Heteroatom number-dependent cluster frameworks in structurally comparable Pd-Au nanoclusters.
Fu, Ziwei; Li, Chen; Tian, Ye; Alam, Fakhari; Hu, Daqiao; Shen, Honglei; Kang, Xi; Zhu, Manzhou; Nanoscale 17 (2025) 4494–4501; doi:10.1039/d4nr05222f

data_1573789
_publ_section_title
;
 Heteroatom number-dependent cluster frameworks in structurally comparable
 Pd-Au nanoclusters.
;
_journal_issue                   8
_journal_name_full               Nanoscale
_journal_page_first              4494
_journal_page_last               4501
_journal_paper_doi               10.1039/d4nr05222f
_journal_volume                  17
_journal_year                    2025
_chemical_formula_moiety         'C83 H79 Au6 N4 P4 Pd S2, C41 H70 N16 Pd2 S8'
_chemical_formula_sum            'C124 H149 Au6 N20 P4 Pd3 S10'
_chemical_formula_weight         3865.10
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-01-10
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-01-12 deposited with the CCDC.	2025-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                99.096(2)
_cell_angle_beta                 90.215(2)
_cell_angle_gamma                91.009(2)
_cell_formula_units_Z            2
_cell_length_a                   16.7465(5)
_cell_length_b                   17.5624(5)
_cell_length_c                   26.3391(7)
_cell_measurement_reflns_used    35935
_cell_measurement_temperature    120
_cell_measurement_theta_max      70.08
_cell_measurement_theta_min      5.29
_cell_volume                     7647.8(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
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.0, Darmstadt 2021
;
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 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 0.961
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_details      '1775 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  0.0646
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            63120
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.227
_diffrn_reflns_theta_min         5.284
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    15.349
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3730
_refine_diff_density_max         3.819
_refine_diff_density_min         -4.188
_refine_diff_density_rms         0.293
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1370
_refine_ls_number_reflns         27202
_refine_ls_number_restraints     2934
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0760
_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^)+(0.1550P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2060
_refine_ls_wR_factor_ref         0.2261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18424
_reflns_number_total             27202
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr05222f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1573789--1573790.cif.'
_cod_database_code               1573789
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C00U \\sim C01S \\sim C033 \\sim C010 \\sim C02K \\sim C011 \\sim C04I \\sim
C012 \\sim C04J \\sim C016 \\sim C044 \\sim C02A \\sim C03Y \\sim C02X \\sim
C05A \\sim C02Y \\sim C023 \\sim C039 \\sim C02R \\sim C01O \\sim C03S \\sim
C019 \\sim C02S \\sim C02O \\sim C03K \\sim C02L \\sim C049 \\sim C034 \\sim
C04Z \\sim C03L \\sim C03N \\sim C01Z \\sim C01X \\sim C01B \\sim C03Q \\sim
C01C \\sim C02B \\sim C03A \\sim C046 \\sim C04R \\sim C02G \\sim C04V \\sim
C03P \\sim C04E \\sim C02M \\sim C01P \\sim C02W \\sim C01D \\sim C03F \\sim
C02Z \\sim C03O \\sim C035 \\sim C042 \\sim C040 \\sim C04F \\sim C03V \\sim
C04M \\sim C01Y \\sim C055 \\sim C01E \\sim C05K \\sim C03W \\sim C03Z \\sim
C047 \\sim C01U \\sim C04P \\sim C021 \\sim C03X \\sim C036 \\sim C01Q \\sim
C04T \\sim C01F \\sim C03I \\sim C01G \\sim C02C \\sim C01H \\sim C050 \\sim
C01I \\sim C03D \\sim C038 \\sim C02D \\sim C04O \\sim C02H \\sim C04N \\sim
C030 \\sim C04D \\sim C03H \\sim C027 \\sim C02J \\sim C01K \\sim C02N \\sim
C01L \\sim C02U \\sim C02I \\sim C031 \\sim C024 \\sim C03B \\sim C03G \\sim
C03J \\sim C01W \\sim C03M \\sim C02F \\sim C03R \\sim C01M \\sim C041 \\sim
C01N \\sim C048 \\sim C01V \\sim C04A \\sim C029 \\sim C04G \\sim C026 \\sim
C04K \\sim C02V \\sim C04U \\sim C1 \\sim C052 \\sim C01R \\sim C056 \\sim C02Q
\\sim C05B \\sim C032 \\sim C14 \\sim C03E: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 3.8A
Uanis(C00U) \\sim Ueq, Uanis(C01S) \\sim Ueq, Uanis(C033) \\sim Ueq,
Uanis(C010) \\sim Ueq, Uanis(C02K) \\sim Ueq, Uanis(C011) \\sim Ueq,
Uanis(C04I) \\sim Ueq, Uanis(C012) \\sim Ueq, Uanis(C04J) \\sim Ueq,
Uanis(C016) \\sim Ueq, Uanis(C044) \\sim Ueq, Uanis(C02A) \\sim Ueq,
Uanis(C03Y) \\sim Ueq, Uanis(C02X) \\sim Ueq, Uanis(C05A) \\sim Ueq,
Uanis(C02Y) \\sim Ueq, Uanis(C023) \\sim Ueq, Uanis(C039) \\sim Ueq,
Uanis(C02R) \\sim Ueq, Uanis(C01O) \\sim Ueq, Uanis(C03S) \\sim Ueq,
Uanis(C019) \\sim Ueq, Uanis(C02S) \\sim Ueq, Uanis(C02O) \\sim Ueq,
Uanis(C03K) \\sim Ueq, Uanis(C02L) \\sim Ueq, Uanis(C049) \\sim Ueq,
Uanis(C034) \\sim Ueq, Uanis(C04Z) \\sim Ueq, Uanis(C03L) \\sim Ueq,
Uanis(C03N) \\sim Ueq, Uanis(C01Z) \\sim Ueq, Uanis(C01X) \\sim Ueq,
Uanis(C01B) \\sim Ueq, Uanis(C03Q) \\sim Ueq, Uanis(C01C) \\sim Ueq,
Uanis(C02B) \\sim Ueq, Uanis(C03A) \\sim Ueq, Uanis(C046) \\sim Ueq,
Uanis(C04R) \\sim Ueq, Uanis(C02G) \\sim Ueq, Uanis(C04V) \\sim Ueq,
Uanis(C03P) \\sim Ueq, Uanis(C04E) \\sim Ueq, Uanis(C02M) \\sim Ueq,
Uanis(C01P) \\sim Ueq, Uanis(C02W) \\sim Ueq, Uanis(C01D) \\sim Ueq,
Uanis(C03F) \\sim Ueq, Uanis(C02Z) \\sim Ueq, Uanis(C03O) \\sim Ueq,
Uanis(C035) \\sim Ueq, Uanis(C042) \\sim Ueq, Uanis(C040) \\sim Ueq,
Uanis(C04F) \\sim Ueq, Uanis(C03V) \\sim Ueq, Uanis(C04M) \\sim Ueq,
Uanis(C01Y) \\sim Ueq, Uanis(C055) \\sim Ueq, Uanis(C01E) \\sim Ueq,
Uanis(C05K) \\sim Ueq, Uanis(C03W) \\sim Ueq, Uanis(C03Z) \\sim Ueq,
Uanis(C047) \\sim Ueq, Uanis(C01U) \\sim Ueq, Uanis(C04P) \\sim Ueq,
Uanis(C021) \\sim Ueq, Uanis(C03X) \\sim Ueq, Uanis(C036) \\sim Ueq,
Uanis(C01Q) \\sim Ueq, Uanis(C04T) \\sim Ueq, Uanis(C01F) \\sim Ueq,
Uanis(C03I) \\sim Ueq, Uanis(C01G) \\sim Ueq, Uanis(C02C) \\sim Ueq,
Uanis(C01H) \\sim Ueq, Uanis(C050) \\sim Ueq, Uanis(C01I) \\sim Ueq,
Uanis(C03D) \\sim Ueq, Uanis(C038) \\sim Ueq, Uanis(C02D) \\sim Ueq,
Uanis(C04O) \\sim Ueq, Uanis(C02H) \\sim Ueq, Uanis(C04N) \\sim Ueq,
Uanis(C030) \\sim Ueq, Uanis(C04D) \\sim Ueq, Uanis(C03H) \\sim Ueq,
Uanis(C027) \\sim Ueq, Uanis(C02J) \\sim Ueq, Uanis(C01K) \\sim Ueq,
Uanis(C02N) \\sim Ueq, Uanis(C01L) \\sim Ueq, Uanis(C02U) \\sim Ueq,
Uanis(C02I) \\sim Ueq, Uanis(C031) \\sim Ueq, Uanis(C024) \\sim Ueq,
Uanis(C03B) \\sim Ueq, Uanis(C03G) \\sim Ueq, Uanis(C03J) \\sim Ueq,
Uanis(C01W) \\sim Ueq, Uanis(C03M) \\sim Ueq, Uanis(C02F) \\sim Ueq,
Uanis(C03R) \\sim Ueq, Uanis(C01M) \\sim Ueq, Uanis(C041) \\sim Ueq,
Uanis(C01N) \\sim Ueq, Uanis(C048) \\sim Ueq, Uanis(C01V) \\sim Ueq,
Uanis(C04A) \\sim Ueq, Uanis(C029) \\sim Ueq, Uanis(C04G) \\sim Ueq,
Uanis(C026) \\sim Ueq, Uanis(C04K) \\sim Ueq, Uanis(C02V) \\sim Ueq,
Uanis(C04U) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C052) \\sim Ueq, Uanis(C01R)
\\sim Ueq, Uanis(C056) \\sim Ueq, Uanis(C02Q) \\sim Ueq, Uanis(C05B) \\sim Ueq,
Uanis(C032) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C03E) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C01M(H01C,H01E), C01S(H01F,H01G), C01X(H01A,H01B), C02D(H02B,H02C), C02G(H02D,
 H02E), C02J(H02G,H02J), C02N(H02M,H02N), C02U(H02O,H02P), C02W(H02Q,H02S),
 C031(H03K,H03M), C033(H03B,H03C), C03B(H03O,H03R), C03F(H03S,H03T), C03J(H03U,
 H03Y), C03K(H03,H), C03M(H2,HA), C03O(H3,HB), C03R(H4,HC), C03Y(H03F,H03J),
 C042(H04K,H04L), C048(H04M,H04Q), C049(H04S,H04U), C04F(H04Z,HD), C04K(H04A,
 H04B), C04U(H04C,H04F), C052(H05A,H05B)
3.b Aromatic/amide H refined with riding coordinates:
 N00S(H00S), N00W(H00W), N00Y(H00Y), N015(H015), C016(H016), C02A(H02A),
 C02X(H02X), C02Y(H02Y), C039(H039), C019(H019), C02L(H02L), C034(H034),
 C03L(H03L), C01Z(H01Z), C03A(H03A), C04R(H04R), C04V(H04V), C04E(H04E),
 C01P(H01P), C01D(H01D), C02Z(H02Z), C035(H035), C040(H040), C03V(H03V),
 C03W(H03W), C047(H047), C04P(H04P), C03X(H03X), C01Q(H01Q), C038(H038),
 C04O(H04O), C04N(H04N), C04D(H04D), C027(H027), C02I(H02I), C024(H024),
 C03G(H03G), C01W(H01W), C02F(H02F), C01V(H01V), C029(H029), C026(H026),
 C02V(H02V), C1(H1), C01R(H01R), C032(H032), C03E(H03E), C03N(H03N), C03Z(H03Z),
  N01T(H01T), C036(H036), C03Q(H03Q), C04T(H04T), C04J(H04J), C03I(H03I),
 C02R(H02R), C050(H050), C046(H046), C03D(H03D), C02K(H02K), C02H(H02H),
 C030(H030), C03P(H03P), C03H(H03H), C044(H044), N043(H043), C14(H14)
3.c Fitted hexagon refined as free rotating group:
 C016(C02A,C02X,C02Y,C039,C01O), C019(C02O,C02L,C034,C03L,C01Z), C01C(C03A,
 C04R,C04V,C04E,C01P), C01D(C02Z,C035,C040,C03V,C01Y), C01E(C03W,C047,C04P,C03X,
 C01Q), C01I(C038,C04O,C04N,C04D,C027), C01L(C02I,C024,C03G,C01W,C02F),
 C01N(C01V,C029,C026,C02V,C1), C01R(C02Q,C032,C03E,C03N,C03Z), C023(C036,C03Q,
 C04T,C04J,C03I), C02C(C02R,C050,C046,C03D,C02K), C02H(C03S,C030,C03P,C03H,C044)
3.d Idealised Me refined as rotating group:
 C041(H04G,H04H,H04I), C04A(H04W,H04X,H04Y), C04I(H04,HE,HF), C04M(H5,HG,HH),
 C04Z(H6,HI,HJ), C055(H05C,H05D,H05E), C056(H05F,H05G,H05H), C05A(H05I,H05J,
 H05K), C05B(H05L,H05M,H05N), C05K(H05O,H05P,H05Q)
;
_shelx_res_checksum              99308
_shelx_hkl_checksum              80702
_shelx_fab_checksum              72967
_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   5.5
_stoe_evaluation_integration_b   -0.6
_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 93.4
_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 140.5
_stoe_evaluation_lana_max_2theta_desired 140.5
_stoe_evaluation_lana_mean_redundancy 2.3
_stoe_evaluation_lana_number_refls_after_or 63121
_stoe_evaluation_lana_number_refls_outliers 5479
_stoe_evaluation_lana_number_refls_total 68600
_stoe_evaluation_lana_number_refls_unique 27203
_stoe_evaluation_lana_number_refls_written 63121
_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 -1
_stoe_evaluation_lana_table
;
2Theta          17.1   31.7   46.3   60.9   75.5   90.1  104.7  119.3  133.9
<Resolution>    4.48   2.72   1.94   1.51   1.24   1.09   0.97   0.89   0.84
N(total)         481   1829   3299   4317  13518  13771  13480  11723   6182
<Redundancy>     1.6    1.8    1.7    1.5    3.1    2.7    2.5    2.3    2.0
Complet. [%%]    92.3   96.8   97.0   94.1   97.8   99.2   98.7   96.8   69.4
<I/sigma>       31.7   22.9   17.3    8.2    6.4    4.3    3.7    3.3    2.7
R(int)         0.049  0.041  0.055  0.088  0.056  0.063  0.076  0.090  0.164
;
_stoe_measurement_identifier     1
_stoe_measurement_max_exposure_per_frame '2.0 s'
_stoe_measurement_mean_exposure_per_frame '1.7 s'
_stoe_measurement_min_exposure_per_frame '1.0 s'
_stoe_measurement_total_exposure_time '52 min'
_stoe_measurement_total_frame_number 1775
_stoe_measurement_total_run_number 31
_stoe_measurement_tube_power     '30.0 W'