#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003629.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003629 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1472 _journal_page_last 1474 _publ_section_title ; 5,5'-Di(anthracenecarboxylic) Anhydride ; _chemical_formula_moiety 'C30 H18 O3' _chemical_formula_sum 'C30 H18 O3' _chemical_formula_weight 426.44 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _symmetry_space_group_name_H-M 'P -1' _cell_length_a 9.834(5) _cell_length_b 10.973(6) _cell_length_c 11.510(6) _cell_angle_alpha 112.51(2) _cell_angle_beta 89.56(2) _cell_angle_gamma 107.24(2) _cell_volume 1087.9(10) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.302 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 12 _cell_measurement_theta_min 15 _cell_measurement_theta_max 16 _exptl_absorpt_coefficient_mu 0.083 _cell_measurement_temperature 295(2) _exptl_crystal_description Lath _exptl_crystal_size_max 0.82 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.19 _exptl_crystal_colour Yellow _chemical_compound_source ; Treatment of 5-anthracenecarboxylic acid with oxalyl chloride yields 5-anthracenecarboxyl chloride, which reacts with residual acid to give 5,5'-di(anthracenecarboxylic) anhydride (1). Crystals of (1) were grown by the slow concentration of a dichloromethane solution. ; _diffrn_measurement_device 'Stoe Stadi-4 four-circle diffractometer' _diffrn_measurement_method ; \w-2\q scans using on-line profile-fitting (Clegg, 1981) ; _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 6230 _reflns_number_total 6230 _reflns_number_observed 4003 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_theta_max 30.02 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 2 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0555 _refine_ls_wR_factor_obs 0.1285 _refine_ls_wR_factor_all 0.1724 _refine_ls_goodness_of_fit_obs 1.070 _refine_ls_goodness_of_fit_all 1.042 _refine_ls_number_reflns 6099 _refine_ls_number_parameters 299 _refine_ls_hydrogen_treatment ; H atoms included in calculated positions and allowed to ride on the corresponding C atoms with U~iso~ = 1.2U~eq~(C) ; _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+0.3047P] wh _refine_ls_shift/esd_max 0.017 _refine_diff_density_max 0.222 _refine_diff_density_min -0.169 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_extinction_coef 0.0064(19) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.001 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.006 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 C11 1 0.6365(2) 0.8355(2) 0.45459(14) 0.0446(4) O11 1 0.52184(14) 0.8336(2) 0.42084(13) 0.0637(4) O 1 0.66610(12) 0.82598(13) 0.56761(10) 0.0520(3) C12 1 0.5608(2) 0.7589(2) 0.62373(14) 0.0429(3) O12 1 0.45730(14) 0.66601(13) 0.56461(11) 0.0615(4) C1 1 1.0130(2) 0.6592(2) 0.2274(2) 0.0693(6) H1A 1 1.0972(2) 0.6721(2) 0.1850(2) 0.083 C2 1 0.9518(3) 0.5356(2) 0.2357(2) 0.0749(6) H2A 1 0.9927(3) 0.4619(2) 0.1994(2) 0.090 C3 1 0.8282(2) 0.5145(2) 0.2974(2) 0.0660(5) H3A 1 0.7859(2) 0.4265(2) 0.3031(2) 0.079 C4 1 0.7682(2) 0.6164(2) 0.3485(2) 0.0531(4) H4A 1 0.6835(2) 0.5993(2) 0.3895(2) 0.064 C4A 1 0.8288(2) 0.7492(2) 0.34266(14) 0.0440(4) C5 1 0.7691(2) 0.8574(2) 0.39180(14) 0.0425(3) C5A 1 0.8297(2) 0.9861(2) 0.38296(15) 0.0455(4) C6 1 0.7750(2) 1.1001(2) 0.4369(2) 0.0584(5) H6A 1 0.6915(2) 1.0897(2) 0.4805(2) 0.070 C7 1 0.8397(2) 1.2230(2) 0.4273(2) 0.0735(6) H7A 1 0.8021(2) 1.2988(2) 0.4652(2) 0.088 C8 1 0.9614(2) 1.2409(3) 0.3626(3) 0.0801(7) H8A 1 1.0049(2) 1.3281(3) 0.3555(3) 0.096 C9 1 1.0170(2) 1.1365(2) 0.3106(2) 0.0703(6) H9A 1 1.0995(2) 1.1502(2) 0.2663(2) 0.084 C9A 1 0.9558(2) 1.0058(2) 0.3202(2) 0.0522(4) C10 1 1.0144(2) 0.8983(2) 0.2712(2) 0.0572(5) H10A 1 1.0991(2) 0.9124(2) 0.2295(2) 0.069 C10A 1 0.9550(2) 0.7713(2) 0.2804(2) 0.0508(4) C1' 1 0.6942(2) 1.1525(2) 1.0439(2) 0.0601(5) H1'A 1 0.7333(2) 1.1916(2) 1.1313(2) 0.072 C2' 1 0.6544(2) 1.2326(2) 0.9959(2) 0.0642(5) H2'A 1 0.6654(2) 1.3278(2) 1.0491(2) 0.077 C3' 1 0.5963(2) 1.1773(2) 0.8674(2) 0.0583(5) H3'A 1 0.5673(2) 1.2351(2) 0.8344(2) 0.070 C4' 1 0.5812(2) 1.0433(2) 0.7901(2) 0.0480(4) H4'A 1 0.5421(2) 1.0078(2) 0.7031(2) 0.058 C4A' 1 0.6228(2) 0.9548(2) 0.83671(14) 0.0410(3) C5' 1 0.6082(2) 0.8151(2) 0.76153(13) 0.0399(3) C5A' 1 0.6443(2) 0.7283(2) 0.81138(15) 0.0438(3) C6' 1 0.6354(2) 0.5876(2) 0.7366(2) 0.0554(4) H6'A 1 0.6012(2) 0.5474(2) 0.6480(2) 0.066 C7' 1 0.6747(3) 0.5099(2) 0.7889(2) 0.0722(6) H7'A 1 0.6690(3) 0.4157(2) 0.7368(2) 0.087 C8' 1 0.7240(3) 0.5658(2) 0.9195(2) 0.0850(7) H8'A 1 0.7495(3) 0.5088(2) 0.9555(2) 0.102 C9' 1 0.7353(3) 0.6984(2) 0.9934(2) 0.0725(6) H9'A 1 0.7689(3) 0.7346(2) 1.0819(2) 0.087 C9A' 1 0.6985(2) 0.7862(2) 0.9428(2) 0.0516(4) C10' 1 0.7155(2) 0.9249(2) 1.0165(2) 0.0554(4) H10B 1 0.7536(2) 0.9629(2) 1.1041(2) 0.066 C0A' 1 0.6794(2) 1.0108(2) 0.96776(15) 0.0477(4) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 C11 0.0477(9) 0.0166(7) 0.0061(6) 0.0512(9) 0.0174(7) 0.0357(7) O11 0.0516(7) 0.0320(7) 0.0127(6) 0.0945(10) 0.0462(8) 0.0648(8) O 0.0455(6) 0.0131(6) 0.0052(5) 0.0745(8) 0.0239(5) 0.0339(5) C12 0.0454(8) 0.0157(7) 0.0056(6) 0.0479(9) 0.0155(6) 0.0351(7) O12 0.0643(8) -0.0002(6) -0.0069(6) 0.0575(8) 0.0164(6) 0.0452(7) C1 0.0589(12) 0.0349(11) 0.0212(10) 0.082(2) 0.0260(11) 0.0711(13) C2 0.0766(14) 0.0341(11) 0.0144(12) 0.0641(13) 0.0180(11) 0.082(2) C3 0.0764(13) 0.0220(10) 0.0072(10) 0.0518(11) 0.0159(9) 0.0643(12) C4 0.0578(10) 0.0150(8) 0.0082(8) 0.0506(10) 0.0170(8) 0.0471(9) C4A 0.0441(8) 0.0151(7) 0.0022(6) 0.0524(9) 0.0150(7) 0.0333(7) C5 0.0430(8) 0.0158(7) 0.0035(6) 0.0531(9) 0.0183(7) 0.0330(7) C5A 0.0434(8) 0.0140(7) -0.0019(6) 0.0539(9) 0.0219(7) 0.0410(8) C6 0.0568(11) 0.0215(9) 0.0024(9) 0.0588(11) 0.0272(9) 0.0644(11) C7 0.0729(14) 0.0237(11) -0.0058(12) 0.0607(13) 0.0363(12) 0.094(2) C8 0.0631(13) 0.0071(11) -0.0115(13) 0.0712(14) 0.0590(14) 0.117(2) C9 0.0465(10) 0.0086(10) -0.0002(10) 0.0831(15) 0.0579(13) 0.094(2) C9A 0.0410(8) 0.0084(8) -0.0022(7) 0.0641(11) 0.0332(9) 0.0549(10) C10 0.0405(9) 0.0168(9) 0.0111(8) 0.0773(13) 0.0340(10) 0.0589(11) C10A 0.0438(9) 0.0179(8) 0.0063(7) 0.0638(11) 0.0208(8) 0.0445(9) C1' 0.0742(12) 0.0099(9) -0.0006(8) 0.0508(10) 0.0104(8) 0.0408(9) C2' 0.0836(14) 0.0165(9) 0.0103(10) 0.0436(10) 0.0142(8) 0.0572(11) C3' 0.0718(12) 0.0212(9) 0.0124(9) 0.0509(10) 0.0271(9) 0.0583(11) C4' 0.0542(9) 0.0168(8) 0.0075(7) 0.0518(9) 0.0213(7) 0.0408(8) C4A' 0.0430(8) 0.0114(6) 0.0064(6) 0.0444(8) 0.0158(6) 0.0340(7) C5' 0.0402(8) 0.0114(6) 0.0059(6) 0.0461(8) 0.0158(6) 0.0321(7) C5A' 0.0440(8) 0.0116(7) 0.0038(6) 0.0463(9) 0.0187(7) 0.0404(8) C6' 0.0618(11) 0.0151(8) 0.0011(8) 0.0472(9) 0.0167(8) 0.0527(10) C7' 0.0843(15) 0.0207(10) -0.0030(12) 0.0506(11) 0.0266(10) 0.0818(15) C8' 0.109(2) 0.0268(13) -0.0138(14) 0.0671(14) 0.0450(13) 0.091(2) C9' 0.092(2) 0.0193(11) -0.0149(11) 0.0681(13) 0.0344(11) 0.0613(12) C9A' 0.0582(10) 0.0134(8) -0.0013(7) 0.0524(10) 0.0229(8) 0.0446(9) C10' 0.0648(11) 0.0108(9) -0.0047(7) 0.0588(11) 0.0176(8) 0.0354(8) C0A' 0.0536(9) 0.0096(7) 0.0018(7) 0.0470(9) 0.0149(7) 0.0363(8)