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_4345082
_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         'C300 H285 Au34 Cu3 P13 S8, 3(F6 Sb)'
_chemical_formula_sum            'C300 H285 Au34 Cu3 F18 P13 S8 Sb3'
_chemical_formula_weight         12144.08
_chemical_name_common            a
_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             2015-10-10
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.2650(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.020(3)
_cell_length_b                   23.988(2)
_cell_length_c                   45.263(4)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.86
_cell_measurement_theta_min      2.17
_cell_volume                     35435(5)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.998
_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  0.2405
_diffrn_reflns_av_unetI/netI     0.2821
_diffrn_reflns_Laue_measured_fraction_full 0.945
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            273363
_diffrn_reflns_point_group_measured_fraction_full 0.945
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         0.635
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.568
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1384 before and 0.0708 after correction.
The Ratio of minimum to maximum transmission is 0.6878.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    2.276
_exptl_crystal_description       block
_exptl_crystal_F_000             21984
_refine_diff_density_max         6.673
_refine_diff_density_min         -5.989
_refine_diff_density_rms         0.440
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.895
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     3043
_refine_ls_number_reflns         65849
_refine_ls_number_restraints     2025
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.2248
_refine_ls_R_factor_gt           0.0997
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1422P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2388
_refine_ls_wR_factor_ref         0.2796
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25056
_reflns_number_total             65849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02016_si_003.cif
_cod_data_source_block           20150628a_0m
_cod_depositor_comments          'Adding full bibliography for 4345082.cif.'
_cod_original_cell_volume        35436(6)
_cod_database_code               4345082
_shelxl_version_number           2014-3
_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
{Cu1, Au32}
{Cu2, Au33}
{Cu3, Au34}
{Cu4, Au35}
{Cu5, Au36}
{Cu6, Au37}
3. Restrained distances
 C45-C46
 1.52 with sigma of 0.02
 C8-C10
 1.52 with sigma of 0.02
 C8-C11
 1.52 with sigma of 0.02
 C8-C9
 1.52 with sigma of 0.02
 C63-C64
 1.52 with sigma of 0.02
 C63-C66
 1.52 with sigma of 0.02
 C63-C65
 1.52 with sigma of 0.02
 C20-C19 = C21-C19 = C22-C19
 1.52 with sigma of 0.02
 C33-C30 = C32-C30 = C31-C30 = C30-C27 = C19-C16 = C8-C5 = C41-C38 = C63-C60
 1.52 with sigma of 0.02
 Sb2-F12 = Sb2-F11 = Sb2-F8 = Sb2-F7 = Sb2-F9 = Sb2-F10
 1.86 with sigma of 0.02
 Sb3-F14 = Sb3-F17 = Sb3-F16 = Sb3-F15 = Sb3-F13 = Sb3-F18
 1.86 with sigma of 0.02
 C44-C41 = C43-C41 = C42-C41
 1.52 with sigma of 0.02
 Sb4-F24 = Sb4-F22 = Sb4-F20 = Sb4-F19
 1.86 with sigma of 0.02
 C53-C52 = C55-C52 = C54-C52
 1.52 with sigma of 0.02
 Sb4-F23 = Sb4-F21
 1.86 with sigma of 0.01
 C10-C11 \\sim C11-C9 \\sim C10-C9 \\sim C20-C21 \\sim C21-C22 \\sim C20-C22
 with sigma of 0.02
 C66-C64 \\sim C64-C65 \\sim C66-C65
 with sigma of 0.02
 F14-F13 \\sim F14-F18 \\sim F14-F15 \\sim F16-F13 \\sim F16-F15 \\sim F16-F18
\\sim F16-F13
 with sigma of 0.01
 C42-C44 \\sim C42-C43 \\sim C43-C44
 with sigma of 0.01
 F10-F9 \\sim F10-F7 \\sim F10-F11 \\sim F10-F8 \\sim F12-F7 \\sim F12-F11
\\sim F12-F8 \\sim F12-F9
 with sigma of 0.01
 F20-F19 \\sim F20-F24 \\sim F22-F24 \\sim F22-F19 \\sim F17-F13 \\sim F17-F14
\\sim F17-F18 \\sim F17-F16
 with sigma of 0.02
 C53-C54 \\sim C54-C55 \\sim C53-C55
 with sigma of 0.01
 F21-F19 \\sim F21-F20 \\sim F21-F22 \\sim F21-F24 \\sim F23-F19 \\sim F23-F20
\\sim F23-F22 \\sim F23-F24
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C18 \\sim C17 \\sim C16 \\sim C15
\\sim C14 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C40 \\sim C39 \\sim C38 \\sim C37 \\sim C36 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89
\\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97
\\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103 \\sim C104
\\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim C114 \\sim C113
\\sim C112 \\sim C111 \\sim C110 \\sim C115 \\sim C120 \\sim C119 \\sim C118
\\sim C117 \\sim C116 \\sim C121 \\sim C126 \\sim C125 \\sim C124 \\sim C123
\\sim C122 \\sim C127 \\sim C128 \\sim C129 \\sim C130 \\sim C131 \\sim C132
\\sim C133 \\sim C134 \\sim C135 \\sim C136 \\sim C137 \\sim C138 \\sim C139
\\sim C144 \\sim C143 \\sim C142 \\sim C141 \\sim C140 \\sim C145 \\sim C146
\\sim C147 \\sim C148 \\sim C149 \\sim C150 \\sim C151 \\sim C152 \\sim C153
\\sim C154 \\sim C155 \\sim C156 \\sim C157 \\sim C162 \\sim C161 \\sim C160
\\sim C159 \\sim C158 \\sim C163 \\sim C164 \\sim C165 \\sim C166 \\sim C167
\\sim C168 \\sim C169 \\sim C170 \\sim C171 \\sim C172 \\sim C173 \\sim C174
\\sim C175 \\sim C176 \\sim C177 \\sim C178 \\sim C179 \\sim C180 \\sim C181
\\sim C186 \\sim C185 \\sim C184 \\sim C183 \\sim C182 \\sim C187 \\sim C188
\\sim C189 \\sim C190 \\sim C191 \\sim C192 \\sim C193 \\sim C198 \\sim C197
\\sim C196 \\sim C195 \\sim C194 \\sim C199 \\sim C204 \\sim C203 \\sim C202
\\sim C201 \\sim C200 \\sim C205 \\sim C206 \\sim C207 \\sim C208 \\sim C209
\\sim C210 \\sim C211 \\sim C212 \\sim C213 \\sim C214 \\sim C215 \\sim C216
\\sim C217 \\sim C218 \\sim C219 \\sim C220 \\sim C221 \\sim C222 \\sim C223
\\sim C224 \\sim C225 \\sim C226 \\sim C227 \\sim C228 \\sim C229 \\sim C234
\\sim C233 \\sim C232 \\sim C231 \\sim C230 \\sim C235 \\sim C240 \\sim C239
\\sim C238 \\sim C237 \\sim C236 \\sim C241 \\sim C246 \\sim C245 \\sim C244
\\sim C243 \\sim C242 \\sim C247 \\sim C252 \\sim C251 \\sim C250 \\sim C249
\\sim C248 \\sim C253 \\sim C258 \\sim C257 \\sim C256 \\sim C255 \\sim C254
\\sim C259 \\sim C260 \\sim C261 \\sim C262 \\sim C263 \\sim C264 \\sim C265
\\sim C266 \\sim C267 \\sim C268 \\sim C269 \\sim C270 \\sim C271 \\sim C272
\\sim C273 \\sim C274 \\sim C275 \\sim C276 \\sim C277 \\sim C278 \\sim C279
\\sim C280 \\sim C281 \\sim C282 \\sim C283 \\sim C284 \\sim C285 \\sim C286
\\sim C287 \\sim C288 \\sim C289 \\sim C290 \\sim C291 \\sim C292 \\sim C293
\\sim C294 \\sim C295 \\sim C300 \\sim C299 \\sim C298 \\sim C297: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01
F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F7 \\sim F8 \\sim F9
\\sim F10 \\sim F11 \\sim F12 \\sim F18 \\sim F15 \\sim F14 \\sim F13 \\sim F22
\\sim F19 \\sim F24 \\sim F16 \\sim F17 \\sim F20 \\sim F21 \\sim F23 \\sim Sb3
\\sim Sb4: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Cu1) = Uanis(Au32)
Uanis(Cu2) = Uanis(Au33)
Uanis(Cu3) = Uanis(Au34)
Uanis(Cu4) = Uanis(Au35)
Uanis(Cu5) = Uanis(Au36)
Uanis(Cu6) = Uanis(Au37)
5. Others
 Fixed Sof: Cu1(0.5) Au32(0.5) Cu2(0.5) Au33(0.5) Cu3(0.5) Au34(0.5) Cu4(0.5)
 Au35(0.5) Cu5(0.5) Au36(0.5) Cu6(0.5) Au37(0.5) Sb3(0.5) Sb4(0.5) F18(0.5)
 F15(0.5) F14(0.5) F13(0.5) F22(0.5) F19(0.5) F24(0.5) F16(0.5) F17(0.5)
 F20(0.5) F21(0.5) F23(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C12(H12A,H12B), C23(H23A,H23B), C34(H34A,H34B), C45(H45A,H45B),
 C56(H56A,H56B)
6.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22C,H22B,H22A), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C18(H18), C17(H17), C15(H15), C14(H14),
 C25(H25), C26(H26), C28(H28), C29(H29), C40(H40), C39(H39), C37(H37), C36(H36),
  C47(H47), C48(H48), C50(H50), C51(H51), C58(H58), C59(H59), C61(H61),
 C62(H62), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C74(H74), C75(H75),
  C76(H76), C77(H77), C78(H78), C80(H80), C81(H81), C82(H82), C83(H83),
 C84(H84), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C92(H92), C93(H93),
  C94(H94), C95(H95), C96(H96), C98(H98), C99(H99), C100(H100), C101(H101),
 C102(H102), C104(H104), C105(H105), C106(H106), C107(H107), C108(H108),
 C114(H114), C113(H113), C112(H112), C111(H111), C110(H110), C120(H120),
 C119(H119), C118(H118), C117(H117), C116(H116), C126(H126), C125(H125),
 C124(H124), C123(H123), C122(H122), C128(H128), C129(H129), C130(H130),
 C131(H131), C132(H132), C134(H134), C135(H135), C136(H136), C137(H137),
 C138(H138), C144(H144), C143(H143), C142(H142), C141(H141), C140(H140),
 C146(H146), C147(H147), C148(H148), C149(H149), C150(H150), C152(H152),
 C153(H153), C154(H154), C155(H155), C156(H156), C162(H162), C161(H161),
 C160(H160), C159(H159), C158(H158), C164(H164), C165(H165), C166(H166),
 C167(H167), C168(H168), C170(H170), C171(H171), C172(H172), C173(H173),
 C174(H174), C176(H176), C177(H177), C178(H178), C179(H179), C180(H180),
 C186(H186), C185(H185), C184(H184), C183(H183), C182(H182), C188(H188),
 C189(H189), C190(H190), C191(H191), C192(H192), C198(H198), C197(H197),
 C196(H196), C195(H195), C194(H194), C204(H204), C203(H203), C202(H202),
 C201(H201), C200(H200), C206(H206), C207(H207), C208(H208), C209(H209),
 C210(H210), C212(H212), C213(H213), C214(H214), C215(H215), C216(H216),
 C218(H218), C219(H219), C220(H220), C221(H221), C222(H222), C224(H224),
 C225(H225), C226(H226), C227(H227), C228(H228), C234(H234), C233(H233),
 C232(H232), C231(H231), C230(H230), C240(H240), C239(H239), C238(H238),
 C237(H237), C236(H236), C246(H246), C245(H245), C244(H244), C243(H243),
 C242(H242), C252(H252), C251(H251), C250(H250), C249(H249), C248(H248),
 C258(H258), C257(H257), C256(H256), C255(H255), C254(H254), C260(H260),
 C261(H261), C262(H262), C263(H263), C264(H264), C266(H266), C267(H267),
 C268(H268), C269(H269), C270(H270), C272(H272), C273(H273), C274(H274),
 C275(H275), C276(H276), C278(H278), C279(H279), C280(H280), C281(H281),
 C282(H282), C284(H284), C285(H285), C286(H286), C287(H287), C288(H288),
 C290(H290), C291(H291), C292(H292), C293(H293), C294(H294), C300(H300),
 C299(H299), C298(H298), C297(H297), C296(H296)
6.d Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7), C13(C18,C17,C16,C15,C14), C35(C40,C39,C38,C37,C36),
 C46(C47,C48,C49,C50,C51), C57(C58,C59,C60,C61,C62), C73(C74,C75,C76,C77,C78),
 C91(C92,C93,C94,C95,C96), C97(C98,C99,C100,C101,C102), C103(C104,C105,C106,
 C107,C108), C109(C114,C113,C112,C111,C110), C115(C120,C119,C118,C117,C116),
 C121(C126,C125,C124,C123,C122), C133(C134,C135,C136,C137,C138), C139(C144,C143,
 C142,C141,C140), C145(C146,C147,C148,C149,C150), C151(C152,C153,C154,C155,
 C156), C157(C162,C161,C160,C159,C158), C163(C164,C165,C166,C167,C168),
 C169(C170,C171,C172,C173,C174), C181(C186,C185,C184,C183,C182), C193(C198,C197,
 C196,C195,C194), C199(C204,C203,C202,C201,C200), C205(C206,C207,C208,C209,
 C210), C211(C212,C213,C214,C215,C216), C217(C218,C219,C220,C221,C222),
 C223(C224,C225,C226,C227,C228), C229(C234,C233,C232,C231,C230), C235(C240,C239,
 C238,C237,C236), C241(C246,C245,C244,C243,C242), C247(C252,C251,C250,C249,
 C248), C253(C258,C257,C256,C255,C254), C259(C260,C261,C262,C263,C264),
 C265(C266,C267,C268,C269,C270), C283(C284,C285,C286,C287,C288), C289(C290,C291,
 C292,C293,C294), C295(C300,C299,C298,C297,C296)
;
_shelx_res_checksum              77449
_shelx_hkl_checksum              83530
_olex2_submission_special_instructions 'No special instructions were received'