# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_Emily073115_0m
_database_code_depnum_ccdc_archive 'CCDC 1523762'
_audit_update_record             
;
2016-12-20 deposited with the CCDC.
2018-08-28 downloaded from the CCDC.
;
_audit_creation_date             2016-12-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4715)
;
_chemical_formula_moiety         'C H2 Cl2, C28 H20 N2 O2'
_chemical_formula_sum            'C29 H22 Cl2 N2 O2'
_chemical_formula_weight         501.42
_chemical_absolute_configuration unk
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cl 0.14873 0.16029 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55739974976
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x+1/2,-y+1/2,-z
3 -x,y+1/2,-z+1/2
4 -x+1/2,-y,z+1/2

_symmetry_Int_Tables_number      19
_cell_length_a                   7.1378(10)
_cell_length_b                   16.682(2)
_cell_length_c                   20.056(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2388.1(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3361
_cell_measurement_temperature    180.45
_cell_measurement_theta_max      23.052
_cell_measurement_theta_min      2.369
_exptl_absorpt_coefficient_mu    0.303
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0961 before and 0.0560 after correction. The Ratio of minimum to maximum transmission is 0.8052. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.3945
_exptl_crystal_description       prism
_exptl_crystal_F_000             1041.5971
_exptl_crystal_recrystallization_method 'Slow evaporation of a DCM solution'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17603
_diffrn_reflns_theta_full        28.6982
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         2.03
_diffrn_ambient_temperature      180.45
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9985
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.997
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              27
_reflns_limit_l_min              -26
_reflns_number_gt                4545
_reflns_number_total             6177
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.6454
_refine_diff_density_min         -0.6401
_refine_diff_density_rms         0.0920
_refine_ls_abs_structure_details 
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.10(7)
_refine_ls_d_res_high            0.7400
_refine_ls_d_res_low             10.0278
_refine_ls_goodness_of_fit_ref   1.0365
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    42
_refine_ls_number_parameters     318
_refine_ls_number_reflns         6177
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0556
_refine_ls_restrained_S_all      1.0365
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0625P)²+0.1921P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1284
_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 O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C29(H29a,H29b)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C11(H11), C18(H18), C24(H24), C23(H23), C3(H3), C2(H2a),
 C8(H8), C7(H7), C13(H13), C14(H14), C15(H15), C16(H16), C26(H26), C27(H27),
 C22(H22), C21(H21), N1(H1)
;
_atom_sites_solution_primary     direct
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_refinement_flags_posn
Cl1 Cl 0.26943(12) 0.07111(5) 0.72797(4) 0.0547(2) Uani 1.000000 .
Cl2 Cl -0.00910(15) -0.02667(6) 0.66138(5) 0.0767(3) Uani 1.000000 .
O1 O 0.3838(3) 0.07588(10) 0.54549(9) 0.0336(4) Uani 1.000000 .
O2 O 0.1504(3) 0.21896(10) 0.58760(10) 0.0326(4) Uani 1.000000 .
H2 H 0.157(5) 0.2158(18) 0.5480(17) 0.0488(7) Uiso 1.000000 R
N1 N 0.3053(3) 0.09987(10) 0.42184(10) 0.0219(4) Uani 1.000000 .
N2 N 0.2093(3) 0.24985(10) 0.46363(10) 0.0230(4) Uani 1.000000 .
C6 C 0.5919(4) -0.26726(15) 0.42462(15) 0.0394(7) Uani 1.000000 .
H6 H 0.6378(4) -0.31959(15) 0.41555(15) 0.0473(8) Uiso 1.000000 R
C5 C 0.6087(4) -0.23491(14) 0.48704(15) 0.0332(6) Uani 1.000000 .
H5 H 0.6646(4) -0.26556(14) 0.52165(15) 0.0399(7) Uiso 1.000000 R
C4 C 0.5436(3) -0.15596(13) 0.50084(13) 0.0261(5) Uani 1.000000 .
C9 C 0.4655(3) -0.10922(13) 0.44960(12) 0.0229(5) Uani 1.000000 .
C10 C 0.4117(3) -0.02674(13) 0.46339(12) 0.0213(5) Uani 1.000000 .
C11 C 0.3519(3) 0.02414(13) 0.41255(12) 0.0220(5) Uani 1.000000 .
H11 H 0.3441(3) 0.00307(13) 0.36863(12) 0.0264(6) Uiso 1.000000 R
C12 C 0.2486(3) 0.15544(13) 0.37319(11) 0.0211(5) Uani 1.000000 .
C17 C 0.1991(3) 0.23303(13) 0.39437(12) 0.0210(5) Uani 1.000000 .
C18 C 0.2578(3) 0.32185(12) 0.48180(12) 0.0222(5) Uani 1.000000 .
H18 H 0.2909(3) 0.35963(12) 0.44837(12) 0.0266(6) Uiso 1.000000 R
C19 C 0.2632(3) 0.34641(13) 0.55052(11) 0.0215(5) Uani 1.000000 .
C20 C 0.3239(3) 0.42644(14) 0.56915(12) 0.0250(5) Uani 1.000000 .
C25 C 0.3177(3) 0.44914(14) 0.63715(13) 0.0292(6) Uani 1.000000 .
C24 C 0.3724(4) 0.52781(17) 0.65567(15) 0.0392(7) Uani 1.000000 .
H24 H 0.3676(4) 0.54324(17) 0.70124(15) 0.0471(8) Uiso 1.000000 R
C23 C 0.4318(4) 0.58177(16) 0.60892(17) 0.0421(7) Uani 1.000000 .
H23 H 0.4678(4) 0.63430(16) 0.62197(17) 0.0505(9) Uiso 1.000000 R
C3 C 0.5601(4) -0.12340(15) 0.56669(14) 0.0313(6) Uani 1.000000 .
H3 H 0.6118(4) -0.15555(15) 0.60118(14) 0.0376(7) Uiso 1.000000 R
C2 C 0.5040(4) -0.04853(15) 0.58071(14) 0.0310(6) Uani 1.000000 .
H2a H 0.5136(4) -0.02964(15) 0.62526(14) 0.0372(7) Uiso 1.000000 R
C1 C 0.4296(3) 0.00431(13) 0.53007(13) 0.0258(5) Uani 1.000000 .
C8 C 0.4444(4) -0.14555(14) 0.38633(14) 0.0312(6) Uani 1.000000 .
H8 H 0.3863(4) -0.11642(14) 0.35128(14) 0.0374(7) Uiso 1.000000 R
C7 C 0.5067(4) -0.22237(15) 0.37463(15) 0.0373(6) Uani 1.000000 .
H7 H 0.4911(4) -0.24519(15) 0.33158(15) 0.0448(8) Uiso 1.000000 R
C13 C 0.2429(4) 0.13696(14) 0.30547(12) 0.0273(5) Uani 1.000000 .
H13 H 0.2769(4) 0.08480(14) 0.29082(12) 0.0328(6) Uiso 1.000000 R
C14 C 0.1881(4) 0.19395(15) 0.25954(13) 0.0315(6) Uani 1.000000 .
H14 H 0.1872(4) 0.18112(15) 0.21339(13) 0.0379(7) Uiso 1.000000 R
C15 C 0.1343(4) 0.27005(15) 0.28042(13) 0.0326(6) Uani 1.000000 .
H15 H 0.0947(4) 0.30886(15) 0.24874(13) 0.0392(7) Uiso 1.000000 R
C16 C 0.1387(4) 0.28888(14) 0.34746(13) 0.0285(6) Uani 1.000000 .
H16 H 0.1000(4) 0.34059(14) 0.36175(13) 0.0342(7) Uiso 1.000000 R
C26 C 0.2578(4) 0.39301(16) 0.68537(14) 0.0353(6) Uani 1.000000 .
H26 H 0.2544(4) 0.40836(16) 0.73097(14) 0.0423(7) Uiso 1.000000 R
C27 C 0.2049(3) 0.31754(15) 0.66807(13) 0.0316(6) Uani 1.000000 .
H27 H 0.1665(3) 0.28072(15) 0.70153(13) 0.0380(7) Uiso 1.000000 R
C28 C 0.2069(3) 0.29382(14) 0.60075(13) 0.0267(5) Uani 1.000000 .
C22 C 0.4395(4) 0.55930(15) 0.54190(14) 0.0328(6) Uani 1.000000 .
H22 H 0.4813(4) 0.59685(15) 0.50955(14) 0.0393(7) Uiso 1.000000 R
C21 C 0.3879(3) 0.48433(14) 0.52224(14) 0.0272(5) Uani 1.000000 .
H21 H 0.3947(3) 0.47041(14) 0.47637(14) 0.0326(6) Uiso 1.000000 R
C29 C 0.0966(4) 0.0681(2) 0.66637(16) 0.0500(8) Uani 1.000000 .
H29a H -0.0002(4) 0.1089(2) 0.67635(16) 0.0600(9) Uiso 1.000000 R
H29b H 0.1533(4) 0.0816(2) 0.62273(16) 0.0600(9) Uiso 1.000000 R
H1 H 0.3103(3) 0.11756(10) 0.46313(10) 0.0263(5) Uiso 1.000000 R


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl1 C29 1.747(3) .
Cl2 C29 1.755(3) .
O1 C1 1.276(3) .
O2 H2 0.80(3) .
O2 C28 1.338(3) .
N1 C11 1.319(3) .
N1 C12 1.405(3) .
N1 H1 0.8800 .
N2 C17 1.419(3) .
N2 C18 1.302(3) .
C6 H6 0.9500 .
C6 C5 1.369(4) .
C6 C7 1.392(4) .
C5 H5 0.9500 .
C5 C4 1.424(3) .
C4 C9 1.405(3) .
C4 C3 1.433(4) .
C9 C10 1.455(3) .
C9 C8 1.414(4) .
C10 C11 1.394(3) .
C10 C1 1.440(4) .
C11 H11 0.9500 .
C12 C17 1.407(3) .
C12 C13 1.393(3) .
C17 C16 1.392(3) .
C18 H18 0.9500 .
C18 C19 1.438(3) .
C19 C20 1.453(3) .
C19 C28 1.395(3) .
C20 C25 1.416(3) .
C20 C21 1.423(3) .
C25 C24 1.419(4) .
C25 C26 1.412(4) .
C24 H24 0.9500 .
C24 C23 1.367(4) .
C23 H23 0.9500 .
C23 C22 1.396(4) .
C3 H3 0.9500 .
C3 C2 1.341(4) .
C2 H2a 0.9500 .
C2 C1 1.446(4) .
C8 H8 0.9500 .
C8 C7 1.376(3) .
C7 H7 0.9500 .
C13 H13 0.9500 .
C13 C14 1.380(3) .
C14 H14 0.9500 .
C14 C15 1.391(4) .
C15 H15 0.9500 .
C15 C16 1.381(4) .
C16 H16 0.9500 .
C26 H26 0.9500 .
C26 C27 1.359(4) .
C27 H27 0.9500 .
C27 C28 1.407(4) .
C22 H22 0.9500 .
C22 C21 1.362(3) .
C21 H21 0.9500 .
C29 H29a 0.9900 .
C29 H29b 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
C28 O2 H2 104(2) . .
C12 N1 C11 127.3(2) . .
H1 N1 C11 116.35(14) . .
H1 N1 C12 116.35(12) . .
C18 N2 C17 118.05(19) . .
C5 C6 H6 120.49(15) . .
C7 C6 H6 120.49(15) . .
C7 C6 C5 119.0(2) . .
H5 C5 C6 119.54(15) . .
C4 C5 C6 120.9(2) . .
C4 C5 H5 119.54(16) . .
C9 C4 C5 120.0(2) . .
C3 C4 C5 120.2(2) . .
C3 C4 C9 119.8(2) . .
C10 C9 C4 119.4(2) . .
C8 C9 C4 117.4(2) . .
C8 C9 C10 123.2(2) . .
C11 C10 C9 121.2(2) . .
C1 C10 C9 119.6(2) . .
C1 C10 C11 119.2(2) . .
C10 C11 N1 123.9(2) . .
H11 C11 N1 118.07(14) . .
H11 C11 C10 118.07(13) . .
C17 C12 N1 118.0(2) . .
C13 C12 N1 122.6(2) . .
C13 C12 C17 119.4(2) . .
C12 C17 N2 117.7(2) . .
C16 C17 N2 123.0(2) . .
C16 C17 C12 119.3(2) . .
H18 C18 N2 118.73(13) . .
C19 C18 N2 122.5(2) . .
C19 C18 H18 118.73(12) . .
C20 C19 C18 121.1(2) . .
C28 C19 C18 120.3(2) . .
C28 C19 C20 118.6(2) . .
C25 C20 C19 119.0(2) . .
C21 C20 C19 123.3(2) . .
C21 C20 C25 117.7(2) . .
C24 C25 C20 119.4(2) . .
C26 C25 C20 119.4(2) . .
C26 C25 C24 121.2(2) . .
H24 C24 C25 119.51(17) . .
C23 C24 C25 121.0(3) . .
C23 C24 H24 119.51(17) . .
H23 C23 C24 120.14(17) . .
C22 C23 C24 119.7(3) . .
C22 C23 H23 120.14(16) . .
H3 C3 C4 119.28(13) . .
C2 C3 C4 121.4(2) . .
C2 C3 H3 119.28(17) . .
H2a C2 C3 118.99(17) . .
C1 C2 C3 122.0(3) . .
C1 C2 H2a 118.99(14) . .
C10 C1 O1 122.6(2) . .
C2 C1 O1 119.6(2) . .
C2 C1 C10 117.7(2) . .
H8 C8 C9 119.41(13) . .
C7 C8 C9 121.2(2) . .
C7 C8 H8 119.41(17) . .
C8 C7 C6 121.3(3) . .
H7 C7 C6 119.36(15) . .
H7 C7 C8 119.36(17) . .
H13 C13 C12 119.79(13) . .
C14 C13 C12 120.4(2) . .
C14 C13 H13 119.79(15) . .
H14 C14 C13 119.80(15) . .
C15 C14 C13 120.4(2) . .
C15 C14 H14 119.80(16) . .
H15 C15 C14 120.18(16) . .
C16 C15 C14 119.6(2) . .
C16 C15 H15 120.18(15) . .
C15 C16 C17 120.8(2) . .
H16 C16 C17 119.58(14) . .
H16 C16 C15 119.58(15) . .
H26 C26 C25 119.22(15) . .
C27 C26 C25 121.6(2) . .
C27 C26 H26 119.22(16) . .
H27 C27 C26 119.91(16) . .
C28 C27 C26 120.2(2) . .
C28 C27 H27 119.91(15) . .
C19 C28 O2 122.1(2) . .
C27 C28 O2 116.7(2) . .
C27 C28 C19 121.3(2) . .
H22 C22 C23 119.52(16) . .
C21 C22 C23 121.0(3) . .
C21 C22 H22 119.52(17) . .
C22 C21 C20 121.2(3) . .
H21 C21 C20 119.39(14) . .
H21 C21 C22 119.39(17) . .
Cl2 C29 Cl1 111.72(16) . .
H29a C29 Cl1 109.28(12) . .
H29a C29 Cl2 109.28(12) . .
H29b C29 Cl1 109.28(11) . .
H29b C29 Cl2 109.28(12) . .
H29b C29 H29a 107.9 . .

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2 N2 0.80(3) 1.82(3) 2.574(3) 156(3) .

_olex2_exptl_crystal_mounting_method 
'Single crystal was mounted on a glass fibre in Paratone-N oil for data collection.'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_UO2L
_database_code_depnum_ccdc_archive 'CCDC 1827293'
_audit_update_record             
;
2018-03-03 deposited with the CCDC.
2018-08-28 downloaded from the CCDC.
;
_audit_creation_date             2017-06-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C28 H20 N2 O5 U), 4(C H2 Cl2)'
_chemical_formula_sum            'C60 H48 Cl8 N4 O10 U2'
_chemical_formula_weight         1744.75
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cl 0.14873 0.16029 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55739974976
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
U -10.21189 10.40537 36.02280 23.41280 14.94910 4.18800 0.52930 3.32530
16.09270 100.61300 13.3965997696
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x-1/2,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   15.4659(12)
_cell_length_b                   19.3294(14)
_cell_length_c                   22.2346(16)
_cell_angle_alpha                90
_cell_angle_beta                 106.655(1)
_cell_angle_gamma                90
_cell_volume                     6368.1(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    180
_cell_measurement_theta_max      25.628
_cell_measurement_theta_min      2.183
_exptl_absorpt_coefficient_mu    5.476
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.3403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1471 before and 0.0559 after correction. The Ratio of minimum to maximum transmission is 0.4566. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.8197
_exptl_crystal_description       block
_exptl_crystal_F_000             3269.1361
_exptl_crystal_recrystallization_method 'Slow diffusion of Hex into DCM'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            74217
_diffrn_reflns_theta_full        25.7632
_diffrn_reflns_theta_max         25.76
_diffrn_reflns_theta_min         1.42
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.9970
_diffrn_measured_fraction_theta_max 0.9970
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -18
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              -12
_reflns_number_gt                9916
_reflns_number_total             12168
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.3260
_refine_diff_density_min         -1.9575
_refine_diff_density_rms         0.2631
_refine_ls_d_res_high            0.8176
_refine_ls_d_res_low             14.3146
_refine_ls_goodness_of_fit_ref   1.0941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    90
_refine_ls_number_parameters     759
_refine_ls_number_reflns         12168
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0440
_refine_ls_restrained_S_all      1.0941
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0179P)²+77.0629P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1031
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O4(H4a,H4b), O6(H6a,H6b)
2.b Secondary CH2 refined with riding coordinates:
 C0aa(H0aa,H0ab), C1aa(H1aa,H1ab), C2aa(H2aa,H2ab), C3aa(H3aa,H3ab)
2.c Aromatic/amide H refined with riding coordinates:
 C29(H29), C28(H28), C21(H21), C20(H20), C19(H19), C18(H18), C9(H9), C10(H10),
 C23(H23), C24(H24), C25(H25), C26(H26), C13(H13), C14(H14), C15(H15), C16(H16),
  C47(H47), C48(H48), C58(H58), C57(H57), C56(H56), C55(H55), C36(H36),
 C35(H35), C51(H51), C52(H52), C53(H53), C54(H54), C40(H40), C39(H39), C38(H38),
  C37(H37), C3(H3), C6(H6), C41(H41), C44(H44)
;
_atom_sites_solution_primary     dual
_atom_sites_special_details      
;
The structure was solved using Patterson Methods, followed by a Tangent Expansion (ShelXS). RE = 0.1, Nqual =  -1, Ralpha = 0.032
;
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_refinement_flags_posn
U1 U -0.080224(16) 1.093558(14) 0.055471(13) 0.01787(8) Uani 1.000000 .
U2 U -0.248341(17) 0.991497(14) -0.199178(13) 0.01985(8) Uani 1.000000 .
O1 O 0.0225(3) 1.0825(3) 0.0343(2) 0.0239(11) Uani 1.000000 .
O2 O -0.0326(3) 1.0031(3) 0.1230(2) 0.0235(11) Uani 1.000000 .
O3 O -0.1824(3) 1.1064(3) 0.0749(2) 0.0234(11) Uani 1.000000 .
O4 O -0.1513(3) 0.9961(3) -0.0083(2) 0.0240(11) Uani 1.000000 .
O5 O -0.1643(3) 1.0049(3) -0.2663(3) 0.0309(13) Uani 1.000000 .
O6 O -0.1256(3) 1.0646(3) -0.1350(2) 0.0235(11) Uani 1.000000 .
O8 O -0.3149(3) 1.0648(3) -0.2297(2) 0.0281(12) Uani 1.000000 .
N1 N -0.0053(4) 1.1368(3) 0.1634(3) 0.0222(14) Uani 1.000000 .
N2 N -0.0549(4) 1.2221(3) 0.0667(3) 0.0231(14) Uani 1.000000 .
N3 N -0.3892(4) 0.9209(3) -0.2061(3) 0.0242(14) Uani 1.000000 .
N4 N -0.3194(4) 0.9318(3) -0.3020(3) 0.0246(14) Uani 1.000000 .
C1 C -0.0595(4) 0.9919(4) 0.1739(4) 0.0250(17) Uani 1.000000 .
C2 C -0.0627(5) 1.0446(4) 0.2162(4) 0.0257(17) Uani 1.000000 .
C3 C -0.0182(5) 1.1103(4) 0.2133(4) 0.0269(18) Uani 1.000000 .
C4 C 0.0485(5) 1.1975(4) 0.1665(4) 0.0255(17) Uani 1.000000 .
C5 C 0.0234(5) 1.2422(4) 0.1155(4) 0.0270(17) Uani 1.000000 .
C6 C -0.1082(6) 1.2710(4) 0.0365(4) 0.0288(18) Uani 1.000000 .
C7 C -0.1882(5) 1.2597(4) -0.0146(4) 0.0259(17) Uani 1.000000 .
C8 C -0.1992(5) 1.1999(4) -0.0516(3) 0.0235(16) Uani 1.000000 .
C9 C -0.2736(5) 1.1942(4) -0.1059(4) 0.0273(17) Uani 1.000000 .
C10 C -0.3366(6) 1.2453(5) -0.1205(4) 0.0331(19) Uani 1.000000 .
C11 C -0.3300(6) 1.3061(4) -0.0848(4) 0.0338(19) Uani 1.000000 .
C12 C -0.2553(6) 1.3145(4) -0.0312(4) 0.033(2) Uani 1.000000 .
C13 C -0.2519(8) 1.3759(5) 0.0031(4) 0.049(3) Uani 1.000000 .
C14 C -0.3185(9) 1.4251(5) -0.0152(5) 0.063(3) Uani 1.000000 .
C15 C -0.3925(8) 1.4162(6) -0.0668(5) 0.060(3) Uani 1.000000 .
C16 C -0.3973(7) 1.3576(5) -0.1002(5) 0.048(3) Uani 1.000000 .
C18 C 0.0752(6) 1.3007(5) 0.1136(4) 0.039(2) Uani 1.000000 .
C19 C 0.1505(6) 1.3145(5) 0.1641(5) 0.044(2) Uani 1.000000 .
C20 C 0.1741(5) 1.2707(5) 0.2148(4) 0.037(2) Uani 1.000000 .
C21 C 0.1249(5) 1.2111(4) 0.2176(4) 0.0288(18) Uani 1.000000 .
C22 C -0.1007(5) 1.0309(5) 0.2667(4) 0.035(2) Uani 1.000000 .
C23 C -0.1199(6) 1.0840(6) 0.3044(5) 0.050(3) Uani 1.000000 .
C24 C -0.1625(9) 1.0693(7) 0.3502(6) 0.073(4) Uani 1.000000 .
C25 C -0.1895(10) 1.0017(8) 0.3579(6) 0.081(4) Uani 1.000000 .
C26 C -0.1719(9) 0.9489(7) 0.3222(6) 0.073(4) Uani 1.000000 .
C27 C -0.1287(6) 0.9629(5) 0.2754(4) 0.043(2) Uani 1.000000 .
C28 C -0.1162(6) 0.9100(5) 0.2345(4) 0.042(2) Uani 1.000000 .
C29 C -0.0849(5) 0.9233(4) 0.1846(4) 0.0313(19) Uani 1.000000 .
C31 C -0.3699(5) 1.0179(4) -0.0992(4) 0.0228(16) Uani 1.000000 .
C32 C -0.4516(5) 0.9862(4) -0.1345(4) 0.0245(17) Uani 1.000000 .
C33 C -0.5342(5) 1.0030(4) -0.1198(4) 0.0266(17) Uani 1.000000 .
C34 C -0.5328(5) 1.0493(4) -0.0707(4) 0.0294(18) Uani 1.000000 .
C35 C -0.4487(5) 1.0799(4) -0.0370(4) 0.0309(19) Uani 1.000000 .
C36 C -0.3715(5) 1.0646(4) -0.0503(4) 0.0283(18) Uani 1.000000 .
C37 C -0.6132(5) 1.0647(5) -0.0551(4) 0.034(2) Uani 1.000000 .
C38 C -0.6927(5) 1.0349(5) -0.0871(4) 0.037(2) Uani 1.000000 .
C39 C -0.6958(5) 0.9908(5) -0.1363(4) 0.037(2) Uani 1.000000 .
C40 C -0.6194(5) 0.9754(5) -0.1533(4) 0.032(2) Uani 1.000000 .
C41 C -0.4508(5) 0.9334(4) -0.1794(4) 0.0271(18) Uani 1.000000 .
C42 C -0.3998(5) 0.8625(4) -0.2468(4) 0.0278(18) Uani 1.000000 .
C43 C -0.3655(5) 0.8689(4) -0.2986(4) 0.0287(18) Uani 1.000000 .
C44 C -0.3206(5) 0.9561(5) -0.3565(4) 0.0318(19) Uani 1.000000 .
C45 C -0.2687(5) 1.0127(5) -0.3681(4) 0.0313(19) Uani 1.000000 .
C46 C -0.1880(5) 1.0315(4) -0.3232(4) 0.0289(18) Uani 1.000000 .
C47 C -0.1277(6) 1.0788(5) -0.3396(4) 0.039(2) Uani 1.000000 .
C48 C -0.1508(7) 1.1086(5) -0.3978(5) 0.047(2) Uani 1.000000 .
C49 C -0.2327(7) 1.0933(5) -0.4437(5) 0.045(2) Uani 1.000000 .
C50 C -0.2932(6) 1.0458(5) -0.4293(4) 0.040(2) Uani 1.000000 .
C51 C -0.3749(7) 1.0335(6) -0.4752(5) 0.056(3) Uani 1.000000 .
C52 C -0.3943(8) 1.0660(7) -0.5323(5) 0.065(3) Uani 1.000000 .
C53 C -0.3349(9) 1.1123(6) -0.5467(6) 0.069(3) Uani 1.000000 .
C54 C -0.2569(8) 1.1266(6) -0.5030(5) 0.060(3) Uani 1.000000 .
C55 C -0.3752(6) 0.8141(5) -0.3405(4) 0.037(2) Uani 1.000000 .
C56 C -0.4192(6) 0.7540(5) -0.3330(5) 0.045(2) Uani 1.000000 .
C57 C -0.4510(7) 0.7474(5) -0.2807(5) 0.050(3) Uani 1.000000 .
C58 C -0.4416(6) 0.8010(5) -0.2377(4) 0.039(2) Uani 1.000000 .
O0aa O -0.2919(3) 1.0028(3) -0.1085(2) 0.0262(12) Uani 1.000000 .
O1aa O -0.1408(3) 1.1481(3) -0.0385(2) 0.0236(11) Uani 1.000000 .
Cl7 Cl -0.7846(4) 1.2606(3) -0.1649(3) 0.160(2) Uani 1.000000 .
Cl8 Cl -0.5953(4) 1.2463(3) -0.1023(4) 0.182(3) Uani 1.000000 .
Cl9 Cl -0.5981(4) 1.1775(3) -0.2822(4) 0.182(3) Uani 1.000000 .
Cl10 Cl -0.5554(4) 1.0499(4) -0.3289(3) 0.163(2) Uani 1.000000 .
C0aa C -0.5254(10) 1.1112(9) -0.2679(8) 0.107(6) Uani 1.000000 .
C1aa C -0.6978(16) 1.2067(10) -0.1402(14) 0.240(17) Uani 1.000000 .
O3aa O -0.1847(3) 0.9173(3) -0.1669(3) 0.0287(12) Uani 1.000000 .
Cl1 Cl -0.1475(4) 0.8048(3) 0.0197(2) 0.1269(18) Uani 1.000000 .
Cl2 Cl -0.3313(4) 0.8092(2) -0.0611(2) 0.1151(16) Uani 1.000000 .
Cl6 Cl -0.3014(7) 1.2149(4) 0.1825(3) 0.224(4) Uani 1.000000 .
Cl0a Cl -0.4357(5) 1.2405(4) 0.0754(4) 0.252(5) Uani 1.000000 .
C2aa C -0.3113(19) 1.2262(13) 0.1074(11) 0.249(17) Uani 1.000000 .
C3aa C -0.2137(12) 0.8081(8) -0.0540(8) 0.114(6) Uani 1.000000 .
H29 H -0.0800(5) 0.8870(4) 0.1569(4) 0.038(2) Uiso 1.000000 R
H28 H -0.1301(6) 0.8636(5) 0.2424(4) 0.050(3) Uiso 1.000000 R
H21 H 0.1421(5) 1.1808(4) 0.2526(4) 0.035(2) Uiso 1.000000 R
H20 H 0.2255(5) 1.2813(5) 0.2489(4) 0.045(3) Uiso 1.000000 R
H19 H 0.1858(6) 1.3546(5) 0.1635(5) 0.052(3) Uiso 1.000000 R
H18 H 0.0594(6) 1.3308(5) 0.0783(4) 0.047(3) Uiso 1.000000 R
H9 H -0.2797(5) 1.1547(4) -0.1321(4) 0.033(2) Uiso 1.000000 R
H10 H -0.3871(6) 1.2397(5) -0.1564(4) 0.040(2) Uiso 1.000000 R
H23 H -0.1035(6) 1.1303(6) 0.2985(5) 0.060(3) Uiso 1.000000 R
H24 H -0.1733(9) 1.1052(7) 0.3763(6) 0.087(4) Uiso 1.000000 R
H25 H -0.2204(10) 0.9923(8) 0.3883(6) 0.097(5) Uiso 1.000000 R
H26 H -0.1886(9) 0.9028(7) 0.3288(6) 0.087(4) Uiso 1.000000 R
H13 H -0.2029(8) 1.3835(5) 0.0396(4) 0.058(3) Uiso 1.000000 R
H14 H -0.3133(9) 1.4667(5) 0.0083(5) 0.075(4) Uiso 1.000000 R
H15 H -0.4386(8) 1.4503(6) -0.0782(5) 0.072(4) Uiso 1.000000 R
H16 H -0.4481(7) 1.3506(5) -0.1357(5) 0.058(3) Uiso 1.000000 R
H47 H -0.0715(6) 1.0896(5) -0.3102(4) 0.046(3) Uiso 1.000000 R
H48 H -0.1104(7) 1.1407(5) -0.4077(5) 0.056(3) Uiso 1.000000 R
H58 H -0.4636(6) 0.7958(5) -0.2022(4) 0.047(3) Uiso 1.000000 R
H57 H -0.4795(7) 0.7056(5) -0.2744(5) 0.060(3) Uiso 1.000000 R
H56 H -0.4276(6) 0.7178(5) -0.3630(5) 0.054(3) Uiso 1.000000 R
H55 H -0.3509(6) 0.8181(5) -0.3750(4) 0.045(3) Uiso 1.000000 R
H36 H -0.3167(5) 1.0854(4) -0.0264(4) 0.034(2) Uiso 1.000000 R
H35 H -0.4475(5) 1.1119(4) -0.0043(4) 0.037(2) Uiso 1.000000 R
H51 H -0.4174(7) 1.0023(6) -0.4668(5) 0.068(3) Uiso 1.000000 R
H52 H -0.4500(8) 1.0565(7) -0.5629(5) 0.078(4) Uiso 1.000000 R
H53 H -0.3491(9) 1.1337(6) -0.5868(6) 0.083(4) Uiso 1.000000 R
H54 H -0.2170(8) 1.1597(6) -0.5121(5) 0.071(4) Uiso 1.000000 R
H40 H -0.6236(5) 0.9457(5) -0.1880(4) 0.039(2) Uiso 1.000000 R
H39 H -0.7518(5) 0.9708(5) -0.1589(4) 0.044(3) Uiso 1.000000 R
H38 H -0.7461(5) 1.0445(5) -0.0756(4) 0.044(3) Uiso 1.000000 R
H37 H -0.6116(5) 1.0962(5) -0.0220(4) 0.040(2) Uiso 1.000000 R
H4a H -0.2096(4) 1.0015(16) -0.019(2) 0.0360(17) Uiso 1.000000 GR
H4b H -0.137(3) 0.9583(4) 0.0135(10) 0.0360(17) Uiso 1.000000 GR
H6a H -0.1436(14) 1.085(2) -0.1059(18) 0.0353(17) Uiso 1.000000 GR
H6b H -0.0791(14) 1.0387(5) -0.118(2) 0.0353(17) Uiso 1.000000 GR
H3 H 0.0030(5) 1.1357(4) 0.2513(4) 0.032(2) Uiso 1.000000 R
H6 H -0.0930(6) 1.3174(4) 0.0492(4) 0.035(2) Uiso 1.000000 R
H41 H -0.5022(5) 0.9040(4) -0.1908(4) 0.032(2) Uiso 1.000000 R
H44 H -0.3598(5) 0.9340(5) -0.3921(4) 0.038(2) Uiso 1.000000 R
H0aa H -0.4637(10) 1.1286(9) -0.2639(8) 0.129(7) Uiso 1.000000 R
H0ab H -0.5251(10) 1.0889(9) -0.2278(8) 0.129(7) Uiso 1.000000 R
H1aa H -0.7122(16) 1.1728(10) -0.1111(14) 0.29(2) Uiso 1.000000 R
H1ab H -0.6905(16) 1.1808(10) -0.1768(14) 0.29(2) Uiso 1.000000 R
H2aa H -0.2766(19) 1.2669(13) 0.1004(11) 0.30(2) Uiso 1.000000 R
H2ab H -0.2916(19) 1.1847(13) 0.0888(11) 0.30(2) Uiso 1.000000 R
H3aa H -0.1984(12) 0.8501(8) -0.0743(8) 0.137(7) Uiso 1.000000 R
H3ab H -0.2005(12) 0.7675(8) -0.0771(8) 0.137(7) Uiso 1.000000 R


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 1.795(5) . ?
U1 O2 2.285(5) . ?
U1 O3 1.771(5) . ?
U1 O4 2.424(5) . ?
U1 N1 2.491(6) . ?
U1 N2 2.516(6) . ?
U1 O1aa 2.288(5) . ?
U2 O5 2.259(5) . ?
U2 O6 2.466(5) . ?
U2 O8 1.769(5) . ?
U2 N3 2.538(6) . ?
U2 N4 2.515(6) . ?
U2 O0aa 2.311(5) . ?
U2 O3aa 1.771(5) . ?
O2 C1 1.330(9) . ?
O4 H4a 0.8700 . ?
O4 H4b 0.8700 . ?
O5 C46 1.315(10) . ?
O6 H6a 0.8700 . ?
O6 H6b 0.8700 . ?
N1 C3 1.290(10) . ?
N1 C4 1.428(9) . ?
N2 C5 1.428(10) . ?
N2 C6 1.307(10) . ?
N3 C41 1.282(9) . ?
N3 C42 1.425(10) . ?
N4 C43 1.424(10) . ?
N4 C44 1.294(10) . ?
C1 C2 1.397(11) . ?
C1 C29 1.422(11) . ?
C2 C3 1.454(11) . ?
C2 C22 1.433(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(11) . ?
C4 C21 1.409(10) . ?
C5 C18 1.396(11) . ?
C6 C7 1.437(11) . ?
C6 H6 0.9500 . ?
C7 C8 1.400(11) . ?
C7 C12 1.455(11) . ?
C8 C9 1.412(10) . ?
C8 O1aa 1.324(9) . ?
C9 C10 1.360(11) . ?
C9 H9 0.9500 . ?
C10 C11 1.404(12) . ?
C10 H10 0.9500 . ?
C11 C12 1.411(12) . ?
C11 C16 1.410(12) . ?
C12 C13 1.404(12) . ?
C13 C14 1.376(14) . ?
C13 H13 0.9500 . ?
C14 C15 1.379(15) . ?
C14 H14 0.9500 . ?
C15 C16 1.346(14) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C18 C19 1.393(12) . ?
C18 H18 0.9500 . ?
C19 C20 1.373(13) . ?
C19 H19 0.9500 . ?
C20 C21 1.392(12) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.408(13) . ?
C22 C27 1.414(13) . ?
C23 C24 1.393(14) . ?
C23 H23 0.9500 . ?
C24 C25 1.396(17) . ?
C24 H24 0.9500 . ?
C25 C26 1.368(18) . ?
C25 H25 0.9500 . ?
C26 C27 1.415(14) . ?
C26 H26 0.9500 . ?
C27 C28 1.418(14) . ?
C28 C29 1.357(12) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C31 C32 1.420(10) . ?
C31 C36 1.419(11) . ?
C31 O0aa 1.315(8) . ?
C32 C33 1.445(10) . ?
C32 C41 1.431(11) . ?
C33 C34 1.407(11) . ?
C33 C40 1.418(10) . ?
C34 C35 1.430(11) . ?
C34 C37 1.415(11) . ?
C35 C36 1.344(11) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C38 1.360(12) . ?
C37 H37 0.9500 . ?
C38 C39 1.377(13) . ?
C38 H38 0.9500 . ?
C39 C40 1.373(11) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 H41 0.9500 . ?
C42 C43 1.404(11) . ?
C42 C58 1.396(11) . ?
C43 C55 1.390(11) . ?
C44 C45 1.424(12) . ?
C44 H44 0.9500 . ?
C45 C46 1.403(11) . ?
C45 C50 1.452(12) . ?
C46 C47 1.428(11) . ?
C47 C48 1.366(13) . ?
C47 H47 0.9500 . ?
C48 C49 1.411(14) . ?
C48 H48 0.9500 . ?
C49 C50 1.412(13) . ?
C49 C54 1.418(14) . ?
C50 C51 1.399(13) . ?
C51 C52 1.370(14) . ?
C51 H51 0.9500 . ?
C52 C53 1.384(16) . ?
C52 H52 0.9500 . ?
C53 C54 1.342(16) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C55 C56 1.380(13) . ?
C55 H55 0.9500 . ?
C56 C57 1.392(13) . ?
C56 H56 0.9500 . ?
C57 C58 1.389(12) . ?
C57 H57 0.9500 . ?
C58 H58 0.9500 . ?
Cl7 C1aa 1.66(2) . ?
Cl8 C1aa 1.74(2) . ?
Cl9 C0aa 1.675(16) . ?
Cl10 C0aa 1.760(19) . ?
C0aa H0aa 0.9900 . ?
C0aa H0ab 0.9900 . ?
C1aa H1aa 0.9900 . ?
C1aa H1ab 0.9900 . ?
Cl1 C3aa 1.665(19) . ?
Cl2 C3aa 1.781(17) . ?
Cl6 C2aa 1.65(2) . ?
Cl0a C2aa 1.87(3) . ?
C2aa H2aa 0.9900 . ?
C2aa H2ab 0.9900 . ?
C3aa H3aa 0.9900 . ?
C3aa H3ab 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
O2 U1 O1 86.4(2) . . ?
O3 U1 O1 178.5(2) . . ?
O3 U1 O2 95.1(2) . . ?
O4 U1 O1 92.4(2) . . ?
O4 U1 O2 78.29(17) . . ?
O4 U1 O3 88.0(2) . . ?
N1 U1 O1 95.2(2) . . ?
N1 U1 O2 69.53(19) . . ?
N1 U1 O3 85.3(2) . . ?
N1 U1 O4 146.34(19) . . ?
N2 U1 O1 91.1(2) . . ?
N2 U1 O2 132.69(19) . . ?
N2 U1 O3 87.8(2) . . ?
N2 U1 O4 148.99(19) . . ?
N2 U1 N1 63.7(2) . . ?
O1aa U1 O1 88.7(2) . . ?
O1aa U1 O2 157.47(18) . . ?
O1aa U1 O3 89.9(2) . . ?
O1aa U1 O4 79.95(17) . . ?
O1aa U1 N1 132.88(19) . . ?
O1aa U1 N2 69.34(19) . . ?
O6 U2 O5 79.84(18) . . ?
O8 U2 O5 92.0(2) . . ?
O8 U2 O6 91.7(2) . . ?
N3 U2 O5 131.93(19) . . ?
N3 U2 O6 148.02(18) . . ?
N3 U2 O8 90.7(2) . . ?
N4 U2 O5 68.63(19) . . ?
N4 U2 O6 148.43(19) . . ?
N4 U2 O8 87.9(2) . . ?
N4 U2 N3 63.5(2) . . ?
O0aa U2 O5 158.85(18) . . ?
O0aa U2 O6 79.01(17) . . ?
O0aa U2 O8 88.7(2) . . ?
O0aa U2 N3 69.17(18) . . ?
O0aa U2 N4 132.51(18) . . ?
O3aa U2 O5 90.1(2) . . ?
O3aa U2 O6 89.0(2) . . ?
O3aa U2 O8 177.8(2) . . ?
O3aa U2 N3 87.5(2) . . ?
O3aa U2 N4 92.5(2) . . ?
O3aa U2 O0aa 89.5(2) . . ?
C1 O2 U1 124.3(4) . . ?
H4a O4 U1 109.3 . . ?
H4b O4 U1 109.2 . . ?
H4b O4 H4a 109.5 . . ?
C46 O5 U2 128.7(5) . . ?
H6a O6 U2 109.6 . . ?
H6b O6 U2 109.2 . . ?
H6b O6 H6a 109.5 . . ?
C3 N1 U1 123.5(5) . . ?
C4 N1 U1 115.3(5) . . ?
C4 N1 C3 121.1(6) . . ?
C5 N2 U1 114.7(5) . . ?
C6 N2 U1 127.3(5) . . ?
C6 N2 C5 117.8(6) . . ?
C41 N3 U2 127.5(5) . . ?
C42 N3 U2 113.9(4) . . ?
C42 N3 C41 118.5(6) . . ?
C43 N4 U2 115.9(5) . . ?
C44 N4 U2 124.8(5) . . ?
C44 N4 C43 119.2(7) . . ?
C2 C1 O2 122.2(7) . . ?
C29 C1 O2 117.6(7) . . ?
C29 C1 C2 120.1(7) . . ?
C3 C2 C1 119.9(7) . . ?
C22 C2 C1 119.7(7) . . ?
C22 C2 C3 120.0(7) . . ?
C2 C3 N1 125.2(7) . . ?
H3 C3 N1 117.4(4) . . ?
H3 C3 C2 117.4(4) . . ?
C5 C4 N1 116.5(7) . . ?
C21 C4 N1 122.4(7) . . ?
C21 C4 C5 121.1(7) . . ?
C4 C5 N2 115.4(7) . . ?
C18 C5 N2 124.5(7) . . ?
C18 C5 C4 120.0(7) . . ?
C7 C6 N2 124.8(7) . . ?
H6 C6 N2 117.6(4) . . ?
H6 C6 C7 117.6(4) . . ?
C8 C7 C6 121.5(7) . . ?
C12 C7 C6 118.7(7) . . ?
C12 C7 C8 119.6(7) . . ?
C9 C8 C7 119.9(7) . . ?
O1aa C8 C7 122.3(7) . . ?
O1aa C8 C9 117.8(7) . . ?
C10 C9 C8 120.0(8) . . ?
H9 C9 C8 120.0(5) . . ?
H9 C9 C10 120.0(5) . . ?
C11 C10 C9 122.8(8) . . ?
H10 C10 C9 118.6(5) . . ?
H10 C10 C11 118.6(5) . . ?
C12 C11 C10 118.8(7) . . ?
C16 C11 C10 121.7(8) . . ?
C16 C11 C12 119.5(8) . . ?
C11 C12 C7 118.8(7) . . ?
C13 C12 C7 124.4(8) . . ?
C13 C12 C11 116.8(8) . . ?
C14 C13 C12 121.0(10) . . ?
H13 C13 C12 119.5(6) . . ?
H13 C13 C14 119.5(6) . . ?
C15 C14 C13 122.2(10) . . ?
H14 C14 C13 118.9(6) . . ?
H14 C14 C15 118.9(6) . . ?
C16 C15 C14 117.8(9) . . ?
H15 C15 C14 121.1(6) . . ?
H15 C15 C16 121.1(6) . . ?
C15 C16 C11 122.7(10) . . ?
H16 C16 C11 118.6(6) . . ?
H16 C16 C15 118.6(6) . . ?
C19 C18 C5 119.0(9) . . ?
H18 C18 C5 120.5(5) . . ?
H18 C18 C19 120.5(6) . . ?
C20 C19 C18 120.6(8) . . ?
H19 C19 C18 119.7(6) . . ?
H19 C19 C20 119.7(5) . . ?
C21 C20 C19 121.8(8) . . ?
H20 C20 C19 119.1(5) . . ?
H20 C20 C21 119.1(5) . . ?
C20 C21 C4 117.5(8) . . ?
H21 C21 C4 121.3(5) . . ?
H21 C21 C20 121.3(5) . . ?
C23 C22 C2 122.4(8) . . ?
C27 C22 C2 119.2(8) . . ?
C27 C22 C23 118.1(8) . . ?
C24 C23 C22 120.7(11) . . ?
H23 C23 C22 119.6(6) . . ?
H23 C23 C24 119.6(7) . . ?
C25 C24 C23 120.1(11) . . ?
H24 C24 C23 120.0(7) . . ?
H24 C24 C25 120.0(7) . . ?
C26 C25 C24 120.7(11) . . ?
H25 C25 C24 119.6(7) . . ?
H25 C25 C26 119.6(7) . . ?
C27 C26 C25 119.9(11) . . ?
H26 C26 C25 120.1(7) . . ?
H26 C26 C27 120.1(7) . . ?
C26 C27 C22 120.4(10) . . ?
C28 C27 C22 118.7(8) . . ?
C28 C27 C26 120.8(10) . . ?
C29 C28 C27 122.2(8) . . ?
H28 C28 C27 118.9(5) . . ?
H28 C28 C29 118.9(6) . . ?
C28 C29 C1 119.6(8) . . ?
H29 C29 C1 120.2(5) . . ?
H29 C29 C28 120.2(6) . . ?
C36 C31 C32 119.4(6) . . ?
O0aa C31 C32 121.9(7) . . ?
O0aa C31 C36 118.7(6) . . ?
C33 C32 C31 118.8(7) . . ?
C41 C32 C31 120.7(7) . . ?
C41 C32 C33 120.2(7) . . ?
C34 C33 C32 120.1(7) . . ?
C40 C33 C32 123.1(7) . . ?
C40 C33 C34 116.9(7) . . ?
C35 C34 C33 118.6(7) . . ?
C37 C34 C33 120.3(7) . . ?
C37 C34 C35 121.0(8) . . ?
C36 C35 C34 121.8(7) . . ?
H35 C35 C34 119.1(5) . . ?
H35 C35 C36 119.1(5) . . ?
C35 C36 C31 121.3(7) . . ?
H36 C36 C31 119.3(4) . . ?
H36 C36 C35 119.3(5) . . ?
C38 C37 C34 120.6(8) . . ?
H37 C37 C34 119.7(5) . . ?
H37 C37 C38 119.7(5) . . ?
C39 C38 C37 119.9(8) . . ?
H38 C38 C37 120.0(5) . . ?
H38 C38 C39 120.0(5) . . ?
C40 C39 C38 121.1(8) . . ?
H39 C39 C38 119.5(5) . . ?
H39 C39 C40 119.5(5) . . ?
C39 C40 C33 121.2(8) . . ?
H40 C40 C33 119.4(5) . . ?
H40 C40 C39 119.4(5) . . ?
C32 C41 N3 127.9(7) . . ?
H41 C41 N3 116.1(4) . . ?
H41 C41 C32 116.1(4) . . ?
C43 C42 N3 116.7(7) . . ?
C58 C42 N3 123.8(7) . . ?
C58 C42 C43 119.5(7) . . ?
C42 C43 N4 115.6(7) . . ?
C55 C43 N4 125.0(7) . . ?
C55 C43 C42 119.4(8) . . ?
C45 C44 N4 126.2(7) . . ?
H44 C44 N4 116.9(5) . . ?
H44 C44 C45 116.9(5) . . ?
C46 C45 C44 120.1(8) . . ?
C50 C45 C44 119.9(7) . . ?
C50 C45 C46 119.5(8) . . ?
C45 C46 O5 122.0(7) . . ?
C47 C46 O5 118.2(7) . . ?
C47 C46 C45 119.7(8) . . ?
C48 C47 C46 120.0(8) . . ?
H47 C47 C46 120.0(5) . . ?
H47 C47 C48 120.0(5) . . ?
C49 C48 C47 122.3(9) . . ?
H48 C48 C47 118.9(5) . . ?
H48 C48 C49 118.9(6) . . ?
C50 C49 C48 119.1(9) . . ?
C54 C49 C48 121.4(9) . . ?
C54 C49 C50 119.4(9) . . ?
C49 C50 C45 119.2(8) . . ?
C51 C50 C45 123.2(9) . . ?
C51 C50 C49 117.6(9) . . ?
C52 C51 C50 120.7(10) . . ?
H51 C51 C50 119.6(6) . . ?
H51 C51 C52 119.6(7) . . ?
C53 C52 C51 121.8(11) . . ?
H52 C52 C51 119.1(7) . . ?
H52 C52 C53 119.1(7) . . ?
C54 C53 C52 119.0(11) . . ?
H53 C53 C52 120.5(7) . . ?
H53 C53 C54 120.5(7) . . ?
C53 C54 C49 121.5(10) . . ?
H54 C54 C49 119.3(6) . . ?
H54 C54 C53 119.3(7) . . ?
C56 C55 C43 121.4(8) . . ?
H55 C55 C43 119.3(5) . . ?
H55 C55 C56 119.3(5) . . ?
C57 C56 C55 118.9(8) . . ?
H56 C56 C55 120.6(5) . . ?
H56 C56 C57 120.6(5) . . ?
C58 C57 C56 121.0(9) . . ?
H57 C57 C56 119.5(5) . . ?
H57 C57 C58 119.5(6) . . ?
C57 C58 C42 119.8(8) . . ?
H58 C58 C42 120.1(5) . . ?
H58 C58 C57 120.1(6) . . ?
C31 O0aa U2 132.0(5) . . ?
C8 O1aa U1 128.6(4) . . ?
Cl10 C0aa Cl9 110.8(9) . . ?
H0aa C0aa Cl9 109.5(6) . . ?
H0aa C0aa Cl10 109.5(6) . . ?
H0ab C0aa Cl9 109.5(6) . . ?
H0ab C0aa Cl10 109.5(6) . . ?
H0ab C0aa H0aa 108.05934308(2) . . ?
Cl8 C1aa Cl7 114.9(12) . . ?
H1aa C1aa Cl7 108.5(11) . . ?
H1aa C1aa Cl8 108.5(9) . . ?
H1ab C1aa Cl7 108.5(11) . . ?
H1ab C1aa Cl8 108.5(12) . . ?
H1ab C1aa H1aa 107.53233615(3) . . ?
Cl0a C2aa Cl6 101.1(9) . . ?
H2aa C2aa Cl6 111.6(12) . . ?
H2aa C2aa Cl0a 111.6(8) . . ?
H2ab C2aa Cl6 111.6(7) . . ?
H2ab C2aa Cl0a 111.6(9) . . ?
H2ab C2aa H2aa 109.36178(8) . . ?
Cl2 C3aa Cl1 114.3(8) . . ?
H3aa C3aa Cl1 108.7(5) . . ?
H3aa C3aa Cl2 108.7(5) . . ?
H3ab C3aa Cl1 108.7(6) . . ?
H3ab C3aa Cl2 108.7(6) . . ?
H3ab C3aa H3aa 107.6 . . ?

_olex2_exptl_crystal_mounting_method 
'a suitable crystal as selected and mounted on a glass fiber usnig paratone-n oil'
_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT971_UO2L                
;
PROBLEM: Check Calcd Residual Density  0.84A From      U2       2.68 eA-3  
RESPONSE: This residual density is close to a uranium atom, and
is not uncommon in structures containing actinide atoms.
;
_vrf_PLAT974_UO2L                
;
PROBLEM: Check Calcd Negative Residual Density on      U1      -1.51 eA-3  
RESPONSE: This negative residual density is close to a uranium atom, and
is not uncommon in structures containing actinide atoms.
;
# end Validation Reply Form
