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_7718256
_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         'C24 H17 O P'
_chemical_formula_sum            'C24 H17 O P'
_chemical_formula_weight         352.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 99.3820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.99820(10)
_cell_length_b                   10.97300(10)
_cell_length_c                   17.4331(2)
_cell_measurement_reflns_used    16136
_cell_measurement_temperature    99.9(6)
_cell_measurement_theta_max      71.7360
_cell_measurement_theta_min      4.4830
_cell_volume                     1887.01(3)
_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      99.9(6)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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    -64.00 -37.00   0.50    0.80    --  -41.10 118.00 168.00   54
  2  \w   -100.00 -74.00   0.50    0.80    --  -41.10-158.00 -71.00   52
  3  \w    -29.00  -4.00   0.50    0.80    --  -41.10 118.00 168.00   50
  4  \w     57.00  82.00   0.50    0.80    --   41.10 158.00 -37.00   50
  5  \w     42.00  77.00   0.50    0.80    --   41.10-118.00  82.00   70
  6  \w      1.00  33.00   0.50    0.80    --   41.10-118.00  82.00   64
  7  \w     58.00  84.00   0.50    6.00    --  100.00-118.00  82.00   52
  8  \w    111.00 145.00   0.50    6.00    --  100.00 118.00 168.00   68
  9  \w    109.00 134.00   0.50    6.00    --  100.00-158.00 -71.00   50
 10  \w    -92.00 -30.00   0.50    0.80    --  -41.10 138.00-180.00  124
 11  \w    -83.00 -58.00   0.50    0.80    --  -41.10 158.00 -37.00   50
 12  \w   -103.00 -75.00   0.50    0.80    --  -41.10 -54.00  30.00   56
 13  \w    -62.00 -33.00   0.50    0.80    --  -41.10 -21.00-150.00   58
 14  \w   -104.00 -79.00   0.50    0.80    --  -41.10 -21.00-150.00   50
 15  \w    -59.00 -24.00   0.50    0.80    --  -41.10 -54.00  30.00   70
 16  \w     34.00  60.00   0.50    0.80    --   41.10  65.00   0.00   52
 17  \w    -19.00  66.00   0.50    0.80    --   41.10 -77.00 -60.00  170
 18  \w     69.00 101.00   0.50    0.80    --   41.10  65.00   0.00   64
 19  \w     -1.00  38.00   0.50    0.80    --   41.10 -32.00 -90.00   78
 20  \w     28.00  82.00   0.50    0.80    --   41.10  43.00 -60.00  108
 21  \w     43.00  68.00   0.50    0.80    --   41.10-158.00 -71.00   50
 22  \w     50.00  99.00   0.50    6.00    --  100.00-111.00 -90.00   98
 23  \w     80.00 114.00   0.50    6.00    --  100.00 -68.00 -90.00   68
 24  \w    105.00 131.00   0.50    6.00    --  100.00  93.00-150.00   52
 25  \w     36.00  67.00   0.50    6.00    --  100.00 -68.00 -90.00   62
 26  \w     42.00 142.00   0.50    6.00    --  100.00 178.00 -60.00  200
 27  \w    108.00 155.00   0.50    6.00    --  100.00  17.00   0.00   94
 28  \w     32.00  58.00   0.50    6.00    --  100.00 -25.00  30.00   52
 29  \w     82.00 108.00   0.50    6.00    --  100.00-111.00 150.00   52
 30  \w     39.00  72.00   0.50    6.00    --  100.00-111.00 150.00   66
 31  \w     95.00 155.00   0.50    6.00    --  100.00  42.00 120.00  120
 32  \w     37.00 108.00   0.50    6.00    --  100.00-111.00  90.00  142
 33  \w     59.00 103.00   0.50    6.00    --  100.00 -25.00-180.00   88
 34  \w     31.00  97.00   0.50    6.00    --  100.00 -93.00 -90.00  132
 35  \w     30.00  55.00   0.50    6.00    --  100.00 -17.00   0.00   50
 36  \w     79.00 105.00   0.50    6.00    --  100.00 -17.00   0.00   52
 37  \w     42.00  85.00   0.50    6.00    --  100.00-111.00 -30.00   86
 38  \w     84.00 140.00   0.50    6.00    --  100.00  59.00-180.00  112
 39  \w     47.00 119.00   0.50    6.00    --  100.00 -77.00  60.00  144
 40  \w     38.00 104.00   0.50    6.00    --  100.00 -25.00 -90.00  132
 41  \w    128.00 153.00   0.50    6.00    --  100.00 111.00-150.00   50
 42  \w     77.00 109.00   0.50    6.00    --  100.00 -25.00  30.00   64
 43  \w     25.00  57.00   0.50    0.80    --   41.10  65.00 -30.00   64
 44  \w    -42.00  -9.00   0.50    0.80    --  -41.10  43.00-180.00   66
 45  \w    -22.00  14.00   0.50    0.80    --  -41.10  32.00  60.00   72
 46  \w    -66.00 -28.00   0.50    0.80    --  -41.10 138.00  60.00   76
 47  \w     31.00  57.00   0.50    0.80    --   41.10  21.00-180.00   52
 48  \w    -22.00  33.00   0.50    0.80    --   41.10 -32.00-150.00  110
 49  \w     72.00  97.00   0.50    0.80    --   41.10  32.00 -60.00   50
 50  \w     59.00  85.00   0.50    0.80    --   41.10  65.00 -30.00   52
 51  \w     82.00 111.00   0.50    0.80    --   41.10  21.00-180.00   58
 52  \w     50.00  75.00   0.50    6.00    --  100.00-133.00   0.00   50
 53  \w    102.00 143.00   0.50    6.00    --  100.00  77.00-120.00   82
 54  \w     91.00 118.00   0.50    6.00    --  100.00  33.00 -60.00   54
 55  \w     50.00  99.00   0.50    6.00    --  100.00 -25.00  90.00   98
 56  \w     73.00 122.00   0.50    6.00    --  100.00 133.00-120.00   98
 57  \w     89.00 115.00   0.50    6.00    --  100.00-133.00   0.00   52
 58  \w     83.00 131.00   0.50    6.00    --  100.00  59.00-150.00   96
 59  \w    122.00 157.00   0.50    6.00    --  100.00  93.00  30.00   70
 60  \w     55.00 116.00   0.50    6.00    --  100.00 -50.00  60.00  122
 61  \w     82.00 108.00   0.50    6.00    --  100.00-133.00 -30.00   52
 62  \w    110.00 149.00   0.50    6.00    --  100.00 133.00-150.00   78
 63  \w     73.00 106.00   0.50    6.00    --  100.00-111.00  30.00   66
 64  \w     94.00 154.00   0.50    6.00    --  100.00 133.00 150.00  120
 65  \w     63.00 108.00   0.50    6.00    --  100.00-111.00-150.00   90
 66  \w    132.00 157.00   0.50    6.00    --  100.00  50.00  90.00   50
 67  \w     61.00 121.00   0.50    6.00    --  100.00 -68.00 120.00  120
 68  \w    104.00 157.00   0.50    6.00    --  100.00  50.00  60.00  106
 69  \w    120.00 152.00   0.50    6.00    --  100.00  77.00-150.00   64
 70  \w     85.00 116.00   0.50    6.00    --  100.00  93.00  60.00   62
 71  \w     68.00  94.00   0.50    6.00    --  100.00-111.00-120.00   52
 72  \w     31.00  65.00   0.50    6.00    --  100.00 -93.00 -30.00   68
 73  \w     58.00  99.00   0.50    6.00    --  100.00 -93.00 120.00   82
 74  \w     89.00 114.00   0.50    6.00    --  100.00  50.00  90.00   50
 75  \w     83.00 108.00   0.50    6.00    --  100.00-111.00 -90.00   50
 76  \w     98.00 124.00   0.50    6.00    --  100.00  33.00 120.00   52
 77  \w    127.00 153.00   0.50    6.00    --  100.00  93.00  60.00   52
 78  \w     76.00 102.00   0.50    6.00    --  100.00 -77.00 -30.00   52
 79  \w     55.00  80.00   0.50    6.00    --  100.00-133.00-180.00   50
 80  \w     79.00 105.00   0.50    6.00    --  100.00-111.00   0.00   52
 81  \w     54.00  79.00   0.50    6.00    --  100.00 -42.00 120.00   50
;
_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      -0.1275340000
_diffrn_orient_matrix_UB_12      0.0797501000
_diffrn_orient_matrix_UB_13      -0.0204901000
_diffrn_orient_matrix_UB_21      -0.0900885000
_diffrn_orient_matrix_UB_22      -0.1139366000
_diffrn_orient_matrix_UB_23      0.0000935000
_diffrn_orient_matrix_UB_31      -0.0036735000
_diffrn_orient_matrix_UB_32      0.0188975000
_diffrn_orient_matrix_UB_33      0.0872165000
_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  0.0556
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21078
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.495
_diffrn_reflns_theta_max         67.495
_diffrn_reflns_theta_min         4.482
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.347
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68950
_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    1.240
_exptl_crystal_description       prism
_exptl_crystal_F_000             736
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0575P)^2^+0.6736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3203
_reflns_number_total             3370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03250k3.cif
_cod_data_source_block           028-010_nop
_cod_database_code               7718256
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C24 H17 O P'
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.774
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C4(H4), C9(H9), C5(H5), C8(H8), C14(H14), C10(H10), C20(H20),
 C18(H18), C24(H24), C15(H15), C16(H16), C21(H21), C22(H22), C17(H17), C23(H23)
2.b :
 C1(H1)
;
_shelx_res_checksum              78018
_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 4.860
_oxdiff_exptl_absorpt_empirical_full_min 0.527