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_7718254
_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         'C31 H21 Au N O P'
_chemical_formula_sum            'C31 H21 Au N O P'
_chemical_formula_weight         651.42
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-07-15 deposited with the CCDC.	2025-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                101.2010(10)
_cell_angle_beta                 103.0650(10)
_cell_angle_gamma                110.1950(10)
_cell_formula_units_Z            2
_cell_length_a                   8.33300(10)
_cell_length_b                   11.2128(2)
_cell_length_c                   14.25730(10)
_cell_measurement_reflns_used    11158
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.1500
_cell_measurement_theta_min      3.3410
_cell_volume                     1162.62(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_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            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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     95.00 177.00   0.50    0.10    --  105.93  45.00-180.00  164
  2  \w     97.00 155.00   0.50    0.10    --  105.93  15.00   0.00  116
  3  \w     99.00 175.00   0.50    0.10    --  105.93  30.00  30.00  152
  4  \w    120.00 176.00   0.50    0.10    --  105.93  39.00  81.00  112
  5  \w     59.00 117.00   0.50    0.05    --   47.38  39.00  81.00  116
  6  \w    -20.00  26.00   0.50    0.05    --   47.38 -19.00 150.00   92
  7  \w    -15.00  10.00   0.50    0.05    --   47.38 -57.00  60.00   50
  8  \w     23.00  62.00   0.50    0.05    --   47.38 -57.00  60.00   78
  9  \w    -17.00  44.00   0.50    0.05    --   47.38 -39.00 -72.00  122
 10  \w     42.00  67.00   0.50    0.10    --  105.93 -61.00  30.00   50
 11  \w     39.00  65.00   0.50    0.10    --  105.93 -61.00  90.00   52
 12  \w     34.00  59.00   0.50    0.10    --  105.93 -61.00   0.00   50
 13  \w     41.00  67.00   0.50    0.10    --  105.93 -61.00-180.00   52
 14  \w     34.00  71.00   0.50    0.10    --  105.93 -61.00-150.00   74
 15  \w     60.00 112.00   0.50    0.10    --  105.93-125.00   0.00  104
 16  \w     33.00 103.00   0.50    0.10    --  105.93 -94.00   0.00  140
 17  \w     38.00  64.00   0.50    0.10    --  105.93 -94.00  90.00   52
 18  \w     62.00 105.00   0.50    0.10    --  105.93 -94.00 150.00   86
 19  \w     48.00  98.00   0.50    0.10    --  105.93 -94.00 -90.00  100
 20  \w     72.00 100.00   0.50    0.10    --  105.93 -94.00-150.00   56
 21  \w     37.00  63.00   0.50    0.10    --  105.93 -94.00-150.00   52
 22  \w     37.00 112.00   0.50    0.10    --  105.93-125.00-180.00  150
 23  \w     20.00  46.00   0.50    0.05    --   47.38-125.00-180.00   52
 24  \w     63.00  89.00   0.50    0.05    --   47.38-125.00-150.00   52
 25  \w     55.00  95.00   0.50    0.05    --   47.38-125.00-180.00   80
 26  \w   -110.00 -84.00   0.50    0.10    -- -105.93 125.00-120.00   52
 27  \w   -111.00 -85.00   0.50    0.10    -- -105.93 125.00 -30.00   52
 28  \w   -110.00 -35.00   0.50    0.10    -- -105.93 125.00  60.00  150
 29  \w   -109.00 -74.00   0.50    0.10    -- -105.93 125.00  90.00   70
 30  \w   -100.00 -70.00   0.50    0.10    -- -105.93  77.00  60.00   60
 31  \w    -65.00 -39.00   0.50    0.10    -- -105.93  77.00  60.00   52
 32  \w    -65.00 -34.00   0.50    0.10    -- -105.93  61.00   0.00   62
 33  \w    -66.00 -37.00   0.50    0.10    -- -105.93  61.00-120.00   58
 34  \w    -35.00  -9.00   0.50    0.05    --  -47.38  39.00  81.00   52
 35  \w   -163.00 -93.00   0.50    0.10    -- -105.93 -30.00 150.00  140
 36  \w   -168.00 -95.00   0.50    0.10    -- -105.93 -45.00 -90.00  146
 37  \w   -120.00 -93.00   0.50    0.10    -- -105.93 -39.00 -72.00   54
 38  \w   -176.00-150.00   0.50    0.10    -- -105.93 -30.00-180.00   52
 39  \w   -120.00 -53.00   0.50    0.05    --  -47.38 -39.00 -72.00  134
 40  \w   -120.00 -76.00   0.50    0.05    --  -47.38-125.00-120.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1099671000
_diffrn_orient_matrix_UB_12      -0.1490963000
_diffrn_orient_matrix_UB_13      -0.0570750000
_diffrn_orient_matrix_UB_21      0.1749182000
_diffrn_orient_matrix_UB_22      -0.0154376000
_diffrn_orient_matrix_UB_23      -0.0047429000
_diffrn_orient_matrix_UB_31      0.0221664000
_diffrn_orient_matrix_UB_32      -0.0323949000
_diffrn_orient_matrix_UB_33      0.1011058000
_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  0.0461
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12886
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.443
_diffrn_reflns_theta_max         67.443
_diffrn_reflns_theta_min         3.334
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.740
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.103a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_description       prism
_exptl_crystal_F_000             632
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.216
_refine_diff_density_min         -1.431
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0424P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4101
_reflns_number_total             4173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03250k3.cif
_cod_data_source_block           0ver0-23725_mel2011n0p
_cod_database_code               7718254
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C31 H21 Au N O P'
_shelx_estimated_absorpt_t_max   0.429
_shelx_estimated_absorpt_t_min   0.269
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C27(H27), C31(H31), C5(H5), C30(H30), C3(H3), C22(H22), C29(H29),
 C21(H21), C28(H28), C10(H10), C23(H23), C8(H8), C16(H16), C24(H24), C13(H13),
 C4(H4), C2(H2), C14(H14), C15(H15), C9(H9)
;
_shelx_res_checksum              1953
_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 1.670
_oxdiff_exptl_absorpt_empirical_full_min 0.495