#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/10/2011023.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_2011023 loop_ _publ_author_name 'Dahl, Tor' _publ_section_title ; Intermolecular interactions and molecular geometry in molecular complexes of N,N-dimethylaniline: the 1:1 complex with 1,2,4,5-tetracyanobenzene ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 708 _journal_page_last 710 _journal_volume 56 _journal_year 2000 _chemical_formula_moiety 'C8 H11 N, C10 H2 N4' _chemical_formula_sum 'C18 H13 N5' _chemical_formula_weight 299.33 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method SHELXL-97 _cell_angle_alpha 74.44(4) _cell_angle_beta 87.05(3) _cell_angle_gamma 80.30(3) _cell_formula_units_Z 2 _cell_length_a 7.325(3) _cell_length_b 7.982(4) _cell_length_c 13.452(6) _cell_measurement_reflns_used 25 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 13.13 _cell_measurement_theta_min 6.45 _cell_volume 746.8(6) _computing_cell_refinement 'CAD4 Software' _computing_data_collection 'CAD4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'XCAD4 (Harms, 1996)' _computing_molecular_graphics 'PLATON (Spek, 1998)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full .999 _diffrn_measured_fraction_theta_max .999 _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71069 _diffrn_reflns_av_R_equivalents .0401 _diffrn_reflns_av_sigmaI/netI .0297 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 3648 _diffrn_reflns_theta_full 27.98 _diffrn_reflns_theta_max 27.98 _diffrn_reflns_theta_min 1.57 _diffrn_standards_decay_% 12 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu .084 _exptl_absorpt_correction_T_max .988 _exptl_absorpt_correction_T_min .973 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details 'Platon (Spek, 1998)' _exptl_crystal_colour Brown _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_meas 'not mesured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description Plate _exptl_crystal_F_000 312 _exptl_crystal_size_max .45 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .15 _refine_diff_density_max .327 _refine_diff_density_min -.289 _refine_ls_extinction_coef .013(4) _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 211 _refine_ls_number_reflns 3603 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.066 _refine_ls_R_factor_all .0732 _refine_ls_R_factor_gt .0427 _refine_ls_shift/su_max .002 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0806P)^2^+0.2695P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_ref .1498 _reflns_number_gt 2501 _reflns_number_total 3603 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file os1110.cif _[local]_cod_data_source_block DMA-TCNB _cod_database_code 2011023 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol C1 .4545(2) .2873(2) .28746(12) .0178(3) Uani d . 1 . . C C2 .5234(2) .3766(2) .19209(12) .0194(3) Uani d . 1 . . C H2 .5195 .5005 .1761 .023 Uiso calc R 1 . . H C3 .5966(2) .2858(2) .12149(13) .0242(4) Uani d . 1 . . C H3 .6413 .3487 .0571 .029 Uiso calc R 1 . . H C4 .6065(2) .1056(3) .14221(15) .0267(4) Uani d . 1 . . C H4 .6552 .0445 .0925 .032 Uiso calc R 1 . . H C5 .5440(2) .0163(2) .23684(15) .0265(4) Uani d . 1 . . C H5 .5526 -.1081 .2528 .032 Uiso calc R 1 . . H C6 .4688(2) .1038(2) .30913(14) .0225(4) Uani d . 1 . . C H6 .4268 .0391 .3738 .027 Uiso calc R 1 . . H N1 .3672(2) .37941(19) .35501(11) .0221(3) Uani d . 1 . . N C7 .4002(3) .5574(2) .34391(16) .0293(4) Uani d . 1 . . C H71 .3288 .6057 .3964 .041 Uiso calc R 1 . . H H72 .3616 .6308 .2751 .041 Uiso calc R 1 . . H H73 .5324 .5562 .3527 .041 Uiso calc R 1 . . H C8 .3250(3) .2832(3) .45917(14) .0307(4) Uani d . 1 . . C H81 .2578 .1883 .4565 .043 Uiso calc R 1 . . H H82 .2481 .3636 .4940 .043 Uiso calc R 1 . . H H83 .4404 .2329 .4974 .043 Uiso calc R 1 . . H C11 -.0416(2) .2050(2) .30765(12) .0160(3) Uani d . 1 . . C C12 -.0001(2) .3693(2) .25121(12) .0164(3) Uani d . 1 . . C C13 .0828(2) .3884(2) .15502(12) .0172(3) Uani d . 1 . . C H13 .1122 .4995 .1171 .021 Uiso calc R 1 . . H C14 .1226(2) .2436(2) .11426(12) .0161(3) Uani d . 1 . . C C15 .0794(2) .0804(2) .17050(12) .0160(3) Uani d . 1 . . C C16 -.0017(2) .0604(2) .26718(12) .0167(3) Uani d . 1 . . C H16 -.0297 -.0510 .3054 .020 Uiso calc R 1 . . H C17 -.1242(2) .1861(2) .40830(13) .0187(3) Uani d . 1 . . C C18 -.0433(2) .5188(2) .29338(13) .0199(3) Uani d . 1 . . C C19 .2067(2) .2641(2) .01405(13) .0184(3) Uani d . 1 . . C C20 .1214(2) -.0682(2) .12705(12) .0190(3) Uani d . 1 . . C N11 -.1864(2) .1714(2) .48905(11) .0257(3) Uani d . 1 . . N N12 -.0801(2) .63783(19) .32639(12) .0247(3) Uani d . 1 . . N N13 .2700(2) .2827(2) -.06665(11) .0252(3) Uani d . 1 . . N N14 .1545(2) -.18553(19) .09263(12) .0259(3) Uani d . 1 . . N 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 C1 .0142(7) .0209(8) .0182(8) -.0039(6) -.0020(6) -.0038(6) C2 .0178(8) .0182(7) .0206(8) -.0036(6) .0000(6) -.0021(6) C3 .0183(8) .0349(10) .0189(8) -.0061(7) .0024(6) -.0056(7) C4 .0200(8) .0333(10) .0308(10) -.0009(7) .0003(7) -.0174(8) C5 .0219(8) .0181(8) .0400(11) -.0020(6) -.0046(7) -.0085(7) C6 .0200(8) .0198(8) .0246(8) -.0051(6) -.0019(6) .0010(6) N1 .0219(7) .0255(7) .0196(7) -.0048(6) .0032(5) -.0072(6) C7 .0291(9) .0283(9) .0356(10) -.0046(7) -.0006(8) -.0169(8) C8 .0271(9) .0465(11) .0183(8) -.0077(8) .0043(7) -.0078(8) C11 .0151(7) .0172(7) .0157(7) -.0039(6) .0013(6) -.0037(6) C12 .0147(7) .0162(7) .0181(7) -.0031(6) -.0001(6) -.0039(6) C13 .0166(7) .0151(7) .0190(8) -.0046(6) -.0013(6) -.0012(6) C14 .0154(7) .0172(7) .0154(7) -.0039(6) -.0001(6) -.0028(6) C15 .0164(7) .0146(7) .0176(7) -.0032(6) -.0009(6) -.0045(6) C16 .0167(7) .0138(7) .0189(8) -.0036(6) .0008(6) -.0028(6) C17 .0179(7) .0157(7) .0224(8) -.0030(6) .0011(6) -.0051(6) C18 .0201(8) .0183(8) .0202(8) -.0055(6) .0026(6) -.0023(6) C19 .0202(8) .0153(7) .0202(8) -.0051(6) -.0008(6) -.0038(6) C20 .0224(8) .0162(7) .0175(7) -.0061(6) .0017(6) -.0016(6) N11 .0271(8) .0268(8) .0230(8) -.0055(6) .0051(6) -.0064(6) N12 .0292(8) .0185(7) .0266(8) -.0046(6) .0059(6) -.0070(6) N13 .0315(8) .0239(7) .0205(7) -.0091(6) .0035(6) -.0043(6) N14 .0342(8) .0196(7) .0255(8) -.0083(6) .0061(6) -.0071(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 N1 . 1.384(2) yes C1 C6 . 1.401(2) ? C1 C2 . 1.404(2) ? C2 C3 . 1.379(2) ? C3 C4 . 1.380(3) ? C4 C5 . 1.379(3) ? C5 C6 . 1.384(3) ? N1 C7 . 1.448(2) yes N1 C8 . 1.451(2) yes C11 C16 . 1.386(2) ? C11 C12 . 1.401(2) ? C11 C17 . 1.435(2) ? C12 C13 . 1.382(2) ? C12 C18 . 1.437(2) ? C13 C14 . 1.390(2) ? C14 C15 . 1.398(2) ? C14 C19 . 1.433(2) ? C15 C16 . 1.382(2) ? C15 C20 . 1.440(2) ? C17 N11 . 1.140(2) ? C18 N12 . 1.140(2) ? C19 N13 . 1.140(2) ? C20 N14 . 1.138(2) ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag N1 C1 C6 121.48(15) ? N1 C1 C2 120.69(15) ? C6 C1 C2 117.75(16) ? C3 C2 C1 120.50(16) ? C4 C3 C2 121.51(17) ? C3 C4 C5 118.33(17) ? C4 C5 C6 121.52(17) ? C5 C6 C1 120.34(16) ? C1 N1 C7 118.76(15) yes C1 N1 C8 119.20(15) yes C7 N1 C8 115.22(15) yes C16 C11 C12 120.35(15) ? C16 C11 C17 119.82(14) ? C12 C11 C17 119.82(14) ? C13 C12 C11 120.38(15) ? C13 C12 C18 119.63(14) ? C11 C12 C18 119.99(15) ? C12 C13 C14 119.33(15) ? C13 C14 C15 120.08(15) ? C13 C14 C19 119.31(14) ? C15 C14 C19 120.61(14) ? C16 C15 C14 120.71(15) ? C16 C15 C20 119.95(14) ? C14 C15 C20 119.34(15) ? C15 C16 C11 119.15(15) ? N11 C17 C11 178.58(18) ? N12 C18 C12 179.04(18) ? N13 C19 C14 178.44(18) ? N14 C20 C15 179.91(18) ? _journal_paper_doi 10.1107/S0108270100003590