#------------------------------------------------------------------------------ #$Date: 2025-08-19 11:43:10 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301803 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/52/2205221.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_2205221 loop_ _publ_author_name 'Fu, Yun-Long' 'Xu, Zhi-Wei' 'Ren, Jia-Lin' 'Ng, Seik Weng' _publ_section_title ; Bis[diethylenetriaminium(3+)] tris(sulfate) monohydrate ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o772 _journal_page_last o773 _journal_paper_doi 10.1107/S1600536805005362 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '2C4 H16 N3 3+, 3S O4 2-, H2 O' _chemical_formula_moiety '2C4 H16 N3 3+, 3S O4 2-, H2 O' _chemical_formula_sum 'C8 H34 N6 O13 S3' _chemical_formula_weight 518.59 _chemical_name_systematic ; Bis[diethylenetriaminium(3+)] tris(sulfate) monohydrate ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 102.045(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.2490(10) _cell_length_b 13.6480(10) _cell_length_c 16.082(2) _cell_measurement_reflns_used 1515 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 27.1 _cell_measurement_theta_min 2.5 _cell_volume 2200.0(4) _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 0.033 _diffrn_reflns_av_sigmaI/netI 0.046 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 6500 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 2.5 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.409 _exptl_absorpt_correction_type none _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 1104 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.52 _refine_diff_density_min -0.37 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 155 _refine_ls_number_reflns 2468 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.06 _refine_ls_R_factor_all 0.074 _refine_ls_R_factor_gt 0.058 _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^)+(0.0814P)^2^+3.1409P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.143 _refine_ls_wR_factor_ref 0.154 _reflns_number_gt 1971 _reflns_number_total 2468 _reflns_threshold_expression I>2\s(I) _cod_data_source_file bt6607.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'None' changed to 'none' 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: '_exptl_absorpt_correction_type' value 'None' changed to 'none' 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 2199.9(4) _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2205221 _cod_database_fobs_code 2205221 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' '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 -0.02979(8) 0.30927(5) 0.53962(5) 0.0325(2) Uani d . 1 . . S S2 0.5000 0.46114(7) 0.7500 0.0282(3) Uani d SD 1 . . S O1 0.1158(2) 0.3145(2) 0.5720(2) 0.0476(6) Uani d . 1 . . O O2 -0.0955(2) 0.3729(2) 0.5922(2) 0.0482(7) Uani d . 1 . . O O3 -0.0618(2) 0.3480(2) 0.4522(2) 0.0484(7) Uani d . 1 . . O O4 -0.0736(3) 0.2083(2) 0.5432(2) 0.0521(7) Uani d . 1 . . O O5 0.4522(6) 0.5410(3) 0.6899(3) 0.056(2) Uani d PD 0.50 A -1 O O6 0.4621(7) 0.3675(3) 0.7073(4) 0.073(2) Uani d PD 0.50 A -1 O O7 0.6473(4) 0.4659(4) 0.7594(4) 0.0530(10) Uani d PD 0.50 A -1 O O8 0.4654(7) 0.4725(5) 0.8317(3) 0.076(2) Uani d PD 0.50 A -1 O O1w 0.0000 0.4740(4) 0.7500 0.139(3) Uani d S 1 . . O N1 0.2490(3) 0.4872(2) 0.5531(2) 0.0374(7) Uani d . 1 . . N N2 0.3032(2) 0.3691(2) 0.3524(2) 0.0277(5) Uani d . 1 . . N N3 0.2069(3) 0.2139(2) 0.1576(2) 0.0380(6) Uani d . 1 . . N C1 0.3239(3) 0.4580(2) 0.4881(2) 0.0345(7) Uani d . 1 . . C C2 0.2300(3) 0.4143(2) 0.4122(2) 0.0354(7) Uani d . 1 . . C C3 0.2146(3) 0.3227(2) 0.2790(2) 0.0331(7) Uani d . 1 . . C C4 0.2948(3) 0.2662(2) 0.2271(2) 0.0355(7) Uani d . 1 . . C H1w1 -0.0261 0.4368 0.7068 0.167 Uiso d . 1 . . H H1n1 0.3031 0.5119 0.5961 0.045 Uiso calc R 1 . . H H1n2 0.2107 0.4366 0.5690 0.045 Uiso calc R 1 . . H H1n3 0.1898 0.5300 0.5320 0.045 Uiso calc R 1 . . H H2n1 0.3502 0.4134 0.3342 0.033 Uiso calc R 1 . . H H2n2 0.3571 0.3257 0.3789 0.033 Uiso calc R 1 . . H H3n1 0.2544 0.1819 0.1286 0.046 Uiso calc R 1 . . H H3n2 0.1574 0.2553 0.1251 0.046 Uiso calc R 1 . . H H3n3 0.1574 0.1737 0.1783 0.046 Uiso calc R 1 . . H H1a 0.3916 0.4103 0.5119 0.041 Uiso calc R 1 . . H H1b 0.3681 0.5148 0.4704 0.041 Uiso calc R 1 . . H H2a 0.1747 0.3652 0.4316 0.043 Uiso calc R 1 . . H H2b 0.1717 0.4652 0.3832 0.043 Uiso calc R 1 . . H H3a 0.1627 0.3726 0.2439 0.040 Uiso calc R 1 . . H H3b 0.1532 0.2788 0.2989 0.040 Uiso calc R 1 . . H H4a 0.3515 0.3108 0.2038 0.043 Uiso calc R 1 . . H H4b 0.3516 0.2196 0.2633 0.043 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 0.0352(4) 0.0303(4) 0.0330(4) 0.0067(3) 0.0095(3) 0.0096(3) S2 0.0310(6) 0.0247(5) 0.0267(5) 0.000 0.0012(4) 0.000 O1 0.0350(10) 0.058(2) 0.047(2) 0.0100(10) 0.0030(10) 0.0200(10) O2 0.051(2) 0.0350(10) 0.064(2) 0.0040(10) 0.0240(10) -0.0050(10) O3 0.0420(10) 0.060(2) 0.0410(10) -0.0030(10) 0.0020(10) 0.0210(10) O4 0.074(2) 0.0290(10) 0.059(2) 0.0030(10) 0.0260(10) 0.0050(10) O5 0.073(4) 0.036(3) 0.044(3) 0.004(2) -0.021(3) 0.007(2) O6 0.079(4) 0.031(3) 0.097(5) -0.013(3) -0.011(3) -0.010(3) O7 0.031(3) 0.065(4) 0.064(3) -0.004(2) 0.013(2) 0.013(3) O8 0.084(5) 0.106(6) 0.049(3) 0.034(4) 0.039(3) 0.018(3) O1w 0.239(8) 0.055(3) 0.083(4) 0.000 -0.059(5) 0.000 N1 0.040(2) 0.038(2) 0.0310(10) 0.0150(10) -0.0030(10) -0.0060(10) N2 0.0270(10) 0.0270(10) 0.0300(10) 0.0020(10) 0.0070(10) 0.0020(10) N3 0.046(2) 0.036(2) 0.035(2) -0.0100(10) 0.0170(10) -0.0050(10) C1 0.028(2) 0.036(2) 0.037(2) 0.0020(10) 0.0030(10) -0.0050(10) C2 0.028(2) 0.044(2) 0.035(2) 0.0020(10) 0.0070(10) -0.0090(10) C3 0.029(2) 0.035(2) 0.035(2) -0.0010(10) 0.0060(10) -0.0050(10) C4 0.034(2) 0.037(2) 0.036(2) 0.0020(10) 0.0070(10) -0.0050(10) 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 _geom_angle_publ_flag O1 S1 O2 108.6(2) yes O1 S1 O3 109.10(10) yes O1 S1 O4 109.2(2) yes O2 S1 O3 107.4(2) yes O2 S1 O4 110.80(10) yes O3 S1 O4 111.7(2) yes O5 S2 O6 108.6(3) yes O5 S2 O7 103.1(3) yes O5 S2 O8 114.1(4) yes O6 S2 O7 104.5(4) yes O6 S2 O8 115.5(4) yes O7 S2 O8 109.9(4) yes C3 N2 C2 113.0(2) yes N1 C1 C2 109.9(2) yes N2 C2 C1 111.5(2) yes N2 C3 C4 110.4(2) yes N3 C4 C3 110.7(3) yes C1 N1 H1n1 109.5 no C1 N1 H1n2 109.5 no H1n1 N1 H1n2 109.5 no C1 N1 H1n3 109.5 no H1n1 N1 H1n3 109.5 no H1n2 N1 H1n3 109.5 no C3 N2 H2n1 109.0 no C2 N2 H2n1 109.0 no C3 N2 H2n2 109.0 no C2 N2 H2n2 109.0 no H2n1 N2 H2n2 107.8 no C4 N3 H3n1 109.5 no C4 N3 H3n2 109.5 no H3n1 N3 H3n2 109.5 no C4 N3 H3n3 109.5 no H3n1 N3 H3n3 109.5 no H3n2 N3 H3n3 109.5 no N1 C1 H1a 109.7 no C2 C1 H1a 109.7 no N1 C1 H1b 109.7 no C2 C1 H1b 109.7 no H1a C1 H1b 108.2 no N2 C2 H2a 109.3 no C1 C2 H2a 109.3 no N2 C2 H2b 109.3 no C1 C2 H2b 109.3 no H2a C2 H2b 108.0 no N2 C3 H3a 109.6 no C4 C3 H3a 109.6 no N2 C3 H3b 109.6 no C4 C3 H3b 109.6 no H3a C3 H3b 108.1 no N3 C4 H4a 109.5 no C3 C4 H4a 109.5 no N3 C4 H4b 109.5 no C3 C4 H4b 109.5 no H4a C4 H4b 108.1 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag S1 O1 1.476(2) yes S1 O2 1.470(2) yes S1 O3 1.473(2) yes S1 O4 1.455(2) yes S2 O5 1.471(3) yes S2 O6 1.465(4) yes S2 O7 1.486(3) yes S2 O8 1.439(4) yes N1 C1 1.474(4) yes N2 C3 1.474(4) yes N2 C2 1.474(4) yes N3 C4 1.466(4) yes C1 C2 1.510(4) yes C3 C4 1.500(4) yes O1w H1w1 0.86 no N1 H1n1 0.86 no N1 H1n2 0.86 no N1 H1n3 0.86 no N2 H2n1 0.86 no N2 H2n2 0.86 no N3 H3n1 0.86 no N3 H3n2 0.86 no N3 H3n3 0.86 no C1 H1a 0.97 no C1 H1b 0.97 no C2 H2a 0.97 no C2 H2b 0.97 no C3 H3a 0.97 no C3 H3b 0.97 no C4 H4a 0.97 no C4 H4b 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 O1w H1w1 O2 . 0.86 2.03 2.875(4) 169 N1 H1n2 O1 . 0.86 1.93 2.772(4) 164 N1 H1n1 O5 . 0.86 1.95 2.793(5) 166 N1 H1n3 O3 5_566 0.86 2.17 2.946(4) 151 N2 H2n2 O1 7_556 0.86 2.07 2.833(3) 148 N2 H2n1 O8 6_565 0.86 1.96 2.788(6) 161 N3 H3n1 O2 8 0.86 1.91 2.738(4) 162 N3 H3n3 O6 8_455 0.86 2.22 3.001(7) 151 N3 H3n3 O7 8_455 0.86 2.32 3.080(6) 147 N3 H3n3 O8 7_556 0.86 2.35 3.122(8) 150 N3 H3n2 O3 2 0.86 1.90 2.755(4) 174 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 C3 N2 C2 C1 178.0(3) no N1 C1 C2 N2 -170.3(2) no C2 N2 C3 C4 -172.1(3) no N2 C3 C4 N3 175.8(2) no loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139067483