Digold(I) Thianthrenyl Complexes. Effect of Diphosphine Ligands on Molecular Structures in the Solid State and in Solution.
Abe, Ryota; Tsuchido, Yoshitaka; Ide, Tomohito; Koizumi, Take-Aki; Osakada, Kohtaro; ACS omega 7 (2022) 9594–9601; doi:10.1021/acsomega.1c06938

data_4519404
_publ_section_title
;
 Digold(I) Thianthrenyl Complexes. Effect of Diphosphine Ligands on
 Molecular Structures in the Solid State and in Solution.
;
_journal_issue                   11
_journal_name_full               'ACS omega'
_journal_page_first              9594
_journal_page_last               9601
_journal_paper_doi               10.1021/acsomega.1c06938
_journal_volume                  7
_journal_year                    2022
_chemical_formula_moiety         '2(C52 H42 Au2 P2 S4), C2 H2 Cl4, C2 H Cl4'
_chemical_formula_sum            'C108 H87 Au4 Cl8 P4 S8'
_chemical_formula_weight         2836.60
_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     dual
_audit_creation_date             2022-01-27
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_cell_angle_alpha                91.5820(10)
_cell_angle_beta                 108.5520(10)
_cell_angle_gamma                96.7650(10)
_cell_formula_units_Z            2
_cell_length_a                   16.0501(2)
_cell_length_b                   17.0934(2)
_cell_length_c                   20.7010(3)
_cell_measurement_reflns_used    31770
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.8100
_cell_measurement_theta_min      3.3180
_cell_volume                     5333.93(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.980
_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    -42.00  25.00   0.50    1.15    --   55.45 -15.00  30.00  134
  2  \w      0.00  50.00   0.50    1.15    --   55.45 -45.00  90.00  100
  3  \w     31.00  81.00   0.50    0.29    --    0.00  19.00 150.00  100
  4  \w     83.00 138.00   0.50    1.15    --   55.45 125.00   0.00  110
  5  \w    103.00 129.00   0.50    1.15    --   55.45 125.00  60.00   52
  6  \w     78.00 103.00   0.50    1.15    --   55.45 143.00  20.00   50
  7  \w    102.00 135.00   0.50    1.15    --   55.45 125.00 -30.00   66
  8  \w    109.00 138.00   0.50    1.15    --   55.45 125.00 -90.00   58
  9  \w    107.00 133.00   0.50    1.15    --   55.45 127.00-148.00   52
 10  \w    118.00 144.00   0.50    1.15    --  110.90 127.00-148.00   52
 11  \w    115.00 141.00   0.50    1.15    --  110.90 111.00-180.00   52
 12  \w     87.00 134.00   0.50    1.15    --   55.45  61.00-120.00   94
 13  \w     79.00 137.00   0.50    1.15    --   55.45 125.00-120.00  116
 14  \w     88.00 113.00   0.50    1.15    --  110.90 111.00-180.00   50
 15  \w     76.00 124.00   0.50    1.15    --  110.90  50.00   0.00   96
 16  \w    137.00 163.00   0.50    1.15    --  110.90  50.00   0.00   52
 17  \w     95.00 120.00   0.50    1.15    --  110.90 143.00  20.00   50
 18  \w     79.00 137.00   0.50    1.15    --   55.45 125.00  90.00  116
 19  \w     88.00 138.00   0.50    1.15    --   55.45 125.00 150.00  100
 20  \w    107.00 134.00   0.50    1.15    --  110.90  77.00 150.00   54
 21  \w     73.00 100.00   0.50    1.15    --  110.90  77.00 150.00   54
 22  \w     28.00  59.00   0.50    1.15    --  110.90 -50.00  90.00   62
 23  \w     77.00 103.00   0.50    1.15    --  110.90 -91.00 120.00   52
 24  \w     72.00 108.00   0.50    1.15    --  110.90-111.00  90.00   72
 25  \w     69.00  96.00   0.50    1.15    --  110.90-127.00 135.00   54
 26  \w     62.00 114.00   0.50    1.15    --   55.45-127.00 135.00  104
 27  \w     55.00  87.00   0.50    1.15    --  110.90-111.00  30.00   64
 28  \w     63.00 122.00   0.50    1.15    --  110.90-143.00 -34.00  118
 29  \w     40.00 126.00   0.50    1.15    --   55.45-143.00 -34.00  172
 30  \w     62.00 108.00   0.50    1.15    --  110.90-111.00-180.00   92
 31  \w     38.00  64.00   0.50    1.15    --  110.90-111.00 -60.00   52
 32  \w     36.00  95.00   0.50    1.15    --  110.90 -77.00-120.00  118
 33  \w     25.00  74.00   0.50    1.15    --  110.90 -63.00 -30.00   98
 34  \w     30.00  59.00   0.50    1.15    --  110.90 -50.00   0.00   58
 35  \w     24.00 108.00   0.50    1.15    --  110.90 -77.00  60.00  168
 36  \w     32.00  67.00   0.50    1.15    --  110.90-111.00  90.00   70
 37  \w     26.00  51.00   0.50    1.15    --  110.90 -50.00 150.00   50
 38  \w     26.00  57.00   0.50    1.15    --  110.90 -50.00 120.00   62
 39  \w     15.00  73.00   0.50    1.15    --  110.90 -91.00 120.00  116
 40  \w     18.00  82.00   0.50    1.15    --   55.45-125.00  90.00  128
 41  \w     31.00  56.00   0.50    0.29    --    0.00-143.00 -34.00   50
 42  \w    -31.00  60.00   0.50    1.15    --   55.45 -61.00 -60.00  182
 43  \w     23.00 107.00   0.50    1.15    --  110.90-111.00   0.00  168
 44  \w     27.00  58.00   0.50    1.15    --  110.90 -50.00 -90.00   62
 45  \w     30.00  57.00   0.50    1.15    --  110.90 -50.00-150.00   54
 46  \w     28.00 104.00   0.50    1.15    --  110.90 -91.00-180.00  152
 47  \w     27.00  76.00   0.50    1.15    --  110.90 -63.00-180.00   98
 48  \w     26.00  59.00   0.50    1.15    --  110.90 -50.00-180.00   66
 49  \w     10.00 173.00   0.50    1.15    --  110.90  12.00-180.00  326
 50  \w     23.00  48.00   0.50    0.29    --    0.00-127.00 135.00   50
 51  \w    -42.00  13.00   0.50    1.15    --   55.45 -15.00 150.00  110
 52  \w    -17.00  23.00   0.50    0.29    --    0.00  19.00 150.00   80
 53  \w    -31.00  23.00   0.50    1.15    --   55.45 -15.00  90.00  108
 54  \w     14.00 106.00   0.50    1.15    --  110.90 -91.00  30.00  184
 55  \w     14.00 106.00   0.50    1.15    --  110.90 -91.00 -60.00  184
 56  \w     10.00 163.00   0.50    1.15    --  110.90   0.00 150.00  306
 57  \w     17.00  45.00   0.50    1.15    --   55.45  61.00-120.00   56
 58  \w     -7.00  20.00   0.50    1.15    --   55.45 -15.00 -60.00   54
 59  \w    -35.00  15.00   0.50    1.15    --   55.45 -15.00-180.00  100
 60  \w    -20.00  54.00   0.50    1.15    --  -28.75  25.00-120.00  148
 61  \w    -50.00 -24.00   0.50    0.29    --    0.00 127.00-148.00   52
 62  \w    -83.00 -58.00   0.50    1.15    --  -28.75 127.00-148.00   50
 63  \w   -103.00 -78.00   0.50    1.15    --  -28.75 143.00  20.00   50
 64  \w   -114.00 -81.00   0.50    1.15    --  -28.75 -91.00 -60.00   66
 65  \w   -106.00 -81.00   0.50    1.15    --  -28.75-143.00 -34.00   50
 66  \w   -121.00 -94.00   0.50    1.15    --  -28.75 -91.00  90.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-DW'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0430150000
_diffrn_orient_matrix_UB_12      0.0000844000
_diffrn_orient_matrix_UB_13      -0.0779738000
_diffrn_orient_matrix_UB_21      -0.0376372000
_diffrn_orient_matrix_UB_22      0.0767639000
_diffrn_orient_matrix_UB_23      0.0094924000
_diffrn_orient_matrix_UB_31      0.0846761000
_diffrn_orient_matrix_UB_32      0.0488253000
_diffrn_orient_matrix_UB_33      -0.0046515000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            55896
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.064
_diffrn_reflns_theta_min         3.331
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              PhotonJet-DW
_exptl_absorpt_coefficient_mu    14.345
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       block
_exptl_crystal_F_000             2750
_exptl_crystal_size_max          0.87
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.653
_refine_diff_density_min         -6.331
_refine_diff_density_rms         0.258
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1177
_refine_ls_number_reflns         20232
_refine_ls_number_restraints     220
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1259P)^2^+53.1503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1912
_refine_ls_wR_factor_ref         0.1961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17880
_reflns_number_total             20232
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao1c06938_si_006.cif
_cod_data_source_block           190416_abe_au2ta2dppb_3
_cod_database_code               4519404
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         AuPSClC50H30
_shelx_estimated_absorpt_t_max   0.301
_shelx_estimated_absorpt_t_min   0.028
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C105-C106
 1.6 with sigma of 0.02
 C108-Cl6
 1.7 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C106 \\sim Cl1 \\sim Cl3 \\sim C105 \\sim Cl4 \\sim Cl2: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
C20 \\sim C21 \\sim C23 \\sim C22 \\sim C24 \\sim C19 \\sim S3 \\sim S4: within
2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
Cl6 \\sim C108 \\sim Cl7 \\sim C107 \\sim Cl5 \\sim Cl8: within 2A with sigma
of 0.0001 and sigma for terminal atoms of 0.0002 within 2A
Uanis(S4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(S4) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C77, C78, C80, C81, C82, C79
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C20, C19, C24, C23, C22, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C55, C56
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 S6, C59
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 S4, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
 Cl8, C107, Cl5, C108, Cl6, Cl7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Ternary CH refined with riding coordinates:
 C106(H106), C105(H105), C107(H107)
5.b Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C49(H49A,H49B), C103(H10A,H10B), C52(H52A,H52B), C104(H10C,
 H10D), C51(H51A,H51B), C101(H10E,H10F), C102(H10G,H10H)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C96(H96), C3(H3), C66(H66), C36(H36), C30(H30), C32(H32), C97(H97),
 C33(H33), C4(H4), C100(H100), C98(H98), C94(H94), C48(H48), C99(H99), C34(H34),
  C26(H26), C29(H29), C93(H93), C44(H44), C47(H47), C42(H42), C35(H35),
 C90(H90), C14(H14), C45(H45), C88(H88), C67(H67), C11(H11), C10(H10), C85(H85),
  C12(H12), C91(H91), C15(H15), C92(H92), C46(H46), C38(H38), C40(H40),
 C68(H68), C28(H28), C86(H86), C27(H27), C9(H9), C41(H41), C87(H87), C76(H76),
 C16(H16), C75(H75), C39(H39), C84(H84), C73(H73), C78(H78), C79(H79), C80(H80),
  C81(H81), C82(H82), C74(H74), C64(H64), C24(H24), C21(H21), C61(H61),
 C63(H63), C56(H56), C62(H62), C58(H58), C57(H57), C23(H23), C22(H22)
5.d Fitted hexagon refined as free rotating group:
 C77(C78,C79,C80,C81,C82)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              31878
_shelx_hkl_checksum              52925
_shelx_fab_checksum              59770
_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 2.961
_oxdiff_exptl_absorpt_empirical_full_min 0.372