New Synthetic Procedures to Catena-Phosphorus Cations: Preparation and Dissociation of the First cyclo-Phosphino-halophosphonium Salts
Jan J. Weigand; Neil Burford; Reagan J. Davidson; T. Stanley Cameron; Patrick Seelheim; Journal of the American Chemical Society 131 (2009) 17943–17953; doi:10.1021/ja907693f

data_4105453
_publ_contact_author_address
;
Institut fr Anorganische und Analytische Chemie
Corrensstrasse 30
WWU Mnster
D-48149 Mnster
Germany
;
_publ_contact_author_email       jweigand@uni-muenster.de
_publ_contact_author_fax         '+49 (251) 83-33108'
_publ_contact_author_name        'Jan J. Weigand'
_publ_contact_author_phone       '+49 (251) 83-36074 '
_publ_section_title
;
 New Synthetic Procedures to Catena-Phosphorus Cations: Preparation and
 Dissociation of the First cyclo-Phosphino-halophosphonium Salts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17943
_journal_page_last               17953
_journal_paper_doi               10.1021/ja907693f
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C6 H11 Cl7 Ga P '
_chemical_formula_sum            'C6 H11 Cl7 Ga P'
_chemical_formula_weight         432.02
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             2007-03-31
_audit_creation_method           'by CrystalStructure 3.8'
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.964(16)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   8.783(2)
_cell_length_b                   13.740(3)
_cell_length_c                   26.015(10)
_cell_measurement_reflns_used    6538
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      35.4
_cell_measurement_theta_min      4.7
_cell_volume                     3137.6(16)
_computing_cell_refinement       PROCESS
_computing_data_collection       PROCESS
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      123.1(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.717
_diffrn_measurement_device_type  'Rigaku RAXIS-UNKNOWN'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            17765
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         35.65
_exptl_absorpt_coefficient_mu    3.015
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_description       needle
_exptl_crystal_F_000             1696.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.22
_refine_diff_density_min         -0.78
_refine_ls_extinction_coef       99(15)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     294
_refine_ls_number_reflns         6005
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    17.4381    -10.4956    13.5316
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0427
_reflns_number_gt                6005
_reflns_number_total             7802
_reflns_threshold_expression     F2^>2.0\s(F2^)
_cod_data_source_file            ja907693f_si_005.cif
_cod_data_source_block           '__Jan9tetrab'
_cod_original_cell_volume        3137.4(15)
_cod_original_formula_sum        'C6 H11 Cl7 Ga P '
_cod_database_code               4105453