# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_cmpd1

_audit_creation_method           SHELXL-97

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H48 F30 K N3 O8 U'
_chemical_formula_weight         1786.14

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'
F F 0.0171 0.0103 '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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c     '
_symmetry_Int_Tables_number      14

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

_cell_length_a                   20.0305(11)
_cell_length_b                   16.0601(8)
_cell_length_c                   20.8994(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.967(3)
_cell_angle_gamma                90.00
_cell_volume                     6673.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    143(1)
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03

_exptl_crystal_density_diffrn    1.778
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3496
_exptl_absorpt_coefficient_mu    2.633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_absorpt_correction_T_min  0.5677
_exptl_absorpt_correction_T_max  0.7456
_diffrn_ambient_temperature      143(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            199405
_diffrn_reflns_av_R_equivalents  0.1622
_diffrn_reflns_av_sigmaI/netI    0.1079
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         27.60
_reflns_number_total             15410
_reflns_number_gt                8222
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0279P)²+39.2539P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         15410
_refine_ls_number_parameters     947
_refine_ls_number_restraints     297
_refine_ls_R_factor_all          0.1525
_refine_ls_R_factor_gt           0.0558
_refine_ls_wR_factor_ref         0.1381
_refine_ls_wR_factor_gt          0.0982
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.299846(15) 0.192890(19) 0.635605(13) 0.03393(9) Uani 1 1 d . . .
F1 F 0.3344(2) 0.3063(3) 0.4998(2) 0.0463(11) Uani 1 1 d . . .
F2 F 0.2940(3) 0.4471(3) 0.4383(2) 0.0624(14) Uani 1 1 d . . .
F3 F 0.1621(3) 0.4730(3) 0.3963(2) 0.0682(16) Uani 1 1 d . . .
F4 F 0.0703(3) 0.3553(4) 0.4194(2) 0.0668(15) Uani 1 1 d . . .
F5 F 0.1094(2) 0.2135(3) 0.4819(2) 0.0539(13) Uani 1 1 d . . .
F6 F 0.2791(2) 0.1532(3) 0.4044(2) 0.0514(12) Uani 1 1 d . . .
F7 F 0.2500(3) 0.0120(3) 0.3395(2) 0.0662(15) Uani 1 1 d . . .
F8 F 0.1862(3) -0.1145(3) 0.3944(3) 0.0741(16) Uani 1 1 d . . .
F9 F 0.1517(3) -0.0955(3) 0.5154(3) 0.0777(17) Uani 1 1 d . . .
F10 F 0.1739(3) 0.0485(3) 0.5780(2) 0.0575(13) Uani 1 1 d . . .
F11 F 0.4388(2) 0.3248(3) 0.7044(2) 0.0494(12) Uani 1 1 d . . .
F12 F 0.5051(3) 0.4634(3) 0.6792(3) 0.0648(15) Uani 1 1 d . . .
F13 F 0.5548(3) 0.4823(3) 0.5647(3) 0.0692(15) Uani 1 1 d . . .
F14 F 0.5372(3) 0.3592(3) 0.4750(2) 0.0613(14) Uani 1 1 d . . .
F15 F 0.4697(2) 0.2204(3) 0.4988(2) 0.0478(12) Uani 1 1 d . . .
F16 F 0.5386(2) 0.1652(3) 0.6871(2) 0.0506(12) Uani 1 1 d . . .
F17 F 0.6082(3) 0.0245(4) 0.6782(2) 0.0738(17) Uani 1 1 d . . .
F18 F 0.5582(3) -0.0998(3) 0.5980(3) 0.0788(18) Uani 1 1 d . . .
F19 F 0.4377(3) -0.0786(3) 0.5237(2) 0.0592(14) Uani 1 1 d . . .
F20 F 0.3709(2) 0.0649(3) 0.5269(2) 0.0451(11) Uani 1 1 d . . .
F21 F 0.1658(2) 0.3345(3) 0.60046(18) 0.0399(11) Uani 1 1 d . . .
F22 F 0.1196(2) 0.4802(3) 0.6403(2) 0.0526(12) Uani 1 1 d . . .
F23 F 0.0925(3) 0.5000(3) 0.7630(2) 0.0660(15) Uani 1 1 d . . .
F24 F 0.1112(2) 0.3689(3) 0.8471(2) 0.0555(13) Uani 1 1 d . . .
F25 F 0.1649(2) 0.2267(3) 0.8109(2) 0.0509(12) Uani 1 1 d . . .
F26 F 0.0667(2) 0.1835(3) 0.6303(2) 0.0580(13) Uani 1 1 d . . .
F27 F -0.0081(3) 0.0478(4) 0.6460(3) 0.0818(18) Uani 1 1 d . . .
F28 F 0.0438(3) -0.0794(3) 0.7246(3) 0.0876(19) Uani 1 1 d . . .
F29 F 0.1728(3) -0.0689(3) 0.7820(3) 0.0771(17) Uani 1 1 d . . .
F30 F 0.2470(3) 0.0672(3) 0.7677(2) 0.0598(14) Uani 1 1 d . . .
O1 O 0.3001(2) 0.3032(3) 0.6345(2) 0.0351(11) Uani 1 1 d . . .
O2 O 0.3033(3) 0.0829(3) 0.6398(2) 0.0422(13) Uani 1 1 d . . .
N1 N 0.2435(3) 0.1833(4) 0.5290(2) 0.0282(14) Uani 1 1 d . . .
N2 N 0.4137(3) 0.1940(4) 0.6129(3) 0.0319(13) Uani 1 1 d . . .
N3 N 0.1991(3) 0.2004(4) 0.6860(3) 0.0337(14) Uani 1 1 d . . .
C1 C 0.2239(4) 0.2555(5) 0.4930(3) 0.0333(18) Uani 1 1 d . . .
C2 C 0.2682(4) 0.3166(5) 0.4810(3) 0.0379(19) Uani 1 1 d . . .
C3 C 0.2483(5) 0.3898(5) 0.4497(4) 0.046(2) Uani 1 1 d . . .
C4 C 0.1814(5) 0.4015(6) 0.4280(4) 0.047(2) Uani 1 1 d . . .
C5 C 0.1362(5) 0.3430(6) 0.4393(4) 0.048(2) Uani 1 1 d . . .
C6 C 0.1557(4) 0.2698(5) 0.4706(3) 0.0382(19) Uani 1 1 d . . .
C7 C 0.2278(4) 0.1081(5) 0.4947(3) 0.0346(19) Uani 1 1 d . . .
C8 C 0.2466(4) 0.0930(5) 0.4327(4) 0.0395(19) Uani 1 1 d . . .
C9 C 0.2325(4) 0.0211(6) 0.3993(4) 0.045(2) Uani 1 1 d . . .
C10 C 0.2003(5) -0.0428(6) 0.4269(5) 0.055(2) Uani 1 1 d . . .
C11 C 0.1840(4) -0.0335(5) 0.4880(5) 0.051(2) Uani 1 1 d . . .
C12 C 0.1964(4) 0.0410(6) 0.5196(4) 0.045(2) Uani 1 1 d . . .
C13 C 0.4499(4) 0.2670(5) 0.6022(4) 0.0336(18) Uani 1 1 d . . .
C14 C 0.4612(4) 0.3327(5) 0.6461(4) 0.042(2) Uani 1 1 d . . .
C15 C 0.4947(4) 0.4028(5) 0.6344(4) 0.047(2) Uani 1 1 d . . .
C16 C 0.5214(4) 0.4129(5) 0.5767(5) 0.049(2) Uani 1 1 d . . .
C17 C 0.5114(4) 0.3500(6) 0.5317(4) 0.044(2) Uani 1 1 d . . .
C18 C 0.4779(4) 0.2794(5) 0.5449(4) 0.0391(19) Uani 1 1 d . . .
C19 C 0.4513(4) 0.1210(5) 0.6076(3) 0.0324(18) Uani 1 1 d . . .
C20 C 0.5130(4) 0.1064(5) 0.6450(3) 0.0388(19) Uani 1 1 d . . .
C21 C 0.5484(4) 0.0340(6) 0.6420(4) 0.048(2) Uani 1 1 d . . .
C22 C 0.5235(5) -0.0286(5) 0.6011(4) 0.050(2) Uani 1 1 d . . .
C23 C 0.4627(4) -0.0170(5) 0.5638(4) 0.042(2) Uani 1 1 d . . .
C24 C 0.4285(4) 0.0560(5) 0.5668(3) 0.0351(18) Uani 1 1 d . . .
C25 C 0.1704(4) 0.2746(5) 0.7048(4) 0.0341(18) Uani 1 1 d . . .
C26 C 0.1561(4) 0.3425(5) 0.6639(3) 0.0361(19) Uani 1 1 d . . .
C27 C 0.1315(4) 0.4166(5) 0.6819(4) 0.0395(19) Uani 1 1 d . . .
C28 C 0.1158(4) 0.4264(5) 0.7443(4) 0.044(2) Uani 1 1 d . . .
C29 C 0.1265(4) 0.3606(6) 0.7866(4) 0.041(2) Uani 1 1 d . . .
C30 C 0.1531(4) 0.2892(5) 0.7671(3) 0.038(2) Uani 1 1 d . . .
C31 C 0.1607(4) 0.1292(5) 0.6986(4) 0.0374(19) Uani 1 1 d . . .
C32 C 0.0942(4) 0.1232(5) 0.6696(4) 0.044(2) Uani 1 1 d . . .
C33 C 0.0549(5) 0.0542(6) 0.6771(5) 0.058(3) Uani 1 1 d . . .
C34 C 0.0806(5) -0.0106(7) 0.7154(5) 0.063(3) Uani 1 1 d . . .
C35 C 0.1459(6) -0.0056(6) 0.7441(4) 0.055(3) Uani 1 1 d . . .
C36 C 0.1839(5) 0.0629(6) 0.7362(4) 0.051(2) Uani 1 1 d . . .
O3 O 0.3539(3) 0.1921(4) 0.7471(2) 0.0417(13) Uani 1 1 d DU B .
C37 C 0.3400(4) 0.2492(6) 0.7982(4) 0.054(2) Uani 1 1 d DU . .
H37a H 0.2984 0.2348 0.8148 0.072 Uiso 0.55 1 calc PR A 1
H37b H 0.3373 0.3063 0.7828 0.072 Uiso 0.55 1 calc PR A 1
H37a' H 0.2921 0.2525 0.8010 0.072 Uiso 0.45 1 calc PR A 2
H37b' H 0.3567 0.3046 0.7905 0.072 Uiso 0.45 1 calc PR A 2
C38 C 0.3993(8) 0.2374(11) 0.8486(8) 0.049(5) Uani 0.55 1 d PDU B 1
H38a H 0.3885 0.2534 0.8909 0.065 Uiso 0.55 1 calc PR B 1
H38b H 0.4378 0.2693 0.8385 0.065 Uiso 0.55 1 calc PR B 1
C39 C 0.4123(11) 0.1447(11) 0.8450(7) 0.055(5) Uani 0.55 1 d PDU B 1
H39a H 0.3806 0.1131 0.8669 0.074 Uiso 0.55 1 calc PR B 1
H39b H 0.4577 0.1308 0.8633 0.074 Uiso 0.55 1 calc PR B 1
C38' C 0.3765(11) 0.2129(14) 0.8585(9) 0.053(5) Uani 0.45 1 d PDU B 2
H38a' H 0.3483 0.1737 0.8781 0.071 Uiso 0.45 1 calc PR B 2
H38b' H 0.3912 0.2561 0.8894 0.071 Uiso 0.45 1 calc PR B 2
C39' C 0.4369(11) 0.1687(13) 0.8346(9) 0.053(6) Uani 0.45 1 d PDU B 2
H39a' H 0.4716 0.2078 0.8259 0.071 Uiso 0.45 1 calc PR B 2
H39b' H 0.4561 0.1268 0.8649 0.071 Uiso 0.45 1 calc PR B 2
C40 C 0.4017(5) 0.1298(6) 0.7729(3) 0.055(2) Uani 1 1 d DU . .
H40a H 0.4437 0.1359 0.7546 0.073 Uiso 0.55 1 calc PR B 1
H40b H 0.3841 0.0743 0.7634 0.073 Uiso 0.55 1 calc PR B 1
H40a' H 0.4336 0.1178 0.7428 0.073 Uiso 0.45 1 calc PR B 2
H40b' H 0.3790 0.0787 0.7822 0.073 Uiso 0.45 1 calc PR B 2
K1 K 0.20081(10) 0.74181(14) 0.57343(9) 0.0551(5) Uani 1 1 d . . .
O4 O 0.1246(4) 0.7511(5) 0.6691(3) 0.087(2) Uani 1 1 d U . .
O5 O 0.3086(4) 0.8121(5) 0.6345(4) 0.100(3) Uani 1 1 d U . .
O6 O 0.2667(4) 0.7300(5) 0.4692(3) 0.085(2) Uani 1 1 d U . .
O7 O 0.1007(3) 0.6761(5) 0.4966(3) 0.080(2) Uani 1 1 d U . .
O8 O 0.2547(4) 0.5985(4) 0.6211(3) 0.076(2) Uani 1 1 d U . .
C41 C 0.0546(6) 0.7389(9) 0.6524(5) 0.095(4) Uani 1 1 d U . .
H41a H 0.0463 0.7018 0.6157 0.127 Uiso 1 1 calc R . .
H41b H 0.0324 0.7916 0.6415 0.127 Uiso 1 1 calc R . .
C42 C 0.0290(5) 0.7017(9) 0.7096(5) 0.092(4) Uani 1 1 d U . .
H42a H -0.0119 0.7296 0.7183 0.122 Uiso 1 1 calc R . .
H42b H 0.0192 0.6430 0.7022 0.122 Uiso 1 1 calc R . .
C43 C 0.0823(6) 0.7122(8) 0.7644(5) 0.087(3) Uani 1 1 d U . .
H43a H 0.0759 0.7628 0.7883 0.116 Uiso 1 1 calc R . .
H43b H 0.0843 0.6649 0.7935 0.116 Uiso 1 1 calc R . .
C44 C 0.1427(6) 0.7172(9) 0.7314(6) 0.094(4) Uani 1 1 d U . .
H44a H 0.1761 0.7523 0.7557 0.125 Uiso 1 1 calc R . .
H44b H 0.1618 0.6621 0.7279 0.125 Uiso 1 1 calc R . .
C45 C 0.3750(6) 0.7799(8) 0.6470(7) 0.113(5) Uani 1 1 d U . .
H45a H 0.3739 0.7202 0.6540 0.151 Uiso 1 1 calc R . .
H45b H 0.4000 0.7909 0.6110 0.151 Uiso 1 1 calc R . .
C46 C 0.4050(7) 0.8212(8) 0.7033(6) 0.109(4) Uani 1 1 d U . .
H46a H 0.4524 0.8313 0.7006 0.145 Uiso 1 1 calc R . .
H46b H 0.4010 0.7877 0.7412 0.145 Uiso 1 1 calc R . .
C47 C 0.3689(6) 0.9004(7) 0.7068(6) 0.090(4) Uani 1 1 d U . .
H47a H 0.3946 0.9464 0.6923 0.120 Uiso 1 1 calc R . .
H47b H 0.3594 0.9116 0.7504 0.120 Uiso 1 1 calc R . .
C48 C 0.3062(6) 0.8872(8) 0.6630(7) 0.114(5) Uani 1 1 d U . .
H48a H 0.2679 0.8897 0.6872 0.152 Uiso 1 1 calc R . .
H48b H 0.3012 0.9306 0.6305 0.152 Uiso 1 1 calc R . .
C49 C 0.2455(8) 0.6816(9) 0.4132(6) 0.113(4) Uani 1 1 d U . .
H49a H 0.2364 0.6247 0.4252 0.151 Uiso 1 1 calc R . .
H49b H 0.2048 0.7049 0.3901 0.151 Uiso 1 1 calc R . .
C50 C 0.2988(7) 0.6835(11) 0.3738(6) 0.120(5) Uani 1 1 d U . .
H50a H 0.2812 0.6812 0.3285 0.159 Uiso 1 1 calc R . .
H50b H 0.3291 0.6369 0.3837 0.159 Uiso 1 1 calc R . .
C51 C 0.3340(6) 0.7635(10) 0.3894(6) 0.107(4) Uani 1 1 d U . .
H51a H 0.3143 0.8079 0.3618 0.142 Uiso 1 1 calc R . .
H51b H 0.3814 0.7590 0.3844 0.142 Uiso 1 1 calc R . .
C52 C 0.3243(6) 0.7794(8) 0.4593(6) 0.091(3) Uani 1 1 d U . .
H52a H 0.3635 0.7621 0.4880 0.121 Uiso 1 1 calc R . .
H52b H 0.3159 0.8380 0.4665 0.121 Uiso 1 1 calc R . .
C53 C 0.0769(5) 0.5929(6) 0.4992(5) 0.068(3) Uani 1 1 d U . .
H53a H 0.0585 0.5831 0.5394 0.090 Uiso 1 1 calc R . .
H53b H 0.1131 0.5536 0.4960 0.090 Uiso 1 1 calc R . .
C54 C 0.0234(6) 0.5836(7) 0.4430(5) 0.086(3) Uani 1 1 d U . .
H54a H 0.0277 0.5305 0.4218 0.115 Uiso 1 1 calc R . .
H54b H -0.0209 0.5868 0.4571 0.115 Uiso 1 1 calc R . .
C55 C 0.0331(7) 0.6498(8) 0.4009(6) 0.104(4) Uani 1 1 d U . .
H55a H -0.0090 0.6665 0.3763 0.138 Uiso 1 1 calc R . .
H55b H 0.0649 0.6349 0.3713 0.138 Uiso 1 1 calc R . .
C56 C 0.0600(7) 0.7159(7) 0.4456(5) 0.095(4) Uani 1 1 d U . .
H56a H 0.0865 0.7551 0.4239 0.127 Uiso 1 1 calc R . .
H56b H 0.0236 0.7459 0.4620 0.127 Uiso 1 1 calc R . .
C57 C 0.2854(6) 0.5692(8) 0.6814(5) 0.082(3) Uani 1 1 d U . .
H57a H 0.2534 0.5373 0.7027 0.109 Uiso 1 1 calc R . .
H57b H 0.3012 0.6155 0.7089 0.109 Uiso 1 1 calc R . .
C58 C 0.3438(7) 0.5147(9) 0.6682(5) 0.103(4) Uani 1 1 d U . .
H58a H 0.3862 0.5398 0.6857 0.137 Uiso 1 1 calc R . .
H58b H 0.3404 0.4601 0.6874 0.137 Uiso 1 1 calc R . .
C59 C 0.3392(6) 0.5082(7) 0.5971(5) 0.076(3) Uani 1 1 d U . .
H59a H 0.3728 0.5428 0.5803 0.101 Uiso 1 1 calc R . .
H59b H 0.3449 0.4510 0.5837 0.101 Uiso 1 1 calc R . .
C60 C 0.2709(6) 0.5384(8) 0.5755(5) 0.088(4) Uani 1 1 d U . .
H60a H 0.2691 0.5634 0.5331 0.117 Uiso 1 1 calc R . .
H60b H 0.2391 0.4927 0.5733 0.117 Uiso 1 1 calc R . .


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
U1 O2 1.770(6) . ?
U1 O1 1.772(5) . ?
U1 N1 2.378(5) . ?
U1 N2 2.386(6) . ?
U1 N3 2.390(6) . ?
U1 O3 2.446(4) . ?
F1 C2 1.347(8) . ?
F2 C3 1.340(9) . ?
F3 C4 1.358(9) . ?
F4 C5 1.350(9) . ?
F5 C6 1.338(9) . ?
F6 C8 1.343(9) . ?
F7 C9 1.347(9) . ?
F8 C10 1.349(10) . ?
F9 C11 1.353(10) . ?
F9 K1 2.995(6) 1_545 ?
F10 C12 1.356(9) . ?
F11 C14 1.354(9) . ?
F12 C15 1.348(9) . ?
F13 C16 1.338(9) . ?
F14 C17 1.358(9) . ?
F15 C18 1.347(8) . ?
F16 C20 1.349(9) . ?
F17 C21 1.345(9) . ?
F18 C22 1.345(9) . ?
F19 C23 1.352(9) . ?
F20 C24 1.346(8) . ?
F21 C26 1.370(8) . ?
F22 C27 1.344(9) . ?
F23 C28 1.347(9) . ?
F24 C29 1.344(8) . ?
F25 C30 1.360(8) . ?
F26 C32 1.344(9) . ?
F27 C33 1.352(11) . ?
F28 C34 1.355(10) . ?
F29 C35 1.359(10) . ?
F30 C36 1.355(10) . ?
N1 C1 1.411(9) . ?
N1 C7 1.420(9) . ?
N2 C19 1.405(9) . ?
N2 C13 1.410(10) . ?
N3 C25 1.400(9) . ?
N3 C31 1.420(9) . ?
C1 C2 1.367(11) . ?
C1 C6 1.407(11) . ?
C2 C3 1.380(11) . ?
C3 C4 1.374(12) . ?
C4 C5 1.346(12) . ?
C5 C6 1.378(12) . ?
C7 C12 1.381(11) . ?
C7 C8 1.413(10) . ?
C8 C9 1.362(11) . ?
C9 C10 1.375(12) . ?
C10 C11 1.365(13) . ?
C11 C12 1.375(12) . ?
C13 C18 1.397(11) . ?
C13 C14 1.399(11) . ?
C14 C15 1.349(11) . ?
C15 C16 1.386(12) . ?
C16 C17 1.377(12) . ?
C17 C18 1.363(11) . ?
C19 C24 1.389(10) . ?
C19 C20 1.401(10) . ?
C20 C21 1.367(11) . ?
C21 C22 1.373(12) . ?
C22 C23 1.377(12) . ?
C23 C24 1.364(11) . ?
C25 C26 1.393(10) . ?
C25 C30 1.407(10) . ?
C26 C27 1.359(11) . ?
C27 C28 1.387(11) . ?
C28 C29 1.377(11) . ?
C29 C30 1.348(11) . ?
C31 C36 1.372(11) . ?
C31 C32 1.399(11) . ?
C32 C33 1.378(12) . ?
C33 C34 1.375(13) . ?
C34 C35 1.375(13) . ?
C35 C36 1.358(13) . ?
O3 C40 1.443(8) . ?
O3 C37 1.460(8) . ?
C37 C38' 1.496(16) . ?
C37 C38 1.500(15) . ?
C38 C39 1.514(16) . ?
C39 C40 1.516(15) . ?
C38' C39' 1.537(18) . ?
C39' C40 1.527(16) . ?
K1 O5 2.626(7) . ?
K1 O7 2.632(6) . ?
K1 O4 2.663(7) . ?
K1 O8 2.682(7) . ?
K1 O6 2.688(7) . ?
K1 F9 2.995(6) 1_565 ?
O4 C44 1.416(13) . ?
O4 C41 1.418(12) . ?
O5 C48 1.350(13) . ?
O5 C45 1.421(13) . ?
O6 C49 1.426(13) . ?
O6 C52 1.436(13) . ?
O7 C56 1.413(11) . ?
O7 C53 1.422(11) . ?
O8 C57 1.413(11) . ?
O8 C60 1.421(11) . ?
C41 C42 1.481(15) . ?
C42 C43 1.479(15) . ?
C43 C44 1.466(15) . ?
C45 C46 1.420(15) . ?
C46 C47 1.470(15) . ?
C47 C48 1.476(14) . ?
C49 C50 1.425(16) . ?
C50 C51 1.483(18) . ?
C51 C52 1.519(16) . ?
C53 C54 1.498(13) . ?
C54 C55 1.408(14) . ?
C55 C56 1.474(15) . ?
C57 C58 1.513(15) . ?
C58 C59 1.481(14) . ?
C59 C60 1.471(14) . ?

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 U1 O1 177.0(2) . . ?
O2 U1 N1 89.6(2) . . ?
O1 U1 N1 93.1(2) . . ?
O2 U1 N2 89.1(2) . . ?
O1 U1 N2 89.2(2) . . ?
N1 U1 N2 99.82(18) . . ?
O2 U1 N3 93.3(2) . . ?
O1 U1 N3 87.7(2) . . ?
N1 U1 N3 94.97(19) . . ?
N2 U1 N3 165.02(18) . . ?
O2 U1 O3 86.4(2) . . ?
O1 U1 O3 90.9(2) . . ?
N1 U1 O3 175.5(2) . . ?
N2 U1 O3 82.32(17) . . ?
N3 U1 O3 83.10(18) . . ?
C11 F9 K1 131.6(5) . 1_545 ?
C1 N1 C7 113.5(5) . . ?
C1 N1 U1 121.1(4) . . ?
C7 N1 U1 125.3(4) . . ?
C19 N2 C13 113.1(5) . . ?
C19 N2 U1 122.9(5) . . ?
C13 N2 U1 124.0(5) . . ?
C25 N3 C31 112.5(6) . . ?
C25 N3 U1 124.3(5) . . ?
C31 N3 U1 123.1(5) . . ?
C2 C1 C6 116.5(7) . . ?
C2 C1 N1 122.8(7) . . ?
C6 C1 N1 120.6(7) . . ?
F1 C2 C1 119.7(7) . . ?
F1 C2 C3 117.5(7) . . ?
C1 C2 C3 122.8(8) . . ?
F2 C3 C4 120.4(8) . . ?
F2 C3 C2 120.3(8) . . ?
C4 C3 C2 119.2(8) . . ?
C5 C4 F3 121.3(9) . . ?
C5 C4 C3 119.7(8) . . ?
F3 C4 C3 119.0(9) . . ?
C4 C5 F4 119.8(8) . . ?
C4 C5 C6 121.4(8) . . ?
F4 C5 C6 118.8(9) . . ?
F5 C6 C5 119.8(8) . . ?
F5 C6 C1 119.8(7) . . ?
C5 C6 C1 120.4(8) . . ?
C12 C7 C8 113.3(7) . . ?
C12 C7 N1 123.8(7) . . ?
C8 C7 N1 122.7(7) . . ?
F6 C8 C9 117.7(7) . . ?
F6 C8 C7 118.6(7) . . ?
C9 C8 C7 123.7(8) . . ?
F7 C9 C8 120.5(8) . . ?
F7 C9 C10 119.8(8) . . ?
C8 C9 C10 119.8(8) . . ?
F8 C10 C11 120.3(9) . . ?
F8 C10 C9 120.4(9) . . ?
C11 C10 C9 119.2(8) . . ?
F9 C11 C10 119.8(8) . . ?
F9 C11 C12 120.4(8) . . ?
C10 C11 C12 119.7(8) . . ?
F10 C12 C11 116.7(8) . . ?
F10 C12 C7 119.1(7) . . ?
C11 C12 C7 124.2(8) . . ?
C18 C13 C14 113.9(7) . . ?
C18 C13 N2 121.4(7) . . ?
C14 C13 N2 124.7(7) . . ?
C15 C14 F11 118.0(8) . . ?
C15 C14 C13 123.7(8) . . ?
F11 C14 C13 118.3(7) . . ?
C14 C15 F12 120.9(8) . . ?
C14 C15 C16 120.6(8) . . ?
F12 C15 C16 118.5(8) . . ?
F13 C16 C17 121.2(8) . . ?
F13 C16 C15 120.9(9) . . ?
C17 C16 C15 117.9(8) . . ?
F14 C17 C18 121.1(8) . . ?
F14 C17 C16 118.4(8) . . ?
C18 C17 C16 120.5(8) . . ?
F15 C18 C17 117.4(7) . . ?
F15 C18 C13 119.1(7) . . ?
C17 C18 C13 123.4(8) . . ?
C24 C19 C20 114.8(7) . . ?
C24 C19 N2 122.5(7) . . ?
C20 C19 N2 122.7(7) . . ?
F16 C20 C21 117.8(7) . . ?
F16 C20 C19 119.2(7) . . ?
C21 C20 C19 122.9(8) . . ?
F17 C21 C20 120.1(8) . . ?
F17 C21 C22 119.8(8) . . ?
C20 C21 C22 120.0(8) . . ?
F18 C22 C21 120.1(8) . . ?
F18 C22 C23 121.0(8) . . ?
C21 C22 C23 118.9(8) . . ?
F19 C23 C24 120.5(8) . . ?
F19 C23 C22 119.2(7) . . ?
C24 C23 C22 120.3(8) . . ?
F20 C24 C23 117.4(7) . . ?
F20 C24 C19 119.6(7) . . ?
C23 C24 C19 123.0(7) . . ?
C26 C25 N3 123.7(6) . . ?
C26 C25 C30 112.5(7) . . ?
N3 C25 C30 123.8(7) . . ?
C27 C26 F21 116.7(7) . . ?
C27 C26 C25 124.7(7) . . ?
F21 C26 C25 118.5(7) . . ?
F22 C27 C26 121.9(7) . . ?
F22 C27 C28 118.7(7) . . ?
C26 C27 C28 119.4(8) . . ?
F23 C28 C29 121.3(7) . . ?
F23 C28 C27 119.9(8) . . ?
C29 C28 C27 118.7(8) . . ?
F24 C29 C30 120.8(8) . . ?
F24 C29 C28 119.4(7) . . ?
C30 C29 C28 119.7(7) . . ?
C29 C30 F25 117.8(6) . . ?
C29 C30 C25 124.8(7) . . ?
F25 C30 C25 117.3(7) . . ?
C36 C31 C32 115.6(8) . . ?
C36 C31 N3 125.3(8) . . ?
C32 C31 N3 119.0(7) . . ?
F26 C32 C33 116.8(8) . . ?
F26 C32 C31 120.8(7) . . ?
C33 C32 C31 122.3(8) . . ?
F27 C33 C34 118.9(9) . . ?
F27 C33 C32 121.3(9) . . ?
C34 C33 C32 119.7(9) . . ?
F28 C34 C35 119.5(10) . . ?
F28 C34 C33 121.9(10) . . ?
C35 C34 C33 118.6(9) . . ?
C36 C35 F29 119.2(10) . . ?
C36 C35 C34 120.8(9) . . ?
F29 C35 C34 119.9(9) . . ?
F30 C36 C35 119.1(8) . . ?
F30 C36 C31 118.0(8) . . ?
C35 C36 C31 122.9(9) . . ?
C40 O3 C37 109.7(5) . . ?
C40 O3 U1 123.8(4) . . ?
C37 O3 U1 126.3(4) . . ?
O3 C37 C38' 104.7(10) . . ?
O3 C37 C38 103.3(9) . . ?
C38' C37 C38 25.3(10) . . ?
C37 C38 C39 102.5(13) . . ?
C38 C39 C40 101.5(13) . . ?
C37 C38' C39' 103.3(15) . . ?
C40 C39' C38' 99.3(15) . . ?
O3 C40 C39 105.6(9) . . ?
O3 C40 C39' 104.5(10) . . ?
C39 C40 C39' 25.9(10) . . ?
O5 K1 O7 171.5(3) . . ?
O5 K1 O4 97.1(3) . . ?
O7 K1 O4 91.0(2) . . ?
O5 K1 O8 85.3(2) . . ?
O7 K1 O8 97.2(2) . . ?
O4 K1 O8 90.6(3) . . ?
O5 K1 O6 88.2(3) . . ?
O7 K1 O6 83.7(2) . . ?
O4 K1 O6 174.5(2) . . ?
O8 K1 O6 91.4(2) . . ?
O5 K1 F9 91.8(2) . 1_565 ?
O7 K1 F9 85.1(2) . 1_565 ?
O4 K1 F9 93.7(2) . 1_565 ?
O8 K1 F9 175.1(2) . 1_565 ?
O6 K1 F9 84.5(2) . 1_565 ?
C44 O4 C41 108.0(9) . . ?
C44 O4 K1 124.2(7) . . ?
C41 O4 K1 116.6(6) . . ?
C48 O5 C45 109.0(8) . . ?
C48 O5 K1 121.9(7) . . ?
C45 O5 K1 129.0(7) . . ?
C49 O6 C52 110.4(9) . . ?
C49 O6 K1 125.2(7) . . ?
C52 O6 K1 124.0(7) . . ?
C56 O7 C53 106.7(7) . . ?
C56 O7 K1 127.3(6) . . ?
C53 O7 K1 126.0(5) . . ?
C57 O8 C60 105.1(8) . . ?
C57 O8 K1 136.8(6) . . ?
C60 O8 K1 116.6(6) . . ?
O4 C41 C42 106.6(9) . . ?
C43 C42 C41 106.9(10) . . ?
C44 C43 C42 101.5(9) . . ?
O4 C44 C43 108.7(10) . . ?
C46 C45 O5 106.0(10) . . ?
C45 C46 C47 106.5(10) . . ?
C46 C47 C48 103.4(9) . . ?
O5 C48 C47 109.3(10) . . ?
C50 C49 O6 107.0(11) . . ?
C49 C50 C51 105.2(12) . . ?
C50 C51 C52 104.1(11) . . ?
O6 C52 C51 104.1(10) . . ?
O7 C53 C54 106.0(8) . . ?
C55 C54 C53 106.0(9) . . ?
C54 C55 C56 102.3(9) . . ?
O7 C56 C55 106.6(9) . . ?
O8 C57 C58 107.0(8) . . ?
C59 C58 C57 105.6(9) . . ?
C60 C59 C58 103.0(9) . . ?
O8 C60 C59 107.4(9) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.60
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         4.084
_refine_diff_density_min         -1.376
_refine_diff_density_rms         0.153
_database_code_depnum_ccdc_archive 'CCDC 965029'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_cmpd2

_audit_creation_method           SHELXL-97

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C80 H84 F20 K2 N4 O10 U'
_chemical_formula_weight         1957.74

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'
F F 0.0171 0.0103 '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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c      '
_symmetry_Int_Tables_number      15

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

_cell_length_a                   34.3892(16)
_cell_length_b                   15.7020(7)
_cell_length_c                   21.1110(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 121.564(2)
_cell_angle_gamma                90.00
_cell_volume                     9713.0(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    143(1)
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08

_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3928
_exptl_absorpt_coefficient_mu    1.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_absorpt_correction_T_min  0.5637
_exptl_absorpt_correction_T_max  0.7456
_diffrn_ambient_temperature      143(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            84416
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         27.57
_reflns_number_total             11131
_reflns_number_gt                6713
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1124P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11131
_refine_ls_number_parameters     583
_refine_ls_number_restraints     217
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0566
_refine_ls_wR_factor_ref         0.1736
_refine_ls_wR_factor_gt          0.1546
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_restrained_S_all      0.980
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_special_details          
;
The data were corrected for the presence of disordered solvent using the
program SQUEEZE.
;

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.2500 0.7500 0.5000 0.04084(12) Uani 1 2 d S . .
K1 K 0.32585(5) 0.80472(9) 0.84168(8) 0.0698(4) Uani 1 1 d . . .
F1 F 0.35919(12) 0.8622(2) 0.6655(2) 0.0676(10) Uani 1 1 d . . .
F2 F 0.44219(15) 0.8675(3) 0.6838(3) 0.0944(14) Uani 1 1 d . . .
F3 F 0.48214(14) 0.7252(4) 0.6727(3) 0.1025(16) Uani 1 1 d . . .
F4 F 0.43758(14) 0.5724(3) 0.6464(3) 0.1042(15) Uani 1 1 d . . .
F5 F 0.35452(12) 0.5660(2) 0.6269(2) 0.0711(10) Uani 1 1 d . . .
F6 F 0.22873(18) 0.9905(3) 0.4704(3) 0.0891(13) Uani 1 1 d . . .
F7 F 0.28620(19) 1.1179(3) 0.5420(3) 0.1273(19) Uani 1 1 d . . .
F8 F 0.33918(18) 1.1172(3) 0.6930(4) 0.132(2) Uani 1 1 d . . .
F9 F 0.32773(16) 0.9904(3) 0.7691(2) 0.1129(17) Uani 1 1 d . C .
F10 F 0.26877(15) 0.8663(3) 0.6988(2) 0.0773(12) Uani 1 1 d . C .
O1 O 0.21216(12) 0.6698(2) 0.4936(2) 0.0453(9) Uani 1 1 d . . .
O2 O 0.2474(2) 0.8380(4) 0.8332(4) 0.114(2) Uani 1 1 d . C .
O5 O 0.4095(2) 0.8106(5) 0.8640(5) 0.132(3) Uani 1 1 d . C .
N1 N 0.30795(15) 0.7126(3) 0.6278(2) 0.0455(10) Uani 1 1 d . . .
N2 N 0.21741(15) 0.8524(3) 0.5452(2) 0.0447(10) Uani 1 1 d . . .
C1 C 0.3522(2) 0.7144(4) 0.6421(3) 0.0507(14) Uani 1 1 d . . .
C2 C 0.3772(2) 0.7907(4) 0.6581(3) 0.0535(15) Uani 1 1 d . . .
C3 C 0.4201(2) 0.7943(5) 0.6684(4) 0.0644(17) Uani 1 1 d . . .
C4 C 0.4409(2) 0.7227(7) 0.6640(4) 0.072(2) Uani 1 1 d . . .
C5 C 0.4184(3) 0.6458(6) 0.6506(4) 0.073(2) Uani 1 1 d . . .
C6 C 0.3749(2) 0.6414(4) 0.6399(3) 0.0548(15) Uani 1 1 d . . .
C7 C 0.30252(19) 0.6757(3) 0.6826(3) 0.0460(13) Uani 1 1 d . . .
C8 C 0.2583(2) 0.6723(4) 0.6728(3) 0.0578(16) Uani 1 1 d . . .
H8 H 0.2334 0.6942 0.6296 0.069 Uiso 1 1 calc R . .
C9 C 0.2515(3) 0.6374(4) 0.7260(4) 0.0661(18) Uani 1 1 d . . .
H9 H 0.2221 0.6347 0.7176 0.079 Uiso 1 1 calc R . .
C10 C 0.2880(3) 0.6059(4) 0.7922(4) 0.0701(19) Uani 1 1 d . . .
H10 H 0.2836 0.5830 0.8287 0.084 Uiso 1 1 calc R . .
C11 C 0.3307(3) 0.6099(4) 0.8019(3) 0.073(2) Uani 1 1 d . . .
H11 H 0.3554 0.5891 0.8458 0.088 Uiso 1 1 calc R . .
C12 C 0.3380(2) 0.6437(3) 0.7486(3) 0.0533(14) Uani 1 1 d . . .
H12 H 0.3675 0.6450 0.7574 0.064 Uiso 1 1 calc R . .
C13 C 0.24666(18) 0.9225(3) 0.5805(3) 0.0468(13) Uani 1 1 d . . .
C14 C 0.2528(2) 0.9895(4) 0.5434(4) 0.0630(17) Uani 1 1 d . . .
C15 C 0.2818(3) 1.0546(4) 0.5807(5) 0.079(2) Uani 1 1 d . . .
C16 C 0.3086(3) 1.0540(5) 0.6565(6) 0.089(3) Uani 1 1 d . C .
C17 C 0.3033(2) 0.9919(5) 0.6952(4) 0.074(2) Uani 1 1 d . . .
C18 C 0.2727(2) 0.9282(4) 0.6572(3) 0.0548(15) Uani 1 1 d . C .
C19 C 0.17699(18) 0.8536(3) 0.5449(3) 0.0454(12) Uani 1 1 d . . .
C20 C 0.1591(2) 0.9284(4) 0.5546(4) 0.0673(19) Uani 1 1 d . . .
H20 H 0.1745 0.9798 0.5626 0.081 Uiso 1 1 calc R . .
C21 C 0.1173(3) 0.9256(6) 0.5520(5) 0.094(3) Uani 1 1 d . . .
H21 H 0.1061 0.9762 0.5594 0.112 Uiso 1 1 calc R . .
C22 C 0.0928(2) 0.8554(5) 0.5398(4) 0.078(2) Uani 1 1 d . . .
H22 H 0.0650 0.8566 0.5374 0.094 Uiso 1 1 calc R . .
C23 C 0.1105(2) 0.7797(5) 0.5306(4) 0.0649(17) Uani 1 1 d . . .
H23 H 0.0945 0.7292 0.5236 0.078 Uiso 1 1 calc R . .
C24 C 0.1505(2) 0.7778(4) 0.5319(4) 0.0532(14) Uani 1 1 d . . .
H24 H 0.1609 0.7264 0.5241 0.064 Uiso 1 1 calc R . .
C25 C 0.2210(5) 0.9164(6) 0.8070(7) 0.166(5) Uani 1 1 d . . .
H25a H 0.2295 0.9479 0.7765 0.199 Uiso 1 1 calc R C .
H25b H 0.2274 0.9518 0.8491 0.199 Uiso 1 1 calc R . .
C26 C 0.1721(4) 0.8960(8) 0.7632(9) 0.170(7) Uani 1 1 d . C .
H26a H 0.1559 0.9191 0.7857 0.204 Uiso 1 1 calc R . .
H26b H 0.1580 0.9162 0.7124 0.204 Uiso 1 1 calc R . .
C27 C 0.1740(4) 0.8086(7) 0.7668(7) 0.160(5) Uani 1 1 d . . .
H27a H 0.1722 0.7855 0.7227 0.192 Uiso 1 1 calc R C .
H27b H 0.1486 0.7864 0.7696 0.192 Uiso 1 1 calc R . .
C28 C 0.2187(4) 0.7834(8) 0.8354(8) 0.139(5) Uani 1 1 d . C .
H28a H 0.2177 0.7905 0.8801 0.167 Uiso 1 1 calc R . .
H28b H 0.2267 0.7250 0.8323 0.167 Uiso 1 1 calc R . .
O3 O 0.3575(2) 0.7165(5) 0.9716(3) 0.1065(18) Uani 1 1 d DU B .
C29 C 0.3275(3) 0.6874(7) 0.9941(5) 0.124(3) Uani 1 1 d DU . .
H29a H 0.3089 0.6407 0.9627 0.165 Uiso 1 1 calc R C .
H29b H 0.3075 0.7330 0.9909 0.165 Uiso 1 1 calc R . .
C30 C 0.3569(4) 0.6585(11) 1.0721(6) 0.178(5) Uani 1 1 d DU B .
H30a H 0.3556 0.6997 1.1052 0.236 Uiso 0.65 1 calc PR A 1
H30b H 0.3457 0.6045 1.0786 0.236 Uiso 0.65 1 calc PR A 1
H30a' H 0.3705 0.6036 1.0743 0.236 Uiso 0.35 1 calc PR A 2
H30b' H 0.3395 0.6539 1.0962 0.236 Uiso 0.35 1 calc PR A 2
C31 C 0.4049(5) 0.6484(15) 1.0921(8) 0.147(6) Uani 0.65 1 d PDU B 1
H31a H 0.4148 0.5895 1.1028 0.196 Uiso 0.65 1 calc PR B 1
H31b H 0.4255 0.6837 1.1342 0.196 Uiso 0.65 1 calc PR B 1
C32 C 0.4012(4) 0.6788(12) 1.0213(7) 0.120(4) Uani 0.65 1 d PDU B 1
H32a H 0.4250 0.7202 1.0333 0.159 Uiso 0.65 1 calc PR B 1
H32b H 0.4058 0.6310 0.9968 0.159 Uiso 0.65 1 calc PR B 1
C31' C 0.3933(13) 0.727(2) 1.1089(15) 0.170(11) Uani 0.35 1 d PDU B 2
H31a' H 0.4231 0.7028 1.1439 0.226 Uiso 0.35 1 calc PR B 2
H31b' H 0.3854 0.7696 1.1333 0.226 Uiso 0.35 1 calc PR B 2
C32' C 0.3905(13) 0.7601(19) 1.0392(10) 0.153(11) Uani 0.35 1 d PDU B 2
H32a' H 0.3828 0.8201 1.0340 0.204 Uiso 0.35 1 calc PR B 2
H32b' H 0.4204 0.7551 1.0451 0.204 Uiso 0.35 1 calc PR B 2
O4 O 0.3555(3) 0.9415(5) 0.9314(4) 0.139(2) Uani 1 1 d DU C .
C33 C 0.3971(7) 0.9241(15) 1.0019(9) 0.205(12) Uani 0.50 1 d PDU C 1
H33a H 0.4235 0.9395 0.9990 0.246 Uiso 0.50 1 calc PR C 1
H33b H 0.3991 0.8638 1.0133 0.246 Uiso 0.50 1 calc PR C 1
C34 C 0.3966(12) 0.9755(13) 1.0622(12) 0.160(8) Uani 0.50 1 d PDU C 1
H34a H 0.3781 0.9493 1.0791 0.192 Uiso 0.50 1 calc PR C 1
H34b H 0.4271 0.9866 1.1042 0.192 Uiso 0.50 1 calc PR C 1
C35 C 0.3745(10) 1.0538(14) 1.0156(11) 0.137(8) Uani 0.50 1 d PDU C 1
H35a H 0.3977 1.0914 1.0179 0.164 Uiso 0.50 1 calc PR C 1
H35b H 0.3580 1.0845 1.0341 0.164 Uiso 0.50 1 calc PR C 1
C36 C 0.3420(8) 1.0258(10) 0.9359(11) 0.138(7) Uani 0.50 1 d PDU C 1
H36a H 0.3107 1.0265 0.9244 0.166 Uiso 0.50 1 calc PR C 1
H36b H 0.3444 1.0631 0.9015 0.166 Uiso 0.50 1 calc PR C 1
C33' C 0.3805(7) 1.0201(11) 0.9455(10) 0.125(6) Uani 0.50 1 d PDU C 2
H33a' H 0.3600 1.0673 0.9197 0.150 Uiso 0.50 1 calc PR C 2
H33b' H 0.4025 1.0160 0.9301 0.150 Uiso 0.50 1 calc PR C 2
C34' C 0.4041(6) 1.0308(16) 1.0287(10) 0.105(5) Uani 0.50 1 d PDU C 2
H34a' H 0.4130 1.0894 1.0439 0.126 Uiso 0.50 1 calc PR C 2
H34b' H 0.4304 0.9938 1.0552 0.126 Uiso 0.50 1 calc PR C 2
C35' C 0.3650(5) 1.0032(15) 1.0383(10) 0.087(4) Uani 0.50 1 d PDU C 2
H35a' H 0.3748 0.9591 1.0758 0.105 Uiso 0.50 1 calc PR C 2
H35b' H 0.3532 1.0510 1.0522 0.105 Uiso 0.50 1 calc PR C 2
C36' C 0.3295(5) 0.9694(16) 0.9620(11) 0.131(6) Uani 0.50 1 d PDU C 2
H36a' H 0.3126 0.9226 0.9661 0.157 Uiso 0.50 1 calc PR C 2
H36b' H 0.3083 1.0139 0.9317 0.157 Uiso 0.50 1 calc PR C 2
C37 C 0.4309(4) 0.8795(9) 0.8578(7) 0.158(5) Uani 1 1 d . . .
H37a H 0.4175 0.9314 0.8630 0.190 Uiso 1 1 calc R C .
H37b H 0.4281 0.8801 0.8097 0.190 Uiso 1 1 calc R . .
C38 C 0.4813(4) 0.8730(10) 0.9203(8) 0.178(6) Uani 1 1 d . C .
H38a H 0.5014 0.8809 0.9014 0.214 Uiso 1 1 calc R . .
H38b H 0.4890 0.9144 0.9593 0.214 Uiso 1 1 calc R . .
C39 C 0.4839(4) 0.7828(11) 0.9477(9) 0.156(5) Uani 1 1 d . . .
H39a H 0.5101 0.7526 0.9532 0.187 Uiso 1 1 calc R C .
H39b H 0.4850 0.7819 0.9945 0.187 Uiso 1 1 calc R . .
C40 C 0.4410(4) 0.7475(6) 0.8872(10) 0.131(5) Uani 1 1 d . C .
H40a H 0.4446 0.7288 0.8468 0.157 Uiso 1 1 calc R . .
H40b H 0.4316 0.6991 0.9047 0.157 Uiso 1 1 calc R . .


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
U1 O1 1.765(3) . ?
U1 O1 1.765(3) 7_566 ?
U1 N2 2.424(4) . ?
U1 N2 2.424(4) 7_566 ?
U1 N1 2.442(4) 7_566 ?
U1 N1 2.442(4) . ?
K1 O2 2.660(6) . ?
K1 O5 2.663(7) . ?
K1 O4 2.686(6) . ?
K1 O3 2.739(6) . ?
K1 F10 2.773(4) . ?
K1 F9 3.310(6) . ?
K1 C33 3.504(16) . ?
F1 C2 1.331(7) . ?
F2 C3 1.323(8) . ?
F3 C4 1.332(8) . ?
F4 C5 1.355(9) . ?
F5 C6 1.330(7) . ?
F6 C14 1.314(8) . ?
F7 C15 1.345(8) . ?
F8 C16 1.354(8) . ?
F9 C17 1.330(8) . ?
F10 C18 1.364(7) . ?
O2 C28 1.327(12) . ?
O2 C25 1.457(10) . ?
O5 C37 1.352(13) . ?
O5 C40 1.356(11) . ?
N1 C1 1.388(7) . ?
N1 C7 1.392(6) . ?
N2 C19 1.386(7) . ?
N2 C13 1.412(7) . ?
C1 C6 1.400(9) . ?
C1 C2 1.408(10) . ?
C2 C3 1.373(9) . ?
C3 C4 1.363(12) . ?
C4 C5 1.382(12) . ?
C5 C6 1.391(10) . ?
C7 C12 1.380(7) . ?
C7 C8 1.426(8) . ?
C8 C9 1.374(9) . ?
C9 C10 1.392(9) . ?
C10 C11 1.373(9) . ?
C11 C12 1.383(8) . ?
C13 C18 1.383(8) . ?
C13 C14 1.392(8) . ?
C14 C15 1.356(10) . ?
C15 C16 1.366(11) . ?
C16 C17 1.345(11) . ?
C17 C18 1.366(9) . ?
C19 C20 1.390(8) . ?
C19 C24 1.434(8) . ?
C20 C21 1.413(10) . ?
C21 C22 1.328(10) . ?
C22 C23 1.393(9) . ?
C23 C24 1.366(9) . ?
C25 C26 1.469(14) . ?
C26 C27 1.374(14) . ?
C27 C28 1.512(14) . ?
O3 C29 1.418(8) . ?
O3 C32 1.435(9) . ?
O3 C32' 1.448(10) . ?
C29 C30 1.483(8) . ?
C30 C31 1.482(9) . ?
C30 C31' 1.514(10) . ?
C31 C32 1.509(9) . ?
C31' C32' 1.519(10) . ?
O4 C36' 1.418(9) . ?
O4 C36 1.423(9) . ?
O4 C33' 1.443(9) . ?
O4 C33 1.452(10) . ?
C33 C34 1.515(10) . ?
C34 C35 1.509(10) . ?
C35 C36 1.518(10) . ?
C33' C34' 1.509(10) . ?
C34' C35' 1.522(9) . ?
C35' C36' 1.519(9) . ?
C37 C38 1.539(13) . ?
C38 C39 1.515(17) . ?
C39 C40 1.463(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O1 180.0(2) . 7_566 ?
O1 U1 N2 91.70(16) . . ?
O1 U1 N2 88.30(16) 7_566 . ?
O1 U1 N2 88.30(16) . 7_566 ?
O1 U1 N2 91.70(16) 7_566 7_566 ?
N2 U1 N2 180.000(1) . 7_566 ?
O1 U1 N1 86.81(16) . 7_566 ?
O1 U1 N1 93.19(16) 7_566 7_566 ?
N2 U1 N1 89.83(15) . 7_566 ?
N2 U1 N1 90.17(15) 7_566 7_566 ?
O1 U1 N1 93.19(16) . . ?
O1 U1 N1 86.81(16) 7_566 . ?
N2 U1 N1 90.17(15) . . ?
N2 U1 N1 89.83(15) 7_566 . ?
N1 U1 N1 180.000(1) 7_566 . ?
O2 K1 O5 165.7(2) . . ?
O2 K1 O4 83.5(2) . . ?
O5 K1 O4 82.6(2) . . ?
O2 K1 O3 91.4(2) . . ?
O5 K1 O3 90.8(2) . . ?
O4 K1 O3 83.8(2) . . ?
O2 K1 F10 75.10(17) . . ?
O5 K1 F10 105.4(2) . . ?
O4 K1 F10 106.2(2) . . ?
O3 K1 F10 161.77(19) . . ?
O2 K1 F9 93.47(17) . . ?
O5 K1 F9 76.7(2) . . ?
O4 K1 F9 61.98(19) . . ?
O3 K1 F9 144.60(18) . . ?
F10 K1 F9 50.47(12) . . ?
O2 K1 C33 97.6(5) . . ?
O5 K1 C33 70.4(5) . . ?
O4 K1 C33 22.6(3) . . ?
O3 K1 C33 66.0(5) . . ?
F10 K1 C33 127.1(4) . . ?
F9 K1 C33 78.6(5) . . ?
C17 F9 K1 113.9(4) . . ?
C18 F10 K1 134.2(4) . . ?
C28 O2 C25 103.4(9) . . ?
C28 O2 K1 128.2(6) . . ?
C25 O2 K1 126.9(7) . . ?
C37 O5 C40 104.5(9) . . ?
C37 O5 K1 127.0(7) . . ?
C40 O5 K1 128.5(6) . . ?
C1 N1 C7 115.9(5) . . ?
C1 N1 U1 113.8(3) . . ?
C7 N1 U1 129.2(4) . . ?
C19 N2 C13 115.4(4) . . ?
C19 N2 U1 132.5(3) . . ?
C13 N2 U1 112.1(3) . . ?
N1 C1 C6 122.8(6) . . ?
N1 C1 C2 122.1(6) . . ?
C6 C1 C2 115.1(6) . . ?
F1 C2 C3 118.3(7) . . ?
F1 C2 C1 118.9(6) . . ?
C3 C2 C1 122.8(7) . . ?
F2 C3 C4 118.6(7) . . ?
F2 C3 C2 120.4(7) . . ?
C4 C3 C2 121.0(8) . . ?
F3 C4 C3 121.8(9) . . ?
F3 C4 C5 119.8(8) . . ?
C3 C4 C5 118.4(7) . . ?
F4 C5 C4 121.1(7) . . ?
F4 C5 C6 117.8(8) . . ?
C4 C5 C6 121.1(7) . . ?
F5 C6 C5 118.8(6) . . ?
F5 C6 C1 119.6(6) . . ?
C5 C6 C1 121.6(7) . . ?
C12 C7 N1 123.9(5) . . ?
C12 C7 C8 116.5(5) . . ?
N1 C7 C8 119.5(5) . . ?
C9 C8 C7 121.4(6) . . ?
C8 C9 C10 120.8(7) . . ?
C11 C10 C9 117.8(6) . . ?
C10 C11 C12 122.2(6) . . ?
C7 C12 C11 121.3(6) . . ?
C18 C13 C14 114.4(6) . . ?
C18 C13 N2 121.0(5) . . ?
C14 C13 N2 124.6(5) . . ?
F6 C14 C15 119.5(6) . . ?
F6 C14 C13 118.8(6) . . ?
C15 C14 C13 121.7(7) . . ?
F7 C15 C14 119.1(8) . . ?
F7 C15 C16 119.7(8) . . ?
C14 C15 C16 121.1(7) . . ?
C17 C16 F8 119.9(9) . . ?
C17 C16 C15 119.5(7) . . ?
F8 C16 C15 120.6(9) . . ?
F9 C17 C16 121.4(8) . . ?
F9 C17 C18 119.7(8) . . ?
C16 C17 C18 118.9(7) . . ?
F10 C18 C17 116.7(6) . . ?
F10 C18 C13 119.1(5) . . ?
C17 C18 C13 124.2(7) . . ?
N2 C19 C20 121.9(5) . . ?
N2 C19 C24 121.6(5) . . ?
C20 C19 C24 116.4(5) . . ?
C19 C20 C21 119.2(7) . . ?
C22 C21 C20 124.2(7) . . ?
C21 C22 C23 117.3(7) . . ?
C24 C23 C22 121.6(7) . . ?
C23 C24 C19 121.2(6) . . ?
O2 C25 C26 109.6(10) . . ?
C27 C26 C25 100.3(10) . . ?
C26 C27 C28 108.0(10) . . ?
O2 C28 C27 101.6(9) . . ?
C29 O3 C32 106.8(8) . . ?
C29 O3 C32' 99.0(17) . . ?
C32 O3 C32' 59.6(17) . . ?
C29 O3 K1 121.4(5) . . ?
C32 O3 K1 131.0(6) . . ?
C32' O3 K1 116.3(12) . . ?
O3 C29 C30 106.1(8) . . ?
C31 C30 C29 111.1(9) . . ?
C31 C30 C31' 55.4(19) . . ?
C29 C30 C31' 104.7(14) . . ?
C30 C31 C32 100.4(10) . . ?
O3 C32 C31 111.6(10) . . ?
C30 C31' C32' 97.6(19) . . ?
O3 C32' C31' 114(2) . . ?
C36' O4 C36 51.4(13) . . ?
C36' O4 C33' 95.2(12) . . ?
C36 O4 C33' 50.9(12) . . ?
C36' O4 C33 96.3(14) . . ?
C36 O4 C33 106.7(12) . . ?
C33' O4 C33 77.8(14) . . ?
C36' O4 K1 118.1(9) . . ?
C36 O4 K1 140.8(10) . . ?
C33' O4 K1 142.6(8) . . ?
C33 O4 K1 112.3(9) . . ?
O4 C33 C34 108.8(16) . . ?
O4 C33 K1 45.2(6) . . ?
C34 C33 K1 141.8(18) . . ?
C35 C34 C33 96.3(16) . . ?
C34 C35 C36 108.2(18) . . ?
O4 C36 C35 105.5(14) . . ?
O4 C33' C34' 103.6(12) . . ?
C33' C34' C35' 98.6(13) . . ?
C36' C35' C34' 103.5(13) . . ?
O4 C36' C35' 104.1(11) . . ?
O5 C37 C38 106.8(11) . . ?
C39 C38 C37 101.7(10) . . ?
C40 C39 C38 101.1(12) . . ?
O5 C40 C39 106.6(10) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.57
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         2.723
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.125

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.003 1050 160 ' '
2 0.500 -0.500 0.291 1050 160 ' '
_database_code_depnum_ccdc_archive 'CCDC 965030'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_cmpd3

_audit_creation_method           SHELXL-97

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49 H44 F15 K N6 O6 U'
_chemical_formula_weight         1375.03

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'
F F 0.0171 0.0103 '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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21 '
_symmetry_Int_Tables_number      19

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

_cell_length_a                   16.6414(17)
_cell_length_b                   19.756(2)
_cell_length_c                   34.283(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11271.1(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    143(1)
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25

_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5392
_exptl_absorpt_coefficient_mu    3.054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_absorpt_correction_T_min  0.6375
_exptl_absorpt_correction_T_max  0.7456
_diffrn_ambient_temperature      143(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            186028
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         27.63
_reflns_number_total             25533
_reflns_number_gt                21932
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0725P)²+198.8134P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.070(8)
_refine_ls_number_reflns         25533
_refine_ls_number_parameters     1406
_refine_ls_number_restraints     1483
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0790
_refine_ls_wR_factor_ref         0.2029
_refine_ls_wR_factor_gt          0.1973
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.000
_refine_special_details          
;
The data were corrected for the presence of disordered solvent using the
program SQUEEZE.
;

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.33350(3) 0.54431(2) 0.145837(12) 0.03322(11) Uani 1 1 d U . .
O1 O 0.3227(6) 0.5256(4) 0.0955(2) 0.0339(17) Uani 1 1 d U . .
O2 O 0.3426(5) 0.5657(5) 0.1957(2) 0.0349(16) Uani 1 1 d U . .
N1 N 0.3936(6) 0.4227(5) 0.1463(3) 0.0351(18) Uani 1 1 d U . .
N2 N 0.4783(6) 0.5050(6) 0.1561(3) 0.038(2) Uani 1 1 d U . .
N3 N 0.2235(6) 0.4670(6) 0.1707(3) 0.041(2) Uani 1 1 d U . .
N4 N 0.1837(5) 0.5561(6) 0.1426(3) 0.0375(18) Uani 1 1 d U . .
N5 N 0.4278(6) 0.6334(6) 0.1185(3) 0.0367(19) Uani 1 1 d U . .
N6 N 0.3038(5) 0.6675(5) 0.1404(2) 0.0244(15) Uani 1 1 d U . .
C1 C 0.3627(6) 0.3581(6) 0.1419(3) 0.0290(18) Uani 1 1 d U . .
C2 C 0.3778(7) 0.3057(7) 0.1687(3) 0.035(2) Uani 1 1 d U . .
C3 C 0.3474(8) 0.2415(7) 0.1644(4) 0.043(2) Uani 1 1 d U . .
C4 C 0.2984(10) 0.2249(7) 0.1334(5) 0.052(3) Uani 1 1 d U . .
C5 C 0.2844(7) 0.2741(7) 0.1071(4) 0.042(2) Uani 1 1 d U . .
C6 C 0.3151(7) 0.3382(6) 0.1104(4) 0.036(2) Uani 1 1 d U . .
C7 C 0.4680(8) 0.4389(7) 0.1522(3) 0.036(2) Uani 1 1 d U . .
C8 C 0.5511(8) 0.5277(9) 0.1634(5) 0.055(4) Uani 1 1 d U . .
H8 H 0.5564 0.5741 0.1671 0.074 Uiso 1 1 calc R . .
C9 C 0.6191(9) 0.4905(9) 0.1660(5) 0.057(4) Uani 1 1 d U . .
H9 H 0.6687 0.5088 0.1727 0.076 Uiso 1 1 calc R . .
C10 C 0.6073(9) 0.4206(9) 0.1575(4) 0.053(3) Uani 1 1 d U . .
H10 H 0.6520 0.3926 0.1560 0.070 Uiso 1 1 calc R . .
C11 C 0.5330(7) 0.3929(8) 0.1515(3) 0.037(2) Uani 1 1 d U . .
H11 H 0.5257 0.3468 0.1472 0.050 Uiso 1 1 calc R . .
C12 C 0.2163(6) 0.4077(7) 0.1909(3) 0.034(2) Uani 1 1 d U . .
C13 C 0.2607(8) 0.3947(7) 0.2250(3) 0.036(2) Uani 1 1 d U . .
C14 C 0.2577(8) 0.3334(7) 0.2445(4) 0.041(2) Uani 1 1 d U . .
C15 C 0.2103(10) 0.2808(8) 0.2315(4) 0.053(3) Uani 1 1 d U . .
C16 C 0.1669(9) 0.2918(8) 0.1971(4) 0.048(3) Uani 1 1 d U . .
C17 C 0.1700(9) 0.3528(8) 0.1781(4) 0.046(3) Uani 1 1 d U . .
C18 C 0.1584(8) 0.5057(6) 0.1596(4) 0.037(2) Uani 1 1 d U . .
C19 C 0.1266(9) 0.6042(9) 0.1257(4) 0.053(3) Uani 1 1 d U . .
H19 H 0.1448 0.6403 0.1107 0.071 Uiso 1 1 calc R . .
C20 C 0.0486(10) 0.5957(10) 0.1319(5) 0.058(3) Uani 1 1 d U . .
H20 H 0.0104 0.6264 0.1229 0.077 Uiso 1 1 calc R . .
C21 C 0.0275(10) 0.5376(9) 0.1528(5) 0.057(3) Uani 1 1 d U . .
H21 H -0.0271 0.5308 0.1569 0.076 Uiso 1 1 calc R . .
C22 C 0.0764(8) 0.4912(8) 0.1675(5) 0.049(3) Uani 1 1 d U . .
H22 H 0.0589 0.4535 0.1813 0.065 Uiso 1 1 calc R . .
C23 C 0.4956(8) 0.6376(6) 0.0973(4) 0.037(2) Uani 1 1 d U . .
C24 C 0.5005(8) 0.6113(7) 0.0584(4) 0.040(3) Uani 1 1 d U . .
C25 C 0.5702(10) 0.6077(9) 0.0380(5) 0.053(3) Uani 1 1 d U . .
C26 C 0.6369(10) 0.6317(9) 0.0514(5) 0.061(3) Uani 1 1 d U . .
C27 C 0.6404(10) 0.6586(10) 0.0896(6) 0.064(4) Uani 1 1 d U . .
C28 C 0.5714(9) 0.6639(7) 0.1113(5) 0.050(3) Uani 1 1 d U . .
C29 C 0.3781(6) 0.6885(7) 0.1208(4) 0.035(2) Uani 1 1 d U . .
C30 C 0.2583(10) 0.7256(8) 0.1466(5) 0.056(3) Uani 1 1 d U . .
H30 H 0.2139 0.7203 0.1627 0.074 Uiso 1 1 calc R . .
C31 C 0.2692(10) 0.7872(8) 0.1326(6) 0.067(4) Uani 1 1 d U . .
H31 H 0.2316 0.8210 0.1373 0.089 Uiso 1 1 calc R . .
C32 C 0.3359(9) 0.8003(8) 0.1115(6) 0.062(4) Uani 1 1 d U . .
H32 H 0.3453 0.8443 0.1029 0.082 Uiso 1 1 calc R . .
C33 C 0.3894(9) 0.7512(7) 0.1025(6) 0.054(3) Uani 1 1 d U . .
H33 H 0.4313 0.7585 0.0850 0.071 Uiso 1 1 calc R . .
F1 F 0.4200(5) 0.3202(4) 0.2015(2) 0.0441(18) Uani 1 1 d U . .
F2 F 0.3605(6) 0.1952(5) 0.1930(3) 0.063(2) Uani 1 1 d U . .
F3 F 0.2694(6) 0.1633(4) 0.1315(3) 0.061(2) Uani 1 1 d U . .
F4 F 0.2367(6) 0.2583(5) 0.0758(3) 0.065(2) Uani 1 1 d U . .
F5 F 0.2965(5) 0.3827(4) 0.0823(2) 0.0475(18) Uani 1 1 d U . .
F6 F 0.3064(5) 0.4428(5) 0.2397(2) 0.0486(17) Uani 1 1 d U . .
F7 F 0.3033(6) 0.3252(5) 0.2766(2) 0.065(3) Uani 1 1 d U . .
F8 F 0.2083(7) 0.2235(5) 0.2506(3) 0.069(3) Uani 1 1 d U . .
F9 F 0.1210(6) 0.2399(5) 0.1841(3) 0.067(3) Uani 1 1 d U . .
F10 F 0.1328(8) 0.3563(5) 0.1457(3) 0.082(3) Uani 1 1 d U . .
F11 F 0.4330(6) 0.5871(6) 0.0428(2) 0.068(3) Uani 1 1 d U . .
F12 F 0.5697(7) 0.5802(6) 0.0014(3) 0.078(3) Uani 1 1 d U . .
F13 F 0.7068(6) 0.6280(7) 0.0308(4) 0.093(4) Uani 1 1 d U . .
F14 F 0.7083(7) 0.6842(8) 0.1046(5) 0.116(5) Uani 1 1 d U . .
F15 F 0.5667(7) 0.6925(5) 0.1456(3) 0.073(3) Uani 1 1 d U . .
K1 K 0.30021(19) 0.57167(17) 0.27190(8) 0.0456(7) Uani 1 1 d U . .
O3 O 0.3893(10) 0.6855(7) 0.2666(4) 0.084(3) Uani 1 1 d U . .
C34 C 0.4396(18) 0.7039(11) 0.2340(7) 0.093(6) Uani 1 1 d U . .
H34q H 0.4956 0.6959 0.2404 0.123 Uiso 1 1 calc R . .
H34b H 0.4259 0.6767 0.2114 0.123 Uiso 1 1 calc R . .
C35 C 0.427(2) 0.7746(15) 0.2256(9) 0.141(9) Uani 1 1 d DU . .
H35a H 0.4016 0.7808 0.2004 0.187 Uiso 1 1 calc R . .
H35b H 0.4770 0.7997 0.2263 0.187 Uiso 1 1 calc R . .
C36 C 0.371(2) 0.7956(16) 0.2587(9) 0.143(9) Uani 1 1 d DU . .
H36a H 0.3880 0.8390 0.2691 0.190 Uiso 1 1 calc R . .
H36b H 0.3167 0.8000 0.2491 0.190 Uiso 1 1 calc R . .
C37 C 0.374(2) 0.7449(12) 0.2890(8) 0.105(7) Uani 1 1 d U . .
H37a H 0.4174 0.7537 0.3073 0.139 Uiso 1 1 calc R . .
H37b H 0.3237 0.7419 0.3030 0.139 Uiso 1 1 calc R . .
O4 O 0.1738(9) 0.6591(9) 0.2593(4) 0.098(4) Uani 1 1 d DU . .
C38 C 0.1207(14) 0.6937(12) 0.2860(7) 0.110(6) Uani 1 1 d DU . .
H38a H 0.1460 0.7005 0.3112 0.146 Uiso 1 1 calc R . .
H38b H 0.1037 0.7371 0.2757 0.146 Uiso 1 1 calc R . .
C39 C 0.0512(16) 0.6445(15) 0.2887(8) 0.123(8) Uani 1 1 d DU . .
H39a H 0.0001 0.6682 0.2890 0.164 Uiso 1 1 calc R . .
H39b H 0.0553 0.6166 0.3119 0.164 Uiso 1 1 calc R . .
C40 C 0.060(2) 0.6024(16) 0.2521(8) 0.143(9) Uani 1 1 d DU . .
H40a H 0.0754 0.5564 0.2586 0.190 Uiso 1 1 calc R . .
H40b H 0.0100 0.6012 0.2377 0.190 Uiso 1 1 calc R . .
C41 C 0.1248(13) 0.6356(16) 0.2281(6) 0.121(7) Uani 1 1 d DU . .
H41a H 0.1040 0.6725 0.2124 0.161 Uiso 1 1 calc R . .
H41b H 0.1527 0.6035 0.2116 0.161 Uiso 1 1 calc R . .
O5 O 0.4489(6) 0.5178(7) 0.2871(3) 0.063(3) Uani 1 1 d U . .
C42 C 0.4780(10) 0.4523(13) 0.2839(7) 0.087(5) Uani 1 1 d U . .
H42a H 0.4778 0.4379 0.2569 0.116 Uiso 1 1 calc R . .
H42b H 0.4448 0.4214 0.2989 0.116 Uiso 1 1 calc R . .
C43 C 0.5610(13) 0.4526(16) 0.2994(9) 0.114(7) Uani 1 1 d U . .
H43a H 0.5621 0.4350 0.3258 0.152 Uiso 1 1 calc R . .
H43b H 0.5957 0.4249 0.2832 0.152 Uiso 1 1 calc R . .
C44 C 0.5868(14) 0.5215(14) 0.2988(11) 0.123(8) Uani 1 1 d U . .
H44a H 0.6367 0.5263 0.2844 0.163 Uiso 1 1 calc R . .
H44b H 0.5943 0.5387 0.3250 0.163 Uiso 1 1 calc R . .
C45 C 0.5174(10) 0.5586(13) 0.2779(6) 0.080(4) Uani 1 1 d U . .
H45a H 0.5110 0.6043 0.2878 0.106 Uiso 1 1 calc R . .
H45b H 0.5263 0.5605 0.2500 0.106 Uiso 1 1 calc R . .
O6 O 0.1980(9) 0.9554(8) 0.1094(4) 0.088(4) Uani 1 1 d U . .
C46 C 0.1948(13) 0.9522(13) 0.0683(6) 0.086(5) Uani 1 1 d U . .
H46a H 0.1401 0.9573 0.0589 0.115 Uiso 1 1 calc R . .
H46b H 0.2165 0.9097 0.0588 0.115 Uiso 1 1 calc R . .
C47 C 0.2448(15) 1.0093(15) 0.0565(8) 0.114(7) Uani 1 1 d U . .
H47a H 0.2651 1.0037 0.0302 0.152 Uiso 1 1 calc R . .
H47b H 0.2158 1.0518 0.0583 0.152 Uiso 1 1 calc R . .
C48 C 0.3114(14) 1.0054(14) 0.0863(8) 0.105(7) Uani 1 1 d U . .
H48A H 0.3491 0.9694 0.0805 0.139 Uiso 1 1 calc R . .
H48B H 0.3398 1.0480 0.0889 0.139 Uiso 1 1 calc R . .
C49 C 0.2629(12) 0.9907(11) 0.1196(7) 0.081(5) Uani 1 1 d U . .
H49A H 0.2942 0.9649 0.1383 0.108 Uiso 1 1 calc R . .
H49B H 0.2466 1.0326 0.1320 0.108 Uiso 1 1 calc R . .
U1' U 0.23118(3) 0.55927(2) 0.392999(11) 0.03069(11) Uani 1 1 d U . .
O1' O 0.2313(5) 0.5368(4) 0.44325(19) 0.0280(14) Uani 1 1 d U . .
O2' O 0.2327(5) 0.5838(4) 0.3429(2) 0.0302(15) Uani 1 1 d U . .
N1' N 0.2347(6) 0.4407(5) 0.3658(3) 0.0372(18) Uani 1 1 d U . .
N2' N 0.3485(6) 0.4733(5) 0.3940(3) 0.0365(18) Uani 1 1 d U . .
N3' N 0.0905(6) 0.5215(5) 0.3936(3) 0.0329(17) Uani 1 1 d U . .
N4' N 0.1018(6) 0.6299(6) 0.3922(3) 0.0378(18) Uani 1 1 d U . .
N5' N 0.2697(7) 0.6765(6) 0.4201(3) 0.0383(19) Uani 1 1 d U . .
N6' N 0.3650(6) 0.6206(6) 0.3896(3) 0.039(2) Uani 1 1 d U . .
C1' C 0.1841(8) 0.3960(7) 0.3458(4) 0.043(2) Uani 1 1 d U . .
C2' C 0.1633(9) 0.3313(8) 0.3584(5) 0.053(3) Uani 1 1 d U . .
C3' C 0.1137(11) 0.2875(10) 0.3392(7) 0.072(4) Uani 1 1 d U . .
C4' C 0.0811(10) 0.3070(11) 0.3046(6) 0.072(3) Uani 1 1 d U . .
C5' C 0.0951(10) 0.3694(11) 0.2928(5) 0.068(3) Uani 1 1 d U . .
C6' C 0.1491(7) 0.4161(8) 0.3104(4) 0.046(2) Uani 1 1 d U . .
C7' C 0.3082(7) 0.4232(7) 0.3753(3) 0.035(2) Uani 1 1 d U . .
C8' C 0.4189(7) 0.4640(9) 0.4081(4) 0.048(3) Uani 1 1 d U . .
H8' H 0.4398 0.4975 0.4243 0.063 Uiso 1 1 calc R . .
C9' C 0.4657(8) 0.4084(7) 0.4011(4) 0.042(3) Uani 1 1 d U . .
H9' H 0.5186 0.4043 0.4095 0.055 Uiso 1 1 calc R . .
C10' C 0.4226(9) 0.3554(8) 0.3784(4) 0.046(3) Uani 1 1 d U . .
H10' H 0.4497 0.3157 0.3721 0.061 Uiso 1 1 calc R . .
C11' C 0.3496(8) 0.3623(8) 0.3673(4) 0.046(3) Uani 1 1 d U . .
H11' H 0.3240 0.3275 0.3539 0.061 Uiso 1 1 calc R . .
C12' C 0.0405(5) 0.4576(7) 0.3968(4) 0.037(2) Uani 1 1 d U . .
C13' C 0.0530(7) 0.4151(7) 0.4286(4) 0.039(2) Uani 1 1 d U . .
C14' C 0.0184(9) 0.3524(8) 0.4311(5) 0.050(3) Uani 1 1 d U . .
C15' C -0.0318(8) 0.3325(8) 0.4013(5) 0.051(3) Uani 1 1 d U . .
C16' C -0.0446(8) 0.3748(9) 0.3689(5) 0.053(3) Uani 1 1 d U . .
C17' C -0.0068(7) 0.4347(8) 0.3667(4) 0.042(2) Uani 1 1 d U . .
C18' C 0.0460(7) 0.5780(6) 0.3916(3) 0.034(2) Uani 1 1 d U . .
C19' C 0.0731(8) 0.6932(8) 0.3916(4) 0.047(3) Uani 1 1 d U . .
H19' H 0.1097 0.7286 0.3933 0.063 Uiso 1 1 calc R . .
C20' C -0.0066(9) 0.7093(8) 0.3886(5) 0.053(3) Uani 1 1 d U . .
H20' H -0.0238 0.7539 0.3865 0.070 Uiso 1 1 calc R . .
C21' C -0.0597(8) 0.6562(9) 0.3891(4) 0.050(3) Uani 1 1 d U . .
H21' H -0.1146 0.6653 0.3883 0.066 Uiso 1 1 calc R . .
C22' C -0.0350(8) 0.5919(8) 0.3905(4) 0.044(3) Uani 1 1 d U . .
H22' H -0.0722 0.5568 0.3908 0.059 Uiso 1 1 calc R . .
C23' C 0.2387(8) 0.7308(7) 0.4406(4) 0.040(2) Uani 1 1 d U . .
C24' C 0.1948(10) 0.7197(8) 0.4755(4) 0.053(3) Uani 1 1 d U . .
C25' C 0.1617(13) 0.7703(10) 0.4950(5) 0.067(4) Uani 1 1 d U . .
C26' C 0.1609(12) 0.8353(9) 0.4816(6) 0.073(3) Uani 1 1 d U . .
C27' C 0.2046(11) 0.8491(9) 0.4480(7) 0.071(3) Uani 1 1 d U . .
C28' C 0.2362(10) 0.7973(8) 0.4283(5) 0.057(3) Uani 1 1 d U . .
C29' C 0.3482(8) 0.6770(6) 0.4092(3) 0.034(2) Uani 1 1 d U . .
C30' C 0.4412(8) 0.6129(8) 0.3755(4) 0.044(3) Uani 1 1 d U . .
H30' H 0.4515 0.5748 0.3605 0.058 Uiso 1 1 calc R . .
C31' C 0.5031(8) 0.6564(8) 0.3818(5) 0.049(3) Uani 1 1 d U . .
H31' H 0.5546 0.6488 0.3721 0.066 Uiso 1 1 calc R . .
C32' C 0.4832(9) 0.7132(8) 0.4038(4) 0.046(3) Uani 1 1 d U . .
H32' H 0.5230 0.7449 0.4092 0.062 Uiso 1 1 calc R . .
C33' C 0.4074(8) 0.7242(8) 0.4178(4) 0.042(3) Uani 1 1 d U . .
H33' H 0.3958 0.7623 0.4328 0.055 Uiso 1 1 calc R . .
F1' F 0.1941(6) 0.3122(5) 0.3950(3) 0.064(2) Uani 1 1 d U . .
F2' F 0.0976(7) 0.2273(6) 0.3548(5) 0.100(4) Uani 1 1 d U . .
F3' F 0.0318(8) 0.2668(9) 0.2849(5) 0.119(5) Uani 1 1 d U . .
F4' F 0.0616(7) 0.3930(8) 0.2580(3) 0.092(4) Uani 1 1 d U . .
F5' F 0.1635(5) 0.4747(5) 0.2946(2) 0.0565(19) Uani 1 1 d U . .
F6' F 0.1037(5) 0.4337(5) 0.4579(2) 0.056(2) Uani 1 1 d U . .
F7' F 0.0269(6) 0.3143(6) 0.4621(3) 0.072(3) Uani 1 1 d U . .
F8' F -0.0675(7) 0.2719(6) 0.4048(4) 0.081(3) Uani 1 1 d U . .
F9' F -0.0898(6) 0.3525(6) 0.3402(3) 0.072(3) Uani 1 1 d U . .
F10' F -0.0191(5) 0.4739(5) 0.3354(2) 0.053(2) Uani 1 1 d U . .
F11' F 0.1891(8) 0.6556(5) 0.4898(3) 0.078(3) Uani 1 1 d U . .
F12' F 0.1183(7) 0.7553(8) 0.5278(3) 0.094(4) Uani 1 1 d U . .
F13' F 0.1264(7) 0.8830(7) 0.5037(4) 0.106(5) Uani 1 1 d U . .
F14' F 0.2059(8) 0.9105(6) 0.4375(5) 0.101(4) Uani 1 1 d U . .
F15' F 0.2731(7) 0.8116(5) 0.3942(3) 0.071(2) Uani 1 1 d U . .
K1' K 0.19410(18) 0.51234(17) 0.51909(8) 0.0407(6) Uani 1 1 d U . .
O3' O 0.3510(7) 0.5517(8) 0.5246(3) 0.070(3) Uani 1 1 d U . .
C34' C 0.3892(12) 0.6014(11) 0.5014(5) 0.072(5) Uani 1 1 d U . .
H34a' H 0.3500 0.6247 0.4853 0.095 Uiso 1 1 calc R . .
H34b' H 0.4287 0.5806 0.4845 0.095 Uiso 1 1 calc R . .
C35' C 0.4263(13) 0.6469(12) 0.5267(7) 0.083(5) Uani 1 1 d U . .
H35a' H 0.3883 0.6795 0.5370 0.111 Uiso 1 1 calc R . .
H35b' H 0.4700 0.6707 0.5140 0.111 Uiso 1 1 calc R . .
C36' C 0.4583(12) 0.5970(12) 0.5597(6) 0.077(5) Uani 1 1 d U . .
H36a' H 0.5071 0.5738 0.5519 0.103 Uiso 1 1 calc R . .
H36b' H 0.4670 0.6202 0.5843 0.103 Uiso 1 1 calc R . .
C37' C 0.3890(9) 0.5512(11) 0.5613(4) 0.064(4) Uani 1 1 d U . .
H37a' H 0.4067 0.5057 0.5676 0.085 Uiso 1 1 calc R . .
H37b' H 0.3518 0.5660 0.5813 0.085 Uiso 1 1 calc R . .
O4' O 0.0472(7) 0.5706(8) 0.5197(3) 0.075(3) Uani 1 1 d U . .
C38' C -0.0013(12) 0.5924(14) 0.4879(5) 0.088(6) Uani 1 1 d U . .
H38a' H -0.0167 0.5538 0.4720 0.117 Uiso 1 1 calc R . .
H38b' H 0.0286 0.6237 0.4716 0.117 Uiso 1 1 calc R . .
C39' C -0.0730(11) 0.6255(13) 0.5034(6) 0.077(5) Uani 1 1 d U . .
H39a' H -0.1187 0.6196 0.4862 0.103 Uiso 1 1 calc R . .
H39b' H -0.0639 0.6735 0.5076 0.103 Uiso 1 1 calc R . .
C40' C -0.0853(12) 0.5861(11) 0.5438(6) 0.072(4) Uani 1 1 d U . .
H40a' H -0.1144 0.6130 0.5628 0.096 Uiso 1 1 calc R . .
H40b' H -0.1120 0.5428 0.5402 0.096 Uiso 1 1 calc R . .
C41' C -0.0005(11) 0.5781(12) 0.5541(5) 0.074(5) Uani 1 1 d U . .
H41a' H 0.0175 0.6174 0.5686 0.098 Uiso 1 1 calc R . .
H41b' H 0.0060 0.5386 0.5706 0.098 Uiso 1 1 calc R . .
O5' O 0.2597(8) 0.3910(6) 0.5131(4) 0.066(3) Uani 1 1 d U . .
C42' C 0.3097(13) 0.3771(11) 0.4794(7) 0.082(4) Uani 1 1 d U . .
H42a' H 0.2810 0.3864 0.4554 0.110 Uiso 1 1 calc R . .
H42b' H 0.3585 0.4039 0.4800 0.110 Uiso 1 1 calc R . .
C43' C 0.327(2) 0.3084(12) 0.4827(8) 0.112(7) Uani 1 1 d U . .
H43a' H 0.2922 0.2834 0.4652 0.149 Uiso 1 1 calc R . .
H43b' H 0.3820 0.3009 0.4744 0.149 Uiso 1 1 calc R . .
C44' C 0.318(2) 0.2838(14) 0.5190(8) 0.122(8) Uani 1 1 d U . .
H44a' H 0.3655 0.2901 0.5349 0.163 Uiso 1 1 calc R . .
H44b' H 0.3023 0.2365 0.5191 0.163 Uiso 1 1 calc R . .
C45' C 0.2483(19) 0.3313(11) 0.5312(7) 0.108(7) Uani 1 1 d U . .
H45a' H 0.1971 0.3119 0.5235 0.143 Uiso 1 1 calc R . .
H45b' H 0.2481 0.3375 0.5593 0.143 Uiso 1 1 calc R . .
O6' O 0.5935(11) 0.3875(9) 0.4779(4) 0.099(5) Uani 1 1 d U . .
C46' C 0.5959(18) 0.3281(12) 0.5003(6) 0.091(6) Uani 1 1 d U . .
H46a' H 0.6460 0.3044 0.4957 0.121 Uiso 1 1 calc R . .
H46b' H 0.5519 0.2985 0.4929 0.121 Uiso 1 1 calc R . .
C47' C 0.5893(14) 0.3461(12) 0.5413(6) 0.081(5) Uani 1 1 d U . .
H47a' H 0.6350 0.3290 0.5558 0.107 Uiso 1 1 calc R . .
H47b' H 0.5405 0.3275 0.5525 0.107 Uiso 1 1 calc R . .
C48' C 0.5874(14) 0.4222(12) 0.5423(6) 0.085(5) Uani 1 1 d U . .
H48a' H 0.5493 0.4382 0.5616 0.114 Uiso 1 1 calc R . .
H48b' H 0.6401 0.4403 0.5484 0.114 Uiso 1 1 calc R . .
C49' C 0.5628(17) 0.4424(14) 0.5034(7) 0.099(6) Uani 1 1 d U . .
H49a' H 0.5048 0.4460 0.5016 0.132 Uiso 1 1 calc R . .
H49b' H 0.5865 0.4856 0.4963 0.132 Uiso 1 1 calc R . .


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
U1 O2 1.769(7) . ?
U1 O1 1.775(7) . ?
U1 N6 2.490(9) . ?
U1 N4 2.507(9) . ?
U1 N3 2.532(11) . ?
U1 N5 2.536(11) . ?
U1 N2 2.556(10) . ?
U1 N1 2.602(9) . ?
O1 K1' 2.738(7) 4_564 ?
O2 K1 2.707(7) . ?
N1 C7 1.294(16) . ?
N1 C1 1.383(16) . ?
N2 C8 1.317(17) . ?
N2 C7 1.324(18) . ?
N3 C12 1.366(17) . ?
N3 C18 1.380(17) . ?
N4 C18 1.229(17) . ?
N4 C19 1.463(19) . ?
N5 C23 1.347(16) . ?
N5 C29 1.369(16) . ?
N6 C30 1.391(17) . ?
N6 C29 1.468(15) . ?
C1 C2 1.405(17) . ?
C1 C6 1.396(17) . ?
C2 F1 1.356(14) . ?
C2 C3 1.37(2) . ?
C3 F2 1.358(16) . ?
C3 C4 1.38(2) . ?
C4 F3 1.310(17) . ?
C4 C5 1.34(2) . ?
C5 C6 1.370(19) . ?
C5 F4 1.373(16) . ?
C6 F5 1.341(15) . ?
C7 C11 1.413(18) . ?
C8 C9 1.35(2) . ?
C9 C10 1.42(2) . ?
C10 C11 1.368(19) . ?
C12 C13 1.407(18) . ?
C12 C17 1.402(19) . ?
C13 F6 1.318(15) . ?
C13 C14 1.383(19) . ?
C14 F7 1.346(15) . ?
C14 C15 1.38(2) . ?
C15 F8 1.309(18) . ?
C15 C16 1.40(2) . ?
C16 F9 1.353(16) . ?
C16 C17 1.37(2) . ?
C17 F10 1.274(18) . ?
C18 C22 1.421(19) . ?
C19 C20 1.33(2) . ?
C20 C21 1.40(2) . ?
C21 C22 1.32(2) . ?
C23 C28 1.45(2) . ?
C23 C24 1.432(17) . ?
C24 F11 1.332(17) . ?
C24 C25 1.356(18) . ?
C25 C26 1.29(3) . ?
C25 F12 1.367(19) . ?
C26 F13 1.363(18) . ?
C26 C27 1.42(3) . ?
C27 F14 1.34(2) . ?
C27 C28 1.37(2) . ?
C28 F15 1.308(19) . ?
C29 C33 1.40(2) . ?
C30 C31 1.32(2) . ?
C31 C32 1.35(3) . ?
C32 C33 1.35(2) . ?
F5 K1' 3.004(9) 4_564 ?
F6 K1 2.776(9) . ?
F11 K1' 3.000(10) 4_564 ?
K1 O2' 2.693(8) . ?
K1 O3 2.700(13) . ?
K1 O4 2.757(14) . ?
K1 O5 2.743(12) . ?
K1 F5' 3.074(9) . ?
O3 C37 1.42(3) . ?
O3 C34 1.44(3) . ?
C34 C35 1.44(3) . ?
C35 C36 1.523(10) . ?
C36 C37 1.44(4) . ?
O4 C41 1.421(10) . ?
O4 C38 1.444(10) . ?
C38 C39 1.514(10) . ?
C39 C40 1.513(10) . ?
C40 C41 1.503(10) . ?
O5 C42 1.39(3) . ?
O5 C45 1.43(2) . ?
C42 C43 1.48(3) . ?
C43 C44 1.43(4) . ?
C44 C45 1.54(3) . ?
O6 C49 1.33(2) . ?
O6 C46 1.41(2) . ?
C46 C47 1.46(3) . ?
C47 C48 1.51(4) . ?
C48 C49 1.43(3) . ?
U1' O1' 1.779(7) . ?
U1' O2' 1.783(7) . ?
U1' N3' 2.457(10) . ?
U1' N1' 2.522(11) . ?
U1' N6' 2.538(10) . ?
U1' N4' 2.565(10) . ?
U1' N5' 2.575(10) . ?
U1' N2' 2.588(10) . ?
O1' K1' 2.716(7) . ?
N1' C7' 1.313(16) . ?
N1' C1' 1.399(17) . ?
N2' C8' 1.281(17) . ?
N2' C7' 1.357(16) . ?
N3' C18' 1.342(14) . ?
N3' C12' 1.517(16) . ?
N4' C19' 1.339(18) . ?
N4' C18' 1.384(17) . ?
N5' C29' 1.358(17) . ?
N5' C23' 1.383(17) . ?
N6' C29' 1.330(17) . ?
N6' C30' 1.364(16) . ?
C1' C2' 1.39(2) . ?
C1' C6' 1.40(2) . ?
C2' C3' 1.37(2) . ?
C2' F1' 1.40(2) . ?
C3' C4' 1.36(3) . ?
C3' F2' 1.33(2) . ?
C4' F3' 1.33(2) . ?
C4' C5' 1.32(3) . ?
C5' F4' 1.40(2) . ?
C5' C6' 1.42(2) . ?
C6' F5' 1.301(18) . ?
C7' C11' 1.413(19) . ?
C8' C9' 1.37(2) . ?
C9' C10' 1.49(2) . ?
C10' C11' 1.28(2) . ?
C12' C17' 1.375(18) . ?
C12' C13' 1.392(19) . ?
C13' F6' 1.363(15) . ?
C13' C14' 1.37(2) . ?
C14' F7' 1.309(18) . ?
C14' C15' 1.38(2) . ?
C15' F8' 1.341(18) . ?
C15' C16' 1.41(2) . ?
C16' F9' 1.314(17) . ?
C16' C17' 1.34(2) . ?
C17' F10' 1.338(16) . ?
C18' C22' 1.376(16) . ?
C19' C20' 1.367(19) . ?
C20' C21' 1.37(2) . ?
C21' C22' 1.34(2) . ?
C23' C28' 1.38(2) . ?
C23' C24' 1.42(2) . ?
C24' C25' 1.32(2) . ?
C24' F11' 1.361(19) . ?
C25' F12' 1.37(2) . ?
C25' C26' 1.36(3) . ?
C26' F13' 1.339(19) . ?
C26' C27' 1.39(3) . ?
C27' F14' 1.26(2) . ?
C27' C28' 1.33(3) . ?
C28' F15' 1.35(2) . ?
C29' C33' 1.390(18) . ?
C30' C31' 1.36(2) . ?
C31' C32' 1.39(2) . ?
C32' C33' 1.37(2) . ?
F6' K1' 3.013(9) . ?
F11' K1' 3.004(10) . ?
K1' O5' 2.642(12) . ?
K1' O4' 2.702(11) . ?
K1' O3' 2.731(11) . ?
K1' O1 2.738(7) 4_565 ?
K1' F11 3.000(10) 4_565 ?
K1' F5 3.004(9) 4_565 ?
K1' C42' 3.563(18) . ?
O3' C37' 1.409(17) . ?
O3' C34' 1.41(2) . ?
C34' C35' 1.39(3) . ?
C35' C36' 1.59(3) . ?
C36' C37' 1.47(2) . ?
O4' C41' 1.431(17) . ?
O4' C38' 1.423(18) . ?
C38' C39' 1.46(3) . ?
C39' C40' 1.60(3) . ?
C40' C41' 1.46(3) . ?
O5' C45' 1.35(2) . ?
O5' C42' 1.45(2) . ?
C42' C43' 1.39(3) . ?
C43' C44' 1.34(3) . ?
C44' C45' 1.55(3) . ?
O6' C46' 1.40(3) . ?
O6' C49' 1.48(3) . ?
C46' C47' 1.46(3) . ?
C47' C48' 1.50(3) . ?
C48' C49' 1.45(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
O2 U1 O1 178.0(4) . . ?
O2 U1 N6 81.7(4) . . ?
O1 U1 N6 96.4(3) . . ?
O2 U1 N4 96.0(3) . . ?
O1 U1 N4 82.9(4) . . ?
N6 U1 N4 73.0(3) . . ?
O2 U1 N3 83.1(4) . . ?
O1 U1 N3 97.4(4) . . ?
N6 U1 N3 118.1(3) . . ?
N4 U1 N3 49.6(4) . . ?
O2 U1 N5 97.9(4) . . ?
O1 U1 N5 81.3(4) . . ?
N6 U1 N5 54.4(3) . . ?
N4 U1 N5 122.3(4) . . ?
N3 U1 N5 171.9(4) . . ?
O2 U1 N2 81.9(4) . . ?
O1 U1 N2 99.5(4) . . ?
N6 U1 N2 119.6(3) . . ?
N4 U1 N2 166.4(4) . . ?
N3 U1 N2 116.8(4) . . ?
N5 U1 N2 71.2(3) . . ?
O2 U1 N1 100.5(4) . . ?
O1 U1 N1 81.5(4) . . ?
N6 U1 N1 168.2(3) . . ?
N4 U1 N1 118.0(4) . . ?
N3 U1 N1 73.7(3) . . ?
N5 U1 N1 113.9(3) . . ?
N2 U1 N1 49.9(3) . . ?
U1 O1 K1' 176.1(4) . 4_564 ?
U1 O2 K1 157.1(4) . . ?
C7 N1 C1 126.9(10) . . ?
C7 N1 U1 98.1(8) . . ?
C1 N1 U1 135.1(7) . . ?
C8 N2 C7 118.3(12) . . ?
C8 N2 U1 142.3(11) . . ?
C7 N2 U1 99.4(8) . . ?
C12 N3 C18 123.1(11) . . ?
C12 N3 U1 138.8(8) . . ?
C18 N3 U1 98.1(8) . . ?
C18 N4 C19 119.5(11) . . ?
C18 N4 U1 104.1(9) . . ?
C19 N4 U1 136.4(9) . . ?
C23 N5 C29 119.1(11) . . ?
C23 N5 U1 139.6(8) . . ?
C29 N5 U1 99.1(7) . . ?
C30 N6 C29 107.1(11) . . ?
C30 N6 U1 154.6(9) . . ?
C29 N6 U1 98.2(7) . . ?
N1 C1 C2 122.9(11) . . ?
N1 C1 C6 123.7(11) . . ?
C2 C1 C6 113.4(11) . . ?
F1 C2 C3 118.2(12) . . ?
F1 C2 C1 118.5(11) . . ?
C3 C2 C1 123.1(12) . . ?
F2 C3 C2 119.2(13) . . ?
F2 C3 C4 119.4(13) . . ?
C2 C3 C4 121.2(13) . . ?
F3 C4 C5 125.0(15) . . ?
F3 C4 C3 118.5(15) . . ?
C5 C4 C3 116.5(13) . . ?
C4 C5 C6 123.3(13) . . ?
C4 C5 F4 117.4(13) . . ?
C6 C5 F4 119.4(13) . . ?
F5 C6 C5 117.4(12) . . ?
F5 C6 C1 120.2(11) . . ?
C5 C6 C1 122.4(12) . . ?
N1 C7 N2 112.5(11) . . ?
N1 C7 C11 124.8(12) . . ?
N2 C7 C11 122.5(12) . . ?
N2 C8 C9 126.8(16) . . ?
C8 C9 C10 113.4(14) . . ?
C11 C10 C9 123.0(15) . . ?
C10 C11 C7 115.5(14) . . ?
N3 C12 C13 122.1(11) . . ?
N3 C12 C17 123.6(12) . . ?
C13 C12 C17 114.1(13) . . ?
F6 C13 C14 117.9(12) . . ?
F6 C13 C12 119.3(12) . . ?
C14 C13 C12 122.8(12) . . ?
F7 C14 C15 119.8(13) . . ?
F7 C14 C13 118.6(12) . . ?
C15 C14 C13 121.6(13) . . ?
F8 C15 C14 120.2(14) . . ?
F8 C15 C16 123.0(14) . . ?
C14 C15 C16 116.8(14) . . ?
F9 C16 C17 122.1(14) . . ?
F9 C16 C15 116.7(14) . . ?
C17 C16 C15 121.2(13) . . ?
F10 C17 C16 116.4(13) . . ?
F10 C17 C12 119.9(13) . . ?
C16 C17 C12 123.5(14) . . ?
N4 C18 N3 108.2(12) . . ?
N4 C18 C22 125.6(13) . . ?
N3 C18 C22 126.2(13) . . ?
C20 C19 N4 119.4(15) . . ?
C19 C20 C21 115.6(17) . . ?
C22 C21 C20 127.6(16) . . ?
C21 C22 C18 112.2(15) . . ?
N5 C23 C28 124.9(12) . . ?
N5 C23 C24 122.0(12) . . ?
C28 C23 C24 113.0(12) . . ?
F11 C24 C25 119.7(13) . . ?
F11 C24 C23 117.1(11) . . ?
C25 C24 C23 123.2(14) . . ?
C26 C25 C24 122.2(16) . . ?
C26 C25 F12 118.5(14) . . ?
C24 C25 F12 119.3(15) . . ?
C25 C26 F13 122.0(17) . . ?
C25 C26 C27 120.2(15) . . ?
F13 C26 C27 117.6(16) . . ?
F14 C27 C28 118.1(18) . . ?
F14 C27 C26 122.0(16) . . ?
C28 C27 C26 119.7(16) . . ?
F15 C28 C27 124.8(15) . . ?
F15 C28 C23 113.7(13) . . ?
C27 C28 C23 121.5(15) . . ?
N5 C29 C33 126.6(12) . . ?
N5 C29 N6 108.0(10) . . ?
C33 C29 N6 124.6(11) . . ?
C31 C30 N6 129.2(16) . . ?
C30 C31 C32 119.0(15) . . ?
C33 C32 C31 121.6(16) . . ?
C32 C33 C29 116.4(15) . . ?
C6 F5 K1' 163.6(7) . 4_564 ?
C13 F6 K1 142.4(8) . . ?
C24 F11 K1' 159.8(10) . 4_564 ?
O2' K1 O3 102.5(4) . . ?
O2' K1 O2 170.0(3) . . ?
O3 K1 O2 80.1(4) . . ?
O2' K1 O4 76.6(3) . . ?
O3 K1 O4 83.5(6) . . ?
O2 K1 O4 94.3(4) . . ?
O2' K1 O5 103.8(3) . . ?
O3 K1 O5 80.8(5) . . ?
O2 K1 O5 86.1(3) . . ?
O4 K1 O5 164.0(5) . . ?
O2' K1 F6 117.1(3) . . ?
O3 K1 F6 135.8(4) . . ?
O2 K1 F6 64.4(3) . . ?
O4 K1 F6 122.7(4) . . ?
O5 K1 F6 71.7(3) . . ?
O2' K1 F5' 61.2(2) . . ?
O3 K1 F5' 160.5(4) . . ?
O2 K1 F5' 114.2(3) . . ?
O4 K1 F5' 82.3(4) . . ?
O5 K1 F5' 112.2(3) . . ?
F6 K1 F5' 63.7(2) . . ?
C37 O3 C34 108.1(17) . . ?
C37 O3 K1 123.7(15) . . ?
C34 O3 K1 125.5(11) . . ?
C35 C34 O3 108(2) . . ?
C34 C35 C36 102(2) . . ?
C37 C36 C35 109(2) . . ?
O3 C37 C36 101(2) . . ?
C41 O4 C38 106.3(18) . . ?
C41 O4 K1 110.6(15) . . ?
C38 O4 K1 131.6(14) . . ?
C39 C38 O4 101.6(18) . . ?
C38 C39 C40 103(2) . . ?
C41 C40 C39 106(2) . . ?
C40 C41 O4 98(2) . . ?
C42 O5 C45 103.3(15) . . ?
C42 O5 K1 131.5(10) . . ?
C45 O5 K1 117.3(12) . . ?
O5 C42 C43 107(2) . . ?
C44 C43 C42 106(2) . . ?
C43 C44 C45 103(2) . . ?
O5 C45 C44 103.1(19) . . ?
C49 O6 C46 108.5(17) . . ?
O6 C46 C47 103(2) . . ?
C48 C47 C46 101(2) . . ?
C49 C48 C47 97.9(19) . . ?
O6 C49 C48 110.7(19) . . ?
O1' U1' O2' 178.4(4) . . ?
O1' U1' N3' 85.3(4) . . ?
O2' U1' N3' 95.9(4) . . ?
O1' U1' N1' 97.3(3) . . ?
O2' U1' N1' 84.0(3) . . ?
N3' U1' N1' 75.1(3) . . ?
O1' U1' N6' 99.4(4) . . ?
O2' U1' N6' 79.2(4) . . ?
N3' U1' N6' 168.9(4) . . ?
N1' U1' N6' 114.0(4) . . ?
O1' U1' N4' 98.4(3) . . ?
O2' U1' N4' 81.6(4) . . ?
N3' U1' N4' 50.7(4) . . ?
N1' U1' N4' 121.4(4) . . ?
N6' U1' N4' 118.4(4) . . ?
O1' U1' N5' 82.8(3) . . ?
O2' U1' N5' 95.7(3) . . ?
N3' U1' N5' 120.5(4) . . ?
N1' U1' N5' 164.3(4) . . ?
N6' U1' N5' 50.9(4) . . ?
N4' U1' N5' 74.0(4) . . ?
O1' U1' N2' 79.8(4) . . ?
O2' U1' N2' 100.4(4) . . ?
N3' U1' N2' 121.3(3) . . ?
N1' U1' N2' 51.6(3) . . ?
N6' U1' N2' 69.6(3) . . ?
N4' U1' N2' 171.9(3) . . ?
N5' U1' N2' 113.4(4) . . ?
U1' O1' K1' 166.2(4) . . ?
U1' O2' K1 148.4(4) . . ?
C7' N1' C1' 121.1(11) . . ?
C7' N1' U1' 100.0(8) . . ?
C1' N1' U1' 138.9(8) . . ?
C8' N2' C7' 121.8(12) . . ?
C8' N2' U1' 142.1(10) . . ?
C7' N2' U1' 95.7(7) . . ?
C18' N3' C12' 113.1(9) . . ?
C18' N3' U1' 105.8(8) . . ?
C12' N3' U1' 141.0(7) . . ?
C19' N4' C18' 116.8(11) . . ?
C19' N4' U1' 143.9(10) . . ?
C18' N4' U1' 99.3(7) . . ?
C29' N5' C23' 119.6(11) . . ?
C29' N5' U1' 98.5(8) . . ?
C23' N5' U1' 142.0(9) . . ?
C29' N6' C30' 117.8(11) . . ?
C29' N6' U1' 101.1(7) . . ?
C30' N6' U1' 141.1(9) . . ?
C2' C1' C6' 115.2(14) . . ?
C2' C1' N1' 125.2(14) . . ?
C6' C1' N1' 119.6(13) . . ?
C3' C2' C1' 125.5(18) . . ?
C3' C2' F1' 118.7(16) . . ?
C1' C2' F1' 115.7(13) . . ?
C4' C3' F2' 121.5(18) . . ?
C4' C3' C2' 118.9(19) . . ?
F2' C3' C2' 120(2) . . ?
C3' C4' F3' 121(2) . . ?
C3' C4' C5' 117.6(16) . . ?
F3' C4' C5' 121(2) . . ?
C4' C5' F4' 120.3(16) . . ?
C4' C5' C6' 125.9(19) . . ?
F4' C5' C6' 113.5(18) . . ?
F5' C6' C1' 122.4(13) . . ?
F5' C6' C5' 121.1(15) . . ?
C1' C6' C5' 116.5(16) . . ?
N1' C7' N2' 112.7(11) . . ?
N1' C7' C11' 129.1(13) . . ?
N2' C7' C11' 118.1(11) . . ?
N2' C8' C9' 124.7(14) . . ?
C8' C9' C10' 112.5(13) . . ?
C11' C10' C9' 122.5(14) . . ?
C10' C11' C7' 119.7(14) . . ?
C17' C12' C13' 118.4(13) . . ?
C17' C12' N3' 122.2(12) . . ?
C13' C12' N3' 118.6(11) . . ?
F6' C13' C14' 117.3(13) . . ?
F6' C13' C12' 120.5(12) . . ?
C14' C13' C12' 122.2(13) . . ?
F7' C14' C13' 121.6(15) . . ?
F7' C14' C15' 120.3(15) . . ?
C13' C14' C15' 117.8(14) . . ?
F8' C15' C14' 117.2(15) . . ?
F8' C15' C16' 122.2(14) . . ?
C14' C15' C16' 120.5(14) . . ?
F9' C16' C17' 121.5(15) . . ?
F9' C16' C15' 118.5(14) . . ?
C17' C16' C15' 119.8(13) . . ?
F10' C17' C16' 118.9(12) . . ?
F10' C17' C12' 120.0(13) . . ?
C16' C17' C12' 121.1(14) . . ?
N3' C18' C22' 135.1(13) . . ?
N3' C18' N4' 104.2(10) . . ?
C22' C18' N4' 120.7(11) . . ?
N4' C19' C20' 124.4(15) . . ?
C19' C20' C21' 116.5(14) . . ?
C22' C21' C20' 121.9(12) . . ?
C21' C22' C18' 119.5(14) . . ?
N5' C23' C28' 126.6(14) . . ?
N5' C23' C24' 120.1(13) . . ?
C28' C23' C24' 112.8(14) . . ?
C25' C24' F11' 119.5(15) . . ?
C25' C24' C23' 121.6(16) . . ?
F11' C24' C23' 118.9(12) . . ?
C24' C25' F12' 118.1(18) . . ?
C24' C25' C26' 123.1(18) . . ?
F12' C25' C26' 118.4(16) . . ?
F13' C26' C25' 118(2) . . ?
F13' C26' C27' 124(2) . . ?
C25' C26' C27' 117.3(16) . . ?
F14' C27' C28' 126(2) . . ?
F14' C27' C26' 115.6(18) . . ?
C28' C27' C26' 118.4(18) . . ?
C27' C28' F15' 117.1(16) . . ?
C27' C28' C23' 126.1(18) . . ?
F15' C28' C23' 116.6(14) . . ?
N6' C29' N5' 109.6(11) . . ?
N6' C29' C33' 121.4(12) . . ?
N5' C29' C33' 128.9(12) . . ?
N6' C30' C31' 125.5(14) . . ?
C30' C31' C32' 114.4(13) . . ?
C31' C32' C33' 122.5(13) . . ?
C32' C33' C29' 118.2(14) . . ?
C6' F5' K1 142.8(8) . . ?
C13' F6' K1' 164.1(9) . . ?
C24' F11' K1' 174.1(10) . . ?
O5' K1' O4' 139.6(5) . . ?
O5' K1' O1' 89.6(3) . . ?
O4' K1' O1' 97.9(3) . . ?
O5' K1' O3' 82.4(5) . . ?
O4' K1' O3' 138.0(5) . . ?
O1' K1' O3' 78.3(3) . . ?
O5' K1' O1 82.4(3) . 4_565 ?
O4' K1' O1 91.0(3) . 4_565 ?
O1' K1' O1 170.9(3) . 4_565 ?
O3' K1' O1 96.3(3) . 4_565 ?
O5' K1' F11 73.6(4) . 4_565 ?
O4' K1' F11 68.8(4) . 4_565 ?
O1' K1' F11 122.5(3) . 4_565 ?
O3' K1' F11 147.4(4) . 4_565 ?
O1 K1' F11 59.3(3) 4_565 4_565 ?
O5' K1' F11' 147.2(3) . . ?
O4' K1' F11' 64.9(4) . . ?
O1' K1' F11' 61.2(2) . . ?
O3' K1' F11' 77.4(4) . . ?
O1 K1' F11' 125.1(3) 4_565 . ?
F11 K1' F11' 133.5(3) 4_565 . ?
O5' K1' F5 131.4(3) . 4_565 ?
O4' K1' F5 75.4(3) . 4_565 ?
O1' K1' F5 123.8(3) . 4_565 ?
O3' K1' F5 72.8(3) . 4_565 ?
O1 K1' F5 60.3(2) 4_565 4_565 ?
F11 K1' F5 107.1(3) 4_565 4_565 ?
F11' K1' F5 65.9(2) . 4_565 ?
O5' K1' F6' 71.6(4) . . ?
O4' K1' F6' 76.9(4) . . ?
O1' K1' F6' 62.6(2) . . ?
O3' K1' F6' 132.3(3) . . ?
O1 K1' F6' 118.3(3) 4_565 . ?
F11 K1' F6' 59.9(2) 4_565 . ?
F11' K1' F6' 103.9(3) . . ?
F5 K1' F6' 152.2(3) 4_565 . ?
O5' K1' C42' 21.0(4) . . ?
O4' K1' C42' 144.2(5) . . ?
O1' K1' C42' 69.2(4) . . ?
O3' K1' C42' 74.0(5) . . ?
O1 K1' C42' 102.4(4) 4_565 . ?
F11 K1' C42' 89.6(4) 4_565 . ?
F11' K1' C42' 126.5(4) . . ?
F5 K1' C42' 139.9(5) 4_565 . ?
F6' K1' C42' 67.5(5) . . ?
C37' O3' C34' 107.8(13) . . ?
C37' O3' K1' 119.3(9) . . ?
C34' O3' K1' 126.1(10) . . ?
O3' C34' C35' 107.3(15) . . ?
C34' C35' C36' 101.0(17) . . ?
C37' C36' C35' 98.4(15) . . ?
O3' C37' C36' 108.3(14) . . ?
C41' O4' C38' 106.6(13) . . ?
C41' O4' K1' 123.5(9) . . ?
C38' O4' K1' 129.5(10) . . ?
O4' C38' C39' 108.7(15) . . ?
C38' C39' C40' 101.6(16) . . ?
C41' C40' C39' 97.9(15) . . ?
O4' C41' C40' 110.3(14) . . ?
C45' O5' C42' 106.3(15) . . ?
C45' O5' K1' 134.5(13) . . ?
C42' O5' K1' 118.1(10) . . ?
C43' C42' O5' 103.8(18) . . ?
C43' C42' K1' 144.3(16) . . ?
O5' C42' K1' 40.8(7) . . ?
C44' C43' C42' 114(2) . . ?
C43' C44' C45' 97(2) . . ?
O5' C45' C44' 108(2) . . ?
C46' O6' C49' 107.5(16) . . ?
O6' C46' C47' 108.8(19) . . ?
C46' C47' C48' 105.4(19) . . ?
C49' C48' C47' 105.2(19) . . ?
O6' C49' C48' 104.0(18) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.63
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         6.413
_refine_diff_density_min         -2.302
_refine_diff_density_rms         0.220

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.177 0.986 0.288 313 65 ' '
2 0.322 1.014 0.788 313 65 ' '
3 0.677 0.514 0.712 313 65 ' '
4 0.822 0.486 0.212 313 65 ' '
_database_code_depnum_ccdc_archive 'CCDC 965031'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_cmpd4tol

_audit_creation_method           SHELXL-97

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C70 H48 F24 K2 N4 O2 U'
_chemical_formula_weight         1749.35

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'
F F 0.0171 0.0103 '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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n     '
_symmetry_Int_Tables_number      14

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

_cell_length_a                   15.9136(9)
_cell_length_b                   21.3308(13)
_cell_length_c                   22.1833(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.360(3)
_cell_angle_gamma                90.00
_cell_volume                     7059.7(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    143(1)
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04

_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3432
_exptl_absorpt_coefficient_mu    2.528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_absorpt_correction_T_min  0.6866
_exptl_absorpt_correction_T_max  0.7456
_diffrn_ambient_temperature      143(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            188472
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         27.55
_reflns_number_total             16272
_reflns_number_gt                12727
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0292P)²+9.9805P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         16272
_refine_ls_number_parameters     999
_refine_ls_number_restraints     750
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0309
_refine_ls_wR_factor_ref         0.0750
_refine_ls_wR_factor_gt          0.0676
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.221
_refine_ls_shift/su_max          0.024
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.529289(8) 0.295317(6) 0.285780(6) 0.02150(4) Uani 1 1 d . . .
N1 N 0.5193(2) 0.35548(15) 0.19201(14) 0.0286(7) Uani 1 1 d . . .
N2 N 0.60549(19) 0.37957(14) 0.35250(14) 0.0265(7) Uani 1 1 d . . .
N3 N 0.5375(2) 0.23342(15) 0.37788(14) 0.0262(6) Uani 1 1 d . . .
N4 N 0.44654(19) 0.21037(14) 0.22153(14) 0.0252(6) Uani 1 1 d . . .
O1 O 0.42557(15) 0.33198(11) 0.28210(11) 0.0237(5) Uani 1 1 d . . .
O2 O 0.63175(16) 0.25868(12) 0.28612(11) 0.0258(5) Uani 1 1 d . C .
C1 C 0.4349(2) 0.37996(18) 0.15309(17) 0.0287(8) Uani 1 1 d . . .
C2 C 0.3595(3) 0.3420(2) 0.13205(17) 0.0319(9) Uani 1 1 d . . .
H2 H 0.3659 0.2991 0.1397 0.042 Uiso 1 1 calc R . .
C3 C 0.2745(3) 0.3661(2) 0.09987(19) 0.0407(10) Uani 1 1 d . . .
H3 H 0.2250 0.3397 0.0871 0.054 Uiso 1 1 calc R . .
C4 C 0.2641(3) 0.4294(2) 0.0870(2) 0.0474(12) Uani 1 1 d . . .
H4 H 0.2073 0.4460 0.0661 0.063 Uiso 1 1 calc R . .
C5 C 0.3379(3) 0.4680(2) 0.1052(2) 0.0460(11) Uani 1 1 d . . .
H5 H 0.3310 0.5105 0.0954 0.061 Uiso 1 1 calc R . .
C6 C 0.4230(3) 0.4441(2) 0.1382(2) 0.0392(10) Uani 1 1 d . . .
H6 H 0.4722 0.4708 0.1506 0.052 Uiso 1 1 calc R . .
C7 C 0.5906(3) 0.36803(18) 0.17139(18) 0.0302(8) Uani 1 1 d . . .
C8 C 0.6785(3) 0.37206(18) 0.2160(2) 0.0319(9) Uani 1 1 d . . .
H8 H 0.6883 0.3688 0.2597 0.042 Uiso 1 1 calc R . .
C9 C 0.7509(3) 0.3809(2) 0.1954(2) 0.0394(10) Uani 1 1 d . A .
C10 C 0.7390(3) 0.3868(3) 0.1311(2) 0.0524(12) Uani 1 1 d . . .
H10 H 0.7876 0.3928 0.1176 0.070 Uiso 1 1 calc R . .
C11 C 0.6530(3) 0.3837(3) 0.0874(2) 0.0558(13) Uani 1 1 d . B .
C12 C 0.5795(3) 0.3745(2) 0.1063(2) 0.0465(11) Uani 1 1 d . . .
H12 H 0.5224 0.3726 0.0754 0.062 Uiso 1 1 calc R . .
C15 C 0.5496(2) 0.43241(17) 0.35122(17) 0.0267(8) Uani 1 1 d . . .
C16 C 0.5283(3) 0.47418(19) 0.30054(19) 0.0348(9) Uani 1 1 d . . .
H16 H 0.5505 0.4675 0.2674 0.046 Uiso 1 1 calc R . .
C17 C 0.4743(3) 0.52605(19) 0.2981(2) 0.0407(10) Uani 1 1 d . . .
H17 H 0.4604 0.5537 0.2637 0.054 Uiso 1 1 calc R . .
C18 C 0.4415(3) 0.5362(2) 0.3472(2) 0.0422(11) Uani 1 1 d . . .
H18 H 0.4064 0.5713 0.3464 0.056 Uiso 1 1 calc R . .
C19 C 0.4607(3) 0.4943(2) 0.3974(2) 0.0422(10) Uani 1 1 d . . .
H19 H 0.4375 0.5006 0.4301 0.056 Uiso 1 1 calc R . .
C20 C 0.5142(3) 0.44298(19) 0.39946(19) 0.0346(9) Uani 1 1 d . . .
H20 H 0.5268 0.4150 0.4336 0.046 Uiso 1 1 calc R . .
C21 C 0.6941(2) 0.38728(18) 0.39319(16) 0.0268(8) Uani 1 1 d . . .
C22 C 0.7561(2) 0.33861(19) 0.40150(18) 0.0326(9) Uani 1 1 d . . .
H22 H 0.7378 0.3015 0.3786 0.043 Uiso 1 1 calc R . .
C23 C 0.8436(3) 0.3441(2) 0.44277(19) 0.0376(10) Uani 1 1 d . . .
C24 C 0.8746(3) 0.3985(2) 0.47742(19) 0.0382(10) Uani 1 1 d . . .
H24 H 0.9335 0.4018 0.5055 0.051 Uiso 1 1 calc R . .
C25 C 0.8152(3) 0.44773(19) 0.46904(18) 0.0316(9) Uani 1 1 d . . .
C26 C 0.7267(2) 0.44275(18) 0.42753(17) 0.0284(8) Uani 1 1 d . . .
H26 H 0.6884 0.4768 0.4225 0.038 Uiso 1 1 calc R . .
C29 C 0.5931(3) 0.17877(18) 0.38742(17) 0.0278(8) Uani 1 1 d . . .
C30 C 0.5584(3) 0.12230(19) 0.3589(2) 0.0348(9) Uani 1 1 d . . .
H30 H 0.4981 0.1198 0.3334 0.046 Uiso 1 1 calc R . .
C31 C 0.6120(3) 0.0694(2) 0.3679(2) 0.0445(11) Uani 1 1 d . C .
H31 H 0.5874 0.0319 0.3482 0.059 Uiso 1 1 calc R . .
C32 C 0.7015(3) 0.0719(2) 0.4056(2) 0.0463(11) Uani 1 1 d . C .
H32 H 0.7373 0.0363 0.4118 0.062 Uiso 1 1 calc R . .
C33 C 0.7373(3) 0.1281(2) 0.4340(2) 0.0414(10) Uani 1 1 d . . .
H33 H 0.7977 0.1304 0.4590 0.055 Uiso 1 1 calc R . .
C34 C 0.6837(3) 0.1811(2) 0.42560(18) 0.0331(9) Uani 1 1 d . . .
H34 H 0.7084 0.2185 0.4456 0.044 Uiso 1 1 calc R . .
C35 C 0.4918(2) 0.23837(17) 0.42059(16) 0.0251(7) Uani 1 1 d . . .
C36 C 0.5022(3) 0.19523(18) 0.47093(18) 0.0304(8) Uani 1 1 d . . .
H36 H 0.5417 0.1618 0.4766 0.040 Uiso 1 1 calc R . .
C37 C 0.4539(3) 0.2024(2) 0.51212(19) 0.0361(9) Uani 1 1 d . . .
C38 C 0.3947(3) 0.2507(2) 0.5059(2) 0.0388(10) Uani 1 1 d . . .
H38 H 0.3620 0.2543 0.5333 0.052 Uiso 1 1 calc R . .
C39 C 0.3853(3) 0.2937(2) 0.45747(18) 0.0334(8) Uani 1 1 d . . .
C40 C 0.4324(2) 0.28847(18) 0.41608(17) 0.0288(8) Uani 1 1 d . . .
H40 H 0.4247 0.3187 0.3844 0.038 Uiso 1 1 calc R . .
C43 C 0.4884(2) 0.17009(19) 0.18931(17) 0.0279(8) Uani 1 1 d . C .
C44 C 0.5371(3) 0.1938(2) 0.15311(18) 0.0345(9) Uani 1 1 d . C .
H44 H 0.5396 0.2369 0.1476 0.046 Uiso 1 1 calc R . .
C45 C 0.5823(3) 0.1539(3) 0.1251(2) 0.0462(12) Uani 1 1 d . C .
H45 H 0.6148 0.1704 0.1011 0.061 Uiso 1 1 calc R . .
C46 C 0.5789(3) 0.0900(3) 0.1330(2) 0.0491(12) Uani 1 1 d . . .
H46 H 0.6097 0.0634 0.1146 0.065 Uiso 1 1 calc R . .
C47 C 0.5302(3) 0.0652(2) 0.1678(2) 0.0455(11) Uani 1 1 d . . .
H47 H 0.5272 0.0220 0.1726 0.061 Uiso 1 1 calc R . .
C48 C 0.4856(3) 0.10509(19) 0.19576(19) 0.0341(9) Uani 1 1 d . . .
H48 H 0.4530 0.0882 0.2194 0.045 Uiso 1 1 calc R . .
C49 C 0.3547(2) 0.20196(17) 0.20478(16) 0.0234(7) Uani 1 1 d . . .
C50 C 0.3004(2) 0.17894(17) 0.14428(17) 0.0262(8) Uani 1 1 d . . .
H50 H 0.3270 0.1638 0.1159 0.035 Uiso 1 1 calc R . .
C51 C 0.2080(2) 0.17855(17) 0.12636(17) 0.0267(8) Uani 1 1 d . . .
C52 C 0.1647(2) 0.20074(18) 0.16616(19) 0.0307(8) Uani 1 1 d . . .
H52 H 0.1025 0.2016 0.1530 0.041 Uiso 1 1 calc R . .
C53 C 0.2176(3) 0.22183(18) 0.22679(19) 0.0305(8) Uani 1 1 d . . .
C54 C 0.3102(2) 0.22083(16) 0.24675(18) 0.0258(8) Uani 1 1 d . . .
H54 H 0.3436 0.2328 0.2886 0.034 Uiso 1 1 calc R . .
C13 C 0.8453(2) 0.38552(17) 0.24552(17) 0.0573(12) Uani 1 1 d GDU . .
F1 F 0.8451(4) 0.4045(3) 0.3016(2) 0.0686(18) Uani 0.60 1 d PGU A 1
F2 F 0.8912(4) 0.4251(3) 0.2240(3) 0.089(2) Uani 0.60 1 d PGU A 1
F3 F 0.8823(5) 0.32991(19) 0.2515(3) 0.117(3) Uani 0.60 1 d PGU A 1
F1' F 0.8500(7) 0.4306(3) 0.2872(4) 0.074(3) Uani 0.40 1 d PGDU A 2
F2' F 0.9090(6) 0.3877(5) 0.2243(4) 0.084(3) Uani 0.40 1 d PGDU A 2
F3' F 0.8624(6) 0.3307(3) 0.2856(4) 0.071(2) Uani 0.40 1 d PGDU A 2
C14 C 0.6367(3) 0.3896(3) 0.0155(2) 0.0928(19) Uani 1 1 d GDU . .
F4 F 0.7039(4) 0.4202(4) 0.0082(5) 0.085(3) Uani 0.45 1 d PGU B 1
F5 F 0.5612(4) 0.4167(5) -0.0186(4) 0.105(3) Uani 0.45 1 d PGU B 1
F6 F 0.6369(8) 0.3316(3) -0.0040(5) 0.142(4) Uani 0.45 1 d PGU B 1
F4' F 0.7056(3) 0.3881(4) -0.0017(4) 0.095(3) Uani 0.55 1 d PGDU B 2
F5' F 0.6012(5) 0.4510(3) -0.0010(4) 0.119(3) Uani 0.55 1 d PGDU B 2
F6' F 0.5727(4) 0.3536(4) -0.0206(3) 0.089(2) Uani 0.55 1 d PGDU B 2
C27 C 0.9059(3) 0.2896(3) 0.4516(3) 0.0545(12) Uani 1 1 d U . .
F7 F 0.9059(3) 0.25342(17) 0.50172(18) 0.0913(11) Uani 1 1 d U . .
F8 F 0.8816(2) 0.25006(16) 0.40226(16) 0.0812(11) Uani 1 1 d U . .
F9 F 0.9896(2) 0.30562(17) 0.4643(2) 0.0942(12) Uani 1 1 d U . .
C28 C 0.8435(3) 0.5069(2) 0.50685(19) 0.0363(9) Uani 1 1 d U . .
F10 F 0.93189(17) 0.51526(14) 0.52867(15) 0.0625(8) Uani 1 1 d U . .
F11 F 0.80993(19) 0.55802(12) 0.47193(12) 0.0522(7) Uani 1 1 d U . .
F12 F 0.8166(2) 0.50968(15) 0.55684(13) 0.0667(9) Uani 1 1 d U . .
C41 C 0.4691(3) 0.1554(3) 0.5644(2) 0.0508(12) Uani 1 1 d U . .
F13 F 0.5547(2) 0.1453(2) 0.59699(19) 0.1046(14) Uani 1 1 d U . .
F14 F 0.4371(4) 0.10089(19) 0.5450(2) 0.1265(17) Uani 1 1 d U . .
F15 F 0.4367(3) 0.1711(2) 0.60873(19) 0.1121(15) Uani 1 1 d U . .
C42 C 0.3257(3) 0.3494(2) 0.4524(2) 0.0457(11) Uani 1 1 d U . .
F16 F 0.2486(2) 0.33382(17) 0.45909(19) 0.0801(10) Uani 1 1 d U . .
F17 F 0.3634(2) 0.39249(15) 0.49690(16) 0.0775(10) Uani 1 1 d U . .
F18 F 0.3043(2) 0.37934(15) 0.39627(14) 0.0668(8) Uani 1 1 d U . .
C55 C 0.1554(3) 0.15408(19) 0.06078(18) 0.0327(9) Uani 1 1 d U . .
F19 F 0.17810(17) 0.09464(12) 0.05295(11) 0.0464(6) Uani 1 1 d U . .
F20 F 0.06732(15) 0.15321(13) 0.04897(11) 0.0476(6) Uani 1 1 d U . .
F21 F 0.16853(18) 0.18727(13) 0.01404(11) 0.0524(7) Uani 1 1 d U . .
C56 C 0.1742(3) 0.2475(2) 0.2712(2) 0.0471(11) Uani 1 1 d U . .
F22 F 0.2150(3) 0.2333(2) 0.33166(16) 0.0879(11) Uani 1 1 d U . .
F23 F 0.1807(3) 0.31022(19) 0.2743(2) 0.1144(15) Uani 1 1 d U . .
F24 F 0.0912(2) 0.2378(3) 0.2543(2) 0.1401(18) Uani 1 1 d U . .
K1 K 0.31355(6) 0.42415(5) 0.24467(5) 0.0429(2) Uani 1 1 d . . .
C57 C 0.1660(3) 0.5411(2) 0.1872(2) 0.0368(9) Uani 1 1 d . . .
C58 C 0.1091(3) 0.4897(2) 0.1713(2) 0.0429(10) Uani 1 1 d . . .
H58 H 0.0780 0.4808 0.1282 0.057 Uiso 1 1 calc R . .
C59 C 0.0978(3) 0.4515(2) 0.2182(2) 0.0456(11) Uani 1 1 d . . .
H59 H 0.0592 0.4173 0.2065 0.061 Uiso 1 1 calc R . .
C60 C 0.1436(3) 0.4637(2) 0.2825(2) 0.0415(10) Uani 1 1 d . . .
H60 H 0.1361 0.4380 0.3141 0.055 Uiso 1 1 calc R . .
C61 C 0.2005(3) 0.5146(2) 0.2991(2) 0.0392(10) Uani 1 1 d . . .
H61 H 0.2314 0.5234 0.3422 0.052 Uiso 1 1 calc R . .
C62 C 0.2119(3) 0.5524(2) 0.2522(2) 0.0383(10) Uani 1 1 d . . .
H62 H 0.2512 0.5862 0.2642 0.051 Uiso 1 1 calc R . .
C63 C 0.1772(4) 0.5839(2) 0.1364(2) 0.0544(13) Uani 1 1 d . . .
H63a H 0.1452 0.6222 0.1353 0.082 Uiso 1 1 calc R . .
H63b H 0.1540 0.5637 0.0952 0.082 Uiso 1 1 calc R . .
H63c H 0.2397 0.5929 0.1463 0.082 Uiso 1 1 calc R . .
K2 K 0.69414(6) 0.14669(5) 0.27854(4) 0.0384(2) Uani 1 1 d . . .
C64 C 0.8616(4) 0.1442(2) 0.2213(2) 0.053(2) Uani 0.65 1 d PGU C 1
C65 C 0.8132(4) 0.0895(3) 0.19791(19) 0.048(2) Uani 0.65 1 d PGU C 1
H65 H 0.7837 0.0844 0.1539 0.064 Uiso 0.65 1 calc PR C 1
C66 C 0.8091(4) 0.0425(2) 0.2405(3) 0.0456(18) Uani 0.65 1 d PGU C 1
H66 H 0.7768 0.0060 0.2249 0.061 Uiso 0.65 1 calc PR C 1
C67 C 0.8533(4) 0.0502(3) 0.3064(3) 0.045(2) Uani 0.65 1 d PGU C 1
H67 H 0.8505 0.0189 0.3348 0.060 Uiso 0.65 1 calc PR C 1
C68 C 0.9017(5) 0.1049(3) 0.32980(19) 0.055(2) Uani 0.65 1 d PGU C 1
H68 H 0.9312 0.1101 0.3738 0.073 Uiso 0.65 1 calc PR C 1
C69 C 0.9058(5) 0.1520(3) 0.2872(3) 0.056(2) Uani 0.65 1 d PGU C 1
H69 H 0.9381 0.1884 0.3028 0.074 Uiso 0.65 1 calc PR C 1
C70 C 0.8662(7) 0.1962(3) 0.1742(4) 0.087(3) Uani 0.65 1 d PGU C 1
H70a H 0.9018 0.2303 0.1979 0.130 Uiso 0.65 1 calc PR C 1
H70b H 0.8067 0.2108 0.1507 0.130 Uiso 0.65 1 calc PR C 1
H70c H 0.8928 0.1797 0.1448 0.130 Uiso 0.65 1 calc PR C 1
C64' C 0.8561(8) 0.1320(5) 0.2153(4) 0.054(4) Uani 0.35 1 d PGU C 2
C65' C 0.8205(8) 0.0728(5) 0.2181(5) 0.050(3) Uani 0.35 1 d PGU C 2
H65' H 0.7870 0.0524 0.1803 0.066 Uiso 0.35 1 calc PR C 2
C66' C 0.8351(9) 0.0442(4) 0.2774(6) 0.050(4) Uani 0.35 1 d PGU C 2
H66' H 0.8113 0.0047 0.2792 0.067 Uiso 0.35 1 calc PR C 2
C67' C 0.8853(7) 0.0749(5) 0.3340(5) 0.048(4) Uani 0.35 1 d PGU C 2
H67' H 0.8950 0.0558 0.3736 0.064 Uiso 0.35 1 calc PR C 2
C68' C 0.9210(8) 0.1341(5) 0.3313(4) 0.050(4) Uani 0.35 1 d PGU C 2
H68' H 0.9545 0.1545 0.3691 0.066 Uiso 0.35 1 calc PR C 2
C69' C 0.9064(9) 0.1627(4) 0.2720(5) 0.056(4) Uani 0.35 1 d PGU C 2
H69' H 0.9301 0.2022 0.2701 0.075 Uiso 0.35 1 calc PR C 2
C70' C 0.8400(14) 0.1636(9) 0.1498(5) 0.094(6) Uani 0.35 1 d PGU C 2
H70a' H 0.8045 0.1365 0.1160 0.141 Uiso 0.35 1 calc PR C 2
H70b' H 0.8965 0.1714 0.1447 0.141 Uiso 0.35 1 calc PR C 2
H70c' H 0.8090 0.2025 0.1480 0.141 Uiso 0.35 1 calc PR C 2


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
U1 O1 1.802(2) . ?
U1 O2 1.806(2) . ?
U1 N2 2.375(3) . ?
U1 N4 2.396(3) . ?
U1 N3 2.398(3) . ?
U1 N1 2.402(3) . ?
N1 C7 1.389(5) . ?
N1 C1 1.420(5) . ?
N2 C21 1.394(4) . ?
N2 C15 1.430(5) . ?
N3 C35 1.384(4) . ?
N3 C29 1.435(5) . ?
N4 C49 1.388(4) . ?
N4 C43 1.422(5) . ?
O1 K1 2.589(2) . ?
O2 K2 2.615(3) . ?
C1 C2 1.388(5) . ?
C1 C6 1.405(6) . ?
C1 K1 3.387(4) . ?
C2 C3 1.389(5) . ?
C2 K1 3.334(4) . ?
C3 C4 1.378(7) . ?
C3 K1 3.294(4) . ?
C4 C5 1.375(7) . ?
C4 K1 3.309(4) . ?
C5 C6 1.392(6) . ?
C5 K1 3.381(4) . ?
C6 K1 3.413(4) . ?
C7 C12 1.400(6) . ?
C7 C8 1.407(5) . ?
C8 C9 1.392(5) . ?
C9 C10 1.378(6) . ?
C9 C13 1.529(5) . ?
C10 C11 1.377(7) . ?
C11 C12 1.385(6) . ?
C11 C14 1.531(6) . ?
C15 C16 1.381(5) . ?
C15 C20 1.390(5) . ?
C16 C17 1.391(6) . ?
C16 K1 3.377(4) . ?
C17 C18 1.378(6) . ?
C17 K1 3.250(4) . ?
C18 C19 1.378(6) . ?
C18 K1 3.437(4) . ?
C19 C20 1.377(6) . ?
C21 C22 1.399(5) . ?
C21 C26 1.405(5) . ?
C22 C23 1.380(5) . ?
C23 C24 1.385(6) . ?
C23 C27 1.496(6) . ?
C24 C25 1.381(6) . ?
C25 C26 1.394(5) . ?
C25 C28 1.495(6) . ?
C29 C30 1.383(6) . ?
C29 C34 1.396(5) . ?
C29 K2 3.404(4) . ?
C30 C31 1.387(6) . ?
C30 K2 3.286(4) . ?
C31 C32 1.380(7) . ?
C31 K2 3.186(5) . ?
C32 C33 1.381(7) . ?
C32 K2 3.205(4) . ?
C33 C34 1.389(6) . ?
C33 K2 3.298(4) . ?
C34 K2 3.404(4) . ?
C35 C40 1.407(5) . ?
C35 C36 1.412(5) . ?
C36 C37 1.392(5) . ?
C37 C38 1.371(6) . ?
C37 C41 1.488(6) . ?
C38 C39 1.382(6) . ?
C39 C40 1.376(5) . ?
C39 C42 1.499(6) . ?
C43 C44 1.392(5) . ?
C43 C48 1.396(6) . ?
C43 K2 3.222(4) . ?
C44 C45 1.393(6) . ?
C44 K2 3.187(4) . ?
C45 C46 1.378(7) . ?
C45 K2 3.250(4) . ?
C46 C47 1.377(7) . ?
C46 K2 3.337(4) . ?
C47 C48 1.385(6) . ?
C47 K2 3.377(4) . ?
C48 K2 3.307(4) . ?
C49 C50 1.408(5) . ?
C49 C54 1.411(5) . ?
C50 C51 1.383(5) . ?
C51 C52 1.379(5) . ?
C51 C55 1.497(5) . ?
C52 C53 1.390(5) . ?
C53 C54 1.383(5) . ?
C53 C56 1.491(6) . ?
C13 F2' 1.260(6) . ?
C13 F2 1.3099 . ?
C13 F1 1.3100 . ?
C13 F3 1.3100 . ?
C13 F1' 1.318(7) . ?
C13 F3' 1.436(6) . ?
C14 F4' 1.282(6) . ?
C14 F4 1.3100 . ?
C14 F6 1.3101 . ?
C14 F5 1.3101 . ?
C14 F6' 1.304(6) . ?
C14 F5' 1.422(7) . ?
C27 F9 1.308(6) . ?
C27 F8 1.328(5) . ?
C27 F7 1.353(7) . ?
C28 F12 1.322(5) . ?
C28 F10 1.331(5) . ?
C28 F11 1.337(5) . ?
C41 F14 1.282(6) . ?
C41 F15 1.304(6) . ?
C41 F13 1.319(6) . ?
C42 F17 1.329(5) . ?
C42 F16 1.328(5) . ?
C42 F18 1.335(5) . ?
C55 F21 1.331(4) . ?
C55 F20 1.333(4) . ?
C55 F19 1.346(5) . ?
C56 F24 1.259(5) . ?
C56 F22 1.306(6) . ?
C56 F23 1.341(6) . ?
K1 C61 3.151(4) . ?
K1 C62 3.212(4) . ?
K1 C60 3.212(4) . ?
K1 C59 3.327(5) . ?
K1 C57 3.359(4) . ?
C57 C58 1.387(6) . ?
C57 C62 1.391(6) . ?
C57 C63 1.508(6) . ?
C58 C59 1.384(6) . ?
C59 C60 1.381(6) . ?
C60 C61 1.380(6) . ?
C61 C62 1.378(6) . ?
K2 C66' 3.138(13) . ?
K2 C67 3.153(5) . ?
K2 C66 3.174(6) . ?
K2 C65' 3.194(13) . ?
K2 C68 3.222(7) . ?
K2 C67' 3.242(10) . ?
C64 C65 1.3949 . ?
C64 C69 1.3950 . ?
C64 C70 1.5402 . ?
C65 C66 1.3950 . ?
C66 C67 1.3950 . ?
C67 C68 1.3950 . ?
C68 C69 1.3951 . ?
C64' C69' 1.3949 . ?
C64' C65' 1.3950 . ?
C64' C70' 1.5400 . ?
C65' C66' 1.3950 . ?
C66' C67' 1.3949 . ?
C67' C68' 1.3950 . ?
C68' C69' 1.3950 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 177.79(10) . . ?
O1 U1 N2 87.76(10) . . ?
O2 U1 N2 93.46(10) . . ?
O1 U1 N4 89.77(10) . . ?
O2 U1 N4 89.07(10) . . ?
N2 U1 N4 176.81(10) . . ?
O1 U1 N3 93.15(10) . . ?
O2 U1 N3 88.68(10) . . ?
N2 U1 N3 91.21(10) . . ?
N4 U1 N3 86.91(10) . . ?
O1 U1 N1 86.87(10) . . ?
O2 U1 N1 91.27(11) . . ?
N2 U1 N1 90.05(11) . . ?
N4 U1 N1 91.83(10) . . ?
N3 U1 N1 178.74(11) . . ?
C7 N1 C1 115.9(3) . . ?
C7 N1 U1 125.0(2) . . ?
C1 N1 U1 119.1(2) . . ?
C21 N2 C15 113.7(3) . . ?
C21 N2 U1 132.4(2) . . ?
C15 N2 U1 113.9(2) . . ?
C35 N3 C29 113.9(3) . . ?
C35 N3 U1 131.0(2) . . ?
C29 N3 U1 114.9(2) . . ?
C49 N4 C43 114.8(3) . . ?
C49 N4 U1 124.5(2) . . ?
C43 N4 U1 120.0(2) . . ?
U1 O1 K1 149.49(12) . . ?
U1 O2 K2 139.26(13) . . ?
C2 C1 C6 117.4(4) . . ?
C2 C1 N1 121.0(3) . . ?
C6 C1 N1 121.5(4) . . ?
C2 C1 K1 76.0(2) . . ?
C6 C1 K1 79.1(2) . . ?
N1 C1 K1 110.7(2) . . ?
C1 C2 C3 121.9(4) . . ?
C1 C2 K1 80.2(2) . . ?
C3 C2 K1 76.3(2) . . ?
C4 C3 C2 119.7(4) . . ?
C4 C3 K1 78.6(3) . . ?
C2 C3 K1 79.6(2) . . ?
C5 C4 C3 119.7(4) . . ?
C5 C4 K1 81.1(3) . . ?
C3 C4 K1 77.3(2) . . ?
C4 C5 C6 120.7(4) . . ?
C4 C5 K1 75.2(3) . . ?
C6 C5 K1 79.5(2) . . ?
C5 C6 C1 120.4(4) . . ?
C5 C6 K1 76.9(3) . . ?
C1 C6 K1 77.0(2) . . ?
N1 C7 C12 122.3(4) . . ?
N1 C7 C8 120.4(3) . . ?
C12 C7 C8 117.2(4) . . ?
C9 C8 C7 120.7(4) . . ?
C10 C9 C8 121.4(4) . . ?
C10 C9 C13 119.5(4) . . ?
C8 C9 C13 119.1(4) . . ?
C11 C10 C9 117.9(4) . . ?
C10 C11 C12 122.2(4) . . ?
C10 C11 C14 119.7(4) . . ?
C12 C11 C14 118.1(4) . . ?
C11 C12 C7 120.6(4) . . ?
C16 C15 C20 118.1(4) . . ?
C16 C15 N2 120.0(3) . . ?
C20 C15 N2 121.9(3) . . ?
C15 C16 C17 121.2(4) . . ?
C15 C16 K1 91.5(2) . . ?
C17 C16 K1 72.8(2) . . ?
C18 C17 C16 119.6(4) . . ?
C18 C17 K1 85.8(3) . . ?
C16 C17 K1 83.1(2) . . ?
C17 C18 C19 119.8(4) . . ?
C17 C18 K1 70.6(2) . . ?
C19 C18 K1 89.8(3) . . ?
C20 C19 C18 120.2(4) . . ?
C19 C20 C15 121.0(4) . . ?
N2 C21 C22 120.3(3) . . ?
N2 C21 C26 123.4(3) . . ?
C22 C21 C26 116.3(3) . . ?
C23 C22 C21 121.8(4) . . ?
C22 C23 C24 121.4(4) . . ?
C22 C23 C27 119.4(4) . . ?
C24 C23 C27 119.1(4) . . ?
C25 C24 C23 117.9(4) . . ?
C24 C25 C26 121.2(4) . . ?
C24 C25 C28 120.5(3) . . ?
C26 C25 C28 118.2(4) . . ?
C25 C26 C21 121.3(4) . . ?
C30 C29 C34 118.3(4) . . ?
C30 C29 N3 120.8(3) . . ?
C34 C29 N3 121.0(4) . . ?
C30 C29 K2 73.3(2) . . ?
C34 C29 K2 78.2(2) . . ?
N3 C29 K2 118.6(2) . . ?
C29 C30 C31 121.0(4) . . ?
C29 C30 K2 82.9(2) . . ?
C31 C30 K2 73.6(2) . . ?
C32 C31 C30 120.7(4) . . ?
C32 C31 K2 78.3(3) . . ?
C30 C31 K2 81.7(3) . . ?
C31 C32 C33 119.0(4) . . ?
C31 C32 K2 76.8(3) . . ?
C33 C32 K2 81.5(3) . . ?
C32 C33 C34 120.6(4) . . ?
C32 C33 K2 74.0(2) . . ?
C34 C33 K2 82.3(2) . . ?
C33 C34 C29 120.5(4) . . ?
C33 C34 K2 73.8(2) . . ?
C29 C34 K2 78.2(2) . . ?
N3 C35 C40 120.6(3) . . ?
N3 C35 C36 123.1(3) . . ?
C40 C35 C36 116.3(3) . . ?
C37 C36 C35 120.5(4) . . ?
C38 C37 C36 122.3(4) . . ?
C38 C37 C41 120.3(4) . . ?
C36 C37 C41 117.4(4) . . ?
C37 C38 C39 117.5(4) . . ?
C40 C39 C38 121.9(4) . . ?
C40 C39 C42 119.5(4) . . ?
C38 C39 C42 118.6(4) . . ?
C39 C40 C35 121.5(4) . . ?
C44 C43 C48 117.7(4) . . ?
C44 C43 N4 121.5(4) . . ?
C48 C43 N4 120.8(4) . . ?
C44 C43 K2 76.1(2) . . ?
C48 C43 K2 81.1(2) . . ?
N4 C43 K2 109.8(2) . . ?
C43 C44 C45 120.8(4) . . ?
C43 C44 K2 78.9(2) . . ?
C45 C44 K2 80.0(2) . . ?
C46 C45 C44 120.0(4) . . ?
C46 C45 K2 81.5(3) . . ?
C44 C45 K2 75.0(2) . . ?
C47 C46 C45 120.4(4) . . ?
C47 C46 K2 79.8(3) . . ?
C45 C46 K2 74.4(2) . . ?
C46 C47 C48 119.4(5) . . ?
C46 C47 K2 76.5(3) . . ?
C48 C47 K2 75.2(2) . . ?
C47 C48 C43 121.7(4) . . ?
C47 C48 K2 80.9(2) . . ?
C43 C48 K2 74.3(2) . . ?
N4 C49 C50 122.7(3) . . ?
N4 C49 C54 120.7(3) . . ?
C50 C49 C54 116.5(3) . . ?
C51 C50 C49 121.0(3) . . ?
C52 C51 C50 122.1(3) . . ?
C52 C51 C55 120.4(3) . . ?
C50 C51 C55 117.4(3) . . ?
C51 C52 C53 117.5(3) . . ?
C54 C53 C52 121.6(4) . . ?
C54 C53 C56 118.7(4) . . ?
C52 C53 C56 119.6(4) . . ?
C53 C54 C49 121.1(3) . . ?
F2' C13 F2 38.4(4) . . ?
F2' C13 F1 127.8(6) . . ?
F2 C13 F1 109.4 . . ?
F2' C13 F3 71.3(4) . . ?
F2 C13 F3 109.4 . . ?
F1 C13 F3 109.4 . . ?
F2' C13 F1' 112.3(5) . . ?
F2 C13 F1' 83.3(4) . . ?
F1 C13 F1' 29.0(4) . . ?
F3 C13 F1' 132.4(6) . . ?
F2' C13 F3' 104.9(4) . . ?
F2 C13 F3' 137.7(5) . . ?
F1 C13 F3' 74.1(4) . . ?
F3 C13 F3' 38.6(4) . . ?
F1' C13 F3' 101.9(4) . . ?
F2' C13 C9 116.5(5) . . ?
F2 C13 C9 107.9(3) . . ?
F1 C13 C9 112.5(4) . . ?
F3 C13 C9 108.0(4) . . ?
F1' C13 C9 111.0(6) . . ?
F3' C13 C9 108.9(4) . . ?
F4' C14 F4 32.3(4) . . ?
F4' C14 F6 77.1(4) . . ?
F4 C14 F6 109.4 . . ?
F4' C14 F5 123.1(6) . . ?
F4 C14 F5 109.4 . . ?
F6 C14 F5 109.4 . . ?
F4' C14 F6' 111.6(5) . . ?
F4 C14 F6' 135.6(5) . . ?
F6 C14 F6' 48.1(4) . . ?
F5 C14 F6' 62.8(4) . . ?
F4' C14 F5' 104.5(5) . . ?
F4 C14 F5' 77.2(4) . . ?
F6 C14 F5' 146.1(5) . . ?
F5 C14 F5' 40.8(4) . . ?
F6' C14 F5' 103.2(4) . . ?
F4' C14 C11 117.2(6) . . ?
F4 C14 C11 108.6(5) . . ?
F6 C14 C11 104.4(6) . . ?
F5 C14 C11 115.3(5) . . ?
F6' C14 C11 113.9(5) . . ?
F5' C14 C11 104.6(5) . . ?
F9 C27 F8 109.1(4) . . ?
F9 C27 F7 105.3(4) . . ?
F8 C27 F7 103.4(4) . . ?
F9 C27 C23 113.8(4) . . ?
F8 C27 C23 113.3(4) . . ?
F7 C27 C23 111.2(4) . . ?
F12 C28 F10 107.4(3) . . ?
F12 C28 F11 105.6(4) . . ?
F10 C28 F11 105.0(3) . . ?
F12 C28 C25 112.8(3) . . ?
F10 C28 C25 113.0(4) . . ?
F11 C28 C25 112.5(3) . . ?
F14 C41 F15 105.8(5) . . ?
F14 C41 F13 104.5(5) . . ?
F15 C41 F13 103.5(5) . . ?
F14 C41 C37 114.3(4) . . ?
F15 C41 C37 114.5(4) . . ?
F13 C41 C37 113.2(4) . . ?
F17 C42 F16 106.6(4) . . ?
F17 C42 F18 105.3(4) . . ?
F16 C42 F18 106.1(4) . . ?
F17 C42 C39 112.5(4) . . ?
F16 C42 C39 112.3(4) . . ?
F18 C42 C39 113.4(4) . . ?
F21 C55 F20 107.1(3) . . ?
F21 C55 F19 106.2(3) . . ?
F20 C55 F19 105.8(3) . . ?
F21 C55 C51 112.6(3) . . ?
F20 C55 C51 113.0(3) . . ?
F19 C55 C51 111.7(3) . . ?
F24 C56 F22 111.3(5) . . ?
F24 C56 F23 103.5(5) . . ?
F22 C56 F23 100.3(4) . . ?
F24 C56 C53 114.9(4) . . ?
F22 C56 C53 114.5(4) . . ?
F23 C56 C53 110.8(4) . . ?
O1 K1 C61 139.75(10) . . ?
O1 K1 C62 158.93(10) . . ?
C61 K1 C62 25.00(11) . . ?
O1 K1 C60 131.64(10) . . ?
C61 K1 C60 25.02(11) . . ?
C62 K1 C60 43.74(11) . . ?
O1 K1 C17 91.38(9) . . ?
C61 K1 C17 86.12(12) . . ?
C62 K1 C17 75.98(11) . . ?
C60 K1 C17 110.88(12) . . ?
O1 K1 C3 84.40(9) . . ?
C61 K1 C3 131.68(11) . . ?
C62 K1 C3 116.32(11) . . ?
C60 K1 C3 117.62(11) . . ?
C17 K1 C3 117.69(12) . . ?
O1 K1 C4 104.41(10) . . ?
C61 K1 C4 115.26(12) . . ?
C62 K1 C4 94.99(12) . . ?
C60 K1 C4 110.79(12) . . ?
C17 K1 C4 103.34(13) . . ?
C3 K1 C4 24.09(11) . . ?
O1 K1 C59 137.97(11) . . ?
C61 K1 C59 43.00(11) . . ?
C62 K1 C59 49.66(11) . . ?
C60 K1 C59 24.31(11) . . ?
C17 K1 C59 125.45(11) . . ?
C3 K1 C59 93.51(11) . . ?
C4 K1 C59 87.50(12) . . ?
O1 K1 C2 62.30(9) . . ?
C61 K1 C2 155.82(10) . . ?
C62 K1 C2 137.08(11) . . ?
C60 K1 C2 139.29(11) . . ?
C17 K1 C2 105.98(11) . . ?
C3 K1 C2 24.19(9) . . ?
C4 K1 C2 42.23(11) . . ?
C59 K1 C2 116.22(11) . . ?
O1 K1 C57 176.66(10) . . ?
C61 K1 C57 43.41(11) . . ?
C62 K1 C57 24.32(10) . . ?
C60 K1 C57 50.41(11) . . ?
C17 K1 C57 89.95(11) . . ?
C3 K1 C57 92.27(11) . . ?
C4 K1 C57 72.30(11) . . ?
C59 K1 C57 42.33(11) . . ?
C2 K1 C57 114.39(10) . . ?
O1 K1 C16 68.06(9) . . ?
C61 K1 C16 107.79(11) . . ?
C62 K1 C16 100.08(11) . . ?
C60 K1 C16 131.13(11) . . ?
C17 K1 C16 24.13(10) . . ?
C3 K1 C16 107.45(11) . . ?
C4 K1 C16 102.44(11) . . ?
C59 K1 C16 149.27(11) . . ?
C2 K1 C16 89.06(10) . . ?
C57 K1 C16 112.89(11) . . ?
O1 K1 C5 102.60(10) . . ?
C61 K1 C5 116.35(12) . . ?
C62 K1 C5 91.83(11) . . ?
C60 K1 C5 122.79(12) . . ?
C17 K1 C5 79.79(12) . . ?
C3 K1 C5 41.78(12) . . ?
C4 K1 C5 23.69(12) . . ?
C59 K1 C5 103.30(12) . . ?
C2 K1 C5 48.32(11) . . ?
C57 K1 C5 74.63(11) . . ?
C16 K1 C5 79.91(11) . . ?
C58 C57 C62 117.5(4) . . ?
C58 C57 C63 121.6(4) . . ?
C62 C57 C63 120.9(4) . . ?
C58 C57 K1 79.5(2) . . ?
C62 C57 K1 71.9(2) . . ?
C63 C57 K1 118.9(3) . . ?
C59 C58 C57 121.2(4) . . ?
C59 C58 K1 75.5(3) . . ?
C57 C58 K1 76.8(2) . . ?
C60 C59 C58 120.4(4) . . ?
C60 C59 K1 73.2(3) . . ?
C58 C59 K1 80.8(3) . . ?
C61 C60 C59 119.1(4) . . ?
C61 C60 K1 75.0(2) . . ?
C59 C60 K1 82.5(3) . . ?
C60 C61 C62 120.4(4) . . ?
C60 C61 K1 80.0(2) . . ?
C62 C61 K1 80.0(2) . . ?
C61 C62 C57 121.4(4) . . ?
C61 C62 K1 75.0(2) . . ?
C57 C62 K1 83.8(2) . . ?
O2 K2 C66' 157.72(17) . . ?
O2 K2 C67 151.73(14) . . ?
C66' K2 C67 11.3(2) . . ?
O2 K2 C66 157.49(11) . . ?
C66' K2 C66 14.2(2) . . ?
C67 K2 C66 25.5 . . ?
O2 K2 C31 100.69(10) . . ?
C66' K2 C31 95.4(2) . . ?
C67 K2 C31 90.89(11) . . ?
C66 K2 C31 101.67(12) . . ?
O2 K2 C44 64.40(9) . . ?
C66' K2 C44 123.9(2) . . ?
C67 K2 C44 135.19(13) . . ?
C66 K2 C44 109.76(13) . . ?
C31 K2 C44 109.85(12) . . ?
O2 K2 C65' 141.9(2) . . ?
C66' K2 C65' 25.44(10) . . ?
C67 K2 C65' 35.0(2) . . ?
C66 K2 C65' 15.7(2) . . ?
C31 K2 C65' 117.4(2) . . ?
C44 K2 C65' 101.9(2) . . ?
O2 K2 C32 107.26(10) . . ?
C66' K2 C32 81.5(2) . . ?
C67 K2 C32 73.82(11) . . ?
C66 K2 C32 92.13(13) . . ?
C31 K2 C32 24.93(12) . . ?
C44 K2 C32 134.64(12) . . ?
C65' K2 C32 106.7(2) . . ?
O2 K2 C43 64.56(9) . . ?
C66' K2 C43 132.8(2) . . ?
C67 K2 C43 142.84(14) . . ?
C66 K2 C43 120.11(12) . . ?
C31 K2 C43 85.01(11) . . ?
C44 K2 C43 25.08(10) . . ?
C65' K2 C43 118.17(19) . . ?
C32 K2 C43 109.63(11) . . ?
O2 K2 C68 126.55(13) . . ?
C66' K2 C68 33.13(18) . . ?
C67 K2 C68 25.2 . . ?
C66 K2 C68 44.39(6) . . ?
C31 K2 C68 103.26(14) . . ?
C44 K2 C68 142.31(12) . . ?
C65' K2 C68 45.10(19) . . ?
C32 K2 C68 80.36(13) . . ?
C43 K2 C68 163.26(11) . . ?
O2 K2 C67' 137.3(2) . . ?
C66' K2 C67' 25.19(8) . . ?
C67 K2 C67' 14.89(18) . . ?
C66 K2 C67' 38.61(17) . . ?
C31 K2 C67' 93.05(17) . . ?
C44 K2 C67' 145.85(19) . . ?
C65' K2 C67' 44.09(12) . . ?
C32 K2 C67' 71.84(17) . . ?
C43 K2 C67' 157.7(2) . . ?
C68 K2 C67' 12.61(18) . . ?
O2 K2 C45 86.70(11) . . ?
C66' K2 C45 99.0(3) . . ?
C67 K2 C45 110.25(14) . . ?
C66 K2 C45 84.88(14) . . ?
C31 K2 C45 118.83(13) . . ?
C44 K2 C45 24.97(11) . . ?
C65' K2 C45 77.2(2) . . ?
C32 K2 C45 141.61(14) . . ?
C43 K2 C45 43.95(10) . . ?
C68 K2 C45 120.22(12) . . ?
C67' K2 C45 121.3(2) . . ?
C65 C64 C69 120.0 . . ?
C65 C64 C70 120.0 . . ?
C69 C64 C70 120.0 . . ?
C65 C64 K2 75.1(2) . . ?
C69 C64 K2 77.1(2) . . ?
C70 C64 K2 118.69(16) . . ?
C64 C65 C66 120.0 . . ?
C64 C65 K2 80.5(2) . . ?
C66 C65 K2 73.99(18) . . ?
C65 C66 C67 120.0 . . ?
C65 C66 K2 81.0(2) . . ?
C67 C66 K2 76.5(2) . . ?
C68 C67 C66 120.0 . . ?
C68 C67 K2 80.1(2) . . ?
C66 C67 K2 78.1(2) . . ?
C67 C68 C69 120.0 . . ?
C67 C68 K2 74.6(2) . . ?
C69 C68 K2 81.16(19) . . ?
C64 C69 C68 120.0 . . ?
C64 C69 K2 78.6(2) . . ?
C68 C69 K2 74.22(18) . . ?
C69' C64' C65' 120.0 . . ?
C69' C64' C70' 120.0 . . ?
C65' C64' C70' 120.0 . . ?
C69' C64' K2 82.1(4) . . ?
C65' C64' K2 71.5(5) . . ?
C70' C64' K2 117.0(3) . . ?
C64' C65' C66' 120.0 . . ?
C64' C65' K2 84.0(5) . . ?
C66' C65' K2 75.0(4) . . ?
C67' C66' C65' 120.0 . . ?
C67' C66' K2 81.6(4) . . ?
C65' C66' K2 79.5(4) . . ?
C66' C67' C68' 120.0 . . ?
C66' C67' K2 73.2(5) . . ?
C68' C67' K2 84.1(5) . . ?
C67' C68' C69' 120.0 . . ?
C67' C68' K2 71.8(4) . . ?
C69' C68' K2 80.3(3) . . ?
C64' C69' C68' 120.0 . . ?
C64' C69' K2 74.2(4) . . ?
C68' C69' K2 76.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.472
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.089
_database_code_depnum_ccdc_archive 'CCDC 965032'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_cmpd4crown

_audit_creation_method           SHELXL-97

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C88 H100 F24 K2 N4 O18 U'
_chemical_formula_weight         2273.95

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'
F F 0.0171 0.0103 '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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c     '
_symmetry_Int_Tables_number      14

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

_cell_length_a                   14.2737(4)
_cell_length_b                   22.2064(7)
_cell_length_c                   32.9180(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.921(2)
_cell_angle_gamma                90.00
_cell_volume                     10378.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    143(1)
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05

_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4584
_exptl_absorpt_coefficient_mu    1.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_absorpt_correction_T_min  0.5977
_exptl_absorpt_correction_T_max  0.7456
_diffrn_ambient_temperature      143(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            157248
_diffrn_reflns_av_R_equivalents  0.1032
_diffrn_reflns_av_sigmaI/netI    0.0970
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         1.43
_diffrn_reflns_theta_max         27.62
_reflns_number_total             23936
_reflns_number_gt                14382
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_refine_special_details          
;
The data were corrected for the presence of disordered solvent using the
program SQUEEZE.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0892P)²+12.4805P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         23936
_refine_ls_number_parameters     1238
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0676
_refine_ls_wR_factor_ref         0.1822
_refine_ls_wR_factor_gt          0.1636
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.263239(17) 0.290791(11) 0.362877(7) 0.03376(9) Uani 1 1 d . . .
K2 K 0.26807(11) -0.28201(7) 0.46029(5) 0.0458(4) Uani 1 1 d . . .
K1 K 0.21004(12) -0.12671(7) 0.30713(5) 0.0480(4) Uani 1 1 d . . .
F1 F 0.4522(6) 0.0344(4) 0.4502(4) 0.194(5) Uani 1 1 d . . .
F2 F 0.4620(5) 0.0879(5) 0.5001(2) 0.155(4) Uani 1 1 d . . .
F3 F 0.4914(4) 0.1251(4) 0.4454(3) 0.166(4) Uani 1 1 d . . .
F4 F 0.0804(7) 0.0851(4) 0.5191(2) 0.149(4) Uani 1 1 d . . .
F5 F 0.0207(6) 0.0506(4) 0.4657(3) 0.160(4) Uani 1 1 d . . .
F6 F 0.1255(6) 0.0018(3) 0.4975(3) 0.147(3) Uani 1 1 d . . .
F7 F 0.2660(4) 0.5036(3) 0.52630(18) 0.0917(18) Uani 1 1 d . . .
F8 F 0.1221(4) 0.4881(2) 0.53110(16) 0.0787(15) Uani 1 1 d . . .
F9 F 0.2264(5) 0.4577(3) 0.57803(16) 0.106(2) Uani 1 1 d . . .
F10 F 0.3051(6) 0.2471(3) 0.57343(17) 0.115(2) Uani 1 1 d . . .
F11 F 0.3340(6) 0.2099(3) 0.5181(2) 0.119(3) Uani 1 1 d . . .
F12 F 0.1997(5) 0.2036(3) 0.5347(3) 0.134(3) Uani 1 1 d . . .
F13 F 0.3124(5) 0.5798(2) 0.27347(19) 0.106(2) Uani 1 1 d . . .
F14 F 0.3748(6) 0.5635(3) 0.2203(2) 0.130(3) Uani 1 1 d . . .
F15 F 0.2303(6) 0.5635(3) 0.2183(3) 0.165(4) Uani 1 1 d . . .
F16 F 0.3376(6) 0.3030(4) 0.1854(3) 0.163(4) Uani 1 1 d . . .
F17 F 0.2306(7) 0.3589(3) 0.1583(2) 0.158(4) Uani 1 1 d . . .
F18 F 0.2034(7) 0.2955(3) 0.1990(2) 0.140(3) Uani 1 1 d . . .
F19 F 0.4991(4) 0.1460(3) 0.19999(17) 0.0952(19) Uani 1 1 d . . .
F20 F 0.4407(5) 0.0606(3) 0.2057(2) 0.119(3) Uani 1 1 d . . .
F21 F 0.3853(4) 0.1182(4) 0.15759(17) 0.112(2) Uani 1 1 d . . .
F22 F 0.0659(5) 0.1453(4) 0.1859(2) 0.146(3) Uani 1 1 d . . .
F23 F 0.0548(5) 0.1019(3) 0.2402(3) 0.145(4) Uani 1 1 d . . .
F24 F 0.0358(4) 0.1932(3) 0.2394(2) 0.106(2) Uani 1 1 d . . .
O1 O 0.3541(3) 0.28142(18) 0.40405(13) 0.0345(10) Uani 1 1 d . . .
O2 O 0.1716(3) 0.30144(18) 0.32206(13) 0.0330(10) Uani 1 1 d . . .
O3 O 0.3576(5) -0.0419(3) 0.3000(2) 0.092(2) Uani 1 1 d . . .
O4 O 0.2028(6) -0.0098(3) 0.3395(2) 0.093(2) Uani 1 1 d . . .
O5 O 0.1151(5) -0.1049(3) 0.37752(18) 0.0730(17) Uani 1 1 d . . .
O6 O 0.1113(4) -0.2189(3) 0.34145(17) 0.0626(15) Uani 1 1 d . . .
O7 O 0.2659(4) -0.2486(3) 0.29881(17) 0.0619(15) Uani 1 1 d . . .
O8 O 0.3745(4) -0.1570(3) 0.2673(2) 0.0718(17) Uani 1 1 d . . .
O9 O 0.0179(4) -0.0970(3) 0.28048(18) 0.0695(17) Uani 1 1 d . . .
O10 O 0.1383(4) -0.1474(3) 0.22815(18) 0.0722(17) Uani 1 1 d . . .
O11 O 0.3852(4) -0.2430(3) 0.39850(18) 0.0708(17) Uani 1 1 d . . .
O12 O 0.3292(4) -0.1630(3) 0.45781(19) 0.0694(16) Uani 1 1 d . . .
O13 O 0.1604(5) -0.1853(3) 0.4914(2) 0.085(2) Uani 1 1 d . . .
O14 O 0.0862(5) -0.3003(4) 0.4874(2) 0.094(2) Uani 1 1 d . . .
O15 O 0.1515(5) -0.3802(3) 0.4309(2) 0.082(2) Uani 1 1 d . . .
O16 O 0.3285(5) -0.3618(3) 0.40419(18) 0.0760(18) Uani 1 1 d . . .
O17 O 0.4550(5) -0.3105(4) 0.4868(2) 0.105(3) Uani 1 1 d . . .
O18 O 0.3172(5) -0.3167(4) 0.5392(2) 0.114(3) Uani 1 1 d . . .
N1 N 0.1793(4) 0.2033(2) 0.38385(17) 0.0387(13) Uani 1 1 d . . .
N2 N 0.1775(4) 0.3520(2) 0.40888(16) 0.0403(13) Uani 1 1 d . . .
N3 N 0.3449(4) 0.3775(2) 0.33747(17) 0.0386(13) Uani 1 1 d . . .
N4 N 0.3493(4) 0.2240(2) 0.32131(17) 0.0369(13) Uani 1 1 d . . .
C1 C 0.0813(5) 0.2001(3) 0.3691(2) 0.0453(17) Uani 1 1 d . . .
C2 C 0.0516(6) 0.1566(4) 0.3409(3) 0.071(3) Uani 1 1 d . . .
H2 H 0.0940 0.1270 0.3329 0.085 Uiso 1 1 calc R . .
C3 C -0.0411(7) 0.1572(6) 0.3245(3) 0.105(4) Uani 1 1 d . . .
H3 H -0.0593 0.1305 0.3026 0.126 Uiso 1 1 calc R . .
C4 C -0.1064(7) 0.1926(6) 0.3375(3) 0.091(3) Uani 1 1 d . . .
H4 H -0.1709 0.1882 0.3274 0.109 Uiso 1 1 calc R . .
C5 C -0.0780(6) 0.2365(5) 0.3661(3) 0.073(3) Uani 1 1 d . . .
H5 H -0.1226 0.2639 0.3752 0.088 Uiso 1 1 calc R . .
C6 C 0.0187(5) 0.2400(4) 0.3819(2) 0.0512(19) Uani 1 1 d . . .
H6 H 0.0391 0.2702 0.4012 0.061 Uiso 1 1 calc R . .
C7 C 0.2084(4) 0.1619(3) 0.4132(2) 0.0339(14) Uani 1 1 d . . .
C8 C 0.3043(5) 0.1476(3) 0.4229(2) 0.0403(16) Uani 1 1 d . . .
H8 H 0.3508 0.1675 0.4091 0.048 Uiso 1 1 calc R . .
C9 C 0.3312(6) 0.1047(3) 0.4522(2) 0.0520(19) Uani 1 1 d . . .
C10 C 0.2702(6) 0.0737(4) 0.4741(2) 0.059(2) Uani 1 1 d . . .
H10 H 0.2911 0.0444 0.4940 0.071 Uiso 1 1 calc R . .
C11 C 0.1746(6) 0.0885(3) 0.4651(2) 0.053(2) Uani 1 1 d . . .
C12 C 0.1436(6) 0.1306(3) 0.4353(2) 0.0510(19) Uani 1 1 d . . .
H12 H 0.0781 0.1383 0.4297 0.061 Uiso 1 1 calc R . .
C13 C 0.4339(7) 0.0895(5) 0.4612(3) 0.076(3) Uani 1 1 d . . .
C14 C 0.1009(9) 0.0575(5) 0.4875(3) 0.082(3) Uani 1 1 d . . .
C15 C 0.1153(5) 0.3972(3) 0.3921(2) 0.0430(17) Uani 1 1 d . . .
C16 C 0.0254(6) 0.4048(4) 0.4063(2) 0.059(2) Uani 1 1 d . . .
H16 H 0.0067 0.3788 0.4269 0.071 Uiso 1 1 calc R . .
C17 C -0.0356(6) 0.4495(4) 0.3904(3) 0.067(3) Uani 1 1 d . . .
H17 H -0.0957 0.4536 0.4001 0.081 Uiso 1 1 calc R . .
C18 C -0.0097(7) 0.4881(4) 0.3606(3) 0.074(3) Uani 1 1 d . . .
H18 H -0.0508 0.5198 0.3508 0.089 Uiso 1 1 calc R . .
C19 C 0.0765(6) 0.4808(3) 0.3447(2) 0.055(2) Uani 1 1 d . . .
H19 H 0.0937 0.5061 0.3234 0.066 Uiso 1 1 calc R . .
C20 C 0.1362(5) 0.4362(3) 0.3607(2) 0.0476(18) Uani 1 1 d . . .
H20 H 0.1949 0.4314 0.3498 0.057 Uiso 1 1 calc R . .
C21 C 0.1954(5) 0.3520(3) 0.4506(2) 0.0378(15) Uani 1 1 d . . .
C22 C 0.1899(5) 0.4045(3) 0.4739(2) 0.0473(18) Uani 1 1 d . . .
H22 H 0.1696 0.4410 0.4609 0.057 Uiso 1 1 calc R . .
C23 C 0.2140(5) 0.4036(4) 0.5161(2) 0.0485(18) Uani 1 1 d . . .
C24 C 0.2408(5) 0.3509(3) 0.5365(2) 0.0467(18) Uani 1 1 d . . .
H24 H 0.2558 0.3507 0.5653 0.056 Uiso 1 1 calc R . .
C25 C 0.2452(5) 0.2991(3) 0.5143(2) 0.0467(18) Uani 1 1 d . . .
C26 C 0.2220(5) 0.2996(3) 0.4714(2) 0.0401(16) Uani 1 1 d . . .
H26 H 0.2248 0.2630 0.4566 0.048 Uiso 1 1 calc R . .
C27 C 0.2076(7) 0.4613(4) 0.5385(3) 0.067(2) Uani 1 1 d . . .
C28 C 0.2701(7) 0.2408(4) 0.5350(3) 0.063(2) Uani 1 1 d . . .
C29 C 0.4055(5) 0.4138(3) 0.3644(2) 0.0457(18) Uani 1 1 d . . .
C30 C 0.3814(6) 0.4295(3) 0.4028(3) 0.056(2) Uani 1 1 d . . .
H30 H 0.3239 0.4146 0.4111 0.067 Uiso 1 1 calc R . .
C31 C 0.4374(7) 0.4659(4) 0.4295(3) 0.076(3) Uani 1 1 d . . .
H31 H 0.4192 0.4759 0.4556 0.091 Uiso 1 1 calc R . .
C32 C 0.5218(7) 0.4875(4) 0.4166(4) 0.081(3) Uani 1 1 d . . .
H32 H 0.5610 0.5132 0.4341 0.097 Uiso 1 1 calc R . .
C33 C 0.5479(7) 0.4721(4) 0.3795(3) 0.084(3) Uani 1 1 d . . .
H33 H 0.6056 0.4868 0.3713 0.101 Uiso 1 1 calc R . .
C34 C 0.4904(6) 0.4345(4) 0.3530(3) 0.072(3) Uani 1 1 d . . .
H34 H 0.5099 0.4235 0.3273 0.086 Uiso 1 1 calc R . .
C35 C 0.3279(5) 0.3980(3) 0.2984(2) 0.0418(16) Uani 1 1 d . . .
C36 C 0.3257(5) 0.4599(3) 0.2887(2) 0.0467(18) Uani 1 1 d . . .
H36 H 0.3389 0.4883 0.3101 0.056 Uiso 1 1 calc R . .
C37 C 0.3049(6) 0.4806(3) 0.2494(2) 0.0509(19) Uani 1 1 d . . .
C38 C 0.2845(5) 0.4417(3) 0.2169(2) 0.0512(19) Uani 1 1 d . . .
H38 H 0.2702 0.4561 0.1898 0.061 Uiso 1 1 calc R . .
C39 C 0.2860(5) 0.3799(4) 0.2261(2) 0.0516(19) Uani 1 1 d . . .
C40 C 0.3069(5) 0.3587(3) 0.2649(2) 0.0416(16) Uani 1 1 d . . .
H40 H 0.3074 0.3164 0.2695 0.050 Uiso 1 1 calc R . .
C41 C 0.3010(7) 0.5467(4) 0.2417(3) 0.068(3) Uani 1 1 d . . .
C42 C 0.2676(8) 0.3355(4) 0.1921(3) 0.068(2) Uani 1 1 d . . .
C43 C 0.4469(5) 0.2193(3) 0.3340(2) 0.0418(16) Uani 1 1 d . . .
C44 C 0.5068(5) 0.2676(4) 0.3312(3) 0.058(2) Uani 1 1 d . . .
H44 H 0.4827 0.3051 0.3209 0.070 Uiso 1 1 calc R . .
C45 C 0.6034(6) 0.2611(5) 0.3435(3) 0.072(3) Uani 1 1 d . . .
H45 H 0.6442 0.2945 0.3413 0.086 Uiso 1 1 calc R . .
C46 C 0.6393(6) 0.2090(5) 0.3584(3) 0.075(3) Uani 1 1 d . . .
H46 H 0.7046 0.2059 0.3672 0.091 Uiso 1 1 calc R . .
C47 C 0.5806(6) 0.1594(5) 0.3611(3) 0.072(3) Uani 1 1 d . . .
H47 H 0.6063 0.1222 0.3712 0.087 Uiso 1 1 calc R . .
C48 C 0.4862(5) 0.1640(4) 0.3493(2) 0.0509(19) Uani 1 1 d . . .
H48 H 0.4466 0.1300 0.3513 0.061 Uiso 1 1 calc R . .
C49 C 0.3183(5) 0.1931(3) 0.2865(2) 0.0359(15) Uani 1 1 d . . .
C50 C 0.3801(5) 0.1696(3) 0.2593(2) 0.0438(17) Uani 1 1 d . . .
H50 H 0.4461 0.1730 0.2663 0.053 Uiso 1 1 calc R . .
C51 C 0.3475(6) 0.1420(3) 0.2233(2) 0.0485(18) Uani 1 1 d . . .
C52 C 0.2543(7) 0.1345(4) 0.2116(3) 0.065(2) Uani 1 1 d . . .
H52 H 0.2333 0.1137 0.1871 0.078 Uiso 1 1 calc R . .
C53 C 0.1902(6) 0.1580(4) 0.2366(3) 0.056(2) Uani 1 1 d . . .
C54 C 0.2225(5) 0.1862(3) 0.2737(2) 0.0473(18) Uani 1 1 d . . .
H54 H 0.1776 0.2009 0.2906 0.057 Uiso 1 1 calc R . .
C55 C 0.4163(7) 0.1155(4) 0.1970(3) 0.066(2) Uani 1 1 d . . .
C56 C 0.0867(7) 0.1523(6) 0.2260(4) 0.095(4) Uani 1 1 d . . .
C57 C 0.3185(10) 0.0160(5) 0.2982(5) 0.123(5) Uani 1 1 d . . .
H57a H 0.2693 0.0189 0.2748 0.147 Uiso 1 1 calc R . .
H57b H 0.3680 0.0461 0.2942 0.147 Uiso 1 1 calc R . .
C58 C 0.2751(10) 0.0294(5) 0.3384(5) 0.117(5) Uani 1 1 d . . .
H58a H 0.3224 0.0235 0.3622 0.140 Uiso 1 1 calc R . .
H58b H 0.2520 0.0715 0.3386 0.140 Uiso 1 1 calc R . .
C59 C 0.1670(12) -0.0047(5) 0.3772(3) 0.117(5) Uani 1 1 d . . .
H59a H 0.1492 0.0377 0.3818 0.140 Uiso 1 1 calc R . .
H59b H 0.2160 -0.0164 0.3993 0.140 Uiso 1 1 calc R . .
C60 C 0.0802(10) -0.0456(6) 0.3782(3) 0.106(4) Uani 1 1 d . . .
H60a H 0.0492 -0.0384 0.4033 0.127 Uiso 1 1 calc R . .
H60b H 0.0341 -0.0380 0.3541 0.127 Uiso 1 1 calc R . .
C61 C 0.0392(8) -0.1457(6) 0.3799(3) 0.091(3) Uani 1 1 d . . .
H61a H -0.0093 -0.1393 0.3565 0.110 Uiso 1 1 calc R . .
H61b H 0.0098 -0.1389 0.4054 0.110 Uiso 1 1 calc R . .
C62 C 0.0763(8) -0.2076(5) 0.3790(3) 0.085(3) Uani 1 1 d . . .
H62a H 0.1273 -0.2130 0.4015 0.102 Uiso 1 1 calc R . .
H62b H 0.0256 -0.2367 0.3831 0.102 Uiso 1 1 calc R . .
C63 C 0.1454(7) -0.2782(3) 0.3380(3) 0.064(2) Uani 1 1 d . . .
H63a H 0.0934 -0.3074 0.3397 0.077 Uiso 1 1 calc R . .
H63b H 0.1948 -0.2866 0.3607 0.077 Uiso 1 1 calc R . .
C64 C 0.1852(7) -0.2848(4) 0.2980(3) 0.071(3) Uani 1 1 d . . .
H64a H 0.2018 -0.3275 0.2935 0.085 Uiso 1 1 calc R . .
H64b H 0.1381 -0.2721 0.2754 0.085 Uiso 1 1 calc R . .
C65 C 0.3151(7) -0.2567(4) 0.2642(3) 0.068(3) Uani 1 1 d . . .
H65a H 0.2752 -0.2448 0.2391 0.082 Uiso 1 1 calc R . .
H65b H 0.3334 -0.2995 0.2616 0.082 Uiso 1 1 calc R . .
C66 C 0.4033(8) -0.2165(5) 0.2706(3) 0.083(3) Uani 1 1 d . . .
H66a H 0.4373 -0.2239 0.2978 0.100 Uiso 1 1 calc R . .
H66b H 0.4464 -0.2256 0.2496 0.100 Uiso 1 1 calc R . .
C67 C 0.4505(7) -0.1185(5) 0.2734(4) 0.087(3) Uani 1 1 d . . .
H67a H 0.4960 -0.1276 0.2535 0.104 Uiso 1 1 calc R . .
H67b H 0.4826 -0.1242 0.3013 0.104 Uiso 1 1 calc R . .
C68 C 0.4175(9) -0.0545(6) 0.2682(4) 0.105(4) Uani 1 1 d . . .
H68a H 0.4721 -0.0268 0.2705 0.126 Uiso 1 1 calc R . .
H68b H 0.3820 -0.0491 0.2410 0.126 Uiso 1 1 calc R . .
C69 C -0.0122(9) -0.0398(5) 0.2653(4) 0.110(4) Uani 1 1 d . . .
H69a H 0.0126 -0.0326 0.2391 0.165 Uiso 1 1 calc R . .
H69b H 0.0110 -0.0086 0.2848 0.165 Uiso 1 1 calc R . .
H69c H -0.0812 -0.0387 0.2615 0.165 Uiso 1 1 calc R . .
C70 C -0.0100(6) -0.1481(4) 0.2546(3) 0.064(2) Uani 1 1 d . . .
H70a H -0.0789 -0.1469 0.2470 0.076 Uiso 1 1 calc R . .
H70b H 0.0050 -0.1859 0.2699 0.076 Uiso 1 1 calc R . .
C71 C 0.0398(6) -0.1478(4) 0.2165(3) 0.070(3) Uani 1 1 d . . .
H71a H 0.0222 -0.1839 0.1999 0.084 Uiso 1 1 calc R . .
H71b H 0.0215 -0.1116 0.2000 0.084 Uiso 1 1 calc R . .
C72 C 0.1908(7) -0.1304(6) 0.1945(3) 0.092(3) Uani 1 1 d . . .
H72a H 0.1926 -0.1644 0.1756 0.138 Uiso 1 1 calc R . .
H72b H 0.2553 -0.1195 0.2051 0.138 Uiso 1 1 calc R . .
H72c H 0.1602 -0.0960 0.1801 0.138 Uiso 1 1 calc R . .
C73 C 0.4371(7) -0.1904(5) 0.4110(3) 0.086(3) Uani 1 1 d . . .
H73a H 0.4707 -0.1753 0.3882 0.103 Uiso 1 1 calc R . .
H73b H 0.4845 -0.2001 0.4342 0.103 Uiso 1 1 calc R . .
C74 C 0.3731(8) -0.1446(5) 0.4231(4) 0.089(3) Uani 1 1 d . . .
H74a H 0.4084 -0.1068 0.4295 0.107 Uiso 1 1 calc R . .
H74b H 0.3243 -0.1364 0.4002 0.107 Uiso 1 1 calc R . .
C75 C 0.2735(9) -0.1161(4) 0.4750(3) 0.091(4) Uani 1 1 d . . .
H75a H 0.3151 -0.0826 0.4852 0.109 Uiso 1 1 calc R . .
H75b H 0.2263 -0.1002 0.4535 0.109 Uiso 1 1 calc R . .
C76 C 0.2277(11) -0.1401(6) 0.5071(4) 0.116(5) Uani 1 1 d . . .
H76a H 0.1948 -0.1075 0.5204 0.140 Uiso 1 1 calc R . .
H76b H 0.2746 -0.1583 0.5277 0.140 Uiso 1 1 calc R . .
C77 C 0.1050(11) -0.2070(7) 0.5204(4) 0.119(5) Uani 1 1 d . . .
H77a H 0.0724 -0.1734 0.5328 0.142 Uiso 1 1 calc R . .
H77b H 0.1444 -0.2285 0.5424 0.142 Uiso 1 1 calc R . .
C78 C 0.0355(9) -0.2487(8) 0.4990(4) 0.118(5) Uani 1 1 d . . .
H78a H -0.0122 -0.2607 0.5173 0.142 Uiso 1 1 calc R . .
H78b H 0.0028 -0.2290 0.4745 0.142 Uiso 1 1 calc R . .
C79 C 0.0283(9) -0.3396(8) 0.4663(4) 0.115(5) Uani 1 1 d . . .
H79a H 0.0013 -0.3210 0.4404 0.138 Uiso 1 1 calc R . .
H79b H -0.0242 -0.3504 0.4824 0.138 Uiso 1 1 calc R . .
C80 C 0.0826(11) -0.3952(7) 0.4574(4) 0.126(6) Uani 1 1 d . . .
H80a H 0.1136 -0.4121 0.4832 0.151 Uiso 1 1 calc R . .
H80b H 0.0391 -0.4260 0.4445 0.151 Uiso 1 1 calc R . .
C81 C 0.2115(10) -0.4295(5) 0.4233(3) 0.104(4) Uani 1 1 d . . .
H81a H 0.1730 -0.4652 0.4145 0.124 Uiso 1 1 calc R . .
H81b H 0.2517 -0.4400 0.4486 0.124 Uiso 1 1 calc R . .
C82 C 0.2704(9) -0.4125(4) 0.3914(3) 0.098(4) Uani 1 1 d . . .
H82a H 0.3108 -0.4470 0.3853 0.117 Uiso 1 1 calc R . .
H82b H 0.2299 -0.4022 0.3661 0.117 Uiso 1 1 calc R . .
C83 C 0.3912(8) -0.3429(5) 0.3742(3) 0.085(3) Uani 1 1 d . . .
H83a H 0.3539 -0.3323 0.3482 0.102 Uiso 1 1 calc R . .
H83b H 0.4343 -0.3763 0.3689 0.102 Uiso 1 1 calc R . .
C84 C 0.4457(7) -0.2907(5) 0.3902(3) 0.086(3) Uani 1 1 d . . .
H84a H 0.4850 -0.3021 0.4156 0.103 Uiso 1 1 calc R . .
H84b H 0.4881 -0.2773 0.3700 0.103 Uiso 1 1 calc R . .
C85 C 0.4970(11) -0.3733(7) 0.4864(5) 0.157(7) Uani 1 1 d . . .
H85a H 0.5611 -0.3727 0.5002 0.236 Uiso 1 1 calc R . .
H85b H 0.4987 -0.3866 0.4581 0.236 Uiso 1 1 calc R . .
H85c H 0.4582 -0.4012 0.5006 0.236 Uiso 1 1 calc R . .
C86 C 0.4685(9) -0.2804(9) 0.5226(3) 0.154(8) Uani 1 1 d . . .
H86a H 0.4428 -0.2391 0.5191 0.185 Uiso 1 1 calc R . .
H86b H 0.5367 -0.2774 0.5315 0.185 Uiso 1 1 calc R . .
C87 C 0.4186(8) -0.3140(7) 0.5549(3) 0.124(5) Uani 1 1 d . . .
H87a H 0.4446 -0.3552 0.5589 0.149 Uiso 1 1 calc R . .
H87b H 0.4270 -0.2924 0.5813 0.149 Uiso 1 1 calc R . .
C88 C 0.2606(8) -0.3473(5) 0.5649(3) 0.096(4) Uani 1 1 d . . .
H88a H 0.2765 -0.3902 0.5653 0.145 Uiso 1 1 calc R . .
H88b H 0.1942 -0.3421 0.5547 0.145 Uiso 1 1 calc R . .
H88c H 0.2717 -0.3309 0.5926 0.145 Uiso 1 1 calc R . .


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
U1 O1 1.789(4) . ?
U1 O2 1.792(4) . ?
U1 N1 2.420(5) . ?
U1 N4 2.434(5) . ?
U1 N3 2.442(5) . ?
U1 N2 2.453(5) . ?
K2 O18 2.731(7) . ?
K2 O16 2.761(6) . ?
K2 O12 2.788(6) . ?
K2 O17 2.792(7) . ?
K2 O15 2.851(6) . ?
K2 O14 2.860(7) . ?
K2 O13 2.889(7) . ?
K2 O11 2.895(6) . ?
K2 C86 3.344(12) . ?
K1 O10 2.733(6) . ?
K1 O6 2.790(6) . ?
K1 O4 2.812(6) . ?
K1 O7 2.843(6) . ?
K1 O5 2.844(6) . ?
K1 O3 2.852(7) . ?
K1 O9 2.869(6) . ?
K1 O8 2.883(6) . ?
K1 C70 3.459(9) . ?
K1 C64 3.539(8) . ?
F1 C13 1.311(12) . ?
F2 C13 1.303(11) . ?
F3 C13 1.287(11) . ?
F4 C14 1.268(12) . ?
F5 C14 1.296(12) . ?
F6 C14 1.318(12) . ?
F7 C27 1.343(10) . ?
F8 C27 1.356(10) . ?
F9 C27 1.305(10) . ?
F10 C28 1.319(10) . ?
F11 C28 1.311(11) . ?
F12 C28 1.299(11) . ?
F13 C41 1.275(10) . ?
F14 C41 1.377(11) . ?
F15 C41 1.261(10) . ?
F16 C42 1.271(11) . ?
F17 C42 1.291(11) . ?
F18 C42 1.312(11) . ?
F19 C55 1.356(10) . ?
F20 C55 1.291(11) . ?
F21 C55 1.330(10) . ?
F22 C56 1.333(13) . ?
F23 C56 1.311(15) . ?
F24 C56 1.272(11) . ?
O3 C57 1.402(13) . ?
O3 C68 1.446(13) . ?
O4 C58 1.355(14) . ?
O4 C59 1.395(13) . ?
O5 C60 1.409(12) . ?
O5 C61 1.420(13) . ?
O6 C62 1.402(11) . ?
O6 C63 1.413(9) . ?
O7 C64 1.403(10) . ?
O7 C65 1.411(10) . ?
O8 C67 1.379(11) . ?
O8 C66 1.384(11) . ?
O9 C69 1.415(11) . ?
O9 C70 1.450(10) . ?
O10 C71 1.419(10) . ?
O10 C72 1.449(11) . ?
O11 C84 1.410(11) . ?
O11 C73 1.421(12) . ?
O12 C74 1.419(12) . ?
O12 C75 1.457(12) . ?
O13 C77 1.387(13) . ?
O13 C76 1.448(14) . ?
O14 C79 1.345(14) . ?
O14 C78 1.426(15) . ?
O15 C80 1.421(14) . ?
O15 C81 1.426(13) . ?
O16 C82 1.436(12) . ?
O16 C83 1.460(12) . ?
O17 C86 1.352(13) . ?
O17 C85 1.520(15) . ?
O18 C88 1.403(12) . ?
O18 C87 1.486(13) . ?
N1 C7 1.367(8) . ?
N1 C1 1.434(9) . ?
N2 C21 1.371(8) . ?
N2 C15 1.415(9) . ?
N3 C35 1.364(8) . ?
N3 C29 1.424(9) . ?
N4 C49 1.370(8) . ?
N4 C43 1.416(8) . ?
C1 C6 1.356(10) . ?
C1 C2 1.375(11) . ?
C2 C3 1.377(13) . ?
C3 C4 1.323(15) . ?
C4 C5 1.387(15) . ?
C5 C6 1.425(11) . ?
C7 C8 1.410(9) . ?
C7 C12 1.416(9) . ?
C8 C9 1.381(10) . ?
C9 C10 1.373(11) . ?
C9 C13 1.504(12) . ?
C10 C11 1.405(11) . ?
C11 C12 1.394(11) . ?
C11 C14 1.511(12) . ?
C15 C20 1.405(10) . ?
C15 C16 1.419(11) . ?
C16 C17 1.387(11) . ?
C17 C18 1.382(13) . ?
C18 C19 1.395(13) . ?
C19 C20 1.375(10) . ?
C21 C26 1.384(9) . ?
C21 C22 1.401(9) . ?
C22 C23 1.396(10) . ?
C23 C24 1.384(10) . ?
C23 C27 1.484(11) . ?
C24 C25 1.368(10) . ?
C25 C26 1.415(10) . ?
C25 C28 1.490(11) . ?
C29 C34 1.385(11) . ?
C29 C30 1.387(11) . ?
C30 C31 1.385(11) . ?
C31 C32 1.402(14) . ?
C32 C33 1.358(15) . ?
C33 C34 1.408(12) . ?
C35 C36 1.409(9) . ?
C35 C40 1.415(10) . ?
C36 C37 1.377(10) . ?
C37 C38 1.380(11) . ?
C37 C41 1.489(11) . ?
C38 C39 1.406(10) . ?
C39 C40 1.365(10) . ?
C39 C42 1.492(11) . ?
C43 C44 1.380(10) . ?
C43 C48 1.420(10) . ?
C44 C45 1.404(12) . ?
C45 C46 1.338(13) . ?
C46 C47 1.392(13) . ?
C47 C48 1.368(11) . ?
C49 C54 1.397(9) . ?
C49 C50 1.419(9) . ?
C50 C51 1.373(10) . ?
C51 C52 1.356(11) . ?
C51 C55 1.494(11) . ?
C52 C53 1.394(12) . ?
C53 C54 1.407(10) . ?
C53 C56 1.487(12) . ?
C57 C58 1.545(18) . ?
C59 C60 1.540(17) . ?
C61 C62 1.476(14) . ?
C63 C64 1.496(13) . ?
C65 C66 1.541(14) . ?
C67 C68 1.501(15) . ?
C70 C71 1.503(12) . ?
C73 C74 1.451(15) . ?
C75 C76 1.403(16) . ?
C77 C78 1.483(19) . ?
C79 C80 1.503(19) . ?
C81 C82 1.462(16) . ?
C83 C84 1.464(14) . ?
C86 C87 1.533(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 178.94(19) . . ?
O1 U1 N1 91.84(18) . . ?
O2 U1 N1 88.57(18) . . ?
O1 U1 N4 89.24(19) . . ?
O2 U1 N4 91.76(18) . . ?
N1 U1 N4 87.99(19) . . ?
O1 U1 N3 90.97(18) . . ?
O2 U1 N3 88.66(18) . . ?
N1 U1 N3 176.57(18) . . ?
N4 U1 N3 90.07(19) . . ?
O1 U1 N2 88.01(19) . . ?
O2 U1 N2 91.02(18) . . ?
N1 U1 N2 88.60(19) . . ?
N4 U1 N2 175.55(18) . . ?
N3 U1 N2 93.47(19) . . ?
O18 K2 O16 112.8(2) . . ?
O18 K2 O12 104.2(3) . . ?
O16 K2 O12 118.0(2) . . ?
O18 K2 O17 59.7(2) . . ?
O16 K2 O17 73.1(2) . . ?
O12 K2 O17 86.1(2) . . ?
O18 K2 O15 101.0(3) . . ?
O16 K2 O15 59.6(2) . . ?
O12 K2 O15 152.74(19) . . ?
O17 K2 O15 116.0(2) . . ?
O18 K2 O14 79.4(2) . . ?
O16 K2 O14 118.3(2) . . ?
O12 K2 O14 116.1(2) . . ?
O17 K2 O14 137.7(2) . . ?
O15 K2 O14 58.7(2) . . ?
O18 K2 O13 88.1(2) . . ?
O16 K2 O13 158.21(19) . . ?
O12 K2 O13 59.0(2) . . ?
O17 K2 O13 125.7(3) . . ?
O15 K2 O13 112.1(2) . . ?
O14 K2 O13 57.4(2) . . ?
O18 K2 O11 130.0(2) . . ?
O16 K2 O11 58.6(2) . . ?
O12 K2 O11 59.37(19) . . ?
O17 K2 O11 71.6(2) . . ?
O15 K2 O11 110.4(2) . . ?
O14 K2 O11 150.49(19) . . ?
O13 K2 O11 113.2(2) . . ?
O18 K2 C86 45.6(3) . . ?
O16 K2 C86 96.4(3) . . ?
O12 K2 C86 75.9(4) . . ?
O17 K2 C86 23.3(3) . . ?
O15 K2 C86 130.4(4) . . ?
O14 K2 C86 123.8(3) . . ?
O13 K2 C86 103.1(3) . . ?
O11 K2 C86 84.7(3) . . ?
O10 K1 O6 96.11(19) . . ?
O10 K1 O4 119.4(2) . . ?
O6 K1 O4 119.0(2) . . ?
O10 K1 O7 80.17(18) . . ?
O6 K1 O7 59.92(17) . . ?
O4 K1 O7 159.59(19) . . ?
O10 K1 O5 129.82(19) . . ?
O6 K1 O5 59.46(19) . . ?
O4 K1 O5 59.7(2) . . ?
O7 K1 O5 113.74(18) . . ?
O10 K1 O3 103.9(2) . . ?
O6 K1 O3 157.8(2) . . ?
O4 K1 O3 58.6(2) . . ?
O7 K1 O3 113.8(2) . . ?
O5 K1 O3 111.9(2) . . ?
O10 K1 O9 59.70(17) . . ?
O6 K1 O9 77.61(18) . . ?
O4 K1 O9 80.3(2) . . ?
O7 K1 O9 117.27(18) . . ?
O5 K1 O9 71.87(18) . . ?
O3 K1 O9 120.9(2) . . ?
O10 K1 O8 76.76(18) . . ?
O6 K1 O8 118.82(18) . . ?
O4 K1 O8 116.8(2) . . ?
O7 K1 O8 58.99(18) . . ?
O5 K1 O8 152.72(19) . . ?
O3 K1 O8 58.3(2) . . ?
O9 K1 O8 135.41(18) . . ?
O10 K1 C70 43.07(19) . . ?
O6 K1 C70 68.33(19) . . ?
O4 K1 C70 104.4(2) . . ?
O7 K1 C70 94.02(19) . . ?
O5 K1 C70 86.9(2) . . ?
O3 K1 C70 133.6(2) . . ?
O9 K1 C70 24.28(18) . . ?
O8 K1 C70 118.7(2) . . ?
O10 K1 C64 74.2(2) . . ?
O6 K1 C64 41.9(2) . . ?
O4 K1 C64 160.2(2) . . ?
O7 K1 C64 22.13(19) . . ?
O5 K1 C64 100.7(2) . . ?
O3 K1 C64 135.7(2) . . ?
O9 K1 C64 96.8(2) . . ?
O8 K1 C64 79.0(2) . . ?
C70 K1 C64 75.1(2) . . ?
C57 O3 C68 114.2(10) . . ?
C57 O3 K1 108.4(7) . . ?
C68 O3 K1 115.4(6) . . ?
C58 O4 C59 108.7(10) . . ?
C58 O4 K1 121.7(7) . . ?
C59 O4 K1 116.4(6) . . ?
C60 O5 C61 108.8(9) . . ?
C60 O5 K1 111.7(6) . . ?
C61 O5 K1 111.5(5) . . ?
C62 O6 C63 113.2(7) . . ?
C62 O6 K1 117.8(6) . . ?
C63 O6 K1 117.3(5) . . ?
C64 O7 C65 112.7(7) . . ?
C64 O7 K1 108.1(5) . . ?
C65 O7 K1 111.6(5) . . ?
C67 O8 C66 110.9(8) . . ?
C67 O8 K1 117.1(6) . . ?
C66 O8 K1 116.0(6) . . ?
C69 O9 C70 116.1(7) . . ?
C69 O9 K1 124.1(7) . . ?
C70 O9 K1 101.3(5) . . ?
C71 O10 C72 111.8(7) . . ?
C71 O10 K1 121.4(5) . . ?
C72 O10 K1 120.7(6) . . ?
C84 O11 C73 111.2(8) . . ?
C84 O11 K2 108.7(6) . . ?
C73 O11 K2 111.4(6) . . ?
C74 O12 C75 114.2(8) . . ?
C74 O12 K2 117.5(6) . . ?
C75 O12 K2 118.7(6) . . ?
C77 O13 C76 113.6(10) . . ?
C77 O13 K2 110.4(7) . . ?
C76 O13 K2 106.5(6) . . ?
C79 O14 C78 110.9(11) . . ?
C79 O14 K2 117.3(8) . . ?
C78 O14 K2 118.1(7) . . ?
C80 O15 C81 113.2(10) . . ?
C80 O15 K2 112.8(6) . . ?
C81 O15 K2 107.8(6) . . ?
C82 O16 C83 113.7(8) . . ?
C82 O16 K2 119.3(7) . . ?
C83 O16 K2 121.5(6) . . ?
C86 O17 C85 116.1(11) . . ?
C86 O17 K2 101.9(8) . . ?
C85 O17 K2 124.8(8) . . ?
C88 O18 C87 114.3(8) . . ?
C88 O18 K2 127.0(7) . . ?
C87 O18 K2 117.7(6) . . ?
C7 N1 C1 114.8(5) . . ?
C7 N1 U1 128.2(4) . . ?
C1 N1 U1 116.0(4) . . ?
C21 N2 C15 115.8(5) . . ?
C21 N2 U1 124.4(4) . . ?
C15 N2 U1 119.1(4) . . ?
C35 N3 C29 115.9(5) . . ?
C35 N3 U1 122.9(4) . . ?
C29 N3 U1 120.9(4) . . ?
C49 N4 C43 115.6(5) . . ?
C49 N4 U1 129.6(4) . . ?
C43 N4 U1 114.7(4) . . ?
C6 C1 C2 120.0(7) . . ?
C6 C1 N1 120.9(7) . . ?
C2 C1 N1 119.1(7) . . ?
C1 C2 C3 118.4(9) . . ?
C4 C3 C2 124.1(10) . . ?
C3 C4 C5 118.0(9) . . ?
C4 C5 C6 119.3(9) . . ?
C1 C6 C5 119.8(8) . . ?
N1 C7 C8 121.9(6) . . ?
N1 C7 C12 121.8(6) . . ?
C8 C7 C12 116.3(6) . . ?
C9 C8 C7 120.4(7) . . ?
C10 C9 C8 124.6(8) . . ?
C10 C9 C13 116.2(7) . . ?
C8 C9 C13 119.2(7) . . ?
C9 C10 C11 115.2(7) . . ?
C12 C11 C10 122.4(7) . . ?
C12 C11 C14 117.6(8) . . ?
C10 C11 C14 120.0(8) . . ?
C11 C12 C7 121.0(7) . . ?
F3 C13 F2 105.7(10) . . ?
F3 C13 F1 108.0(11) . . ?
F2 C13 F1 101.3(9) . . ?
F3 C13 C9 115.6(8) . . ?
F2 C13 C9 113.3(9) . . ?
F1 C13 C9 111.9(9) . . ?
F4 C14 F5 104.2(11) . . ?
F4 C14 F6 109.1(9) . . ?
F5 C14 F6 103.1(10) . . ?
F4 C14 C11 114.2(9) . . ?
F5 C14 C11 113.8(8) . . ?
F6 C14 C11 111.6(10) . . ?
C20 C15 N2 123.5(7) . . ?
C20 C15 C16 115.9(7) . . ?
N2 C15 C16 120.6(7) . . ?
C17 C16 C15 121.0(9) . . ?
C18 C17 C16 120.6(9) . . ?
C17 C18 C19 120.3(8) . . ?
C20 C19 C18 118.5(8) . . ?
C19 C20 C15 123.7(8) . . ?
N2 C21 C26 120.6(6) . . ?
N2 C21 C22 122.2(6) . . ?
C26 C21 C22 117.2(6) . . ?
C23 C22 C21 120.8(7) . . ?
C24 C23 C22 121.4(7) . . ?
C24 C23 C27 121.2(7) . . ?
C22 C23 C27 117.4(7) . . ?
C25 C24 C23 118.5(6) . . ?
C24 C25 C26 120.6(7) . . ?
C24 C25 C28 120.5(7) . . ?
C26 C25 C28 118.8(7) . . ?
C21 C26 C25 121.5(6) . . ?
F9 C27 F7 105.7(7) . . ?
F9 C27 F8 107.1(8) . . ?
F7 C27 F8 102.4(8) . . ?
F9 C27 C23 115.1(8) . . ?
F7 C27 C23 112.6(7) . . ?
F8 C27 C23 112.9(7) . . ?
F12 C28 F11 103.7(9) . . ?
F12 C28 F10 106.9(8) . . ?
F11 C28 F10 104.5(8) . . ?
F12 C28 C25 113.7(8) . . ?
F11 C28 C25 113.8(7) . . ?
F10 C28 C25 113.3(8) . . ?
C34 C29 C30 118.1(7) . . ?
C34 C29 N3 120.8(7) . . ?
C30 C29 N3 121.2(7) . . ?
C31 C30 C29 122.8(9) . . ?
C30 C31 C32 117.9(10) . . ?
C33 C32 C31 120.6(8) . . ?
C32 C33 C34 120.7(9) . . ?
C29 C34 C33 119.9(10) . . ?
N3 C35 C36 122.4(7) . . ?
N3 C35 C40 122.1(6) . . ?
C36 C35 C40 115.4(6) . . ?
C37 C36 C35 122.3(7) . . ?
C36 C37 C38 121.8(7) . . ?
C36 C37 C41 119.2(7) . . ?
C38 C37 C41 118.9(7) . . ?
C37 C38 C39 116.6(7) . . ?
C40 C39 C38 122.3(7) . . ?
C40 C39 C42 118.5(7) . . ?
C38 C39 C42 119.2(7) . . ?
C39 C40 C35 121.6(7) . . ?
F15 C41 F13 110.9(9) . . ?
F15 C41 F14 102.3(8) . . ?
F13 C41 F14 102.9(8) . . ?
F15 C41 C37 114.1(8) . . ?
F13 C41 C37 115.5(7) . . ?
F14 C41 C37 109.7(8) . . ?
F16 C42 F17 109.7(9) . . ?
F16 C42 F18 102.7(9) . . ?
F17 C42 F18 101.0(9) . . ?
F16 C42 C39 115.1(9) . . ?
F17 C42 C39 113.9(8) . . ?
F18 C42 C39 113.0(8) . . ?
C44 C43 N4 121.3(7) . . ?
C44 C43 C48 118.1(7) . . ?
N4 C43 C48 120.6(6) . . ?
C43 C44 C45 119.9(8) . . ?
C46 C45 C44 121.4(9) . . ?
C45 C46 C47 119.9(8) . . ?
C48 C47 C46 120.3(9) . . ?
C47 C48 C43 120.5(8) . . ?
N4 C49 C54 122.0(6) . . ?
N4 C49 C50 122.9(6) . . ?
C54 C49 C50 115.0(6) . . ?
C51 C50 C49 122.1(7) . . ?
C52 C51 C50 122.4(7) . . ?
C52 C51 C55 118.1(7) . . ?
C50 C51 C55 119.4(7) . . ?
C51 C52 C53 118.1(7) . . ?
C52 C53 C54 120.2(7) . . ?
C52 C53 C56 121.8(8) . . ?
C54 C53 C56 118.0(8) . . ?
C49 C54 C53 122.3(7) . . ?
F20 C55 F21 108.2(8) . . ?
F20 C55 F19 104.0(8) . . ?
F21 C55 F19 104.3(8) . . ?
F20 C55 C51 115.1(8) . . ?
F21 C55 C51 112.0(8) . . ?
F19 C55 C51 112.5(7) . . ?
F24 C56 F23 104.7(11) . . ?
F24 C56 F22 110.5(10) . . ?
F23 C56 F22 101.7(9) . . ?
F24 C56 C53 116.5(8) . . ?
F23 C56 C53 111.3(10) . . ?
F22 C56 C53 110.9(10) . . ?
O3 C57 C58 109.5(11) . . ?
O4 C58 C57 105.9(9) . . ?
O4 C59 C60 109.8(9) . . ?
O5 C60 C59 105.4(10) . . ?
O5 C61 C62 108.4(9) . . ?
O6 C62 C61 110.2(8) . . ?
O6 C63 C64 109.1(7) . . ?
O7 C64 C63 108.2(7) . . ?
O7 C64 K1 49.8(4) . . ?
C63 C64 K1 82.6(4) . . ?
O7 C65 C66 106.5(7) . . ?
O8 C66 C65 108.1(8) . . ?
O8 C67 C68 109.7(8) . . ?
O3 C68 C67 107.6(9) . . ?
O9 C70 C71 111.2(7) . . ?
O9 C70 K1 54.4(4) . . ?
C71 C70 K1 86.1(5) . . ?
O10 C71 C70 108.5(7) . . ?
O11 C73 C74 109.4(8) . . ?
O12 C74 C73 111.3(9) . . ?
C76 C75 O12 109.7(9) . . ?
C75 C76 O13 109.8(10) . . ?
O13 C77 C78 106.9(11) . . ?
O14 C78 C77 107.2(10) . . ?
O14 C79 C80 109.4(11) . . ?
O15 C80 C79 109.3(10) . . ?
O15 C81 C82 109.2(8) . . ?
O16 C82 C81 110.3(9) . . ?
O16 C83 C84 108.9(8) . . ?
O11 C84 C83 110.6(8) . . ?
O17 C86 C87 109.2(13) . . ?
O17 C86 K2 54.8(6) . . ?
C87 C86 K2 89.5(7) . . ?
O18 C87 C86 106.5(8) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.62
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.848
_refine_diff_density_min         -1.472
_refine_diff_density_rms         0.122

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.289 0.493 0.107 179 51 ' '
2 0.289 1.007 0.607 179 50 ' '
3 0.154 0.204 0.118 30 4 ' '
4 0.154 0.296 0.618 30 5 ' '
5 0.223 0.003 0.186 25 5 ' '
6 0.223 0.497 0.686 25 5 ' '
7 0.711 0.993 0.393 179 51 ' '
8 0.711 0.507 0.893 179 50 ' '
9 0.777 0.503 0.314 25 5 ' '
10 0.777 -0.003 0.814 25 5 ' '
11 0.846 0.704 0.382 30 5 ' '
12 0.846 0.796 0.882 30 5 ' '

#===END
_database_code_depnum_ccdc_archive 'CCDC 965033'
