#------------------------------------------------------------------------------ #$Date: 2014-07-12 14:53:54 +0100 (Sat, 12 Jul 2014) $ #$Revision: 120119 $ #$URL: svn://www.crystallography.net/cod/cif/4/06/02/4060208.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4060208 loop_ _publ_author_name 'Tomoyuki Akutagawa' 'Sadamu Takeda' 'Tatsuo Hasegawa' 'Takayoshi Nakamura' _publ_section_title ; Proton Transfer and a Dielectric Phase Transition in the Molecular Conductor (HDABCO+)2(TCNQ)3 ; _journal_name_full 'Journal of the American Chemical Society' _journal_volume 126 _journal_page_first 291 _journal_page_last 294 _journal_year 2004 _chemical_formula_sum 'C24 H19 N8' _chemical_formula_moiety 'C24 H19 N8' _chemical_formula_weight 419.47 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' _cell_length_a 7.8164(7) _cell_length_b 10.3585(3) _cell_length_c 14.020(1) _cell_angle_alpha 88(2) _cell_angle_beta 83.944(3) _cell_angle_gamma 69.911(3) _cell_volume 1060.0(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3255 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 27.3 _cell_measurement_temperature 473.1 _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 438.00 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.992 _exptl_absorpt_correction_T_max 0.992 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 8124 _diffrn_reflns_av_R_equivalents 0.062 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9088 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9088 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _reflns_number_total 4415 _reflns_number_gt 2285 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0730 _refine_ls_wR_factor_ref 0.0720 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 2309 _refine_ls_number_parameters 309 _refine_ls_goodness_of_fit_ref 0.674 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 8051.2800 11215.9000 3287.7500 ; _refine_ls_shift/su_max 0.1740 _refine_diff_density_max 0.34 _refine_diff_density_min -0.28 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N(1) N 0.6314(4) 0.8668(3) 0.5016(2) 0.0481(8) Uani 1.00 1 d . . . N(2) N 0.8713(4) 0.6308(3) 0.5011(2) 0.0450(8) Uani 1.00 1 d . . . N(3) N 0.2407(5) 0.7825(5) 0.6666(2) 0.083(1) Uani 1.00 1 d . . . N(4) N -0.2537(5) 0.7777(4) 0.8305(2) 0.070(1) Uani 1.00 1 d . . . N(5) N 0.6507(5) 0.8982(4) 1.1889(3) 0.075(1) Uani 1.00 1 d . . . N(6) N 0.1511(5) 0.9073(4) 1.3420(2) 0.070(1) Uani 1.00 1 d . . . N(7) N 0.5989(5) 0.4467(4) 0.6628(2) 0.069(1) Uani 1.00 1 d . . . N(8) N 0.0801(5) 0.4356(5) 0.7988(3) 0.079(1) Uani 1.00 1 d . . . C(1) C 0.1352(4) 0.8104(3) 0.9192(2) 0.0423(8) Uani 1.00 1 d . . . C(2) C 0.3151(4) 0.8168(3) 0.9201(2) 0.0447(8) Uani 1.00 1 d . . . C(3) C 0.3788(4) 0.8372(4) 1.0022(2) 0.0458(9) Uani 1.00 1 d . . . C(4) C 0.2730(5) 0.8479(3) 1.0924(2) 0.0426(8) Uani 1.00 1 d . . . C(5) C 0.0937(4) 0.8402(3) 1.0925(2) 0.0424(8) Uani 1.00 1 d . . . C(6) C 0.0289(4) 0.8209(3) 1.0099(2) 0.0439(8) Uani 1.00 1 d . . . C(7) C 0.0685(4) 0.7938(3) 0.8341(2) 0.0464(9) Uani 1.00 1 d . . . C(8) C 0.1671(5) 0.7858(4) 0.7416(3) 0.054(1) Uani 1.00 1 d . . . C(9) C -0.1112(5) 0.7840(4) 0.8338(2) 0.051(1) Uani 1.00 1 d . . . C(10) C 0.3388(4) 0.8706(3) 1.1775(2) 0.0450(9) Uani 1.00 1 d . . . C(11) C 0.5126(5) 0.8848(4) 1.1809(2) 0.050(1) Uani 1.00 1 d . . . C(12) C 0.2322(5) 0.8886(4) 1.2680(2) 0.0480(9) Uani 1.00 1 d . . . C(13) C 0.4461(4) 0.4792(3) 0.9092(2) 0.0410(8) Uani 1.00 1 d . . . C(14) C 0.6198(4) 0.4905(3) 0.9171(2) 0.0444(8) Uani 1.00 1 d . . . C(15) C 0.3281(4) 0.4903(3) 0.9962(2) 0.0436(8) Uani 1.00 1 d . . . C(16) C 0.3911(5) 0.4586(3) 0.8190(2) 0.0471(9) Uani 1.00 1 d . . . C(17) C 0.5072(5) 0.4526(4) 0.7333(2) 0.051(1) Uani 1.00 1 d . . . C(18) C 0.2176(5) 0.4474(4) 0.8087(2) 0.054(1) Uani 1.00 1 d . . . C(19) C 0.6666(5) 0.8259(4) 0.6012(2) 0.057(1) Uani 1.00 1 d . . . C(20) C 0.8206(6) 0.6878(4) 0.5995(2) 0.055(1) Uani 1.00 1 d . . . C(21) C 0.8040(5) 0.8693(4) 0.4462(3) 0.065(1) Uani 1.00 1 d . . . C(22) C 0.9442(5) 0.7238(4) 0.4413(3) 0.062(1) Uani 1.00 1 d . . . C(23) C 0.5661(5) 0.7670(4) 0.4573(3) 0.061(1) Uani 1.00 1 d . . . C(24) C 0.7066(5) 0.6219(4) 0.4614(2) 0.052(1) Uani 1.00 1 d . . . H(1) H 0.5000 1.0000 0.5000 0.18(4) Uiso 1.00 1 c . . . H(2) H 1.0000 0.5000 0.5000 0.14(3) Uiso 1.00 1 c . . . H(3) H 0.5583(5) 0.8214(4) 0.6366(2) 0.068(1) Uiso 1.00 1 c . . . H(4) H 0.7059(5) 0.8909(4) 0.6309(2) 0.068(1) Uiso 1.00 1 c . . . H(5) H 0.7764(6) 0.6290(4) 0.6400(2) 0.068(2) Uiso 1.00 1 c . . . H(6) H 0.9251(6) 0.6973(4) 0.6233(2) 0.068(2) Uiso 1.00 1 c . . . H(7) H 0.7857(5) 0.9030(4) 0.3832(3) 0.074(2) Uiso 1.00 1 c . . . H(8) H 0.8465(5) 0.9280(4) 0.4809(3) 0.074(2) Uiso 1.00 1 c . . . H(9) H 0.9806(5) 0.6938(4) 0.3764(3) 0.070(2) Uiso 1.00 1 c . . . H(10) H 1.0487(5) 0.7213(4) 0.4714(3) 0.070(2) Uiso 1.00 1 c . . . H(11) H 0.4504(5) 0.7674(4) 0.4863(3) 0.075(2) Uiso 1.00 1 c . . . H(12) H 0.5575(5) 0.7903(4) 0.3917(3) 0.075(2) Uiso 1.00 1 c . . . H(13) H 0.6528(5) 0.5665(4) 0.4999(2) 0.064(1) Uiso 1.00 1 c . . . H(14) H 0.7450(5) 0.5821(4) 0.3989(2) 0.064(1) Uiso 1.00 1 c . . . H(15) H 0.3930(4) 0.8059(3) 0.8619(2) 0.054(1) Uiso 1.00 1 c . . . H(16) H 0.4983(4) 0.8422(4) 0.9998(2) 0.056(1) Uiso 1.00 1 c . . . H(17) H 0.0163(4) 0.8559(3) 1.1512(2) 0.051(1) Uiso 1.00 1 c . . . H(18) H -0.0866(4) 0.8085(3) 1.0150(2) 0.052(1) Uiso 1.00 1 c . . . H(19) H 0.7024(4) 0.4827(3) 0.8609(2) 0.053(1) Uiso 1.00 1 c . . . H(20) H 0.2121(4) 0.4816(3) 0.9916(2) 0.054(1) Uiso 1.00 1 c . . . 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 N(1) 0.041(1) 0.043(2) 0.055(2) -0.010(1) 0.001(1) 0.007(1) N(2) 0.049(2) 0.037(1) 0.048(2) -0.011(1) -0.009(1) -0.000(1) N(3) 0.073(2) 0.137(4) 0.042(2) -0.044(3) 0.008(2) 0.006(2) N(4) 0.049(2) 0.103(3) 0.064(2) -0.034(2) -0.007(1) 0.003(2) N(5) 0.056(2) 0.082(3) 0.096(3) -0.037(2) -0.010(2) 0.004(2) N(6) 0.069(2) 0.094(3) 0.055(2) -0.043(2) 0.010(2) -0.008(2) N(7) 0.081(2) 0.090(2) 0.046(2) -0.044(2) 0.000(1) 0.001(2) N(8) 0.060(2) 0.095(3) 0.086(2) -0.030(2) -0.012(2) -0.011(2) C(1) 0.043(2) 0.033(1) 0.049(2) -0.010(1) -0.001(1) 0.005(1) C(2) 0.041(2) 0.048(2) 0.044(2) -0.017(1) 0.004(1) 0.005(1) C(3) 0.034(2) 0.054(2) 0.052(2) -0.019(1) 0.003(1) -0.001(1) C(4) 0.041(2) 0.041(2) 0.047(2) -0.017(1) 0.001(1) -0.002(1) C(5) 0.038(2) 0.046(2) 0.043(2) -0.017(1) 0.006(1) 0.001(1) C(6) 0.033(1) 0.048(2) 0.050(2) -0.014(1) 0.000(1) 0.006(1) C(7) 0.039(2) 0.050(2) 0.051(2) -0.016(2) -0.004(1) 0.006(1) C(8) 0.052(2) 0.067(2) 0.045(2) -0.022(2) -0.002(1) 0.003(1) C(9) 0.050(2) 0.059(2) 0.046(2) -0.021(2) -0.004(1) 0.006(1) C(10) 0.043(2) 0.044(2) 0.050(2) -0.020(2) 0.002(1) 0.001(1) C(11) 0.051(2) 0.053(2) 0.049(2) -0.021(2) -0.006(1) 0.004(1) C(12) 0.053(2) 0.061(2) 0.038(2) -0.031(2) -0.006(1) -0.002(1) C(13) 0.045(2) 0.047(2) 0.036(1) -0.022(1) -0.003(1) 0.001(1) C(14) 0.048(2) 0.050(2) 0.035(2) -0.019(1) 0.004(1) 0.001(1) C(15) 0.037(2) 0.046(2) 0.050(2) -0.019(1) -0.002(1) 0.004(1) C(16) 0.054(2) 0.047(2) 0.038(2) -0.015(2) -0.004(1) 0.004(1) C(17) 0.069(2) 0.060(2) 0.030(2) -0.028(2) -0.010(1) 0.002(1) C(18) 0.056(2) 0.062(2) 0.045(2) -0.021(2) -0.005(1) -0.004(1) C(19) 0.064(2) 0.054(2) 0.051(2) -0.019(2) 0.007(1) -0.009(2) C(20) 0.073(2) 0.054(2) 0.044(2) -0.023(2) -0.024(2) 0.005(1) C(21) 0.055(2) 0.045(2) 0.084(3) -0.012(2) 0.019(2) 0.017(2) C(22) 0.044(2) 0.046(2) 0.086(3) -0.008(2) 0.014(2) 0.009(2) C(23) 0.052(2) 0.069(2) 0.066(2) -0.021(2) -0.021(2) 0.007(2) C(24) 0.062(2) 0.048(2) 0.051(2) -0.022(2) -0.018(1) 0.001(1) _cod_database_code 4060208 _journal_paper_doi 10.1021/ja0377697