Simple synthetic access to [Au(IBiox)Cl] complexes
Martynova, Ekaterina A.; Zuccarello, Marco; kronenberg, domenic; Belis, Marek; Cavallo, Luigi; Baudoin, Olivier; Kwit, Marcin; Van Hecke, Kristof; Zhang, Ziyun; czapik, agnieszka; Nolan, Steven P.; Dalton Transactions  (2023) –; doi:10.1039/D3DT01357J

data_7713007
_publ_section_title
;
 Simple synthetic access to [Au(IBiox)Cl] complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01357J
_journal_year                    2023
_chemical_formula_moiety         'C17 H24 Au Cl N2 O2'
_chemical_formula_sum            'C17 H24 Au Cl N2 O2'
_chemical_formula_weight         520.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-03-31 deposited with the CCDC.	2023-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.9660(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.18045(11)
_cell_length_b                   11.01060(13)
_cell_length_c                   25.1159(4)
_cell_measurement_reflns_used    25475
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.0650
_cell_measurement_theta_min      2.4640
_cell_volume                     1708.91(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.86a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.86a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.86a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_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      3.00 103.00   1.00    2.50    --   14.00-126.00 127.00  100
  2  \w     13.00 114.00   1.00    2.50    --   14.00-143.00 -41.00  101
  3  \w   -151.00 -66.00   1.00    7.50    --  -36.11-143.00 -41.00   85
  4  \w   -150.00 -76.00   1.00    7.50    --  -36.11-126.00 127.00   74
  5  \w   -112.00  -3.00   1.00    7.50    --  -36.11 126.00-155.00  109
  6  \w      3.00 112.00   1.00    7.50    --   36.19-126.00 127.00  109
  7  \w     76.00 150.00   1.00    7.50    --   36.19 126.00-155.00   74
  8  \w     13.00 124.00   1.00    7.50    --   36.19-143.00 -41.00  111
  9  \w   -128.00 -82.00   1.00    2.50    --  -13.92 -99.00   0.00   46
 10  \w   -128.00 -82.00   1.00    2.50    --  -13.92 -99.00 150.00   46
 11  \w    -53.00  39.00   1.00    2.50    --   14.00  77.00  60.00   92
 12  \w    -53.00  39.00   1.00    2.50    --   14.00  77.00 120.00   92
 13  \w    -53.00  39.00   1.00    2.50    --   14.00  77.00 -60.00   92
 14  \w    -53.00  39.00   1.00    2.50    --   14.00  77.00-180.00   92
 15  \w    -53.00  39.00   1.00    2.50    --   14.00  77.00-150.00   92
 16  \w    -53.00  39.00   1.00    2.50    --   14.00  77.00 -30.00   92
 17  \w    -53.00  39.00   1.00    2.50    --   14.00  77.00  90.00   92
 18  \w   -153.00 -80.00   1.00    7.50    --  -36.11 -77.00   0.00   73
 19  \w   -153.00 -83.00   1.00    7.50    --  -36.11 -94.00  30.00   70
 20  \w   -153.00 -80.00   1.00    7.50    --  -36.11 -77.00 -90.00   73
 21  \w   -153.00 -80.00   1.00    7.50    --  -36.11 -77.00-150.00   73
 22  \w   -153.00 -80.00   1.00    7.50    --  -36.11 -77.00  60.00   73
 23  \w    -31.00  39.00   1.00    7.50    --   36.19  77.00-180.00   70
 24  \w    -43.00  11.00   1.00    7.50    --   36.19 111.00   0.00   54
 25  \w    -31.00  39.00   1.00    7.50    --   36.19  77.00 120.00   70
 26  \w    -31.00  39.00   1.00    7.50    --   36.19  77.00-120.00   70
 27  \w    -31.00  39.00   1.00    7.50    --   36.19  77.00   0.00   70
 28  \w    -31.00  39.00   1.00    7.50    --   36.19  77.00  60.00   70
 29  \w    -31.00  39.00   1.00    7.50    --   36.19  77.00 -90.00   70
 30  \w    -31.00  39.00   1.00    7.50    --   36.19  77.00 -30.00   70
 31  \w    -43.00  11.00   1.00    7.50    --   36.19 111.00 150.00   54
 32  \w    -43.00  11.00   1.00    7.50    --   36.19 111.00 -90.00   54
 33  \w    -31.00  39.00   1.00    7.50    --   36.19  77.00  30.00   70
 34  \w    -43.00  11.00   1.00    7.50    --   36.19 111.00 -30.00   54
 35  \w    -80.00 -35.00   1.00    7.50    --   36.19 178.00-180.00   45
 36  \w    -43.00  11.00   1.00    7.50    --   36.19 111.00-180.00   54
 37  \w    -31.00  39.00   1.00    7.50    --   36.19  77.00  90.00   70
 38  \w     80.00 129.00   1.00    2.50    --   14.00  77.00  60.00   49
 39  \w   -101.00 129.00   1.00    2.50    --   14.00 -19.00 -60.00  230
 40  \w   -101.00 129.00   1.00    2.50    --   14.00 -19.00  90.00  230
 41  \w   -101.00 129.00   1.00    2.50    --   14.00  37.00  60.00  230
 42  \w   -101.00 129.00   1.00    2.50    --   14.00 -19.00   0.00  230
 43  \w   -101.00 129.00   1.00    2.50    --   14.00  37.00-150.00  230
 44  \w     80.00 129.00   1.00    2.50    --   14.00  77.00 150.00   49
 45  \w     80.00 129.00   1.00    2.50    --   14.00  77.00   0.00   49
 46  \w   -153.00 -80.00   1.00    7.50    --  -36.11 -77.00-180.00   73
 47  \w   -149.00 -83.00   1.00    7.50    --  -36.11-111.00-150.00   66
 48  \w     80.00 152.00   1.00    7.50    --   36.19  77.00 -30.00   72
 49  \w     83.00 149.00   1.00    7.50    --   36.19 111.00 150.00   66
 50  \w    -79.00 152.00   1.00    7.50    --   36.19  30.00 -90.00  231
 51  \w    -41.00 152.00   1.00    7.50    --   36.19  61.00  60.00  193
 52  \w     83.00 149.00   1.00    7.50    --   36.19 111.00  90.00   66
 53  \w    -79.00 152.00   1.00    7.50    --   36.19  30.00  30.00  231
 54  \w     80.00 152.00   1.00    7.50    --   36.19  77.00 -60.00   72
 55  \w    -79.00 152.00   1.00    7.50    --   36.19  30.00-150.00  231
 56  \w     83.00 134.00   1.00    7.50    --   36.19 111.00 -60.00   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0262980000
_diffrn_orient_matrix_UB_12      -0.0077227000
_diffrn_orient_matrix_UB_13      0.0273898000
_diffrn_orient_matrix_UB_21      0.1073107000
_diffrn_orient_matrix_UB_22      -0.0159536000
_diffrn_orient_matrix_UB_23      -0.0067088000
_diffrn_orient_matrix_UB_31      0.0309849000
_diffrn_orient_matrix_UB_32      0.0619079000
_diffrn_orient_matrix_UB_33      0.0016903000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            7151
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.113
_diffrn_reflns_theta_min         2.433
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.776
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.86a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.024
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.037
_refine_diff_density_min         -1.473
_refine_diff_density_rms         0.181
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.049(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7151
_refine_ls_number_restraints     417
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0077P)^2^+34.5348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0861
_reflns_Friedel_coverage         0.874
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.955
_reflns_number_gt                7009
_reflns_number_total             7151
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01357j2.cif
_cod_data_source_block           new
_cod_database_code               7713007
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C17 H24 Au1 Cl1 N2 O2'
_shelx_estimated_absorpt_t_max   0.779
_shelx_estimated_absorpt_t_min   0.127
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8096(13)
 0.1904(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B),
  C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C30(H30A,
 H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B)
;
_shelx_res_checksum              34847
_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 3.694
_oxdiff_exptl_absorpt_empirical_full_min 0.457