# Supplementary Information (SI) for Chemical Communications.
# 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. 
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#######################################################################

data_shelx
_audit_block_doi                 10.5517/ccdc.csd.cc24vdkz
_database_code_depnum_ccdc_archive 'CCDC 1991581'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D1CC00867F 2021
loop_
_audit_author_name
_audit_author_address
'Michael Boreen'
;University of California, Berkeley
United States of America
;
_audit_update_record             
;
2020-03-19 deposited with the CCDC.	2024-08-21 downloaded from the CCDC.
;
_audit_creation_date             2020-01-20
_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        Th(TPTA)4
_chemical_formula_moiety         'C60 H88 N4 O4 Th'
_chemical_formula_sum            'C60 H88 N4 O4 Th'
_chemical_formula_weight         1161.38
_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 0.0034 0.0017 'Calculated using XDISP in WinGX (Farrugia, 1999)'
H H 0.0000 0.0000 'Calculated using XDISP in WinGX (Farrugia, 1999)'
N N 0.0065 0.0035 'Calculated using XDISP in WinGX (Farrugia, 1999)'
O O 0.0115 0.0064 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Th Th -7.9004 9.3112 'Calculated using XDISP in WinGX (Farrugia, 1999)'

_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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
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                   26.5272(17)
_cell_length_b                   11.0968(7)
_cell_length_c                   21.0598(13)
_cell_angle_alpha                90
_cell_angle_beta                 107.646(4)
_cell_angle_gamma                90
_cell_volume                     5907.6(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    25021
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.042
_cell_measurement_theta_min      1.040
_shelx_estimated_absorpt_T_max   0.536
_shelx_estimated_absorpt_T_min   0.204
_exptl_absorpt_coefficient_mu    2.739
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.026
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.343
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25021
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.343
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         26.042
_diffrn_reflns_theta_min         1.040
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.343
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON-II CPAD detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5253
_reflns_number_total             5433
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A Bruker, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker, Madison WI'
_computing_data_reduction        'SAINT V8.38A Bruker, Madison WI'
_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
_refine_diff_density_max         1.865
_refine_diff_density_min         -4.197
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.489
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5433
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0646
_refine_ls_restrained_S_all      1.488
_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)+84.8249P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1547
_refine_special_details          
;
 Refined as a 3-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.952(2)
 0.0142(19) 0.0334(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C23) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C21) = Uanis(C21A)
Uanis(C23) = Uanis(C23A)
4. Others
 Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C15A)=Sof(H15D)=Sof(H15E)=
 Sof(H15F)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(1)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
 Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=Sof(C21A)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(2)
 Sof(C21)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=
 Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C10(H10), C11(H11), C18(H18), C19(H19), C25(H25), C26(H26)
5.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C24A(H24D,H24E,H24F), C13A(H13D,H13E,H13F), C15A(H15D,H15E,H15F), C22A(H22D,
 H22E,H22F), C14A(H14D,H14E,H14F), C23A(H23D,H23E,H23F), C28(H28A,H28B,H28C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4644(3) 0.4130(8) 0.3337(5) 0.044(2) Uani 1 1 d . . . . .
C2 C 0.4351(3) 0.3340(7) 0.3687(4) 0.0348(19) Uani 1 1 d . . . . .
C3 C 0.4357(4) 0.3541(10) 0.4326(5) 0.052(3) Uani 1 1 d . . . . .
H3 H 0.4578 0.4157 0.4578 0.062 Uiso 1 1 calc R . . . .
C4 C 0.4048(4) 0.2865(10) 0.4618(5) 0.049(2) Uani 1 1 d . . . . .
H4 H 0.4056 0.3040 0.5063 0.059 Uiso 1 1 calc R . . . .
C5 C 0.3732(3) 0.1957(8) 0.4286(4) 0.0350(19) Uani 1 1 d . . . . .
C6 C 0.3408(3) 0.1184(8) 0.4630(5) 0.043(2) Uani 1 1 d . . . . .
C7 C 0.3148(5) 0.1982(11) 0.5028(7) 0.073(4) Uani 1 1 d . . . . .
H7A H 0.2943 0.1480 0.5244 0.110 Uiso 1 1 calc GR . . . .
H7B H 0.2912 0.2559 0.4729 0.110 Uiso 1 1 calc GR . . . .
H7C H 0.3421 0.2419 0.5369 0.110 Uiso 1 1 calc GR . . . .
C8 C 0.2969(4) 0.0484(10) 0.4126(6) 0.060(3) Uani 1 1 d . . . . .
H8A H 0.3126 -0.0143 0.3918 0.091 Uiso 1 1 calc GR . . . .
H8B H 0.2762 0.1036 0.3783 0.091 Uiso 1 1 calc GR . . . .
H8C H 0.2738 0.0109 0.4355 0.091 Uiso 1 1 calc GR . . . .
C9 C 0.3777(4) 0.0309(9) 0.5094(5) 0.054(3) Uani 1 1 d . . . . .
H9A H 0.3946 -0.0204 0.4839 0.081 Uiso 1 1 calc GR . . . .
H9B H 0.3575 -0.0194 0.5313 0.081 Uiso 1 1 calc GR . . . .
H9C H 0.4049 0.0757 0.5431 0.081 Uiso 1 1 calc GR . . . .
C10 C 0.3711(4) 0.1780(8) 0.3631(5) 0.048(2) Uani 1 1 d . . . . .
H10 H 0.3483 0.1177 0.3378 0.058 Uiso 1 1 calc R . . . .
C11 C 0.4015(4) 0.2463(8) 0.3333(5) 0.048(2) Uani 1 1 d . . . . .
H11 H 0.3992 0.2324 0.2879 0.057 Uiso 1 1 calc R . . . .
C12 C 0.5580(3) 0.3477(8) 0.3835(4) 0.0352(19) Uani 1 1 d . . . . .
C13 C 0.5524(8) 0.2236(18) 0.3453(13) 0.038(6) Uani 0.47(3) 1 d . . . A 1
H13A H 0.5168 0.1911 0.3385 0.057 Uiso 0.47(3) 1 calc GR . . A 1
H13B H 0.5787 0.1665 0.3717 0.057 Uiso 0.47(3) 1 calc GR . . A 1
H13C H 0.5583 0.2361 0.3020 0.057 Uiso 0.47(3) 1 calc GR . . A 1
C14 C 0.6106(10) 0.399(2) 0.3886(14) 0.043(6) Uani 0.47(3) 1 d . U . A 1
H14A H 0.6109 0.4273 0.3447 0.065 Uiso 0.47(3) 1 calc GR . . A 1
H14B H 0.6378 0.3372 0.4047 0.065 Uiso 0.47(3) 1 calc GR . . A 1
H14C H 0.6178 0.4670 0.4199 0.065 Uiso 0.47(3) 1 calc GR . . A 1
C15 C 0.5580(9) 0.315(2) 0.4559(10) 0.048(7) Uani 0.47(3) 1 d . . . A 1
H15A H 0.5553 0.3894 0.4800 0.073 Uiso 0.47(3) 1 calc GR . . A 1
H15B H 0.5910 0.2735 0.4792 0.073 Uiso 0.47(3) 1 calc GR . . A 1
H15C H 0.5279 0.2629 0.4538 0.073 Uiso 0.47(3) 1 calc GR . . A 1
C16 C 0.5821(3) 0.7577(7) 0.2771(4) 0.0313(18) Uani 1 1 d . . . . .
C17 C 0.6292(3) 0.8395(7) 0.3010(4) 0.0315(18) Uani 1 1 d . . . . .
C18 C 0.6798(3) 0.7952(8) 0.3159(4) 0.037(2) Uani 1 1 d . . . . .
H18 H 0.6853 0.7109 0.3142 0.044 Uiso 1 1 calc R . . . .
C19 C 0.7225(4) 0.8712(8) 0.3331(5) 0.044(2) Uani 1 1 d . . . . .
H19 H 0.7569 0.8387 0.3407 0.052 Uiso 1 1 calc R . . . .
C20 C 0.7167(4) 0.9942(8) 0.3397(5) 0.043(2) Uani 1 1 d . . . . .
C21 C 0.7608(11) 1.087(3) 0.3662(14) 0.043(5) Uani 0.59(2) 1 d . . . B 1
C22 C 0.7634(9) 1.144(2) 0.4343(12) 0.080(8) Uani 0.59(2) 1 d . . . B 1
H22A H 0.7698 1.0807 0.4683 0.120 Uiso 0.59(2) 1 calc GR . . B 1
H22B H 0.7298 1.1843 0.4308 0.120 Uiso 0.59(2) 1 calc GR . . B 1
H22C H 0.7923 1.2027 0.4467 0.120 Uiso 0.59(2) 1 calc GR . . B 1
C23 C 0.7528(15) 1.191(4) 0.3115(14) 0.049(6) Uani 0.59(2) 1 d . U . B 1
H23A H 0.7815 1.2495 0.3261 0.073 Uiso 0.59(2) 1 calc GR . . B 1
H23B H 0.7188 1.2311 0.3058 0.073 Uiso 0.59(2) 1 calc GR . . B 1
H23C H 0.7531 1.1554 0.2689 0.073 Uiso 0.59(2) 1 calc GR . . B 1
C24 C 0.8132(7) 1.029(2) 0.3725(14) 0.066(7) Uani 0.59(2) 1 d . . . B 1
H24A H 0.8177 0.9581 0.4012 0.099 Uiso 0.59(2) 1 calc GR . . B 1
H24B H 0.8415 1.0872 0.3921 0.099 Uiso 0.59(2) 1 calc GR . . B 1
H24C H 0.8146 1.0053 0.3283 0.099 Uiso 0.59(2) 1 calc GR . . B 1
C25 C 0.6652(4) 1.0378(8) 0.3262(6) 0.051(3) Uani 1 1 d . . . . .
H25 H 0.6597 1.1217 0.3301 0.062 Uiso 1 1 calc R . . . .
C26 C 0.6220(3) 0.9619(7) 0.3072(5) 0.038(2) Uani 1 1 d . . . . .
H26 H 0.5873 0.9937 0.2983 0.045 Uiso 1 1 calc R . . . .
C27 C 0.5502(4) 0.8157(9) 0.1571(4) 0.042(2) Uani 1 1 d . . . . .
C29 C 0.5213(4) 0.9362(10) 0.1530(5) 0.059(3) Uani 1 1 d . . . . .
H29A H 0.4874 0.9232 0.1616 0.089 Uiso 1 1 calc GR . . . .
H29B H 0.5149 0.9706 0.1084 0.089 Uiso 1 1 calc GR . . . .
H29C H 0.5430 0.9918 0.1863 0.089 Uiso 1 1 calc GR . . . .
C30 C 0.5190(5) 0.7361(13) 0.1013(5) 0.078(4) Uani 1 1 d . . . . .
H30A H 0.5369 0.6581 0.1039 0.116 Uiso 1 1 calc GR . . . .
H30B H 0.5164 0.7744 0.0584 0.116 Uiso 1 1 calc GR . . . .
H30C H 0.4834 0.7239 0.1050 0.116 Uiso 1 1 calc GR . . . .
N1 N 0.5151(2) 0.4242(6) 0.3421(4) 0.0354(15) Uani 1 1 d . . . . .
N2 N 0.5490(3) 0.7546(6) 0.2201(3) 0.0334(15) Uani 1 1 d . . . . .
O1 O 0.4337(3) 0.4840(7) 0.2890(4) 0.069(3) Uani 1 1 d . . . . .
O2 O 0.5746(2) 0.6822(5) 0.3210(3) 0.0340(13) Uani 1 1 d . . . . .
Th1 Th 0.5000 0.57942(4) 0.2500 0.02772(14) Uani 1 2 d S T P . .
C24A C 0.8031(11) 1.025(3) 0.305(2) 0.080(13) Uani 0.41(2) 1 d . . . B 2
H24D H 0.7828 1.0273 0.2579 0.119 Uiso 0.41(2) 1 calc GR . . B 2
H24E H 0.8140 0.9423 0.3184 0.119 Uiso 0.41(2) 1 calc GR . . B 2
H24F H 0.8346 1.0763 0.3130 0.119 Uiso 0.41(2) 1 calc GR . . B 2
C13A C 0.5459(9) 0.2243(19) 0.3878(19) 0.074(10) Uani 0.53(3) 1 d . . . A 2
H13D H 0.5217 0.2157 0.4147 0.112 Uiso 0.53(3) 1 calc GR . . A 2
H13E H 0.5785 0.1794 0.4088 0.112 Uiso 0.53(3) 1 calc GR . . A 2
H13F H 0.5290 0.1925 0.3430 0.112 Uiso 0.53(3) 1 calc GR . . A 2
C15A C 0.5727(7) 0.417(3) 0.4499(10) 0.067(8) Uani 0.53(3) 1 d . . . A 2
H15D H 0.5416 0.4227 0.4657 0.101 Uiso 0.53(3) 1 calc GR . . A 2
H15E H 0.5849 0.4980 0.4434 0.101 Uiso 0.53(3) 1 calc GR . . A 2
H15F H 0.6011 0.3739 0.4831 0.101 Uiso 0.53(3) 1 calc GR . . A 2
C22A C 0.7985(13) 1.056(3) 0.4199(17) 0.086(13) Uani 0.41(2) 1 d . . . B 2
H22D H 0.8291 1.1096 0.4329 0.129 Uiso 0.41(2) 1 calc GR . . B 2
H22E H 0.8105 0.9719 0.4286 0.129 Uiso 0.41(2) 1 calc GR . . B 2
H22F H 0.7745 1.0750 0.4458 0.129 Uiso 0.41(2) 1 calc GR . . B 2
C21A C 0.7695(16) 1.071(5) 0.346(2) 0.043(5) Uani 0.41(2) 1 d . . . B 2
C14A C 0.6047(10) 0.372(2) 0.3531(17) 0.057(8) Uani 0.53(3) 1 d . . . A 2
H14D H 0.6373 0.3354 0.3817 0.086 Uiso 0.53(3) 1 calc GR . . A 2
H14E H 0.6099 0.4592 0.3504 0.086 Uiso 0.53(3) 1 calc GR . . A 2
H14F H 0.5959 0.3370 0.3084 0.086 Uiso 0.53(3) 1 calc GR . . A 2
C23A C 0.753(2) 1.200(6) 0.335(2) 0.049(6) Uani 0.41(2) 1 d . . . B 2
H23D H 0.7826 1.2488 0.3304 0.073 Uiso 0.41(2) 1 calc GR . . B 2
H23E H 0.7422 1.2294 0.3726 0.073 Uiso 0.41(2) 1 calc GR . . B 2
H23F H 0.7231 1.2073 0.2938 0.073 Uiso 0.41(2) 1 calc GR . . B 2
C28 C 0.6056(4) 0.8357(10) 0.1521(5) 0.050(2) Uani 1 1 d . . . . .
H28A H 0.6234 0.8985 0.1837 0.075 Uiso 1 1 calc GR . . . .
H28B H 0.6033 0.8609 0.1068 0.075 Uiso 1 1 calc GR . . . .
H28C H 0.6258 0.7605 0.1627 0.075 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
C1 C2 1.504(11) . ?
C1 N1 1.309(10) . ?
C1 O1 1.306(11) . ?
C1 Th1 2.902(8) . ?
C2 C3 1.360(13) . ?
C2 C11 1.376(13) . ?
C3 H3 0.9500 . ?
C3 C4 1.386(13) . ?
C4 H4 0.9500 . ?
C4 C5 1.360(13) . ?
C5 C6 1.541(11) . ?
C5 C10 1.377(13) . ?
C6 C7 1.521(14) . ?
C6 C8 1.529(15) . ?
C6 C9 1.508(12) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 0.9500 . ?
C10 C11 1.390(12) . ?
C11 H11 0.9500 . ?
C12 C13 1.58(2) . ?
C12 C14 1.48(3) . ?
C12 C15 1.56(2) . ?
C12 N1 1.475(11) . ?
C12 C13A 1.42(2) . ?
C12 C15A 1.54(2) . ?
C12 C14A 1.58(2) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.502(11) . ?
C16 N2 1.254(10) . ?
C16 O2 1.308(9) . ?
C16 Th1 2.869(8) . ?
C17 C18 1.375(11) . ?
C17 C26 1.383(11) . ?
C18 H18 0.9500 . ?
C18 C19 1.368(12) . ?
C19 H19 0.9500 . ?
C19 C20 1.386(13) . ?
C20 C21 1.53(3) . ?
C20 C25 1.397(13) . ?
C20 C21A 1.61(4) . ?
C21 C22 1.55(3) . ?
C21 C23 1.60(5) . ?
C21 C24 1.50(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25 0.9500 . ?
C25 C26 1.380(12) . ?
C26 H26 0.9500 . ?
C27 C29 1.530(14) . ?
C27 C30 1.503(14) . ?
C27 N2 1.499(10) . ?
C27 C28 1.521(12) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
N1 Th1 2.534(7) . ?
N2 Th1 2.523(6) . ?
O1 Th1 2.402(6) . ?
O2 Th1 2.378(6) . ?
Th1 C1 2.902(8) 2_655 ?
Th1 C16 2.869(8) 2_655 ?
Th1 N1 2.534(7) 2_655 ?
Th1 N2 2.523(6) 2_655 ?
Th1 O1 2.402(6) 2_655 ?
Th1 O2 2.378(6) 2_655 ?
C24A H24D 0.9800 . ?
C24A H24E 0.9800 . ?
C24A H24F 0.9800 . ?
C24A C21A 1.49(4) . ?
C13A H13D 0.9800 . ?
C13A H13E 0.9800 . ?
C13A H13F 0.9800 . ?
C15A H15D 0.9800 . ?
C15A H15E 0.9800 . ?
C15A H15F 0.9800 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C22A C21A 1.53(6) . ?
C21A C23A 1.50(8) . ?
C14A H14D 0.9800 . ?
C14A H14E 0.9800 . ?
C14A H14F 0.9800 . ?
C23A H23D 0.9800 . ?
C23A H23E 0.9800 . ?
C23A H23F 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 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
C2 C1 Th1 168.6(6) . . ?
N1 C1 C2 130.7(8) . . ?
N1 C1 Th1 60.7(4) . . ?
O1 C1 C2 113.8(7) . . ?
O1 C1 N1 115.5(7) . . ?
O1 C1 Th1 54.9(4) . . ?
C3 C2 C1 122.4(8) . . ?
C3 C2 C11 117.7(8) . . ?
C11 C2 C1 119.4(8) . . ?
C2 C3 H3 119.4 . . ?
C2 C3 C4 121.3(9) . . ?
C4 C3 H3 119.4 . . ?
C3 C4 H4 119.1 . . ?
C5 C4 C3 121.8(9) . . ?
C5 C4 H4 119.1 . . ?
C4 C5 C6 121.0(8) . . ?
C4 C5 C10 116.9(8) . . ?
C10 C5 C6 122.1(8) . . ?
C7 C6 C5 110.2(8) . . ?
C7 C6 C8 107.5(9) . . ?
C8 C6 C5 111.9(8) . . ?
C9 C6 C5 108.6(7) . . ?
C9 C6 C7 109.3(9) . . ?
C9 C6 C8 109.3(8) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 C10 H10 119.3 . . ?
C5 C10 C11 121.5(9) . . ?
C11 C10 H10 119.3 . . ?
C2 C11 C10 120.6(9) . . ?
C2 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C14 C12 C13 108.3(13) . . ?
C14 C12 C15 107.2(14) . . ?
C15 C12 C13 105.5(13) . . ?
N1 C12 C13 105.3(10) . . ?
N1 C12 C14 111.3(11) . . ?
N1 C12 C15 118.7(10) . . ?
N1 C12 C15A 100.9(10) . . ?
N1 C12 C14A 102.8(11) . . ?
C13A C12 N1 116.3(12) . . ?
C13A C12 C15A 115.1(18) . . ?
C13A C12 C14A 114.4(15) . . ?
C15A C12 C14A 105.6(15) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 Th1 170.9(6) . . ?
N2 C16 C17 127.4(7) . . ?
N2 C16 O2 116.5(7) . . ?
N2 C16 Th1 61.4(4) . . ?
O2 C16 C17 116.1(7) . . ?
O2 C16 Th1 55.2(4) . . ?
C18 C17 C16 121.0(7) . . ?
C18 C17 C26 118.9(8) . . ?
C26 C17 C16 120.1(7) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 C17 120.9(8) . . ?
C19 C18 H18 119.6 . . ?
C18 C19 H19 119.1 . . ?
C18 C19 C20 121.7(9) . . ?
C20 C19 H19 119.1 . . ?
C19 C20 C21 127.1(14) . . ?
C19 C20 C25 116.9(9) . . ?
C19 C20 C21A 114.2(19) . . ?
C25 C20 C21 115.8(14) . . ?
C25 C20 C21A 127(2) . . ?
C20 C21 C22 115.3(16) . . ?
C20 C21 C23 108(2) . . ?
C22 C21 C23 109(3) . . ?
C24 C21 C20 110(2) . . ?
C24 C21 C22 108(2) . . ?
C24 C21 C23 107(2) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C20 C25 H25 119.2 . . ?
C26 C25 C20 121.6(8) . . ?
C26 C25 H25 119.2 . . ?
C17 C26 H26 120.0 . . ?
C25 C26 C17 120.0(8) . . ?
C25 C26 H26 120.0 . . ?
C30 C27 C29 108.7(9) . . ?
C30 C27 C28 110.2(9) . . ?
N2 C27 C29 107.5(7) . . ?
N2 C27 C30 105.8(8) . . ?
N2 C27 C28 114.0(7) . . ?
C28 C27 C29 110.3(8) . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C1 N1 C12 127.1(7) . . ?
C1 N1 Th1 92.5(5) . . ?
C12 N1 Th1 139.3(5) . . ?
C16 N2 C27 129.7(7) . . ?
C16 N2 Th1 92.7(5) . . ?
C27 N2 Th1 136.1(5) . . ?
C1 O1 Th1 98.7(5) . . ?
C16 O2 Th1 98.0(5) . . ?
C1 Th1 C1 101.0(4) 2_655 . ?
C16 Th1 C1 133.3(3) . . ?
C16 Th1 C1 133.3(3) 2_655 2_655 ?
C16 Th1 C1 101.1(2) . 2_655 ?
C16 Th1 C1 101.1(2) 2_655 . ?
C16 Th1 C16 92.8(3) . 2_655 ?
N1 Th1 C1 91.6(2) 2_655 . ?
N1 Th1 C1 26.8(2) . . ?
N1 Th1 C1 26.8(2) 2_655 2_655 ?
N1 Th1 C1 91.6(2) . 2_655 ?
N1 Th1 C16 112.5(2) 2_655 2_655 ?
N1 Th1 C16 123.7(2) . 2_655 ?
N1 Th1 C16 123.7(2) 2_655 . ?
N1 Th1 C16 112.5(2) . . ?
N1 Th1 N1 94.3(3) 2_655 . ?
N2 Th1 C1 158.4(3) 2_655 2_655 ?
N2 Th1 C1 158.4(3) . . ?
N2 Th1 C1 92.9(2) . 2_655 ?
N2 Th1 C1 92.9(2) 2_655 . ?
N2 Th1 C16 25.9(2) 2_655 2_655 ?
N2 Th1 C16 80.6(2) 2_655 . ?
N2 Th1 C16 25.9(2) . . ?
N2 Th1 C16 80.6(2) . 2_655 ?
N2 Th1 N1 107.9(2) . 2_655 ?
N2 Th1 N1 137.8(2) . . ?
N2 Th1 N1 137.8(2) 2_655 2_655 ?
N2 Th1 N1 107.9(2) 2_655 . ?
N2 Th1 N2 79.2(3) . 2_655 ?
O1 Th1 C1 26.4(2) 2_655 2_655 ?
O1 Th1 C1 109.5(3) 2_655 . ?
O1 Th1 C1 109.5(3) . 2_655 ?
O1 Th1 C1 26.4(2) . . ?
O1 Th1 C16 77.4(2) 2_655 . ?
O1 Th1 C16 145.8(3) 2_655 2_655 ?
O1 Th1 C16 145.8(3) . . ?
O1 Th1 C16 77.4(2) . 2_655 ?
O1 Th1 N1 53.1(2) . . ?
O1 Th1 N1 90.0(3) 2_655 . ?
O1 Th1 N1 90.0(3) . 2_655 ?
O1 Th1 N1 53.2(2) 2_655 2_655 ?
O1 Th1 N2 155.8(2) 2_655 2_655 ?
O1 Th1 N2 76.6(2) 2_655 . ?
O1 Th1 N2 76.6(2) . 2_655 ?
O1 Th1 N2 155.8(2) . . ?
O1 Th1 O1 127.7(4) 2_655 . ?
O2 Th1 C1 109.0(2) 2_655 . ?
O2 Th1 C1 109.0(2) . 2_655 ?
O2 Th1 C1 106.6(2) . . ?
O2 Th1 C1 106.6(2) 2_655 2_655 ?
O2 Th1 C16 103.4(2) . 2_655 ?
O2 Th1 C16 26.8(2) . . ?
O2 Th1 C16 26.8(2) 2_655 2_655 ?
O2 Th1 C16 103.4(2) 2_655 . ?
O2 Th1 N1 86.4(2) 2_655 2_655 ?
O2 Th1 N1 135.67(19) . 2_655 ?
O2 Th1 N1 86.4(2) . . ?
O2 Th1 N1 135.67(19) 2_655 . ?
O2 Th1 N2 52.7(2) 2_655 2_655 ?
O2 Th1 N2 52.7(2) . . ?
O2 Th1 N2 82.4(2) 2_655 . ?
O2 Th1 N2 82.4(2) . 2_655 ?
O2 Th1 O1 82.5(2) . 2_655 ?
O2 Th1 O1 123.5(3) . . ?
O2 Th1 O1 123.5(3) 2_655 2_655 ?
O2 Th1 O1 82.6(2) 2_655 . ?
O2 Th1 O2 122.7(3) . 2_655 ?
H24D C24A H24E 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
C21A C24A H24D 109.5 . . ?
C21A C24A H24E 109.5 . . ?
C21A C24A H24F 109.5 . . ?
C12 C13A H13D 109.5 . . ?
C12 C13A H13E 109.5 . . ?
C12 C13A H13F 109.5 . . ?
H13D C13A H13E 109.5 . . ?
H13D C13A H13F 109.5 . . ?
H13E C13A H13F 109.5 . . ?
C12 C15A H15D 109.5 . . ?
C12 C15A H15E 109.5 . . ?
C12 C15A H15F 109.5 . . ?
H15D C15A H15E 109.5 . . ?
H15D C15A H15F 109.5 . . ?
H15E C15A H15F 109.5 . . ?
H22D C22A H22E 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
C21A C22A H22D 109.5 . . ?
C21A C22A H22E 109.5 . . ?
C21A C22A H22F 109.5 . . ?
C24A C21A C20 115(3) . . ?
C24A C21A C22A 110(4) . . ?
C24A C21A C23A 116(4) . . ?
C22A C21A C20 100(3) . . ?
C23A C21A C20 107(3) . . ?
C23A C21A C22A 107(4) . . ?
C12 C14A H14D 109.5 . . ?
C12 C14A H14E 109.5 . . ?
C12 C14A H14F 109.5 . . ?
H14D C14A H14E 109.5 . . ?
H14D C14A H14F 109.5 . . ?
H14E C14A H14F 109.5 . . ?
C21A C23A H23D 109.5 . . ?
C21A C23A H23E 109.5 . . ?
C21A C23A H23F 109.5 . . ?
H23D C23A H23E 109.5 . . ?
H23D C23A H23F 109.5 . . ?
H23E C23A H23F 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.952(2)
2 0.0142(19)
3 0.0334(15)
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hexane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# 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_mds_3_183
_audit_block_doi                 10.5517/ccdc.csd.cc24vdl0
_database_code_depnum_ccdc_archive 'CCDC 1991582'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D1CC00867F 2021
loop_
_audit_author_name
_audit_author_address
'Michael Boreen'
;University of California, Berkeley
United States of America
;
_audit_update_record             
;
2020-03-19 deposited with the CCDC.	2024-08-21 downloaded from the CCDC.
;
_audit_creation_date             2019-11-21
_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        Th(ArFTA)4
_chemical_formula_moiety         'C52 H48 F24 N4 O4 Th, C6 H14'
_chemical_formula_sum            'C58 H62 F24 N4 O4 Th'
_chemical_formula_weight         1567.15
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Th C80 H80 F24 N4 O4'
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'
F F 0.0171 0.0103 '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                   10.7799(2)
_cell_length_b                   14.0321(3)
_cell_length_c                   22.2223(5)
_cell_angle_alpha                90
_cell_angle_beta                 102.024(2)
_cell_angle_gamma                90
_cell_volume                     3287.70(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    33897
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.7270
_cell_measurement_theta_min      3.2620
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.382
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.63a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.801
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -45.00  21.00   0.50    6.00    --   -2.02 -77.00 -60.00  132
  2  ω    -45.00  21.00   0.50    6.00    --   -2.02 -77.00  60.00  132
  3  ω    -12.00  36.00   0.50    6.00    --    2.33 -99.00 120.00   96
  4  ω    -75.00  15.00   0.50    6.00    --    2.33 -38.00 -30.00  180
  5  ω    -79.00  11.00   0.50    6.00    --   -2.02 -38.00-150.00  180
  6  ω    -71.00  17.00   0.50    6.00    --    2.33 -57.00-180.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0097602000
_diffrn_orient_matrix_UB_12      -0.0442563000
_diffrn_orient_matrix_UB_13      -0.0156986000
_diffrn_orient_matrix_UB_21      -0.0287312000
_diffrn_orient_matrix_UB_22      0.0240565000
_diffrn_orient_matrix_UB_23      -0.0274513000
_diffrn_orient_matrix_UB_31      0.0600496000
_diffrn_orient_matrix_UB_32      0.0043413000
_diffrn_orient_matrix_UB_33      -0.0080432000
_diffrn_oxdiff_digest_frames     
;
01167b51101fd2a014d3581e8aa5ab9ee70089612ef
;
_diffrn_oxdiff_digest_hkl        
;
017cf3351ddae64a5c6a4cb8d4f9ce119c517b
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6324
_reflns_number_total             6726
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6726
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0219
_refine_ls_restrained_S_all      1.045
_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)+(0.0320P)²+1.8207P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0535
_refine_ls_wR_factor_ref         0.0543
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C30(0.5) H30A(0.5) H30B(0.5) C32(0.5) H32A(0.5) H32B(0.5)
 H32C(0.5) C28(0.5) H28A(0.5) H28B(0.5) C31(0.5) H31A(0.5) H31B(0.5) C29(0.5)
 H29A(0.5) H29B(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C28(H28A,H28B), C31(H31A,H31B), C29(H29A,H29B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C8(H8), C24(H24), C22(H22), C20(H20)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C4(H4A,H4B,H4C), C32(H32A,H32B,H32C), C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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 0.2500 0.63271(2) 0.2500 0.01811(4) Uani 1 2 d S T P . .
O2 O 0.43636(15) 0.71715(12) 0.29986(8) 0.0280(4) Uani 1 1 d . . . . .
O1 O 0.08345(14) 0.54519(11) 0.28014(7) 0.0243(3) Uani 1 1 d . . . . .
N1 N 0.27363(18) 0.50382(13) 0.33343(9) 0.0232(4) Uani 1 1 d . . . . .
N2 N 0.26448(17) 0.76085(14) 0.33261(9) 0.0246(4) Uani 1 1 d . . . . .
F6 F -0.25833(19) 0.35388(16) 0.44660(11) 0.0672(6) Uani 1 1 d . . . . .
F3 F -0.0487(2) 0.09329(14) 0.35904(12) 0.0750(6) Uani 1 1 d . . . . .
F12 F 0.4334(2) 1.13264(12) 0.34293(12) 0.0747(7) Uani 1 1 d . . . . .
C1 C 0.1526(2) 0.48895(15) 0.32015(10) 0.0208(4) Uani 1 1 d . . . . .
F7 F 0.89701(18) 0.87907(17) 0.47159(13) 0.0747(7) Uani 1 1 d . . . . .
C12 C -0.0004(2) 0.44185(17) 0.38388(11) 0.0266(5) Uani 1 1 d . . . . .
H12 H -0.0004 0.5063 0.3969 0.032 Uiso 1 1 calc R . . . .
F4 F -0.0915(2) 0.4031(2) 0.50621(9) 0.0892(8) Uani 1 1 d . . . . .
C7 C 0.0767(2) 0.41388(16) 0.34472(10) 0.0242(5) Uani 1 1 d . . . . .
C2 C 0.3844(2) 0.77324(16) 0.33445(10) 0.0241(5) Uani 1 1 d . . . . .
F8 F 0.7922(2) 0.8485(2) 0.54009(10) 0.0905(9) Uani 1 1 d . . . . .
F9 F 0.81443(19) 0.74359(15) 0.47469(12) 0.0755(7) Uani 1 1 d . . . . .
F11 F 0.4945(3) 1.14574(15) 0.43961(12) 0.0791(7) Uani 1 1 d . . . . .
F10 F 0.6279(2) 1.15580(15) 0.38292(15) 0.0868(8) Uani 1 1 d . . . . .
F1 F -0.0919(3) 0.14729(16) 0.26675(13) 0.0934(9) Uani 1 1 d . . . . .
C11 C -0.0780(2) 0.37575(18) 0.40426(12) 0.0322(6) Uani 1 1 d . . . . .
C3 C 0.3737(2) 0.45324(17) 0.37809(11) 0.0273(5) Uani 1 1 d . . . . .
C10 C -0.0812(3) 0.2822(2) 0.38472(12) 0.0362(6) Uani 1 1 d . . . . .
H10 H -0.1349 0.2372 0.3986 0.043 Uiso 1 1 calc R . . . .
C19 C 0.4760(2) 0.84341(17) 0.37067(11) 0.0252(5) Uani 1 1 d . . . . .
C6 C 0.4331(3) 0.37860(19) 0.34321(13) 0.0394(6) Uani 1 1 d . . . . .
H6A H 0.3693 0.3306 0.3263 0.059 Uiso 1 1 calc GR . . . .
H6B H 0.5039 0.3479 0.3713 0.059 Uiso 1 1 calc GR . . . .
H6C H 0.4642 0.4093 0.3096 0.059 Uiso 1 1 calc GR . . . .
F2 F 0.1002(3) 0.12467(13) 0.31222(14) 0.0811(8) Uani 1 1 d . . . . .
C8 C 0.0741(2) 0.32010(17) 0.32477(11) 0.0301(5) Uani 1 1 d . . . . .
H8 H 0.1264 0.3005 0.2975 0.036 Uiso 1 1 calc R . . . .
F5 F -0.1957(3) 0.49595(17) 0.44005(14) 0.0918(9) Uani 1 1 d . . . . .
C24 C 0.4568(2) 0.94088(18) 0.36382(11) 0.0292(5) Uani 1 1 d . . . . .
H24 H 0.3820 0.9646 0.3377 0.035 Uiso 1 1 calc R . . . .
C15 C 0.1806(2) 0.80637(18) 0.36897(12) 0.0320(5) Uani 1 1 d . . . . .
C22 C 0.6561(2) 0.9696(2) 0.43366(12) 0.0343(6) Uani 1 1 d . . . . .
H22 H 0.7171 1.0126 0.4557 0.041 Uiso 1 1 calc R . . . .
C23 C 0.5474(2) 1.00380(18) 0.39539(12) 0.0319(5) Uani 1 1 d . . . . .
C9 C -0.0056(3) 0.25480(18) 0.34490(13) 0.0369(6) Uani 1 1 d . . . . .
C5 C 0.3298(3) 0.4072(3) 0.43199(13) 0.0464(7) Uani 1 1 d . . . . .
H5A H 0.2788 0.4529 0.4498 0.070 Uiso 1 1 calc GR . . . .
H5B H 0.4038 0.3883 0.4633 0.070 Uiso 1 1 calc GR . . . .
H5C H 0.2785 0.3509 0.4176 0.070 Uiso 1 1 calc GR . . . .
C16 C 0.0793(3) 0.7313(2) 0.37189(15) 0.0423(7) Uani 1 1 d . . . . .
H16A H 0.0348 0.7150 0.3301 0.064 Uiso 1 1 calc GR . . . .
H16B H 0.0185 0.7567 0.3950 0.064 Uiso 1 1 calc GR . . . .
H16C H 0.1196 0.6741 0.3925 0.064 Uiso 1 1 calc GR . . . .
C17 C 0.2469(3) 0.8323(3) 0.43445(15) 0.0497(8) Uani 1 1 d . . . . .
H17A H 0.2975 0.7779 0.4534 0.075 Uiso 1 1 calc GR . . . .
H17B H 0.1832 0.8482 0.4585 0.075 Uiso 1 1 calc GR . . . .
H17C H 0.3025 0.8872 0.4335 0.075 Uiso 1 1 calc GR . . . .
C20 C 0.5863(2) 0.80900(18) 0.40793(11) 0.0289(5) Uani 1 1 d . . . . .
H20 H 0.6009 0.7423 0.4117 0.035 Uiso 1 1 calc R . . . .
C21 C 0.6752(2) 0.87223(19) 0.43962(12) 0.0328(6) Uani 1 1 d . . . . .
C18 C 0.1156(3) 0.8920(2) 0.33383(19) 0.0544(9) Uani 1 1 d . . . . .
H18A H 0.1783 0.9423 0.3330 0.082 Uiso 1 1 calc GR . . . .
H18B H 0.0495 0.9158 0.3542 0.082 Uiso 1 1 calc GR . . . .
H18C H 0.0773 0.8729 0.2916 0.082 Uiso 1 1 calc GR . . . .
C4 C 0.4721(3) 0.5296(2) 0.40257(14) 0.0423(7) Uani 1 1 d . . . . .
H4A H 0.5039 0.5575 0.3683 0.064 Uiso 1 1 calc GR . . . .
H4B H 0.5427 0.5008 0.4319 0.064 Uiso 1 1 calc GR . . . .
H4C H 0.4330 0.5795 0.4233 0.064 Uiso 1 1 calc GR . . . .
C14 C -0.1564(3) 0.4067(2) 0.44835(14) 0.0447(7) Uani 1 1 d . . . . .
C26 C 0.5255(3) 1.1090(2) 0.38970(15) 0.0459(7) Uani 1 1 d . . . . .
C25 C 0.7940(3) 0.8356(2) 0.48133(14) 0.0457(7) Uani 1 1 d . . . . .
C13 C -0.0112(4) 0.1550(2) 0.32106(18) 0.0548(9) Uani 1 1 d . . . . .
C30 C -0.2389(5) 0.7474(5) 0.2329(3) 0.0412(14) Uani 0.5 1 d . . . A -1
H30A H -0.1505 0.7509 0.2269 0.049 Uiso 0.5 1 calc R . . A -1
H30B H -0.2957 0.7543 0.1920 0.049 Uiso 0.5 1 calc R . . A -1
C32 C -0.257(2) 0.9261(5) 0.2591(9) 0.053(3) Uani 0.5 1 d . . . A -1
H32A H -0.2200 0.9344 0.2229 0.080 Uiso 0.5 1 calc GR . . A -1
H32B H -0.2059 0.9598 0.2942 0.080 Uiso 0.5 1 calc GR . . A -1
H32C H -0.3437 0.9521 0.2505 0.080 Uiso 0.5 1 calc GR . . A -1
C28 C -0.2608(6) 0.5678(5) 0.2830(3) 0.0478(15) Uani 0.5 1 d . . . A -1
H28A H -0.3430 0.5645 0.2961 0.057 Uiso 0.5 1 calc R . . A -1
H28B H -0.1952 0.5716 0.3214 0.057 Uiso 0.5 1 calc R . . A -1
C31 C -0.2614(6) 0.8303(5) 0.2727(3) 0.0503(15) Uani 0.5 1 d . . . A -1
H31A H -0.3465 0.8193 0.2817 0.060 Uiso 0.5 1 calc R . . A -1
H31B H -0.2002 0.8217 0.3123 0.060 Uiso 0.5 1 calc R . . A -1
C29 C -0.2600(17) 0.6492(4) 0.2582(8) 0.040(3) Uani 0.5 1 d . . . A -1
H29A H -0.3333 0.6715 0.2749 0.048 Uiso 0.5 1 calc R . . A -1
H29B H -0.3004 0.6246 0.2170 0.048 Uiso 0.5 1 calc R . . A -1
C27 C -0.244(4) 0.4706(5) 0.2572(15) 0.059(5) Uani 0.5 1 d . . . A -1
H27A H -0.3087 0.4606 0.2197 0.089 Uiso 0.5 1 calc GR . . A -1
H27B H -0.2527 0.4219 0.2876 0.089 Uiso 0.5 1 calc GR . . A -1
H27C H -0.1595 0.4661 0.2475 0.089 Uiso 0.5 1 calc GR . . A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Th1 O2 2.3957(15) 2 ?
Th1 O2 2.3957(15) . ?
Th1 O1 2.3836(15) 2 ?
Th1 O1 2.3836(15) . ?
Th1 N1 2.5644(19) 2 ?
Th1 N1 2.5645(19) . ?
Th1 N2 2.5510(19) . ?
Th1 N2 2.5510(19) 2 ?
Th1 C1 2.878(2) . ?
Th1 C1 2.878(2) 2 ?
Th1 C2 2.894(2) 2 ?
Th1 C2 2.894(2) . ?
O2 C2 1.305(3) . ?
O1 C1 1.301(3) . ?
N1 C1 1.294(3) . ?
N1 C3 1.485(3) . ?
N2 C2 1.297(3) . ?
N2 C15 1.478(3) . ?
F6 C14 1.319(3) . ?
F3 C13 1.330(4) . ?
F12 C26 1.321(4) . ?
C1 C7 1.504(3) . ?
F7 C25 1.324(4) . ?
C12 H12 0.9500 . ?
C12 C7 1.380(3) . ?
C12 C11 1.387(3) . ?
F4 C14 1.331(4) . ?
C7 C8 1.387(3) . ?
C2 C19 1.504(3) . ?
F8 C25 1.322(4) . ?
F9 C25 1.323(4) . ?
F11 C26 1.328(4) . ?
F10 C26 1.319(4) . ?
F1 C13 1.337(4) . ?
C11 C10 1.381(4) . ?
C11 C14 1.486(4) . ?
C3 C6 1.521(4) . ?
C3 C5 1.520(4) . ?
C3 C4 1.526(3) . ?
C10 H10 0.9500 . ?
C10 C9 1.376(4) . ?
C19 C24 1.387(3) . ?
C19 C20 1.386(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
F2 C13 1.327(5) . ?
C8 H8 0.9500 . ?
C8 C9 1.392(4) . ?
F5 C14 1.323(4) . ?
C24 H24 0.9500 . ?
C24 C23 1.393(3) . ?
C15 C16 1.528(4) . ?
C15 C17 1.525(4) . ?
C15 C18 1.521(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.382(4) . ?
C22 C21 1.385(4) . ?
C23 C26 1.496(4) . ?
C9 C13 1.494(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C20 H20 0.9500 . ?
C20 C21 1.385(3) . ?
C21 C25 1.507(4) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.512(8) . ?
C30 C29 1.523(9) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C32 C31 1.381(10) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.269(10) . ?
C28 C27 1.503(18) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 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
O2 Th1 O2 120.72(8) 2 . ?
O2 Th1 N1 129.09(6) 2 . ?
O2 Th1 N1 93.84(6) . . ?
O2 Th1 N1 129.09(6) . 2 ?
O2 Th1 N1 93.84(6) 2 2 ?
O2 Th1 N2 84.49(6) 2 . ?
O2 Th1 N2 53.06(6) 2 2 ?
O2 Th1 N2 53.05(6) . . ?
O2 Th1 N2 84.49(6) . 2 ?
O2 Th1 C1 117.49(6) . . ?
O2 Th1 C1 103.39(6) . 2 ?
O2 Th1 C1 117.49(6) 2 2 ?
O2 Th1 C1 103.39(6) 2 . ?
O2 Th1 C2 102.78(6) 2 . ?
O2 Th1 C2 102.78(6) . 2 ?
O2 Th1 C2 26.48(6) 2 2 ?
O2 Th1 C2 26.48(6) . . ?
O1 Th1 O2 77.09(5) 2 . ?
O1 Th1 O2 137.14(6) 2 2 ?
O1 Th1 O2 137.13(6) . . ?
O1 Th1 O2 77.09(5) . 2 ?
O1 Th1 O1 117.97(8) 2 . ?
O1 Th1 N1 53.18(5) 2 2 ?
O1 Th1 N1 82.68(6) . 2 ?
O1 Th1 N1 53.18(5) . . ?
O1 Th1 N1 82.68(6) 2 . ?
O1 Th1 N2 95.61(6) 2 2 ?
O1 Th1 N2 128.95(5) . 2 ?
O1 Th1 N2 95.60(6) . . ?
O1 Th1 N2 128.95(5) 2 . ?
O1 Th1 C1 26.55(6) 2 2 ?
O1 Th1 C1 26.55(6) . . ?
O1 Th1 C1 99.92(6) . 2 ?
O1 Th1 C1 99.92(6) 2 . ?
O1 Th1 C2 103.22(6) 2 . ?
O1 Th1 C2 118.26(6) 2 2 ?
O1 Th1 C2 103.22(6) . 2 ?
O1 Th1 C2 118.26(6) . . ?
N1 Th1 N1 90.30(8) 2 . ?
N1 Th1 C1 84.54(6) . 2 ?
N1 Th1 C1 84.54(6) 2 . ?
N1 Th1 C1 26.71(6) . . ?
N1 Th1 C1 26.71(6) 2 2 ?
N1 Th1 C2 155.53(6) 2 . ?
N1 Th1 C2 92.91(6) . . ?
N1 Th1 C2 155.54(6) . 2 ?
N1 Th1 C2 92.91(6) 2 2 ?
N2 Th1 N1 89.70(6) 2 2 ?
N2 Th1 N1 177.85(6) . 2 ?
N2 Th1 N1 89.70(6) . . ?
N2 Th1 N1 177.84(6) 2 . ?
N2 Th1 N2 90.37(9) . 2 ?
N2 Th1 C1 155.39(6) 2 . ?
N2 Th1 C1 94.51(6) 2 2 ?
N2 Th1 C1 94.52(6) . . ?
N2 Th1 C1 155.39(6) . 2 ?
N2 Th1 C2 86.20(6) 2 . ?
N2 Th1 C2 26.60(6) 2 2 ?
N2 Th1 C2 86.20(6) . 2 ?
N2 Th1 C2 26.60(6) . . ?
C1 Th1 C1 91.01(9) . 2 ?
C1 Th1 C2 129.70(6) . 2 ?
C1 Th1 C2 108.43(6) 2 2 ?
C1 Th1 C2 108.43(6) . . ?
C1 Th1 C2 129.70(6) 2 . ?
C2 Th1 C2 94.11(9) 2 . ?
C2 O2 Th1 98.58(13) . . ?
C1 O1 Th1 98.45(12) . . ?
C1 N1 Th1 90.30(13) . . ?
C1 N1 C3 129.3(2) . . ?
C3 N1 Th1 140.26(14) . . ?
C2 N2 Th1 91.63(14) . . ?
C2 N2 C15 130.1(2) . . ?
C15 N2 Th1 138.20(14) . . ?
O1 C1 Th1 55.00(10) . . ?
O1 C1 C7 113.30(18) . . ?
N1 C1 Th1 62.99(12) . . ?
N1 C1 O1 117.7(2) . . ?
N1 C1 C7 129.0(2) . . ?
C7 C1 Th1 167.08(15) . . ?
C7 C12 H12 120.0 . . ?
C7 C12 C11 120.0(2) . . ?
C11 C12 H12 120.0 . . ?
C12 C7 C1 118.3(2) . . ?
C12 C7 C8 119.8(2) . . ?
C8 C7 C1 121.6(2) . . ?
O2 C2 Th1 54.93(11) . . ?
O2 C2 C19 113.29(19) . . ?
N2 C2 Th1 61.77(12) . . ?
N2 C2 O2 116.6(2) . . ?
N2 C2 C19 130.1(2) . . ?
C19 C2 Th1 167.77(16) . . ?
C12 C11 C14 119.0(2) . . ?
C10 C11 C12 120.7(3) . . ?
C10 C11 C14 120.3(2) . . ?
N1 C3 C6 108.21(19) . . ?
N1 C3 C5 115.3(2) . . ?
N1 C3 C4 104.89(19) . . ?
C6 C3 C4 109.3(2) . . ?
C5 C3 C6 110.0(2) . . ?
C5 C3 C4 108.9(2) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 C11 119.2(2) . . ?
C9 C10 H10 120.4 . . ?
C24 C19 C2 121.3(2) . . ?
C20 C19 C2 118.5(2) . . ?
C20 C19 C24 119.9(2) . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C7 C8 H8 120.2 . . ?
C7 C8 C9 119.6(2) . . ?
C9 C8 H8 120.2 . . ?
C19 C24 H24 120.1 . . ?
C19 C24 C23 119.8(2) . . ?
C23 C24 H24 120.1 . . ?
N2 C15 C16 104.45(19) . . ?
N2 C15 C17 114.0(2) . . ?
N2 C15 C18 109.2(2) . . ?
C17 C15 C16 108.7(2) . . ?
C18 C15 C16 108.0(2) . . ?
C18 C15 C17 112.1(3) . . ?
C23 C22 H22 120.3 . . ?
C23 C22 C21 119.4(2) . . ?
C21 C22 H22 120.3 . . ?
C24 C23 C26 120.1(2) . . ?
C22 C23 C24 120.4(2) . . ?
C22 C23 C26 119.5(2) . . ?
C10 C9 C8 120.7(2) . . ?
C10 C9 C13 120.3(3) . . ?
C8 C9 C13 119.0(3) . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C20 H20 120.1 . . ?
C21 C20 C19 119.8(2) . . ?
C21 C20 H20 120.1 . . ?
C22 C21 C20 120.7(2) . . ?
C22 C21 C25 119.1(2) . . ?
C20 C21 C25 120.2(2) . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
F6 C14 F4 105.9(3) . . ?
F6 C14 C11 113.6(3) . . ?
F6 C14 F5 106.7(3) . . ?
F4 C14 C11 111.7(3) . . ?
F5 C14 F4 105.0(3) . . ?
F5 C14 C11 113.2(2) . . ?
F12 C26 F11 106.3(3) . . ?
F12 C26 C23 113.2(2) . . ?
F11 C26 C23 112.0(3) . . ?
F10 C26 F12 107.1(3) . . ?
F10 C26 F11 105.3(3) . . ?
F10 C26 C23 112.3(3) . . ?
F7 C25 C21 112.2(3) . . ?
F8 C25 F7 106.5(3) . . ?
F8 C25 F9 106.3(3) . . ?
F8 C25 C21 112.0(3) . . ?
F9 C25 F7 105.5(3) . . ?
F9 C25 C21 113.8(2) . . ?
F3 C13 F1 107.1(3) . . ?
F3 C13 C9 112.4(3) . . ?
F1 C13 C9 111.5(3) . . ?
F2 C13 F3 106.8(3) . . ?
F2 C13 F1 106.2(3) . . ?
F2 C13 C9 112.5(3) . . ?
H30A C30 H30B 107.5 . . ?
C31 C30 H30A 108.5 . . ?
C31 C30 H30B 108.5 . . ?
C31 C30 C29 115.1(6) . . ?
C29 C30 H30A 108.5 . . ?
C29 C30 H30B 108.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H28A C28 H28B 105.8 . . ?
C29 C28 H28A 104.9 . . ?
C29 C28 H28B 104.9 . . ?
C29 C28 C27 129.7(14) . . ?
C27 C28 H28A 104.9 . . ?
C27 C28 H28B 104.9 . . ?
C30 C31 H31A 105.5 . . ?
C30 C31 H31B 105.5 . . ?
C32 C31 C30 127.2(8) . . ?
C32 C31 H31A 105.5 . . ?
C32 C31 H31B 105.5 . . ?
H31A C31 H31B 106.1 . . ?
C30 C29 H29A 92.6 . . ?
C30 C29 H29B 92.6 . . ?
C28 C29 C30 171.7(17) . . ?
C28 C29 H29A 92.6 . . ?
C28 C29 H29B 92.6 . . ?
H29A C29 H29B 103.0 . . ?
C28 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
C28 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 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 O2 C2 N2 3.7(2) . . . . ?
Th1 O2 C2 C19 -176.24(16) . . . . ?
Th1 O1 C1 N1 6.2(2) . . . . ?
Th1 O1 C1 C7 -173.73(15) . . . . ?
Th1 N1 C1 O1 -5.7(2) . . . . ?
Th1 N1 C1 C7 174.2(2) . . . . ?
Th1 N1 C3 C6 -77.2(3) . . . . ?
Th1 N1 C3 C5 159.1(2) . . . . ?
Th1 N1 C3 C4 39.3(3) . . . . ?
Th1 N2 C2 O2 -3.4(2) . . . . ?
Th1 N2 C2 C19 176.5(2) . . . . ?
Th1 N2 C15 C16 26.4(3) . . . . ?
Th1 N2 C15 C17 144.8(2) . . . . ?
Th1 N2 C15 C18 -89.0(3) . . . . ?
Th1 C1 C7 C12 -94.6(7) . . . . ?
Th1 C1 C7 C8 79.6(7) . . . . ?
Th1 C2 C19 C24 105.7(7) . . . . ?
Th1 C2 C19 C20 -69.3(8) . . . . ?
O2 C2 C19 C24 120.4(2) . . . . ?
O2 C2 C19 C20 -54.7(3) . . . . ?
O1 C1 C7 C12 -71.0(3) . . . . ?
O1 C1 C7 C8 103.2(2) . . . . ?
N1 C1 C7 C12 109.1(3) . . . . ?
N1 C1 C7 C8 -76.7(3) . . . . ?
N2 C2 C19 C24 -59.5(4) . . . . ?
N2 C2 C19 C20 125.5(3) . . . . ?
C1 N1 C3 C6 96.7(3) . . . . ?
C1 N1 C3 C5 -26.9(4) . . . . ?
C1 N1 C3 C4 -146.7(2) . . . . ?
C1 C7 C8 C9 -174.7(2) . . . . ?
C12 C7 C8 C9 -0.5(3) . . . . ?
C12 C11 C10 C9 0.4(4) . . . . ?
C12 C11 C14 F6 155.2(3) . . . . ?
C12 C11 C14 F4 -85.1(3) . . . . ?
C12 C11 C14 F5 33.2(4) . . . . ?
C7 C12 C11 C10 -1.4(4) . . . . ?
C7 C12 C11 C14 177.6(2) . . . . ?
C7 C8 C9 C10 -0.5(4) . . . . ?
C7 C8 C9 C13 177.6(3) . . . . ?
C2 N2 C15 C16 -150.9(3) . . . . ?
C2 N2 C15 C17 -32.4(4) . . . . ?
C2 N2 C15 C18 93.8(3) . . . . ?
C2 C19 C24 C23 -176.2(2) . . . . ?
C2 C19 C20 C21 177.1(2) . . . . ?
C11 C12 C7 C1 175.8(2) . . . . ?
C11 C12 C7 C8 1.5(3) . . . . ?
C11 C10 C9 C8 0.5(4) . . . . ?
C11 C10 C9 C13 -177.5(3) . . . . ?
C3 N1 C1 Th1 -176.1(3) . . . . ?
C3 N1 C1 O1 178.1(2) . . . . ?
C3 N1 C1 C7 -1.9(4) . . . . ?
C10 C11 C14 F6 -25.8(4) . . . . ?
C10 C11 C14 F4 93.9(3) . . . . ?
C10 C11 C14 F5 -147.8(3) . . . . ?
C10 C9 C13 F3 -26.1(4) . . . . ?
C10 C9 C13 F1 94.1(4) . . . . ?
C10 C9 C13 F2 -146.7(3) . . . . ?
C19 C24 C23 C22 -0.3(4) . . . . ?
C19 C24 C23 C26 -178.2(3) . . . . ?
C19 C20 C21 C22 -1.1(4) . . . . ?
C19 C20 C21 C25 178.7(2) . . . . ?
C8 C9 C13 F3 155.8(3) . . . . ?
C8 C9 C13 F1 -84.0(4) . . . . ?
C8 C9 C13 F2 35.2(4) . . . . ?
C24 C19 C20 C21 1.9(4) . . . . ?
C24 C23 C26 F12 -15.3(4) . . . . ?
C24 C23 C26 F11 104.9(3) . . . . ?
C24 C23 C26 F10 -136.7(3) . . . . ?
C15 N2 C2 Th1 178.2(3) . . . . ?
C15 N2 C2 O2 174.8(2) . . . . ?
C15 N2 C2 C19 -5.4(4) . . . . ?
C22 C23 C26 F12 166.8(3) . . . . ?
C22 C23 C26 F11 -73.0(4) . . . . ?
C22 C23 C26 F10 45.3(4) . . . . ?
C22 C21 C25 F7 -48.1(4) . . . . ?
C22 C21 C25 F8 71.6(4) . . . . ?
C22 C21 C25 F9 -167.7(3) . . . . ?
C23 C22 C21 C20 -0.3(4) . . . . ?
C23 C22 C21 C25 179.9(3) . . . . ?
C20 C19 C24 C23 -1.2(4) . . . . ?
C20 C21 C25 F7 132.1(3) . . . . ?
C20 C21 C25 F8 -108.2(3) . . . . ?
C20 C21 C25 F9 12.5(4) . . . . ?
C21 C22 C23 C24 1.0(4) . . . . ?
C21 C22 C23 C26 179.0(3) . . . . ?
C14 C11 C10 C9 -178.6(3) . . . . ?
C29 C30 C31 C32 -175.4(16) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.300
_oxdiff_exptl_absorpt_empirical_full_min 0.640
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hexane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# 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_MDS_3_8
_database_code_depnum_ccdc_archive 'CCDC 2377153'
loop_
_audit_author_name
_audit_author_address
'Simon J. Teat'
;Lawrence Berkeley National Laboratory
United States of America
;
_audit_update_record             
;
2024-08-12 deposited with the CCDC.	2024-08-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H64 N4 O4 Th'
_chemical_formula_weight         800.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 'Calculated using XDISP in WinGX (Farrugia, 1999)'
H H 0.0000 0.0000 'Calculated using XDISP in WinGX (Farrugia, 1999)'
N N 0.0065 0.0035 'Calculated using XDISP in WinGX (Farrugia, 1999)'
O O 0.0115 0.0064 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Th Th -7.9004 9.3112 'Calculated using XDISP in WinGX (Farrugia, 1999)'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.8073(4)
_cell_length_b                   24.7927(11)
_cell_length_c                   17.2472(7)
_cell_angle_alpha                90
_cell_angle_beta                 94.9595(16)
_cell_angle_gamma                90
_cell_volume                     3751.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9921
_cell_measurement_theta_min      2.8905
_cell_measurement_theta_max      31.4076

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_F_000             1624
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    4.275
_shelx_estimated_absorpt_T_min   0.513
_shelx_estimated_absorpt_T_max   0.700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.586
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_process_details   'SADABS 2016/2 Bruker AXS Madison WI USA'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Light Source beamline 12.2.1'
_diffrn_measurement_device_type  'Bruker D8 with PHOTONII detector'
_diffrn_measurement_method       'ω/θ shutterless scans'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            67351
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.525
_diffrn_reflns_theta_max         31.467
_diffrn_reflns_theta_full        25.930
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11511
_reflns_number_gt                6998
_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.
 
 _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 APEX 3'
_computing_cell_refinement       'Bruker SAINT v8.40a'
_computing_data_reduction        'Bruker SAINT v8.40a'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_publication_material  'Bruker SHELXTL & local programs'
_refine_special_details          
;
 All non-hydrogen atoms were refined anisotropically. Hydrogen
 atoms were placed geometrically on the carbon atoms constrained
 and refined using a riding model.
 Displacement parameter restraints were used to model the ligands.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0138P)²+7.0437P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     isomor
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11511
_refine_ls_number_parameters     731
_refine_ls_number_restraints     1448
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0313
_refine_ls_wR_factor_ref         0.0660
_refine_ls_wR_factor_gt          0.0581
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.013
_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
Th1 Th 0.24508(2) 0.37492(2) 0.75031(2) 0.01379(3) Uani 1 1 d . . . . .
O1 O 0.5072(3) 0.37512(15) 0.79284(16) 0.0168(5) Uani 0.7093(12) 1 d . U P A 1
C1 C 0.4993(5) 0.3746(3) 0.8684(3) 0.0138(7) Uani 0.7093(12) 1 d . U P A 1
C5 C 0.3230(6) 0.3715(4) 0.9733(3) 0.0230(10) Uani 0.7093(12) 1 d . U P A 1
C6 C 0.3846(7) 0.3205(3) 1.0139(4) 0.0424(17) Uani 0.7093(12) 1 d . U P A 1
H6A H 0.356677 0.320146 1.067633 0.064 Uiso 0.7093(12) 1 calc R U P A 1
H6B H 0.341006 0.288794 0.986226 0.064 Uiso 0.7093(12) 1 calc R U P A 1
H6C H 0.495887 0.319669 1.013833 0.064 Uiso 0.7093(12) 1 calc R U P A 1
C7 C 0.1490(5) 0.3671(3) 0.9685(3) 0.0327(13) Uani 0.7093(12) 1 d . U P A 1
H7A H 0.115559 0.365590 1.021217 0.049 Uiso 0.7093(12) 1 calc R U P A 1
H7B H 0.103675 0.398706 0.941276 0.049 Uiso 0.7093(12) 1 calc R U P A 1
H7C H 0.116527 0.334329 0.940081 0.049 Uiso 0.7093(12) 1 calc R U P A 1
C8 C 0.3717(8) 0.4230(3) 1.0177(4) 0.0428(16) Uani 0.7093(12) 1 d . U P A 1
H8A H 0.343697 0.420286 1.071296 0.064 Uiso 0.7093(12) 1 calc R U P A 1
H8B H 0.482242 0.427508 1.017965 0.064 Uiso 0.7093(12) 1 calc R U P A 1
H8C H 0.320171 0.454115 0.992145 0.064 Uiso 0.7093(12) 1 calc R U P A 1
N1 N 0.3629(5) 0.3736(3) 0.8916(2) 0.0159(7) Uani 0.7093(12) 1 d . U P A 1
C9 C 0.6503(5) 0.3759(3) 0.9163(3) 0.0190(8) Uani 0.7093(12) 1 d . U P A 1
H9A H 0.632089 0.375525 0.972724 0.023 Uiso 0.7093(12) 1 calc R U P A 1
C10 C 0.7416(6) 0.3248(2) 0.8975(4) 0.0298(13) Uani 0.7093(12) 1 d . U P A 1
H10A H 0.840495 0.325119 0.928313 0.045 Uiso 0.7093(12) 1 calc R U P A 1
H10B H 0.684518 0.292567 0.910320 0.045 Uiso 0.7093(12) 1 calc R U P A 1
H10C H 0.757723 0.324448 0.841982 0.045 Uiso 0.7093(12) 1 calc R U P A 1
C11 C 0.7373(6) 0.4266(2) 0.8990(4) 0.0292(13) Uani 0.7093(12) 1 d . U P A 1
H11A H 0.835312 0.426882 0.930529 0.044 Uiso 0.7093(12) 1 calc R U P A 1
H11B H 0.755075 0.427299 0.843662 0.044 Uiso 0.7093(12) 1 calc R U P A 1
H11C H 0.677801 0.458322 0.911493 0.044 Uiso 0.7093(12) 1 calc R U P A 1
O2 O 0.0752(4) 0.30705(13) 0.7941(2) 0.0192(7) Uani 0.7093(12) 1 d . U P A 1
C2 C 0.1475(6) 0.2640(2) 0.7736(3) 0.0155(9) Uani 0.7093(12) 1 d . U P A 1
C12 C 0.3747(6) 0.2314(3) 0.7107(4) 0.0195(10) Uani 0.7093(12) 1 d . U P A 1
C13 C 0.5039(5) 0.2618(2) 0.6754(3) 0.0239(11) Uani 0.7093(12) 1 d . U P A 1
H13A H 0.575168 0.235870 0.655742 0.036 Uiso 0.7093(12) 1 calc R U P A 1
H13B H 0.461176 0.284643 0.632518 0.036 Uiso 0.7093(12) 1 calc R U P A 1
H13C H 0.557933 0.284451 0.715445 0.036 Uiso 0.7093(12) 1 calc R U P A 1
C14 C 0.4454(6) 0.1960(2) 0.7768(4) 0.0297(13) Uani 0.7093(12) 1 d . U P A 1
H14A H 0.512686 0.169264 0.755716 0.045 Uiso 0.7093(12) 1 calc R U P A 1
H14B H 0.504527 0.218605 0.815035 0.045 Uiso 0.7093(12) 1 calc R U P A 1
H14C H 0.364470 0.177540 0.801922 0.045 Uiso 0.7093(12) 1 calc R U P A 1
C15 C 0.2911(6) 0.1983(2) 0.6436(4) 0.0293(13) Uani 0.7093(12) 1 d . U P A 1
H15A H 0.360631 0.171141 0.625346 0.044 Uiso 0.7093(12) 1 calc R U P A 1
H15B H 0.202250 0.180332 0.662431 0.044 Uiso 0.7093(12) 1 calc R U P A 1
H15C H 0.257616 0.222507 0.600527 0.044 Uiso 0.7093(12) 1 calc R U P A 1
N2 N 0.2720(6) 0.27258(18) 0.7391(3) 0.0137(10) Uani 0.7093(12) 1 d . U P A 1
C16 C 0.0751(6) 0.2116(2) 0.7933(4) 0.0226(11) Uani 0.7093(12) 1 d . U P A 1
H16A H 0.135225 0.181344 0.772911 0.027 Uiso 0.7093(12) 1 calc R U P A 1
C17 C 0.0798(7) 0.2067(2) 0.8822(4) 0.0375(14) Uani 0.7093(12) 1 d . U P A 1
H17A H 0.032795 0.172588 0.895835 0.056 Uiso 0.7093(12) 1 calc R U P A 1
H17B H 0.185965 0.207607 0.904481 0.056 Uiso 0.7093(12) 1 calc R U P A 1
H17C H 0.023736 0.236848 0.902901 0.056 Uiso 0.7093(12) 1 calc R U P A 1
C18 C -0.0896(6) 0.2085(2) 0.7557(4) 0.0355(14) Uani 0.7093(12) 1 d . U P A 1
H18A H -0.134975 0.174010 0.769223 0.053 Uiso 0.7093(12) 1 calc R U P A 1
H18B H -0.149310 0.238205 0.774983 0.053 Uiso 0.7093(12) 1 calc R U P A 1
H18C H -0.089327 0.211217 0.699060 0.053 Uiso 0.7093(12) 1 calc R U P A 1
O3 O 0.0781(4) 0.44231(13) 0.7991(2) 0.0169(7) Uani 0.7093(12) 1 d . U P A 1
C3 C 0.1503(6) 0.4853(2) 0.7785(3) 0.0166(9) Uani 0.7093(12) 1 d . U P A 1
C19 C 0.3733(6) 0.5185(2) 0.7135(4) 0.0184(10) Uani 0.7093(12) 1 d . U P A 1
C20 C 0.2895(6) 0.5535(2) 0.6499(3) 0.0301(13) Uani 0.7093(12) 1 d . U P A 1
H20A H 0.359773 0.580484 0.631986 0.045 Uiso 0.7093(12) 1 calc R U P A 1
H20B H 0.251826 0.530576 0.606084 0.045 Uiso 0.7093(12) 1 calc R U P A 1
H20C H 0.203374 0.571678 0.671109 0.045 Uiso 0.7093(12) 1 calc R U P A 1
C21 C 0.5013(6) 0.4876(2) 0.6782(3) 0.0239(11) Uani 0.7093(12) 1 d . U P A 1
H21A H 0.572339 0.513348 0.657727 0.036 Uiso 0.7093(12) 1 calc R U P A 1
H21B H 0.555768 0.465269 0.718331 0.036 Uiso 0.7093(12) 1 calc R U P A 1
H21C H 0.457583 0.464566 0.635807 0.036 Uiso 0.7093(12) 1 calc R U P A 1
C22 C 0.4473(6) 0.5537(2) 0.7798(3) 0.0281(13) Uani 0.7093(12) 1 d . U P A 1
H22A H 0.513318 0.580721 0.758348 0.042 Uiso 0.7093(12) 1 calc R U P A 1
H22B H 0.367558 0.571983 0.806255 0.042 Uiso 0.7093(12) 1 calc R U P A 1
H22C H 0.508099 0.530973 0.817182 0.042 Uiso 0.7093(12) 1 calc R U P A 1
N3 N 0.2733(6) 0.47738(19) 0.7424(3) 0.0160(10) Uani 0.7093(12) 1 d . U P A 1
C23 C 0.0818(6) 0.5386(2) 0.8022(4) 0.0224(11) Uani 0.7093(12) 1 d . U P A 1
H23A H 0.141856 0.569290 0.782815 0.027 Uiso 0.7093(12) 1 calc R U P A 1
C24 C 0.0869(7) 0.5408(2) 0.8901(4) 0.0392(15) Uani 0.7093(12) 1 d . U P A 1
H24A H 0.043118 0.575007 0.905993 0.059 Uiso 0.7093(12) 1 calc R U P A 1
H24B H 0.028043 0.510727 0.908881 0.059 Uiso 0.7093(12) 1 calc R U P A 1
H24C H 0.192922 0.538188 0.912227 0.059 Uiso 0.7093(12) 1 calc R U P A 1
C25 C -0.0835(6) 0.5422(2) 0.7672(4) 0.0386(15) Uani 0.7093(12) 1 d . U P A 1
H25A H -0.086152 0.540801 0.710266 0.058 Uiso 0.7093(12) 1 calc R U P A 1
H25B H -0.141809 0.511947 0.785832 0.058 Uiso 0.7093(12) 1 calc R U P A 1
H25C H -0.128336 0.576272 0.782896 0.058 Uiso 0.7093(12) 1 calc R U P A 1
O4 O 0.3117(3) 0.37489(14) 0.62091(16) 0.0165(5) Uani 0.7093(12) 1 d . U P A 1
C4 C 0.1755(5) 0.3769(3) 0.5842(3) 0.0149(8) Uani 0.7093(12) 1 d . U P A 1
C26 C -0.1029(6) 0.3801(3) 0.6029(3) 0.0246(10) Uani 0.7093(12) 1 d . U P A 1
C27 C -0.1869(4) 0.3774(2) 0.6761(2) 0.0217(8) Uani 0.7093(12) 1 d . U P A 1
H27A H -0.297013 0.379021 0.661887 0.033 Uiso 0.7093(12) 1 calc R U P A 1
H27B H -0.161756 0.343556 0.703575 0.033 Uiso 0.7093(12) 1 calc R U P A 1
H27C H -0.156268 0.407931 0.710000 0.033 Uiso 0.7093(12) 1 calc R U P A 1
C28 C -0.1404(7) 0.4366(3) 0.5645(4) 0.0491(17) Uani 0.7093(12) 1 d . U P A 1
H28A H -0.249349 0.438421 0.547482 0.074 Uiso 0.7093(12) 1 calc R U P A 1
H28B H -0.114398 0.465134 0.602650 0.074 Uiso 0.7093(12) 1 calc R U P A 1
H28C H -0.080905 0.441328 0.519581 0.074 Uiso 0.7093(12) 1 calc R U P A 1
C29 C -0.1561(7) 0.3345(3) 0.5512(4) 0.058(2) Uani 0.7093(12) 1 d . U P A 1
H29A H -0.265419 0.338401 0.536195 0.087 Uiso 0.7093(12) 1 calc R U P A 1
H29B H -0.100298 0.334730 0.504431 0.087 Uiso 0.7093(12) 1 calc R U P A 1
H29C H -0.137549 0.300290 0.578941 0.087 Uiso 0.7093(12) 1 calc R U P A 1
N4 N 0.0618(5) 0.3775(2) 0.6286(2) 0.0147(7) Uani 0.7093(12) 1 d . U P A 1
C30 C 0.1724(7) 0.3760(4) 0.4965(3) 0.0230(10) Uani 0.7093(12) 1 d . U P A 1
H30A H 0.067620 0.385820 0.474022 0.028 Uiso 0.7093(12) 1 calc R U P A 1
C31 C 0.2833(8) 0.4160(3) 0.4691(3) 0.0429(15) Uani 0.7093(12) 1 d . U P A 1
H31A H 0.279785 0.414911 0.412136 0.064 Uiso 0.7093(12) 1 calc R U P A 1
H31B H 0.256304 0.452295 0.485792 0.064 Uiso 0.7093(12) 1 calc R U P A 1
H31C H 0.386387 0.407051 0.491279 0.064 Uiso 0.7093(12) 1 calc R U P A 1
C32 C 0.2090(8) 0.3187(2) 0.4703(4) 0.0403(14) Uani 0.7093(12) 1 d . U P A 1
H32A H 0.134911 0.293389 0.488985 0.060 Uiso 0.7093(12) 1 calc R U P A 1
H32B H 0.203669 0.317412 0.413321 0.060 Uiso 0.7093(12) 1 calc R U P A 1
H32C H 0.311804 0.308719 0.491764 0.060 Uiso 0.7093(12) 1 calc R U P A 1
O1' O 0.1844(8) 0.3740(4) 0.8772(4) 0.0257(15) Uani 0.2907(12) 1 d . U P A 2
C1' C 0.3214(15) 0.3732(9) 0.9135(8) 0.0230(18) Uani 0.2907(12) 1 d . U P A 2
C5' C 0.5971(15) 0.3708(8) 0.8944(8) 0.0250(19) Uani 0.2907(12) 1 d . U P A 2
C6' C 0.6450(19) 0.4252(8) 0.9411(11) 0.059(4) Uani 0.2907(12) 1 d . U P A 2
H6'A H 0.754755 0.424665 0.956370 0.089 Uiso 0.2907(12) 1 calc R U P A 2
H6'B H 0.620310 0.456487 0.907552 0.089 Uiso 0.2907(12) 1 calc R U P A 2
H6'C H 0.589122 0.427661 0.987667 0.089 Uiso 0.2907(12) 1 calc R U P A 2
C7' C 0.6832(12) 0.3731(6) 0.8221(7) 0.030(2) Uani 0.2907(12) 1 d . U P A 2
H7'A H 0.793006 0.373066 0.837290 0.045 Uiso 0.2907(12) 1 calc R U P A 2
H7'B H 0.656612 0.341656 0.789361 0.045 Uiso 0.2907(12) 1 calc R U P A 2
H7'C H 0.655564 0.406152 0.793033 0.045 Uiso 0.2907(12) 1 calc R U P A 2
C8' C 0.6425(18) 0.3208(8) 0.9384(11) 0.060(4) Uani 0.2907(12) 1 d . U P A 2
H8'A H 0.752386 0.321635 0.953370 0.089 Uiso 0.2907(12) 1 calc R U P A 2
H8'B H 0.587191 0.318679 0.985175 0.089 Uiso 0.2907(12) 1 calc R U P A 2
H8'C H 0.617903 0.289277 0.905419 0.089 Uiso 0.2907(12) 1 calc R U P A 2
N1' N 0.4335(15) 0.3709(6) 0.8711(6) 0.0196(18) Uani 0.2907(12) 1 d . U P A 2
C9' C 0.3249(18) 0.3737(11) 1.0030(8) 0.029(2) Uani 0.2907(12) 1 d . U P A 2
H9'A H 0.433046 0.379384 1.024221 0.035 Uiso 0.2907(12) 1 calc R U P A 2
C10' C 0.274(2) 0.3183(8) 1.0305(10) 0.055(4) Uani 0.2907(12) 1 d . U P A 2
H10D H 0.339582 0.290304 1.010738 0.083 Uiso 0.2907(12) 1 calc R U P A 2
H10E H 0.283217 0.317306 1.087501 0.083 Uiso 0.2907(12) 1 calc R U P A 2
H10F H 0.168284 0.311823 1.010813 0.083 Uiso 0.2907(12) 1 calc R U P A 2
C11' C 0.234(2) 0.4191(8) 1.0296(10) 0.061(4) Uani 0.2907(12) 1 d . U P A 2
H11D H 0.272569 0.453098 1.009862 0.091 Uiso 0.2907(12) 1 calc R U P A 2
H11E H 0.127033 0.414453 1.009891 0.091 Uiso 0.2907(12) 1 calc R U P A 2
H11F H 0.241966 0.419936 1.086579 0.091 Uiso 0.2907(12) 1 calc R U P A 2
O2' O 0.4186(10) 0.3064(4) 0.7000(5) 0.0286(19) Uani 0.2907(12) 1 d . U P A 2
C2' C 0.3424(16) 0.2626(7) 0.7212(9) 0.021(2) Uani 0.2907(12) 1 d . U P A 2
C12' C 0.1229(17) 0.2294(7) 0.7842(9) 0.0225(19) Uani 0.2907(12) 1 d . U P A 2
C13' C -0.0072(15) 0.2594(6) 0.8217(9) 0.033(3) Uani 0.2907(12) 1 d . U P A 2
H13D H -0.075992 0.233041 0.842358 0.049 Uiso 0.2907(12) 1 calc R U P A 2
H13E H 0.036456 0.282518 0.864012 0.049 Uiso 0.2907(12) 1 calc R U P A 2
H13F H -0.064192 0.281693 0.782197 0.049 Uiso 0.2907(12) 1 calc R U P A 2
C14' C 0.2068(17) 0.1961(6) 0.8509(9) 0.037(3) Uani 0.2907(12) 1 d . U P A 2
H14D H 0.137810 0.168656 0.868675 0.056 Uiso 0.2907(12) 1 calc R U P A 2
H14E H 0.296171 0.178593 0.831906 0.056 Uiso 0.2907(12) 1 calc R U P A 2
H14F H 0.239616 0.220153 0.894316 0.056 Uiso 0.2907(12) 1 calc R U P A 2
C15' C 0.0465(15) 0.1952(6) 0.7192(9) 0.035(3) Uani 0.2907(12) 1 d . U P A 2
H15D H -0.017139 0.167732 0.741245 0.052 Uiso 0.2907(12) 1 calc R U P A 2
H15E H -0.017160 0.218202 0.683397 0.052 Uiso 0.2907(12) 1 calc R U P A 2
H15F H 0.124550 0.177574 0.690811 0.052 Uiso 0.2907(12) 1 calc R U P A 2
N2' N 0.2199(16) 0.2713(6) 0.7549(9) 0.020(2) Uani 0.2907(12) 1 d . U P A 2
C16' C 0.4187(17) 0.2114(7) 0.6995(10) 0.029(2) Uani 0.2907(12) 1 d . U P A 2
H16B H 0.357854 0.180959 0.718996 0.034 Uiso 0.2907(12) 1 calc R U P A 2
C17' C 0.5836(15) 0.2052(6) 0.7381(10) 0.042(3) Uani 0.2907(12) 1 d . U P A 2
H17D H 0.626854 0.171090 0.721590 0.063 Uiso 0.2907(12) 1 calc R U P A 2
H17E H 0.646216 0.235274 0.722172 0.063 Uiso 0.2907(12) 1 calc R U P A 2
H17F H 0.581994 0.205398 0.794820 0.063 Uiso 0.2907(12) 1 calc R U P A 2
C18' C 0.4085(17) 0.2064(7) 0.6089(9) 0.041(3) Uani 0.2907(12) 1 d . U P A 2
H18D H 0.458306 0.172946 0.594406 0.061 Uiso 0.2907(12) 1 calc R U P A 2
H18E H 0.301289 0.205782 0.588272 0.061 Uiso 0.2907(12) 1 calc R U P A 2
H18F H 0.459657 0.237286 0.587050 0.061 Uiso 0.2907(12) 1 calc R U P A 2
O3' O 0.4203(10) 0.4411(4) 0.7046(5) 0.0276(18) Uani 0.2907(12) 1 d . U P A 2
C3' C 0.3480(17) 0.4834(7) 0.7252(9) 0.024(2) Uani 0.2907(12) 1 d . U P A 2
C19' C 0.1205(16) 0.5163(7) 0.7900(9) 0.0226(19) Uani 0.2907(12) 1 d . U P A 2
C20' C 0.0533(15) 0.5528(6) 0.7221(9) 0.038(3) Uani 0.2907(12) 1 d . U P A 2
H20D H -0.014946 0.579639 0.742265 0.057 Uiso 0.2907(12) 1 calc R U P A 2
H20E H 0.136507 0.571256 0.698675 0.057 Uiso 0.2907(12) 1 calc R U P A 2
H20F H -0.003819 0.530587 0.682710 0.057 Uiso 0.2907(12) 1 calc R U P A 2
C21' C -0.0068(14) 0.4840(6) 0.8212(8) 0.031(3) Uani 0.2907(12) 1 d . U P A 2
H21D H -0.078967 0.508542 0.843138 0.046 Uiso 0.2907(12) 1 calc R U P A 2
H21E H -0.059697 0.463106 0.778815 0.046 Uiso 0.2907(12) 1 calc R U P A 2
H21F H 0.035971 0.459330 0.861851 0.046 Uiso 0.2907(12) 1 calc R U P A 2
C22' C 0.2044(17) 0.5530(6) 0.8518(9) 0.036(3) Uani 0.2907(12) 1 d . U P A 2
H22D H 0.132254 0.578777 0.871046 0.054 Uiso 0.2907(12) 1 calc R U P A 2
H22E H 0.248720 0.530889 0.895166 0.054 Uiso 0.2907(12) 1 calc R U P A 2
H22F H 0.285732 0.572565 0.828492 0.054 Uiso 0.2907(12) 1 calc R U P A 2
N3' N 0.2220(16) 0.4766(6) 0.7587(9) 0.021(2) Uani 0.2907(12) 1 d . U P A 2
C23' C 0.4191(17) 0.5372(7) 0.7042(10) 0.028(2) Uani 0.2907(12) 1 d . U P A 2
H23B H 0.357300 0.567391 0.723462 0.033 Uiso 0.2907(12) 1 calc R U P A 2
C24' C 0.5805(16) 0.5411(6) 0.7416(10) 0.040(3) Uani 0.2907(12) 1 d . U P A 2
H24D H 0.625016 0.575622 0.727760 0.061 Uiso 0.2907(12) 1 calc R U P A 2
H24E H 0.579609 0.538666 0.798238 0.061 Uiso 0.2907(12) 1 calc R U P A 2
H24F H 0.641441 0.511452 0.722931 0.061 Uiso 0.2907(12) 1 calc R U P A 2
C25' C 0.4185(18) 0.5412(6) 0.6150(9) 0.039(3) Uani 0.2907(12) 1 d . U P A 2
H25D H 0.313571 0.538671 0.591324 0.059 Uiso 0.2907(12) 1 calc R U P A 2
H25E H 0.462448 0.575890 0.601178 0.059 Uiso 0.2907(12) 1 calc R U P A 2
H25F H 0.479254 0.511755 0.595830 0.059 Uiso 0.2907(12) 1 calc R U P A 2
O4' O -0.0125(8) 0.3729(4) 0.7055(4) 0.0239(14) Uani 0.2907(12) 1 d . U P A 2
C4' C -0.0033(14) 0.3738(8) 0.6292(7) 0.0198(17) Uani 0.2907(12) 1 d . U P A 2
C26' C 0.1729(15) 0.3773(9) 0.5260(8) 0.0203(19) Uani 0.2907(12) 1 d . U P A 2
C27' C 0.3464(12) 0.3719(7) 0.5297(8) 0.037(3) Uani 0.2907(12) 1 d . U P A 2
H27D H 0.379071 0.372469 0.476775 0.056 Uiso 0.2907(12) 1 calc R U P A 2
H27E H 0.393692 0.402014 0.559583 0.056 Uiso 0.2907(12) 1 calc R U P A 2
H27F H 0.377489 0.337778 0.554950 0.056 Uiso 0.2907(12) 1 calc R U P A 2
C28' C 0.1247(18) 0.4279(6) 0.4819(8) 0.038(3) Uani 0.2907(12) 1 d . U P A 2
H28D H 0.155403 0.425554 0.428772 0.056 Uiso 0.2907(12) 1 calc R U P A 2
H28E H 0.013723 0.431806 0.480254 0.056 Uiso 0.2907(12) 1 calc R U P A 2
H28F H 0.173650 0.459231 0.508190 0.056 Uiso 0.2907(12) 1 calc R U P A 2
C29' C 0.1069(16) 0.3263(7) 0.4810(9) 0.039(3) Uani 0.2907(12) 1 d . U P A 2
H29D H 0.134282 0.327484 0.427128 0.059 Uiso 0.2907(12) 1 calc R U P A 2
H29E H 0.149436 0.293607 0.506402 0.059 Uiso 0.2907(12) 1 calc R U P A 2
H29F H -0.004349 0.325878 0.481260 0.059 Uiso 0.2907(12) 1 calc R U P A 2
N4' N 0.1325(14) 0.3761(7) 0.6075(7) 0.0208(17) Uani 0.2907(12) 1 d . U P A 2
C30' C -0.1529(13) 0.3777(8) 0.5804(8) 0.027(2) Uani 0.2907(12) 1 d . U P A 2
H30B H -0.134121 0.379586 0.524098 0.032 Uiso 0.2907(12) 1 calc R U P A 2
C31' C -0.2458(13) 0.4243(6) 0.6008(9) 0.036(3) Uani 0.2907(12) 1 d . U P A 2
H31D H -0.341487 0.424758 0.567268 0.054 Uiso 0.2907(12) 1 calc R U P A 2
H31E H -0.268230 0.421458 0.655344 0.054 Uiso 0.2907(12) 1 calc R U P A 2
H31F H -0.189470 0.457766 0.593399 0.054 Uiso 0.2907(12) 1 calc R U P A 2
C32' C -0.2443(14) 0.3217(6) 0.5973(9) 0.036(3) Uani 0.2907(12) 1 d . U P A 2
H32D H -0.183001 0.290623 0.583811 0.054 Uiso 0.2907(12) 1 calc R U P A 2
H32E H -0.262266 0.319890 0.652516 0.054 Uiso 0.2907(12) 1 calc R U P A 2
H32F H -0.342181 0.321157 0.565601 0.054 Uiso 0.2907(12) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Th1 O1' 2.298(7) . ?
Th1 O4' 2.334(7) . ?
Th1 O4 2.356(3) . ?
Th1 O1 2.361(3) . ?
Th1 O2 2.416(3) . ?
Th1 O3 2.424(3) . ?
Th1 O3' 2.430(9) . ?
Th1 O2' 2.491(9) . ?
Th1 N3' 2.533(15) . ?
Th1 N4 2.536(4) . ?
Th1 N1' 2.550(11) . ?
Th1 N3 2.557(5) . ?
O1 C1 1.312(5) . ?
C1 N1 1.299(5) . ?
C1 C9 1.503(6) . ?
C5 N1 1.482(7) . ?
C5 C6 1.524(10) . ?
C5 C8 1.530(11) . ?
C5 C7 1.531(7) . ?
C9 C11 1.515(8) . ?
C9 C10 1.550(8) . ?
O2 C2 1.306(6) . ?
C2 N2 1.309(7) . ?
C2 C16 1.499(7) . ?
C12 N2 1.475(7) . ?
C12 C14 1.527(8) . ?
C12 C13 1.535(7) . ?
C12 C15 1.552(8) . ?
C16 C17 1.534(9) . ?
C16 C18 1.538(8) . ?
O3 C3 1.305(6) . ?
C3 N3 1.310(7) . ?
C3 C23 1.525(7) . ?
C19 N3 1.463(7) . ?
C19 C21 1.531(7) . ?
C19 C20 1.537(8) . ?
C19 C22 1.539(8) . ?
C23 C24 1.513(8) . ?
C23 C25 1.529(8) . ?
O4 C4 1.308(5) . ?
C4 N4 1.312(6) . ?
C4 C30 1.510(7) . ?
C26 N4 1.480(7) . ?
C26 C29 1.491(9) . ?
C26 C27 1.519(6) . ?
C26 C28 1.571(10) . ?
C30 C31 1.498(9) . ?
C30 C32 1.534(10) . ?
O1' C1' 1.310(15) . ?
C1' N1' 1.280(15) . ?
C1' C9' 1.541(19) . ?
C5' N1' 1.462(17) . ?
C5' C8' 1.49(2) . ?
C5' C7' 1.515(17) . ?
C5' C6' 1.61(2) . ?
C9' C11' 1.48(3) . ?
C9' C10' 1.53(3) . ?
O2' C2' 1.343(16) . ?
C2' N2' 1.287(18) . ?
C2' C16' 1.50(2) . ?
C12' N2' 1.46(2) . ?
C12' C15' 1.52(2) . ?
C12' C14' 1.55(2) . ?
C12' C13' 1.553(19) . ?
C16' C17' 1.552(19) . ?
C16' C18' 1.56(2) . ?
O3' C3' 1.293(17) . ?
C3' N3' 1.306(17) . ?
C3' C23' 1.53(2) . ?
C19' N3' 1.46(2) . ?
C19' C21' 1.513(19) . ?
C19' C22' 1.54(2) . ?
C19' C20' 1.56(2) . ?
C23' C24' 1.51(2) . ?
C23' C25' 1.54(2) . ?
O4' C4' 1.325(14) . ?
C4' N4' 1.285(15) . ?
C4' C30' 1.504(17) . ?
C26' N4' 1.479(17) . ?
C26' C28' 1.51(2) . ?
C26' C27' 1.530(17) . ?
C26' C29' 1.57(3) . ?
C30' C31' 1.48(2) . ?
C30' C32' 1.64(2) . ?

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 O4' 90.9(2) . . ?
O4 Th1 O1 88.71(9) . . ?
O4 Th1 O2 120.51(12) . . ?
O1 Th1 O2 121.30(12) . . ?
O4 Th1 O3 122.48(11) . . ?
O1 Th1 O3 119.80(11) . . ?
O2 Th1 O3 87.76(9) . . ?
O1' Th1 O3' 121.5(3) . . ?
O4' Th1 O3' 122.3(3) . . ?
O1' Th1 O2' 121.7(3) . . ?
O4' Th1 O2' 118.5(3) . . ?
O3' Th1 O2' 85.5(3) . . ?
O1' Th1 N3' 85.9(4) . . ?
O4' Th1 N3' 87.7(4) . . ?
O3' Th1 N3' 53.4(4) . . ?
O2' Th1 N3' 138.9(4) . . ?
O4 Th1 N4 53.75(12) . . ?
O1 Th1 N4 142.42(13) . . ?
O2 Th1 N4 84.79(14) . . ?
O3 Th1 N4 84.73(15) . . ?
O1' Th1 N1' 53.8(3) . . ?
O4' Th1 N1' 144.6(4) . . ?
O3' Th1 N1' 84.5(4) . . ?
O2' Th1 N1' 83.3(4) . . ?
N3' Th1 N1' 92.4(5) . . ?
O4 Th1 N3 85.21(15) . . ?
O1 Th1 N3 85.28(15) . . ?
O2 Th1 N3 140.73(14) . . ?
O3 Th1 N3 53.01(14) . . ?
N4 Th1 N3 89.36(18) . . ?
C1 O1 Th1 100.0(2) . . ?
N1 C1 O1 115.9(4) . . ?
N1 C1 C9 129.0(4) . . ?
O1 C1 C9 115.1(4) . . ?
N1 C1 Th1 62.4(3) . . ?
O1 C1 Th1 53.5(2) . . ?
C9 C1 Th1 168.5(3) . . ?
N1 C5 C6 111.2(6) . . ?
N1 C5 C8 111.6(6) . . ?
C6 C5 C8 112.9(5) . . ?
N1 C5 C7 105.7(4) . . ?
C6 C5 C7 106.3(6) . . ?
C8 C5 C7 108.8(5) . . ?
C1 N1 C5 126.5(4) . . ?
C1 N1 Th1 91.0(3) . . ?
C5 N1 Th1 142.6(3) . . ?
C1 C9 C11 110.4(5) . . ?
C1 C9 C10 108.5(5) . . ?
C11 C9 C10 110.8(4) . . ?
C2 O2 Th1 98.9(3) . . ?
O2 C2 N2 116.0(5) . . ?
O2 C2 C16 114.8(5) . . ?
N2 C2 C16 129.2(5) . . ?
O2 C2 Th1 54.9(3) . . ?
N2 C2 Th1 61.1(3) . . ?
C16 C2 Th1 169.6(4) . . ?
N2 C12 C14 111.9(5) . . ?
N2 C12 C13 106.8(5) . . ?
C14 C12 C13 108.0(4) . . ?
N2 C12 C15 110.4(5) . . ?
C14 C12 C15 112.9(5) . . ?
C13 C12 C15 106.5(5) . . ?
C2 N2 C12 126.9(5) . . ?
C2 N2 Th1 92.3(4) . . ?
C12 N2 Th1 140.8(4) . . ?
C2 C16 C17 108.6(5) . . ?
C2 C16 C18 110.6(5) . . ?
C17 C16 C18 111.1(5) . . ?
C3 O3 Th1 98.3(3) . . ?
O3 C3 N3 116.7(5) . . ?
O3 C3 C23 115.0(5) . . ?
N3 C3 C23 128.3(5) . . ?
O3 C3 Th1 55.4(3) . . ?
N3 C3 Th1 61.3(3) . . ?
C23 C3 Th1 170.2(4) . . ?
N3 C19 C21 105.9(5) . . ?
N3 C19 C20 111.7(5) . . ?
C21 C19 C20 108.8(5) . . ?
N3 C19 C22 111.8(5) . . ?
C21 C19 C22 107.5(4) . . ?
C20 C19 C22 110.9(5) . . ?
C3 N3 C19 127.2(5) . . ?
C3 N3 Th1 92.0(4) . . ?
C19 N3 Th1 140.8(4) . . ?
C24 C23 C3 108.7(5) . . ?
C24 C23 C25 109.8(5) . . ?
C3 C23 C25 109.3(5) . . ?
C4 O4 Th1 99.5(3) . . ?
O4 C4 N4 115.6(4) . . ?
O4 C4 C30 114.9(4) . . ?
N4 C4 C30 129.5(4) . . ?
O4 C4 Th1 53.8(2) . . ?
N4 C4 Th1 61.8(3) . . ?
C30 C4 Th1 168.6(4) . . ?
N4 C26 C29 113.3(5) . . ?
N4 C26 C27 106.5(4) . . ?
C29 C26 C27 108.3(5) . . ?
N4 C26 C28 109.3(5) . . ?
C29 C26 C28 112.3(6) . . ?
C27 C26 C28 106.8(5) . . ?
C4 N4 C26 127.1(4) . . ?
C4 N4 Th1 91.1(3) . . ?
C26 N4 Th1 141.8(3) . . ?
C31 C30 C4 110.6(6) . . ?
C31 C30 C32 111.2(5) . . ?
C4 C30 C32 108.8(6) . . ?
C1' O1' Th1 100.1(7) . . ?
N1' C1' O1' 116.8(12) . . ?
N1' C1' C9' 128.5(13) . . ?
O1' C1' C9' 114.6(11) . . ?
N1' C1' Th1 64.0(8) . . ?
O1' C1' Th1 52.9(6) . . ?
C9' C1' Th1 167.4(9) . . ?
N1' C5' C8' 110.9(14) . . ?
N1' C5' C7' 108.9(11) . . ?
C8' C5' C7' 108.5(14) . . ?
N1' C5' C6' 110.2(13) . . ?
C8' C5' C6' 113.4(14) . . ?
C7' C5' C6' 104.6(13) . . ?
C1' N1' C5' 129.3(12) . . ?
C1' N1' Th1 89.2(9) . . ?
C5' N1' Th1 141.3(9) . . ?
C11' C9' C10' 114.0(15) . . ?
C11' C9' C1' 110.6(16) . . ?
C10' C9' C1' 108.7(17) . . ?
C2' O2' Th1 96.9(8) . . ?
N2' C2' O2' 116.4(15) . . ?
N2' C2' C16' 131.8(16) . . ?
O2' C2' C16' 111.8(13) . . ?
N2' C2' Th1 60.0(10) . . ?
O2' C2' Th1 56.4(7) . . ?
C16' C2' Th1 168.2(10) . . ?
N2' C12' C15' 112.1(13) . . ?
N2' C12' C14' 112.3(13) . . ?
C15' C12' C14' 113.8(14) . . ?
N2' C12' C13' 106.1(13) . . ?
C15' C12' C13' 106.2(12) . . ?
C14' C12' C13' 105.6(12) . . ?
C2' N2' C12' 125.0(15) . . ?
C2' N2' Th1 94.4(11) . . ?
C12' N2' Th1 140.6(10) . . ?
C2' C16' C17' 113.6(13) . . ?
C2' C16' C18' 109.2(13) . . ?
C17' C16' C18' 113.0(13) . . ?
C3' O3' Th1 96.7(8) . . ?
O3' C3' N3' 118.3(15) . . ?
O3' C3' C23' 114.8(13) . . ?
N3' C3' C23' 126.8(16) . . ?
O3' C3' Th1 56.9(7) . . ?
N3' C3' Th1 61.5(10) . . ?
C23' C3' Th1 171.5(11) . . ?
N3' C19' C21' 105.7(13) . . ?
N3' C19' C22' 112.4(12) . . ?
C21' C19' C22' 113.1(13) . . ?
N3' C19' C20' 108.5(13) . . ?
C21' C19' C20' 109.3(12) . . ?
C22' C19' C20' 107.7(13) . . ?
C3' N3' C19' 130.2(16) . . ?
C3' N3' Th1 91.6(11) . . ?
C19' N3' Th1 138.1(10) . . ?
C24' C23' C3' 110.1(13) . . ?
C24' C23' C25' 110.1(13) . . ?
C3' C23' C25' 109.1(13) . . ?
C4' O4' Th1 100.8(6) . . ?
N4' C4' O4' 115.4(10) . . ?
N4' C4' C30' 128.8(12) . . ?
O4' C4' C30' 115.5(11) . . ?
N4' C4' Th1 63.0(7) . . ?
O4' C4' Th1 52.5(5) . . ?
C30' C4' Th1 167.2(9) . . ?
N4' C26' C28' 114.5(15) . . ?
N4' C26' C27' 106.3(11) . . ?
C28' C26' C27' 109.2(14) . . ?
N4' C26' C29' 110.2(14) . . ?
C28' C26' C29' 110.2(12) . . ?
C27' C26' C29' 106.0(14) . . ?
C4' N4' C26' 125.7(11) . . ?
C4' N4' Th1 90.7(8) . . ?
C26' N4' Th1 143.6(9) . . ?
C31' C30' C4' 113.2(14) . . ?
C31' C30' C32' 109.2(10) . . ?
C4' C30' C32' 105.4(14) . . ?

_refine_diff_density_max         0.906
_refine_diff_density_min         -1.505
_refine_diff_density_rms         0.095

