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_7713006
_publ_section_title
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 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         'C11 H16 Au Cl N2 O2'
_chemical_formula_sum            'C11 H16 Au Cl N2 O2'
_chemical_formula_weight         440.68
_chemical_name_systematic        EM329
_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             2022-02-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-01-26 deposited with the CCDC.	2023-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                67.245(4)
_cell_angle_beta                 67.968(4)
_cell_angle_gamma                88.758(3)
_cell_formula_units_Z            2
_cell_length_a                   8.9640(4)
_cell_length_b                   9.0310(3)
_cell_length_c                   9.5445(4)
_cell_measurement_reflns_used    9606
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.9990
_cell_measurement_theta_min      3.1940
_cell_volume                     653.57(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.915
_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    -25.00  21.00   1.00    1.00    --    7.76  77.00 -90.00   46
  2  \w    -25.00  21.00   1.00    1.00    --    7.76  77.00   0.00   46
  3  \w    -17.00  82.00   1.00    1.00    --    7.76  38.00 -90.00   99
  4  \w    -83.00  16.00   1.00    1.00    --   -8.62 -38.00  60.00   99
  5  \w    -67.00  32.00   1.00    1.00    --    7.76 -38.00 150.00   99
  6  \w    -15.00  49.00   1.00    1.00    --    7.76 -99.00  90.00   64
  7  \w    -41.00  21.00   1.00    1.00    --   -8.62  77.00 -30.00   62
  8  \w    -15.00  10.00   1.00    1.00    --   -8.62-101.00 -20.00   25
  9  \w    -41.00  21.00   1.00    1.00    --   -8.62  77.00-120.00   62
 10  \w    -11.00  15.00   1.00    1.00    --   -8.77  77.00-180.00   26
 11  \w    -25.00  21.00   1.00    1.00    --    7.83  77.00 120.00   46
 12  \w    -41.00 -10.00   1.00    1.00    --   -8.77  77.00 150.00   31
 13  \w    -64.00  36.00   1.00    1.00    --    7.83 -57.00 120.00  100
 14  \w    -25.00  21.00   1.00    1.00    --    7.83  77.00  60.00   46
 15  \w    -15.00  49.00   1.00    1.00    --    7.83-100.00 -20.00   64
 16  \w    -15.00  49.00   1.00    1.00    --    7.83 -99.00-120.00   64
;
_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      0.0703494000
_diffrn_orient_matrix_UB_12      -0.0205190000
_diffrn_orient_matrix_UB_13      -0.0509467000
_diffrn_orient_matrix_UB_21      -0.0265850000
_diffrn_orient_matrix_UB_22      -0.0832846000
_diffrn_orient_matrix_UB_23      0.0537016000
_diffrn_orient_matrix_UB_31      -0.0422596000
_diffrn_orient_matrix_UB_32      -0.0071360000
_diffrn_orient_matrix_UB_33      -0.0472846000
_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  0.0680
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17973
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.728
_diffrn_reflns_theta_min         2.472
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.451
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.503
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    2.239
_exptl_crystal_description       irregular
_exptl_crystal_F_000             416
_exptl_crystal_preparation       Synthesis
_exptl_crystal_recrystallization_method 'Pentane diffusion in DCM'
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.157
_refine_diff_density_max         3.179
_refine_diff_density_min         -2.728
_refine_diff_density_rms         0.265
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.216
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         3083
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.215
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0091P)^2^+11.7268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2823
_reflns_number_total             3083
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01357j2.cif
_cod_data_source_block           em329
_cod_database_code               7713006
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H16 Au Cl N2 O2'
_shelx_estimated_absorpt_t_max   0.267
_shelx_estimated_absorpt_t_min   0.191
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9680(9)
 0.0320(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C6(H6A,H6B)
4.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              23866
_olex2_date_sample_data_collection 2022-02-11
_olex2_exptl_crystal_mounting_method 'Litho loop'
_olex2_submission_original_sample_id EM329
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.330
_oxdiff_exptl_absorpt_empirical_full_min 0.677