#------------------------------------------------------------------------------ #$Date: 2008-01-26 17:25:03 +0000 (Sat, 26 Jan 2008) $ #$Revision: 20 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003697.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_2003697 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1341 _journal_page_last 1345 _publ_section_title ; Conformation at the Amide N atom of 1-Carboxamide Indole Derivatives ; _chemical_formula_sum 'C17 H16 N2 O3' _chemical_formula_analytical 'C17 H16 N2 O3' _chemical_formula_weight 296.33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _symmetry_space_group_name_H-M 'P 21/c' _cell_length_a 6.926(1) _cell_length_b 15.054(3) _cell_length_c 14.471(2) _cell_angle_alpha 90 _cell_angle_beta 99.94(1) _cell_angle_gamma 90 _cell_volume 1486.2(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_radiation 'CuK\a' _cell_measurement_wavelength 1.54178 _diffrn_radiation_type 'CuK\a~1~' _diffrn_radiation_wavelength 1.5405620 _cell_measurement_reflns_used 30 _cell_measurement_theta_min 22 _cell_measurement_theta_max 34 _exptl_absorpt_coefficient_mu 0.714 _cell_measurement_temperature 293(2) _exptl_crystal_description ; small tabular prisms ; _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.26 _exptl_crystal_colour 'colourless, slightly brown' _chemical_compound_source ; chemical synthesis ; _diffrn_measurement_device 'Siemens-AED diffractometer' _diffrn_measurement_method '\q/2\q scan' _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 2950 _reflns_number_total 2841 _reflns_number_observed 1913 _reflns_observed_criterion 'I>2\s(I)' _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_theta_max 70.14 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 1 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'within statistical fluctuation' _refine_ls_structure_factor_coef 'Fsqd' _refine_ls_R_factor_obs 0.0375 _refine_ls_wR_factor_obs 0.0923 _refine_ls_wR_factor_all 0.1096 _refine_ls_goodness_of_fit_obs 0.968 _refine_ls_goodness_of_fit_all 0.921 _refine_ls_number_reflns 2841 _refine_ls_number_parameters 264 _refine_ls_hydrogen_treatment 'refall' _refine_ls_weighting_scheme 'w = 1/[\s^2^(F~o~^2^) + (0.0630P)^2^] where P = _refine_ls_shift/esd_max 0.010 _refine_diff_density_max 0.239 _refine_diff_density_min -0.207 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_extinction_coef 0.007(1) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'O ' 'Oxygen ' 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 0.0492 0.0322 'N ' 'Nitrogen ' 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 0.0311 0.0180 'C ' 'Carbon ' 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 0.0181 0.0091 'H ' 'Hydrogen ' 'Int. Tab. C, 4.2.6.8, 6.1.1.4' 0.0000 0.0000 ; PARST (Nardelli, 1983); PARSTCIF (Nardelli, 1991) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv O1 0.1603(2) 0.68304(9) 0.7990(1) 0.0598(5) O2 -0.3915(2) 1.01255(9) 0.39329(9) 0.0550(5) O3 -0.5671(3) 1.1152(1) 0.0822(1) 0.0855(7) N1 -0.2856(2) 0.9035(1) 0.5465(1) 0.0476(5) N2 -0.1417(3) 0.9602(1) 0.3246(1) 0.0477(5) C1 0.3619(4) 0.6729(2) 0.7953(2) 0.0834(11) C2 0.0522(3) 0.7382(1) 0.7332(1) 0.0477(6) C3 -0.1292(3) 0.7644(1) 0.7558(1) 0.0537(7) C4 -0.2529(3) 0.8196(1) 0.6978(1) 0.0522(7) C5 -0.1928(3) 0.8488(1) 0.6159(1) 0.0440(6) C6 -0.0142(3) 0.8214(1) 0.5914(1) 0.0427(5) C7 0.1128(3) 0.7652(1) 0.6518(1) 0.0479(6) C8 -0.0046(3) 0.8605(1) 0.5025(1) 0.0464(6) C9 -0.1716(3) 0.9104(1) 0.4779(1) 0.0440(5) C10 -0.2438(3) 0.9658(1) 0.3957(1) 0.0439(6) C11 -0.1773(3) 1.0049(1) 0.2370(1) 0.0465(6) C12 -0.0217(4) 1.0106(2) 0.1883(2) 0.0604(8) C13 -0.0503(4) 1.0527(2) 0.1022(2) 0.0731(9) C14 -0.2288(4) 1.0889(2) 0.0637(2) 0.0693(8) C15 -0.3819(3) 1.0824(1) 0.1123(1) 0.0588(7) C16 -0.3580(3) 1.0395(1) 0.1990(1) 0.0531(6) C17 -0.6046(6) 1.1573(3) -0.0072(2) 0.0955(14) H1N -0.4006(36) 0.9334(16) 0.5479(16) 0.0684(70) H2N -0.0360(32) 0.9268(13) 0.3329(14) 0.0494(56) H3 -0.1643(28) 0.7427(13) 0.8165(14) 0.0495(52) H4 -0.3726(34) 0.8412(15) 0.7122(16) 0.0658(64) H7 0.2595(28) 0.7401(13) 0.6360(13) 0.0491(51) H8 0.1186(31) 0.8550(15) 0.4639(15) 0.0625(60) H11 0.4072(42) 0.6386(21) 0.8546(20) 0.1023(93) H12 0.4354(41) 0.7263(20) 0.7902(20) 0.0922(93) H13 0.3753(41) 0.6399(21) 0.7334(20) 0.0961(96) H121 0.1077(37) 0.9854(16) 0.2204(18) 0.0782(74) H131 0.0573(40) 1.0575(17) 0.0671(19) 0.0821(78) H141 -0.2417(37) 1.1176(18) 0.0066(19) 0.0805(77) H161 -0.4699(37) 1.0362(16) 0.2335(17) 0.0682(65) H171 -0.7439(60) 1.1730(28) -0.0169(27) 0.148(15) H172 -0.5629(61) 1.1179(27) -0.0607(29) 0.152(16) H173 -0.5209(41) 1.2128(20) -0.0013(18) 0.0835(86) 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 O1 0.0601(8) 0.0206(7) 0.0075(6) 0.0602(8) 0.0063(7) 0.0580(8) O2 0.0605(8) 0.0068(6) 0.0135(6) 0.0609(8) 0.0143(7) 0.0450(7) O3 0.0814(11) 0.0352(10) 0.0096(8) 0.1070(14) 0.0299(10) 0.0670(10) N1 0.0543(9) 0.0041(7) 0.0111(7) 0.0468(8) 0.0069(7) 0.0427(8) N2 0.0580(10) 0.0034(6) 0.0101(7) 0.0461(8) 0.0097(7) 0.0396(8) C1 0.0595(15) 0.0440(18) 0.0120(13) 0.0989(21) 0.0154(14) 0.0915(21) C2 0.0554(11) 0.0054(7) 0.0051(8) 0.0418(9) -0.0004(8) 0.0446(9) C3 0.0656(13) 0.0091(8) 0.0164(9) 0.0512(11) 0.0027(9) 0.0467(10) C4 0.0586(12) 0.0069(8) 0.0187(9) 0.0513(10) 0.0075(9) 0.0500(10) C5 0.0542(11) -0.0002(7) 0.0080(7) 0.0380(8) 0.0001(7) 0.0399(8) C6 0.0503(10) -0.0017(7) 0.0068(7) 0.0388(8) -0.0007(7) 0.0388(9) C7 0.0521(11) 0.0033(7) 0.0071(8) 0.0470(10) 0.0013(8) 0.0443(10) C8 0.0538(11) 0.0000(7) 0.0089(7) 0.0483(10) 0.0031(8) 0.0374(8) C9 0.0548(10) -0.0011(7) 0.0085(7) 0.0422(9) -0.0021(8) 0.0353(8) C10 0.0541(11) -0.0022(7) 0.0069(7) 0.0397(9) -0.0009(7) 0.0376(8) C11 0.0614(11) 0.0000(7) 0.0097(8) 0.0417(9) 0.0023(8) 0.0369(8) C12 0.0637(13) 0.0072(10) 0.0148(10) 0.0705(14) 0.0040(11) 0.0490(11) C13 0.0765(16) 0.0151(12) 0.0244(12) 0.0921(17) 0.0018(13) 0.0552(13) C14 0.0867(16) 0.0171(11) 0.0162(11) 0.0749(15) 0.0026(13) 0.0480(11) C15 0.0719(14) 0.0076(8) 0.0074(10) 0.0552(11) 0.0081(10) 0.0482(11) C16 0.0627(13) 0.0055(8) 0.0131(9) 0.0549(11) 0.0067(9) 0.0432(10) C17 0.1023(24) 0.0412(18) -0.0010(16) 0.1062(25) 0.0204(21) 0.0724(18)