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_1575249
_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      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_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                 91.303(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1435(8)
_cell_length_b                   14.3139(9)
_cell_length_c                   4.1064(3)
_cell_measurement_reflns_used    1333
_cell_measurement_temperature    99.94(13)
_cell_measurement_theta_max      27.3570
_cell_measurement_theta_min      2.8450
_cell_volume                     713.59(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 (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      99.94(13)
_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 0.903
_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    -39.00  52.00   1.00   30.00    --   16.01 -77.00 -90.00   91
  2  \w    -41.00  50.00   1.00   30.00    --   16.01 -77.00 150.00   91
  3  \w    -40.00  50.00   1.00   30.00    --   16.01 -77.00  30.00   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      0.0184234000
_diffrn_orient_matrix_UB_12      -0.0300765000
_diffrn_orient_matrix_UB_13      0.0461220000
_diffrn_orient_matrix_UB_21      0.1712920000
_diffrn_orient_matrix_UB_22      0.0063606000
_diffrn_orient_matrix_UB_23      -0.0008739000
_diffrn_orient_matrix_UB_31      -0.0133987000
_diffrn_orient_matrix_UB_32      0.0389210000
_diffrn_orient_matrix_UB_33      0.0357527000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            2447
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.671
_diffrn_reflns_theta_min         2.200
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.398
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37365
_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    2.509
_exptl_crystal_description       block
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.899
_refine_diff_density_min         -1.853
_refine_diff_density_rms         0.300
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         952
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0571P)^2^+6.7757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1105
_reflns_Friedel_coverage         0.000
_reflns_number_gt                912
_reflns_number_total             952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04306a2.cif
_cod_data_source_block           czw-0618-pbbr44bpe-photo
_cod_depositor_comments
'Adding full bibliography for 1575246--1575255.cif.'
_cod_database_code               1575249
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pb Br C N'
_shelx_estimated_absorpt_t_max   0.623
_shelx_estimated_absorpt_t_min   0.229
_diffrn_oxdiff_digest_frames
;
01b6c7f932cad1f0530aa83fdf8faed2a4000273fa9
;
_diffrn_oxdiff_digest_hkl
;
018c8d84a9057fa5f48b483aa76d3f98d1b514
;
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Restrained distances
 C4-C2
 1.5 with sigma of 0.1
 C1-C1_$2
 1.5 with sigma of 0.1
 C1-C1_$1
 1.5 with sigma of 0.1
 C2_$2-C2
 1.5 with sigma of 0.1
 C2_$2-C1
 1.5 with sigma of 0.1
 C2_$2-C1_$3
 1.5 with sigma of 0.1
 C1-C1_$1 \\sim C1_$2-C1
 with sigma of 0.02
 C2_$2-C1_$3 \\sim C2_$2-C1
 with sigma of 0.02
 C2-C1_$1 \\sim C2_$3-C1_$1
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C4 \\sim C11 \\sim C8 \\sim C3 \\sim C6: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 C4, C11, C6, C3, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Fixed Sof: C3(0.5) N003(0.5) C6(0.5) C11(0.5) C4(0.5) C8(0.5) C2(0.25) C1(0.25)
5.a Fitted hexagon refined as free rotating group:
 C3(N003,C6,C11,C4,C8)
;
_shelx_res_checksum              2714
_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 1.990
_oxdiff_exptl_absorpt_empirical_full_min 0.644