data_2003447 _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 O8,1.04(C H2 Cl2),Cs +,Cl O4 -' _chemical_formula_sum 'C65 H66 Cl3 Cs O12' _chemical_formula_weight 1283 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x,y,1/2-z' '-x,-y,1/2+z' '1/2+x,1/2-y,z' '1/2-x,1/2+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 n a m' _cell_length_a 17.088(5) _cell_length_b 19.691(6) _cell_length_c 20.392(6) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 6861(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 15 _cell_measurement_theta_min 7.4 _cell_measurement_theta_max 10.4 _exptl_absorpt_coefficient_mu 0.65 _cell_measurement_temperature 115 _exptl_crystal_description 'prismatic needle' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _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 integration _exptl_absorpt_correction_T_min 0.872 _exptl_absorpt_correction_T_max 0.925 _diffrn_reflns_number 6698 _reflns_number_total 5072 _reflns_number_observed 3064 _reflns_observed_criterion 'F > 4sigma(F)' _diffrn_reflns_av_R_equivalents 'unknown' _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _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 0.091 _refine_ls_wR_factor_obs 0.079 _refine_ls_wR_factor_all 0.108 _refine_ls_goodness_of_fit_obs 1.83 _refine_ls_goodness_of_fit_all 1.62 _refine_ls_number_reflns 3064 _refine_ls_number_parameters 207 _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme 'sigma' _refine_ls_shift/esd_max 0.16 _refine_diff_density_max 0.92 _refine_diff_density_min -0.99 _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 ? ? Cs+ ? 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 Cs46 0.3701(1) 0.2489(1) 0.7500 0.0223(3) Cl47 0.1212(3) 0.1567(2) 0.7500 0.022(1) O48 0.1160(5) 0.1151(4) 0.6921(4) 0.031(3) O49 0.1946(7) 0.1921(7) 0.7500 0.040(5) O50 0.0577(7) 0.2055(6) 0.7500 0.029(4) Cl'* 0.3119(3) 0.4257(2) 0.1785(2) 0.043(2) C1 0.4457(7) 0.0240(5) 0.8095(6) 0.020(3) C2 0.4170(7) -0.0433(6) 0.6913(6) 0.026(3) C3 0.4021(10) -0.0766(8) 0.7500 0.026(5) C4 0.3740(12) -0.1480(9) 0.7500 0.039(5) C7 0.4594(10) 0.0553(9) 0.7500 0.023(5) O8 0.4877(6) 0.1226(5) 0.7500 0.023(3) C9 0.5718(10) 0.1245(8) 0.7500 0.022(4) C10 0.4671(6) 0.0580(6) 0.6274(5) 0.015(3) C11 0.5337(6) 0.0359(5) 0.5934(5) 0.017(3) C12 0.5558(7) 0.0659(6) 0.5332(6) 0.023(3) C13 0.6302(7) 0.0430(5) 0.4995(5) 0.026(3) C14 0.5083(7) 0.1161(6) 0.5089(6) 0.023(3) C15 0.4410(6) 0.1391(5) 0.5406(6) 0.018(3) C16 0.4215(7) 0.1108(6) 0.6006(6) 0.020(3) O17 0.3569(4) 0.1334(4) 0.6356(4) 0.023(2) C18 0.2858(7) 0.1013(6) 0.6153(6) 0.024(3) C19 0.3898(7) 0.1933(6) 0.5109(6) 0.022(3) C20 0.3505(6) 0.1806(6) 0.4525(6) 0.022(3) C21 0.3024(7) 0.2301(5) 0.4239(6) 0.022(3) C22 0.2567(8) 0.2156(7) 0.3618(7) 0.046(4) C23 0.2987(7) 0.2945(6) 0.4537(6) 0.025(3) C24 0.3380(7) 0.3070(6) 0.5130(6) 0.018(3) C25 0.3835(6) 0.2577(6) 0.5405(4) 0.018(2) O26 0.4243(4) 0.2704(3) 0.5984(4) 0.021(2) C27 0.5013(8) 0.2952(6) 0.5863(6) 0.036(4) C28 0.3360(7) 0.3794(6) 0.5394(6) 0.020(3) C29 0.3632(7) 0.4320(6) 0.5010(5) 0.023(3) C30 0.3626(7) 0.4980(5) 0.5246(5) 0.022(3) C31 0.3957(7) 0.5553(6) 0.4823(6) 0.037(4) C32 0.3319(7) 0.5104(6) 0.5855(6) 0.022(3) C33 0.3031(7) 0.4584(6) 0.6254(6) 0.020(3) C34 0.3061(7) 0.3914(6) 0.6021(6) 0.024(3) O35 0.2750(4) 0.3395(4) 0.6416(4) 0.022(2) C36 0.2017(7) 0.3134(6) 0.6199(6) 0.026(3) C37 0.2684(6) 0.4773(5) 0.6905(5) 0.015(3) C38 0.2071(7) 0.5245(6) 0.6910(6) 0.022(3) C39 0.1746(9) 0.5485(8) 0.7500 0.012(4) C40 0.1088(10) 0.5996(8) 0.7500 0.027(5) C43 0.2981(10) 0.4526(9) 0.7500 0.021(5) O44 0.3615(7) 0.4092(5) 0.7500 0.023(3) C45 0.4362(13) 0.4433(11) 0.7500 0.055(7) C'* 0.2965(14) 0.4709(12) 0.2500 0.020(6) Cl"** 0.9044(13) 0.8598(11) 0.7500 0.100(8) Cl'"*** 0.9960(21) 0.8086(18) 0.6374(15) 0.137(14) H2 0.412 -0.057 0.640 0.04 H4A 0.311 -0.148 0.750 0.04 H4B 0.396 -0.175 0.793 0.04 H9A 0.588 0.177 0.750 0.04 H9B 0.594 0.099 0.793 0.04 H11 0.569 -0.005 0.613 0.04 H13A 0.638 0.071 0.455 0.04 H13B 0.626 -0.011 0.489 0.04 H13C 0.680 0.052 0.531 0.04 H14 0.524 0.139 0.463 0.04 H18A 0.238 0.121 0.644 0.04 H18B 0.290 0.047 0.622 0.04 H18C 0.275 0.112 0.564 0.04 H20 0.357 0.132 0.429 0.04 H22A 0.267 0.164 0.347 0.04 H22B 0.276 0.250 0.324 0.04 H22C 0.195 0.223 0.371 0.04 H23 0.266 0.335 0.431 0.04 H27A 0.531 0.304 0.632 0.04 H27B 0.498 0.342 0.559 0.04 H27C 0.534 0.258 0.558 0.04 H29 0.385 0.422 0.452 0.04 H31A 0.390 0.603 0.508 0.04 H31B 0.363 0.558 0.437 0.04 H31C 0.457 0.545 0.472 0.04 H32 0.330 0.562 0.603 0.04 H36A 0.182 0.274 0.653 0.04 H36B 0.208 0.292 0.571 0.04 H36C 0.159 0.354 0.619 0.04 H38 0.184 0.543 0.645 0.04 H40A 0.131 0.651 0.750 0.04 H40B 0.074 0.591 0.793 0.04 H45A 0.482 0.405 0.750 0.04 H45B 0.442 0.475 0.707 0.04 H'A* 0.336 0.514 0.250 0.06 H'B* 0.237 0.489 0.250 0.06 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 Cs46 0.0291(6) 0.0030(7) 0.000 0.0175(4) 0.000 0.0203(5) Cl47 0.019(2) 0.002(3) 0.000 0.023(2) 0.000 0.023(2) O48 0.028(5) 0.002(5) -0.006(5) 0.041(5) -0.011(4) 0.022(4) O49 0.034(9) -0.019(8) 0.000 0.047(10) 0.000 0.039(9) O50 0.039(9) 0.011(7) 0.000 0.023(7) 0.000 0.024(7) Cl' 0.069(4) -0.005(3) 0.013(3) 0.039(3) -0.010(2) 0.022(3)