Electronic Supplementary Material for CrystEngComm This Journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Richard Robson' 'Brendan F. Abrahams' 'Michael Moylan' 'Simon D. Orchard' _publ_contact_author_name 'Prof Richard Robson' _publ_contact_author_address ; School of Chemistry Univesity of Melbourne Swanston Street Parkville Victoria 3010 AUSTRALIA ; _publ_contact_author_email R.ROBSON@UNIMELB.EDU.AU _publ_section_title ; Channel-Containing Lanthanide Mucate Structures ; data_lab78i1a _database_code_CSD 212789 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(galactarato)dilanthanum(III)octahydrate ; _chemical_name_common tris(galactarato)dilanthanum(iii)octahydrate _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H40 La2 O32' _chemical_formula_weight 1046.32 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 10.3426(15) _cell_length_b 10.3426(15) _cell_length_c 8.9709(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 831.0(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5038 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.34 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.091 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 518 _exptl_absorpt_coefficient_mu 2.656 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.813 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; Sheldrick, G. M., SADABS ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.0 _diffrn_reflns_number 5212 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0155 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.34 _reflns_number_total 1269 _reflns_number_gt 1268 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Analysis of the diffraction data suggested that the Laue symmetry was 6/m. The structure was originally solved in the space group P-6 with disordered ligand and metal centres. The refinement was very unsatisfactory and as a consequence the crystal was solved and refined in the space group P-3 as a twinned crystal. This led to a far more satisfactory refinement. Two significant, unique peaks of electron density were found within the hexagonal channels. These were refined as the oxygen atoms of water molecules with fixed isotropic displacement parameters. The site occupancies of these two sites were refined giving a total of 1.37 water molecules per asymmetric unit. This corresponds to 8.23 water molecules per formula unit which is in good agreement with the microanalytical data. 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+0.4460P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1269 _refine_ls_number_parameters 76 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0228 _refine_ls_R_factor_gt 0.0228 _refine_ls_wR_factor_ref 0.0596 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 O3 O 0.6962(3) 0.0894(3) 0.4413(3) 0.0322(6) Uani 1 1 d . . . C3 C 0.5383(4) -0.0120(4) 0.4328(4) 0.0209(6) Uani 1 1 d . . . H3 H 0.5208 -0.1142 0.4367 0.025 Uiso 1 1 calc R . . O5 O 1.0022(13) 0.1798(14) 0.1064(10) 0.120 Uiso 0.786(18) 1 d P . . O4 O 0.9067(18) 0.0851(16) 0.6308(15) 0.120 Uiso 0.586(17) 1 d P . . O1A O 0.6486(3) 0.0822(3) 0.0795(3) 0.0235(5) Uani 1 1 d . . . O1B O 0.5196(3) -0.1587(3) 0.1384(3) 0.0256(5) Uani 1 1 d . . . C1 C 0.5548(4) -0.0251(4) 0.1573(4) 0.0194(6) Uani 1 1 d . . . La1 La 0.6667 0.3333 0.04936(3) 0.01544(10) Uani 1 3 d S . . O2 O 0.5113(4) 0.1602(3) 0.2660(3) 0.0289(6) Uani 1 1 d . . . C2 C 0.4796(4) 0.0092(4) 0.2851(4) 0.0208(7) Uani 1 1 d . . . H2 H 0.3715 -0.0587 0.2801 0.025 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 O3 0.0246(12) 0.0428(15) 0.0242(12) 0.0050(12) -0.0009(11) 0.0132(11) C3 0.0273(16) 0.0197(14) 0.0154(16) 0.0017(12) 0.0015(13) 0.0116(13) O1A 0.0286(13) 0.0212(11) 0.0221(14) 0.0027(9) 0.0054(10) 0.0135(10) O1B 0.0294(13) 0.0203(12) 0.0242(12) -0.0030(10) -0.0064(11) 0.0101(10) C1 0.0228(15) 0.0223(15) 0.0136(14) -0.0002(13) -0.0036(13) 0.0116(13) La1 0.01677(11) 0.01677(11) 0.01277(14) 0.000 0.000 0.00839(6) O2 0.0473(17) 0.0290(14) 0.0221(12) 0.0067(10) 0.0111(12) 0.0279(13) C2 0.0214(17) 0.0212(16) 0.0180(15) 0.0033(12) 0.0021(12) 0.0092(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O3 C3 1.435(4) . ? C3 C2 1.518(4) . ? C3 C3 1.529(7) 4_656 ? O1A C1 1.258(4) . ? O1A La1 2.524(3) . ? O1B C1 1.252(4) . ? O1B La1 2.516(3) 4_655 ? C1 C2 1.523(5) . ? La1 O1B 2.516(3) 4_655 ? La1 O1B 2.516(3) 5_665 ? La1 O1B 2.516(3) 6 ? La1 O1A 2.524(3) 2_655 ? La1 O1A 2.524(3) 3_665 ? La1 O2 2.586(3) 2_655 ? La1 O2 2.586(3) . ? La1 O2 2.586(3) 3_665 ? O2 C2 1.437(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 _geom_angle_publ_flag O3 C3 C2 109.4(3) . . ? O3 C3 C3 109.4(4) . 4_656 ? C2 C3 C3 112.9(3) . 4_656 ? C1 O1A La1 126.5(2) . . ? C1 O1B La1 125.3(2) . 4_655 ? O1B C1 O1A 124.7(3) . . ? O1B C1 C2 117.3(3) . . ? O1A C1 C2 118.1(3) . . ? O1B La1 O1B 80.08(10) 4_655 5_665 ? O1B La1 O1B 80.08(10) 4_655 6 ? O1B La1 O1B 80.08(10) 5_665 6 ? O1B La1 O1A 72.34(9) 4_655 . ? O1B La1 O1A 73.03(8) 5_665 . ? O1B La1 O1A 144.11(9) 6 . ? O1B La1 O1A 144.11(9) 4_655 2_655 ? O1B La1 O1A 72.34(9) 5_665 2_655 ? O1B La1 O1A 73.03(8) 6 2_655 ? O1A La1 O1A 118.87(2) . 2_655 ? O1B La1 O1A 73.03(8) 4_655 3_665 ? O1B La1 O1A 144.11(9) 5_665 3_665 ? O1B La1 O1A 72.34(9) 6 3_665 ? O1A La1 O1A 118.87(2) . 3_665 ? O1A La1 O1A 118.87(2) 2_655 3_665 ? O1B La1 O2 143.95(9) 4_655 2_655 ? O1B La1 O2 91.06(9) 5_665 2_655 ? O1B La1 O2 133.03(9) 6 2_655 ? O1A La1 O2 71.65(9) . 2_655 ? O1A La1 O2 60.41(8) 2_655 2_655 ? O1A La1 O2 124.57(9) 3_665 2_655 ? O1B La1 O2 91.06(9) 4_655 . ? O1B La1 O2 133.03(9) 5_665 . ? O1B La1 O2 143.95(9) 6 . ? O1A La1 O2 60.41(8) . . ? O1A La1 O2 124.57(9) 2_655 . ? O1A La1 O2 71.65(9) 3_665 . ? O2 La1 O2 69.69(11) 2_655 . ? O1B La1 O2 133.03(9) 4_655 3_665 ? O1B La1 O2 143.95(9) 5_665 3_665 ? O1B La1 O2 91.06(9) 6 3_665 ? O1A La1 O2 124.57(9) . 3_665 ? O1A La1 O2 71.65(9) 2_655 3_665 ? O1A La1 O2 60.41(8) 3_665 3_665 ? O2 La1 O2 69.69(11) 2_655 3_665 ? O2 La1 O2 69.69(11) . 3_665 ? C2 O2 La1 124.6(2) . . ? O2 C2 C3 111.7(3) . . ? O2 C2 C1 107.3(3) . . ? C3 C2 C1 109.7(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.34 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.973 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.115 #===END data_ceb78j1a _database_code_CSD 212790 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(galactarato)dicerium(III)octahydrate ; _chemical_name_common tris(galactarato)dicerium(iii)octahydrate _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H40 Ce2 O32' _chemical_formula_weight 1048.74 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 10.2880(15) _cell_length_b 10.2880(15) _cell_length_c 8.9427(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 819.7(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4824 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.49 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 2.863 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.870 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; Sheldrick, G. M., SADABS ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5183 _diffrn_reflns_av_R_equivalents 0.0160 _diffrn_reflns_av_sigmaI/netI 0.0138 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1272 _reflns_number_gt 1269 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Analysis of the diffraction data suggested that the Laue symmetry was 6/m. The structure was originally solved in the space group P-6 with disordered ligand and metal centres. The refinement was very unsatisfactory and as a consequence the crystal was solved and refined in the space group P-3 as a twinned crystal. This led to a far more satisfactory refinement. Three significant, unique peaks of electron density were found within the hexagonal channels. These were refined as the oxygen atoms of water molecules with a common isotropic displacement parameter (which was also refined). The two highest peaks were closer than would be expected on the basis of a normal hydrogen bonding interaction and accordingly they were refined such that the sum of their site occupancies was 1. The site occupancy of the third oxygen atom was refined. The sum of the site occupancies of these three sites was 1.22 water molecules per asymmetric unit. This corresponds to 7.32 water molecules per formula unit which is in good agreement with the microanalytical data. 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+0.4725P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1272 _refine_ls_number_parameters 82 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_gt 0.0229 _refine_ls_wR_factor_ref 0.0596 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 O3 O 0.6965(3) 0.6076(3) 0.4409(3) 0.0318(6) Uani 1 1 d . . . O1A O 0.6491(3) 0.5663(3) 0.0782(3) 0.0232(5) Uani 1 1 d . . . O1B O 0.5187(3) 0.6782(3) 0.1371(3) 0.0248(6) Uani 1 1 d . . . C1 C 0.5545(4) 0.5798(4) 0.1562(4) 0.0186(6) Uani 1 1 d . . . O4 O 0.8211(16) 0.8204(16) -0.1035(12) 0.105(3) Uiso 0.630(12) 1 d P . . O5 O 0.899(3) 0.817(2) 0.643(2) 0.105(3) Uiso 0.370(12) 1 d P . . O6 O 0.850(4) 0.881(4) 0.589(4) 0.105(3) Uiso 0.216(18) 1 d P . . Ce1 Ce 0.6667 0.3333 0.04988(3) 0.01498(10) Uani 1 3 d S . . O2 O 0.5120(4) 0.3510(3) 0.2654(3) 0.0284(6) Uani 1 1 d . . . C3 C 0.5381(4) 0.5503(4) 0.4334(4) 0.0203(6) Uani 1 1 d . . . H3 H 0.5201 0.6352 0.4376 0.036(13) Uiso 1 1 calc R . . C2 C 0.4790(4) 0.4701(4) 0.2844(4) 0.0196(7) Uani 1 1 d . . . H2 H 0.3702 0.4291 0.2793 0.043(16) 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 O3 0.0241(13) 0.0396(15) 0.0242(13) -0.0046(13) -0.0006(12) 0.0103(11) O1A 0.0279(13) 0.0232(12) 0.0225(15) 0.0012(10) 0.0048(10) 0.0158(11) O1B 0.0268(13) 0.0290(13) 0.0247(13) -0.0025(11) -0.0059(11) 0.0185(12) C1 0.0213(15) 0.0216(16) 0.0136(14) -0.0016(14) -0.0029(13) 0.0114(13) Ce1 0.01619(11) 0.01619(11) 0.01257(14) 0.000 0.000 0.00809(6) O2 0.0465(17) 0.0203(13) 0.0216(13) 0.0030(11) 0.0109(12) 0.0192(12) C3 0.0275(16) 0.0221(15) 0.0146(16) -0.0004(13) 0.0023(14) 0.0148(13) C2 0.0211(17) 0.0231(18) 0.0161(15) 0.0004(12) 0.0022(12) 0.0123(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O3 C3 1.431(4) . ? O1A C1 1.260(4) . ? O1A Ce1 2.505(3) . ? O1B C1 1.250(4) . ? O1B Ce1 2.494(3) 4_665 ? C1 C2 1.522(5) . ? O5 O6 1.13(4) . ? Ce1 O1B 2.494(3) 5 ? Ce1 O1B 2.494(3) 6_655 ? Ce1 O1B 2.494(3) 4_665 ? Ce1 O1A 2.505(3) 3_665 ? Ce1 O1A 2.505(3) 2_655 ? Ce1 O2 2.563(3) 3_665 ? Ce1 O2 2.563(3) 2_655 ? Ce1 O2 2.563(3) . ? O2 C2 1.435(5) . ? C3 C3 1.515(7) 4_666 ? C3 C2 1.525(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 _geom_angle_publ_flag C1 O1A Ce1 126.2(2) . . ? C1 O1B Ce1 125.5(2) . 4_665 ? O1B C1 O1A 124.8(3) . . ? O1B C1 C2 117.1(3) . . ? O1A C1 C2 118.1(3) . . ? O1B Ce1 O1B 79.99(11) 5 6_655 ? O1B Ce1 O1B 79.99(11) 5 4_665 ? O1B Ce1 O1B 79.99(11) 6_655 4_665 ? O1B Ce1 O1A 72.75(9) 5 3_665 ? O1B Ce1 O1A 72.18(9) 6_655 3_665 ? O1B Ce1 O1A 143.72(9) 4_665 3_665 ? O1B Ce1 O1A 72.18(9) 5 2_655 ? O1B Ce1 O1A 143.72(9) 6_655 2_655 ? O1B Ce1 O1A 72.75(9) 4_665 2_655 ? O1A Ce1 O1A 118.99(2) 3_665 2_655 ? O1B Ce1 O1A 143.72(9) 5 . ? O1B Ce1 O1A 72.75(9) 6_655 . ? O1B Ce1 O1A 72.18(9) 4_665 . ? O1A Ce1 O1A 118.99(2) 3_665 . ? O1A Ce1 O1A 118.99(2) 2_655 . ? O1B Ce1 O2 133.09(10) 5 3_665 ? O1B Ce1 O2 91.16(10) 6_655 3_665 ? O1B Ce1 O2 143.97(10) 4_665 3_665 ? O1A Ce1 O2 60.76(9) 3_665 3_665 ? O1A Ce1 O2 124.87(10) 2_655 3_665 ? O1A Ce1 O2 71.85(9) . 3_665 ? O1B Ce1 O2 91.16(10) 5 2_655 ? O1B Ce1 O2 143.97(10) 6_655 2_655 ? O1B Ce1 O2 133.08(10) 4_665 2_655 ? O1A Ce1 O2 71.85(9) 3_665 2_655 ? O1A Ce1 O2 60.76(9) 2_655 2_655 ? O1A Ce1 O2 124.87(10) . 2_655 ? O2 Ce1 O2 69.62(12) 3_665 2_655 ? O1B Ce1 O2 143.97(10) 5 . ? O1B Ce1 O2 133.08(10) 6_655 . ? O1B Ce1 O2 91.16(10) 4_665 . ? O1A Ce1 O2 124.87(10) 3_665 . ? O1A Ce1 O2 71.85(9) 2_655 . ? O1A Ce1 O2 60.76(9) . . ? O2 Ce1 O2 69.62(12) 3_665 . ? O2 Ce1 O2 69.62(12) 2_655 . ? C2 O2 Ce1 124.7(2) . . ? O3 C3 C3 109.8(4) . 4_666 ? O3 C3 C2 109.1(3) . . ? C3 C3 C2 112.8(4) 4_666 . ? O2 C2 C1 107.0(3) . . ? O2 C2 C3 111.4(3) . . ? C1 C2 C3 109.8(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.710 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.125 #===END data_prb77d1a _database_code_CSD 212791 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(galactarato)dipraseodymium(III)octahydrate ; _chemical_name_common tris(galactarato)dipraseodymium(iii)octahydrate _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H40 O32 Pr2' _chemical_formula_weight 1050.32 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 10.2182(14) _cell_length_b 10.2182(14) _cell_length_c 8.9084(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 805.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2221 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 25.62 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 522 _exptl_absorpt_coefficient_mu 3.112 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.854 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; Sheldrick, G. M., SADABS ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5121 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 27.52 _reflns_number_total 1230 _reflns_number_gt 1222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Analysis of the diffraction data suggested that the Laue symmetry was 6/m. The structure was originally solved in the space group P-6 with disordered ligand and metal centres. The refinement was very unsatisfactory and as a consequence the crystal was solved and refined in the space group P-3 as a twinned crystal. This led to a far more satisfactory refinement. Three significant, unique peaks of electron density were found within the hexagonal channels. These were refined as the oxygen atoms of water molecules with a common isotropic displacement parameter (which was also refined). The two highest peaks were closer than would be expected on the basis of a normal hydrogen bonding interaction and accordingly they were refined such that the sum of their site occupancies was 1. The site occupancy of the third oxygen atom was refined. The sum of the site occupancies of these three sites was 1.43 water molecules per asymmetric unit. This corresponds to 8.58 water molecules per formula unit, which is in good agreement with the microanalytical data. 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1230 _refine_ls_number_parameters 82 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0773 _refine_ls_wR_factor_gt 0.0773 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 O4 O 0.814(3) -0.022(4) -0.069(4) 0.129(7) Uiso 0.46(2) 1 d P . . O5 O 0.907(3) 0.081(3) 0.637(2) 0.129(7) Uiso 0.54(2) 1 d P . . O6 O 0.830(4) 0.017(4) -0.140(5) 0.129(7) Uiso 0.43(5) 1 d P . . O3 O 0.6976(4) 0.0875(5) 0.4395(5) 0.0308(9) Uani 1 1 d . . . C3 C 0.5373(6) -0.0133(6) 0.4327(7) 0.0216(10) Uani 1 1 d . . . H3 H 0.5179 -0.1173 0.4370 0.021(14) Uiso 1 1 calc R . . O1A O 0.6501(4) 0.0842(4) 0.0774(4) 0.0213(8) Uani 1 1 d . . . O1B O 0.5178(5) -0.1597(4) 0.1329(5) 0.0232(8) Uani 1 1 d . . . C1 C 0.5542(6) -0.0250(6) 0.1551(6) 0.0186(10) Uani 1 1 d . . . Pr1 Pr 0.6667 0.3333 0.05196(5) 0.01315(14) Uani 1 3 d S . . O2 O 0.5117(6) 0.1625(5) 0.2647(5) 0.0273(10) Uani 1 1 d . . . C2 C 0.4777(7) 0.0090(7) 0.2834(5) 0.0189(11) Uani 1 1 d . . . H2 H 0.3682 -0.0591 0.2780 0.04(2) 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 O3 0.0225(18) 0.043(2) 0.0228(19) 0.0044(18) -0.0009(19) 0.0132(17) C3 0.026(2) 0.019(2) 0.020(3) 0.001(2) 0.002(2) 0.012(2) O1A 0.0248(19) 0.0209(18) 0.017(2) 0.0029(14) 0.0035(14) 0.0108(15) O1B 0.023(2) 0.0164(19) 0.024(2) -0.0010(15) -0.0057(15) 0.0044(15) C1 0.022(2) 0.021(2) 0.012(2) -0.001(2) -0.004(2) 0.010(2) Pr1 0.01418(15) 0.01418(15) 0.01110(19) 0.000 0.000 0.00709(8) O2 0.047(3) 0.025(2) 0.0184(18) 0.0073(15) 0.0076(17) 0.025(2) C2 0.021(3) 0.020(2) 0.015(2) 0.0011(19) 0.0021(19) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O4 O6 0.72(5) . ? O3 C3 1.435(6) . ? C3 C3 1.516(11) 4_656 ? C3 C2 1.527(7) . ? O1A C1 1.261(6) . ? O1A Pr1 2.476(4) . ? O1B C1 1.249(6) . ? O1B Pr1 2.463(4) 4_655 ? C1 C2 1.520(8) . ? Pr1 O1B 2.463(4) 5_665 ? Pr1 O1B 2.463(4) 4_655 ? Pr1 O1B 2.463(4) 6 ? Pr1 O1A 2.476(4) 2_655 ? Pr1 O1A 2.476(4) 3_665 ? Pr1 O2 2.526(4) 2_655 ? Pr1 O2 2.526(4) . ? Pr1 O2 2.526(4) 3_665 ? O2 C2 1.437(7) . ? 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 _geom_angle_publ_flag O3 C3 C3 109.5(6) . 4_656 ? O3 C3 C2 109.1(4) . . ? C3 C3 C2 112.8(5) 4_656 . ? C1 O1A Pr1 125.7(3) . . ? C1 O1B Pr1 126.7(3) . 4_655 ? O1B C1 O1A 124.0(5) . . ? O1B C1 C2 117.9(5) . . ? O1A C1 C2 118.1(4) . . ? O1B Pr1 O1B 80.19(15) 5_665 4_655 ? O1B Pr1 O1B 80.19(15) 5_665 6 ? O1B Pr1 O1B 80.19(15) 4_655 6 ? O1B Pr1 O1A 72.26(13) 5_665 . ? O1B Pr1 O1A 71.72(13) 4_655 . ? O1B Pr1 O1A 143.29(14) 6 . ? O1B Pr1 O1A 71.72(13) 5_665 2_655 ? O1B Pr1 O1A 143.29(14) 4_655 2_655 ? O1B Pr1 O1A 72.26(13) 6 2_655 ? O1A Pr1 O1A 119.17(3) . 2_655 ? O1B Pr1 O1A 143.29(14) 5_665 3_665 ? O1B Pr1 O1A 72.26(13) 4_655 3_665 ? O1B Pr1 O1A 71.72(13) 6 3_665 ? O1A Pr1 O1A 119.17(3) . 3_665 ? O1A Pr1 O1A 119.17(3) 2_655 3_665 ? O1B Pr1 O2 90.82(13) 5_665 2_655 ? O1B Pr1 O2 143.41(15) 4_655 2_655 ? O1B Pr1 O2 133.42(15) 6 2_655 ? O1A Pr1 O2 71.76(14) . 2_655 ? O1A Pr1 O2 61.58(13) 2_655 2_655 ? O1A Pr1 O2 125.67(14) 3_665 2_655 ? O1B Pr1 O2 133.42(15) 5_665 . ? O1B Pr1 O2 90.82(13) 4_655 . ? O1B Pr1 O2 143.41(15) 6 . ? O1A Pr1 O2 61.58(13) . . ? O1A Pr1 O2 125.67(14) 2_655 . ? O1A Pr1 O2 71.76(14) 3_665 . ? O2 Pr1 O2 69.87(17) 2_655 . ? O1B Pr1 O2 143.41(15) 5_665 3_665 ? O1B Pr1 O2 133.42(15) 4_655 3_665 ? O1B Pr1 O2 90.82(13) 6 3_665 ? O1A Pr1 O2 125.67(14) . 3_665 ? O1A Pr1 O2 71.76(14) 2_655 3_665 ? O1A Pr1 O2 61.58(13) 3_665 3_665 ? O2 Pr1 O2 69.87(17) 2_655 3_665 ? O2 Pr1 O2 69.87(17) . 3_665 ? C2 O2 Pr1 124.5(3) . . ? O2 C2 C1 106.9(4) . . ? O2 C2 C3 111.5(4) . . ? C1 C2 C3 109.4(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 3.700 _refine_diff_density_min -0.801 _refine_diff_density_rms 0.166 #===END data_ndb78kha _database_code_CSD 212792 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(galactarato)dineodymium(III)octahydrate ; _chemical_name_common tris(galactarato)dineodymium(iii)octahydrate _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H40 Nd2 O32' _chemical_formula_weight 1056.98 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 10.2151(14) _cell_length_b 10.2151(14) _cell_length_c 8.9021(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 804.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4515 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.43 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_absorpt_coefficient_mu 3.315 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.819 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; Sheldrick, G. M., SADABS ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5116 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0175 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1230 _reflns_number_gt 1228 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Analysis of the diffraction data suggested that the Laue symmetry was 6/m. The structure was originally solved in the space group P-6 with disordered ligand and metal centres. The refinement was very unsatisfactory and as a consequence the crystal was solved and refined in the space group P-3 as a twinned crystal. This led to a far more satisfactory refinement. Three significant, unique peaks of electron density were found within the hexagonal channels. These were refined as the oxygen atoms of water molecules with a common, fixed isotropic displacement parameter. The two highest peaks were closer than would be expected on the basis of a normal hydrogen bonding interaction and accordingly they were refined such that the sum of their site occupancies was 1. The site occupancy of the third oxygen atom was refined. The sum of the site occupancies of these three sites was 1.36 water molecules per asymmetric unit. This corresponds to 8.16 water molecules per formula unit. 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+0.3972P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1230 _refine_ls_number_parameters 81 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0212 _refine_ls_R_factor_gt 0.0211 _refine_ls_wR_factor_ref 0.0565 _refine_ls_wR_factor_gt 0.0565 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 O4 O 0.1786(11) 0.1795(11) 0.1031(9) 0.080 Uiso 0.716(10) 1 d P . . O5 O 0.151(2) 0.118(3) 0.413(2) 0.080 Uiso 0.284(10) 1 d P . . O6 O 0.104(2) 0.1857(19) 0.351(2) 0.080 Uiso 0.358(14) 1 d P . . O3 O 0.6974(3) 0.6096(3) 0.4408(4) 0.0301(6) Uani 1 1 d . . . O1A O 0.6500(3) 0.5660(3) 0.0764(3) 0.0214(6) Uani 1 1 d . . . O1B O 0.5175(3) 0.6784(3) 0.1354(3) 0.0242(6) Uani 1 1 d . . . C1 C 0.5543(4) 0.5796(4) 0.1550(4) 0.0177(7) Uani 1 1 d . . . Nd1 Nd 0.6667 0.3333 0.05114(4) 0.01376(10) Uani 1 3 d S . . O2 O 0.5112(4) 0.3496(3) 0.2633(3) 0.0268(7) Uani 1 1 d . . . C3 C 0.5376(4) 0.5505(4) 0.4326(5) 0.0194(7) Uani 1 1 d . . . H3 H 0.5187 0.6355 0.4371 0.036(13) Uiso 1 1 calc R . . C2 C 0.4782(5) 0.4698(4) 0.2832(4) 0.0182(8) Uani 1 1 d . . . H2 H 0.3686 0.4288 0.2780 0.034(14) 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 O3 0.0222(13) 0.0362(15) 0.0263(14) -0.0054(14) -0.0015(13) 0.0102(11) O1A 0.0250(13) 0.0192(12) 0.0232(16) 0.0022(10) 0.0045(11) 0.0134(11) O1B 0.0256(14) 0.0260(14) 0.0266(15) -0.0043(12) -0.0060(12) 0.0171(13) C1 0.0200(17) 0.0196(17) 0.0133(15) -0.0031(14) -0.0040(14) 0.0097(14) Nd1 0.01465(11) 0.01465(11) 0.01198(13) 0.000 0.000 0.00733(5) O2 0.0427(18) 0.0180(14) 0.0231(14) 0.0044(12) 0.0118(13) 0.0178(13) C3 0.0252(17) 0.0221(16) 0.0150(18) 0.0011(14) 0.0032(15) 0.0148(14) C2 0.0189(18) 0.0207(19) 0.0167(16) 0.0015(13) 0.0037(13) 0.0111(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O5 O6 1.16(2) . ? O3 C3 1.431(4) . ? O1A C1 1.265(5) . ? O1A Nd1 2.477(3) . ? O1B C1 1.253(5) . ? O1B Nd1 2.466(3) 4_665 ? C1 C2 1.515(5) . ? Nd1 O1B 2.466(3) 5 ? Nd1 O1B 2.466(3) 6_655 ? Nd1 O1B 2.466(3) 4_665 ? Nd1 O1A 2.477(3) 3_665 ? Nd1 O1A 2.477(3) 2_655 ? Nd1 O2 2.526(3) 3_665 ? Nd1 O2 2.526(3) 2_655 ? Nd1 O2 2.526(3) . ? O2 C2 1.438(5) . ? C3 C3 1.517(8) 4_666 ? C3 C2 1.522(5) . ? 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 _geom_angle_publ_flag C1 O1A Nd1 125.7(2) . . ? C1 O1B Nd1 125.7(2) . 4_665 ? O1B C1 O1A 124.9(4) . . ? O1B C1 C2 116.9(3) . . ? O1A C1 C2 118.3(3) . . ? O1B Nd1 O1B 79.65(11) 5 6_655 ? O1B Nd1 O1B 79.65(11) 5 4_665 ? O1B Nd1 O1B 79.65(11) 6_655 4_665 ? O1B Nd1 O1A 72.22(9) 5 3_665 ? O1B Nd1 O1A 72.01(9) 6_655 3_665 ? O1B Nd1 O1A 142.90(10) 4_665 3_665 ? O1B Nd1 O1A 72.01(9) 5 2_655 ? O1B Nd1 O1A 142.90(10) 6_655 2_655 ? O1B Nd1 O1A 72.22(9) 4_665 2_655 ? O1A Nd1 O1A 119.18(2) 3_665 2_655 ? O1B Nd1 O1A 142.90(10) 5 . ? O1B Nd1 O1A 72.22(9) 6_655 . ? O1B Nd1 O1A 72.01(9) 4_665 . ? O1A Nd1 O1A 119.18(2) 3_665 . ? O1A Nd1 O1A 119.18(2) 2_655 . ? O1B Nd1 O2 133.31(10) 5 3_665 ? O1B Nd1 O2 91.01(10) 6_655 3_665 ? O1B Nd1 O2 143.79(10) 4_665 3_665 ? O1A Nd1 O2 61.44(9) 3_665 3_665 ? O1A Nd1 O2 125.88(10) 2_655 3_665 ? O1A Nd1 O2 71.82(10) . 3_665 ? O1B Nd1 O2 91.01(10) 5 2_655 ? O1B Nd1 O2 143.80(10) 6_655 2_655 ? O1B Nd1 O2 133.31(10) 4_665 2_655 ? O1A Nd1 O2 71.82(10) 3_665 2_655 ? O1A Nd1 O2 61.44(9) 2_655 2_655 ? O1A Nd1 O2 125.88(10) . 2_655 ? O2 Nd1 O2 70.18(12) 3_665 2_655 ? O1B Nd1 O2 143.79(10) 5 . ? O1B Nd1 O2 133.31(10) 6_655 . ? O1B Nd1 O2 91.01(10) 4_665 . ? O1A Nd1 O2 125.88(10) 3_665 . ? O1A Nd1 O2 71.82(10) 2_655 . ? O1A Nd1 O2 61.44(9) . . ? O2 Nd1 O2 70.18(12) 3_665 . ? O2 Nd1 O2 70.18(12) 2_655 . ? C2 O2 Nd1 124.9(2) . . ? O3 C3 C3 109.2(4) . 4_666 ? O3 C3 C2 109.6(3) . . ? C3 C3 C2 113.1(4) 4_666 . ? O2 C2 C1 106.7(3) . . ? O2 C2 C3 111.7(3) . . ? C1 C2 C3 109.8(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.152 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.119 #===END data_ndb78k1a _database_code_CSD 212793 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetraaquotris(galactarato)dineodymium(III)decahydrate ; _chemical_name_common tetraaquotris(galactarato)dineodymium(iii)decahydrate _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H52 Nd2 O38' _chemical_formula_weight 1165.08 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.8647(9) _cell_length_b 19.6810(16) _cell_length_c 19.9740(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4271.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3381 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 26.02 _exptl_crystal_description trigonal _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 2.517 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.926 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; Sheldrick, G, M,. SADABS ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 25100 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.54 _reflns_number_total 4851 _reflns_number_gt 3590 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+19.6000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4851 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 O4B O 0.2598(4) 0.8832(2) 0.6896(2) 0.0268(10) Uani 1 1 d . . . O9B O -0.2469(4) 0.6887(2) 0.8178(2) 0.0311(10) Uani 1 1 d . . . O6 O 0.1349(4) 0.7843(2) 0.8141(2) 0.0240(9) Uani 1 1 d . . . O9A O -0.1977(4) 0.6017(2) 0.7531(2) 0.0333(11) Uani 1 1 d . . . O7 O -0.1227(4) 0.7787(2) 0.6977(2) 0.0212(9) Uani 1 1 d . . . C6 C 0.0723(5) 0.7993(3) 0.7528(3) 0.0191(12) Uani 1 1 d . . . H6 H 0.1192 0.7796 0.7157 0.019 Uiso 1 1 calc R . . C7 C -0.0539(5) 0.7640(3) 0.7561(3) 0.0186(12) Uani 1 1 d . . . H7 H -0.0986 0.7840 0.7939 0.019 Uiso 1 1 calc R . . O4A O 0.2166(4) 0.9570(2) 0.7704(2) 0.0289(10) Uani 1 1 d . . . C5 C 0.0604(5) 0.8758(3) 0.7411(3) 0.0187(12) Uani 1 1 d . . . H5 H 0.0130 0.8834 0.7001 0.019 Uiso 1 1 calc R . . O11 O -0.0220(4) 1.0252(2) 0.6986(2) 0.0367(12) Uani 1 1 d . . . O5 O 0.0005(4) 0.9104(2) 0.7953(2) 0.0202(9) Uani 1 1 d . . . C8 C -0.0444(5) 0.6882(3) 0.7694(3) 0.0192(13) Uani 1 1 d . . . H8 H 0.0068 0.6806 0.8091 0.019 Uiso 1 1 calc R . . C4 C 0.1878(5) 0.9079(3) 0.7327(3) 0.0202(13) Uani 1 1 d . . . C9 C -0.1733(5) 0.6580(3) 0.7814(3) 0.0199(13) Uani 1 1 d . . . O2 O 0.0370(4) 1.1012(2) 0.9232(2) 0.0234(9) Uani 1 1 d . . . O1A O 0.2575(4) 1.0561(3) 0.8817(2) 0.0333(11) Uani 1 1 d . . . C3 C 0.0643(5) 0.9990(3) 0.9854(3) 0.0204(12) Uani 1 1 d . . . H3 H 0.1193 0.9740 1.0155 0.020 Uiso 1 1 calc R . . O1B O 0.3363(4) 1.0643(3) 0.9859(2) 0.0426(13) Uani 1 1 d . . . C2 C 0.1161(6) 1.0712(3) 0.9726(3) 0.0227(13) Uani 1 1 d . . . H2 H 0.1160 1.0981 1.0139 0.023 Uiso 1 1 calc R . . C1 C 0.2479(6) 1.0640(3) 0.9445(3) 0.0288(15) Uani 1 1 d . . . O12 O -0.0383(5) 0.7398(2) 0.5717(2) 0.0394(12) Uani 1 1 d . . . O13 O 0.5720(6) 1.0607(4) 0.9300(3) 0.075(2) Uani 1 1 d . . . O14 O 0.1010(6) 0.8383(3) 0.9392(3) 0.0552(16) Uani 1 1 d . . . O15 O -0.1914(6) 0.6937(4) 0.9762(3) 0.076(2) Uani 1 1 d . . . O16 O 0.1763(5) 0.8184(3) 0.5717(3) 0.0514(15) Uani 1 1 d . . . Nd1 Nd 0.06667(3) 1.034010(15) 0.816411(15) 0.01657(10) Uani 1 1 d . . . O10 O -0.1568(4) 1.0296(2) 0.8411(2) 0.0257(10) Uani 1 1 d . . . O8 O 0.0095(4) 0.6531(2) 0.7126(2) 0.0233(10) Uani 1 1 d . . . O3 O 0.0598(4) 0.9658(2) 0.9213(2) 0.0265(9) 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 O4B 0.022(2) 0.025(2) 0.033(2) -0.005(2) 0.006(2) -0.0034(18) O9B 0.024(2) 0.025(2) 0.044(3) -0.009(2) 0.011(2) -0.0010(18) O6 0.018(2) 0.023(2) 0.031(2) 0.005(2) -0.005(2) -0.0002(17) O9A 0.023(2) 0.027(2) 0.050(3) -0.016(2) 0.013(2) -0.008(2) O7 0.0143(19) 0.023(2) 0.027(2) 0.0020(18) -0.0040(17) 0.0010(17) C6 0.018(3) 0.014(3) 0.025(3) -0.002(2) 0.004(3) 0.000(2) C7 0.016(3) 0.013(3) 0.027(3) -0.004(2) -0.002(3) -0.001(2) O4A 0.018(2) 0.019(2) 0.050(3) -0.011(2) 0.006(2) -0.0034(18) C5 0.020(3) 0.015(3) 0.021(3) 0.000(2) 0.002(3) -0.001(2) O11 0.032(2) 0.040(3) 0.037(3) -0.002(2) -0.011(2) 0.002(2) O5 0.016(2) 0.015(2) 0.029(2) -0.0021(17) 0.0024(18) 0.0003(16) C8 0.012(3) 0.015(3) 0.030(3) -0.005(2) 0.005(2) -0.002(2) C4 0.015(3) 0.016(3) 0.029(3) 0.004(3) 0.001(3) 0.002(2) C9 0.018(3) 0.015(3) 0.027(3) 0.001(3) -0.003(3) 0.000(2) O2 0.025(2) 0.019(2) 0.027(2) -0.0014(19) -0.0032(18) -0.0011(18) O1A 0.021(2) 0.054(3) 0.024(2) -0.006(2) 0.000(2) -0.006(2) C3 0.024(3) 0.018(3) 0.019(3) -0.001(2) -0.004(3) 0.000(3) O1B 0.023(2) 0.068(4) 0.037(3) -0.011(3) -0.008(2) -0.005(2) C2 0.023(3) 0.025(3) 0.020(3) -0.004(3) -0.002(3) 0.000(3) C1 0.026(3) 0.033(4) 0.027(4) -0.005(3) -0.004(3) -0.006(3) O12 0.051(3) 0.026(3) 0.041(3) 0.003(2) 0.007(2) 0.001(2) O13 0.062(4) 0.107(6) 0.057(4) 0.016(4) 0.005(4) -0.009(4) O14 0.088(5) 0.034(3) 0.044(3) 0.000(3) 0.004(3) 0.015(3) O15 0.070(5) 0.105(6) 0.052(4) 0.010(4) -0.007(3) -0.017(4) O16 0.059(4) 0.053(4) 0.042(3) 0.000(3) -0.001(3) -0.020(3) Nd1 0.01569(15) 0.01282(15) 0.02121(16) 0.00018(14) 0.00112(14) -0.00007(13) O10 0.0152(19) 0.029(2) 0.033(2) 0.001(2) -0.0107(18) 0.0023(19) O8 0.020(2) 0.017(2) 0.034(2) -0.0067(19) 0.0081(19) 0.0012(17) O3 0.035(2) 0.022(2) 0.023(2) -0.0027(19) 0.0026(19) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O4B C4 1.261(7) . ? O9B C9 1.237(7) . ? O6 C6 1.431(7) . ? O9A C9 1.272(7) . ? O9A Nd1 2.393(4) 3_546 ? O7 C7 1.415(7) . ? C6 C5 1.530(7) . ? C6 C7 1.538(7) . ? C7 C8 1.519(8) . ? O4A C4 1.263(7) . ? O4A Nd1 2.408(4) . ? C5 O5 1.434(7) . ? C5 C4 1.531(8) . ? O11 Nd1 2.548(5) . ? O5 Nd1 2.572(4) . ? C8 O8 1.451(7) . ? C8 C9 1.541(8) . ? O2 C2 1.434(7) . ? O2 Nd1 2.531(4) . ? O1A C1 1.267(8) . ? O1A Nd1 2.488(4) . ? C3 O3 1.439(7) . ? C3 C3 1.515(12) 5_577 ? C3 C2 1.551(8) . ? O1B C1 1.267(8) . ? C2 C1 1.545(9) . ? Nd1 O9A 2.393(4) 3_556 ? Nd1 O10 2.479(4) . ? Nd1 O3 2.489(4) . ? Nd1 O8 2.552(4) 3_556 ? O8 Nd1 2.552(4) 3_546 ? 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 _geom_angle_publ_flag C9 O9A Nd1 128.2(4) . 3_546 ? O6 C6 C5 111.9(5) . . ? O6 C6 C7 107.2(4) . . ? C5 C6 C7 112.1(5) . . ? O7 C7 C8 112.4(5) . . ? O7 C7 C6 110.1(5) . . ? C8 C7 C6 112.9(4) . . ? C4 O4A Nd1 122.7(4) . . ? O5 C5 C6 113.0(5) . . ? O5 C5 C4 107.3(5) . . ? C6 C5 C4 110.3(5) . . ? C5 O5 Nd1 116.5(3) . . ? O8 C8 C7 111.0(5) . . ? O8 C8 C9 107.8(5) . . ? C7 C8 C9 110.1(5) . . ? O4B C4 O4A 123.2(5) . . ? O4B C4 C5 118.4(5) . . ? O4A C4 C5 118.3(5) . . ? O9B C9 O9A 123.5(5) . . ? O9B C9 C8 119.4(5) . . ? O9A C9 C8 117.1(5) . . ? C2 O2 Nd1 106.7(3) . . ? C1 O1A Nd1 118.2(4) . . ? O3 C3 C3 108.9(6) . 5_577 ? O3 C3 C2 106.4(5) . . ? C3 C3 C2 111.9(6) 5_577 . ? O2 C2 C1 110.1(5) . . ? O2 C2 C3 105.9(5) . . ? C1 C2 C3 108.1(5) . . ? O1B C1 O1A 125.7(6) . . ? O1B C1 C2 117.7(6) . . ? O1A C1 C2 116.5(5) . . ? O9A Nd1 O4A 74.13(15) 3_556 . ? O9A Nd1 O10 135.85(14) 3_556 . ? O4A Nd1 O10 135.77(14) . . ? O9A Nd1 O1A 73.21(16) 3_556 . ? O4A Nd1 O1A 75.31(15) . . ? O10 Nd1 O1A 135.88(14) . . ? O9A Nd1 O3 143.70(15) 3_556 . ? O4A Nd1 O3 90.10(15) . . ? O10 Nd1 O3 77.55(14) . . ? O1A Nd1 O3 71.20(15) . . ? O9A Nd1 O2 105.86(15) 3_556 . ? O4A Nd1 O2 137.48(14) . . ? O10 Nd1 O2 74.10(13) . . ? O1A Nd1 O2 64.69(14) . . ? O3 Nd1 O2 64.47(13) . . ? O9A Nd1 O11 74.21(16) 3_556 . ? O4A Nd1 O11 81.97(16) . . ? O10 Nd1 O11 79.10(15) . . ? O1A Nd1 O11 144.23(15) . . ? O3 Nd1 O11 136.77(15) . . ? O2 Nd1 O11 139.98(14) . . ? O9A Nd1 O8 63.24(13) 3_556 3_556 ? O4A Nd1 O8 135.28(14) . 3_556 ? O10 Nd1 O8 76.11(13) . 3_556 ? O1A Nd1 O8 103.24(15) . 3_556 ? O3 Nd1 O8 132.62(13) . 3_556 ? O2 Nd1 O8 70.75(13) . 3_556 ? O11 Nd1 O8 74.35(15) . 3_556 ? O9A Nd1 O5 126.72(15) 3_556 . ? O4A Nd1 O5 62.02(13) . . ? O10 Nd1 O5 74.09(13) . . ? O1A Nd1 O5 118.95(15) . . ? O3 Nd1 O5 67.61(13) . . ? O2 Nd1 O5 126.67(13) . . ? O11 Nd1 O5 71.23(14) . . ? O8 Nd1 O5 137.81(13) 3_556 . ? C8 O8 Nd1 119.0(3) . 3_546 ? C3 O3 Nd1 120.2(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.951 _refine_diff_density_min -1.657 _refine_diff_density_rms 0.151 #===END data_eub92a1a _database_code_CSD 212794 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetraaquotris(galactarato)dieuropium(III)decahydrate ; _chemical_name_common tetraaquotris(galactarato)dieuropium(iii)decahydrate _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H52 Eu2 O38' _chemical_formula_weight 1180.52 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.761(4) _cell_length_b 19.427(7) _cell_length_c 19.681(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4114(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2130 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 24.46 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.025 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 3.138 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; Sheldrick, G, M,. SADABS ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 24104 _diffrn_reflns_av_R_equivalents 0.0985 _diffrn_reflns_av_sigmaI/netI 0.0783 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.58 _reflns_number_total 4701 _reflns_number_gt 3246 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+21.6782P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4701 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1140 _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.1384 _refine_ls_wR_factor_gt 0.1249 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.145 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 O12 O -0.0389(7) 0.7405(4) 0.5710(4) 0.0377(18) Uani 1 1 d . . . O13 O 0.5734(8) 1.0593(5) 0.9293(4) 0.067(3) Uani 1 1 d . . . O14 O 0.0999(8) 0.8380(4) 0.9395(4) 0.051(2) Uani 1 1 d . . . O15 O -0.1912(9) 0.6925(5) 0.9748(4) 0.072(3) Uani 1 1 d . . . O16 O 0.1761(8) 0.8190(4) 0.5707(4) 0.051(2) Uani 1 1 d . . . O4B O 0.2589(5) 0.8838(3) 0.6892(3) 0.0247(14) Uani 1 1 d . . . O9B O -0.2479(6) 0.6873(3) 0.8181(4) 0.0292(15) Uani 1 1 d . . . O6 O 0.1354(5) 0.7837(3) 0.8141(3) 0.0237(14) Uani 1 1 d . . . O9A O -0.1988(5) 0.6008(3) 0.7515(4) 0.0286(15) Uani 1 1 d . . . O7 O -0.1239(6) 0.7787(3) 0.6973(3) 0.0209(14) Uani 1 1 d . . . C6 C 0.0715(8) 0.7991(4) 0.7525(4) 0.0188(18) Uani 1 1 d . . . H6 H 0.1183 0.7792 0.7145 0.019 Uiso 1 1 calc R . . C7 C -0.0538(7) 0.7640(4) 0.7563(4) 0.0144(17) Uani 1 1 d . . . H7 H -0.0984 0.7839 0.7950 0.014 Uiso 1 1 calc R . . O4A O 0.2156(5) 0.9578(3) 0.7694(4) 0.0273(15) Uani 1 1 d . . . C5 C 0.0598(8) 0.8759(4) 0.7410(4) 0.0163(18) Uani 1 1 d . . . H5 H 0.0119 0.8837 0.6994 0.016 Uiso 1 1 calc R . . O11 O -0.0196(6) 1.0254(3) 0.7002(3) 0.0313(16) Uani 1 1 d . . . O5 O 0.0005(5) 0.9108(3) 0.7958(3) 0.0174(13) Uani 1 1 d . . . C8 C -0.0449(7) 0.6872(4) 0.7685(5) 0.0164(19) Uani 1 1 d . . . H8 H 0.0065 0.6790 0.8088 0.016 Uiso 1 1 calc R . . C4 C 0.1885(8) 0.9082(4) 0.7326(5) 0.018(2) Uani 1 1 d . . . C9 C -0.1741(8) 0.6570(4) 0.7806(5) 0.0168(19) Uani 1 1 d . . . O2 O 0.0391(5) 1.1012(3) 0.9217(3) 0.0215(14) Uani 1 1 d . . . O1A O 0.2573(6) 1.0545(4) 0.8814(3) 0.0296(16) Uani 1 1 d . . . C3 C 0.0633(8) 0.9990(4) 0.9847(4) 0.0159(17) Uani 1 1 d . . . H3 H 0.1194 0.9735 1.0148 0.016 Uiso 1 1 calc R . . O1B O 0.3368(6) 1.0637(4) 0.9849(4) 0.0416(19) Uani 1 1 d . . . C2 C 0.1168(8) 1.0705(5) 0.9713(5) 0.021(2) Uani 1 1 d . . . H2 H 0.1166 1.0979 1.0131 0.021 Uiso 1 1 calc R . . C1 C 0.2494(9) 1.0632(5) 0.9440(5) 0.029(2) Uani 1 1 d . . . Eu1 Eu 0.06754(4) 1.03365(2) 0.81643(2) 0.01433(13) Uani 1 1 d . . . O10 O -0.1520(5) 1.0295(3) 0.8400(3) 0.0214(13) Uani 1 1 d . . . O8 O 0.0087(5) 0.6522(3) 0.7121(3) 0.0209(14) Uani 1 1 d . . . O3 O 0.0587(6) 0.9663(3) 0.9203(3) 0.0250(13) 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 O12 0.046(5) 0.029(4) 0.038(4) 0.004(3) 0.008(4) -0.001(3) O13 0.057(6) 0.095(7) 0.047(5) 0.020(5) 0.009(5) -0.018(5) O14 0.080(7) 0.031(4) 0.041(5) -0.001(4) 0.001(4) 0.016(4) O15 0.070(7) 0.095(8) 0.050(6) 0.003(5) -0.009(5) -0.009(6) O16 0.058(6) 0.047(5) 0.048(5) -0.001(4) 0.000(4) -0.014(4) O4B 0.020(3) 0.025(3) 0.029(4) -0.008(3) 0.004(3) -0.006(3) O9B 0.023(3) 0.023(3) 0.042(4) -0.011(3) 0.009(3) 0.000(3) O6 0.021(3) 0.018(3) 0.033(4) 0.003(3) -0.009(3) 0.000(2) O9A 0.020(3) 0.018(3) 0.048(4) -0.010(3) 0.011(3) -0.010(3) O7 0.019(3) 0.020(3) 0.024(4) 0.002(3) -0.002(3) 0.003(2) C6 0.020(4) 0.012(4) 0.025(5) -0.005(3) 0.010(4) -0.002(4) C7 0.009(4) 0.013(4) 0.021(4) -0.007(3) -0.004(4) -0.005(3) O4A 0.017(3) 0.013(3) 0.052(4) -0.011(3) 0.005(3) -0.004(3) C5 0.016(4) 0.005(4) 0.027(5) -0.004(3) -0.006(4) 0.000(3) O11 0.024(3) 0.034(4) 0.036(4) -0.004(3) -0.007(3) 0.002(3) O5 0.013(3) 0.014(3) 0.026(4) -0.004(3) 0.004(3) 0.001(2) C8 0.013(4) 0.014(4) 0.023(5) -0.002(4) 0.006(4) -0.005(3) C4 0.016(4) 0.008(4) 0.030(5) 0.005(4) -0.005(4) -0.003(3) C9 0.013(4) 0.013(4) 0.025(5) 0.002(4) 0.000(4) -0.001(3) O2 0.021(3) 0.018(3) 0.025(3) 0.003(3) 0.001(3) -0.001(3) O1A 0.017(3) 0.047(5) 0.024(4) -0.005(3) -0.001(3) -0.007(3) C3 0.019(4) 0.019(4) 0.010(4) -0.001(3) 0.000(4) 0.004(4) O1B 0.025(4) 0.065(5) 0.035(4) -0.006(4) -0.005(3) -0.004(4) C2 0.020(4) 0.025(5) 0.020(5) -0.007(4) 0.004(4) -0.007(4) C1 0.024(5) 0.033(6) 0.029(6) -0.001(5) 0.001(5) -0.012(4) Eu1 0.01372(19) 0.01008(19) 0.0192(2) 0.0004(2) 0.0013(2) -0.00018(18) O10 0.013(3) 0.025(3) 0.026(3) -0.001(3) -0.012(2) 0.004(3) O8 0.017(3) 0.011(3) 0.034(4) -0.006(3) 0.006(3) 0.000(2) O3 0.031(3) 0.025(3) 0.019(3) 0.003(3) 0.000(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O4B C4 1.236(10) . ? O9B C9 1.233(10) . ? O6 C6 1.426(11) . ? O9A C9 1.261(10) . ? O9A Eu1 2.342(6) 3_546 ? O7 C7 1.413(10) . ? C6 C7 1.513(10) . ? C6 C5 1.513(10) . ? C7 C8 1.514(11) . ? O4A C4 1.241(10) . ? O4A Eu1 2.359(6) . ? C5 O5 1.425(10) . ? C5 C4 1.529(11) . ? O11 Eu1 2.478(6) . ? O5 Eu1 2.527(6) . ? C8 O8 1.423(10) . ? C8 C9 1.528(11) . ? C4 Eu1 3.218(9) . ? O2 C2 1.418(11) . ? O2 Eu1 2.471(6) . ? O1A C1 1.245(11) . ? O1A Eu1 2.443(6) . ? C3 O3 1.420(9) . ? C3 C3 1.489(17) 5_577 ? C3 C2 1.526(12) . ? O1B C1 1.238(12) . ? C2 C1 1.532(13) . ? C2 Eu1 3.176(9) . ? C1 Eu1 3.234(10) . ? Eu1 O9A 2.342(6) 3_556 ? Eu1 O10 2.409(6) . ? Eu1 O3 2.428(6) . ? Eu1 O8 2.509(6) 3_556 ? O8 Eu1 2.509(6) 3_546 ? 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 _geom_angle_publ_flag C9 O9A Eu1 127.9(5) . 3_546 ? O6 C6 C7 107.0(7) . . ? O6 C6 C5 112.0(7) . . ? C7 C6 C5 112.2(7) . . ? O7 C7 C6 110.1(7) . . ? O7 C7 C8 111.3(7) . . ? C6 C7 C8 113.3(6) . . ? C4 O4A Eu1 123.8(6) . . ? O5 C5 C6 113.2(7) . . ? O5 C5 C4 107.0(6) . . ? C6 C5 C4 110.2(7) . . ? C5 O5 Eu1 116.3(4) . . ? O8 C8 C7 112.0(7) . . ? O8 C8 C9 107.8(7) . . ? C7 C8 C9 110.2(7) . . ? O4B C4 O4A 123.8(8) . . ? O4B C4 C5 118.2(7) . . ? O4A C4 C5 118.0(8) . . ? O4B C4 Eu1 153.2(6) . . ? O4A C4 Eu1 37.5(4) . . ? C5 C4 Eu1 83.7(5) . . ? O9B C9 O9A 123.3(8) . . ? O9B C9 C8 119.7(7) . . ? O9A C9 C8 117.0(7) . . ? C2 O2 Eu1 106.4(5) . . ? C1 O1A Eu1 118.9(6) . . ? O3 C3 C3 109.9(9) . 5_577 ? O3 C3 C2 105.4(6) . . ? C3 C3 C2 113.1(9) 5_577 . ? O2 C2 C3 106.2(7) . . ? O2 C2 C1 110.3(7) . . ? C3 C2 C1 109.1(7) . . ? O2 C2 Eu1 48.3(4) . . ? C3 C2 Eu1 84.1(5) . . ? C1 C2 Eu1 78.3(5) . . ? O1B C1 O1A 126.4(9) . . ? O1B C1 C2 118.5(9) . . ? O1A C1 C2 115.0(8) . . ? O1B C1 Eu1 165.0(8) . . ? O1A C1 Eu1 41.4(4) . . ? C2 C1 Eu1 74.1(5) . . ? O9A Eu1 O4A 73.5(2) 3_556 . ? O9A Eu1 O10 136.1(2) 3_556 . ? O4A Eu1 O10 135.8(2) . . ? O9A Eu1 O3 143.5(2) 3_556 . ? O4A Eu1 O3 91.2(2) . . ? O10 Eu1 O3 77.4(2) . . ? O9A Eu1 O1A 72.7(2) 3_556 . ? O4A Eu1 O1A 75.2(2) . . ? O10 Eu1 O1A 136.4(2) . . ? O3 Eu1 O1A 71.4(2) . . ? O9A Eu1 O2 104.9(2) 3_556 . ? O4A Eu1 O2 138.1(2) . . ? O10 Eu1 O2 74.60(19) . . ? O3 Eu1 O2 64.9(2) . . ? O1A Eu1 O2 64.9(2) . . ? O9A Eu1 O11 74.8(2) 3_556 . ? O4A Eu1 O11 81.5(2) . . ? O10 Eu1 O11 78.7(2) . . ? O3 Eu1 O11 136.7(2) . . ? O1A Eu1 O11 144.1(2) . . ? O2 Eu1 O11 139.6(2) . . ? O9A Eu1 O8 63.76(19) 3_556 3_556 ? O4A Eu1 O8 134.9(2) . 3_556 ? O10 Eu1 O8 75.7(2) . 3_556 ? O3 Eu1 O8 132.1(2) . 3_556 ? O1A Eu1 O8 103.8(2) . 3_556 ? O2 Eu1 O8 70.1(2) . 3_556 ? O11 Eu1 O8 74.3(2) . 3_556 ? O9A Eu1 O5 127.3(2) 3_556 . ? O4A Eu1 O5 62.59(19) . . ? O10 Eu1 O5 73.71(19) . . ? O3 Eu1 O5 67.4(2) . . ? O1A Eu1 O5 118.7(2) . . ? O2 Eu1 O5 126.93(19) . . ? O11 Eu1 O5 71.5(2) . . ? O8 Eu1 O5 137.58(19) 3_556 . ? O9A Eu1 C2 108.8(2) 3_556 . ? O4A Eu1 C2 113.9(2) . . ? O10 Eu1 C2 89.2(2) . . ? O3 Eu1 C2 47.2(2) . . ? O1A Eu1 C2 47.2(2) . . ? O2 Eu1 C2 25.4(2) . . ? O11 Eu1 C2 164.6(2) . . ? O8 Eu1 C2 93.6(2) 3_556 . ? O5 Eu1 C2 114.5(2) . . ? O9A Eu1 C4 83.4(2) 3_556 . ? O4A Eu1 C4 18.7(2) . . ? O10 Eu1 C4 118.0(2) . . ? O3 Eu1 C4 92.2(2) . . ? O1A Eu1 C4 93.2(2) . . ? O2 Eu1 C4 151.9(2) . . ? O11 Eu1 C4 68.3(2) . . ? O8 Eu1 C4 135.5(2) 3_556 . ? O5 Eu1 C4 46.95(19) . . ? C2 Eu1 C4 126.5(2) . . ? O9A Eu1 C1 88.8(2) 3_556 . ? O4A Eu1 C1 90.4(2) . . ? O10 Eu1 C1 116.7(2) . . ? O3 Eu1 C1 57.7(2) . . ? O1A Eu1 C1 19.7(2) . . ? O2 Eu1 C1 47.9(2) . . ? O11 Eu1 C1 163.2(2) . . ? O8 Eu1 C1 102.1(2) 3_556 . ? O5 Eu1 C1 117.7(2) . . ? C2 Eu1 C1 27.6(2) . . ? C4 Eu1 C1 106.7(2) . . ? C8 O8 Eu1 118.8(4) . 3_546 ? C3 O3 Eu1 120.6(5) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.338 _refine_diff_density_min -1.588 _refine_diff_density_rms 0.203 #===END