . . ?
Ge6 Ge2 Ge1 57.52(2) . . ?
Zn Ge2 Ge1 58.96(2) . . ?
Ge7 Ge2 Ge3 57.00(2) . . ?
Ge6 Ge2 Ge3 103.54(2) . . ?
Zn Ge2 Ge3 57.28(2) . . ?
Ge1 Ge2 Ge3 90.06(2) . . ?
Ge8 Ge3 Ge7 68.12(2) . . ?
Ge8 Ge3 Zn 112.11(3) . . ?
Ge7 Ge3 Zn 111.18(3) . . ?
Ge8 Ge3 Ge4 57.10(2) . . ?
Ge7 Ge3 Ge4 103.45(2) . . ?
Zn Ge3 Ge4 57.93(2) . . ?
Ge8 Ge3 Ge2 104.11(2) . . ?
Ge7 Ge3 Ge2 56.61(2) . . ?
Zn Ge3 Ge2 57.55(2) . . ?
Ge4 Ge3 Ge2 88.98(2) . . ?
Ge8 Ge4 Ge5 67.36(2) . . ?
Ge8 Ge4 Zn 111.19(3) . . ?
Ge5 Ge4 Zn 112.57(3) . . ?
Ge8 Ge4 Ge1 104.69(2) . . ?
Ge5 Ge4 Ge1 57.35(2) . . ?
Zn Ge4 Ge1 59.04(2) . . ?
Ge8 Ge4 Ge3 56.77(2) . . ?
Ge5 Ge4 Ge3 103.59(2) . . ?
Zn Ge4 Ge3 57.29(2) . . ?
Ge1 Ge4 Ge3 90.56(2) . . ?
Ge1 Ge5 Ge4 64.77(2) . . ?
Ge1 Ge5 Ge9 109.61(3) . . ?
Ge4 Ge5 Ge9 108.08(3) . . ?
Ge1 Ge5 Ge6 57.095(19) . . ?
Ge4 Ge5 Ge6 102.41(2) . . ?
Ge9 Ge5 Ge6 57.57(2) . . ?
Ge1 Ge5 Ge8 101.98(2) . . ?
Ge4 Ge5 Ge8 56.07(2) . . ?
Ge9 Ge5 Ge8 56.35(2) . . ?
Ge6 Ge5 Ge8 90.70(2) . . ?
Ge2 Ge6 Ge1 65.06(2) . . ?
Ge2 Ge6 Ge9 108.19(3) . . ?
Ge1 Ge6 Ge9 108.62(3) . . ?
Ge2 Ge6 Ge5 102.49(2) . . ?
Ge1 Ge6 Ge5 56.661(19) . . ?
Ge9 Ge6 Ge5 56.92(2) . . ?
Ge2 Ge6 Ge7 56.29(2) . . ?
Ge1 Ge6 Ge7 101.90(2) . . ?
Ge9 Ge6 Ge7 56.39(2) . . ?
Ge5 Ge6 Ge7 90.47(2) . . ?
Ge2 Ge7 Ge3 66.39(2) . . ?
Ge2 Ge7 Ge9 109.97(3) . . ?
Ge3 Ge7 Ge9 108.39(3) . . ?
Ge2 Ge7 Ge6 57.01(2) . . ?
Ge3 Ge7 Ge6 103.34(2) . . ?
Ge9 Ge7 Ge6 57.61(2) . . ?
Ge2 Ge7 Ge8 102.34(2) . . ?
Ge3 Ge7 Ge8 55.779(19) . . ?
Ge9 Ge7 Ge8 56.31(2) . . ?
Ge6 Ge7 Ge8 90.20(2) . . ?
Ge3 Ge8 Ge4 66.12(2) . . ?
Ge3 Ge8 Ge9 108.42(3) . . ?
Ge4 Ge8 Ge9 108.80(3) . . ?
Ge3 Ge8 Ge5 102.59(2) . . ?
Ge4 Ge8 Ge5 56.58(2) . . ?
Ge9 Ge8 Ge5 56.61(2) . . ?
Ge3 Ge8 Ge7 56.100(19) . . ?
Ge4 Ge8 Ge7 101.42(2) . . ?
Ge9 Ge8 Ge7 56.01(2) . . ?
Ge5 Ge8 Ge7 88.64(2) . . ?
Ge7 Ge9 Ge8 67.68(2) . . ?
Ge7 Ge9 Ge5 101.60(2) . . ?
Ge8 Ge9 Ge5 67.04(2) . . ?
Ge7 Ge9 Ge6 66.00(2) . . ?
Ge8 Ge9 Ge6 101.96(2) . . ?
Ge5 Ge9 Ge6 65.51(2) . . ?
C1 Zn Ge3 132.13(17) . . ?
C1 Zn Ge2 125.19(16) . . ?
Ge3 Zn Ge2 65.17(2) . . ?
C1 Zn Ge4 137.39(16) . . ?
Ge3 Zn Ge4 64.78(2) . . ?
Ge2 Zn Ge4 97.33(2) . . ?
C1 Zn Ge1 129.97(17) . . ?
Ge3 Zn Ge1 97.41(2) . . ?
Ge2 Zn Ge1 63.62(2) . . ?
Ge4 Zn Ge1 63.10(2) . . ?
C2 C1 Zn 113.6(4) . . ?
C2 C1 H1A 108.8 . . ?
Zn C1 H1A 108.8 . . ?
C2 C1 H1B 108.8 . . ?
Zn C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O1 K1 O4 133.87(11) . . ?
O1 K1 O6 126.60(11) . . ?
O4 K1 O6 94.77(11) . . ?
O1 K1 O3 93.76(11) . . ?
O4 K1 O3 60.22(10) . . ?
O6 K1 O3 135.45(11) . . ?
O1 K1 O5 106.56(11) . . ?
O4 K1 O5 112.15(10) . . ?
O6 K1 O5 60.07(11) . . ?
O3 K1 O5 93.80(10) . . ?
O1 K1 O2 58.75(10) . . ?
O4 K1 O2 95.51(10) . . ?
O6 K1 O2 104.01(11) . . ?
O3 K1 O2 113.94(10) . . ?
O5 K1 O2 148.29(11) . . ?
O1 K1 N2 118.45(11) . . ?
O4 K1 N2 60.77(11) . . ?
O6 K1 N2 61.03(12) . . ?
O3 K1 N2 119.54(12) . . ?
O5 K1 N2 119.51(12) . . ?
O2 K1 N2 60.59(11) . . ?
O1 K1 N1 60.78(11) . . ?
O4 K1 N1 119.55(11) . . ?
O6 K1 N1 119.49(11) . . ?
O3 K1 N1 60.61(11) . . ?
O5 K1 N1 61.15(11) . . ?
O2 K1 N1 118.62(11) . . ?
N2 K1 N1 179.21(12) . . ?
O1 K1 N7 61.28(13) . . ?
O4 K1 N7 157.35(14) . . ?
O6 K1 N7 65.98(13) . . ?
O3 K1 N7 142.09(14) . . ?
O5 K1 N7 69.70(12) . . ?
O2 K1 N7 78.80(12) . . ?
N2 K1 N7 98.03(15) . . ?
N1 K1 N7 81.76(14) . . ?
C15 N1 C3 110.1(4) . . ?
C15 N1 C9 110.4(4) . . ?
C3 N1 C9 109.7(4) . . ?
C15 N1 K1 110.3(3) . . ?
C3 N1 K1 107.5(3) . . ?
C9 N1 K1 108.8(3) . . ?
C8 N2 C14 109.0(4) . . ?
C8 N2 C20 110.3(4) . . ?
C14 N2 C20 109.4(4) . . ?
C8 N2 K1 110.5(3) . . ?
C14 N2 K1 110.2(3) . . ?
C20 N2 K1 107.4(3) . . ?
C5 O1 C4 111.7(4) . . ?
C5 O1 K1 119.5(3) . . ?
C4 O1 K1 121.1(3) . . ?
C7 O2 C6 111.5(4) . . ?
C7 O2 K1 114.1(3) . . ?
C6 O2 K1 112.9(3) . . ?
C11 O3 C10 109.7(4) . . ?
C11 O3 K1 113.8(3) . . ?
C10 O3 K1 117.6(3) . . ?
C12 O4 C13 111.4(4) . . ?
C12 O4 K1 115.8(3) . . ?
C13 O4 K1 118.3(3) . . ?
C17 O5 C16 110.7(4) . . ?
C17 O5 K1 114.5(3) . . ?
C16 O5 K1 112.7(3) . . ?
C18 O6 C19 112.0(4) . . ?
C18 O6 K1 112.7(3) . . ?
C19 O6 K1 119.3(3) . . ?
N1 C3 C4 115.8(4) . . ?
N1 C3 H3A 108.3 . . ?
C4 C3 H3A 108.3 . . ?
N1 C3 H3B 108.3 . . ?
C4 C3 H3B 108.3 . . ?
H3A C3 H3B 107.4 . . ?
O1 C4 C3 109.6(4) . . ?
O1 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
O1 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
O1 C5 C6 109.0(4) . . ?
O1 C5 H5A 109.9 . . ?
C6 C5 H5A 109.9 . . ?
O1 C5 H5B 109.9 . . ?
C6 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
O2 C6 C5 110.5(4) . . ?
O2 C6 H6A 109.5 . . ?
C5 C6 H6A 109.5 . . ?
O2 C6 H6B 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
O2 C7 C8 108.8(4) . . ?
O2 C7 H7A 109.9 . . ?
C8 C7 H7A 109.9 . . ?
O2 C7 H7B 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
N2 C8 C7 114.6(5) . . ?
N2 C8 H8A 108.6 . . ?
C7 C8 H8A 108.6 . . ?
N2 C8 H8B 108.6 . . ?
C7 C8 H8B 108.6 . . ?
H8A C8 H8B 107.6 . . ?
N1 C9 C10 113.7(4) . . ?
N1 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
N1 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
O3 C10 C9 108.4(4) . . ?
O3 C10 H10A 110.0 . . ?
C9 C10 H10A 110.0 . . ?
O3 C10 H10B 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
O3 C11 C12 109.0(4) . . ?
O3 C11 H11A 109.9 . . ?
C12 C11 H11A 109.9 . . ?
O3 C11 H11B 109.9 . . ?
C12 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
O4 C12 C11 110.2(4) . . ?
O4 C12 H12A 109.6 . . ?
C11 C12 H12A 109.6 . . ?
O4 C12 H12B 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
O4 C13 C14 110.0(4) . . ?
O4 C13 H13A 109.7 . . ?
C14 C13 H13A 109.7 . . ?
O4 C13 H13B 109.7 . . ?
C14 C13 H13B 109.7 . . ?
H13A C13 H13B 108.2 . . ?
N2 C14 C13 112.6(5) . . ?
N2 C14 H14A 109.1 . . ?
C13 C14 H14A 109.1 . . ?
N2 C14 H14B 109.1 . . ?
C13 C14 H14B 109.1 . . ?
H14A C14 H14B 107.8 . . ?
N1 C15 C16 114.0(4) . . ?
N1 C15 H15A 108.8 . . ?
C16 C15 H15A 108.8 . . ?
N1 C15 H15B 108.8 . . ?
C16 C15 H15B 108.8 . . ?
H15A C15 H15B 107.6 . . ?
O5 C16 C15 110.0(4) . . ?
O5 C16 H16A 109.7 . . ?
C15 C16 H16A 109.7 . . ?
O5 C16 H16B 109.7 . . ?
C15 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
O5 C17 C18 110.0(5) . . ?
O5 C17 H17A 109.7 . . ?
C18 C17 H17A 109.7 . . ?
O5 C17 H17B 109.7 . . ?
C18 C17 H17B 109.7 . . ?
H17A C17 H17B 108.2 . . ?
O6 C18 C17 109.5(4) . . ?
O6 C18 H18A 109.8 . . ?
C17 C18 H18A 109.8 . . ?
O6 C18 H18B 109.8 . . ?
C17 C18 H18B 109.8 . . ?
H18A C18 H18B 108.2 . . ?
O6 C19 C20 109.6(4) . . ?
O6 C19 H19A 109.8 . . ?
C20 C19 H19A 109.8 . . ?
O6 C19 H19B 109.8 . . ?
C20 C19 H19B 109.8 . . ?
H19A C19 H19B 108.2 . . ?
N2 C20 C19 115.1(5) . . ?
N2 C20 H20A 108.5 . . ?
C19 C20 H20A 108.5 . . ?
N2 C20 H20B 108.5 . . ?
C19 C20 H20B 108.5 . . ?
H20A C20 H20B 107.5 . . ?
K1 N7 H7C 109.5 . . ?
K1 N7 H7D 109.5 . . ?
H7C N7 H7D 109.5 . . ?
K1 N7 H7E 109.5 . . ?
H7C N7 H7E 109.5 . . ?
H7D N7 H7E 109.5 . . ?
O10 K2 O11 115.88(11) . . ?
O10 K2 O12 94.13(11) . . ?
O11 K2 O12 59.85(10) . . ?
O10 K2 O9 60.80(10) . . ?
O11 K2 O9 93.39(10) . . ?
O12 K2 O9 132.26(10) . . ?
O10 K2 O7 137.31(11) . . ?
O11 K2 O7 100.24(11) . . ?
O12 K2 O7 124.66(11) . . ?
O9 K2 O7 96.83(10) . . ?
O10 K2 O8 98.13(10) . . ?
O11 K2 O8 141.68(11) . . ?
O12 K2 O8 102.71(10) . . ?
O9 K2 O8 119.61(10) . . ?
O7 K2 O8 59.70(9) . . ?
O10 K2 N4 61.31(10) . . ?
O11 K2 N4 119.83(11) . . ?
O12 K2 N4 60.56(11) . . ?
O9 K2 N4 121.31(11) . . ?
O7 K2 N4 119.65(10) . . ?
O8 K2 N4 60.98(10) . . ?
O10 K2 N3 119.62(10) . . ?
O11 K2 N3 60.11(11) . . ?
O12 K2 N3 119.22(11) . . ?
O9 K2 N3 59.58(10) . . ?
O7 K2 N3 59.61(10) . . ?
O8 K2 N3 118.41(10) . . ?
N4 K2 N3 179.05(11) . . ?
O10 K2 H8C 137.3 . . ?
O11 K2 H8C 64.3 . . ?
O12 K2 H8C 46.9 . . ?
O9 K2 H8C 155.2 . . ?
O7 K2 H8C 77.8 . . ?
O8 K2 H8C 78.9 . . ?
N4 K2 H8C 81.3 . . ?
N3 K2 H8C 97.9 . . ?
C21 N3 C27 110.6(4) . . ?
C21 N3 C33 108.9(4) . . ?
C27 N3 C33 110.9(4) . . ?
C21 N3 K2 108.7(3) . . ?
C27 N3 K2 109.0(3) . . ?
C33 N3 K2 108.7(3) . . ?
C32 N4 C38 110.8(4) . . ?
C32 N4 C26 109.2(4) . . ?
C38 N4 C26 109.5(4) . . ?
C32 N4 K2 108.6(3) . . ?
C38 N4 K2 108.9(3) . . ?
C26 N4 K2 109.8(3) . . ?
C23 O7 C22 110.3(4) . . ?
C23 O7 K2 114.6(3) . . ?
C22 O7 K2 118.1(3) . . ?
C24 O8 C25 109.6(4) . . ?
C24 O8 K2 114.8(3) . . ?
C25 O8 K2 112.8(3) . . ?
C29 O9 C28 111.0(3) . . ?
C29 O9 K2 112.8(3) . . ?
C28 O9 K2 118.5(3) . . ?
C30 O10 C31 109.8(4) . . ?
C30 O10 K2 116.7(3) . . ?
C31 O10 K2 115.7(3) . . ?
C34 O11 C35 110.7(4) . . ?
C34 O11 K2 115.8(3) . . ?
C35 O11 K2 117.9(3) . . ?
C37 O12 C36 111.0(4) . . ?
C37 O12 K2 117.6(3) . . ?
C36 O12 K2 112.4(3) . . ?
N3 C21 C22 114.0(4) . . ?
N3 C21 H21A 108.8 . . ?
C22 C21 H21A 108.8 . . ?
N3 C21 H21B 108.8 . . ?
C22 C21 H21B 108.8 . . ?
H21A C21 H21B 107.6 . . ?
O7 C22 C21 109.1(4) . . ?
O7 C22 H22A 109.9 . . ?
C21 C22 H22A 109.9 . . ?
O7 C22 H22B 109.9 . . ?
C21 C22 H22B 109.9 . . ?
H22A C22 H22B 108.3 . . ?
O7 C23 C24 110.1(4) . . ?
O7 C23 H23A 109.6 . . ?
C24 C23 H23A 109.6 . . ?
O7 C23 H23B 109.6 . . ?
C24 C23 H23B 109.6 . . ?
H23A C23 H23B 108.2 . . ?
O8 C24 C23 108.8(4) . . ?
O8 C24 H24A 109.9 . . ?
C23 C24 H24A 109.9 . . ?
O8 C24 H24B 109.9 . . ?
C23 C24 H24B 109.9 . . ?
H24A C24 H24B 108.3 . . ?
O8 C25 C26 109.5(4) . . ?
O8 C25 H25A 109.8 . . ?
C26 C25 H25A 109.8 . . ?
O8 C25 H25B 109.8 . . ?
C26 C25 H25B 109.8 . . ?
H25A C25 H25B 108.2 . . ?
N4 C26 C25 113.7(4) . . ?
N4 C26 H26A 108.8 . . ?
C25 C26 H26A 108.8 . . ?
N4 C26 H26B 108.8 . . ?
C25 C26 H26B 108.8 . . ?
H26A C26 H26B 107.7 . . ?
N3 C27 C28 113.2(4) . . ?
N3 C27 H27A 108.9 . . ?
C28 C27 H27A 108.9 . . ?
N3 C27 H27B 108.9 . . ?
C28 C27 H27B 108.9 . . ?
H27A C27 H27B 107.7 . . ?
O9 C28 C27 109.6(4) . . ?
O9 C28 H28A 109.7 . . ?
C27 C28 H28A 109.7 . . ?
O9 C28 H28B 109.7 . . ?
C27 C28 H28B 109.7 . . ?
H28A C28 H28B 108.2 . . ?
O9 C29 C30 111.2(4) . . ?
O9 C29 H29A 109.4 . . ?
C30 C29 H29A 109.4 . . ?
O9 C29 H29B 109.4 . . ?
C30 C29 H29B 109.4 . . ?
H29A C29 H29B 108.0 . . ?
O10 C30 C29 109.8(4) . . ?
O10 C30 H30A 109.7 . . ?
C29 C30 H30A 109.7 . . ?
O10 C30 H30B 109.7 . . ?
C29 C30 H30B 109.7 . . ?
H30A C30 H30B 108.2 . . ?
O10 C31 C32 108.6(4) . . ?
O10 C31 H31A 110.0 . . ?
C32 C31 H31A 110.0 . . ?
O10 C31 H31B 110.0 . . ?
C32 C31 H31B 110.0 . . ?
H31A C31 H31B 108.4 . . ?
N4 C32 C31 114.2(4) . . ?
N4 C32 H32A 108.7 . . ?
C31 C32 H32A 108.7 . . ?
N4 C32 H32B 108.7 . . ?
C31 C32 H32B 108.7 . . ?
H32A C32 H32B 107.6 . . ?
N3 C33 C34 113.6(4) . . ?
N3 C33 H33A 108.8 . . ?
C34 C33 H33A 108.8 . . ?
N3 C33 H33B 108.8 . . ?
C34 C33 H33B 108.8 . . ?
H33A C33 H33B 107.7 . . ?
O11 C34 C33 109.3(4) . . ?
O11 C34 H34A 109.8 . . ?
C33 C34 H34A 109.8 . . ?
O11 C34 H34B 109.8 . . ?
C33 C34 H34B 109.8 . . ?
H34A C34 H34B 108.3 . . ?
O11 C35 C36 108.8(5) . . ?
O11 C35 H35A 109.9 . . ?
C36 C35 H35A 109.9 . . ?
O11 C35 H35B 109.9 . . ?
C36 C35 H35B 109.9 . . ?
H35A C35 H35B 108.3 . . ?
O12 C36 C35 109.1(4) . . ?
O12 C36 H36A 109.9 . . ?
C35 C36 H36A 109.9 . . ?
O12 C36 H36B 109.9 . . ?
C35 C36 H36B 109.9 . . ?
H36A C36 H36B 108.3 . . ?
O12 C37 C38 109.8(4) . . ?
O12 C37 H37A 109.7 . . ?
C38 C37 H37A 109.7 . . ?
O12 C37 H37B 109.7 . . ?
C38 C37 H37B 109.7 . . ?
H37A C37 H37B 108.2 . . ?
N4 C38 C37 113.5(4) . . ?
N4 C38 H38A 108.9 . . ?
C37 C38 H38A 108.9 . . ?
N4 C38 H38B 108.9 . . ?
C37 C38 H38B 108.9 . . ?
H38A C38 H38B 107.7 . . ?
H8C N8 H8D 109.5 . . ?
H8C N8 H8E 109.5 . . ?
H8D N8 H8E 109.5 . . ?
O18 K3 O15 142.27(12) . . ?
O18 K3 O16 100.69(13) . . ?
O15 K3 O16 59.88(10) . . ?
O18 K3 O17 59.93(12) . . ?
O15 K3 O17 100.51(10) . . ?
O16 K3 O17 121.18(11) . . ?
O18 K3 O13 116.50(13) . . ?
O15 K3 O13 96.29(11) . . ?
O16 K3 O13 137.38(11) . . ?
O17 K3 O13 96.22(11) . . ?
O18 K3 O14 97.57(12) . . ?
O15 K3 O14 115.59(11) . . ?
O16 K3 O14 96.67(10) . . ?
O17 K3 O14 137.69(11) . . ?
O13 K3 O14 60.10(10) . . ?
O18 K3 N6 61.01(13) . . ?
O15 K3 N6 119.36(12) . . ?
O16 K3 N6 60.77(12) . . ?
O17 K3 N6 119.77(13) . . ?
O13 K3 N6 119.69(12) . . ?
O14 K3 N6 60.88(12) . . ?
O18 K3 N5 119.35(12) . . ?
O15 K3 N5 60.81(11) . . ?
O16 K3 N5 119.55(11) . . ?
O17 K3 N5 60.71(12) . . ?
O13 K3 N5 59.62(11) . . ?
O14 K3 N5 118.40(12) . . ?
N6 K3 N5 179.28(13) . . ?
C45 N5 C39 109.4(4) . . ?
C45 N5 C51 110.4(4) . . ?
C39 N5 C51 109.9(4) . . ?
C45 N5 K3 109.1(3) . . ?
C39 N5 K3 110.2(3) . . ?
C51 N5 K3 107.8(3) . . ?
C44 N6 C56 110.3(5) . . ?
C44 N6 C50 108.7(5) . . ?
C56 N6 C50 109.1(5) . . ?
C44 N6 K3 109.4(4) . . ?
C56 N6 K3 110.2(3) . . ?
C50 N6 K3 109.1(3) . . ?
C40 O13 C41 110.8(4) . . ?
C40 O13 K3 119.8(3) . . ?
C41 O13 K3 114.9(3) . . ?
C42 O14 C43 110.6(4) . . ?
C42 O14 K3 113.0(3) . . ?
C43 O14 K3 116.6(3) . . ?
C47 O15 C46 109.8(4) . . ?
C47 O15 K3 117.1(3) . . ?
C46 O15 K3 117.3(3) . . ?
C49 O16 C48 111.3(4) . . ?
C49 O16 K3 118.6(3) . . ?
C48 O16 K3 115.5(3) . . ?
C52 O17 C53 110.6(4) . . ?
C52 O17 K3 117.5(3) . . ?
C53 O17 K3 113.4(3) . . ?
C54 O18 C55 111.3(5) . . ?
C54 O18 K3 115.8(3) . . ?
C55 O18 K3 117.1(3) . . ?
N5 C39 C40 114.3(4) . . ?
N5 C39 H39A 108.7 . . ?
C40 C39 H39A 108.7 . . ?
N5 C39 H39B 108.7 . . ?
C40 C39 H39B 108.7 . . ?
H39A C39 H39B 107.6 . . ?
O13 C40 C39 108.9(5) . . ?
O13 C40 H40A 109.9 . . ?
C39 C40 H40A 109.9 . . ?
O13 C40 H40B 109.9 . . ?
C39 C40 H40B 109.9 . . ?
H40A C40 H40B 108.3 . . ?
O13 C41 C42 110.2(5) . . ?
O13 C41 H41A 109.6 . . ?
C42 C41 H41A 109.6 . . ?
O13 C41 H41B 109.6 . . ?
C42 C41 H41B 109.6 . . ?
H41A C41 H41B 108.1 . . ?
O14 C42 C41 110.0(5) . . ?
O14 C42 H42A 109.7 . . ?
C41 C42 H42A 109.7 . . ?
O14 C42 H42B 109.7 . . ?
C41 C42 H42B 109.7 . . ?
H42A C42 H42B 108.2 . . ?
O14 C43 C44 109.5(5) . . ?
O14 C43 H43A 109.8 . . ?
C44 C43 H43A 109.8 . . ?
O14 C43 H43B 109.8 . . ?
C44 C43 H43B 109.8 . . ?
H43A C43 H43B 108.2 . . ?
N6 C44 C43 113.5(5) . . ?
N6 C44 H44A 108.9 . . ?
C43 C44 H44A 108.9 . . ?
N6 C44 H44B 108.9 . . ?
C43 C44 H44B 108.9 . . ?
H44A C44 H44B 107.7 . . ?
N5 C45 C46 114.7(5) . . ?
N5 C45 H45A 108.6 . . ?
C46 C45 H45A 108.6 . . ?
N5 C45 H45B 108.6 . . ?
C46 C45 H45B 108.6 . . ?
H45A C45 H45B 107.6 . . ?
O15 C46 C45 109.5(4) . . ?
O15 C46 H46A 109.8 . . ?
C45 C46 H46A 109.8 . . ?
O15 C46 H46B 109.8 . . ?
C45 C46 H46B 109.8 . . ?
H46A C46 H46B 108.2 . . ?
O15 C47 C48 110.1(4) . . ?
O15 C47 H47A 109.6 . . ?
C48 C47 H47A 109.6 . . ?
O15 C47 H47B 109.6 . . ?
C48 C47 H47B 109.6 . . ?
H47A C47 H47B 108.2 . . ?
O16 C48 C47 110.9(4) . . ?
O16 C48 H48A 109.5 . . ?
C47 C48 H48A 109.5 . . ?
O16 C48 H48B 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 108.1 . . ?
O16 C49 C50 110.4(5) . . ?
O16 C49 H49A 109.6 . . ?
C50 C49 H49A 109.6 . . ?
O16 C49 H49B 109.6 . . ?
C50 C49 H49B 109.6 . . ?
H49A C49 H49B 108.1 . . ?
C49 C50 N6 114.3(5) . . ?
C49 C50 H50A 108.7 . . ?
N6 C50 H50A 108.7 . . ?
C49 C50 H50B 108.7 . . ?
N6 C50 H50B 108.7 . . ?
H50A C50 H50B 107.6 . . ?
N5 C51 C52 114.2(4) . . ?
N5 C51 H51A 108.7 . . ?
C52 C51 H51A 108.7 . . ?
N5 C51 H51B 108.7 . . ?
C52 C51 H51B 108.7 . . ?
H51A C51 H51B 107.6 . . ?
O17 C52 C51 109.0(4) . . ?
O17 C52 H52A 109.9 . . ?
C51 C52 H52A 109.9 . . ?
O17 C52 H52B 109.9 . . ?
C51 C52 H52B 109.9 . . ?
H52A C52 H52B 108.3 . . ?
O17 C53 C54 109.9(5) . . ?
O17 C53 H53A 109.7 . . ?
C54 C53 H53A 109.7 . . ?
O17 C53 H53B 109.7 . . ?
C54 C53 H53B 109.7 . . ?
H53A C53 H53B 108.2 . . ?
O18 C54 C53 109.7(5) . . ?
O18 C54 H54A 109.7 . . ?
C53 C54 H54A 109.7 . . ?
O18 C54 H54B 109.7 . . ?
C53 C54 H54B 109.7 . . ?
H54A C54 H54B 108.2 . . ?
O18 C55 C56 108.9(6) . . ?
O18 C55 H55A 109.9 . . ?
C56 C55 H55A 109.9 . . ?
O18 C55 H55B 109.9 . . ?
C56 C55 H55B 109.9 . . ?
H55A C55 H55B 108.3 . . ?
N6 C56 C55 114.0(5) . . ?
N6 C56 H56A 108.7 . . ?
C55 C56 H56A 108.7 . . ?
N6 C56 H56B 108.7 . . ?
C55 C56 H56B 108.7 . . ?
H56A C56 H56B 107.6 . . ?
H9C N9 H9D 109.5 . . ?
H9C N9 H9E 109.5 . . ?
H9D N9 H9E 109.5 . . ?
H10C N10 H10D 109.5 . . ?
H10C N10 H10E 109.5 . . ?
H10D N10 H10E 109.5 . . ?
H11C N11 H11D 109.5 . . ?
H11C N11 H11E 109.5 . . ?
H11D N11 H11E 109.5 . . ?
H12C N12 H12D 109.5 . . ?
H12C N12 H12E 109.5 . . ?
H12D N12 H12E 109.5 . . ?
H13C N13 H13D 109.5 . . ?
H13C N13 H13E 109.5 . . ?
H13D N13 H13E 109.5 . . ?
H14C N14 H14D 109.5 . . ?
H14C N14 H14E 109.5 . . ?
H14D N14 H14E 109.5 . . ?

_refine_diff_density_max         1.012
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.121


#============================================================================== 
# END of CIF  
#============================================================================== 
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ammonia'
####################################################################### 
# 
# 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_KM-668
_database_code_depnum_ccdc_archive 'CCDC 1982124'
loop_
_audit_author_name
_audit_author_address
'Wilhelm Klein'
;Technische Universitaet Muenchen
Germany
;
_audit_update_record             
;
2020-02-05 deposited with the CCDC.	2020-04-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         '2(C12 H30 K N2 O6), C8 H36 N8 Zn5, H3 N'
_chemical_formula_sum            'C32 H99 K2 N13 O12 Zn5'
_chemical_formula_weight         1263.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.554(2)
_cell_length_b                   14.140(3)
_cell_length_c                   18.988(4)
_cell_angle_alpha                89.02(3)
_cell_angle_beta                 77.37(3)
_cell_angle_gamma                87.11(3)
_cell_volume                     3023.2(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    177980
_cell_measurement_theta_min      3.345
_cell_measurement_theta_max      34.015

_exptl_crystal_description       column
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_exptl_absorpt_coefficient_mu    2.148
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.875
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            69261
_diffrn_reflns_av_unetI/netI     0.0114
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.423
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             11852
_reflns_number_gt                10537
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_computing_data_collection       'STOE X-AREA 1.76'
_computing_cell_refinement       'STOE X-AREA 1.76'
_computing_data_reduction        'STOE X-AREA 1.76'
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  SHELXL-2014/7
_computing_molecular_graphics    'DIAMOND 3.2k'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0237P)²+3.0835P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11852
_refine_ls_number_parameters     611
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0668
_refine_ls_wR_factor_gt          0.0613
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.79740(2) 0.40189(2) 0.23892(2) 0.02924(6) Uani 1 1 d . . . . .
Zn2 Zn 0.66436(3) 0.61265(2) 0.31820(2) 0.03186(7) Uani 1 1 d . . . . .
Zn3 Zn 0.91586(3) 0.58439(2) 0.31693(2) 0.03356(7) Uani 1 1 d . . . . .
Zn4 Zn 0.91558(2) 0.25427(2) 0.09308(2) 0.02881(6) Uani 1 1 d . . . . .
Zn5 Zn 0.82431(2) 0.15669(2) 0.22809(2) 0.02823(6) Uani 1 1 d . . . . .
N1 N 0.64619(16) 0.48804(13) 0.26739(10) 0.0292(4) Uani 1 1 d . . . . .
H1C H 0.5896 0.4547 0.2971 0.035 Uiso 1 1 calc R U . . .
H1D H 0.6192 0.5027 0.2268 0.035 Uiso 1 1 calc R U . . .
N2 N 0.93925(18) 0.44925(16) 0.27329(12) 0.0419(5) Uani 1 1 d . . . . .
H2C H 1.0028 0.4484 0.2353 0.050 Uiso 1 1 calc R U . . .
H2D H 0.9571 0.4080 0.3071 0.050 Uiso 1 1 calc R U . . .
N3 N 0.84816(18) 0.38819(13) 0.12949(10) 0.0332(4) Uani 1 1 d . . . . .
H3C H 0.9044 0.4307 0.1126 0.040 Uiso 1 1 calc R U . . .
H3D H 0.7844 0.4037 0.1100 0.040 Uiso 1 1 calc R U . . .
N4 N 0.75531(17) 0.27435(13) 0.28867(10) 0.0306(4) Uani 1 1 d . . . . .
H4C H 0.6748 0.2718 0.3006 0.037 Uiso 1 1 calc R U . . .
H4D H 0.7818 0.2718 0.3305 0.037 Uiso 1 1 calc R U . . .
N5 N 0.8182(2) 0.65622(16) 0.25145(11) 0.0414(5) Uani 1 1 d . . . . .
H5C H 0.8252 0.7201 0.2506 0.050 Uiso 1 1 calc R U . . .
H5D H 0.8313 0.6328 0.2059 0.050 Uiso 1 1 calc R U . . .
N6 N 0.76062(18) 0.56035(14) 0.39288(10) 0.0332(4) Uani 1 1 d . . . . .
H6C H 0.7507 0.5962 0.4333 0.040 Uiso 1 1 calc R U . . .
H6D H 0.7501 0.4982 0.4044 0.040 Uiso 1 1 calc R U . . .
N7 N 0.76173(16) 0.18347(13) 0.13475(10) 0.0291(4) Uani 1 1 d . . . . .
H7C H 0.6942 0.2213 0.1417 0.035 Uiso 1 1 calc R U . . .
H7D H 0.7544 0.1304 0.1099 0.035 Uiso 1 1 calc R U . . .
N8 N 0.98990(17) 0.20449(15) 0.17754(11) 0.0348(4) Uani 1 1 d . . . . .
H8C H 1.0158 0.2509 0.2021 0.042 Uiso 1 1 calc R U . . .
H8D H 1.0469 0.1573 0.1648 0.042 Uiso 1 1 calc R U . . .
C25 C 0.5213(2) 0.70678(16) 0.34709(13) 0.0371(5) Uani 1 1 d . . . . .
H25A H 0.5418 0.7544 0.3794 0.044 Uiso 1 1 calc R U . . .
H25B H 0.5092 0.7406 0.3030 0.044 Uiso 1 1 calc R U . . .
C26 C 0.4029(3) 0.66613(17) 0.38478(15) 0.0437(6) Uani 1 1 d . . . . .
H26A H 0.3410 0.7172 0.3938 0.066 Uiso 1 1 calc R U . . .
H26B H 0.4109 0.6369 0.4307 0.066 Uiso 1 1 calc R U . . .
H26C H 0.3810 0.6183 0.3539 0.066 Uiso 1 1 calc R U . . .
C27 C 1.0585(2) 0.65113(18) 0.33680(13) 0.0391(6) Uani 1 1 d . . . . .
H27A H 1.0347 0.6825 0.3843 0.047 Uiso 1 1 calc R U . . .
H27B H 1.1223 0.6028 0.3398 0.047 Uiso 1 1 calc R U . . .
C28 C 1.1080(2) 0.72452(18) 0.28030(15) 0.0413(6) Uani 1 1 d . . . . .
H28A H 1.1247 0.6958 0.2323 0.062 Uiso 1 1 calc R U . . .
H28B H 1.1816 0.7474 0.2902 0.062 Uiso 1 1 calc R U . . .
H28C H 1.0498 0.7777 0.2820 0.062 Uiso 1 1 calc R U . . .
C29 C 1.0033(2) 0.23848(17) -0.01141(13) 0.0352(5) Uani 1 1 d . . . . .
H29A H 1.0893 0.2426 -0.0137 0.042 Uiso 1 1 calc R U . . .
H29B H 0.9908 0.1740 -0.0270 0.042 Uiso 1 1 calc R U . . .
C30 C 0.9683(3) 0.3090(3) -0.06493(15) 0.0634(9) Uani 1 1 d . . . . .
H30A H 1.0147 0.2943 -0.1135 0.095 Uiso 1 1 calc R U . . .
H30B H 0.9842 0.3731 -0.0519 0.095 Uiso 1 1 calc R U . . .
H30C H 0.8836 0.3053 -0.0640 0.095 Uiso 1 1 calc R U . . .
C31 C 0.81646(19) 0.02159(15) 0.26747(12) 0.0288(5) Uani 1 1 d . . . . .
H31A H 0.8185 0.0223 0.3193 0.035 Uiso 1 1 calc R U . . .
H31B H 0.7404 -0.0044 0.2632 0.035 Uiso 1 1 calc R U . . .
C32 C 0.9196(2) -0.0428(2) 0.22705(16) 0.0465(6) Uani 1 1 d . . . . .
H32A H 0.9195 -0.0420 0.1754 0.070 Uiso 1 1 calc R U . . .
H32B H 0.9103 -0.1076 0.2458 0.070 Uiso 1 1 calc R U . . .
H32C H 0.9949 -0.0199 0.2341 0.070 Uiso 1 1 calc R U . . .
K1 K 0.24704(4) 0.17915(3) 0.42840(3) 0.03089(11) Uani 1 1 d . . . . .
O1 O 0.04902(14) 0.30624(11) 0.41660(9) 0.0338(4) Uani 1 1 d . . . . .
O2 O 0.26532(14) 0.37197(10) 0.43653(8) 0.0302(3) Uani 1 1 d . . . . .
O3 O 0.47677(14) 0.25350(11) 0.41308(8) 0.0322(3) Uani 1 1 d . . . . .
O4 O 0.44838(14) 0.05619(11) 0.42083(9) 0.0327(3) Uani 1 1 d . . . . .
O5 O 0.24262(16) -0.00810(11) 0.38186(9) 0.0372(4) Uani 1 1 d . . . . .
O6 O 0.02781(15) 0.10668(12) 0.42379(10) 0.0383(4) Uani 1 1 d . . . . .
C1 C 0.0565(2) 0.39626(16) 0.44832(13) 0.0355(5) Uani 1 1 d . . . . .
H1A H 0.0463 0.3893 0.5013 0.043 Uiso 1 1 calc R U . . .
H1B H -0.0070 0.4409 0.4385 0.043 Uiso 1 1 calc R U . . .
C2 C 0.1762(2) 0.43352(16) 0.41608(13) 0.0359(5) Uani 1 1 d . . . . .
H2A H 0.1886 0.4362 0.3628 0.043 Uiso 1 1 calc R U . . .
H2B H 0.1811 0.4983 0.4338 0.043 Uiso 1 1 calc R U . . .
C3 C 0.3808(2) 0.40664(17) 0.41201(14) 0.0388(6) Uani 1 1 d . . . . .
H3A H 0.3815 0.4731 0.4275 0.047 Uiso 1 1 calc R U . . .
H3B H 0.4030 0.4050 0.3586 0.047 Uiso 1 1 calc R U . . .
C4 C 0.4679(2) 0.34623(17) 0.44284(14) 0.0365(5) Uani 1 1 d . . . . .
H4A H 0.5467 0.3744 0.4312 0.044 Uiso 1 1 calc R U . . .
H4B H 0.4414 0.3428 0.4960 0.044 Uiso 1 1 calc R U . . .
C5 C 0.5487(2) 0.18975(18) 0.44623(13) 0.0352(5) Uani 1 1 d . . . . .
H5A H 0.5112 0.1812 0.4979 0.042 Uiso 1 1 calc R U . . .
H5B H 0.6279 0.2156 0.4428 0.042 Uiso 1 1 calc R U . . .
C6 C 0.5615(2) 0.09655(18) 0.40809(13) 0.0365(5) Uani 1 1 d . . . . .
H6A H 0.5918 0.1061 0.3556 0.044 Uiso 1 1 calc R U . . .
H6B H 0.6187 0.0535 0.4264 0.044 Uiso 1 1 calc R U . . .
C7 C 0.4506(2) -0.02496(17) 0.37740(15) 0.0415(6) Uani 1 1 d . . . . .
H7A H 0.5152 -0.0704 0.3844 0.050 Uiso 1 1 calc R U . . .
H7B H 0.4659 -0.0062 0.3258 0.050 Uiso 1 1 calc R U . . .
C8 C 0.3339(2) -0.07069(17) 0.39808(15) 0.0417(6) Uani 1 1 d . . . . .
H8A H 0.3374 -0.1305 0.3712 0.050 Uiso 1 1 calc R U . . .
H8B H 0.3162 -0.0858 0.4503 0.050 Uiso 1 1 calc R U . . .
C9 C 0.1291(3) -0.04582(18) 0.40475(19) 0.0508(7) Uani 1 1 d . . . . .
H9A H 0.1111 -0.0549 0.4578 0.061 Uiso 1 1 calc R U . . .
H9B H 0.1283 -0.1082 0.3821 0.061 Uiso 1 1 calc R U . . .
C10 C 0.0364(3) 0.0207(2) 0.3838(2) 0.0586(9) Uani 1 1 d . . . . .
H10A H 0.0583 0.0347 0.3315 0.070 Uiso 1 1 calc R U . . .
H10B H -0.0413 -0.0091 0.3942 0.070 Uiso 1 1 calc R U . . .
C11 C -0.0605(2) 0.17165(19) 0.40597(15) 0.0412(6) Uani 1 1 d . . . . .
H11A H -0.1397 0.1446 0.4202 0.049 Uiso 1 1 calc R U . . .
H11B H -0.0433 0.1834 0.3532 0.049 Uiso 1 1 calc R U . . .
C12 C -0.0600(2) 0.26317(18) 0.44523(14) 0.0386(6) Uani 1 1 d . . . . .
H12A H -0.1276 0.3058 0.4387 0.046 Uiso 1 1 calc R U . . .
H12B H -0.0681 0.2507 0.4975 0.046 Uiso 1 1 calc R U . . .
N9 N 0.2094(2) 0.18889(17) 0.58724(13) 0.0526(6) Uani 1 1 d . . . . .
H9C H 0.2675 0.2223 0.5992 0.079 Uiso 1 1 calc R U . . .
H9D H 0.2117 0.1293 0.6058 0.079 Uiso 1 1 calc R U . . .
H9E H 0.1373 0.2181 0.6056 0.079 Uiso 1 1 calc R U . . .
N10A N 0.2345(9) 0.2120(11) 0.2786(4) 0.105(3) Uani 0.86(3) 1 d . U P . .
H10C H 0.1765 0.2572 0.2764 0.157 Uiso 0.86(3) 1 calc R U P . .
H10D H 0.2175 0.1573 0.2593 0.157 Uiso 0.86(3) 1 calc R U P . .
H10E H 0.3055 0.2317 0.2533 0.157 Uiso 0.86(3) 1 calc R U P . .
N10B N 0.229(3) 0.2334(16) 0.2782(17) 0.024(9) Uani 0.14(3) 1 d . . P . .
H10F H 0.1955 0.2193 0.2406 0.036 Uiso 0.14(3) 1 calc R U P . .
H10G H 0.1946 0.2887 0.2987 0.036 Uiso 0.14(3) 1 calc R U P . .
H10H H 0.2164 0.1860 0.3117 0.036 Uiso 0.14(3) 1 calc R U P . .
K2 K 0.5000 0.5000 0.0000 0.03021(14) Uani 1 2 d S . P . .
O7 O 0.29402(15) 0.50853(12) 0.10965(9) 0.0395(4) Uani 1 1 d . . . . .
O8 O 0.50198(15) 0.58240(11) 0.13344(8) 0.0342(4) Uani 1 1 d . . . . .
O9 O 0.69104(15) 0.61250(12) 0.01141(9) 0.0382(4) Uani 1 1 d . . . . .
C13 C 0.2108(3) 0.4384(2) 0.10640(17) 0.0617(9) Uani 1 1 d . . . . .
H13A H 0.1326 0.4576 0.1371 0.074 Uiso 1 1 calc R U . . .
H13B H 0.2380 0.3773 0.1249 0.074 Uiso 1 1 calc R U . . .
C14 C 0.3109(3) 0.5233(2) 0.18093(14) 0.0517(7) Uani 1 1 d . . . . .
H14A H 0.3486 0.4656 0.1983 0.062 Uiso 1 1 calc R U . . .
H14B H 0.2334 0.5368 0.2143 0.062 Uiso 1 1 calc R U . . .
C15 C 0.3892(2) 0.6055(2) 0.17917(13) 0.0440(6) Uani 1 1 d . . . . .
H15A H 0.3525 0.6627 0.1606 0.053 Uiso 1 1 calc R U . . .
H15B H 0.3990 0.6188 0.2285 0.053 Uiso 1 1 calc R U . . .
C16 C 0.5811(2) 0.65789(16) 0.12870(13) 0.0342(5) Uani 1 1 d . . . . .
H16A H 0.5885 0.6758 0.1776 0.041 Uiso 1 1 calc R U . . .
H16B H 0.5496 0.7140 0.1057 0.041 Uiso 1 1 calc R U . . .
C17 C 0.6996(2) 0.62601(17) 0.08487(13) 0.0365(5) Uani 1 1 d . . . . .
H17A H 0.7582 0.6741 0.0868 0.044 Uiso 1 1 calc R U . . .
H17B H 0.7269 0.5659 0.1048 0.044 Uiso 1 1 calc R U . . .
C18 C 0.8012(2) 0.5731(2) -0.03053(17) 0.0541(8) Uani 1 1 d . . . . .
H18A H 0.8207 0.5109 -0.0102 0.065 Uiso 1 1 calc R U . . .
H18B H 0.8661 0.6156 -0.0291 0.065 Uiso 1 1 calc R U . . .
N11 N 0.6277(2) 0.31740(16) 0.01236(13) 0.0469(5) Uani 1 1 d . . . . .
H11C H 0.5794 0.2694 0.0095 0.070 Uiso 1 1 calc R U . . .
H11D H 0.6497 0.3141 0.0555 0.070 Uiso 1 1 calc R U . . .
H11E H 0.6935 0.3121 -0.0241 0.070 Uiso 1 1 calc R U . . .
K3 K 0.5000 0.0000 0.0000 0.03051(14) Uani 1 2 d S . P . .
O10 O 0.49142(14) -0.09037(12) 0.13375(8) 0.0329(3) Uani 1 1 d . . . . .
O11 O 0.27598(14) -0.03411(11) 0.09522(9) 0.0326(3) Uani 1 1 d . . . . .
O12 O 0.29511(13) 0.01641(11) -0.05182(9) 0.0316(3) Uani 1 1 d . . . . .
C19 C 0.3822(2) -0.0791(2) 0.18574(13) 0.0403(6) Uani 1 1 d . . . . .
H19A H 0.3710 -0.0131 0.2036 0.048 Uiso 1 1 calc R U . . .
H19B H 0.3833 -0.1221 0.2273 0.048 Uiso 1 1 calc R U . . .
C20 C 0.2827(2) -0.10178(19) 0.15072(14) 0.0405(6) Uani 1 1 d . . . . .
H20A H 0.2969 -0.1662 0.1300 0.049 Uiso 1 1 calc R U . . .
H20B H 0.2068 -0.1001 0.1871 0.049 Uiso 1 1 calc R U . . .
C21 C 0.1904(2) -0.05824(18) 0.05497(13) 0.0353(5) Uani 1 1 d . . . . .
H21A H 0.1116 -0.0634 0.0879 0.042 Uiso 1 1 calc R U . . .
H21B H 0.2138 -0.1201 0.0312 0.042 Uiso 1 1 calc R U . . .
C22 C 0.1837(2) 0.01677(19) -0.00051(14) 0.0375(5) Uani 1 1 d . . . . .
H22A H 0.1191 0.0044 -0.0253 0.045 Uiso 1 1 calc R U . . .
H22B H 0.1665 0.0795 0.0229 0.045 Uiso 1 1 calc R U . . .
C23 C 0.2970(2) 0.0880(2) -0.10617(14) 0.0404(6) Uani 1 1 d . . . . .
H23A H 0.2948 0.1514 -0.0846 0.048 Uiso 1 1 calc R U . . .
H23B H 0.2265 0.0842 -0.1276 0.048 Uiso 1 1 calc R U . . .
C24 C 0.4085(2) 0.0731(2) -0.16366(13) 0.0408(6) Uani 1 1 d . . . . .
H24A H 0.4147 0.0074 -0.1818 0.049 Uiso 1 1 calc R U . . .
H24B H 0.4064 0.1169 -0.2047 0.049 Uiso 1 1 calc R U . . .
N12 N 0.3873(2) 0.17836(17) 0.07015(14) 0.0551(6) Uani 1 1 d . . . . .
H12C H 0.3796 0.2222 0.0357 0.083 Uiso 1 1 calc R U . . .
H12D H 0.4335 0.2007 0.0987 0.083 Uiso 1 1 calc R U . . .
H12E H 0.3144 0.1667 0.0976 0.083 Uiso 1 1 calc R U . . .
N13A N 0.4894(5) 0.3201(9) 0.1911(6) 0.076(4) Uani 0.53(2) 1 d . . P . .
H13C H 0.5069 0.2645 0.2123 0.114 Uiso 0.53(2) 1 calc R U P . .
H13D H 0.4095 0.3274 0.1954 0.114 Uiso 0.53(2) 1 calc R U P . .
H13E H 0.5151 0.3690 0.2133 0.114 Uiso 0.53(2) 1 calc R U P . .
N13B N 0.4871(8) 0.2539(17) 0.2252(7) 0.113(6) Uani 0.47(2) 1 d . U P . .
H13F H 0.5244 0.1955 0.2179 0.169 Uiso 0.47(2) 1 calc R U P . .
H13G H 0.5161 0.2855 0.2585 0.169 Uiso 0.47(2) 1 calc R U P . .
H13H H 0.5002 0.2870 0.1829 0.169 Uiso 0.47(2) 1 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N2 2.038(2) . ?
Zn1 N3 2.042(2) . ?
Zn1 N4 2.052(2) . ?
Zn1 N1 2.0550(19) . ?
Zn2 C25 2.052(3) . ?
Zn2 N5 2.060(2) . ?
Zn2 N1 2.0649(19) . ?
Zn2 N6 2.089(2) . ?
Zn2 Zn3 2.9081(7) . ?
Zn3 C27 2.047(2) . ?
Zn3 N5 2.075(2) . ?
Zn3 N2 2.077(2) . ?
Zn3 N6 2.080(2) . ?
Zn4 C29 2.031(2) . ?
Zn4 N8 2.075(2) . ?
Zn4 N7 2.080(2) . ?
Zn4 N3 2.081(2) . ?
Zn4 Zn5 2.9037(10) . ?
Zn5 C31 2.039(2) . ?
Zn5 N4 2.063(2) . ?
Zn5 N7 2.0778(19) . ?
Zn5 N8 2.084(2) . ?
N1 H1C 0.9100 . ?
N1 H1D 0.9100 . ?
N2 H2C 0.9100 . ?
N2 H2D 0.9100 . ?
N3 H3C 0.9100 . ?
N3 H3D 0.9100 . ?
N4 H4C 0.9100 . ?
N4 H4D 0.9100 . ?
N5 H5C 0.9100 . ?
N5 H5D 0.9100 . ?
N6 H6C 0.9100 . ?
N6 H6D 0.9100 . ?
N7 H7C 0.9100 . ?
N7 H7D 0.9100 . ?
N8 H8C 0.9100 . ?
N8 H8D 0.9100 . ?
C25 C26 1.534(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.520(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.515(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.534(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
K1 O2 2.7548(16) . ?
K1 O6 2.7992(18) . ?
K1 O5 2.8121(18) . ?
K1 O4 2.8124(18) . ?
K1 O3 2.8581(18) . ?
K1 O1 2.8827(18) . ?
K1 N10A 2.908(8) . ?
K1 N9 2.956(2) . ?
K1 N10B 2.99(3) . ?
O1 C12 1.422(3) . ?
O1 C1 1.432(3) . ?
O2 C3 1.423(3) . ?
O2 C2 1.429(3) . ?
O3 C5 1.426(3) . ?
O3 C4 1.427(3) . ?
O4 C7 1.420(3) . ?
O4 C6 1.423(3) . ?
O5 C9 1.417(3) . ?
O5 C8 1.424(3) . ?
O6 C11 1.430(3) . ?
O6 C10 1.431(3) . ?
C1 C2 1.503(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.497(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.500(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.496(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.504(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.505(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
N9 H9C 0.9100 . ?
N9 H9D 0.9100 . ?
N9 H9E 0.9100 . ?
N10A H10C 0.9100 . ?
N10A H10D 0.9100 . ?
N10A H10E 0.9100 . ?
N10B N13B 2.96(3) . ?
N10B H10F 0.9100 . ?
N10B H10G 0.9100 . ?
N10B H10H 0.9100 . ?
K2 O7 2.7976(19) 2_665 ?
K2 O7 2.7976(19) . ?
K2 O8 2.8119(17) 2_665 ?
K2 O8 2.8119(17) . ?
K2 O9 2.8328(18) . ?
K2 O9 2.8328(18) 2_665 ?
K2 N11 2.940(2) . ?
K2 N11 2.940(2) 2_665 ?
O7 C13 1.427(3) . ?
O7 C14 1.429(3) . ?
O8 C15 1.425(3) . ?
O8 C16 1.429(3) . ?
O9 C17 1.436(3) . ?
O9 C18 1.437(3) . ?
C13 C18 1.489(4) 2_665 ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.504(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.491(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C13 1.489(4) 2_665 ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
N11 N13A 3.421(11) . ?
N11 H11C 0.9100 . ?
N11 H11D 0.9100 . ?
N11 H11E 0.9100 . ?
K3 O12 2.7535(16) . ?
K3 O12 2.7535(16) 2_655 ?
K3 O10 2.8079(17) 2_655 ?
K3 O10 2.8079(17) . ?
K3 O11 2.8724(18) . ?
K3 O11 2.8724(18) 2_655 ?
K3 N12 2.976(3) 2_655 ?
K3 N12 2.976(3) . ?
O10 C19 1.425(3) . ?
O10 C24 1.428(3) 2_655 ?
O11 C20 1.423(3) . ?
O11 C21 1.432(3) . ?
O12 C23 1.430(3) . ?
O12 C22 1.434(3) . ?
C19 C20 1.499(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.493(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.504(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 O10 1.428(3) 2_655 ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
N12 H12C 0.9100 . ?
N12 H12D 0.9100 . ?
N12 H12E 0.9100 . ?
N13A H13C 0.9100 . ?
N13A H13D 0.9100 . ?
N13A H13E 0.9100 . ?
N13B H13F 0.9100 . ?
N13B H13G 0.9100 . ?
N13B H13H 0.9100 . ?

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
N2 Zn1 N3 106.87(9) . . ?
N2 Zn1 N4 108.02(9) . . ?
N3 Zn1 N4 111.63(8) . . ?
N2 Zn1 N1 113.78(8) . . ?
N3 Zn1 N1 111.13(8) . . ?
N4 Zn1 N1 105.44(8) . . ?
C25 Zn2 N5 119.75(10) . . ?
C25 Zn2 N1 119.86(9) . . ?
N5 Zn2 N1 99.32(9) . . ?
C25 Zn2 N6 121.85(9) . . ?
N5 Zn2 N6 90.44(8) . . ?
N1 Zn2 N6 99.60(8) . . ?
C25 Zn2 Zn3 143.02(7) . . ?
N5 Zn2 Zn3 45.51(6) . . ?
N1 Zn2 Zn3 97.09(6) . . ?
N6 Zn2 Zn3 45.64(6) . . ?
C27 Zn3 N5 116.48(9) . . ?
C27 Zn3 N2 119.88(10) . . ?
N5 Zn3 N2 102.54(9) . . ?
C27 Zn3 N6 125.19(9) . . ?
N5 Zn3 N6 90.31(8) . . ?
N2 Zn3 N6 96.56(9) . . ?
C27 Zn3 Zn2 142.71(8) . . ?
N5 Zn3 Zn2 45.11(6) . . ?
N2 Zn3 Zn2 97.25(6) . . ?
N6 Zn3 Zn2 45.91(6) . . ?
C29 Zn4 N8 121.44(9) . . ?
C29 Zn4 N7 121.41(9) . . ?
N8 Zn4 N7 90.59(8) . . ?
C29 Zn4 N3 119.08(9) . . ?
N8 Zn4 N3 101.79(8) . . ?
N7 Zn4 N3 96.42(8) . . ?
C29 Zn4 Zn5 145.19(7) . . ?
N8 Zn4 Zn5 45.85(6) . . ?
N7 Zn4 Zn5 45.67(5) . . ?
N3 Zn4 Zn5 95.65(6) . . ?
C31 Zn5 N4 123.90(8) . . ?
C31 Zn5 N7 117.19(9) . . ?
N4 Zn5 N7 101.08(8) . . ?
C31 Zn5 N8 118.05(9) . . ?
N4 Zn5 N8 99.87(8) . . ?
N7 Zn5 N8 90.41(8) . . ?
C31 Zn5 Zn4 138.47(7) . . ?
N4 Zn5 Zn4 97.62(6) . . ?
N7 Zn5 Zn4 45.73(5) . . ?
N8 Zn5 Zn4 45.60(6) . . ?
Zn1 N1 Zn2 115.87(9) . . ?
Zn1 N1 H1C 108.3 . . ?
Zn2 N1 H1C 108.3 . . ?
Zn1 N1 H1D 108.3 . . ?
Zn2 N1 H1D 108.3 . . ?
H1C N1 H1D 107.4 . . ?
Zn1 N2 Zn3 115.39(11) . . ?
Zn1 N2 H2C 108.4 . . ?
Zn3 N2 H2C 108.4 . . ?
Zn1 N2 H2D 108.4 . . ?
Zn3 N2 H2D 108.4 . . ?
H2C N2 H2D 107.5 . . ?
Zn1 N3 Zn4 115.42(10) . . ?
Zn1 N3 H3C 108.4 . . ?
Zn4 N3 H3C 108.4 . . ?
Zn1 N3 H3D 108.4 . . ?
Zn4 N3 H3D 108.4 . . ?
H3C N3 H3D 107.5 . . ?
Zn1 N4 Zn5 115.01(9) . . ?
Zn1 N4 H4C 108.5 . . ?
Zn5 N4 H4C 108.5 . . ?
Zn1 N4 H4D 108.5 . . ?
Zn5 N4 H4D 108.5 . . ?
H4C N4 H4D 107.5 . . ?
Zn2 N5 Zn3 89.38(8) . . ?
Zn2 N5 H5C 113.7 . . ?
Zn3 N5 H5C 113.7 . . ?
Zn2 N5 H5D 113.7 . . ?
Zn3 N5 H5D 113.7 . . ?
H5C N5 H5D 111.0 . . ?
Zn3 N6 Zn2 88.45(7) . . ?
Zn3 N6 H6C 113.9 . . ?
Zn2 N6 H6C 113.9 . . ?
Zn3 N6 H6D 113.9 . . ?
Zn2 N6 H6D 113.9 . . ?
H6C N6 H6D 111.1 . . ?
Zn5 N7 Zn4 88.60(7) . . ?
Zn5 N7 H7C 113.9 . . ?
Zn4 N7 H7C 113.9 . . ?
Zn5 N7 H7D 113.9 . . ?
Zn4 N7 H7D 113.9 . . ?
H7C N7 H7D 111.1 . . ?
Zn4 N8 Zn5 88.54(8) . . ?
Zn4 N8 H8C 113.9 . . ?
Zn5 N8 H8C 113.9 . . ?
Zn4 N8 H8D 113.9 . . ?
Zn5 N8 H8D 113.9 . . ?
H8C N8 H8D 111.1 . . ?
C26 C25 Zn2 117.09(16) . . ?
C26 C25 H25A 108.0 . . ?
Zn2 C25 H25A 108.0 . . ?
C26 C25 H25B 108.0 . . ?
Zn2 C25 H25B 108.0 . . ?
H25A C25 H25B 107.3 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 Zn3 114.32(17) . . ?
C28 C27 H27A 108.7 . . ?
Zn3 C27 H27A 108.7 . . ?
C28 C27 H27B 108.7 . . ?
Zn3 C27 H27B 108.7 . . ?
H27A C27 H27B 107.6 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 Zn4 116.22(18) . . ?
C30 C29 H29A 108.2 . . ?
Zn4 C29 H29A 108.2 . . ?
C30 C29 H29B 108.2 . . ?
Zn4 C29 H29B 108.2 . . ?
H29A C29 H29B 107.4 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 Zn5 111.97(17) . . ?
C32 C31 H31A 109.2 . . ?
Zn5 C31 H31A 109.2 . . ?
C32 C31 H31B 109.2 . . ?
Zn5 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O2 K1 O6 119.51(5) . . ?
O2 K1 O5 165.27(5) . . ?
O6 K1 O5 61.38(6) . . ?
O2 K1 O4 120.30(5) . . ?
O6 K1 O4 120.17(5) . . ?
O5 K1 O4 60.53(5) . . ?
O2 K1 O3 60.95(5) . . ?
O6 K1 O3 172.54(5) . . ?
O5 K1 O3 116.07(6) . . ?
O4 K1 O3 59.71(5) . . ?
O2 K1 O1 59.81(5) . . ?
O6 K1 O1 60.03(5) . . ?
O5 K1 O1 117.27(5) . . ?
O4 K1 O1 172.78(5) . . ?
O3 K1 O1 119.02(5) . . ?
O2 K1 N10A 86.3(3) . . ?
O6 K1 N10A 77.82(19) . . ?
O5 K1 N10A 79.5(3) . . ?
O4 K1 N10A 104.4(3) . . ?
O3 K1 N10A 94.90(19) . . ?
O1 K1 N10A 68.5(3) . . ?
O2 K1 N9 83.26(7) . . ?
O6 K1 N9 97.03(7) . . ?
O5 K1 N9 111.44(7) . . ?
O4 K1 N9 91.20(7) . . ?
O3 K1 N9 90.42(7) . . ?
O1 K1 N9 95.95(7) . . ?
N10A K1 N9 164.2(3) . . ?
O2 K1 N10B 80.8(4) . . ?
O6 K1 N10B 79.3(5) . . ?
O5 K1 N10B 85.1(4) . . ?
O4 K1 N10B 108.5(6) . . ?
O3 K1 N10B 93.6(5) . . ?
O1 K1 N10B 64.3(6) . . ?
N10A K1 N10B 5.8(6) . . ?
N9 K1 N10B 159.1(5) . . ?
C12 O1 C1 112.84(18) . . ?
C12 O1 K1 110.45(13) . . ?
C1 O1 K1 111.66(13) . . ?
C3 O2 C2 111.70(17) . . ?
C3 O2 K1 116.33(13) . . ?
C2 O2 K1 118.78(13) . . ?
C5 O3 C4 111.85(18) . . ?
C5 O3 K1 109.01(13) . . ?
C4 O3 K1 110.85(13) . . ?
C7 O4 C6 111.39(18) . . ?
C7 O4 K1 114.30(14) . . ?
C6 O4 K1 117.97(13) . . ?
C9 O5 C8 111.66(19) . . ?
C9 O5 K1 112.24(14) . . ?
C8 O5 K1 114.66(14) . . ?
C11 O6 C10 111.10(19) . . ?
C11 O6 K1 117.03(14) . . ?
C10 O6 K1 114.23(16) . . ?
O1 C1 C2 108.29(19) . . ?
O1 C1 H1A 110.0 . . ?
C2 C1 H1A 110.0 . . ?
O1 C1 H1B 110.0 . . ?
C2 C1 H1B 110.0 . . ?
H1A C1 H1B 108.4 . . ?
O2 C2 C1 108.66(18) . . ?
O2 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
O2 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.3 . . ?
O2 C3 C4 109.18(19) . . ?
O2 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 . . ?
O2 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.3 . . ?
O3 C4 C3 109.3(2) . . ?
O3 C4 H4A 109.8 . . ?
C3 C4 H4A 109.8 . . ?
O3 C4 H4B 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.3 . . ?
O3 C5 C6 108.49(19) . . ?
O3 C5 H5A 110.0 . . ?
C6 C5 H5A 110.0 . . ?
O3 C5 H5B 110.0 . . ?
C6 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
O4 C6 C5 108.68(18) . . ?
O4 C6 H6A 110.0 . . ?
C5 C6 H6A 110.0 . . ?
O4 C6 H6B 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.3 . . ?
O4 C7 C8 109.4(2) . . ?
O4 C7 H7A 109.8 . . ?
C8 C7 H7A 109.8 . . ?
O4 C7 H7B 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
O5 C8 C7 109.5(2) . . ?
O5 C8 H8A 109.8 . . ?
C7 C8 H8A 109.8 . . ?
O5 C8 H8B 109.8 . . ?
C7 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
O5 C9 C10 109.7(2) . . ?
O5 C9 H9A 109.7 . . ?
C10 C9 H9A 109.7 . . ?
O5 C9 H9B 109.7 . . ?
C10 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
O6 C10 C9 109.3(2) . . ?
O6 C10 H10A 109.8 . . ?
C9 C10 H10A 109.8 . . ?
O6 C10 H10B 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.3 . . ?
O6 C11 C12 109.05(19) . . ?
O6 C11 H11A 109.9 . . ?
C12 C11 H11A 109.9 . . ?
O6 C11 H11B 109.9 . . ?
C12 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
O1 C12 C11 108.3(2) . . ?
O1 C12 H12A 110.0 . . ?
C11 C12 H12A 110.0 . . ?
O1 C12 H12B 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
K1 N9 H9C 109.5 . . ?
K1 N9 H9D 109.5 . . ?
H9C N9 H9D 109.5 . . ?
K1 N9 H9E 109.5 . . ?
H9C N9 H9E 109.5 . . ?
H9D N9 H9E 109.5 . . ?
K1 N10A H10C 109.5 . . ?
K1 N10A H10D 109.5 . . ?
H10C N10A H10D 109.5 . . ?
K1 N10A H10E 109.5 . . ?
H10C N10A H10E 109.5 . . ?
H10D N10A H10E 109.5 . . ?
N13B N10B K1 94.7(8) . . ?
N13B N10B H10F 109.5 . . ?
K1 N10B H10F 144.8 . . ?
N13B N10B H10G 109.5 . . ?
K1 N10B H10G 84.7 . . ?
H10F N10B H10G 109.5 . . ?
N13B N10B H10H 109.5 . . ?
H10F N10B H10H 109.5 . . ?
H10G N10B H10H 109.5 . . ?
O7 K2 O7 180.0 2_665 . ?
O7 K2 O8 59.77(5) 2_665 2_665 ?
O7 K2 O8 120.23(5) . 2_665 ?
O7 K2 O8 120.23(5) 2_665 . ?
O7 K2 O8 59.77(5) . . ?
O8 K2 O8 180.0 2_665 . ?
O7 K2 O9 61.03(5) 2_665 . ?
O7 K2 O9 118.97(5) . . ?
O8 K2 O9 119.17(5) 2_665 . ?
O8 K2 O9 60.84(5) . . ?
O7 K2 O9 118.97(5) 2_665 2_665 ?
O7 K2 O9 61.03(5) . 2_665 ?
O8 K2 O9 60.83(5) 2_665 2_665 ?
O8 K2 O9 119.16(5) . 2_665 ?
O9 K2 O9 180.0 . 2_665 ?
O7 K2 N11 71.89(7) 2_665 . ?
O7 K2 N11 108.11(7) . . ?
O8 K2 N11 78.95(6) 2_665 . ?
O8 K2 N11 101.05(6) . . ?
O9 K2 N11 95.44(6) . . ?
O9 K2 N11 84.56(6) 2_665 . ?
O7 K2 N11 108.11(7) 2_665 2_665 ?
O7 K2 N11 71.89(7) . 2_665 ?
O8 K2 N11 101.05(6) 2_665 2_665 ?
O8 K2 N11 78.95(6) . 2_665 ?
O9 K2 N11 84.56(6) . 2_665 ?
O9 K2 N11 95.44(6) 2_665 2_665 ?
N11 K2 N11 180.0 . 2_665 ?
C13 O7 C14 113.4(2) . . ?
C13 O7 K2 115.41(15) . . ?
C14 O7 K2 115.93(15) . . ?
C15 O8 C16 111.95(18) . . ?
C15 O8 K2 116.52(14) . . ?
C16 O8 K2 114.11(13) . . ?
C17 O9 C18 110.6(2) . . ?
C17 O9 K2 112.70(14) . . ?
C18 O9 K2 110.75(14) . . ?
O7 C13 C18 110.0(2) . 2_665 ?
O7 C13 H13A 109.7 . . ?
C18 C13 H13A 109.7 2_665 . ?
O7 C13 H13B 109.7 . . ?
C18 C13 H13B 109.7 2_665 . ?
H13A C13 H13B 108.2 . . ?
O7 C14 C15 108.7(2) . . ?
O7 C14 H14A 110.0 . . ?
C15 C14 H14A 110.0 . . ?
O7 C14 H14B 110.0 . . ?
C15 C14 H14B 110.0 . . ?
H14A C14 H14B 108.3 . . ?
O8 C15 C14 108.8(2) . . ?
O8 C15 H15A 109.9 . . ?
C14 C15 H15A 109.9 . . ?
O8 C15 H15B 109.9 . . ?
C14 C15 H15B 109.9 . . ?
H15A C15 H15B 108.3 . . ?
O8 C16 C17 108.91(19) . . ?
O8 C16 H16A 109.9 . . ?
C17 C16 H16A 109.9 . . ?
O8 C16 H16B 109.9 . . ?
C17 C16 H16B 109.9 . . ?
H16A C16 H16B 108.3 . . ?
O9 C17 C16 109.47(19) . . ?
O9 C17 H17A 109.8 . . ?
C16 C17 H17A 109.8 . . ?
O9 C17 H17B 109.8 . . ?
C16 C17 H17B 109.8 . . ?
H17A C17 H17B 108.2 . . ?
O9 C18 C13 108.9(3) . 2_665 ?
O9 C18 H18A 109.9 . . ?
C13 C18 H18A 109.9 2_665 . ?
O9 C18 H18B 109.9 . . ?
C13 C18 H18B 109.9 2_665 . ?
H18A C18 H18B 108.3 . . ?
K2 N11 N13A 86.7(2) . . ?
K2 N11 H11C 109.5 . . ?
N13A N11 H11C 84.5 . . ?
K2 N11 H11D 109.5 . . ?
H11C N11 H11D 109.5 . . ?
K2 N11 H11E 109.5 . . ?
N13A N11 H11E 152.4 . . ?
H11C N11 H11E 109.5 . . ?
H11D N11 H11E 109.5 . . ?
O12 K3 O12 180.0 . 2_655 ?
O12 K3 O10 61.65(5) . 2_655 ?
O12 K3 O10 118.35(5) 2_655 2_655 ?
O12 K3 O10 118.35(5) . . ?
O12 K3 O10 61.65(5) 2_655 . ?
O10 K3 O10 180.0 2_655 . ?
O12 K3 O11 60.45(5) . . ?
O12 K3 O11 119.54(5) 2_655 . ?
O10 K3 O11 120.53(5) 2_655 . ?
O10 K3 O11 59.47(5) . . ?
O12 K3 O11 119.55(5) . 2_655 ?
O12 K3 O11 60.46(5) 2_655 2_655 ?
O10 K3 O11 59.47(5) 2_655 2_655 ?
O10 K3 O11 120.53(5) . 2_655 ?
O11 K3 O11 180.0 . 2_655 ?
O12 K3 N12 101.21(7) . 2_655 ?
O12 K3 N12 78.79(7) 2_655 2_655 ?
O10 K3 N12 92.13(7) 2_655 2_655 ?
O10 K3 N12 87.87(7) . 2_655 ?
O11 K3 N12 111.00(6) . 2_655 ?
O11 K3 N12 69.01(6) 2_655 2_655 ?
O12 K3 N12 78.79(7) . . ?
O12 K3 N12 101.21(7) 2_655 . ?
O10 K3 N12 87.87(7) 2_655 . ?
O10 K3 N12 92.13(7) . . ?
O11 K3 N12 69.00(6) . . ?
O11 K3 N12 110.99(6) 2_655 . ?
N12 K3 N12 180.0 2_655 . ?
C19 O10 C24 112.11(18) . 2_655 ?
C19 O10 K3 116.28(13) . . ?
C24 O10 K3 113.02(13) 2_655 . ?
C20 O11 C21 111.39(18) . . ?
C20 O11 K3 114.34(13) . . ?
C21 O11 K3 110.62(13) . . ?
C23 O12 C22 112.40(18) . . ?
C23 O12 K3 113.77(13) . . ?
C22 O12 K3 117.93(13) . . ?
O10 C19 C20 108.6(2) . . ?
O10 C19 H19A 110.0 . . ?
C20 C19 H19A 110.0 . . ?
O10 C19 H19B 110.0 . . ?
C20 C19 H19B 110.0 . . ?
H19A C19 H19B 108.3 . . ?
O11 C20 C19 109.1(2) . . ?
O11 C20 H20A 109.9 . . ?
C19 C20 H20A 109.9 . . ?
O11 C20 H20B 109.9 . . ?
C19 C20 H20B 109.9 . . ?
H20A C20 H20B 108.3 . . ?
O11 C21 C22 109.12(19) . . ?
O11 C21 H21A 109.9 . . ?
C22 C21 H21A 109.9 . . ?
O11 C21 H21B 109.9 . . ?
C22 C21 H21B 109.9 . . ?
H21A C21 H21B 108.3 . . ?
O12 C22 C21 108.89(19) . . ?
O12 C22 H22A 109.9 . . ?
C21 C22 H22A 109.9 . . ?
O12 C22 H22B 109.9 . . ?
C21 C22 H22B 109.9 . . ?
H22A C22 H22B 108.3 . . ?
O12 C23 C24 108.9(2) . . ?
O12 C23 H23A 109.9 . . ?
C24 C23 H23A 109.9 . . ?
O12 C23 H23B 109.9 . . ?
C24 C23 H23B 109.9 . . ?
H23A C23 H23B 108.3 . . ?
O10 C24 C23 109.0(2) 2_655 . ?
O10 C24 H24A 109.9 2_655 . ?
C23 C24 H24A 109.9 . . ?
O10 C24 H24B 109.9 2_655 . ?
C23 C24 H24B 109.9 . . ?
H24A C24 H24B 108.3 . . ?
K3 N12 H12C 109.5 . . ?
K3 N12 H12D 109.5 . . ?
H12C N12 H12D 109.5 . . ?
K3 N12 H12E 109.5 . . ?
H12C N12 H12E 109.5 . . ?
H12D N12 H12E 109.5 . . ?
N11 N13A H13C 109.5 . . ?
N11 N13A H13D 109.5 . . ?
H13C N13A H13D 109.5 . . ?
N11 N13A H13E 109.5 . . ?
H13C N13A H13E 109.5 . . ?
H13D N13A H13E 109.5 . . ?
N10B N13B H13F 109.5 . . ?
N10B N13B H13G 109.5 . . ?
H13F N13B H13G 109.5 . . ?
N10B N13B H13H 109.5 . . ?
H13F N13B H13H 109.5 . . ?
H13G N13B H13H 109.5 . . ?

_refine_diff_density_max         0.768
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.056


#============================================================================== 
# END of CIF  
#============================================================================== 
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ammonia'
####################################################################### 
# 
# 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_CW-34
_database_code_depnum_ccdc_archive 'CCDC 1982128'
loop_
_audit_author_name
_audit_author_address
'Wilhelm Klein'
;Technische Universitaet Muenchen
Germany
;
_audit_update_record             
;
2020-02-05 deposited with the CCDC.	2020-04-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C22 H39 K O6, 2(H3 N)'
_chemical_formula_sum            'C22 H45 K N2 O6'
_chemical_formula_weight         472.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.1910(2)
_cell_length_b                   16.1458(3)
_cell_length_c                   32.8773(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5409.7(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    188962
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      33.53

_exptl_crystal_description       fragment
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_exptl_absorpt_coefficient_mu    0.231
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            148069
_diffrn_reflns_av_unetI/netI     0.0115
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         3.007
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5311
_reflns_number_gt                4543
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_computing_data_collection       'STOE X-AREA 1.76'
_computing_cell_refinement       'STOE X-AREA 1.76'
_computing_data_reduction        'STOE X-AREA 1.76'
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  SHELXL-2014/7
_computing_molecular_graphics    'DIAMOND 3.2k'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0511P)²+2.1500P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5311
_refine_ls_number_parameters     295
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0987
_refine_ls_wR_factor_gt          0.0939
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K K 0.50772(3) 0.34842(2) 0.13215(2) 0.02746(10) Uani 1 1 d . . . . .
O1 O 0.37851(10) 0.30318(6) 0.05447(3) 0.0339(2) Uani 1 1 d . . . . .
O2 O 0.64936(11) 0.33682(7) 0.04840(3) 0.0407(3) Uani 1 1 d . . . . .
O3 O 0.79068(11) 0.35687(7) 0.12026(4) 0.0461(3) Uani 1 1 d . . . . .
O4 O 0.68966(12) 0.27888(7) 0.19016(3) 0.0438(3) Uani 1 1 d . . . . .
O5 O 0.42503(13) 0.22969(7) 0.20032(3) 0.0450(3) Uani 1 1 d . . . . .
O6 O 0.29988(10) 0.21977(7) 0.12467(3) 0.0374(3) Uani 1 1 d . . . . .
C1 C 0.44676(17) 0.30668(11) 0.01685(5) 0.0416(4) Uani 1 1 d . . . . .
H1A H 0.3861 0.3237 -0.0051 0.050 Uiso 1 1 calc R U . . .
H1B H 0.4825 0.2514 0.0100 0.050 Uiso 1 1 calc R U . . .
C2 C 0.55595(18) 0.36788(11) 0.02053(5) 0.0437(4) Uani 1 1 d . . . . .
H2A H 0.5975 0.3767 -0.0063 0.052 Uiso 1 1 calc R U . . .
H2B H 0.5214 0.4216 0.0303 0.052 Uiso 1 1 calc R U . . .
C3 C 0.76290(17) 0.38802(11) 0.05066(6) 0.0470(4) Uani 1 1 d . . . . .
H3A H 0.7375 0.4451 0.0583 0.056 Uiso 1 1 calc R U . . .
H3B H 0.8071 0.3900 0.0239 0.056 Uiso 1 1 calc R U . . .
C4 C 0.85294(16) 0.35313(12) 0.08161(6) 0.0523(5) Uani 1 1 d . . . . .
H4A H 0.8743 0.2950 0.0748 0.063 Uiso 1 1 calc R U . . .
H4B H 0.9357 0.3853 0.0822 0.063 Uiso 1 1 calc R U . . .
C5 C 0.87226(18) 0.32439(13) 0.15150(7) 0.0599(5) Uani 1 1 d . . . . .
H5A H 0.9556 0.3558 0.1527 0.072 Uiso 1 1 calc R U . . .
H5B H 0.8930 0.2656 0.1458 0.072 Uiso 1 1 calc R U . . .
C6 C 0.8014(2) 0.33149(13) 0.19093(7) 0.0624(6) Uani 1 1 d . . . . .
H6A H 0.8601 0.3152 0.2135 0.075 Uiso 1 1 calc R U . . .
H6B H 0.7736 0.3895 0.1954 0.075 Uiso 1 1 calc R U . . .
C7 C 0.6292(2) 0.26935(14) 0.22877(5) 0.0614(6) Uani 1 1 d . . . . .
H7A H 0.5866 0.3219 0.2370 0.074 Uiso 1 1 calc R U . . .
H7B H 0.6958 0.2548 0.2495 0.074 Uiso 1 1 calc R U . . .
C8 C 0.5294(2) 0.20225(14) 0.22576(5) 0.0607(6) Uani 1 1 d . . . . .
H8A H 0.5698 0.1518 0.2141 0.073 Uiso 1 1 calc R U . . .
H8B H 0.4953 0.1887 0.2531 0.073 Uiso 1 1 calc R U . . .
C9 C 0.3382(2) 0.16391(10) 0.18972(5) 0.0507(5) Uani 1 1 d . . . . .
H9A H 0.2966 0.1413 0.2146 0.061 Uiso 1 1 calc R U . . .
H9B H 0.3879 0.1188 0.1764 0.061 Uiso 1 1 calc R U . . .
C10 C 0.23587(18) 0.19558(10) 0.16167(5) 0.0440(4) Uani 1 1 d . . . . .
H10A H 0.1701 0.1519 0.1561 0.053 Uiso 1 1 calc R U . . .
H10B H 0.1904 0.2437 0.1740 0.053 Uiso 1 1 calc R U . . .
C11 C 0.20931(15) 0.24093(11) 0.09370(6) 0.0453(4) Uani 1 1 d . . . . .
H11A H 0.1717 0.2964 0.0991 0.054 Uiso 1 1 calc R U . . .
H11B H 0.1367 0.2002 0.0931 0.054 Uiso 1 1 calc R U . . .
C12 C 0.27990(16) 0.24104(11) 0.05385(5) 0.0429(4) Uani 1 1 d . . . . .
H12A H 0.3204 0.1862 0.0490 0.051 Uiso 1 1 calc R U . . .
H12B H 0.2172 0.2522 0.0315 0.051 Uiso 1 1 calc R U . . .
C13 C 0.35996(14) 0.50864(8) 0.11829(4) 0.0296(3) Uani 1 1 d . . . . .
C14 C 0.48935(13) 0.53996(8) 0.12115(4) 0.0268(3) Uani 1 1 d . . . . .
C15 C 0.53061(14) 0.53336(8) 0.16212(4) 0.0285(3) Uani 1 1 d . . . . .
C16 C 0.42716(15) 0.49785(8) 0.18445(4) 0.0321(3) Uani 1 1 d . . . . .
C17 C 0.32189(14) 0.48243(8) 0.15753(5) 0.0327(3) Uani 1 1 d . . . . .
C18 C 0.27520(16) 0.50576(10) 0.08082(5) 0.0421(4) Uani 1 1 d . . . . .
H18A H 0.2018 0.5445 0.0839 0.063 Uiso 1 1 calc R U . . .
H18B H 0.2411 0.4495 0.0771 0.063 Uiso 1 1 calc R U . . .
H18C H 0.3275 0.5214 0.0570 0.063 Uiso 1 1 calc R U . . .
C19 C 0.56897(15) 0.57888(9) 0.08764(5) 0.0347(3) Uani 1 1 d . . . . .
H19A H 0.5606 0.6393 0.0891 0.052 Uiso 1 1 calc R U . . .
H19B H 0.5367 0.5594 0.0612 0.052 Uiso 1 1 calc R U . . .
H19C H 0.6614 0.5633 0.0908 0.052 Uiso 1 1 calc R U . . .
C20 C 0.66149(16) 0.56203(10) 0.17813(5) 0.0411(4) Uani 1 1 d . . . . .
H20A H 0.6676 0.6224 0.1757 0.062 Uiso 1 1 calc R U . . .
H20B H 0.7320 0.5362 0.1623 0.062 Uiso 1 1 calc R U . . .
H20C H 0.6700 0.5461 0.2068 0.062 Uiso 1 1 calc R U . . .
C21 C 0.4249(2) 0.48017(11) 0.22941(5) 0.0506(5) Uani 1 1 d . . . . .
H21A H 0.3594 0.5156 0.2426 0.076 Uiso 1 1 calc R U . . .
H21B H 0.5117 0.4915 0.2410 0.076 Uiso 1 1 calc R U . . .
H21C H 0.4022 0.4219 0.2339 0.076 Uiso 1 1 calc R U . . .
C22 C 0.19184(17) 0.44475(10) 0.16866(6) 0.0509(5) Uani 1 1 d . . . . .
H22A H 0.1668 0.4628 0.1960 0.076 Uiso 1 1 calc R U . . .
H22B H 0.1990 0.3842 0.1681 0.076 Uiso 1 1 calc R U . . .
H22C H 0.1250 0.4627 0.1491 0.076 Uiso 1 1 calc R U . . .
N1 N 0.58941(18) 0.15699(12) 0.09498(6) 0.0678(5) Uani 1 1 d . . . . .
H1C H 0.5051 0.1632 0.1036 0.102 Uiso 1 1 calc R U . . .
H1D H 0.6309 0.2069 0.0957 0.102 Uiso 1 1 calc R U . . .
H1E H 0.6320 0.1207 0.1116 0.102 Uiso 1 1 calc R U . . .
N2 N 0.5903(2) 0.08695(14) 0.00329(7) 0.0719(5) Uani 1 1 d . . . . .
H2C H 0.596(3) 0.0995(19) 0.0319(10) 0.108 Uiso 1 1 d . U . . .
H2D H 0.669(3) 0.094(2) -0.0092(9) 0.108 Uiso 1 1 d . U . . .
H2E H 0.571(3) 0.038(2) 0.0023(10) 0.108 Uiso 1 1 d . U . . .


_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
K O4 2.8872(11) . ?
K O3 2.9132(12) . ?
K O1 2.9647(10) . ?
K O6 2.9768(11) . ?
K C17 2.9941(14) . ?
K C13 3.0278(13) . ?
K O5 3.0673(11) . ?
K C16 3.0744(14) . ?
K O2 3.1146(11) . ?
K C14 3.1194(13) . ?
K C15 3.1531(13) . ?
K N1 3.4263(18) . ?
O1 C12 1.4201(19) . ?
O1 C1 1.4201(18) . ?
O2 C2 1.413(2) . ?
O2 C3 1.424(2) . ?
O3 C4 1.422(2) . ?
O3 C5 1.422(2) . ?
O4 C7 1.419(2) . ?
O4 C6 1.421(2) . ?
O5 C8 1.424(2) . ?
O5 C9 1.426(2) . ?
O6 C11 1.416(2) . ?
O6 C10 1.4346(18) . ?
C1 C2 1.493(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.481(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.489(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.489(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.483(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.495(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C17 1.412(2) . ?
C13 C14 1.4154(19) . ?
C13 C18 1.505(2) . ?
C14 C15 1.4149(19) . ?
C14 C19 1.5057(19) . ?
C15 C16 1.407(2) . ?
C15 C20 1.507(2) . ?
C16 C17 1.413(2) . ?
C16 C21 1.506(2) . ?
C17 C22 1.504(2) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
N1 N2 3.220(3) . ?
N1 H1C 0.9100 . ?
N1 H1D 0.9100 . ?
N1 H1E 0.9100 . ?
N2 H2C 0.96(3) . ?
N2 H2D 0.91(3) . ?
N2 H2E 0.82(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
O4 K O3 58.08(4) . . ?
O4 K O1 139.33(3) . . ?
O3 K O1 109.61(3) . . ?
O4 K O6 103.90(3) . . ?
O3 K O6 136.55(3) . . ?
O1 K O6 56.00(3) . . ?
O4 K C17 120.21(4) . . ?
O3 K C17 129.02(4) . . ?
O1 K C17 97.89(4) . . ?
O6 K C17 94.43(3) . . ?
O4 K C13 138.68(4) . . ?
O3 K C13 115.60(4) . . ?
O1 K C13 81.95(3) . . ?
O6 K C13 103.29(3) . . ?
C17 K C13 27.12(4) . . ?
O4 K O5 56.68(4) . . ?
O3 K O5 113.54(4) . . ?
O1 K O5 110.70(3) . . ?
O6 K O5 55.17(3) . . ?
C17 K O5 94.26(4) . . ?
C13 K O5 120.48(4) . . ?
O4 K C16 96.16(4) . . ?
O3 K C16 107.62(4) . . ?
O1 K C16 123.81(4) . . ?
O6 K C16 113.81(4) . . ?
C17 K C16 26.88(4) . . ?
C13 K C16 44.01(4) . . ?
O5 K C16 90.48(3) . . ?
O4 K O2 105.25(3) . . ?
O3 K O2 54.93(3) . . ?
O1 K O2 55.21(3) . . ?
O6 K O2 102.40(3) . . ?
C17 K O2 125.66(4) . . ?
C13 K O2 98.56(4) . . ?
O5 K O2 137.37(3) . . ?
C16 K O2 131.71(3) . . ?
O4 K C14 120.04(4) . . ?
O3 K C14 89.85(3) . . ?
O1 K C14 96.76(3) . . ?
O6 K C14 129.75(3) . . ?
C17 K C14 43.77(4) . . ?
C13 K C14 26.57(4) . . ?
O5 K C14 133.46(3) . . ?
C16 K C14 43.17(4) . . ?
O2 K C14 89.14(3) . . ?
O4 K C15 96.57(3) . . ?
O3 K C15 85.66(4) . . ?
O1 K C15 122.37(3) . . ?
O6 K C15 137.67(3) . . ?
C17 K C15 43.56(4) . . ?
C13 K C15 43.50(4) . . ?
O5 K C15 112.57(3) . . ?
C16 K C15 26.07(4) . . ?
O2 K C15 107.39(3) . . ?
C14 K C15 26.07(4) . . ?
O4 K N1 74.26(4) . . ?
O3 K N1 75.75(4) . . ?
O1 K N1 65.07(4) . . ?
O6 K N1 60.92(4) . . ?
C17 K N1 154.82(4) . . ?
C13 K N1 146.92(4) . . ?
O5 K N1 76.33(4) . . ?
C16 K N1 166.48(4) . . ?
O2 K N1 61.17(4) . . ?
C14 K N1 150.18(4) . . ?
C15 K N1 161.40(4) . . ?
C12 O1 C1 111.23(12) . . ?
C12 O1 K 120.05(8) . . ?
C1 O1 K 121.52(9) . . ?
C2 O2 C3 112.04(13) . . ?
C2 O2 K 103.86(9) . . ?
C3 O2 K 107.19(9) . . ?
C4 O3 C5 111.66(14) . . ?
C4 O3 K 124.04(10) . . ?
C5 O3 K 117.69(11) . . ?
C7 O4 C6 113.39(15) . . ?
C7 O4 K 110.72(10) . . ?
C6 O4 K 107.08(10) . . ?
C8 O5 C9 112.06(14) . . ?
C8 O5 K 114.74(11) . . ?
C9 O5 K 117.22(9) . . ?
C11 O6 C10 112.27(12) . . ?
C11 O6 K 110.79(9) . . ?
C10 O6 K 116.32(9) . . ?
O1 C1 C2 108.71(13) . . ?
O1 C1 H1A 109.9 . . ?
C2 C1 H1A 109.9 . . ?
O1 C1 H1B 109.9 . . ?
C2 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
O2 C2 C1 108.65(13) . . ?
O2 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
O2 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.3 . . ?
O2 C3 C4 108.56(14) . . ?
O2 C3 H3A 110.0 . . ?
C4 C3 H3A 110.0 . . ?
O2 C3 H3B 110.0 . . ?
C4 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
O3 C4 C3 108.75(14) . . ?
O3 C4 H4A 109.9 . . ?
C3 C4 H4A 109.9 . . ?
O3 C4 H4B 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
O3 C5 C6 108.48(16) . . ?
O3 C5 H5A 110.0 . . ?
C6 C5 H5A 110.0 . . ?
O3 C5 H5B 110.0 . . ?
C6 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
O4 C6 C5 109.12(15) . . ?
O4 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
O4 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
O4 C7 C8 108.43(15) . . ?
O4 C7 H7A 110.0 . . ?
C8 C7 H7A 110.0 . . ?
O4 C7 H7B 110.0 . . ?
C8 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
O5 C8 C7 108.83(15) . . ?
O5 C8 H8A 109.9 . . ?
C7 C8 H8A 109.9 . . ?
O5 C8 H8B 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
O5 C9 C10 109.37(13) . . ?
O5 C9 H9A 109.8 . . ?
C10 C9 H9A 109.8 . . ?
O5 C9 H9B 109.8 . . ?
C10 C9 H9B 109.8 . . ?
H9A C9 H9B 108.2 . . ?
O6 C10 C9 107.55(13) . . ?
O6 C10 H10A 110.2 . . ?
C9 C10 H10A 110.2 . . ?
O6 C10 H10B 110.2 . . ?
C9 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
O6 C11 C12 108.47(13) . . ?
O6 C11 H11A 110.0 . . ?
C12 C11 H11A 110.0 . . ?
O6 C11 H11B 110.0 . . ?
C12 C11 H11B 110.0 . . ?
H11A C11 H11B 108.4 . . ?
O1 C12 C11 109.20(13) . . ?
O1 C12 H12A 109.8 . . ?
C11 C12 H12A 109.8 . . ?
O1 C12 H12B 109.8 . . ?
C11 C12 H12B 109.8 . . ?
H12A C12 H12B 108.3 . . ?
C17 C13 C14 107.60(12) . . ?
C17 C13 C18 125.50(13) . . ?
C14 C13 C18 126.87(14) . . ?
C17 C13 K 75.11(8) . . ?
C14 C13 K 80.33(8) . . ?
C18 C13 K 112.47(9) . . ?
C15 C14 C13 108.25(12) . . ?
C15 C14 C19 124.60(13) . . ?
C13 C14 C19 127.05(13) . . ?
C15 C14 K 78.30(7) . . ?
C13 C14 K 73.10(7) . . ?
C19 C14 K 117.79(9) . . ?
C16 C15 C14 107.75(12) . . ?
C16 C15 C20 127.32(13) . . ?
C14 C15 C20 124.92(13) . . ?
C16 C15 K 73.84(8) . . ?
C14 C15 K 75.64(7) . . ?
C20 C15 K 117.75(9) . . ?
C15 C16 C17 108.30(12) . . ?
C15 C16 C21 126.94(15) . . ?
C17 C16 C21 124.75(15) . . ?
C15 C16 K 80.09(8) . . ?
C17 C16 K 73.39(8) . . ?
C21 C16 K 113.85(9) . . ?
C13 C17 C16 108.11(12) . . ?
C13 C17 C22 125.86(15) . . ?
C16 C17 C22 126.03(15) . . ?
C13 C17 K 77.77(8) . . ?
C16 C17 K 79.73(8) . . ?
C22 C17 K 109.45(9) . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C15 C20 H20A 109.5 . . ?
C15 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C15 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N2 N1 K 130.65(7) . . ?
N2 N1 H1C 109.5 . . ?
K N1 H1C 63.9 . . ?
N2 N1 H1D 109.5 . . ?
K N1 H1D 46.0 . . ?
H1C N1 H1D 109.5 . . ?
N2 N1 H1E 109.5 . . ?
K N1 H1E 118.9 . . ?
H1C N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
N1 N2 H2D 112(2) . . ?
H2C N2 H2D 111(3) . . ?
N1 N2 H2E 112(2) . . ?
H2C N2 H2E 105(3) . . ?
H2D N2 H2E 108(3) . . ?

_refine_diff_density_max         0.354
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.037


#============================================================================== 
# END of CIF 
#============================================================================== 
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ammonia'
