Diphosphiranium (P2C) or Diphosphetanium (P2C2) Cyclic Cations: Different Fates for the Electrophile-Initiated Cyclodimerization of a Phosphaalkene
Joshua I. Bates; Derek P. Gates; Journal of the American Chemical Society 128 (2006) 15998–15999; doi:10.1021/ja0667662

data_4111224
_publ_section_title
;
 Diphosphiranium (P2C) or Diphosphetanium (P2C2) Cyclic Cations: Different
 Fates for the Electrophile-Initiated Cyclodimerization of a Phosphaalkene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15998
_journal_page_last               15999
_journal_paper_doi               10.1021/ja0667662
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C18 H39 P2, C F3 O3 S'
_chemical_formula_sum            'C19 H39 F3 O3 P2 S'
_chemical_formula_weight         466.50
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.656(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6083(3)
_cell_length_b                   21.4647(8)
_cell_length_c                   13.8064(5)
_cell_measurement_reflns_used    5200
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.83
_cell_measurement_theta_min      3.02
_cell_volume                     2489.09(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker X8 APEX'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31780
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.874
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.6379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                4777
_reflns_number_total             5915
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0667662si20061031_012124.cif
_cod_data_source_block           dg035_0m
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4111224