#------------------------------------------------------------------------------ #$Date: 2008-01-26 15:05:32 +0200 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2013127.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2013127 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2003 _journal_volume 59 _journal_page_first m16 _journal_page_last m17 _publ_section_title ; [7,13-bis(2-aminobenzyl)-1,4,10-trioxa- 7,13-diazacyclopentadecane]diisothiocyanatobarium(II) ; loop_ _publ_author_name 'Avecilla, Fernando' 'Esteban, David' 'Platas-Iglesias, Carlos' 'De Blas, Andres' 'Rodr\'iguez-Blas, Teresa' _chemical_formula_moiety 'C26 H36 Ba N6 O3 S2' _chemical_formula_sum 'C26 H36 Ba N6 O3 S2' _chemical_formula_iupac '[Ba (C24 H36 N4 O3) (N C S)2]' _chemical_formula_weight 682.07 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.4878(2) _cell_length_b 12.2591(2) _cell_length_c 11.9750(3) _cell_angle_alpha 90 _cell_angle_beta 95.0290(10) _cell_angle_gamma 90 _cell_volume 1533.71(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _exptl_crystal_density_diffrn 1.477 _diffrn_ambient_temperature 298(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 Ba1 0.30229(4) 0.52484(4) 0.68663(3) 0.03547(12) Uani d DU 1 . . Ba S1S 0.6349(3) 0.6227(3) 0.3902(3) 0.0919(11) Uani d . 1 A . S O1 0.1370(6) 0.6189(5) 0.8216(5) 0.0526(16) Uani d . 1 A . O N1SA 0.519(3) 0.530(3) 0.568(3) 0.090(8) Uani d PDU 0.66(8) A 1 N N1SB 0.477(5) 0.513(3) 0.526(5) 0.073(10) Uani d PDU 0.34(8) A 2 N C1S 0.5540(10) 0.5660(7) 0.4809(11) 0.071(3) Uani d DU 1 . . C N1 0.2146(8) 0.3717(6) 0.5147(8) 0.044(2) Uani d . 1 A . N H1C 0.1631 0.3534 0.5701 0.053 Uiso d R 1 . . H H1D 0.2229 0.2927 0.4923 0.053 Uiso d R 1 . . H C1 0.1862(10) 0.6691(8) 0.9246(8) 0.066(3) Uani d . 1 . . C H1A 0.1169 0.6843 0.9710 0.079 Uiso calc R 1 A . H H1B 0.2282 0.7374 0.9095 0.079 Uiso calc R 1 . . H O2 0.4271(10) 0.7202(8) 0.7456(7) 0.094(4) Uani d . 1 A . O N2 0.4378(8) 0.3381(7) 0.7918(7) 0.042(2) Uani d . 1 A . N H2C 0.4405 0.2778 0.7287 0.050 Uiso d R 1 . . H H2D 0.3868 0.3099 0.8537 0.050 Uiso d R 1 . . H S2S 0.1675(3) 0.2467(3) 0.9475(2) 0.0767(9) Uani d . 1 A . S C2S 0.1387(8) 0.3094(7) 0.8264(8) 0.044(2) Uani d . 1 . . C N2S 0.1225(8) 0.3524(7) 0.7429(7) 0.061(2) Uani d . 1 A . N C2 0.2809(9) 0.5911(8) 0.9845(7) 0.059(3) Uani d . 1 A . C H2A 0.3059 0.6199 1.0586 0.070 Uiso calc R 1 . . H H2B 0.2381 0.5220 0.9941 0.070 Uiso calc R 1 . . H N3 0.3981(8) 0.5705(5) 0.9273(6) 0.047(2) Uani d . 1 A . N O3 0.2743(8) 0.7114(6) 0.5562(8) 0.097(3) Uani d . 1 A . O C3 0.4817(10) 0.6715(7) 0.9351(8) 0.057(3) Uani d . 1 . . C H3A 0.4330 0.7322 0.9612 0.069 Uiso calc R 1 A . H H3B 0.5541 0.6590 0.9897 0.069 Uiso calc R 1 . . H N4 0.0412(6) 0.5855(5) 0.5831(6) 0.0385(17) Uani d . 1 A . N C4 0.5296(14) 0.7007(12) 0.8252(13) 0.075(5) Uani d . 1 A . C H4A 0.5828 0.7655 0.8340 0.090 Uiso calc R 1 . . H H4B 0.5816 0.6417 0.8000 0.090 Uiso calc R 1 . . H C5 0.4316(12) 0.8004(9) 0.6673(13) 0.100(5) Uani d . 1 . . C H5A 0.5082 0.7898 0.6287 0.120 Uiso calc R 1 A . H H5B 0.4404 0.8698 0.7061 0.120 Uiso calc R 1 . . H C6 0.3252(14) 0.8078(8) 0.5853(10) 0.091(4) Uani d . 1 A . C H6A 0.2600 0.8531 0.6144 0.109 Uiso calc R 1 . . H H6B 0.3525 0.8432 0.5190 0.109 Uiso calc R 1 . . H C7 0.1745(11) 0.7041(9) 0.4733(11) 0.060(4) Uani d . 1 . . C H7A 0.1912 0.6438 0.4242 0.072 Uiso calc R 1 A . H H7B 0.1725 0.7704 0.4289 0.072 Uiso calc R 1 . . H C8 0.0465(9) 0.6880(7) 0.5154(8) 0.046(2) Uani d . 1 A . C H8A -0.0179 0.6846 0.4522 0.055 Uiso calc R 1 . . H H8B 0.0270 0.7499 0.5613 0.055 Uiso calc R 1 . . H C9 -0.0358(8) 0.6026(8) 0.6794(8) 0.053(3) Uani d . 1 . . C H9A -0.0532 0.5320 0.7114 0.064 Uiso calc R 1 A . H H9B -0.1174 0.6341 0.6517 0.064 Uiso calc R 1 . . H C10 0.0235(10) 0.6745(8) 0.7714(8) 0.059(3) Uani d . 1 A . C H10A 0.0466 0.7444 0.7411 0.071 Uiso calc R 1 . . H H10B -0.0365 0.6869 0.8272 0.071 Uiso calc R 1 . . H C11 -0.0242(8) 0.4961(6) 0.5132(7) 0.045(3) Uani d . 1 . . C H11A -0.1123 0.5172 0.4929 0.054 Uiso calc R 1 A . H H11B -0.0252 0.4303 0.5582 0.054 Uiso calc R 1 . . H C12 0.0399(9) 0.4709(7) 0.4063(7) 0.046(2) Uani d . 1 A . C C13 -0.0167(10) 0.5113(14) 0.3050(8) 0.073(3) Uani d . 1 . . C H13 -0.0912 0.5527 0.3024 0.087 Uiso calc R 1 A . H C14 0.0419(15) 0.4879(10) 0.2084(10) 0.097(5) Uani d . 1 A . C H14 0.0068 0.5146 0.1398 0.116 Uiso calc R 1 . . H C15 0.1508(13) 0.4257(11) 0.2130(10) 0.087(4) Uani d . 1 . . C H15 0.1871 0.4083 0.1472 0.104 Uiso calc R 1 A . H C16 0.2064(10) 0.3892(8) 0.3130(9) 0.067(3) Uani d . 1 A . C H16 0.2826 0.3502 0.3150 0.080 Uiso calc R 1 . . H C17 0.1517(9) 0.4092(7) 0.4106(8) 0.045(2) Uani d . 1 . . C C18 0.4672(10) 0.4792(7) 0.9861(8) 0.051(3) Uani d . 1 . . C H18A 0.4077 0.4196 0.9933 0.062 Uiso calc R 1 A . H H18B 0.4973 0.5030 1.0611 0.062 Uiso calc R 1 . . H C19 0.5802(9) 0.4374(7) 0.9282(7) 0.047(2) Uani d . 1 A . C C20 0.7049(11) 0.4644(8) 0.9691(9) 0.065(3) Uani d . 1 . . C H20 0.7176 0.5089 1.0320 0.078 Uiso calc R 1 A . H C21 0.8086(10) 0.4271(10) 0.9193(10) 0.071(3) Uani d . 1 A . C H21 0.8907 0.4457 0.9487 0.085 Uiso calc R 1 . . H C22 0.7917(10) 0.3624(10) 0.8262(10) 0.075(3) Uani d . 1 . . C H22 0.8622 0.3394 0.7904 0.090 Uiso calc R 1 A . H C23 0.6688(9) 0.3310(8) 0.7849(8) 0.054(3) Uani d . 1 A . C H23 0.6568 0.2854 0.7228 0.064 Uiso calc R 1 . . H C24 0.5633(12) 0.3690(10) 0.8381(11) 0.040(3) Uani d . 1 . . C 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 Ba1 0.0388(2) 0.0302(2) 0.0380(2) -0.0017(5) 0.00632(15) 0.0000(5) S1S 0.081(2) 0.071(2) 0.128(3) 0.0080(17) 0.031(2) 0.045(2) O1 0.057(4) 0.046(4) 0.056(4) 0.011(3) 0.015(3) -0.017(3) N1SA 0.097(13) 0.063(12) 0.121(14) -0.002(16) 0.065(12) -0.021(15) N1SB 0.069(18) 0.050(17) 0.106(19) -0.035(15) 0.048(15) -0.043(16) C1S 0.060(7) 0.033(6) 0.128(9) -0.001(4) 0.047(6) 0.001(5) N1 0.048(6) 0.032(5) 0.054(6) -0.006(4) 0.006(5) -0.009(4) C1 0.073(8) 0.076(8) 0.050(6) 0.008(6) 0.023(6) -0.019(6) O2 0.122(8) 0.093(7) 0.063(6) -0.059(6) -0.023(6) 0.025(5) N2 0.045(6) 0.035(5) 0.045(6) 0.005(4) 0.008(4) 0.003(4) S2S 0.075(2) 0.098(2) 0.0565(18) -0.0038(17) -0.0001(15) 0.0260(16) C2S 0.029(5) 0.051(6) 0.052(6) 0.000(4) 0.009(4) -0.006(5) N2S 0.062(6) 0.065(6) 0.057(6) -0.008(5) 0.003(5) 0.025(5) C2 0.071(8) 0.067(7) 0.040(6) 0.002(5) 0.010(5) -0.012(5) N3 0.062(6) 0.045(5) 0.036(5) -0.007(4) 0.005(4) -0.011(3) O3 0.075(6) 0.056(6) 0.152(9) -0.033(4) -0.043(6) 0.048(6) C3 0.063(8) 0.036(6) 0.072(7) -0.013(5) 0.000(6) -0.009(5) N4 0.036(4) 0.037(4) 0.044(4) 0.004(3) 0.008(3) 0.004(3) C4 0.070(11) 0.071(10) 0.084(11) -0.029(9) 0.005(9) -0.003(8) C5 0.091(10) 0.048(8) 0.163(14) -0.028(7) 0.015(10) 0.021(8) C6 0.154(14) 0.029(7) 0.089(9) -0.015(7) 0.006(9) 0.009(6) C7 0.047(7) 0.038(7) 0.095(11) 0.003(5) 0.010(7) 0.024(6) C8 0.050(6) 0.033(5) 0.054(6) 0.013(4) 0.003(5) 0.005(4) C9 0.031(6) 0.060(7) 0.070(7) 0.011(5) 0.014(5) -0.001(5) C10 0.051(7) 0.060(7) 0.068(7) 0.013(5) 0.013(6) -0.011(5) C11 0.034(5) 0.045(8) 0.056(6) -0.001(4) 0.003(4) 0.002(4) C12 0.050(6) 0.045(6) 0.043(5) -0.007(4) 0.003(5) 0.006(4) C13 0.090(7) 0.069(9) 0.056(6) 0.005(8) -0.010(5) -0.004(8) C14 0.143(13) 0.095(14) 0.050(7) -0.025(9) -0.006(7) 0.001(6) C15 0.115(12) 0.100(11) 0.050(8) -0.030(9) 0.032(8) -0.014(7) C16 0.071(7) 0.082(8) 0.050(6) -0.018(6) 0.020(5) -0.006(6) C17 0.048(6) 0.029(5) 0.059(7) -0.013(4) 0.008(5) -0.012(5) C18 0.072(8) 0.044(6) 0.037(6) -0.003(5) 0.000(5) 0.007(4) C19 0.052(7) 0.043(6) 0.045(6) -0.012(5) 0.006(5) 0.002(4) C20 0.074(9) 0.057(7) 0.061(7) -0.008(6) -0.014(6) 0.001(5) C21 0.049(8) 0.083(9) 0.077(8) -0.016(6) -0.018(6) 0.020(7) C22 0.043(7) 0.099(9) 0.083(9) 0.000(6) 0.014(6) 0.026(7) C23 0.049(7) 0.053(6) 0.060(7) 0.006(5) 0.014(5) 0.009(5) C24 0.038(7) 0.036(6) 0.043(7) 0.002(5) -0.008(5) 0.006(5) 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 Ba1 O1 . 2.727(5) yes Ba1 O3 . 2.771(7) yes Ba1 N1SB . 2.776(15) yes Ba1 N1SA . 2.788(11) yes Ba1 O2 . 2.790(9) yes Ba1 N1 . 2.877(8) yes Ba1 N2 . 2.921(8) yes Ba1 N2S . 2.950(8) yes Ba1 N4 . 2.999(7) yes Ba1 N3 . 3.020(7) yes S1S C1S . 1.596(10) ? O1 C1 . 1.434(10) ? O1 C10 . 1.455(11) ? N1SA C1S . 1.215(17) ? N1SB C1S . 1.202(18) ? N1 C17 . 1.433(12) ? N1 N2 . 3.911(12) ? N1 H1C . 0.9185 ? N1 H1D . 1.0115 ? C1 C2 . 1.513(13) ? C1 H1A . 0.9700 ? C1 H1B . 0.9700 ? O2 C5 . 1.362(13) ? O2 C4 . 1.393(15) ? N2 C24 . 1.434(13) ? N2 H2C . 1.0594 ? N2 H2D . 1.0111 ? S2S C2S . 1.646(10) ? C2S N2S . 1.130(10) ? C2 N3 . 1.480(11) ? C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? N3 C18 . 1.478(10) ? N3 C3 . 1.516(11) ? N3 N4 . 5.322(10) ? O3 C6 . 1.330(12) ? O3 C7 . 1.381(13) ? C3 C4 . 1.493(16) ? C3 H3A . 0.9700 ? C3 H3B . 0.9700 ? N4 C9 . 1.480(10) ? N4 C8 . 1.499(10) ? N4 C11 . 1.506(9) ? C4 H4A . 0.9700 ? C4 H4B . 0.9700 ? C5 C6 . 1.423(15) ? C5 H5A . 0.9700 ? C5 H5B . 0.9700 ? C6 H6A . 0.9700 ? C6 H6B . 0.9700 ? C7 C8 . 1.488(13) ? C7 H7A . 0.9700 ? C7 H7B . 0.9700 ? C8 H8A . 0.9700 ? C8 H8B . 0.9700 ? C9 C10 . 1.502(12) ? C9 H9A . 0.9700 ? C9 H9B . 0.9700 ? C10 H10A . 0.9700 ? C10 H10B . 0.9700 ? C11 C12 . 1.529(11) ? C11 H11A . 0.9700 ? C11 H11B . 0.9700 ? C12 C17 . 1.393(12) ? C12 C13 . 1.394(12) ? C13 C14 . 1.387(14) ? C13 H13 . 0.9300 ? C14 C15 . 1.371(16) ? C14 H14 . 0.9300 ? C15 C16 . 1.360(15) ? C15 H15 . 0.9300 ? C16 C17 . 1.369(12) ? C16 H16 . 0.9300 ? C18 C19 . 1.514(13) ? C18 H18A . 0.9700 ? C18 H18B . 0.9700 ? C19 C24 . 1.366(15) ? C19 C20 . 1.395(13) ? C20 C21 . 1.364(14) ? C20 H20 . 0.9300 ? C21 C22 . 1.367(14) ? C21 H21 . 0.9300 ? C22 C23 . 1.394(13) ? C22 H22 . 0.9300 ? C23 C24 . 1.404(15) ? C23 H23 . 0.9300 ?