#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/33/2003398.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_2003398 loop_ _publ_author_name 'P\`epe, G.' 'Reboul, J.-P.' 'Brun, P.' 'Zylber, J.' _publ_section_title ; 3-Oxo-2-phenyl-3a,4,5,7a-tetrahydro-5,7a-epoxyisoindoline-4-carboxylic Acid in Two Crystalline Phases, Solvated with DMSO and Unsolvated ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 729 _journal_page_last 732 _journal_paper_doi 10.1107/S010827019401142X _journal_volume 51 _journal_year 1995 _chemical_formula_moiety 'C15 H13 N1 O4' _chemical_formula_structural 'C15 H13 N1 O4' _chemical_formula_sum 'C15 H13 N O4' _chemical_formula_weight 271.27 _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-A 2ya' _symmetry_space_group_name_H-M 'A 1 2/a 1' _atom_type_scat_source ' International Tables for X-ray Crystallography (1974, Vol. IV, Table 2.2B)' _cell_angle_alpha 90.00 _cell_angle_beta 81.41(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 16.961(5) _cell_length_b 13.219(2) _cell_length_c 11.598(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 45 _cell_measurement_theta_min 15 _cell_volume 2571.2(10) _computing_cell_refinement 'CAD-4 Operations Manual' _computing_data_collection 'CAD-4 Operations Manual (Enraf-Nonius, 1977)' _computing_data_reduction 'program elaborated at CRMC2' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'Word 5.0 on Machintoch LC II' _computing_structure_refinement 'SHELX76 (Sheldrick, 1976)' _computing_structure_solution 'MULTAN80 (Main et al., 1980)' _diffrn_ambient_temperature 293 _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_av_sigmaI/netI 0.1928 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 5489 _diffrn_reflns_reduction_process 'SDP system' _diffrn_reflns_theta_max 45 _diffrn_reflns_theta_min 2 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 4 _exptl_absorpt_coefficient_mu 0.76 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_meas 1.41(2) _exptl_crystal_density_method flotation _exptl_crystal_description 'square prism' _exptl_crystal_F_000 1136 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _refine_diff_density_max .25 _refine_diff_density_min -.23 _refine_ls_goodness_of_fit_all 0.93 _refine_ls_goodness_of_fit_obs 0.93 _refine_ls_hydrogen_treatment ; H-atom displacement parameters not refined ; _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 220 _refine_ls_number_reflns 2552 _refine_ls_number_restraints 0 _refine_ls_R_factor_all .041 _refine_ls_R_factor_obs .041 _refine_ls_shift/esd_max .13 _refine_ls_shift/esd_mean .13 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme unit _refine_ls_wR_factor_all .041 _refine_ls_wR_factor_obs .041 _reflns_number_observed 2552 _reflns_number_total 5489 _reflns_observed_criterion refl_obs_if_I_>_3.0_sigma(I) _cod_data_source_file pa1143.cif _cod_data_source_block pepe2 _cod_original_cell_volume 2571.6(7) _cod_original_sg_symbol_H-M 'A 2/a' _cod_original_formula_sum 'C15 H13 N1 O4' _cod_database_code 2003398 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,+y,-z -x,-y,-z 1/2+x,-y,+z x,1/2+y,1/2+z 1/2-x,1/2+y,1/2-z -x,1/2-y,1/2-z 1/2+x,1/2-y,1/2+z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_B_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_type_symbol C1 -.0087(1) -.1955(1) -.4759(2) 3.0(1) Uani d C C2 .0484(1) -.1829(2) -.4045(2) 3.6(1) Uani d C C3 .1128(1) -.1198(2) -.4366(2) 3.2(1) Uani d C C4 .1182(1) -.0656(1) -.5385(2) 3.2(1) Uani d C C5 .0596(1) -.0742(1) -.6104(1) 2.5(1) Uani d C C6 -.0043(1) -.1400(1) -.5801(1) 2.0(1) Uani d C N7 -.0642(1) -.1524(1) -.6497(1) 2.0(1) Uani d N C8 -.1442(1) -.1923(1) -.6012(1) 2.6(1) Uani d C C9 -.1931(1) -.1682(1) -.6921(1) 1.7(1) Uani d C C10 -.1348(1) -.1663(1) -.8076(1) 1.8(1) Uani d C C11 -.0583(1) -.1360(1) -.7685(1) 2.2(1) Uani d O O12 .0041(1) -.1060(1) -.8290(1) 3.0(1) Uani d C C13 -.2709(1) -.2161(1) -.7113(2) 3.1(1) Uani d C C14 -.3052(1) -.1531(2) -.7761(2) 3.0(1) Uani d C C15 -.2512(1) -.0624(1) -.7945(1) 2.6(1) Uani d C C16 -.1775(1) -.0947(1) -.8848(1) 2.6(1) Uani d C C17 -.1285(1) -.0056(1) -.9375(1) 2.1(1) Uani d C O18 -.0864(1) -.0294(1) -1.0369(1) 4.1(1) Uani d O O19 -.1283(1) .0763(1) -.8954(1) 5.1(1) Uani d O O20 -.2166(1) -.0624(1) -.6875(1) 2.2(1) Uani d O H1 -.058(1) -.245(2) -.452(2) ? ? ? ? H2 .048(1) -.233(2) -.324(2) ? ? ? ? H3 .152(1) -.099(2) -.393(2) ? ? ? ? H4 .172(1) -.017(2) -.567(2) ? ? ? ? H5 .067(1) -.026(2) -.694(2) ? ? ? ? H6 -.172(1) -.159(2) -.533(2) ? ? ? ? H7 -.145(1) -.283(2) -.570(2) ? ? ? ? H8 -.126(1) -.227(2) -.847(2) ? ? ? ? H9 -.285(1) -.277(2) -.690(2) ? ? ? ? H10 -.356(1) -.176(2) -.811(2) ? ? ? ? H11 -.284(1) -.003(2) -.810(2) ? ? ? ? H12 -.191(1) -.135(2) -.949(2) ? ? ? ? H13 -.065(1) .013(2) -1.081(2) ? ? ? ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 6 1 3 4 5 1 8 3 1 5 4 2 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 C11 C10 C9 102.4(3) yes C11 C10 C16 120.9(4) yes C16 C10 C9 102.5(3) yes C10 C11 N7 108.9(4) yes C10 C11 O12 128.3(4) yes N7 C11 O12 122.7(4) yes C14 C13 C9 106.9(5) yes C13 C14 C15 105.9(5) yes C14 C15 C16 106.6(4) yes C14 C15 O20 101.2(4) yes C16 C15 O20 100.8(3) yes C10 C16 C15 100.1(3) yes C10 C16 C17 115.5(4) yes C15 C16 C17 113.1(4) yes C16 C17 O18 111.4(4) yes C16 C17 O19 125.3(4) yes O18 C17 O19 123.4(4) yes C1 C2 C3 120.7(6) yes C2 C3 C4 119.7(6) yes C3 C4 C5 120.7(5) yes C4 C5 C6 119.8(4) yes C1 C6 C5 118.8(4) yes C1 C6 N7 119.0(4) yes C5 C6 N7 122.2(4) yes C9 C8 N7 103.4(4) yes C10 C9 C8 105.7(4) yes C10 C9 C13 109.9(4) yes C10 C9 O20 98.8(3) yes C13 C9 C8 127.9(4) yes C13 C9 O20 99.7(3) yes C8 C9 O20 111.3(4) yes C11 N7 C6 127.3(4) yes C11 N7 C8 111.1(4) yes C6 N7 C8 121.6(4) yes C15 O20 C9 96.5(4) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag C1 C2 1.375(4) yes C1 C6 1.406(3) yes C10 C9 1.542(3) yes C10 C11 1.492(3) yes C10 C16 1.554(3) yes C11 N7 1.383(3) yes C11 O12 1.244(3) yes C13 C9 1.510(3) yes C13 C14 1.314(4) yes C14 C15 1.505(3) yes C15 C16 1.565(3) yes C15 O20 1.450(3) yes C16 C17 1.517(3) yes C17 O18 1.301(3) yes C17 O19 1.188(3) yes C2 C3 1.381(4) yes C3 C4 1.374(4) yes C4 C5 1.394(3) yes C5 C6 1.393(3) yes C6 N7 1.399(3) yes C8 N7 1.486(3) yes C8 C9 1.472(3) yes C9 O20 1.453(3) yes