Chelation-activated ultralong room-temperature phosphorescence and thermo-/excitation-dependent persistent luminescence
Siqin, Wu; Zhou, Bo; Fang, Xiaoyu; Yan, Dongpeng; Chemical Communications  (2022) –; doi:10.1039/D2CC01485H

data_7130029
_publ_section_title
;
 Chelation-activated ultralong room-temperature phosphorescence and
 thermo-/excitation-dependent persistent luminescence
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01485H
_journal_year                    2022
_chemical_formula_moiety         '0.125(C18 H18 Cd2 Cl4 N2 O10), 0.25(H2 O)'
_chemical_formula_sum            'C2.25 H2.75 Cd0.25 Cl0.5 N0.25 O1.5'
_chemical_formula_weight         103.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-11-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-11-22 deposited with the CCDC.	2022-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                97.5378(13)
_cell_angle_beta                 107.1123(13)
_cell_angle_gamma                114.8620(17)
_cell_formula_units_Z            8
_cell_length_a                   8.13035(13)
_cell_length_b                   9.45773(18)
_cell_length_c                   10.76925(13)
_cell_measurement_reflns_used    6233
_cell_measurement_temperature    300
_cell_measurement_theta_max      76.1710
_cell_measurement_theta_min      4.4620
_cell_volume                     686.37(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      300
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.948
_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     35.00 119.00   0.50    0.05    --   46.95  38.00  64.00  168
  2  \w    129.00 178.00   0.50    0.05    --  104.75  30.00 150.00   98
  3  \w     93.00 123.00   0.50    0.05    --  104.75  30.00 150.00   60
  4  \w    118.00 157.00   0.50    0.05    --  104.75  38.00  64.00   78
  5  \w    127.00 165.00   0.50    0.05    --  104.75  45.00 -90.00   76
  6  \w     92.00 132.00   0.50    0.05    --  104.75  30.00-180.00   80
  7  \w    138.00 163.00   0.50    0.05    --  104.75  30.00-180.00   50
  8  \w     60.00  86.00   0.50    0.05    --  104.75 -94.00-150.00   52
  9  \w     38.00  68.00   0.50    0.05    --  104.75-125.00 -90.00   60
 10  \w     69.00  95.00   0.50    0.05    --   46.95-125.00 -90.00   52
 11  \w     77.00 106.00   0.50    0.05    --  104.75-125.00 -90.00   58
 12  \w     77.00 107.00   0.50    0.05    --  104.75-125.00  30.00   60
 13  \w     82.00 116.00   0.50    0.05    --  104.75-125.00  60.00   68
 14  \w     37.00  79.00   0.50    0.05    --  104.75-125.00  60.00   84
 15  \w     35.00  60.00   0.50    0.05    --  104.75-125.00  30.00   50
 16  \w     32.00  58.00   0.50    0.05    --  104.75 -94.00  60.00   52
 17  \w     70.00 102.00   0.50    0.05    --  104.75 -94.00  60.00   64
 18  \w     38.00  64.00   0.50    0.05    --  104.75 -94.00 -90.00   52
 19  \w     46.00  73.00   0.50    0.05    --  104.75 -61.00 -30.00   54
 20  \w     33.00  71.00   0.50    0.05    --  104.75 -61.00 -60.00   76
 21  \w     36.00  63.00   0.50    0.05    --  104.75 -61.00  30.00   54
 22  \w     38.00  73.00   0.50    0.05    --  104.75 -61.00  60.00   70
 23  \w     38.00  64.00   0.50    0.05    --  104.75 -61.00 150.00   52
 24  \w    131.00 178.00   0.50    0.05    --  104.75 125.00-120.00   94
 25  \w    -26.00  41.00   0.50    0.05    --   46.95 -38.00 -90.00  134
 26  \w    -23.00  28.00   0.50    0.05    --   46.95 -19.00 120.00  102
 27  \w    103.00 129.00   0.50    0.05    --  104.75 125.00-120.00   52
 28  \w    -78.00 -12.00   0.50    0.05    --  -46.95 125.00-180.00  132
 29  \w   -117.00 -32.00   0.50    0.05    -- -102.00 125.00 -90.00  170
 30  \w    -71.00 -46.00   0.50    0.05    -- -102.00 125.00-180.00   50
 31  \w   -117.00 -77.00   0.50    0.05    -- -102.00 125.00-180.00   80
 32  \w   -103.00 -38.00   0.50    0.05    -- -102.00  77.00-150.00  130
 33  \w    -57.00 -32.00   0.50    0.05    -- -102.00  61.00 -90.00   50
 34  \w    -95.00 -70.00   0.50    0.05    -- -102.00  77.00 -30.00   50
 35  \w    -34.00  25.00   0.50    0.05    --  -46.95  38.00  64.00  118
 36  \w   -120.00 -40.00   0.50    0.05    --  -46.95 -38.00 -90.00  160
 37  \w   -175.00 -96.00   0.50    0.05    -- -102.00 -38.00 -90.00  158
 38  \w   -163.00 -96.00   0.50    0.05    -- -102.00 -45.00  60.00  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1357034000
_diffrn_orient_matrix_UB_12      0.0072446000
_diffrn_orient_matrix_UB_13      -0.0759549000
_diffrn_orient_matrix_UB_21      0.0653278000
_diffrn_orient_matrix_UB_22      0.1820216000
_diffrn_orient_matrix_UB_23      0.0163413000
_diffrn_orient_matrix_UB_31      0.1693517000
_diffrn_orient_matrix_UB_32      0.0457571000
_diffrn_orient_matrix_UB_33      0.1359637000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7604
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.375
_diffrn_reflns_theta_min         4.494
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64091
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.996
_exptl_crystal_description       block
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2725
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+0.2294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2618
_reflns_number_total             2725
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01485h2.cif
_cod_data_source_block           exp_2495
_cod_original_formula_sum        'C2.25 H2.75 Cd0.25 Cl0.50 N0.25 O1.50'
_cod_database_code               7130029
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         CNHOCdCl
_reflns_odcompleteness_completeness 99.06
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O6(H6a,H6b)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4)
2.c Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C1(H1a,H1b,H1c)
2.d Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_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 1.445
_oxdiff_exptl_absorpt_empirical_full_min 0.762