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_4515752
_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        dichloromethane
_chemical_formula_moiety
'C29 H19 Au Cl F12 N O2 P, F6 Sb, 2.5(C H2 Cl2)'
_chemical_formula_sum            'C31.5 H24 Au Cl6 F18 N O2 P Sb'
_chemical_formula_weight         1352.90
_chemical_name_systematic
;
 N-(2,6-dimethoxy-phenyl)-2-di-(3,5-ditrifluoromethylphenyl)-
 phosphinylchlorogold(i)-pyridinium hexafluoroantimonate
 dichloromethane
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                TIH-TB-409_8975_100_K
_audit_creation_date             2018-08-15
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                73.397(2)
_cell_angle_beta                 82.399(2)
_cell_angle_gamma                85.849(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9106(12)
_cell_length_b                   12.9646(17)
_cell_length_c                   19.744(3)
_cell_measurement_reflns_used    9791
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.0026
_cell_measurement_theta_min      2.6616
_cell_volume                     2165.1(5)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2005-2013)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 1997-2012)'
_computing_structure_refinement  'SHELXL (G. M. Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            59997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         1.084
_diffrn_source                   1\mS
_exptl_absorpt_coefficient_mu    4.525
_exptl_absorpt_correction_T_max  0.63944
_exptl_absorpt_correction_T_min  0.19638
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.075
_exptl_crystal_description       prism
_exptl_crystal_F_000             1290
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.382
_refine_diff_density_min         -3.307
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         13208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+24.5786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1264
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12266
_reflns_number_total             13208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b03271_si_010.cif
_cod_data_source_block           17
_cod_original_formula_sum        'C31.50 H24 Au Cl6 F18 N O2 P Sb'
_cod_database_code               4515752
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.363
_shelx_estimated_absorpt_t_max   0.742
_shelx_res_checksum              85462
_shelx_hkl_checksum              34481