#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003232.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_2003232 _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 'C15 H28 O6 ' _chemical_formula_sum 'C15 H28 O6 ' _chemical_formula_weight 304.38 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _symmetry_space_group_name_H-M 'P -1' _cell_length_a 5.765(2) _cell_length_b 11.951(2) _cell_length_c 13.325(2) _cell_angle_alpha 98.17(2) _cell_angle_beta 91.71(2) _cell_angle_gamma 101.48(2) _cell_volume 889.0(3) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.137 _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 9.00 _cell_measurement_theta_max 20.00 _exptl_absorpt_coefficient_mu 0.08 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_size_rad ? _exptl_crystal_colour colorless _chemical_compound_source 'synthesised by the authors' _diffrn_measurement_device 'Enraf 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 3866 _reflns_number_total 3866 _reflns_number_observed 2008 _reflns_observed_criterion 'Inet > 3.0\s(Inet)' _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_max 26.90 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% '1.0' _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.040 _refine_ls_wR_factor_obs 0.057 _refine_ls_wR_factor_all 0.065 _refine_ls_goodness_of_fit_obs 1.55 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 2008 _refine_ls_number_parameters 199 _refine_ls_hydrogen_treatment ; Hydroxyl H atoms refined isotropically, others riding (C-H 0.95 \%A) ; _refine_ls_weighting_scheme '1/[\s^2^(F) + 0.0008F^2^]' _refine_ls_shift/esd_max 0.008 _refine_diff_density_max 0.20 _refine_diff_density_min -0.13 _refine_ls_extinction_method 'Larson (1970)' _refine_ls_extinction_coef 1.5E3(9) 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 0.9480(3) 0.30937(15) 0.08673(12) 0.0751(10) O2 1.3350(3) 0.37190(15) 0.10601(13) 0.0837(11) C1 1.1359(4) 0.38058(17) 0.12883(15) 0.0508(11) C2 1.0872(4) 0.47917(16) 0.20541(14) 0.0515(11) C21 0.9584(5) 0.5544(2) 0.1488(2) 0.0767(18) C22 1.3203(5) 0.5501(2) 0.2576(2) 0.0704(14) C3 0.9265(4) 0.42770(18) 0.28290(15) 0.0538(11) O4 1.0474(2) 0.35808(12) 0.33298(11) 0.0577(9) C5 0.9153(4) 0.30244(17) 0.40600(15) 0.0513(11) C6 1.0597(4) 0.22684(16) 0.45158(14) 0.0479(11) C61 1.2895(4) 0.3004(2) 0.50456(18) 0.0667(14) C62 0.9120(5) 0.1637(2) 0.52775(17) 0.0671(15) C7 1.1238(3) 0.14002(17) 0.36721(15) 0.0498(11) O8 0.9138(2) 0.07096(12) 0.31744(10) 0.0567(8) C9 0.9547(4) -0.00265(18) 0.22991(15) 0.0531(11) C10 0.7156(3) -0.06416(16) 0.17768(14) 0.0459(10) C101 0.5622(5) -0.1298(2) 0.25027(18) 0.0679(14) C102 0.5886(4) 0.0238(2) 0.13940(17) 0.0639(14) C11 0.7579(4) -0.14781(17) 0.08726(15) 0.0533(12) O11 0.5711(3) -0.21681(18) 0.04338(15) 0.0968(13) O12 0.9569(3) -0.15011(14) 0.05777(13) 0.0820(11) H1 0.988(7) 0.250(3) 0.039(3) 0.150(13) H11 0.612(7) -0.263(4) -0.010(3) 0.173(17) H21C 1.059 0.587 0.100 0.0893 H21A 0.817 0.508 0.115 0.0893 H21B 0.922 0.615 0.196 0.0893 H22C 1.418 0.582 0.208 0.0761 H22A 1.288 0.611 0.306 0.0761 H22B 1.399 0.502 0.291 0.0761 H3A 0.784 0.382 0.250 0.0640 H3B 0.890 0.488 0.331 0.0640 H5A 0.881 0.359 0.458 0.0607 H5B 0.771 0.256 0.375 0.0607 H61C 1.378 0.252 0.532 0.0740 H61A 1.380 0.339 0.457 0.0740 H61B 1.253 0.355 0.557 0.0740 H62C 1.001 0.116 0.557 0.0775 H62A 0.873 0.219 0.580 0.0775 H62B 0.770 0.118 0.494 0.0775 H7A 1.214 0.092 0.395 0.0587 H7B 1.214 0.180 0.320 0.0587 H9A 1.045 0.041 0.185 0.0613 H9B 1.038 -0.058 0.249 0.0613 H101C 0.415 -0.167 0.216 0.0751 H101A 0.640 -0.186 0.272 0.0751 H101B 0.536 -0.077 0.307 0.0751 H102C 0.440 -0.015 0.107 0.0732 H102A 0.565 0.078 0.195 0.0732 H102B 0.683 0.063 0.093 0.0732 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 0.0702(11) -0.0034(9) 0.0081(9) 0.0683(10) -0.0277(8) 0.0683(10) O2 0.0609(11) 0.0143(9) 0.0035(9) 0.0877(12) -0.0412(10) 0.0859(12) C1 0.0577(13) 0.0075(10) 0.0026(10) 0.0460(11) -0.0022(9) 0.0445(11) C2 0.0633(13) 0.0123(10) 0.0031(10) 0.0421(10) -0.0027(9) 0.0469(11) C21 0.103(2) 0.0335(16) 0.0088(17) 0.0632(15) 0.0127(14) 0.0716(16) C22 0.0760(16) 0.0005(12) 0.0062(14) 0.0501(12) -0.0166(12) 0.0722(15) C3 0.0604(13) 0.0211(11) 0.0029(10) 0.0524(12) -0.0027(10) 0.0494(11) O4 0.0537(9) 0.0237(8) 0.0113(7) 0.0685(9) 0.0151(7) 0.0578(9) C5 0.0515(12) 0.0133(10) 0.0087(9) 0.0549(12) -0.0026(9) 0.0458(11) C6 0.0528(11) 0.0129(9) 0.0004(9) 0.0497(11) -0.0048(8) 0.0388(10) C61 0.0681(15) 0.0150(13) -0.0129(12) 0.0673(14) -0.0161(12) 0.0565(13) C62 0.0861(18) 0.0198(14) 0.0129(13) 0.0678(15) 0.0058(12) 0.0486(12) C7 0.0461(11) 0.0124(10) -0.0017(9) 0.0517(11) -0.0058(9) 0.0484(11) O8 0.0457(8) 0.0074(7) 0.0014(6) 0.0641(9) -0.0202(7) 0.0500(8) C9 0.0494(12) 0.0139(10) 0.0013(10) 0.0570(12) -0.0147(10) 0.0473(11) C10 0.0471(11) 0.0095(9) 0.0023(9) 0.0453(10) -0.0048(8) 0.0420(10) C101 0.0755(16) -0.0012(13) 0.0090(12) 0.0621(14) 0.0009(12) 0.0576(13) C102 0.0678(15) 0.0188(12) -0.0057(12) 0.0628(13) -0.0038(12) 0.0590(13) C11 0.0558(13) 0.0096(10) -0.0011(10) 0.0494(11) -0.0095(9) 0.0490(11) O11 0.0602(11) 0.0047(10) -0.0015(10) 0.1050(14) -0.0603(12) 0.0971(14) O12 0.0610(10) -0.0023(9) 0.0179(9) 0.0832(12) -0.0382(9) 0.0805(11)