Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' _publ_section_title ; A 3,12-connected vertice sharing adamantoid hydrogen bonded network featuring tetrameric clusters of cyclotriveratrylene ; _audit_creation_method SHELXL-97 _publ_contact_author_name ' Michaele J. Hardie' _publ_contact_author_address ; School of Chemistry University of Leeds Leeds LS2 9JT UNITED KINGDOM ; _publ_contact_author_email ' m.j.hardie@chem.leeds.ac.uk ' _publ_contact_author_fax ' 44-113-233 6565 ' loop_ _publ_author_name _publ_author_address ' Michaele J. Hardie ' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; ' Colin L. Raston' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; ' Antonio Salinas ' ; School of Chemistry Monash University Clayton 3168 Victoria AUSTRALIA ; data_c: _database_code_CSD 166360 _chemical_name_systematic ; octaaquostrontium(II) tetra(cyclotriveratrylene) tetrahydrate [cobalt(III)bis(dicarbollide)] acetonitrile clathrate ; _chemical_name_common '[Sr(H2O)8](H2O)4[(CH3CN)(CTV)][Co(C2B9H11)2]2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H50 B9 Co0.50 N O9 Sr0.25' _chemical_formula_weight 729.38 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' 'B' 'B' 0.0013 0.0007 '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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sr' 'Sr' -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x+1/2, z+1/2' '-x+1/2, -y+1/2, z' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'y, -x-1/2, -z-1/2' 'x-1/2, y-1/2, -z' '-y-1/2, x, -z-1/2' _cell_length_a 17.7771(2) _cell_length_b 17.7771(2) _cell_length_c 23.6753(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7481.99(15) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3064 _exptl_absorpt_coefficient_mu 0.648 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.9204 _exptl_absorpt_correction_T_max 0.9380 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 46587 _diffrn_reflns_av_R_equivalents 0.0796 _diffrn_reflns_av_sigmaI/netI 0.0659 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8567 _reflns_number_gt 6202 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0406P)^2^+3.3790P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8567 _refine_ls_number_parameters 658 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1023 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sr1 Sr 0.2500 0.2500 0.2500 0.01990(10) Uani 1 4 d S . . Co1 Co 0.7500 0.2500 0.035039(16) 0.01953(10) Uani 1 2 d S . . O1 O 0.63773(10) 0.88550(9) -0.05418(6) 0.0332(4) Uani 1 1 d . . . C1 C 0.65357(11) 0.85801(12) 0.10146(9) 0.0208(4) Uani 1 1 d . . . B1 B 0.63245(14) 0.25725(14) 0.03306(10) 0.0243(5) Uani 1 1 d . . . H1D H 0.6047(13) 0.2023(13) 0.0273(9) 0.027(6) Uiso 1 1 d . . . O2 O 0.64497(9) 0.74153(9) -0.05192(6) 0.0323(4) Uani 1 1 d . . . C2 C 0.64690(12) 0.89462(12) 0.04893(9) 0.0234(5) Uani 1 1 d . . . B2 B 0.67498(14) 0.29441(14) 0.09621(10) 0.0241(5) Uani 1 1 d . . . H2 H 0.6445(12) 0.9500(13) 0.0487(9) 0.026(6) Uiso 1 1 d . . . H2D H 0.6732(12) 0.2675(13) 0.1384(10) 0.027(6) Uiso 1 1 d . . . O3 O 0.44070(8) 0.55868(8) 0.15714(6) 0.0255(3) Uani 1 1 d . . . C3 C 0.64253(12) 0.85486(12) -0.00095(9) 0.0250(5) Uani 1 1 d . . . B3 B 0.74932(14) 0.35598(14) 0.07343(11) 0.0246(5) Uani 1 1 d . . . H3D H 0.8022(12) 0.3712(12) 0.0941(9) 0.024(6) Uiso 1 1 d . . . O4 O 0.36757(8) 0.63856(8) 0.22777(6) 0.0279(3) Uani 1 1 d . . . C4 C 0.64548(12) 0.77600(12) 0.00000(8) 0.0244(5) Uani 1 1 d . . . B4 B 0.70667(15) 0.43168(15) 0.03415(11) 0.0286(6) Uani 1 1 d . . . H4D H 0.7350(12) 0.4850(13) 0.0314(9) 0.024(6) Uiso 1 1 d . . . O5 O 0.38716(8) 1.03114(8) 0.23528(6) 0.0274(3) Uani 1 1 d . . . C5 C 0.65019(12) 0.73964(12) 0.05146(9) 0.0224(4) Uani 1 1 d . . . B5 B 0.66402(15) 0.39554(15) -0.02715(11) 0.0281(6) Uani 1 1 d . . . H5 H 0.6525(12) 0.6866(13) 0.0525(9) 0.025(6) Uiso 1 1 d . . . H5D H 0.6686(12) 0.4194(13) -0.0686(10) 0.029(6) Uiso 1 1 d . . . O6 O 0.46721(8) 1.10607(8) 0.16372(6) 0.0274(3) Uani 1 1 d . . . C6 C 0.65380(11) 0.77980(11) 0.10270(9) 0.0205(4) Uani 1 1 d . . . B6 B 0.59139(15) 0.33389(15) -0.00580(11) 0.0271(6) Uani 1 1 d . . . H6D H 0.5477(13) 0.3219(12) -0.0351(9) 0.027(6) Uiso 1 1 d . . . O7 O 0.28784(10) 0.50589(10) 0.16822(8) 0.0434(5) Uani 1 1 d D . . C7 C 0.65739(11) 0.73355(12) 0.15654(9) 0.0204(4) Uani 1 1 d . . . B7 B 0.58831(14) 0.33312(14) 0.06903(11) 0.0257(5) Uani 1 1 d . . . H7A H 0.6866(11) 0.7631(12) 0.1872(9) 0.018(5) Uiso 1 1 d . . . H7B H 0.6874(12) 0.6855(12) 0.1505(9) 0.021(5) Uiso 1 1 d . . . H7D H 0.5349(12) 0.3256(12) 0.0906(9) 0.025(6) Uiso 1 1 d . . . H7V H 0.2506(15) 0.5379(16) 0.1630(14) 0.073(11) Uiso 1 1 d D . . H7W H 0.3283(15) 0.5333(19) 0.1732(16) 0.093(13) Uiso 1 1 d D . . O8 O 0.31950(11) 0.37034(10) 0.21791(8) 0.0430(5) Uani 1 1 d D . . C8 C 0.58025(11) 0.71182(11) 0.17889(8) 0.0184(4) Uani 1 1 d . . . B8 B 0.66062(14) 0.39407(14) 0.09395(11) 0.0256(5) Uani 1 1 d . . . H8D H 0.6554(14) 0.4247(14) 0.1322(11) 0.040(7) Uiso 1 1 d . . . H8V H 0.2985(16) 0.4099(14) 0.1997(12) 0.063(10) Uiso 1 1 d D . . H8W H 0.3606(16) 0.384(2) 0.2362(16) 0.109(15) Uiso 1 1 d D . . O9 O 0.32249(11) 0.19373(11) 0.16372(8) 0.0426(4) Uani 1 1 d D . . C9 C 0.54701(11) 0.64618(11) 0.15697(9) 0.0199(4) Uani 1 1 d . . . B9 B 0.60854(15) 0.41799(15) 0.03204(11) 0.0276(5) Uani 1 1 d . . . H9 H 0.5751(12) 0.6173(12) 0.1301(9) 0.022(6) Uiso 1 1 d . . . H9D H 0.5676(13) 0.4656(14) 0.0290(10) 0.034(6) Uiso 1 1 d . . . H9V H 0.3558(17) 0.1576(16) 0.1693(16) 0.087(12) Uiso 1 1 d D . . H9W H 0.3253(17) 0.2037(17) 0.1271(8) 0.064(10) Uiso 1 1 d D . . C10 C 0.47677(11) 0.62274(11) 0.17428(8) 0.0208(4) Uani 1 1 d . . . C11 C 0.43684(11) 0.66637(12) 0.21380(8) 0.0214(4) Uani 1 1 d . . . C12 C 0.46934(12) 0.73009(12) 0.23572(8) 0.0202(4) Uani 1 1 d . . . H12 H 0.4443(11) 0.7595(11) 0.2628(9) 0.014(5) Uiso 1 1 d . . . C13 C 0.54166(11) 0.75403(11) 0.21892(8) 0.0195(4) Uani 1 1 d . . . C14 C 0.57311(12) 0.82456(11) 0.24630(9) 0.0202(4) Uani 1 1 d . . . H14A H 0.6285(13) 0.8224(12) 0.2471(9) 0.019(5) Uiso 1 1 d . . . H14B H 0.5573(12) 0.8249(12) 0.2841(10) 0.022(6) Uiso 1 1 d . . . C15 C 0.54801(11) 0.89826(11) 0.21997(8) 0.0194(4) Uani 1 1 d . . . C16 C 0.47996(12) 0.92935(12) 0.23896(9) 0.0217(4) Uani 1 1 d . . . H16 H 0.4515(12) 0.9039(12) 0.2667(9) 0.017(5) Uiso 1 1 d . . . C17 C 0.45319(12) 0.99714(12) 0.21899(9) 0.0227(4) Uani 1 1 d . . . C18 C 0.49620(12) 1.03742(11) 0.17928(9) 0.0218(4) Uani 1 1 d . . . C19 C 0.56266(12) 1.00665(12) 0.15987(9) 0.0219(4) Uani 1 1 d . . . H19 H 0.5924(12) 1.0347(13) 0.1366(9) 0.023(6) Uiso 1 1 d . . . C20 C 0.58959(11) 0.93675(11) 0.17897(8) 0.0197(4) Uani 1 1 d . . . C21 C 0.66255(12) 0.90725(12) 0.15403(9) 0.0214(4) Uani 1 1 d . . . H21A H 0.6929(14) 0.9508(14) 0.1432(10) 0.036(7) Uiso 1 1 d . . . H21B H 0.6896(12) 0.8807(12) 0.1825(9) 0.019(5) Uiso 1 1 d . . . C22 C 0.6364(2) 0.96524(15) -0.05902(12) 0.0437(7) Uani 1 1 d . . . H22A H 0.5924(15) 0.9855(14) -0.0379(11) 0.037(7) Uiso 1 1 d . . . H22B H 0.6315(15) 0.9760(15) -0.0997(13) 0.046(8) Uiso 1 1 d . . . H22C H 0.6868(17) 0.9875(16) -0.0430(12) 0.056(9) Uiso 1 1 d . . . C23 C 0.65004(17) 0.66111(14) -0.05295(12) 0.0359(6) Uani 1 1 d . . . H23A H 0.6519(13) 0.6478(13) -0.0930(11) 0.033(6) Uiso 1 1 d . . . H23B H 0.6955(14) 0.6432(13) -0.0347(10) 0.028(6) Uiso 1 1 d . . . H23C H 0.6056(15) 0.6396(15) -0.0340(11) 0.040(7) Uiso 1 1 d . . . C24 C 0.47860(14) 0.51376(14) 0.11589(10) 0.0284(5) Uani 1 1 d . . . H24A H 0.4474(13) 0.4728(14) 0.1102(9) 0.026(6) Uiso 1 1 d . . . H24B H 0.5275(14) 0.4959(13) 0.1312(10) 0.030(6) Uiso 1 1 d . . . H24C H 0.4871(13) 0.5435(14) 0.0807(11) 0.035(7) Uiso 1 1 d . . . C25 C 0.32263(16) 0.68477(19) 0.26268(15) 0.0490(8) Uani 1 1 d . . . H25A H 0.3451(18) 0.6936(18) 0.3009(15) 0.072(11) Uiso 1 1 d . . . H25B H 0.3161(17) 0.7339(19) 0.2445(13) 0.062(10) Uiso 1 1 d . . . H25C H 0.2760(17) 0.6574(16) 0.2661(12) 0.050(8) Uiso 1 1 d . . . C26 C 0.34062(15) 0.99083(16) 0.27432(11) 0.0347(6) Uani 1 1 d . . . H26A H 0.3271(16) 0.9410(18) 0.2582(12) 0.055(9) Uiso 1 1 d . . . H26B H 0.3675(15) 0.9840(14) 0.3091(12) 0.041(7) Uiso 1 1 d . . . H26C H 0.2938(16) 1.0202(15) 0.2805(11) 0.045(7) Uiso 1 1 d . . . C27 C 0.51134(15) 1.15017(15) 0.12542(13) 0.0383(6) Uani 1 1 d . . . H27A H 0.5178(15) 1.1238(15) 0.0884(12) 0.044(8) Uiso 1 1 d . . . H27B H 0.5630(17) 1.1607(16) 0.1420(12) 0.057(8) Uiso 1 1 d . . . H27C H 0.4838(15) 1.1947(15) 0.1209(10) 0.041(7) Uiso 1 1 d . . . C28 C 0.45356(15) 0.83452(18) 0.09977(12) 0.0371(6) Uani 1 1 d . . . H28A H 0.469(2) 0.788(2) 0.1143(15) 0.080(12) Uiso 1 1 d . . . H28B H 0.4534(16) 0.8297(16) 0.0579(14) 0.058(9) Uiso 1 1 d . . . H28C H 0.4844(19) 0.876(2) 0.1091(15) 0.079(11) Uiso 1 1 d . . . C29 C 0.37985(14) 0.85176(13) 0.12194(10) 0.0335(5) Uani 1 1 d . . . C30 C 0.74363(13) 0.35552(12) 0.00133(9) 0.0251(5) Uani 1 1 d . . . H30D H 0.7878(13) 0.3639(12) -0.0204(10) 0.025(6) Uiso 1 1 d . . . C31 C 0.67854(12) 0.29998(12) -0.02126(9) 0.0245(5) Uani 1 1 d . . . H31D H 0.6879(12) 0.2787(12) -0.0578(10) 0.027(6) Uiso 1 1 d . . . N45 N 0.32156(14) 0.86576(15) 0.13863(11) 0.0568(7) 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 Sr1 0.02018(13) 0.02018(13) 0.0193(2) 0.000 0.000 0.000 Co1 0.0209(2) 0.0218(2) 0.01595(19) 0.000 0.000 0.00008(16) O1 0.0515(10) 0.0281(9) 0.0200(8) 0.0037(6) -0.0032(7) -0.0059(8) C1 0.0142(10) 0.0255(11) 0.0227(11) -0.0002(8) 0.0004(8) 0.0004(8) B1 0.0227(12) 0.0280(13) 0.0222(12) -0.0002(10) -0.0022(10) 0.0014(11) O2 0.0468(10) 0.0284(9) 0.0217(8) -0.0037(6) 0.0003(7) -0.0035(8) C2 0.0226(11) 0.0220(11) 0.0256(11) 0.0019(9) -0.0001(8) -0.0018(9) B2 0.0248(13) 0.0293(13) 0.0181(12) -0.0007(10) 0.0021(10) 0.0010(11) O3 0.0213(8) 0.0241(8) 0.0311(8) -0.0087(6) 0.0032(6) -0.0023(6) C3 0.0253(11) 0.0275(12) 0.0221(12) 0.0038(9) -0.0007(8) -0.0034(9) B3 0.0265(13) 0.0249(13) 0.0224(12) -0.0025(10) 0.0013(10) -0.0021(11) O4 0.0210(8) 0.0301(8) 0.0325(9) -0.0065(7) 0.0081(6) -0.0039(7) C4 0.0246(11) 0.0284(12) 0.0201(11) -0.0026(8) 0.0022(8) -0.0024(10) B4 0.0307(14) 0.0239(13) 0.0312(14) -0.0001(11) 0.0063(11) 0.0002(11) O5 0.0246(8) 0.0256(8) 0.0321(8) 0.0027(6) 0.0065(6) 0.0027(7) C5 0.0213(11) 0.0211(11) 0.0247(11) 0.0001(9) 0.0004(8) -0.0008(9) B5 0.0330(14) 0.0278(13) 0.0234(13) 0.0041(10) 0.0037(10) 0.0084(11) O6 0.0268(8) 0.0193(8) 0.0360(9) 0.0054(6) 0.0032(7) 0.0017(6) C6 0.0132(10) 0.0242(11) 0.0240(11) 0.0004(8) 0.0010(8) 0.0004(8) B6 0.0261(14) 0.0321(14) 0.0232(13) -0.0014(10) -0.0028(10) 0.0055(11) O7 0.0308(10) 0.0365(10) 0.0630(13) 0.0140(9) -0.0049(9) -0.0084(9) C7 0.0175(10) 0.0223(11) 0.0214(11) 0.0004(8) -0.0010(8) 0.0014(9) B7 0.0236(13) 0.0294(13) 0.0243(13) 0.0012(10) 0.0024(10) 0.0018(11) O8 0.0430(11) 0.0349(10) 0.0511(12) 0.0140(9) -0.0175(9) -0.0145(9) C8 0.0165(10) 0.0202(10) 0.0184(10) 0.0041(8) -0.0013(8) 0.0023(8) B8 0.0270(13) 0.0281(13) 0.0216(13) -0.0023(10) 0.0026(10) 0.0025(11) O9 0.0494(11) 0.0515(11) 0.0268(10) 0.0040(8) 0.0131(8) 0.0183(10) C9 0.0198(10) 0.0223(11) 0.0176(10) 0.0005(8) -0.0005(8) 0.0057(9) B9 0.0291(13) 0.0297(14) 0.0241(13) -0.0010(10) 0.0023(10) 0.0050(11) C10 0.0196(10) 0.0224(11) 0.0204(10) 0.0009(8) -0.0039(8) 0.0006(9) C11 0.0186(10) 0.0243(11) 0.0212(10) 0.0024(8) 0.0015(8) 0.0006(9) C12 0.0213(11) 0.0222(11) 0.0172(10) -0.0003(8) 0.0016(8) 0.0039(9) C13 0.0208(10) 0.0202(10) 0.0175(10) 0.0028(8) -0.0022(8) 0.0025(8) C14 0.0221(11) 0.0221(10) 0.0165(11) 0.0002(8) -0.0019(8) 0.0006(9) C15 0.0215(10) 0.0197(10) 0.0169(10) -0.0022(8) -0.0044(8) -0.0023(8) C16 0.0245(11) 0.0227(11) 0.0179(11) -0.0012(8) -0.0006(8) -0.0036(9) C17 0.0226(11) 0.0233(11) 0.0221(11) -0.0040(9) -0.0007(8) 0.0007(9) C18 0.0232(11) 0.0187(10) 0.0235(11) 0.0000(8) -0.0037(9) -0.0010(9) C19 0.0217(11) 0.0224(11) 0.0214(11) -0.0008(9) 0.0007(8) -0.0054(9) C20 0.0209(10) 0.0203(10) 0.0179(10) -0.0028(8) -0.0034(8) -0.0032(8) C21 0.0188(10) 0.0231(11) 0.0222(11) 0.0006(9) -0.0019(8) -0.0028(9) C22 0.071(2) 0.0302(14) 0.0297(15) 0.0094(11) -0.0160(14) -0.0125(14) C23 0.0487(17) 0.0290(13) 0.0298(14) -0.0064(10) 0.0017(12) -0.0015(12) C24 0.0272(13) 0.0236(12) 0.0343(14) -0.0093(10) -0.0001(10) 0.0012(10) C25 0.0303(14) 0.0519(19) 0.065(2) -0.0243(16) 0.0256(14) -0.0125(14) C26 0.0283(13) 0.0426(16) 0.0333(14) 0.0069(12) 0.0099(11) 0.0040(12) C27 0.0302(14) 0.0241(13) 0.0606(19) 0.0161(12) 0.0074(13) -0.0006(11) C28 0.0340(14) 0.0475(17) 0.0299(14) -0.0072(12) -0.0071(11) 0.0029(13) C29 0.0344(14) 0.0322(13) 0.0338(13) -0.0018(10) -0.0114(11) 0.0004(11) C30 0.0256(12) 0.0256(12) 0.0241(12) 0.0013(9) 0.0062(9) -0.0010(10) C31 0.0268(11) 0.0273(11) 0.0193(11) -0.0010(9) -0.0019(9) 0.0041(9) N45 0.0386(14) 0.0679(18) 0.0640(17) -0.0054(13) -0.0092(12) 0.0109(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 Sr1 O8 2.5847(17) 3 ? Sr1 O8 2.5847(17) 6_566 ? Sr1 O8 2.5847(17) . ? Sr1 O8 2.5847(17) 8_656 ? Sr1 O9 2.6143(17) 8_656 ? Sr1 O9 2.6143(17) 6_566 ? Sr1 O9 2.6143(17) . ? Sr1 O9 2.6143(17) 3 ? Co1 C30 2.042(2) 3_655 ? Co1 C30 2.042(2) . ? Co1 C31 2.044(2) . ? Co1 C31 2.044(2) 3_655 ? Co1 B3 2.092(2) 3_655 ? Co1 B3 2.092(2) . ? Co1 B1 2.094(2) 3_655 ? Co1 B1 2.094(2) . ? Co1 B2 2.121(2) 3_655 ? Co1 B2 2.121(2) . ? O1 C3 1.376(2) . ? O1 C22 1.422(3) . ? C1 C6 1.391(3) . ? C1 C2 1.409(3) . ? C1 C21 1.530(3) . ? B1 C31 1.703(3) . ? B1 B7 1.778(4) . ? B1 B6 1.799(4) . ? B1 B2 1.801(3) . ? O2 C4 1.373(3) . ? O2 C23 1.433(3) . ? C2 C3 1.378(3) . ? B2 B8 1.791(4) . ? B2 B3 1.799(3) . ? B2 B7 1.806(3) . ? O3 C10 1.369(2) . ? O3 C24 1.430(3) . ? C3 C4 1.403(3) . ? B3 C30 1.710(3) . ? B3 B8 1.784(4) . ? B3 B4 1.803(4) . ? O4 C11 1.368(2) . ? O4 C25 1.413(3) . ? C4 C5 1.382(3) . ? B4 C30 1.694(3) . ? B4 B5 1.759(4) . ? B4 B9 1.762(4) . ? B4 B8 1.767(4) . ? O5 C17 1.376(3) . ? O5 C26 1.433(3) . ? C5 C6 1.409(3) . ? B5 C30 1.722(3) . ? B5 C31 1.724(3) . ? B5 B9 1.759(4) . ? B5 B6 1.767(4) . ? O6 C18 1.375(2) . ? O6 C27 1.433(3) . ? C6 C7 1.518(3) . ? B6 C31 1.702(3) . ? B6 B9 1.769(4) . ? B6 B7 1.773(3) . ? C7 C8 1.520(3) . ? B7 B9 1.781(4) . ? B7 B8 1.782(4) . ? C8 C13 1.390(3) . ? C8 C9 1.407(3) . ? B8 B9 1.785(4) . ? C9 C10 1.379(3) . ? C10 C11 1.407(3) . ? C11 C12 1.373(3) . ? C12 C13 1.411(3) . ? C13 C14 1.518(3) . ? C14 C15 1.518(3) . ? C15 C20 1.399(3) . ? C15 C16 1.404(3) . ? C16 C17 1.379(3) . ? C17 C18 1.408(3) . ? C18 C19 1.381(3) . ? C19 C20 1.406(3) . ? C20 C21 1.519(3) . ? C28 C29 1.445(4) . ? C29 N45 1.137(3) . ? C30 C31 1.612(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 O8 Sr1 O8 94.96(2) 3 6_566 ? O8 Sr1 O8 145.81(9) 3 . ? O8 Sr1 O8 94.96(2) 6_566 . ? O8 Sr1 O8 94.96(2) 3 8_656 ? O8 Sr1 O8 145.81(9) 6_566 8_656 ? O8 Sr1 O8 94.96(2) . 8_656 ? O8 Sr1 O9 145.15(6) 3 8_656 ? O8 Sr1 O9 71.89(6) 6_566 8_656 ? O8 Sr1 O9 68.82(6) . 8_656 ? O8 Sr1 O9 81.45(6) 8_656 8_656 ? O8 Sr1 O9 68.82(6) 3 6_566 ? O8 Sr1 O9 81.45(6) 6_566 6_566 ? O8 Sr1 O9 145.15(6) . 6_566 ? O8 Sr1 O9 71.89(6) 8_656 6_566 ? O9 Sr1 O9 77.22(8) 8_656 6_566 ? O8 Sr1 O9 71.89(6) 3 . ? O8 Sr1 O9 68.82(6) 6_566 . ? O8 Sr1 O9 81.45(6) . . ? O8 Sr1 O9 145.15(6) 8_656 . ? O9 Sr1 O9 127.63(5) 8_656 . ? O9 Sr1 O9 127.63(5) 6_566 . ? O8 Sr1 O9 81.45(6) 3 3 ? O8 Sr1 O9 145.15(6) 6_566 3 ? O8 Sr1 O9 71.89(6) . 3 ? O8 Sr1 O9 68.82(6) 8_656 3 ? O9 Sr1 O9 127.63(5) 8_656 3 ? O9 Sr1 O9 127.63(5) 6_566 3 ? O9 Sr1 O9 77.22(8) . 3 ? C30 Co1 C30 133.98(12) 3_655 . ? C30 Co1 C31 100.31(9) 3_655 . ? C30 Co1 C31 46.48(9) . . ? C30 Co1 C31 46.48(9) 3_655 3_655 ? C30 Co1 C31 100.31(9) . 3_655 ? C31 Co1 C31 98.63(12) . 3_655 ? C30 Co1 B3 48.86(9) 3_655 3_655 ? C30 Co1 B3 176.07(10) . 3_655 ? C31 Co1 B3 132.71(9) . 3_655 ? C31 Co1 B3 83.58(9) 3_655 3_655 ? C30 Co1 B3 176.07(10) 3_655 . ? C30 Co1 B3 48.86(9) . . ? C31 Co1 B3 83.58(9) . . ? C31 Co1 B3 132.71(9) 3_655 . ? B3 Co1 B3 128.49(14) 3_655 . ? C30 Co1 B1 83.07(9) 3_655 3_655 ? C30 Co1 B1 95.92(10) . 3_655 ? C31 Co1 B1 129.21(9) . 3_655 ? C31 Co1 B1 48.59(9) 3_655 3_655 ? B3 Co1 B1 87.05(10) 3_655 3_655 ? B3 Co1 B1 94.07(10) . 3_655 ? C30 Co1 B1 95.92(9) 3_655 . ? C30 Co1 B1 83.07(9) . . ? C31 Co1 B1 48.59(9) . . ? C31 Co1 B1 129.21(9) 3_655 . ? B3 Co1 B1 94.07(10) 3_655 . ? B3 Co1 B1 87.05(10) . . ? B1 Co1 B1 177.43(14) 3_655 . ? C30 Co1 B2 83.69(9) 3_655 3_655 ? C30 Co1 B2 130.07(9) . 3_655 ? C31 Co1 B2 175.99(9) . 3_655 ? C31 Co1 B2 83.84(9) 3_655 3_655 ? B3 Co1 B2 50.54(10) 3_655 3_655 ? B3 Co1 B2 92.42(10) . 3_655 ? B1 Co1 B2 50.58(10) 3_655 3_655 ? B1 Co1 B2 131.73(10) . 3_655 ? C30 Co1 B2 130.07(9) 3_655 . ? C30 Co1 B2 83.69(9) . . ? C31 Co1 B2 83.84(9) . . ? C31 Co1 B2 175.99(9) 3_655 . ? B3 Co1 B2 92.42(10) 3_655 . ? B3 Co1 B2 50.54(10) . . ? B1 Co1 B2 131.73(10) 3_655 . ? B1 Co1 B2 50.58(10) . . ? B2 Co1 B2 93.88(14) 3_655 . ? C3 O1 C22 118.01(18) . . ? C6 C1 C2 118.73(19) . . ? C6 C1 C21 123.68(19) . . ? C2 C1 C21 117.56(19) . . ? C31 B1 B7 103.63(17) . . ? C31 B1 B6 58.09(14) . . ? B7 B1 B6 59.42(14) . . ? C31 B1 B2 105.14(17) . . ? B7 B1 B2 60.61(14) . . ? B6 B1 B2 108.49(18) . . ? C31 B1 Co1 64.18(11) . . ? B7 B1 Co1 118.45(15) . . ? B6 B1 Co1 117.58(16) . . ? B2 B1 Co1 65.49(11) . . ? C4 O2 C23 117.39(18) . . ? C3 C2 C1 121.6(2) . . ? B8 B2 B3 59.59(14) . . ? B8 B2 B1 106.15(17) . . ? B3 B2 B1 106.42(17) . . ? B8 B2 B7 59.38(14) . . ? B3 B2 B7 106.74(17) . . ? B1 B2 B7 59.06(14) . . ? B8 B2 Co1 115.94(15) . . ? B3 B2 Co1 63.88(11) . . ? B1 B2 Co1 63.93(11) . . ? B7 B2 Co1 115.78(15) . . ? C10 O3 C24 116.51(16) . . ? O1 C3 C2 125.8(2) . . ? O1 C3 C4 114.38(18) . . ? C2 C3 C4 119.77(19) . . ? C30 B3 B8 102.79(17) . . ? C30 B3 B2 104.65(17) . . ? B8 B3 B2 59.98(14) . . ? C30 B3 B4 57.58(14) . . ? B8 B3 B4 59.02(14) . . ? B2 B3 B4 107.45(18) . . ? C30 B3 Co1 64.04(11) . . ? B8 B3 Co1 117.74(15) . . ? B2 B3 Co1 65.58(11) . . ? B4 B3 Co1 116.78(15) . . ? C11 O4 C25 116.13(18) . . ? O2 C4 C5 125.5(2) . . ? O2 C4 C3 115.54(18) . . ? C5 C4 C3 118.94(19) . . ? C30 B4 B5 59.78(14) . . ? C30 B4 B9 105.10(18) . . ? B5 B4 B9 59.96(15) . . ? C30 B4 B8 104.18(18) . . ? B5 B4 B8 108.86(18) . . ? B9 B4 B8 60.77(14) . . ? C30 B4 B3 58.45(14) . . ? B5 B4 B3 109.52(18) . . ? B9 B4 B3 109.14(18) . . ? B8 B4 B3 59.94(14) . . ? C17 O5 C26 116.99(17) . . ? C4 C5 C6 121.7(2) . . ? C30 B5 C31 55.80(13) . . ? C30 B5 B4 58.23(14) . . ? C31 B5 B4 103.21(17) . . ? C30 B5 B9 104.04(17) . . ? C31 B5 B9 104.06(18) . . ? B4 B5 B9 60.11(15) . . ? C30 B5 B6 103.43(17) . . ? C31 B5 B6 58.35(14) . . ? B4 B5 B6 107.78(18) . . ? B9 B5 B6 60.22(15) . . ? C18 O6 C27 116.75(17) . . ? C1 C6 C5 119.22(19) . . ? C1 C6 C7 124.00(19) . . ? C5 C6 C7 116.77(18) . . ? C31 B6 B5 59.55(14) . . ? C31 B6 B9 104.55(18) . . ? B5 B6 B9 59.67(15) . . ? C31 B6 B7 103.90(17) . . ? B5 B6 B7 108.25(18) . . ? B9 B6 B7 60.38(14) . . ? C31 B6 B1 58.15(13) . . ? B5 B6 B1 108.63(18) . . ? B9 B6 B1 108.13(18) . . ? B7 B6 B1 59.70(14) . . ? C6 C7 C8 113.07(16) . . ? B6 B7 B1 60.88(14) . . ? B6 B7 B9 59.72(14) . . ? B1 B7 B9 108.54(18) . . ? B6 B7 B8 107.70(18) . . ? B1 B7 B8 107.56(17) . . ? B9 B7 B8 60.14(14) . . ? B6 B7 B2 109.44(17) . . ? B1 B7 B2 60.33(14) . . ? B9 B7 B2 109.01(18) . . ? B8 B7 B2 59.89(14) . . ? C13 C8 C9 119.47(18) . . ? C13 C8 C7 123.06(18) . . ? C9 C8 C7 117.47(18) . . ? B4 B8 B7 107.40(18) . . ? B4 B8 B3 61.04(14) . . ? B7 B8 B3 108.46(17) . . ? B4 B8 B9 59.48(15) . . ? B7 B8 B9 59.92(14) . . ? B3 B8 B9 108.98(17) . . ? B4 B8 B2 109.41(17) . . ? B7 B8 B2 60.73(14) . . ? B3 B8 B2 60.43(14) . . ? B9 B8 B2 109.52(18) . . ? C10 C9 C8 121.41(19) . . ? B5 B9 B4 59.94(15) . . ? B5 B9 B6 60.11(15) . . ? B4 B9 B6 107.56(18) . . ? B5 B9 B7 108.22(18) . . ? B4 B9 B7 107.64(18) . . ? B6 B9 B7 59.90(14) . . ? B5 B9 B8 108.02(18) . . ? B4 B9 B8 59.75(14) . . ? B6 B9 B8 107.69(18) . . ? B7 B9 B8 59.95(14) . . ? O3 C10 C9 125.99(18) . . ? O3 C10 C11 114.79(17) . . ? C9 C10 C11 119.21(19) . . ? O4 C11 C12 125.84(18) . . ? O4 C11 C10 114.56(18) . . ? C12 C11 C10 119.57(18) . . ? C11 C12 C13 121.69(19) . . ? C8 C13 C12 118.62(18) . . ? C8 C13 C14 123.73(18) . . ? C12 C13 C14 117.65(18) . . ? C15 C14 C13 115.42(16) . . ? C20 C15 C16 119.01(18) . . ? C20 C15 C14 123.49(18) . . ? C16 C15 C14 117.49(18) . . ? C17 C16 C15 122.1(2) . . ? O5 C17 C16 125.61(19) . . ? O5 C17 C18 115.30(18) . . ? C16 C17 C18 119.08(19) . . ? O6 C18 C19 125.67(19) . . ? O6 C18 C17 115.27(18) . . ? C19 C18 C17 119.05(19) . . ? C18 C19 C20 122.3(2) . . ? C15 C20 C19 118.40(19) . . ? C15 C20 C21 123.52(18) . . ? C19 C20 C21 118.09(18) . . ? C20 C21 C1 115.14(17) . . ? N45 C29 C28 179.0(3) . . ? C31 C30 B4 111.30(18) . . ? C31 C30 B3 112.12(17) . . ? B4 C30 B3 63.97(15) . . ? C31 C30 B5 62.17(14) . . ? B4 C30 B5 61.99(15) . . ? B3 C30 B5 115.95(18) . . ? C31 C30 Co1 66.85(11) . . ? B4 C30 Co1 125.21(15) . . ? B3 C30 Co1 67.10(11) . . ? B5 C30 Co1 125.34(15) . . ? C30 C31 B6 111.41(17) . . ? C30 C31 B1 111.58(17) . . ? B6 C31 B1 63.76(14) . . ? C30 C31 B5 62.03(14) . . ? B6 C31 B5 62.11(15) . . ? B1 C31 B5 115.37(17) . . ? C30 C31 Co1 66.67(11) . . ? B6 C31 Co1 125.40(15) . . ? B1 C31 Co1 67.23(11) . . ? B5 C31 Co1 125.04(15) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.293 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.068 #===END data_c2: _database_code_CSD 166361 _audit_creation_method SHELXL-97 _chemical_name_systematic ; octaaquolanthanum/sodium tetra(cyclotriveratrylene)tetrahydrate [cobalt(III)bis(dicarbollide)] acetonitrile clathrate ; _chemical_name_common '[La0.5Na0.5(H2O)8](H2O)4[(CH3CN)(CTV)][Co(C2B9H11)2]2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H50 B9 Co0.50 La0.13 N Na0.13 O9' _chemical_formula_weight 727.71 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' 'B' 'B' 0.0013 0.0007 '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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x+1/2, z+1/2' '-x+1/2, -y+1/2, z' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'y, -x-1/2, -z-1/2' 'x-1/2, y-1/2, -z' '-y-1/2, x, -z-1/2' _cell_length_a 17.6914(3) _cell_length_b 17.6914(3) _cell_length_c 23.6592(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7405.0(2) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description fragment _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3056 _exptl_absorpt_coefficient_mu 0.441 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 45683 _diffrn_reflns_av_R_equivalents 0.068 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7271 _reflns_number_gt 5082 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1127P)^2^+25.0370P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7271 _refine_ls_number_parameters 459 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1130 _refine_ls_R_factor_gt 0.0776 _refine_ls_wR_factor_ref 0.2324 _refine_ls_wR_factor_gt 0.2068 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.2500 0.7500 0.03365(3) 0.0194(2) Uani 1 2 d S . . C11 C 0.3006(3) 0.8211(3) -0.02290(18) 0.0253(10) Uani 1 1 d . . . H11 H 0.2691 0.8156 -0.0637 0.030 Uiso 1 1 calc R . . B17 B 0.2954(3) 0.8242(3) 0.0951(2) 0.0252(11) Uani 1 1 d . . . H17 H 0.2643 0.8227 0.1363 0.030 Uiso 1 1 calc R . . B22 B 0.3956(3) 0.8383(3) 0.0928(2) 0.0280(11) Uani 1 1 d . . . H22 H 0.4287 0.8440 0.1329 0.034 Uiso 1 1 calc R . . B24 B 0.3967(3) 0.8350(3) -0.0289(2) 0.0290(12) Uani 1 1 d . . . H24 H 0.4290 0.8373 -0.0696 0.035 Uiso 1 1 calc R . . B25 B 0.4328(3) 0.7920(3) 0.0323(2) 0.0293(12) Uani 1 1 d . . . H25 H 0.4906 0.7660 0.0321 0.035 Uiso 1 1 calc R . . C27 C 0.3561(3) 0.7547(3) -0.00060(18) 0.0262(10) Uani 1 1 d . . . H27 H 0.3648 0.7013 -0.0252 0.031 Uiso 1 1 calc R . . B29 B 0.2594(3) 0.8677(3) 0.0316(2) 0.0241(10) Uani 1 1 d . . . H29 H 0.2023 0.8950 0.0304 0.029 Uiso 1 1 calc R . . B31 B 0.4202(3) 0.8909(3) 0.0304(2) 0.0273(11) Uani 1 1 d . . . H31 H 0.4690 0.9312 0.0297 0.033 Uiso 1 1 calc R . . B32 B 0.3351(3) 0.9115(3) 0.0676(2) 0.0280(11) Uani 1 1 d . . . H32 H 0.3278 0.9661 0.0909 0.034 Uiso 1 1 calc R . . B35 B 0.3355(3) 0.9086(3) -0.0071(2) 0.0275(11) Uani 1 1 d . . . H35 H 0.3276 0.9604 -0.0336 0.033 Uiso 1 1 calc R . . B36 B 0.3567(3) 0.7497(3) 0.0717(2) 0.0267(11) Uani 1 1 d . . . H36 H 0.3662 0.6973 0.0973 0.032 Uiso 1 1 calc R . . La2 La 0.2500 0.2500 0.2500 0.0445(3) Uani 0.50 4 d SP . 1 O3 O 0.05689(17) 0.56022(17) -0.15751(13) 0.0268(7) Uani 1 1 d . . . O1 O 0.60697(17) 0.53422(18) -0.16343(15) 0.0328(8) Uani 1 1 d . . . O2 O 0.13699(19) 0.63341(17) -0.22875(14) 0.0309(8) Uani 1 1 d . . . C3 C 0.2536(2) 0.4595(2) -0.21878(17) 0.0201(9) Uani 1 1 d . . . C4 C 0.1650(2) 0.5642(2) -0.21405(17) 0.0219(9) Uani 1 1 d . . . O5 O 0.53213(18) 0.61369(18) -0.23584(14) 0.0334(8) Uani 1 1 d . . . C6 C 0.4298(2) 0.5206(2) -0.23897(18) 0.0242(9) Uani 1 1 d . . . H6 H 0.4033 0.5489 -0.2667 0.029 Uiso 1 1 calc R . . C7 C 0.3985(2) 0.4525(2) -0.21944(17) 0.0220(9) Uani 1 1 d . . . C8 C 0.2114(2) 0.4209(2) -0.17872(17) 0.0189(8) Uani 1 1 d . . . C9 C 0.2295(2) 0.5313(2) -0.23632(17) 0.0205(9) Uani 1 1 d . . . H9 H 0.2579 0.5579 -0.2640 0.025 Uiso 1 1 calc R . . C10 C 0.2329(2) 0.3434(2) -0.15607(19) 0.0240(9) Uani 1 1 d . . . H10A H 0.1862 0.3140 -0.1491 0.029 Uiso 1 1 calc R . . H10B H 0.2626 0.3163 -0.1851 0.029 Uiso 1 1 calc R . . C12 C 0.2785(2) 0.3470(2) -0.10184(18) 0.0226(9) Uani 1 1 d . . . C13 C 0.1455(2) 0.4540(2) -0.15694(17) 0.0204(9) Uani 1 1 d . . . H13 H 0.1167 0.4274 -0.1295 0.024 Uiso 1 1 calc R . . C14 C 0.5383(2) 0.5050(3) -0.17876(19) 0.0265(10) Uani 1 1 d . . . O15 O 0.3825(2) 0.3588(2) 0.05638(16) 0.0514(11) Uani 1 1 d . . . C16 C 0.0125(3) 0.5220(3) -0.1158(2) 0.0308(11) Uani 1 1 d . . . H16A H -0.0322 0.5524 -0.1069 0.046 Uiso 1 1 calc R . . H16B H 0.0427 0.5148 -0.0815 0.046 Uiso 1 1 calc R . . H16C H -0.0033 0.4727 -0.1305 0.046 Uiso 1 1 calc R . . C18 C 0.4368(2) 0.4113(2) -0.17789(18) 0.0235(9) Uani 1 1 d . . . C19 C 0.3245(2) 0.4274(2) -0.24626(18) 0.0232(9) Uani 1 1 d . . . H19A H 0.3218 0.3715 -0.2448 0.028 Uiso 1 1 calc R . . H19B H 0.3250 0.4423 -0.2866 0.028 Uiso 1 1 calc R . . C20 C 0.3575(3) 0.3473(2) -0.1004(2) 0.0260(10) Uani 1 1 d . . . C21 C 0.4983(2) 0.5478(2) -0.21903(18) 0.0250(10) Uani 1 1 d . . . C23 C 0.5070(3) 0.4387(3) -0.1587(2) 0.0276(10) Uani 1 1 d . . . H23 H 0.5338 0.4106 -0.1310 0.033 Uiso 1 1 calc R . . C26 C 0.4073(3) 0.3382(2) -0.1529(2) 0.0276(10) Uani 1 1 d . . . H26A H 0.4510 0.3059 -0.1429 0.033 Uiso 1 1 calc R . . H26B H 0.3779 0.3113 -0.1822 0.033 Uiso 1 1 calc R . . O28 O 0.2378(2) 0.3548(2) 0.05248(14) 0.0429(9) Uani 1 1 d . . . C30 C 0.2736(3) 0.3546(3) 0.0010(2) 0.0336(12) Uani 1 1 d . . . C33 C 0.3524(3) 0.3568(3) 0.0027(2) 0.0359(12) Uani 1 1 d . . . C37 C 0.2380(3) 0.3506(2) -0.0509(2) 0.0278(10) Uani 1 1 d . . . H37 H 0.1844 0.3504 -0.0521 0.033 Uiso 1 1 calc R . . C38 C 0.3927(3) 0.3527(3) -0.0467(2) 0.0341(12) Uani 1 1 d . . . H38 H 0.4463 0.3534 -0.0449 0.041 Uiso 1 1 calc R . . C40 C 0.1821(4) 0.6777(3) -0.2650(3) 0.0556(17) Uani 1 1 d . . . H40A H 0.1563 0.7255 -0.2729 0.083 Uiso 1 1 calc R . . H40B H 0.1907 0.6503 -0.3004 0.083 Uiso 1 1 calc R . . H40C H 0.2308 0.6880 -0.2467 0.083 Uiso 1 1 calc R . . C41 C 0.4942(3) 0.6570(3) -0.2777(2) 0.0457(14) Uani 1 1 d . . . H41A H 0.5234 0.7028 -0.2858 0.069 Uiso 1 1 calc R . . H41B H 0.4439 0.6711 -0.2638 0.069 Uiso 1 1 calc R . . H41C H 0.4891 0.6270 -0.3123 0.069 Uiso 1 1 calc R . . C43 C 0.4621(4) 0.3621(5) 0.0614(3) 0.071(2) Uani 1 1 d . . . H43A H 0.4761 0.3627 0.1015 0.107 Uiso 1 1 calc R . . H43B H 0.4808 0.4081 0.0431 0.107 Uiso 1 1 calc R . . H43C H 0.4845 0.3178 0.0431 0.107 Uiso 1 1 calc R . . C44 C 0.6507(3) 0.4906(3) -0.1243(3) 0.0486(15) Uani 1 1 d . . . H44A H 0.6985 0.5166 -0.1166 0.073 Uiso 1 1 calc R . . H44B H 0.6611 0.4407 -0.1404 0.073 Uiso 1 1 calc R . . H44C H 0.6224 0.4847 -0.0889 0.073 Uiso 1 1 calc R . . C46 C 0.1569(3) 0.3525(3) 0.0523(2) 0.0470(14) Uani 1 1 d . . . H46A H 0.1383 0.3538 0.0913 0.071 Uiso 1 1 calc R . . H46B H 0.1399 0.3058 0.0340 0.071 Uiso 1 1 calc R . . H46C H 0.1373 0.3962 0.0316 0.071 Uiso 1 1 calc R . . O47 O 0.3689(3) 0.1898(3) 0.2294(4) 0.133(3) Uani 1 1 d . . . O49 O 0.3061(5) 0.3160(6) 0.1639(3) 0.147(3) Uani 1 1 d . . . O4 O 0.4970(2) 0.2095(2) 0.17301(18) 0.0547(11) Uani 1 1 d . A 1 C2 C 0.1218(2) 0.5246(2) -0.17462(17) 0.0209(9) Uani 1 1 d . . . N6 N 0.6279(4) 0.3188(3) 0.1450(3) 0.0750(18) Uani 1 1 d . . . C1 C 0.6656(3) 0.4468(3) 0.1029(2) 0.0430(13) Uani 1 1 d . . . H1A H 0.6317 0.4860 0.1176 0.064 Uiso 1 1 calc R . . H1B H 0.6611 0.4445 0.0617 0.064 Uiso 1 1 calc R . . H1C H 0.7178 0.4589 0.1132 0.064 Uiso 1 1 calc R . . C5 C 0.6453(3) 0.3757(3) 0.1265(2) 0.0422(13) Uani 1 1 d . . . Na2 Na 0.2500 0.2500 0.2500 0.0445(3) Uani 0.50 4 d SP . . 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 Co1 0.0223(4) 0.0224(4) 0.0136(4) 0.000 0.000 -0.0019(3) C11 0.026(2) 0.030(2) 0.020(2) 0.0015(18) 0.0010(17) -0.0046(19) B17 0.031(3) 0.028(3) 0.016(2) -0.001(2) -0.001(2) -0.004(2) B22 0.033(3) 0.032(3) 0.019(2) -0.001(2) -0.004(2) -0.006(2) B24 0.031(3) 0.033(3) 0.023(3) 0.000(2) 0.005(2) -0.008(2) B25 0.023(3) 0.033(3) 0.032(3) -0.002(2) -0.001(2) -0.004(2) C27 0.028(2) 0.028(2) 0.022(2) -0.0001(18) 0.0030(18) -0.0023(19) B29 0.033(3) 0.022(3) 0.017(2) -0.0005(19) 0.000(2) -0.001(2) B31 0.026(3) 0.034(3) 0.022(2) -0.001(2) -0.003(2) -0.005(2) B32 0.033(3) 0.029(3) 0.022(3) -0.003(2) 0.002(2) -0.006(2) B35 0.032(3) 0.029(3) 0.022(3) 0.004(2) 0.002(2) -0.007(2) B36 0.029(3) 0.030(3) 0.021(2) 0.001(2) -0.002(2) -0.003(2) La2 0.0363(4) 0.0363(4) 0.0609(8) 0.000 0.000 0.000 O3 0.0264(17) 0.0258(17) 0.0283(16) -0.0019(13) 0.0077(13) 0.0052(13) O1 0.0204(16) 0.0277(18) 0.050(2) -0.0035(15) -0.0074(14) -0.0001(13) O2 0.0387(19) 0.0185(16) 0.0355(18) 0.0087(13) 0.0081(14) 0.0074(14) C3 0.018(2) 0.020(2) 0.021(2) -0.0050(16) -0.0040(16) -0.0027(16) C4 0.029(2) 0.018(2) 0.018(2) -0.0005(17) -0.0013(17) -0.0013(18) O5 0.0270(18) 0.0301(18) 0.0431(19) 0.0020(15) -0.0020(15) -0.0057(14) C6 0.025(2) 0.026(2) 0.021(2) -0.0049(18) 0.0034(18) 0.0020(18) C7 0.020(2) 0.023(2) 0.023(2) -0.0110(17) 0.0033(17) 0.0018(17) C8 0.020(2) 0.017(2) 0.019(2) -0.0033(16) -0.0043(16) -0.0028(16) C9 0.023(2) 0.021(2) 0.017(2) 0.0019(16) 0.0003(16) -0.0027(17) C10 0.025(2) 0.016(2) 0.030(2) -0.0016(17) -0.0019(18) -0.0032(17) C12 0.028(2) 0.0098(19) 0.030(2) -0.0003(16) -0.0071(18) -0.0005(16) C13 0.023(2) 0.019(2) 0.019(2) -0.0001(16) -0.0004(16) -0.0060(17) C14 0.020(2) 0.026(2) 0.034(2) -0.0105(19) 0.0016(19) 0.0017(18) O15 0.051(2) 0.070(3) 0.033(2) -0.0185(19) -0.0173(18) 0.025(2) C16 0.026(2) 0.033(3) 0.033(3) -0.006(2) 0.011(2) -0.004(2) C18 0.023(2) 0.019(2) 0.029(2) -0.0111(18) 0.0000(18) 0.0049(17) C19 0.022(2) 0.025(2) 0.023(2) -0.0084(17) 0.0003(17) 0.0007(18) C20 0.029(2) 0.013(2) 0.035(3) -0.0023(18) -0.0050(19) -0.0001(18) C21 0.025(2) 0.024(2) 0.027(2) -0.0061(18) 0.0056(18) -0.0018(18) C23 0.024(2) 0.023(2) 0.036(3) -0.0053(19) -0.0030(19) 0.0083(18) C26 0.024(2) 0.018(2) 0.040(3) -0.0048(19) -0.006(2) 0.0066(18) O28 0.057(3) 0.046(2) 0.0259(18) -0.0032(16) -0.0002(16) 0.0122(18) C30 0.045(3) 0.024(2) 0.031(3) -0.0033(19) -0.004(2) 0.011(2) C33 0.046(3) 0.033(3) 0.029(3) -0.011(2) -0.010(2) 0.014(2) C37 0.031(3) 0.020(2) 0.032(2) -0.0004(18) -0.0026(19) 0.0015(19) C38 0.031(3) 0.024(2) 0.047(3) -0.006(2) -0.014(2) 0.007(2) C40 0.067(4) 0.029(3) 0.071(4) 0.027(3) 0.027(3) 0.013(3) C41 0.055(4) 0.040(3) 0.042(3) 0.013(2) -0.010(3) -0.014(3) C43 0.051(4) 0.107(6) 0.055(4) -0.046(4) -0.024(3) 0.038(4) C44 0.026(3) 0.028(3) 0.091(5) -0.001(3) -0.021(3) 0.002(2) C46 0.056(4) 0.049(3) 0.036(3) 0.001(2) 0.008(3) 0.007(3) O47 0.053(3) 0.052(3) 0.293(10) 0.056(5) 0.017(4) 0.022(3) O49 0.140(7) 0.213(9) 0.087(5) 0.057(5) -0.013(4) -0.074(6) O4 0.053(3) 0.044(2) 0.067(3) 0.001(2) 0.004(2) 0.0146(19) C2 0.022(2) 0.021(2) 0.020(2) -0.0053(16) 0.0004(17) -0.0020(17) N6 0.090(5) 0.046(4) 0.089(5) -0.011(3) -0.007(4) -0.008(3) C1 0.049(3) 0.044(3) 0.036(3) -0.013(2) 0.006(2) -0.002(3) C5 0.044(3) 0.033(3) 0.049(3) -0.016(3) -0.003(3) 0.002(2) Na2 0.0363(4) 0.0363(4) 0.0609(8) 0.000 0.000 0.000 _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 Co1 C11 2.044(4) 3_565 ? Co1 C11 2.044(4) . ? Co1 C27 2.046(4) 3_565 ? Co1 C27 2.046(4) . ? Co1 B29 2.089(5) 3_565 ? Co1 B29 2.089(5) . ? Co1 B36 2.091(5) . ? Co1 B36 2.091(5) 3_565 ? Co1 B17 2.117(5) . ? Co1 B17 2.117(5) 3_565 ? C11 C27 1.620(6) . ? C11 B29 1.695(7) . ? C11 B35 1.708(7) . ? C11 B24 1.723(7) . ? B17 B22 1.791(8) . ? B17 B36 1.794(8) . ? B17 B29 1.804(7) . ? B17 B32 1.818(7) . ? B22 B25 1.775(7) . ? B22 B36 1.782(7) . ? B22 B32 1.783(8) . ? B22 B31 1.797(7) . ? B24 C27 1.727(7) . ? B24 B25 1.756(8) . ? B24 B31 1.767(7) . ? B24 B35 1.770(8) . ? B25 C27 1.699(7) . ? B25 B31 1.764(8) . ? B25 B36 1.800(7) . ? C27 B36 1.713(7) . ? B29 B32 1.768(7) . ? B29 B35 1.783(7) . ? B31 B35 1.769(7) . ? B31 B32 1.781(8) . ? B32 B35 1.768(7) . ? La2 O47 2.408(5) 6_566 ? La2 O47 2.408(5) 3 ? La2 O47 2.408(5) . ? La2 O47 2.408(5) 8_656 ? La2 O49 2.549(6) 3 ? La2 O49 2.549(6) . ? La2 O49 2.549(6) 6_566 ? La2 O49 2.549(6) 8_656 ? O3 C2 1.372(5) . ? O3 C16 1.430(5) . ? O1 C14 1.370(5) . ? O1 C44 1.433(6) . ? O2 C4 1.366(5) . ? O2 C40 1.409(6) . ? C3 C8 1.387(6) . ? C3 C9 1.404(6) . ? C3 C19 1.523(6) . ? C4 C9 1.384(6) . ? C4 C2 1.395(6) . ? O5 C21 1.370(5) . ? O5 C41 1.420(6) . ? C6 C21 1.386(6) . ? C6 C7 1.405(6) . ? C7 C18 1.398(6) . ? C7 C19 1.521(6) . ? C8 C13 1.402(6) . ? C8 C10 1.520(6) . ? C10 C12 1.517(6) . ? C12 C20 1.399(6) . ? C12 C37 1.403(7) . ? C13 C2 1.383(6) . ? C14 C23 1.380(7) . ? C14 C21 1.407(7) . ? O15 C33 1.377(6) . ? O15 C43 1.414(7) . ? C18 C23 1.409(6) . ? C18 C26 1.514(6) . ? C20 C38 1.418(7) . ? C20 C26 1.531(7) . ? O28 C30 1.374(6) . ? O28 C46 1.431(7) . ? C30 C37 1.380(7) . ? C30 C33 1.395(7) . ? C33 C38 1.371(7) . ? N6 C5 1.141(8) . ? C1 C5 1.422(8) . ? 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 C11 Co1 C11 98.2(2) 3_565 . ? C11 Co1 C27 46.68(18) 3_565 3_565 ? C11 Co1 C27 99.64(18) . 3_565 ? C11 Co1 C27 99.64(18) 3_565 . ? C11 Co1 C27 46.68(18) . . ? C27 Co1 C27 133.3(2) 3_565 . ? C11 Co1 B29 48.42(18) 3_565 3_565 ? C11 Co1 B29 129.31(19) . 3_565 ? C27 Co1 B29 83.00(19) 3_565 3_565 ? C27 Co1 B29 95.95(19) . 3_565 ? C11 Co1 B29 129.31(19) 3_565 . ? C11 Co1 B29 48.42(18) . . ? C27 Co1 B29 95.95(19) 3_565 . ? C27 Co1 B29 83.00(19) . . ? B29 Co1 B29 177.4(3) 3_565 . ? C11 Co1 B36 132.5(2) 3_565 . ? C11 Co1 B36 83.55(19) . . ? C27 Co1 B36 176.8(2) 3_565 . ? C27 Co1 B36 48.90(19) . . ? B29 Co1 B36 94.5(2) 3_565 . ? B29 Co1 B36 86.6(2) . . ? C11 Co1 B36 83.55(19) 3_565 3_565 ? C11 Co1 B36 132.5(2) . 3_565 ? C27 Co1 B36 48.90(19) 3_565 3_565 ? C27 Co1 B36 176.8(2) . 3_565 ? B29 Co1 B36 86.6(2) 3_565 3_565 ? B29 Co1 B36 94.5(2) . 3_565 ? B36 Co1 B36 129.0(3) . 3_565 ? C11 Co1 B17 176.15(19) 3_565 . ? C11 Co1 B17 84.34(18) . . ? C27 Co1 B17 130.16(19) 3_565 . ? C27 Co1 B17 84.21(19) . . ? B29 Co1 B17 131.6(2) 3_565 . ? B29 Co1 B17 50.79(19) . . ? B36 Co1 B17 50.5(2) . . ? B36 Co1 B17 92.6(2) 3_565 . ? C11 Co1 B17 84.34(18) 3_565 3_565 ? C11 Co1 B17 176.15(19) . 3_565 ? C27 Co1 B17 84.21(19) 3_565 3_565 ? C27 Co1 B17 130.16(19) . 3_565 ? B29 Co1 B17 50.79(19) 3_565 3_565 ? B29 Co1 B17 131.6(2) . 3_565 ? B36 Co1 B17 92.6(2) . 3_565 ? B36 Co1 B17 50.5(2) 3_565 3_565 ? B17 Co1 B17 93.3(3) . 3_565 ? C27 C11 B29 111.4(3) . . ? C27 C11 B35 111.6(4) . . ? B29 C11 B35 63.2(3) . . ? C27 C11 B24 62.1(3) . . ? B29 C11 B24 114.7(4) . . ? B35 C11 B24 62.1(3) . . ? C27 C11 Co1 66.7(2) . . ? B29 C11 Co1 67.2(2) . . ? B35 C11 Co1 125.0(3) . . ? B24 C11 Co1 125.0(3) . . ? B22 B17 B36 59.6(3) . . ? B22 B17 B29 105.4(3) . . ? B36 B17 B29 105.6(3) . . ? B22 B17 B32 59.2(3) . . ? B36 B17 B32 106.2(4) . . ? B29 B17 B32 58.4(3) . . ? B22 B17 Co1 116.2(3) . . ? B36 B17 Co1 64.0(2) . . ? B29 B17 Co1 63.8(2) . . ? B32 B17 Co1 115.3(3) . . ? B25 B22 B36 60.8(3) . . ? B25 B22 B32 106.8(4) . . ? B36 B22 B32 108.2(4) . . ? B25 B22 B17 109.1(4) . . ? B36 B22 B17 60.2(3) . . ? B32 B22 B17 61.1(3) . . ? B25 B22 B31 59.2(3) . . ? B36 B22 B31 108.6(4) . . ? B32 B22 B31 59.7(3) . . ? B17 B22 B31 109.7(4) . . ? C11 B24 C27 56.0(3) . . ? C11 B24 B25 103.3(3) . . ? C27 B24 B25 58.4(3) . . ? C11 B24 B31 104.3(4) . . ? C27 B24 B31 104.5(3) . . ? B25 B24 B31 60.1(3) . . ? C11 B24 B35 58.5(3) . . ? C27 B24 B35 103.8(4) . . ? B25 B24 B35 107.5(4) . . ? B31 B24 B35 60.0(3) . . ? C27 B25 B24 59.9(3) . . ? C27 B25 B31 105.8(4) . . ? B24 B25 B31 60.3(3) . . ? C27 B25 B22 104.6(4) . . ? B24 B25 B22 109.3(4) . . ? B31 B25 B22 61.0(3) . . ? C27 B25 B36 58.5(3) . . ? B24 B25 B36 109.5(4) . . ? B31 B25 B36 109.3(4) . . ? B22 B25 B36 59.8(3) . . ? C11 C27 B25 110.5(4) . . ? C11 C27 B36 111.5(4) . . ? B25 C27 B36 63.7(3) . . ? C11 C27 B24 61.9(3) . . ? B25 C27 B24 61.7(3) . . ? B36 C27 B24 115.2(4) . . ? C11 C27 Co1 66.6(2) . . ? B25 C27 Co1 124.5(3) . . ? B36 C27 Co1 66.9(2) . . ? B24 C27 Co1 124.6(3) . . ? C11 B29 B32 104.6(4) . . ? C11 B29 B35 58.7(3) . . ? B32 B29 B35 59.7(3) . . ? C11 B29 B17 105.9(4) . . ? B32 B29 B17 61.2(3) . . ? B35 B29 B17 109.5(4) . . ? C11 B29 Co1 64.4(2) . . ? B32 B29 Co1 119.1(3) . . ? B35 B29 Co1 118.5(3) . . ? B17 B29 Co1 65.4(2) . . ? B25 B31 B24 59.7(3) . . ? B25 B31 B35 107.2(4) . . ? B24 B31 B35 60.1(3) . . ? B25 B31 B32 107.3(4) . . ? B24 B31 B32 107.9(4) . . ? B35 B31 B32 59.7(3) . . ? B25 B31 B22 59.8(3) . . ? B24 B31 B22 107.8(4) . . ? B35 B31 B22 107.4(4) . . ? B32 B31 B22 59.8(3) . . ? B29 B32 B35 60.6(3) . . ? B29 B32 B31 108.3(4) . . ? B35 B32 B31 59.8(3) . . ? B29 B32 B22 107.3(4) . . ? B35 B32 B22 108.1(4) . . ? B31 B32 B22 60.6(3) . . ? B29 B32 B17 60.4(3) . . ? B35 B32 B17 109.6(4) . . ? B31 B32 B17 109.2(4) . . ? B22 B32 B17 59.7(3) . . ? C11 B35 B32 104.1(3) . . ? C11 B35 B31 104.8(4) . . ? B32 B35 B31 60.5(3) . . ? C11 B35 B24 59.4(3) . . ? B32 B35 B24 108.4(4) . . ? B31 B35 B24 59.9(3) . . ? C11 B35 B29 58.1(3) . . ? B32 B35 B29 59.7(3) . . ? B31 B35 B29 108.1(4) . . ? B24 B35 B29 108.2(4) . . ? C27 B36 B22 103.7(4) . . ? C27 B36 B17 105.5(4) . . ? B22 B36 B17 60.1(3) . . ? C27 B36 B25 57.8(3) . . ? B22 B36 B25 59.4(3) . . ? B17 B36 B25 107.9(4) . . ? C27 B36 Co1 64.2(2) . . ? B22 B36 Co1 117.9(3) . . ? B17 B36 Co1 65.5(2) . . ? B25 B36 Co1 116.9(3) . . ? O47 La2 O47 92.36(9) 6_566 3 ? O47 La2 O47 92.36(9) 6_566 . ? O47 La2 O47 156.6(5) 3 . ? O47 La2 O47 156.6(5) 6_566 8_656 ? O47 La2 O47 92.36(9) 3 8_656 ? O47 La2 O47 92.36(9) . 8_656 ? O47 La2 O49 65.8(3) 6_566 3 ? O47 La2 O49 72.6(3) 3 3 ? O47 La2 O49 88.6(3) . 3 ? O47 La2 O49 137.3(3) 8_656 3 ? O47 La2 O49 137.3(3) 6_566 . ? O47 La2 O49 88.6(3) 3 . ? O47 La2 O49 72.6(3) . . ? O47 La2 O49 65.8(3) 8_656 . ? O49 La2 O49 73.9(4) 3 . ? O47 La2 O49 72.6(3) 6_566 6_566 ? O47 La2 O49 137.3(3) 3 6_566 ? O47 La2 O49 65.8(3) . 6_566 ? O47 La2 O49 88.6(3) 8_656 6_566 ? O49 La2 O49 129.7(2) 3 6_566 ? O49 La2 O49 129.7(2) . 6_566 ? O47 La2 O49 88.6(3) 6_566 8_656 ? O47 La2 O49 65.8(3) 3 8_656 ? O47 La2 O49 137.3(3) . 8_656 ? O47 La2 O49 72.6(3) 8_656 8_656 ? O49 La2 O49 129.7(2) 3 8_656 ? O49 La2 O49 129.7(2) . 8_656 ? O49 La2 O49 73.9(4) 6_566 8_656 ? C2 O3 C16 116.5(3) . . ? C14 O1 C44 116.6(4) . . ? C4 O2 C40 116.6(4) . . ? C8 C3 C9 119.0(4) . . ? C8 C3 C19 123.5(4) . . ? C9 C3 C19 117.6(4) . . ? O2 C4 C9 125.3(4) . . ? O2 C4 C2 115.0(4) . . ? C9 C4 C2 119.7(4) . . ? C21 O5 C41 117.1(4) . . ? C21 C6 C7 122.0(4) . . ? C18 C7 C6 119.2(4) . . ? C18 C7 C19 123.9(4) . . ? C6 C7 C19 116.9(4) . . ? C3 C8 C13 119.5(4) . . ? C3 C8 C10 123.4(4) . . ? C13 C8 C10 117.0(4) . . ? C4 C9 C3 121.2(4) . . ? C12 C10 C8 113.1(3) . . ? C20 C12 C37 119.2(4) . . ? C20 C12 C10 123.5(4) . . ? C37 C12 C10 117.3(4) . . ? C2 C13 C8 121.2(4) . . ? O1 C14 C23 125.8(4) . . ? O1 C14 C21 115.0(4) . . ? C23 C14 C21 119.2(4) . . ? C33 O15 C43 117.6(5) . . ? C7 C18 C23 118.2(4) . . ? C7 C18 C26 123.6(4) . . ? C23 C18 C26 118.2(4) . . ? C7 C19 C3 114.9(3) . . ? C12 C20 C38 117.4(4) . . ? C12 C20 C26 123.8(4) . . ? C38 C20 C26 118.7(4) . . ? O5 C21 C6 125.4(4) . . ? O5 C21 C14 115.8(4) . . ? C6 C21 C14 118.9(4) . . ? C14 C23 C18 122.4(4) . . ? C18 C26 C20 115.2(3) . . ? C30 O28 C46 117.3(4) . . ? O28 C30 C37 125.3(5) . . ? O28 C30 C33 115.8(4) . . ? C37 C30 C33 118.9(5) . . ? C38 C33 O15 125.9(5) . . ? C38 C33 C30 119.5(4) . . ? O15 C33 C30 114.5(5) . . ? C30 C37 C12 122.2(4) . . ? C33 C38 C20 122.7(5) . . ? O3 C2 C13 125.5(4) . . ? O3 C2 C4 115.2(4) . . ? C13 C2 C4 119.4(4) . . ? N6 C5 C1 178.9(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.467 _refine_diff_density_min -2.802 _refine_diff_density_rms 0.106 #===END data_c3: _database_code_CSD 166362 _audit_creation_method SHELXL-97 _chemical_name_systematic ; octaaquoyttrium/sodium tetra(cyclotriveratrylene)tetrahydrate [cobalt(III)bis(dicarbollide)] acetonitrile clathrate ; _chemical_name_common '[Y0.5Na0.5(H2O)8](H2O)4[(CH3CN)(CTV)][Co(C2B9H11)2]2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H50 B9 Co0.50 N Na0.125 O9 Y0.125' _chemical_formula_weight 721.46 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' 'B' 'B' 0.0013 0.0007 '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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Y' 'Y' -2.7962 3.5667 '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' '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 P4(2)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x+1/2, z+1/2' '-x+1/2, -y+1/2, z' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'y, -x-1/2, -z-1/2' 'x-1/2, y-1/2, -z' '-y-1/2, x, -z-1/2' _cell_length_a 17.6918(3) _cell_length_b 17.6918(3) _cell_length_c 23.7339(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7428.7(2) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3038 _exptl_absorpt_coefficient_mu 0.492 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 71696 _diffrn_reflns_av_R_equivalents 0.106 _diffrn_reflns_av_sigmaI/netI 0.0682 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8139 _reflns_number_gt 5624 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0800P)^2^+25.0935P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8139 _refine_ls_number_parameters 467 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1335 _refine_ls_R_factor_gt 0.0885 _refine_ls_wR_factor_ref 0.2135 _refine_ls_wR_factor_gt 0.1906 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.2500 0.7500 0.03384(3) 0.01695(19) Uani 1 2 d S . . Y2 Y 0.2500 0.2500 0.7500 0.0651(6) Uani 0.50 4 d SP . 1 O1 O 0.44292(14) 0.55983(14) 0.34276(12) 0.0225(6) Uani 1 1 d . . . O2 O 0.36303(16) 0.63329(15) 0.27139(12) 0.0262(7) Uani 1 1 d . . . O3 O -0.10695(16) 0.53439(16) 0.33588(13) 0.0303(7) Uani 1 1 d . . . O4 O -0.03188(17) 0.61378(17) 0.26391(13) 0.0310(7) Uani 1 1 d . . . C5 C 0.3782(2) 0.5243(2) 0.32544(16) 0.0179(8) Uani 1 1 d . . . C6 C 0.2466(2) 0.4593(2) 0.28116(16) 0.0172(8) Uani 1 1 d . . . C7 C 0.0703(2) 0.5208(2) 0.26064(17) 0.0222(8) Uani 1 1 d . . . H7 H 0.0970 0.5491 0.2331 0.027 Uiso 1 1 calc R . . C8 C 0.2889(2) 0.4205(2) 0.32135(16) 0.0177(8) Uani 1 1 d . . . C9 C 0.2708(2) 0.5311(2) 0.26399(16) 0.0186(8) Uani 1 1 d . . . H9 H 0.2421 0.5579 0.2367 0.022 Uiso 1 1 calc R . . C10 C 0.3350(2) 0.5638(2) 0.28570(16) 0.0185(8) Uani 1 1 d . . . C11 C 0.2667(2) 0.3428(2) 0.34387(18) 0.0211(8) Uani 1 1 d . . . H11A H 0.2370 0.3159 0.3148 0.025 Uiso 1 1 calc R . . H11B H 0.3131 0.3131 0.3511 0.025 Uiso 1 1 calc R . . C12 C -0.0072(2) 0.4383(2) 0.34033(19) 0.0256(9) Uani 1 1 d . . . H12 H -0.0341 0.4100 0.3678 0.031 Uiso 1 1 calc R . . C13 C 0.0926(2) 0.3380(2) 0.34635(19) 0.0257(9) Uani 1 1 d . . . H13A H 0.1225 0.3112 0.3173 0.031 Uiso 1 1 calc R . . H13B H 0.0490 0.3054 0.3561 0.031 Uiso 1 1 calc R . . C14 C 0.2449(2) 0.6442(2) -0.00008(17) 0.0216(8) Uani 1 1 d . . . H14 H 0.2983 0.6355 -0.0246 0.026 Uiso 1 1 calc R . . C15 C 0.3545(2) 0.4537(2) 0.34293(16) 0.0190(8) Uani 1 1 d . . . H15 H 0.3835 0.4271 0.3702 0.023 Uiso 1 1 calc R . . O16 O 0.2604(2) 0.3558(2) 0.55179(14) 0.0438(9) Uani 1 1 d . . . O17 O 0.1160(2) 0.3611(2) 0.55466(15) 0.0511(10) Uani 1 1 d . . . C18 C 0.1759(2) 0.4275(2) 0.25343(17) 0.0214(8) Uani 1 1 d . . . H18A H 0.1785 0.3716 0.2547 0.026 Uiso 1 1 calc R . . H18B H 0.1757 0.4427 0.2133 0.026 Uiso 1 1 calc R . . C19 C 0.4870(2) 0.5219(2) 0.38419(18) 0.0268(9) Uani 1 1 d . . . H19A H 0.5317 0.5524 0.3931 0.040 Uiso 1 1 calc R . . H19B H 0.5029 0.4726 0.3696 0.040 Uiso 1 1 calc R . . H19C H 0.4568 0.5148 0.4184 0.040 Uiso 1 1 calc R . . C20 C -0.0382(2) 0.5051(2) 0.32042(18) 0.0242(9) Uani 1 1 d . . . C21 C 0.1012(2) 0.4525(2) 0.28012(17) 0.0208(8) Uani 1 1 d . . . C22 C 0.2207(2) 0.3470(2) 0.39761(18) 0.0228(9) Uani 1 1 d . . . C24 C 0.2253(3) 0.3554(2) 0.50031(19) 0.0326(11) Uani 1 1 d . . . B25 B 0.1645(3) 0.6037(3) -0.0285(2) 0.0257(10) Uani 1 1 d . . . H25 H 0.1618 0.5717 -0.0692 0.031 Uiso 1 1 calc R . . C26 C 0.1786(2) 0.6994(2) -0.02232(16) 0.0216(9) Uani 1 1 d . . . H26 H 0.1841 0.7308 -0.0631 0.026 Uiso 1 1 calc R . . C27 C 0.0629(2) 0.4112(2) 0.32117(18) 0.0240(9) Uani 1 1 d . . . C28 C 0.1459(3) 0.3581(3) 0.5015(2) 0.0345(11) Uani 1 1 d . . . C29 C 0.1417(2) 0.3474(2) 0.39874(19) 0.0262(9) Uani 1 1 d . . . C30 C 0.0019(2) 0.5479(2) 0.28051(17) 0.0231(9) Uani 1 1 d . . . C31 C 0.2609(2) 0.3511(2) 0.44868(18) 0.0258(9) Uani 1 1 d . . . H31 H 0.3146 0.3510 0.4476 0.031 Uiso 1 1 calc R . . B32 B 0.1617(3) 0.6040(3) 0.0925(2) 0.0252(10) Uani 1 1 d . . . H32 H 0.1561 0.5706 0.1323 0.030 Uiso 1 1 calc R . . B33 B 0.2079(3) 0.5669(3) 0.0324(2) 0.0255(10) Uani 1 1 d . . . H33 H 0.2339 0.5092 0.0319 0.031 Uiso 1 1 calc R . . B34 B 0.1752(3) 0.7045(3) 0.09472(19) 0.0215(9) Uani 1 1 d . . . H34 H 0.1763 0.7353 0.1359 0.026 Uiso 1 1 calc R . . B35 B 0.1323(2) 0.7414(3) 0.03196(19) 0.0209(9) Uani 1 1 d . . . H35 H 0.1054 0.7987 0.0308 0.025 Uiso 1 1 calc R . . C36 C 0.1063(3) 0.3537(2) 0.4516(2) 0.0321(11) Uani 1 1 d . . . H36 H 0.0527 0.3549 0.4530 0.039 Uiso 1 1 calc R . . B37 B 0.1092(3) 0.5800(3) 0.0308(2) 0.0254(10) Uani 1 1 d . . . H37 H 0.0690 0.5311 0.0302 0.031 Uiso 1 1 calc R . . B38 B 0.0912(3) 0.6645(3) -0.0065(2) 0.0244(10) Uani 1 1 d . . . H38 H 0.0393 0.6722 -0.0328 0.029 Uiso 1 1 calc R . . B39 B 0.0884(3) 0.6653(3) 0.0678(2) 0.0253(10) Uani 1 1 d . . . H39 H 0.0339 0.6729 0.0911 0.030 Uiso 1 1 calc R . . B40 B 0.2504(3) 0.6433(3) 0.0716(2) 0.0234(10) Uani 1 1 d . . . H40 H 0.3030 0.6339 0.0970 0.028 Uiso 1 1 calc R . . C41 C -0.1512(3) 0.4908(3) 0.3740(2) 0.0434(13) Uani 1 1 d . . . H41A H -0.1986 0.5174 0.3819 0.065 Uiso 1 1 calc R . . H41B H -0.1231 0.4836 0.4092 0.065 Uiso 1 1 calc R . . H41C H -0.1624 0.4415 0.3571 0.065 Uiso 1 1 calc R . . C43 C 0.3177(3) 0.6772(3) 0.2354(3) 0.0507(15) Uani 1 1 d . . . H43A H 0.3432 0.7252 0.2275 0.076 Uiso 1 1 calc R . . H43B H 0.2690 0.6872 0.2536 0.076 Uiso 1 1 calc R . . H43C H 0.3093 0.6498 0.2000 0.076 Uiso 1 1 calc R . . C45 C 0.0069(3) 0.6585(3) 0.2229(2) 0.0451(13) Uani 1 1 d . . . H45A H -0.0226 0.7041 0.2149 0.068 Uiso 1 1 calc R . . H45B H 0.0133 0.6292 0.1883 0.068 Uiso 1 1 calc R . . H45C H 0.0566 0.6729 0.2376 0.068 Uiso 1 1 calc R . . C47 C 0.0361(3) 0.3649(4) 0.5594(3) 0.073(2) Uani 1 1 d . . . H47A H 0.0219 0.3664 0.5993 0.109 Uiso 1 1 calc R . . H47B H 0.0135 0.3204 0.5416 0.109 Uiso 1 1 calc R . . H47C H 0.0177 0.4107 0.5407 0.109 Uiso 1 1 calc R . . O48 O 0.1876(3) 0.3663(3) 0.7703(3) 0.117(3) Uani 1 1 d . . . C49 C 0.3405(3) 0.3526(3) 0.5522(2) 0.0476(13) Uani 1 1 d . . . H49A H 0.3587 0.3531 0.5912 0.071 Uiso 1 1 calc R . . H49B H 0.3609 0.3965 0.5320 0.071 Uiso 1 1 calc R . . H49C H 0.3573 0.3061 0.5336 0.071 Uiso 1 1 calc R . . O50 O 0.1945(4) 0.3150(4) 0.6637(2) 0.120(2) Uani 1 1 d . . . C42 C 0.5523(3) 0.3336(3) 0.1028(2) 0.0373(11) Uani 1 1 d . . . H42A H 0.5138 0.3695 0.1155 0.056 Uiso 1 1 calc R . . H42B H 0.5387 0.2826 0.1153 0.056 Uiso 1 1 calc R . . H42C H 0.5552 0.3347 0.0615 0.056 Uiso 1 1 calc R . . N44 N 0.6816(3) 0.3715(3) 0.1436(2) 0.0682(15) Uani 1 1 d . . . C46 C 0.6243(3) 0.3542(3) 0.1261(2) 0.0378(11) Uani 1 1 d . . . O5 O 0.2102(2) 0.4967(2) 0.82793(17) 0.0495(10) Uani 1 1 d . . . H8 H 0.250(3) 0.537(3) 0.833(2) 0.058(17) Uiso 1 1 d . . . H1 H 0.170(4) 0.521(4) 0.823(3) 0.08(2) Uiso 1 1 d . . . Na2 Na 0.2500 0.2500 0.7500 0.0651(6) Uani 0.50 4 d SP . 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 Co1 0.0169(4) 0.0192(4) 0.0148(4) 0.000 0.000 -0.0024(3) Y2 0.0365(6) 0.0365(6) 0.1223(19) 0.000 0.000 0.000 O1 0.0185(14) 0.0181(14) 0.0308(16) 0.0002(11) -0.0071(12) -0.0020(11) O2 0.0272(15) 0.0169(14) 0.0344(18) 0.0084(12) -0.0063(12) -0.0050(11) O3 0.0206(15) 0.0265(16) 0.0438(19) -0.0043(13) 0.0065(13) 0.0001(12) O4 0.0267(16) 0.0304(17) 0.0361(18) 0.0036(13) 0.0004(13) 0.0053(13) C5 0.0194(19) 0.0168(18) 0.018(2) -0.0051(15) 0.0002(15) 0.0018(15) C6 0.0152(18) 0.0165(18) 0.020(2) -0.0073(15) 0.0059(15) 0.0009(14) C7 0.021(2) 0.025(2) 0.021(2) -0.0055(17) -0.0008(16) -0.0049(16) C8 0.0185(19) 0.0135(18) 0.021(2) -0.0029(15) 0.0050(15) 0.0032(14) C9 0.0191(19) 0.0197(19) 0.017(2) 0.0019(15) -0.0025(15) 0.0027(15) C10 0.0221(19) 0.0109(17) 0.023(2) 0.0002(15) 0.0029(16) -0.0002(14) C11 0.0197(19) 0.0122(18) 0.031(2) -0.0003(16) 0.0047(16) 0.0005(14) C12 0.021(2) 0.020(2) 0.035(3) -0.0057(18) 0.0046(18) -0.0080(16) C13 0.024(2) 0.0145(19) 0.039(3) -0.0068(17) 0.0067(18) -0.0033(16) C14 0.022(2) 0.020(2) 0.023(2) -0.0011(16) 0.0012(16) -0.0030(16) C15 0.0215(19) 0.0152(18) 0.020(2) -0.0006(15) 0.0012(16) 0.0066(14) O16 0.051(2) 0.050(2) 0.0297(19) -0.0058(16) 0.0016(16) -0.0148(17) O17 0.050(2) 0.065(3) 0.039(2) -0.0193(18) 0.0187(17) -0.0230(19) C18 0.0192(19) 0.021(2) 0.024(2) -0.0056(16) 0.0003(16) -0.0036(15) C19 0.023(2) 0.024(2) 0.034(3) -0.0028(18) -0.0114(18) 0.0051(16) C20 0.0174(19) 0.023(2) 0.033(2) -0.0087(17) -0.0003(17) -0.0030(15) C21 0.0180(19) 0.0220(19) 0.022(2) -0.0103(16) -0.0017(16) -0.0041(15) C22 0.030(2) 0.0088(17) 0.029(2) 0.0003(15) 0.0067(18) -0.0007(15) C24 0.040(3) 0.024(2) 0.034(3) -0.0050(19) 0.006(2) -0.0143(19) B25 0.028(2) 0.024(2) 0.025(3) -0.002(2) 0.001(2) -0.0088(19) C26 0.021(2) 0.026(2) 0.017(2) 0.0000(16) -0.0016(15) -0.0074(16) C27 0.022(2) 0.0175(19) 0.032(2) -0.0065(17) 0.0001(17) -0.0079(16) C28 0.041(3) 0.028(2) 0.035(3) -0.013(2) 0.015(2) -0.017(2) C29 0.028(2) 0.0096(18) 0.041(3) -0.0031(17) 0.0088(19) -0.0044(15) C30 0.024(2) 0.023(2) 0.023(2) -0.0058(17) -0.0061(17) -0.0023(16) C31 0.029(2) 0.0142(19) 0.034(3) -0.0017(17) 0.0045(18) -0.0056(16) B32 0.025(2) 0.028(2) 0.022(3) 0.0043(19) 0.0002(19) -0.0039(19) B33 0.026(2) 0.019(2) 0.031(3) 0.001(2) 0.001(2) -0.0045(18) B34 0.021(2) 0.026(2) 0.018(2) 0.0024(18) 0.0015(18) -0.0049(18) B35 0.020(2) 0.023(2) 0.020(2) -0.0025(19) 0.0010(18) -0.0034(17) C36 0.027(2) 0.023(2) 0.046(3) -0.0072(19) 0.014(2) -0.0094(17) B37 0.024(2) 0.028(2) 0.024(3) -0.002(2) 0.003(2) -0.0091(18) B38 0.020(2) 0.025(2) 0.028(3) 0.000(2) -0.0023(19) -0.0078(18) B39 0.021(2) 0.030(3) 0.025(3) 0.000(2) 0.0033(19) -0.0034(19) B40 0.025(2) 0.024(2) 0.021(3) 0.0019(19) -0.0017(19) -0.0026(18) C41 0.025(2) 0.030(3) 0.075(4) 0.001(2) 0.019(2) -0.0051(19) C43 0.060(3) 0.028(3) 0.064(4) 0.028(2) -0.025(3) -0.013(2) C45 0.054(3) 0.042(3) 0.039(3) 0.014(2) 0.010(2) 0.013(2) C47 0.046(3) 0.110(6) 0.063(4) -0.052(4) 0.027(3) -0.041(4) O48 0.066(3) 0.045(3) 0.242(7) -0.045(4) -0.071(4) 0.023(2) C49 0.050(3) 0.053(3) 0.040(3) -0.002(2) -0.007(2) -0.014(3) O50 0.109(5) 0.159(6) 0.092(4) 0.055(4) 0.022(4) 0.047(4) C42 0.033(3) 0.045(3) 0.034(3) -0.009(2) 0.015(2) -0.003(2) N44 0.039(3) 0.084(4) 0.082(4) 0.006(3) 0.006(3) -0.009(3) C46 0.034(3) 0.037(3) 0.043(3) 0.002(2) 0.013(2) 0.005(2) O5 0.031(2) 0.049(2) 0.069(3) -0.0059(19) -0.0021(18) 0.0114(18) Na2 0.0365(6) 0.0365(6) 0.1223(19) 0.000 0.000 0.000 _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 Co1 C14 2.040(4) . ? Co1 C14 2.040(4) 3_565 ? Co1 C26 2.043(4) 3_565 ? Co1 C26 2.043(4) . ? Co1 B35 2.088(4) 3_565 ? Co1 B35 2.088(4) . ? Co1 B40 2.089(5) 3_565 ? Co1 B40 2.089(5) . ? Co1 B34 2.119(4) 3_565 ? Co1 B34 2.119(4) . ? Y2 O48 2.384(4) 6_567 ? Y2 O48 2.384(4) 8_657 ? Y2 O48 2.384(4) 3 ? Y2 O48 2.384(4) . ? Y2 O50 2.547(5) 3 ? Y2 O50 2.547(5) 6_567 ? Y2 O50 2.547(5) . ? Y2 O50 2.547(5) 8_657 ? O1 C5 1.369(4) . ? O1 C19 1.423(5) . ? O2 C10 1.368(4) . ? O2 C43 1.406(5) . ? O3 C20 1.373(5) . ? O3 C41 1.424(5) . ? O4 C30 1.368(5) . ? O4 C45 1.429(6) . ? C5 C15 1.381(5) . ? C5 C10 1.401(5) . ? C6 C8 1.393(5) . ? C6 C9 1.401(5) . ? C6 C18 1.521(5) . ? C7 C30 1.384(6) . ? C7 C21 1.404(6) . ? C8 C15 1.399(5) . ? C8 C11 1.525(5) . ? C9 C10 1.376(5) . ? C11 C22 1.515(6) . ? C12 C20 1.385(6) . ? C12 C27 1.405(6) . ? C13 C27 1.520(6) . ? C13 C29 1.525(6) . ? C14 C26 1.616(6) . ? C14 B33 1.700(6) . ? C14 B40 1.704(6) . ? C14 B25 1.731(6) . ? O16 C24 1.371(6) . ? O16 C49 1.418(6) . ? O17 C28 1.370(6) . ? O17 C47 1.420(7) . ? C18 C21 1.530(5) . ? C20 C30 1.404(6) . ? C21 C27 1.394(6) . ? C22 C29 1.399(6) . ? C22 C31 1.407(6) . ? C24 C31 1.379(6) . ? C24 C28 1.406(7) . ? B25 C26 1.718(6) . ? B25 B33 1.762(7) . ? B25 B38 1.763(7) . ? B25 B37 1.765(7) . ? C26 B35 1.698(6) . ? C26 B38 1.706(6) . ? C28 C36 1.377(7) . ? C29 C36 1.407(6) . ? B32 B33 1.770(7) . ? B32 B37 1.785(7) . ? B32 B40 1.787(7) . ? B32 B39 1.789(7) . ? B32 B34 1.793(7) . ? B33 B37 1.762(7) . ? B33 B40 1.805(7) . ? B34 B35 1.795(6) . ? B34 B40 1.801(7) . ? B34 B39 1.802(6) . ? B35 B39 1.773(6) . ? B35 B38 1.792(6) . ? B37 B38 1.766(7) . ? B37 B39 1.784(7) . ? B38 B39 1.764(7) . ? C42 C46 1.436(7) . ? N44 C46 1.137(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 Co1 C14 133.5(2) . 3_565 ? C14 Co1 C26 99.89(16) . 3_565 ? C14 Co1 C26 46.63(16) 3_565 3_565 ? C14 Co1 C26 46.63(16) . . ? C14 Co1 C26 99.89(16) 3_565 . ? C26 Co1 C26 98.5(2) 3_565 . ? C14 Co1 B35 95.85(17) . 3_565 ? C14 Co1 B35 83.18(16) 3_565 3_565 ? C26 Co1 B35 48.52(17) 3_565 3_565 ? C26 Co1 B35 129.38(17) . 3_565 ? C14 Co1 B35 83.18(16) . . ? C14 Co1 B35 95.85(17) 3_565 . ? C26 Co1 B35 129.38(17) 3_565 . ? C26 Co1 B35 48.52(17) . . ? B35 Co1 B35 177.6(3) 3_565 . ? C14 Co1 B40 176.54(18) . 3_565 ? C14 Co1 B40 48.72(17) 3_565 3_565 ? C26 Co1 B40 83.47(17) 3_565 3_565 ? C26 Co1 B40 132.32(17) . 3_565 ? B35 Co1 B40 86.98(18) 3_565 3_565 ? B35 Co1 B40 94.07(18) . 3_565 ? C14 Co1 B40 48.72(17) . . ? C14 Co1 B40 176.54(18) 3_565 . ? C26 Co1 B40 132.32(17) 3_565 . ? C26 Co1 B40 83.47(17) . . ? B35 Co1 B40 94.07(18) 3_565 . ? B35 Co1 B40 86.98(18) . . ? B40 Co1 B40 129.2(3) 3_565 . ? C14 Co1 B34 130.21(17) . 3_565 ? C14 Co1 B34 83.84(17) 3_565 3_565 ? C26 Co1 B34 83.81(16) 3_565 3_565 ? C26 Co1 B34 176.26(18) . 3_565 ? B35 Co1 B34 50.52(18) 3_565 3_565 ? B35 Co1 B34 131.67(18) . 3_565 ? B40 Co1 B34 50.67(18) 3_565 3_565 ? B40 Co1 B34 92.79(18) . 3_565 ? C14 Co1 B34 83.84(17) . . ? C14 Co1 B34 130.21(17) 3_565 . ? C26 Co1 B34 176.26(17) 3_565 . ? C26 Co1 B34 83.81(16) . . ? B35 Co1 B34 131.67(18) 3_565 . ? B35 Co1 B34 50.52(18) . . ? B40 Co1 B34 92.79(18) 3_565 . ? B40 Co1 B34 50.67(18) . . ? B34 Co1 B34 94.0(3) 3_565 . ? O48 Y2 O48 156.6(4) 6_567 8_657 ? O48 Y2 O48 92.35(7) 6_567 3 ? O48 Y2 O48 92.35(7) 8_657 3 ? O48 Y2 O48 92.35(7) 6_567 . ? O48 Y2 O48 92.35(7) 8_657 . ? O48 Y2 O48 156.6(4) 3 . ? O48 Y2 O50 73.4(2) 6_567 3 ? O48 Y2 O50 87.7(2) 8_657 3 ? O48 Y2 O50 66.1(2) 3 3 ? O48 Y2 O50 137.0(2) . 3 ? O48 Y2 O50 66.1(2) 6_567 6_567 ? O48 Y2 O50 137.0(2) 8_657 6_567 ? O48 Y2 O50 87.7(2) 3 6_567 ? O48 Y2 O50 73.4(2) . 6_567 ? O50 Y2 O50 130.33(18) 3 6_567 ? O48 Y2 O50 87.7(2) 6_567 . ? O48 Y2 O50 73.4(2) 8_657 . ? O48 Y2 O50 137.0(2) 3 . ? O48 Y2 O50 66.1(2) . . ? O50 Y2 O50 72.9(3) 3 . ? O50 Y2 O50 130.33(18) 6_567 . ? O48 Y2 O50 137.0(2) 6_567 8_657 ? O48 Y2 O50 66.1(2) 8_657 8_657 ? O48 Y2 O50 73.4(2) 3 8_657 ? O48 Y2 O50 87.7(2) . 8_657 ? O50 Y2 O50 130.33(18) 3 8_657 ? O50 Y2 O50 72.9(3) 6_567 8_657 ? O50 Y2 O50 130.33(18) . 8_657 ? C5 O1 C19 116.7(3) . . ? C10 O2 C43 116.2(3) . . ? C20 O3 C41 116.9(3) . . ? C30 O4 C45 117.3(3) . . ? O1 C5 C15 125.4(3) . . ? O1 C5 C10 115.4(3) . . ? C15 C5 C10 119.2(3) . . ? C8 C6 C9 118.8(3) . . ? C8 C6 C18 123.7(3) . . ? C9 C6 C18 117.5(3) . . ? C30 C7 C21 121.8(4) . . ? C6 C8 C15 119.3(3) . . ? C6 C8 C11 123.1(3) . . ? C15 C8 C11 117.6(3) . . ? C10 C9 C6 121.7(3) . . ? O2 C10 C9 125.7(3) . . ? O2 C10 C5 114.7(3) . . ? C9 C10 C5 119.5(3) . . ? C22 C11 C8 112.9(3) . . ? C20 C12 C27 122.0(4) . . ? C27 C13 C29 115.1(3) . . ? C26 C14 B33 110.8(3) . . ? C26 C14 B40 111.9(3) . . ? B33 C14 B40 64.1(3) . . ? C26 C14 B25 61.7(3) . . ? B33 C14 B25 61.8(3) . . ? B40 C14 B25 115.7(3) . . ? C26 C14 Co1 66.77(19) . . ? B33 C14 Co1 125.2(3) . . ? B40 C14 Co1 67.1(2) . . ? B25 C14 Co1 124.7(3) . . ? C5 C15 C8 121.4(4) . . ? C24 O16 C49 117.3(4) . . ? C28 O17 C47 117.4(4) . . ? C6 C18 C21 115.0(3) . . ? O3 C20 C12 125.6(4) . . ? O3 C20 C30 115.0(4) . . ? C12 C20 C30 119.4(4) . . ? C27 C21 C7 119.4(4) . . ? C27 C21 C18 123.8(4) . . ? C7 C21 C18 116.7(4) . . ? C29 C22 C31 119.2(4) . . ? C29 C22 C11 123.6(4) . . ? C31 C22 C11 117.2(4) . . ? O16 C24 C31 125.8(4) . . ? O16 C24 C28 115.8(4) . . ? C31 C24 C28 118.4(4) . . ? C26 B25 C14 55.9(2) . . ? C26 B25 B33 103.3(3) . . ? C14 B25 B33 58.2(2) . . ? C26 B25 B38 58.7(2) . . ? C14 B25 B38 103.6(3) . . ? B33 B25 B38 107.6(3) . . ? C26 B25 B37 104.2(3) . . ? C14 B25 B37 104.0(3) . . ? B33 B25 B37 59.9(3) . . ? B38 B25 B37 60.1(3) . . ? C14 C26 B35 111.6(3) . . ? C14 C26 B38 111.5(3) . . ? B35 C26 B38 63.5(3) . . ? C14 C26 B25 62.5(3) . . ? B35 C26 B25 115.2(3) . . ? B38 C26 B25 62.0(3) . . ? C14 C26 Co1 66.60(19) . . ? B35 C26 Co1 67.1(2) . . ? B38 C26 Co1 125.1(3) . . ? B25 C26 Co1 125.3(3) . . ? C21 C27 C12 118.4(4) . . ? C21 C27 C13 123.6(4) . . ? C12 C27 C13 118.0(4) . . ? O17 C28 C36 126.7(4) . . ? O17 C28 C24 113.9(4) . . ? C36 C28 C24 119.3(4) . . ? C22 C29 C36 117.5(4) . . ? C22 C29 C13 123.5(4) . . ? C36 C29 C13 118.9(4) . . ? O4 C30 C7 125.3(4) . . ? O4 C30 C20 115.7(4) . . ? C7 C30 C20 118.9(4) . . ? C24 C31 C22 122.5(4) . . ? B33 B32 B37 59.4(3) . . ? B33 B32 B40 61.0(3) . . ? B37 B32 B40 108.8(3) . . ? B33 B32 B39 107.2(3) . . ? B37 B32 B39 59.9(3) . . ? B40 B32 B39 108.1(3) . . ? B33 B32 B34 109.2(3) . . ? B37 B32 B34 109.2(3) . . ? B40 B32 B34 60.4(3) . . ? B39 B32 B34 60.4(3) . . ? C14 B33 B37 105.5(3) . . ? C14 B33 B25 60.0(3) . . ? B37 B33 B25 60.1(3) . . ? C14 B33 B32 104.2(3) . . ? B37 B33 B32 60.7(3) . . ? B25 B33 B32 108.8(3) . . ? C14 B33 B40 58.1(2) . . ? B37 B33 B40 109.0(3) . . ? B25 B33 B40 109.2(3) . . ? B32 B33 B40 60.0(3) . . ? B32 B34 B35 106.3(3) . . ? B32 B34 B40 59.6(3) . . ? B35 B34 B40 106.2(3) . . ? B32 B34 B39 59.7(3) . . ? B35 B34 B39 59.0(3) . . ? B40 B34 B39 106.9(3) . . ? B32 B34 Co1 116.1(3) . . ? B35 B34 Co1 63.9(2) . . ? B40 B34 Co1 63.8(2) . . ? B39 B34 Co1 115.9(3) . . ? C26 B35 B39 104.0(3) . . ? C26 B35 B38 58.5(2) . . ? B39 B35 B38 59.3(3) . . ? C26 B35 B34 105.4(3) . . ? B39 B35 B34 60.7(3) . . ? B38 B35 B34 108.5(3) . . ? C26 B35 Co1 64.34(19) . . ? B39 B35 Co1 118.8(3) . . ? B38 B35 Co1 118.0(3) . . ? B34 B35 Co1 65.6(2) . . ? C28 C36 C29 123.0(4) . . ? B33 B37 B25 60.0(3) . . ? B33 B37 B38 107.5(3) . . ? B25 B37 B38 59.9(3) . . ? B33 B37 B39 107.8(3) . . ? B25 B37 B39 107.8(3) . . ? B38 B37 B39 59.6(3) . . ? B33 B37 B32 59.9(3) . . ? B25 B37 B32 108.1(3) . . ? B38 B37 B32 107.6(3) . . ? B39 B37 B32 60.2(3) . . ? C26 B38 B25 59.3(3) . . ? C26 B38 B39 104.1(3) . . ? B25 B38 B39 108.8(4) . . ? C26 B38 B37 104.7(3) . . ? B25 B38 B37 60.0(3) . . ? B39 B38 B37 60.7(3) . . ? C26 B38 B35 58.0(2) . . ? B25 B38 B35 108.5(3) . . ? B39 B38 B35 59.8(3) . . ? B37 B38 B35 108.3(3) . . ? B38 B39 B35 60.9(3) . . ? B38 B39 B37 59.7(3) . . ? B35 B39 B37 108.4(3) . . ? B38 B39 B32 107.6(3) . . ? B35 B39 B32 107.5(3) . . ? B37 B39 B32 59.9(3) . . ? B38 B39 B34 109.5(3) . . ? B35 B39 B34 60.3(3) . . ? B37 B39 B34 108.9(3) . . ? B32 B39 B34 59.9(3) . . ? C14 B40 B32 103.3(3) . . ? C14 B40 B34 104.9(3) . . ? B32 B40 B34 60.0(3) . . ? C14 B40 B33 57.9(3) . . ? B32 B40 B33 59.1(3) . . ? B34 B40 B33 107.4(3) . . ? C14 B40 Co1 64.1(2) . . ? B32 B40 Co1 117.9(3) . . ? B34 B40 Co1 65.5(2) . . ? B33 B40 Co1 117.0(3) . . ? N44 C46 C42 178.5(6) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.881 _refine_diff_density_min -1.968 _refine_diff_density_rms 0.086