A dual-functional 3D cerium MOF heterogeneous catalyst for catalysing Knoevenagel condensation and cyanosilylation
Zhao, Peiran; Liu, Yuqian; He, Cheng; Duan, Chunying; New Journal of Chemistry 47 (2023) 19114–19121; doi:10.1039/D3NJ02630B

data_7062786
_publ_section_title
;
 A dual-functional 3D cerium MOF heterogeneous catalyst for catalysing
 Knoevenagel condensation and cyanosilylation
;
_journal_issue                   41
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19114
_journal_page_last               19121
_journal_paper_doi               10.1039/D3NJ02630B
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C16 H10 N O9 Tb, 3[H2O]'
_chemical_formula_sum            'C16 H16 N O12 Tb'
_chemical_formula_weight         573.229
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_symmetry_Int_Tables_number      52
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-20
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-09-28 deposited with the CCDC.	2023-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9732(6)
_cell_length_b                   13.3957(8)
_cell_length_c                   14.6655(9)
_cell_measurement_reflns_used    5736
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.66
_cell_volume                     1762.83(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.00
_diffrn_measured_fraction_theta_full 0.9853
_diffrn_measured_fraction_theta_max 0.9853
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_Laue_measured_fraction_full 0.9853
_diffrn_reflns_Laue_measured_fraction_max 0.9853
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15940
_diffrn_reflns_point_group_measured_fraction_full 0.9853
_diffrn_reflns_point_group_measured_fraction_max 0.9853
_diffrn_reflns_theta_full        24.9934
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.90
_exptl_absorpt_coefficient_mu    4.085
_exptl_absorpt_correction_T_max  0.3334
_exptl_absorpt_correction_T_min  0.2587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.156
_exptl_crystal_description       block
_exptl_crystal_F_000             1117.031
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.2613
_refine_diff_density_min         -1.2759
_refine_diff_density_rms         0.2860
_refine_ls_d_res_high            0.8411
_refine_ls_d_res_low             5.2278
_refine_ls_goodness_of_fit_ref   1.0523
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    11
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0523
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+27.2211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0799
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              0
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                1184
_reflns_number_total             1537
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3nj02630b2.cif
_cod_data_source_block           TB
_cod_depositor_comments
'Adding full bibliography for 7062785--7062786.cif.'
_cod_original_formula_sum        'C16 H16 N1 O12 Tb1'
_cod_database_code               7062786
_exptl_absorpt_special_details
;
 SADABS 2016/2 was used for absorption correction.
 R(int) was  0.0355 after correction. The Ratio of minimum to maximum transmission is 0.2587 and 0.3334. 
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H00a(0.5) H00b(0.5)
3.a Rotating group:
 O006(H00a,H00b)
3.b Aromatic/amide H refined with riding coordinates:
 N005(H005), C00A(H00c), C00B(H00d), C00C(H00e)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 120 electrons were 
found in a volume of 348\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 3[H2O] per Formula Unit 
which account for 120 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'