#------------------------------------------------------------------------------ #$Date: 2016-03-24 01:30:03 +0200 (Thu, 24 Mar 2016) $ #$Revision: 179532 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/50/01/4500164.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_4500164 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_absolute_configuration syn _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 L-tartrate' _chemical_name_systematic ; ? ; _space_group_IT_number 20 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'C 2c 2' _symmetry_space_group_name_H-M 'C 2 2 21' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary 'EDMA (van Smaalen, S. et al., 2003)' _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 5.5800(6) _cell_length_b 9.1055(6) _cell_length_c 12.0180(11) _cell_measurement_reflns_used 4035 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 2.91 _cell_volume 610.62(10) _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 0.991 _diffrn_measured_fraction_theta_max 0.991 _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 0.0750 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 3280 _diffrn_reflns_theta_full 27.64 _diffrn_reflns_theta_max 27.64 _diffrn_reflns_theta_min 3.39 _exptl_absorpt_coefficient_mu 0.162 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method 'not measured' _exptl_crystal_description sheet _exptl_crystal_F_000 164 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.264 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.074 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 61 _refine_ls_number_reflns 696 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.916 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0462 _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^)+(0.0878P)^2^+1.1217P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1193 _refine_ls_wR_factor_ref 0.1337 _reflns_number_gt 578 _reflns_number_total 696 _reflns_threshold_expression >2\s(I) _cod_data_source_file cg101170k_si_002.cif _cod_data_source_block 3-Li2LTartrate_(C2221) _cod_database_code 4500164 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, -z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, 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 O1A O 0.3004(4) 0.6905(2) 0.93429(18) 0.0166(5) Uani 1 1 d O1B O 0.1260(4) 0.4886(2) 0.86640(19) 0.0167(5) Uani 1 1 d O2 O 0.7115(4) 0.6376(2) 0.84039(19) 0.0165(5) Uani 1 1 d H2O H 0.842(8) 0.587(4) 0.854(3) 0.025 Uiso 1 1 d C1 C 0.3001(5) 0.5752(3) 0.8766(2) 0.0125(6) Uani 1 1 d C2 C 0.5286(5) 0.5349(3) 0.8134(3) 0.0145(7) Uani 1 1 d H2 H 0.578(6) 0.442(4) 0.842(3) 0.017 Uiso 1 1 d Li1 Li 0.1004(9) 0.2974(6) 0.9323(4) 0.0156(10) Uani 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 O1A 0.0164(10) 0.0165(10) 0.0167(11) -0.0021(9) 0.0008(9) -0.0023(9) O1B 0.0145(10) 0.0149(9) 0.0206(12) 0.0018(9) 0.0000(8) -0.0032(9) O2 0.0124(9) 0.0167(10) 0.0204(13) -0.0039(8) -0.0005(10) 0.0002(9) C1 0.0151(14) 0.0139(13) 0.0086(14) 0.0023(12) -0.0015(12) 0.0014(11) C2 0.0134(12) 0.0103(13) 0.0197(18) 0.0012(12) -0.0023(12) 0.0000(10) Li1 0.018(2) 0.016(2) 0.012(3) -0.0032(19) -0.002(2) -0.005(2) 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 C1 O1A Li1 114.5(3) . 5 C1 O1A Li1 119.9(3) . 3_567 Li1 O1A Li1 118.33(16) 5 3_567 C1 O1B Li1 125.9(2) . . C2 O2 Li1 113.3(2) . 5 C2 O2 H2O 107(2) . . Li1 O2 H2O 124(3) 5 . O1B C1 O1A 125.3(3) . . O1B C1 C2 116.5(2) . . O1A C1 C2 118.2(3) . . O1B C1 Li1 165.8(3) . 5 O1A C1 Li1 40.56(19) . 5 C2 C1 Li1 77.7(2) . 5 O2 C2 C1 109.1(2) . . O2 C2 C2 111.8(3) . 4_656 C1 C2 C2 108.3(3) . 4_656 O2 C2 H2 107(2) . . C1 C2 H2 106(2) . . C2 C2 H2 114(2) 4_656 . O1B Li1 O2 115.1(3) . 5_445 O1B Li1 O1A 121.7(3) . 5_445 O2 Li1 O1A 84.6(2) 5_445 5_445 O1B Li1 O1A 104.2(2) . 3_567 O2 Li1 O1A 109.2(3) 5_445 3_567 O1A Li1 O1A 120.8(3) 5_445 3_567 O1B Li1 C1 128.4(2) . 5_445 O2 Li1 C1 59.63(16) 5_445 5_445 O1A Li1 C1 24.99(12) 5_445 5_445 O1A Li1 C1 126.7(3) 3_567 5_445 O1B Li1 Li1 119.8(3) . 7_457 O2 Li1 Li1 110.6(3) 5_445 7_457 O1A Li1 Li1 31.01(8) 5_445 7_457 O1A Li1 Li1 95.3(3) 3_567 7_457 C1 Li1 Li1 53.97(14) 5_445 7_457 O1B Li1 Li1 111.9(2) . 7_557 O2 Li1 Li1 79.4(2) 5_445 7_557 O1A Li1 Li1 125.9(3) 5_445 7_557 O1A Li1 Li1 30.66(14) 3_567 7_557 C1 Li1 Li1 116.3(3) 5_445 7_557 Li1 Li1 Li1 113.2(3) 7_457 7_557 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O1A C1 1.258(4) . O1A Li1 1.936(6) 5 O1A Li1 1.956(6) 3_567 O1B C1 1.257(4) . O1B Li1 1.918(6) . O2 C2 1.422(3) . O2 Li1 1.929(6) 5 O2 H2O 0.88(5) . C1 C2 1.529(4) . C1 Li1 2.711(6) 5 C2 C2 1.556(7) 4_656 C2 H2 0.95(4) . Li1 O2 1.929(6) 5_445 Li1 O1A 1.936(6) 5_445 Li1 O1A 1.956(6) 3_567 Li1 C1 2.711(6) 5_445 Li1 Li1 3.343(6) 7_457 Li1 Li1 3.343(6) 7_557 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 0.88(5) 1.82(5) 2.699(3) 173(4) 1_655 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 Li1 O1B C1 O1A -106.8(3) . . Li1 O1B C1 C2 73.0(4) . . Li1 O1B C1 Li1 -105.3(10) . 5 Li1 O1A C1 O1B 179.5(3) 5 . Li1 O1A C1 O1B 29.8(4) 3_567 . Li1 O1A C1 C2 -0.3(4) 5 . Li1 O1A C1 C2 -149.9(3) 3_567 . Li1 O1A C1 Li1 -149.6(3) 3_567 5 Li1 O2 C2 C1 -5.8(3) 5 . Li1 O2 C2 C2 114.1(3) 5 4_656 O1B C1 C2 O2 -175.7(2) . . O1A C1 C2 O2 4.0(4) . . Li1 C1 C2 O2 3.9(2) 5 . O1B C1 C2 C2 62.4(3) . 4_656 O1A C1 C2 C2 -117.9(2) . 4_656 Li1 C1 C2 C2 -118.06(15) 5 4_656 C1 O1B Li1 O2 -92.4(3) . 5_445 C1 O1B Li1 O1A 168.0(3) . 5_445 C1 O1B Li1 O1A 27.0(4) . 3_567 C1 O1B Li1 C1 -162.5(3) . 5_445 C1 O1B Li1 Li1 131.8(3) . 7_457 C1 O1B Li1 Li1 -4.2(4) . 7_557