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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/1/57/09/1570973.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_1570973
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 Mn0.5 N4 O5 Pb'
_chemical_formula_sum            'C9 H5 Mn0.5 N4 O5 Pb'
_chemical_formula_weight         483.83
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-05-31
_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                 120.864(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.1891(17)
_cell_length_b                   7.1383(4)
_cell_length_c                   14.0543(11)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    210.0
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.90
_cell_volume                     2255.3(3)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      210.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0490
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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            16442
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.372
_diffrn_reflns_theta_min         2.900
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.522
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.3498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1483 before and 0.0740 after correction.
The Ratio of minimum to maximum transmission is 0.4694.
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    2.850
_exptl_crystal_description       block
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          2
_exptl_crystal_size_mid          2
_exptl_crystal_size_min          2
_refine_diff_density_max         1.437
_refine_diff_density_min         -1.361
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2067
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0277P)²+10.5744P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0571
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1973
_reflns_number_total             2067
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cy01549a2.cif
_cod_data_source_block           mo_5wxy_0m_a
_cod_depositor_comments
'Adding full bibliography for 1570973--1570975.cif.'
_cod_original_formula_sum        'C9 H5 Mn0.50 N4 O5 Pb'
_cod_database_code               1570973
_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   0.013
_shelx_estimated_absorpt_t_min   0.013
_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
 Mn1-H5A \\sim Mn1-H5B
 with sigma of 0.02
3.a Free rotating group:
 O5(H5A,H5B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6)
;
_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 0.06117(2) 0.13605(2) 0.17500(2) 0.01595(9) Uani 1 1 d . . . . .
Mn1 Mn 0.500000 0.80189(13) 0.750000 0.0146(2) Uani 1 2 d DS T P . .
O1 O 0.16148(17) 0.1650(5) 0.2369(3) 0.0277(9) Uani 1 1 d . . . . .
O2 O 0.14360(17) 0.3416(5) 0.3445(3) 0.0288(9) Uani 1 1 d . . . . .
O3 O 0.44961(16) 0.5863(5) 0.5070(3) 0.0249(8) Uani 1 1 d . . . . .
O4 O 0.44040(16) 0.5712(5) 0.6540(3) 0.0225(7) Uani 1 1 d . . . . .
O5 O 0.5578(2) 1.0068(7) 0.8672(3) 0.0433(12) Uani 1 1 d G . . . .
H5A H 0.589425 1.024765 0.864458 0.065 Uiso 1 1 d DG U . . .
H5B H 0.570539 0.973606 0.934572 0.065 Uiso 1 1 d DG U . . .
N1 N 0.40940(18) 0.3086(6) 0.3305(3) 0.0184(8) Uani 1 1 d . . . . .
N2 N 0.44311(18) 0.1691(6) 0.3274(3) 0.0180(9) Uani 1 1 d . . . . .
N3 N 0.43698(19) 0.0215(6) 0.3753(3) 0.0204(9) Uani 1 1 d . . . . .
N4 N 0.3991(2) 0.0600(6) 0.4106(4) 0.0211(9) Uani 1 1 d . . . . .
C1 C 0.2407(2) 0.3520(6) 0.3726(4) 0.0173(10) Uani 1 1 d . . . . .
C2 C 0.2577(2) 0.4928(7) 0.4508(4) 0.0207(10) Uani 1 1 d . . . . .
H2 H 0.229627 0.546560 0.465459 0.025 Uiso 1 1 calc R U . . .
C3 C 0.3159(2) 0.5541(7) 0.5073(4) 0.0210(10) Uani 1 1 d . . . . .
H3 H 0.327532 0.648253 0.561331 0.025 Uiso 1 1 calc R U . . .
C4 C 0.3578(2) 0.4774(6) 0.4848(4) 0.0158(9) Uani 1 1 d . . . . .
C5 C 0.3407(2) 0.3357(6) 0.4057(4) 0.0148(10) Uani 1 1 d . . . . .
C6 C 0.2821(2) 0.2730(6) 0.3508(4) 0.0167(10) Uani 1 1 d . . . . .
H6 H 0.270415 0.176097 0.298409 0.020 Uiso 1 1 calc R U . . .
C7 C 0.3833(2) 0.2402(6) 0.3821(4) 0.0141(9) Uani 1 1 d . . . . .
C8 C 0.1781(2) 0.2838(7) 0.3147(4) 0.0188(10) Uani 1 1 d . . . . .
C9 C 0.4197(2) 0.5497(6) 0.5512(4) 0.0175(10) Uani 1 1 d . . . . .
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'
Mn Mn 0.3368 0.7283 '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
O1 Pb1 O2 51.46(12) . . ?
O1 Pb1 O3 84.60(13) . 4_545 ?
O1 Pb1 N1 77.55(13) . 4_545 ?
O3 Pb1 O2 127.93(12) 4_545 . ?
O3 Pb1 N1 72.61(13) 4_545 4_545 ?
N1 Pb1 O2 114.98(13) 4_545 . ?
O4 Mn1 O4 82.66(19) . 2_656 ?
O4 Mn1 N2 85.88(14) . 6_566 ?
O4 Mn1 N2 85.88(14) 2_656 5_666 ?
O4 Mn1 N2 102.08(14) . 5_666 ?
O4 Mn1 N2 102.09(14) 2_656 6_566 ?
O5 Mn1 O4 170.22(14) 2_656 2_656 ?
O5 Mn1 O4 170.22(14) . . ?
O5 Mn1 O4 92.33(17) . 2_656 ?
O5 Mn1 O4 92.33(17) 2_656 . ?
O5 Mn1 O5 93.8(3) 2_656 . ?
O5 Mn1 N2 86.98(15) . 6_566 ?
O5 Mn1 N2 85.85(15) 2_656 6_566 ?
O5 Mn1 N2 85.85(15) . 5_666 ?
O5 Mn1 N2 86.98(15) 2_656 5_666 ?
N2 Mn1 N2 169.5(2) 6_566 5_666 ?
C8 O1 Pb1 101.8(3) . . ?
C8 O2 Pb1 85.0(3) . . ?
C9 O3 Pb1 141.5(3) . 4 ?
C9 O4 Mn1 123.1(3) . . ?
Mn1 O5 H5A 112.6 . . ?
Mn1 O5 H5B 112.4 . . ?
H5A O5 H5B 104.5 . . ?
N2 N1 Pb1 118.5(3) . 4 ?
C7 N1 Pb1 128.6(3) . 4 ?
C7 N1 N2 106.2(4) . . ?
N1 N2 Mn1 123.6(3) . 5_666 ?
N3 N2 Mn1 127.5(3) . 5_666 ?
N3 N2 N1 108.9(4) . . ?
N2 N3 Pb1 129.1(3) . 4_545 ?
N2 N3 N4 109.6(4) . . ?
N4 N3 Pb1 113.5(3) . 4_545 ?
N3 N4 C7 104.9(4) . . ?
C2 C1 C6 120.1(5) . . ?
C2 C1 C8 119.1(4) . . ?
C6 C1 C8 120.8(4) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 C1 119.8(4) . . ?
C3 C2 H2 120.1 . . ?
C2 C3 H3 119.7 . . ?
C2 C3 C4 120.6(4) . . ?
C4 C3 H3 119.7 . . ?
C3 C4 C9 116.8(4) . . ?
C5 C4 C3 119.6(4) . . ?
C5 C4 C9 123.5(4) . . ?
C4 C5 C7 122.7(4) . . ?
C6 C5 C4 119.2(4) . . ?
C6 C5 C7 118.1(4) . . ?
C1 C6 C5 120.7(4) . . ?
C1 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
N1 C7 N4 110.5(4) . . ?
N1 C7 C5 127.9(4) . . ?
N4 C7 C5 121.6(4) . . ?
O1 C8 C1 118.9(4) . . ?
O2 C8 O1 121.5(5) . . ?
O2 C8 C1 119.5(4) . . ?
O3 C9 O4 122.1(5) . . ?
O3 C9 C4 121.2(4) . . ?
O4 C9 C4 116.7(4) . . ?
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 O1 2.314(4) . ?
Pb1 O2 2.685(4) . ?
Pb1 O3 2.451(3) 4_545 ?
Pb1 N1 2.475(4) 4_545 ?
Mn1 O4 2.193(4) . ?
Mn1 O4 2.193(4) 2_656 ?
Mn1 O5 2.141(4) . ?
Mn1 O5 2.141(4) 2_656 ?
Mn1 N2 2.260(4) 5_666 ?
Mn1 N2 2.260(4) 6_566 ?
O1 C8 1.271(6) . ?
O2 C8 1.245(6) . ?
O3 C9 1.251(6) . ?
O4 C9 1.264(6) . ?
O5 H5A 0.8593 . ?
O5 H5B 0.8601 . ?
N1 N2 1.346(6) . ?
N1 C7 1.319(6) . ?
N2 N3 1.304(6) . ?
N3 N4 1.346(5) . ?
N4 C7 1.348(6) . ?
C1 C2 1.384(7) . ?
C1 C6 1.388(7) . ?
C1 C8 1.489(7) . ?
C2 H2 0.9400 . ?
C2 C3 1.380(7) . ?
C3 H3 0.9400 . ?
C3 C4 1.400(7) . ?
C4 C5 1.396(7) . ?
C4 C9 1.489(7) . ?
C5 C6 1.390(7) . ?
C5 C7 1.483(6) . ?
C6 H6 0.9400 . ?
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 O1 C8 O2 5.3(5) . . . . ?
Pb1 O1 C8 C1 -175.9(3) . . . . ?
Pb1 O2 C8 O1 -4.5(5) . . . . ?
Pb1 O2 C8 C1 176.7(4) . . . . ?
Pb1 O3 C9 O4 -165.4(4) 4 . . . ?
Pb1 O3 C9 C4 14.9(8) 4 . . . ?
Pb1 N1 N2 Mn1 -25.8(4) 4 . . 5_666 ?
Pb1 N1 N2 N3 154.1(3) 4 . . . ?
Pb1 N1 C7 N4 -150.9(3) 4 . . . ?
Pb1 N1 C7 C5 31.0(7) 4 . . . ?
Pb1 N3 N4 C7 -152.8(3) 4_545 . . . ?
Mn1 O4 C9 O3 36.5(6) . . . . ?
Mn1 O4 C9 C4 -143.8(3) . . . . ?
Mn1 N2 N3 Pb1 -33.5(6) 5_666 . . 4_545 ?
Mn1 N2 N3 N4 -179.8(3) 5_666 . . . ?
N1 N2 N3 Pb1 146.6(3) . . . 4_545 ?
N1 N2 N3 N4 0.3(5) . . . . ?
N2 N1 C7 N4 -0.7(5) . . . . ?
N2 N1 C7 C5 -178.9(5) . . . . ?
N2 N3 N4 C7 -0.7(5) . . . . ?
N3 N4 C7 N1 0.9(5) . . . . ?
N3 N4 C7 C5 179.1(4) . . . . ?
C1 C2 C3 C4 1.1(8) . . . . ?
C2 C1 C6 C5 -1.0(7) . . . . ?
C2 C1 C8 O1 174.6(5) . . . . ?
C2 C1 C8 O2 -6.6(7) . . . . ?
C2 C3 C4 C5 -1.0(7) . . . . ?
C2 C3 C4 C9 -178.9(4) . . . . ?
C3 C4 C5 C6 -0.1(7) . . . . ?
C3 C4 C5 C7 -176.4(4) . . . . ?
C3 C4 C9 O3 -137.1(5) . . . . ?
C3 C4 C9 O4 43.2(6) . . . . ?
C4 C5 C6 C1 1.1(7) . . . . ?
C4 C5 C7 N1 -71.8(7) . . . . ?
C4 C5 C7 N4 110.3(5) . . . . ?
C5 C4 C9 O3 45.0(7) . . . . ?
C5 C4 C9 O4 -134.7(5) . . . . ?
C6 C1 C2 C3 -0.2(7) . . . . ?
C6 C1 C8 O1 -7.0(7) . . . . ?
C6 C1 C8 O2 171.8(5) . . . . ?
C6 C5 C7 N1 111.9(6) . . . . ?
C6 C5 C7 N4 -66.0(6) . . . . ?
C7 N1 N2 Mn1 -179.6(3) . . . 5_666 ?
C7 N1 N2 N3 0.3(5) . . . . ?
C7 C5 C6 C1 177.5(4) . . . . ?
C8 C1 C2 C3 178.3(4) . . . . ?
C8 C1 C6 C5 -179.4(4) . . . . ?
C9 C4 C5 C6 177.6(4) . . . . ?
C9 C4 C5 C7 1.4(7) . . . . ?
