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_1575246
_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         '2(C6 H5 Br N Pb0.5)'
_chemical_formula_sum            'C12 H10 Br2 N2 Pb'
_chemical_formula_weight         549.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_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                 114.092(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8800(9)
_cell_length_b                   4.13160(10)
_cell_length_c                   17.4968(7)
_cell_measurement_reflns_used    3963
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.7850
_cell_measurement_theta_min      2.5600
_cell_volume                     1377.93(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 0.985
_diffrn_measured_fraction_theta_max 0.986
_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  50.00   1.00   18.00    --   15.85 -77.00-150.00   90
  2  \w    -37.00  50.00   1.00   18.00    --   15.85 -77.00  90.00   87
  3  \w    -41.00  50.00   1.00   18.00    --   15.85 -77.00 -30.00   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      0.0371526000
_diffrn_orient_matrix_UB_12      -0.0093401000
_diffrn_orient_matrix_UB_13      0.0166082000
_diffrn_orient_matrix_UB_21      -0.0016946000
_diffrn_orient_matrix_UB_22      -0.1681346000
_diffrn_orient_matrix_UB_23      0.0071530000
_diffrn_orient_matrix_UB_31      -0.0017023000
_diffrn_orient_matrix_UB_32      -0.0334128000
_diffrn_orient_matrix_UB_33      -0.0405263000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6882
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.328
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.022
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47597
_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    2.648
_exptl_crystal_description       plate
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.808
_refine_diff_density_min         -2.262
_refine_diff_density_rms         0.279
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2466
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0445
_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/[\s^2^(Fo^2^)+(0.0118P)^2^+47.8779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2236
_reflns_number_total             2466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04306a2.cif
_cod_data_source_block           czw-0510-pbbr-22bpe
_cod_depositor_comments
'Adding full bibliography for 1575246--1575255.cif.'
_cod_database_code               1575246
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pb Br C N'
_shelx_estimated_absorpt_t_max   0.714
_shelx_estimated_absorpt_t_min   0.327
_diffrn_oxdiff_digest_frames
;
01543e99b78b3938225cfb02bd3dfc223e000273bf2
;
_diffrn_oxdiff_digest_hkl
;
01d96589a9318c681ed4bfa208142acde17c49
;
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(N005) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C006) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
2.a Aromatic/amide H refined with riding coordinates:
 C006(H006), C008(H008), C009(H009), C00A(H00A), C00B(H00B), C00D(H00D),
 C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H)
;
_shelx_res_checksum              51769
_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 1.744
_oxdiff_exptl_absorpt_empirical_full_min 0.737