Synthesis of RhH-doped Au-Ag alloy nanoclusters and dopant evolution.
Han, Sang Myeong; Song, Suhwan; Yi, Hanseok; Sim, Eunji; Lee, Dongil; Nanoscale 16 (2024) 4851–4857; doi:10.1039/d3nr05654f

data_1570943
_publ_section_title
;
 Synthesis of RhH-doped Au-Ag alloy nanoclusters and dopant evolution.
;
_journal_issue                   9
_journal_name_full               Nanoscale
_journal_page_first              4851
_journal_page_last               4857
_journal_paper_doi               10.1039/d3nr05654f
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety
'0.03(C144 H162 Ag14.24 Au9.76 Rh S18), 0.1(C H2 Cl2), 0.07(C24 H20 P)'
_chemical_formula_sum
'C6.43 H6.89 Ag0.39 Au0.39 Cl0.26 P0.07 Rh0.03 S0.59'
_chemical_formula_weight         237.68
_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
_audit_block_doi                 10.5517/ccdc.csd.cc2c5rfr
_audit_creation_date             2021-11-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-06-20 deposited with the CCDC.	2024-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                86.42(3)
_cell_angle_beta                 73.32(3)
_cell_angle_gamma                62.20(3)
_cell_formula_units_Z            61
_cell_length_a                   19.803(4)
_cell_length_b                   19.885(4)
_cell_length_c                   32.507(7)
_cell_measurement_reflns_used    130267
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.592
_cell_measurement_theta_min      0.458
_cell_volume                     10808(5)
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.839
_diffrn_measured_fraction_theta_max 0.839
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8000
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 0.839
_diffrn_reflns_Laue_measured_fraction_max 0.839
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            69644
_diffrn_reflns_point_group_measured_fraction_full 0.839
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.042
_diffrn_reflns_theta_min         1.162
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    9.505
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.580
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.228
_exptl_crystal_description       plate
_exptl_crystal_F_000             6794
_refine_diff_density_max         3.275
_refine_diff_density_min         -3.626
_refine_diff_density_rms         0.251
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2275
_refine_ls_number_reflns         35829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0916
_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^)+(0.1960P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2592
_refine_ls_wR_factor_ref         0.2792
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24625
_reflns_number_total             35829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr05654f2.cif
_cod_data_source_block           au12_7_a
_cod_depositor_comments          'Adding full bibliography for 1570943.cif.'
_cod_database_code               1570943
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Au1, Ag1}
{Au2, Ag2}
{Au3, Ag3}
{Au4, Ag4}
{Au5, Ag5}
{Au6, Ag6}
{Au7, Ag7}
{Au8, Ag8}
{Au9, Ag9}
{Au10, Ag10}
{Au11, Ag11}
{Au12, Ag12}
{Ag13, Au13}
{Ag14, Au14}
{Ag15, Au15}
{Ag16, Au16}
{Ag17, Au17}
{Ag18, Au18}
{Ag19, Au19}
{Ag20, Au20}
{Ag24, Au24}
{Ag23, Au23}
{Ag22, Au22}
{Ag21, Au21}
3. Uiso/Uaniso restraints and constraints
Uanis(Au1) = Uanis(Ag1)
Uanis(Au2) = Uanis(Ag2)
Uanis(Au3) = Uanis(Ag3)
Uanis(Au6) = Uanis(Ag6)
Uanis(Au11) = Uanis(Ag11)
Uanis(Au10) = Uanis(Ag10)
Uanis(Au12) = Uanis(Ag12)
Uanis(Au9) = Uanis(Ag9)
Uanis(Au7) = Uanis(Ag7)
Uanis(Au8) = Uanis(Ag8)
Uanis(Au4) = Uanis(Ag4)
Uanis(Au5) = Uanis(Ag5)
Uanis(Ag13) = Uanis(Au13)
Uanis(Ag14) = Uanis(Au14)
Uanis(Ag15) = Uanis(Au15)
Uanis(Ag16) = Uanis(Au16)
Uanis(Ag17) = Uanis(Au17)
Uanis(Ag18) = Uanis(Au18)
Uanis(Ag19) = Uanis(Au19)
Uanis(Ag20) = Uanis(Au20)
Uanis(Ag24) = Uanis(Au24)
Uanis(Ag23) = Uanis(Au23)
Uanis(Ag22) = Uanis(Au22)
Uanis(Ag21) = Uanis(Au21)
4. Others
 Sof(Ag1)=1-FVAR(1)
 Sof(Au1)=FVAR(1)
 Sof(Ag2)=1-FVAR(2)
 Sof(Au2)=FVAR(2)
 Sof(Ag3)=1-FVAR(3)
 Sof(Au3)=FVAR(3)
 Sof(Ag4)=1-FVAR(4)
 Sof(Au4)=FVAR(4)
 Sof(Ag5)=1-FVAR(5)
 Sof(Au5)=FVAR(5)
 Sof(Ag6)=1-FVAR(6)
 Sof(Au6)=FVAR(6)
 Sof(Ag11)=1-FVAR(7)
 Sof(Au7)=FVAR(7)
 Sof(Ag10)=1-FVAR(8)
 Sof(Au8)=FVAR(8)
 Sof(Ag12)=1-FVAR(9)
 Sof(Au9)=FVAR(9)
 Sof(Ag9)=1-FVAR(10)
 Sof(Au10)=FVAR(10)
 Sof(Ag7)=1-FVAR(11)
 Sof(Au11)=FVAR(11)
 Sof(Ag8)=1-FVAR(12)
 Sof(Au12)=FVAR(12)
 Sof(Au13)=1-FVAR(13)
 Sof(Ag13)=FVAR(13)
 Sof(Au14)=1-FVAR(14)
 Sof(Ag14)=FVAR(14)
 Sof(Au15)=1-FVAR(15)
 Sof(Ag15)=FVAR(15)
 Sof(Au16)=1-FVAR(16)
 Sof(Ag16)=FVAR(16)
 Sof(Au17)=1-FVAR(17)
 Sof(Ag17)=FVAR(17)
 Sof(Au18)=1-FVAR(18)
 Sof(Ag18)=FVAR(18)
 Sof(Au19)=1-FVAR(19)
 Sof(Ag19)=FVAR(19)
 Sof(Au20)=1-FVAR(20)
 Sof(Ag20)=FVAR(20)
 Sof(Au21)=1-FVAR(21)
 Sof(Ag21)=FVAR(21)
 Sof(Au22)=1-FVAR(22)
 Sof(Ag22)=FVAR(22)
 Sof(Au23)=1-FVAR(23)
 Sof(Ag23)=FVAR(23)
 Sof(Au24)=1-FVAR(24)
 Sof(Ag24)=FVAR(24)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B)
5.b Aromatic/amide H refined with riding coordinates:
 C54(H54), C55(H55), C57(H57), C62(H62), C63(H63), C65(H65), C70(H70),
 C71(H71), C73(H73), C78(H78), C79(H79), C81(H81), C86(H86), C87(H87), C89(H89),
  C94(H94), C95(H95), C97(H97), C102(H102), C103(H103), C105(H105), C110(H110),
 C111(H111), C113(H113), C118(H118), C119(H119), C121(H121), C126(H126),
 C127(H127), C129(H129), C134(H134), C135(H135), C137(H137), C142(H142),
 C143(H143), C145(H145), C150(H150), C151(H151), C153(H153), C158(H158),
 C159(H159), C161(H161), C166(H166), C167(H167), C169(H169), C174(H174),
 C175(H175), C177(H177), C182(H182), C183(H183), C185(H185), C190(H190),
 C191(H191), C193(H193), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30),
 C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39),
  C40(H40), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48),
 C49(H49), C50(H50), C51(H51), C52(H52)
5.c Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C67(H67A,H67B,H67C), C68(H68A,H68B,
 H68C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C83(H83A,H83B,H83C), C84(H84A,
 H84B,H84C), C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C99(H99A,H99B,H99C),
 C100(H10A,H10B,H10C), C107(H10D,H10E,H10F), C108(H10G,H10H,H10I), C115(H11A,
 H11B,H11C), C116(H11D,H11E,H11F), C123(H12A,H12B,H12C), C124(H12D,H12E,H12F),
 C131(H13A,H13B,H13C), C132(H13D,H13E,H13F), C139(H13G,H13H,H13I), C140(H14A,
 H14B,H14C), C147(H14D,H14E,H14F), C148(H14G,H14H,H14I), C155(H15A,H15B,H15C),
 C156(H15D,H15E,H15F), C163(H16A,H16B,H16C), C164(H16D,H16E,H16F), C171(H17A,
 H17B,H17C), C172(H17D,H17E,H17F), C179(H17G,H17H,H17I), C180(H18A,H18B,H18C),
 C187(H18D,H18E,H18F), C188(H18G,H18H,H18I), C195(H19A,H19B,H19C), C196(H19D,
 H19E,H19F)
;
_shelx_res_checksum              29193
_shelx_fab_checksum              28194
_olex2_submission_special_instructions 'No special instructions were received'