Chiral copper-hydride nanoclusters: synthesis, structure, and assembly.
Wang, Lin; Yan, Xiaodan; Tian, Guolong; Xie, Zhenlang; Shi, Shanshan; Zhang, Yuhao; Li, Simin; Sun, Xueli; Sun, Jing; He, Jinlu; Shen, Hui; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d2dt03788b

data_7712386
_publ_section_title
;
 Chiral copper-hydride nanoclusters: synthesis, structure, and assembly.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt03788b
_journal_year                    2023
_chemical_formula_moiety
'C138 H142 Cu14 P7 S3, 1.5[CH3OH], 2[(CH3CH2)2O]'
_chemical_formula_sum            'C147.5 H152 Cu14 O5.5 P7 S3'
_chemical_formula_weight         3215.21
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc2ddx2t
_audit_creation_date             2022-11-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2022-12-24 deposited with the CCDC.	2023-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   17.6260(3)
_cell_length_b                   17.6260(3)
_cell_length_c                   154.6133(19)
_cell_measurement_reflns_used    17773
_cell_measurement_temperature    99.8(9)
_cell_measurement_theta_max      65.4930
_cell_measurement_theta_min      2.9420
_cell_volume                     41599.2(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -42.00  35.00   0.50    2.50    --  -43.22  37.00-150.00  154
  2  \w   -113.00 -74.00   0.50    2.50    --  -43.22-125.00 120.00   78
  3  \w    -73.00  28.00   0.50    2.50    --  -43.22  77.00  90.00  202
  4  \w     -9.00  17.00   0.50    2.50    --   45.10 -19.00-120.00   52
  5  \w     10.00  42.00   0.50    2.50    --   45.10 -37.00-150.00   64
  6  \w    -34.00  25.00   0.50    2.50    --   45.10 -19.00 -60.00  118
  7  \w    -32.00   0.00   0.50    2.50    --   45.10 -19.00  30.00   64
  8  \w    -35.00  -9.00   0.50    8.00    --  -88.32  30.00 -60.00   52
  9  \w   -105.00 -60.00   0.50    8.00    --  -88.32  77.00 -60.00   90
 10  \w    -35.00 -10.00   0.50    8.00    --  -88.32  30.00-120.00   50
 11  \w    -35.00 -10.00   0.50    8.00    --  -88.32  30.00 -90.00   50
 12  \w    -51.00 -23.00   0.50    8.00    --  -88.32  45.00  90.00   56
 13  \w    -47.00 -20.00   0.50    8.00    --  -88.32  61.00  90.00   54
 14  \w   -165.00 -71.00   0.50    8.00    --  -88.32 -45.00   0.00  188
 15  \w   -164.00-135.00   0.50    8.00    --  -88.32 -94.00 -30.00   58
 16  \w   -105.00 -59.00   0.50    8.00    --  -88.32  77.00-120.00   92
 17  \w    -43.00 -12.00   0.50    8.00    --  -88.32  45.00 150.00   62
 18  \w    -52.00 -26.00   0.50    8.00    --  -88.32  77.00-120.00   52
 19  \w   -121.00 -85.00   0.50    8.00    --  -88.32 -94.00 -30.00   72
 20  \w    -90.00 -64.00   0.50    8.00    --  -88.32 125.00  60.00   52
 21  \w    -50.00 -14.00   0.50    8.00    --  -88.32 125.00  60.00   72
 22  \w     14.00 106.00   0.50    8.00    --   90.19 -94.00 -30.00  184
 23  \w    133.00 162.00   0.50    8.00    --   90.19 125.00  30.00   58
 24  \w     19.00  45.00   0.50    8.00    --   90.19 -45.00 -30.00   52
 25  \w     14.00  39.00   0.50    8.00    --   90.19 -45.00 150.00   50
 26  \w     92.00 117.00   0.50    8.00    --   90.19-125.00  30.00   50
 27  \w     67.00 100.00   0.50    8.00    --   90.19 -94.00 120.00   66
 28  \w     67.00 107.00   0.50    8.00    --   90.19-125.00  90.00   80
 29  \w     31.00  57.00   0.50    8.00    --   90.19-125.00  90.00   52
 30  \w     34.00  59.00   0.50    8.00    --   90.19 -61.00 120.00   50
 31  \w     13.00  38.00   0.50    8.00    --   90.19 -45.00 120.00   50
 32  \w     33.00  59.00   0.50    8.00    --   90.19-125.00  30.00   52
 33  \w     22.00  57.00   0.50    8.00    --   90.19 -61.00 -60.00   70
 34  \w     32.00 171.00   0.50    8.00    --   90.19  15.00 -90.00  278
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       182
_diffrn_reflns_limit_l_min       -178
_diffrn_reflns_number            116089
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.084
_diffrn_reflns_theta_max         66.084
_diffrn_reflns_theta_min         2.951
_exptl_absorpt_coefficient_mu    3.856
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       block
_exptl_crystal_F_000             19680
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.238
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         8043
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+155.9336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7309
_reflns_number_total             8043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03788b2.cif
_cod_data_source_block           cu14
_cod_original_cell_volume        41599.2(15)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'C147.50 H152 Cu14 O5.50 P7 S3'
_cod_database_code               7712386
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.699
_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. Restrained distances
 Cu2-HA \\sim Cu3-HA \\sim Cu1-HA
 with sigma of 0.02
 Cu1-HB \\sim Cu4-HB
 with sigma of 0.02
 Cu5-HC \\sim Cu5-H
 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C36(H36), C42(H42), C38(H38), C41(H41), C2(H2), C30(H30), C3(H3),
 C26(H26), C35(H35), C40(H40), C14(H14), C23(H23), C18(H18), C6(H6), C4(H4),
 C32(H32), C20(H20), C12(H12), C34(H34), C16(H16), C29(H29), C39(H39), C33(H33),
  C27(H27), C17(H17), C8(H8), C28(H28), C15(H15), C5(H5), C11(H11), C22(H22),
 C21(H21), C10(H10), C9(H9)
3.b Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C46(H46A,H46B,H46C), C45(H45A,H45B,H45C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              62296
_shelx_fab_checksum              86413
_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
;