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_4112239
_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            'C12 H20 I P'
_chemical_formula_weight         322.15
_chemical_name_common            '[CyPVi3]+I-'
_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                 90.2530(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.10980(10)
_cell_length_b                   24.8571(6)
_cell_length_c                   8.1218(2)
_cell_measurement_reflns_used    35444
_cell_measurement_temperature    143(2)
_cell_volume                     1435.34(5)
_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 0.950
_diffrn_measured_fraction_theta_max 0.950
_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  0.044
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            35444
_diffrn_reflns_theta_full        26.15
_diffrn_reflns_theta_max         26.15
_diffrn_reflns_theta_min         3.28
_exptl_absorpt_coefficient_mu    2.310
_exptl_absorpt_correction_T_max  0.815
_exptl_absorpt_correction_T_min  0.441
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Platon Delabs
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       plate
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         2720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0162P)^2^+1.4398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0597
_reflns_number_gt                2480
_reflns_number_total             2720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0399019si20031202_101949.cif
_cod_data_source_block           uwe29
_cod_database_code               4112239