#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003446.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_2003446 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 894 _journal_page_last 904 _publ_section_title ; Octaanisyl Cavitands and a Related Caviplex ; _chemical_formula_moiety 'C64 H64 O8, C2 H5 OH' _chemical_formula_sum 'C66 H70 O9' _chemical_formula_structural 'C64 H64 O8, C2 H5 OH' _chemical_formula_weight 1007 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '1/2+x,1/2-y,1/2+z' '1/2-x,1/2+y,1/2-z' _symmetry_space_group_name_H-M 'P 21/n' _cell_length_a 14.117(6) _cell_length_b 27.796(9) _cell_length_c 14.845(4) _cell_angle_alpha 90.0 _cell_angle_beta 94.29(3) _cell_angle_gamma 90.0 _cell_volume 5809(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _cell_measurement_reflns_used 15 _cell_measurement_theta_min 50 _cell_measurement_theta_max 70 _exptl_absorpt_coefficient_mu 0.53 _cell_measurement_temperature 115 _exptl_crystal_description 'clear, chunky' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_size_rad ? _exptl_crystal_colour colorless _chemical_compound_source 'Cram et al. (1987)' _diffrn_measurement_device 'Syntex P\=1 diffractometer' _diffrn_measurement_method \q/2\q _exptl_absorpt_correction_type 'none' _diffrn_reflns_number 11032 _reflns_number_total 8217 _reflns_number_observed 7590 _reflns_observed_criterion 'F > 3 sigma(F)' _diffrn_reflns_av_R_equivalents 0.05 _diffrn_reflns_theta_max 75 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.082 _refine_ls_wR_factor_obs 0.085 _refine_ls_wR_factor_all 0.088 _refine_ls_goodness_of_fit_obs 3.53 _refine_ls_goodness_of_fit_all 3.48 _refine_ls_number_reflns 8209 _refine_ls_number_parameters 733 _refine_ls_hydrogen_treatment ; H riding on attached C, or as part of rigid CH~3~ group, C-H 1.08\%A, fixed ; _refine_ls_weighting_scheme 'sigma' _refine_ls_shift/esd_max 1.1 _refine_diff_density_max 1.0 _refine_diff_density_min -0.32 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C ? International_Tables_Vol_IV_Table_2.2B ? ? H ? International_Tables_Vol_IV_Table_2.2B ? ? O ? International_Tables_Vol_IV_Table_2.2B ? ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv C1 0.35106(28) 0.14875(11) 0.04031(23) 0.0253(9) C2 0.41951(31) 0.12470(11) -0.00584(26) 0.0326(10) C3 0.47750(31) 0.14870(11) -0.06359(27) 0.0341(10) C4 0.54827(40) 0.12244(14) -0.11731(38) 0.0592(14) C5 0.46794(29) 0.19912(11) -0.07193(24) 0.0285(10) C6 0.40161(29) 0.22419(11) -0.02524(23) 0.0263(9) C7 0.34126(29) 0.19863(11) 0.02806(24) 0.0262(9) O8 0.27075(20) 0.22273(8) 0.07000(16) 0.0302(7) C9 0.18888(32) 0.23218(12) 0.00888(26) 0.0374(11) C10 0.39377(29) 0.27770(10) -0.03219(23) 0.0281(9) C11 0.36519(35) 0.29926(11) -0.11401(25) 0.0385(12) C12 0.35331(42) 0.34946(12) -0.12122(27) 0.0482(15) C13 0.31972(64) 0.37216(15) -0.21006(32) 0.0889(29) C14 0.36892(37) 0.37658(11) -0.04351(25) 0.0410(13) C15 0.40106(31) 0.35633(10) 0.04005(24) 0.0309(10) C16 0.41498(28) 0.30619(10) 0.04433(23) 0.0272(9) O17 0.45098(20) 0.28493(7) 0.12405(16) 0.0294(7) C18 0.55113(35) 0.28057(20) 0.12830(33) 0.0543(15) C19 0.42374(31) 0.38828(10) 0.11949(23) 0.0302(10) C20 0.48196(30) 0.42841(10) 0.10886(24) 0.0313(10) C21 0.50726(31) 0.45999(10) 0.18043(25) 0.0312(10) C22 0.56886(35) 0.50380(11) 0.16657(28) 0.0420(12) C23 0.47377(29) 0.45032(10) 0.26419(24) 0.0279(9) C24 0.41423(28) 0.41088(9) 0.27788(23) 0.0251(9) C25 0.38795(29) 0.38049(10) 0.20408(24) 0.0274(9) O26 0.32746(21) 0.34258(7) 0.21846(17) 0.0302(7) C27 0.23261(37) 0.34989(16) 0.18316(35) 0.0524(14) C28 0.37470(29) 0.40322(10) 0.36732(23) 0.0249(9) C29 0.30806(30) 0.43543(10) 0.39703(25) 0.0301(10) C30 0.27004(32) 0.43020(11) 0.48070(25) 0.0335(10) C31 0.20073(39) 0.46709(13) 0.51343(30) 0.0497(13) C32 0.29843(30) 0.39053(11) 0.53394(24) 0.0310(10) C33 0.36696(29) 0.35814(10) 0.50712(23) 0.0266(9) C34 0.40625(28) 0.36522(9) 0.42393(23) 0.0247(9) O35 0.48348(20) 0.33878(7) 0.39990(17) 0.0310(7) C36 0.46566(32) 0.28969(11) 0.37167(26) 0.0341(10) C37 0.40119(29) 0.31857(10) 0.56898(22) 0.0261(10) C38 0.49105(30) 0.32200(10) 0.61621(22) 0.0287(10) C39 0.52614(28) 0.28638(10) 0.67493(22) 0.0261(9) C40 0.62255(31) 0.29120(12) 0.72673(25) 0.0332(11) C41 0.47129(29) 0.24494(10) 0.68412(22) 0.0262(10) C42 0.38197(30) 0.23992(10) 0.63657(23) 0.0270(10) C43 0.34610(28) 0.27763(10) 0.58228(23) 0.0261(10) O44 0.25206(21) 0.27450(8) 0.54621(17) 0.0327(8) C45 0.23676(33) 0.26478(12) 0.45236(25) 0.0348(11) C46 0.33088(28) 0.19293(10) 0.64139(24) 0.0250(9) C47 0.28557(30) 0.17910(11) 0.71792(25) 0.0303(10) C48 0.24344(32) 0.13386(12) 0.72321(25) 0.0337(11) C49 0.19570(39) 0.11892(15) 0.80730(28) 0.0502(14) C50 0.24577(32) 0.10274(11) 0.64879(24) 0.0332(10) C51 0.28976(29) 0.11564(10) 0.57097(23) 0.0270(9) C52 0.33414(29) 0.16096(10) 0.56884(23) 0.0257(9) O53 0.38366(19) 0.17444(7) 0.49589(16) 0.0270(6) C54 0.47896(31) 0.15644(12) 0.49991(29) 0.0382(11) C55 0.29586(29) 0.08218(10) 0.49380(23) 0.0269(9) C56 0.33596(32) 0.03616(11) 0.50809(26) 0.0323(10) C57 0.34820(32) 0.00527(11) 0.43587(25) 0.0325(10) C58 0.39156(40) -0.04421(12) 0.45350(29) 0.0465(14) C59 0.32216(30) 0.02095(10) 0.34824(24) 0.0305(10) C60 0.28066(28) 0.06619(10) 0.33226(23) 0.0264(9) C61 0.26529(28) 0.09560(10) 0.40586(24) 0.0266(9) O62 0.21596(19) 0.13879(7) 0.39135(16) 0.0281(7) C63 0.11938(32) 0.13506(12) 0.41444(28) 0.0388(11) C64 0.25233(28) 0.08098(9) 0.23688(23) 0.0257(9) C65 0.17026(27) 0.06165(9) 0.19321(22) 0.0249(9) C66 0.14397(28) 0.07143(9) 0.10267(23) 0.0249(9) C67 0.05654(30) 0.04913(11) 0.05501(25) 0.0319(10) C68 0.20268(28) 0.10098(10) 0.05535(23) 0.0275(10) C69 0.28666(28) 0.12071(9) 0.09697(22) 0.0265(9) C70 0.30969(29) 0.11100(10) 0.18787(24) 0.0282(9) O71 0.39499(22) 0.12803(9) 0.22909(18) 0.0375(8) C72 0.38981(41) 0.17743(13) 0.26021(30) 0.0500(14) O73* 0.0816(6) 0.4142(3) 0.7032(5) 0.073(3) C74* 0.0762(10) 0.4516(4) 0.7594(8) 0.067(3) C75* 0.0319(11) 0.4940(4) 0.7122(9) 0.064(3) O76** 0.1464(10) 0.4746(4) 0.7621(8) 0.089(4) C77** 0.0780(16) 0.5076(6) 0.7307(13) 0.074(5) C78** -0.0036(16) 0.4861(6) 0.6691(14) 0.063(4) O79*** 0.0519(13) 0.4349(6) 0.8093(11) 0.070(4) C80*** 0.0592(15) 0.3864(6) 0.8139(13) 0.053(4) C81*** 0.1206(24) 0.3477(11) 0.7807(21) 0.114(9) H2 0.4277 0.0863 0.0032 0.100 H4A 0.5422 0.0865 -0.0908 0.100 H4B 0.6164 0.1374 -0.0941 0.100 H4C 0.5422 0.1211 -0.1902 0.100 H5 0.5128 0.2186 -0.1152 0.100 H9A 0.1396 0.2527 0.0461 0.100 H9B 0.1571 0.1982 -0.0115 0.100 H9C 0.2057 0.2520 -0.0503 0.100 H11 0.3517 0.2771 -0.1733 0.100 H13A 0.2915 0.4081 -0.2070 0.100 H13B 0.2622 0.3471 -0.2248 0.100 H13C 0.3684 0.3704 -0.2626 0.100 H14 0.3559 0.4148 -0.0471 0.100 H18A 0.5674 0.2650 0.1943 0.100 H18B 0.5830 0.3158 0.1260 0.100 H18C 0.5791 0.2578 0.0777 0.100 H20 0.5082 0.4352 0.0435 0.100 H22A 0.6191 0.5067 0.2246 0.100 H22B 0.5177 0.5326 0.1680 0.100 H22C 0.6061 0.5063 0.1056 0.100 H23 0.4942 0.4737 0.3204 0.100 H27A 0.1990 0.3156 0.1927 0.100 H27B 0.2261 0.3590 0.1123 0.100 H27C 0.1984 0.3772 0.2211 0.100 H29 0.2851 0.4652 0.3541 0.100 H31A 0.1509 0.4500 0.5545 0.100 H31B 0.1625 0.4872 0.4600 0.100 H31C 0.2455 0.4911 0.5552 0.100 H32 0.2670 0.3848 0.5972 0.100 H36A 0.5334 0.2753 0.3554 0.100 H36B 0.4155 0.2870 0.3133 0.100 H36C 0.4397 0.2695 0.4268 0.100 H38 0.5341 0.3534 0.6064 0.100 H40A 0.6311 0.3298 0.7258 0.100 H40B 0.6820 0.2744 0.6971 0.100 H40C 0.6197 0.2792 0.7956 0.100 H41 0.4981 0.2164 0.7284 0.100 H45A 0.1604 0.2645 0.4402 0.100 H45B 0.2652 0.2311 0.4301 0.100 H45C 0.2659 0.2941 0.4154 0.100 H47 0.2831 0.2039 0.7738 0.100 H49A 0.1947 0.0808 0.8209 0.100 H49B 0.1237 0.1321 0.7975 0.100 H49C 0.2322 0.1374 0.8637 0.100 H50 0.2126 0.0678 0.6518 0.100 H54A 0.5103 0.1731 0.4436 0.100 H54B 0.4736 0.1181 0.4886 0.100 H54C 0.5229 0.1634 0.5612 0.100 H56 0.3575 0.0246 0.5760 0.100 H58A 0.4179 -0.0602 0.3938 0.100 H58B 0.3337 -0.0655 0.4752 0.100 H58C 0.4480 -0.0428 0.5068 0.100 H59 0.3341 -0.0022 0.2918 0.100 H63A 0.0905 0.1710 0.4146 0.100 H63B 0.1108 0.1183 0.4788 0.100 H63C 0.0823 0.1143 0.3611 0.100 H65 0.1258 0.0385 0.2305 0.100 H67A 0.0376 0.0652 -0.0102 0.100 H67B -0.0039 0.0502 0.0953 0.100 H67C 0.0777 0.0122 0.0460 0.100 H68 0.1832 0.1089 -0.0148 0.100 H72A 0.4638 0.1852 0.2782 0.100 H72B 0.3499 0.1817 0.3189 0.100 H72C 0.3628 0.2019 0.2080 0.100 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 C1 0.0258(24) -0.0050(13) -0.0089(16) 0.0246(13) 0.0046(11) 0.0239(19) C2 0.0337(27) -0.0010(15) -0.0046(19) 0.0269(13) 0.0049(13) 0.0361(22) C3 0.0330(27) 0.0006(14) 0.0026(20) 0.0256(13) 0.0024(14) 0.0437(24) C4 0.0630(38) 0.0081(20) 0.0327(30) 0.0360(16) 0.0025(19) 0.0826(36) C5 0.0319(25) -0.0048(14) -0.0025(17) 0.0269(13) 0.0021(12) 0.0260(19) C6 0.0330(25) -0.0048(14) -0.0076(17) 0.0227(12) 0.0001(12) 0.0217(19) C7 0.0290(24) -0.0029(14) -0.0040(17) 0.0246(12) 0.0007(12) 0.0242(19) O8 0.0342(18) 0.0003(11) -0.0018(12) 0.0298(9) 0.0017(9) 0.0260(14) C9 0.0413(29) 0.0025(17) -0.0005(20) 0.0396(15) 0.0084(15) 0.0307(22) C10 0.0375(25) -0.0058(14) 0.0007(17) 0.0209(12) 0.0004(11) 0.0257(19) C11 0.0679(34) -0.0063(17) -0.0017(20) 0.0247(14) -0.0005(13) 0.0220(20) C12 0.0922(42) 0.0002(20) -0.0069(23) 0.0244(14) 0.0030(13) 0.0263(22) C13 0.2009(85) 0.0065(32) -0.0272(37) 0.0354(17) 0.0030(17) 0.0250(27) C14 0.0728(36) -0.0017(17) -0.0022(21) 0.0254(12) 0.0019(12) 0.0240(21) C15 0.0461(27) -0.0035(14) 0.0012(18) 0.0226(12) 0.0009(11) 0.0238(19) C16 0.0349(25) -0.0025(14) -0.0036(17) 0.0233(12) 0.0033(12) 0.0223(18) O17 0.0381(18) -0.0025(10) -0.0031(11) 0.0272(9) 0.0029(8) 0.0222(13) C18 0.0367(32) -0.0018(26) -0.0035(23) 0.0819(32) 0.0093(23) 0.0433(28) C19 0.0455(27) -0.0014(14) 0.0004(18) 0.0231(11) 0.0005(11) 0.0216(19) C20 0.0433(27) -0.0010(14) 0.0053(18) 0.0223(11) 0.0020(11) 0.0287(19) C21 0.0401(26) 0.0002(14) 0.0031(19) 0.0195(11) 0.0038(12) 0.0339(21) C22 0.0564(32) -0.0072(16) 0.0147(22) 0.0235(12) 0.0010(14) 0.0476(25) C23 0.0334(25) 0.0002(13) -0.0004(18) 0.0201(11) -0.0024(11) 0.0298(20) C24 0.0334(24) 0.0026(13) -0.0014(16) 0.0205(10) 0.0026(11) 0.0208(18) C25 0.0332(24) -0.0012(13) -0.0020(17) 0.0201(11) 0.0032(11) 0.0283(20) O26 0.0332(19) -0.0066(10) -0.0057(12) 0.0254(9) 0.0029(9) 0.0308(14) C27 0.0390(34) -0.0053(22) -0.0026(25) 0.0565(22) 0.0172(22) 0.0608(32) C28 0.0313(24) -0.0016(13) -0.0047(16) 0.0226(11) -0.0010(11) 0.0198(18) C29 0.0383(27) 0.0038(14) -0.0018(18) 0.0244(11) 0.0023(12) 0.0269(20) C30 0.0429(28) 0.0067(15) 0.0036(19) 0.0288(13) -0.0003(13) 0.0290(20) C31 0.0677(36) 0.0220(20) 0.0191(24) 0.0387(16) 0.0037(16) 0.0449(25) C32 0.0386(27) 0.0022(15) 0.0016(18) 0.0294(12) 0.0003(12) 0.0248(19) C33 0.0345(25) 0.0010(13) -0.0049(17) 0.0239(11) 0.0009(11) 0.0203(18) C34 0.0304(24) 0.0003(13) -0.0043(16) 0.0209(10) 0.0004(11) 0.0217(18) O35 0.0361(18) 0.0034(10) 0.0022(12) 0.0237(9) 0.0023(9) 0.0333(14) C36 0.0426(27) 0.0065(15) 0.0012(19) 0.0241(12) -0.0043(13) 0.0354(22) C37 0.0341(26) -0.0014(13) -0.0020(17) 0.0221(11) 0.0011(11) 0.0214(18) C38 0.0404(28) -0.0026(14) -0.0010(18) 0.0254(12) -0.0013(11) 0.0198(18) C39 0.0308(24) -0.0021(14) -0.0049(16) 0.0258(12) -0.0019(11) 0.0207(18) C40 0.0383(28) -0.0063(16) -0.0098(18) 0.0356(14) -0.0015(13) 0.0238(20) C41 0.0349(27) 0.0008(14) -0.0057(17) 0.0236(11) -0.0002(11) 0.0190(17) C42 0.0379(27) -0.0028(14) -0.0018(18) 0.0202(11) -0.0007(11) 0.0222(18) C43 0.0291(26) -0.0005(14) -0.0047(17) 0.0266(12) 0.0025(12) 0.0215(18) O44 0.0342(20) -0.0013(11) -0.0075(12) 0.0355(10) 0.0022(10) 0.0269(14) C45 0.0408(28) 0.0017(16) -0.0110(19) 0.0328(13) 0.0009(13) 0.0288(21) C46 0.0246(23) -0.0026(13) -0.0082(16) 0.0237(12) 0.0040(12) 0.0252(19) C47 0.0326(26) -0.0068(15) -0.0052(17) 0.0307(13) -0.0006(13) 0.0264(20) C48 0.0410(28) -0.0121(17) -0.0051(18) 0.0345(15) 0.0026(13) 0.0245(20) C49 0.0689(38) -0.0293(23) 0.0057(23) 0.0526(19) -0.0029(17) 0.0293(24) C50 0.0455(28) -0.0103(16) -0.0057(18) 0.0294(13) 0.0050(12) 0.0233(20) C51 0.0328(25) -0.0025(14) -0.0091(17) 0.0240(12) 0.0036(12) 0.0226(19) C52 0.0304(24) -0.0028(14) -0.0062(16) 0.0238(12) 0.0036(11) 0.0215(19) O53 0.0308(17) 0.0006(10) -0.0018(11) 0.0254(8) 0.0019(8) 0.0241(13) C54 0.0316(27) 0.0040(16) -0.0003(20) 0.0367(15) 0.0021(15) 0.0459(24) C55 0.0356(25) -0.0031(13) -0.0076(17) 0.0215(11) 0.0024(11) 0.0223(19) C56 0.0428(28) -0.0004(15) -0.0125(18) 0.0229(12) 0.0041(12) 0.0289(21) C57 0.0429(28) -0.0006(14) -0.0106(19) 0.0216(12) 0.0025(12) 0.0310(21) C58 0.0760(39) 0.0110(18) -0.0121(23) 0.0245(13) 0.0003(14) 0.0364(24) C59 0.0383(26) 0.0011(14) -0.0078(18) 0.0209(12) 0.0005(12) 0.0307(20) C60 0.0311(24) -0.0030(14) -0.0073(17) 0.0213(11) 0.0022(11) 0.0254(19) C61 0.0289(24) -0.0023(13) -0.0073(17) 0.0198(11) 0.0038(11) 0.0298(20) O62 0.0323(17) 0.0020(10) -0.0045(12) 0.0216(8) 0.0029(8) 0.0294(14) C63 0.0384(28) 0.0024(17) 0.0039(20) 0.0363(15) 0.0046(15) 0.0419(24) C64 0.0320(25) -0.0009(13) -0.0059(16) 0.0215(10) 0.0005(11) 0.0223(18) C65 0.0299(24) -0.0029(12) -0.0065(16) 0.0194(10) 0.0003(10) 0.0241(18) C66 0.0288(24) -0.0024(12) -0.0066(16) 0.0196(10) 0.0004(11) 0.0251(18) C67 0.0354(26) -0.0065(14) -0.0157(18) 0.0245(12) 0.0032(12) 0.0331(21) C68 0.0346(26) -0.0021(14) -0.0081(17) 0.0223(11) 0.0011(11) 0.0239(19) C69 0.0320(24) -0.0045(13) -0.0029(17) 0.0217(10) 0.0023(11) 0.0250(19) C70 0.0298(25) -0.0054(14) -0.0108(17) 0.0261(11) 0.0003(12) 0.0268(20) O71 0.0394(20) -0.0157(12) -0.0170(13) 0.0373(12) 0.0063(11) 0.0329(16) C72 0.0704(39) -0.0289(22) -0.0133(23) 0.0401(18) 0.0030(16) 0.0369(25)