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_7708868
_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 Eu N2 O7, C4 H9 N O'
_chemical_formula_sum            'C29 H30 Eu N3 O8'
_chemical_formula_weight         700.52
_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                112.081(3)
_cell_angle_beta                 92.335(3)
_cell_angle_gamma                107.726(3)
_cell_formula_units_Z            2
_cell_length_a                   8.9015(4)
_cell_length_b                   13.3596(5)
_cell_length_c                   13.7307(5)
_cell_measurement_reflns_used    10533
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.9210
_cell_measurement_theta_min      2.3730
_cell_volume                     1418.81(11)
_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(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.839
_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     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.839
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7466
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.847
_diffrn_reflns_theta_min         2.440
_exptl_absorpt_coefficient_mu    2.265
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59039
_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    1.640
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.499
_refine_diff_density_min         -1.348
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         7466
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0323P)^2^+4.8064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6672
_reflns_number_total             7466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03188k2.cif
_cod_data_source_block           1-Eu_tw
_cod_original_cell_volume        1418.81(10)
_cod_database_code               7708868
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8310(18)
 0.1690(18)
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
 Eu1-O7A \\sim Eu1-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              4481
_olex2_submission_special_instructions 'No special instructions were received'