#------------------------------------------------------------------------------ #$Date: 2016-06-25 09:42:02 +0100 (Sat, 25 Jun 2016) $ #$Revision: 183932 $ #$URL: svn://www.crystallography.net/cod/cif/3/50/00/3500038.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_3500038 loop_ _publ_author_name 'Armel Le Bail' _journal_name_full 'Personal communication to COD' _journal_year 2016 _chemical_formula_sum 'C4 H4 Ca O6' _chemical_formula_weight 188.149 _chemical_name_systematic ; Calcium tartrate anhydrous form II ; _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 geom _atom_sites_solution_primary direct _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 7.618(8) _cell_length_b 9.945(16) _cell_length_c 7.219(4) _cell_measurement_temperature 293(2) _cell_volume 546.9(11) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0726 _diffrn_reflns_av_sigmaI/netI 0.0850 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 757 _diffrn_reflns_theta_full 27.33 _diffrn_reflns_theta_max 27.33 _diffrn_reflns_theta_min 3.37 _exptl_absorpt_coefficient_mu 1.103 _exptl_crystal_density_diffrn 2.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 376 _exptl_special_details ; Synthesis: Acide tartrique : 3.10-3 mole soit 0.4503 g NaOH (6 mol/L, soit 12 g dans 50 mL) : 3.10-3 mole soit 1 mL CaCl2.2H2O : 3.10-3 mole soit 0.4410 g 15 mL Eau X-ray measurement october 2008 Unpublished ; _refine_diff_density_max 0.669 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.123 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(14) _refine_ls_extinction_coef 0.002(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 56 _refine_ls_number_reflns 624 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.148 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0532 _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^)+(0.0539P)^2^+1.1037P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1162 _refine_ls_wR_factor_ref 0.1342 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _reflns_number_gt 484 _reflns_number_total 624 _reflns_threshold_expression >2sigma(I) _cod_data_source_file vmmw65f.cif _cod_data_source_block vmmw65f _cod_database_code 3500038 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 _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca Ca 1.5000 0.58868(16) 0.7500 0.0115(4) Uani 1 2 d S . . O1 O 1.4316(6) 0.3684(4) 0.5743(6) 0.0143(10) Uani 1 1 d . . . O2 O 1.6875(6) 0.7864(4) 0.7022(6) 0.0169(12) Uani 1 1 d . . . O3 O 1.1991(6) 0.5424(4) 0.7987(6) 0.0173(12) Uani 1 1 d D . . H3 H 1.170(8) 0.456(2) 0.779(11) 0.017(18) Uiso 1 1 d D . . C1 C 1.8430(8) 0.7760(6) 0.6481(8) 0.0125(13) Uani 1 1 d . . . C2 C 1.0676(8) 0.6400(6) 0.8302(9) 0.0124(12) Uani 1 1 d . . . H2 H 1.0066 0.6182 0.9458 0.015 Uiso 1 1 calc R . . 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 Ca 0.0117(7) 0.0088(7) 0.0138(8) 0.000 -0.0001(10) 0.000 O1 0.021(2) 0.0083(19) 0.014(2) 0.0023(16) 0.0032(18) -0.0045(17) O2 0.015(2) 0.009(2) 0.028(3) 0.0034(18) 0.0044(19) -0.0019(18) O3 0.009(2) 0.0103(19) 0.033(3) -0.0044(18) 0.0003(19) 0.0016(16) C1 0.018(3) 0.011(3) 0.008(3) -0.004(2) -0.001(2) 0.002(3) C2 0.013(3) 0.010(3) 0.014(3) 0.002(2) 0.001(3) 0.002(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ca Ca 0.2030 0.3060 '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' 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' 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 O3 Ca O3 157.5(2) . 4_856 O3 Ca O1 95.66(16) . 2_865 O3 Ca O1 88.26(16) 4_856 2_865 O3 Ca O1 88.26(16) . 3_566 O3 Ca O1 95.66(16) 4_856 3_566 O1 Ca O1 159.8(2) 2_865 3_566 O3 Ca O2 137.82(16) . . O3 Ca O2 64.59(16) 4_856 . O1 Ca O2 82.55(15) 2_865 . O1 Ca O2 81.31(15) 3_566 . O3 Ca O2 64.59(16) . 4_856 O3 Ca O2 137.82(16) 4_856 4_856 O1 Ca O2 81.31(15) 2_865 4_856 O1 Ca O2 82.55(15) 3_566 4_856 O2 Ca O2 73.5(2) . 4_856 O3 Ca O1 73.29(15) . . O3 Ca O1 87.55(16) 4_856 . O1 Ca O1 131.55(13) 2_865 . O1 Ca O1 68.51(18) 3_566 . O2 Ca O1 136.65(15) . . O2 Ca O1 129.10(16) 4_856 . O3 Ca O1 87.55(16) . 4_856 O3 Ca O1 73.29(15) 4_856 4_856 O1 Ca O1 68.51(18) 2_865 4_856 O1 Ca O1 131.55(13) 3_566 4_856 O2 Ca O1 129.10(16) . 4_856 O2 Ca O1 136.65(15) 4_856 4_856 O1 Ca O1 64.1(2) . 4_856 C1 O1 O2 27.2(3) 5_445 5_445 C1 O1 C2 34.9(3) 5_445 8_746 O2 O1 C2 62.1(2) 5_445 8_746 C1 O1 Ca 130.5(4) 5_445 2_864 O2 O1 Ca 129.8(2) 5_445 2_864 C2 O1 Ca 116.5(2) 8_746 2_864 C1 O1 Ca 121.3(4) 5_445 . O2 O1 Ca 105.9(2) 5_445 . C2 O1 Ca 131.9(3) 8_746 . Ca O1 Ca 106.27(16) 2_864 . C1 O1 O1 79.2(3) 5_445 4_856 O2 O1 O1 86.2(2) 5_445 4_856 C2 O1 O1 74.35(18) 8_746 4_856 Ca O1 O1 143.9(3) 2_864 4_856 Ca O1 O1 57.95(11) . 4_856 C1 O1 O1 146.7(4) 5_445 3_566 O2 O1 O1 119.69(18) 5_445 3_566 C2 O1 O1 174.6(3) 8_746 3_566 Ca O1 O1 58.23(16) 2_864 3_566 Ca O1 O1 53.25(16) . 3_566 O1 O1 O1 110.53(16) 4_856 3_566 C1 O1 O3 82.8(4) 5_445 . O2 O1 O3 59.22(19) 5_445 . C2 O1 O3 113.7(3) 8_746 . Ca O1 O3 123.5(2) 2_864 . Ca O1 O3 49.93(13) . . O1 O1 O3 73.79(18) 4_856 . O1 O1 O3 70.52(18) 3_566 . C1 O1 O2 103.9(4) 5_445 3_566 O2 O1 O2 126.3(2) 5_445 3_566 C2 O1 O2 73.6(2) 8_746 3_566 Ca O1 O2 49.60(12) 2_864 3_566 Ca O1 O2 126.42(18) . 3_566 O1 O1 O2 110.3(2) 4_856 3_566 O1 O1 O2 102.10(19) 3_566 3_566 O3 O1 O2 172.59(19) . 3_566 C1 O1 O2 81.6(3) 5_445 2_864 O2 O1 O2 86.31(16) 5_445 2_864 C2 O1 O2 77.6(2) 8_746 2_864 Ca O1 O2 48.97(12) 2_864 2_864 Ca O1 O2 150.43(18) . 2_864 O1 O1 O2 151.29(12) 4_856 2_864 O1 O1 O2 97.2(2) 3_566 2_864 O3 O1 O2 124.5(2) . 2_864 O2 O1 O2 54.55(17) 3_566 2_864 C1 O2 O1 27.4(3) . 5 C1 O2 C2 34.5(3) . 4_856 O1 O2 C2 61.9(2) 5 4_856 C1 O2 Ca 121.9(4) . . O1 O2 Ca 146.7(2) 5 . C2 O2 Ca 88.9(2) 4_856 . C1 O2 O3 66.7(4) . 4_856 O1 O2 O3 93.7(2) 5 4_856 C2 O2 O3 32.85(19) 4_856 4_856 Ca O2 O3 56.00(15) . 4_856 C1 O2 O3 97.5(4) . 5 O1 O2 O3 74.3(2) 5 5 C2 O2 O3 126.1(3) 4_856 5 Ca O2 O3 139.0(2) . 5 O3 O2 O3 153.83(19) 4_856 5 C1 O2 O2 173.4(4) . 4_856 O1 O2 O2 155.2(2) 5 4_856 C2 O2 O2 141.79(19) 4_856 4_856 Ca O2 O2 53.23(11) . 4_856 O3 O2 O2 109.06(14) 4_856 4_856 O3 O2 O2 88.32(14) 5 4_856 C1 O2 O1 110.1(4) . 3_566 O1 O2 O1 115.30(18) 5 3_566 C2 O2 O1 97.0(2) 4_856 3_566 Ca O2 O1 49.09(11) . 3_566 O3 O2 O1 75.43(17) 4_856 3_566 O3 O2 O1 130.66(19) 5 3_566 O2 O2 O1 63.42(16) 4_856 3_566 C1 O2 O1 119.1(4) . 2_865 O1 O2 O1 138.9(2) 5 2_865 C2 O2 O1 90.6(2) 4_856 2_865 Ca O2 O1 48.47(10) . 2_865 O3 O2 O1 69.32(17) 4_856 2_865 O3 O2 O1 104.47(18) 5 2_865 O2 O2 O1 62.03(15) 4_856 2_865 O1 O2 O1 96.83(17) 3_566 2_865 C2 O3 Ca 125.3(4) . . C2 O3 C1 37.5(3) . 4_856 Ca O3 C1 88.0(2) . 4_856 C2 O3 C2 36.5(4) . 4_756 Ca O3 C2 132.4(3) . 4_756 C1 O3 C2 63.9(2) 4_856 4_756 C2 O3 O2 65.9(3) . 4_856 Ca O3 O2 59.40(14) . 4_856 C1 O3 O2 28.93(18) 4_856 4_856 C2 O3 O2 84.5(2) 4_756 4_856 C2 O3 O2 132.9(4) . 5_445 Ca O3 O2 100.44(19) . 5_445 C1 O3 O2 168.7(3) 4_856 5_445 C2 O3 O2 104.8(2) 4_756 5_445 O2 O3 O2 156.8(2) 4_856 5_445 C2 O3 O1 156.1(4) . . Ca O3 O1 56.78(14) . . C1 O3 O1 137.8(3) 4_856 . C2 O3 O1 121.5(3) 4_756 . O2 O3 O1 110.4(2) 4_856 . O2 O3 O1 46.53(15) 5_445 . C2 O3 O3 92.1(3) . 3_567 Ca O3 O3 101.36(11) . 3_567 C1 O3 O3 96.7(2) 4_856 3_567 C2 O3 O3 118.5(2) 4_756 3_567 O2 O3 O3 105.3(2) 4_856 3_567 O2 O3 O3 89.1(2) 5_445 3_567 O1 O3 O3 111.3(2) . 3_567 C2 O3 O3 49.1(3) . 4_756 Ca O3 O3 155.6(2) . 4_756 C1 O3 O3 84.54(19) 4_856 4_756 C2 O3 O3 26.02(18) 4_756 4_756 O2 O3 O3 109.04(14) 4_856 4_756 O2 O3 O3 84.71(14) 5_445 4_756 O1 O3 O3 117.4(2) . 4_756 O3 O3 O3 102.51(16) 3_567 4_756 C2 O3 H3 121(4) . . Ca O3 H3 114(4) . . C1 O3 H3 158(4) 4_856 . C2 O3 H3 97(4) 4_756 . O2 O3 H3 169(5) 4_856 . O2 O3 H3 14(4) 5_445 . O1 O3 H3 60(5) . . O3 O3 H3 83(5) 3_567 . O3 O3 H3 74(4) 4_756 . O2 C1 O1 125.4(6) . 5 O2 C1 C2 117.7(5) . 4_856 O1 C1 C2 116.9(5) 5 4_856 O2 C1 O3 84.4(4) . 4_856 O1 C1 O3 148.7(5) 5 4_856 C2 C1 O3 34.4(3) 4_856 4_856 O3 C2 C1 108.0(5) . 4_856 O3 C2 C2 110.6(5) . 4_756 C1 C2 C2 112.0(4) 4_856 4_756 O3 C2 O1 134.6(5) . 8_756 C1 C2 O1 28.2(3) 4_856 8_756 C2 C2 O1 102.6(2) 4_756 8_756 O3 C2 O2 81.3(4) . 4_856 C1 C2 O2 27.8(3) 4_856 4_856 C2 C2 O2 116.6(4) 4_756 4_856 O1 C2 O2 56.0(2) 8_756 4_856 O3 C2 O3 104.8(4) . 4_756 C1 C2 O3 140.0(4) 4_856 4_756 C2 C2 O3 32.9(3) 4_756 4_756 O1 C2 O3 119.6(3) 8_756 4_756 O2 C2 O3 149.4(3) 4_856 4_756 O3 C2 H2 108.7 . . C1 C2 H2 108.7 4_856 . C2 C2 H2 108.7 4_756 . O1 C2 H2 88.0 8_756 . O2 C2 H2 126.3 4_856 . O3 C2 H2 80.9 4_756 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ca O3 2.364(5) . Ca O3 2.364(5) 4_856 Ca O1 2.436(5) 2_865 Ca O1 2.436(5) 3_566 Ca O2 2.454(5) . Ca O2 2.454(5) 4_856 Ca O1 2.584(6) . Ca O1 2.584(5) 4_856 O1 C1 1.259(8) 5_445 O1 O2 2.231(6) 5_445 O1 C2 2.374(8) 8_746 O1 Ca 2.436(5) 2_864 O1 O1 2.743(9) 4_856 O1 O1 2.829(9) 3_566 O1 O3 2.959(7) . O1 O2 3.186(6) 3_566 O1 O2 3.226(6) 2_864 O2 C1 1.252(7) . O2 O1 2.231(6) 5 O2 C2 2.378(8) 4_856 O2 O3 2.576(7) 4_856 O2 O3 2.641(7) 5 O2 O2 2.939(9) 4_856 O2 O1 3.186(6) 3_566 O2 O1 3.226(6) 2_865 O3 C2 1.414(8) . O3 C1 2.376(8) 4_856 O3 C2 2.436(8) 4_756 O3 O2 2.576(7) 4_856 O3 O2 2.641(7) 5_445 O3 O3 3.027(9) 3_567 O3 O3 3.114(9) 4_756 O3 H3 0.898(10) . C1 O1 1.259(8) 5 C1 C2 1.522(9) 4_856 C1 O3 2.376(8) 4_856 C2 C1 1.522(9) 4_856 C2 C2 1.549(12) 4_756 C2 O1 2.374(8) 8_756 C2 O2 2.378(8) 4_856 C2 O3 2.436(8) 4_756 C2 H2 0.9800 . _cod_database_fobs_code 3500038