A series of microporous and robust Ln-MOFs showing luminescent properties and catalytic performances towards Knoevenagel reactions
Yao, Qing-Xia; Tian, Miaomiao; Zheng, Jun; Xue, Jintang; Pan, Xuze; Zhou, Dandan; Li, Yun-Wu; Duan, Wen-zeng; Su, Jie; Huang, Xianqiang; Dalton Transactions  (2021) –; doi:10.1039/D1DT03188K

data_7708867
_publ_section_title
;
 A series of microporous and robust Ln-MOFs showing luminescent properties
 and catalytic performances towards Knoevenagel reactions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03188K
_journal_year                    2021
_chemical_formula_moiety         'C25 H21 N2 O7 Tb, C4 H9 N O'
_chemical_formula_sum            'C29 H30 N3 O8 Tb'
_chemical_formula_weight         707.48
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-11-15
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2021-11-15 deposited with the CCDC.	2021-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                112.117(3)
_cell_angle_beta                 92.467(2)
_cell_angle_gamma                107.814(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9166(2)
_cell_length_b                   13.3917(4)
_cell_length_c                   13.7454(5)
_cell_measurement_reflns_used    12113
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.6610
_cell_measurement_theta_min      2.4200
_cell_volume                     1424.16(9)
_computing_cell_refinement
'CrysAlisPro 1.171.39.29a (Rigaku Oxford Diffraction, 2015)'
_computing_data_collection
'CrysAlisPro 1.171.39.29a (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction
'CrysAlisPro 1.171.39.29a (Rigaku Oxford Diffraction, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.842
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7507
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.786
_diffrn_reflns_theta_min         2.439
_exptl_absorpt_coefficient_mu    2.538
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.927
_refine_diff_density_min         -1.532
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         7507
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0374P)^2^+5.5256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6926
_reflns_number_total             7507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03188k2.cif
_cod_data_source_block           1-Tb_tw
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '__diffrn_measurement_device' was replaced with
'_diffrn_measurement_device'.

Automatic conversion script
Id: cif_correct_tags 7550 2019-12-06 10:49:48Z antanas 
;
_cod_original_cell_volume        1424.15(8)
_cod_database_code               7708867
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.778(2)
 0.222(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O7A-C22A = O7B-C22B
 1.2 with sigma of 0.02
 N1B-C1A = N1A-C1B = N1B-C8A = N1A-C8B = N1B-C15A = N1A-C15B
 1.49 with sigma of 0.02
 C22A-N2A = C22B-N2B
 1.27 with sigma of 0.02
 N2A-C24A = N2A-C25A = N2B-C24B = N2B-C25B
 1.5 with sigma of 0.02
 C22A-C23A = C22B-C23B
 1.54 with sigma of 0.02
 C4A-C7 = C4B-C7 = C18A-C21 = C18B-C21
 1.52 with sigma of 0.02
 Tb1-O7A \\sim Tb1-O7B
 with sigma of 0.02
4. Restrained planarity
 O7A, N2A, C22A, C23A, C24A, C25A
 with sigma of 0.1
 O7B, N2B, C22B, C23B, C24B, C25B
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(C24A) \\sim Ueq, Uanis(C25A) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C1A) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C4A)
\\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C1B) \\sim Ueq,
Uanis(C2B) \\sim Ueq, Uanis(C3B) \\sim Ueq, Uanis(C4B) \\sim Ueq, Uanis(C5B)
\\sim Ueq, Uanis(C6B) \\sim Ueq: with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(N1B) = Uanis(N1A)
Uanis(O7A) = Uanis(O7B)
Uanis(N2A) = Uanis(N2B)
Uanis(C22A) = Uanis(C22B)
Uanis(C23A) = Uanis(C23B)
Uanis(C24A) = Uanis(C24B)
Uanis(C25A) = Uanis(C25B) = Uanis(C28)
Uanis(C8A) = Uanis(C8B)
Uanis(C9A) = Uanis(C9B)
Uanis(C10A) = Uanis(C10B)
Uanis(C11A) = Uanis(C11B)
Uanis(C12A) = Uanis(C12B)
Uanis(C13A) = Uanis(C13B)
Uanis(C1A) = Uanis(C1B)
Uanis(C2A) = Uanis(C2B)
Uanis(C3A) = Uanis(C3B)
Uanis(C4A) = Uanis(C4B)
Uanis(C5A) = Uanis(C5B)
Uanis(C6A) = Uanis(C6B)
Uanis(C15A) = Uanis(C15B)
Uanis(C16A) = Uanis(C16B)
Uanis(C17A) = Uanis(C17B)
Uanis(C18A) = Uanis(C18B) = Uanis(C4A)
Uanis(C19A) = Uanis(C19B)
Uanis(C20A) = Uanis(C20B)
6. Others
 Sof(O7B)=Sof(N2B)=Sof(C22B)=Sof(C23B)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24B)=
 Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25B)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(O7A)=Sof(N2A)=Sof(C22A)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24A)=
 Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
 Fixed Sof: N1B(0.5) N1A(0.5) C1A(0.5) C2A(0.5) H2A(0.5) C3A(0.5) H3A(0.5)
 C4A(0.5) C5A(0.5) H5A(0.5) C6A(0.5) H6A(0.5) C1B(0.5) C2B(0.5) H2B(0.5)
 C3B(0.5) H3B(0.5) C4B(0.5) C5B(0.5) H5B(0.5) C6B(0.5) H6B(0.5) C8A(0.5)
 C9A(0.5) H9A(0.5) C10A(0.5) H10A(0.5) C11A(0.5) C12A(0.5) H12A(0.5) C13A(0.5)
 H13A(0.5) C8B(0.5) C9B(0.5) H9B(0.5) C10B(0.5) H10B(0.5) C11B(0.5) C12B(0.5)
 H12B(0.5) C13B(0.5) H13B(0.5) C15A(0.5) C16A(0.5) H16A(0.5) C17A(0.5)
 H17A(0.5) C18A(0.5) C19A(0.5) H19A(0.5) C20A(0.5) H20A(0.5) C15B(0.5)
 C16B(0.5) H16B(0.5) C17B(0.5) H17B(0.5) C18B(0.5) C19B(0.5) H19B(0.5)
 C20B(0.5) H20B(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A), C2B(H2B), C3B(H3B), C5B(H5B),
 C6B(H6B), C9A(H9A), C10A(H10A), C12A(H12A), C13A(H13A), C9B(H9B), C10B(H10B),
 C12B(H12B), C13B(H13B), C16A(H16A), C17A(H17A), C19A(H19A), C20A(H20A),
 C16B(H16B), C17B(H17B), C19B(H19B), C20B(H20B)
7.b Fitted hexagon refined as free rotating group:
 C1A(C2A,C3A,C4A,C5A,C6A), C1B(C2B,C3B,C4B,C5B,C6B), C8A(C9A,C10A,C11A,C12A,
 C13A), C8B(C9B,C10B,C11B,C12B,C13B), C15A(C16A,C17A,C18A,C19A,C20A), C15B(C16B,
 C17B,C18B,C19B,C20B)
7.c Idealised Me refined with riding coordinates:
 C23A(H23A,H23B,H23C), C23B(H23D,H23E,H23F)
7.d Idealised Me refined as rotating group:
 C24A(H24A,H24B,H24C), C24B(H24D,H24E,H24F), C25A(H25A,H25B,H25C), C25B(H25D,
 H25E,H25F), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              90333
_olex2_submission_special_instructions 'No special instructions were received'