#------------------------------------------------------------------------------ #$Date: 2011-09-10 05:16:28 +0200 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2009121.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_2009121 loop_ _publ_author_name 'Blackburn, A. C.' 'Fitzgerald, L. J.' 'Gerkin, R. E.' _publ_section_title ; C---H···O interactions in acenaphthene-5,6-dicarboxylic anhydride ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1852 _journal_page_last 1854 _journal_volume 55 _journal_year 1999 _chemical_formula_moiety 'C14 H8 O3 ' _chemical_formula_sum 'C14 H8 O3' _chemical_formula_weight 224.22 _chemical_name_common 'acenaphthene-5,6-dicarboxylic anhydride' _chemical_name_systematic ' ?' _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _cell_angle_alpha 90 _cell_angle_beta 117.850(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.140(2) _cell_length_b 9.6710(10) _cell_length_c 7.621(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 296 _cell_measurement_theta_max 17.4 _cell_measurement_theta_min 16.5 _cell_volume 986.6(3) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988) ; _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1995)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'TEXSAN and PLATON (Spek, 1990) ' _computing_structure_refinement TEXSAN _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 296 _diffrn_measurement_device_type AFC5S _diffrn_measurement_method '\w/2\q scans ' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 1241 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 2.0 _diffrn_standards_decay_% ' +- 1.1 (average maximum relative intensity)' _diffrn_standards_interval_count 150 _diffrn_standards_number 6 _exptl_absorpt_coefficient_mu 0.107 _exptl_absorpt_correction_type none _exptl_crystal_colour 'pale amber' _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method none _exptl_crystal_description 'uncut irregular polyhedron' _exptl_crystal_F_000 464 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.23 _refine_diff_density_max 0.25 _refine_diff_density_min -0.20 _refine_ls_extinction_coef '3.1(8) \\times 10^-7^' _refine_ls_extinction_method ' Zachariasen (1963, 1968)' _refine_ls_goodness_of_fit_ref 1.85 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 96 _refine_ls_number_reflns 1129 _refine_ls_R_factor_gt 0.041 _refine_ls_shift/su_max 0.0002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'w = 1/[\s^2^~cs~ + (0.014 I)^2^]' _refine_ls_wR_factor_ref 0.079 _reflns_number_gt 785 _reflns_number_total 1129 _reflns_threshold_expression 'I > 2.0\s~I~' _[local]_cod_data_source_file fr1213.cif _[local]_cod_data_source_block 1 _[local]_cod_cif_authors_sg_H-M 'C 2/c' _[local]_cod_chemical_formula_sum_orig 'C14 H8 O3 ' _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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 986.6(2) _cod_database_code 2009121 loop_ _symmetry_equiv_pos_as_xyz x,y,z '-x, y, 1/2-z' '-x, -y, -z' 'x, -y, 1/2+z' '1/2+x, 1/2+y, z' '1/2-x, 1/2+y, 1/2-z' '1/2-x, 1/2-y, -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_U_iso_or_equiv _atom_site_adp_type O1 -0.14627(9) 0.80330(10) -0.0169(2) 0.0677(4) Uij O2 0.0000 0.79300(10) 0.2500 0.0494(4) Uij C1 -0.05200(10) 0.1358(2) 0.1571(3) 0.0566(6) Uij C2 -0.07890(10) 0.28690(10) 0.1088(2) 0.0413(4) Uij C3 -0.15960(10) 0.3543(2) -0.0358(2) 0.0476(5) Uij C4 -0.16170(10) 0.4997(2) -0.0386(2) 0.0440(4) Uij C5 -0.08360(10) 0.57760(10) 0.1006(2) 0.0362(4) Uij C6 0.0000 0.5099(2) 0.2500 0.0339(5) Uij C7 0.0000 0.3661(2) 0.2500 0.0360(6) Uij C8 -0.08360(10) 0.7285(2) 0.0994(2) 0.0445(5) Uij H1A -0.1010(10) 0.089(2) 0.188(2) 0.062(5) Uiso H1B -0.0530(10) 0.091(2) 0.041(3) 0.078(6) Uiso H3 -0.2170(10) 0.306(2) -0.138(2) 0.061(5) Uiso H4 -0.2150(10) 0.546(2) -0.136(2) 0.059(5) Uiso 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 0.0673(8) 0.0431(7) 0.0682(8) 0.0130(6) 0.0113(7) 0.0134(6) O2 0.0590(10) 0.0300(8) 0.0490(9) 0.0000 0.0163(8) 0.0000 C1 0.0680(10) 0.0322(8) 0.0770(10) -0.0067(8) 0.0396(10) -0.0061(8) C2 0.0476(9) 0.0315(8) 0.0511(9) -0.0054(7) 0.0282(8) -0.0050(7) C3 0.0444(10) 0.0461(9) 0.0488(10) -0.0126(7) 0.0188(8) -0.0100(8) C4 0.0385(9) 0.0475(9) 0.0398(9) 0.0005(7) 0.0131(7) 0.0022(8) C5 0.0409(8) 0.0318(7) 0.0370(8) 0.0008(6) 0.0191(6) 0.0018(6) C6 0.0370(10) 0.0314(10) 0.0370(10) 0.0000 0.0194(9) 0.0000 C7 0.0400(10) 0.0300(10) 0.0430(10) 0.0000 0.0229(10) 0.0000 C8 0.0502(10) 0.0373(9) 0.0438(9) 0.0032(7) 0.0202(7) 0.0045(7) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H 0 0 'Stewart, Davidson & Simpson (1965)' C 0.003 0.002 'Creagh & McAuley (1992)' O 0.011 0.006 'Creagh & McAuley (1992)' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle _geom_angle_publ_flag C8 O2 C8 2_555 127.0(2) yes C1 C1 C2 2_555 105.37(9) no C1 C1 H1A 2_555 110.0(9) no C1 C1 H1B 2_555 113.9(10) no C2 C1 H1A ? 110.7(9) no C2 C1 H1B ? 108.0(10) no H1A C1 H1B ? 108.0(10) no C1 C2 C3 ? 133.80(10) no C1 C2 C7 ? 107.70(10) no C3 C2 C7 ? 118.50(10) no C2 C3 C4 ? 119.60(10) no C2 C3 H3 ? 122.8(9) no C4 C3 H3 ? 117.6(9) no C3 C4 C5 ? 121.80(10) no C3 C4 H4 ? 120.0(9) no C5 C4 H4 ? 118.2(9) no C4 C5 C6 ? 119.40(10) no C4 C5 C8 ? 122.80(10) no C6 C5 C8 ? 117.90(10) no C5 C6 C5 2_555 124.6(2) no C5 C6 C7 ? 117.70(9) no C5 C6 C7 2_555 117.70(9) no C2 C7 C2 2_555 113.9(2) no C2 C7 C6 ? 123.05(9) no C2 C7 C6 2_555 123.05(9) no O1 C8 O2 ? 116.10(10) yes O1 C8 C5 ? 127.5(2) yes O2 C8 C5 ? 116.40(10) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C8 ? 1.193(2) yes O2 C8 ? 1.397(2) yes O2 C8 2_555 1.397(2) no C1 C1 2_555 1.550(4) yes C1 C2 ? 1.515(2) yes C1 H1A ? 0.99(2) no C1 H1B ? 0.98(2) no C2 C3 ? 1.369(2) no C2 C7 ? 1.404(2) no C3 C4 ? 1.406(2) no C3 H3 ? 0.970(10) no C4 C5 ? 1.385(2) no C4 H4 ? 0.92(2) no C5 C6 ? 1.407(2) no C5 C8 ? 1.459(2) yes C6 C7 ? 1.390(3) 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 C3 H3 O1 6_444 0.970(10) 2.47(2) 3.338(2) 148.0(10) yes C1 H1A O1 4_565 0.99(2) 2.84(2) 3.445(2) 120.0(10) yes C1 H1B O2 3_565 0.98(2) 2.91(2) 3.606(2) 128.0(10) yes