#------------------------------------------------------------------------------ #$Date: 2025-08-19 11:01:59 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301802 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/19/2101965.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_2101965 loop_ _publ_author_name 'Feng Xue' 'Thomas C. W. Mak' _publ_section_title ; Channel- and layer-type anionic host structures in inclusion compounds of urea, tetraalkylammonium terephthalate/trimesate and water ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 142 _journal_page_last 154 _journal_paper_doi 10.1107/S0108768199011283 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac '2[N(C4 H9)4]+,C8 H4 O4 2-,6(C H4 N2 O),2(H2 O)' _chemical_formula_sum 'C46 H104 N14 O12' _chemical_formula_weight 1045.43 _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 SHELXL97 _cell_angle_alpha 105.06(2) _cell_angle_beta 94.910(10) _cell_angle_gamma 93.82(2) _cell_formula_units_Z 1 _cell_length_a 8.390(2) _cell_length_b 9.894(2) _cell_length_c 18.908(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 15 _cell_measurement_theta_min 5 _cell_volume 1503.6(6) _computing_cell_refinement 'MSC/AFC (MSC, 1988)' _computing_data_collection 'MSC/AFC (MSC, 1988)' _computing_data_reduction 'MSC/AFC (MSC, 1988)' _computing_molecular_graphics 'Siemens SHELXTL-PC (Siemens, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .985 _diffrn_measured_fraction_theta_max .985 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method '\w scan' _diffrn_radiation_monochromator graphite _diffrn_radiation_source ; Rigaku RU-200 rotating-anode generator operated at 50kV and 90mA ; _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0185 _diffrn_reflns_av_sigmaI/netI .0528 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 5604 _diffrn_reflns_theta_full 25.14 _diffrn_reflns_theta_max 25.14 _diffrn_reflns_theta_min 2.14 _diffrn_standards_decay_% -.36 _diffrn_standards_interval_count 197 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu .084 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min .951 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'psi scan (Kopfmann & Huber, 1968)' _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 574 _exptl_crystal_size_max .40 _exptl_crystal_size_mid .38 _exptl_crystal_size_min .22 _refine_diff_density_max .319 _refine_diff_density_min -.313 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 325 _refine_ls_number_reflns 5277 _refine_ls_number_restraints 67 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all .1041 _refine_ls_R_factor_gt .0503 _refine_ls_shift/su_max .000 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+0.1259P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .1642 _reflns_number_gt 2982 _reflns_number_total 5277 _reflns_threshold_expression I>2\s(I) _cod_data_source_file hr0043.cif _cod_data_source_block compd1 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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 'Triclinic' changed to 'triclinic' 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 The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+0.1259P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+0.1259P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 1503.6(2) _cod_database_code 2101965 _cod_database_fobs_code 2101965 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_type_symbol C1 .9589(3) .1839(2) -.03177(12) .0526(6) Uani d D 1 C O1 .8567(2) .14061(17) .00384(9) .0605(4) Uani d D 1 O N1 .9502(3) .3089(2) -.04676(11) .0653(6) Uani d D 1 N H1A .8742 .3598 -.0319 .078 Uiso calc R 1 H H1B 1.0207 .3380 -.0712 .078 Uiso calc R 1 H N2 1.0768(2) .1074(2) -.05694(11) .0667(6) Uani d D 1 N H2A 1.0841 .0263 -.0489 .080 Uiso calc R 1 H H2B 1.1456 .1391 -.0813 .080 Uiso calc R 1 H C2 .7819(3) .4801(2) .12811(12) .0482(5) Uani d D 1 C O2 .7496(2) .48508(17) .06272(8) .0593(4) Uani d D 1 O N3 .8076(2) .3595(2) .14417(10) .0610(5) Uani d D 1 N H3A .8023 .2829 .1095 .073 Uiso calc R 1 H H3B .8296 .3583 .1893 .073 Uiso calc R 1 H N4 .7935(2) .5958(2) .18342(10) .0587(5) Uani d D 1 N H4A .7788 .6755 .1748 .070 Uiso calc R 1 H H4B .8157 .5912 .2279 .070 Uiso calc R 1 H C3 .5428(3) -.1820(2) .09938(12) .0518(6) Uani d D 1 C O3 .66105(19) -.15794(16) .14637(8) .0598(4) Uani d D 1 O N5 .5029(3) -.3112(2) .05539(11) .0668(6) Uani d D 1 N H5A .5594 -.3787 .0595 .080 Uiso calc R 1 H H5B .4207 -.3269 .0230 .080 Uiso calc R 1 H N6 .4510(3) -.0807(2) .09192(13) .0802(7) Uani d D 1 N H6A .4734 .0033 .1200 .096 Uiso calc R 1 H H6B .3694 -.0992 .0590 .096 Uiso calc R 1 H C4 .8915(3) .4774(2) .34632(12) .0483(5) Uani d D 1 C O4 .8560(2) .35831(18) .30353(9) .0752(6) Uani d D 1 O O5 .8868(2) .59110(18) .32875(8) .0661(5) Uani d D 1 O C5 .9462(2) .4881(2) .42630(11) .0416(5) Uani d D 1 C C6 .9891(3) .6183(2) .47560(11) .0508(6) Uani d D 1 C H6C .9820 .6991 .4595 .061 Uiso calc R 1 H C7 .9575(3) .3699(2) .45156(12) .0510(6) Uani d D 1 C H7 .9290 .2814 .4193 .061 Uiso calc R 1 H N7 .3708(2) .67174(19) .29879(9) .0488(4) Uani d D 1 N C8 .5364(3) .7504(2) .31717(12) .0518(6) Uani d D 1 C H8A .6153 .6823 .3139 .062 Uiso calc R 1 H H8B .5536 .8001 .2801 .062 Uiso calc R 1 H C9 .5672(3) .8544(3) .39183(13) .0627(7) Uani d D 1 C H9A .5534 .8065 .4299 .075 Uiso calc R 1 H H9B .4907 .9247 .3960 .075 Uiso calc R 1 H C10 .7370(3) .9250(3) .40214(15) .0677(7) Uani d D 1 C H10A .8121 .8536 .3933 .081 Uiso calc R 1 H H10B .7473 .9787 .3663 .081 Uiso calc R 1 H C11 .7790(4) 1.0211(3) .47833(17) .0883(9) Uani d D 1 C H11A .8869 1.0637 .4828 .132 Uiso calc R 1 H H11B .7709 .9679 .5139 .132 Uiso calc R 1 H H11C .7061 1.0930 .4869 .132 Uiso calc R 1 H C12 .3359(3) .5858(2) .35255(12) .0527(6) Uani d D 1 C H12A .3353 .6502 .4009 .063 Uiso calc R 1 H H12B .2285 .5384 .3380 .063 Uiso calc R 1 H C13 .4496(3) .4770(3) .35927(14) .0640(7) Uani d D 1 C H13A .5540 .5231 .3821 .077 Uiso calc R 1 H H13B .4628 .4183 .3107 .077 Uiso calc R 1 H C14 .3828(3) .3866(3) .40587(15) .0697(7) Uani d D 1 C H14A .3679 .4467 .4539 .084 Uiso calc R 1 H H14B .2783 .3414 .3826 .084 Uiso calc R 1 H C15 .4895(4) .2761(3) .41598(18) .0903(9) Uani d D 1 C H15A .4417 .2225 .4457 .136 Uiso calc R 1 H H15B .5925 .3201 .4400 .136 Uiso calc R 1 H H15C .5028 .2148 .3688 .136 Uiso calc R 1 H C16 .3691(3) .5771(3) .22132(12) .0555(6) Uani d D 1 C H16A .3910 .6359 .1888 .067 Uiso calc R 1 H H16B .4565 .5176 .2210 .067 Uiso calc R 1 H C17 .2167(3) .4846(3) .18990(14) .0742(8) Uani d D 1 C H17A .1298 .5423 .1845 .089 Uiso calc R 1 H H17B .1885 .4294 .2233 .089 Uiso calc R 1 H C18 .2381(4) .3874(3) .11571(15) .0789(8) Uani d D 1 C H18A .1334 .3422 .0928 .095 Uiso calc R 1 H H18B .2771 .4441 .0849 .095 Uiso calc R 1 H C19 .3482(4) .2767(3) .11619(18) .0984(11) Uani d D 1 C H19A .3531 .2214 .0667 .148 Uiso calc R 1 H H19B .3094 .2173 .1451 .148 Uiso calc R 1 H H19C .4536 .3196 .1371 .148 Uiso calc R 1 H C20 .2394(3) .7721(2) .30362(13) .0562(6) Uani d D 1 C H20A .1364 .7165 .2908 .067 Uiso calc R 1 H H20B .2428 .8267 .3545 .067 Uiso calc R 1 H C21 .2467(3) .8726(3) .25614(16) .0761(8) Uani d D 1 C H21A .2298 .8209 .2046 .091 Uiso calc R 1 H H21B .3517 .9251 .2653 .091 Uiso calc R 1 H C22 .1143(4) .9754(4) .2745(2) .1171(13) Uani d D 1 C H22A .0098 .9228 .2593 .176 Uiso calc R 1 H H22B .1227 1.0153 .3274 .176 Uiso calc R 1 H C23 .1241(6) 1.0900(4) .2389(3) .1418(16) Uani d D 1 C H23A .0395 1.1492 .2524 .213 Uiso calc R 1 H H23B .1131 1.0518 .1864 .213 Uiso calc R 1 H H23C .2262 1.1443 .2544 .213 Uiso calc R 1 H O1W .6301(3) .1113(3) .24613(15) .1206(9) Uani d . 1 O H1WA .6772 .0456 .2198 .181 Uiso d R 1 H H1WB .6899 .1880 .2571 .181 Uiso d 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 C1 .0520(13) .0580(14) .0435(12) .0010(11) -.0014(10) .0091(11) O1 .0621(10) .0588(10) .0630(10) .0060(8) .0136(8) .0187(8) N1 .0669(13) .0660(13) .0712(13) .0085(11) .0121(11) .0307(11) N2 .0676(13) .0675(13) .0726(14) .0124(11) .0214(11) .0265(11) C2 .0426(12) .0606(14) .0441(12) .0102(10) .0047(9) .0176(11) O2 .0765(11) .0651(10) .0368(8) .0173(8) -.0021(7) .0142(7) N3 .0797(14) .0574(12) .0462(11) .0082(10) -.0012(10) .0163(9) N4 .0732(13) .0650(12) .0390(10) .0199(10) .0022(9) .0136(9) C3 .0505(13) .0589(14) .0501(13) .0070(11) .0080(11) .0202(11) O3 .0571(10) .0614(10) .0569(9) .0069(8) -.0059(8) .0121(8) N5 .0690(13) .0671(14) .0575(12) .0081(11) -.0119(10) .0099(11) N6 .0751(15) .0698(15) .0939(17) .0186(12) -.0092(13) .0215(13) C4 .0466(12) .0563(14) .0421(11) .0042(10) .0016(9) .0147(11) O4 .1118(15) .0608(11) .0441(9) .0007(10) -.0123(9) .0066(8) O5 .0916(13) .0602(10) .0459(9) .0042(9) -.0098(8) .0194(8) C5 .0384(11) .0474(12) .0388(10) .0020(9) .0034(9) .0120(9) C6 .0628(14) .0461(13) .0448(12) .0015(11) .0001(10) .0172(10) C7 .0614(14) .0438(12) .0442(12) -.0004(10) -.0034(10) .0093(10) N7 .0436(10) .0568(11) .0453(10) .0014(8) .0060(8) .0128(8) C8 .0443(12) .0613(14) .0491(12) -.0005(11) .0077(10) .0141(11) C9 .0571(15) .0654(15) .0602(15) -.0039(12) .0070(12) .0096(12) C10 .0555(15) .0629(15) .0801(18) .0006(12) .0010(13) .0141(14) C11 .080(2) .076(2) .091(2) -.0095(16) -.0126(17) .0021(17) C12 .0498(13) .0617(14) .0483(12) -.0009(11) .0099(10) .0181(11) C13 .0592(15) .0708(16) .0689(16) .0108(13) .0128(12) .0277(13) C14 .0765(17) .0699(17) .0675(16) .0057(14) .0113(13) .0262(13) C15 .108(2) .084(2) .090(2) .0180(18) .0130(18) .0409(17) C16 .0567(14) .0647(15) .0424(12) .0030(12) .0052(10) .0104(11) C17 .0523(15) .0865(19) .0685(17) .0009(14) -.0060(12) -.0012(15) C18 .0758(18) .085(2) .0619(16) .0055(16) -.0120(14) .0011(15) C19 .117(3) .087(2) .084(2) .022(2) .0076(19) .0093(18) C20 .0480(13) .0592(14) .0622(14) .0096(11) .0073(11) .0161(12) C21 .0707(18) .0762(18) .0877(19) .0080(15) -.0003(15) .0355(16) C22 .098(3) .116(3) .171(4) .034(2) .016(2) .091(3) C23 .155(4) .116(3) .159(4) .036(3) -.010(3) .046(3) O1W .1060(18) .0903(16) .138(2) -.0045(13) .0184(15) -.0177(15) 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' O O .0106 .0060 '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_3 _geom_angle O1 C1 N2 . 121.5(2) O1 C1 N1 . 120.4(2) N2 C1 N1 . 118.0(2) O2 C2 N4 . 120.8(2) O2 C2 N3 . 121.4(2) N4 C2 N3 . 117.80(19) O3 C3 N6 . 121.2(2) O3 C3 N5 . 120.6(2) N6 C3 N5 . 118.2(2) O4 C4 O5 . 125.3(2) O4 C4 C5 . 118.2(2) O5 C4 C5 . 116.54(19) C7 C5 C6 . 118.34(19) C7 C5 C4 . 121.48(19) C6 C5 C4 . 120.17(19) C5 C6 C7 2_766 121.1(2) C5 C7 C6 2_766 120.6(2) C8 N7 C16 . 105.53(16) C8 N7 C12 . 112.06(17) C16 N7 C12 . 110.82(17) C8 N7 C20 . 111.54(17) C16 N7 C20 . 111.63(17) C12 N7 C20 . 105.40(16) C9 C8 N7 . 115.68(18) C8 C9 C10 . 109.6(2) C11 C10 C9 . 111.8(2) C13 C12 N7 . 116.72(18) C12 C13 C14 . 109.5(2) C15 C14 C13 . 113.1(2) C17 C16 N7 . 116.31(19) C16 C17 C18 . 110.2(2) C19 C18 C17 . 116.3(2) C21 C20 N7 . 116.7(2) C20 C21 C22 . 109.0(2) C23 C22 C21 . 113.8(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance C1 O1 . 1.253(3) C1 N2 . 1.331(3) C1 N1 . 1.344(3) C2 O2 . 1.257(2) C2 N4 . 1.326(3) C2 N3 . 1.332(3) C3 O3 . 1.240(3) C3 N6 . 1.333(3) C3 N5 . 1.334(3) C4 O4 . 1.245(3) C4 O5 . 1.255(3) C4 C5 . 1.517(3) C5 C7 . 1.380(3) C5 C6 . 1.383(3) C6 C7 2_766 1.384(3) C7 C6 2_766 1.384(3) N7 C8 . 1.513(3) N7 C16 . 1.518(3) N7 C12 . 1.520(3) N7 C20 . 1.525(3) C8 C9 . 1.505(3) C9 C10 . 1.518(3) C10 C11 . 1.503(4) C12 C13 . 1.507(3) C13 C14 . 1.523(3) C14 C15 . 1.498(4) C16 C17 . 1.503(3) C17 C18 . 1.513(3) C18 C19 . 1.481(4) C20 C21 . 1.505(3) C21 C22 . 1.556(4) C22 C23 . 1.462(5) 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 N1 H1A O2 . .86 2.27 3.045(3) 149.2 yes N1 H1B O2 2_765 .86 2.48 3.218(3) 144.2 yes N2 H2A O1 2_755 .86 2.11 2.951(3) 164.4 yes N2 H2B O3 2_755 .86 2.15 2.980(3) 163.4 yes N3 H3A O1 . .86 2.23 3.037(3) 156.8 yes N3 H3B O4 . .86 2.15 3.009(2) 173.4 yes N4 H4A O3 1_565 .86 2.14 2.962(3) 160.7 yes N4 H4B O5 . .86 1.95 2.805(2) 174.2 yes N5 H5A O2 1_545 .86 2.16 3.003(3) 165.4 yes N5 H5B O2 2_655 .86 2.26 3.024(2) 148.2 yes N6 H6A O1W . .86 2.55 3.219(3) 135.1 yes N6 H6B O1 2_655 .86 2.11 2.955(3) 168.8 yes O1W H1WA O3 . .85 2.12 2.879(3) 148.6 yes O1W H1WB O4 . .85 2.06 2.898(3) 167.0 yes loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139063381