#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/70/2007020.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_2007020 loop_ _publ_author_name ' Sybolt Harkema' 'Jan-Dirk van Loon' 'Willem Verboom' 'David N. Reinhoudt' _publ_section_title ; 15,17-Di-2-propenylcalix[4]arene-25,26,27,28-tetrol: Self-Complexation and C---H···O Interactions ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 269 _journal_page_last 271 _journal_volume 54 _journal_year 1998 _chemical_formula_sum 'C34 H32 O4' _chemical_formula_weight 504.6 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_type_scat_source IntTabIV _audit_creation_method 'manual editing of form.cif' _cell_angle_alpha 90. _cell_angle_beta 102.91(2) _cell_angle_gamma 90. _cell_formula_units_Z 4 _cell_length_a 16.206(2) _cell_length_b 8.991(4) _cell_length_c 18.665(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 14.1 _cell_measurement_theta_min 7.0 _cell_volume 2650.9(13) _computing_cell_refinement 'CAD-4 Express' _computing_data_collection 'CAD-4 Express (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD-4 Express' _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 4810 _diffrn_reflns_theta_max 25 _diffrn_standards_decay_% <3 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_description parallelepiped _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.32 _refine_diff_density_min -0.40 _refine_ls_extinction_coef 2.5E-7(4) _refine_ls_extinction_method 'Zachariasen (1963)' _refine_ls_goodness_of_fit_all 0.817 _refine_ls_goodness_of_fit_obs 1.073 _refine_ls_hydrogen_treatment 'H atoms treated as riding atoms except for hydroxyl H atoms' _refine_ls_number_parameters 360 _refine_ls_number_reflns 4666 _refine_ls_R_factor_all 0.184 _refine_ls_R_factor_obs .096 _refine_ls_shift/esd_max 0.02 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'w = 1/\s^2^(F^2^)' _refine_ls_wR_factor_all 0.113 _refine_ls_wR_factor_obs .101 _reflns_number_observed 2444 _reflns_number_total 4666 _reflns_observed_criterion I>\s(I) _[local]_cod_data_source_file ka1242.cif _[local]_cod_data_source_block global _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_original_cell_volume 2651(2) _cod_database_code 2007020 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z O7 .23270(10) .2300(2) .09630(10) O17 .33970(10) .4492(2) .14830(10) O27 .39540(10) .4175(2) .02650(10) O37 .29730(10) .1859(2) -.02330(10) C1 .1473(2) .2705(3) .0828(2) C2 .0925(2) .2068(3) .0229(2) C3 .0072(2) .2451(4) .0117(2) C4 -.0236(2) .3436(4) .0565(2) C5 .0350(2) .4068(4) .1142(2) C6 .1211(2) .3723(3) .1286(2) C9 -.1162(2) .3802(4) .0431(2) C10 .1818(2) .4496(4) .1906(2) C11 .2969(2) .5842(3) .1442(2) C12 .2208(2) .5894(4) .1662(2) C13 .1807(2) .7262(4) .1644(2) C14 .2144(2) .8521(4) .1401(2) C15 .2903(2) .8430(4) .1174(2) C16 .3334(2) .7095(4) .1194(2) C20 .4164(2) .7027(4) .0947(2) C21 .3918(2) .5394(4) -.0192(2) C22 .4047(2) .6809(4) .0126(2) C23 .4044(2) .8014(4) -.0344(2) C24 .3897(2) .7864(4) -.1094(2) C25 .3756(2) .6442(4) -.1388(2) C26 .3752(2) .5193(4) -.0953(2) C29 .3906(2) .9199(4) -.1579(2) C30 .3552(2) .3661(4) -.1290(2) C31 .2364(2) .2352(3) -.0836(2) C32 .2636(2) .3211(4) -.1358(2) C33 .2019(2) .3685(4) -.1968(2) C34 .1176(2) .3294(4) -.2048(2) C35 .0938(2) .2417(4) -.1521(2) C36 .1519(2) .1940(3) -.0905(2) C40 .1226(2) .1066(3) -.0312(2) C60 -.1643(2) .2964(4) .0888(2) C70 -.1377(3) .2060(5) .1417(2) C80 .4696(3) .9397(4) -.1872(2) C90 .5352(3) .8620(5) -.1756(3) H7 .278(3) .307(5) .124(2) H17 .369(2) .449(4) .105(2) H27 .360(2) .318(5) .001(2) H37 .277(2) .182(5) .018(2) H3 -.0316 .2020 -.0287 H5 .0159 .4769 .1449 H9A -.1408 .3609 -.0071 H9B -.1212 .4831 .0530 H10A .2258 .3822 .2114 H10B .1517 .4773 .2267 H13 .1293 .7330 .1805 H14 .1859 .9448 .1386 H15 .3132 .9297 .1001 H20A .4500 .6239 .1195 H20B .4447 .7947 .1075 H23 .4144 .8981 -.0138 H25 .3662 .6323 -.1906 H29A .3840 1.0066 -.1306 H29B .3440 .9114 -.1989 H30A .3908 .2951 -.0995 H30B .3664 .3670 -.1769 H33 .2180 .4281 -.2335 H34 .0764 .3625 -.2463 H35 .0361 .2137 -.1581 H40A .0774 .0430 -.0537 H40B .1686 .0485 -.0052 H60 -.2239 .3109 .0760 H70A -.1772 .1599 .1654 H70B -.0790 .1857 .1577 H80 .4694 1.0214 -.2195 H90A .5807 .8868 -.1978 H90B .5397 .7785 -.1437 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O7 .0570(10) .0520(10) .0850(10) .0010(10) .0140(10) .0040(10) O17 .0660(10) .0620(10) .0630(10) .0020(10) .0110(10) .0040(10) O27 .0630(10) .0520(10) .0810(10) .0010(10) .0190(10) .0080(10) O37 .0650(10) .0560(10) .0830(10) .0030(10) .0200(10) .0010(10) C1 .054(2) .043(2) .061(2) -.004(2) .0140(10) .008(2) C2 .060(2) .042(2) .062(2) -.012(2) .0230(10) -.001(2) C3 .062(2) .054(2) .059(2) -.013(2) .0210(10) .004(2) C4 .054(2) .053(2) .057(2) .000(2) .0180(10) .001(2) C5 .070(2) .052(2) .056(2) .001(2) .0210(10) .003(2) C6 .058(2) .050(2) .050(2) -.006(2) .0120(10) -.002(2) C9 .075(2) .061(2) .065(2) -.003(2) .024(2) .003(2) C10 .068(2) .061(2) .052(2) -.007(2) .0190(10) .005(2) C11 .056(2) .051(2) .049(2) .005(2) .0010(10) -.004(2) C12 .053(2) .059(2) .043(2) -.007(2) .0090(10) .003(2) C13 .060(2) .061(2) .056(2) .000(2) .0170(10) -.001(2) C14 .077(2) .047(2) .063(2) -.002(2) .017(2) -.005(2) C15 .072(2) .052(2) .055(2) -.005(2) .015(2) .004(2) C16 .055(2) .053(2) .047(2) -.012(2) .0070(10) -.001(2) C20 .056(2) .055(2) .062(2) -.015(2) .009(2) -.001(2) C21 .044(2) .052(2) .064(2) .001(2) .0180(10) .002(2) C22 .040(2) .052(2) .067(2) -.002(2) .0110(10) -.002(2) C23 .060(2) .051(2) .076(2) -.008(2) .020(2) -.005(2) C24 .067(2) .056(2) .065(2) -.005(2) .021(2) .002(2) C25 .065(2) .068(2) .062(2) -.008(2) .0230(10) -.003(2) C26 .048(2) .055(2) .070(2) -.011(2) .0210(10) -.006(2) C29 .095(3) .082(3) .074(2) -.012(2) .021(2) .007(2) C30 .071(2) .060(2) .079(2) -.011(2) .0390(10) -.015(2) C31 .062(2) .039(2) .071(2) -.004(2) .0260(10) -.014(2) C32 .069(2) .046(2) .063(2) -.003(2) .0300(10) -.017(2) C33 .092(2) .060(2) .059(2) -.009(2) .030(2) -.012(2) C34 .075(2) .080(2) .062(2) -.002(2) .020(2) -.019(2) C35 .063(2) .066(2) .072(2) -.003(2) .024(2) -.019(2) C36 .067(2) .036(2) .070(2) -.003(2) .024(2) -.015(2) C40 .062(2) .049(2) .081(2) -.011(2) .025(2) -.013(2) C60 .062(2) .084(3) .087(2) .009(2) .034(2) -.003(2) C70 .113(3) .093(3) .099(2) -.003(3) .056(2) .018(2) C80 .123(3) .073(3) .081(2) -.025(3) .016(2) .005(2) C90 .074(3) .105(3) .179(4) .003(3) .028(3) .020(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O7 C1 1.400(4) yes O7 H7 1.05(4) yes O17 C11 1.392(4) yes O17 H17 1.03(4) yes O27 C21 1.382(4) yes O27 H27 1.11(5) yes O37 C31 1.392(3) yes O37 H37 .91(5) yes C1 C2 1.386(4) yes C1 C6 1.383(4) yes C2 C3 1.394(4) yes C2 C40 1.512(5) yes C3 C4 1.386(5) yes C3 H3 .951 no C4 C5 1.388(4) yes C4 C9 1.501(4) yes C5 C6 1.395(4) yes C5 H5 .950 no C6 C10 1.511(4) yes C9 C60 1.483(6) yes C9 H9A .951 no C9 H9B .950 no C10 C12 1.521(5) yes C10 H10A .950 no C10 H10B .951 no C11 C12 1.387(5) yes C11 C16 1.399(4) yes C12 C13 1.389(5) yes C13 C14 1.378(5) yes C13 H13 .950 no C14 C15 1.390(5) yes C14 H14 .951 no C15 C16 1.386(5) yes C15 H15 .951 no C16 C20 1.517(4) yes C20 C22 1.514(4) yes C20 H20A .951 no C20 H20B .950 no C21 C22 1.400(4) yes C21 C26 1.397(4) yes C22 C23 1.392(5) yes C23 C24 1.374(4) yes C23 H23 .951 no C24 C25 1.390(5) yes C24 C29 1.506(5) yes C25 C26 1.387(5) yes C25 H25 .950 no C26 C30 1.520(4) yes C29 C80 1.511(6) yes C29 H29A .951 no C29 H29B .950 no C30 C32 1.517(4) yes C30 H30A .951 no C30 H30B .950 no C31 C32 1.389(4) yes C31 C36 1.397(4) yes C32 C33 1.404(4) yes C33 C34 1.386(5) yes C33 H33 .951 no C34 C35 1.382(5) yes C34 H34 .950 no C35 C36 1.381(4) yes C35 H35 .950 no C36 C40 1.518(5) yes C40 H40A .950 no C40 H40B .950 no C60 C70 1.277(5) yes C60 H60 .950 no C70 H70A .951 no C70 H70B .950 no C80 C90 1.249(6) yes C80 H80 .950 no C90 H90A .951 no C90 H90B .950 no 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 O7 C1 C2 117.9(3) yes C2 C1 C6 122.9(3) yes O7 C1 C6 119.3(2) yes C1 C2 C40 122.7(3) yes C3 C2 C40 120.3(2) yes C1 C2 C3 117.0(3) yes C2 C3 C4 123.1(3) yes C3 C4 C5 117.0(3) yes C3 C4 C9 121.4(3) yes C5 C4 C9 121.7(3) yes C4 C5 C6 122.7(3) yes C1 C6 C10 122.7(3) yes C5 C6 C10 119.8(3) yes C1 C6 C5 117.4(2) yes C4 C9 C60 115.3(3) yes C6 C10 C12 113.2(2) yes O17 C11 C16 118.7(3) yes C12 C11 C16 122.8(3) yes O17 C11 C12 118.6(3) yes C10 C12 C13 121.1(3) yes C10 C12 C11 121.3(3) yes C11 C12 C13 117.7(3) yes C12 C13 C14 121.3(3) yes C13 C14 C15 119.7(4) yes C14 C15 C16 121.3(4) yes C15 C16 C20 120.2(3) yes C11 C16 C20 122.5(3) yes C11 C16 C15 117.3(3) yes C16 C20 C22 113.2(2) yes O27 C21 C26 119.8(3) yes O27 C21 C22 118.5(3) yes C22 C21 C26 121.7(3) yes C20 C22 C23 121.2(3) yes C20 C22 C21 121.3(3) yes C21 C22 C23 117.5(3) yes C22 C23 C24 122.7(4) yes C23 C24 C29 120.8(3) yes C23 C24 C25 117.9(4) yes C25 C24 C29 121.2(3) yes C24 C25 C26 122.4(3) yes C25 C26 C30 121.4(3) yes C21 C26 C30 120.9(3) yes C21 C26 C25 117.8(3) yes C24 C29 C80 115.8(3) yes C26 C30 C32 113.0(3) yes O37 C31 C32 117.7(3) yes C32 C31 C36 122.7(3) yes O37 C31 C36 119.7(3) yes C30 C32 C31 123.3(2) yes C30 C32 C33 119.5(3) yes C31 C32 C33 117.3(3) yes C32 C33 C34 121.0(4) yes C33 C34 C35 119.6(3) yes C34 C35 C36 121.6(4) yes C31 C36 C40 122.0(2) yes C31 C36 C35 117.9(3) yes C35 C36 C40 120.2(3) yes C2 C40 C36 112.3(3) yes C9 C60 C70 129.6(3) yes C29 C80 C90 129.0(4) yes C1 O7 H7 118(2) yes C11 O17 H17 106(3) yes C21 O27 H27 115(2) yes C31 O37 H37 112(2) yes O7 H7 O17 166(4) yes O17 H17 O27 165(3) yes O27 H27 O37 168(4) yes O7 H37 O37 164(4) yes C2 C3 H3 118.6 no C4 C3 H3 118.5 no C4 C5 H5 118.8 no C6 C5 H5 118.6 no H9A C9 H9B 109.5 no C4 C9 H9A 107.9 no C60 C9 H9A 108.4 no C60 C9 H9B 107.7 no C4 C9 H9B 107.9 no C6 C10 H10A 108.8 no C12 C10 H10B 108.0 no C12 C10 H10A 109.0 no H10A C10 H10B 109.5 no C6 C10 H10B 108.4 no C14 C13 H13 119.6 no C12 C13 H13 119.2 no C15 C14 H14 120.0 no C13 C14 H14 120.3 no C16 C15 H15 119.2 no C14 C15 H15 119.6 no C16 C20 H20A 109.5 no C22 C20 H20A 109.0 no H20A C20 H20B 109.5 no C22 C20 H20B 108.1 no C16 C20 H20B 107.5 no C24 C23 H23 118.5 no C22 C23 H23 118.7 no C26 C25 H25 119.0 no C24 C25 H25 118.7 no C24 C29 H29A 108.2 no C24 C29 H29B 108.0 no C80 C29 H29A 107.7 no C80 C29 H29B 107.7 no H29A C29 H29B 109.5 no C32 C30 H30B 108.3 no C26 C30 H30B 108.2 no H30A C30 H30B 109.5 no C26 C30 H30A 108.8 no C32 C30 H30A 109.0 no C32 C33 H33 119.8 no C34 C33 H33 119.2 no C33 C34 H34 120.4 no C35 C34 H34 120.0 no C36 C35 H35 119.1 no C34 C35 H35 119.4 no C2 C40 H40A 108.8 no C36 C40 H40B 108.6 no C2 C40 H40B 108.7 no C36 C40 H40A 108.9 no H40A C40 H40B 109.5 no C9 C60 H60 114.9 no C70 C60 H60 115.4 no H70A C70 H70B 120.0 no C60 C70 H70A 119.5 no C60 C70 H70B 120.5 no C90 C80 H80 115.2 no C29 C80 H80 115.9 no C80 C90 H90A 120.4 no H90A C90 H90B 120.1 no C80 C90 H90B 119.6 no _journal_paper_doi 10.1107/S0108270197010937