#------------------------------------------------------------------------------ #$Date: 2016-02-19 22:18:51 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176760 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/04/2010421.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_2010421 loop_ _publ_author_name 'Liu, X.-L.' 'Wang, J.-L.' 'Liu, J.-W.' 'Miao, F.-M.' _publ_section_title 6'-Diethylamino-2'-nitrospiro[isobenzofuran-1(3H),9'-[9H]xanthen]-3-one _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 324 _journal_page_last 326 _journal_paper_doi 10.1107/S0108270194005949 _journal_volume 51 _journal_year 1995 _chemical_formula_moiety 'C24 H20 N2 O5' _chemical_formula_sum 'C24 H20 N2 O5' _chemical_formula_weight 416.44 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_type_scat_source IntTabIV _cell_angle_alpha 80.41(2) _cell_angle_beta 79.91(2) _cell_angle_gamma 80.96(2) _cell_formula_units_Z 2 _cell_length_a 8.342(3) _cell_length_b 9.861(2) _cell_length_c 12.735(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 295 _cell_measurement_theta_max 15 _cell_measurement_theta_min 10 _cell_volume 1008.1(5) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.012 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2022 _diffrn_reflns_theta_max 25 _diffrn_standards_decay_% 0.1 _diffrn_standards_interval_time 60 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type none _exptl_crystal_colour 'light yellow' _exptl_crystal_density_diffrn 1.372 _exptl_crystal_description prism _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _refine_diff_density_max 0.141 _refine_diff_density_min -0.120 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 0.721 _refine_ls_hydrogen_treatment refall _refine_ls_number_parameters 280 _refine_ls_number_reflns 1262 _refine_ls_R_factor_obs 0.035 _refine_ls_shift/esd_max 0.01 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme unit _refine_ls_wR_factor_obs 0.034 _reflns_number_observed 1262 _reflns_number_total 1728 _reflns_observed_criterion |F~o~|>3.0\s(|F~o~|) _cod_data_source_file ab1138.cif _cod_data_source_block ab1138_structure_1_of_1 _cod_database_code 2010421 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z O1 .6912(3) .4355(2) .1180(2) O2 .9686(3) .7396(2) .1105(3) O3 1.0858(3) .9290(3) .1116(3) O4 .9293(5) .8466(4) -.2853(4) O5 .8371(6) .6974(4) -.3576(3) N1 .6553(5) .3107(4) .4952(3) N2 .8688(5) .7414(4) -.2812(4) C1 .9622(4) .8780(4) .1164(4) C2 .8009(4) .7010(4) .1196(4) C3 .6807(6) .3298(5) .6017(5) C4 .8439(7) .2726(7) .6266(5) C5 .5944(6) .1815(5) .4879(5) C6 .7247(7) .0684(5) .4574(6) C11 .7541(5) .5274(4) .4101(4) C12 .6955(5) .4011(4) .4035(4) C13 .6772(5) .3772(4) .3037(4) C14 .7136(4) .4712(4) .2146(4) C15 .7696(4) .5973(4) .2162(4) C16 .7844(5) .6190(4) .3190(4) C21 .7351(5) .5168(4) .0224(4) C22 .7178(5) .4660(4) -.0686(4) C23 .7610(6) .5395(4) -.1661(4) C24 .8232(5) .6625(4) -.1748(4) C25 .8397(5) .7120(4) -.0827(4) C26 .7940(4) .6424(4) .0193(4) C31 .7887(4) .9397(4) .1275(4) C32 .7218(5) 1.0746(4) .1372(4) C33 .5532(5) 1.1042(4) .1469(4) C34 0.4564(4) 1.0016(4) .1482(4) C35 0.5250(4) .8678(4) .1372(4) C36 0.6935(4) .8383(3) .1275(4) H11 0.7708 .5500 .4775 H13 0.6434 .2931 .2857 H22 0.6769 .3749 -.0569 H23 .7460 .5084 -.2249 H25 .8894 .8003 -.0864 H32 .7916 1.1425 .1352 H33 .5042 1.1950 .1547 H34 .3473 1.0229 .1505 H35 .4652 .7957 .1402 H301 .5943 .2857 .6678 H302 .6548 .4329 .6103 H501 .4938 .2064 .4350 H502 .5390 .1524 .5517 H401 .8698 .2812 .7162 H402 .8962 .1678 .6345 H403 .9315 .3161 .5783 H601 .6836 -.0175 .4532 H602 .7903 .0837 .3874 H603 .7968 .0264 .5190 H16 .8285 .7103 .3195 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 C14 O1 C21 120.9(8) yes C1 O2 C2 111.0(3) yes C3 N1 C5 116.3(6) yes C3 N1 C12 123.5(7) yes C5 N1 C12 120.0(7) yes O4 N2 O5 125.7(5) yes O4 N2 C24 117.7(9) yes O5 N2 C24 116.5(4) yes O2 C1 O3 121.0(4) yes O2 C1 C31 107.9(3) yes O3 C1 C31 131.1(4) yes O2 C2 C15 109.5(5) yes O2 C2 C26 107.3(4) yes O2 C2 C36 102.4(3) yes C15 C2 C26 110.9(5) yes C15 C2 C36 113.1(5) yes C26 C2 C36 113.1(5) yes N1 C3 C4 113.7(6) yes N1 C5 C6 114.3(5) yes C12 C11 C16 119.2(7) yes N1 C12 C11 120.2(8) yes N1 C12 C13 122.2(8) yes C11 C12 C13 117.5(9) yes C12 C13 C14 120.8(8) yes O1 C14 C13 115.7(7) yes O1 C14 C15 120.1(8) yes C13 C14 C15 124.3(7) yes C2 C15 C14 123.5(7) yes C2 C15 C16 123.1(7) yes C14 C15 C16 113.3(7) yes C11 C16 C15 124.9(7) yes O1 C21 C22 115.6(7) yes O1 C21 C26 121.2(9) yes C22 C21 C26 123.1(4) yes C21 C22 C23 119.1(9) yes C22 C23 C24 120.7(8) yes N2 C24 C23 120.0(9) yes N2 C24 C25 120.5(9) yes C23 C24 C25 119.5(4) yes C24 C25 C26 122.2(9) yes C2 C26 C21 122.4(8) yes C2 C26 C25 122.2(7) yes C21 C26 C25 115.4(9) yes C1 C31 C32 129.1(4) yes C1 C31 C36 108.8(3) yes C32 C31 C36 122.1(4) yes C31 C32 C33 117.0(4) yes C32 C33 C34 121.1(4) yes C33 C34 C35 121.3(4) yes C34 C35 C36 117.5(4) yes C2 C36 C31 109.8(3) yes C2 C36 C35 129.2(3) yes C31 C36 C35 121.0(3) yes H301 C3 H302 100.6(6) no H402 C4 H403 101.1(6) no H501 C5 H502 102.0(5) no H601 C6 H602 100.9(7) no H601 C6 H603 96.4(5) no H602 C6 H603 112.5(6) no 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 C14 . . 1.385(7) yes O1 C21 . . 1.367(8) yes O2 C1 . . 1.372(5) yes O2 C2 . . 1.487(5) yes O3 C1 . . 1.204(4) yes O4 N2 . . 1.213(8) yes O5 N2 . . 1.213(9) yes N1 C3 . . 1.456(7) yes N1 C5 . . 1.465(7) yes N1 C12 . . 1.372(8) yes N2 C24 . . 1.466(9) yes C1 C31 . . 1.471(5) yes C2 C15 . . 1.476(7) yes C2 C26 . . 1.499(8) yes C2 C36 . . 1.510(6) yes C3 C4 . . 1.456(7) yes C5 C6 . . 1.481(8) yes C11 C12 . . 1.427(8) yes C11 C16 . . 1.358(7) yes C12 C13 . . 1.369(9) yes C13 C14 . . 1.363(8) yes C14 C15 . . 1.400(8) yes C15 C16 . . 1.390(7) yes C21 C22 . . 1.370(10) yes C21 C26 . . 1.395(8) yes C22 C23 . . 1.350(9) yes C23 C24 . . 1.374(9) yes C24 C25 . . 1.379(9) yes C25 C26 . . 1.385(8) yes C31 C32 . . 1.376(5) yes C31 C36 . . 1.371(5) yes C32 C33 . . 1.379(6) yes C33 C34 . . 1.386(6) yes C34 C35 . . 1.372(5) yes C35 C36 . . 1.378(5) yes C3 H301 . . 1.087(7) no C3 H302 . . 1.027(6) no C4 H402 . . 1.052(7) no C4 H403 . . 0.976(7) no C5 H501 . . 1.138(6) no C5 H502 . . 0.888(6) no C6 H601 . . 0.975(6) no C6 H602 . . 0.963(7) no C6 H603 . . 1.062(7) no C11 H11 . . 0.960(7) no C13 H13 . . 0.989(6) no C16 H16 . . 1.027(6) no C22 H22 . . 0.989(7) no C23 H23 . . 0.890(8) no C25 H25 . . 1.013(6) no C32 H32 . . 0.949(4) no C33 H33 . . 0.938(4) no C34 H34 . . 0.898(4) no C35 H35 . . 0.922(4) no