Synthesis and Oxidation of Phosphine Cations†
Mehta, Meera; Johnstone, Tim; Lam, Jolie; Bidraha, Bid; Hermannsdorfer, Andre; Driess, Matthias; Stephan, Douglas W.; Dalton Trans.  (2017) –; doi:10.1039/C7DT03175K

data_7044347
_publ_section_title
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 Synthesis and Oxidation of Phosphine Cations&#x2020;
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03175K
_journal_year                    2017
_chemical_formula_sum            'C108.5 H65 B2 F47 N4 P'
_chemical_formula_weight         2370.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-09-26 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                83.610(2)
_cell_angle_beta                 89.0867(19)
_cell_angle_gamma                73.915(3)
_cell_formula_units_Z            2
_cell_length_a                   15.5736(4)
_cell_length_b                   17.4980(5)
_cell_length_c                   18.9275(4)
_cell_measurement_reflns_used    17804
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.5930
_cell_measurement_theta_min      2.9340
_cell_volume                     4924.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.5435
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34478
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.492
_diffrn_reflns_theta_max         67.492
_diffrn_reflns_theta_min         2.349
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.538
_exptl_absorpt_correction_T_max  0.8920
_exptl_absorpt_correction_T_min  0.4914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       needle
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.538
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     1687
_refine_ls_number_reflns         17749
_refine_ls_number_restraints     1255
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1237P)^2^+6.2063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1983
_refine_ls_wR_factor_ref         0.2143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14663
_reflns_number_total             17749
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03175k2.cif
_cod_data_source_block           4b
_cod_original_cell_volume        4924.5(2)
_cod_original_formula_sum        'C108.50 H65 B2 F47 N4 P'
_cod_database_code               7044347
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.492
_shelx_estimated_absorpt_t_max   0.892
_exptl_absorpt_special_details
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_shelx_res_checksum              4482