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_4132074
_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         'C12 H10 Au F2 N2, C2 F6 N O4 S2'
_chemical_formula_sum            'C14 H10 Au F8 N3 O4 S2'
_chemical_formula_weight         697.34
_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     iterative
_audit_creation_date             2017-06-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.710(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1314(3)
_cell_length_b                   14.0057(6)
_cell_length_c                   17.5690(7)
_cell_measurement_reflns_used    9159
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.32
_cell_volume                     2000.71(14)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0304
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34892
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.599
_diffrn_reflns_theta_min         1.860
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.664
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4063
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1258 before and 0.0425 after correction. The Ratio of minimum to maximum transmission is 0.5449. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.315
_exptl_crystal_description       needle
_exptl_crystal_F_000             1320
_exptl_crystal_recrystallization_method
'obtained from layering a dichloromethane solution with hexane'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.451
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4628
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0179
_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^)+(0.0216P)^2^+3.2045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0451
_refine_ls_wR_factor_ref         0.0462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4271
_reflns_number_total             4628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01411_si_002.cif
_cod_data_source_block           mh801_0m
_cod_database_code               4132074
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.515
_shelx_estimated_absorpt_t_min   0.207
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F3A-F4A = F4A-F5A = F5A-F3A = F3B-F4B = F4B-F5B = F5B-F3B
 2.153 with sigma of 0.01
 S2-C13A \\sim S2-C13B
 with sigma of 0.01
 C13A-F3A \\sim C13B-F3B \\sim C13A-F4A \\sim C13B-F4B \\sim C13A-F5A \\sim
C13B-F5B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C13A \\sim F3A \\sim F4A \\sim F5A \\sim F3B \\sim F4B \\sim F5B \\sim C13B:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(C13B)=1-FVAR(1)
 Sof(C13A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10)
;
_shelx_res_checksum              16082
_shelx_hkl_checksum              94914
_olex2_exptl_crystal_mounting_method mounted
_olex2_submission_special_instructions 'No special instructions were received'