#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003286.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_2003286 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 533 _journal_page_last 535 _publ_section_title ; 3-{2-[4-(4-Fluorobenzoyl)-1-piperidinyl]ethyl}-2-methyl-4H-pyrido[1,2-a]- pyrimidine-4-one (Pirenperone)* F/N* Internal code of the Janssen Research Foundation:R47465 ; _chemical_formula_moiety 'C23 H24 F1 N3 O2 ' _chemical_formula_sum 'C23 H24 F N3 O2' _[local]_cod_chemical_formula_sum_orig 'C23 H24 F1 N3 O2 ' _chemical_formula_weight 393.45 _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 P21/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 17.144(1) _cell_length_b 11.450(3) _cell_length_c 10.179(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.757(8) _cell_angle_gamma 90.00 _cell_volume 1997.9(6) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_meas 1.32 _exptl_crystal_density_method 'flotation in n-heptane/CCl4' _cell_measurement_radiation 'Cu K\a' _cell_measurement_wavelength 1.54184 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 20 _cell_measurement_theta_max 25 _exptl_absorpt_coefficient_mu .740 _cell_measurement_temperature 293 _exptl_crystal_description 'prism' _exptl_crystal_size_max .50 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .10 _exptl_crystal_colour 'colourless' _chemical_compound_source 'Janssen Research Foundation, Belgium' _diffrn_measurement_device 'Hilger & Watts four-circle diffractometer' _diffrn_measurement_method '\w/2\q scan' _exptl_absorpt_correction_type 'empirical (North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min .915 _exptl_absorpt_correction_T_max .997 _diffrn_reflns_number 3491 _reflns_number_total 3170 _reflns_number_observed 1167 _reflns_observed_criterion '> 6.0 sigma(F)' _diffrn_reflns_av_R_equivalents .0244 _diffrn_reflns_theta_max 70.00 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count 50 _diffrn_standards_decay_% <3 _refine_ls_structure_factor_coef 'Fsqd' _refine_ls_R_factor_obs .0748 _refine_ls_wR_factor_obs .1648 _refine_ls_wR_factor_all .2297 _refine_ls_goodness_of_fit_obs 1.44 _refine_ls_goodness_of_fit_all 1.13 _refine_ls_number_reflns 3170 _refine_ls_number_parameters 264 _refine_ls_hydrogen_treatment 'noref' _refine_ls_weighting_scheme ; w=1/[\s^2^(F~o~^2^) + (0.0566P)^2^ + 2.5198P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max .026 _refine_diff_density_max .26 _refine_diff_density_min -.16 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1994)' _refine_ls_extinction_coef .0014(3) loop_ _atom_type_symbol _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C 'IT.4 Tab.2.2B 2.3.1' .0181 .0091 H 'IT.4 Tab.2.2B 2.3.1' .0000 .0000 F 'IT.4 Tab.2.2B 2.3.1' .0727 .0534 N 'IT.4 Tab.2.2B 2.3.1' .0311 .0180 O 'IT.4 Tab.2.2B 2.3.1' .0492 .0322 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv F1 .9128(2) .5792(4) .5902(4) .095(2) C2 .8561(4) .5108(6) .5350(7) .060(3) C3 .7848(4) .5081(6) .5914(7) .067(3) C4 .7276(4) .4390(6) .5351(6) .060(3) C5 .7430(3) .3752(6) .4224(6) .053(2) C6 .8168(3) .3828(6) .3692(6) .060(3) C7 .8745(4) .4487(6) .4270(7) .065(3) C8 .6837(4) .2991(7) .3561(7) .069(3) O9 .7008(3) .2527(5) .2529(6) .113(3) C10 .6034(4) .2822(6) .4094(7) .069(3) C11 .5496(4) .3727(7) .3537(9) .093(4) C12 .4654(4) .3543(7) .396(1) .116(5) N13 .4385(3) .2410(5) .3587(6) .069(2) C14 .4848(4) .1534(7) .4190(9) .103(4) C15 .5703(4) .1630(7) .376(1) .106(4) C16 .3550(4) .2253(7) .3914(8) .085(3) C17 .3183(3) .1273(6) .3109(7) .065(3) C18 .2304(3) .1227(6) .3237(6) .055(2) C19 .1902(4) .0515(6) .4068(6) .057(2) C20 .2323(4) -.0301(6) .4993(7) .082(3) N21 .1116(3) .0444(4) .4124(5) .056(2) C22 .0711(3) .1124(5) .3326(6) .048(2) N23 .1050(3) .1919(4) .2487(5) .050(2) C24 .1885(4) .2022(6) .2409(7) .057(3) O25 .2147(3) .2746(4) .1654(5) .079(2) C26 -.0116(4) .1055(6) .3312(6) .060(3) C27 -.0550(4) .1717(6) .2487(7) .068(3) C28 -.0182(4) .2521(7) .1661(7) .069(3) C29 .0593(4) .2608(6) .1673(7) .063(3) H3 .7747(4) .5518(6) .6662(7) .083 H4 .6785(4) .4351(6) .5727(6) .076 H6 .8274(3) .3423(6) .2923(6) .075 H7 .9246(4) .4505(6) .3931(7) .081 H10 .6057(4) .2908(6) .5052(7) .086 H11A .5519(4) .3706(7) .2586(9) .117 H11B .5669(4) .4493(7) .3825(9) .117 H12A .4620(4) .3631(7) .490(1) .146 H12B .4323(4) .4130(7) .355(1) .146 H14A .4646(4) .0771(7) .3952(9) .129 H14B .4821(4) .1611(7) .5138(9) .129 H15A .6011(4) .1033(7) .420(1) .132 H15B .5735(4) .1500(7) .282(1) .132 H16A .3270(4) .2975(7) .3742(8) .106 H16B .3505(4) .2076(7) .4841(8) .106 H17A .3313(3) .1380(6) .2192(7) .081 H17B .3403(3) .0533(6) .3395(7) .081 H20A .275(2) .011(1) .541(3) .102 H20B .252(2) -.095(2) .451(1) .102 H20C .1968(7) -.058(3) .565(3) .102 H26 -.0362(4) .0544(6) .3883(6) .075 H27 -.1090(4) .1640(6) .2466(7) .085 H28 -.0479(4) .2994(7) .1105(7) .087 H29 .0832(4) .3144(6) .1122(7) .078 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 F1 .078(3) -.027(3) -.022(3) .097(3) -.004(3) .108(4) C2 .054(4) -.007(4) -.014(4) .052(5) .008(4) .075(5) C3 .060(4) .002(4) -.004(4) .072(5) -.007(4) .068(5) C4 .045(4) .002(4) -.001(3) .073(5) .000(4) .064(5) C5 .043(3) .000(3) .002(3) .056(4) .011(4) .059(4) C6 .051(4) .004(4) .010(3) .060(5) -.002(4) .068(5) C7 .041(4) -.001(4) .001(3) .070(5) .015(4) .084(5) C8 .054(4) -.005(4) .010(4) .081(6) -.015(4) .072(5) O9 .082(4) -.037(4) .026(3) .140(5) -.067(4) .117(5) C10 .050(4) -.012(4) -.004(3) .080(6) -.027(4) .077(5) C11 .072(5) .000(4) .007(5) .058(5) .000(5) .151(8) C12 .058(5) -.002(5) .019(6) .081(7) -.039(7) .21(1) N13 .039(3) .003(3) -.007(3) .054(4) -.025(4) .112(5) C14 .068(5) -.017(5) -.014(5) .083(6) .034(6) .160(9) C15 .052(5) .002(4) -.017(5) .080(6) .024(6) .186(9) C16 .046(4) -.003(4) .002(4) .090(6) -.037(5) .118(7) C17 .045(4) -.004(4) .007(3) .065(5) -.020(4) .085(5) C18 .039(3) -.004(3) .001(3) .062(5) -.019(4) .063(4) C19 .050(4) .006(4) .000(3) .058(5) -.002(4) .063(4) C20 .066(5) .014(4) .004(4) .089(6) .010(5) .090(6) N21 .042(3) -.002(3) .007(3) .060(4) .007(3) .065(4) C22 .044(3) .000(3) -.002(3) .044(4) -.007(3) .055(4) N23 .049(3) .000(3) .002(2) .041(3) .000(3) .060(3) C24 .054(4) -.012(4) .012(3) .060(5) -.008(4) .059(4) O25 .071(3) -.019(3) .015(3) .082(4) .020(3) .085(4) C26 .047(4) -.004(4) .003(3) .071(5) -.007(4) .063(4) C27 .047(4) .003(4) -.006(4) .073(5) -.009(4) .083(5) C28 .061(4) .013(4) -.012(4) .080(6) .002(4) .067(5) C29 .066(4) -.001(4) .000(4) .059(5) .007(4) .063(5) _cod_database_code 2003286