Restriction of intramolecular rotation for functionalizing metal nanoclusters.
Xin, Junsheng; Xu, Jing; Zhu, Chen; Tian, Yupeng; Zhang, Qiong; Kang, Xi; Zhu, Manzhou; Chemical science 14 (2023) 8474–8482; doi:10.1039/d3sc01698f

data_1569583
_publ_section_title
;
 Restriction of intramolecular rotation for functionalizing metal
 nanoclusters.
;
_journal_issue                   32
_journal_name_full               'Chemical science'
_journal_page_first              8474
_journal_page_last               8482
_journal_paper_doi               10.1039/d3sc01698f
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C129 H93 Ag13 Au4 Cl18 P6 S9'
_chemical_formula_sum            'C129 H93 Ag13 Au4 Cl18 P6 S9'
_chemical_formula_weight         4945.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-14
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-30 deposited with the CCDC.	2023-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.9510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.1353(4)
_cell_length_b                   24.3999(4)
_cell_length_c                   26.5043(4)
_cell_measurement_reflns_used    63734
_cell_measurement_temperature    120
_cell_measurement_theta_max      70.16
_cell_measurement_theta_min      3.34
_cell_volume                     15606.2(4)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.153.0 (STOE, 2018)'
_computing_data_reduction
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 2018)
;
_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  (Sheldrick, 2015)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      '1440 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  0.0564
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            85780
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        62.496
_diffrn_reflns_theta_max         62.496
_diffrn_reflns_theta_min         3.335
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    24.508
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.0394
_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            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.105
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9336
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.698
_refine_diff_density_min         -1.928
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1576
_refine_ls_number_reflns         24713
_refine_ls_number_restraints     1530
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0577P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1078
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17662
_reflns_number_total             24713
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01698f2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 1569583.cif.'
_cod_database_code               1569583
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.245
_shelx_estimated_absorpt_t_min   0.157
_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
C01H \\sim C01I \\sim C01L \\sim C01M \\sim C01N \\sim C01O \\sim C01P \\sim
C01Q \\sim C01R \\sim C01S \\sim C01U \\sim C01V \\sim C01W \\sim C01X \\sim
C01Y \\sim C01Z \\sim C020 \\sim C021 \\sim C022 \\sim C023 \\sim C024 \\sim
C025 \\sim C026 \\sim C027 \\sim C028 \\sim C029 \\sim C02A \\sim C02B \\sim
C02C \\sim C02D \\sim C02E \\sim C02F \\sim C02G \\sim C02H \\sim C04R \\sim
C0AA \\sim C6 \\sim C7 \\sim C033 \\sim C02I \\sim C02J \\sim C02K \\sim C02L
\\sim C02M \\sim C02N \\sim C02O \\sim C02P \\sim C02Q \\sim C02R \\sim C02S
\\sim C02T \\sim C02U \\sim C02V \\sim C02X \\sim C02Y \\sim C02Z \\sim C030
\\sim C031 \\sim C032 \\sim C034 \\sim C035 \\sim C036 \\sim C037 \\sim C038
\\sim C039 \\sim C03B \\sim C03C \\sim C03D \\sim C03E \\sim C03F \\sim C03H
\\sim C03I \\sim C03J \\sim C03K \\sim C03L \\sim C03N \\sim C03O \\sim C03P
\\sim C03Q \\sim C03S \\sim C03T \\sim C03V \\sim C03W \\sim C03X \\sim C03Y
\\sim C040 \\sim C041 \\sim C043 \\sim C044 \\sim C046 \\sim C048 \\sim C049
\\sim C04B \\sim C04I \\sim C2 \\sim C12 \\sim C9 \\sim C051 \\sim C04C \\sim
C04D \\sim C04E \\sim C04F \\sim C04G \\sim C04H \\sim C04J \\sim C04K \\sim
C04L \\sim C04M \\sim C04N \\sim C04O \\sim C04P \\sim C04T \\sim C04V \\sim
C04W \\sim C04X \\sim C04Y \\sim C04Z \\sim C055 \\sim C057 \\sim C05A \\sim
C05C \\sim C05M \\sim C1 \\sim C16 \\sim C03G \\sim C052 \\sim C059 \\sim C056
\\sim C3: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(C01H) \\sim Ueq, Uanis(C01I) \\sim Ueq, Uanis(C01L) \\sim Ueq,
Uanis(C01M) \\sim Ueq, Uanis(C01N) \\sim Ueq, Uanis(C01O) \\sim Ueq,
Uanis(C01P) \\sim Ueq, Uanis(C01Q) \\sim Ueq, Uanis(C01R) \\sim Ueq,
Uanis(C01S) \\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(C025) \\sim Ueq, Uanis(C026) \\sim Ueq, Uanis(C027) \\sim Ueq,
Uanis(C028) \\sim Ueq, Uanis(C029) \\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(C04R) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C6)
\\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C033) \\sim Ueq, Uanis(C02I) \\sim Ueq,
Uanis(C02J) \\sim Ueq, Uanis(C02K) \\sim Ueq, Uanis(C02L) \\sim Ueq,
Uanis(C02M) \\sim Ueq, Uanis(C02N) \\sim Ueq, Uanis(C02O) \\sim Ueq,
Uanis(C02P) \\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(C02X) \\sim Ueq, Uanis(C02Y) \\sim Ueq,
Uanis(C02Z) \\sim Ueq, Uanis(C030) \\sim Ueq, Uanis(C031) \\sim Ueq,
Uanis(C032) \\sim Ueq, Uanis(C034) \\sim Ueq, Uanis(C035) \\sim Ueq,
Uanis(C036) \\sim Ueq, Uanis(C037) \\sim Ueq, Uanis(C038) \\sim Ueq,
Uanis(C039) \\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(C03I) \\sim Ueq, Uanis(C03J) \\sim Ueq,
Uanis(C03K) \\sim Ueq, Uanis(C03L) \\sim Ueq, Uanis(C03N) \\sim Ueq,
Uanis(C03O) \\sim Ueq, Uanis(C03P) \\sim Ueq, Uanis(C03Q) \\sim Ueq,
Uanis(C03S) \\sim Ueq, Uanis(C03T) \\sim Ueq, Uanis(C03V) \\sim Ueq,
Uanis(C03W) \\sim Ueq, Uanis(C03X) \\sim Ueq, Uanis(C03Y) \\sim Ueq,
Uanis(C040) \\sim Ueq, Uanis(C041) \\sim Ueq, Uanis(C043) \\sim Ueq,
Uanis(C044) \\sim Ueq, Uanis(C046) \\sim Ueq, Uanis(C048) \\sim Ueq,
Uanis(C049) \\sim Ueq, Uanis(C04B) \\sim Ueq, Uanis(C04I) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C051) \\sim Ueq,
Uanis(C04C) \\sim Ueq, Uanis(C04D) \\sim Ueq, Uanis(C04E) \\sim Ueq,
Uanis(C04F) \\sim Ueq, Uanis(C04G) \\sim Ueq, Uanis(C04H) \\sim Ueq,
Uanis(C04J) \\sim Ueq, Uanis(C04K) \\sim Ueq, Uanis(C04L) \\sim Ueq,
Uanis(C04M) \\sim Ueq, Uanis(C04N) \\sim Ueq, Uanis(C04O) \\sim Ueq,
Uanis(C04P) \\sim Ueq, Uanis(C04T) \\sim Ueq, Uanis(C04V) \\sim Ueq,
Uanis(C04W) \\sim Ueq, Uanis(C04X) \\sim Ueq, Uanis(C04Y) \\sim Ueq,
Uanis(C04Z) \\sim Ueq, Uanis(C055) \\sim Ueq, Uanis(C057) \\sim Ueq,
Uanis(C05A) \\sim Ueq, Uanis(C05C) \\sim Ueq, Uanis(C05M) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C03G) \\sim Ueq, Uanis(C052) \\sim Ueq,
Uanis(C059) \\sim Ueq, Uanis(C056) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C01M(H01A,H01B), C01N(H01C,H01D), C02F(H02A,H02B)
3.b Aromatic/amide H refined with riding coordinates:
 C01Q(H01Q), C01U(H01U), C01V(H01V), C01Y(H01Y), C01Z(H01Z), C021(H021),
 C023(H023), C025(H025), C02G(H02G), C04R(H04R), C0AA(H0AA), C6(H6), C7(H7),
 C033(H033), C02L(H02L), C02M(H02M), C02N(H02N), C02P(H02P), C02Q(H02Q),
 C02S(H02S), C02U(H02U), C02X(H02X), C02Z(H02Z), C032(H032), C034(H034),
 C035(H035), C036(H036), C037(H037), C038(H038), C039(H039), C03B(H03B),
 C03C(H03C), C03D(H03D), C03E(H03E), C03F(H03F), C03H(H03H), C03I(H03I),
 C03J(H03J), C03K(H03K), C03N(H03N), C03O(H03O), C03P(H03P), C03Q(H03Q),
 C03S(H03S), C03T(H03T), C03V(H03V), C03W(H03W), C03X(H03X), C03Y(H03Y),
 C040(H040), C041(H041), C043(H043), C044(H044), C046(H046), C049(H049),
 C04I(H04I), C2(H2), C12(H12), C9(H9), C051(H051), C04C(H04C), C04D(H04D),
 C04E(H04E), C04F(H04F), C04G(H04G), C04H(H04H), C04K(H04K), C04L(H04L),
 C04M(H04M), C04N(H04N), C04O(H04O), C04P(H04P), C04T(H04T), C04V(H04V),
 C04W(H04W), C04X(H04X), C04Y(H04Y), C04Z(H04Z), C055(H055), C057(H057),
 C05A(H05A), C05C(H05C), C05M(H05M), C1(H1), C052(H052), C059(H059), C056(H056)
3.c Fitted hexagon refined as free rotating group:
 C02H(C04R,C0AA,C6,C7,C033), C04B(C04I,C2,C12,C9,C051), C16(C03G,C052,C059,
 C056,C3)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              67044
_shelx_fab_checksum              33433
_olex2_submission_special_instructions 'No special instructions were received'