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_4515749
_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        'dichloormethane, pentane'
_chemical_formula_moiety         'C26 H37 N P, F6 Sb'
_chemical_formula_sum            'C26 H37 F6 N P Sb'
_chemical_formula_weight         630.28
_chemical_name_systematic
;
 N-(2,4,6-trimethyl-phenyl)-2-dicyclohexylphosphinyl-pyridinium 
 hexafluoroantimonate
;
_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     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                WID-WA-100-02_9294_150_K
_audit_creation_date             2018-08-14
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 112.626(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8885(9)
_cell_length_b                   13.3919(6)
_cell_length_c                   15.6069(18)
_cell_measurement_reflns_used    61383
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.9997
_cell_measurement_theta_min      2.6534
_cell_volume                     2679.4(4)
_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 0.992
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            56140
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.059
_diffrn_reflns_theta_min         2.927
_diffrn_source                   '0.2 x 2mm^2^ focus rotating anode'
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_T_max  0.95096
_exptl_absorpt_correction_T_min  0.87548
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.198
_refine_diff_density_min         -1.755
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         11816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+2.5900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10182
_reflns_number_total             11816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b03271_si_003.cif
_cod_data_source_block           9ab
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4515749
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              25330
_shelx_hkl_checksum              84879