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_7709695
_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         'C17 H12 Au F6 N O4'
_chemical_formula_sum            'C17 H12 Au F6 N O4'
_chemical_formula_weight         605.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-27 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.225(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.349(3)
_cell_length_b                   19.446(5)
_cell_length_c                   9.020(3)
_cell_measurement_reflns_used    9826
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.29
_cell_volume                     1759.6(9)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            46733
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.560
_diffrn_reflns_theta_min         2.284
_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
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.448
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1203 before and 0.0499 after correction.
The Ratio of minimum to maximum transmission is 0.5557.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.285
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.977
_refine_diff_density_min         -1.447
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         5374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0178
_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^)+(0.0105P)^2^+2.6848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0393
_refine_ls_wR_factor_ref         0.0398
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5081
_reflns_number_total             5374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00371f2.cif
_cod_data_source_block           mo_il_dimethyl_0m_a
_cod_database_code               7709695
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.201
_shelx_estimated_absorpt_t_min   0.096
_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:
 C11(H11), C5(H5), C8(H8), C10(H10), C9(H9), C3(H3)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              60577
_shelx_hkl_checksum              64714
_olex2_date_sample_data_collection 2021-05-25
_olex2_date_sample_submission    2021-04-29
_olex2_exptl_crystal_mounting_method
'Frozen on a Mitegen cryoloop using Paretone oil.'
_olex2_submission_special_instructions 'No special instructions were received'