N-Arylpyridiniophosphines: Synthesis, Structure, and Applications in Au(I) Catalysis
Tinnermann, Hendrik; Nicholls, Leo D. M.; Johannsen, Tim; Wille, Christian; Golz, Christopher; Goddard, Richard; Alcarazo, Manuel; ACS Catalysis 8 (2018) 10457–; doi:10.1021/acscatal.8b03271

data_4515746
_publ_section_title
;
 N-Arylpyridiniophosphines: Synthesis, Structure, and Applications in
 Au(I) Catalysis
;
_journal_issue                   11
_journal_name_full               'ACS Catalysis'
_journal_page_first              10457
_journal_paper_doi               10.1021/acscatal.8b03271
_journal_volume                  8
_journal_year                    2018
_chemical_compound_source        acetonitrile
_chemical_formula_moiety         'C30 H21 Au Cl F12 N P, F6 Sb, C2 H3 N'
_chemical_formula_sum            'C32 H24 Au Cl F18 N2 P Sb'
_chemical_formula_weight         1163.67
_chemical_name_systematic
;
 N-(2,4,6-trimethyl-phenyl)-2-di-(3,5-ditrifluoromethylphenyl)-
 phosphinylchlorogold(i)-pyridinium hexafluoroantimonate acetonitrile
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                TIH-TB-354_8893_100_K
_audit_creation_date             2018-08-15
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 103.535(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7962(6)
_cell_length_b                   27.1915(18)
_cell_length_c                   16.0760(14)
_cell_measurement_reflns_used    118592
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.0997
_cell_measurement_theta_min      2.7051
_cell_volume                     3738.3(5)
_computing_cell_refinement       'REVALCCD V. 1.6, 2008'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'REVALCCD V. 1.6, 2008'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 1997-2013)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios focusing multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            111778
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.184
_diffrn_reflns_theta_min         2.712
_diffrn_source                   '0.2 x 2mm^2^ focus rotating anode'
_exptl_absorpt_coefficient_mu    4.875
_exptl_absorpt_correction_T_max  0.76040
_exptl_absorpt_correction_T_min  0.44907
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.068
_exptl_crystal_description       plate
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.189
_refine_diff_density_min         -1.863
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         14268
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+5.4843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12884
_reflns_number_total             14268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b03271_si_009.cif
_cod_data_source_block           14
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4515746
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.414
_shelx_estimated_absorpt_t_max   0.759
_shelx_res_checksum              54751
_shelx_hkl_checksum              22018