#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003767.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_2003767 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1995 _journal_volume 51 _journal_page_first 1609 _journal_page_last 1614 _publ_section_title ; The Cyclic Depsipeptide Backbone of the Didemnins ; _chemical_formula_moiety 'C42 H66 Br N5 O11, H2 O' _chemical_formula_sum 'C42 H68 Br N5 O12' _chemical_formula_weight 914.95 _symmetry_cell_setting monoclinic _space_group_IT_number 4 _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _[local]_cod_cif_authors_sg_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,y+1/2,-z' _cell_length_a 13.663(4) _cell_length_b 15.342(3) _cell_length_c 23.557(5) _cell_angle_alpha 90. _cell_angle_beta 97.64(3) _cell_angle_gamma 90. _cell_volume 4894(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_meas ? _diffrn_radiation_type 'CuK\a' _diffrn_radiation_wavelength 1.54184 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.5 _cell_measurement_theta_max 32.8 _exptl_absorpt_coefficient_mu 1.627 _cell_measurement_temperature 298 _exptl_crystal_description 'plate' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.05 _exptl_crystal_size_rad ? _exptl_crystal_colour 'clear' _chemical_compound_source 'MeOH evaporation' _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 9007 _reflns_number_total 8610 _reflns_number_observed 5138 _reflns_observed_criterion F^2^>3\s(F^2^) _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_theta_max 65 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 58.33 _diffrn_standards_decay_% 18.0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.065 _refine_ls_wR_factor_obs 0.077 _refine_ls_goodness_of_fit_obs 2.49 _refine_ls_number_reflns 5138 _refine_ls_number_parameters 558 _refine_ls_hydrogen_treatment 'noref' _refine_ls_weighting_scheme '1/\s^2^(F)' _refine_ls_shift/esd_max 0.11 _refine_diff_density_max 0.56 _refine_diff_density_min -0.43 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _atom_type_scat_source 'MolEN (Fair, 1990)' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_B_iso_or_equiv Br .07942(8) 0 .49987(6) 8.41(3) C1 -.4040(7) .1380(6) .4174(4) 6.9(3) C3 -.3005(6) .0446(6) .4795(4) 6.0(2) C4 -.1922(7) .0527(6) .5004(4) 5.9(2) C5 -.1716(6) .1034(7) .5592(3) 5.9(2) C7 -.1394(7) .2497(7) .6005(4) 6.2(2) C8 -.0421(7) .2947(6) .5925(4) 6.3(2) C9 .0403(7) .2319(7) .5992(4) 6.9(3) C10 .1376(7) .2680(7) .5879(4) 6.4(2) C12 .3072(8) .2331(8) .5963(5) 9.3(3) C13 .3221(7) .2379(7) .5358(5) 7.7(3) C14 .2638(6) .1794(7) .4921(4) 6.5(2) C15 .1902(6) .2339(6) .4494(4) 5.7(2) C17 .0353(6) .2195(7) .3816(4) 6.0(2) C18 -.0562(6) .2562(6) .4054(4) 5.1(2) C20 -.1966(6) .3516(6) .3894(4) 5.8(2) C21 -.2746(6) .2781(6) .3840(3) 5.3(2) C23 -.4379(6) .2285(6) .4026(4) 5.7(2) C25 -.3636(7) .0079(7) .5205(4) 7.4(3) C28 -.2281(7) .3135(7) .6024(4) 8.6(3) C29 -.2223(9) .3480(11) .6638(6) 13.4(5) C30 -.3085(12) .4196(14) .6660(7) 16.9(6) C31 -.3248(9) .2642(11) .5821(6) 11.5(4) C34 .3729(8) .1614(12) .6294(5) 11.4(4) C35 .3529(11) .1500(15) .6919(5) 15.3(6) C36 .4569(13) .1568(17) .6255(7) 31.9(7) C38 .3260(8) .1293(9) .4572(6) 11.2(4) C40 .0012(8) .1465(7) .3425(4) 7.3(3) C41 .0820(9) .0913(10) .3170(5) 10.7(4) C42 .0300(11) .0291(11) .2689(5) 13.6(5) C43 .1478(9) .1498(14) .2888(5) 14.9(6) C45 -.0830(8) .3565(8) .3190(5) 8.5(3) C46 -.1795(9) .3972(9) .2921(6) 10.3(4) C47 -.2232(8) .4274(7) .3474(5) 8.5(3) C49 -.3765(7) .3742(7) .4419(4) 7.6(3) C50 -.4954(7) .2300(7) .3403(4) 6.5(2) C51 -.5351(6) .3189(7) .3212(3) 5.9(2) C52 -.4943(6) .3678(7) .2818(4) 6.2(2) C53 -.5322(7) .4460(7) .2610(3) 6.6(2) C54 -.6103(7) .4809(7) .2788(3) 6.5(2) C55 -.6547(7) .4348(8) .3200(4) 7.4(3) C56 -.6150(7) .3568(8) .3407(4) 6.7(2) C58 -.7281(11) .5935(10) .2700(5) 11.6(4) N6 -.1594(5) .1887(5) .5526(3) 5.3(2) N16 .1056(6) .1896(5) .4290(3) 5.8(2) N19 -.1077(5) .3166(5) .3726(3) 5.7(2) N22 -.3576(5) .2936(5) .4121(3) 5.6(2) N26 -.1483(6) -.0334(6) .5127(3) 7.1(2) O2 -.3305(4) .1314(4) .4621(2) 5.7(1) O11 .2101(4) .2093(5) .6056(3) 7.8(2) O24 -.4444(5) .0742(5) .3948(3) 8.4(2) O27 -.1688(6) .0662(5) .6046(2) 8.4(2) O32 -.0213(6) .3686(5) .6268(3) 10.4(2) O33 .1538(5) .3350(5) .5666(3) 8.8(2) O37 .3856(6) .2840(7) .5210(4) 12.6(3) O39 .2073(4) .3086(4) .4329(3) 7.1(2) O44 -.0811(4) .2292(4) .4502(2) 5.8(1) O48 -.2685(4) .2122(4) .3559(2) 6.0(1) O57 -.6466(5) .5553(5) .2538(3) 8.6(2) Ow -.2168(6) -.0015(6) .8612(3) 9.7(2) Br' .07007(7) -.04447(8) .97901(5) 7.03(2) C1' -.4108(6) .0849(7) .9200(4) 5.7(2) C3' -.3049(6) -.0061(6) .9871(4) 5.6(2) C4' -.1942(6) .0019(6) 1.0035(3) 4.6(2) C5' -.1645(6) .0351(5) 1.0629(3) 4.8(2) C7' -.1226(6) .1662(6) 1.1233(4) 5.6(2) C8' -.0242(6) .2180(6) 1.1186(3) 5.7(2) C9' .0555(6) .1599(6) 1.1023(3) 5.4(2) C10' .1430(6) .2104(6) 1.0912(4) 5.4(2) C12' .3161(6) .1946(7) 1.0780(4) 6.9(2) C13' .3387(7) .1586(7) 1.0234(4) 6.7(2) C14' .2614(6) .1184(6) .9798(4) 5.7(2) C15' .1942(5) .1912(6) .9538(3) 4.9(2) C17' .0311(6) .2147(6) .8953(3) 5.1(2) C18' -.0621(5) .2336(5) .9233(3) 4.5(2) C20' -.2136(6) .3147(5) .9188(4) 4.8(2) C21' -.2849(5) .2406(5) .9023(3) 4.4(2) C23' -.4469(6) .1734(6) .9050(3) 5.1(2) C25' -.3624(7) -.0379(7) 1.0339(4) 7.7(3) C28' -.2033(7) .2209(7) 1.1437(4) 7.3(3) C29' -.2859(8) .1657(9) 1.1573(5) 9.8(3) C30' -.3478(10) .2071(11) 1.1969(6) 12.0(4) C31' -.2364(8) .2938(9) 1.1040(6) 10.3(4) C34' .3934(7) .1800(8) 1.1299(4) 7.3(3) C35' .3668(11) .2262(14) 1.1809(6) 15.9(6) C36' .4071(9) .0876(10) 1.1434(6) 12.7(4) C38' .3034(7) .0676(7) .9325(5) 8.2(3) C40' -.0003(6) .1670(7) .8394(4) 6.2(2) C41' .0821(8) .1612(9) .7988(4) 8.8(3) C42' .0420(11) .1034(11) .7501(5) 13.3(4) C43' .1080(10) .2508(12) .7773(5) 12.6(5) C45' -.0959(7) .3614(7) .8557(4) 7.0(2) C46' -.1833(9) .4133(9) .8452(5) 11.8(4) C47' -.2474(7) .3992(6) .8869(4) 7.0(3) C49' -.4019(7) .3095(7) .9622(4) 7.0(2) C50' -.4884(6) .1790(7) .8406(3) 6.2(2) C51' -.5297(6) .2662(6) .8225(4) 5.9(2) C52' -.4815(8) .3153(9) .7811(4) 8.3(3) C53' -.5194(10) .3928(10) .7585(5) 11.3(4) C54' -.6131(10) .4195(9) .7767(5) 10.4(4) C55' -.6582(8) .3764(7) .8184(5) 8.4(3) C56' -.6141(7) .2979(8) .8411(4) 7.5(3) C58' -.6873(31) .5250(15) .6968(10) 39(2) N6' -.1565(5) .1227(4) 1.0681(2) 4.6(1) N16' .1037(5) .1629(5) .9357(3) 5.3(2) N19' -.1170(4) .2984(4) .9000(3) 4.8(2) N22' -.3727(5) .2413(4) .9235(3) 4.8(2) N26' -.1534(5) -.0854(5) .9984(3) 6.0(2) O2' -.3402(4) .0804(4) .9677(2) 5.3(1) O11' .2219(4) .1561(4) 1.0896(3) 6.0(1) O24' -.4448(5) .0190(4) .8962(3) 7.9(2) O27' -.1467(5) -.0151(4) 1.1027(2) 7.0(2) O32' .0088(5) .2541(5) 1.1738(2) 7.2(2) O33' .1478(4) .2861(4) 1.0835(3) 7.4(2) O37' .4277(5) .1622(8) 1.0138(3) 11.8(3) O39' .2239(4) .2635(4) .9466(3) 6.2(1) O44' -.0838(4) .1882(4) .9640(2) 5.0(1) O48' -.2648(4) .1826(4) .8697(2) 5.1(1) O57' -.657(1) .4923(7) .7556(4) 17.7(4) Ow' .0318(6) .4297(6) 1.1598(3) 10.7(2) H3 -.3116 .0027 .4497 7 H4 -.1639 .0821 .4715 7 HN6 -.1649 .2120 .5142 6 H7 -.1313 .2209 .6355 8 H8 -.0508 .3183 .5542 7 H9a .0242 .1866 .5723 8 H9b .0480 .2111 .6365 8 H12 .3250 .2915 .6093 10 H14 .2296 .1379 .5114 8 HN16 .0935 .1374 .4472 7 H17 .0660 .2631 .3612 7 H20 -.1905 .3720 .4281 7 H23 -.4805 .2448 .4290 7 H25a -.3427 -.0495 .5317 9 H25b -.3595 .0434 .5544 9 H25c -.4312 .0057 .5037 9 H26a -.0808 -.0289 .5259 8 H26b -.1811 -.0627 .5411 8 H26c -.1580 -.0681 .4785 8 H28 -.2259 .3635 .5777 11 H29a -.1642 .3698 .6778 15 H29b -.2415 .2995 .6883 15 H30a -.3127 .4446 .7029 19 H30b -.3004 .4691 .6403 19 H30c -.3757 .3978 .6522 19 H31a -.3315 .2472 .5413 13 H31b -.3391 .2165 .6033 13 H31c -.3854 .3047 .5816 13 H34 .3557 .0951 .6053 16 H35a .2879 .1346 .6986 17 H35b .3989 .1138 .7165 17 H35c .3638 .2099 .7098 17 H36a .4755 .1757 .5890 24 H36b .4677 .2320 .6429 24 H36c .5027 .1360 .6496 24 H38a .2887 .0921 .4313 13 H38b .3655 .1671 .4374 13 H38c .3723 .0932 .4827 13 H40a -.0420 .1692 .3098 9 H40b -.0374 .1065 .3617 9 H41 .1188 .0515 .3433 14 H42a -.0158 -.0115 .2838 17 H42b -.0094 .0601 .2380 17 H42c .0752 -.0072 .2510 17 H43a .1843 .1885 .3185 17 H43b .2013 .1188 .2731 17 H43c .1167 .1863 .2601 17 H45a -.0331 .3982 .3247 10 H45b -.0644 .3118 .2932 10 H46a -.2195 .3569 .2693 12 H46b -.1656 .4457 .2680 12 H47a -.1932 .4803 .3599 11 H47b -.2916 .4338 .3374 11 H49a -.4339 .3735 .4587 9 H49b -.3207 .3879 .4715 9 H49c -.3789 .4234 .4152 9 H50a -.5515 .1910 .3408 8 H50b -.4549 .2093 .3150 8 H52 -.4362 .3457 .2676 8 H53 -.5010 .4749 .2329 8 H55 -.7119 .4590 .3348 8 H56 -.6468 .3285 .3694 8 H58a -.7472 .6464 .2489 13 H58b -.7863 .5549 .2627 13 H58c -.7214 .6074 .3098 13 H3' -.3175 -.0482 .9579 7 H4' -.1685 .0434 .9793 6 HN6' -.1716 .1577 1.0350 5 H7' -.1114 .1233 1.1525 6 H8' -.0321 .2591 1.0883 7 H9a' .0310 .1284 1.0690 6 H9b' .0738 .1201 1.1331 6 H12' .3119 .2566 1.0761 8 H14' .2266 .0756 .9978 7 HN16' .0825 .1084 .9483 6 H17' .0657 .2664 .8873 6 H20' -.2106 .3192 .9588 5 H23' -.5013 .1851 .9242 6 H25a' -.3375 -.0954 1.0481 9 H25b' -.3519 .0001 1.0675 9 H25c' -.4300 -.0431 1.0222 9 H26a' -.0832 -.0850 1.0089 8 H26b' -.1809 -.1249 1.0239 8 H26c' -.1683 -.1067 .9605 8 H28' -.1754 .2510 1.1768 9 H29a' -.2574 .1115 1.1750 12 H29b' -.3271 .1494 1.1235 12 H30a' -.3999 .1677 1.2049 14 H30b' -.3090 .2202 1.2329 14 H30c' -.3771 .2586 1.1810 14 H31a' -.1817 .3274 1.0945 12 H31b' -.2683 .2694 1.0670 12 H31c' -.2825 .3300 1.1180 12 H34' .4562 .1995 1.1226 9 H35a' .3530 .2894 1.1708 17 H35b' .3003 .2070 1.1898 17 H35c' .4101 .2241 1.2133 17 H36a' .4267 .0550 1.1113 14 H36b' .4565 .0771 1.1755 14 H36c' .3466 .0600 1.1521 14 H38a' .2497 .0421 .9054 10 H38b' .3416 .1024 .9106 10 H38c' .3428 .0189 .9478 10 H40a' -.0549 .1991 .8193 7 H40b' -.0185 .1110 .8467 7 H41' .1450 .1438 .8163 11 H42a' .0251 .0475 .7646 14 H42b' -.0210 .1270 .7302 14 H42c' .0845 .0962 .7227 14 H43a' .1338 .2933 .8101 15 H43b' .1547 .2552 .7519 15 H43c' .0491 .2860 .7594 15 H45a' -.0400 .3967 .8690 8 H45b' -.0826 .3318 .8216 8 H46a' -.2178 .3972 .8083 15 H46b' -.1655 .4726 .8443 15 H47a' -.2424 .4472 .9137 9 H47b' -.3144 .3947 .8700 9 H49a' -.4661 .2979 .9713 9 H49b' -.3564 .3115 .9964 9 H49c' -.4024 .3656 .9439 9 H50a' -.5381 .1366 .8320 7 H50b' -.4353 .1666 .8184 7 H52' -.4223 .2932 .7695 8 H53' -.4869 .4266 .7328 8 H55' -.7163 .3988 .8312 8 H56' -.6433 .2669 .8695 8 H58a' -.7109 .5690 .7142 35 H58b' -.6498 .5000 .6860 35 H58c' -.7487 .4738 .7070 35