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_7062785
_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 Ce N O9, 3[H2O]'
_chemical_formula_sum            'C16 H16 Ce N O12'
_chemical_formula_weight         554.42
_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
_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
;
2023-09-26 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                   8.9711(17)
_cell_length_b                   13.666(3)
_cell_length_c                   14.756(3)
_cell_measurement_reflns_used    6070
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.05
_cell_volume                     1809.1(6)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      210.00
_diffrn_measured_fraction_theta_full 0.9931
_diffrn_measured_fraction_theta_max 0.9931
_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  0.0263
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.9931
_diffrn_reflns_Laue_measured_fraction_max 0.9931
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13550
_diffrn_reflns_point_group_measured_fraction_full 0.9931
_diffrn_reflns_point_group_measured_fraction_max 0.9931
_diffrn_reflns_theta_full        24.9951
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.99
_exptl_absorpt_coefficient_mu    2.588
_exptl_absorpt_correction_T_max  0.5629
_exptl_absorpt_correction_T_min  0.4913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2 was used for absorption correction.
 R(int) was  0.0245 after correction. The Ratio of minimum to maximum transmission is 0.4913 and 0.5629 
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.032
_exptl_crystal_description       block
_exptl_crystal_F_000             1088.689
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.0588
_refine_diff_density_min         -0.5725
_refine_diff_density_rms         0.0916
_refine_ls_d_res_high            0.8410
_refine_ls_d_res_low             5.1008
_refine_ls_goodness_of_fit_ref   1.0642
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    11
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0642
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+3.9530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0697
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              0
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                1409
_reflns_number_total             1588
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3nj02630b2.cif
_cod_data_source_block           Ce_new
_cod_depositor_comments
'Adding full bibliography for 7062785--7062786.cif.'
_cod_original_cell_volume        1809.2(6)
_cod_original_formula_sum        'C16 H16 Ce1 N1 O12'
_cod_database_code               7062785
_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: H1Wa(0.5) H1Wb(0.5) O2W(0.25) H2Wa(0.25) H2Wb(0.25) O3W(0.25)
 H3Wa(0.25) H3Wb(0.25)
 Fixed Uiso: C11(0.07) C12(0.07) C9(0.07)
3.a Riding coordinates:
 O1W(H1Wa,H1Wb)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C5(H5), C7(H7)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 108 electrons were 
found in a volume of 344\%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'