Air- and water-stable Lewis acids: synthesis and reactivity of P-trifluoromethyl electrophilic phosphonium cations.
Fasano, V.; LaFortune, J. H. W.; Bayne, J. M.; Ingleson, M. J.; Stephan, D. W.; Chemical communications (Cambridge, England) 54 (2018) 662–665; doi:10.1039/c7cc09128a

data_7121036
_publ_section_title
;
 Air- and water-stable Lewis acids: synthesis and reactivity of
 P-trifluoromethyl electrophilic phosphonium cations.
;
_journal_issue                   6
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              662
_journal_page_last               665
_journal_paper_doi               10.1039/c7cc09128a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C19 H15 F3 P, C F3 O3 S'
_chemical_formula_sum            'C20 H15 F6 O3 P S'
_chemical_formula_weight         480.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
2017-11-17 deposited with the CCDC.
2017-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.9081(6)
_cell_length_b                   8.3531(2)
_cell_length_c                   22.4426(7)
_cell_measurement_reflns_used    13297
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.3880
_cell_measurement_theta_min      2.7820
_cell_volume                     4107.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     60.77 246.77   1.20    8.00    --   90.16  73.87-103.01  155
  2  \w     82.70 268.70   1.20    8.00    --  112.08  73.87  26.22  155
  3  \w   -108.25  77.76   1.20    8.00    --  -78.86  73.87 -60.62  155
  4  \f      6.61 156.69   1.20    8.00 -11.66  18.13  73.87    --   125
  5  \w    -83.92 102.08   1.20    8.00    --  -54.53  73.87  51.70  155
  6  \f    -41.99 205.34   1.20    8.00  73.16 102.95  73.87    --   206
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0210234000
_diffrn_orient_matrix_UB_12      0.0331739000
_diffrn_orient_matrix_UB_13      -0.0643538000
_diffrn_orient_matrix_UB_21      0.0664765000
_diffrn_orient_matrix_UB_22      0.0140396000
_diffrn_orient_matrix_UB_23      0.0217525000
_diffrn_orient_matrix_UB_31      0.0090260000
_diffrn_orient_matrix_UB_32      -0.1808226000
_diffrn_orient_matrix_UB_33      -0.0101347000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17128
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.265
_diffrn_reflns_theta_min         3.939
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.836
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0784P)^2^+1.9697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1219
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3618
_reflns_number_total             3836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09128a2.cif
_cod_data_source_block           xmji84
_cod_depositor_comments
'Adding full bibliography for 7121036--7121038.cif.'
_cod_database_code               7121036
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C20 H15 P1 O3 S1 F6'
_reflns_odcompleteness_completeness 91.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.10
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00H(H00H), C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L),
 C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R),
 C00S(H00S), C00T(H00T), C00V(H00V)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.634
_oxdiff_exptl_absorpt_empirical_full_min 0.480