#------------------------------------------------------------------------------ #$Date: 2008-01-26 17:25:03 +0000 (Sat, 26 Jan 2008) $ #$Revision: 20 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003230.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_2003230 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 454 _journal_page_last 458 _publ_section_title ; Ligands for Application in Coordination Chemistry: Structures of Three Dicarboxylic Acids ; _chemical_formula_moiety 'C20 H30 O8 ' _chemical_formula_sum 'C20 H30 O8 ' _chemical_formula_weight 398.45 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y,1/2+z x,-y,1/2-z 1/2+x,1/2-y,z 1/2-x,1/2+y,-z 1/2-x,1/2-y,1/2+z 1/2+x,1/2+y,1/2-z _symmetry_space_group_name_H-M 'P c a n' _cell_length_a 11.321(3) _cell_length_b 10.782(2) _cell_length_c 17.916(4) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 2186.9(8) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_wavelength 0.71067 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.00 _cell_measurement_theta_max 18.00 _exptl_absorpt_coefficient_mu 0.09 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_size_rad ? _exptl_crystal_colour colorless _chemical_compound_source 'synthesised by the authors' _diffrn_measurement_device 'Nonius CAD-4 ' _diffrn_measurement_method '\q/2\q scan b/P/b ' _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0000 _diffrn_reflns_number 3344 _reflns_number_total 1714 _reflns_number_observed 955 _reflns_observed_criterion 'Inet > 3.0\s(Inet)' _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_theta_max 23.93 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% '1.0' _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.071 _refine_ls_wR_factor_obs 0.082 _refine_ls_wR_factor_all 0.088 _refine_ls_goodness_of_fit_obs 2.04 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 955 _refine_ls_number_parameters 131 _refine_ls_hydrogen_treatment ; Hydroxyl H atoms refined isotropically, others riding (C-H 0.95 \%A) ; _refine_ls_weighting_scheme '1/[\s^2^(F) + 0.0010F^2^]' _refine_ls_shift/esd_max 0.001 _refine_diff_density_max 0.28 _refine_diff_density_min -0.30 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C ? 'International Tables Vol. IV Table 2.2B' 0.002 0.002 H ? 'International Tables Vol. IV Table 2.2B' 0.000 0.000 O ? 'International Tables Vol. IV Table 2.2B' 0.008 0.006 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv O1 0.4159(3) 0.4709(3) 0.0832(2) 0.086(2) O2 0.4078(3) 0.6179(3) 0.0000(2) 0.089(2) C1 0.3739(4) 0.5758(4) 0.0590(3) 0.056(2) C2 0.2865(4) 0.6385(3) 0.1094(2) 0.060(2) C21 0.2224(5) 0.7430(5) 0.0670(3) 0.088(3) C22 0.3533(5) 0.6921(5) 0.1751(3) 0.095(4) C3 0.1979(4) 0.5455(4) 0.1387(3) 0.075(3) O4 0.1414(4) 0.4907(3) 0.07598(19) 0.092(2) C5 0.0805(6) 0.3775(5) 0.0928(4) 0.122(5) C6 -0.0431(5) 0.3941(4) 0.1140(3) 0.088(3) O7 -0.0477(3) 0.4482(3) 0.18594(16) 0.0691(18) C11 -0.1559(4) 0.4720(3) 0.2155(2) 0.054(2) C12 -0.2612(4) 0.4437(4) 0.1814(3) 0.076(3) C13 -0.3666(5) 0.4719(6) 0.2155(3) 0.103(4) H1 0.474(5) 0.444(6) 0.042(3) 0.12(2) H21C 0.279 0.801 0.049 0.0985 H21A 0.180 0.709 0.026 0.0985 H21B 0.169 0.784 0.100 0.0985 H22C 0.409 0.751 0.158 0.1049 H22A 0.299 0.732 0.208 0.1049 H22B 0.393 0.627 0.201 0.1049 H3A 0.141 0.586 0.169 0.0851 H3B 0.237 0.484 0.167 0.0851 H5A 0.083 0.326 0.050 0.1317 H5B 0.120 0.338 0.133 0.1317 H6A -0.082 0.316 0.115 0.0981 H6B -0.081 0.447 0.079 0.0981 H12 -0.261 0.404 0.134 0.0858 H13 -0.439 0.453 0.192 0.1130 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 O1 0.112(3) 0.028(2) 0.023(2) 0.057(2) 0.0174(17) 0.089(2) O2 0.120(3) 0.0285(19) 0.041(2) 0.0508(18) 0.0205(18) 0.097(2) C1 0.066(3) -0.000(2) 0.004(2) 0.037(2) 0.003(2) 0.065(3) C2 0.070(3) 0.002(2) 0.007(2) 0.040(2) -0.007(2) 0.070(3) C21 0.086(4) 0.019(3) 0.023(3) 0.063(3) 0.003(3) 0.116(4) C22 0.097(4) 0.000(3) 0.002(3) 0.074(3) -0.035(3) 0.113(4) C3 0.094(3) -0.005(3) 0.016(3) 0.069(3) -0.013(2) 0.063(3) O4 0.112(3) -0.041(2) 0.027(2) 0.083(2) -0.0264(18) 0.082(2) C5 0.141(6) -0.044(4) 0.067(4) 0.075(4) -0.061(4) 0.150(6) C6 0.110(4) -0.031(3) 0.027(3) 0.065(3) -0.029(3) 0.089(4) O7 0.076(2) -0.0089(16) 0.0075(16) 0.0582(18) -0.0137(16) 0.073(2) C11 0.055(2) -0.002(2) 0.004(2) 0.041(2) 0.0109(19) 0.067(2) C12 0.076(4) -0.012(3) -0.009(3) 0.070(3) 0.010(3) 0.081(3) C13 0.069(3) -0.014(4) -0.010(3) 0.125(5) 0.017(4) 0.114(5)