Insights into Alkene Activation by Gold: Nucleophile Activation with Base as a Trigger for Generation of Lewis Acidic Gold
Zhu, Yuyang; Zhou, Wentong; Petryna, Ellen M.; Rogers, Brock R.; Day, Cynthia S.; Jones, Amanda C.; ACS Catalysis  (2016) 7357–; doi:10.1021/acscatal.6b01674

data_4513967
_publ_section_title
;
 Insights into Alkene Activation by Gold: Nucleophile Activation with Base
 as a Trigger for Generation of Lewis Acidic Gold
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              7357
_journal_paper_doi               10.1021/acscatal.6b01674
_journal_year                    2016
_chemical_formula_sum            'C61.75 H82.75 Au3 B Cl5.25 F4 O P3'
_chemical_formula_weight         1797.76
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/11
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.4511(17)
_cell_length_b                   14.4307(9)
_cell_length_c                   18.9787(12)
_cell_measurement_reflns_used    9610
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      3.50
_cell_volume                     6970.4(8)
_computing_cell_refinement       'Bruker APEX2 v2014.11'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker APEX2 v2014.11'
_computing_molecular_graphics    'Bruker APEX2 v2014.11'
_computing_publication_material  'Bruker APEX2 v2014.11'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX CCD'
_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  0.0581
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            128264
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_reduction_process narrow-frame
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.043
_diffrn_reflns_theta_min         3.499
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    6.616
_exptl_absorpt_correction_T_max  0.2602
_exptl_absorpt_correction_T_min  0.1446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for scaling and absorption effects using the
 multi--scan technique (SADABS). The ratio of minimum
 to maximum apparent transmission was 0.556. The
 calculated minimum and maximum transmission
 coefficients (based on crystal size) are 0.212 and 0.458.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       block
_exptl_crystal_F_000             3494
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.140
_exptl_transmission_factor_max   0.2602
_exptl_transmission_factor_min   0.1446
_refine_diff_density_max         2.318
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.264(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         20372
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0478P)^2^+4.0868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.946
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                18354
_reflns_number_total             20372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs6b01674_si_002.cif
_cod_data_source_block           a37v_redo
_cod_database_code               4513967
_shelx_shelxl_version_number     2014/11
_shelx_estimated_absorpt_t_min   0.212
_shelx_estimated_absorpt_t_max   0.458
_computing.bruker_data_scaling   'SADABS V2014/5 (Bruker AXS)'
_shelx_res_checksum              21512
_shelx_hkl_checksum              51498