High-temperature negative thermal quenching phosphors from molecular-based materials.
Miao, Huixian; Zhou, Yujie; Wang, Pingping; Huang, Zetao; Zhaxi, Wenjiang; Liu, Luying; Duan, Fengnan; Wang, Jinmin; Ma, Xiao; Jiang, Shenlong; Huang, Wei; Zhang, Qun; Wu, Dayu; Chemical communications (Cambridge, England) 59 (2023) 1229–1232; doi:10.1039/d2cc05921e

data_7131159
_publ_section_title
;
 High-temperature negative thermal quenching phosphors from
 molecular-based materials.
;
_journal_issue                   9
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1229
_journal_page_last               1232
_journal_paper_doi               10.1039/d2cc05921e
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C32 H36 Cu4 I4 N8'
_chemical_formula_sum            'C32 H36 Cu4 I4 N8'
_chemical_formula_weight         1294.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-12-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-12-31 deposited with the CCDC.	2023-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.860(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9276(2)
_cell_length_b                   14.0857(4)
_cell_length_c                   29.8293(8)
_cell_measurement_reflns_used    16877
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.9650
_cell_measurement_theta_min      1.6390
_cell_volume                     3750.66(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.64a (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  'SHELXL-2019/2 (Sheldrick, 2019)'
_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 1.000
_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  34.00   0.50    0.68    --  -11.30 -99.00-120.00   90
  2  \w    -11.00  14.00   0.50    0.68    --  -11.30 -99.00 -90.00   50
  3  \w     -8.00  55.00   0.50    0.68    --   10.52 -99.00 -30.00  126
  4  \w    -26.00   1.00   0.50    0.68    --   10.52  92.00 175.00   54
  5  \w    -53.00  -7.00   0.50    0.68    --  -11.30  92.00 175.00   92
  6  \w    -29.00  69.00   0.50    0.68    --  -11.30  19.00  60.00  196
  7  \w    -23.00   9.00   0.50    0.68    --   10.52 -92.00  62.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0319241000
_diffrn_orient_matrix_UB_12      0.0225314000
_diffrn_orient_matrix_UB_13      -0.0191328000
_diffrn_orient_matrix_UB_21      -0.0458681000
_diffrn_orient_matrix_UB_22      -0.0403516000
_diffrn_orient_matrix_UB_23      -0.0039658000
_diffrn_orient_matrix_UB_31      -0.0565540000
_diffrn_orient_matrix_UB_32      0.0200054000
_diffrn_orient_matrix_UB_33      0.0135271000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            27355
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.346
_diffrn_reflns_theta_min         1.599
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.566
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.64a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.292
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.924
_refine_diff_density_min         -2.022
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         6863
_refine_ls_number_restraints     1716
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0768
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+151.7966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.1848
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6172
_reflns_number_total             6863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05921e2.cif
_cod_data_source_block           CP2
_cod_depositor_comments
'Adding full bibliography for 7131158--7131159.cif.'
_cod_database_code               7131159
_shelx_shelxl_version_number     2019/2
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9936(5)
 0.0064(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1A
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(I1A) \\sim Ueq, Uanis(I4A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Same fragment restrains
{C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2, C8_2, C9_2, C10_2, C11_2, C12_2,
C13_2, C14_2, C15_2, C16_2, N1_2, N2_2, N3_2, N4_2}
{C1_3, C2_3, C3_3, C4_3, C5_3, C6_3, C7_3, C8_3, C9_3, C10_3, C11_3, C12_3,
C13_3, C14_3, C15_3, C16_3, N1_3, N2_3, N3_3, N4_3}
{C1_4, C2_4, C3_4, C4_4, C5_4, C6_4, C7_4, C8_4, C9_4, C10_4, C11_4, C12_4,
C13_4, C14_4, C15_4, C16_4, N1_4, N2_4, N3_4, N4_4}
as
{C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1, C8_1, C9_1, C10_1, C11_1, C12_1,
C13_1, C14_1, C15_1, C16_1, N1_1, N2_1, N3_1, N4_1} sigma for 1-2: 0.01 1-3:
0.04
5. Others
 Sof(Cu1A)=Sof(Cu2A)=Sof(Cu3A)=Sof(Cu4A)=Sof(I1A)=Sof(I2A)=Sof(I3A)=Sof(I4A)=
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8)=Sof(C9)=
 Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C13)=
 Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(N1)=Sof(N2)=Sof(N3)=Sof(N4)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=
 Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(C7)=
 Sof(H7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(C12)=
 Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=
 Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(N1)=Sof(N2)=Sof(N3)=Sof(N4)=1-FVAR(1)
 Sof(Cu1)=Sof(Cu2)=Sof(Cu3)=Sof(Cu4)=Sof(I1)=Sof(I2)=Sof(I3)=Sof(I4)=Sof(C1)=
 Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=
 Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=
 Sof(C10)=Sof(H10)=Sof(C11)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(C14)=
 Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(N1)=
 Sof(N2)=Sof(N3)=Sof(N4)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(C3)=
 Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(C7)=Sof(H7)=
 Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(C12)=Sof(H12A)=
 Sof(H12B)=Sof(C13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16A)=
 Sof(H16B)=Sof(H16C)=Sof(N1)=Sof(N2)=Sof(N3)=Sof(N4)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C12(H12A,H12B), C5(H5A,H5B), C12(H12A,H12B), C5(H5A,H5B),
 C12(H12A,H12B), C5(H5A,H5B), C12(H12A,H12B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15), C3(H3),
 C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15), C3(H3), C4(H4),
 C7(H7), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15), C3(H3), C4(H4), C7(H7),
 C8(H8), C9(H9), C10(H10), C14(H14), C15(H15)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C1(H1A,H1B,H1C), C16(H16A,H16B,H16C),
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C1(H1A,H1B,H1C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              7944
_shelx_hkl_checksum              37468
_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 1.285
_oxdiff_exptl_absorpt_empirical_full_min 0.704