Cyclometalated Au(III) complexes with alkynylphosphine oxide ligands: synthesis and photophysical properties.
Luginin, Maksim; Snetkov, Dmitry; Sizova, Anastasia; Paderina, Aleksandra; Sizov, Vladimir; Grachova, Elena; Dalton transactions (Cambridge, England : 2003) 54 (2025) 2950–2963; doi:10.1039/d4dt03250k

data_7718253
_publ_section_title
;
 Cyclometalated Au(III) complexes with alkynylphosphine oxide ligands:
 synthesis and photophysical properties.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2950
_journal_page_last               2963
_journal_paper_doi               10.1039/d4dt03250k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C26 H19 O P, C3 H6 O'
_chemical_formula_sum            'C29 H25 O2 P'
_chemical_formula_weight         436.46
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-24
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-15 deposited with the CCDC.	2025-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                72.6870(10)
_cell_angle_beta                 71.715(2)
_cell_angle_gamma                86.117(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2516(2)
_cell_length_b                   9.8241(2)
_cell_length_c                   14.3433(2)
_cell_measurement_reflns_used    10645
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.7020
_cell_measurement_theta_min      3.3310
_cell_volume                     1181.26(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     -9.00  17.00   0.50    0.20    --  -41.10  41.00-143.00   52
  2  \w    -97.00 -66.00   0.50    0.20    --  -41.10 -41.00  64.00   62
  3  \w    -62.00 -36.00   0.50    0.20    --  -41.10 -41.00  64.00   52
  4  \w    -41.00 -15.00   0.50    0.20    --  -41.10  41.00-143.00   52
  5  \w     88.00 144.00   0.50    0.80    --  100.00  41.00-143.00  112
  6  \w     41.00  85.00   0.50    0.80    --  100.00 -41.00  64.00   88
  7  \w     -7.00  21.00   0.50    0.20    --  -41.10  32.00  60.00   56
  8  \w    -43.00 -11.00   0.50    0.20    --  -41.10  32.00  60.00   64
  9  \w    -58.00 -15.00   0.50    0.20    --  -41.10 138.00 -30.00   86
 10  \w    -96.00 -67.00   0.50    0.20    --  -41.10 138.00 -30.00   58
 11  \w    -59.00  24.00   0.50    0.20    --  -41.10  77.00  90.00  166
 12  \w     34.00  65.00   0.50    0.20    --   41.10  21.00  30.00   62
 13  \w     70.00  95.00   0.50    0.20    --   41.10  21.00  30.00   50
 14  \w     65.00  91.00   0.50    0.20    --   41.10  41.00-143.00   52
 15  \w     30.00  76.00   0.50    0.20    --   41.10-104.00-180.00   92
 16  \w     19.00  48.00   0.50    0.20    --   41.10 -54.00  90.00   58
 17  \w    -13.00  12.00   0.50    0.20    --   41.10 -41.00  64.00   50
 18  \w     57.00  96.00   0.50    0.20    --   41.10  32.00 -30.00   78
 19  \w     38.00  63.00   0.50    0.20    --   41.10  41.00-143.00   50
 20  \w    -22.00  47.00   0.50    0.20    --   41.10 -54.00-120.00  138
 21  \w     -6.00  26.00   0.50    0.20    --   41.10-104.00 -30.00   64
 22  \w     30.00  65.00   0.50    0.20    --   41.10-104.00 -30.00   70
 23  \w     29.00  54.00   0.50    0.20    --   41.10 -43.00-120.00   50
 24  \w     39.00 106.00   0.50    0.20    --   41.10  32.00 -90.00  134
 25  \w     26.00  51.00   0.50    0.20    --   41.10 -43.00 150.00   50
 26  \w     -2.00  24.00   0.50    0.20    --   41.10-104.00-180.00   52
 27  \w     92.00 156.00   0.50    0.80    --  100.00  25.00 120.00  128
 28  \w     40.00  65.00   0.50    0.80    --  100.00 -77.00  30.00   50
 29  \w     40.00  79.00   0.50    0.80    --  100.00 -59.00 -60.00   78
 30  \w    132.00 157.00   0.50    0.80    --  100.00  77.00-150.00   50
 31  \w     53.00  79.00   0.50    0.80    --  100.00 -25.00 -60.00   52
 32  \w     41.00  92.00   0.50    0.80    --  100.00 -77.00 150.00  102
 33  \w    101.00 126.00   0.50    0.80    --  100.00 -77.00  30.00   50
 34  \w     89.00 151.00   0.50    0.80    --  100.00  42.00   0.00  124
 35  \w     37.00  62.00   0.50    0.80    --  100.00-111.00 150.00   50
 36  \w    128.00 155.00   0.50    0.80    --  100.00 111.00 -60.00   54
 37  \w     72.00  97.00   0.50    0.80    --  100.00   8.00   0.00   50
 38  \w     68.00 112.00   0.50    0.80    --  100.00 -59.00 120.00   88
 39  \w     58.00 116.00   0.50    0.80    --  100.00 -50.00 150.00  116
 40  \w     89.00 114.00   0.50    0.80    --  100.00 -17.00-150.00   50
 41  \w     32.00  67.00   0.50    0.80    --  100.00 -93.00 -30.00   70
 42  \w     70.00  96.00   0.50    0.80    --  100.00 178.00 150.00   52
 43  \w     37.00 102.00   0.50    0.80    --  100.00-111.00 120.00  130
 44  \w     64.00 109.00   0.50    0.80    --  100.00 -33.00  60.00   90
 45  \w     42.00 101.00   0.50    0.80    --  100.00 -33.00-150.00  118
 46  \w     46.00 113.00   0.50    0.80    --  100.00-133.00 -60.00  134
 47  \w     86.00 148.00   0.50    0.80    --  100.00  17.00-180.00  124
 48  \w     42.00  75.00   0.50    0.80    --  100.00 -17.00-150.00   66
 49  \w    129.00 155.00   0.50    0.80    --  100.00  17.00  90.00   52
 50  \w     97.00 144.00   0.50    0.80    --  100.00 178.00 150.00   94
 51  \w     97.00 125.00   0.50    0.80    --  100.00  59.00-180.00   56
 52  \w    128.00 155.00   0.50    0.80    --  100.00  59.00-180.00   54
 53  \w     90.00 115.00   0.50    0.80    --  100.00  17.00  90.00   50
 54  \w     84.00 117.00   0.50    0.80    --  100.00-133.00 120.00   66
 55  \w    110.00 136.00   0.50    0.80    --  100.00   8.00   0.00   52
 56  \w     49.00 108.00   0.50    0.80    --  100.00-111.00 -60.00  118
 57  \w     91.00 119.00   0.50    0.80    --  100.00 -87.00 120.00   56
 58  \w     56.00  81.00   0.50    0.80    --  100.00-133.00 120.00   50
 59  \w     98.00 124.00   0.50    0.80    --  100.00 133.00-120.00   52
 60  \w    129.00 154.00   0.50    0.80    --  100.00 133.00-120.00   50
 61  \w     40.00 103.00   0.50    0.80    --  100.00 -33.00 -60.00  126
 62  \w     47.00  73.00   0.50    0.80    --  100.00 -77.00   0.00   52
 63  \w     78.00 112.00   0.50    0.80    --  100.00 -87.00 -60.00   68
 64  \w     74.00 108.00   0.50    0.80    --  100.00-111.00   0.00   68
 65  \w     68.00 108.00   0.50    0.80    --  100.00-111.00-180.00   80
 66  \w     81.00 106.00   0.50    0.80    --  100.00-111.00 150.00   50
 67  \w     73.00 116.00   0.50    0.80    --  100.00-133.00 -30.00   86
 68  \w     87.00 157.00   0.50    0.80    --  100.00  50.00-120.00  140
 69  \w     51.00  77.00   0.50    0.80    --  100.00 -87.00 120.00   52
 70  \w     50.00  98.00   0.50    0.80    --  100.00-111.00 -30.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0136170000
_diffrn_orient_matrix_UB_12      -0.1612230000
_diffrn_orient_matrix_UB_13      0.0475066000
_diffrn_orient_matrix_UB_21      0.1749036000
_diffrn_orient_matrix_UB_22      0.0174924000
_diffrn_orient_matrix_UB_23      -0.0392093000
_diffrn_orient_matrix_UB_31      -0.0018237000
_diffrn_orient_matrix_UB_32      0.0265099000
_diffrn_orient_matrix_UB_33      0.1009527000
_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  0.0253
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11900
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.496
_diffrn_reflns_theta_max         67.496
_diffrn_reflns_theta_min         3.393
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.101a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       prism
_exptl_crystal_F_000             460
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.4730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0885
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4084
_reflns_number_total             4248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03250k3.cif
_cod_data_source_block           028-010_2op
_cod_original_cell_volume        1181.27(4)
_cod_database_code               7718253
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C26 H19 O P'
_shelx_estimated_absorpt_t_max   0.778
_shelx_estimated_absorpt_t_min   0.685
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C5(H5), C25(H25), C24(H24), C4(H4), C8(H8), C26(H26), C16(H16),
 C22(H22), C18(H18), C21(H21), C19(H19), C12(H12), C14(H14), C20(H20), C15(H15),
  C13(H13)
2.b :
 C1(H1)
;
_shelx_res_checksum              54878
_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 1.718
_oxdiff_exptl_absorpt_empirical_full_min 0.665