#------------------------------------------------------------------------------
#$Date: 2025-10-06 09:51:21 +0200 (Mon 06 de Oct de 2025) $
#$Revision: 302531 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/52/1575248.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_1575248
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         '0.5(C24 H20 I4 N4 Pb2)'
_chemical_formula_sum            'C12 H10 I2 N2 Pb'
_chemical_formula_weight         643.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-29
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6147(9)
_cell_length_b                   10.2110(3)
_cell_length_c                   7.2904(3)
_cell_measurement_reflns_used    3115
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.2610
_cell_measurement_theta_min      2.3160
_cell_volume                     1460.16(10)
_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 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -41.00  52.00   1.00    3.00    --   16.01 -77.00   0.00   93
  2  ω    -41.00  52.00   1.00    3.00    --   16.01 -77.00-120.00   93
  3  ω    -42.00  50.00   1.00    3.00    --   16.01 -77.00 120.00   92
;
_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      -0.0044033000
_diffrn_orient_matrix_UB_12      0.0040900000
_diffrn_orient_matrix_UB_13      0.0964029000
_diffrn_orient_matrix_UB_21      0.0275664000
_diffrn_orient_matrix_UB_22      0.0449026000
_diffrn_orient_matrix_UB_23      0.0051913000
_diffrn_orient_matrix_UB_31      -0.0230278000
_diffrn_orient_matrix_UB_32      0.0527851000
_diffrn_orient_matrix_UB_33      -0.0119772000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7186
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.346
_diffrn_reflns_theta_min         3.588
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.764
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30917
_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    2.926
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.716
_refine_diff_density_min         -1.261
_refine_diff_density_rms         0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.256
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1326
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.238
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0349
_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)+(0.0090P)²+11.2187P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0578
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1118
_reflns_number_total             1326
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5sc04306a2.cif
_cod_data_source_block           czw-0410-pbicn
_cod_depositor_comments
'Adding full bibliography for 1575246--1575255.cif.'
_cod_database_code               1575248
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N Pb I'
_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   0.451
_shelx_estimated_absorpt_t_min   0.175
_diffrn_oxdiff_digest_frames
;
0148631ab031f0e733da39c771f8a3856c000293815
;
_diffrn_oxdiff_digest_hkl
;
01b1a000c0afb50cb3142a3fa90d631e931e49
;
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.001 and sigma
for terminal atoms of 0.002
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C6(H6), C1(H1), C4(H4)
;
_shelx_res_file
;
TITL czw-0410-pbicn_a.res in Pbcn
    czw-0410-pbicn.res
    created by SHELXL-2018/3 at 13:03:46 on 10-Apr-2024
REM Old TITL czw-0410-pbicn_a.res in Pbcn
REM SHELXT solution in Pbcn: R1 0.144, Rweak 0.005, Alpha 0.033
REM <I/s> 0.710 for 263 systematic absences, Orientation as input
REM Formula found by SHELXT: C12 N2 I3
CELL 0.71073 19.6147 10.211 7.2904 90 90 90
ZERR 4 0.0009 0.0003 0.0003 0 0 0
LATT 1
SYMM 0.5-X,0.5-Y,0.5+Z
SYMM -X,+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H I N Pb
UNIT 48 40 8 8 4
ISOR 0.001 0.002 C5 C1 C2 C3 C4 C6

L.S. 4 0 0
PLAN  20
SIZE 0.06 0.09 0.17
TEMP -173.15(10)
list 4
fmap 2 53
acta
SHEL 999 0.83
OMIT 2 0 0
OMIT 1 1 0
OMIT 1 4 8
OMIT 1 0 8
OMIT 4 7 7
OMIT 4 3 7
OMIT 4 7 7
OMIT 5 2 7
OMIT 5 6 7
OMIT 4 1 10
OMIT 7 2 7
OMIT 6 3 7
REM <olex2.extras>
REM <HklSrc "%.\\CZW-0410-PbICN.hkl">
REM </olex2.extras>

WGHT    0.009000   11.218700
FVAR       0.17945
PB1   5    0.500000    0.392526    0.250000    10.50000    0.01181    0.00694 =
         0.01421    0.00000    0.00063    0.00000
I1    3    0.594549    0.624628    0.107470    11.00000    0.01521    0.01181 =
         0.01520    0.00173   -0.00092   -0.00409
N1    4    0.406863    0.219045    0.391192    11.00000    0.00964    0.01704 =
         0.00929    0.00071    0.00131   -0.00036
C5    1    0.417557    0.100803    0.467985    11.00000    0.01151    0.01138 =
         0.01123   -0.00052   -0.00015   -0.00029
C3    1    0.297823    0.071374    0.516499    11.00000    0.01844    0.01837 =
         0.01858    0.00031   -0.00024   -0.00007
AFIX  43
H3    2    0.260536    0.020695    0.559828    11.00000   -1.20000
AFIX   0
C2    1    0.286610    0.193503    0.437532    11.00000    0.01931    0.01921 =
         0.01974   -0.00006    0.00006   -0.00009
AFIX  43
H2    2    0.241804    0.227907    0.426284    11.00000   -1.20000
AFIX   0
C6    1    0.489398    0.058978    0.479172    11.00000    0.01411    0.01401 =
         0.01413   -0.00008   -0.00003   -0.00035
AFIX  43
H6    2    0.523216    0.123108    0.454002    11.00000   -1.20000
AFIX   0
C1    1    0.342018    0.262944    0.376317    11.00000    0.01697    0.01674 =
         0.01687    0.00012   -0.00022    0.00004
AFIX  43
H1    2    0.334479    0.345860    0.320804    11.00000   -1.20000
AFIX   0
C4    1    0.363690    0.024367    0.531397    11.00000    0.01787    0.01747 =
         0.01741    0.00004   -0.00046   -0.00031
AFIX  43
H4    2    0.372106   -0.059113    0.584282    11.00000   -1.20000
AFIX   0
HKLF 4




REM  czw-0410-pbicn_a.res in Pbcn
REM wR2 = 0.0578, GooF = S = 1.256, Restrained GooF = 1.238 for all data
REM R1 = 0.0349 for 1118 Fo > 4sig(Fo) and 0.0453 for all 1326 data
REM 78 parameters refined using 36 restraints

END

WGHT      0.0089     11.2221

REM Highest difference peak  1.716,  deepest hole -1.261,  1-sigma level  0.262
Q1    1   0.3137  0.3797  0.5362  11.00000  0.05    1.72
Q2    1   0.5000  0.1754  0.7500  10.50000  0.05    1.70
Q3    1   0.4001  0.3872  0.3931  11.00000  0.05    1.35
Q4    1   0.1826  0.1180  0.3680  11.00000  0.05    1.26
Q5    1   0.4995  0.3919  0.1270  11.00000  0.05    1.13
Q6    1   0.5000  0.6149  0.2500  10.50000  0.05    1.11
Q7    1   0.4031  0.1429  0.3874  11.00000  0.05    1.08
Q8    1   0.2571  0.1222  0.3680  11.00000  0.05    0.99
Q9    1   0.2814  0.1172  0.2146  11.00000  0.05    0.97
Q10   1   0.4164  0.2824  0.4640  11.00000  0.05    0.97
Q11   1   0.5000  0.1644  0.2500  10.50000  0.05    0.87
Q12   1   0.5000  0.3046  0.2500  10.50000  0.05    0.86
Q13   1   0.3421  0.0566  0.5951  11.00000  0.05    0.85
Q14   1   0.4021  0.3399  0.5707  11.00000  0.05    0.84
Q15   1   0.4012  0.3922  0.5382  11.00000  0.05    0.84
Q16   1   0.2802 -0.1239  0.5172  11.00000  0.05    0.83
Q17   1   0.2805  0.1192  0.7160  11.00000  0.05    0.82
Q18   1   0.6361  0.6355 -0.0386  11.00000  0.05    0.80
Q19   1   0.1980  0.1397  0.5466  11.00000  0.05    0.79
Q20   1   0.5050  0.6147  0.1103  11.00000  0.05    0.79
;
_shelx_res_checksum              61287
_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 2.516
_oxdiff_exptl_absorpt_empirical_full_min 0.694
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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
Pb1 Pb 0.500000 0.39253(4) 0.250000 0.01099(13) Uani 1 2 d S T P . .
I1 I 0.59455(3) 0.62463(5) 0.10747(8) 0.01408(15) Uani 1 1 d . . . . .
N1 N 0.4069(3) 0.2190(6) 0.3912(9) 0.0120(15) Uani 1 1 d . . . . .
C5 C 0.4176(4) 0.1008(7) 0.4680(12) 0.0114(18) Uani 1 1 d . U . . .
C3 C 0.2978(4) 0.0714(8) 0.5165(12) 0.018(2) Uani 1 1 d . U . . .
H3 H 0.260536 0.020695 0.559828 0.022 Uiso 1 1 calc R . . . .
C2 C 0.2866(5) 0.1935(8) 0.4375(12) 0.019(2) Uani 1 1 d . U . . .
H2 H 0.241804 0.227907 0.426284 0.023 Uiso 1 1 calc R . . . .
C6 C 0.4894(4) 0.0590(7) 0.4792(12) 0.0141(18) Uani 1 1 d . U . . .
H6 H 0.523216 0.123108 0.454002 0.017 Uiso 1 1 calc R . . . .
C1 C 0.3420(4) 0.2629(8) 0.3763(12) 0.017(2) Uani 1 1 d . U . . .
H1 H 0.334479 0.345860 0.320804 0.020 Uiso 1 1 calc R . . . .
C4 C 0.3637(4) 0.0244(8) 0.5314(12) 0.018(2) Uani 1 1 d . U . . .
H4 H 0.372106 -0.059113 0.584282 0.021 Uiso 1 1 calc R . . . .
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
Pb1 0.0118(2) 0.0069(2) 0.0142(2) 0.000 0.0006(2) 0.000
I1 0.0152(3) 0.0118(3) 0.0152(3) 0.0017(2) -0.0009(2) -0.0041(2)
N1 0.010(4) 0.017(4) 0.009(4) 0.001(3) 0.001(3) 0.000(3)
C5 0.012(2) 0.011(2) 0.011(2) -0.0005(10) -0.0001(10) -0.0003(10)
C3 0.018(2) 0.018(2) 0.019(2) 0.0003(10) -0.0002(10) -0.0001(10)
C2 0.019(2) 0.019(2) 0.020(2) -0.0001(10) 0.0001(10) -0.0001(10)
C6 0.014(2) 0.014(2) 0.014(2) -0.0001(10) 0.0000(10) -0.0003(10)
C1 0.017(2) 0.017(2) 0.017(2) 0.0001(10) -0.0002(10) 0.0000(10)
C4 0.018(2) 0.017(2) 0.017(2) 0.0000(10) -0.0005(10) -0.0003(10)
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'
I I -0.4742 1.8119 '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
I1 Pb1 I1 83.78(2) . 3_655 ?
I1 Pb1 I1 88.223(15) . 7_566 ?
I1 Pb1 I1 96.455(14) . 5_665 ?
I1 Pb1 I1 173.73(2) 5_665 7_566 ?
I1 Pb1 I1 96.455(14) 3_655 7_566 ?
I1 Pb1 I1 88.223(15) 3_655 5_665 ?
N1 Pb1 I1 92.58(14) . 7_566 ?
N1 Pb1 I1 88.30(14) . 3_655 ?
N1 Pb1 I1 92.58(14) 3_655 5_665 ?
N1 Pb1 I1 83.37(14) 3_655 7_566 ?
N1 Pb1 I1 172.08(14) . . ?
N1 Pb1 I1 172.08(14) 3_655 3_655 ?
N1 Pb1 I1 83.37(14) . 5_665 ?
N1 Pb1 I1 88.30(14) 3_655 . ?
N1 Pb1 N1 99.6(3) . 3_655 ?
Pb1 I1 Pb1 83.545(14) . 5_665 ?
C5 N1 Pb1 129.1(5) . . ?
C5 N1 C1 118.5(7) . . ?
C1 N1 Pb1 112.4(5) . . ?
N1 C5 C6 115.5(7) . . ?
N1 C5 C4 121.5(7) . . ?
C4 C5 C6 123.0(7) . . ?
C4 C3 C2 119.4(8) . . ?
C1 C2 C3 118.2(8) . . ?
C6 C6 C5 125.6(10) 5_656 . ?
N1 C1 C2 123.2(8) . . ?
C3 C4 C5 119.2(8) . . ?
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 I1 3.2034(6) 7_566 ?
Pb1 I1 3.1837(6) . ?
Pb1 I1 3.2034(6) 5_665 ?
Pb1 I1 3.1838(6) 3_655 ?
Pb1 N1 2.745(6) . ?
Pb1 N1 2.745(6) 3_655 ?
N1 C5 1.347(10) . ?
N1 C1 1.353(10) . ?
C5 C6 1.475(11) . ?
C5 C4 1.393(11) . ?
C3 C2 1.391(12) . ?
C3 C4 1.383(11) . ?
C2 C1 1.372(12) . ?
C6 C6 1.310(15) 5_656 ?
