Crystal Structures of Two New Gold-Copper Bimetallic Nanoclusters: CuxAu25-x(PPh3)10(PhC2H4S)5Cl2(2+) and Cu3Au34(PPh3)13((t)BuPhCH2S)6S2(3).
Yang, Sha; Chai, Jinsong; Chen, Tao; Rao, Bo; Pan, Yiting; Yu, Haizhu; Zhu, Manzhou; Inorganic chemistry 56 (2017) 1771–1774; doi:10.1021/acs.inorgchem.6b02016

data_4345356
_publ_section_title
;
 Crystal Structures of Two New Gold-Copper Bimetallic Nanoclusters:
 CuxAu25-x(PPh3)10(PhC2H4S)5Cl2(2+) and
 Cu3Au34(PPh3)13((t)BuPhCH2S)6S2(3).
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1771
_journal_page_last               1774
_journal_paper_doi               10.1021/acs.inorgchem.6b02016
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety
'C220 H196 Au21.23 Cl2 Cu3.77 P10 S5, 2(F6 Sb)'
_chemical_formula_sum            'C220 H196 Au21.23 Cl2 Cu3.77 F12 P10 S5 Sb2'
_chemical_formula_weight         8273.30
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.170(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.159(6)
_cell_length_b                   22.308(4)
_cell_length_c                   34.068(7)
_cell_measurement_reflns_used    9717
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.09
_cell_measurement_theta_min      2.21
_cell_volume                     22744(8)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1793
_diffrn_reflns_av_unetI/netI     0.1939
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            171386
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.330
_diffrn_reflns_theta_min         1.541
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.405
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.3382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1561 before and 0.0684 after correction.
The Ratio of minimum to maximum transmission is 0.4537.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.416
_exptl_crystal_description       block
_exptl_crystal_F_000             15106
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.278
_refine_diff_density_min         -3.364
_refine_diff_density_rms         0.455
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2462
_refine_ls_number_reflns         46800
_refine_ls_number_restraints     1656
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.1966
_refine_ls_R_factor_gt           0.0855
_refine_ls_shift/su_max          0.077
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0989P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1824
_refine_ls_wR_factor_ref         0.2140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21546
_reflns_number_total             46800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02016_si_002.cif
_cod_data_source_block           20151121b_0m
_cod_original_cell_volume        22743(8)
_cod_database_code               4345356
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Au24, Cu24}
{Au25, Cu25}
{Au1, Cu1}
{Au2, Cu2}
{Au3, Cu3}
{Au4, Cu4}
{Au5, Cu5}
{Au6, Cu6}
{Au7, Cu7}
{Au8, Cu8}
{Au9, Cu9}
{Au10, Cu10}
{Au11, Cu11}
3. Uiso/Uaniso restraints and constraints
C11 \\sim C16: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C1 \\sim C2 \\sim C3 \\sim C8: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.01
C173 \\sim C174 \\sim C175 \\sim C176 \\sim C177 \\sim C178: within 1.7A with
sigma of 0.005 and sigma for terminal atoms of 0.01
C179 \\sim C180 \\sim C181 \\sim C182 \\sim C183 \\sim C184: within 1.7A with
sigma of 0.005 and sigma for terminal atoms of 0.01
C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
C9 \\sim C10 \\sim C11 \\sim C16 \\sim C15 \\sim C14 \\sim C13 \\sim C12:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
F5 \\sim Sb1 \\sim F7 \\sim F2 \\sim F1 \\sim F4 \\sim F3: within 2A with sigma
of 0.005 and sigma for terminal atoms of 0.01
Sb2 \\sim F9 \\sim F11 \\sim F10 \\sim F12 \\sim F8 \\sim F13: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim
Ueq, Uanis(F5) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9)
\\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq,
Uanis(F13) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(P1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq,
Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq,
Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50)
\\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq,
Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq,
Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq,
Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71)
\\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq,
Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78)
\\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq,
Uanis(C82) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C85)
\\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C88) \\sim Ueq,
Uanis(C89) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C92)
\\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C95) \\sim Ueq,
Uanis(C96) \\sim Ueq, Uanis(C97) \\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C99)
\\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq,
Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C105) \\sim Ueq,
Uanis(C106) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C108) \\sim Ueq,
Uanis(C109) \\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(C111) \\sim Ueq,
Uanis(C112) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C114) \\sim Ueq,
Uanis(C115) \\sim Ueq, Uanis(C116) \\sim Ueq, Uanis(C117) \\sim Ueq,
Uanis(C118) \\sim Ueq, Uanis(C119) \\sim Ueq, Uanis(C120) \\sim Ueq,
Uanis(C121) \\sim Ueq, Uanis(C122) \\sim Ueq, Uanis(C123) \\sim Ueq,
Uanis(C124) \\sim Ueq, Uanis(C125) \\sim Ueq, Uanis(C126) \\sim Ueq,
Uanis(C127) \\sim Ueq, Uanis(C128) \\sim Ueq, Uanis(C129) \\sim Ueq,
Uanis(C130) \\sim Ueq, Uanis(C131) \\sim Ueq, Uanis(C132) \\sim Ueq,
Uanis(C133) \\sim Ueq, Uanis(C134) \\sim Ueq, Uanis(C135) \\sim Ueq,
Uanis(C136) \\sim Ueq, Uanis(C137) \\sim Ueq, Uanis(C138) \\sim Ueq,
Uanis(C139) \\sim Ueq, Uanis(C140) \\sim Ueq, Uanis(C141) \\sim Ueq,
Uanis(C142) \\sim Ueq, Uanis(C143) \\sim Ueq, Uanis(C144) \\sim Ueq,
Uanis(C145) \\sim Ueq, Uanis(C146) \\sim Ueq, Uanis(C147) \\sim Ueq,
Uanis(C148) \\sim Ueq, Uanis(C149) \\sim Ueq, Uanis(C150) \\sim Ueq,
Uanis(C151) \\sim Ueq, Uanis(C152) \\sim Ueq, Uanis(C153) \\sim Ueq,
Uanis(C154) \\sim Ueq, Uanis(C155) \\sim Ueq, Uanis(C156) \\sim Ueq,
Uanis(C157) \\sim Ueq, Uanis(C158) \\sim Ueq, Uanis(C159) \\sim Ueq,
Uanis(C160) \\sim Ueq, Uanis(C161) \\sim Ueq, Uanis(C162) \\sim Ueq,
Uanis(C163) \\sim Ueq, Uanis(C164) \\sim Ueq, Uanis(C165) \\sim Ueq,
Uanis(C166) \\sim Ueq, Uanis(C167) \\sim Ueq, Uanis(C168) \\sim Ueq,
Uanis(C169) \\sim Ueq, Uanis(C170) \\sim Ueq, Uanis(C171) \\sim Ueq,
Uanis(C172) \\sim Ueq, Uanis(C173) \\sim Ueq, Uanis(C174) \\sim Ueq,
Uanis(C175) \\sim Ueq, Uanis(C176) \\sim Ueq, Uanis(C177) \\sim Ueq,
Uanis(C178) \\sim Ueq, Uanis(C179) \\sim Ueq, Uanis(C180) \\sim Ueq,
Uanis(C181) \\sim Ueq, Uanis(C182) \\sim Ueq, Uanis(C183) \\sim Ueq,
Uanis(C184) \\sim Ueq, Uanis(C185) \\sim Ueq, Uanis(C186) \\sim Ueq,
Uanis(C187) \\sim Ueq, Uanis(C188) \\sim Ueq, Uanis(C189) \\sim Ueq,
Uanis(C190) \\sim Ueq, Uanis(C191) \\sim Ueq, Uanis(C192) \\sim Ueq,
Uanis(C193) \\sim Ueq, Uanis(C194) \\sim Ueq, Uanis(C195) \\sim Ueq,
Uanis(C196) \\sim Ueq, Uanis(C197) \\sim Ueq, Uanis(C198) \\sim Ueq,
Uanis(C199) \\sim Ueq, Uanis(C200) \\sim Ueq, Uanis(C201) \\sim Ueq,
Uanis(C202) \\sim Ueq, Uanis(C203) \\sim Ueq, Uanis(C204) \\sim Ueq,
Uanis(C205) \\sim Ueq, Uanis(C206) \\sim Ueq, Uanis(C207) \\sim Ueq,
Uanis(C208) \\sim Ueq, Uanis(C209) \\sim Ueq, Uanis(C210) \\sim Ueq,
Uanis(C211) \\sim Ueq, Uanis(C212) \\sim Ueq, Uanis(C213) \\sim Ueq,
Uanis(C214) \\sim Ueq, Uanis(C215) \\sim Ueq, Uanis(C216) \\sim Ueq,
Uanis(C217) \\sim Ueq, Uanis(C218) \\sim Ueq, Uanis(C219) \\sim Ueq,
Uanis(C220) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(P2) \\sim Ueq, Uanis(P1) \\sim Ueq, Uanis(P4) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(Au24) = Uanis(Cu24)
Uanis(Au25) = Uanis(Cu25)
Uanis(Au1) = Uanis(Cu1)
Uanis(Au2) = Uanis(Cu2)
Uanis(Au3) = Uanis(Cu3)
Uanis(Au4) = Uanis(Cu4)
Uanis(Au5) = Uanis(Cu5)
Uanis(Au6) = Uanis(Cu6)
Uanis(Au7) = Uanis(Cu7)
Uanis(Au8) = Uanis(Cu8)
Uanis(Au9) = Uanis(Cu9)
Uanis(Au10) = Uanis(Cu10)
Uanis(Au11) = Uanis(Cu11)
4. Others
 Sof(Cu1)=Sof(Cu2)=Sof(Cu3)=Sof(Cu4)=Sof(Cu5)=Sof(Cu6)=Sof(Cu7)=Sof(Cu8)=
 Sof(Cu9)=Sof(Cu10)=Sof(Cu11)=1-FVAR(1)
 Sof(Au1)=Sof(Au2)=Sof(Au3)=Sof(Au4)=Sof(Au5)=Sof(Au6)=Sof(Au7)=Sof(Au8)=
 Sof(Au9)=Sof(Au10)=Sof(Au11)=FVAR(1)
 Fixed Sof: Au24(0.5) Au25(0.5) Cu24(0.5) Cu25(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C9(H9A,H9B), C10(H10A,H10B), C17(H17A,H17B),
 C18(H18A,H18B), C25(H25A,H25B), C26(H26A,H26B), C33(H33A,H33B), C34(H34A,H34B),
  C58(H58A,H58B)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C6(H6), C5(H5), C4(H4), C16(H16), C15(H15), C14(H14),
 C13(H13), C12(H12), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C28(H28),
  C29(H29), C30(H30), C31(H31), C32(H32), 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), C54(H54), C55(H55), C56(H56),
 C57(H57), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C66(H66), C67(H67),
  C68(H68), C69(H69), C70(H70), C72(H72), C73(H73), C74(H74), C75(H75),
 C76(H76), C78(H78), C79(H79), C80(H80), C81(H81), C82(H82), C84(H84), C85(H85),
  C86(H86), C87(H87), C88(H88), C90(H90), C91(H91), C92(H92), C93(H93),
 C94(H94), C96(H96), C97(H97), C98(H98), C99(H99), C100(H100), C102(H102),
 C103(H103), C104(H104), C105(H105), C106(H106), C108(H108), C109(H109),
 C110(H110), C111(H111), C112(H112), C114(H114), C115(H115), C116(H116),
 C117(H117), C118(H118), C120(H120), C121(H121), C122(H122), C123(H123),
 C124(H124), C126(H126), C127(H127), C128(H128), C129(H129), C130(H130),
 C132(H132), C133(H133), C134(H134), C135(H135), C136(H136), C138(H138),
 C139(H139), C140(H140), C141(H141), C142(H142), C144(H144), C145(H145),
 C146(H146), C147(H147), C148(H148), C150(H150), C151(H151), C152(H152),
 C153(H153), C154(H154), C156(H156), C157(H157), C158(H158), C159(H159),
 C160(H160), C162(H162), C163(H163), C164(H164), C165(H165), C166(H166),
 C168(H168), C169(H169), C170(H170), C171(H171), C172(H172), C174(H174),
 C175(H175), C176(H176), C177(H177), C178(H178), C180(H180), C181(H181),
 C182(H182), C183(H183), C184(H184), C186(H186), C187(H187), C188(H188),
 C189(H189), C190(H190), C192(H192), C193(H193), C194(H194), C195(H195),
 C196(H196), C198(H198), C199(H199), C200(H200), C201(H201), C202(H202),
 C204(H204), C205(H205), C206(H206), C207(H207), C208(H208), C210(H210),
 C211(H211), C212(H212), C213(H213), C214(H214), C216(H216), C217(H217),
 C218(H218), C219(H219), C220(H220)
5.c Fitted hexagon refined as free rotating group:
 C3(C8,C7,C6,C5,C4), C11(C16,C15,C14,C13,C12)
;
_shelx_res_checksum              68831
_shelx_hkl_checksum              19183
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'