Benzo-1,3,2-diazaphospholide and benzo-1,3,2-diazaphospholium: an isoelectronic aromatic anion-cation pair.
Schmid, Dirk; Loscher, Sebastian; Gudat, Dietrich; Bubrin, Denis; Hartenbach, Ingo; Schleid, Thomas; Benko, Zoltán; Nyulászi, László; Chemical communications (Cambridge, England) 34 (2009) 830–832; doi:10.1039/b817046k

data_7104177
_publ_section_title
;
 Benzo-1,3,2-diazaphospholide and benzo-1,3,2-diazaphospholium: an
 isoelectronic aromatic anion-cation pair.
;
_journal_issue                   7
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              830
_journal_page_last               832
_journal_paper_doi               10.1039/b817046k
_journal_volume                  34
_journal_year                    2009
_chemical_formula_sum            'C7 H6 F3 N2 O3 P S'
_chemical_formula_weight         286.17
_chemical_name_common
'Benzo-1,3,2H-Diazaphospholenium Trifluormethane sulfonate'
_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                114.374(4)
_cell_angle_beta                 112.907(4)
_cell_angle_gamma                92.534(4)
_cell_formula_units_Z            4
_cell_length_a                   9.9377(7)
_cell_length_b                   11.2028(8)
_cell_length_c                   11.6347(8)
_cell_measurement_reflns_used    10799
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      1.02
_cell_volume                     1053.91(13)
_computing_cell_refinement       'DENZO (W. Minor & Z. Otwinowski)'
_computing_data_collection       'Nonius Collect Software'
_computing_data_reduction        'DENZO (W. Minor & Z. Otwinowski)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'four-circle, ccd detector'
_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  0.1513
_diffrn_reflns_av_sigmaI/netI    0.1427
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15230
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    0.500
_exptl_absorpt_correction_T_max  0.9529
_exptl_absorpt_correction_T_min  0.7698
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'HABITUS (W. Herrendorf)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath-shaped
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1397
_refine_ls_R_factor_gt           0.0638
_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^)+(0.0620P)^2^+0.1748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1576
_reflns_number_gt                2912
_reflns_number_total             5077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b817046k.txt
_cod_data_source_block           c:\crystal\x-red32\dsnov07
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7104177