# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email tang@ciac.jl.cn _publ_contact_author_name 'Jinkui Tang' _publ_author_name 'Jinkui Tang' data_1 _database_code_depnum_ccdc_archive 'CCDC 836162' #TrackingRef '- Ln4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C126 H112 Dy4 N4 O34' _chemical_formula_weight 2876.20 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' Dy Dy -0.1892 4.4098 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.3812(10) _cell_length_b 15.6120(10) _cell_length_c 15.9042(11) _cell_angle_alpha 111.3530(10) _cell_angle_beta 97.8070(10) _cell_angle_gamma 118.4660(10) _cell_volume 2895.1(3) _cell_formula_units_Z 1 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 5006 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 26.07 _exptl_crystal_description stick _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 2.636 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6207 _exptl_absorpt_correction_T_max 0.6778 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 187(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16228 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.1035 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 26.11 _reflns_number_total 11381 _reflns_number_gt 7257 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 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^)+(0.0479P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11381 _refine_ls_number_parameters 760 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0946 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1225 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _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 0.59188(3) -0.29789(3) 0.10683(3) 0.02557(12) Uani 1 1 d . . . Dy2 Dy 0.76275(3) 0.12328(3) 0.31245(3) 0.02177(11) Uani 1 1 d . . . N1 N 0.8496(5) 0.1234(5) 0.4597(4) 0.0235(14) Uani 1 1 d . . . N2 N 1.0295(5) 0.4276(5) 0.3415(5) 0.0274(15) Uani 1 1 d . . . O1 O 0.9291(4) 0.2814(4) 0.3950(4) 0.0273(13) Uani 1 1 d . . . H1 H 0.9555 0.3043 0.3510 0.033 Uiso 1 1 calc R . . O2 O 0.9378(5) 0.0210(5) 0.5490(4) 0.0426(16) Uani 1 1 d . . . O3 O 1.2207(5) 0.4884(5) 0.2970(4) 0.0447(16) Uani 1 1 d . . . O4 O 0.6476(4) 0.1839(4) 0.2977(4) 0.0296(13) Uani 1 1 d . . . O5 O 0.7258(4) 0.2237(4) 0.4452(4) 0.0310(13) Uani 1 1 d . . . O6 O 0.8207(4) 0.1964(4) 0.2043(4) 0.0300(13) Uani 1 1 d . . . O7 O 0.6670(4) 0.0323(4) 0.1375(4) 0.0294(13) Uani 1 1 d . . . O8 O 0.8227(4) 0.0152(4) 0.2489(4) 0.0344(14) Uani 1 1 d . . . O9 O 0.7511(4) -0.1525(4) 0.1241(4) 0.0354(14) Uani 1 1 d . . . O10 O 0.6170(4) -0.0243(4) 0.3003(4) 0.0329(14) Uani 1 1 d . . . O11 O 0.5569(4) -0.2043(4) 0.2290(4) 0.0369(15) Uani 1 1 d . . . O12 O 0.7132(4) -0.2529(4) 0.2543(4) 0.0359(14) Uani 1 1 d . . . O13 O 0.5538(4) -0.4099(4) 0.1929(4) 0.0360(14) Uani 1 1 d . . . O14 O 0.6447(5) -0.4135(5) 0.0464(4) 0.0491(17) Uani 1 1 d . . . O15 O 0.5577(5) -0.3612(5) -0.0698(4) 0.0478(17) Uani 1 1 d . . . H15 H 0.5081 -0.4395 -0.1126 0.057 Uiso 1 1 calc R . . O16 O 0.5487(4) -0.1901(4) 0.0554(4) 0.0367(14) Uani 1 1 d . . . H16 H 0.6071 -0.1159 0.0768 0.044 Uiso 1 1 calc R . . O17 O 0.4078(4) -0.4126(4) 0.0358(4) 0.0407(15) Uani 1 1 d . . . C1 C 0.9998(6) 0.3507(6) 0.4816(6) 0.0205(16) Uani 1 1 d . . . C2 C 0.9989(5) 0.3212(6) 0.5559(6) 0.0231(17) Uani 1 1 d . . . C3 C 1.0785(6) 0.3998(6) 0.6475(6) 0.0316(19) Uani 1 1 d . . . H3 H 1.0796 0.3769 0.6952 0.038 Uiso 1 1 calc R . . C4 C 1.1581(7) 0.5109(6) 0.6753(6) 0.031(2) Uani 1 1 d . . . C5 C 1.1583(6) 0.5371(6) 0.6017(6) 0.031(2) Uani 1 1 d . . . H5 H 1.2125 0.6105 0.6166 0.037 Uiso 1 1 calc R . . C6 C 1.0817(6) 0.4606(6) 0.5044(6) 0.0234(18) Uani 1 1 d . . . C7 C 0.9281(6) 0.2083(6) 0.5391(6) 0.0242(17) Uani 1 1 d . . . H7 H 0.9413 0.1960 0.5923 0.029 Uiso 1 1 calc R . . C8 C 0.7934(6) 0.0124(6) 0.4561(6) 0.0282(18) Uani 1 1 d . . . H8A H 0.7194 -0.0119 0.4500 0.034 Uiso 1 1 calc R . . H8B H 0.7890 -0.0427 0.3963 0.034 Uiso 1 1 calc R . . C9 C 0.8426(6) 0.0084(6) 0.5409(6) 0.0278(19) Uani 1 1 d . . . C10 C 0.8171(7) -0.0026(6) 0.6149(6) 0.032(2) Uani 1 1 d . . . H10 H 0.7555 -0.0108 0.6270 0.038 Uiso 1 1 calc R . . C11 C 0.8973(7) 0.0001(7) 0.6716(7) 0.042(2) Uani 1 1 d . . . H11 H 0.9010 -0.0066 0.7288 0.051 Uiso 1 1 calc R . . C12 C 0.9674(7) 0.0140(8) 0.6283(7) 0.049(3) Uani 1 1 d . . . H12 H 1.0307 0.0185 0.6508 0.059 Uiso 1 1 calc R . . C13 C 1.2438(7) 0.5919(6) 0.7740(6) 0.043(2) Uani 1 1 d . . . H13A H 1.2825 0.5609 0.7887 0.064 Uiso 1 1 calc R . . H13B H 1.2120 0.6058 0.8224 0.064 Uiso 1 1 calc R . . H13C H 1.2935 0.6623 0.7761 0.064 Uiso 1 1 calc R . . C14 C 1.0928(6) 0.4929(6) 0.4329(6) 0.0255(18) Uani 1 1 d . . . H14 H 1.1501 0.5670 0.4524 0.031 Uiso 1 1 calc R . . C15 C 1.0503(6) 0.4644(6) 0.2691(6) 0.032(2) Uani 1 1 d . . . H15A H 1.0821 0.5457 0.2999 0.038 Uiso 1 1 calc R . . H15B H 0.9817 0.4251 0.2151 0.038 Uiso 1 1 calc R . . C16 C 1.1238(7) 0.4416(6) 0.2288(6) 0.034(2) Uani 1 1 d . . . C17 C 1.1219(8) 0.3938(7) 0.1385(6) 0.042(2) Uani 1 1 d . . . H17 H 1.0643 0.3558 0.0786 0.050 Uiso 1 1 calc R . . C18 C 1.2238(8) 0.4119(8) 0.1512(8) 0.049(3) Uani 1 1 d . . . H18 H 1.2477 0.3891 0.1008 0.058 Uiso 1 1 calc R . . C19 C 1.2794(8) 0.4669(8) 0.2470(8) 0.053(3) Uani 1 1 d . . . H19 H 1.3496 0.4880 0.2760 0.064 Uiso 1 1 calc R . . C20 C 0.6544(6) 0.2132(6) 0.3850(6) 0.0260(18) Uani 1 1 d . . . C21 C 0.5731(6) 0.2310(6) 0.4142(6) 0.0272(18) Uani 1 1 d . . . C22 C 0.5695(6) 0.2495(6) 0.5056(6) 0.034(2) Uani 1 1 d . . . H22 H 0.6203 0.2535 0.5510 0.041 Uiso 1 1 calc R . . C23 C 0.4920(7) 0.2620(7) 0.5306(8) 0.048(3) Uani 1 1 d . . . H23 H 0.4898 0.2744 0.5931 0.057 Uiso 1 1 calc R . . C24 C 0.4184(7) 0.2567(7) 0.4660(8) 0.050(3) Uani 1 1 d . . . H24 H 0.3642 0.2635 0.4829 0.060 Uiso 1 1 calc R . . C25 C 0.4236(7) 0.2414(8) 0.3766(8) 0.052(3) Uani 1 1 d . . . H25 H 0.3737 0.2398 0.3325 0.062 Uiso 1 1 calc R . . C26 C 0.4998(7) 0.2284(7) 0.3495(7) 0.040(2) Uani 1 1 d . . . H26 H 0.5022 0.2177 0.2874 0.048 Uiso 1 1 calc R . . C27 C 0.7395(6) 0.1125(6) 0.1304(6) 0.0243(17) Uani 1 1 d . . . C28 C 0.7268(6) 0.1050(6) 0.0333(6) 0.0269(18) Uani 1 1 d . . . C29 C 0.8163(7) 0.1751(8) 0.0206(7) 0.046(2) Uani 1 1 d . . . H29 H 0.8842 0.2259 0.0727 0.056 Uiso 1 1 calc R . . C30 C 0.8040(8) 0.1693(8) -0.0708(7) 0.057(3) Uani 1 1 d . . . H30 H 0.8646 0.2156 -0.0810 0.068 Uiso 1 1 calc R . . C31 C 0.7053(8) 0.0974(8) -0.1461(7) 0.052(3) Uani 1 1 d . . . H31 H 0.6972 0.0954 -0.2072 0.063 Uiso 1 1 calc R . . C32 C 0.6194(8) 0.0290(7) -0.1311(6) 0.046(2) Uani 1 1 d . . . H32 H 0.5511 -0.0208 -0.1827 0.055 Uiso 1 1 calc R . . C33 C 0.6291(7) 0.0304(7) -0.0436(6) 0.036(2) Uani 1 1 d . . . H33 H 0.5686 -0.0199 -0.0358 0.044 Uiso 1 1 calc R . . C34 C 0.5487(6) -0.1261(6) 0.2728(5) 0.0230(17) Uani 1 1 d . . . C35 C 0.4514(5) -0.1527(6) 0.2966(5) 0.0214(17) Uani 1 1 d . . . C36 C 0.4496(6) -0.0684(7) 0.3670(6) 0.0321(19) Uani 1 1 d . . . H36 H 0.5110 0.0067 0.4009 0.039 Uiso 1 1 calc R . . C37 C 0.3593(8) -0.0945(8) 0.3870(7) 0.044(2) Uani 1 1 d . . . H37 H 0.3588 -0.0378 0.4364 0.053 Uiso 1 1 calc R . . C38 C 0.2686(7) -0.2032(9) 0.3353(8) 0.053(3) Uani 1 1 d . . . H38 H 0.2058 -0.2206 0.3488 0.064 Uiso 1 1 calc R . . C39 C 0.2691(7) -0.2859(8) 0.2650(7) 0.043(2) Uani 1 1 d . . . H39 H 0.2063 -0.3600 0.2290 0.052 Uiso 1 1 calc R . . C40 C 0.3614(6) -0.2611(6) 0.2464(6) 0.031(2) Uani 1 1 d . . . H40 H 0.3625 -0.3188 0.1991 0.038 Uiso 1 1 calc R . . C41 C 0.8252(6) -0.0510(6) 0.1779(6) 0.0238(17) Uani 1 1 d . . . C42 C 0.9258(6) -0.0079(6) 0.1572(6) 0.0278(19) Uani 1 1 d . . . C43 C 1.0050(6) 0.1058(7) 0.2058(7) 0.041(2) Uani 1 1 d . . . H43 H 0.9945 0.1562 0.2509 0.049 Uiso 1 1 calc R . . C44 C 1.0977(8) 0.1462(10) 0.1896(9) 0.066(3) Uani 1 1 d . . . H44 H 1.1503 0.2247 0.2229 0.080 Uiso 1 1 calc R . . C45 C 1.1162(8) 0.0770(12) 0.1274(10) 0.077(4) Uani 1 1 d . . . H45 H 1.1818 0.1062 0.1180 0.092 Uiso 1 1 calc R . . C46 C 1.0379(9) -0.0379(11) 0.0772(8) 0.063(3) Uani 1 1 d . . . H46 H 1.0505 -0.0869 0.0331 0.075 Uiso 1 1 calc R . . C47 C 0.9405(7) -0.0825(8) 0.0908(6) 0.038(2) Uani 1 1 d . . . H47 H 0.8866 -0.1607 0.0559 0.046 Uiso 1 1 calc R . . C48 C 0.6628(6) -0.4849(6) 0.0215(6) 0.0281(19) Uani 1 1 d . . . C49 C 0.7761(6) -0.4501(6) 0.0581(5) 0.0245(17) Uani 1 1 d . . . C50 C 0.8574(6) -0.3388(6) 0.1262(6) 0.032(2) Uani 1 1 d . . . H50 H 0.8409 -0.2852 0.1500 0.038 Uiso 1 1 calc R . . C51 C 0.9613(7) -0.3064(8) 0.1589(7) 0.042(2) Uani 1 1 d . . . H51 H 1.0169 -0.2304 0.2046 0.051 Uiso 1 1 calc R . . C52 C 0.9841(7) -0.3836(9) 0.1255(7) 0.049(3) Uani 1 1 d . . . H52 H 1.0562 -0.3603 0.1485 0.059 Uiso 1 1 calc R . . C53 C 0.9050(7) -0.4962(8) 0.0585(7) 0.044(2) Uani 1 1 d . . . H53 H 0.9220 -0.5495 0.0373 0.053 Uiso 1 1 calc R . . C54 C 0.8000(6) -0.5280(6) 0.0234(6) 0.0313(19) Uani 1 1 d . . . H54 H 0.7450 -0.6033 -0.0244 0.038 Uiso 1 1 calc R . . C55 C 0.6475(7) -0.3378(7) 0.2585(6) 0.031(2) Uani 1 1 d . . . C56 C 0.6799(7) -0.3531(7) 0.3417(6) 0.033(2) Uani 1 1 d . . . C57 C 0.7797(7) -0.2738(7) 0.4145(6) 0.037(2) Uani 1 1 d . . . H57 H 0.8289 -0.2099 0.4110 0.044 Uiso 1 1 calc R . . C58 C 0.8090(8) -0.2871(8) 0.4940(7) 0.049(3) Uani 1 1 d . . . H58 H 0.8776 -0.2315 0.5446 0.059 Uiso 1 1 calc R . . C59 C 0.7396(9) -0.3796(9) 0.4993(8) 0.056(3) Uani 1 1 d . . . H59 H 0.7600 -0.3885 0.5531 0.067 Uiso 1 1 calc R . . C60 C 0.6394(9) -0.4603(9) 0.4254(8) 0.060(3) Uani 1 1 d . . . H60 H 0.5909 -0.5250 0.4283 0.072 Uiso 1 1 calc R . . C61 C 0.6103(8) -0.4469(7) 0.3486(7) 0.049(3) Uani 1 1 d . . . H61 H 0.5412 -0.5025 0.2987 0.059 Uiso 1 1 calc R . . C62 C 0.4498(7) -0.2218(7) -0.0015(8) 0.060(3) Uani 1 1 d . . . H62A H 0.4055 -0.3027 -0.0467 0.090 Uiso 1 1 calc R . . H62B H 0.4608 -0.1818 -0.0386 0.090 Uiso 1 1 calc R . . H62C H 0.4138 -0.2031 0.0409 0.090 Uiso 1 1 calc R . . C63 C 0.6017(8) -0.2971(7) -0.1149(7) 0.052(3) Uani 1 1 d . . . H63A H 0.6540 -0.2184 -0.0650 0.079 Uiso 1 1 calc R . . H63B H 0.5447 -0.3036 -0.1587 0.079 Uiso 1 1 calc R . . H63C H 0.6370 -0.3245 -0.1525 0.079 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0189(2) 0.01658(19) 0.0292(2) 0.00526(17) 0.00587(18) 0.00743(16) Dy2 0.0194(2) 0.01600(19) 0.0212(2) 0.00744(17) 0.00441(17) 0.00643(16) N1 0.025(4) 0.021(3) 0.021(4) 0.010(3) 0.006(3) 0.011(3) N2 0.032(4) 0.026(3) 0.023(4) 0.011(3) 0.007(3) 0.016(3) O1 0.021(3) 0.021(3) 0.025(3) 0.015(3) 0.006(3) -0.001(2) O2 0.042(4) 0.063(4) 0.052(4) 0.040(4) 0.020(3) 0.039(3) O3 0.042(4) 0.053(4) 0.041(4) 0.021(3) 0.017(3) 0.029(3) O4 0.026(3) 0.028(3) 0.027(3) 0.011(3) 0.008(3) 0.012(3) O5 0.029(3) 0.033(3) 0.032(3) 0.014(3) 0.009(3) 0.021(3) O6 0.025(3) 0.022(3) 0.022(3) 0.008(3) -0.001(3) 0.004(2) O7 0.029(3) 0.023(3) 0.024(3) 0.011(3) 0.007(3) 0.008(3) O8 0.046(4) 0.034(3) 0.027(3) 0.011(3) 0.014(3) 0.028(3) O9 0.025(3) 0.024(3) 0.037(4) 0.010(3) 0.008(3) 0.005(3) O10 0.025(3) 0.025(3) 0.040(4) 0.019(3) 0.007(3) 0.009(3) O11 0.033(3) 0.031(3) 0.046(4) 0.014(3) 0.018(3) 0.020(3) O12 0.033(3) 0.031(3) 0.036(4) 0.011(3) 0.011(3) 0.017(3) O13 0.031(3) 0.023(3) 0.035(4) 0.009(3) 0.006(3) 0.009(3) O14 0.051(4) 0.049(4) 0.044(4) 0.007(3) 0.010(3) 0.040(4) O15 0.063(4) 0.027(3) 0.033(4) 0.010(3) 0.010(3) 0.018(3) O16 0.029(3) 0.019(3) 0.041(4) 0.009(3) 0.000(3) 0.008(3) O17 0.024(3) 0.033(3) 0.054(4) 0.020(3) 0.006(3) 0.013(3) C1 0.019(4) 0.024(4) 0.024(4) 0.014(4) 0.009(4) 0.015(3) C2 0.015(4) 0.021(4) 0.023(4) 0.010(4) 0.002(3) 0.006(3) C3 0.031(5) 0.035(5) 0.025(5) 0.014(4) 0.004(4) 0.018(4) C4 0.036(5) 0.027(4) 0.018(4) 0.007(4) 0.003(4) 0.014(4) C5 0.020(4) 0.020(4) 0.027(5) 0.003(4) -0.004(4) 0.004(3) C6 0.018(4) 0.025(4) 0.031(5) 0.016(4) 0.019(4) 0.011(4) C7 0.024(4) 0.034(4) 0.026(5) 0.022(4) 0.015(4) 0.017(4) C8 0.025(4) 0.028(4) 0.029(5) 0.017(4) 0.010(4) 0.011(4) C9 0.028(5) 0.016(4) 0.037(5) 0.012(4) 0.011(4) 0.012(4) C10 0.036(5) 0.030(4) 0.034(5) 0.020(4) 0.021(4) 0.017(4) C11 0.052(6) 0.049(6) 0.033(5) 0.025(5) 0.013(5) 0.031(5) C12 0.039(6) 0.060(6) 0.056(7) 0.035(6) 0.008(5) 0.032(5) C13 0.042(6) 0.026(4) 0.025(5) 0.007(4) -0.007(4) 0.007(4) C14 0.028(4) 0.019(4) 0.030(5) 0.015(4) 0.016(4) 0.010(4) C15 0.037(5) 0.025(4) 0.027(5) 0.018(4) 0.009(4) 0.012(4) C16 0.034(5) 0.026(4) 0.022(5) 0.007(4) 0.003(4) 0.008(4) C17 0.052(6) 0.045(5) 0.025(5) 0.020(5) 0.012(5) 0.023(5) C18 0.054(7) 0.052(6) 0.060(7) 0.037(6) 0.038(6) 0.033(6) C19 0.055(7) 0.062(7) 0.065(8) 0.036(6) 0.030(6) 0.042(6) C20 0.026(4) 0.011(3) 0.031(5) 0.006(4) 0.009(4) 0.008(3) C21 0.023(4) 0.016(4) 0.036(5) 0.010(4) 0.013(4) 0.008(3) C22 0.034(5) 0.031(4) 0.031(5) 0.010(4) 0.011(4) 0.017(4) C23 0.042(6) 0.036(5) 0.058(7) 0.014(5) 0.029(6) 0.021(5) C24 0.027(5) 0.042(6) 0.073(8) 0.022(6) 0.019(6) 0.020(5) C25 0.044(6) 0.059(6) 0.065(8) 0.031(6) 0.018(6) 0.038(6) C26 0.037(5) 0.036(5) 0.041(6) 0.015(5) 0.007(5) 0.022(4) C27 0.024(4) 0.022(4) 0.021(4) 0.008(4) 0.004(4) 0.013(4) C28 0.027(4) 0.023(4) 0.023(5) 0.009(4) 0.007(4) 0.012(4) C29 0.038(6) 0.058(6) 0.035(6) 0.024(5) 0.016(5) 0.022(5) C30 0.048(7) 0.064(7) 0.047(7) 0.035(6) 0.017(6) 0.018(6) C31 0.060(7) 0.070(7) 0.033(6) 0.034(6) 0.015(6) 0.035(6) C32 0.055(6) 0.043(5) 0.023(5) 0.012(5) -0.001(5) 0.024(5) C33 0.034(5) 0.034(5) 0.031(5) 0.019(4) 0.007(4) 0.012(4) C34 0.015(4) 0.023(4) 0.021(4) 0.009(4) 0.003(3) 0.007(3) C35 0.017(4) 0.024(4) 0.020(4) 0.011(4) 0.006(3) 0.010(3) C36 0.029(5) 0.043(5) 0.025(5) 0.019(4) 0.010(4) 0.019(4) C37 0.057(7) 0.071(7) 0.034(6) 0.028(6) 0.026(5) 0.052(6) C38 0.029(6) 0.086(8) 0.059(7) 0.043(7) 0.029(6) 0.034(6) C39 0.023(5) 0.053(6) 0.058(7) 0.042(6) 0.014(5) 0.014(5) C40 0.039(5) 0.023(4) 0.027(5) 0.014(4) 0.011(4) 0.014(4) C41 0.025(4) 0.023(4) 0.027(5) 0.015(4) 0.005(4) 0.016(4) C42 0.018(4) 0.032(4) 0.029(5) 0.018(4) 0.003(4) 0.011(4) C43 0.023(5) 0.041(5) 0.057(7) 0.032(5) 0.012(5) 0.013(4) C44 0.033(6) 0.080(8) 0.081(9) 0.061(8) 0.016(6) 0.015(6) C45 0.032(6) 0.134(12) 0.093(11) 0.097(11) 0.028(7) 0.036(8) C46 0.068(8) 0.127(10) 0.055(7) 0.067(8) 0.047(7) 0.075(8) C47 0.043(5) 0.056(6) 0.034(5) 0.028(5) 0.020(5) 0.034(5) C48 0.028(5) 0.023(4) 0.039(5) 0.017(4) 0.014(4) 0.017(4) C49 0.027(4) 0.031(4) 0.018(4) 0.013(4) 0.011(4) 0.018(4) C50 0.024(5) 0.029(4) 0.027(5) 0.010(4) 0.002(4) 0.009(4) C51 0.031(5) 0.043(5) 0.036(6) 0.021(5) 0.011(5) 0.010(5) C52 0.015(5) 0.087(8) 0.036(6) 0.037(6) 0.009(4) 0.018(5) C53 0.045(6) 0.060(6) 0.055(7) 0.034(6) 0.026(5) 0.042(6) C54 0.025(4) 0.030(4) 0.032(5) 0.013(4) 0.011(4) 0.013(4) C55 0.034(5) 0.028(4) 0.031(5) 0.006(4) 0.011(4) 0.024(4) C56 0.047(5) 0.031(4) 0.030(5) 0.013(4) 0.013(4) 0.030(4) C57 0.045(6) 0.040(5) 0.034(5) 0.015(5) 0.016(5) 0.032(5) C58 0.054(6) 0.057(6) 0.032(6) 0.009(5) 0.004(5) 0.042(6) C59 0.075(8) 0.057(7) 0.056(7) 0.026(6) 0.023(7) 0.053(7) C60 0.082(9) 0.050(6) 0.054(7) 0.030(6) 0.028(7) 0.038(7) C61 0.069(7) 0.028(5) 0.031(6) 0.012(5) 0.011(5) 0.020(5) C62 0.039(6) 0.035(5) 0.092(9) 0.036(6) 0.006(6) 0.013(5) C63 0.062(7) 0.031(5) 0.049(7) 0.013(5) 0.023(6) 0.020(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O11 2.273(5) . ? Dy1 O14 2.278(5) . ? Dy1 O9 2.300(5) . ? Dy1 O17 2.307(5) . ? Dy1 O12 2.417(6) . ? Dy1 O16 2.421(5) . ? Dy1 O15 2.495(6) . ? Dy1 O13 2.502(5) . ? Dy1 C55 2.825(9) . ? Dy2 O10 2.238(5) . ? Dy2 O1 2.252(5) . ? Dy2 O8 2.284(5) . ? Dy2 O4 2.396(5) . ? Dy2 O6 2.435(5) . ? Dy2 O7 2.438(5) . ? Dy2 O5 2.450(5) . ? Dy2 N1 2.533(6) . ? Dy2 C20 2.766(7) . ? Dy2 C27 2.802(8) . ? N1 C7 1.284(9) . ? N1 C8 1.496(9) . ? N2 C14 1.300(9) . ? N2 C15 1.471(9) . ? O1 C1 1.280(8) . ? O1 H1 0.9500 . ? O2 C12 1.342(10) . ? O2 C9 1.363(9) . ? O3 C19 1.359(10) . ? O3 C16 1.371(9) . ? O4 C20 1.264(9) . ? O5 C20 1.256(9) . ? O6 C27 1.256(8) . ? O7 C27 1.277(8) . ? O8 C41 1.243(9) . ? O9 C41 1.252(8) . ? O10 C34 1.264(8) . ? O11 C34 1.242(8) . ? O12 C55 1.261(9) . ? O13 C55 1.274(9) . ? O14 C48 1.216(8) . ? O15 C63 1.409(10) . ? O15 H15 0.9500 . ? O16 C62 1.401(10) . ? O16 H16 0.9500 . ? O17 C48 1.258(8) 2_645 ? C1 C2 1.414(10) . ? C1 C6 1.424(9) . ? C2 C3 1.382(10) . ? C2 C7 1.453(9) . ? C3 C4 1.405(10) . ? C3 H3 0.9500 . ? C4 C5 1.373(11) . ? C4 C13 1.485(10) . ? C5 C6 1.423(10) . ? C5 H5 0.9500 . ? C6 C14 1.401(10) . ? C7 H7 0.9500 . ? C8 C9 1.491(11) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.334(11) . ? C10 C11 1.400(11) . ? C10 H10 0.9500 . ? C11 C12 1.331(12) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14 0.9500 . ? C15 C16 1.494(11) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.343(11) . ? C17 C18 1.424(12) . ? C17 H17 0.9500 . ? C18 C19 1.336(13) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.501(10) . ? C21 C22 1.390(11) . ? C21 C26 1.393(11) . ? C22 C23 1.382(11) . ? C22 H22 0.9500 . ? C23 C24 1.370(13) . ? C23 H23 0.9500 . ? C24 C25 1.374(13) . ? C24 H24 0.9500 . ? C25 C26 1.378(12) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.483(11) . ? C28 C33 1.380(10) . ? C28 C29 1.390(11) . ? C29 C30 1.404(13) . ? C29 H29 0.9500 . ? C30 C31 1.379(12) . ? C30 H30 0.9500 . ? C31 C32 1.368(13) . ? C31 H31 0.9500 . ? C32 C33 1.371(11) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.493(10) . ? C35 C40 1.379(9) . ? C35 C36 1.399(10) . ? C36 C37 1.368(11) . ? C36 H36 0.9500 . ? C37 C38 1.385(12) . ? C37 H37 0.9500 . ? C38 C39 1.370(13) . ? C38 H38 0.9500 . ? C39 C40 1.388(11) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.505(10) . ? C42 C43 1.383(10) . ? C42 C47 1.393(11) . ? C43 C44 1.363(12) . ? C43 H43 0.9500 . ? C44 C45 1.349(16) . ? C44 H44 0.9500 . ? C45 C46 1.393(15) . ? C45 H45 0.9500 . ? C46 C47 1.407(12) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 O17 1.258(8) 2_645 ? C48 C49 1.505(10) . ? C49 C54 1.382(10) . ? C49 C50 1.395(10) . ? C50 C51 1.377(11) . ? C50 H50 0.9500 . ? C51 C52 1.358(12) . ? C51 H51 0.9500 . ? C52 C53 1.397(12) . ? C52 H52 0.9500 . ? C53 C54 1.398(11) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.491(11) . ? C56 C57 1.375(11) . ? C56 C61 1.399(11) . ? C57 C58 1.404(12) . ? C57 H57 0.9500 . ? C58 C59 1.369(13) . ? C58 H58 0.9500 . ? C59 C60 1.386(13) . ? C59 H59 0.9500 . ? C60 C61 1.366(13) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Dy1 O14 149.6(2) . . ? O11 Dy1 O9 100.68(19) . . ? O14 Dy1 O9 88.7(2) . . ? O11 Dy1 O17 81.7(2) . . ? O14 Dy1 O17 104.7(2) . . ? O9 Dy1 O17 149.3(2) . . ? O11 Dy1 O12 75.31(19) . . ? O14 Dy1 O12 78.5(2) . . ? O9 Dy1 O12 78.4(2) . . ? O17 Dy1 O12 130.8(2) . . ? O11 Dy1 O16 74.4(2) . . ? O14 Dy1 O16 135.9(2) . . ? O9 Dy1 O16 74.09(19) . . ? O17 Dy1 O16 77.22(18) . . ? O12 Dy1 O16 133.94(17) . . ? O11 Dy1 O15 140.6(2) . . ? O14 Dy1 O15 69.0(2) . . ? O9 Dy1 O15 82.1(2) . . ? O17 Dy1 O15 77.4(2) . . ? O12 Dy1 O15 142.2(2) . . ? O16 Dy1 O15 68.57(19) . . ? O11 Dy1 O13 78.43(19) . . ? O14 Dy1 O13 73.7(2) . . ? O9 Dy1 O13 130.56(19) . . ? O17 Dy1 O13 80.08(19) . . ? O12 Dy1 O13 53.19(18) . . ? O16 Dy1 O13 146.63(19) . . ? O15 Dy1 O13 129.17(17) . . ? O11 Dy1 C55 74.9(2) . . ? O14 Dy1 C55 74.8(2) . . ? O9 Dy1 C55 104.4(2) . . ? O17 Dy1 C55 105.7(2) . . ? O12 Dy1 C55 26.38(19) . . ? O16 Dy1 C55 148.4(2) . . ? O15 Dy1 C55 143.1(2) . . ? O13 Dy1 C55 26.81(19) . . ? O10 Dy2 O1 153.0(2) . . ? O10 Dy2 O8 90.28(19) . . ? O1 Dy2 O8 92.89(19) . . ? O10 Dy2 O4 82.99(18) . . ? O1 Dy2 O4 105.22(17) . . ? O8 Dy2 O4 152.37(19) . . ? O10 Dy2 O6 136.60(18) . . ? O1 Dy2 O6 70.40(17) . . ? O8 Dy2 O6 84.32(18) . . ? O4 Dy2 O6 82.41(18) . . ? O10 Dy2 O7 83.09(18) . . ? O1 Dy2 O7 123.77(18) . . ? O8 Dy2 O7 77.48(18) . . ? O4 Dy2 O7 75.12(18) . . ? O6 Dy2 O7 53.67(16) . . ? O10 Dy2 O5 81.47(18) . . ? O1 Dy2 O5 83.06(18) . . ? O8 Dy2 O5 151.53(19) . . ? O4 Dy2 O5 53.71(18) . . ? O6 Dy2 O5 120.05(17) . . ? O7 Dy2 O5 127.82(17) . . ? O10 Dy2 N1 82.59(19) . . ? O1 Dy2 N1 72.00(18) . . ? O8 Dy2 N1 77.36(19) . . ? O4 Dy2 N1 127.76(19) . . ? O6 Dy2 N1 136.95(18) . . ? O7 Dy2 N1 150.87(18) . . ? O5 Dy2 N1 74.59(18) . . ? O10 Dy2 C20 77.6(2) . . ? O1 Dy2 C20 97.8(2) . . ? O8 Dy2 C20 167.9(2) . . ? O4 Dy2 C20 27.2(2) . . ? O6 Dy2 C20 104.5(2) . . ? O7 Dy2 C20 100.9(2) . . ? O5 Dy2 C20 27.0(2) . . ? N1 Dy2 C20 100.6(2) . . ? O10 Dy2 C27 110.1(2) . . ? O1 Dy2 C27 96.8(2) . . ? O8 Dy2 C27 79.7(2) . . ? O4 Dy2 C27 77.6(2) . . ? O6 Dy2 C27 26.58(17) . . ? O7 Dy2 C27 27.09(18) . . ? O5 Dy2 C27 128.70(19) . . ? N1 Dy2 C27 153.8(2) . . ? C20 Dy2 C27 104.4(2) . . ? C7 N1 C8 117.5(6) . . ? C7 N1 Dy2 127.5(5) . . ? C8 N1 Dy2 114.6(4) . . ? C14 N2 C15 121.1(6) . . ? C1 O1 Dy2 140.8(5) . . ? C1 O1 H1 109.6 . . ? Dy2 O1 H1 109.6 . . ? C12 O2 C9 105.8(7) . . ? C19 O3 C16 106.6(7) . . ? C20 O4 Dy2 93.0(5) . . ? C20 O5 Dy2 90.7(5) . . ? C27 O6 Dy2 93.2(4) . . ? C27 O7 Dy2 92.5(4) . . ? C41 O8 Dy2 150.8(5) . . ? C41 O9 Dy1 144.6(5) . . ? C34 O10 Dy2 157.4(5) . . ? C34 O11 Dy1 150.5(5) . . ? C55 O12 Dy1 95.2(5) . . ? C55 O13 Dy1 90.9(5) . . ? C48 O14 Dy1 168.9(6) . . ? C63 O15 Dy1 129.0(5) . . ? C63 O15 H15 115.5 . . ? Dy1 O15 H15 115.5 . . ? C62 O16 Dy1 129.1(5) . . ? C62 O16 H16 115.5 . . ? Dy1 O16 H16 115.5 . . ? C48 O17 Dy1 136.7(5) 2_645 . ? O1 C1 C2 121.8(6) . . ? O1 C1 C6 119.3(7) . . ? C2 C1 C6 118.8(7) . . ? C3 C2 C1 118.7(7) . . ? C3 C2 C7 116.8(7) . . ? C1 C2 C7 123.9(7) . . ? C2 C3 C4 124.9(8) . . ? C2 C3 H3 117.6 . . ? C4 C3 H3 117.6 . . ? C5 C4 C3 115.2(7) . . ? C5 C4 C13 121.4(7) . . ? C3 C4 C13 123.1(8) . . ? C4 C5 C6 123.7(7) . . ? C4 C5 H5 118.1 . . ? C6 C5 H5 118.1 . . ? C14 C6 C5 119.4(7) . . ? C14 C6 C1 122.0(7) . . ? C5 C6 C1 118.5(7) . . ? N1 C7 C2 126.7(7) . . ? N1 C7 H7 116.6 . . ? C2 C7 H7 116.6 . . ? C9 C8 N1 116.3(6) . . ? C9 C8 H8A 108.2 . . ? N1 C8 H8A 108.2 . . ? C9 C8 H8B 108.2 . . ? N1 C8 H8B 108.2 . . ? H8A C8 H8B 107.4 . . ? C10 C9 O2 109.4(7) . . ? C10 C9 C8 135.3(8) . . ? O2 C9 C8 115.3(7) . . ? C9 C10 C11 107.8(8) . . ? C9 C10 H10 126.1 . . ? C11 C10 H10 126.1 . . ? C12 C11 C10 105.2(8) . . ? C12 C11 H11 127.4 . . ? C10 C11 H11 127.4 . . ? C11 C12 O2 111.8(8) . . ? C11 C12 H12 124.1 . . ? O2 C12 H12 124.1 . . ? C4 C13 H13A 109.5 . . ? C4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 C6 124.0(7) . . ? N2 C14 H14 118.0 . . ? C6 C14 H14 118.0 . . ? N2 C15 C16 112.2(6) . . ? N2 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? N2 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C17 C16 O3 110.2(8) . . ? C17 C16 C15 134.5(8) . . ? O3 C16 C15 114.9(7) . . ? C16 C17 C18 105.8(9) . . ? C16 C17 H17 127.1 . . ? C18 C17 H17 127.1 . . ? C19 C18 C17 107.3(9) . . ? C19 C18 H18 126.3 . . ? C17 C18 H18 126.3 . . ? C18 C19 O3 110.0(9) . . ? C18 C19 H19 125.0 . . ? O3 C19 H19 125.0 . . ? O5 C20 O4 120.6(7) . . ? O5 C20 C21 120.7(8) . . ? O4 C20 C21 118.7(7) . . ? O5 C20 Dy2 62.3(4) . . ? O4 C20 Dy2 59.9(4) . . ? C21 C20 Dy2 165.3(5) . . ? C22 C21 C26 119.3(8) . . ? C22 C21 C20 120.5(8) . . ? C26 C21 C20 120.2(8) . . ? C23 C22 C21 120.0(9) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 120.6(10) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 119.4(9) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C24 C25 C26 121.3(9) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C25 C26 C21 119.3(9) . . ? C25 C26 H26 120.3 . . ? C21 C26 H26 120.3 . . ? O6 C27 O7 120.6(7) . . ? O6 C27 C28 120.4(7) . . ? O7 C27 C28 119.0(7) . . ? O6 C27 Dy2 60.2(4) . . ? O7 C27 Dy2 60.4(4) . . ? C28 C27 Dy2 179.1(5) . . ? C33 C28 C29 120.0(8) . . ? C33 C28 C27 121.5(7) . . ? C29 C28 C27 118.5(7) . . ? C28 C29 C30 118.5(9) . . ? C28 C29 H29 120.8 . . ? C30 C29 H29 120.8 . . ? C31 C30 C29 121.1(9) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C32 C31 C30 118.6(9) . . ? C32 C31 H31 120.7 . . ? C30 C31 H31 120.7 . . ? C31 C32 C33 121.7(9) . . ? C31 C32 H32 119.1 . . ? C33 C32 H32 119.1 . . ? C32 C33 C28 119.9(8) . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? O11 C34 O10 125.2(7) . . ? O11 C34 C35 118.2(6) . . ? O10 C34 C35 116.5(6) . . ? C40 C35 C36 119.8(7) . . ? C40 C35 C34 119.5(7) . . ? C36 C35 C34 120.8(7) . . ? C37 C36 C35 119.7(8) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C36 C37 C38 120.3(8) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C39 C38 C37 120.3(8) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C38 C39 C40 120.0(8) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C35 C40 C39 119.9(8) . . ? C35 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? O8 C41 O9 124.6(7) . . ? O8 C41 C42 118.0(7) . . ? O9 C41 C42 117.4(7) . . ? C43 C42 C47 119.9(8) . . ? C43 C42 C41 120.0(7) . . ? C47 C42 C41 120.1(7) . . ? C44 C43 C42 120.8(10) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C45 C44 C43 121.3(11) . . ? C45 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C44 C45 C46 119.2(10) . . ? C44 C45 H45 120.4 . . ? C46 C45 H45 120.4 . . ? C45 C46 C47 121.0(10) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C42 C47 C46 117.6(9) . . ? C42 C47 H47 121.2 . . ? C46 C47 H47 121.2 . . ? O14 C48 O17 123.9(7) . 2_645 ? O14 C48 C49 119.1(7) . . ? O17 C48 C49 117.0(7) 2_645 . ? C54 C49 C50 120.0(7) . . ? C54 C49 C48 120.1(7) . . ? C50 C49 C48 119.9(7) . . ? C51 C50 C49 120.1(8) . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C52 C51 C50 119.7(8) . . ? C52 C51 H51 120.2 . . ? C50 C51 H51 120.2 . . ? C51 C52 C53 122.1(8) . . ? C51 C52 H52 119.0 . . ? C53 C52 H52 119.0 . . ? C52 C53 C54 118.0(8) . . ? C52 C53 H53 121.0 . . ? C54 C53 H53 121.0 . . ? C49 C54 C53 120.2(8) . . ? C49 C54 H54 119.9 . . ? C53 C54 H54 119.9 . . ? O12 C55 O13 120.7(8) . . ? O12 C55 C56 119.4(8) . . ? O13 C55 C56 119.9(8) . . ? O12 C55 Dy1 58.4(4) . . ? O13 C55 Dy1 62.3(4) . . ? C56 C55 Dy1 177.3(5) . . ? C57 C56 C61 118.4(8) . . ? C57 C56 C55 120.2(8) . . ? C61 C56 C55 121.4(8) . . ? C56 C57 C58 120.1(9) . . ? C56 C57 H57 120.0 . . ? C58 C57 H57 120.0 . . ? C59 C58 C57 120.6(10) . . ? C59 C58 H58 119.7 . . ? C57 C58 H58 119.7 . . ? C58 C59 C60 119.4(10) . . ? C58 C59 H59 120.3 . . ? C60 C59 H59 120.3 . . ? C61 C60 C59 120.1(10) . . ? C61 C60 H60 119.9 . . ? C59 C60 H60 119.9 . . ? C60 C61 C56 121.4(10) . . ? C60 C61 H61 119.3 . . ? C56 C61 H61 119.3 . . ? O16 C62 H62A 109.5 . . ? O16 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? O16 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? O15 C63 H63A 109.5 . . ? O15 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? O15 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O10 Dy2 N1 C7 -148.2(6) . . . . ? O1 Dy2 N1 C7 22.5(6) . . . . ? O8 Dy2 N1 C7 119.9(6) . . . . ? O4 Dy2 N1 C7 -73.0(6) . . . . ? O6 Dy2 N1 C7 52.7(7) . . . . ? O7 Dy2 N1 C7 150.7(5) . . . . ? O5 Dy2 N1 C7 -65.0(6) . . . . ? C20 Dy2 N1 C7 -72.3(6) . . . . ? C27 Dy2 N1 C7 90.4(7) . . . . ? O10 Dy2 N1 C8 24.4(5) . . . . ? O1 Dy2 N1 C8 -164.9(5) . . . . ? O8 Dy2 N1 C8 -67.6(5) . . . . ? O4 Dy2 N1 C8 99.5(5) . . . . ? O6 Dy2 N1 C8 -134.7(4) . . . . ? O7 Dy2 N1 C8 -36.8(7) . . . . ? O5 Dy2 N1 C8 107.5(5) . . . . ? C20 Dy2 N1 C8 100.2(5) . . . . ? C27 Dy2 N1 C8 -97.1(6) . . . . ? O10 Dy2 O1 C1 -8.8(10) . . . . ? O8 Dy2 O1 C1 -105.1(7) . . . . ? O4 Dy2 O1 C1 96.0(7) . . . . ? O6 Dy2 O1 C1 172.0(8) . . . . ? O7 Dy2 O1 C1 178.1(7) . . . . ? O5 Dy2 O1 C1 46.6(7) . . . . ? N1 Dy2 O1 C1 -29.4(7) . . . . ? C20 Dy2 O1 C1 69.3(7) . . . . ? C27 Dy2 O1 C1 174.9(7) . . . . ? O10 Dy2 O4 C20 76.6(4) . . . . ? O1 Dy2 O4 C20 -77.2(4) . . . . ? O8 Dy2 O4 C20 153.6(4) . . . . ? O6 Dy2 O4 C20 -144.4(4) . . . . ? O7 Dy2 O4 C20 161.2(4) . . . . ? O5 Dy2 O4 C20 -8.0(4) . . . . ? N1 Dy2 O4 C20 1.6(5) . . . . ? C27 Dy2 O4 C20 -171.0(5) . . . . ? O10 Dy2 O5 C20 -79.5(4) . . . . ? O1 Dy2 O5 C20 122.7(4) . . . . ? O8 Dy2 O5 C20 -154.1(4) . . . . ? O4 Dy2 O5 C20 8.0(4) . . . . ? O6 Dy2 O5 C20 60.1(5) . . . . ? O7 Dy2 O5 C20 -5.2(5) . . . . ? N1 Dy2 O5 C20 -164.1(5) . . . . ? C27 Dy2 O5 C20 29.5(5) . . . . ? O10 Dy2 O6 C27 -6.0(5) . . . . ? O1 Dy2 O6 C27 173.5(5) . . . . ? O8 Dy2 O6 C27 78.4(4) . . . . ? O4 Dy2 O6 C27 -77.3(4) . . . . ? O7 Dy2 O6 C27 -0.3(4) . . . . ? O5 Dy2 O6 C27 -117.2(4) . . . . ? N1 Dy2 O6 C27 143.0(4) . . . . ? C20 Dy2 O6 C27 -93.2(4) . . . . ? O10 Dy2 O7 C27 176.3(4) . . . . ? O1 Dy2 O7 C27 -6.9(5) . . . . ? O8 Dy2 O7 C27 -91.9(4) . . . . ? O4 Dy2 O7 C27 91.7(4) . . . . ? O6 Dy2 O7 C27 0.2(4) . . . . ? O5 Dy2 O7 C27 102.7(4) . . . . ? N1 Dy2 O7 C27 -122.7(5) . . . . ? C20 Dy2 O7 C27 100.3(4) . . . . ? O10 Dy2 O8 C41 85.8(11) . . . . ? O1 Dy2 O8 C41 -121.1(11) . . . . ? O4 Dy2 O8 C41 10.5(13) . . . . ? O6 Dy2 O8 C41 -51.1(11) . . . . ? O7 Dy2 O8 C41 2.9(11) . . . . ? O5 Dy2 O8 C41 158.2(10) . . . . ? N1 Dy2 O8 C41 168.1(11) . . . . ? C20 Dy2 O8 C41 86.5(15) . . . . ? C27 Dy2 O8 C41 -24.6(11) . . . . ? O11 Dy1 O9 C41 10.5(9) . . . . ? O14 Dy1 O9 C41 -140.4(9) . . . . ? O17 Dy1 O9 C41 102.2(9) . . . . ? O12 Dy1 O9 C41 -61.9(9) . . . . ? O16 Dy1 O9 C41 80.7(9) . . . . ? O15 Dy1 O9 C41 150.6(9) . . . . ? O13 Dy1 O9 C41 -73.3(9) . . . . ? C55 Dy1 O9 C41 -66.5(9) . . . . ? O1 Dy2 O10 C34 -111.0(14) . . . . ? O8 Dy2 O10 C34 -14.1(14) . . . . ? O4 Dy2 O10 C34 139.0(14) . . . . ? O6 Dy2 O10 C34 67.9(14) . . . . ? O7 Dy2 O10 C34 63.2(14) . . . . ? O5 Dy2 O10 C34 -166.8(14) . . . . ? N1 Dy2 O10 C34 -91.3(14) . . . . ? C20 Dy2 O10 C34 166.0(14) . . . . ? C27 Dy2 O10 C34 65.0(14) . . . . ? O14 Dy1 O11 C34 155.4(9) . . . . ? O9 Dy1 O11 C34 49.5(10) . . . . ? O17 Dy1 O11 C34 -99.5(10) . . . . ? O12 Dy1 O11 C34 124.4(10) . . . . ? O16 Dy1 O11 C34 -20.5(10) . . . . ? O15 Dy1 O11 C34 -41.0(11) . . . . ? O13 Dy1 O11 C34 179.0(10) . . . . ? C55 Dy1 O11 C34 151.7(10) . . . . ? O11 Dy1 O12 C55 85.6(4) . . . . ? O14 Dy1 O12 C55 -78.9(5) . . . . ? O9 Dy1 O12 C55 -169.9(5) . . . . ? O17 Dy1 O12 C55 20.7(5) . . . . ? O16 Dy1 O12 C55 135.9(4) . . . . ? O15 Dy1 O12 C55 -109.6(5) . . . . ? O13 Dy1 O12 C55 -0.8(4) . . . . ? O11 Dy1 O13 C55 -79.5(4) . . . . ? O14 Dy1 O13 C55 88.4(4) . . . . ? O9 Dy1 O13 C55 14.8(5) . . . . ? O17 Dy1 O13 C55 -162.9(5) . . . . ? O12 Dy1 O13 C55 0.8(4) . . . . ? O16 Dy1 O13 C55 -115.3(5) . . . . ? O15 Dy1 O13 C55 132.3(4) . . . . ? O11 Dy1 O14 C48 39(3) . . . . ? O9 Dy1 O14 C48 148(3) . . . . ? O17 Dy1 O14 C48 -60(3) . . . . ? O12 Dy1 O14 C48 70(3) . . . . ? O16 Dy1 O14 C48 -146(3) . . . . ? O15 Dy1 O14 C48 -130(3) . . . . ? O13 Dy1 O14 C48 15(3) . . . . ? C55 Dy1 O14 C48 43(3) . . . . ? O11 Dy1 O15 C63 72.0(8) . . . . ? O14 Dy1 O15 C63 -116.8(8) . . . . ? O9 Dy1 O15 C63 -25.2(7) . . . . ? O17 Dy1 O15 C63 131.8(7) . . . . ? O12 Dy1 O15 C63 -84.5(8) . . . . ? O16 Dy1 O15 C63 50.8(7) . . . . ? O13 Dy1 O15 C63 -162.4(7) . . . . ? C55 Dy1 O15 C63 -128.7(7) . . . . ? O11 Dy1 O16 C62 -92.5(8) . . . . ? O14 Dy1 O16 C62 90.5(8) . . . . ? O9 Dy1 O16 C62 161.3(8) . . . . ? O17 Dy1 O16 C62 -7.7(8) . . . . ? O12 Dy1 O16 C62 -143.1(7) . . . . ? O15 Dy1 O16 C62 73.7(8) . . . . ? O13 Dy1 O16 C62 -55.9(9) . . . . ? C55 Dy1 O16 C62 -106.9(8) . . . . ? O11 Dy1 O17 C48 -147.8(8) . . . 2_645 ? O14 Dy1 O17 C48 1.9(8) . . . 2_645 ? O9 Dy1 O17 C48 115.2(8) . . . 2_645 ? O12 Dy1 O17 C48 -85.4(8) . . . 2_645 ? O16 Dy1 O17 C48 136.5(8) . . . 2_645 ? O15 Dy1 O17 C48 65.9(8) . . . 2_645 ? O13 Dy1 O17 C48 -68.2(8) . . . 2_645 ? C55 Dy1 O17 C48 -76.1(8) . . . 2_645 ? Dy2 O1 C1 C2 21.0(11) . . . . ? Dy2 O1 C1 C6 -158.9(5) . . . . ? O1 C1 C2 C3 179.1(7) . . . . ? C6 C1 C2 C3 -0.9(11) . . . . ? O1 C1 C2 C7 8.2(11) . . . . ? C6 C1 C2 C7 -171.9(7) . . . . ? C1 C2 C3 C4 4.3(12) . . . . ? C7 C2 C3 C4 175.9(7) . . . . ? C2 C3 C4 C5 -5.0(12) . . . . ? C2 C3 C4 C13 -178.6(8) . . . . ? C3 C4 C5 C6 2.5(12) . . . . ? C13 C4 C5 C6 176.3(8) . . . . ? C4 C5 C6 C14 -175.7(8) . . . . ? C4 C5 C6 C1 0.4(12) . . . . ? O1 C1 C6 C14 -5.3(11) . . . . ? C2 C1 C6 C14 174.7(7) . . . . ? O1 C1 C6 C5 178.7(7) . . . . ? C2 C1 C6 C5 -1.3(10) . . . . ? C8 N1 C7 C2 174.7(7) . . . . ? Dy2 N1 C7 C2 -13.0(11) . . . . ? C3 C2 C7 N1 -179.9(7) . . . . ? C1 C2 C7 N1 -8.8(12) . . . . ? C7 N1 C8 C9 -7.4(10) . . . . ? Dy2 N1 C8 C9 179.3(5) . . . . ? C12 O2 C9 C10 1.7(9) . . . . ? C12 O2 C9 C8 -179.6(7) . . . . ? N1 C8 C9 C10 109.5(10) . . . . ? N1 C8 C9 O2 -68.8(9) . . . . ? O2 C9 C10 C11 -1.5(9) . . . . ? C8 C9 C10 C11 -179.9(8) . . . . ? C9 C10 C11 C12 0.7(10) . . . . ? C10 C11 C12 O2 0.3(11) . . . . ? C9 O2 C12 C11 -1.2(10) . . . . ? C15 N2 C14 C6 -175.6(7) . . . . ? C5 C6 C14 N2 177.3(7) . . . . ? C1 C6 C14 N2 1.3(12) . . . . ? C14 N2 C15 C16 86.7(9) . . . . ? C19 O3 C16 C17 -1.0(9) . . . . ? C19 O3 C16 C15 -175.1(7) . . . . ? N2 C15 C16 C17 131.1(10) . . . . ? N2 C15 C16 O3 -56.7(9) . . . . ? O3 C16 C17 C18 0.0(10) . . . . ? C15 C16 C17 C18 172.4(9) . . . . ? C16 C17 C18 C19 1.1(10) . . . . ? C17 C18 C19 O3 -1.8(11) . . . . ? C16 O3 C19 C18 1.7(10) . . . . ? Dy2 O5 C20 O4 -14.3(7) . . . . ? Dy2 O5 C20 C21 163.5(6) . . . . ? Dy2 O4 C20 O5 14.7(7) . . . . ? Dy2 O4 C20 C21 -163.2(5) . . . . ? O10 Dy2 C20 O5 95.5(4) . . . . ? O1 Dy2 C20 O5 -57.5(4) . . . . ? O8 Dy2 C20 O5 94.7(11) . . . . ? O4 Dy2 C20 O5 -165.7(7) . . . . ? O6 Dy2 C20 O5 -129.2(4) . . . . ? O7 Dy2 C20 O5 175.8(4) . . . . ? N1 Dy2 C20 O5 15.6(5) . . . . ? C27 Dy2 C20 O5 -156.6(4) . . . . ? O10 Dy2 C20 O4 -98.8(4) . . . . ? O1 Dy2 C20 O4 108.2(4) . . . . ? O8 Dy2 C20 O4 -99.6(11) . . . . ? O6 Dy2 C20 O4 36.6(4) . . . . ? O7 Dy2 C20 O4 -18.5(4) . . . . ? O5 Dy2 C20 O4 165.7(7) . . . . ? N1 Dy2 C20 O4 -178.7(4) . . . . ? C27 Dy2 C20 O4 9.1(5) . . . . ? O10 Dy2 C20 C21 -10(2) . . . . ? O1 Dy2 C20 C21 -163(2) . . . . ? O8 Dy2 C20 C21 -11(3) . . . . ? O4 Dy2 C20 C21 88(2) . . . . ? O6 Dy2 C20 C21 125(2) . . . . ? O7 Dy2 C20 C21 70(2) . . . . ? O5 Dy2 C20 C21 -106(2) . . . . ? N1 Dy2 C20 C21 -90(2) . . . . ? C27 Dy2 C20 C21 97(2) . . . . ? O5 C20 C21 C22 -5.9(10) . . . . ? O4 C20 C21 C22 172.0(7) . . . . ? Dy2 C20 C21 C22 92(2) . . . . ? O5 C20 C21 C26 174.6(7) . . . . ? O4 C20 C21 C26 -7.5(10) . . . . ? Dy2 C20 C21 C26 -88(2) . . . . ? C26 C21 C22 C23 1.7(11) . . . . ? C20 C21 C22 C23 -177.8(7) . . . . ? C21 C22 C23 C24 -0.2(13) . . . . ? C22 C23 C24 C25 -1.6(14) . . . . ? C23 C24 C25 C26 1.7(14) . . . . ? C24 C25 C26 C21 -0.2(14) . . . . ? C22 C21 C26 C25 -1.6(12) . . . . ? C20 C21 C26 C25 177.9(7) . . . . ? Dy2 O6 C27 O7 0.4(7) . . . . ? Dy2 O6 C27 C28 -179.2(6) . . . . ? Dy2 O7 C27 O6 -0.4(7) . . . . ? Dy2 O7 C27 C28 179.2(6) . . . . ? O10 Dy2 C27 O6 175.6(4) . . . . ? O1 Dy2 C27 O6 -6.2(4) . . . . ? O8 Dy2 C27 O6 -97.9(4) . . . . ? O4 Dy2 C27 O6 98.0(4) . . . . ? O7 Dy2 C27 O6 179.6(7) . . . . ? O5 Dy2 C27 O6 80.4(5) . . . . ? N1 Dy2 C27 O6 -68.7(6) . . . . ? C20 Dy2 C27 O6 93.7(4) . . . . ? O10 Dy2 C27 O7 -3.9(5) . . . . ? O1 Dy2 C27 O7 174.3(4) . . . . ? O8 Dy2 C27 O7 82.6(4) . . . . ? O4 Dy2 C27 O7 -81.6(4) . . . . ? O6 Dy2 C27 O7 -179.6(7) . . . . ? O5 Dy2 C27 O7 -99.2(4) . . . . ? N1 Dy2 C27 O7 111.8(5) . . . . ? C20 Dy2 C27 O7 -85.8(4) . . . . ? O10 Dy2 C27 C28 -53(36) . . . . ? O1 Dy2 C27 C28 125(36) . . . . ? O8 Dy2 C27 C28 34(36) . . . . ? O4 Dy2 C27 C28 -131(36) . . . . ? O6 Dy2 C27 C28 132(36) . . . . ? O7 Dy2 C27 C28 -49(36) . . . . ? O5 Dy2 C27 C28 -148(36) . . . . ? N1 Dy2 C27 C28 63(36) . . . . ? C20 Dy2 C27 C28 -135(36) . . . . ? O6 C27 C28 C33 -163.2(7) . . . . ? O7 C27 C28 C33 17.2(11) . . . . ? Dy2 C27 C28 C33 66(36) . . . . ? O6 C27 C28 C29 16.9(11) . . . . ? O7 C27 C28 C29 -162.7(7) . . . . ? Dy2 C27 C28 C29 -114(36) . . . . ? C33 C28 C29 C30 1.1(13) . . . . ? C27 C28 C29 C30 -179.0(8) . . . . ? C28 C29 C30 C31 1.3(15) . . . . ? C29 C30 C31 C32 -1.9(16) . . . . ? C30 C31 C32 C33 0.1(15) . . . . ? C31 C32 C33 C28 2.3(14) . . . . ? C29 C28 C33 C32 -2.8(13) . . . . ? C27 C28 C33 C32 177.3(8) . . . . ? Dy1 O11 C34 O10 -48.7(15) . . . . ? Dy1 O11 C34 C35 132.0(8) . . . . ? Dy2 O10 C34 O11 9(2) . . . . ? Dy2 O10 C34 C35 -171.2(10) . . . . ? O11 C34 C35 C40 -19.3(11) . . . . ? O10 C34 C35 C40 161.4(7) . . . . ? O11 C34 C35 C36 162.6(7) . . . . ? O10 C34 C35 C36 -16.8(11) . . . . ? C40 C35 C36 C37 1.3(12) . . . . ? C34 C35 C36 C37 179.4(7) . . . . ? C35 C36 C37 C38 -2.2(13) . . . . ? C36 C37 C38 C39 1.0(14) . . . . ? C37 C38 C39 C40 1.1(14) . . . . ? C36 C35 C40 C39 0.9(12) . . . . ? C34 C35 C40 C39 -177.3(7) . . . . ? C38 C39 C40 C35 -2.1(13) . . . . ? Dy2 O8 C41 O9 -74.4(13) . . . . ? Dy2 O8 C41 C42 108.3(10) . . . . ? Dy1 O9 C41 O8 -11.1(14) . . . . ? Dy1 O9 C41 C42 166.2(6) . . . . ? O8 C41 C42 C43 -10.6(11) . . . . ? O9 C41 C42 C43 171.9(7) . . . . ? O8 C41 C42 C47 167.8(7) . . . . ? O9 C41 C42 C47 -9.7(11) . . . . ? C47 C42 C43 C44 0.0(13) . . . . ? C41 C42 C43 C44 178.5(8) . . . . ? C42 C43 C44 C45 -1.3(16) . . . . ? C43 C44 C45 C46 1.4(17) . . . . ? C44 C45 C46 C47 -0.3(16) . . . . ? C43 C42 C47 C46 1.0(12) . . . . ? C41 C42 C47 C46 -177.4(8) . . . . ? C45 C46 C47 C42 -0.9(14) . . . . ? Dy1 O14 C48 O17 64(3) . . . 2_645 ? Dy1 O14 C48 C49 -118(3) . . . . ? O14 C48 C49 C54 -173.7(8) . . . . ? O17 C48 C49 C54 4.7(11) 2_645 . . . ? O14 C48 C49 C50 5.4(12) . . . . ? O17 C48 C49 C50 -176.2(7) 2_645 . . . ? C54 C49 C50 C51 -0.1(12) . . . . ? C48 C49 C50 C51 -179.1(8) . . . . ? C49 C50 C51 C52 -0.8(13) . . . . ? C50 C51 C52 C53 -0.1(14) . . . . ? C51 C52 C53 C54 1.9(14) . . . . ? C50 C49 C54 C53 1.9(12) . . . . ? C48 C49 C54 C53 -179.1(7) . . . . ? C52 C53 C54 C49 -2.7(13) . . . . ? Dy1 O12 C55 O13 1.4(7) . . . . ? Dy1 O12 C55 C56 -178.2(6) . . . . ? Dy1 O13 C55 O12 -1.3(7) . . . . ? Dy1 O13 C55 C56 178.3(6) . . . . ? O11 Dy1 C55 O12 -87.2(4) . . . . ? O14 Dy1 C55 O12 94.7(5) . . . . ? O9 Dy1 C55 O12 10.2(5) . . . . ? O17 Dy1 C55 O12 -163.9(4) . . . . ? O16 Dy1 C55 O12 -72.8(6) . . . . ? O15 Dy1 C55 O12 106.2(5) . . . . ? O13 Dy1 C55 O12 178.6(7) . . . . ? O11 Dy1 C55 O13 94.1(4) . . . . ? O14 Dy1 C55 O13 -83.9(4) . . . . ? O9 Dy1 C55 O13 -168.5(4) . . . . ? O17 Dy1 C55 O13 17.5(5) . . . . ? O12 Dy1 C55 O13 -178.6(7) . . . . ? O16 Dy1 C55 O13 108.5(5) . . . . ? O15 Dy1 C55 O13 -72.4(6) . . . . ? O11 Dy1 C55 C56 -51(12) . . . . ? O14 Dy1 C55 C56 130(12) . . . . ? O9 Dy1 C55 C56 46(12) . . . . ? O17 Dy1 C55 C56 -128(12) . . . . ? O12 Dy1 C55 C56 36(12) . . . . ? O16 Dy1 C55 C56 -37(13) . . . . ? O15 Dy1 C55 C56 142(12) . . . . ? O13 Dy1 C55 C56 -146(13) . . . . ? O12 C55 C56 C57 1.7(11) . . . . ? O13 C55 C56 C57 -177.9(7) . . . . ? Dy1 C55 C56 C57 -33(13) . . . . ? O12 C55 C56 C61 -178.9(8) . . . . ? O13 C55 C56 C61 1.5(12) . . . . ? Dy1 C55 C56 C61 146(12) . . . . ? C61 C56 C57 C58 -1.0(12) . . . . ? C55 C56 C57 C58 178.4(7) . . . . ? C56 C57 C58 C59 1.0(13) . . . . ? C57 C58 C59 C60 -0.3(14) . . . . ? C58 C59 C60 C61 -0.4(15) . . . . ? C59 C60 C61 C56 0.5(15) . . . . ? C57 C56 C61 C60 0.2(14) . . . . ? C55 C56 C61 C60 -179.2(9) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.11 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.959 _refine_diff_density_min -1.042 _refine_diff_density_rms 0.161 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 836163' #TrackingRef '- Ln4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C126 H112 Gd4 N4 O34' _chemical_formula_weight 2855.20 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' Gd Gd -0.1653 3.9035 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.3896(11) _cell_length_b 15.6333(12) _cell_length_c 15.922(2) _cell_angle_alpha 111.269(2) _cell_angle_beta 97.9220(10) _cell_angle_gamma 118.3440(10) _cell_volume 2908.7(5) _cell_formula_units_Z 1 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 5027 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 25.98 _exptl_crystal_description stick _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 2.334 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7209 _exptl_absorpt_correction_T_max 0.8174 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16051 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0994 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 26.06 _reflns_number_total 11293 _reflns_number_gt 7268 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 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^)+(0.0360P)^2^+0.0035P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11293 _refine_ls_number_parameters 760 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0922 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1129 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.019 _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 Gd1 Gd 0.40805(3) 1.29812(3) 0.39318(3) 0.02776(11) Uani 1 1 d . . . Gd2 Gd 0.23742(3) 0.87605(3) 0.18757(2) 0.02387(10) Uani 1 1 d . . . N1 N 0.1485(4) 0.8760(5) 0.0392(4) 0.0276(13) Uani 1 1 d . . . N2 N -0.0310(4) 0.5716(5) 0.1574(4) 0.0293(14) Uani 1 1 d . . . O1 O 0.0697(3) 0.7182(4) 0.1046(3) 0.0274(11) Uani 1 1 d . . . H1 H 0.0429 0.6962 0.1488 0.033 Uiso 1 1 calc R . . O2 O -0.2199(4) 0.5118(5) 0.2025(4) 0.0506(15) Uani 1 1 d . . . O3 O 0.0596(4) 0.9771(5) -0.0510(4) 0.0524(16) Uani 1 1 d . . . O4 O 0.2754(4) 0.7746(4) 0.0542(3) 0.0356(12) Uani 1 1 d . . . O5 O 0.3550(4) 0.8155(4) 0.2020(3) 0.0334(12) Uani 1 1 d . . . O6 O 0.1789(3) 0.8027(4) 0.2970(3) 0.0305(12) Uani 1 1 d . . . O7 O 0.3326(4) 0.9660(4) 0.3639(3) 0.0329(12) Uani 1 1 d . . . O8 O 0.3830(4) 1.0254(4) 0.1988(4) 0.0388(13) Uani 1 1 d . . . O9 O 0.4438(4) 1.2044(4) 0.2696(4) 0.0391(13) Uani 1 1 d . . . O10 O 0.1764(4) 0.9846(4) 0.2530(3) 0.0394(13) Uani 1 1 d . . . O11 O 0.2470(4) 1.1517(4) 0.3756(4) 0.0425(14) Uani 1 1 d . . . O12 O 0.2862(4) 1.2537(5) 0.2452(3) 0.0394(13) Uani 1 1 d . . . O13 O 0.4454(4) 1.4102(4) 0.3069(4) 0.0383(13) Uani 1 1 d . . . O14 O 0.3533(4) 1.4131(5) 0.4538(4) 0.0509(15) Uani 1 1 d . . . O15 O 0.5935(4) 1.4120(5) 0.4631(4) 0.0459(14) Uani 1 1 d . . . O16 O 0.4428(5) 1.3618(5) 0.5708(4) 0.0528(15) Uani 1 1 d . . . H16A H 0.4918 1.4399 0.6134 0.063 Uiso 1 1 calc R . . O17 O 0.4511(4) 1.1878(4) 0.4438(3) 0.0381(13) Uani 1 1 d . . . H17A H 0.3927 1.1141 0.4230 0.046 Uiso 1 1 calc R . . C1 C -0.0010(5) 0.6487(6) 0.0179(5) 0.0253(16) Uani 1 1 d . . . C2 C -0.0816(5) 0.5398(5) -0.0052(5) 0.0227(15) Uani 1 1 d . . . C3 C -0.1602(5) 0.4612(6) -0.1029(5) 0.0341(18) Uani 1 1 d . . . H3 H -0.2137 0.3876 -0.1182 0.041 Uiso 1 1 calc R . . C4 C -0.1590(6) 0.4913(7) -0.1744(5) 0.0368(19) Uani 1 1 d . . . C5 C -0.0797(5) 0.5997(6) -0.1495(5) 0.0303(17) Uani 1 1 d . . . H5 H -0.0797 0.6210 -0.1983 0.036 Uiso 1 1 calc R . . C6 C -0.0006(5) 0.6784(6) -0.0574(5) 0.0265(16) Uani 1 1 d . . . C7 C -0.0929(5) 0.5066(6) 0.0674(5) 0.0284(16) Uani 1 1 d . . . H7 H -0.1493 0.4324 0.0479 0.034 Uiso 1 1 calc R . . C8 C -0.0501(6) 0.5362(7) 0.2299(5) 0.042(2) Uani 1 1 d . . . H8A H 0.0188 0.5763 0.2837 0.050 Uiso 1 1 calc R . . H8B H -0.0807 0.4554 0.1997 0.050 Uiso 1 1 calc R . . C9 C -0.1233(6) 0.5573(7) 0.2703(5) 0.0375(19) Uani 1 1 d . . . C10 C -0.2223(7) 0.5890(8) 0.3498(7) 0.057(3) Uani 1 1 d D . . H10 H -0.2446 0.6135 0.4009 0.068 Uiso 1 1 calc R . . C11 C -0.2789(7) 0.5328(9) 0.2549(7) 0.063(3) Uani 1 1 d . . . H11 H -0.3499 0.5101 0.2268 0.075 Uiso 1 1 calc R . . C12 C -0.1243(7) 0.6049(7) 0.3597(6) 0.048(2) Uani 1 1 d DU . . H12 H -0.0668 0.6431 0.4197 0.058 Uiso 1 1 calc R . . C13 C -0.2451(6) 0.4069(7) -0.2755(5) 0.052(2) Uani 1 1 d . . . H13A H -0.2121 0.4048 -0.3240 0.078 Uiso 1 1 calc R . . H13B H -0.2940 0.4285 -0.2869 0.078 Uiso 1 1 calc R . . H13C H -0.2847 0.3330 -0.2809 0.078 Uiso 1 1 calc R . . C14 C 0.0695(5) 0.7911(6) -0.0396(5) 0.0289(17) Uani 1 1 d . . . H14 H 0.0555 0.8039 -0.0924 0.035 Uiso 1 1 calc R . . C15 C 0.2039(5) 0.9863(6) 0.0433(5) 0.0327(17) Uani 1 1 d . . . H15A H 0.2073 1.0405 0.1027 0.039 Uiso 1 1 calc R . . H15B H 0.2782 1.0112 0.0503 0.039 Uiso 1 1 calc R . . C16 C 0.1561(6) 0.9907(6) -0.0407(5) 0.0327(18) Uani 1 1 d . . . C17 C 0.1008(6) 0.9980(7) -0.1731(6) 0.045(2) Uani 1 1 d . . . H17 H 0.0978 1.0041 -0.2305 0.054 Uiso 1 1 calc R . . C18 C 0.0304(8) 0.9837(9) -0.1315(6) 0.061(3) Uani 1 1 d . . . H18 H -0.0330 0.9786 -0.1551 0.073 Uiso 1 1 calc R . . C19 C 0.1823(6) 1.0024(7) -0.1135(6) 0.044(2) Uani 1 1 d . . . H19 H 0.2448 1.0120 -0.1241 0.053 Uiso 1 1 calc R . . C20 C 0.3475(5) 0.7867(6) 0.1142(5) 0.0300(17) Uani 1 1 d . . . C21 C 0.4278(5) 0.7676(6) 0.0840(5) 0.0327(17) Uani 1 1 d . . . C22 C 0.4318(6) 0.7518(7) -0.0057(6) 0.041(2) Uani 1 1 d . . . H22 H 0.3815 0.7493 -0.0501 0.049 Uiso 1 1 calc R . . C23 C 0.5093(7) 0.7394(8) -0.0313(6) 0.053(2) Uani 1 1 d . . . H23 H 0.5118 0.7283 -0.0935 0.064 Uiso 1 1 calc R . . C24 C 0.5830(6) 0.7431(7) 0.0332(7) 0.052(2) Uani 1 1 d . . . H24 H 0.6361 0.7348 0.0155 0.063 Uiso 1 1 calc R . . C25 C 0.5790(6) 0.7588(8) 0.1226(7) 0.054(2) Uani 1 1 d . . . H25 H 0.6295 0.7610 0.1666 0.065 Uiso 1 1 calc R . . C26 C 0.5030(6) 0.7714(7) 0.1497(6) 0.048(2) Uani 1 1 d . . . H26 H 0.5011 0.7825 0.2119 0.057 Uiso 1 1 calc R . . C27 C 0.2600(6) 0.8862(6) 0.3701(5) 0.0274(16) Uani 1 1 d . . . C28 C 0.2708(6) 0.8941(6) 0.4676(5) 0.0288(16) Uani 1 1 d . . . C29 C 0.1847(7) 0.8245(8) 0.4810(6) 0.053(2) Uani 1 1 d . . . H29 H 0.1170 0.7735 0.4289 0.064 Uiso 1 1 calc R . . C30 C 0.1956(7) 0.8281(8) 0.5704(6) 0.063(3) Uani 1 1 d . . . H30 H 0.1355 0.7791 0.5791 0.076 Uiso 1 1 calc R . . C31 C 0.2921(8) 0.9016(8) 0.6455(6) 0.057(3) Uani 1 1 d . . . H31 H 0.2988 0.9040 0.7066 0.068 Uiso 1 1 calc R . . C32 C 0.3784(7) 0.9713(8) 0.6341(6) 0.058(3) Uani 1 1 d . . . H32 H 0.4457 1.0222 0.6866 0.069 Uiso 1 1 calc R . . C33 C 0.3677(6) 0.9678(7) 0.5448(5) 0.048(2) Uani 1 1 d . . . H33 H 0.4283 1.0172 0.5368 0.058 Uiso 1 1 calc R . . C34 C 0.1743(5) 1.0512(6) 0.3221(5) 0.0257(16) Uani 1 1 d . . . C35 C 0.0743(5) 1.0087(6) 0.3437(5) 0.0295(17) Uani 1 1 d . . . C36 C -0.0047(6) 0.8961(7) 0.2957(6) 0.049(2) Uani 1 1 d . . . H36 H 0.0056 0.8457 0.2505 0.059 Uiso 1 1 calc R . . C37 C -0.0984(7) 0.8550(10) 0.3117(8) 0.077(4) Uani 1 1 d . . . H37 H -0.1509 0.7768 0.2793 0.093 Uiso 1 1 calc R . . C38 C -0.1155(8) 0.9259(13) 0.3736(9) 0.085(5) Uani 1 1 d . . . H38 H -0.1810 0.8981 0.3832 0.102 Uiso 1 1 calc R . . C39 C -0.0383(8) 1.0375(11) 0.4221(7) 0.067(3) Uani 1 1 d . . . H39 H -0.0503 1.0871 0.4661 0.081 Uiso 1 1 calc R . . C40 C 0.0579(6) 1.0805(8) 0.4085(6) 0.046(2) Uani 1 1 d . . . H40 H 0.1115 1.1584 0.4436 0.055 Uiso 1 1 calc R . . C41 C 0.4506(5) 1.1255(6) 0.2262(5) 0.0272(16) Uani 1 1 d . . . C42 C 0.5502(5) 1.1529(6) 0.2033(5) 0.0254(16) Uani 1 1 d . . . C43 C 0.5499(6) 1.0683(7) 0.1333(5) 0.0316(17) Uani 1 1 d . . . H43 H 0.4881 0.9939 0.0997 0.038 Uiso 1 1 calc R . . C44 C 0.6415(7) 1.0939(8) 0.1126(6) 0.049(2) Uani 1 1 d . . . H44 H 0.6422 1.0375 0.0633 0.059 Uiso 1 1 calc R . . C45 C 0.7311(7) 1.2020(9) 0.1644(7) 0.055(3) Uani 1 1 d . . . H45 H 0.7942 1.2192 0.1518 0.066 Uiso 1 1 calc R . . C46 C 0.7309(6) 1.2865(8) 0.2349(6) 0.044(2) Uani 1 1 d . . . H46 H 0.7932 1.3606 0.2702 0.053 Uiso 1 1 calc R . . C47 C 0.6391(5) 1.2614(6) 0.2530(5) 0.0318(17) Uani 1 1 d . . . H47 H 0.6372 1.3187 0.2995 0.038 Uiso 1 1 calc R . . C48 C 0.3366(5) 1.4869(7) 0.4800(5) 0.0275(16) Uani 1 1 d . . . C49 C 0.2234(5) 1.4515(6) 0.4429(5) 0.0260(16) Uani 1 1 d . . . C50 C 0.1431(5) 1.3410(7) 0.3750(5) 0.0369(19) Uani 1 1 d . . . H50 H 0.1610 1.2886 0.3523 0.044 Uiso 1 1 calc R . . C51 C 0.0390(6) 1.3055(8) 0.3400(6) 0.053(2) Uani 1 1 d . . . H51 H -0.0155 1.2297 0.2937 0.064 Uiso 1 1 calc R . . C52 C 0.0159(7) 1.3846(10) 0.3746(7) 0.058(3) Uani 1 1 d . . . H52 H -0.0559 1.3620 0.3519 0.070 Uiso 1 1 calc R . . C53 C 0.0942(7) 1.4943(9) 0.4407(6) 0.050(2) Uani 1 1 d . . . H53 H 0.0765 1.5470 0.4618 0.060 Uiso 1 1 calc R . . C54 C 0.1994(6) 1.5289(7) 0.4771(5) 0.0365(19) Uani 1 1 d . . . H54 H 0.2536 1.6043 0.5246 0.044 Uiso 1 1 calc R . . C55 C 0.3507(6) 1.3376(7) 0.2408(6) 0.0386(19) Uani 1 1 d . . . C56 C 0.3203(6) 1.3544(7) 0.1586(5) 0.039(2) Uani 1 1 d . . . C57 C 0.2205(6) 1.2736(7) 0.0843(5) 0.044(2) Uani 1 1 d . . . H57 H 0.1723 1.2094 0.0875 0.053 Uiso 1 1 calc R . . C58 C 0.1908(8) 1.2859(9) 0.0054(6) 0.058(3) Uani 1 1 d . . . H58 H 0.1224 1.2306 -0.0454 0.070 Uiso 1 1 calc R . . C59 C 0.2618(10) 1.3795(10) 0.0016(7) 0.071(3) Uani 1 1 d . . . H59 H 0.2418 1.3879 -0.0525 0.085 Uiso 1 1 calc R . . C60 C 0.3594(9) 1.4596(9) 0.0735(7) 0.067(3) Uani 1 1 d . . . H60 H 0.4072 1.5239 0.0702 0.080 Uiso 1 1 calc R . . C61 C 0.3887(8) 1.4468(8) 0.1516(7) 0.060(3) Uani 1 1 d . . . H61 H 0.4574 1.5027 0.2017 0.072 Uiso 1 1 calc R . . C62 C 0.4001(7) 1.2987(8) 0.6152(6) 0.060(3) Uani 1 1 d . . . H62A H 0.3485 1.2202 0.5654 0.090 Uiso 1 1 calc R . . H62B H 0.3642 1.3254 0.6525 0.090 Uiso 1 1 calc R . . H62C H 0.4574 1.3058 0.6592 0.090 Uiso 1 1 calc R . . C63 C 0.5499(6) 1.2189(8) 0.4990(7) 0.069(3) Uani 1 1 d . . . H63A H 0.5811 1.1918 0.4556 0.103 Uiso 1 1 calc R . . H63B H 0.5407 1.1864 0.5421 0.103 Uiso 1 1 calc R . . H63C H 0.5973 1.3004 0.5382 0.103 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01939(19) 0.0191(2) 0.0308(2) 0.00466(16) 0.00638(16) 0.00808(17) Gd2 0.0212(2) 0.0199(2) 0.0216(2) 0.00785(16) 0.00517(15) 0.00829(17) N1 0.029(3) 0.023(3) 0.035(4) 0.018(3) 0.010(3) 0.016(3) N2 0.032(3) 0.032(4) 0.019(3) 0.015(3) 0.009(3) 0.013(3) O1 0.026(3) 0.028(3) 0.017(2) 0.009(2) 0.007(2) 0.011(2) O2 0.044(4) 0.057(4) 0.041(3) 0.017(3) 0.015(3) 0.027(3) O3 0.049(4) 0.072(5) 0.063(4) 0.044(4) 0.028(3) 0.041(4) O4 0.029(3) 0.036(3) 0.034(3) 0.012(3) 0.004(2) 0.020(3) O5 0.031(3) 0.036(3) 0.034(3) 0.018(3) 0.012(2) 0.019(3) O6 0.022(3) 0.026(3) 0.024(3) 0.010(2) 0.001(2) 0.004(2) O7 0.034(3) 0.023(3) 0.022(3) 0.007(2) 0.003(2) 0.009(3) O8 0.028(3) 0.028(3) 0.051(3) 0.021(3) 0.010(3) 0.010(3) O9 0.042(3) 0.033(3) 0.046(3) 0.014(3) 0.023(3) 0.026(3) O10 0.063(4) 0.040(3) 0.033(3) 0.016(3) 0.022(3) 0.041(3) O11 0.022(3) 0.024(3) 0.048(4) 0.010(3) 0.004(2) 0.000(3) O12 0.033(3) 0.035(3) 0.036(3) 0.016(3) 0.005(2) 0.014(3) O13 0.031(3) 0.024(3) 0.042(3) 0.009(3) 0.003(2) 0.013(3) O14 0.045(3) 0.049(4) 0.046(4) 0.006(3) 0.008(3) 0.034(3) O15 0.025(3) 0.038(4) 0.054(4) 0.017(3) 0.001(3) 0.013(3) O16 0.078(4) 0.023(3) 0.040(3) 0.010(3) 0.020(3) 0.021(3) O17 0.025(3) 0.020(3) 0.044(3) 0.009(2) -0.002(2) 0.006(2) C1 0.021(4) 0.023(4) 0.026(4) 0.009(3) 0.008(3) 0.011(3) C2 0.013(3) 0.009(3) 0.035(4) 0.007(3) 0.013(3) 0.000(3) C3 0.030(4) 0.028(4) 0.030(4) 0.011(4) 0.006(3) 0.011(4) C4 0.029(4) 0.033(5) 0.030(4) 0.009(4) 0.005(3) 0.011(4) C5 0.030(4) 0.036(5) 0.023(4) 0.014(4) 0.010(3) 0.018(4) C6 0.020(4) 0.030(4) 0.019(4) 0.011(3) 0.001(3) 0.009(3) C7 0.027(4) 0.020(4) 0.044(5) 0.019(4) 0.018(4) 0.014(3) C8 0.047(5) 0.041(5) 0.038(5) 0.027(4) 0.015(4) 0.020(4) C9 0.033(4) 0.036(5) 0.035(5) 0.022(4) 0.012(4) 0.011(4) C10 0.062(6) 0.059(7) 0.060(6) 0.034(6) 0.037(5) 0.035(6) C11 0.051(6) 0.074(8) 0.079(8) 0.044(6) 0.039(6) 0.038(6) C12 0.053(5) 0.044(5) 0.039(5) 0.019(4) 0.022(4) 0.021(4) C13 0.052(6) 0.040(5) 0.030(5) 0.011(4) -0.003(4) 0.013(5) C14 0.032(4) 0.036(5) 0.032(4) 0.022(4) 0.019(4) 0.022(4) C15 0.031(4) 0.028(4) 0.031(4) 0.016(4) 0.009(3) 0.011(4) C16 0.034(4) 0.027(4) 0.044(5) 0.023(4) 0.020(4) 0.016(4) C17 0.048(5) 0.057(6) 0.038(5) 0.029(5) 0.009(4) 0.032(5) C18 0.070(7) 0.091(9) 0.056(6) 0.047(6) 0.023(5) 0.062(7) C19 0.046(5) 0.038(5) 0.051(5) 0.021(4) 0.017(4) 0.027(5) C20 0.024(4) 0.015(4) 0.037(5) 0.013(3) 0.009(3) 0.003(3) C21 0.027(4) 0.027(4) 0.035(4) 0.007(4) 0.005(3) 0.017(4) C22 0.028(4) 0.042(5) 0.042(5) 0.013(4) 0.009(4) 0.019(4) C23 0.053(6) 0.053(6) 0.062(6) 0.025(5) 0.031(5) 0.036(5) C24 0.041(5) 0.053(6) 0.065(6) 0.020(5) 0.024(5) 0.033(5) C25 0.039(5) 0.065(7) 0.064(6) 0.024(5) 0.012(5) 0.041(5) C26 0.044(5) 0.048(6) 0.044(5) 0.020(5) 0.012(4) 0.025(5) C27 0.030(4) 0.033(5) 0.031(4) 0.018(4) 0.016(3) 0.022(4) C28 0.034(4) 0.020(4) 0.027(4) 0.010(3) 0.008(3) 0.014(4) C29 0.041(5) 0.065(7) 0.031(5) 0.025(5) 0.009(4) 0.016(5) C30 0.041(5) 0.076(8) 0.045(6) 0.037(6) 0.020(5) 0.010(5) C31 0.077(7) 0.060(7) 0.024(5) 0.020(5) 0.011(5) 0.036(6) C32 0.058(6) 0.061(7) 0.029(5) 0.018(5) -0.004(4) 0.025(6) C33 0.047(5) 0.040(5) 0.035(5) 0.018(4) 0.005(4) 0.013(5) C34 0.023(4) 0.020(4) 0.024(4) 0.008(3) 0.000(3) 0.009(3) C35 0.020(4) 0.035(5) 0.030(4) 0.018(4) 0.005(3) 0.013(4) C36 0.032(5) 0.047(6) 0.058(6) 0.032(5) 0.006(4) 0.014(5) C37 0.034(6) 0.088(9) 0.103(9) 0.073(8) 0.015(6) 0.014(6) C38 0.039(6) 0.148(14) 0.101(10) 0.097(10) 0.039(7) 0.045(8) C39 0.070(7) 0.126(11) 0.054(6) 0.058(7) 0.039(6) 0.073(8) C40 0.047(5) 0.066(7) 0.040(5) 0.031(5) 0.021(4) 0.038(5) C41 0.022(4) 0.025(4) 0.027(4) 0.011(3) 0.003(3) 0.012(4) C42 0.021(4) 0.028(4) 0.025(4) 0.014(3) 0.004(3) 0.013(3) C43 0.046(5) 0.039(5) 0.017(4) 0.013(3) 0.012(3) 0.030(4) C44 0.058(6) 0.078(8) 0.036(5) 0.026(5) 0.026(5) 0.054(6) C45 0.036(5) 0.099(9) 0.065(6) 0.059(7) 0.033(5) 0.045(6) C46 0.025(4) 0.050(6) 0.053(5) 0.036(5) 0.015(4) 0.011(4) C47 0.026(4) 0.033(5) 0.030(4) 0.016(4) 0.009(3) 0.013(4) C48 0.029(4) 0.035(5) 0.025(4) 0.015(4) 0.016(3) 0.021(4) C49 0.024(4) 0.023(4) 0.024(4) 0.008(3) 0.007(3) 0.012(3) C50 0.025(4) 0.034(5) 0.034(4) 0.015(4) 0.007(3) 0.007(4) C51 0.037(5) 0.059(7) 0.032(5) 0.019(5) 0.004(4) 0.011(5) C52 0.025(5) 0.098(9) 0.055(6) 0.049(6) 0.017(4) 0.028(6) C53 0.054(6) 0.076(8) 0.054(6) 0.044(6) 0.034(5) 0.047(6) C54 0.040(5) 0.044(5) 0.033(4) 0.020(4) 0.018(4) 0.026(4) C55 0.039(5) 0.041(5) 0.044(5) 0.016(4) 0.018(4) 0.031(5) C56 0.054(5) 0.041(5) 0.030(4) 0.012(4) 0.012(4) 0.037(5) C57 0.043(5) 0.048(6) 0.040(5) 0.013(4) 0.011(4) 0.032(5) C58 0.065(7) 0.080(8) 0.053(6) 0.024(6) 0.020(5) 0.062(7) C59 0.108(10) 0.072(8) 0.057(7) 0.029(6) 0.031(7) 0.070(8) C60 0.103(9) 0.047(6) 0.048(6) 0.020(5) 0.024(6) 0.045(7) C61 0.077(7) 0.047(6) 0.053(6) 0.024(5) 0.019(5) 0.035(6) C62 0.067(7) 0.048(6) 0.057(6) 0.024(5) 0.030(5) 0.027(6) C63 0.040(6) 0.050(6) 0.089(8) 0.037(6) -0.006(5) 0.014(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O14 2.297(5) . ? Gd1 O9 2.301(5) . ? Gd1 O15 2.327(5) . ? Gd1 O11 2.327(5) . ? Gd1 O12 2.431(5) . ? Gd1 O17 2.451(5) . ? Gd1 O13 2.509(5) . ? Gd1 O16 2.512(5) . ? Gd1 C55 2.838(8) . ? Gd2 O8 2.263(5) . ? Gd2 O1 2.268(4) . ? Gd2 O10 2.312(5) . ? Gd2 O5 2.428(4) . ? Gd2 O7 2.460(4) . ? Gd2 O6 2.462(4) . ? Gd2 O4 2.479(5) . ? Gd2 N1 2.560(5) . ? Gd2 C20 2.792(7) . ? Gd2 C27 2.815(7) . ? N1 C14 1.286(8) . ? N1 C15 1.487(8) . ? N2 C7 1.282(8) . ? N2 C8 1.458(8) . ? O1 C1 1.283(7) . ? O1 H1 0.9500 . ? O2 C9 1.370(8) . ? O2 C11 1.386(9) . ? O3 C18 1.355(8) . ? O3 C16 1.373(8) . ? O4 C20 1.248(8) . ? O5 C20 1.274(7) . ? O6 C27 1.252(8) . ? O7 C27 1.268(8) . ? O8 C41 1.247(8) . ? O9 C41 1.238(8) . ? O10 C34 1.227(8) . ? O11 C34 1.243(8) . ? O12 C55 1.248(9) . ? O13 C55 1.288(9) . ? O14 C48 1.239(8) . ? O15 C48 1.247(9) 2_686 ? O16 C62 1.387(9) . ? O16 H16A 0.9500 . ? O17 C63 1.393(8) . ? O17 H17A 0.9500 . ? C1 C2 1.410(9) . ? C1 C6 1.433(8) . ? C2 C7 1.428(9) . ? C2 C3 1.441(9) . ? C3 C4 1.380(9) . ? C3 H3 0.9500 . ? C4 C5 1.391(10) . ? C4 C13 1.516(10) . ? C5 C6 1.388(9) . ? C5 H5 0.9500 . ? C6 C14 1.449(9) . ? C7 H7 0.9500 . ? C8 C9 1.480(10) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C12 1.351(10) . ? C10 C11 1.327(11) . ? C10 C12 1.382(10) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14 0.9500 . ? C15 C16 1.476(9) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C19 1.324(9) . ? C17 C18 1.319(10) . ? C17 C19 1.421(10) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.502(9) . ? C21 C22 1.374(9) . ? C21 C26 1.412(9) . ? C22 C23 1.386(10) . ? C22 H22 0.9500 . ? C23 C24 1.385(11) . ? C23 H23 0.9500 . ? C24 C25 1.370(10) . ? C24 H24 0.9500 . ? C25 C26 1.374(10) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.491(9) . ? C28 C29 1.364(10) . ? C28 C33 1.378(10) . ? C29 C30 1.387(10) . ? C29 H29 0.9500 . ? C30 C31 1.360(11) . ? C30 H30 0.9500 . ? C31 C32 1.349(11) . ? C31 H31 0.9500 . ? C32 C33 1.386(10) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.506(9) . ? C35 C40 1.374(10) . ? C35 C36 1.378(10) . ? C36 C37 1.377(11) . ? C36 H36 0.9500 . ? C37 C38 1.351(15) . ? C37 H37 0.9500 . ? C38 C39 1.361(15) . ? C38 H38 0.9500 . ? C39 C40 1.392(11) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.520(9) . ? C42 C47 1.379(9) . ? C42 C43 1.384(9) . ? C43 C44 1.394(9) . ? C43 H43 0.9500 . ? C44 C45 1.379(12) . ? C44 H44 0.9500 . ? C45 C46 1.390(12) . ? C45 H45 0.9500 . ? C46 C47 1.378(9) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 O15 1.247(9) 2_686 ? C48 C49 1.501(9) . ? C49 C54 1.377(9) . ? C49 C50 1.389(10) . ? C50 C51 1.368(10) . ? C50 H50 0.9500 . ? C51 C52 1.392(12) . ? C51 H51 0.9500 . ? C52 C53 1.371(13) . ? C52 H52 0.9500 . ? C53 C54 1.390(10) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.484(10) . ? C56 C61 1.383(11) . ? C56 C57 1.388(10) . ? C57 C58 1.388(11) . ? C57 H57 0.9500 . ? C58 C59 1.379(13) . ? C58 H58 0.9500 . ? C59 C60 1.355(13) . ? C59 H59 0.9500 . ? C60 C61 1.378(11) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O14 Gd1 O9 149.61(19) . . ? O14 Gd1 O15 105.8(2) . . ? O9 Gd1 O15 80.93(19) . . ? O14 Gd1 O11 88.0(2) . . ? O9 Gd1 O11 100.96(18) . . ? O15 Gd1 O11 149.53(18) . . ? O14 Gd1 O12 78.25(18) . . ? O9 Gd1 O12 75.31(17) . . ? O15 Gd1 O12 130.43(18) . . ? O11 Gd1 O12 78.40(18) . . ? O14 Gd1 O17 136.03(18) . . ? O9 Gd1 O17 74.21(17) . . ? O15 Gd1 O17 77.33(17) . . ? O11 Gd1 O17 74.07(17) . . ? O12 Gd1 O17 133.60(17) . . ? O14 Gd1 O13 73.92(18) . . ? O9 Gd1 O13 78.28(17) . . ? O15 Gd1 O13 80.10(17) . . ? O11 Gd1 O13 130.27(17) . . ? O12 Gd1 O13 52.95(16) . . ? O17 Gd1 O13 146.66(16) . . ? O14 Gd1 O16 68.90(18) . . ? O9 Gd1 O16 140.71(18) . . ? O15 Gd1 O16 77.94(19) . . ? O11 Gd1 O16 82.20(18) . . ? O12 Gd1 O16 142.20(18) . . ? O17 Gd1 O16 69.07(17) . . ? O13 Gd1 O16 129.07(17) . . ? O14 Gd1 C55 74.8(2) . . ? O9 Gd1 C55 74.88(19) . . ? O15 Gd1 C55 105.8(2) . . ? O11 Gd1 C55 104.0(2) . . ? O12 Gd1 C55 25.96(19) . . ? O17 Gd1 C55 147.96(19) . . ? O13 Gd1 C55 27.00(19) . . ? O16 Gd1 C55 143.0(2) . . ? O8 Gd2 O1 152.30(16) . . ? O8 Gd2 O10 90.11(18) . . ? O1 Gd2 O10 92.35(18) . . ? O8 Gd2 O5 83.36(17) . . ? O1 Gd2 O5 105.96(16) . . ? O10 Gd2 O5 152.07(17) . . ? O8 Gd2 O7 84.07(17) . . ? O1 Gd2 O7 123.33(15) . . ? O10 Gd2 O7 77.03(16) . . ? O5 Gd2 O7 75.30(16) . . ? O8 Gd2 O6 137.11(16) . . ? O1 Gd2 O6 70.54(15) . . ? O10 Gd2 O6 83.50(16) . . ? O5 Gd2 O6 83.02(15) . . ? O7 Gd2 O6 53.13(15) . . ? O8 Gd2 O4 81.72(17) . . ? O1 Gd2 O4 83.45(15) . . ? O10 Gd2 O4 152.44(16) . . ? O5 Gd2 O4 53.16(15) . . ? O7 Gd2 O4 127.64(15) . . ? O6 Gd2 O4 120.01(16) . . ? O8 Gd2 N1 82.16(17) . . ? O1 Gd2 N1 71.48(17) . . ? O10 Gd2 N1 77.63(17) . . ? O5 Gd2 N1 127.81(16) . . ? O7 Gd2 N1 151.02(17) . . ? O6 Gd2 N1 136.50(16) . . ? O4 Gd2 N1 75.22(16) . . ? O8 Gd2 C20 77.83(19) . . ? O1 Gd2 C20 98.46(18) . . ? O10 Gd2 C20 167.94(19) . . ? O5 Gd2 C20 27.12(16) . . ? O7 Gd2 C20 101.13(19) . . ? O6 Gd2 C20 105.09(18) . . ? O4 Gd2 C20 26.55(16) . . ? N1 Gd2 C20 100.70(19) . . ? O8 Gd2 C27 110.8(2) . . ? O1 Gd2 C27 96.74(19) . . ? O10 Gd2 C27 79.03(18) . . ? O5 Gd2 C27 78.04(17) . . ? O7 Gd2 C27 26.76(17) . . ? O6 Gd2 C27 26.37(18) . . ? O4 Gd2 C27 128.47(17) . . ? N1 Gd2 C27 153.26(18) . . ? C20 Gd2 C27 104.8(2) . . ? C14 N1 C15 118.0(6) . . ? C14 N1 Gd2 127.4(5) . . ? C15 N1 Gd2 114.3(4) . . ? C7 N2 C8 121.4(6) . . ? C1 O1 Gd2 141.0(4) . . ? C1 O1 H1 109.5 . . ? Gd2 O1 H1 109.5 . . ? C9 O2 C11 105.9(6) . . ? C18 O3 C16 106.2(6) . . ? C20 O4 Gd2 90.9(4) . . ? C20 O5 Gd2 92.6(4) . . ? C27 O6 Gd2 92.8(4) . . ? C27 O7 Gd2 92.4(4) . . ? C41 O8 Gd2 157.8(5) . . ? C41 O9 Gd1 149.4(5) . . ? C34 O10 Gd2 152.1(5) . . ? C34 O11 Gd1 144.1(5) . . ? C55 O12 Gd1 95.5(4) . . ? C55 O13 Gd1 90.9(5) . . ? C48 O14 Gd1 167.9(5) . . ? C48 O15 Gd1 136.3(5) 2_686 . ? C62 O16 Gd1 128.9(5) . . ? C62 O16 H16A 115.6 . . ? Gd1 O16 H16A 115.6 . . ? C63 O17 Gd1 128.5(5) . . ? C63 O17 H17A 115.7 . . ? Gd1 O17 H17A 115.7 . . ? O1 C1 C2 119.7(6) . . ? O1 C1 C6 121.8(6) . . ? C2 C1 C6 118.5(6) . . ? C1 C2 C7 121.9(6) . . ? C1 C2 C3 119.8(6) . . ? C7 C2 C3 118.2(6) . . ? C4 C3 C2 121.0(7) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 118.1(7) . . ? C3 C4 C13 119.3(7) . . ? C5 C4 C13 122.6(7) . . ? C6 C5 C4 123.6(7) . . ? C6 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? C5 C6 C1 119.0(7) . . ? C5 C6 C14 117.1(6) . . ? C1 C6 C14 123.3(6) . . ? N2 C7 C2 123.4(7) . . ? N2 C7 H7 118.3 . . ? C2 C7 H7 118.3 . . ? N2 C8 C9 112.9(6) . . ? N2 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? N2 C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C12 C9 O2 108.1(7) . . ? C12 C9 C8 136.8(7) . . ? O2 C9 C8 115.0(7) . . ? C11 C10 C12 106.4(8) . . ? C11 C10 H10 126.8 . . ? C12 C10 H10 126.8 . . ? C10 C11 O2 110.5(8) . . ? C10 C11 H11 124.8 . . ? O2 C11 H11 124.8 . . ? C9 C12 C10 109.1(8) . . ? C9 C12 H12 125.4 . . ? C10 C12 H12 125.4 . . ? C4 C13 H13A 109.5 . . ? C4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 C6 127.5(6) . . ? N1 C14 H14 116.3 . . ? C6 C14 H14 116.3 . . ? C16 C15 N1 116.5(6) . . ? C16 C15 H15A 108.2 . . ? N1 C15 H15A 108.2 . . ? C16 C15 H15B 108.2 . . ? N1 C15 H15B 108.2 . . ? H15A C15 H15B 107.3 . . ? C19 C16 O3 108.8(7) . . ? C19 C16 C15 135.4(7) . . ? O3 C16 C15 115.8(6) . . ? C18 C17 C19 105.2(7) . . ? C18 C17 H17 127.4 . . ? C19 C17 H17 127.4 . . ? C17 C18 O3 111.6(7) . . ? C17 C18 H18 124.2 . . ? O3 C18 H18 124.2 . . ? C16 C19 C17 108.3(7) . . ? C16 C19 H19 125.9 . . ? C17 C19 H19 125.9 . . ? O4 C20 O5 121.1(6) . . ? O4 C20 C21 120.5(6) . . ? O5 C20 C21 118.5(6) . . ? O4 C20 Gd2 62.6(4) . . ? O5 C20 Gd2 60.3(3) . . ? C21 C20 Gd2 166.1(5) . . ? C22 C21 C26 119.6(7) . . ? C22 C21 C20 120.3(6) . . ? C26 C21 C20 120.1(7) . . ? C21 C22 C23 120.0(7) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.3(8) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 119.8(7) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 121.0(7) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C25 C26 C21 119.4(7) . . ? C25 C26 H26 120.3 . . ? C21 C26 H26 120.3 . . ? O6 C27 O7 121.7(6) . . ? O6 C27 C28 119.5(6) . . ? O7 C27 C28 118.8(6) . . ? O6 C27 Gd2 60.9(3) . . ? O7 C27 Gd2 60.8(3) . . ? C28 C27 Gd2 178.1(5) . . ? C29 C28 C33 118.4(7) . . ? C29 C28 C27 120.2(6) . . ? C33 C28 C27 121.4(7) . . ? C28 C29 C30 120.3(8) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C31 C30 C29 120.2(8) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C32 C31 C30 120.6(8) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C31 C32 C33 119.3(8) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C28 C33 C32 121.2(8) . . ? C28 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? O10 C34 O11 125.8(7) . . ? O10 C34 C35 117.7(6) . . ? O11 C34 C35 116.5(7) . . ? C40 C35 C36 118.6(7) . . ? C40 C35 C34 121.4(7) . . ? C36 C35 C34 120.0(7) . . ? C37 C36 C35 121.4(9) . . ? C37 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? C38 C37 C36 120.0(11) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 119.6(10) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C38 C39 C40 121.3(10) . . ? C38 C39 H39 119.3 . . ? C40 C39 H39 119.3 . . ? C35 C40 C39 119.2(9) . . ? C35 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? O9 C41 O8 126.1(7) . . ? O9 C41 C42 117.1(6) . . ? O8 C41 C42 116.8(7) . . ? C47 C42 C43 121.3(7) . . ? C47 C42 C41 119.3(7) . . ? C43 C42 C41 119.4(6) . . ? C42 C43 C44 119.1(8) . . ? C42 C43 H43 120.4 . . ? C44 C43 H43 120.4 . . ? C45 C44 C43 119.2(8) . . ? C45 C44 H44 120.4 . . ? C43 C44 H44 120.4 . . ? C44 C45 C46 121.3(7) . . ? C44 C45 H45 119.3 . . ? C46 C45 H45 119.3 . . ? C47 C46 C45 119.2(8) . . ? C47 C46 H46 120.4 . . ? C45 C46 H46 120.4 . . ? C46 C47 C42 119.8(8) . . ? C46 C47 H47 120.1 . . ? C42 C47 H47 120.1 . . ? O14 C48 O15 124.7(7) . 2_686 ? O14 C48 C49 117.6(7) . . ? O15 C48 C49 117.7(7) 2_686 . ? C54 C49 C50 120.2(7) . . ? C54 C49 C48 119.7(7) . . ? C50 C49 C48 120.1(7) . . ? C51 C50 C49 121.7(8) . . ? C51 C50 H50 119.1 . . ? C49 C50 H50 119.1 . . ? C50 C51 C52 117.5(8) . . ? C50 C51 H51 121.2 . . ? C52 C51 H51 121.2 . . ? C53 C52 C51 121.6(8) . . ? C53 C52 H52 119.2 . . ? C51 C52 H52 119.2 . . ? C52 C53 C54 120.3(9) . . ? C52 C53 H53 119.8 . . ? C54 C53 H53 119.8 . . ? C49 C54 C53 118.6(8) . . ? C49 C54 H54 120.7 . . ? C53 C54 H54 120.7 . . ? O12 C55 O13 120.6(7) . . ? O12 C55 C56 120.6(7) . . ? O13 C55 C56 118.8(8) . . ? O12 C55 Gd1 58.5(4) . . ? O13 C55 Gd1 62.1(4) . . ? C56 C55 Gd1 177.9(5) . . ? C61 C56 C57 118.2(8) . . ? C61 C56 C55 122.5(8) . . ? C57 C56 C55 119.2(8) . . ? C56 C57 C58 120.5(9) . . ? C56 C57 H57 119.7 . . ? C58 C57 H57 119.7 . . ? C59 C58 C57 119.1(9) . . ? C59 C58 H58 120.4 . . ? C57 C58 H58 120.4 . . ? C60 C59 C58 121.3(10) . . ? C60 C59 H59 119.3 . . ? C58 C59 H59 119.3 . . ? C59 C60 C61 119.3(10) . . ? C59 C60 H60 120.3 . . ? C61 C60 H60 120.3 . . ? C60 C61 C56 121.5(9) . . ? C60 C61 H61 119.3 . . ? C56 C61 H61 119.3 . . ? O16 C62 H62A 109.5 . . ? O16 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? O16 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? O17 C63 H63A 109.5 . . ? O17 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? O17 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O8 Gd2 N1 C14 148.9(6) . . . . ? O1 Gd2 N1 C14 -22.5(5) . . . . ? O10 Gd2 N1 C14 -119.3(6) . . . . ? O5 Gd2 N1 C14 73.6(6) . . . . ? O7 Gd2 N1 C14 -148.8(5) . . . . ? O6 Gd2 N1 C14 -52.8(6) . . . . ? O4 Gd2 N1 C14 65.4(5) . . . . ? C20 Gd2 N1 C14 72.9(6) . . . . ? C27 Gd2 N1 C14 -89.6(7) . . . . ? O8 Gd2 N1 C15 -24.2(4) . . . . ? O1 Gd2 N1 C15 164.4(5) . . . . ? O10 Gd2 N1 C15 67.6(4) . . . . ? O5 Gd2 N1 C15 -99.5(5) . . . . ? O7 Gd2 N1 C15 38.1(6) . . . . ? O6 Gd2 N1 C15 134.1(4) . . . . ? O4 Gd2 N1 C15 -107.7(5) . . . . ? C20 Gd2 N1 C15 -100.2(4) . . . . ? C27 Gd2 N1 C15 97.3(6) . . . . ? O8 Gd2 O1 C1 12.0(9) . . . . ? O10 Gd2 O1 C1 106.7(7) . . . . ? O5 Gd2 O1 C1 -94.7(7) . . . . ? O7 Gd2 O1 C1 -177.3(6) . . . . ? O6 Gd2 O1 C1 -171.1(7) . . . . ? O4 Gd2 O1 C1 -46.0(7) . . . . ? N1 Gd2 O1 C1 30.6(6) . . . . ? C20 Gd2 O1 C1 -68.0(7) . . . . ? C27 Gd2 O1 C1 -174.1(7) . . . . ? O8 Gd2 O4 C20 79.3(4) . . . . ? O1 Gd2 O4 C20 -124.1(4) . . . . ? O10 Gd2 O4 C20 153.4(4) . . . . ? O5 Gd2 O4 C20 -8.6(4) . . . . ? O7 Gd2 O4 C20 3.5(5) . . . . ? O6 Gd2 O4 C20 -61.1(4) . . . . ? N1 Gd2 O4 C20 163.3(4) . . . . ? C27 Gd2 O4 C20 -30.7(5) . . . . ? O8 Gd2 O5 C20 -76.2(4) . . . . ? O1 Gd2 O5 C20 77.1(4) . . . . ? O10 Gd2 O5 C20 -153.8(4) . . . . ? O7 Gd2 O5 C20 -161.8(4) . . . . ? O6 Gd2 O5 C20 144.5(4) . . . . ? O4 Gd2 O5 C20 8.4(4) . . . . ? N1 Gd2 O5 C20 -1.6(5) . . . . ? C27 Gd2 O5 C20 170.8(4) . . . . ? O8 Gd2 O6 C27 4.7(5) . . . . ? O1 Gd2 O6 C27 -173.2(4) . . . . ? O10 Gd2 O6 C27 -78.4(4) . . . . ? O5 Gd2 O6 C27 77.1(4) . . . . ? O7 Gd2 O6 C27 0.3(4) . . . . ? O4 Gd2 O6 C27 116.9(4) . . . . ? N1 Gd2 O6 C27 -142.7(4) . . . . ? C20 Gd2 O6 C27 93.0(4) . . . . ? O8 Gd2 O7 C27 -177.2(4) . . . . ? O1 Gd2 O7 C27 7.1(4) . . . . ? O10 Gd2 O7 C27 91.3(4) . . . . ? O5 Gd2 O7 C27 -92.5(4) . . . . ? O6 Gd2 O7 C27 -0.3(4) . . . . ? O4 Gd2 O7 C27 -102.4(4) . . . . ? N1 Gd2 O7 C27 120.9(4) . . . . ? C20 Gd2 O7 C27 -100.9(4) . . . . ? O1 Gd2 O8 C41 111.6(12) . . . . ? O10 Gd2 O8 C41 16.3(12) . . . . ? O5 Gd2 O8 C41 -136.5(12) . . . . ? O7 Gd2 O8 C41 -60.6(12) . . . . ? O6 Gd2 O8 C41 -64.2(13) . . . . ? O4 Gd2 O8 C41 169.9(12) . . . . ? N1 Gd2 O8 C41 93.8(12) . . . . ? C20 Gd2 O8 C41 -163.4(12) . . . . ? C27 Gd2 O8 C41 -62.0(12) . . . . ? O14 Gd1 O9 C41 -153.3(8) . . . . ? O15 Gd1 O9 C41 101.0(9) . . . . ? O11 Gd1 O9 C41 -48.1(9) . . . . ? O12 Gd1 O9 C41 -122.9(9) . . . . ? O17 Gd1 O9 C41 21.7(9) . . . . ? O13 Gd1 O9 C41 -177.3(9) . . . . ? O16 Gd1 O9 C41 42.9(10) . . . . ? C55 Gd1 O9 C41 -149.8(9) . . . . ? O8 Gd2 O10 C34 -83.4(11) . . . . ? O1 Gd2 O10 C34 124.2(11) . . . . ? O5 Gd2 O10 C34 -7.5(13) . . . . ? O7 Gd2 O10 C34 0.5(10) . . . . ? O6 Gd2 O10 C34 54.1(11) . . . . ? O4 Gd2 O10 C34 -155.5(9) . . . . ? N1 Gd2 O10 C34 -165.4(11) . . . . ? C20 Gd2 O10 C34 -82.1(14) . . . . ? C27 Gd2 O10 C34 27.8(11) . . . . ? O14 Gd1 O11 C34 141.2(8) . . . . ? O9 Gd1 O11 C34 -9.5(8) . . . . ? O15 Gd1 O11 C34 -100.3(8) . . . . ? O12 Gd1 O11 C34 62.8(8) . . . . ? O17 Gd1 O11 C34 -79.5(8) . . . . ? O13 Gd1 O11 C34 74.3(9) . . . . ? O16 Gd1 O11 C34 -149.8(8) . . . . ? C55 Gd1 O11 C34 67.4(8) . . . . ? O14 Gd1 O12 C55 79.3(4) . . . . ? O9 Gd1 O12 C55 -85.5(4) . . . . ? O15 Gd1 O12 C55 -21.5(5) . . . . ? O11 Gd1 O12 C55 169.7(5) . . . . ? O17 Gd1 O12 C55 -135.9(4) . . . . ? O13 Gd1 O12 C55 0.7(4) . . . . ? O16 Gd1 O12 C55 109.1(5) . . . . ? O14 Gd1 O13 C55 -87.9(4) . . . . ? O9 Gd1 O13 C55 79.6(4) . . . . ? O15 Gd1 O13 C55 162.3(4) . . . . ? O11 Gd1 O13 C55 -14.9(5) . . . . ? O12 Gd1 O13 C55 -0.7(4) . . . . ? O17 Gd1 O13 C55 114.4(4) . . . . ? O16 Gd1 O13 C55 -132.2(4) . . . . ? O9 Gd1 O14 C48 -45(3) . . . . ? O15 Gd1 O14 C48 54(2) . . . . ? O11 Gd1 O14 C48 -154(2) . . . . ? O12 Gd1 O14 C48 -75(2) . . . . ? O17 Gd1 O14 C48 142(2) . . . . ? O13 Gd1 O14 C48 -21(2) . . . . ? O16 Gd1 O14 C48 124(2) . . . . ? C55 Gd1 O14 C48 -49(2) . . . . ? O14 Gd1 O15 C48 -1.3(7) . . . 2_686 ? O9 Gd1 O15 C48 148.3(7) . . . 2_686 ? O11 Gd1 O15 C48 -115.4(7) . . . 2_686 ? O12 Gd1 O15 C48 86.6(7) . . . 2_686 ? O17 Gd1 O15 C48 -135.9(7) . . . 2_686 ? O13 Gd1 O15 C48 68.8(7) . . . 2_686 ? O16 Gd1 O15 C48 -65.0(7) . . . 2_686 ? C55 Gd1 O15 C48 77.0(7) . . . 2_686 ? O14 Gd1 O16 C62 116.7(7) . . . . ? O9 Gd1 O16 C62 -72.0(7) . . . . ? O15 Gd1 O16 C62 -130.9(7) . . . . ? O11 Gd1 O16 C62 25.8(7) . . . . ? O12 Gd1 O16 C62 85.3(7) . . . . ? O17 Gd1 O16 C62 -50.0(6) . . . . ? O13 Gd1 O16 C62 162.6(6) . . . . ? C55 Gd1 O16 C62 128.7(7) . . . . ? O14 Gd1 O17 C63 -92.3(7) . . . . ? O9 Gd1 O17 C63 91.4(7) . . . . ? O15 Gd1 O17 C63 7.4(7) . . . . ? O11 Gd1 O17 C63 -162.0(7) . . . . ? O12 Gd1 O17 C63 142.1(6) . . . . ? O13 Gd1 O17 C63 55.9(8) . . . . ? O16 Gd1 O17 C63 -74.4(7) . . . . ? C55 Gd1 O17 C63 107.1(7) . . . . ? Gd2 O1 C1 C2 157.4(5) . . . . ? Gd2 O1 C1 C6 -22.4(10) . . . . ? O1 C1 C2 C7 5.6(10) . . . . ? C6 C1 C2 C7 -174.6(6) . . . . ? O1 C1 C2 C3 -179.2(6) . . . . ? C6 C1 C2 C3 0.6(9) . . . . ? C1 C2 C3 C4 -0.9(10) . . . . ? C7 C2 C3 C4 174.4(6) . . . . ? C2 C3 C4 C5 0.0(11) . . . . ? C2 C3 C4 C13 -178.4(7) . . . . ? C3 C4 C5 C6 1.4(11) . . . . ? C13 C4 C5 C6 179.6(7) . . . . ? C4 C5 C6 C1 -1.7(11) . . . . ? C4 C5 C6 C14 -173.5(7) . . . . ? O1 C1 C6 C5 -179.5(6) . . . . ? C2 C1 C6 C5 0.7(10) . . . . ? O1 C1 C6 C14 -8.2(10) . . . . ? C2 C1 C6 C14 171.9(6) . . . . ? C8 N2 C7 C2 175.8(6) . . . . ? C1 C2 C7 N2 -1.0(10) . . . . ? C3 C2 C7 N2 -176.2(6) . . . . ? C7 N2 C8 C9 -87.1(9) . . . . ? C11 O2 C9 C12 -0.8(9) . . . . ? C11 O2 C9 C8 175.1(7) . . . . ? N2 C8 C9 C12 -130.7(10) . . . . ? N2 C8 C9 O2 54.9(9) . . . . ? C12 C10 C11 O2 -0.1(11) . . . . ? C9 O2 C11 C10 0.6(10) . . . . ? O2 C9 C12 C10 0.8(10) . . . . ? C8 C9 C12 C10 -173.9(9) . . . . ? C11 C10 C12 C9 -0.4(11) . . . . ? C15 N1 C14 C6 -175.0(6) . . . . ? Gd2 N1 C14 C6 12.1(10) . . . . ? C5 C6 C14 N1 -178.8(6) . . . . ? C1 C6 C14 N1 9.8(11) . . . . ? C14 N1 C15 C16 6.0(9) . . . . ? Gd2 N1 C15 C16 179.8(5) . . . . ? C18 O3 C16 C19 -1.4(9) . . . . ? C18 O3 C16 C15 -179.9(7) . . . . ? N1 C15 C16 C19 -109.3(10) . . . . ? N1 C15 C16 O3 68.7(9) . . . . ? C19 C17 C18 O3 -0.8(11) . . . . ? C16 O3 C18 C17 1.4(11) . . . . ? O3 C16 C19 C17 0.9(10) . . . . ? C15 C16 C19 C17 179.0(9) . . . . ? C18 C17 C19 C16 -0.1(11) . . . . ? Gd2 O4 C20 O5 15.4(7) . . . . ? Gd2 O4 C20 C21 -164.5(6) . . . . ? Gd2 O5 C20 O4 -15.7(7) . . . . ? Gd2 O5 C20 C21 164.2(6) . . . . ? O8 Gd2 C20 O4 -95.8(4) . . . . ? O1 Gd2 C20 O4 56.2(4) . . . . ? O10 Gd2 C20 O4 -97.2(9) . . . . ? O5 Gd2 C20 O4 164.9(6) . . . . ? O7 Gd2 C20 O4 -177.2(4) . . . . ? O6 Gd2 C20 O4 128.3(4) . . . . ? N1 Gd2 C20 O4 -16.4(4) . . . . ? C27 Gd2 C20 O4 155.6(4) . . . . ? O8 Gd2 C20 O5 99.3(4) . . . . ? O1 Gd2 C20 O5 -108.6(4) . . . . ? O10 Gd2 C20 O5 97.9(9) . . . . ? O7 Gd2 C20 O5 17.9(4) . . . . ? O6 Gd2 C20 O5 -36.6(4) . . . . ? O4 Gd2 C20 O5 -164.9(6) . . . . ? N1 Gd2 C20 O5 178.8(4) . . . . ? C27 Gd2 C20 O5 -9.3(4) . . . . ? O8 Gd2 C20 C21 11(2) . . . . ? O1 Gd2 C20 C21 163(2) . . . . ? O10 Gd2 C20 C21 9(3) . . . . ? O5 Gd2 C20 C21 -89(2) . . . . ? O7 Gd2 C20 C21 -71(2) . . . . ? O6 Gd2 C20 C21 -125(2) . . . . ? O4 Gd2 C20 C21 106(2) . . . . ? N1 Gd2 C20 C21 90(2) . . . . ? C27 Gd2 C20 C21 -98(2) . . . . ? O4 C20 C21 C22 9.0(11) . . . . ? O5 C20 C21 C22 -170.9(7) . . . . ? Gd2 C20 C21 C22 -90(2) . . . . ? O4 C20 C21 C26 -174.1(7) . . . . ? O5 C20 C21 C26 6.0(11) . . . . ? Gd2 C20 C21 C26 87(2) . . . . ? C26 C21 C22 C23 0.1(12) . . . . ? C20 C21 C22 C23 177.0(8) . . . . ? C21 C22 C23 C24 -0.1(13) . . . . ? C22 C23 C24 C25 0.2(14) . . . . ? C23 C24 C25 C26 -0.2(14) . . . . ? C24 C25 C26 C21 0.2(14) . . . . ? C22 C21 C26 C25 -0.2(13) . . . . ? C20 C21 C26 C25 -177.1(8) . . . . ? Gd2 O6 C27 O7 -0.5(7) . . . . ? Gd2 O6 C27 C28 177.9(5) . . . . ? Gd2 O7 C27 O6 0.5(7) . . . . ? Gd2 O7 C27 C28 -177.9(5) . . . . ? O8 Gd2 C27 O6 -176.5(4) . . . . ? O1 Gd2 C27 O6 6.5(4) . . . . ? O10 Gd2 C27 O6 97.6(4) . . . . ? O5 Gd2 C27 O6 -98.5(4) . . . . ? O7 Gd2 C27 O6 -179.5(7) . . . . ? O4 Gd2 C27 O6 -80.5(4) . . . . ? N1 Gd2 C27 O6 68.0(6) . . . . ? C20 Gd2 C27 O6 -94.2(4) . . . . ? O8 Gd2 C27 O7 3.0(4) . . . . ? O1 Gd2 C27 O7 -174.0(4) . . . . ? O10 Gd2 C27 O7 -82.9(4) . . . . ? O5 Gd2 C27 O7 81.0(4) . . . . ? O6 Gd2 C27 O7 179.5(7) . . . . ? O4 Gd2 C27 O7 99.0(4) . . . . ? N1 Gd2 C27 O7 -112.5(5) . . . . ? C20 Gd2 C27 O7 85.4(4) . . . . ? O8 Gd2 C27 C28 82(17) . . . . ? O1 Gd2 C27 C28 -95(17) . . . . ? O10 Gd2 C27 C28 -4(17) . . . . ? O5 Gd2 C27 C28 160(17) . . . . ? O7 Gd2 C27 C28 79(17) . . . . ? O6 Gd2 C27 C28 -101(17) . . . . ? O4 Gd2 C27 C28 178(100) . . . . ? N1 Gd2 C27 C28 -33(17) . . . . ? C20 Gd2 C27 C28 165(17) . . . . ? O6 C27 C28 C29 -14.1(10) . . . . ? O7 C27 C28 C29 164.3(7) . . . . ? Gd2 C27 C28 C29 86(17) . . . . ? O6 C27 C28 C33 163.4(7) . . . . ? O7 C27 C28 C33 -18.2(10) . . . . ? Gd2 C27 C28 C33 -96(17) . . . . ? C33 C28 C29 C30 -0.5(13) . . . . ? C27 C28 C29 C30 177.0(8) . . . . ? C28 C29 C30 C31 0.5(15) . . . . ? C29 C30 C31 C32 -0.5(16) . . . . ? C30 C31 C32 C33 0.4(15) . . . . ? C29 C28 C33 C32 0.5(12) . . . . ? C27 C28 C33 C32 -177.0(7) . . . . ? C31 C32 C33 C28 -0.5(14) . . . . ? Gd2 O10 C34 O11 71.1(14) . . . . ? Gd2 O10 C34 C35 -110.2(10) . . . . ? Gd1 O11 C34 O10 11.6(13) . . . . ? Gd1 O11 C34 C35 -167.1(5) . . . . ? O10 C34 C35 C40 -168.9(7) . . . . ? O11 C34 C35 C40 10.0(10) . . . . ? O10 C34 C35 C36 8.9(10) . . . . ? O11 C34 C35 C36 -172.2(6) . . . . ? C40 C35 C36 C37 -0.2(11) . . . . ? C34 C35 C36 C37 -178.1(7) . . . . ? C35 C36 C37 C38 1.9(13) . . . . ? C36 C37 C38 C39 -2.1(15) . . . . ? C37 C38 C39 C40 0.7(15) . . . . ? C36 C35 C40 C39 -1.2(11) . . . . ? C34 C35 C40 C39 176.6(6) . . . . ? C38 C39 C40 C35 1.0(12) . . . . ? Gd1 O9 C41 O8 47.8(13) . . . . ? Gd1 O9 C41 C42 -132.7(7) . . . . ? Gd2 O8 C41 O9 -12.6(17) . . . . ? Gd2 O8 C41 C42 167.9(9) . . . . ? O9 C41 C42 C47 17.9(9) . . . . ? O8 C41 C42 C47 -162.5(6) . . . . ? O9 C41 C42 C43 -162.3(6) . . . . ? O8 C41 C42 C43 17.3(9) . . . . ? C47 C42 C43 C44 -0.2(10) . . . . ? C41 C42 C43 C44 -180.0(6) . . . . ? C42 C43 C44 C45 2.0(11) . . . . ? C43 C44 C45 C46 -1.9(12) . . . . ? C44 C45 C46 C47 -0.1(12) . . . . ? C45 C46 C47 C42 1.9(11) . . . . ? C43 C42 C47 C46 -1.8(10) . . . . ? C41 C42 C47 C46 178.0(6) . . . . ? Gd1 O14 C48 O15 -59(3) . . . 2_686 ? Gd1 O14 C48 C49 123(2) . . . . ? O14 C48 C49 C54 173.9(6) . . . . ? O15 C48 C49 C54 -4.3(10) 2_686 . . . ? O14 C48 C49 C50 -5.5(10) . . . . ? O15 C48 C49 C50 176.3(7) 2_686 . . . ? C54 C49 C50 C51 0.2(11) . . . . ? C48 C49 C50 C51 179.6(6) . . . . ? C49 C50 C51 C52 0.2(11) . . . . ? C50 C51 C52 C53 0.6(12) . . . . ? C51 C52 C53 C54 -1.8(13) . . . . ? C50 C49 C54 C53 -1.4(10) . . . . ? C48 C49 C54 C53 179.3(6) . . . . ? C52 C53 C54 C49 2.1(11) . . . . ? Gd1 O12 C55 O13 -1.3(7) . . . . ? Gd1 O12 C55 C56 177.8(6) . . . . ? Gd1 O13 C55 O12 1.3(7) . . . . ? Gd1 O13 C55 C56 -177.9(6) . . . . ? O14 Gd1 C55 O12 -94.4(4) . . . . ? O9 Gd1 C55 O12 87.4(4) . . . . ? O15 Gd1 C55 O12 163.2(4) . . . . ? O11 Gd1 C55 O12 -10.4(5) . . . . ? O17 Gd1 C55 O12 71.8(6) . . . . ? O13 Gd1 C55 O12 -178.7(7) . . . . ? O16 Gd1 C55 O12 -106.0(5) . . . . ? O14 Gd1 C55 O13 84.3(4) . . . . ? O9 Gd1 C55 O13 -93.8(4) . . . . ? O15 Gd1 C55 O13 -18.1(4) . . . . ? O11 Gd1 C55 O13 168.4(4) . . . . ? O12 Gd1 C55 O13 178.7(7) . . . . ? O17 Gd1 C55 O13 -109.4(5) . . . . ? O16 Gd1 C55 O13 72.8(5) . . . . ? O14 Gd1 C55 C56 -158(17) . . . . ? O9 Gd1 C55 C56 23(17) . . . . ? O15 Gd1 C55 C56 99(17) . . . . ? O11 Gd1 C55 C56 -74(17) . . . . ? O12 Gd1 C55 C56 -64(17) . . . . ? O17 Gd1 C55 C56 8(17) . . . . ? O13 Gd1 C55 C56 117(17) . . . . ? O16 Gd1 C55 C56 -170(16) . . . . ? O12 C55 C56 C61 179.1(7) . . . . ? O13 C55 C56 C61 -1.8(11) . . . . ? Gd1 C55 C56 C61 -118(16) . . . . ? O12 C55 C56 C57 -2.7(11) . . . . ? O13 C55 C56 C57 176.5(6) . . . . ? Gd1 C55 C56 C57 60(17) . . . . ? C61 C56 C57 C58 -0.2(11) . . . . ? C55 C56 C57 C58 -178.5(7) . . . . ? C56 C57 C58 C59 0.2(12) . . . . ? C57 C58 C59 C60 -0.4(14) . . . . ? C58 C59 C60 C61 0.6(15) . . . . ? C59 C60 C61 C56 -0.6(14) . . . . ? C57 C56 C61 C60 0.4(13) . . . . ? C55 C56 C61 C60 178.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.989 _refine_diff_density_min -0.929 _refine_diff_density_rms 0.148