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_1575254
_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         'C12 H10 Cl2 N2 Pb'
_chemical_formula_sum            'C12 H10 Cl2 N2 Pb'
_chemical_formula_weight         460.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-12-03
_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                 97.269(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.9385(3)
_cell_length_b                   28.0476(15)
_cell_length_c                   11.9766(7)
_cell_measurement_reflns_used    2703
_cell_measurement_temperature    99.93(16)
_cell_measurement_theta_max      28.1090
_cell_measurement_theta_min      2.8890
_cell_volume                     1312.37(15)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.90 (release 15-09-2023))'
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      99.93(16)
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.885
_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    -42.00  48.00   0.50   60.00    --   12.44 -77.00 120.00  180
  2  \w    -41.00  48.00   0.50   60.00    --   12.44 -77.00-120.00  178
  3  \w    -41.00  48.00   0.50   60.00    --   12.44 -77.00   0.00  178
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Mo, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4008
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.311
_diffrn_reflns_theta_min         2.247
_exptl_absorpt_coefficient_mu    13.240
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66663
_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    2.330
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.055
_refine_diff_density_min         -1.410
_refine_diff_density_rms         0.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         1451
_refine_ls_number_restraints     454
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0403P)^2^+5.4229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1376
_reflns_number_total             1451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04306a2.cif
_cod_data_source_block           ericwu132a_mo100k_autored
_cod_depositor_comments
'Adding full bibliography for 1575246--1575255.cif.'
_cod_original_cell_volume        1312.35(14)
_cod_database_code               1575254
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.778
_shelx_estimated_absorpt_t_min   0.692
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C13-C1 = C43-C4 = C33-C3 = C23-C2
 1.52 with sigma of 0.02
 C12-C11 = C13-C12 = C14-C13 = C15-C14
 1.38 with sigma of 0.02
 C22-C21 = C23-C22 = C24-C23 = C25-C24
 1.38 with sigma of 0.02
 C32-C31 = C33-C32 = C34-C33 = C35-C34
 1.38 with sigma of 0.02
 C42-C41 = C43-C42 = C44-C43 = C45-C44
 1.38 with sigma of 0.02
 N1-C11 = N1-C15 = N2-C21 = N2-C25 = N4-C31 = N4-C35 = N3-C41 = N3-C45
 1.36 with sigma of 0.02
 C11-C13
 2.38 with sigma of 0.02
 C12-C14
 2.38 with sigma of 0.02
 C13-C15
 2.38 with sigma of 0.02
 C21-C23
 2.38 with sigma of 0.02
 C22-C24
 2.38 with sigma of 0.02
 C23-C25
 2.38 with sigma of 0.02
 C31-C33
 2.38 with sigma of 0.02
 C32-C34
 2.38 with sigma of 0.02
 C33-C35
 2.38 with sigma of 0.02
 C41-C43
 2.38 with sigma of 0.02
 C42-C44
 2.38 with sigma of 0.02
 C43-C45
 2.38 with sigma of 0.02
 C4-C1 \\sim C2-C1 \\sim C3-C2 \\sim C4-C3
 with sigma of 0.02
3. Restrained planarity
 N1, C11, C12, C13, C14, C15
 with sigma of 0.02
 N2, C21, C22, C23, C24, C25
 with sigma of 0.02
 N4, C31, C32, C33, C34, C35
 with sigma of 0.02
 N3, C41, C42, C43, C44, C45
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(N2)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(C13) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C22) \\sim Ueq,
Uanis(N3) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(N4)
\\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq,
Uanis(C43) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C34) \\sim Ueq:
with sigma of 0.003 and sigma for terminal atoms of 0.005
5. Rigid body (RIGU) restrains
 Pb01, N1, N2, N3, N4, C1, C2, C3, C4, C11, C12, C13, C14, C15, C21, C22, C23,
 C24, C25, C31, C32, C33, C34, C35, C41, C42, C43, C44, C45
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: N1(0.25) N2(0.25) N3(0.25) N4(0.25) C1(0.25) H1(0.25) C2(0.25)
 H2(0.25) C3(0.25) H3(0.25) C4(0.25) H4(0.25) C11(0.25) H11(0.25) C12(0.25)
 H12(0.25) C13(0.25) C14(0.25) H14(0.25) C15(0.25) H15(0.25) C21(0.25)
 H21(0.25) C22(0.25) H22(0.25) C23(0.25) C24(0.25) H24(0.25) C25(0.25)
 H25(0.25) C31(0.25) H31(0.25) C32(0.25) H32(0.25) C33(0.25) C34(0.25)
 H34(0.25) C35(0.25) H35(0.25) C41(0.25) H41(0.25) C42(0.25) H42(0.25)
 C43(0.25) C44(0.25) H44(0.25) C45(0.25) H45(0.25)
7.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
7.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C14(H14), C15(H15), C21(H21), C22(H22), C24(H24),
 C25(H25), C31(H31), C32(H32), C34(H34), C35(H35), C41(H41), C42(H42), C44(H44),
  C45(H45)
;
_shelx_res_checksum              68687
_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
;