#------------------------------------------------------------------------------ #$Date: 2017-10-13 03:08:28 +0300 (Fri, 13 Oct 2017) $ #$Revision: 201955 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/49/2004996.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_2004996 loop_ _publ_author_name 'Feeder, N.' 'Jones, W.' _publ_section_title ; Four \w-Phthalimidoaliphatic Peracids ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1516 _journal_page_last 1520 _journal_paper_doi 10.1107/S010827019501701X _journal_volume 52 _journal_year 1996 _chemical_formula_moiety 'C13 H13 N1 O5' _chemical_formula_sum 'C13 H13 N O5' _chemical_formula_weight 263.24 _chemical_name_common '5-phthalimidoperpentanoic acid' _chemical_name_systematic ; 1,3-dihydro-1,3-dioxo-2H-isoindole-2-pentaneperoxoic acid ; _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' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 98.22(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.7773(10) _cell_length_b 4.7222(10) _cell_length_c 19.935(4) _cell_measurement_reflns_used 25 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 15 _cell_measurement_theta_min 8 _cell_volume 631.4(2) _computing_cell_refinement 'CAD-4 Software (SETANG)' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1995)' _computing_molecular_graphics TEXSAN _computing_publication_material SHELXL93 _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 295(2) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.1128 _diffrn_reflns_av_sigmaI/netI 0.0925 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2277 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_min 2.06 _diffrn_standards_decay_% 1 _diffrn_standards_interval_count 100 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 0.108 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 276 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.270 _refine_diff_density_min -0.193 _refine_ls_extinction_coef 0.067(15) _refine_ls_extinction_method SHELXL93 _refine_ls_goodness_of_fit_all 1.014 _refine_ls_goodness_of_fit_obs 1.144 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_parameters 178 _refine_ls_number_reflns 2181 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.051 _refine_ls_restrained_S_obs 1.143 _refine_ls_R_factor_all 0.1621 _refine_ls_R_factor_obs 0.0611 _refine_ls_shift/esd_max 0.004 _refine_ls_shift/esd_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.1032P)^2^] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_wR_factor_all 0.2020 _refine_ls_wR_factor_obs 0.1526 _reflns_number_observed 1145 _reflns_number_total 2214 _reflns_observed_criterion >2sigma(I) _cod_data_source_file ha1155.cif _cod_data_source_block III _cod_original_cell_volume 631.5(2) _cod_original_sg_symbol_Hall 'P 2y1' _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 2004996 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' 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 N1 0.046(2) 0.069(4) 0.054(3) -0.001(3) 0.000(2) 0.004(3) O8 0.061(2) 0.097(4) 0.080(3) 0.023(3) 0.020(2) 0.001(3) O7 0.084(3) 0.139(5) 0.068(3) 0.003(3) 0.029(2) 0.016(3) O130 0.115(4) 0.073(3) 0.089(3) 0.031(3) -0.032(3) -0.025(3) O131 0.068(2) 0.078(3) 0.059(2) 0.003(2) -0.010(2) -0.011(2) O132 0.075(3) 0.100(3) 0.079(3) -0.005(3) -0.026(2) 0.008(3) C6 0.042(3) 0.066(4) 0.056(3) -0.004(3) 0.003(2) -0.011(3) C5 0.037(3) 0.093(5) 0.075(4) 0.002(3) 0.005(3) -0.016(4) C4 0.052(3) 0.065(4) 0.082(5) 0.014(3) -0.011(3) -0.005(4) C3 0.067(4) 0.068(4) 0.063(4) 0.002(4) 0.000(3) -0.001(4) C2 0.054(3) 0.064(4) 0.061(4) 0.007(3) 0.009(3) 0.005(3) C1 0.043(3) 0.048(3) 0.052(3) 0.001(3) 0.005(2) -0.004(3) C8 0.051(3) 0.065(4) 0.058(3) -0.003(3) 0.002(3) -0.006(3) C7 0.053(3) 0.081(5) 0.051(4) -0.012(3) 0.006(3) -0.003(4) C9 0.067(4) 0.057(4) 0.067(4) -0.002(3) -0.008(3) 0.008(4) C10 0.062(3) 0.055(4) 0.058(3) 0.001(3) -0.006(3) -0.001(3) C11 0.067(4) 0.057(4) 0.055(3) 0.002(3) -0.005(3) 0.004(3) C12 0.060(3) 0.067(4) 0.051(3) 0.008(3) -0.004(3) -0.003(3) C13 0.070(4) 0.044(3) 0.057(4) 0.001(3) -0.001(3) -0.007(3) loop_ _atom_site_label _atom_site_occupancy _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_type_symbol N1 1 0.9699(6) -0.1681(11) 0.2068(2) 0.0571(13) Uani d . N O8 1 1.1739(6) -0.1546(11) 0.1239(2) 0.0784(14) Uani d . O O7 1 0.7138(6) -0.0776(14) 0.2678(2) 0.095(2) Uani d . O O130 1 1.7588(7) -0.5699(12) 0.4191(2) 0.097(2) Uani d . O O131 1 1.7438(6) -0.2359(9) 0.4971(2) 0.0700(13) Uani d . O O132 1 1.9133(6) -0.3809(11) 0.5341(2) 0.0884(15) Uani d . O C6 1 0.7335(7) 0.1531(13) 0.1609(3) 0.0546(15) Uani d . C C5 1 0.5736(7) 0.3306(16) 0.1466(3) 0.068(2) Uani d . C H2 1 0.4788(7) 0.3459(16) 0.1758(3) 0.064(8) Uiso calc R H C4 1 0.5570(8) 0.4880(15) 0.0868(3) 0.069(2) Uani d . C H3 1 0.4510(8) 0.6129(15) 0.0763(3) 0.064(8) Uiso calc R H C3 1 0.6959(8) 0.4597(15) 0.0436(3) 0.067(2) Uani d . C H4 1 0.6808(8) 0.5640(15) 0.0036(3) 0.064(8) Uiso calc R H C2 1 0.8574(8) 0.2807(13) 0.0578(3) 0.060(2) Uani d . C H5 1 0.9519(8) 0.2642(13) 0.0284(3) 0.064(8) Uiso calc R H C1 1 0.8733(7) 0.1271(13) 0.1172(3) 0.0478(13) Uani d . C C8 1 1.0252(8) -0.0747(14) 0.1460(3) 0.058(2) Uani d . C C7 1 0.7948(8) -0.0348(15) 0.2196(3) 0.062(2) Uani d . C C9 1 1.0874(9) -0.3570(15) 0.2546(3) 0.065(2) Uani d . C H9A 1 1.1607(9) -0.4882(15) 0.2300(3) 0.086(15) Uiso calc R H H9B 1 0.9988(9) -0.4663(15) 0.2788(3) 0.086(15) Uiso calc R H C10 1 1.2326(8) -0.1932(13) 0.3051(3) 0.060(2) Uani d . C H10A 1 1.3065(8) -0.0621(13) 0.2807(3) 0.084(15) Uiso calc R H H10B 1 1.1581(8) -0.0829(13) 0.3340(3) 0.084(15) Uiso calc R H C11 1 1.3787(8) -0.3814(14) 0.3491(3) 0.061(2) Uani d . C H11A 1 1.3060(8) -0.5189(14) 0.3722(3) 0.058(11) Uiso calc R H H11B 1 1.4598(8) -0.4837(14) 0.3209(3) 0.058(11) Uiso calc R H C12 1 1.5112(7) -0.2081(14) 0.4006(3) 0.061(2) Uani d . C H12A 1 1.5624(7) -0.0485(14) 0.3778(3) 0.112(18) Uiso calc R H H12B 1 1.4315(7) -0.1331(14) 0.4333(3) 0.112(18) Uiso calc R H C13 1 1.6832(9) -0.3686(15) 0.4379(3) 0.0578(15) Uani d . C 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' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 '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 C8 N1 C7 111.0(4) no C8 N1 C9 125.1(5) no C7 N1 C9 123.7(5) no C13 O131 O132 110.4(4) no C5 C6 C1 121.2(6) no C5 C6 C7 131.0(5) no C1 C6 C7 107.8(5) no C6 C5 C4 118.0(5) no C3 C4 C5 120.4(6) no C4 C3 C2 121.8(6) no C1 C2 C3 117.4(5) no C2 C1 C6 121.2(5) no C2 C1 C8 130.2(5) no C6 C1 C8 108.6(5) no O8 C8 N1 123.9(5) no O8 C8 C1 129.4(6) no N1 C8 C1 106.7(5) no O7 C7 N1 124.9(6) no O7 C7 C6 129.1(6) no N1 C7 C6 105.9(4) no N1 C9 C10 111.4(5) no C11 C10 C9 113.2(5) no C12 C11 C10 110.7(5) no C13 C12 C11 114.2(5) no O130 C13 O131 124.5(6) no O130 C13 C12 126.9(5) no O131 C13 C12 108.5(5) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag N1 C8 1.390(7) no N1 C7 1.399(7) no N1 C9 1.457(7) no O8 C8 1.215(6) no O7 C7 1.191(6) no O130 C13 1.167(7) no O131 C13 1.348(7) no O131 O132 1.446(6) no C6 C5 1.368(8) no C6 C1 1.382(7) no C6 C7 1.480(8) no C5 C4 1.395(8) no C4 C3 1.370(8) no C3 C2 1.380(8) no C2 C1 1.379(7) no C1 C8 1.459(8) no C9 C10 1.515(8) no C10 C11 1.513(7) no C11 C12 1.506(7) no C12 C13 1.496(8) no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 _geom_contact_publ_flag O132 O130 2.715(7) 2_956 no O132 O132 3.044(7) 2_956 no O130 O132 2.715(7) 2_946 no O132 O132 3.044(7) 2_946 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 C1 C6 C5 C4 -0.8(8) no C7 C6 C5 C4 178.7(6) no C6 C5 C4 C3 1.2(9) no C5 C4 C3 C2 -1.1(9) no C4 C3 C2 C1 0.7(8) no C3 C2 C1 C6 -0.4(8) no C3 C2 C1 C8 -179.5(6) no C5 C6 C1 C2 0.5(8) no C7 C6 C1 C2 -179.2(5) no C5 C6 C1 C8 179.7(5) no C7 C6 C1 C8 0.1(6) no C7 N1 C8 O8 178.7(6) no C9 N1 C8 O8 4.6(9) no C7 N1 C8 C1 -1.3(6) no C9 N1 C8 C1 -175.4(5) no C2 C1 C8 O8 -0.1(10) no C6 C1 C8 O8 -179.3(6) no C2 C1 C8 N1 179.9(6) no C6 C1 C8 N1 0.7(6) no C8 N1 C7 O7 179.3(6) no C9 N1 C7 O7 -6.5(9) no C8 N1 C7 C6 1.4(6) no C9 N1 C7 C6 175.6(5) no C5 C6 C7 O7 1.7(11) no C1 C6 C7 O7 -178.7(6) no C5 C6 C7 N1 179.5(6) no C1 C6 C7 N1 -0.9(6) no C8 N1 C9 C10 88.3(7) no C7 N1 C9 C10 -85.1(6) no N1 C9 C10 C11 -171.4(5) no C9 C10 C11 C12 -176.9(5) no C10 C11 C12 C13 -169.5(5) no O132 O131 C13 O130 -0.8(9) no O132 O131 C13 C12 -178.7(4) no C11 C12 C13 O130 25.0(9) no C11 C12 C13 O131 -157.2(5) no loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 16081732