#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003494.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_2003494 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 967 _journal_page_last 970 _publ_section_title ; (+-)-3-Methyl-1,1-diphenyl-2-butyl 3-Acetamidocrotonate and its Hydrogenation Product ; _chemical_formula_moiety 'C23 H27 N O3' _chemical_formula_sum 'C23 H27 N O3' _chemical_formula_weight 365.47 loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '-x,-y,-z' '-x,1/2+y,1/2-z' '+x,1/2-y,1/2+z' _symmetry_space_group_name_H-M 'P 21/c' _cell_length_a 11.049(4) _cell_length_b 18.659(6) _cell_length_c 11.602(4) _cell_angle_alpha 90.00 _cell_angle_beta 117.08(2) _cell_angle_gamma 90.00 _cell_volume 2129.7(12) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.14 _exptl_crystal_density_meas ? _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.3 _cell_measurement_theta_max 21.4 _exptl_absorpt_coefficient_mu 0.56 _cell_measurement_temperature 293 _exptl_crystal_description prism _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_colour colourless _chemical_compound_source ? _diffrn_measurement_device 'Enraf-Nonius CAD-4 diffractometer' _diffrn_measurement_method \q/2\q _exptl_absorpt_correction_type none _diffrn_reflns_number 4367 _reflns_number_total 3413 _reflns_number_observed 2748 _reflns_observed_criterion refl_observed_if_I_>_3.0_sigma(I) _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_theta_max 64.81 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 5 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.051 _refine_ls_wR_factor_obs 0.070 _refine_ls_goodness_of_fit_obs 0.67 _refine_ls_number_reflns 2742 _refine_ls_number_parameters 244 _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F) + 0.0002F^2^] ; _refine_ls_shift/esd_max 0.01 _refine_diff_density_max 0.19 _refine_diff_density_min -0.21 _refine_ls_extinction_method none _atom_type_scat_source 'International_Tables_for_X-ray_Crystallography (1974 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv C1 0.6902(2) 0.1491(1) 0.0436(2) 0.059(2) C2 0.6533(2) 0.0973(1) -0.0599(2) 0.068(3) C3 0.6518(2) 0.0258(1) -0.0451(2) 0.068(3) C4 0.6116(3) -0.0231(1) -0.1593(3) 0.103(4) N5 0.6864(2) -0.0029(1) 0.0760(2) 0.068(2) C6 0.6886(2) -0.0736(1) 0.1114(3) 0.079(3) O7 0.6522(2) -0.1222(1) 0.0347(2) 0.117(3) C8 0.7391(3) -0.0845(1) 0.2535(3) 0.100(4) O9 0.7312(2) 0.1360(1) 0.1579(2) 0.071(2) O10 0.6755(1) 0.2163(1) -0.0037(1) 0.060(2) C11 0.7172(2) 0.2774(1) 0.0840(2) 0.055(2) C12 0.5918(2) 0.3168(1) 0.0724(2) 0.072(3) C13 0.5169(2) 0.2739(1) 0.1307(3) 0.104(4) C14 0.4966(3) 0.3397(2) -0.0656(3) 0.123(5) C15 0.8104(2) 0.3223(1) 0.0471(2) 0.056(2) C16 0.9344(2) 0.2816(1) 0.0558(2) 0.056(2) C17 0.9999(2) 0.2296(1) 0.1468(2) 0.076(3) C18 1.1190(2) 0.1984(1) 0.1588(3) 0.084(3) C19 1.1745(2) 0.2185(1) 0.0804(3) 0.081(3) C20 1.1093(3) 0.2697(2) -0.0122(3) 0.092(3) C21 0.9900(2) 0.3008(1) -0.0253(2) 0.072(3) C22 0.8584(2) 0.3901(1) 0.1290(2) 0.065(3) C23 0.8453(3) 0.4560(1) 0.0707(3) 0.106(4) C24 0.8943(4) 0.5172(1) 0.1443(5) 0.141(7) C25 0.9587(3) 0.5134(2) 0.2771(5) 0.129(6) C26 0.9715(3) 0.4490(1) 0.3360(3) 0.101(4) C27 0.9219(2) 0.3877(1) 0.2620(3) 0.076(3) H2 0.62698 0.11594 -0.14895 0.075 H4a 0.58921 0.00616 -0.23867 0.114 H4b 0.68887 -0.05614 -0.14376 0.114 H4c 0.53029 -0.05174 -0.17100 0.114 HN5 0.71379 0.03267 0.14792 0.075 H8a 0.73786 -0.13680 0.27182 0.110 H8b 0.83422 -0.06598 0.30114 0.110 H8c 0.67924 -0.05811 0.28267 0.110 H11 0.76828 0.26381 0.17743 0.060 H12 0.62566 0.36198 0.12361 0.079 H13a 0.43520 0.30125 0.12162 0.114 H13b 0.48761 0.22700 0.08460 0.114 H13c 0.57849 0.26512 0.22453 0.114 H14a 0.41635 0.36531 -0.06705 0.136 H14b 0.54587 0.37250 -0.09812 0.136 H14c 0.46484 0.29643 -0.12247 0.136 H15 0.75280 0.33512 -0.04589 0.062 H17 0.96105 0.21393 0.20552 0.084 H18 1.16474 0.16073 0.22598 0.093 H19 1.26113 0.19635 0.09017 0.089 H20 1.14845 0.28475 -0.07103 0.101 H21 0.94343 0.33764 -0.09411 0.079 H23 0.79995 0.45954 -0.02596 0.117 H24 0.88286 0.56468 0.10060 0.155 H25 0.99571 0.55779 0.32989 0.142 H26 1.01658 0.44583 0.43265 0.111 H27 0.93263 0.34049 0.30645 0.084 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 0.0526(10) -0.0016(8) 0.0246(10) 0.0478(11) -0.0021(10) 0.0611(14) C2 0.0710(12) 0.0005(9) 0.0276(10) 0.0574(12) -0.0089(11) 0.0575(13) C3 0.0613(11) 0.0008(9) 0.0299(11) 0.0555(12) -0.0164(11) 0.0698(15) C4 0.1247(21) 0.0017(14) 0.0471(16) 0.0719(15) -0.0240(14) 0.0836(18) N5 0.0663(10) -0.0003(7) 0.0264(9) 0.0469(9) -0.0080(9) 0.0690(13) C6 0.0660(12) -0.0008(9) 0.0433(13) 0.0472(12) -0.0073(13) 0.1029(20) O7 0.1295(15) -0.0141(9) 0.0754(13) 0.0569(10) -0.0246(11) 0.1344(17) C8 0.1006(18) 0.0011(13) 0.0424(17) 0.0673(15) 0.0134(15) 0.1024(21) O9 0.0847(10) -0.0038(7) 0.0263(8) 0.0502(8) -0.0020(7) 0.0564(10) O10 0.0592(7) -0.0047(5) 0.0218(6) 0.0478(7) -0.0043(6) 0.0545(8) C11 0.0486(9) -0.0050(7) 0.0209(9) 0.0459(10) -0.0051(9) 0.0540(12) C12 0.0532(10) -0.0019(9) 0.0292(11) 0.0602(12) -0.0111(12) 0.0816(16) C13 0.0756(14) -0.0231(12) 0.0673(16) 0.0854(16) -0.0348(16) 0.1313(24) C14 0.0746(16) 0.0481(18) 0.0249(16) 0.1504(28) 0.0191(22) 0.1098(24) C15 0.0508(9) 0.0016(7) 0.0215(9) 0.0469(10) 0.0090(9) 0.0544(12) C16 0.0530(10) -0.0069(8) 0.0247(9) 0.0451(10) -0.0031(9) 0.0536(12) C17 0.0629(11) 0.0126(10) 0.0417(11) 0.0661(13) 0.0207(12) 0.0837(16) C18 0.0608(12) 0.0099(10) 0.0433(13) 0.0649(13) 0.0150(13) 0.1063(20) C19 0.0612(12) -0.0044(10) 0.0440(13) 0.0642(13) -0.0166(13) 0.0995(19) C20 0.0787(15) -0.0171(14) 0.0553(14) 0.1012(19) -0.0167(15) 0.0829(17) C21 0.0684(12) -0.0068(10) 0.0347(11) 0.0718(13) 0.0012(11) 0.0601(14) C22 0.0522(10) 0.0021(8) 0.0324(11) 0.0413(10) 0.0072(10) 0.0833(16) C23 0.1131(20) 0.0046(12) 0.0555(18) 0.0482(13) 0.0189(15) 0.1247(25) C24 0.1416(28) -0.0010(16) 0.0774(29) 0.0403(14) 0.0126(21) 0.1936(41) C25 0.0949(20) -0.0116(14) 0.0629(24) 0.0579(18) -0.0366(23) 0.1920(39) C26 0.0792(15) -0.0106(12) 0.0374(16) 0.0689(16) -0.0331(16) 0.1207(24) C27 0.0676(12) -0.0053(9) 0.0273(12) 0.0520(12) -0.0076(12) 0.0844(17)