# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global #TrackingRef 'final cif.cif' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Annie K. Powell' _publ_contact_author_email Annie.Powell@kit.edu _publ_section_title ; Fine-tuning of lanthanide -- monocarboxylate coordination networks through ligand decoration ; loop_ _publ_author_name 'Zeeshan Majeed' 'George E. Kostakis' 'Yanhua Lan' 'Annie K. Powell' # end Validation Reply Form data_mz-757 _database_code_depnum_ccdc_archive 'CCDC 824458' #TrackingRef 'final cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H16 Dy Na O9' _chemical_formula_weight 453.71 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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0858(11) _cell_length_b 9.1643(12) _cell_length_c 9.7940(13) _cell_angle_alpha 112.078(10) _cell_angle_beta 101.018(10) _cell_angle_gamma 93.931(10) _cell_volume 732.88(16) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 13653 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.20 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.056 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 438 _exptl_absorpt_coefficient_mu 5.164 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4249 _exptl_absorpt_correction_T_max 0.6262 _exptl_absorpt_process_details 'XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate ( 34 cm diameter )' _diffrn_detector_type STOE _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5298 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0320 _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 -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 26.75 _reflns_number_total 3111 _reflns_number_gt 2980 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0491P)^2^+0.8082P] 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 3111 _refine_ls_number_parameters 188 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0700 _refine_ls_wR_factor_gt 0.0691 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.038 _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 Dy1 Dy 0.129071(16) 0.840119(16) 0.446298(17) 0.02321(8) Uani 1 1 d . . . Na1 Na 0.5000 1.0000 0.5000 0.0305(4) Uani 1 2 d S . . Na2 Na 0.0000 0.5000 0.5000 0.0300(4) Uani 1 2 d S . . O1 O 0.2077(3) 0.7048(3) 0.6122(3) 0.0321(6) Uani 1 1 d . . . O2 O 0.3664(3) 0.9147(3) 0.6493(3) 0.0297(5) Uani 1 1 d . . . C1 C 0.3305(5) 0.8025(5) 0.6855(5) 0.0293(8) Uani 1 1 d . . . C2 C 0.4285(5) 0.7815(6) 0.8173(5) 0.0389(10) Uani 1 1 d . . . H2A H 0.5348 0.7920 0.8111 0.058 Uiso 1 1 calc R . . H2B H 0.3970 0.6757 0.8142 0.058 Uiso 1 1 calc R . . H2C H 0.4175 0.8633 0.9124 0.058 Uiso 1 1 calc R . . O3 O 0.0466(4) 0.8128(4) 0.1848(3) 0.0384(7) Uani 1 1 d . . . O4 O -0.0755(3) 0.9589(3) 0.3436(3) 0.0282(5) Uani 1 1 d . . . C3 C -0.0566(5) 0.8950(5) 0.2081(5) 0.0309(8) Uani 1 1 d . . . C4 C -0.1604(6) 0.9166(7) 0.0821(6) 0.0495(12) Uani 1 1 d . . . H4A H -0.1144 1.0062 0.0648 0.074 Uiso 1 1 calc R . . H4B H -0.2574 0.9388 0.1089 0.074 Uiso 1 1 calc R . . H4C H -0.1776 0.8193 -0.0104 0.074 Uiso 1 1 calc R . . O5 O 0.2528(3) 1.0822(3) 0.4581(3) 0.0278(5) Uani 1 1 d . . . O6 O 0.0986(3) 1.2656(3) 0.5091(3) 0.0303(6) Uani 1 1 d . . . C5 C 0.2198(4) 1.2187(4) 0.4766(4) 0.0282(7) Uani 1 1 d . . . C6 C 0.3302(5) 1.3327(5) 0.4538(6) 0.0387(9) Uani 1 1 d . . . H6A H 0.4188 1.2825 0.4292 0.058 Uiso 1 1 calc R . . H6B H 0.3625 1.4297 0.5469 0.058 Uiso 1 1 calc R . . H6C H 0.2810 1.3602 0.3704 0.058 Uiso 1 1 calc R . . O7 O 0.3354(3) 0.7617(3) 0.3412(3) 0.0303(6) Uani 1 1 d . . . O8 O 0.2924(4) 0.5089(4) 0.1756(4) 0.0422(7) Uani 1 1 d . . . C7 C 0.3659(5) 0.6471(5) 0.2329(4) 0.0306(8) Uani 1 1 d . . . C8 C 0.5014(6) 0.6809(6) 0.1741(6) 0.0462(11) Uani 1 1 d . . . H8A H 0.4675 0.6635 0.0673 0.069 Uiso 1 1 calc R . . H8B H 0.5742 0.6094 0.1839 0.069 Uiso 1 1 calc R . . H8C H 0.5499 0.7918 0.2332 0.069 Uiso 1 1 calc R . . O9 O 0.0557(3) 0.5497(3) 0.2889(3) 0.0316(6) Uani 1 1 d D . . H91 H 0.140(5) 0.522(6) 0.260(6) 0.038 Uiso 1 1 d D . . C9 C -0.0794(5) 0.4785(6) 0.1666(5) 0.0430(10) Uani 1 1 d . . . H9A H -0.0833 0.3626 0.1217 0.064 Uiso 1 1 calc R . . H9B H -0.0766 0.5211 0.0890 0.064 Uiso 1 1 calc R . . H9C H -0.1697 0.5037 0.2066 0.064 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 Dy1 0.02019(11) 0.01883(11) 0.03144(11) 0.01033(7) 0.00679(7) 0.00421(7) Na1 0.0243(10) 0.0250(10) 0.0429(11) 0.0129(9) 0.0104(9) 0.0043(8) Na2 0.0284(11) 0.0222(9) 0.0416(11) 0.0148(9) 0.0087(9) 0.0051(8) O1 0.0300(14) 0.0248(12) 0.0417(15) 0.0162(11) 0.0035(11) 0.0017(10) O2 0.0256(13) 0.0246(13) 0.0393(14) 0.0129(11) 0.0085(11) 0.0032(10) C1 0.0267(19) 0.0241(17) 0.0360(19) 0.0104(15) 0.0075(15) 0.0062(14) C2 0.035(2) 0.040(2) 0.040(2) 0.0186(19) 0.0012(18) 0.0034(18) O3 0.0418(17) 0.0395(16) 0.0360(14) 0.0134(13) 0.0121(13) 0.0202(13) O4 0.0254(13) 0.0257(12) 0.0325(13) 0.0096(10) 0.0081(10) 0.0065(10) C3 0.032(2) 0.0285(18) 0.0322(18) 0.0126(15) 0.0056(15) 0.0066(15) C4 0.047(3) 0.069(3) 0.039(2) 0.025(2) 0.011(2) 0.029(3) O5 0.0217(12) 0.0241(12) 0.0414(14) 0.0151(11) 0.0103(10) 0.0066(9) O6 0.0258(13) 0.0232(12) 0.0471(15) 0.0156(11) 0.0156(11) 0.0082(10) C5 0.0254(18) 0.0243(16) 0.0334(18) 0.0104(14) 0.0061(14) 0.0039(14) C6 0.031(2) 0.0296(19) 0.068(3) 0.028(2) 0.0208(19) 0.0080(16) O7 0.0237(13) 0.0253(13) 0.0392(14) 0.0083(11) 0.0103(11) 0.0051(10) O8 0.0401(17) 0.0268(14) 0.0518(18) 0.0039(13) 0.0184(14) 0.0015(12) C7 0.0307(19) 0.0273(17) 0.0361(18) 0.0138(15) 0.0089(15) 0.0082(15) C8 0.046(3) 0.042(2) 0.046(2) 0.0070(19) 0.023(2) 0.001(2) O9 0.0289(14) 0.0268(13) 0.0368(14) 0.0094(11) 0.0099(11) 0.0020(11) C9 0.037(2) 0.042(2) 0.040(2) 0.0093(18) 0.0055(18) -0.0082(18) _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 Dy1 O7 2.336(3) . ? Dy1 O4 2.349(3) 2_576 ? Dy1 O5 2.369(3) . ? Dy1 O6 2.408(3) 2_576 ? Dy1 O1 2.425(3) . ? Dy1 O3 2.438(3) . ? Dy1 O4 2.457(3) . ? Dy1 O9 2.487(3) . ? Dy1 O2 2.491(3) . ? Na1 O7 2.353(3) . ? Na1 O7 2.353(3) 2_676 ? Na1 O2 2.373(3) . ? Na1 O2 2.373(3) 2_676 ? Na1 O5 2.427(3) . ? Na1 O5 2.427(3) 2_676 ? Na2 O1 2.337(3) 2_566 ? Na2 O1 2.337(3) . ? Na2 O6 2.409(3) 1_545 ? Na2 O6 2.409(3) 2_576 ? Na2 O9 2.411(3) 2_566 ? Na2 O9 2.411(3) . ? O1 C1 1.279(5) . ? O2 C1 1.250(5) . ? C1 C2 1.505(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 C3 1.244(5) . ? O4 C3 1.284(5) . ? O4 Dy1 2.349(3) 2_576 ? C3 C4 1.489(6) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? O5 C5 1.261(4) . ? O6 C5 1.263(5) . ? O6 Dy1 2.408(3) 2_576 ? O6 Na2 2.409(3) 1_565 ? C5 C6 1.504(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O7 C7 1.272(5) . ? O8 C7 1.253(5) . ? C7 C8 1.515(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O9 C9 1.452(5) . ? O9 H91 0.88(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? 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 O7 Dy1 O4 139.59(9) . 2_576 ? O7 Dy1 O5 77.13(9) . . ? O4 Dy1 O5 74.56(9) 2_576 . ? O7 Dy1 O6 141.94(9) . 2_576 ? O4 Dy1 O6 73.03(9) 2_576 2_576 ? O5 Dy1 O6 140.55(9) . 2_576 ? O7 Dy1 O1 87.25(10) . . ? O4 Dy1 O1 87.13(9) 2_576 . ? O5 Dy1 O1 126.75(9) . . ? O6 Dy1 O1 73.25(9) 2_576 . ? O7 Dy1 O3 75.89(10) . . ? O4 Dy1 O3 124.67(9) 2_576 . ? O5 Dy1 O3 78.48(10) . . ? O6 Dy1 O3 102.34(11) 2_576 . ? O1 Dy1 O3 145.93(10) . . ? O7 Dy1 O4 125.33(9) . . ? O4 Dy1 O4 73.89(10) 2_576 . ? O5 Dy1 O4 75.51(9) . . ? O6 Dy1 O4 74.37(9) 2_576 . ? O1 Dy1 O4 146.06(10) . . ? O3 Dy1 O4 52.82(9) . . ? O7 Dy1 O9 74.68(9) . . ? O4 Dy1 O9 140.53(10) 2_576 . ? O5 Dy1 O9 144.20(9) . . ? O6 Dy1 O9 68.61(9) 2_576 . ? O1 Dy1 O9 73.45(9) . . ? O3 Dy1 O9 73.61(10) . . ? O4 Dy1 O9 103.72(9) . . ? O7 Dy1 O2 69.51(9) . . ? O4 Dy1 O2 75.33(9) 2_576 . ? O5 Dy1 O2 74.00(9) . . ? O6 Dy1 O2 117.78(9) 2_576 . ? O1 Dy1 O2 52.93(9) . . ? O3 Dy1 O2 139.53(10) . . ? O4 Dy1 O2 141.22(9) . . ? O9 Dy1 O2 115.04(9) . . ? O7 Na1 O7 180.0 . 2_676 ? O7 Na1 O2 71.32(10) . . ? O7 Na1 O2 108.68(10) 2_676 . ? O7 Na1 O2 108.68(10) . 2_676 ? O7 Na1 O2 71.32(10) 2_676 2_676 ? O2 Na1 O2 180.000(2) . 2_676 ? O7 Na1 O5 75.70(9) . . ? O7 Na1 O5 104.30(9) 2_676 . ? O2 Na1 O5 75.12(9) . . ? O2 Na1 O5 104.88(9) 2_676 . ? O7 Na1 O5 104.30(9) . 2_676 ? O7 Na1 O5 75.70(9) 2_676 2_676 ? O2 Na1 O5 104.88(9) . 2_676 ? O2 Na1 O5 75.12(9) 2_676 2_676 ? O5 Na1 O5 179.999(1) . 2_676 ? O1 Na2 O1 180.0 2_566 . ? O1 Na2 O6 74.80(9) 2_566 1_545 ? O1 Na2 O6 105.20(9) . 1_545 ? O1 Na2 O6 105.20(9) 2_566 2_576 ? O1 Na2 O6 74.80(9) . 2_576 ? O6 Na2 O6 179.998(1) 1_545 2_576 ? O1 Na2 O9 76.41(10) 2_566 2_566 ? O1 Na2 O9 103.59(10) . 2_566 ? O6 Na2 O9 69.85(10) 1_545 2_566 ? O6 Na2 O9 110.16(10) 2_576 2_566 ? O1 Na2 O9 103.59(10) 2_566 . ? O1 Na2 O9 76.41(10) . . ? O6 Na2 O9 110.16(10) 1_545 . ? O6 Na2 O9 69.84(10) 2_576 . ? O9 Na2 O9 180.0 2_566 . ? C1 O1 Na2 170.2(3) . . ? C1 O1 Dy1 94.6(2) . . ? Na2 O1 Dy1 95.01(10) . . ? C1 O2 Na1 146.0(3) . . ? C1 O2 Dy1 92.2(2) . . ? Na1 O2 Dy1 90.05(9) . . ? O2 C1 O1 120.2(4) . . ? O2 C1 C2 121.0(4) . . ? O1 C1 C2 118.8(4) . . ? O2 C1 Dy1 61.6(2) . . ? O1 C1 Dy1 58.64(19) . . ? C2 C1 Dy1 176.1(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C3 O3 Dy1 95.1(2) . . ? C3 O4 Dy1 155.9(2) . 2_576 ? C3 O4 Dy1 93.1(2) . . ? Dy1 O4 Dy1 106.11(10) 2_576 . ? O3 C3 O4 118.9(4) . . ? O3 C3 C4 121.4(4) . . ? O4 C3 C4 119.7(4) . . ? O3 C3 Dy1 58.9(2) . . ? O4 C3 Dy1 59.95(19) . . ? C4 C3 Dy1 176.9(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C5 O5 Dy1 136.6(2) . . ? C5 O5 Na1 129.4(2) . . ? Dy1 O5 Na1 91.71(9) . . ? C5 O6 Dy1 137.8(2) . 2_576 ? C5 O6 Na2 127.8(2) . 1_565 ? Dy1 O6 Na2 93.63(9) 2_576 1_565 ? O5 C5 O6 124.7(3) . . ? O5 C5 C6 117.9(3) . . ? O6 C5 C6 117.4(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C7 O7 Dy1 139.4(3) . . ? C7 O7 Na1 126.0(2) . . ? Dy1 O7 Na1 94.46(9) . . ? O8 C7 O7 123.7(4) . . ? O8 C7 C8 119.0(4) . . ? O7 C7 C8 117.3(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C9 O9 Na2 105.7(2) . . ? C9 O9 Dy1 124.7(3) . . ? Na2 O9 Dy1 91.60(9) . . ? C9 O9 H91 113(3) . . ? Na2 O9 H91 118(3) . . ? Dy1 O9 H91 103(3) . . ? O9 C9 H9A 109.5 . . ? O9 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O9 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H91 O8 0.88(3) 1.74(4) 2.589(4) 162(5) . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.834 _refine_diff_density_min -1.715 _refine_diff_density_rms 0.150 #============================================================================== data_mz-1017 _database_code_depnum_ccdc_archive 'CCDC 824459' #TrackingRef 'final cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H28 Dy Na O8' _chemical_formula_weight 533.87 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' 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4122 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-y, x+1/2, z+1/4' 'y+1/2, -x, z+3/4' '-x+1/2, y, -z+3/4' 'x, -y+1/2, -z+1/4' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1, z+1' '-y+1/2, x+1, z+3/4' 'y+1, -x+1/2, z+5/4' '-x+1, y+1/2, -z+5/4' 'x+1/2, -y+1, -z+3/4' 'y+1, x+1, -z+1' '-y+1/2, -x+1/2, -z+1/2' _cell_length_a 16.3848(7) _cell_length_b 16.3848(7) _cell_length_c 16.3848(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4398.7(3) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 21249 _cell_measurement_theta_min 1.24 _cell_measurement_theta_max 27.26 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 3.451 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4449 _exptl_absorpt_correction_T_max 0.5452 _exptl_absorpt_process_details 'XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate ( 34 cm diameter )' _diffrn_detector_type STOE _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12857 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.79 _reflns_number_total 2326 _reflns_number_gt 2245 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0430P)^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 H D (1983), Acta Cryst. A39, 876-881, 1362 Friedel pairs'" _refine_ls_abs_structure_Flack 0.005(16) _refine_ls_number_reflns 2326 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0581 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Dy1 Dy 0.586864(7) 0.413136(7) 0.0000 0.03128(8) Uani 1 2 d S . . Na1 Na 0.57272(12) 0.2500 0.1250 0.0352(5) Uani 1 2 d S . . O1 O 0.66867(17) 0.35551(17) 0.10870(17) 0.0437(7) Uani 1 1 d . . . O2 O 0.73440(16) 0.42430(17) 0.01563(15) 0.0414(6) Uani 1 1 d . . . C1 C 0.7348(2) 0.3846(2) 0.0813(2) 0.0374(7) Uani 1 1 d . . . C2 C 0.8129(2) 0.3743(3) 0.1284(3) 0.0499(10) Uani 1 1 d . . . H2A H 0.8116 0.4122 0.1753 0.060 Uiso 1 1 calc R . . H2B H 0.8140 0.3181 0.1507 0.060 Uiso 1 1 calc R . . C3 C 0.8896(3) 0.3879(5) 0.0839(3) 0.0776(16) Uani 1 1 d . . . H3A H 0.8891 0.4439 0.0613 0.093 Uiso 1 1 calc R . . H3B H 0.8920 0.3494 0.0374 0.093 Uiso 1 1 calc R . . C4 C 0.9668(3) 0.3772(5) 0.1355(4) 0.0810(17) Uani 1 1 d . . . H4A H 1.0149 0.3882 0.1017 0.122 Uiso 1 1 calc R . . H4B H 0.9693 0.3212 0.1562 0.122 Uiso 1 1 calc R . . H4C H 0.9655 0.4154 0.1814 0.122 Uiso 1 1 calc R . . O3 O 0.5890(2) 0.52540(16) 0.08255(17) 0.0476(6) Uani 1 1 d . . . O4 O 0.50746(17) 0.63281(17) 0.09725(16) 0.0402(6) Uani 1 1 d . . . C5 C 0.5693(2) 0.5916(2) 0.1157(3) 0.0356(8) Uani 1 1 d . . . C6 C 0.6211(3) 0.6251(4) 0.1856(3) 0.0661(12) Uani 1 1 d . . . H6A H 0.6280 0.6845 0.1768 0.079 Uiso 1 1 calc R . . H6B H 0.5897 0.6183 0.2368 0.079 Uiso 1 1 calc R . . C7 C 0.7040(3) 0.5891(4) 0.1987(4) 0.0807(16) Uani 1 1 d . . . H7A H 0.7250 0.6065 0.2526 0.097 Uiso 1 1 calc R . . H7B H 0.6997 0.5288 0.1989 0.097 Uiso 1 1 calc R . . C8 C 0.7612(6) 0.6143(5) 0.1352(6) 0.120(3) Uani 1 1 d . . . H8A H 0.8143 0.5886 0.1449 0.180 Uiso 1 1 calc R . . H8B H 0.7674 0.6738 0.1364 0.180 Uiso 1 1 calc R . . H8C H 0.7404 0.5975 0.0818 0.180 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 Dy1 0.03257(9) 0.03257(9) 0.02869(11) 0.00474(6) 0.00474(6) 0.00315(8) Na1 0.0395(11) 0.0339(9) 0.0323(9) 0.0079(8) 0.000 0.000 O1 0.0409(12) 0.0488(15) 0.0415(15) 0.0142(11) -0.0045(11) -0.0046(12) O2 0.0380(11) 0.0551(14) 0.0311(13) 0.0050(11) 0.0022(10) 0.0020(12) C1 0.0389(18) 0.0366(16) 0.0366(18) -0.0022(14) -0.0045(15) 0.0031(14) C2 0.045(2) 0.054(2) 0.051(2) 0.008(2) -0.010(2) -0.0003(18) C3 0.042(2) 0.144(6) 0.047(2) 0.010(3) -0.0035(19) 0.002(3) C4 0.048(2) 0.124(5) 0.071(3) 0.000(4) -0.013(3) 0.002(3) O3 0.0555(16) 0.0405(13) 0.0467(14) -0.0021(11) 0.0132(14) 0.0047(13) O4 0.0384(13) 0.0426(13) 0.0397(14) -0.0118(11) -0.0121(11) 0.0071(11) C5 0.0351(16) 0.0354(15) 0.0363(18) 0.0002(13) -0.0014(13) 0.0061(16) C6 0.057(3) 0.074(3) 0.068(3) -0.006(3) -0.030(3) 0.001(2) C7 0.059(3) 0.083(4) 0.100(4) -0.001(4) -0.026(3) -0.001(3) C8 0.101(5) 0.120(6) 0.139(7) 0.002(6) 0.038(6) -0.005(5) _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 Dy1 O3 2.283(3) . ? Dy1 O3 2.283(3) 8_665 ? Dy1 O4 2.344(2) 15_444 ? Dy1 O4 2.344(2) 10_554 ? Dy1 O1 2.421(2) . ? Dy1 O1 2.421(2) 8_665 ? Dy1 O2 2.438(3) . ? Dy1 O2 2.438(3) 8_665 ? Dy1 C1 2.805(4) 8_665 ? Dy1 C1 2.805(4) . ? Dy1 Na1 3.37538(19) 4_564 ? Na1 O2 2.319(2) 8_665 ? Na1 O2 2.319(2) 3_645 ? Na1 O1 2.352(3) . ? Na1 O1 2.352(3) 6 ? Na1 O4 2.370(3) 13_544 ? Na1 O4 2.370(3) 10_554 ? Na1 Dy1 3.37541(19) 3_645 ? O1 C1 1.266(5) . ? O2 C1 1.257(4) . ? O2 Na1 2.319(2) 4_564 ? C1 C2 1.504(5) . ? C2 C3 1.469(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.530(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? O3 C5 1.255(4) . ? O4 C5 1.254(4) . ? O4 Dy1 2.344(2) 10_554 ? O4 Na1 2.370(3) 10_554 ? C5 C6 1.528(5) . ? C6 C7 1.495(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.460(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? 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 Dy1 O3 112.02(17) . 8_665 ? O3 Dy1 O4 82.34(10) . 15_444 ? O3 Dy1 O4 82.29(10) 8_665 15_444 ? O3 Dy1 O4 82.30(10) . 10_554 ? O3 Dy1 O4 82.34(10) 8_665 10_554 ? O4 Dy1 O4 152.33(13) 15_444 10_554 ? O3 Dy1 O1 82.54(10) . . ? O3 Dy1 O1 151.16(10) 8_665 . ? O4 Dy1 O1 125.41(10) 15_444 . ? O4 Dy1 O1 74.91(10) 10_554 . ? O3 Dy1 O1 151.16(10) . 8_665 ? O3 Dy1 O1 82.53(10) 8_665 8_665 ? O4 Dy1 O1 74.91(10) 15_444 8_665 ? O4 Dy1 O1 125.41(10) 10_554 8_665 ? O1 Dy1 O1 96.28(14) . 8_665 ? O3 Dy1 O2 82.09(11) . . ? O3 Dy1 O2 149.56(9) 8_665 . ? O4 Dy1 O2 72.75(9) 15_444 . ? O4 Dy1 O2 127.34(9) 10_554 . ? O1 Dy1 O2 53.34(9) . . ? O1 Dy1 O2 74.46(9) 8_665 . ? O3 Dy1 O2 149.56(9) . 8_665 ? O3 Dy1 O2 82.09(11) 8_665 8_665 ? O4 Dy1 O2 127.34(9) 15_444 8_665 ? O4 Dy1 O2 72.75(9) 10_554 8_665 ? O1 Dy1 O2 74.46(9) . 8_665 ? O1 Dy1 O2 53.34(9) 8_665 8_665 ? O2 Dy1 O2 99.20(13) . 8_665 ? O3 Dy1 C1 167.14(11) . 8_665 ? O3 Dy1 C1 80.79(11) 8_665 8_665 ? O4 Dy1 C1 101.15(10) 15_444 8_665 ? O4 Dy1 C1 98.93(10) 10_554 8_665 ? O1 Dy1 C1 85.42(10) . 8_665 ? O1 Dy1 C1 26.76(10) 8_665 8_665 ? O2 Dy1 C1 87.10(10) . 8_665 ? O2 Dy1 C1 26.59(10) 8_665 8_665 ? O3 Dy1 C1 80.79(11) . . ? O3 Dy1 C1 167.14(11) 8_665 . ? O4 Dy1 C1 98.93(10) 15_444 . ? O4 Dy1 C1 101.14(10) 10_554 . ? O1 Dy1 C1 26.76(10) . . ? O1 Dy1 C1 85.42(10) 8_665 . ? O2 Dy1 C1 26.59(10) . . ? O2 Dy1 C1 87.10(10) 8_665 . ? C1 Dy1 C1 86.42(15) 8_665 . ? O3 Dy1 Na1 106.99(8) . 4_564 ? O3 Dy1 Na1 106.23(7) 8_665 4_564 ? O4 Dy1 Na1 44.59(7) 15_444 4_564 ? O4 Dy1 Na1 163.07(7) 10_554 4_564 ? O1 Dy1 Na1 91.99(7) . 4_564 ? O1 Dy1 Na1 44.17(7) 8_665 4_564 ? O2 Dy1 Na1 43.39(6) . 4_564 ? O2 Dy1 Na1 93.66(7) 8_665 4_564 ? C1 Dy1 Na1 68.85(8) 8_665 4_564 ? C1 Dy1 Na1 67.38(8) . 4_564 ? O2 Na1 O2 177.58(17) 8_665 3_645 ? O2 Na1 O1 78.00(10) 8_665 . ? O2 Na1 O1 100.36(11) 3_645 . ? O2 Na1 O1 100.35(11) 8_665 6 ? O2 Na1 O1 78.00(10) 3_645 6 ? O1 Na1 O1 96.10(15) . 6 ? O2 Na1 O4 106.96(10) 8_665 13_544 ? O2 Na1 O4 74.44(9) 3_645 13_544 ? O1 Na1 O4 170.96(11) . 13_544 ? O1 Na1 O4 75.71(9) 6 13_544 ? O2 Na1 O4 74.44(9) 8_665 10_554 ? O2 Na1 O4 106.96(10) 3_645 10_554 ? O1 Na1 O4 75.71(9) . 10_554 ? O1 Na1 O4 170.96(11) 6 10_554 ? O4 Na1 O4 112.70(15) 13_544 10_554 ? O2 Na1 Dy1 133.53(7) 8_665 3_645 ? O2 Na1 Dy1 46.24(7) 3_645 3_645 ? O1 Na1 Dy1 127.23(9) . 3_645 ? O1 Na1 Dy1 45.82(6) 6 3_645 ? O4 Na1 Dy1 43.96(6) 13_544 3_645 ? O4 Na1 Dy1 142.74(8) 10_554 3_645 ? C1 O1 Na1 152.8(3) . . ? C1 O1 Dy1 93.8(2) . . ? Na1 O1 Dy1 90.01(10) . . ? C1 O2 Na1 149.4(3) . 4_564 ? C1 O2 Dy1 93.2(2) . . ? Na1 O2 Dy1 90.37(9) 4_564 . ? O2 C1 O1 119.6(3) . . ? O2 C1 C2 120.1(4) . . ? O1 C1 C2 120.3(3) . . ? O2 C1 Dy1 60.20(19) . . ? O1 C1 Dy1 59.45(19) . . ? C2 C1 Dy1 176.1(3) . . ? C3 C2 C1 117.2(4) . . ? C3 C2 H2A 108.0 . . ? C1 C2 H2A 108.0 . . ? C3 C2 H2B 108.0 . . ? C1 C2 H2B 108.0 . . ? H2A C2 H2B 107.2 . . ? C2 C3 C4 114.6(4) . . ? C2 C3 H3A 108.6 . . ? C4 C3 H3A 108.6 . . ? C2 C3 H3B 108.6 . . ? C4 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C5 O3 Dy1 161.6(3) . . ? C5 O4 Dy1 121.6(2) . 10_554 ? C5 O4 Na1 146.8(2) . 10_554 ? Dy1 O4 Na1 91.44(10) 10_554 10_554 ? O4 C5 O3 124.6(4) . . ? O4 C5 C6 115.9(4) . . ? O3 C5 C6 119.5(4) . . ? C7 C6 C5 118.0(5) . . ? C7 C6 H6A 107.8 . . ? C5 C6 H6A 107.8 . . ? C7 C6 H6B 107.8 . . ? C5 C6 H6B 107.8 . . ? H6A C6 H6B 107.1 . . ? C8 C7 C6 111.7(6) . . ? C8 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? C8 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.625 _refine_diff_density_min -1.446 _refine_diff_density_rms 0.089