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_7044346
_publ_section_title
;
 Synthesis and Oxidation of Phosphine Cations&#x2020;
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03175K
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_sum            'C26 H30 F3 N2 O5 P S'
_chemical_formula_weight         570.55
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4215(11)
_cell_length_b                   10.4310(13)
_cell_length_c                   24.812(3)
_cell_measurement_reflns_used    8861
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     2697.2(5)
_computing_cell_refinement       'Bruker, APEX II'
_computing_data_collection       'Bruker, APEX II'
_computing_data_reduction        'Bruker, SAINT'
_computing_molecular_graphics    'ORTEP 3'
_computing_publication_material  'Bruker, SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            24768
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.608
_diffrn_reflns_theta_min         1.641
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       needle
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 2266 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(2)
_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     347
_refine_ls_number_reflns         6250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0351P)^2^+0.3046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0690
_reflns_Friedel_coverage         0.771
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                5640
_reflns_number_total             6250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03175k2.cif
_cod_data_source_block           1
_cod_original_cell_volume        2697.2(6)
_cod_database_code               7044346
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.894
_shelx_estimated_absorpt_t_max   0.981
_exptl_absorpt_special_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0633 before and 0.0430 after correction.
The Ratio of minimum to maximum transmission is 0.9474.
The \l/2 correction factor is 0.00150.
;
_shelx_res_checksum              43858