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_1575253
_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           26
_space_group_name_Hall           'P 2c -2'
_space_group_name_H-M_alt        'P m c 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.3660(3)
_cell_length_b                   9.7804(4)
_cell_length_c                   18.0733(8)
_cell_measurement_reflns_used    5240
_cell_measurement_temperature    99.97(10)
_cell_measurement_theta_max      28.1740
_cell_measurement_theta_min      2.0880
_cell_volume                     771.75(7)
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -11.00  94.00   1.00   11.50    --   15.85  57.00 150.00  105
  2  \w     -5.00  93.00   1.00   11.50    --   15.85  57.00 -90.00   98
  3  \w    -13.00  92.00   1.00   11.50    --   15.85  37.00  60.00  105
  4  \w    -36.00  52.00   1.00   11.50    --   15.85 -77.00 -90.00   88
  5  \w    -33.00  52.00   1.00   11.50    --   15.85 -77.00   0.00   85
  6  \w    -42.00  52.00   1.00   11.50    --   15.85 -77.00 120.00   94
;
_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      0.1502375000
_diffrn_orient_matrix_UB_12      -0.0213777000
_diffrn_orient_matrix_UB_13      0.0091953000
_diffrn_orient_matrix_UB_21      -0.0602368000
_diffrn_orient_matrix_UB_22      -0.0615272000
_diffrn_orient_matrix_UB_23      0.0149998000
_diffrn_orient_matrix_UB_31      0.0137463000
_diffrn_orient_matrix_UB_32      -0.0319062000
_diffrn_orient_matrix_UB_33      -0.0350806000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9852
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         26.698
_diffrn_reflns_theta_min         2.251
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.909
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28092
_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    2.699
_exptl_crystal_description       block
_exptl_crystal_F_000             542
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.170
_refine_diff_density_min         -2.320
_refine_diff_density_rms         0.216
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.44(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         1873
_refine_ls_number_restraints     257
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0352P)^2^+7.9567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1776
_reflns_number_total             1873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04306a2.cif
_cod_data_source_block           czw-0507-pbicn-24bpe
_cod_depositor_comments
'Adding full bibliography for 1575246--1575255.cif.'
_cod_original_cell_volume        771.75(6)
_cod_database_code               1575253
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N Pb I'
_shelx_estimated_absorpt_t_max   0.587
_shelx_estimated_absorpt_t_min   0.199
_diffrn_oxdiff_digest_frames
;
01434622160f60191ab6a862269fc13df20002749da
;
_diffrn_oxdiff_digest_hkl
;
01f8ef3f9e28040b2761b159bde424712c8eb8
;
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.55932
 0.44068
2. Restrained distances
 C8-C15 = C15-C5
 1.4 with sigma of 0.02
 C5A-C2A
 1.4 with sigma of 0.1
 C2A-N1 = N1-C2
 1.6 with sigma of 0.1
 C2AA_$1-C1AA_$1
 1.5 with sigma of 0.1
 C8-C5
 2.598 with sigma of 0.04
 C8-C0AA \\sim C8-C15
 with sigma of 0.02
 C8-C15 \\sim C5-C15
 with sigma of 0.02
 C5-C15 \\sim C5-C2
 with sigma of 0.02
 C3AA-C2AA \\sim C2AA-C2AA_$2 \\sim C3AA_$2-C2AA_$2 \\sim C3AA-C3AA_$2
 with sigma of 0.02
3. Restrained planarity
 C0AA, C8, C15, C5, C2
 with sigma of 0.1
 N2, C6, C16, C1AA, C3, C1
 with sigma of 0.1
4. Rigid bond restraints
 N2, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
C0AA \\sim C8 \\sim C15 \\sim C5 \\sim C2 \\sim N1 \\sim C8A \\sim C15A \\sim
C5A \\sim C2A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C3) \\sim Ueq, Uanis(C1AA) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C16) \\sim
Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
6. Rigid body (RIGU) restrains
 C2, C0AA, C5, C8, C15, N1, C2A, C5A, C8A, C15A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
7. Others
 Fixed Sof: I1(0.25) I4(0.25) C1AA(0.5) C16(0.5) C6(0.5) N2(0.5) C1(0.5)
 C3(0.5) C2AA(0.5) C3AA(0.5) C0AA(0.5) C8A(0.25) C15A(0.25) C5A(0.25) C2A(0.25)
 C8(0.25) C15(0.25) C5(0.25) C2(0.25)
8.a Fitted hexagon refined as free rotating group:
 C1AA(C16,C6,N2,C1,C3), N1(C0AA,C8A,C15A,C5A,C2A)
;
_shelx_res_checksum              8590
_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 2.186
_oxdiff_exptl_absorpt_empirical_full_min 0.703