#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/36/2003615.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2003615 loop_ _publ_author_name 'Ting, Y.' 'Verboom, W.' 'Reinhoudt, D. N.' 'Harkema, S.' _publ_section_title ; 1,3-Diethoxy-2,4-didehydroxy-p-tert-butylcalix[4]arene ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1465 _journal_page_last 1467 _journal_volume 51 _journal_year 1995 _chemical_formula_moiety 'C48 H64 O2' _chemical_formula_sum 'C48 H64 O2' _chemical_formula_weight 673.0 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_type_scat_source IntTabIV _cell_angle_alpha 81.48(3) _cell_angle_beta 73.48(3) _cell_angle_gamma 79.60(2) _cell_formula_units_Z 2 _cell_length_a 10.412(3) _cell_length_b 12.900(2) _cell_length_c 16.892(5) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(1) _cell_measurement_theta_max 14.1 _cell_measurement_theta_min 7.0 _cell_volume 2128.1(10) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 7425 _diffrn_reflns_theta_max 25.0 _diffrn_standards_decay_% 4 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.058 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.05 _exptl_crystal_description parallelepiped _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _refine_diff_density_max 0.33 _refine_diff_density_min -0.19 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 2.38 _refine_ls_hydrogen_treatment 'All H-atoms treated as riding atoms' _refine_ls_number_parameters 451 _refine_ls_number_reflns 3390 _refine_ls_R_factor_obs 0.070 _refine_ls_shift/esd_max 0.19 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'w = 1/\s^2^(F)' _refine_ls_wR_factor_obs 0.080 _reflns_number_observed 3390 _reflns_number_total 7425 _reflns_observed_criterion I>3\s(I) _[local]_cod_data_source_file ab1130.cif _[local]_cod_data_source_block ab1130a _cod_original_cell_volume 2128.0(10) _cod_database_code 2003615 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_B_iso_or_equiv O31 -.2077(3) .3305(3) .3516(2) 6.27(9) O71 .1558(3) .0545(2) .2759(2) 5.60(9) C1 .1293(4) .3509(3) .2173(3) 3.7(1) C2 .2612(4) .3155(3) .2220(3) 3.7(1) C3 .3276(4) .3820(3) .2481(3) 4.2(1) C4 .2669(4) .4821(3) .2702(3) 3.8(1) C5 .1336(4) .5125(3) .2673(3) 4.1(1) C6 .0637(4) .4487(3) .2410(3) 3.8(1) C7 .3450(4) .5522(3) .2991(3) 4.8(1) C8 .4800(6) .5613(5) .2349(5) 10.8(2) C9 .2725(6) .6627(4) .3090(4) 11.3(2) C10 .3803(7) .5011(5) .3757(4) 13.5(2) C20 -.0815(4) .4889(3) .2395(3) 5.3(1) C21 -.2118(4) .3349(3) .2705(3) 4.2(1) C22 -.1542(4) .4140(3) .2143(3) 4.0(1) C23 -.1666(4) .4246(3) .1342(3) 4.3(1) C24 -.2335(4) .3586(3) .1069(3) 4.0(1) C25 -.2875(4) .2802(3) .1652(3) 4.0(1) C26 -.2791(4) .2665(3) .2462(3) 4.1(1) C27 -.2439(4) .3722(4) .0179(3) 4.8(1) C28 -.3510(6) .3186(6) .0063(4) 14.5(2) C29 -.2716(8) .4890(5) -.0138(4) 11.8(3) C30 -.1099(7) .3312(7) -.0378(4) 12.7(3) C32 -.1179(5) .2458(5) .3811(3) 7.1(2) C33 -.0670(7) .2789(6) .4425(4) 13.3(3) C40 -.3448(4) .1803(3) .3061(3) 5.0(1) C41 -.1361(4) .0508(3) .2463(3) 4.3(1) C42 -.2607(4) .0701(3) .3022(3) 4.1(1) C43 -.3116(4) -.0124(3) .3562(3) 4.7(1) C44 -.2433(4) -.1151(3) .3566(3) 4.7(1) C45 -.1182(4) -.1314(3) .2997(3) 4.7(1) C46 -.0625(4) -.0508(3) .2445(3) 4.2(1) C47 -.3047(6) -.2038(4) .4166(3) 6.4(2) C48 -.327(1) -.1814(6) .5047(4) 13.9(3) C49 -.4422(8) -.2072(6) .4125(7) 23.7(4) C50 -.223(1) -.3053(5) .4064(6) 23.0(4) C60 .0699(4) -.0766(3) .1807(3) 5.7(1) C61 .1983(4) .0691(3) .1898(3) 4.1(1) C62 .1543(4) .0111(3) .1425(3) 4.1(1) C63 .1950(4) .0314(3) .0575(3) 4.3(1) C64 .2801(4) .1055(3) .0167(3) 4.2(1) C65 .3181(4) .1625(3) .0679(3) 4.0(1) C66 .2808(4) .1460(3) .1527(3) 4.1(1) C67 .3296(5) .1237(4) -.0780(3) 5.2(1) C68 .3280(9) .0275(5) -.1194(4) 13.9(3) C69 .4771(6) .1418(6) -.1061(4) 9.7(2) C70 .2453(7) .2178(6) -.1106(4) 14.3(3) C72 .2318(7) -.0302(5) .3143(3) 8.6(2) C73 .173(1) -.0404(8) .4036(4) 15.0(4) C80 .3338(4) .2062(3) .2037(3) 4.9(1) H1 .083816 .307429 .196968 ? H3 .417964 .358117 .251334 ? H5 .088479 .579738 .283974 ? H25 -.33374 .233474 .148828 ? H23 -.126698 .479015 .095857 ? H41 -.099529 .107276 .208849 ? H43 -.397721 .001545 .394622 ? H45 -.068199 -.200710 .298642 ? H63 .162762 -.007307 .025276 ? H65 .372858 .216136 .042797 ? H8A .530340 .604139 .252074 ? H8B .530843 .492836 .227489 ? H8C .461742 .592875 .184019 ? H9A .323836 .703477 .327329 ? H9B .258969 .694473 .256996 ? H9C .187273 .659837 .348518 ? H10A .4289 .5446 .3936 ? H10B .299731 .490396 .417879 ? H10C .434823 .434604 .364904 ? H28A -.353157 .329749 -.050236 ? H28B -.333189 .244807 .022208 ? H28C -.436020 .347227 .040095 ? H29A -.277954 .494755 -.069360 ? H29B -.354435 .520570 .020298 ? H29C -.199986 .524192 -.012069 ? H30A -.114477 .338830 -.093736 ? H30B -.043228 .369971 -.033460 ? H30C -.086417 .258386 -.020546 ? H48A -.365705 -.237219 .542042 ? H48B -.243033 -.175270 .513425 ? H48C -.387152 -.116737 .513988 ? H49A -.480123 -.262839 .450292 ? H49B -.496924 -.141436 .425543 ? H49C -.438313 -.218695 .357526 ? H50A -.264277 -.358594 .445187 ? H50B -.211774 -.321435 .351599 ? H50C -.136596 -.302400 .414165 ? H68A .359482 .041903 -.177873 ? H68B .385963 -.030699 -.100591 ? H68C .238620 .010622 -.105382 ? H69A .505644 .152651 -.164980 ? H69B .485883 .202511 -.083441 ? H69C .531761 .081602 -.086966 ? H70A .276798 .228258 -.169319 ? H70B .153034 .207317 -.095289 ? H70C .253234 .278384 -.087427 ? H32A -.044855 .223337 .335858 ? H32B -.166379 .188435 .406152 ? H33A -.007862 .222879 .462597 ? H33B -.019078 .336485 .417147 ? H33C -.140602 .301583 .487441 ? H72A .321611 -.015274 .303254 ? H72B .233448 -.094529 .292645 ? H73A .222992 -.096168 .430589 ? H73B .170849 .024479 .424502 ? H73C .082686 -.054777 .413893 ? H20A -.082097 .551741 .202252 ? H20B -.130674 .505120 .293980 ? H40A -.428484 .176964 .295226 ? H40B -.361196 .199214 .360765 ? H60A .050333 -.103082 .136587 ? H60B .124145 -.130659 .206540 ? H80A .329485 .165029 .255642 ? H80B .425652 .212190 .175620 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C21 O31 C32 117.6(3) yes C61 O71 C72 115.6(3) yes C2 C1 C6 121.0(4) yes C1 C2 C3 118.6(3) yes C1 C2 C80 123.3(4) yes C3 C2 C80 118.1(4) yes C2 C3 C4 122.3(4) yes C3 C4 C5 117.0(4) yes C3 C4 C7 120.1(4) yes C5 C4 C7 122.9(3) yes C4 C5 C6 122.5(4) yes C1 C6 C5 118.6(4) yes C1 C6 C20 122.7(4) yes C5 C6 C20 118.7(3) yes C4 C7 C8 109.4(4) yes C4 C7 C9 113.2(4) yes C4 C7 C10 110.1(5) yes C8 C7 C9 106.7(4) yes C8 C7 C10 105.3(5) yes C9 C7 C10 111.8(5) yes C6 C20 C22 116.2(3) yes O31 C21 C26 121.3(4) yes O31 C21 C22 118.1(4) yes C26 C21 C22 120.4(4) yes C21 C26 C25 118.3(4) yes C21 C26 C40 121.9(4) yes C25 C26 C40 119.9(4) yes C26 C25 C24 123.7(4) yes C25 C24 C23 115.7(4) yes C25 C24 C27 122.8(4) yes C23 C24 C27 121.5(4) yes C24 C23 C22 123.0(4) yes C20 C22 C21 121.1(4) yes C20 C22 C23 120.0(4) yes C21 C22 C23 118.8(4) yes C24 C27 C28 113.6(4) yes C24 C27 C29 111.6(4) yes C24 C27 C30 109.2(4) yes C28 C27 C29 107.6(5) yes C28 C27 C30 109.5(5) yes C29 C27 C30 105.0(5) yes O31 C32 C33 110.8(6) yes C26 C40 C42 115.1(3) yes C42 C41 C46 120.6(4) yes C40 C42 C41 122.2(4) yes C40 C42 C43 118.9(3) yes C41 C42 C43 119.0(4) yes C42 C43 C44 122.9(4) yes C43 C44 C45 116.5(4) yes C43 C44 C47 120.9(4) yes C45 C44 C47 122.6(4) yes C44 C45 C46 122.7(4) yes C41 C46 C45 118.3(3) yes C41 C46 C60 122.1(3) yes C45 C46 C60 119.4(3) yes C44 C47 C48 110.5(6) yes C44 C47 C49 111.2(5) yes C44 C47 C50 113.4(5) yes C48 C47 C49 102.3(7) yes C48 C47 C50 107.8(7) yes C49 C47 C50 111.1(7) yes C46 C60 C62 118.6(4) yes O71 C61 C62 120.3(4) yes O71 C61 C66 118.6(4) yes C62 C61 C66 121.1(4) yes C60 C62 C61 122.4(5) yes C60 C62 C63 119.4(5) yes C61 C62 C63 118.1(4) yes C62 C63 C64 123.4(5) yes C63 C64 C65 115.4(4) yes C63 C64 C67 122.9(5) yes C65 C64 C67 121.7(4) yes C64 C65 C66 123.8(4) yes C61 C66 C65 118.1(4) yes C61 C66 C80 121.4(4) yes C65 C66 C80 120.5(4) yes C64 C67 C68 112.2(5) yes C64 C67 C69 111.5(5) yes C64 C67 C70 110.5(4) yes C68 C67 C69 104.3(5) yes C68 C67 C70 109.6(6) yes C69 C67 C70 108.7(5) yes O71 C72 C73 110.0(5) yes C2 C80 C66 117.7(4) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O31 C21 1.375(6) yes O31 C32 1.433(6) yes O71 C61 1.388(5) yes O71 C72 1.418(7) yes C1 C2 1.388(6) yes C1 C6 1.378(5) yes C2 C3 1.381(7) yes C2 C80 1.506(5) yes C3 C4 1.386(5) yes C4 C5 1.385(6) yes C4 C7 1.530(7) yes C5 C6 1.383(7) yes C6 C20 1.513(6) yes C7 C8 1.523(7) yes C7 C9 1.497(6) yes C7 C10 1.475(9) yes C20 C22 1.504(7) yes C21 C26 1.391(7) yes C21 C22 1.382(6) yes C26 C25 1.379(7) yes C26 C40 1.508(6) yes C25 C24 1.380(5) yes C24 C23 1.392(7) yes C24 C27 1.520(7) yes C23 C22 1.379(7) yes C27 C28 1.485(9) yes C27 C29 1.526(7) yes C27 C30 1.498(7) yes C32 C33 1.44(2) yes C40 C42 1.529(5) yes C41 C42 1.376(6) yes C41 C46 1.394(5) yes C42 C43 1.374(6) yes C43 C44 1.387(6) yes C44 C45 1.384(5) yes C44 C47 1.515(6) yes C45 C46 1.382(6) yes C46 C60 1.506(6) yes C47 C48 1.500(10) yes C47 C49 1.460(10) yes C47 C50 1.433(8) yes C60 C62 1.513(6) yes C61 C62 1.386(8) yes C61 C66 1.390(6) yes C62 C63 1.375(6) yes C63 C64 1.392(6) yes C64 C65 1.390(8) yes C64 C67 1.530(6) yes C65 C66 1.369(7) yes C66 C80 1.507(7) yes C67 C68 1.517(9) yes C67 C69 1.524(7) yes C67 C70 1.496(9) yes C72 C73 1.455(9) yes C1 H1 0.950(5) no C3 H3 0.951(4) no C5 H5 0.951(4) no C8 H8A 0.951(7) no C8 H8B 0.951(6) no C8 H8C 0.950(7) no C9 H9A 0.951(7) no C9 H9B 0.950(7) no C9 H9C 0.950(6) no C10 H10A 0.950(8) no C10 H10B 0.951(6) no C10 H10C 0.951(6) no C20 H20A 0.950(4) no C20 H20B 0.951(5) no C23 H23 0.950(5) no C25 H25 0.951(4) no C28 H28A 0.951(7) no C28 H28B 0.950(7) no C28 H28C 0.951(6) no C29 H29A 0.951(8) no C29 H29B 0.950(7) no C29 H29C 0.950(9) no C30 H30A 0.951(7) no C30 H30B 0.950(10) no C30 H30C 0.950(8) no C32 H32A 0.951(5) no C32 H32B 0.950(6) no C33 H33A 0.951(7) no C33 H33B 0.950(8) no C33 H33C 0.951(6) no C40 H40A 0.951(6) no C40 H40B 0.950(5) no C41 H41 0.950(4) no C43 H43 0.951(4) no C45 H45 0.950(4) no C48 H48A 0.950(7) no C48 H48B 0.96(2) no C48 H48C 0.951(7) no C49 H49A 0.950(9) no C49 H49B 0.950(8) no C49 H49C 0.950(10) no C50 H50A 0.951(8) no C50 H50B 0.960(10) no C50 H50C 0.950(10) no C60 H60A 0.950(6) no C60 H60B 0.950(5) no C63 H63 0.950(6) no C65 H65 0.951(4) no C68 H68A 0.950(6) no C68 H68B 0.950(7) no C68 H68C 0.950(10) no C69 H69A 0.950(7) no C69 H69B 0.950(8) no C69 H69C 0.950(6) no C70 H70A 0.950(7) no C70 H70B 0.950(7) no C70 H70C 0.950(9) no C72 H72A 0.950(7) no C72 H72B 0.950(6) no C73 H73A 0.951(9) no C73 H73B 0.96(2) no C73 H73C 0.95(2) no C80 H80A 0.950(4) no C80 H80B 0.950(4) no _journal_paper_doi 10.1107/S0108270194014150