Metal–organic frameworks incorporating azobenzene-based ligands as a heterogeneous Lewis-acid catalyst for cyanosilylation of imines
Saeed, Aasim; Zhang, Xiao-Yu; Huang, Zi-Qing; Zhao, Xin-Yang; Xu, Lei; Zhao, Yue; Sun, Wei-Yin; Zhao, Jing; RSC Advances 12 (2022) 35461–35468; doi:10.1039/D2RA06858C

data_7246002
_publ_section_title
;
 Metal--organic frameworks incorporating azobenzene-based ligands as a
 heterogeneous Lewis-acid catalyst for cyanosilylation of imines
;
_journal_issue                   54
_journal_name_full               'RSC Advances'
_journal_page_first              35461
_journal_page_last               35468
_journal_paper_doi               10.1039/D2RA06858C
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C26 H18 N6 O10 Zn2, 4(H2 O)'
_chemical_formula_sum            'C26 H26 N6 O14 Zn2'
_chemical_formula_weight         777.27
_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   mixed
_audit_creation_date             2021-01-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-09-03 deposited with the CCDC.	2022-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                96.2350(10)
_cell_angle_beta                 104.8540(10)
_cell_angle_gamma                112.3330(10)
_cell_formula_units_Z            1
_cell_length_a                   7.8726(3)
_cell_length_b                   9.1910(3)
_cell_length_c                   11.7294(4)
_cell_measurement_reflns_used    6755
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      53.880
_cell_measurement_theta_min      4.650
_cell_volume                     738.39(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193.02
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7625
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.880
_diffrn_reflns_theta_min         4.650
_diffrn_source_current           2.86
_diffrn_source_power             0.1993706
_diffrn_source_voltage           69.71
_exptl_absorpt_coefficient_mu    1.794
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.6428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0922 before and 0.0484 after correction.
The Ratio of minimum to maximum transmission is 0.8564.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       block
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.487
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+1.2598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2479
_reflns_number_total             2661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra06858c2.cif
_cod_data_source_block           20200605znl1l2dma_0m_a
_cod_database_code               7246002
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.814
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups, All O(H,H,H) groups
2.a Riding coordinates:
 O6(H6A,H6B), O7(H5B,H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13)
2.c Idealised tetrahedral OH refined as rotating group:
 O5(H5A)
;
_shelx_res_checksum              24484
_olex2_submission_special_instructions 'No special instructions were received'