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_4519403
_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         'C49 H36 Au2 P2 S4'
_chemical_formula_sum            'C49 H36 Au2 P2 S4'
_chemical_formula_weight         1208.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 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                 96.0050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.3012(12)
_cell_length_b                   8.9089(8)
_cell_length_c                   16.7670(14)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      29.03
_cell_measurement_theta_min      2.59
_cell_volume                     2124.5(3)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0138
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12225
_diffrn_reflns_point_group_measured_fraction_full 0.688
_diffrn_reflns_point_group_measured_fraction_max 0.612
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.057
_diffrn_reflns_theta_min         1.782
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.205
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_description       block
_exptl_crystal_F_000             1164
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.002(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.735
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         6950
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.735
_refine_ls_R_factor_all          0.0130
_refine_ls_R_factor_gt           0.0125
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0272
_refine_ls_wR_factor_ref         0.0273
_reflns_Friedel_coverage         0.338
_reflns_Friedel_fraction_full    0.381
_reflns_Friedel_fraction_max     0.310
_reflns_number_gt                6767
_reflns_number_total             6950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao1c06938_si_002.cif
_cod_data_source_block           abe_468_2_0m_a
_cod_database_code               4519403
_shelx_shelxl_version_number     2018/3
_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:
 C49(H49A,H49B)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C45(H45), C42(H42), C47(H47), C4(H4), C23(H23), C28(H28), C32(H32),
 C8(H8), C22(H22), C35(H35), C3(H3), C27(H27), C44(H44), C11(H11), C26(H26),
 C14(H14), C36(H36), C15(H15), C20(H20), C46(H46), C29(H29), C41(H41), C9(H9),
 C48(H48), C39(H39), C21(H21), C10(H10), C2(H2), C40(H40), C34(H34), C38(H38),
 C30(H30), C33(H33)
;
_shelx_res_checksum              84153
_shelx_hkl_checksum              55411
_olex2_submission_special_instructions 'No special instructions were received'