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_4132075
_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         'C14 H9 Au F2 I N2 S, C2 F6 N O4 S2'
_chemical_formula_sum            'C16 H9 Au F8 I N3 O4 S3'
_chemical_formula_weight         879.31
_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     direct
_audit_creation_date             2017-06-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.4823(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6761(3)
_cell_length_b                   10.1045(2)
_cell_length_c                   16.7196(3)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.49
_cell_volume                     2351.54(8)
_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      100.02
_diffrn_detector                 'Bruker area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0409
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            52232
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.110
_diffrn_reflns_theta_min         2.390
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.930
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0843 before and 0.0492 after correction. The Ratio of minimum to maximum transmission is 0.6993. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.484
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_recrystallization_method
'Crystallised from a dichloromethane solution layered with hexane at -20 degreesC.'
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.084
_refine_diff_density_max         1.833
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         6907
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0208
_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^)+(0.0147P)^2^+4.1355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0435
_refine_ls_wR_factor_ref         0.0451
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6096
_reflns_number_total             6907
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01411_si_008.cif
_cod_data_source_block           test1
_cod_database_code               4132075
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 S2-C15 \\sim S2A-C15A
 with sigma of 0.01
 S2-N3 \\sim S2A-N3
 with sigma of 0.01
 F3-F4 \\sim F3A-F4A \\sim F4-F5 \\sim F4A-F5A \\sim F5-F3 \\sim F5A-F3A
 with sigma of 0.01
 S2-O1 \\sim S2A-O1A \\sim S2-O2 \\sim S2A-O2A
 with sigma of 0.01
 O1-O2 \\sim O1A-O2A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C15 \\sim C15A \\sim F3 \\sim F3A \\sim F4 \\sim F4A \\sim F5 \\sim F5A \\sim
O1 \\sim O1A \\sim O2 \\sim O2A \\sim S2 \\sim S2A: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(C15A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(O1A)=Sof(O2A)=Sof(S2A)=1-FVAR(1)
 Sof(C15)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(O1)=Sof(O2)=Sof(S2)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13), C14(H14)
;
_shelx_res_checksum              79910
_shelx_hkl_checksum              66948
_olex2_submission_special_instructions 'No special instructions were received'