A porous and photoactive Ti-MOF based on a novel tetranuclear [Ti<sub>2</sub>Tb<sub>2</sub>] cluster.
Yao, Qingxia; Pan, Xuze; Si, Xuezhen; Wang, Xin; Zhang, Xiaoying; Hou, Jinle; Su, Jie; Qiu, Yi; Li, Jun; Chemical communications (Cambridge, England) 60 (2024) 2188–2191; doi:10.1039/d3cc06114k

data_7132789
_publ_section_title
;
 A porous and photoactive Ti-MOF based on a novel tetranuclear
 [Ti<sub>2</sub>Tb<sub>2</sub>] cluster.
;
_journal_issue                   16
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2188
_journal_page_last               2191
_journal_paper_doi               10.1039/d3cc06114k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C41.5 H45.5 N6.5 O18 Tb Ti'
_chemical_formula_sum            'C41.5 H45.5 N6.5 O18 Tb Ti'
_chemical_formula_weight         1130.13
_space_group_crystal_system      cubic
_space_group_IT_number           223
_space_group_name_Hall           '-P 4n 2 3'
_space_group_name_H-M_alt        'P m -3 n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2024-01-19 deposited with the CCDC.	2024-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   25.9298(2)
_cell_length_b                   25.9298(2)
_cell_length_c                   25.9298(2)
_cell_measurement_reflns_used    4215
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      54.0920
_cell_measurement_theta_min      2.9780
_cell_volume                     17434.0(2)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14119
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.015
_diffrn_reflns_theta_max         25.015
_diffrn_reflns_theta_min         1.571
_exptl_absorpt_coefficient_mu    1.388
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38904
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             5304
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.715
_refine_diff_density_min         -1.318
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.250
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2682
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.307
_refine_ls_R_factor_all          0.1375
_refine_ls_R_factor_gt           0.1114
_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/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3084
_refine_ls_wR_factor_ref         0.3339
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1766
_reflns_number_total             2682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc06114k2.cif
_cod_data_source_block           3_sq_sq
_cod_original_cell_volume        17434.0(4)
_cod_database_code               7132789
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.934
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1A-C2 = C8-C5
 1.5 with sigma of 0.005
 C8-N1 = C8-N1_$1
 1.39 with sigma of 0.005
 C8-C8_$2 = N1-N1_$1
 2.4 with sigma of 0.04
 C9-O5A = C9-O5B
 1.27 with sigma of 0.01
 C9-C10
 1.5 with sigma of 0.01
 Tb1A-O5A = Tb1B-O5B
 2.5 with sigma of 0.005
 Tb1B-O4B = Tb1A-O4A
 2.38 with sigma of 0.005
 O1A-Ti1A = O2B-Ti1B = O3A-Ti1A = O3B-Ti1B
 2 with sigma of 0.02
 Ti1A-O3A = Ti1B-O3B = Ti1A-O1A = Ti1B-O2B
 2 with sigma of 0.003
 O2B-C1B = C1B-O1B
 1.3 with sigma of 0.02
3. Restrained planarity
 O1A, O2A, C1A, C2
 with sigma of 0.1
 N1, N1_$1, C5, C8, C8_$2
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O5A \\sim C9 \\sim C10: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(O2A) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1A) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq,
Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim
Ueq, Uanis(O3A) \\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(O5A) \\sim Ueq: with
sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O1A) = Uanis(O1B) = Uanis(O6B) = Uanis(O6A) = Uanis(O2A) = Uanis(O2B)
Uanis(O3A) = Uanis(O3B) = Uanis(O4B) = Uanis(O4A)
Uanis(C1A) = Uanis(C1B) = Uanis(C2)
Uanis(O5A) = Uanis(O5B)
Uanis(C9) = Uanis(C10)
5. Others
 Sof(O1B)=Sof(O2B)=Sof(C1B)=1-FVAR(1)
 Sof(O5B)=0.5*(1-FVAR(2))
 Sof(Tb1B)=Sof(Ti1B)=Sof(O3B)=Sof(O4B)=Sof(O6B)=0.25*(1-FVAR(2))
 Sof(Tb1A)=Sof(Ti1A)=Sof(O3A)=Sof(O4A)=Sof(O6A)=0.25*FVAR(2)
 Sof(O5A)=0.5*FVAR(2)
 Sof(O1A)=Sof(O2A)=Sof(C1A)=FVAR(1)
 U11(C1A)=U11(C1B)=U11(C2)=0.5*FVAR(3)
 U22(C1A)=U22(C1B)=U22(C2)=0.5*FVAR(4)
 U33(C1A)=U33(C1B)=U33(C2)=0.5*FVAR(5)
 Fixed Sof: H10B(0.25) H10C(0.25) H10A(0.25)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7)
6.b Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7)
6.c Idealised Me refined with riding coordinates:
 C10(H10B,H10C,H10A)
;
_shelx_res_checksum              94527
_shelx_fab_checksum              46519
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'