Diphosphine-protected ultrasmall gold nanoclusters: opened icosahedral Au<sub>13</sub> and heart-shaped Au<sub>8</sub> clusters.
Zhang, Shan-Shan; Feng, Lei; Senanayake, Ravithree D.; Aikens, Christine M.; Wang, Xing-Po; Zhao, Quan-Qin; Tung, Chen-Ho; Sun, Di; Chemical science 9 (2018) 1251–1258; doi:10.1039/c7sc03566g

data_1553987
_publ_section_title
;
 Diphosphine-protected ultrasmall gold nanoclusters: opened icosahedral
 Au<sub>13</sub> and heart-shaped Au<sub>8</sub> clusters.
;
_journal_issue                   5
_journal_name_full               'Chemical science'
_journal_page_first              1251
_journal_page_last               1258
_journal_paper_doi               10.1039/c7sc03566g
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C100 H88 Au8 P8 S2, 2(C H2 Cl2), 2(Cl)'
_chemical_formula_sum            'C102 H92 Au8 Cl6 P8 S2'
_chemical_formula_weight         3418.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_Hall           '-C 2a 2ac'
_space_group_name_H-M_alt        'C c c a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-02-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-10-02 deposited with the CCDC.
2017-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.105(6)
_cell_length_b                   29.820(7)
_cell_length_c                   28.748(6)
_cell_measurement_reflns_used    4065
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      22.524
_cell_measurement_theta_min      2.477
_cell_volume                     23236(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_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_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1300
_diffrn_reflns_av_unetI/netI     0.0899
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10236
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.97
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.385
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1256 before and 0.0714 after correction.
The Ratio of minimum to maximum transmission is 0.5200.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             12720
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.478
_refine_diff_density_min         -1.434
_refine_diff_density_rms         0.297
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         10236
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+979.5162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1549
_reflns_number_gt                6685
_reflns_number_total             10236
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7sc03566g2.cif
_cod_data_source_block           SD_Au2
_cod_original_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c e'
_cod_database_code               1553987
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.2
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C38(H38A,H38B), C51(H51A,H51B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C21(H21), C19(H19), C16(H16), C27(H27), C35(H35), C45(H45), C18(H18),
 C2(H2), C15(H15), C11(H11), C6(H6), C12(H12), C5(H5), C4(H4), C33(H33), C8(H8),
  C46(H46), C40(H40), C10(H10), C25(H25), C37(H37), C22(H22), C31(H31),
 C17(H17), C36(H36), C43(H43), C44(H44), C28(H28), C9(H9), C49(H49), C29(H29),
 C48(H48), C41(H41), C42(H42), C47(H47), C34(H34), C30(H30), C23(H23), C24(H24)
;
_shelx_res_checksum              56643
_shelx_fab_checksum              97873