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#$Date: 2024-04-05 01:20:53 +0300 (Fri, 05 Apr 2024) $
#$Revision: 290793 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/09/1570975.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1570975
loop_
_publ_author_name
'Wang, Xiyu'
'Yang, Guo-Ping'
'Wang, Yao-Yu'
_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 & 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       'φ and ω 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 λ/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/[σ²(Fo²)+(0.0450P)²+0.2096P] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.06147(2) 0.86698(3) 0.17024(2) 0.01678(11) Uani 1 1 d . . . . .
Cd1 Cd 0.500000 0.79672(7) 0.250000 0.01725(16) Uani 1 2 d DS T P . .
O2 O 0.44803(19) 0.4201(6) 0.5128(3) 0.0252(9) Uani 1 1 d . . . . .
O1 O 0.43687(19) 0.4441(6) 0.6581(3) 0.0278(9) Uani 1 1 d . . . . .
O4 O 0.1619(2) 0.8405(5) 0.2328(4) 0.0272(10) Uani 1 1 d . . . . .
O3 O 0.1414(2) 0.6653(6) 0.3373(4) 0.0287(10) Uani 1 1 d . . . . .
O5 O 0.5542(6) 1.0317(18) 0.3618(9) 0.038(4) Uani 0.62(3) 1 d D . P A 1
H5A H 0.582358 1.057698 0.349456 0.057 Uiso 0.62(3) 1 d R U P A 1
H5B H 0.572008 0.995327 0.429556 0.057 Uiso 0.62(3) 1 d R U P A 1
N1 N 0.4103(2) 0.6922(6) 0.3368(4) 0.0181(10) Uani 1 1 d . . . . .
N2 N 0.4439(2) 0.8308(7) 0.3336(4) 0.0200(12) Uani 1 1 d . . . . .
N3 N 0.4357(2) 0.9791(6) 0.3759(4) 0.0250(11) Uani 1 1 d . . . . .
N4 N 0.3973(2) 0.9421(6) 0.4098(4) 0.0244(12) Uani 1 1 d . . . . .
C1 C 0.3393(3) 0.6689(7) 0.4060(4) 0.0156(11) Uani 1 1 d . . . . .
C2 C 0.2812(3) 0.7317(7) 0.3496(4) 0.0176(11) Uani 1 1 d . . . . .
H2 H 0.270499 0.827971 0.297928 0.021 Uiso 1 1 calc R U . . .
C3 C 0.2389(3) 0.6535(6) 0.3687(5) 0.0169(12) Uani 1 1 d . . . . .
C4 C 0.2555(3) 0.5135(7) 0.4476(5) 0.0203(12) Uani 1 1 d . . . . .
H4 H 0.227033 0.459865 0.460704 0.024 Uiso 1 1 calc R U . . .
C5 C 0.3133(3) 0.4532(7) 0.5065(5) 0.0222(12) Uani 1 1 d . . . . .
H5 H 0.324352 0.360335 0.560211 0.027 Uiso 1 1 calc R U . . .
C6 C 0.3553(2) 0.5311(7) 0.4856(4) 0.0168(11) Uani 1 1 d . . . . .
C7 C 0.4172(3) 0.4617(7) 0.5548(4) 0.0190(12) Uani 1 1 d . . . . .
C8 C 0.1768(3) 0.7234(7) 0.3097(5) 0.0216(12) Uani 1 1 d . . . . .
C9 C 0.3823(3) 0.7638(7) 0.3838(4) 0.0158(11) Uani 1 1 d . . . . .
O6 O 0.5832(11) 0.934(4) 0.3929(13) 0.049(7) Uani 0.38(3) 1 d D U P A 2
H6A H 0.615792 0.889272 0.397267 0.073 Uiso 0.38(3) 1 d R U P A 2
H6B H 0.584502 1.053172 0.379327 0.073 Uiso 0.38(3) 1 d R U P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Pb1 O1 141.09(12) 4 7_566 ?
O2 Pb1 O3 128.23(13) 4 . ?
O2 Pb1 N1 71.80(14) 4 4 ?
O2 Pb1 C8 106.37(14) 4 . ?
O1 Pb1 C8 92.35(14) 7_566 . ?
O4 Pb1 O2 84.38(14) . 4 ?
O4 Pb1 O1 101.52(14) . 7_566 ?
O4 Pb1 O3 52.01(13) . . ?
O4 Pb1 N1 77.84(14) . 4 ?
O4 Pb1 C8 26.09(13) . . ?
O3 Pb1 O1 81.12(13) . 7_566 ?
O3 Pb1 C8 25.96(14) . . ?
N1 Pb1 O1 72.02(13) 4 7_566 ?
N1 Pb1 O3 115.99(15) 4 . ?
N1 Pb1 C8 97.99(15) 4 . ?
O1 Cd1 O1 81.3(2) 6_565 5_666 ?
O1 Cd1 N2 84.38(15) 5_666 2_655 ?
O1 Cd1 N2 105.04(16) 6_565 2_655 ?
O1 Cd1 N2 84.38(16) 6_565 . ?
O1 Cd1 N2 105.05(16) 5_666 . ?
O1 Cd1 O6 75.2(9) 6_565 2_655 ?
O1 Cd1 O6 75.2(9) 5_666 . ?
O1 Cd1 O6 155.3(8) 6_565 . ?
O1 Cd1 O6 155.3(8) 5_666 2_655 ?
O5 Cd1 O1 99.2(5) . 5_666 ?
O5 Cd1 O1 99.2(5) 2_655 6_565 ?
O5 Cd1 O1 168.8(2) . 6_565 ?
O5 Cd1 O1 168.8(2) 2_655 5_666 ?
O5 Cd1 O5 82.4(9) . 2_655 ?
O5 Cd1 N2 84.7(3) . . ?
O5 Cd1 N2 84.7(3) 2_655 2_655 ?
O5 Cd1 N2 86.1(3) . 2_655 ?
O5 Cd1 N2 86.1(3) 2_655 . ?
O5 Cd1 O6 24.4(6) 2_655 2_655 ?
O5 Cd1 O6 105.3(13) . 2_655 ?
N2 Cd1 N2 167.8(3) 2_655 . ?
O6 Cd1 N2 94.5(6) . . ?
O6 Cd1 N2 80.2(5) 2_655 . ?
O6 Cd1 O6 129.0(17) 2_655 . ?
C7 O2 Pb1 140.6(4) . 4_545 ?
Cd1 O1 Pb1 101.49(13) 5_666 7_566 ?
C7 O1 Pb1 139.8(3) . 7_566 ?
C7 O1 Cd1 118.3(3) . 5_666 ?
C8 O4 Pb1 100.2(3) . . ?
C8 O3 Pb1 85.4(3) . . ?
Cd1 O5 H5A 109.1 . . ?
Cd1 O5 H5B 109.5 . . ?
H5A O5 H5B 104.4 . . ?
N2 N1 Pb1 119.3(3) . 4_545 ?
C9 N1 Pb1 130.2(3) . 4_545 ?
C9 N1 N2 105.3(4) . . ?
N1 N2 Cd1 122.1(3) . . ?
N3 N2 Cd1 128.1(4) . . ?
N3 N2 N1 109.7(4) . . ?
N2 N3 N4 109.0(4) . . ?
N3 N4 C9 105.3(4) . . ?
C2 C1 C6 119.3(5) . . ?
C2 C1 C9 117.4(5) . . ?
C6 C1 C9 123.1(5) . . ?
C1 C2 H2 119.7 . . ?
C1 C2 C3 120.7(5) . . ?
C3 C2 H2 119.7 . . ?
C2 C3 C4 119.3(5) . . ?
C2 C3 C8 120.7(5) . . ?
C4 C3 C8 119.9(5) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 C3 120.6(5) . . ?
C5 C4 H4 119.7 . . ?
C4 C5 H5 120.2 . . ?
C4 C5 C6 119.5(5) . . ?
C6 C5 H5 120.2 . . ?
C1 C6 C5 120.5(5) . . ?
C1 C6 C7 123.2(5) . . ?
C5 C6 C7 116.2(5) . . ?
O2 C7 O1 121.7(5) . . ?
O2 C7 C6 121.5(5) . . ?
O1 C7 C6 116.8(5) . . ?
O4 C8 Pb1 53.7(3) . . ?
O4 C8 C3 118.4(5) . . ?
O3 C8 Pb1 68.6(3) . . ?
O3 C8 O4 122.3(6) . . ?
O3 C8 C3 119.3(5) . . ?
C3 C8 Pb1 171.3(4) . . ?
N1 C9 N4 110.7(4) . . ?
N1 C9 C1 127.0(4) . . ?
N4 C9 C1 122.4(4) . . ?
Cd1 O6 H6A 110.9 . . ?
Cd1 O6 H6B 110.8 . . ?
H6A O6 H6B 103.2 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O2 2.483(4) 4 ?
Pb1 O1 2.753(4) 7_566 ?
Pb1 O4 2.328(4) . ?
Pb1 O3 2.655(4) . ?
Pb1 N1 2.486(4) 4 ?
Pb1 C8 2.841(6) . ?
Cd1 O1 2.300(4) 6_565 ?
Cd1 O1 2.300(4) 5_666 ?
Cd1 O5 2.263(7) . ?
Cd1 O5 2.263(7) 2_655 ?
Cd1 N2 2.317(4) 2_655 ?
Cd1 N2 2.317(4) . ?
Cd1 O6 2.311(13) 2_655 ?
Cd1 O6 2.311(13) . ?
O2 C7 1.256(6) . ?
O1 C7 1.275(6) . ?
O4 C8 1.269(6) . ?
O3 C8 1.248(7) . ?
O5 H5A 0.8614 . ?
O5 H5B 0.8613 . ?
N1 N2 1.352(6) . ?
N1 C9 1.319(7) . ?
N2 N3 1.298(7) . ?
N3 N4 1.343(6) . ?
N4 C9 1.345(7) . ?
C1 C2 1.391(8) . ?
C1 C6 1.394(7) . ?
C1 C9 1.487(7) . ?
C2 H2 0.9400 . ?
C2 C3 1.392(8) . ?
C3 C4 1.398(7) . ?
C3 C8 1.494(8) . ?
C4 H4 0.9400 . ?
C4 C5 1.382(9) . ?
C5 H5 0.9400 . ?
C5 C6 1.397(7) . ?
C6 C7 1.496(8) . ?
O6 H6A 0.8888 . ?
O6 H6B 0.8882 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb1 O2 C7 O1 167.0(4) 4_545 . . . ?
Pb1 O2 C7 C6 -11.9(9) 4_545 . . . ?
Pb1 O1 C7 O2 137.0(5) 7_566 . . . ?
Pb1 O1 C7 C6 -44.0(8) 7_566 . . . ?
Pb1 O4 C8 O3 -4.6(6) . . . . ?
Pb1 O4 C8 C3 175.4(4) . . . . ?
Pb1 O3 C8 O4 4.0(5) . . . . ?
Pb1 O3 C8 C3 -176.0(4) . . . . ?
Pb1 N1 N2 Cd1 26.7(5) 4_545 . . . ?
Pb1 N1 N2 N3 -157.7(4) 4_545 . . . ?
Pb1 N1 C9 N4 153.7(4) 4_545 . . . ?
Pb1 N1 C9 C1 -27.1(9) 4_545 . . . ?
Cd1 O1 C7 O2 -34.1(7) 5_666 . . . ?
Cd1 O1 C7 C6 144.8(4) 5_666 . . . ?
Cd1 N2 N3 N4 176.2(4) . . . . ?
N1 N2 N3 N4 1.0(6) . . . . ?
N2 N1 C9 N4 0.1(6) . . . . ?
N2 N1 C9 C1 179.4(5) . . . . ?
N2 N3 N4 C9 -0.8(6) . . . . ?
N3 N4 C9 N1 0.4(7) . . . . ?
N3 N4 C9 C1 -178.9(5) . . . . ?
C1 C2 C3 C4 1.5(8) . . . . ?
C1 C2 C3 C8 178.8(5) . . . . ?
C1 C6 C7 O2 -47.1(8) . . . . ?
C1 C6 C7 O1 134.0(5) . . . . ?
C2 C1 C6 C5 1.7(8) . . . . ?
C2 C1 C6 C7 -176.6(5) . . . . ?
C2 C1 C9 N1 -114.6(6) . . . . ?
C2 C1 C9 N4 64.6(7) . . . . ?
C2 C3 C4 C5 0.2(8) . . . . ?
C2 C3 C8 O4 8.0(8) . . . . ?
C2 C3 C8 O3 -172.0(5) . . . . ?
C3 C4 C5 C6 -1.0(8) . . . . ?
C4 C3 C8 O4 -174.8(5) . . . . ?
C4 C3 C8 O3 5.2(8) . . . . ?
C4 C5 C6 C1 0.1(8) . . . . ?
C4 C5 C6 C7 178.5(5) . . . . ?
C5 C6 C7 O2 134.6(5) . . . . ?
C5 C6 C7 O1 -44.4(7) . . . . ?
C6 C1 C2 C3 -2.5(8) . . . . ?
C6 C1 C9 N1 70.1(8) . . . . ?
C6 C1 C9 N4 -110.7(6) . . . . ?
C8 C3 C4 C5 -177.1(5) . . . . ?
C9 N1 N2 Cd1 -176.2(4) . . . . ?
C9 N1 N2 N3 -0.7(6) . . . . ?
C9 C1 C2 C3 -178.0(5) . . . . ?
C9 C1 C6 C5 176.9(5) . . . . ?
C9 C1 C6 C7 -1.4(8) . . . . ?
