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_7718259
_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         'C43 H29 Au N O P, C2 H3 N'
_chemical_formula_sum            'C45 H32 Au N2 O P'
_chemical_formula_weight         844.66
_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             2023-10-19
_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                97.520(3)
_cell_angle_beta                 109.673(3)
_cell_angle_gamma                103.850(3)
_cell_formula_units_Z            2
_cell_length_a                   10.8168(4)
_cell_length_b                   11.9335(4)
_cell_length_c                   14.7148(5)
_cell_measurement_reflns_used    14202
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.2440
_cell_measurement_theta_min      3.8730
_cell_volume                     1689.46(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.95a (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                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3829
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_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     23.00  50.00   1.00   50.00    --  -16.94  19.00 120.00   27
  2  \w   -100.00 -65.00   1.00   50.00    --  -16.94 178.00   0.00   35
  3  \w    -40.00  16.00   1.00   50.00    --  -16.94 -77.00 150.00   56
  4  \w   -105.00 -71.00   1.00   50.00    --  -16.94-178.00-180.00   34
  5  \w    -42.00   4.00   1.00   50.00    --  -16.94 -77.00   0.00   46
  6  \w    -91.00 -66.00   1.00   50.00    --  -16.94 178.00-120.00   25
  7  \w    -37.00 -11.00   1.00   50.00    --   18.97 -38.00-180.00   26
  8  \w      5.00  31.00   1.00   50.00    --   18.97 -38.00-180.00   26
  9  \w    -69.00 102.00   1.00   50.00    --   18.97   0.00  30.00  171
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0718898000
_diffrn_orient_matrix_UB_12      0.0219718000
_diffrn_orient_matrix_UB_13      0.0284341000
_diffrn_orient_matrix_UB_21      -0.0049649000
_diffrn_orient_matrix_UB_22      0.0583155000
_diffrn_orient_matrix_UB_23      0.0088942000
_diffrn_orient_matrix_UB_31      -0.0122165000
_diffrn_orient_matrix_UB_32      -0.0087052000
_diffrn_orient_matrix_UB_33      0.0433733000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16342
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         3.019
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.442
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.95a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       prism
_exptl_crystal_F_000             836
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0175
_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^)+(0.0146P)^2^+0.7029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0390
_refine_ls_wR_factor_ref         0.0399
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6233
_reflns_number_total             6587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03250k3.cif
_cod_data_source_block           0ver0-24646_mel224_1n2p
_cod_original_cell_volume        1689.46(11)
_cod_database_code               7718259
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C43 H29 Au N O P'
_shelx_estimated_absorpt_t_max   0.718
_shelx_estimated_absorpt_t_min   0.470
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C24(H24), C25(H25), C13(H13), C30(H30), C33(H33), C10(H10), C2(H2),
 C39(H39), C31(H31), C22(H22), C27(H27), C34(H34), C15(H15), C28(H28), C21(H21),
  C37(H37), C40(H40), C42(H42), C9(H9), C35(H35), C41(H41), C8(H8), C5(H5),
 C14(H14), C43(H43), C36(H36), C3(H3), C4(H4)
2.b Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC)
;
_shelx_res_checksum              25041
_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 1.318
_oxdiff_exptl_absorpt_empirical_full_min 0.792