Catalytic comparison of cyanosilylation/Knoevenagel condensation reactions by Pb-based heterometallic organic frameworks with different second metal ions
Wang, Xiyu; Yang, Guo-Ping; Wang, Yao-Yu; Catalysis Science & Technology 14 (2024) 1613–1621; doi:10.1039/D3CY01549A

data_1570975
_publ_section_title
;
 Catalytic comparison of cyanosilylation/Knoevenagel condensation
 reactions by Pb-based heterometallic organic frameworks with different
 second metal ions
;
_journal_issue                   6
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              1613
_journal_page_last               1621
_journal_paper_doi               10.1039/D3CY01549A
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C9 H5 Cd0.5 N4 O5 Pb'
_chemical_formula_sum            'C9 H5 Cd0.5 N4 O5 Pb'
_chemical_formula_weight         512.56
_chemical_name_systematic        PbCd
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-08-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-08-28 deposited with the CCDC.	2024-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.5110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.2822(12)
_cell_length_b                   7.2428(2)
_cell_length_c                   14.0420(6)
_cell_measurement_reflns_used    4829
_cell_measurement_temperature    210.0
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.90
_cell_volume                     2302.86(16)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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      210.0
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6736
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.393
_diffrn_reflns_theta_min         2.903
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.576
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4100
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1182 before and 0.0508 after correction.
The Ratio of minimum to maximum transmission is 0.5502.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.957
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.485
_refine_diff_density_min         -1.637
_refine_diff_density_rms         0.286
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2094
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0267
_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^)+(0.0450P)^2^+0.2096P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1990
_reflns_number_total             2094
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cy01549a2.cif
_cod_data_source_block           mo_5wxypb_0m_a
_cod_depositor_comments
'Adding full bibliography for 1570973--1570975.cif.'
_cod_original_formula_sum        'C9 H5 Cd0.50 N4 O5 Pb'
_cod_database_code               1570975
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.746
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Cd1-O5 \\sim Cd1-O6
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(O6)=Sof(H6A)=Sof(H6B)=1-FVAR(1)
 Sof(O5)=Sof(H5A)=Sof(H5B)=FVAR(1)
5.a Rotating group:
 O5(H5A,H5B), O6(H6A,H6B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5)
;
_shelx_res_checksum              53123
_shelx_hkl_checksum              40120
_olex2_submission_special_instructions 'No special instructions were received'