#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/09/4500934.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4500934
loop_
_publ_author_name
'Thuéry, Pierre'
_publ_section_title
;
 Uranyl--Alkali Metal Ion Heterometallic Complexes with Cucurbit[6]uril
 and a Sulfonated Catechol
;
_journal_issue                   7
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3282
_journal_paper_doi               10.1021/cg2005375
_journal_volume                  11
_journal_year                    2011
_chemical_formula_sum            'C120 H153 K3 N75 O64.5 U3'
_chemical_formula_weight         4509.56
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   27.3529(13)
_cell_length_b                   27.3529(13)
_cell_length_c                   12.2825(5)
_cell_measurement_reflns_used    182977
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.23
_cell_volume                     7958.4(6)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and three ω scans with 2° steps (320 frames)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            182977
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.244
_exptl_absorpt_correction_T_max  0.723
_exptl_absorpt_correction_T_min  0.531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             4494
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.119
_refine_diff_density_min         -1.424
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         10055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0719P)²+17.3761P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1221
_reflns_number_gt                8221
_reflns_number_total             10055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg2005375_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        7958.4(19)
_cod_original_formula_sum        'C120 H153 K3 N75 O64.50 U3'
_cod_database_code               4500934
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
U U 0.752198(9) 0.346734(9) 0.603194(17) 0.02602(9) Uani 1 1 d .
K K 0.73794(6) 0.28240(6) 0.27505(11) 0.0379(3) Uani 1 1 d .
O1 O 0.74825(18) 0.34690(18) 0.4580(3) 0.0328(10) Uani 1 1 d .
O2 O 0.76157(18) 0.34523(18) 0.7466(4) 0.0332(10) Uani 1 1 d .
O3 O 0.85042(19) 0.4199(2) 0.6036(4) 0.0425(12) Uani 1 1 d .
O4 O 0.9086(2) 0.3958(2) 0.5282(5) 0.0559(14) Uani 1 1 d .
O5 O 0.6667 0.3333 0.6291(6) 0.0287(16) Uani 1 3 d S
O6 O 0.68369(17) 0.24985(17) 0.6016(3) 0.0276(9) Uani 1 1 d .
H6 H 0.6863 0.2237 0.5499 0.033 Uiso 1 1 d R
O7 O 0.8119(2) 0.3002(2) 0.5767(4) 0.0382(11) Uani 1 1 d .
H7A H 0.8433 0.3272 0.5349 0.046 Uiso 1 1 d R
H7B H 0.7978 0.2689 0.5236 0.046 Uiso 1 1 d R
O8 O 0.7168(3) 0.1865(2) 0.1795(5) 0.0568(14) Uani 1 1 d .
O9 O 0.8420(2) 0.2928(2) 0.3290(5) 0.0597(16) Uani 1 1 d .
O10 O 0.6667 0.3333 0.3021(11) 0.035(4) Uani 0.50 3 d SP
O11 O 0.77031(17) 0.30209(16) 0.0567(3) 0.0282(9) Uani 1 1 d .
O12 O 0.7074(2) 0.08513(18) -0.2023(3) 0.0343(10) Uani 1 1 d .
O13 O 0.63945(18) 0.24306(17) 0.1907(3) 0.0295(9) Uani 1 1 d .
O14 O 0.58910(19) 0.01971(18) -0.0363(3) 0.0341(10) Uani 1 1 d .
O15 O 0.66909(16) 0.18909(15) 0.4118(3) 0.0242(8) Uani 1 1 d .
O16 O 0.59875(18) -0.03800(17) 0.2086(3) 0.0320(10) Uani 1 1 d .
O17 O 0.80127(18) 0.19734(17) 0.5069(3) 0.0313(9) Uani 1 1 d .
O18 O 0.72579(18) -0.03280(17) 0.3016(3) 0.0275(9) Uani 1 1 d .
O19 O 0.92224(18) 0.25832(18) 0.3660(4) 0.0365(10) Uani 1 1 d .
O20 O 0.84106(19) 0.03322(18) 0.1398(4) 0.0363(10) Uani 1 1 d .
O21 O 0.90900(18) 0.31136(18) 0.1410(4) 0.0334(10) Uani 1 1 d .
O22 O 0.8383(2) 0.09125(18) -0.1163(4) 0.0414(11) Uani 1 1 d .
O23 O 0.9833(2) 0.3989(2) 0.2952(4) 0.0509(13) Uani 1 1 d .
H23A H 0.9620 0.3745 0.2448 0.061 Uiso 1 1 d R
H23B H 0.9586 0.3932 0.3507 0.061 Uiso 1 1 d R
N1 N 0.7432(2) 0.1218(2) 0.1434(4) 0.0310(11) Uani 1 1 d .
N2 N 0.7973(2) 0.2630(2) -0.0808(4) 0.0269(11) Uani 1 1 d .
N3 N 0.7079(2) 0.2421(2) -0.0737(4) 0.0270(11) Uani 1 1 d .
N4 N 0.6829(2) 0.1534(2) -0.1658(4) 0.0297(11) Uani 1 1 d .
N5 N 0.7734(2) 0.1806(2) -0.1941(4) 0.0296(11) Uani 1 1 d .
N6 N 0.6211(2) 0.1943(2) 0.0277(4) 0.0254(10) Uani 1 1 d .
N7 N 0.5731(2) 0.1481(2) 0.1763(4) 0.0270(11) Uani 1 1 d .
N8 N 0.5568(2) 0.0604(2) 0.0891(4) 0.0270(11) Uani 1 1 d .
N9 N 0.5946(2) 0.1055(2) -0.0672(4) 0.0299(11) Uani 1 1 d .
N10 N 0.5908(2) 0.11039(19) 0.3409(4) 0.0228(10) Uani 1 1 d .
N11 N 0.6451(2) 0.09772(19) 0.4582(4) 0.0236(10) Uani 1 1 d .
N12 N 0.6181(2) 0.00719(19) 0.3745(4) 0.0222(10) Uani 1 1 d .
N13 N 0.5629(2) 0.0190(2) 0.2594(4) 0.0287(11) Uani 1 1 d .
N14 N 0.7325(2) 0.10317(19) 0.5157(4) 0.0236(10) Uani 1 1 d .
N15 N 0.8223(2) 0.1255(2) 0.5009(4) 0.0289(11) Uani 1 1 d .
N16 N 0.7921(2) 0.0339(2) 0.4174(4) 0.0283(11) Uani 1 1 d .
N17 N 0.7025(2) 0.0096(2) 0.4390(4) 0.0248(10) Uani 1 1 d .
N18 N 0.9090(2) 0.1690(2) 0.3952(4) 0.0334(12) Uani 1 1 d .
N19 N 0.9521(2) 0.2142(2) 0.2431(4) 0.0324(12) Uani 1 1 d .
N20 N 0.9184(2) 0.1235(2) 0.1519(4) 0.0298(11) Uani 1 1 d .
N21 N 0.8762(2) 0.0785(2) 0.3046(4) 0.0332(12) Uani 1 1 d .
N22 N 0.9446(2) 0.2561(2) 0.0744(4) 0.0317(12) Uani 1 1 d .
N23 N 0.8842(2) 0.2678(2) -0.0263(4) 0.0273(11) Uani 1 1 d .
N24 N 0.8595(2) 0.1839(2) -0.1348(4) 0.0276(11) Uani 1 1 d .
N25 N 0.9083(2) 0.1641(2) -0.0148(4) 0.0285(11) Uani 1 1 d .
C1 C 0.8993(3) 0.4289(3) 0.5794(5) 0.0332(14) Uani 1 1 d .
H1 H 0.9302 0.4627 0.6020 0.040 Uiso 1 1 calc R
C2 C 0.7094(3) 0.1439(3) 0.1378(6) 0.0443(18) Uani 1 1 d .
H2 H 0.6766 0.1240 0.0970 0.053 Uiso 1 1 calc R
C3 C 0.7942(4) 0.1493(4) 0.2078(8) 0.064(2) Uani 1 1 d .
H3A H 0.7925 0.1759 0.2563 0.096 Uiso 1 1 calc R
H3B H 0.8262 0.1687 0.1605 0.096 Uiso 1 1 calc R
H3C H 0.7978 0.1215 0.2494 0.096 Uiso 1 1 calc R
C4 C 0.7289(3) 0.0690(3) 0.0884(7) 0.0483(18) Uani 1 1 d .
H4A H 0.6945 0.0561 0.0479 0.072 Uiso 1 1 calc R
H4B H 0.7238 0.0411 0.1414 0.072 Uiso 1 1 calc R
H4C H 0.7588 0.0752 0.0396 0.072 Uiso 1 1 calc R
C5 C 0.7592(3) 0.2719(2) -0.0238(5) 0.0280(13) Uani 1 1 d .
C6 C 0.7727(3) 0.2330(2) -0.1831(5) 0.0287(13) Uani 1 1 d .
H6A H 0.7897 0.2576 -0.2465 0.034 Uiso 1 1 calc R
C7 C 0.7102(3) 0.2141(3) -0.1723(4) 0.0277(13) Uani 1 1 d .
H7 H 0.6967 0.2260 -0.2353 0.033 Uiso 1 1 calc R
C8 C 0.7196(3) 0.1341(3) -0.1874(4) 0.0297(13) Uani 1 1 d .
C9 C 0.6576(3) 0.2428(3) -0.0371(5) 0.0294(13) Uani 1 1 d .
H9A H 0.6689 0.2767 0.0054 0.035 Uiso 1 1 calc R
H9B H 0.6369 0.2441 -0.1001 0.035 Uiso 1 1 calc R
C10 C 0.6225(3) 0.1169(3) -0.1722(5) 0.0332(14) Uani 1 1 d .
H10A H 0.6145 0.0814 -0.2051 0.040 Uiso 1 1 calc R
H10B H 0.6070 0.1342 -0.2194 0.040 Uiso 1 1 calc R
C11 C 0.6145(3) 0.2001(3) 0.1377(5) 0.0272(13) Uani 1 1 d .
C12 C 0.5762(3) 0.1410(3) -0.0142(5) 0.0290(13) Uani 1 1 d .
H12 H 0.5504 0.1468 -0.0609 0.035 Uiso 1 1 calc R
C13 C 0.5459(2) 0.1076(2) 0.0893(5) 0.0259(12) Uani 1 1 d .
H13 H 0.5053 0.0942 0.0865 0.031 Uiso 1 1 calc R
C14 C 0.5815(2) 0.0585(3) -0.0073(5) 0.0290(13) Uani 1 1 d .
C15 C 0.5634(3) 0.1392(3) 0.2914(5) 0.0275(13) Uani 1 1 d .
H15A H 0.5231 0.1171 0.3043 0.033 Uiso 1 1 calc R
H15B H 0.5771 0.1755 0.3268 0.033 Uiso 1 1 calc R
C16 C 0.5306(3) 0.0127(2) 0.1612(5) 0.0272(13) Uani 1 1 d .
H16A H 0.5251 -0.0206 0.1223 0.033 Uiso 1 1 calc R
H16B H 0.4937 0.0065 0.1818 0.033 Uiso 1 1 calc R
C17 C 0.6382(2) 0.1381(2) 0.4038(4) 0.0209(11) Uani 1 1 d .
C18 C 0.5621(2) 0.0498(2) 0.3542(4) 0.0223(11) Uani 1 1 d .
H18 H 0.5238 0.0350 0.3824 0.027 Uiso 1 1 calc R
C19 C 0.5999(2) 0.0408(2) 0.4359(4) 0.0214(11) Uani 1 1 d .
H19 H 0.5793 0.0214 0.5021 0.026 Uiso 1 1 calc R
C20 C 0.5940(2) -0.0072(2) 0.2727(5) 0.0254(12) Uani 1 1 d .
C21 C 0.6860(2) 0.1114(2) 0.5443(4) 0.0252(12) Uani 1 1 d .
H21A H 0.7008 0.1505 0.5650 0.030 Uiso 1 1 calc R
H21B H 0.6669 0.0883 0.6073 0.030 Uiso 1 1 calc R
C22 C 0.6425(2) -0.0230(2) 0.4270(5) 0.0253(12) Uani 1 1 d .
H22A H 0.6255 -0.0351 0.4985 0.030 Uiso 1 1 calc R
H22B H 0.6331 -0.0565 0.3848 0.030 Uiso 1 1 calc R
C23 C 0.7872(2) 0.1477(2) 0.5075(4) 0.0253(12) Uani 1 1 d .
C24 C 0.7308(2) 0.0493(2) 0.5269(4) 0.0234(12) Uani 1 1 d .
H24 H 0.7159 0.0321 0.5981 0.028 Uiso 1 1 calc R
C25 C 0.7934(2) 0.0652(2) 0.5133(5) 0.0246(12) Uani 1 1 d .
H25 H 0.8071 0.0540 0.5771 0.030 Uiso 1 1 calc R
C26 C 0.7389(2) 0.0006(2) 0.3760(5) 0.0247(12) Uani 1 1 d .
C27 C 0.8830(3) 0.1607(3) 0.5014(5) 0.0341(14) Uani 1 1 d .
H27A H 0.8987 0.1438 0.5493 0.041 Uiso 1 1 calc R
H27B H 0.8927 0.1972 0.5314 0.041 Uiso 1 1 calc R
C28 C 0.8402(3) 0.0317(3) 0.3742(5) 0.0310(14) Uani 1 1 d .
H28A H 0.8624 0.0305 0.4345 0.037 Uiso 1 1 calc R
H28B H 0.8266 -0.0031 0.3333 0.037 Uiso 1 1 calc R
C29 C 0.9263(2) 0.2177(3) 0.3374(5) 0.0332(14) Uani 1 1 d .
C30 C 0.9241(3) 0.1303(3) 0.3426(5) 0.0320(14) Uani 1 1 d .
H30 H 0.9494 0.1232 0.3880 0.038 Uiso 1 1 calc R
C31 C 0.9534(2) 0.1621(3) 0.2365(5) 0.0309(14) Uani 1 1 d .
H31 H 0.9922 0.1694 0.2321 0.037 Uiso 1 1 calc R
C32 C 0.8745(3) 0.0740(3) 0.1926(5) 0.0314(14) Uani 1 1 d .
C33 C 0.9792(2) 0.2609(3) 0.1670(5) 0.0328(14) Uani 1 1 d .
H33A H 0.9892 0.2957 0.2052 0.039 Uiso 1 1 calc R
H33B H 1.0139 0.2634 0.1411 0.039 Uiso 1 1 calc R
C34 C 0.9311(3) 0.1322(3) 0.0367(5) 0.0313(14) Uani 1 1 d .
H34A H 0.9157 0.0958 0.0012 0.038 Uiso 1 1 calc R
H34B H 0.9717 0.1520 0.0270 0.038 Uiso 1 1 calc R
C35 C 0.9117(2) 0.2812(2) 0.0701(5) 0.0302(14) Uani 1 1 d .
C36 C 0.9403(3) 0.2255(2) -0.0249(5) 0.0304(13) Uani 1 1 d .
H36 H 0.9775 0.2383 -0.0574 0.037 Uiso 1 1 calc R
C37 C 0.9031(3) 0.2386(3) -0.0989(5) 0.0318(14) Uani 1 1 d .
H37 H 0.9246 0.2625 -0.1605 0.038 Uiso 1 1 calc R
C38 C 0.8659(3) 0.1416(3) -0.0912(5) 0.0301(13) Uani 1 1 d .
C39 C 0.8568(3) 0.2982(2) -0.0658(5) 0.0295(13) Uani 1 1 d .
H39A H 0.8636 0.3278 -0.0143 0.035 Uiso 1 1 calc R
H39B H 0.8738 0.3160 -0.1346 0.035 Uiso 1 1 calc R
C40 C 0.8222(3) 0.1755(3) -0.2246(5) 0.0339(14) Uani 1 1 d .
H40A H 0.8090 0.1382 -0.2551 0.041 Uiso 1 1 calc R
H40B H 0.8431 0.2030 -0.2808 0.041 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
U U -9.6767 9.6646 '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'
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
O2 U O1 174.5(2) . .
O2 U O5 90.4(2) . .
O1 U O5 94.8(2) . .
O2 U O6 91.42(17) . .
O1 U O6 88.84(17) . .
O5 U O6 68.49(10) . .
O2 U O6 96.04(17) . 2_655
O1 U O6 87.61(16) . 2_655
O5 U O6 67.55(9) . 2_655
O6 U O6 135.39(15) . 2_655
O2 U O3 84.48(19) . .
O1 U O3 92.51(18) . .
O5 U O3 141.76(12) . .
O6 U O3 149.26(15) . .
O6 U O3 75.35(15) 2_655 .
O2 U O7 88.81(17) . .
O1 U O7 85.89(17) . .
O5 U O7 146.04(11) . .
O6 U O7 77.59(15) . .
O6 U O7 146.23(14) 2_655 .
O3 U O7 71.89(16) . .
O13 K O8 75.14(16) . .
O13 K O1 110.11(14) . .
O8 K O1 152.20(16) . .
O13 K O11 81.86(13) . .
O8 K O11 70.00(16) . .
O1 K O11 137.04(13) . .
O13 K O9 160.08(14) . .
O8 K O9 85.01(16) . .
O1 K O9 88.23(14) . .
O11 K O9 89.97(16) . .
O13 K O15 77.08(13) . .
O8 K O15 69.83(16) . .
O1 K O15 84.48(12) . .
O11 K O15 138.16(12) . .
O9 K O15 97.78(16) . .
O13 K O10 55.68(17) . .
O8 K O10 130.64(19) . .
O1 K O10 59.1(2) . .
O11 K O10 103.9(3) . .
O9 K O10 144.23(18) . .
O15 K O10 93.46(18) . .
O13 K O13 84.20(17) . 2_655
O8 K O13 134.03(16) . 2_655
O1 K O13 73.54(12) . 2_655
O11 K O13 66.67(11) . 2_655
O9 K O13 109.25(16) . 2_655
O15 K O13 144.13(12) . 2_655
O10 K O13 50.98(16) . 2_655
U O1 K 142.3(2) . .
C1 O3 U 141.9(4) . .
U O5 U 117.94(9) . 3_665
U O5 U 117.94(9) . 2_655
U O5 U 117.95(9) 3_665 2_655
U O6 U 104.60(15) . 3_665
U O6 H6 121.0 . .
U O6 H6 115.3 3_665 .
U O7 H7A 103.7 . .
U O7 H7B 116.6 . .
H7A O7 H7B 97.3 . .
C2 O8 K 177.4(5) . .
K O10 K 118.73(10) . 3_665
K O10 K 118.73(10) . 2_655
K O10 K 118.73(10) 3_665 2_655
C5 O11 K 134.2(4) . .
C11 O13 K 126.0(4) . .
C11 O13 K 103.4(4) . 3_665
K O13 K 126.30(15) . 3_665
C17 O15 K 138.5(3) . .
H23A O23 H23B 104.0 . .
C2 N1 C3 120.0(6) . .
C2 N1 C4 121.4(6) . .
C3 N1 C4 118.6(6) . .
C5 N2 C39 121.6(5) . .
C5 N2 C6 111.1(5) . .
C39 N2 C6 122.4(5) . .
C5 N3 C7 112.9(5) . .
C5 N3 C9 123.2(5) . .
C7 N3 C9 123.6(5) . .
C8 N4 C7 112.0(5) . .
C8 N4 C10 121.9(5) . .
C7 N4 C10 123.2(5) . .
C8 N5 C6 111.7(5) . .
C8 N5 C40 122.0(5) . .
C6 N5 C40 125.7(5) . .
C11 N6 C9 120.5(5) . .
C11 N6 C12 111.6(5) . .
C9 N6 C12 125.4(5) . .
C11 N7 C15 119.9(5) . .
C11 N7 C13 112.1(5) . .
C15 N7 C13 128.0(5) . .
C14 N8 C16 121.7(5) . .
C14 N8 C13 110.9(5) . .
C16 N8 C13 124.8(5) . .
C14 N9 C10 122.9(5) . .
C14 N9 C12 111.9(5) . .
C10 N9 C12 125.2(5) . .
C17 N10 C18 113.0(4) . .
C17 N10 C15 122.4(5) . .
C18 N10 C15 122.4(5) . .
C17 N11 C21 122.9(5) . .
C17 N11 C19 112.6(4) . .
C21 N11 C19 123.3(4) . .
C20 N12 C22 122.2(5) . .
C20 N12 C19 112.7(4) . .
C22 N12 C19 122.0(4) . .
C20 N13 C18 113.7(5) . .
C20 N13 C16 122.4(5) . .
C18 N13 C16 123.7(5) . .
C23 N14 C21 122.1(5) . .
C23 N14 C24 111.8(5) . .
C21 N14 C24 123.4(5) . .
C23 N15 C25 113.4(5) . .
C23 N15 C27 122.0(5) . .
C25 N15 C27 123.7(5) . .
C26 N16 C25 113.5(5) . .
C26 N16 C28 121.4(5) . .
C25 N16 C28 124.8(5) . .
C26 N17 C22 122.5(5) . .
C26 N17 C24 112.9(5) . .
C22 N17 C24 124.0(5) . .
C29 N18 C27 121.5(5) . .
C29 N18 C30 113.0(5) . .
C27 N18 C30 125.3(5) . .
C29 N19 C31 112.4(5) . .
C29 N19 C33 121.9(5) . .
C31 N19 C33 125.4(5) . .
C32 N20 C34 122.3(5) . .
C32 N20 C31 113.0(5) . .
C34 N20 C31 124.3(5) . .
C32 N21 C28 122.3(5) . .
C32 N21 C30 112.5(5) . .
C28 N21 C30 124.2(5) . .
C35 N22 C33 123.1(5) . .
C35 N22 C36 111.8(5) . .
C33 N22 C36 125.1(5) . .
C35 N23 C39 120.9(5) . .
C35 N23 C37 112.5(5) . .
C39 N23 C37 122.4(5) . .
C38 N24 C37 111.8(5) . .
C38 N24 C40 123.1(5) . .
C37 N24 C40 123.5(5) . .
C38 N25 C34 123.3(5) . .
C38 N25 C36 110.2(5) . .
C34 N25 C36 122.6(5) . .
O4 C1 O3 124.3(6) . .
O4 C1 H1 117.8 . .
O3 C1 H1 117.8 . .
O8 C2 N1 127.0(6) . .
O8 C2 H2 116.5 . .
N1 C2 H2 116.5 . .
N1 C3 H3A 109.5 . .
N1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
N1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N1 C4 H4A 109.5 . .
N1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
N1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
O11 C5 N3 126.9(6) . .
O11 C5 N2 125.1(6) . .
N3 C5 N2 107.9(5) . .
N5 C6 N2 113.8(5) . .
N5 C6 C7 103.9(5) . .
N2 C6 C7 103.7(5) . .
N5 C6 H6A 111.6 . .
N2 C6 H6A 111.6 . .
C7 C6 H6A 111.6 . .
N4 C7 N3 115.3(5) . .
N4 C7 C6 104.0(5) . .
N3 C7 C6 103.3(5) . .
N4 C7 H7 111.2 . .
N3 C7 H7 111.2 . .
C6 C7 H7 111.2 . .
O12 C8 N4 126.7(6) . .
O12 C8 N5 125.5(6) . .
N4 C8 N5 107.7(5) . .
N6 C9 N3 112.6(5) . .
N6 C9 H9A 109.1 . .
N3 C9 H9A 109.1 . .
N6 C9 H9B 109.1 . .
N3 C9 H9B 109.1 . .
H9A C9 H9B 107.8 . .
N4 C10 N9 113.4(5) . .
N4 C10 H10A 108.9 . .
N9 C10 H10A 108.9 . .
N4 C10 H10B 108.9 . .
N9 C10 H10B 108.9 . .
H10A C10 H10B 107.7 . .
O13 C11 N6 126.4(6) . .
O13 C11 N7 125.9(6) . .
N6 C11 N7 107.7(5) . .
N6 C12 N9 115.4(5) . .
N6 C12 C13 103.7(4) . .
N9 C12 C13 103.6(5) . .
N6 C12 H12 111.2 . .
N9 C12 H12 111.2 . .
C13 C12 H12 111.2 . .
N7 C13 N8 114.9(5) . .
N7 C13 C12 103.6(5) . .
N8 C13 C12 103.6(5) . .
N7 C13 H13 111.4 . .
N8 C13 H13 111.4 . .
C12 C13 H13 111.4 . .
O14 C14 N9 125.3(6) . .
O14 C14 N8 125.4(6) . .
N9 C14 N8 109.3(5) . .
N7 C15 N10 113.5(5) . .
N7 C15 H15A 108.9 . .
N10 C15 H15A 108.9 . .
N7 C15 H15B 108.9 . .
N10 C15 H15B 108.9 . .
H15A C15 H15B 107.7 . .
N8 C16 N13 113.9(5) . .
N8 C16 H16A 108.8 . .
N13 C16 H16A 108.8 . .
N8 C16 H16B 108.8 . .
N13 C16 H16B 108.8 . .
H16A C16 H16B 107.7 . .
O15 C17 N10 126.9(5) . .
O15 C17 N11 125.6(5) . .
N10 C17 N11 107.5(5) . .
N13 C18 N10 114.8(5) . .
N13 C18 C19 103.0(4) . .
N10 C18 C19 103.5(4) . .
N13 C18 H18 111.6 . .
N10 C18 H18 111.6 . .
C19 C18 H18 111.6 . .
N11 C19 N12 113.5(5) . .
N11 C19 C18 103.3(4) . .
N12 C19 C18 103.3(4) . .
N11 C19 H19 112.0 . .
N12 C19 H19 112.0 . .
C18 C19 H19 112.0 . .
O16 C20 N13 126.8(5) . .
O16 C20 N12 126.1(5) . .
N13 C20 N12 107.0(5) . .
N14 C21 N11 114.2(5) . .
N14 C21 H21A 108.7 . .
N11 C21 H21A 108.7 . .
N14 C21 H21B 108.7 . .
N11 C21 H21B 108.7 . .
H21A C21 H21B 107.6 . .
N17 C22 N12 113.8(5) . .
N17 C22 H22A 108.8 . .
N12 C22 H22A 108.8 . .
N17 C22 H22B 108.8 . .
N12 C22 H22B 108.8 . .
H22A C22 H22B 107.7 . .
O17 C23 N15 126.5(6) . .
O17 C23 N14 125.9(5) . .
N15 C23 N14 107.6(5) . .
N17 C24 N14 114.9(4) . .
N17 C24 C25 103.3(4) . .
N14 C24 C25 103.5(4) . .
N17 C24 H24 111.5 . .
N14 C24 H24 111.5 . .
C25 C24 H24 111.5 . .
N15 C25 N16 115.4(5) . .
N15 C25 C24 103.3(5) . .
N16 C25 C24 103.0(4) . .
N15 C25 H25 111.5 . .
N16 C25 H25 111.5 . .
C24 C25 H25 111.5 . .
O18 C26 N16 126.6(5) . .
O18 C26 N17 126.2(6) . .
N16 C26 N17 107.2(5) . .
N15 C27 N18 114.3(5) . .
N15 C27 H27A 108.7 . .
N18 C27 H27A 108.7 . .
N15 C27 H27B 108.7 . .
N18 C27 H27B 108.7 . .
H27A C27 H27B 107.6 . .
N21 C28 N16 114.3(5) . .
N21 C28 H28A 108.7 . .
N16 C28 H28A 108.7 . .
N21 C28 H28B 108.7 . .
N16 C28 H28B 108.7 . .
H28A C28 H28B 107.6 . .
O19 C29 N18 126.3(6) . .
O19 C29 N19 125.9(6) . .
N18 C29 N19 107.7(6) . .
N21 C30 N18 114.0(5) . .
N21 C30 C31 103.9(5) . .
N18 C30 C31 102.6(5) . .
N21 C30 H30 111.9 . .
N18 C30 H30 111.9 . .
C31 C30 H30 111.9 . .
N19 C31 N20 115.2(5) . .
N19 C31 C30 104.3(5) . .
N20 C31 C30 103.0(5) . .
N19 C31 H31 111.2 . .
N20 C31 H31 111.2 . .
C30 C31 H31 111.2 . .
O20 C32 N20 126.4(6) . .
O20 C32 N21 126.1(6) . .
N20 C32 N21 107.4(5) . .
N22 C33 N19 113.9(5) . .
N22 C33 H33A 108.8 . .
N19 C33 H33A 108.8 . .
N22 C33 H33B 108.8 . .
N19 C33 H33B 108.8 . .
H33A C33 H33B 107.7 . .
N20 C34 N25 112.7(5) . .
N20 C34 H34A 109.1 . .
N25 C34 H34A 109.1 . .
N20 C34 H34B 109.1 . .
N25 C34 H34B 109.1 . .
H34A C34 H34B 107.8 . .
O21 C35 N23 126.3(6) . .
O21 C35 N22 125.6(6) . .
N23 C35 N22 108.1(5) . .
N22 C36 N25 115.0(5) . .
N22 C36 C37 103.5(5) . .
N25 C36 C37 103.4(5) . .
N22 C36 H36 111.5 . .
N25 C36 H36 111.5 . .
C37 C36 H36 111.5 . .
N24 C37 N23 115.0(5) . .
N24 C37 C36 103.8(5) . .
N23 C37 C36 103.0(5) . .
N24 C37 H37 111.5 . .
N23 C37 H37 111.5 . .
C36 C37 H37 111.5 . .
O22 C38 N24 125.7(6) . .
O22 C38 N25 125.4(6) . .
N24 C38 N25 109.0(5) . .
N2 C39 N23 113.4(5) . .
N2 C39 H39A 108.9 . .
N23 C39 H39A 108.9 . .
N2 C39 H39B 108.9 . .
N23 C39 H39B 108.9 . .
H39A C39 H39B 107.7 . .
N24 C40 N5 113.4(5) . .
N24 C40 H40A 108.9 . .
N5 C40 H40A 108.9 . .
N24 C40 H40B 108.9 . .
N5 C40 H40B 108.9 . .
H40A C40 H40B 107.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U O2 1.783(4) .
U O1 1.787(4) .
U O5 2.2027(11) .
U O6 2.360(4) .
U O6 2.411(4) 2_655
U O3 2.418(4) .
U O7 2.544(4) .
K O13 2.567(4) .
K O8 2.659(5) .
K O1 2.783(4) .
K O11 2.791(4) .
K O9 2.794(5) .
K O15 2.841(4) .
K O10 2.927(2) .
K O13 3.073(4) 2_655
O3 C1 1.269(8) .
O4 C1 1.229(8) .
O5 U 2.2027(10) 3_665
O5 U 2.2027(10) 2_655
O6 U 2.411(4) 3_665
O6 H6 0.9861 .
O7 H7A 0.9554 .
O7 H7B 0.9876 .
O8 C2 1.195(8) .
O10 K 2.927(2) 3_665
O10 K 2.927(2) 2_655
O11 C5 1.225(7) .
O12 C8 1.222(7) .
O13 C11 1.213(7) .
O13 K 3.073(4) 3_665
O14 C14 1.231(7) .
O15 C17 1.221(7) .
O16 C20 1.206(7) .
O17 C23 1.212(7) .
O18 C26 1.214(7) .
O19 C29 1.221(8) .
O20 C32 1.217(8) .
O21 C35 1.226(7) .
O22 C38 1.233(7) .
O23 H23A 0.8818 .
O23 H23B 0.9163 .
N1 C2 1.334(8) .
N1 C3 1.446(9) .
N1 C4 1.459(8) .
N2 C5 1.376(8) .
N2 C39 1.431(8) .
N2 C6 1.467(7) .
N3 C5 1.364(8) .
N3 C7 1.450(7) .
N3 C9 1.458(8) .
N4 C8 1.373(8) .
N4 C7 1.443(8) .
N4 C10 1.444(8) .
N5 C8 1.384(8) .
N5 C6 1.450(8) .
N5 C40 1.458(8) .
N6 C11 1.382(8) .
N6 C9 1.436(8) .
N6 C12 1.452(7) .
N7 C11 1.384(8) .
N7 C15 1.436(7) .
N7 C13 1.450(7) .
N8 C14 1.377(8) .
N8 C16 1.438(8) .
N8 C13 1.462(7) .
N9 C14 1.365(8) .
N9 C10 1.451(8) .
N9 C12 1.454(8) .
N10 C17 1.368(7) .
N10 C18 1.446(7) .
N10 C15 1.464(7) .
N11 C17 1.381(7) .
N11 C21 1.446(7) .
N11 C19 1.450(7) .
N12 C20 1.376(7) .
N12 C22 1.445(7) .
N12 C19 1.455(7) .
N13 C20 1.370(7) .
N13 C18 1.443(7) .
N13 C16 1.452(7) .
N14 C23 1.382(7) .
N14 C21 1.443(8) .
N14 C24 1.458(7) .
N15 C23 1.373(8) .
N15 C25 1.436(7) .
N15 C27 1.443(8) .
N16 C26 1.371(8) .
N16 C25 1.446(7) .
N16 C28 1.447(8) .
N17 C26 1.377(7) .
N17 C22 1.433(7) .
N17 C24 1.450(7) .
N18 C29 1.370(8) .
N18 C27 1.449(8) .
N18 C30 1.465(8) .
N19 C29 1.386(8) .
N19 C31 1.443(8) .
N19 C33 1.452(8) .
N20 C32 1.378(8) .
N20 C34 1.448(8) .
N20 C31 1.449(8) .
N21 C32 1.380(8) .
N21 C28 1.443(8) .
N21 C30 1.444(8) .
N22 C35 1.380(8) .
N22 C33 1.443(8) .
N22 C36 1.451(8) .
N23 C35 1.353(8) .
N23 C39 1.450(8) .
N23 C37 1.454(7) .
N24 C38 1.364(8) .
N24 C37 1.440(8) .
N24 C40 1.441(8) .
N25 C38 1.375(8) .
N25 C34 1.448(8) .
N25 C36 1.459(7) .
C1 H1 0.9300 .
C2 H2 0.9300 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C6 C7 1.525(9) .
C6 H6A 0.9800 .
C7 H7 0.9800 .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C12 C13 1.544(9) .
C12 H12 0.9800 .
C13 H13 0.9800 .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C18 C19 1.547(8) .
C18 H18 0.9800 .
C19 H19 0.9800 .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C24 C25 1.551(8) .
C24 H24 0.9800 .
C25 H25 0.9800 .
C27 H27A 0.9700 .
C27 H27B 0.9700 .
C28 H28A 0.9700 .
C28 H28B 0.9700 .
C30 C31 1.550(9) .
C30 H30 0.9800 .
C31 H31 0.9800 .
C33 H33A 0.9700 .
C33 H33B 0.9700 .
C34 H34A 0.9700 .
C34 H34B 0.9700 .
C36 C37 1.537(9) .
C36 H36 0.9800 .
C37 H37 0.9800 .
C39 H39A 0.9700 .
C39 H39B 0.9700 .
C40 H40A 0.9700 .
C40 H40B 0.9700 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O6 H6 O15 0.99 1.88 2.774(5) 148.7
O7 H7A O4 0.96 1.83 2.696(7) 148.7
O7 H7B O17 0.99 2.02 2.813(6) 136.2
O23 H23A O21 0.88 2.05 2.929(6) 173.8
