Tetragonal Phosphorus(V) Cations As Tunable and Robust Catalytic Lewis Acids
Gilhula, James Connor; Radosevich, Alexander; Chemical Science  (2019) –; doi:10.1039/C9SC02463H

data_1551497
_publ_section_title
;
 Tetragonal Phosphorus(V) Cations As Tunable and Robust Catalytic Lewis
 Acids
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02463H
_journal_year                    2019
_chemical_formula_sum            'C69 H11 B F41 N4 P'
_chemical_formula_weight         1716.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-03-21 deposited with the CCDC.    2019-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 127.241(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.0082(11)
_cell_length_b                   18.2410(9)
_cell_length_c                   18.4271(9)
_cell_measurement_reflns_used    9332
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.92
_cell_measurement_theta_min      2.23
_cell_volume                     6156.8(5)
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.4
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Photon2 CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            290451
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.420
_diffrn_reflns_theta_min         1.576
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Herbst-Irmer et al., 2015)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_description       plate
_exptl_crystal_F_000             3368
_exptl_crystal_size_max          0.429
_exptl_crystal_size_mid          0.426
_exptl_crystal_size_min          0.058
_exptl_transmission_factor_max   0.7471
_exptl_transmission_factor_min   0.6692
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 11332 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         30013
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0494P)^2^+2.0399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                25991
_reflns_number_total             30013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02463h2.cif
_cod_data_source_block           cg424
_cod_database_code               1551497
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.911
_shelx_estimated_absorpt_t_max   0.987
_exptl_absorpt_special_details
'Bruker D8 Venture Kappa DUO four-circle diffractometer, Bruker Photon2 CPAD.'
_shelx_res_checksum              50183