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_7718258
_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         'C47 H29 Au N O P'
_chemical_formula_sum            'C47 H29 Au N O P'
_chemical_formula_weight         851.65
_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             2024-11-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-11-01 deposited with the CCDC.	2025-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.3580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.09660(10)
_cell_length_b                   20.6876(2)
_cell_length_c                   11.94570(10)
_cell_measurement_reflns_used    13938
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.3800
_cell_measurement_theta_min      3.1490
_cell_volume                     3462.24(5)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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    -11.00  18.00   0.50    0.35    --  -38.45  96.00  15.00   58
  2  \w    -65.00 -26.00   0.50    0.35    --  -38.45  96.00  15.00   78
  3  \w     43.00  87.00   0.50    1.40    --  100.00 -96.00 -94.00   88
  4  \w     98.00 152.00   0.50    1.40    --  100.00  96.00  15.00  108
  5  \w    -51.00  -9.00   0.50    0.35    --  -38.45  32.00-150.00   84
  6  \w    -58.00 -27.00   0.50    0.35    --  -38.45  54.00  30.00   62
  7  \w    -56.00 -31.00   0.50    0.35    --  -38.45 -65.00  90.00   50
  8  \w    -55.00  -5.00   0.50    0.35    --  -38.45  43.00 -30.00  100
  9  \w     -6.00  27.00   0.50    0.35    --  -38.45  32.00-150.00   66
 10  \w   -101.00 -65.00   0.50    0.35    --  -38.45 -65.00  90.00   72
 11  \w    -99.00 -29.00   0.50    0.35    --  -38.45 -32.00-150.00  140
 12  \w    -12.00  21.00   0.50    0.35    --  -38.45  54.00  30.00   66
 13  \w    -48.00  22.00   0.50    0.35    --  -38.45  54.00-150.00  140
 14  \w      1.00  26.00   0.50    0.35    --  -38.45  43.00 -30.00   50
 15  \w     -4.00  21.00   0.50    0.35    --  -38.45  43.00   0.00   50
 16  \w    -51.00 -24.00   0.50    0.35    --  -38.45  43.00   0.00   54
 17  \w     74.00  99.00   0.50    0.35    --   38.45  32.00-120.00   50
 18  \w     36.00  61.00   0.50    0.35    --   38.45 -96.00 -94.00   50
 19  \w     26.00  63.00   0.50    0.35    --   38.45  65.00  30.00   74
 20  \w     84.00 110.00   0.50    1.40    --  100.00 -53.00 120.00   52
 21  \w     37.00  68.00   0.50    1.40    --  100.00 -53.00 120.00   62
 22  \w    111.00 137.00   0.50    1.40    --  100.00  93.00 -90.00   52
 23  \w     49.00 117.00   0.50    1.40    --  100.00-133.00 150.00  136
 24  \w     84.00 157.00   0.50    1.40    --  100.00  93.00   0.00  146
 25  \w     50.00  76.00   0.50    1.40    --  100.00 -53.00   0.00   52
 26  \w     94.00 157.00   0.50    1.40    --  100.00  77.00-180.00  126
 27  \w     32.00 129.00   0.50    1.40    --  100.00 -86.00 -90.00  194
 28  \w     67.00 108.00   0.50    1.40    --  100.00-111.00 150.00   82
 29  \w     44.00 102.00   0.50    1.40    --  100.00 -93.00 150.00  116
 30  \w     27.00  72.00   0.50    1.40    --  100.00 -93.00-120.00   90
 31  \w     85.00 111.00   0.50    1.40    --  100.00  93.00 150.00   52
 32  \w     71.00 122.00   0.50    1.40    --  100.00 -61.00 -90.00  102
 33  \w     86.00 157.00   0.50    1.40    --  100.00  30.00 -30.00  142
 34  \w     86.00 130.00   0.50    1.40    --  100.00  30.00-180.00   88
 35  \w     79.00 156.00   0.50    1.40    --  100.00  69.00 -90.00  154
 36  \w     87.00 123.00   0.50    1.40    --  100.00  22.00  60.00   72
 37  \w     40.00  65.00   0.50    1.40    --  100.00-111.00  30.00   50
 38  \w    126.00 153.00   0.50    1.40    --  100.00  93.00 150.00   54
 39  \w     44.00 104.00   0.50    1.40    --  100.00 -69.00 -90.00  120
 40  \w     86.00 147.00   0.50    1.40    --  100.00 111.00 -30.00  122
;
_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      0.0323109000
_diffrn_orient_matrix_UB_12      0.0536330000
_diffrn_orient_matrix_UB_13      -0.0767890000
_diffrn_orient_matrix_UB_21      0.0795632000
_diffrn_orient_matrix_UB_22      -0.0444982000
_diffrn_orient_matrix_UB_23      -0.0343391000
_diffrn_orient_matrix_UB_31      -0.0687289000
_diffrn_orient_matrix_UB_32      -0.0261795000
_diffrn_orient_matrix_UB_33      -0.0988118000
_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  0.0352
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19947
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.485
_diffrn_reflns_theta_max         67.485
_diffrn_reflns_theta_min         3.154
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.723
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64978
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       prism
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.563
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         6209
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0319P)^2^+7.8814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5793
_reflns_number_total             6209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03250k3.cif
_cod_data_source_block           031-004_au6
_cod_database_code               7718258
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C47 H29 Au N O P'
_shelx_estimated_absorpt_t_max   0.722
_shelx_estimated_absorpt_t_min   0.476
_reflns_odcompleteness_completeness 98.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     70.93
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C20) = Uanis(C27)
Uanis(C20) = Uanis(C47) = Uanis(C42) = Uanis(C27) = Uanis(C26) = Uanis(C21)
3.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C2(H2), C22(H22), C35(H35), C15(H15), C37(H37), C23(H23), C13(H13),
 C34(H34), C46(H46), C45(H45), C16(H16), C44(H44), C8(H8), C10(H10), C3(H3),
 C24(H24), C33(H33), C9(H9), C14(H14), C43(H43), C38(H38), C39(H39), C4(H4),
 C41(H41), C31(H31), C5(H5), C40(H40), C32(H32)
;
_shelx_res_checksum              23976
_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 1.932
_oxdiff_exptl_absorpt_empirical_full_min 0.579