# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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. 
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data_i222_a
_database_code_depnum_ccdc_archive 'CCDC 1960645'
loop_
_audit_author_name
_audit_author_address
'Yingjie Zhang' ANSTO
_audit_update_record             
;
2019-10-22 deposited with the CCDC.	2019-12-03 downloaded from the CCDC.
;
_audit_creation_date             2019-08-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C60 H60 Cl4 N40 O41 Th4), 6(Cl)'
_chemical_formula_sum            'C30 H30 Cl8 N20 O20.50 Th2'
_chemical_formula_weight         1746.42
_chemical_melting_point          ?
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'
Th Th -7.2400 8.8979 '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      orthorhombic
_space_group_IT_number           71
_space_group_name_H-M_alt        'I m m m'
_space_group_name_Hall           '-I 2 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   10.812(2)
_cell_length_b                   21.943(4)
_cell_length_c                   30.221(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7170(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.996
_cell_measurement_theta_min      1.147
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.510
_exptl_absorpt_correction_T_max  0.4359
_exptl_absorpt_correction_T_min  0.2867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1359 before and 0.0873 after correction.
The Ratio of minimum to maximum transmission is 0.6577.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3320
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            44391
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.147
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           
'silicon double crystal monochromated synchrotron'
_diffrn_source                   'Australian Synchrotron MX2'
_diffrn_measurement_device_type  'Eiga Detector'
_diffrn_measurement_method       'π  scans'
_diffrn_radiation_wavelength     0.7108
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3097
_reflns_number_total             3491
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'BlueIce (McPhillips, et al., 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.417
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.205
_refine_ls_extinction_coef       0.00162(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3491
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0578
_refine_ls_restrained_S_all      1.049
_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)+(0.1238P)²+81.3311P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1766
_refine_ls_wR_factor_ref         0.1821
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O4) = Uanis(O5) = Uanis(O6) = Uanis(O10) = Uanis(O9)
3. Others
 Fixed Sof: Th1(0.25) Th2(0.25) O4(0.25) O5(0.125) O6(0.25) O8(0.5) O9(0.25)
 O10(0.25) Cl5(0.075) Cl3(0.175)
4.a Ternary CH refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C11(H11)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C5(H5A,H5B), C9(H9A,H9B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Th1 Th 0.5000 0.90809(3) 0.33741(2) 0.0232(3) Uani 0.5 2 d S T P . .
Th2 Th 0.5000 0.76344(3) 0.39770(2) 0.0244(3) Uani 0.5 2 d S T P . .
Cl1 Cl 0.5000 0.79103(11) 0.30776(8) 0.0312(5) Uani 1 2 d S T P . .
O1 O 0.2845(5) 0.9048(2) 0.3165(2) 0.0427(14) Uani 1 1 d . . . . .
O2 O 0.2857(4) 0.7371(2) 0.38277(17) 0.0347(11) Uani 1 1 d . . . . .
O3 O 0.2819(6) 0.6721(3) 0.5000 0.0331(15) Uani 1 2 d S T P . .
O4 O 0.5000 0.9149(8) 0.2531(5) 0.0467(19) Uani 0.5 2 d S T P . .
O5 O 0.5000 1.0000 0.3057(7) 0.0467(19) Uani 0.5 4 d S T P . .
O6 O 0.6356(14) 1.0000 0.3771(5) 0.0467(19) Uani 0.5 2 d S T P . .
O7 O 0.6289(6) 0.8559(3) 0.39412(18) 0.0517(15) Uani 1 1 d . . . . .
O8 O 0.6254(12) 0.7787(6) 0.4647(3) 0.052(3) Uani 0.5 1 d . . . . .
O9 O 0.5000 0.6700(8) 0.4435(5) 0.0467(19) Uani 0.5 2 d S T P . .
O10 O 0.5000 0.6631(8) 0.3540(5) 0.0467(19) Uani 0.5 2 d S T P . .
N1 N 0.1125(4) 0.9452(2) 0.28330(17) 0.0219(11) Uani 1 1 d . . . . .
N2 N 0.1128(4) 0.8467(2) 0.30047(17) 0.0226(11) Uani 1 1 d . . . . .
N3 N 0.1123(5) 0.7505(2) 0.33927(17) 0.0223(11) Uani 1 1 d . . . . .
N4 N 0.1125(5) 0.6776(2) 0.39006(16) 0.0224(11) Uani 1 1 d . . . . .
N5 N 0.1128(5) 0.6340(2) 0.46350(17) 0.0251(11) Uani 1 1 d . . . . .
C1 C 0.1711(8) 1.0000 0.2672(3) 0.0239(18) Uani 1 2 d S T P . .
H1A H 0.1688 1.0000 0.2351 0.029 Uiso 1 2 calc RS T P . .
H1B H 0.2572 1.0000 0.2762 0.029 Uiso 1 2 calc RS T P . .
C2 C 0.1792(6) 0.8988(3) 0.3015(2) 0.0252(13) Uani 1 1 d . . . . .
C3 C 0.0000 0.9224(4) 0.2627(3) 0.0183(16) Uani 1 2 d S T P . .
H3 H 0.0000 0.9285 0.2305 0.022 Uiso 1 2 calc RS T P . .
C4 C 0.0000 0.8537(4) 0.2753(3) 0.0179(16) Uani 1 2 d S T P . .
H4 H 0.0000 0.8276 0.2490 0.022 Uiso 1 2 calc RS T P . .
C5 C 0.1706(5) 0.7870(3) 0.3047(2) 0.0242(13) Uani 1 1 d . . . . .
H5A H 0.2576 0.7921 0.3115 0.029 Uiso 1 1 calc R . . . .
H5B H 0.1644 0.7656 0.2767 0.029 Uiso 1 1 calc R . . . .
C6 C 0.1804(6) 0.7230(3) 0.3718(2) 0.0238(13) Uani 1 1 d . . . . .
C7 C 0.0000 0.7159(4) 0.3301(3) 0.0193(17) Uani 1 2 d S T P . .
H7 H 0.0000 0.6987 0.3002 0.023 Uiso 1 2 calc RS T P . .
C8 C 0.0000 0.6664(4) 0.3659(3) 0.0190(17) Uani 1 2 d S T P . .
H8 H 0.0000 0.6255 0.3528 0.023 Uiso 1 2 calc RS T P . .
C9 C 0.1668(5) 0.6327(3) 0.41984(19) 0.0232(13) Uani 1 1 d . . . . .
H9A H 0.1557 0.5924 0.4073 0.028 Uiso 1 1 calc R . . . .
H9B H 0.2549 0.6402 0.4222 0.028 Uiso 1 1 calc R . . . .
C10 C 0.1803(8) 0.6493(4) 0.5000 0.0247(18) Uani 1 2 d S T P . .
C11 C 0.0000 0.6025(4) 0.4746(3) 0.0225(18) Uani 1 2 d S T P . .
H11 H 0.0000 0.5609 0.4628 0.027 Uiso 1 2 calc RS T P . .
Cl5 Cl 0.256(3) 0.5000 0.3531(6) 0.074(8) Uani 0.15 2 d S T P . .
Cl4 Cl 0.2420(7) 0.5000 0.5000 0.095(2) Uani 1 4 d S T P . .
Cl2 Cl 0.2497(3) 0.62617(12) 0.29847(8) 0.0685(7) Uani 1 1 d . . . . .
Cl3 Cl 0.0000 0.5000 0.3722(3) 0.082(2) Uani 0.7 4 d S T P . .


_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
Th1 Th1 4.0333(15) 2_675 ?
Th1 Th2 3.6599(11) . ?
Th1 Cl1 2.720(3) . ?
Th1 O1 2.415(5) 12_655 ?
Th1 O1 2.415(5) . ?
Th1 O4 2.553(15) . ?
Th1 O5 2.232(9) . ?
Th1 O6 2.767(11) 2_675 ?
Th1 O6 2.767(11) . ?
Th1 O7 2.488(6) . ?
Th1 O7 2.488(6) 12_655 ?
Th2 Cl1 2.785(3) . ?
Th2 O2 2.430(5) 12_655 ?
Th2 O2 2.430(5) . ?
Th2 O7 2.464(6) 12_655 ?
Th2 O7 2.464(6) . ?
Th2 O8 2.459(11) . ?
Th2 O8 2.459(11) 12_655 ?
Th2 O9 2.475(17) . ?
Th2 O10 2.568(17) . ?
O1 C2 1.233(8) . ?
O2 C6 1.225(8) . ?
O3 C10 1.208(11) . ?
O5 Th1 2.232(9) 2_675 ?
O6 Th1 2.767(10) 2_675 ?
N1 C1 1.443(7) . ?
N1 C2 1.364(8) . ?
N1 C3 1.456(6) . ?
N2 C2 1.349(8) . ?
N2 C4 1.445(6) . ?
N2 C5 1.458(7) . ?
N3 C5 1.459(8) . ?
N3 C6 1.368(8) . ?
N3 C7 1.459(7) . ?
N4 C6 1.354(8) . ?
N4 C8 1.440(6) . ?
N4 C9 1.459(7) . ?
N5 C9 1.443(7) . ?
N5 C10 1.365(7) . ?
N5 C11 1.441(7) . ?
C1 N1 1.443(7) 11_575 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C3 N1 1.456(7) 12 ?
C3 H3 0.9800 . ?
C3 C4 1.556(11) . ?
C4 N2 1.445(6) 12 ?
C4 H4 0.9800 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C7 N3 1.459(7) 12 ?
C7 H7 0.9800 . ?
C7 C8 1.535(11) . ?
C8 N4 1.440(6) 12 ?
C8 H8 0.9800 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N5 1.364(7) 10_556 ?
C11 N5 1.441(7) 12 ?
C11 C11 1.536(16) 10_556 ?
C11 H11 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Th2 Th1 Th1 150.140(17) . 2_675 ?
Cl1 Th1 Th1 160.77(5) . 2_675 ?
Cl1 Th1 Th2 49.09(5) . . ?
Cl1 Th1 O6 146.2(3) . 2_675 ?
Cl1 Th1 O6 146.2(3) . . ?
O1 Th1 Th1 91.72(11) . 2_675 ?
O1 Th1 Th1 91.72(11) 12_655 2_675 ?
O1 Th1 Th2 95.98(11) 12_655 . ?
O1 Th1 Th2 95.98(11) . . ?
O1 Th1 Cl1 83.43(12) . . ?
O1 Th1 Cl1 83.43(12) 12_655 . ?
O1 Th1 O1 149.5(3) . 12_655 ?
O1 Th1 O4 74.97(15) . . ?
O1 Th1 O4 74.98(15) 12_655 . ?
O1 Th1 O6 130.3(3) 12_655 2_675 ?
O1 Th1 O6 67.9(3) 12_655 . ?
O1 Th1 O6 67.9(3) . 2_675 ?
O1 Th1 O6 130.3(3) . . ?
O1 Th1 O7 134.97(19) . . ?
O1 Th1 O7 68.0(2) . 12_655 ?
O1 Th1 O7 134.97(19) 12_655 12_655 ?
O1 Th1 O7 68.0(2) 12_655 . ?
O4 Th1 Th1 86.7(4) . 2_675 ?
O4 Th1 Th2 123.2(4) . . ?
O4 Th1 Cl1 74.1(4) . . ?
O4 Th1 O6 113.0(4) . 2_675 ?
O4 Th1 O6 113.0(4) . . ?
O5 Th1 Th1 25.4(5) . 2_675 ?
O5 Th1 Th2 175.5(5) . . ?
O5 Th1 Cl1 135.4(5) . . ?
O5 Th1 O1 85.12(17) . . ?
O5 Th1 O1 85.12(17) . 12_655 ?
O5 Th1 O4 61.3(6) . . ?
O5 Th1 O6 61.8(5) . 2_675 ?
O5 Th1 O6 61.8(5) . . ?
O5 Th1 O7 135.3(3) . . ?
O5 Th1 O7 135.3(3) . 12_655 ?
O6 Th1 Th1 43.2(2) . 2_675 ?
O6 Th1 Th1 43.2(2) 2_675 2_675 ?
O6 Th1 Th2 114.6(2) 2_675 . ?
O6 Th1 Th2 114.6(2) . . ?
O6 Th1 O6 64.0(6) 2_675 . ?
O7 Th1 Th1 117.39(14) . 2_675 ?
O7 Th1 Th1 117.39(14) 12_655 2_675 ?
O7 Th1 Th2 42.10(15) . . ?
O7 Th1 Th2 42.10(15) 12_655 . ?
O7 Th1 Cl1 78.03(15) . . ?
O7 Th1 Cl1 78.03(15) 12_655 . ?
O7 Th1 O4 135.6(3) 12_655 . ?
O7 Th1 O4 135.6(3) . . ?
O7 Th1 O6 74.9(3) . . ?
O7 Th1 O6 109.5(3) . 2_675 ?
O7 Th1 O6 74.9(3) 12_655 2_675 ?
O7 Th1 O6 109.5(3) 12_655 . ?
O7 Th1 O7 68.1(3) 12_655 . ?
Cl1 Th2 Th1 47.59(5) . . ?
O2 Th2 Th1 96.53(11) . . ?
O2 Th2 Th1 96.53(11) 12_655 . ?
O2 Th2 Cl1 82.55(12) . . ?
O2 Th2 Cl1 82.55(12) 12_655 . ?
O2 Th2 O2 144.9(3) 12_655 . ?
O2 Th2 O7 136.61(19) 12_655 12_655 ?
O2 Th2 O7 136.61(19) . . ?
O2 Th2 O7 69.4(2) 12_655 . ?
O2 Th2 O7 69.42(19) . 12_655 ?
O2 Th2 O8 70.1(3) . 12_655 ?
O2 Th2 O8 135.3(3) 12_655 12_655 ?
O2 Th2 O8 135.3(3) . . ?
O2 Th2 O8 70.1(3) 12_655 . ?
O2 Th2 O9 84.66(16) . . ?
O2 Th2 O9 84.66(16) 12_655 . ?
O2 Th2 O10 72.58(13) 12_655 . ?
O2 Th2 O10 72.58(13) . . ?
O7 Th2 Th1 42.59(14) 12_655 . ?
O7 Th2 Th1 42.59(14) . . ?
O7 Th2 Cl1 77.18(13) 12_655 . ?
O7 Th2 Cl1 77.18(13) . . ?
O7 Th2 O7 68.9(3) 12_655 . ?
O7 Th2 O9 135.0(3) . . ?
O7 Th2 O9 135.0(3) 12_655 . ?
O7 Th2 O10 133.1(3) 12_655 . ?
O7 Th2 O10 133.1(3) . . ?
O8 Th2 Th1 107.0(3) 12_655 . ?
O8 Th2 Th1 107.0(3) . . ?
O8 Th2 Cl1 140.7(3) 12_655 . ?
O8 Th2 Cl1 140.7(3) . . ?
O8 Th2 O7 67.2(3) . . ?
O8 Th2 O7 103.7(4) . 12_655 ?
O8 Th2 O7 103.7(4) 12_655 . ?
O8 Th2 O7 67.2(3) 12_655 12_655 ?
O8 Th2 O8 66.9(6) . 12_655 ?
O8 Th2 O9 69.6(4) . . ?
O8 Th2 O9 69.6(4) 12_655 . ?
O8 Th2 O10 122.7(4) 12_655 . ?
O8 Th2 O10 122.7(4) . . ?
O9 Th2 Th1 175.8(4) . . ?
O9 Th2 Cl1 136.6(4) . . ?
O9 Th2 O10 65.0(5) . . ?
O10 Th2 Th1 119.2(3) . . ?
O10 Th2 Cl1 71.6(3) . . ?
Th1 Cl1 Th2 83.33(7) . . ?
C2 O1 Th1 172.1(6) . . ?
C6 O2 Th2 174.9(5) . . ?
Th1 O5 Th1 129.2(10) . 2_675 ?
Th1 O6 Th1 93.6(5) . 2_675 ?
Th2 O7 Th1 95.3(2) . . ?
C1 N1 C3 120.6(6) . . ?
C2 N1 C1 121.8(6) . . ?
C2 N1 C3 110.9(5) . . ?
C2 N2 C4 111.8(5) . . ?
C2 N2 C5 122.1(5) . . ?
C4 N2 C5 120.1(5) . . ?
C6 N3 C5 121.6(5) . . ?
C6 N3 C7 110.8(5) . . ?
C7 N3 C5 120.5(6) . . ?
C6 N4 C8 112.2(5) . . ?
C6 N4 C9 122.0(5) . . ?
C8 N4 C9 122.4(5) . . ?
C10 N5 C9 121.8(5) . . ?
C10 N5 C11 112.5(6) . . ?
C11 N5 C9 123.0(6) . . ?
N1 C1 N1 112.8(7) . 11_575 ?
N1 C1 H1A 109.0 . . ?
N1 C1 H1A 109.0 11_575 . ?
N1 C1 H1B 109.0 11_575 . ?
N1 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
O1 C2 N1 123.8(6) . . ?
O1 C2 N2 126.1(6) . . ?
N2 C2 N1 110.0(5) . . ?
N1 C3 N1 113.3(7) 12 . ?
N1 C3 H3 112.2 12 . ?
N1 C3 H3 112.2 . . ?
N1 C3 C4 103.2(5) 12 . ?
N1 C3 C4 103.2(5) . . ?
C4 C3 H3 112.2 . . ?
N2 C4 N2 115.2(7) 12 . ?
N2 C4 C3 103.4(4) 12 . ?
N2 C4 C3 103.4(4) . . ?
N2 C4 H4 111.4 12 . ?
N2 C4 H4 111.4 . . ?
C3 C4 H4 111.4 . . ?
N2 C5 N3 111.8(5) . . ?
N2 C5 H5A 109.3 . . ?
N2 C5 H5B 109.3 . . ?
N3 C5 H5A 109.3 . . ?
N3 C5 H5B 109.3 . . ?
H5A C5 H5B 107.9 . . ?
O2 C6 N3 125.6(6) . . ?
O2 C6 N4 125.4(6) . . ?
N4 C6 N3 109.0(5) . . ?
N3 C7 N3 112.7(7) 12 . ?
N3 C7 H7 112.1 . . ?
N3 C7 H7 112.1 12 . ?
N3 C7 C8 103.5(5) 12 . ?
N3 C7 C8 103.5(5) . . ?
C8 C7 H7 112.1 . . ?
N4 C8 N4 115.3(7) . 12 ?
N4 C8 C7 103.7(4) 12 . ?
N4 C8 C7 103.7(4) . . ?
N4 C8 H8 111.2 . . ?
N4 C8 H8 111.2 12 . ?
C7 C8 H8 111.2 . . ?
N4 C9 H9A 109.0 . . ?
N4 C9 H9B 109.0 . . ?
N5 C9 N4 112.8(5) . . ?
N5 C9 H9A 109.0 . . ?
N5 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
O3 C10 N5 126.1(4) . . ?
O3 C10 N5 126.1(4) . 10_556 ?
N5 C10 N5 107.9(8) 10_556 . ?
N5 C11 N5 115.6(7) . 12 ?
N5 C11 C11 103.4(4) . 10_556 ?
N5 C11 C11 103.4(4) 12 10_556 ?
N5 C11 H11 111.3 12 . ?
N5 C11 H11 111.3 . . ?
C11 C11 H11 111.3 10_556 . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 120.4 53.8 ?
2 -0.956 0.000 0.500 690.8 204.3 ?
3 -0.549 0.500 0.000 690.8 204.3 ?
4 0.500 0.500 0.500 120.4 53.8 ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT975_i222_a              
;
PROBLEM: Check Calcd Resid. Dens.  1.01A   From O4              3.51 eA-3  
RESPONSE: The alert arises due to the oxygen atom disorders.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p1
_database_code_depnum_ccdc_archive 'CCDC 1960646'
loop_
_audit_author_name
_audit_author_address
'Yingjie Zhang' ANSTO
_audit_update_record             
;
2019-10-22 deposited with the CCDC.	2019-12-03 downloaded from the CCDC.
;
_audit_creation_date             2019-08-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.5(Cl3 H4 O4 U), 0.5(Cl H6 O6 U), 0.5(Cl), 0.5(C60 H60 N40 O20), O'
_chemical_formula_sum            'C30 H36 Cl2.50 N20 O16 U'
_chemical_formula_weight         1259.44
_chemical_melting_point          ?
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      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                   17.212(3)
_cell_length_b                   19.456(4)
_cell_length_c                   21.391(4)
_cell_angle_alpha                66.03(3)
_cell_angle_beta                 86.24(3)
_cell_angle_gamma                72.18(3)
_cell_volume                     6217(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      1.203
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.784
_exptl_absorpt_correction_T_max  0.4345
_exptl_absorpt_correction_T_min  0.1584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1834 before and 0.0991 after correction.
The Ratio of minimum to maximum transmission is 0.3646.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2474
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1027
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_Laue_measured_fraction_full 0.933
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            67008
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.203
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_radiation_type           
'silicon double crystal monochromated synchrotron'
_diffrn_source                   'Australian Synchrotron MX2'
_diffrn_measurement_device_type  'Eiga Detector'
_diffrn_measurement_method       'π  scans'
_diffrn_radiation_wavelength     0.71078
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13870
_reflns_number_total             20452
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'BlueIce (McPhillips, et al., 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.880
_refine_diff_density_min         -1.689
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1221
_refine_ls_number_reflns         20452
_refine_ls_number_restraints     1350
_refine_ls_R_factor_all          0.1206
_refine_ls_R_factor_gt           0.1056
_refine_ls_restrained_S_all      1.028
_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)+(0.2000P)²+5.8580P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3066
_refine_ls_wR_factor_ref         0.3225
_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 O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O1W) = Uanis(O2W) = Uanis(O6W) = Uanis(O5W) = Uanis(O4W) = Uanis(O3W) =
Uanis(O8W)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB), O6W(H6WA,H6WB)
4.b Ternary CH refined with riding coordinates:
 C4(H4), C5(H5), C10(H10), C11(H11), C15(H15), C16(H16), C21(H21), C22(H22),
 C28(H28), C29(H29), C33(H33), C34(H34), C39(H39), C40(H40), C45(H45), C46(H46),
  C51(H51), C52(H52), C57(H57), C58(H58)
4.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C7(H7A,H7B), C9(H9A,H9B), C13(H13A,H13B), C18(H18A,
 H18B), C19(H19A,H19B), C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B),
 C31(H31A,H31B), C36(H36A,H36B), C37(H37A,H37B), C42(H42A,H42B), C43(H43A,H43B),
  C48(H48A,H48B), C49(H49A,H49B), C54(H54A,H54B), C55(H55A,H55B), C60(H60A,H60B)
;
_atom_sites_solution_hydrogens   mixed
_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 0.83461(3) 0.36533(3) 0.03223(2) 0.0790(2) Uani 1 1 d . U . . .
Cl1 Cl 0.7321(2) 0.50790(19) 0.02337(19) 0.0992(9) Uani 1 1 d . U . . .
Cl2 Cl 0.6884(3) 0.3715(3) -0.0188(2) 0.1147(11) Uani 1 1 d . U . . .
Cl3 Cl 0.8619(3) 0.2188(2) 0.0274(2) 0.1120(11) Uani 1 1 d . U . . .
O1 O 0.8607(6) 0.4074(6) -0.0550(5) 0.103(2) Uani 1 1 d . U . . .
O1W O 0.9113(7) 0.4424(6) 0.0564(6) 0.1212(12) Uani 1 1 d . U . . .
H1WA H 0.8855 0.4969 0.0363 0.182 Uiso 1 1 d GR . . . .
H1WB H 0.9614 0.4391 0.0363 0.182 Uiso 1 1 d GR . . . .
O2 O 0.8093(4) 0.3213(4) 0.1203(3) 0.0750(17) Uani 1 1 d . U . . .
O2W O 0.9776(7) 0.2905(6) 0.0653(6) 0.1212(12) Uani 1 1 d . U . . .
H2WA H 0.9862 0.2421 0.0701 0.182 Uiso 1 1 d GR . . . .
H2WB H 0.9900 0.2854 0.1061 0.182 Uiso 1 1 d GR . . . .
U2 U 0.87197(5) 0.94470(3) -0.08304(3) 0.1203(3) Uani 1 1 d . U . . .
Cl4 Cl 0.9609(3) 0.8843(3) -0.1716(3) 0.1352(14) Uani 1 1 d . U . . .
O3 O 0.9111(9) 0.8579(7) -0.0093(7) 0.154(4) Uani 1 1 d . U . . .
O3W O 1.0178(7) 0.9488(6) -0.0813(6) 0.1212(12) Uani 1 1 d . U . . .
O4 O 0.8429(11) 1.0355(8) -0.1501(8) 0.173(5) Uani 1 1 d . U . . .
O4W O 0.8870(7) 1.0267(6) -0.0090(6) 0.1212(12) Uani 1 1 d . U . . .
H4WA H 0.8735 1.0154 0.0413 0.182 Uiso 1 1 d GR . . . .
H4WB H 0.9076 1.0754 -0.0256 0.182 Uiso 1 1 d GR . . . .
O5W O 0.7397(7) 0.9793(6) -0.0421(6) 0.1212(12) Uani 1 1 d . U . . .
H5WA H 0.7123 0.9436 -0.0062 0.182 Uiso 1 1 d GR . . . .
H5WB H 0.6981 1.0333 -0.0572 0.182 Uiso 1 1 d GR . . . .
O6W O 0.7901(7) 0.9082(6) -0.1298(6) 0.1212(12) Uani 1 1 d . U . . .
H6WA H 0.8047 0.9060 -0.1773 0.182 Uiso 1 1 d GR . . . .
H6WB H 0.7300 0.9473 -0.1471 0.182 Uiso 1 1 d GR . . . .
Cl5 Cl 0.90168(19) 0.6195(2) -0.0512(2) 0.1020(10) Uani 1 1 d . U . . .
O5 O 0.8569(5) 0.8350(5) 0.1775(5) 0.092(2) Uani 1 1 d . U . . .
O6 O 0.6964(6) 0.7132(5) 0.2148(5) 0.098(2) Uani 1 1 d . U . . .
O7 O 0.5872(5) 0.5695(5) 0.3617(5) 0.105(3) Uani 1 1 d . U . . .
O8 O 0.5943(5) 0.4471(5) 0.5677(5) 0.096(2) Uani 1 1 d . U . . .
O9 O 0.6907(5) 0.4173(5) 0.7276(6) 0.107(3) Uani 1 1 d . U . . .
O10 O 1.1173(5) 0.5257(4) 0.2080(5) 0.092(2) Uani 1 1 d . U . . .
O11 O 0.9496(5) 0.4202(4) 0.2147(5) 0.088(2) Uani 1 1 d . U . . .
O12 O 0.8526(4) 0.2861(4) 0.3442(4) 0.0774(18) Uani 1 1 d . U . . .
O13 O 0.8545(4) 0.1702(4) 0.5485(4) 0.085(2) Uani 1 1 d . U . . .
O14 O 0.9604(5) 0.1316(4) 0.7182(4) 0.0824(19) Uani 1 1 d . U . . .
N1 N 0.9906(5) 0.7811(5) 0.1598(5) 0.075(2) Uani 1 1 d . U . . .
N2 N 0.8950(6) 0.7403(5) 0.1332(5) 0.079(2) Uani 1 1 d . U . . .
N3 N 1.0942(5) 0.6603(5) 0.1683(5) 0.075(2) Uani 1 1 d . U . . .
N4 N 0.9993(6) 0.6181(5) 0.1458(5) 0.078(2) Uani 1 1 d . U . . .
N5 N 0.7922(6) 0.6731(5) 0.1497(6) 0.086(2) Uani 1 1 d . U . . .
N6 N 0.7151(6) 0.5975(6) 0.2005(6) 0.089(2) Uani 1 1 d . U . . .
N7 N 0.8959(6) 0.5535(5) 0.1507(6) 0.084(2) Uani 1 1 d . U . . .
N8 N 0.8110(6) 0.4847(5) 0.1896(5) 0.080(2) Uani 1 1 d . U . . .
N9 N 0.6487(5) 0.5125(5) 0.2893(6) 0.082(2) Uani 1 1 d . U . . .
N10 N 0.6157(6) 0.4362(5) 0.3899(6) 0.087(2) Uani 1 1 d . U . . .
N11 N 0.7499(5) 0.3998(5) 0.2787(5) 0.0757(19) Uani 1 1 d . U . . .
N12 N 0.7261(5) 0.3255(5) 0.3849(5) 0.0725(19) Uani 1 1 d . U . . .
N13 N 0.6199(6) 0.3613(5) 0.5111(5) 0.085(2) Uani 1 1 d . U . . .
N14 N 0.6452(5) 0.3128(5) 0.6252(6) 0.084(2) Uani 1 1 d . U . . .
N15 N 0.7226(5) 0.2490(5) 0.5047(5) 0.074(2) Uani 1 1 d . U . . .
N16 N 0.7533(5) 0.2013(5) 0.6175(5) 0.081(2) Uani 1 1 d . U . . .
N17 N 0.7104(5) 0.2931(5) 0.7295(5) 0.078(2) Uani 1 1 d . U . . .
N18 N 0.7986(5) 0.3087(5) 0.7889(5) 0.078(2) Uani 1 1 d . U . . .
N19 N 0.8197(5) 0.1870(5) 0.7205(5) 0.076(2) Uani 1 1 d . U . . .
N20 N 0.9049(6) 0.1929(5) 0.7899(6) 0.084(2) Uani 1 1 d . U . . .
C1 C 1.0225(7) 0.8421(6) 0.1645(7) 0.085(3) Uani 1 1 d . U . . .
H1A H 1.0348 0.8745 0.1192 0.102 Uiso 1 1 calc R . . . .
H1B H 0.9806 0.8761 0.1808 0.102 Uiso 1 1 calc R . . . .
C2 C 0.9073(7) 0.7908(6) 0.1593(6) 0.076(2) Uani 1 1 d . U . . .
C3 C 0.8120(7) 0.7476(7) 0.1163(7) 0.089(3) Uani 1 1 d . U . . .
H3A H 0.8039 0.7661 0.0670 0.106 Uiso 1 1 calc R . . . .
H3B H 0.7745 0.7870 0.1298 0.106 Uiso 1 1 calc R . . . .
C4 C 1.0337(7) 0.7325(6) 0.1240(6) 0.075(2) Uani 1 1 d . U . . .
H4 H 1.0568 0.7625 0.0825 0.091 Uiso 1 1 calc R . . . .
C5 C 0.9656(7) 0.7026(6) 0.1072(6) 0.077(2) Uani 1 1 d . U . . .
H5 H 0.9581 0.7169 0.0580 0.092 Uiso 1 1 calc R . . . .
C6 C 1.0747(7) 0.5947(6) 0.1757(6) 0.078(2) Uani 1 1 d . U . . .
C7 C 0.9739(8) 0.5669(7) 0.1207(7) 0.089(3) Uani 1 1 d . U . . .
H7A H 1.0165 0.5166 0.1335 0.107 Uiso 1 1 calc R . . . .
H7B H 0.9660 0.5919 0.0710 0.107 Uiso 1 1 calc R . . . .
C8 C 0.7312(7) 0.6683(6) 0.1911(7) 0.080(2) Uani 1 1 d . U . . .
C9 C 0.6364(7) 0.5852(7) 0.2282(7) 0.092(3) Uani 1 1 d . U . . .
H9A H 0.6056 0.6295 0.2390 0.110 Uiso 1 1 calc R . . . .
H9B H 0.6043 0.5839 0.1933 0.110 Uiso 1 1 calc R . . . .
C10 C 0.8136(7) 0.6116(7) 0.1221(7) 0.085(3) Uani 1 1 d . U . . .
H10 H 0.8081 0.6340 0.0719 0.102 Uiso 1 1 calc R . . . .
C11 C 0.7582(7) 0.5626(6) 0.1544(7) 0.081(2) Uani 1 1 d . U . . .
H11 H 0.7205 0.5656 0.1202 0.097 Uiso 1 1 calc R . . . .
C12 C 0.8915(7) 0.4794(6) 0.1884(6) 0.079(2) Uani 1 1 d . U . . .
C13 C 0.7873(7) 0.4130(6) 0.2148(7) 0.083(3) Uani 1 1 d . U . . .
H13A H 0.7493 0.4169 0.1811 0.099 Uiso 1 1 calc R . . . .
H13B H 0.8354 0.3683 0.2206 0.099 Uiso 1 1 calc R . . . .
C14 C 0.6143(7) 0.5136(6) 0.3474(7) 0.085(3) Uani 1 1 d . U . . .
C15 C 0.6640(6) 0.4377(6) 0.2859(7) 0.078(2) Uani 1 1 d . U . . .
H15 H 0.6281 0.4416 0.2501 0.093 Uiso 1 1 calc R . . . .
C16 C 0.6470(6) 0.3827(6) 0.3575(6) 0.079(2) Uani 1 1 d . U . . .
H16 H 0.6069 0.3574 0.3546 0.095 Uiso 1 1 calc R . . . .
C17 C 0.7822(6) 0.3315(6) 0.3385(6) 0.075(2) Uani 1 1 d . U . . .
C18 C 0.5687(7) 0.4170(7) 0.4482(7) 0.087(3) Uani 1 1 d . U . . .
H18A H 0.5293 0.3940 0.4407 0.105 Uiso 1 1 calc R . . . .
H18B H 0.5384 0.4649 0.4538 0.105 Uiso 1 1 calc R . . . .
C19 C 0.7322(7) 0.2490(6) 0.4380(6) 0.081(2) Uani 1 1 d . U . . .
H19A H 0.6908 0.2299 0.4280 0.097 Uiso 1 1 calc R . . . .
H19B H 0.7853 0.2126 0.4378 0.097 Uiso 1 1 calc R . . . .
C20 C 0.6175(7) 0.3807(7) 0.5691(7) 0.089(3) Uani 1 1 d . U . . .
C21 C 0.6446(7) 0.2783(6) 0.5331(6) 0.082(2) Uani 1 1 d . U . . .
H21 H 0.6014 0.2607 0.5228 0.098 Uiso 1 1 calc R . . . .
C22 C 0.6651(7) 0.2451(6) 0.6078(7) 0.082(2) Uani 1 1 d . U . . .
H22 H 0.6330 0.2099 0.6330 0.098 Uiso 1 1 calc R . . . .
C23 C 0.7848(7) 0.2031(6) 0.5568(6) 0.075(2) Uani 1 1 d . U . . .
C24 C 0.6343(7) 0.3092(7) 0.6954(7) 0.089(3) Uani 1 1 d . U . . .
H24A H 0.5975 0.3592 0.6933 0.106 Uiso 1 1 calc R . . . .
H24B H 0.6097 0.2683 0.7214 0.106 Uiso 1 1 calc R . . . .
C25 C 0.7975(7) 0.1445(6) 0.6832(6) 0.082(3) Uani 1 1 d . U . . .
H25A H 0.8468 0.1090 0.6754 0.098 Uiso 1 1 calc R . . . .
H25B H 0.7636 0.1131 0.7109 0.098 Uiso 1 1 calc R . . . .
C26 C 0.7280(7) 0.3466(7) 0.7470(7) 0.082(3) Uani 1 1 d . U . . .
C27 C 0.8185(7) 0.3423(8) 0.8357(9) 0.103(4) Uani 1 1 d . U . . .
H27A H 0.7839 0.3965 0.8223 0.123 Uiso 1 1 calc R . . . .
H27B H 0.8084 0.3119 0.8825 0.123 Uiso 1 1 calc R . . . .
C28 C 0.7658(6) 0.2142(6) 0.7639(6) 0.078(2) Uani 1 1 d . U . . .
H28 H 0.7369 0.1765 0.7909 0.093 Uiso 1 1 calc R . . . .
C29 C 0.8242(6) 0.2244(6) 0.8102(7) 0.079(2) Uani 1 1 d . U . . .
H29 H 0.8183 0.1963 0.8591 0.095 Uiso 1 1 calc R . . . .
C30 C 0.9028(7) 0.1643(6) 0.7409(6) 0.075(2) Uani 1 1 d . U . . .
O7W O 0.4978(4) 0.8363(5) 0.0860(5) 0.093(2) Uani 1 1 d . U . . .
O8W O 0.5889(7) 0.7072(6) 0.0389(6) 0.1212(12) Uani 1 1 d . U . . .
O15 O 0.2134(5) 0.1721(5) 0.2029(5) 0.090(2) Uani 1 1 d . U . . .
O16 O 0.4454(5) 0.1434(5) 0.1420(5) 0.094(2) Uani 1 1 d . U . . .
O17 O 0.6865(5) 0.0207(5) 0.1752(5) 0.091(2) Uani 1 1 d . U . . .
O18 O 0.8444(5) -0.1544(4) 0.3262(4) 0.0839(19) Uani 1 1 d . U . . .
O19 O 0.8535(6) -0.3096(5) 0.5214(5) 0.096(2) Uani 1 1 d . U . . .
O20 O 0.2764(5) 0.3980(5) 0.3121(4) 0.087(2) Uani 1 1 d . U . . .
O21 O 0.4887(4) 0.3914(4) 0.2304(4) 0.0776(18) Uani 1 1 d . U . . .
O22 O 0.7078(4) 0.2541(4) 0.2899(4) 0.0785(18) Uani 1 1 d . U . . .
O23 O 0.8585(5) 0.0767(4) 0.4418(4) 0.091(2) Uani 1 1 d . U . . .
O24 O 0.9129(6) -0.0915(4) 0.6398(4) 0.091(2) Uani 1 1 d . U . . .
N21 N 0.1431(5) 0.2736(5) 0.2355(5) 0.0731(19) Uani 1 1 d . U . . .
N22 N 0.2500(5) 0.2863(5) 0.1722(5) 0.0738(19) Uani 1 1 d . U . . .
N23 N 0.1760(5) 0.3545(5) 0.2852(5) 0.0735(19) Uani 1 1 d . U . . .
N24 N 0.2688(5) 0.3817(5) 0.2112(5) 0.0735(19) Uani 1 1 d . U . . .
N25 N 0.3843(5) 0.2729(5) 0.1292(5) 0.078(2) Uani 1 1 d . U . . .
N26 N 0.5196(5) 0.2296(5) 0.1228(5) 0.076(2) Uani 1 1 d . U . . .
N27 N 0.4039(5) 0.3715(5) 0.1641(5) 0.0714(19) Uani 1 1 d . U . . .
N28 N 0.5366(5) 0.3294(5) 0.1572(5) 0.0718(19) Uani 1 1 d . U . . .
N29 N 0.6630(5) 0.1533(5) 0.1485(5) 0.073(2) Uani 1 1 d . U . . .
N30 N 0.7813(5) 0.0685(5) 0.2016(5) 0.075(2) Uani 1 1 d . U . . .
N31 N 0.6760(5) 0.2480(4) 0.1899(4) 0.0669(18) Uani 1 1 d . U . . .
N32 N 0.7868(5) 0.1585(4) 0.2535(4) 0.0661(18) Uani 1 1 d . U . . .
N33 N 0.8703(5) -0.0379(5) 0.2991(5) 0.0721(19) Uani 1 1 d . U . . .
N34 N 0.9239(5) -0.1384(4) 0.3981(5) 0.0723(19) Uani 1 1 d . U . . .
N35 N 0.8831(5) 0.0544(4) 0.3453(5) 0.075(2) Uani 1 1 d . U . . .
N36 N 0.9321(5) -0.0455(5) 0.4451(5) 0.075(2) Uani 1 1 d . U . . .
N37 N 0.9403(6) -0.2377(5) 0.5145(5) 0.0763(19) Uani 1 1 d . U . . .
N38 N 0.9026(6) -0.3035(5) 0.6155(5) 0.078(2) Uani 1 1 d . U . . .
N39 N 0.9504(5) -0.1449(5) 0.5603(5) 0.0725(19) Uani 1 1 d . U . . .
N40 N 0.9341(5) -0.2230(5) 0.6657(5) 0.0712(19) Uani 1 1 d . U . . .
C31 C 0.0713(7) 0.2472(7) 0.2607(6) 0.077(2) Uani 1 1 d . U . . .
H31A H 0.0223 0.2899 0.2374 0.092 Uiso 1 1 calc R . . . .
H31B H 0.0735 0.2032 0.2494 0.092 Uiso 1 1 calc R . . . .
C32 C 0.2007(7) 0.2388(7) 0.2039(6) 0.078(2) Uani 1 1 d . U . . .
C33 C 0.1453(6) 0.3505(6) 0.2256(6) 0.069(2) Uani 1 1 d . U . . .
H33 H 0.0930 0.3914 0.2059 0.083 Uiso 1 1 calc R . . . .
C34 C 0.2161(6) 0.3640(6) 0.1767(6) 0.075(2) Uani 1 1 d . U . . .
H34 H 0.1956 0.4069 0.1317 0.090 Uiso 1 1 calc R . . . .
C35 C 0.2448(7) 0.3802(6) 0.2736(6) 0.077(2) Uani 1 1 d . U . . .
C36 C 0.3003(7) 0.2796(8) 0.1176(7) 0.084(3) Uani 1 1 d . U . . .
H36A H 0.2774 0.3257 0.0757 0.100 Uiso 1 1 calc R . . . .
H36B H 0.2987 0.2336 0.1111 0.100 Uiso 1 1 calc R . . . .
C37 C 0.3264(6) 0.4250(6) 0.1760(6) 0.076(2) Uani 1 1 d . U . . .
H37A H 0.3392 0.4499 0.2034 0.092 Uiso 1 1 calc R . . . .
H37B H 0.3008 0.4663 0.1323 0.092 Uiso 1 1 calc R . . . .
C38 C 0.4512(7) 0.2077(7) 0.1329(6) 0.079(2) Uani 1 1 d . U . . .
C39 C 0.4100(6) 0.3426(7) 0.1114(6) 0.077(2) Uani 1 1 d . U . . .
H39 H 0.3822 0.3848 0.0681 0.092 Uiso 1 1 calc R . . . .
C40 C 0.5037(6) 0.3123(6) 0.1047(6) 0.070(2) Uani 1 1 d . U . . .
H40 H 0.5198 0.3397 0.0587 0.085 Uiso 1 1 calc R . . . .
C41 C 0.4778(6) 0.3668(6) 0.1884(6) 0.072(2) Uani 1 1 d . U . . .
C42 C 0.5927(6) 0.1856(7) 0.0995(6) 0.077(3) Uani 1 1 d . U . . .
H42A H 0.5813 0.1428 0.0933 0.092 Uiso 1 1 calc R . . . .
H42B H 0.6055 0.2206 0.0555 0.092 Uiso 1 1 calc R . . . .
C43 C 0.6199(6) 0.3273(6) 0.1605(6) 0.077(3) Uani 1 1 d . U . . .
H43A H 0.6252 0.3554 0.1876 0.092 Uiso 1 1 calc R . . . .
H43B H 0.6348 0.3546 0.1145 0.092 Uiso 1 1 calc R . . . .
C44 C 0.7072(6) 0.0749(6) 0.1757(6) 0.075(2) Uani 1 1 d . U . . .
C45 C 0.7097(6) 0.2031(6) 0.1500(5) 0.069(2) Uani 1 1 d . U . . .
H45 H 0.7203 0.2366 0.1038 0.083 Uiso 1 1 calc R . . . .
C46 C 0.7908(6) 0.1425(5) 0.1931(5) 0.065(2) Uani 1 1 d . U . . .
H46 H 0.8392 0.1512 0.1682 0.079 Uiso 1 1 calc R . . . .
C47 C 0.7229(6) 0.2233(5) 0.2481(6) 0.069(2) Uani 1 1 d . U . . .
C48 C 0.8499(6) -0.0043(6) 0.2245(6) 0.073(2) Uani 1 1 d . U . . .
H48A H 0.8974 0.0063 0.2003 0.087 Uiso 1 1 calc R . . . .
H48B H 0.8364 -0.0429 0.2130 0.087 Uiso 1 1 calc R . . . .
C49 C 0.8615(6) 0.1359(5) 0.2939(6) 0.072(2) Uani 1 1 d . U . . .
H49A H 0.8553 0.1711 0.3168 0.087 Uiso 1 1 calc R . . . .
H49B H 0.9057 0.1419 0.2637 0.087 Uiso 1 1 calc R . . . .
C50 C 0.8777(6) -0.1156(6) 0.3403(6) 0.073(2) Uani 1 1 d . U . . .
C51 C 0.9256(6) -0.0108(5) 0.3246(5) 0.069(2) Uani 1 1 d . U . . .
H51 H 0.9684 0.0013 0.2934 0.083 Uiso 1 1 calc R . . . .
C52 C 0.9610(6) -0.0805(5) 0.3955(5) 0.071(2) Uani 1 1 d . U . . .
H52 H 1.0208 -0.1006 0.3979 0.085 Uiso 1 1 calc R . . . .
C53 C 0.8887(7) 0.0332(6) 0.4142(6) 0.078(3) Uani 1 1 d . U . . .
C54 C 0.9603(8) -0.2204(6) 0.4447(5) 0.078(3) Uani 1 1 d . U . . .
H54A H 0.9423 -0.2537 0.4290 0.093 Uiso 1 1 calc R . . . .
H54B H 1.0192 -0.2338 0.4430 0.093 Uiso 1 1 calc R . . . .
C55 C 0.9732(9) -0.0792(7) 0.5105(6) 0.090(3) Uani 1 1 d . U . . .
H55A H 0.9628 -0.0385 0.5279 0.108 Uiso 1 1 calc R . . . .
H55B H 1.0315 -0.0966 0.5056 0.108 Uiso 1 1 calc R . . . .
C56 C 0.8948(8) -0.2866(6) 0.5483(6) 0.080(2) Uani 1 1 d . U . . .
C57 C 0.9834(7) -0.2247(6) 0.5602(6) 0.075(2) Uani 1 1 d . U . . .
H57 H 1.0424 -0.2388 0.5544 0.090 Uiso 1 1 calc R . . . .
C58 C 0.9632(6) -0.2764(6) 0.6324(5) 0.071(2) Uani 1 1 d . U . . .
H58 H 1.0112 -0.3205 0.6579 0.085 Uiso 1 1 calc R . . . .
C59 C 0.9291(7) -0.1464(6) 0.6232(6) 0.074(2) Uani 1 1 d . U . . .
C60 C 0.8824(8) -0.3748(6) 0.6655(6) 0.081(3) Uani 1 1 d . U . . .
H60A H 0.8584 -0.3964 0.6409 0.097 Uiso 1 1 calc R . . . .
H60B H 0.9322 -0.4147 0.6906 0.097 Uiso 1 1 calc R . . . .


_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 Cl1 2.732(3) . ?
U1 Cl2 2.758(4) . ?
U1 Cl3 2.788(4) . ?
U1 O1 1.796(9) . ?
U1 O1W 2.487(12) . ?
U1 O2 1.811(7) . ?
U1 O2W 2.424(11) . ?
U2 Cl4 2.764(5) . ?
U2 O3 1.753(12) . ?
U2 O3W 2.539(12) . ?
U2 O4 1.710(14) . ?
U2 O4W 2.735(10) . ?
U2 O5W 2.383(11) . ?
U2 O6W 2.206(12) . ?
O5 C2 1.189(13) . ?
O6 C8 1.175(13) . ?
O7 C14 1.198(13) . ?
O8 C20 1.219(14) . ?
O9 C26 1.228(13) . ?
O10 C6 1.236(13) . ?
O11 C12 1.218(13) . ?
O12 C17 1.242(12) . ?
O13 C23 1.214(13) . ?
O14 C30 1.195(12) . ?
N1 C1 1.491(14) . ?
N1 C2 1.388(14) . ?
N1 C4 1.454(13) . ?
N2 C2 1.383(14) . ?
N2 C3 1.448(15) . ?
N2 C5 1.422(14) . ?
N3 C4 1.452(13) . ?
N3 C6 1.362(14) . ?
N3 C27 1.485(16) 2_766 ?
N4 C5 1.449(13) . ?
N4 C6 1.347(14) . ?
N4 C7 1.483(15) . ?
N5 C3 1.467(16) . ?
N5 C8 1.329(16) . ?
N5 C10 1.480(15) . ?
N6 C8 1.418(15) . ?
N6 C9 1.490(16) . ?
N6 C11 1.459(16) . ?
N7 C7 1.499(16) . ?
N7 C10 1.494(14) . ?
N7 C12 1.360(15) . ?
N8 C11 1.418(14) . ?
N8 C12 1.357(15) . ?
N8 C13 1.453(14) . ?
N9 C9 1.451(15) . ?
N9 C14 1.347(16) . ?
N9 C15 1.429(13) . ?
N10 C14 1.402(15) . ?
N10 C16 1.430(15) . ?
N10 C18 1.423(16) . ?
N11 C13 1.432(15) . ?
N11 C15 1.465(13) . ?
N11 C17 1.405(15) . ?
N12 C16 1.443(12) . ?
N12 C17 1.333(14) . ?
N12 C19 1.437(14) . ?
N13 C18 1.466(15) . ?
N13 C20 1.430(16) . ?
N13 C21 1.412(13) . ?
N14 C20 1.347(16) . ?
N14 C22 1.448(14) . ?
N14 C24 1.477(16) . ?
N15 C19 1.425(14) . ?
N15 C21 1.484(14) . ?
N15 C23 1.397(13) . ?
N16 C22 1.476(13) . ?
N16 C23 1.365(15) . ?
N16 C25 1.463(15) . ?
N17 C24 1.426(15) . ?
N17 C26 1.355(14) . ?
N17 C28 1.444(13) . ?
N18 C26 1.371(14) . ?
N18 C27 1.504(15) . ?
N18 C29 1.439(13) . ?
N19 C25 1.496(14) . ?
N19 C28 1.409(14) . ?
N19 C30 1.404(14) . ?
N20 C1 1.440(14) 2_766 ?
N20 C29 1.453(14) . ?
N20 C30 1.378(14) . ?
C1 N20 1.440(14) 2_766 ?
C4 C5 1.576(16) . ?
C10 C11 1.494(17) . ?
C15 C16 1.543(17) . ?
C21 C22 1.479(17) . ?
C27 N3 1.485(16) 2_766 ?
C28 C29 1.561(16) . ?
O15 C32 1.256(13) . ?
O16 C38 1.221(13) . ?
O17 C44 1.217(13) . ?
O18 C50 1.207(13) . ?
O19 C56 1.223(14) . ?
O20 C35 1.225(13) . ?
O21 C41 1.224(12) . ?
O22 C47 1.242(12) . ?
O23 C53 1.196(13) . ?
O24 C59 1.206(12) . ?
N21 C31 1.468(14) . ?
N21 C32 1.331(14) . ?
N21 C33 1.436(12) . ?
N22 C32 1.389(15) . ?
N22 C34 1.486(13) . ?
N22 C36 1.432(15) . ?
N23 C33 1.451(14) . ?
N23 C35 1.393(14) . ?
N23 C60 1.494(14) 2_656 ?
N24 C34 1.403(14) . ?
N24 C35 1.362(15) . ?
N24 C37 1.469(14) . ?
N25 C36 1.441(14) . ?
N25 C38 1.406(13) . ?
N25 C39 1.451(15) . ?
N26 C38 1.346(15) . ?
N26 C40 1.432(13) . ?
N26 C42 1.473(13) . ?
N27 C37 1.499(12) . ?
N27 C39 1.435(14) . ?
N27 C41 1.369(13) . ?
N28 C40 1.481(13) . ?
N28 C41 1.362(14) . ?
N28 C43 1.427(13) . ?
N29 C42 1.458(13) . ?
N29 C44 1.367(13) . ?
N29 C45 1.446(14) . ?
N30 C44 1.373(14) . ?
N30 C46 1.434(13) . ?
N30 C48 1.459(11) . ?
N31 C43 1.445(11) . ?
N31 C45 1.434(12) . ?
N31 C47 1.357(13) . ?
N32 C46 1.441(13) . ?
N32 C47 1.364(12) . ?
N32 C49 1.443(12) . ?
N33 C48 1.478(14) . ?
N33 C50 1.376(13) . ?
N33 C51 1.445(13) . ?
N34 C50 1.352(14) . ?
N34 C52 1.437(13) . ?
N34 C54 1.453(13) . ?
N35 C49 1.462(13) . ?
N35 C51 1.477(12) . ?
N35 C53 1.361(14) . ?
N36 C52 1.466(13) . ?
N36 C53 1.371(13) . ?
N36 C55 1.410(15) . ?
N37 C54 1.434(14) . ?
N37 C56 1.364(15) . ?
N37 C57 1.407(14) . ?
N38 C56 1.343(14) . ?
N38 C58 1.427(14) . ?
N38 C60 1.492(14) . ?
N39 C55 1.438(15) . ?
N39 C57 1.482(12) . ?
N39 C59 1.363(14) . ?
N40 C31 1.454(14) 2_656 ?
N40 C58 1.439(12) . ?
N40 C59 1.374(14) . ?
C31 N40 1.454(14) 2_656 ?
C33 C34 1.567(15) . ?
C39 C40 1.557(14) . ?
C45 C46 1.571(12) . ?
C51 C52 1.566(14) . ?
C57 C58 1.550(16) . ?
C60 N23 1.494(14) 2_656 ?

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
Cl1 U1 Cl2 76.99(12) . . ?
Cl1 U1 Cl3 151.13(12) . . ?
Cl2 U1 Cl3 74.59(14) . . ?
O1 U1 Cl1 92.2(3) . . ?
O1 U1 Cl2 87.5(3) . . ?
O1 U1 Cl3 91.6(3) . . ?
O1 U1 O1W 86.4(4) . . ?
O1 U1 O2 179.1(4) . . ?
O1 U1 O2W 89.1(4) . . ?
O1W U1 Cl1 69.0(3) . . ?
O1W U1 Cl2 145.2(3) . . ?
O1W U1 Cl3 139.8(3) . . ?
O2 U1 Cl1 88.8(2) . . ?
O2 U1 Cl2 92.6(2) . . ?
O2 U1 Cl3 87.6(2) . . ?
O2 U1 O1W 94.0(4) . . ?
O2 U1 O2W 90.3(4) . . ?
O2W U1 Cl1 137.0(3) . . ?
O2W U1 Cl2 146.0(3) . . ?
O2W U1 Cl3 71.7(3) . . ?
O2W U1 O1W 68.2(4) . . ?
O3 U2 Cl4 94.6(5) . . ?
O3 U2 O3W 82.0(6) . . ?
O3 U2 O4W 87.5(6) . . ?
O3 U2 O5W 94.7(5) . . ?
O3 U2 O6W 100.5(6) . . ?
O3W U2 Cl4 69.8(2) . . ?
O3W U2 O4W 69.7(3) . . ?
O4 U2 Cl4 88.4(6) . . ?
O4 U2 O3 170.9(8) . . ?
O4 U2 O3W 91.1(7) . . ?
O4 U2 O4W 84.6(6) . . ?
O4 U2 O5W 87.8(7) . . ?
O4 U2 O6W 88.5(7) . . ?
O4W U2 Cl4 138.7(3) . . ?
O5W U2 Cl4 144.5(3) . . ?
O5W U2 O3W 145.5(3) . . ?
O5W U2 O4W 75.9(4) . . ?
O6W U2 Cl4 72.4(3) . . ?
O6W U2 O3W 142.1(4) . . ?
O6W U2 O4W 147.7(4) . . ?
O6W U2 O5W 72.3(4) . . ?
C2 N1 C1 120.8(8) . . ?
C2 N1 C4 112.2(9) . . ?
C4 N1 C1 120.8(9) . . ?
C2 N2 C3 118.5(9) . . ?
C2 N2 C5 114.3(9) . . ?
C5 N2 C3 124.6(10) . . ?
C4 N3 C27 117.9(10) . 2_766 ?
C6 N3 C4 111.9(9) . . ?
C6 N3 C27 118.8(9) . 2_766 ?
C5 N4 C7 116.6(10) . . ?
C6 N4 C5 114.5(9) . . ?
C6 N4 C7 120.7(9) . . ?
C3 N5 C10 122.8(11) . . ?
C8 N5 C3 120.3(9) . . ?
C8 N5 C10 113.0(10) . . ?
C8 N6 C9 119.4(10) . . ?
C8 N6 C11 112.7(10) . . ?
C11 N6 C9 122.0(10) . . ?
C10 N7 C7 122.9(10) . . ?
C12 N7 C7 121.3(9) . . ?
C12 N7 C10 112.0(10) . . ?
C11 N8 C13 125.8(10) . . ?
C12 N8 C11 113.8(9) . . ?
C12 N8 C13 119.5(9) . . ?
C14 N9 C9 120.4(9) . . ?
C14 N9 C15 112.1(10) . . ?
C15 N9 C9 122.1(11) . . ?
C14 N10 C16 112.5(10) . . ?
C14 N10 C18 123.5(9) . . ?
C18 N10 C16 121.3(10) . . ?
C13 N11 C15 124.8(10) . . ?
C17 N11 C13 122.3(9) . . ?
C17 N11 C15 109.8(9) . . ?
C17 N12 C16 112.9(9) . . ?
C17 N12 C19 118.6(8) . . ?
C19 N12 C16 120.4(9) . . ?
C20 N13 C18 120.6(8) . . ?
C21 N13 C18 123.9(10) . . ?
C21 N13 C20 109.7(10) . . ?
C20 N14 C22 110.9(10) . . ?
C20 N14 C24 122.3(9) . . ?
C22 N14 C24 124.8(10) . . ?
C19 N15 C21 126.6(8) . . ?
C23 N15 C19 121.2(8) . . ?
C23 N15 C21 110.7(9) . . ?
C23 N16 C22 111.2(9) . . ?
C23 N16 C25 121.3(9) . . ?
C25 N16 C22 125.4(10) . . ?
C24 N17 C28 122.9(9) . . ?
C26 N17 C24 122.5(9) . . ?
C26 N17 C28 112.7(9) . . ?
C26 N18 C27 120.2(8) . . ?
C26 N18 C29 113.0(9) . . ?
C29 N18 C27 119.3(10) . . ?
C28 N19 C25 121.8(10) . . ?
C30 N19 C25 116.2(8) . . ?
C30 N19 C28 114.2(9) . . ?
C1 N20 C29 122.9(10) 2_766 . ?
C30 N20 C1 117.4(9) . 2_766 ?
C30 N20 C29 112.9(9) . . ?
N20 C1 N1 112.0(8) 2_766 . ?
O5 C2 N1 125.8(11) . . ?
O5 C2 N2 127.4(11) . . ?
N2 C2 N1 106.8(9) . . ?
N2 C3 N5 113.2(9) . . ?
N1 C4 C5 103.2(9) . . ?
N3 C4 N1 112.9(9) . . ?
N3 C4 C5 103.7(8) . . ?
N2 C5 N4 115.3(10) . . ?
N2 C5 C4 102.8(8) . . ?
N4 C5 C4 101.0(8) . . ?
O10 C6 N3 125.5(11) . . ?
O10 C6 N4 126.0(11) . . ?
N4 C6 N3 108.3(9) . . ?
N4 C7 N7 110.3(10) . . ?
O6 C8 N5 127.7(11) . . ?
O6 C8 N6 126.3(12) . . ?
N5 C8 N6 106.0(10) . . ?
N9 C9 N6 112.4(9) . . ?
N5 C10 N7 111.2(10) . . ?
N5 C10 C11 105.0(10) . . ?
C11 C10 N7 102.0(9) . . ?
N6 C11 C10 102.5(9) . . ?
N8 C11 N6 112.9(10) . . ?
N8 C11 C10 105.1(9) . . ?
O11 C12 N7 125.7(11) . . ?
O11 C12 N8 127.6(11) . . ?
N7 C12 N8 106.7(9) . . ?
N11 C13 N8 111.8(9) . . ?
O7 C14 N9 127.5(12) . . ?
O7 C14 N10 125.0(13) . . ?
N9 C14 N10 107.6(9) . . ?
N9 C15 N11 114.2(9) . . ?
N9 C15 C16 104.8(10) . . ?
N11 C15 C16 103.7(8) . . ?
N10 C16 N12 115.7(10) . . ?
N10 C16 C15 102.3(9) . . ?
N12 C16 C15 103.6(9) . . ?
O12 C17 N11 122.7(11) . . ?
O12 C17 N12 128.0(11) . . ?
N12 C17 N11 109.3(8) . . ?
N10 C18 N13 112.1(9) . . ?
N15 C19 N12 113.4(9) . . ?
O8 C20 N13 125.8(12) . . ?
O8 C20 N14 126.2(13) . . ?
N14 C20 N13 108.0(9) . . ?
N13 C21 N15 112.0(10) . . ?
N13 C21 C22 105.8(9) . . ?
C22 C21 N15 104.3(8) . . ?
N14 C22 N16 113.4(9) . . ?
N14 C22 C21 105.3(9) . . ?
N16 C22 C21 105.5(10) . . ?
O13 C23 N15 124.9(11) . . ?
O13 C23 N16 126.8(10) . . ?
N16 C23 N15 108.3(9) . . ?
N17 C24 N14 111.5(10) . . ?
N16 C25 N19 110.0(9) . . ?
O9 C26 N17 127.4(11) . . ?
O9 C26 N18 124.6(11) . . ?
N17 C26 N18 107.9(9) . . ?
N3 C27 N18 109.4(10) 2_766 . ?
N17 C28 C29 103.4(8) . . ?
N19 C28 N17 114.1(10) . . ?
N19 C28 C29 102.7(9) . . ?
N18 C29 N20 113.9(10) . . ?
N18 C29 C28 102.2(8) . . ?
N20 C29 C28 103.3(9) . . ?
O14 C30 N19 128.0(10) . . ?
O14 C30 N20 126.5(10) . . ?
N20 C30 N19 105.3(9) . . ?
C32 N21 C31 122.8(9) . . ?
C32 N21 C33 113.3(9) . . ?
C33 N21 C31 121.8(8) . . ?
C32 N22 C34 110.3(8) . . ?
C32 N22 C36 124.0(9) . . ?
C36 N22 C34 119.9(10) . . ?
C33 N23 C60 119.7(9) . 2_656 ?
C35 N23 C33 113.3(9) . . ?
C35 N23 C60 118.6(9) . 2_656 ?
C34 N24 C37 122.9(10) . . ?
C35 N24 C34 114.3(9) . . ?
C35 N24 C37 119.3(9) . . ?
C36 N25 C39 121.1(9) . . ?
C38 N25 C36 124.2(9) . . ?
C38 N25 C39 110.7(9) . . ?
C38 N26 C40 113.0(8) . . ?
C38 N26 C42 120.8(9) . . ?
C40 N26 C42 119.9(10) . . ?
C39 N27 C37 123.3(8) . . ?
C41 N27 C37 120.2(8) . . ?
C41 N27 C39 113.6(8) . . ?
C41 N28 C40 113.8(8) . . ?
C41 N28 C43 122.1(9) . . ?
C43 N28 C40 121.8(9) . . ?
C44 N29 C42 122.8(9) . . ?
C44 N29 C45 112.4(8) . . ?
C45 N29 C42 120.3(9) . . ?
C44 N30 C46 114.1(8) . . ?
C44 N30 C48 123.1(9) . . ?
C46 N30 C48 121.8(9) . . ?
C45 N31 C43 122.7(9) . . ?
C47 N31 C43 120.4(8) . . ?
C47 N31 C45 112.6(7) . . ?
C46 N32 C49 119.0(8) . . ?
C47 N32 C46 112.2(8) . . ?
C47 N32 C49 121.7(8) . . ?
C50 N33 C48 121.7(8) . . ?
C50 N33 C51 110.7(8) . . ?
C51 N33 C48 119.1(9) . . ?
C50 N34 C52 112.9(9) . . ?
C50 N34 C54 123.5(8) . . ?
C52 N34 C54 119.2(9) . . ?
C49 N35 C51 119.3(9) . . ?
C53 N35 C49 124.5(8) . . ?
C53 N35 C51 113.6(8) . . ?
C53 N36 C52 112.5(9) . . ?
C53 N36 C55 122.2(9) . . ?
C55 N36 C52 120.2(8) . . ?
C56 N37 C54 123.6(9) . . ?
C56 N37 C57 111.7(9) . . ?
C57 N37 C54 122.5(10) . . ?
C56 N38 C58 113.5(10) . . ?
C56 N38 C60 118.3(9) . . ?
C58 N38 C60 121.5(9) . . ?
C55 N39 C57 120.9(9) . . ?
C59 N39 C55 120.3(9) . . ?
C59 N39 C57 113.2(8) . . ?
C58 N40 C31 124.7(8) . 2_656 ?
C59 N40 C31 121.0(8) . 2_656 ?
C59 N40 C58 112.7(9) . . ?
N40 C31 N21 113.0(8) 2_656 . ?
O15 C32 N21 127.7(12) . . ?
O15 C32 N22 122.4(10) . . ?
N21 C32 N22 109.9(9) . . ?
N21 C33 N23 114.8(9) . . ?
N21 C33 C34 104.0(8) . . ?
N23 C33 C34 100.9(8) . . ?
N22 C34 C33 101.9(8) . . ?
N24 C34 N22 114.5(8) . . ?
N24 C34 C33 104.6(9) . . ?
O20 C35 N23 126.2(11) . . ?
O20 C35 N24 127.7(11) . . ?
N24 C35 N23 106.0(9) . . ?
N22 C36 N25 114.0(9) . . ?
N24 C37 N27 111.7(8) . . ?
O16 C38 N25 123.9(11) . . ?
O16 C38 N26 127.3(10) . . ?
N26 C38 N25 108.7(9) . . ?
N25 C39 C40 103.4(8) . . ?
N27 C39 N25 115.2(10) . . ?
N27 C39 C40 104.3(8) . . ?
N26 C40 N28 113.4(8) . . ?
N26 C40 C39 103.9(9) . . ?
N28 C40 C39 101.1(8) . . ?
O21 C41 N27 126.2(9) . . ?
O21 C41 N28 126.8(9) . . ?
N28 C41 N27 107.0(9) . . ?
N29 C42 N26 111.5(8) . . ?
N28 C43 N31 113.2(9) . . ?
O17 C44 N29 126.7(10) . . ?
O17 C44 N30 125.8(9) . . ?
N29 C44 N30 107.5(9) . . ?
N29 C45 C46 103.5(8) . . ?
N31 C45 N29 113.9(9) . . ?
N31 C45 C46 103.1(8) . . ?
N30 C46 N32 116.9(9) . . ?
N30 C46 C45 101.9(8) . . ?
N32 C46 C45 102.6(7) . . ?
O22 C47 N31 124.6(8) . . ?
O22 C47 N32 126.3(9) . . ?
N31 C47 N32 109.0(8) . . ?
N30 C48 N33 112.4(8) . . ?
N32 C49 N35 112.7(8) . . ?
O18 C50 N33 123.6(10) . . ?
O18 C50 N34 127.2(10) . . ?
N34 C50 N33 109.2(9) . . ?
N33 C51 N35 113.3(8) . . ?
N33 C51 C52 103.7(8) . . ?
N35 C51 C52 101.8(8) . . ?
N34 C52 N36 114.3(9) . . ?
N34 C52 C51 102.6(8) . . ?
N36 C52 C51 103.7(7) . . ?
O23 C53 N35 124.5(10) . . ?
O23 C53 N36 127.2(11) . . ?
N35 C53 N36 108.3(9) . . ?
N37 C54 N34 114.1(8) . . ?
N36 C55 N39 115.0(10) . . ?
O19 C56 N37 125.4(11) . . ?
O19 C56 N38 126.5(12) . . ?
N38 C56 N37 108.1(10) . . ?
N37 C57 N39 114.4(8) . . ?
N37 C57 C58 104.7(9) . . ?
N39 C57 C58 100.9(8) . . ?
N38 C58 N40 115.2(9) . . ?
N38 C58 C57 101.2(8) . . ?
N40 C58 C57 104.7(8) . . ?
O24 C59 N39 126.5(11) . . ?
O24 C59 N40 126.0(11) . . ?
N39 C59 N40 107.4(8) . . ?
N23 C60 N38 111.0(8) 2_656 . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.231 -0.564 -0.517 2414.8 580.3 ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT029_p1                  
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.933 Why?  
RESPONSE: The alert arises due to only one-circle data colection is possible 
on MX2 beamline at the AUstralian SYnchrotron.
;
_vrf_PLAT973_p1                  
;
PROBLEM: Check Calcd Positive Resid. Density on        U1       3.42 eA-3  
RESPONSE: The alert arises due to ineffective absorption corrections as a result of
one-circle data colection.
;
_vrf_PLAT975_p1                  
;
PROBLEM: Check Calcd Resid. Dens.  0.80A   From O8W             2.45 eA-3  
RESPONSE: The alert arises due to ineffective absorption corrections as a result of
one-circle data colection.
;
_vrf_PLAT233_p1                  
;
PROBLEM: Hirshfeld (M-X Solvent)    U1       --O1W      .       21.0 s.u.  
RESPONSE: The alert arises due to ineffective absorption corrections as a result of
one-circle data colection.
;
_vrf_PLAT306_p1                  
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O7W Check 
RESPONSE: The alert arises due to no hydrogen atoms were added on the water molecule.
;
_vrf_PLAT420_p1                  
;
PROBLEM: D-H Without Acceptor       O2W      --H2WB     .     Please Check 
RESPONSE: The alert arises as no hydrogen atoms were added on some water molecules.
;
_vrf_PLAT911_p1                  
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.595       1469 Report
RESPONSE: The alert arises due to ineffective absorption corrections as a result of
one-circle data colection.
;
# end Validation Reply Form
