#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/05/2010561.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_2010561 loop_ _publ_author_name 'Baouid, A.' 'Hasnaoui, H.' 'Benharref, A.' 'Aatif, A.' 'Essaber, M.' 'Lavergne, J. P.' 'Pierrot, M.' _publ_section_title 3,3'-Dimesityl-7-methyl-9a-phenyl-4,4',5,5',6,8,9,9a-octahydro-7H-1,2,4-oxadiazolo[4,5-d][1,4]diazepine-8-spiro-5'-isoxazole _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first e25 _journal_page_last e26 _journal_volume 56 _journal_year 2000 _chemical_formula_sum 'C33 H38 N4 O2' _chemical_formula_weight 522.69 _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' _atom_type_scat_source 'Waasmaier & Kirfel (1995)' _cell_angle_alpha 90.000(10) _cell_angle_beta 101.078(3) _cell_angle_gamma 90.000(10) _cell_formula_units_Z 4 _cell_length_a 22.9235(7) _cell_length_b 9.9309(5) _cell_length_c 12.8363(7) _cell_measurement_reflns_used 11268 _cell_measurement_temperature 298 _cell_measurement_theta_max 25.2 _cell_measurement_theta_min 1 _cell_volume 2867.7(2) _computing_data_collection 'KappaCCD Reference Manual (Nonius, 1998)' _computing_data_reduction 'maXus (Mackay et al., 1998)' _computing_molecular_graphics maXus _computing_publication_material maXus _computing_structure_refinement maXus _computing_structure_solution maXus _diffrn_measurement_device KappaCCD _diffrn_measurement_method \f _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .071 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 4771 _diffrn_reflns_theta_max 24.19 _exptl_absorpt_coefficient_mu .077 _exptl_absorpt_correction_type none _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.20 _exptl_crystal_density_meas none _exptl_crystal_description 'thin plate' _exptl_crystal_size_max .30 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .10 _refine_diff_density_max .21 _refine_diff_density_min -.33 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.575 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 352 _refine_ls_number_reflns 3640 _refine_ls_R_factor_gt .073 _refine_ls_shift/esd_mean .00065 _refine_ls_shift/su_max .0037 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'w = 1/[\s^2^(F~o~^2^) + 0.03F~o~^2^]' _refine_ls_wR_factor_ref .083 _reflns_number_gt 3640 _reflns_number_total 4280 _reflns_threshold_expression refl_observed_if_I_>_1.75\s(I) _[local]_cod_data_source_file qa0187.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _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: '_atom_site_thermal_displace_type' tag value 'Uij' was replaced with 'Uani' value 39 times. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 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 ; _cod_original_cell_volume 2867.8(4) _cod_database_code 2010561 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z -X,+Y+1/2,-Z+1/2 +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 O1 .0658(6) .0498(6) .0274(4) -.0023(4) .0106(3) -.0036(4) O11 .0679(6) .0630(7) .0495(6) .0118(5) .0113(4) -.0148(5) N4 .0586(6) .0390(7) .0279(5) -.0048(5) .0122(4) -.0019(4) C91 .0584(7) .0419(8) .0277(6) -.0044(6) .0107(5) -.0020(5) N21 .0576(7) .0593(9) .0557(8) .0100(5) .0155(5) -.0041(6) C5 .0790(9) .0466(8) .0263(6) -.0023(7) .0133(6) -.0025(6) N2 .0631(7) .0467(7) .0376(7) -.0034(5) .0119(5) -.0064(5) N7 .0544(7) .0640(9) .0512(7) -.0067(5) .0187(5) .0065(6) C11 .0620(8) .0425(9) .0489(8) .0006(6) .0058(6) -.0059(6) C43 .0484(7) .0560(10) .0571(9) .0074(6) .0132(6) -.0033(7) C10 .0582(8) .0380(8) .0401(7) -.0016(6) .0116(5) -.0066(6) C31 .0514(7) .0463(8) .0476(8) -.0008(6) .0170(5) -.0006(7) C20 .0540(8) .0514(9) .0371(7) -.0059(6) .0088(5) .0058(6) C8 .0553(7) .0460(8) .0407(7) .0019(6) .0152(5) -.0037(6) C9 .0572(8) .0435(8) .0396(7) -.0051(6) .0098(5) .0005(6) C47 .0537(8) .0590(10) .0660(10) .0070(7) .0163(7) .0097(8) C3 .0448(7) .0436(8) .0360(7) -.0032(5) .0072(5) -.0063(6) C41 .0513(7) .0500(9) .0437(7) .0022(6) .0107(5) -.0048(6) C15 .0677(9) .0432(9) .0517(8) -.0082(6) .0130(6) -.0111(7) C42 .0448(7) .0533(9) .0516(8) .0072(6) .0148(5) .0010(7) C13 .0950(10) .0346(8) .0600(10) .0046(8) .0206(8) -.0019(7) C45 .0700(10) .0740(10) .0560(10) .0263(9) .0000(7) .0007(9) C12 .0840(10) .0430(9) .0541(9) .0092(7) .0037(7) -.0023(7) C16 .0616(9) .0620(10) .0760(10) -.0038(7) -.0121(7) .0109(9) C21 .0637(9) .0710(10) .0850(10) -.0165(8) .0161(8) -.0170(10) C44 .0584(9) .0630(10) .0640(10) .0117(7) .0022(7) -.0105(8) C48 .0681(9) .0620(10) .0660(10) -.0124(7) .0106(7) -.0077(8) C14 .0840(10) .0388(9) .0750(10) -.0151(7) .0241(8) -.0113(8) C50 .0840(10) .0700(10) .0880(10) -.0111(9) .0215(9) .0190(10) C6 .0840(10) .0770(10) .0399(8) .0026(8) .0301(7) .0026(7) C46 .0710(10) .0710(10) .0630(10) .0209(8) .0160(8) .0204(9) C18 .0710(10) .0680(10) .0810(10) -.0219(8) .0037(8) -.0056(9) C25 .0610(10) .0760(10) .0780(10) -.0078(8) .0212(8) -.0094(9) C23 .0590(10) .095(2) .107(2) -.0220(10) .0020(9) .0170(10) C17 .127(2) .0460(10) .0770(10) -.0002(9) .0220(10) .0041(9) C19 .0650(10) .100(2) .0970(10) -.0102(9) .0283(9) .0290(10) C24 .0570(10) .101(2) .1010(10) -.0030(10) .0251(8) .0070(10) C22 .0830(10) .087(2) .130(2) -.0350(10) .0000(10) -.0240(10) C49 .121(2) .102(2) .0710(10) .0340(10) -.0110(10) .0020(10) 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_occupancy O1 -.17658(4) -.18110(10) -.81897(6) .0481(5) Uani 1.00 O11 -.31419(4) .07160(10) -.72296(8) .0609(5) Uani 1.00 N4 -.16773(4) -.20420(10) -.64187(8) .0421(5) Uani 1.00 C91 -.16641(5) -.10160(10) -.72308(9) .0431(6) Uani 1.00 N21 -.36212(5) .09350(10) -.80870(10) .0580(6) Uani 1.00 C5 -.18798(6) -.1722(2) -.54480(10) .0511(7) Uani 1.00 N2 -.17360(5) -.32400(10) -.79071(9) .0496(6) Uani 1.00 N7 -.28569(5) -.15570(10) -.67058(9) .0567(6) Uani 1.00 C11 -.11917(6) -.4771(2) -.54710(10) .0522(7) Uani 1.00 C43 -.43471(6) -.0847(2) -1.03090(10) .0543(7) Uani 1.00 C10 -.16936(5) -.45240(10) -.62760(10) .0459(6) Uani 1.00 C31 -.35796(5) .0115(2) -.88370(10) .0486(7) Uani 1.00 C20 -.10415(5) -.0395(2) -.70550(10) .0480(7) Uani 1.00 C8 -.27863(6) -.0489(2) -.74370(10) .0475(7) Uani 1.00 C9 -.21548(6) .0032(2) -.72800(10) .0473(6) Uani 1.00 C47 -.39271(6) .1363(2) -1.05270(10) .0598(8) Uani 1.00 C3 -.17134(5) -.32690(10) -.69000(10) .0421(6) Uani 1.00 C41 -.30602(5) -.0815(2) -.85910(10) .0488(7) Uani 1.00 C15 -.21680(6) -.5434(2) -.64490(10) .0549(7) Uani 1.00 C42 -.39734(5) .0217(2) -.98970(10) .0501(7) Uani 1.00 C13 -.16629(8) -.6781(2) -.49560(10) .0637(9) Uani 1.00 C45 -.45790(7) .0273(2) -1.20100(10) .0680(10) Uani 1.00 C12 -.11922(7) -.5886(2) -.48280(10) .0619(8) Uani 1.00 C16 -.06649(7) -.3850(2) -.53000(10) .0692(9) Uani 1.00 C21 -.08979(7) .0783(2) -.6507(2) .0740(10) Uani 1.00 C44 -.46501(6) -.0779(2) -1.13500(10) .0632(8) Uani 1.00 C48 -.44429(7) -.2029(2) -.96360(10) .0662(9) Uani 1.00 C14 -.21390(7) -.6554(2) -.57770(10) .0663(9) Uani 1.00 C50 -.35824(8) .2580(2) -1.0101(2) .0810(10) Uani 1.00 C6 -.25360(7) -.1340(2) -.56180(10) .0664(9) Uani 1.00 C46 -.42256(7) .1352(2) -1.15800(10) .0690(10) Uani 1.00 C18 -.27030(7) -.5229(2) -.7302(2) .0750(10) Uani 1.00 C25 -.05881(7) -.1095(2) -.7393(2) .0722(9) Uani 1.00 C23 .01282(8) .0525(3) -.6606(2) .0890(10) Uani 1.00 C17 -.16610(10) -.7961(2) -.4220(2) .0840(10) Uani 1.00 C19 -.34725(8) -.1940(3) -.6727(2) .0870(10) Uani 1.00 C24 -.00100(7) -.0632(3) -.7169(2) .0870(10) Uani 1.00 C22 -.03150(10) .1238(3) -.6279(2) .1030(10) Uani 1.00 C49 -.48820(10) .0276(3) -1.3161(2) .1010(10) Uani 1.00 H5A -.16408 -.09882 -.51193 .05000 Uiso 1.00 H5B -.18098 -.25022 -.49993 .05000 Uiso 1.00 H41A -.27722 -.06507 -.90296 .05000 Uiso 1.00 H41B -.31772 -.17437 -.86466 .05000 Uiso 1.00 H12 -.08502 -.60353 -.42794 .05000 Uiso 1.00 H16A -.07359 -.31296 -.58083 .05000 Uiso .50 H16B -.03179 -.43436 -.53923 .05000 Uiso .50 H16C -.06029 -.34836 -.45953 .05000 Uiso .50 H21 -.12059 .12918 -.62781 .05000 Uiso 1.00 H44 -.49151 -.15057 -1.16080 .05000 Uiso 1.00 H48A -.42059 -.19367 -.89363 .05000 Uiso .50 H48B -.43329 -.28387 -.99583 .05000 Uiso .50 H48C -.48559 -.20717 -.95903 .05000 Uiso .50 H14 -.24670 -.71728 -.59027 .05000 Uiso 1.00 H50A -.34044 .24308 -.93704 .05000 Uiso .50 H50B -.38434 .33438 -1.01554 .05000 Uiso .50 H50C -.32764 .27468 -1.05014 .05000 Uiso .50 H6A -.25550 -.04051 -.54389 .05000 Uiso 1.00 H6B -.27130 -.18711 -.51369 .05000 Uiso 1.00 H46 -.41806 .21184 -1.20143 .05000 Uiso 1.00 H18A -.26590 -.44263 -.76960 .05000 Uiso 1.00 H18B -.30470 -.51483 -.69830 .05000 Uiso 1.00 H18C -.27490 -.59903 -.77710 .05000 Uiso 1.00 H25 -.06831 -.19088 -.77930 .05000 Uiso 1.00 H23 .05302 .08476 -.64323 .05000 Uiso 1.00 H17A -.12980 -.79617 -.37020 .05000 Uiso .50 H17B -.16900 -.87807 -.46220 .05000 Uiso .50 H17C -.19930 -.78937 -.38670 .05000 Uiso .50 H19A -.36725 -.20757 -.74476 .05000 Uiso 1.00 H19B -.36675 -.12337 -.64126 .05000 Uiso 1.00 H19C -.34845 -.27567 -.63316 .05000 Uiso 1.00 H24 .02940 -.11367 -.74151 .05000 Uiso 1.00 H22 -.02282 .20644 -.58914 .05000 Uiso 1.00 H49A -.51079 -.05370 -1.33272 .05000 Uiso 1.00 H49B -.45879 .03380 -1.35992 .05000 Uiso 1.00 H49C -.51429 .10390 -1.32912 .05000 Uiso 1.00 H50D -.37654 .30558 -.95574 .05000 Uiso .50 H48D -.47759 -.25787 -1.00093 .05000 Uiso .50 H50E -.31984 .20888 -.98694 .05000 Uiso .50 H16D -.07449 -.28716 -.51103 .05000 Uiso .50 H17D -.13170 -.85947 -.42560 .05000 Uiso .50 H48E -.4496 -.145 -.899 .050 Uiso .50 H16E -.03229 -.41166 -.46923 .05000 Uiso .50 H17E -.15670 -.75227 -.35510 .05000 Uiso .50 H50F -.35324 .33658 -1.05264 .05000 Uiso .50 H17F -.20570 -.84187 -.43710 .05000 Uiso .50 H48F -.40669 -.25477 -.96083 .05000 Uiso .50 H16F -.05109 -.37946 -.59763 .05000 Uiso .50 H9A -.20728 .05562 -.65929 .05000 Uiso 1.00 H9B -.21308 .06572 -.78909 .05000 Uiso 1.00 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C91 . . 1.443(2) yes O1 N2 . . 1.463(2) yes O11 N21 . . 1.414(2) yes O11 C8 . . 1.501(2) yes N4 C91 . . 1.461(2) yes N4 C5 . . 1.446(2) yes N4 C3 . . 1.362(2) yes C91 C20 . . 1.531(2) ? C91 C9 . . 1.525(2) yes N21 C31 . . 1.279(2) yes C5 C6 . . 1.526(3) yes N2 C3 . . 1.284(2) yes N7 C8 . . 1.446(2) yes N7 C6 . . 1.464(2) yes N7 C19 . . 1.457(3) no C11 C10 . . 1.412(2) no C11 C12 . . 1.382(3) no C11 C16 . . 1.497(3) no C43 C42 . . 1.398(3) no C43 C44 . . 1.385(3) no C43 C48 . . 1.498(3) no C10 C3 . . 1.477(2) no C10 C15 . . 1.399(2) no C31 C41 . . 1.492(2) yes C31 C42 . . 1.485(2) no C20 C21 . . 1.372(3) no C20 C25 . . 1.387(3) no C8 C9 . . 1.514(2) yes C8 C41 . . 1.527(2) yes C47 C42 . . 1.412(3) no C47 C50 . . 1.489(3) no C47 C46 . . 1.393(3) no C15 C14 . . 1.402(3) no C15 C18 . . 1.493(3) no C13 C12 . . 1.383(3) no C13 C14 . . 1.382(3) no C13 C17 . . 1.505(3) no C45 C44 . . 1.374(3) no C45 C46 . . 1.392(3) no C45 C49 . . 1.507(3) no C21 C22 . . 1.387(3) no C25 C24 . . 1.380(3) no C23 C24 . . 1.361(4) no C23 C22 . . 1.370(4) no 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 C91 O1 N2 109.10(10) yes N21 O11 C8 110.6(2) yes C91 N4 C5 121.1(2) yes C91 N4 C3 107.90(10) yes C5 N4 C3 125.8(2) yes O1 C91 N4 101.8(2) yes O1 C91 C20 109.90(10) no O1 C91 C9 110.00(10) yes N4 C91 C20 108.80(10) yes N4 C91 C9 112.90(10) yes C20 C91 C9 113.0(2) ? O11 N21 C31 109.2(2) yes N4 C5 C6 113.7(2) yes O1 N2 C3 105.2(2) yes C8 N7 C6 114.4(2) yes C8 N7 C19 114.1(2) ? C6 N7 C19 111.3(2) yes C10 C11 C12 118.8(2) ? C10 C11 C16 121.5(2) ? C12 C11 C16 119.7(2) ? C42 C43 C44 119.0(2) ? C42 C43 C48 121.4(2) ? C44 C43 C48 119.5(2) ? C11 C10 C3 118.6(2) ? C11 C10 C15 120.2(2) ? C3 C10 C15 121.1(2) yes N21 C31 C41 114.0(2) yes N21 C31 C42 121.8(2) ? C41 C31 C42 123.8(2) ? C91 C20 C21 123.0(2) ? C91 C20 C25 119.0(2) ? C21 C20 C25 117.8(2) ? O11 C8 N7 109.7(2) yes O11 C8 C9 104.0(2) yes O11 C8 C41 101.8(2) yes N7 C8 C9 112.8(2) yes N7 C8 C41 113.5(2) yes C9 C8 C41 114.0(2) yes C91 C9 C8 116.8(2) yes C42 C47 C50 122.5(2) ? C42 C47 C46 118.2(2) ? C50 C47 C46 119.3(2) ? N4 C3 N2 115.1(2) yes N4 C3 C10 121.1(2) ? N2 C3 C10 123.8(2) ? C31 C41 C8 103.7(2) yes C10 C15 C14 118.1(2) ? C10 C15 C18 122.2(2) ? C14 C15 C18 119.7(2) ? C43 C42 C31 121.0(2) ? C43 C42 C47 120.0(2) ? C31 C42 C47 118.7(2) ? C12 C13 C14 118.0(2) ? C12 C13 C17 121.2(2) ? C14 C13 C17 120.8(2) ? C44 C45 C46 118.0(2) ? C44 C45 C49 121.3(2) ? C46 C45 C49 120.7(2) ? C11 C12 C13 122.3(2) ? C20 C21 C22 120.8(2) ? C43 C44 C45 122.4(2) ? C15 C14 C13 122.4(2) ? C5 C6 N7 113.6(2) yes C47 C46 C45 122.0(2) ? C20 C25 C24 121.0(2) ? C24 C23 C22 119.2(2) ? C25 C24 C23 120.5(2) ? C21 C22 C23 120.5(3) ? _cod_database_fobs_code 2010561 _journal_paper_doi 10.1107/S0108270199016091