Gram-Scale Preparation of Stable Hydride M@Cu<sub>24</sub> (M = Au/Cu) Nanoclusters.
Chen, Along; Kang, Xi; Jin, Shan; Du, Wenjun; Wang, Shuxin; Zhu, Manzhou; The journal of physical chemistry letters 10 (2019) 6124–6128; doi:10.1021/acs.jpclett.9b02297

data_8000392
_publ_section_title
;
 Gram-Scale Preparation of Stable Hydride M@Cu<sub>24</sub> (M = Au/Cu)
 Nanoclusters.
;
_journal_issue                   20
_journal_name_full               'The journal of physical chemistry letters'
_journal_page_first              6124
_journal_page_last               6128
_journal_paper_doi               10.1021/acs.jpclett.9b02297
_journal_volume                  10
_journal_year                    2019
_chemical_formula_moiety         '2(C108 H72 Au0.5 Cu12 F18 P6)'
_chemical_formula_sum            'C216 H144 Au Cu24 F36 P12'
_chemical_formula_weight         5516.87
_space_group_crystal_system      orthorhombic
_space_group_IT_number           30
_space_group_name_Hall           'P 2 -2bc'
_space_group_name_H-M_alt        'P n c 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-13 deposited with the CCDC.	2019-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.5313(12)
_cell_length_b                   22.4275(9)
_cell_length_c                   32.5487(14)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    170
_cell_measurement_theta_max      24.58
_cell_measurement_theta_min      2.17
_cell_volume                     25207.4(17)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0954
_diffrn_reflns_av_unetI/netI     0.1257
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            109788
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.083
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.700
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0932 before and 0.0688 after correction. The Ratio of minimum to maximum transmission is 0.7276. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             10876
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         8.943
_refine_diff_density_min         -1.540
_refine_diff_density_rms         0.205
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.436(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2136
_refine_ls_number_reflns         41384
_refine_ls_number_restraints     5005
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.1369
_refine_ls_R_factor_gt           0.0758
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1283P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1897
_refine_ls_wR_factor_ref         0.2154
_reflns_Friedel_coverage         0.961
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                23898
_reflns_number_total             41384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jz9b02297_si_003.cif
_cod_data_source_block           20190312c_0m
_cod_database_code               8000392
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.774
_shelx_estimated_absorpt_t_min   0.774
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.564(9)
 0.436(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
C5 \\sim C16 \\sim C49 \\sim C26 \\sim C9FA \\sim C42 \\sim C10 \\sim C123
\\sim C156 \\sim C105 \\sim C192 \\sim C72 \\sim C11 \\sim C1AA \\sim C57 \\sim
C70 \\sim C69 \\sim C0AA \\sim C15 \\sim C46 \\sim C67 \\sim C1BA \\sim C43
\\sim C17 \\sim C22 \\sim C115 \\sim C7BA \\sim C8BA \\sim C0CA \\sim C9BA
\\sim C27 \\sim C93 \\sim C5DA \\sim C5AA \\sim C128 \\sim C98 \\sim C29 \\sim
C50 \\sim C191 \\sim C8AA \\sim C124 \\sim C52 \\sim C34 \\sim C176 \\sim C140
\\sim C186 \\sim C136 \\sim C150 \\sim C36 \\sim C48 \\sim C0FA \\sim C9EA
\\sim C8EA \\sim C1FA \\sim C44 \\sim C80 \\sim C2DA \\sim C122 \\sim C1DA
\\sim C91 \\sim C51 \\sim C189 \\sim C4FA \\sim C59 \\sim C3FA \\sim C2FA \\sim
C53 \\sim C68 \\sim C77 \\sim C134 \\sim C163 \\sim C94 \\sim C55 \\sim C175
\\sim C187 \\sim C81 \\sim C138 \\sim C33 \\sim C56 \\sim C3DA \\sim C132 \\sim
C4DA \\sim C83 \\sim C97 \\sim C62 \\sim C76 \\sim C147 \\sim C89 \\sim C146
\\sim C190 \\sim C74 \\sim C168 \\sim C162 \\sim C84 \\sim C181 \\sim C121
\\sim C75 \\sim C73 \\sim C3AA \\sim C4EA \\sim C155 \\sim C107 \\sim C79 \\sim
C199 \\sim C3CA \\sim C5EA \\sim C78 \\sim C118 \\sim C99 \\sim C154 \\sim C130
\\sim C2AA \\sim C103 \\sim C54 \\sim C8 \\sim C71 \\sim C117 \\sim C5CA \\sim
C180 \\sim C113 \\sim C19 \\sim C173 \\sim C2EA \\sim C1EA \\sim C0EA \\sim
C127 \\sim C61 \\sim C95 \\sim C66 \\sim C58 \\sim C6CA \\sim C87 \\sim C64
\\sim C182 \\sim C65 \\sim C38 \\sim C1CA \\sim C60 \\sim C3BA \\sim C144 \\sim
C188 \\sim C7EA \\sim C159 \\sim C126 \\sim C133 \\sim C32 \\sim C88 \\sim C4CA
\\sim C139 \\sim C119 \\sim C135 \\sim C0BA \\sim C82 \\sim C109 \\sim C9AA
\\sim C25 \\sim C137 \\sim C198 \\sim C172 \\sim C63 \\sim C4GA \\sim C92 \\sim
C145 \\sim C116 \\sim C2BA \\sim C112 \\sim C129 \\sim C148 \\sim C153 \\sim
C110 \\sim C114 \\sim C7AA \\sim C6AA \\sim C104 \\sim C174 \\sim C141 \\sim
C3EA \\sim C177 \\sim C169 \\sim C111 \\sim C183 \\sim C4AA \\sim C131 \\sim
C142 \\sim C9DA \\sim C184 \\sim C7CA \\sim C8CA \\sim C6EA \\sim C2CA \\sim
C0DA \\sim C9CA \\sim C102 \\sim C5BA \\sim C6BA \\sim C4BA \\sim C166 \\sim
C90 \\sim C23 \\sim C6DA \\sim C6GA \\sim C35 \\sim C41 \\sim C7DA \\sim C12
\\sim C5FA \\sim C5GA \\sim C8FA \\sim C7FA \\sim C6FA \\sim C0GA \\sim C47
\\sim C31 \\sim C3GA \\sim C2GA \\sim C1GA: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(F36) = Uanis(C4DA)
Uanis(F0AA) = Uanis(C5CA)
Uanis(F42) = Uanis(C4CA)
Uanis(F6AA) = Uanis(C9EA)
Uanis(F13) = Uanis(C63)
Uanis(F55) = Uanis(C112)
4.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C49(H49), C9FA(H9FA), C42(H42), C123(H123), C156(H156), C192(H192),
 C72(H72), C1AA(H1AA), C57(H57), C69(H69), C0AA(H0AA), C46(H46), C67(H67),
 C43(H43), C17(H17), C115(H115), C7BA(H7BA), C0CA(H0CA), C9BA(H9BA), C93(H93),
 C5DA(H5DA), C128(H128), C98(H98), C50(H50), C191(H191), C124(H124), C52(H52),
 C176(H176), C140(H140), C136(H136), C150(H150), C48(H48), C0FA(H0FA),
 C8EA(H8EA), C1FA(H1FA), C80(H80), C2DA(H2DA), C1DA(H1DA), C91(H91), C189(H189),
  C4FA(H4FA), C3FA(H3FA), C2FA(H2FA), C68(H68), C77(H77), C163(H163), C94(H94),
 C175(H175), C187(H187), C138(H138), C33(H33), C3DA(H3DA), C132(H132), C83(H83),
  C97(H97), C76(H76), C147(H147), C146(H146), C190(H190), C168(H168),
 C162(H162), C181(H181), C121(H121), C73(H73), C3AA(H3AA), C155(H155),
 C107(H107), C199(H199), C3CA(H3CA), C78(H78), C118(H118), C154(H154),
 C130(H130), C103(H103), C54(H54), C71(H71), C117(H117), C180(H180), C113(H113),
  C173(H173), C2EA(H2EA), C0EA(H0EA), C127(H127), C95(H95), C66(H66),
 C6CA(H6CA), C87(H87), C182(H182), C65(H65), C1CA(H1CA), C60(H60), C3BA(H3BA),
 C188(H188), C7EA(H7EA), C126(H126), C32(H32), C88(H88), C139(H139), C119(H119),
  C0BA(H0BA), C82(H82), C9AA(H9AA), C25(H25), C198(H198), C172(H172),
 C4GA(H4GA), C92(H92), C116(H116), C2BA(H2BA), C129(H129), C148(H148),
 C110(H110), C114(H114), C6AA(H6AA), C104(H104), C141(H141), C3EA(H3EA),
 C169(H169), C111(H111), C4AA(H4AA), C131(H131), C9DA(H9DA), C184(H184),
 C8CA(H8CA), C6EA(H6EA), C0DA(H0DA), C9CA(H9CA), C102(H102), C5BA(H5BA),
 C4BA(H4BA), C166(H166), C6DA(H6DA), C6GA(H6GA), C41(H41), C7DA(H7DA),
 C5FA(H5FA), C5GA(H5GA), C7FA(H7FA), C6FA(H6FA), C47(H47), C31(H31), C2GA(H2GA),
  C1GA(H1GA)
4.b Fitted hexagon refined as free rotating group:
 C5(C16,C49,C26,C9FA,C42), C10(C123,C156,C105,C192,C72), C11(C1AA,C57,C70,C69,
 C0AA), C15(C46,C67,C1BA,C43,C17), C22(C115,C7BA,C8BA,C0CA,C9BA), C27(C93,C5DA,
 C5AA,C128,C98), C29(C50,C191,C8AA,C124,C52), C34(C176,C140,C186,C136,C150),
 C36(C48,C0FA,C9EA,C8EA,C1FA), C44(C80,C2DA,C122,C1DA,C91), C51(C189,C4FA,C59,
 C3FA,C2FA), C53(C68,C77,C134,C163,C94), C55(C175,C187,C81,C138,C33), C56(C3DA,
 C132,C4DA,C83,C97), C62(C76,C147,C89,C146,C190), C74(C168,C162,C84,C181,C121),
 C75(C73,C3AA,C4EA,C155,C107), C79(C199,C3CA,C5EA,C78,C118), C99(C154,C130,C2AA,
 C103,C54), C8(C71,C117,C5CA,C180,C113), C19(C173,C2EA,C1EA,C0EA,C127), C61(C95,
 C66,C58,C6CA,C87), C64(C182,C65,C38,C1CA,C60), C3BA(C144,C188,C7EA,C159,C126),
 C133(C32,C88,C4CA,C139,C119), C135(C0BA,C82,C109,C9AA,C25), C137(C198,C172,C63,
 C4GA,C92), C145(C116,C2BA,C112,C129,C148), C153(C110,C114,C7AA,C6AA,C104),
 C174(C141,C3EA,C177,C169,C111), C183(C4AA,C131,C142,C9DA,C184), C7CA(C8CA,C6EA,
 C2CA,C0DA,C9CA), C102(C5BA,C6BA,C4BA,C166,C90), C23(C6DA,C6GA,C35,C41,C7DA),
 C12(C5FA,C5GA,C8FA,C7FA,C6FA), C0GA(C47,C31,C3GA,C2GA,C1GA)
;
_shelx_res_checksum              12776
_shelx_hkl_checksum              39347
_shelx_fab_checksum              59629
_olex2_submission_special_instructions 'No special instructions were received'