Lewis Acid Catalysis with Cationic Dinuclear Gold(II,II) and Gold(III,III) Phosphorus Ylide Complexes
Reiner, Benjamin R.; Bezpalko, Mark W.; Foxman, Bruce M.; Wade, Casey R.; Organometallics 35 (2016) 2830–; doi:10.1021/acs.organomet.6b00403

data_4086592
_publ_section_title
;
 Lewis Acid Catalysis with Cationic Dinuclear Gold(II,II) and
 Gold(III,III) Phosphorus Ylide Complexes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              2830
_journal_paper_doi               10.1021/acs.organomet.6b00403
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C35 H36 Au2 F6 N2 O6 P2 S2'
_chemical_formula_sum            'C35 H36 Au2 F6 N2 O6 P2 S2'
_chemical_formula_weight         1214.69
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2015-09-23
_audit_creation_method           CRYSTALS_ver_14.61_build_00000
_cell_angle_alpha                115.350(7)
_cell_angle_beta                 104.860(7)
_cell_angle_gamma                103.390(7)
_cell_formula_units_Z            4
_cell_length_a                   14.562(3)
_cell_length_b                   18.699(4)
_cell_length_c                   19.343(4)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.86
_cell_measurement_theta_min      2.24
_cell_volume                     4234.7(16)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27877
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         26.145
_diffrn_reflns_theta_min         1.268
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.164
_exptl_absorpt_correction_T_max  0.49
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       acicular
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.070
_platon_squeeze_details
;
It became apparent during the structure solution that 
the structure contained significant void volume (392.8 \%A3 
per unit cell (9.3%)).  Electron density difference maps did 
not reveal significant electron density in the void areas, 
and a ?test? PLATON SQUEEZE run suggested only a small improvement 
in R1 (0.0025).  It was decided not to process the data using 
SQUEEZE: the data quality and/or probable desolvation of the 
original acetonitrile solvate contributed to the inability to 
further model the contents of the void areas. 
;
_refine_diff_density_max         5.32
_refine_diff_density_min         -4.60
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9818
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     992
_refine_ls_number_reflns         27877
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.1244
_refine_ls_R_factor_gt           0.0825
_refine_ls_shift/su_max          0.0129241
_refine_ls_shift/su_mean         0.0017654
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.12P)^2^ +62.96P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2362
_refine_ls_wR_factor_gt          0.2078
_refine_ls_wR_factor_ref         0.2362
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              20
_reflns_limit_k_min              -23
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                18269
_reflns_number_total             20374
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.70
_oxford_diffrn_Wilson_scale      44.14
_oxford_refine_ls_r_factor_ref   0.1244
_oxford_refine_ls_scale          0.17609(10)
_oxford_reflns_number_all        27877
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'br3_70_0m in P-1'
_cod_data_source_file            om6b00403_si_002.cif
_cod_data_source_block           3_OTf
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4086591--4086592.cif.
;
_cod_original_cell_volume        4234.9(15)
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4086592
_platon_squeeze_void_probe_radius 1.20