#------------------------------------------------------------------------------ #$Date: 2008-01-26 18:25:03 +0100 (Sat, 26 Jan 2008) $ #$Revision: 20 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003234.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_2003234 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 519 _journal_page_last 521 _publ_section_title ; 6-Ethyl-9-fluoro-6,7-dihydro-8-(4-hydroxy-1-piperidino)- 5-methyl-1-oxo-1H,5H-benzo[i,j]quinolizine-2-carboxylic Acid ; _chemical_formula_moiety 'C21 H25 F N2 O4' _chemical_formula_sum 'C21 H25 F N2 O4' _chemical_formula_weight 388.44 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y,1/2+z' '1/2-x,1/2+y,1/2+z' '1/2+x,1/2-y, +z' _symmetry_space_group_name_H-M 'P n a 21' _cell_length_a 15.387(2) _cell_length_b 7.705(2) _cell_length_c 16.013(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1898(1) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_meas 1.355(3) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.7107 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.2 _cell_measurement_theta_max 16.5 _exptl_absorpt_coefficient_mu 0.094 _cell_measurement_temperature 296 _exptl_crystal_description 'plate-like' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.4 _exptl_crystal_colour 'colorless' _chemical_compound_source ;synthesized and crystallized from EtOH/H~2~O solution ; _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 1948 _reflns_number_total 1948 _reflns_number_observed 1188 _reflns_observed_criterion I>3\s(I) _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 25.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 'no significant change' _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.036 _refine_ls_wR_factor_obs 0.040 _refine_ls_wR_factor_all ? _refine_ls_goodness_of_fit_obs 1.20 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 1188 _refine_ls_number_parameters 277 _refine_ls_hydrogen_treatment refU _refine_ls_weighting_scheme 'w = 4F~o~^2^/\s^2^(F~o~)^2^' _refine_ls_shift/esd_max 0.33 _refine_diff_density_max 0.13 _refine_diff_density_min -0.15 _refine_ls_extinction_method 'not applied' _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C 'International Tables' 0.003 0.002 H 'International Tables' 0.000 0.000 O 'International Tables' 0.011 0.006 N 'International Tables' 0.006 0.003 F 'International Tables' 0.017 0.010 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? ; AFC/MSC Data Collection and Refinement Software (Rigaku Corporation, 1988) ; ; AFC/MSC Data Collection and RefinementSoftware ; ; TEXSAN PROCESS (Molecular Structure Corporation, 1985) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_B_iso_or_equiv F(1) 0.1474(2) -0.0310(3) 0.9711 4.6(1) O(1) 0.1816(3) 0.7914(5) 0.6302(3) 5.8(2) O(2) 0.0859(2) 0.7853(5) 0.7330(3) 4.9(2) O(3) 0.0715(2) 0.5136(4) 0.8220(3) 4.1(2) O(4) 0.3934(3) -0.4027(5) 1.0608(3) 6.0(2) N(1) 0.2847(2) 0.3171(4) 0.7022(3) 2.6(2) N(2) 0.3005(2) -0.1666(4) 0.8946(3) 2.7(2) C(1) 0.2497(3) 0.4703(6) 0.6799(3) 3.1(2) C(2) 0.1791(3) 0.5409(6) 0.7167(4) 3.3(2) C(3) 0.1362(3) 0.4520(6) 0.7834(3) 2.9(2) C(4) 0.1732(3) 0.2864(5) 0.8067(3) 2.6(2) C(5) 0.1383(3) 0.1914(6) 0.8735(3) 3.0(2) C(6) 0.1807(3) 0.0482(6) 0.9013(3) 3.1(2) C(7) 0.2560(3) -0.0184(5) 0.8647(3) 2.5(2) C(8) 0.2876(2) 0.0658(5) 0.7938(3) 2.3(2) C(9) 0.2485(3) 0.2222(6) 0.7675(3) 2.5(2) C(10) 0.3690(3) 0.2600(6) 0.6641(3) 3.0(2) C(11) 0.3662(3) 0.0635(6) 0.6565(3) 3.0(2) C(12) 0.3601(3) -0.0166(6) 0.7429(3) 2.7(2) C(13) 0.4444(3) 0.3332(6) 0.7145(4) 4.0(3) C(14) 0.1495(3) 0.7132(6) 0.6884(4) 4.1(3) C(15) 0.2539(3) -0.3032(6) 0.9397(3) 3.4(2) C(16) 0.3068(4) -0.4699(6) 0.9376(4) 3.8(2) C(17) 0.3982(3) -0.4447(6) 0.9741(4) 4.1(2) C(18) 0.4417(3) -0.2925(6) 0.9305(4) 4.2(3) C(19) 0.3854(3) -0.1303(6) 0.9335(3) 3.1(2) C(20) 0.4430(3) -0.0041(6) 0.6058(4) 3.9(3) C(21) 0.4344(4) -0.1965(8) 0.5850(4) 5.5(3) H(1) 0.2765 0.5297 0.6310 4(1) H(2) 0.0846 0.2424 0.9038 4(1) H(3) 0.3688 0.3184 0.6100 4(1) H(4) 0.3189 0.0374 0.6170 3(1) H(5) 0.4153 0.0020 0.7718 5(1) H(6) 0.3496 -0.1390 0.7369 4(1) H(7) 0.4516 0.2908 0.7723 3(1) H(8) 0.4970 0.3137 0.6822 7(2) H(9) 0.4443 0.4831 0.7239 7(2) H(10) 0.1840 -0.3115 0.9109 4(1) H(11) 0.2469 -0.2681 1.0018 4(1) H(12) 0.3134 -0.5206 0.8819 3(1) H(13) 0.2782 -0.5601 0.9712 7(2) H(14) 0.4256 -0.5585 0.9672 4(1) H(15) 0.4398 -0.3470 0.8634 7(2) H(16) 0.5061 -0.2743 0.9650 4(1) H(17) 0.3813 -0.0942 0.9975 3(1) H(18) 0.4201 -0.0349 0.9032 2.3(9) H(19) 0.4450 0.0645 0.5525 3(1) H(20) 0.5016 0.0248 0.6388 5(1) H(21) 0.4511 -0.2394 0.6321 6(2) H(22) 0.3684 -0.2192 0.5543 12(3) H(23) 0.4770 -0.2204 0.5448 4(1) H(24) 0.0689 0.7153 0.7691 7(2) H(25) 0.3717 -0.5022 1.0819 11(2) 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 F(1) 0.063(2) 0.006(2) 0.023(2) 0.062(2) 0.017(2) 0.049(2) O(1) 0.080(3) 0.017(2) 0.005(2) 0.053(2) 0.034(2) 0.088(3) O(2) 0.061(3) 0.015(2) -0.003(2) 0.041(2) 0.004(2) 0.084(3) O(3) 0.040(2) 0.009(2) 0.002(2) 0.051(2) 0.001(2) 0.065(2) O(4) 0.108(3) -0.032(2) -0.035(2) 0.063(2) 0.028(2) 0.056(2) N(1) 0.034(2) 0.002(2) -0.000(2) 0.032(2) 0.009(2) 0.034(2) N(2) 0.032(2) -0.008(2) 0.000(2) 0.034(2) 0.013(2) 0.037(2) C(1) 0.045(3) -0.002(2) -0.006(2) 0.035(3) 0.007(2) 0.038(3) C(2) 0.036(3) 0.004(2) -0.011(2) 0.039(3) 0.006(2) 0.049(3) C(3) 0.031(2) 0.004(2) -0.004(2) 0.039(3) -0.006(2) 0.042(3) C(4) 0.030(2) 0.000(2) -0.000(2) 0.031(2) 0.001(2) 0.038(3) C(5) 0.032(2) -0.000(2) 0.005(2) 0.040(3) -0.002(2) 0.042(3) C(6) 0.040(3) -0.006(2) 0.009(2) 0.041(3) 0.010(2) 0.035(3) C(7) 0.032(2) -0.002(2) -0.002(2) 0.032(2) 0.006(2) 0.031(2) C(8) 0.027(2) 0.000(2) -0.004(2) 0.032(2) 0.003(2) 0.030(2) C(9) 0.031(2) -0.002(2) -0.004(2) 0.034(3) 0.001(2) 0.028(2) C(10) 0.041(3) 0.003(2) 0.005(2) 0.040(3) 0.012(2) 0.034(2) C(11) 0.037(3) 0.004(2) -0.001(2) 0.047(3) 0.005(2) 0.031(2) C(12) 0.035(3) 0.004(2) 0.005(2) 0.033(2) 0.005(2) 0.036(3) C(13) 0.036(3) -0.006(2) 0.001(3) 0.046(3) 0.004(3) 0.069(4) C(14) 0.046(3) 0.004(3) -0.014(3) 0.043(3) 0.006(3) 0.068(4) C(15) 0.042(3) -0.006(2) 0.002(2) 0.040(3) 0.011(3) 0.046(3) C(16) 0.062(3) -0.012(2) -0.007(3) 0.035(3) 0.005(3) 0.046(3) C(17) 0.058(3) -0.003(2) -0.022(3) 0.035(3) 0.015(3) 0.065(3) C(18) 0.048(3) -0.005(2) -0.013(3) 0.045(3) 0.017(3) 0.066(4) C(19) 0.041(3) -0.013(2) -0.007(2) 0.035(2) 0.011(2) 0.042(3) C(20) 0.053(4) 0.012(3) 0.017(3) 0.053(3) 0.007(3) 0.042(3) C(21) 0.084(5) 0.018(3) 0.013(3) 0.072(4) -0.010(3) 0.053(4)