#------------------------------------------------------------------------------ #$Date: 2015-04-02 14:22:18 +0300 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/82/2008248.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_2008248 loop_ _publ_author_name 'Zukerman-Schpector, J.' 'Biaggio, Francisco C.' 'Rufino, Alessandra R.' 'Caracelli, I.' _publ_section_title ; Two new spiro lactam-lactones ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 416 _journal_page_last 419 _journal_paper_doi 10.1107/S0108270198010403 _journal_volume 55 _journal_year 1999 _chemical_formula_moiety 'C10 H15 N O3' _chemical_formula_sum 'C10 H15 N O3' _chemical_formula_weight 197.23 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _cell_angle_alpha 90.00 _cell_angle_beta 108.980(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.9910(10) _cell_length_b 10.0980(10) _cell_length_c 10.5760(10) _cell_measurement_reflns_used 23 _cell_measurement_temperature 293 _cell_measurement_theta_max 14.74 _cell_measurement_theta_min 9.77 _cell_volume 1008.99(18) _computing_cell_refinement 'CAD4 Software (Enraf-Nonius,1989)' _computing_data_collection 'CAD4 Software (Enraf-Nonius,1989)' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1995)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997) and PARST95 (Nardelli, 1995)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1985)' _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _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 0.71073 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 1656 _diffrn_reflns_theta_max 24.00 _diffrn_standards_decay_% 1.1% _diffrn_standards_interval_time 30 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.096 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_meas ? _exptl_crystal_description irregular _exptl_crystal_F_000 424.0 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.177 _refine_diff_density_min -0.198 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 0.970 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 128 _refine_ls_number_reflns 1558 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.970 _refine_ls_restrained_S_obs 0.970 _refine_ls_R_factor_all 0.1631 _refine_ls_R_factor_gt 0.047 _refine_ls_shift/su_max <0.0001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0544P)^2^+0.1276P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1326 _refine_ls_wR_factor_ref 0.104 _reflns_number_gt 742 _reflns_number_total 1558 _reflns_threshold_expression F^2^>2\sF^2^ _[local]_cod_data_source_file fg1506.cif _[local]_cod_data_source_block 2 _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_hydrogen_treatment' value ' constr ' changed to 'constr' 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: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0544P)^2^+0.1276P] 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^)+(0.0544P)^2^+0.1276P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 2008248 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol N 0.8385(3) 0.1120(3) 0.9420(3) 0.0441(8) Uani d . 1 . . N H1N 0.9126 0.0866 0.9243 0.053 Uiso calc R 1 . . H O3 0.5458(3) 0.0294(3) 0.8002(3) 0.0735(9) Uani d . 1 . . O O2 0.5752(3) 0.1331(3) 0.6277(2) 0.0672(8) Uani d . 1 . . O O1 0.9327(2) 0.0045(3) 1.1336(2) 0.0564(7) Uani d . 1 . . O C1 0.6112(4) 0.1073(4) 0.7583(4) 0.0518(10) Uani d . 1 . . C C3 0.6763(4) 0.2248(4) 0.6008(3) 0.0607(11) Uani d . 1 . . C H3 0.6377 0.3148 0.5915 0.073 Uiso calc R 1 . . H C4 0.8024(4) 0.2164(4) 0.7247(3) 0.0525(10) Uani d . 1 . . C H4A 0.8549 0.2989 0.7406 0.063 Uiso calc R 1 . . H H4B 0.8650 0.1452 0.7180 0.063 Uiso calc R 1 . . H C5 0.7400(3) 0.1889(3) 0.8358(3) 0.0419(9) Uani d . 1 . . C C7 0.8357(4) 0.0730(3) 1.0627(4) 0.0465(9) Uani d . 1 . . C C8 0.7140(4) 0.1088(4) 1.1106(4) 0.0657(12) Uani d . 1 . . C H8A 0.7343 0.0747 1.2006 0.079 Uiso calc R 1 . . H H8B 0.6302 0.0635 1.0543 0.079 Uiso calc R 1 . . H C9 0.6795(4) 0.2545(5) 1.1121(4) 0.0793(13) Uani d . 1 . . C H9A 0.7667 0.3029 1.1532 0.095 Uiso calc R 1 . . H H9B 0.6197 0.2671 1.1672 0.095 Uiso calc R 1 . . H C10 0.6054(4) 0.3126(4) 0.9744(4) 0.0760(13) Uani d . 1 . . C H10A 0.5219 0.2600 0.9308 0.091 Uiso calc R 1 . . H H10B 0.5739 0.4015 0.9854 0.091 Uiso calc R 1 . . H C11 0.6955(4) 0.3191(4) 0.8839(4) 0.0619(11) Uani d . 1 . . C H11A 0.7808 0.3681 0.9305 0.074 Uiso calc R 1 . . H H11B 0.6441 0.3703 0.8055 0.074 Uiso calc R 1 . . H C12 0.6995(4) 0.1845(5) 0.4730(4) 0.0790(14) Uani d . 1 . . C H12A 0.7613 0.2470 0.4517 0.119 Uiso calc R 1 . . H H12B 0.6104 0.1826 0.4021 0.119 Uiso calc R 1 . . H H12C 0.7418 0.0980 0.4835 0.119 Uiso calc R 1 . . H 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 N 0.0308(16) 0.053(2) 0.0478(17) 0.0056(14) 0.0121(13) 0.0069(16) O3 0.0551(18) 0.083(2) 0.083(2) -0.0224(15) 0.0236(15) -0.0029(17) O2 0.0538(17) 0.084(2) 0.0562(17) -0.0142(15) 0.0071(13) 0.0021(16) O1 0.0475(16) 0.0691(17) 0.0497(14) 0.0167(14) 0.0120(12) 0.0111(14) C1 0.040(2) 0.058(3) 0.055(3) 0.000(2) 0.0132(19) -0.001(2) C3 0.058(3) 0.064(3) 0.057(2) 0.012(2) 0.015(2) 0.015(2) C4 0.045(2) 0.050(2) 0.058(2) 0.0066(19) 0.0119(18) 0.015(2) C5 0.0317(19) 0.041(2) 0.047(2) 0.0037(17) 0.0040(17) 0.0070(18) C7 0.045(2) 0.047(2) 0.047(2) -0.002(2) 0.0148(19) -0.008(2) C8 0.054(2) 0.084(3) 0.067(3) 0.015(2) 0.029(2) 0.008(2) C9 0.062(3) 0.106(4) 0.077(3) 0.020(3) 0.033(2) -0.010(3) C10 0.067(3) 0.070(3) 0.091(3) 0.024(2) 0.026(3) -0.010(3) C11 0.056(2) 0.051(3) 0.069(3) 0.0121(19) 0.008(2) -0.001(2) C12 0.072(3) 0.101(4) 0.059(3) 0.017(3) 0.015(2) 0.017(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' 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' 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 C7 N C5 132.2(3) yes C1 O2 C3 110.7(3) yes O3 C1 O2 121.0(3) no O3 C1 C5 128.6(3) no O2 C1 C5 110.4(3) no O2 C3 C4 103.4(3) no O2 C3 C12 108.8(3) no C4 C3 C12 116.2(3) no C3 C4 C5 104.2(3) no N C5 C1 111.6(3) no N C5 C4 110.4(3) no C1 C5 C4 99.7(3) no N C5 C11 113.6(3) no C1 C5 C11 111.0(3) no C4 C5 C11 109.7(3) no O1 C7 N 119.3(3) no O1 C7 C8 119.6(3) no N C7 C8 121.2(3) no C7 C8 C9 116.7(3) no C8 C9 C10 114.1(3) no C11 C10 C9 114.7(3) no C10 C11 C5 118.1(3) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag N C7 1.345(4) yes N C5 1.454(4) yes O3 C1 1.197(4) no O2 C1 1.335(4) yes O2 C3 1.465(4) yes O1 C7 1.227(4) yes C1 C5 1.523(5) no C3 C4 1.496(4) no C3 C12 1.500(5) no C4 C5 1.524(4) no C5 C11 1.527(5) no C7 C8 1.505(5) no C8 C9 1.512(5) no C9 C10 1.520(5) no C10 C11 1.514(5) no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N H1N O 3_757 0.86 2.055 2.905(3) 169 yes