#------------------------------------------------------------------------------ #$Date: 2009-11-18 14:56:34 +0000 (Wed, 18 Nov 2009) $ #$Revision: 858 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003317.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_2003317 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 782 _journal_page_last 786 _publ_section_title ; Two [7.3.1]Azabicyclo-z-1,5-diyne-3-ene Analogues of Dynemicin A ; _chemical_formula_moiety 'C30 H31 N1 O5' _chemical_formula_sum 'C30 H31 N O5' _[local]_cod_chemical_formula_sum_orig 'C30 H31 N1 O5' _chemical_formula_weight 485.58 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _symmetry_space_group_name_H-M 'P -1' _cell_length_a 10.747(3) _cell_length_b 11.529(3) _cell_length_c 11.661(2) _cell_angle_alpha 89.82(2) _cell_angle_beta 70.51(2) _cell_angle_gamma 67.43(2) _cell_volume 1244.7(6) _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.30 _exptl_crystal_density_meas ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 41 _cell_measurement_theta_min 7.55 _cell_measurement_theta_max 10.9 _exptl_absorpt_coefficient_mu 0.08198 _cell_measurement_temperature 173(1) _exptl_crystal_description 'plate' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_colour 'colorless' _diffrn_measurement_device 'Nicolet P3' _diffrn_measurement_method \w _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 6040 _reflns_number_total 5736 _reflns_number_observed 4452 _reflns_observed_criterion 'refl_observed_if_F_>_4.0_sigma(F)' _diffrn_reflns_av_R_equivalents 0.015 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_standards_number 4 _diffrn_standards_interval_count 96 _diffrn_standards_decay_% 1.3 _refine_ls_structure_factor_coef 'F' _refine_ls_R_factor_obs 0.0530 _refine_ls_wR_factor_obs 0.0692 _refine_ls_wR_factor_all 0.0713 _refine_ls_goodness_of_fit_obs 2.297 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 4452 _refine_ls_number_parameters 434 _refine_ls_hydrogen_treatment 'refall' _refine_ls_weighting_scheme 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/esd_max 0.002 _refine_diff_density_max 0.49 _refine_diff_density_min -0.31 _refine_ls_extinction_method 'modified Larson (SHELXTL-Plus)' _refine_ls_extinction_coef 1.4E-6(2) loop_ _atom_type_symbol _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C 'International Tables Vol.IV' .002 .002 H 'International Tables Vol.IV' 0 0 O 'International Tables Vol.IV' .008 .006 N 'International Tables Vol.IV' .004 .003 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _computing_structure_solution ; MPLN (Cordes, 1983) and FUER (Larson, 1982) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv C1 0.4156(2) -0.1028(2) -0.1035(2) 0.0273(8) C2 0.4859(2) -0.2250(2) -0.1972(2) 0.0336(9) C3 0.4722(2) -0.1942(2) -0.3156(2) 0.0334(8) C4 0.4467(2) -0.1518(2) -0.4029(2) 0.0388(9) C5 0.3928(3) -0.0788(3) -0.4880(2) 0.0446(11) C6 0.2821(3) 0.0343(3) -0.4465(2) 0.0423(11) C7 0.2208(2) 0.0780(2) -0.3173(2) 0.0339(9) C8 0.1891(2) 0.0938(2) -0.2088(2) 0.0296(8) C9 0.1736(2) 0.0896(2) -0.0783(2) 0.0280(8) N10 0.2423(2) 0.1636(2) -0.04115(14) 0.0266(6) C10a 0.3934(2) 0.1240(2) -0.1094(2) 0.0236(7) C11 0.4548(2) 0.2113(2) -0.1438(2) 0.0253(7) C12 0.6015(2) 0.1713(2) -0.2099(2) 0.0272(8) C13 0.6872(2) 0.0417(2) -0.2434(2) 0.0272(7) C14 0.6252(2) -0.0451(2) -0.2114(2) 0.0269(8) C14a 0.4793(2) -0.0062(2) -0.1442(2) 0.0233(7) C15 0.2517(2) -0.0500(2) -0.0662(2) 0.0289(8) O16 0.1853(2) -0.1146(2) -0.0273(2) 0.0444(7) O17 0.83253(14) -0.00977(14) -0.30981(14) 0.0394(6) C18 0.9058(3) 0.0721(3) -0.3299(3) 0.0622(12) C19 0.1725(2) 0.2556(2) 0.0606(2) 0.0276(7) O20 0.22829(14) 0.31668(13) 0.09188(12) 0.0328(6) O21 0.0379(2) 0.26417(14) 0.11771(13) 0.0386(6) C22 -0.0640(2) 0.3605(2) 0.2261(2) 0.0288(7) C23 -0.1956(2) 0.3278(2) 0.2628(2) 0.0341(8) C24 -0.3159(2) 0.4224(2) 0.3743(2) 0.0322(8) C25 -0.2612(3) 0.4136(3) 0.4811(2) 0.0435(10) C26 -0.1280(2) 0.4457(2) 0.4423(2) 0.0424(10) C27 -0.0077(2) 0.3501(2) 0.3305(2) 0.0369(9) C28 -0.1039(2) 0.4932(2) 0.1906(2) 0.0324(8) C29 -0.2238(2) 0.5878(2) 0.3016(2) 0.0351(8) C30 -0.1683(3) 0.5800(2) 0.4072(2) 0.0439(10) C31 -0.3564(2) 0.5559(2) 0.3404(2) 0.0337(8) C1A 0.2352(6) 0.5804(5) 0.2108(5) 0.059(3) C2A 0.2996(5) 0.5780(3) 0.0702(3) 0.090(3) C3A 0.4623(4) 0.5154(3) 0.0525(2) 0.061(2) O4A 0.4660(5) 0.5169(4) 0.1514(4) 0.075(3) H18A 1.0062(3) 0.0240(3) -0.3772(3) 0.081(10) H18B 0.8650(3) 0.1377(3) -0.3740(3) 0.12(2) H18C 0.8962(3) 0.1098(3) -0.2524(3) 0.073(9) H1 0.436(2) -0.132(2) -0.032(2) 0.030(5) H9 0.076(2) 0.119(2) -0.018(2) 0.034(6) H6 0.244(3) 0.081(2) -0.502(2) 0.042(6) H5 0.438(3) -0.113(2) -0.576(2) 0.049(7) H2A 0.432(2) -0.284(2) -0.164(2) 0.039(6) H2B 0.583(3) -0.270(2) -0.203(2) 0.042(6) H11 0.394(2) 0.303(2) -0.125(2) 0.033(6) H12 0.642(2) 0.241(2) -0.237(2) 0.026(5) H14 0.688(2) -0.139(2) -0.233(2) 0.029(5) H23A -0.166(2) 0.240(2) 0.282(2) 0.038(6) H23B -0.229(2) 0.329(2) 0.196(2) 0.034(6) H24 -0.404(2) 0.401(2) 0.399(2) 0.036(6) H25A -0.236(3) 0.324(3) 0.509(2) 0.057(7) H25B -0.338(3) 0.476(3) 0.557(2) 0.061(8) H26 -0.082(3) 0.438(3) 0.515(2) 0.066(8) H27A 0.073(2) 0.375(2) 0.307(2) 0.037(6) H27B 0.021(2) 0.264(2) 0.343(2) 0.037(6) H28A -0.140(3) 0.493(2) 0.121(2) 0.048(7) H28B -0.024(3) 0.512(2) 0.168(2) 0.036(6) H29 -0.249(2) 0.671(2) 0.279(2) 0.036(6) H30A -0.072(3) 0.605(2) 0.375(2) 0.056(7) H30B -0.249(3) 0.647(3) 0.481(2) 0.062(8) H31A -0.431(2) 0.619(2) 0.412(2) 0.034(6) H31B -0.392(2) 0.558(2) 0.268(2) 0.037(6) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 C1 0.0312(10) -0.0151(8) -0.0118(8) 0.0295(10) 0.0066(10) 0.0253(10) C2 0.0328(11) -0.0121(9) -0.0131(8) 0.0242(11) 0.0037(12) 0.0439(10) C3 0.0319(11) -0.0134(9) -0.0050(8) 0.0278(11) -0.0079(11) 0.0360(10) C4 0.0367(12) -0.0189(9) -0.0047(9) 0.0432(12) -0.0109(11) 0.0328(12) C5 0.0472(14) -0.0273(10) -0.0106(10) 0.0647(14) -0.0024(11) 0.025(2) C6 0.0463(14) -0.0316(10) -0.0185(11) 0.0643(14) 0.0114(11) 0.029(2) C7 0.0334(11) -0.0187(9) -0.0175(9) 0.0397(11) 0.0055(11) 0.0364(11) C8 0.0248(10) -0.0108(8) -0.0136(8) 0.0289(10) -0.0000(11) 0.0370(10) C9 0.0216(9) -0.0134(8) -0.0043(8) 0.0343(9) -0.0039(10) 0.0264(10) N10 0.0221(8) -0.0114(6) -0.0044(6) 0.0297(8) -0.0051(8) 0.0255(8) C10a 0.0211(9) -0.0105(7) -0.0072(7) 0.0285(9) -0.0000(9) 0.0214(9) C11 0.0280(10) -0.0110(8) -0.0101(7) 0.0246(10) 0.0018(9) 0.0243(9) C12 0.0290(10) -0.0173(8) -0.0094(8) 0.0339(10) 0.0040(9) 0.0232(10) C13 0.0225(9) -0.0120(7) -0.0081(8) 0.0344(9) 0.0024(9) 0.0249(10) C14 0.0249(10) -0.0090(8) -0.0107(8) 0.0273(10) 0.0023(10) 0.0280(10) C14a 0.0249(9) -0.0125(7) -0.0103(7) 0.0278(9) 0.0035(9) 0.0205(9) C15 0.0324(10) -0.0194(8) -0.0066(8) 0.0356(10) 0.0005(9) 0.0215(11) O16 0.0404(9) -0.0283(7) -0.0076(7) 0.0445(9) 0.0091(10) 0.0516(9) O17 0.0209(7) -0.0136(6) -0.0042(7) 0.0422(7) -0.0011(9) 0.0490(8) C18 0.0318(13) -0.0288(13) 0.002(2) 0.0634(13) -0.012(2) 0.082(2) C19 0.0260(10) -0.0103(8) -0.0069(7) 0.0282(10) -0.0012(9) 0.0259(9) O20 0.0284(7) -0.0147(6) -0.0062(6) 0.0340(7) -0.0075(8) 0.0338(7) O21 0.0268(7) -0.0165(6) 0.0033(6) 0.0427(7) -0.0166(8) 0.0368(9) C22 0.0236(9) -0.0075(8) -0.0020(8) 0.0278(9) -0.0068(10) 0.0264(10) C23 0.0291(11) -0.0151(9) -0.0025(9) 0.0312(11) -0.0031(11) 0.0370(11) C24 0.0243(10) -0.0113(8) -0.0028(8) 0.0319(10) 0.0019(11) 0.0340(10) C25 0.0346(12) -0.0076(10) -0.0046(10) 0.0511(12) 0.0055(11) 0.0296(14) C26 0.0302(11) -0.0063(9) -0.0107(10) 0.0579(11) -0.0039(11) 0.0280(15) C27 0.0250(11) -0.0043(9) -0.0074(9) 0.0382(11) 0.0008(12) 0.0361(12) C28 0.0281(10) -0.0175(9) -0.0087(9) 0.0383(10) 0.0049(11) 0.0329(11) C29 0.0287(11) -0.0091(9) -0.0093(9) 0.0253(11) 0.0026(12) 0.0461(10) C30 0.0315(12) -0.0111(10) -0.0069(10) 0.0438(12) -0.0188(13) 0.0465(13) C31 0.0252(10) -0.0075(9) -0.0094(9) 0.0314(10) 0.0023(12) 0.0389(10) C1A 0.080(4) -0.046(3) -0.007(2) 0.042(4) 0.002(3) 0.061(3) C2A 0.155(4) -0.068(2) -0.046(2) 0.069(4) 0.019(2) 0.072(2) C3A 0.127(3) -0.061(2) -0.0608(14) 0.049(3) 0.0274(15) 0.0547(15) O4A 0.106(4) -0.039(3) -0.042(2) 0.055(4) 0.012(3) 0.077(2)