#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:51:12 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180359 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/28/7202853.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_7202853
loop_
_publ_author_name
'Bernardo Masci'
'Pierre Thuéry'
_publ_section_title
;
 Versatility of {M(30-crown-10)} (M = K+, Ba2+) as a guest in UO22+
 complexes of [3.1.3.1]- and [3.3.3]homooxacalixarenes
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              582
_journal_paper_doi               10.1039/b703172f
_journal_volume                  9
_journal_year                    2007
_chemical_formula_sum            'C132 H216 K4 O48 U2'
_chemical_formula_weight         3203.51
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.061(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.0923(7)
_cell_length_b                   24.6602(9)
_cell_length_c                   25.5672(16)
_cell_measurement_reflns_used    116766
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.96
_cell_volume                     7426.9(7)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'one φ and five ω scans with 2° steps'
_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  0.0729
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            116766
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    2.370
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_correction_T_min  0.433
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2003)'
_exptl_crystal_colour            'translucent light orange-yellow'
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3304
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.434
_refine_diff_density_min         -1.480
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     854
_refine_ls_number_reflns         14080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0433P)²+33.0564P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1208
_reflns_number_gt                10501
_reflns_number_total             14080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b703172f.txt
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7202853
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'
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
U U 0.048024(19) 0.884442(9) 0.084182(9) 0.02675(8) Uani 1 1 d . . .
K1 K -0.08827(12) 0.67770(6) 0.28719(6) 0.0383(3) Uani 1 1 d . . .
K2 K -0.10947(18) 1.02275(7) 0.05047(7) 0.0612(5) Uani 1 1 d . . .
O1 O -0.0569(3) 0.94191(16) 0.12280(15) 0.0295(9) Uani 1 1 d . . .
O2 O 0.2018(3) 0.93146(15) 0.13019(15) 0.0287(9) Uani 1 1 d . . .
O3 O 0.3370(3) 0.82045(15) 0.14294(16) 0.0287(9) Uani 1 1 d . . .
O4 O 0.1491(3) 0.83101(15) 0.03885(15) 0.0292(9) Uani 1 1 d . . .
O5 O -0.1079(3) 0.84391(16) 0.03262(16) 0.0323(10) Uani 1 1 d . . .
O6 O -0.2358(3) 0.85252(16) 0.12331(16) 0.0322(10) Uani 1 1 d . . .
O7 O 0.0334(4) 0.93487(15) 0.03085(16) 0.0328(10) Uani 1 1 d . . .
O8 O 0.0621(3) 0.83578(15) 0.13740(16) 0.0300(9) Uani 1 1 d . . .
O9 O 0.0045(5) 0.76416(19) 0.23076(19) 0.0535(13) Uani 1 1 d . . .
O10 O -0.0201(4) 0.66252(19) 0.18816(19) 0.0514(13) Uani 1 1 d . . .
O11 O 0.1216(4) 0.61468(18) 0.27645(17) 0.0410(11) Uani 1 1 d . . .
O12 O -0.0458(4) 0.57071(17) 0.32359(19) 0.0428(11) Uani 1 1 d . . .
O13 O -0.2709(4) 0.60064(18) 0.27867(19) 0.0451(12) Uani 1 1 d . . .
O14 O -0.3217(4) 0.70019(19) 0.22247(19) 0.0464(12) Uani 1 1 d . . .
O15 O -0.2699(4) 0.75111(18) 0.32537(19) 0.0451(12) Uani 1 1 d . . .
O16 O -0.1439(4) 0.69641(19) 0.42159(19) 0.0472(12) Uani 1 1 d . . .
O17 O 0.0599(4) 0.68553(18) 0.38421(18) 0.0429(11) Uani 1 1 d . . .
O18 O 0.0791(5) 0.7928(2) 0.3433(2) 0.0663(16) Uani 1 1 d . . .
O19 O 0.0265(5) 1.1116(2) 0.1228(2) 0.0606(14) Uani 1 1 d . . .
H19A H 0.0582 1.1345 0.1523 0.073 Uiso 1 1 d R . .
H19B H -0.0232 1.1250 0.1020 0.073 Uiso 1 1 d R . .
O20 O -0.1843(4) 1.13027(18) 0.0541(2) 0.0525(13) Uani 1 1 d . . .
H20A H -0.1653 1.1452 0.0223 0.063 Uiso 1 1 d R . .
H20B H -0.2389 1.1492 0.0644 0.063 Uiso 1 1 d R . .
O21 O -0.2641(5) 1.0014(2) -0.0531(2) 0.0613(15) Uani 1 1 d . . .
H21A H -0.2386 0.9680 -0.0621 0.074 Uiso 1 1 d R . .
H21B H -0.2405 1.0233 -0.0754 0.074 Uiso 1 1 d R . .
O22 O 0.2541(5) 0.7573(2) 0.2219(2) 0.0716(17) Uani 1 1 d . . .
H22A H 0.2968 0.7725 0.2034 0.086 Uiso 1 1 d R . .
H22B H 0.1671 0.7559 0.2130 0.086 Uiso 1 1 d R . .
O23 O 0.1552(4) 1.1647(2) 0.2165(2) 0.0707(16) Uani 1 1 d . . .
H23A H 0.1648 1.1947 0.2373 0.085 Uiso 1 1 d R . .
H23B H 0.2131 1.1425 0.2186 0.085 Uiso 1 1 d R . .
O24 O -0.1872(4) 0.89895(19) -0.06120(19) 0.0496(13) Uani 1 1 d . . .
H24A H -0.1670 0.8869 -0.0255 0.059 Uiso 1 1 d R . .
H24B H -0.1233 0.8983 -0.0747 0.059 Uiso 1 1 d R . .
C1 C -0.1787(5) 0.9267(2) 0.1832(2) 0.0267(13) Uani 1 1 d . . .
C2 C -0.0756(5) 0.9459(2) 0.1727(2) 0.0271(13) Uani 1 1 d . . .
C3 C 0.0013(5) 0.9716(2) 0.2142(2) 0.0260(13) Uani 1 1 d . . .
C4 C -0.0214(5) 0.9739(2) 0.2653(2) 0.0289(14) Uani 1 1 d . . .
H4 H 0.0310 0.9910 0.2926 0.035 Uiso 1 1 calc R . .
C5 C -0.1183(5) 0.9519(2) 0.2776(2) 0.0289(14) Uani 1 1 d . . .
C6 C -0.1965(5) 0.9291(2) 0.2349(2) 0.0298(14) Uani 1 1 d . . .
H6 H -0.2634 0.9148 0.2412 0.036 Uiso 1 1 calc R . .
C7 C -0.1416(5) 0.9540(3) 0.3339(3) 0.0347(15) Uani 1 1 d . . .
C8 C -0.2497(6) 0.9872(3) 0.3320(3) 0.0451(18) Uani 1 1 d . . .
H8A H -0.2677 0.9867 0.3667 0.068 Uiso 1 1 calc R . .
H8B H -0.3114 0.9717 0.3059 0.068 Uiso 1 1 calc R . .
H8C H -0.2376 1.0239 0.3222 0.068 Uiso 1 1 calc R . .
C9 C -0.0463(6) 0.9801(3) 0.3751(3) 0.0411(16) Uani 1 1 d . . .
H9A H 0.0234 0.9610 0.3760 0.062 Uiso 1 1 calc R . .
H9B H -0.0637 0.9783 0.4099 0.062 Uiso 1 1 calc R . .
H9C H -0.0382 1.0173 0.3656 0.062 Uiso 1 1 calc R . .
C10 C -0.1599(6) 0.8959(3) 0.3523(3) 0.0453(18) Uani 1 1 d . . .
H10A H -0.0912 0.8754 0.3553 0.068 Uiso 1 1 calc R . .
H10B H -0.2200 0.8790 0.3266 0.068 Uiso 1 1 calc R . .
H10C H -0.1797 0.8971 0.3866 0.068 Uiso 1 1 calc R . .
C11 C 0.1099(5) 0.9964(2) 0.2046(2) 0.0270(13) Uani 1 1 d . . .
H11A H 0.0990 1.0051 0.1667 0.032 Uiso 1 1 calc R . .
H11B H 0.1248 1.0300 0.2246 0.032 Uiso 1 1 calc R . .
C12 C 0.2124(5) 0.9596(2) 0.2208(2) 0.0267(13) Uani 1 1 d . . .
C13 C 0.2534(5) 0.9292(2) 0.1823(2) 0.0262(13) Uani 1 1 d . . .
C14 C 0.3530(5) 0.8979(2) 0.2002(2) 0.0266(13) Uani 1 1 d . . .
C15 C 0.4033(5) 0.8951(2) 0.2545(2) 0.0275(13) Uani 1 1 d . . .
H15 H 0.4676 0.8736 0.2653 0.033 Uiso 1 1 calc R . .
C16 C 0.3626(5) 0.9228(2) 0.2936(2) 0.0280(13) Uani 1 1 d . . .
C17 C 0.2668(5) 0.9556(2) 0.2750(2) 0.0276(13) Uani 1 1 d . . .
H17 H 0.2382 0.9755 0.2999 0.033 Uiso 1 1 calc R . .
C18 C 0.4178(5) 0.9216(2) 0.3536(2) 0.0294(14) Uani 1 1 d . . .
C19 C 0.3297(5) 0.9070(3) 0.3864(3) 0.0368(15) Uani 1 1 d . . .
H19C H 0.3658 0.9065 0.4239 0.055 Uiso 1 1 calc R . .
H19D H 0.2986 0.8718 0.3758 0.055 Uiso 1 1 calc R . .
H19E H 0.2699 0.9334 0.3800 0.055 Uiso 1 1 calc R . .
C20 C 0.4659(5) 0.9775(2) 0.3717(3) 0.0349(15) Uani 1 1 d . . .
H20C H 0.5226 0.9871 0.3524 0.052 Uiso 1 1 calc R . .
H20D H 0.4995 0.9767 0.4095 0.052 Uiso 1 1 calc R . .
H20E H 0.4059 1.0038 0.3646 0.052 Uiso 1 1 calc R . .
C21 C 0.5131(6) 0.8795(3) 0.3665(3) 0.0403(16) Uani 1 1 d . . .
H21C H 0.5723 0.8892 0.3488 0.060 Uiso 1 1 calc R . .
H21D H 0.4835 0.8445 0.3542 0.060 Uiso 1 1 calc R . .
H21E H 0.5432 0.8783 0.4046 0.060 Uiso 1 1 calc R . .
C22 C 0.4021(5) 0.8686(2) 0.1603(2) 0.0312(14) Uani 1 1 d . . .
H22C H 0.4017 0.8919 0.1297 0.037 Uiso 1 1 calc R . .
H22D H 0.4801 0.8588 0.1762 0.037 Uiso 1 1 calc R . .
C23 C 0.3657(5) 0.7971(2) 0.0963(2) 0.0310(14) Uani 1 1 d . . .
H23C H 0.4389 0.7792 0.1066 0.037 Uiso 1 1 calc R . .
H23D H 0.3715 0.8255 0.0708 0.037 Uiso 1 1 calc R . .
C24 C 0.2776(5) 0.7569(2) 0.0704(2) 0.0294(14) Uani 1 1 d . . .
C25 C 0.1717(5) 0.7762(2) 0.0409(2) 0.0276(13) Uani 1 1 d . . .
C26 C 0.0931(5) 0.7393(2) 0.0128(2) 0.0249(13) Uani 1 1 d . . .
C27 C 0.1190(5) 0.6845(2) 0.0171(2) 0.0290(14) Uani 1 1 d . . .
H27 H 0.0662 0.6602 -0.0020 0.035 Uiso 1 1 calc R . .
C28 C 0.2201(5) 0.6637(2) 0.0484(2) 0.0296(14) Uani 1 1 d . . .
C29 C 0.2987(5) 0.7019(2) 0.0739(2) 0.0300(14) Uani 1 1 d . . .
H29 H 0.3682 0.6898 0.0941 0.036 Uiso 1 1 calc R . .
C30 C 0.2460(5) 0.6024(2) 0.0510(3) 0.0321(14) Uani 1 1 d . . .
C31 C 0.3202(7) 0.5889(3) 0.0111(3) 0.058(2) Uani 1 1 d . . .
H31A H 0.3887 0.6099 0.0197 0.086 Uiso 1 1 calc R . .
H31B H 0.2793 0.5974 -0.0247 0.086 Uiso 1 1 calc R . .
H31C H 0.3387 0.5510 0.0134 0.086 Uiso 1 1 calc R . .
C32 C 0.3066(6) 0.5865(3) 0.1075(3) 0.0463(18) Uani 1 1 d . . .
H32A H 0.2620 0.5976 0.1323 0.069 Uiso 1 1 calc R . .
H32B H 0.3793 0.6040 0.1166 0.069 Uiso 1 1 calc R . .
H32C H 0.3167 0.5479 0.1094 0.069 Uiso 1 1 calc R . .
C33 C 0.1380(5) 0.5684(2) 0.0350(3) 0.0370(16) Uani 1 1 d . . .
H33A H 0.1563 0.5308 0.0420 0.055 Uiso 1 1 calc R . .
H33B H 0.1052 0.5733 -0.0025 0.055 Uiso 1 1 calc R . .
H33C H 0.0847 0.5796 0.0555 0.055 Uiso 1 1 calc R . .
C34 C -0.0191(5) 0.7581(2) -0.0216(2) 0.0275(13) Uani 1 1 d . . .
H34A H -0.0354 0.7377 -0.0549 0.033 Uiso 1 1 calc R . .
H34B H -0.0132 0.7961 -0.0304 0.033 Uiso 1 1 calc R . .
C35 C -0.1162(5) 0.7509(2) 0.0064(2) 0.0284(13) Uani 1 1 d . . .
C36 C -0.1571(5) 0.7945(2) 0.0313(2) 0.0296(14) Uani 1 1 d . . .
C37 C -0.2526(5) 0.7875(2) 0.0530(2) 0.0307(14) Uani 1 1 d . . .
C38 C -0.2993(5) 0.7357(3) 0.0541(2) 0.0334(15) Uani 1 1 d . . .
H38 H -0.3610 0.7312 0.0698 0.040 Uiso 1 1 calc R . .
C39 C -0.2564(5) 0.6906(2) 0.0325(2) 0.0296(14) Uani 1 1 d . . .
C40 C -0.1671(5) 0.7001(2) 0.0073(2) 0.0291(14) Uani 1 1 d . . .
H40 H -0.1401 0.6713 -0.0097 0.035 Uiso 1 1 calc R . .
C41 C -0.3065(6) 0.6338(3) 0.0343(3) 0.0383(16) Uani 1 1 d . . .
C42 C -0.2104(6) 0.5909(3) 0.0454(3) 0.055(2) Uani 1 1 d . . .
H42A H -0.1572 0.5997 0.0782 0.082 Uiso 1 1 calc R . .
H42B H -0.1722 0.5908 0.0163 0.082 Uiso 1 1 calc R . .
H42C H -0.2423 0.5557 0.0485 0.082 Uiso 1 1 calc R . .
C43 C -0.3688(7) 0.6289(3) 0.0799(3) 0.055(2) Uani 1 1 d . . .
H43A H -0.3173 0.6369 0.1135 0.082 Uiso 1 1 calc R . .
H43B H -0.3973 0.5927 0.0809 0.082 Uiso 1 1 calc R . .
H43C H -0.4310 0.6541 0.0740 0.082 Uiso 1 1 calc R . .
C44 C -0.3852(6) 0.6216(3) -0.0191(3) 0.0508(19) Uani 1 1 d . . .
H44A H -0.4134 0.5853 -0.0190 0.076 Uiso 1 1 calc R . .
H44B H -0.3447 0.6253 -0.0472 0.076 Uiso 1 1 calc R . .
H44C H -0.4477 0.6466 -0.0253 0.076 Uiso 1 1 calc R . .
C45 C -0.3038(5) 0.8353(3) 0.0735(3) 0.0341(15) Uani 1 1 d . . .
H45A H -0.3111 0.8647 0.0477 0.041 Uiso 1 1 calc R . .
H45B H -0.3791 0.8262 0.0780 0.041 Uiso 1 1 calc R . .
C46 C -0.2679(5) 0.9051(2) 0.1377(3) 0.0310(14) Uani 1 1 d . . .
H46A H -0.3400 0.9031 0.1481 0.037 Uiso 1 1 calc R . .
H46B H -0.2767 0.9293 0.1071 0.037 Uiso 1 1 calc R . .
C47 C -0.0779(6) 0.7527(3) 0.1816(3) 0.0446(18) Uani 1 1 d . . .
H47A H -0.0908 0.7845 0.1587 0.054 Uiso 1 1 calc R . .
H47B H -0.1496 0.7416 0.1892 0.054 Uiso 1 1 calc R . .
C48 C -0.0290(6) 0.7088(3) 0.1557(3) 0.0504(19) Uani 1 1 d . . .
H48A H -0.0770 0.7013 0.1207 0.060 Uiso 1 1 calc R . .
H48B H 0.0455 0.7193 0.1510 0.060 Uiso 1 1 calc R . .
C49 C 0.0763(7) 0.6300(3) 0.1828(3) 0.062(2) Uani 1 1 d . . .
H49A H 0.1436 0.6524 0.1868 0.074 Uiso 1 1 calc R . .
H49B H 0.0617 0.6127 0.1479 0.074 Uiso 1 1 calc R . .
C50 C 0.0924(8) 0.5889(3) 0.2256(3) 0.059(2) Uani 1 1 d . . .
H50A H 0.0230 0.5683 0.2227 0.071 Uiso 1 1 calc R . .
H50B H 0.1523 0.5641 0.2218 0.071 Uiso 1 1 calc R . .
C51 C 0.1476(6) 0.5784(3) 0.3205(3) 0.0422(17) Uani 1 1 d . . .
H51A H 0.1658 0.5992 0.3535 0.051 Uiso 1 1 calc R . .
H51B H 0.2145 0.5576 0.3181 0.051 Uiso 1 1 calc R . .
C52 C 0.0536(6) 0.5398(3) 0.3232(3) 0.0501(19) Uani 1 1 d . . .
H52A H 0.0399 0.5158 0.2924 0.060 Uiso 1 1 calc R . .
H52B H 0.0739 0.5180 0.3555 0.060 Uiso 1 1 calc R . .
C53 C -0.1384(6) 0.5360(3) 0.3253(3) 0.0486(19) Uani 1 1 d . . .
H53A H -0.1197 0.5133 0.3571 0.058 Uiso 1 1 calc R . .
H53B H -0.1534 0.5125 0.2941 0.058 Uiso 1 1 calc R . .
C54 C -0.2423(6) 0.5691(3) 0.3263(3) 0.0460(18) Uani 1 1 d . . .
H54A H -0.3050 0.5453 0.3286 0.055 Uiso 1 1 calc R . .
H54B H -0.2276 0.5926 0.3575 0.055 Uiso 1 1 calc R . .
C55 C -0.3779(6) 0.6256(3) 0.2732(3) 0.0459(18) Uani 1 1 d . . .
H55A H -0.3774 0.6493 0.3036 0.055 Uiso 1 1 calc R . .
H55B H -0.4362 0.5984 0.2720 0.055 Uiso 1 1 calc R . .
C56 C -0.4018(6) 0.6578(3) 0.2220(3) 0.0509(19) Uani 1 1 d . . .
H56A H -0.4007 0.6337 0.1922 0.061 Uiso 1 1 calc R . .
H56B H -0.4772 0.6734 0.2164 0.061 Uiso 1 1 calc R . .
C57 C -0.3590(6) 0.7537(3) 0.2322(3) 0.0501(19) Uani 1 1 d . . .
H57A H -0.4308 0.7608 0.2073 0.060 Uiso 1 1 calc R . .
H57B H -0.3042 0.7798 0.2251 0.060 Uiso 1 1 calc R . .
C58 C -0.3734(6) 0.7618(3) 0.2880(3) 0.0470(18) Uani 1 1 d . . .
H58A H -0.3969 0.7989 0.2923 0.056 Uiso 1 1 calc R . .
H58B H -0.4321 0.7377 0.2947 0.056 Uiso 1 1 calc R . .
C59 C -0.2777(6) 0.7613(3) 0.3789(3) 0.0486(19) Uani 1 1 d . . .
H59A H -0.3343 0.7375 0.3881 0.058 Uiso 1 1 calc R . .
H59B H -0.3022 0.7984 0.3818 0.058 Uiso 1 1 calc R . .
C60 C -0.1667(6) 0.7525(3) 0.4175(3) 0.0455(18) Uani 1 1 d . . .
H60A H -0.1068 0.7712 0.4051 0.055 Uiso 1 1 calc R . .
H60B H -0.1698 0.7670 0.4525 0.055 Uiso 1 1 calc R . .
C61 C -0.0373(6) 0.6837(3) 0.4571(3) 0.055(2) Uani 1 1 d . . .
H61A H -0.0498 0.6616 0.4866 0.066 Uiso 1 1 calc R . .
H61B H 0.0004 0.7169 0.4718 0.066 Uiso 1 1 calc R . .
C62 C 0.0350(6) 0.6539(3) 0.4270(3) 0.0474(18) Uani 1 1 d . . .
H62A H 0.1055 0.6438 0.4515 0.057 Uiso 1 1 calc R . .
H62B H -0.0035 0.6209 0.4124 0.057 Uiso 1 1 calc R . .
C63 C 0.1555(6) 0.7199(3) 0.4002(3) 0.0499(19) Uani 1 1 d . . .
H63A H 0.2232 0.6983 0.4132 0.060 Uiso 1 1 calc R . .
H63B H 0.1450 0.7435 0.4291 0.060 Uiso 1 1 calc R . .
C64 C 0.1686(6) 0.7530(3) 0.3532(3) 0.055(2) Uani 1 1 d . . .
H64A H 0.2420 0.7708 0.3608 0.066 Uiso 1 1 calc R . .
H64B H 0.1632 0.7301 0.3219 0.066 Uiso 1 1 calc R . .
C65 C 0.0797(7) 0.8277(3) 0.2999(3) 0.057(2) Uani 1 1 d . . .
H65A H 0.1523 0.8249 0.2901 0.069 Uiso 1 1 calc R . .
H65B H 0.0711 0.8648 0.3110 0.069 Uiso 1 1 calc R . .
C66 C -0.0130(6) 0.8150(3) 0.2520(3) 0.0409(17) Uani 1 1 d . . .
H66A H -0.0855 0.8151 0.2623 0.049 Uiso 1 1 calc R . .
H66B H -0.0153 0.8427 0.2249 0.049 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 U O7 179.01(17) . . ?
O8 U O1 93.10(16) . . ?
O7 U O1 86.00(16) . . ?
O8 U O5 94.00(16) . . ?
O7 U O5 86.49(17) . . ?
O1 U O5 93.13(14) . . ?
O8 U O2 91.29(16) . . ?
O7 U O2 88.22(16) . . ?
O1 U O2 85.94(14) . . ?
O5 U O2 174.68(14) . . ?
O8 U O4 91.67(16) . . ?
O7 U O4 89.23(16) . . ?
O1 U O4 175.11(13) . . ?
O5 U O4 85.48(14) . . ?
O2 U O4 95.01(14) . . ?
O17 K1 O12 74.39(14) . . ?
O17 K1 O10 123.69(15) . . ?
O12 K1 O10 95.90(14) . . ?
O17 K1 O13 116.83(14) . . ?
O12 K1 O13 59.01(13) . . ?
O10 K1 O13 102.47(15) . . ?
O17 K1 O9 98.65(14) . . ?
O12 K1 O9 141.65(15) . . ?
O10 K1 O9 56.02(14) . . ?
O13 K1 O9 144.35(15) . . ?
O17 K1 O14 146.99(14) . . ?
O12 K1 O14 115.97(14) . . ?
O10 K1 O14 87.67(14) . . ?
O13 K1 O14 57.88(14) . . ?
O9 K1 O14 90.65(14) . . ?
O17 K1 O11 74.18(13) . . ?
O12 K1 O11 57.01(13) . . ?
O10 K1 O11 55.90(13) . . ?
O13 K1 O11 107.26(13) . . ?
O9 K1 O11 84.68(14) . . ?
O14 K1 O11 138.52(13) . . ?
O17 K1 O15 92.19(13) . . ?
O12 K1 O15 121.54(13) . . ?
O10 K1 O15 134.99(14) . . ?
O13 K1 O15 80.07(13) . . ?
O9 K1 O15 96.03(14) . . ?
O14 K1 O15 55.21(13) . . ?
O11 K1 O15 166.27(13) . . ?
O7 K2 O1 138.98(14) 3_575 . ?
O7 K2 O20 79.99(13) 3_575 . ?
O1 K2 O20 134.69(14) . . ?
O7 K2 O7 80.41(13) 3_575 . ?
O1 K2 O7 60.41(12) . . ?
O20 K2 O7 157.57(15) . . ?
O7 K2 O21 68.13(13) 3_575 . ?
O1 K2 O21 119.46(14) . . ?
O20 K2 O21 93.11(16) . . ?
O7 K2 O21 89.61(14) . . ?
O7 K2 O19 87.62(14) 3_575 . ?
O1 K2 O19 95.87(14) . . ?
O20 K2 O19 56.18(15) . . ?
O7 K2 O19 112.20(14) . . ?
O21 K2 O19 144.55(14) . . ?
C2 O1 U 133.3(3) . . ?
C2 O1 K2 122.1(3) . . ?
U O1 K2 103.38(14) . . ?
C13 O2 U 129.4(3) . . ?
C23 O3 C22 111.7(4) . . ?
C25 O4 U 132.2(3) . . ?
C36 O5 U 135.4(3) . . ?
C45 O6 C46 111.6(4) . . ?
U O7 K2 148.9(2) . 3_575 ?
U O7 K2 110.05(17) . . ?
K2 O7 K2 99.60(13) 3_575 . ?
C66 O9 C47 112.2(5) . . ?
C66 O9 K1 110.5(4) . . ?
C47 O9 K1 91.2(4) . . ?
C48 O10 C49 110.7(6) . . ?
C48 O10 K1 114.7(4) . . ?
C49 O10 K1 123.8(4) . . ?
C51 O11 C50 114.2(5) . . ?
C51 O11 K1 106.9(4) . . ?
C50 O11 K1 105.8(4) . . ?
C53 O12 C52 110.5(5) . . ?
C53 O12 K1 119.4(4) . . ?
C52 O12 K1 126.3(4) . . ?
C55 O13 C54 111.3(5) . . ?
C55 O13 K1 112.9(4) . . ?
C54 O13 K1 105.2(4) . . ?
C56 O14 C57 115.9(5) . . ?
C56 O14 K1 115.1(4) . . ?
C57 O14 K1 111.7(4) . . ?
C59 O15 C58 112.1(5) . . ?
C59 O15 K1 127.0(4) . . ?
C58 O15 K1 117.9(4) . . ?
C60 O16 C61 113.2(6) . . ?
C63 O17 C62 113.8(5) . . ?
C63 O17 K1 129.2(4) . . ?
C62 O17 K1 116.7(4) . . ?
C65 O18 C64 114.7(6) . . ?
C6 C1 C2 120.0(5) . . ?
C6 C1 C46 121.2(5) . . ?
C2 C1 C46 118.8(5) . . ?
O1 C2 C3 121.9(5) . . ?
O1 C2 C1 119.9(5) . . ?
C3 C2 C1 118.1(5) . . ?
C2 C3 C4 119.5(5) . . ?
C2 C3 C11 120.7(5) . . ?
C4 C3 C11 119.8(5) . . ?
C5 C4 C3 123.4(6) . . ?
C4 C5 C6 115.9(5) . . ?
C4 C5 C7 123.0(5) . . ?
C6 C5 C7 121.1(5) . . ?
C1 C6 C5 122.8(6) . . ?
C9 C7 C5 113.3(5) . . ?
C9 C7 C8 107.7(5) . . ?
C5 C7 C8 108.9(5) . . ?
C9 C7 C10 108.7(6) . . ?
C5 C7 C10 109.0(5) . . ?
C8 C7 C10 109.0(6) . . ?
C12 C11 C3 113.6(5) . . ?
C17 C12 C13 119.5(5) . . ?
C17 C12 C11 119.1(5) . . ?
C13 C12 C11 121.4(5) . . ?
O2 C13 C12 120.8(5) . . ?
O2 C13 C14 121.0(5) . . ?
C12 C13 C14 118.1(5) . . ?
C15 C14 C13 120.0(5) . . ?
C15 C14 C22 120.8(5) . . ?
C13 C14 C22 119.3(5) . . ?
C14 C15 C16 123.4(5) . . ?
C15 C16 C17 116.0(5) . . ?
C15 C16 C18 124.6(5) . . ?
C17 C16 C18 119.3(5) . . ?
C12 C17 C16 122.9(5) . . ?
C20 C18 C16 109.8(5) . . ?
C20 C18 C21 109.3(5) . . ?
C16 C18 C21 111.5(5) . . ?
C20 C18 C19 108.0(5) . . ?
C16 C18 C19 110.6(5) . . ?
C21 C18 C19 107.6(5) . . ?
O3 C22 C14 109.8(5) . . ?
O3 C23 C24 110.6(5) . . ?
C29 C24 C25 119.8(6) . . ?
C29 C24 C23 121.3(6) . . ?
C25 C24 C23 118.8(5) . . ?
O4 C25 C26 121.1(5) . . ?
O4 C25 C24 119.9(5) . . ?
C26 C25 C24 119.0(5) . . ?
C27 C26 C25 118.8(5) . . ?
C27 C26 C34 120.1(5) . . ?
C25 C26 C34 121.1(5) . . ?
C26 C27 C28 123.7(6) . . ?
C29 C28 C27 115.9(5) . . ?
C29 C28 C30 122.2(5) . . ?
C27 C28 C30 121.8(5) . . ?
C24 C29 C28 122.6(6) . . ?
C32 C30 C33 108.2(5) . . ?
C32 C30 C31 110.3(6) . . ?
C33 C30 C31 107.1(5) . . ?
C32 C30 C28 110.1(5) . . ?
C33 C30 C28 111.9(5) . . ?
C31 C30 C28 109.1(5) . . ?
C26 C34 C35 112.2(5) . . ?
C36 C35 C40 118.7(5) . . ?
C36 C35 C34 121.1(5) . . ?
C40 C35 C34 120.2(5) . . ?
O5 C36 C35 120.4(5) . . ?
O5 C36 C37 120.0(5) . . ?
C35 C36 C37 119.6(5) . . ?
C38 C37 C36 119.6(5) . . ?
C38 C37 C45 121.1(6) . . ?
C36 C37 C45 119.2(5) . . ?
C39 C38 C37 122.2(6) . . ?
C38 C39 C40 116.4(6) . . ?
C38 C39 C41 122.3(5) . . ?
C40 C39 C41 121.3(5) . . ?
C39 C40 C35 123.1(5) . . ?
C44 C41 C43 110.9(6) . . ?
C44 C41 C39 109.1(5) . . ?
C43 C41 C39 111.1(5) . . ?
C44 C41 C42 109.0(6) . . ?
C43 C41 C42 106.6(6) . . ?
C39 C41 C42 110.2(5) . . ?
O6 C45 C37 110.6(5) . . ?
O6 C46 C1 109.5(5) . . ?
O9 C47 C48 105.5(6) . . ?
O10 C48 C47 108.8(6) . . ?
O10 C49 C50 106.7(6) . . ?
O11 C50 C49 109.7(7) . . ?
O11 C51 C52 113.9(6) . . ?
O12 C52 C51 108.2(6) . . ?
O12 C53 C54 109.9(5) . . ?
O13 C54 C53 109.0(6) . . ?
O13 C55 C56 108.0(6) . . ?
O14 C56 C55 112.7(6) . . ?
O14 C57 C58 113.6(6) . . ?
O15 C58 C57 110.1(6) . . ?
O15 C59 C60 111.6(6) . . ?
O16 C60 C59 108.8(6) . . ?
O16 C61 C62 109.3(6) . . ?
O17 C62 C61 112.2(6) . . ?
O17 C63 C64 108.8(6) . . ?
O18 C64 C63 107.6(6) . . ?
O18 C65 C66 112.4(7) . . ?
O9 C66 C65 110.8(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U O8 1.793(4) . ?
U O7 1.824(4) . ?
U O1 2.272(4) . ?
U O5 2.274(4) . ?
U O2 2.280(4) . ?
U O4 2.284(4) . ?
U K2 3.9066(16) . ?
U K2 4.3355(16) 3_575 ?
K1 O17 2.719(5) . ?
K1 O12 2.806(4) . ?
K1 O10 2.859(5) . ?
K1 O13 2.884(5) . ?
K1 O9 2.936(5) . ?
K1 O14 2.984(5) . ?
K1 O11 3.041(5) . ?
K1 O15 3.166(5) . ?
K2 O7 2.669(4) 3_575 ?
K2 O1 2.696(4) . ?
K2 O20 2.810(5) . ?
K2 O7 2.885(4) . ?
K2 O21 2.923(6) . ?
K2 O19 3.090(6) . ?
K2 K2 4.245(3) 3_575 ?
K2 U 4.3357(16) 3_575 ?
O1 C2 1.348(7) . ?
O2 C13 1.339(7) . ?
O3 C23 1.437(7) . ?
O3 C22 1.438(7) . ?
O4 C25 1.377(7) . ?
O5 C36 1.352(7) . ?
O6 C45 1.415(7) . ?
O6 C46 1.425(7) . ?
O7 K2 2.669(4) 3_575 ?
O9 C66 1.402(8) . ?
O9 C47 1.445(8) . ?
O10 C48 1.400(8) . ?
O10 C49 1.446(9) . ?
O11 C51 1.417(8) . ?
O11 C50 1.418(8) . ?
O12 C53 1.419(8) . ?
O12 C52 1.424(8) . ?
O13 C55 1.412(8) . ?
O13 C54 1.420(8) . ?
O14 C56 1.422(8) . ?
O14 C57 1.434(8) . ?
O15 C59 1.416(8) . ?
O15 C58 1.417(8) . ?
O16 C60 1.411(8) . ?
O16 C61 1.434(8) . ?
O17 C63 1.417(8) . ?
O17 C62 1.429(8) . ?
O18 C65 1.406(9) . ?
O18 C64 1.438(9) . ?
C1 C6 1.386(8) . ?
C1 C2 1.417(8) . ?
C1 C46 1.495(8) . ?
C2 C3 1.395(8) . ?
C3 C4 1.397(8) . ?
C3 C11 1.517(8) . ?
C4 C5 1.390(8) . ?
C5 C6 1.392(8) . ?
C5 C7 1.528(8) . ?
C7 C9 1.517(9) . ?
C7 C8 1.533(9) . ?
C7 C10 1.541(9) . ?
C11 C12 1.516(8) . ?
C12 C17 1.398(8) . ?
C12 C13 1.413(8) . ?
C13 C14 1.416(8) . ?
C14 C15 1.385(8) . ?
C14 C22 1.479(8) . ?
C15 C16 1.390(8) . ?
C16 C17 1.406(8) . ?
C16 C18 1.528(8) . ?
C18 C20 1.526(8) . ?
C18 C21 1.531(8) . ?
C18 C19 1.540(8) . ?
C23 C24 1.494(8) . ?
C24 C29 1.380(8) . ?
C24 C25 1.414(8) . ?
C25 C26 1.393(8) . ?
C26 C27 1.385(8) . ?
C26 C34 1.514(8) . ?
C27 C28 1.399(8) . ?
C28 C29 1.391(8) . ?
C28 C30 1.542(8) . ?
C30 C32 1.516(9) . ?
C30 C33 1.528(9) . ?
C30 C31 1.539(9) . ?
C34 C35 1.517(8) . ?
C35 C36 1.396(8) . ?
C35 C40 1.397(8) . ?
C36 C37 1.401(8) . ?
C37 C38 1.398(8) . ?
C37 C45 1.483(8) . ?
C38 C39 1.392(8) . ?
C39 C40 1.397(8) . ?
C39 C41 1.533(9) . ?
C41 C44 1.508(10) . ?
C41 C43 1.530(9) . ?
C41 C42 1.548(10) . ?
C47 C48 1.461(10) . ?
C49 C50 1.470(11) . ?
C51 C52 1.495(10) . ?
C53 C54 1.503(10) . ?
C55 C56 1.502(10) . ?
C57 C58 1.490(10) . ?
C59 C60 1.492(10) . ?
C61 C62 1.483(10) . ?
C63 C64 1.492(10) . ?
C65 C66 1.495(10) . ?
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
_geom_hbond_site_symmetry_A
O19 H19B O20 0.78 2.06 2.789(8) 155.8 .
O19 H19A O23 0.95 1.94 2.861(8) 163.4 .
O20 H20A O4 0.97 1.72 2.682(6) 172.4 3_575
O20 H20B O16 0.90 1.93 2.819(7) 172.2 2_455
O21 H21B O2 0.88 1.93 2.804(6) 174.0 3_575
O21 H21A O24 0.93 1.81 2.717(7) 164.8 .
O22 H22A O3 0.86 2.09 2.902(6) 157.1 .
O22 H22B O9 1.03 2.12 3.081(8) 154.3 .
O23 H23B O11 0.88 2.09 2.936(7) 160.8 2
O23 H23A O22 0.90 1.99 2.850(8) 157.7 2
O24 H24A O5 0.94 1.83 2.734(6) 160.0 .
O24 H24B O19 0.92 1.90 2.777(7) 160.9 3_575
