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_4105456
_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         'Cl8 Ga P '
_chemical_formula_sum            'Cl8 Ga P'
_chemical_formula_weight         384.32
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      57
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_audit_creation_date             2008-02-25
_audit_creation_method           'by CrystalStructure 3.8'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   6.1146(3)
_cell_length_b                   13.5142(10)
_cell_length_c                   13.7921(10)
_cell_measurement_reflns_used    5452
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      72.2
_cell_measurement_theta_min      3.6
_cell_volume                     1139.70(13)
_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 0.980
_diffrn_measured_fraction_theta_max 0.385
_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  0.030
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8903
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         72.2
_exptl_absorpt_coefficient_mu    4.361
_exptl_absorpt_correction_T_max  0.476
_exptl_absorpt_correction_T_min  0.274
_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    2.240
_exptl_crystal_description       needle
_exptl_crystal_F_000             728.00
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.97
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_number_parameters     52
_refine_ls_number_reflns         1397
_refine_ls_R_factor_gt           0.0338
_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)
    13.6747    -5.4480    9.5903
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0376
_reflns_number_gt                1397
_reflns_number_total             1656
_reflns_threshold_expression     F2^>2.0\s(F2^)
_cod_data_source_file            ja907693f_si_008.cif
_cod_data_source_block           '__Jan6'
_cod_original_formula_sum        'Cl8 Ga P '
_cod_database_code               4105456