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_1571982
_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         'C88 H72 Au4 O2 P4, 2(C2 F6 N O4 S2)'
_chemical_formula_sum            'C92 H72 Au4 F12 N2 O10 P4 S4'
_chemical_formula_weight         2633.50
_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             2023-04-17
_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                90.7460(10)
_cell_angle_beta                 91.7370(10)
_cell_angle_gamma                91.3300(10)
_cell_formula_units_Z            4
_cell_length_a                   15.3967(2)
_cell_length_b                   23.3887(2)
_cell_length_c                   27.0694(3)
_cell_measurement_reflns_used    46682
_cell_measurement_temperature    100.03(10)
_cell_measurement_theta_max      74.1210
_cell_measurement_theta_min      4.0450
_cell_volume                     9739.91(19)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.03(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_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    -67.00  31.00   1.00    1.20    --  -41.81  57.00 -90.00   98
  2  \w    -65.00  32.00   1.00    1.20    --  -41.81  38.00  60.00   97
  3  \w   -112.00 -17.00   1.00    1.20    --  -41.81 -57.00 120.00   95
  4  \w     27.00  98.00   1.00    1.20    --   41.81-125.00  30.00   71
  5  \w     37.00  62.00   1.00    1.20    --   41.81-125.00-180.00   25
  6  \w     34.00 136.00   1.00    4.79    --  107.37 -30.00-180.00  102
  7  \w    122.00 149.00   1.00    4.79    --  107.37  77.00-150.00   27
  8  \w     43.00  70.00   1.00    4.79    --  107.37 -77.00-120.00   27
  9  \w    117.00 174.00   1.00    4.79    --  107.37  77.00-120.00   57
 10  \w     35.00 132.00   1.00    4.79    --  107.37 -45.00 -60.00   97
 11  \w     58.00 112.00   1.00    4.79    --  107.37-125.00 -30.00   54
 12  \w     80.00 106.00   1.00    4.79    --  107.37 -95.00-150.00   26
 13  \w     41.00 128.00   1.00    4.79    --  107.37 -45.00  90.00   87
 14  \w     63.00 106.00   1.00    4.79    --  107.37 -95.00   0.00   43
 15  \w     47.00 112.00   1.00    4.79    --  107.37-125.00   0.00   65
 16  \w     62.00 105.00   1.00    4.79    --  107.37 -95.00-180.00   43
 17  \w     33.00 106.00   1.00    4.79    --  107.37 -95.00  90.00   73
 18  \w     54.00 171.00   1.00    4.79    --  107.37   0.00-150.00  117
 19  \w     99.00 124.00   1.00    4.79    --  107.37-140.00 -95.48   25
 20  \w     42.00  67.00   1.00    1.20    --   42.31 -38.00 -30.00   25
 21  \w     63.00  89.00   1.00    4.79    --  107.37-125.00-120.00   26
 22  \w   -117.00 -18.00   1.00    1.20    --  -42.31 -38.00   0.00   99
 23  \w   -114.00 -14.00   1.00    1.20    --  -42.31 -57.00 -60.00  100
 24  \w      9.00  42.00   1.00    1.20    --   42.31  79.00  84.27   33
 25  \w      9.00  42.00   1.00    1.20    --   42.31  79.00-137.13   33
 26  \w      9.00  42.00   1.00    1.20    --   42.31  80.00 -67.62   33
 27  \w      8.00  34.00   1.00    1.20    --   42.31  83.00-104.95   26
 28  \w     55.00 178.00   1.00    4.79    --  107.37  15.00  30.00  123
 29  \w     80.00 178.00   1.00    4.79    --  107.37  52.00-150.10   98
 30  \w     82.00 178.00   1.00    4.79    --  107.37  45.00 -60.00   96
 31  \w     78.00 178.00   1.00    4.79    --  107.37  61.00  30.00  100
 32  \w     78.00 178.00   1.00    4.79    --  107.37  61.00 150.00  100
 33  \w     80.00 178.00   1.00    4.79    --  107.37  52.00  89.63   98
 34  \w     78.00 178.00   1.00    4.79    --  107.37  61.00 120.00  100
 35  \w     78.00 178.00   1.00    4.79    --  107.37  60.00  -6.24  100
 36  \w     78.00 178.00   1.00    4.79    --  107.37  61.00-180.00  100
 37  \w     78.00 178.00   1.00    4.79    --  107.37  61.00  60.00  100
 38  \w     79.00 178.00   1.00    4.79    --  107.37  57.00-101.51   99
 39  \w     79.00 178.00   1.00    4.79    --  107.37  30.00 -90.00   99
 40  \w    -87.00  -6.00   1.00    1.20    --  -42.31 125.00  60.00   81
 41  \w      8.00  34.00   1.00    1.20    --   42.31  83.00 -10.30   26
 42  \w      8.00  34.00   1.00    1.20    --   42.31  83.00 134.73   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0332072000
_diffrn_orient_matrix_UB_12      0.0323077000
_diffrn_orient_matrix_UB_13      0.0453815000
_diffrn_orient_matrix_UB_21      0.0872897000
_diffrn_orient_matrix_UB_22      -0.0093647000
_diffrn_orient_matrix_UB_23      0.0277001000
_diffrn_orient_matrix_UB_31      0.0361128000
_diffrn_orient_matrix_UB_32      0.0566591000
_diffrn_orient_matrix_UB_33      -0.0203896000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            60249
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.204
_diffrn_reflns_theta_min         3.476
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.170
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_description       block
_exptl_crystal_F_000             5064
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         6.159
_refine_diff_density_min         -3.798
_refine_diff_density_rms         0.416
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2310
_refine_ls_number_reflns         60249
_refine_ls_number_restraints     1699
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0929
_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^)+(0.1720P)^2^+166.4250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2487
_refine_ls_wR_factor_ref         0.2556
_reflns_Friedel_coverage         0.000
_reflns_number_gt                52739
_reflns_number_total             60249
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9849\% 
around [-0.32 0.00 0.95] (reciprocal) or [-0.71 -0.00 0.71] (direct)
;
_cod_data_source_file            d4sc01618a2.cif
_cod_data_source_block           1_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 1571982--1571985.cif.'
_cod_database_code               1571982
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H P Au'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5808(8)
 0.4192(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 S1-C26
 1.795 with sigma of 0.02
 F2-C61
 1.362 with sigma of 0.02
 C61-F1
 1.362 with sigma of 0.02
 F22-C61
 1.362 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C021) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C05M) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C03X) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C08M) \\sim Ueq, Uanis(C06N) \\sim Ueq, Uanis(C044) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C61) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C01T) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C07R) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C01W, Au03, C03X, P00P, Au06, Au08, Au07, C01N, C09E, C05C, C069, C9, P00I,
 P00K, C01X, C03K, C09G, P00Q, C03A, C06K, C04G, C05W, C49, C15, C18, C080,
 C083, C018, C02A, C02N, C13, C026, C02S, C07L, C044, O01C, C098, C02T, C052,
 C05I, C021, C057, C025, C089, C093, C08T, C08W, C45, C42, C39, C08A, C02Z, C8,
 C01F, C04B, C05Y, C03R, C01A, C08N, C032, C06J, C08B, C09S, C44, C04R, C043,
 C04U, C06N, C040, C09P, C09D, C37, C31, C43, C068, C03J, C022, C065, C05H,
 C06M, C02J, C04H, C08O, C05X, C06E, C48, C32, O01P, C08Q, C08S, C06D, C06L,
 C09N, C02C, C049, C06Q, C06I, C07R
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N13, S1, O8, O11, C26, S2, F14, F27, F29, O23, O1, F1, F2, F22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Au04, Au01, Au02, P00N, C01U, Au05, P00F, P00O, C019, C056, C073, C084, C01T,
 P00L, C02Y, C04X, C067, C031, C046, C05A, C055, C06C, C02E, C07K, C05O, C7,
 C05U, C02K, C02W, C023, C02L, C06W, C02R, C074, C02U, C03P, C1, C03U, C045,
 C09J, C04O, C075, C05E, C05Z, C02G, C04C, H06C, C03L, H02E, C02X, H07K, C05T,
 H05O, C07W, C08Z, H7, C04M, H05U, C04Q, O016, C02D, C02V, C05M, C047, C05S,
 C09Q, C02B, H02R, C03D, H074, C05B, H02U, C03V, H03P, C06Y, H1, C11, H03U,
 C04A, H045, C059, C05G, H09J, H04O, C086, H075, C03O, H05E, C07T, H05Z, C27,
 H02G, C03T, C05V, H03L, C05F, H02X, C05L, H05T, H07W, C062, H08Z, H04M, C02Q,
 H04Q, C05R, H02D, H02V, C03Y, H05M, C07C, H047, C029, H05S, C06A, H09Q, C01Z,
 H02B, C07A, H03D, C048, H05B, H03V, C08L, H06Y, C04I, H11, H04A, H059, C095,
 H05G, C04F, H086, H03O, H07T, C34, H27, H03T, C07S, H05V, H05F, H05L, H062,
 O03Z, H05a, H05c, H05h, H03Y, C08M, H07e, H029, C03C, H06A, H01Z, C05D, H07d,
 H048, H08L, H04I, H095, H04F, H34, H07S, C077, H08M, H03C, H05D, H07a, H07b,
 H07c
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Aromatic/amide H refined with riding coordinates:
 C018(H018), C01A(H01A), C01F(H01F), C01W(H01W), C01Z(H01Z), C022(H022),
 C029(H029), C02B(H02B), C02C(H02C), C02D(H02D), C02E(H02E), C02G(H02G),
 C02J(H02J), C02R(H02R), C02U(H02U), C02V(H02V), C02X(H02X), C02Z(H02Z),
 C032(H032), C03C(H03C), C03D(H03D), C03J(H03J), C03K(H03K), C03L(H03L),
 C03O(H03O), C03P(H03P), C03R(H03R), C03T(H03T), C03U(H03U), C03V(H03V),
 C03Y(H03Y), C040(H040), C044(H044), C045(H045), C047(H047), C048(H048),
 C049(H049), C04A(H04A), C04B(H04B), C04F(H04F), C04G(H04G), C04H(H04H),
 C04I(H04I), C04M(H04M), C04O(H04O), C04Q(H04Q), C04U(H04U), C052(H052),
 C059(H059), C05B(H05B), C05D(H05D), C05E(H05E), C05F(H05F), C05G(H05G),
 C05H(H05i), C05I(H05j), C05L(H05L), C05M(H05M), C05O(H05O), C05S(H05S),
 C05T(H05T), C05U(H05U), C05V(H05V), C05W(H05W), C05X(H05X), C05Y(H05Y),
 C05Z(H05Z), C062(H062), C065(H065), C068(H068), C06A(H06A), C06C(H06C),
 C06D(H06D), C06E(H06E), C06J(H06J), C06L(H06L), C06M(H06M), C06N(H06N),
 C06Q(H06Q), C06Y(H06Y), C074(H074), C075(H075), C07A(H07d), C07C(H07e),
 C07K(H07K), C07R(H07R), C07S(H07S), C07T(H07T), C07W(H07W), C080(H080),
 C083(H083), C086(H086), C089(H089), C08A(H08A), C08B(H08B), C08L(H08L),
 C08M(H08M), C08N(H08N), C08O(H08O), C08Q(H08Q), C08S(H08S), C08T(H08T),
 C08W(H08W), C08Z(H08Z), C093(H093), C095(H095), C098(H098), C09D(H09D),
 C09G(H09G), C09J(H09J), C09N(H09N), C09P(H09P), C09Q(H09Q), C09S(H09S), C8(H8),
  C15(H15), C18(H18), C31(H31), C39(H39), C42(H42), C43(H43), C45(H45),
 C48(H48), C49(H49), C1(H1), C11(H11), C27(H27), C34(H34), C32(H32), C37(H37),
 C44(H44), C7(H7)
6.b Idealised Me refined as rotating group:
 C04R(H04c,H04d,H04e), C05R(H05a,H05c,H05h), C06I(H06b,H06f,H06g), C077(H07a,
 H07b,H07c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              27770
_shelx_hkl_checksum              69684
_shelx_fab_checksum              4531
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.560
_oxdiff_exptl_absorpt_empirical_full_min 0.724
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2