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_7130030
_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         'C21 H17 Cd N5 O11'
_chemical_formula_sum            'C21 H17 Cd N5 O11'
_chemical_formula_weight         627.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-12-26
_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                90
_cell_angle_beta                 100.388(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4639(4)
_cell_length_b                   14.5590(4)
_cell_length_c                   14.1126(4)
_cell_measurement_reflns_used    10021
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.7140
_cell_measurement_theta_min      4.3530
_cell_volume                     2316.83(12)
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.963
_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     58.00 114.00   0.50    0.05    --   46.95  61.00 -83.00  112
  2  \w     89.00 159.00   0.50    0.06    --  104.75  61.00 -83.00  140
  3  \w    117.00 177.00   0.50    0.06    --  104.75  45.00-150.00  120
  4  \w     93.00 177.00   0.50    0.06    --  104.75  15.00-180.00  168
  5  \w     38.00  72.00   0.50    0.06    --  104.75 -61.00 -60.00   68
  6  \w     32.00  62.00   0.50    0.06    --  104.75 -77.00  30.00   60
  7  \w     76.00 108.00   0.50    0.06    --  104.75 -77.00  30.00   64
  8  \w     33.00  73.00   0.50    0.06    --  104.75 -61.00 137.00   80
  9  \w    -25.00  62.00   0.50    0.05    --   46.95 -61.00 137.00  174
 10  \w     36.00  72.00   0.50    0.06    --  104.75 -61.00-180.00   72
 11  \w     71.00 104.00   0.50    0.06    --  104.75 -94.00 -90.00   66
 12  \w    -57.00  25.00   0.50    0.05    --  -46.95  61.00 -83.00  164
 13  \w    -67.00 -39.00   0.50    0.06    -- -102.00  61.00 -90.00   56
 14  \w    -61.00 -36.00   0.50    0.06    -- -102.00  61.00-150.00   50
 15  \w    -62.00 -29.00   0.50    0.06    -- -102.00  61.00 -83.00   66
 16  \w    -69.00 -44.00   0.50    0.06    -- -102.00  61.00-120.00   50
 17  \w    -68.00 -29.00   0.50    0.06    -- -102.00  61.00 -30.00   78
 18  \w    -54.00 -29.00   0.50    0.06    -- -102.00  61.00  30.00   50
 19  \w    -56.00 -31.00   0.50    0.06    -- -102.00  61.00 120.00   50
 20  \w   -158.00-132.00   0.50    0.06    -- -102.00 -45.00  30.00   52
 21  \w   -168.00-143.00   0.50    0.06    -- -102.00 -61.00 137.00   50
 22  \w    -99.00 -74.00   0.50    0.05    --  -46.95 -61.00 137.00   50
 23  \w   -130.00 -91.00   0.50    0.06    -- -102.00 -45.00  30.00   78
 24  \w   -115.00 -74.00   0.50    0.05    --  -46.95-125.00 -90.00   82
 25  \w   -118.00 -89.00   0.50    0.05    --  -46.95-125.00-120.00   58
 26  \w   -169.00-119.00   0.50    0.06    -- -102.00 -94.00-120.00  100
;
_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      0.1035827000
_diffrn_orient_matrix_UB_12      -0.0679749000
_diffrn_orient_matrix_UB_13      0.0018239000
_diffrn_orient_matrix_UB_21      -0.0169523000
_diffrn_orient_matrix_UB_22      -0.0343796000
_diffrn_orient_matrix_UB_23      0.0998306000
_diffrn_orient_matrix_UB_31      -0.0874708000
_diffrn_orient_matrix_UB_32      -0.0734277000
_diffrn_orient_matrix_UB_33      -0.0484710000
_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  0.0445
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16419
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.268
_diffrn_reflns_theta_min         4.401
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.219
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30094
_exptl_absorpt_correction_type   multi-scan
_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 yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.067
_refine_diff_density_min         -1.820
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         4672
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0839P)^2^+6.0637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4290
_reflns_number_total             4672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01485h2.cif
_cod_data_source_block           20201201-5
_cod_depositor_comments
;

2025-03-05
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C2.55 H2.06 Cd0.12 N0.61 O1.33'
_cod_original_formula_weight         76.10
_cod_original_formula_moiety         '0.121(C21 H17 Cd N5 O11)'
_cod_original_formula_units_Z            33
_cod_original_cell_volume        2316.85(13)
_cod_database_code               7130030
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         CHONCd
_reflns_odcompleteness_completeness 99.88
_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
2.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C19(H19), C21(H21), C23(H23), C26(H26),
 C29(H29), C30(H30), C33(H33)
2.b Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
2.c Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_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 2.697
_oxdiff_exptl_absorpt_empirical_full_min 0.630