Au<sub>54</sub>(Et<sub>3</sub>P)<sub>18</sub>Cl<sub>12</sub>: a structurally related cluster to Au<sub>32</sub>(Et<sub>3</sub>P)<sub>12</sub>Cl<sub>8</sub> gives insight into the formation process.
Kenzler, Sebastian; Schrenk, Claudio; Schnepf, Andreas; Dalton transactions (Cambridge, England : 2003) 49 (2020) 10765–10771; doi:10.1039/d0dt02262d

data_7704720
_publ_section_title
;
 Au<sub>54</sub>(Et<sub>3</sub>P)<sub>18</sub>Cl<sub>12</sub>: a
 structurally related cluster to
 Au<sub>32</sub>(Et<sub>3</sub>P)<sub>12</sub>Cl<sub>8</sub> gives insight
 into the formation process.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10765
_journal_page_last               10771
_journal_paper_doi               10.1039/d0dt02262d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C108 H270 Au53.95 Cl12 P18'
_chemical_formula_sum            'C108 H270 Au53.95 Cl12 P18'
_chemical_formula_weight         13178.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-04-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-24 deposited with the CCDC.	2020-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.8630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.4195(13)
_cell_length_b                   20.9254(15)
_cell_length_c                   27.3606(19)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.241
_cell_measurement_theta_min      2.216
_cell_volume                     10521.8(13)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            153737
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.500
_diffrn_reflns_theta_max         24.500
_diffrn_reflns_theta_min         2.085
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    37.752
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.3756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1677 before and 0.0703 after correction. The Ratio of minimum to maximum transmission is 0.5034. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    4.160
_exptl_crystal_description       block
_exptl_crystal_F_000             11308
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: EtOH, CH2Cl2, THF'
_exptl_crystal_size_max          0.079
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.029
_refine_diff_density_max         3.353
_refine_diff_density_min         -1.751
_refine_diff_density_rms         0.294
_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     910
_refine_ls_number_reflns         17511
_refine_ls_number_restraints     194
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0220P)^2^+145.9614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0730
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14044
_reflns_number_total             17511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02262d2.cif
_cod_data_source_block           39
_cod_depositor_comments          'Adding full bibliography for 7704720.cif.'
_cod_database_code               7704720
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 H10F-H10T
 2 with sigma of 0.02
 C132-C133 \\sim C127-C126 \\sim C129-C128 \\sim C134-C135 \\sim C137-C136
\\sim C131-C130 \\sim C101-
 C102 \\sim C153-C152 \\sim C151-C150 \\sim C155-C154
 with sigma of 0.02
 C106-C105 \\sim C106-C107
 with sigma of 0.02
 P9-C107 \\sim P9-C105
 with sigma of 0.02
 C106-C107 \\sim C106-C105 \\sim C104-C103 \\sim C101-C102
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C131 \\sim C137: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C130 \\sim C136: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C129 \\sim C135: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C128 \\sim C134: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C126 \\sim C132: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C127 \\sim C133: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C103: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C104: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C131) \\sim Ueq, Uanis(C130) \\sim Ueq, Uanis(C126) \\sim Ueq,
Uanis(C127) \\sim Ueq, Uanis(C128) \\sim Ueq, Uanis(C129) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C152) \\sim Ueq, Uanis(C151) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C103) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C106) \\sim Ueq, Uanis(C105) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C152) \\sim Ueq, Uanis(C153) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Au1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(P4A)=Sof(H10P)=Sof(H10Q)=Sof(H10R)=Sof(C107)=Sof(H10S)=Sof(H10T)=
 Sof(C132)=Sof(H13F)=Sof(H13G)=Sof(C133)=Sof(H13H)=Sof(H13I)=Sof(H13J)=
 Sof(C134)=Sof(H13K)=Sof(H13L)=Sof(C135)=Sof(H13M)=Sof(H13N)=Sof(H13O)=
 Sof(C136)=Sof(H13P)=Sof(H13Q)=Sof(C137)=Sof(H13R)=Sof(H13S)=Sof(H13T)=1-FVAR(1)
 Sof(P4)=Sof(C105)=Sof(H10K)=Sof(H10L)=Sof(H10M)=Sof(H10N)=Sof(H10O)=Sof(C126)=
 Sof(H12P)=Sof(H12Q)=Sof(C127)=Sof(H12R)=Sof(H12S)=Sof(H12T)=Sof(C128)=
 Sof(H12U)=Sof(H12V)=Sof(C129)=Sof(H12W)=Sof(H12X)=Sof(H12Y)=Sof(C130)=
 Sof(H13A)=Sof(H13B)=Sof(C131)=Sof(H13C)=Sof(H13D)=Sof(H13E)=FVAR(1)
 Sof(Au1A)=0.5*(1-FVAR(3))
 Sof(Au1)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C103(H10F,H10G), C105(H10K,H10L), C107(H10S,H10T), C108(H10U,
 H10V), C110(H11A,H11B), C112(H11F,H11G), C114(H11K,H11L), C116(H11P,H11Q),
 C118(H11U,H11V), C120(H12A,H12B), C122(H12F,H12G), C124(H12K,H12L), C126(H12P,
 H12Q), C128(H12U,H12V), C130(H13A,H13B), C132(H13F,H13G), C134(H13K,H13L),
 C136(H13P,H13Q), C138(H13U,H13V), C140(H14A,H14B), C142(H14F,H14G), C144(H14K,
 H14L), C146(H14P,H14Q), C148(H14U,H14V), C150(H15A,H15B), C152(H15F,H15G),
 C154(H15K,H15L), C156(H15P,H15Q), C158(H15U,H15V), C160(H16A,H16B)
5.b Me refined with riding coordinates:
 C102(H10C,H10D,H10E), C104(H10H,H10I,H10J), C106(H10M,H10N,H10O), C106(H10P,
 H10Q,H10R), C109(H10W,H10X,H10Y), C111(H11C,H11D,H11E), C113(H11H,H11I,H11J),
 C115(H11M,H11N,H11O), C117(H11R,H11S,H11T), C119(H11W,H11X,H11Y), C121(H12C,
 H12D,H12E), C123(H12H,H12I,H12J), C125(H12M,H12N,H12O), C127(H12R,H12S,H12T),
 C129(H12W,H12X,H12Y), C131(H13C,H13D,H13E), C133(H13H,H13I,H13J), C135(H13M,
 H13N,H13O), C137(H13R,H13S,H13T), C139(H13W,H13X,H13Y), C141(H14C,H14D,H14E),
 C143(H14H,H14I,H14J), C145(H14M,H14N,H14O), C147(H14R,H14S,H14T), C149(H14W,
 H14X,H14Y), C151(H15C,H15D,H15E), C153(H15H,H15I,H15J), C155(H15M,H15N,H15O),
 C157(H15R,H15S,H15T), C159(H15W,H15X,H15Y), C161(H16C,H16D,H16E)
;
_shelx_res_checksum              61284
_shelx_fab_checksum              38159
_olex2_submission_special_instructions 'No special instructions were received'