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_4105449
_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         'C24 H44 Cl5 Ga P4 '
_chemical_formula_sum            'C24 H44 Cl5 Ga P4'
_chemical_formula_weight         703.49
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             2008-02-25
_audit_creation_method           'by CrystalStructure 3.8'
_cell_angle_alpha                90.0000
_cell_angle_beta                 104.27(5)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   18.491(9)
_cell_length_b                   9.143(9)
_cell_length_c                   19.970(5)
_cell_measurement_reflns_used    4446
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      72.4
_cell_measurement_theta_min      3.1
_cell_volume                     3272(4)
_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 0.984
_diffrn_measured_fraction_theta_max 0.612
_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  0.115
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       22
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_diffrn_reflns_limit_l_max       42
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_diffrn_reflns_number            79803
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         72.77
_exptl_absorpt_coefficient_mu    1.458
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             1456.00
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.12
_refine_diff_density_min         -0.93
_refine_ls_extinction_coef       60(21)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    refall
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_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    14.7332    0.7557    11.9822
;
_refine_ls_weighting_scheme      calc
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_reflns_threshold_expression     F2^>2.0\s(F2^)
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_cod_data_source_block           '__Jan8mono'
_cod_original_cell_volume        3272(5)
_cod_original_formula_sum        'C24 H44 Cl5 Ga P4 '
_cod_database_code               4105449