# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_Th_TMBiPDA
_database_code_depnum_ccdc_archive 'CCDC 1999186'
loop_
_audit_author_name
_audit_author_address
'Yanqiu Yang'
;Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics
China
;
_audit_update_record             
;
2020-11-20 deposited with the CCDC.	2020-12-03 downloaded from the CCDC.
;
_audit_creation_date             2019-05-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C32 H40 N8 O6 Th, 3(Cl O4), 2(C16 H18 N4 O2), 2(O)'
_chemical_formula_sum            'C64 H76 Cl3 N16 O24 Th'
_chemical_formula_weight         1791.79
_chemical_melting_point          ?
_chemical_oxdiff_formula         c12h12n2o3u1
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      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/n 1'
_space_group_name_Hall           '-P 2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   16.5157(16)
_cell_length_b                   14.3850(14)
_cell_length_c                   17.7543(14)
_cell_angle_alpha                90
_cell_angle_beta                 97.528(10)
_cell_angle_gamma                90
_cell_volume                     4181.7(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3277
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.4240
_cell_measurement_theta_min      3.6260
_shelx_estimated_absorpt_T_max   0.640
_shelx_estimated_absorpt_T_min   0.548
_exptl_absorpt_coefficient_mu    1.957
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1810
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0983
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11137
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.856
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0874
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -22.00  19.00   1.00   12.50    --  -14.81 -99.00  90.00   41
  2  ω      9.00  49.00   1.00   12.50    --   17.08 -99.00  30.00   40
  3  ω    -52.00  34.00   1.00   12.50    --   17.08 -38.00-180.00   86
  4  ω    -76.00 -16.00   1.00   12.50    --  -14.81 -19.00 -90.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0235209000
_diffrn_orient_matrix_UB_12      0.0264322000
_diffrn_orient_matrix_UB_13      -0.0229575000
_diffrn_orient_matrix_UB_21      -0.0137406000
_diffrn_orient_matrix_UB_22      0.0415762000
_diffrn_orient_matrix_UB_23      0.0156656000
_diffrn_orient_matrix_UB_31      0.0337187000
_diffrn_orient_matrix_UB_32      -0.0015254000
_diffrn_orient_matrix_UB_33      0.0291630000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6590
_reflns_number_total             11137
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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         1.108
_refine_diff_density_min         -1.361
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         11137
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.0777
_refine_ls_restrained_S_all      1.019
_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)+(0.1375P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2046
_refine_ls_wR_factor_ref         0.2211
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.6061(17)
 0.3939(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3.a Rotating group:
 O3(H3A,H3B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C18(H18), C19(H19), C20(H20),
 C26(H26), C27(H27), C28(H28)
3.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C)
;
_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
Th1 Th 0.7500 0.69491(4) 0.7500 0.0529(2) Uani 1 2 d S T P . .
O1 O 0.8310(7) 0.7861(6) 0.8435(5) 0.067(3) Uani 1 1 d . . . . .
O2 O 0.6669(4) 0.5632(5) 0.7076(4) 0.054(2) Uani 1 1 d . . . . .
O3 O 0.7858(5) 0.6342(6) 0.6301(4) 0.066(2) Uani 1 1 d . . . . .
H3A H 0.8319 0.6026 0.6374 0.100 Uiso 1 1 d GR . . . .
H3B H 0.7971 0.6798 0.6001 0.100 Uiso 1 1 d GR . . . .
N1 N 0.6845(6) 0.8365(6) 0.8199(5) 0.052(2) Uani 1 1 d . . . . .
N2 N 0.5891(6) 0.6984(7) 0.7568(5) 0.047(2) Uani 1 1 d . . . . .
N3 N 0.8690(8) 0.8918(8) 0.9353(6) 0.079(4) Uani 1 1 d . . . . .
N4 N 0.5749(6) 0.4615(10) 0.7324(6) 0.073(3) Uani 1 1 d . . . . .
C1 C 0.7326(10) 0.8969(9) 0.8570(7) 0.071(4) Uani 1 1 d . . . . .
C2 C 0.7132(14) 0.9869(12) 0.8709(11) 0.135(8) Uani 1 1 d . . . . .
H2 H 0.7505 1.0294 0.8947 0.162 Uiso 1 1 calc R . . . .
C3 C 0.6304(13) 1.0093(10) 0.8456(13) 0.143(8) Uani 1 1 d . . . . .
H3 H 0.6125 1.0696 0.8526 0.171 Uiso 1 1 calc R . . . .
C4 C 0.5767(14) 0.9469(12) 0.8117(11) 0.143(10) Uani 1 1 d . . . . .
H4 H 0.5226 0.9630 0.7961 0.172 Uiso 1 1 calc R . . . .
C5 C 0.6048(11) 0.8583(11) 0.8010(8) 0.087(5) Uani 1 1 d . . . . .
C6 C 0.5497(8) 0.7809(12) 0.7665(8) 0.077(4) Uani 1 1 d . . . . .
C7 C 0.4664(9) 0.7939(12) 0.7443(9) 0.090(5) Uani 1 1 d . . . . .
H7 H 0.4420 0.8514 0.7496 0.108 Uiso 1 1 calc R . . . .
C8 C 0.4224(9) 0.7207(14) 0.7151(9) 0.093(5) Uani 1 1 d . . . . .
H8 H 0.3670 0.7274 0.6983 0.112 Uiso 1 1 calc R . . . .
C9 C 0.4615(8) 0.6325(11) 0.7100(9) 0.082(4) Uani 1 1 d . . . . .
H9 H 0.4314 0.5807 0.6918 0.099 Uiso 1 1 calc R . . . .
C10 C 0.5452(7) 0.6255(8) 0.7325(6) 0.050(3) Uani 1 1 d . . . . .
C11 C 0.8136(8) 0.8567(11) 0.8803(6) 0.063(4) Uani 1 1 d . . . . .
C12 C 0.9524(12) 0.8455(12) 0.9464(9) 0.112(6) Uani 1 1 d . . . . .
H12A H 0.9469 0.7823 0.9624 0.168 Uiso 1 1 calc GR . . . .
H12B H 0.9879 0.8786 0.9844 0.168 Uiso 1 1 calc GR . . . .
H12C H 0.9752 0.8464 0.8993 0.168 Uiso 1 1 calc GR . . . .
C13 C 0.8545(12) 0.9650(12) 0.9895(9) 0.124(7) Uani 1 1 d . . . . .
H13A H 0.8703 1.0240 0.9708 0.186 Uiso 1 1 calc GR . . . .
H13B H 0.8861 0.9524 1.0377 0.186 Uiso 1 1 calc GR . . . .
H13C H 0.7976 0.9664 0.9953 0.186 Uiso 1 1 calc GR . . . .
C14 C 0.5976(8) 0.5493(10) 0.7242(6) 0.053(3) Uani 1 1 d . . . . .
C15 C 0.6322(8) 0.3825(9) 0.7199(7) 0.074(4) Uani 1 1 d . . . . .
H15A H 0.6681 0.4015 0.6844 0.111 Uiso 1 1 calc GR . . . .
H15B H 0.6010 0.3296 0.7000 0.111 Uiso 1 1 calc GR . . . .
H15C H 0.6638 0.3662 0.7673 0.111 Uiso 1 1 calc GR . . . .
C16 C 0.5028(9) 0.4333(11) 0.7707(9) 0.096(5) Uani 1 1 d . . . . .
H16A H 0.5214 0.4003 0.8167 0.143 Uiso 1 1 calc GR . . . .
H16B H 0.4676 0.3937 0.7373 0.143 Uiso 1 1 calc GR . . . .
H16C H 0.4732 0.4877 0.7824 0.143 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.2500 0.5193(6) 0.7500 0.121(2) Uiso 1 2 d S T P . .
O6 O 0.3172(14) 0.4609(15) 0.7517(14) 0.261(10) Uiso 1 1 d . . . . .
O7 O 0.2501(13) 0.5859(13) 0.6849(11) 0.218(8) Uiso 1 1 d . . . . .
Cl2 Cl 0.5281(5) 1.1415(5) 0.6700(4) 0.148(2) Uiso 1 1 d . . . . .
O8 O 0.4968(13) 1.0571(16) 0.6523(12) 0.234(9) Uiso 1 1 d . . . . .
O9 O 0.4790(16) 1.2063(15) 0.6328(15) 0.255(11) Uiso 1 1 d . . . . .
O10 O 0.5502(10) 1.1693(11) 0.7466(10) 0.163(6) Uiso 1 1 d . . . . .
O11 O 0.5912(15) 1.1308(16) 0.6507(13) 0.239(9) Uiso 1 1 d . . . . .
O4 O 0.7026(6) 0.4538(6) 0.9062(5) 0.074(3) Uani 1 1 d . . . . .
N5 N 0.8959(8) 0.4567(7) 0.9777(5) 0.068(3) Uani 1 1 d . . . . .
N6 N 0.7511(9) 0.3267(8) 0.9631(6) 0.092(4) Uani 1 1 d . . . . .
C17 C 0.8215(8) 0.4732(9) 0.9910(7) 0.061(3) Uani 1 1 d . . . . .
C18 C 0.8064(9) 0.5480(10) 1.0374(8) 0.080(4) Uani 1 1 d . . . . .
H18 H 0.7532 0.5602 1.0464 0.096 Uiso 1 1 calc R . . . .
C19 C 0.8669(9) 0.6019(10) 1.0689(8) 0.084(4) Uani 1 1 d . . . . .
H19 H 0.8563 0.6510 1.1002 0.101 Uiso 1 1 calc R . . . .
C20 C 0.9433(9) 0.5846(9) 1.0552(8) 0.073(4) Uani 1 1 d . . . . .
H20 H 0.9862 0.6217 1.0770 0.088 Uiso 1 1 calc R . . . .
C21 C 0.9583(7) 0.5112(11) 1.0082(7) 0.069(4) Uani 1 1 d . . . . .
C22 C 0.7546(8) 0.4156(9) 0.9493(6) 0.058(3) Uani 1 1 d . . . . .
C23 C 0.6912(12) 0.2677(12) 0.9191(10) 0.123(7) Uani 1 1 d . . . . .
H23A H 0.6435 0.3037 0.9014 0.184 Uiso 1 1 calc GR . . . .
H23B H 0.6764 0.2177 0.9503 0.184 Uiso 1 1 calc GR . . . .
H23C H 0.7140 0.2428 0.8763 0.184 Uiso 1 1 calc GR . . . .
C24 C 0.8154(13) 0.2748(13) 1.0172(12) 0.149(10) Uani 1 1 d . . . . .
H24A H 0.8611 0.2596 0.9911 0.223 Uiso 1 1 calc GR . . . .
H24B H 0.7921 0.2186 1.0341 0.223 Uiso 1 1 calc GR . . . .
H24C H 0.8334 0.3134 1.0602 0.223 Uiso 1 1 calc GR . . . .
O5 O 0.6984(7) 0.7497(8) 0.9834(5) 0.092(3) Uani 1 1 d . . . . .
N7 N 0.5678(6) 0.5971(7) 1.0174(5) 0.060(3) Uani 1 1 d . . . . .
N8 N 0.6599(9) 0.7649(9) 1.0986(6) 0.093(4) Uani 1 1 d . . . . .
C25 C 0.5699(9) 0.6891(9) 0.9981(8) 0.066(4) Uani 1 1 d . . . . .
C26 C 0.5111(10) 0.7318(9) 0.9528(10) 0.081(4) Uani 1 1 d . . . . .
H26 H 0.5164 0.7938 0.9394 0.097 Uiso 1 1 calc R . . . .
C27 C 0.4412(11) 0.6814(10) 0.9260(10) 0.090(5) Uani 1 1 d . . . . .
H27 H 0.3970 0.7120 0.8989 0.108 Uiso 1 1 calc R . . . .
C28 C 0.4364(9) 0.5896(10) 0.9385(7) 0.076(4) Uani 1 1 d . . . . .
H28 H 0.3931 0.5542 0.9152 0.092 Uiso 1 1 calc R . . . .
C29 C 0.5004(8) 0.5493(7) 0.9889(7) 0.058(3) Uani 1 1 d . . . . .
C30 C 0.6491(10) 0.7369(10) 1.0268(8) 0.072(4) Uani 1 1 d . . . . .
C31 C 0.7349(12) 0.8115(11) 1.1278(10) 0.108(6) Uani 1 1 d . . . . .
H31A H 0.7674 0.7714 1.1629 0.162 Uiso 1 1 calc GR . . . .
H31B H 0.7225 0.8676 1.1533 0.162 Uiso 1 1 calc GR . . . .
H31C H 0.7648 0.8267 1.0865 0.162 Uiso 1 1 calc GR . . . .
C32 C 0.6046(14) 0.7487(16) 1.1522(9) 0.142(8) Uani 1 1 d . . . . .
H32A H 0.6298 0.7664 1.2020 0.213 Uiso 1 1 calc GR . . . .
H32B H 0.5907 0.6839 1.1522 0.213 Uiso 1 1 calc GR . . . .
H32C H 0.5560 0.7849 1.1387 0.213 Uiso 1 1 calc GR . . . .
O12 O 0.6055(13) 1.0273(14) 1.0498(12) 0.244(9) Uiso 1 1 d . . . . .


_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 O1 2.384(7) 2_656 ?
Th1 O1 2.384(8) . ?
Th1 O2 2.402(7) . ?
Th1 O2 2.402(7) 2_656 ?
Th1 O3 2.443(7) 2_656 ?
Th1 O3 2.443(7) . ?
Th1 N1 2.686(9) 2_656 ?
Th1 N1 2.686(9) . ?
Th1 N2 2.676(10) 2_656 ?
Th1 N2 2.676(10) . ?
O1 C11 1.261(16) . ?
O2 C14 1.235(13) . ?
O3 H3A 0.8824 . ?
O3 H3B 0.8810 . ?
N1 C1 1.296(14) . ?
N1 C5 1.353(17) . ?
N2 C6 1.374(16) . ?
N2 C10 1.315(13) . ?
N3 C11 1.346(15) . ?
N3 C12 1.519(19) . ?
N3 C13 1.467(18) . ?
N4 C14 1.330(16) . ?
N4 C15 1.515(17) . ?
N4 C16 1.502(18) . ?
C1 C2 1.36(2) . ?
C1 C11 1.466(18) . ?
C2 H2 0.9300 . ?
C2 C3 1.42(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.35(2) . ?
C4 H4 0.9300 . ?
C4 C5 1.38(2) . ?
C5 C6 1.52(2) . ?
C6 C7 1.394(19) . ?
C7 H7 0.9300 . ?
C7 C8 1.34(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.43(2) . ?
C9 H9 0.9300 . ?
C9 C10 1.392(16) . ?
C10 C14 1.417(16) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
Cl1 O6 1.39(2) 2_556 ?
Cl1 O6 1.39(2) . ?
Cl1 O7 1.502(19) . ?
Cl1 O7 1.502(19) 2_556 ?
Cl2 O8 1.34(2) . ?
Cl2 O9 1.35(2) . ?
Cl2 O10 1.419(17) . ?
Cl2 O11 1.15(2) . ?
O4 C22 1.206(13) . ?
N5 C17 1.303(16) . ?
N5 C21 1.351(16) . ?
N6 C22 1.306(15) . ?
N6 C23 1.452(17) . ?
N6 C24 1.53(2) . ?
C17 C18 1.397(18) . ?
C17 C22 1.496(17) . ?
C18 H18 0.9300 . ?
C18 C19 1.329(17) . ?
C19 H19 0.9300 . ?
C19 C20 1.339(19) . ?
C20 H20 0.9300 . ?
C20 C21 1.387(18) . ?
C21 C21 1.48(3) 3_767 ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
O5 C30 1.207(17) . ?
N7 C25 1.368(14) . ?
N7 C29 1.348(13) . ?
N8 C30 1.326(16) . ?
N8 C31 1.444(19) . ?
N8 C32 1.42(2) . ?
C25 C26 1.33(2) . ?
C25 C30 1.51(2) . ?
C26 H26 0.9300 . ?
C26 C27 1.39(2) . ?
C27 H27 0.9300 . ?
C27 C28 1.343(17) . ?
C28 H28 0.9300 . ?
C28 C29 1.417(16) . ?
C29 C29 1.47(2) 3_667 ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Th1 O1 113.2(4) 2_656 . ?
O1 Th1 O2 88.3(3) . 2_656 ?
O1 Th1 O2 153.9(3) 2_656 2_656 ?
O1 Th1 O2 153.9(3) . . ?
O1 Th1 O2 88.3(3) 2_656 . ?
O1 Th1 O3 128.7(4) . . ?
O1 Th1 O3 76.6(3) 2_656 . ?
O1 Th1 O3 76.6(3) . 2_656 ?
O1 Th1 O3 128.7(4) 2_656 2_656 ?
O1 Th1 N1 71.4(3) . 2_656 ?
O1 Th1 N1 58.9(3) . . ?
O1 Th1 N1 58.9(3) 2_656 2_656 ?
O1 Th1 N1 71.4(3) 2_656 . ?
O1 Th1 N2 63.3(4) 2_656 . ?
O1 Th1 N2 115.4(4) . . ?
O1 Th1 N2 63.3(4) . 2_656 ?
O1 Th1 N2 115.4(4) 2_656 2_656 ?
O2 Th1 O2 75.9(4) . 2_656 ?
O2 Th1 O3 78.3(3) . 2_656 ?
O2 Th1 O3 78.3(3) 2_656 . ?
O2 Th1 O3 68.8(3) 2_656 2_656 ?
O2 Th1 O3 68.8(3) . . ?
O2 Th1 N1 119.7(3) . . ?
O2 Th1 N1 119.7(3) 2_656 2_656 ?
O2 Th1 N1 134.5(3) . 2_656 ?
O2 Th1 N1 134.5(3) 2_656 . ?
O2 Th1 N2 59.9(3) . . ?
O2 Th1 N2 122.1(3) . 2_656 ?
O2 Th1 N2 59.9(3) 2_656 2_656 ?
O2 Th1 N2 122.1(3) 2_656 . ?
O3 Th1 O3 138.1(4) 2_656 . ?
O3 Th1 N1 146.3(3) . . ?
O3 Th1 N1 73.2(3) . 2_656 ?
O3 Th1 N1 146.3(3) 2_656 2_656 ?
O3 Th1 N1 73.2(3) 2_656 . ?
O3 Th1 N2 113.6(3) 2_656 2_656 ?
O3 Th1 N2 113.6(3) . . ?
O3 Th1 N2 67.2(3) . 2_656 ?
O3 Th1 N2 67.2(3) 2_656 . ?
N1 Th1 N1 81.3(4) . 2_656 ?
N2 Th1 N1 118.0(3) 2_656 . ?
N2 Th1 N1 60.2(3) 2_656 2_656 ?
N2 Th1 N1 118.0(3) . 2_656 ?
N2 Th1 N1 60.2(3) . . ?
N2 Th1 N2 177.8(4) 2_656 . ?
C11 O1 Th1 131.2(8) . . ?
C14 O2 Th1 124.3(8) . . ?
Th1 O3 H3A 111.1 . . ?
Th1 O3 H3B 110.8 . . ?
H3A O3 H3B 103.0 . . ?
C1 N1 Th1 119.1(9) . . ?
C1 N1 C5 118.8(12) . . ?
C5 N1 Th1 119.9(8) . . ?
C6 N2 Th1 120.8(8) . . ?
C10 N2 Th1 118.5(8) . . ?
C10 N2 C6 118.6(10) . . ?
C11 N3 C12 116.7(12) . . ?
C11 N3 C13 126.2(15) . . ?
C13 N3 C12 116.9(11) . . ?
C14 N4 C15 120.4(11) . . ?
C14 N4 C16 123.9(13) . . ?
C16 N4 C15 114.3(12) . . ?
N1 C1 C2 125.8(16) . . ?
N1 C1 C11 110.7(11) . . ?
C2 C1 C11 123.4(15) . . ?
C1 C2 H2 123.3 . . ?
C1 C2 C3 113.5(15) . . ?
C3 C2 H2 123.3 . . ?
C2 C3 H3 118.7 . . ?
C4 C3 C2 122.7(15) . . ?
C4 C3 H3 118.7 . . ?
C3 C4 H4 121.2 . . ?
C3 C4 C5 117.7(18) . . ?
C5 C4 H4 121.2 . . ?
N1 C5 C4 121.0(16) . . ?
N1 C5 C6 116.3(13) . . ?
C4 C5 C6 122.7(17) . . ?
N2 C6 C5 114.6(12) . . ?
N2 C6 C7 123.2(14) . . ?
C7 C6 C5 122.2(15) . . ?
C6 C7 H7 121.1 . . ?
C8 C7 C6 117.8(15) . . ?
C8 C7 H7 121.1 . . ?
C7 C8 H8 120.2 . . ?
C7 C8 C9 119.6(13) . . ?
C9 C8 H8 120.2 . . ?
C8 C9 H9 120.5 . . ?
C10 C9 C8 119.0(13) . . ?
C10 C9 H9 120.5 . . ?
N2 C10 C9 121.4(12) . . ?
N2 C10 C14 109.5(10) . . ?
C9 C10 C14 128.5(12) . . ?
O1 C11 N3 119.8(13) . . ?
O1 C11 C1 115.7(10) . . ?
N3 C11 C1 124.4(14) . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 H13A 109.5 . . ?
N3 C13 H13B 109.5 . . ?
N3 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O2 C14 N4 117.7(12) . . ?
O2 C14 C10 119.7(12) . . ?
N4 C14 C10 122.6(12) . . ?
N4 C15 H15A 109.5 . . ?
N4 C15 H15B 109.5 . . ?
N4 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N4 C16 H16A 109.5 . . ?
N4 C16 H16B 109.5 . . ?
N4 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O6 Cl1 O6 106(2) . 2_556 ?
O6 Cl1 O7 116.8(11) . 2_556 ?
O6 Cl1 O7 108.8(14) . . ?
O6 Cl1 O7 116.8(11) 2_556 . ?
O6 Cl1 O7 108.8(14) 2_556 2_556 ?
O7 Cl1 O7 100.7(16) 2_556 . ?
O8 Cl2 O9 108.8(14) . . ?
O8 Cl2 O10 121.4(13) . . ?
O9 Cl2 O10 109.7(15) . . ?
O11 Cl2 O8 98.4(17) . . ?
O11 Cl2 O9 117.2(19) . . ?
O11 Cl2 O10 101.1(14) . . ?
C17 N5 C21 120.6(12) . . ?
C22 N6 C23 121.0(13) . . ?
C22 N6 C24 123.5(13) . . ?
C23 N6 C24 114.9(14) . . ?
N5 C17 C18 119.5(13) . . ?
N5 C17 C22 117.5(13) . . ?
C18 C17 C22 122.7(13) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 C17 121.0(15) . . ?
C19 C18 H18 119.5 . . ?
C18 C19 H19 120.4 . . ?
C18 C19 C20 119.3(15) . . ?
C20 C19 H19 120.4 . . ?
C19 C20 H20 120.1 . . ?
C19 C20 C21 119.8(12) . . ?
C21 C20 H20 120.1 . . ?
N5 C21 C20 119.7(12) . . ?
N5 C21 C21 118.4(17) . 3_767 ?
C20 C21 C21 121.9(16) . 3_767 ?
O4 C22 N6 121.3(12) . . ?
O4 C22 C17 118.7(12) . . ?
N6 C22 C17 119.9(12) . . ?
N6 C23 H23A 109.5 . . ?
N6 C23 H23B 109.5 . . ?
N6 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N6 C24 H24A 109.5 . . ?
N6 C24 H24B 109.5 . . ?
N6 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C29 N7 C25 116.5(11) . . ?
C30 N8 C31 119.2(14) . . ?
C30 N8 C32 125.2(15) . . ?
C32 N8 C31 115.6(13) . . ?
N7 C25 C30 114.0(13) . . ?
C26 C25 N7 123.9(13) . . ?
C26 C25 C30 121.8(12) . . ?
C25 C26 H26 120.8 . . ?
C25 C26 C27 118.3(13) . . ?
C27 C26 H26 120.8 . . ?
C26 C27 H27 119.4 . . ?
C28 C27 C26 121.3(15) . . ?
C28 C27 H27 119.4 . . ?
C27 C28 H28 121.6 . . ?
C27 C28 C29 116.8(13) . . ?
C29 C28 H28 121.6 . . ?
N7 C29 C28 122.6(11) . . ?
N7 C29 C29 115.3(14) . 3_667 ?
C28 C29 C29 122.1(15) . 3_667 ?
O5 C30 N8 123.3(15) . . ?
O5 C30 C25 118.9(12) . . ?
N8 C30 C25 117.8(15) . . ?
N8 C31 H31A 109.5 . . ?
N8 C31 H31B 109.5 . . ?
N8 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N8 C32 H32A 109.5 . . ?
N8 C32 H32B 109.5 . . ?
N8 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Th1 O1 C11 N3 174.5(8) . . . . ?
Th1 O1 C11 C1 -7.6(18) . . . . ?
Th1 O2 C14 N4 -146.5(8) . . . . ?
Th1 O2 C14 C10 34.6(13) . . . . ?
Th1 N1 C1 C2 154.1(14) . . . . ?
Th1 N1 C1 C11 -23.7(12) . . . . ?
Th1 N1 C5 C4 -154.7(14) . . . . ?
Th1 N1 C5 C6 24.1(15) . . . . ?
Th1 N2 C6 C5 -21.6(15) . . . . ?
Th1 N2 C6 C7 156.5(12) . . . . ?
Th1 N2 C10 C9 -157.8(10) . . . . ?
Th1 N2 C10 C14 14.4(12) . . . . ?
N1 C1 C2 C3 5(3) . . . . ?
N1 C1 C11 O1 20.5(16) . . . . ?
N1 C1 C11 N3 -161.7(12) . . . . ?
N1 C5 C6 N2 -1.8(18) . . . . ?
N1 C5 C6 C7 -179.9(14) . . . . ?
N2 C6 C7 C8 3(2) . . . . ?
N2 C10 C14 O2 -30.5(14) . . . . ?
N2 C10 C14 N4 150.5(11) . . . . ?
C1 N1 C5 C4 9(2) . . . . ?
C1 N1 C5 C6 -172.7(11) . . . . ?
C1 C2 C3 C4 1(3) . . . . ?
C2 C1 C11 O1 -157.4(16) . . . . ?
C2 C1 C11 N3 20(2) . . . . ?
C2 C3 C4 C5 -1(4) . . . . ?
C3 C4 C5 N1 -4(3) . . . . ?
C3 C4 C5 C6 177.5(19) . . . . ?
C4 C5 C6 N2 177.0(16) . . . . ?
C4 C5 C6 C7 -1(2) . . . . ?
C5 N1 C1 C2 -9(2) . . . . ?
C5 N1 C1 C11 173.0(11) . . . . ?
C5 C6 C7 C8 -179.2(15) . . . . ?
C6 N2 C10 C9 5.9(18) . . . . ?
C6 N2 C10 C14 178.1(10) . . . . ?
C6 C7 C8 C9 2(2) . . . . ?
C7 C8 C9 C10 -3(2) . . . . ?
C8 C9 C10 N2 -1(2) . . . . ?
C8 C9 C10 C14 -171.9(13) . . . . ?
C9 C10 C14 O2 141.0(14) . . . . ?
C9 C10 C14 N4 -38(2) . . . . ?
C10 N2 C6 C5 175.0(11) . . . . ?
C10 N2 C6 C7 -7(2) . . . . ?
C11 C1 C2 C3 -177.8(16) . . . . ?
C12 N3 C11 O1 3.1(19) . . . . ?
C12 N3 C11 C1 -174.5(13) . . . . ?
C13 N3 C11 O1 -171.3(14) . . . . ?
C13 N3 C11 C1 11(2) . . . . ?
C15 N4 C14 O2 -1.4(17) . . . . ?
C15 N4 C14 C10 177.6(10) . . . . ?
C16 N4 C14 O2 164.2(11) . . . . ?
C16 N4 C14 C10 -16.8(18) . . . . ?
N5 C17 C18 C19 -1(2) . . . . ?
N5 C17 C22 O4 -117.4(14) . . . . ?
N5 C17 C22 N6 66.3(17) . . . . ?
C17 N5 C21 C20 1.2(18) . . . . ?
C17 N5 C21 C21 179.4(13) . . . 3_767 ?
C17 C18 C19 C20 1(2) . . . . ?
C18 C17 C22 O4 56.9(18) . . . . ?
C18 C17 C22 N6 -119.5(16) . . . . ?
C18 C19 C20 C21 0(2) . . . . ?
C19 C20 C21 N5 -1(2) . . . . ?
C19 C20 C21 C21 -179.4(16) . . . 3_767 ?
C21 N5 C17 C18 -0.2(18) . . . . ?
C21 N5 C17 C22 174.2(11) . . . . ?
C22 C17 C18 C19 -174.9(13) . . . . ?
C23 N6 C22 O4 9(2) . . . . ?
C23 N6 C22 C17 -174.7(15) . . . . ?
C24 N6 C22 O4 180.0(16) . . . . ?
C24 N6 C22 C17 -4(2) . . . . ?
N7 C25 C26 C27 3(2) . . . . ?
N7 C25 C30 O5 101.0(16) . . . . ?
N7 C25 C30 N8 -80.6(17) . . . . ?
C25 N7 C29 C28 3.1(18) . . . . ?
C25 N7 C29 C29 -179.5(12) . . . 3_667 ?
C25 C26 C27 C28 -7(3) . . . . ?
C26 C25 C30 O5 -74(2) . . . . ?
C26 C25 C30 N8 104.8(18) . . . . ?
C26 C27 C28 C29 9(3) . . . . ?
C27 C28 C29 N7 -7(2) . . . . ?
C27 C28 C29 C29 176.0(16) . . . 3_667 ?
C29 N7 C25 C26 -1.2(19) . . . . ?
C29 N7 C25 C30 -175.7(11) . . . . ?
C30 C25 C26 C27 177.1(14) . . . . ?
C31 N8 C30 O5 -1(3) . . . . ?
C31 N8 C30 C25 -179.6(14) . . . . ?
C32 N8 C30 O5 -177.9(18) . . . . ?
C32 N8 C30 C25 4(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.128
_oxdiff_exptl_absorpt_empirical_full_min 0.873
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.6061(17) 3776 16824 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.3939(17) 3820 16823 nmt 0.0819 -0.0014 -0.9167 -0.0001 -1.0006 -0.0003
-1.0827 -0.0012 -0.0849

_twin_special_details            
;
Component 2 rotated by 179.9536° 
 around [-0.71 0.00 0.71] (reciprocal) or [-0.76 0.00 0.65] (direct)
;

# start Validation Reply Form
_vrf_PLAT602_Th_TMBiPDA          
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! Info
RESPONSE: Huge cavities occure in the system because of the co-crystallization 
of the complex compound with two free ligand molecules.
;
_vrf_PLAT234_Th_TMBiPDA          
;
PROBLEM: Large Hirshfeld Difference C3 --C4 . 0.26 Ang
RESPONSE: It is caused by the thermal vibration difference between them.
;
_vrf_PLAT306_Th_TMBiPDA          
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O12 Check
RESPONSE: This is a water molecule of crystallisation. 
The H atoms could not be located in this heavy atom containing structure.
;
_vrf_PLAT342_Th_TMBiPDA          
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.02013 Ang.
RESPONSE: Moderate data quality in context with desolvation and
 Th as heavy atom.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Th_TMPhenDA
_database_code_depnum_ccdc_archive 'CCDC 1999187'
loop_
_audit_author_name
_audit_author_address
'Yanqiu Yang'
;Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics
China
;
_audit_update_record             
;
2020-11-20 deposited with the CCDC.	2020-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H44 Cl4 N8 O22 Th'
_chemical_formula_weight         1362.67

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.4288(10)
_cell_length_b                   13.2281(5)
_cell_length_c                   33.7824(13)
_cell_angle_alpha                90
_cell_angle_beta                 93.0280(10)
_cell_angle_gamma                90
_cell_volume                     10455.2(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9987
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      25.66

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_F_000             5392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    3.143
_shelx_estimated_absorpt_T_min   0.704
_shelx_estimated_absorpt_T_max   0.787
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38312
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         2.066
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_full        25.008
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             9172
_reflns_number_gt                7589
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0534P)²+45.2796P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9172
_refine_ls_number_parameters     656
_refine_ls_number_restraints     115
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.1186
_refine_ls_wR_factor_gt          0.1119
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
C1 C 0.4556(5) 0.7481(10) 0.6366(4) 0.151(5) Uani 1 1 d . . . . .
H1A H 0.473787 0.685575 0.630212 0.226 Uiso 1 1 calc R U . . .
H1B H 0.474668 0.777120 0.659708 0.226 Uiso 1 1 calc R U . . .
H1C H 0.457658 0.794102 0.614696 0.226 Uiso 1 1 calc R U . . .
C2 C 0.3544(5) 0.8176(8) 0.6384(4) 0.148(5) Uani 1 1 d . . . . .
H2A H 0.368140 0.873619 0.654179 0.222 Uiso 1 1 calc R U . . .
H2B H 0.317050 0.798553 0.646183 0.222 Uiso 1 1 calc R U . . .
H2C H 0.352227 0.836669 0.610904 0.222 Uiso 1 1 calc R U . . .
C3 C 0.3714(4) 0.6385(7) 0.6533(2) 0.084(2) Uani 1 1 d . . . . .
C4 C 0.4057(3) 0.5508(7) 0.6673(2) 0.080(2) Uani 1 1 d . . . . .
C5 C 0.4606(4) 0.5525(8) 0.6869(2) 0.092(3) Uani 1 1 d . . . . .
H5 H 0.478411 0.614077 0.692403 0.110 Uiso 1 1 calc R U . . .
C6 C 0.4869(4) 0.4672(10) 0.6973(2) 0.099(3) Uani 1 1 d . . . . .
H6 H 0.523802 0.468848 0.708814 0.118 Uiso 1 1 calc R U . . .
C7 C 0.4595(4) 0.3765(9) 0.6912(2) 0.088(3) Uani 1 1 d . . . . .
C8 C 0.4832(5) 0.2797(11) 0.7016(3) 0.120(4) Uani 1 1 d . . . . .
H8 H 0.521227 0.275847 0.710900 0.144 Uiso 1 1 calc R U . . .
C9 C 0.4530(5) 0.1961(10) 0.6983(3) 0.111(4) Uani 1 1 d . . . . .
H9 H 0.470811 0.135300 0.705271 0.133 Uiso 1 1 calc R U . . .
C10 C 0.3923(5) 0.1936(8) 0.6841(3) 0.095(3) Uani 1 1 d . . . . .
C11 C 0.3585(6) 0.1124(9) 0.6805(3) 0.118(4) Uani 1 1 d . . . . .
H11 H 0.374300 0.049452 0.686596 0.142 Uiso 1 1 calc R U . . .
C12 C 0.3027(5) 0.1167(7) 0.6684(3) 0.107(3) Uani 1 1 d . . . . .
H12 H 0.280297 0.058748 0.666548 0.129 Uiso 1 1 calc R U . . .
C13 C 0.2796(4) 0.2137(6) 0.6586(2) 0.080(2) Uani 1 1 d . . . . .
C14 C 0.2199(4) 0.2388(6) 0.6463(2) 0.076(2) Uani 1 1 d . . . . .
C15 C 0.1189(4) 0.2184(8) 0.6359(3) 0.119(4) Uani 1 1 d . . . . .
H15A H 0.103032 0.260354 0.655688 0.178 Uiso 1 1 calc R U . . .
H15B H 0.094273 0.161535 0.630480 0.178 Uiso 1 1 calc R U . . .
H15C H 0.122533 0.256771 0.612029 0.178 Uiso 1 1 calc R U . . .
C16 C 0.1767(6) 0.0801(10) 0.6674(5) 0.182(7) Uani 1 1 d . . . . .
H16A H 0.203391 0.078869 0.689971 0.273 Uiso 1 1 calc R U . . .
H16B H 0.188540 0.032741 0.647937 0.273 Uiso 1 1 calc R U . . .
H16C H 0.139406 0.062065 0.675525 0.273 Uiso 1 1 calc R U . . .
C17 C 0.4026(3) 0.3783(7) 0.6748(2) 0.072(2) Uani 1 1 d . . . . .
C18 C 0.3690(3) 0.2871(6) 0.6720(2) 0.071(2) Uani 1 1 d . . . . .
C19 C 0.4250(4) 0.3365(8) 0.5028(3) 0.112(3) Uani 1 1 d . . . . .
H19A H 0.400516 0.373286 0.484266 0.168 Uiso 1 1 calc R U . . .
H19B H 0.432380 0.270562 0.492400 0.168 Uiso 1 1 calc R U . . .
H19C H 0.460436 0.372252 0.507227 0.168 Uiso 1 1 calc R U . . .
C20 C 0.4003(4) 0.2256(7) 0.5573(3) 0.104(3) Uani 1 1 d . . . . .
H20A H 0.438671 0.212493 0.567260 0.156 Uiso 1 1 calc R U . . .
H20B H 0.389498 0.177027 0.537159 0.156 Uiso 1 1 calc R U . . .
H20C H 0.374787 0.220607 0.578554 0.156 Uiso 1 1 calc R U . . .
C21 C 0.3676(3) 0.5047(6) 0.54741(19) 0.0633(17) Uani 1 1 d . . . . .
C22 C 0.4066(3) 0.5583(7) 0.5248(2) 0.079(2) Uani 1 1 d . . . . .
H22 H 0.438419 0.525667 0.515539 0.095 Uiso 1 1 calc R U . . .
C23 C 0.3973(4) 0.6576(7) 0.5165(2) 0.090(3) Uani 1 1 d . . . . .
H23 H 0.423364 0.692930 0.501915 0.108 Uiso 1 1 calc R U . . .
C24 C 0.3497(3) 0.7067(7) 0.5294(2) 0.077(2) Uani 1 1 d . . . . .
C25 C 0.3354(4) 0.8083(7) 0.5205(3) 0.092(3) Uani 1 1 d . . . . .
H25 H 0.359588 0.846197 0.505409 0.111 Uiso 1 1 calc R U . . .
C26 C 0.2881(4) 0.8514(7) 0.5333(3) 0.095(3) Uani 1 1 d . . . . .
H26 H 0.279460 0.917903 0.526413 0.114 Uiso 1 1 calc R U . . .
C27 C 0.2503(4) 0.7947(6) 0.5577(2) 0.077(2) Uani 1 1 d . . . . .
C28 C 0.2003(4) 0.8346(7) 0.5732(3) 0.088(2) Uani 1 1 d . . . . .
H28 H 0.190029 0.901239 0.567683 0.105 Uiso 1 1 calc R U . . .
C29 C 0.1672(3) 0.7777(6) 0.5958(2) 0.077(2) Uani 1 1 d . . . . .
H29 H 0.134793 0.805058 0.606459 0.092 Uiso 1 1 calc R U . . .
C30 C 0.1823(3) 0.6769(5) 0.6030(2) 0.0600(17) Uani 1 1 d . . . . .
C31 C 0.0737(4) 0.5264(7) 0.6575(4) 0.115(4) Uani 1 1 d . . . . .
H31A H 0.098294 0.468277 0.659191 0.172 Uiso 1 1 calc R U . . .
H31B H 0.036443 0.506514 0.647211 0.172 Uiso 1 1 calc R U . . .
H31C H 0.070870 0.555031 0.683459 0.172 Uiso 1 1 calc R U . . .
C32 C 0.0563(3) 0.6717(8) 0.6117(3) 0.112(3) Uani 1 1 d . . . . .
H32A H 0.055957 0.733945 0.626274 0.168 Uiso 1 1 calc R U . . .
H32B H 0.018844 0.642100 0.610793 0.168 Uiso 1 1 calc R U . . .
H32C H 0.067178 0.684950 0.585153 0.168 Uiso 1 1 calc R U . . .
C33 C 0.2636(3) 0.6928(5) 0.5680(2) 0.0626(17) Uani 1 1 d . . . . .
C34 C 0.3141(3) 0.6505(5) 0.55355(19) 0.0611(17) Uani 1 1 d . . . . .
C35 C 0.1632(5) 0.4279(9) 0.5479(3) 0.130 Uani 1 1 d . . . . .
H35A H 0.147069 0.361522 0.550027 0.195 Uiso 1 1 calc R U . . .
H35B H 0.159594 0.449949 0.520833 0.195 Uiso 1 1 calc R U . . .
H35C H 0.143328 0.474016 0.564256 0.195 Uiso 1 1 calc R U . . .
C36 C 0.3694(3) 0.3955(5) 0.55890(19) 0.0612(17) Uani 1 1 d . . . . .
C37 C 0.1529(3) 0.5997(6) 0.6268(2) 0.0657(18) Uani 1 1 d . . . . .
C38 C 0.2403(7) 0.5288(10) 0.7240(4) 0.170(5) Uani 1 1 d . U . . .
H38A H 0.199655 0.519290 0.721664 0.255 Uiso 1 1 calc R U . . .
H38B H 0.249228 0.597911 0.718282 0.255 Uiso 1 1 calc R U . . .
H38C H 0.254157 0.512699 0.750532 0.255 Uiso 1 1 calc DR U . . .
Cl1 Cl 0.33259(11) 0.31546(19) 0.78215(7) 0.0925(6) Uani 1 1 d . . . . .
Cl2 Cl 0.52932(8) 0.46256(16) 0.59174(6) 0.0766(5) Uani 1 1 d . . . . .
Cl3 Cl 0.26837(14) 0.3725(2) 0.45330(8) 0.1109(8) Uani 1 1 d D . . . .
N1 N 0.3949(4) 0.7289(6) 0.6444(2) 0.103(2) Uani 1 1 d . . . . .
N2 N 0.3775(2) 0.4649(5) 0.66272(16) 0.0692(16) Uani 1 1 d . . . . .
N3 N 0.3131(3) 0.2950(5) 0.65967(15) 0.0639(15) Uani 1 1 d . . . . .
N4 N 0.1749(4) 0.1828(6) 0.6502(2) 0.102(2) Uani 1 1 d . . . . .
N5 N 0.3970(2) 0.3264(5) 0.54056(18) 0.0727(17) Uani 1 1 d . . . . .
N6 N 0.3242(2) 0.5526(4) 0.56346(15) 0.0570(13) Uani 1 1 d . . . . .
N7 N 0.2310(2) 0.6375(4) 0.59032(16) 0.0575(13) Uani 1 1 d . . . . .
N8 N 0.0975(3) 0.6016(5) 0.6312(2) 0.0838(19) Uani 1 1 d . . . . .
O1 O 0.3188(2) 0.6238(4) 0.64788(14) 0.0725(13) Uani 1 1 d . . . . .
O2 O 0.2121(2) 0.3259(4) 0.63154(17) 0.0787(14) Uani 1 1 d . . . . .
O3 O 0.3411(2) 0.3734(3) 0.58843(13) 0.0640(12) Uani 1 1 d . . . . .
O4 O 0.1841(2) 0.5324(4) 0.64299(16) 0.0784(14) Uani 1 1 d . . . . .
O5 O 0.2653(3) 0.4680(4) 0.69834(15) 0.0890(17) Uani 1 1 d . U . . .
H5A H 0.250116 0.411024 0.702694 0.107 Uiso 1 1 d DR U . . .
O6 O 0.2216(2) 0.4251(4) 0.56064(15) 0.0803(14) Uani 1 1 d . . . . .
H6A H 0.237240 0.462959 0.543980 0.096 Uiso 1 1 d R U . . .
O7 O 0.3647(4) 0.3979(7) 0.7687(3) 0.161(3) Uani 1 1 d . . . . .
O8 O 0.3671(5) 0.2391(8) 0.7947(4) 0.216(5) Uani 1 1 d . . . . .
O9 O 0.2972(4) 0.3479(8) 0.8118(2) 0.169(4) Uani 1 1 d . . . . .
O10 O 0.2969(4) 0.2829(7) 0.7502(2) 0.154(3) Uani 1 1 d . . . . .
O11 O 0.5695(3) 0.4489(6) 0.6241(2) 0.115(2) Uani 1 1 d . . . . .
O12 O 0.5233(5) 0.5630(7) 0.5837(4) 0.207(5) Uani 1 1 d . . . . .
O13 O 0.5448(4) 0.4115(9) 0.5592(2) 0.189(5) Uani 1 1 d . . . . .
O14 O 0.4754(3) 0.4346(9) 0.6017(2) 0.173(4) Uani 1 1 d . . . . .
O15 O 0.2815(4) 0.4298(5) 0.48592(19) 0.140(3) Uani 1 1 d D . . . .
O16 O 0.2331(6) 0.2964(9) 0.4614(4) 0.329(10) Uani 1 1 d D . . . .
O17 O 0.2439(7) 0.4244(8) 0.4231(3) 0.267(8) Uani 1 1 d D . . . .
O18 O 0.3171(5) 0.3285(13) 0.4424(4) 0.318(8) Uani 1 1 d D U . . .
Th1 Th 0.27398(2) 0.46662(2) 0.62491(2) 0.05330(10) Uani 1 1 d . . . . .
Cl4 Cl 0.9967(5) 0.4441(8) 0.5382(4) 0.526(7) Uani 1 1 d D U . . .
O20 O 1.0312(11) 0.3664(17) 0.5682(8) 0.573(7) Uani 1 1 d D U . . .
O19 O 0.9436(10) 0.4888(18) 0.5598(8) 0.574(7) Uani 1 1 d D U . . .
O22 O 1.0402(10) 0.5293(16) 0.5262(9) 0.576(10) Uani 1 1 d D U . . .
O21 O 0.9756(13) 0.3785(18) 0.5001(7) 0.597 Uani 1 1 d D U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.482(13) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 N1 1.516(13) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 O1 1.251(9) . ?
C3 N1 1.356(11) . ?
C3 C4 1.476(12) . ?
C4 N2 1.321(10) . ?
C4 C5 1.413(11) . ?
C5 C6 1.324(13) . ?
C5 H5 0.9300 . ?
C6 C7 1.372(13) . ?
C6 H6 0.9300 . ?
C7 C17 1.416(10) . ?
C7 C8 1.432(15) . ?
C8 C9 1.314(15) . ?
C8 H8 0.9300 . ?
C9 C10 1.477(14) . ?
C9 H9 0.9300 . ?
C10 C11 1.336(15) . ?
C10 C18 1.404(11) . ?
C11 C12 1.349(15) . ?
C11 H11 0.9300 . ?
C12 C13 1.425(11) . ?
C12 H12 0.9300 . ?
C13 N3 1.329(10) . ?
C13 C14 1.476(11) . ?
C14 O2 1.265(9) . ?
C14 N4 1.302(10) . ?
C15 N4 1.451(12) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 N4 1.477(13) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 N2 1.341(9) . ?
C17 C18 1.441(11) . ?
C18 N3 1.358(9) . ?
C19 N5 1.470(10) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 N5 1.449(11) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 N6 1.337(8) . ?
C21 C22 1.412(11) . ?
C21 C36 1.496(10) . ?
C22 C23 1.358(11) . ?
C22 H22 0.9300 . ?
C23 C24 1.382(11) . ?
C23 H23 0.9300 . ?
C24 C34 1.409(10) . ?
C24 C25 1.413(11) . ?
C25 C26 1.336(12) . ?
C25 H25 0.9300 . ?
C26 C27 1.452(12) . ?
C26 H26 0.9300 . ?
C27 C28 1.410(11) . ?
C27 C33 1.423(10) . ?
C28 C29 1.347(12) . ?
C28 H28 0.9300 . ?
C29 C30 1.398(10) . ?
C29 H29 0.9300 . ?
C30 N7 1.344(8) . ?
C30 C37 1.490(10) . ?
C31 N8 1.464(11) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 N8 1.470(10) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 N7 1.323(9) . ?
C33 C34 1.417(9) . ?
C34 N6 1.356(8) . ?
C35 O6 1.413(11) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 O3 1.260(8) . ?
C36 N5 1.295(8) . ?
C37 O4 1.258(8) . ?
C37 N8 1.315(8) . ?
C38 O5 1.340(12) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
Cl1 O8 1.348(9) . ?
Cl1 O9 1.402(8) . ?
Cl1 O10 1.400(8) . ?
Cl1 O7 1.414(8) . ?
Cl2 O13 1.354(7) . ?
Cl2 O12 1.362(9) . ?
Cl2 O14 1.376(7) . ?
Cl2 O11 1.415(6) . ?
Cl3 O17 1.333(8) . ?
Cl3 O16 1.340(9) . ?
Cl3 O18 1.349(10) . ?
Cl3 O15 1.360(6) . ?
N2 Th1 2.681(6) . ?
N3 Th1 2.694(6) . ?
N6 Th1 2.692(6) . ?
N7 Th1 2.714(5) . ?
O1 Th1 2.438(5) . ?
O2 Th1 2.377(5) . ?
O3 Th1 2.392(4) . ?
O4 Th1 2.389(5) . ?
O5 Th1 2.500(5) . ?
O5 H5A 0.8499 . ?
O6 Th1 2.498(5) . ?
O6 H6A 0.8500 . ?
Cl4 O22 1.588(18) . ?
Cl4 O19 1.590(18) . ?
Cl4 O21 1.607(18) . ?
Cl4 O20 1.630(18) . ?
O22 O21 1.54(3) 5_766 ?

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
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O1 C3 N1 120.8(8) . . ?
O1 C3 C4 116.2(8) . . ?
N1 C3 C4 122.9(8) . . ?
N2 C4 C5 120.4(9) . . ?
N2 C4 C3 112.2(7) . . ?
C5 C4 C3 127.2(8) . . ?
C6 C5 C4 120.6(10) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C7 119.9(9) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C6 C7 C17 117.9(9) . . ?
C6 C7 C8 125.0(9) . . ?
C17 C7 C8 117.1(11) . . ?
C9 C8 C7 122.1(10) . . ?
C9 C8 H8 119.0 . . ?
C7 C8 H8 119.0 . . ?
C8 C9 C10 123.4(10) . . ?
C8 C9 H9 118.3 . . ?
C10 C9 H9 118.3 . . ?
C11 C10 C18 117.5(9) . . ?
C11 C10 C9 127.1(10) . . ?
C18 C10 C9 115.4(11) . . ?
C10 C11 C12 123.6(10) . . ?
C10 C11 H11 118.2 . . ?
C12 C11 H11 118.2 . . ?
C11 C12 C13 117.3(10) . . ?
C11 C12 H12 121.4 . . ?
C13 C12 H12 121.4 . . ?
N3 C13 C12 120.4(9) . . ?
N3 C13 C14 112.0(7) . . ?
C12 C13 C14 127.6(9) . . ?
O2 C14 N4 117.1(8) . . ?
O2 C14 C13 115.6(8) . . ?
N4 C14 C13 127.3(8) . . ?
N4 C15 H15A 109.5 . . ?
N4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N4 C16 H16A 109.5 . . ?
N4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C17 C7 121.4(9) . . ?
N2 C17 C18 117.8(6) . . ?
C7 C17 C18 120.8(8) . . ?
N3 C18 C10 120.8(9) . . ?
N3 C18 C17 118.1(6) . . ?
C10 C18 C17 121.0(8) . . ?
N5 C19 H19A 109.5 . . ?
N5 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N5 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N5 C20 H20A 109.5 . . ?
N5 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N5 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N6 C21 C22 120.6(7) . . ?
N6 C21 C36 111.3(6) . . ?
C22 C21 C36 128.0(7) . . ?
C23 C22 C21 119.8(7) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C24 120.8(8) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
C23 C24 C34 116.6(8) . . ?
C23 C24 C25 124.5(8) . . ?
C34 C24 C25 118.9(7) . . ?
C26 C25 C24 121.9(8) . . ?
C26 C25 H25 119.1 . . ?
C24 C25 H25 119.1 . . ?
C25 C26 C27 120.3(8) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C28 C27 C33 116.1(8) . . ?
C28 C27 C26 124.2(8) . . ?
C33 C27 C26 119.7(7) . . ?
C29 C28 C27 121.1(8) . . ?
C29 C28 H28 119.5 . . ?
C27 C28 H28 119.5 . . ?
C28 C29 C30 118.9(7) . . ?
C28 C29 H29 120.5 . . ?
C30 C29 H29 120.5 . . ?
N7 C30 C29 121.7(7) . . ?
N7 C30 C37 109.3(6) . . ?
C29 C30 C37 128.9(6) . . ?
N8 C31 H31A 109.5 . . ?
N8 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N8 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N8 C32 H32A 109.5 . . ?
N8 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N8 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N7 C33 C34 119.8(6) . . ?
N7 C33 C27 122.5(6) . . ?
C34 C33 C27 117.7(7) . . ?
N6 C34 C24 123.0(6) . . ?
N6 C34 C33 115.5(6) . . ?
C24 C34 C33 121.5(7) . . ?
O6 C35 H35A 109.5 . . ?
O6 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O6 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O3 C36 N5 120.8(7) . . ?
O3 C36 C21 114.9(6) . . ?
N5 C36 C21 124.3(7) . . ?
O4 C37 N8 121.1(8) . . ?
O4 C37 C30 116.4(6) . . ?
N8 C37 C30 122.4(7) . . ?
O5 C38 H38A 109.5 . . ?
O5 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O5 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O8 Cl1 O9 111.9(7) . . ?
O8 Cl1 O10 109.6(7) . . ?
O9 Cl1 O10 107.1(6) . . ?
O8 Cl1 O7 111.0(7) . . ?
O9 Cl1 O7 109.8(6) . . ?
O10 Cl1 O7 107.2(6) . . ?
O13 Cl2 O12 110.7(8) . . ?
O13 Cl2 O14 110.7(6) . . ?
O12 Cl2 O14 103.0(7) . . ?
O13 Cl2 O11 111.5(5) . . ?
O12 Cl2 O11 109.6(6) . . ?
O14 Cl2 O11 111.0(5) . . ?
O17 Cl3 O16 107.4(7) . . ?
O17 Cl3 O18 110.5(8) . . ?
O16 Cl3 O18 105.8(8) . . ?
O17 Cl3 O15 113.7(6) . . ?
O16 Cl3 O15 111.6(7) . . ?
O18 Cl3 O15 107.6(6) . . ?
C3 N1 C1 126.5(9) . . ?
C3 N1 C2 116.9(9) . . ?
C1 N1 C2 116.3(9) . . ?
C4 N2 C17 119.4(7) . . ?
C4 N2 Th1 118.9(5) . . ?
C17 N2 Th1 121.6(5) . . ?
C13 N3 C18 120.2(7) . . ?
C13 N3 Th1 118.9(5) . . ?
C18 N3 Th1 119.9(5) . . ?
C14 N4 C15 120.3(8) . . ?
C14 N4 C16 123.8(10) . . ?
C15 N4 C16 115.9(9) . . ?
C36 N5 C20 118.7(7) . . ?
C36 N5 C19 127.4(8) . . ?
C20 N5 C19 113.9(7) . . ?
C21 N6 C34 118.7(6) . . ?
C21 N6 Th1 119.0(5) . . ?
C34 N6 Th1 121.1(4) . . ?
C33 N7 C30 119.6(6) . . ?
C33 N7 Th1 119.5(4) . . ?
C30 N7 Th1 119.2(4) . . ?
C37 N8 C31 117.8(7) . . ?
C37 N8 C32 126.1(8) . . ?
C31 N8 C32 116.1(7) . . ?
C3 O1 Th1 125.7(5) . . ?
C14 O2 Th1 132.3(5) . . ?
C36 O3 Th1 132.5(4) . . ?
C37 O4 Th1 130.2(5) . . ?
C38 O5 Th1 135.1(7) . . ?
C38 O5 H5A 102.6 . . ?
Th1 O5 H5A 102.8 . . ?
C35 O6 Th1 133.0(6) . . ?
C35 O6 H6A 103.1 . . ?
Th1 O6 H6A 103.7 . . ?
O2 Th1 O4 73.19(18) . . ?
O2 Th1 O3 93.78(17) . . ?
O4 Th1 O3 158.88(18) . . ?
O2 Th1 O1 153.19(18) . . ?
O4 Th1 O1 88.77(18) . . ?
O3 Th1 O1 108.65(17) . . ?
O2 Th1 O6 68.65(19) . . ?
O4 Th1 O6 84.44(18) . . ?
O3 Th1 O6 75.23(16) . . ?
O1 Th1 O6 130.36(18) . . ?
O2 Th1 O5 80.2(2) . . ?
O4 Th1 O5 67.94(18) . . ?
O3 Th1 O5 127.26(16) . . ?
O1 Th1 O5 74.58(19) . . ?
O6 Th1 O5 143.4(2) . . ?
O2 Th1 N2 119.29(19) . . ?
O4 Th1 N2 132.02(18) . . ?
O3 Th1 N2 68.76(16) . . ?
O1 Th1 N2 59.48(18) . . ?
O6 Th1 N2 143.38(17) . . ?
O5 Th1 N2 69.28(19) . . ?
O2 Th1 N6 134.20(17) . . ?
O4 Th1 N6 118.07(16) . . ?
O3 Th1 N6 59.62(16) . . ?
O1 Th1 N6 71.72(16) . . ?
O6 Th1 N6 68.72(17) . . ?
O5 Th1 N6 145.48(19) . . ?
N2 Th1 N6 87.11(17) . . ?
O2 Th1 N3 59.61(18) . . ?
O4 Th1 N3 118.67(18) . . ?
O3 Th1 N3 64.69(16) . . ?
O1 Th1 N3 116.70(18) . . ?
O6 Th1 N3 109.50(18) . . ?
O5 Th1 N3 67.50(17) . . ?
N2 Th1 N3 60.5(2) . . ?
N6 Th1 N3 122.67(16) . . ?
O2 Th1 N7 118.56(17) . . ?
O4 Th1 N7 59.60(17) . . ?
O3 Th1 N7 116.55(16) . . ?
O1 Th1 N7 64.57(16) . . ?
O6 Th1 N7 69.79(17) . . ?
O5 Th1 N7 111.92(17) . . ?
N2 Th1 N7 121.23(19) . . ?
N6 Th1 N7 58.91(16) . . ?
N3 Th1 N7 178.07(18) . . ?
O22 Cl4 O19 112.4(9) . . ?
O22 Cl4 O21 110.7(11) . . ?
O19 Cl4 O21 110.8(10) . . ?
O22 Cl4 O20 107.5(10) . . ?
O19 Cl4 O20 108.9(10) . . ?
O21 Cl4 O20 106.2(9) . . ?
O21 O22 Cl4 125(2) 5_766 . ?
O22 O21 Cl4 95.1(19) 5_766 . ?

_refine_diff_density_max         1.530
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.089



_vrf_PLAT260_Th_TMPhenDA         
;
PROBLEM: Large Average Ueq of Residue Including Cl4 0.569 Check
RESPONSE: It is caused by heavy disorder of perchlorate.
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