N-Heterocyclic carbene-stabilized gold-copper nanoclusters: synthesis, bonding and mechanochromism.
Zuo, Dongjie; Guo, Huifang; Xu, Qinghua; He, Ayisha; Li, Zilin; Li, Simin; Shen, Hui; Nanoscale 16 (2024) 20228–20234; doi:10.1039/d4nr03320e

data_1572813
_publ_section_title
;
 N-Heterocyclic carbene-stabilized gold-copper nanoclusters: synthesis,
 bonding and mechanochromism.
;
_journal_issue                   43
_journal_name_full               Nanoscale
_journal_page_first              20228
_journal_page_last               20234
_journal_paper_doi               10.1039/d4nr03320e
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety         'C53 H44 Au3.1 Cu0.9 N4'
_chemical_formula_sum            'C53 H44 Au3.1 Cu0.9 N4'
_chemical_formula_weight         1404.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-11-17 deposited with the CCDC.	2024-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.2160(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.30910(10)
_cell_length_b                   15.7826(2)
_cell_length_c                   25.6534(2)
_cell_measurement_reflns_used    22252
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.6340
_cell_measurement_theta_min      3.4920
_cell_volume                     4506.21(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.92a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.92a 64-bit (release 05-10-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.92a (Rigaku OD, 2023)'
_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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.954
_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     53.00  98.00   0.50    0.24    --  106.44-125.00-150.00   90
  2  \w     45.00  98.00   0.50    0.24    --  106.44 -95.00  30.00  106
  3  \w     45.00 100.00   0.50    0.24    --  106.44 -92.00 109.00  110
  4  \w     42.00  78.00   0.50    0.06    --   42.49 -92.00 109.00   72
  5  \w    -26.00  37.00   0.50    0.06    --   42.49 -92.00 109.00  126
  6  \w     32.00  67.00   0.50    0.24    --  106.44 -61.00   0.00   70
  7  \w     35.00  73.00   0.50    0.24    --  106.44 -61.00  30.00   76
  8  \w     35.00  72.00   0.50    0.24    --  106.44 -61.00 -60.00   74
  9  \w     34.00 106.00   0.50    0.24    --  106.44 -77.00 -90.00  144
 10  \w     38.00  67.00   0.50    0.24    --  106.44 -61.00-180.00   58
 11  \w     93.00 155.00   0.50    0.24    --  106.44  92.00-137.00  124
 12  \w    -24.00  37.00   0.50    0.06    --  -42.49  19.00 150.00  122
 13  \w    -22.00  37.00   0.50    0.06    --  -42.49  19.00-150.00  118
 14  \w     -4.00  22.00   0.50    0.06    --  -42.49  19.00-180.00   52
 15  \w    -77.00  29.00   0.50    0.06    --  -42.49  92.00-137.00  212
 16  \w    -81.00 -27.00   0.50    0.24    --  -99.00 125.00-120.00  108
 17  \w    -86.00 -60.00   0.50    0.24    --  -99.00  92.00-137.00   52
 18  \w    -66.00 -26.00   0.50    0.24    --  -99.00  61.00-180.00   80
 19  \w    -49.00 -24.00   0.50    0.24    --  -99.00  45.00-180.00   50
 20  \w    -49.00 -23.00   0.50    0.24    --  -99.00  45.00-150.00   52
 21  \w    -49.00 -24.00   0.50    0.24    --  -99.00  45.00-120.00   50
 22  \w    -49.00 -23.00   0.50    0.24    --  -99.00  45.00 -30.00   52
 23  \w    -48.00 -23.00   0.50    0.24    --  -99.00  45.00   0.00   50
 24  \w    -49.00 -24.00   0.50    0.24    --  -99.00  45.00  60.00   50
 25  \w    -49.00 -23.00   0.50    0.24    --  -99.00  45.00  90.00   52
 26  \w    -49.00 -24.00   0.50    0.24    --  -99.00  45.00 150.00   50
 27  \w   -172.00-110.00   0.50    0.24    --  -99.00 -92.00 109.00  124
;
_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      0.0313738000
_diffrn_orient_matrix_UB_12      0.0873159000
_diffrn_orient_matrix_UB_13      -0.0207055000
_diffrn_orient_matrix_UB_21      -0.0725802000
_diffrn_orient_matrix_UB_22      -0.0216892000
_diffrn_orient_matrix_UB_23      -0.0550447000
_diffrn_orient_matrix_UB_31      -0.1135920000
_diffrn_orient_matrix_UB_32      0.0378970000
_diffrn_orient_matrix_UB_33      0.0162670000
_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  0.0371
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            29993
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.033
_diffrn_reflns_theta_min         3.302
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.333
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.92a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_description       block
_exptl_crystal_F_000             2644
_refine_diff_density_max         2.270
_refine_diff_density_min         -2.367
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         8861
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+30.9860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0853
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8076
_reflns_number_total             8861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr03320e3.cif
_cod_data_source_block           zdj-au3cu-xqh_auto
_cod_depositor_comments          'Adding full bibliography for 1572813.cif.'
_cod_original_formula_sum        'C53 H44 Au3.10 Cu0.90 N4'
_cod_database_code               1572813
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.89
_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. Shared sites
{Au04, Cu04}
3. Uiso/Uaniso restraints and constraints
Uanis(C00U) \\sim Ueq, Uanis(C01K) \\sim Ueq, Uanis(C01N) \\sim Ueq,
Uanis(C01L) \\sim Ueq, Uanis(C00E) \\sim Ueq, Uanis(C010) \\sim Ueq,
Uanis(C00K) \\sim Ueq, Uanis(C00F) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(Au04) = Uanis(Cu04)
4. Others
 Fixed Sof: Au04(0.1) Cu04(0.9)
5.a Ternary CH refined with riding coordinates:
 C00I(H00I), C015(H015)
5.b Secondary CH2 refined with riding coordinates:
 C00V(H00E,H00F)
5.c Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00J(H00J), C00O(H00O), C00S(H00S), C00T(H00T), C00U(H00U),
 C00W(H00W), C00X(H00X), C00Z(H00Z), C010(H010), C013(H013), C014(H014),
 C016(H016), C017(H017), C019(H019), C01C(H01G), C01D(H01H), C01E(H01I),
 C01F(H01J), C01G(H01K), C01H(H01L), C01I(H01M), C01K(H01Q), C01L(H01R),
 C01M(H01S), C01N(H01T), C01O(H01U), C01P(H01V)
5.d Idealised Me refined as rotating group:
 C00P(H00B,H00C,H00D), C01A(H01A,H01B,H01C), C01B(H01D,H01E,H01F), C01J(H01N,
 H01O,H01P)
;
_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 2.962
_oxdiff_exptl_absorpt_empirical_full_min 0.623