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_7708869
_publ_section_title
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 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 Pr, C4 H9 N O'
_chemical_formula_sum            'C29 H30 N3 O8 Pr'
_chemical_formula_weight         689.47
_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
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2021-11-15 deposited with the CCDC.	2021-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                112.080(3)
_cell_angle_beta                 92.371(3)
_cell_angle_gamma                107.734(3)
_cell_formula_units_Z            2
_cell_length_a                   8.9119(3)
_cell_length_b                   13.3816(5)
_cell_length_c                   13.7490(5)
_cell_measurement_reflns_used    9634
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.0130
_cell_measurement_theta_min      2.4150
_cell_volume                     1424.45(10)
_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 0.998
_diffrn_measured_fraction_theta_max 0.850
_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     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_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            7574
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.782
_diffrn_reflns_theta_min         2.438
_exptl_absorpt_coefficient_mu    1.765
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80462
_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            green
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.501
_refine_diff_density_min         -1.423
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         7574
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0385P)^2^+6.9991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1363
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6889
_reflns_number_total             7574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03188k2.cif
_cod_data_source_block           1-Pr_tw
_cod_database_code               7708869
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.789(2)
 0.211(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
 Pr1-O7A \\sim Pr1-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              275
_olex2_submission_special_instructions 'No special instructions were received'