#------------------------------------------------------------------------------
#$Date: 2025-10-06 10:51:21 +0300 (Mon, 06 Oct 2025) $
#$Revision: 302531 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/52/1575250.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_1575250
loop_
_publ_author_name
'Chen, Zhongwei'
'Wu, Jin'
'Deng, Zeyu'
'Chen, Congcong'
'Feng, Jianning'
'Ma, Baixu'
'Tao, Lizhi'
'Mao, Lingling'
'Lu, Haipeng'
_publ_section_title
;
 Topochemical photocycloaddition in two-dimensional lead-halide
 coordination polymers with tunable phosphorescence.
;
_journal_issue                   35
_journal_name_full               'Chemical science'
_journal_page_first              16004
_journal_page_last               16015
_journal_paper_doi               10.1039/d5sc04306a
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C12 H10 Cl2 N2 Pb'
_chemical_formula_sum            'C12 H10 Cl2 N2 Pb'
_chemical_formula_weight         460.31
_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   geom
_audit_creation_date             2024-12-03
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-03 deposited with the CCDC.	2025-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                74.107(5)
_cell_angle_beta                 85.675(5)
_cell_angle_gamma                81.700(5)
_cell_formula_units_Z            1
_cell_length_a                   4.0476(2)
_cell_length_b                   8.8861(5)
_cell_length_c                   9.5086(5)
_cell_measurement_reflns_used    1770
_cell_measurement_temperature    99.97(10)
_cell_measurement_theta_max      29.2040
_cell_measurement_theta_min      2.8040
_cell_volume                     325.25(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00  29.00   1.00    1.50    --   15.85 -66.00-167.00   73
  2  ω    -19.00  92.00   1.00    1.50    --   15.85  66.00 -32.00  111
  3  ω    -40.00  51.00   1.00    1.50    --   15.85 -77.00  90.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1745695000
_diffrn_orient_matrix_UB_12      0.0155413000
_diffrn_orient_matrix_UB_13      -0.0104473000
_diffrn_orient_matrix_UB_21      0.0243371000
_diffrn_orient_matrix_UB_22      0.0679621000
_diffrn_orient_matrix_UB_23      -0.0577163000
_diffrn_orient_matrix_UB_31      0.0184461000
_diffrn_orient_matrix_UB_32      -0.0463048000
_diffrn_orient_matrix_UB_33      -0.0508319000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2030
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.728
_diffrn_reflns_theta_min         2.809
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.356
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.350
_exptl_crystal_description       block
_exptl_crystal_F_000             212
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.060
_refine_diff_density_min         -1.578
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0278
_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)+(0.0331P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1358
_reflns_number_total             1360
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5sc04306a2.cif
_cod_data_source_block           czw-0611-pbclcn
_cod_depositor_comments
'Adding full bibliography for 1575246--1575255.cif.'
_cod_database_code               1575250
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Pb Cl C N'
_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   0.690
_shelx_estimated_absorpt_t_min   0.379
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C003(H003), C006(H006), C007(H007), C008(H008), C009(H009)
;
_shelx_res_file
;
TITL czw-0611-pbclcn_a.res in P-1
    czw-0611-pbclcn.res
    created by SHELXL-2019/3 at 16:19:15 on 03-Dec-2024
REM Old TITL CZW-0611-PbClCN in P1
REM SHELXT solution in P-1: R1 0.059, Rweak 0.264, Alpha 0.031
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C14 Cl2 Pb
CELL 0.71073 4.0476 8.8861 9.5086 74.107 85.675 81.7
ZERR 1 0.0002 0.0005 0.0005 0.005 0.005 0.005
LATT 1
SFAC C H Cl N Pb
UNIT 12 10 2 2 1

L.S. 4 0 0
PLAN  1
SIZE 0.03 0.08 0.09
TEMP -173
CONF
list 4
fmap 2 53
acta
MORE -1
BOND $H
SHEL 999 0.79
OMIT -3 0 1
OMIT -1 4 0
OMIT -1 4 2
OMIT 0 0 1
OMIT 0 0 5
OMIT 0 1 0
OMIT 1 -4 2
OMIT 1 -4 3
OMIT 2 3 2
REM <olex2.extras>
REM <HklSrc "%.\\CZW-0611-PbClCN.hkl">
REM </olex2.extras>

WGHT    0.033100
FVAR       0.66141
PB01  5    0.500000    0.500000    1.000000    10.50000    0.01093    0.01498 =
         0.01399   -0.00732   -0.00055   -0.00224
CL02  3    0.965895    0.693400    0.824703    11.00000    0.01903    0.02039 =
         0.02163   -0.00039    0.00116   -0.00136
C003  1    0.565772    0.065341    0.492801    11.00000    0.02055    0.02413 =
         0.02184   -0.00363   -0.00061   -0.00108
AFIX  43
H003  2    0.669178    0.110599    0.400828    11.00000   -1.20000
AFIX   0
N004  4    0.555410    0.318779    0.816324    11.00000    0.02290    0.02211 =
         0.01623   -0.00762   -0.00748    0.00266
C005  1    0.564743    0.146700    0.608540    11.00000    0.01585    0.02253 =
         0.01874   -0.00809   -0.00607    0.00534
C006  1    0.431027    0.180729    0.849882    11.00000    0.02606    0.01474 =
         0.02378   -0.00675   -0.00616   -0.00022
AFIX  43
H006  2    0.340365    0.141847    0.946005    11.00000   -1.20000
AFIX   0
C007  1    0.685640    0.370436    0.681543    11.00000    0.02316    0.02119 =
         0.02257   -0.00758   -0.00461   -0.00108
AFIX  43
H007  2    0.776679    0.467485    0.656971    11.00000   -1.20000
AFIX   0
C008  1    0.429051    0.092448    0.750493    11.00000    0.02395    0.01458 =
         0.02287   -0.01079   -0.00566    0.00305
AFIX  43
H008  2    0.336348   -0.004234    0.778341    11.00000   -1.20000
AFIX   0
C009  1    0.694661    0.289105    0.575157    11.00000    0.02479    0.02642 =
         0.01769   -0.01296   -0.00579    0.00023
AFIX  43
H009  2    0.789095    0.330745    0.480306    11.00000   -1.20000
AFIX   0
HKLF 4




REM  czw-0611-pbclcn_a.res in P-1
REM wR2 = 0.0664, GooF = S = 1.060, Restrained GooF = 1.060 for all data
REM R1 = 0.0278 for 1358 Fo > 4sig(Fo) and 0.0282 for all 1360 data
REM 79 parameters refined using 0 restraints

END

WGHT      0.0331      0.0000

REM Highest difference peak  2.060,  deepest hole -1.578,  1-sigma level  0.226
Q1    1   0.6226  0.3994  1.0458  11.00000  0.05    2.06
;
_shelx_res_checksum              60796
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.140
_oxdiff_exptl_absorpt_empirical_full_min 0.769
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Pb01 Pb 0.500000 0.500000 1.000000 0.01255(12) Uani 1 2 d S . P . .
Cl02 Cl 0.9659(4) 0.69340(19) 0.82470(16) 0.0216(3) Uani 1 1 d . . . . .
C003 C 0.5658(17) 0.0653(8) 0.4928(7) 0.0229(14) Uani 1 1 d . . . . .
H003 H 0.669178 0.110599 0.400828 0.027 Uiso 1 1 calc R U . . .
N004 N 0.5554(14) 0.3188(7) 0.8163(5) 0.0201(11) Uani 1 1 d . . . . .
C005 C 0.5647(16) 0.1467(8) 0.6085(7) 0.0190(13) Uani 1 1 d . . . . .
C006 C 0.4310(17) 0.1807(8) 0.8499(7) 0.0212(13) Uani 1 1 d . . . . .
H006 H 0.340365 0.141847 0.946005 0.025 Uiso 1 1 calc R U . . .
C007 C 0.6856(17) 0.3704(8) 0.6815(7) 0.0219(14) Uani 1 1 d . . . . .
H007 H 0.776679 0.467485 0.656971 0.026 Uiso 1 1 calc R U . . .
C008 C 0.4291(17) 0.0924(8) 0.7505(7) 0.0196(13) Uani 1 1 d . . . . .
H008 H 0.336348 -0.004234 0.778341 0.024 Uiso 1 1 calc R U . . .
C009 C 0.6947(17) 0.2891(8) 0.5752(7) 0.0217(14) Uani 1 1 d . . . . .
H009 H 0.789095 0.330745 0.480306 0.026 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb01 0.01093(17) 0.01498(18) 0.01399(17) -0.00732(11) -0.00055(11) -0.00224(12)
Cl02 0.0190(7) 0.0204(8) 0.0216(8) -0.0004(6) 0.0012(6) -0.0014(6)
C003 0.021(3) 0.024(3) 0.022(3) -0.004(3) -0.001(3) -0.001(3)
N004 0.023(3) 0.022(3) 0.016(3) -0.008(2) -0.007(2) 0.003(2)
C005 0.016(3) 0.023(3) 0.019(3) -0.008(2) -0.006(2) 0.005(3)
C006 0.026(4) 0.015(3) 0.024(3) -0.007(2) -0.006(3) 0.000(3)
C007 0.023(3) 0.021(3) 0.023(3) -0.008(3) -0.005(3) -0.001(3)
C008 0.024(3) 0.015(3) 0.023(3) -0.011(2) -0.006(3) 0.003(3)
C009 0.025(3) 0.026(4) 0.018(3) -0.013(3) -0.006(3) 0.000(3)
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'
Cl Cl 0.1484 0.1585 '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'
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
Cl02 Pb01 Cl02 180.0 2_667 . ?
Cl02 Pb01 Cl02 180.0 1_455 2_767 ?
Cl02 Pb01 Cl02 90.36(4) . 2_767 ?
Cl02 Pb01 Cl02 89.64(4) . 1_455 ?
Cl02 Pb01 Cl02 89.64(4) 2_667 2_767 ?
Cl02 Pb01 Cl02 90.36(4) 2_667 1_455 ?
N004 Pb01 Cl02 92.89(12) 2_667 1_455 ?
N004 Pb01 Cl02 88.65(13) . 2_667 ?
N004 Pb01 Cl02 91.35(13) . . ?
N004 Pb01 Cl02 87.11(12) . 1_455 ?
N004 Pb01 Cl02 88.65(13) 2_667 . ?
N004 Pb01 Cl02 91.35(13) 2_667 2_667 ?
N004 Pb01 Cl02 87.11(12) 2_667 2_767 ?
N004 Pb01 Cl02 92.89(12) . 2_767 ?
N004 Pb01 N004 180.0 2_667 . ?
Pb01 Cl02 Pb01 89.64(4) . 1_655 ?
C003 C003 H003 117.5 2_656 . ?
C003 C003 C005 124.9(8) 2_656 . ?
C005 C003 H003 117.5 . . ?
C006 N004 Pb01 122.2(4) . . ?
C007 N004 Pb01 119.8(4) . . ?
C007 N004 C006 117.7(6) . . ?
C008 C005 C003 124.1(6) . . ?
C009 C005 C003 118.7(6) . . ?
C009 C005 C008 117.2(6) . . ?
N004 C006 H006 118.6 . . ?
N004 C006 C008 122.9(6) . . ?
C008 C006 H006 118.6 . . ?
N004 C007 H007 118.4 . . ?
N004 C007 C009 123.2(6) . . ?
C009 C007 H007 118.4 . . ?
C005 C008 H008 120.2 . . ?
C006 C008 C005 119.5(6) . . ?
C006 C008 H008 120.2 . . ?
C005 C009 C007 119.5(6) . . ?
C005 C009 H009 120.2 . . ?
C007 C009 H009 120.2 . . ?
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
Pb01 Cl02 2.8602(15) 2_667 ?
Pb01 Cl02 2.8822(16) 2_767 ?
Pb01 Cl02 2.8602(15) . ?
Pb01 Cl02 2.8822(16) 1_455 ?
Pb01 N004 2.659(5) 2_667 ?
Pb01 N004 2.659(5) . ?
C003 C003 1.316(14) 2_656 ?
C003 H003 0.9500 . ?
C003 C005 1.472(9) . ?
N004 C006 1.342(9) . ?
N004 C007 1.333(9) . ?
C005 C008 1.401(9) . ?
C005 C009 1.388(10) . ?
C006 H006 0.9500 . ?
C006 C008 1.385(9) . ?
C007 H007 0.9500 . ?
C007 C009 1.391(9) . ?
C008 H008 0.9500 . ?
C009 H009 0.9500 . ?
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
Pb01 N004 C006 C008 173.6(5) . . . . ?
Pb01 N004 C007 C009 -173.9(5) . . . . ?
C003 C003 C005 C008 1.5(13) 2_656 . . . ?
C003 C003 C005 C009 -176.0(9) 2_656 . . . ?
C003 C005 C008 C006 -177.9(6) . . . . ?
C003 C005 C009 C007 177.8(6) . . . . ?
N004 C006 C008 C005 0.7(10) . . . . ?
N004 C007 C009 C005 -0.3(11) . . . . ?
C006 N004 C007 C009 0.7(10) . . . . ?
C007 N004 C006 C008 -0.9(10) . . . . ?
C008 C005 C009 C007 0.1(10) . . . . ?
C009 C005 C008 C006 -0.3(9) . . . . ?
