#------------------------------------------------------------------------------ #$Date: 2008-01-26 18:25:03 +0100 (Sat, 26 Jan 2008) $ #$Revision: 20 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003231.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_2003231 _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 'C12 H22 O6 ' _chemical_formula_sum 'C12 H22 O6 ' _chemical_formula_weight 262.30 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 1/2-x,1/2+y,-z 1/2+x,1/2-y,z _symmetry_space_group_name_H-M 'P 21/a' _cell_length_a 12.457(3) _cell_length_b 9.828(2) _cell_length_c 12.588(2) _cell_angle_alpha 90.0 _cell_angle_beta 106.79(2) _cell_angle_gamma 90.0 _cell_volume 1475.4(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.181 _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 18.00 _exptl_absorpt_coefficient_mu 0.09 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_size_rad ? _exptl_crystal_colour colorless _chemical_compound_source 'synthesised by 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 3347 _reflns_number_total 3209 _reflns_number_observed 1511 _reflns_observed_criterion 'Inet > 3.0\s(Inet)' _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_theta_max 26.91 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% '2.0' _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.038 _refine_ls_wR_factor_obs 0.052 _refine_ls_wR_factor_all 0.061 _refine_ls_goodness_of_fit_obs 1.35 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 1511 _refine_ls_number_parameters 172 _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 0.006 _refine_diff_density_max 0.12 _refine_diff_density_min -0.11 _refine_ls_extinction_method 'Larson (1970)' _refine_ls_extinction_coef 4.4E3(15) 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 0.00869(16) -0.15882(19) 0.07014(17) 0.0744(13) O2 0.13893(14) -0.01560(18) 0.05392(16) 0.0734(12) C1 0.1121(2) -0.1220(2) 0.0900(2) 0.0514(14) C2 0.1974(2) -0.2201(2) 0.1606(2) 0.0541(14) C21 0.1905(3) -0.3551(3) 0.0974(2) 0.078(2) C22 0.3143(2) -0.1604(3) 0.1865(2) 0.0770(19) C3 0.1655(2) -0.2470(2) 0.2669(2) 0.0606(16) O4 0.16385(14) -0.12087(15) 0.31971(13) 0.0622(11) C5 0.1285(2) -0.1305(3) 0.4173(2) 0.0620(16) C6 0.1362(2) 0.0060(3) 0.4708(2) 0.0636(17) O7 0.05352(14) 0.09987(17) 0.41246(14) 0.0655(11) C8 0.0817(2) 0.1699(2) 0.3257(2) 0.0623(16) C9 -0.0049(2) 0.2824(2) 0.2840(2) 0.0548(14) C91 -0.1209(2) 0.2233(3) 0.2328(2) 0.0724(17) C92 0.0337(3) 0.3649(3) 0.1976(2) 0.0737(19) C10 -0.0043(2) 0.3750(2) 0.3802(2) 0.0530(14) O10 -0.08870(14) 0.39596(18) 0.40930(14) 0.0663(11) O11 0.08976(15) 0.4315(2) 0.42822(18) 0.0938(15) H1 -0.038(3) -0.093(4) 0.031(3) 0.153(16) H11 0.088(3) 0.492(4) 0.501(4) 0.186(17) H21C 0.210 -0.340 0.031 0.0894 H21A 0.241 -0.419 0.142 0.0894 H21B 0.116 -0.390 0.080 0.0894 H22C 0.332 -0.145 0.119 0.0870 H22A 0.317 -0.077 0.225 0.0870 H22B 0.367 -0.222 0.231 0.0870 H3A 0.219 -0.306 0.314 0.0698 H3B 0.093 -0.288 0.249 0.0698 H5A 0.053 -0.162 0.398 0.0725 H5B 0.175 -0.193 0.467 0.0725 H6A 0.208 0.043 0.476 0.0736 H6B 0.128 -0.006 0.543 0.0736 H8A 0.154 0.208 0.353 0.0751 H8B 0.081 0.109 0.267 0.0751 H91C -0.173 0.295 0.208 0.0803 H91A -0.120 0.167 0.172 0.0803 H91B -0.142 0.171 0.287 0.0803 H92C -0.018 0.436 0.170 0.0863 H92A 0.106 0.402 0.232 0.0863 H92B 0.037 0.307 0.138 0.0863 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 0.0559(12) -0.0022(10) 0.0143(10) 0.0666(12) 0.0263(11) 0.0960(14) O2 0.0607(11) -0.0003(9) 0.0212(10) 0.0679(12) 0.0304(10) 0.0910(13) C1 0.0548(16) 0.0008(12) 0.0239(12) 0.0499(14) 0.0013(12) 0.0545(14) C2 0.0566(15) 0.0097(12) 0.0191(12) 0.0500(14) 0.0023(12) 0.0573(14) C21 0.103(2) 0.0197(15) 0.0308(17) 0.0606(17) -0.0007(14) 0.0751(18) C22 0.0575(17) 0.0126(15) 0.0208(15) 0.086(2) 0.0089(17) 0.088(2) C3 0.0707(17) 0.0109(12) 0.0148(13) 0.0497(14) 0.0086(13) 0.0590(15) O4 0.0838(12) 0.0059(9) 0.0316(9) 0.0514(10) 0.0037(8) 0.0585(10) C5 0.0653(16) 0.0057(13) 0.0196(13) 0.0692(17) 0.0115(13) 0.0532(14) C6 0.0642(16) 0.0092(14) 0.0167(12) 0.0768(19) 0.0048(14) 0.0498(14) O7 0.0637(11) 0.0148(9) 0.0312(9) 0.0745(12) 0.0145(9) 0.0662(11) C8 0.0741(17) 0.0049(13) 0.0333(14) 0.0591(15) -0.0037(13) 0.0622(15) C9 0.0628(16) 0.0004(12) 0.0185(12) 0.0514(14) -0.0073(12) 0.0515(14) C91 0.0777(18) -0.0058(16) 0.0102(14) 0.0710(18) -0.0149(14) 0.0623(16) C92 0.098(2) 0.0032(15) 0.0362(16) 0.0637(17) -0.0009(14) 0.0672(17) C10 0.0502(15) 0.0012(12) 0.0138(12) 0.0546(15) -0.0052(12) 0.0536(14) O10 0.0533(10) -0.0016(9) 0.0226(9) 0.0783(12) -0.0196(9) 0.0702(11) O11 0.0596(12) -0.0234(12) 0.0319(11) 0.1243(17) -0.0637(14) 0.1027(16)