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_4515748
_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, pentane'
_chemical_formula_moiety         'C26 H37 Au Cl N P, F6 Sb'
_chemical_formula_sum            'C26 H37 Au Cl F6 N P Sb'
_chemical_formula_weight         862.70
_chemical_name_systematic
;
  N-(2,4,6-trimethyl-phenyl)-2-dicyclohexylphosphinylchlorogold(i)-
 pyridinium hexafluoroantimonate
;
_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-689-01_9727_150_K
_audit_creation_date             2018-08-14
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                82.428(8)
_cell_angle_beta                 84.084(5)
_cell_angle_gamma                87.346(9)
_cell_formula_units_Z            4
_cell_length_a                   10.6409(9)
_cell_length_b                   16.737(2)
_cell_length_c                   17.0626(14)
_cell_measurement_reflns_used    89097
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.0999
_cell_measurement_theta_min      2.6253
_cell_volume                     2994.6(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      150(2)
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            80573
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.149
_diffrn_reflns_theta_min         2.942
_exptl_absorpt_coefficient_mu    5.992
_exptl_absorpt_correction_T_max  0.7155
_exptl_absorpt_correction_T_min  0.3886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_description       needle
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.876
_refine_diff_density_min         -5.354
_refine_diff_density_rms         0.271
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         22772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0587
_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^)+(0.0771P)^2^+7.7497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1562
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16411
_reflns_number_total             22772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b03271_si_008.cif
_cod_data_source_block           13
_cod_original_cell_volume        2994.5(5)
_cod_database_code               4515748
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.586
_shelx_estimated_absorpt_t_max   0.890
_exptl_absorpt_special_details
' Additional spherical absorption correction with mu*r =  0.23 '
_shelx_res_checksum              53457
_shelx_hkl_checksum              16325