Supplementary Material (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Annie Powell' _publ_contact_author_email POWELL@CHEMIE.UNI-KARLSRUHE.DE _publ_section_title ; [LnNa(PhCO2)4] (Ln= Ho, Dy): The First Examples of Chiral srs 3D-Networks constructed using the Monotopic Benzoate Ligand ; loop_ _publ_author_name 'Annie Powell' 'Christopher E Anson' 'George E Kostakis' 'Yanhua Lan.' 'Zeeshan Majeed' 'Kartik C. Mondal' # Attachment 'NaLn-helices2.cif' data_z55 _database_code_depnum_ccdc_archive 'CCDC 751549' #TrackingRef 'NaLn-helices2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H20 Ho Na O8' _chemical_formula_sum 'C28 H20 Ho Na O8' _chemical_formula_weight 672.36 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' Ho Ho -0.2175 4.6783 '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 tetragonal _symmetry_space_group_name_H-M 'I 41' _symmetry_space_group_name_Hall 'I 4bw' 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+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' _cell_length_a 16.1249(3) _cell_length_b 16.1249(3) _cell_length_c 19.5060(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5071.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7001 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 28.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2640 _exptl_absorpt_coefficient_mu 3.188 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.659 _exptl_absorpt_correction_T_max 0.853 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker AXS Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11574 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4906 _reflns_number_gt 4545 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_data_reduction 'SAINT+ 6.45 (Bruker AXS Inc., 2003)' _computing_structure_solution 'SHELXTL 6.12 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.12 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'SHELXTL 6.12 (BrukerAXS Inc., 2003)' _computing_publication_material 'SHELXTL 6.12 (BrukerAXS Inc., 2003)' _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. The phenyl groups of two of the four benzoate ligands were disordered, and both were refined as a pair of rigid hexagons with 50:50 occupancy. For each ligand, the dihedral between the planes of the two hexagons was relatively small, and corresponding pairs of carbon atoms could be refined with common anisotropic thermal parameters. All H-atoms were placed in calculated positions. ; _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^)+(0.0292P)^2^+1.2702P] 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, 2231 Friedel pairs' _refine_ls_abs_structure_Flack -0.016(10) _refine_ls_number_reflns 4906 _refine_ls_number_parameters 331 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0532 _refine_ls_wR_factor_gt 0.0520 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Ho1 Ho 0.588536(11) 0.411475(11) 0.686670(18) 0.01857(5) Uani 1 1 d . . . Na1 Na 0.74999(12) 0.40261(13) 0.56179(10) 0.0283(4) Uani 1 1 d . A . O1 O 0.49977(19) 0.37192(19) 0.77713(16) 0.0243(7) Uani 1 1 d . . . O2 O 0.40984(19) 0.47207(19) 0.75065(16) 0.0253(7) Uani 1 1 d . . . C1 C 0.4331(3) 0.4123(3) 0.7876(3) 0.0236(11) Uani 1 1 d . . . C2 C 0.3796(3) 0.3879(3) 0.8467(3) 0.0288(11) Uani 1 1 d . . . C3 C 0.4027(3) 0.3241(3) 0.8903(3) 0.0313(11) Uani 1 1 d . . . H3A H 0.4521 0.2937 0.8817 0.038 Uiso 1 1 calc R . . C4 C 0.3532(4) 0.3047(3) 0.9470(3) 0.0461(15) Uani 1 1 d . . . H4A H 0.3695 0.2616 0.9774 0.055 Uiso 1 1 calc R . . C5 C 0.2815(4) 0.3475(4) 0.9586(3) 0.0586(19) Uani 1 1 d . . . H5A H 0.2488 0.3351 0.9978 0.070 Uiso 1 1 calc R . . C6 C 0.2564(4) 0.4086(4) 0.9140(4) 0.063(2) Uani 1 1 d . . . H6A H 0.2052 0.4364 0.9216 0.075 Uiso 1 1 calc R . . C7 C 0.3048(4) 0.4297(4) 0.8583(3) 0.0446(14) Uani 1 1 d . . . H7A H 0.2875 0.4725 0.8280 0.054 Uiso 1 1 calc R . . O3 O 0.62786(19) 0.50004(19) 0.59646(16) 0.0245(7) Uani 1 1 d . . . O4 O 0.52809(19) 0.59022(19) 0.62274(16) 0.0248(7) Uani 1 1 d . . . C8 C 0.5876(3) 0.5671(3) 0.5858(3) 0.0233(11) Uani 1 1 d . . . C9 C 0.6126(3) 0.6203(3) 0.5266(3) 0.0281(11) Uani 1 1 d . . . C10 C 0.6764(3) 0.5973(3) 0.4833(3) 0.0316(11) Uani 1 1 d . . . H10A H 0.7073 0.5484 0.4924 0.038 Uiso 1 1 calc R . . C11 C 0.6957(3) 0.6463(4) 0.4260(3) 0.0445(14) Uani 1 1 d . . . H11A H 0.7382 0.6297 0.3953 0.053 Uiso 1 1 calc R . . C12 C 0.6524(4) 0.7183(4) 0.4150(3) 0.060(2) Uani 1 1 d . . . H12A H 0.6649 0.7513 0.3760 0.073 Uiso 1 1 calc R . . C13 C 0.5910(4) 0.7437(4) 0.4597(4) 0.062(2) Uani 1 1 d . . . H13A H 0.5630 0.7948 0.4524 0.074 Uiso 1 1 calc R . . C14 C 0.5704(4) 0.6945(4) 0.5150(3) 0.0455(14) Uani 1 1 d . . . H14A H 0.5274 0.7113 0.5453 0.055 Uiso 1 1 calc R . . O5 O 0.73592(17) 0.41417(17) 0.68288(18) 0.0275(6) Uani 1 1 d . A . O6 O 0.6841(2) 0.3638(2) 0.77878(17) 0.0294(8) Uani 1 1 d . A . C15 C 0.7457(3) 0.3857(3) 0.7431(2) 0.0265(10) Uani 1 1 d . . . C16A C 0.8300(9) 0.3707(12) 0.7663(7) 0.031(3) Uani 0.50 1 d PG A 1 C17A C 0.8971(13) 0.4014(15) 0.7294(7) 0.048(2) Uani 0.50 1 d PG A 1 H17A H 0.8881 0.4296 0.6873 0.058 Uiso 0.50 1 calc PR A 1 C18A C 0.9772(11) 0.3908(12) 0.7541(8) 0.065(3) Uani 0.50 1 d PG A 1 H18A H 1.0230 0.4118 0.7289 0.078 Uiso 0.50 1 calc PR A 1 C19A C 0.9903(6) 0.3495(7) 0.8157(7) 0.057(4) Uani 0.50 1 d PG A 1 H19A H 1.0451 0.3422 0.8326 0.069 Uiso 0.50 1 calc PR A 1 C20A C 0.9233(6) 0.3188(7) 0.8526(5) 0.054(3) Uani 0.50 1 d PG A 1 H20A H 0.9322 0.2905 0.8947 0.064 Uiso 0.50 1 calc PR A 1 C21A C 0.8431(5) 0.3294(7) 0.8279(6) 0.048(3) Uani 0.50 1 d PG A 1 H21A H 0.7973 0.3084 0.8531 0.058 Uiso 0.50 1 calc PR A 1 C16B C 0.8329(9) 0.3881(12) 0.7748(7) 0.031(3) Uani 0.50 1 d PG A 2 C17B C 0.9002(13) 0.4035(15) 0.7320(5) 0.048(2) Uani 0.50 1 d PG A 2 H17B H 0.8916 0.4123 0.6844 0.058 Uiso 0.50 1 calc PR A 2 C18B C 0.9800(11) 0.4058(12) 0.7590(7) 0.065(3) Uani 0.50 1 d PG A 2 H18B H 1.0259 0.4163 0.7298 0.078 Uiso 0.50 1 calc PR A 2 C19B C 0.9925(6) 0.3928(7) 0.8287(7) 0.057(4) Uani 0.50 1 d PG A 2 H19B H 1.0470 0.3944 0.8471 0.069 Uiso 0.50 1 calc PR A 2 C20B C 0.9252(6) 0.3774(7) 0.8714(5) 0.054(3) Uani 0.50 1 d PG A 2 H20B H 0.9338 0.3685 0.9190 0.064 Uiso 0.50 1 calc PR A 2 C21B C 0.8455(5) 0.3751(7) 0.8445(6) 0.048(3) Uani 0.50 1 d PG A 2 H21B H 0.7995 0.3646 0.8737 0.058 Uiso 0.50 1 calc PR A 2 O7 O 0.6360(2) 0.31600(19) 0.59495(17) 0.0284(8) Uani 1 1 d . . . O8 O 0.58599(17) 0.26430(17) 0.69083(18) 0.0270(6) Uani 1 1 d . . . C22 C 0.6141(3) 0.2537(3) 0.6305(2) 0.0264(10) Uani 1 1 d . A . C23A C 0.6153(12) 0.1668(11) 0.5995(8) 0.0354(19) Uani 0.50 1 d PG A 1 C24A C 0.6012(15) 0.0994(16) 0.6423(5) 0.046(2) Uani 0.50 1 d PG A 1 H24A H 0.5939 0.1076 0.6901 0.055 Uiso 0.50 1 calc PR A 1 C25A C 0.5980(12) 0.0197(13) 0.6151(8) 0.068(3) Uani 0.50 1 d PG A 1 H25A H 0.5884 -0.0264 0.6443 0.082 Uiso 0.50 1 calc PR A 1 C26A C 0.6088(8) 0.0076(7) 0.5451(9) 0.064(5) Uani 0.50 1 d PG A 1 H26A H 0.6065 -0.0468 0.5265 0.077 Uiso 0.50 1 calc PR A 1 C27A C 0.6228(8) 0.0751(6) 0.5023(5) 0.061(3) Uani 0.50 1 d PG A 1 H27A H 0.6302 0.0668 0.4545 0.073 Uiso 0.50 1 calc PR A 1 C28A C 0.6261(8) 0.1547(6) 0.5295(7) 0.050(3) Uani 0.50 1 d PG A 1 H28A H 0.6357 0.2008 0.5002 0.060 Uiso 0.50 1 calc PR A 1 C23B C 0.6264(12) 0.1697(11) 0.6064(8) 0.0354(19) Uani 0.50 1 d PG A 2 C24B C 0.5940(15) 0.1029(16) 0.6426(8) 0.046(2) Uani 0.50 1 d PG A 2 H24B H 0.5641 0.1121 0.6839 0.055 Uiso 0.50 1 calc PR A 2 C25B C 0.6055(13) 0.0226(13) 0.6185(9) 0.068(3) Uani 0.50 1 d PG A 2 H25B H 0.5833 -0.0231 0.6433 0.082 Uiso 0.50 1 calc PR A 2 C26B C 0.6493(9) 0.0090(7) 0.5582(8) 0.064(5) Uani 0.50 1 d PG A 2 H26B H 0.6571 -0.0458 0.5417 0.077 Uiso 0.50 1 calc PR A 2 C27B C 0.6817(7) 0.0758(6) 0.5220(5) 0.061(3) Uani 0.50 1 d PG A 2 H27B H 0.7116 0.0666 0.4807 0.073 Uiso 0.50 1 calc PR A 2 C28B C 0.6702(7) 0.1561(6) 0.5461(7) 0.050(3) Uani 0.50 1 d PG A 2 H28B H 0.6924 0.2018 0.5213 0.060 Uiso 0.50 1 calc PR A 2 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 Ho1 0.01813(10) 0.01813(10) 0.01946(8) 0.00229(9) 0.00227(8) 0.00261(8) Na1 0.0291(9) 0.0329(10) 0.0229(9) -0.0004(7) 0.0070(7) 0.0001(8) O1 0.0255(17) 0.0224(16) 0.0250(18) 0.0006(13) 0.0055(13) 0.0008(13) O2 0.0340(18) 0.0202(16) 0.0216(17) -0.0013(13) 0.0010(14) -0.0001(14) C1 0.027(3) 0.018(2) 0.026(3) -0.0042(19) 0.002(2) -0.003(2) C2 0.035(3) 0.024(2) 0.027(3) -0.001(2) 0.009(2) -0.001(2) C3 0.038(3) 0.024(2) 0.031(3) -0.001(2) 0.006(2) -0.004(2) C4 0.065(4) 0.038(3) 0.035(4) 0.005(3) 0.011(3) -0.011(3) C5 0.074(5) 0.056(4) 0.046(4) 0.000(3) 0.040(3) -0.007(3) C6 0.065(4) 0.057(4) 0.066(6) 0.006(3) 0.045(4) 0.019(3) C7 0.046(3) 0.041(3) 0.048(4) 0.007(3) 0.015(3) 0.012(3) O3 0.0213(16) 0.0249(17) 0.0273(18) 0.0064(13) 0.0019(13) 0.0023(13) O4 0.0231(17) 0.0297(18) 0.0215(17) 0.0011(13) -0.0010(13) -0.0005(13) C8 0.015(2) 0.032(3) 0.022(3) 0.000(2) -0.0032(18) -0.003(2) C9 0.022(2) 0.036(3) 0.026(3) 0.008(2) -0.003(2) 0.003(2) C10 0.025(2) 0.035(3) 0.035(3) 0.009(2) 0.001(2) -0.003(2) C11 0.034(3) 0.066(4) 0.033(4) 0.009(3) 0.008(2) -0.009(3) C12 0.050(4) 0.081(5) 0.050(4) 0.040(3) 0.001(3) -0.002(3) C13 0.044(4) 0.070(5) 0.070(6) 0.045(4) 0.001(3) 0.014(3) C14 0.042(3) 0.045(3) 0.049(4) 0.016(3) 0.002(3) 0.010(3) O5 0.0221(15) 0.0340(17) 0.0264(16) 0.0084(18) 0.0010(15) 0.0056(13) O6 0.0224(17) 0.037(2) 0.0292(19) 0.0096(15) 0.0032(14) 0.0062(15) C15 0.025(2) 0.023(2) 0.032(3) 0.0042(19) 0.0003(19) 0.0078(19) C16A 0.026(3) 0.041(8) 0.027(4) 0.004(4) -0.001(2) 0.006(4) C17A 0.026(3) 0.059(4) 0.060(6) 0.026(3) -0.004(3) 0.008(3) C18A 0.027(3) 0.085(8) 0.083(6) 0.046(5) 0.001(3) 0.005(4) C19A 0.030(4) 0.075(10) 0.067(8) 0.019(8) -0.013(4) 0.006(6) C20A 0.036(4) 0.084(9) 0.041(6) 0.018(6) -0.010(4) 0.009(6) C21A 0.034(4) 0.077(10) 0.032(6) 0.005(6) -0.003(4) -0.001(6) C16B 0.026(3) 0.041(8) 0.027(4) 0.004(4) -0.001(2) 0.006(4) C17B 0.026(3) 0.059(4) 0.060(6) 0.026(3) -0.004(3) 0.008(3) C18B 0.027(3) 0.085(8) 0.083(6) 0.046(5) 0.001(3) 0.005(4) C19B 0.030(4) 0.075(10) 0.067(8) 0.019(8) -0.013(4) 0.006(6) C20B 0.036(4) 0.084(9) 0.041(6) 0.018(6) -0.010(4) 0.009(6) C21B 0.034(4) 0.077(10) 0.032(6) 0.005(6) -0.003(4) -0.001(6) O7 0.033(2) 0.0217(17) 0.0302(19) 0.0003(14) 0.0074(15) 0.0066(14) O8 0.0333(16) 0.0227(15) 0.0252(17) 0.0034(15) 0.0084(17) 0.0066(13) C22 0.021(2) 0.023(2) 0.035(3) 0.0024(19) 0.0027(19) 0.0071(18) C23A 0.051(5) 0.023(3) 0.033(4) -0.001(2) 0.013(3) 0.007(3) C24A 0.055(5) 0.029(3) 0.054(5) -0.002(3) 0.033(3) 0.006(3) C25A 0.093(6) 0.022(3) 0.088(6) -0.002(3) 0.051(5) 0.006(3) C26A 0.096(14) 0.029(3) 0.068(8) -0.009(4) 0.016(9) 0.013(6) C27A 0.112(11) 0.042(5) 0.029(6) -0.004(4) 0.007(6) 0.033(7) C28A 0.081(11) 0.034(4) 0.034(7) -0.001(4) 0.013(7) 0.011(6) C23B 0.051(5) 0.023(3) 0.033(4) -0.001(2) 0.013(3) 0.007(3) C24B 0.055(5) 0.029(3) 0.054(5) -0.002(3) 0.033(3) 0.006(3) C25B 0.093(6) 0.022(3) 0.088(6) -0.002(3) 0.051(5) 0.006(3) C26B 0.096(14) 0.029(3) 0.068(8) -0.009(4) 0.016(9) 0.013(6) C27B 0.112(11) 0.042(5) 0.029(6) -0.004(4) 0.007(6) 0.033(7) C28B 0.081(11) 0.034(4) 0.034(7) -0.001(4) 0.013(7) 0.011(6) _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 Ho1 O2 2.255(3) 6_554 ? Ho1 O4 2.257(3) 6_554 ? Ho1 O3 2.353(3) . ? Ho1 O1 2.360(3) . ? Ho1 O8 2.375(3) . ? Ho1 O5 2.378(3) . ? Ho1 O7 2.481(3) . ? Ho1 O6 2.489(3) . ? Na1 O8 2.378(4) 4_564 ? Na1 O5 2.380(4) . ? Na1 O6 2.395(4) 4_564 ? Na1 O7 2.397(4) . ? Na1 O1 2.608(4) 4_564 ? Na1 O3 2.608(4) . ? O1 C1 1.273(6) . ? O1 Na1 2.608(4) 3_645 ? O2 C1 1.260(6) . ? O2 Ho1 2.255(3) 6_554 ? C1 C2 1.493(7) . ? C2 C3 1.386(7) . ? C2 C7 1.399(7) . ? C3 C4 1.399(7) . ? C3 H3A 0.9500 . ? C4 C5 1.366(9) . ? C4 H4A 0.9500 . ? C5 C6 1.375(10) . ? C5 H5A 0.9500 . ? C6 C7 1.382(8) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? O3 C8 1.278(6) . ? O4 C8 1.256(6) . ? O4 Ho1 2.257(3) 6_554 ? C8 C9 1.494(7) . ? C9 C10 1.382(7) . ? C9 C14 1.395(7) . ? C10 C11 1.402(7) . ? C10 H10A 0.9500 . ? C11 C12 1.373(9) . ? C11 H11A 0.9500 . ? C12 C13 1.382(10) . ? C12 H12A 0.9500 . ? C13 C14 1.378(8) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? O5 C15 1.272(5) . ? O6 C15 1.263(5) . ? O6 Na1 2.395(4) 3_645 ? C15 C16A 1.453(12) . ? C15 C16B 1.537(12) . ? C16A C17A 1.3900 . ? C16A C21A 1.3900 . ? C17A C18A 1.3900 . ? C17A H17A 0.9500 . ? C18A C19A 1.3900 . ? C18A H18A 0.9500 . ? C19A C20A 1.3900 . ? C19A H19A 0.9500 . ? C20A C21A 1.3900 . ? C20A H20A 0.9500 . ? C21A H21A 0.9500 . ? C16B C17B 1.3900 . ? C16B C21B 1.3900 . ? C17B C18B 1.3900 . ? C17B H17B 0.9500 . ? C18B C19B 1.3900 . ? C18B H18B 0.9500 . ? C19B C20B 1.3900 . ? C19B H19B 0.9500 . ? C20B C21B 1.3900 . ? C20B H20B 0.9500 . ? C21B H21B 0.9500 . ? O7 C22 1.271(5) . ? O8 C22 1.272(5) . ? O8 Na1 2.378(4) 3_645 ? C22 C23B 1.449(15) . ? C22 C23A 1.527(14) . ? C23A C24A 1.3900 . ? C23A C28A 1.3900 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A C27A 1.3900 . ? C26A H26A 0.9500 . ? C27A C28A 1.3900 . ? C27A H27A 0.9500 . ? C28A H28A 0.9500 . ? C23B C24B 1.3900 . ? C23B C28B 1.3900 . ? C24B C25B 1.3900 . ? C24B H24B 0.9500 . ? C25B C26B 1.3900 . ? C25B H25B 0.9500 . ? C26B C27B 1.3900 . ? C26B H26B 0.9500 . ? C27B C28B 1.3900 . ? C27B H27B 0.9500 . ? C28B H28B 0.9500 . ? 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 O2 Ho1 O4 109.00(12) 6_554 6_554 ? O2 Ho1 O3 84.57(11) 6_554 . ? O4 Ho1 O3 79.56(11) 6_554 . ? O2 Ho1 O1 79.53(11) 6_554 . ? O4 Ho1 O1 84.52(11) 6_554 . ? O3 Ho1 O1 152.44(10) . . ? O2 Ho1 O8 144.43(11) 6_554 . ? O4 Ho1 O8 89.56(11) 6_554 . ? O3 Ho1 O8 129.54(11) . . ? O1 Ho1 O8 72.18(10) . . ? O2 Ho1 O5 89.45(11) 6_554 . ? O4 Ho1 O5 144.67(12) 6_554 . ? O3 Ho1 O5 72.33(11) . . ? O1 Ho1 O5 129.37(11) . . ? O8 Ho1 O5 92.10(10) . . ? O2 Ho1 O7 155.80(11) 6_554 . ? O4 Ho1 O7 81.45(11) 6_554 . ? O3 Ho1 O7 75.77(11) . . ? O1 Ho1 O7 123.96(11) . . ? O8 Ho1 O7 53.85(11) . . ? O5 Ho1 O7 71.36(11) . . ? O2 Ho1 O6 81.41(12) 6_554 . ? O4 Ho1 O6 155.66(11) 6_554 . ? O3 Ho1 O6 124.09(11) . . ? O1 Ho1 O6 75.65(11) . . ? O8 Ho1 O6 71.16(11) . . ? O5 Ho1 O6 53.80(11) . . ? O7 Ho1 O6 97.91(10) . . ? O8 Na1 O5 171.08(14) 4_564 . ? O8 Na1 O6 72.78(12) 4_564 4_564 ? O5 Na1 O6 112.68(13) . 4_564 ? O8 Na1 O7 112.78(13) 4_564 . ? O5 Na1 O7 72.82(12) . . ? O6 Na1 O7 108.65(13) 4_564 . ? O8 Na1 O1 67.85(11) 4_564 4_564 ? O5 Na1 O1 106.37(12) . 4_564 ? O6 Na1 O1 72.85(12) 4_564 4_564 ? O7 Na1 O1 178.47(15) . 4_564 ? O8 Na1 O3 106.50(12) 4_564 . ? O5 Na1 O3 67.88(11) . . ? O6 Na1 O3 178.65(15) 4_564 . ? O7 Na1 O3 72.67(12) . . ? O1 Na1 O3 105.83(12) 4_564 . ? C1 O1 Ho1 119.6(3) . . ? C1 O1 Na1 148.6(3) . 3_645 ? Ho1 O1 Na1 91.80(11) . 3_645 ? C1 O2 Ho1 161.8(3) . 6_554 ? O2 C1 O1 123.4(5) . . ? O2 C1 C2 118.1(4) . . ? O1 C1 C2 118.5(4) . . ? C3 C2 C7 119.4(5) . . ? C3 C2 C1 120.9(4) . . ? C7 C2 C1 119.7(5) . . ? C2 C3 C4 119.8(5) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C5 C4 C3 120.1(6) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 120.4(5) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C5 C6 C7 120.5(6) . . ? C5 C6 H6A 119.7 . . ? C7 C6 H6A 119.7 . . ? C6 C7 C2 119.7(6) . . ? C6 C7 H7A 120.2 . . ? C2 C7 H7A 120.2 . . ? C8 O3 Ho1 119.9(3) . . ? C8 O3 Na1 148.3(3) . . ? Ho1 O3 Na1 91.82(11) . . ? C8 O4 Ho1 161.8(3) . 6_554 ? O4 C8 O3 123.1(5) . . ? O4 C8 C9 118.6(4) . . ? O3 C8 C9 118.3(4) . . ? C10 C9 C14 119.6(5) . . ? C10 C9 C8 121.3(4) . . ? C14 C9 C8 119.1(5) . . ? C9 C10 C11 120.1(5) . . ? C9 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C12 C11 C10 119.3(5) . . ? C12 C11 H11A 120.4 . . ? C10 C11 H11A 120.4 . . ? C11 C12 C13 121.0(5) . . ? C11 C12 H12A 119.5 . . ? C13 C12 H12A 119.5 . . ? C14 C13 C12 119.8(6) . . ? C14 C13 H13A 120.1 . . ? C12 C13 H13A 120.1 . . ? C13 C14 C9 120.2(6) . . ? C13 C14 H14A 119.9 . . ? C9 C14 H14A 119.9 . . ? C15 O5 Ho1 95.1(3) . . ? C15 O5 Na1 151.3(3) . . ? Ho1 O5 Na1 97.17(13) . . ? C15 O6 Na1 145.2(3) . 3_645 ? C15 O6 Ho1 90.2(3) . . ? Na1 O6 Ho1 93.98(13) 3_645 . ? O6 C15 O5 120.8(4) . . ? O6 C15 C16A 121.2(8) . . ? O5 C15 C16A 117.6(7) . . ? O6 C15 C16B 120.4(7) . . ? O5 C15 C16B 118.4(7) . . ? C17A C16A C21A 120.0 . . ? C17A C16A C15 120.5(11) . . ? C21A C16A C15 119.4(11) . . ? C16A C17A C18A 120.0 . . ? C16A C17A H17A 120.0 . . ? C18A C17A H17A 120.0 . . ? C19A C18A C17A 120.0 . . ? C19A C18A H18A 120.0 . . ? C17A C18A H18A 120.0 . . ? C18A C19A C20A 120.0 . . ? C18A C19A H19A 120.0 . . ? C20A C19A H19A 120.0 . . ? C19A C20A C21A 120.0 . . ? C19A C20A H20A 120.0 . . ? C21A C20A H20A 120.0 . . ? C20A C21A C16A 120.0 . . ? C20A C21A H21A 120.0 . . ? C16A C21A H21A 120.0 . . ? C17B C16B C21B 120.0 . . ? C17B C16B C15 118.5(11) . . ? C21B C16B C15 121.5(11) . . ? C16B C17B C18B 120.0 . . ? C16B C17B H17B 120.0 . . ? C18B C17B H17B 120.0 . . ? C19B C18B C17B 120.0 . . ? C19B C18B H18B 120.0 . . ? C17B C18B H18B 120.0 . . ? C18B C19B C20B 120.0 . . ? C18B C19B H19B 120.0 . . ? C20B C19B H19B 120.0 . . ? C21B C20B C19B 120.0 . . ? C21B C20B H20B 120.0 . . ? C19B C20B H20B 120.0 . . ? C20B C21B C16B 120.0 . . ? C20B C21B H21B 120.0 . . ? C16B C21B H21B 120.0 . . ? C22 O7 Na1 145.2(3) . . ? C22 O7 Ho1 90.6(3) . . ? Na1 O7 Ho1 94.00(12) . . ? C22 O8 Ho1 95.5(2) . . ? C22 O8 Na1 151.3(3) . 3_645 ? Ho1 O8 Na1 97.44(13) . 3_645 ? O7 C22 O8 119.9(4) . . ? O7 C22 C23B 121.6(9) . . ? O8 C22 C23B 118.3(8) . . ? O7 C22 C23A 120.3(8) . . ? O8 C22 C23A 119.6(8) . . ? C24A C23A C28A 120.0 . . ? C24A C23A C22 118.6(13) . . ? C28A C23A C22 121.4(13) . . ? C25A C24A C23A 120.0 . . ? C25A C24A H24A 120.0 . . ? C23A C24A H24A 120.0 . . ? C24A C25A C26A 120.0 . . ? C24A C25A H25A 120.0 . . ? C26A C25A H25A 120.0 . . ? C25A C26A C27A 120.0 . . ? C25A C26A H26A 120.0 . . ? C27A C26A H26A 120.0 . . ? C28A C27A C26A 120.0 . . ? C28A C27A H27A 120.0 . . ? C26A C27A H27A 120.0 . . ? C27A C28A C23A 120.0 . . ? C27A C28A H28A 120.0 . . ? C23A C28A H28A 120.0 . . ? C24B C23B C28B 120.0 . . ? C24B C23B C22 120.6(13) . . ? C28B C23B C22 119.4(13) . . ? C23B C24B C25B 120.0 . . ? C23B C24B H24B 120.0 . . ? C25B C24B H24B 120.0 . . ? C26B C25B C24B 120.0 . . ? C26B C25B H25B 120.0 . . ? C24B C25B H25B 120.0 . . ? C25B C26B C27B 120.0 . . ? C25B C26B H26B 120.0 . . ? C27B C26B H26B 120.0 . . ? C26B C27B C28B 120.0 . . ? C26B C27B H27B 120.0 . . ? C28B C27B H27B 120.0 . . ? C27B C28B C23B 120.0 . . ? C27B C28B H28B 120.0 . . ? C23B C28B H28B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.959 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.080 ####################################################### data_z589 _database_code_depnum_ccdc_archive 'CCDC 751550' #TrackingRef 'NaLn-helices2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H20 Dy Na O8' _chemical_formula_weight 669.93 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 'I 41' _symmetry_space_group_name_Hall 'I 4bw' 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+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' _cell_length_a 16.1379(15) _cell_length_b 16.1379(15) _cell_length_c 19.5507(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5091.6(8) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2310 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 26.27 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2632 _exptl_absorpt_coefficient_mu 3.003 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.655 _exptl_absorpt_correction_T_max 0.897 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker AXS Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9112 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0546 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.16 _reflns_number_total 4512 _reflns_number_gt 4099 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_data_reduction 'SAINT+ 6.45 (Bruker AXS Inc., 2003)' _computing_structure_solution 'SHELXTL 6.12 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.12 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'SHELXTL 6.12 (BrukerAXS Inc., 2003)' _computing_publication_material 'SHELXTL 6.12 (BrukerAXS Inc., 2003)' _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. The phenyl groups of two of the four benzoate ligands were disordered, and each was refined as a pair of rigid hexagons with 50:50 occupancy. For each ligand, the dihedral between the planes of the two hexagons was relatively small, and corresponding pairs of carbon atoms could be refined with common anisotropic thermal parameters. All H-atoms were placed in calculated positions. ; _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^)+(0.0658P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _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, 1304 Friedel pairs' _refine_ls_abs_structure_Flack 0.18(2) _refine_ls_number_reflns 4512 _refine_ls_number_parameters 332 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.0997 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.059 _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 0.588132(18) 0.411859(19) 0.68673(4) 0.01804(10) Uani 1 1 d . . . Na1 Na 0.7500(2) 0.4029(2) 0.56176(19) 0.0282(7) Uani 1 1 d . A . O1 O 0.5000(3) 0.3711(3) 0.7777(3) 0.0219(11) Uani 1 1 d . . . O2 O 0.4100(3) 0.4715(3) 0.7511(3) 0.0239(12) Uani 1 1 d . . . C1 C 0.4339(6) 0.4114(5) 0.7887(5) 0.0229(18) Uani 1 1 d . . . C2 C 0.3802(6) 0.3875(5) 0.8467(5) 0.032(2) Uani 1 1 d . . . C3 C 0.4027(6) 0.3238(5) 0.8908(5) 0.031(2) Uani 1 1 d . . . H3A H 0.4518 0.2929 0.8828 0.037 Uiso 1 1 calc R . . C4 C 0.3526(8) 0.3058(6) 0.9469(6) 0.053(3) Uani 1 1 d . . . H4A H 0.3684 0.2628 0.9775 0.063 Uiso 1 1 calc R . . C5 C 0.2807(9) 0.3492(7) 0.9587(7) 0.072(4) Uani 1 1 d . . . H5A H 0.2483 0.3380 0.9982 0.086 Uiso 1 1 calc R . . C6 C 0.2556(9) 0.4098(8) 0.9122(9) 0.079(5) Uani 1 1 d . . . H6A H 0.2042 0.4374 0.9185 0.095 Uiso 1 1 calc R . . C7 C 0.3044(7) 0.4296(6) 0.8578(7) 0.052(3) Uani 1 1 d . . . H7A H 0.2875 0.4720 0.8271 0.062 Uiso 1 1 calc R . . O3 O 0.6286(3) 0.4999(3) 0.5958(3) 0.0241(12) Uani 1 1 d . . . O4 O 0.5290(3) 0.5895(3) 0.6220(3) 0.0244(12) Uani 1 1 d . . . C8 C 0.5888(4) 0.5667(6) 0.5859(5) 0.0201(17) Uani 1 1 d . . . C9 C 0.6128(5) 0.6200(6) 0.5258(5) 0.030(2) Uani 1 1 d . . . C10 C 0.6753(6) 0.5986(7) 0.4818(5) 0.039(2) Uani 1 1 d . . . H10A H 0.7063 0.5496 0.4903 0.047 Uiso 1 1 calc R . . C11 C 0.6943(6) 0.6461(8) 0.4258(6) 0.056(3) Uani 1 1 d . . . H11A H 0.7366 0.6294 0.3950 0.067 Uiso 1 1 calc R . . C12 C 0.6509(8) 0.7183(10) 0.4152(7) 0.076(5) Uani 1 1 d . . . H12A H 0.6626 0.7509 0.3760 0.092 Uiso 1 1 calc R . . C13 C 0.5907(8) 0.7442(9) 0.4606(9) 0.083(6) Uani 1 1 d . . . H13A H 0.5635 0.7959 0.4544 0.099 Uiso 1 1 calc R . . C14 C 0.5709(7) 0.6946(7) 0.5143(7) 0.057(3) Uani 1 1 d . . . H14A H 0.5278 0.7108 0.5446 0.068 Uiso 1 1 calc R . . O5 O 0.7358(3) 0.4145(3) 0.6828(3) 0.0292(12) Uani 1 1 d . A . O6 O 0.6836(4) 0.3639(4) 0.7784(3) 0.0297(14) Uani 1 1 d . A . C15 C 0.7466(5) 0.3858(5) 0.7430(4) 0.0231(16) Uani 1 1 d U . . C16A C 0.8326(14) 0.3778(14) 0.7677(10) 0.040(3) Uani 0.50 1 d PGU A 1 C17A C 0.901(2) 0.414(2) 0.7363(12) 0.046(8) Uani 0.50 1 d PGU A 1 H17A H 0.8932 0.4471 0.6963 0.055 Uiso 0.50 1 calc PR A 1 C18A C 0.9795(16) 0.403(2) 0.7634(16) 0.088(7) Uani 0.50 1 d PGU A 1 H18A H 1.0260 0.4284 0.7419 0.106 Uiso 0.50 1 calc PR A 1 C19A C 0.9903(9) 0.356(2) 0.8219(16) 0.107(12) Uani 0.50 1 d PGU A 1 H19A H 1.0442 0.3481 0.8404 0.128 Uiso 0.50 1 calc PR A 1 C20A C 0.9223(10) 0.3190(14) 0.8533(10) 0.061(7) Uani 0.50 1 d PGU A 1 H20A H 0.9297 0.2863 0.8933 0.074 Uiso 0.50 1 calc PR A 1 C21A C 0.8434(9) 0.3301(10) 0.8262(8) 0.036(4) Uani 0.50 1 d PGU A 1 H21A H 0.7970 0.3050 0.8477 0.044 Uiso 0.50 1 calc PR A 1 C16B C 0.8296(14) 0.3821(14) 0.7744(10) 0.040(3) Uani 0.50 1 d PG A 2 C17B C 0.896(2) 0.3903(19) 0.7292(9) 0.046(8) Uani 0.50 1 d PG A 2 H17B H 0.8856 0.3942 0.6814 0.055 Uiso 0.50 1 calc PR A 2 C18B C 0.9764(16) 0.393(2) 0.7539(13) 0.088(7) Uani 0.50 1 d PG A 2 H18B H 1.0215 0.3983 0.7230 0.106 Uiso 0.50 1 calc PR A 2 C19B C 0.9911(9) 0.3870(19) 0.8238(15) 0.107(12) Uani 0.50 1 d PG A 2 H19B H 1.0462 0.3886 0.8407 0.128 Uiso 0.50 1 calc PR A 2 C20B C 0.9251(10) 0.3788(14) 0.8690(10) 0.061(7) Uani 0.50 1 d PG A 2 H20B H 0.9351 0.3749 0.9167 0.074 Uiso 0.50 1 calc PR A 2 C21B C 0.8443(9) 0.3764(11) 0.8443(9) 0.036(4) Uani 0.50 1 d PG A 2 H21B H 0.7992 0.3708 0.8751 0.044 Uiso 0.50 1 calc PR A 2 O7 O 0.6368(4) 0.3154(3) 0.5952(3) 0.0282(14) Uani 1 1 d . . . O8 O 0.5852(3) 0.2643(3) 0.6904(4) 0.0291(11) Uani 1 1 d . . . C22 C 0.6137(5) 0.2531(5) 0.6305(5) 0.0278(18) Uani 1 1 d U A . C23A C 0.6329(12) 0.1699(14) 0.6094(10) 0.021(4) Uani 0.50 1 d PGU A 1 C24A C 0.6035(17) 0.102(2) 0.6461(11) 0.050(5) Uani 0.50 1 d PGU A 1 H24A H 0.5772 0.1103 0.6890 0.060 Uiso 0.50 1 calc PR A 1 C25A C 0.6124(17) 0.0226(16) 0.6198(17) 0.081(7) Uani 0.50 1 d PGU A 1 H25A H 0.5923 -0.0236 0.6448 0.097 Uiso 0.50 1 calc PR A 1 C26A C 0.6508(13) 0.0108(9) 0.5569(16) 0.070(9) Uani 0.50 1 d PGU A 1 H26A H 0.6570 -0.0436 0.5390 0.084 Uiso 0.50 1 calc PR A 1 C27A C 0.6803(13) 0.0784(10) 0.5203(10) 0.062(7) Uani 0.50 1 d PGU A 1 H27A H 0.7066 0.0703 0.4773 0.075 Uiso 0.50 1 calc PR A 1 C28A C 0.6714(12) 0.1580(9) 0.5466(9) 0.047(5) Uani 0.50 1 d PGU A 1 H28A H 0.6915 0.2043 0.5215 0.057 Uiso 0.50 1 calc PR A 1 C23B C 0.6096(11) 0.1679(14) 0.5965(10) 0.021(4) Uani 0.50 1 d PG A 2 C24B C 0.5923(17) 0.102(2) 0.6396(9) 0.050(5) Uani 0.50 1 d PG A 2 H24B H 0.5812 0.1111 0.6866 0.060 Uiso 0.50 1 calc PR A 2 C25B C 0.5913(17) 0.0213(17) 0.6138(15) 0.081(7) Uani 0.50 1 d PG A 2 H25B H 0.5796 -0.0240 0.6433 0.097 Uiso 0.50 1 calc PR A 2 C26B C 0.6076(13) 0.0074(9) 0.5449(16) 0.070(9) Uani 0.50 1 d PG A 2 H26B H 0.6070 -0.0475 0.5273 0.084 Uiso 0.50 1 calc PR A 2 C27B C 0.6249(13) 0.0737(10) 0.5019(10) 0.062(7) Uani 0.50 1 d PG A 2 H27B H 0.6360 0.0641 0.4548 0.075 Uiso 0.50 1 calc PR A 2 C28B C 0.6258(12) 0.1539(9) 0.5276(9) 0.047(5) Uani 0.50 1 d PG A 2 H28B H 0.6376 0.1993 0.4982 0.057 Uiso 0.50 1 calc PR A 2 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 0.01454(17) 0.01466(17) 0.02493(15) 0.00254(15) 0.00245(15) 0.00173(12) Na1 0.0243(16) 0.0278(17) 0.0325(17) 0.0019(14) 0.0080(13) -0.0010(13) O1 0.018(3) 0.014(2) 0.033(3) 0.003(2) 0.006(2) 0.001(2) O2 0.028(3) 0.014(3) 0.030(3) 0.002(2) -0.001(2) -0.004(2) C1 0.024(4) 0.017(4) 0.028(5) 0.001(3) 0.002(4) -0.006(3) C2 0.040(5) 0.014(4) 0.041(6) -0.001(4) 0.017(4) 0.006(4) C3 0.035(5) 0.021(4) 0.036(5) -0.003(4) 0.007(4) -0.002(4) C4 0.089(8) 0.027(4) 0.043(7) 0.004(5) 0.026(6) -0.017(5) C5 0.107(11) 0.045(7) 0.063(8) 0.002(6) 0.064(8) 0.009(7) C6 0.081(10) 0.063(8) 0.093(13) 0.001(8) 0.059(9) 0.022(7) C7 0.047(6) 0.032(5) 0.076(8) 0.007(5) 0.029(6) 0.010(4) O3 0.016(2) 0.026(3) 0.030(3) 0.006(2) 0.006(2) 0.004(2) O4 0.018(3) 0.024(3) 0.031(3) 0.000(2) -0.003(2) -0.005(2) C8 0.013(4) 0.022(4) 0.026(4) 0.000(4) -0.004(3) -0.002(3) C9 0.013(4) 0.040(5) 0.036(5) 0.011(4) -0.005(4) 0.004(4) C10 0.021(4) 0.056(6) 0.041(6) 0.011(5) 0.001(4) -0.001(4) C11 0.027(5) 0.090(9) 0.051(8) 0.017(7) 0.004(5) -0.009(5) C12 0.045(7) 0.109(11) 0.075(10) 0.070(9) 0.006(6) 0.006(7) C13 0.056(8) 0.090(11) 0.102(14) 0.074(10) 0.005(8) 0.021(7) C14 0.040(6) 0.052(7) 0.077(9) 0.036(6) 0.008(6) 0.022(5) O5 0.020(2) 0.032(3) 0.035(3) 0.013(3) 0.003(3) 0.007(2) O6 0.022(3) 0.029(3) 0.038(3) 0.013(3) 0.008(3) 0.007(2) C15 0.019(3) 0.016(3) 0.035(4) 0.007(3) 0.001(3) 0.006(3) C16A 0.016(4) 0.056(6) 0.048(6) 0.021(5) 0.002(4) 0.009(4) C17A 0.026(5) 0.035(19) 0.077(12) 0.043(11) -0.010(7) -0.005(9) C18A 0.012(4) 0.128(15) 0.124(15) 0.088(12) 0.003(7) 0.014(6) C19A 0.019(5) 0.18(3) 0.123(16) 0.104(17) -0.014(7) 0.004(9) C20A 0.026(6) 0.104(19) 0.053(12) 0.035(13) -0.007(7) 0.011(11) C21A 0.024(5) 0.051(11) 0.034(9) 0.011(7) -0.001(5) 0.004(8) C16B 0.016(4) 0.056(6) 0.048(6) 0.021(5) 0.002(4) 0.009(4) C17B 0.026(5) 0.035(19) 0.077(12) 0.043(11) -0.010(7) -0.005(9) C18B 0.012(4) 0.128(15) 0.124(15) 0.088(12) 0.003(7) 0.014(6) C19B 0.019(5) 0.18(3) 0.123(16) 0.104(17) -0.014(7) 0.004(9) C20B 0.026(6) 0.104(19) 0.053(12) 0.035(13) -0.007(7) 0.011(11) C21B 0.024(5) 0.051(11) 0.034(9) 0.011(7) -0.001(5) 0.004(8) O7 0.033(3) 0.012(3) 0.040(3) 0.003(2) 0.011(3) 0.007(2) O8 0.031(3) 0.023(3) 0.033(3) 0.007(3) 0.008(3) 0.007(2) C22 0.019(4) 0.021(4) 0.043(5) -0.001(3) 0.010(4) 0.005(3) C23A 0.010(11) 0.020(4) 0.032(8) -0.005(5) -0.005(7) 0.005(7) C24A 0.063(9) 0.021(4) 0.066(10) -0.006(5) 0.042(8) 0.005(6) C25A 0.100(17) 0.016(4) 0.127(13) 0.001(7) 0.079(13) 0.005(8) C26A 0.08(2) 0.023(5) 0.107(17) -0.014(8) 0.05(2) 0.005(10) C27A 0.12(2) 0.023(6) 0.046(12) -0.017(7) 0.020(12) 0.002(12) C28A 0.079(17) 0.022(5) 0.040(11) -0.010(6) 0.018(10) -0.011(9) C23B 0.010(11) 0.020(4) 0.032(8) -0.005(5) -0.005(7) 0.005(7) C24B 0.063(9) 0.021(4) 0.066(10) -0.006(5) 0.042(8) 0.005(6) C25B 0.100(17) 0.016(4) 0.127(13) 0.001(7) 0.079(13) 0.005(8) C26B 0.08(2) 0.023(5) 0.107(17) -0.014(8) 0.05(2) 0.005(10) C27B 0.12(2) 0.023(6) 0.046(12) -0.017(7) 0.020(12) 0.002(12) C28B 0.079(17) 0.022(5) 0.040(11) -0.010(6) 0.018(10) -0.011(9) _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 O2 2.265(5) 6_554 ? Dy1 O4 2.274(6) 6_554 ? Dy1 O3 2.368(6) . ? Dy1 O1 2.370(5) . ? Dy1 O8 2.383(5) . ? Dy1 O5 2.385(5) . ? Dy1 O6 2.487(6) . ? Dy1 O7 2.499(6) . ? Na1 O5 2.386(8) . ? Na1 O8 2.392(8) 4_564 ? Na1 O6 2.398(7) 4_564 ? Na1 O7 2.400(7) . ? Na1 O1 2.592(6) 4_564 ? Na1 O3 2.595(6) . ? O1 C1 1.268(10) . ? O1 Na1 2.592(6) 3_645 ? O2 C1 1.276(10) . ? O2 Dy1 2.265(5) 6_554 ? C1 C2 1.478(14) . ? C2 C3 1.390(13) . ? C2 C7 1.417(13) . ? C3 C4 1.394(14) . ? C3 H3A 0.9500 . ? C4 C5 1.375(18) . ? C4 H4A 0.9500 . ? C5 C6 1.40(2) . ? C5 H5A 0.9500 . ? C6 C7 1.361(17) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? O3 C8 1.270(10) . ? O4 C8 1.251(10) . ? O4 Dy1 2.274(6) 6_554 ? C8 C9 1.507(13) . ? C9 C10 1.370(13) . ? C9 C14 1.398(13) . ? C10 C11 1.370(15) . ? C10 H10A 0.9500 . ? C11 C12 1.375(18) . ? C11 H11A 0.9500 . ? C12 C13 1.38(2) . ? C12 H12A 0.9500 . ? C13 C14 1.359(16) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? O5 C15 1.276(10) . ? O6 C15 1.280(10) . ? O6 Na1 2.398(7) 3_645 ? C15 C16A 1.47(2) . ? C15 C16B 1.474(19) . ? C16A C17A 1.3900 . ? C16A C21A 1.3900 . ? C17A C18A 1.3900 . ? C17A H17A 0.9500 . ? C18A C19A 1.3900 . ? C18A H18A 0.9500 . ? C19A C20A 1.3900 . ? C19A H19A 0.9500 . ? C20A C21A 1.3900 . ? C20A H20A 0.9500 . ? C21A H21A 0.9500 . ? C16B C17B 1.3900 . ? C16B C21B 1.3900 . ? C17B C18B 1.3900 . ? C17B H17B 0.9500 . ? C18B C19B 1.3900 . ? C18B H18B 0.9500 . ? C19B C20B 1.3900 . ? C19B H19B 0.9500 . ? C20B C21B 1.3900 . ? C20B H20B 0.9500 . ? C21B H21B 0.9500 . ? O7 C22 1.274(10) . ? O8 C22 1.271(10) . ? O8 Na1 2.392(8) 3_645 ? C22 C23A 1.44(2) . ? C22 C23B 1.53(2) . ? C23A C24A 1.3900 . ? C23A C28A 1.3900 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A C27A 1.3900 . ? C26A H26A 0.9500 . ? C27A C28A 1.3900 . ? C27A H27A 0.9500 . ? C28A H28A 0.9500 . ? C23B C24B 1.3900 . ? C23B C28B 1.3900 . ? C24B C25B 1.3900 . ? C24B H24B 0.9500 . ? C25B C26B 1.3900 . ? C25B H25B 0.9500 . ? C26B C27B 1.3900 . ? C26B H26B 0.9500 . ? C27B C28B 1.3900 . ? C27B H27B 0.9500 . ? C28B H28B 0.9500 . ? 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 O2 Dy1 O4 109.2(2) 6_554 6_554 ? O2 Dy1 O3 85.1(2) 6_554 . ? O4 Dy1 O3 79.5(2) 6_554 . ? O2 Dy1 O1 79.7(2) 6_554 . ? O4 Dy1 O1 85.2(2) 6_554 . ? O3 Dy1 O1 153.55(17) . . ? O2 Dy1 O8 144.5(2) 6_554 . ? O4 Dy1 O8 89.4(2) 6_554 . ? O3 Dy1 O8 128.9(2) . . ? O1 Dy1 O8 71.85(19) . . ? O2 Dy1 O5 89.4(2) 6_554 . ? O4 Dy1 O5 144.4(2) 6_554 . ? O3 Dy1 O5 71.94(19) . . ? O1 Dy1 O5 128.9(2) . . ? O8 Dy1 O5 92.22(18) . . ? O2 Dy1 O6 81.4(2) 6_554 . ? O4 Dy1 O6 155.86(19) 6_554 . ? O3 Dy1 O6 123.86(19) . . ? O1 Dy1 O6 75.22(19) . . ? O8 Dy1 O6 71.3(2) . . ? O5 Dy1 O6 53.8(2) . . ? O2 Dy1 O7 155.75(19) 6_554 . ? O4 Dy1 O7 81.8(2) 6_554 . ? O3 Dy1 O7 75.49(19) . . ? O1 Dy1 O7 123.58(19) . . ? O8 Dy1 O7 53.5(2) . . ? O5 Dy1 O7 71.0(2) . . ? O6 Dy1 O7 97.31(19) . . ? O5 Na1 O8 170.9(2) . 4_564 ? O5 Na1 O6 112.9(2) . 4_564 ? O8 Na1 O6 72.7(2) 4_564 4_564 ? O5 Na1 O7 72.7(2) . . ? O8 Na1 O7 113.0(2) 4_564 . ? O6 Na1 O7 108.3(2) 4_564 . ? O5 Na1 O1 106.3(2) . 4_564 ? O8 Na1 O1 67.89(19) 4_564 4_564 ? O6 Na1 O1 72.8(2) 4_564 4_564 ? O7 Na1 O1 178.7(3) . 4_564 ? O5 Na1 O3 68.04(19) . . ? O8 Na1 O3 106.2(2) 4_564 . ? O6 Na1 O3 178.4(3) 4_564 . ? O7 Na1 O3 73.2(2) . . ? O1 Na1 O3 105.7(2) 4_564 . ? C1 O1 Dy1 119.3(5) . . ? C1 O1 Na1 148.4(5) . 3_645 ? Dy1 O1 Na1 92.26(19) . 3_645 ? C1 O2 Dy1 161.3(6) . 6_554 ? O1 C1 O2 123.1(9) . . ? O1 C1 C2 119.3(8) . . ? O2 C1 C2 117.6(8) . . ? C3 C2 C7 119.0(9) . . ? C3 C2 C1 121.1(8) . . ? C7 C2 C1 119.9(9) . . ? C2 C3 C4 119.5(9) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C5 C4 C3 121.0(11) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C4 C5 C6 119.5(11) . . ? C4 C5 H5A 120.3 . . ? C6 C5 H5A 120.3 . . ? C7 C6 C5 120.4(12) . . ? C7 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? C6 C7 C2 120.4(12) . . ? C6 C7 H7A 119.8 . . ? C2 C7 H7A 119.8 . . ? C8 O3 Dy1 118.9(5) . . ? C8 O3 Na1 148.8(5) . . ? Dy1 O3 Na1 92.21(19) . . ? C8 O4 Dy1 162.2(6) . 6_554 ? O4 C8 O3 123.7(8) . . ? O4 C8 C9 118.1(8) . . ? O3 C8 C9 118.2(7) . . ? C10 C9 C14 118.2(9) . . ? C10 C9 C8 122.4(8) . . ? C14 C9 C8 119.4(9) . . ? C9 C10 C11 121.7(10) . . ? C9 C10 H10A 119.2 . . ? C11 C10 H10A 119.2 . . ? C10 C11 C12 118.7(11) . . ? C10 C11 H11A 120.7 . . ? C12 C11 H11A 120.7 . . ? C11 C12 C13 121.2(11) . . ? C11 C12 H12A 119.4 . . ? C13 C12 H12A 119.4 . . ? C14 C13 C12 118.9(12) . . ? C14 C13 H13A 120.6 . . ? C12 C13 H13A 120.6 . . ? C13 C14 C9 121.2(12) . . ? C13 C14 H14A 119.4 . . ? C9 C14 H14A 119.4 . . ? C15 O5 Dy1 95.8(4) . . ? C15 O5 Na1 150.8(5) . . ? Dy1 O5 Na1 97.2(2) . . ? C15 O6 Na1 145.3(5) . 3_645 ? C15 O6 Dy1 91.0(5) . . ? Na1 O6 Dy1 94.2(2) 3_645 . ? O5 C15 O6 119.3(7) . . ? O5 C15 C16A 117.5(10) . . ? O6 C15 C16A 123.1(11) . . ? O5 C15 C16B 121.5(10) . . ? O6 C15 C16B 119.1(11) . . ? C17A C16A C21A 120.0 . . ? C17A C16A C15 124.1(14) . . ? C21A C16A C15 115.9(14) . . ? C18A C17A C16A 120.0 . . ? C18A C17A H17A 120.0 . . ? C16A C17A H17A 120.0 . . ? C17A C18A C19A 120.0 . . ? C17A C18A H18A 120.0 . . ? C19A C18A H18A 120.0 . . ? C20A C19A C18A 120.0 . . ? C20A C19A H19A 120.0 . . ? C18A C19A H19A 120.0 . . ? C19A C20A C21A 120.0 . . ? C19A C20A H20A 120.0 . . ? C21A C20A H20A 120.0 . . ? C20A C21A C16A 120.0 . . ? C20A C21A H21A 120.0 . . ? C16A C21A H21A 120.0 . . ? C17B C16B C21B 120.0 . . ? C17B C16B C15 115.4(16) . . ? C21B C16B C15 124.5(16) . . ? C16B C17B C18B 120.0 . . ? C16B C17B H17B 120.0 . . ? C18B C17B H17B 120.0 . . ? C17B C18B C19B 120.0 . . ? C17B C18B H18B 120.0 . . ? C19B C18B H18B 120.0 . . ? C18B C19B C20B 120.0 . . ? C18B C19B H19B 120.0 . . ? C20B C19B H19B 120.0 . . ? C21B C20B C19B 120.0 . . ? C21B C20B H20B 120.0 . . ? C19B C20B H20B 120.0 . . ? C20B C21B C16B 120.0 . . ? C20B C21B H21B 120.0 . . ? C16B C21B H21B 120.0 . . ? C22 O7 Na1 146.5(6) . . ? C22 O7 Dy1 90.7(5) . . ? Na1 O7 Dy1 93.9(2) . . ? C22 O8 Dy1 96.1(5) . . ? C22 O8 Na1 150.6(5) . 3_645 ? Dy1 O8 Na1 97.1(2) . 3_645 ? O8 C22 O7 119.5(7) . . ? O8 C22 C23A 118.3(11) . . ? O7 C22 C23A 121.2(12) . . ? O8 C22 C23B 120.8(11) . . ? O7 C22 C23B 119.1(12) . . ? C24A C23A C28A 120.0 . . ? C24A C23A C22 120.9(16) . . ? C28A C23A C22 118.5(17) . . ? C23A C24A C25A 120.0 . . ? C23A C24A H24A 120.0 . . ? C25A C24A H24A 120.0 . . ? C26A C25A C24A 120.0 . . ? C26A C25A H25A 120.0 . . ? C24A C25A H25A 120.0 . . ? C27A C26A C25A 120.0 . . ? C27A C26A H26A 120.0 . . ? C25A C26A H26A 120.0 . . ? C26A C27A C28A 120.0 . . ? C26A C27A H27A 120.0 . . ? C28A C27A H27A 120.0 . . ? C27A C28A C23A 120.0 . . ? C27A C28A H28A 120.0 . . ? C23A C28A H28A 120.0 . . ? C24B C23B C28B 120.0 . . ? C24B C23B C22 116.0(17) . . ? C28B C23B C22 123.9(17) . . ? C23B C24B C25B 120.0 . . ? C23B C24B H24B 120.0 . . ? C25B C24B H24B 120.0 . . ? C26B C25B C24B 120.0 . . ? C26B C25B H25B 120.0 . . ? C24B C25B H25B 120.0 . . ? C25B C26B C27B 120.0 . . ? C25B C26B H26B 120.0 . . ? C27B C26B H26B 120.0 . . ? C28B C27B C26B 120.0 . . ? C28B C27B H27B 120.0 . . ? C26B C27B H27B 120.0 . . ? C27B C28B C23B 120.0 . . ? C27B C28B H28B 120.0 . . ? C23B C28B H28B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.251 _refine_diff_density_min -1.025 _refine_diff_density_rms 0.130