Single Ligand Exchange on an Au-Cu Bimetal Nanocluster and Mechanism
Song, Yongbo; Lv, Ying; Zhou, Meng; Luo, Tian-Yi; Zhao, Shuo; Rosi, Nathaniel L.; Yu, Haizhu; Zhu, Manzhou; Jin, Rongchao; Nanoscale  (2018) –; doi:10.1039/C8NR01611A

data_1549465
_publ_section_title
;
 Single Ligand Exchange on an Au-Cu Bimetal Nanocluster and Mechanism
;
_journal_name_full               Nanoscale
_journal_paper_doi               10.1039/C8NR01611A
_journal_year                    2018
_chemical_formula_moiety         'C105 H87 Au13 Cu4 N3 P3 Se9'
_chemical_formula_sum            'C105 H87 Au13 Cu4 N3 P3 Se9'
_chemical_formula_weight         5009.05
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2018-02-25 deposited with the CCDC.
2018-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   24.2592(6)
_cell_length_b                   24.2592(6)
_cell_length_c                   74.473(2)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      68.24
_cell_measurement_theta_min      3.17
_cell_volume                     37956.2(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      230.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8
_diffrn_detector_type            'APEX II CCD'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8 Prospector Ultra'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0898
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       89
_diffrn_reflns_limit_l_min       -88
_diffrn_reflns_number            86209
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.451
_diffrn_reflns_theta_min         2.415
_diffrn_source                   'IMuS micro-focus source'
_diffrn_source_target            Cu
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    31.860
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.3212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1747 before and 0.0874 after correction.
The Ratio of minimum to maximum transmission is 0.4265.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.630
_exptl_crystal_description       rod
_exptl_crystal_F_000             26784
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.052
_refine_diff_density_min         -3.787
_refine_diff_density_rms         0.416
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7764
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0960P)^2^+2952.5500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.2014
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5700
_reflns_number_total             7764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nr01611a2.cif
_cod_data_source_block           ltysyb20170226_0m_a
_cod_original_cell_volume        37956(2)
_cod_database_code               1549465
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.362
_shelx_estimated_absorpt_t_min   0.069
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C47 \\sim C52 \\sim C51 \\sim C50 \\sim C49 \\sim C48: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C26 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 C47, C52, C51, C50, C49, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26, C21, C22, C23, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
  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)
;
_shelx_res_checksum              62969
_olex2_submission_special_instructions 'No special instructions were received'