#------------------------------------------------------------------------------ #$Date: 2009-11-14 13:09:05 +0000 (Sat, 14 Nov 2009) $ #$Revision: 846 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003448.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_2003448 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 894 _journal_page_last 904 _publ_section_title ; Octaanisyl Cavitands and a Related Caviplex ; _chemical_formula_sum 'C56 H48 O8' _chemical_formula_structural 'C56 H48 O8' _chemical_formula_weight 849.0 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' _symmetry_space_group_name_H-M 'P -1' _cell_length_a 7.924(2) _cell_length_b 11.433(3) _cell_length_c 25.541(6) _cell_angle_alpha 79.12(2) _cell_angle_beta 83.61(2) _cell_angle_gamma 87.60(2) _cell_volume 2257.6(10) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.249 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 15 _cell_measurement_theta_min 9 _cell_measurement_theta_max 11 _exptl_absorpt_coefficient_mu 0.047 _cell_measurement_temperature 296 _exptl_crystal_description 'plates and prisms' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _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 8012 _reflns_number_total 8012 _reflns_number_observed 4918 _reflns_observed_criterion 'F > 2sigma(F)' _diffrn_reflns_av_R_equivalents 'unknown' _diffrn_reflns_theta_max 25.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.5 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.112 _refine_ls_wR_factor_obs 0.096 _refine_ls_wR_factor_all 0.109 _refine_ls_goodness_of_fit_obs 1.49 _refine_ls_goodness_of_fit_all 1.21 _refine_ls_number_reflns 4918 _refine_ls_number_parameters 606 _refine_ls_hydrogen_treatment ; H riding on attached C, or as part of rigid CH~3~ group, C-H 1.08\%A, fixed at U~eq~(attached C) + 0.01\%A^2^ ; _refine_ls_weighting_scheme '1/[\s^2^(F) + 0.0002F^2^]' _refine_ls_shift/esd_max 0.14 _refine_diff_density_max 0.48 _refine_diff_density_min -0.38 _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 0.5194(8) 0.3912(5) 0.9049(2) 0.058(2) C2 0.6543(8) 0.4299(5) 0.9268(2) 0.068(2) C3 0.7730(8) 0.5071(5) 0.8955(2) 0.071(3) C4 0.7597(8) 0.5440(5) 0.8415(2) 0.067(2) C5 0.6235(7) 0.5089(5) 0.8184(2) 0.053(2) C6 0.5021(7) 0.4338(5) 0.8504(2) 0.053(2) O7 0.3683(5) 0.3983(3) 0.8278(1) 0.061(2) C8 0.2179(8) 0.4705(6) 0.8314(3) 0.092(3) C9 0.5992(7) 0.5527(5) 0.7605(2) 0.050(2) C10 0.5163(7) 0.6585(5) 0.7453(2) 0.057(2) C11 0.4840(8) 0.7003(5) 0.6926(2) 0.065(2) C12 0.5363(8) 0.6312(5) 0.6548(2) 0.065(2) C13 0.6197(7) 0.5233(5) 0.6682(2) 0.053(2) C14 0.6546(7) 0.4855(5) 0.7212(2) 0.055(2) O15 0.7492(6) 0.3821(4) 0.7350(2) 0.081(2) C16 0.6561(10) 0.2747(6) 0.7460(3) 0.101(3) C17 0.6713(8) 0.4516(5) 0.6254(2) 0.056(2) C18 0.8378(8) 0.4499(5) 0.6025(2) 0.065(2) C19 0.8806(9) 0.3908(6) 0.5600(2) 0.078(3) C20 0.7576(10) 0.3300(5) 0.5422(2) 0.076(3) C21 0.5944(8) 0.3275(5) 0.5649(2) 0.057(2) C22 0.5493(7) 0.3903(5) 0.6059(2) 0.065(2) O23A* 0.3760(8) 0.4185(6) 0.6173(2) 0.079(3) C24A* 0.3027(11) 0.3605(10) 0.6686(3) 0.114(5) C25 0.4628(8) 0.2625(5) 0.5455(2) 0.064(2) C26 0.3856(9) 0.3117(6) 0.4994(2) 0.075(3) C27 0.2607(8) 0.2517(6) 0.4832(2) 0.072(2) C28 0.2029(8) 0.1436(5) 0.5128(2) 0.066(2) C29 0.2769(8) 0.0927(5) 0.5594(2) 0.058(2) C30 0.4099(8) 0.1514(5) 0.5739(2) 0.060(2) O31 0.4894(6) 0.1004(4) 0.6181(1) 0.071(2) C32 0.6119(9) 0.0124(6) 0.6073(3) 0.090(3) C33 0.2066(8) -0.0209(5) 0.5926(2) 0.062(2) C34 0.2033(8) -0.1231(5) 0.5719(2) 0.074(3) C35 0.1321(9) -0.2249(5) 0.6020(2) 0.083(3) C36 0.0661(8) -0.2268(5) 0.6545(2) 0.074(3) C37 0.0720(7) -0.1261(5) 0.6768(2) 0.058(2) C38 0.1366(7) -0.0222(5) 0.6453(2) 0.058(2) O39 0.1342(5) 0.0802(3) 0.6662(1) 0.062(2) C40 -0.0183(10) 0.1446(7) 0.6647(3) 0.106(3) C41 0.0033(8) -0.1285(4) 0.7341(2) 0.054(2) C42 -0.1673(9) -0.1438(5) 0.7498(2) 0.072(3) C43 -0.2355(8) -0.1426(5) 0.8024(2) 0.073(2) C44 -0.1263(8) -0.1299(5) 0.8396(2) 0.061(2) C45 0.0462(8) -0.1188(4) 0.8259(2) 0.054(2) C46 0.1073(7) -0.1156(5) 0.7726(2) 0.049(2) O47 0.2800(5) -0.1092(4) 0.7567(1) 0.067(2) C48 0.3627(8) 0.0000(6) 0.7579(2) 0.077(3) C49 0.1600(7) -0.1131(5) 0.8680(2) 0.051(2) C50 0.2721(8) -0.2076(5) 0.8831(2) 0.065(2) C51 0.3789(8) -0.2027(5) 0.9225(2) 0.075(2) C52 0.3743(8) -0.1031(6) 0.9460(2) 0.072(3) C53 0.2682(7) -0.0080(5) 0.9311(2) 0.052(2) C54 0.1576(7) -0.0149(5) 0.8926(2) 0.049(2) O55 0.0402(5) 0.0740(4) 0.8806(2) 0.065(2) C56 0.0864(9) 0.1699(6) 0.8394(3) 0.097(3) C57 0.2746(7) 0.1063(5) 0.9507(2) 0.056(2) C58 0.1664(7) 0.1351(6) 0.9939(2) 0.070(2) C59 0.1759(9) 0.2449(6) 1.0081(2) 0.082(3) C60 0.2894(8) 0.3280(6) 0.9799(2) 0.072(2) C61 0.3981(7) 0.3030(5) 0.9369(2) 0.056(2) C62 0.3895(7) 0.1919(5) 0.9233(2) 0.055(2) O63 0.4918(5) 0.1640(3) 0.8798(1) 0.061(2) C64 0.6591(8) 0.1269(6) 0.8900(3) 0.086(3) O23B** 0.4052(10) 0.3553(11) 0.6397(4) 0.056(5) C24B** 0.2545(12) 0.4216(22) 0.6248(10) 0.124(12) H2 0.668 0.400 0.969 0.08 H3 0.875 0.538 0.914 0.08 H4 0.855 0.600 0.817 0.08 H8A 0.127 0.439 0.809 0.10 H8B 0.240 0.564 0.816 0.10 H8C 0.169 0.458 0.873 0.10 H10 0.474 0.712 0.775 0.07 H11 0.419 0.785 0.681 0.08 H12 0.512 0.662 0.614 0.07 H16A 0.736 0.206 0.766 0.11 H16B 0.624 0.250 0.710 0.11 H16C 0.541 0.285 0.772 0.11 H18 0.934 0.494 0.618 0.07 H19 1.009 0.392 0.541 0.09 H20 0.792 0.283 0.509 0.09 H24A 0.167 0.378 0.674 0.13 H24B 0.361 0.386 0.701 0.13 H24C 0.326 0.267 0.669 0.13 H26 0.425 0.397 0.477 0.08 H27 0.206 0.289 0.447 0.08 H28 0.102 0.099 0.500 0.08 H32A 0.663 -0.034 0.643 0.10 H32B 0.712 0.060 0.581 0.10 H32C 0.559 -0.051 0.588 0.10 H34 0.258 -0.123 0.531 0.09 H35 0.128 -0.304 0.585 0.10 H36 0.010 -0.307 0.678 0.09 H40A -0.009 0.225 0.680 0.12 H40B -0.132 0.099 0.683 0.12 H40C -0.023 0.167 0.622 0.12 H42 -0.250 -0.157 0.721 0.08 H43 -0.370 -0.151 0.814 0.08 H44 -0.178 -0.129 0.880 0.07 H48A 0.482 -0.008 0.734 0.09 H48B 0.387 0.017 0.797 0.09 H48C 0.289 0.073 0.738 0.09 H50 0.276 -0.285 0.864 0.07 H51 0.465 -0.276 0.934 0.09 H52 0.456 -0.100 0.977 0.08 H56A 0.009 0.249 0.841 0.10 H56B 0.065 0.135 0.804 0.10 H56C 0.219 0.191 0.837 0.10 H58 0.076 0.071 1.016 0.08 H59 0.093 0.266 1.042 0.09 H60 0.293 0.414 0.991 0.08 H64A 0.730 0.110 0.853 0.09 H64B 0.668 0.050 0.921 0.09 H64C 0.711 0.203 0.902 0.09 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 0.076(4) -0.007(3) -0.002(3) 0.067(4) -0.018(3) 0.036(3) C2 0.083(5) -0.025(4) -0.009(3) 0.089(5) -0.016(3) 0.036(3) C3 0.083(5) -0.017(4) -0.021(3) 0.083(5) -0.023(3) 0.055(4) C4 0.068(4) -0.016(3) -0.010(3) 0.076(4) -0.015(3) 0.059(4) C5 0.061(4) -0.002(3) -0.003(3) 0.056(4) -0.019(3) 0.046(3) C6 0.060(4) -0.004(3) -0.007(3) 0.061(4) -0.025(3) 0.046(3) O7 0.063(3) -0.006(2) -0.010(2) 0.070(3) -0.020(2) 0.055(2) C8 0.059(5) 0.000(4) -0.018(4) 0.096(6) -0.030(5) 0.126(6) C9 0.057(4) -0.005(3) 0.000(3) 0.058(4) -0.013(3) 0.037(3) C10 0.059(4) -0.004(3) -0.005(3) 0.058(4) -0.024(3) 0.060(4) C11 0.095(5) -0.002(3) -0.015(3) 0.054(4) -0.010(3) 0.049(3) C12 0.103(5) -0.007(4) -0.003(3) 0.052(4) -0.009(3) 0.041(3) C13 0.061(4) -0.010(3) 0.006(3) 0.059(4) -0.017(3) 0.040(3) C14 0.054(4) 0.002(3) -0.005(3) 0.065(4) -0.013(3) 0.045(3) O15 0.095(4) 0.025(3) -0.015(2) 0.085(3) -0.027(3) 0.065(3) C16 0.140(7) 0.038(5) 0.003(5) 0.077(5) -0.016(4) 0.080(5) C17 0.076(4) -0.005(3) 0.001(3) 0.054(4) -0.007(3) 0.037(3) C18 0.075(5) -0.008(3) 0.003(3) 0.064(4) -0.012(3) 0.054(4) C19 0.084(5) 0.000(4) 0.023(4) 0.084(5) -0.029(4) 0.066(4) C20 0.111(6) -0.008(4) 0.001(4) 0.068(4) -0.028(3) 0.054(4) C21 0.084(5) -0.004(3) 0.010(3) 0.049(4) -0.011(3) 0.035(3) C22 0.072(5) -0.013(4) 0.016(3) 0.073(4) -0.023(3) 0.052(4) O23A 0.100(7) -0.016(5) 0.016(4) 0.091(6) -0.028(4) 0.048(4) C24A 0.092(10) -0.020(8) 0.014(8) 0.139(12) -0.061(9) 0.121(11) C25 0.104(5) -0.011(4) 0.005(3) 0.058(4) -0.015(3) 0.032(3) C26 0.113(6) -0.007(4) -0.005(4) 0.069(4) -0.005(3) 0.040(3) C27 0.101(5) -0.005(4) -0.011(3) 0.072(5) -0.004(3) 0.041(3) C28 0.088(5) -0.008(4) -0.009(3) 0.069(4) -0.010(3) 0.042(3) C29 0.085(5) -0.001(3) -0.008(3) 0.061(4) -0.017(3) 0.032(3) C30 0.093(5) 0.000(4) -0.009(3) 0.063(4) -0.013(3) 0.026(3) O31 0.109(4) -0.010(3) -0.013(2) 0.064(3) -0.006(2) 0.039(2) C32 0.113(6) -0.004(5) -0.037(4) 0.077(5) 0.004(4) 0.078(5) C33 0.088(5) -0.006(3) -0.017(3) 0.063(4) -0.012(3) 0.041(3) C34 0.121(6) -0.010(4) -0.014(3) 0.067(4) -0.024(3) 0.042(3) C35 0.151(7) -0.026(4) -0.020(4) 0.050(4) -0.012(3) 0.053(4) C36 0.116(6) -0.027(4) -0.015(3) 0.064(4) -0.006(3) 0.044(3) C37 0.083(4) -0.012(3) -0.013(3) 0.058(4) -0.014(3) 0.039(3) C38 0.081(4) -0.005(3) -0.015(3) 0.058(4) -0.014(3) 0.039(3) O39 0.085(3) 0.000(2) -0.010(2) 0.058(3) -0.022(2) 0.049(2) C40 0.110(7) 0.013(5) -0.013(5) 0.081(6) -0.044(5) 0.134(7) C41 0.068(4) -0.012(3) -0.012(3) 0.050(3) -0.008(3) 0.046(3) C42 0.090(5) -0.027(4) -0.023(4) 0.079(5) -0.006(3) 0.050(4) C43 0.066(4) -0.027(4) -0.007(3) 0.089(5) -0.007(4) 0.065(4) C44 0.078(5) -0.021(3) -0.009(3) 0.067(4) -0.007(3) 0.041(3) C45 0.071(4) -0.004(3) -0.014(3) 0.048(3) -0.011(3) 0.044(3) C46 0.049(4) -0.007(3) -0.004(3) 0.058(4) -0.009(3) 0.039(3) O47 0.079(3) 0.006(2) -0.012(2) 0.080(3) -0.025(2) 0.048(2) C48 0.070(5) -0.022(4) -0.002(3) 0.107(6) -0.016(4) 0.055(4) C49 0.067(4) -0.008(3) 0.003(3) 0.056(4) -0.011(3) 0.029(3) C50 0.095(5) 0.001(4) -0.010(3) 0.054(4) -0.008(3) 0.046(3) C51 0.104(5) 0.007(4) -0.032(4) 0.065(4) -0.003(3) 0.057(4) C52 0.095(5) -0.001(4) -0.028(3) 0.076(5) -0.005(3) 0.047(4) C53 0.063(4) -0.012(3) -0.004(3) 0.065(4) -0.009(3) 0.030(3) C54 0.045(3) -0.001(3) 0.005(3) 0.063(4) -0.005(3) 0.036(3) O55 0.062(3) -0.004(2) -0.009(2) 0.067(3) -0.020(2) 0.071(3) C56 0.085(5) -0.006(4) -0.015(5) 0.079(5) 0.012(5) 0.117(6) C57 0.067(4) -0.013(3) -0.005(3) 0.071(4) -0.014(3) 0.033(3) C58 0.074(4) -0.027(4) 0.015(3) 0.094(5) -0.027(3) 0.044(3) C59 0.114(6) -0.024(4) 0.019(4) 0.091(5) -0.029(4) 0.044(4) C60 0.099(5) -0.015(4) 0.006(3) 0.070(4) -0.022(3) 0.049(4) C61 0.073(4) -0.012(3) -0.001(3) 0.071(4) -0.021(3) 0.030(3) C62 0.059(4) -0.009(3) -0.004(3) 0.073(4) -0.014(3) 0.036(3) O63 0.065(3) 0.004(2) 0.004(2) 0.075(3) -0.020(2) 0.044(2) C64 0.074(5) 0.022(4) 0.004(4) 0.107(6) -0.015(4) 0.072(4)