Diphosphine-Phosphenium Coordination Complexes Representing Monocations with Pendant Donors and Ligand Tethered Dications
Neil Burford; David E. Herbert; Paul J. Ragogna; Robert McDonald; Michael J. Ferguson; Journal of the American Chemical Society 126 (2004) 17067–17073; doi:10.1021/ja0452121

data_4113342
_publ_contact_author_address
;Department of Chemistry
Dalhousie University
Halifax, NS
B3H 4J3, CANADA
;
_publ_contact_author_email       Neil.Burford@dal.ca
_publ_contact_author_fax         1-902-494-1310
_publ_contact_author_name        'Neil Burford'
_publ_contact_author_phone       1-902-4943190
_publ_section_title
;
 Diphosphine-Phosphenium Coordination Complexes Representing Monocations
 with Pendant Donors and Ligand Tethered Dications
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17067
_journal_page_last               17073
_journal_paper_doi               10.1021/ja0452121
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C27 H28 P3, C F3 O3 S'
_chemical_formula_sum            'C28 H28 F3 O3 P3 S'
_chemical_formula_weight         594.47
_chemical_melting_point          378
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.473(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3944(15)
_cell_length_b                   15.5061(17)
_cell_length_c                   15.1833(17)
_cell_measurement_reflns_used    3204
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.931
_cell_measurement_theta_min      2.627
_cell_volume                     2870.2(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_sigmaI/netI    0.0811
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13539
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.71
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  0.9774
_exptl_absorpt_correction_T_min  0.8638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1986)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       Block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0654
_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^)+(0.0956P)^2^+1.1936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1577
_refine_ls_wR_factor_ref         0.1800
_reflns_number_gt                3361
_reflns_number_total             5057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0452121si20041007_081423_1.cif
_cod_data_source_block           dal0351
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4113342