Synthesis of substituted (N,C) and (N,C,C) Au(iii) complexes: the influence of sterics and electronics on cyclometalation reactions
Hylland, Knut T.; Schmidtke, Inga L.; Wragg, David S.; Nova, Ainara; Tilset, Mats; Dalton Transactions  (2022) –; doi:10.1039/D2DT00371F

data_7709705
_publ_section_title
;
 Synthesis of substituted (N,C) and (N,C,C) Au(iii) complexes: the
 influence of sterics and electronics on cyclometalation reactions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00371F
_journal_year                    2022
_chemical_formula_moiety         'C27 H6 Au F16 N O4'
_chemical_formula_sum            'C27 H6 Au F16 N O4'
_chemical_formula_weight         909.29
_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
_audit_creation_date             2021-12-21
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2021-12-21 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                86.998(4)
_cell_angle_beta                 82.480(3)
_cell_angle_gamma                73.200(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0544(3)
_cell_length_b                   12.1925(6)
_cell_length_c                   15.7587(7)
_cell_measurement_reflns_used    3832
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      50.638
_cell_measurement_theta_min      3.789
_cell_volume                     1468.59(11)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement
;
%$getVar(refinement_reference_short)%
;
_computing_structure_solution
;
%$getVar(solution_reference_short)%
;
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker Photon 100 area detector'
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f shutterless scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_Laue_measured_fraction_full 0.914
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7414
_diffrn_reflns_point_group_measured_fraction_full 0.914
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        50.416
_diffrn_reflns_theta_max         50.416
_diffrn_reflns_theta_min         2.829
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    10.716
_exptl_absorpt_correction_T_max  0.725
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1038 before and 0.0560 after correction.
 
For component 2:
 wR2(int) was 0.1055 before and 0.0544 after correction.
 The Ratio of minimum to maximum transmission is 0.71.

Final HKLF 4 output contains 12412 reflections, Rint = 0.0767
 (9567 with I > 3sig(I), Rint = 0.0683)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.056
_exptl_crystal_description       needle
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.699
_refine_diff_density_min         -0.968
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         7414
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0563P)^2^+13.0020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1434
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6056
_reflns_number_total             7414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00371f2.cif
_cod_data_source_block           il-134-cu_sq
_cod_database_code               7709705
_shelx_shelxl_version_number     2018/3
_publ_section_exptl
;
Any special experimental details
;
_shelx_estimated_absorpt_t_max   0.739
_shelx_estimated_absorpt_t_min   0.315
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.38286
 0.61714
2. Rigid body (RIGU) restrains
 N1, C1, C2, C3, C4, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C11(H11)
;
_shelx_res_checksum              39459
_shelx_hkl_checksum              52797
_shelx_fab_checksum              79654
_platon_squeeze_void_probe_radius 1.20
_olex2_date_sample_data_collection 2021-06-03
_olex2_date_sample_submission    2021-06-01
_olex2_exptl_crystal_mounting_method
'Frozen on a Mitegen cryoloop using Paretone oil.'
_olex2_submission_original_sample_id IL134
_olex2_submission_special_instructions 'No special instructions were received'