#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2011741.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2011741 loop_ _publ_author_name 'Sato, Kiyoshi' 'Arai, Sadao' 'Yamagishi, Takamichi' 'Tanase, Tomoaki' _publ_section_title ; Quinolizinium hexafluorophosphate ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 174 _journal_page_last 175 _journal_volume 57 _journal_year 2001 _chemical_formula_moiety 'C9 H8 N + , P F6 -' _chemical_formula_structural 'C9 H8 N + , P F6 -' _chemical_formula_sum 'C9 H8 F6 N P' _chemical_formula_weight 275.13 _chemical_melting_point 272.8(3) _chemical_name_systematic 'Quinolizinium hexafluorophosphate' _space_group_IT_number 12 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 1 2/m 1' _cell_angle_alpha 90 _cell_angle_beta 115.33(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.505(3) _cell_length_b 9.541(3) _cell_length_c 6.827(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 145.2 _cell_measurement_theta_max 15 _cell_measurement_theta_min 14 _cell_volume 500.7(3) _computing_cell_refinement 'Rigaku/AFC Diffractometer Control Software' _computing_data_collection 'Rigaku/AFC Diffractometer Control Software (Rigaku Corporation, 1995)' _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1998)' _computing_molecular_graphics 'ORTEPIII (Johnson & Burnett, 1996)' _computing_publication_material TEXSAN _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SIR92 (Altomare et al., 1994) and DIRDIF94 (Beurskens et al., 1994)' _diffrn_ambient_temperature 145.2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Rigaku AFC-7R' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .7107 _diffrn_reflns_av_R_equivalents .015 _diffrn_reflns_av_sigmaI/netI .010 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 656 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_reflns_theta_full 27.49 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_min 3.30 _diffrn_standards_decay_% -.62 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu .338 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.825 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle-like _exptl_crystal_F_000 276.00 _exptl_crystal_size_max .44 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .20 _refine_diff_density_max .29 _refine_diff_density_min -.32 _refine_ls_extinction_coef .020 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 54 _refine_ls_number_reflns 562 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.085 _refine_ls_R_factor_all .028 _refine_ls_R_factor_gt .025 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.0321P)^2^+0.3901P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .068 _reflns_number_gt 562 _reflns_number_total 615 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bj1008.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'C 2/m' _[local]_cod_chemical_formula_sum_orig 'C9 H8 F6 N1 P1' _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value '272.5-273' was changed to '272.8(3)' - the average value was taken and precision was estimated. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2011741 loop_ _symmetry_equiv_pos_as_xyz x,y,z x,-y,z -x,-y,-z -x,y,-z 1/2+x,1/2+y,z 1/2+x,1/2-y,z 1/2-x,1/2-y,-z 1/2-x,1/2+y,-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol P1 1 0 3/2 .0212(2) Uani d S 1.00 P F1 .9788(2) 0 1.2550(2) .0361(3) Uani d S 1.00 F F2 1.14610(10) .11821(9) 1.5603(2) .0410(3) Uani d . 1.00 F N5 1 -.4278(2) 1 .0211(3) Uani d SP .50 N C9a 1 -.4278(2) 1 .0211(3) Uani d SP .50 C C1 .9306(2) -.35620(10) 1.1234(2) .0265(3) Uani d . 1.00 C C2 .8607(2) -.4262(2) 1.2391(2) .0296(3) Uani d . 1.00 C H1 .934(2) -.259(2) 1.119(2) .03610(5) Uiso d . 1.00 H H2 .812(2) -.379(2) 1.318(3) .04139(6) Uiso d . 1.00 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol P1 .0218(3) .0199(3) .0217(3) 0 .0092(2) 0 P F1 .0454(7) .0401(7) .0250(6) 0 .0171(5) 0 F F2 .0411(5) .0390(5) .0466(5) -.0187(4) .0223(4) -.0105(4) F N5 .0186(7) .0203(8) .0204(7) 0 .0044(6) 0 N C9a .0186(7) .0203(8) .0204(7) 0 .0044(6) 0 C C1 .0248(6) .0245(6) .0262(6) .0015(5) .0070(5) -.0038(5) C C2 .0259(6) .0377(8) .0244(6) .0023(5) .0100(5) -.0048(5) C loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .003 .002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H .000 .000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N .006 .003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P .102 .094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F .017 .010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -1 -1 1 -1 -2 -1 -3 0 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag F2 P1 F2 1_555 1_555 2_555 89.92(7) yes F2 P1 F2 1_555 1_555 3_758 180.0 yes F2 P1 F2 1_555 1_555 4_758 90.08(7) yes F2 P1 F1 1_555 1_555 1_555 89.81(5) yes F2 P1 F1 1_555 1_555 3_758 90.19(5) yes F2 P1 F2 2_555 1_555 3_758 90.08(7) no F2 P1 F2 2_555 1_555 4_758 180.0 no F2 P1 F1 2_555 1_555 1_555 89.81(5) no F2 P1 F1 2_555 1_555 3_758 90.19(5) no F2 P1 F2 3_758 1_555 4_758 89.92(7) no F2 P1 F1 3_758 1_555 1_555 90.19(5) no F2 P1 F1 3_758 1_555 3_758 89.81(5) no F2 P1 F1 4_758 1_555 1_555 90.19(5) no F2 P1 F1 4_758 1_555 3_758 89.81(5) no F1 P1 F1 1_555 1_555 3_758 180.0 yes N5/C9a N5/C9a C1 2_545 1_555 1_555 119.31(8) yes N5/C9a N5/C9a C1 2_545 1_555 4_757 119.31(8) no C1 N5/C9a C1 1_555 1_555 4_757 121.4(2) yes H1 C1 C2 1_555 1_555 1_555 122.0(10) no H1 C1 N5/C9a 1_555 1_555 1_555 115.0(10) no C2 C1 N5/C9a 1_555 1_555 1_555 121.00(10) yes H2 C2 C1 1_555 1_555 1_555 121.0(10) no H2 C2 C2 1_555 1_555 2_545 119.0(10) no C1 C2 C2 1_555 1_555 2_545 119.65(9) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag P1 F1 1_555 1_555 1.6030(10) yes P1 F1 1_555 3_758 1.6030(10) no P1 F2 1_555 1_555 1.5962(9) yes P1 F2 1_555 2_555 1.5962(9) no P1 F2 1_555 3_758 1.5962(9) no P1 F2 1_555 4_758 1.5962(9) no N5/C9a N5/C9a 1_555 2_545 1.378(3) yes N5/C9a C1 1_555 1_555 1.396(2) yes N5/C9a C1 1_555 4_757 1.396(2) no C1 C2 1_555 1_555 1.352(2) yes C2 C2 1_555 2_545 1.408(3) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N5/C9a N5/C9a C1 C2 2_545 1_555 1_555 1_555 -1.30(10) no N5/C9a N5/C9a C1 C2 1_555 2_545 3_747 3_747 1.30(10) no N5/C9a C1 C2 C2 1_555 1_555 1_555 2_545 1.30(10) no N5/C9a C1 C2 C2 1_555 4_757 4_757 3_747 1.30(10) no C1 N5/C9a N5/C9a C1 1_555 1_555 2_545 2_545 .0 no C1 N5/C9a N5/C9a C1 1_555 1_555 2_545 3_747 180.0 no C1 N5/C9a C1 C2 1_555 1_555 4_757 4_757 178.70(10) no C1 C2 C2 C1 1_555 1_555 2_545 2_545 .0 no