Isolation of crystalline carbene-stabilized P(2)-radical cations and P(2)-dications.
Back, Olivier; Donnadieu, Bruno; Parameswaran, Pattiyil; Frenking, Gernot; Bertrand, Guy; Nature chemistry 2 (2010) 369–373; doi:10.1038/nchem.617

data_1508029
_publ_section_title
;
 Isolation of crystalline carbene-stabilized P(2)-radical cations and
 P(2)-dications.
;
_journal_issue                   5
_journal_name_full               'Nature chemistry'
_journal_page_first              369
_journal_page_last               373
_journal_paper_doi               10.1038/nchem.617
_journal_volume                  2
_journal_year                    2010
_chemical_formula_moiety         'C84 H77 B F21 N4 P2'
_chemical_formula_sum            'C84 H77 B F21 N4 P2'
_chemical_formula_weight         1614.25
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 97.9780(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4547(11)
_cell_length_b                   39.760(4)
_cell_length_c                   16.5856(15)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      2.63
_cell_volume                     8133.7(13)
_computing_cell_refinement       'Bruker APEX2'
_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    Sir97
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47514
_diffrn_reflns_theta_full        24.41
_diffrn_reflns_theta_max         24.41
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.9825
_exptl_absorpt_correction_T_min  0.9461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             3332
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.00033(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1089
_refine_ls_number_reflns         13377
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0683P)^2^+5.4405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1416
_reflns_number_gt                10508
_reflns_number_total             13377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.617-s3.cif
_cod_data_source_block           NHCP2NHC_BArF_4^+.^
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        8133.8(13)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1508029