Multinuclear Cu <sub><i>n</i></sub> S <sub><i>m</i></sub> clusters encapsulated by aromatic micelles as aqueous red-to-NIR phosphorescent ink.
Toyama, Kazuki; Tanaka, Yuya; Yoshizawa, Michito; Chemical science 16 (2025) 16751–16756; doi:10.1039/d5sc04122h

data_1575311
_publ_section_title
;
 Multinuclear Cu <sub><i>n</i></sub> S <sub><i>m</i></sub> clusters
 encapsulated by aromatic micelles as aqueous red-to-NIR phosphorescent
 ink.
;
_journal_issue                   36
_journal_name_full               'Chemical science'
_journal_page_first              16751
_journal_page_last               16756
_journal_paper_doi               10.1039/d5sc04122h
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C36 H36 Cu6 N6 S6'
_chemical_formula_sum            'C36 H36 Cu6 N6 S6'
_chemical_formula_weight         1126.37
_chemical_name_systematic        1c
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-01-30 deposited with the CCDC.	2025-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.2150(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.1291(3)
_cell_length_b                   9.53910(10)
_cell_length_c                   18.9461(3)
_cell_measurement_reflns_used    13737
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      74.2850
_cell_measurement_theta_min      4.6580
_cell_volume                     3988.55(9)
_computing_cell_refinement       'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      103(2)
_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 0.962
_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     12.00 116.00   0.50    0.05    --   41.30  77.00  90.00  208
  2  \w     19.00  46.00   0.50    0.05    --   41.30  57.00  30.00   54
  3  \w     16.00 121.00   0.50    0.05    --   41.30  26.00   9.00  210
  4  \w     80.00 178.00   0.50    0.06    --  105.51  26.00   9.00  196
  5  \w     12.00 116.00   0.50    0.05    --   41.30  77.00-180.00  208
  6  \w    -38.00  39.00   0.50    0.05    --   41.30 -26.00-153.00  154
  7  \w     30.00  56.00   0.50    0.06    --  105.51 -45.00-150.00   52
  8  \w     31.00  76.00   0.50    0.06    --  105.51 -61.00-150.00   90
  9  \w     30.00  56.00   0.50    0.06    --  105.51 -45.00-120.00   52
 10  \w     30.00  56.00   0.50    0.06    --  105.51 -45.00 -90.00   52
 11  \w     30.00  56.00   0.50    0.06    --  105.51 -45.00  90.00   52
 12  \w     30.00  56.00   0.50    0.06    --  105.51 -45.00 120.00   52
 13  \w     30.00  56.00   0.50    0.06    --  105.51 -45.00 150.00   52
 14  \w     31.00  76.00   0.50    0.06    --  105.51 -61.00 150.00   90
 15  \w     19.00  93.00   0.50    0.05    --   41.30-125.00 150.00  148
 16  \w     34.00 111.00   0.50    0.06    --  105.51-125.00 150.00  154
 17  \w    -24.00  39.00   0.50    0.05    --  -41.30  19.00  90.00  126
 18  \w    -28.00  38.00   0.50    0.05    --  -41.30  26.00   9.00  132
 19  \w    -97.00 -30.00   0.50    0.06    -- -104.00  77.00 -60.00  134
 20  \w    -66.00 -30.00   0.50    0.06    -- -104.00  61.00-150.00   72
 21  \w    -66.00 -30.00   0.50    0.06    -- -104.00  61.00-180.00   72
 22  \w    -66.00 -30.00   0.50    0.06    -- -104.00  61.00 -60.00   72
 23  \w    -66.00 -30.00   0.50    0.06    -- -104.00  61.00 -30.00   72
 24  \w    -66.00 -30.00   0.50    0.06    -- -104.00  61.00-120.00   72
 25  \w    -66.00 -30.00   0.50    0.06    -- -104.00  61.00   0.00   72
 26  \w    -66.00 -30.00   0.50    0.06    -- -104.00  61.00 150.00   72
 27  \w    -66.00 -30.00   0.50    0.06    -- -104.00  61.00 120.00   72
 28  \w   -112.00 -32.00   0.50    0.06    -- -104.00 125.00  30.00  160
 29  \w   -120.00 -16.00   0.50    0.05    --  -41.30 -26.00-153.00  208
 30  \w   -175.00 -78.00   0.50    0.06    -- -104.00 -26.00-153.00  194
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0628360000
_diffrn_orient_matrix_UB_12      0.0172137000
_diffrn_orient_matrix_UB_13      0.0288548000
_diffrn_orient_matrix_UB_21      -0.0301958000
_diffrn_orient_matrix_UB_22      -0.0524445000
_diffrn_orient_matrix_UB_23      -0.0710041000
_diffrn_orient_matrix_UB_31      0.0032301000
_diffrn_orient_matrix_UB_32      -0.1518408000
_diffrn_orient_matrix_UB_33      0.0277825000
_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  0.0284
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19053
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.010
_diffrn_reflns_theta_min         4.006
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.713
_exptl_absorpt_correction_T_max  0.511
_exptl_absorpt_correction_T_min  0.469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.125a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             2256
_exptl_crystal_preparation
'Recrystallized from CH2Cl2/Et2O at r.t.,Luminescent'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+6.7956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3676
_reflns_number_total             3944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04122h2.cif
_cod_data_source_block           1c
_cod_depositor_comments
'Adding full bibliography for 1575310--1575311.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1575311
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         Cu6S6N6C36H36
_shelx_estimated_absorpt_t_max   0.553
_shelx_estimated_absorpt_t_min   0.285
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C8(H8), C9(H9), C4(H4), C1(H1), C13(H13), C16(H16), C15(H15), C3(H3)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C12(H12A,H12B,H12C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              13632
_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 1.964
_oxdiff_exptl_absorpt_empirical_full_min 0.703