Divergent catalytic behaviors of assembled organogold(i) clusters derived from enyne cyclization.
Liu, Qian; Zhai, Xiao-Yi; Jian, Rui-Jun; Zhao, Liang; Chemical science 15 (2024) 11311–11320; doi:10.1039/d4sc01618a

data_1571985
_publ_section_title
;
 Divergent catalytic behaviors of assembled organogold(i) clusters derived
 from enyne cyclization.
;
_journal_issue                   29
_journal_name_full               'Chemical science'
_journal_page_first              11311
_journal_page_last               11320
_journal_paper_doi               10.1039/d4sc01618a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C186 H135 Au14 P5, 2(C2 F6 N O4 S2)'
_chemical_formula_sum            'C190 H135 Au14 F12 N2 O8 P5 S4'
_chemical_formula_weight         5842.61
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-08-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-02-06 deposited with the CCDC.	2024-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                84.197(2)
_cell_angle_beta                 78.827(2)
_cell_angle_gamma                76.291(2)
_cell_formula_units_Z            2
_cell_length_a                   16.0520(4)
_cell_length_b                   18.4672(5)
_cell_length_c                   33.1755(8)
_cell_measurement_reflns_used    28456
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.0260
_cell_measurement_theta_min      3.7290
_cell_volume                     9357.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.78a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.78a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.78a (Rigaku OD, 2020)'
_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)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -45.00 -10.00   0.50    0.50    --   43.00  18.00-180.00   70
  2  \w     33.00 132.00   0.50    0.50    --   43.00  55.00  90.00  198
  3  \w     52.00 132.00   0.50    0.50    --   43.00  55.00   0.00  160
  4  \w     58.00  85.00   0.50    0.50    --   43.00  18.00-180.00   54
  5  \w     59.00 132.00   0.50    0.50    --   43.00  55.00 150.00  146
  6  \w     55.00 132.00   0.50    0.50    --   43.00  55.00-150.00  154
  7  \w     65.00 132.00   0.50    0.50    --   43.00  55.00 -60.00  134
  8  \w    -45.00   1.00   0.50    0.50    --   43.00  55.00-150.00   92
  9  \w      7.00  33.00   0.50    1.13    --   90.00  46.00 120.00   52
 10  \w     13.00  44.00   0.50    1.13    --   90.00  28.00 150.00   62
 11  \w      2.00  83.00   0.50    1.13    --   90.00  46.00 -90.00  162
 12  \w    140.00 178.00   0.50    1.13    --   90.00  46.00 -90.00   76
 13  \w      2.00  81.00   0.50    1.13    --   90.00  46.00  60.00  158
 14  \w     97.00 174.00   0.50    1.13    --   90.00  46.00  60.00  154
 15  \w     23.00  50.00   0.50    1.13    --   90.00  46.00  30.00   54
 16  \w     98.00 166.00   0.50    1.13    --   90.00  46.00  90.00  136
 17  \w    130.00 178.00   0.50    1.13    --   90.00  46.00 150.00   96
 18  \w    123.00 163.00   0.50    1.13    --   90.00  46.00 -60.00   80
 19  \w    100.00 178.00   0.50    1.13    --   90.00  46.00-150.00  156
 20  \w     39.00  78.00   0.50    1.13    --   90.00  46.00  90.00   78
 21  \w     66.00  95.00   0.50    1.13    --   90.00  28.00-180.00   58
 22  \w     77.00 103.00   0.50    1.13    --   90.00  46.00 150.00   52
 23  \w    106.00 131.00   0.50    1.13    --   90.00   9.00-150.00   50
 24  \w     50.00 135.00   0.50    1.13    --   90.00  28.00 150.00  170
 25  \w      7.00  42.00   0.50    1.13    --   90.00  18.00 -30.00   70
 26  \w     57.00  82.00   0.50    1.13    --   90.00  18.00 -30.00   50
 27  \w    128.00 179.00   0.50    1.13    --   90.00  18.00 -30.00  102
 28  \w    108.00 134.00   0.50    1.13    --   90.00  46.00-120.00   52
 29  \w    143.00 178.00   0.50    1.13    --   90.00  46.00-120.00   70
 30  \w     61.00  97.00   0.50    1.13    --   90.00  46.00   0.00   72
 31  \w    118.00 176.00   0.50    1.13    --   90.00  46.00 -30.00  116
 32  \w     22.00  60.00   0.50    1.13    --   90.00  46.00 -60.00   76
 33  \w      2.00  83.00   0.50    1.13    --   90.00  37.00-150.00  162
 34  \w     81.00 106.00   0.50    1.13    --   90.00  46.00 -30.00   50
 35  \w     99.00 179.00   0.50    1.13    --   90.00  37.00-150.00  160
 36  \w     28.00  54.00   0.50    1.13    --   90.00  18.00-180.00   52
 37  \w     94.00 125.00   0.50    1.13    --   90.00  18.00-180.00   62
 38  \w    140.00 165.00   0.50    1.13    --   90.00  46.00-180.00   50
 39  \w    102.00 134.00   0.50    1.13    --   90.00  18.00   0.00   64
 40  \w    148.00 175.00   0.50    1.13    --   90.00  18.00   0.00   54
 41  \w     97.00 133.00   0.50    1.13    --   90.00  37.00   0.00   72
 42  \w     12.00 176.00   0.50    1.13    --   90.00  37.00 120.00  328
 43  \w    136.00 164.00   0.50    1.13    --   90.00  46.00   0.00   56
 44  \w    100.00 125.00   0.50    1.13    --   90.00  28.00-180.00   50
 45  \w     11.00  42.00   0.50    1.13    --   90.00  46.00 -30.00   62
 46  \w    146.00 179.00   0.50    1.13    --   90.00  46.00 120.00   66
 47  \w    115.00 176.00   0.50    1.13    --   90.00  46.00  30.00  122
 48  \w     77.00 147.00   0.50    1.13    --   90.00  18.00-150.00  140
 49  \w    153.00 178.00   0.50    1.13    --   90.00   9.00-150.00   50
 50  \w    135.00 160.00   0.50    1.13    --   90.00  28.00-120.00   50
 51  \w    154.00 179.00   0.50    1.13    --   90.00  37.00 -60.00   50
 52  \w     89.00 114.00   0.50    1.13    --   90.00  37.00 150.00   50
 53  \w     20.00  45.00   0.50    1.13    --   90.00   0.00-150.00   50
 54  \w    126.00 151.00   0.50    1.13    --   90.00   0.00-150.00   50
 55  \w     75.00 179.00   0.50    1.13    --   90.00  28.00 -90.00  208
 56  \w    141.00 166.00   0.50    1.13    --   90.00  37.00 -30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.945
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            151922
_diffrn_reflns_point_group_measured_fraction_full 0.945
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        66.737
_diffrn_reflns_theta_max         66.737
_diffrn_reflns_theta_min         3.566
_exptl_absorpt_coefficient_mu    21.412
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.78a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_density_diffrn    2.074
_exptl_crystal_description       block
_exptl_crystal_F_000             5412
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.145
_refine_diff_density_min         -2.735
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2114
_refine_ls_number_reflns         31332
_refine_ls_number_restraints     567
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0657
_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^)+(0.1005P)^2^+80.1442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1737
_refine_ls_wR_factor_ref         0.1842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23694
_reflns_number_total             31332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01618a2.cif
_cod_data_source_block           20211116-lq-r239
_cod_depositor_comments
'Adding full bibliography for 1571982--1571985.cif.'
_cod_database_code               1571985
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N16-S1
 1.54 with sigma of 0.02
 S1-O38
 1.45 with sigma of 0.02
 N16-S2
 1.54 with sigma of 0.02
 S2-O8
 1.45 with sigma of 0.02
 S1-C2
 1.878 with sigma of 0.02
 S1-O11
 1.45 with sigma of 0.02
 C2-F47
 1.38 with sigma of 0.02
 C2-F19
 1.38 with sigma of 0.02
 C2-F17
 1.38 with sigma of 0.02
 S2-O13
 1.45 with sigma of 0.02
 C3-S2
 1.85 with sigma of 0.02
 C3-F59
 1.35 with sigma of 0.02
 C3-F1
 1.35 with sigma of 0.02
 C3-F60
 1.35 with sigma of 0.02
 F60-C3 = C3-F1
 1.35 with sigma of 0.02
 F59-C3 = C3-F1
 1.35 with sigma of 0.02
 F59-C3 = C3-F60
 1.35 with sigma of 0.02
 S2-F59
 2.6 with sigma of 0.02
 S2-F60
 2.6 with sigma of 0.02
 S2-F1
 2.6 with sigma of 0.02
 F59-F1
 2.277 with sigma of 0.04
 F59-F60
 2.277 with sigma of 0.04
 F60-F1
 2.277 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C03G \\sim C04H \\sim C057 \\sim C1 \\sim C25 \\sim C05G: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(F1) \\sim Ueq, Uanis(S1) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O38)
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N16) \\sim Ueq, Uanis(F17) \\sim Ueq,
Uanis(F19) \\sim Ueq, Uanis(F47) \\sim Ueq, Uanis(S2) \\sim Ueq, Uanis(O8)
\\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(F59) \\sim Ueq,
Uanis(F60) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C02X) \\sim Ueq, Uanis(C04O) \\sim Ueq, Uanis(C04W) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C05J) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(F01X) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Au2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C38, C04M, C036, C04Z, C31, C24, C01J, C01W, C00Z, C00N, C018, C01G, C02C,
 C03T, C052, C026
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C05M, C53, C41, C049, C03S, C37, C01O, C016, C01C, C00O, C00P, C011, C032,
 C03F, C02M, C01K
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F60, S1, O11, O38, C2, N16, F17, F19, F47, S2, O8, O13, C3, F1, F59
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Au2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Au)=1-FVAR(1)
 Sof(Au1)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C00U(H00U), C012(H012), C014(H014), C015(H015), C016(H016), C017(H017),
 C01G(H01G), C01H(H01H), C01K(H01K), C01L(H01L), C01M(H01M), C01U(H01U),
 C021(H021), C024(H024), C025(H025), C026(H026), C027(H027), C02A(H02A),
 C02B(H02B), C02C(H02C), C02E(H02E), C02F(H02F), C02H(H02H), C02J(H02J),
 C02M(H02M), C02Q(H02Q), C02S(H02S), C02T(H02T), C02U(H02U), C02V(H02V),
 C02W(H02W), C02Y(H02Y), C02Z(H02Z), C030(H030), C032(H032), C034(H034),
 C035(H035), C039(H039), C03A(H03A), C03B(H03B), C03C(H03C), C03D(H03D),
 C03E(H03E), C03F(H03F), C03H(H03H), C03I(H03I), C03J(H03J), C03K(H03K),
 C03L(H03L), C03M(H03M), C03O(H03O), C03P(H03P), C03Q(H03Q), C03T(H03T),
 C03V(H03V), C03W(H03W), C03X(H03X), C03Y(H03Y), C03Z(H03Z), C040(H040),
 C041(H041), C042(H042), C043(H043), C044(H044), C045(H045), C046(H046),
 C047(H047), C048(H048), C049(H049), C04A(H04A), C04C(H04C), C04E(H04E),
 C04F(H04F), C04G(H04G), C04H(H04H), C04I(H04I), C04J(H04J), C04K(H04K),
 C04L(H04L), C04M(H04M), C04N(H04N), C04O(H04O), C04P(H04P), C04Q(H04Q),
 C04S(H04S), C04U(H04U), C04W(H04W), C04X(H04X), C04Y(H04Y), C04Z(H04Z),
 C050(H050), C051(H051), C052(H052), C053(H053), C054(H054), C055(H055),
 C056(H056), C057(H057), C058(H058), C059(H059), C05A(H05A), C05B(H05B),
 C05C(H05C), C05F(H05F), C05G(H05G), C05H(H05H), C05I(H05I), C05J(H05J),
 C05L(H05L), C05M(H05M), C05N(H05N), C05O(H05O), C37(H37), C41(H41), C48(H48),
 C04V(H04V), C04R(H04R), C033(H033), C34(H34), C53(H53), C6(H6), C1(H1), C9(H9),
  C11(H11), C24(H24), C25(H25), C31(H31), C33(H33), C38(H38), C39(H39),
 C12(H12), C14(H14), C5(H5), C26(H26), C27(H27)
6.b Fitted hexagon refined as free rotating group:
 C48(C04V,C04R,C033,C03R,C34)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              99516
_shelx_hkl_checksum              23470
_shelx_fab_checksum              65160
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;