#------------------------------------------------------------------------------ #$Date: 2017-01-11 11:54:23 +0000 (Wed, 11 Jan 2017) $ #$Revision: 190394 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/32/2003264.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_2003264 loop_ _publ_author_name 'Kivikoski, J.' 'Howard, J. A. K.' 'Kelly, P.' 'Parker, D.' _publ_section_title ; Tetraethylammonium Perchlorate at 150 K ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 535 _journal_page_last 536 _journal_paper_doi 10.1107/S0108270194008619 _journal_volume 51 _journal_year 1995 _chemical_formula_moiety 'C8 H20 Cl N O4' _chemical_formula_structural '((C2H5)4 N) (Cl O4)' _chemical_formula_sum 'C8 H20 Cl N O4' _chemical_formula_weight 229.70 _chemical_name_systematic 'Tetraethylammonium perchlorate' _space_group_IT_number 9 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'C -2yc' _symmetry_space_group_name_H-M 'C 1 c 1' _atom_type_scat_source IntTabIV _audit_creation_method CRYSTALS _cell_angle_alpha 90.000 _cell_angle_beta 114.86(3) _cell_angle_gamma 90.000 _cell_formula_units_Z 4 _cell_length_a 12.514(5) _cell_length_b 7.433(4) _cell_length_c 13.956(6) _cell_measurement_reflns_used 25 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 15 _cell_measurement_theta_min 8 _cell_volume 1177.9(10) _computing_cell_refinement MSC/AFC _computing_data_collection MSC/AFC _computing_data_reduction 'TEXSAN Version 5.0 (MSC, 1989)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material CRYSTALS _computing_structure_refinement CRYSTALS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_measurement_device 'Rigaku AFC6S 4-circle diffractometer' _diffrn_measurement_method '2\q/\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_number 2305 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 3.00 _diffrn_standards_decay_% 5.4 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.314 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.941 _exptl_absorpt_correction_type empirical _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.30 _exptl_crystal_description plate _exptl_crystal_F_000 496 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.60 _refine_diff_density_max 0.33 _refine_diff_density_min -0.56 _refine_ls_extinction_method none _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 125 _refine_ls_number_reflns 1068 _refine_ls_number_restraints 2 _refine_ls_restrained_S_obs 1.0468 _refine_ls_R_factor_obs 0.0489 _refine_ls_shift/esd_max 0.002 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme ;w = w'[1-(\DF/6\sF)^2^]^2^, where w' is a Chebyshev polynomial for F~c~ with 5 coefficients (2.27, 1.51, 2.35, 0.492 and 0.783). ; _refine_ls_wR_factor_obs 0.0517 _reflns_limit_h_max 16 _reflns_limit_h_min 0 _reflns_limit_k_max 8 _reflns_limit_k_min -9 _reflns_limit_l_max 8 _reflns_limit_l_min -8 _reflns_number_observed 1068 _reflns_number_total 1352 _reflns_observed_criterion >3.0sigma(I) _cod_data_source_file hu1122.cif _cod_data_source_block park1 _cod_depositor_comments ; Moving the _atom_type_scat_dispersion_real and _atom_type_scat_dispersion_imag data items into the _atom_type loop. Antanas Vaitkus, 2017-01-11 ; _cod_original_cell_volume 1178.0(10) _cod_original_sg_symbol_H-M 'C c' _cod_database_code 2003264 loop_ _symmetry_equiv_pos_as_xyz X,Y,Z X+1/2,Y+1/2,Z X,-Y,Z+1/2 X+1/2,-Y+1/2,Z+1/2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Cl1 0.0273(4) 0.0005(5) 0.0097(3) 0.0260(4) 0.0023(5) 0.0260(4) O1 0.058(2) 0.016(2) 0.028(2) 0.053(2) 0.026(2) 0.051(2) O2 0.073(1) -0.008(1) 0.026(1) 0.073(1) -0.008(1) 0.073(1) O3 0.086(2) 0.016(2) 0.045(2) 0.086(2) 0.016(2) 0.086(2) O4 0.119(5) 0.002(3) 0.069(3) 0.082(4) -0.011(3) 0.071(3) O22 0.020(1) -0.008(1) 0.004(1) 0.020(1) -0.008(1) 0.020(1) O33 0.046(2) 0.016(2) 0.028(2) 0.046(2) 0.016(2) 0.046(2) N1 0.023(2) -0.003(1) 0.003(1) 0.022(2) 0.000(1) 0.019(1) C1 0.016(2) 0.001(2) -0.002(2) 0.042(2) 0.007(2) 0.025(2) C2 0.049(3) 0.004(2) 0.013(2) 0.026(2) -0.004(2) 0.027(2) C3 0.029(2) -0.005(2) 0.012(2) 0.031(2) 0.005(2) 0.035(2) C4 0.033(2) 0.003(2) 0.010(2) 0.018(2) 0.008(2) 0.033(2) C11 0.027(2) -0.000(3) 0.014(2) 0.070(4) 0.009(3) 0.044(3) C22 0.085(5) 0.011(3) 0.027(3) 0.027(3) 0.000(3) 0.054(4) C33 0.061(4) -0.001(3) 0.038(4) 0.059(4) -0.003(3) 0.050(4) C44 0.034(3) 0.004(2) 0.004(3) 0.037(3) 0.012(3) 0.045(3) loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Cl1 1.0000 0.5364(2) 0.1269(1) 0.3694(2) 0.0268 Uani O1 1.0000 0.5470(4) 0.0104(6) 0.4535(3) 0.0470 Uani O2 0.714(7) 0.5828(7) 0.297(1) 0.4009(6) 0.0736 Uani O3 0.737(9) 0.4121(7) 0.148(1) 0.3011(6) 0.0809 Uani O4 1.0000 0.5778(5) 0.0405(8) 0.3011(4) 0.0701 Uani O22 0.286(7) 0.6427(8) 0.243(1) 0.4213(8) 0.0189 Uani O33 0.263(9) 0.437(1) 0.245(2) 0.348(1) 0.0397 Uani N1 1.0000 0.9060(3) 0.1206(5) 0.1181(3) 0.0224 Uani C1 1.0000 1.0298(4) 0.1220(6) 0.2058(3) 0.0267 Uani C2 1.0000 0.8954(4) -0.0075(6) 0.0297(3) 0.0326 Uani C3 1.0000 0.8222(4) 0.0585(6) 0.1641(3) 0.0310 Uani C4 1.0000 0.8764(4) 0.3094(5) 0.0726(3) 0.0272 Uani C11 1.0000 1.1259(5) 0.1669(9) 0.1707(5) 0.0431 Uani C22 1.0000 0.9356(7) -0.2004(8) 0.0641(5) 0.0493 Uani C33 1.0000 0.8156(6) 0.180(1) 0.2473(5) 0.0487 Uani C44 1.0000 0.7517(5) 0.3345(9) -0.0102(5) 0.0395 Uani H11 1.0000 1.0465(4) -0.0002(6) 0.2389(3) 0.0800 Uiso H12 1.0000 1.0333(4) 0.2132(6) 0.2597(3) 0.0800 Uiso H21 1.0000 0.9456(4) 0.0413(6) -0.0043(3) 0.0800 Uiso H22 1.0000 0.8112(4) -0.0090(6) -0.0229(3) 0.0800 Uiso H31 1.0000 0.8479(4) -0.0634(6) 0.1958(3) 0.0800 Uiso H32 1.0000 0.7420(4) 0.0499(6) 0.1046(3) 0.0800 Uiso H41 1.0000 0.9309(4) 0.3399(5) 0.0393(3) 0.0800 Uiso H42 1.0000 0.8895(4) 0.3950(5) 0.1318(3) 0.0800 Uiso H111 1.0000 1.2049(5) 0.1648(9) 0.2321(5) 0.0800 Uiso H112 1.0000 1.1242(5) 0.0760(9) 0.1172(5) 0.0800 Uiso H113 1.0000 1.1110(5) 0.2894(9) 0.1380(5) 0.0800 Uiso H221 1.0000 0.9257(7) -0.2731(8) 0.0006(5) 0.0800 Uiso H222 1.0000 1.0201(7) -0.2024(8) 0.1160(5) 0.0800 Uiso H223 1.0000 0.8857(7) -0.2527(8) 0.0974(5) 0.0800 Uiso H331 1.0000 0.7578(6) 0.129(1) 0.2722(5) 0.0800 Uiso H332 1.0000 0.8947(6) 0.190(1) 0.3082(5) 0.0800 Uiso H333 1.0000 0.7889(6) 0.303(1) 0.2170(5) 0.0800 Uiso H441 1.0000 0.7396(5) 0.4615(9) -0.0362(5) 0.0800 Uiso H442 1.0000 0.7372(5) 0.2510(9) -0.0706(5) 0.0800 Uiso H443 1.0000 0.6957(5) 0.3061(9) 0.0219(5) 0.0800 Uiso loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C ' 0.0020 0.0020 'H ' 0.0000 0.0000 'N ' 0.0040 0.0030 'O ' 0.0080 0.0060 'Cl ' 0.1320 0.1590 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 O1 Cl1 O2 114.5(4) yes O1 Cl1 O3 108.0(3) yes O2 Cl1 O3 107.6(6) yes O1 Cl1 O4 110.3(3) yes O2 Cl1 O4 113.9(4) yes O3 Cl1 O4 101.6(4) yes O1 Cl1 O22 101.3(5) no O2 Cl1 O22 31.7(4) no O3 Cl1 O22 138.5(6) no O4 Cl1 O22 94.9(5) no O1 Cl1 O33 108.3(5) no O2 Cl1 O33 73.8(8) no O3 Cl1 O33 37.7(6) no O4 Cl1 O33 131.5(7) no O22 Cl1 O33 105.3(8) no Cl1 O2 O22 81.6(10) no Cl1 O2 O33 54.8(6) no O22 O2 O33 136.1(11) no Cl1 O3 O33 70.7(10) no Cl1 O22 O2 66.6(9) no Cl1 O33 O2 51.5(6) no Cl1 O33 O3 71.5(10) no O2 O33 O3 117.6(13) no C1 N1 C2 111.7(3) yes C1 N1 C3 108.3(3) yes C2 N1 C3 108.3(3) yes C1 N1 C4 108.5(3) yes C2 N1 C4 108.5(3) yes C3 N1 C4 111.5(3) yes N1 C1 C11 114.8(4) yes N1 C1 H11 108.1(2) no C11 C1 H11 108.0(3) no N1 C1 H12 108.6(2) no C11 C1 H12 107.7(3) no H11 C1 H12 109.47 no N1 C2 C22 115.3(4) yes N1 C2 H21 107.4(2) no C22 C2 H21 107.5(4) no N1 C2 H22 108.0(2) no C22 C2 H22 109.0(3) no H21 C2 H22 109.47 no N1 C3 C33 114.7(4) yes N1 C3 H31 108.2(2) no C33 C3 H31 108.4(3) no N1 C3 H32 107.4(2) no C33 C3 H32 108.6(3) no H31 C3 H32 109.47 no N1 C4 C44 115.1(4) yes N1 C4 H41 108.0(2) no C44 C4 H41 107.6(3) no N1 C4 H42 108.4(2) no C44 C4 H42 108.1(3) no H41 C4 H42 109.47 no C1 C11 H111 110.6(3) no C1 C11 H112 108.7(3) no H111 C11 H112 109.48 no C1 C11 H113 109.1(3) no H111 C11 H113 109.48 no H112 C11 H113 109.48 no C2 C22 H221 109.1(3) no C2 C22 H222 110.4(3) no H221 C22 H222 109.48 no C2 C22 H223 108.9(4) no H221 C22 H223 109.48 no H222 C22 H223 109.48 no C3 C33 H331 108.7(3) no C3 C33 H332 109.9(3) no H331 C33 H332 109.48 no C3 C33 H333 109.8(3) no H331 C33 H333 109.48 no H332 C33 H333 109.48 no C4 C44 H441 110.1(3) no C4 C44 H442 109.4(3) no H441 C44 H442 109.48 no C4 C44 H443 108.9(3) no H441 C44 H443 109.48 no H442 C44 H443 109.48 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Cl1 O1 1.420(4) yes Cl1 O2 1.383(8) yes Cl1 O3 1.452(8) yes Cl1 O4 1.416(4) yes Cl1 O22 1.490(9) no Cl1 O33 1.440(10) no O2 O22 0.790(10) no O2 O33 1.70(2) no O3 O33 0.94(2) no N1 C1 1.518(5) yes N1 C2 1.519(5) yes N1 C3 1.515(5) yes N1 C4 1.521(5) yes C1 C11 1.515(7) yes C1 H11 1.00 no C1 H12 1.00 no C2 C22 1.528(7) yes C2 H21 1.00 no C2 H22 1.00 no C3 C33 1.503(8) yes C3 H31 1.00 no C3 H32 1.00 no C4 C44 1.513(7) yes C4 H41 1.00 no C4 H42 1.00 no C11 H111 1.00 no C11 H112 1.00 no C11 H113 1.00 no C22 H221 1.00 no C22 H222 1.00 no C22 H223 1.00 no C33 H331 1.00 no C33 H332 1.00 no C33 H333 1.00 no C44 H441 1.00 no C44 H442 1.00 no C44 H443 1.00 no 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 _geom_torsion_publ_flag C11 C1 N1 C2 56.1(5) yes C11 C1 N1 C3 175.3(4) yes C11 C1 N1 C4 -63.5(5) yes C22 C2 N1 C1 53.9(5) yes C22 C2 N1 C3 -65.3(5) yes C22 C2 N1 C4 173.5(4) yes C33 C3 N1 C1 63.2(5) yes C33 C3 N1 C2 -175.5(4) yes C33 C3 N1 C4 -56.2(5) yes C44 C4 N1 C1 -175.3(4) yes C44 C4 N1 C2 63.2(5) yes C44 C4 N1 C3 -56.1(5) yes