#------------------------------------------------------------------------------
#$Date: 2024-09-06 03:17:17 +0300 (Fri, 06 Sep 2024) $
#$Revision: 294521 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/89/7248921.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_7248921
loop_
_publ_author_name
'Yang, Shun-Yi'
'Zhang, Qian'
'Zhang, Yang-Lu'
'Tan, Tie-Shen'
'Zhu, Junlun'
'Yang, Xiaodong'
'Shi, Le'
'Yang, Jiong'
'Shao, Dong'
_publ_section_title
;
 Highly proton-conducting lanthanide metal--organic frameworks featuring
 highly oxygenated ligands with slow magnetic relaxation or magnetocaloric
 effect
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              4181
_journal_page_last               4189
_journal_paper_doi               10.1039/D4CE00501E
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C12 H12 O12 Tb'
_chemical_formula_sum            'C12 H12 O12 Tb'
_chemical_formula_weight         507.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-01-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-17 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                85.893(5)
_cell_angle_beta                 76.937(5)
_cell_angle_gamma                63.663(5)
_cell_formula_units_Z            2
_cell_length_a                   10.3636(17)
_cell_length_b                   11.0274(16)
_cell_length_c                   11.1750(17)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    304.00
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.67
_cell_volume                     1114.3(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      304.00
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32186
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.537
_diffrn_reflns_theta_min         2.062
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.219
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_correction_T_min  0.240
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       block
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         5091
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0184
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0179P)²+0.5155P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0443
_refine_ls_wR_factor_ref         0.0448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4776
_reflns_number_total             5091
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00501e2.cif
_cod_data_source_block           Tb
_cod_depositor_comments
'Adding full bibliography for 7248921--7248922.cif.'
_cod_database_code               7248921
_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_max   0.661
_shelx_estimated_absorpt_t_min   0.390
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 Tb1-H7A \\sim Tb1-H7B
 with sigma of 0.02
 Tb1-H9A \\sim Tb1-H9B
 with sigma of 0.02
 Tb1-H12A \\sim Tb1-H12B
 with sigma of 0.02
3.a Free rotating group:
 O7(H7A,H7B), O9(H9A,H9B), O12(H12A,H12B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C5(H5A)
3.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O5(H5), O18(H18)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Tb1 Tb 0.53580(2) 0.50509(2) 0.29515(2) 0.01690(4) Uani 1 1 d D . . . .
O1 O 0.4566(2) 0.32745(17) 0.59400(15) 0.0294(4) Uani 1 1 d . . . . .
O2 O 1.0242(3) -0.1645(3) -0.1864(3) 0.0846(11) Uani 1 1 d . . . . .
H2 H 1.106110 -0.229189 -0.201188 0.127 Uiso 1 1 calc R U . . .
O4 O 0.23116(18) 0.59162(18) 0.64414(15) 0.0280(4) Uani 1 1 d . . . . .
O5 O 0.4317(5) -0.0987(3) 0.72616(19) 0.0928(12) Uani 1 1 d . . . . .
H5 H 0.451002 -0.178921 0.720369 0.139 Uiso 1 1 calc R U . . .
O6 O 0.5327(2) 0.30778(18) 0.38984(16) 0.0327(4) Uani 1 1 d . . . . .
O7 O 0.3718(3) 0.7199(2) 0.22891(18) 0.0523(6) Uani 1 1 d G . . . .
H7A H 0.355541 0.736783 0.156928 0.078 Uiso 1 1 d DG U . . .
H7B H 0.302104 0.785972 0.273511 0.078 Uiso 1 1 d DG U . . .
O8 O 0.31891(18) 0.57367(19) 0.44232(16) 0.0308(4) Uani 1 1 d . . . . .
O9 O 0.6813(3) 0.5726(2) 0.13277(19) 0.0492(6) Uani 1 1 d G . . . .
H9A H 0.678714 0.650619 0.121710 0.074 Uiso 1 1 d DG U . . .
H9B H 0.751457 0.522672 0.075816 0.074 Uiso 1 1 d DG U . . .
O10 O 0.70946(18) 0.30960(17) 0.16409(14) 0.0273(4) Uani 1 1 d . . . . .
O12 O 0.4093(2) 0.4626(2) 0.16076(17) 0.0384(5) Uani 1 1 d G . . . .
H12A H 0.460033 0.410118 0.098130 0.058 Uiso 1 1 d DG U . . .
H12B H 0.336387 0.524361 0.135991 0.058 Uiso 1 1 d DG U . . .
O14 O 0.6237(2) 0.2651(2) 0.01656(18) 0.0479(6) Uani 1 1 d . . . . .
C1 C 0.1073(3) 0.5359(3) 0.5187(2) 0.0266(5) Uani 1 1 d . . . . .
C2 C 0.4645(4) 0.0738(3) 0.6062(2) 0.0407(7) Uani 1 1 d . . . . .
H2A H 0.440872 0.123181 0.678534 0.049 Uiso 1 1 calc R U . . .
C3 C 0.8846(3) 0.0284(3) -0.0553(3) 0.0409(7) Uani 1 1 d . . . . .
H3 H 0.806273 0.047163 -0.092393 0.049 Uiso 1 1 calc R U . . .
C4 C 0.4981(3) 0.1276(2) 0.4955(2) 0.0268(5) Uani 1 1 d . . . . .
C5 C 0.1081(3) 0.4995(3) 0.4021(2) 0.0390(7) Uani 1 1 d . . . . .
H5A H 0.181488 0.498635 0.336008 0.047 Uiso 1 1 calc R U . . .
C6 C 0.4952(3) 0.2640(2) 0.4941(2) 0.0241(5) Uani 1 1 d . . . . .
C7 C 0.0017(3) 0.4646(3) 0.3826(2) 0.0387(7) Uani 1 1 d . . . . .
O18 O 0.0091(3) 0.4304(4) 0.26560(18) 0.0802(11) Uani 1 1 d . . . . .
H18 H -0.062290 0.416920 0.264134 0.120 Uiso 1 1 calc R U . . .
C9 C 0.4650(4) -0.0527(3) 0.6125(2) 0.0410(7) Uani 1 1 d . . . . .
C10 C 0.7234(3) 0.2384(2) 0.0737(2) 0.0266(5) Uani 1 1 d . . . . .
C11 C 1.0158(3) -0.0854(3) -0.0936(3) 0.0382(7) Uani 1 1 d . . . . .
C12 C 0.2272(2) 0.5706(2) 0.5347(2) 0.0236(5) Uani 1 1 d . . . . .
C13 C 0.8670(3) 0.1154(2) 0.0371(2) 0.0261(5) Uani 1 1 d . . . . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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 Tb1 O4 72.52(6) 2_666 2_666 ?
O1 Tb1 O6 121.20(6) 2_666 . ?
O1 Tb1 O7 73.06(7) 2_666 . ?
O1 Tb1 O9 82.55(7) 2_666 . ?
O1 Tb1 O10 137.47(6) 2_666 . ?
O1 Tb1 O12 144.57(7) 2_666 . ?
O4 Tb1 O7 137.74(8) 2_666 . ?
O4 Tb1 O10 70.15(5) 2_666 . ?
O6 Tb1 O4 79.53(6) . 2_666 ?
O6 Tb1 O7 140.49(8) . . ?
O6 Tb1 O9 140.46(7) . . ?
O6 Tb1 O10 70.74(6) . . ?
O6 Tb1 O12 83.49(7) . . ?
O7 Tb1 O10 126.19(6) . . ?
O8 Tb1 O1 77.94(6) . 2_666 ?
O8 Tb1 O4 120.07(6) . 2_666 ?
O8 Tb1 O6 73.18(7) . . ?
O8 Tb1 O7 74.93(8) . . ?
O8 Tb1 O9 146.23(7) . . ?
O8 Tb1 O10 139.59(6) . . ?
O8 Tb1 O12 87.00(6) . . ?
O9 Tb1 O4 78.78(8) . 2_666 ?
O9 Tb1 O7 73.13(9) . . ?
O9 Tb1 O10 70.93(7) . . ?
O9 Tb1 O12 93.42(8) . . ?
O12 Tb1 O4 141.36(6) . 2_666 ?
O12 Tb1 O7 72.10(8) . . ?
O12 Tb1 O10 71.53(6) . . ?
C6 O1 Tb1 147.51(15) . 2_666 ?
C11 O2 H2 109.5 . . ?
C12 O4 Tb1 119.38(15) . 2_666 ?
C9 O5 H5 109.5 . . ?
C6 O6 Tb1 141.65(15) . . ?
Tb1 O7 H7A 125.8 . . ?
Tb1 O7 H7B 127.7 . . ?
H7A O7 H7B 104.5 . . ?
C12 O8 Tb1 159.84(18) . . ?
Tb1 O9 H9A 127.8 . . ?
Tb1 O9 H9B 127.6 . . ?
H9A O9 H9B 104.5 . . ?
C10 O10 Tb1 142.98(15) . . ?
Tb1 O12 H12A 118.6 . . ?
Tb1 O12 H12B 123.5 . . ?
H12A O12 H12B 104.5 . . ?
C5 C1 C7 119.1(2) . 2_566 ?
C5 C1 C12 118.8(2) . . ?
C7 C1 C12 122.1(2) 2_566 . ?
C4 C2 H2A 119.3 . . ?
C4 C2 C9 121.5(2) . . ?
C9 C2 H2A 119.3 . . ?
C11 C3 H3 119.2 . . ?
C11 C3 C13 121.6(2) . . ?
C13 C3 H3 119.2 . . ?
C2 C4 C6 119.2(2) . . ?
C2 C4 C9 119.1(2) . 2_656 ?
C9 C4 C6 121.7(2) 2_656 . ?
C1 C5 H5A 119.4 . . ?
C7 C5 C1 121.1(2) . . ?
C7 C5 H5A 119.4 . . ?
O1 C6 O6 124.5(2) . . ?
O1 C6 C4 118.4(2) . . ?
O6 C6 C4 117.2(2) . . ?
C5 C7 C1 119.8(2) . 2_566 ?
O18 C7 C1 122.3(2) . 2_566 ?
O18 C7 C5 117.9(2) . . ?
C7 O18 H18 109.5 . . ?
O5 C9 C2 117.5(2) . . ?
O5 C9 C4 123.0(2) . 2_656 ?
C2 C9 C4 119.5(2) . 2_656 ?
O10 C10 C13 116.9(2) . . ?
O14 C10 O10 123.4(2) . . ?
O14 C10 C13 119.7(2) . . ?
O2 C11 C3 117.7(2) . . ?
O2 C11 C13 122.8(2) . 2_755 ?
C3 C11 C13 119.5(2) . 2_755 ?
O4 C12 C1 117.2(2) . . ?
O8 C12 O4 123.6(2) . . ?
O8 C12 C1 119.2(2) . . ?
C3 C13 C10 119.4(2) . . ?
C3 C13 C11 118.9(2) . 2_755 ?
C11 C13 C10 121.7(2) 2_755 . ?
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
Tb1 O1 2.3349(16) 2_666 ?
Tb1 O4 2.4046(16) 2_666 ?
Tb1 O6 2.3603(16) . ?
Tb1 O7 2.407(2) . ?
Tb1 O8 2.3082(17) . ?
Tb1 O9 2.3842(18) . ?
Tb1 O10 2.4186(16) . ?
Tb1 O12 2.3941(18) . ?
O1 C6 1.248(3) . ?
O2 H2 0.8200 . ?
O2 C11 1.365(3) . ?
O4 C12 1.275(3) . ?
O5 H5 0.8200 . ?
O5 C9 1.362(3) . ?
O6 C6 1.274(3) . ?
O7 H7A 0.8498 . ?
O7 H7B 0.8504 . ?
O8 C12 1.245(3) . ?
O9 H9A 0.8502 . ?
O9 H9B 0.8502 . ?
O10 C10 1.267(3) . ?
O12 H12A 0.8501 . ?
O12 H12B 0.8498 . ?
O14 C10 1.250(3) . ?
C1 C5 1.387(3) . ?
C1 C7 1.391(3) 2_566 ?
C1 C12 1.501(3) . ?
C2 H2A 0.9300 . ?
C2 C4 1.374(3) . ?
C2 C9 1.390(3) . ?
C3 H3 0.9300 . ?
C3 C11 1.381(4) . ?
C3 C13 1.385(3) . ?
C4 C6 1.490(3) . ?
C4 C9 1.392(3) 2_656 ?
C5 H5A 0.9300 . ?
C5 C7 1.381(3) . ?
C7 O18 1.364(3) . ?
O18 H18 0.8200 . ?
C10 C13 1.496(3) . ?
C11 C13 1.395(3) 2_755 ?
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
Tb1 O1 C6 O6 -23.1(5) 2_666 . . . ?
Tb1 O1 C6 C4 156.8(2) 2_666 . . . ?
Tb1 O4 C12 O8 -41.7(3) 2_666 . . . ?
Tb1 O4 C12 C1 136.21(18) 2_666 . . . ?
Tb1 O6 C6 O1 -10.0(4) . . . . ?
Tb1 O6 C6 C4 170.06(19) . . . . ?
Tb1 O8 C12 O4 78.9(5) . . . . ?
Tb1 O8 C12 C1 -99.0(5) . . . . ?
Tb1 O10 C10 O14 3.1(5) . . . . ?
Tb1 O10 C10 C13 -175.96(17) . . . . ?
O10 C10 C13 C3 175.4(3) . . . . ?
O10 C10 C13 C11 -4.5(4) . . . 2_755 ?
O14 C10 C13 C3 -3.7(4) . . . . ?
O14 C10 C13 C11 176.4(3) . . . 2_755 ?
C1 C5 C7 C1 -0.8(5) . . . 2_566 ?
C1 C5 C7 O18 179.8(3) . . . . ?
C2 C4 C6 O1 -2.7(4) . . . . ?
C2 C4 C6 O6 177.3(3) . . . . ?
C4 C2 C9 O5 179.4(3) . . . . ?
C4 C2 C9 C4 0.7(5) . . . 2_656 ?
C5 C1 C12 O4 -173.8(3) . . . . ?
C5 C1 C12 O8 4.2(4) . . . . ?
C7 C1 C5 C7 0.8(5) 2_566 . . . ?
C7 C1 C12 O4 4.3(4) 2_566 . . . ?
C7 C1 C12 O8 -177.7(3) 2_566 . . . ?
C9 C2 C4 C6 179.7(3) . . . . ?
C9 C2 C4 C9 -0.7(5) . . . 2_656 ?
C9 C4 C6 O1 177.8(3) 2_656 . . . ?
C9 C4 C6 O6 -2.3(4) 2_656 . . . ?
C11 C3 C13 C10 179.1(3) . . . . ?
C11 C3 C13 C11 -1.0(5) . . . 2_755 ?
C12 C1 C5 C7 179.0(3) . . . . ?
C13 C3 C11 O2 -179.1(3) . . . . ?
C13 C3 C11 C13 1.0(5) . . . 2_755 ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.458 0.076 -0.221 442.3 125.5 ?
