# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_201116_uo2_tbupdiop_red2
_database_code_depnum_ccdc_archive 'CCDC 2118195'
loop_
_audit_author_name
_audit_author_address
'Tomoyuki Takeyama'
;Tokyo Institute of Technology
Japan
;
_audit_update_record             
;
2022-04-05 deposited with the CCDC.	2022-04-06 downloaded from the CCDC.
;
_audit_creation_date             2021-04-08
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C35 H45 N3 O4 U, C5 H5 N'
_chemical_formula_sum            'C40 H50 N4 O4 U'
_chemical_formula_weight         888.87
_chemical_melting_point          ?
_chemical_oxdiff_formula         C35H47N3O4U1
_chemical_oxdiff_usercomment     201116_UO2_tBupdiop_red
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.4156(5)
_cell_length_b                   13.2468(5)
_cell_length_c                   14.4323(8)
_cell_angle_alpha                68.939(4)
_cell_angle_beta                 68.074(5)
_cell_angle_gamma                81.267(3)
_cell_volume                     1888.95(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8389
_cell_measurement_temperature    113
_cell_measurement_theta_max      24.1730
_cell_measurement_theta_min      1.8880
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.341
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71415
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.60a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             884
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -17 0 0.0261
-14 -1 1 0.1058
-2 17 0 0.0363
15 -1 -1 0.1264
6 -14 5 0.0523
-2 -7 -20 0.0324
-6 15 -3 0.0420
2 6 20 0.0138

_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.048
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.6182 -17.3356 0.1899 -0.0000 -0.3511 0.9363
-14.4728 -1.4653 1.2567 -0.0000 -0.9529 -0.3032
-2.1166 17.1819 -0.0597 0.0000 0.2524 -0.9676
14.5078 -1.2307 -1.2219 0.0000 0.8944 0.4472
6.1189 -14.2682 4.9309 -0.2502 -0.0813 0.9648
-1.6079 -6.7538 -19.5349 0.9415 0.3059 0.1414
-6.0267 14.9323 -3.3301 0.1732 0.0563 -0.9833
1.7935 6.2750 19.6043 -0.9452 -0.3071 -0.1104

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0970
_diffrn_reflns_av_unetI/netI     0.1272
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41195
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.992
_diffrn_reflns_theta_min         1.886
_diffrn_ambient_temperature      113
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -73.00  75.00   0.50  100.00    --   20.00  54.00 -95.53  296
  2  ω     82.00 109.00   0.50  100.00    --   20.00  54.00 -95.53   54
  3  ω    -73.00 -35.00   0.50  100.00    --   20.00  54.00  30.00   76
  4  ω     20.00  47.00   0.50  100.00    --   20.00  54.00  30.00   54
  5  ω     67.00 107.00   0.50  100.00    --   20.00  54.00  30.00   80
  6  ω    -72.00  44.50   0.50  100.00    --   20.00  54.00 -30.00  233
  7  ω    -74.00 -24.00   0.50  100.00    --   20.00  54.00-150.00  100
  8  ω     35.00  74.00   0.50  100.00    --   20.00  54.00-150.00   78
  9  ω    -62.00 -21.00   0.50  100.00    --   20.00  54.00  90.00   82
 10  ω     -8.00  45.00   0.50  100.00    --   20.00  54.00  90.00  106
 11  ω     85.00 110.00   0.50  100.00    --   20.00  54.00  90.00   50
 12  ω    -16.00  96.00   0.50  100.00    --   20.00  54.00-167.52  224
 13  ω    -68.00 -29.00   0.50  100.00    --   20.00  54.00  60.00   78
 14  ω    -74.00 107.00   0.50  100.00    --   20.00  54.00-180.00  362
 15  ω    -60.00 -35.00   0.50  100.00    --   20.00  54.00 -90.00   50
 16  ω     -1.00  44.00   0.50  100.00    --   20.00  54.00 -60.00   90
 17  ω    -35.00 -10.00   0.50  100.00    --   20.00  54.00   0.00   50
 18  ω     77.00 102.00   0.50  100.00    --   20.00  54.00   0.00   50
 19  ω    -73.00  62.00   0.50  100.00    --   20.00  54.00 150.00  270
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0040682000
_diffrn_orient_matrix_UB_12      -0.0006667000
_diffrn_orient_matrix_UB_13      -0.0476303000
_diffrn_orient_matrix_UB_21      0.0611415000
_diffrn_orient_matrix_UB_22      0.0221245000
_diffrn_orient_matrix_UB_23      -0.0283413000
_diffrn_orient_matrix_UB_31      0.0270783000
_diffrn_orient_matrix_UB_32      -0.0529495000
_diffrn_orient_matrix_UB_33      0.0088379000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7834
_reflns_number_total             11337
_reflns_odcompleteness_completeness 98.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         6.541
_refine_diff_density_min         -4.709
_refine_diff_density_rms         0.296
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         11337
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0722
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1027P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.1817
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C14) = Uanis(C19) = Uanis(C18) = Uanis(C17) = Uanis(C16) = Uanis(C15)
Uanis(O3) = Uanis(O4) = Uanis(N3) = Uanis(N2) = Uanis(N1)
3.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C7(H7), C11(H11), C13(H13), C10(H10), C15(H15), C17(H17), C5(H5),
 C3(H3), C36(H36), C37(H37), C40(H40), C38(H38), C39(H39)
3.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C23(H23A,H23B,H23C), C21(H21A,H21B,H21C), C34(H34A,H34B,
 H34C), C27(H27A,H27B,H27C), C33(H33A,H33B,H33C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C35(H35A,H35B,H35C),
 C22(H22A,H22B,H22C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.68063(3) 0.61617(2) 0.58569(2) 0.01885(10) Uani 1 1 d . . . . .
O1 O 0.7971(6) 0.7110(5) 0.4899(5) 0.0268(13) Uani 1 1 d . . . . .
O4 O 0.5287(5) 0.7414(5) 0.6105(4) 0.0219(6) Uani 1 1 d . . . . .
O3 O 0.7634(5) 0.5954(4) 0.7100(4) 0.0219(6) Uani 1 1 d . . . . .
O2 O 0.5711(5) 0.5143(5) 0.6746(5) 0.0254(12) Uani 1 1 d . . . . .
N1 N 0.8470(6) 0.4621(6) 0.6038(5) 0.0219(6) Uani 1 1 d . . . . .
N2 N 0.7394(6) 0.5137(5) 0.4559(5) 0.0219(6) Uani 1 1 d . . . . .
N3 N 0.5547(6) 0.6661(6) 0.4602(5) 0.0219(6) Uani 1 1 d . . . . .
C8 C 0.8344(7) 0.4394(6) 0.4527(6) 0.0195(15) Uani 1 1 d . . . . .
C12 C 0.6821(7) 0.5369(6) 0.3837(6) 0.0200(15) Uani 1 1 d . . . . .
C9 C 0.8760(7) 0.3885(6) 0.3761(6) 0.0199(15) Uani 1 1 d . . . . .
H9 H 0.944614 0.337835 0.373957 0.024 Uiso 1 1 calc R U . . .
C7 C 0.8901(7) 0.4127(6) 0.5348(6) 0.0195(15) Uani 1 1 d . . . . .
H7 H 0.956610 0.360286 0.537487 0.023 Uiso 1 1 calc R U . . .
C18 C 0.3460(8) 0.8532(6) 0.5882(6) 0.0209(7) Uani 1 1 d . . . . .
C11 C 0.7152(7) 0.4874(7) 0.3085(6) 0.0212(16) Uani 1 1 d . . . . .
H11 H 0.670409 0.503446 0.260886 0.025 Uiso 1 1 calc R U . . .
C28 C 0.2101(8) 0.9193(7) 0.3656(7) 0.0256(18) Uani 1 1 d . . . . .
N4 N 0.4763(8) 0.2668(7) 0.8518(6) 0.0378(19) Uani 1 1 d . . . . .
C6 C 0.8817(7) 0.4376(6) 0.6928(6) 0.0182(15) Uani 1 1 d . . . . .
C14 C 0.4591(7) 0.7455(6) 0.4749(6) 0.0209(7) Uani 1 1 d . . . . .
C13 C 0.5785(7) 0.6191(6) 0.3919(6) 0.0207(16) Uani 1 1 d . . . . .
H13 H 0.530357 0.636535 0.346730 0.025 Uiso 1 1 calc R U . . .
C10 C 0.8152(7) 0.4136(7) 0.3032(7) 0.0238(17) Uani 1 1 d . . . . .
H10 H 0.841965 0.380252 0.250106 0.029 Uiso 1 1 calc R U . . .
C15 C 0.3841(7) 0.7877(6) 0.4119(6) 0.0209(7) Uani 1 1 d . . . . .
H15 H 0.397446 0.764553 0.353481 0.025 Uiso 1 1 calc R U . . .
C17 C 0.2718(7) 0.8912(6) 0.5258(6) 0.0209(7) Uani 1 1 d . . . . .
H17 H 0.203724 0.939300 0.544863 0.025 Uiso 1 1 calc R U . . .
C20 C 0.7871(8) 0.5658(7) 0.9118(7) 0.0225(16) Uani 1 1 d . . . . .
C1 C 0.8289(7) 0.5109(6) 0.7502(6) 0.0199(16) Uani 1 1 d . . . . .
C5 C 0.9529(7) 0.3464(6) 0.7293(6) 0.0218(16) Uani 1 1 d . . . . .
H5 H 0.989014 0.299780 0.688405 0.026 Uiso 1 1 calc R U . . .
C24 C 1.0390(8) 0.2192(7) 0.8681(7) 0.0230(17) Uani 1 1 d . . . . .
C16 C 0.2899(7) 0.8636(6) 0.4351(6) 0.0209(7) Uani 1 1 d . . . . .
C3 C 0.9182(7) 0.3970(6) 0.8798(6) 0.0207(16) Uani 1 1 d . . . . .
H3 H 0.931914 0.383042 0.944345 0.025 Uiso 1 1 calc R U . . .
C31 C 0.0693(8) 0.8937(7) 0.4310(7) 0.0284(19) Uani 1 1 d . . . . .
H31A H 0.057626 0.815456 0.455316 0.043 Uiso 1 1 calc R U . . .
H31B H 0.017904 0.930957 0.386808 0.043 Uiso 1 1 calc R U . . .
H31C H 0.043214 0.918400 0.492300 0.043 Uiso 1 1 calc R U . . .
C2 C 0.8465(7) 0.4895(7) 0.8472(6) 0.0214(16) Uani 1 1 d . . . . .
C23 C 0.8129(9) 0.5270(8) 1.0162(7) 0.033(2) Uani 1 1 d . . . . .
H23A H 0.784607 0.452498 1.056123 0.049 Uiso 1 1 calc R U . . .
H23B H 0.767028 0.573999 1.058024 0.049 Uiso 1 1 calc R U . . .
H23C H 0.903710 0.529839 1.001220 0.049 Uiso 1 1 calc R U . . .
C21 C 0.8400(9) 0.6782(7) 0.8499(7) 0.031(2) Uani 1 1 d . . . . .
H21A H 0.931247 0.675148 0.835271 0.047 Uiso 1 1 calc R U . . .
H21B H 0.799258 0.726458 0.891358 0.047 Uiso 1 1 calc R U . . .
H21C H 0.823735 0.705628 0.782981 0.047 Uiso 1 1 calc R U . . .
C19 C 0.4458(7) 0.7802(6) 0.5605(6) 0.0209(7) Uani 1 1 d . . . . .
C34 C 0.3010(9) 0.7875(7) 0.7851(7) 0.0295(19) Uani 1 1 d . . . . .
H34A H 0.375714 0.739472 0.776233 0.044 Uiso 1 1 calc R U . . .
H34B H 0.227341 0.748876 0.796615 0.044 Uiso 1 1 calc R U . . .
H34C H 0.286044 0.810191 0.846172 0.044 Uiso 1 1 calc R U . . .
C4 C 0.9710(7) 0.3236(6) 0.8251(6) 0.0205(16) Uani 1 1 d . . . . .
C27 C 1.0451(9) 0.2052(7) 0.9759(7) 0.0290(19) Uani 1 1 d . . . . .
H27A H 1.083430 0.268927 0.971413 0.043 Uiso 1 1 calc R U . . .
H27B H 1.096159 0.140581 0.997148 0.043 Uiso 1 1 calc R U . . .
H27C H 0.959475 0.197112 1.028368 0.043 Uiso 1 1 calc R U . . .
C33 C 0.4362(9) 0.9490(7) 0.6663(7) 0.0293(19) Uani 1 1 d . . . . .
H33A H 0.421290 0.971057 0.727793 0.044 Uiso 1 1 calc R U . . .
H33B H 0.448753 1.013360 0.603030 0.044 Uiso 1 1 calc R U . . .
H33C H 0.511603 0.901927 0.656408 0.044 Uiso 1 1 calc R U . . .
C29 C 0.2456(9) 0.8827(8) 0.2705(7) 0.033(2) Uani 1 1 d . . . . .
H29A H 0.335711 0.894576 0.229611 0.049 Uiso 1 1 calc R U . . .
H29B H 0.195894 0.924300 0.226053 0.049 Uiso 1 1 calc R U . . .
H29C H 0.228178 0.805572 0.294287 0.049 Uiso 1 1 calc R U . . .
C32 C 0.3229(8) 0.8882(7) 0.6843(7) 0.0284(19) Uani 1 1 d . . . . .
C30 C 0.2242(10) 1.0433(7) 0.3270(8) 0.034(2) Uani 1 1 d . . . . .
H30A H 0.193008 1.068815 0.388075 0.052 Uiso 1 1 calc R U . . .
H30B H 0.175069 1.078373 0.280404 0.052 Uiso 1 1 calc R U . . .
H30C H 0.313401 1.061443 0.288056 0.052 Uiso 1 1 calc R U . . .
C26 C 0.9718(9) 0.1222(7) 0.8775(8) 0.034(2) Uani 1 1 d . . . . .
H26A H 0.881490 0.127145 0.917136 0.051 Uiso 1 1 calc R U . . .
H26B H 1.007746 0.054968 0.914811 0.051 Uiso 1 1 calc R U . . .
H26C H 0.983280 0.122532 0.806657 0.051 Uiso 1 1 calc R U . . .
C25 C 1.1761(8) 0.2191(8) 0.7904(7) 0.032(2) Uani 1 1 d . . . . .
H25A H 1.174916 0.232656 0.719347 0.048 Uiso 1 1 calc R U . . .
H25B H 1.216810 0.148624 0.813812 0.048 Uiso 1 1 calc R U . . .
H25C H 1.223438 0.275954 0.788707 0.048 Uiso 1 1 calc R U . . .
C36 C 0.5748(9) 0.2981(8) 0.8640(8) 0.035(2) Uani 1 1 d . . . . .
H36 H 0.620353 0.359414 0.810639 0.042 Uiso 1 1 calc R U . . .
C35 C 0.2060(9) 0.9608(8) 0.7044(8) 0.036(2) Uani 1 1 d . . . . .
H35A H 0.132229 0.922769 0.715351 0.054 Uiso 1 1 calc R U . . .
H35B H 0.217471 1.027180 0.643191 0.054 Uiso 1 1 calc R U . . .
H35C H 0.192986 0.979290 0.767512 0.054 Uiso 1 1 calc R U . . .
C37 C 0.6129(9) 0.2461(8) 0.9494(8) 0.036(2) Uani 1 1 d . . . . .
H37 H 0.682406 0.271241 0.955636 0.043 Uiso 1 1 calc R U . . .
C40 C 0.4168(10) 0.1829(9) 0.9270(9) 0.044(3) Uani 1 1 d . . . . .
H40 H 0.346850 0.159892 0.919523 0.052 Uiso 1 1 calc R U . . .
C38 C 0.5478(12) 0.1569(10) 1.0255(10) 0.055(3) Uani 1 1 d . . . . .
H38 H 0.573456 0.117698 1.084470 0.066 Uiso 1 1 calc R U . . .
C22 C 0.6435(8) 0.5663(10) 0.9408(9) 0.042(3) Uani 1 1 d . . . . .
H22A H 0.622605 0.592945 0.875953 0.064 Uiso 1 1 calc R U . . .
H22B H 0.603482 0.613558 0.983417 0.064 Uiso 1 1 calc R U . . .
H22C H 0.612582 0.492546 0.981458 0.064 Uiso 1 1 calc R U . . .
C39 C 0.4452(11) 0.1244(10) 1.0161(9) 0.048(3) Uani 1 1 d . . . . .
H39 H 0.396472 0.064373 1.068697 0.058 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.773(6) . ?
U1 O4 2.231(5) . ?
U1 O3 2.241(5) . ?
U1 O2 1.761(6) . ?
U1 N1 2.578(6) . ?
U1 N2 2.532(6) . ?
U1 N3 2.565(6) . ?
O4 C19 1.334(9) . ?
O3 C1 1.324(9) . ?
N1 C7 1.291(10) . ?
N1 C6 1.398(9) . ?
N2 C8 1.349(9) . ?
N2 C12 1.351(10) . ?
N3 C14 1.407(10) . ?
N3 C13 1.274(10) . ?
C8 C9 1.396(10) . ?
C8 C7 1.459(11) . ?
C12 C11 1.372(11) . ?
C12 C13 1.481(11) . ?
C9 H9 0.9500 . ?
C9 C10 1.387(11) . ?
C7 H7 0.9500 . ?
C18 C17 1.377(10) . ?
C18 C19 1.412(11) . ?
C18 C32 1.537(11) . ?
C11 H11 0.9500 . ?
C11 C10 1.383(11) . ?
C28 C16 1.525(11) . ?
C28 C31 1.546(12) . ?
C28 C29 1.512(12) . ?
C28 C30 1.547(12) . ?
N4 C36 1.346(13) . ?
N4 C40 1.298(13) . ?
C6 C1 1.421(10) . ?
C6 C5 1.400(10) . ?
C14 C15 1.394(10) . ?
C14 C19 1.415(11) . ?
C13 H13 0.9500 . ?
C10 H10 0.9500 . ?
C15 H15 0.9500 . ?
C15 C16 1.388(10) . ?
C17 H17 0.9500 . ?
C17 C16 1.417(10) . ?
C20 C2 1.532(10) . ?
C20 C23 1.533(12) . ?
C20 C21 1.515(12) . ?
C20 C22 1.533(12) . ?
C1 C2 1.410(11) . ?
C5 H5 0.9500 . ?
C5 C4 1.393(11) . ?
C24 C4 1.522(11) . ?
C24 C27 1.526(11) . ?
C24 C26 1.534(12) . ?
C24 C25 1.549(12) . ?
C3 H3 0.9500 . ?
C3 C2 1.400(10) . ?
C3 C4 1.398(11) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C34 C32 1.547(12) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C33 C32 1.518(12) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C32 C35 1.520(12) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C36 H36 0.9500 . ?
C36 C37 1.372(13) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C37 H37 0.9500 . ?
C37 C38 1.371(15) . ?
C40 H40 0.9500 . ?
C40 C39 1.371(15) . ?
C38 H38 0.9500 . ?
C38 C39 1.374(16) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C39 H39 0.9500 . ?

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 O4 94.4(2) . . ?
O1 U1 O3 91.4(2) . . ?
O1 U1 N1 92.1(3) . . ?
O1 U1 N2 87.7(2) . . ?
O1 U1 N3 90.3(2) . . ?
O4 U1 O3 103.22(19) . . ?
O4 U1 N1 166.4(2) . . ?
O4 U1 N2 128.9(2) . . ?
O4 U1 N3 65.3(2) . . ?
O3 U1 N1 64.6(2) . . ?
O3 U1 N2 127.8(2) . . ?
O3 U1 N3 168.50(19) . . ?
O2 U1 O1 175.1(3) . . ?
O2 U1 O4 89.7(2) . . ?
O2 U1 O3 90.4(2) . . ?
O2 U1 N1 84.5(2) . . ?
O2 U1 N2 87.6(2) . . ?
O2 U1 N3 88.9(2) . . ?
N2 U1 N1 63.3(2) . . ?
N2 U1 N3 63.6(2) . . ?
N3 U1 N1 126.7(2) . . ?
C19 O4 U1 128.1(5) . . ?
C1 O3 U1 127.1(5) . . ?
C7 N1 U1 120.3(5) . . ?
C7 N1 C6 124.8(7) . . ?
C6 N1 U1 114.8(5) . . ?
C8 N2 U1 120.6(5) . . ?
C8 N2 C12 118.3(7) . . ?
C12 N2 U1 121.0(5) . . ?
C14 N3 U1 115.1(5) . . ?
C13 N3 U1 120.5(5) . . ?
C13 N3 C14 124.4(7) . . ?
N2 C8 C9 121.9(7) . . ?
N2 C8 C7 116.8(7) . . ?
C9 C8 C7 121.3(7) . . ?
N2 C12 C11 123.0(7) . . ?
N2 C12 C13 115.3(7) . . ?
C11 C12 C13 121.7(7) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 C8 118.6(7) . . ?
C10 C9 H9 120.7 . . ?
N1 C7 C8 118.4(7) . . ?
N1 C7 H7 120.8 . . ?
C8 C7 H7 120.8 . . ?
C17 C18 C19 117.4(7) . . ?
C17 C18 C32 122.0(7) . . ?
C19 C18 C32 120.6(7) . . ?
C12 C11 H11 120.6 . . ?
C12 C11 C10 118.7(7) . . ?
C10 C11 H11 120.6 . . ?
C16 C28 C31 109.5(7) . . ?
C16 C28 C30 110.0(7) . . ?
C29 C28 C16 112.7(7) . . ?
C29 C28 C31 107.8(7) . . ?
C29 C28 C30 108.9(8) . . ?
C30 C28 C31 107.9(7) . . ?
C40 N4 C36 115.9(9) . . ?
N1 C6 C1 113.2(6) . . ?
N1 C6 C5 125.2(7) . . ?
C5 C6 C1 121.5(7) . . ?
N3 C14 C19 113.6(7) . . ?
C15 C14 N3 124.1(7) . . ?
C15 C14 C19 122.3(7) . . ?
N3 C13 C12 119.4(7) . . ?
N3 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C9 C10 H10 120.3 . . ?
C11 C10 C9 119.5(7) . . ?
C11 C10 H10 120.3 . . ?
C14 C15 H15 120.3 . . ?
C16 C15 C14 119.5(7) . . ?
C16 C15 H15 120.3 . . ?
C18 C17 H17 117.7 . . ?
C18 C17 C16 124.6(7) . . ?
C16 C17 H17 117.7 . . ?
C2 C20 C23 112.0(7) . . ?
C2 C20 C22 108.2(7) . . ?
C21 C20 C2 110.4(7) . . ?
C21 C20 C23 107.6(7) . . ?
C21 C20 C22 111.8(8) . . ?
C22 C20 C23 106.8(8) . . ?
O3 C1 C6 117.7(7) . . ?
O3 C1 C2 123.3(7) . . ?
C2 C1 C6 119.0(7) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 C6 120.5(7) . . ?
C4 C5 H5 119.8 . . ?
C4 C24 C27 112.6(7) . . ?
C4 C24 C26 109.6(6) . . ?
C4 C24 C25 109.5(7) . . ?
C27 C24 C26 109.1(7) . . ?
C27 C24 C25 107.9(7) . . ?
C26 C24 C25 108.1(7) . . ?
C15 C16 C28 122.6(7) . . ?
C15 C16 C17 117.3(7) . . ?
C17 C16 C28 120.0(7) . . ?
C2 C3 H3 117.4 . . ?
C4 C3 H3 117.4 . . ?
C4 C3 C2 125.3(7) . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C1 C2 C20 119.8(7) . . ?
C3 C2 C20 123.3(7) . . ?
C3 C2 C1 117.0(7) . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O4 C19 C18 123.7(7) . . ?
O4 C19 C14 117.7(7) . . ?
C18 C19 C14 118.6(7) . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
C5 C4 C24 119.8(7) . . ?
C5 C4 C3 116.8(7) . . ?
C3 C4 C24 123.3(7) . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C18 C32 C34 109.7(7) . . ?
C33 C32 C18 109.6(7) . . ?
C33 C32 C34 109.8(7) . . ?
C33 C32 C35 108.6(8) . . ?
C35 C32 C18 112.0(7) . . ?
C35 C32 C34 106.9(8) . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N4 C36 H36 118.3 . . ?
N4 C36 C37 123.4(9) . . ?
C37 C36 H36 118.3 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C36 C37 H37 121.0 . . ?
C38 C37 C36 118.0(9) . . ?
C38 C37 H37 121.0 . . ?
N4 C40 H40 116.9 . . ?
N4 C40 C39 126.2(10) . . ?
C39 C40 H40 116.9 . . ?
C37 C38 H38 120.1 . . ?
C37 C38 C39 119.8(10) . . ?
C39 C38 H38 120.1 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C40 C39 C38 116.6(10) . . ?
C40 C39 H39 121.7 . . ?
C38 C39 H39 121.7 . . ?

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 O4 C19 C18 174.5(6) . . . . ?
U1 O4 C19 C14 -5.4(11) . . . . ?
U1 O3 C1 C6 17.8(10) . . . . ?
U1 O3 C1 C2 -161.0(6) . . . . ?
U1 N1 C7 C8 -5.5(10) . . . . ?
U1 N1 C6 C1 -6.8(9) . . . . ?
U1 N1 C6 C5 168.5(7) . . . . ?
U1 N2 C8 C9 -174.4(6) . . . . ?
U1 N2 C8 C7 7.0(10) . . . . ?
U1 N2 C12 C11 176.6(6) . . . . ?
U1 N2 C12 C13 -4.3(9) . . . . ?
U1 N3 C14 C15 176.8(6) . . . . ?
U1 N3 C14 C19 -2.8(9) . . . . ?
U1 N3 C13 C12 -1.5(10) . . . . ?
O3 C1 C2 C20 0.6(12) . . . . ?
O3 C1 C2 C3 -180.0(7) . . . . ?
N1 C6 C1 O3 -4.8(11) . . . . ?
N1 C6 C1 C2 174.0(7) . . . . ?
N1 C6 C5 C4 -173.2(8) . . . . ?
N2 C8 C9 C10 -1.7(12) . . . . ?
N2 C8 C7 N1 -0.9(11) . . . . ?
N2 C12 C11 C10 -2.7(12) . . . . ?
N2 C12 C13 N3 3.8(11) . . . . ?
N3 C14 C15 C16 178.1(8) . . . . ?
N3 C14 C19 O4 5.0(11) . . . . ?
N3 C14 C19 C18 -174.9(7) . . . . ?
C8 N2 C12 C11 0.8(12) . . . . ?
C8 N2 C12 C13 179.9(7) . . . . ?
C8 C9 C10 C11 -0.3(12) . . . . ?
C12 N2 C8 C9 1.5(12) . . . . ?
C12 N2 C8 C7 -177.2(7) . . . . ?
C12 C11 C10 C9 2.4(13) . . . . ?
C9 C8 C7 N1 -179.6(8) . . . . ?
C7 N1 C6 C1 174.5(8) . . . . ?
C7 N1 C6 C5 -10.2(13) . . . . ?
C7 C8 C9 C10 176.9(8) . . . . ?
C18 C17 C16 C28 -173.9(8) . . . . ?
C18 C17 C16 C15 4.3(13) . . . . ?
C11 C12 C13 N3 -177.1(8) . . . . ?
N4 C36 C37 C38 0.8(16) . . . . ?
N4 C40 C39 C38 -1.1(19) . . . . ?
C6 N1 C7 C8 173.2(7) . . . . ?
C6 C1 C2 C20 -178.2(7) . . . . ?
C6 C1 C2 C3 1.2(11) . . . . ?
C6 C5 C4 C24 174.8(7) . . . . ?
C6 C5 C4 C3 -1.7(12) . . . . ?
C14 N3 C13 C12 179.8(7) . . . . ?
C14 C15 C16 C28 175.6(8) . . . . ?
C14 C15 C16 C17 -2.5(12) . . . . ?
C13 N3 C14 C15 -4.4(13) . . . . ?
C13 N3 C14 C19 175.9(8) . . . . ?
C13 C12 C11 C10 178.2(8) . . . . ?
C15 C14 C19 O4 -174.7(7) . . . . ?
C15 C14 C19 C18 5.4(13) . . . . ?
C17 C18 C19 O4 176.5(8) . . . . ?
C17 C18 C19 C14 -3.7(12) . . . . ?
C17 C18 C32 C34 122.6(9) . . . . ?
C17 C18 C32 C33 -116.6(9) . . . . ?
C17 C18 C32 C35 4.1(12) . . . . ?
C1 C6 C5 C4 1.7(12) . . . . ?
C5 C6 C1 O3 179.7(7) . . . . ?
C5 C6 C1 C2 -1.5(12) . . . . ?
C31 C28 C16 C15 119.8(9) . . . . ?
C31 C28 C16 C17 -62.1(10) . . . . ?
C2 C3 C4 C5 1.6(12) . . . . ?
C2 C3 C4 C24 -174.8(8) . . . . ?
C23 C20 C2 C1 178.0(8) . . . . ?
C23 C20 C2 C3 -1.3(12) . . . . ?
C21 C20 C2 C1 -62.1(10) . . . . ?
C21 C20 C2 C3 118.5(9) . . . . ?
C19 C18 C17 C16 -1.1(13) . . . . ?
C19 C18 C32 C34 -57.6(10) . . . . ?
C19 C18 C32 C33 63.1(10) . . . . ?
C19 C18 C32 C35 -176.2(8) . . . . ?
C19 C14 C15 C16 -2.2(13) . . . . ?
C4 C3 C2 C20 178.1(8) . . . . ?
C4 C3 C2 C1 -1.4(13) . . . . ?
C27 C24 C4 C5 -177.4(7) . . . . ?
C27 C24 C4 C3 -1.1(11) . . . . ?
C29 C28 C16 C15 -0.1(12) . . . . ?
C29 C28 C16 C17 177.9(8) . . . . ?
C32 C18 C17 C16 178.7(8) . . . . ?
C32 C18 C19 O4 -3.3(13) . . . . ?
C32 C18 C19 C14 176.5(8) . . . . ?
C30 C28 C16 C15 -121.8(9) . . . . ?
C30 C28 C16 C17 56.3(11) . . . . ?
C26 C24 C4 C5 -55.8(10) . . . . ?
C26 C24 C4 C3 120.4(9) . . . . ?
C25 C24 C4 C5 62.6(10) . . . . ?
C25 C24 C4 C3 -121.2(8) . . . . ?
C36 N4 C40 C39 -0.1(17) . . . . ?
C36 C37 C38 C39 -2.0(17) . . . . ?
C37 C38 C39 C40 2.2(18) . . . . ?
C40 N4 C36 C37 0.3(15) . . . . ?
C22 C20 C2 C1 60.6(10) . . . . ?
C22 C20 C2 C3 -118.8(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.301
_oxdiff_exptl_absorpt_empirical_full_min 0.805

# start Validation Reply Form
_vrf_PLAT971_201116_uo2_tbupdiop_red2 
;
PROBLEM: Check Calcd Resid. Dens.  0.92A   From U1               7.13 eA-3
PROBLEM: Check Calcd Resid. Dens.  0.93A   From U1               6.94 eA-3
PROBLEM: Check Calcd Resid. Dens.  0.97A   From U1               4.07 eA-3
PROBLEM: Check Calcd Resid. Dens.  0.97A   From U1               4.03 eA-3
PROBLEM: Check Calcd Resid. Dens.  0.21A   From U1               3.33 eA-3 
RESPONSE: We think that the insufficient or incorrect absorption 
correction is responsible of the residual densities. 
We applied the numerical absorption correction by using 
indexed crystal faces. Even though, the large peaks 
around U atoms remained. No better results have 
been obtained in use of the empirical absorption 
correction with strong absorber options. 
Despite many trials, we cannot correct this issue. 
Such an observation is frequently occurred 
in the compounds including a heavy atom. 
;
_vrf_PLAT972_201116_uo2_tbupdiop_red2 
;
PROBLEM: Check Calcd Resid. Dens.  0.81A    From U1             -4.93 eA-3
PROBLEM: Check Calcd Resid. Dens.  0.81A    From U1             -4.53 eA-3
RESPONSE: We think that the insufficient or incorrect absorption 
correction is responsible of the residual densities. 
We applied the numerical absorption correction by using 
indexed crystal faces. Even though, the large peaks 
around U atoms remained. No better results have 
been obtained in use of the empirical absorption 
correction with strong absorber options. 
Despite many trials, we cannot correct this issue. 
Such an observation is frequently occurred 
in the compounds including a heavy atom. 
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_UO2tBupdaop
_database_code_depnum_ccdc_archive 'CCDC 2118196'
loop_
_audit_author_name
_audit_author_address
'Tomoyuki Takeyama'
;Tokyo Institute of Technology
Japan
;
_audit_update_record             
;
2022-04-05 deposited with the CCDC.	2022-04-06 downloaded from the CCDC.
;
_audit_creation_date             2021-03-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C35 H49 N3 O4 U, C H2 Cl2'
_chemical_formula_sum            'C36 H51 Cl2 N3 O4 U'
_chemical_formula_weight         898.72
_chemical_melting_point          ?
_chemical_oxdiff_formula         C35H49N3O4U1Cl2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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'

_cell_length_a                   13.9394(7)
_cell_length_b                   13.7474(11)
_cell_length_c                   21.7612(11)
_cell_angle_alpha                90
_cell_angle_beta                 91.234(4)
_cell_angle_gamma                90
_cell_volume                     4169.1(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3838
_cell_measurement_temperature    123
_cell_measurement_theta_max      74.4720
_cell_measurement_theta_min      3.7790
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.423
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1784
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -9 0 0.1749
0 9 0 0.0811
-2 0 -14 0.0054
2 0 14 0.0072
9 0 -2 0.0072
-9 0 2 0.0144

_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.013
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.5443 -8.9064 0.1619 -0.0171 0.0591 0.9981
0.0671 8.9224 0.1743 -0.0412 -0.0166 -0.9990
-1.9987 0.0013 -13.9973 0.9531 0.3622 -0.0324
1.9987 -0.0013 13.9973 -0.9531 -0.3622 0.0324
9.0007 0.0037 -1.9992 -0.4469 0.8968 -0.0031
-9.0007 -0.0037 1.9992 0.4469 -0.8968 0.0031

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1993
_diffrn_reflns_av_unetI/netI     0.1915
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25037
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.013
_diffrn_reflns_theta_min         3.803
_diffrn_ambient_temperature      123
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -27.00  23.00   0.50   40.00    --    0.00  77.00 -90.00  100
  2  ω     18.00  86.00   0.50   40.00    --    0.00  82.00 -60.00  136
  3  ω    -22.00   6.00   0.50   40.00    --    0.00 -37.00-120.00   56
  4  ω     45.00  78.00   0.50   40.00    --    0.00  77.00 -90.00   66
  5  ω    -72.00 -47.00   0.50   40.00    --    0.00 -37.00-120.00   50
  6  ω    -29.00   4.00   0.50   40.00    --    0.00  82.00 -60.00   66
  7  ω     93.00 118.00   0.50  120.00    --   96.10 -82.00 -60.00   50
  8  ω      8.00 107.00   0.50  120.00    --   96.10 -30.00 150.00  198
  9  ω      8.00  33.00   0.50  120.00    --   96.10   0.00-180.00   50
 10  ω     10.00 119.00   0.50  120.00    --   96.10 -15.00-150.00  218
 11  ω     27.00 111.00   0.50  120.00    --   96.10 -30.00  60.00  168
 12  ω     16.00 118.00   0.50  120.00    --   96.10 -61.00-180.00  204
 13  ω     83.00 108.00   0.50  120.00    --   96.10 -82.00 -30.00   50
 14  ω     77.00 104.00   0.50  120.00    --   96.10 -82.00   0.00   54
 15  ω     73.00 119.00   0.50  120.00    --   96.10 -82.00 -90.00   92
 16  ω    134.00 159.00   0.50  120.00    --   96.10   0.00-180.00   50
 17  ω     82.00 126.00   0.50  120.00    --   96.10 -82.00  52.39   88
 18  ω     49.00 114.00   0.50  120.00    --   96.10 -82.00  22.85  130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual home/near'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0627822000
_diffrn_orient_matrix_UB_12      -0.0029918000
_diffrn_orient_matrix_UB_13      -0.0591262000
_diffrn_orient_matrix_UB_21      0.0910069000
_diffrn_orient_matrix_UB_22      -0.0017810000
_diffrn_orient_matrix_UB_23      -0.0388745000
_diffrn_orient_matrix_UB_31      0.0002089000
_diffrn_orient_matrix_UB_32      -0.1120126000
_diffrn_orient_matrix_UB_33      0.0022736000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3745
_reflns_number_total             8183
_reflns_odcompleteness_completeness 99.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         3.182
_refine_diff_density_min         -6.316
_refine_diff_density_rms         0.301
_refine_ls_extinction_coef       0.00029(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         8183
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1934
_refine_ls_R_factor_gt           0.1061
_refine_ls_restrained_S_all      1.016
_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)+(0.1876P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2765
_refine_ls_wR_factor_ref         0.3447
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C6) = Uanis(C1) = Uanis(C2)
Uanis(C19) = Uanis(C14) = Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C18)
Uanis(O3) = Uanis(O4) = Uanis(N3) = Uanis(N2) = Uanis(N1)
Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(C10) = Uanis(C11) = Uanis(C12) =
Uanis(C13)
Uanis(C23) = Uanis(C21) = Uanis(C20) = Uanis(C22)
Uanis(C25) = Uanis(C26) = Uanis(C24) = Uanis(C27)
Uanis(C32) = Uanis(C33) = Uanis(C34) = Uanis(C35)
Uanis(C30) = Uanis(C29) = Uanis(C31) = Uanis(C28)
Uanis(O1) = Uanis(O2)
Uanis(O3) = Uanis(N1) = Uanis(N2) = Uanis(O1) = Uanis(O2) = Uanis(O4) =
Uanis(N3)
Uanis(C36) = Uanis(Cl2) = Uanis(Cl1)
3.a Ternary CH refined with riding coordinates:
 N1(H1), N3(H3)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C13(H13A,H13B), C36(H36A,H36B)
3.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C17(H17), C11(H11), C5(H5), C3(H3A), C10(H10), C15(H15)
3.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C35(H35A,H35B,H35C), C31(H31A,H31B,H31C), C22(H22A,H22B,
 H22C), C33(H33A,H33B,H33C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C34(H34A,
 H34B,H34C), C21(H21A,H21B,H21C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C),
 C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.62291(4) 0.41065(7) 0.71521(3) 0.0573(4) Uani 1 1 d . . . . .
Cl1 Cl 0.3923(4) 0.1232(6) 0.6653(3) 0.0832(15) Uani 1 1 d . . . . .
Cl2 Cl 0.2218(4) 0.2347(6) 0.6973(3) 0.0832(15) Uani 1 1 d . . . . .
O3 O 0.5473(10) 0.4029(12) 0.8024(7) 0.0639(18) Uani 1 1 d . . . . .
O4 O 0.5801(10) 0.5601(13) 0.6876(6) 0.0639(18) Uani 1 1 d . . . . .
N1 N 0.6354(12) 0.2439(16) 0.7672(8) 0.0639(18) Uani 1 1 d . . . . .
H1 H 0.692188 0.245858 0.796003 0.077 Uiso 1 1 calc R U . . .
O1 O 0.7299(9) 0.4507(14) 0.7528(6) 0.0639(18) Uani 1 1 d . . . . .
N2 N 0.7298(12) 0.2880(17) 0.6612(8) 0.0639(18) Uani 1 1 d . . . . .
C14 C 0.7007(13) 0.5794(19) 0.6165(9) 0.057(3) Uani 1 1 d . . . . .
C9 C 0.7778(13) 0.130(2) 0.6453(9) 0.063(3) Uani 1 1 d . . . . .
H9 H 0.771921 0.063375 0.655623 0.075 Uiso 1 1 calc R U . . .
C32 C 0.7995(14) 0.795(2) 0.5288(9) 0.067(4) Uani 1 1 d . . . . .
C17 C 0.6735(12) 0.774(2) 0.6105(8) 0.057(3) Uani 1 1 d . . . . .
H17 H 0.664325 0.842567 0.609286 0.069 Uiso 1 1 calc R U . . .
C8 C 0.7228(13) 0.197(2) 0.6762(9) 0.063(3) Uani 1 1 d . . . . .
C16 C 0.7450(13) 0.734(2) 0.5755(8) 0.057(3) Uani 1 1 d . . . . .
C6 C 0.5499(12) 0.229(2) 0.8044(8) 0.060(3) Uani 1 1 d . . . . .
C23 C 0.2806(13) 0.3898(19) 0.9088(10) 0.061(3) Uani 1 1 d . . . . .
H23A H 0.233980 0.351525 0.884625 0.092 Uiso 1 1 calc R U . . .
H23B H 0.250389 0.450284 0.922340 0.092 Uiso 1 1 calc R U . . .
H23C H 0.302021 0.352170 0.944803 0.092 Uiso 1 1 calc R U . . .
C11 C 0.8467(13) 0.253(2) 0.5867(9) 0.063(3) Uani 1 1 d . . . . .
H11 H 0.889796 0.274372 0.556332 0.075 Uiso 1 1 calc R U . . .
C28 C 0.5343(13) 0.769(2) 0.6854(9) 0.074(4) Uani 1 1 d . . . . .
C20 C 0.3676(14) 0.4140(19) 0.8689(10) 0.061(3) Uani 1 1 d . . . . .
O2 O 0.5275(9) 0.3613(14) 0.6729(6) 0.0639(18) Uani 1 1 d . . . . .
C2 C 0.4209(12) 0.313(2) 0.8550(8) 0.060(3) Uani 1 1 d . . . . .
N3 N 0.7027(12) 0.4691(17) 0.6149(8) 0.0639(18) Uani 1 1 d . . . . .
H3 H 0.663072 0.446253 0.578846 0.077 Uiso 1 1 calc R U . . .
C4 C 0.4274(12) 0.137(2) 0.8547(8) 0.060(3) Uani 1 1 d . . . . .
C18 C 0.6127(13) 0.717(2) 0.6484(8) 0.057(3) Uani 1 1 d . . . . .
C5 C 0.5134(12) 0.142(2) 0.8216(8) 0.060(3) Uani 1 1 d . . . . .
H5 H 0.546083 0.083830 0.811289 0.072 Uiso 1 1 calc R U . . .
C7 C 0.6501(14) 0.159(2) 0.7230(9) 0.063(3) Uani 1 1 d . . . . .
H7A H 0.588909 0.140527 0.702182 0.075 Uiso 1 1 calc R U . . .
H7B H 0.676158 0.101438 0.745195 0.075 Uiso 1 1 calc R U . . .
C3 C 0.3837(12) 0.225(2) 0.8705(8) 0.060(3) Uani 1 1 d . . . . .
H3A H 0.325986 0.223395 0.892915 0.072 Uiso 1 1 calc R U . . .
C10 C 0.8392(13) 0.155(2) 0.6013(9) 0.063(3) Uani 1 1 d . . . . .
H10 H 0.876305 0.107788 0.580878 0.075 Uiso 1 1 calc R U . . .
C35 C 0.7413(14) 0.800(2) 0.4700(9) 0.067(4) Uani 1 1 d . . . . .
H35A H 0.728401 0.734500 0.454643 0.101 Uiso 1 1 calc R U . . .
H35B H 0.777067 0.836857 0.439328 0.101 Uiso 1 1 calc R U . . .
H35C H 0.680401 0.833404 0.477631 0.101 Uiso 1 1 calc R U . . .
C19 C 0.6305(13) 0.621(2) 0.6529(9) 0.057(3) Uani 1 1 d . . . . .
C31 C 0.5258(13) 0.881(2) 0.6721(10) 0.074(4) Uani 1 1 d . . . . .
H31A H 0.573617 0.916407 0.697232 0.111 Uiso 1 1 calc R U . . .
H31B H 0.461376 0.903786 0.682345 0.111 Uiso 1 1 calc R U . . .
H31C H 0.537143 0.893546 0.628508 0.111 Uiso 1 1 calc R U . . .
C1 C 0.5051(12) 0.319(2) 0.8193(8) 0.060(3) Uani 1 1 d . . . . .
C22 C 0.3287(13) 0.455(2) 0.8085(9) 0.061(3) Uani 1 1 d . . . . .
H22A H 0.276254 0.413737 0.792981 0.092 Uiso 1 1 calc R U . . .
H22B H 0.380087 0.456555 0.778448 0.092 Uiso 1 1 calc R U . . .
H22C H 0.304806 0.521121 0.815096 0.092 Uiso 1 1 calc R U . . .
C33 C 0.8999(13) 0.755(2) 0.5169(9) 0.067(4) Uani 1 1 d . . . . .
H33A H 0.938688 0.757983 0.554951 0.101 Uiso 1 1 calc R U . . .
H33B H 0.930286 0.794904 0.485299 0.101 Uiso 1 1 calc R U . . .
H33C H 0.895248 0.687733 0.502730 0.101 Uiso 1 1 calc R U . . .
C24 C 0.3789(18) 0.041(3) 0.8742(13) 0.086(4) Uani 1 1 d . . . . .
C29 C 0.5439(13) 0.750(2) 0.7542(9) 0.074(4) Uani 1 1 d . . . . .
H29A H 0.573072 0.686312 0.761397 0.111 Uiso 1 1 calc R U . . .
H29B H 0.480225 0.751991 0.772409 0.111 Uiso 1 1 calc R U . . .
H29C H 0.584514 0.800703 0.773059 0.111 Uiso 1 1 calc R U . . .
C12 C 0.7874(13) 0.322(2) 0.6187(9) 0.063(3) Uani 1 1 d . . . . .
C15 C 0.7580(13) 0.632(2) 0.5787(8) 0.057(3) Uani 1 1 d . . . . .
H15 H 0.805644 0.601224 0.555155 0.069 Uiso 1 1 calc R U . . .
C30 C 0.4360(12) 0.722(2) 0.6642(9) 0.074(4) Uani 1 1 d . . . . .
H30A H 0.436473 0.710264 0.619813 0.111 Uiso 1 1 calc R U . . .
H30B H 0.383568 0.766701 0.673756 0.111 Uiso 1 1 calc R U . . .
H30C H 0.426779 0.660390 0.685839 0.111 Uiso 1 1 calc R U . . .
C13 C 0.7934(13) 0.429(2) 0.6114(9) 0.063(3) Uani 1 1 d . . . . .
H13A H 0.835610 0.456682 0.644076 0.075 Uiso 1 1 calc R U . . .
H13B H 0.821235 0.444869 0.571128 0.075 Uiso 1 1 calc R U . . .
C34 C 0.8125(15) 0.8984(19) 0.5536(10) 0.067(4) Uani 1 1 d . . . . .
H34A H 0.749472 0.928756 0.558278 0.101 Uiso 1 1 calc R U . . .
H34B H 0.850267 0.936516 0.524777 0.101 Uiso 1 1 calc R U . . .
H34C H 0.846044 0.896074 0.593626 0.101 Uiso 1 1 calc R U . . .
C21 C 0.4351(13) 0.4825(19) 0.9048(10) 0.061(3) Uani 1 1 d . . . . .
H21A H 0.411853 0.549521 0.900750 0.092 Uiso 1 1 calc R U . . .
H21B H 0.499817 0.477828 0.888418 0.092 Uiso 1 1 calc R U . . .
H21C H 0.436636 0.463902 0.948322 0.092 Uiso 1 1 calc R U . . .
C36 C 0.3472(15) 0.230(2) 0.7022(12) 0.0832(15) Uani 1 1 d . . . . .
H36A H 0.368061 0.229548 0.745968 0.100 Uiso 1 1 calc R U . . .
H36B H 0.374262 0.288286 0.682615 0.100 Uiso 1 1 calc R U . . .
C26 C 0.3632(17) 0.044(2) 0.9413(12) 0.086(4) Uani 1 1 d . . . . .
H26A H 0.337718 -0.018913 0.954836 0.129 Uiso 1 1 calc R U . . .
H26B H 0.317280 0.095464 0.950560 0.129 Uiso 1 1 calc R U . . .
H26C H 0.424249 0.056823 0.962968 0.129 Uiso 1 1 calc R U . . .
C25 C 0.4396(18) -0.045(2) 0.8577(13) 0.086(4) Uani 1 1 d . . . . .
H25A H 0.500034 -0.042340 0.881466 0.129 Uiso 1 1 calc R U . . .
H25B H 0.453131 -0.042403 0.813692 0.129 Uiso 1 1 calc R U . . .
H25C H 0.405330 -0.104815 0.867037 0.129 Uiso 1 1 calc R U . . .
C27 C 0.2793(17) 0.036(2) 0.8412(12) 0.086(4) Uani 1 1 d . . . . .
H27A H 0.244554 -0.021474 0.855095 0.129 Uiso 1 1 calc R U . . .
H27B H 0.287749 0.032458 0.796681 0.129 Uiso 1 1 calc R U . . .
H27C H 0.242489 0.094740 0.851010 0.129 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 O3 2.193(14) . ?
U1 O4 2.220(18) . ?
U1 N1 2.56(2) . ?
U1 O1 1.773(14) . ?
U1 N2 2.554(19) . ?
U1 O2 1.738(14) . ?
U1 N3 2.599(17) . ?
Cl1 C36 1.79(3) . ?
Cl2 C36 1.75(2) . ?
O3 C1 1.35(3) . ?
O4 C19 1.34(3) . ?
N1 H1 1.0000 . ?
N1 C6 1.47(2) . ?
N1 C7 1.53(3) . ?
N2 C8 1.29(3) . ?
N2 C12 1.32(2) . ?
C14 N3 1.52(3) . ?
C14 C19 1.40(3) . ?
C14 C15 1.37(3) . ?
C9 H9 0.9500 . ?
C9 C8 1.38(3) . ?
C9 C10 1.34(3) . ?
C32 C16 1.53(3) . ?
C32 C35 1.50(3) . ?
C32 C33 1.53(3) . ?
C32 C34 1.53(3) . ?
C17 H17 0.9500 . ?
C17 C16 1.39(2) . ?
C17 C18 1.43(3) . ?
C8 C7 1.55(3) . ?
C16 C15 1.40(3) . ?
C6 C5 1.36(3) . ?
C6 C1 1.42(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C23 C20 1.54(3) . ?
C11 H11 0.9500 . ?
C11 C10 1.38(3) . ?
C11 C12 1.44(3) . ?
C28 C18 1.55(3) . ?
C28 C31 1.58(4) . ?
C28 C29 1.52(3) . ?
C28 C30 1.57(3) . ?
C20 C2 1.61(3) . ?
C20 C22 1.52(3) . ?
C20 C21 1.53(3) . ?
C2 C3 1.36(3) . ?
C2 C1 1.42(2) . ?
N3 H3 1.0000 . ?
N3 C13 1.38(3) . ?
C4 C5 1.41(2) . ?
C4 C3 1.40(3) . ?
C4 C24 1.55(4) . ?
C18 C19 1.33(3) . ?
C5 H5 0.9500 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C3 H3A 0.9500 . ?
C10 H10 0.9500 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C24 C26 1.48(4) . ?
C24 C25 1.49(4) . ?
C24 C27 1.55(3) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C12 C13 1.49(3) . ?
C15 H15 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?

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
O3 U1 O4 98.5(6) . . ?
O3 U1 N1 66.6(6) . . ?
O3 U1 N2 131.5(6) . . ?
O3 U1 N3 164.7(7) . . ?
O4 U1 N1 164.6(5) . . ?
O4 U1 N2 130.0(6) . . ?
O4 U1 N3 66.6(6) . . ?
N1 U1 N3 128.4(6) . . ?
O1 U1 O3 91.8(6) . . ?
O1 U1 O4 93.2(7) . . ?
O1 U1 N1 91.5(7) . . ?
O1 U1 N2 85.6(7) . . ?
O1 U1 N3 85.4(6) . . ?
N2 U1 N1 65.0(6) . . ?
N2 U1 N3 63.4(7) . . ?
O2 U1 O3 93.6(6) . . ?
O2 U1 O4 91.1(7) . . ?
O2 U1 N1 85.9(7) . . ?
O2 U1 O1 172.5(7) . . ?
O2 U1 N2 86.9(7) . . ?
O2 U1 N3 90.7(6) . . ?
C1 O3 U1 119.8(13) . . ?
C19 O4 U1 126.4(13) . . ?
U1 N1 H1 107.4 . . ?
C6 N1 U1 108.7(14) . . ?
C6 N1 H1 107.4 . . ?
C6 N1 C7 111.2(18) . . ?
C7 N1 U1 114.6(12) . . ?
C7 N1 H1 107.4 . . ?
C8 N2 U1 118.2(13) . . ?
C8 N2 C12 124(2) . . ?
C12 N2 U1 117.4(18) . . ?
C19 C14 N3 116(2) . . ?
C15 C14 N3 120.4(19) . . ?
C15 C14 C19 123(2) . . ?
C8 C9 H9 118.6 . . ?
C10 C9 H9 118.6 . . ?
C10 C9 C8 123(3) . . ?
C16 C32 C34 109.4(18) . . ?
C35 C32 C16 109.1(17) . . ?
C35 C32 C33 110.7(18) . . ?
C35 C32 C34 108(2) . . ?
C33 C32 C16 113(2) . . ?
C33 C32 C34 106.7(19) . . ?
C16 C17 H17 118.8 . . ?
C16 C17 C18 122(2) . . ?
C18 C17 H17 118.8 . . ?
N2 C8 C9 118(2) . . ?
N2 C8 C7 123(2) . . ?
C9 C8 C7 118(2) . . ?
C17 C16 C32 121(2) . . ?
C17 C16 C15 118(2) . . ?
C15 C16 C32 120.8(19) . . ?
C5 C6 N1 126(2) . . ?
C5 C6 C1 122.1(17) . . ?
C1 C6 N1 112(2) . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
C10 C11 H11 120.8 . . ?
C10 C11 C12 118(2) . . ?
C12 C11 H11 120.8 . . ?
C18 C28 C31 114.1(19) . . ?
C18 C28 C30 106(2) . . ?
C29 C28 C18 112.9(17) . . ?
C29 C28 C31 110(2) . . ?
C29 C28 C30 106.2(18) . . ?
C30 C28 C31 106.4(17) . . ?
C23 C20 C2 106.9(19) . . ?
C22 C20 C23 107.3(16) . . ?
C22 C20 C2 108.4(17) . . ?
C22 C20 C21 115(2) . . ?
C21 C20 C23 109.0(17) . . ?
C21 C20 C2 110.2(16) . . ?
C3 C2 C20 122.7(16) . . ?
C3 C2 C1 121(2) . . ?
C1 C2 C20 116(2) . . ?
U1 N3 H3 108.8 . . ?
C14 N3 U1 106.3(12) . . ?
C14 N3 H3 108.8 . . ?
C13 N3 U1 109.3(14) . . ?
C13 N3 C14 114.7(18) . . ?
C13 N3 H3 108.8 . . ?
C5 C4 C24 124(3) . . ?
C3 C4 C5 117(2) . . ?
C3 C4 C24 118.5(18) . . ?
C17 C18 C28 119(2) . . ?
C19 C18 C17 118.2(19) . . ?
C19 C18 C28 123(2) . . ?
C6 C5 C4 121(2) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
N1 C7 C8 105(2) . . ?
N1 C7 H7A 110.8 . . ?
N1 C7 H7B 110.8 . . ?
C8 C7 H7A 110.8 . . ?
C8 C7 H7B 110.8 . . ?
H7A C7 H7B 108.9 . . ?
C2 C3 C4 122.5(17) . . ?
C2 C3 H3A 118.8 . . ?
C4 C3 H3A 118.8 . . ?
C9 C10 C11 118(2) . . ?
C9 C10 H10 121.1 . . ?
C11 C10 H10 121.1 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O4 C19 C14 116(2) . . ?
C18 C19 O4 124.0(19) . . ?
C18 C19 C14 120(2) . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O3 C1 C6 118.9(16) . . ?
O3 C1 C2 124(2) . . ?
C6 C1 C2 117(2) . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C4 C24 C27 107(2) . . ?
C26 C24 C4 109(2) . . ?
C26 C24 C25 111(3) . . ?
C26 C24 C27 108(2) . . ?
C25 C24 C4 111(2) . . ?
C25 C24 C27 111(3) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N2 C12 C11 118(2) . . ?
N2 C12 C13 117(2) . . ?
C11 C12 C13 124.2(19) . . ?
C14 C15 C16 119(2) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N3 C13 C12 109.7(18) . . ?
N3 C13 H13A 109.7 . . ?
N3 C13 H13B 109.7 . . ?
C12 C13 H13A 109.7 . . ?
C12 C13 H13B 109.7 . . ?
H13A C13 H13B 108.2 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Cl1 C36 H36A 109.3 . . ?
Cl1 C36 H36B 109.3 . . ?
Cl2 C36 Cl1 111.4(15) . . ?
Cl2 C36 H36A 109.3 . . ?
Cl2 C36 H36B 109.3 . . ?
H36A C36 H36B 108.0 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?

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 C6 36(2) . . . . ?
U1 O3 C1 C2 -148.6(14) . . . . ?
U1 O4 C19 C14 20(2) . . . . ?
U1 O4 C19 C18 -164.9(15) . . . . ?
U1 N1 C6 C5 156.3(15) . . . . ?
U1 N1 C6 C1 -21.4(17) . . . . ?
U1 N1 C7 C8 41.2(17) . . . . ?
U1 N2 C8 C9 177.5(13) . . . . ?
U1 N2 C8 C7 3(3) . . . . ?
U1 N2 C12 C11 -178.6(13) . . . . ?
U1 N2 C12 C13 7(2) . . . . ?
U1 N3 C13 C12 53.0(19) . . . . ?
N1 C6 C5 C4 -176.5(16) . . . . ?
N1 C6 C1 O3 -4(2) . . . . ?
N1 C6 C1 C2 179.6(15) . . . . ?
N2 C8 C7 N1 -29(3) . . . . ?
N2 C12 C13 N3 -42(3) . . . . ?
C14 N3 C13 C12 172.3(16) . . . . ?
C9 C8 C7 N1 156.0(18) . . . . ?
C32 C16 C15 C14 -173.2(17) . . . . ?
C17 C16 C15 C14 -1(3) . . . . ?
C17 C18 C19 O4 178.9(17) . . . . ?
C17 C18 C19 C14 -6(3) . . . . ?
C8 N2 C12 C11 0(3) . . . . ?
C8 N2 C12 C13 -174.3(19) . . . . ?
C8 C9 C10 C11 0(3) . . . . ?
C16 C17 C18 C28 -179.6(17) . . . . ?
C16 C17 C18 C19 5(3) . . . . ?
C6 N1 C7 C8 164.8(16) . . . . ?
C23 C20 C2 C3 8(2) . . . . ?
C23 C20 C2 C1 -179.0(16) . . . . ?
C11 C12 C13 N3 144.2(19) . . . . ?
C28 C18 C19 O4 3(3) . . . . ?
C28 C18 C19 C14 178.1(18) . . . . ?
C20 C2 C3 C4 175.7(17) . . . . ?
C20 C2 C1 O3 7(3) . . . . ?
C20 C2 C1 C6 -177.0(15) . . . . ?
N3 C14 C19 O4 7(3) . . . . ?
N3 C14 C19 C18 -168.1(18) . . . . ?
N3 C14 C15 C16 171.6(17) . . . . ?
C18 C17 C16 C32 171.5(18) . . . . ?
C18 C17 C16 C15 -1(3) . . . . ?
C5 C6 C1 O3 177.8(17) . . . . ?
C5 C6 C1 C2 2(2) . . . . ?
C5 C4 C3 C2 0(3) . . . . ?
C5 C4 C24 C26 126(2) . . . . ?
C5 C4 C24 C25 5(3) . . . . ?
C5 C4 C24 C27 -117(2) . . . . ?
C7 N1 C6 C5 29(3) . . . . ?
C7 N1 C6 C1 -148.4(16) . . . . ?
C3 C2 C1 O3 -179.3(16) . . . . ?
C3 C2 C1 C6 -3(2) . . . . ?
C3 C4 C5 C6 -2(3) . . . . ?
C3 C4 C24 C26 -54(3) . . . . ?
C3 C4 C24 C25 -176(2) . . . . ?
C3 C4 C24 C27 63(3) . . . . ?
C10 C9 C8 N2 1(3) . . . . ?
C10 C9 C8 C7 176.2(18) . . . . ?
C10 C11 C12 N2 1(3) . . . . ?
C10 C11 C12 C13 174.9(19) . . . . ?
C35 C32 C16 C17 -83(3) . . . . ?
C35 C32 C16 C15 90(2) . . . . ?
C19 C14 N3 U1 -23.5(19) . . . . ?
C19 C14 N3 C13 -144.5(17) . . . . ?
C19 C14 C15 C16 -1(3) . . . . ?
C31 C28 C18 C17 5(3) . . . . ?
C31 C28 C18 C19 -179.6(19) . . . . ?
C1 C6 C5 C4 1(3) . . . . ?
C1 C2 C3 C4 3(3) . . . . ?
C22 C20 C2 C3 -108(2) . . . . ?
C22 C20 C2 C1 66(2) . . . . ?
C33 C32 C16 C17 153.9(19) . . . . ?
C33 C32 C16 C15 -34(3) . . . . ?
C24 C4 C5 C6 177.8(18) . . . . ?
C24 C4 C3 C2 -179.6(18) . . . . ?
C29 C28 C18 C17 -122(2) . . . . ?
C29 C28 C18 C19 53(3) . . . . ?
C12 N2 C8 C9 -1(3) . . . . ?
C12 N2 C8 C7 -175.8(18) . . . . ?
C12 C11 C10 C9 -1(3) . . . . ?
C15 C14 N3 U1 163.3(14) . . . . ?
C15 C14 N3 C13 42(3) . . . . ?
C15 C14 C19 O4 -180.0(18) . . . . ?
C15 C14 C19 C18 5(3) . . . . ?
C30 C28 C18 C17 122(2) . . . . ?
C30 C28 C18 C19 -63(3) . . . . ?
C34 C32 C16 C17 35(2) . . . . ?
C34 C32 C16 C15 -152.5(19) . . . . ?
C21 C20 C2 C3 126(2) . . . . ?
C21 C20 C2 C1 -61(2) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.588 0.000 342.1 125.9 ?
2 0.042 0.208 0.625 7.2 0.2 ?
3 -0.042 0.792 0.375 7.2 0.0 ?
4 0.500 0.403 0.500 342.1 125.9 ?
5 0.458 0.708 0.875 7.2 0.0 ?
6 0.542 0.292 0.125 7.2 0.2 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_platon_squeeze_special_details  ?
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_original_sample_id 210317UO2-tBupdaop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.827
_oxdiff_exptl_absorpt_empirical_full_min 0.340

# start Validation Reply Form
_vrf_PLAT973_UO2tBupdaop         
;
PROBLEM: Check Calcd Positive Resid. Density on U1               5.48 eA-3
RESPONSE: We think that the insufficient or incorrect absorption 
correction is responsible of the residual densities. 
We applied the numerical absorption correction by using 
indexed crystal faces. Even though, the large peaks 
around U atoms remained. No better results have 
been obtained in use of the empirical absorption 
correction with strong absorber options. 
Despite many trials, we cannot correct this issue. 
Such an observation is frequently occurred 
in the compounds including a heavy atom. 
;
_vrf_RINTA01_UO2tBupdaop         
;
PROBLEM: The value of Rint is greater than 0.18 Rint given       0.199
RESPONSE: The investigated single crystal was a small-sized, 
brittle and poorly diffracting needle. Numerous datasets were collected
on single crystals from different batches, whereof the one of the highest
quality is  reported herein.
;
_vrf_PLAT020_UO2tBupdaop         
;
PROBLEM: The Value of Rint is Greater Than 0.12 Rint given       0.199
RESPONSE: The investigated single crystal was a small-sized, 
brittle and poorly diffracting needle. Numerous datasets were collected
on single crystals from different batches, whereof the one of the highest
quality is  reported herein.
;
_vrf_PLAT342_UO2tBupdaop         
;
PROBLEM: Low Bond Precision on C-C Bonds                         0.03441 Ang.
RESPONSE: The investigated single crystal was a small-sized, 
brittle and poorly diffracting needle. Numerous datasets were collected
on single crystals from different batches, whereof the one of the highest
quality is  reported herein. However, such low precision in bond lengths
had to appear due to weak diffractions and disordering atomic locations.
;
# end Validation Reply Form
_chemical_properties_physical    Air-sensitive
