#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2004276.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_2004276 loop_ _publ_author_name 'Bolte, M.' _publ_section_title ; Structural Investigation of Dihydrooxazinones ; _journal_issue 12 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 2587 _journal_page_last 2593 _journal_volume 51 _journal_year 1995 _chemical_formula_sum 'C16 H21 N O4' _chemical_formula_weight 291.3 _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90 _cell_angle_beta 98.920(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.0390(10) _cell_length_b 11.0970(10) _cell_length_c 8.4980(10) _cell_measurement_reflns_used 45 _cell_measurement_temperature 293 _cell_measurement_theta_max 12.5 _cell_measurement_theta_min 10 _cell_volume 748.93(15) _computing_molecular_graphics 'SHELXTL (Sheldrick, 1983)' _computing_structure_refinement 'modified version of SHELX76 (Sheldrick, 1976)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_measurement_device 'Stoe-Siemens four-circle' _diffrn_measurement_method '\w/2\q profile-fitting (Clegg, 1981)' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1428 _diffrn_reflns_theta_max 25 _diffrn_standards_decay_% negligible _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.06 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.292 _exptl_crystal_description block _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _refine_diff_density_max 0.14 _refine_diff_density_min -0.13 _refine_ls_extinction_coef '\c = 0.009(1)' _refine_ls_extinction_method 'F^*^ = F[1+0.002\cF^2^/sin(2\q)]^-1/4^' _refine_ls_goodness_of_fit_obs 1.37 _refine_ls_hydrogen_treatment 'H atoms see text' _refine_ls_number_parameters 205 _refine_ls_number_reflns 1170 _refine_ls_R_factor_obs 0.027 _refine_ls_shift/esd_max 0.002 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme ' 1/[\s^2^(F)+0.003F^2^]' _refine_ls_wR_factor_obs 0.033 _reflns_number_observed 1170 _reflns_number_total 1252 _reflns_observed_criterion F>3\s(F) _[local]_cod_data_source_file ka1140.cif _[local]_cod_data_source_block 5 _[local]_cod_cif_authors_sg_Hall 'P 2y1' _cod_original_cell_volume 748.9(4) _cod_database_code 2004276 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv O(1) .66160(10) .4688 .58090(10) .0460(10) C(2) .7593(2) .5078(3) .4769(2) .0440(10) C(3) .7269(2) .4618(3) .3054(2) .0400(10) N(4) .5768(2) .3872(3) .2632(2) .0380(10) C(5) .5039(2) .3472(3) .3723(2) .0370(10) C(6) .5448(2) .3713(4) .5482(2) .0390(10) O(21) .8668(2) .5804(3) .5214(2) .0590(10) C(31) .7103(3) .5693(4) .1949(3) .054(2) O(51) .3724(2) .2712(3) .3429(2) .0470(10) C(52) .3241(3) .2336(4) .1800(2) .055(2) C(61) .3896(2) .4009(4) .6232(2) .0440(10) C(62) .3005(3) .5114(4) .5473(3) .062(2) C(63) .4353(3) .4161(5) .8042(3) .065(2) C(1') .8833(2) .3843(4) .2854(2) .0400(10) O(1') .8967(2) .2976(3) .4098(2) .0520(10) C(2') .8749(2) .3291(4) .1221(2) .037(2) C(3') .9402(3) .3884(5) .0019(3) .045(2) C(4') .9352(3) .3379(5) -.1475(3) .058(2) C(5') .8642(3) .2271(5) -.1795(3) .059(2) C(6') .7947(3) .1666(5) -.0631(3) .053(2) C(7') .8021(3) .2184(5) .0873(3) .045(2) H(6) .5937 .2979 .5941 .070 H(31a) .8122 .6159 .2085 .070 H(31b) .6179 .6198 .2126 .070 H(31c) .6892 .5376 .0886 .070 H(52a) .2377 .1735 .1761 .070 H(52b) .4186 .2007 .1380 .070 H(52c) .2811 .3020 .1175 .070 H(61) .3136 .3340 .6041 .070 H(62a) .1988 .5272 .5899 .070 H(62b) .2741 .4998 .4342 .070 H(62c) .3758 .5786 .5691 .070 H(63a) .4947 .3459 .8489 .070 H(63b) .3356 .4271 .8518 .070 H(63c) .5065 .4855 .8248 .070 H(1') .9828 .4332 .2937 .070 H(1'O) .9690(17) .243(2) .406(3) .070 H(3') .9905 .4663 .0228 .070 H(4') .9816 .3809 -.2286 .070 H(5') .8622 .1914 -.2827 .070 H(6') .7423 .0894 -.0855 .070 H(7') .7552 .1757 .1683 .070 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C(3) C(2) O(1) 119.3(2) yes N(4) C(3) C(2) 115.8(2) yes C(5) N(4) C(3) 118.8(2) yes C(5) C(6) O(1) 111.3(2) yes C(6) O(1) C(2) 123.3(2) yes O(21) C(2) O(1) 118.4(2) yes O(21) C(2) C(3) 122.3(2) yes O(51) C(5) N(4) 121.9(2) yes O(51) C(5) C(6) 109.9(2) yes C(52) O(51) C(5) 116.6(2) yes C(31) C(3) N(4) 107.7(2) no C(1') C(3) N(4) 108.1(3) no C(61) C(6) C(5) 112.80(10) no C(62) C(61) C(6) 111.2(2) no C(63) C(61) C(62) 111.3(3) no C(2') C(1') C(3) 113.8(2) no C(3') C(2') C(1') 121.1(3) no C(7') C(2') C(3') 117.6(3) no C(5') C(4') C(3') 119.9(3) no C(7') C(6') C(5') 119.4(5) no C(31) C(3) C(2) 108.3(3) no C(1') C(3) C(2) 105.5(2) no C(1') C(3) C(31) 111.3(2) no C(6) C(5) N(4) 128.2(2) no C(61) C(6) O(1) 108.1(3) no C(63) C(61) C(6) 111.0(2) no O(1') C(1') C(3) 105.2(2) no C(2') C(1') O(1') 113.4(3) no C(7') C(2') C(1') 121.2(3) no C(4') C(3') C(2') 121.6(4) no C(6') C(5') C(4') 119.9(3) no C(6') C(7') C(2') 121.5(3) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O(1) C(2) 1.342(3) yes C(2) C(3) 1.528(3) yes C(3) N(4) 1.461(3) yes N(4) C(5) 1.253(3) yes C(5) C(6) 1.503(3) yes O(1) C(6) 1.432(3) yes C(2) O(21) 1.199(4) yes C(5) O(51) 1.346(3) yes O(51) C(52) 1.440(3) yes C(3) C(1') 1.555(4) no C(6) C(61) 1.523(3) no C(61) C(62) 1.513(6) no C(1') O(1') 1.421(4) no C(2') C(3') 1.385(4) no C(3') C(4') 1.383(4) no C(5') C(6') 1.383(5) no C(3) C(31) 1.511(5) no C(61) C(63) 1.534(3) no C(1') C(2') 1.509(4) no C(2') C(7') 1.372(6) no C(4') C(5') 1.365(7) no C(6') C(7') 1.395(5) no 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 _geom_torsion_publ_flag O(1) C(2) C(3) N(4) 6.5(3) yes C(2) C(3) N(4) C(5) -13.2(3) yes C(3) N(4) C(5) C(6) 3.7(3) yes N(4) C(5) C(6) O(1) 12.1(3) yes C(5) C(6) O(1) C(2) -18.9(3) yes C(6) O(1) C(2) C(3) 10.5(3) yes N(4) C(5) O(51) C(52) 2.7(3) yes