# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_210519_uo2meosaldien_o
_database_code_depnum_ccdc_archive 'CCDC 2177295'
loop_
_audit_author_name
_audit_author_address
'Tomoyuki Takeyama'
;Tokyo Institute of Thechnology
Japan
;
_audit_update_record             
;
2022-06-06 deposited with the CCDC.	2022-08-22 downloaded from the CCDC.
;
_audit_creation_date             2021-05-20
_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         'C28 H38 N2 O7 U, C5 H5 N'
_chemical_formula_sum            'C33 H43 N3 O7 U'
_chemical_formula_weight         831.73
_chemical_melting_point          ?
_chemical_oxdiff_formula         C29H34N3O4U1
_chemical_oxdiff_usercomment     210519_UO2MeOsaldien_O
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                   10.19370(10)
_cell_length_b                   13.0886(2)
_cell_length_c                   13.2854(2)
_cell_angle_alpha                75.1030(10)
_cell_angle_beta                 80.7980(10)
_cell_angle_gamma                71.7900(10)
_cell_volume                     1621.06(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    18600
_cell_measurement_temperature    123
_cell_measurement_theta_max      30.5830
_cell_measurement_theta_min      2.0450
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.057
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80705
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             820
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 -13 -16 0.0923
13 -1 -4 0.0643
10 12 14 0.0573
-13 0 2 0.0528
2 -13 -14 0.0802
9 -8 8 0.0415
0 11 16 0.0826
6 18 7 0.0497
7 5 -14 0.0966
-8 -12 8 0.0696
-8 10 -3 0.0247

_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.084
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
-2.6756 -12.6366 -16.3818 0.0000 0.2152 0.9766
12.7901 -1.2116 -3.8159 -0.0000 -0.8797 0.4755
9.6310 12.0057 14.3440 -0.0000 -0.6936 -0.7203
-13.4184 -0.1963 2.0475 0.0000 0.9265 -0.3764
1.5694 -12.5925 -14.4271 0.0991 -0.0893 0.9911
8.6775 -7.7472 7.7471 0.7386 -0.6650 0.1104
0.0680 11.4561 16.3492 0.0412 -0.0371 -0.9985
5.5046 18.2497 7.1539 -0.6124 -0.3536 -0.7071
6.9771 4.7544 -13.7265 -0.7120 -0.4111 0.5692
-8.1654 -11.9902 8.0936 0.8557 0.4941 -0.1537
-8.2176 10.4115 -2.9877 -0.6900 0.6213 -0.3714

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32663
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.896
_diffrn_reflns_theta_min         2.043
_diffrn_ambient_temperature      123
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -72.00  76.00   0.50   15.26    --   20.00  54.00  30.00  296
  2  ω    -74.00  38.00   0.50   15.26    --   20.00  54.00 150.00  224
  3  ω     47.00  90.00   0.50   15.26    --   20.00  54.00 150.00   86
  4  ω    -70.00  10.00   0.50   15.26    --   20.00  54.00-150.00  160
  5  ω     38.00  63.00   0.50   15.26    --   20.00  54.00-150.00   50
  6  ω    -71.00  71.00   0.50   15.26    --   20.00  54.00  90.00  284
  7  ω    -74.00  32.00   0.50   15.26    --   20.00  54.00   0.00  212
  8  ω     69.00  94.00   0.50   15.26    --   20.00  54.00   0.00   50
  9  ω    -55.00 -28.00   0.50   15.26    --   20.00  54.00-106.60   54
 10  ω     63.00  88.00   0.50   15.26    --   20.00  54.00-106.60   50
 11  ω    -73.00 -39.00   0.50   15.26    --   20.00  54.00 -30.00   68
 12  ω     21.00  46.00   0.50   15.26    --   20.00  54.00 -30.00   50
 13  ω    -66.00 -40.00   0.50   15.26    --   20.00  54.00  60.00   52
 14  ω     17.00  42.00   0.50   15.26    --   20.00  54.00  60.00   50
 15  ω     55.00  81.00   0.50   15.26    --   20.00  54.00  60.00   52
 16  ω    -31.00  -6.00   0.50   15.26    --   20.00  54.00 -60.00   50
 17  ω      3.00  28.00   0.50   15.26    --   20.00  54.00 -60.00   50
 18  ω     85.00 110.00   0.50   15.26    --   20.00  54.00 -60.00   50
 19  ω    -69.00 -44.00   0.50   15.26    --   20.00  54.00-180.00   50
 20  ω    -66.00  54.00   0.50   15.26    --   20.00  54.00 -90.00  240
;
_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      0.0064964000
_diffrn_orient_matrix_UB_12      -0.0503124000
_diffrn_orient_matrix_UB_13      0.0377489000
_diffrn_orient_matrix_UB_21      -0.0697564000
_diffrn_orient_matrix_UB_22      0.0033689000
_diffrn_orient_matrix_UB_23      -0.0043409000
_diffrn_orient_matrix_UB_31      0.0223198000
_diffrn_orient_matrix_UB_32      -0.0296452000
_diffrn_orient_matrix_UB_33      -0.0403911000
_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                8730
_reflns_number_total             9686
_reflns_odcompleteness_completeness 98.92
_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         1.993
_refine_diff_density_min         -1.498
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         9686
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0287
_refine_ls_restrained_S_all      1.029
_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)+(0.0347P)²+1.7594P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0673
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C33) = Uanis(C32) = Uanis(C31) = Uanis(C30) = Uanis(C29) = Uanis(N3)
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C10(H10A,H10B)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C7(H7), C12(H12), C16(H16), C3(H3), C5(H5), C32(H32), C33(H33),
 C31(H31), C30(H30), C29(H29)
3.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C27(H27A,H27B,
 H27C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C23(H23A,
 H23B,H23C)
;
_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 0.28249(2) 0.44931(2) 0.35390(2) 0.01351(3) Uani 1 1 d . . . . .
O3 O 0.2017(2) 0.30683(16) 0.43907(16) 0.0152(4) Uani 1 1 d . . . . .
O4 O 0.3264(2) 0.40408(17) 0.19794(16) 0.0171(4) Uani 1 1 d . . . . .
O7 O 0.3133(2) 0.61187(18) 0.41468(18) 0.0210(5) Uani 1 1 d . . . . .
O1 O 0.1164(2) 0.53657(18) 0.31468(18) 0.0203(4) Uani 1 1 d . . . . .
O2 O 0.4484(2) 0.36877(18) 0.39838(17) 0.0191(4) Uani 1 1 d . . . . .
O6 O 0.2612(3) 0.6354(2) -0.21167(18) 0.0271(5) Uani 1 1 d . . . . .
N1 N 0.1976(3) 0.4676(2) 0.5393(2) 0.0173(5) Uani 1 1 d . . . . .
O5 O 0.3546(3) 0.00229(19) 0.80505(18) 0.0271(5) Uani 1 1 d . . . . .
N2 N 0.4112(3) 0.5737(2) 0.2278(2) 0.0184(5) Uani 1 1 d . . . . .
C18 C 0.3036(3) 0.4632(2) 0.1011(2) 0.0163(5) Uani 1 1 d . . . . .
C8 C 0.1422(3) 0.5807(2) 0.5546(3) 0.0210(6) Uani 1 1 d . . . . .
H8A H 0.117602 0.579799 0.629902 0.025 Uiso 1 1 calc R U . . .
H8B H 0.057370 0.618849 0.517405 0.025 Uiso 1 1 calc R U . . .
C15 C 0.2779(3) 0.5849(3) -0.1080(2) 0.0215(6) Uani 1 1 d . . . . .
C13 C 0.3446(3) 0.5612(3) 0.0642(2) 0.0189(6) Uani 1 1 d . . . . .
C2 C 0.2590(3) 0.1186(2) 0.5380(2) 0.0150(5) Uani 1 1 d . . . . .
C14 C 0.3338(3) 0.6207(3) -0.0407(2) 0.0209(6) Uani 1 1 d . . . . .
H14 H 0.364794 0.684898 -0.064454 0.025 Uiso 1 1 calc R U . . .
C17 C 0.2440(3) 0.4278(2) 0.0303(2) 0.0169(6) Uani 1 1 d . . . . .
C9 C 0.2515(3) 0.6411(3) 0.5121(3) 0.0206(6) Uani 1 1 d . . . . .
H9A H 0.208532 0.721808 0.501063 0.025 Uiso 1 1 calc R U . . .
H9B H 0.322835 0.619337 0.562199 0.025 Uiso 1 1 calc R U . . .
C7 C 0.2048(3) 0.3877(3) 0.6191(2) 0.0185(6) Uani 1 1 d . . . . .
H7 H 0.180085 0.405997 0.685601 0.022 Uiso 1 1 calc R U . . .
C1 C 0.2370(3) 0.2344(2) 0.5281(2) 0.0149(5) Uani 1 1 d . . . . .
C6 C 0.2474(3) 0.2706(2) 0.6174(2) 0.0169(6) Uani 1 1 d . . . . .
C11 C 0.4928(3) 0.6179(3) 0.2776(3) 0.0220(6) Uani 1 1 d . . . . .
H11A H 0.536244 0.668464 0.224012 0.026 Uiso 1 1 calc R U . . .
H11B H 0.567423 0.556955 0.313121 0.026 Uiso 1 1 calc R U . . .
C12 C 0.4123(3) 0.6006(3) 0.1282(3) 0.0208(6) Uani 1 1 d . . . . .
H12 H 0.462455 0.651458 0.092616 0.025 Uiso 1 1 calc R U . . .
C25 C 0.1988(3) 0.3215(2) 0.0638(2) 0.0183(6) Uani 1 1 d . . . . .
C20 C 0.0867(3) 0.1264(3) 0.4204(3) 0.0231(6) Uani 1 1 d . . . . .
H20A H 0.025178 0.103728 0.480881 0.035 Uiso 1 1 calc R U . . .
H20B H 0.072889 0.101204 0.360567 0.035 Uiso 1 1 calc R U . . .
H20C H 0.065590 0.206981 0.402895 0.035 Uiso 1 1 calc R U . . .
C16 C 0.2336(3) 0.4904(3) -0.0717(2) 0.0194(6) Uani 1 1 d . . . . .
H16 H 0.194294 0.467377 -0.119137 0.023 Uiso 1 1 calc R U . . .
C26 C 0.1000(3) 0.3216(3) 0.1641(2) 0.0210(6) Uani 1 1 d . . . . .
H26A H 0.149306 0.321147 0.221895 0.031 Uiso 1 1 calc R U . . .
H26B H 0.067009 0.255976 0.180865 0.031 Uiso 1 1 calc R U . . .
H26C H 0.020834 0.387948 0.153524 0.031 Uiso 1 1 calc R U . . .
C3 C 0.2972(3) 0.0485(2) 0.6322(2) 0.0192(6) Uani 1 1 d . . . . .
H3 H 0.312585 -0.028264 0.638859 0.023 Uiso 1 1 calc R U . . .
C28 C 0.1190(4) 0.3089(3) -0.0193(3) 0.0270(7) Uani 1 1 d . . . . .
H28A H 0.036596 0.372353 -0.031793 0.040 Uiso 1 1 calc R U . . .
H28B H 0.090711 0.241033 0.005511 0.040 Uiso 1 1 calc R U . . .
H28C H 0.178953 0.305376 -0.084548 0.040 Uiso 1 1 calc R U . . .
C27 C 0.3291(4) 0.2229(3) 0.0798(3) 0.0238(7) Uani 1 1 d . . . . .
H27A H 0.386946 0.221353 0.013451 0.036 Uiso 1 1 calc R U . . .
H27B H 0.302058 0.154420 0.103938 0.036 Uiso 1 1 calc R U . . .
H27C H 0.381475 0.229967 0.132128 0.036 Uiso 1 1 calc R U . . .
C10 C 0.3987(3) 0.6796(3) 0.3566(3) 0.0230(6) Uani 1 1 d . . . . .
H10A H 0.454392 0.692908 0.403891 0.028 Uiso 1 1 calc R U . . .
H10B H 0.340531 0.751681 0.320381 0.028 Uiso 1 1 calc R U . . .
C5 C 0.2859(3) 0.1948(3) 0.7123(2) 0.0186(6) Uani 1 1 d . . . . .
H5 H 0.292021 0.220542 0.771574 0.022 Uiso 1 1 calc R U . . .
C21 C 0.3389(4) 0.1028(3) 0.3516(3) 0.0241(7) Uani 1 1 d . . . . .
H21A H 0.319598 0.183089 0.328460 0.036 Uiso 1 1 calc R U . . .
H21B H 0.326583 0.072470 0.294732 0.036 Uiso 1 1 calc R U . . .
H21C H 0.434588 0.070724 0.370764 0.036 Uiso 1 1 calc R U . . .
C22 C 0.2667(4) -0.0510(3) 0.4751(3) 0.0283(7) Uani 1 1 d . . . . .
H22A H 0.363750 -0.086061 0.490117 0.042 Uiso 1 1 calc R U . . .
H22B H 0.248312 -0.075486 0.416368 0.042 Uiso 1 1 calc R U . . .
H22C H 0.205986 -0.071889 0.536983 0.042 Uiso 1 1 calc R U . . .
C19 C 0.2387(3) 0.0750(2) 0.4469(2) 0.0184(6) Uani 1 1 d . . . . .
C4 C 0.3143(3) 0.0844(3) 0.7182(2) 0.0193(6) Uani 1 1 d . . . . .
C24 C 0.2909(5) 0.7394(3) -0.2466(3) 0.0349(9) Uani 1 1 d . . . . .
H24A H 0.276796 0.767796 -0.321034 0.052 Uiso 1 1 calc R U . . .
H24B H 0.387358 0.729908 -0.236037 0.052 Uiso 1 1 calc R U . . .
H24C H 0.228889 0.791720 -0.206563 0.052 Uiso 1 1 calc R U . . .
C23 C 0.3915(5) 0.0344(3) 0.8881(3) 0.0378(9) Uani 1 1 d . . . . .
H23A H 0.463926 0.071728 0.861836 0.057 Uiso 1 1 calc R U . . .
H23B H 0.426317 -0.031088 0.942791 0.057 Uiso 1 1 calc R U . . .
H23C H 0.309936 0.084723 0.917123 0.057 Uiso 1 1 calc R U . . .
C32 C 0.0540(7) 0.9203(5) 0.2600(5) 0.0765(7) Uani 1 1 d . . . . .
H32 H 0.023775 0.938111 0.326455 0.092 Uiso 1 1 calc R U . . .
C33 C 0.0529(7) 0.8233(5) 0.2470(5) 0.0765(7) Uani 1 1 d . . . . .
H33 H 0.021167 0.773692 0.304175 0.092 Uiso 1 1 calc R U . . .
C31 C 0.0960(7) 0.9925(5) 0.1828(5) 0.0765(7) Uani 1 1 d . . . . .
H31 H 0.093429 1.061859 0.194196 0.092 Uiso 1 1 calc R U . . .
N3 N 0.0951(6) 0.7942(4) 0.1564(4) 0.0765(7) Uani 1 1 d . . . . .
C30 C 0.1414(7) 0.9699(5) 0.0904(5) 0.0765(7) Uani 1 1 d . . . . .
H30 H 0.175179 1.020598 0.035650 0.092 Uiso 1 1 calc R U . . .
C29 C 0.1383(7) 0.8669(5) 0.0750(5) 0.0765(7) Uani 1 1 d . . . . .
H29 H 0.166281 0.849216 0.008318 0.092 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 2.239(2) . ?
U1 O4 2.239(2) . ?
U1 O7 2.581(2) . ?
U1 O1 1.792(2) . ?
U1 O2 1.791(2) . ?
U1 N1 2.523(3) . ?
U1 N2 2.531(2) . ?
O3 C1 1.332(3) . ?
O4 C18 1.335(3) . ?
O7 C9 1.436(4) . ?
O7 C10 1.434(4) . ?
O6 C15 1.378(4) . ?
O6 C24 1.431(4) . ?
N1 C8 1.466(4) . ?
N1 C7 1.276(4) . ?
O5 C4 1.376(4) . ?
O5 C23 1.416(4) . ?
N2 C11 1.462(4) . ?
N2 C12 1.278(4) . ?
C18 C13 1.417(4) . ?
C18 C17 1.432(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.519(4) . ?
C15 C14 1.374(5) . ?
C15 C16 1.393(4) . ?
C13 C14 1.413(4) . ?
C13 C12 1.449(5) . ?
C2 C1 1.434(4) . ?
C2 C3 1.379(4) . ?
C2 C19 1.531(4) . ?
C14 H14 0.9500 . ?
C17 C25 1.537(4) . ?
C17 C16 1.393(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C7 H7 0.9500 . ?
C7 C6 1.461(4) . ?
C1 C6 1.416(4) . ?
C6 C5 1.414(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C10 1.518(5) . ?
C12 H12 0.9500 . ?
C25 C26 1.536(4) . ?
C25 C28 1.540(4) . ?
C25 C27 1.534(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C20 C19 1.542(4) . ?
C16 H16 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C3 H3 0.9500 . ?
C3 C4 1.396(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C5 H5 0.9500 . ?
C5 C4 1.366(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C21 C19 1.537(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C22 C19 1.538(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C32 H32 0.9500 . ?
C32 C33 1.327(8) . ?
C32 C31 1.321(8) . ?
C33 H33 0.9500 . ?
C33 N3 1.322(8) . ?
C31 H31 0.9500 . ?
C31 C30 1.315(8) . ?
N3 C29 1.361(8) . ?
C30 H30 0.9500 . ?
C30 C29 1.424(8) . ?
C29 H29 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
O3 U1 O7 131.93(7) . . ?
O3 U1 N1 70.29(8) . . ?
O3 U1 N2 164.48(8) . . ?
O4 U1 O3 96.22(7) . . ?
O4 U1 O7 131.85(7) . . ?
O4 U1 N1 165.90(8) . . ?
O4 U1 N2 70.27(8) . . ?
O1 U1 O3 94.11(9) . . ?
O1 U1 O4 88.39(9) . . ?
O1 U1 O7 87.89(9) . . ?
O1 U1 N1 88.54(10) . . ?
O1 U1 N2 93.13(9) . . ?
O2 U1 O3 87.63(9) . . ?
O2 U1 O4 95.00(9) . . ?
O2 U1 O7 88.27(9) . . ?
O2 U1 O1 176.00(10) . . ?
O2 U1 N1 88.67(9) . . ?
O2 U1 N2 86.04(9) . . ?
N1 U1 O7 61.75(7) . . ?
N1 U1 N2 123.64(8) . . ?
N2 U1 O7 62.04(8) . . ?
C1 O3 U1 129.87(18) . . ?
C18 O4 U1 132.65(18) . . ?
C9 O7 U1 123.62(17) . . ?
C10 O7 U1 123.43(18) . . ?
C10 O7 C9 112.9(2) . . ?
C15 O6 C24 115.9(3) . . ?
C8 N1 U1 115.60(19) . . ?
C7 N1 U1 125.5(2) . . ?
C7 N1 C8 118.8(3) . . ?
C4 O5 C23 116.4(3) . . ?
C11 N2 U1 114.41(19) . . ?
C12 N2 U1 127.5(2) . . ?
C12 N2 C11 118.1(3) . . ?
O4 C18 C13 120.0(3) . . ?
O4 C18 C17 121.7(3) . . ?
C13 C18 C17 118.2(3) . . ?
N1 C8 H8A 109.9 . . ?
N1 C8 H8B 109.9 . . ?
N1 C8 C9 108.8(2) . . ?
H8A C8 H8B 108.3 . . ?
C9 C8 H8A 109.9 . . ?
C9 C8 H8B 109.9 . . ?
O6 C15 C16 115.5(3) . . ?
C14 C15 O6 125.1(3) . . ?
C14 C15 C16 119.4(3) . . ?
C18 C13 C12 122.2(3) . . ?
C14 C13 C18 121.7(3) . . ?
C14 C13 C12 115.9(3) . . ?
C1 C2 C19 120.7(3) . . ?
C3 C2 C1 118.0(3) . . ?
C3 C2 C19 121.3(3) . . ?
C15 C14 C13 119.4(3) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C18 C17 C25 121.4(3) . . ?
C16 C17 C18 117.7(3) . . ?
C16 C17 C25 120.8(3) . . ?
O7 C9 C8 107.5(2) . . ?
O7 C9 H9A 110.2 . . ?
O7 C9 H9B 110.2 . . ?
C8 C9 H9A 110.2 . . ?
C8 C9 H9B 110.2 . . ?
H9A C9 H9B 108.5 . . ?
N1 C7 H7 117.0 . . ?
N1 C7 C6 126.0(3) . . ?
C6 C7 H7 117.0 . . ?
O3 C1 C2 121.4(3) . . ?
O3 C1 C6 120.5(3) . . ?
C6 C1 C2 118.1(3) . . ?
C1 C6 C7 121.5(3) . . ?
C5 C6 C7 116.9(3) . . ?
C5 C6 C1 121.3(3) . . ?
N2 C11 H11A 109.8 . . ?
N2 C11 H11B 109.8 . . ?
N2 C11 C10 109.2(2) . . ?
H11A C11 H11B 108.3 . . ?
C10 C11 H11A 109.8 . . ?
C10 C11 H11B 109.8 . . ?
N2 C12 C13 126.5(3) . . ?
N2 C12 H12 116.7 . . ?
C13 C12 H12 116.7 . . ?
C17 C25 C28 112.0(3) . . ?
C26 C25 C17 111.0(2) . . ?
C26 C25 C28 106.1(3) . . ?
C27 C25 C17 108.3(2) . . ?
C27 C25 C26 111.0(3) . . ?
C27 C25 C28 108.4(3) . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
C15 C16 C17 123.5(3) . . ?
C15 C16 H16 118.2 . . ?
C17 C16 H16 118.2 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C2 C3 H3 118.3 . . ?
C2 C3 C4 123.5(3) . . ?
C4 C3 H3 118.3 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O7 C10 C11 106.9(2) . . ?
O7 C10 H10A 110.3 . . ?
O7 C10 H10B 110.3 . . ?
C11 C10 H10A 110.3 . . ?
C11 C10 H10B 110.3 . . ?
H10A C10 H10B 108.6 . . ?
C6 C5 H5 120.2 . . ?
C4 C5 C6 119.6(3) . . ?
C4 C5 H5 120.2 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
C2 C19 C20 108.5(2) . . ?
C2 C19 C21 110.5(3) . . ?
C2 C19 C22 111.8(3) . . ?
C21 C19 C20 111.0(3) . . ?
C21 C19 C22 107.3(3) . . ?
C22 C19 C20 107.7(3) . . ?
O5 C4 C3 115.2(3) . . ?
C5 C4 O5 125.4(3) . . ?
C5 C4 C3 119.3(3) . . ?
O6 C24 H24A 109.5 . . ?
O6 C24 H24B 109.5 . . ?
O6 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O5 C23 H23A 109.5 . . ?
O5 C23 H23B 109.5 . . ?
O5 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C33 C32 H32 119.2 . . ?
C31 C32 H32 119.2 . . ?
C31 C32 C33 121.6(7) . . ?
C32 C33 H33 119.2 . . ?
N3 C33 C32 121.5(6) . . ?
N3 C33 H33 119.2 . . ?
C32 C31 H31 119.5 . . ?
C30 C31 C32 121.0(7) . . ?
C30 C31 H31 119.5 . . ?
C33 N3 C29 118.4(6) . . ?
C31 C30 H30 121.1 . . ?
C31 C30 C29 117.9(6) . . ?
C29 C30 H30 121.1 . . ?
N3 C29 C30 119.5(6) . . ?
N3 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?

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 C2 -135.3(2) . . . . ?
U1 O3 C1 C6 47.7(4) . . . . ?
U1 O4 C18 C13 49.6(4) . . . . ?
U1 O4 C18 C17 -133.4(2) . . . . ?
U1 O7 C9 C8 -13.9(3) . . . . ?
U1 O7 C10 C11 -16.3(3) . . . . ?
U1 N1 C8 C9 -55.7(3) . . . . ?
U1 N1 C7 C6 -8.0(4) . . . . ?
U1 N2 C11 C10 -56.7(3) . . . . ?
U1 N2 C12 C13 -3.2(5) . . . . ?
O3 C1 C6 C7 7.2(4) . . . . ?
O3 C1 C6 C5 -179.5(3) . . . . ?
O4 C18 C13 C14 174.2(3) . . . . ?
O4 C18 C13 C12 0.3(4) . . . . ?
O4 C18 C17 C25 2.1(4) . . . . ?
O4 C18 C17 C16 -175.2(3) . . . . ?
O6 C15 C14 C13 179.9(3) . . . . ?
O6 C15 C16 C17 179.1(3) . . . . ?
N1 C8 C9 O7 42.3(3) . . . . ?
N1 C7 C6 C1 -23.7(5) . . . . ?
N1 C7 C6 C5 162.7(3) . . . . ?
N2 C11 C10 O7 45.0(3) . . . . ?
C18 C13 C14 C15 2.1(5) . . . . ?
C18 C13 C12 N2 -19.7(5) . . . . ?
C18 C17 C25 C26 53.4(4) . . . . ?
C18 C17 C25 C28 171.8(3) . . . . ?
C18 C17 C25 C27 -68.6(3) . . . . ?
C18 C17 C16 C15 -0.1(4) . . . . ?
C8 N1 C7 C6 175.2(3) . . . . ?
C13 C18 C17 C25 179.1(3) . . . . ?
C13 C18 C17 C16 1.8(4) . . . . ?
C2 C1 C6 C7 -169.9(3) . . . . ?
C2 C1 C6 C5 3.4(4) . . . . ?
C2 C3 C4 O5 -179.1(3) . . . . ?
C2 C3 C4 C5 3.3(5) . . . . ?
C14 C15 C16 C17 -0.7(5) . . . . ?
C14 C13 C12 N2 166.1(3) . . . . ?
C17 C18 C13 C14 -2.9(4) . . . . ?
C17 C18 C13 C12 -176.8(3) . . . . ?
C9 O7 C10 C11 161.3(3) . . . . ?
C7 N1 C8 C9 121.5(3) . . . . ?
C7 C6 C5 C4 173.9(3) . . . . ?
C1 C2 C3 C4 0.5(4) . . . . ?
C1 C2 C19 C20 -60.9(3) . . . . ?
C1 C2 C19 C21 61.0(3) . . . . ?
C1 C2 C19 C22 -179.5(3) . . . . ?
C1 C6 C5 C4 0.3(4) . . . . ?
C6 C5 C4 O5 179.0(3) . . . . ?
C6 C5 C4 C3 -3.6(4) . . . . ?
C11 N2 C12 C13 176.5(3) . . . . ?
C12 N2 C11 C10 123.5(3) . . . . ?
C12 C13 C14 C15 176.4(3) . . . . ?
C25 C17 C16 C15 -177.4(3) . . . . ?
C16 C15 C14 C13 -0.3(5) . . . . ?
C16 C17 C25 C26 -129.3(3) . . . . ?
C16 C17 C25 C28 -11.0(4) . . . . ?
C16 C17 C25 C27 108.6(3) . . . . ?
C3 C2 C1 O3 179.2(3) . . . . ?
C3 C2 C1 C6 -3.8(4) . . . . ?
C3 C2 C19 C20 118.3(3) . . . . ?
C3 C2 C19 C21 -119.8(3) . . . . ?
C3 C2 C19 C22 -0.3(4) . . . . ?
C10 O7 C9 C8 168.5(3) . . . . ?
C19 C2 C1 O3 -1.6(4) . . . . ?
C19 C2 C1 C6 175.4(3) . . . . ?
C19 C2 C3 C4 -178.7(3) . . . . ?
C24 O6 C15 C14 -7.3(5) . . . . ?
C24 O6 C15 C16 172.9(3) . . . . ?
C23 O5 C4 C3 171.5(3) . . . . ?
C23 O5 C4 C5 -11.1(5) . . . . ?
C32 C33 N3 C29 -1.0(11) . . . . ?
C32 C31 C30 C29 2.6(11) . . . . ?
C33 C32 C31 C30 -1.5(12) . . . . ?
C33 N3 C29 C30 2.1(10) . . . . ?
C31 C32 C33 N3 0.6(12) . . . . ?
C31 C30 C29 N3 -2.9(11) . . . . ?

_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 1.260
_oxdiff_exptl_absorpt_empirical_full_min 0.847
####################################################################### 
# 
# 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_210120_uo2meosalidien_s
_database_code_depnum_ccdc_archive 'CCDC 2177296'
loop_
_audit_author_name
_audit_author_address
'Tomoyuki Takeyama'
;Tokyo Institute of Thechnology
Japan
;
_audit_update_record             
;
2022-06-06 deposited with the CCDC.	2022-08-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_210120_uo2meosalidien_s 
;
PROBLEM: Check Calcd Resid. Dens.  0.92Ang From U1              4.17 eA-3
RESPONSE: We think that the insufficient or incorrect absorption correction is responsible of the residual densities. We applied the empirical absorption correction with strong absorber options. Even though, the large peaks around U atoms remained. Despite many trials, we cannot correct this issue. Such an observation is frequently occurred in the compounds including a heavy atom.
;
_vrf_PLAT971_210120_uo2meosalidien_s_2 
;
PROBLEM: Check Calcd Resid. Dens.  1.00Ang From O1              3.88 eA-3
RESPONSE: We think that the insufficient or incorrect absorption correction is responsible of the residual densities. We applied the empirical absorption correction with strong absorber options. Even though, the large peaks around U atoms remained. Despite many trials, we cannot correct this issue. Such an observation is frequently occurred in the compounds including a heavy atom.
;
_vrf_PLAT972_210120_uo2meosalidien_s 
;
PROBLEM: Check Calcd Resid. Dens.  0.94Ang From U1             -4.16 eA-3
RESPONSE: We think that the insufficient or incorrect absorption correction is responsible of the residual densities. We applied the empirical absorption correction with strong absorber options. Even though, the large peaks around U atoms remained. Despite many trials, we cannot correct this issue. Such an observation is frequently occurred in the compounds including a heavy atom.
;
_vrf_PLAT972_210120_uo2meosalidien_s_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.94Ang From U1             -4.02 eA-3
RESPONSE: We think that the insufficient or incorrect absorption correction is responsible of the residual densities. We applied the empirical absorption correction with strong absorber options. Even though, the large peaks around U atoms remained. Despite many trials, we cannot correct this issue. Such an observation is frequently occurred in the compounds including a heavy atom.
;
_vrf_PLAT972_210120_uo2meosalidien_s_3 
;
PROBLEM: Check Calcd Resid. Dens.  0.89Ang From U1             -3.77 eA-3
RESPONSE: We think that the insufficient or incorrect absorption correction is responsible of the residual densities. We applied the empirical absorption correction with strong absorber options. Even though, the large peaks around U atoms remained. Despite many trials, we cannot correct this issue. Such an observation is frequently occurred in the compounds including a heavy atom.
;
_vrf_PLAT972_210120_uo2meosalidien_s_4 
;
PROBLEM: Check Calcd Resid. Dens.  0.89Ang From U1             -3.58 eA-3
RESPONSE: We think that the insufficient or incorrect absorption correction is responsible of the residual densities. We applied the empirical absorption correction with strong absorber options. Even though, the large peaks around U atoms remained. Despite many trials, we cannot correct this issue. Such an observation is frequently occurred in the compounds including a heavy atom.
;
_vrf_PLAT973_210120_uo2meosalidien_s 
;
PROBLEM: Check Calcd Positive Resid. Density on        U1       2.18 eA-3
RESPONSE: We think that the insufficient or incorrect absorption correction is responsible of the residual densities. We applied the empirical absorption correction with strong absorber options. Even though, the large peaks around U atoms remained. Despite many trials, we cannot correct this issue. Such an observation is frequently occurred in the compounds including a heavy atom.
;
_vrf_PLAT971_210120_uo2meosalidien_s_3 
;
PROBLEM: Check Calcd Resid. Dens.  0.95Ang From U1              3.14 eA-3
RESPONSE: We think that the insufficient or incorrect absorption correction is responsible of the residual densities. We applied the empirical absorption correction with strong absorber options. Even though, the large peaks around U atoms remained. Despite many trials, we cannot correct this issue. Such an observation is frequently occurred in the compounds including a heavy atom.
;
_vrf_PLAT971_210120_uo2meosalidien_s_4 
;
PROBLEM: Check Calcd Resid. Dens.  1.01Ang From U1              2.89 eA-3
RESPONSE: We think that the insufficient or incorrect absorption correction is responsible of the residual densities. We applied the empirical absorption correction with strong absorber options. Even though, the large peaks around U atoms remained. Despite many trials, we cannot correct this issue. Such an observation is frequently occurred in the compounds including a heavy atom.
;
_vrf_PLAT971_210120_uo2meosalidien_s_5 
;
PROBLEM: Check Calcd Resid. Dens.  1.15Ang From U1              2.49 eA-3
RESPONSE: We think that the insufficient or incorrect absorption correction is responsible of the residual densities. We applied the empirical absorption correction with strong absorber options. Even though, the large peaks around U atoms remained. Despite many trials, we cannot correct this issue. Such an observation is frequently occurred in the compounds including a heavy atom.
;
_vrf_PLAT972_210120_uo2meosalidien_s_5 
;
PROBLEM: Check Calcd Resid. Dens.  1.30Ang From U1             -1.54 eA-3
RESPONSE: We think that the insufficient or incorrect absorption correction is responsible of the residual densities. We applied the empirical absorption correction with strong absorber options. Even though, the large peaks around U atoms remained. Despite many trials, we cannot correct this issue. Such an observation is frequently occurred in the compounds including a heavy atom.
;
# Added during the CSD deposition process: Monday 06 June 2022 03:18 PM
# end Validation Reply Form

_audit_creation_date             2022-05-22
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H38 N2 O6 S U, C H2 Cl2'
_chemical_formula_sum            'C29 H40 Cl2 N2 O6 S U'
_chemical_formula_weight         853.62
_chemical_melting_point          ?
_chemical_oxdiff_formula         C29H34N3O6S1U1
_chemical_oxdiff_usercomment     210120_UO2MeOsalidien_S
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'
S S 0.1246 0.1234 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   16.3889(14)
_cell_length_b                   18.8968(9)
_cell_length_c                   10.3557(6)
_cell_angle_alpha                90
_cell_angle_beta                 98.602(7)
_cell_angle_gamma                90
_cell_volume                     3171.1(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6606
_cell_measurement_temperature    113
_cell_measurement_theta_max      28.8330
_cell_measurement_theta_min      1.7350
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.396
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21185
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 3 -14 0.2612
-14 -21 -1 0.0382
-3 -1 15 0.3652
22 1 2 0.0354
3 26 0 0.1116
-23 -2 0 0.0046

_exptl_crystal_size_max          0.661
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.053
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
4.8912 3.3785 -14.4642 0.0000 0.1053 0.9944
-13.9521 -20.7523 -1.0928 -0.0000 -0.9992 0.0400
-3.3074 -1.0191 14.6027 0.0000 0.0084 -1.0000
22.1590 1.4621 1.9108 -0.7369 0.6635 -0.1293
3.3613 26.3294 0.0556 0.4996 0.8653 0.0411
-22.7936 -1.6301 -0.0228 0.7431 -0.6691 -0.0000

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1055
_diffrn_reflns_av_unetI/netI     0.1154
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            35851
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.890
_diffrn_reflns_theta_min         2.262
_diffrn_ambient_temperature      113
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.993
_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    -73.00 -20.50   0.50   90.00    --   20.00  54.00 -30.00  105
  2  ω      4.00 106.50   0.50   90.00    --   20.00  54.00 -30.00  205
  3  ω    -69.00  -0.50   0.50   90.00    --   20.00  54.00-150.00  137
  4  ω     17.00  70.50   0.50   90.00    --   20.00  54.00-150.00  107
  5  ω    -36.00   3.50   0.50   90.00    --   20.00  54.00-180.00   79
  6  ω     34.00  67.50   0.50   90.00    --   20.00  54.00-180.00   67
  7  ω    -71.00 -40.50   0.50   90.00    --   20.00  54.00  30.00   61
  8  ω    -74.00  48.50   0.50   90.00    --   20.00  54.00 -90.00  245
  9  ω    -67.00  77.50   0.50   90.00    --   20.00  54.00  -8.79  289
;
_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      -0.0342679000
_diffrn_orient_matrix_UB_12      0.0233618000
_diffrn_orient_matrix_UB_13      -0.0061311000
_diffrn_orient_matrix_UB_21      0.0272471000
_diffrn_orient_matrix_UB_22      0.0293672000
_diffrn_orient_matrix_UB_23      0.0087938000
_diffrn_orient_matrix_UB_31      -0.0000539000
_diffrn_orient_matrix_UB_32      0.0017107000
_diffrn_orient_matrix_UB_33      -0.0683707000
_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                5994
_reflns_number_total             9534
_reflns_odcompleteness_completeness 98.95
_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         4.306
_refine_diff_density_min         -4.642
_refine_diff_density_rms         0.264
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         9534
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_gt           0.0662
_refine_ls_restrained_S_all      0.976
_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)+(0.0940P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1746
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C12) = Uanis(C13) = Uanis(C14) = Uanis(C15) = Uanis(C16) = Uanis(C17) =
Uanis(C18)
Uanis(Cl1A) = Uanis(Cl1B) = Uanis(Cl2A) = Uanis(Cl2B)
Uanis(O1) = Uanis(O2)
3. Others
 Fixed Sof: Cl2B(0.8) Cl1A(0.8) H29A(0.8) H29B(0.8) H29C(0.2) H29D(0.2)
 Cl1B(0.2) Cl2A(0.2)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C10(H10A,H10B), C8(H8A,H8B), C9(H9A,H9B), C29(H29A,H29B),
 C29(H29C,H29D)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C16(H16), C7(H7), C3(H3), C12(H12), C14(H14)
4.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C26(H26A,H26B,H26C), C20(H20A,H20B,H20C), C25(H25A,H25B,
 H25C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C)
;
_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 0.71479(2) 0.33713(2) 0.42130(3) 0.02304(10) Uani 1 1 d . . . . .
S1 S 0.61346(14) 0.20706(10) 0.4348(2) 0.0301(4) Uani 1 1 d . . . . .
Cl2B Cl 0.6322(4) 0.7069(3) -0.0150(5) 0.1110(16) Uani 0.8 1 d . . P A 1
O1 O 0.7378(4) 0.3247(3) 0.5929(5) 0.0274(9) Uani 1 1 d . . . . .
Cl1A Cl 0.7325(4) 0.6911(3) 0.2406(5) 0.1110(16) Uani 0.8 1 d . . P A 2
O2 O 0.6872(4) 0.3412(3) 0.2488(5) 0.0274(9) Uani 1 1 d . . . . .
O4 O 0.8406(3) 0.3708(3) 0.3889(5) 0.0268(12) Uani 1 1 d . . . . .
O5 O 0.5032(4) 0.5379(3) 0.8552(6) 0.0392(15) Uani 1 1 d . . . . .
N2 N 0.7977(4) 0.2257(3) 0.3951(6) 0.0246(14) Uani 1 1 d . . . . .
O3 O 0.6808(3) 0.4476(3) 0.4711(5) 0.0274(12) Uani 1 1 d . . . . .
O6 O 1.0361(4) 0.2965(3) 0.0214(6) 0.0373(14) Uani 1 1 d . . . . .
C21 C 0.7555(6) 0.5906(4) 0.5255(9) 0.040(2) Uani 1 1 d . . . . .
H21A H 0.740981 0.556663 0.454282 0.061 Uiso 1 1 calc R U . . .
H21B H 0.810397 0.610176 0.521187 0.061 Uiso 1 1 calc R U . . .
H21C H 0.714855 0.629028 0.517182 0.061 Uiso 1 1 calc R U . . .
C17 C 0.9165(5) 0.4048(4) 0.2164(8) 0.0283(7) Uani 1 1 d . . . . .
C5 C 0.5131(5) 0.4579(4) 0.6729(8) 0.0267(16) Uani 1 1 d . . . . .
H5 H 0.460009 0.438395 0.675942 0.032 Uiso 1 1 calc R U . . .
N1 N 0.5589(4) 0.3462(3) 0.4074(7) 0.0269(14) Uani 1 1 d . . . . .
C4 C 0.5451(5) 0.5088(4) 0.7608(8) 0.0307(18) Uani 1 1 d . . . . .
C16 C 0.9672(5) 0.3826(4) 0.1292(8) 0.0283(7) Uani 1 1 d . . . . .
H16 H 0.991069 0.417037 0.079550 0.034 Uiso 1 1 calc R U . . .
C15 C 0.9851(5) 0.3084(4) 0.1109(8) 0.0283(7) Uani 1 1 d . . . . .
C26 C 0.7999(5) 0.4935(4) 0.1934(8) 0.0345(19) Uani 1 1 d . . . . .
H26A H 0.781087 0.477463 0.103861 0.052 Uiso 1 1 calc R U . . .
H26B H 0.786260 0.543633 0.201194 0.052 Uiso 1 1 calc R U . . .
H26C H 0.772560 0.465652 0.254286 0.052 Uiso 1 1 calc R U . . .
C6 C 0.5613(5) 0.4351(4) 0.5767(7) 0.0254(16) Uani 1 1 d . . . . .
C1 C 0.6387(5) 0.4660(4) 0.5677(7) 0.0233(15) Uani 1 1 d . . . . .
C11 C 0.7701(5) 0.1588(4) 0.4466(8) 0.0279(17) Uani 1 1 d . . . . .
H11A H 0.771817 0.162684 0.542316 0.033 Uiso 1 1 calc R U . . .
H11B H 0.807797 0.120135 0.429328 0.033 Uiso 1 1 calc R U . . .
C2 C 0.6704(5) 0.5194(4) 0.6600(8) 0.0293(17) Uani 1 1 d . . . . .
C7 C 0.5228(5) 0.3848(4) 0.4832(8) 0.0295(18) Uani 1 1 d . . . . .
H7 H 0.464668 0.379632 0.476791 0.035 Uiso 1 1 calc R U . . .
C3 C 0.6221(5) 0.5376(4) 0.7540(8) 0.0315(19) Uani 1 1 d . . . . .
H3 H 0.642976 0.571882 0.817512 0.038 Uiso 1 1 calc R U . . .
C20 C 0.8253(6) 0.4977(5) 0.6766(9) 0.038(2) Uani 1 1 d . . . . .
H20A H 0.812913 0.460172 0.611345 0.058 Uiso 1 1 calc R U . . .
H20B H 0.830012 0.477321 0.764343 0.058 Uiso 1 1 calc R U . . .
H20C H 0.877487 0.520609 0.665475 0.058 Uiso 1 1 calc R U . . .
C24 C 0.8946(5) 0.4835(4) 0.2262(8) 0.0274(16) Uani 1 1 d . . . . .
C18 C 0.8825(5) 0.3526(4) 0.2930(8) 0.0283(7) Uani 1 1 d . . . . .
C19 C 0.7559(5) 0.5526(4) 0.6586(8) 0.0308(18) Uani 1 1 d . . . . .
C25 C 0.9248(6) 0.5117(5) 0.3607(8) 0.0358(19) Uani 1 1 d . . . . .
H25A H 0.900280 0.484161 0.425384 0.054 Uiso 1 1 calc R U . . .
H25B H 0.908718 0.561445 0.365587 0.054 Uiso 1 1 calc R U . . .
H25C H 0.985050 0.507774 0.378895 0.054 Uiso 1 1 calc R U . . .
C10 C 0.6825(5) 0.1414(4) 0.3827(8) 0.0295(18) Uani 1 1 d . . . . .
H10A H 0.666861 0.093539 0.409134 0.035 Uiso 1 1 calc R U . . .
H10B H 0.679028 0.142274 0.286401 0.035 Uiso 1 1 calc R U . . .
C8 C 0.5050(6) 0.3028(5) 0.3121(9) 0.040(2) Uani 1 1 d . . . . .
H8A H 0.491744 0.329328 0.229190 0.047 Uiso 1 1 calc R U . . .
H8B H 0.452701 0.293042 0.345733 0.047 Uiso 1 1 calc R U . . .
C23 C 0.4216(6) 0.5139(6) 0.8577(9) 0.048(3) Uani 1 1 d . . . . .
H23A H 0.388516 0.521516 0.771880 0.072 Uiso 1 1 calc R U . . .
H23B H 0.397351 0.540261 0.924040 0.072 Uiso 1 1 calc R U . . .
H23C H 0.422555 0.463336 0.878798 0.072 Uiso 1 1 calc R U . . .
C12 C 0.8580(5) 0.2227(4) 0.3312(8) 0.0283(7) Uani 1 1 d . . . . .
H12 H 0.881224 0.177035 0.324149 0.034 Uiso 1 1 calc R U . . .
C9 C 0.5474(6) 0.2319(4) 0.2862(8) 0.0329(19) Uani 1 1 d . . . . .
H9A H 0.580356 0.237616 0.214214 0.039 Uiso 1 1 calc R U . . .
H9B H 0.505325 0.194821 0.261160 0.039 Uiso 1 1 calc R U . . .
C14 C 0.9481(5) 0.2602(4) 0.1792(8) 0.0283(7) Uani 1 1 d . . . . .
H14 H 0.957913 0.211319 0.166643 0.034 Uiso 1 1 calc R U . . .
C22 C 0.7768(7) 0.6078(5) 0.7676(10) 0.050(3) Uani 1 1 d . . . . .
H22A H 0.832666 0.625912 0.766292 0.076 Uiso 1 1 calc R U . . .
H22B H 0.773785 0.585684 0.852374 0.076 Uiso 1 1 calc R U . . .
H22C H 0.737201 0.646910 0.753590 0.076 Uiso 1 1 calc R U . . .
C13 C 0.8964(5) 0.2801(4) 0.2670(8) 0.0283(7) Uani 1 1 d . . . . .
C27 C 0.9349(6) 0.5282(4) 0.1279(8) 0.0342(19) Uani 1 1 d . . . . .
H27A H 0.994598 0.530555 0.156166 0.051 Uiso 1 1 calc R U . . .
H27B H 0.911781 0.576164 0.123867 0.051 Uiso 1 1 calc R U . . .
H27C H 0.923743 0.506363 0.041212 0.051 Uiso 1 1 calc R U . . .
C28 C 1.0625(6) 0.2256(5) 0.0103(9) 0.043(2) Uani 1 1 d . . . . .
H28A H 1.095243 0.222137 -0.061288 0.065 Uiso 1 1 calc R U . . .
H28B H 1.014271 0.194574 -0.007668 0.065 Uiso 1 1 calc R U . . .
H28C H 1.096347 0.211168 0.092198 0.065 Uiso 1 1 calc R U . . .
C29 C 0.7287(10) 0.6964(10) 0.0758(14) 0.108(6) Uani 1 1 d . . . . .
H29A H 0.761372 0.740562 0.089508 0.130 Uiso 0.8 1 calc R U P A 1
H29B H 0.761588 0.657331 0.045916 0.130 Uiso 0.8 1 calc R U P A 1
H29C H 0.741332 0.744856 0.048321 0.130 Uiso 0.2 1 calc R U P A 2
H29D H 0.767517 0.662610 0.044252 0.130 Uiso 0.2 1 calc R U P A 2
Cl1B Cl 0.6678(19) 0.6704(11) 0.2254(19) 0.1110(16) Uani 0.2 1 d . . P A 1
Cl2A Cl 0.632(2) 0.6749(12) 0.023(2) 0.1110(16) Uani 0.2 1 d . . P A 2


_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 S1 2.981(2) . ?
U1 O1 1.776(5) . ?
U1 O2 1.778(5) . ?
U1 O4 2.231(5) . ?
U1 N2 2.543(6) . ?
U1 O3 2.241(5) . ?
U1 N1 2.543(7) . ?
S1 C10 1.815(9) . ?
S1 C9 1.806(8) . ?
Cl2B C29 1.728(16) . ?
Cl1A C29 1.702(15) . ?
O4 C18 1.333(10) . ?
O5 C4 1.390(10) . ?
O5 C23 1.416(12) . ?
N2 C11 1.469(9) . ?
N2 C12 1.270(10) . ?
O3 C1 1.343(9) . ?
O6 C15 1.356(10) . ?
O6 C28 1.417(10) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C21 C19 1.553(12) . ?
C17 C16 1.381(11) . ?
C17 C24 1.537(11) . ?
C17 C18 1.429(11) . ?
C5 H5 0.9500 . ?
C5 C4 1.373(11) . ?
C5 C6 1.427(11) . ?
N1 C7 1.279(10) . ?
N1 C8 1.470(10) . ?
C4 C3 1.385(12) . ?
C16 H16 0.9500 . ?
C16 C15 1.451(11) . ?
C15 C14 1.351(11) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C26 C24 1.550(11) . ?
C6 C1 1.412(11) . ?
C6 C7 1.435(11) . ?
C1 C2 1.434(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C10 1.524(12) . ?
C2 C3 1.387(12) . ?
C2 C19 1.536(12) . ?
C7 H7 0.9500 . ?
C3 H3 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C20 C19 1.530(11) . ?
C24 C25 1.505(11) . ?
C24 C27 1.545(11) . ?
C18 C13 1.422(10) . ?
C19 C22 1.537(11) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.551(12) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C12 H12 0.9500 . ?
C12 C13 1.464(11) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C14 H14 0.9500 . ?
C14 C13 1.384(11) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 H29C 0.9900 . ?
C29 H29D 0.9900 . ?
C29 Cl1B 2.02(3) . ?
C29 Cl2A 1.65(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 S1 83.17(18) . . ?
O1 U1 O2 174.4(2) . . ?
O1 U1 O4 97.2(2) . . ?
O1 U1 N2 87.7(2) . . ?
O1 U1 O3 85.1(2) . . ?
O1 U1 N1 97.3(2) . . ?
O2 U1 S1 91.32(18) . . ?
O2 U1 O4 86.5(2) . . ?
O2 U1 N2 89.4(2) . . ?
O2 U1 O3 99.0(2) . . ?
O2 U1 N1 80.7(2) . . ?
O4 U1 S1 140.88(15) . . ?
O4 U1 N2 72.5(2) . . ?
O4 U1 O3 92.1(2) . . ?
O4 U1 N1 156.3(2) . . ?
N2 U1 S1 68.42(16) . . ?
N2 U1 N1 126.7(2) . . ?
O3 U1 S1 126.70(15) . . ?
O3 U1 N2 162.1(2) . . ?
O3 U1 N1 70.6(2) . . ?
N1 U1 S1 59.73(14) . . ?
C10 S1 U1 100.0(3) . . ?
C9 S1 U1 90.8(3) . . ?
C9 S1 C10 104.2(4) . . ?
C18 O4 U1 129.0(5) . . ?
C4 O5 C23 116.9(7) . . ?
C11 N2 U1 118.4(5) . . ?
C12 N2 U1 124.2(5) . . ?
C12 N2 C11 117.1(7) . . ?
C1 O3 U1 125.9(5) . . ?
C15 O6 C28 116.1(7) . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
C16 C17 C24 120.4(7) . . ?
C16 C17 C18 118.4(7) . . ?
C18 C17 C24 121.1(7) . . ?
C4 C5 H5 120.7 . . ?
C4 C5 C6 118.5(8) . . ?
C6 C5 H5 120.7 . . ?
C7 N1 U1 123.8(5) . . ?
C7 N1 C8 116.3(7) . . ?
C8 N1 U1 119.8(5) . . ?
C5 C4 O5 124.3(8) . . ?
C5 C4 C3 120.2(8) . . ?
C3 C4 O5 115.4(7) . . ?
C17 C16 H16 118.9 . . ?
C17 C16 C15 122.2(7) . . ?
C15 C16 H16 118.9 . . ?
O6 C15 C16 114.1(7) . . ?
C14 C15 O6 128.0(8) . . ?
C14 C15 C16 117.8(8) . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
C5 C6 C7 116.0(7) . . ?
C1 C6 C5 121.2(7) . . ?
C1 C6 C7 122.5(7) . . ?
O3 C1 C6 120.6(7) . . ?
O3 C1 C2 120.2(7) . . ?
C6 C1 C2 119.1(7) . . ?
N2 C11 H11A 109.6 . . ?
N2 C11 H11B 109.6 . . ?
N2 C11 C10 110.4(6) . . ?
H11A C11 H11B 108.1 . . ?
C10 C11 H11A 109.6 . . ?
C10 C11 H11B 109.6 . . ?
C1 C2 C19 121.4(7) . . ?
C3 C2 C1 117.0(8) . . ?
C3 C2 C19 121.5(7) . . ?
N1 C7 C6 126.5(8) . . ?
N1 C7 H7 116.7 . . ?
C6 C7 H7 116.7 . . ?
C4 C3 C2 123.9(8) . . ?
C4 C3 H3 118.0 . . ?
C2 C3 H3 118.0 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
C17 C24 C26 109.8(6) . . ?
C17 C24 C27 111.1(7) . . ?
C25 C24 C17 110.8(7) . . ?
C25 C24 C26 109.9(7) . . ?
C25 C24 C27 107.6(7) . . ?
C27 C24 C26 107.5(6) . . ?
O4 C18 C17 121.5(7) . . ?
O4 C18 C13 120.3(7) . . ?
C13 C18 C17 118.2(8) . . ?
C2 C19 C21 108.3(7) . . ?
C2 C19 C22 111.9(8) . . ?
C20 C19 C21 109.0(7) . . ?
C20 C19 C2 112.6(7) . . ?
C20 C19 C22 106.9(7) . . ?
C22 C19 C21 108.0(7) . . ?
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 . . ?
S1 C10 H10A 110.1 . . ?
S1 C10 H10B 110.1 . . ?
C11 C10 S1 108.2(5) . . ?
C11 C10 H10A 110.1 . . ?
C11 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
N1 C8 H8A 109.4 . . ?
N1 C8 H8B 109.4 . . ?
N1 C8 C9 111.0(7) . . ?
H8A C8 H8B 108.0 . . ?
C9 C8 H8A 109.4 . . ?
C9 C8 H8B 109.4 . . ?
O5 C23 H23A 109.5 . . ?
O5 C23 H23B 109.5 . . ?
O5 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N2 C12 H12 115.7 . . ?
N2 C12 C13 128.7(8) . . ?
C13 C12 H12 115.7 . . ?
S1 C9 H9A 110.2 . . ?
S1 C9 H9B 110.2 . . ?
C8 C9 S1 107.7(6) . . ?
C8 C9 H9A 110.2 . . ?
C8 C9 H9B 110.2 . . ?
H9A C9 H9B 108.5 . . ?
C15 C14 H14 119.1 . . ?
C15 C14 C13 121.8(8) . . ?
C13 C14 H14 119.1 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C13 C12 122.4(8) . . ?
C14 C13 C18 121.2(8) . . ?
C14 C13 C12 116.4(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 . . ?
O6 C28 H28A 109.5 . . ?
O6 C28 H28B 109.5 . . ?
O6 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Cl2B C29 H29A 114.3 . . ?
Cl2B C29 H29B 114.3 . . ?
Cl2B C29 Cl1B 85.9(11) . . ?
Cl1A C29 H29C 111.4 . . ?
Cl1A C29 H29D 111.4 . . ?
H29A C29 H29B 111.5 . . ?
H29C C29 H29D 109.3 . . ?
Cl1B C29 H29A 114.3 . . ?
Cl1B C29 H29B 114.3 . . ?
Cl2A C29 Cl1A 101.8(14) . . ?
Cl2A C29 H29C 111.4 . . ?
Cl2A C29 H29D 111.4 . . ?

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 S1 C10 C11 41.0(6) . . . . ?
U1 S1 C9 C8 -62.4(6) . . . . ?
U1 O4 C18 C17 126.8(7) . . . . ?
U1 O4 C18 C13 -55.0(10) . . . . ?
U1 N2 C11 C10 59.0(7) . . . . ?
U1 N2 C12 C13 4.1(12) . . . . ?
U1 O3 C1 C6 -53.9(9) . . . . ?
U1 O3 C1 C2 128.6(6) . . . . ?
U1 N1 C7 C6 7.8(11) . . . . ?
U1 N1 C8 C9 30.5(9) . . . . ?
O4 C18 C13 C12 7.6(12) . . . . ?
O4 C18 C13 C14 -171.9(7) . . . . ?
O5 C4 C3 C2 -174.9(7) . . . . ?
N2 C11 C10 S1 -66.9(8) . . . . ?
N2 C12 C13 C18 15.0(13) . . . . ?
N2 C12 C13 C14 -165.5(8) . . . . ?
O3 C1 C2 C3 177.6(7) . . . . ?
O3 C1 C2 C19 -5.0(11) . . . . ?
O6 C15 C14 C13 -179.2(8) . . . . ?
C17 C16 C15 O6 -179.9(7) . . . . ?
C17 C16 C15 C14 2.3(12) . . . . ?
C17 C18 C13 C12 -174.1(7) . . . . ?
C17 C18 C13 C14 6.3(12) . . . . ?
C5 C4 C3 C2 1.4(12) . . . . ?
C5 C6 C1 O3 -175.3(7) . . . . ?
C5 C6 C1 C2 2.3(11) . . . . ?
C5 C6 C7 N1 -164.0(8) . . . . ?
N1 C8 C9 S1 31.4(9) . . . . ?
C4 C5 C6 C1 -2.8(11) . . . . ?
C4 C5 C6 C7 -176.7(7) . . . . ?
C16 C17 C24 C26 119.8(8) . . . . ?
C16 C17 C24 C25 -118.7(8) . . . . ?
C16 C17 C24 C27 0.9(11) . . . . ?
C16 C17 C18 O4 172.5(7) . . . . ?
C16 C17 C18 C13 -5.7(11) . . . . ?
C16 C15 C14 C13 -1.8(12) . . . . ?
C15 C14 C13 C18 -2.6(13) . . . . ?
C15 C14 C13 C12 177.9(7) . . . . ?
C6 C5 C4 O5 176.9(7) . . . . ?
C6 C5 C4 C3 1.0(11) . . . . ?
C6 C1 C2 C3 0.0(11) . . . . ?
C6 C1 C2 C19 177.3(7) . . . . ?
C1 C6 C7 N1 22.2(12) . . . . ?
C1 C2 C3 C4 -1.9(12) . . . . ?
C1 C2 C19 C21 61.8(9) . . . . ?
C1 C2 C19 C20 -58.8(10) . . . . ?
C1 C2 C19 C22 -179.3(7) . . . . ?
C11 N2 C12 C13 178.4(8) . . . . ?
C7 N1 C8 C9 -146.8(8) . . . . ?
C7 C6 C1 O3 -1.8(11) . . . . ?
C7 C6 C1 C2 175.8(7) . . . . ?
C3 C2 C19 C21 -121.0(8) . . . . ?
C3 C2 C19 C20 118.4(8) . . . . ?
C3 C2 C19 C22 -2.1(11) . . . . ?
C24 C17 C16 C15 -176.0(7) . . . . ?
C24 C17 C18 O4 -9.9(12) . . . . ?
C24 C17 C18 C13 171.8(7) . . . . ?
C18 C17 C16 C15 1.6(12) . . . . ?
C18 C17 C24 C26 -57.7(10) . . . . ?
C18 C17 C24 C25 63.9(10) . . . . ?
C18 C17 C24 C27 -176.5(7) . . . . ?
C19 C2 C3 C4 -179.2(7) . . . . ?
C10 S1 C9 C8 -162.9(6) . . . . ?
C8 N1 C7 C6 -175.1(7) . . . . ?
C23 O5 C4 C5 -1.3(11) . . . . ?
C23 O5 C4 C3 174.8(7) . . . . ?
C12 N2 C11 C10 -115.6(8) . . . . ?
C9 S1 C10 C11 134.3(6) . . . . ?
C28 O6 C15 C16 173.4(7) . . . . ?
C28 O6 C15 C14 -9.0(12) . . . . ?

_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 2.756
_oxdiff_exptl_absorpt_empirical_full_min 0.441
####################################################################### 
# 
# 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_211115_uo2meosaldien
_database_code_depnum_ccdc_archive 'CCDC 2177297'
loop_
_audit_author_name
_audit_author_address
'Tomoyuki Takeyama'
;Tokyo Institute of Thechnology
Japan
;
_audit_update_record             
;
2022-06-06 deposited with the CCDC.	2022-08-22 downloaded from the CCDC.
;
_audit_creation_date             2021-11-22
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H39 N3 O6 U, C H2 Cl2'
_chemical_formula_sum            'C29 H41 Cl2 N3 O6 U'
_chemical_formula_weight         836.58
_chemical_melting_point          ?
_chemical_oxdiff_formula         C29H34N3O6U1
_chemical_oxdiff_usercomment     211115_UO2MeOsaldien
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'

_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/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   9.9547(2)
_cell_length_b                   29.1269(5)
_cell_length_c                   11.6812(2)
_cell_angle_alpha                90
_cell_angle_beta                 106.798(2)
_cell_angle_gamma                90
_cell_volume                     3242.44(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16046
_cell_measurement_temperature    123
_cell_measurement_theta_max      30.7740
_cell_measurement_theta_min      2.0130
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.214
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62171
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1640
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 38 1 0.0721
-5 -38 0 0.0465
8 19 -14 0.0718
-1 20 14 0.1352
13 2 0 0.0398
6 -20 -14 0.1016
-13 -2 0 0.0184
-5 -5 16 0.1449

_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.059
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
4.3984 38.4801 0.9352 0.0000 0.8480 0.5300
-4.8774 -38.3624 0.3705 -0.0000 -0.8878 -0.4603
7.5083 18.5475 -13.8042 0.0000 0.8721 -0.4893
-1.4818 20.2404 14.1056 0.0929 0.0414 0.9948
13.3876 1.7144 0.1532 0.9109 0.4055 0.0767
6.4731 -19.5287 -13.9983 0.2473 0.1101 -0.9627
-13.3623 -1.8434 -0.2443 -0.9104 -0.4053 -0.0830
-4.9610 -5.2961 16.2833 0.1272 -0.5984 0.7911

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36149
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.960
_diffrn_reflns_theta_min         2.296
_diffrn_ambient_temperature      123
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      6.00  35.00   0.50   28.35    --   20.00  54.00  90.00   58
  2  ω     43.00  86.00   0.50   28.35    --   20.00  54.00  90.00   86
  3  ω    -74.00 109.00   0.50   28.35    --   20.00  54.00-150.00  366
  4  ω    -50.00 -15.00   0.50   28.35    --   20.00  54.00-120.00   70
  5  ω     48.00  73.00   0.50   28.35    --   20.00  54.00-120.00   50
  6  ω    -70.00   2.00   0.50   28.35    --   20.00  54.00  30.00  144
  7  ω     55.00  80.00   0.50   28.35    --   20.00  54.00  30.00   50
  8  ω     85.00 110.00   0.50   28.35    --   20.00  54.00  30.00   50
  9  ω    -29.00  -1.00   0.50   28.35    --   20.00  54.00 150.00   56
 10  ω     59.00  84.00   0.50   28.35    --   20.00  54.00 150.00   50
 11  ω    -71.00  28.00   0.50   28.35    --   20.00  54.00 -30.00  198
 12  ω    -27.00  -2.00   0.50   28.35    --   20.00  54.00  90.00   50
;
_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      0.0688281000
_diffrn_orient_matrix_UB_12      -0.0084996000
_diffrn_orient_matrix_UB_13      0.0260161000
_diffrn_orient_matrix_UB_21      0.0280633000
_diffrn_orient_matrix_UB_22      0.0193618000
_diffrn_orient_matrix_UB_23      -0.0219008000
_diffrn_orient_matrix_UB_31      0.0035711000
_diffrn_orient_matrix_UB_32      0.0120627000
_diffrn_orient_matrix_UB_33      0.0535920000
_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                7869
_reflns_number_total             9910
_reflns_odcompleteness_completeness 99.96
_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         1.732
_refine_diff_density_min         -1.817
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         9910
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0333
_refine_ls_restrained_S_all      1.068
_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)+(0.0193P)²+4.7176P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0624
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H9AA(0.6) H9AB(0.6) H9BC(0.4) H9BD(0.4) H11C(0.4) H11D(0.4)
 H11B(0.6) H11A(0.6) N3A(0.6) H3A(0.6) C10B(0.4) H10A(0.4) H10B(0.4) N3B(0.4)
 H3B(0.4) C10A(0.6) H10C(0.6) H10D(0.6)
3.a Ternary CH refined with riding coordinates:
 N3A(H3A), N3B(H3B)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9AA,H9AB), C9(H9BC,H9BD), C8(H8A,H8B), C11(H11C,H11D), C11(H11B,H11A),
 C10B(H10A,H10B), C29(H29A,H29B), C10A(H10C,H10D)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C3(H3), C14(H14), C12(H12), C16(H16)
3.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C21(H21A,H21B,H21C), C28(H28A,
 H28B,H28C)
;
_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 0.71958(2) 0.44582(2) 0.42211(2) 0.01576(3) Uani 1 1 d . . . . .
Cl2 Cl 0.61582(15) 0.35804(4) 0.78360(13) 0.0590(3) Uani 1 1 d . . . . .
Cl1 Cl 0.42488(15) 0.31697(5) 0.57145(11) 0.0654(4) Uani 1 1 d . . . . .
O3 O 0.5849(2) 0.43446(7) 0.23456(18) 0.0193(5) Uani 1 1 d . . . . .
O2 O 0.5615(2) 0.44638(8) 0.46551(19) 0.0230(5) Uani 1 1 d . . . . .
O5 O 0.1307(3) 0.51837(9) -0.0850(2) 0.0287(6) Uani 1 1 d . . . . .
O4 O 0.7587(2) 0.37047(7) 0.45238(18) 0.0193(5) Uani 1 1 d . . . . .
O1 O 0.8862(2) 0.44969(8) 0.3925(2) 0.0235(5) Uani 1 1 d . . . . .
O6 O 1.2083(3) 0.26083(8) 0.6846(2) 0.0265(5) Uani 1 1 d . . . . .
C4 C 0.2467(4) 0.50016(12) -0.0024(3) 0.0215(7) Uani 1 1 d . . . . .
C5 C 0.3613(3) 0.52506(11) 0.0605(3) 0.0189(6) Uani 1 1 d . . . . .
H5 H 0.366185 0.557090 0.046791 0.023 Uiso 1 1 calc R U . . .
C7 C 0.5835(3) 0.53236(11) 0.2142(3) 0.0182(6) Uani 1 1 d . . . . .
H7 H 0.589922 0.562105 0.182833 0.022 Uiso 1 1 calc R U . . .
C3 C 0.2425(4) 0.45321(11) 0.0182(3) 0.0222(7) Uani 1 1 d . . . . .
H3 H 0.161212 0.436604 -0.024262 0.027 Uiso 1 1 calc R U . . .
N2 N 0.8452(3) 0.43125(9) 0.6427(2) 0.0177(5) Uani 1 1 d . . . . .
N1 N 0.6744(3) 0.52210(9) 0.3133(2) 0.0193(6) Uani 1 1 d . . . . .
C6 C 0.4716(3) 0.50280(11) 0.1454(3) 0.0174(6) Uani 1 1 d . . . . .
C2 C 0.3509(4) 0.42935(11) 0.0978(3) 0.0189(6) Uani 1 1 d . . . . .
C1 C 0.4711(3) 0.45481(11) 0.1618(3) 0.0180(6) Uani 1 1 d . . . . .
C23 C 0.1335(4) 0.56647(12) -0.1051(3) 0.0286(8) Uani 1 1 d . . . . .
H23A H 0.046903 0.575697 -0.165393 0.043 Uiso 1 1 calc R U . . .
H23B H 0.214362 0.574001 -0.133460 0.043 Uiso 1 1 calc R U . . .
H23C H 0.141134 0.582872 -0.030207 0.043 Uiso 1 1 calc R U . . .
C14 C 1.0717(3) 0.33040(11) 0.6833(3) 0.0193(6) Uani 1 1 d . . . . .
H14 H 1.127453 0.339229 0.760789 0.023 Uiso 1 1 calc R U . . .
C9 C 0.7652(4) 0.56266(10) 0.5003(3) 0.0223(7) Uani 1 1 d . . . . .
H9AA H 0.827652 0.587429 0.543441 0.027 Uiso 0.6 1 calc R U P A 1
H9AB H 0.667810 0.569495 0.500497 0.027 Uiso 0.6 1 calc R U P A 1
H9BC H 0.852565 0.577165 0.549942 0.027 Uiso 0.4 1 calc R U P B 2
H9BD H 0.686455 0.583525 0.499716 0.027 Uiso 0.4 1 calc R U P B 2
C13 C 0.9569(3) 0.35789(10) 0.6213(3) 0.0171(6) Uani 1 1 d . . . . .
C15 C 1.1027(4) 0.29122(11) 0.6323(3) 0.0202(7) Uani 1 1 d . . . . .
C12 C 0.9278(3) 0.39777(11) 0.6844(3) 0.0188(6) Uani 1 1 d . . . . .
H12 H 0.976450 0.399219 0.767242 0.023 Uiso 1 1 calc R U . . .
C20 C 0.3596(4) 0.36559(12) 0.2470(3) 0.0293(8) Uani 1 1 d . . . . .
H20A H 0.453051 0.375359 0.295208 0.044 Uiso 1 1 calc R U . . .
H20B H 0.349967 0.332374 0.255401 0.044 Uiso 1 1 calc R U . . .
H20C H 0.287998 0.381540 0.274544 0.044 Uiso 1 1 calc R U . . .
C22 C 0.1958(4) 0.35789(13) 0.0442(3) 0.0337(9) Uani 1 1 d . . . . .
H22A H 0.121998 0.373892 0.068756 0.051 Uiso 1 1 calc R U . . .
H22B H 0.192485 0.325031 0.061252 0.051 Uiso 1 1 calc R U . . .
H22C H 0.181006 0.362344 -0.041701 0.051 Uiso 1 1 calc R U . . .
C17 C 0.9049(4) 0.30415(11) 0.4538(3) 0.0192(6) Uani 1 1 d . . . . .
C8 C 0.7744(4) 0.55802(12) 0.3736(3) 0.0249(7) Uani 1 1 d . . . . .
H8A H 0.750447 0.587564 0.330655 0.030 Uiso 1 1 calc R U . . .
H8B H 0.870890 0.549408 0.374584 0.030 Uiso 1 1 calc R U . . .
C18 C 0.8715(3) 0.34549(10) 0.5061(3) 0.0169(6) Uani 1 1 d . . . . .
C16 C 1.0189(4) 0.27892(11) 0.5179(3) 0.0217(7) Uani 1 1 d . . . . .
H16 H 1.041981 0.251751 0.482701 0.026 Uiso 1 1 calc R U . . .
C19 C 0.3404(4) 0.37743(11) 0.1141(3) 0.0224(7) Uani 1 1 d . . . . .
C24 C 1.2944(4) 0.27247(13) 0.8018(3) 0.0300(8) Uani 1 1 d . . . . .
H24A H 1.338368 0.302426 0.799435 0.045 Uiso 1 1 calc R U . . .
H24B H 1.367387 0.249093 0.829472 0.045 Uiso 1 1 calc R U . . .
H24C H 1.236423 0.273871 0.856683 0.045 Uiso 1 1 calc R U . . .
C11 C 0.8314(5) 0.46697(12) 0.7292(3) 0.0328(9) Uani 1 1 d . . . . .
H11C H 0.907646 0.463406 0.804834 0.039 Uiso 0.4 1 calc R U P C 2
H11D H 0.740639 0.463292 0.746957 0.039 Uiso 0.4 1 calc R U P C 2
H11B H 0.770471 0.455292 0.776292 0.039 Uiso 0.6 1 calc R U P D 1
H11A H 0.925021 0.473420 0.785290 0.039 Uiso 0.6 1 calc R U P D 1
N3A N 0.8121(6) 0.51646(18) 0.5571(5) 0.0173(10) Uani 0.6 1 d . . P E 1
H3A H 0.916880 0.515686 0.579260 0.021 Uiso 0.6 1 calc R U P E 1
C26 C 0.8220(4) 0.32550(13) 0.2366(3) 0.0348(9) Uani 1 1 d . . . . .
H26A H 0.764577 0.315892 0.157176 0.052 Uiso 1 1 calc R U . . .
H26B H 0.919402 0.329678 0.235716 0.052 Uiso 1 1 calc R U . . .
H26C H 0.785930 0.354533 0.258258 0.052 Uiso 1 1 calc R U . . .
C27 C 0.6646(4) 0.27948(12) 0.3302(3) 0.0315(8) Uani 1 1 d . . . . .
H27A H 0.623519 0.307986 0.349498 0.047 Uiso 1 1 calc R U . . .
H27B H 0.664275 0.256158 0.390564 0.047 Uiso 1 1 calc R U . . .
H27C H 0.609175 0.268541 0.251315 0.047 Uiso 1 1 calc R U . . .
C21 C 0.4526(4) 0.35354(13) 0.0692(3) 0.0326(9) Uani 1 1 d . . . . .
H21A H 0.435455 0.359860 -0.016181 0.049 Uiso 1 1 calc R U . . .
H21B H 0.448632 0.320347 0.081648 0.049 Uiso 1 1 calc R U . . .
H21C H 0.545522 0.365106 0.113565 0.049 Uiso 1 1 calc R U . . .
C25 C 0.8161(4) 0.28851(12) 0.3288(3) 0.0248(7) Uani 1 1 d . . . . .
C10B C 0.8391(12) 0.5139(4) 0.6780(9) 0.024(2) Uani 0.4 1 d . . P E 2
H10A H 0.815052 0.537112 0.730831 0.029 Uiso 0.4 1 calc R U P E 2
H10B H 0.936822 0.519769 0.677183 0.029 Uiso 0.4 1 calc R U P E 2
C29 C 0.5800(5) 0.34775(18) 0.6292(4) 0.0573(14) Uani 1 1 d . . . . .
H29A H 0.572820 0.377470 0.586698 0.069 Uiso 1 1 calc R U . . .
H29B H 0.658881 0.330354 0.614514 0.069 Uiso 1 1 calc R U . . .
C28 C 0.8730(5) 0.24415(13) 0.2899(3) 0.0392(10) Uani 1 1 d . . . . .
H28A H 0.815566 0.235709 0.209420 0.059 Uiso 1 1 calc R U . . .
H28B H 0.869416 0.219458 0.345960 0.059 Uiso 1 1 calc R U . . .
H28C H 0.970267 0.248890 0.289472 0.059 Uiso 1 1 calc R U . . .
N3B N 0.7448(9) 0.5198(3) 0.5557(7) 0.0179(16) Uani 0.4 1 d . . P E 2
H3B H 0.649929 0.523325 0.567940 0.021 Uiso 0.4 1 calc R U P E 2
C10A C 0.7713(7) 0.5100(2) 0.6685(7) 0.0220(14) Uani 0.6 1 d . . P E 1
H10C H 0.805246 0.536361 0.722716 0.026 Uiso 0.6 1 calc R U P E 1
H10D H 0.667729 0.508988 0.649096 0.026 Uiso 0.6 1 calc R U P E 1


_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 2.238(2) . ?
U1 O2 1.788(2) . ?
U1 O4 2.239(2) . ?
U1 O1 1.793(2) . ?
U1 N2 2.554(3) . ?
U1 N1 2.535(3) . ?
U1 N3A 2.594(5) . ?
U1 N3B 2.630(8) . ?
Cl2 C29 1.761(5) . ?
Cl1 C29 1.744(5) . ?
O3 C1 1.342(4) . ?
O5 C4 1.380(4) . ?
O5 C23 1.422(4) . ?
O4 C18 1.333(4) . ?
O6 C15 1.375(4) . ?
O6 C24 1.430(4) . ?
C4 C5 1.372(5) . ?
C4 C3 1.391(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.407(4) . ?
C7 H7 0.9500 . ?
C7 N1 1.281(4) . ?
C7 C6 1.453(4) . ?
C3 H3 0.9500 . ?
C3 C2 1.390(5) . ?
N2 C12 1.278(4) . ?
N2 C11 1.483(4) . ?
N1 C8 1.475(4) . ?
C6 C1 1.411(4) . ?
C2 C1 1.423(4) . ?
C2 C19 1.531(5) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C14 H14 0.9500 . ?
C14 C13 1.412(4) . ?
C14 C15 1.364(4) . ?
C9 H9AA 0.9900 . ?
C9 H9AB 0.9900 . ?
C9 H9BC 0.9900 . ?
C9 H9BD 0.9900 . ?
C9 C8 1.515(5) . ?
C9 N3A 1.514(6) . ?
C9 N3B 1.447(9) . ?
C13 C12 1.449(4) . ?
C13 C18 1.415(4) . ?
C15 C16 1.402(5) . ?
C12 H12 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C20 C19 1.547(5) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C22 C19 1.544(5) . ?
C17 C18 1.432(4) . ?
C17 C16 1.377(4) . ?
C17 C25 1.541(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C16 H16 0.9500 . ?
C19 C21 1.531(5) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C11 H11C 0.9900 . ?
C11 H11D 0.9900 . ?
C11 H11B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 C10B 1.503(12) . ?
C11 C10A 1.479(8) . ?
N3A H3A 1.0000 . ?
N3A C10A 1.482(9) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C26 C25 1.536(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C27 C25 1.536(5) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C25 C28 1.531(5) . ?
C10B H10A 0.9900 . ?
C10B H10B 0.9900 . ?
C10B N3B 1.476(13) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
N3B H3B 1.0000 . ?
C10A H10C 0.9900 . ?
C10A H10D 0.9900 . ?

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 92.14(8) . . ?
O3 U1 N2 160.62(8) . . ?
O3 U1 N1 70.69(8) . . ?
O3 U1 N3A 136.00(13) . . ?
O3 U1 N3B 129.00(19) . . ?
O2 U1 O3 87.22(9) . . ?
O2 U1 O4 95.25(10) . . ?
O2 U1 O1 173.45(10) . . ?
O2 U1 N2 85.98(9) . . ?
O2 U1 N1 95.23(10) . . ?
O2 U1 N3A 90.42(15) . . ?
O2 U1 N3B 76.4(2) . . ?
O4 U1 N2 70.47(8) . . ?
O4 U1 N1 159.38(8) . . ?
O4 U1 N3A 131.79(13) . . ?
O4 U1 N3B 136.65(19) . . ?
O1 U1 O3 98.41(9) . . ?
O1 U1 O4 87.92(9) . . ?
O1 U1 N2 89.70(9) . . ?
O1 U1 N1 83.57(10) . . ?
O1 U1 N3A 83.21(15) . . ?
O1 U1 N3B 97.4(2) . . ?
N2 U1 N3A 62.23(13) . . ?
N2 U1 N3B 66.59(19) . . ?
N1 U1 N2 128.02(8) . . ?
N1 U1 N3A 65.79(14) . . ?
N1 U1 N3B 63.37(19) . . ?
C1 O3 U1 135.41(18) . . ?
C4 O5 C23 116.2(3) . . ?
C18 O4 U1 133.9(2) . . ?
C15 O6 C24 116.2(3) . . ?
O5 C4 C3 116.0(3) . . ?
C5 C4 O5 124.7(3) . . ?
C5 C4 C3 119.3(3) . . ?
C4 C5 H5 120.3 . . ?
C4 C5 C6 119.5(3) . . ?
C6 C5 H5 120.3 . . ?
N1 C7 H7 116.9 . . ?
N1 C7 C6 126.2(3) . . ?
C6 C7 H7 116.9 . . ?
C4 C3 H3 118.3 . . ?
C2 C3 C4 123.4(3) . . ?
C2 C3 H3 118.3 . . ?
C12 N2 U1 125.8(2) . . ?
C12 N2 C11 116.9(3) . . ?
C11 N2 U1 117.1(2) . . ?
C7 N1 U1 129.3(2) . . ?
C7 N1 C8 118.0(3) . . ?
C8 N1 U1 112.6(2) . . ?
C5 C6 C7 115.7(3) . . ?
C5 C6 C1 121.3(3) . . ?
C1 C6 C7 122.9(3) . . ?
C3 C2 C1 117.6(3) . . ?
C3 C2 C19 120.6(3) . . ?
C1 C2 C19 121.8(3) . . ?
O3 C1 C6 119.2(3) . . ?
O3 C1 C2 122.0(3) . . ?
C6 C1 C2 118.7(3) . . ?
O5 C23 H23A 109.5 . . ?
O5 C23 H23B 109.5 . . ?
O5 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C15 C14 C13 120.1(3) . . ?
H9AA C9 H9AB 108.9 . . ?
H9BC C9 H9BD 107.6 . . ?
C8 C9 H9AA 110.8 . . ?
C8 C9 H9AB 110.8 . . ?
C8 C9 H9BC 108.6 . . ?
C8 C9 H9BD 108.6 . . ?
N3A C9 H9AA 110.8 . . ?
N3A C9 H9AB 110.8 . . ?
N3A C9 C8 104.5(3) . . ?
N3B C9 H9BC 108.6 . . ?
N3B C9 H9BD 108.6 . . ?
N3B C9 C8 114.6(4) . . ?
C14 C13 C12 116.4(3) . . ?
C14 C13 C18 121.2(3) . . ?
C18 C13 C12 122.3(3) . . ?
O6 C15 C16 115.3(3) . . ?
C14 C15 O6 125.8(3) . . ?
C14 C15 C16 118.9(3) . . ?
N2 C12 C13 128.3(3) . . ?
N2 C12 H12 115.9 . . ?
C13 C12 H12 115.9 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
C18 C17 C25 120.8(3) . . ?
C16 C17 C18 118.3(3) . . ?
C16 C17 C25 120.9(3) . . ?
N1 C8 C9 107.9(3) . . ?
N1 C8 H8A 110.1 . . ?
N1 C8 H8B 110.1 . . ?
C9 C8 H8A 110.1 . . ?
C9 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
O4 C18 C13 120.1(3) . . ?
O4 C18 C17 121.7(3) . . ?
C13 C18 C17 118.1(3) . . ?
C15 C16 H16 118.3 . . ?
C17 C16 C15 123.4(3) . . ?
C17 C16 H16 118.3 . . ?
C2 C19 C20 110.6(3) . . ?
C2 C19 C22 112.6(3) . . ?
C22 C19 C20 105.9(3) . . ?
C21 C19 C2 108.9(3) . . ?
C21 C19 C20 110.6(3) . . ?
C21 C19 C22 108.2(3) . . ?
O6 C24 H24A 109.5 . . ?
O6 C24 H24B 109.5 . . ?
O6 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N2 C11 H11C 109.7 . . ?
N2 C11 H11D 109.7 . . ?
N2 C11 H11B 109.2 . . ?
N2 C11 H11A 109.2 . . ?
N2 C11 C10B 110.0(5) . . ?
H11C C11 H11D 108.2 . . ?
H11B C11 H11A 107.9 . . ?
C10B C11 H11C 109.7 . . ?
C10B C11 H11D 109.7 . . ?
C10A C11 N2 111.9(4) . . ?
C10A C11 H11B 109.2 . . ?
C10A C11 H11A 109.2 . . ?
U1 N3A H3A 107.5 . . ?
C9 N3A U1 115.4(3) . . ?
C9 N3A H3A 107.5 . . ?
C10A N3A U1 107.1(4) . . ?
C10A N3A C9 111.7(5) . . ?
C10A N3A H3A 107.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C26 C25 C17 109.2(3) . . ?
C27 C25 C17 109.7(3) . . ?
C27 C25 C26 111.4(3) . . ?
C28 C25 C17 111.7(3) . . ?
C28 C25 C26 106.9(3) . . ?
C28 C25 C27 107.9(3) . . ?
C11 C10B H10A 108.9 . . ?
C11 C10B H10B 108.9 . . ?
H10A C10B H10B 107.7 . . ?
N3B C10B C11 113.5(8) . . ?
N3B C10B H10A 108.9 . . ?
N3B C10B H10B 108.9 . . ?
Cl2 C29 H29A 109.2 . . ?
Cl2 C29 H29B 109.2 . . ?
Cl1 C29 Cl2 112.2(2) . . ?
Cl1 C29 H29A 109.2 . . ?
Cl1 C29 H29B 109.2 . . ?
H29A C29 H29B 107.9 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
U1 N3B H3B 103.7 . . ?
C9 N3B U1 116.3(4) . . ?
C9 N3B C10B 113.6(7) . . ?
C9 N3B H3B 103.7 . . ?
C10B N3B U1 113.8(6) . . ?
C10B N3B H3B 103.7 . . ?
C11 C10A N3A 110.6(5) . . ?
C11 C10A H10C 109.5 . . ?
C11 C10A H10D 109.5 . . ?
N3A C10A H10C 109.5 . . ?
N3A C10A H10D 109.5 . . ?
H10C C10A H10D 108.1 . . ?

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 50.9(4) . . . . ?
U1 O3 C1 C2 -130.7(3) . . . . ?
U1 O4 C18 C13 47.9(4) . . . . ?
U1 O4 C18 C17 -136.4(3) . . . . ?
U1 N2 C12 C13 -8.2(5) . . . . ?
U1 N2 C11 C10B -39.9(6) . . . . ?
U1 N2 C11 C10A -12.5(5) . . . . ?
U1 N1 C8 C9 -57.0(3) . . . . ?
U1 N3A C10A C11 59.0(6) . . . . ?
O5 C4 C5 C6 178.0(3) . . . . ?
O5 C4 C3 C2 179.5(3) . . . . ?
O6 C15 C16 C17 177.3(3) . . . . ?
C4 C5 C6 C7 -175.4(3) . . . . ?
C4 C5 C6 C1 4.2(5) . . . . ?
C4 C3 C2 C1 0.7(5) . . . . ?
C4 C3 C2 C19 -178.6(3) . . . . ?
C5 C4 C3 C2 -1.8(5) . . . . ?
C5 C6 C1 O3 173.1(3) . . . . ?
C5 C6 C1 C2 -5.3(4) . . . . ?
C7 N1 C8 C9 125.7(3) . . . . ?
C7 C6 C1 O3 -7.3(4) . . . . ?
C7 C6 C1 C2 174.3(3) . . . . ?
C3 C4 C5 C6 -0.6(5) . . . . ?
C3 C2 C1 O3 -175.5(3) . . . . ?
C3 C2 C1 C6 2.8(4) . . . . ?
C3 C2 C19 C20 -124.0(3) . . . . ?
C3 C2 C19 C22 -5.7(4) . . . . ?
C3 C2 C19 C21 114.3(3) . . . . ?
N2 C11 C10B N3B 49.8(9) . . . . ?
N2 C11 C10A N3A -31.3(7) . . . . ?
N1 C7 C6 C5 161.9(3) . . . . ?
N1 C7 C6 C1 -17.7(5) . . . . ?
C6 C7 N1 U1 7.3(5) . . . . ?
C6 C7 N1 C8 -176.0(3) . . . . ?
C1 C2 C19 C20 56.7(4) . . . . ?
C1 C2 C19 C22 175.0(3) . . . . ?
C1 C2 C19 C21 -65.0(4) . . . . ?
C23 O5 C4 C5 0.4(5) . . . . ?
C23 O5 C4 C3 179.0(3) . . . . ?
C14 C13 C12 N2 168.6(3) . . . . ?
C14 C13 C18 O4 175.9(3) . . . . ?
C14 C13 C18 C17 0.0(5) . . . . ?
C14 C15 C16 C17 -0.7(5) . . . . ?
C9 N3A C10A C11 -173.8(4) . . . . ?
C13 C14 C15 O6 -177.8(3) . . . . ?
C13 C14 C15 C16 0.0(5) . . . . ?
C15 C14 C13 C12 177.3(3) . . . . ?
C15 C14 C13 C18 0.3(5) . . . . ?
C12 N2 C11 C10B 134.7(5) . . . . ?
C12 N2 C11 C10A 162.1(4) . . . . ?
C12 C13 C18 O4 -0.9(5) . . . . ?
C12 C13 C18 C17 -176.9(3) . . . . ?
C8 C9 N3A U1 -40.9(4) . . . . ?
C8 C9 N3A C10A -163.5(4) . . . . ?
C8 C9 N3B U1 -2.2(6) . . . . ?
C8 C9 N3B C10B 132.9(7) . . . . ?
C18 C13 C12 N2 -14.4(5) . . . . ?
C18 C17 C16 C15 1.0(5) . . . . ?
C18 C17 C25 C26 60.5(4) . . . . ?
C18 C17 C25 C27 -61.8(4) . . . . ?
C18 C17 C25 C28 178.6(3) . . . . ?
C16 C17 C18 O4 -176.5(3) . . . . ?
C16 C17 C18 C13 -0.6(5) . . . . ?
C16 C17 C25 C26 -119.0(3) . . . . ?
C16 C17 C25 C27 118.7(3) . . . . ?
C16 C17 C25 C28 -0.9(5) . . . . ?
C19 C2 C1 O3 3.8(5) . . . . ?
C19 C2 C1 C6 -177.9(3) . . . . ?
C24 O6 C15 C14 -1.6(5) . . . . ?
C24 O6 C15 C16 -179.5(3) . . . . ?
C11 N2 C12 C13 177.7(3) . . . . ?
C11 C10B N3B U1 -36.1(10) . . . . ?
C11 C10B N3B C9 -172.3(6) . . . . ?
N3A C9 C8 N1 63.0(4) . . . . ?
C25 C17 C18 O4 4.0(5) . . . . ?
C25 C17 C18 C13 179.8(3) . . . . ?
C25 C17 C16 C15 -179.4(3) . . . . ?
N3B C9 C8 N1 37.3(5) . . . . ?

_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 1.545
_oxdiff_exptl_absorpt_empirical_full_min 0.866
