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_7709700
_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 H15 Au F3 N O2'
_chemical_formula_sum            'C17 H15 Au F3 N O2'
_chemical_formula_weight         519.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-10-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-10-06 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.368(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   26.1042(19)
_cell_length_b                   13.5893(10)
_cell_length_c                   19.3988(14)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      2.23
_cell_volume                     6363.7(8)
_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  0.0368
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            84078
_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         30.587
_diffrn_reflns_theta_min         2.231
_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    9.289
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0992 before and 0.0444 after correction.
The Ratio of minimum to maximum transmission is 0.8177.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.168
_exptl_crystal_description       block
_exptl_crystal_F_000             3936
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.127
_refine_diff_density_min         -1.163
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         19420
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          1.947
_refine_ls_shift/su_mean         0.146
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+46.6151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0633
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                13543
_reflns_number_total             19420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00371f2.cif
_cod_data_source_block           mo_il_63_tol_0m_b
_cod_database_code               7709700
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.336
_shelx_estimated_absorpt_t_min   0.234
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C01Y) = Uanis(C01P) = Uanis(C026) = Uanis(C01H) = Uanis(C02A) =
Uanis(C015) = Uanis(C027) = Uanis(C00N) = Uanis(C02T) = Uanis(C02H) =
Uanis(C024) = Uanis(C00H) = Uanis(C021) = Uanis(C01W) = Uanis(C02D) =
Uanis(C02R) = Uanis(C01M) = Uanis(C01B) = Uanis(C02M) = Uanis(C00Q) =
Uanis(C01X) = Uanis(C02C) = Uanis(C019) = Uanis(C02P) = Uanis(C02G) =
Uanis(C014) = Uanis(C00Y) = Uanis(C00S) = Uanis(C00I) = Uanis(C00R) =
Uanis(C01O) = Uanis(C00X) = Uanis(C01J) = Uanis(C01N) = Uanis(C01I) =
Uanis(C023) = Uanis(C013) = Uanis(C02I) = Uanis(C017) = Uanis(C01L) =
Uanis(C00M) = Uanis(C00O) = Uanis(C016) = Uanis(C02Q)
Uanis(C02B) = Uanis(C01Q) = Uanis(C00B) = Uanis(C029) = Uanis(C02J) =
Uanis(C02N) = Uanis(C02U) = Uanis(C02L)
Uanis(N01K) = Uanis(N00A) = Uanis(N00K) = Uanis(N00W)
Uanis(C01Z) = Uanis(C00T) = Uanis(C02F) = Uanis(C020) = Uanis(C00V) =
Uanis(C01D) = Uanis(C01U) = Uanis(C028)
Uanis(C3) = Uanis(C012) = Uanis(C00U) = Uanis(C025)
Uanis(C7) = Uanis(C01V) = Uanis(C02S) = Uanis(C01S)
Uanis(O2) = Uanis(O1) = Uanis(O00G) = Uanis(O00L) = Uanis(O007) = Uanis(O00J) =
Uanis(O00Z) = Uanis(O009)
3.a Secondary CH2 refined with riding coordinates:
 C00B(H00C,H00D), C00T(H00E,H00F), C00V(H00A,H00B), C01D(H01A,H01B), C01Q(H01C,
 H01D), C01U(H01G,H01K), C01Z(H01E,H01F), C020(H02D,H02E), C028(H02R,H02S),
 C02F(H02J,H02K), C02N(H02Z,H), C02U(H02O,H02Q)
3.b Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00M(H00M), C00Q(H00Q), C014(H014), C016(H016), C019(H019),
 C01H(H01H), C01I(H01I), C01J(H01J), C01N(H01N), C01O(H01O), C01P(H01P),
 C01W(H01W), C01X(H01X), C01Y(H01Y), C023(H023), C024(H024), C026(H026),
 C02C(H02U), C02G(H02G), C02M(H02Y), C02P(H02P), C02R(H02), C02T(H02T)
3.c Idealised Me refined as rotating group:
 C029(H02F,H02H,H02I), C02B(H02A,H02B,H02C), C02J(H02V,H02W,H02X), C02L(H02L,
 H02M,H02N)
;
_shelx_res_checksum              53450
_shelx_hkl_checksum              95378
_olex2_date_sample_data_collection 2021-08-24
_olex2_date_sample_submission    2021-08-22
_olex2_submission_special_instructions 'No special instructions were received'