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_1573790
_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
'C166 H157 Au12 N8 P8 Pd S4, 2(C44 H76.259 N16 Pd2 S8)'
_chemical_formula_sum            'C254 H309.49 Au12 N40 P8 Pd5 S20'
_chemical_formula_weight         7707.44
_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     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                90
_cell_angle_beta                 90.68(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.130(3)
_cell_length_b                   53.449(11)
_cell_length_c                   17.415(4)
_cell_measurement_reflns_used    46543
_cell_measurement_temperature    120
_cell_measurement_theta_max      70.08
_cell_measurement_theta_min      3.64
_cell_volume                     15944(6)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -61
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            93160
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        62.500
_diffrn_reflns_theta_max         62.500
_diffrn_reflns_theta_min         3.641
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.290
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       block
_exptl_crystal_F_000             7463
_refine_diff_density_max         2.660
_refine_diff_density_min         -2.884
_refine_diff_density_rms         0.275
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1468
_refine_ls_number_reflns         24096
_refine_ls_number_restraints     3058
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1041P)^2^+256.2924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1759
_refine_ls_wR_factor_ref         0.1854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19756
_reflns_number_total             24096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr05222f2.cif
_cod_data_source_block           2_sq
_cod_depositor_comments
'Adding full bibliography for 1573789--1573790.cif.'
_cod_database_code               1573790
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H03Y,H03L,H03M} of C03Y, {H05Q,H05O,H05P} of C05A, All
  C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  {H03I,H03J,H03K} of C03U, {H03U,H03V,H03W} of C037, {H0A,H0B,H0C} of C0,
  {H04K,H04L,H04M} of C04M, {HAA,HAB,HAC} of CA, {H4AA,H4AB,H4AC} of C4A, {H2A,
  H2B,H2C} of C2, {H7BA,H7BB,H7BC} of C7B, {H4BA,H4BB,H4BC} of C4B, {H6BA,H6BB,
  H6BC} of C6B, {H05A,H05B,H05C} of C051, {H6AA,H6AB,H6AC} of C6A, {HBA,HBB,
  HBC} of CB, {H04N,H04O,H04P} of C04T
2. Restrained distances
 C7B-C05H
 1.72 with sigma of 0.01
 C7A-C05H
 1.72 with sigma of 0.01
 C7A-C05I
 2.7 with sigma of 0.01
 H00O-H03G
 1.89 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C00U \\sim C039 \\sim C03P \\sim C01L \\sim C02O \\sim C023 \\sim C04P \\sim
C03M \\sim C02H \\sim C01W \\sim C032 \\sim C015 \\sim C046 \\sim C00W \\sim
C05I \\sim C012 \\sim C02E \\sim C016 \\sim C02I \\sim C01C \\sim C02V \\sim
C02X \\sim C03C \\sim C022 \\sim C03Z \\sim C02P \\sim C04C \\sim C01M \\sim
C057 \\sim C019 \\sim C7B \\sim C01A \\sim C03J \\sim C01D \\sim C02B \\sim
C027 \\sim C024 \\sim C02U \\sim C02M \\sim C02S \\sim C02R \\sim C021 \\sim
C030 \\sim C01R \\sim C037 \\sim C01E \\sim C03H \\sim C01J \\sim C03U \\sim
C033 \\sim C044 \\sim C04F \\sim C048 \\sim C03B \\sim C04L \\sim C01Z \\sim
C051 \\sim C01F \\sim C05C \\sim C01G \\sim C4B \\sim C01H \\sim C6B \\sim C042
\\sim C038 \\sim C04V \\sim C02C \\sim C05F \\sim C02F \\sim C04U \\sim C02Z
\\sim C026 \\sim C029 \\sim C01I \\sim C02G \\sim C01K \\sim C02L \\sim C01N
\\sim C02N \\sim C01Q \\sim C02Q \\sim C01T \\sim C02T \\sim C02A \\sim C02W
\\sim C02J \\sim C031 \\sim C03N \\sim C035 \\sim C02D \\sim C03A \\sim C02Y
\\sim C03G \\sim C01U \\sim C03L \\sim C01V \\sim C03S \\sim C03X \\sim C03Y
\\sim C040 \\sim C041 \\sim C04S \\sim C0 \\sim C050 \\sim C047 \\sim C025
\\sim C04B \\sim C01X \\sim C04D \\sim C01Y \\sim C04M \\sim C02K \\sim C04T
\\sim C034 \\sim C056 \\sim C043 \\sim C05A \\sim C04X \\sim C05H \\sim C03R
\\sim CB \\sim C020 \\sim C1 \\sim C028 \\sim C3 \\sim C03Q \\sim C04A: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
C02Y \\sim P00H: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
C7B \\sim C7A \\sim CB \\sim CA \\sim C6B \\sim C6A \\sim C4B \\sim C4A \\sim
C0 \\sim C2: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
Uanis(C00U) \\sim Ueq, Uanis(C039) \\sim Ueq, Uanis(C03P) \\sim Ueq,
Uanis(C01L) \\sim Ueq, Uanis(C02O) \\sim Ueq, Uanis(C023) \\sim Ueq,
Uanis(C04P) \\sim Ueq, Uanis(C03M) \\sim Ueq, Uanis(C02H) \\sim Ueq,
Uanis(C01W) \\sim Ueq, Uanis(C032) \\sim Ueq, Uanis(C015) \\sim Ueq,
Uanis(C046) \\sim Ueq, Uanis(C00W) \\sim Ueq, Uanis(C05I) \\sim Ueq,
Uanis(C012) \\sim Ueq, Uanis(C02E) \\sim Ueq, Uanis(C016) \\sim Ueq,
Uanis(C02I) \\sim Ueq, Uanis(C01C) \\sim Ueq, Uanis(C02V) \\sim Ueq,
Uanis(C02X) \\sim Ueq, Uanis(C03C) \\sim Ueq, Uanis(C022) \\sim Ueq,
Uanis(C03Z) \\sim Ueq, Uanis(C02P) \\sim Ueq, Uanis(C04C) \\sim Ueq,
Uanis(C01M) \\sim Ueq, Uanis(C057) \\sim Ueq, Uanis(C019) \\sim Ueq, Uanis(C7B)
\\sim Ueq, Uanis(C01A) \\sim Ueq, Uanis(C03J) \\sim Ueq, Uanis(C01D) \\sim Ueq,
Uanis(C02B) \\sim Ueq, Uanis(C027) \\sim Ueq, Uanis(C024) \\sim Ueq,
Uanis(C02U) \\sim Ueq, Uanis(C02M) \\sim Ueq, Uanis(C02S) \\sim Ueq,
Uanis(C02R) \\sim Ueq, Uanis(C021) \\sim Ueq, Uanis(C030) \\sim Ueq,
Uanis(C01R) \\sim Ueq, Uanis(C037) \\sim Ueq, Uanis(C01E) \\sim Ueq,
Uanis(C03H) \\sim Ueq, Uanis(C01J) \\sim Ueq, Uanis(C03U) \\sim Ueq,
Uanis(C033) \\sim Ueq, Uanis(C044) \\sim Ueq, Uanis(C04F) \\sim Ueq,
Uanis(C048) \\sim Ueq, Uanis(C03B) \\sim Ueq, Uanis(C04L) \\sim Ueq,
Uanis(C01Z) \\sim Ueq, Uanis(C051) \\sim Ueq, Uanis(C01F) \\sim Ueq,
Uanis(C05C) \\sim Ueq, Uanis(C01G) \\sim Ueq, Uanis(C4B) \\sim Ueq, Uanis(C01H)
\\sim Ueq, Uanis(C6B) \\sim Ueq, Uanis(C042) \\sim Ueq, Uanis(C038) \\sim Ueq,
Uanis(C04V) \\sim Ueq, Uanis(C02C) \\sim Ueq, Uanis(C05F) \\sim Ueq,
Uanis(C02F) \\sim Ueq, Uanis(C04U) \\sim Ueq, Uanis(C02Z) \\sim Ueq,
Uanis(C026) \\sim Ueq, Uanis(C029) \\sim Ueq, Uanis(C01I) \\sim Ueq,
Uanis(C02G) \\sim Ueq, Uanis(C01K) \\sim Ueq, Uanis(C02L) \\sim Ueq,
Uanis(C01N) \\sim Ueq, Uanis(C02N) \\sim Ueq, Uanis(C01Q) \\sim Ueq,
Uanis(C02Q) \\sim Ueq, Uanis(C01T) \\sim Ueq, Uanis(C02T) \\sim Ueq,
Uanis(C02A) \\sim Ueq, Uanis(C02W) \\sim Ueq, Uanis(C02J) \\sim Ueq,
Uanis(C031) \\sim Ueq, Uanis(C03N) \\sim Ueq, Uanis(C035) \\sim Ueq,
Uanis(C02D) \\sim Ueq, Uanis(C03A) \\sim Ueq, Uanis(C02Y) \\sim Ueq,
Uanis(C03G) \\sim Ueq, Uanis(C01U) \\sim Ueq, Uanis(C03L) \\sim Ueq,
Uanis(C01V) \\sim Ueq, Uanis(C03S) \\sim Ueq, Uanis(C03X) \\sim Ueq,
Uanis(C03Y) \\sim Ueq, Uanis(C040) \\sim Ueq, Uanis(C041) \\sim Ueq,
Uanis(C04S) \\sim Ueq, Uanis(C0) \\sim Ueq, Uanis(C050) \\sim Ueq, Uanis(C047)
\\sim Ueq, Uanis(C025) \\sim Ueq, Uanis(C04B) \\sim Ueq, Uanis(C01X) \\sim Ueq,
Uanis(C04D) \\sim Ueq, Uanis(C01Y) \\sim Ueq, Uanis(C04M) \\sim Ueq,
Uanis(C02K) \\sim Ueq, Uanis(C04T) \\sim Ueq, Uanis(C034) \\sim Ueq,
Uanis(C056) \\sim Ueq, Uanis(C043) \\sim Ueq, Uanis(C05A) \\sim Ueq,
Uanis(C04X) \\sim Ueq, Uanis(C05H) \\sim Ueq, Uanis(C03R) \\sim Ueq, Uanis(CB)
\\sim Ueq, Uanis(C020) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C028) \\sim Ueq,
Uanis(C3) \\sim Ueq, Uanis(C03Q) \\sim Ueq, Uanis(C04A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C02Y) \\sim Ueq, Uanis(P00H) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C4B) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C0) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C7B) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C6B) \\sim Ueq,
Uanis(C6A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H05J)=Sof(H05K)=FVAR(1)
 Fixed Sof: H03Y(0.5) H03L(0.5) H03M(0.5) C0(0.5) H0A(0.5) H0B(0.5) H0C(0.5)
 H05Q(0.5) H05O(0.5) H05P(0.5) H05H(0.5) H05I(0.5) H05F(0.5) H05G(0.5)
 H05L(0.5) H05M(0.5) CB(0.5) HBA(0.5) HBB(0.5) HBC(0.5) C4B(0.5) H4BA(0.5)
 H4BB(0.5) H4BC(0.5) C7B(0.5) H7BA(0.5) H7BB(0.5) H7BC(0.5) H3BC(0.5) H3BD(0.5)
 H3AA(0.5) H3AB(0.5) C6B(0.5) H6BA(0.5) H6BB(0.5) H6BC(0.5) C6A(0.5) H6AA(0.5)
 H6AB(0.5) H6AC(0.5) CA(0.5) HAA(0.5) HAB(0.5) HAC(0.5) C7A(0.5) C2(0.5)
 H2A(0.5) H2B(0.5) H2C(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5) H4AC(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C01G(H01A,H01B), C01Q(H01C,H01D), C01X(H01E,H01F), C02G(H02A,H02B), C02Q(H02C,
 H02D), C02R(H02E,H02F), C02T(H02G,H02H), C02W(H02L,H02M), C030(H03A,H03B),
 C032(H03C,H03D), C035(H03E,H03F), C03A(H03G,H03H), C03G(H03Z,H), C03P(H03,HA),
 C03S(H1,HB), C03Y(H03L,H03M), C03Z(H03N,H03O), C046(H04A,H04B), C048(H04T,
 H04W), C04B(H04C,H04D), C04C(H04E,H04F), C04D(H04G,H04H), C04L(H04I,H04J),
 C057(H05D,H05E), C05A(H05O,H05P), C05C(H05H,H05I), C05C(H05F,H05G), C05H(H05J,
 H05K), C05I(H05L,H05M), C1(H1A,H1B), C3(H3BC,H3BD), C3(H3AA,H3AB)
5.b Aromatic/amide H refined with riding coordinates:
 N00O(H00O), N00R(H00R), N00S(H00S), N00T(H00T), C01L(H01L), C023(H023),
 C03M(H03P), C01W(H01W), C015(H015), N013(H013), N014(H014), C01C(H01G),
 C02X(H02X), C022(H022), C02P(H02P), C01M(H01M), N017(H017), C027(H027),
 C02U(H02U), C02S(H02S), C021(H021), C01R(H01R), C01J(H01J), C033(H033),
 C04F(H04Q), C03B(H03Q), C01Z(H01Z), C01H(H01H), C042(H042), C04V(H04V),
 C05F(H05N), C04U(H04U), N01O(H01O), C01T(H01T), C02A(H02N), C02J(H02O),
 C03N(H2), C02D(H02Q), C01V(H01V), C03X(H03X), C040(H040), C04S(H04S),
 C050(H050), C01Y(H01Y), C034(H034), C043(H043), C04X(H04X), C03R(H03R),
 C028(H028), C03Q(H03S), C04A(H04R), C039(H039), C03J(H03T), C02F(H02I),
 C02B(H02J), C02Z(H02Z), C02H(H02K), C024(H024), C02I(H02R), C02L(H02T),
 C02O(H02V), C03C(H3), C03H(H4), C03Y(H03Y), C041(H041), C044(H044), C047(H047),
  C04P(H04Y), C056(H056), C05A(H05Q), N5(H5)
5.c Fitted hexagon refined as free rotating group:
 C00U(C01L,C023,C03M,C01W,C015), C016(C01C,C02X,C022,C02P,C01M), C01D(C027,
 C02U,C02S,C021,C01R), C01E(C01J,C033,C04F,C03B,C01Z), C01H(C042,C04V,C05F,C04U,
 C026), C01T(C02A,C02J,C03N,C02D,C02Y), C01V(C03X,C040,C04S,C050,C025),
 C01Y(C02K,C034,C043,C04X,C03R), C028(C03Q,C04A,C039,C038,C03J), C02F(C02B,C02Z,
 C02H,C029,C024)
5.d Idealised Me refined as rotating group:
 C037(H03U,H03V,H03W), C03U(H03I,H03J,H03K), C0(H0A,H0B,H0C), C04M(H04K,H04L,
 H04M), C04T(H04N,H04O,H04P), C051(H05A,H05B,H05C), CB(HBA,HBB,HBC), C4B(H4BA,
 H4BB,H4BC), C7B(H7BA,H7BB,H7BC), C6B(H6BA,H6BB,H6BC), C6A(H6AA,H6AB,H6AC),
 CA(HAA,HAB,HAC), C2(H2A,H2B,H2C), C4A(H4AA,H4AB,H4AC)
;
_shelx_res_checksum              97694
_shelx_hkl_checksum              76134
_shelx_fab_checksum              99449
_olex2_submission_special_instructions 'No special instructions were received'