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_4519405
_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(C51 H40 Au2 P2 S4), 3(C3 H6 O)'
_chemical_formula_sum            'C111 H98 Au4 O3 P4 S8'
_chemical_formula_weight         2648.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4800(4)
_cell_length_b                   16.1182(3)
_cell_length_c                   33.0678(6)
_cell_measurement_reflns_used    17770
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.6800
_cell_measurement_theta_min      3.6120
_cell_volume                     9849.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.54a (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 0.998
_diffrn_measured_fraction_theta_max 0.948
_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    -24.00  57.00   0.50    0.33    --   46.45 -55.00 119.00  162
  2  \w     39.00  65.00   0.50    1.34    --  104.61 -55.00 119.00   52
  3  \w     33.00  73.00   0.50    1.34    --  104.61 -61.00  90.00   80
  4  \w    -23.00  11.00   0.50    0.33    --   46.45 -19.00  60.00   68
  5  \w    -21.00  18.00   0.50    0.33    --  -46.45  19.00   0.00   78
  6  \w    -58.00 -33.00   0.50    1.34    -- -102.00  61.00  30.00   50
  7  \w    -71.00 -37.00   0.50    1.34    -- -102.00  65.00  75.00   68
  8  \w    -69.00 -30.00   0.50    1.34    -- -102.00  61.00  60.00   78
  9  \w    -91.00 -48.00   0.50    1.34    -- -102.00  77.00 150.00   86
 10  \w    -95.00 -33.00   0.50    1.34    -- -102.00  77.00 120.00  124
 11  \w   -175.00-113.00   0.50    1.34    -- -102.00 -65.00 -60.00  124
 12  \w   -107.00 -65.00   0.50    0.33    --  -46.45-139.00-110.00   84
 13  \w   -152.00 -72.00   0.50    1.34    -- -102.00-130.00  63.00  160
;
_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      -0.0621699000
_diffrn_orient_matrix_UB_12      -0.0616684000
_diffrn_orient_matrix_UB_13      0.0074917000
_diffrn_orient_matrix_UB_21      -0.0082644000
_diffrn_orient_matrix_UB_22      -0.0126303000
_diffrn_orient_matrix_UB_23      -0.0459317000
_diffrn_orient_matrix_UB_31      0.0550909000
_diffrn_orient_matrix_UB_32      -0.0718052000
_diffrn_orient_matrix_UB_33      0.0016421000
_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  0.0339
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            38754
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.995
_diffrn_reflns_theta_min         3.587
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.557
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.54a (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    1.786
_exptl_crystal_description       block
_exptl_crystal_F_000             5168
_refine_diff_density_max         2.237
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.125
_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     590
_refine_ls_number_reflns         9762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0415P)^2^+22.0761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8672
_reflns_number_total             9762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao1c06938_si_004.cif
_cod_data_source_block           190710_abe_2
_cod_database_code               4519405
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         AuSPC50H50
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C50(H50A,H50B), C49(H49A,H49B)
2.b Aromatic/amide H refined with riding coordinates:
 C48(H48), C2(H2), C3(H3), C44(H44), C47(H47), C14(H14), C38(H38), C46(H46),
 C8(H8), C15(H15), C4(H4), C41(H41), C45(H45), C32(H32), C42(H42), C39(H39),
 C16(H16), C40(H40), C9(H9), C11(H11), C36(H36), C10(H10), C26(H26), C20(H20),
 C30(H30), C35(H35), C22(H22), C28(H28), C33(H33), C23(H23), C27(H27), C34(H34),
  C29(H29), C21(H21)
2.c Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C53(H53A,H53B,H53C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              38216
_shelx_hkl_checksum              64852
_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 1.765
_oxdiff_exptl_absorpt_empirical_full_min 0.765