#------------------------------------------------------------------------------ #$Date: 2008-01-27 07:32:27 +0000 (Sun, 27 Jan 2008) $ #$Revision: 23 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000136.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_4000136 _journal_name_full 'Chemistry of Materials' _journal_year 2002 loop_ _publ_author_name 'Homayoun Nozary' 'Claude Piguet' 'Jean-Pierre Rivera' 'Paul Tissot' 'Pierre-Yves Morgantini' 'Jacques Weber' 'Bernardinelli, G\'erald' 'Jean-Claude G. Bnzli' 'Robert Deschenaux' 'Bertrand Donnio' 'Daniel Guillon' _publ_section_title ; Aromatic Bent-Core Liquid Crystals: an Opportunity for Introducing Terdentate Binding Units into Mesophases ; _chemical_formula_moiety ; Lu (C75 H85 N5 O10) (C F3 C O2)3 (H2 O) ; _chemical_formula_sum 'C81 H87 N5 O17 F9 Lu' _chemical_formula_weight 1748.7 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '-x,-y,-z' _cell_length_a 13.6773(11) _cell_length_b 14.6177(11) _cell_length_c 20.809(2) _cell_angle_alpha 75.803(11) _cell_angle_beta 79.667(11) _cell_angle_gamma 89.016(10) _cell_volume 3966.3(7) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_meas not_measured _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7996 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.9 _cell_measurement_temperature 200 _exptl_absorpt_coefficient_mu 1.34 _exptl_crystal_description 'plate' _exptl_crystal_size_max .30 _exptl_crystal_size_mid .11 _exptl_crystal_size_min .04 _exptl_crystal_colour colorless _diffrn_measurement_device_type 'Stoe Ipds' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean 6 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'XRED; Stoe & Cie, 1999' _exptl_absorpt_correction_T_min .7843 _exptl_absorpt_correction_T_max .9517 _diffrn_reflns_number .391100+05 _reflns_number_total .143570+05 _reflns_number_gt 9083 _reflns_threshold_expression 'refl observed if Fo > 4.0 \s(Fo)' _diffrn_reflns_theta_max 25.9 _diffrn_reflns_av_R_equivalents .067 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .041 _refine_ls_wR_factor_ref .04 _refine_ls_goodness_of_fit_ref .989 _refine_ls_number_reflns 9083 _refine_ls_number_parameters 1051 _refine_ls_weighting_scheme calc _refine_ls_weighting_details '\w=1/[\s^2^(Fo)+0.0003(Fo^2^)]' _refine_ls_hydrogen_treatment ; Observed and refined with a fixed value of Uiso for hydrogen atoms of the water molecule. All other H atoms calculated. ; _refine_ls_shift/su_max .019 _refine_diff_density_max 1.195 _refine_diff_density_min -2.265 _refine_ls_extinction_method none _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack none loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Lu .361206(19) .15243(3) .548913(16) .02354(17) 1.00000 Uani O01 .3956(4) -.0036(4) .5617(3) .036(4) 1.00000 Uani O1 .7719(3) .5280(4) .3771(3) .044(4) 1.00000 Uani O2 .8599(3) .4714(4) .4607(3) .046(4) 1.00000 Uani O3 1.1063(3) .8397(4) .2712(3) .047(4) 1.00000 Uani O4 1.2411(4) .7579(4) .2410(3) .051(4) 1.00000 Uani O5 1.3818(4) 1.1920(4) .1220(3) .056(5) 1.00000 Uani O6 -.0367(3) -.2278(4) .7283(3) .040(4) 1.00000 Uani O7 .0389(4) -.3218(4) .6637(3) .049(4) 1.00000 Uani O8 -.3204(4) -.5934(4) .8455(3) .058(5) 1.00000 Uani O9 -.4571(4) -.5145(5) .8254(4) .086(6) 1.00000 Uani O10 -.6277(4) -.9302(4) .9768(3) .063(5) 1.00000 Uani N1 .2326(3) .2657(4) .5086(3) .026(4) 1.00000 Uani N2 .4313(3) .3033(4) .4725(3) .027(4) 1.00000 Uani N3 .4154(3) .4593(4) .4333(3) .026(4) 1.00000 Uani N4 .1920(3) .0885(4) .5841(3) .029(4) 1.00000 Uani N5 .0280(3) .0920(4) .5850(3) .029(4) 1.00000 Uani C1 .2616(4) .3501(4) .4666(3) .026(5) 1.00000 Uani C2 .1980(5) .4061(5) .4279(4) .035(6) 1.00000 Uani C3 .1018(4) .3709(5) .4345(4) .036(5) 1.00000 Uani C4 .0720(4) .2844(5) .4771(4) .035(6) 1.00000 Uani C5 .1381(4) .2324(5) .5147(3) .027(5) 1.00000 Uani C6 .3688(4) .3724(4) .4583(3) .026(5) 1.00000 Uani C7 .5261(4) .3454(5) .4520(4) .029(5) 1.00000 Uani C8 .6207(5) .3065(5) .4473(4) .035(5) 1.00000 Uani C9 .7019(5) .3672(5) .4234(4) .038(6) 1.00000 Uani C10 .6894(5) .4648(5) .4049(4) .034(5) 1.00000 Uani C11 .5981(4) .5068(5) .4061(4) .034(5) 1.00000 Uani C12 .5159(4) .4435(5) .4286(4) .028(5) 1.00000 Uani C13 .8499(4) .5275(5) .4086(4) .034(5) 1.00000 Uani C14 .9193(4) .6080(5) .3718(4) .032(5) 1.00000 Uani C15 1.0123(4) .6140(5) .3901(4) .035(5) 1.00000 Uani C16 1.0785(4) .6888(5) .3551(4) .036(5) 1.00000 Uani C17 1.0481(5) .7579(5) .3041(4) .037(5) 1.00000 Uani C18 .9559(5) .7554(5) .2861(4) .041(6) 1.00000 Uani C19 .8909(5) .6789(5) .3208(4) .041(6) 1.00000 Uani C20 1.2019(5) .8325(6) .2397(4) .039(6) 1.00000 Uani C21 1.2483(5) .9268(5) .2068(3) .033(5) 1.00000 Uani C22 1.3504(5) .9347(5) .1860(4) .041(6) 1.00000 Uani C23 1.3991(5) 1.0216(6) .1579(4) .046(6) 1.00000 Uani C24 1.3426(5) 1.1017(6) .1485(4) .040(6) 1.00000 Uani C25 1.2400(5) 1.0951(6) .1679(4) .046(6) 1.00000 Uani C26 1.1924(5) 1.0082(6) .1978(4) .043(6) 1.00000 Uani C27 1.4887(6) 1.2041(6) .1079(5) .056(7) 1.00000 Uani C28 1.5114(6) 1.3091(6) .0797(4) .055(7) 1.00000 Uani C29 1.6245(5) 1.3296(6) .0576(5) .058(7) 1.00000 Uani C30 1.6479(5) 1.4349(6) .0308(4) .054(7) 1.00000 Uani C31 1.7592(5) 1.4592(6) .0080(5) .058(7) 1.00000 Uani C32 1.7816(5) 1.5647(6) -.0160(4) .047(6) 1.00000 Uani C33 1.8924(5) 1.5892(6) -.0404(4) .052(7) 1.00000 Uani C34 1.9140(5) 1.6956(5) -.0689(4) .049(6) 1.00000 Uani C35 2.0225(5) 1.7252(6) -.0900(5) .055(7) 1.00000 Uani C36 2.0394(6) 1.8313(6) -.1185(4) .054(7) 1.00000 Uani C37 2.1502(7) 1.8620(7) -.1375(5) .076(9) 1.00000 Uani C38 2.1640(9) 1.9685(8) -.1670(6) .106(11) 1.00000 Uani C39 .3750(5) .5538(5) .4115(4) .035(5) 1.00000 Uani C40 .3815(5) .5824(6) .3352(4) .048(6) 1.00000 Uani C41 .1193(4) .1384(5) .5612(4) .028(5) 1.00000 Uani C42 .1487(4) .0035(5) .6242(4) .029(5) 1.00000 Uani C43 .1902(4) -.0767(5) .6600(4) .039(6) 1.00000 Uani C44 .1286(5) -.1551(5) .6932(4) .040(6) 1.00000 Uani C45 .0264(5) -.1499(5) .6913(4) .036(6) 1.00000 Uani C46 -.0179(5) -.0719(5) .6590(4) .034(5) 1.00000 Uani C47 .0473(4) .0052(5) .6248(4) .029(5) 1.00000 Uani C48 -.0267(5) -.3092(5) .7064(4) .035(5) 1.00000 Uani C49 -.1071(5) -.3804(5) .7451(4) .033(5) 1.00000 Uani C50 -.0957(4) -.4732(5) .7403(4) .038(6) 1.00000 Uani C51 -.1701(5) -.5419(5) .7716(4) .043(6) 1.00000 Uani C52 -.2537(5) -.5163(5) .8102(4) .041(6) 1.00000 Uani C53 -.2678(5) -.4246(5) .8159(4) .043(6) 1.00000 Uani C54 -.1932(5) -.3564(5) .7838(4) .041(6) 1.00000 Uani C55 -.4180(6) -.5856(6) .8489(5) .055(7) 1.00000 Uani C56 -.4724(6) -.6765(6) .8842(4) .045(6) 1.00000 Uani C57 -.4251(5) -.7604(6) .9086(4) .052(7) 1.00000 Uani C58 -.4802(5) -.8421(6) .9396(4) .049(6) 1.00000 Uani C59 -.5834(5) -.8413(6) .9462(4) .046(6) 1.00000 Uani C60 -.6312(5) -.7618(6) .9239(5) .056(7) 1.00000 Uani C61 -.5753(6) -.6788(6) .8916(4) .055(7) 1.00000 Uani C62 -.7337(5) -.9385(6) .9878(4) .049(6) 1.00000 Uani C63 -.7593(5) -1.0426(6) 1.0187(5) .056(7) 1.00000 Uani C64 -.8679(6) -1.0687(6) 1.0376(4) .056(7) 1.00000 Uani C65 -.8869(6) -1.1742(6) 1.0695(5) .058(7) 1.00000 Uani C66 -.9944(6) -1.2087(6) 1.0877(4) .052(6) 1.00000 Uani C67 -1.0090(6) -1.3138(6) 1.1192(4) .059(7) 1.00000 Uani C68 -1.1143(6) -1.3496(6) 1.1391(4) .053(6) 1.00000 Uani C69 -1.1288(6) -1.4552(6) 1.1723(5) .060(7) 1.00000 Uani C70 -1.2339(6) -1.4895(6) 1.1945(4) .060(7) 1.00000 Uani C71 -1.2513(6) -1.5950(6) 1.2254(4) .058(7) 1.00000 Uani C72 -1.3584(6) -1.6272(7) 1.2462(5) .070(8) 1.00000 Uani C73 -1.3765(7) -1.7321(8) 1.2718(6) .085(9) 1.00000 Uani C74 -.0734(4) .1180(5) .5734(4) .032(5) 1.00000 Uani C75 -.0984(5) .0895(6) .5128(4) .044(6) 1.00000 Uani C1a .3463(4) .1791(6) .6753(4) .033(6) 1.00000 Uani C2a .3500(5) .1960(6) .7448(4) .043(6) 1.00000 Uani O1a .3423(3) .0959(4) .6709(3) .041(4) 1.00000 Uani O2a .3455(3) .2501(4) .6270(3) .039(4) 1.00000 Uani F1a .3988(4) .1317(5) .7807(3) .079(5) 1.00000 Uani F2a .2585(4) .1924(4) .7803(3) .076(5) 1.00000 Uani F3a .3882(6) .2788(5) .7410(3) .120(7) 1.00000 Uani C1b .6004(4) .1216(5) .5693(4) .034(5) 1.00000 Uani C2b .6444(5) .1405(8) .6277(5) .067(8) 1.00000 Uani O1b .5156(3) .1522(3) .5648(3) .037(4) 1.00000 Uani O2b .6569(3) .0838(4) .5318(3) .040(4) 1.00000 Uani F1b .7084(4) .2140(5) .6047(4) .106(7) 1.00000 Uani F2b .5768(4) .1624(7) .6750(3) .143(8) 1.00000 Uani F3b .6959(4) .0669(5) .6552(3) .100(6) 1.00000 Uani C1c .3899(5) .1272(5) .3903(4) .031(5) 1.00000 Uani C2c .3243(4) .1803(5) .3389(3) .062(9) 1.00000 Uani O1c .3525(4) .1326(4) .4490(3) .055(5) 1.00000 Uani O2c .4656(4) .0929(4) .3690(3) .067(5) 1.00000 Uani F1c .3444(10) .1538(10) .2828(7) .11(3) .50000 Uani F2c .3414(8) .2727(6) .3263(6) .057(9) .50000 Uani F3c .2319(8) .1619(9) .3646(6) .109(17) .50000 Uani F3c' .2400(11) .1359(13) .3505(8) .23(3) .50000 Uani F2c' .3099(15) .2663(14) .3459(8) .23(4) .50000 Uani F1c' .3656(10) .1842(13) .2794(7) .090(14) .50000 Uani H011 .380(5) -.037(6) .535(4) .05000 1.00000 Uiso H012 .456(5) -.039(5) .582(4) .05000 1.00000 Uiso H2 .22266 .47458 .39413 .05000 1.00000 Uiso H3 .04988 .41189 .40534 .05000 1.00000 Uiso H4 -.00335 .25722 .48161 .05000 1.00000 Uiso H8 .62938 .23044 .46218 .05000 1.00000 Uiso H9 .77644 .33889 .41883 .05000 1.00000 Uiso H11 .58992 .58294 .39052 .05000 1.00000 Uiso H15 1.03306 .56035 .43150 .05000 1.00000 Uiso H16 1.15213 .69307 .36748 .05000 1.00000 Uiso H18 .93414 .81109 .24609 .05000 1.00000 Uiso H19 .81777 .67494 .30816 .05000 1.00000 Uiso H22 1.39404 .87075 .19213 .05000 1.00000 Uiso H23 1.47978 1.02678 .14331 .05000 1.00000 Uiso H25 1.19630 1.15865 .15946 .05000 1.00000 Uiso H26 1.11192 1.00330 .21395 .05000 1.00000 Uiso H271 1.51844 1.17875 .15419 .05000 1.00000 Uiso H272 1.52100 1.16519 .07121 .05000 1.00000 Uiso H281 1.47524 1.33447 .03633 .05000 1.00000 Uiso H282 1.48308 1.34626 .11840 .05000 1.00000 Uiso H291 1.66071 1.30262 .10054 .05000 1.00000 Uiso H292 1.65232 1.29393 .01786 .05000 1.00000 Uiso H301 1.61062 1.46127 -.01224 .05000 1.00000 Uiso H302 1.61838 1.47008 .07052 .05000 1.00000 Uiso H311 1.79658 1.43095 .05061 .05000 1.00000 Uiso H312 1.78791 1.42642 -.03289 .05000 1.00000 Uiso H321 1.74239 1.59340 -.05757 .05000 1.00000 Uiso H322 1.75465 1.59733 .02544 .05000 1.00000 Uiso H331 1.93099 1.56426 .00192 .05000 1.00000 Uiso H332 1.92033 1.55304 -.07983 .05000 1.00000 Uiso H341 1.87846 1.71876 -.11270 .05000 1.00000 Uiso H342 1.88119 1.73125 -.03007 .05000 1.00000 Uiso H351 2.05859 1.70340 -.04605 .05000 1.00000 Uiso H352 2.05627 1.68940 -.12836 .05000 1.00000 Uiso H361 2.00553 1.85258 -.16329 .05000 1.00000 Uiso H362 2.00325 1.86710 -.08058 .05000 1.00000 Uiso H371 2.18402 1.84175 -.09274 .05000 1.00000 Uiso H372 2.18678 1.82551 -.17506 .05000 1.00000 Uiso H381 2.13038 1.98853 -.21194 .05000 1.00000 Uiso H382 2.12762 2.00477 -.12962 .05000 1.00000 Uiso H383 2.24261 1.99004 -.18063 .05000 1.00000 Uiso H391 .29739 .55302 .43582 .05000 1.00000 Uiso H392 .41743 .60509 .42643 .05000 1.00000 Uiso H401 .45906 .58336 .31100 .05000 1.00000 Uiso H402 .33902 .53129 .32039 .05000 1.00000 Uiso H403 .35160 .65238 .31915 .05000 1.00000 Uiso H43 .26930 -.07769 .66193 .05000 1.00000 Uiso H44 .15914 -.21937 .72003 .05000 1.00000 Uiso H46 -.09766 -.06973 .65957 .05000 1.00000 Uiso H50 -.02703 -.49241 .71140 .05000 1.00000 Uiso H51 -.16225 -.61388 .76574 .05000 1.00000 Uiso H53 -.33655 -.40557 .84479 .05000 1.00000 Uiso H54 -.20196 -.28413 .78893 .05000 1.00000 Uiso H57 -.34427 -.76080 .90318 .05000 1.00000 Uiso H58 -.44352 -.90721 .95910 .05000 1.00000 Uiso H60 -.71209 -.76254 .93043 .05000 1.00000 Uiso H61 -.61332 -.61447 .87191 .05000 1.00000 Uiso H621 -.76744 -.89621 1.02195 .05000 1.00000 Uiso H622 -.76026 -.91531 .94000 .05000 1.00000 Uiso H631 -.72547 -1.08176 .98239 .05000 1.00000 Uiso H632 -.72662 -1.06377 1.06407 .05000 1.00000 Uiso H641 -.90295 -1.02952 1.07364 .05000 1.00000 Uiso H642 -.90126 -1.04976 .99252 .05000 1.00000 Uiso H651 -.84779 -1.21229 1.03424 .05000 1.00000 Uiso H652 -.85573 -1.19127 1.11570 .05000 1.00000 Uiso H661 -1.03395 -1.17107 1.12330 .05000 1.00000 Uiso H662 -1.02602 -1.19206 1.04182 .05000 1.00000 Uiso H671 -.97043 -1.35085 1.08292 .05000 1.00000 Uiso H672 -.97518 -1.33014 1.16421 .05000 1.00000 Uiso H681 -1.15326 -1.31154 1.17449 .05000 1.00000 Uiso H682 -1.14751 -1.33504 1.09394 .05000 1.00000 Uiso H691 -1.09289 -1.49390 1.13638 .05000 1.00000 Uiso H692 -1.09336 -1.47087 1.21656 .05000 1.00000 Uiso H701 -1.26932 -1.45209 1.23151 .05000 1.00000 Uiso H702 -1.27016 -1.47125 1.15037 .05000 1.00000 Uiso H711 -1.21530 -1.63261 1.18900 .05000 1.00000 Uiso H712 -1.21659 -1.61320 1.27031 .05000 1.00000 Uiso H721 -1.39255 -1.59384 1.28605 .05000 1.00000 Uiso H722 -1.39435 -1.60322 1.20259 .05000 1.00000 Uiso H731 -1.34199 -1.76573 1.23227 .05000 1.00000 Uiso H732 -1.34019 -1.75635 1.31573 .05000 1.00000 Uiso H733 -1.45400 -1.75583 1.28699 .05000 1.00000 Uiso H741 -.12667 .08326 .61795 .05000 1.00000 Uiso H742 -.07939 .19441 .56526 .05000 1.00000 Uiso H751 -.04510 .12439 .46822 .05000 1.00000 Uiso H752 -.09238 .01324 .52091 .05000 1.00000 Uiso H753 -.17311 .10882 .50424 .05000 1.00000 Uiso