#------------------------------------------------------------------------------ #$Date: 2008-01-26 14:05:32 +0100 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003380.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_2003380 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 663 _journal_page_last 666 _publ_section_title ; [Aib^5,6^-D-Ala^8^]-Cyclolinopeptide A Grown from a Benzene/Acetonitrile Mixture ; _chemical_formula_moiety 'C50 H71 N9 O9,C2 H3 N1,2(H2 O1)' _chemical_formula_sum 'C52 H78 N10 O11' _chemical_formula_weight 1019.2 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '1/2-x,-y,1/2+z' '-x,1/2+y,1/2-z' '1/2+x,1/2-y,-z' _symmetry_space_group_name_H-M 'P 21 21 21' _cell_length_a 29.835(5) _cell_length_b 19.784(2) _cell_length_c 9.913(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5851(1) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.157 _exptl_crystal_density_meas ? _diffrn_radiation_type 'CuK\a' _diffrn_radiation_wavelength 1.54056 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 20 _cell_measurement_theta_max 24 _exptl_absorpt_coefficient_mu 0.573 _cell_measurement_temperature 293 _exptl_crystal_description 'Needle' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_size_rad ? _exptl_crystal_colour 'Colourless' _chemical_compound_source ; Slow evaporation from benzene and acetonitrile solution ; _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\w-2\q' _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 5786 _reflns_number_total 5754 _reflns_number_observed 4162 _reflns_observed_criterion I>=3.0\s(I) _diffrn_reflns_av_R_equivalents '?' _diffrn_reflns_theta_max 70 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 3 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.068 _refine_ls_wR_factor_obs 0.071 _refine_ls_goodness_of_fit_obs 2.18 _refine_ls_number_reflns 4162 _refine_ls_number_parameters 658 _refine_ls_hydrogen_treatment 'noref' _refine_ls_weighting_scheme 'w = 1/\s^2^(F~o~)' _refine_ls_shift/esd_max 0.19 _refine_diff_density_max 0.36 _refine_diff_density_min -0.20 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _atom_type_scat_source 'IntTabIV' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_B_iso_or_equiv N1 .1449(1) .3088(2) .7989(5) 3.53(8) C1a .1658(2) .3619(3) .7220(7) 3.89(8) C1b .1448(2) .4273(4) .7809(9) 5.29(9) C1g .1289(4) .4065(5) .9198(11) 8.71(9) C1d .1172(2) .3349(4) .9105(8) 5.07(9) C1 .2175(2) .3616(3) .7450(7) 3.90(8) O1 .2337(1) .3342(2) .8429(5) 5.12(8) N2 .2421(2) .3952(3) .6528(6) 4.01(8) C2a .2256(2) .4382(3) .5431(7) 4.26(8) C2b .2634(3) .4901(4) .5290(9) 6.08(9) C2g .3047(2) .4507(4) .5628(8) 5.69(9) C2d .2910(2) .4051(4) .6791(9) 5.29(9) C2 .2164(2) .4019(3) .4111(7) 4.15(8) O2 .1939(2) .4318(3) .3261(6) 6.92(8) N3 .2329(2) .3415(3) .3910(5) 3.85(8) C3a .2276(2) .3081(3) .2621(6) 4.17(8) C3b .2704(2) .2693(4) .2205(8) 5.22(9) C3g .3100(2) .3155(4) .2002(7) 4.32(8) C31d .3440(3) .3187(5) .2978(8) 5.96(9) C32d .3137(2) .3551(4) .0867(8) 5.20(9) C31e .3804(3) .3634(5) .2794(10) 7.13(9) C32e .3505(3) .3978(4) .0698(9) 6.02(9) C3z .3839(3) .4003(4) .1673(10) 6.62(9) C3 .1881(2) .2591(3) .2571(7) 4.28(8) O3 .1645(2) .2550(3) .1562(5) 6.15(8) N4 .1809(2) .2214(3) .3677(5) 3.72(8) C4a .1485(2) .1662(3) .3668(6) 3.66(8) C4b .1667(2) .1054(4) .4398(7) 4.65(8) C4g .2024(3) .0702(4) .3586(7) 4.98(9) C41d .2465(3) .0920(4) .3616(9) 6.14(9) C42d .1912(3) .0175(4) .2720(9) 6.80(9) C41e .2794(3) .0629(5) .2771(11) 7.99(9) C42e .2244(4) -.0123(5) .1875(10) 7.92(9) C4z .2656(4) .0129(6) .1948(10) 8.56(9) C4 .1026(2) .1900(3) .4185(6) 3.83(8) O4 .0828(1) .1623(2) .5128(4) 4.03(7) N5 .0854(2) .2407(3) .3483(6) 4.39(8) C5a .0425(2) .2726(3) .3824(7) 4.51(8) C51b .0478(3) .3120(4) .5140(8) 6.02(9) C52b .0291(3) .3211(4) .2668(9) 6.25(9) C5 .0054(2) .2189(4) .3928(7) 4.43(8) O5 -.0231(1) .2209(3) .4837(5) 5.35(7) N6 .0060(2) .1715(3) .2971(5) 4.41(8) C6a -.0286(2) .1196(4) .2799(7) 5.42(8) C61b -.0108(3) .0674(5) .1770(8) 7.17(9) C62b -.0706(3) .1511(6) .2290(10) 8.44(9) C6 -.0369(2) .0802(4) .4108(7) 4.59(8) O6 -.0729(1) .0520(3) .4306(5) 6.15(8) N7 -.0016(2) .0714(3) .4910(5) 3.83(8) C7a -.0038(2) .0297(3) .6098(6) 4.11(8) C7b .0256(3) -.0336(4) .5985(7) 5.20(9) C71g .0739(3) -.0161(4) .5803(9) 6.60(9) C72g .0082(3) -.0772(4) .4835(9) 6.42(9) C7d .1059(4) -.0767(7) .5903(14) 11.90(9) C7 .0045(2) .0701(4) .7383(6) 4.27(8) O7 .0130(2) .0410(3) .8453(5) 6.18(8) N8 .0013(2) .1374(3) .7307(5) 3.84(8) C8a .0030(2) .1776(4) .8551(6) 4.36(8) C8b -.0175(3) .2453(5) .8342(8) 6.45(9) C8 .0511(2) .1856(3) .9106(6) 4.17(8) O8 .0559(1) .1977(3) 1.0309(4) 5.47(7) N9 .0849(2) .1827(3) .8214(5) 3.72(8) C9a .1318(2) .1906(3) .8609(6) 3.70(8) C9b .1576(2) .1244(3) .8583(7) 4.52(8) C91g .1338(3) .0709(4) .9399(8) 5.99(9) C92g .2047(3) .1348(4) .9140(9) 6.59(9) C9 .1523(2) .2439(3) .7698(6) 3.39(8) O9 .1753(1) .2289(2) .6694(4) 4.31(7) O1w -.1038(3) -.0373(5) .2096(10) 13.40(9) O2w .0853(5) -.1128(9) .0163(16) 28.05(9) N1s .2325(3) -.2352(4) .0743(7) 7.42(9) C1s .1988(5) -.2207(9) .1669(14) 16.93(9) C2s .1783(6) -.2027(9) .3164(15) 18.13(9) H1 .1599 .3593 .6264 ? H2 .1194 .4420 .7264 ? H3 .1660 .4632 .7812 ? H4 .1046 .4362 .9531 ? H5 .1532 .4140 .9873 ? H6 .1208 .3099 .9923 ? H7 .0844 .3302 .8882 ? H8 .1963 .4586 .5638 ? H9 .2590 .5268 .5895 ? H10 .2639 .5072 .4387 ? H11 .3292 .4798 .5859 ? H12 .3145 .4235 .4863 ? H13 .3081 .3627 .6787 ? H14 .2980 .4263 .7650 ? H15 .2494 .3194 .4593 ? H16 .2202 .3435 .1982 ? H17 .2642 .2453 .1393 ? H18 .2767 .2379 .2906 ? H19 .3413 .2924 .3787 ? H20 .4033 .3670 .3463 ? H21 .4107 .4270 .1497 ? H22 .3527 .4286 -.0085 ? H23 .2896 .3542 0.0208 ? H24 .1963 .2321 .4489 ? H25 .1435 .1485 .2756 ? H26 .1422 .0738 .4582 ? H27 .1782 .1195 .5244 ? H28 .2550 .1251 .4269 ? H29 .3109 .0781 .2760 ? H30 .2874 -.0088 .1363 ? H31 .2154 -.0490 .1212 ? H32 .1601 .0026 .2687 ? H33 .1016 .2578 .2715 ? H34 .0205 .3349 .5385 ? H35 .0571 .2844 .5853 ? H36 .0703 .3479 .5026 ? H37 .0020 .3434 .2852 ? H38 .0524 .3548 .2546 ? H39 .0268 .2962 .1850 ? H40 .0310 .1698 .2353 ? H41 -.0325 .0323 .1613 ? H42 -.0034 .0872 .0920 ? H43 .0159 .0457 .2113 ? H44 -.0941 .1182 .2241 ? H45 -.0813 .1823 .3055 ? H46 -.0681 .1765 .1546 ? H47 .0255 .0946 .4681 ? H48 -.0326 .0097 .6141 ? H49 .0244 -.0578 .6848 ? H50 .0854 .0174 .6377 ? H51 .0793 .0007 .4859 ? H52 .0281 -.1168 .4763 ? H53 -.0202 -.0901 .4977 ? H54 .0123 -.0521 .4021 ? H55 .1346 -.0770 .5804 ? H56 .0994 -.1016 .6847 ? H57 .0933 -.1182 .5328 ? H58 .0000 .1590 .6454 ? H59 -.0152 .1555 .9195 ? H60 -.0167 .2709 .9141 ? H61 -.0009 .2692 .7650 ? H62 -.0476 .2409 .8035 ? H63 .0785 .1762 .7273 ? H64 .1314 .2027 .9552 ? H65 .1610 .1076 .7640 ? H66 .1491 .0270 .9432 ? H67 .1320 .0845 1.0364 ? H68 .1037 .0621 .9129 ? H69 .2219 .0952 .9109 ? H70 .2194 .1702 .8655 ? H71 .2016 .1493 1.0065 ?