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_7718257
_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         'C41 H27 Au N O P, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C41.5 H28 Au Cl N O P'
_chemical_formula_weight         820.03
_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             2023-07-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-07-15 deposited with the CCDC.	2025-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                110.4550(10)
_cell_angle_beta                 90.6980(10)
_cell_angle_gamma                92.1300(10)
_cell_formula_units_Z            4
_cell_length_a                   8.28270(10)
_cell_length_b                   18.7788(2)
_cell_length_c                   22.4908(2)
_cell_measurement_reflns_used    22703
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.0020
_cell_measurement_theta_min      2.0920
_cell_volume                     3274.18(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (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 2018/2 (Sheldrick, 2018)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     21.00  68.00   0.50    0.20    --   35.49-112.00 -56.00   94
  2  \w     66.00  92.00   0.50    0.25    --  100.00-112.00 -56.00   52
  3  \w    119.00 145.00   0.50    0.25    --  100.00 112.00  36.00   52
  4  \w     31.00  56.00   0.50    0.25    --  100.00-112.00 -56.00   50
  5  \w    -11.00  14.00   0.50    0.20    --  -35.49 104.00-150.00   50
  6  \w    -30.00  14.00   0.50    0.20    --  -35.49 104.00 -30.00   88
  7  \w   -103.00 -72.00   0.50    0.20    --  -35.49 -65.00  90.00   62
  8  \w    -72.00 -21.00   0.50    0.20    --  -35.49 104.00-150.00  102
  9  \w    -75.00 -44.00   0.50    0.20    --  -35.49 138.00  90.00   62
 10  \w   -103.00 -56.00   0.50    0.20    --  -35.49 -54.00-180.00   94
 11  \w    -36.00  30.00   0.50    0.20    --  -35.49  65.00  60.00  132
 12  \w    -46.00 -14.00   0.50    0.20    --  -35.49  77.00  60.00   64
 13  \w    -62.00  30.00   0.50    0.20    --  -35.49  65.00  30.00  184
 14  \w    -64.00  -9.00   0.50    0.20    --  -35.49 -65.00  90.00  110
 15  \w    -64.00 -38.00   0.50    0.20    --  -35.49 104.00 -30.00   52
 16  \w    -71.00 -26.00   0.50    0.20    --  -35.49 112.00  36.00   90
 17  \w    -51.00  26.00   0.50    0.20    --  -35.49  54.00 -30.00  154
 18  \w    -59.00 -20.00   0.50    0.20    --  -35.49 -32.00 150.00   78
 19  \w   -102.00  -9.00   0.50    0.20    --  -35.49 -65.00 120.00  186
 20  \w    -40.00 -15.00   0.50    0.20    --  -35.49 -54.00-180.00   50
 21  \w    -81.00 -19.00   0.50    0.20    --  -35.49 138.00  30.00  124
 22  \w     10.00  35.00   0.50    0.20    --  -35.49  77.00  60.00   50
 23  \w    -31.00  61.00   0.50    0.20    --   35.49 -65.00 150.00  184
 24  \w     71.00  96.00   0.50    0.20    --   35.49  43.00  30.00   50
 25  \w     10.00  80.00   0.50    0.20    --   35.49  65.00 -60.00  140
 26  \w     16.00  50.00   0.50    0.20    --   35.49  43.00  30.00   68
 27  \w     54.00 107.00   0.50    0.20    --   35.49  11.00-150.00  106
 28  \w      7.00  39.00   0.50    0.20    --   35.49  11.00-150.00   64
 29  \w      2.00  29.00   0.50    0.20    --   35.49 -21.00-150.00   54
 30  \w     37.00  65.00   0.50    0.20    --   35.49 -21.00-150.00   56
 31  \w    -38.00  -4.00   0.50    0.20    --   35.49 -21.00-150.00   68
 32  \w     62.00 119.00   0.50    0.25    --  100.00 -77.00 -30.00  114
 33  \w     84.00 156.00   0.50    0.25    --  100.00  91.00 150.00  144
 34  \w     65.00 124.00   0.50    0.25    --  100.00 -61.00  90.00  118
 35  \w     75.00 101.00   0.50    0.25    --  100.00-149.00 -60.00   52
 36  \w     86.00 135.00   0.50    0.25    --  100.00  30.00  30.00   98
 37  \w     27.00  98.00   0.50    0.25    --  100.00-107.00 120.00  142
 38  \w     76.00 104.00   0.50    0.25    --  100.00 -91.00-150.00   56
 39  \w     36.00  70.00   0.50    0.25    --  100.00 -91.00-150.00   68
 40  \w    101.00 157.00   0.50    0.25    --  100.00  45.00  60.00  112
 41  \w     26.00 101.00   0.50    0.25    --  100.00-107.00   0.00  150
 42  \w    124.00 150.00   0.50    0.25    --  100.00  61.00-120.00   52
 43  \w     64.00  93.00   0.50    0.25    --  100.00 -45.00 -60.00   58
 44  \w    121.00 156.00   0.50    0.25    --  100.00  45.00 -30.00   70
 45  \w     65.00 156.00   0.50    0.25    --  100.00 149.00 150.00  182
 46  \w     87.00 112.00   0.50    0.25    --  100.00-125.00-150.00   50
 47  \w     88.00 116.00   0.50    0.25    --  100.00  61.00-120.00   56
 48  \w     32.00  64.00   0.50    0.25    --  100.00-125.00-150.00   64
 49  \w     65.00  90.00   0.50    0.25    --  100.00 -86.00  30.00   50
 50  \w     48.00  73.00   0.50    0.25    --  100.00-107.00  30.00   50
 51  \w     77.00 113.00   0.50    0.25    --  100.00 -37.00 120.00   72
 52  \w     25.00  76.00   0.50    0.25    --  100.00 -91.00-180.00  102
 53  \w     34.00 124.00   0.50    0.25    --  100.00 -61.00-180.00  180
 54  \w    111.00 157.00   0.50    0.25    --  100.00  53.00 -60.00   92
 55  \w     32.00  58.00   0.50    0.25    --  100.00 -45.00 -60.00   52
 56  \w     83.00 143.00   0.50    0.25    --  100.00 107.00-120.00  120
 57  \w     37.00  90.00   0.50    0.25    --  100.00-149.00  60.00  106
 58  \w    104.00 129.00   0.50    0.25    --  100.00-149.00  60.00   50
 59  \w     48.00  73.00   0.50    0.25    --  100.00-107.00  90.00   50
 60  \w     34.00 112.00   0.50    0.25    --  100.00-125.00 120.00  156
 61  \w     51.00  90.00   0.50    0.25    --  100.00-107.00 -30.00   78
 62  \w     33.00 105.00   0.50    0.25    --  100.00 -96.00 161.73  144
 63  \w    131.00 156.00   0.50    0.25    --  100.00  77.00 -30.00   50
 64  \w     91.00 117.00   0.50    0.25    --  100.00  77.00 -30.00   52
 65  \w     34.00  60.00   0.50    0.25    --  100.00 -86.00 -30.00   52
 66  \w     61.00 104.00   0.50    0.25    --  100.00  15.00 -90.00   86
 67  \w    128.00 153.00   0.50    0.25    --  100.00  22.00 -90.00   50
 68  \w     30.00  68.00   0.50    0.25    --  100.00 -37.00   0.00   76
 69  \w     79.00 114.00   0.50    0.25    --  100.00  22.00 -90.00   70
 70  \w     38.00  98.00   0.50    0.25    --  100.00-107.00 150.00  120
 71  \w     76.00 109.00   0.50    0.25    --  100.00 -77.00-150.00   66
 72  \w     86.00 111.00   0.50    0.25    --  100.00-125.00 -60.00   50
 73  \w     87.00 129.00   0.50    0.25    --  100.00 -77.00  60.00   84
 74  \w    116.00 141.00   0.50    0.25    --  100.00  77.00-150.00   50
 75  \w    109.00 134.00   0.50    0.25    --  100.00  15.00  30.00   50
 76  \w     67.00  92.00   0.50    0.25    --  100.00  15.00  30.00   50
 77  \w     42.00  68.00   0.50    0.25    --  100.00-107.00-180.00   52
 78  \w     80.00 105.00   0.50    0.25    --  100.00-107.00-180.00   50
 79  \w     31.00  71.00   0.50    0.25    --  100.00-125.00 -60.00   80
 80  \w     60.00  85.00   0.50    0.25    --  100.00-125.00  60.00   50
 81  \w     80.00 130.00   0.50    0.25    --  100.00  61.00   0.00  100
 82  \w     71.00 105.00   0.50    0.25    --  100.00 -97.00-156.45   68
 83  \w     85.00 157.00   0.50    0.25    --  100.00  77.00 -90.00  144
 84  \w     78.00 117.00   0.50    0.25    --  100.00 -30.00 -60.00   78
 85  \w     46.00  82.00   0.50    0.25    --  100.00-149.00 120.00   72
 86  \w    104.00 129.00   0.50    0.25    --  100.00-149.00 120.00   50
 87  \w     25.00  58.00   0.50    0.25    --  100.00 -91.00 120.00   66
 88  \w     81.00 107.00   0.50    0.25    --  100.00  45.00 -30.00   52
 89  \w    -21.00   4.00   0.50    0.20    --  -35.49 112.00  36.00   50
 90  \w    -43.00 -18.00   0.50    0.20    --    8.00 122.00 -23.66   50
 91  \w    -30.00  -5.00   0.50    0.20    --   20.00 121.00-129.00   50
 92  \w    -49.00 -24.00   0.50    0.20    --   24.00 156.00 -60.32   50
 93  \w     -8.00   7.50   0.50    0.20    --   28.00  96.00 115.68   31
;
_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      -0.0418551000
_diffrn_orient_matrix_UB_12      0.0327078000
_diffrn_orient_matrix_UB_13      0.0707140000
_diffrn_orient_matrix_UB_21      -0.0893435000
_diffrn_orient_matrix_UB_22      0.0643810000
_diffrn_orient_matrix_UB_23      -0.0120486000
_diffrn_orient_matrix_UB_31      -0.1579056000
_diffrn_orient_matrix_UB_32      -0.0496663000
_diffrn_orient_matrix_UB_33      -0.0142447000
_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  0.0330
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            35609
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.496
_diffrn_reflns_theta_max         67.496
_diffrn_reflns_theta_min         2.097
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.926
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_description       prism
_exptl_crystal_F_000             1612
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.922
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         11732
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+0.6311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0640
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10787
_reflns_number_total             11732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03250k3.cif
_cod_data_source_block           1ver0-23647_mel-183_auto
_cod_original_formula_sum        'C41.50 H28 Au Cl N O P'
_cod_database_code               7718257
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C83 H56 Au2 N2 O2 P2 Cl2'
_shelx_estimated_absorpt_t_max   0.587
_shelx_estimated_absorpt_t_min   0.219
_reflns_odcompleteness_completeness 89.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     75.12
_olex2_refinement_description
;
1. Restrained distances
 Cl-C02H
 1.8 with sigma of 0.02
 Cl06-C02H = Cl-C02H
 1.77 with sigma of 0.05
2. Others
 Fixed Sof: Cl06(0.7) H02H(0.7) H02M(0.7) H02N(0.3) H02O(0.3) Cl(0.3)
3.a Secondary CH2 refined with riding coordinates:
 C02H(H02H,H02M), C02H(H02N,H02O)
3.b Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00M(H00M), C00N(H00N), C00P(H00P), C00R(H00R), C00T(H00T),
 C00W(H00W), C00X(H00X), C00Y(H00Y), C011(H011), C013(H013), C017(H017),
 C018(H018), C01A(H01A), C01E(H01E), C01F(H01F), C01G(H01G), C01H(H01H),
 C01K(H01K), C01L(H01L), C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P),
 C01Q(H01Q), C01R(H01R), C01S(H01S), C01T(H01T), C01U(H01U), C01V(H01V),
 C01W(H01W), C01X(H01X), C01Y(H01Y), C01Z(H01Z), C020(H020), C021(H021),
 C022(H022), C023(H023), C024(H024), C025(H025), C026(H026), C028(H028),
 C029(H029), C02A(H02A), C02B(H02B), C02C(H02C), C02D(H02D), C02E(H02E),
 C02F(H02F), C02G(H02G), C02I(H02I), C02J(H02J), C02K(H02K), C02L(H02L)
;
_shelx_res_checksum              12334
_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 1.685
_oxdiff_exptl_absorpt_empirical_full_min 0.687