# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Annie Powell' _publ_contact_author_email ANNIE.POWELL@KIT.EDU _publ_section_title ; Novel Mixed-Valent CoII2CoIII4LnIII4 Aggregates with Ligands Derived from tris-(hydroxymethyl) aminomethane (Tris) ; loop_ _publ_author_name 'Annie Powell' 'Christopher E. Anso' 'Yanhua Lan.' 'Huan-Yong Li.' 'Jiang Long.' ; Tong-Bu Lu ; 'Hua Xiang.' # Attachment 'hua_co6ln4.cif' data_hua416 _database_code_depnum_ccdc_archive 'CCDC 758590' #TrackingRef 'hua_co6ln4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H98 Co6 N12 O50 Y4, 2(N O3), 7(H2 O), 6(C H4 O)' _chemical_formula_sum 'C52 H136 Co6 N14 O69 Y4' _chemical_formula_weight 2770.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7727(14) _cell_length_b 13.6246(15) _cell_length_c 16.6712(18) _cell_angle_alpha 72.353(2) _cell_angle_beta 70.913(2) _cell_angle_gamma 72.982(2) _cell_volume 2551.6(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6811 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.98 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.803 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 3.310 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.393 _exptl_absorpt_correction_T_max 0.506 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker AXS Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19033 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.98 _reflns_number_total 11005 _reflns_number_gt 8185 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_data_reduction 'SAINT+ 6.45 (Bruker AXS Inc., 2003)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The nitrate counterion and the lattice solvent molecules showed two-fold disorder and were refined using partial isotropic atoms, with geometrical restraints as appropriate. ; _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^)+(0.0931P)^2^+5.6116P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11005 _refine_ls_number_parameters 639 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1634 _refine_ls_wR_factor_gt 0.1483 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.065 _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 Y1 Y 0.33928(4) 0.29491(4) 0.73666(3) 0.02203(14) Uani 1 1 d . . . Y2 Y 0.14262(4) 0.22325(4) 0.98100(3) 0.02447(14) Uani 1 1 d . . . Co1 Co 0.38852(6) 0.50056(5) 0.57865(5) 0.02146(17) Uani 1 1 d . . . Co2 Co 0.57208(6) 0.30129(5) 0.56541(5) 0.02187(17) Uani 1 1 d . . . Co3 Co 0.09847(6) 0.21090(5) 0.80236(5) 0.02309(17) Uani 1 1 d . . . N1 N 0.6151(4) 0.2230(3) 0.4751(3) 0.0276(10) Uani 1 1 d . . . H11 H 0.6562 0.2567 0.4228 0.033 Uiso 1 1 calc R . . H12 H 0.6545 0.1552 0.4916 0.033 Uiso 1 1 calc R . . C1 C 0.4974(5) 0.2265(4) 0.4728(4) 0.0273(12) Uani 1 1 d . . . C2 C 0.4415(5) 0.3449(4) 0.4512(4) 0.0260(11) Uani 1 1 d . . . H2C H 0.4604 0.3730 0.3872 0.031 Uiso 1 1 calc R . . H2D H 0.3580 0.3549 0.4733 0.031 Uiso 1 1 calc R . . O1 O 0.4830(3) 0.4006(3) 0.4918(2) 0.0224(8) Uani 1 1 d . . . C3 C 0.4410(5) 0.1743(4) 0.5655(4) 0.0296(12) Uani 1 1 d . . . H3C H 0.3586 0.1855 0.5730 0.035 Uiso 1 1 calc R . . H3D H 0.4733 0.0975 0.5772 0.035 Uiso 1 1 calc R . . O2 O 0.4599(3) 0.2193(3) 0.6250(2) 0.0249(8) Uani 1 1 d . . . C4 C 0.4969(5) 0.1684(5) 0.4078(4) 0.0363(14) Uani 1 1 d . . . H4C H 0.5222 0.0917 0.4301 0.044 Uiso 1 1 calc R . . H4D H 0.4181 0.1812 0.4039 0.044 Uiso 1 1 calc R . . O3 O 0.5654(4) 0.1981(4) 0.3247(3) 0.0478(12) Uani 1 1 d . . . H3 H 0.5262 0.2444 0.2935 0.072 Uiso 1 1 calc R . . N2 N 0.6721(4) 0.2281(3) 0.6416(3) 0.0286(10) Uani 1 1 d . . . H21 H 0.6364 0.1880 0.6929 0.034 Uiso 1 1 calc R . . H22 H 0.7373 0.1869 0.6146 0.034 Uiso 1 1 calc R . . C5 C 0.6944(5) 0.3240(4) 0.6551(4) 0.0293(12) Uani 1 1 d . . . C6 C 0.5760(5) 0.3894(4) 0.6920(4) 0.0291(12) Uani 1 1 d . . . H6A H 0.5516 0.3632 0.7560 0.035 Uiso 1 1 calc R . . H6B H 0.5797 0.4643 0.6796 0.035 Uiso 1 1 calc R . . O4 O 0.4962(3) 0.3806(3) 0.6528(2) 0.0230(8) Uani 1 1 d . . . C7 C 0.7471(5) 0.3817(4) 0.5636(4) 0.0305(12) Uani 1 1 d . . . H7A H 0.7476 0.4542 0.5636 0.037 Uiso 1 1 calc R . . H7B H 0.8263 0.3443 0.5426 0.037 Uiso 1 1 calc R . . O5 O 0.6813(3) 0.3849(3) 0.5082(2) 0.0242(8) Uani 1 1 d . . . C8 C 0.7697(5) 0.2954(5) 0.7172(4) 0.0391(15) Uani 1 1 d . . . H8A H 0.7712 0.3605 0.7313 0.047 Uiso 1 1 calc R . . H8B H 0.7364 0.2485 0.7723 0.047 Uiso 1 1 calc R . . O6 O 0.8824(4) 0.2444(4) 0.6816(3) 0.0484(12) Uani 1 1 d . . . H6 H 0.8818 0.1882 0.6710 0.073 Uiso 1 1 calc R . . N3 N 0.0675(4) 0.3144(4) 0.6999(3) 0.0277(10) Uani 1 1 d . . . H31 H 0.1248 0.3000 0.6517 0.033 Uiso 1 1 calc R . . H32 H 0.0009 0.3099 0.6926 0.033 Uiso 1 1 calc R . . C9 C 0.0580(5) 0.4246(4) 0.7064(4) 0.0294(12) Uani 1 1 d . . . C10 C 0.0700(5) 0.4175(4) 0.7973(4) 0.0281(12) Uani 1 1 d . . . H10A H 0.1018 0.4768 0.7946 0.034 Uiso 1 1 calc R . . H10B H -0.0057 0.4230 0.8395 0.034 Uiso 1 1 calc R . . O7 O 0.1427(3) 0.3197(3) 0.8259(2) 0.0245(8) Uani 1 1 d . . . C11 C 0.1521(5) 0.4712(4) 0.6332(4) 0.0300(12) Uani 1 1 d . . . H11A H 0.1411 0.4747 0.5763 0.036 Uiso 1 1 calc R . . H11B H 0.1453 0.5442 0.6366 0.036 Uiso 1 1 calc R . . O8 O 0.2620(3) 0.4128(3) 0.6370(2) 0.0245(8) Uani 1 1 d . . . C12 C -0.0585(3) 0.4913(3) 0.6976(3) 0.0390(15) Uani 1 1 d . . . H12A H -0.1173 0.4649 0.7492 0.047 Uiso 1 1 calc R . . H12B H -0.0621 0.5651 0.6971 0.047 Uiso 1 1 calc R . . O9 O -0.0834(3) 0.4898(3) 0.6210(3) 0.0552(13) Uani 1 1 d . . . H9 H -0.1480 0.5276 0.6191 0.083 Uiso 1 1 calc R . . N4 N 0.0796(4) 0.0893(4) 0.7755(3) 0.0286(10) Uani 1 1 d . . . H41 H 0.0114 0.0712 0.8074 0.034 Uiso 1 1 calc R . . H42 H 0.0869 0.0992 0.7170 0.034 Uiso 1 1 calc R . . C13 C 0.1773(5) 0.0110(4) 0.8038(4) 0.0300(13) Uani 1 1 d . . . C14 C 0.2807(5) 0.0576(4) 0.7488(4) 0.0348(14) Uani 1 1 d . . . H14A H 0.3451 0.0234 0.7754 0.042 Uiso 1 1 calc R . . H14B H 0.3036 0.0449 0.6894 0.042 Uiso 1 1 calc R . . O10 O 0.2523(3) 0.1684(3) 0.7441(3) 0.0257(8) Uani 1 1 d . . . C15 C 0.1557(5) 0.0117(4) 0.8992(4) 0.0308(13) Uani 1 1 d . . . H15A H 0.0913 -0.0220 0.9354 0.037 Uiso 1 1 calc R . . H15B H 0.2237 -0.0282 0.9202 0.037 Uiso 1 1 calc R . . O11 O 0.1304(3) 0.1179(3) 0.9057(2) 0.0270(8) Uani 1 1 d . . . C16 C 0.1894(5) -0.1001(4) 0.7931(4) 0.0353(14) Uani 1 1 d . . . H16A H 0.2519 -0.1489 0.8174 0.042 Uiso 1 1 calc R . . H16B H 0.1185 -0.1249 0.8269 0.042 Uiso 1 1 calc R . . O12 O 0.2117(4) -0.1033(3) 0.7050(3) 0.0417(11) Uani 1 1 d . . . H121 H 0.1936 -0.0420 0.6754 0.063 Uiso 1 1 calc R . . O13 O 0.3356(3) 0.5810(3) 0.6756(2) 0.0270(8) Uani 1 1 d . . . O14 O 0.3099(3) 0.4465(3) 0.7934(2) 0.0267(8) Uani 1 1 d . . . C17 C 0.3078(5) 0.5450(4) 0.7559(4) 0.0284(12) Uani 1 1 d . . . C18 C 0.2686(7) 0.6208(5) 0.8146(5) 0.054(2) Uani 1 1 d . . . H18A H 0.2958 0.6858 0.7828 0.081 Uiso 1 1 calc R . . H18B H 0.2989 0.5887 0.8658 0.081 Uiso 1 1 calc R . . H18C H 0.1855 0.6374 0.8334 0.081 Uiso 1 1 calc R . . O15 O 0.3262(3) 0.2233(3) 0.8933(3) 0.0283(8) Uani 1 1 d . . . O16 O 0.4932(3) 0.1873(3) 0.8040(3) 0.0374(10) Uani 1 1 d . . . C19 C 0.4341(5) 0.1856(5) 0.8804(4) 0.0339(13) Uani 1 1 d . . . C20 C 0.4854(6) 0.1453(8) 0.9558(5) 0.065(2) Uani 1 1 d . . . H20A H 0.5672 0.1424 0.9347 0.097 Uiso 1 1 calc R . . H20B H 0.4722 0.0745 0.9863 0.097 Uiso 1 1 calc R . . H20C H 0.4506 0.1926 0.9960 0.097 Uiso 1 1 calc R . . O17 O -0.0600(3) 0.2477(3) 0.8593(2) 0.0271(8) Uani 1 1 d . . . O18 O -0.0462(3) 0.2708(3) 0.9832(3) 0.0262(8) Uani 1 1 d . . . C21 C -0.1014(5) 0.2640(4) 0.9358(4) 0.0263(12) Uani 1 1 d . . . C22 C -0.2290(5) 0.2843(5) 0.9671(4) 0.0335(13) Uani 1 1 d . . . H22A H -0.2522 0.2710 1.0309 0.050 Uiso 1 1 calc R . . H22B H -0.2567 0.2372 0.9483 0.050 Uiso 1 1 calc R . . H22C H -0.2611 0.3577 0.9424 0.050 Uiso 1 1 calc R . . N5 N 0.1826(5) 0.0104(4) 1.0864(4) 0.0355(12) Uani 1 1 d . . . O19 O 0.2635(3) 0.0469(3) 1.0291(3) 0.0336(9) Uani 1 1 d . . . O20 O 0.0858(3) 0.0720(3) 1.0966(3) 0.0343(9) Uani 1 1 d . . . O21 O 0.1973(4) -0.0802(4) 1.1317(4) 0.0552(14) Uani 1 1 d . . . N6 N 0.1218(6) 0.2635(5) 1.1455(4) 0.0527(16) Uani 1 1 d . . . O22 O 0.0368(4) 0.2837(3) 1.1165(3) 0.0375(10) Uani 1 1 d . . . O23 O 0.2168(4) 0.2229(4) 1.0993(3) 0.0439(11) Uani 1 1 d . . . O24 O 0.1141(6) 0.2828(6) 1.2148(4) 0.084(2) Uani 1 1 d . . . O25 O 0.1614(4) 0.4012(3) 0.9550(3) 0.0336(10) Uani 1 1 d D . . H25 H 0.218(4) 0.418(5) 0.913(3) 0.040 Uiso 1 1 d D . . C23 C 0.1392(9) 0.4743(7) 1.0065(6) 0.078(3) Uani 1 1 d . . . H23A H 0.1610 0.5400 0.9690 0.116 Uiso 1 1 calc R . . H23B H 0.1832 0.4447 1.0500 0.116 Uiso 1 1 calc R . . H23C H 0.0582 0.4890 1.0361 0.116 Uiso 1 1 calc R . . O31 O 0.1515(6) 0.1544(4) 0.5692(4) 0.0763(18) Uani 1 1 d D . . N31A N 0.1303(9) 0.2454(9) 0.5031(7) 0.059(3) Uiso 0.62 1 d PD A 1 O32A O 0.0548(10) 0.3327(8) 0.5085(7) 0.085(3) Uiso 0.62 1 d PD A 1 O33A O 0.1865(16) 0.2344(14) 0.4207(9) 0.185(8) Uiso 0.62 1 d PD A 1 O34A O 0.2628(10) -0.0034(9) 0.4753(8) 0.085(3) Uiso 0.62 1 d P B 1 N31B N 0.1920(14) 0.0709(14) 0.5358(12) 0.064(5) Uiso 0.38 1 d PD A 2 O32B O 0.2947(10) 0.0187(10) 0.5129(8) 0.049(3) Uiso 0.38 1 d PD A 2 O33B O 0.1085(15) 0.0360(17) 0.5199(17) 0.129(8) Uiso 0.38 1 d PD A 2 O34B O 0.160(2) 0.3434(13) 0.4932(14) 0.110(7) Uiso 0.38 1 d PD C 2 O41A O 0.1067(12) -0.0709(11) 0.3704(9) 0.083(4) Uiso 0.50 1 d PD D 1 C41A C 0.149(3) 0.021(2) 0.3001(19) 0.134(12) Uiso 0.50 1 d PD D 1 O41B O 0.1110(19) -0.1418(17) 0.4876(14) 0.144(7) Uiso 0.50 1 d P E 2 O42A O 0.0757(17) -0.0996(14) 0.6058(13) 0.130(6) Uiso 0.50 1 d PD F 1 C42A C 0.0825(13) -0.2049(11) 0.5936(10) 0.050(4) Uiso 0.50 1 d PD F 1 O42B O 0.101(2) -0.224(2) 0.6609(19) 0.190(11) Uiso 0.50 1 d P G 2 O43 O 0.4657(10) 0.3703(10) 1.2133(7) 0.156(4) Uiso 1 1 d D . . H43 H 0.4916 0.4016 1.1617 0.234 Uiso 1 1 calc RD . . C43 C 0.3449(12) 0.3866(12) 1.2317(10) 0.132(5) Uiso 1 1 d D . . H43A H 0.3120 0.3725 1.2950 0.198 Uiso 1 1 calc R . . H43B H 0.3264 0.3387 1.2074 0.198 Uiso 1 1 calc R . . H43C H 0.3138 0.4597 1.2054 0.198 Uiso 1 1 calc R . . O44X O 0.5520(15) 0.5017(13) 1.0486(11) 0.113(5) Uiso 0.50 1 d PD H -1 C44X C 0.5457(17) 0.6080(14) 1.0474(13) 0.075(5) Uiso 0.50 1 d PD H -1 O45A O 0.391(2) -0.0094(18) 0.3152(14) 0.155(8) Uiso 0.50 1 d PD I 1 C45A C 0.4029(18) 0.0716(16) 0.2328(13) 0.077(5) Uiso 0.50 1 d PD I 1 O45B O 0.311(3) 0.108(3) 0.292(2) 0.234(14) Uiso 0.50 1 d P J 2 O46B O 0.509(3) 0.165(3) 0.188(2) 0.224(13) Uiso 0.50 1 d P K 2 O47B O 0.087(3) -0.001(3) 0.318(2) 0.186(11) Uiso 0.50 1 d P L 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 Y1 0.0210(3) 0.0152(2) 0.0288(3) -0.0083(2) 0.0018(2) -0.00823(19) Y2 0.0231(3) 0.0203(3) 0.0295(3) -0.0081(2) 0.0000(2) -0.0092(2) Co1 0.0209(4) 0.0153(3) 0.0272(4) -0.0070(3) 0.0002(3) -0.0076(3) Co2 0.0194(3) 0.0148(3) 0.0295(4) -0.0073(3) 0.0007(3) -0.0065(3) Co3 0.0216(4) 0.0184(3) 0.0293(4) -0.0100(3) 0.0019(3) -0.0093(3) N1 0.024(2) 0.018(2) 0.036(3) -0.0110(19) 0.004(2) -0.0062(18) C1 0.023(3) 0.024(3) 0.035(3) -0.013(2) 0.003(2) -0.011(2) C2 0.023(3) 0.024(3) 0.034(3) -0.012(2) -0.002(2) -0.009(2) O1 0.0228(18) 0.0183(17) 0.0273(19) -0.0069(14) -0.0017(15) -0.0098(15) C3 0.029(3) 0.023(3) 0.038(3) -0.014(2) 0.002(2) -0.011(2) O2 0.0240(19) 0.0177(18) 0.033(2) -0.0100(15) 0.0021(16) -0.0102(15) C4 0.039(3) 0.032(3) 0.044(4) -0.021(3) 0.001(3) -0.015(3) O3 0.048(3) 0.049(3) 0.048(3) -0.021(2) 0.004(2) -0.021(2) N2 0.024(2) 0.020(2) 0.037(3) -0.0027(19) -0.004(2) -0.0051(18) C5 0.028(3) 0.025(3) 0.036(3) -0.003(2) -0.009(2) -0.012(2) C6 0.031(3) 0.027(3) 0.031(3) -0.006(2) -0.005(2) -0.012(2) O4 0.0196(18) 0.0196(18) 0.030(2) -0.0078(15) -0.0021(15) -0.0075(14) C7 0.025(3) 0.026(3) 0.040(3) -0.003(2) -0.006(2) -0.012(2) O5 0.0233(19) 0.0194(18) 0.029(2) -0.0045(15) -0.0025(15) -0.0102(15) C8 0.039(4) 0.035(3) 0.041(4) 0.001(3) -0.011(3) -0.015(3) O6 0.040(3) 0.043(3) 0.068(3) -0.005(2) -0.024(2) -0.014(2) N3 0.028(2) 0.027(2) 0.030(2) -0.0099(19) -0.001(2) -0.012(2) C9 0.029(3) 0.022(3) 0.036(3) -0.007(2) -0.002(2) -0.011(2) C10 0.023(3) 0.022(3) 0.039(3) -0.012(2) 0.000(2) -0.009(2) O7 0.0251(19) 0.0152(17) 0.033(2) -0.0092(15) -0.0009(16) -0.0085(15) C11 0.026(3) 0.022(3) 0.040(3) -0.006(2) -0.003(2) -0.010(2) O8 0.0215(18) 0.0203(18) 0.029(2) -0.0055(15) 0.0012(15) -0.0098(15) C12 0.030(3) 0.041(4) 0.048(4) -0.008(3) -0.009(3) -0.013(3) O9 0.050(3) 0.047(3) 0.075(4) -0.008(3) -0.030(3) -0.011(2) N4 0.030(3) 0.027(2) 0.033(3) -0.014(2) 0.002(2) -0.016(2) C13 0.026(3) 0.021(3) 0.043(3) -0.014(2) 0.002(2) -0.010(2) C14 0.033(3) 0.020(3) 0.049(4) -0.017(3) 0.007(3) -0.012(2) O10 0.0196(18) 0.0182(18) 0.038(2) -0.0128(16) 0.0038(16) -0.0083(15) C15 0.031(3) 0.015(3) 0.045(3) -0.011(2) -0.003(3) -0.008(2) O11 0.029(2) 0.0163(18) 0.035(2) -0.0088(15) -0.0015(17) -0.0091(15) C16 0.034(3) 0.023(3) 0.048(4) -0.017(3) 0.004(3) -0.013(2) O12 0.056(3) 0.024(2) 0.049(3) -0.0143(19) -0.008(2) -0.013(2) O13 0.030(2) 0.0178(18) 0.031(2) -0.0096(16) 0.0033(16) -0.0110(16) O14 0.029(2) 0.0177(18) 0.034(2) -0.0098(15) 0.0005(16) -0.0124(15) C17 0.026(3) 0.020(3) 0.040(3) -0.015(2) 0.000(2) -0.007(2) C18 0.087(6) 0.030(3) 0.038(4) -0.016(3) 0.012(4) -0.026(4) O15 0.024(2) 0.025(2) 0.036(2) -0.0077(17) -0.0042(17) -0.0086(16) O16 0.025(2) 0.033(2) 0.039(2) 0.0008(18) 0.0031(18) -0.0043(17) C19 0.030(3) 0.026(3) 0.041(3) -0.003(3) -0.003(3) -0.011(2) C20 0.036(4) 0.095(7) 0.048(4) 0.012(4) -0.015(3) -0.016(4) O17 0.0232(19) 0.027(2) 0.033(2) -0.0122(16) 0.0001(16) -0.0111(16) O18 0.0246(19) 0.0203(18) 0.035(2) -0.0108(16) -0.0031(16) -0.0068(15) C21 0.025(3) 0.016(2) 0.034(3) -0.006(2) 0.003(2) -0.008(2) C22 0.027(3) 0.033(3) 0.039(3) -0.011(3) -0.001(2) -0.010(2) N5 0.038(3) 0.025(3) 0.045(3) -0.004(2) -0.011(2) -0.014(2) O19 0.026(2) 0.027(2) 0.043(2) 0.0003(18) -0.0062(18) -0.0115(17) O20 0.032(2) 0.033(2) 0.037(2) -0.0084(18) -0.0005(18) -0.0153(19) O21 0.059(3) 0.025(2) 0.070(3) 0.008(2) -0.010(3) -0.020(2) N6 0.062(4) 0.061(4) 0.045(4) -0.022(3) -0.008(3) -0.024(3) O22 0.038(2) 0.039(2) 0.038(2) -0.0163(19) -0.003(2) -0.012(2) O23 0.043(3) 0.044(3) 0.049(3) -0.015(2) -0.011(2) -0.013(2) O24 0.093(5) 0.118(6) 0.065(4) -0.057(4) -0.021(4) -0.021(4) O25 0.040(2) 0.025(2) 0.037(2) -0.0165(18) 0.0044(19) -0.0153(18) C23 0.117(8) 0.051(5) 0.054(5) -0.031(4) 0.022(5) -0.034(5) O31 0.097(5) 0.055(4) 0.073(4) -0.028(3) -0.009(4) -0.012(3) _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 Y1 O8 2.199(4) . ? Y1 O10 2.263(3) . ? Y1 O2 2.293(4) . ? Y1 O14 2.408(3) . ? Y1 O4 2.425(3) . ? Y1 O7 2.449(4) . ? Y1 O16 2.456(4) . ? Y1 O15 2.463(4) . ? Y2 O11 2.239(4) . ? Y2 O18 2.298(4) . ? Y2 O15 2.323(4) . ? Y2 O25 2.400(4) . ? Y2 O23 2.451(5) . ? Y2 O20 2.458(4) . ? Y2 O22 2.468(4) . ? Y2 O19 2.504(4) . ? Y2 O7 2.520(4) . ? Co1 O5 1.997(4) 2_666 ? Co1 O13 2.047(4) . ? Co1 O8 2.094(3) . ? Co1 O1 2.121(4) . ? Co1 O4 2.159(4) . ? Co1 O1 2.227(3) 2_666 ? Co2 O5 1.886(3) . ? Co2 O2 1.902(3) . ? Co2 O1 1.908(4) . ? Co2 O4 1.910(4) . ? Co2 N2 1.946(5) . ? Co2 N1 1.948(4) . ? Co3 O10 1.889(4) . ? Co3 O11 1.890(4) . ? Co3 O7 1.913(3) . ? Co3 O17 1.920(4) . ? Co3 N3 1.928(5) . ? Co3 N4 1.938(4) . ? N1 C1 1.503(7) . ? N1 H11 0.9200 . ? N1 H12 0.9200 . ? C1 C3 1.522(8) . ? C1 C4 1.526(8) . ? C1 C2 1.545(8) . ? C2 O1 1.447(6) . ? C2 H2C 0.9900 . ? C2 H2D 0.9900 . ? O1 Co1 2.227(3) 2_666 ? C3 O2 1.425(7) . ? C3 H3C 0.9900 . ? C3 H3D 0.9900 . ? C4 O3 1.386(7) . ? C4 H4C 0.9900 . ? C4 H4D 0.9900 . ? O3 H3 0.8400 . ? N2 C5 1.508(7) . ? N2 H21 0.9200 . ? N2 H22 0.9200 . ? C5 C7 1.520(8) . ? C5 C8 1.529(9) . ? C5 C6 1.547(8) . ? C6 O4 1.427(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O5 1.421(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? O5 Co1 1.997(4) 2_666 ? C8 O6 1.419(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? O6 H6 0.8400 . ? N3 C9 1.504(7) . ? N3 H31 0.9200 . ? N3 H32 0.9200 . ? C9 C12 1.528(7) . ? C9 C11 1.534(8) . ? C9 C10 1.544(8) . ? C10 O7 1.430(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O8 1.408(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O9 1.4208 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? O9 H9 0.8400 . ? N4 C13 1.490(8) . ? N4 H41 0.9200 . ? N4 H42 0.9200 . ? C13 C15 1.524(9) . ? C13 C14 1.528(7) . ? C13 C16 1.535(7) . ? C14 O10 1.429(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O11 1.417(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O12 1.413(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? O12 H121 0.8400 . ? O13 C17 1.246(7) . ? O14 C17 1.293(6) . ? C17 C18 1.505(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O15 C19 1.291(7) . ? O16 C19 1.249(7) . ? C19 C20 1.490(10) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? O17 C21 1.272(7) . ? O18 C21 1.255(7) . ? C21 C22 1.509(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? N5 O21 1.234(7) . ? N5 O19 1.263(6) . ? N5 O20 1.267(7) . ? N6 O24 1.229(8) . ? N6 O22 1.254(8) . ? N6 O23 1.275(8) . ? O25 C23 1.414(8) . ? O25 H25 0.86(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? O31 N31B 1.313(16) . ? O31 N31A 1.413(11) . ? N31A O32A 1.300(13) . ? N31A O33A 1.357(15) . ? N31B O32B 1.290(17) . ? N31B O33B 1.411(19) . ? O41A C41A 1.522(19) . ? O42A C42A 1.483(16) . ? O43 C43 1.433(13) . ? O43 H43 0.8400 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? O44X C44X 1.422(16) . ? O45A C45A 1.473(17) . ? 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 Y1 O10 94.75(14) . . ? O8 Y1 O2 86.42(14) . . ? O10 Y1 O2 78.20(12) . . ? O8 Y1 O14 82.80(13) . . ? O10 Y1 O14 141.81(13) . . ? O2 Y1 O14 139.14(12) . . ? O8 Y1 O4 80.08(13) . . ? O10 Y1 O4 143.99(12) . . ? O2 Y1 O4 65.97(12) . . ? O14 Y1 O4 73.37(12) . . ? O8 Y1 O7 82.43(13) . . ? O10 Y1 O7 67.27(12) . . ? O2 Y1 O7 142.50(12) . . ? O14 Y1 O7 74.65(12) . . ? O4 Y1 O7 145.10(11) . . ? O8 Y1 O16 156.54(13) . . ? O10 Y1 O16 100.38(14) . . ? O2 Y1 O16 79.33(14) . . ? O14 Y1 O16 95.86(15) . . ? O4 Y1 O16 77.13(13) . . ? O7 Y1 O16 119.95(13) . . ? O8 Y1 O15 146.66(13) . . ? O10 Y1 O15 87.56(13) . . ? O2 Y1 O15 126.39(13) . . ? O14 Y1 O15 75.29(13) . . ? O4 Y1 O15 116.11(12) . . ? O7 Y1 O15 67.82(13) . . ? O16 Y1 O15 52.67(13) . . ? O11 Y2 O18 77.55(13) . . ? O11 Y2 O15 87.46(13) . . ? O18 Y2 O15 145.00(14) . . ? O11 Y2 O25 138.04(14) . . ? O18 Y2 O25 94.19(14) . . ? O15 Y2 O25 76.10(14) . . ? O11 Y2 O23 142.67(15) . . ? O18 Y2 O23 124.51(15) . . ? O15 Y2 O23 85.99(15) . . ? O25 Y2 O23 75.17(15) . . ? O11 Y2 O20 77.46(14) . . ? O18 Y2 O20 83.60(14) . . ? O15 Y2 O20 124.05(14) . . ? O25 Y2 O20 143.20(14) . . ? O23 Y2 O20 76.08(15) . . ? O11 Y2 O22 138.46(14) . . ? O18 Y2 O22 72.61(14) . . ? O15 Y2 O22 132.78(14) . . ? O25 Y2 O22 73.16(14) . . ? O23 Y2 O22 52.04(16) . . ? O20 Y2 O22 71.15(14) . . ? O11 Y2 O19 73.93(14) . . ? O18 Y2 O19 130.62(13) . . ? O15 Y2 O19 72.58(13) . . ? O25 Y2 O19 133.36(14) . . ? O23 Y2 O19 69.04(15) . . ? O20 Y2 O19 51.48(13) . . ? O22 Y2 O19 104.93(15) . . ? O11 Y2 O7 68.62(12) . . ? O18 Y2 O7 76.29(13) . . ? O15 Y2 O7 68.79(13) . . ? O25 Y2 O7 69.46(13) . . ? O23 Y2 O7 140.33(14) . . ? O20 Y2 O7 143.43(13) . . ? O22 Y2 O7 128.62(14) . . ? O19 Y2 O7 126.33(13) . . ? O5 Co1 O13 96.87(15) 2_666 . ? O5 Co1 O8 100.94(15) 2_666 . ? O13 Co1 O8 93.45(14) . . ? O5 Co1 O1 95.87(15) 2_666 . ? O13 Co1 O1 164.33(16) . . ? O8 Co1 O1 93.04(14) . . ? O5 Co1 O4 168.30(14) 2_666 . ? O13 Co1 O4 88.65(15) . . ? O8 Co1 O4 88.97(14) . . ? O1 Co1 O4 77.22(14) . . ? O5 Co1 O1 74.97(14) 2_666 2_666 ? O13 Co1 O1 88.43(14) . 2_666 ? O8 Co1 O1 175.69(14) . 2_666 ? O1 Co1 O1 86.11(13) . 2_666 ? O4 Co1 O1 94.96(13) . 2_666 ? O5 Co2 O2 178.56(16) . . ? O5 Co2 O1 85.58(15) . . ? O2 Co2 O1 94.22(16) . . ? O5 Co2 O4 93.74(15) . . ? O2 Co2 O4 84.83(15) . . ? O1 Co2 O4 88.81(16) . . ? O5 Co2 N2 84.34(18) . . ? O2 Co2 N2 95.66(18) . . ? O1 Co2 N2 167.05(17) . . ? O4 Co2 N2 83.77(18) . . ? O5 Co2 N1 95.23(17) . . ? O2 Co2 N1 86.17(17) . . ? O1 Co2 N1 82.71(18) . . ? O4 Co2 N1 167.14(18) . . ? N2 Co2 N1 106.3(2) . . ? O10 Co3 O11 88.18(17) . . ? O10 Co3 O7 86.92(15) . . ? O11 Co3 O7 90.18(16) . . ? O10 Co3 O17 176.48(16) . . ? O11 Co3 O17 92.08(17) . . ? O7 Co3 O17 96.59(16) . . ? O10 Co3 N3 92.28(19) . . ? O11 Co3 N3 175.57(18) . . ? O7 Co3 N3 85.45(18) . . ? O17 Co3 N3 87.73(19) . . ? O10 Co3 N4 84.29(17) . . ? O11 Co3 N4 86.36(19) . . ? O7 Co3 N4 170.65(18) . . ? O17 Co3 N4 92.22(18) . . ? N3 Co3 N4 98.1(2) . . ? C1 N1 Co2 97.5(3) . . ? C1 N1 H11 112.3 . . ? Co2 N1 H11 112.3 . . ? C1 N1 H12 112.3 . . ? Co2 N1 H12 112.3 . . ? H11 N1 H12 109.9 . . ? N1 C1 C3 104.5(5) . . ? N1 C1 C4 112.8(4) . . ? C3 C1 C4 110.8(4) . . ? N1 C1 C2 105.1(4) . . ? C3 C1 C2 110.5(4) . . ? C4 C1 C2 112.7(5) . . ? O1 C2 C1 108.8(4) . . ? O1 C2 H2C 109.9 . . ? C1 C2 H2C 109.9 . . ? O1 C2 H2D 109.9 . . ? C1 C2 H2D 109.9 . . ? H2C C2 H2D 108.3 . . ? C2 O1 Co2 109.5(3) . . ? C2 O1 Co1 128.6(3) . . ? Co2 O1 Co1 97.64(16) . . ? C2 O1 Co1 124.7(3) . 2_666 ? Co2 O1 Co1 95.29(15) . 2_666 ? Co1 O1 Co1 93.89(13) . 2_666 ? O2 C3 C1 109.0(4) . . ? O2 C3 H3C 109.9 . . ? C1 C3 H3C 109.9 . . ? O2 C3 H3D 109.9 . . ? C1 C3 H3D 109.9 . . ? H3C C3 H3D 108.3 . . ? C3 O2 Co2 109.8(3) . . ? C3 O2 Y1 132.4(3) . . ? Co2 O2 Y1 107.15(15) . . ? O3 C4 C1 114.1(5) . . ? O3 C4 H4C 108.7 . . ? C1 C4 H4C 108.7 . . ? O3 C4 H4D 108.7 . . ? C1 C4 H4D 108.7 . . ? H4C C4 H4D 107.6 . . ? C4 O3 H3 109.5 . . ? C5 N2 Co2 97.9(3) . . ? C5 N2 H21 112.2 . . ? Co2 N2 H21 112.2 . . ? C5 N2 H22 112.2 . . ? Co2 N2 H22 112.2 . . ? H21 N2 H22 109.8 . . ? N2 C5 C7 104.0(5) . . ? N2 C5 C8 112.6(5) . . ? C7 C5 C8 113.3(5) . . ? N2 C5 C6 105.3(4) . . ? C7 C5 C6 110.0(5) . . ? C8 C5 C6 111.1(5) . . ? O4 C6 C5 109.6(4) . . ? O4 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? O4 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? C6 O4 Co2 109.9(3) . . ? C6 O4 Co1 130.6(3) . . ? Co2 O4 Co1 96.32(16) . . ? C6 O4 Y1 121.9(3) . . ? Co2 O4 Y1 101.95(14) . . ? Co1 O4 Y1 90.63(13) . . ? O5 C7 C5 108.1(4) . . ? O5 C7 H7A 110.1 . . ? C5 C7 H7A 110.1 . . ? O5 C7 H7B 110.1 . . ? C5 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? C7 O5 Co2 111.8(3) . . ? C7 O5 Co1 134.0(3) . 2_666 ? Co2 O5 Co1 104.14(17) . 2_666 ? O6 C8 C5 112.6(5) . . ? O6 C8 H8A 109.1 . . ? C5 C8 H8A 109.1 . . ? O6 C8 H8B 109.1 . . ? C5 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C8 O6 H6 109.5 . . ? C9 N3 Co3 111.8(4) . . ? C9 N3 H31 109.2 . . ? Co3 N3 H31 109.2 . . ? C9 N3 H32 109.2 . . ? Co3 N3 H32 109.2 . . ? H31 N3 H32 107.9 . . ? N3 C9 C12 109.3(4) . . ? N3 C9 C11 108.7(4) . . ? C12 C9 C11 110.4(4) . . ? N3 C9 C10 107.6(4) . . ? C12 C9 C10 109.2(4) . . ? C11 C9 C10 111.5(5) . . ? O7 C10 C9 110.3(4) . . ? O7 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? O7 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C10 O7 Co3 107.4(3) . . ? C10 O7 Y1 115.2(3) . . ? Co3 O7 Y1 98.66(14) . . ? C10 O7 Y2 127.1(3) . . ? Co3 O7 Y2 93.95(14) . . ? Y1 O7 Y2 108.11(14) . . ? O8 C11 C9 113.3(5) . . ? O8 C11 H11A 108.9 . . ? C9 C11 H11A 108.9 . . ? O8 C11 H11B 108.9 . . ? C9 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C11 O8 Co1 114.3(3) . . ? C11 O8 Y1 136.1(3) . . ? Co1 O8 Y1 98.97(15) . . ? O9 C12 C9 113.1(3) . . ? O9 C12 H12A 109.0 . . ? C9 C12 H12A 109.0 . . ? O9 C12 H12B 109.0 . . ? C9 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C12 O9 H9 109.5 . . ? C13 N4 Co3 98.2(3) . . ? C13 N4 H41 112.1 . . ? Co3 N4 H41 112.1 . . ? C13 N4 H42 112.1 . . ? Co3 N4 H42 112.1 . . ? H41 N4 H42 109.8 . . ? N4 C13 C15 104.7(4) . . ? N4 C13 C14 104.6(5) . . ? C15 C13 C14 109.9(5) . . ? N4 C13 C16 113.6(5) . . ? C15 C13 C16 111.4(5) . . ? C14 C13 C16 112.2(5) . . ? O10 C14 C13 108.9(4) . . ? O10 C14 H14A 109.9 . . ? C13 C14 H14A 109.9 . . ? O10 C14 H14B 109.9 . . ? C13 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? C14 O10 Co3 110.6(3) . . ? C14 O10 Y1 138.1(3) . . ? Co3 O10 Y1 106.16(16) . . ? O11 C15 C13 108.3(5) . . ? O11 C15 H15A 110.0 . . ? C13 C15 H15A 110.0 . . ? O11 C15 H15B 110.0 . . ? C13 C15 H15B 110.0 . . ? H15A C15 H15B 108.4 . . ? C15 O11 Co3 110.6(3) . . ? C15 O11 Y2 143.9(4) . . ? Co3 O11 Y2 104.28(15) . . ? O12 C16 C13 112.4(5) . . ? O12 C16 H16A 109.1 . . ? C13 C16 H16A 109.1 . . ? O12 C16 H16B 109.1 . . ? C13 C16 H16B 109.1 . . ? H16A C16 H16B 107.9 . . ? C16 O12 H121 109.5 . . ? C17 O13 Co1 128.0(3) . . ? C17 O14 Y1 132.1(4) . . ? O13 C17 O14 124.9(5) . . ? O13 C17 C18 118.2(5) . . ? O14 C17 C18 116.9(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C19 O15 Y2 150.0(4) . . ? C19 O15 Y1 93.4(3) . . ? Y2 O15 Y1 114.40(16) . . ? C19 O16 Y1 94.8(4) . . ? O16 C19 O15 118.5(6) . . ? O16 C19 C20 121.7(6) . . ? O15 C19 C20 119.8(6) . . ? O16 C19 Y1 59.3(3) . . ? O15 C19 Y1 59.7(3) . . ? C20 C19 Y1 170.8(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C21 O17 Co3 125.9(4) . . ? C21 O18 Y2 133.9(3) . . ? O18 C21 O17 125.9(5) . . ? O18 C21 C22 119.0(5) . . ? O17 C21 C22 115.0(5) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O21 N5 O19 121.7(5) . . ? O21 N5 O20 121.4(5) . . ? O19 N5 O20 116.9(5) . . ? O21 N5 Y2 178.7(4) . . ? O19 N5 Y2 59.5(3) . . ? O20 N5 Y2 57.4(3) . . ? N5 O19 Y2 94.8(3) . . ? N5 O20 Y2 96.8(3) . . ? O24 N6 O22 121.6(7) . . ? O24 N6 O23 121.4(7) . . ? O22 N6 O23 117.1(5) . . ? O24 N6 Y2 178.4(6) . . ? O22 N6 Y2 58.9(3) . . ? O23 N6 Y2 58.2(3) . . ? N6 O22 Y2 95.3(4) . . ? N6 O23 Y2 95.6(4) . . ? C23 O25 Y2 136.2(4) . . ? C23 O25 H25 103(5) . . ? Y2 O25 H25 115(5) . . ? O25 C23 H23A 109.5 . . ? O25 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O25 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N31B O31 N31A 109.7(10) . . ? O32A N31A O33A 115.1(11) . . ? O32A N31A O31 129.5(10) . . ? O33A N31A O31 114.8(10) . . ? O32B N31B O31 130.7(14) . . ? O32B N31B O33B 115.7(14) . . ? O31 N31B O33B 113.6(13) . . ? C43 O43 H43 109.5 . . ? O43 C43 H43A 109.5 . . ? O43 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O43 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H11 O13 0.92 2.33 3.118(6) 144.0 2_666 N1 H12 O34A 0.92 2.03 2.946(13) 177.1 2_656 N1 H12 O32B 0.92 2.28 3.122(12) 151.2 2_656 O3 H3 O43 0.84 1.96 2.781(13) 165.8 1_554 N2 H21 O16 0.92 2.13 2.939(6) 145.6 . N2 H22 O41A 0.92 2.18 2.993(16) 146.2 2_656 N2 H22 O41B 0.92 2.19 3.07(2) 158.8 2_656 O6 H6 O41A 0.84 1.87 2.708(15) 171.1 2_656 O6 H6 O47B 0.84 2.42 3.22(3) 159.6 2_656 N3 H31 O34B 0.92 2.44 3.20(2) 139.1 . N3 H32 O6 0.92 2.05 2.925(6) 159.3 1_455 O9 H9 O34B 0.84 2.16 2.652(19) 117.6 2_566 N4 H41 O20 0.92 2.48 3.281(6) 146.3 2_557 N4 H41 O21 0.92 2.50 3.389(7) 161.6 2_557 N4 H42 O31 0.92 2.29 3.165(8) 159.7 . O12 H121 O32B 0.84 2.58 3.119(14) 122.8 . O25 H25 O14 0.86(4) 1.94(4) 2.753(5) 157(6) . O43 H43 O44X 0.84 2.03 2.86(2) 167.9 . _diffrn_measured_fraction_theta_max 0.897 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.240 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.148 ############################################################### data_10428 _database_code_depnum_ccdc_archive 'CCDC 758591' #TrackingRef 'hua_co6ln4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H96 Co6 Gd4 N12 O50, 2(N O3), 5(C H4 O), 4(H2 O)' _chemical_formula_sum 'C50 H124 Co6 Gd4 N14 O65' _chemical_formula_weight 2944.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8831(6) _cell_length_b 13.6555(5) _cell_length_c 16.0874(6) _cell_angle_alpha 72.486(3) _cell_angle_beta 71.881(4) _cell_angle_gamma 73.986(4) _cell_volume 2512.73(18) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 2617 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 63.65 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.946 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1460 _exptl_absorpt_coefficient_mu 25.278 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0449 _exptl_absorpt_correction_T_max 0.0501 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20277 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.1543 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 6.15 _diffrn_reflns_theta_max 89.74 _reflns_number_total 10863 _reflns_number_gt 6337 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'FRAMBO (BrukerAXS Inc., 2003)' _computing_cell_refinement 'FRAMBO (BrukerAXS Inc., 2003)' _computing_data_reduction 'SAINT+ 6.0 (Bruker AXS Inc., 2000)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A ligand hydroxyl group and the lattice solvent molecules showed two-fold disorder and were refined using partial isotropic atoms, with geometrical restraints as appropriate. The terminal ligand on Gd(2) appears to be a superposition of a methanol and an aquo ligand, which were refined with a common full-occupancy oxygen and a half-occupancy carbon. No attempt was made to locate the H-atoms on the half-water, or on the disordered lattice solvent molecules. The nitrate counterion was clearly disordered, but attempts to "split" it in the refinement proved problematic, even with restraints, and it was refined with full-occupancy isotropic atoms. N-H and O-H H atoms were refined with their respective X-H distances restrained to 0.88(4) Ang. ; _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^)+(0.0472P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10863 _refine_ls_number_parameters 618 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1166 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _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 Gd1 Gd 0.34379(4) 0.29167(4) 0.74403(3) 0.01419(13) Uani 1 1 d . . . Gd2 Gd 0.14422(4) 0.21721(4) 0.99363(3) 0.02040(15) Uani 1 1 d . D . Co1 Co 0.39069(10) 0.49958(10) 0.58073(8) 0.0153(3) Uani 1 1 d . . . Co2 Co 0.57305(10) 0.30345(10) 0.56826(8) 0.0169(3) Uani 1 1 d . . . Co3 Co 0.10341(10) 0.20544(10) 0.80524(8) 0.0202(3) Uani 1 1 d . . . N1 N 0.6163(6) 0.2262(6) 0.4759(5) 0.0275(19) Uani 1 1 d D . . H11 H 0.658(6) 0.263(6) 0.420(4) 0.033 Uiso 1 1 d D . . H12 H 0.652(7) 0.162(4) 0.477(6) 0.033 Uiso 1 1 d D . . C1 C 0.5030(7) 0.2252(7) 0.4715(6) 0.030(2) Uani 1 1 d . . . C2 C 0.4465(7) 0.3402(7) 0.4488(6) 0.027(2) Uani 1 1 d . . . H2A H 0.4656 0.3686 0.3828 0.032 Uiso 1 1 calc R . . H2B H 0.3645 0.3474 0.4701 0.032 Uiso 1 1 calc R . . O1 O 0.4848(5) 0.3984(5) 0.4928(4) 0.0305(16) Uani 1 1 d . . . C3 C 0.4460(8) 0.1730(7) 0.5659(6) 0.033(2) Uani 1 1 d . . . H3A H 0.3653 0.1827 0.5714 0.039 Uiso 1 1 calc R . . H3B H 0.4779 0.0969 0.5788 0.039 Uiso 1 1 calc R . . O2 O 0.4627(5) 0.2196(5) 0.6284(4) 0.0328(16) Uani 1 1 d . . . C4 C 0.5026(9) 0.1679(8) 0.4046(6) 0.044(3) Uani 1 1 d . . . H4A H 0.5296 0.0919 0.4271 0.052 Uiso 1 1 calc R . . H4B H 0.4248 0.1778 0.4011 0.052 Uiso 1 1 calc R . . O3 O 0.5670(7) 0.1999(7) 0.3194(5) 0.068(2) Uani 1 1 d . . . H3 H 0.6326 0.1944 0.3218 0.101 Uiso 1 1 calc R . . N2 N 0.6709(7) 0.2344(6) 0.6485(6) 0.037(2) Uani 1 1 d D . . H21 H 0.640(7) 0.200(7) 0.706(4) 0.045 Uiso 1 1 d D . . H22 H 0.739(5) 0.193(7) 0.635(6) 0.045 Uiso 1 1 d D . . C5 C 0.6894(8) 0.3325(7) 0.6624(6) 0.030(2) Uani 1 1 d . . . C6 C 0.5773(8) 0.3944(7) 0.6982(6) 0.033(2) Uani 1 1 d . . . H6A H 0.5534 0.3690 0.7643 0.040 Uiso 1 1 calc R . . H6B H 0.5806 0.4694 0.6843 0.040 Uiso 1 1 calc R . . O4 O 0.4985(5) 0.3816(5) 0.6557(4) 0.0297(15) Uani 1 1 d . . . C7 C 0.7438(8) 0.3905(8) 0.5669(6) 0.037(3) Uani 1 1 d . . . H7A H 0.7430 0.4635 0.5661 0.045 Uiso 1 1 calc R . . H7B H 0.8221 0.3546 0.5473 0.045 Uiso 1 1 calc R . . O5 O 0.6798(5) 0.3895(5) 0.5084(4) 0.0321(16) Uani 1 1 d . . . C8 C 0.7618(8) 0.3095(9) 0.7251(8) 0.051(3) Uani 1 1 d . . . H8A H 0.7666 0.3762 0.7347 0.062 Uiso 1 1 calc R . . H8B H 0.7272 0.2672 0.7840 0.062 Uiso 1 1 calc R . . O6 O 0.8725(6) 0.2537(6) 0.6919(5) 0.060(2) Uani 1 1 d . . . H6 H 0.8836 0.1941 0.7264 0.090 Uiso 1 1 calc R . . N3 N 0.0734(7) 0.3105(7) 0.6989(5) 0.032(2) Uani 1 1 d D . . H31 H 0.117(7) 0.286(7) 0.653(4) 0.038 Uiso 1 1 d D . . H32 H 0.004(5) 0.319(7) 0.685(6) 0.038 Uiso 1 1 d D . . C9 C 0.0650(7) 0.4202(7) 0.7066(6) 0.027(2) Uani 1 1 d . B . C10 C 0.0767(7) 0.4093(7) 0.8020(6) 0.030(2) Uani 1 1 d . . . H10A H 0.1085 0.4679 0.8009 0.036 Uiso 1 1 calc R . . H10B H 0.0017 0.4147 0.8440 0.036 Uiso 1 1 calc R . . O7 O 0.1442(5) 0.3146(5) 0.8338(4) 0.0278(15) Uani 1 1 d . . . C11 C 0.1580(8) 0.4676(8) 0.6337(7) 0.041(3) Uani 1 1 d . . . H11A H 0.1488 0.4707 0.5741 0.049 Uiso 1 1 calc R . . H11B H 0.1505 0.5404 0.6374 0.049 Uiso 1 1 calc R . . O8 O 0.2659(5) 0.4112(5) 0.6402(4) 0.0312(16) Uani 1 1 d . . . C12 C -0.0484(8) 0.4854(8) 0.6942(7) 0.042(3) Uani 1 1 d D . . H12A H -0.1069 0.4547 0.7438 0.051 Uiso 0.75 1 calc PR A 1 H12B H -0.0540 0.5570 0.6997 0.051 Uiso 0.75 1 calc PR A 1 H12C H -0.0532 0.4881 0.6332 0.051 Uiso 0.25 1 d PR A 2 H12D H -0.1066 0.4485 0.7380 0.051 Uiso 0.25 1 d PR A 2 O9A O -0.0693(10) 0.4925(11) 0.6173(7) 0.077(4) Uani 0.75 1 d PD B 1 H9A H -0.1102 0.4504 0.6251 0.116 Uiso 0.75 1 calc PR B 1 O9B O -0.068(2) 0.5810(18) 0.702(2) 0.055(8) Uiso 0.25 1 d PD B 2 H9B H -0.1055 0.5844 0.7548 0.082 Uiso 0.25 1 calc PR B 2 N4 N 0.0871(7) 0.0848(7) 0.7751(6) 0.036(2) Uani 1 1 d D . . H41 H 0.029(5) 0.056(7) 0.815(5) 0.043 Uiso 1 1 d D . . H42 H 0.103(8) 0.098(7) 0.713(3) 0.043 Uiso 1 1 d D . . C13 C 0.1805(8) 0.0057(7) 0.8066(7) 0.035(3) Uani 1 1 d . . . C14 C 0.2838(8) 0.0535(8) 0.7529(7) 0.045(3) Uani 1 1 d . . . H14A H 0.3453 0.0204 0.7832 0.054 Uiso 1 1 calc R . . H14B H 0.3090 0.0406 0.6917 0.054 Uiso 1 1 calc R . . O10 O 0.2559(5) 0.1633(5) 0.7473(4) 0.0333(16) Uani 1 1 d . . . C15 C 0.1581(8) 0.0047(7) 0.9037(7) 0.035(3) Uani 1 1 d . . . H15A H 0.0941 -0.0294 0.9391 0.042 Uiso 1 1 calc R . . H15B H 0.2241 -0.0356 0.9268 0.042 Uiso 1 1 calc R . . O11 O 0.1334(5) 0.1110(5) 0.9127(4) 0.0330(16) Uani 1 1 d . . . C16 C 0.1883(9) -0.0989(8) 0.7936(7) 0.044(3) Uani 1 1 d . . . H16A H 0.2463 -0.1498 0.8217 0.053 Uiso 1 1 calc R . . H16B H 0.1163 -0.1213 0.8248 0.053 Uiso 1 1 calc R . . O12 O 0.2144(7) -0.1011(7) 0.7022(5) 0.067(2) Uani 1 1 d . . . H121 H 0.1728 -0.1342 0.6953 0.101 Uiso 1 1 calc RD . . O13 O 0.3392(5) 0.5774(5) 0.6821(4) 0.0360(17) Uani 1 1 d . . . O14 O 0.3134(5) 0.4444(5) 0.8038(4) 0.0376(17) Uani 1 1 d . . . C17 C 0.3087(8) 0.5405(8) 0.7648(7) 0.035(3) Uani 1 1 d . . . C18 C 0.2692(11) 0.6190(9) 0.8242(8) 0.069(4) Uani 1 1 d . . . H18A H 0.2692 0.5815 0.8866 0.103 Uiso 1 1 calc R . . H18B H 0.1935 0.6573 0.8211 0.103 Uiso 1 1 calc R . . H18C H 0.3194 0.6686 0.8031 0.103 Uiso 1 1 calc R . . O15 O 0.3301(5) 0.2159(5) 0.9077(4) 0.0350(17) Uani 1 1 d . . . O16 O 0.4970(5) 0.1932(5) 0.8187(4) 0.0421(19) Uani 1 1 d . . . C19 C 0.4353(8) 0.1867(8) 0.8983(7) 0.037(3) Uani 1 1 d . . . C20 C 0.4794(9) 0.1514(11) 0.9776(7) 0.066(4) Uani 1 1 d . . . H20A H 0.5531 0.1059 0.9643 0.099 Uiso 1 1 calc R . . H20B H 0.4290 0.1122 1.0274 0.099 Uiso 1 1 calc R . . H20C H 0.4860 0.2122 0.9945 0.099 Uiso 1 1 calc R . . O17 O -0.0530(5) 0.2397(5) 0.8613(4) 0.0314(16) Uani 1 1 d . . . O18 O -0.0436(5) 0.2632(5) 0.9911(4) 0.0365(17) Uani 1 1 d . . . C21 C -0.0966(8) 0.2577(7) 0.9390(7) 0.034(3) Uani 1 1 d . . . C22 C -0.2228(8) 0.2805(9) 0.9660(7) 0.047(3) Uani 1 1 d . . . H22A H -0.2510 0.3541 0.9396 0.071 Uiso 1 1 calc R . . H22B H -0.2487 0.2669 1.0317 0.071 Uiso 1 1 calc R . . H22C H -0.2503 0.2353 0.9441 0.071 Uiso 1 1 calc R . . N5 N 0.1835(8) 0.0038(8) 1.1065(6) 0.048(2) Uani 1 1 d . . . O19 O 0.2608(6) 0.0411(6) 1.0467(5) 0.057(2) Uani 1 1 d . . . O20 O 0.0877(6) 0.0612(6) 1.1149(4) 0.0456(19) Uani 1 1 d . . . O21 O 0.1996(8) -0.0853(6) 1.1574(6) 0.083(3) Uani 1 1 d . . . N6 N 0.1159(10) 0.2433(9) 1.1723(7) 0.069(3) Uani 1 1 d . . . O22 O 0.0330(7) 0.2757(7) 1.1359(5) 0.066(2) Uani 1 1 d . . . O23 O 0.2125(7) 0.2076(7) 1.1257(6) 0.066(2) Uani 1 1 d . . . O24 O 0.1016(9) 0.2463(11) 1.2524(7) 0.133(5) Uani 1 1 d . . . O25 O 0.1693(6) 0.3935(6) 0.9700(5) 0.051(2) Uani 1 1 d . . . H25 H 0.2377 0.4067 0.9286 0.076 Uiso 1 1 calc R C 1 C23A C 0.106(2) 0.479(2) 1.004(2) 0.091(10) Uiso 0.50 1 d P D 1 H23A H 0.1476 0.5358 0.9812 0.137 Uiso 0.50 1 calc PR D 1 H23B H 0.0888 0.4593 1.0696 0.137 Uiso 0.50 1 calc PR D 1 H23C H 0.0363 0.5028 0.9842 0.137 Uiso 0.50 1 calc PR D 1 N8 N 0.114(2) 0.2396(16) 0.5108(16) 0.238(12) Uiso 1 1 d DU E 1 O26 O 0.1148(11) 0.1508(12) 0.5704(10) 0.143(5) Uiso 1 1 d DU E 1 O27 O 0.1601(14) 0.3159(16) 0.4955(12) 0.195(7) Uiso 1 1 d DU E 1 O28 O 0.0403(19) 0.2772(18) 0.4650(15) 0.260(10) Uiso 1 1 d DU E 1 O31A O 0.2984(14) 0.0066(13) 1.4943(11) 0.048(5) Uiso 0.50 1 d P F 1 O31B O 0.2647(18) -0.0027(18) 1.4766(14) 0.084(7) Uiso 0.50 1 d P G 2 O32A O 0.8828(13) 0.2084(13) 1.3662(11) 0.132(6) Uiso 0.75 1 d P H 1 O32B O 0.195(3) 0.445(3) 1.111(2) 0.074(10) Uiso 0.25 1 d P I 2 O41 O 0.3078(15) 0.0982(15) 1.3004(12) 0.214(7) Uiso 1 1 d D . . C41 C 0.3908(15) 0.0429(14) 1.2419(12) 0.115(6) Uiso 1 1 d D . . O42 O 0.8853(10) 0.1263(10) 0.5515(9) 0.130(4) Uiso 1 1 d D . . C42 C 0.907(2) 0.0390(19) 0.6198(15) 0.184(10) Uiso 1 1 d D . . O43X O 0.4461(19) 0.3607(18) 0.2135(15) 0.121(8) Uiso 0.50 1 d PD . . C43X C 0.330(2) 0.375(3) 0.250(2) 0.112(12) Uiso 0.50 1 d PD . . 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 0.0161(3) 0.0117(3) 0.0142(3) -0.0018(2) 0.0014(2) -0.0092(2) Gd2 0.0198(3) 0.0226(3) 0.0163(3) -0.0015(2) 0.0012(2) -0.0103(2) Co1 0.0187(7) 0.0133(7) 0.0145(7) 0.0006(5) -0.0028(5) -0.0099(5) Co2 0.0178(7) 0.0141(7) 0.0180(7) 0.0010(6) -0.0010(5) -0.0111(5) Co3 0.0214(7) 0.0187(7) 0.0199(7) -0.0038(6) 0.0025(6) -0.0128(6) N1 0.027(5) 0.020(4) 0.030(5) -0.005(4) 0.001(4) -0.007(4) C1 0.029(5) 0.028(6) 0.036(6) -0.008(5) -0.001(5) -0.016(4) C2 0.026(5) 0.033(6) 0.029(5) -0.011(5) -0.009(4) -0.011(4) O1 0.022(3) 0.021(4) 0.049(4) -0.015(3) 0.004(3) -0.012(3) C3 0.037(6) 0.023(6) 0.036(6) -0.013(5) 0.003(5) -0.010(5) O2 0.035(4) 0.036(4) 0.031(4) -0.010(3) 0.004(3) -0.025(3) C4 0.066(8) 0.044(7) 0.023(6) -0.016(5) 0.008(5) -0.027(6) O3 0.076(6) 0.078(6) 0.054(5) -0.026(5) 0.008(4) -0.040(6) N2 0.029(5) 0.028(5) 0.044(6) 0.006(4) -0.003(4) -0.012(4) C5 0.038(6) 0.027(6) 0.030(5) 0.003(4) -0.016(5) -0.015(5) C6 0.048(6) 0.028(6) 0.029(6) 0.001(5) -0.010(5) -0.025(5) O4 0.034(4) 0.038(4) 0.022(3) -0.003(3) -0.004(3) -0.023(3) C7 0.037(6) 0.037(6) 0.039(6) -0.002(5) -0.007(5) -0.020(5) O5 0.030(4) 0.034(4) 0.032(4) 0.008(3) -0.009(3) -0.023(3) C8 0.040(7) 0.047(7) 0.064(8) 0.001(6) -0.012(6) -0.020(6) O6 0.057(5) 0.041(5) 0.076(6) 0.011(4) -0.033(4) -0.011(4) N3 0.035(5) 0.035(5) 0.027(5) -0.006(4) -0.007(4) -0.012(4) C9 0.023(5) 0.024(5) 0.034(6) 0.001(4) -0.008(4) -0.011(4) C10 0.025(5) 0.023(5) 0.041(6) -0.006(5) -0.001(4) -0.011(4) O7 0.025(3) 0.024(4) 0.031(4) 0.000(3) -0.006(3) -0.009(3) C11 0.046(7) 0.044(7) 0.031(6) 0.011(5) -0.013(5) -0.026(5) O8 0.033(4) 0.027(4) 0.030(4) 0.005(3) -0.007(3) -0.015(3) C12 0.033(6) 0.043(7) 0.047(7) -0.003(6) -0.009(5) -0.011(5) O9A 0.066(8) 0.123(12) 0.064(8) -0.009(7) -0.034(6) -0.048(7) N4 0.042(5) 0.032(5) 0.032(5) -0.010(4) 0.007(4) -0.021(4) C13 0.038(6) 0.023(6) 0.037(6) -0.008(5) 0.004(5) -0.010(5) C14 0.039(6) 0.034(6) 0.057(7) -0.008(6) 0.007(5) -0.021(5) O10 0.039(4) 0.027(4) 0.037(4) -0.008(3) -0.001(3) -0.020(3) C15 0.033(6) 0.018(5) 0.050(7) -0.012(5) 0.000(5) -0.004(4) O11 0.036(4) 0.026(4) 0.032(4) -0.004(3) 0.001(3) -0.011(3) C16 0.048(7) 0.029(6) 0.045(7) -0.011(5) 0.008(5) -0.012(5) O12 0.087(7) 0.059(6) 0.063(6) -0.027(5) 0.010(5) -0.044(5) O13 0.038(4) 0.035(4) 0.034(4) -0.007(3) 0.004(3) -0.020(3) O14 0.045(4) 0.022(4) 0.044(4) -0.009(3) 0.002(3) -0.017(3) C17 0.046(6) 0.034(6) 0.028(6) -0.007(5) -0.001(5) -0.022(5) C18 0.109(11) 0.041(7) 0.053(8) -0.023(6) 0.012(7) -0.031(7) O15 0.026(4) 0.045(4) 0.030(4) -0.005(3) -0.001(3) -0.012(3) O16 0.035(4) 0.048(5) 0.031(4) 0.002(3) 0.001(3) -0.013(3) C19 0.037(6) 0.033(6) 0.040(7) -0.003(5) -0.008(5) -0.012(5) C20 0.054(8) 0.091(10) 0.034(7) 0.005(7) -0.012(6) -0.005(7) O17 0.026(3) 0.036(4) 0.031(4) -0.007(3) 0.002(3) -0.015(3) O18 0.044(4) 0.037(4) 0.030(4) -0.009(3) -0.003(3) -0.016(3) C21 0.033(6) 0.023(6) 0.041(7) -0.011(5) 0.002(5) -0.008(5) C22 0.039(6) 0.063(8) 0.041(7) -0.014(6) -0.006(5) -0.015(6) N5 0.041(6) 0.052(7) 0.053(6) -0.012(5) -0.008(5) -0.017(5) O19 0.040(4) 0.058(5) 0.059(5) 0.010(4) 0.000(4) -0.029(4) O20 0.039(4) 0.055(5) 0.034(4) 0.004(4) -0.001(3) -0.021(4) O21 0.114(8) 0.035(5) 0.085(7) 0.029(5) -0.030(6) -0.030(5) N6 0.063(8) 0.093(9) 0.058(8) -0.035(7) -0.017(7) -0.006(7) O22 0.054(5) 0.106(7) 0.046(5) -0.028(5) -0.005(4) -0.028(5) O23 0.052(5) 0.085(7) 0.065(6) -0.028(5) -0.013(5) -0.011(5) O24 0.132(9) 0.248(15) 0.055(7) -0.074(9) -0.021(7) -0.056(10) O25 0.061(5) 0.047(5) 0.044(5) -0.014(4) -0.002(4) -0.020(4) _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 O8 2.226(6) . ? Gd1 O2 2.297(6) . ? Gd1 O10 2.315(6) . ? Gd1 O14 2.439(6) . ? Gd1 O4 2.458(6) . ? Gd1 O16 2.487(7) . ? Gd1 O15 2.492(6) . ? Gd1 O7 2.513(6) . ? Gd2 O11 2.275(6) . ? Gd2 O18 2.336(7) . ? Gd2 O15 2.362(6) . ? Gd2 O25 2.418(7) . ? Gd2 O23 2.497(8) . ? Gd2 O7 2.515(6) . ? Gd2 O19 2.517(7) . ? Gd2 O20 2.519(7) . ? Gd2 O22 2.522(7) . ? Co1 O5 1.979(6) 2_666 ? Co1 O13 2.052(6) . ? Co1 O8 2.091(6) . ? Co1 O1 2.136(6) . ? Co1 O4 2.149(6) . ? Co1 O1 2.230(6) 2_666 ? Co2 O4 1.880(6) . ? Co2 O1 1.883(6) . ? Co2 O5 1.894(6) . ? Co2 O2 1.909(6) . ? Co2 N1 1.933(8) . ? Co2 N2 1.942(9) . ? Co3 O11 1.897(6) . ? Co3 O10 1.903(6) . ? Co3 O17 1.923(6) . ? Co3 O7 1.925(6) . ? Co3 N4 1.931(9) . ? Co3 N3 1.939(8) . ? N1 C1 1.487(11) . ? N1 H11 0.96(4) . ? N1 H12 0.87(4) . ? C1 C4 1.513(13) . ? C1 C3 1.515(12) . ? C1 C2 1.522(12) . ? C2 O1 1.467(10) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O1 Co1 2.230(6) 2_666 ? C3 O2 1.434(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O3 1.375(11) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O3 H3 0.8400 . ? N2 C5 1.513(12) . ? N2 H21 0.92(4) . ? N2 H22 0.90(4) . ? C5 C8 1.490(14) . ? C5 C6 1.494(12) . ? C5 C7 1.543(12) . ? C6 O4 1.460(11) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O5 1.436(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? O5 Co1 1.979(6) 2_666 ? C8 O6 1.440(12) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? O6 H6 0.8400 . ? N3 C9 1.511(12) . ? N3 H31 0.87(4) . ? N3 H32 0.96(4) . ? C9 C12 1.524(12) . ? C9 C11 1.526(12) . ? C9 C10 1.547(13) . ? C10 O7 1.395(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O8 1.411(10) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O9B 1.299(19) . ? C12 O9A 1.316(12) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 H12C 0.9900 . ? C12 H12D 0.9899 . ? O9A H12C 0.3597 . ? O9A H9A 0.8400 . ? O9B H9B 0.8400 . ? N4 C13 1.485(13) . ? N4 H41 0.92(4) . ? N4 H42 0.92(4) . ? C13 C16 1.477(13) . ? C13 C15 1.494(13) . ? C13 C14 1.539(13) . ? C14 O10 1.424(11) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O11 1.440(10) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O12 1.411(12) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? O12 H121 0.8400 . ? O13 C17 1.248(10) . ? O14 C17 1.267(11) . ? C17 C18 1.528(13) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O15 C19 1.276(11) . ? O16 C19 1.272(11) . ? C19 C20 1.454(14) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? O17 C21 1.268(11) . ? O18 C21 1.264(12) . ? C21 C22 1.513(13) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? N5 O21 1.249(11) . ? N5 O19 1.252(10) . ? N5 O20 1.258(10) . ? N6 O24 1.255(12) . ? N6 O22 1.284(12) . ? N6 O23 1.286(11) . ? O25 C23A 1.38(3) . ? O25 H25 0.9500 . ? C23A H23A 0.9800 . ? C23A H23B 0.9800 . ? C23A H23C 0.9800 . ? N8 O27 1.259(15) . ? N8 O28 1.287(16) . ? N8 O26 1.300(15) . ? O41 C41 1.398(16) . ? O42 C42 1.388(18) . ? O43X C43X 1.41(2) . ? 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 Gd1 O2 86.7(2) . . ? O8 Gd1 O10 94.0(2) . . ? O2 Gd1 O10 78.0(2) . . ? O8 Gd1 O14 81.9(2) . . ? O2 Gd1 O14 138.9(2) . . ? O10 Gd1 O14 141.9(2) . . ? O8 Gd1 O4 79.2(2) . . ? O2 Gd1 O4 65.2(2) . . ? O10 Gd1 O4 142.8(2) . . ? O14 Gd1 O4 73.9(2) . . ? O8 Gd1 O16 155.9(2) . . ? O2 Gd1 O16 81.6(2) . . ? O10 Gd1 O16 104.0(2) . . ? O14 Gd1 O16 93.1(2) . . ? O4 Gd1 O16 76.8(2) . . ? O8 Gd1 O15 146.4(2) . . ? O2 Gd1 O15 126.3(2) . . ? O10 Gd1 O15 87.8(2) . . ? O14 Gd1 O15 76.4(2) . . ? O4 Gd1 O15 117.9(2) . . ? O16 Gd1 O15 51.9(2) . . ? O8 Gd1 O7 81.0(2) . . ? O2 Gd1 O7 141.7(2) . . ? O10 Gd1 O7 67.0(2) . . ? O14 Gd1 O7 75.0(2) . . ? O4 Gd1 O7 145.0(2) . . ? O16 Gd1 O7 120.6(2) . . ? O15 Gd1 O7 68.81(19) . . ? O11 Gd2 O18 77.2(2) . . ? O11 Gd2 O15 87.5(2) . . ? O18 Gd2 O15 146.0(2) . . ? O11 Gd2 O25 139.0(2) . . ? O18 Gd2 O25 96.4(2) . . ? O15 Gd2 O25 75.6(2) . . ? O11 Gd2 O23 140.3(3) . . ? O18 Gd2 O23 124.0(2) . . ? O15 Gd2 O23 86.8(3) . . ? O25 Gd2 O23 76.6(3) . . ? O11 Gd2 O7 68.7(2) . . ? O18 Gd2 O7 75.4(2) . . ? O15 Gd2 O7 70.8(2) . . ? O25 Gd2 O7 70.6(2) . . ? O23 Gd2 O7 143.8(3) . . ? O11 Gd2 O19 74.0(2) . . ? O18 Gd2 O19 130.0(2) . . ? O15 Gd2 O19 71.9(2) . . ? O25 Gd2 O19 131.6(3) . . ? O23 Gd2 O19 66.9(3) . . ? O7 Gd2 O19 127.4(2) . . ? O11 Gd2 O20 77.7(2) . . ? O18 Gd2 O20 84.4(2) . . ? O15 Gd2 O20 122.1(2) . . ? O25 Gd2 O20 142.6(2) . . ? O23 Gd2 O20 72.4(3) . . ? O7 Gd2 O20 143.7(2) . . ? O19 Gd2 O20 50.3(2) . . ? O11 Gd2 O22 137.4(3) . . ? O18 Gd2 O22 72.1(3) . . ? O15 Gd2 O22 133.5(3) . . ? O25 Gd2 O22 74.1(3) . . ? O23 Gd2 O22 52.4(3) . . ? O7 Gd2 O22 128.0(2) . . ? O19 Gd2 O22 104.6(3) . . ? O20 Gd2 O22 70.6(3) . . ? O5 Co1 O13 97.8(3) 2_666 . ? O5 Co1 O8 99.8(2) 2_666 . ? O13 Co1 O8 92.7(2) . . ? O5 Co1 O1 96.8(3) 2_666 . ? O13 Co1 O1 163.1(3) . . ? O8 Co1 O1 93.1(2) . . ? O5 Co1 O4 168.1(2) 2_666 . ? O13 Co1 O4 88.9(2) . . ? O8 Co1 O4 89.7(2) . . ? O1 Co1 O4 75.3(2) . . ? O5 Co1 O1 74.9(2) 2_666 2_666 ? O13 Co1 O1 89.2(2) . 2_666 ? O8 Co1 O1 174.6(2) . 2_666 ? O1 Co1 O1 86.4(2) . 2_666 ? O4 Co1 O1 95.4(2) . 2_666 ? O4 Co2 O1 88.1(3) . . ? O4 Co2 O5 94.0(3) . . ? O1 Co2 O5 85.7(3) . . ? O4 Co2 O2 85.1(3) . . ? O1 Co2 O2 93.2(3) . . ? O5 Co2 O2 178.6(3) . . ? O4 Co2 N1 167.1(3) . . ? O1 Co2 N1 82.9(3) . . ? O5 Co2 N1 94.5(3) . . ? O2 Co2 N1 86.2(3) . . ? O4 Co2 N2 83.7(3) . . ? O1 Co2 N2 166.9(3) . . ? O5 Co2 N2 84.7(3) . . ? O2 Co2 N2 96.3(3) . . ? N1 Co2 N2 106.8(4) . . ? O11 Co3 O10 87.9(3) . . ? O11 Co3 O17 92.1(3) . . ? O10 Co3 O17 175.7(3) . . ? O11 Co3 O7 90.3(3) . . ? O10 Co3 O7 88.4(3) . . ? O17 Co3 O7 95.9(3) . . ? O11 Co3 N4 85.9(3) . . ? O10 Co3 N4 83.2(3) . . ? O17 Co3 N4 92.6(3) . . ? O7 Co3 N4 170.9(3) . . ? O11 Co3 N3 175.6(3) . . ? O10 Co3 N3 93.0(3) . . ? O17 Co3 N3 87.4(3) . . ? O7 Co3 N3 85.5(3) . . ? N4 Co3 N3 98.5(4) . . ? C1 N1 Co2 98.4(5) . . ? C1 N1 H11 113(5) . . ? Co2 N1 H11 111(5) . . ? C1 N1 H12 104(6) . . ? Co2 N1 H12 129(6) . . ? H11 N1 H12 102(7) . . ? N1 C1 C4 114.1(8) . . ? N1 C1 C3 105.5(8) . . ? C4 C1 C3 110.3(8) . . ? N1 C1 C2 105.1(7) . . ? C4 C1 C2 111.8(8) . . ? C3 C1 C2 109.8(7) . . ? O1 C2 C1 108.7(7) . . ? O1 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? O1 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.3 . . ? C2 O1 Co2 109.3(5) . . ? C2 O1 Co1 129.8(5) . . ? Co2 O1 Co1 98.5(3) . . ? C2 O1 Co1 123.1(5) . 2_666 ? Co2 O1 Co1 95.4(3) . 2_666 ? Co1 O1 Co1 93.6(2) . 2_666 ? O2 C3 C1 108.5(8) . . ? O2 C3 H3A 110.0 . . ? C1 C3 H3A 110.0 . . ? O2 C3 H3B 110.0 . . ? C1 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? C3 O2 Co2 109.7(5) . . ? C3 O2 Gd1 133.2(5) . . ? Co2 O2 Gd1 107.4(3) . . ? O3 C4 C1 114.3(9) . . ? O3 C4 H4A 108.7 . . ? C1 C4 H4A 108.7 . . ? O3 C4 H4B 108.7 . . ? C1 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C4 O3 H3 109.5 . . ? C5 N2 Co2 97.2(5) . . ? C5 N2 H21 103(6) . . ? Co2 N2 H21 117(6) . . ? C5 N2 H22 107(7) . . ? Co2 N2 H22 127(6) . . ? H21 N2 H22 103(8) . . ? C8 C5 C6 110.3(8) . . ? C8 C5 N2 112.8(8) . . ? C6 C5 N2 107.3(8) . . ? C8 C5 C7 111.5(8) . . ? C6 C5 C7 110.7(8) . . ? N2 C5 C7 104.0(8) . . ? O4 C6 C5 108.1(7) . . ? O4 C6 H6A 110.1 . . ? C5 C6 H6A 110.1 . . ? O4 C6 H6B 110.1 . . ? C5 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? C6 O4 Co2 110.5(5) . . ? C6 O4 Co1 129.0(5) . . ? Co2 O4 Co1 98.1(3) . . ? C6 O4 Gd1 121.3(5) . . ? Co2 O4 Gd1 102.3(3) . . ? Co1 O4 Gd1 90.8(2) . . ? O5 C7 C5 106.9(7) . . ? O5 C7 H7A 110.3 . . ? C5 C7 H7A 110.3 . . ? O5 C7 H7B 110.3 . . ? C5 C7 H7B 110.3 . . ? H7A C7 H7B 108.6 . . ? C7 O5 Co2 111.6(5) . . ? C7 O5 Co1 133.3(6) . 2_666 ? Co2 O5 Co1 104.0(3) . 2_666 ? O6 C8 C5 112.6(9) . . ? O6 C8 H8A 109.1 . . ? C5 C8 H8A 109.1 . . ? O6 C8 H8B 109.1 . . ? C5 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C8 O6 H6 109.5 . . ? C9 N3 Co3 112.1(6) . . ? C9 N3 H31 123(7) . . ? Co3 N3 H31 107(6) . . ? C9 N3 H32 100(6) . . ? Co3 N3 H32 118(6) . . ? H31 N3 H32 97(8) . . ? N3 C9 C12 108.5(8) . . ? N3 C9 C11 109.0(8) . . ? C12 C9 C11 110.1(8) . . ? N3 C9 C10 106.3(7) . . ? C12 C9 C10 111.1(8) . . ? C11 C9 C10 111.6(8) . . ? O7 C10 C9 112.9(7) . . ? O7 C10 H10A 109.0 . . ? C9 C10 H10A 109.0 . . ? O7 C10 H10B 109.0 . . ? C9 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C10 O7 Co3 107.4(5) . . ? C10 O7 Gd1 114.3(5) . . ? Co3 O7 Gd1 98.0(2) . . ? C10 O7 Gd2 129.0(5) . . ? Co3 O7 Gd2 94.7(2) . . ? Gd1 O7 Gd2 107.0(2) . . ? O8 C11 C9 113.6(8) . . ? O8 C11 H11A 108.8 . . ? C9 C11 H11A 108.8 . . ? O8 C11 H11B 108.8 . . ? C9 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C11 O8 Co1 114.6(5) . . ? C11 O8 Gd1 137.2(5) . . ? Co1 O8 Gd1 99.1(3) . . ? O9B C12 C9 114.8(16) . . ? O9A C12 C9 115.5(10) . . ? O9A C12 H12A 108.4 . . ? C9 C12 H12A 108.4 . . ? O9A C12 H12B 108.4 . . ? C9 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? C9 C12 H12C 108.3 . . ? H12A C12 H12C 114.4 . . ? C9 C12 H12D 108.2 . . ? H12C C12 H12D 107.3 . . ? C12 O9A H9A 109.5 . . ? C12 O9B H9B 109.5 . . ? C13 N4 Co3 99.8(6) . . ? C13 N4 H41 99(6) . . ? Co3 N4 H41 113(6) . . ? C13 N4 H42 109(6) . . ? Co3 N4 H42 107(6) . . ? H41 N4 H42 126(9) . . ? C16 C13 N4 112.6(9) . . ? C16 C13 C15 111.9(8) . . ? N4 C13 C15 104.9(7) . . ? C16 C13 C14 113.5(8) . . ? N4 C13 C14 103.8(8) . . ? C15 C13 C14 109.4(9) . . ? O10 C14 C13 109.1(8) . . ? O10 C14 H14A 109.9 . . ? C13 C14 H14A 109.9 . . ? O10 C14 H14B 109.9 . . ? C13 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? C14 O10 Co3 111.0(5) . . ? C14 O10 Gd1 137.3(6) . . ? Co3 O10 Gd1 105.7(3) . . ? O11 C15 C13 109.0(8) . . ? O11 C15 H15A 109.9 . . ? C13 C15 H15A 109.9 . . ? O11 C15 H15B 109.9 . . ? C13 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? C15 O11 Co3 109.9(5) . . ? C15 O11 Gd2 145.1(6) . . ? Co3 O11 Gd2 103.7(3) . . ? O12 C16 C13 113.1(9) . . ? O12 C16 H16A 109.0 . . ? C13 C16 H16A 109.0 . . ? O12 C16 H16B 109.0 . . ? C13 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C16 O12 H121 109.5 . . ? C17 O13 Co1 128.0(6) . . ? C17 O14 Gd1 131.0(6) . . ? O13 C17 O14 126.2(9) . . ? O13 C17 C18 116.3(9) . . ? O14 C17 C18 117.5(9) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C19 O15 Gd2 152.1(6) . . ? C19 O15 Gd1 94.6(6) . . ? Gd2 O15 Gd1 112.7(3) . . ? C19 O16 Gd1 95.0(6) . . ? O16 C19 O15 117.7(9) . . ? O16 C19 C20 123.0(9) . . ? O15 C19 C20 119.3(9) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C21 O17 Co3 127.0(7) . . ? C21 O18 Gd2 134.1(6) . . ? O18 C21 O17 125.3(9) . . ? O18 C21 C22 119.5(9) . . ? O17 C21 C22 115.1(10) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O21 N5 O19 122.4(10) . . ? O21 N5 O20 120.7(9) . . ? O19 N5 O20 116.9(9) . . ? N5 O19 Gd2 96.5(6) . . ? N5 O20 Gd2 96.3(6) . . ? O24 N6 O22 119.9(11) . . ? O24 N6 O23 121.0(11) . . ? O22 N6 O23 119.1(10) . . ? N6 O22 Gd2 93.5(6) . . ? N6 O23 Gd2 94.7(6) . . ? C23A O25 Gd2 133.9(14) . . ? C23A O25 H25 113.1 . . ? Gd2 O25 H25 113.1 . . ? O25 C23A H23A 109.5 . . ? O25 C23A H23B 109.5 . . ? H23A C23A H23B 109.5 . . ? O25 C23A H23C 109.5 . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? O27 N8 O28 103(2) . . ? O27 N8 O26 134(2) . . ? O28 N8 O26 122(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H11 O13 0.96(4) 2.30(6) 3.134(10) 144(7) 2_666 N1 H12 O31A 0.87(4) 2.16(5) 3.005(18) 165(8) 2_657 N1 H12 O31B 0.87(4) 2.16(5) 3.00(2) 162(8) 2_657 O3 H3 N1 0.84 2.58 2.922(12) 105.8 . N2 H21 O16 0.92(4) 2.15(6) 2.964(10) 148(8) . N2 H22 O42 0.90(4) 2.10(5) 2.950(14) 156(8) . O6 H6 O21 0.84 2.19 2.907(11) 142.9 2_657 N3 H31 O27 0.87(4) 2.34(6) 3.097(19) 144(8) . N3 H32 O6 0.96(4) 2.08(6) 2.941(12) 149(8) 1_455 O9A H9A O6 0.84 2.62 3.326(16) 142.6 1_455 O9B H9B O32B 0.84 2.08 2.90(4) 166.3 2_567 N4 H41 O20 0.92(4) 2.29(5) 3.170(10) 160(8) 2_557 N4 H42 O26 0.92(4) 2.17(4) 3.074(17) 170(8) . O12 H121 O32A 0.84 1.99 2.786(18) 158.0 2_657 O25 H25 O14 0.95 1.92 2.754(9) 145.3 . _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 68.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.867 _refine_diff_density_min -1.624 _refine_diff_density_rms 0.159 ############################################################## data_hua374 _database_code_depnum_ccdc_archive 'CCDC 758592' #TrackingRef 'hua_co6ln4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H98 Co6 Dy4 N12 O50, 2(N O3), 6(H2 O), 4(C H4 O)' _chemical_formula_sum 'C50 H126 Co6 Dy4 N14 O66' _chemical_formula_weight 2983.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8569(15) _cell_length_b 13.6424(16) _cell_length_c 16.3608(19) _cell_angle_alpha 72.386(2) _cell_angle_beta 71.502(2) _cell_angle_gamma 73.644(2) _cell_volume 2538.5(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10112 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.98 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.951 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1478 _exptl_absorpt_coefficient_mu 3.968 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.315 _exptl_absorpt_correction_T_max 0.539 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker AXS Inc., 2005)' _exptl_special_details ; Several crystals were investigated; all showed poorly-resolved twinning to a certain extent, such that it did not prove possible to integrate the datasets with two twin domains, in consequence of the large proportion of overlapped reflections. The crystal used here showed only minor twinning, and could be refined satisfactorily, albeit with rather large residual density peaks near the Dy centres. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17186 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.98 _reflns_number_total 10754 _reflns_number_gt 8149 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_data_reduction 'SAINT+ 6.45 (Bruker AXS Inc., 2003)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The larger than normal residual electron density peaks were near the Dy atoms, and result from the small degree of twinning found for this crystal (see above). A ligand hydroxyl group, the terminal methanol ligand, the nitrate counterion and the lattice solvent molecules showed two-fold disorder and were refined using partial isotropic atoms, with geometrical restraints as appropriate. N-H and O-H H atoms were refined with their respective X-H distances restrained to 0.88(4) Ang. The refined structure contains a void of ca. 110 Ang^3^ which presumably contains the two lattice MeOH molecules found in the Co6Y4 analogue, but missing here. The formulation given here only includes the lattice solvent that was located and refined. ; _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^)+(0.1178P)^2^+13.5861P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10754 _refine_ls_number_parameters 642 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1899 _refine_ls_wR_factor_gt 0.1669 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.071 _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 0.34135(3) 0.29285(3) 0.74065(2) 0.02335(13) Uani 1 1 d . . . Dy2 Dy 0.14336(3) 0.21957(3) 0.98729(3) 0.02760(14) Uani 1 1 d . C . Co1 Co 0.39028(9) 0.49953(8) 0.57998(7) 0.0229(2) Uani 1 1 d . . . Co2 Co 0.57190(9) 0.30218(8) 0.56723(7) 0.0232(2) Uani 1 1 d . . . Co3 Co 0.10137(9) 0.20700(9) 0.80377(7) 0.0259(3) Uani 1 1 d . . . N1 N 0.6148(6) 0.2242(6) 0.4763(5) 0.0291(16) Uani 1 1 d D . . H11 H 0.657(7) 0.162(4) 0.489(7) 0.035 Uiso 1 1 d D . . H12 H 0.648(8) 0.260(7) 0.424(4) 0.035 Uiso 1 1 d D . . C1 C 0.4998(7) 0.2253(7) 0.4726(6) 0.0269(18) Uani 1 1 d . . . C2 C 0.4435(7) 0.3428(7) 0.4502(6) 0.0264(17) Uani 1 1 d . . . H2C H 0.4625 0.3712 0.3852 0.032 Uiso 1 1 calc R . . H2D H 0.3610 0.3512 0.4718 0.032 Uiso 1 1 calc R . . O1 O 0.4832(5) 0.3995(5) 0.4927(4) 0.0260(13) Uani 1 1 d . . . C3 C 0.4434(7) 0.1728(7) 0.5665(6) 0.0288(18) Uani 1 1 d . . . H3C H 0.3620 0.1831 0.5731 0.035 Uiso 1 1 calc R . . H3D H 0.4753 0.0964 0.5789 0.035 Uiso 1 1 calc R . . O2 O 0.4616(5) 0.2187(4) 0.6271(4) 0.0245(12) Uani 1 1 d . . . C4 C 0.4983(9) 0.1661(8) 0.4064(6) 0.038(2) Uani 1 1 d . . . H4C H 0.5250 0.0898 0.4286 0.046 Uiso 1 1 calc R . . H4D H 0.4202 0.1771 0.4028 0.046 Uiso 1 1 calc R . . O3 O 0.5651(7) 0.1991(7) 0.3218(5) 0.052(2) Uani 1 1 d . . . H3 H 0.5333 0.2007 0.2837 0.077 Uiso 1 1 calc R . . N2 N 0.6691(6) 0.2321(6) 0.6455(5) 0.0302(16) Uani 1 1 d D . . H21 H 0.740(4) 0.202(8) 0.630(7) 0.036 Uiso 1 1 d D . . H22 H 0.634(8) 0.193(7) 0.696(4) 0.036 Uiso 1 1 d D . . C5 C 0.6913(7) 0.3285(7) 0.6600(6) 0.032(2) Uani 1 1 d . . . C6 C 0.5752(8) 0.3920(7) 0.6957(6) 0.0306(19) Uani 1 1 d . . . H6A H 0.5503 0.3656 0.7607 0.037 Uiso 1 1 calc R . . H6B H 0.5786 0.4668 0.6833 0.037 Uiso 1 1 calc R . . O4 O 0.4973(5) 0.3821(4) 0.6541(4) 0.0240(12) Uani 1 1 d . . . C7 C 0.7445(8) 0.3857(7) 0.5659(6) 0.032(2) Uani 1 1 d . . . H7A H 0.7453 0.4584 0.5652 0.038 Uiso 1 1 calc R . . H7B H 0.8228 0.3487 0.5458 0.038 Uiso 1 1 calc R . . O5 O 0.6798(5) 0.3876(4) 0.5085(4) 0.0253(12) Uani 1 1 d . . . C8 C 0.7658(9) 0.3028(9) 0.7224(7) 0.045(3) Uani 1 1 d . . . H8A H 0.7698 0.3689 0.7335 0.053 Uiso 1 1 calc R . . H8B H 0.7315 0.2589 0.7798 0.053 Uiso 1 1 calc R . . O6 O 0.8769(7) 0.2485(6) 0.6889(6) 0.056(2) Uani 1 1 d . . . H6 H 0.8761 0.1859 0.6927 0.084 Uiso 1 1 calc R . . N3 N 0.0715(6) 0.3118(6) 0.6983(5) 0.0285(16) Uani 1 1 d D . . H31 H 0.009(5) 0.301(8) 0.695(7) 0.034 Uiso 1 1 d D . . H32 H 0.124(6) 0.293(8) 0.652(5) 0.034 Uiso 1 1 d D . . C9 C 0.0619(7) 0.4215(7) 0.7063(6) 0.0304(19) Uani 1 1 d . B . C10 C 0.0734(7) 0.4134(7) 0.7987(6) 0.0299(19) Uani 1 1 d . . . H10A H 0.1052 0.4725 0.7966 0.036 Uiso 1 1 calc R . . H10B H -0.0016 0.4186 0.8409 0.036 Uiso 1 1 calc R . . O7 O 0.1447(5) 0.3155(4) 0.8290(4) 0.0259(12) Uani 1 1 d . . . C11 C 0.1561(7) 0.4686(7) 0.6332(7) 0.033(2) Uani 1 1 d . . . H11A H 0.1465 0.4720 0.5747 0.040 Uiso 1 1 calc R . . H11B H 0.1494 0.5414 0.6369 0.040 Uiso 1 1 calc R . . O8 O 0.2651(5) 0.4100(4) 0.6395(4) 0.0248(12) Uani 1 1 d . . . C12 C -0.0512(8) 0.4869(8) 0.6943(7) 0.045(3) Uani 1 1 d D . . H12A H -0.1101 0.4583 0.7447 0.054 Uiso 0.79 1 calc PR A 1 H12B H -0.0556 0.5594 0.6971 0.054 Uiso 0.79 1 calc PR A 1 H12C H -0.0595 0.4871 0.6361 0.054 Uiso 0.21 1 d PR A 2 H12D H -0.1109 0.4548 0.7410 0.054 Uiso 0.21 1 d PR A 2 O9A O -0.0750(8) 0.4913(8) 0.6165(7) 0.051(2) Uiso 0.79 1 d PD B 1 H9A H -0.0737 0.4304 0.6139 0.077 Uiso 0.79 1 calc PR B 1 O9B O -0.063(4) 0.587(2) 0.699(3) 0.072(12) Uiso 0.21 1 d PD B 2 H9B H -0.0121 0.6144 0.6587 0.108 Uiso 0.21 1 calc PR B 2 N4 N 0.0836(7) 0.0857(6) 0.7754(5) 0.0322(17) Uani 1 1 d D . . H41 H 0.097(9) 0.114(8) 0.719(3) 0.039 Uiso 1 1 d D . . H42 H 0.027(6) 0.061(8) 0.815(5) 0.039 Uiso 1 1 d D . . C13 C 0.1789(7) 0.0077(7) 0.8061(6) 0.033(2) Uani 1 1 d . . . C14 C 0.2831(8) 0.0553(7) 0.7510(7) 0.035(2) Uani 1 1 d . . . H14A H 0.3457 0.0226 0.7798 0.042 Uiso 1 1 calc R . . H14B H 0.3074 0.0422 0.6908 0.042 Uiso 1 1 calc R . . O10 O 0.2534(5) 0.1651(5) 0.7458(4) 0.0291(13) Uani 1 1 d . . . C15 C 0.1565(8) 0.0074(7) 0.9033(6) 0.033(2) Uani 1 1 d . . . H15A H 0.0925 -0.0266 0.9391 0.040 Uiso 1 1 calc R . . H15B H 0.2232 -0.0324 0.9256 0.040 Uiso 1 1 calc R . . O11 O 0.1316(5) 0.1136(5) 0.9105(4) 0.0296(13) Uani 1 1 d . . . C16 C 0.1905(8) -0.1018(8) 0.7943(7) 0.040(2) Uani 1 1 d . . . H16A H 0.2523 -0.1503 0.8191 0.048 Uiso 1 1 calc R . . H16B H 0.1205 -0.1273 0.8281 0.048 Uiso 1 1 calc R . . O12 O 0.2123(7) -0.1039(6) 0.7046(5) 0.0505(19) Uani 1 1 d D . . H121 H 0.282(4) -0.141(9) 0.696(10) 0.076 Uiso 1 1 d D . . O13 O 0.3377(5) 0.5796(5) 0.6784(4) 0.0309(14) Uani 1 1 d . . . O14 O 0.3115(5) 0.4442(5) 0.7988(4) 0.0295(13) Uani 1 1 d . . . C17 C 0.3099(7) 0.5424(7) 0.7618(6) 0.0272(18) Uani 1 1 d . . . C18 C 0.2722(11) 0.6185(8) 0.8200(7) 0.054(3) Uani 1 1 d . . . H18A H 0.3172 0.6729 0.7949 0.081 Uiso 1 1 calc R . . H18B H 0.2817 0.5812 0.8794 0.081 Uiso 1 1 calc R . . H18C H 0.1930 0.6512 0.8238 0.081 Uiso 1 1 calc R . . O15 O 0.3277(5) 0.2186(5) 0.9006(4) 0.0325(14) Uani 1 1 d . . . O16 O 0.4938(6) 0.1898(6) 0.8118(5) 0.0453(18) Uani 1 1 d . . . C19 C 0.4341(8) 0.1851(8) 0.8900(6) 0.037(2) Uani 1 1 d . . . C20 C 0.4829(9) 0.1486(11) 0.9666(8) 0.059(3) Uani 1 1 d . . . H20A H 0.5640 0.1238 0.9467 0.089 Uiso 1 1 calc R . . H20B H 0.4493 0.0908 1.0092 0.089 Uiso 1 1 calc R . . H20C H 0.4678 0.2066 0.9950 0.089 Uiso 1 1 calc R . . O17 O -0.0553(5) 0.2425(5) 0.8598(4) 0.0299(13) Uani 1 1 d . . . O18 O -0.0446(5) 0.2669(5) 0.9869(4) 0.0305(13) Uani 1 1 d . . . C21 C -0.0979(7) 0.2611(6) 0.9368(6) 0.0272(18) Uani 1 1 d . . . C22 C -0.2248(8) 0.2812(8) 0.9662(6) 0.038(2) Uani 1 1 d . . . H22A H -0.2494 0.2751 1.0303 0.057 Uiso 1 1 calc R . . H22B H -0.2513 0.2294 0.9517 0.057 Uiso 1 1 calc R . . H22C H -0.2557 0.3520 0.9355 0.057 Uiso 1 1 calc R . . N5 N 0.1832(7) 0.0069(6) 1.0986(6) 0.0395(19) Uani 1 1 d . . . O19 O 0.2619(6) 0.0436(5) 1.0377(5) 0.0402(16) Uani 1 1 d . . . O20 O 0.0864(5) 0.0671(6) 1.1063(5) 0.0407(16) Uani 1 1 d . . . O21 O 0.1981(8) -0.0823(6) 1.1462(7) 0.070(3) Uani 1 1 d . . . N6 N 0.1187(10) 0.2573(9) 1.1576(7) 0.058(3) Uani 1 1 d . . . O22 O 0.0371(6) 0.2796(7) 1.1263(5) 0.0481(18) Uani 1 1 d . . . O23 O 0.2143(7) 0.2175(7) 1.1128(5) 0.0509(19) Uani 1 1 d . . . O24 O 0.1113(10) 0.2699(13) 1.2317(9) 0.118(5) Uani 1 1 d . . . O25 O 0.1644(6) 0.3963(6) 0.9629(5) 0.0438(18) Uani 1 1 d D . . H25 H 0.215(7) 0.433(8) 0.928(6) 0.053 Uiso 1 1 d D . . C23A C 0.136(2) 0.474(2) 1.0148(18) 0.083(7) Uiso 0.65 1 d PD C -1 H23A H 0.1583 0.5391 0.9763 0.124 Uiso 0.65 1 calc PR C -1 H23B H 0.1754 0.4472 1.0620 0.124 Uiso 0.65 1 calc PR C -1 H23C H 0.0549 0.4878 1.0411 0.124 Uiso 0.65 1 calc PR C -1 C23B C 0.080(3) 0.487(3) 0.986(4) 0.087(14) Uiso 0.35 1 d PD . -2 H23D H 0.1137 0.5492 0.9645 0.130 Uiso 0.35 1 calc PR . -2 H23E H 0.0514 0.4739 1.0509 0.130 Uiso 0.35 1 calc PR . -2 H23F H 0.0182 0.4988 0.9593 0.130 Uiso 0.35 1 calc PR . -2 N31A N 0.136(5) 0.232(3) 0.508(4) 0.35(3) Uiso 0.65 1 d PDU D 1 O31A O 0.1542(14) 0.1521(11) 0.5713(10) 0.067(4) Uiso 0.65 1 d PDU D 1 O32A O 0.1651(17) 0.3157(13) 0.5017(13) 0.101(6) Uiso 0.65 1 d PDU D 1 O33A O 0.057(4) 0.242(3) 0.470(3) 0.28(2) Uiso 0.65 1 d PDU D 1 N31B N 0.1258(19) 0.2464(16) 0.5013(15) 0.042(6) Uiso 0.35 1 d PDU E 2 O31B O 0.102(3) 0.1635(17) 0.5625(18) 0.077(9) Uiso 0.35 1 d PDU E 2 O32B O 0.189(4) 0.233(3) 0.426(2) 0.18(2) Uiso 0.35 1 d PDU E 2 O33B O 0.057(2) 0.3346(17) 0.5037(19) 0.079(8) Uiso 0.35 1 d PDU E 2 O41 O 0.4524(16) 0.3635(15) 0.2170(13) 0.151(6) Uiso 1 1 d . . . C41 C 0.334(2) 0.3745(19) 0.2445(17) 0.122(7) Uiso 1 1 d . . . O42A O 0.700(2) -0.108(2) 0.695(2) 0.114(9) Uiso 0.50 1 d P F 1 O42B O 0.605(4) 0.010(4) 0.690(3) 0.186(17) Uiso 0.50 1 d P F 2 C42 C 0.604(2) -0.059(2) 0.7631(17) 0.119(7) Uiso 1 1 d . . . O43A O 0.2699(18) -0.0004(16) 0.4756(14) 0.066(5) Uiso 0.50 1 d P G 1 O44A O 0.898(2) 0.069(2) 0.6231(19) 0.107(8) Uiso 0.50 1 d P H 1 O45A O 0.119(2) -0.233(2) 0.661(2) 0.108(8) Uiso 0.50 1 d P I 1 O43B O 0.2996(15) 0.0079(14) 0.4964(12) 0.054(4) Uiso 0.50 1 d P J 2 O44B O 0.884(2) 0.125(2) 0.5431(19) 0.105(8) Uiso 0.50 1 d P K 2 O45B O 0.088(3) -0.196(3) 0.601(3) 0.147(12) Uiso 0.50 1 d P L 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0245(2) 0.0208(2) 0.0208(2) -0.00468(15) 0.00725(15) -0.01344(15) Dy2 0.0274(2) 0.0283(2) 0.0230(2) -0.00587(17) 0.00666(16) -0.01450(17) Co1 0.0245(5) 0.0200(5) 0.0211(5) -0.0046(4) 0.0055(4) -0.0131(4) Co2 0.0242(5) 0.0205(5) 0.0204(5) -0.0026(4) 0.0060(4) -0.0131(4) Co3 0.0268(6) 0.0240(6) 0.0233(6) -0.0071(5) 0.0088(4) -0.0152(5) N1 0.029(4) 0.026(4) 0.029(4) -0.012(3) 0.009(3) -0.015(3) C1 0.033(4) 0.023(4) 0.024(4) -0.013(3) 0.007(3) -0.012(3) C2 0.029(4) 0.026(4) 0.024(4) -0.010(3) 0.004(3) -0.013(3) O1 0.035(3) 0.027(3) 0.017(3) -0.009(2) 0.006(2) -0.019(3) C3 0.031(4) 0.027(4) 0.025(4) -0.007(4) 0.005(3) -0.014(4) O2 0.025(3) 0.017(3) 0.025(3) -0.006(2) 0.009(2) -0.010(2) C4 0.046(5) 0.034(5) 0.033(5) -0.014(4) 0.011(4) -0.022(4) O3 0.061(5) 0.057(5) 0.038(4) -0.023(4) 0.017(4) -0.035(4) N2 0.028(4) 0.026(4) 0.027(4) 0.004(3) 0.003(3) -0.013(3) C5 0.029(4) 0.034(5) 0.030(5) 0.002(4) -0.002(4) -0.019(4) C6 0.039(5) 0.030(5) 0.023(4) -0.002(4) -0.003(4) -0.017(4) O4 0.025(3) 0.024(3) 0.022(3) -0.005(2) 0.004(2) -0.016(2) C7 0.033(4) 0.035(5) 0.028(4) 0.002(4) -0.003(4) -0.023(4) O5 0.025(3) 0.020(3) 0.023(3) 0.004(2) 0.000(2) -0.010(2) C8 0.044(5) 0.048(6) 0.037(5) 0.009(5) -0.005(4) -0.028(5) O6 0.049(4) 0.047(5) 0.073(6) -0.009(4) -0.020(4) -0.012(4) N3 0.029(4) 0.033(4) 0.022(4) -0.003(3) 0.003(3) -0.018(3) C9 0.033(4) 0.026(4) 0.027(4) -0.003(4) 0.004(4) -0.015(4) C10 0.031(4) 0.027(4) 0.029(4) -0.010(4) 0.007(4) -0.014(4) O7 0.027(3) 0.023(3) 0.023(3) -0.005(2) 0.007(2) -0.014(2) C11 0.029(4) 0.027(4) 0.038(5) 0.001(4) -0.002(4) -0.014(4) O8 0.026(3) 0.023(3) 0.021(3) -0.003(2) 0.003(2) -0.011(2) C12 0.035(5) 0.037(5) 0.052(6) -0.005(5) 0.005(5) -0.017(4) N4 0.037(4) 0.031(4) 0.023(4) -0.006(3) 0.012(3) -0.022(3) C13 0.029(4) 0.021(4) 0.038(5) -0.009(4) 0.015(4) -0.017(4) C14 0.033(5) 0.026(4) 0.035(5) -0.008(4) 0.013(4) -0.015(4) O10 0.029(3) 0.023(3) 0.030(3) -0.007(2) 0.009(2) -0.016(2) C15 0.038(5) 0.022(4) 0.036(5) -0.007(4) 0.005(4) -0.016(4) O11 0.033(3) 0.024(3) 0.026(3) -0.005(2) 0.006(2) -0.011(3) C16 0.033(5) 0.033(5) 0.049(6) -0.015(4) 0.010(4) -0.016(4) O12 0.060(5) 0.042(4) 0.049(4) -0.022(4) 0.006(4) -0.021(4) O13 0.035(3) 0.029(3) 0.026(3) -0.009(3) 0.012(3) -0.021(3) O14 0.036(3) 0.025(3) 0.026(3) -0.006(3) 0.005(3) -0.016(3) C17 0.025(4) 0.029(4) 0.026(4) -0.005(4) 0.002(3) -0.013(3) C18 0.085(9) 0.034(5) 0.037(6) -0.015(5) 0.014(6) -0.029(6) O15 0.030(3) 0.036(3) 0.026(3) -0.002(3) 0.004(3) -0.016(3) O16 0.035(4) 0.049(4) 0.034(4) -0.004(3) 0.017(3) -0.016(3) C19 0.034(5) 0.040(5) 0.026(5) 0.003(4) 0.005(4) -0.018(4) C20 0.038(6) 0.083(9) 0.038(6) 0.012(6) -0.004(5) -0.019(6) O17 0.030(3) 0.030(3) 0.028(3) -0.011(3) 0.007(3) -0.015(3) O18 0.027(3) 0.031(3) 0.031(3) -0.011(3) 0.005(3) -0.012(3) C21 0.028(4) 0.020(4) 0.027(4) -0.004(3) 0.004(3) -0.009(3) C22 0.033(5) 0.046(6) 0.030(5) -0.012(4) 0.007(4) -0.017(4) N5 0.038(4) 0.032(4) 0.042(5) -0.001(4) 0.004(4) -0.020(4) O19 0.037(3) 0.038(4) 0.040(4) -0.002(3) 0.004(3) -0.022(3) O20 0.032(3) 0.049(4) 0.036(4) -0.004(3) 0.008(3) -0.026(3) O21 0.076(6) 0.037(4) 0.074(6) 0.013(4) -0.001(5) -0.027(4) N6 0.067(7) 0.076(7) 0.044(6) -0.032(5) -0.003(5) -0.027(6) O22 0.041(4) 0.062(5) 0.042(4) -0.023(4) 0.005(3) -0.016(4) O23 0.052(4) 0.064(5) 0.044(4) -0.017(4) -0.007(4) -0.023(4) O24 0.084(8) 0.204(16) 0.101(10) -0.103(11) -0.015(7) -0.020(9) O25 0.051(4) 0.039(4) 0.040(4) -0.020(3) 0.015(3) -0.025(3) _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 O8 2.192(6) . ? Dy1 O10 2.299(6) . ? Dy1 O2 2.302(5) . ? Dy1 O14 2.414(6) . ? Dy1 O4 2.457(5) . ? Dy1 O16 2.466(8) . ? Dy1 O7 2.467(5) . ? Dy1 O15 2.471(6) . ? Dy2 O11 2.243(6) . ? Dy2 O18 2.320(6) . ? Dy2 O15 2.343(6) . ? Dy2 O25 2.400(7) . ? Dy2 O20 2.481(6) . ? Dy2 O23 2.488(8) . ? Dy2 O22 2.497(7) . ? Dy2 O19 2.510(7) . ? Dy2 O7 2.521(6) . ? Co1 O5 1.994(6) 2_666 ? Co1 O13 2.050(6) . ? Co1 O8 2.104(5) . ? Co1 O1 2.123(6) . ? Co1 O4 2.138(6) . ? Co1 O1 2.236(5) 2_666 ? Co2 O5 1.895(5) . ? Co2 O1 1.897(6) . ? Co2 O4 1.901(6) . ? Co2 O2 1.903(5) . ? Co2 N2 1.929(8) . ? Co2 N1 1.937(7) . ? Co3 O10 1.889(6) . ? Co3 O11 1.905(6) . ? Co3 O7 1.911(6) . ? Co3 O17 1.918(6) . ? Co3 N4 1.936(8) . ? Co3 N3 1.945(8) . ? N1 C1 1.494(11) . ? N1 H11 0.87(4) . ? N1 H12 0.89(4) . ? C1 C3 1.522(11) . ? C1 C4 1.542(12) . ? C1 C2 1.545(12) . ? C2 O1 1.455(10) . ? C2 H2C 0.9900 . ? C2 H2D 0.9900 . ? O1 Co1 2.236(5) 2_666 ? C3 O2 1.427(11) . ? C3 H3C 0.9900 . ? C3 H3D 0.9900 . ? C4 O3 1.394(11) . ? C4 H4C 0.9900 . ? C4 H4D 0.9900 . ? O3 H3 0.8400 . ? N2 C5 1.520(12) . ? N2 H21 0.88(4) . ? N2 H22 0.90(4) . ? C5 C8 1.515(14) . ? C5 C6 1.530(13) . ? C5 C7 1.534(11) . ? C6 O4 1.431(10) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O5 1.431(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? O5 Co1 1.994(6) 2_666 ? C8 O6 1.429(14) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? O6 H6 0.8400 . ? N3 C9 1.508(11) . ? N3 H31 0.88(4) . ? N3 H32 0.89(4) . ? C9 C12 1.515(14) . ? C9 C10 1.533(13) . ? C9 C11 1.538(11) . ? C10 O7 1.438(11) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O8 1.423(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O9B 1.36(2) . ? C12 O9A 1.380(14) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 H12C 0.9900 . ? C12 H12D 0.9899 . ? O9A H12C 0.4101 . ? O9A H9A 0.8400 . ? O9B H9B 0.8400 . ? N4 C13 1.489(13) . ? N4 H41 0.87(4) . ? N4 H42 0.88(4) . ? C13 C15 1.522(13) . ? C13 C16 1.523(12) . ? C13 C14 1.549(11) . ? C14 O10 1.420(10) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O11 1.427(10) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O12 1.412(13) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? O12 H121 0.888(19) . ? O13 C17 1.273(10) . ? O14 C17 1.289(10) . ? C17 C18 1.497(13) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O15 C19 1.288(11) . ? O16 C19 1.259(11) . ? C19 C20 1.468(15) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? O17 C21 1.277(10) . ? O18 C21 1.254(11) . ? C21 C22 1.516(12) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? N5 O21 1.230(11) . ? N5 O19 1.270(10) . ? N5 O20 1.275(11) . ? N6 O22 1.235(13) . ? N6 O24 1.244(14) . ? N6 O23 1.280(13) . ? O25 C23A 1.45(2) . ? O25 C23B 1.46(3) . ? O25 H25 0.88(2) . ? C23A H23A 0.9800 . ? C23A H23B 0.9800 . ? C23A H23C 0.9800 . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? N31A O32A 1.266(19) . ? N31A O31A 1.286(19) . ? N31A O33A 1.297(19) . ? N31B O33B 1.280(17) . ? N31B O32B 1.284(18) . ? N31B O31B 1.301(17) . ? O41 C41 1.42(3) . ? O42A C42 1.53(4) . ? O42B C42 1.27(5) . ? 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 Dy1 O10 94.1(2) . . ? O8 Dy1 O2 86.7(2) . . ? O10 Dy1 O2 78.19(19) . . ? O8 Dy1 O14 82.5(2) . . ? O10 Dy1 O14 141.7(2) . . ? O2 Dy1 O14 139.11(18) . . ? O8 Dy1 O4 79.5(2) . . ? O10 Dy1 O4 143.53(19) . . ? O2 Dy1 O4 65.68(18) . . ? O14 Dy1 O4 73.58(19) . . ? O8 Dy1 O16 156.4(2) . . ? O10 Dy1 O16 102.2(2) . . ? O2 Dy1 O16 80.2(2) . . ? O14 Dy1 O16 94.7(2) . . ? O4 Dy1 O16 77.2(2) . . ? O8 Dy1 O7 81.7(2) . . ? O10 Dy1 O7 66.7(2) . . ? O2 Dy1 O7 141.87(19) . . ? O14 Dy1 O7 75.08(19) . . ? O4 Dy1 O7 145.15(18) . . ? O16 Dy1 O7 120.4(2) . . ? O8 Dy1 O15 146.7(2) . . ? O10 Dy1 O15 87.5(2) . . ? O2 Dy1 O15 126.0(2) . . ? O14 Dy1 O15 76.0(2) . . ? O4 Dy1 O15 117.24(19) . . ? O16 Dy1 O15 52.3(2) . . ? O7 Dy1 O15 68.4(2) . . ? O11 Dy2 O18 77.6(2) . . ? O11 Dy2 O15 87.5(2) . . ? O18 Dy2 O15 145.5(2) . . ? O11 Dy2 O25 139.1(2) . . ? O18 Dy2 O25 94.8(2) . . ? O15 Dy2 O25 76.3(2) . . ? O11 Dy2 O20 77.6(2) . . ? O18 Dy2 O20 84.1(2) . . ? O15 Dy2 O20 123.1(2) . . ? O25 Dy2 O20 142.3(2) . . ? O11 Dy2 O23 142.0(3) . . ? O18 Dy2 O23 124.0(2) . . ? O15 Dy2 O23 86.4(2) . . ? O25 Dy2 O23 75.0(3) . . ? O20 Dy2 O23 74.7(2) . . ? O11 Dy2 O22 138.3(2) . . ? O18 Dy2 O22 72.8(2) . . ? O15 Dy2 O22 132.6(2) . . ? O25 Dy2 O22 72.9(2) . . ? O20 Dy2 O22 70.8(3) . . ? O23 Dy2 O22 51.4(3) . . ? O11 Dy2 O19 73.6(2) . . ? O18 Dy2 O19 130.7(2) . . ? O15 Dy2 O19 71.9(2) . . ? O25 Dy2 O19 132.6(2) . . ? O20 Dy2 O19 51.2(2) . . ? O23 Dy2 O19 68.8(3) . . ? O22 Dy2 O19 104.8(3) . . ? O11 Dy2 O7 68.8(2) . . ? O18 Dy2 O7 76.0(2) . . ? O15 Dy2 O7 69.5(2) . . ? O25 Dy2 O7 70.4(2) . . ? O20 Dy2 O7 143.7(2) . . ? O23 Dy2 O7 141.5(2) . . ? O22 Dy2 O7 128.8(2) . . ? O19 Dy2 O7 126.2(2) . . ? O5 Co1 O13 96.9(3) 2_666 . ? O5 Co1 O8 100.7(2) 2_666 . ? O13 Co1 O8 93.3(2) . . ? O5 Co1 O1 96.2(2) 2_666 . ? O13 Co1 O1 164.3(3) . . ? O8 Co1 O1 92.8(2) . . ? O5 Co1 O4 168.1(2) 2_666 . ? O13 Co1 O4 89.1(2) . . ? O8 Co1 O4 89.2(2) . . ? O1 Co1 O4 76.5(2) . . ? O5 Co1 O1 74.8(2) 2_666 2_666 ? O13 Co1 O1 88.9(2) . 2_666 ? O8 Co1 O1 175.2(2) . 2_666 ? O1 Co1 O1 86.3(2) . 2_666 ? O4 Co1 O1 95.1(2) . 2_666 ? O5 Co2 O1 85.6(2) . . ? O5 Co2 O4 93.4(2) . . ? O1 Co2 O4 88.0(2) . . ? O5 Co2 O2 178.9(3) . . ? O1 Co2 O2 93.9(2) . . ? O4 Co2 O2 85.6(2) . . ? O5 Co2 N2 84.7(3) . . ? O1 Co2 N2 166.8(3) . . ? O4 Co2 N2 83.6(3) . . ? O2 Co2 N2 95.7(3) . . ? O5 Co2 N1 94.9(3) . . ? O1 Co2 N1 83.1(3) . . ? O4 Co2 N1 167.3(3) . . ? O2 Co2 N1 86.0(3) . . ? N2 Co2 N1 106.6(4) . . ? O10 Co3 O11 88.4(3) . . ? O10 Co3 O7 87.3(2) . . ? O11 Co3 O7 90.1(3) . . ? O10 Co3 O17 176.0(3) . . ? O11 Co3 O17 91.9(3) . . ? O7 Co3 O17 96.6(2) . . ? O10 Co3 N4 83.7(3) . . ? O11 Co3 N4 86.4(3) . . ? O7 Co3 N4 170.4(3) . . ? O17 Co3 N4 92.4(3) . . ? O10 Co3 N3 92.3(3) . . ? O11 Co3 N3 175.2(3) . . ? O7 Co3 N3 85.3(3) . . ? O17 Co3 N3 87.6(3) . . ? N4 Co3 N3 98.3(3) . . ? C1 N1 Co2 98.1(5) . . ? C1 N1 H11 115(7) . . ? Co2 N1 H11 114(7) . . ? C1 N1 H12 107(7) . . ? Co2 N1 H12 112(7) . . ? H11 N1 H12 110(10) . . ? N1 C1 C3 104.7(7) . . ? N1 C1 C4 114.0(7) . . ? C3 C1 C4 110.0(7) . . ? N1 C1 C2 105.1(6) . . ? C3 C1 C2 110.1(7) . . ? C4 C1 C2 112.5(8) . . ? O1 C2 C1 108.7(7) . . ? O1 C2 H2C 109.9 . . ? C1 C2 H2C 109.9 . . ? O1 C2 H2D 109.9 . . ? C1 C2 H2D 109.9 . . ? H2C C2 H2D 108.3 . . ? C2 O1 Co2 109.4(5) . . ? C2 O1 Co1 129.5(5) . . ? Co2 O1 Co1 98.1(2) . . ? C2 O1 Co1 123.6(4) . 2_666 ? Co2 O1 Co1 95.5(2) . 2_666 ? Co1 O1 Co1 93.7(2) . 2_666 ? O2 C3 C1 108.6(6) . . ? O2 C3 H3C 110.0 . . ? C1 C3 H3C 110.0 . . ? O2 C3 H3D 110.0 . . ? C1 C3 H3D 110.0 . . ? H3C C3 H3D 108.4 . . ? C3 O2 Co2 110.0(5) . . ? C3 O2 Dy1 132.4(5) . . ? Co2 O2 Dy1 107.2(2) . . ? O3 C4 C1 112.6(7) . . ? O3 C4 H4C 109.1 . . ? C1 C4 H4C 109.1 . . ? O3 C4 H4D 109.1 . . ? C1 C4 H4D 109.1 . . ? H4C C4 H4D 107.8 . . ? C4 O3 H3 109.5 . . ? C5 N2 Co2 98.6(5) . . ? C5 N2 H21 95(7) . . ? Co2 N2 H21 127(7) . . ? C5 N2 H22 112(7) . . ? Co2 N2 H22 112(7) . . ? H21 N2 H22 110(9) . . ? C8 C5 N2 113.6(8) . . ? C8 C5 C6 111.7(8) . . ? N2 C5 C6 105.0(6) . . ? C8 C5 C7 112.4(7) . . ? N2 C5 C7 103.1(7) . . ? C6 C5 C7 110.4(8) . . ? O4 C6 C5 109.4(7) . . ? O4 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? O4 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? C6 O4 Co2 110.4(5) . . ? C6 O4 Co1 130.6(5) . . ? Co2 O4 Co1 97.4(2) . . ? C6 O4 Dy1 120.9(5) . . ? Co2 O4 Dy1 101.5(2) . . ? Co1 O4 Dy1 90.6(2) . . ? O5 C7 C5 108.2(6) . . ? O5 C7 H7A 110.0 . . ? C5 C7 H7A 110.0 . . ? O5 C7 H7B 110.0 . . ? C5 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? C7 O5 Co2 111.3(4) . . ? C7 O5 Co1 134.0(5) . 2_666 ? Co2 O5 Co1 104.1(3) . 2_666 ? O6 C8 C5 113.3(9) . . ? O6 C8 H8A 108.9 . . ? C5 C8 H8A 108.9 . . ? O6 C8 H8B 108.9 . . ? C5 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C8 O6 H6 109.5 . . ? C9 N3 Co3 111.5(6) . . ? C9 N3 H31 113(7) . . ? Co3 N3 H31 103(7) . . ? C9 N3 H32 115(7) . . ? Co3 N3 H32 107(7) . . ? H31 N3 H32 105(9) . . ? N3 C9 C12 108.9(7) . . ? N3 C9 C10 107.8(7) . . ? C12 C9 C10 110.7(8) . . ? N3 C9 C11 108.3(7) . . ? C12 C9 C11 110.0(7) . . ? C10 C9 C11 111.1(7) . . ? O7 C10 C9 110.8(7) . . ? O7 C10 H10A 109.5 . . ? C9 C10 H10A 109.5 . . ? O7 C10 H10B 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? C10 O7 Co3 107.5(5) . . ? C10 O7 Dy1 115.0(4) . . ? Co3 O7 Dy1 99.2(2) . . ? C10 O7 Dy2 127.2(5) . . ? Co3 O7 Dy2 94.3(2) . . ? Dy1 O7 Dy2 107.8(2) . . ? O8 C11 C9 113.1(7) . . ? O8 C11 H11A 109.0 . . ? C9 C11 H11A 109.0 . . ? O8 C11 H11B 109.0 . . ? C9 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C11 O8 Co1 113.5(5) . . ? C11 O8 Dy1 137.2(5) . . ? Co1 O8 Dy1 99.3(2) . . ? O9B C12 C9 111(2) . . ? O9A C12 C9 115.7(9) . . ? C9 C12 H12A 108.4 . . ? O9A C12 H12B 108.4 . . ? C9 C12 H12B 108.4 . . ? H12A C12 H12B 107.4 . . ? O9B C12 H12C 109.1 . . ? C9 C12 H12C 109.7 . . ? O9B C12 H12D 109.8 . . ? C9 C12 H12D 109.0 . . ? H12C C12 H12D 108.0 . . ? C12 O9A H9A 109.5 . . ? C12 O9B H9B 109.5 . . ? C13 N4 Co3 98.6(5) . . ? C13 N4 H41 116(7) . . ? Co3 N4 H41 93(7) . . ? C13 N4 H42 100(7) . . ? Co3 N4 H42 109(7) . . ? H41 N4 H42 134(10) . . ? N4 C13 C15 105.2(7) . . ? N4 C13 C16 113.4(8) . . ? C15 C13 C16 111.5(8) . . ? N4 C13 C14 104.3(7) . . ? C15 C13 C14 109.9(8) . . ? C16 C13 C14 112.1(7) . . ? O10 C14 C13 108.1(7) . . ? O10 C14 H14A 110.1 . . ? C13 C14 H14A 110.1 . . ? O10 C14 H14B 110.1 . . ? C13 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? C14 O10 Co3 111.6(5) . . ? C14 O10 Dy1 136.6(5) . . ? Co3 O10 Dy1 105.9(3) . . ? O11 C15 C13 108.3(7) . . ? O11 C15 H15A 110.0 . . ? C13 C15 H15A 110.0 . . ? O11 C15 H15B 110.0 . . ? C13 C15 H15B 110.0 . . ? H15A C15 H15B 108.4 . . ? C15 O11 Co3 110.1(5) . . ? C15 O11 Dy2 144.6(6) . . ? Co3 O11 Dy2 104.0(3) . . ? O12 C16 C13 112.7(8) . . ? O12 C16 H16A 109.1 . . ? C13 C16 H16A 109.1 . . ? O12 C16 H16B 109.1 . . ? C13 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? C16 O12 H121 100(10) . . ? C17 O13 Co1 127.8(6) . . ? C17 O14 Dy1 132.8(6) . . ? O13 C17 O14 124.3(8) . . ? O13 C17 C18 117.3(8) . . ? O14 C17 C18 118.4(8) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C19 O15 Dy2 150.9(6) . . ? C19 O15 Dy1 94.3(5) . . ? Dy2 O15 Dy1 113.6(3) . . ? C19 O16 Dy1 95.4(6) . . ? O16 C19 O15 117.3(9) . . ? O16 C19 C20 122.1(9) . . ? O15 C19 C20 120.5(9) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C21 O17 Co3 126.4(6) . . ? C21 O18 Dy2 133.7(5) . . ? O18 C21 O17 125.9(8) . . ? O18 C21 C22 119.2(8) . . ? O17 C21 C22 114.9(8) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O21 N5 O19 122.4(9) . . ? O21 N5 O20 121.6(8) . . ? O19 N5 O20 116.0(8) . . ? N5 O19 Dy2 95.8(5) . . ? N5 O20 Dy2 97.0(5) . . ? O22 N6 O24 122.7(11) . . ? O22 N6 O23 118.4(9) . . ? O24 N6 O23 118.9(11) . . ? N6 O22 Dy2 95.5(6) . . ? N6 O23 Dy2 94.7(6) . . ? C23A O25 Dy2 137.3(12) . . ? C23B O25 Dy2 129(2) . . ? C23A O25 H25 84(8) . . ? C23B O25 H25 95(8) . . ? Dy2 O25 H25 134(8) . . ? O25 C23A H23A 109.5 . . ? O25 C23A H23B 109.5 . . ? H23A C23A H23B 109.5 . . ? O25 C23A H23C 109.5 . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? O25 C23B H23D 109.5 . . ? O25 C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? O25 C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? O32A N31A O31A 119(2) . . ? O32A N31A O33A 117(2) . . ? O31A N31A O33A 120(2) . . ? O33B N31B O32B 117.8(17) . . ? O33B N31B O31B 119.0(16) . . ? O32B N31B O31B 117.8(16) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H11 O43A 0.87(4) 2.12(5) 2.98(2) 169(9) 2_656 N1 H11 O43B 0.87(4) 2.18(6) 2.99(2) 154(9) 2_656 N1 H12 O13 0.89(4) 2.33(6) 3.129(9) 150(9) 2_666 N2 H21 O44A 0.88(4) 2.31(6) 3.14(3) 158(10) . N2 H21 O44B 0.88(4) 2.17(7) 2.98(3) 152(9) . N2 H22 O16 0.90(4) 2.16(7) 2.951(9) 147(9) . N3 H31 O6 0.88(4) 2.06(4) 2.928(11) 170(9) 1_455 N3 H32 O32A 0.89(4) 2.29(7) 3.05(2) 143(9) . N4 H41 O31A 0.87(4) 2.23(5) 3.084(17) 167(10) . N4 H42 O20 0.88(4) 2.39(6) 3.210(9) 155(9) 2_557 O3 H3 O41 0.84 2.27 2.74(2) 115.2 . O6 H6 O44A 0.84 2.13 2.87(3) 146.6 . O9A H9A O33B 0.84 2.46 3.04(3) 126.5 . O9B H9B O33A 0.84 2.50 3.02(5) 120.9 2_566 O12 H121 O3 0.888(19) 1.86(3) 2.743(12) 171(13) 2_656 O25 H25 O14 0.88(2) 2.06(9) 2.761(9) 135(10) . _diffrn_measured_fraction_theta_max 0.882 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 5.874 _refine_diff_density_min -2.605 _refine_diff_density_rms 0.300