Co-ligand triphenylphosphine/alkynyl-stabilized undecagold nanocluster with a capped crown structure
Gao, Yan-Li; Bi, Shiqing; Wang, Yufei; Li, Jian; Su, Ting; Gao, Xuchun; RSC Advances 12 (2022) 11047–11051; doi:10.1039/D2RA01080A

data_7244736
_publ_section_title
;
 Co-ligand triphenylphosphine/alkynyl-stabilized undecagold nanocluster
 with a capped crown structure
;
_journal_issue                   18
_journal_name_full               'RSC Advances'
_journal_page_first              11047
_journal_page_last               11051
_journal_paper_doi               10.1039/D2RA01080A
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C162 H128 Au11 F6 P8, F6 Sb'
_chemical_formula_sum            'C162 H128 Au11 F12 P8 Sb'
_chemical_formula_weight         4838.78
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-12-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-12-09 deposited with the CCDC.	2022-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                80.8164(10)
_cell_angle_beta                 82.7276(10)
_cell_angle_gamma                63.1499(17)
_cell_formula_units_Z            2
_cell_length_a                   16.0672(3)
_cell_length_b                   17.0707(3)
_cell_length_c                   32.9542(3)
_cell_measurement_reflns_used    35367
_cell_measurement_temperature    99.9(6)
_cell_measurement_theta_max      65.5670
_cell_measurement_theta_min      2.6900
_cell_volume                     7945.6(2)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.9(6)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            85279
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        65.693
_diffrn_reflns_theta_max         65.693
_diffrn_reflns_theta_min         2.722
_exptl_absorpt_coefficient_mu    21.146
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12256
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.023
_exptl_crystal_description       rod
_exptl_crystal_F_000             4496
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         7.613
_refine_diff_density_min         -6.219
_refine_diff_density_rms         0.317
_refine_ls_extinction_coef       0.000007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1773
_refine_ls_number_reflns         26720
_refine_ls_number_restraints     241
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0650
_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^)+(0.1077P)^2^+181.0618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.1851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23105
_reflns_number_total             26720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra01080a2.cif
_cod_data_source_block           1_sq
_cod_original_cell_volume        7945.5(2)
_cod_database_code               7244736
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.186
_shelx_estimated_absorpt_t_min   0.101
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F6-F4
 2.08 with sigma of 0.02
 F5-C18
 1.3 with sigma of 0.02
 C18-F4
 1.3 with sigma of 0.02
 F6-C18
 1.3 with sigma of 0.02
 F4-F5
 2.08 with sigma of 0.02
 F6-F5
 2.08 with sigma of 0.02
3. Rigid bond restraints
 C5, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F6, F5, C18, C16, C15, C14, C13
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.002
 F4, F11, F10, C118, C119, C123, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C27, C28
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C7A, C9A, F9, C109, C114, C8, C21, C111, C112, C113, C20, C22, C23, C27, C28,
 C29, C5, C10, C10A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C9) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F6) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(F4) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(C118)
\\sim Ueq, Uanis(C119) \\sim Ueq, Uanis(C123) \\sim Ueq, Uanis(C9) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(C7A) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(C109)
\\sim Ueq, Uanis(C114) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C21) \\sim Ueq,
Uanis(C111) \\sim Ueq, Uanis(C112) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C10A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.005
5. Others
 Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=1-
 FVAR(1)
 Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C6A(H6A), C7(H7), C7A(H7A), C9(H9), C9A(H9A), C10(H10), C10A(H10A),
 C13(H13), C14(H14), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41),
  C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50),
 C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59),
  C60(H60), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C68(H68),
 C69(H69), C70(H70), C71(H71), C72(H72), C74(H74), C75(H75), C76(H76), C77(H77),
  C78(H78), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C86(H86),
 C87(H87), C88(H88), C89(H89), C90(H90), C92(H92), C93(H93), C94(H94), C95(H95),
  C96(H96), C98(H98), C99(H99), C100(H100), C101(H101), C102(H102), C104(H104),
 C105(H105), C106(H106), C107(H107), C108(H108), C110(H110), C114(H114),
 C113(H113), C112(H112), C111(H111), C116(H116), C117(H117), C118(H118),
 C119(H119), C120(H120), C122(H122), C123(H123), C124(H124), C125(H125),
 C126(H126), C128(H128), C129(H129), C130(H130), C131(H131), C132(H132),
 C134(H134), C135(H135), C136(H136), C137(H137), C138(H138), C140(H140),
 C141(H141), C142(H142), C143(H143), C144(H144), C146(H146), C147(H147),
 C148(H148), C149(H149), C150(H150), C152(H152), C153(H153), C154(H154),
 C155(H155), C156(H156), C158(H158), C159(H159), C160(H160), C161(H161),
 C162(H162)
6.b Fitted hexagon refined as free rotating group:
 C110(C109,C114,C113,C112,C111)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              32044
_shelx_fab_checksum              14133
_olex2_submission_special_instructions 'No special instructions were received'