#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/52/2205222.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_2205222 loop_ _publ_author_name 'Fu, Yun-Long' 'Xu, Zhi-Wei' 'Ren, Jia-Lin' 'Ng, Seik Weng' _publ_section_title ; Triethylenetetraminium(4+) bis(sulfate) monohydrate ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o774 _journal_page_last o775 _journal_paper_doi 10.1107/S1600536805005477 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac 'C6 H22 N4 4+ , 2S O4 2- , H2 O' _chemical_formula_moiety 'C6 H22 N4 4+ , 2S O4 2- , H2 O' _chemical_formula_sum 'C6 H24 N4 O9 S2' _chemical_formula_weight 360.41 _chemical_name_systematic ; Trimethylenetetraaminium(4+) bis(sulfate) monohydrate ; _space_group_IT_number 58 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2 2n' _symmetry_space_group_name_H-M 'P n n m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.3192(8) _cell_length_b 22.253(3) _cell_length_c 5.4903(7) _cell_measurement_reflns_used 861 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 23.5 _cell_measurement_theta_min 3.4 _cell_volume 772.05(17) _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_collection 'SMART (Bruker, 2002)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 0.97 _diffrn_measured_fraction_theta_max 0.97 _diffrn_measurement_device_type 'Bruker APEX area-detector' _diffrn_measurement_method '\f and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI 0.033 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_number 3543 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 1.8 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.393 _exptl_absorpt_correction_type none _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_meas ? _exptl_crystal_density_method . _exptl_crystal_description block _exptl_crystal_F_000 384 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _refine_diff_density_max 0.57 _refine_diff_density_min -0.51 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.14 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 113 _refine_ls_number_reflns 946 _refine_ls_number_restraints 148 _refine_ls_restrained_S_all 1.11 _refine_ls_R_factor_all 0.081 _refine_ls_R_factor_gt 0.070 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0921P)^2^+1.2465P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.174 _refine_ls_wR_factor_ref 0.185 _reflns_number_gt 840 _reflns_number_total 946 _reflns_threshold_expression I>2\s(I) _cod_data_source_file bt6608.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 772.1(2) _cod_database_code 2205222 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' '-x-1/2, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' 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 S1 0.2004(2) 0.35894(4) 0.5000 0.0247(4) Uani d SD 1 . . S O1 0.3600(10) 0.3110(3) 0.483(4) 0.034(2) Uani d PDU 0.25 A -1 O O2 -0.0124(9) 0.3318(3) 0.472(4) 0.040(3) Uani d PDU 0.25 B -1 O O3 0.234(3) 0.4028(5) 0.306(2) 0.039(4) Uani d PDU 0.25 A -1 O O4 0.215(3) 0.3881(6) 0.7382(16) 0.033(3) Uani d PDU 0.25 A -1 O O5 0.156(3) 0.3167(7) 0.301(2) 0.027(3) Uani d PDU 0.25 A -2 O O6 0.4171(9) 0.3820(3) 0.474(4) 0.045(3) Uani d PDU 0.25 A -2 O O7 0.178(3) 0.3280(8) 0.735(2) 0.032(4) Uani d PDU 0.25 A -2 O O8 0.0490(10) 0.4091(2) 0.488(5) 0.036(2) Uani d PDU 0.25 C -2 O O1W 0.5000 0.5000 0.5000 0.160(5) Uani d SU 1 . . O N1 0.5074(6) 0.29452(16) 0.0000 0.0324(9) Uani d S 1 . . N N2 0.8959(6) 0.42124(15) 0.0000 0.0302(9) Uani d S 1 . . N C1 0.7079(8) 0.3255(2) 0.0000 0.0440(10) Uani d S 1 . . C C2 0.6924(7) 0.3914(2) 0.0000 0.0390(10) Uani d S 1 . . C C3 0.8940(7) 0.48638(19) 0.0000 0.0390(10) Uani d S 1 . . C H1W1 0.5946 0.5260 0.4685 0.192 Uiso d P 0.25 D -3 H H1W2 0.5269 0.4676 0.4242 0.192 Uiso d P 0.25 E -3 H H1N1 0.5288 0.2564 0.0000 0.039 Uiso calc SR 1 . . H H1N2 0.4369 0.3044 0.1279 0.039 Uiso calc R 1 . . H H2N 0.9650 0.4094 -0.1262 0.036 Uiso calc R 1 . . H H1 0.7874 0.3131 0.1425 0.053 Uiso calc R 1 . . H H2 0.6135 0.4040 0.1427 0.047 Uiso calc R 1 . . H H3 0.8177 0.5002 0.1426 0.047 Uiso calc R 1 . . H 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 0.0245(6) 0.0217(6) 0.0278(6) -0.0004(4) 0.000 0.000 O1 0.041(4) 0.033(3) 0.027(6) 0.013(3) 0.004(7) 0.000(6) O2 0.036(4) 0.040(4) 0.044(8) -0.006(3) -0.020(6) 0.011(5) O3 0.049(7) 0.033(7) 0.036(6) -0.005(5) 0.002(5) 0.008(5) O4 0.033(5) 0.035(6) 0.033(6) 0.002(5) -0.004(5) -0.005(5) O5 0.030(6) 0.020(6) 0.030(6) -0.010(4) 0.005(5) -0.007(5) O6 0.038(4) 0.046(4) 0.051(8) -0.013(3) 0.017(6) -0.003(6) O7 0.032(7) 0.034(7) 0.030(6) 0.001(5) 0.007(5) -0.002(5) O8 0.051(4) 0.026(3) 0.032(5) 0.012(3) -0.009(8) -0.001(8) O1W 0.162(8) 0.120(7) 0.198(9) -0.068(6) 0.000 0.000 N1 0.029(2) 0.021(2) 0.047(2) 0.002(2) 0.000 0.000 N2 0.024(2) 0.022(2) 0.045(2) 0.002(2) 0.000 0.000 C1 0.025(2) 0.025(2) 0.081(4) 0.002(2) 0.000 0.000 C2 0.024(2) 0.023(2) 0.071(4) 0.000(2) 0.000 0.000 C3 0.028(2) 0.020(2) 0.069(4) 0.003(2) 0.000 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 '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 O2 . . 108.6(5) no O1 S1 O3 . . 109.9(5) no O1 S1 O4 . . 109.7(5) no O2 S1 O3 . . 109.2(5) no O2 S1 O4 . . 109.2(5) no O3 S1 O4 . . 110.3(4) no O5 S1 O6 . . 109.4(5) no O5 S1 O7 . . 109.6(4) no O5 S1 O8 . . 109.1(5) no O6 S1 O7 . . 109.8(5) no O6 S1 O8 . . 109.8(5) no O7 S1 O8 . . 109.7(5) no C2 N2 C3 . . 116.9(4) no N1 C1 C2 . . 114.7(4) no N2 C2 C1 . . 113.5(4) no N2 C3 C3 . 5_765 113.9(5) no H1W1 O1W H1W2 . . 109.7 no C1 N1 H1N1 . . 109.5 no C1 N1 H1N2 . . 109.5 no H1N1 N1 H1N2 . . 109.5 no C2 N2 H2N . . 108.1 no C3 N2 H2N . . 108.1 no N1 C1 H1 . . 108.6 no C2 C1 H1 . . 108.6 no N2 C2 H2 . . 108.9 no C1 C2 H2 . . 108.9 no N2 C3 H3 . . 108.8 no C3 C3 H3 5_765 . 108.8 no 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 . 1.470(5) no S1 O2 . 1.482(6) no S1 O3 . 1.461(6) no S1 O4 . 1.463(6) no S1 O5 . 1.471(6) no S1 O6 . 1.469(5) no S1 O7 . 1.468(7) no S1 O8 . 1.472(5) no N1 C1 . 1.443(6) no N2 C2 . 1.448(6) no N2 C3 . 1.450(5) no C1 C2 . 1.469(7) no C3 C3 5_765 1.470(9) no O1W H1W1 . 0.85 no O1W H1W2 . 0.85 no N1 H1N1 . 0.86 no N1 H1N2 . 0.86 no N2 H2N . 0.86 no C1 H1 . 0.97 no C2 H2 . 0.97 no C3 H3 . 0.97 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1W H1W1 O3 5_666 0.85 2.29 2.940(10) 134 yes O1W H1W1 O3 2_665 0.85 2.12 2.940(10) 163 yes O1W H1W2 O6 . 0.85 2.05 2.681(7) 131 yes O1W H1W2 O6 6_556 0.85 2.10 2.681(7) 125 yes O1W H1W1 O6 5_666 0.85 2.07 2.681(7) 128 yes O1W H1W1 O6 2_665 0.85 2.05 2.681(7) 131 yes N1 H1N1 O2 3 0.86 1.98 2.818(8) 163 yes N1 H1N1 O5 3 0.86 2.12 2.86(2) 145 yes N1 H1N2 O1 . 0.86 2.01 2.83(2) 159 yes N1 H1N2 O7 6_556 0.86 1.88 2.65(2) 148 yes N2 H2N O3 6_655 0.86 1.97 2.75(2) 150 yes N2 H2N O4 1_654 0.86 1.81 2.58(2) 149 yes N2 H2N O7 1_654 0.86 2.38 3.10(2) 141 yes N2 H2N O8 6_655 0.86 2.06 2.86(3) 156 yes N2 H2N O8 1_654 0.86 2.18 2.98(3) 155 yes 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_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C3 N2 C2 C1 . 180.0 no N1 C1 C2 N2 . 180.0 no C2 N2 C3 C3 5_765 180.0 no