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_1576292
_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 ab
_chemical_formula_moiety         'C16 H15 N3 O'
_chemical_formula_sum            'C16 H15 N3 O'
_chemical_formula_weight         265.31
_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             2024-06-20
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.02560(10)
_cell_length_b                   10.7811(4)
_cell_length_c                   24.3162(7)
_cell_measurement_reflns_used    3010
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      77.5600
_cell_measurement_theta_min      3.6360
_cell_volume                     1317.49(7)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_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     61.00  87.00   0.50    2.00    --    2.20  25.00 -41.00   52
  2  \w    141.00 167.00   0.50    7.00    --  106.30  25.00 -41.00   52
  3  \w     50.00  75.00   0.50    7.00    --  106.30 -25.00 154.00   50
  4  \w     82.00 140.00   0.50    7.00    --  106.30  25.00 -41.00  116
  5  \w    -16.00  49.00   0.50    2.00    --    2.20  77.00-150.00  130
  6  \w    -30.00  25.00   0.50    2.00    --    2.20  82.00 -30.00  110
  7  \w    -54.00 -29.00   0.50    2.00    --    2.20 -25.00 154.00   50
  8  \w    115.00 191.00   0.50    7.00    --  106.30  19.00  30.00  152
  9  \w     77.00 124.00   0.50    7.00    --  106.30 -77.00 -30.00   94
 10  \w     24.00  49.00   0.50    7.00    --  106.30 -77.00 -30.00   50
 11  \w     86.00 116.00   0.50    7.00    --  106.30  38.00-180.00   60
 12  \w     28.00 125.00   0.50    7.00    --  106.30 -57.00  30.00  194
 13  \w    -56.00 -31.00   0.50    2.00    --    0.90 -26.00 155.00   50
 14  \w    169.00 194.00   0.50    7.00    --  105.10  82.00  90.00   50
 15  \w    102.00 128.00   0.50    7.00    --  105.10  82.00  90.00   52
 16  \w     72.00  99.00   0.50    7.00    --  105.10 -26.00 155.00   54
 17  \w     34.00  81.00   0.50    7.00    --  105.10 -57.00 150.00   94
 18  \w     82.00 108.00   0.50    7.00    --  105.10 -57.00 150.00   52
 19  \w     69.00 112.00   0.50    7.00    --  105.10 -77.00  30.00   86
;
_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      -0.1020390000
_diffrn_orient_matrix_UB_12      -0.0260519000
_diffrn_orient_matrix_UB_13      0.0586217000
_diffrn_orient_matrix_UB_21      -0.2708586000
_diffrn_orient_matrix_UB_22      -0.0400120000
_diffrn_orient_matrix_UB_23      -0.0236484000
_diffrn_orient_matrix_UB_31      0.1008230000
_diffrn_orient_matrix_UB_32      -0.1347046000
_diffrn_orient_matrix_UB_33      -0.0042800000
_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  0.0520
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            7298
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.098
_diffrn_reflns_theta_min         3.635
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67465
_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    1.338
_exptl_crystal_description       needle
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 885 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2714
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0833P)^2^+0.2681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1410
_reflns_Friedel_coverage         0.662
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.940
_reflns_number_gt                2411
_reflns_number_total             2714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04965b2.cif
_cod_data_source_block           S_HL2
_cod_database_code               1576292
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'c n o h'
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C00A(H00A)
1.b Aromatic/amide H refined with riding coordinates:
 N003(H003), N004(H004), C006(H006), C008(H008), C00C(H00C), C00D(H00D),
 C00E(H00E), C00G(H00G), C00H(H00H), C00J(H00J), C00K(H00K)
1.c Idealised Me refined as rotating group:
 C00I(H00B,H00F,H00I)
;
_shelx_res_checksum              13201
_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 1.415
_oxdiff_exptl_absorpt_empirical_full_min 0.684