#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003445.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_2003445 _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_moiety 'C64 H64 O8,0.7(C H2 Cl2)' _chemical_formula_sum 'C65 H66 Cl2 O8' _chemical_formula_structural 'C64 H64 O8,0.7(C H2 Cl2)' _chemical_formula_weight 1022 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' 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' _cell_length_a 14.936(4) _cell_length_b 15.088(4) _cell_length_c 25.727(6) _cell_angle_alpha 90.0 _cell_angle_beta 92.44(2) _cell_angle_gamma 90.0 _cell_volume 5792(3) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.173 _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 60 _exptl_absorpt_coefficient_mu 1.35 _cell_measurement_temperature 113 _exptl_crystal_description 'clear, chunky' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.41 _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 6624 _reflns_number_total 5816 _reflns_number_observed 5140 _reflns_observed_criterion 'F > 4sigma(F)' _diffrn_reflns_av_R_equivalents 'unknown' _diffrn_reflns_theta_max 75 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 29 _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.2 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.070 _refine_ls_wR_factor_obs 0.076 _refine_ls_wR_factor_all 0.081 _refine_ls_goodness_of_fit_obs 2.85 _refine_ls_goodness_of_fit_all 2.81 _refine_ls_number_reflns 5140 _refine_ls_number_parameters 727 _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 0.62 _refine_diff_density_max 0.51 _refine_diff_density_min -0.47 _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 ? ? Cl ? 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 0.8528(3) -0.0330(3) 0.3549(2) 0.024(2) C2 0.8479(3) -0.1242(3) 0.3619(2) 0.028(2) C3 0.8325(3) -0.1815(3) 0.3198(2) 0.031(2) C4 0.8274(4) -0.2801(3) 0.3284(2) 0.042(2) C5 0.8251(3) -0.1441(3) 0.2703(2) 0.030(2) C6 0.8292(3) -0.0542(3) 0.2614(2) 0.023(2) C7 0.8421(3) 0.0019(3) 0.3047(2) 0.026(2) O8 0.8448(2) 0.0925(2) 0.2972(1) 0.030(1) C9 0.7606(4) 0.1336(4) 0.3053(2) 0.043(2) C10 0.8216(3) -0.0163(3) 0.2076(2) 0.025(2) C11 0.7441(3) -0.0278(3) 0.1767(2) 0.027(2) C12 0.7352(3) 0.0073(3) 0.1265(2) 0.028(2) C13 0.6487(4) -0.0024(4) 0.0946(2) 0.042(2) C14 0.8068(3) 0.0542(3) 0.1083(2) 0.029(2) C15 0.8867(3) 0.0659(3) 0.1377(2) 0.027(2) C16 0.8933(3) 0.0295(3) 0.1873(2) 0.024(2) O17 0.9716(2) 0.0423(2) 0.2166(1) 0.030(1) C18 1.0281(4) -0.0330(4) 0.2196(2) 0.046(2) C19 0.9634(3) 0.1158(3) 0.1160(2) 0.024(2) C20 1.0271(3) 0.0697(3) 0.0884(2) 0.030(2) C21 1.1006(3) 0.1135(3) 0.0681(2) 0.029(2) C22 1.1697(4) 0.0622(4) 0.0393(2) 0.040(2) C23 1.1079(4) 0.2035(4) 0.0766(2) 0.032(2) C24 1.0442(4) 0.2513(3) 0.1034(2) 0.029(2) C25 0.9725(3) 0.2050(3) 0.1232(2) 0.025(2) O26 0.9057(2) 0.2514(2) 0.1470(1) 0.030(1) C27 0.9237(4) 0.2670(3) 0.2015(2) 0.034(2) C28 1.0510(3) 0.3497(3) 0.1099(2) 0.028(2) C29 0.9984(3) 0.4053(3) 0.0796(2) 0.032(2) C30 1.0028(3) 0.4967(3) 0.0836(2) 0.032(2) C31 0.9431(4) 0.5572(4) 0.0506(2) 0.043(2) C32 1.0629(3) 0.5317(3) 0.1213(2) 0.030(2) C33 1.1152(3) 0.4785(3) 0.1543(2) 0.025(2) C34 1.1104(3) 0.3878(3) 0.1473(2) 0.025(2) O35 1.1578(2) 0.3301(2) 0.1803(1) 0.032(1) C36 1.2523(3) 0.3311(4) 0.1775(2) 0.043(2) C37 1.1663(3) 0.5200(3) 0.1989(2) 0.025(2) C38 1.2373(3) 0.5781(3) 0.1915(2) 0.028(2) C39 1.2854(3) 0.6167(3) 0.2335(2) 0.026(2) C40 1.3649(3) 0.6758(3) 0.2249(2) 0.029(2) C41 1.2597(3) 0.5962(3) 0.2837(2) 0.027(2) C42 1.1875(3) 0.5402(3) 0.2918(2) 0.025(2) C43 1.1412(3) 0.5036(3) 0.2494(2) 0.027(2) O44 1.0672(2) 0.4502(2) 0.2570(1) 0.031(1) C45 0.9857(4) 0.4985(4) 0.2560(2) 0.043(2) C46 1.1562(3) 0.5228(3) 0.3453(2) 0.026(2) C47 1.1250(3) 0.5911(3) 0.3755(2) 0.029(2) C48 1.0901(4) 0.5764(3) 0.4238(2) 0.033(2) C49 1.0560(4) 0.6518(4) 0.4551(2) 0.050(2) C50 1.0888(3) 0.4899(3) 0.4419(2) 0.027(2) C51 1.1203(3) 0.4202(3) 0.4139(2) 0.023(2) C52 1.1555(3) 0.4369(3) 0.3656(2) 0.026(2) O53 1.1847(2) 0.3660(2) 0.3369(1) 0.032(1) C54 1.2800(4) 0.3566(4) 0.3373(2) 0.048(2) C55 1.1221(3) 0.3280(3) 0.4356(2) 0.025(2) C56 1.1988(3) 0.2968(3) 0.4627(2) 0.031(2) C57 1.2035(4) 0.2132(3) 0.4844(2) 0.034(2) C58 1.2898(3) 0.1828(4) 0.5127(2) 0.050(2) C59 1.1283(3) 0.1589(3) 0.4790(2) 0.032(2) C60 1.0508(3) 0.1861(3) 0.4522(2) 0.022(2) C61 1.0489(3) 0.2719(3) 0.4302(2) 0.024(2) O62 0.9705(2) 0.3018(2) 0.4062(1) 0.027(1) C63 0.9638(3) 0.2894(3) 0.3504(2) 0.031(2) C64 0.9699(3) 0.1300(3) 0.4482(2) 0.024(2) C65 0.9081(3) 0.1322(3) 0.4877(2) 0.025(2) C66 0.8291(3) 0.0839(3) 0.4845(2) 0.028(2) C67 0.7620(3) 0.0897(4) 0.5273(2) 0.034(2) C68 0.8108(3) 0.0312(3) 0.4405(2) 0.025(2) C69 0.8716(3) 0.0258(3) 0.4009(2) 0.024(2) C70 0.9507(3) 0.0751(3) 0.4052(2) 0.023(2) O71 1.0113(2) 0.0706(2) 0.3662(1) 0.029(1) C72 1.0693(4) -0.0049(4) 0.3713(2) 0.043(2) Cl1* 0.2233(2) 0.2277(1) 0.9243(1) 0.066(1) Cl2** 0.0615(2) 0.2374(2) 0.8599(1) 0.071(1) C73* 0.1206(6) 0.1773(6) 0.9092(3) 0.057(2) Cl3*** 0.0156(13) 0.1906(13) 0.9315(8) 0.082(6) Cl4**** 0.0173(15) 0.2165(13) 0.8868(8) 0.048(6) H2 0.856 -0.151 0.401 0.04 H4A 0.815 -0.313 0.292 0.06 H4B 0.773 -0.295 0.354 0.06 H4C 0.890 -0.303 0.346 0.06 H5 0.816 -0.188 0.237 0.04 H9A 0.766 0.204 0.299 0.04 H9B 0.741 0.121 0.345 0.04 H9C 0.710 0.106 0.278 0.04 H11 0.689 -0.065 0.192 0.04 H13A 0.602 -0.041 0.116 0.05 H13B 0.662 -0.035 0.058 0.05 H13C 0.620 0.062 0.087 0.05 H14 0.801 0.083 0.070 0.04 H18A 1.088 -0.018 0.243 0.06 H18B 1.047 -0.051 0.181 0.06 H18C 0.993 -0.087 0.237 0.06 H20 1.020 -0.001 0.083 0.04 H22A 1.221 0.107 0.027 0.05 H22B 1.138 0.030 0.006 0.05 H22C 1.200 0.013 0.065 0.05 H23 1.165 0.238 0.062 0.04 H27A 0.869 0.303 0.217 0.04 H27B 0.985 0.305 0.207 0.04 H27C 0.931 0.204 0.222 0.04 H29 0.951 0.377 0.051 0.04 H31A 0.902 0.518 0.024 0.05 H31B 0.984 0.602 0.029 0.05 H31C 0.901 0.595 0.075 0.05 H32 1.069 0.603 0.125 0.04 H36A 1.281 0.284 0.205 0.06 H36B 1.277 0.397 0.187 0.06 H36C 1.270 0.314 0.139 0.06 H38 1.256 0.594 0.152 0.04 H40A 1.393 0.699 0.262 0.04 H40B 1.344 0.732 0.201 0.04 H40C 1.415 0.639 0.205 0.04 H41 1.296 0.624 0.317 0.04 H45A 0.931 0.454 0.262 0.06 H45B 0.976 0.531 0.219 0.06 H45C 0.989 0.548 0.286 0.06 H47 1.128 0.658 0.361 0.04 H49A 1.032 0.627 0.491 0.08 H49B 1.002 0.684 0.433 0.08 H49C 1.110 0.699 0.463 0.08 H50 1.062 0.477 0.479 0.04 H54A 1.297 0.300 0.314 0.06 H54B 1.306 0.347 0.377 0.06 H54C 1.309 0.416 0.321 0.06 H56 1.257 0.340 0.467 0.04 H58A 1.281 0.116 0.527 0.06 H58B 1.306 0.227 0.545 0.06 H58C 1.344 0.184 0.486 0.06 H59 1.130 0.094 0.496 0.04 H63A 0.900 0.315 0.335 0.04 H63B 0.968 0.220 0.342 0.04 H63C 1.018 0.324 0.333 0.04 H65 0.922 0.173 0.522 0.04 H67A 0.705 0.047 0.518 0.05 H67B 0.739 0.157 0.531 0.05 H67C 0.794 0.068 0.564 0.05 H68 0.749 -0.006 0.437 0.04 H72A 1.115 -0.005 0.340 0.05 H72B 1.030 -0.065 0.370 0.05 H72C 1.107 -0.002 0.408 0.05 H73A* 0.131 0.110 0.895 0.08 H73B* 0.081 0.174 0.944 0.08 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 0.021(3) 0.001(2) 0.002(2) 0.030(3) -0.002(2) 0.023(3) C2 0.033(3) -0.007(3) 0.004(2) 0.028(3) 0.002(2) 0.024(3) C3 0.035(3) -0.007(3) 0.003(3) 0.028(3) 0.001(3) 0.031(3) C4 0.064(4) -0.007(3) 0.001(3) 0.029(3) 0.005(3) 0.033(3) C5 0.031(3) -0.009(3) 0.002(2) 0.035(4) -0.004(3) 0.023(3) C6 0.025(3) -0.006(2) 0.000(2) 0.028(3) -0.004(2) 0.018(3) C7 0.026(3) -0.004(2) 0.006(2) 0.020(3) 0.004(2) 0.031(3) O8 0.037(2) 0.001(2) 0.002(2) 0.029(2) 0.000(2) 0.025(2) C9 0.047(4) 0.015(3) -0.002(3) 0.041(4) 0.007(3) 0.041(3) C10 0.028(3) -0.003(3) 0.006(3) 0.024(3) -0.005(2) 0.024(3) C11 0.026(3) -0.006(3) 0.002(3) 0.030(3) -0.003(2) 0.026(3) C12 0.028(3) -0.007(3) -0.006(3) 0.029(3) -0.002(2) 0.026(3) C13 0.041(4) -0.012(3) -0.007(3) 0.047(4) 0.011(3) 0.038(3) C14 0.033(3) -0.006(3) 0.001(3) 0.031(3) 0.001(2) 0.023(3) C15 0.031(3) -0.002(3) 0.003(3) 0.029(3) -0.006(2) 0.021(3) C16 0.024(3) -0.003(3) 0.000(3) 0.028(3) -0.004(2) 0.021(3) O17 0.025(2) -0.005(2) -0.003(2) 0.036(2) 0.000(2) 0.028(2) C18 0.032(4) 0.003(3) 0.001(3) 0.049(4) -0.011(3) 0.058(4) C19 0.020(3) -0.006(3) -0.002(2) 0.030(3) 0.000(2) 0.021(3) C20 0.033(3) -0.007(3) 0.003(3) 0.033(3) -0.002(2) 0.025(3) C21 0.032(3) -0.002(3) 0.002(3) 0.034(3) 0.000(2) 0.020(3) C22 0.046(4) 0.000(3) 0.017(3) 0.043(4) -0.005(3) 0.033(3) C23 0.032(3) -0.005(3) 0.003(3) 0.042(4) 0.004(3) 0.022(3) C24 0.032(3) -0.008(3) -0.002(3) 0.030(3) 0.001(2) 0.024(3) C25 0.022(3) -0.001(3) 0.001(2) 0.037(4) -0.004(2) 0.018(3) O26 0.028(2) -0.004(2) 0.002(2) 0.034(2) -0.001(2) 0.029(2) C27 0.039(4) -0.004(3) 0.009(3) 0.039(3) -0.007(3) 0.026(3) C28 0.025(3) -0.006(3) 0.002(3) 0.037(3) 0.004(3) 0.022(3) C29 0.025(3) -0.010(3) -0.003(3) 0.040(4) 0.001(3) 0.030(3) C30 0.027(3) -0.003(3) -0.004(3) 0.038(4) 0.000(3) 0.030(3) C31 0.037(4) 0.001(3) -0.009(3) 0.050(4) 0.008(3) 0.039(3) C32 0.032(3) -0.006(3) 0.005(3) 0.030(3) 0.004(3) 0.028(3) C33 0.023(3) -0.005(3) 0.003(2) 0.031(3) 0.004(2) 0.022(3) C34 0.025(3) -0.002(3) 0.001(3) 0.029(3) 0.007(2) 0.020(3) O35 0.030(2) -0.007(2) -0.005(2) 0.034(2) 0.004(2) 0.030(2) C36 0.032(4) 0.005(3) 0.005(3) 0.045(4) 0.005(3) 0.053(4) C37 0.026(3) -0.004(3) 0.000(2) 0.026(3) 0.003(2) 0.022(3) C38 0.025(3) 0.002(3) 0.005(3) 0.031(3) 0.007(2) 0.029(3) C39 0.027(3) -0.001(3) 0.000(3) 0.026(3) -0.001(2) 0.025(3) C40 0.029(3) -0.007(3) 0.005(2) 0.032(3) 0.004(2) 0.027(3) C41 0.030(3) 0.000(3) 0.005(3) 0.025(3) 0.001(2) 0.026(3) C42 0.028(3) -0.002(3) 0.002(3) 0.026(3) -0.001(2) 0.020(3) C43 0.023(3) -0.005(3) 0.001(3) 0.025(3) 0.004(2) 0.032(3) O44 0.029(2) -0.010(2) 0.005(2) 0.039(2) 0.000(2) 0.024(2) C45 0.029(4) -0.003(3) 0.010(3) 0.060(4) -0.001(3) 0.041(4) C46 0.029(3) -0.010(3) 0.003(2) 0.026(3) 0.002(2) 0.022(3) C47 0.039(3) -0.007(3) 0.007(3) 0.022(3) -0.006(2) 0.027(3) C48 0.040(4) -0.008(3) 0.008(3) 0.029(3) -0.004(2) 0.029(3) C49 0.077(5) -0.001(3) 0.025(3) 0.031(3) -0.006(3) 0.045(4) C50 0.028(3) -0.005(3) 0.004(2) 0.032(3) -0.001(2) 0.021(3) C51 0.019(3) -0.007(2) -0.001(2) 0.031(3) -0.003(2) 0.018(3) C52 0.028(3) -0.001(3) 0.004(2) 0.028(3) -0.009(2) 0.022(3) O53 0.037(2) -0.001(2) 0.008(2) 0.032(2) -0.005(2) 0.028(2) C54 0.036(4) 0.009(3) 0.018(3) 0.053(4) -0.001(3) 0.057(4) C55 0.028(3) -0.001(3) 0.003(2) 0.029(3) -0.002(2) 0.017(3) C56 0.024(3) -0.006(3) -0.002(3) 0.042(4) 0.002(3) 0.026(3) C57 0.037(4) -0.003(3) -0.005(3) 0.036(4) 0.007(3) 0.029(3) C58 0.029(4) -0.010(3) -0.018(3) 0.061(4) 0.026(3) 0.058(4) C59 0.029(3) -0.005(3) -0.001(3) 0.036(3) 0.007(3) 0.032(3) C60 0.023(3) -0.002(3) 0.000(2) 0.027(3) 0.003(2) 0.016(3) C61 0.017(3) 0.004(3) 0.003(2) 0.036(3) -0.002(2) 0.018(3) O62 0.025(2) 0.000(2) 0.001(2) 0.029(2) 0.000(2) 0.026(2) C63 0.031(3) 0.003(3) -0.006(2) 0.041(3) -0.001(2) 0.021(3) C64 0.028(3) 0.000(3) -0.003(3) 0.022(3) 0.008(2) 0.021(3) C65 0.024(3) -0.001(3) -0.001(3) 0.028(3) 0.005(2) 0.023(3) C66 0.027(3) 0.002(3) 0.006(3) 0.029(3) 0.003(2) 0.028(3) C67 0.030(3) -0.002(3) 0.003(3) 0.049(4) -0.007(3) 0.022(3) C68 0.030(3) 0.002(3) -0.001(3) 0.024(3) 0.002(2) 0.021(3) C69 0.025(3) 0.003(3) -0.001(2) 0.027(3) 0.004(2) 0.019(3) C70 0.025(3) -0.001(3) 0.003(3) 0.025(3) 0.002(2) 0.020(3) O71 0.028(2) -0.003(2) 0.009(2) 0.034(2) -0.001(2) 0.026(2) C72 0.031(4) 0.011(3) 0.016(3) 0.046(4) 0.001(3) 0.053(4) Cl1 0.089(2) -0.017(1) 0.002(1) 0.048(1) 0.001(1) 0.059(1) Cl2 0.069(2) 0.010(2) -0.010(2) 0.058(2) -0.030(2) 0.084(2) _cod_database_code 2003445