Eight-electron copper-hydride nanoclusters: synthesis, structure, alloying chemistry and photoluminescence
Sun, Jing; Liu, Jiahe; Su, Hai-Feng; Li, Simin; Tang, Xiongkai; Xie, Zhenlang; Xu, Zhen; Jiang, Wenya; Wei, Jianyu; Gong, Xuekun; He, Ayisha; Wang, Song; Jiang, De-en; Zheng, Nanfeng; Shen, Hui; Chemical Science 16 (2025) 6392–6401; doi:10.1039/D4SC08547G

data_1574112
_publ_section_title
;
 Eight-electron copper-hydride nanoclusters: synthesis, structure,
 alloying chemistry and photoluminescence
;
_journal_issue                   15
_journal_name_full               'Chemical Science'
_journal_page_first              6392
_journal_page_last               6401
_journal_paper_doi               10.1039/D4SC08547G
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety
'C204 H150 Cu47 F36 O24 P5 Se15, 1.5(C2 H4 Cl4)'
_chemical_formula_sum            'C207 H156 Cl6 Cu47 F36 O24 P5 Se15'
_chemical_formula_weight         8249.64
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-11-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-11-12 deposited with the CCDC.	2025-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   21.8398(5)
_cell_length_b                   21.8398(5)
_cell_length_c                   33.3259(5)
_cell_measurement_reflns_used    11804
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      75.4930
_cell_measurement_theta_min      2.6330
_cell_volume                     13766.1(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.92a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.92a (Rigaku OD, 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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.936
_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    -21.00  26.00   0.50    0.20    --  -47.96  11.00-128.00   94
  2  \w   -166.00 -95.00   0.50    1.74    --  -99.00-120.00-115.00  142
  3  \w   -167.00 -99.00   0.50    1.74    --  -99.00 -99.00  30.00  136
  4  \w     -5.00  27.00   0.50    0.20    --  -47.96  19.00 -60.00   64
  5  \w    -71.00 -45.00   0.50    0.20    --  -47.96 125.00 -56.00   52
  6  \w     35.00 101.00   0.50    1.74    --  105.22 -99.00 -60.00  132
  7  \w     93.50  99.00   0.50    1.74    --  105.22 -99.00 -30.00   11
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            30008
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.677
_diffrn_reflns_theta_min         2.336
_exptl_absorpt_coefficient_mu    7.487
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72118
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.990
_exptl_crystal_description       block
_exptl_crystal_F_000             7928
_refine_diff_density_max         1.654
_refine_diff_density_min         -1.702
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         9230
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0552
_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^)+(0.1003P)^2^+41.2904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7223
_reflns_number_total             9230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08547g2.cif
_cod_data_source_block           sj-cu47_auto
_cod_depositor_comments
'Adding full bibliography for 1574111--1574112.cif.'
_cod_original_cell_volume        13766.0(6)
_cod_database_code               1574112
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(Cl2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
3. Others
 Fixed Sof: H2A(0.5) H2B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C00X(H00X), C00Y(H00Y), C00Z(H00Z), C011(H011), C012(H012), C014(H014),
 C015(H015), C017(H017), C018(H018), C019(H019), C01A(H01A), C01C(H01C),
 C01D(H01D), C01E(H01E), C01F(H01F), C01G(H01G), C01I(H01I), C01J(H01J),
 C01K(H01K), C01L(H01L), C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P),
 C01Q(H01Q), C01R(H01R)
;
_shelx_res_checksum              47122
_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
;