# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 1145/128 data_Gordon1 #----------------------------------------------------------------------- _publ_requested_journal ' J. Materials Chem.' _publ_contact_letter ; Dear Sir, The following CIF file is sent as supplementary data to the paper "Ionic Liquid Crystals: Hexafluorophosphate Salts" by CM Gordon, JD Holbrey, AR Kennedy and KR Seddon which has been submitted to you for consideration for publication. If there are any problems with this file or its transmission please contact me. Yours Sincerely, Alan Kennedy. ; _publ_contact_author_phone ' 0141 552 4400 ext 4241 ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email 'a.r.kennedy@ccsun.strath.ac.uk' _publ_contact_author ; Dr Alan R. Kennedy Dept. of P & A Chemistry University of Strathclyde 295 Cathedral St. Glasgow G1 1XL Scotland ; #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'SIR' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _audit_creation_date 'Tue Jul 7 11:25:49 1998' _audit_creation_method 'from TEXRAY.INF file' #----------------------------------------------------------------------- _cell_length_a 9.175(2) _cell_length_b 9.849(3) _cell_length_c 22.197(4) _cell_angle_alpha 90 _cell_angle_beta 94.13(2) _cell_angle_gamma 90 _cell_volume 2000.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 123 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.15 _cell_measurement_theta_max 17.35 #----------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y, -z' ' -x, -y, -z' '1/2+x,1/2-y, +z' #----------------------------------------------------------------------- _exptl_crystal_description 'plate' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.700 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 396.40 _chemical_formula_analytical ? _chemical_formula_sum 'C16 H31 F6 N2 P ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 840.00 _exptl_absorpt_coefficient_mu 0.192 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.938 #----------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'Rigaku AFC7S' _diffrn_measurement_method '\w/2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.52 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 4676 _reflns_number_total 4401 _reflns_number_observed 2497 _reflns_observed_criterion 'I>2\s(I)' _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 26.51 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.09542 _diffrn_orient_matrix_UB_12 -0.04142 _diffrn_orient_matrix_UB_13 -0.01487 _diffrn_orient_matrix_UB_21 0.01951 _diffrn_orient_matrix_UB_22 0.02456 _diffrn_orient_matrix_UB_23 -0.04238 _diffrn_orient_matrix_UB_31 0.04955 _diffrn_orient_matrix_UB_32 -0.08938 _diffrn_orient_matrix_UB_33 -0.00477 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 64 0.003 0.002 'International Tables' H 0 124 0.000 0.000 'International Tables' F 0 24 0.017 0.010 'International Tables' N 0 8 0.006 0.003 'International Tables' P 0 4 0.102 0.094 'International Tables' #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom P(1) 0.30121(7) 0.01795(7) 0.36776(3) 0.0287 Uij ? ? F(1) 0.4299(2) -0.0865(2) 0.35835(7) 0.0389 Uij ? ? F(2) 0.2302(2) -0.0884(2) 0.41232(7) 0.0438 Uij ? ? F(3) 0.2059(2) -0.0476(2) 0.31236(6) 0.0410 Uij ? ? F(4) 0.3948(2) 0.0813(2) 0.42465(8) 0.0598 Uij ? ? F(5) 0.3724(2) 0.1223(2) 0.32414(8) 0.0527 Uij ? ? F(6) 0.1705(2) 0.1207(2) 0.37804(9) 0.0572 Uij ? ? N(1) 0.8772(2) -0.1167(2) 0.43703(9) 0.0293 Uij ? ? N(2) 0.8330(2) -0.0020(2) 0.35516(8) 0.0244 Uij ? ? C(1) 0.9462(3) -0.2120(3) 0.4812(1) 0.0413 Uij ? ? C(2) 0.9127(3) -0.1016(2) 0.3807(1) 0.0272 Uij ? ? C(3) 0.7698(3) -0.0246(3) 0.4477(1) 0.0367 Uij ? ? C(4) 0.7424(3) 0.0463(3) 0.3969(1) 0.0348 Uij ? ? C(5) 0.8387(3) 0.0468(2) 0.2925(1) 0.0295 Uij ? ? C(6) 0.6989(3) 0.0152(2) 0.2545(1) 0.0265 Uij ? ? C(7) 0.6753(3) -0.1358(2) 0.2443(1) 0.0283 Uij ? ? C(8) 0.5303(3) -0.1707(3) 0.2095(1) 0.0299 Uij ? ? C(9) 0.5099(3) -0.1100(3) 0.1465(1) 0.0287 Uij ? ? C(10) 0.3727(3) -0.1634(2) 0.1112(1) 0.0279 Uij ? ? C(11) 0.3428(3) -0.1012(3) 0.0487(1) 0.0307 Uij ? ? C(12) 0.2057(3) -0.1575(3) 0.0150(1) 0.0290 Uij ? ? C(13) 0.1679(3) -0.0932(3) -0.0466(1) 0.0328 Uij ? ? C(14) 0.0297(3) -0.1482(2) -0.0789(1) 0.0296 Uij ? ? C(15) -0.0128(3) -0.0824(3) -0.1390(1) 0.0433 Uij ? ? C(16) -0.1506(4) -0.1377(3) -0.1712(1) 0.0519 Uij ? ? H(1) 0.8759 -0.2467 0.5032 0.0496 Uij ? ? H(2) 0.9857 -0.2809 0.4625 0.0496 Uij ? ? H(3) 1.0056 -0.1682 0.5099 0.0496 Uij ? ? H(4) 0.9810 -0.1546 0.3594 0.0326 Uij ? ? H(5) 0.7316 -0.0212 0.4827 0.0441 Uij ? ? H(6) 0.6752 0.1176 0.3881 0.0417 Uij ? ? H(7) 0.9242 0.0048 0.2765 0.0354 Uij ? ? H(8) 0.8554 0.1435 0.2942 0.0354 Uij ? ? H(9) 0.7064 0.0584 0.2164 0.0318 Uij ? ? H(10) 0.6161 0.0524 0.2724 0.0318 Uij ? ? H(11) 0.7567 -0.1706 0.2204 0.0339 Uij ? ? H(12) 0.6763 -0.1828 0.2825 0.0339 Uij ? ? H(13) 0.5236 -0.2697 0.2042 0.0359 Uij ? ? H(14) 0.4525 -0.1414 0.2351 0.0359 Uij ? ? H(15) 0.5065 -0.0054 0.1499 0.0344 Uij ? ? H(16) 0.5917 -0.1266 0.1234 0.0344 Uij ? ? H(17) 0.2843 -0.1440 0.1348 0.0335 Uij ? ? H(18) 0.3790 -0.2647 0.1059 0.0335 Uij ? ? H(19) 0.3347 -0.0077 0.0521 0.0368 Uij ? ? H(20) 0.4250 -0.1114 0.0243 0.0368 Uij ? ? H(21) 0.1187 -0.1471 0.0384 0.0348 Uij ? ? H(22) 0.2128 -0.2581 0.0101 0.0348 Uij ? ? H(23) 0.1594 0.0002 -0.0409 0.0394 Uij ? ? H(24) 0.2468 -0.1021 -0.0706 0.0394 Uij ? ? H(25) -0.0523 -0.1393 -0.0533 0.0356 Uij ? ? H(26) 0.0373 -0.2444 -0.0828 0.0356 Uij ? ? H(27) 0.0611 -0.0875 -0.1629 0.0519 Uij ? ? H(28) -0.0290 0.0196 -0.1312 0.0519 Uij ? ? H(29) -0.1709 -0.0986 -0.2067 0.0623 Uij ? ? H(30) -0.2400 -0.1202 -0.1476 0.0623 Uij ? ? H(31) -0.1396 -0.2310 -0.1798 0.0623 Uij ? ? 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 P(1) 0.0306(3) 0.0274(3) 0.0279(3) -0.0002(3) 0.0008(3) -0.0043(3) F(1) 0.0371(8) 0.0366(9) 0.0430(9) 0.0081(7) 0.0029(7) 0.0021(7) F(2) 0.0367(9) 0.062(1) 0.0317(8) -0.0087(8) -0.0013(7) 0.0138(8) F(3) 0.0449(9) 0.0495(10) 0.0271(8) -0.0021(8) -0.0078(7) -0.0020(7) F(4) 0.0433(10) 0.088(1) 0.048(1) -0.0226(10) 0.0029(8) -0.035(1) F(5) 0.054(1) 0.0353(9) 0.070(1) -0.0028(8) 0.0128(9) 0.0171(9) F(6) 0.0425(10) 0.0416(10) 0.089(1) 0.0082(8) 0.0144(9) -0.0173(10) N(1) 0.035(1) 0.027(1) 0.025(1) -0.0095(10) -0.0050(9) 0.0002(9) N(2) 0.024(1) 0.023(1) 0.025(1) -0.0053(9) -0.0025(8) -0.0003(8) C(1) 0.055(2) 0.036(2) 0.031(1) -0.009(1) -0.010(1) 0.007(1) C(2) 0.025(1) 0.025(1) 0.031(1) -0.003(1) -0.003(1) 0.000(1) C(3) 0.041(2) 0.044(2) 0.026(1) -0.002(1) 0.004(1) -0.010(1) C(4) 0.036(1) 0.033(1) 0.035(1) 0.004(1) -0.001(1) -0.008(1) C(5) 0.033(1) 0.025(1) 0.030(1) -0.004(1) -0.002(1) 0.005(1) C(6) 0.028(1) 0.025(1) 0.026(1) 0.000(1) -0.0035(10) 0.002(1) C(7) 0.032(1) 0.026(1) 0.026(1) 0.002(1) -0.006(1) 0.000(1) C(8) 0.034(1) 0.028(1) 0.027(1) -0.005(1) -0.005(1) -0.001(1) C(9) 0.029(1) 0.031(1) 0.025(1) -0.001(1) -0.002(1) 0.000(1) C(10) 0.031(1) 0.025(1) 0.027(1) -0.001(1) -0.005(1) 0.001(1) C(11) 0.033(1) 0.032(1) 0.026(1) -0.003(1) -0.002(1) 0.003(1) C(12) 0.034(1) 0.027(1) 0.025(1) 0.000(1) -0.004(1) 0.001(1) C(13) 0.033(1) 0.039(2) 0.026(1) -0.001(1) -0.003(1) 0.004(1) C(14) 0.036(1) 0.026(1) 0.027(1) 0.000(1) -0.002(1) 0.000(1) C(15) 0.039(2) 0.063(2) 0.027(1) -0.002(2) -0.003(1) 0.011(1) C(16) 0.072(2) 0.042(2) 0.037(2) 0.004(2) -0.025(2) -0.003(1) #----------------------------------------------------------------------- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '1/\s^2^(F)' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen_type_2_Gaussian_isotropic' _refine_ls_extinction_coef '5.4(8)x10^-7^' _refine_ls_number_reflns 2497 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_obs 0.0394 _refine_ls_R_factor_all 0.1082 _refine_ls_wR_factor_obs 0.0435 _refine_ls_wR_factor_all 0.0519 _refine_ls_goodness_of_fit_obs 1.339 _refine_ls_shift/esd_max 0.0003 _refine_diff_density_min -0.24 _refine_diff_density_max 0.22 #----------------------------------------------------------------------- _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag P(1) F(1) 1.591(2) ? ? yes P(1) F(2) 1.610(2) ? ? yes P(1) F(3) 1.593(2) ? ? yes P(1) F(4) 1.602(2) ? ? yes P(1) F(5) 1.584(2) ? ? yes P(1) F(6) 1.599(2) ? ? yes N(1) C(1) 1.468(3) ? ? yes N(1) C(2) 1.322(3) ? ? yes N(1) C(3) 1.373(4) ? ? yes N(2) C(2) 1.326(3) ? ? yes N(2) C(4) 1.374(3) ? ? yes N(2) C(5) 1.477(3) ? ? yes C(3) C(4) 1.334(4) ? ? yes C(5) C(6) 1.515(3) ? ? yes C(6) C(7) 1.518(3) ? ? yes C(7) C(8) 1.528(3) ? ? yes C(8) C(9) 1.521(3) ? ? yes C(9) C(10) 1.526(3) ? ? yes C(10) C(11) 1.524(3) ? ? yes C(11) C(12) 1.520(3) ? ? yes C(12) C(13) 1.524(3) ? ? yes C(13) C(14) 1.511(4) ? ? yes C(14) C(15) 1.509(4) ? ? yes C(15) C(16) 1.508(4) ? ? yes #----------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F(1) P(1) F(2) 89.84(9) ? ? ? yes F(1) P(1) F(3) 90.45(8) ? ? ? yes F(1) P(1) F(4) 89.68(9) ? ? ? yes F(1) P(1) F(5) 89.81(9) ? ? ? yes F(1) P(1) F(6) 178.87(10) ? ? ? yes F(2) P(1) F(3) 89.23(8) ? ? ? yes F(2) P(1) F(4) 89.26(9) ? ? ? yes F(2) P(1) F(5) 179.54(9) ? ? ? yes F(2) P(1) F(6) 89.03(9) ? ? ? yes F(3) P(1) F(4) 178.49(10) ? ? ? yes F(3) P(1) F(5) 91.06(9) ? ? ? yes F(3) P(1) F(6) 89.49(9) ? ? ? yes F(4) P(1) F(5) 90.45(10) ? ? ? yes F(4) P(1) F(6) 90.35(10) ? ? ? yes F(5) P(1) F(6) 91.32(10) ? ? ? yes C(1) N(1) C(2) 125.5(2) ? ? ? yes C(1) N(1) C(3) 126.0(2) ? ? ? yes C(2) N(1) C(3) 108.5(2) ? ? ? yes C(2) N(2) C(4) 108.0(2) ? ? ? yes C(2) N(2) C(5) 126.0(2) ? ? ? yes C(4) N(2) C(5) 125.9(2) ? ? ? yes N(1) C(2) N(2) 108.8(2) ? ? ? yes N(1) C(3) C(4) 107.1(2) ? ? ? yes N(2) C(4) C(3) 107.6(2) ? ? ? yes N(2) C(5) C(6) 111.8(2) ? ? ? yes C(5) C(6) C(7) 113.0(2) ? ? ? yes C(6) C(7) C(8) 114.0(2) ? ? ? yes C(7) C(8) C(9) 114.9(2) ? ? ? yes C(8) C(9) C(10) 112.3(2) ? ? ? yes C(9) C(10) C(11) 114.6(2) ? ? ? yes C(10) C(11) C(12) 112.9(2) ? ? ? yes C(11) C(12) C(13) 114.6(2) ? ? ? yes C(12) C(13) C(14) 113.9(2) ? ? ? yes C(13) C(14) C(15) 114.8(2) ? ? ? yes C(14) C(15) C(16) 114.7(2) ? ? ? yes #----------------------------------------------------------------------- #===END