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_4519406
_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         'C50 H38 Au2 P2 S4'
_chemical_formula_sum            'C50 H38 Au2 P2 S4'
_chemical_formula_weight         1222.91
_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     dual
_audit_creation_date             2021-10-20
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.3680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.37680(10)
_cell_length_b                   16.5846(2)
_cell_length_c                   21.3999(2)
_cell_measurement_reflns_used    14468
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.8280
_cell_measurement_theta_min      3.3810
_cell_volume                     4306.46(8)
_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                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_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    -36.00  35.00   0.50    0.11    --   55.45 -30.00 -30.00  142
  2  \w      1.00  27.00   0.50    0.05    --    0.00-102.00 -41.00   52
  3  \w     35.00 102.00   0.50    0.11    --   55.45-102.00 -41.00  134
  4  \w     67.00 104.00   0.50    0.11    --  110.90-102.00 -41.00   74
  5  \w     71.00 105.00   0.50    0.11    --  110.90-111.00  60.00   68
  6  \w     49.00 108.00   0.50    0.11    --  110.90 -77.00   0.00  118
  7  \w     41.00  76.00   0.50    0.11    --  110.90 -63.00  30.00   70
  8  \w     28.00  63.00   0.50    0.11    --  110.90 -63.00   0.00   70
  9  \w     24.00  75.00   0.50    0.11    --  110.90 -63.00 -60.00  102
 10  \w     24.00  67.00   0.50    0.11    --  110.90 -63.00 -30.00   86
 11  \w     23.00  59.00   0.50    0.11    --  110.90-111.00  60.00   72
 12  \w     31.00  57.00   0.50    0.11    --  110.90 -50.00  90.00   52
 13  \w     26.00  51.00   0.50    0.11    --  110.90 -50.00 150.00   50
 14  \w     32.00  58.00   0.50    0.11    --  110.90 -50.00 120.00   52
 15  \w     28.00  54.00   0.50    0.11    --  110.90 -50.00  60.00   52
 16  \w     63.00 112.00   0.50    0.11    --  110.90  50.00  90.00   98
 17  \w    134.00 163.00   0.50    0.11    --  110.90  50.00  90.00   58
 18  \w    126.00 173.00   0.50    0.11    --  110.90 102.00  61.00   94
 19  \w    102.00 128.00   0.50    0.11    --   55.45 102.00  61.00   52
 20  \w     86.00 130.00   0.50    0.11    --   55.45 125.00 120.00   88
 21  \w     91.00 120.00   0.50    0.11    --  110.90 102.00  61.00   58
 22  \w     95.00 166.00   0.50    0.11    --  110.90 111.00  30.00  142
 23  \w     91.00 156.00   0.50    0.11    --  110.90 111.00 -60.00  130
 24  \w    109.00 138.00   0.50    0.11    --   55.45 125.00-150.00   58
 25  \w    110.00 136.00   0.50    0.11    --   55.45 125.00-180.00   52
 26  \w     97.00 143.00   0.50    0.11    --  110.90 111.00 -90.00   92
 27  \w     85.00 111.00   0.50    0.11    --   55.45 125.00 -60.00   52
 28  \w     83.00 134.00   0.50    0.11    --   55.45 125.00  90.00  102
 29  \w     26.00  54.00   0.50    0.11    --  110.90 -50.00-180.00   56
 30  \w     24.00  74.00   0.50    0.11    --  110.90 -63.00-180.00  100
 31  \w    -34.00  37.00   0.50    0.11    --   55.45 -30.00  30.00  142
 32  \w    -37.00  34.00   0.50    0.11    --   55.45 -30.00  90.00  142
 33  \w    -35.00  15.00   0.50    0.11    --   55.45 -15.00 120.00  100
 34  \w    -38.00  11.00   0.50    0.11    --  -28.75 102.00  61.00   98
 35  \w    -17.00  14.00   0.50    0.05    --    0.00 102.00  61.00   62
 36  \w    -50.00 -23.00   0.50    0.05    --    0.00 102.00  61.00   54
 37  \w   -121.00 -80.00   0.50    0.11    --  -28.75 -91.00   0.00   82
 38  \w   -125.00 -83.00   0.50    0.11    --  -28.75 -91.00  60.00   84
 39  \w   -117.00 -91.00   0.50    0.11    --  -28.75 -91.00-180.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0408932000
_diffrn_orient_matrix_UB_12      0.0877527000
_diffrn_orient_matrix_UB_13      0.0097609000
_diffrn_orient_matrix_UB_21      -0.0826405000
_diffrn_orient_matrix_UB_22      0.0154381000
_diffrn_orient_matrix_UB_23      0.0439737000
_diffrn_orient_matrix_UB_31      0.0872578000
_diffrn_orient_matrix_UB_32      -0.0263165000
_diffrn_orient_matrix_UB_33      0.0579589000
_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  0.0280
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23685
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.939
_diffrn_reflns_theta_min         3.397
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.415
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29314
_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    1.886
_exptl_crystal_description       block
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.611
_refine_diff_density_min         -1.711
_refine_diff_density_rms         0.127
_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     523
_refine_ls_number_reflns         8175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0315P)^2^+4.8797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7467
_reflns_number_total             8175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao1c06938_si_003.cif
_cod_data_source_block           abe3
_cod_database_code               4519406
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C30H30S4P2Au2
_chemical_oxdiff_usercomment     free
_shelx_estimated_absorpt_t_max   0.308
_shelx_estimated_absorpt_t_min   0.168
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B)
2.b Aromatic/amide H refined with riding coordinates:
 C50(H50), C2(H2), C40(H40), C36(H36), C47(H47), C34(H34), C4(H4), C14(H14),
 C28(H28), C37(H37), C42(H42), C5(H5), C30(H30), C20(H20), C9(H9), C35(H35),
 C10(H10), C11(H11), C3(H3), C32(H32), C49(H49), C38(H38), C48(H48), C24(H24),
 C31(H31), C23(H23), C22(H22), C18(H18), C41(H41), C17(H17), C21(H21), C29(H29),
  C16(H16), C15(H15)
;
_shelx_res_checksum              11758
_shelx_hkl_checksum              63063
_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 2.661
_oxdiff_exptl_absorpt_empirical_full_min 0.670