2,6,10-Tris(dialkylamino)trioxatriangulenium Ions. Synthesis, Structure, and Properties of Exceptionally Stable Carbenium Ions
Bo W. Laursen; Frederik C. Krebs; Merete F. Nielsen; Klaus Bechgaard; Jørn B. Christensen; Niels Harrit; Journal of the American Chemical Society 120 (1998) 12255–12263; doi:10.1021/ja982550r

data_4116899
_publ_section_title
;
 2,6,10-Tris(dialkylamino)trioxatriangulenium Ions. Synthesis, Structure,
 and Properties of Exceptionally Stable Carbenium Ions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12255
_journal_page_last               12263
_journal_paper_doi               10.1021/ja982550r
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C31 H30 F6 N3 O3 P'
_chemical_formula_weight         637.55
_chemical_name_systematic
; 
 2,6,10-Tris(N-pyrrolidinyl)trioxatriangulenium hexafluoro-
 phosphate 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 95.74(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.546(3)
_cell_length_b                   8.343(2)
_cell_length_c                   22.604(5)
_cell_measurement_temperature    120(2)
_cell_volume                     2729.4(11)
_computing_cell_refinement       'SAINT Siemens'
_computing_data_collection       'SMART Siemens'
_computing_data_reduction        'SAINT Siemens'
_computing_molecular_graphics    'SHELXTL (Sheldrick)'
_computing_publication_material  'XCIF (Sheldrick)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       'omega scan, frame data integration'
_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  0.2444
_diffrn_reflns_av_sigmaI/netI    0.2054
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            27660
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.183
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       needle
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.025
_refine_ls_goodness_of_fit_obs   1.181
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_restrained_S_obs      1.181
_refine_ls_R_factor_all          0.2431
_refine_ls_R_factor_obs          0.0881
_refine_ls_shift/esd_max         0.010
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+8.4530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2507
_refine_ls_wR_factor_obs         0.1705
_reflns_number_observed          2148
_reflns_number_total             5586
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja982550r.cif
_cod_data_source_block           compound5b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+8.4530P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+8.4530P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2729.4(9)
_cod_database_code               4116899