# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Mikael Hakansson' _publ_contact_author_email HSON@CHEM.GU.SE _publ_section_title ; ; loop_ _publ_author_name 'Mikael Hakansson' 'Anders Lennartson' # Attachment '1a_new.cif' data_1a _database_code_depnum_ccdc_archive 'CCDC 699737' _audit_creation_method SHELXL-97 _chemical_name_systematic ;Pentasodium tris(2,2?-oxydiacetato)-dysprosium(III) bis(tetrafluoroborate) hexahydrate ; _chemical_name_common ; Pentasodium tris(2,2?-oxydiacetato)-dysprosium(iii) bis(tetrafluoroborate) hexahydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 B2 Dy F8 Na5 O21' _chemical_formula_sum 'C12 H24 B2 Dy F8 Na5 O21' _chemical_formula_weight 955.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 2' _symmetry_int_tables_number 155 _symmetry_space_group_name_Hall 'R 3 2"' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' 'y+1/3, x+2/3, -z+2/3' _cell_length_a 9.638(2) _cell_length_b 9.638(2) _cell_length_c 27.840(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2239.6(9) _cell_formula_units_Z 3 _cell_measurement_temperature 289(2) _cell_measurement_reflns_used 5017 _cell_measurement_theta_min 4.39 _cell_measurement_theta_max 26.00 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1401 _exptl_absorpt_coefficient_mu 2.711 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3377 _exptl_absorpt_correction_T_max 0.7612 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'rotating anode' _diffrn_source_type RU-H3R _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS IIC image-plate system' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean 105 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5017 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 4.39 _diffrn_reflns_theta_max 26.00 _reflns_number_total 960 _reflns_number_gt 959 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear(Rigaku, 2000)' _computing_cell_refinement 'CrystalClear(Rigaku, 2000)' _computing_data_reduction 'CrystalClear(Rigaku, 2000)' _computing_structure_solution 'CrystalClear(Rigaku, 2000)' _computing_structure_refinement 'SIR92 (Altomare et al., 1993)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) and PLUTON (Spek, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0166P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack (1983), 392 Friedel pairs' _refine_ls_abs_structure_Flack -0.029(16) _refine_ls_number_reflns 960 _refine_ls_number_parameters 76 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0257 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0555 _refine_ls_wR_factor_gt 0.0554 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 C1 C 0.3403(4) 0.1880(9) 0.76794(13) 0.0207(14) Uani 1 1 d . . . C2 C 0.2858(5) 0.0480(5) 0.80145(15) 0.0272(9) Uani 1 1 d . . . H2B H 0.1928 0.0324 0.8194 0.033 Uiso 1 1 calc R . . H2A H 0.2560 -0.0487 0.7832 0.033 Uiso 1 1 calc R . . O1 O 0.4124(4) 0.0791(4) 0.8333 0.0243(9) Uani 1 2 d S . . O2 O 0.4780(3) 0.3066(3) 0.77509(10) 0.0237(6) Uani 1 1 d . . . O3 O 0.2524(4) 0.1741(4) 0.73364(11) 0.0363(8) Uani 1 1 d . . . O4 O 0.5928(4) 0.4805(4) 0.69107(12) 0.0388(10) Uani 1 1 d . . . F1 F 0.3333 0.6667 0.78578(16) 0.0720(15) Uani 1 3 d S . . F2 F 0.2475(8) 0.5131(3) 0.71985(12) 0.0614(8) Uani 1 1 d . . . Na1 Na 0.3333 0.3815(3) 0.6667 0.0443(7) Uani 1 2 d S . . Na2 Na 0.0000 0.0000 0.69996(8) 0.0278(5) Uani 1 3 d S . . Dy1 Dy 0.6667 0.3333 0.8333 0.01566(14) Uani 1 6 d S . . B1 B 0.3333 0.6667 0.7369(2) 0.0344(15) Uani 1 3 d S . . 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 C1 0.0195(16) 0.022(4) 0.0213(17) -0.0004(18) -0.0036(12) 0.0106(19) C2 0.020(2) 0.030(2) 0.024(2) 0.0031(18) -0.0064(17) 0.0074(19) O1 0.0194(15) 0.0194(15) 0.025(2) 0.0058(9) -0.0058(9) 0.0033(17) O2 0.0217(15) 0.0256(15) 0.0209(14) 0.0014(12) -0.0049(12) 0.0097(12) O3 0.0327(17) 0.0378(18) 0.0322(17) 0.0020(13) -0.0149(14) 0.0131(14) O4 0.041(2) 0.040(2) 0.0292(16) 0.0021(13) -0.0069(13) 0.015(2) F1 0.092(2) 0.092(2) 0.031(2) 0.000 0.000 0.0462(12) F2 0.056(3) 0.0439(14) 0.0677(17) -0.0116(13) -0.006(3) 0.012(3) Na1 0.0334(15) 0.0463(13) 0.0489(17) 0.0002(6) 0.0003(13) 0.0167(8) Na2 0.0292(7) 0.0292(7) 0.0250(11) 0.000 0.000 0.0146(4) Dy1 0.01749(16) 0.01749(16) 0.01199(19) 0.000 0.000 0.00875(8) B1 0.039(2) 0.039(2) 0.025(3) 0.000 0.000 0.0195(12) _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 C1 O3 1.238(5) . ? C1 O2 1.261(5) . ? C1 C2 1.503(8) . ? C2 O1 1.415(4) . ? C2 H2B 0.9700 . ? C2 H2A 0.9700 . ? O1 Dy1 2.450(4) . ? O2 Dy1 2.352(3) . ? O3 Na2 2.352(3) . ? O3 Na1 2.554(4) . ? O4 Na1 2.289(3) . ? F1 B1 1.359(8) . ? F2 B1 1.370(4) . ? F2 Na1 2.353(6) . ? Na2 O4 2.472(4) 12_446 ? 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 C1 O2 124.9(6) . . ? O3 C1 C2 117.9(4) . . ? O2 C1 C2 116.9(4) . . ? O1 C2 C1 108.8(3) . . ? O1 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? O1 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? H2B C2 H2A 108.3 . . ? C2 O1 Dy1 122.5(2) . . ? C1 O2 Dy1 127.9(3) . . ? C1 O3 Na2 142.4(4) . . ? C1 O3 Na1 123.6(4) . . ? Na2 O3 Na1 93.98(11) . . ? Na1 O4 Na2 97.82(12) . 10_556 ? B1 F2 Na1 128.0(4) . . ? O4 Na1 O4 165.1(2) 11_556 . ? O4 Na1 F2 101.18(19) 11_556 11_556 ? O4 Na1 F2 89.48(18) . 11_556 ? O4 Na1 F2 101.18(19) . . ? F2 Na1 F2 88.72(19) 11_556 . ? O4 Na1 O3 83.40(12) . 11_556 ? F2 Na1 O3 172.10(17) . 11_556 ? O4 Na1 O3 83.40(12) 11_556 . ? O4 Na1 O3 87.25(12) . . ? F2 Na1 O3 84.86(11) . . ? O3 Na1 O3 101.89(19) 11_556 . ? O3 Na2 O3 105.16(11) . 3 ? O3 Na2 O4 85.80(11) . 12_446 ? O3 Na2 O4 83.96(11) 3 12_446 ? O3 Na2 O4 162.92(14) . 10_456 ? O4 Na2 O4 82.33(13) 12_446 10_456 ? O3 Na2 O4 162.92(14) 3 11_556 ? O3 Na2 O4 85.80(11) 2 11_556 ? O3 Na2 Na1 145.33(9) 3 . ? O3 Na2 Na1 101.01(9) 2 . ? O4 Na2 Na1 77.21(9) 12_446 . ? O4 Na2 Na1 119.55(10) 10_456 . ? O3 Na2 Na1 145.33(9) . 2 ? O3 Na2 Na1 145.33(9) 2 3 ? O4 Na2 Na1 77.21(9) 10_456 3 ? O4 Na2 Na1 119.55(10) 11_556 3 ? O2 Dy1 O2 88.18(14) 16_556 . ? O2 Dy1 O2 147.83(14) 17_656 . ? O2 Dy1 O2 127.64(14) 18_546 . ? O2 Dy1 O2 77.72(11) 2_655 . ? O2 Dy1 O1 63.82(7) . . ? O2 Dy1 O1 135.91(7) 3_665 . ? O1 Dy1 O1 120.000(1) 2_655 . ? F1 B1 F2 110.3(3) . . ? F2 B1 F2 108.6(3) 3_565 . ? F1 B1 F2 110.3(3) . 2_665 ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.888 _refine_diff_density_min -0.835 _refine_diff_density_rms 0.110 # Attachment '1b_new.cif' data_1b _database_code_depnum_ccdc_archive 'CCDC 721015' _audit_creation_method SHELXL-97 _chemical_name_systematic ;Pentasodium tris(2,2?-oxydiacetato)-erbium(III) bis(tetrafluoroborate) hexahydrate ; _chemical_name_common ; Pentasodium tris(2,2?-oxydiacetato)-erbium(iii) bis(tetrafluoroborate) hexahydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 B2 Er F8 Na5 O21' _chemical_formula_sum 'C12 H24 B2 Er F8 Na5 O21' _chemical_formula_weight 960.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 2' _symmetry_space_group_name_Hall 'R 3 2"' _symmetry_int_tables_number 155 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' 'y+1/3, x+2/3, -z+2/3' _cell_length_a 9.6578(15) _cell_length_b 9.6578(15) _cell_length_c 27.923(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2255.5(6) _cell_formula_units_Z 3 _cell_measurement_temperature 289(2) _cell_measurement_reflns_used 4432 _cell_measurement_theta_min 4.93 _cell_measurement_theta_max 25.96 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.121 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1407 _exptl_absorpt_coefficient_mu 2.998 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4205 _exptl_absorpt_correction_T_max 0.5494 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 289(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'rotating anode' _diffrn_source_type 'Rigaku RU-H3R' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS IIC image-plate system' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean 105 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4432 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 4.93 _diffrn_reflns_theta_max 25.96 _reflns_number_total 873 _reflns_number_gt 872 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear(Rigaku, 2000)' _computing_cell_refinement 'CrystalClear(Rigaku, 2000)' _computing_data_reduction 'CrystalClear(Rigaku, 2000)' _computing_structure_solution 'CrystalClear(Rigaku, 2000)' _computing_structure_refinement 'SIR92 (Altomare et al., 1993)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) and PLUTON (Spek, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0458P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack (1983), 359 Friedel pairs' _refine_ls_abs_structure_Flack -0.051(17) _refine_ls_number_reflns 873 _refine_ls_number_parameters 76 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0163 _refine_ls_R_factor_gt 0.0149 _refine_ls_wR_factor_ref 0.0691 _refine_ls_wR_factor_gt 0.0403 _refine_ls_goodness_of_fit_ref 1.428 _refine_ls_restrained_S_all 1.428 _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 C1 C 0.6589(5) 0.8121(11) 0.23228(15) 0.0204(17) Uani 1 1 d . . . C2 C 0.7139(6) 0.9515(6) 0.19854(19) 0.0257(10) Uani 1 1 d . . . H2B H 0.7440 1.0486 0.2165 0.031 Uiso 1 1 calc R . . H2A H 0.8063 0.9664 0.1806 0.031 Uiso 1 1 calc R . . O1 O 0.5857(5) 0.9190(5) 0.1667 0.0221(11) Uani 1 2 d S . . O2 O 0.5189(4) 0.6903(4) 0.22457(13) 0.0209(7) Uani 1 1 d . . . O3 O 0.7451(5) 0.8215(5) 0.26606(15) 0.0321(9) Uani 1 1 d . . . O4 O 0.4063(5) 0.5201(5) 0.30931(16) 0.0360(10) Uani 1 1 d . . . F1 F 0.6667 0.3333 0.2143(2) 0.072(2) Uani 1 3 d S . . F2 F 0.7587(10) 0.4870(5) 0.28042(18) 0.0565(14) Uani 1 1 d . . . Na1 Na 0.6667 0.6185(4) 0.3333 0.0417(8) Uani 1 2 d S . . Na2 Na 1.0000 1.0000 0.29968(11) 0.0249(6) Uani 1 3 d S . . Er1 Er 0.3333 0.6667 0.1667 0.0124(2) Uani 1 6 d S . . B1 B 0.6667 0.3333 0.2629(3) 0.0318(16) Uani 1 3 d S . . 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 C1 0.0162(18) 0.023(4) 0.019(2) -0.002(2) -0.0029(14) 0.0079(19) C2 0.019(2) 0.027(2) 0.024(2) 0.004(2) -0.0054(19) 0.005(2) O1 0.0187(17) 0.0187(17) 0.023(3) 0.0050(9) -0.0050(9) 0.0050(18) O2 0.0193(16) 0.0221(16) 0.0181(16) 0.0015(13) -0.0048(13) 0.0080(14) O3 0.0272(18) 0.0348(19) 0.0277(19) 0.0022(15) -0.0136(15) 0.0105(15) O4 0.038(2) 0.034(2) 0.0278(19) 0.0011(15) -0.0047(15) 0.012(2) F1 0.094(3) 0.094(3) 0.027(3) 0.000 0.000 0.0470(17) F2 0.048(3) 0.0380(17) 0.069(2) -0.0103(15) -0.004(3) 0.011(3) Na1 0.0323(17) 0.0443(15) 0.044(2) -0.0009(7) -0.0017(15) 0.0161(9) Na2 0.0254(8) 0.0254(8) 0.0239(13) 0.000 0.000 0.0127(4) Er1 0.0143(2) 0.0143(2) 0.0087(2) 0.000 0.000 0.00716(10) B1 0.035(3) 0.035(3) 0.024(4) 0.000 0.000 0.0177(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 C1 O3 1.231(6) . ? C1 O2 1.291(6) . ? C1 C2 1.506(9) . ? C2 O1 1.426(5) . ? C2 H2B 0.9700 . ? C2 H2A 0.9700 . ? O1 Er1 2.437(5) . ? O2 Er1 2.339(3) . ? O3 Na2 2.381(4) . ? O3 Na1 2.542(5) . ? O4 Na1 2.299(4) . ? O4 Na2 2.468(5) 16_565 ? F1 B1 1.359(11) . ? F2 B1 1.383(5) . ? F2 Na1 2.391(8) . ? Na1 O4 2.299(4) 17_655 ? Na2 O4 2.468(5) 18 ? 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 C1 O2 123.8(7) . . ? O3 C1 C2 119.4(5) . . ? O2 C1 C2 116.8(5) . . ? O1 C2 C1 108.3(4) . . ? O1 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? O1 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? H2B C2 H2A 108.4 . . ? C2 O1 Er1 123.0(3) . . ? C1 O2 Er1 127.3(4) . . ? C1 O3 Na2 140.5(5) . . ? C1 O3 Na1 125.4(4) . . ? Na2 O3 Na1 93.93(14) . . ? Na1 O4 Na2 98.03(17) . 16_565 ? B1 F2 Na1 125.3(5) . . ? O4 Na1 O4 164.6(3) 17_655 . ? O4 Na1 F2 88.3(2) . 17_655 ? O4 Na1 F2 102.8(2) . . ? F2 Na1 F2 88.4(3) 17_655 . ? O4 Na1 O3 83.57(16) . 17_655 ? F2 Na1 O3 170.4(2) . 17_655 ? O4 Na1 O3 83.57(16) 17_655 . ? O4 Na1 O3 86.88(15) . . ? F2 Na1 O3 84.63(15) . . ? O3 Na1 O3 103.0(3) 17_655 . ? O3 Na2 O3 105.48(14) . 3_675 ? O3 Na2 O4 86.04(15) . 18 ? O3 Na2 O4 162.40(18) . 16_665 ? O3 Na2 O4 86.05(15) 3_675 16_665 ? O4 Na2 O4 82.02(17) 18 16_665 ? O3 Na2 O4 83.54(15) . 17_655 ? O3 Na2 O4 162.40(18) 3_675 17_655 ? O3 Na2 O4 86.04(15) 2_765 17_655 ? O2 Er1 O2 146.82(18) 12_455 3_565 ? O2 Er1 O2 77.47(14) 2_665 3_565 ? O2 Er1 O2 88.29(18) 10_565 . ? O2 Er1 O2 146.82(18) 11 . ? O2 Er1 O2 128.81(17) 12_455 . ? O2 Er1 O1 73.41(9) 10_565 . ? O2 Er1 O1 135.85(9) 11 . ? O2 Er1 O1 64.40(9) . . ? O1 Er1 O1 120.000(1) 2_665 . ? F1 B1 F2 110.7(4) . . ? F2 B1 F2 108.2(4) 3_665 . ? _diffrn_measured_fraction_theta_max 0.868 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.853 _refine_diff_density_max 0.696 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.196 # Attachment '1c_new.cif' data_1c _database_code_depnum_ccdc_archive 'CCDC 721016' _audit_creation_method SHELXL-97 _chemical_name_systematic ;Pentasodium tris(2,2?-oxydiacetato)-praseodymium(III) bis(tetrafluoroborate) hexahydrate ; _chemical_name_common ; Pentasodium tris(2,2?-oxydiacetato)-praseodymium(iii) bis(tetrafluoroborate) hexahydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 B2 F8 Na5 O21 Pr1' _chemical_formula_sum 'C12 H24 B2 F8 Na5 O21 Pr1' _chemical_formula_weight 933.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 2' _symmetry_int_tables_number 155 _symmetry_space_group_name_Hall 'R 3 2"' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' 'y+1/3, x+2/3, -z+2/3' _cell_length_a 9.710(2) _cell_length_b 9.710(2) _cell_length_c 28.170(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2300.2(8) _cell_formula_units_Z 3 _cell_measurement_temperature 289(2) _cell_measurement_reflns_used 6034 _cell_measurement_theta_min 4.34 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.022 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1380 _exptl_absorpt_coefficient_mu 1.792 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4889 _exptl_absorpt_correction_T_max 0.64 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 289(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'rotating anode' _diffrn_source_type 'Rigaku RU-H3R' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS IIC image-plate system' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean 105 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6034 _diffrn_reflns_av_R_equivalents 0.0807 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 4.34 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1155 _reflns_number_gt 1153 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear(Rigaku, 2000)' _computing_cell_refinement 'CrystalClear(Rigaku, 2000)' _computing_data_reduction 'CrystalClear(Rigaku, 2000)' _computing_structure_solution 'CrystalClear(Rigaku, 2000)' _computing_structure_refinement 'SIR92 (Altomare et al., 1993)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) and PLUTON (Spek, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0501P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack (1983), 483 Friedel pairs' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 1155 _refine_ls_number_parameters 76 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0772 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 C1 C 0.6641(5) 0.8192(13) 0.23319(13) 0.0387(14) Uani 1 1 d . . . C2 C 0.7188(5) 0.9593(6) 0.19902(18) 0.0461(10) Uani 1 1 d . . . H2A H 0.7470 1.0555 0.2167 0.055 Uiso 1 1 calc R . . H2B H 0.8120 0.9751 0.1817 0.055 Uiso 1 1 calc R . . O1 O 0.5941(4) 0.9274(4) 0.1667 0.0388(9) Uani 1 2 d S . . O2 O 0.5302(4) 0.7009(4) 0.22634(11) 0.0419(7) Uani 1 1 d . . . O3 O 0.7524(5) 0.8347(5) 0.26716(14) 0.0611(12) Uani 1 1 d . . . O4 O 0.4112(4) 0.5230(4) 0.30932(14) 0.0578(11) Uani 1 1 d . . . F1 F 0.6667 0.3333 0.2153(2) 0.101(2) Uani 1 3 d S . . F2 F 0.7483(10) 0.4868(4) 0.28077(15) 0.0891(11) Uani 1 1 d . . . Na1 Na 0.6667 0.6179(4) 0.3333 0.0677(9) Uani 1 2 d S . . Na2 Na 1.0000 1.0000 0.30064(9) 0.0384(5) Uani 1 3 d S . . Pr1 Pr 0.3333 0.6667 0.1667 0.02591(15) Uani 1 6 d S . . B1 B 0.6667 0.3333 0.2635(3) 0.0538(17) Uani 1 3 d S . . 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 C1 0.0390(16) 0.042(4) 0.0394(17) -0.010(2) -0.0117(14) 0.023(2) C2 0.035(2) 0.049(2) 0.046(3) -0.003(2) -0.0054(19) 0.0150(19) O1 0.0348(15) 0.0348(15) 0.041(2) 0.0027(8) -0.0027(8) 0.0127(17) O2 0.0422(16) 0.0432(16) 0.0375(16) 0.0004(13) -0.0124(13) 0.0193(14) O3 0.0540(19) 0.067(3) 0.056(2) -0.0057(16) -0.0261(17) 0.0255(17) O4 0.064(3) 0.052(3) 0.0465(18) 0.0021(14) -0.0091(15) 0.020(2) F1 0.129(3) 0.129(3) 0.044(3) 0.000 0.000 0.0644(17) F2 0.078(3) 0.0605(17) 0.095(3) -0.0089(16) -0.019(4) 0.009(3) Na1 0.0573(18) 0.0682(15) 0.074(2) -0.0013(8) -0.0026(16) 0.0287(9) Na2 0.0386(7) 0.0386(7) 0.0382(11) 0.000 0.000 0.0193(3) Pr1 0.02944(17) 0.02944(17) 0.01885(19) 0.000 0.000 0.01472(9) B1 0.057(3) 0.057(3) 0.047(4) 0.000 0.000 0.0287(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 C1 O3 1.243(6) . ? C1 O2 1.246(7) . ? C1 C2 1.528(11) . ? C2 O1 1.421(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? O1 C2 1.420(5) 12_455 ? O1 Pr1 2.532(4) . ? O2 Pr1 2.440(3) . ? O3 Na2 2.321(4) . ? O3 Na1 2.617(5) . ? O4 Na1 2.274(4) . ? O4 Na2 2.475(5) 16_565 ? F1 B1 1.359(10) . ? F2 B1 1.380(4) . ? F2 Na1 2.335(8) . ? Na1 F2 2.335(8) 17_655 ? 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 C1 O2 124.7(8) . . ? O3 C1 C2 117.7(6) . . ? O2 C1 C2 117.4(5) . . ? O1 C2 C1 109.3(3) . . ? O1 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? O1 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.3 . . ? C2 O1 C2 115.3(5) 12_455 . ? C2 O1 Pr1 122.4(3) 12_455 . ? C2 O1 Pr1 122.4(3) . . ? C1 O2 Pr1 128.1(4) . . ? C1 O3 Na2 144.1(5) . . ? C1 O3 Na1 121.9(5) . . ? Na2 O3 Na1 93.99(13) . . ? Na1 O4 Na2 99.10(15) . 16_565 ? B1 F2 Na1 130.1(5) . . ? O4 Na1 O4 163.9(3) 17_655 . ? O4 Na1 F2 90.6(2) . 17_655 ? O4 Na1 F2 100.9(2) . . ? F2 Na1 F2 88.7(2) 17_655 . ? O4 Na1 O3 82.04(15) . 17_655 ? F2 Na1 O3 173.9(2) . 17_655 ? O4 Na1 O3 82.03(15) 17_655 . ? O4 Na1 O3 87.60(14) . . ? F2 Na1 O3 173.9(2) 17_655 . ? F2 Na1 O3 85.92(13) . . ? O3 Na1 O3 99.6(2) 17_655 . ? O3 Na2 O3 104.61(14) . 3_675 ? O3 Na2 O4 85.76(14) . 18 ? O3 Na2 O4 163.75(16) . 16_665 ? O4 Na2 O4 82.84(14) 18 16_665 ? O3 Na2 O4 84.29(14) . 17_655 ? O3 Na2 O4 163.75(16) 3_675 17_655 ? O3 Na2 O4 85.76(14) 2_765 17_655 ? O4 Na2 O4 82.83(14) 16_665 17_655 ? O2 Pr1 O2 150.42(16) 10_565 2_665 ? O2 Pr1 O2 125.23(16) 11 2_665 ? O2 Pr1 O2 88.68(17) 11 3_565 ? O2 Pr1 O2 150.42(16) 11 . ? O2 Pr1 O2 125.24(16) 12_455 . ? O2 Pr1 O2 77.77(13) 2_665 . ? O2 Pr1 O2 77.78(13) 3_565 . ? O2 Pr1 O1 75.21(8) 10_565 . ? O2 Pr1 O1 135.66(8) 11 . ? O2 Pr1 O1 62.62(8) . . ? O1 Pr1 O1 120.000(1) . 3_565 ? F1 B1 F2 110.6(4) . . ? F2 B1 F2 108.3(4) 3_665 . ? F2 B1 F2 108.3(4) . 2_655 ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.705 _refine_diff_density_min -1.009 _refine_diff_density_rms 0.114 # Attachment '2_new.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 721017' _audit_creation_method SHELXL-97 _chemical_name_systematic ;Trisodium tris(2,2?-oxydiacetato)-gadolinium(III) hexaahydrate ; _chemical_name_common 'Trisodium tris(2,2?-oxydiacetato)-gadolinium(iii) hexaahydrate' _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 Gd Na3 O15, 8(H2 O)' _chemical_formula_sum 'C12 H28 Gd Na3 O23' _chemical_formula_weight 766.57 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' Gd Gd -0.1653 3.9035 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_space_group_name_Hall 'C -2yc' _symmetry_int_tables_number 9 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 17.535(4) _cell_length_b 8.4677(16) _cell_length_c 19.207(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.483(16) _cell_angle_gamma 90.00 _cell_volume 2653.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 289(2) _cell_measurement_reflns_used 7088 _cell_measurement_theta_min 4.24 _cell_measurement_theta_max 24.99 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.878 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1460 _exptl_absorpt_coefficient_mu 2.644 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4758 _exptl_absorpt_correction_T_max 0.7670 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 289(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'rotating anode' _diffrn_source_type RU-H3R _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS IIC image-plate system' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean 105 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7088 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.24 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3974 _reflns_number_gt 3871 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear(Rigaku, 2000)' _computing_cell_refinement 'CrystalClear(Rigaku, 2000)' _computing_data_reduction 'CrystalClear(Rigaku, 2000)' _computing_structure_solution 'CrystalClear(Rigaku, 2000)' _computing_structure_refinement 'SIR92 (Altomare et al., 1993)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) and PLUTON (Spek, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0401P)^2^+2.0052P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.315(9) _refine_ls_number_reflns 3974 _refine_ls_number_parameters 353 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0217 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0546 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_restrained_S_all 0.905 _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 O16 O 0.6882(5) 0.5328(6) 0.7531(4) 0.0717(18) Uani 1 1 d . . . O17 O 0.7746(3) 0.7192(6) 0.9300(3) 0.0421(12) Uani 1 1 d . . . O18 O 0.5553(4) 0.4264(6) 0.8344(3) 0.0360(12) Uani 1 1 d . . . O19 O 0.4893(4) 1.1064(7) 0.9222(3) 0.0462(13) Uani 1 1 d . . . O20 O 0.6583(3) 1.1593(6) 0.8879(3) 0.0399(12) Uani 1 1 d . . . O21 O 0.3766(3) 1.6401(7) 0.3603(3) 0.0447(13) Uani 1 1 d . . . O22 O 0.7730(3) 1.2505(8) 0.8208(3) 0.0551(15) Uani 1 1 d . . . O23 O 0.3945(4) 1.0035(7) 0.5012(3) 0.0609(13) Uani 1 1 d . . . Na3 Na 0.4862(2) 1.4349(3) 0.4059(2) 0.0241(7) Uani 1 1 d . . . C1 C 0.8747(4) 0.8961(9) 0.5139(4) 0.0223(11) Uani 1 1 d . . . C2 C 0.9269(6) 1.0296(9) 0.5606(6) 0.0302(18) Uani 1 1 d . . . H2A H 0.9811 0.9903 0.5902 0.036 Uiso 1 1 calc R . . H2B H 0.9327 1.1123 0.5280 0.036 Uiso 1 1 calc R . . C3 C 0.9445(4) 1.1701(7) 0.6723(3) 0.0250(14) Uani 1 1 d . . . H3A H 0.9573 1.2737 0.6579 0.030 Uiso 1 1 calc R . . H3B H 0.9951 1.1102 0.6921 0.030 Uiso 1 1 calc R . . C4 C 0.9072(4) 1.1869(7) 0.7319(4) 0.0204(14) Uani 1 1 d . . . C5 C 0.9111(4) 0.6870(9) 0.7100(4) 0.0244(14) Uani 1 1 d . . . C6 C 0.8456(6) 0.5719(8) 0.6624(6) 0.034(2) Uani 1 1 d . . . H6A H 0.8628 0.5247 0.6245 0.041 Uiso 1 1 calc R . . H6B H 0.8382 0.4880 0.6937 0.041 Uiso 1 1 calc R . . C7 C 0.7078(7) 0.5595(7) 0.5776(6) 0.037(2) Uani 1 1 d . . . H7A H 0.6925 0.4762 0.6046 0.045 Uiso 1 1 calc R . . H7B H 0.7264 0.5110 0.5408 0.045 Uiso 1 1 calc R . . C8 C 0.6357(5) 0.6624(8) 0.5393(4) 0.0273(16) Uani 1 1 d . . . C9 C 0.6368(4) 1.1864(7) 0.5038(4) 0.0187(13) Uani 1 1 d . . . C10 C 0.5952(4) 1.1778(7) 0.5602(3) 0.0204(12) Uani 1 1 d . . . H10A H 0.5829 1.2835 0.5725 0.024 Uiso 1 1 calc R . . H10B H 0.5441 1.1200 0.5390 0.024 Uiso 1 1 calc R . . C11 C 0.6098(6) 1.0553(7) 0.6750(6) 0.030(2) Uani 1 1 d . . . H11A H 0.5548 1.0191 0.6460 0.036 Uiso 1 1 calc R . . H11B H 0.6052 1.1466 0.7038 0.036 Uiso 1 1 calc R . . C12 C 0.6556(4) 0.9252(7) 0.7284(4) 0.0190(15) Uani 1 1 d . . . Gd1 Gd 0.76805(3) 0.947136(15) 0.62250(3) 0.01385(7) Uani 1 1 d . . . O1 O 0.8111(3) 0.8548(5) 0.5250(3) 0.0279(11) Uani 1 1 d . . . O2 O 0.8888(3) 1.0919(6) 0.6090(3) 0.0223(9) Uani 1 1 d . . . O3 O 0.8327(3) 1.1482(5) 0.7135(2) 0.0232(9) Uani 1 1 d . . . O4 O 0.9001(3) 0.8350(5) 0.4670(3) 0.0301(10) Uani 1 1 d . . . O5 O 0.9519(3) 1.2419(6) 0.7939(2) 0.0322(10) Uani 1 1 d . . . O6 O 0.8909(3) 0.8303(5) 0.7046(3) 0.0269(10) Uani 1 1 d . . . O7 O 0.7721(4) 0.6527(3) 0.6284(4) 0.0253(7) Uani 1 1 d . . . O8 O 0.6458(3) 0.8109(5) 0.5452(3) 0.0306(11) Uani 1 1 d . . . O9 O 0.9794(3) 0.6355(6) 0.7486(3) 0.0381(11) Uani 1 1 d . . . O10 O 0.5717(3) 0.5960(7) 0.5020(3) 0.0411(12) Uani 1 1 d . . . O11 O 0.7093(3) 1.1333(5) 0.5238(2) 0.0261(10) Uani 1 1 d . . . O12 O 0.6483(3) 1.0994(7) 0.6268(2) 0.0206(8) Uani 1 1 d . . . O13 O 0.7204(3) 0.8754(6) 0.7197(3) 0.0246(10) Uani 1 1 d . . . O14 O 0.5977(2) 1.2424(5) 0.4412(2) 0.0232(8) Uani 1 1 d . . . O15 O 0.6285(3) 0.8763(5) 0.7740(3) 0.0351(11) Uani 1 1 d . . . Na2 Na 0.5458(3) 0.9641(3) 0.8417(2) 0.0263(7) Uani 1 1 d . . . Na1 Na 0.64274(13) 0.6440(2) 0.84212(10) 0.0361(4) 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 O16 0.108(5) 0.049(3) 0.089(4) -0.001(2) 0.074(4) 0.000(3) O17 0.036(2) 0.056(3) 0.040(3) -0.0072(19) 0.0203(19) 0.009(2) O18 0.046(3) 0.025(2) 0.044(3) -0.0067(16) 0.025(2) -0.0040(17) O19 0.057(3) 0.031(2) 0.063(3) -0.006(2) 0.036(2) -0.001(2) O20 0.038(3) 0.052(3) 0.029(3) 0.0011(19) 0.012(2) 0.005(2) O21 0.044(3) 0.048(3) 0.037(3) 0.003(2) 0.010(3) 0.004(2) O22 0.042(3) 0.074(3) 0.057(3) -0.010(2) 0.026(2) 0.007(2) O23 0.063(3) 0.045(2) 0.083(4) -0.012(3) 0.037(3) -0.009(3) Na3 0.0215(13) 0.0284(12) 0.0257(14) -0.0008(9) 0.0127(11) 0.0000(9) C1 0.018(3) 0.030(3) 0.022(3) 0.003(3) 0.010(2) 0.004(3) C2 0.030(4) 0.045(3) 0.027(3) -0.006(3) 0.024(3) 0.001(3) C3 0.023(3) 0.027(3) 0.025(3) -0.005(2) 0.008(2) -0.011(2) C4 0.023(3) 0.012(3) 0.019(3) 0.001(2) 0.000(2) -0.005(2) C5 0.017(3) 0.037(3) 0.020(3) 0.004(2) 0.009(2) 0.003(2) C6 0.035(4) 0.022(3) 0.048(4) 0.009(3) 0.018(3) 0.015(3) C7 0.044(5) 0.022(3) 0.043(4) -0.011(2) 0.014(4) -0.005(2) C8 0.027(3) 0.032(3) 0.025(3) -0.014(2) 0.011(3) -0.013(3) C9 0.021(3) 0.016(2) 0.022(3) 0.002(2) 0.011(2) -0.004(2) C10 0.013(2) 0.027(3) 0.019(3) 0.0079(19) 0.0028(19) 0.001(2) C11 0.023(3) 0.039(4) 0.035(4) 0.020(2) 0.018(3) 0.018(2) C12 0.027(3) 0.016(2) 0.017(3) -0.0012(18) 0.012(3) 0.000(2) Gd1 0.01225(9) 0.01519(10) 0.01377(10) 0.00095(11) 0.00437(6) 0.00088(11) O1 0.030(2) 0.033(2) 0.028(2) -0.0092(16) 0.019(2) -0.0065(18) O2 0.016(2) 0.0275(17) 0.021(2) -0.0054(19) 0.0043(17) -0.0032(18) O3 0.022(2) 0.0259(19) 0.024(2) -0.0077(14) 0.0105(17) -0.0026(15) O4 0.036(2) 0.031(2) 0.035(2) -0.0073(15) 0.0257(18) 0.0008(16) O5 0.039(2) 0.0335(19) 0.0206(19) -0.0036(15) 0.0061(17) -0.0148(17) O6 0.025(2) 0.016(2) 0.030(2) 0.0035(16) -0.0019(18) 0.0064(15) O7 0.0195(13) 0.0171(11) 0.0361(19) -0.0027(19) 0.0065(14) 0.0012(19) O8 0.018(2) 0.032(3) 0.036(3) -0.003(2) 0.0025(19) -0.0040(18) O9 0.0203(19) 0.045(3) 0.043(2) 0.0123(18) 0.0048(17) 0.0132(18) O10 0.025(2) 0.051(3) 0.042(3) -0.017(2) 0.0062(19) -0.015(2) O11 0.0209(19) 0.033(2) 0.027(2) 0.0114(16) 0.0115(17) 0.0089(16) O12 0.019(2) 0.0291(19) 0.0173(19) 0.0056(17) 0.0112(16) 0.0073(19) O13 0.024(2) 0.028(2) 0.024(2) 0.0099(16) 0.0119(19) 0.0099(16) O14 0.0210(16) 0.0282(17) 0.0171(18) 0.0064(14) 0.0032(14) 0.0047(14) O15 0.047(2) 0.032(2) 0.039(2) 0.0139(18) 0.030(2) 0.0107(19) Na2 0.0299(15) 0.0241(11) 0.0231(14) 0.0009(9) 0.0075(11) 0.0056(9) Na1 0.0511(11) 0.0281(9) 0.0349(10) -0.0009(8) 0.0226(9) -0.0029(8) _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 O16 Na1 2.334(5) . ? O17 Na1 2.397(6) . ? O18 Na1 2.367(6) . ? O19 Na2 2.439(6) . ? O20 Na2 2.476(7) . ? O21 Na3 2.500(7) . ? Na3 O14 2.443(5) . ? C1 O4 1.255(8) . ? C1 O1 1.259(8) . ? C1 C2 1.522(11) . ? C2 O2 1.428(10) . ? C3 O2 1.415(8) . ? C3 C4 1.520(9) . ? C4 O5 1.250(8) . ? C4 O3 1.265(8) . ? C5 O9 1.233(9) . ? C5 O6 1.258(8) . ? C5 C6 1.528(12) . ? C6 O7 1.392(10) . ? C7 O7 1.429(11) . ? C7 C8 1.489(12) . ? C8 O10 1.224(9) . ? C8 O8 1.269(8) . ? C9 O14 1.240(8) . ? C9 O11 1.268(8) . ? C9 C10 1.512(9) . ? C10 O12 1.440(7) . ? C11 O12 1.383(10) . ? C11 C12 1.519(9) . ? C12 O15 1.212(8) . ? C12 O13 1.278(8) . ? Gd1 O6 2.370(5) . ? Gd1 O13 2.387(4) . ? Gd1 O11 2.390(4) . ? Gd1 O1 2.393(4) . ? Gd1 O3 2.406(4) . ? Gd1 O8 2.409(5) . ? Gd1 O7 2.496(3) . ? Gd1 O12 2.491(5) . ? Gd1 O2 2.541(5) . ? O15 Na1 2.325(4) . ? O15 Na2 2.393(6) . ? 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 Na1 O18 Na3 91.93(19) . 2_575 ? O10 Na3 O4 99.1(2) 1_565 3_455 ? O10 Na3 O14 87.3(2) 1_565 . ? O4 Na3 O14 102.32(18) 3_455 . ? O10 Na3 O18 81.7(2) 1_565 2_574 ? O4 Na3 O18 169.6(2) 3_455 2_574 ? O14 Na3 O18 88.0(2) . 2_574 ? O10 Na3 O21 93.4(2) 1_565 . ? O4 Na3 O21 82.8(2) 3_455 . ? O14 Na3 O21 174.6(3) . . ? O18 Na3 O21 86.8(2) 2_574 . ? O10 Na3 O5 155.1(2) 1_565 4_474 ? O4 Na3 O5 102.4(2) 3_455 4_474 ? O14 Na3 O5 75.87(15) . 4_474 ? O18 Na3 O5 79.4(2) 2_574 4_474 ? O21 Na3 O5 101.6(2) . 4_474 ? O10 Na3 Na1 91.67(18) 1_565 2_574 ? O4 Na3 Na1 146.62(15) 3_455 2_574 ? O14 Na3 Na1 46.41(12) . 2_574 ? O18 Na3 Na1 43.19(14) 2_574 2_574 ? O21 Na3 Na1 128.2(2) . 2_574 ? O5 Na3 Na1 63.41(13) 4_474 2_574 ? O10 Na3 Na2 126.14(16) 1_565 2_574 ? O4 Na3 Na2 98.08(13) 3_455 2_574 ? O14 Na3 Na2 39.08(14) . 2_574 ? O18 Na3 Na2 89.59(14) 2_574 2_574 ? O21 Na3 Na2 139.27(18) . 2_574 ? O5 Na3 Na2 38.09(12) 4_474 2_574 ? Na1 Na3 Na2 51.38(5) 2_574 2_574 ? O4 C1 O1 125.2(6) . . ? O4 C1 C2 115.8(6) . . ? O1 C1 C2 119.0(6) . . ? O2 C2 C1 109.6(7) . . ? O2 C3 C4 109.8(5) . . ? O5 C4 O3 125.8(6) . . ? O5 C4 C3 117.4(6) . . ? O3 C4 C3 116.8(6) . . ? O9 C5 O6 124.9(7) . . ? O9 C5 C6 119.0(7) . . ? O6 C5 C6 116.0(6) . . ? O7 C6 C5 109.3(5) . . ? O7 C7 C8 109.2(5) . . ? O10 C8 O8 125.1(7) . . ? O10 C8 C7 116.8(6) . . ? O8 C8 C7 118.1(7) . . ? O14 C9 O11 124.4(6) . . ? O14 C9 C10 118.2(6) . . ? O11 C9 C10 117.4(6) . . ? O12 C10 C9 109.5(5) . . ? O12 C11 C12 112.4(6) . . ? O15 C12 O13 125.7(6) . . ? O15 C12 C11 119.0(6) . . ? O13 C12 C11 115.3(6) . . ? O6 Gd1 O13 82.32(17) . . ? O6 Gd1 O11 145.68(17) . . ? O13 Gd1 O11 128.03(15) . . ? O6 Gd1 O1 85.05(18) . . ? O13 Gd1 O1 146.16(11) . . ? O11 Gd1 O1 76.26(16) . . ? O6 Gd1 O3 74.96(15) . . ? O13 Gd1 O3 79.54(17) . . ? O11 Gd1 O3 93.50(11) . . ? O1 Gd1 O3 126.86(15) . . ? O6 Gd1 O8 126.66(11) . . ? O13 Gd1 O8 82.71(17) . . ? O11 Gd1 O8 78.41(16) . . ? O1 Gd1 O8 79.97(17) . . ? O3 Gd1 O8 149.68(16) . . ? O6 Gd1 O7 63.17(17) . . ? O13 Gd1 O7 73.91(19) . . ? O11 Gd1 O7 133.79(18) . . ? O1 Gd1 O7 72.36(18) . . ? O3 Gd1 O7 132.53(17) . . ? O8 Gd1 O7 63.50(18) . . ? O6 Gd1 O12 139.95(16) . . ? O13 Gd1 O12 64.20(14) . . ? O11 Gd1 O12 63.99(14) . . ? O1 Gd1 O12 134.99(16) . . ? O3 Gd1 O12 77.76(16) . . ? O8 Gd1 O12 72.42(17) . . ? O7 Gd1 O12 121.76(19) . . ? O6 Gd1 O2 71.42(17) . . ? O13 Gd1 O2 138.28(17) . . ? O11 Gd1 O2 74.54(16) . . ? O1 Gd1 O2 64.13(15) . . ? O3 Gd1 O2 62.89(15) . . ? O8 Gd1 O2 139.01(16) . . ? O7 Gd1 O2 118.39(18) . . ? O12 Gd1 O2 119.84(9) . . ? C1 O1 Gd1 126.5(4) . . ? C3 O2 C2 113.0(6) . . ? C3 O2 Gd1 118.5(4) . . ? C2 O2 Gd1 119.6(4) . . ? C4 O3 Gd1 123.4(4) . . ? C1 O4 Na3 131.6(4) . 3_545 ? C4 O5 Na2 138.1(4) . 3 ? C4 O5 Na3 117.7(4) . 4_575 ? Na2 O5 Na3 102.7(2) 3 4_575 ? C5 O6 Gd1 128.1(4) . . ? C6 O7 C7 114.4(4) . . ? C6 O7 Gd1 121.2(4) . . ? C7 O7 Gd1 121.2(4) . . ? C8 O8 Gd1 126.4(5) . . ? C5 O9 Na2 143.7(5) . 3_545 ? C8 O10 Na3 156.0(5) . 1_545 ? C9 O11 Gd1 124.5(4) . . ? C11 O12 C10 113.8(6) . . ? C11 O12 Gd1 120.5(4) . . ? C10 O12 Gd1 119.2(3) . . ? C12 O13 Gd1 126.9(4) . . ? C9 O14 Na3 128.8(4) . . ? C9 O14 Na1 131.9(4) . 2_574 ? Na3 O14 Na1 88.62(16) . 2_574 ? C9 O14 Na2 113.0(4) . 2_574 ? Na3 O14 Na2 102.9(2) . 2_574 ? Na1 O14 Na2 79.38(16) 2_574 2_574 ? C12 O15 Na1 134.9(4) . . ? C12 O15 Na2 139.7(4) . . ? Na1 O15 Na2 85.32(16) . . ? O9 Na2 O15 90.5(2) 3_455 . ? O9 Na2 O19 88.5(2) 3_455 . ? O15 Na2 O19 164.9(3) . . ? O9 Na2 O5 96.6(2) 3_455 3_445 ? O15 Na2 O5 90.91(19) . 3_445 ? O19 Na2 O5 104.1(2) . 3_445 ? O9 Na2 O20 88.1(2) 3_455 . ? O15 Na2 O20 80.8(2) . . ? O19 Na2 O20 84.2(2) . . ? O5 Na2 O20 170.5(2) 3_445 . ? O9 Na2 O14 171.2(3) 3_455 2_575 ? O15 Na2 O14 94.29(18) . 2_575 ? O19 Na2 O14 88.8(2) . 2_575 ? O5 Na2 O14 75.89(16) 3_445 2_575 ? O20 Na2 O14 100.0(2) . 2_575 ? O9 Na2 Na1 131.6(2) 3_455 . ? O15 Na2 Na1 46.44(12) . . ? O19 Na2 Na1 139.2(2) . . ? O5 Na2 Na1 68.49(13) 3_445 . ? O20 Na2 Na1 102.23(19) . . ? O14 Na2 Na1 50.33(11) 2_575 . ? O9 Na2 Na3 133.64(17) 3_455 2_575 ? O15 Na2 Na3 100.98(14) . 2_575 ? O19 Na2 Na3 90.55(18) . 2_575 ? O5 Na2 Na3 39.21(15) 3_445 2_575 ? O20 Na2 Na3 137.87(16) . 2_575 ? O14 Na2 Na3 37.99(13) 2_575 2_575 ? Na1 Na2 Na3 57.63(9) . 2_575 ? O15 Na1 O16 85.65(19) . . ? O15 Na1 O18 133.6(2) . . ? O16 Na1 O18 91.6(2) . . ? O15 Na1 O17 92.8(2) . . ? O16 Na1 O17 97.0(3) . . ? O18 Na1 O17 133.4(2) . . ? O15 Na1 O14 95.96(16) . 2_575 ? O16 Na1 O14 177.9(2) . 2_575 ? O18 Na1 O14 88.26(16) . 2_575 ? O17 Na1 O14 81.63(17) . 2_575 ? O15 Na1 Na2 48.24(13) . . ? O16 Na1 Na2 131.62(19) . . ? O18 Na1 Na2 109.15(17) . . ? O17 Na1 Na2 98.73(15) . . ? O14 Na1 Na2 50.29(13) 2_575 . ? O15 Na1 Na3 115.31(14) . 2_575 ? O16 Na1 Na3 135.29(19) . 2_575 ? O18 Na1 Na3 44.88(14) . 2_575 ? O17 Na1 Na3 119.25(16) . 2_575 ? O14 Na1 Na3 44.97(11) 2_575 2_575 ? Na2 Na1 Na3 70.99(10) . 2_575 ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 0.466 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.072 # Attachment '3_new.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 721018' _chemical_name_systematic ;Ammonium trisodium tris(2,2?-oxydiacetato)-praseodymium(III)tiocyanate tetraahydrate ; _audit_creation_method SHELXL-97 _chemical_name_common ; Ammonium trisodium tris(2,2?-oxydiacetato)- praseodymium(iii)tiocyanate tetraahydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C13 H24 N2 Na3 O19 Pr S' _chemical_formula_sum 'C13 H24 N2 Na3 O19 Pr S' _chemical_formula_weight 754.29 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 '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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1741(11) _cell_length_b 9.3387(16) _cell_length_c 17.7642(16) _cell_angle_alpha 83.75(2) _cell_angle_beta 72.724(10) _cell_angle_gamma 86.44(2) _cell_volume 1443.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 289(2) _cell_measurement_reflns_used 8956 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 24.99 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 1.885 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5314 _exptl_absorpt_correction_T_max 0.7500 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 289(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'rotating anode' _diffrn_source_type RU-H3R _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS IIC image-plate system' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean 105 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8956 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_sigmaI/netI 0.0692 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4584 _reflns_number_gt 4293 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear(Rigaku, 2000)' _computing_cell_refinement 'CrystalClear(Rigaku, 2000)' _computing_data_reduction 'CrystalClear(Rigaku, 2000)' _computing_structure_solution 'CrystalClear(Rigaku, 2000)' _computing_structure_refinement 'SIR92 (Altomare et al., 1993)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) and PLUTON (Spek, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0589P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4584 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0951 _refine_ls_wR_factor_gt 0.0941 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.003 _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 C1 C 0.6695(4) 0.2054(4) 0.8264(3) 0.0266(9) Uani 1 1 d . . . C2 C 0.5659(5) 0.2371(5) 0.9167(3) 0.0327(10) Uani 1 1 d . . . H2A H 0.5220 0.1490 0.9467 0.039 Uiso 1 1 calc R . . H2B H 0.6276 0.2774 0.9446 0.039 Uiso 1 1 calc R . . C3 C 0.3402(5) 0.3659(4) 0.9872(2) 0.0315(9) Uani 1 1 d . . . H3A H 0.2864 0.2795 1.0132 0.038 Uiso 1 1 calc R . . H3B H 0.3958 0.3975 1.0208 0.038 Uiso 1 1 calc R . . C4 C 0.2298(4) 0.4836(4) 0.9700(2) 0.0229(8) Uani 1 1 d . . . C5 C 0.7118(4) 0.6998(4) 0.7703(2) 0.0231(8) Uani 1 1 d . . . C6 C 0.6110(4) 0.8110(4) 0.7366(3) 0.0324(10) Uani 1 1 d . . . H6A H 0.5832 0.8905 0.7695 0.039 Uiso 1 1 calc R . . H6B H 0.6676 0.8489 0.6836 0.039 Uiso 1 1 calc R . . C7 C 0.3954(4) 0.8380(4) 0.6838(3) 0.0268(9) Uani 1 1 d . . . H7A H 0.4658 0.8640 0.6320 0.032 Uiso 1 1 calc R . . H7B H 0.3558 0.9259 0.7082 0.032 Uiso 1 1 calc R . . C8 C 0.2650(4) 0.7547(4) 0.6753(2) 0.0205(8) Uani 1 1 d . . . C9 C 0.2436(4) 0.2327(4) 0.7045(3) 0.0273(9) Uani 1 1 d . . . C10 C 0.3719(5) 0.2371(4) 0.6185(3) 0.0341(10) Uani 1 1 d . . . H10A H 0.4265 0.1449 0.6114 0.041 Uiso 1 1 calc R . . H10B H 0.3248 0.2597 0.5763 0.041 Uiso 1 1 calc R . . C11 C 0.6023(4) 0.3545(4) 0.5424(2) 0.0258(9) Uani 1 1 d . . . H11A H 0.6615 0.2645 0.5373 0.031 Uiso 1 1 calc R . . H11B H 0.5642 0.3752 0.4968 0.031 Uiso 1 1 calc R . . C12 C 0.6978(4) 0.4749(4) 0.5487(2) 0.0251(9) Uani 1 1 d . . . C13 C 0.1571(5) 0.8983(4) 0.8847(3) 0.0326(10) Uani 1 1 d . . . N1 N 0.0650(5) 0.8505(4) 0.8622(3) 0.0434(10) Uani 1 1 d . . . O1 O 0.6382(3) 0.2678(3) 0.75840(19) 0.0317(7) Uani 1 1 d . . . O2 O 0.4493(3) 0.3377(3) 0.90554(16) 0.0281(6) Uani 1 1 d . . . O3 O 0.2441(3) 0.5282(3) 0.89058(17) 0.0303(6) Uani 1 1 d . . . O4 O 0.7802(4) 0.1226(3) 0.8255(2) 0.0426(8) Uani 1 1 d . . . O5 O 0.1338(3) 0.5241(3) 1.03665(17) 0.0334(7) Uani 1 1 d . . . O6 O 0.6583(3) 0.5771(3) 0.80007(18) 0.0286(6) Uani 1 1 d . . . O7 O 0.4773(3) 0.7464(3) 0.73407(18) 0.0250(6) Uani 1 1 d . . . O8 O 0.2571(3) 0.6227(3) 0.70251(17) 0.0265(6) Uani 1 1 d . . . O9 O 0.8425(3) 0.7353(3) 0.7645(2) 0.0376(8) Uani 1 1 d . . . O10 O 0.1731(3) 0.8233(3) 0.64066(18) 0.0308(7) Uani 1 1 d . . . O11 O 0.2579(3) 0.3041(3) 0.76460(19) 0.0317(7) Uani 1 1 d . . . O12 O 0.4718(3) 0.3459(3) 0.61825(16) 0.0275(6) Uani 1 1 d . . . O13 O 0.6537(3) 0.5420(3) 0.61701(19) 0.0404(8) Uani 1 1 d . . . O14 O 0.1330(3) 0.1599(3) 0.7106(2) 0.0482(9) Uani 1 1 d . . . O15 O 0.8132(3) 0.5017(3) 0.48482(19) 0.0390(8) Uani 1 1 d . . . O16 O 0.7311(4) 0.9814(3) 0.5140(2) 0.0472(8) Uani 1 1 d . . . O17 O -0.0658(4) 0.7470(3) 0.5106(2) 0.0445(8) Uani 1 1 d . . . O18 O -0.0522(3) 0.4347(3) 0.7385(2) 0.0463(9) Uani 1 1 d . . . O19 O 0.8500(4) 0.1071(3) 0.6281(2) 0.0400(8) Uani 1 1 d . . . N2 N 0.0013(4) 0.2126(4) 0.9124(2) 0.0393(9) Uani 1 1 d . . . S1 S 0.28425(16) 0.96940(15) 0.91944(10) 0.0548(4) Uani 1 1 d . . . Pr1 Pr 0.453829(18) 0.473221(17) 0.756330(11) 0.01729(11) Uani 1 1 d . . . Na1 Na 0.02091(17) 0.60233(17) 0.83614(10) 0.0319(4) Uani 1 1 d . . . Na2 Na 0.96443(16) -0.02968(16) 0.73585(12) 0.0311(4) Uani 1 1 d . . . Na3 Na 0.02948(19) 0.62731(17) 0.62484(10) 0.0346(4) 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 C1 0.022(2) 0.016(2) 0.041(3) -0.0034(17) -0.0087(18) 0.0022(14) C2 0.025(2) 0.036(2) 0.036(2) 0.0004(18) -0.0118(18) 0.0106(16) C3 0.027(2) 0.038(2) 0.025(2) -0.0025(17) -0.0032(17) 0.0089(16) C4 0.0182(18) 0.018(2) 0.032(2) -0.0048(15) -0.0045(16) -0.0044(14) C5 0.0148(18) 0.020(2) 0.036(2) -0.0057(16) -0.0083(16) -0.0048(14) C6 0.0206(19) 0.022(2) 0.056(3) 0.0002(18) -0.0151(19) -0.0058(14) C7 0.0170(18) 0.025(2) 0.037(2) 0.0051(17) -0.0089(17) -0.0006(14) C8 0.0178(18) 0.018(2) 0.024(2) -0.0016(14) -0.0040(15) 0.0013(13) C9 0.0204(19) 0.0123(19) 0.049(3) 0.0002(16) -0.0111(18) -0.0022(14) C10 0.032(2) 0.023(2) 0.049(3) -0.0076(18) -0.010(2) -0.0122(16) C11 0.0220(19) 0.022(2) 0.031(2) -0.0071(16) -0.0037(16) 0.0011(14) C12 0.0211(19) 0.023(2) 0.028(2) -0.0014(16) -0.0028(16) 0.0014(14) C13 0.034(2) 0.026(2) 0.037(2) -0.0033(18) -0.0103(19) 0.0065(17) N1 0.045(2) 0.029(2) 0.063(3) -0.0095(19) -0.026(2) 0.0051(17) O1 0.0263(15) 0.0260(16) 0.0398(17) -0.0036(13) -0.0069(13) 0.0087(11) O2 0.0212(13) 0.0294(15) 0.0277(15) 0.0006(11) -0.0018(11) 0.0124(10) O3 0.0239(14) 0.0275(15) 0.0336(16) 0.0010(12) -0.0026(12) 0.0071(11) O4 0.0299(16) 0.0378(18) 0.059(2) -0.0094(15) -0.0136(15) 0.0199(13) O5 0.0259(15) 0.0301(16) 0.0362(17) -0.0050(12) 0.0025(13) 0.0053(11) O6 0.0183(13) 0.0246(15) 0.0463(18) 0.0000(12) -0.0151(12) -0.0043(10) O7 0.0175(13) 0.0128(14) 0.0473(17) 0.0016(11) -0.0146(12) -0.0017(9) O8 0.0211(13) 0.0160(14) 0.0430(17) 0.0022(11) -0.0117(12) -0.0026(10) O9 0.0194(15) 0.0241(16) 0.072(2) -0.0031(15) -0.0183(15) -0.0024(11) O10 0.0219(14) 0.0286(16) 0.0459(18) 0.0005(13) -0.0182(13) 0.0035(11) O11 0.0227(14) 0.0247(16) 0.0458(18) -0.0025(13) -0.0056(13) -0.0102(11) O12 0.0219(13) 0.0243(15) 0.0348(16) -0.0075(11) -0.0029(12) -0.0087(10) O13 0.0355(17) 0.0353(18) 0.0411(18) -0.0154(13) 0.0105(14) -0.0181(13) O14 0.0251(16) 0.0307(18) 0.087(3) -0.0056(17) -0.0114(17) -0.0152(13) O15 0.0270(15) 0.0368(18) 0.0434(19) -0.0115(14) 0.0090(14) -0.0105(12) O16 0.050(2) 0.0373(19) 0.056(2) 0.0002(15) -0.0179(17) -0.0065(14) O17 0.0414(19) 0.0362(18) 0.059(2) -0.0022(15) -0.0181(16) -0.0078(14) O18 0.0236(16) 0.0280(16) 0.080(3) 0.0030(16) -0.0064(16) -0.0022(11) O19 0.0360(17) 0.0357(19) 0.049(2) -0.0032(14) -0.0137(15) 0.0000(13) N2 0.034(2) 0.030(2) 0.047(2) -0.0021(16) -0.0045(17) 0.0081(14) S1 0.0461(7) 0.0503(8) 0.0796(10) -0.0106(7) -0.0350(7) 0.0004(6) Pr1 0.01197(13) 0.01445(15) 0.02403(16) -0.00090(9) -0.00330(9) -0.00114(8) Na1 0.0236(8) 0.0287(9) 0.0408(10) 0.0033(7) -0.0077(7) -0.0018(6) Na2 0.0213(8) 0.0210(9) 0.0522(10) -0.0049(7) -0.0121(7) -0.0004(6) Na3 0.0323(9) 0.0297(9) 0.0383(9) -0.0066(7) -0.0032(7) -0.0031(7) _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 C1 O4 1.236(5) . ? C1 O1 1.383(6) . ? C1 C2 1.651(6) . ? C2 O2 1.424(4) . ? C3 C4 1.517(6) . ? C3 O2 1.537(4) . ? C4 O5 1.325(5) . ? C4 O3 1.397(5) . ? C5 O9 1.236(5) . ? C5 O6 1.272(5) . ? C5 C6 1.538(6) . ? C6 O7 1.414(5) . ? C7 O7 1.498(5) . ? C7 C8 1.519(5) . ? C8 O8 1.272(5) . ? C8 O10 1.287(5) . ? C8 Na3 2.931(4) . ? C9 O14 1.228(5) . ? C9 O11 1.360(5) . ? C9 C10 1.627(6) . ? C10 O12 1.408(4) . ? C11 C12 1.501(5) . ? C11 O12 1.512(4) . ? C12 O15 1.315(5) . ? C12 O13 1.368(5) . ? C13 N1 1.165(6) . ? C13 S1 1.672(5) . ? N1 Na1 2.492(4) . ? O1 Pr1 2.482(3) . ? O2 Pr1 2.800(3) . ? O3 Na1 2.542(3) . ? O3 Pr1 2.659(3) . ? O4 Na2 2.452(3) . ? O6 Pr1 2.514(3) . ? O7 Pr1 2.551(3) . ? O8 Pr1 2.558(3) . ? O8 Na1 2.695(3) . ? O8 Na3 2.820(3) . ? O10 Na3 2.407(3) . ? O11 Pr1 2.427(3) . ? O12 Pr1 2.798(3) . ? O13 Pr1 2.647(3) . ? O17 Na3 2.563(4) . ? O18 Na3 2.520(4) . ? O18 Na1 2.706(4) . ? O19 Na2 2.626(4) . ? Pr1 Na1 3.9587(17) . ? Na1 Na3 3.713(3) . ? 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 O4 C1 O1 123.2(4) . . ? O4 C1 C2 113.1(4) . . ? O1 C1 C2 123.7(3) . . ? O2 C2 C1 104.9(3) . . ? C4 C3 O2 104.8(3) . . ? O5 C4 O3 132.0(4) . . ? O5 C4 C3 110.8(4) . . ? O3 C4 C3 117.2(3) . . ? O9 C5 O6 124.2(4) . . ? O9 C5 C6 117.0(3) . . ? O6 C5 C6 118.8(3) . . ? O7 C6 C5 110.3(3) . . ? O7 C7 C8 109.3(3) . . ? O8 C8 O10 125.7(4) . . ? O8 C8 C7 117.0(3) . . ? O10 C8 C7 117.3(3) . . ? O8 C8 Na3 72.4(2) . . ? O10 C8 Na3 53.8(2) . . ? C7 C8 Na3 167.7(3) . . ? O14 C9 O11 123.0(4) . . ? O14 C9 C10 114.4(4) . . ? O11 C9 C10 122.6(3) . . ? O12 C10 C9 105.6(3) . . ? C12 C11 O12 105.4(3) . . ? O15 C12 O13 129.3(4) . . ? O15 C12 C11 113.0(3) . . ? O13 C12 C11 117.6(3) . . ? N1 C13 S1 178.0(4) . . ? C13 N1 Na1 133.0(4) . . ? C13 N1 Na2 125.4(4) . 1_465 ? Na1 N1 Na2 91.40(15) . 1_465 ? C1 O1 Pr1 123.7(2) . . ? C2 O2 C3 108.5(3) . . ? C2 O2 Pr1 122.3(2) . . ? C3 O2 Pr1 128.9(2) . . ? C4 O3 Na1 124.4(2) . . ? C4 O3 Pr1 132.7(2) . . ? Na1 O3 Pr1 99.10(11) . . ? C1 O4 Na2 140.0(3) . . ? C4 O5 Na1 135.5(3) . 2_567 ? C5 O6 Pr1 120.9(3) . . ? C6 O7 C7 112.1(3) . . ? C6 O7 Pr1 120.5(2) . . ? C7 O7 Pr1 121.7(2) . . ? C8 O8 Pr1 127.0(2) . . ? C8 O8 Na1 107.2(2) . . ? Pr1 O8 Na1 97.77(10) . . ? C8 O8 Na3 82.1(2) . . ? Pr1 O8 Na3 147.44(11) . . ? Na1 O8 Na3 84.59(9) . . ? C5 O9 Na2 132.4(3) . 1_565 ? C5 O9 Na1 125.4(3) . 1_655 ? Na2 O9 Na1 97.87(12) 1_565 1_655 ? C5 O9 Na3 105.4(3) . 1_655 ? Na2 O9 Na3 94.07(12) 1_565 1_655 ? Na1 O9 Na3 87.56(10) 1_655 1_655 ? C8 O10 Na3 100.6(2) . . ? C8 O10 Na2 112.2(2) . 1_465 ? Na3 O10 Na2 101.53(11) . 1_465 ? C9 O11 Pr1 126.4(2) . . ? C10 O12 C11 110.5(3) . . ? C10 O12 Pr1 121.2(2) . . ? C11 O12 Pr1 126.8(2) . . ? C12 O13 Pr1 131.8(2) . . ? C9 O14 Na2 163.6(3) . 1_455 ? C12 O15 Na3 137.8(2) . 2_666 ? Na3 O18 Na1 90.47(11) . . ? O11 Pr1 O1 89.43(10) . . ? O11 Pr1 O6 155.06(11) . . ? O1 Pr1 O6 76.36(10) . . ? O11 Pr1 O7 135.96(9) . . ? O1 Pr1 O7 134.07(9) . . ? O6 Pr1 O7 63.26(9) . . ? O11 Pr1 O8 75.66(9) . . ? O1 Pr1 O8 153.86(10) . . ? O6 Pr1 O8 124.61(9) . . ? O7 Pr1 O8 61.55(8) . . ? O11 Pr1 O13 118.74(10) . . ? O1 Pr1 O13 81.92(11) . . ? O6 Pr1 O13 79.94(10) . . ? O7 Pr1 O13 70.78(9) . . ? O8 Pr1 O13 86.58(10) . . ? O11 Pr1 O3 77.74(10) . . ? O1 Pr1 O3 118.88(9) . . ? O6 Pr1 O3 91.16(9) . . ? O7 Pr1 O3 84.31(9) . . ? O8 Pr1 O3 79.30(9) . . ? O13 Pr1 O3 154.98(9) . . ? O11 Pr1 O12 63.24(9) . . ? O1 Pr1 O12 76.66(10) . . ? O6 Pr1 O12 130.50(8) . . ? O7 Pr1 O12 113.31(9) . . ? O8 Pr1 O12 77.46(9) . . ? O13 Pr1 O12 55.72(8) . . ? O3 Pr1 O12 138.31(8) . . ? O11 Pr1 O2 83.95(10) . . ? O1 Pr1 O2 63.52(9) . . ? O6 Pr1 O2 71.42(9) . . ? O7 Pr1 O2 117.92(9) . . ? O8 Pr1 O2 133.86(8) . . ? O13 Pr1 O2 139.03(10) . . ? O3 Pr1 O2 55.88(8) . . ? O12 Pr1 O2 128.32(8) . . ? O11 Pr1 Na1 61.78(7) . . ? O1 Pr1 Na1 144.52(7) . . ? O6 Pr1 Na1 121.18(7) . . ? O7 Pr1 Na1 78.90(6) . . ? O8 Pr1 Na1 42.43(7) . . ? O13 Pr1 Na1 128.85(9) . . ? O3 Pr1 Na1 39.34(7) . . ? O12 Pr1 Na1 104.66(6) . . ? O2 Pr1 Na1 91.47(6) . . ? N1 Na1 O5 107.87(14) . 2_567 ? N1 Na1 O3 84.95(13) . . ? O5 Na1 O3 83.86(11) 2_567 . ? N1 Na1 O9 82.90(13) . 1_455 ? O5 Na1 O9 109.30(12) 2_567 1_455 ? O3 Na1 O9 164.32(12) . 1_455 ? N1 Na1 O8 90.34(13) . . ? O5 Na1 O8 153.69(11) 2_567 . ? O3 Na1 O8 78.91(10) . . ? O9 Na1 O8 91.27(11) 1_455 . ? N1 Na1 O18 147.01(15) . . ? O5 Na1 O18 96.92(11) 2_567 . ? O3 Na1 O18 119.81(11) . . ? O9 Na1 O18 68.28(11) 1_455 . ? O8 Na1 O18 75.12(10) . . ? N1 Na1 Na3 105.83(12) . . ? O5 Na1 Na3 136.45(10) 2_567 . ? O3 Na1 Na3 126.07(8) . . ? O9 Na1 Na3 49.20(9) 1_455 . ? O8 Na1 Na3 49.13(7) . . ? O18 Na1 Na3 42.74(8) . . ? N1 Na1 Na2 47.30(11) . 1_465 ? O5 Na1 Na2 130.60(9) 2_567 1_465 ? O3 Na1 Na2 124.54(9) . 1_465 ? O9 Na1 Na2 40.21(7) 1_455 1_465 ? O8 Na1 Na2 75.71(7) . 1_465 ? O18 Na1 Na2 99.91(9) . 1_465 ? Na3 Na1 Na2 62.16(5) . 1_465 ? N1 Na1 Pr1 97.83(11) . . ? O5 Na1 Pr1 116.78(9) 2_567 . ? O3 Na1 Pr1 41.55(6) . . ? O9 Na1 Pr1 130.91(9) 1_455 . ? O8 Na1 Pr1 39.80(6) . . ? O18 Na1 Pr1 89.72(8) . . ? Na3 Na1 Pr1 84.53(4) . . ? Na2 Na1 Pr1 109.42(5) 1_465 . ? O14 Na2 O4 86.66(13) 1_655 . ? O14 Na2 O9 166.05(13) 1_655 1_545 ? O4 Na2 O9 103.19(13) . 1_545 ? O14 Na2 O10 89.28(12) 1_655 1_645 ? O4 Na2 O10 175.89(12) . 1_645 ? O9 Na2 O10 80.69(10) 1_545 1_645 ? O14 Na2 O19 86.88(13) 1_655 . ? O4 Na2 O19 83.74(12) . . ? O9 Na2 O19 103.81(12) 1_545 . ? O10 Na2 O19 96.73(12) 1_645 . ? O14 Na2 N1 91.53(15) 1_655 1_645 ? O4 Na2 N1 89.26(14) . 1_645 ? O9 Na2 N1 78.91(13) 1_545 1_645 ? O10 Na2 N1 90.17(12) 1_645 1_645 ? O19 Na2 N1 172.90(12) . 1_645 ? O14 Na2 Na1 125.22(11) 1_655 1_645 ? O4 Na2 Na1 112.13(11) . 1_645 ? O9 Na2 Na1 41.93(8) 1_545 1_645 ? O10 Na2 Na1 69.80(8) 1_645 1_645 ? O19 Na2 Na1 143.48(9) . 1_645 ? N1 Na2 Na1 41.30(9) 1_645 1_645 ? O14 Na2 Na3 125.95(11) 1_655 1_645 ? O4 Na2 Na3 146.51(10) . 1_645 ? O9 Na2 Na3 46.54(9) 1_545 1_645 ? O10 Na2 Na3 37.60(7) 1_645 1_645 ? O19 Na2 Na3 90.09(9) . 1_645 ? N1 Na2 Na3 96.43(10) 1_645 1_645 ? Na1 Na2 Na3 58.14(4) 1_645 1_645 ? O10 Na3 O15 108.38(12) . 2_666 ? O10 Na3 O18 118.23(14) . . ? O15 Na3 O18 104.47(12) 2_666 . ? O10 Na3 O17 98.58(12) . . ? O15 Na3 O17 79.17(13) 2_666 . ? O18 Na3 O17 138.47(13) . . ? O10 Na3 O9 77.00(10) . 1_455 ? O15 Na3 O9 171.40(12) 2_666 1_455 ? O18 Na3 O9 66.92(11) . 1_455 ? O17 Na3 O9 107.03(12) . 1_455 ? O10 Na3 O8 50.90(9) . . ? O15 Na3 O8 94.76(11) 2_666 . ? O18 Na3 O8 75.91(11) . . ? O17 Na3 O8 145.60(11) . . ? O9 Na3 O8 83.43(10) 1_455 . ? O10 Na3 C8 25.57(10) . . ? O15 Na3 C8 100.90(12) 2_666 . ? O18 Na3 C8 98.28(13) . . ? O17 Na3 C8 122.01(12) . . ? O9 Na3 C8 81.06(10) 1_455 . ? O8 Na3 C8 25.46(9) . . ? O10 Na3 Na1 72.42(9) . . ? O15 Na3 Na1 131.04(11) 2_666 . ? O18 Na3 Na1 46.79(10) . . ? O17 Na3 Na1 149.74(10) . . ? O9 Na3 Na1 43.24(7) 1_455 . ? O8 Na3 Na1 46.28(7) . . ? C8 Na3 Na1 58.21(8) . . ? O10 Na3 Na2 40.87(7) . 1_465 ? O15 Na3 Na2 147.75(9) 2_666 1_465 ? O18 Na3 Na2 101.22(10) . 1_465 ? O17 Na3 Na2 94.25(9) . 1_465 ? O9 Na3 Na2 39.39(7) 1_455 1_465 ? O8 Na3 Na2 72.91(7) . 1_465 ? C8 Na3 Na2 55.92(8) . 1_465 ? Na1 Na3 Na2 59.70(5) . 1_465 ? _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.904 _refine_diff_density_max 1.103 _refine_diff_density_min -1.093 _refine_diff_density_rms 0.111 _diffrn_ambient_pressure 105