#------------------------------------------------------------------------------ #$Date: 2009-11-18 14:56:34 +0000 (Wed, 18 Nov 2009) $ #$Revision: 858 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003196.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_2003196 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 262 _journal_page_last 265 _publ_section_title ; Novel N-Acyl \a-Azidopyrrolidines (N-Acyliminium-Ion Precursors) ; _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _publ_author_name 'Vincent M. Lynch' 'Christopher Hulme' 'Philip Magnus' 'Brian E. Davis' _chemical_formula_moiety 'C17 H17 N5 O' _chemical_formula_sum 'C17 H17 N5 O' _[local]_cod_chemical_formula_sum_orig 'C17 H17 N5 O1' _chemical_formula_weight 307.35 _cell_length_a 10.026(4) _cell_length_b 9.230(3) _cell_length_c 16.943(7) _cell_angle_alpha 90.0 _cell_angle_beta 97.30(3) _cell_angle_gamma 90.0 _cell_volume 1555.2(10) _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.31 _exptl_crystal_density_meas ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 40 _cell_measurement_theta_min 8.8 _cell_measurement_theta_max 12.05 _exptl_absorpt_coefficient_mu 0.08084 _cell_measurement_temperature 173(1) _exptl_crystal_description block _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.27 _exptl_crystal_colour 'colorless' _diffrn_measurement_device 'Nicolet R3 diffractometer' _diffrn_measurement_method \w-scan _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 7762 _reflns_number_total 3551 _reflns_number_observed 2331 _reflns_observed_criterion refl_observed_if_F_>_4.0_sigma(F) _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _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 0.0489 _refine_ls_wR_factor_obs 0.0499 _refine_ls_wR_factor_all 0.0575 _refine_ls_goodness_of_fit_obs 1.329 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 2331 _refine_ls_number_parameters 276 _refine_ls_hydrogen_treatment 'refall' _refine_ls_weighting_scheme 'calc w=1/[\s^2^(F)+0.0004F^2^]' _refine_ls_shift/esd_max 0.002 _refine_diff_density_max 0.45 _refine_diff_density_min -0.24 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_data_collection ; Siemens P3/V Data Collection System (1989) ; _computing_data_reduction ; Siemens P3/V Data Collection System ; _computing_structure_solution ;MPLN (Cordes, 1983); FUER (Larson, 1982); PLATON92 (Spek, 1992) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv N1 0.2937(2) -0.4524(2) 1.24896(10) 0.0297(5) C2 0.2271(2) -0.5630(3) 1.29072(12) 0.0326(7) C3 0.2040(3) -0.4937(3) 1.3695(2) 0.0480(9) C4 0.2867(3) -0.3562(3) 1.3761(2) 0.0511(10) C5 0.2915(3) -0.3112(2) 1.28994(13) 0.0345(8) N6 0.0925(2) -0.6027(2) 1.24834(12) 0.0459(7) N7 0.0905(2) -0.6468(2) 1.17968(13) 0.0404(7) N8 0.0728(2) -0.6826(3) 1.1150(2) 0.0668(10) C9 0.3769(2) -0.4919(2) 1.19457(11) 0.0261(6) O10 0.40832(14) -0.6177(2) 1.18424(8) 0.0327(5) N11 0.4238(2) -0.3771(2) 1.15135(10) 0.0277(5) C12 0.5518(2) -0.3915(2) 1.12278(12) 0.0253(6) C13 0.6622(2) -0.4360(2) 1.17462(13) 0.0317(7) C14 0.7873(2) -0.4479(3) 1.1483(2) 0.0382(7) C15 0.8022(2) -0.4142(2) 1.0700(2) 0.0395(8) C16 0.6925(2) -0.3689(2) 1.01869(14) 0.0375(8) C17 0.5667(2) -0.3568(2) 1.04472(12) 0.0308(7) C18 0.3379(2) -0.2585(2) 1.12381(11) 0.0250(6) C19 0.2044(2) -0.2822(3) 1.09426(13) 0.0340(7) C20 0.1214(3) -0.1657(3) 1.07083(14) 0.0394(8) C21 0.1717(3) -0.0266(3) 1.07454(13) 0.0386(8) C22 0.3058(3) -0.0028(3) 1.10202(13) 0.0362(7) C23 0.3889(2) -0.1186(2) 1.12716(13) 0.0313(7) H2 0.282(2) -0.653(2) 1.2950(12) 0.033(6) H3A 0.220(3) -0.559(4) 1.411(2) 0.084(10) H3B 0.104(3) -0.462(3) 1.363(2) 0.091(11) H4A 0.251(2) -0.280(3) 1.4083(14) 0.048(7) H4B 0.397(3) -0.379(3) 1.404(2) 0.076(9) H5A 0.377(2) -0.257(3) 1.2849(14) 0.047(7) H5B 0.209(3) -0.250(3) 1.2663(14) 0.056(7) H13 0.651(2) -0.456(2) 1.2296(13) 0.039(6) H14 0.867(2) -0.475(2) 1.1839(13) 0.048(7) H15 0.892(2) -0.422(3) 1.0506(13) 0.043(6) H16 0.703(2) -0.342(2) 0.9630(14) 0.043(6) H17 0.487(2) -0.326(2) 1.0076(13) 0.030(6) H19 0.169(2) -0.377(2) 1.0940(12) 0.037(6) H20 0.029(3) -0.184(3) 1.0496(14) 0.047(7) H21 0.113(3) 0.053(3) 1.0574(15) 0.059(8) H22 0.347(2) 0.095(3) 1.1032(13) 0.040(6) H23 0.478(2) -0.100(2) 1.1460(12) 0.032(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 N1 0.0329(10) 0.0014(8) 0.0108(8) 0.0226(9) 0.0029(7) 0.0353(9) C2 0.0287(12) -0.0004(10) 0.0073(10) 0.0295(12) 0.0075(10) 0.0403(12) C3 0.058(2) -0.0108(14) 0.0134(13) 0.051(2) 0.0058(12) 0.0362(13) C4 0.071(2) 0.0025(14) 0.0199(14) 0.043(2) -0.0008(12) 0.0427(14) C5 0.0409(14) 0.0016(11) 0.0134(11) 0.0281(12) -0.0013(10) 0.0367(12) N6 0.0304(11) -0.0044(10) 0.0091(9) 0.0634(14) -0.0021(10) 0.0450(12) N7 0.0262(10) -0.0031(9) 0.0062(10) 0.0342(11) -0.0071(10) 0.0610(14) N8 0.0478(15) -0.0042(13) -0.0011(12) 0.078(2) -0.0357(14) 0.072(2) C9 0.0221(10) 0.0034(9) -0.0004(8) 0.0259(11) 0.0029(8) 0.0293(10) O10 0.0326(9) 0.0048(7) 0.0070(7) 0.0243(8) 0.0022(6) 0.0418(8) N11 0.0256(9) 0.0055(8) 0.0065(7) 0.0252(9) 0.0060(7) 0.0331(9) C12 0.0240(10) 0.0001(8) 0.0046(9) 0.0190(10) -0.0019(8) 0.0332(11) C13 0.0320(12) 0.0044(10) 0.0022(10) 0.0268(11) 0.0035(9) 0.0358(12) C14 0.0228(11) 0.0040(10) -0.0007(11) 0.0327(12) 0.0022(11) 0.0576(15) C15 0.0291(13) -0.0000(10) 0.0173(12) 0.0300(12) -0.0008(11) 0.062(2) C16 0.0442(14) -0.0013(11) 0.0165(11) 0.0312(12) -0.0004(10) 0.0400(13) C17 0.0327(12) 0.0016(10) 0.0037(10) 0.0271(11) 0.0020(9) 0.0327(11) C18 0.0263(11) 0.0066(9) 0.0039(8) 0.0249(10) 0.0042(8) 0.0238(10) C19 0.0316(13) 0.0009(10) 0.0007(10) 0.0313(13) 0.0033(10) 0.0381(12) C20 0.0300(13) 0.0079(11) -0.0008(10) 0.0448(14) 0.0078(11) 0.0419(13) C21 0.0427(14) 0.0182(12) 0.0041(11) 0.0376(14) 0.0068(10) 0.0353(12) C22 0.0471(15) 0.0043(11) 0.0066(11) 0.0263(11) 0.0041(9) 0.0356(12) C23 0.0297(12) 0.0015(10) -0.0003(9) 0.0285(11) 0.0036(9) 0.0347(12)