#------------------------------------------------------------------------------ #$Date: 2016-03-24 01:30:03 +0200 (Thu, 24 Mar 2016) $ #$Revision: 179532 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/50/01/4500165.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_4500165 loop_ _publ_author_name 'Yeung, Hamish H.-M.' 'Kosa, Monica' 'Parrinello, Michele' 'Forster, Paul M.' 'Cheetham, Anthony K.' _publ_section_title ; Structural Diversity and Energetics in Anhydrous Lithium Tartrates: Experimental and Computational Studies of Novel Chiral Polymorphs and Their Racemic and Meso Analogues ; _journal_issue 1 _journal_name_full 'Crystal Growth & Design' _journal_page_first 221 _journal_paper_doi 10.1021/cg101170k _journal_volume 11 _journal_year 2011 _chemical_formula_moiety '(Li 1+)2 (C4 H4 O6 2-)' _chemical_formula_sum 'C4 H4 Li2 O6' _chemical_formula_weight 161.95 _chemical_name_common 'Dilithium meso-tartrate' _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 100.474(9) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.0522(9) _cell_length_b 5.3351(8) _cell_length_c 9.8636(14) _cell_measurement_reflns_used 10520 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 2.91 _cell_volume 313.18(8) _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_molecular_graphics ; 'Ortep-3 for Windows (Farrugia, 1997), DIAMOND (Brandenburg, K., 1999) & Mercury (Macrae, C.F. et al., 2006)' ; _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution "'Superflip' (Palatinus L., Chapuis G., 2007)" _diffrn_ambient_temperature 120(2) _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 3246 _diffrn_reflns_theta_full 27.59 _diffrn_reflns_theta_max 27.59 _diffrn_reflns_theta_min 3.42 _exptl_absorpt_coefficient_mu 0.158 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_description rod _exptl_crystal_F_000 164 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.316 _refine_diff_density_min -0.263 _refine_diff_density_rms 0.073 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 62 _refine_ls_number_reflns 713 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.018 _refine_ls_R_factor_all 0.1059 _refine_ls_R_factor_gt 0.0810 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+1.1685P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1736 _refine_ls_wR_factor_ref 0.1906 _reflns_number_gt 543 _reflns_number_total 713 _reflns_threshold_expression >2\s(I) _cod_data_source_file cg101170k_si_002.cif _cod_data_source_block 4-Li2mesoTartrate _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 4500165 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags Li1 Li 1.1163(10) 0.5018(12) 0.1961(6) 0.0309(14) Uani 1 1 d . C1 C 0.7704(6) 0.7963(7) 0.0435(4) 0.0316(9) Uani 1 1 d D O1A O 0.9100(4) 0.7701(5) 0.1526(2) 0.0321(7) Uani 1 1 d . O1B O 0.7525(5) 0.6594(5) -0.0606(3) 0.0392(8) Uani 1 1 d . C2 C 0.6233(8) 1.0354(9) 0.0291(4) 0.0269(11) Uani 0.785(8) 1 d PD H2 H 0.6791 1.1606 -0.0290 0.032 Uiso 0.785(8) 1 calc PR C20 C 0.546(2) 0.929(3) 0.0651(16) 0.0269(11) Uani 0.215(8) 1 d PD H20 H 0.4377 0.8157 0.0955 0.032 Uiso 0.215(8) 1 calc PR O2 O 0.6312(6) 1.1284(7) 0.1670(3) 0.0568(11) Uani 1 1 d D H2O H 0.492(11) 1.255(12) 0.157(6) 0.085 Uiso 1 1 d . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.034(3) 0.031(3) 0.026(3) 0.000(3) 0.004(2) 0.011(3) C1 0.0326(19) 0.035(2) 0.0252(17) -0.0044(15) -0.0003(14) 0.0093(16) O1A 0.0348(14) 0.0310(14) 0.0273(13) 0.0000(11) -0.0027(10) 0.0077(11) O1B 0.0416(16) 0.0433(17) 0.0302(14) -0.0100(12) 0.0000(11) 0.0175(13) C2 0.034(3) 0.021(2) 0.025(2) -0.0040(18) 0.0029(17) 0.0043(19) C20 0.034(3) 0.021(2) 0.025(2) -0.0040(18) 0.0029(17) 0.0043(19) O2 0.057(2) 0.066(2) 0.0374(16) -0.0261(15) -0.0169(14) 0.0338(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O1B Li1 O1A 121.9(3) 3_765 . O1B Li1 O2 105.6(3) 3_765 2_745 O1A Li1 O2 107.1(3) . 2_745 O1B Li1 O1A 110.8(3) 3_765 2_745 O1A Li1 O1A 120.4(3) . 2_745 O2 Li1 O1A 81.7(2) 2_745 2_745 O1B C1 O1A 125.9(3) . . O1B C1 C2 116.4(3) . . O1A C1 C2 117.3(3) . . O1B C1 C20 115.2(6) . . O1A C1 C20 113.4(6) . . C2 C1 C20 31.6(7) . . C1 O1A Li1 126.4(3) . . C1 O1A Li1 116.6(3) . 2_755 Li1 O1A Li1 116.30(17) . 2_755 C1 O1B Li1 150.1(3) . 3_765 O2 C2 C2 107.4(5) . 3_675 O2 C2 C1 106.1(3) . . C2 C2 C1 109.5(5) 3_675 . O2 C2 H2 111.2 . . C2 C2 H2 111.2 3_675 . C1 C2 H2 111.2 . . O2 C20 C20 104.3(15) . 3_675 O2 C20 C1 102.3(9) . . C20 C20 C1 107.8(15) 3_675 . O2 C20 H20 113.8 . . C20 C20 H20 113.8 3_675 . C1 C20 H20 113.8 . . C2 O2 C20 33.7(7) . . C2 O2 Li1 114.7(3) . 2_755 C20 O2 Li1 110.4(6) . 2_755 C2 O2 H2O 104(3) . . C20 O2 H2O 103(3) . . Li1 O2 H2O 141(3) 2_755 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Li1 O1B 1.882(6) 3_765 Li1 O1A 1.897(6) . Li1 O2 1.966(7) 2_745 Li1 O1A 1.966(7) 2_745 C1 O1B 1.248(4) . C1 O1A 1.249(4) . C1 C2 1.547(5) . C1 C20 1.579(14) . O1A Li1 1.966(7) 2_755 O1B Li1 1.882(6) 3_765 C2 O2 1.441(5) . C2 C2 1.545(10) 3_675 C2 H2 0.9800 . C20 O2 1.488(13) . C20 C20 1.51(3) 3_675 C20 H20 0.9800 . O2 Li1 1.966(7) 2_755 O2 H2O 1.07(7) . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2O O1B 1.07(7) 1.67(6) 2.625(4) 146(5) 3_675 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 O1B C1 O1A Li1 -5.4(7) . . C2 C1 O1A Li1 -178.3(4) . . C20 C1 O1A Li1 147.0(8) . . O1B C1 O1A Li1 -175.8(4) . 2_755 C2 C1 O1A Li1 11.3(5) . 2_755 C20 C1 O1A Li1 -23.5(9) . 2_755 O1B Li1 O1A C1 33.6(6) 3_765 . O2 Li1 O1A C1 155.2(3) 2_745 . O1A Li1 O1A C1 -114.6(4) 2_745 . O1B Li1 O1A Li1 -155.9(4) 3_765 2_755 O2 Li1 O1A Li1 -34.4(4) 2_745 2_755 O1A Li1 O1A Li1 55.9(5) 2_745 2_755 O1A C1 O1B Li1 -51.0(9) . 3_765 C2 C1 O1B Li1 121.9(6) . 3_765 C20 C1 O1B Li1 157.0(10) . 3_765 O1B C1 C2 O2 166.7(4) . . O1A C1 C2 O2 -19.7(5) . . C20 C1 C2 O2 71.0(10) . . O1B C1 C2 C2 51.1(6) . 3_675 O1A C1 C2 C2 -135.3(5) . 3_675 C20 C1 C2 C2 -44.7(10) . 3_675 O1B C1 C20 O2 -164.1(7) . . O1A C1 C20 O2 40.5(13) . . C2 C1 C20 O2 -64.1(9) . . O1B C1 C20 C20 -54.4(17) . 3_675 O1A C1 C20 C20 150.1(12) . 3_675 C2 C1 C20 C20 45.5(13) . 3_675 C2 C2 O2 C20 46.0(11) 3_675 . C1 C2 O2 C20 -71.0(10) . . C2 C2 O2 Li1 136.0(4) 3_675 2_755 C1 C2 O2 Li1 19.0(5) . 2_755 C20 C20 O2 C2 -46.6(13) 3_675 . C1 C20 O2 C2 65.6(10) . . C20 C20 O2 Li1 -150.9(12) 3_675 2_755 C1 C20 O2 Li1 -38.7(12) . 2_755