Excimer emission and magnetoluminescence of radical-based zinc(II) complexes doped in host crystals.
Kimura, Shun; Kimura, Shojiro; Nishihara, Hiroshi; Kusamoto, Tetsuro; Chemical communications (Cambridge, England) 56 (2020) 11195–11198; doi:10.1039/d0cc04830e

data_7127152
_publ_section_title
;
 Excimer emission and magnetoluminescence of radical-based zinc(II)
 complexes doped in host crystals.
;
_journal_issue                   76
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11195
_journal_page_last               11198
_journal_paper_doi               10.1039/d0cc04830e
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         '2(C23 H8 Cl8 F6 N O2 Zn0.5)'
_chemical_formula_sum            'C46 H16 Cl16 F12 N2 O4 Zn'
_chemical_formula_weight         1521.18
_chemical_name_systematic        Zn(hfac)2(aH-PyBTM)2
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-05 deposited with the CCDC.	2020-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                97.411(4)
_cell_angle_beta                 94.728(4)
_cell_angle_gamma                90.909(5)
_cell_formula_units_Z            2
_cell_length_a                   8.9829(6)
_cell_length_b                   15.1174(8)
_cell_length_c                   20.8813(7)
_cell_measurement_reflns_used    8472
_cell_measurement_temperature    123
_cell_measurement_theta_max      31.3680
_cell_measurement_theta_min      2.6350
_cell_volume                     2801.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_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      4.00  45.00   0.25    4.16    --   12.59  57.00  30.00  164
  2  \w    -16.00  78.00   0.25    4.16    --   12.59  76.00 -38.00  376
  3  \w     40.00  91.00   0.25    4.16    --   12.59 179.00 -60.00  204
  4  \w     40.00  84.00   0.25    4.16    --   12.59 179.00 150.00  176
  5  \w    -78.00   9.00   0.25    4.16    --  -11.26 -57.00  30.00  348
  6  \w    -14.00  13.00   0.25    4.16    --   12.59 -99.00  90.00  108
  7  \w     46.00  82.00   0.25    4.16    --   12.59-179.00   0.00  144
  8  \w    -13.00  40.00   0.25    4.16    --   12.59 -76.00-164.00  212
  9  \w    -54.00 -16.00   0.25    4.16    --   12.59 -76.00-164.00  152
 10  \w    -87.00 -48.00   0.25    4.16    --  -11.26-179.00  60.00  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0138049000
_diffrn_orient_matrix_UB_12      -0.0444442000
_diffrn_orient_matrix_UB_13      0.0058577000
_diffrn_orient_matrix_UB_21      0.0469357000
_diffrn_orient_matrix_UB_22      0.0162596000
_diffrn_orient_matrix_UB_23      0.0281878000
_diffrn_orient_matrix_UB_31      -0.0623582000
_diffrn_orient_matrix_UB_32      0.0007865000
_diffrn_orient_matrix_UB_33      0.0187902000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34662
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.246
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.288
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.271
_refine_diff_density_min         -1.051
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         12845
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1285
_refine_ls_R_factor_gt           0.0792
_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^)+(0.1500P)^2^+0.3482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2202
_refine_ls_wR_factor_ref         0.2601
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7635
_reflns_number_total             12845
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04830e2.cif
_cod_data_source_block           aHPy-Zn
_cod_depositor_comments          'Adding full bibliography for 7127152.cif.'
_cod_database_code               7127152
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C46H16N2Cl16O4F12Zn
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.783
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Sof(C24B)=Sof(H24B)=1-FVAR(1)
 Sof(C24)=Sof(H24)=FVAR(1)
 Sof(C1B)=Sof(H1B)=1-FVAR(2)
 Sof(C1)=Sof(H1)=FVAR(2)
 Sof(F10)=Sof(F11)=Sof(F12)=1-FVAR(3)
 Sof(F11B)=Sof(F12B)=Sof(F10B)=FVAR(3)
 Sof(F8B)=Sof(F7B)=Sof(F9B)=1-FVAR(4)
 Sof(F8)=Sof(F9)=Sof(F7)=FVAR(4)
3.a Ternary CH refined with riding coordinates:
 C24(H24), C1(H1), C24B(H24B), C1B(H1B)
3.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C18(H18), C41(H41), C37(H37), C8(H8), C25(H25), C43(H43), C29(H29),
 C35(H35), C12(H12), C20(H20), C6(H6), C14(H14), C2(H2)
;
_shelx_res_checksum              34013
_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 1.733
_oxdiff_exptl_absorpt_empirical_full_min 0.570