The Tetra(vinyl)phosphonium Cation [(CH2CH)4P]+
Uwe V. Monkowius; Stefan D. Nogai; Hubert Schmidbaur; Journal of the American Chemical Society 126 (2004) 1632–1633; doi:10.1021/ja0399019

data_4112241
_publ_contact_author_address
;
 Anorganische und Analytische Chemie 
 Technische Universitaet Muenchen 
 Lichtenbergstr. 4 
 Garching 
 D-85747 
 GERMANY 
;
_publ_contact_author_email       H.Schmidbaur@lrz.tu-muenchen.de
_publ_contact_author_fax         '++49 89 2891-3125'
_publ_contact_author_name        'Prof Hubert Schmidbaur'
_publ_contact_author_phone       '++49 89 2891-3130'
_publ_section_title
;
 The Tetra(vinyl)phosphonium Cation [(CH2CH)4P]+
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1632
_journal_page_last               1633
_journal_paper_doi               10.1021/ja0399019
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C27 H30 B P'
_chemical_formula_weight         396.29
_chemical_name_common            '[BVi4]-[MePPh3]+'
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.1099(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.31080(10)
_cell_length_b                   14.5850(2)
_cell_length_c                   15.6994(3)
_cell_measurement_reflns_used    53207
_cell_measurement_temperature    143(2)
_cell_volume                     2324.26(6)
_computing_cell_refinement       DENZO
_computing_data_collection       XPRESS
_computing_data_reduction        SCALEPACK
_computing_molecular_graphics    SHELXTL-PLUS
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'NONIUS DIP 2020'
_diffrn_measurement_method       phi-rotation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            53207
_diffrn_reflns_theta_full        25.45
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         4284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+1.3944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1031
_reflns_number_gt                3983
_reflns_number_total             4284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0399019si20031202_102037.cif
_cod_data_source_block           uwe41
_cod_database_code               4112241