#------------------------------------------------------------------------------
#$Date: 2016-02-04 02:20:22 +0200 (Thu, 04 Feb 2016) $
#$Revision: 175561 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/46/4344670.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_4344670
loop_
_publ_author_name
'Mäkelä, Toni'
'Minkkinen, Miia-Elina'
'Rissanen, Kari'
_publ_section_title
;
 Ion Pair Binding in the Solid-State with Ditopic Crown Ether Uranyl
 Salophen Receptors.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1339
_journal_page_last               1346
_journal_paper_doi               10.1021/acs.inorgchem.5b02780
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'C30 H32 F K N2 O10 U, 1.5(C2 H3 N), 0.5(C H4 O)'
_chemical_formula_sum            'C33.5 H38.5 F K N3.5 O10.5 U'
_chemical_formula_weight         954.31
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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
_audit_creation_date             2015-09-15
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.516(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3600(7)
_cell_length_b                   16.1948(6)
_cell_length_c                   15.6551(7)
_cell_measurement_temperature    123(2)
_cell_volume                     3570.8(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Bruker-Nonius Kappa CCD with APEXII detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0761
_diffrn_reflns_laue_measured_fraction_full 0.892
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19443
_diffrn_reflns_point_group_measured_fraction_full 0.892
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         24.992
_diffrn_reflns_theta_min         2.838
_exptl_absorpt_coefficient_mu    4.730
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0994 before and 0.0655 after correction.
The Ratio of minimum to maximum transmission is 0.5809.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_description       plate
_exptl_crystal_F_000             1872
_exptl_crystal_recrystallization_method 'Evaporation of acetonitrile'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.084
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         6255
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+17.0691P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4924
_reflns_number_total             6255
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b02780_si_013.cif
_cod_data_source_block           R2_KF
_cod_original_formula_sum        'C33.50 H38.50 F K N3.50 O10.50 U'
_cod_database_code               4344670
_shelxl_version_number           2013-4
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.331
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N4-C33
 1.13 with sigma of 0.01
 C33-C34
 1.45 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C33 \\sim O11: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.01
Uanis(N4) = Uanis(C33)
Uanis(C33) = Uanis(C34)
Uanis(O11) = Uanis(C35)
4. Others
 Fixed Sof: O11(0.5) H11A(0.5) C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5) N4(0.5)
 C33(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C17(H17), C20(H20)
5.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C35(H35A,H35B,H35C), C34(H34A,H34B,H34C)
5.d Idealised tetrahedral OH refined as rotating group:
 O11(H11A)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.32197(2) 0.27221(2) 0.47819(2) 0.02028(8) Uani 1 1 d . . . .
K1 K -0.00893(9) 0.70022(8) 0.11907(9) 0.0286(3) Uani 1 1 d . . . .
F1 F 0.4638(2) 0.2130(2) 0.5340(2) 0.0276(8) Uani 1 1 d . . . .
O1 O 0.2642(3) 0.1893(2) 0.5115(3) 0.0257(9) Uani 1 1 d . . . .
O2 O 0.3709(3) 0.3568(2) 0.4393(3) 0.0274(10) Uani 1 1 d . . . .
O3 O 0.3178(3) 0.1936(2) 0.3542(3) 0.0231(9) Uani 1 1 d . . . .
O4 O 0.3735(3) 0.3184(3) 0.6287(3) 0.0292(10) Uani 1 1 d . . . .
O5 O -0.0385(3) 0.5211(2) 0.1594(3) 0.0235(9) Uani 1 1 d . . . .
O6 O -0.1425(3) 0.5914(3) -0.0110(3) 0.0299(10) Uani 1 1 d . . . .
O7 O -0.1874(3) 0.7632(3) -0.0157(3) 0.0298(10) Uani 1 1 d . . . .
O8 O -0.0720(3) 0.8625(3) 0.1332(3) 0.0354(11) Uani 1 1 d . . . .
O9 O 0.0485(3) 0.7825(2) 0.2999(3) 0.0351(11) Uani 1 1 d . . . .
O10 O 0.0206(3) 0.6116(2) 0.3065(3) 0.0246(9) Uani 1 1 d . . . .
N1 N 0.1616(3) 0.2918(3) 0.3355(3) 0.0204(11) Uani 1 1 d . . . .
N2 N 0.2026(3) 0.3781(3) 0.4947(3) 0.0194(10) Uani 1 1 d . . . .
C1 C 0.1176(4) 0.2359(3) 0.2746(4) 0.0210(12) Uani 1 1 d . . . .
H1 H 0.0539 0.2479 0.2339 0.025 Uiso 1 1 calc R . . .
C2 C 0.1550(4) 0.1574(3) 0.2620(4) 0.0218(13) Uani 1 1 d . . . .
C3 C 0.0911(5) 0.0998(4) 0.2030(4) 0.0278(14) Uani 1 1 d . . . .
H3 H 0.0251 0.1119 0.1777 0.033 Uiso 1 1 calc R . . .
C4 C 0.1218(5) 0.0257(4) 0.1808(4) 0.0286(15) Uani 1 1 d . . . .
H4 H 0.0777 -0.0131 0.1411 0.034 Uiso 1 1 calc R . . .
C5 C 0.2187(4) 0.0095(4) 0.2182(4) 0.0263(14) Uani 1 1 d . . . .
H5 H 0.2411 -0.0406 0.2027 0.032 Uiso 1 1 calc R . . .
C6 C 0.2832(4) 0.0646(4) 0.2773(4) 0.0260(14) Uani 1 1 d . . . .
H6 H 0.3488 0.0511 0.3026 0.031 Uiso 1 1 calc R . . .
C7 C 0.2540(4) 0.1402(4) 0.3009(4) 0.0238(13) Uani 1 1 d . . . .
C8 C 0.1903(4) 0.3959(4) 0.5688(4) 0.0237(13) Uani 1 1 d . . . .
H8 H 0.1381 0.4311 0.5607 0.028 Uiso 1 1 calc R . . .
C9 C 0.2449(4) 0.3695(3) 0.6622(4) 0.0230(13) Uani 1 1 d . . . .
C10 C 0.2074(5) 0.3824(4) 0.7304(4) 0.0321(15) Uani 1 1 d . . . .
H10 H 0.1482 0.4098 0.7132 0.039 Uiso 1 1 calc R . . .
C11 C 0.2545(5) 0.3564(4) 0.8206(5) 0.0387(17) Uani 1 1 d . . . .
H11 H 0.2272 0.3634 0.8650 0.046 Uiso 1 1 calc R . . .
C12 C 0.3423(5) 0.3197(6) 0.8456(5) 0.054(2) Uani 1 1 d . . . .
H12 H 0.3763 0.3029 0.9083 0.065 Uiso 1 1 calc R . . .
C13 C 0.3815(5) 0.3071(5) 0.7826(5) 0.050(2) Uani 1 1 d . . . .
H13 H 0.4425 0.2823 0.8027 0.060 Uiso 1 1 calc R . . .
C14 C 0.3343(4) 0.3298(4) 0.6882(4) 0.0276(14) Uani 1 1 d . . . .
C15 C 0.1190(4) 0.3700(3) 0.3285(4) 0.0206(13) Uani 1 1 d . . . .
C16 C 0.1429(4) 0.4163(4) 0.4098(4) 0.0219(13) Uani 1 1 d . . . .
C17 C 0.1100(4) 0.4979(3) 0.4057(4) 0.0213(13) Uani 1 1 d . . . .
H17 H 0.1274 0.5297 0.4611 0.026 Uiso 1 1 calc R . . .
C18 C 0.0521(4) 0.5317(3) 0.3206(4) 0.0229(13) Uani 1 1 d . . . .
C19 C 0.0227(4) 0.4829(3) 0.2403(4) 0.0219(13) Uani 1 1 d . . . .
C20 C 0.0571(4) 0.4039(3) 0.2436(4) 0.0220(13) Uani 1 1 d . . . .
H20 H 0.0388 0.3723 0.1881 0.026 Uiso 1 1 calc R . . .
C21 C -0.0755(4) 0.4708(4) 0.0767(4) 0.0272(14) Uani 1 1 d . . . .
H21A H -0.0893 0.4144 0.0924 0.033 Uiso 1 1 calc R . . .
H21B H -0.0288 0.4668 0.0480 0.033 Uiso 1 1 calc R . . .
C22 C -0.1639(4) 0.5109(4) 0.0115(4) 0.0309(15) Uani 1 1 d . . . .
H22A H -0.1924 0.4775 -0.0460 0.037 Uiso 1 1 calc R . . .
H22B H -0.2103 0.5145 0.0407 0.037 Uiso 1 1 calc R . . .
C23 C -0.2254(5) 0.6304(4) -0.0785(4) 0.0337(16) Uani 1 1 d . . . .
H23A H -0.2765 0.6317 -0.0551 0.040 Uiso 1 1 calc R . . .
H23B H -0.2485 0.5983 -0.1372 0.040 Uiso 1 1 calc R . . .
C24 C -0.2024(5) 0.7148(4) -0.0964(4) 0.0338(16) Uani 1 1 d . . . .
H24A H -0.1444 0.7147 -0.1095 0.041 Uiso 1 1 calc R . . .
H24B H -0.2552 0.7381 -0.1511 0.041 Uiso 1 1 calc R . . .
C25 C -0.1652(5) 0.8464(4) -0.0273(4) 0.0340(16) Uani 1 1 d . . . .
H25A H -0.2164 0.8709 -0.0824 0.041 Uiso 1 1 calc R . . .
H25B H -0.1052 0.8489 -0.0368 0.041 Uiso 1 1 calc R . . .
C26 C -0.1548(5) 0.8934(4) 0.0592(5) 0.0373(17) Uani 1 1 d . . . .
H26A H -0.1479 0.9532 0.0503 0.045 Uiso 1 1 calc R . . .
H26B H -0.2114 0.8851 0.0735 0.045 Uiso 1 1 calc R . . .
C27 C -0.0606(5) 0.8947(4) 0.2206(5) 0.0414(18) Uani 1 1 d . . . .
H27A H -0.1103 0.8724 0.2395 0.050 Uiso 1 1 calc R . . .
H27B H -0.0663 0.9556 0.2174 0.050 Uiso 1 1 calc R . . .
C28 C 0.0361(5) 0.8699(4) 0.2900(5) 0.050(2) Uani 1 1 d . . . .
H28A H 0.0847 0.8931 0.2702 0.059 Uiso 1 1 calc R . . .
H28B H 0.0463 0.8942 0.3514 0.059 Uiso 1 1 calc R . . .
C29 C 0.0059(5) 0.7471(4) 0.3567(4) 0.0331(16) Uani 1 1 d . . . .
H29A H -0.0635 0.7422 0.3210 0.040 Uiso 1 1 calc R . . .
H29B H 0.0174 0.7826 0.4115 0.040 Uiso 1 1 calc R . . .
C30 C 0.0482(5) 0.6636(4) 0.3876(4) 0.0290(15) Uani 1 1 d . . . .
H30A H 0.1182 0.6677 0.4180 0.035 Uiso 1 1 calc R . . .
H30B H 0.0248 0.6402 0.4329 0.035 Uiso 1 1 calc R . . .
N3 N -0.1107(6) 0.4070(4) 0.3919(5) 0.060(2) Uani 1 1 d . . . .
C31 C -0.1517(6) 0.3980(5) 0.3156(6) 0.048(2) Uani 1 1 d . . . .
C32 C -0.2057(7) 0.3869(6) 0.2160(6) 0.070(3) Uani 1 1 d . . . .
H32A H -0.2685 0.3645 0.2051 0.105 Uiso 1 1 calc GR . . .
H32B H -0.1720 0.3485 0.1915 0.105 Uiso 1 1 calc GR . . .
H32C H -0.2129 0.4403 0.1844 0.105 Uiso 1 1 calc GR . . .
O11 O -0.0832(9) 0.8659(9) 0.4952(9) 0.075(3) Uani 0.5 1 d . P A 2
H11A H -0.1405 0.8596 0.4595 0.112 Uiso 0.5 1 calc GR P A 2
C35 C -0.0736(16) 0.9344(17) 0.5442(16) 0.075(3) Uani 0.5 1 d . P A 2
H35A H -0.1137 0.9778 0.5041 0.112 Uiso 0.5 1 calc GR P A 2
H35B H -0.0071 0.9521 0.5692 0.112 Uiso 0.5 1 calc GR P A 2
H35C H -0.0930 0.9239 0.5958 0.112 Uiso 0.5 1 calc GR P A 2
N4 N -0.0802(10) 0.9311(9) 0.4141(8) 0.059(2) Uani 0.5 1 d D P B 1
C33 C -0.0796(13) 0.9318(13) 0.4865(9) 0.059(2) Uani 0.5 1 d D P B 1
C34 C -0.0785(17) 0.9256(15) 0.5795(10) 0.059(2) Uani 0.5 1 d D P B 1
H34A H -0.1030 0.8715 0.5872 0.089 Uiso 0.5 1 calc GR P B 1
H34B H -0.1185 0.9691 0.5882 0.089 Uiso 0.5 1 calc GR P B 1
H34C H -0.0133 0.9321 0.6258 0.089 Uiso 0.5 1 calc GR P B 1
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'
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'
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'
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
F1 U1 K1 42.96(9) . 2_545
F1 U1 O3 77.60(12) . .
F1 U1 O4 81.59(13) . .
F1 U1 N1 146.75(13) . .
F1 U1 N2 150.27(13) . .
O1 U1 K1 114.39(13) . 2_545
O1 U1 F1 94.83(15) . .
O1 U1 O3 88.86(16) . .
O1 U1 O4 87.36(17) . .
O1 U1 N1 86.10(16) . .
O1 U1 N2 90.83(16) . .
O2 U1 K1 67.82(14) . 2_545
O2 U1 F1 89.13(16) . .
O2 U1 O1 175.80(17) . .
O2 U1 O3 90.64(16) . .
O2 U1 O4 94.60(17) . .
O2 U1 N1 89.83(16) . .
O2 U1 N2 86.39(17) . .
O3 U1 K1 44.53(9) . 2_545
O3 U1 N1 69.18(14) . .
O3 U1 N2 131.77(13) . .
O4 U1 K1 119.32(10) . 2_545
O4 U1 O3 158.45(14) . .
O4 U1 N1 131.59(14) . .
O4 U1 N2 69.52(14) . .
N1 U1 K1 106.94(10) . 2_545
N2 U1 K1 152.77(10) . 2_545
N2 U1 N1 62.69(14) . .
F1 K1 O3 61.28(10) 2 2
F1 K1 O5 111.26(11) 2 .
F1 K1 O6 77.58(11) 2 .
F1 K1 O7 80.41(11) 2 .
F1 K1 O8 102.12(12) 2 .
F1 K1 O9 136.33(12) 2 .
F1 K1 O10 148.92(11) 2 .
O3 K1 O5 99.60(12) 2 .
O3 K1 O6 119.76(13) 2 .
O3 K1 O7 138.94(12) 2 .
O3 K1 O8 113.22(13) 2 .
O3 K1 O9 88.86(12) 2 .
O3 K1 O10 95.22(11) 2 .
O5 K1 O10 49.20(10) . .
O6 K1 O5 55.53(11) . .
O6 K1 O7 59.68(12) . .
O6 K1 O9 145.56(13) . .
O6 K1 O10 100.36(11) . .
O7 K1 O5 108.11(12) . .
O7 K1 O9 112.11(12) . .
O7 K1 O10 125.81(12) . .
O8 K1 O5 141.52(13) . .
O8 K1 O6 117.19(13) . .
O8 K1 O7 58.52(12) . .
O8 K1 O9 58.96(12) . .
O8 K1 O10 106.11(12) . .
O9 K1 O5 104.21(11) . .
O9 K1 O10 55.07(10) . .
U1 F1 K1 103.82(12) . 2_545
U1 O2 K1 85.29(14) . 2_545
U1 O3 K1 100.26(13) . 2_545
C7 O3 U1 131.2(4) . .
C7 O3 K1 126.0(3) . 2_545
C14 O4 U1 135.2(4) . .
C19 O5 K1 120.8(3) . .
C19 O5 C21 116.7(4) . .
C21 O5 K1 113.1(3) . .
C22 O6 K1 124.2(3) . .
C22 O6 C23 111.1(5) . .
C23 O6 K1 115.4(3) . .
C24 O7 K1 102.9(3) . .
C25 O7 K1 102.8(3) . .
C25 O7 C24 111.8(5) . .
C26 O8 K1 118.9(4) . .
C27 O8 K1 120.3(4) . .
C27 O8 C26 112.5(5) . .
C28 O9 K1 111.7(4) . .
C29 O9 K1 112.7(3) . .
C29 O9 C28 113.2(6) . .
C18 O10 K1 119.7(3) . .
C18 O10 C30 116.7(4) . .
C30 O10 K1 116.1(3) . .
C1 N1 U1 125.9(4) . .
C1 N1 C15 118.8(5) . .
C15 N1 U1 115.3(3) . .
C8 N2 U1 127.2(4) . .
C8 N2 C16 118.4(5) . .
C16 N2 U1 114.4(3) . .
N1 C1 C2 126.8(5) . .
C3 C2 C1 117.7(5) . .
C3 C2 C7 120.1(5) . .
C7 C2 C1 122.0(5) . .
C4 C3 C2 121.6(6) . .
C3 C4 C5 118.2(6) . .
C6 C5 C4 121.4(6) . .
C5 C6 K1 158.6(4) . 2_545
C5 C6 C7 121.5(6) . .
C7 C6 K1 73.8(3) . 2_545
O3 C7 K1 37.3(3) . 2_545
O3 C7 C2 122.6(5) . .
O3 C7 C6 120.2(5) . .
C2 C7 K1 153.2(4) . 2_545
C6 C7 K1 85.0(4) . 2_545
C6 C7 C2 117.1(5) . .
N2 C8 C9 128.4(6) . .
C10 C9 C8 118.5(5) . .
C10 C9 C14 119.2(5) . .
C14 C9 C8 122.2(6) . .
C11 C10 C9 121.7(6) . .
C10 C11 K1 98.2(4) . 3_566
C10 C11 C12 118.5(7) . .
C12 C11 K1 133.2(5) . 3_566
C13 C12 C11 121.6(7) . .
C12 C13 C14 122.0(7) . .
O4 C14 C9 121.8(5) . .
O4 C14 C13 121.2(6) . .
C13 C14 C9 116.9(6) . .
C16 C15 N1 117.9(5) . .
C16 C15 C20 119.1(5) . .
C20 C15 N1 122.9(5) . .
C15 C16 N2 117.1(5) . .
C15 C16 C17 120.3(5) . .
C17 C16 N2 122.6(5) . .
C18 C17 C16 119.7(5) . .
O10 C18 K1 43.0(3) . .
O10 C18 C17 125.4(5) . .
O10 C18 C19 115.0(5) . .
C17 C18 K1 152.7(4) . .
C17 C18 C19 119.6(5) . .
C19 C18 K1 77.6(3) . .
O5 C19 K1 41.6(2) . .
O5 C19 C18 115.3(5) . .
C18 C19 K1 82.1(3) . .
C20 C19 K1 145.1(4) . .
C20 C19 O5 124.0(5) . .
C20 C19 C18 120.6(5) . .
C19 C20 C15 120.3(5) . .
O5 C21 K1 46.8(2) . .
O5 C21 C22 107.2(5) . .
C22 C21 K1 78.6(3) . .
O6 C22 K1 38.0(2) . .
O6 C22 C21 109.5(5) . .
C21 C22 K1 79.1(3) . .
O6 C23 K1 44.1(3) . .
O6 C23 C24 109.9(5) . .
C24 C23 K1 70.7(3) . .
O7 C24 K1 53.7(3) . .
O7 C24 C23 108.0(5) . .
C23 C24 K1 86.0(3) . .
O7 C25 K1 53.9(3) . .
O7 C25 C26 108.1(5) . .
C26 C25 K1 87.4(3) . .
O8 C26 K1 41.6(3) . .
O8 C26 C25 107.0(5) . .
C25 C26 K1 68.9(3) . .
O8 C27 K1 40.8(3) . .
O8 C27 C28 107.9(6) . .
C28 C27 K1 76.6(4) . .
O9 C28 K1 47.3(3) . .
O9 C28 C27 113.1(5) . .
C27 C28 K1 80.2(4) . .
O9 C29 K1 46.7(3) . .
O9 C29 C30 108.6(5) . .
C30 C29 K1 89.1(4) . .
O10 C30 K1 44.9(2) . .
O10 C30 C29 107.9(5) . .
C29 C30 K1 68.9(3) . .
N3 C31 C32 179.5(11) . .
N4 C33 C34 175(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 K1 3.9261(14) 2_545
U1 F1 2.215(3) .
U1 O1 1.798(4) .
U1 O2 1.782(4) .
U1 O3 2.301(4) .
U1 O4 2.291(4) .
U1 N1 2.601(4) .
U1 N2 2.597(5) .
K1 F1 2.755(4) 2
K1 O3 2.798(4) 2
K1 O5 3.040(4) .
K1 O6 2.851(4) .
K1 O7 2.897(4) .
K1 O8 2.839(5) .
K1 O9 2.928(5) .
K1 O10 3.132(4) .
F1 K1 2.755(4) 2_545
O2 K1 3.648(4) 2_545
O3 K1 2.798(4) 2_545
O3 C7 1.322(7) .
O4 C14 1.309(7) .
O5 C19 1.386(6) .
O5 C21 1.441(7) .
O6 C22 1.423(7) .
O6 C23 1.436(7) .
O7 C24 1.425(7) .
O7 C25 1.419(7) .
O8 C26 1.427(7) .
O8 C27 1.410(8) .
O9 C28 1.430(7) .
O9 C29 1.417(8) .
O10 C18 1.369(6) .
O10 C30 1.439(7) .
N1 C1 1.292(7) .
N1 C15 1.411(7) .
N2 C8 1.282(7) .
N2 C16 1.421(7) .
C1 C2 1.442(8) .
C2 C3 1.400(8) .
C2 C7 1.422(8) .
C3 C4 1.382(8) .
C4 C5 1.391(9) .
C5 C6 1.379(8) .
C6 K1 3.872(6) 2_545
C6 C7 1.403(8) .
C7 K1 3.732(6) 2_545
C8 C9 1.430(8) .
C9 C10 1.416(9) .
C9 C14 1.421(8) .
C10 C11 1.371(9) .
C11 K1 4.335(7) 3_566
C11 C12 1.380(10) .
C12 C13 1.361(10) .
C13 C14 1.411(9) .
C15 C16 1.394(8) .
C15 C20 1.401(8) .
C16 C17 1.407(8) .
C17 C18 1.386(8) .
C18 C19 1.399(8) .
C19 C20 1.378(8) .
C21 C22 1.483(8) .
C23 C24 1.467(9) .
C25 C26 1.505(9) .
C27 C28 1.503(9) .
C29 C30 1.494(8) .
N3 C31 1.116(9) .
C31 C32 1.455(11) .
O11 C35 1.32(3) .
N4 C33 1.129(9) .
C33 C34 1.453(9) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
U1 O3 C7 K1 -158.2(6) . 2_545
U1 O3 C7 C2 46.5(8) . .
U1 O3 C7 C6 -136.3(5) . .
U1 O4 C14 C9 -45.7(8) . .
U1 O4 C14 C13 137.8(6) . .
U1 N1 C1 C2 -12.7(8) . .
U1 N1 C15 C16 -23.6(6) . .
U1 N1 C15 C20 153.9(5) . .
U1 N2 C8 C9 7.5(9) . .
U1 N2 C16 C15 31.0(6) . .
U1 N2 C16 C17 -147.6(5) . .
K1 O3 C7 C2 -155.3(4) 2_545 .
K1 O3 C7 C6 21.9(7) 2_545 .
K1 O5 C19 C18 40.2(6) . .
K1 O5 C19 C20 -137.0(5) . .
K1 O5 C21 C22 -55.0(5) . .
K1 O6 C22 C21 -38.7(7) . .
K1 O6 C23 C24 28.8(6) . .
K1 O7 C24 C23 70.7(5) . .
K1 O7 C25 C26 -72.7(5) . .
K1 O8 C26 C25 -24.4(7) . .
K1 O8 C27 C28 41.6(7) . .
K1 O9 C28 C27 49.7(8) . .
K1 O9 C29 C30 70.1(5) . .
K1 O10 C18 C17 146.8(5) . .
K1 O10 C18 C19 -32.2(6) . .
K1 O10 C30 C29 30.8(6) . .
K1 C6 C7 O3 -13.1(4) 2_545 .
K1 C6 C7 C2 164.2(5) 2_545 .
K1 C11 C12 C13 135.4(7) 3_566 .
K1 C18 C19 O5 -25.6(4) . .
K1 C18 C19 C20 151.6(6) . .
K1 C19 C20 C15 127.5(6) . .
K1 C21 C22 O6 23.1(4) . .
K1 C23 C24 O7 -49.7(4) . .
K1 C25 C26 O8 17.1(5) . .
K1 C27 C28 O9 -34.6(6) . .
K1 C29 C30 O10 -22.8(5) . .
F1 U1 O2 K1 38.35(10) . 2_545
O3 U1 O2 K1 -39.24(11) . 2_545
O4 U1 O2 K1 119.84(11) . 2_545
O5 C19 C20 C15 179.8(5) . .
O5 C21 C22 K1 37.5(4) . .
O5 C21 C22 O6 60.6(6) . .
O6 C23 C24 K1 -20.8(5) . .
O6 C23 C24 O7 -70.5(7) . .
O7 C25 C26 K1 50.6(4) . .
O7 C25 C26 O8 67.6(6) . .
O8 C27 C28 K1 -26.5(4) . .
O8 C27 C28 O9 -61.1(8) . .
O9 C29 C30 K1 -43.2(4) . .
O9 C29 C30 O10 -66.0(6) . .
O10 C18 C19 K1 21.9(4) . .
O10 C18 C19 O5 -3.7(8) . .
O10 C18 C19 C20 173.5(5) . .
N1 U1 O2 K1 -108.42(12) . 2_545
N1 C1 C2 C3 169.2(6) . .
N1 C1 C2 C7 -16.1(9) . .
N1 C15 C16 N2 -4.9(8) . .
N1 C15 C16 C17 173.7(5) . .
N1 C15 C20 C19 -175.6(5) . .
N2 U1 O2 K1 -171.06(11) . 2_545
N2 C8 C9 C10 -167.0(6) . .
N2 C8 C9 C14 11.9(10) . .
N2 C16 C17 C18 179.8(5) . .
C1 N1 C15 C16 153.7(5) . .
C1 N1 C15 C20 -28.8(8) . .
C1 C2 C3 C4 174.6(6) . .
C1 C2 C7 K1 -31.4(12) . 2_545
C1 C2 C7 O3 2.9(9) . .
C1 C2 C7 C6 -174.4(5) . .
C2 C3 C4 C5 -0.5(9) . .
C3 C2 C7 K1 143.2(7) . 2_545
C3 C2 C7 O3 177.5(5) . .
C3 C2 C7 C6 0.2(8) . .
C3 C4 C5 C6 1.2(9) . .
C4 C5 C6 K1 -133.3(10) . 2_545
C4 C5 C6 C7 -1.3(9) . .
C5 C6 C7 K1 -163.6(5) . 2_545
C5 C6 C7 O3 -176.8(5) . .
C5 C6 C7 C2 0.6(9) . .
C7 C2 C3 C4 -0.2(9) . .
C8 N2 C16 C15 -146.2(6) . .
C8 N2 C16 C17 35.2(8) . .
C8 C9 C10 C11 177.9(6) . .
C8 C9 C14 O4 3.1(9) . .
C8 C9 C14 C13 179.7(6) . .
C9 C10 C11 K1 -147.3(5) . 3_566
C9 C10 C11 C12 2.7(11) . .
C10 C9 C14 O4 -178.0(6) . .
C10 C9 C14 C13 -1.4(9) . .
C10 C11 C12 C13 -1.8(13) . .
C11 C12 C13 C14 -0.7(14) . .
C12 C13 C14 O4 178.9(7) . .
C12 C13 C14 C9 2.3(11) . .
C14 C9 C10 C11 -1.1(9) . .
C15 N1 C1 C2 170.4(5) . .
C15 C16 C17 C18 1.2(9) . .
C16 N2 C8 C9 -175.7(6) . .
C16 C15 C20 C19 1.9(9) . .
C16 C17 C18 K1 -120.9(8) . .
C16 C17 C18 O10 -175.5(5) . .
C16 C17 C18 C19 3.5(9) . .
C17 C18 C19 K1 -157.2(5) . .
C17 C18 C19 O5 177.2(5) . .
C17 C18 C19 C20 -5.6(9) . .
C18 O10 C30 K1 149.8(6) . .
C18 O10 C30 C29 -179.5(5) . .
C18 C19 C20 C15 2.8(9) . .
C19 O5 C21 K1 -146.9(5) . .
C19 O5 C21 C22 158.1(5) . .
C20 C15 C16 N2 177.4(5) . .
C20 C15 C16 C17 -3.9(9) . .
C21 O5 C19 K1 144.2(6) . .
C21 O5 C19 C18 -175.7(5) . .
C21 O5 C19 C20 7.2(8) . .
C22 O6 C23 K1 148.2(6) . .
C22 O6 C23 C24 176.9(5) . .
C23 O6 C22 K1 -144.8(6) . .
C23 O6 C22 C21 176.4(5) . .
C24 O7 C25 K1 -109.7(4) . .
C24 O7 C25 C26 177.6(5) . .
C25 O7 C24 K1 109.6(4) . .
C25 O7 C24 C23 -179.7(5) . .
C26 O8 C27 K1 148.0(6) . .
C26 O8 C27 C28 -170.4(5) . .
C27 O8 C26 K1 -148.5(6) . .
C27 O8 C26 C25 -172.9(5) . .
C28 O9 C29 K1 128.0(5) . .
C28 O9 C29 C30 -161.9(5) . .
C29 O9 C28 K1 -128.5(5) . .
C29 O9 C28 C27 -78.8(8) . .
C30 O10 C18 K1 -148.7(6) . .
C30 O10 C18 C17 -1.9(9) . .
C30 O10 C18 C19 179.1(5) . .
