#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2002997.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_2002997 loop_ _publ_author_name 'Malchus, M.' 'Jansen, M.' _publ_section_title ; Structural Investigations of the Phase Transitions of Tetramethylammonium Sulfate ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 494 _journal_page_last 502 _journal_volume 54 _journal_year 1998 _chemical_formula_moiety '2 (C4 H12 N +) (S O4 2-)' _chemical_formula_sum 'C8 H24 N2 O4 S' _chemical_formula_weight 244.35 _chemical_name_systematic ; Tetramethylammonium Sulfate ; _chemical_temperature_decomposition 565 _space_group_IT_number 125 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'P 4 2 -1ab' _symmetry_space_group_name_H-M 'P 4/n b m :1' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.8948(9) _cell_length_b 10.8948(9) _cell_length_c 10.789(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 23.3 _cell_measurement_theta_min 3.2 _cell_volume 1280.6(3) _computing_cell_refinement 'CELDIM (Enraf-Nonius, 1989)' _computing_data_collection 'CAD4 software (Enraf-Nonius, 1989)' _computing_data_reduction 'CADSHEL (Kopf \& Ruebcke, 1993)' _computing_molecular_graphics 'KPLOT (Hundt, 1979), ORTEPII (Johson, 1971)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71070 _diffrn_reflns_av_R_equivalents 0.0151 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 3770 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_min 1.89 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.252 _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_correction_T_min 0.932 _exptl_absorpt_correction_type 'numerical with FACE cards' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description 'see Fig. 4' _exptl_crystal_F_000 536 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _refine_diff_density_max 0.364 _refine_diff_density_min -0.283 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 10.(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.312 _refine_ls_goodness_of_fit_obs 1.344 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 81 _refine_ls_number_reflns 792 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.324 _refine_ls_restrained_S_obs 1.358 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_obs 0.0667 _refine_ls_shift/esd_max <0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'w=1/[\s^2^(Fo^2^)+(0.0087P)^2^+0.9623P], where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.1233 _refine_ls_wR_factor_obs 0.1181 _reflns_number_observed 701 _reflns_number_total 792 _reflns_observed_criterion I>2sigma(I) _[local]_cod_data_source_file jz0003.cif _[local]_cod_data_source_block neub3 _[local]_cod_cif_authors_sg_H-M 'P 4/n b m' _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' tag was changed to '_chemical_temperature_decomposition' since the value had been 'decomposition at 565 K'. The value 'decomposition at 565 K' was changed to '565'. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2002997 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, y+1/2, -z' '-x+1/2, -y+1/2, -z' '-x, y, -z' 'x, -y, -z' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' '-y, x, z' 'y, -x, z' '-y+1/2, x+1/2, -z' 'y+1/2, -x+1/2, -z' '-y, -x, -z' 'y, x, -z' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' 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 S1 0.0243(4) 0.0243(4) 0.0252(6) 0.000 0.000 0.000 O1 0.0580(12) 0.0580(12) 0.061(2) 0.011(2) 0.0198(10) -0.0198(10) N1 0.0301(8) 0.0301(8) 0.0321(12) 0.0002(11) -0.0014(8) 0.0014(8) C1 0.049(2) 0.0412(15) 0.053(2) -0.0030(12) -0.0167(14) -0.0029(13) C2 0.0434(14) 0.0434(14) 0.041(2) 0.010(2) -0.0068(11) 0.0068(11) C3 0.050(2) 0.050(2) 0.046(2) 0.016(2) 0.0028(12) -0.0028(12) S2 0.0376(6) 0.0376(6) 0.0362(8) 0.000 0.000 0.000 O3 0.22(3) 0.22(3) 0.20(3) -0.09(3) -0.01(3) -0.18(2) O4 0.140(11) 0.140(11) 0.035(6) 0.000 0.000 0.000 O5 0.109(14) 0.027(5) 0.083(12) 0.000 -0.033(12) 0.000 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_refinement_flags _atom_site_occupancy _atom_site_type_symbol S1 0.0 0.5000 0.0 0.0246(3) Uani d S 1 S O1 0.0775(2) 0.4225(2) -0.0772(3) 0.0591(9) Uani d S 1 O N1 0.2193(2) 0.2807(2) 0.2515(2) 0.0308(6) Uani d S 1 N C1 0.1412(3) 0.2007(3) 0.1717(3) 0.0479(7) Uani d . 1 C C2 0.2980(2) 0.2020(2) 0.3320(4) 0.0427(9) Uani d S 1 C C3 0.1399(3) 0.3601(3) 0.3300(4) 0.0489(10) Uani d S 1 C H1 0.195(3) 0.150(4) 0.118(3) 0.071(11) Uiso d . 1 H H2 0.094(3) 0.146(3) 0.223(3) 0.070(11) Uiso d . 1 H H3 0.090(3) 0.249(3) 0.119(3) 0.066(10) Uiso d . 1 H H4 0.344(3) 0.255(3) 0.386(2) 0.045(8) Uiso d . 1 H H5 0.349(3) 0.151(3) 0.281(4) 0.046(12) Uiso d S 1 H H6 0.090(3) 0.410(3) 0.281(4) 0.052(12) Uiso d S 1 H H7 0.190(3) 0.409(3) 0.387(3) 0.061(10) Uiso d . 1 H S2 0.0 0.0 0.5000 0.0371(4) Uani d SD 1 S O3 0.025(4) 0.1009(19) 0.5604(17) 0.210(16) Uani d PD 0.25 O O4 0.0 0.0 0.6382(11) 0.105(7) Uani d SPD 0.40 O O5 0.0 0.1370(12) 0.5000 0.073(5) Uani d SPD 0.30 O loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 S1 O1 2_565 6_565 109.08(13) n O1 S1 O1 2_565 5 109.08(13) y O1 S1 O1 6_565 5 110.2(3) y O1 S1 O1 2_565 . 110.2(3) n O1 S1 O1 6_565 . 109.08(13) n O1 S1 O1 5 . 109.08(13) n C3 N1 C2 . . 109.7(3) y C3 N1 C1 . 15 109.6(2) n C2 N1 C1 . 15 109.2(2) n C3 N1 C1 . . 109.6(2) y C2 N1 C1 . . 109.2(2) y C1 N1 C1 15 . 109.5(3) y N1 C1 H1 . . 109.1(19) y N1 C1 H2 . . 109.6(18) y H1 C1 H2 . . 108.(3) y N1 C1 H3 . . 111.(2) y H1 C1 H3 . . 108.(2) y H2 C1 H3 . . 112.(3) y N1 C2 H4 . . 108.0(18) y N1 C2 H5 . . 109.(2) y H4 C2 H5 . . 113.(2) y N1 C3 H6 . . 111.(3) y N1 C3 H7 . . 110.(2) y H6 C3 H7 . . 112.(2) y O3 S2 O3 13_556 6_556 75.6(8) n O3 S2 O3 13_556 . 127.(4) n O3 S2 O3 6_556 . 156.(4) n O3 S2 O3 13_556 14_556 120.2(19) n O3 S2 O3 6_556 14_556 75.6(8) n O3 S2 O3 . 14_556 84.(3) n O3 S2 O3 13_556 5_556 75.6(8) n O3 S2 O3 6_556 5_556 120.2(19) n O3 S2 O3 . 5_556 65.(2) n O3 S2 O3 14_556 5_556 75.6(8) n O3 S2 O3 13_556 10 156.(4) n O3 S2 O3 6_556 10 84.(3) n O3 S2 O3 . 10 75.6(8) n O3 S2 O3 14_556 10 65.(2) n O3 S2 O3 5_556 10 127.(4) n O3 S2 O3 13_556 2 84.(3) n O3 S2 O3 6_556 2 65.(2) n O3 S2 O3 . 2 120.2(19) n O3 S2 O3 14_556 2 127.(4) n O3 S2 O3 5_556 2 156.(4) n O3 S2 O3 10 2 75.6(8) n O3 S2 O3 13_556 9 65.(2) n O3 S2 O3 6_556 9 127.(4) n O3 S2 O3 . 9 75.6(8) n O3 S2 O3 14_556 9 156.(4) n O3 S2 O3 5_556 9 84.(3) n O3 S2 O3 10 9 120.2(19) n O3 S2 O3 2 9 75.6(8) n O3 S2 O4 13_556 5_556 60.1(9) n O3 S2 O4 6_556 5_556 60.1(9) n O3 S2 O4 . 5_556 119.9(9) n O3 S2 O4 14_556 5_556 60.1(9) n O3 S2 O4 5_556 5_556 60.1(9) n O3 S2 O4 10 5_556 119.9(9) n O3 S2 O4 2 5_556 119.9(9) n O3 S2 O4 9 5_556 119.9(9) n O3 S2 O4 13_556 . 119.9(9) n O3 S2 O4 6_556 . 119.9(9) n O3 S2 O4 . . 60.1(9) n O3 S2 O4 14_556 . 119.9(9) n O3 S2 O4 5_556 . 119.9(9) n O3 S2 O4 10 . 60.1(9) n O3 S2 O4 2 . 60.1(9) n O3 S2 O4 9 . 60.1(9) n O4 S2 O4 5_556 . 180.0000(10) n O3 S2 O5 13_556 10 147.3(11) n O3 S2 O5 6_556 10 77.9(18) n O3 S2 O5 . 10 77.9(18) n O3 S2 O5 14_556 10 32.7(11) n O3 S2 O5 5_556 10 102.1(18) n O3 S2 O5 10 10 32.7(11) n O3 S2 O5 2 10 102.1(18) n O3 S2 O5 9 10 147.3(11) n O4 S2 O5 5_556 10 90.0000(10) n O4 S2 O5 . 10 90.0000(10) n O3 S2 O5 13_556 . 102.1(18) n O3 S2 O5 6_556 . 147.3(11) n O3 S2 O5 . . 32.7(11) n O3 S2 O5 14_556 . 77.9(18) n O3 S2 O5 5_556 . 32.7(11) n O3 S2 O5 10 . 102.1(18) n O3 S2 O5 2 . 147.3(11) n O3 S2 O5 9 . 77.9(18) n O4 S2 O5 5_556 . 90.0000(10) n O4 S2 O5 . . 90.0000(10) n O5 S2 O5 10 . 90.000(2) n O5 O3 S2 . . 86.4(15) n O5 O3 O4 . . 143.(3) n S2 O3 O4 . . 66.4(10) n O5 O3 O3 . 5_556 29.1(15) n S2 O3 O3 . 5_556 57.3(11) n O4 O3 O3 . 5_556 118.(2) n O5 O3 O3 . 9 88.(4) n S2 O3 O3 . 9 52.2(4) n O4 O3 O3 . 9 55.4(3) n O3 O3 O3 5_556 9 71.(3) n O5 O3 O3 . 10 126.(2) n S2 O3 O3 . 10 52.2(4) n O4 O3 O3 . 10 55.4(3) n O3 O3 O3 5_556 10 101.5(9) n O3 O3 O3 9 10 90.000(8) n O5 O3 O3 . 14_556 77.8(17) n S2 O3 O3 . 14_556 48.0(16) n O4 O3 O3 . 14_556 100.(2) n O3 O3 O3 5_556 14_556 60.(2) n O3 O3 O3 9 14_556 99.3(11) n O3 O3 O3 10 14_556 50.(2) n O5 O3 O5 . 10 104.(3) n S2 O3 O5 . 10 55.7(13) n O4 O3 O5 . 10 82.4(15) n O3 O3 O5 5_556 10 86.(2) n O3 O3 O5 9 10 105.7(15) n O3 O3 O5 10 10 27.2(13) n O3 O3 O5 14_556 10 26.6(14) n O3 O4 O3 2 9 69.2(6) n O3 O4 O3 2 10 69.2(6) n O3 O4 O3 9 10 106.9(12) n O3 O4 O3 2 . 106.9(12) n O3 O4 O3 9 . 69.2(6) n O3 O4 O3 10 . 69.2(6) n O3 O4 S2 2 . 53.5(6) n O3 O4 S2 9 . 53.5(6) n O3 O4 S2 10 . 53.5(6) n O3 O4 S2 . . 53.5(6) n O3 O5 O3 5_556 . 122.(3) n O3 O5 S2 5_556 . 60.9(15) n O3 O5 S2 . . 60.9(15) n O3 O5 O3 5_556 14_556 65.(3) n O3 O5 O3 . 14_556 76.(2) n S2 O5 O3 . 14_556 46.4(9) n O3 O5 O3 5_556 9 76.(2) n O3 O5 O3 . 9 65.(3) n S2 O5 O3 . 9 46.4(9) n O3 O5 O3 14_556 9 92.7(18) n 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 S1 O1 2_565 1.456(3) y S1 O1 6_565 1.456(3) y S1 O1 5 1.456(3) y S1 O1 . 1.456(3) n N1 C3 . 1.489(5) n N1 C2 . 1.491(4) n N1 C1 15 1.492(3) y N1 C1 . 1.492(3) y C1 H1 . 1.00(4) y C1 H2 . 0.96(3) y C1 H3 . 0.95(4) y C2 H4 . 0.96(3) y C2 H5 . 0.96(4) y C3 H6 . 0.93(4) y C3 H7 . 0.98(3) y S2 O3 13_556 1.307(14) n S2 O3 6_556 1.307(14) n S2 O3 . 1.307(14) y S2 O3 14_556 1.307(14) n S2 O3 5_556 1.307(14) n S2 O3 10 1.307(14) n S2 O3 2 1.307(14) n S2 O3 9 1.307(14) n S2 O4 5_556 1.491(12) n S2 O4 . 1.491(12) y S2 O5 10 1.492(13) n S2 O5 . 1.492(13) y O3 O5 . 0.81(3) n O3 O4 . 1.41(2) n O3 O3 5_556 1.41(4) n O3 O3 9 1.60(3) n O3 O3 10 1.60(3) n O3 O3 14_556 1.75(6) n O3 O5 10 1.77(4) n O4 O3 2 1.41(2) n O4 O3 9 1.41(2) n O4 O3 10 1.41(2) n O5 O3 5_556 0.81(3) n O5 O3 14_556 1.77(4) n O5 O3 9 1.77(4) n