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_7718255
_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         'C37 H25 Au N O P, C0.5 H Cl, H O0.5'
_chemical_formula_sum            'C37.5 H27 Au Cl N O1.5 P'
_chemical_formula_weight         778.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-19
_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                90
_cell_angle_beta                 107.8800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.4494(2)
_cell_length_b                   10.04070(10)
_cell_length_c                   28.6890(3)
_cell_measurement_reflns_used    14126
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.0180
_cell_measurement_theta_min      1.6680
_cell_volume                     6154.39(11)
_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 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     73.00  99.00   0.50    0.20    --   35.49  53.00 -79.00   52
  2  \w    -27.00   9.00   0.50    0.20    --   35.49 -53.00 135.00   72
  3  \w     20.00  51.00   0.50    0.20    --   35.49 -53.00 135.00   62
  4  \w     27.00  57.00   0.50    0.20    --   35.49  53.00 -79.00   60
  5  \w     33.00 122.00   0.50    0.30    --  100.00 -53.00 135.00  178
  6  \w     85.00 154.00   0.50    0.30    --  100.00  53.00 -79.00  138
  7  \w   -103.00 -70.00   0.50    0.20    --  -35.49 -53.00 135.00   66
  8  \w    -34.00   9.00   0.50    0.20    --  -35.49  65.00   0.00   86
  9  \w   -102.00 -77.00   0.50    0.20    --  -35.49 -43.00 120.00   50
 10  \w    -59.00 -14.00   0.50    0.20    --  -35.49 -43.00 120.00   90
 11  \w   -109.00  -6.00   0.50    0.20    --  -35.49 -21.00 150.00  206
 12  \w    -30.00  -5.00   0.50    0.20    --  -35.49  53.00 -79.00   50
 13  \w    -30.00   3.00   0.50    0.20    --   35.49 -32.00 -60.00   66
 14  \w     10.00  53.00   0.50    0.20    --   35.49 -32.00 -60.00   86
 15  \w     38.00  81.00   0.50    0.20    --   35.49  21.00  90.00   86
 16  \w     19.00 104.00   0.50    0.20    --   35.49  32.00 -90.00  170
 17  \w      4.00  67.00   0.50    0.20    --   35.49-104.00   0.00  126
 18  \w     61.00  86.00   0.50    0.20    --   35.49-138.00-150.00   50
 19  \w     86.00 111.00   0.50    0.20    --   35.49  21.00  90.00   50
 20  \w     74.00 156.00   0.50    0.30    --  100.00  69.00 -30.00  164
 21  \w     26.00  52.00   0.50    0.30    --  100.00 -22.00 120.00   52
 22  \w    109.00 134.00   0.50    0.30    --  100.00  45.00-120.00   50
 23  \w    101.00 134.00   0.50    0.30    --  100.00 107.00 -90.00   66
 24  \w     77.00 147.00   0.50    0.30    --  100.00  53.00 -60.00  140
 25  \w     81.00 106.00   0.50    0.30    --  100.00  45.00-120.00   50
 26  \w     22.00  71.00   0.50    0.30    --  100.00 -91.00 -30.00   98
 27  \w     31.00  94.00   0.50    0.30    --  100.00-125.00 120.00  126
 28  \w     39.00  98.00   0.50    0.30    --  100.00-125.00  60.00  118
 29  \w     77.00 106.00   0.50    0.30    --  100.00  61.00 150.00   58
 30  \w     73.00 114.00   0.50    0.30    --  100.00  22.00  60.00   82
 31  \w    112.00 157.00   0.50    0.30    --  100.00  37.00-150.00   90
 32  \w     95.00 144.00   0.50    0.30    --  100.00  15.00  30.00   98
 33  \w     33.00  82.00   0.50    0.30    --  100.00 -30.00 150.00   98
 34  \w     86.00 155.00   0.50    0.30    --  100.00 107.00-150.00  138
 35  \w     84.00 128.00   0.50    0.30    --  100.00 -22.00 120.00   88
 36  \w     35.00  60.00   0.50    0.30    --  100.00 -61.00 -90.00   50
 37  \w     83.00 122.00   0.50    0.30    --  100.00  91.00  30.00   78
 38  \w     88.00 124.00   0.50    0.30    --  100.00 -61.00 -90.00   72
 39  \w     88.00 114.00   0.50    0.30    --  100.00  37.00  60.00   52
 40  \w     93.00 118.00   0.50    0.30    --  100.00 107.00-120.00   50
 41  \w     67.00 125.00   0.50    0.30    --  100.00 -61.00  30.00  116
 42  \w     62.00  91.00   0.50    0.30    --  100.00  15.00  30.00   58
;
_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      -0.0297489000
_diffrn_orient_matrix_UB_12      -0.0869707000
_diffrn_orient_matrix_UB_13      -0.0454563000
_diffrn_orient_matrix_UB_21      0.0655763000
_diffrn_orient_matrix_UB_22      -0.0460764000
_diffrn_orient_matrix_UB_23      0.0003218000
_diffrn_orient_matrix_UB_31      -0.0036534000
_diffrn_orient_matrix_UB_32      -0.1176677000
_diffrn_orient_matrix_UB_33      0.0334623000
_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  0.0380
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            16229
_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         3.237
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.534
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80625
_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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_description       prism
_exptl_crystal_F_000             3056
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.720
_refine_diff_density_min         -1.330
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         5522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+16.8641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5454
_reflns_number_total             5522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03250k3.cif
_cod_data_source_block           0ver0-23685_mel1801n1p
_cod_original_formula_sum        'C37.50 H27 Au Cl N O1.50 P'
_cod_database_code               7718255
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C37 H25 Au N O P'
_shelx_estimated_absorpt_t_max   0.284
_shelx_estimated_absorpt_t_min   0.187
_reflns_odcompleteness_completeness 89.31
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     75.12
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H1WB(0.1) H1WA(0.9) H1SA(0.5) H1SB(0.5)
3.a Free rotating group:
 O1W(H1WB,H1WA)
3.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
3.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C25(H25), C27(H27), C9(H9), C24(H24), C22(H22), C13(H13), C10(H10),
 C8(H8), C15(H15), C4(H4), C29(H29), C2(H2), C37(H37), C33(H33), C16(H16),
 C3(H3), C5(H5), C14(H14), C36(H36), C28(H28), C30(H30), C31(H31), C34(H34),
 C35(H35)
;
_shelx_res_checksum              84619
_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 1.220
_oxdiff_exptl_absorpt_empirical_full_min 0.775