#------------------------------------------------------------------------------ #$Date: 2008-03-16 06:59:57 +0000 (Sun, 16 Mar 2008) $ #$Revision: 274 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003049.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_2003049 _journal_name_full 'Acta Crystallographica, Section B' _journal_year 1998 _journal_volume B54 _journal_page_first 907 _journal_page_last 911 _chemical_name_systematic ; 2,4-diisopropyl-1-{4'-(S)-phenylalaninocarbonylphenyl}-2,2-dimethyl- 1,2-dihydrobenzocyclobuten-1-ol Methyl Ester ; _chemical_formula_moiety 'C33 H39 N1 O4' _chemical_formula_sum 'C33 H39 N1 O4' _chemical_formula_structural ? _chemical_formula_weight 513.68 _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X+0.5,-Y,+Z+0.5 +X+0.5,-Y+0.5,-Z -X,+Y+0.5,-Z+0.5 _cell_length_a 11.525(9) _cell_length_b 28.238(11) _cell_length_c 9.317(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3032(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 8.2 _cell_measurement_theta_max 13.4 _cell_measurement_temperature '298' _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Colourless' _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.125 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type 'none' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Rigaku AFC-5' _diffrn_measurement_method \w _diffrn_reflns_number 2946 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% 0 _reflns_number_total 2946 _reflns_number_observed 1410 _reflns_threshold_expression '|F~o~| > 3\s(|F~o~|)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.077 _refine_ls_wR_factor_obs 0.066 _refine_ls_goodness_of_fit_obs 1.31 _refine_ls_number_reflns 1410 _refine_ls_number_parameters 343 _refine_ls_hydrogen_treatment 'H atoms riding' _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s ^2^(F) + 0.0009F^2^]' _refine_ls_shift/esd_max 0.01 _refine_ls_shift/esd_mean 0.0024 _refine_diff_density_max 0.21 _refine_diff_density_min -0.22 _refine_ls_extinction_method 'None' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _atom_type_scat_source 'International Tables Vol.IV(1974)' _computing_data_collection ; MSC/AFC (Molecular Structure Corporation, 1988) ; _computing_cell_refinement ; MSC/AFC (Molecular Structure Corporation, 1988) ; _computing_data_reduction ; CRYSTAN-GM (Edwards, Gilmore, Mackay & Stewart, 1996) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy O1 1.2396(6) 0.0972(2) 0.9975(7) 0.094(3) Uij 1.000 O2 0.7314(6) 0.0321(2) 0.5632(6) 0.075(3) Uij 1.000 O3 0.4293(7) -0.0463(4) 0.7570(10) 0.143(5) Uij 1.000 O4 0.5307(7) 0.0007(3) 0.9000(10) 0.105(4) Uij 1.000 N5 0.7295(7) -0.0120(3) 0.7636(8) 0.072(3) Uij 1.000 C6 1.3032(8) 0.1474(4) 0.6760(10) 0.072(4) Uij 1.000 C7 1.3397(9) 0.1889(4) 0.6090(10) 0.086(5) Uij 1.000 C8 1.3100(10) 0.2337(5) 0.6530(10) 0.093(5) Uij 1.000 C9 1.2440(10) 0.2386(4) 0.7800(10) 0.100(6) Uij 1.000 C10 1.2098(9) 0.1988(4) 0.8480(10) 0.083(5) Uij 1.000 C11 1.2347(9) 0.1541(4) 0.7960(10) 0.072(4) Uij 1.000 C12 1.1681(9) 0.1269(4) 0.9110(10) 0.076(4) Uij 1.000 C13 1.0684(8) 0.0976(3) 0.8460(10) 0.062(4) Uij 1.000 C14 1.0433(9) 0.0528(4) 0.8920(10) 0.074(4) Uij 1.000 C15 0.9490(9) 0.0275(3) 0.8360(10) 0.071(4) Uij 1.000 C16 0.8786(9) 0.0465(3) 0.7360(10) 0.058(4) Uij 1.000 C17 0.9057(9) 0.0903(4) 0.6830(10) 0.069(4) Uij 1.000 C18 1.0007(9) 0.1155(3) 0.7360(10) 0.077(4) Uij 1.000 C19 1.3320(10) 0.0978(5) 0.6210(10) 0.098(6) Uij 1.000 C20 1.4590(10) 0.0885(4) 0.6260(10) 0.142(7) Uij 1.000 C21 1.2860(10) 0.0918(5) 0.465(2) 0.164(8) Uij 1.000 C22 1.3490(10) 0.2789(4) 0.578(2) 0.119(7) Uij 1.000 C23 1.4760(10) 0.2815(5) 0.5640(10) 0.159(8) Uij 1.000 C24 1.288(2) 0.2838(6) 0.440(2) 0.230(10) Uij 1.000 C25 1.1410(9) 0.1798(4) 0.9740(10) 0.078(5) Uij 1.000 C26 1.0150(9) 0.1970(4) 0.9840(10) 0.108(5) Uij 1.000 C27 1.1990(10) 0.1888(5) 1.1180(10) 0.124(6) Uij 1.000 C28 0.7715(9) 0.0220(3) 0.6810(10) 0.062(4) Uij 1.000 C29 0.6332(9) -0.0413(4) 0.7230(10) 0.074(5) Uij 1.000 C30 0.5210(10) -0.0284(5) 0.7920(10) 0.095(6) Uij 1.000 C31 0.4280(10) 0.0131(5) 0.9780(10) 0.151(7) Uij 1.000 C32 0.6610(10) -0.0934(4) 0.7480(10) 0.084(5) Uij 1.000 C33 0.7610(10) -0.1124(4) 0.6650(10) 0.078(5) Uij 1.000 C34 0.7540(10) -0.1226(4) 0.5210(10) 0.097(6) Uij 1.000 C35 0.847(2) -0.1398(5) 0.4510(10) 0.116(7) Uij 1.000 C36 0.9520(10) -0.1475(5) 0.521(2) 0.138(8) Uij 1.000 C37 0.956(2) -0.1377(7) 0.665(2) 0.155(9) Uij 1.000 C38 0.865(2) -0.1205(5) 0.735(2) 0.119(7) Uij 1.000 H1 1.20870 0.09940 1.09300 0.15 Uiso 1.000 H5 0.76440 -0.01720 0.85590 0.10 Uiso 1.000 H7 1.39200 0.18430 0.52980 0.10 Uiso 1.000 H9 1.22720 0.26940 0.81880 0.10 Uiso 1.000 H14 1.09540 0.03770 0.95790 0.10 Uiso 1.000 H15 0.92910 -0.00320 0.87360 0.10 Uiso 1.000 H17 0.86070 0.10250 0.60510 0.10 Uiso 1.000 H18 1.01810 0.14640 0.69880 0.10 Uiso 1.000 H19 1.29330 0.07550 0.68170 0.20 Uiso 1.000 H20A 1.47300 0.05660 0.59410 0.20 Uiso 1.000 H20B 1.48580 0.09280 0.72270 0.20 Uiso 1.000 H20C 1.49810 0.11080 0.56480 0.20 Uiso 1.000 H21A 1.29950 0.05990 0.43270 0.20 Uiso 1.000 H21B 1.32690 0.11400 0.40530 0.20 Uiso 1.000 H21C 1.20450 0.09910 0.46170 0.20 Uiso 1.000 H22 1.32560 0.30520 0.63620 0.20 Uiso 1.000 H23A 1.50220 0.31040 0.52070 0.20 Uiso 1.000 H23B 1.49920 0.25520 0.50550 0.20 Uiso 1.000 H23C 1.51020 0.27830 0.65730 0.20 Uiso 1.000 H24A 1.31460 0.31270 0.39650 0.20 Uiso 1.000 H24B 1.20690 0.28540 0.46150 0.20 Uiso 1.000 H24C 1.30200 0.25720 0.37780 0.20 Uiso 1.000 H26A 0.97170 0.18490 1.06380 0.20 Uiso 1.000 H26B 0.97730 0.18690 0.89710 0.20 Uiso 1.000 H26C 1.01370 0.23100 0.98820 0.20 Uiso 1.000 H27A 1.15540 0.17670 1.19770 0.20 Uiso 1.000 H27B 1.20940 0.22230 1.13010 0.20 Uiso 1.000 H27C 1.27330 0.17370 1.11580 0.20 Uiso 1.000 H29 0.62280 -0.03790 0.62160 0.10 Uiso 1.000 H31A 0.43400 0.03400 1.05840 0.15 Uiso 1.000 H31B 0.39180 -0.01550 1.00990 0.15 Uiso 1.000 H31C 0.37940 0.02810 0.90770 0.15 Uiso 1.000 H32A 0.59300 -0.11180 0.72540 0.10 Uiso 1.000 H32B 0.67810 -0.09690 0.84800 0.10 Uiso 1.000 H34 0.68220 -0.11900 0.47030 0.10 Uiso 1.000 H35 0.84690 -0.14640 0.34950 0.10 Uiso 1.000 H36 1.02040 -0.16010 0.47620 0.10 Uiso 1.000 H37 1.02550 -0.14190 0.72070 0.10 Uiso 1.000 H38 0.86620 -0.11280 0.83540 0.10 Uiso 1.000 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.080(5) 0.104(5) 0.097(6) 0.009(5) -0.015(5) 0.025(5) O2 0.093(5) 0.086(5) 0.044(4) -0.021(4) -0.004(4) 0.004(4) O3 0.090(6) 0.217(10) 0.121(7) -0.041(7) 0.026(6) -0.032(8) O4 0.092(6) 0.097(6) 0.127(7) 0.016(5) 0.001(7) -0.016(6) N5 0.081(6) 0.084(6) 0.050(5) -0.041(5) -0.009(5) 0.002(5) C6 0.053(6) 0.079(8) 0.083(8) 0.002(6) 0.007(7) 0.007(7) C7 0.080(8) 0.080(8) 0.097(9) -0.014(7) 0.037(8) 0.018(8) C8 0.094(9) 0.081(9) 0.105(10) -0.009(8) 0.016(8) 0.006(9) C9 0.099(9) 0.066(8) 0.136(11) -0.026(7) 0.010(10) -0.022(8) C10 0.082(8) 0.094(9) 0.072(8) -0.035(8) 0.005(7) -0.010(8) C11 0.057(7) 0.067(7) 0.092(8) -0.021(6) 0.006(7) -0.011(7) C12 0.067(7) 0.068(7) 0.092(9) -0.016(6) -0.001(8) 0.006(7) C13 0.075(7) 0.068(7) 0.045(6) 0.003(6) 0.017(6) 0.012(6) C14 0.067(7) 0.076(7) 0.078(8) 0.011(6) 0.000(7) 0.015(7) C15 0.071(7) 0.056(7) 0.085(8) -0.010(6) 0.001(7) 0.021(6) C16 0.062(7) 0.053(7) 0.060(6) -0.003(6) 0.006(6) -0.004(6) C17 0.076(7) 0.067(7) 0.063(7) -0.006(6) -0.015(7) 0.004(6) C18 0.090(8) 0.076(7) 0.065(7) -0.014(7) -0.014(7) 0.032(6) C19 0.085(9) 0.109(10) 0.100(10) 0.013(8) 0.023(9) -0.011(9) C20 0.160(10) 0.140(10) 0.120(10) 0.040(10) 0.020(10) -0.020(10) C21 0.170(10) 0.160(10) 0.160(10) -0.010(10) -0.060(10) -0.070(10) C22 0.130(10) 0.090(10) 0.140(10) -0.040(10) 0.020(10) 0.000(10) C23 0.140(10) 0.190(10) 0.140(10) -0.090(10) -0.010(10) 0.070(10) C24 0.26(2) 0.19(2) 0.25(2) -0.130(10) -0.12(2) 0.13(2) C25 0.070(7) 0.093(8) 0.070(8) 0.001(6) -0.006(7) -0.009(7) C26 0.078(8) 0.125(10) 0.121(10) 0.002(8) 0.002(8) -0.031(9) C27 0.097(9) 0.172(12) 0.103(10) 0.005(9) -0.010(8) -0.037(9) C28 0.070(7) 0.066(6) 0.049(6) -0.020(6) 0.023(7) -0.006(6) C29 0.080(8) 0.091(9) 0.050(6) -0.017(7) -0.014(6) 0.004(6) C30 0.070(9) 0.117(11) 0.098(11) -0.011(9) -0.001(9) -0.009(9) C31 0.120(10) 0.160(10) 0.170(10) 0.050(10) 0.030(10) -0.040(10) C32 0.091(9) 0.088(8) 0.074(8) -0.014(7) -0.005(8) 0.008(8) C33 0.069(8) 0.068(7) 0.097(10) -0.013(6) -0.011(9) 0.007(7) C34 0.090(10) 0.140(10) 0.060(10) -0.020(10) 0.000(10) -0.010(10) C35 0.110(10) 0.160(10) 0.080(10) -0.010(10) 0.020(10) 0.000(10) C36 0.070(10) 0.150(10) 0.18(2) 0.020(10) 0.030(10) -0.010(10) C37 0.120(10) 0.22(2) 0.130(10) 0.010(10) -0.040(10) -0.030(10) C38 0.110(10) 0.150(10) 0.100(10) 0.010(10) 0.010(10) 0.000(10)