#------------------------------------------------------------------------------
#$Date: 2025-11-29 21:59:23 +0100 (Sat 29 de Nov de 2025) $
#$Revision: 303807 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/90/7719077.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_7719077
loop_
_publ_author_name
'Saccone, Marco'
'Valkonen, Arto'
'Rissanen, Kari'
'Cametti, Massimo'
_publ_section_title
;
 X-ray crystallographic and computational studies of quaternary ammonium
 chloride salt complexes with uranyl-salophen compounds.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15043
_journal_page_last               15054
_journal_paper_doi               10.1039/d5dt01115a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'C34 H26 Cl N2 O6 U, C8 H20 N, C3 H6 O, 0.33(H2 O)'
_chemical_formula_sum            'C45 H52.66 Cl N3 O7.33 U'
_chemical_formula_weight         1026.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-06-18 deposited with the CCDC.	2025-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.3950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1252(3)
_cell_length_b                   20.4511(4)
_cell_length_c                   15.7079(3)
_cell_measurement_reflns_used    125191
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.283
_cell_measurement_theta_min      0.407
_cell_volume                     4395.17(15)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker, 2008)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    SHELXL-2019/2
_computing_publication_material  SHELXL-2019/2
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX-II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1000
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            57725
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         2.400
_exptl_absorpt_coefficient_mu    3.806
_exptl_absorpt_correction_T_max  0.5612
_exptl_absorpt_correction_T_min  0.4625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker, 2012)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       block
_exptl_crystal_F_000             2045
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         7946
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0160P)²+10.2921P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6108
_reflns_number_total             7946
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt01115a2.cif
_cod_data_source_block           '[DMDPA][1-Cl]'
_cod_depositor_comments
'Adding full bibliography for 7719076--7719077.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7719077
_shelx_shelxl_version_number     2019/3
_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_min   0.349
_shelx_estimated_absorpt_t_max   0.599
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
U1 U 0.30294(2) 0.35510(2) 0.43583(2) 0.02235(7) Uani 1 1 d . . . . .
Cl1 Cl 0.36551(11) 0.37305(7) 0.28584(8) 0.0339(3) Uani 1 1 d . . . . .
O1 O 0.2233(3) 0.29050(18) 0.3882(2) 0.0314(9) Uani 1 1 d D . . . .
O2 O 0.3799(2) 0.41888(17) 0.4916(2) 0.0261(8) Uani 1 1 d . . . . .
O10 O 0.1940(2) 0.43231(18) 0.3684(2) 0.0248(8) Uani 1 1 d . . . . .
O15 O 0.1030(3) 0.48221(19) 0.2122(2) 0.0324(9) Uani 1 1 d . . . . .
O26 O 0.4350(3) 0.28854(19) 0.4644(2) 0.0321(9) Uani 1 1 d . . . . .
O31 O 0.5484(3) 0.21011(19) 0.3800(2) 0.0305(9) Uani 1 1 d . . . . .
N7 N 0.1783(3) 0.3791(2) 0.5260(3) 0.0237(10) Uani 1 1 d . . . . .
N23 N 0.3250(3) 0.2948(2) 0.5859(3) 0.0243(10) Uani 1 1 d . . . . .
C1 C 0.2849(4) 0.3258(3) 0.6504(3) 0.0248(12) Uani 1 1 d . . . . .
C2 C 0.3177(4) 0.3159(3) 0.7413(3) 0.0283(13) Uani 1 1 d . . . . .
H2 H 0.370500 0.286805 0.763765 0.034 Uiso 1 1 calc R U . . .
C3 C 0.2736(4) 0.3481(3) 0.7979(3) 0.0320(13) Uani 1 1 d . . . . .
H3 H 0.295046 0.340288 0.859324 0.038 Uiso 1 1 calc R U . . .
C4 C 0.1987(5) 0.3917(3) 0.7667(4) 0.0392(15) Uani 1 1 d . . . . .
H4 H 0.169066 0.413882 0.806556 0.047 Uiso 1 1 calc R U . . .
C5 C 0.1663(5) 0.4032(3) 0.6770(3) 0.0356(14) Uani 1 1 d . . . . .
H5 H 0.115717 0.434039 0.655440 0.043 Uiso 1 1 calc R U . . .
C6 C 0.2082(4) 0.3695(3) 0.6189(3) 0.0287(13) Uani 1 1 d . . . . .
C8 C 0.0862(4) 0.3882(3) 0.4909(3) 0.0292(13) Uani 1 1 d . . . . .
H8 H 0.043292 0.382186 0.528174 0.035 Uiso 1 1 calc R U . . .
C9 C 0.0417(4) 0.4065(3) 0.4013(3) 0.0254(12) Uani 1 1 d . . . . .
C10 C 0.0979(4) 0.4307(3) 0.3460(3) 0.0257(12) Uani 1 1 d . . . . .
C11 C 0.0456(4) 0.4565(3) 0.2622(3) 0.0270(12) Uani 1 1 d . . . . .
C12 C -0.0544(4) 0.4540(3) 0.2376(4) 0.0346(14) Uani 1 1 d . . . . .
H12 H -0.087838 0.470987 0.181990 0.042 Uiso 1 1 calc R U . . .
C13 C -0.1081(4) 0.4273(3) 0.2923(4) 0.0398(15) Uani 1 1 d . . . . .
H13 H -0.177354 0.424998 0.273337 0.048 Uiso 1 1 calc R U . . .
C14 C -0.0608(4) 0.4044(3) 0.3730(4) 0.0380(15) Uani 1 1 d . . . . .
H14 H -0.097491 0.386776 0.410684 0.046 Uiso 1 1 calc R U . . .
C16 C 0.0517(5) 0.5090(4) 0.1299(4) 0.0554(19) Uani 1 1 d . . . . .
H16A H 0.015410 0.548523 0.139924 0.066 Uiso 1 1 calc R U . . .
H16B H 0.003821 0.476696 0.097613 0.066 Uiso 1 1 calc R U . . .
C17 C 0.1234(5) 0.5267(4) 0.0759(4) 0.0427(16) Uani 1 1 d . . . . .
C18 C 0.1802(5) 0.4789(4) 0.0533(4) 0.057(2) Uani 1 1 d . . . . .
H18 H 0.178627 0.435795 0.075362 0.068 Uiso 1 1 calc R U . . .
C19 C 0.2418(5) 0.4940(5) -0.0033(5) 0.067(2) Uani 1 1 d . . . . .
H19 H 0.283021 0.461491 -0.018152 0.080 Uiso 1 1 calc R U . . .
C20 C 0.2407(5) 0.5557(5) -0.0357(4) 0.058(2) Uani 1 1 d . . . . .
H20 H 0.278858 0.566317 -0.075802 0.069 Uiso 1 1 calc R U . . .
C21 C 0.1844(6) 0.6020(4) -0.0101(4) 0.061(2) Uani 1 1 d . . . . .
H21 H 0.184912 0.645540 -0.031202 0.073 Uiso 1 1 calc R U . . .
C22 C 0.1272(5) 0.5869(4) 0.0455(4) 0.0548(19) Uani 1 1 d . . . . .
H22 H 0.089207 0.620303 0.062883 0.066 Uiso 1 1 calc R U . . .
C24 C 0.3589(4) 0.2358(3) 0.6029(3) 0.0266(12) Uani 1 1 d . . . . .
H24 H 0.348252 0.215613 0.654223 0.032 Uiso 1 1 calc R U . . .
C25 C 0.4110(4) 0.1978(3) 0.5518(3) 0.0282(13) Uani 1 1 d . . . . .
C26 C 0.4508(4) 0.2274(3) 0.4863(3) 0.0277(13) Uani 1 1 d . . . . .
C27 C 0.5093(4) 0.1867(3) 0.4463(3) 0.0244(12) Uani 1 1 d . . . . .
C28 C 0.5235(4) 0.1218(3) 0.4679(3) 0.0295(13) Uani 1 1 d . . . . .
H28 H 0.561580 0.095485 0.439251 0.035 Uiso 1 1 calc R U . . .
C29 C 0.4823(4) 0.0941(3) 0.5319(3) 0.0327(14) Uani 1 1 d . . . . .
H29 H 0.492174 0.049027 0.545943 0.039 Uiso 1 1 calc R U . . .
C30 C 0.4279(4) 0.1316(3) 0.5745(3) 0.0292(13) Uani 1 1 d . . . . .
H30 H 0.401697 0.112893 0.619107 0.035 Uiso 1 1 calc R U . . .
C32 C 0.6075(4) 0.2687(3) 0.4000(4) 0.0393(15) Uani 1 1 d . . . . .
H32A H 0.651816 0.265538 0.459503 0.047 Uiso 1 1 calc R U . . .
H32B H 0.565162 0.307531 0.397913 0.047 Uiso 1 1 calc R U . . .
C33 C 0.6654(4) 0.2744(3) 0.3323(3) 0.0295(13) Uani 1 1 d . . . . .
C34 C 0.6243(4) 0.3015(3) 0.2505(3) 0.0339(14) Uani 1 1 d . . . . .
H34 H 0.560222 0.319379 0.238731 0.041 Uiso 1 1 calc R U . . .
C35 C 0.6746(5) 0.3028(3) 0.1870(4) 0.0401(15) Uani 1 1 d . . . . .
H35 H 0.645674 0.322068 0.131570 0.048 Uiso 1 1 calc R U . . .
C36 C 0.7677(5) 0.2764(3) 0.2025(4) 0.0453(16) Uani 1 1 d . . . . .
H36 H 0.801445 0.276310 0.157177 0.054 Uiso 1 1 calc R U . . .
C37 C 0.8110(5) 0.2503(3) 0.2834(4) 0.0479(17) Uani 1 1 d . . . . .
H37 H 0.875587 0.233427 0.295143 0.057 Uiso 1 1 calc R U . . .
C38 C 0.7589(5) 0.2490(3) 0.3481(4) 0.0409(16) Uani 1 1 d . . . . .
H38 H 0.788033 0.230297 0.403819 0.049 Uiso 1 1 calc R U . . .
N39 N 0.3982(3) 0.5738(2) 0.3188(3) 0.0310(11) Uani 1 1 d . . . . .
C40 C 0.3181(4) 0.5588(3) 0.2398(4) 0.0451(16) Uani 1 1 d . . . . .
H40A H 0.297654 0.513225 0.242367 0.068 Uiso 1 1 calc R U . . .
H40B H 0.262536 0.587807 0.238393 0.068 Uiso 1 1 calc R U . . .
H40C H 0.341513 0.565526 0.186723 0.068 Uiso 1 1 calc R U . . .
C41 C 0.4297(4) 0.6433(3) 0.3151(4) 0.0372(13) Uani 1 1 d . . . . .
H41A H 0.482409 0.653030 0.367182 0.056 Uiso 1 1 calc R U . . .
H41B H 0.453106 0.650033 0.262077 0.056 Uiso 1 1 calc R U . . .
H41C H 0.374129 0.672315 0.313747 0.056 Uiso 1 1 calc R U . . .
C42 C 0.4842(5) 0.5282(3) 0.3227(4) 0.0431(16) Uani 1 1 d . . . . .
H42A H 0.538040 0.541145 0.373315 0.052 Uiso 1 1 calc R U . . .
H42B H 0.464144 0.483317 0.334087 0.052 Uiso 1 1 calc R U . . .
C43 C 0.5228(5) 0.5268(4) 0.2419(5) 0.0559(19) Uani 1 1 d . . . . .
H43A H 0.538342 0.571871 0.226655 0.067 Uiso 1 1 calc R U . . .
H43B H 0.472393 0.508884 0.191942 0.067 Uiso 1 1 calc R U . . .
C44 C 0.6142(6) 0.4848(4) 0.2583(6) 0.086(3) Uani 1 1 d . . . . .
H44A H 0.639054 0.484068 0.205309 0.129 Uiso 1 1 calc R U . . .
H44B H 0.664192 0.502966 0.307339 0.129 Uiso 1 1 calc R U . . .
H44C H 0.598382 0.440112 0.272698 0.129 Uiso 1 1 calc R U . . .
C45 C 0.3639(6) 0.5629(3) 0.4009(4) 0.057(2) Uani 1 1 d D . . . .
H45A H 0.338789 0.517575 0.398918 0.069 Uiso 1 1 calc R U . A 1
H45B H 0.421849 0.565423 0.451454 0.069 Uiso 1 1 calc R U . A 1
C46 C 0.288(2) 0.6068(16) 0.420(2) 0.087(6) Uani 0.59(3) 1 d D U P B 1
H46A H 0.225643 0.603163 0.374294 0.104 Uiso 0.59(3) 1 calc R U P B 1
H46B H 0.309691 0.652991 0.424541 0.104 Uiso 0.59(3) 1 calc R U P B 1
C47 C 0.277(2) 0.5804(10) 0.5105(15) 0.077(5) Uani 0.59(3) 1 d D U P B 1
H47A H 0.227910 0.606191 0.529879 0.116 Uiso 0.59(3) 1 calc R U P B 1
H47B H 0.256678 0.534466 0.504196 0.116 Uiso 0.59(3) 1 calc R U P B 1
H47C H 0.340015 0.583873 0.554018 0.116 Uiso 0.59(3) 1 calc R U P B 1
C46B C 0.274(3) 0.601(2) 0.403(3) 0.086(6) Uani 0.41(3) 1 d D U P B 2
H46C H 0.224796 0.589231 0.348462 0.103 Uiso 0.41(3) 1 calc R U P B 2
H46D H 0.290515 0.647204 0.397764 0.103 Uiso 0.41(3) 1 calc R U P B 2
C47B C 0.219(3) 0.5974(15) 0.479(2) 0.081(6) Uani 0.41(3) 1 d D U P B 2
H47D H 0.162723 0.626681 0.464617 0.122 Uiso 0.41(3) 1 calc R U P B 2
H47E H 0.197536 0.552539 0.484324 0.122 Uiso 0.41(3) 1 calc R U P B 2
H47F H 0.263924 0.611102 0.534128 0.122 Uiso 0.41(3) 1 calc R U P B 2
O49 O -0.0617(6) 0.2474(5) 0.5617(6) 0.081(3) Uani 0.670(7) 1 d D U P C 1
C48 C 0.0794(8) 0.2129(6) 0.5167(7) 0.068(3) Uani 0.670(7) 1 d D U P C 1
H48A H 0.093423 0.165980 0.516871 0.102 Uiso 0.670(7) 1 calc R U P C 1
H48B H 0.140948 0.237412 0.531605 0.102 Uiso 0.670(7) 1 calc R U P C 1
H48C H 0.041183 0.225991 0.458237 0.102 Uiso 0.670(7) 1 calc R U P C 1
C49 C 0.0215(6) 0.2274(6) 0.5841(5) 0.068(3) Uani 0.670(7) 1 d D U P C 1
C50 C 0.0694(9) 0.2124(7) 0.6799(6) 0.075(4) Uani 0.670(7) 1 d D U P C 1
H50A H 0.022068 0.219257 0.715277 0.113 Uiso 0.670(7) 1 calc R U P C 1
H50B H 0.125625 0.241352 0.700794 0.113 Uiso 0.670(7) 1 calc R U P C 1
H50C H 0.091398 0.166764 0.685365 0.113 Uiso 0.670(7) 1 calc R U P C 1
O52 O -0.0001(15) 0.2568(9) 0.5638(12) 0.072(5) Uani 0.330(7) 1 d D U P C 2
C51 C 0.1248(15) 0.1805(9) 0.6328(15) 0.066(5) Uani 0.330(7) 1 d D U P C 2
H51A H 0.099968 0.136541 0.639610 0.099 Uiso 0.330(7) 1 calc R U P C 2
H51B H 0.180737 0.189887 0.682295 0.099 Uiso 0.330(7) 1 calc R U P C 2
H51C H 0.145492 0.182713 0.577720 0.099 Uiso 0.330(7) 1 calc R U P C 2
C52 C 0.0446(16) 0.2305(11) 0.6307(11) 0.062(5) Uani 0.330(7) 1 d D U P C 2
C53 C 0.0308(16) 0.2566(10) 0.7170(13) 0.065(5) Uani 0.330(7) 1 d D U P C 2
H53A H 0.092107 0.276013 0.750759 0.097 Uiso 0.330(7) 1 calc R U P C 2
H53B H 0.011944 0.220723 0.750795 0.097 Uiso 0.330(7) 1 calc R U P C 2
H53C H -0.020646 0.289944 0.705409 0.097 Uiso 0.330(7) 1 calc R U P C 2
O54 O 0.053852 0.203375 0.404305 0.103 Uani 0.330(7) 1 d G . P C 2
H54A H 0.021919 0.221369 0.438937 0.155 Uiso 0.330(7) 1 d DG U P C 2
H54B H 0.085000 0.235610 0.387400 0.155 Uiso 0.330(7) 1 d DG U P C 2
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
O1 U1 O2 175.39(15) . . ?
O1 U1 O26 92.33(16) . . ?
O2 U1 O26 88.31(15) . . ?
O1 U1 O10 92.06(15) . . ?
O2 U1 O10 88.88(14) . . ?
O26 U1 O10 159.93(12) . . ?
O1 U1 N7 85.72(15) . . ?
O2 U1 N7 90.39(15) . . ?
O26 U1 N7 130.56(13) . . ?
O10 U1 N7 69.32(12) . . ?
O1 U1 N23 87.13(15) . . ?
O2 U1 N23 88.87(14) . . ?
O26 U1 N23 68.22(13) . . ?
O10 U1 N23 131.58(12) . . ?
N7 U1 N23 62.34(13) . . ?
O1 U1 Cl1 92.48(12) . . ?
O2 U1 Cl1 92.13(11) . . ?
O26 U1 Cl1 79.93(9) . . ?
O10 U1 Cl1 80.32(9) . . ?
N7 U1 Cl1 149.48(10) . . ?
N23 U1 Cl1 148.10(10) . . ?
C10 O10 U1 129.8(3) . . ?
C11 O15 C16 115.4(4) . . ?
C26 O26 U1 135.2(3) . . ?
C27 O31 C32 116.1(4) . . ?
C8 N7 C6 117.8(4) . . ?
C8 N7 U1 123.1(3) . . ?
C6 N7 U1 117.9(3) . . ?
C24 N23 C1 117.1(4) . . ?
C24 N23 U1 125.4(3) . . ?
C1 N23 U1 117.0(3) . . ?
C6 C1 C2 118.9(5) . . ?
C6 C1 N23 116.2(4) . . ?
C2 C1 N23 124.8(5) . . ?
C3 C2 C1 120.1(5) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 120.8(5) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C3 C4 C5 120.0(5) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 119.7(5) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C1 120.4(5) . . ?
C5 C6 N7 122.5(5) . . ?
C1 C6 N7 117.1(5) . . ?
N7 C8 C9 127.0(5) . . ?
N7 C8 H8 116.5 . . ?
C9 C8 H8 116.5 . . ?
C10 C9 C14 120.7(5) . . ?
C10 C9 C8 121.3(5) . . ?
C14 C9 C8 117.8(5) . . ?
O10 C10 C9 123.2(5) . . ?
O10 C10 C11 119.7(5) . . ?
C9 C10 C11 117.0(5) . . ?
O15 C11 C12 124.8(5) . . ?
O15 C11 C10 115.1(5) . . ?
C12 C11 C10 120.2(5) . . ?
C11 C12 C13 121.6(5) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
C14 C13 C12 119.5(5) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C14 C9 120.9(6) . . ?
C13 C14 H14 119.6 . . ?
C9 C14 H14 119.6 . . ?
O15 C16 C17 109.8(5) . . ?
O15 C16 H16A 109.7 . . ?
C17 C16 H16A 109.7 . . ?
O15 C16 H16B 109.7 . . ?
C17 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
C22 C17 C18 119.5(7) . . ?
C22 C17 C16 121.0(7) . . ?
C18 C17 C16 119.4(7) . . ?
C17 C18 C19 119.8(7) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C20 C19 C18 118.9(7) . . ?
C20 C19 H19 120.6 . . ?
C18 C19 H19 120.6 . . ?
C19 C20 C21 119.3(7) . . ?
C19 C20 H20 120.4 . . ?
C21 C20 H20 120.4 . . ?
C20 C21 C22 120.9(8) . . ?
C20 C21 H21 119.5 . . ?
C22 C21 H21 119.5 . . ?
C17 C22 C21 121.6(8) . . ?
C17 C22 H22 119.2 . . ?
C21 C22 H22 119.2 . . ?
N23 C24 C25 126.7(5) . . ?
N23 C24 H24 116.7 . . ?
C25 C24 H24 116.7 . . ?
C30 C25 C26 121.4(5) . . ?
C30 C25 C24 117.0(5) . . ?
C26 C25 C24 121.3(5) . . ?
O26 C26 C25 121.8(5) . . ?
O26 C26 C27 121.6(5) . . ?
C25 C26 C27 116.5(5) . . ?
C28 C27 O31 117.4(5) . . ?
C28 C27 C26 121.4(5) . . ?
O31 C27 C26 121.0(5) . . ?
C27 C28 C29 120.5(5) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
C30 C29 C28 120.5(5) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C29 C30 C25 119.6(5) . . ?
C29 C30 H30 120.2 . . ?
C25 C30 H30 120.2 . . ?
O31 C32 C33 107.3(4) . . ?
O31 C32 H32A 110.3 . . ?
C33 C32 H32A 110.3 . . ?
O31 C32 H32B 110.3 . . ?
C33 C32 H32B 110.3 . . ?
H32A C32 H32B 108.5 . . ?
C38 C33 C34 118.6(5) . . ?
C38 C33 C32 120.6(5) . . ?
C34 C33 C32 120.7(5) . . ?
C35 C34 C33 120.7(6) . . ?
C35 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
C34 C35 C36 120.6(5) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C37 C36 C35 119.9(6) . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 C38 119.2(6) . . ?
C36 C37 H37 120.4 . . ?
C38 C37 H37 120.4 . . ?
C33 C38 C37 121.0(5) . . ?
C33 C38 H38 119.5 . . ?
C37 C38 H38 119.5 . . ?
C40 N39 C41 109.6(4) . . ?
C40 N39 C45 110.1(5) . . ?
C41 N39 C45 109.7(4) . . ?
C40 N39 C42 110.0(4) . . ?
C41 N39 C42 110.1(4) . . ?
C45 N39 C42 107.4(5) . . ?
N39 C40 H40A 109.5 . . ?
N39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
N39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N39 C41 H41A 109.5 . . ?
N39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
N39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 N39 115.6(5) . . ?
C43 C42 H42A 108.4 . . ?
N39 C42 H42A 108.4 . . ?
C43 C42 H42B 108.4 . . ?
N39 C42 H42B 108.4 . . ?
H42A C42 H42B 107.5 . . ?
C42 C43 C44 109.9(6) . . ?
C42 C43 H43A 109.7 . . ?
C44 C43 H43A 109.7 . . ?
C42 C43 H43B 109.7 . . ?
C44 C43 H43B 109.7 . . ?
H43A C43 H43B 108.2 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 N39 119.1(10) . . ?
C46B C45 N39 113.7(13) . . ?
C46 C45 H45A 107.5 . . ?
N39 C45 H45A 107.5 . . ?
C46 C45 H45B 107.5 . . ?
N39 C45 H45B 107.5 . . ?
H45A C45 H45B 107.0 . . ?
C45 C46 C47 102.3(14) . . ?
C45 C46 H46A 111.3 . . ?
C47 C46 H46A 111.3 . . ?
C45 C46 H46B 111.3 . . ?
C47 C46 H46B 111.3 . . ?
H46A C46 H46B 109.2 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C46B C47B 125(3) . . ?
C45 C46B H46C 106.0 . . ?
C47B C46B H46C 106.0 . . ?
C45 C46B H46D 106.0 . . ?
C47B C46B H46D 106.0 . . ?
H46C C46B H46D 106.3 . . ?
C46B C47B H47D 109.5 . . ?
C46B C47B H47E 109.5 . . ?
H47D C47B H47E 109.5 . . ?
C46B C47B H47F 109.5 . . ?
H47D C47B H47F 109.5 . . ?
H47E C47B H47F 109.5 . . ?
C49 C48 H48A 109.5 . . ?
C49 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C49 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O49 C49 C48 121.0(9) . . ?
O49 C49 C50 121.2(9) . . ?
C48 C49 C50 117.7(9) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C52 C51 H51A 109.5 . . ?
C52 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C52 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
O52 C52 C53 117.7(18) . . ?
O52 C52 C51 122.9(19) . . ?
C53 C52 C51 118.7(11) . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
H54A O54 H54B 104.5 . . ?
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 O1 1.776(4) . ?
U1 O2 1.783(3) . ?
U1 O26 2.262(4) . ?
U1 O10 2.274(3) . ?
U1 N7 2.567(4) . ?
U1 N23 2.609(4) . ?
U1 Cl1 2.7389(13) . ?
O10 C10 1.315(6) . ?
O15 C11 1.366(6) . ?
O15 C16 1.424(7) . ?
O26 C26 1.302(6) . ?
O31 C27 1.380(6) . ?
O31 C32 1.449(7) . ?
N7 C8 1.294(7) . ?
N7 C6 1.428(6) . ?
N23 C24 1.303(7) . ?
N23 C1 1.426(6) . ?
C1 C6 1.397(7) . ?
C1 C2 1.401(7) . ?
C2 C3 1.376(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.377(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(7) . ?
C5 H5 0.9500 . ?
C8 C9 1.440(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.404(7) . ?
C9 C14 1.406(8) . ?
C10 C11 1.440(7) . ?
C11 C12 1.369(8) . ?
C12 C13 1.391(8) . ?
C12 H12 0.9500 . ?
C13 C14 1.361(8) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C16 C17 1.519(9) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C22 1.327(9) . ?
C17 C18 1.365(10) . ?
C18 C19 1.425(11) . ?
C18 H18 0.9500 . ?
C19 C20 1.359(11) . ?
C19 H19 0.9500 . ?
C20 C21 1.362(11) . ?
C20 H20 0.9500 . ?
C21 C22 1.364(10) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C24 C25 1.444(7) . ?
C24 H24 0.9500 . ?
C25 C30 1.405(7) . ?
C25 C26 1.423(7) . ?
C26 C27 1.425(7) . ?
C27 C28 1.372(8) . ?
C28 C29 1.400(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.372(7) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C32 C33 1.499(8) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C38 1.382(8) . ?
C33 C34 1.387(7) . ?
C34 C35 1.363(8) . ?
C34 H34 0.9500 . ?
C35 C36 1.386(9) . ?
C35 H35 0.9500 . ?
C36 C37 1.374(9) . ?
C36 H36 0.9500 . ?
C37 C38 1.396(8) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
N39 C40 1.488(7) . ?
N39 C41 1.493(7) . ?
N39 C45 1.504(7) . ?
N39 C42 1.520(8) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.501(9) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.520(10) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.487(14) . ?
C45 C46B 1.493(17) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.563(15) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C46B C47B 1.567(16) . ?
C46B H46C 0.9900 . ?
C46B H46D 0.9900 . ?
C47B H47D 0.9800 . ?
C47B H47E 0.9800 . ?
C47B H47F 0.9800 . ?
O49 C49 1.2098(10) . ?
C48 C49 1.5198(10) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C50 1.5198(10) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
O52 C52 1.211(10) . ?
C51 C52 1.521(10) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 C53 1.514(10) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
O54 H54A 0.8700 . ?
O54 H54B 0.8699 . ?
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
C24 N23 C1 C6 -148.1(5) . . . . ?
U1 N23 C1 C6 24.0(6) . . . . ?
C24 N23 C1 C2 32.6(8) . . . . ?
U1 N23 C1 C2 -155.2(4) . . . . ?
C6 C1 C2 C3 1.0(8) . . . . ?
N23 C1 C2 C3 -179.8(5) . . . . ?
C1 C2 C3 C4 -1.7(9) . . . . ?
C2 C3 C4 C5 0.4(9) . . . . ?
C3 C4 C5 C6 1.6(9) . . . . ?
C4 C5 C6 C1 -2.3(9) . . . . ?
C4 C5 C6 N7 -179.9(5) . . . . ?
C2 C1 C6 C5 1.0(8) . . . . ?
N23 C1 C6 C5 -178.3(5) . . . . ?
C2 C1 C6 N7 178.8(5) . . . . ?
N23 C1 C6 N7 -0.5(7) . . . . ?
C8 N7 C6 C5 -37.9(8) . . . . ?
U1 N7 C6 C5 153.9(5) . . . . ?
C8 N7 C6 C1 144.3(5) . . . . ?
U1 N7 C6 C1 -23.9(6) . . . . ?
C6 N7 C8 C9 172.0(5) . . . . ?
U1 N7 C8 C9 -20.5(8) . . . . ?
N7 C8 C9 C10 -14.3(9) . . . . ?
N7 C8 C9 C14 170.7(5) . . . . ?
U1 O10 C10 C9 44.0(7) . . . . ?
U1 O10 C10 C11 -138.1(4) . . . . ?
C14 C9 C10 O10 -178.4(5) . . . . ?
C8 C9 C10 O10 6.8(8) . . . . ?
C14 C9 C10 C11 3.7(8) . . . . ?
C8 C9 C10 C11 -171.2(5) . . . . ?
C16 O15 C11 C12 1.3(8) . . . . ?
C16 O15 C11 C10 -178.8(5) . . . . ?
O10 C10 C11 O15 -0.9(7) . . . . ?
C9 C10 C11 O15 177.1(4) . . . . ?
O10 C10 C11 C12 178.9(5) . . . . ?
C9 C10 C11 C12 -3.0(8) . . . . ?
O15 C11 C12 C13 -179.7(5) . . . . ?
C10 C11 C12 C13 0.4(8) . . . . ?
C11 C12 C13 C14 1.7(9) . . . . ?
C12 C13 C14 C9 -1.0(9) . . . . ?
C10 C9 C14 C13 -1.7(9) . . . . ?
C8 C9 C14 C13 173.3(5) . . . . ?
C11 O15 C16 C17 -171.8(5) . . . . ?
O15 C16 C17 C22 -124.1(6) . . . . ?
O15 C16 C17 C18 60.3(8) . . . . ?
C22 C17 C18 C19 -0.8(9) . . . . ?
C16 C17 C18 C19 174.9(5) . . . . ?
C17 C18 C19 C20 -1.7(9) . . . . ?
C18 C19 C20 C21 3.0(10) . . . . ?
C19 C20 C21 C22 -1.9(10) . . . . ?
C18 C17 C22 C21 2.1(10) . . . . ?
C16 C17 C22 C21 -173.6(6) . . . . ?
C20 C21 C22 C17 -0.7(10) . . . . ?
C1 N23 C24 C25 -173.4(5) . . . . ?
U1 N23 C24 C25 15.2(8) . . . . ?
N23 C24 C25 C30 -170.5(5) . . . . ?
N23 C24 C25 C26 14.7(8) . . . . ?
U1 O26 C26 C25 -44.4(7) . . . . ?
U1 O26 C26 C27 136.0(4) . . . . ?
C30 C25 C26 O26 179.5(5) . . . . ?
C24 C25 C26 O26 -5.9(8) . . . . ?
C30 C25 C26 C27 -0.8(7) . . . . ?
C24 C25 C26 C27 173.7(5) . . . . ?
C32 O31 C27 C28 -129.0(5) . . . . ?
C32 O31 C27 C26 55.2(6) . . . . ?
O26 C26 C27 C28 -178.2(5) . . . . ?
C25 C26 C27 C28 2.2(7) . . . . ?
O26 C26 C27 O31 -2.6(8) . . . . ?
C25 C26 C27 O31 177.7(4) . . . . ?
O31 C27 C28 C29 -177.2(4) . . . . ?
C26 C27 C28 C29 -1.5(8) . . . . ?
C27 C28 C29 C30 -0.6(8) . . . . ?
C28 C29 C30 C25 1.9(8) . . . . ?
C26 C25 C30 C29 -1.1(8) . . . . ?
C24 C25 C30 C29 -175.9(5) . . . . ?
C27 O31 C32 C33 163.7(4) . . . . ?
O31 C32 C33 C38 -93.5(6) . . . . ?
O31 C32 C33 C34 82.5(7) . . . . ?
C38 C33 C34 C35 0.3(9) . . . . ?
C32 C33 C34 C35 -175.7(5) . . . . ?
C33 C34 C35 C36 0.7(9) . . . . ?
C34 C35 C36 C37 -2.0(10) . . . . ?
C35 C36 C37 C38 2.1(10) . . . . ?
C34 C33 C38 C37 -0.1(9) . . . . ?
C32 C33 C38 C37 175.9(6) . . . . ?
C36 C37 C38 C33 -1.1(10) . . . . ?
C40 N39 C42 C43 54.3(7) . . . . ?
C41 N39 C42 C43 -66.6(6) . . . . ?
C45 N39 C42 C43 174.1(5) . . . . ?
N39 C42 C43 C44 174.4(5) . . . . ?
C40 N39 C45 C46 -68(2) . . . . ?
C41 N39 C45 C46 53(2) . . . . ?
C42 N39 C45 C46 173(2) . . . . ?
C40 N39 C45 C46B -56(3) . . . . ?
C41 N39 C45 C46B 65(3) . . . . ?
C42 N39 C45 C46B -175(3) . . . . ?
N39 C45 C46 C47 -178.1(12) . . . . ?
N39 C45 C46B C47B 178(3) . . . . ?
