#------------------------------------------------------------------------------ #$Date: 2016-03-26 00:30:19 +0100 (Sat, 26 Mar 2016) $ #$Revision: 180104 $ #$URL: svn://www.crystallography.net/cod/cif/7/10/02/7100274.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_7100274 loop_ _publ_author_name 'Carl Redshaw' 'Mark R.J. Elsegood' _publ_section_title ; Synthesis of bis(bora)calix[4]arenes bearing perfluoroaryl substituents ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/b509556e _journal_year 2005 _chemical_formula_sum 'C68 H65 B2 F18 N3 O4' _chemical_formula_weight 1351.85 _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' _cell_angle_alpha 90.00 _cell_angle_beta 107.495(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 23.8326(10) _cell_length_b 15.2792(6) _cell_length_c 19.0184(8) _cell_measurement_temperature 150(2) _cell_volume 6605.1(5) _diffrn_ambient_temperature 150(2) _exptl_crystal_density_diffrn 1.359 _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 7100274 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_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.08907(8) 1.03080(11) 0.27371(9) 0.0244(3) Uani 1 1 d . . . O1 O 0.08199(5) 0.99658(7) 0.20557(6) 0.0267(2) Uani 1 1 d . . . O2 O 0.08075(5) 0.98879(7) 0.33251(6) 0.0259(2) Uani 1 1 d . . . C1 C 0.08678(7) 0.91101(10) 0.18249(8) 0.0239(3) Uani 1 1 d . . . C2 C 0.04677(7) 0.88107(10) 0.11709(8) 0.0247(3) Uani 1 1 d . . . C3 C 0.06016(7) 0.80220(11) 0.08808(9) 0.0296(3) Uani 1 1 d . . . H3 H 0.0345 0.7825 0.0423 0.035 Uiso 1 1 calc R . . C4 C 0.10910(8) 0.75113(11) 0.12287(9) 0.0311(4) Uani 1 1 d . A . C5 C 0.14552(7) 0.78100(12) 0.19071(9) 0.0305(3) Uani 1 1 d . . . H5 H 0.1780 0.7462 0.2172 0.037 Uiso 1 1 calc R . . C6 C 0.13534(7) 0.86046(11) 0.22051(9) 0.0265(3) Uani 1 1 d . . . C7 C 0.12108(9) 0.66435(13) 0.08943(11) 0.0382(4) Uani 1 1 d DU . . C8 C 0.0851(2) 0.6570(3) 0.0082(2) 0.0527(13) Uani 0.517(4) 1 d PDU A 1 H8A H 0.0957 0.7049 -0.0196 0.079 Uiso 0.517(4) 1 calc PR A 1 H8B H 0.0431 0.6606 0.0037 0.079 Uiso 0.517(4) 1 calc PR A 1 H8C H 0.0934 0.6008 -0.0114 0.079 Uiso 0.517(4) 1 calc PR A 1 C9 C 0.1074(3) 0.5935(3) 0.1350(3) 0.0649(16) Uani 0.517(4) 1 d PDU A 1 H9A H 0.1315 0.6007 0.1864 0.097 Uiso 0.517(4) 1 calc PR A 1 H9B H 0.1159 0.5366 0.1167 0.097 Uiso 0.517(4) 1 calc PR A 1 H9C H 0.0657 0.5962 0.1321 0.097 Uiso 0.517(4) 1 calc PR A 1 C10 C 0.1864(2) 0.6633(3) 0.0927(3) 0.0574(13) Uani 0.517(4) 1 d PDU A 1 H10A H 0.1938 0.7100 0.0612 0.086 Uiso 0.517(4) 1 calc PR A 1 H10B H 0.1961 0.6066 0.0752 0.086 Uiso 0.517(4) 1 calc PR A 1 H10C H 0.2110 0.6726 0.1436 0.086 Uiso 0.517(4) 1 calc PR A 1 C8X C 0.0668(2) 0.6016(3) 0.0762(5) 0.071(2) Uani 0.483(4) 1 d PDU A 2 H8X1 H 0.0594 0.5898 0.1232 0.106 Uiso 0.483(4) 1 calc PR A 2 H8X2 H 0.0750 0.5465 0.0548 0.106 Uiso 0.483(4) 1 calc PR A 2 H8X3 H 0.0321 0.6294 0.0422 0.106 Uiso 0.483(4) 1 calc PR A 2 C9X C 0.1749(2) 0.6132(3) 0.1382(3) 0.0500(12) Uani 0.483(4) 1 d PDU A 2 H9X1 H 0.1692 0.6008 0.1862 0.075 Uiso 0.483(4) 1 calc PR A 2 H9X2 H 0.2106 0.6483 0.1454 0.075 Uiso 0.483(4) 1 calc PR A 2 H9X3 H 0.1790 0.5579 0.1140 0.075 Uiso 0.483(4) 1 calc PR A 2 C10X C 0.1322(3) 0.6818(3) 0.0161(3) 0.0533(13) Uani 0.483(4) 1 d PDU A 2 H10D H 0.1398 0.6263 -0.0053 0.080 Uiso 0.483(4) 1 calc PR A 2 H10E H 0.1664 0.7203 0.0238 0.080 Uiso 0.483(4) 1 calc PR A 2 H10F H 0.0976 0.7100 -0.0177 0.080 Uiso 0.483(4) 1 calc PR A 2 C11 C 0.17265(7) 0.88686(11) 0.29691(9) 0.0276(3) Uani 1 1 d . . . H11A H 0.1785 0.9511 0.2993 0.033 Uiso 1 1 calc R . . H11B H 0.2117 0.8584 0.3087 0.033 Uiso 1 1 calc R . . C12 C 0.09443(7) 0.90614(10) 0.36266(8) 0.0230(3) Uani 1 1 d . . . C13 C 0.14134(7) 0.85853(10) 0.35182(8) 0.0253(3) Uani 1 1 d . . . C14 C 0.15669(7) 0.77939(11) 0.38911(9) 0.0280(3) Uani 1 1 d . . . H14 H 0.1877 0.7458 0.3810 0.034 Uiso 1 1 calc R . . C15 C 0.12800(7) 0.74789(10) 0.43788(9) 0.0278(3) Uani 1 1 d . . . C16 C 0.08192(7) 0.79796(10) 0.44715(8) 0.0262(3) Uani 1 1 d . . . H16 H 0.0620 0.7777 0.4805 0.031 Uiso 1 1 calc R . . C17 C 0.06351(7) 0.87668(10) 0.40974(8) 0.0228(3) Uani 1 1 d . . . C18 C 0.14479(9) 0.66043(12) 0.47908(11) 0.0375(4) Uani 1 1 d . . . C19 C 0.1547(2) 0.6743(2) 0.56086(16) 0.1136(17) Uani 1 1 d . . . H19A H 0.1172 0.6882 0.5695 0.170 Uiso 1 1 calc R . . H19B H 0.1823 0.7228 0.5782 0.170 Uiso 1 1 calc R . . H19C H 0.1710 0.6208 0.5877 0.170 Uiso 1 1 calc R . . C20 C 0.09653(16) 0.59574(19) 0.4470(3) 0.1221(19) Uani 1 1 d . . . H20A H 0.1075 0.5387 0.4707 0.183 Uiso 1 1 calc R . . H20B H 0.0904 0.5902 0.3939 0.183 Uiso 1 1 calc R . . H20C H 0.0601 0.6160 0.4556 0.183 Uiso 1 1 calc R . . C21 C 0.20184(12) 0.62235(16) 0.47046(16) 0.0624(7) Uani 1 1 d . . . H21A H 0.2115 0.5679 0.4988 0.094 Uiso 1 1 calc R . . H21B H 0.2339 0.6646 0.4888 0.094 Uiso 1 1 calc R . . H21C H 0.1966 0.6102 0.4183 0.094 Uiso 1 1 calc R . . C22 C 0.01132(7) 0.92692(10) 0.42064(8) 0.0243(3) Uani 1 1 d . . . H22A H 0.0162 0.9323 0.4740 0.029 Uiso 1 1 calc R . . H22B H 0.0105 0.9867 0.4002 0.029 Uiso 1 1 calc R . . C23 C 0.10692(7) 1.13267(10) 0.28486(9) 0.0266(3) Uani 1 1 d . . . C24 C 0.14669(8) 1.16452(11) 0.35148(9) 0.0323(4) Uani 1 1 d . . . C25 C 0.16811(9) 1.25012(12) 0.35828(10) 0.0374(4) Uani 1 1 d . . . H25 H 0.1951 1.2690 0.4034 0.045 Uiso 1 1 calc R . . C26 C 0.15030(9) 1.30729(12) 0.29974(10) 0.0367(4) Uani 1 1 d . B . C27 C 0.10924(8) 1.28103(11) 0.23497(10) 0.0327(4) Uani 1 1 d . . . H27 H 0.0955 1.3212 0.1954 0.039 Uiso 1 1 calc R . . C28 C 0.08815(7) 1.19569(11) 0.22806(9) 0.0277(3) Uani 1 1 d . . . C29 C 0.16775(9) 1.11004(12) 0.42138(10) 0.0395(4) Uani 1 1 d . . . F1 F 0.19199(5) 1.03374(7) 0.41143(6) 0.0424(3) Uani 1 1 d . . . F2 F 0.12446(6) 1.09259(8) 0.45096(6) 0.0478(3) Uani 1 1 d . . . F3 F 0.20967(7) 1.15167(8) 0.47461(6) 0.0586(4) Uani 1 1 d . . . C30 C 0.17569(11) 1.39844(14) 0.30616(12) 0.0502(5) Uani 1 1 d DU . . F4 F 0.1831(4) 1.4328(4) 0.3694(3) 0.102(2) Uani 0.594(13) 1 d PDU B 1 F5 F 0.1446(4) 1.4517(4) 0.2589(5) 0.146(4) Uani 0.594(13) 1 d PDU B 1 F6 F 0.2290(3) 1.3961(5) 0.2996(7) 0.117(3) Uani 0.594(13) 1 d PDU B 1 F4X F 0.2060(6) 1.4175(6) 0.3723(4) 0.134(5) Uani 0.406(13) 1 d PDU B 2 F5X F 0.1339(4) 1.4576(6) 0.2893(8) 0.108(4) Uani 0.406(13) 1 d PDU B 2 F6X F 0.2041(7) 1.4149(6) 0.2611(7) 0.104(4) Uani 0.406(13) 1 d PDU B 2 C31 C 0.04211(8) 1.17511(11) 0.15604(9) 0.0319(4) Uani 1 1 d . . . F7 F 0.06372(5) 1.13485(8) 0.10702(6) 0.0422(3) Uani 1 1 d . . . F8 F -0.00124(4) 1.12500(7) 0.16505(6) 0.0347(2) Uani 1 1 d . . . F9 F 0.01618(6) 1.24828(8) 0.12205(7) 0.0531(3) Uani 1 1 d . . . N1 N 0.0000 0.5478(4) 0.2500 0.146(2) Uani 1 2 d S . . C32 C 0.0000 0.6247(4) 0.2500 0.0850(13) Uani 1 2 d S . . C33 C 0.0000 0.7196(3) 0.2500 0.0601(9) Uani 1 2 d S . . N2 N 0.22388(13) 0.8551(2) 0.69434(18) 0.1032(11) Uani 1 1 d . . . C34 C 0.20286(11) 0.9021(2) 0.64810(15) 0.0610(6) Uani 1 1 d . . . C35 C 0.17575(10) 0.96117(16) 0.58760(13) 0.0505(5) Uani 1 1 d . . . H35A H 0.2062 0.9972 0.5769 0.076 Uiso 1 1 calc R . . H35B H 0.1475 0.9990 0.6013 0.076 Uiso 1 1 calc R . . H35C H 0.1552 0.9271 0.5438 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0258(8) 0.0223(8) 0.0235(8) 0.0014(6) 0.0049(6) -0.0010(6) O1 0.0337(6) 0.0223(5) 0.0222(5) -0.0002(4) 0.0053(4) -0.0011(4) O2 0.0314(6) 0.0209(5) 0.0255(5) 0.0038(4) 0.0088(4) 0.0028(4) C1 0.0288(7) 0.0227(7) 0.0220(7) 0.0000(5) 0.0101(6) -0.0025(6) C2 0.0278(7) 0.0250(7) 0.0226(7) 0.0000(6) 0.0096(6) -0.0018(6) C3 0.0323(8) 0.0306(8) 0.0267(8) -0.0053(6) 0.0103(6) -0.0012(7) C4 0.0344(8) 0.0304(8) 0.0322(8) -0.0037(7) 0.0155(7) 0.0020(7) C5 0.0305(8) 0.0338(9) 0.0292(8) 0.0018(7) 0.0118(7) 0.0046(7) C6 0.0262(7) 0.0308(8) 0.0238(7) 0.0012(6) 0.0091(6) -0.0009(6) C7 0.0430(10) 0.0335(9) 0.0394(10) -0.0058(7) 0.0143(8) 0.0077(8) C8 0.066(3) 0.043(2) 0.043(2) -0.0157(17) 0.007(2) 0.020(2) C9 0.113(5) 0.029(2) 0.062(3) 0.0004(19) 0.041(3) 0.009(2) C10 0.056(2) 0.065(3) 0.053(3) -0.014(2) 0.019(2) 0.024(2) C8X 0.057(3) 0.036(2) 0.132(6) -0.037(3) 0.047(4) -0.013(2) C9X 0.061(3) 0.036(2) 0.052(3) -0.0042(19) 0.017(2) 0.017(2) C10X 0.068(3) 0.053(3) 0.044(2) -0.006(2) 0.025(2) 0.020(2) C11 0.0248(7) 0.0319(8) 0.0252(7) 0.0012(6) 0.0061(6) 0.0009(6) C12 0.0265(7) 0.0197(7) 0.0195(7) 0.0011(5) 0.0021(6) -0.0003(5) C13 0.0258(7) 0.0268(8) 0.0215(7) -0.0001(6) 0.0042(6) -0.0003(6) C14 0.0295(8) 0.0270(8) 0.0258(7) -0.0002(6) 0.0056(6) 0.0052(6) C15 0.0338(8) 0.0218(7) 0.0245(7) 0.0022(6) 0.0039(6) 0.0024(6) C16 0.0315(8) 0.0240(7) 0.0220(7) 0.0019(6) 0.0065(6) -0.0006(6) C17 0.0263(7) 0.0216(7) 0.0185(7) -0.0018(5) 0.0037(5) -0.0002(6) C18 0.0457(10) 0.0270(9) 0.0389(10) 0.0108(7) 0.0115(8) 0.0095(7) C19 0.206(4) 0.096(2) 0.0565(16) 0.0494(17) 0.066(2) 0.102(3) C20 0.083(2) 0.0393(15) 0.200(5) 0.052(2) -0.023(2) -0.0166(14) C21 0.0686(16) 0.0434(12) 0.0766(17) 0.0207(12) 0.0242(13) 0.0237(11) C22 0.0293(7) 0.0232(7) 0.0200(7) 0.0006(5) 0.0066(6) 0.0021(6) C23 0.0317(8) 0.0241(7) 0.0236(7) 0.0009(6) 0.0080(6) -0.0017(6) C24 0.0375(9) 0.0283(8) 0.0268(8) 0.0000(6) 0.0032(7) -0.0026(7) C25 0.0434(10) 0.0296(9) 0.0323(9) -0.0038(7) 0.0009(7) -0.0066(7) C26 0.0433(10) 0.0265(8) 0.0370(9) -0.0019(7) 0.0070(8) -0.0078(7) C27 0.0411(9) 0.0256(8) 0.0301(8) 0.0025(6) 0.0086(7) -0.0041(7) C28 0.0325(8) 0.0257(8) 0.0240(7) 0.0009(6) 0.0072(6) -0.0030(6) C29 0.0516(11) 0.0315(9) 0.0262(8) -0.0006(7) -0.0020(8) -0.0045(8) F1 0.0452(6) 0.0323(6) 0.0383(6) 0.0039(4) -0.0046(5) 0.0004(5) F2 0.0708(8) 0.0441(7) 0.0269(5) 0.0039(5) 0.0124(5) -0.0008(6) F3 0.0775(9) 0.0424(7) 0.0334(6) -0.0001(5) -0.0172(6) -0.0125(6) C30 0.0615(13) 0.0327(10) 0.0479(12) -0.0010(9) 0.0038(10) -0.0145(9) F4 0.183(6) 0.048(2) 0.099(4) -0.046(3) 0.081(4) -0.051(3) F5 0.171(6) 0.043(3) 0.141(5) 0.044(3) -0.079(5) -0.055(3) F6 0.103(4) 0.056(3) 0.229(9) -0.046(4) 0.105(5) -0.046(3) F4X 0.195(9) 0.063(5) 0.071(4) 0.027(3) -0.072(5) -0.082(5) F5X 0.086(4) 0.029(3) 0.199(11) -0.008(5) 0.025(5) 0.011(2) F6X 0.161(10) 0.046(4) 0.148(7) -0.010(4) 0.111(7) -0.041(5) C31 0.0395(9) 0.0257(8) 0.0272(8) 0.0046(6) 0.0049(7) -0.0039(7) F7 0.0536(7) 0.0493(7) 0.0239(5) -0.0035(4) 0.0119(5) -0.0128(5) F8 0.0312(5) 0.0333(5) 0.0364(5) -0.0003(4) 0.0054(4) -0.0046(4) F9 0.0626(8) 0.0312(6) 0.0461(7) 0.0112(5) -0.0133(6) -0.0028(5) N1 0.204(7) 0.092(4) 0.133(5) 0.000 0.036(5) 0.000 C32 0.105(4) 0.090(4) 0.058(2) 0.000 0.021(2) 0.000 C33 0.064(2) 0.067(2) 0.0456(17) 0.000 0.0115(16) 0.000 N2 0.0687(16) 0.136(3) 0.096(2) 0.057(2) 0.0099(15) 0.0008(17) C34 0.0431(12) 0.0792(18) 0.0569(14) 0.0131(13) 0.0093(10) -0.0063(12) C35 0.0437(11) 0.0575(13) 0.0474(12) 0.0017(10) 0.0096(9) -0.0029(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 O2 1.355(2) . ? B1 O1 1.360(2) . ? B1 C23 1.611(2) . ? O1 C1 1.3949(19) . ? O2 C12 1.3848(18) . ? C1 C2 1.397(2) . ? C1 C6 1.398(2) . ? C2 C3 1.402(2) . ? C2 C22 1.525(2) 2 ? C3 C4 1.394(2) . ? C4 C5 1.398(2) . ? C4 C7 1.534(2) . ? C5 C6 1.392(2) . ? C6 C11 1.513(2) . ? C7 C9 1.484(5) . ? C7 C10X 1.520(5) . ? C7 C8 1.528(4) . ? C7 C10 1.541(5) . ? C7 C9X 1.550(5) . ? C7 C8X 1.568(5) . ? C11 C13 1.518(2) . ? C12 C17 1.394(2) . ? C12 C13 1.400(2) . ? C13 C14 1.394(2) . ? C14 C15 1.393(2) . ? C15 C16 1.392(2) . ? C15 C18 1.540(2) . ? C16 C17 1.399(2) . ? C17 C22 1.528(2) . ? C18 C20 1.500(4) . ? C18 C19 1.516(3) . ? C18 C21 1.532(3) . ? C22 C2 1.525(2) 2 ? C23 C28 1.416(2) . ? C23 C24 1.421(2) . ? C24 C25 1.396(2) . ? C24 C29 1.520(2) . ? C25 C26 1.378(3) . ? C26 C27 1.382(3) . ? C26 C30 1.509(3) . ? C27 C28 1.389(2) . ? C28 C31 1.508(2) . ? C29 F1 1.339(2) . ? C29 F2 1.342(3) . ? C29 F3 1.349(2) . ? C30 F6X 1.266(7) . ? C30 F5 1.272(6) . ? C30 F4 1.275(5) . ? C30 F4X 1.281(6) . ? C30 F5X 1.312(7) . ? C30 F6 1.313(6) . ? C31 F8 1.338(2) . ? C31 F7 1.342(2) . ? C31 F9 1.345(2) . ? N1 C32 1.175(7) . ? C32 C33 1.450(7) . ? N2 C34 1.129(4) . ? C34 C35 1.452(3) . ?