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_1572631
_publ_section_title
;
 Size disproportionation among nanocluster transformations.
;
_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         'C336 H225 Ag26 Cu17 F90 P7 S30'
_chemical_formula_sum            'C336 H225 Ag26 Cu17 F90 P7 S30'
_chemical_formula_weight         11035.54
_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             2024-07-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-07-12 deposited with the CCDC.	2024-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   28.6272(9)
_cell_length_b                   28.6272(9)
_cell_length_c                   108.574(5)
_cell_measurement_reflns_used    10524
_cell_measurement_temperature    120
_cell_measurement_theta_max      69.01
_cell_measurement_theta_min      5.86
_cell_volume                     77057(5)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection       'X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)'
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      '1508 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_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       132
_diffrn_reflns_limit_l_min       -77
_diffrn_reflns_number            147010
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.050
_diffrn_reflns_theta_min         5.886
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    10.415
_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_colour            'metallic blackish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             32106
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.219
_refine_diff_density_min         -2.586
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1349
_refine_ls_number_reflns         31928
_refine_ls_number_restraints     1368
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0682P)^2^+758.2009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1309
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26107
_reflns_number_total             31928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04884a2.cif
_cod_data_source_block           1_CCDC2
_cod_depositor_comments
'Adding full bibliography for 1572629--1572632.cif.'
_cod_original_cell_volume        77057(6)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1572631
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.422
_shelx_estimated_absorpt_t_min   0.422
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C00X \\sim C011 \\sim C012 \\sim C013 \\sim C014 \\sim C015 \\sim C017 \\sim
C018 \\sim C019 \\sim C01B \\sim C01C \\sim C01D \\sim C01E \\sim C01F \\sim
C01G \\sim C01H \\sim C01I \\sim C01J \\sim C01K \\sim C01M \\sim C01N \\sim
C01O \\sim C01P \\sim C01R \\sim C01S \\sim C01T \\sim C01U \\sim C01V \\sim
C01W \\sim C01X \\sim C01Y \\sim C01Z \\sim C020 \\sim C021 \\sim C022 \\sim
C023 \\sim C024 \\sim C026 \\sim C027 \\sim C028 \\sim C02A \\sim C02B \\sim
C02C \\sim C02D \\sim C02E \\sim C02F \\sim C02G \\sim C02H \\sim C02I \\sim
C02J \\sim C02L \\sim C02M \\sim C02N \\sim C02Q \\sim C02R \\sim C02S \\sim
C02T \\sim C02U \\sim C02V \\sim C02W \\sim C02X \\sim C02Y \\sim C030 \\sim
C031 \\sim C034 \\sim C035 \\sim C036 \\sim C037 \\sim C038 \\sim C03A \\sim
C03B \\sim C03C \\sim C03D \\sim C03E \\sim C03F \\sim C03H \\sim C03J \\sim
C03K \\sim C03L \\sim C03M \\sim C03N \\sim C03P \\sim C03Q \\sim C03R \\sim
C03S \\sim C03U \\sim C03V \\sim C03X \\sim C03Y \\sim C03Z \\sim C040 \\sim
C041 \\sim C046 \\sim C048 \\sim C04B \\sim C04C \\sim C04D \\sim C04E \\sim
C04G \\sim C04H \\sim C04I \\sim C04J \\sim C04M \\sim C04N \\sim C04O \\sim
C04Q \\sim C04S \\sim C04T \\sim C04U \\sim C04V \\sim C9 \\sim C12: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C00X) \\sim Ueq, Uanis(C011) \\sim Ueq, Uanis(C012) \\sim Ueq,
Uanis(C013) \\sim Ueq, Uanis(C014) \\sim Ueq, Uanis(C015) \\sim Ueq,
Uanis(C017) \\sim Ueq, Uanis(C018) \\sim Ueq, Uanis(C019) \\sim Ueq,
Uanis(C01B) \\sim Ueq, Uanis(C01C) \\sim Ueq, Uanis(C01D) \\sim Ueq,
Uanis(C01E) \\sim Ueq, Uanis(C01F) \\sim Ueq, Uanis(C01G) \\sim Ueq,
Uanis(C01H) \\sim Ueq, Uanis(C01I) \\sim Ueq, Uanis(C01J) \\sim Ueq,
Uanis(C01K) \\sim Ueq, Uanis(C01M) \\sim Ueq, Uanis(C01N) \\sim Ueq,
Uanis(C01O) \\sim Ueq, Uanis(C01P) \\sim Ueq, Uanis(C01R) \\sim Ueq,
Uanis(C01S) \\sim Ueq, Uanis(C01T) \\sim Ueq, Uanis(C01U) \\sim Ueq,
Uanis(C01V) \\sim Ueq, Uanis(C01W) \\sim Ueq, Uanis(C01X) \\sim Ueq,
Uanis(C01Y) \\sim Ueq, Uanis(C01Z) \\sim Ueq, Uanis(C020) \\sim Ueq,
Uanis(C021) \\sim Ueq, Uanis(C022) \\sim Ueq, Uanis(C023) \\sim Ueq,
Uanis(C024) \\sim Ueq, Uanis(C026) \\sim Ueq, Uanis(C027) \\sim Ueq,
Uanis(C028) \\sim Ueq, Uanis(C02A) \\sim Ueq, Uanis(C02B) \\sim Ueq,
Uanis(C02C) \\sim Ueq, Uanis(C02D) \\sim Ueq, Uanis(C02E) \\sim Ueq,
Uanis(C02F) \\sim Ueq, Uanis(C02G) \\sim Ueq, Uanis(C02H) \\sim Ueq,
Uanis(C02I) \\sim Ueq, Uanis(C02J) \\sim Ueq, Uanis(C02L) \\sim Ueq,
Uanis(C02M) \\sim Ueq, Uanis(C02N) \\sim Ueq, Uanis(C02Q) \\sim Ueq,
Uanis(C02R) \\sim Ueq, Uanis(C02S) \\sim Ueq, Uanis(C02T) \\sim Ueq,
Uanis(C02U) \\sim Ueq, Uanis(C02V) \\sim Ueq, Uanis(C02W) \\sim Ueq,
Uanis(C02X) \\sim Ueq, Uanis(C02Y) \\sim Ueq, Uanis(C030) \\sim Ueq,
Uanis(C031) \\sim Ueq, Uanis(C034) \\sim Ueq, Uanis(C035) \\sim Ueq,
Uanis(C036) \\sim Ueq, Uanis(C037) \\sim Ueq, Uanis(C038) \\sim Ueq,
Uanis(C03A) \\sim Ueq, Uanis(C03B) \\sim Ueq, Uanis(C03C) \\sim Ueq,
Uanis(C03D) \\sim Ueq, Uanis(C03E) \\sim Ueq, Uanis(C03F) \\sim Ueq,
Uanis(C03H) \\sim Ueq, Uanis(C03J) \\sim Ueq, Uanis(C03K) \\sim Ueq,
Uanis(C03L) \\sim Ueq, Uanis(C03M) \\sim Ueq, Uanis(C03N) \\sim Ueq,
Uanis(C03P) \\sim Ueq, Uanis(C03Q) \\sim Ueq, Uanis(C03R) \\sim Ueq,
Uanis(C03S) \\sim Ueq, Uanis(C03U) \\sim Ueq, Uanis(C03V) \\sim Ueq,
Uanis(C03X) \\sim Ueq, Uanis(C03Y) \\sim Ueq, Uanis(C03Z) \\sim Ueq,
Uanis(C040) \\sim Ueq, Uanis(C041) \\sim Ueq, Uanis(C046) \\sim Ueq,
Uanis(C048) \\sim Ueq, Uanis(C04B) \\sim Ueq, Uanis(C04C) \\sim Ueq,
Uanis(C04D) \\sim Ueq, Uanis(C04E) \\sim Ueq, Uanis(C04G) \\sim Ueq,
Uanis(C04H) \\sim Ueq, Uanis(C04I) \\sim Ueq, Uanis(C04J) \\sim Ueq,
Uanis(C04M) \\sim Ueq, Uanis(C04N) \\sim Ueq, Uanis(C04O) \\sim Ueq,
Uanis(C04Q) \\sim Ueq, Uanis(C04S) \\sim Ueq, Uanis(C04T) \\sim Ueq,
Uanis(C04U) \\sim Ueq, Uanis(C04V) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C12)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F0) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F02K) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F04W) \\sim Ueq, Uanis(F1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Sof(F0)=1-FVAR(1)
 Sof(F1)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C013(H013), C012(H012), C01C(H01C), C01O(H01O), C01J(H01J), C03F(H03F),
 C022(H022), C02C(H02C), C015(H015), C019(H019), C01E(H01E), C018(H018),
 C02B(H02B), C02A(H02A), C02G(H02G), C03U(H03U), C03S(H03S), C01W(H01W),
 C02M(H02M), C04H(H04H), C036(H036), C02F(H02F), C01K(H01K), C01D(H01D),
 C01H(H01H), C01U(H01U), C01X(H01X), C01P(H01P), C01R(H01R), C01T(H01T),
 C02T(H02T), C04M(H04M), C04S(H04S), C04D(H04D), C01V(H01V), C02N(H02N),
 C03R(H03R), C040(H040), C038(H038), C020(H020), C024(H024), C027(H027),
 C02E(H02E), C02Y(H02Y), C03J(H03J), C02W(H02W), C03D(H03D), C02L(H02L),
 C034(H034), C03E(H03E), C04E(H04E), C03Y(H03Y), C02Q(H02Q), C04O(H04O),
 C04I(H04I), C01Y(H01Y), C02U(H02U), C03P(H03P), C030(H030), C035(H035),
 C03H(H03H), C03A(H03A), C03X(H03X), C03V(H03V), C03Q(H03Q), C03B(H03B),
 C02R(H02R), C046(H046), C031(H031), C03L(H03L), C04J(H04J), C04C(H04C),
 C03N(H03N), C04N(H04N), C04T(H04T)
4.b Fitted hexagon refined as free rotating group:
 C013(C00X,C012,C01C,C017,C01O), C014(C01J,C03F,C028,C022,C02C), C01E(C01B,
 C018,C02B,C02D,C02A), C01I(C02G,C03U,C048,C03S,C01W), C01M(C02M,C04H,C03Z,C036,
 C02F), C01N(C01K,C01D,C01H,C01U,C01X), C01T(C02T,C04M,C04S,C04D,C02J),
 C01V(C02N,C03R,C040,C038,C023), C02E(C02Y,C03J,C02W,C03D,C01Z), C02L(C021,C034,
 C03E,C04E,C03Y), C02Q(C04G,C04O,C04I,C02V,C01Y), C037(C03P,C030,C035,C03H,
 C03A), C03X(C03V,C03Q,C03B,C02R,C02X), C046(C02I,C031,C03L,C02H,C04J),
 C04C(C03K,C03N,C04N,C04V,C04T)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              17076
_shelx_hkl_checksum              5802
_shelx_fab_checksum              86689
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '60.0 mm'
_stoe_detector_pixelsize_x       '0.172 mm'
_stoe_detector_pixelsize_y       '0.172 mm'
_stoe_detector_size_x            '8.4 cm'
_stoe_detector_size_y            '10.6 cm'
_stoe_evaluation_integration_a   6.5
_stoe_evaluation_integration_b   0.1
_stoe_evaluation_integration_ems 0.010
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 74.1
_stoe_evaluation_lana_dxs_max_order 3
_stoe_evaluation_lana_dys_max_order 3
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 140.2
_stoe_evaluation_lana_max_2theta_desired 140.2
_stoe_evaluation_lana_mean_redundancy 3.1
_stoe_evaluation_lana_number_refls_after_or 147125
_stoe_evaluation_lana_number_refls_outliers 39133
_stoe_evaluation_lana_number_refls_total 186258
_stoe_evaluation_lana_number_refls_unique 48169
_stoe_evaluation_lana_number_refls_written 147125
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group 3
_stoe_evaluation_lana_table
;
2Theta          18.4   32.8   47.2   61.6   76.0   90.4  104.8  119.2  133.6
<Resolution>    4.28   2.65   1.91   1.50   1.24   1.09   0.97   0.90   0.85
N(total)        1965   6851  11556  14415  38213  35139  34257  29552  14310
<Redundancy>     2.6    2.8    2.6    2.2    4.1    3.4    3.2    2.9    2.2
Complet. [%%]    72.5   79.5   78.5   74.2   79.9   78.7   76.6   73.7   57.6
<I/sigma>       87.4   94.0   58.4   26.2   17.9   10.1    7.3    7.8    6.9
R(int)         0.017  0.017  0.021  0.030  0.032  0.042  0.060  0.056  0.067
;
_stoe_measurement_identifier     1
_stoe_measurement_max_exposure_per_frame '30.0 s'
_stoe_measurement_mean_exposure_per_frame '22.2 s'
_stoe_measurement_min_exposure_per_frame '5.0 s'
_stoe_measurement_total_exposure_time '9.3 h'
_stoe_measurement_total_frame_number 1508
_stoe_measurement_total_run_number 25
_stoe_measurement_tube_power     '30.0 W'