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_7709706
_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
'C43 H35 Au2 F6 N3 O10, 2(C H2 Cl2), C2 H F3 O2, C2 H0.026 F3 O2'
_chemical_formula_sum            'C49 H40.03 Au2 Cl4 F12 N3 O14'
_chemical_formula_weight         1658.60
_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   mixed
_audit_creation_date             2021-12-04
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2021-12-04 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                86.730(5)
_cell_angle_beta                 82.867(5)
_cell_angle_gamma                76.625(4)
_cell_formula_units_Z            2
_cell_length_a                   11.978(2)
_cell_length_b                   14.129(3)
_cell_length_c                   16.804(4)
_cell_measurement_reflns_used    9448
_cell_measurement_temperature    99.9
_cell_measurement_theta_max      22.10
_cell_measurement_theta_min      2.26
_cell_volume                     2744.1(10)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.9
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0801
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            47330
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        22.142
_diffrn_reflns_theta_max         22.142
_diffrn_reflns_theta_min         1.482
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    5.644
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.4100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1365 before and 0.0949 after correction.
The Ratio of minimum to maximum transmission is 0.5506.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.007
_exptl_crystal_description       plate
_exptl_crystal_F_000             1602
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.283
_refine_diff_density_min         -4.044
_refine_diff_density_rms         0.309
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.286
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         6777
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.287
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0905
_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^)+232.4826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2123
_refine_ls_wR_factor_ref         0.2330
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5268
_reflns_number_total             6777
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00371f2.cif
_cod_data_source_block           test_1ang_a
_cod_original_cell_volume        2744.0(10)
_cod_database_code               7709706
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.631
_shelx_estimated_absorpt_t_min   0.211
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All Cl(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O12-H12
 0.96 with sigma of 0.02
 O13-H14
 0.96 with sigma of 0.02
 C43-F3B \\sim C43-F3A \\sim C43-F2B \\sim C43-F2A \\sim C43-F1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2B \\sim F3B \\sim F2A \\sim F3A: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 1.7A
Uanis(O1) = Uanis(O2) = Uanis(O3) = Uanis(O4) = Uanis(O7) = Uanis(O8) =
Uanis(O10) = Uanis(O9) = Uanis(O5) = Uanis(O6) = Uanis(O11) = Uanis(O12) =
Uanis(O13) = Uanis(O14)
Uanis(N1) = Uanis(N2) = Uanis(N3)
Uanis(C42) = Uanis(C43) = Uanis(C14) = Uanis(C15) = Uanis(C45) = Uanis(C46) =
Uanis(C48)
Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C6) =
Uanis(C11) = Uanis(C10) = Uanis(C9) = Uanis(C8) = Uanis(C7) = Uanis(C12) =
Uanis(C13)
Uanis(C26) = Uanis(C25) = Uanis(C24) = Uanis(C23) = Uanis(C22) = Uanis(C21) =
Uanis(C16) = Uanis(C17) = Uanis(C18) = Uanis(C19) = Uanis(C20) = Uanis(C27) =
Uanis(C28)
Uanis(C29) = Uanis(C30) = Uanis(C31) = Uanis(C32) = Uanis(C33) = Uanis(C34) =
Uanis(C39) = Uanis(C38) = Uanis(C37) = Uanis(C36) = Uanis(C35) = Uanis(C41) =
Uanis(C40)
Uanis(F5) = Uanis(F1) = Uanis(F2A) = Uanis(F2B) = Uanis(F3A) = Uanis(F3B)
4. Rigid body (RIGU) restrains
 F1, F2B, F3B, F2A, F3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F2B)=Sof(F3B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C44(H9,H10), C49(H11,H13)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H), C2(HA), C3(HB), C4(HC), C9(HD), C11(HE), C18(HL), C23(HM), C24(HN),
 C25(HO), C26(HP), C29(HW), C30(HX), C31(HY), C32(HZ), C37(H1), C39(H2)
6.c Tetrahedral OH refined with riding coordinates:
 O13(H14)
6.d Idealised Me refined as rotating group:
 C12(HF,HG,HH), C13(HI,HJ,HK), C27(HQ,HR,HS), C28(HT,HU,HV), C40(H3,H4,H5),
 C41(H6,H7,H8)
;
_shelx_res_checksum              5549
_shelx_hkl_checksum              896
_olex2_date_sample_data_collection 2020-09-25
_olex2_date_sample_submission    2020-08-20
_olex2_exptl_crystal_mounting_method
'Frozen on a Mitegen cryoloop using Paretone oil.'
_olex2_submission_special_instructions 'No special instructions were received'