#------------------------------------------------------------------------------ #$Date: 2009-11-16 03:43:51 +0200 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2003032.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_2003032 _journal_name_full 'Acta Crystallographica, Section B' _journal_volume 54 _journal_year 1998 _journal_page_first 872 _journal_page_last 876 _chemical_name_systematic ; (Z)-3-[3-(3,5-dichloro-2,4,6-trimethylphenyl)isoxazol-4-yl]but-2-enal (ethoxycarbonyl)hydrazone - ethyl acetate solvate ; _chemical_formula_moiety 'C19 H21 Cl2 N3 O3, 0.34(C4 H8 O2)' _chemical_formula_sum 'C20.36 H23.72 Cl2 N3 O3.68' _chemical_formula_weight 440.1 _symmetry_cell_setting monoclinic _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M ' P 21/c ' 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 _cell_length_a 8.230(5) _cell_length_b 35.820(10) _cell_length_c 8.042(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.11(3) _cell_angle_gamma 90.00 _cell_volume 2309(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.3 _cell_measurement_theta_max 17.5 _cell_measurement_temperature 293 _exptl_crystal_description 'thin plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_meas 1.29 _exptl_crystal_density_method 'Floating crystals method' _exptl_crystal_F_000 921.3 _exptl_absorpt_coefficient_mu 0.31 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_process_details 'North, Phillips & Mathews (1968)' _exptl_absorpt_correction_T_min 0.775 _exptl_absorpt_correction_T_max 1.00 _diffrn_ambient_temperature 293 _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_source ' X-ray ' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD-4F' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 4029 _diffrn_reflns_av_R_equivalents 0. _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 2 _diffrn_standards_interval_time 240 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 19 -1 2 9 -4 _reflns_number_total 4029 _reflns_number_gt 1762 _reflns_threshold_expression ' Fo > 4 \s(Fo)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_gt 0.072 _refine_ls_wR_factor_ref 0.228 _refine_ls_goodness_of_fit_ref 0.96 _refine_ls_number_reflns 4029 _refine_ls_number_parameters 245 _refine_ls_number_restraints 2 _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo^2^)+(0.1196P)^2^], where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/esd_max -0.04 _refine_ls_shift/esd_mean 0.003 _refine_diff_density_max 0.32 _refine_diff_density_min -0.29 _refine_ls_extinction_method none _refine_ls_extinction_coef none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'CL' 'CL' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol O1 0.2756(6) 0.14710(10) -0.1837(4) 0.087(2) aniso . . O N2 0.3465(6) 0.11180(10) -0.1460(5) 0.077(2) aniso . . N C3 0.3725(6) 0.10770(10) 0.0191(6) 0.057(2) aniso . . C C4 0.3226(6) 0.14000(10) 0.0982(6) 0.056(2) aniso . . C C5 0.2631(7) 0.16310(10) -0.0342(6) 0.067(2) aniso . . C C6 0.4443(6) 0.07320(10) 0.1031(6) 0.052(2) aniso . . C C7 0.3418(7) 0.04160(10) 0.1035(6) 0.059(2) aniso . . C C8 0.4146(8) 0.01020(10) 0.1905(7) 0.066(2) aniso . . C C9 0.5804(8) 0.00830(10) 0.2754(7) 0.067(3) aniso . . C C10 0.6754(7) 0.0398(2) 0.2693(6) 0.061(2) aniso . . C C11 0.6148(7) 0.0724(2) 0.1859(6) 0.059(2) aniso . . C C12 0.1594(8) 0.0423(2) 0.0182(7) 0.080(3) aniso . . C CL13 0.2879(3) -0.02854(4) 0.1949(2) 0.0979(8) aniso . . CL C14 0.6516(9) -0.0272(2) 0.3725(8) 0.092(3) aniso . . C CL15 0.8862(2) 0.03848(5) 0.3723(2) 0.0970(7) aniso . . CL C16 0.7254(8) 0.1040(2) 0.1779(8) 0.086(3) aniso . . C C17 0.3321(6) 0.1473(2) 0.2824(6) 0.061(2) aniso . . C C18 0.2632(8) 0.1177(2) 0.3778(7) 0.079(2) aniso . . C C19 0.4000(6) 0.17880(10) 0.3574(6) 0.053(2) aniso . . C C20 0.4746(6) 0.2080(2) 0.2752(6) 0.059(2) aniso . . C N21 0.5274(5) 0.23790(10) 0.3528(5) 0.0580(10) aniso . . N N22 0.5946(6) 0.26320(10) 0.2579(5) 0.066(2) aniso . . N C23 0.6573(7) 0.2953(2) 0.3279(7) 0.065(2) aniso . . C O24 0.6620(6) 0.30510(10) 0.4718(5) 0.094(2) aniso . . O O25 0.7142(5) 0.31560(10) 0.2142(5) 0.081(2) aniso . . O C26 0.813(3) 0.3491(3) 0.2810(10) 0.085(5) iso . . C C26' 0.737(4) 0.3556(6) 0.259(2) 0.075(6) iso . . C C27 0.816(2) 0.3713(3) 0.1460(10) 0.203(7) aniso . . C H5 0.21940 0.18880 -0.02218 0.0674 iso d . H H121 0.12100 0.06680 -0.04660 0.0801 iso d . H H122 0.09332 0.03904 0.10729 0.0801 iso d . H H123 0.13616 0.02131 -0.06491 0.0801 iso d . H H141 0.57950 -0.03470 0.44720 0.0919 iso d . H H142 0.76756 -0.02088 0.44699 0.0919 iso d . H H143 0.66489 -0.04706 0.29216 0.0919 iso d . H H161 0.78440 0.11100 0.29530 0.0864 iso d . H H162 0.65480 0.12530 0.12322 0.0864 iso calc C16 H H163 0.80130 0.10000 0.11120 0.0864 iso d . H H181 0.26150 0.13020 0.48580 0.0791 iso calc C18 H H182 0.32120 0.09380 0.38850 0.0791 iso d . H H183 0.14627 0.11321 0.31471 0.0791 iso d . H H19 0.40000 0.18220 0.48130 0.0534 iso calc C19 H H20 0.48430 0.20450 0.15430 0.0591 iso calc C20 H H22 0.59690 0.25760 0.13740 0.0671 iso calc N22 H H261 0.93139 0.34134 0.34745 0.0846 iso calc C26 H H262 0.76205 0.36214 0.37265 0.0846 iso calc C26 H H61' 0.81057 0.35895 0.37849 0.0751 iso calc C26' H H62' 0.62765 0.36844 0.25724 0.0751 iso calc C26' H H271 0.88207 0.39406 0.18974 0.2031 iso calc C27 H H272 0.69838 0.37937 0.08165 0.2031 iso calc C27 H H273 0.86772 0.35857 0.05645 0.2031 iso calc C27 H H71' 0.83045 0.39888 0.17098 0.2031 iso calc C27 H H72' 0.74161 0.36914 0.02252 0.2031 iso calc C27 H H73' 0.92453 0.35965 0.14377 0.2031 iso calc C27 H 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 0.134(4) 0.068(2) 0.046(2) 0.023(2) -0.003(2) 0.0089(19) N2 0.107(4) 0.075(3) 0.048(3) 0.010(3) 0.015(3) -0.004(2) C3 0.056(3) 0.065(3) 0.046(3) -0.005(3) 0.007(2) -0.005(2) C4 0.061(3) 0.061(3) 0.042(3) -0.003(3) 0.007(2) -0.003(2) C5 0.096(4) 0.056(3) 0.043(3) 0.015(3) 0.001(3) -0.004(3) C6 0.067(4) 0.045(3) 0.045(3) 0.003(3) 0.018(3) -0.003(2) C7 0.073(4) 0.057(3) 0.051(3) 0.011(3) 0.023(3) -0.006(3) C8 0.093(5) 0.060(3) 0.054(3) -0.005(3) 0.034(3) -0.012(3) C9 0.096(5) 0.055(3) 0.054(3) 0.021(3) 0.028(3) 0.003(3) C10 0.062(3) 0.074(4) 0.049(3) 0.005(3) 0.017(3) 0.004(3) C11 0.059(3) 0.072(4) 0.048(3) 0.002(3) 0.018(3) 0.007(3) C12 0.081(4) 0.088(4) 0.073(4) -0.019(3) 0.021(3) -0.010(3) CL13 0.1439(16) 0.0662(9) 0.0928(12) -0.0309(10) 0.0463(11) -0.0060(8) C14 0.143(6) 0.067(4) 0.073(4) 0.038(4) 0.040(4) 0.019(3) CL15 0.0775(11) 0.1216(15) 0.0887(11) 0.0250(10) 0.0122(9) 0.0258(10) C16 0.082(4) 0.088(4) 0.086(4) -0.006(4) 0.010(4) 0.021(3) C17 0.068(4) 0.072(4) 0.044(3) 0.010(3) 0.018(3) 0.006(3) C18 0.106(5) 0.073(4) 0.063(3) -0.010(3) 0.030(3) -0.003(3) C19 0.067(3) 0.050(3) 0.047(3) 0.002(3) 0.019(2) -0.006(2) C20 0.065(4) 0.073(4) 0.040(3) -0.000(3) 0.013(2) -0.008(3) N21 0.072(3) 0.061(3) 0.042(2) 0.000(2) 0.017(2) 0.002(2) N22 0.097(3) 0.068(3) 0.036(2) -0.016(3) 0.024(2) -0.007(2) C23 0.075(4) 0.076(4) 0.045(3) -0.000(3) 0.014(3) -0.009(3) O24 0.137(4) 0.092(3) 0.062(3) -0.041(3) 0.041(2) -0.030(2) O25 0.105(3) 0.078(3) 0.063(2) -0.021(2) 0.026(2) -0.002(2) C27 0.302(16) 0.139(8) 0.151(9) -0.090(10) 0.016(10) -0.003(7)