A Crystalline Phosphinyl Radical Cation
Olivier Back; Mehmet Ali Celik; Gernot Frenking; Mohand Melaimi; Bruno Donnadieu; Guy Bertrand; Journal of the American Chemical Society 132 (2010) 10262–10263; doi:10.1021/ja1046846

data_4102776
_publ_contact_author             'Prof G. Bertrand'
_publ_contact_author_address
;
University of California
UCR-CNRS Joint Research Lab
(UMR 2282) 
Department of Chemistry
Riverside, CA 92521 USA 
;
_publ_contact_author_email       ' guy.bertrand@ucr.edu '
_publ_contact_author_fax         951-827-4713
_publ_section_title
;
 A Crystalline Phosphinyl Radical Cation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10262
_journal_page_last               10263
_journal_paper_doi               10.1021/ja1046846
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C56 H53 B Cl0.06 F20 N2 P'
_chemical_formula_sum            'C56 H53 B Cl0.06 F20 N2 P'
_chemical_formula_weight         1177.91
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.283(2)
_cell_angle_beta                 91.586(2)
_cell_angle_gamma                100.116(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4126(13)
_cell_length_b                   13.1288(15)
_cell_length_c                   18.984(2)
_cell_measurement_reflns_used    5747
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.80
_cell_measurement_theta_min      4.77
_cell_volume                     2631.9(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Ortep3
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir 97'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.883
_diffrn_measured_fraction_theta_max 0.883
_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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24760
_diffrn_reflns_theta_full        33.51
_diffrn_reflns_theta_max         33.51
_diffrn_reflns_theta_min         4.30
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  0.9983
_exptl_absorpt_correction_T_min  0.9601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         18262
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.057
_refine_ls_shift/su_mean         0.036
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.6508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1502
_reflns_number_gt                11552
_reflns_number_total             19262
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1046846_si_001.cif
_cod_data_source_block           2+^.^.
_cod_original_cell_volume        2631.8(5)
_cod_database_code               4102776