#------------------------------------------------------------------------------ #$Date: 2011-01-02 20:00:31 +0000 (Sun, 02 Jan 2011) $ #$Revision: 5310 $ #$URL: svn://www.crystallography.net/cod/cif/2/2103742.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2103742 loop_ _publ_author_name 'Kaftory, Menahem' 'Botoshansky, Mark' 'Kapon, Moshe' 'Shteiman, Vitaly' _publ_section_title ; Irreversible single-crystal to polycrystal and reversible single-crystal to single-crystal phase transformations in cyanurates ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 791 _journal_page_last 799 _journal_volume 57 _journal_year 2001 _chemical_formula_moiety 'C6 H9 N3 O3' _chemical_formula_sum 'C6 H9 N3 O3' _chemical_formula_weight 171.16 _chemical_name_common 'OON (methoxy cyanurate)' _chemical_name_systematic ; 4,6-Dimethoxy-3-methyl-dihydro-triazine-2-one ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 92.07(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 13.480(2) _cell_length_b 14.172(2) _cell_length_c 8.4330(10) _cell_measurement_reflns_used 3758 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 28.2 _cell_measurement_theta_min 1.0 _cell_volume 1610.0(2) _computing_cell_refinement 'DENZO SMN (Otwinowski & Minor,1997)' _computing_data_collection 'KappaCCD (Nonius,2000)' _computing_data_reduction 'DENZO SMN (Otwinowski & Minor,1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full .944 _diffrn_measured_fraction_theta_max .944 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method phi-scan _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71070 _diffrn_reflns_av_R_equivalents .046 _diffrn_reflns_av_sigmaI/netI .0423 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 3758 _diffrn_reflns_theta_full 28.26 _diffrn_reflns_theta_max 28.26 _diffrn_reflns_theta_min 2.09 _diffrn_standards_number no _exptl_absorpt_coefficient_mu .115 _exptl_absorpt_correction_type none _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 720 _exptl_crystal_size_max .35 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .3 _refine_diff_density_max .223 _refine_diff_density_min -.184 _refine_ls_extinction_coef .046(7) _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 224 _refine_ls_number_reflns 3758 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.041 _refine_ls_R_factor_all .0995 _refine_ls_R_factor_gt .0559 _refine_ls_shift/su_max .158 _refine_ls_shift/su_mean .004 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0773P)^2^+0.7666P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .1803 _reflns_number_gt 2273 _reflns_number_total 3758 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file av0042.cif _[local]_cod_data_source_block LTP _[local]_cod_cif_authors_sg_H-M 'P 21 /n' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value 'None' changed to 'none' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 2103742 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol O11 .11930(16) -.09655(14) .7723(2) .0723(6) Uani d . 1 O O12 .12214(13) -.03273(13) .24944(19) .0576(5) Uani d . 1 O O13 .15749(13) .20508(12) .6010(2) .0542(5) Uani d . 1 O N11 .13655(14) .05751(13) .7000(2) .0441(5) Uani d . 1 N N12 .11726(13) -.06465(13) .5092(2) .0420(5) Uani d . 1 N N13 .14134(14) .09077(14) .4230(2) .0439(5) Uani d . 1 N C11 .12442(17) -.03665(17) .6687(3) .0446(5) Uani d . 1 C C12 .12741(14) .00114(17) .3955(2) .0407(5) Uani d . 1 C C13 .14419(15) .11299(16) .5788(3) .0389(5) Uani d . 1 C C14 .1049(2) -.16529(17) .4719(4) .0593(7) Uani d . 1 C H14A .0650 -.1720 .3759 .089 Uiso calc R 1 H H14B .0727 -.1962 .5573 .089 Uiso calc R 1 H H14C .1688 -.1934 .4581 .089 Uiso calc R 1 H C15 .1289(2) .0353(2) .1206(3) .0720(9) Uani d . 1 C H15A .0754 .0797 .1255 .108 Uiso calc R 1 H H15B .1248 .0027 .0207 .108 Uiso calc R 1 H H15C .1911 .0681 .1306 .108 Uiso calc R 1 H C16 .1601(2) .2405(2) .7618(3) .0701(8) Uani d . 1 C H16A .0962 .2321 .8064 .105 Uiso calc R 1 H H16B .1767 .3063 .7615 .105 Uiso calc R 1 H H16C .2092 .2065 .8242 .105 Uiso calc R 1 H O21 .09978(19) .65764(14) 1.2798(2) .0806(7) Uani d . 1 O O22 .11168(12) .59344(13) .75859(18) .0521(5) Uani d . 1 O O23 .14528(13) .35632(11) 1.1130(2) .0534(5) Uani d . 1 O N21 .12268(14) .50404(13) 1.2092(2) .0440(5) Uani d . 1 N N22 .10644(13) .62603(13) 1.0175(2) .0406(5) Uani d . 1 N N23 .12913(13) .46987(13) .9328(2) .0407(5) Uani d . 1 N C21 .10944(18) .59785(17) 1.1775(3) .0459(6) Uani d . 1 C C22 .11627(14) .55969(16) .9045(2) .0375(5) Uani d . 1 C C23 .13180(15) .44823(15) 1.0888(3) .0376(5) Uani d . 1 C C24 .0944(2) .72659(17) .9794(3) .0563(7) Uani d . 1 C H24A .1569 .7521 .9490 .084 Uiso calc R 1 H H24B .0721 .7597 1.0708 .084 Uiso calc R 1 H H24C .0464 .7337 .8934 .084 Uiso calc R 1 H C25 .1210(2) .5256(2) .6301(3) .0648(8) Uani d . 1 C H25A .1838 .4940 .6414 .097 Uiso calc R 1 H H25B .1168 .5580 .5301 .097 Uiso calc R 1 H H25C .0684 .4800 .6343 .097 Uiso calc R 1 H C26 .1506(2) .3232(2) 1.2754(3) .0665(8) Uani d . 1 C H26A .2017 .3569 1.3338 .100 Uiso calc R 1 H H26B .1655 .2569 1.2770 .100 Uiso calc R 1 H H26C .0880 .3337 1.3232 .100 Uiso calc R 1 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 O11 .1178(17) .0489(12) .0504(12) -.0053(11) .0054(10) .0144(10) O12 .0698(11) .0662(13) .0369(9) -.0008(9) .0015(7) -.0144(8) O13 .0736(11) .0344(10) .0546(11) -.0034(8) .0033(8) -.0070(8) N11 .0577(11) .0414(11) .0333(10) .0003(9) .0028(8) -.0024(8) N12 .0475(10) .0352(11) .0432(11) -.0018(8) .0012(8) -.0065(8) N13 .0552(11) .0402(12) .0363(10) .0005(8) .0023(8) -.0008(8) C11 .0544(13) .0402(14) .0392(13) -.0002(10) .0022(9) .0034(10) C12 .0392(11) .0480(14) .0347(12) .0018(9) .0004(8) -.0068(10) C13 .0413(11) .0354(13) .0398(12) .0014(9) .0019(8) -.0029(10) C14 .0654(16) .0384(15) .0739(19) -.0042(11) .0021(13) -.0123(13) C15 .090(2) .093(2) .0334(14) .0019(17) .0034(12) -.0005(14) C16 .091(2) .0542(18) .0657(19) -.0028(14) .0043(14) -.0282(15) O21 .150(2) .0465(11) .0453(11) .0054(12) .0063(11) -.0125(9) O22 .0644(10) .0589(11) .0328(9) -.0021(8) .0005(7) .0116(8) O23 .0754(11) .0334(10) .0512(10) .0030(8) .0006(8) .0064(8) N21 .0606(12) .0376(11) .0337(10) -.0008(9) .0011(8) .0032(8) N22 .0510(10) .0324(10) .0385(10) -.0021(8) .0020(7) .0046(8) N23 .0517(11) .0378(11) .0326(10) .0000(8) .0002(7) -.0009(8) C21 .0670(15) .0376(13) .0332(12) -.0020(11) .0017(10) .0008(10) C22 .0380(11) .0441(13) .0302(11) -.0040(9) .0007(8) .0065(9) C23 .0404(11) .0347(12) .0377(12) -.0008(8) .0002(8) .0036(9) C24 .0737(16) .0330(13) .0624(17) .0023(11) .0042(12) .0101(12) C25 .0781(18) .088(2) .0285(13) -.0035(15) -.0003(11) .0008(13) C26 .092(2) .0480(16) .0585(17) .0026(14) -.0034(14) .0225(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C12 O12 C15 116.9(2) C13 O13 C16 118.1(2) C13 N11 C11 116.83(19) C12 N12 C11 118.79(19) C12 N12 C14 122.2(2) C11 N12 C14 118.9(2) C12 N13 C13 113.55(19) O11 C11 N11 123.3(2) O11 C11 N12 119.0(2) N11 C11 N12 117.7(2) N13 C12 O12 121.5(2) N13 C12 N12 124.4(2) O12 C12 N12 114.1(2) N11 C13 O13 119.9(2) N11 C13 N13 128.7(2) O13 C13 N13 111.4(2) N12 C14 H14A 109.5 N12 C14 H14B 109.5 H14A C14 H14B 109.5 N12 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 O12 C15 H15A 109.5 O12 C15 H15B 109.5 H15A C15 H15B 109.5 O12 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 O13 C16 H16A 109.5 O13 C16 H16B 109.5 H16A C16 H16B 109.5 O13 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 C22 O22 C25 116.8(2) C23 O23 C26 117.7(2) C23 N21 C21 117.08(19) C22 N22 C21 118.69(19) C22 N22 C24 122.30(19) C21 N22 C24 119.0(2) C22 N23 C23 113.50(18) O21 C21 N21 123.6(2) O21 C21 N22 118.8(2) N21 C21 N22 117.6(2) N23 C22 O22 121.7(2) N23 C22 N22 124.45(19) O22 C22 N22 113.8(2) N21 C23 O23 119.6(2) N21 C23 N23 128.7(2) O23 C23 N23 111.76(19) N22 C24 H24A 109.5 N22 C24 H24B 109.5 H24A C24 H24B 109.5 N22 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 O22 C25 H25A 109.5 O22 C25 H25B 109.5 H25A C25 H25B 109.5 O22 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 O23 C26 H26A 109.5 O23 C26 H26B 109.5 H26A C26 H26B 109.5 O23 C26 H26C 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O11 C11 1.221(3) O12 C12 1.321(3) O12 C15 1.458(3) O13 C13 1.330(3) O13 C16 1.445(3) N11 C13 1.297(3) N11 C11 1.369(3) N12 C12 1.348(3) N12 C11 1.402(3) N12 C14 1.469(3) N13 C12 1.304(3) N13 C13 1.350(3) C14 H14A .9600 C14 H14B .9600 C14 H14C .9600 C15 H15A .9600 C15 H15B .9600 C15 H15C .9600 C16 H16A .9600 C16 H16B .9600 C16 H16C .9600 O21 C21 1.220(3) O22 C22 1.319(2) O22 C25 1.457(3) O23 C23 1.330(3) O23 C26 1.447(3) N21 C23 1.297(3) N21 C21 1.367(3) N22 C22 1.349(3) N22 C21 1.406(3) N22 C24 1.469(3) N23 C22 1.306(3) N23 C23 1.350(3) C24 H24A .9600 C24 H24B .9600 C24 H24C .9600 C25 H25A .9600 C25 H25B .9600 C25 H25C .9600 C26 H26A .9600 C26 H26B .9600 C26 H26C .9600 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C13 N11 C11 O11 177.7(2) C13 N11 C11 N12 -2.5(3) C12 N12 C11 O11 -177.1(2) C14 N12 C11 O11 -.6(3) C12 N12 C11 N11 3.2(3) C14 N12 C11 N11 179.6(2) C13 N13 C12 O12 179.63(18) C13 N13 C12 N12 -.4(3) C15 O12 C12 N13 -2.2(3) C15 O12 C12 N12 177.8(2) C11 N12 C12 N13 -1.7(3) C14 N12 C12 N13 -178.0(2) C11 N12 C12 O12 178.26(18) C14 N12 C12 O12 1.9(3) C11 N11 C13 O13 -179.06(19) C11 N11 C13 N13 .4(3) C16 O13 C13 N11 -1.7(3) C16 O13 C13 N13 178.72(19) C12 N13 C13 N11 1.2(3) C12 N13 C13 O13 -179.36(18) C23 N21 C21 O21 179.9(2) C23 N21 C21 N22 .2(3) C22 N22 C21 O21 -179.4(2) C24 N22 C21 O21 1.6(3) C22 N22 C21 N21 .3(3) C24 N22 C21 N21 -178.7(2) C23 N23 C22 O22 -179.90(17) C23 N23 C22 N22 .0(3) C25 O22 C22 N23 .4(3) C25 O22 C22 N22 -179.53(19) C21 N22 C22 N23 -.4(3) C24 N22 C22 N23 178.5(2) C21 N22 C22 O22 179.53(18) C24 N22 C22 O22 -1.5(3) C21 N21 C23 O23 179.70(19) C21 N21 C23 N23 -.7(3) C26 O23 C23 N21 -.9(3) C26 O23 C23 N23 179.4(2) C22 N23 C23 N21 .6(3) C22 N23 C23 O23 -179.80(18)