Circularly polarized luminescence and performance modulation of chiral europium-titanium (Eu<sub>2</sub>Ti<sub>4</sub>)-oxo clusters.
Liu, Wei-Dong; Li, Guan-Jun; Xu, Han; Deng, Yong-Kai; Du, Ming-Hao; Long, La-Sheng; Zheng, Lan-Sun; Kong, Xiang-Jian; Chemical communications (Cambridge, England) 59 (2023) 346–349; doi:10.1039/d2cc05816b

data_7131111
_publ_section_title
;
 Circularly polarized luminescence and performance modulation of chiral
 europium-titanium (Eu<sub>2</sub>Ti<sub>4</sub>)-oxo clusters.
;
_journal_issue                   3
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              346
_journal_page_last               349
_journal_paper_doi               10.1039/d2cc05816b
_journal_volume                  59
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C17 H18 N2'
_chemical_formula_sum            'C17 H18 N2'
_chemical_formula_weight         250.33
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-11-29 deposited with the CCDC.	2022-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.18570(10)
_cell_length_b                   9.95130(10)
_cell_length_c                   14.77970(10)
_cell_measurement_reflns_used    27089
_cell_measurement_temperature    100.0(8)
_cell_measurement_theta_max      75.0210
_cell_measurement_theta_min      2.9840
_cell_volume                     1351.01(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(8)
_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 0.980
_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  52.00   0.50    0.20    --   43.34  82.00 -96.00   82
  2  \w    103.00 128.00   0.50    0.60    --  109.59  82.00 -96.00   50
  3  \w     45.00  70.00   0.50    0.60    --  109.59 -61.00  90.00   50
  4  \w     40.00  69.00   0.50    0.60    --  109.59 -61.00  30.00   58
  5  \w     45.00 104.00   0.50    0.60    --  109.59 -77.00-180.00  118
  6  \w    -75.00  -6.00   0.50    0.20    --  -43.34  82.00 -96.00  138
  7  \w    -99.00 -74.00   0.50    0.60    --  -96.00  82.00 -96.00   50
  8  \w    -90.00 -51.00   0.50    0.60    --  -96.00 125.00  90.00   78
  9  \w      0.00  31.00   0.50    0.20    --  -43.34  82.00 -96.00   62
 10  \w   -100.00 -71.00   0.50    0.20    --  -43.34 -77.00   0.00   58
 11  \w   -102.00 -76.00   0.50    0.20    --  -43.34 -77.00  90.00   52
 12  \w    -71.00 -12.00   0.50    0.20    --  -43.34 -77.00  90.00  118
 13  \w    -73.00 -19.00   0.50    0.20    --  -43.34 -57.00  90.00  108
 14  \w    -66.00 -12.00   0.50    0.20    --  -43.34 -77.00   0.00  108
 15  \w   -117.00 -12.00   0.50    0.20    --  -43.34 -77.00-120.00  210
 16  \w   -111.00 -12.00   0.50    0.20    --  -43.34 -77.00 -60.00  198
 17  \w    -76.00 -19.00   0.50    0.20    --  -43.34 -57.00   0.00  114
 18  \w   -116.00 -54.00   0.50    0.20    --  -43.34 -57.00 150.00  124
 19  \w    -52.00 -24.00   0.50    0.20    --  -43.34 -57.00 150.00   56
 20  \w    -45.00 -18.00   0.50    0.20    --  -43.34 -37.00 150.00   54
 21  \w    -96.00 -60.00   0.50    0.20    --  -43.34 -37.00 150.00   72
 22  \w   -103.00 -65.00   0.50    0.60    --  -96.00 -79.00 173.75   76
 23  \w   -171.00-110.00   0.50    0.60    --  -96.00 -79.00 173.75  122
 24  \w   -170.00-127.00   0.50    0.60    --  -96.00 -77.00  90.00   86
 25  \w    -92.00 -66.00   0.50    0.60    --  -96.00 -77.00  90.00   52
 26  \w   -138.00-112.00   0.50    0.60    --  -96.00 -77.00  30.00   52
 27  \w   -147.00-111.00   0.50    0.60    --  -96.00 -77.00 120.00   72
 28  \w   -109.00 -66.00   0.50    0.60    --  -96.00 -77.00 120.00   86
 29  \w   -170.00 -65.00   0.50    0.60    --  -96.00 -77.00  45.99  210
 30  \w   -171.00 -65.00   0.50    0.60    --  -96.00 -77.00 -30.00  212
 31  \w    -96.00 -65.00   0.50    0.60    --  -96.00 -77.00-126.90   62
 32  \w   -170.00 -65.00   0.50    0.60    --  -96.00 -77.00-150.00  210
 33  \w   -168.00-128.00   0.50    0.60    --  -96.00 -77.00-126.90   80
 34  \w   -168.00-121.00   0.50    0.60    --  -96.00 -77.00-107.48   94
 35  \w   -126.00 -99.00   0.50    0.60    --  -96.00 -77.00-126.90   54
 36  \w   -170.00-104.00   0.50    0.60    --  -96.00 -77.00-180.00  132
 37  \w    -95.00 -66.00   0.50    0.60    --  -96.00 -77.00-180.00   58
 38  \w    -90.00 -65.00   0.50    0.60    --  -96.00 -77.00 -20.05   50
 39  \w    -92.00 -65.00   0.50    0.60    --  -96.00 -77.00  30.00   54
 40  \w   -113.00 -65.00   0.50    0.60    --  -96.00 -77.00 154.55   96
 41  \w   -171.00-122.00   0.50    0.60    --  -96.00 -77.00 154.55   98
 42  \w   -164.00-113.00   0.50    0.60    --  -96.00 -76.00  97.87  102
 43  \w   -101.00 -65.00   0.50    0.60    --  -96.00 -76.00  97.87   72
 44  \w   -168.00-128.00   0.50    0.60    --  -96.00 -76.00 -38.36   80
 45  \w   -170.00 -66.00   0.50    0.60    --  -96.00 -75.00 -91.27  208
 46  \w    -90.00 -65.00   0.50    0.60    --  -96.00 -77.00-107.48   50
 47  \w   -121.00 -66.00   0.50    0.60    --  -96.00 -76.00 -38.36  110
 48  \w    -96.00 -66.00   0.50    0.60    --  -96.00 -74.00 -13.70   60
 49  \w   -138.00 -67.00   0.50    0.60    --  -96.00 -72.00  -4.27  142
 50  \w   -154.00-127.00   0.50    0.60    --  -96.00 -72.00  57.38   54
 51  \w   -106.00 -67.00   0.50    0.60    --  -96.00 -72.00  57.38   78
 52  \w   -118.00 -68.00   0.50    0.60    --  -96.00 -69.00  68.21  100
 53  \w   -167.00-122.00   0.50    0.60    --  -96.00 -69.00  68.21   90
 54  \w   -152.00 -68.00   0.50    0.60    --  -96.00 -70.00 -76.53  168
 55  \w    -95.00 -70.00   0.50    0.60    --  -96.00 -61.00-180.00   50
 56  \w   -171.00 -69.00   0.50    0.60    --  -96.00 -67.00   1.17  204
 57  \w    -52.00 -10.00   0.50    0.20    --  -43.34 -82.00 141.00   84
 58  \w   -162.00 -63.00   0.50    0.60    --  -96.00 -82.00 141.00  198
 59  \w    -91.00 -63.00   0.50    0.60    --  -96.00 -81.00 -48.26   56
 60  \w   -124.00 -99.00   0.50    0.60    --  -96.00 -81.00 -48.26   50
 61  \w   -146.00-112.00   0.50    0.60    --  -96.00 -82.00-132.88   68
 62  \w   -103.00 -63.00   0.50    0.60    --  -96.00 -82.00-132.88   80
 63  \w    -88.00 -63.00   0.50    0.60    --  -96.00 -81.00 152.59   50
 64  \w     47.00  74.00   0.50    0.60    --  109.59 -82.00 141.00   54
 65  \w     53.00 116.00   0.50    0.60    --  109.59-125.00 120.00  126
 66  \w     84.00 116.00   0.50    0.60    --  109.59-125.00  60.00   64
 67  \w     50.00  76.00   0.50    0.60    --  109.59-125.00  60.00   52
 68  \w     59.00 110.00   0.50    0.60    --  109.59-125.00   0.00  102
 69  \w     77.00 113.00   0.50    0.60    --  109.59-125.00-120.00   72
 70  \w     70.00 115.00   0.50    0.60    --  109.59-125.00-150.00   90
 71  \w     36.00  62.00   0.50    0.60    --  109.59-125.00-150.00   52
 72  \w     36.00  99.00   0.50    0.60    --  109.59 -94.00 -90.00  126
 73  \w     35.00 108.00   0.50    0.60    --  109.59 -94.00   0.00  146
 74  \w     31.00  98.00   0.50    0.20    --   43.34-125.00  90.00  134
 75  \w     31.00  96.00   0.50    0.20    --   43.34-125.00  30.00  130
 76  \w     -3.00  42.00   0.50    0.20    --   43.34 -82.00 141.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0826702000
_diffrn_orient_matrix_UB_12      -0.0513343000
_diffrn_orient_matrix_UB_13      0.0838280000
_diffrn_orient_matrix_UB_21      0.0172096000
_diffrn_orient_matrix_UB_22      0.1455643000
_diffrn_orient_matrix_UB_23      0.0338457000
_diffrn_orient_matrix_UB_31      -0.1449029000
_diffrn_orient_matrix_UB_32      -0.0120219000
_diffrn_orient_matrix_UB_33      0.0518766000
_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  0.0235
_diffrn_reflns_av_unetI/netI     0.0085
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29776
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.079
_diffrn_reflns_theta_min         5.359
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       block
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.134
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 1091 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0398P)^2^+0.2456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0711
_reflns_Friedel_coverage         0.695
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.937
_reflns_number_gt                2669
_reflns_number_total             2680
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05816b2.cif
_cod_data_source_block           -pbpy
_cod_depositor_comments
'Adding full bibliography for 7131110--7131117.cif.'
_cod_database_code               7131111
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C22 N2'
_shelx_estimated_absorpt_t_max   0.873
_shelx_estimated_absorpt_t_min   0.807
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. 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
2.a Ternary CH refined with riding coordinates:
 C13(H13), C12(H12)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C17(H17A,H17B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C4(H4), C3(H3), C2(H2), C1(H1)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              98486
_shelx_hkl_checksum              75950
_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 1.311
_oxdiff_exptl_absorpt_empirical_full_min 0.660