#------------------------------------------------------------------------------
#$Date: 2021-07-05 19:19:16 +0300 (Mon, 05 Jul 2021) $
#$Revision: 267027 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/83/7128321.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7128321
loop_
_publ_author_name
'Donnarumma, P. Rafael'
'Frojmovic, Sahara'
'Marino, Paola'
'Bicalho, Hudson A.'
'Titi, Hatem M.'
'Howarth, Ashlee J.'
_publ_section_title
;
 Synthetic approaches for accessing rare-earth analogues of UiO-66.
;
_journal_issue                   50
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6121
_journal_page_last               6124
_journal_paper_doi               10.1039/d1cc01552d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_sum            'C24 H12 O16 Tm3'
_chemical_formula_weight         1063.13
_chemical_name_systematic
catena-[bis(m-hydroxo)-bis(m-oxo)-tris(m-terephthalato)-tri-Thulium]
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-03-18 deposited with the CCDC.	2021-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.2553(16)
_cell_length_b                   21.2553(16)
_cell_length_c                   21.2553(16)
_cell_measurement_reflns_used    492
_cell_measurement_temperature    253(2)
_cell_measurement_theta_max      72.435
_cell_measurement_theta_min      3.602
_cell_volume                     9602.9(13)
_computing_cell_refinement       'Bruker APEX3'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker APEX3'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      253(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker AXS D8'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1137
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43503
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.435
_diffrn_reflns_theta_min         3.602
_exptl_absorpt_coefficient_mu    10.408
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             3928
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dimethylacetamide'
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.092
_refine_diff_density_min         -1.084
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     27
_refine_ls_number_reflns         539
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0574P)²+293.7238P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1065
_reflns_Friedel_coverage         0.000
_reflns_number_gt                492
_reflns_number_total             539
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc01552d2.cif
_cod_data_source_block           AH59
_cod_depositor_comments          'Adding full bibliography for 7128321.cif.'
_cod_original_cell_volume        9603(2)
_cod_database_code               7128321
_shelx_shelxl_version_number     2017/1
_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.
;
_shelx_estimated_absorpt_t_min   0.624
_shelx_estimated_absorpt_t_max   0.681
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'
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 . .
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'
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 . ?
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 . ?
