#------------------------------------------------------------------------------ #$Date: 2011-09-17 22:27:16 +0200 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003257.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_2003257 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 527 _journal_page_last 529 _publ_section_title ; 2,2-Dimethyl-5-(2-methyl-4-phenyl-3,4-diaza-2-butenylidene)-1,3-dioxane -4,6-dione ; _chemical_formula_sum 'C15 H16 N2 O4' _chemical_formula_structural 'C15 H16 N2 O4' _chemical_formula_weight 288.30 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _symmetry_space_group_name_H-M 'P -1' _cell_length_a 7.544(3) _cell_length_b 8.576(3) _cell_length_c 12.014(7) _cell_angle_alpha 78.01(3) _cell_angle_beta 83.36(3) _cell_angle_gamma 71.41(3) _cell_volume 719.6(6) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 12 _cell_measurement_theta_min 15 _cell_measurement_theta_max 16 _exptl_absorpt_coefficient_mu 0.098 _cell_measurement_temperature 295(2) _exptl_crystal_description Lath _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.075 _exptl_crystal_colour Orange _chemical_compound_source ; The title compound was obtained by the reaction of PhNHN=C(Me)CHO with 2,2-dimethyl-1,3-dioxane-4,6-dione. Crystals were grown from ethanol (McNab & Stobie, 1982). ; _diffrn_measurement_device 'Stoe Stadi-4' _diffrn_measurement_method '\w-2\q' _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 1858 _reflns_number_total 1847 _reflns_number_observed 1499 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0116 _diffrn_reflns_theta_max 22.52 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 2.0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0397 _refine_ls_wR_factor_obs 0.1285 _refine_ls_wR_factor_all 0.1394 _refine_ls_goodness_of_fit_obs 1.124 _refine_ls_goodness_of_fit_all 1.056 _refine_ls_number_reflns 1845 _refine_ls_number_parameters 185 _refine_ls_hydrogen_treatment ; H10 was constrained to lie 1.00\%A from N10, other H atoms were placed in calculated positions. ; _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.1000P)^2^ + 0.0000P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.367 _refine_diff_density_max 0.216 _refine_diff_density_min -0.200 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_extinction_coef 0.0458(87) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.001 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.003 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.006 loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv O1 1 0.2374(2) 0.2956(2) 0.82567(12) 0.0474(5) C2 1 0.2004(3) 0.4137(2) 0.7209(2) 0.0408(6) C2A 1 0.2316(4) 0.3119(3) 0.6290(2) 0.0569(7) H2A1 1 0.1422(4) 0.2507(3) 0.6405(2) 0.068 H2A2 1 0.3560(4) 0.2349(3) 0.6315(2) 0.068 H2A3 1 0.2164(4) 0.3848(3) 0.5561(2) 0.068 C2B 1 0.0055(3) 0.5346(3) 0.7267(2) 0.0554(7) H2B1 1 -0.0843(3) 0.4738(3) 0.7411(2) 0.066 H2B2 1 -0.0175(3) 0.6115(3) 0.6556(2) 0.066 H2B3 1 -0.0056(3) 0.5954(3) 0.7871(2) 0.066 O3 1 0.3367(2) 0.5016(2) 0.69950(11) 0.0439(4) C4 1 0.3673(3) 0.5714(2) 0.7839(2) 0.0400(6) O4 1 0.4654(2) 0.6617(2) 0.76169(13) 0.0602(5) C5 1 0.2926(3) 0.5147(2) 0.8982(2) 0.0355(5) C6 1 0.2617(3) 0.3502(3) 0.9186(2) 0.0412(6) O6 1 0.2589(3) 0.2608(2) 1.01041(13) 0.0615(5) C7 1 0.2684(3) 0.5915(2) 0.9891(2) 0.0384(5) H7 1 0.2526(3) 0.5235(2) 1.0583(2) 0.046 C8 1 0.2622(3) 0.7571(2) 1.0000(2) 0.0364(5) C8M 1 0.2414(3) 0.9034(3) 0.9051(2) 0.0491(6) H8M1 1 0.1892(19) 0.8770(21) 0.8333(9) 0.059 H8M2 1 0.3715(12) 0.9315(20) 0.8794(13) 0.059 H8M3 1 0.1399(15) 1.0095(14) 0.9346(14) 0.059 N9 1 0.2675(2) 0.7654(2) 1.10718(14) 0.0381(5) N10 1 0.2704(2) 0.9075(2) 1.13387(13) 0.0387(5) H10 1 0.2641(29) 1.0112(15) 1.0761(13) 0.046 C1P 1 0.2730(2) 0.9166(2) 1.24865(8) 0.0354(5) C2P 1 0.3019(2) 1.05723(14) 1.27502(9) 0.0419(6) C3P 1 0.3058(2) 1.06988(15) 1.38855(11) 0.0490(6) C4P 1 0.2809(2) 0.9418(2) 1.47570(8) 0.0561(7) C5P 1 0.2520(3) 0.8012(2) 1.44930(9) 0.0610(7) C6P 1 0.2481(2) 0.78853(15) 1.33577(11) 0.0526(6) H2P 1 0.3212(3) 1.1564(2) 1.20754(12) 0.063 H3P 1 0.3282(4) 1.1788(2) 1.4090(2) 0.063 H4P 1 0.2839(3) 0.9516(3) 1.56359(9) 0.063 H5P 1 0.2327(4) 0.7020(2) 1.51678(12) 0.063 H6P 1 0.2257(4) 0.6796(2) 1.3153(2) 0.063 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 O1 0.0747(11) -0.0237(7) -0.0103(7) 0.0318(8) -0.0091(7) 0.0440(9) C2 0.0549(13) -0.0176(10) -0.0049(9) 0.0363(12) -0.0094(9) 0.0358(12) C2A 0.071(2) -0.0186(12) -0.0072(11) 0.0578(15) -0.0252(12) 0.0497(14) C2B 0.0556(15) -0.0120(12) -0.0080(11) 0.055(2) -0.0148(12) 0.055(2) O3 0.0563(10) -0.0222(7) 0.0015(7) 0.0456(9) -0.0134(7) 0.0365(8) C4 0.0519(13) -0.0153(10) -0.0026(10) 0.0302(11) -0.0097(9) 0.0414(12) O4 0.0803(12) -0.0465(10) 0.0118(8) 0.0594(11) -0.0168(8) 0.0579(11) C5 0.0452(12) -0.0147(9) -0.0054(9) 0.0287(11) -0.0055(9) 0.0359(11) C6 0.0535(13) -0.0151(10) -0.0069(9) 0.0338(12) -0.0077(10) 0.0393(13) O6 0.1102(14) -0.0391(9) -0.0128(8) 0.0409(9) 0.0033(8) 0.0425(10) C7 0.0495(13) -0.0181(10) -0.0044(9) 0.0353(12) -0.0038(9) 0.0337(11) C8 0.0448(12) -0.0161(9) -0.0023(9) 0.0325(11) -0.0103(9) 0.0369(12) C8M 0.074(2) -0.0180(11) -0.0045(11) 0.0340(12) -0.0080(10) 0.0416(13) N9 0.0478(11) -0.0166(8) -0.0030(8) 0.0330(10) -0.0115(8) 0.0391(10) N10 0.0520(11) -0.0166(8) -0.0026(8) 0.0317(10) -0.0115(8) 0.0376(10) C1P 0.0349(11) -0.0117(9) -0.0025(8) 0.0376(12) -0.0119(9) 0.0367(12) C2P 0.0494(13) -0.0088(10) -0.0046(10) 0.0338(12) -0.0145(10) 0.0437(13) C3P 0.0578(14) -0.0099(11) -0.0112(11) 0.0447(13) -0.0186(11) 0.0473(14) C4P 0.064(2) -0.0192(13) -0.0034(11) 0.068(2) -0.0214(12) 0.0407(13) C5P 0.079(2) -0.0386(14) 0.0020(12) 0.070(2) -0.0068(12) 0.0433(14) C6P 0.069(2) -0.0339(12) -0.0003(11) 0.0545(15) -0.0093(11) 0.0445(14) _cod_database_code 2003257