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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AH59
_database_code_depnum_ccdc_archive 'CCDC 2071285'
loop_
_audit_author_name
_audit_author_address
'Hatem Titi'
;McGill University
Canada
;
_audit_update_record             
;
2021-03-18 deposited with the CCDC.	2021-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        
catena-[bis(m-hydroxo)-bis(m-oxo)-tris(m-terephthalato)-tri-Thulium]
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H12 O16 Tm3'
_chemical_formula_weight         1063.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -8.0393 4.1821 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'

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

_cell_length_a                   21.2553(16)
_cell_length_b                   21.2553(16)
_cell_length_c                   21.2553(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9603(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    253(2)
_cell_measurement_reflns_used    492
_cell_measurement_theta_min      3.602
_cell_measurement_theta_max      72.435

_exptl_crystal_description       octahedron
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_F_000             3928
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    10.408
_shelx_estimated_absorpt_T_min   0.624
_shelx_estimated_absorpt_T_max   0.681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5001
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      253(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker AXS D8'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            43503
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_av_R_equivalents  0.1137
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.602
_diffrn_reflns_theta_max         72.435
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             539
_reflns_number_gt                492
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker APEX3'
_computing_data_reduction        'Bruker APEX3'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0574P)²+293.7238P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_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         539
_refine_ls_number_parameters     27
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.1065
_refine_ls_wR_factor_gt          0.0950
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.121
_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
Tm Tm 0.37277(3) 0.500000 0.500000 0.0150(3) Uani 1 8 d S T P . .
O2 O 0.44085(17) 0.55915(17) 0.55915(17) 0.0085(13) Uani 1 6 d S T P . .
O1 O 0.3263(3) 0.4036(2) 0.500000 0.0417(13) Uani 1 2 d S T P . .
C1 C 0.3465(4) 0.3465(4) 0.500000 0.041(3) Uani 1 4 d S T P . .
C2 C 0.2964(4) 0.2964(4) 0.500000 0.046(3) Uani 1 4 d S TU P . .
C3 C 0.3127(6) 0.2336(5) 0.500000 0.075(3) Uani 1 2 d S TU P . .
H3 H 0.355385 0.222006 0.500000 0.091 Uiso 1 2 calc R U 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
Tm O1 2.275(5) . ?
Tm O1 2.275(5) 115 ?
Tm O1 2.275(5) 99_565 ?
Tm O1 2.275(5) 17_556 ?
Tm O2 2.2925(18) . ?
Tm O2 2.2926(18) 99_565 ?
Tm O2 2.2926(18) 98_556 ?
Tm O2 2.2926(18) 4_566 ?
Tm Tm 3.8246(9) 101_666 ?
Tm Tm 3.8246(9) 105_666 ?
Tm Tm 3.8246(9) 5 ?
Tm Tm 3.8246(9) 9 ?
O1 C1 1.287(8) . ?
C1 C2 1.508(16) . ?
C2 C3 1.379(13) . ?
C2 C3 1.379(13) 13_556 ?
C3 C3 1.39(2) 181 ?
C3 H3 0.9400 . ?

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 Tm O1 79.14(12) . 115 ?
O1 Tm O1 128.6(3) . 99_565 ?
O1 Tm O1 79.14(12) 115 99_565 ?
O1 Tm O1 79.14(12) . 17_556 ?
O1 Tm O1 128.6(3) 115 17_556 ?
O1 Tm O1 79.14(12) 99_565 17_556 ?
O1 Tm O2 140.18(8) . . ?
O1 Tm O2 140.18(8) 115 . ?
O1 Tm O2 77.29(17) 99_565 . ?
O1 Tm O2 77.29(17) 17_556 . ?
O1 Tm O2 77.29(17) . 99_565 ?
O1 Tm O2 140.18(8) 115 99_565 ?
O1 Tm O2 140.18(8) 99_565 99_565 ?
O1 Tm O2 77.29(17) 17_556 99_565 ?
O2 Tm O2 66.52(17) . 99_565 ?
O1 Tm O2 140.18(8) . 98_556 ?
O1 Tm O2 77.29(17) 115 98_556 ?
O1 Tm O2 77.29(17) 99_565 98_556 ?
O1 Tm O2 140.18(8) 17_556 98_556 ?
O2 Tm O2 66.52(17) . 98_556 ?
O2 Tm O2 101.7(3) 99_565 98_556 ?
O1 Tm O2 77.29(17) . 4_566 ?
O1 Tm O2 77.29(17) 115 4_566 ?
O1 Tm O2 140.18(8) 99_565 4_566 ?
O1 Tm O2 140.18(8) 17_556 4_566 ?
O2 Tm O2 101.7(3) . 4_566 ?
O2 Tm O2 66.52(17) 99_565 4_566 ?
O2 Tm O2 66.52(17) 98_556 4_566 ?
O1 Tm Tm 160.73(15) . 101_666 ?
O1 Tm Tm 107.87(10) 115 101_666 ?
O1 Tm Tm 70.72(15) 99_565 101_666 ?
O1 Tm Tm 107.87(10) 17_556 101_666 ?
O2 Tm Tm 33.47(7) . 101_666 ?
O2 Tm Tm 86.64(14) 99_565 101_666 ?
O2 Tm Tm 33.47(7) 98_556 101_666 ?
O2 Tm Tm 86.64(14) 4_566 101_666 ?
O1 Tm Tm 107.87(10) . 105_666 ?
O1 Tm Tm 160.72(15) 115 105_666 ?
O1 Tm Tm 107.87(10) 99_565 105_666 ?
O1 Tm Tm 70.72(15) 17_556 105_666 ?
O2 Tm Tm 33.47(7) . 105_666 ?
O2 Tm Tm 33.47(7) 99_565 105_666 ?
O2 Tm Tm 86.64(13) 98_556 105_666 ?
O2 Tm Tm 86.64(13) 4_566 105_666 ?
Tm Tm Tm 60.0 101_666 105_666 ?
O1 Tm Tm 70.72(15) . 5 ?
O1 Tm Tm 107.87(10) 115 5 ?
O1 Tm Tm 160.72(15) 99_565 5 ?
O1 Tm Tm 107.87(10) 17_556 5 ?
O2 Tm Tm 86.64(13) . 5 ?
O2 Tm Tm 33.47(7) 99_565 5 ?
O2 Tm Tm 86.64(13) 98_556 5 ?
O2 Tm Tm 33.47(7) 4_566 5 ?
Tm Tm Tm 90.0 101_666 5 ?
Tm Tm Tm 60.0 105_666 5 ?
O1 Tm Tm 107.87(10) . 9 ?
O1 Tm Tm 70.72(15) 115 9 ?
O1 Tm Tm 107.87(10) 99_565 9 ?
O1 Tm Tm 160.72(15) 17_556 9 ?
O2 Tm Tm 86.64(14) . 9 ?
O2 Tm Tm 86.64(14) 99_565 9 ?
O2 Tm Tm 33.47(7) 98_556 9 ?
O2 Tm Tm 33.47(7) 4_566 9 ?
Tm Tm Tm 60.0 101_666 9 ?
Tm Tm Tm 90.0 105_666 9 ?
Tm Tm Tm 60.0 5 9 ?
Tm O2 Tm 113.06(13) . 105_666 ?
Tm O2 Tm 113.06(13) . 101_666 ?
Tm O2 Tm 113.06(13) 105_666 101_666 ?
C1 O1 Tm 134.8(6) . . ?
O1 C1 O1 129.0(10) 13_556 . ?
O1 C1 C2 115.5(5) 13_556 . ?
O1 C1 C2 115.5(5) . . ?
C3 C2 C3 119.2(14) . 13_556 ?
C3 C2 C1 120.4(7) . . ?
C3 C2 C1 120.4(7) 13_556 . ?
C2 C3 C3 120.4(7) . 181 ?
C2 C3 H3 119.8 . . ?
C3 C3 H3 119.8 181 . ?

_refine_diff_density_max         1.092
_refine_diff_density_min         -1.084
_refine_diff_density_rms         0.165





_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dimethylacetamide'
