Pyrido-annellated diazaphospholenes and phospholenium ions
Benkő, Zoltán; Burck, Sebastian; Gudat, Dietrich; Nieger, Martin; Nyulászi, László; Shore, Nicholas; Dalton Transactions  (2008) 4937–4945; doi:10.1039/b804621b

data_7004241
_publ_section_title
;
 Pyrido-annellated diazaphospholenes and phospholenium ions
;
_journal_issue                   36
_journal_name_full               'Dalton Transactions'
_journal_page_first              4937
_journal_page_last               4945
_journal_paper_doi               10.1039/b804621b
_journal_year                    2008
_chemical_formula_moiety         'C10 H14 N2 P, C F3 S O3'
_chemical_formula_sum            'C11 H14 F3 N2 O3 P S'
_chemical_formula_weight         342.27
_chemical_name_common
;3-Tert.-butyl-(1,5-a)-pyridine-(1,3,2)-diazaphospholenium-
triflate
;
_chemical_name_systematic
;
3-Tert.-butyl-[1,5-a]-pyridine-[1,3,2]-diazaphospholenium-
triflate
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.492(2)
_cell_length_b                   10.685(1)
_cell_length_c                   15.309(1)
_cell_measurement_reflns_used    162
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     3024.9(5)
_computing_cell_refinement       DIRAX/Collect
_computing_data_collection       Collect
_computing_data_reduction        EVALCCD
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 1 deg.'
_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  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            53188
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    0.362
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.002
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.17(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         6883
_refine_ls_number_restraints     303
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0754
_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^)+(0.0592P)^2^+8.5802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1585
_reflns_number_gt                6107
_reflns_number_total             6883
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b804621b.txt
_cod_data_source_block           dg006_hy_compound_2b_otf
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               7004241