#------------------------------------------------------------------------------ #$Date: 2008-01-26 14:05:32 +0100 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003003.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_2003003 _journal_name_full 'Acta Crystallographica, Section B' _journal_year 1998 _journal_volume B54 _journal_page_first 450 _journal_page_last 455 _chemical_name_common 'gamma-Cyclodextrin methanol' _chemical_formula_moiety 'C48 H80 O40, n C1 H4 O1, m H2 O' _chemical_formula_sum ? _chemical_formula_weight 1530.12 _symmetry_cell_setting 'tetragonal' _symmetry_space_group_name_H-M 'P 4 21 2' _symmetry_space_group_name_Hall 'P 4ab 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y+1/2, x+1/2, z' 'y+1/2, -x+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'y, x, -z' '-y, -x, -z' _cell_length_a 23.808(4) _cell_length_b 23.808(4) _cell_length_c 23.140(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13116(4) _cell_formula_units_Z 6 _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293(2) _exptl_crystal_description 'square bipyramid' _exptl_crystal_colour colourless _exptl_crystal_size_max .5 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .2 _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 4704 _exptl_absorpt_coefficient_mu .994 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54176 _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator Ni-filter _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 6681 _diffrn_reflns_av_R_equivalents .043 _diffrn_reflns_av_sigmaI/netI .0974 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 59.83 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 4.2 _reflns_number_total 5389 _reflns_number_observed 3860 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all .1520 _refine_ls_R_factor_obs .0860 _refine_ls_wR_factor_all .2618 _refine_ls_wR_factor_obs .2201 _refine_ls_goodness_of_fit_all 1.009 _refine_ls_goodness_of_fit_obs 1.339 _refine_ls_restrained_S_all 1.072 _refine_ls_restrained_S_obs 1.325 _refine_ls_number_reflns 5376 _refine_ls_number_parameters 773 _refine_ls_number_restraints 136 _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1241P)^2^], where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/esd_max -.001 _refine_ls_shift/esd_mean .000 _refine_diff_density_max .30 _refine_diff_density_min -.26 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -.2(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0181 .0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0492 .0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Isomorphous structure (Ding, Steiner & Saenger, 1990)' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol C11 .6663(5) .2384(5) .9516(4) .060(3) Uani d . 1 . C H11 .6657(5) .2789(5) .9595(4) .072 Uiso calc R 1 . H C21 .7038(4) .2272(5) .8998(4) .055(3) Uani d . 1 . C H21 .7405(4) .2448(5) .9061(4) .066 Uiso calc R 1 . H C31 .7116(5) .1628(4) .8917(3) .051(3) Uani d . 1 . C H31 .6751(5) .1463(4) .8819(3) .061 Uiso calc R 1 . H C41 .7319(4) .1369(5) .9462(4) .049(3) Uani d . 1 . C H41 .7695(4) .1511(5) .9554(4) .058 Uiso calc R 1 . H C51 .6913(4) .1504(4) .9962(4) .061(3) Uani d D 1 . C H51 .6542(4) .1345(4) .9880(4) .073 Uiso calc R 1 . H C61 .7119(6) .1300(5) 1.0551(4) .093(5) Uani d D 1 . C H611 .6899(6) .1476(5) 1.0854(4) .111 Uiso calc PR .56(2) 1 H H612 .7068(6) .0897(5) 1.0579(4) .111 Uiso calc PR .56(2) 1 H H618 .7209(6) .0903(5) 1.0532(4) .111 Uiso calc PR .44(2) 2 H H619 .7457(6) .1503(5) 1.0660(4) .111 Uiso calc PR .44(2) 2 H O21 .6789(3) .2500(3) .8488(3) .061(2) Uani d . 1 . O O31 .7496(3) .1526(3) .8451(3) .058(2) Uani d . 1 . O O41 .7340(3) .0776(3) .9375(3) .059(2) Uani d . 1 . O O51 .6876(3) .2103(3) .9998(3) .058(2) Uani d . 1 . O O61A .7695(5) .1433(7) 1.0629(5) .071(6) Uani d PDU .56(2) 1 O O61B .6690(9) .1394(10) 1.0968(5) .129(11) Uani d PDU .44(2) 2 O C12 .4482(5) .2844(5) .9505(4) .053(3) Uani d . 1 . C H12 .4188(5) .3126(5) .9570(4) .064 Uiso calc R 1 . H C22 .4844(4) .3039(5) .8996(4) .059(3) Uani d . 1 . C H22 .4986(4) .3418(5) .9072(4) .071 Uiso calc R 1 . H C32 .5332(5) .2643(5) .8894(4) .060(3) Uani d . 1 . C H32 .5191(5) .2270(5) .8791(4) .072 Uiso calc R 1 . H C42 .5684(5) .2609(6) .9467(5) .065(4) Uani d . 1 . C H42 .5845(5) .2977(6) .9558(5) .078 Uiso calc R 1 . H C52 .5294(4) .2417(5) .9955(3) .065(3) Uani d D 1 . C H52 .5145(4) .2043(5) .9869(3) .078 Uiso calc R 1 . H C62 .5576(6) .2416(6) 1.0542(4) .096(5) Uani d D 1 . C H621 .5292(6) .2407(6) 1.0842(4) .115 Uiso calc PR .58(2) 3 H H622 .5806(6) .2082(6) 1.0579(4) .115 Uiso calc PR .58(2) 3 H H628 .5936(6) .2226(6) 1.0517(4) .115 Uiso calc PR .42(2) 4 H H629 .5642(6) .2799(6) 1.0668(4) .115 Uiso calc PR .42(2) 4 H O22 .4500(3) .3042(4) .8467(3) .077(3) Uani d . 1 . O O32 .5683(3) .2854(4) .8443(3) .068(2) Uani d . 1 . O O42 .6123(3) .2205(3) .9378(3) .057(2) Uani d . 1 . O O52 .4830(3) .2819(4) 1.0013(3) .076(2) Uani d . 1 . O O62A .5915(6) .2897(6) 1.0613(5) .080(6) Uani d PDU .58(2) 3 O O62B .5222(9) .2133(10) 1.0946(6) .116(11) Uani d PDU .42(2) 4 O C13 .6360(4) .2569(4) .6272(4) .046(3) Uani d . 1 . C H13 .6725(4) .2744(4) .6193(4) .056 Uiso calc R 1 . H C23 .6104(5) .2853(5) .6784(5) .061(3) Uani d . 1 . C H23 .6073(5) .3253(5) .6693(5) .073 Uiso calc R 1 . H C33 .5500(5) .2626(5) .6875(4) .055(3) Uani d . 1 . C H33 .5515(5) .2230(5) .6992(4) .066 Uiso calc R 1 . H C43 .5172(4) .2681(5) .6329(4) .051(3) Uani d . 1 . C H43 .5129(4) .3079(5) .6230(4) .061 Uiso calc R 1 . H C53 .5468(5) .2380(5) .5848(3) .065(3) Uani d D 1 . C H53 .5501(5) .1984(5) .5958(3) .079 Uiso calc R 1 . H C63 .5165(6) .2406(5) .5261(5) .103(6) Uani d D 1 . C H631 .5356(6) .2164(5) .4986(5) .123 Uiso calc PR .89(2) 5 H H632 .4783(6) .2273(5) .5304(5) .123 Uiso calc PR .89(2) 5 H H638 .4879(6) .2118(5) .5243(5) .123 Uiso calc PR .11(2) 6 H H639 .4984(6) .2769(5) .5217(5) .123 Uiso calc PR .11(2) 6 H O23 .6428(3) .2804(3) .7300(3) .064(2) Uani d . 1 . O O33 .5219(3) .2953(4) .7320(3) .075(2) Uani d . 1 . O O43 .4635(3) .2439(3) .6431(3) .057(2) Uani d . 1 . O O53 .6037(3) .2606(4) .5783(3) .065(2) Uani d . 1 . O O63A .5160(5) .2959(5) .5050(4) .105(5) Uani d PDU .89(2) 5 O O63B .5553(12) .233(2) .4811(6) .04(2) Uiso d PD .11(2) 6 O C14 .7765(5) .0835(4) .6266(4) .054(3) Uani d . 1 . C H14 .8149(5) .0710(4) .6186(4) .065 Uiso calc R 1 . H C24 .7775(5) .1229(4) .6770(5) .052(3) Uani d . 1 . C H24 .8022(5) .1544(4) .6670(5) .062 Uiso calc R 1 . H C34 .7190(5) .1465(4) .6885(4) .059(3) Uani d . 1 . C H34 .6928(5) .1162(4) .6981(4) .071 Uiso calc R 1 . H C44 .7008(5) .1761(4) .6326(4) .050(3) Uani d . 1 . C H44 .7269(5) .2067(4) .6233(4) .060 Uiso calc R 1 . H C54 .7008(5) .1334(5) .5854(4) .064(3) Uani d D 1 . C H54 .6753(5) .1029(5) .5965(4) .076 Uiso calc R 1 . H C64 .6813(6) .1569(6) .5277(4) .102(6) Uani d D 1 . C H641 .6805(6) .1271(6) .4992(4) .122 Uiso calc PR .69(3) 7 H H642 .6435(6) .1717(6) .5316(4) .122 Uiso calc PR .69(3) 7 H H648 .6478(6) .1371(6) .5153(4) .122 Uiso calc PR .31(3) 8 H H649 .6718(6) .1963(6) .5323(4) .122 Uiso calc PR .31(3) 8 H O24 .7986(3) .0978(3) .7287(3) .065(2) Uani d . 1 . O O34 .7194(3) .1886(3) .7336(2) .057(2) Uani d . 1 . O O44 .6452(3) .1980(3) .6415(3) .056(2) Uani d . 1 . O O54 .7555(4) .1106(3) .5778(3) .064(2) Uani d . 1 . O O64A .7173(5) .1994(5) .5093(4) .074(6) Uani d PDU .69(3) 7 O O64B .7233(15) .151(3) .4853(10) .21(3) Uani d PDU .31(3) 8 O C15 .7381(5) .1607(4) .2816(4) .058(3) Uani d . 1 . C H15 .7519(5) .1987(4) .2900(4) .069 Uiso calc R 1 . H C25 .7734(5) .1367(5) .2318(4) .059(3) Uani d . 1 . C H25 .8133(5) .1389(5) .2420(4) .071 Uiso calc R 1 . H C35 .7580(5) .0777(4) .2218(5) .057(3) Uani d . 1 . C H35 .7192(5) .0754(4) .2082(5) .069 Uiso calc R 1 . H C45 .7650(5) .0422(5) .2765(4) .056(3) Uani d . 1 . C H45 .8043(5) .0421(5) .2889(4) .067 Uiso calc R 1 . H C55 .7272(6) .0712(5) .3231(5) .069(4) Uani d . 1 . C H55 .6877(6) .0706(5) .3113(5) .083 Uiso calc R 1 . H C65 .7346(9) .0443(6) .3826(6) .107(6) Uani d . 1 . C H651 .7104(9) .0634(6) .4099(6) .129 Uiso calc R 1 . H H652 .7226(9) .0054(6) .3806(6) .129 Uiso calc R 1 . H O25 .7636(4) .1696(3) .1807(3) .070(2) Uani d . 1 . O O35 .7960(4) .0538(3) .1782(3) .077(3) Uani d . 1 . O O45 .7470(3) -.0117(3) .2661(3) .053(2) Uani d . 1 . O O55 .7465(3) .1279(3) .3304(3) .066(2) Uani d . 1 . O O65 .7910(8) .0463(6) .4033(5) .145(8) Uani d P .85(3) . O C16 .5564(5) .2852(5) .2822(4) .056(3) Uani d . 1 . C H16 .5402(5) .3221(5) .2908(4) .067 Uiso calc R 1 . H C26 .5958(4) .2905(5) .2312(4) .053(3) Uani d . 1 . C H26 .6234(4) .3196(5) .2405(4) .063 Uiso calc R 1 . H C36 .6265(4) .2376(5) .2209(4) .055(3) Uani d . 1 . C H36 .5991(4) .2086(5) .2105(4) .066 Uiso calc R 1 . H C46 .6552(5) .2198(5) .2762(4) .053(3) Uani d . 1 . C H46 .6839(5) .2474(5) .2874(4) .063 Uiso calc R 1 . H C56 .6129(4) .2123(5) .3241(5) .057(3) Uani d . 1 . C H56 .5855(4) .1838(5) .3124(5) .068 Uiso calc R 1 . H C66 .6377(5) .1961(5) .3825(4) .071(4) Uani d . 1 . C H661 .6076(5) .1917(5) .4104(4) .085 Uiso calc R 1 . H H662 .6568(5) .1603(5) .3790(4) .085 Uiso calc R 1 . H O26 .5655(3) .3084(3) .1820(3) .067(2) Uani d . 1 . O O36 .6655(3) .2428(3) .1749(3) .064(2) Uani d . 1 . O O46 .6813(3) .1651(3) .2639(3) .060(2) Uani d . 1 . O O56 .5845(3) .2653(3) .3315(3) .060(2) Uani d . 1 . O O66 .6757(4) .2368(4) .4024(3) .090(3) Uani d . 1 . O OW1 .6734(5) .3826(5) .5460(5) .117(4) Uani d U 1 . O OW2 .4103(8) .4089(9) .1643(10) .240(8) Uani d U 1 . O OW3 .3187(10) .3577(9) .5386(9) .292(12) Uani d U 1 . O OW4 .5922(17) .4669(18) .9644(14) .56(3) Uani d U 1 . O OW5 .4131(15) .3660(16) 1.0689(17) .38(3) Uani d PU .80(4) . O OW6 .587(2) .513(3) .4460(18) .54(4) Uani d PU .75(4) . O OW7 .5685(12) .4103(13) .3925(13) .239(19) Uani d PU .69(4) . O OW8 .5774(16) .4586(16) .2877(17) .34(3) Uani d PU .70(4) . O OW9 .5836(9) .4040(8) .8337(12) .117(12) Uani d PU .56(3) . O OW10 .972(2) .340(2) .202(2) .40(4) Uani d PU .57(4) . O OW11 .435(2) .423(2) .290(3) .35(4) Uani d PU .58(5) . O OW12 .4512(19) .394(2) .367(2) .32(3) Uani d PU .58(5) . O OW13 .3599(16) .0872(16) .7882(15) .18(2) Uani d PU .39(3) . O OW14 .613(2) .386(2) .876(3) .09(2) Uiso d P .18(3) . O OW15 .575(6) -.006(7) .341(4) .29(8) Uiso d P .15(2) . O OW16 .0000 .5000 .190(3) .07(3) Uiso d SP .18(4) . O OW17 1.0000 .0000 .146(5) .29(9) Uiso d SP .23(5) . O 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 C11 .062(8) .081(9) .036(5) -.019(7) -.015(5) .011(5) C21 .037(6) .084(9) .043(5) .002(6) -.004(5) -.002(5) C31 .065(7) .057(7) .031(5) -.012(6) .004(5) -.022(5) C41 .054(7) .063(7) .029(5) -.005(6) -.004(5) -.010(5) C51 .084(9) .051(7) .048(6) -.024(6) -.004(6) -.006(5) C61 .179(17) .067(9) .033(6) .023(11) .004(9) .011(6) O21 .062(5) .068(5) .052(4) -.001(4) -.001(4) .011(4) O31 .056(5) .066(5) .051(4) -.002(4) .007(4) -.002(4) O41 .082(6) .047(5) .049(4) .002(4) -.004(4) -.003(4) O51 .063(5) .071(5) .041(3) -.006(4) -.001(3) -.002(4) O61A .071(11) .087(11) .056(8) .007(8) -.008(7) -.021(7) O61B .176(19) .140(17) .070(12) .042(15) .007(12) -.035(12) C12 .056(7) .060(8) .043(6) .002(6) -.006(5) -.009(5) C22 .045(7) .068(8) .064(6) -.010(6) -.017(6) -.006(6) C32 .071(8) .069(8) .041(5) .001(7) -.006(5) -.009(6) C42 .062(8) .085(9) .049(6) -.025(8) -.003(6) .004(6) C52 .074(8) .093(10) .029(5) .006(7) .011(5) -.016(6) C62 .082(10) .176(17) .029(6) -.025(11) .003(6) .001(8) O22 .052(5) .120(8) .060(4) .013(5) -.006(4) .008(5) O32 .062(5) .095(6) .048(4) -.019(5) .003(4) .006(4) O42 .038(4) .082(6) .052(4) -.002(4) .005(3) -.003(4) O52 .072(6) .102(7) .054(4) -.002(5) -.003(4) -.029(5) O62A .069(10) .132(13) .038(7) -.026(9) .004(6) -.009(7) O62B .132(18) .130(18) .087(13) .019(14) -.019(12) .011(13) C13 .048(6) .020(5) .071(7) -.005(5) -.011(5) .021(5) C23 .080(9) .034(7) .070(7) .010(6) -.003(7) .003(6) C33 .060(8) .065(8) .040(5) -.009(6) -.002(5) -.005(5) C43 .036(6) .075(8) .042(5) -.023(6) -.002(5) .014(5) C53 .060(8) .103(10) .033(5) -.005(7) .014(5) .001(6) C63 .086(11) .156(17) .066(7) .042(11) -.015(8) -.027(10) O23 .056(5) .074(6) .061(5) .007(4) -.021(4) -.012(4) O33 .068(6) .094(7) .062(4) .018(5) -.002(4) -.025(5) O43 .065(5) .063(5) .044(4) -.005(4) -.001(3) .012(4) O53 .061(5) .091(6) .043(4) -.001(5) .003(4) .025(4) O63A .108(9) .114(9) .093(6) .005(7) -.015(7) .032(7) C14 .061(7) .047(7) .055(6) -.016(6) .007(6) .017(5) C24 .055(7) .044(7) .057(7) .001(6) .011(6) -.003(5) C34 .093(10) .032(6) .052(6) -.001(6) .013(6) -.002(5) C44 .063(8) .043(6) .043(5) .003(6) .003(5) .003(5) C54 .080(9) .071(8) .040(5) .009(7) -.007(6) .011(5) C64 .129(14) .124(14) .052(6) .058(12) .003(8) .004(8) O24 .071(5) .078(6) .048(4) .006(5) -.027(4) .000(4) O34 .072(5) .060(5) .040(3) .000(4) -.008(3) .001(3) O44 .066(5) .068(5) .033(3) -.010(4) .001(3) -.003(3) O54 .086(6) .071(5) .034(4) .021(5) .010(4) .005(3) O64A .081(9) .081(10) .059(7) .007(7) .003(6) .019(6) O64B .22(3) .21(4) .21(3) .00(2) -.00(2) .01(2) C15 .081(9) .033(6) .059(7) -.022(6) .006(6) .000(5) C25 .051(7) .068(8) .057(7) -.016(6) -.012(6) .011(6) C35 .067(8) .042(7) .063(6) .011(6) .001(6) .006(5) C45 .060(8) .068(8) .040(5) .018(7) .003(5) .006(5) C55 .100(11) .060(8) .048(6) .007(7) .008(7) .008(6) C65 .174(19) .079(10) .069(8) .015(11) -.004(11) .038(8) O25 .086(6) .067(5) .057(4) -.007(5) -.011(4) .013(4) O35 .094(7) .066(5) .073(5) .001(5) .034(5) .000(4) O45 .053(5) .036(4) .069(4) -.002(4) -.011(4) .009(4) O55 .083(6) .052(5) .063(5) .015(5) -.003(4) .017(4) O65 .188(18) .148(13) .099(10) .025(12) -.027(10) .046(9) C16 .057(7) .068(8) .042(5) -.002(6) -.011(5) .001(5) C26 .050(7) .061(8) .048(6) -.007(6) -.005(5) .005(6) C36 .044(7) .077(9) .043(5) -.012(6) .005(5) .012(6) C46 .072(8) .051(7) .036(5) .010(6) -.013(5) -.009(5) C56 .046(7) .067(8) .058(6) -.007(6) -.006(6) .003(6) C66 .081(9) .086(9) .045(6) .005(8) .020(6) .013(6) O26 .073(5) .070(5) .056(4) .010(4) -.015(4) .012(4) O36 .071(5) .075(6) .045(4) -.006(5) .006(4) .008(4) O46 .049(5) .058(5) .071(4) -.005(4) -.013(4) -.003(4) O56 .061(5) .079(6) .039(4) .003(5) -.008(3) .001(4) O66 .087(7) .119(8) .065(5) -.038(6) -.028(5) .025(5) OW1 .127(7) .120(7) .102(6) -.039(6) -.005(6) .017(5) OW2 .227(11) .244(11) .248(12) .021(9) .012(9) .039(9) OW3 .295(14) .296(14) .283(14) .026(10) -.025(9) -.004(9) OW4 .57(3) .57(3) .55(3) .003(11) .004(11) -.006(11) OW5 .39(3) .39(3) .38(3) .018(10) -.020(10) -.002(10) OW6 .54(5) .54(5) .54(5) .000(11) -.008(11) .003(11) OW7 .23(2) .25(2) .24(2) .014(10) .018(10) .005(10) OW8 .34(3) .35(3) .33(3) .013(10) .006(10) .004(10) OW9 .097(15) .099(14) .156(18) -.023(10) .043(13) -.001(12) OW10 .40(4) .40(4) .39(4) .004(11) .002(11) .000(11) OW11 .35(4) .35(4) .35(4) .000(11) -.001(11) .003(11) OW12 .32(4) .32(4) .32(4) .001(10) -.007(10) -.007(11) OW13 .18(2) .18(2) .17(2) .002(10) .003(10) -.009(10)