Triple-Helical Aggregates of Copper(I) Cyclic Trinuclear Complexes for Circularly Polarized Luminescence
Huang, Guo-Quan; Yang, Hu; Xia, Ri-Qin; Wu, Kun; Huang, Yong-Liang; Hao, De-Bo; Li, Shun-Bo; Lu, Weigang; Zheng, Ji; Zhou, Xiao-Ping; Li, Dan; Chemical Science  (2025) –; doi:10.1039/D5SC04965B

data_1576289
_publ_section_title
;
 Triple-Helical Aggregates of Copper(I) Cyclic Trinuclear Complexes for
 Circularly Polarized Luminescence
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D5SC04965B
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C12 H13 N3 O'
_chemical_formula_sum            'C12 H13 N3 O'
_chemical_formula_weight         215.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-06-28
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-08-19 deposited with the CCDC.	2025-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.300(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.3639(3)
_cell_length_b                   5.08840(10)
_cell_length_c                   11.5646(3)
_cell_measurement_reflns_used    5775
_cell_measurement_temperature    100.01(16)
_cell_measurement_theta_max      77.3660
_cell_measurement_theta_min      3.7970
_cell_volume                     547.69(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(16)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_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     47.00  75.00   0.50    0.50    --   -2.20  38.00-150.00   56
  2  \w    -27.00  -1.00   0.50    0.50    --   -2.20 -38.00 150.00   52
  3  \w    -48.00 -17.00   0.50    0.50    --   -2.20 -77.00 -90.00   62
  4  \w    -92.00 -33.00   0.50    0.50    --   -2.20 -19.00  90.00  118
  5  \w    -45.00   1.00   0.50    0.50    --   -2.20 -77.00-150.00   92
  6  \w    -20.00  29.00   0.50    0.50    --   -2.20 -77.00-120.00   98
  7  \w    -31.00   7.00   0.50    0.50    --   -2.20  19.00-180.00   76
  8  \w    -29.00   3.00   0.50    0.50    --   -2.20  19.00   0.00   64
  9  \w     47.00  85.00   0.50    0.50    --   -2.20  38.00-120.00   76
 10  \w     -7.00  25.00   0.50    0.50    --   -2.20 -19.00  90.00   64
 11  \w     44.00  70.00   0.50    0.50    --   -2.20  19.00   0.00   52
 12  \w     33.00  64.00   0.50    0.50    --   -2.20  19.00-180.00   62
 13  \w    -17.00   8.00   0.50    0.50    --   -2.20 -38.00  60.00   50
 14  \w    -22.00  18.00   0.50    0.50    --   -2.20  38.00-120.00   80
 15  \w    -92.00 -67.00   0.50    0.50    --   -2.20 -38.00 150.00   50
 16  \w    -19.00  46.00   0.50    0.50    --    2.20  38.00  30.00  130
 17  \w     53.00  79.00   0.50    0.50    --    2.20  38.00  30.00   52
 18  \w    -67.00 -42.00   0.50    0.50    --    2.20 -57.00 120.00   50
 19  \w    168.00 194.00   0.50    0.50    --  106.30  57.00  60.00   52
 20  \w     82.00 109.00   0.50    0.50    --  106.30  57.00-120.00   54
 21  \w     78.00 111.00   0.50    0.50    --  106.30  70.00 -70.38   66
 22  \w     77.00 103.00   0.50    0.50    --  106.30  77.00  60.00   52
 23  \w     87.00 116.00   0.50    0.50    --  106.30  38.00-120.00   58
 24  \w     82.00 108.00   0.50    0.50    --  106.30  82.00  60.00   52
 25  \w     78.00 105.00   0.50    0.50    --  106.30  77.00 -90.00   54
 26  \w    120.00 196.00   0.50    0.50    --  106.30  72.00-166.99  152
 27  \w     88.00 155.00   0.50    0.50    --  106.30  38.00  60.00  134
 28  \w     84.00 109.00   0.50    0.50    --  106.30  57.00  60.00   50
 29  \w    146.00 194.00   0.50    0.50    --  106.30  38.00 -30.00   96
 30  \w     37.00  69.00   0.50    0.50    --  106.30 -77.00-150.00   64
 31  \w     76.00 102.00   0.50    0.50    --  106.30  73.00  13.61   52
 32  \w    122.00 148.00   0.50    0.50    --  106.30  57.00 150.00   52
 33  \w    147.00 173.00   0.50    0.50    --  106.30  77.00 -60.00   52
 34  \w     86.00 116.00   0.50    0.50    --  106.30  57.00 150.00   60
 35  \w     85.00 145.00   0.50    0.50    --  106.30  38.00  30.00  120
 36  \w     85.00 147.00   0.50    0.50    --  106.30  38.00 -90.00  124
 37  \w     17.00 131.00   0.50    0.50    --  106.30 -82.00 -60.00  228
 38  \w     77.00 105.00   0.50    0.50    --  106.30  72.00-166.99   56
 39  \w     85.00 118.00   0.50    0.50    --  106.30  38.00-150.00   66
 40  \w    163.00 189.00   0.50    0.50    --  106.30  57.00 -90.00   52
 41  \w     90.00 184.00   0.50    0.50    --  106.30  38.00-180.00  188
 42  \w     77.00 105.00   0.50    0.50    --  106.30  77.00 -60.00   56
 43  \w     85.00 123.00   0.50    0.50    --  106.30  38.00 120.00   76
 44  \w     76.00 102.00   0.50    0.50    --  106.30  77.00  30.00   52
 45  \w     52.00 110.00   0.50    0.50    --  106.30 -77.00  60.00  116
 46  \w     89.00 127.00   0.50    0.50    --  106.30  38.00 -60.00   76
 47  \w     82.00 108.00   0.50    0.50    --  106.30  57.00 -90.00   52
 48  \w     77.00 103.00   0.50    0.50    --  106.30  76.00 165.68   52
 49  \w     76.00 101.00   0.50    0.50    --  106.30  77.00 120.00   50
 50  \w    132.00 195.00   0.50    0.50    --  106.30  77.00 120.00  126
 51  \w     18.00 140.00   0.50    0.50    --  106.30 -82.00 120.00  244
 52  \w     79.00 106.00   0.50    0.50    --  106.30  77.00 150.00   54
 53  \w     75.00 109.00   0.50    0.50    --  106.30 -77.00-150.00   68
 54  \w    139.00 164.00   0.50    0.50    --  106.30  70.00 -70.38   50
 55  \w    159.00 185.00   0.50    0.50    --  106.30  73.00  13.61   52
 56  \w     86.00 118.00   0.50    0.50    --  106.30  38.00 150.00   64
 57  \w     78.00 104.00   0.50    0.50    --  106.30  77.00  90.00   52
 58  \w     96.00 142.00   0.50    0.50    --  106.30  38.00 -30.00   92
 59  \w    158.00 184.00   0.50    0.50    --  106.30  50.00  -9.63   52
 60  \w     85.00 128.00   0.50    0.50    --  106.30  38.00   0.00   86
 61  \w     92.00 152.00   0.50    0.50    --  106.30  38.00  90.00  120
 62  \w     86.00 112.00   0.50    0.50    --  106.30  50.00  -9.63   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1174802000
_diffrn_orient_matrix_UB_12      -0.1950611000
_diffrn_orient_matrix_UB_13      -0.0483800000
_diffrn_orient_matrix_UB_21      0.0033774000
_diffrn_orient_matrix_UB_22      0.1166993000
_diffrn_orient_matrix_UB_23      -0.1226233000
_diffrn_orient_matrix_UB_31      0.1165550000
_diffrn_orient_matrix_UB_32      -0.1998953000
_diffrn_orient_matrix_UB_33      -0.0243283000
_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  0.0430
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9080
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.453
_diffrn_reflns_theta_min         3.846
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       needle
_exptl_crystal_F_000             228
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.148
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 898 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.15(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2284
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0507P)^2^+0.1258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1011
_reflns_Friedel_coverage         0.764
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.949
_reflns_number_gt                2166
_reflns_number_total             2284
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04965b2.cif
_cod_data_source_block           R_HL1
_cod_database_code               1576289
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N H O'
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C00A(H00A)
1.b Aromatic/amide H refined with riding coordinates:
 N002(H002), N004(H004), C005(H005), C009(H009), C00C(H00E), C00D(H00F),
 C00E(H00G), C00F(H00H), C00G(H00I)
1.c Idealised Me refined as rotating group:
 C00B(H00B,H00C,H00D)
;
_shelx_res_checksum              65442
_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 4.161
_oxdiff_exptl_absorpt_empirical_full_min 0.686