#------------------------------------------------------------------------------
#$Date: 2022-04-28 00:56:54 +0300 (Thu, 28 Apr 2022) $
#$Revision: 274721 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/00/7130029.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7130029
loop_
_publ_author_name
'Siqin, Wu'
'Zhou, Bo'
'Fang, Xiaoyu'
'Yan, Dongpeng'
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     35.00 119.00   0.50    0.05    --   46.95  38.00  64.00  168
  2  ω    129.00 178.00   0.50    0.05    --  104.75  30.00 150.00   98
  3  ω     93.00 123.00   0.50    0.05    --  104.75  30.00 150.00   60
  4  ω    118.00 157.00   0.50    0.05    --  104.75  38.00  64.00   78
  5  ω    127.00 165.00   0.50    0.05    --  104.75  45.00 -90.00   76
  6  ω     92.00 132.00   0.50    0.05    --  104.75  30.00-180.00   80
  7  ω    138.00 163.00   0.50    0.05    --  104.75  30.00-180.00   50
  8  ω     60.00  86.00   0.50    0.05    --  104.75 -94.00-150.00   52
  9  ω     38.00  68.00   0.50    0.05    --  104.75-125.00 -90.00   60
 10  ω     69.00  95.00   0.50    0.05    --   46.95-125.00 -90.00   52
 11  ω     77.00 106.00   0.50    0.05    --  104.75-125.00 -90.00   58
 12  ω     77.00 107.00   0.50    0.05    --  104.75-125.00  30.00   60
 13  ω     82.00 116.00   0.50    0.05    --  104.75-125.00  60.00   68
 14  ω     37.00  79.00   0.50    0.05    --  104.75-125.00  60.00   84
 15  ω     35.00  60.00   0.50    0.05    --  104.75-125.00  30.00   50
 16  ω     32.00  58.00   0.50    0.05    --  104.75 -94.00  60.00   52
 17  ω     70.00 102.00   0.50    0.05    --  104.75 -94.00  60.00   64
 18  ω     38.00  64.00   0.50    0.05    --  104.75 -94.00 -90.00   52
 19  ω     46.00  73.00   0.50    0.05    --  104.75 -61.00 -30.00   54
 20  ω     33.00  71.00   0.50    0.05    --  104.75 -61.00 -60.00   76
 21  ω     36.00  63.00   0.50    0.05    --  104.75 -61.00  30.00   54
 22  ω     38.00  73.00   0.50    0.05    --  104.75 -61.00  60.00   70
 23  ω     38.00  64.00   0.50    0.05    --  104.75 -61.00 150.00   52
 24  ω    131.00 178.00   0.50    0.05    --  104.75 125.00-120.00   94
 25  ω    -26.00  41.00   0.50    0.05    --   46.95 -38.00 -90.00  134
 26  ω    -23.00  28.00   0.50    0.05    --   46.95 -19.00 120.00  102
 27  ω    103.00 129.00   0.50    0.05    --  104.75 125.00-120.00   52
 28  ω    -78.00 -12.00   0.50    0.05    --  -46.95 125.00-180.00  132
 29  ω   -117.00 -32.00   0.50    0.05    -- -102.00 125.00 -90.00  170
 30  ω    -71.00 -46.00   0.50    0.05    -- -102.00 125.00-180.00   50
 31  ω   -117.00 -77.00   0.50    0.05    -- -102.00 125.00-180.00   80
 32  ω   -103.00 -38.00   0.50    0.05    -- -102.00  77.00-150.00  130
 33  ω    -57.00 -32.00   0.50    0.05    -- -102.00  61.00 -90.00   50
 34  ω    -95.00 -70.00   0.50    0.05    -- -102.00  77.00 -30.00   50
 35  ω    -34.00  25.00   0.50    0.05    --  -46.95  38.00  64.00  118
 36  ω   -120.00 -40.00   0.50    0.05    --  -46.95 -38.00 -90.00  160
 37  ω   -175.00 -96.00   0.50    0.05    -- -102.00 -38.00 -90.00  158
 38  ω   -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       'ω 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/[σ²(Fo²)+(0.0398P)²+0.2294P] where P=(Fo²+2Fc²)/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 > 2σ(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
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.18921(3) 0.66029(2) 0.66862(2) 0.03774(9) Uani 1 1 d . . . . .
Cl1 Cl 0.20715(11) 0.75794(10) 0.90451(8) 0.04811(18) Uani 1 1 d . . . . .
Cl2 Cl 0.17734(11) 0.52414(10) 0.43380(8) 0.04677(18) Uani 1 1 d . . . . .
O4 O 0.4194(3) 1.1586(3) 0.6066(2) 0.0430(5) Uani 1 1 d . . . . .
O1 O 0.7495(3) 0.6531(3) 0.8722(2) 0.0467(5) Uani 1 1 d . . . . .
O2 O 0.4269(3) 0.5685(3) 0.7747(2) 0.0441(5) Uani 1 1 d . . . . .
O5 O 1.0766(3) 1.2046(3) 0.8064(3) 0.0509(6) Uani 1 1 d . . . . .
H5 H 1.156481 1.178182 0.846769 0.076 Uiso 1 1 calc R U . . .
O3 O 0.2064(3) 0.9083(3) 0.6011(2) 0.0438(5) Uani 1 1 d . . . . .
C6 C 0.7400(4) 1.1185(3) 0.7220(3) 0.0368(6) Uani 1 1 d . . . . .
H6 H 0.763097 1.215910 0.701506 0.044 Uiso 1 1 calc R U . . .
N1 N 0.5095(3) 0.8567(3) 0.7208(2) 0.0320(5) Uani 1 1 d . . . . .
C2 C 0.5978(4) 0.6695(3) 0.8077(3) 0.0347(6) Uani 1 1 d . . . . .
C4 C 0.8542(4) 0.9429(4) 0.8131(3) 0.0373(6) Uani 1 1 d . . . . .
H4 H 0.954544 0.920559 0.854412 0.045 Uiso 1 1 calc R U . . .
C8 C 0.3723(4) 1.0156(3) 0.6289(3) 0.0352(6) Uani 1 1 d . . . . .
C5 C 0.8959(4) 1.0902(4) 0.7827(3) 0.0370(6) Uani 1 1 d . . . . .
C7 C 0.5511(4) 0.9989(3) 0.6932(3) 0.0319(5) Uani 1 1 d . . . . .
C3 C 0.6587(4) 0.8308(3) 0.7798(3) 0.0325(5) Uani 1 1 d . . . . .
O6 O 1.3521(4) 1.1250(3) 0.9106(3) 0.0597(6) Uani 1 1 d G . . . .
H6A H 1.474193 1.178394 0.960357 0.090 Uiso 1 1 d G U . . .
H6B H 1.317756 1.028238 0.914982 0.090 Uiso 1 1 d G U . . .
C9 C 0.2609(6) 1.1949(5) 0.5495(4) 0.0519(8) Uani 1 1 d . . . . .
H9A H 0.160372 1.107449 0.469792 0.078 Uiso 1 1 calc R U . . .
H9B H 0.311507 1.294423 0.525635 0.078 Uiso 1 1 calc R U . . .
H9C H 0.206271 1.206745 0.615502 0.078 Uiso 1 1 calc R U . . .
C1 C 0.7134(6) 0.5015(4) 0.9053(4) 0.0577(9) Uani 1 1 d . . . . .
H1A H 0.624292 0.411131 0.824782 0.086 Uiso 1 1 calc R U . . .
H1B H 0.656616 0.493404 0.972340 0.086 Uiso 1 1 calc R U . . .
H1C H 0.835308 0.499699 0.940502 0.086 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Cd1 Cl2 171.73(3) . . ?
Cl2 Cd1 Cl1 95.36(3) 2_566 . ?
Cl2 Cd1 Cl2 84.60(3) 2_566 . ?
O2 Cd1 Cl1 86.87(6) . . ?
O2 Cd1 Cl2 123.10(5) . 2_566 ?
O2 Cd1 Cl2 86.25(6) . . ?
O2 Cd1 O3 136.56(7) . . ?
O3 Cd1 Cl1 95.67(6) . . ?
O3 Cd1 Cl2 99.90(5) . 2_566 ?
O3 Cd1 Cl2 92.48(6) . . ?
N1 Cd1 Cl1 92.54(6) . . ?
N1 Cd1 Cl2 89.20(6) . . ?
N1 Cd1 Cl2 166.18(6) . 2_566 ?
N1 Cd1 O2 68.59(7) . . ?
N1 Cd1 O3 67.98(7) . . ?
Cd1 Cl2 Cd1 95.40(3) 2_566 . ?
C8 O4 C9 117.7(3) . . ?
C2 O1 C1 118.3(3) . . ?
C2 O2 Cd1 113.91(18) . . ?
C5 O5 H5 109.5 . . ?
C8 O3 Cd1 114.14(18) . . ?
C5 C6 H6 120.7 . . ?
C7 C6 H6 120.7 . . ?
C7 C6 C5 118.5(3) . . ?
C7 N1 Cd1 121.55(18) . . ?
C3 N1 Cd1 120.41(18) . . ?
C3 N1 C7 118.0(2) . . ?
O1 C2 C3 111.9(2) . . ?
O2 C2 O1 125.2(3) . . ?
O2 C2 C3 122.9(2) . . ?
C5 C4 H4 120.9 . . ?
C3 C4 H4 120.9 . . ?
C3 C4 C5 118.2(3) . . ?
O4 C8 C7 111.6(2) . . ?
O3 C8 O4 125.5(3) . . ?
O3 C8 C7 122.9(2) . . ?
O5 C5 C6 117.8(3) . . ?
O5 C5 C4 123.5(3) . . ?
C6 C5 C4 118.7(3) . . ?
C6 C7 C8 123.4(2) . . ?
N1 C7 C6 123.2(3) . . ?
N1 C7 C8 113.4(2) . . ?
N1 C3 C2 114.1(2) . . ?
N1 C3 C4 123.4(3) . . ?
C4 C3 C2 122.5(2) . . ?
H6A O6 H6B 104.5 . . ?
O4 C9 H9A 109.5 . . ?
O4 C9 H9B 109.5 . . ?
O4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 Cl1 2.5260(8) . ?
Cd1 Cl2 2.6381(8) . ?
Cd1 Cl2 2.5160(8) 2_566 ?
Cd1 O2 2.483(2) . ?
Cd1 O3 2.506(2) . ?
Cd1 N1 2.312(2) . ?
O4 C8 1.319(3) . ?
O4 C9 1.455(4) . ?
O1 C2 1.308(3) . ?
O1 C1 1.453(4) . ?
O2 C2 1.213(4) . ?
O5 H5 0.8200 . ?
O5 C5 1.328(4) . ?
O3 C8 1.212(4) . ?
C6 H6 0.9300 . ?
C6 C5 1.396(4) . ?
C6 C7 1.379(4) . ?
N1 C7 1.340(3) . ?
N1 C3 1.331(4) . ?
C2 C3 1.495(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.396(4) . ?
C4 C3 1.388(4) . ?
C8 C7 1.500(4) . ?
O6 H6A 0.8499 . ?
O6 H6B 0.8501 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cd1 O2 C2 O1 175.9(2) . . . . ?
Cd1 O2 C2 C3 -3.2(3) . . . . ?
Cd1 O3 C8 O4 -178.4(2) . . . . ?
Cd1 O3 C8 C7 2.2(3) . . . . ?
Cd1 N1 C7 C6 -179.6(2) . . . . ?
Cd1 N1 C7 C8 0.9(3) . . . . ?
Cd1 N1 C3 C2 -0.5(3) . . . . ?
Cd1 N1 C3 C4 179.6(2) . . . . ?
O4 C8 C7 C6 -1.2(4) . . . . ?
O4 C8 C7 N1 178.3(2) . . . . ?
O1 C2 C3 N1 -176.6(2) . . . . ?
O1 C2 C3 C4 3.4(4) . . . . ?
O2 C2 C3 N1 2.6(4) . . . . ?
O2 C2 C3 C4 -177.4(3) . . . . ?
O3 C8 C7 C6 178.3(3) . . . . ?
O3 C8 C7 N1 -2.2(4) . . . . ?
C5 C6 C7 N1 0.2(4) . . . . ?
C5 C6 C7 C8 179.6(3) . . . . ?
C5 C4 C3 N1 -0.1(4) . . . . ?
C5 C4 C3 C2 179.9(3) . . . . ?
C7 C6 C5 O5 178.1(3) . . . . ?
C7 C6 C5 C4 -0.7(4) . . . . ?
C7 N1 C3 C2 179.5(2) . . . . ?
C7 N1 C3 C4 -0.5(4) . . . . ?
C3 N1 C7 C6 0.4(4) . . . . ?
C3 N1 C7 C8 -179.1(2) . . . . ?
C3 C4 C5 O5 -178.1(3) . . . . ?
C3 C4 C5 C6 0.7(4) . . . . ?
C9 O4 C8 O3 3.0(4) . . . . ?
C9 O4 C8 C7 -177.5(2) . . . . ?
C1 O1 C2 O2 1.4(5) . . . . ?
C1 O1 C2 C3 -179.4(3) . . . . ?
