# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_200716qzh_3_0m_sq
_database_code_depnum_ccdc_archive 'CCDC 2067961'
loop_
_audit_author_name
_audit_author_address
'Zi-Jian Li'
;Shanghai Institute of Applied Physics, CAS
China
;
_audit_update_record             
;
2021-03-04 deposited with the CCDC.	2021-04-19 downloaded from the CCDC.
;
_audit_creation_date             2020-07-22
_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         '0.5(C68 H36 O16 Th2)'
_chemical_formula_sum            'C34 H18 O8 Th'
_chemical_formula_weight         786.52
_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 0.0148 0.0070 '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'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -3.9342 9.9644 '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                   5.640(3)
_cell_length_b                   11.024(6)
_cell_length_c                   28.315(15)
_cell_angle_alpha                90
_cell_angle_beta                 92.102(12)
_cell_angle_gamma                90
_cell_volume                     1759.3(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.911
_cell_measurement_theta_min      3.063
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.221
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1585 before and 0.1031 after correction. The Ratio of minimum to maximum transmission is 0.6103. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.006
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.003
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.1094
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3260
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.186
_diffrn_reflns_theta_min         7.837
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2367
_reflns_number_total             3260
_reflns_special_details          
;
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 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         4.030
_refine_diff_density_min         -3.269
_refine_diff_density_rms         0.275
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3260
_refine_ls_number_restraints     109
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.0970
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1410P)²+18.4174P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2586
_refine_ls_wR_factor_ref         0.2768
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.617(5)
 0.383(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C17-C14
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim O1 \\sim O2:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim O4: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
O3 \\sim C17 \\sim O4 \\sim C14: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C7(H7), C6(H6), C9(H9), C12(H12), C13(H13), C15(H15), C16(H16)
5.b Fitted hexagon refined as free rotating group:
 C5(C4,C3,C2,C7,C6), C11(C12,C13,C14,C15,C16)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Th1 Th 0.7500 0.52520(9) 0.7500 0.0604(4) Uani 1 2 d S T P . .
O1 O 0.709(3) 0.6437(13) 0.6739(5) 0.073(3) Uani 1 1 d . U . . .
O2 O 0.996(3) 0.6995(12) 0.7297(6) 0.068(3) Uani 1 1 d . U . . .
C1 C 0.894(5) 0.705(2) 0.6862(9) 0.076(3) Uani 1 1 d . U . . .
C5 C 1.239(3) 0.8937(15) 0.5774(5) 0.079(4) Uani 1 1 d . U . . .
C4 C 1.022(3) 0.8376(16) 0.5678(4) 0.083(4) Uani 1 1 d G U . . .
H4 H 0.9525 0.8414 0.5376 0.099 Uiso 1 1 calc R . . . .
C3 C 0.909(3) 0.7759(16) 0.6035(6) 0.082(4) Uani 1 1 d G U . . .
H3 H 0.7641 0.7384 0.5971 0.098 Uiso 1 1 calc R . . . .
C2 C 1.014(3) 0.7703(15) 0.6487(5) 0.080(4) Uani 1 1 d G U . . .
C7 C 1.231(3) 0.8264(15) 0.6582(4) 0.080(4) Uani 1 1 d G U . . .
H7 H 1.3008 0.8226 0.6885 0.096 Uiso 1 1 calc R . . . .
C6 C 1.344(2) 0.8881(14) 0.6226(5) 0.078(4) Uani 1 1 d G U . . .
H6 H 1.4891 0.9256 0.6290 0.093 Uiso 1 1 calc R . . . .
C8 C 1.382(4) 0.9552(18) 0.5383(8) 0.066(6) Uani 1 1 d . . . . .
C9 C 1.431(5) 0.883(2) 0.5013(9) 0.077(7) Uani 1 1 d . . . . .
H9 H 1.3772 0.8030 0.5016 0.093 Uiso 1 1 calc R . . . .
C10 C 1.440(4) 1.077(2) 0.5381(9) 0.069(6) Uani 1 1 d . . . . .
C11 C 1.382(3) 1.1625(12) 0.5774(5) 0.071(4) Uani 1 1 d . U . . .
C12 C 1.552(2) 1.2484(13) 0.5909(5) 0.069(4) Uani 1 1 d G U . . .
H12 H 1.6978 1.2493 0.5767 0.083 Uiso 1 1 calc R . . . .
C13 C 1.503(2) 1.3330(12) 0.6257(6) 0.073(4) Uani 1 1 d G U . . .
H13 H 1.6167 1.3905 0.6347 0.088 Uiso 1 1 calc R . . . .
C14 C 1.285(3) 1.3317(12) 0.6469(5) 0.071(3) Uani 1 1 d DG U . . .
C15 C 1.115(2) 1.2458(13) 0.6334(5) 0.075(4) Uani 1 1 d G U . . .
H15 H 0.9691 1.2449 0.6476 0.090 Uiso 1 1 calc R . . . .
C16 C 1.164(2) 1.1612(12) 0.5987(6) 0.074(4) Uani 1 1 d G U . . .
H16 H 1.0502 1.1037 0.5896 0.089 Uiso 1 1 calc R . . . .
O4 O 1.400(3) 1.4692(14) 0.7049(5) 0.066(3) Uani 1 1 d . U . . .
O3 O 1.021(3) 1.4400(16) 0.6933(6) 0.077(4) Uani 1 1 d . U . . .
C17 C 1.227(4) 1.4244(18) 0.6826(7) 0.066(3) 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
Th1 O1 2.524(14) . ?
Th1 O1 2.524(15) 2_656 ?
Th1 O2 2.451(13) 2_656 ?
Th1 O2 2.451(13) . ?
Th1 C1 2.82(2) 2_656 ?
Th1 C1 2.82(2) . ?
Th1 O4 2.390(15) 2_746 ?
Th1 O4 2.390(15) 1_445 ?
Th1 O3 2.443(14) 2_646 ?
Th1 O3 2.443(14) 1_545 ?
O1 C1 1.28(3) . ?
O2 C1 1.34(3) . ?
C1 C2 1.47(2) . ?
C5 C4 1.3900 . ?
C5 C6 1.3900 . ?
C5 C8 1.55(2) . ?
C4 C3 1.3900 . ?
C3 C2 1.3900 . ?
C2 C7 1.3900 . ?
C7 C6 1.3900 . ?
C8 C9 1.35(3) . ?
C8 C10 1.38(3) . ?
C9 C10 1.43(3) 3_876 ?
C10 C9 1.43(3) 3_876 ?
C10 C11 1.50(3) . ?
C11 C12 1.3900 . ?
C11 C16 1.3900 . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C14 C15 1.3900 . ?
C14 C17 1.481(15) . ?
C15 C16 1.3900 . ?
O4 Th1 2.390(15) 1_665 ?
O4 C17 1.25(3) . ?
O3 Th1 2.443(14) 1_565 ?
O3 C17 1.23(3) . ?

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 117.7(7) 2_656 . ?
O1 Th1 C1 99.5(7) 2_656 . ?
O1 Th1 C1 27.0(7) . . ?
O1 Th1 C1 99.5(7) . 2_656 ?
O1 Th1 C1 27.0(7) 2_656 2_656 ?
O2 Th1 O1 76.1(5) 2_656 . ?
O2 Th1 O1 55.2(5) . . ?
O2 Th1 O1 55.2(5) 2_656 2_656 ?
O2 Th1 O1 76.1(5) . 2_656 ?
O2 Th1 O2 76.7(8) 2_656 . ?
O2 Th1 C1 28.4(6) 2_656 2_656 ?
O2 Th1 C1 28.4(6) . . ?
O2 Th1 C1 77.2(7) 2_656 . ?
O2 Th1 C1 77.2(7) . 2_656 ?
C1 Th1 C1 90.9(11) 2_656 . ?
O4 Th1 O1 68.3(5) 1_445 . ?
O4 Th1 O1 129.6(5) 2_746 . ?
O4 Th1 O1 129.6(5) 1_445 2_656 ?
O4 Th1 O1 68.3(5) 2_746 2_656 ?
O4 Th1 O2 82.2(6) 1_445 2_656 ?
O4 Th1 O2 82.2(6) 2_746 . ?
O4 Th1 O2 122.8(5) 1_445 . ?
O4 Th1 O2 122.8(6) 2_746 2_656 ?
O4 Th1 C1 105.7(7) 1_445 2_656 ?
O4 Th1 C1 95.2(7) 2_746 2_656 ?
O4 Th1 C1 105.7(7) 2_746 . ?
O4 Th1 C1 95.2(7) 1_445 . ?
O4 Th1 O4 150.0(8) 1_445 2_746 ?
O4 Th1 O3 74.3(5) 2_746 1_545 ?
O4 Th1 O3 94.2(5) 2_746 2_646 ?
O4 Th1 O3 94.2(5) 1_445 1_545 ?
O4 Th1 O3 74.3(5) 1_445 2_646 ?
O3 Th1 O1 71.2(6) 1_545 . ?
O3 Th1 O1 71.2(6) 2_646 2_656 ?
O3 Th1 O1 136.1(6) 2_646 . ?
O3 Th1 O1 136.1(6) 1_545 2_656 ?
O3 Th1 O2 145.9(6) 1_545 2_656 ?
O3 Th1 O2 77.0(6) 1_545 . ?
O3 Th1 O2 77.0(6) 2_646 2_656 ?
O3 Th1 O2 145.9(6) 2_646 . ?
O3 Th1 C1 153.2(7) 2_646 . ?
O3 Th1 C1 69.3(7) 2_646 2_656 ?
O3 Th1 C1 69.3(7) 1_545 . ?
O3 Th1 C1 153.2(8) 1_545 2_656 ?
O3 Th1 O3 134.8(9) 1_545 2_646 ?
C1 O1 Th1 89.4(14) . . ?
C1 O2 Th1 91.2(12) . . ?
O1 C1 Th1 63.6(11) . . ?
O1 C1 O2 123(2) . . ?
O1 C1 C2 117(2) . . ?
O2 C1 Th1 60.4(10) . . ?
O2 C1 C2 120(2) . . ?
C2 C1 Th1 163.7(18) . . ?
C4 C5 C6 120.0 . . ?
C4 C5 C8 122.1(13) . . ?
C6 C5 C8 117.7(13) . . ?
C3 C4 C5 120.0 . . ?
C4 C3 C2 120.0 . . ?
C3 C2 C1 119.9(15) . . ?
C7 C2 C1 120.1(15) . . ?
C7 C2 C3 120.0 . . ?
C2 C7 C6 120.0 . . ?
C7 C6 C5 120.0 . . ?
C9 C8 C5 114.9(19) . . ?
C9 C8 C10 121(2) . . ?
C10 C8 C5 123.9(18) . . ?
C8 C9 C10 123(2) . 3_876 ?
C8 C10 C9 116(2) . 3_876 ?
C8 C10 C11 123(2) . . ?
C9 C10 C11 121(2) 3_876 . ?
C12 C11 C10 117.6(13) . . ?
C12 C11 C16 120.0 . . ?
C16 C11 C10 122.3(13) . . ?
C11 C12 C13 120.0 . . ?
C14 C13 C12 120.0 . . ?
C13 C14 C15 120.0 . . ?
C13 C14 C17 120.5(13) . . ?
C15 C14 C17 119.4(13) . . ?
C14 C15 C16 120.0 . . ?
C15 C16 C11 120.0 . . ?
C17 O4 Th1 171.7(15) . 1_665 ?
C17 O3 Th1 146.9(15) . 1_565 ?
O4 C17 C14 115.6(18) . . ?
O3 C17 C14 119.9(19) . . ?
O3 C17 O4 123.6(16) . . ?

_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.045 0.500 0.000 161 38 ' '
2 0.047 0.929 0.250 131 41 ' '
3 -0.024 0.500 0.500 161 38 ' '
4 -0.091 0.071 0.750 131 41 ' '

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.617(5)
2 0.383(5)

####################################################################### 
# 
# 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_200716qzh_1_0m_sq
_database_code_depnum_ccdc_archive 'CCDC 2067963'
loop_
_audit_author_name
_audit_author_address
'Zi-Jian Li'
;Shanghai Institute of Applied Physics, CAS
China
;
_audit_update_record             
;
2021-03-04 deposited with the CCDC.	2021-04-19 downloaded from the CCDC.
;
_audit_creation_date             2020-07-23
_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         'C37 H27 N O10 Th'
_chemical_formula_sum            'C37 H27 N O10 Th'
_chemical_formula_weight         877.63
_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 0.0148 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -3.9342 9.9644 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.0770(15)
_cell_length_b                   31.421(4)
_cell_length_c                   14.830(2)
_cell_angle_alpha                90
_cell_angle_beta                 112.117(4)
_cell_angle_gamma                90
_cell_volume                     5213.5(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      54.911
_cell_measurement_theta_min      7.71
_shelx_estimated_absorpt_T_max   0.981
_shelx_estimated_absorpt_T_min   0.963
_exptl_absorpt_coefficient_mu    6.275
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1585 before and 0.1031 after correction. The Ratio of minimum to maximum transmission is 0.6103. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.006
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.003
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0832
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            44198
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.998
_diffrn_reflns_theta_min         3.054
_diffrn_ambient_temperature      189.7
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6461
_reflns_number_total             9616
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 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         3.893
_refine_diff_density_min         -2.290
_refine_diff_density_rms         0.234
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         9616
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_gt           0.0949
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1823P)²+20.0120P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2562
_refine_ls_wR_factor_ref         0.2882
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Rotating group:
 O9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C12(H12), C15(H15), C16(H16),
 C18(H18), C19(H19), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28), C29(H29),
  C31(H31), C32(H32), C35(H35)
2.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C)
;
_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 0.19337(4) -0.01290(2) 1.11805(4) 0.0630(2) Uani 1 1 d . . . . .
O1 O 0.1466(8) 0.0482(3) 1.0070(7) 0.067(2) Uani 1 1 d . . . . .
O2 O -0.0236(9) 0.0513(3) 0.8791(9) 0.078(3) Uani 1 1 d . . . . .
O3 O 0.6030(9) 0.0489(3) 0.7913(9) 0.082(3) Uani 1 1 d . . . . .
O4 O 0.7556(9) 0.0896(3) 0.8762(9) 0.081(3) Uani 1 1 d . . . . .
O5 O 0.5831(9) 0.4624(3) 0.6797(8) 0.078(3) Uani 1 1 d . . . . .
O6 O 0.4202(9) 0.4622(3) 0.5440(8) 0.073(2) Uani 1 1 d . . . . .
O7 O -0.0713(16) 0.4718(5) 0.8620(10) 0.120(5) Uani 1 1 d . . . . .
O8 O -0.1670(9) 0.4595(3) 0.7034(8) 0.077(3) Uani 1 1 d . . . . .
O9 O 0.2343(11) -0.0276(4) 1.2923(9) 0.093(3) Uani 1 1 d . . . . .
H9A H 0.2743 -0.0507 1.3194 0.140 Uiso 1 1 d GR . . . .
H9B H 0.1759 -0.0336 1.3123 0.140 Uiso 1 1 d GR . . . .
O10 O 0.3243(10) -0.0142(4) 1.0230(10) 0.081(3) Uani 1 1 d . . . . .
N1 N 0.3630(15) -0.0192(5) 0.8851(13) 0.102(5) Uani 1 1 d . . . . .
C1 C 0.0755(12) 0.0649(4) 0.9324(11) 0.060(3) Uani 1 1 d . . . . .
C2 C 0.1132(13) 0.1082(4) 0.9096(11) 0.069(4) Uani 1 1 d . . . . .
C3 C 0.0361(13) 0.1328(5) 0.8357(12) 0.079(4) Uani 1 1 d . . . . .
H3 H -0.0439 0.1238 0.8016 0.095 Uiso 1 1 calc R . . . .
C4 C 0.0760(12) 0.1711(5) 0.8111(14) 0.085(5) Uani 1 1 d . . . . .
H4 H 0.0222 0.1874 0.7591 0.102 Uiso 1 1 calc R . . . .
C5 C 0.1895(12) 0.1862(4) 0.8589(13) 0.077(4) Uani 1 1 d . . . . .
C6 C 0.2677(12) 0.1600(4) 0.9348(11) 0.068(4) Uani 1 1 d . . . . .
H6 H 0.3481 0.1688 0.9682 0.081 Uiso 1 1 calc R . . . .
C7 C 0.2316(12) 0.1235(5) 0.9601(11) 0.069(4) Uani 1 1 d . . . . .
H7 H 0.2854 0.1074 1.0126 0.083 Uiso 1 1 calc R . . . .
C8 C 0.2387(11) 0.2265(4) 0.8352(12) 0.067(4) Uani 1 1 d . . . . .
C9 C 0.1690(12) 0.2622(4) 0.8207(13) 0.080(4) Uani 1 1 d . . . . .
H9 H 0.0941 0.2592 0.8270 0.096 Uiso 1 1 calc R . . . .
C10 C 0.1981(12) 0.3032(4) 0.7972(12) 0.072(4) Uani 1 1 d . . . . .
C11 C 0.3086(13) 0.3044(4) 0.7826(13) 0.077(4) Uani 1 1 d . . . . .
C12 C 0.3757(15) 0.2694(7) 0.7899(16) 0.108(7) Uani 1 1 d . . . . .
H12 H 0.4467 0.2718 0.7769 0.129 Uiso 1 1 calc R . . . .
C13 C 0.3446(13) 0.2293(4) 0.8162(12) 0.076(4) Uani 1 1 d . . . . .
C14 C 0.4183(14) 0.1912(4) 0.8155(12) 0.076(4) Uani 1 1 d . . . . .
C15 C 0.5407(13) 0.1948(4) 0.8696(13) 0.081(5) Uani 1 1 d . . . . .
H15 H 0.5731 0.2199 0.9054 0.097 Uiso 1 1 calc R . . . .
C16 C 0.6152(14) 0.1601(4) 0.8698(14) 0.090(5) Uani 1 1 d . . . . .
H16 H 0.6995 0.1626 0.9008 0.108 Uiso 1 1 calc R . . . .
C17 C 0.5626(13) 0.1209(4) 0.8227(13) 0.076(4) Uani 1 1 d . . . . .
C18 C 0.4437(16) 0.1195(5) 0.7733(13) 0.086(5) Uani 1 1 d . . . . .
H18 H 0.4093 0.0943 0.7389 0.103 Uiso 1 1 calc R . . . .
C19 C 0.3690(14) 0.1537(5) 0.7706(13) 0.081(4) Uani 1 1 d . . . . .
H19 H 0.2849 0.1510 0.7381 0.097 Uiso 1 1 calc R . . . .
C20 C 0.6446(13) 0.0845(6) 0.8304(12) 0.079(4) Uani 1 1 d . . . . .
C21 C 0.1234(13) 0.3402(5) 0.7938(13) 0.076(4) Uani 1 1 d . . . . .
C22 C 0.0067(14) 0.3426(4) 0.7313(12) 0.078(4) Uani 1 1 d . . . . .
H22 H -0.0296 0.3195 0.6890 0.093 Uiso 1 1 calc R . . . .
C23 C -0.0577(16) 0.3789(5) 0.7304(14) 0.085(5) Uani 1 1 d . . . . .
H23 H -0.1357 0.3812 0.6818 0.102 Uiso 1 1 calc R . . . .
C24 C -0.0186(15) 0.4103(5) 0.7920(14) 0.084(5) Uani 1 1 d . . . . .
C25 C 0.1005(16) 0.4101(6) 0.8568(14) 0.092(5) Uani 1 1 d . . . . .
H25 H 0.1309 0.4333 0.9001 0.111 Uiso 1 1 calc R . . . .
C26 C 0.1737(15) 0.3767(5) 0.8581(14) 0.085(5) Uani 1 1 d . . . . .
H26 H 0.2557 0.3771 0.8999 0.102 Uiso 1 1 calc R . . . .
C27 C 0.3490(13) 0.3440(4) 0.7473(13) 0.073(4) Uani 1 1 d . . . . .
C28 C 0.2837(12) 0.3594(5) 0.6527(14) 0.082(5) Uani 1 1 d . . . . .
H28 H 0.2101 0.3461 0.6149 0.099 Uiso 1 1 calc R . . . .
C29 C 0.3224(14) 0.3924(5) 0.6144(13) 0.081(4) Uani 1 1 d . . . . .
H29 H 0.2774 0.4016 0.5499 0.097 Uiso 1 1 calc R . . . .
C30 C 0.4295(13) 0.4130(5) 0.6702(12) 0.069(4) Uani 1 1 d . . . . .
C31 C 0.4917(17) 0.4000(6) 0.7606(15) 0.104(6) Uani 1 1 d . . . . .
H31 H 0.5612 0.4152 0.7994 0.125 Uiso 1 1 calc R . . . .
C32 C 0.4561(15) 0.3637(6) 0.8001(16) 0.101(6) Uani 1 1 d . . . . .
H32 H 0.5056 0.3531 0.8622 0.121 Uiso 1 1 calc R . . . .
C33 C 0.4807(15) 0.4485(4) 0.6264(14) 0.073(4) Uani 1 1 d . . . . .
C34 C -0.0883(15) 0.4509(4) 0.7852(15) 0.079(5) Uani 1 1 d . . . . .
C35 C 0.3128(16) -0.0043(6) 0.9397(19) 0.095(6) Uani 1 1 d . . . . .
H35 H 0.2576 0.0181 0.9118 0.114 Uiso 1 1 calc R . . . .
C36 C 0.4490(16) -0.0569(6) 0.9209(16) 0.106(6) Uani 1 1 d . . . . .
H36A H 0.4109 -0.0827 0.8858 0.159 Uiso 1 1 calc GR . . . .
H36B H 0.4691 -0.0610 0.9908 0.159 Uiso 1 1 calc GR . . . .
H36C H 0.5221 -0.0511 0.9091 0.159 Uiso 1 1 calc GR . . . .
C37 C 0.345(3) -0.0035(6) 0.7886(18) 0.116(8) Uani 1 1 d . . . . .
H37A H 0.2726 0.0140 0.7643 0.174 Uiso 1 1 calc GR . . . .
H37B H 0.3367 -0.0276 0.7446 0.174 Uiso 1 1 calc GR . . . .
H37C H 0.4141 0.0138 0.7917 0.174 Uiso 1 1 calc GR . . . .


_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 2.452(8) . ?
Th1 O2 2.393(9) 3_557 ?
Th1 O3 2.578(10) 3_657 ?
Th1 O4 2.481(10) 3_657 ?
Th1 O5 2.458(9) 4_566 ?
Th1 O6 2.405(12) 2_546 ?
Th1 O8 2.379(10) 4_666 ?
Th1 O9 2.485(12) . ?
Th1 O10 2.483(11) . ?
Th1 C20 2.889(16) 3_657 ?
O1 C1 1.234(16) . ?
O2 Th1 2.393(9) 3_557 ?
O2 C1 1.236(17) . ?
O3 Th1 2.578(10) 3_657 ?
O3 C20 1.27(2) . ?
O4 Th1 2.481(10) 3_657 ?
O4 C20 1.264(18) . ?
O5 Th1 2.458(9) 4_665 ?
O5 C33 1.268(19) . ?
O6 Th1 2.405(12) 2_556 ?
O6 C33 1.241(19) . ?
O7 C34 1.26(2) . ?
O8 Th1 2.379(10) 4_565 ?
O8 C34 1.26(2) . ?
O9 H9A 0.8795 . ?
O9 H9B 0.8826 . ?
O10 C35 1.23(3) . ?
N1 C35 1.27(3) . ?
N1 C36 1.53(2) . ?
N1 C37 1.45(3) . ?
C1 C2 1.514(17) . ?
C2 C3 1.38(2) . ?
C2 C7 1.424(19) . ?
C3 H3 0.9500 . ?
C3 C4 1.395(18) . ?
C4 H4 0.9500 . ?
C4 C5 1.37(2) . ?
C5 C6 1.43(2) . ?
C5 C8 1.496(17) . ?
C6 H6 0.9500 . ?
C6 C7 1.330(17) . ?
C7 H7 0.9500 . ?
C8 C9 1.370(19) . ?
C8 C13 1.413(17) . ?
C9 H9 0.9500 . ?
C9 C10 1.411(16) . ?
C10 C11 1.430(18) . ?
C10 C21 1.461(19) . ?
C11 C12 1.35(2) . ?
C11 C27 1.501(17) . ?
C12 H12 0.9500 . ?
C12 C13 1.41(2) . ?
C13 C14 1.492(18) . ?
C14 C15 1.40(2) . ?
C14 C19 1.38(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.413(17) . ?
C16 H16 0.9500 . ?
C16 C17 1.44(2) . ?
C17 C18 1.34(2) . ?
C17 C20 1.488(19) . ?
C18 H18 0.9500 . ?
C18 C19 1.39(2) . ?
C19 H19 0.9500 . ?
C20 Th1 2.889(16) 3_657 ?
C21 C22 1.37(2) . ?
C21 C26 1.47(2) . ?
C22 H22 0.9500 . ?
C22 C23 1.378(18) . ?
C23 H23 0.9500 . ?
C23 C24 1.31(3) . ?
C24 C25 1.40(2) . ?
C24 C34 1.511(18) . ?
C25 H25 0.9500 . ?
C25 C26 1.37(2) . ?
C26 H26 0.9500 . ?
C27 C28 1.41(2) . ?
C27 C32 1.38(2) . ?
C28 H28 0.9500 . ?
C28 C29 1.35(2) . ?
C29 H29 0.9500 . ?
C29 C30 1.40(2) . ?
C30 C31 1.33(2) . ?
C30 C33 1.535(19) . ?
C31 H31 0.9500 . ?
C31 C32 1.42(2) . ?
C32 H32 0.9500 . ?
C35 H35 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 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
O1 Th1 O3 128.8(3) . 3_657 ?
O1 Th1 O4 140.7(4) . 3_657 ?
O1 Th1 O5 74.0(3) . 4_566 ?
O1 Th1 O9 138.5(4) . . ?
O1 Th1 O10 70.5(4) . . ?
O1 Th1 C20 138.5(4) . 3_657 ?
O2 Th1 O1 115.1(3) 3_557 . ?
O2 Th1 O3 115.1(3) 3_557 3_657 ?
O2 Th1 O4 73.3(3) 3_557 3_657 ?
O2 Th1 O5 74.4(4) 3_557 4_566 ?
O2 Th1 O6 71.5(4) 3_557 2_546 ?
O2 Th1 O9 74.0(4) 3_557 . ?
O2 Th1 O10 137.3(4) 3_557 . ?
O2 Th1 C20 95.8(4) 3_557 3_657 ?
O3 Th1 C20 26.1(4) 3_657 3_657 ?
O4 Th1 O3 51.7(3) 3_657 3_657 ?
O4 Th1 O9 80.5(4) 3_657 . ?
O4 Th1 O10 78.5(4) 3_657 . ?
O4 Th1 C20 25.8(4) 3_657 3_657 ?
O5 Th1 O3 129.3(4) 4_566 3_657 ?
O5 Th1 O4 140.9(3) 4_566 3_657 ?
O5 Th1 O9 69.9(4) 4_566 . ?
O5 Th1 O10 140.5(4) 4_566 . ?
O5 Th1 C20 144.3(4) 4_566 3_657 ?
O6 Th1 O1 71.5(3) 2_546 . ?
O6 Th1 O3 116.8(3) 2_546 3_657 ?
O6 Th1 O4 76.0(4) 2_546 3_657 ?
O6 Th1 O5 113.4(4) 2_546 4_566 ?
O6 Th1 O9 142.5(4) 2_546 . ?
O6 Th1 O10 70.9(4) 2_546 . ?
O6 Th1 C20 94.9(4) 2_546 3_657 ?
O8 Th1 O1 75.1(4) 4_666 . ?
O8 Th1 O2 141.9(4) 4_666 3_557 ?
O8 Th1 O3 71.7(3) 4_666 3_657 ?
O8 Th1 O4 123.4(3) 4_666 3_657 ?
O8 Th1 O5 73.8(3) 4_666 4_566 ?
O8 Th1 O6 141.7(4) 4_666 2_546 ?
O8 Th1 O9 75.8(4) 4_666 . ?
O8 Th1 O10 80.7(4) 4_666 . ?
O8 Th1 C20 97.8(4) 4_666 3_657 ?
O9 Th1 O3 66.4(4) . 3_657 ?
O9 Th1 C20 74.4(4) . 3_657 ?
O10 Th1 O3 66.6(4) . 3_657 ?
O10 Th1 O9 131.9(4) . . ?
O10 Th1 C20 68.0(4) . 3_657 ?
C1 O1 Th1 147.4(8) . . ?
C1 O2 Th1 142.5(10) . 3_557 ?
C20 O3 Th1 90.7(9) . 3_657 ?
C20 O4 Th1 95.4(10) . 3_657 ?
C33 O5 Th1 121.8(10) . 4_665 ?
C33 O6 Th1 178.1(10) . 2_556 ?
C34 O8 Th1 142.4(9) . 4_565 ?
Th1 O9 H9A 119.2 . . ?
Th1 O9 H9B 121.2 . . ?
H9A O9 H9B 92.4 . . ?
C35 O10 Th1 135.3(11) . . ?
C35 N1 C36 119.2(19) . . ?
C35 N1 C37 125.1(18) . . ?
C37 N1 C36 115.7(14) . . ?
O1 C1 O2 127.3(12) . . ?
O1 C1 C2 114.7(13) . . ?
O2 C1 C2 117.9(13) . . ?
C3 C2 C1 120.8(13) . . ?
C3 C2 C7 118.3(12) . . ?
C7 C2 C1 120.8(13) . . ?
C2 C3 H3 120.1 . . ?
C2 C3 C4 119.7(14) . . ?
C4 C3 H3 120.1 . . ?
C3 C4 H4 118.7 . . ?
C5 C4 C3 122.7(14) . . ?
C5 C4 H4 118.7 . . ?
C4 C5 C6 116.5(12) . . ?
C4 C5 C8 125.4(14) . . ?
C6 C5 C8 118.1(12) . . ?
C5 C6 H6 119.0 . . ?
C7 C6 C5 122.0(13) . . ?
C7 C6 H6 119.0 . . ?
C2 C7 H7 119.6 . . ?
C6 C7 C2 120.8(13) . . ?
C6 C7 H7 119.6 . . ?
C9 C8 C5 117.1(11) . . ?
C9 C8 C13 117.8(12) . . ?
C13 C8 C5 124.7(11) . . ?
C8 C9 H9 116.9 . . ?
C8 C9 C10 126.2(12) . . ?
C10 C9 H9 116.9 . . ?
C9 C10 C11 113.2(12) . . ?
C9 C10 C21 121.8(12) . . ?
C11 C10 C21 124.9(10) . . ?
C10 C11 C27 121.3(12) . . ?
C12 C11 C10 122.3(12) . . ?
C12 C11 C27 116.1(13) . . ?
C11 C12 H12 118.8 . . ?
C11 C12 C13 122.5(14) . . ?
C13 C12 H12 118.8 . . ?
C8 C13 C14 122.6(12) . . ?
C12 C13 C8 117.7(13) . . ?
C12 C13 C14 119.5(12) . . ?
C15 C14 C13 116.0(13) . . ?
C19 C14 C13 122.7(14) . . ?
C19 C14 C15 121.2(13) . . ?
C14 C15 H15 120.8 . . ?
C14 C15 C16 118.4(14) . . ?
C16 C15 H15 120.8 . . ?
C15 C16 H16 120.1 . . ?
C15 C16 C17 119.7(14) . . ?
C17 C16 H16 120.1 . . ?
C16 C17 C20 117.4(14) . . ?
C18 C17 C16 118.5(13) . . ?
C18 C17 C20 124.1(14) . . ?
C17 C18 H18 118.7 . . ?
C17 C18 C19 122.5(15) . . ?
C19 C18 H18 118.7 . . ?
C14 C19 C18 119.3(15) . . ?
C14 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
O3 C20 Th1 63.2(8) . 3_657 ?
O3 C20 C17 120.2(14) . . ?
O4 C20 Th1 58.8(8) . 3_657 ?
O4 C20 O3 120.9(14) . . ?
O4 C20 C17 119.0(15) . . ?
C17 C20 Th1 169.5(12) . 3_657 ?
C10 C21 C26 120.1(14) . . ?
C22 C21 C10 122.1(15) . . ?
C22 C21 C26 117.8(14) . . ?
C21 C22 H22 120.5 . . ?
C21 C22 C23 119.0(16) . . ?
C23 C22 H22 120.5 . . ?
C22 C23 H23 117.8 . . ?
C24 C23 C22 124.4(18) . . ?
C24 C23 H23 117.8 . . ?
C23 C24 C25 119.0(15) . . ?
C23 C24 C34 123.1(17) . . ?
C25 C24 C34 116.9(17) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 C24 120.3(17) . . ?
C26 C25 H25 119.8 . . ?
C21 C26 H26 120.5 . . ?
C25 C26 C21 118.9(16) . . ?
C25 C26 H26 120.5 . . ?
C28 C27 C11 119.8(14) . . ?
C32 C27 C11 122.2(15) . . ?
C32 C27 C28 117.5(14) . . ?
C27 C28 H28 119.0 . . ?
C29 C28 C27 122.0(14) . . ?
C29 C28 H28 119.0 . . ?
C28 C29 H29 120.2 . . ?
C28 C29 C30 119.6(16) . . ?
C30 C29 H29 120.2 . . ?
C29 C30 C33 120.9(15) . . ?
C31 C30 C29 119.9(14) . . ?
C31 C30 C33 119.0(15) . . ?
C30 C31 H31 119.4 . . ?
C30 C31 C32 121.2(16) . . ?
C32 C31 H31 119.4 . . ?
C27 C32 C31 119.4(18) . . ?
C27 C32 H32 120.3 . . ?
C31 C32 H32 120.3 . . ?
O5 C33 C30 116.1(16) . . ?
O6 C33 O5 124.7(13) . . ?
O6 C33 C30 119.1(14) . . ?
O7 C34 C24 118.8(17) . . ?
O8 C34 O7 124.4(13) . . ?
O8 C34 C24 116.5(15) . . ?
O10 C35 N1 130(2) . . ?
O10 C35 H35 114.8 . . ?
N1 C35 H35 114.8 . . ?
N1 C36 H36A 109.5 . . ?
N1 C36 H36B 109.5 . . ?
N1 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N1 C37 H37A 109.5 . . ?
N1 C37 H37B 109.5 . . ?
N1 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_a_sq
_database_code_depnum_ccdc_archive 'CCDC 2067962'
loop_
_audit_author_name
_audit_author_address
'Zi-Jian Li'
;Shanghai Institute of Applied Physics, CAS
China
;
_audit_update_record             
;
2021-03-04 deposited with the CCDC.	2021-04-19 downloaded from the CCDC.
;
_audit_creation_date             2020-06-29
_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         '0.13(C272 H144 O120 Th16)'
_chemical_formula_sum            'C34 H18 O15 Th2'
_chemical_formula_weight         1130.56
_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 0.0148 0.0070 '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'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -3.3219 10.6097 '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           64
_space_group_name_H-M_alt        'C m c e'
_space_group_name_Hall           '-C 2bc 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   33.443(2)
_cell_length_b                   16.4404(9)
_cell_length_c                   20.0127(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     11003.4(11)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.97
_cell_measurement_theta_min      3.845
_shelx_estimated_absorpt_T_max   0.799
_shelx_estimated_absorpt_T_min   0.591
_exptl_absorpt_coefficient_mu    11.747
_exptl_absorpt_correction_T_max  0.65
_exptl_absorpt_correction_T_min  0.24
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             4176
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30910
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.946
_diffrn_reflns_theta_min         3.238
_diffrn_ambient_temperature      170.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3943
_reflns_number_total             5329
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 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         14.779
_refine_diff_density_min         -3.033
_refine_diff_density_rms         0.340
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         5329
_refine_ls_number_restraints     357
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0808
_refine_ls_restrained_S_all      1.037
_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)+(0.1469P)²+283.5223P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2164
_refine_ls_wR_factor_ref         0.2356
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
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 Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C7(H7), C9(H9), C11(H11), C15(H15), C16(H16),
 C17(H17), C18(H18)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Th1 Th 0.25475(2) 0.86605(3) 0.52234(2) 0.0252(2) Uani 1 1 d . U . . .
O1 O 0.2362(3) 1.0000 0.5000 0.023(2) Uani 1 2 d S TU P . .
O2 O 0.2762(2) 0.7569(5) 0.4521(3) 0.0173(15) Uani 1 1 d . U . . .
O3 O 0.2928(3) 0.6501(5) 0.5678(5) 0.036(2) Uani 1 1 d . U . . .
O4 O 0.3073(3) 0.7824(6) 0.5753(5) 0.045(2) Uani 1 1 d . U . . .
O5 O 0.2931(4) 0.5862(7) 0.9309(6) 0.066(3) Uani 1 1 d . U . . .
O6 O 0.1842(3) 0.8974(7) 0.5619(7) 0.062(3) Uani 1 1 d . U . . .
C1 C 0.4631(4) 0.6316(8) 0.7185(8) 0.037(3) Uani 1 1 d . U . . .
O7 O 0.2473(4) 0.8772(9) 0.6393(9) 0.084(5) Uani 1 1 d . U . . .
C2 C 0.4253(4) 0.6516(9) 0.6833(7) 0.036(3) Uani 1 1 d . U . . .
C3 C 0.3991(4) 0.6363(8) 0.8317(8) 0.039(3) Uani 1 1 d . U . . .
H3 H 0.4051 0.6903 0.8180 0.046 Uiso 1 1 calc R . . . .
C4 C 0.3541(4) 0.6895(9) 0.6204(7) 0.040(3) Uani 1 1 d . U . . .
C5 C 0.3637(4) 0.6222(9) 0.8651(9) 0.044(4) Uani 1 1 d . U . . .
H5 H 0.3457 0.6657 0.8739 0.053 Uiso 1 1 calc R . . . .
C6 C 0.5000 0.6493(13) 0.6893(11) 0.043(5) Uani 1 2 d S TU P . .
H6 H 0.5000 0.6750 0.6468 0.051 Uiso 1 2 calc RS T P . .
C7 C 0.3622(4) 0.6094(8) 0.6369(7) 0.035(3) Uani 1 1 d . U . . .
H7 H 0.3435 0.5680 0.6262 0.042 Uiso 1 1 calc R . . . .
C8 C 0.3163(5) 0.5251(10) 0.9205(10) 0.063(5) Uani 1 1 d . U . . .
C9 C 0.5000 0.5757(12) 0.8107(10) 0.035(4) Uani 1 2 d S TU P . .
H9 H 0.5000 0.5519 0.8539 0.042 Uiso 1 2 calc RS T P . .
C10 C 0.3153(4) 0.7073(9) 0.5844(8) 0.043(3) Uani 1 1 d . U . . .
C11 C 0.3971(4) 0.5898(9) 0.6685(7) 0.037(3) Uani 1 1 d . U . . .
H11 H 0.4024 0.5350 0.6805 0.045 Uiso 1 1 calc R . . . .
C12 C 0.4637(4) 0.5920(10) 0.7811(7) 0.038(3) Uani 1 1 d . U . . .
C13 C 0.4261(4) 0.5757(9) 0.8172(7) 0.038(3) Uani 1 1 d . U . . .
C14 C 0.3544(4) 0.5420(9) 0.8863(8) 0.048(4) Uani 1 1 d . U . . .
O8 O 0.3085(4) 0.4512(7) 0.9336(8) 0.091(5) Uani 1 1 d . U . . .
C15 C 0.4185(5) 0.4966(9) 0.8411(9) 0.060(4) Uani 1 1 d . U . . .
H15 H 0.4375 0.4543 0.8347 0.072 Uiso 1 1 calc R . . . .
C16 C 0.4180(5) 0.7302(10) 0.6620(10) 0.069(5) Uani 1 1 d . U . . .
H16 H 0.4374 0.7716 0.6683 0.083 Uiso 1 1 calc R . . . .
C17 C 0.3824(5) 0.4812(11) 0.8744(10) 0.078(6) Uani 1 1 d . U . . .
H17 H 0.3769 0.4275 0.8893 0.094 Uiso 1 1 calc R . . . .
C18 C 0.3816(5) 0.7476(11) 0.6310(10) 0.082(6) Uani 1 1 d . U . . .
H18 H 0.3762 0.8018 0.6172 0.099 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
Th1 Th1 3.9322(9) 13_566 ?
Th1 O1 2.332(3) . ?
Th1 O2 2.327(7) 13_566 ?
Th1 O2 2.389(7) . ?
Th1 O3 2.418(9) 13_566 ?
Th1 O4 2.470(9) . ?
Th1 O5 2.370(10) 11_575 ?
Th1 O6 2.541(10) . ?
Th1 O7 2.361(18) . ?
Th1 O8 2.444(10) 10_567 ?
O1 Th1 2.332(3) 4_576 ?
O2 Th1 2.327(7) 13_566 ?
O3 Th1 2.418(9) 13_566 ?
O3 C10 1.251(16) . ?
O4 C10 1.276(16) . ?
O5 Th1 2.369(10) 11_576 ?
O5 C8 1.285(19) . ?
C1 C2 1.484(18) . ?
C1 C6 1.395(16) . ?
C1 C12 1.41(2) . ?
C2 C11 1.420(19) . ?
C2 C16 1.38(2) . ?
C3 C5 1.38(2) . ?
C3 C13 1.38(2) . ?
C4 C7 1.384(19) . ?
C4 C10 1.512(17) . ?
C4 C18 1.34(2) . ?
C5 C14 1.420(19) . ?
C6 C1 1.395(16) 12_655 ?
C7 C11 1.364(18) . ?
C8 C14 1.474(18) . ?
C8 O8 1.270(18) . ?
C9 C12 1.377(15) 12_655 ?
C9 C12 1.377(15) . ?
C12 C13 1.475(17) . ?
C13 C15 1.409(19) . ?
C14 C17 1.39(2) . ?
O8 Th1 2.443(10) 10_557 ?
C15 C17 1.40(2) . ?
C16 C18 1.395(19) . ?

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 Th1 148.37(14) . 13_566 ?
O1 Th1 O2 132.59(17) . . ?
O1 Th1 O3 77.6(3) . 13_566 ?
O1 Th1 O4 142.9(3) . . ?
O1 Th1 O5 71.5(3) . 11_575 ?
O1 Th1 O6 67.7(4) . . ?
O1 Th1 O7 95.1(3) . . ?
O1 Th1 O8 74.0(3) . 10_567 ?
O2 Th1 Th1 33.02(17) . 13_566 ?
O2 Th1 Th1 34.02(17) 13_566 13_566 ?
O2 Th1 O1 138.1(3) 13_566 . ?
O2 Th1 O2 67.0(3) 13_566 . ?
O2 Th1 O3 71.1(3) . 13_566 ?
O2 Th1 O3 77.1(3) 13_566 13_566 ?
O2 Th1 O4 74.8(3) 13_566 . ?
O2 Th1 O4 67.7(3) . . ?
O2 Th1 O5 134.3(3) 13_566 11_575 ?
O2 Th1 O6 127.9(3) . . ?
O2 Th1 O6 72.3(3) 13_566 . ?
O2 Th1 O7 78.6(4) 13_566 . ?
O2 Th1 O8 138.2(4) 13_566 10_567 ?
O2 Th1 O8 114.9(4) . 10_567 ?
O3 Th1 Th1 70.8(2) 13_566 13_566 ?
O3 Th1 O4 136.6(3) 13_566 . ?
O3 Th1 O6 69.2(4) 13_566 . ?
O3 Th1 O8 144.6(4) 13_566 10_567 ?
O4 Th1 Th1 67.3(2) . 13_566 ?
O4 Th1 O6 129.8(4) . . ?
O5 Th1 Th1 100.9(3) 11_575 13_566 ?
O5 Th1 O2 68.4(3) 11_575 . ?
O5 Th1 O3 79.4(5) 11_575 13_566 ?
O5 Th1 O4 97.5(4) 11_575 . ?
O5 Th1 O6 132.5(4) 11_575 . ?
O5 Th1 O8 71.9(5) 11_575 10_567 ?
O6 Th1 Th1 101.1(3) . 13_566 ?
O7 Th1 Th1 107.0(4) . 13_566 ?
O7 Th1 O2 132.3(4) . . ?
O7 Th1 O3 132.7(4) . 13_566 ?
O7 Th1 O4 72.1(4) . . ?
O7 Th1 O5 142.9(5) . 11_575 ?
O7 Th1 O6 65.0(4) . . ?
O7 Th1 O8 71.1(5) . 10_567 ?
O8 Th1 Th1 134.2(3) 10_567 13_566 ?
O8 Th1 O4 68.9(4) 10_567 . ?
O8 Th1 O6 117.1(5) 10_567 . ?
Th1 O1 Th1 149.1(5) . 4_576 ?
Th1 O2 Th1 113.0(3) 13_566 . ?
C10 O3 Th1 132.6(9) . 13_566 ?
C10 O4 Th1 138.6(8) . . ?
C8 O5 Th1 135.3(12) . 11_576 ?
C6 C1 C2 120.5(14) . . ?
C6 C1 C12 117.1(13) . . ?
C12 C1 C2 122.4(11) . . ?
C11 C2 C1 120.5(12) . . ?
C16 C2 C1 120.3(13) . . ?
C16 C2 C11 119.1(13) . . ?
C13 C3 C5 123.0(13) . . ?
C7 C4 C10 117.8(12) . . ?
C18 C4 C7 120.3(13) . . ?
C18 C4 C10 121.7(13) . . ?
C3 C5 C14 119.2(14) . . ?
C1 C6 C1 124.2(19) . 12_655 ?
C11 C7 C4 120.2(14) . . ?
O5 C8 C14 116.7(13) . . ?
O8 C8 O5 126.2(14) . . ?
O8 C8 C14 116.9(14) . . ?
C12 C9 C12 123.6(18) . 12_655 ?
O3 C10 O4 124.3(12) . . ?
O3 C10 C4 119.8(12) . . ?
O4 C10 C4 115.8(12) . . ?
C7 C11 C2 119.8(14) . . ?
C1 C12 C13 120.5(11) . . ?
C9 C12 C1 118.9(12) . . ?
C9 C12 C13 120.3(13) . . ?
C3 C13 C12 122.1(13) . . ?
C3 C13 C15 118.5(13) . . ?
C15 C13 C12 119.3(13) . . ?
C5 C14 C8 120.1(13) . . ?
C17 C14 C5 118.0(13) . . ?
C17 C14 C8 121.8(14) . . ?
C8 O8 Th1 140.6(10) . 10_557 ?
C17 C15 C13 119.0(14) . . ?
C2 C16 C18 119.0(15) . . ?
C14 C17 C15 122.1(15) . . ?
C4 C18 C16 121.4(16) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
