Size disproportionation among nanocluster transformations.
Zhu, Chen; Lu, Luyao; Li, Fei; Kang, Xi; Zhu, Manzhou; Chemical science 15 (2024) 16637–16644; doi:10.1039/d4sc04884a

data_1572632
_publ_section_title
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 Size disproportionation among nanocluster transformations.
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_journal_issue                   40
_journal_name_full               'Chemical science'
_journal_page_first              16637
_journal_page_last               16644
_journal_paper_doi               10.1039/d4sc04884a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety
'C372 H255 Ag27 Au2 Cl11 Cu27 F90 P9 S33, Cu, 3(Cl)'
_chemical_formula_sum            'C372 H255 Ag27 Au2 Cl14 Cu28 F90 P9 S33'
_chemical_formula_weight         13353.30
_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
_audit_creation_date             2024-05-14
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
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_audit_update_record
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2024-07-12 deposited with the CCDC.	2024-09-16 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 91.097(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   41.4184(15)
_cell_length_b                   29.7952(15)
_cell_length_c                   47.331(2)
_cell_measurement_reflns_used    18370
_cell_measurement_temperature    120
_cell_measurement_theta_max      67.59
_cell_measurement_theta_min      5.86
_cell_volume                     58399(4)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)
;
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details      '949 frames, detector distance = 60 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.1062
_diffrn_reflns_av_unetI/netI     0.2686
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            229084
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        62.500
_diffrn_reflns_theta_max         62.500
_diffrn_reflns_theta_min         5.803
_exptl_absorpt_coefficient_mu    11.528
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             25748
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.662
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.713
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     4516
_refine_ls_number_reflns         90602
_refine_ls_number_restraints     9509
_refine_ls_restrained_S_all      0.735
_refine_ls_R_factor_all          0.1678
_refine_ls_R_factor_gt           0.0708
_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^)+(0.0862P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1744
_refine_ls_wR_factor_ref         0.2025
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25326
_reflns_number_total             90602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04884a2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
'Adding full bibliography for 1572629--1572632.cif.'
_cod_original_cell_volume        58399(5)
_cod_database_code               1572632
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.459
_shelx_estimated_absorpt_t_min   0.338
_olex2_refinement_description
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1. Restrained distances
 C1_31-P1_31
 1.9 with sigma of 0.01
 P1_31-C6_31
 2.7 with sigma of 0.01
2. Restrained planarity
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(Cl12) \\sim Ueq, Uanis(Cl11) \\sim Ueq, Uanis(Cl9) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
: with sigma of 0.015 and sigma for terminal atoms of 0.03
4.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C3(H3), C2(H2), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2),
 C3(H3), C5(H5), C6(H6), C6(H6), C5(H5), C3(H3), C2(H2), C6(H6), C5(H5), C3(H3),
  C2(H2), C3(H3), C2(H2), C6(H6), C5(H5), C6(H6), C5(H5), C3(H3), C2(H2),
 C6(H6), C5(H5), C3(H3), C2(H2), C3(H3), C2(H2), C6(H6), C5(H5), C5(H5), C3(H3),
  C2(H2), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5),
 C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2),
  C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C6(H6), C5(H5),
 C3(H3), C2(H2), C6(H6), C2(H2), C3(H3), C5(H5), C2(H2), C3(H3), C5(H5), C6(H6),
  C6(H6), C5(H5), C3(H3), C2(H2), C6(H6), C5(H5), C3(H3), C2(H2), C2(H2),
 C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C6(H6), C5(H5), C3(H3),
  C2(H2), C6(H6), C2(H2), C3(H3), C5(H5), C2(H2), C6(H6), C5(H5), C3(H3),
 C2(H2), C3(H3), C5(H5), C6(H6), C6(H6), C5(H5), C3(H3), C2(H2), C2(H2), C6(H6),
  C5(H5), C3(H3), C12(H12), C11(H11), C10(H10), C9(H9), C8(H8), C18(H18),
 C17(H17), C16(H16), C15(H15), C14(H14), C6(H6), C5(H5), C4(H4), C3(H3), C2(H2),
  C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C10(H10), C9(H9), C8(H8),
 C12(H12), C11(H11), C6(H6), C2(H2), C3(H3), C4(H4), C5(H5), C18(H18), C17(H17),
  C16(H16), C15(H15), C14(H14), C6(H6), C2(H2), C3(H3), C4(H4), C5(H5), C8(H8),
 C9(H9), C10(H10), C11(H11), C12(H12), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6),
 C16(H16), C17(H17), C18(H18), C14(H14), C15(H15), C9(H9), C8(H8), C12(H12),
 C11(H11), C10(H10), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C6(H6),
 C2(H2), C3(H3), C4(H4), C5(H5), C11(H11), C10(H10), C9(H9), C8(H8), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C8(H8), C9(H9), C10(H10),
 C11(H11), C12(H12), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C2(H2), C6(H6),
 C5(H5), C4(H4), C3(H3), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14),
  C15(H15), C16(H16), C17(H17), C18(H18), C6(H6), C5(H5), C4(H4), C3(H3),
 C2(H2), C12(H12), C8(H8), C9(H9), C10(H10), C11(H11), C18(H18), C17(H17),
 C16(H16), C15(H15), C14(H14), C18(H18), C17(H17), C16(H16), C15(H15), C14(H14),
  C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C6(H6), C5(H5), C4(H4), C3(H3),
 C2(H2), C3(H3), C5(H5), C6(H6), C2(H2)
4.b Fitted hexagon refined as free rotating group:
 C1(C6,C5,C4,C3,C2), C1(C2,C3,C4,C5,C6), C1(C2,C3,C4,C5,C6), C1(C6,C5,C4,C3,
 C2), C1(C6,C5,C4,C3,C2), C4(C3,C2,C1,C6,C5), C1(C6,C5,C4,C3,C2), C1(C6,C5,C4,
 C3,C2), C3(C2,C1,C6,C5,C4), C5(C4,C3,C2,C1,C6), C2(C3,C4,C5,C6,C1), C1(C2,C3,
 C4,C5,C6), C1(C2,C3,C4,C5,C6), C1(C2,C3,C4,C5,C6), C1(C2,C3,C4,C5,C6), C1(C2,
 C3,C4,C5,C6), C1(C6,C5,C4,C3,C2), C2(C3,C4,C5,C6,C1), C1(C6,C5,C4,C3,C2),
 C1(C6,C5,C4,C3,C2), C2(C3,C4,C5,C6,C1), C1(C2,C3,C4,C5,C6), C1(C6,C5,C4,C3,C2),
  C6(C1,C2,C3,C4,C5), C2(C1,C6,C5,C4,C3), C1(C2,C3,C4,C5,C6), C1(C6,C5,C4,C3,
 C2), C2(C1,C6,C5,C4,C3), C7(C12,C11,C10,C9,C8), C18(C17,C16,C15,C14,C13),
 C6(C5,C4,C3,C2,C1), C13(C14,C15,C16,C17,C18), C10(C9,C8,C7,C12,C11), C6(C1,C2,
 C3,C4,C5), C18(C17,C16,C15,C14,C13), C6(C1,C2,C3,C4,C5), C7(C8,C9,C10,C11,C12),
  C1(C2,C3,C4,C5,C6), C16(C17,C18,C13,C14,C15), C9(C8,C7,C12,C11,C10), C14(C15,
 C16,C17,C18,C13), C6(C1,C2,C3,C4,C5), C11(C10,C9,C8,C7,C12), C14(C15,C16,C17,
 C18,C13), C7(C8,C9,C10,C11,C12), C1(C2,C3,C4,C5,C6), C2(C1,C6,C5,C4,C3), C8(C9,
 C10,C11,C12,C7), C13(C14,C15,C16,C17,C18), C1(C6,C5,C4,C3,C2), C12(C7,C8,C9,
 C10,C11), C13(C18,C17,C16,C15,C14), C8(C9,C10,C11,C12,C7), C6(C5,C4,C3,C2,C1),
 C3(C4,C5,C6,C1,C2)
;
_shelx_res_checksum              73064
_shelx_hkl_checksum              77435
_shelx_fab_checksum              45699
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
__vrf_plat026_1_sq
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PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        28% Check 
RESPONSE: The crystal quality is not very good, we tried many 
times and couldn't get a high quality crystal
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