# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_COMPOUND1
_database_code_depnum_ccdc_archive 'CCDC 1423711'
_audit_update_record             
;
2015-11-30 deposited with the CCDC.
2015-12-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            "1,3,5-tri(4'-carboxylphenyl) benzoic thorium"
_chemical_melting_point          N/A
_chemical_formula_moiety         Th2(C27H15O6)2Cl7(C7H11N2)5
_chemical_formula_sum            'C89 H85 Cl7 N10 O12 Th2'
_chemical_formula_weight         2198.89

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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   17.427(3)
_cell_length_b                   30.021(5)
_cell_length_c                   18.374(4)
_cell_angle_alpha                90
_cell_angle_beta                 114.813(4)
_cell_angle_gamma                90
_cell_volume                     8725(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    8652
_cell_measurement_theta_min      2.333
_cell_measurement_theta_max      26.095

_exptl_crystal_description       bulk
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_F_000             4336
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    3.686
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'BRUKER apex II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_detector_area_resol_mean 0
_diffrn_reflns_number            129349
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_av_R_equivalents  0.1517
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.333
_diffrn_reflns_theta_max         26.095
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.876
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8652
_reflns_number_gt                6757
_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 SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0097P)²+928.2795P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8652
_refine_ls_number_parameters     583
_refine_ls_number_restraints     150
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0843
_refine_ls_wR_factor_ref         0.1867
_refine_ls_wR_factor_gt          0.1730
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.053
_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 0.30378(3) 0.61037(2) 0.41391(3) 0.01807(14) Uani 1 1 d . . . . .
Cl1 Cl 0.2296(3) 0.57154(14) 0.5111(3) 0.0448(11) Uani 1 1 d . . . . .
Cl2 Cl 0.2557(3) 0.62119(13) 0.2499(3) 0.0382(9) Uani 1 1 d . . . . .
Cl3 Cl 0.4213(3) 0.62540(16) 0.5701(3) 0.0536(12) Uani 1 1 d . . . . .
O1 O 0.3691(7) 0.5344(3) 0.4373(7) 0.029(2) Uani 1 1 d . . . . .
O2 O 0.2370(6) 0.5378(3) 0.3476(6) 0.028(2) Uani 1 1 d . . . . .
O3 O -0.0600(6) 0.1125(3) 0.3924(6) 0.030(2) Uani 1 1 d . U . . .
O4 O -0.1213(7) 0.1766(3) 0.4025(7) 0.038(3) Uani 1 1 d . U . . .
O5 O 0.7316(7) 0.1742(3) 0.4404(8) 0.040(3) Uani 1 1 d . . . . .
O6 O 0.6484(6) 0.1267(3) 0.3518(7) 0.034(3) Uani 1 1 d . . . . .
C1 C 0.3009(9) 0.5154(4) 0.3906(9) 0.021(3) Uani 1 1 d . . . . .
C2 C 0.3722(9) 0.4409(4) 0.4310(9) 0.022(3) Uani 1 1 d . . . . .
H2A H 0.4238 0.4555 0.4626 0.026 Uiso 1 1 calc R U . . .
C3 C 0.2996(9) 0.4661(4) 0.3867(9) 0.023(3) Uani 1 1 d . . . . .
C4 C 0.2262(9) 0.4432(5) 0.3396(9) 0.027(3) Uani 1 1 d . . . . .
H4A H 0.1774 0.4597 0.3070 0.032 Uiso 1 1 calc R U . . .
C5 C 0.2212(9) 0.3968(4) 0.3383(9) 0.026(3) Uani 1 1 d . . . . .
H5A H 0.1695 0.3822 0.3068 0.031 Uiso 1 1 calc R U . . .
C6 C 0.2934(8) 0.3723(4) 0.3840(8) 0.019(3) Uani 1 1 d . . . . .
C7 C 0.3689(9) 0.3948(5) 0.4289(9) 0.026(3) Uani 1 1 d . . . . .
H7A H 0.4187 0.3782 0.4584 0.031 Uiso 1 1 calc R U . . .
C8 C 0.2925(9) 0.3229(4) 0.3842(9) 0.023(3) Uani 1 1 d . . . . .
C9 C 0.3625(9) 0.2995(5) 0.3881(10) 0.027(3) Uani 1 1 d . . . . .
H9A H 0.4112 0.3154 0.3918 0.033 Uiso 1 1 calc R U . . .
C10 C 0.3635(9) 0.2524(5) 0.3867(9) 0.025(3) Uani 1 1 d . . . . .
C11 C 0.2909(9) 0.2300(5) 0.3806(10) 0.030(4) Uani 1 1 d . . . . .
H11A H 0.2893 0.1985 0.3768 0.036 Uiso 1 1 calc R U . . .
C12 C 0.2214(9) 0.2525(4) 0.3798(9) 0.021(3) Uani 1 1 d . . . . .
C13 C 0.2222(8) 0.2996(4) 0.3794(9) 0.022(3) Uani 1 1 d . U . . .
H13A H 0.1736 0.3155 0.3759 0.026 Uiso 1 1 calc R U . . .
C14 C 0.1457(8) 0.2280(4) 0.3777(9) 0.021(3) Uani 1 1 d . . . . .
C15 C 0.1349(10) 0.1823(5) 0.3612(11) 0.040(4) Uani 1 1 d . U . . .
H15A H 0.1733 0.1669 0.3456 0.048 Uiso 1 1 calc R U . . .
C16 C 0.0690(10) 0.1592(5) 0.3672(11) 0.038(4) Uani 1 1 d . U . . .
H16A H 0.0659 0.1278 0.3595 0.046 Uiso 1 1 calc R U . . .
C17 C 0.0094(8) 0.1796(4) 0.3835(9) 0.021(3) Uani 1 1 d . . . . .
C18 C 0.0159(12) 0.2262(6) 0.3957(16) 0.063(7) Uani 1 1 d . . . . .
H18A H -0.0270 0.2421 0.4037 0.076 Uiso 1 1 calc R U . . .
C19 C 0.0852(11) 0.2483(6) 0.3958(12) 0.042(4) Uani 1 1 d . U . . .
H19A H 0.0914 0.2791 0.4090 0.051 Uiso 1 1 calc R U . . .
C20 C -0.0595(8) 0.1558(4) 0.3946(7) 0.014(3) Uani 1 1 d . U . . .
C21 C 0.4395(9) 0.2285(5) 0.3892(10) 0.027(3) Uani 1 1 d . U . . .
C22 C 0.5199(10) 0.2442(5) 0.4358(11) 0.035(4) Uani 1 1 d . U . . .
H22A H 0.5266 0.2707 0.4662 0.042 Uiso 1 1 calc R U . . .
C23 C 0.5901(9) 0.2222(5) 0.4390(10) 0.027(3) Uani 1 1 d . U . . .
H23A H 0.6449 0.2328 0.4728 0.032 Uiso 1 1 calc R U . . .
C24 C 0.5811(9) 0.1844(5) 0.3928(9) 0.026(3) Uani 1 1 d . . . . .
C25 C 0.5009(9) 0.1685(5) 0.3456(10) 0.034(4) Uani 1 1 d . . . . .
H25A H 0.4943 0.1426 0.3137 0.041 Uiso 1 1 calc R U . . .
C26 C 0.4295(9) 0.1903(5) 0.3446(11) 0.034(4) Uani 1 1 d . . . . .
H26A H 0.3746 0.1789 0.3134 0.040 Uiso 1 1 calc R U . . .
C27 C 0.6559(9) 0.1611(4) 0.3931(9) 0.026(3) Uani 1 1 d . . . . .
N1 N 0.4452(9) 0.5053(5) 0.8112(9) 0.045(4) Uani 1 1 d . . . . .
N2 N 0.3242(10) 0.5008(5) 0.7077(9) 0.047(4) Uani 1 1 d . . . . .
C28 C 0.5214(13) 0.4909(8) 0.8806(13) 0.064(6) Uani 1 1 d . . . . .
H28A H 0.5577 0.5168 0.9042 0.095 Uiso 1 1 calc R U . . .
H28B H 0.5052 0.4773 0.9206 0.095 Uiso 1 1 calc R U . . .
H28C H 0.5521 0.4691 0.8633 0.095 Uiso 1 1 calc R U . . .
C29 C 0.3835(11) 0.4772(6) 0.7665(11) 0.042(4) Uani 1 1 d . . . . .
H29A H 0.3821 0.4460 0.7751 0.051 Uiso 1 1 calc R U . . .
C30 C 0.3517(14) 0.5449(6) 0.7147(12) 0.051(5) Uani 1 1 d . . . . .
H30A H 0.3228 0.5686 0.6798 0.061 Uiso 1 1 calc R U . . .
C31 C 0.4239(12) 0.5479(6) 0.7775(12) 0.044(4) Uani 1 1 d . . . . .
H31A H 0.4562 0.5743 0.7969 0.053 Uiso 1 1 calc R U . . .
C32 C 0.2437(12) 0.4820(7) 0.6445(12) 0.055(5) Uani 1 1 d . . . . .
H32A H 0.2204 0.4592 0.6686 0.066 Uiso 1 1 calc R U . . .
H32B H 0.2013 0.5060 0.6221 0.066 Uiso 1 1 calc R U . . .
C33 C 0.2615(17) 0.4614(8) 0.5790(14) 0.071(7) Uani 1 1 d . . . . .
H33A H 0.2811 0.4804 0.5490 0.086 Uiso 1 1 calc R U . . .
C34 C 0.2522(19) 0.4207(9) 0.5607(17) 0.093(10) Uani 1 1 d . . . . .
H34A H 0.2327 0.4007 0.5894 0.111 Uiso 1 1 calc R U . . .
H34B H 0.2648 0.4099 0.5183 0.111 Uiso 1 1 calc R U . . .
N3 N 0.7421(10) 0.1993(5) 0.6509(9) 0.049(4) Uani 1 1 d . . . . .
N4 N 0.6443(10) 0.1528(5) 0.6335(10) 0.050(4) Uani 1 1 d . . . . .
C35 C 0.8172(18) 0.2206(10) 0.6493(17) 0.096(10) Uani 1 1 d . . . . .
H35A H 0.8252 0.2500 0.6747 0.145 Uiso 1 1 calc R U . . .
H35B H 0.8670 0.2021 0.6785 0.145 Uiso 1 1 calc R U . . .
H35C H 0.8095 0.2240 0.5936 0.145 Uiso 1 1 calc R U . . .
C36 C 0.7142(14) 0.1602(7) 0.6221(13) 0.058(6) Uani 1 1 d . . . . .
H36A H 0.7387 0.1404 0.5975 0.070 Uiso 1 1 calc R U . . .
C37 C 0.6317(13) 0.1879(6) 0.6726(11) 0.049(5) Uani 1 1 d . . . . .
H37A H 0.5873 0.1910 0.6893 0.059 Uiso 1 1 calc R U . . .
C38 C 0.6923(14) 0.2172(7) 0.6838(13) 0.056(5) Uani 1 1 d . . . . .
H38A H 0.6995 0.2453 0.7097 0.068 Uiso 1 1 calc R U . . .
C39 C 0.5859(19) 0.1126(8) 0.6070(15) 0.085(8) Uani 1 1 d . . . . .
H39A H 0.6157 0.0871 0.5962 0.102 Uiso 1 1 calc R U . . .
H39B H 0.5689 0.1038 0.6501 0.102 Uiso 1 1 calc R U . . .
C40 C 0.517(2) 0.1230(12) 0.540(2) 0.124(12) Uani 1 1 d . U . . .
H40A H 0.5255 0.1281 0.4930 0.149 Uiso 1 1 calc R U . . .
C41 C 0.432(2) 0.1273(11) 0.533(2) 0.130(12) Uani 1 1 d . U . . .
H41A H 0.4203 0.1226 0.5787 0.156 Uiso 1 1 calc R U . . .
H41B H 0.3875 0.1349 0.4831 0.156 Uiso 1 1 calc R U . . .
N5 N 0.0303(13) 0.4977(8) 0.3414(13) 0.093(11) Uani 0.5 1 d D U P A -1
N6 N -0.0356(11) 0.5104(8) 0.2157(12) 0.076(8) Uani 0.5 1 d D U P A -1
C42 C 0.080(2) 0.4758(12) 0.4164(17) 0.13(2) Uani 0.5 1 d D U P A -1
H42A H 0.0854 0.4949 0.4603 0.199 Uiso 0.5 1 d R U P A -1
H42B H 0.0525 0.4486 0.4195 0.199 Uiso 0.5 1 d R U P A -1
H42C H 0.1351 0.4693 0.4193 0.199 Uiso 0.5 1 d R U P A -1
C43 C 0.0112(17) 0.4785(7) 0.2686(15) 0.084(10) Uani 0.5 1 d D U P A -1
H43A H 0.0274 0.4497 0.2570 0.100 Uiso 0.5 1 d R U P A -1
C44 C -0.0457(19) 0.5475(8) 0.2528(15) 0.073(10) Uani 0.5 1 d D U P A -1
H44A H -0.0764 0.5740 0.2279 0.088 Uiso 0.5 1 d R U P A -1
C45 C -0.0025(19) 0.5393(8) 0.3352(15) 0.091(11) Uani 0.5 1 d D U P A -1
H45A H 0.0023 0.5586 0.3785 0.109 Uiso 0.5 1 d R U P A -1
C46 C -0.0706(17) 0.5053(12) 0.1299(13) 0.075(9) Uani 0.5 1 d D U P A -1
H46A H -0.1243 0.5201 0.1061 0.090 Uiso 0.5 1 d R U P A -1
H46B H -0.0798 0.4743 0.1167 0.090 Uiso 0.5 1 d R U P A -1
C47 C -0.015(2) 0.5221(17) 0.0926(17) 0.085(11) Uani 0.5 1 d D U P A -1
H47A H -0.0260 0.5191 0.0370 0.103 Uiso 0.5 1 d R U P A -1
C48 C 0.053(2) 0.5440(16) 0.141(3) 0.103(16) Uani 0.5 1 d D U P A -1
H48A H 0.0616 0.5461 0.1960 0.123 Uiso 0.5 1 d R U P A -1
H48B H 0.0929 0.5570 0.1240 0.123 Uiso 0.5 1 d R U P A -1
Cl4 Cl 0.0000 0.3662(2) 0.2500 0.0507(17) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Th1 O4 2.435(11) 3 ?
Th1 O5 2.450(10) 3_455 ?
Th1 O1 2.505(9) . ?
Th1 O6 2.506(10) 3_455 ?
Th1 O2 2.530(10) . ?
Th1 O3 2.566(9) 3 ?
Th1 Cl3 2.775(5) . ?
Th1 Cl2 2.787(4) . ?
Th1 Cl1 2.856(4) . ?
Th1 C1 2.879(13) . ?
Th1 C27 2.878(13) 3_455 ?
Th1 C20 2.893(12) 3 ?
O1 C1 1.271(17) . ?
O2 C1 1.255(17) . ?
O3 C20 1.299(16) . ?
O3 Th1 2.566(9) 3_445 ?
O4 C20 1.305(15) . ?
O4 Th1 2.435(11) 3_445 ?
O5 C27 1.299(18) . ?
O5 Th1 2.450(10) 3_545 ?
O6 C27 1.254(17) . ?
O6 Th1 2.506(10) 3_545 ?
C1 C3 1.483(17) . ?
C2 C7 1.384(19) . ?
C2 C3 1.404(19) . ?
C3 C4 1.39(2) . ?
C4 C5 1.393(18) . ?
C5 C6 1.394(19) . ?
C6 C7 1.398(19) . ?
C6 C8 1.483(17) . ?
C8 C9 1.385(18) . ?
C8 C13 1.381(18) . ?
C9 C10 1.412(19) . ?
C10 C11 1.395(19) . ?
C10 C21 1.491(18) . ?
C11 C12 1.381(19) . ?
C12 C13 1.415(18) . ?
C12 C14 1.497(17) . ?
C14 C19 1.37(2) . ?
C14 C15 1.40(2) . ?
C15 C16 1.39(2) . ?
C16 C17 1.34(2) . ?
C17 C18 1.41(2) . ?
C17 C20 1.484(17) . ?
C18 C19 1.38(2) . ?
C20 Th1 2.893(12) 3_445 ?
C21 C26 1.38(2) . ?
C21 C22 1.38(2) . ?
C22 C23 1.37(2) . ?
C23 C24 1.38(2) . ?
C24 C25 1.38(2) . ?
C24 C27 1.478(18) . ?
C25 C26 1.399(19) . ?
C27 Th1 2.878(13) 3_545 ?
N1 C29 1.34(2) . ?
N1 C31 1.40(2) . ?
N1 C28 1.47(2) . ?
N2 C29 1.34(2) . ?
N2 C30 1.39(2) . ?
N2 C32 1.51(2) . ?
C30 C31 1.31(3) . ?
C32 C33 1.50(3) . ?
C33 C34 1.26(3) . ?
N3 C36 1.29(2) . ?
N3 C38 1.36(2) . ?
N3 C35 1.47(2) . ?
N4 C36 1.34(2) . ?
N4 C37 1.34(2) . ?
N4 C39 1.52(3) . ?
C37 C38 1.32(3) . ?
C39 C40 1.34(4) . ?
C40 C41 1.44(4) . ?
N5 C45 1.357(9) . ?
N5 C43 1.363(9) . ?
N5 C42 1.443(9) . ?
N6 C44 1.356(9) . ?
N6 C43 1.364(9) . ?
N6 C46 1.439(9) . ?
C44 C45 1.401(9) . ?
C46 C47 1.494(10) . ?
C47 C48 1.315(10) . ?

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
O4 Th1 O5 73.6(3) 3 3_455 ?
O4 Th1 O1 122.5(3) 3 . ?
O5 Th1 O1 155.8(4) 3_455 . ?
O4 Th1 O6 108.5(4) 3 3_455 ?
O5 Th1 O6 52.4(3) 3_455 3_455 ?
O1 Th1 O6 125.6(3) . 3_455 ?
O4 Th1 O2 144.8(4) 3 . ?
O5 Th1 O2 126.7(3) 3_455 . ?
O1 Th1 O2 51.8(3) . . ?
O6 Th1 O2 76.0(3) 3_455 . ?
O4 Th1 O3 53.3(3) 3 3 ?
O5 Th1 O3 126.6(3) 3_455 3 ?
O1 Th1 O3 70.5(3) . 3 ?
O6 Th1 O3 144.9(4) 3_455 3 ?
O2 Th1 O3 102.5(3) . 3 ?
O4 Th1 Cl3 76.5(3) 3 . ?
O5 Th1 Cl3 83.4(3) 3_455 . ?
O1 Th1 Cl3 83.4(3) . . ?
O6 Th1 Cl3 128.8(3) 3_455 . ?
O2 Th1 Cl3 129.0(2) . . ?
O3 Th1 Cl3 80.0(3) 3 . ?
O4 Th1 Cl2 75.0(3) 3 . ?
O5 Th1 Cl2 100.2(3) 3_455 . ?
O1 Th1 Cl2 101.6(3) . . ?
O6 Th1 Cl2 73.0(3) 3_455 . ?
O2 Th1 Cl2 73.2(2) . . ?
O3 Th1 Cl2 73.1(3) 3 . ?
Cl3 Th1 Cl2 148.84(14) . . ?
O4 Th1 Cl1 141.9(3) 3 . ?
O5 Th1 Cl1 77.9(3) 3_455 . ?
O1 Th1 Cl1 79.2(3) . . ?
O6 Th1 Cl1 71.2(3) 3_455 . ?
O2 Th1 Cl1 73.3(3) . . ?
O3 Th1 Cl1 142.9(3) 3 . ?
Cl3 Th1 Cl1 75.57(15) . . ?
Cl2 Th1 Cl1 135.57(13) . . ?
O4 Th1 C1 140.5(3) 3 . ?
O5 Th1 C1 145.6(4) 3_455 . ?
O1 Th1 C1 26.1(4) . . ?
O6 Th1 C1 100.2(4) 3_455 . ?
O2 Th1 C1 25.8(4) . . ?
O3 Th1 C1 87.8(3) 3 . ?
Cl3 Th1 C1 105.9(3) . . ?
Cl2 Th1 C1 88.6(3) . . ?
Cl1 Th1 C1 72.8(3) . . ?
O4 Th1 C27 92.3(4) 3 3_455 ?
O5 Th1 C27 26.7(4) 3_455 3_455 ?
O1 Th1 C27 145.3(4) . 3_455 ?
O6 Th1 C27 25.8(4) 3_455 3_455 ?
O2 Th1 C27 100.7(4) . 3_455 ?
O3 Th1 C27 143.3(4) 3 3_455 ?
Cl3 Th1 C27 106.4(3) . 3_455 ?
Cl2 Th1 C27 87.1(3) . 3_455 ?
Cl1 Th1 C27 71.6(3) . 3_455 ?
C1 Th1 C27 123.0(4) . 3_455 ?
O4 Th1 C20 26.6(3) 3 3 ?
O5 Th1 C20 100.0(4) 3_455 3 ?
O1 Th1 C20 96.4(3) . 3 ?
O6 Th1 C20 129.8(4) 3_455 3 ?
O2 Th1 C20 125.6(3) . 3 ?
O3 Th1 C20 26.7(3) 3 3 ?
Cl3 Th1 C20 76.2(3) . 3 ?
Cl2 Th1 C20 72.6(3) . 3 ?
Cl1 Th1 C20 151.8(3) . 3 ?
C1 Th1 C20 114.3(3) . 3 ?
C27 Th1 C20 118.2(4) 3_455 3 ?
C1 O1 Th1 93.6(8) . . ?
C1 O2 Th1 92.8(8) . . ?
C20 O3 Th1 90.8(7) . 3_445 ?
C20 O4 Th1 96.7(8) . 3_445 ?
C27 O5 Th1 95.3(8) . 3_545 ?
C27 O6 Th1 93.9(9) . 3_545 ?
O2 C1 O1 121.2(12) . . ?
O2 C1 C3 120.8(13) . . ?
O1 C1 C3 118.0(12) . . ?
O2 C1 Th1 61.3(7) . . ?
O1 C1 Th1 60.3(6) . . ?
C3 C1 Th1 174.3(10) . . ?
C7 C2 C3 120.4(13) . . ?
C4 C3 C2 117.6(12) . . ?
C4 C3 C1 121.1(13) . . ?
C2 C3 C1 121.3(13) . . ?
C3 C4 C5 122.7(14) . . ?
C4 C5 C6 118.8(13) . . ?
C5 C6 C7 119.3(12) . . ?
C5 C6 C8 121.4(12) . . ?
C7 C6 C8 119.3(12) . . ?
C2 C7 C6 121.1(13) . . ?
C9 C8 C13 118.9(11) . . ?
C9 C8 C6 119.9(12) . . ?
C13 C8 C6 121.2(12) . . ?
C8 C9 C10 121.6(12) . . ?
C11 C10 C9 117.8(12) . . ?
C11 C10 C21 122.2(12) . . ?
C9 C10 C21 120.0(12) . . ?
C12 C11 C10 121.9(12) . . ?
C11 C12 C13 118.5(12) . . ?
C11 C12 C14 121.4(12) . . ?
C13 C12 C14 120.1(11) . . ?
C8 C13 C12 121.2(12) . . ?
C19 C14 C15 116.2(13) . . ?
C19 C14 C12 122.2(12) . . ?
C15 C14 C12 121.5(12) . . ?
C16 C15 C14 120.8(14) . . ?
C17 C16 C15 122.3(14) . . ?
C16 C17 C18 117.9(13) . . ?
C16 C17 C20 123.9(12) . . ?
C18 C17 C20 118.1(12) . . ?
C19 C18 C17 119.3(15) . . ?
C18 C19 C14 123.1(16) . . ?
O3 C20 O4 119.2(11) . . ?
O3 C20 C17 118.2(11) . . ?
O4 C20 C17 122.6(11) . . ?
O3 C20 Th1 62.5(6) . 3_445 ?
O4 C20 Th1 56.7(7) . 3_445 ?
C17 C20 Th1 178.9(10) . 3_445 ?
C26 C21 C22 119.7(13) . . ?
C26 C21 C10 119.6(13) . . ?
C22 C21 C10 120.7(13) . . ?
C23 C22 C21 121.0(15) . . ?
C22 C23 C24 120.0(14) . . ?
C25 C24 C23 119.4(13) . . ?
C25 C24 C27 119.7(13) . . ?
C23 C24 C27 120.8(13) . . ?
C24 C25 C26 120.3(15) . . ?
C21 C26 C25 119.5(14) . . ?
O6 C27 O5 118.1(12) . . ?
O6 C27 C24 121.3(13) . . ?
O5 C27 C24 120.4(13) . . ?
O6 C27 Th1 60.3(7) . 3_545 ?
O5 C27 Th1 58.0(7) . 3_545 ?
C24 C27 Th1 172.3(10) . 3_545 ?
C29 N1 C31 108.0(15) . . ?
C29 N1 C28 123.1(16) . . ?
C31 N1 C28 128.9(17) . . ?
C29 N2 C30 108.0(16) . . ?
C29 N2 C32 125.1(16) . . ?
C30 N2 C32 126.9(17) . . ?
N2 C29 N1 107.9(16) . . ?
C31 C30 N2 108.3(18) . . ?
C30 C31 N1 107.8(17) . . ?
C33 C32 N2 109.6(17) . . ?
C34 C33 C32 125(2) . . ?
C36 N3 C38 109.9(17) . . ?
C36 N3 C35 125(2) . . ?
C38 N3 C35 125.2(19) . . ?
C36 N4 C37 108.5(17) . . ?
C36 N4 C39 127.7(19) . . ?
C37 N4 C39 123.8(17) . . ?
N3 C36 N4 107.3(19) . . ?
C38 C37 N4 107.8(17) . . ?
C37 C38 N3 106.5(18) . . ?
C40 C39 N4 109(2) . . ?
C39 C40 C41 126(4) . . ?
C45 N5 C43 112.7(9) . . ?
C45 N5 C42 124.1(14) . . ?
C43 N5 C42 123.1(13) . . ?
C44 N6 C43 112.5(9) . . ?
C44 N6 C46 123.6(13) . . ?
C43 N6 C46 123.9(13) . . ?
N5 C43 N6 103.3(9) . . ?
N6 C44 C45 106.0(9) . . ?
N5 C45 C44 105.5(9) . . ?
N6 C46 C47 114.1(13) . . ?
C48 C47 C46 115.4(16) . . ?

_refine_diff_density_max         2.832
_refine_diff_density_min         -4.335
_refine_diff_density_rms         0.227

####################################################################### 
# 
# 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_compound3
_database_code_depnum_ccdc_archive 'CCDC 1423712'
_audit_update_record             
;
2015-11-25 deposited with the CCDC.
2015-12-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            "4,4',4'-nitrilotribenzoic thorium"
_chemical_melting_point          N/A
_chemical_formula_moiety         Th2(C21H1206N)3(H2O)2
_chemical_formula_sum            'C63 H36 N3 O20 Th2'
_chemical_formula_weight         1619.03

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   24.8612(19)
_cell_length_b                   24.8612(19)
_cell_length_c                   28.260(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     15127(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    3751
_cell_measurement_theta_min      2.713
_cell_measurement_theta_max      27.297

_exptl_crystal_description       cubic
_exptl_crystal_colour            claybank
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.066
_exptl_crystal_F_000             4650
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.025
_exptl_absorpt_coefficient_mu    2.993
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'BRUKER apex II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_detector_area_resol_mean 0
_diffrn_reflns_number            24919
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.713
_diffrn_reflns_theta_max         27.297
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             3751
_reflns_number_gt                2376
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0371P)²+35.2887P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3751
_refine_ls_number_parameters     135
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0242
_refine_ls_wR_factor_ref         0.0711
_refine_ls_wR_factor_gt          0.0625
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_restrained_S_all      0.957
_refine_ls_shift/su_max          0.000
_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 0.6667 0.3333 -0.01223(2) 0.02591(7) Uani 1 3 d S T P . .
O1 O 0.61050(12) 0.38978(11) -0.05093(9) 0.0484(6) Uani 1 1 d . . . . .
C3 C 0.65485(16) 0.50075(16) -0.05072(13) 0.0402(8) Uani 1 1 d . . . . .
C1 C 0.65348(16) 0.61110(17) -0.07154(15) 0.0511(11) Uani 1 1 d . . . . .
C9 C 0.65703(17) 0.44269(16) -0.04123(12) 0.0403(8) Uani 1 1 d . . . . .
N1 N 0.65388(16) 0.6667 -0.0833 0.0605(14) Uani 1 2 d S T P . .
C2 C 0.70427(16) 0.61315(16) -0.04778(15) 0.0526(10) Uani 1 1 d . . . . .
H2A H 0.7383 0.6520 -0.0383 0.063 Uiso 1 1 calc R U . . .
C6 C 0.70469(17) 0.55828(16) -0.03808(14) 0.0485(9) Uani 1 1 d . . . . .
H6A H 0.7396 0.5603 -0.0226 0.058 Uiso 1 1 calc R U . . .
C5 C 0.60260(18) 0.55327(18) -0.08258(17) 0.0640(13) Uani 1 1 d . . . . .
H5A H 0.5673 0.5511 -0.0975 0.077 Uiso 1 1 calc R U . . .
C7 C 0.59620(19) 0.6667 -0.0833 0.0508(15) Uani 1 2 d S T P . .
C4 C 0.60293(18) 0.49873(17) -0.07205(15) 0.0578(11) Uani 1 1 d . . . . .
H4A H 0.5676 0.4597 -0.0794 0.069 Uiso 1 1 calc R U . . .
C8 C 0.55899(17) 0.64881(19) -0.04314(15) 0.0593(12) Uani 1 1 d . . . . .
H8A H 0.5721 0.6368 -0.0155 0.071 Uiso 1 1 calc R U . . .
O2 O 0.70557(12) 0.44675(11) -0.02334(10) 0.0498(7) Uani 1 1 d . . . . .
C11 C 0.48318(18) 0.6667 -0.0833 0.0371(11) Uani 1 2 d S T P . .
C10 C 0.50258(17) 0.64836(18) -0.04292(14) 0.0523(10) Uani 1 1 d . . . . .
H10A H 0.4773 0.6356 -0.0153 0.063 Uiso 1 1 calc R U . . .
C12 C 0.42288(16) 0.6667 -0.0833 0.0298(10) Uani 1 2 d S T P . .
O3 O 0.38812(10) 0.64411(10) -0.04766(8) 0.0355(5) Uani 1 1 d . . . . .
O5 O 0.6667 0.3333 -0.10313(19) 0.0737(16) Uani 1 3 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Th1 O3 2.408(2) 20 ?
Th1 O3 2.408(2) 21_655 ?
Th1 O3 2.408(2) 19_665 ?
Th1 O2 2.501(2) 3_665 ?
Th1 O2 2.501(2) 2_655 ?
Th1 O2 2.501(2) . ?
Th1 O5 2.569(5) . ?
Th1 O1 2.660(2) 2_655 ?
Th1 O1 2.660(2) 3_665 ?
Th1 O1 2.660(2) . ?
Th1 C9 2.962(3) 2_655 ?
Th1 C9 2.962(3) . ?
O1 C9 1.274(4) . ?
C3 C6 1.392(5) . ?
C3 C4 1.403(5) . ?
C3 C9 1.495(4) . ?
C1 C2 1.408(5) . ?
C1 C5 1.395(5) . ?
C1 N1 1.416(4) . ?
C9 O2 1.265(4) . ?
N1 C7 1.434(6) . ?
N1 C1 1.416(4) 11_564 ?
C2 C6 1.397(5) . ?
C5 C4 1.392(5) . ?
C7 C8 1.390(4) . ?
C7 C8 1.390(4) 11_564 ?
C8 C10 1.397(5) . ?
C11 C10 1.401(4) 11_564 ?
C11 C10 1.401(4) . ?
C11 C12 1.499(6) . ?
C12 O3 1.262(3) 11_564 ?
C12 O3 1.262(3) . ?
O3 Th1 2.408(2) 19_665 ?

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
O3 Th1 O3 76.05(8) 20 21_655 ?
O3 Th1 O3 76.05(8) 20 19_665 ?
O3 Th1 O3 76.05(8) 21_655 19_665 ?
O3 Th1 O2 72.62(8) 20 3_665 ?
O3 Th1 O2 76.74(8) 21_655 3_665 ?
O3 Th1 O2 142.45(9) 19_665 3_665 ?
O3 Th1 O2 76.74(8) 20 2_655 ?
O3 Th1 O2 142.45(9) 21_655 2_655 ?
O3 Th1 O2 72.62(8) 19_665 2_655 ?
O2 Th1 O2 118.45(3) 3_665 2_655 ?
O3 Th1 O2 142.45(9) 20 . ?
O3 Th1 O2 72.62(8) 21_655 . ?
O3 Th1 O2 76.74(8) 19_665 . ?
O2 Th1 O2 118.45(3) 3_665 . ?
O2 Th1 O2 118.45(3) 2_655 . ?
O3 Th1 O5 134.66(5) 20 . ?
O3 Th1 O5 134.66(5) 21_655 . ?
O3 Th1 O5 134.66(5) 19_665 . ?
O2 Th1 O5 82.79(7) 3_665 . ?
O2 Th1 O5 82.79(7) 2_655 . ?
O2 Th1 O5 82.79(7) . . ?
O3 Th1 O1 70.05(8) 20 2_655 ?
O3 Th1 O1 137.41(8) 21_655 2_655 ?
O3 Th1 O1 118.16(7) 19_665 2_655 ?
O2 Th1 O1 69.17(8) 3_665 2_655 ?
O2 Th1 O1 50.41(8) 2_655 2_655 ?
O2 Th1 O1 146.93(9) . 2_655 ?
O5 Th1 O1 65.72(6) . 2_655 ?
O3 Th1 O1 118.16(7) 20 3_665 ?
O3 Th1 O1 70.05(8) 21_655 3_665 ?
O3 Th1 O1 137.41(8) 19_665 3_665 ?
O2 Th1 O1 50.42(8) 3_665 3_665 ?
O2 Th1 O1 146.93(9) 2_655 3_665 ?
O2 Th1 O1 69.16(8) . 3_665 ?
O5 Th1 O1 65.72(6) . 3_665 ?
O1 Th1 O1 104.27(7) 2_655 3_665 ?
O3 Th1 O1 137.41(8) 20 . ?
O3 Th1 O1 118.16(7) 21_655 . ?
O3 Th1 O1 70.05(8) 19_665 . ?
O2 Th1 O1 146.93(9) 3_665 . ?
O2 Th1 O1 69.17(8) 2_655 . ?
O2 Th1 O1 50.42(8) . . ?
O5 Th1 O1 65.72(6) . . ?
O1 Th1 O1 104.26(7) 2_655 . ?
O1 Th1 O1 104.26(7) 3_665 . ?
O3 Th1 C9 70.49(8) 20 2_655 ?
O3 Th1 C9 146.53(9) 21_655 2_655 ?
O3 Th1 C9 94.79(9) 19_665 2_655 ?
O2 Th1 C9 93.81(9) 3_665 2_655 ?
O2 Th1 C9 25.00(9) 2_655 2_655 ?
O2 Th1 C9 137.36(9) . 2_655 ?
O5 Th1 C9 73.93(7) . 2_655 ?
O1 Th1 C9 25.46(8) 2_655 2_655 ?
O1 Th1 C9 127.60(9) 3_665 2_655 ?
O1 Th1 C9 87.21(8) . 2_655 ?
O3 Th1 C9 146.53(9) 20 . ?
O3 Th1 C9 94.79(9) 21_655 . ?
O3 Th1 C9 70.49(8) 19_665 . ?
O2 Th1 C9 137.36(9) 3_665 . ?
O2 Th1 C9 93.81(9) 2_655 . ?
O2 Th1 C9 25.00(9) . . ?
O5 Th1 C9 73.93(7) . . ?
O1 Th1 C9 127.60(9) 2_655 . ?
O1 Th1 C9 87.21(8) 3_665 . ?
O1 Th1 C9 25.47(8) . . ?
C9 Th1 C9 112.65(6) 2_655 . ?
C9 O1 Th1 90.6(2) . . ?
C6 C3 C4 118.5(3) . . ?
C6 C3 C9 120.2(3) . . ?
C4 C3 C9 121.3(3) . . ?
C2 C1 C5 118.6(3) . . ?
C2 C1 N1 120.5(3) . . ?
C5 C1 N1 120.9(3) . . ?
O2 C9 O1 120.4(3) . . ?
O2 C9 C3 119.2(3) . . ?
O1 C9 C3 120.4(3) . . ?
O2 C9 Th1 56.69(17) . . ?
O1 C9 Th1 63.90(18) . . ?
C3 C9 Th1 173.8(3) . . ?
C7 N1 C1 118.7(2) . 11_564 ?
C7 N1 C1 118.7(2) . . ?
C1 N1 C1 122.5(4) 11_564 . ?
C6 C2 C1 120.2(3) . . ?
C2 C6 C3 121.1(3) . . ?
C1 C5 C4 120.8(4) . . ?
C8 C7 C8 119.2(5) . 11_564 ?
C8 C7 N1 120.4(2) . . ?
C8 C7 N1 120.4(2) 11_564 . ?
C5 C4 C3 120.7(4) . . ?
C10 C8 C7 120.8(4) . . ?
C9 O2 Th1 98.3(2) . . ?
C10 C11 C10 119.1(4) 11_564 . ?
C10 C11 C12 120.4(2) 11_564 . ?
C10 C11 C12 120.4(2) . . ?
C8 C10 C11 120.1(4) . . ?
O3 C12 O3 124.9(4) 11_564 . ?
O3 C12 C11 117.56(19) 11_564 . ?
O3 C12 C11 117.6(2) . . ?
C12 O3 Th1 143.07(18) . 19_665 ?

_refine_diff_density_max         1.468
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.076



####################################################################### 
# 
# 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_compound2
_database_code_depnum_ccdc_archive 'CCDC 1432698'
_audit_update_record             
;
2015-11-25 deposited with the CCDC.
2015-12-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            "1,3,5-tri(4'-carboxylphenyl) benzoic thorium"
_chemical_melting_point          N/A
_chemical_formula_moiety         Th(C27H15O6)Cl3(C7H11N2)2
_chemical_formula_sum            'C41 H37 Cl3 N4 O6 Th'
_chemical_formula_weight         1020.13

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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   17.273(2)
_cell_length_b                   15.263(2)
_cell_length_c                   17.298(2)
_cell_angle_alpha                90
_cell_angle_beta                 118.669(3)
_cell_angle_gamma                90
_cell_volume                     4001.3(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9392
_cell_measurement_theta_min      2.310
_cell_measurement_theta_max      27.561

_exptl_crystal_description       bulk
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_F_000             2000
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    3.979
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'BRUKER apex II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_detector_area_resol_mean 0
_diffrn_reflns_number            52294
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.310
_diffrn_reflns_theta_max         27.561
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9392
_reflns_number_gt                6629
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0555P)²+40.2687P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9392
_refine_ls_number_parameters     482
_refine_ls_number_restraints     415
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0610
_refine_ls_wR_factor_ref         0.1480
_refine_ls_wR_factor_gt          0.1320
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.006
_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 0.71782(2) 1.08494(3) 0.77262(2) 0.03479(12) Uani 1 1 d . U . . .
C7 C 0.3873(5) 1.0757(7) 0.5394(5) 0.0302(19) Uani 1 1 d . U . . .
H7A H 0.4195 1.0457 0.5158 0.036 Uiso 1 1 calc R U . . .
C6 C 0.2958(5) 1.0744(7) 0.4949(6) 0.031(2) Uani 1 1 d . U . . .
H6A H 0.2656 1.0425 0.4414 0.037 Uiso 1 1 calc R U . . .
C5 C 0.2472(5) 1.1200(6) 0.5284(5) 0.0266(18) Uani 1 1 d . U . . .
C4 C 0.2929(5) 1.1664(7) 0.6064(6) 0.031(2) Uani 1 1 d . U . . .
H4A H 0.2610 1.1986 0.6289 0.038 Uiso 1 1 calc R U . . .
C3 C 0.3844(5) 1.1666(7) 0.6521(6) 0.034(2) Uani 1 1 d . U . . .
H3A H 0.4146 1.1976 0.7061 0.041 Uiso 1 1 calc R U . . .
C8 C 0.1493(5) 1.1167(6) 0.4798(5) 0.0271(19) Uani 1 1 d . U . . .
C1 C 0.5308(5) 1.1155(7) 0.6704(5) 0.0297(19) Uani 1 1 d . U . . .
C2 C 0.4322(5) 1.1212(7) 0.6187(5) 0.0291(19) Uani 1 1 d . U . . .
C10 C 0.0119(5) 1.1128(6) 0.3418(5) 0.0251(18) Uani 1 1 d . U . . .
C14 C -0.0365(5) 1.1108(6) 0.2437(5) 0.0262(18) Uani 1 1 d . U . . .
Cl3 Cl 0.73717(19) 1.2663(2) 0.7683(2) 0.0642(9) Uani 1 1 d . U . . .
Cl1 Cl 0.7517(3) 0.9200(3) 0.7355(3) 0.0932(12) Uani 1 1 d . . . . .
Cl2 Cl 0.63657(19) 0.9707(4) 0.8416(2) 0.0990(16) Uani 1 1 d . U . . .
O1 O 0.5716(3) 1.0671(5) 0.6426(4) 0.0377(16) Uani 1 1 d . U . . .
O2 O 0.5719(4) 1.1560(5) 0.7418(4) 0.0479(19) Uani 1 1 d . U . . .
C12 C 0.0081(5) 1.1198(6) 0.4815(5) 0.0200(16) Uani 1 1 d . U . . .
C19 C -0.1162(5) 1.1562(6) 0.1985(5) 0.0261(18) Uani 1 1 d . U . . .
H19A H -0.1384 1.1895 0.2299 0.031 Uiso 1 1 calc R U . . .
C17 C -0.1317(5) 1.1042(5) 0.0603(5) 0.0234(17) Uani 1 1 d . U . . .
C21 C -0.0421(5) 1.1221(6) 0.5307(5) 0.0195(16) Uani 1 1 d . U . . .
C16 C -0.0521(6) 1.0592(7) 0.1056(5) 0.034(2) Uani 1 1 d . U . . .
H16A H -0.0304 1.0255 0.0739 0.040 Uiso 1 1 calc R U . . .
C13 C 0.1009(5) 1.1208(6) 0.5249(5) 0.0204(16) Uani 1 1 d . U . . .
H13A H 0.1318 1.1245 0.5874 0.024 Uiso 1 1 calc R U . . .
C15 C -0.0048(5) 1.0635(7) 0.1962(5) 0.032(2) Uani 1 1 d . U . . .
H15A H 0.0501 1.0338 0.2264 0.039 Uiso 1 1 calc R U . . .
N3 N 0.5641(7) 0.3475(9) 0.8575(9) 0.085(3) Uani 1 1 d . U . . .
C11 C -0.0343(5) 1.1165(6) 0.3895(5) 0.0253(18) Uani 1 1 d . U . . .
H11A H -0.0970 1.1168 0.3582 0.030 Uiso 1 1 calc R U . . .
C18 C -0.1621(5) 1.1522(6) 0.1077(5) 0.0298(19) Uani 1 1 d . U . . .
H18A H -0.2162 1.1833 0.0771 0.036 Uiso 1 1 calc R U . . .
C9 C 0.1053(5) 1.1120(6) 0.3881(5) 0.0258(19) Uani 1 1 d . U . . .
H9A H 0.1378 1.1082 0.3568 0.031 Uiso 1 1 calc R U . . .
N1 N 0.8960(7) 0.6552(7) 0.5259(9) 0.068(3) Uani 1 1 d . U . . .
N2 N 0.7939(7) 0.6577(8) 0.5623(8) 0.072(3) Uani 1 1 d . U . . .
C29 C 0.8723(8) 0.6785(9) 0.6363(11) 0.069(3) Uani 1 1 d . U . . .
H29A H 0.8806 0.6922 0.6933 0.083 Uiso 1 1 calc R U . . .
C28 C 0.9340(9) 0.6752(9) 0.6108(12) 0.076(4) Uani 1 1 d . U . . .
H28A H 0.9952 0.6856 0.6476 0.091 Uiso 1 1 calc R U . . .
C36 C 0.4993(10) 0.3642(13) 0.8789(14) 0.102(5) Uani 1 1 d . U . . .
H36A H 0.4603 0.4129 0.8590 0.123 Uiso 1 1 calc R U . . .
C38 C 0.6000(7) 0.2731(9) 0.8906(10) 0.079(3) Uani 1 1 d . U . . .
H38A H 0.6443 0.2449 0.8820 0.095 Uiso 1 1 calc R U . . .
N4 N 0.5636(8) 0.2409(9) 0.9410(11) 0.109(4) Uani 1 1 d D U . . .
C35 C 0.5960(14) 0.4073(14) 0.8096(15) 0.124(6) Uani 1 1 d . U . . .
H35A H 0.5589 0.4599 0.7902 0.187 Uiso 1 1 calc R U . . .
H35B H 0.6573 0.4242 0.8492 0.187 Uiso 1 1 calc R U . . .
H35C H 0.5926 0.3769 0.7582 0.187 Uiso 1 1 calc R U . . .
C30 C 0.8132(9) 0.6421(9) 0.4960(11) 0.068(3) Uani 1 1 d . U . . .
H30A H 0.7724 0.6245 0.4377 0.082 Uiso 1 1 calc R U . . .
C31 C 0.7091(10) 0.6463(15) 0.5591(12) 0.105(5) Uani 1 1 d . U . . .
H31A H 0.6636 0.6327 0.4980 0.126 Uiso 1 1 calc R U . . .
H31B H 0.6920 0.7012 0.5773 0.126 Uiso 1 1 calc R U . . .
C37 C 0.4994(11) 0.3017(14) 0.9318(16) 0.121(6) Uani 1 1 d . U . . .
H37A H 0.4627 0.2987 0.9586 0.146 Uiso 1 1 calc R U . . .
C20 C -0.1810(5) 1.1017(6) -0.0374(5) 0.030(2) Uani 1 1 d . U . . .
C22 C -0.1330(5) 1.1327(7) 0.4884(6) 0.036(2) Uani 1 1 d . U . . .
H22A H -0.1636 1.1427 0.4267 0.043 Uiso 1 1 calc R U . . .
C26 C -0.0005(6) 1.1106(8) 0.6218(6) 0.049(3) Uani 1 1 d . U . . .
H26A H 0.0618 1.1035 0.6533 0.059 Uiso 1 1 calc R U . . .
C23 C -0.1802(5) 1.1289(7) 0.5349(5) 0.031(2) Uani 1 1 d . U . . .
H23A H -0.2427 1.1342 0.5039 0.037 Uiso 1 1 calc R U . . .
C24 C -0.1385(5) 1.1178(6) 0.6239(5) 0.0233(17) Uani 1 1 d . U . . .
C27 C -0.1892(5) 1.1115(5) 0.6732(5) 0.0187(15) Uani 1 1 d . U . . .
C25 C -0.0473(6) 1.1094(9) 0.6669(6) 0.054(3) Uani 1 1 d . U . . .
H25A H -0.0168 1.1027 0.7291 0.064 Uiso 1 1 calc R U . . .
O5 O -0.2711(3) 1.1145(4) 0.6345(4) 0.0282(14) Uani 1 1 d . U . . .
O6 O -0.1462(4) 1.1048(6) 0.7580(4) 0.050(2) Uani 1 1 d . U . . .
O3 O -0.1535(4) 1.0561(4) -0.0800(4) 0.0317(15) Uani 1 1 d . U . . .
O4 O -0.2519(5) 1.1440(6) -0.0783(4) 0.061(2) Uani 1 1 d . U . . .
C34 C 0.9450(12) 0.6473(11) 0.4767(14) 0.103(5) Uani 1 1 d . U . . .
H34A H 0.9042 0.6321 0.4153 0.154 Uiso 1 1 calc R U . . .
H34B H 0.9740 0.7031 0.4787 0.154 Uiso 1 1 calc R U . . .
H34C H 0.9897 0.6012 0.5032 0.154 Uiso 1 1 calc R U . . .
C32 C 0.7144(14) 0.5721(18) 0.6201(15) 0.134(7) Uani 1 1 d . U . . .
H32A H 0.7287 0.5152 0.6083 0.161 Uiso 1 1 calc R U . . .
C33 C 0.7020(17) 0.580(2) 0.6816(17) 0.183(11) Uani 1 1 d . U . . .
H33A H 0.6876 0.6363 0.6953 0.219 Uiso 1 1 calc R U . . .
H33B H 0.7064 0.5312 0.7171 0.219 Uiso 1 1 calc R U . . .
C39 C 0.5906(14) 0.1712(13) 1.0086(13) 0.126(7) Uiso 1 1 d D . . . .
H39A H 0.6225 0.2018 1.0659 0.152 Uiso 1 1 calc R U . . .
H39B H 0.6355 0.1364 1.0022 0.152 Uiso 1 1 calc R U . . .
C40 C 0.5318(19) 0.1041(19) 1.021(2) 0.230(16) Uiso 1 1 d D . . . .
H40A H 0.5024 0.0563 0.9828 0.276 Uiso 1 1 calc R U . . .
C41 C 0.529(3) 0.122(3) 1.087(2) 0.28(2) Uiso 1 1 d D . . . .
H41A H 0.5606 0.1710 1.1208 0.337 Uiso 1 1 calc R U . . .
H41B H 0.4952 0.0868 1.1048 0.337 Uiso 1 1 calc R 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 2.462(5) . ?
Th1 O3 2.490(5) 1_656 ?
Th1 O6 2.499(6) 1_655 ?
Th1 O5 2.527(6) 1_655 ?
Th1 O4 2.539(7) 1_656 ?
Th1 O2 2.554(6) . ?
Th1 Cl1 2.730(5) . ?
Th1 Cl3 2.794(4) . ?
Th1 Cl2 2.835(3) . ?
Th1 C27 2.889(8) 1_655 ?
Th1 C1 2.881(8) . ?
Th1 C20 2.900(8) 1_656 ?
C7 C6 1.387(10) . ?
C7 C2 1.394(12) . ?
C6 C5 1.411(12) . ?
C5 C4 1.386(12) . ?
C5 C8 1.486(10) . ?
C4 C3 1.388(11) . ?
C3 C2 1.397(12) . ?
C8 C9 1.394(11) . ?
C8 C13 1.390(11) . ?
C1 O2 1.254(10) . ?
C1 O1 1.264(11) . ?
C1 C2 1.499(10) . ?
C10 C9 1.416(10) . ?
C10 C11 1.397(11) . ?
C10 C14 1.489(11) . ?
C14 C15 1.390(12) . ?
C14 C19 1.397(11) . ?
C12 C11 1.398(11) . ?
C12 C13 1.407(10) . ?
C12 C21 1.479(10) . ?
C19 C18 1.379(11) . ?
C17 C18 1.378(12) . ?
C17 C16 1.394(11) . ?
C17 C20 1.483(11) . ?
C21 C26 1.394(11) . ?
C21 C22 1.387(11) . ?
C16 C15 1.377(12) . ?
N3 C38 1.288(19) . ?
N3 C36 1.36(2) . ?
N3 C35 1.50(2) . ?
N1 C28 1.325(19) . ?
N1 C30 1.283(16) . ?
N1 C34 1.465(19) . ?
N2 C30 1.360(18) . ?
N2 C29 1.381(18) . ?
N2 C31 1.450(17) . ?
C29 C28 1.335(18) . ?
C36 C37 1.32(3) . ?
C38 N4 1.39(2) . ?
N4 C37 1.395(19) . ?
N4 C39 1.480(2) . ?
C31 C32 1.52(3) . ?
C20 O4 1.261(10) . ?
C20 O3 1.259(10) . ?
C20 Th1 2.900(8) 1_454 ?
C22 C23 1.394(11) . ?
C26 C25 1.367(12) . ?
C23 C24 1.362(12) . ?
C24 C25 1.387(12) . ?
C24 C27 1.491(11) . ?
C27 O5 1.241(9) . ?
C27 O6 1.292(10) . ?
C27 Th1 2.889(8) 1_455 ?
O5 Th1 2.527(6) 1_455 ?
O6 Th1 2.499(6) 1_455 ?
O3 Th1 2.489(5) 1_454 ?
O4 Th1 2.539(7) 1_454 ?
C32 C33 1.19(3) . ?
C39 C40 1.530(2) . ?
C40 C41 1.190(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 O3 159.5(2) . 1_656 ?
O1 Th1 O6 121.55(19) . 1_655 ?
O3 Th1 O6 72.8(2) 1_656 1_655 ?
O1 Th1 O5 70.50(19) . 1_655 ?
O3 Th1 O5 124.36(18) 1_656 1_655 ?
O6 Th1 O5 51.78(18) 1_655 1_655 ?
O1 Th1 O4 126.0(2) . 1_656 ?
O3 Th1 O4 51.30(19) 1_656 1_656 ?
O6 Th1 O4 108.3(3) 1_655 1_656 ?
O5 Th1 O4 145.6(3) 1_655 1_656 ?
O1 Th1 O2 51.6(2) . . ?
O3 Th1 O2 126.5(2) 1_656 . ?
O6 Th1 O2 144.0(3) 1_655 . ?
O5 Th1 O2 104.0(2) 1_655 . ?
O4 Th1 O2 76.3(2) 1_656 . ?
O1 Th1 Cl1 85.68(19) . . ?
O3 Th1 Cl1 83.77(17) 1_656 . ?
O6 Th1 Cl1 76.7(2) 1_655 . ?
O5 Th1 Cl1 79.62(17) 1_655 . ?
O4 Th1 Cl1 127.1(2) 1_656 . ?
O2 Th1 Cl1 130.10(19) . . ?
O1 Th1 Cl3 99.73(19) . . ?
O3 Th1 Cl3 98.20(17) 1_656 . ?
O6 Th1 Cl3 75.3(2) 1_655 . ?
O5 Th1 Cl3 74.56(15) 1_655 . ?
O4 Th1 Cl3 72.9(2) 1_656 . ?
O2 Th1 Cl3 72.08(19) . . ?
Cl1 Th1 Cl3 149.94(10) . . ?
O1 Th1 Cl2 79.52(16) . . ?
O3 Th1 Cl2 80.76(16) 1_656 . ?
O6 Th1 Cl2 142.8(2) 1_655 . ?
O5 Th1 Cl2 141.70(16) 1_655 . ?
O4 Th1 Cl2 72.1(2) 1_656 . ?
O2 Th1 Cl2 73.2(2) . . ?
Cl1 Th1 Cl2 74.78(14) . . ?
Cl3 Th1 Cl2 135.25(12) . . ?
O1 Th1 C27 95.2(2) . 1_655 ?
O3 Th1 C27 99.0(2) 1_656 1_655 ?
O6 Th1 C27 26.5(2) 1_655 1_655 ?
O5 Th1 C27 25.38(19) 1_655 1_655 ?
O4 Th1 C27 130.7(3) 1_656 1_655 ?
O2 Th1 C27 126.2(2) . 1_655 ?
Cl1 Th1 C27 75.30(17) . 1_655 ?
Cl3 Th1 C27 74.77(16) . 1_655 ?
Cl2 Th1 C27 149.92(19) . 1_655 ?
O1 Th1 C1 25.9(2) . . ?
O3 Th1 C1 147.6(2) 1_656 . ?
O6 Th1 C1 138.6(2) 1_655 . ?
O5 Th1 C1 87.8(2) 1_655 . ?
O4 Th1 C1 100.9(2) 1_656 . ?
O2 Th1 C1 25.8(2) . . ?
Cl1 Th1 C1 108.0(2) . . ?
Cl3 Th1 C1 86.3(2) . . ?
Cl2 Th1 C1 73.89(19) . . ?
C27 Th1 C1 113.0(2) 1_655 . ?
O1 Th1 C20 147.3(2) . 1_656 ?
O3 Th1 C20 25.6(2) 1_656 1_656 ?
O6 Th1 C20 91.1(2) 1_655 1_656 ?
O5 Th1 C20 141.0(2) 1_655 1_656 ?
O4 Th1 C20 25.7(2) 1_656 1_656 ?
O2 Th1 C20 101.4(2) . 1_656 ?
Cl1 Th1 C20 105.5(2) . 1_656 ?
Cl3 Th1 C20 85.9(2) . 1_656 ?
Cl2 Th1 C20 74.2(2) . 1_656 ?
C27 Th1 C20 117.2(2) 1_655 1_656 ?
C1 Th1 C20 124.8(2) . 1_656 ?
C6 C7 C2 120.0(8) . . ?
C7 C6 C5 120.6(8) . . ?
C4 C5 C6 118.6(7) . . ?
C4 C5 C8 122.0(8) . . ?
C6 C5 C8 119.4(8) . . ?
C3 C4 C5 121.0(9) . . ?
C4 C3 C2 120.1(8) . . ?
C9 C8 C13 119.6(7) . . ?
C9 C8 C5 119.8(7) . . ?
C13 C8 C5 120.6(7) . . ?
O2 C1 O1 120.5(7) . . ?
O2 C1 C2 120.2(8) . . ?
O1 C1 C2 119.2(8) . . ?
O2 C1 Th1 62.4(4) . . ?
O1 C1 Th1 58.2(4) . . ?
C2 C1 Th1 173.8(7) . . ?
C3 C2 C7 119.6(7) . . ?
C3 C2 C1 120.7(8) . . ?
C7 C2 C1 119.6(8) . . ?
C9 C10 C11 119.0(7) . . ?
C9 C10 C14 120.6(7) . . ?
C11 C10 C14 120.4(7) . . ?
C15 C14 C19 119.2(8) . . ?
C15 C14 C10 121.3(7) . . ?
C19 C14 C10 119.5(8) . . ?
C1 O1 Th1 95.9(5) . . ?
C1 O2 Th1 91.8(5) . . ?
C11 C12 C13 116.7(7) . . ?
C11 C12 C21 121.6(7) . . ?
C13 C12 C21 121.7(7) . . ?
C18 C19 C14 119.4(8) . . ?
C18 C17 C16 118.8(8) . . ?
C18 C17 C20 121.2(7) . . ?
C16 C17 C20 120.0(7) . . ?
C26 C21 C22 116.7(7) . . ?
C26 C21 C12 121.4(7) . . ?
C22 C21 C12 121.8(7) . . ?
C15 C16 C17 120.2(8) . . ?
C8 C13 C12 122.5(7) . . ?
C16 C15 C14 120.7(8) . . ?
C38 N3 C36 109.0(17) . . ?
C38 N3 C35 123.7(13) . . ?
C36 N3 C35 127.1(15) . . ?
C12 C11 C10 122.5(7) . . ?
C17 C18 C19 121.7(8) . . ?
C8 C9 C10 119.6(7) . . ?
C28 N1 C30 110.2(13) . . ?
C28 N1 C34 123.1(13) . . ?
C30 N1 C34 126.7(15) . . ?
C30 N2 C29 107.1(11) . . ?
C30 N2 C31 126.7(13) . . ?
C29 N2 C31 125.9(13) . . ?
C28 C29 N2 105.5(14) . . ?
N1 C28 C29 109.1(14) . . ?
C37 C36 N3 109.0(16) . . ?
N3 C38 N4 109.1(12) . . ?
C38 N4 C37 105.5(16) . . ?
C38 N4 C39 133.3(13) . . ?
C37 N4 C39 120.0(18) . . ?
N1 C30 N2 108.0(14) . . ?
N2 C31 C32 109.8(15) . . ?
C36 C37 N4 107.2(17) . . ?
O4 C20 O3 119.5(8) . . ?
O4 C20 C17 119.8(8) . . ?
O3 C20 C17 120.6(7) . . ?
O4 C20 Th1 60.9(5) . 1_454 ?
O3 C20 Th1 58.7(4) . 1_454 ?
C17 C20 Th1 176.0(7) . 1_454 ?
C23 C22 C21 121.2(8) . . ?
C25 C26 C21 121.4(8) . . ?
C24 C23 C22 121.2(8) . . ?
C23 C24 C25 117.8(8) . . ?
C23 C24 C27 121.1(7) . . ?
C25 C24 C27 121.0(8) . . ?
O5 C27 O6 120.1(7) . . ?
O5 C27 C24 121.3(7) . . ?
O6 C27 C24 118.6(7) . . ?
O5 C27 Th1 60.8(4) . 1_455 ?
O6 C27 Th1 59.6(4) . 1_455 ?
C24 C27 Th1 175.3(5) . 1_455 ?
C26 C25 C24 121.6(9) . . ?
C27 O5 Th1 93.9(5) . 1_455 ?
C27 O6 Th1 93.9(5) . 1_455 ?
C20 O3 Th1 95.7(5) . 1_454 ?
C20 O4 Th1 93.4(5) . 1_454 ?
C33 C32 C31 124(3) . . ?
N4 C39 C40 128(2) . . ?
C41 C40 C39 108(3) . . ?

_refine_diff_density_max         3.357
_refine_diff_density_min         -2.356
_refine_diff_density_rms         0.193



