#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003050.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_2003050 _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-(3'-methoxycarbonylphenyl)-2,2-dimethyl- 1,2-dihydrobenzocyclobuten-1-ol ; _chemical_formula_moiety 'C24 H30 O3' _chemical_formula_sum 'C24 H30 O3' _chemical_formula_structural ? _chemical_formula_weight 366.50 _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'P 21 n b ' _symmetry_space_group_name_Hall 'P -2bc 21' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z +X+0.5,-Y,-Z +X+0.5,-Y+0.5,+Z+0.5 +X,+Y+0.5,-Z+0.5 _cell_length_a 11.691(2) _cell_length_b 17.510(3) _cell_length_c 10.683(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2186.9(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _cell_measurement_temperature '293' _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Colourless' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _exptl_crystal_density_diffrn 1.113 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 0.072 _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 \q-2\q _diffrn_reflns_number 1087 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_theta_max 20.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% 0 _reflns_number_total 1087 _reflns_number_observed 822 _reflns_threshold_expression '|F~o~| > 3\s(|F~o~|)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.049 _refine_ls_wR_factor_obs 0.047 _refine_ls_goodness_of_fit_obs 1.16 _refine_ls_number_reflns 822 _refine_ls_number_parameters 243 _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 0.0016 _refine_diff_density_max 0.14 _refine_diff_density_min -0.13 _refine_ls_extinction_method 'None' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _atom_type_scat_source 'International Tables Vol.IV(1974)' ; MSC/AFC (Molecular Structure Corporation, 1988) ; ; MSC/AFC (Molecular Structure Corporation, 1988) ; ; 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 0.0000 0.1667(3) 0.9724(5) 0.059(2) Uij 1.000 O2 -0.4164(8) 0.3998(4) 0.6929(7) 0.094(3) Uij 1.000 O3 -0.4321(7) 0.3595(4) 0.8891(7) 0.078(3) Uij 1.000 C4 -0.2051(9) 0.2358(5) 1.1851(8) 0.045(3) Uij 1.000 C5 -0.2812(9) 0.2134(5) 1.2771(8) 0.052(4) Uij 1.000 C6 -0.3333(9) 0.1414(6) 1.2821(8) 0.052(4) Uij 1.000 C7 -0.3100(10) 0.0882(5) 1.1900(10) 0.058(4) Uij 1.000 C8 -0.2334(9) 0.1085(5) 1.0964(8) 0.047(4) Uij 1.000 C9 -0.1841(8) 0.1798(5) 1.0937(8) 0.043(3) Uij 1.000 C10 -0.1229(7) 0.1662(5) 0.9704(8) 0.053(4) Uij 1.000 C11 -0.1573(9) 0.2159(5) 0.8614(7) 0.045(4) Uij 1.000 C12 -0.2528(9) 0.2628(5) 0.8706(8) 0.049(4) Uij 1.000 C13 -0.2830(10) 0.3078(5) 0.7700(10) 0.059(4) Uij 1.000 C14 -0.2190(10) 0.3066(7) 0.6600(10) 0.080(5) Uij 1.000 C15 -0.1280(10) 0.2604(7) 0.6520(10) 0.085(5) Uij 1.000 C16 -0.0937(9) 0.2147(5) 0.7500(10) 0.069(4) Uij 1.000 C17 -0.1520(9) 0.3141(4) 1.1793(8) 0.052(4) Uij 1.000 C18 -0.0650(10) 0.3253(6) 1.2820(10) 0.097(5) Uij 1.000 C19 -0.2390(10) 0.3766(5) 1.1860(10) 0.096(5) Uij 1.000 C20 -0.4120(10) 0.1239(5) 1.3939(9) 0.072(4) Uij 1.000 C21 -0.3450(10) 0.0919(7) 1.5039(8) 0.100(5) Uij 1.000 C22 -0.5118(9) 0.0725(6) 1.3602(8) 0.080(5) Uij 1.000 C23 -0.1814(8) 0.0822(5) 0.9747(8) 0.053(4) Uij 1.000 C24 -0.0980(9) 0.0157(5) 0.9872(9) 0.070(4) Uij 1.000 C25 -0.2670(10) 0.0654(5) 0.8694(8) 0.073(4) Uij 1.000 C26 -0.3810(10) 0.3601(6) 0.7760(10) 0.073(6) Uij 1.000 C27 -0.5320(10) 0.4062(7) 0.9040(10) 0.106(5) Uij 1.000 H1 0.02220 0.14870 1.05370 0.12 Uiso 1.000 H5 -0.29780 0.24900 1.34300 0.08 Uiso 1.000 H7 -0.34690 0.03930 1.19120 0.08 Uiso 1.000 H12 -0.29520 0.26580 0.94740 0.08 Uiso 1.000 H14 -0.24090 0.33750 0.58920 0.08 Uiso 1.000 H15 -0.08160 0.25980 0.57760 0.08 Uiso 1.000 H16 -0.02830 0.18170 0.74460 0.08 Uiso 1.000 H17 -0.11250 0.31950 1.10100 0.12 Uiso 1.000 H18A -0.02860 0.37440 1.27920 0.12 Uiso 1.000 H18B -0.00770 0.28610 1.27570 0.12 Uiso 1.000 H18C -0.10440 0.31990 1.36040 0.12 Uiso 1.000 H19A -0.20250 0.42570 1.18270 0.12 Uiso 1.000 H19B -0.28290 0.37230 1.26110 0.12 Uiso 1.000 H19C -0.28890 0.37110 1.11490 0.12 Uiso 1.000 H20 -0.44880 0.17000 1.42080 0.12 Uiso 1.000 H21A -0.39610 0.08190 1.57250 0.12 Uiso 1.000 H21B -0.28790 0.12850 1.52750 0.12 Uiso 1.000 H21C -0.30820 0.04580 1.47710 0.12 Uiso 1.000 H22A -0.56270 0.06250 1.42880 0.12 Uiso 1.000 H22B -0.47760 0.02550 1.33300 0.12 Uiso 1.000 H22C -0.55410 0.09430 1.29190 0.12 Uiso 1.000 H24A -0.06520 -0.00230 0.91030 0.12 Uiso 1.000 H24B -0.13410 -0.02690 1.02780 0.12 Uiso 1.000 H24C -0.03680 0.03400 1.03910 0.12 Uiso 1.000 H25A -0.23430 0.04740 0.79250 0.12 Uiso 1.000 H25B -0.30390 0.11350 0.85380 0.12 Uiso 1.000 H25C -0.32340 0.02920 0.89690 0.12 Uiso 1.000 H27A -0.57310 0.40660 0.98170 0.12 Uiso 1.000 H27B -0.58480 0.39270 0.83940 0.12 Uiso 1.000 H27C -0.50480 0.45730 0.88990 0.12 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 0.047(4) 0.080(5) 0.050(4) 0.005(3) -0.002(3) -0.006(3) O2 0.117(6) 0.077(5) 0.089(5) -0.004(5) -0.057(5) 0.022(5) O3 0.073(5) 0.075(5) 0.087(6) 0.021(4) -0.020(5) 0.006(4) C4 0.049(6) 0.050(6) 0.035(6) 0.002(5) -0.007(5) 0.009(5) C5 0.066(7) 0.047(6) 0.043(7) -0.002(6) 0.004(6) -0.001(5) C6 0.051(6) 0.059(7) 0.047(7) 0.008(6) -0.003(6) 0.010(6) C7 0.065(7) 0.046(6) 0.064(7) 0.002(5) -0.001(6) -0.002(7) C8 0.043(6) 0.051(7) 0.047(6) 0.004(5) -0.009(5) -0.008(6) C9 0.051(6) 0.051(7) 0.028(5) 0.002(6) 0.002(5) 0.004(5) C10 0.038(6) 0.060(7) 0.063(7) -0.002(5) -0.005(5) -0.003(5) C11 0.055(7) 0.050(6) 0.030(6) -0.018(6) -0.010(5) 0.001(5) C12 0.053(7) 0.054(6) 0.041(7) -0.005(6) -0.006(5) 0.002(5) C13 0.063(7) 0.053(7) 0.062(8) -0.006(6) -0.016(7) 0.010(6) C14 0.095(9) 0.092(9) 0.051(8) -0.006(7) -0.004(8) 0.015(7) C15 0.091(9) 0.123(11) 0.040(7) -0.013(8) 0.012(7) 0.014(7) C16 0.068(7) 0.080(8) 0.059(7) 0.000(6) 0.004(7) -0.001(6) C17 0.063(7) 0.040(6) 0.054(6) 0.001(5) 0.007(6) 0.000(5) C18 0.095(8) 0.074(7) 0.120(10) -0.023(6) -0.052(9) 0.013(7) C19 0.095(8) 0.053(7) 0.141(10) -0.005(7) -0.030(8) 0.000(7) C20 0.084(8) 0.080(7) 0.051(7) -0.003(6) 0.015(7) 0.003(6) C21 0.095(8) 0.155(10) 0.050(7) -0.034(8) 0.009(7) 0.022(7) C22 0.052(7) 0.119(9) 0.070(7) -0.006(7) 0.016(6) 0.014(7) C23 0.055(6) 0.052(7) 0.051(6) 0.011(5) -0.011(6) -0.010(5) C24 0.078(7) 0.053(6) 0.079(7) -0.002(6) 0.001(6) -0.012(5) C25 0.074(7) 0.085(7) 0.061(6) -0.018(6) -0.013(6) -0.012(6) C26 0.080(10) 0.050(10) 0.080(10) -0.020(10) -0.030(10) 0.020(10) C27 0.080(9) 0.094(8) 0.145(10) 0.028(7) -0.035(8) -0.023(8)