Non-palindromic (C^C^D) gold(III) pincer complexes are not accessible by intramolecular oxidative addition of biphenylenes - an experimental and quantum chemical study.
Feuerstein, Wolfram; Breher, Frank; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9754–9767; doi:10.1039/d1dt00953b

data_7707638
_publ_section_title
;
 Non-palindromic (C^C^D) gold(III) pincer complexes are not accessible by
 intramolecular oxidative addition of biphenylenes - an experimental and
 quantum chemical study.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9754
_journal_page_last               9767
_journal_paper_doi               10.1039/d1dt00953b
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C34 H28 Au N4, C F3 O3 S'
_chemical_formula_sum            'C35 H28 Au F3 N4 O3 S'
_chemical_formula_weight         838.64
_chemical_name_systematic        WF067
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-07-22 deposited with the CCDC.	2021-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0660(16)
_cell_length_b                   19.896(4)
_cell_length_c                   20.237(4)
_cell_measurement_reflns_used    64616
_cell_measurement_temperature    200
_cell_measurement_theta_max      29.4
_cell_measurement_theta_min      1.5
_cell_volume                     3247.7(11)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            59026
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         1.435
_exptl_absorpt_coefficient_mu    4.653
_exptl_absorpt_correction_T_max  0.6038
_exptl_absorpt_correction_T_min  0.3852
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'Stoe & Cie, X-RED, version 1.28b: Program for data reduction and absorptioncorrection, Stoe &CieGmbH, Darmatadt, Germany, 2005.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       needle
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.650
_refine_diff_density_min         -1.476
_refine_diff_density_rms         0.140
_refine_ls_abs_structure_details
;
 Flack x determined using 2800 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.027(2)
_refine_ls_extinction_coef       0.0044(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         8060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+7.2063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1105
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7179
_reflns_number_total             8060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00953b2.cif
_cod_data_source_block           hw_a_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7707636--7707640.cif.'
_cod_database_code               7707638
_shelx_shelxl_version_number     2017/1
_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.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C209(H209), C103(H103), C12(H12), C22(H22), C102(H102), C11(H11), C203(H203),
 C106(H106), C208(H208), C201(H201), C107(H107), C206(H206), C207(H207),
 C109(H109), C21(H21), C108(H108), C101(H101), C202(H202)
2.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              3509
_shelx_hkl_checksum              16139
_olex2_exptl_crystal_mounting_method 'glas needle'
_olex2_submission_special_instructions 'No special instructions were received'