Oxidative Addition, Transmetalation, and Reductive Elimination at a 2,2'-Bipyridyl-Ligated Gold Center.
Harper, Matthew J.; Arthur, Christopher J.; Crosby, John; Emmett, Edward J.; Falconer, Rosalyn L.; Fensham-Smith, Andrew J; Gates, Paul J.; Leman, Thomas; McGrady, John E.; Bower, John F.; Russell, Christopher A.; Journal of the American Chemical Society 140 (2018) 4440–4445; doi:10.1021/jacs.8b01411

data_4132073
_publ_section_title
;
 Oxidative Addition, Transmetalation, and Reductive Elimination at a
 2,2'-Bipyridyl-Ligated Gold Center.
;
_journal_issue                   12
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4440
_journal_page_last               4445
_journal_paper_doi               10.1021/jacs.8b01411
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C22 H15 Au F2 I N2, C2 F6 N O4 S2, C7 H8'
_chemical_formula_sum            'C31 H23 Au F8 I N3 O4 S2'
_chemical_formula_weight         1041.51
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                92.573(2)
_cell_angle_beta                 102.927(2)
_cell_angle_gamma                95.368(2)
_cell_formula_units_Z            4
_cell_length_a                   9.7482(4)
_cell_length_b                   18.0342(6)
_cell_length_c                   20.0241(7)
_cell_measurement_reflns_used    6273
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      27.969
_cell_measurement_theta_min      2.274
_cell_volume                     3408.1(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      101.13
_diffrn_detector                 'Bruker area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_device_type  'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            57496
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.012
_diffrn_reflns_theta_min         1.137
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.430
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6032
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0690 before and 0.0445 after correction. The Ratio of minimum to maximum transmission is 0.8090. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.030
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.477
_exptl_crystal_size_mid          0.265
_exptl_crystal_size_min          0.249
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     975
_refine_ls_number_reflns         16334
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0184P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0453
_refine_ls_wR_factor_ref         0.0469
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14204
_reflns_number_total             16334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01411_si_007.cif
_cod_data_source_block           testt1
_cod_database_code               4132073
_shelxl_version_number           2013-4
_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. Restrained distances
 C52-C59B = C52B-C58B
 1.49 with sigma of 0.02
 C53-C59B = C57-C59B = C53B-C58B = C57B-C58B
 2.5 with sigma of 0.04
 F12-F13A = F13A-F11A = F11A-F12 = F12A-F13 = F13-F11 = F11-F12A
 2.158 with sigma of 0.01
 C59-F12 \\sim C1A-F12A \\sim C59-F13A \\sim C1A-F13 \\sim C59-F11A \\sim
C1A-F11
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C58B) \\sim Ueq, Uanis(C52B) \\sim Ueq, Uanis(C53B) \\sim Ueq,
Uanis(C57B) \\sim Ueq, Uanis(C54B) \\sim Ueq, Uanis(C56B) \\sim Ueq,
Uanis(C55B) \\sim Ueq, Uanis(C58B) \\sim Ueq, Uanis(C52B) \\sim Ueq,
Uanis(C53B) \\sim Ueq, Uanis(C52B) \\sim Ueq, Uanis(C57B) \\sim Ueq,
Uanis(C52B) \\sim Ueq, Uanis(C54B) \\sim Ueq, Uanis(C53B) \\sim Ueq,
Uanis(C57B) \\sim Ueq, Uanis(C56B) \\sim Ueq, Uanis(C55B) \\sim Ueq,
Uanis(C54B) \\sim Ueq, Uanis(C56B) \\sim Ueq, Uanis(C55B) \\sim Ueq,
Uanis(C59B) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C55) \\sim Ueq,
Uanis(C53) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C52)
\\sim Ueq, Uanis(C59B) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C54) \\sim Ueq,
Uanis(C53) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C55)
\\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C55) \\sim Ueq:
with sigma of 0.002 and sigma for terminal atoms of 0.005
Uanis(C59) = Uanis(C1A)
4. Others
 Sof(C58B)=Sof(H58A)=Sof(H58B)=Sof(H58C)=Sof(C52B)=Sof(C53B)=Sof(H53B)=
 Sof(C54B)=Sof(H54B)=Sof(C55B)=Sof(H55B)=Sof(C56B)=Sof(H56B)=Sof(C57B)=
 Sof(H57B)=1-FVAR(1)
 Sof(C52)=Sof(C53)=Sof(H53)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55)=Sof(C56)=
 Sof(H56)=Sof(C57)=Sof(H57)=Sof(C59B)=Sof(H59A)=Sof(H59B)=Sof(H59C)=FVAR(1)
 Sof(F11)=Sof(F13)=Sof(F12A)=Sof(C1A)=1-FVAR(2)
 Sof(F12)=Sof(C59)=Sof(F11A)=Sof(F13A)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C32(H32), C1(H1), C10(H10), C26(H26), C7(H7), C4(H4), C22(H22), C12(H12),
 C29(H29), C21(H21), C15(H15), C44(H44), C37(H37), C41(H41), C40(H40), C43(H43),
  C34(H34), C23(H23), C3(H3), C18(H18), C30(H30), C13(H13), C20(H20), C8(H8),
 C42(H42), C14(H14), C19(H19), C35(H35), C25(H25), C36(H36), C46(H46), C53(H53),
  C54(H54), C55(H55), C56(H56), C57(H57), C50(H50), C48(H48), C49(H49),
 C47(H47), C53B(H53B), C54B(H54B), C55B(H55B), C56B(H56B), C57B(H57B)
5.b Fitted hexagon refined as free rotating group:
 C52(C53,C54,C55,C56,C57), C52B(C53B,C54B,C55B,C56B,C57B)
5.c Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C59B(H59A,H59B,H59C), C58B(H58A,H58B,H58C)
;
_shelx_res_checksum              67402
_shelx_hkl_checksum              99907
_olex2_submission_special_instructions 'No special instructions were received'