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_1571984
_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         'C276 H216 Au28 P8'
_chemical_formula_sum            'C276 H216 Au28 P8'
_chemical_formula_weight         9295.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-18
_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
_cell_angle_beta                 114.081(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   47.3293(7)
_cell_length_b                   20.0353(5)
_cell_length_c                   41.2327(6)
_cell_measurement_reflns_used    34889
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.5030
_cell_measurement_theta_min      3.6760
_cell_volume                     35696.4(13)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4273
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.978
_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  32.00   0.60    6.06    --  -40.76  38.00   0.00  165
  2  \w   -110.00 -14.00   0.60    6.06    --  -40.76 -38.00-180.00  160
  3  \w   -114.00 -60.00   0.60    6.06    --  -40.76-151.00   2.00   90
  4  \w    -31.00  13.40   0.60    6.06    --   40.76 -57.00  60.00   74
  5  \w     32.00  89.00   0.60    6.06    --   40.76-125.00  60.00   95
  6  \w     36.00  97.20   0.60    6.06    --   40.76-125.00-150.00  102
  7  \w    105.00 171.60   0.60   24.25    --  111.38  77.00 120.00  111
  8  \w     52.00  79.00   0.60   24.25    --  111.38 -95.00 -90.00   45
  9  \w    103.00 175.60   0.60   24.25    --  111.38  77.00 -30.00  121
 10  \w     46.00 137.20   0.60   24.25    --  111.38 -45.00  30.00  152
 11  \w     44.00 111.80   0.60   24.25    --  111.38-125.00   0.00  113
 12  \w     56.00  83.00   0.60   24.25    --  111.38 -95.00   0.00   45
 13  \w     38.00 138.20   0.60   24.25    --  111.38 -45.00 150.00  167
 14  \w     78.00 105.00   0.60   24.25    --  111.38 -95.00-180.00   45
 15  \w     28.00 105.40   0.60   24.25    --  111.38 -95.00  30.00  129
 16  \w     86.00 174.20   0.60   24.25    --  111.38  45.00  90.00  147
 17  \w    104.00 176.00   0.60   24.25    --  111.38  77.00-180.00  120
 18  \w     55.00 105.40   0.60   24.25    --  111.38 -95.00  90.00   84
 19  \w     86.00 122.00   0.60   24.25    --  111.38  30.00 -90.00   60
 20  \w     81.00 105.60   0.60   24.25    --  111.38 -95.00-150.00   41
 21  \w     62.00  96.80   0.60   24.25    --  111.38 -95.00 150.00   58
;
_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      0.0322052000
_diffrn_orient_matrix_UB_12      -0.0330864000
_diffrn_orient_matrix_UB_13      0.0143856000
_diffrn_orient_matrix_UB_21      0.0149668000
_diffrn_orient_matrix_UB_22      0.0684555000
_diffrn_orient_matrix_UB_23      0.0005495000
_diffrn_orient_matrix_UB_31      0.0032797000
_diffrn_orient_matrix_UB_32      0.0112541000
_diffrn_orient_matrix_UB_33      0.0383351000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            121541
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.559
_diffrn_reflns_theta_min         3.567
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.618
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53497
_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 dark red'
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_description       block
_exptl_crystal_F_000             16816
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.480
_refine_diff_density_min         -2.963
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1339
_refine_ls_number_reflns         36215
_refine_ls_number_restraints     337
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0925P)^2^+264.0749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1678
_refine_ls_wR_factor_ref         0.1809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25596
_reflns_number_total             36215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01618a2.cif
_cod_data_source_block           au28
_cod_depositor_comments
'Adding full bibliography for 1571982--1571985.cif.'
_cod_database_code               1571984
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H P Au'
_chemical_oxdiff_usercomment     'Colorless Plate Crystals'
_reflns_odcompleteness_completeness 90.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C26-C11
 1.4 with sigma of 0.02
 C36-C029
 1.4 with sigma of 0.02
 C159-C36
 1.4 with sigma of 0.02
 C11-C55
 1.4 with sigma of 0.02
 C029-C26
 1.4 with sigma of 0.02
 C55-C159
 1.4 with sigma of 0.02
3. Rigid bond restraints
 C30, C037
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C159)
\\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C029) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C53)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C33) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C039)
\\sim Ueq, Uanis(C02W) \\sim Ueq, Uanis(C02K) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C55, C159, C36, C029, C26, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C48, C25, C12, C19, C03A, C02H
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C20, C030, C02Y, C9, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C029, C26, C11, C55, C159, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C02Q, C7, C02T, C5, C02A, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, C53, C44, C45, C3, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C23, C14, C158, C37, C02J, C038
 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:
 C00M(H00M), C00U(H00U), C00W(H00W), C01B(H01d), C01D(H01e), C01E(H01f),
 C01F(H01g), C01G(H01h), C01L(H01L), C01P(H01P), C01U(H01U), C01Y(H01Y),
 C020(H020), C021(H021), C022(H022), C023(H023), C024(H024), C025(H025),
 C02B(H02B), C02C(H02C), C29(H29), C4(H4), C27(H27), C02U(H02U), C02E(H02E),
 C02F(H02F), C02G(H02G), C02K(H02K), C02M(H02M), C02N(H02N), C02O(H02O),
 C02P(H02P), C02Q(H02Q), C02R(H02R), C02S(H02S), C02T(H02T), C02W(H02W), C9(H9),
  C16(H16), C21(H21), C20(H20), C030(H030), C033(H033), C034(H034), C035(H035),
 C036(H036), C18(H18), C6(H6), C33(H33), C10(H10), C30(H30), C039(H039),
 C03D(H03D), C03E(H03E), C03F(H03F), C13(H13), C15(H15), C17(H17), C24(H24),
 C31(H31), C143(H143), C75(H75), C8(H8), C131(H131), C5(H5), C7(H7), C22(H22),
 C2(H2), C32(H32), C3(H3), C45(H45), C44(H44), C25(H25), C12(H12), C19(H19),
 C03A(H03g), C48(H48), C35(H35), C34(H34), C28(H28), C158(H158), C37(H37),
 C038(H038), C23(H23), C14(H14), C159(H159), C36(H36), C029(H029), C11(H11),
 C55(H55)
6.b Fitted hexagon refined as free rotating group:
 C02C(C29,C4,C27,C02U,C01M), C02Y(C9,C16,C21,C20,C030), C037(C18,C6,C33,C10,
 C30), C53(C2,C32,C3,C45,C44), C25(C12,C19,C03A,C02H,C48), C158(C37,C02J,C038,
 C23,C14)
6.c Idealised Me refined as rotating group:
 C00T(H00a,H00b,H00c), C011(H01a,H01b,H01c), C02I(H02a,H02d,H02h), C02L(H02i,
 H02j,H02l), C032(H03a,H03b,H03c), C1(H1a,H1b,H1c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              88054
_shelx_hkl_checksum              41029
_shelx_fab_checksum              37603
_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 1.996
_oxdiff_exptl_absorpt_empirical_full_min 0.660