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_1575252
_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         'Br2 C12 N2 Pb'
_chemical_formula_sum            'C12 Br2 N2 Pb'
_chemical_formula_weight         539.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_atom_sites_solution_primary     dual
_audit_creation_date             2024-12-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_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                   8.8284(2)
_cell_length_b                   18.8885(5)
_cell_length_c                   4.15040(10)
_cell_measurement_reflns_used    3810
_cell_measurement_temperature    99.95(11)
_cell_measurement_theta_max      28.3070
_cell_measurement_theta_min      2.5540
_cell_volume                     692.10(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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.95(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     -9.00  91.00   1.00   12.00    --   15.85  57.00 -90.00  100
  2  \w     -8.00  90.00   1.00   12.00    --   15.85  37.00-180.00   98
  3  \w     -6.00  94.00   1.00   12.00    --   15.85  57.00  30.00  100
  4  \w    -15.00  59.00   1.00   12.00    --   15.85 -99.00   0.00   74
  5  \w    -39.00  52.00   1.00   12.00    --   15.85 -77.00 120.00   91
  6  \w    -38.00  52.00   1.00   12.00    --   15.85 -77.00-120.00   90
;
_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      -0.0346519000
_diffrn_orient_matrix_UB_12      0.0148812000
_diffrn_orient_matrix_UB_13      -0.0577909000
_diffrn_orient_matrix_UB_21      -0.0120649000
_diffrn_orient_matrix_UB_22      0.0092703000
_diffrn_orient_matrix_UB_23      0.1606484000
_diffrn_orient_matrix_UB_31      0.0079929000
_diffrn_orient_matrix_UB_32      0.0783967000
_diffrn_orient_matrix_UB_33      -0.0080188000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            8361
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         2.156
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.939
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48905
_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    2.587
_exptl_crystal_description       plate
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.631
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         844
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0236P)^2^+4.3835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0634
_reflns_Friedel_coverage         0.000
_reflns_number_gt                732
_reflns_number_total             844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04306a2.cif
_cod_data_source_block           czw-0704-22bpe-pbbr-photo
_cod_depositor_comments
'Adding full bibliography for 1575246--1575255.cif.'
_cod_database_code               1575252
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pb Br C N '
_shelx_estimated_absorpt_t_max   0.615
_shelx_estimated_absorpt_t_min   0.367
_diffrn_oxdiff_digest_frames
;
015c626b6722ddd571ae242ba5692deeeb000274872
;
_diffrn_oxdiff_digest_hkl
;
019cba770abf2f5399e446f2003b2251ff9bec
;
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Restrained distances
 Pb01-Br \\sim Pb01-Br1
 with sigma of 0.02
 C3-C0 \\sim C3-C4
 with sigma of 0.02
 C6-C4 \\sim C6-C0
 with sigma of 0.02
 C3-C5 \\sim C3-C1
 with sigma of 0.02
 C003-C1 \\sim C003-C5
 with sigma of 0.02
 Pb01-N0 \\sim Pb01-N1
 with sigma of 0.02
 N0-C003 \\sim N1-C003
 with sigma of 0.02
 N1-C6 \\sim N0-C6
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Br \\sim Br1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C0 \\sim C4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C5 \\sim C1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N1 \\sim N0: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N0) \\sim Ueq, Uanis(C003) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C0) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N0) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 Br1, Br
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C4, C0
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C5, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N0, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: Br(0.25) C0(0.25) N0(0.25) C1(0.25) C6(0.5) Br1(0.25) C2(0.5)
 C4(0.25) C5(0.25) N1(0.25)
;
_shelx_res_checksum              83742
_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 1.702
_oxdiff_exptl_absorpt_empirical_full_min 0.699