#------------------------------------------------------------------------------ #$Date: 2025-08-18 23:52:38 +0100 (Mon, 18 Aug 2025) $ #$Revision: 301791 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/63/2006342.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_2006342 loop_ _publ_author_name 'Prakash, Gautam' 'Fettinger, James C.' 'Falvey, Daniel E.' _publ_section_title (6Z,8Z)-2,4,6-Trimethyl-8-phenyl-7-oxa-2,4-diazabicyclo[4.2.0]octane-3,5-dione _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 979 _journal_page_last 981 _journal_paper_doi 10.1107/S0108270197002850 _journal_volume 53 _journal_year 1997 _chemical_formula_sum 'C14 H16 N2 O3' _chemical_formula_weight 260.29 _chemical_name_systematic (6Z,8Z)-2,4,6-Trimethyl-8-phenyl-7-oxa-2,4-diazabicyclo[4.2.0]octane-3,5-dione _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 93.541(7) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.9803(8) _cell_length_b 16.3083(10) _cell_length_c 9.2752(7) _cell_measurement_reflns_used 25 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 18.9 _cell_measurement_theta_min 17.6 _cell_volume 1355.79(18) _computing_cell_refinement 'CAD-4 EXPRESS' _computing_data_collection 'CAD-4 EXPRESS (Enraf-Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms, 1993), SHELXTL-Plus (Sheldrick, 1991)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976) in SHELXTL-Plus' _computing_publication_material SHELXTL-Plus _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 153(2) _diffrn_measurement_device 'Enraf CAD4' _diffrn_measurement_method '\w/2\q scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0138 _diffrn_reflns_av_sigmaI/netI 0.0176 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 2540 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_min 2.27 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 6 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_T_max 0.9788 _exptl_absorpt_correction_T_min 0.9737 _exptl_absorpt_correction_type integration _exptl_crystal_colour 'clear, colorless' _exptl_crystal_density_diffrn 1.275 _exptl_crystal_description block _exptl_crystal_F_000 552 _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.250 _refine_diff_density_max 0.179 _refine_diff_density_min -0.149 _refine_ls_extinction_coef 0.0044(12) _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_all 1.038 _refine_ls_goodness_of_fit_obs 1.066 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 237 _refine_ls_number_reflns 2381 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.038 _refine_ls_restrained_S_obs 1.066 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_obs .0422 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.5644P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1083 _refine_ls_wR_factor_obs .0967 _reflns_number_observed 1856 _reflns_number_total 2381 _reflns_observed_criterion >2sigma(I) _cod_data_source_file sx1020.cif _cod_data_source_block f _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. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 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. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.5644P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.5644P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 1355.8(2) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2006342 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 C1 .0548(12) .0430(11) .0459(11) .0024(9) .0154(9) -.0028(9) C2 .096(2) .0419(12) .0562(13) .0122(12) .0317(13) .0060(10) C3 .079(2) .081(2) .0600(14) .042(2) .0154(13) .0198(13) C4 .0536(15) .095(2) .093(2) .0168(14) .0003(13) .033(2) C5 .0424(12) .072(2) .079(2) .0032(11) .0018(11) .0251(13) C6 .0411(10) .0455(10) .0364(9) .0028(8) .0073(8) .0025(8) O7 .0403(7) .0556(8) .0365(7) .0082(6) -.0002(5) -.0109(6) C7 .0385(9) .0445(10) .0337(9) -.0016(8) .0013(8) .0032(8) N8 .0990(14) .0388(9) .0333(8) .0058(9) -.0133(9) -.0030(7) C8 .0596(12) .0380(10) .0294(9) .0056(9) .0045(8) .0031(8) O9 .1085(13) .0379(8) .0681(10) .0041(8) -.0191(9) -.0048(7) N9 .0543(10) .0429(9) .0390(9) .0097(7) -.0019(7) .0039(7) C9 .0681(13) .0381(11) .0415(11) .0094(10) .0017(9) -.0050(8) C10 .0348(9) .0538(12) .0419(10) .0042(9) .0027(8) .0019(9) O10 .0555(9) .0756(10) .0576(9) -.0043(8) -.0212(7) .0075(8) C11 .0400(10) .0428(10) .0408(10) .0051(8) .0074(8) -.0032(8) C12 .217(5) .050(2) .065(2) -.010(2) -.077(3) -.0010(14) C13 .099(2) .0536(15) .065(2) .0175(15) -.015(2) .0170(13) C14 .0503(13) .0501(13) .085(2) .0054(11) .0228(13) .0069(13) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol C1 .1783(2) 1.34400(12) -.4947(2) .0474(5) Uani d . 1 . C H1 .287(2) 1.3496(12) -.481(2) .053(6) Uiso d . 1 . H C2 .0912(3) 1.40493(14) -.5622(2) .0635(7) Uani d . 1 . C H2 .143(2) 1.4532(15) -.589(2) .066(7) Uiso d . 1 . H C3 -.0601(3) 1.3950(2) -.5835(3) .0729(8) Uani d . 1 . C H3 -.125(3) 1.4377(16) -.627(3) .090(8) Uiso d . 1 . H C4 -.1267(3) 1.3252(2) -.5396(3) .0807(8) Uani d . 1 . C H4 -.241(3) 1.3200(18) -.560(3) .111(10) Uiso d . 1 . H C5 -.0417(2) 1.2646(2) -.4713(3) .0646(6) Uani d . 1 . C H5 -.088(3) 1.2128(16) -.445(3) .079(8) Uiso d . 1 . H C6 .1111(2) 1.27336(11) -.4484(2) .0408(4) Uani d . 1 . C O7 .32835(13) 1.23013(8) -.28877(13) .0443(4) Uani d . 1 . O C7 .2003(2) 1.20440(11) -.3827(2) .0390(4) Uani d . 1 . C H7 .1353(19) 1.1661(10) -.3326(19) .037(5) Uiso d . 1 . H N8 .2729(2) 1.07354(10) -.5131(2) .0578(5) Uani d . 1 . N C8 .3059(2) 1.15748(11) -.4772(2) .0423(5) Uani d . 1 . C H8 .322(2) 1.1860(11) -.565(2) .047(5) Uiso d . 1 . H O9 .2586(2) .94141(9) -.4467(2) .0725(5) Uani d . 1 . O N9 .3980(2) 1.02611(9) -.2992(2) .0456(4) Uani d . 1 . N C9 .3047(2) 1.01047(12) -.4239(2) .0493(5) Uani d . 1 . C C10 .4568(2) 1.10057(12) -.2575(2) .0435(5) Uani d . 1 . C O10 .5311(2) 1.10867(10) -.1441(2) .0639(4) Uani d . 1 . O C11 .4263(2) 1.17306(11) -.3575(2) .0410(4) Uani d . 1 . C C12 .1605(7) 1.0605(2) -.6325(4) .114(2) Uani d . 1 . C H12A .153(4) 1.009(3) -.648(4) .144(14) Uiso d . 1 . H H12B .186(3) 1.096(2) -.705(4) .112(11) Uiso d . 1 . H H12C .071(6) 1.075(4) -.613(7) .23(3) Uiso d . 1 . H C13 .4302(4) .9548(2) -.2042(3) .0735(8) Uani d . 1 . C H13A .526(5) .968(3) -.151(5) .168(17) Uiso d . 1 . H H13B .466(4) .914(2) -.254(4) .125(13) Uiso d . 1 . H H13C .352(6) .943(3) -.152(6) .20(2) Uiso d . 1 . H C14 .5689(3) 1.2140(2) -.3946(3) .0612(6) Uani d . 1 . C H14A .548(2) 1.2604(15) -.456(3) .067(7) Uiso d . 1 . H H14B .627(3) 1.1748(14) -.447(3) .069(7) Uiso d . 1 . H H14C .634(3) 1.2302(17) -.306(3) .099(10) Uiso d . 1 . H loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 _geom_angle_publ_flag C6 C1 C2 119.5(2) no C6 C1 H1 119.2(12) no C2 C1 H1 121.2(12) no C3 C2 C1 120.3(2) no C3 C2 H2 123.5(14) no C1 C2 H2 116.1(14) no C4 C3 C2 120.5(2) no C4 C3 H3 117.3(16) no C2 C3 H3 122.3(16) no C3 C4 C5 119.7(2) no C3 C4 H4 117.5(17) no C5 C4 H4 122.7(17) no C4 C5 C6 120.8(2) no C4 C5 H5 120.0(14) no C6 C5 H5 119.1(14) no C1 C6 C5 119.1(2) no C1 C6 C7 121.5(2) yes C5 C6 C7 119.2(2) yes C11 O7 C7 91.69(12) yes O7 C7 C6 114.26(15) yes O7 C7 C8 89.57(13) yes C6 C7 C8 118.62(15) yes O7 C7 H7 111.5(10) no C6 C7 H7 110.5(10) no C8 C7 H7 110.9(10) no C9 N8 C8 123.7(2) yes C9 N8 C12 117.8(2) yes C8 N8 C12 115.9(2) yes N8 C8 C11 117.1(2) yes N8 C8 C7 118.8(2) yes C11 C8 C7 86.36(13) yes N8 C8 H8 107.8(11) no C11 C8 H8 113.8(11) no C7 C8 H8 111.9(11) no C10 N9 C9 126.3(2) yes C10 N9 C13 118.1(2) yes C9 N9 C13 115.6(2) yes O9 C9 N8 123.2(2) yes O9 C9 N9 119.3(2) yes N8 C9 N9 117.5(2) yes O10 C10 N9 121.4(2) yes O10 C10 C11 120.8(2) yes N9 C10 C11 117.8(2) yes O7 C11 C14 111.3(2) yes O7 C11 C10 108.76(14) yes C14 C11 C10 111.2(2) yes O7 C11 C8 90.29(13) yes C14 C11 C8 119.0(2) yes C10 C11 C8 114.2(2) yes N8 C12 H12A 108.(3) no N8 C12 H12B 106.(2) no H12A C12 H12B 120.(3) no N8 C12 H12C 114.(4) no H12A C12 H12C 104.(4) no H12B C12 H12C 105.(4) no N9 C13 H13A 105.(2) no N9 C13 H13B 110.(2) no H13A C13 H13B 96.(3) no N9 C13 H13C 111.(3) no H13A C13 H13C 118.(4) no H13B C13 H13C 116.(4) no C11 C14 H14A 110.2(14) no C11 C14 H14B 108.3(13) no H14A C14 H14B 108.6(19) no C11 C14 H14C 112.7(16) no H14A C14 H14C 111.(2) no H14B C14 H14C 106.(2) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 C6 . 1.381(3) no C1 C2 . 1.389(3) no C1 H1 . .98(2) no C2 C3 . 1.371(4) no C2 H2 . .95(2) no C3 C4 . 1.359(4) no C3 H3 . .98(3) no C4 C5 . 1.379(3) no C4 H4 . 1.03(3) no C5 C6 . 1.382(3) no C5 H5 . .98(3) no C6 C7 . 1.489(2) yes O7 C11 . 1.454(2) yes O7 C7 . 1.461(2) yes C7 C8 . 1.534(3) yes C7 H7 . .99(2) no N8 C9 . 1.340(2) yes N8 C8 . 1.435(2) yes N8 C12 . 1.467(4) yes C8 C11 . 1.522(3) yes C8 H8 . .96(2) no O9 C9 . 1.214(2) yes N9 C10 . 1.370(2) yes N9 C9 . 1.409(2) yes N9 C13 . 1.477(3) yes C10 O10 . 1.217(2) yes C10 C11 . 1.518(3) yes C11 C14 . 1.503(3) yes C12 H12A . .85(4) no C12 H12B . .92(3) no C12 H12C . .87(6) no C13 H13A . .99(5) no C13 H13B . .88(4) no C13 H13C . .90(5) no C14 H14A . .96(2) no C14 H14B . .97(2) no C14 H14C . 1.01(3) no loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 101715606