#------------------------------------------------------------------------------ #$Date: 2009-11-14 14:09:05 +0100 (Sat, 14 Nov 2009) $ #$Revision: 846 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003382.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_2003382 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 688 _journal_page_last 690 _publ_section_title ; Z-AzPro-AzPro-OBzl ; _chemical_formula_moiety 'C23 H26 N4 O5' _chemical_formula_sum 'C23 H26 N4 O5' _chemical_formula_weight 438.48 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,z+1/2' _symmetry_space_group_name_H-M 'P 21' _cell_length_a 9.386(1) _cell_length_b 27.912(3) _cell_length_c 9.463(1) _cell_angle_alpha 90 _cell_angle_beta 115.27(2) _cell_angle_gamma 90 _cell_volume 2242 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.30 _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 30 _exptl_absorpt_coefficient_mu 0.68 _cell_measurement_temperature 295 _exptl_crystal_description 'parallelepiped' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_size_rad ? _exptl_crystal_colour 'colourless' _chemical_compound_source ? _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w-2\q' _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 4602 _reflns_number_total 4509 _reflns_number_observed 4239 _reflns_observed_criterion I>3\s(I) _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_theta_max 70 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% none _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.031 _refine_ls_wR_factor_obs 0.035 _refine_ls_goodness_of_fit_obs 2.37 _refine_ls_number_reflns 4239 _refine_ls_number_parameters 368 _refine_ls_hydrogen_treatment 'refxyz' _refine_ls_weighting_scheme 'w = 0.0316/[\s^2^(F) + 0.00013F^2^]' _refine_ls_shift/esd_max 0.21 _refine_diff_density_max 0.15 _refine_diff_density_min -0.16 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _atom_type_scat_source 'SHELX76 (Sheldrick, 1976)' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_B_iso_or_equiv C(1A) .2514(3) .177 -.3442(4) 5.49(9) C(2A) .2868(3) .2233(1) -.2975(4) 5.87(9) C(3A) .4273(3) .2350(1) -.1729(3) 5.18(8) C(4A) .5341(3) .19979(9) -.0942(3) 4.04(7) C(5A) .4969(3) .1534(1) -.1444(4) 5.47(9) C(6A) .3581(4) .1419(1) -.2660(4) 6.4(1) C(7A) .6874(3) .2117(1) .0406(3) 4.70(8) O(1A) .6545(2) .21786(7) .1755(2) 4.66(5) C(8A) .7810(3) .22897(9) .3088(3) 4.22(7) O(2A) .9150(2) .22918(7) .3247(2) 5.21(5) N(1A) .7377(2) .23986(8) .4243(2) 4.43(6) C(9A) .8499(3) .2410(1) .5903(3) 4.46(7) C(10A) .7474(3) .2288(1) .6730(3) 5.79(9) C(11A) .6011(3) .2062(1) .5487(3) 4.67(7) N(2A) .5824(2) .23035(8) .4052(2) 3.96(5) C(12A) .4804(3) .26941(9) .3465(3) 3.72(6) O(3A) .5184(2) .30823(7) .3189(2) 5.65(6) N(3A) .3301(2) .25790(7) .3258(2) 3.66(5) C(13A) .2547(3) .2122(1) .2589(3) 4.52(7) C(14A) .1456(3) .2249(1) .0919(3) 5.31(9) C(15A) .0951(3) .2760(1) .0995(3) 4.67(7) N(4A) .2148(2) .29336(7) .2502(2) 3.96(5) C(16A) .1817(3) .32696(9) .3335(3) 4.16(7) O(4A) .0692(2) .35323(7) .2794(2) 5.10(5) O(5A) .2942(2) .32891(6) .4810(2) 5.02(5) C(17A) .2881(5) .3690(1) .5725(4) 7.1(1) C(18A) .4236(3) .36426(9) .7286(3) 4.70(8) C(19A) .5745(4) .3577(1) .7452(4) 5.89(9) C(20A) .6967(4) .3509(1) .8900(4) 6.2(1) C(21A) .6694(4) .3524(1) 1.0197(4) 6.3(1) C(22A) .5214(4) .3589(1) 1.0065(4) 6.7(1) C(23A) .3984(4) .3647(1) .8605(4) 5.85(9) C(1B) -.4687(5) .5192(3) -.2082(5) 8.8(1) C(2B) -.4520(5) .5671(3) -.2053(5) 8.7(1) C(3B) -.3214(4) .5892(2) -.0862(4) 6.9(1) C(4B) -.2087(3) .5617(1) .0249(3) 5.32(7) C(5B) -.2270(4) .5126(1) .0186(5) 6.7(1) C(6B) -.3570(5) .4917(2) -.0975(6) 8.5(1) C(7B) -.0662(4) .5845(1) .1512(4) 6.28(9) O(1B) -.0559(2) .56790(7) .3003(2) 4.81(4) C(8B) .0516(3) .59030(9) .4248(3) 4.63(6) O(2B) .1380(2) .62172(7) .4218(3) 6.40(6) N(1B) .0573(3) .57240(8) .5602(3) 5.36(6) C(9B) .1309(4) .5967(1) .7092(4) 6.41(9) C(10B) .0187(5) .5899(2) .7818(5) 7.6(1) C(11B) -.1170(4) .5612(1) .6682(4) 5.62(8) N(2B) -.0592(3) .54041(7) .5586(2) 4.64(5) C(12B) -.0079(3) .49275(9) .5778(3) 4.05(6) O(3B) .1196(2) .47992(7) .5904(3) 6.11(6) N(3B) -.1223(2) .46290(7) .5828(2) 4.15(5) C(13B) -.2900(3) .4664(1) .4782(4) 5.49(7) C(14B) -.3253(5) .4216(1) .3845(5) 7.3(1) C(15B) -.1930(3) .3876(1) .4633(3) 5.19(7) N(4B) -.0841(2) .41396(7) .6011(2) 4.28(5) C(16B) -.0203(3) .39530(9) .7467(3) 4.12(6) O(4B) -.0077(2) .35270(6) .7734(2) 5.39(5) O(5B) .0337(2) .42984(6) .8550(2) 4.89(4) C(17B) .1140(4) .4144(1) 1.0160(3) 5.19(7) C(18B) .2059(3) .45686(9) 1.1075(3) 4.32(6) C(19B) .2992(4) .4833(1) 1.0558(3) 5.33(7) C(20B) .3838(4) .5222(1) 1.1417(4) 5.83(8) C(21B) .3745(4) .5350(1) 1.2783(4) 5.87(8) C(22B) .2840(3) .5084(1) 1.3312(3) 5.66(8) C(23B) .1995(3) .4696(1) 1.2465(3) 4.78(6) H(C1A) .154(3) .1673(9) -.424(3) ? H(C2A) .217(3) .2429(9) -.342(3) ? H(C3A) .449(3) .267(1) -.125(3) ? H(C5A) .569(3) .1329(9) -.096(3) ? H(C6A) .339(3) .111(1) -.306(3) ? H(C7A) .771(3) .1850(9) .060(3) ? H'(C7A) .733(3) .2409(9) .025(3) ? H(C9A) .942(3) .2167(9) .606(3) ? H'(C9A) .902(3) .271(1) .617(3) ? H(C10A) .714(3) .255(1) .715(3) ? H'(C10A) .803(3) .2101(9) .764(3) ? H(C11A) .504(3) .2117(9) .560(3) ? H'(C11A) .615(3) .170(1) .536(3) ? H(C13A) .191(3) .2003(9) .323(3) ? H'(C13A) .335(3) .189(1) .267(3) ? H(C14A) .207(3) .228(1) .031(3) ? H'(C14A) .059(3) .2049(9) .046(3) ? H(C15A) -.009(3) .2776(9) .107(3) ? H'(C15A) .095(3) .2939(9) .010(3) ? H(C17A) .200(3) .379(1) .558(3) ? H'(C17A) .312(3) .399(1) .518(3) ? H(C19A) .583(3) .354(1) .662(3) ? H(C20A) .804(3) .3447(9) .912(3) ? H(C21A) .760(3) .3471(9) 1.119(3) ? H(C22A) .492(3) .3581(9) 1.092(3) ? H(C23A) .293(3) .3676(9) .850(3) ? H(C1B) -.564(4) .498(1) -.295(4) ? H(C2B) -.521(4) .587(1) -.275(4) ? H(C3B) -.315(4) .620(1) -.069(4) ? H(C5B) -.156(4) .492(1) .103(4) ? H(C6B) -.369(4) .461(1) -.110(4) ? H(C7B) -.072(4) .620(1) .156(4) ? H'(C7B) .032(4) .578(1) .144(4) ? H(C9B) .228(4) .580(1) .785(4) ? H'(C9B) .150(4) .622(1) .701(4) ? H(C10B) -.007(4) .610(1) .834(4) ? H'(C10B) .088(4) .567(1) .884(4) ? H(C11B) -.150(3) .534(1) .714(4) ? H'(C11B) -.208(4) .581(1) .599(4) ? H(C13B) -.305(4) .496(1) .424(4) ? H'(C13B) -.353(3) .462(1) .545(3) ? H(C14B) -.420(4) .409(1) .338(4) ? H'(C14B) -.314(4) .429(1) .304(4) ? H(C15B) -.137(4) .380(1) .409(4) ? H'(C15B) -.228(3) .359(1) .500(4) ? H(C17B) .192(4) .386(1) 1.021(4) ? H'(C17B) .028(4) .408(1) 1.048(4) ? H(C19B) .295(3) .473(1) .960(4) ? H(C20B) .445(4) .539(1) 1.102(4) ? H(C21B) .431(3) .565(1) 1.346(4) ? H(C22B) .271(3) .517(1) 1.424(4) ? H(C23B) .136(3) .453(1) 1.276(4) ?