#------------------------------------------------------------------------------
#$Date: 2022-05-05 23:29:32 +0300 (Thu, 05 May 2022) $
#$Revision: 274970 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/43/7244318.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_7244318
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         'C36 H36 N24 O12, C19 H22 N2 O4, 16(H2 O)'
_chemical_formula_sum            'C55 H90 N26 O32'
_chemical_formula_weight         1627.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-07-28
_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                90
_cell_angle_beta                 99.494(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0060(13)
_cell_length_b                   20.6811(16)
_cell_length_c                   22.944(2)
_cell_measurement_reflns_used    9405
_cell_measurement_temperature    292.52
_cell_measurement_theta_max      31.41
_cell_measurement_theta_min      2.99
_cell_volume                     7022.9(10)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      292.52
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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  0.0512
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            88830
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.415
_diffrn_reflns_theta_min         2.988
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1101 before and 0.0628 after correction. The Ratio of minimum to maximum transmission is 0.8681. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       block
_exptl_crystal_F_000             3432
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         11573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0556
_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)+(0.0559P)²+9.4104P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8074
_reflns_number_total             11573
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce01330k2.cif
_cod_data_source_block           C7BPCA3_CB6
_cod_depositor_comments
'Adding full bibliography for 7244318--7244323.cif.'
_cod_original_cell_volume        7022.8(10)
_cod_database_code               7244318
_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   0.987
_shelx_estimated_absorpt_t_min   0.939
_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. Others
 Fixed Sof: H10A(0.5) H10B(0.5)
3.a Free rotating group:
 O17(H17A,H17B), O9(H9C,H9D), O15(H15A,H15B)
3.b Ternary CH refined with riding coordinates:
 C17(H17), C28(H28), C27(H27), C20(H20), C19(H19), C18(H18)
3.c Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C21(H21A,H21B), C25(H25A,H25B), C23(H23A,H23B), C12(H12A,
 H12B), C16(H16A,H16B), C8(H8A,H8B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B)
3.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
O8 O 0.00300(8) 0.61799(6) 0.59133(5) 0.0315(3) Uani 1 1 d . . . . .
O1 O -0.45170(13) 0.70126(10) 0.86821(9) 0.0662(5) Uani 1 1 d . . . . .
N1 N -0.18008(11) 0.74894(7) 0.90988(7) 0.0340(3) Uani 1 1 d . . . . .
O3 O -0.01732(9) 0.92637(6) 0.89641(6) 0.0360(3) Uani 1 1 d . . . . .
O5 O -0.29894(10) 0.78507(7) 0.75404(6) 0.0384(3) Uani 1 1 d . . . . .
O4 O -0.21724(9) 0.93958(7) 0.79953(6) 0.0371(3) Uani 1 1 d . . . . .
O7 O 0.20817(9) 0.62169(7) 0.69339(6) 0.0370(3) Uani 1 1 d . . . . .
O6 O -0.08846(9) 0.77221(7) 0.54523(6) 0.0400(3) Uani 1 1 d . . . . .
N2 N 0.12922(10) 0.93274(7) 0.87848(6) 0.0293(3) Uani 1 1 d . . . . .
N10 N -0.13695(9) 0.62237(7) 0.62095(6) 0.0256(3) Uani 1 1 d . . . . .
N5 N -0.22507(10) 0.94155(7) 0.69825(6) 0.0298(3) Uani 1 1 d . . . . .
N12 N 0.11136(10) 0.56446(7) 0.74274(6) 0.0292(3) Uani 1 1 d . . . . .
N4 N -0.11696(10) 0.99750(7) 0.75417(6) 0.0292(3) Uani 1 1 d . . . . .
N6 N -0.28115(10) 0.83511(7) 0.66685(6) 0.0283(3) Uani 1 1 d . . . . .
N7 N -0.27922(10) 0.72778(7) 0.67020(6) 0.0284(3) Uani 1 1 d . . . . .
N11 N -0.02863(9) 0.56352(7) 0.67334(6) 0.0280(3) Uani 1 1 d . . . . .
N3 N 0.02308(10) 0.99156(7) 0.82327(6) 0.0276(3) Uani 1 1 d . . . . .
N13 N 0.22012(10) 0.62316(7) 0.79535(6) 0.0300(3) Uani 1 1 d . . . . .
O17 O -0.39357(11) 0.59435(9) 0.56499(8) 0.0515(4) Uani 1 1 d G . . . .
H17A H -0.4465 0.6053 0.5698 0.077 Uiso 1 1 d G U . . .
H17B H -0.4013 0.5604 0.5441 0.077 Uiso 1 1 d G U . . .
N9 N -0.20510(10) 0.72312(7) 0.58270(7) 0.0298(3) Uani 1 1 d . . . . .
N8 N -0.19581(10) 0.83022(7) 0.58546(7) 0.0300(3) Uani 1 1 d . . . . .
O9 O 0.11523(13) 0.96808(9) 0.51748(9) 0.0604(5) Uani 1 1 d G . . . .
H9C H 0.1016 0.9429 0.4881 0.091 Uiso 1 1 d G U . . .
H9D H 0.0850 0.9538 0.5430 0.091 Uiso 1 1 d G U . . .
O10 O -0.46793(13) 0.89175(11) 0.53620(8) 0.0614(5) Uani 1 1 d . . . . .
O2 O -0.42609(12) 0.61016(9) 0.91916(9) 0.0632(5) Uani 1 1 d . . . . .
O11 O -0.38164(14) 1.00999(10) 0.55593(8) 0.0606(5) Uani 1 1 d . . . . .
O16 O -0.19877(16) 0.49197(10) 0.54253(10) 0.0655(5) Uani 1 1 d . . . . .
O15 O -0.32748(14) 0.89332(12) 0.87557(9) 0.0724(6) Uani 1 1 d G . . . .
H15A H -0.3775 0.8747 0.8634 0.109 Uiso 1 1 d G U . . .
H15B H -0.3009 0.9013 0.8463 0.109 Uiso 1 1 d G U . . .
C17 C 0.18031(11) 0.97428(8) 0.84478(7) 0.0269(3) Uani 1 1 d . . . . .
H17 H 0.2223 1.0021 0.8708 0.032 Uiso 1 1 calc R U . . .
C24 C -0.04877(11) 0.60314(7) 0.62531(7) 0.0243(3) Uani 1 1 d . . . . .
C11 C 0.03914(11) 0.94813(8) 0.86876(7) 0.0266(3) Uani 1 1 d . . . . .
C26 C 0.18254(11) 0.60538(8) 0.73897(7) 0.0270(3) Uani 1 1 d . . . . .
C13 C -0.18866(11) 0.95715(8) 0.75507(7) 0.0270(3) Uani 1 1 d . . . . .
C28 C 0.18420(11) 0.58575(8) 0.83968(7) 0.0249(3) Uani 1 1 d . . . . .
H28 H 0.2308 0.5581 0.8619 0.030 Uiso 1 1 calc R U . . .
C27 C 0.10860(11) 0.54489(7) 0.80282(7) 0.0250(3) Uani 1 1 d . . . . .
H27 H 0.1207 0.4985 0.8082 0.030 Uiso 1 1 calc R U . . .
C20 C -0.28369(11) 0.74186(8) 0.60775(7) 0.0260(3) Uani 1 1 d . . . . .
H20 H -0.3396 0.7254 0.5843 0.031 Uiso 1 1 calc R U . . .
C19 C -0.27973(11) 0.81684(8) 0.60627(7) 0.0259(3) Uani 1 1 d . . . . .
H19 H -0.3315 0.8349 0.5796 0.031 Uiso 1 1 calc R U . . .
O12 O -0.50529(17) 0.82831(13) 0.63803(10) 0.0758(6) Uani 1 1 d . . . . .
C18 C 0.10581(11) 1.01453(8) 0.80565(7) 0.0259(3) Uani 1 1 d . . . . .
H18 H 0.1142 1.0610 0.8129 0.031 Uiso 1 1 calc R U . . .
C14 C -0.30272(11) 0.90007(8) 0.68351(8) 0.0287(3) Uani 1 1 d . . . . .
H14A H -0.3438 0.9194 0.6511 0.034 Uiso 1 1 calc R U . . .
H14B H -0.3339 0.8977 0.7172 0.034 Uiso 1 1 calc R U . . .
C21 C -0.16924(13) 0.89469(8) 0.57087(7) 0.0311(3) Uani 1 1 d . . . . .
H21A H -0.2220 0.9173 0.5506 0.037 Uiso 1 1 calc R U . . .
H21B H -0.1262 0.8914 0.5438 0.037 Uiso 1 1 calc R U . . .
C25 C 0.05916(12) 0.53420(8) 0.69154(7) 0.0279(3) Uani 1 1 d . . . . .
H25A H 0.0509 0.4889 0.7002 0.033 Uiso 1 1 calc R U . . .
H25B H 0.0929 0.5365 0.6590 0.033 Uiso 1 1 calc R U . . .
C22 C -0.15514(11) 0.77503(8) 0.56905(7) 0.0280(3) Uani 1 1 d . . . . .
C15 C -0.28746(11) 0.78280(8) 0.70276(7) 0.0274(3) Uani 1 1 d . . . . .
C23 C -0.18398(12) 0.65707(8) 0.57009(7) 0.0283(3) Uani 1 1 d . . . . .
H23A H -0.1469 0.6568 0.5392 0.034 Uiso 1 1 calc R U . . .
H23B H -0.2397 0.6344 0.5551 0.034 Uiso 1 1 calc R U . . .
C12 C -0.06326(11) 1.02346(8) 0.80675(7) 0.0281(3) Uani 1 1 d . . . . .
H12A H -0.0971 1.0198 0.8392 0.034 Uiso 1 1 calc R U . . .
H12B H -0.0529 1.0691 0.8006 0.034 Uiso 1 1 calc R U . . .
C2 C -0.30545(13) 0.68422(9) 0.92267(8) 0.0334(4) Uani 1 1 d . . . . .
C16 C -0.29902(12) 0.66426(8) 0.69176(8) 0.0307(3) Uani 1 1 d . . . . .
H16A H -0.3254 0.6693 0.7274 0.037 Uiso 1 1 calc R U . . .
H16B H -0.3435 0.6432 0.6623 0.037 Uiso 1 1 calc R U . . .
C3 C -0.26548(13) 0.72979(9) 0.89120(8) 0.0339(4) Uani 1 1 d . . . . .
H3 H -0.2980 0.7473 0.8568 0.041 Uiso 1 1 calc R U . . .
C4 C -0.25473(14) 0.65874(10) 0.97354(9) 0.0396(4) Uani 1 1 d . . . . .
H4 H -0.2800 0.6278 0.9953 0.047 Uiso 1 1 calc R U . . .
C5 C -0.16734(15) 0.67896(11) 0.99196(10) 0.0448(5) Uani 1 1 d . . . . .
H5 H -0.1336 0.6623 1.0263 0.054 Uiso 1 1 calc R U . . .
C8 C -0.08778(14) 0.75870(9) 0.83260(9) 0.0370(4) Uani 1 1 d . . . . .
H8A H -0.1301 0.7299 0.8088 0.044 Uiso 1 1 calc R U . . .
H8B H -0.0414 0.7323 0.8556 0.044 Uiso 1 1 calc R U . . .
C6 C -0.13048(14) 0.72424(10) 0.95892(10) 0.0416(4) Uani 1 1 d . . . . .
H6 H -0.0711 0.7378 0.9706 0.050 Uiso 1 1 calc R U . . .
C1 C -0.40272(15) 0.66372(11) 0.90177(9) 0.0434(4) Uani 1 1 d . . . . .
C7 C -0.13664(15) 0.79577(9) 0.87391(10) 0.0420(5) Uani 1 1 d . . . . .
H7A H -0.0944 0.8229 0.8996 0.050 Uiso 1 1 calc R U . . .
H7B H -0.1822 0.8234 0.8515 0.050 Uiso 1 1 calc R U . . .
C9 C -0.04450(15) 0.80181(9) 0.79213(9) 0.0393(4) Uani 1 1 d . . . . .
H9A H -0.0902 0.8295 0.7700 0.047 Uiso 1 1 calc R U . . .
H9B H 0.0002 0.8292 0.8155 0.047 Uiso 1 1 calc R U . . .
C10 C 0.0000 0.76241(14) 0.7500 0.0443(7) Uani 1 2 d S T P . .
H10A H -0.0451 0.7347 0.7273 0.053 Uiso 0.5 1 calc R U P . .
H10B H 0.0451 0.7347 0.7727 0.053 Uiso 0.5 1 calc R U P . .
H11A H -0.355(2) 1.0109(17) 0.5229(16) 0.083(10) Uiso 1 1 d . . . . .
H11B H -0.418(3) 1.047(2) 0.558(2) 0.131(16) Uiso 1 1 d . . . . .
H16C H -0.178(2) 0.4626(16) 0.5731(14) 0.070(10) Uiso 1 1 d . . . . .
H16D H -0.270(3) 0.487(2) 0.5353(18) 0.117(14) Uiso 1 1 d . . . . .
H10C H -0.479(3) 0.884(2) 0.494(2) 0.113(14) Uiso 1 1 d . . . . .
H10D H -0.449(3) 0.939(2) 0.542(2) 0.126(16) Uiso 1 1 d . . . . .
H12C H -0.490(3) 0.841(2) 0.599(2) 0.110(13) Uiso 1 1 d . . . . .
O13 O -0.5000 0.89013(13) 0.7500 0.0631(7) Uani 1 2 d S T P . .
O14 O -0.5000 0.66000(13) 0.7500 0.0643(7) Uani 1 2 d S T P . .
H14 H -0.485(2) 0.6860(16) 0.7818(14) 0.078(10) Uiso 1 1 d . . . . .
H12D H -0.509(3) 0.784(2) 0.6329(19) 0.105(14) Uiso 1 1 d . . . . .
H13 H -0.500(2) 0.8606(18) 0.7818(14) 0.088(11) Uiso 1 1 d . . . . .
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'
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
C3 N1 C6 121.54(16) . . ?
C3 N1 C7 119.78(17) . . ?
C6 N1 C7 118.57(18) . . ?
C11 N2 C17 111.61(14) . . ?
C11 N2 C21 121.57(14) . 2_556 ?
C21 N2 C17 124.16(15) 2_556 . ?
C24 N10 C28 111.63(13) . 2_556 ?
C24 N10 C23 122.59(13) . . ?
C23 N10 C28 122.45(14) . 2_556 ?
C13 N5 C17 112.47(14) . 2_556 ?
C13 N5 C14 123.01(14) . . ?
C14 N5 C17 124.42(14) . 2_556 ?
C26 N12 C27 112.15(14) . . ?
C26 N12 C25 122.57(13) . . ?
C25 N12 C27 123.95(14) . . ?
C13 N4 C18 112.11(14) . 2_556 ?
C13 N4 C12 123.31(13) . . ?
C12 N4 C18 124.44(14) . 2_556 ?
C19 N6 C14 122.43(14) . . ?
C15 N6 C19 112.65(14) . . ?
C15 N6 C14 122.16(13) . . ?
C15 N7 C20 112.06(13) . . ?
C15 N7 C16 121.39(13) . . ?
C16 N7 C20 122.59(14) . . ?
C24 N11 C27 112.14(13) . 2_556 ?
C24 N11 C25 123.61(13) . . ?
C25 N11 C27 123.35(13) . 2_556 ?
C11 N3 C18 112.17(14) . . ?
C11 N3 C12 122.44(13) . . ?
C18 N3 C12 123.29(13) . . ?
C26 N13 C28 112.04(14) . . ?
C26 N13 C16 122.99(14) . 2_556 ?
C16 N13 C28 123.77(14) 2_556 . ?
H17A O17 H17B 104.5 . . ?
C22 N9 C20 113.07(14) . . ?
C22 N9 C23 123.22(14) . . ?
C23 N9 C20 123.62(14) . . ?
C19 N8 C21 122.78(14) . . ?
C22 N8 C19 112.43(14) . . ?
C22 N8 C21 123.34(14) . . ?
H9C O9 H9D 104.4 . . ?
H10C O10 H10D 106(3) . . ?
H11A O11 H11B 111(3) . . ?
H16C O16 H16D 105(3) . . ?
H15A O15 H15B 109.6 . . ?
N2 C17 H17 111.4 . . ?
N2 C17 C18 103.36(13) . . ?
N5 C17 N2 115.45(14) 2_556 . ?
N5 C17 H17 111.4 2_556 . ?
N5 C17 C18 103.09(13) 2_556 . ?
C18 C17 H17 111.4 . . ?
O8 C24 N10 125.89(15) . . ?
O8 C24 N11 125.70(15) . . ?
N11 C24 N10 108.40(13) . . ?
O3 C11 N2 125.34(16) . . ?
O3 C11 N3 125.91(16) . . ?
N3 C11 N2 108.75(13) . . ?
O7 C26 N12 125.55(16) . . ?
O7 C26 N13 126.51(16) . . ?
N13 C26 N12 107.93(13) . . ?
O4 C13 N5 125.78(16) . . ?
O4 C13 N4 125.39(16) . . ?
N4 C13 N5 108.79(13) . . ?
N10 C28 N13 115.76(13) 2_556 . ?
N10 C28 H28 111.2 2_556 . ?
N10 C28 C27 103.63(12) 2_556 . ?
N13 C28 H28 111.2 . . ?
N13 C28 C27 103.39(12) . . ?
C27 C28 H28 111.2 . . ?
N12 C27 N11 116.20(14) . 2_556 ?
N12 C27 C28 103.56(12) . . ?
N12 C27 H27 111.1 . . ?
N11 C27 C28 103.06(12) 2_556 . ?
N11 C27 H27 111.1 2_556 . ?
C28 C27 H27 111.1 . . ?
N7 C20 H20 111.6 . . ?
N7 C20 C19 103.06(13) . . ?
N9 C20 N7 115.46(14) . . ?
N9 C20 H20 111.6 . . ?
N9 C20 C19 102.84(13) . . ?
C19 C20 H20 111.6 . . ?
N6 C19 N8 114.83(14) . . ?
N6 C19 C20 103.51(12) . . ?
N6 C19 H19 111.4 . . ?
N8 C19 C20 103.71(12) . . ?
N8 C19 H19 111.4 . . ?
C20 C19 H19 111.4 . . ?
H12C O12 H12D 99(3) . . ?
N4 C18 C17 103.41(12) 2_556 . ?
N4 C18 H18 111.5 2_556 . ?
N3 C18 N4 114.95(14) . 2_556 ?
N3 C18 C17 103.36(12) . . ?
N3 C18 H18 111.5 . . ?
C17 C18 H18 111.5 . . ?
N5 C14 N6 114.01(13) . . ?
N5 C14 H14A 108.8 . . ?
N5 C14 H14B 108.8 . . ?
N6 C14 H14A 108.8 . . ?
N6 C14 H14B 108.8 . . ?
H14A C14 H14B 107.6 . . ?
N2 C21 H21A 108.7 2_556 . ?
N2 C21 H21B 108.7 2_556 . ?
N8 C21 N2 114.10(14) . 2_556 ?
N8 C21 H21A 108.7 . . ?
N8 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
N12 C25 N11 113.53(13) . . ?
N12 C25 H25A 108.9 . . ?
N12 C25 H25B 108.9 . . ?
N11 C25 H25A 108.9 . . ?
N11 C25 H25B 108.9 . . ?
H25A C25 H25B 107.7 . . ?
O6 C22 N9 125.72(16) . . ?
O6 C22 N8 126.64(16) . . ?
N9 C22 N8 107.60(13) . . ?
O5 C15 N6 125.76(16) . . ?
O5 C15 N7 126.53(16) . . ?
N6 C15 N7 107.70(13) . . ?
N10 C23 H23A 108.8 . . ?
N10 C23 H23B 108.8 . . ?
N9 C23 N10 113.65(13) . . ?
N9 C23 H23A 108.8 . . ?
N9 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
N4 C12 N3 113.74(13) . . ?
N4 C12 H12A 108.8 . . ?
N4 C12 H12B 108.8 . . ?
N3 C12 H12A 108.8 . . ?
N3 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
C3 C2 C4 118.22(18) . . ?
C3 C2 C1 120.15(18) . . ?
C4 C2 C1 121.63(17) . . ?
N7 C16 H16A 108.9 . . ?
N7 C16 H16B 108.9 . . ?
N13 C16 N7 113.23(14) 2_556 . ?
N13 C16 H16A 108.9 2_556 . ?
N13 C16 H16B 108.9 2_556 . ?
H16A C16 H16B 107.7 . . ?
N1 C3 C2 120.53(18) . . ?
N1 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C2 C4 H4 119.8 . . ?
C5 C4 C2 120.40(18) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 H5 120.4 . . ?
C4 C5 C6 119.1(2) . . ?
C6 C5 H5 120.4 . . ?
H8A C8 H8B 107.8 . . ?
C7 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
C7 C8 C9 113.04(16) . . ?
C9 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
N1 C6 C5 120.2(2) . . ?
N1 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
O1 C1 O2 125.7(2) . . ?
O1 C1 C2 117.36(19) . . ?
O2 C1 C2 116.9(2) . . ?
N1 C7 C8 108.76(15) . . ?
N1 C7 H7A 109.9 . . ?
N1 C7 H7B 109.9 . . ?
C8 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 108.0 . . ?
C10 C9 C8 110.94(17) . . ?
C10 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
C9 C10 C9 114.3(2) . 2_556 ?
C9 C10 H10A 108.7 . . ?
C9 C10 H10A 108.7 2_556 . ?
C9 C10 H10B 108.7 . . ?
C9 C10 H10B 108.7 2_556 . ?
H10A C10 H10B 107.6 . . ?
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
O8 C24 1.2270(19) . ?
O1 C1 1.245(3) . ?
N1 C3 1.342(3) . ?
N1 C6 1.343(3) . ?
N1 C7 1.490(2) . ?
O3 C11 1.2247(19) . ?
O5 C15 1.218(2) . ?
O4 C13 1.2249(19) . ?
O7 C26 1.2200(19) . ?
O6 C22 1.218(2) . ?
N2 C17 1.456(2) . ?
N2 C11 1.371(2) . ?
N2 C21 1.449(2) 2_556 ?
N10 C24 1.369(2) . ?
N10 C28 1.4503(19) 2_556 ?
N10 C23 1.450(2) . ?
N5 C17 1.450(2) 2_556 ?
N5 C13 1.366(2) . ?
N5 C14 1.442(2) . ?
N12 C26 1.377(2) . ?
N12 C27 1.444(2) . ?
N12 C25 1.443(2) . ?
N4 C13 1.365(2) . ?
N4 C18 1.453(2) 2_556 ?
N4 C12 1.439(2) . ?
N6 C19 1.444(2) . ?
N6 C14 1.448(2) . ?
N6 C15 1.373(2) . ?
N7 C20 1.453(2) . ?
N7 C15 1.378(2) . ?
N7 C16 1.452(2) . ?
N11 C24 1.366(2) . ?
N11 C27 1.451(2) 2_556 ?
N11 C25 1.448(2) . ?
N3 C11 1.368(2) . ?
N3 C18 1.448(2) . ?
N3 C12 1.448(2) . ?
N13 C26 1.373(2) . ?
N13 C28 1.451(2) . ?
N13 C16 1.448(2) 2_556 ?
O17 H17A 0.8512 . ?
O17 H17B 0.8475 . ?
N9 C20 1.447(2) . ?
N9 C22 1.375(2) . ?
N9 C23 1.442(2) . ?
N8 C19 1.445(2) . ?
N8 C21 1.447(2) . ?
N8 C22 1.376(2) . ?
O9 H9C 0.8498 . ?
O9 H9D 0.8505 . ?
O10 H10C 0.97(4) . ?
O10 H10D 1.02(5) . ?
O2 C1 1.247(3) . ?
O11 H11A 0.92(4) . ?
O11 H11B 0.95(5) . ?
O16 H16C 0.94(3) . ?
O16 H16D 1.06(5) . ?
O15 H15A 0.8494 . ?
O15 H15B 0.8516 . ?
C17 N5 1.450(2) 2_556 ?
C17 H17 0.9800 . ?
C17 C18 1.555(2) . ?
C28 N10 1.4504(19) 2_556 ?
C28 H28 0.9800 . ?
C28 C27 1.549(2) . ?
C27 N11 1.451(2) 2_556 ?
C27 H27 0.9800 . ?
C20 H20 0.9800 . ?
C20 C19 1.552(2) . ?
C19 H19 0.9800 . ?
O12 H12C 0.99(4) . ?
O12 H12D 0.92(4) . ?
C18 N4 1.453(2) 2_556 ?
C18 H18 0.9800 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C21 N2 1.449(2) 2_556 ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C2 C3 1.383(2) . ?
C2 C4 1.388(3) . ?
C2 C1 1.520(3) . ?
C16 N13 1.448(2) 2_556 ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C4 C5 1.375(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.377(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.501(3) . ?
C8 C9 1.509(2) . ?
C6 H6 0.9300 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.502(2) . ?
C10 C9 1.502(2) 2_556 ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
O13 H13 0.95(3) . ?
O14 H14 0.91(3) . ?
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
N2 C17 C18 N4 -118.93(13) . . . 2_556 ?
N2 C17 C18 N3 1.23(15) . . . . ?
N10 C28 C27 N12 121.04(13) 2_556 . . . ?
N10 C28 C27 N11 -0.44(15) 2_556 . . 2_556 ?
N5 C17 C18 N4 1.65(15) 2_556 . . 2_556 ?
N5 C17 C18 N3 121.80(13) 2_556 . . . ?
N7 C20 C19 N6 -4.56(15) . . . . ?
N7 C20 C19 N8 115.65(14) . . . . ?
N13 C28 C27 N12 -0.12(15) . . . . ?
N13 C28 C27 N11 -121.60(13) . . . 2_556 ?
N9 C20 C19 N6 -124.93(13) . . . . ?
N9 C20 C19 N8 -4.72(16) . . . . ?
C17 N2 C11 O3 -170.88(15) . . . . ?
C17 N2 C11 N3 9.16(18) . . . . ?
C17 N5 C13 O4 175.11(16) 2_556 . . . ?
C17 N5 C13 N4 -2.74(19) 2_556 . . . ?
C17 N5 C14 N6 80.4(2) 2_556 . . . ?
C24 N10 C23 N9 -111.75(17) . . . . ?
C24 N11 C25 N12 104.69(17) . . . . ?
C11 N2 C17 N5 -118.03(16) . . . 2_556 ?
C11 N2 C17 C18 -6.27(17) . . . . ?
C11 N3 C18 N4 116.08(16) . . . 2_556 ?
C11 N3 C18 C17 4.16(17) . . . . ?
C11 N3 C12 N4 -103.66(17) . . . . ?
C26 N12 C27 N11 118.19(16) . . . 2_556 ?
C26 N12 C27 C28 5.99(17) . . . . ?
C26 N12 C25 N11 -104.08(18) . . . . ?
C26 N13 C28 N10 -118.35(16) . . . 2_556 ?
C26 N13 C28 C27 -5.78(17) . . . . ?
C13 N5 C14 N6 -103.41(18) . . . . ?
C13 N4 C12 N3 102.85(18) . . . . ?
C28 N10 C24 O8 167.83(15) 2_556 . . . ?
C28 N10 C24 N11 -11.00(18) 2_556 . . . ?
C28 N10 C23 N9 90.60(18) 2_556 . . . ?
C28 N13 C26 O7 -169.03(16) . . . . ?
C28 N13 C26 N12 9.71(18) . . . . ?
C27 N12 C26 O7 168.94(16) . . . . ?
C27 N12 C26 N13 -9.81(18) . . . . ?
C27 N12 C25 N11 90.14(19) . . . . ?
C27 N11 C24 O8 -168.11(15) 2_556 . . . ?
C27 N11 C24 N10 10.72(18) 2_556 . . . ?
C27 N11 C25 N12 -87.04(19) 2_556 . . . ?
C20 N7 C15 O5 168.87(17) . . . . ?
C20 N7 C15 N6 -10.63(19) . . . . ?
C20 N7 C16 N13 90.72(19) . . . 2_556 ?
C20 N9 C22 O6 -176.61(17) . . . . ?
C20 N9 C22 N8 1.53(19) . . . . ?
C20 N9 C23 N10 -83.3(2) . . . . ?
C19 N6 C14 N5 -91.76(19) . . . . ?
C19 N6 C15 O5 -172.19(17) . . . . ?
C19 N6 C15 N7 7.32(19) . . . . ?
C19 N8 C21 N2 81.5(2) . . . 2_556 ?
C19 N8 C22 O6 173.13(17) . . . . ?
C19 N8 C22 N9 -4.99(19) . . . . ?
C18 N4 C13 O4 -173.92(16) 2_556 . . . ?
C18 N4 C13 N5 3.94(18) 2_556 . . . ?
C18 N4 C12 N3 -81.82(19) 2_556 . . . ?
C18 N3 C11 O3 171.73(15) . . . . ?
C18 N3 C11 N2 -8.31(18) . . . . ?
C18 N3 C12 N4 94.09(18) . . . . ?
C14 N5 C13 O4 -1.5(3) . . . . ?
C14 N5 C13 N4 -179.32(14) . . . . ?
C14 N6 C19 N8 84.69(19) . . . . ?
C14 N6 C19 C20 -162.98(14) . . . . ?
C14 N6 C15 O5 -10.6(3) . . . . ?
C14 N6 C15 N7 168.91(15) . . . . ?
C21 N2 C17 N5 80.3(2) 2_556 . . 2_556 ?
C21 N2 C17 C18 -167.94(14) 2_556 . . . ?
C21 N2 C11 O3 -8.7(3) 2_556 . . . ?
C21 N2 C11 N3 171.38(14) 2_556 . . . ?
C21 N8 C19 N6 -75.0(2) . . . . ?
C21 N8 C19 C20 172.78(14) . . . . ?
C21 N8 C22 O6 6.5(3) . . . . ?
C21 N8 C22 N9 -171.57(15) . . . . ?
C25 N12 C26 O7 1.6(3) . . . . ?
C25 N12 C26 N13 -177.10(14) . . . . ?
C25 N12 C27 N11 -74.7(2) . . . 2_556 ?
C25 N12 C27 C28 173.07(14) . . . . ?
C25 N11 C24 O8 1.3(3) . . . . ?
C25 N11 C24 N10 -179.84(14) . . . . ?
C22 N9 C20 N7 -109.29(16) . . . . ?
C22 N9 C20 C19 2.13(18) . . . . ?
C22 N9 C23 N10 100.43(18) . . . . ?
C22 N8 C19 N6 118.31(16) . . . . ?
C22 N8 C19 C20 6.11(18) . . . . ?
C22 N8 C21 N2 -113.30(18) . . . 2_556 ?
C15 N6 C19 N8 -113.77(16) . . . . ?
C15 N6 C19 C20 -1.45(17) . . . . ?
C15 N6 C14 N5 108.44(18) . . . . ?
C15 N7 C20 N9 120.67(16) . . . . ?
C15 N7 C20 C19 9.38(17) . . . . ?
C15 N7 C16 N13 -113.45(17) . . . 2_556 ?
C23 N10 C24 O8 8.0(2) . . . . ?
C23 N10 C24 N11 -170.80(14) . . . . ?
C23 N9 C20 N7 74.1(2) . . . . ?
C23 N9 C20 C19 -174.47(14) . . . . ?
C23 N9 C22 O6 0.0(3) . . . . ?
C23 N9 C22 N8 178.15(15) . . . . ?
C12 N4 C13 O4 1.9(3) . . . . ?
C12 N4 C13 N5 179.78(14) . . . . ?
C12 N3 C11 O3 7.7(3) . . . . ?
C12 N3 C11 N2 -172.34(14) . . . . ?
C12 N3 C18 N4 -80.05(19) . . . 2_556 ?
C12 N3 C18 C17 168.03(14) . . . . ?
C2 C4 C5 C6 -0.8(3) . . . . ?
C16 N7 C20 N9 -81.48(19) . . . . ?
C16 N7 C20 C19 167.22(14) . . . . ?
C16 N7 C15 O5 10.7(3) . . . . ?
C16 N7 C15 N6 -168.78(15) . . . . ?
C16 N13 C26 O7 -1.1(3) 2_556 . . . ?
C16 N13 C26 N12 177.59(15) 2_556 . . . ?
C16 N13 C28 N10 73.9(2) 2_556 . . 2_556 ?
C16 N13 C28 C27 -173.56(14) 2_556 . . . ?
C3 N1 C6 C5 -1.1(3) . . . . ?
C3 N1 C7 C8 -92.0(2) . . . . ?
C3 C2 C4 C5 0.5(3) . . . . ?
C3 C2 C1 O1 -21.2(3) . . . . ?
C3 C2 C1 O2 157.8(2) . . . . ?
C4 C2 C3 N1 -0.5(3) . . . . ?
C4 C2 C1 O1 158.2(2) . . . . ?
C4 C2 C1 O2 -22.8(3) . . . . ?
C4 C5 C6 N1 1.1(3) . . . . ?
C8 C9 C10 C9 179.8(2) . . . 2_556 ?
C6 N1 C3 C2 0.8(3) . . . . ?
C6 N1 C7 C8 84.5(2) . . . . ?
C1 C2 C3 N1 178.91(17) . . . . ?
C1 C2 C4 C5 -178.91(19) . . . . ?
C7 N1 C3 C2 177.12(16) . . . . ?
C7 N1 C6 C5 -177.47(18) . . . . ?
C7 C8 C9 C10 -177.55(17) . . . . ?
C9 C8 C7 N1 177.55(18) . . . . ?
