[Au<sub>18</sub>(dppm)<sub>6</sub>Cl<sub>4</sub>]<sup>4+</sup>: a phosphine-protected gold nanocluster with rich charge states.
Zhang, Shan-Shan; Senanayake, Ravithree D.; Zhao, Quan-Qin; Su, Hai-Feng; Aikens, Christine M.; Wang, Xing-Po; Tung, Chen-Ho; Sun, Di; Zheng, Lan-Sun; Dalton transactions (Cambridge, England : 2003) 48 (2019) 3635–3640; doi:10.1039/c9dt00042a

data_7048829
_publ_section_title
;
 [Au<sub>18</sub>(dppm)<sub>6</sub>Cl<sub>4</sub>]<sup>4+</sup>: a
 phosphine-protected gold nanocluster with rich charge states.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3635
_journal_page_last               3640
_journal_paper_doi               10.1039/c9dt00042a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C150 H132 Au18 Cl4 P12, 3(Cl), F6 P, 2(C6 H6)'
_chemical_formula_sum            'C162 H144 Au18 Cl7 F6 P13'
_chemical_formula_weight         6400.92
_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             2018-11-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-23 deposited with the CCDC.
2019-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                70.259(2)
_cell_angle_beta                 82.278(2)
_cell_angle_gamma                90.156(2)
_cell_formula_units_Z            1
_cell_length_a                   15.442(4)
_cell_length_b                   15.608(4)
_cell_length_c                   18.615(4)
_cell_measurement_reflns_used    9359
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.559
_cell_measurement_theta_min      2.284
_cell_volume                     4179.0(18)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX3 (Bruker AXS Inc.,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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1924
_diffrn_reflns_av_unetI/netI     0.1353
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49605
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.388
_exptl_absorpt_coefficient_mu    16.017
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2276
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1463 before and 0.0687 after correction. The Ratio of minimum to maximum transmission is 0.3053. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.543
_exptl_crystal_description       block
_exptl_crystal_F_000             2906
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.195
_refine_diff_density_min         -3.299
_refine_diff_density_rms         0.486
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     928
_refine_ls_number_reflns         14723
_refine_ls_number_restraints     486
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1272
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1228P)^2^+148.9741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1998
_refine_ls_wR_factor_ref         0.2566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9077
_reflns_number_total             14723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00042a2.cif
_cod_data_source_block           p
_cod_depositor_comments          'Adding full bibliography for 7048829.cif.'
_cod_original_cell_volume        4179.0(17)
_cod_database_code               7048829
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.361
_shelx_estimated_absorpt_t_min   0.297
_exptl_absorpt_special_details   sadabs
_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
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
C57 \\sim C57 \\sim C58 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim C74 \\sim C75 \\sim C75:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C20 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C25:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
C32 \\sim C33 \\sim C34 \\sim C35 \\sim C35 \\sim C36 \\sim C36 \\sim C37:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
C79 \\sim C79 \\sim C78 \\sim C77 \\sim C76 \\sim C81 \\sim C80 \\sim C80:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
P3 \\sim P4 \\sim C38: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
P1 \\sim P2 \\sim C13: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
C79 \\sim C78 \\sim C77 \\sim C76 \\sim C81 \\sim C80: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
Cl4 \\sim Cl4A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(P5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C38) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
3. Others
 Fixed Sof: Cl4(0.6) Cl4A(0.4)
4.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C38(H38A,H38B), C63(H63A,H63B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49),
 C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C58(H58), C59(H59),
  C60(H60), C61(H61), C62(H62), C65(H65), C66(H66), C67(H67), C68(H68),
 C69(H69), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C79(H79), C78(H78),
  C77(H77), C76(H76), C81(H81), C80(H80)
4.c Fitted hexagon refined as free rotating group:
 C79(C78,C77,C76,C81,C80)
;
_olex2_submission_special_instructions 'No special instructions were received'