#------------------------------------------------------------------------------
#$Date: 2022-05-05 23:29:32 +0300 (Thu, 05 May 2022) $
#$Revision: 274970 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/43/7244320.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_7244320
loop_
_publ_author_name
'Li, Feize'
'Mei, Lei'
'Peng, Haiyue'
'Hu, Kongqiu'
'Chai, Zhifang'
'Liu, Ning'
_publ_section_title
;
 Impact of the proximity effect on uranyl coordination of conformationally
 variable weakly-bonded cucurbit[6]uril-bipyridinium pseudorotaxane
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1955
_journal_page_last               1965
_journal_paper_doi               10.1039/D1CE01330K
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety
'C18 H25 N2 O20 S2 U2, C36 H36 N24 O12, 4(H2 O), 4(O)'
_chemical_formula_sum            'C54 H69 N26 O40 S2 U2'
_chemical_formula_weight         2262.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-08-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-01-12 deposited with the CCDC.	2022-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                105.650(2)
_cell_angle_beta                 95.320(2)
_cell_angle_gamma                113.732(2)
_cell_formula_units_Z            1
_cell_length_a                   12.4914(7)
_cell_length_b                   13.5836(7)
_cell_length_c                   13.6906(6)
_cell_measurement_reflns_used    7925
_cell_measurement_temperature    292.26
_cell_measurement_theta_max      32.21
_cell_measurement_theta_min      2.92
_cell_volume                     1993.62(18)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      292.26
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14537
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.923
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.220
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.5123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0930 before and 0.0570 after correction. The Ratio of minimum to maximum transmission is 0.6861. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_description       block
_exptl_crystal_F_000             1111
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.068
_refine_diff_density_min         -1.673
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         6611
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0480
_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)+(0.0797P)²+5.2082P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5629
_reflns_number_total             6611
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce01330k2.cif
_cod_data_source_block           URCP3
_cod_depositor_comments
'Adding full bibliography for 7244318--7244323.cif.'
_cod_database_code               7244320
_shelx_shelxl_version_number     2014/7
_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   0.364
_shelx_estimated_absorpt_t_min   0.283
_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 O(H,H) groups
2. Restrained distances
 C9-C10
 1.45 with sigma of 0.02
 C8-C9
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim
Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.001
Uanis(O19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(O20) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.001
Uanis(O22) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C10(0.5) C9(0.5) H9(0.5) O19(0.5) O20(0.25) O21(0.25)
5.a Free rotating group:
 O17(H17A,H17B), O18(H18A,H18B)
5.b Rotating group:
 O4(H4A,H4B), O6(H6A,H6B)
5.c Ternary CH refined with riding coordinates:
 C19(H19), C21(H21), C20(H20), C17(H17), C22(H22), C18(H18), C9(H9)
5.d Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C23(H23A,H23B), C15(H15A,H15B), C11(H11A,H11B), C13(H13A,
 H13B), C27(H27A,H27B), C7(H7A,H7B), C8(H8A,H8B)
5.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C5(H5), C4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U -0.99251(2) -1.28295(3) 0.13347(2) 0.02249(13) Uani 1 1 d . . . . .
O13 O -0.5076(6) -0.8382(7) 0.5202(6) 0.0453(17) Uani 1 1 d . . . . .
S1 S -1.16855(18) -1.5957(2) 0.02418(16) 0.0283(5) Uani 1 1 d . . . . .
O7 O -1.1423(5) -1.6487(6) -0.0751(4) 0.0295(14) Uani 1 1 d . . . . .
O8 O -1.2977(6) -1.6429(7) 0.0103(7) 0.062(2) Uani 1 1 d . . . . .
O9 O -1.1081(8) -1.6117(7) 0.1096(5) 0.060(2) Uani 1 1 d . . . . .
O5 O -1.1196(5) -1.4721(5) 0.0389(5) 0.0334(14) Uani 1 1 d . . . . .
O10 O -1.1665(7) -1.1158(8) 0.2414(8) 0.084(3) Uani 1 1 d . . . . .
O4 O -1.2002(5) -1.3208(6) 0.1402(5) 0.0312(14) Uani 1 1 d . . . . .
H4A H -1.2071 -1.2557 0.1802 0.047 Uiso 1 1 d R U . . .
H4B H -1.2359 -1.3718 0.1764 0.047 Uiso 1 1 d R U . . .
O1 O -0.9728(5) -1.3163(6) 0.2477(5) 0.0336(15) Uani 1 1 d . . . . .
O3 O -0.9858(6) -1.1081(5) 0.2423(5) 0.0363(15) Uani 1 1 d . . . . .
O15 O -0.2798(5) -0.4608(6) 0.2492(5) 0.0317(14) Uani 1 1 d . . . . .
O6 O -0.7842(6) -1.1272(6) 0.1994(6) 0.0472(18) Uani 1 1 d . . . . .
H6A H -0.7814 -1.0623 0.1970 0.071 Uiso 1 1 d R U . . .
H6B H -0.7385 -1.1400 0.1575 0.071 Uiso 1 1 d R U . . .
O2 O -1.0149(6) -1.2469(6) 0.0211(5) 0.0375(16) Uani 1 1 d . . . . .
O14 O -0.0815(6) -0.4112(6) 0.4898(6) 0.0421(17) Uani 1 1 d . . . . .
O12 O -0.6795(6) -0.8945(6) 0.2770(5) 0.0391(16) Uani 1 1 d . . . . .
N10 N -0.3256(6) -0.6404(7) 0.2527(5) 0.0267(16) Uani 1 1 d . . . . .
O16 O -0.4660(6) -0.3364(6) 0.2316(6) 0.0444(17) Uani 1 1 d . . . . .
N11 N -0.4599(6) -0.6151(7) 0.1570(5) 0.0253(16) Uani 1 1 d . . . . .
N5 N -0.4835(6) -0.8180(7) 0.2574(6) 0.0328(18) Uani 1 1 d . . . . .
N3 N -0.7467(7) -0.6937(7) 0.1714(6) 0.0338(18) Uani 1 1 d . . . . .
O11 O -0.8784(6) -0.7630(7) 0.2726(6) 0.0493(19) Uani 1 1 d . . . . .
N1 N -0.8364(6) -0.8118(7) 0.4974(6) 0.0334(18) Uani 1 1 d . . . . .
N12 N -0.5910(6) -0.5260(7) 0.1467(6) 0.0325(18) Uani 1 1 d . . . . .
N7 N -0.3169(7) -0.6964(7) 0.5989(6) 0.0352(19) Uani 1 1 d . . . . .
N4 N -0.6179(6) -0.7874(7) 0.1694(6) 0.0310(17) Uani 1 1 d . . . . .
N8 N -0.1492(6) -0.5293(7) 0.5880(6) 0.0332(18) Uani 1 1 d . . . . .
N9 N -0.1982(6) -0.6060(7) 0.4162(6) 0.0283(16) Uani 1 1 d . . . . .
C3 C -0.8844(8) -0.9025(10) 0.4089(8) 0.039(2) Uani 1 1 d . . . . .
H3 H -0.8338 -0.9231 0.3715 0.047 Uiso 1 1 calc R U . . .
N13 N -0.6665(7) -0.4191(8) 0.2387(6) 0.0365(19) Uani 1 1 d . . . . .
C19 C -0.4156(8) -0.7561(9) 0.1953(7) 0.033(2) Uani 1 1 d . . . . .
H19 H -0.3821 -0.8000 0.1503 0.040 Uiso 1 1 calc R U . . .
N6 N -0.3647(6) -0.7785(7) 0.4273(6) 0.0327(17) Uani 1 1 d . . . . .
N2 N -0.8282(6) -0.5868(7) 0.2542(6) 0.0324(18) Uani 1 1 d . . . . .
C26 C -0.3480(7) -0.5614(8) 0.2238(6) 0.0250(19) Uani 1 1 d . . . . .
C25 C -0.5040(7) -0.5563(9) 0.1029(7) 0.032(2) Uani 1 1 d . . . . .
H25A H -0.4366 -0.4873 0.1040 0.039 Uiso 1 1 calc R U . . .
H25B H -0.5398 -0.6047 0.0307 0.039 Uiso 1 1 calc R U . . .
C21 C -0.7184(7) -0.6049(9) 0.1247(7) 0.034(2) Uani 1 1 d . . . . .
H21 H -0.7552 -0.6363 0.0499 0.041 Uiso 1 1 calc R U . . .
C23 C -0.6718(9) -0.3138(9) 0.2939(7) 0.039(2) Uani 1 1 d . . . . .
H23A H -0.7398 -0.3110 0.2565 0.047 Uiso 1 1 calc R U . . .
H23B H -0.5996 -0.2492 0.2946 0.047 Uiso 1 1 calc R U . . .
C16 C -0.4089(8) -0.7791(9) 0.5144(8) 0.034(2) Uani 1 1 d . . . . .
C6 C -0.9092(9) -0.7804(8) 0.5508(8) 0.036(2) Uani 1 1 d . . . . .
H6 H -0.8758 -0.7168 0.6112 0.044 Uiso 1 1 calc R U . . .
C15 C -0.4334(9) -0.8619(9) 0.3268(8) 0.039(2) Uani 1 1 d . . . . .
H15A H -0.4988 -0.9250 0.3367 0.046 Uiso 1 1 calc R U . . .
H15B H -0.3824 -0.8915 0.2932 0.046 Uiso 1 1 calc R U . . .
C11 C -0.9102(7) -0.5566(9) 0.3125(7) 0.035(2) Uani 1 1 d . . . . .
H11A H -0.9533 -0.5300 0.2716 0.042 Uiso 1 1 calc R U . . .
H11B H -0.9689 -0.6246 0.3216 0.042 Uiso 1 1 calc R U . . .
C20 C -0.5101(7) -0.7371(8) 0.1306(7) 0.0277(19) Uani 1 1 d . . . . .
H20 H -0.5233 -0.7753 0.0558 0.033 Uiso 1 1 calc R U . . .
C13 C -0.7350(8) -0.7971(9) 0.1280(8) 0.037(2) Uani 1 1 d . . . . .
H13A H -0.7477 -0.8164 0.0530 0.045 Uiso 1 1 calc R U . . .
H13B H -0.7971 -0.8589 0.1426 0.045 Uiso 1 1 calc R U . . .
C27 C -0.2063(7) -0.6157(9) 0.3073(7) 0.033(2) Uani 1 1 d . . . . .
H27A H -0.1860 -0.6761 0.2726 0.040 Uiso 1 1 calc R U . . .
H27B H -0.1476 -0.5449 0.3027 0.040 Uiso 1 1 calc R U . . .
C2 C -1.0064(8) -0.9653(8) 0.3725(7) 0.0290(19) Uani 1 1 d . . . . .
C12 C -0.8240(7) -0.6889(8) 0.2377(7) 0.032(2) Uani 1 1 d . . . . .
C17 C -0.2022(8) -0.6501(8) 0.5702(7) 0.031(2) Uani 1 1 d . . . . .
H17 H -0.1452 -0.6716 0.6021 0.038 Uiso 1 1 calc R U . . .
C24 C -0.5632(8) -0.4185(9) 0.2079(7) 0.033(2) Uani 1 1 d . . . . .
C28 C -0.1365(7) -0.5036(10) 0.4973(7) 0.035(2) Uani 1 1 d . . . . .
C22 C -0.7708(8) -0.5267(9) 0.1864(7) 0.033(2) Uani 1 1 d . . . . .
H22 H -0.8287 -0.5187 0.1395 0.040 Uiso 1 1 calc R U . . .
C14 C -0.6019(7) -0.8377(8) 0.2394(7) 0.030(2) Uani 1 1 d . . . . .
C5 C -1.0328(9) -0.8409(9) 0.5175(8) 0.043(2) Uani 1 1 d . . . . .
H5 H -1.0826 -0.8194 0.5554 0.052 Uiso 1 1 calc R U . . .
C4 C -1.0799(8) -0.9326(9) 0.4282(8) 0.039(2) Uani 1 1 d . . . . .
H4 H -1.1628 -0.9738 0.4044 0.046 Uiso 1 1 calc R U . . .
C1 C -1.0567(8) -1.0708(9) 0.2767(8) 0.041(2) Uani 1 1 d . . . . .
C7 C -0.7050(10) -0.7424(13) 0.5339(11) 0.070(4) Uani 1 1 d . U . . .
H7A H -0.6848 -0.7133 0.6094 0.084 Uiso 1 1 calc R U . . .
H7B H -0.6663 -0.7911 0.5116 0.084 Uiso 1 1 calc R U . . .
C18 C -0.2361(8) -0.7057(9) 0.4492(7) 0.033(2) Uani 1 1 d . . . . .
H18 H -0.1925 -0.7504 0.4257 0.040 Uiso 1 1 calc R U . . .
O17 O -0.5945(8) -1.1393(9) 0.1258(8) 0.078(3) Uani 1 1 d G . . . .
H17A H -0.6157 -1.1329 0.0679 0.117 Uiso 1 1 d G U . . .
H17B H -0.5951 -1.2046 0.1093 0.117 Uiso 1 1 d G U . . .
O18 O -0.7038(9) -1.0683(12) 0.4414(10) 0.097(4) Uani 1 1 d G . . . .
H18A H -0.6840 -1.0743 0.3832 0.145 Uiso 1 1 d G U . . .
H18B H -0.7707 -1.0655 0.4365 0.145 Uiso 1 1 d G U . . .
C10 C -0.489(4) -0.544(4) 0.449(3) 0.113(13) Uani 0.5 1 d D U P . .
C9 C -0.533(2) -0.565(3) 0.539(3) 0.117(13) Uani 0.5 1 d D U P . .
H9 H -0.4851 -0.5793 0.5892 0.140 Uiso 0.5 1 calc R U P . .
C8 C -0.6574(14) -0.646(2) 0.4955(17) 0.129(7) Uani 1 1 d D U . . .
H8A H -0.6683 -0.6765 0.4206 0.155 Uiso 1 1 calc R U . . .
H8B H -0.7056 -0.6050 0.5082 0.155 Uiso 1 1 calc R U . . .
O19 O -1.138(2) -1.822(2) 0.1533(19) 0.091(6) Uani 0.5 1 d . U P . .
O20 O -1.158(4) -1.866(4) 0.249(3) 0.082(10) Uani 0.25 1 d . U P . .
O21 O -1.220(5) -1.873(5) 0.058(4) 0.108(17) Uani 0.25 1 d . . P . .
O22 O -0.3879(17) -1.0905(19) 0.2765(17) 0.191(7) Uani 1 1 d . U . . .
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'
S S 0.1246 0.1234 '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
O7 U1 O4 148.6(2) 2_325 . ?
O7 U1 O3 138.1(2) 2_325 . ?
O7 U1 O6 70.1(2) 2_325 . ?
O5 U1 O7 78.2(2) . 2_325 ?
O5 U1 O4 70.4(2) . . ?
O5 U1 O3 143.6(2) . . ?
O5 U1 O6 148.3(2) . . ?
O4 U1 O6 141.2(2) . . ?
O1 U1 O7 89.3(2) . 2_325 ?
O1 U1 O5 91.4(3) . . ?
O1 U1 O4 91.1(2) . . ?
O1 U1 O3 87.5(3) . . ?
O1 U1 O6 87.7(3) . . ?
O1 U1 O2 178.0(3) . . ?
O3 U1 O4 73.2(2) . . ?
O3 U1 O6 68.0(2) . . ?
O2 U1 O7 92.7(3) . 2_325 ?
O2 U1 O5 89.4(3) . . ?
O2 U1 O4 87.4(2) . . ?
O2 U1 O3 90.8(3) . . ?
O2 U1 O6 92.6(3) . . ?
O8 S1 O7 107.9(4) . . ?
O8 S1 O5 108.8(4) . . ?
O9 S1 O7 109.8(4) . . ?
O9 S1 O8 114.5(5) . . ?
O9 S1 O5 109.7(4) . . ?
O5 S1 O7 105.8(4) . . ?
S1 O7 U1 139.9(3) . 2_325 ?
S1 O5 U1 151.4(4) . . ?
U1 O4 H4A 113.1 . . ?
U1 O4 H4B 114.2 . . ?
H4A O4 H4B 100.1 . . ?
C1 O3 U1 138.9(6) . . ?
U1 O6 H6A 111.0 . . ?
U1 O6 H6B 110.3 . . ?
H6A O6 H6B 103.2 . . ?
C19 N10 C27 121.8(8) . . ?
C26 N10 C19 112.6(7) . . ?
C26 N10 C27 122.5(7) . . ?
C26 N11 C25 122.1(8) . . ?
C26 N11 C20 111.2(7) . . ?
C20 N11 C25 125.0(7) . . ?
C19 N5 C15 123.3(7) . . ?
C14 N5 C19 113.0(7) . . ?
C14 N5 C15 123.5(8) . . ?
C13 N3 C21 123.5(8) . . ?
C12 N3 C21 111.9(8) . . ?
C12 N3 C13 120.9(8) . . ?
C3 N1 C7 121.0(9) . . ?
C6 N1 C3 119.5(8) . . ?
C6 N1 C7 119.4(9) . . ?
C25 N12 C21 123.9(8) . . ?
C24 N12 C25 122.5(8) . . ?
C24 N12 C21 113.5(8) . . ?
C16 N7 C23 121.5(8) . 2_446 ?
C16 N7 C17 112.4(7) . . ?
C17 N7 C23 123.4(8) . 2_446 ?
C13 N4 C20 124.2(8) . . ?
C14 N4 C20 112.9(7) . . ?
C14 N4 C13 122.5(7) . . ?
C11 N8 C17 124.3(8) 2_446 . ?
C28 N8 C11 121.2(9) . 2_446 ?
C28 N8 C17 112.9(8) . . ?
C27 N9 C18 121.9(8) . . ?
C28 N9 C27 123.4(8) . . ?
C28 N9 C18 113.8(7) . . ?
N1 C3 H3 119.3 . . ?
N1 C3 C2 121.4(9) . . ?
C2 C3 H3 119.3 . . ?
C24 N13 C23 121.8(8) . . ?
C24 N13 C22 112.2(8) . . ?
C22 N13 C23 123.9(8) . . ?
N10 C19 H19 111.7 . . ?
N10 C19 C20 102.5(8) . . ?
N5 C19 N10 115.4(8) . . ?
N5 C19 H19 111.7 . . ?
N5 C19 C20 103.3(7) . . ?
C20 C19 H19 111.7 . . ?
C16 N6 C15 121.6(8) . . ?
C16 N6 C18 113.5(8) . . ?
C15 N6 C18 123.3(8) . . ?
C12 N2 C11 122.7(8) . . ?
C12 N2 C22 113.1(8) . . ?
C22 N2 C11 122.2(8) . . ?
O15 C26 N10 125.9(8) . . ?
O15 C26 N11 125.2(8) . . ?
N10 C26 N11 108.9(8) . . ?
N11 C25 H25A 108.8 . . ?
N11 C25 H25B 108.8 . . ?
N12 C25 N11 113.7(7) . . ?
N12 C25 H25A 108.8 . . ?
N12 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
N3 C21 N12 115.3(7) . . ?
N3 C21 H21 111.8 . . ?
N3 C21 C22 103.2(7) . . ?
N12 C21 H21 111.8 . . ?
N12 C21 C22 102.2(8) . . ?
C22 C21 H21 111.8 . . ?
N7 C23 H23A 109.0 2_446 . ?
N7 C23 H23B 109.0 2_446 . ?
N13 C23 N7 112.8(8) . 2_446 ?
N13 C23 H23A 109.0 . . ?
N13 C23 H23B 109.0 . . ?
H23A C23 H23B 107.8 . . ?
O13 C16 N7 124.9(9) . . ?
O13 C16 N6 127.8(9) . . ?
N6 C16 N7 107.3(8) . . ?
N1 C6 H6 119.4 . . ?
N1 C6 C5 121.3(9) . . ?
C5 C6 H6 119.4 . . ?
N5 C15 H15A 108.7 . . ?
N5 C15 H15B 108.7 . . ?
N6 C15 N5 114.3(8) . . ?
N6 C15 H15A 108.7 . . ?
N6 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
N8 C11 N2 113.5(7) 2_446 . ?
N8 C11 H11A 108.9 2_446 . ?
N8 C11 H11B 108.9 2_446 . ?
N2 C11 H11A 108.9 . . ?
N2 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
N11 C20 N4 114.4(7) . . ?
N11 C20 C19 104.3(7) . . ?
N11 C20 H20 111.6 . . ?
N4 C20 C19 102.8(7) . . ?
N4 C20 H20 111.6 . . ?
C19 C20 H20 111.6 . . ?
N3 C13 N4 112.9(8) . . ?
N3 C13 H13A 109.0 . . ?
N3 C13 H13B 109.0 . . ?
N4 C13 H13A 109.0 . . ?
N4 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
N10 C27 H27A 108.9 . . ?
N10 C27 H27B 108.9 . . ?
N9 C27 N10 113.3(6) . . ?
N9 C27 H27A 108.9 . . ?
N9 C27 H27B 108.9 . . ?
H27A C27 H27B 107.7 . . ?
C3 C2 C4 118.4(9) . . ?
C3 C2 C1 119.8(8) . . ?
C4 C2 C1 121.8(8) . . ?
O11 C12 N3 125.8(10) . . ?
O11 C12 N2 126.8(9) . . ?
N2 C12 N3 107.4(8) . . ?
N7 C17 H17 111.2 . . ?
N7 C17 C18 103.2(7) . . ?
N8 C17 N7 115.3(7) . . ?
N8 C17 H17 111.2 . . ?
N8 C17 C18 104.1(7) . . ?
C18 C17 H17 111.2 . . ?
O16 C24 N12 126.2(9) . . ?
O16 C24 N13 126.0(10) . . ?
N12 C24 N13 107.8(8) . . ?
O14 C28 N8 127.2(10) . . ?
O14 C28 N9 126.5(8) . . ?
N9 C28 N8 106.3(9) . . ?
N13 C22 N2 115.0(8) . . ?
N13 C22 C21 103.7(7) . . ?
N13 C22 H22 111.5 . . ?
N2 C22 C21 103.0(8) . . ?
N2 C22 H22 111.5 . . ?
C21 C22 H22 111.5 . . ?
O12 C14 N5 125.5(9) . . ?
O12 C14 N4 126.6(8) . . ?
N4 C14 N5 107.8(7) . . ?
C6 C5 H5 120.8 . . ?
C4 C5 C6 118.4(9) . . ?
C4 C5 H5 120.8 . . ?
C2 C4 H4 119.5 . . ?
C5 C4 C2 120.9(9) . . ?
C5 C4 H4 119.5 . . ?
O10 C1 O3 125.6(10) . . ?
O10 C1 C2 116.3(9) . . ?
O3 C1 C2 118.1(8) . . ?
N1 C7 H7A 108.8 . . ?
N1 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C8 C7 N1 113.7(11) . . ?
C8 C7 H7A 108.8 . . ?
C8 C7 H7B 108.8 . . ?
N9 C18 N6 117.1(7) . . ?
N9 C18 C17 101.9(8) . . ?
N9 C18 H18 111.4 . . ?
N6 C18 C17 102.9(7) . . ?
N6 C18 H18 111.4 . . ?
C17 C18 H18 111.4 . . ?
H17A O17 H17B 104.5 . . ?
H18A O18 H18B 109.4 . . ?
C9 C10 C10 55(2) 2_446 2_446 ?
C9 C10 C10 50(2) . 2_446 ?
C9 C10 C9 106(3) 2_446 . ?
C10 C9 C10 74(3) 2_446 . ?
C10 C9 H9 118.8 2_446 . ?
C10 C9 H9 118.8 . . ?
C10 C9 C8 114(3) 2_446 . ?
C8 C9 C10 104(3) . . ?
C8 C9 H9 118.8 . . ?
C7 C8 H8A 108.0 . . ?
C7 C8 H8B 108.0 . . ?
C9 C8 C7 117.0(19) . . ?
C9 C8 H8A 108.0 . . ?
C9 C8 H8B 108.0 . . ?
H8A C8 H8B 107.3 . . ?
O21 O19 O20 124(3) . . ?
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 O7 2.334(6) 2_325 ?
U1 O5 2.311(6) . ?
U1 O4 2.449(5) . ?
U1 O1 1.764(6) . ?
U1 O3 2.403(6) . ?
U1 O6 2.483(6) . ?
U1 O2 1.767(6) . ?
O13 C16 1.194(11) . ?
S1 O7 1.489(6) . ?
S1 O8 1.447(7) . ?
S1 O9 1.446(7) . ?
S1 O5 1.483(7) . ?
O7 U1 2.334(5) 2_325 ?
O10 C1 1.238(12) . ?
O4 H4A 0.9468 . ?
O4 H4B 0.9493 . ?
O3 C1 1.254(11) . ?
O15 C26 1.210(11) . ?
O6 H6A 0.8775 . ?
O6 H6B 0.8778 . ?
O14 C28 1.203(12) . ?
O12 C14 1.227(11) . ?
N10 C19 1.449(12) . ?
N10 C26 1.355(11) . ?
N10 C27 1.467(10) . ?
O16 C24 1.211(12) . ?
N11 C26 1.380(10) . ?
N11 C25 1.445(11) . ?
N11 C20 1.438(12) . ?
N5 C19 1.447(12) . ?
N5 C15 1.464(12) . ?
N5 C14 1.378(11) . ?
N3 C21 1.450(12) . ?
N3 C13 1.441(13) . ?
N3 C12 1.393(12) . ?
O11 C12 1.214(11) . ?
N1 C3 1.346(13) . ?
N1 C6 1.346(12) . ?
N1 C7 1.476(13) . ?
N12 C25 1.435(11) . ?
N12 C21 1.462(11) . ?
N12 C24 1.354(13) . ?
N7 C23 1.462(11) 2_446 ?
N7 C16 1.390(13) . ?
N7 C17 1.455(11) . ?
N4 C20 1.466(10) . ?
N4 C13 1.460(10) . ?
N4 C14 1.361(12) . ?
N8 C11 1.424(12) 2_446 ?
N8 C17 1.440(12) . ?
N8 C28 1.383(11) . ?
N9 C27 1.450(11) . ?
N9 C28 1.380(13) . ?
N9 C18 1.455(12) . ?
C3 H3 0.9300 . ?
C3 C2 1.372(13) . ?
N13 C23 1.457(13) . ?
N13 C24 1.391(12) . ?
N13 C22 1.441(13) . ?
C19 H19 0.9800 . ?
C19 C20 1.555(12) . ?
N6 C16 1.361(12) . ?
N6 C15 1.439(13) . ?
N6 C18 1.456(11) . ?
N2 C11 1.471(11) . ?
N2 C12 1.368(13) . ?
N2 C22 1.451(12) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C21 H21 0.9800 . ?
C21 C22 1.564(14) . ?
C23 N7 1.462(11) 2_446 ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C6 H6 0.9300 . ?
C6 C5 1.383(14) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C11 N8 1.424(12) 2_446 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C20 H20 0.9800 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C2 C4 1.376(12) . ?
C2 C1 1.509(14) . ?
C17 H17 0.9800 . ?
C17 C18 1.559(13) . ?
C22 H22 0.9800 . ?
C5 H5 0.9300 . ?
C5 C4 1.359(14) . ?
C4 H4 0.9300 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.47(2) . ?
C18 H18 0.9800 . ?
O17 H17A 0.8494 . ?
O17 H17B 0.8503 . ?
O18 H18A 0.8496 . ?
O18 H18B 0.8504 . ?
C10 C10 1.69(7) 2_446 ?
C10 C9 1.443(19) . ?
C10 C9 1.35(5) 2_446 ?
C9 C10 1.35(5) 2_446 ?
C9 H9 0.9800 . ?
C9 C8 1.439(19) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
O19 O20 1.58(5) . ?
O19 O21 1.38(6) . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 O3 C1 O10 -17.8(19) . . . . ?
U1 O3 C1 C2 159.1(7) . . . . ?
O7 S1 O5 U1 -120.0(8) . . . . ?
O8 S1 O7 U1 -141.5(6) . . . 2_325 ?
O8 S1 O5 U1 124.4(8) . . . . ?
O9 S1 O7 U1 -16.1(8) . . . 2_325 ?
O9 S1 O5 U1 -1.6(9) . . . . ?
O5 S1 O7 U1 102.2(6) . . . 2_325 ?
N10 C19 C20 N11 1.9(8) . . . . ?
N10 C19 C20 N4 -117.9(7) . . . . ?
N5 C19 C20 N11 122.1(8) . . . . ?
N5 C19 C20 N4 2.3(9) . . . . ?
N3 C21 C22 N13 116.6(7) . . . . ?
N3 C21 C22 N2 -3.7(9) . . . . ?
N1 C3 C2 C4 0.7(15) . . . . ?
N1 C3 C2 C1 -176.1(9) . . . . ?
N1 C6 C5 C4 -1.0(16) . . . . ?
N1 C7 C8 C9 172(3) . . . . ?
N12 C21 C22 N13 -3.5(8) . . . . ?
N12 C21 C22 N2 -123.7(7) . . . . ?
N7 C17 C18 N9 119.9(7) . . . . ?
N7 C17 C18 N6 -1.9(9) . . . . ?
N8 C17 C18 N9 -0.9(8) . . . . ?
N8 C17 C18 N6 -122.6(7) . . . . ?
C3 N1 C6 C5 1.2(14) . . . . ?
C3 N1 C7 C8 90.9(16) . . . . ?
C3 C2 C4 C5 -0.5(15) . . . . ?
C3 C2 C1 O10 -172.0(11) . . . . ?
C3 C2 C1 O3 10.8(14) . . . . ?
C19 N10 C26 O15 -169.8(8) . . . . ?
C19 N10 C26 N11 7.9(9) . . . . ?
C19 N10 C27 N9 -93.8(10) . . . . ?
C19 N5 C15 N6 82.4(12) . . . . ?
C19 N5 C14 O12 175.0(9) . . . . ?
C19 N5 C14 N4 -2.4(11) . . . . ?
C26 N10 C19 N5 -117.3(8) . . . . ?
C26 N10 C19 C20 -5.9(9) . . . . ?
C26 N10 C27 N9 107.7(9) . . . . ?
C26 N11 C25 N12 -103.7(9) . . . . ?
C26 N11 C20 N4 114.2(7) . . . . ?
C26 N11 C20 C19 2.6(9) . . . . ?
C25 N11 C26 O15 5.0(13) . . . . ?
C25 N11 C26 N10 -172.6(7) . . . . ?
C25 N11 C20 N4 -80.1(10) . . . . ?
C25 N11 C20 C19 168.3(7) . . . . ?
C25 N12 C21 N3 71.9(11) . . . . ?
C25 N12 C21 C22 -176.9(7) . . . . ?
C25 N12 C24 O16 1.3(14) . . . . ?
C25 N12 C24 N13 -178.8(7) . . . . ?
C21 N3 C13 N4 91.9(10) . . . . ?
C21 N3 C12 O11 166.4(9) . . . . ?
C21 N3 C12 N2 -12.6(10) . . . . ?
C21 N12 C25 N11 -81.9(10) . . . . ?
C21 N12 C24 O16 -174.9(9) . . . . ?
C21 N12 C24 N13 5.0(10) . . . . ?
C23 N7 C16 O13 9.4(15) 2_446 . . . ?
C23 N7 C16 N6 -170.6(8) 2_446 . . . ?
C23 N7 C17 N8 -79.2(10) 2_446 . . . ?
C23 N7 C17 C18 168.0(8) 2_446 . . . ?
C23 N13 C24 O16 8.2(14) . . . . ?
C23 N13 C24 N12 -171.7(8) . . . . ?
C23 N13 C22 N2 -77.7(11) . . . . ?
C23 N13 C22 C21 170.5(8) . . . . ?
C16 N7 C17 N8 119.3(9) . . . . ?
C16 N7 C17 C18 6.5(10) . . . . ?
C16 N6 C15 N5 105.2(10) . . . . ?
C16 N6 C18 N9 -114.1(9) . . . . ?
C16 N6 C18 C17 -3.3(10) . . . . ?
C6 N1 C3 C2 -1.1(14) . . . . ?
C6 N1 C7 C8 -85.8(17) . . . . ?
C6 C5 C4 C2 0.6(16) . . . . ?
C15 N5 C19 N10 -73.1(11) . . . . ?
C15 N5 C19 C20 175.9(8) . . . . ?
C15 N5 C14 O12 -1.1(15) . . . . ?
C15 N5 C14 N4 -178.4(8) . . . . ?
C15 N6 C16 O13 -6.2(15) . . . . ?
C15 N6 C16 N7 173.9(8) . . . . ?
C15 N6 C18 N9 79.7(12) . . . . ?
C15 N6 C18 C17 -169.5(8) . . . . ?
C11 N8 C17 N7 76.5(10) 2_446 . . . ?
C11 N8 C17 C18 -171.2(7) 2_446 . . . ?
C11 N8 C28 O14 -3.1(13) 2_446 . . . ?
C11 N8 C28 N9 176.0(7) 2_446 . . . ?
C11 N2 C12 N3 173.9(7) . . . . ?
C11 N2 C12 O11 -5.1(14) . . . . ?
C11 N2 C22 N13 80.1(10) . . . . ?
C11 N2 C22 C21 -167.7(7) . . . . ?
C20 N11 C26 O15 171.2(8) . . . . ?
C20 N11 C26 N10 -6.4(9) . . . . ?
C20 N11 C25 N12 92.0(10) . . . . ?
C20 N4 C13 N3 -82.8(11) . . . . ?
C20 N4 C14 O12 -173.2(9) . . . . ?
C20 N4 C14 N5 4.1(10) . . . . ?
C13 N3 C21 N12 -80.9(11) . . . . ?
C13 N3 C21 C22 168.6(7) . . . . ?
C13 N3 C12 O11 7.2(14) . . . . ?
C13 N3 C12 N2 -171.8(7) . . . . ?
C13 N4 C20 N11 71.4(11) . . . . ?
C13 N4 C20 C19 -176.2(8) . . . . ?
C13 N4 C14 O12 -0.9(15) . . . . ?
C13 N4 C14 N5 176.4(8) . . . . ?
C27 N10 C19 N5 82.2(10) . . . . ?
C27 N10 C19 C20 -166.4(7) . . . . ?
C27 N10 C26 O15 -9.4(13) . . . . ?
C27 N10 C26 N11 168.2(7) . . . . ?
C27 N9 C28 O14 -0.7(13) . . . . ?
C27 N9 C28 N8 -179.8(7) . . . . ?
C27 N9 C18 N6 -72.1(10) . . . . ?
C27 N9 C18 C17 176.5(6) . . . . ?
C12 N3 C21 N12 120.5(9) . . . . ?
C12 N3 C21 C22 10.0(9) . . . . ?
C12 N3 C13 N4 -111.3(9) . . . . ?
C12 N2 C11 N8 108.9(10) . . . 2_446 ?
C12 N2 C22 N13 -115.8(9) . . . . ?
C12 N2 C22 C21 -3.7(9) . . . . ?
C17 N7 C16 O13 171.3(9) . . . . ?
C17 N7 C16 N6 -8.7(10) . . . . ?
C17 N8 C28 O14 -169.4(8) . . . . ?
C17 N8 C28 N9 9.7(9) . . . . ?
C24 N12 C25 N11 102.4(10) . . . . ?
C24 N12 C21 N3 -112.0(9) . . . . ?
C24 N12 C21 C22 -0.8(9) . . . . ?
C24 N13 C23 N7 -113.0(9) . . . 2_446 ?
C24 N13 C22 N2 118.5(8) . . . . ?
C24 N13 C22 C21 6.8(9) . . . . ?
C28 N8 C17 N7 -117.7(8) . . . . ?
C28 N8 C17 C18 -5.4(9) . . . . ?
C28 N9 C27 N10 -108.0(9) . . . . ?
C28 N9 C18 N6 118.3(9) . . . . ?
C28 N9 C18 C17 7.0(9) . . . . ?
C22 N13 C23 N7 84.7(10) . . . 2_446 ?
C22 N13 C24 O16 172.4(9) . . . . ?
C22 N13 C24 N12 -7.5(10) . . . . ?
C22 N2 C11 N8 -88.6(10) . . . 2_446 ?
C22 N2 C12 N3 9.9(10) . . . . ?
C22 N2 C12 O11 -169.1(9) . . . . ?
C14 N5 C19 N10 110.8(9) . . . . ?
C14 N5 C19 C20 -0.1(11) . . . . ?
C14 N5 C15 N6 -102.0(10) . . . . ?
C14 N4 C20 N11 -116.5(8) . . . . ?
C14 N4 C20 C19 -4.0(10) . . . . ?
C14 N4 C13 N3 105.7(10) . . . . ?
C4 C2 C1 O10 11.2(16) . . . . ?
C4 C2 C1 O3 -165.9(9) . . . . ?
C1 C2 C4 C5 176.3(10) . . . . ?
C7 N1 C3 C2 -177.8(10) . . . . ?
C7 N1 C6 C5 178.0(11) . . . . ?
C18 N9 C27 N10 83.5(10) . . . . ?
C18 N9 C28 O14 168.7(8) . . . . ?
C18 N9 C28 N8 -10.4(9) . . . . ?
C18 N6 C16 O13 -172.6(10) . . . . ?
C18 N6 C16 N7 7.4(11) . . . . ?
C18 N6 C15 N5 -89.7(10) . . . . ?
C10 C10 C9 C8 111(4) 2_446 . . . ?
C10 C9 C8 C7 137(3) . . . . ?
C10 C9 C8 C7 -144(4) 2_446 . . . ?
C9 C10 C9 C10 0.003(4) 2_446 . . 2_446 ?
C9 C10 C9 C8 111(4) 2_446 . . . ?
