In Situ Two-Phase Ligand Exchange: A New Method for the Synthesis of Alloy Nanoclusters with Precise Atomic Structures.
Yang, Sha; Chai, Jinsong; Song, Yongbo; Fan, Jiqiang; Chen, Tao; Wang, Shuxin; Yu, Haizhu; Li, Xiaowu; Zhu, Manzhou; Journal of the American Chemical Society 139 (2017) 5668–5671; doi:10.1021/jacs.7b00668

data_4125915
_publ_section_title
;
 In Situ Two-Phase Ligand Exchange: A New Method for the Synthesis of
 Alloy Nanoclusters with Precise Atomic Structures.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5668
_journal_page_last               5671
_journal_paper_doi               10.1021/jacs.7b00668
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C60 H135 Au20.66 Cu0.34 S15'
_chemical_formula_sum            'C60 H135 Au20.65 Cu0.35 S15'
_chemical_formula_weight         5427.17
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-03-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                102.605(2)
_cell_angle_beta                 97.567(2)
_cell_angle_gamma                99.053(2)
_cell_formula_units_Z            2
_cell_length_a                   14.6485(14)
_cell_length_b                   15.5804(15)
_cell_length_c                   27.395(3)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    130
_cell_measurement_theta_max      29.80
_cell_measurement_theta_min      2.29
_cell_volume                     5935.6(10)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      130.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0832
_diffrn_reflns_av_unetI/netI     0.1364
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            40519
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.499
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         0.773
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    25.753
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.2631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1639 before and 0.0718 after correction.
The Ratio of minimum to maximum transmission is 0.3527.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.037
_exptl_crystal_description       block
_exptl_crystal_F_000             4753
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         10.033
_refine_diff_density_min         -13.253
_refine_diff_density_rms         0.840
_refine_ls_extinction_coef       0.000049(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     912
_refine_ls_number_reflns         22009
_refine_ls_number_restraints     576
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1169
_refine_ls_R_factor_gt           0.0867
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1365P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2134
_refine_ls_wR_factor_ref         0.2362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14907
_reflns_number_total             22009
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00668_si_004.cif
_cod_data_source_block           mo_dm16336_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 4125915.cif.
;
_cod_database_code               4125915
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.060
_shelx_estimated_absorpt_t_min   0.043
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Au, Cu}
3. Uiso/Uaniso restraints and constraints
C41 \\sim C42 \\sim C43 \\sim C44: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(S2) \\sim Ueq, Uanis(S6) \\sim Ueq, Uanis(S1) \\sim Ueq, Uanis(S7) \\sim
Ueq, Uanis(S11) \\sim Ueq, Uanis(S8) \\sim Ueq, Uanis(S15) \\sim Ueq,
Uanis(S13) \\sim Ueq, Uanis(S9) \\sim Ueq, Uanis(S3) \\sim Ueq, Uanis(S10)
\\sim Ueq, Uanis(S14) \\sim Ueq, Uanis(S5) \\sim Ueq, Uanis(S4) \\sim Ueq,
Uanis(S12) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.01
Uanis(C30) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C26) \\sim Ueq,
Uanis(C5) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(C41) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C45) \\sim Ueq,
Uanis(C47) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C53)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C48) \\sim Ueq,
Uanis(C36) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C8) \\sim Ueq,
Uanis(C59) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C58) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C55)
\\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C9) \\sim Ueq,
Uanis(C60) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C11) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(Au8) \\sim Ueq, Uanis(Au15) \\sim Ueq, Uanis(Au14) \\sim Ueq, Uanis(Au1)
\\sim Ueq, Uanis(Au21) \\sim Ueq, Uanis(Au20) \\sim Ueq, Uanis(Au11) \\sim Ueq,
Uanis(Au13) \\sim Ueq, Uanis(Au2) \\sim Ueq: with sigma of 0.0005 and sigma for
terminal atoms of 0.001
Uanis(Au1) \\sim Ueq, Uanis(Au5) \\sim Ueq, Uanis(Au2) \\sim Ueq, Uanis(Au15)
\\sim Ueq, Uanis(Au4) \\sim Ueq, Uanis(Au16) \\sim Ueq, Uanis(Au7) \\sim Ueq,
Uanis(Au20) \\sim Ueq, Uanis(Au21) \\sim Ueq, Uanis(Au8) \\sim Ueq, Uanis(Au11)
\\sim Ueq, Uanis(Au14) \\sim Ueq, Uanis(Au19) \\sim Ueq, Uanis(Au6) \\sim Ueq,
Uanis(Au9) \\sim Ueq, Uanis(Au13) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(Au16) \\sim Ueq: with sigma of 0.0002 and sigma for terminal atoms of
0.0004
Uanis(Au) \\sim Ueq, Uanis(Au17) \\sim Ueq: with sigma of 0.0005 and sigma for
terminal atoms of 0.001
Uanis(Au) = Uanis(Cu)
4. Others
 Sof(Cu)=1-FVAR(1)
 Sof(Au)=FVAR(1)
5.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,
 H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C),
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,
 H56B,H56C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C)
;
_shelx_res_checksum              14409
_shelx_hkl_checksum              85735
_shelx_fab_checksum              98586
_olex2_submission_special_instructions 'No special instructions were received'