#------------------------------------------------------------------------------ #$Date: 2008-01-13 23:15:36 +0100 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003392.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_2003392 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 777 _journal_page_last 780 _publ_section_title ; 2-Methylthio-10,11-dihydro-11-(4-methylpiperazin-1-yl)dibenzo[b,f]thiepine Maleic Acid (Metitepine Maleate) Internal code of the Janssen Research Foundation: R27199. ; _chemical_formula_moiety 'C20 H25 N2 S2 1+, C4 H3 O4 1-' _chemical_formula_sum 'C24 H28 N2 O4 S2' _chemical_formula_weight 472.61 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' _symmetry_space_group_name_H-M 'P 21/c' _cell_length_a 10.206(2) _cell_length_b 9.692(1) _cell_length_c 24.498(1) _cell_angle_alpha 90.00 _cell_angle_beta 91.91(2) _cell_angle_gamma 90.00 _cell_volume 2421.9(5) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_meas 1.299 _exptl_crystal_density_method 'flotation in n-heptane/CCl~4~' _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 16 _cell_measurement_theta_min 13 _cell_measurement_theta_max 30 _exptl_absorpt_coefficient_mu 2.260 _cell_measurement_temperature 293 _exptl_crystal_description 'prism' _exptl_crystal_size_max .26 _exptl_crystal_size_mid .26 _exptl_crystal_size_min .16 _exptl_crystal_colour 'colourless' _chemical_compound_source 'Janssen Research Foundation, Beerse, 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 .797 _exptl_absorpt_correction_T_max .996 _diffrn_reflns_number 4223 _reflns_number_total 3867 _reflns_number_observed 2816 _reflns_observed_criterion 'F^2^ > 3\s(F^2^)' _diffrn_reflns_av_R_equivalents .0140 _diffrn_reflns_theta_max 65.00 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_standards_number 3 _diffrn_standards_interval_count 50 _diffrn_standards_decay_% <1.0 _refine_ls_structure_factor_coef 'Fsqd' _refine_ls_R_factor_obs .0478 _refine_ls_wR_factor_obs .1492 _refine_ls_wR_factor_all .1730 _refine_ls_goodness_of_fit_obs 1.066 _refine_ls_goodness_of_fit_all 1.051 _refine_ls_number_reflns 3867 _refine_ls_number_parameters 293 _refine_ls_hydrogen_treatment 'noref' _refine_ls_weighting_scheme ; w=1/[\s^2^(Fo^2^)+(0.1025P)^2^+0.8810P] where P=(Fo^2^+2F~c~^2^)/3 ; _refine_ls_shift/esd_max <0.001 _refine_diff_density_max .41 _refine_diff_density_min -.29 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1994)' _refine_ls_extinction_coef .0021(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 N 'IT.4 Tab.2.2B 2.3.1' .0311 .0180 O 'IT.4 Tab.2.2B 2.3.1' .0492 .0322 S 'IT.4 Tab.2.2B 2.3.1' .3331 .5567 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv C1 .3431(4) .7079(5) .0712(2) .084(2) S2 .3196(1) .6274(1) .13483(4) .0883(4) C3 .1681(3) .6912(4) .1560(1) .057(1) C4 .1431(3) .6806(4) .2105(1) .055(1) C5 .0261(3) .7243(3) .2333(1) .049(1) C6 -.0698(3) .7773(3) .1971(1) .050(1) C7 -.0446(3) .7870(4) .1418(1) .059(1) C8 .0720(3) .7460(4) .1209(1) .063(1) C9 .0153(3) .7003(4) .2946(1) .056(1) C10 -.1024(4) .7618(5) .3220(2) .070(1) C11 -.2279(3) .6892(4) .3066(2) .068(1) C12 -.2930(3) .7222(3) .2573(1) .055(1) S13 -.22549(9) .8466(1) .21355(4) .0672(3) C14 -.2833(4) .5869(5) .3383(2) .092(2) C15 -.4025(4) .5262(5) .3226(2) .094(2) C16 -.4675(4) .5689(5) .2760(2) .086(2) C17 -.4129(3) .6648(4) .2435(2) .067(1) N18 .1428(3) .7341(3) .32206(9) .0489(8) C19 .1764(4) .8797(4) .3242(1) .062(1) C20 .3175(4) .8975(4) .3437(1) .067(1) N21 .3412(3) .8306(3) .3978(1) .0560(8) C22 .2994(3) .6833(4) .3959(1) .056(1) C23 .1587(3) .6743(3) .3765(1) .052(1) C24 .4796(4) .8443(5) .4180(2) .081(2) O25 .3171(3) 1.1342(3) .4533(1) .090(1) C26 .2146(3) 1.0839(4) .4722(1) .063(1) O27 .1824(3) .9608(3) .4660(1) .075(1) C28 .1223(4) 1.1727(4) .5022(2) .069(1) C29 .1241(4) 1.3069(4) .5112(2) .068(1) C30 .2171(4) 1.4156(4) .4963(2) .073(1) O31 .3188(3) 1.3839(3) .4680(2) .099(1) O32 .1952(4) 1.5343(3) .5089(2) .111(2) H1A .280(2) .673(2) .0447(3) .106 H1B .430(1) .689(3) .0594(6) .106 H1C .332(3) .8058(6) .0749(3) .106 H4 .2074(3) .6423(4) .2336(1) .069 H7 -.1092(3) .8227(4) .1182(1) .074 H8 .0866(3) .7547(4) .0838(1) .079 H9 .0057(3) .6003(4) .2987(1) .070 H10A -.0882(4) .7572(5) .3613(2) .087 H10B -.1103(4) .8583(5) .3119(2) .087 H14 -.2402(4) .5586(5) .3705(2) .115 H15 -.4377(4) .4568(5) .3439(2) .117 H16 -.5493(4) .5322(5) .2666(2) .107 H17 -.4570(3) .6922(4) .2114(2) .084 H19A .1191(4) .9271(4) .3489(1) .078 H19B .1639(4) .9201(4) .2882(1) .078 H20A .3749(4) .8569(4) .3173(1) .084 H20B .3378(4) .9951(4) .3465(1) .084 H21 .2901(3) .8746(3) .4221(1) .070 H22A .3098(3) .6426(4) .4319(1) .070 H22B .3540(3) .6324(4) .3712(1) .070 H23A .1312(3) .5785(3) .3757(1) .065 H23B .1040(3) .7235(3) .4017(1) .065 H24A .4907(7) .798(2) .4524(6) .101 H24B .5008(9) .9402(5) .423(1) .101 H24C .5365(4) .804(3) .3920(6) .101 H28 .0521(4) 1.1261(4) .5171(2) .086 H29 .0533(4) 1.3388(4) .5305(2) .086 H31 .326(3) 1.2997(3) .466(2) .124 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 C1 .079(3) .013(2) .019(2) .104(3) .002(2) .071(2) S2 .0718(6) .0448(7) .0103(4) .137(1) .0078(6) .0562(5) C3 .054(2) .010(2) .000(1) .071(2) .000(2) .047(2) C4 .053(2) .015(2) -.002(1) .070(2) .000(1) .043(2) C5 .045(2) .005(1) -.003(1) .055(2) -.004(1) .046(2) C6 .049(2) .004(1) .000(1) .050(2) .002(1) .051(2) C7 .057(2) .009(2) -.006(1) .067(2) .007(2) .053(2) C8 .059(2) .012(2) -.002(1) .083(2) .004(2) .047(2) C9 .051(2) .000(2) .000(1) .071(2) -.004(2) .045(2) C10 .066(2) .009(2) .002(2) .088(3) -.014(2) .056(2) C11 .052(2) .006(2) .009(2) .086(3) .002(2) .066(2) C12 .045(2) .005(1) .006(1) .058(2) -.008(2) .063(2) S13 .0541(5) .0163(4) .0065(4) .0669(6) .0139(4) .0808(6) C14 .065(2) .016(3) .020(2) .119(4) .036(3) .093(3) C15 .073(3) .000(2) .034(3) .084(3) .024(3) .126(4) C16 .057(2) -.009(2) .013(2) .081(3) -.012(3) .119(4) C17 .053(2) .002(2) .003(2) .073(2) -.012(2) .075(2) N18 .052(1) -.005(1) -.001(1) .053(2) .004(1) .041(1) C19 .078(2) -.007(2) -.001(2) .055(2) .009(2) .054(2) C20 .076(2) -.024(2) .006(2) .069(2) .007(2) .057(2) N21 .050(1) -.009(1) .004(1) .064(2) .000(1) .054(2) C22 .058(2) -.004(2) -.002(1) .059(2) .003(1) .052(2) C23 .057(2) -.011(1) .001(1) .054(2) .004(1) .045(2) C24 .055(2) -.014(2) -.005(2) .094(3) -.008(2) .093(3) O25 .066(2) -.008(1) .031(2) .074(2) -.007(2) .133(3) C26 .059(2) -.004(2) .000(2) .065(2) -.003(2) .063(2) O27 .079(2) -.011(1) .013(1) .063(2) -.012(1) .085(2) C28 .072(2) -.013(2) .016(2) .066(2) -.009(2) .070(2) C29 .082(3) -.006(2) .017(2) .067(2) -.003(2) .058(2) C30 .093(3) -.014(2) .008(2) .067(3) -.001(2) .058(2) O31 .090(2) -.020(2) .032(2) .073(2) -.001(2) .137(3) O32 .157(3) -.020(2) .039(2) .064(2) -.015(2) .113(3)