#------------------------------------------------------------------------------
#$Date: 2025-08-05 01:18:24 +0300 (Tue, 05 Aug 2025) $
#$Revision: 301457 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/53/1575310.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1575310
loop_
_publ_author_name
'Toyama, Kazuki'
'Tanaka, Yuya'
'Yoshizawa, Michito'
_publ_section_title
;
 Multinuclear CunSm Clusters Encapsulated by Aromatic Micelles as Aqueous
 Red-to-NIR Phosphorescent Ink
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D5SC04122H
_journal_year                    2025
_chemical_formula_moiety         'C36 H36 Cu6 N6 S6'
_chemical_formula_sum            'C36 H36 Cu6 N6 S6'
_chemical_formula_weight         1126.31
_chemical_name_systematic        1a
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-01-30
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   12.5474(2)
_cell_length_b                   12.5474(2)
_cell_length_c                   21.7649(3)
_cell_measurement_reflns_used    8113
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      76.3490
_cell_measurement_theta_min      4.4930
_cell_volume                     2967.53(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.107a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.107a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.107a (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 0.995
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     31.00  63.00   0.50    0.05    --  102.75 -51.00 140.00   64
  2  ω     31.00 115.00   0.50    0.05    --  102.75  -3.00 -80.00  168
  3  ω     94.00 174.00   0.50    0.05    --  102.75  45.00  60.00  160
  4  ω     55.00 157.00   0.50    0.05    --  102.75 162.00-134.00  204
  5  ω     55.00 157.00   0.50    0.05    --  102.75 162.00-134.00  204
  6  ω    -24.00  26.00   0.50    0.05    --  -47.66  19.00   0.00  100
  7  ω    -24.00  26.00   0.50    0.05    --  -47.66  19.00 -60.00  100
  8  ω    -24.00  26.00   0.50    0.05    --  -47.66  19.00 -90.00  100
  9  ω    -66.00 -31.00   0.50    0.05    -- -102.75  61.00 -30.00   70
 10  ω    -66.00 -31.00   0.50    0.05    -- -102.75  61.00 -60.00   70
 11  ω    -66.00 -31.00   0.50    0.05    -- -102.75  61.00-120.00   70
 12  ω   -175.00 -94.00   0.50    0.05    -- -102.75 -15.00-150.00  162
 13  ω   -175.00 -94.00   0.50    0.05    -- -102.75 -15.00-150.00  162
 14  ω   -119.00 -67.00   0.50    0.05    --  -47.66-137.00 -89.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0444759000
_diffrn_orient_matrix_UB_12      -0.0742210000
_diffrn_orient_matrix_UB_13      -0.0377253000
_diffrn_orient_matrix_UB_21      0.0254723000
_diffrn_orient_matrix_UB_22      -0.0489984000
_diffrn_orient_matrix_UB_23      0.0598858000
_diffrn_orient_matrix_UB_31      -0.1320578000
_diffrn_orient_matrix_UB_32      -0.1105474000
_diffrn_orient_matrix_UB_33      -0.0012011000
_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  0.0268
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6369
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.279
_diffrn_reflns_theta_min         5.754
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.767
_exptl_absorpt_correction_T_max  0.323
_exptl_absorpt_correction_T_min  0.258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.107a (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    1.891
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             1692
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.522
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.225
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1354
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.225
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0505
_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/[σ²(Fo²)+(0.0552P)²+40.2249P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1364
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1344
_reflns_number_total             1354
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5sc04122h2.cif
_cod_data_source_block           1a
_cod_original_cell_volume        2967.53(10)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1575310
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         CuSNCH
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.345
_shelx_estimated_absorpt_t_min   0.345
_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:
 C2(H2), C4(H4), C3(H3)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_shelx_res_file
;
TITL kt422-1_cu6s6me_auto_a.res in R-3
    kt422-1_cu6s6me_auto.res
    created by SHELXL-2019/3 at 19:59:08 on 30-Jan-2025
REM Old TITL kt422-1_cu6s6me_auto_a.res in R-3
REM SHELXT solution in R-3: R1 0.069, Rweak 0.007, Alpha 0.043
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C6 Cu N S
CELL 1.54184 12.5474 12.5474 21.7649 90 90 120
ZERR 3 0.0002 0.0002 0.0003 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H Cu N S
UNIT 108 108 18 18 18

L.S. 10
PLAN  1
SIZE 0.2 0.2 0.2
TEMP -170(2)
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%./KT422-1_Cu6S6Me_auto.hkl">
REM </olex2.extras>

WGHT    0.055200   40.224903
FVAR       0.18523
CU1   3    0.374718    0.538442    0.714483    11.00000    0.01932    0.02048 =
         0.01831   -0.00082   -0.00014    0.00922
S1    5    0.378806    0.524385    0.574111    11.00000    0.01983    0.02107 =
         0.01739   -0.00089    0.00085    0.01005
N1    4    0.416600    0.420986    0.672651    11.00000    0.01464    0.01777 =
         0.02397   -0.00235   -0.00168    0.00672
C2    1    0.448494    0.347966    0.575850    11.00000    0.01684    0.02211 =
         0.02920   -0.00301    0.00365    0.00764
AFIX  43
H2    2    0.448066    0.350438    0.532230    11.00000   -1.20000
AFIX   0
C1    1    0.416804    0.421740    0.610540    11.00000    0.01569    0.01929 =
         0.02333   -0.00019    0.00191    0.00580
C5    1    0.447763    0.344815    0.702500    11.00000    0.01615    0.01960 =
         0.03335    0.00004   -0.00253    0.00723
C4    1    0.480119    0.269750    0.669814    11.00000    0.01765    0.02132 =
         0.03909    0.00262   -0.00112    0.01177
AFIX  43
H4    2    0.501996    0.217348    0.691086    11.00000   -1.20000
AFIX   0
C6    1    0.446740    0.349030    0.770507    11.00000    0.03520    0.02941 =
         0.03516    0.00461   -0.00729    0.01634
AFIX 137
H6A   2    0.492716    0.434841    0.784249    11.00000   -1.50000
H6B   2    0.485229    0.303819    0.787162    11.00000   -1.50000
H6C   2    0.361598    0.311220    0.785099    11.00000   -1.50000
AFIX   0
C3    1    0.480278    0.271797    0.606109    11.00000    0.01822    0.02705 =
         0.04902   -0.00896    0.00223    0.01124
AFIX  43
H3    2    0.502234    0.220835    0.583527    11.00000   -1.20000
AFIX   0
HKLF 4




REM  kt422-1_cu6s6me_auto_a.res in R-3
REM wR2 = 0.1364, GooF = S = 1.225, Restrained GooF = 1.225 for all data
REM R1 = 0.0505 for 1344 Fo > 4sig(Fo) and 0.0507 for all 1354 data
REM 83 parameters refined using 0 restraints

END

WGHT      0.0552     40.2243

REM Highest difference peak  2.522,  deepest hole -0.890,  1-sigma level  0.134
Q1    1   0.3896  0.5435  0.6181  11.00000  0.05    2.52
;
_shelx_res_checksum              47263
_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 1.637
_oxdiff_exptl_absorpt_empirical_full_min 0.715
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.37472(6) 0.53844(6) 0.71448(3) 0.0197(3) Uani 1 1 d . . . . .
S1 S 0.37881(9) 0.52439(9) 0.57411(5) 0.0195(3) Uani 1 1 d . . . . .
N1 N 0.4166(3) 0.4210(3) 0.67265(16) 0.0194(7) Uani 1 1 d . . . . .
C2 C 0.4485(4) 0.3480(4) 0.5759(2) 0.0236(9) Uani 1 1 d . . . . .
H2 H 0.448066 0.350438 0.532230 0.028 Uiso 1 1 calc R U . . .
C1 C 0.4168(4) 0.4217(4) 0.6105(2) 0.0207(8) Uani 1 1 d . . . . .
C5 C 0.4478(4) 0.3448(4) 0.7025(2) 0.0238(9) Uani 1 1 d . . . . .
C4 C 0.4801(4) 0.2697(4) 0.6698(2) 0.0251(10) Uani 1 1 d . . . . .
H4 H 0.501996 0.217348 0.691086 0.030 Uiso 1 1 calc R U . . .
C6 C 0.4467(5) 0.3490(5) 0.7705(2) 0.0332(11) Uani 1 1 d . . . . .
H6A H 0.492716 0.434841 0.784249 0.050 Uiso 1 1 calc R U . . .
H6B H 0.485229 0.303819 0.787162 0.050 Uiso 1 1 calc R U . . .
H6C H 0.361598 0.311220 0.785099 0.050 Uiso 1 1 calc R U . . .
C3 C 0.4803(4) 0.2718(5) 0.6061(3) 0.0315(11) Uani 1 1 d . . . . .
H3 H 0.502234 0.220835 0.583527 0.038 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0193(4) 0.0205(4) 0.0183(4) -0.0008(2) -0.0001(2) 0.0092(3)
S1 0.0198(5) 0.0211(5) 0.0174(5) -0.0009(4) 0.0009(3) 0.0101(4)
N1 0.0146(16) 0.0178(17) 0.0240(17) -0.0023(14) -0.0017(13) 0.0067(14)
C2 0.017(2) 0.022(2) 0.029(2) -0.0030(17) 0.0037(16) 0.0076(17)
C1 0.0157(19) 0.019(2) 0.023(2) -0.0002(16) 0.0019(16) 0.0058(16)
C5 0.0161(19) 0.020(2) 0.033(2) 0.0000(17) -0.0025(17) 0.0072(17)
C4 0.018(2) 0.021(2) 0.039(3) 0.0026(19) -0.0011(18) 0.0118(18)
C6 0.035(3) 0.029(2) 0.035(3) 0.005(2) -0.007(2) 0.016(2)
C3 0.018(2) 0.027(2) 0.049(3) -0.009(2) 0.002(2) 0.0112(19)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cu1 Cu1 Cu1 71.96(3) 15_556 14_456 ?
S1 Cu1 Cu1 72.97(3) 14_456 14_456 ?
S1 Cu1 Cu1 73.06(3) 15_556 15_556 ?
S1 Cu1 Cu1 131.90(3) 14_456 15_556 ?
S1 Cu1 Cu1 132.04(3) 15_556 14_456 ?
S1 Cu1 S1 109.72(6) 15_556 14_456 ?
N1 Cu1 Cu1 88.89(10) . 14_456 ?
N1 Cu1 Cu1 87.68(11) . 15_556 ?
N1 Cu1 S1 123.36(11) . 14_456 ?
N1 Cu1 S1 121.28(11) . 15_556 ?
Cu1 S1 Cu1 95.17(5) 14_456 15_556 ?
C1 S1 Cu1 104.50(15) . 15_556 ?
C1 S1 Cu1 106.74(14) . 14_456 ?
C1 N1 Cu1 116.6(3) . . ?
C1 N1 C5 118.7(4) . . ?
C5 N1 Cu1 124.7(3) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
C3 C2 C1 118.7(4) . . ?
N1 C1 S1 116.9(3) . . ?
N1 C1 C2 122.4(4) . . ?
C2 C1 S1 120.6(3) . . ?
N1 C5 C4 120.9(4) . . ?
N1 C5 C6 116.1(4) . . ?
C4 C5 C6 123.0(4) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 C5 119.8(4) . . ?
C3 C4 H4 120.1 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C2 C3 C4 119.6(4) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 Cu1 2.8329(10) 15_556 ?
Cu1 Cu1 2.8330(10) 14_456 ?
Cu1 S1 2.2574(12) 14_456 ?
Cu1 S1 2.2513(12) 15_556 ?
Cu1 N1 2.013(4) . ?
S1 C1 1.769(5) . ?
N1 C1 1.352(6) . ?
N1 C5 1.365(6) . ?
C2 H2 0.9500 . ?
C2 C1 1.398(6) . ?
C2 C3 1.374(7) . ?
C5 C4 1.393(6) . ?
C5 C6 1.481(7) . ?
C4 H4 0.9500 . ?
C4 C3 1.387(8) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C3 H3 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 S1 C1 N1 -48.8(3) 14_456 . . . ?
Cu1 S1 C1 N1 51.3(3) 15_556 . . . ?
Cu1 S1 C1 C2 -127.1(3) 15_556 . . . ?
Cu1 S1 C1 C2 132.9(3) 14_456 . . . ?
Cu1 N1 C1 S1 -0.6(4) . . . . ?
Cu1 N1 C1 C2 177.7(3) . . . . ?
Cu1 N1 C5 C4 -177.5(3) . . . . ?
Cu1 N1 C5 C6 1.6(5) . . . . ?
N1 C5 C4 C3 -0.3(6) . . . . ?
C1 N1 C5 C4 0.5(6) . . . . ?
C1 N1 C5 C6 179.5(4) . . . . ?
C1 C2 C3 C4 0.1(7) . . . . ?
C5 N1 C1 S1 -178.7(3) . . . . ?
C5 N1 C1 C2 -0.4(6) . . . . ?
C5 C4 C3 C2 0.0(7) . . . . ?
C6 C5 C4 C3 -179.3(4) . . . . ?
C3 C2 C1 S1 178.4(3) . . . . ?
C3 C2 C1 N1 0.2(7) . . . . ?
