Topochemical photocycloaddition in two-dimensional lead-halide coordination polymers with tunable phosphorescence.
Chen, Zhongwei; Wu, Jin; Deng, Zeyu; Chen, Congcong; Feng, Jianning; Ma, Baixu; Tao, Lizhi; Mao, Lingling; Lu, Haipeng; Chemical science 16 (2025) 16004–16015; doi:10.1039/d5sc04306a

data_1575247
_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 I4 N4 Pb2)'
_chemical_formula_sum            'C12 I2 N2 Pb'
_chemical_formula_weight         633.13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_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            2
_cell_length_a                   9.6885(6)
_cell_length_b                   17.9090(11)
_cell_length_c                   4.3360(3)
_cell_measurement_reflns_used    2727
_cell_measurement_temperature    99.97(11)
_cell_measurement_theta_max      29.3960
_cell_measurement_theta_min      3.0780
_cell_volume                     752.35(8)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -40.00  51.00   1.00    8.00    --   15.85 -77.00 -30.00   91
  2  \w    -40.00  51.00   1.00    8.00    --   15.85 -77.00-150.00   91
  3  \w    -41.00  50.00   1.00    8.00    --   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       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0011965000
_diffrn_orient_matrix_UB_12      0.0712195000
_diffrn_orient_matrix_UB_13      -0.0365766000
_diffrn_orient_matrix_UB_21      -0.0030882000
_diffrn_orient_matrix_UB_22      0.0166794000
_diffrn_orient_matrix_UB_23      0.1590065000
_diffrn_orient_matrix_UB_31      0.0394653000
_diffrn_orient_matrix_UB_32      -0.0008854000
_diffrn_orient_matrix_UB_33      0.0135625000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            4152
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.345
_diffrn_reflns_theta_min         2.274
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.295
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42137
_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            'light yellow'
_exptl_crystal_density_diffrn    2.795
_exptl_crystal_description       plate
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.549
_refine_diff_density_min         -2.112
_refine_diff_density_rms         0.336
_refine_ls_abs_structure_details
;
 Flack x determined using 442 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.265
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1382
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0605
_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/[\s^2^(Fo^2^)+(0.0001P)^2^+56.3077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1381
_reflns_Friedel_coverage         0.628
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1311
_reflns_number_total             1382
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04306a2.cif
_cod_data_source_block           czw-0423-pbicn-24bpe
_cod_depositor_comments
'Adding full bibliography for 1575246--1575255.cif.'
_cod_database_code               1575247
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pb I C N'
_diffrn_oxdiff_digest_frames
;
0122a3da9f0c6f47cb417795a4f42a88dd0002850c3
;
_diffrn_oxdiff_digest_hkl
;
01c9236ce7156c00188447742a21ed0cb8d62c
;
_reflns_odcompleteness_completeness 99.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Restrained distances
 C2B-C1B \\sim C2A-C1B
 with sigma of 0.02
 C3B-C2A \\sim C3B-C2B
 with sigma of 0.02
 C4-C3B \\sim C4-C3A
 with sigma of 0.02
 C3B-C2B \\sim C3A-C2A
 with sigma of 0.02
 C2B-C1B \\sim C2A-C1A
 with sigma of 0.02
 N1-C1B \\sim N1-C1A
 with sigma of 0.02
 C7_$1-C3B \\sim C7_$1-C3A
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C2B \\sim C2A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C3B \\sim C3A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C1B \\sim C1A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Pb1 \\sim N1 \\sim I1 \\sim C1B \\sim C5 \\sim C1A \\sim C2B \\sim C4 \\sim C6
\\sim C2A \\sim C3B \\sim C3A \\sim C7: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3B) \\sim
Ueq, Uanis(C2B) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C5)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 C2B, C2A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C3A, C3B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C1B, C1A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Others
 Fixed Sof: C1B(0.5) C2B(0.5) C3B(0.5) C6(0.48) C7(0.52) C2A(0.5) C3A(0.5)
 C1A(0.5)
;
_shelx_res_checksum              97944
_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 2.016
_oxdiff_exptl_absorpt_empirical_full_min 0.554