# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 919823' #TrackingRef '1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71 H80 Cu4 Eu2 N20 O31 W2' _chemical_formula_weight 2635.33 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7978(10) _cell_length_b 12.9032(14) _cell_length_c 17.8446(19) _cell_angle_alpha 95.7840(10) _cell_angle_beta 98.2840(10) _cell_angle_gamma 104.6560(10) _cell_volume 2137.5(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2569 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 24.21 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.047 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1284 _exptl_absorpt_coefficient_mu 5.192 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5097 _exptl_absorpt_correction_T_max 0.5746 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex2 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15155 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_unetI/netI 0.0565 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7470 _reflns_number_gt 6120 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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 thermal parameters of C28, c29, C30,c27, c26, O13, o15, C36, and O16 were restrained. Also some O--H and H...H distances are restrained. ; _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^)+(0.0407P)^2^+4.2536P] 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 7470 _refine_ls_number_parameters 616 _refine_ls_number_restraints 97 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0980 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.009 _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 W1 W 0.95603(2) 1.255539(17) 0.238729(11) 0.02595(6) Uani 1 1 d . . . Cu1 Cu 0.96670(6) 0.86669(5) 0.29665(3) 0.02586(16) Uani 1 1 d . A . Cu2 Cu 0.18291(6) 0.68058(5) 0.23519(3) 0.02838(16) Uani 1 1 d . . . Eu1 Eu 0.58200(2) 0.727964(18) 0.260269(13) 0.01975(6) Uani 1 1 d . . . N1 N 0.9538(4) 1.0423(3) 0.3274(2) 0.0321(12) Uani 1 1 d . . . N2 N 0.7418(6) 1.3028(6) 0.3572(3) 0.083(2) Uani 1 1 d . . . N3 N 0.7557(5) 1.3877(5) 0.1430(3) 0.0594(16) Uani 1 1 d . . . N4 N 1.1496(5) 1.3808(4) 0.4061(2) 0.0452(14) Uani 1 1 d . . . N5 N 1.1648(4) 1.4808(4) 0.1990(2) 0.0347(12) Uani 1 1 d . . . N6 N 1.2727(5) 1.2087(4) 0.2422(3) 0.0432(14) Uani 1 1 d . . . N7 N 0.9696(6) 1.1570(4) 0.0623(3) 0.0537(16) Uani 1 1 d . . . N8 N 0.6486(5) 1.0676(4) 0.1776(3) 0.0656(17) Uani 1 1 d . . . C1 C 0.9522(5) 1.1175(4) 0.2986(3) 0.0292(14) Uani 1 1 d . A . C2 C 0.8168(6) 1.2849(5) 0.3158(3) 0.0480(17) Uani 1 1 d . . . C3 C 0.8245(5) 1.3425(5) 0.1769(3) 0.0391(16) Uani 1 1 d . . . C4 C 1.0840(5) 1.3380(4) 0.3475(3) 0.0313(13) Uani 1 1 d . . . C5 C 1.0924(5) 1.4023(4) 0.2117(3) 0.0300(14) Uani 1 1 d . . . C6 C 1.1624(6) 1.2237(4) 0.2409(3) 0.0313(14) Uani 1 1 d . . . C7 C 0.9645(6) 1.1925(4) 0.1228(3) 0.0373(16) Uani 1 1 d . . . C8 C 0.7543(6) 1.1341(5) 0.1967(3) 0.0450(16) Uani 1 1 d . . . C9 C -0.0577(5) 0.5778(5) 0.4029(3) 0.0393(16) Uani 1 1 d . . . H9A H -0.1418 0.5982 0.3791 0.059 Uiso 1 1 calc R . . H9B H -0.0361 0.6052 0.4578 0.059 Uiso 1 1 calc R . . H9C H -0.0775 0.4988 0.3956 0.059 Uiso 1 1 calc R . . C10 C 0.0676(5) 0.6255(5) 0.3668(3) 0.0341(14) Uani 1 1 d . . . C11 C 0.2044(6) 0.6507(5) 0.4089(3) 0.0461(17) Uani 1 1 d . A . H11 H 0.2113 0.6350 0.4599 0.055 Uiso 1 1 calc R . . C12 C 0.3312(5) 0.6955(5) 0.3862(3) 0.0382(15) Uani 1 1 d . . . C13 C 0.4684(5) 0.7328(5) 0.4426(3) 0.0433(17) Uani 1 1 d . A . C14 C 0.4702(6) 0.7411(7) 0.5200(3) 0.078(3) Uani 1 1 d . . . H14 H 0.3831 0.7185 0.5388 0.093 Uiso 1 1 calc R A . C15 C 0.5965(6) 0.7816(7) 0.5700(3) 0.073(3) Uani 1 1 d . A . H15 H 0.5981 0.7902 0.6237 0.088 Uiso 1 1 calc R . . C16 C 0.7201(6) 0.8096(5) 0.5413(3) 0.0450(17) Uani 1 1 d . . . H16 H 0.8100 0.8369 0.5746 0.054 Uiso 1 1 calc R A . C17 C 0.7122(5) 0.7975(4) 0.4628(3) 0.0263(13) Uani 1 1 d . A . C18 C 0.8438(5) 0.8228(4) 0.4265(3) 0.0222(12) Uani 1 1 d . . . C19 C 0.9771(5) 0.8637(4) 0.4725(3) 0.0262(13) Uani 1 1 d . A . H19 H 0.9787 0.8775 0.5260 0.031 Uiso 1 1 calc R . . C20 C 1.1087(5) 0.8867(4) 0.4484(3) 0.0280(13) Uani 1 1 d . . . C21 C 1.2427(6) 0.9156(5) 0.5090(3) 0.0421(17) Uani 1 1 d . A . H21A H 1.2439 0.8542 0.5370 0.063 Uiso 1 1 calc R . . H21B H 1.2434 0.9788 0.5446 0.063 Uiso 1 1 calc R . . H21C H 1.3274 0.9324 0.4845 0.063 Uiso 1 1 calc R . . C22 C -0.0932(5) 0.6159(5) 0.0242(3) 0.0387(16) Uani 1 1 d . . . H22A H -0.1424 0.5413 0.0291 0.058 Uiso 1 1 calc R . . H22B H -0.0689 0.6185 -0.0271 0.058 Uiso 1 1 calc R . . H22C H -0.1563 0.6625 0.0322 0.058 Uiso 1 1 calc RD . . C23 C 0.0416(5) 0.6547(4) 0.0831(3) 0.0269(13) Uani 1 1 d . . . C24 C 0.1743(5) 0.6864(4) 0.0591(3) 0.0279(13) Uani 1 1 d . A . H24 H 0.1740 0.6759 0.0056 0.033 Uiso 1 1 calc R . . C25 C 0.3052(5) 0.7314(4) 0.1063(3) 0.0239(12) Uani 1 1 d . . . C26 C 0.4342(6) 0.7798(5) 0.0737(3) 0.0442(14) Uani 1 1 d U A . C27 C 0.4215(7) 0.8158(6) 0.0028(3) 0.0634(14) Uani 1 1 d U . . H27 H 0.3300 0.8075 -0.0271 0.076 Uiso 1 1 calc R A . C28 C 0.5441(7) 0.8634(7) -0.0225(4) 0.0794(15) Uani 1 1 d U A . H28 H 0.5393 0.8877 -0.0711 0.095 Uiso 1 1 calc R . . C29 C 0.6768(7) 0.8761(7) 0.0238(4) 0.0762(15) Uani 1 1 d U . . H29 H 0.7633 0.9079 0.0068 0.091 Uiso 1 1 calc R A . C30 C 0.6801(6) 0.8423(6) 0.0935(3) 0.0554(15) Uani 1 1 d U A . C31 C 0.8184(5) 0.8611(4) 0.1466(3) 0.0303(14) Uani 1 1 d . . . C32 C 0.9452(5) 0.9013(4) 0.1217(3) 0.0292(14) Uani 1 1 d . A . H32 H 0.9399 0.9180 0.0709 0.035 Uiso 1 1 calc R . . C33 C 1.0839(5) 0.9199(4) 0.1664(3) 0.0254(13) Uani 1 1 d . . . C34 C 1.2095(5) 0.9670(4) 0.1293(3) 0.0278(13) Uani 1 1 d . A . H34A H 1.2250 1.0455 0.1327 0.042 Uiso 1 1 calc R . . H34B H 1.1900 0.9348 0.0754 0.042 Uiso 1 1 calc R . . H34C H 1.2954 0.9514 0.1556 0.042 Uiso 1 1 calc R . . N9 N 0.5882(4) 0.7629(3) 0.4131(2) 0.0272(11) Uani 1 1 d . A . N10 N 0.5630(4) 0.7933(3) 0.1188(2) 0.0279(11) Uani 1 1 d . A . O1 O 0.0397(3) 0.6405(3) 0.29681(19) 0.0343(10) Uani 1 1 d . . . O2 O 0.3470(3) 0.7075(3) 0.31556(18) 0.0308(9) Uani 1 1 d . A . O3 O 0.8190(3) 0.8029(2) 0.35213(16) 0.0212(8) Uani 1 1 d . A . O4 O 1.1251(3) 0.8838(3) 0.37935(19) 0.0338(10) Uani 1 1 d . A . O5 O 0.0258(3) 0.6598(3) 0.15283(19) 0.0316(9) Uani 1 1 d . . . O6 O 0.3302(3) 0.7384(3) 0.17930(18) 0.0267(9) Uani 1 1 d . A . O7 O 0.8044(3) 0.8356(3) 0.21488(17) 0.0295(9) Uani 1 1 d . A . O8 O 1.1109(3) 0.9022(3) 0.23429(18) 0.0304(10) Uani 1 1 d . A . O9 O 0.4444(3) 0.5699(3) 0.1722(2) 0.0373(10) Uani 1 1 d . A . H9D H 0.3667 0.5400 0.1890 0.056 Uiso 1 1 d R . . H9E H 0.4953 0.5237 0.1681 0.056 Uiso 1 1 d R . . O10 O 0.5637(4) 0.5712(3) 0.3246(2) 0.0400(11) Uani 1 1 d . A . H10A H 0.5097 0.5142 0.2939 0.060 Uiso 1 1 d R . . H10B H 0.5256 0.5801 0.3651 0.060 Uiso 1 1 d R . . O11 O 0.7345(3) 0.6193(3) 0.2095(2) 0.0401(11) Uani 1 1 d . A . H11A H 0.8230 0.6458 0.2010 0.060 Uiso 1 1 d R . . H11B H 0.7086 0.5478 0.1971 0.060 Uiso 1 1 d R . . O12 O 0.5797(4) 0.9133(3) 0.28302(19) 0.0319(9) Uani 0.50 1 d P A 1 O17 O 0.3980(8) 1.0056(9) 0.3316(6) 0.088(4) Uani 0.50 1 d PD B 1 H17A H 0.3694(15) 0.976(4) 0.2811(10) 0.105 Uiso 0.50 1 d PD C 1 H17B H 0.3060(14) 0.993(5) 0.3407(12) 0.105 Uiso 0.50 1 d PD D 1 O12' O 0.5797(4) 0.9133(3) 0.28302(19) 0.0319(9) Uani 0.50 1 d PD A 2 C35 C 0.4855(9) 0.9640(8) 0.3217(5) 0.029(2) Uani 0.50 1 d PDU A 2 H35A H 0.5146 1.0424 0.3212 0.043 Uiso 0.50 1 calc PR A 2 H35B H 0.4927 0.9494 0.3748 0.043 Uiso 0.50 1 calc PR A 2 H35C H 0.3862 0.9341 0.2951 0.043 Uiso 0.50 1 calc PR A 2 O13 O 0.6265(5) 0.5195(4) 0.4660(3) 0.0952(18) Uani 1 1 d DU . . H13B H 0.7076(15) 0.5034(15) 0.4790(13) 0.114 Uiso 1 1 d D . . H13A H 0.6345(18) 0.5772(15) 0.4980(13) 0.114 Uiso 1 1 d D . . O15 O 0.5233(5) 0.3806(4) 0.2445(3) 0.0888(18) Uani 1 1 d U . . H15A H 0.4446 0.3318 0.2506 0.107 Uiso 1 1 d R . . H15B H 0.5974 0.3632 0.2641 0.107 Uiso 1 1 d R . . O16 O 0.5119(8) 0.4487(6) 0.0622(5) 0.155(3) Uani 1 1 d DU . . H16A H 0.5963 0.4588 0.0695 0.186 Uiso 1 1 d R . . C36 C 0.4159(17) 0.3434(12) 0.0782(9) 0.260(5) Uani 1 1 d DU . . H36A H 0.3154 0.3444 0.0667 0.391 Uiso 1 1 calc R . . H36B H 0.4404 0.3357 0.1322 0.391 Uiso 1 1 calc R . . H36C H 0.4301 0.2822 0.0460 0.391 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01681(9) 0.03599(11) 0.02266(10) 0.01485(9) -0.00011(8) 0.00074(8) Cu1 0.0192(3) 0.0348(3) 0.0165(3) 0.0066(2) -0.0002(2) -0.0048(3) Cu2 0.0172(3) 0.0471(4) 0.0221(3) 0.0077(3) 0.0026(2) 0.0105(3) Eu1 0.01915(11) 0.02135(11) 0.01787(12) 0.00491(9) 0.00363(9) 0.00290(9) N1 0.027(2) 0.035(2) 0.027(2) 0.0040(19) -0.0032(18) 0.0005(19) N2 0.057(3) 0.163(5) 0.065(3) 0.067(3) 0.042(3) 0.058(3) N3 0.033(3) 0.084(3) 0.068(3) 0.049(3) 0.003(2) 0.015(3) N4 0.046(3) 0.071(3) 0.024(2) 0.005(2) 0.002(2) 0.028(2) N5 0.027(2) 0.035(2) 0.039(3) 0.010(2) 0.0067(19) 0.000(2) N6 0.030(2) 0.057(3) 0.040(3) -0.005(2) 0.002(2) 0.014(2) N7 0.066(3) 0.051(3) 0.031(3) 0.003(2) -0.005(3) 0.001(3) N8 0.030(3) 0.073(3) 0.084(4) 0.056(3) -0.012(3) -0.010(3) C1 0.021(2) 0.038(3) 0.022(3) 0.005(2) -0.002(2) 0.000(2) C2 0.024(3) 0.078(4) 0.051(3) 0.038(3) 0.011(3) 0.017(3) C3 0.023(3) 0.053(3) 0.039(3) 0.021(3) 0.001(2) 0.002(3) C4 0.032(3) 0.050(3) 0.020(2) 0.015(2) 0.008(2) 0.020(2) C5 0.024(2) 0.041(3) 0.021(3) 0.008(2) 0.000(2) 0.004(2) C6 0.034(3) 0.037(3) 0.019(3) 0.001(2) 0.000(2) 0.006(2) C7 0.037(3) 0.034(3) 0.030(3) 0.010(2) -0.005(2) -0.005(2) C8 0.023(3) 0.063(3) 0.043(3) 0.041(3) -0.007(2) -0.004(3) C9 0.027(3) 0.051(3) 0.044(3) 0.005(3) 0.011(2) 0.016(2) C10 0.026(2) 0.054(3) 0.032(3) 0.010(2) 0.014(2) 0.021(2) C11 0.034(3) 0.083(4) 0.036(3) 0.027(3) 0.017(2) 0.030(3) C12 0.032(3) 0.071(4) 0.024(3) 0.018(2) 0.009(2) 0.031(3) C13 0.027(2) 0.087(4) 0.024(3) 0.009(3) 0.010(2) 0.027(3) C14 0.029(3) 0.195(8) 0.019(3) 0.022(4) 0.012(2) 0.039(4) C15 0.046(3) 0.172(7) 0.015(3) 0.021(4) 0.010(2) 0.049(4) C16 0.034(3) 0.090(4) 0.015(3) 0.009(3) -0.002(2) 0.027(3) C17 0.026(2) 0.038(3) 0.018(2) 0.005(2) -0.002(2) 0.017(2) C18 0.026(2) 0.019(2) 0.022(2) 0.0035(19) 0.005(2) 0.0082(19) C19 0.036(3) 0.026(2) 0.011(2) 0.000(2) -0.002(2) 0.003(2) C20 0.027(3) 0.022(2) 0.028(3) 0.002(2) 0.000(2) -0.001(2) C21 0.031(3) 0.053(4) 0.030(3) -0.003(3) -0.002(2) -0.003(3) C22 0.023(3) 0.044(3) 0.038(3) 0.009(3) -0.006(2) -0.005(2) C23 0.027(2) 0.029(2) 0.022(2) 0.009(2) -0.003(2) 0.004(2) C24 0.022(2) 0.030(3) 0.027(3) 0.003(2) 0.000(2) 0.001(2) C25 0.027(2) 0.020(2) 0.026(3) 0.012(2) 0.003(2) 0.007(2) C26 0.024(2) 0.073(3) 0.028(2) 0.025(2) -0.001(2) -0.004(2) C27 0.036(2) 0.099(2) 0.041(2) 0.036(2) -0.0049(19) -0.011(2) C28 0.048(2) 0.121(3) 0.049(2) 0.045(2) -0.004(2) -0.018(2) C29 0.045(2) 0.117(3) 0.048(2) 0.044(2) -0.003(2) -0.020(2) C30 0.030(2) 0.094(3) 0.030(2) 0.033(2) 0.000(2) -0.013(2) C31 0.029(3) 0.036(3) 0.021(2) 0.015(2) 0.000(2) -0.001(2) C32 0.026(2) 0.036(3) 0.020(2) 0.006(2) 0.003(2) -0.002(2) C33 0.026(2) 0.029(3) 0.018(2) 0.001(2) 0.002(2) 0.003(2) C34 0.027(2) 0.036(3) 0.018(2) 0.003(2) 0.010(2) 0.001(2) N9 0.0250(19) 0.046(2) 0.017(2) 0.0104(18) 0.0042(16) 0.0185(18) N10 0.023(2) 0.036(2) 0.017(2) 0.0070(18) -0.0027(17) -0.0030(18) O1 0.0177(16) 0.060(2) 0.0272(19) 0.0056(17) 0.0076(14) 0.0121(16) O2 0.0190(16) 0.054(2) 0.0213(17) 0.0070(16) 0.0025(14) 0.0125(15) O3 0.0211(15) 0.0266(16) 0.0118(15) 0.0026(13) 0.0004(13) 0.0006(13) O4 0.0202(17) 0.049(2) 0.0264(19) 0.0127(17) 0.0013(14) -0.0013(16) O5 0.0195(16) 0.049(2) 0.0288(19) 0.0143(16) 0.0017(14) 0.0116(15) O6 0.0193(15) 0.0379(18) 0.0225(17) 0.0127(15) 0.0001(13) 0.0060(14) O7 0.0193(16) 0.047(2) 0.0146(16) 0.0091(15) 0.0015(13) -0.0062(15) O8 0.0207(16) 0.047(2) 0.0185(17) 0.0058(16) 0.0040(14) 0.0001(16) O9 0.0168(16) 0.039(2) 0.053(2) 0.0071(18) 0.0029(16) 0.0041(15) O10 0.042(2) 0.036(2) 0.039(2) 0.0140(17) 0.0061(18) 0.0018(17) O11 0.0212(17) 0.041(2) 0.054(2) -0.0085(19) 0.0075(17) 0.0058(16) O12 0.0376(19) 0.0265(17) 0.0310(19) 0.0042(15) 0.0068(16) 0.0070(15) O17 0.035(5) 0.107(8) 0.100(8) -0.030(7) 0.015(5) -0.004(5) O12' 0.0376(19) 0.0265(17) 0.0310(19) 0.0042(15) 0.0068(16) 0.0070(15) C35 0.017(4) 0.034(4) 0.031(5) -0.005(4) -0.009(4) 0.013(4) O13 0.056(3) 0.131(4) 0.066(3) 0.070(3) -0.026(2) -0.035(3) O15 0.075(3) 0.052(3) 0.153(4) 0.013(3) 0.054(3) 0.022(2) O16 0.119(4) 0.146(5) 0.198(5) -0.038(4) 0.032(4) 0.054(4) C36 0.250(8) 0.263(8) 0.262(8) 0.022(6) 0.034(6) 0.070(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C2 2.142(6) . ? W1 C6 2.159(6) . ? W1 C1 2.162(5) . ? W1 C4 2.163(5) . ? W1 C7 2.166(6) . ? W1 C8 2.167(5) . ? W1 C5 2.167(5) . ? W1 C3 2.170(6) . ? Cu1 O8 1.916(3) . ? Cu1 O7 1.926(3) . ? Cu1 O3 1.930(3) . ? Cu1 O4 1.933(3) . ? Cu1 N1 2.317(5) . ? Cu1 Eu1 3.6714(7) . ? Cu2 O1 1.907(3) . ? Cu2 O6 1.911(3) . ? Cu2 O5 1.913(3) . ? Cu2 O2 1.927(3) . ? Cu2 Eu1 3.7543(7) . ? Eu1 O12 2.392(3) . ? Eu1 O10 2.405(4) . ? Eu1 O9 2.409(3) . ? Eu1 O11 2.493(4) . ? Eu1 O3 2.542(3) . ? Eu1 O7 2.557(3) . ? Eu1 O2 2.597(3) . ? Eu1 N9 2.709(4) . ? Eu1 O6 2.715(3) . ? Eu1 N10 2.736(4) . ? Eu1 H10A 2.8172 . ? Eu1 H10B 2.8151 . ? N1 C1 1.145(7) . ? N2 C2 1.162(8) . ? N3 C3 1.146(8) . ? N4 C4 1.149(6) . ? N5 C5 1.144(6) . ? N6 C6 1.142(7) . ? N7 C7 1.142(7) . ? N8 C8 1.146(7) . ? C9 C10 1.492(7) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 O1 1.284(6) . ? C10 C11 1.380(7) . ? C11 C12 1.368(7) . ? C11 H11 0.9500 . ? C12 O2 1.311(6) . ? C12 C13 1.496(7) . ? C13 N9 1.340(7) . ? C13 C14 1.371(8) . ? C14 C15 1.364(8) . ? C14 H14 0.9500 . ? C15 C16 1.362(8) . ? C15 H15 0.9500 . ? C16 C17 1.383(7) . ? C16 H16 0.9500 . ? C17 N9 1.341(6) . ? C17 C18 1.504(7) . ? C18 O3 1.301(5) . ? C18 C19 1.383(6) . ? C19 C20 1.388(7) . ? C19 H19 0.9500 . ? C20 O4 1.263(6) . ? C20 C21 1.514(7) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.504(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 O5 1.272(6) . ? C23 C24 1.403(7) . ? C24 C25 1.379(6) . ? C24 H24 0.9500 . ? C25 O6 1.280(6) . ? C25 C26 1.487(7) . ? C26 N10 1.356(6) . ? C26 C27 1.391(8) . ? C27 C28 1.366(9) . ? C27 H27 0.9500 . ? C28 C29 1.399(9) . ? C28 H28 0.9500 . ? C29 C30 1.356(9) . ? C29 H29 0.9500 . ? C30 N10 1.327(7) . ? C30 C31 1.487(7) . ? C31 O7 1.311(6) . ? C31 C32 1.376(7) . ? C32 C33 1.422(6) . ? C32 H32 0.9500 . ? C33 O8 1.259(6) . ? C33 C34 1.504(7) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O9 H9D 0.8719 . ? O9 H9E 0.8717 . ? O10 H10A 0.8707 . ? O10 H10B 0.8706 . ? O11 H11A 0.8889 . ? O11 H11B 0.8887 . ? O17 H17A 0.920(16) . ? O17 H17B 0.916(14) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? O13 H13B 0.876(14) . ? O13 H13A 0.871(15) . ? O15 H15A 0.8923 . ? O15 H15B 0.8509 . ? O16 C36 1.524(13) . ? O16 H16A 0.7938 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 W1 C6 139.8(2) . . ? C2 W1 C1 81.8(2) . . ? C6 W1 C1 73.3(2) . . ? C2 W1 C4 70.9(2) . . ? C6 W1 C4 74.31(19) . . ? C1 W1 C4 80.68(19) . . ? C2 W1 C7 144.7(2) . . ? C6 W1 C7 73.0(2) . . ? C1 W1 C7 102.8(2) . . ? C4 W1 C7 144.4(2) . . ? C2 W1 C8 74.9(2) . . ? C6 W1 C8 123.5(2) . . ? C1 W1 C8 71.40(19) . . ? C4 W1 C8 138.2(2) . . ? C7 W1 C8 73.7(2) . . ? C2 W1 C5 113.4(2) . . ? C6 W1 C5 75.4(2) . . ? C1 W1 C5 144.59(19) . . ? C4 W1 C5 75.34(19) . . ? C7 W1 C5 83.10(19) . . ? C8 W1 C5 141.94(19) . . ? C2 W1 C3 76.3(2) . . ? C6 W1 C3 139.1(2) . . ? C1 W1 C3 144.60(19) . . ? C4 W1 C3 116.8(2) . . ? C7 W1 C3 80.9(2) . . ? C8 W1 C3 76.2(2) . . ? C5 W1 C3 70.58(19) . . ? O8 Cu1 O7 96.44(13) . . ? O8 Cu1 O3 169.12(15) . . ? O7 Cu1 O3 81.50(13) . . ? O8 Cu1 O4 85.40(14) . . ? O7 Cu1 O4 174.70(16) . . ? O3 Cu1 O4 95.76(13) . . ? O8 Cu1 N1 95.80(16) . . ? O7 Cu1 N1 92.01(15) . . ? O3 Cu1 N1 94.95(15) . . ? O4 Cu1 N1 92.75(15) . . ? O8 Cu1 Eu1 135.16(9) . . ? O7 Cu1 Eu1 41.13(10) . . ? O3 Cu1 Eu1 40.72(8) . . ? O4 Cu1 Eu1 135.50(10) . . ? N1 Cu1 Eu1 98.79(10) . . ? O1 Cu2 O6 173.06(16) . . ? O1 Cu2 O5 85.52(14) . . ? O6 Cu2 O5 96.26(14) . . ? O1 Cu2 O2 97.08(14) . . ? O6 Cu2 O2 80.97(14) . . ? O5 Cu2 O2 176.92(15) . . ? O1 Cu2 Eu1 136.05(10) . . ? O6 Cu2 Eu1 43.70(9) . . ? O5 Cu2 Eu1 137.62(11) . . ? O2 Cu2 Eu1 40.13(10) . . ? O12 Eu1 O10 140.70(12) . . ? O12 Eu1 O9 136.03(12) . . ? O10 Eu1 O9 71.07(12) . . ? O12 Eu1 O11 138.75(12) . . ? O10 Eu1 O11 71.14(13) . . ? O9 Eu1 O11 67.31(11) . . ? O12 Eu1 O3 80.93(11) . . ? O10 Eu1 O3 84.16(11) . . ? O9 Eu1 O3 141.86(12) . . ? O11 Eu1 O3 77.60(11) . . ? O12 Eu1 O7 74.45(12) . . ? O10 Eu1 O7 126.50(12) . . ? O9 Eu1 O7 114.03(11) . . ? O11 Eu1 O7 64.31(12) . . ? O3 Eu1 O7 59.16(10) . . ? O12 Eu1 O2 79.56(12) . . ? O10 Eu1 O2 75.86(13) . . ? O9 Eu1 O2 84.10(11) . . ? O11 Eu1 O2 141.69(12) . . ? O3 Eu1 O2 118.06(10) . . ? O7 Eu1 O2 153.98(12) . . ? O12 Eu1 N9 76.81(12) . . ? O10 Eu1 N9 64.31(13) . . ? O9 Eu1 N9 127.03(12) . . ? O11 Eu1 N9 119.36(13) . . ? O3 Eu1 N9 59.43(11) . . ? O7 Eu1 N9 114.89(10) . . ? O2 Eu1 N9 59.01(10) . . ? O12 Eu1 O6 74.22(11) . . ? O10 Eu1 O6 114.25(11) . . ? O9 Eu1 O6 62.88(11) . . ? O11 Eu1 O6 123.10(11) . . ? O3 Eu1 O6 155.08(10) . . ? O7 Eu1 O6 114.23(10) . . ? O2 Eu1 O6 55.90(10) . . ? N9 Eu1 O6 111.89(11) . . ? O12 Eu1 N10 75.05(12) . . ? O10 Eu1 N10 143.21(12) . . ? O9 Eu1 N10 74.38(12) . . ? O11 Eu1 N10 84.28(13) . . ? O3 Eu1 N10 117.48(10) . . ? O7 Eu1 N10 59.02(10) . . ? O2 Eu1 N10 112.91(11) . . ? N9 Eu1 N10 151.77(13) . . ? O6 Eu1 N10 57.68(11) . . ? O12 Eu1 Cu1 78.57(8) . . ? O10 Eu1 Cu1 104.59(9) . . ? O9 Eu1 Cu1 130.99(9) . . ? O11 Eu1 Cu1 65.44(8) . . ? O3 Eu1 Cu1 29.69(7) . . ? O7 Eu1 Cu1 29.70(7) . . ? O2 Eu1 Cu1 143.83(7) . . ? N9 Eu1 Cu1 88.03(8) . . ? O6 Eu1 Cu1 140.94(7) . . ? N10 Eu1 Cu1 88.65(8) . . ? O10 Eu1 H10A 16.9 . . ? O9 Eu1 H10A 54.2 . . ? O11 Eu1 H10A 67.7 . . ? O3 Eu1 H10A 99.4 . . ? O7 Eu1 H10A 130.4 . . ? O2 Eu1 H10A 75.1 . . ? N9 Eu1 H10A 78.8 . . ? O6 Eu1 H10A 101.5 . . ? N10 Eu1 H10A 127.4 . . ? Cu1 Eu1 H10A 115.5 . . ? O10 Eu1 H10B 17.0 . . ? O9 Eu1 H10B 80.8 . . ? O11 Eu1 H10B 87.6 . . ? O3 Eu1 H10B 83.3 . . ? O7 Eu1 H10B 136.2 . . ? O2 Eu1 H10B 62.2 . . ? N9 Eu1 H10B 49.6 . . ? O6 Eu1 H10B 109.2 . . ? N10 Eu1 H10B 155.2 . . ? Cu1 Eu1 H10B 109.2 . . ? H10A Eu1 H10B 29.2 . . ? C1 N1 Cu1 139.4(4) . . ? N1 C1 W1 176.3(5) . . ? N2 C2 W1 178.7(6) . . ? N3 C3 W1 178.7(6) . . ? N4 C4 W1 178.5(5) . . ? N5 C5 W1 178.5(4) . . ? N6 C6 W1 178.8(5) . . ? N7 C7 W1 178.3(5) . . ? N8 C8 W1 176.7(5) . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C10 C11 123.8(5) . . ? O1 C10 C9 116.5(4) . . ? C11 C10 C9 119.6(5) . . ? C12 C11 C10 128.1(5) . . ? C12 C11 H11 115.9 . . ? C10 C11 H11 115.9 . . ? O2 C12 C11 125.2(5) . . ? O2 C12 C13 113.8(4) . . ? C11 C12 C13 120.9(5) . . ? N9 C13 C14 122.2(5) . . ? N9 C13 C12 116.0(4) . . ? C14 C13 C12 121.8(5) . . ? C15 C14 C13 120.3(6) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 118.5(5) . . ? C16 C15 H15 120.7 . . ? C14 C15 H15 120.7 . . ? C15 C16 C17 118.7(5) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? N9 C17 C16 123.3(5) . . ? N9 C17 C18 114.6(4) . . ? C16 C17 C18 122.1(4) . . ? O3 C18 C19 125.9(4) . . ? O3 C18 C17 114.7(4) . . ? C19 C18 C17 119.4(4) . . ? C18 C19 C20 126.6(4) . . ? C18 C19 H19 116.7 . . ? C20 C19 H19 116.7 . . ? O4 C20 C19 124.8(4) . . ? O4 C20 C21 117.3(4) . . ? C19 C20 C21 117.9(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 C23 C24 124.2(4) . . ? O5 C23 C22 116.4(4) . . ? C24 C23 C22 119.3(4) . . ? C25 C24 C23 125.8(5) . . ? C25 C24 H24 117.1 . . ? C23 C24 H24 117.1 . . ? O6 C25 C24 126.2(5) . . ? O6 C25 C26 113.3(4) . . ? C24 C25 C26 120.5(4) . . ? N10 C26 C27 122.3(5) . . ? N10 C26 C25 116.5(4) . . ? C27 C26 C25 121.0(5) . . ? C28 C27 C26 118.2(6) . . ? C28 C27 H27 120.9 . . ? C26 C27 H27 120.9 . . ? C27 C28 C29 119.3(6) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C30 C29 C28 119.0(6) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? N10 C30 C29 123.1(5) . . ? N10 C30 C31 116.3(5) . . ? C29 C30 C31 120.7(5) . . ? O7 C31 C32 126.3(4) . . ? O7 C31 C30 114.1(4) . . ? C32 C31 C30 119.7(5) . . ? C31 C32 C33 124.8(5) . . ? C31 C32 H32 117.6 . . ? C33 C32 H32 117.6 . . ? O8 C33 C32 126.1(4) . . ? O8 C33 C34 117.2(4) . . ? C32 C33 C34 116.7(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C13 N9 C17 116.9(4) . . ? C13 N9 Eu1 121.0(3) . . ? C17 N9 Eu1 121.6(3) . . ? C30 N10 C26 118.1(4) . . ? C30 N10 Eu1 120.7(3) . . ? C26 N10 Eu1 121.2(3) . . ? C10 O1 Cu2 123.5(3) . . ? C12 O2 Cu2 121.0(3) . . ? C12 O2 Eu1 126.6(3) . . ? Cu2 O2 Eu1 111.29(14) . . ? C18 O3 Cu1 119.1(3) . . ? C18 O3 Eu1 129.5(3) . . ? Cu1 O3 Eu1 109.59(12) . . ? C20 O4 Cu1 122.1(3) . . ? C23 O5 Cu2 122.4(3) . . ? C25 O6 Cu2 121.6(3) . . ? C25 O6 Eu1 123.5(3) . . ? Cu2 O6 Eu1 107.20(13) . . ? C31 O7 Cu1 121.6(3) . . ? C31 O7 Eu1 129.0(3) . . ? Cu1 O7 Eu1 109.17(14) . . ? C33 O8 Cu1 123.0(3) . . ? Eu1 O9 H9D 109.5 . . ? Eu1 O9 H9E 109.5 . . ? H9D O9 H9E 109.4 . . ? Eu1 O10 H10A 109.4 . . ? Eu1 O10 H10B 109.3 . . ? H10A O10 H10B 109.4 . . ? Eu1 O11 H11A 125.6 . . ? Eu1 O11 H11B 125.1 . . ? H11A O11 H11B 109.4 . . ? H17A O17 H17B 93.4(14) . . ? H17A C35 H35A 80.3 . . ? H17A C35 H35B 124.0 . . ? H35A C35 H35B 109.5 . . ? H17A C35 H35C 29.3 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? H13B O13 H13A 103.6(14) . . ? H15A O15 H15B 109.7 . . ? C36 O16 H16A 120.0 . . ? O16 C36 H36A 109.5 . . ? O16 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O16 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.470 _refine_diff_density_min -1.479 _refine_diff_density_rms 0.157 data_2 _database_code_depnum_ccdc_archive 'CCDC 919824' #TrackingRef '2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71 H80 Cu4 Gd2 N20 O31 W2' _chemical_formula_weight 2645.91 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8007(14) _cell_length_b 12.9131(18) _cell_length_c 17.873(3) _cell_angle_alpha 95.901(2) _cell_angle_beta 98.437(2) _cell_angle_gamma 104.623(2) _cell_volume 2141.8(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2181 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 24.91 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.051 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1286 _exptl_absorpt_coefficient_mu 5.266 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4862 _exptl_absorpt_correction_T_max 0.5476 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex2 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15272 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_unetI/netI 0.0527 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7482 _reflns_number_gt 6121 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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 thermal parameters of C28, c29, C30,c27, c26, O13, o15, C36, and O16 were restrained. Also some O--H and H...H distances are restrained. ; _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^)+(0.0571P)^2^+3.6159P] 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 7482 _refine_ls_number_parameters 616 _refine_ls_number_restraints 93 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1091 _refine_ls_wR_factor_gt 0.1011 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.008 _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 W1 W 0.955465(19) 1.254953(14) 0.239121(10) 0.02490(5) Uani 1 1 d . . . Cu1 Cu 0.96648(6) 0.86614(4) 0.29638(3) 0.02512(14) Uani 1 1 d . . . Cu2 Cu 0.18221(6) 0.68026(5) 0.23439(3) 0.02760(15) Uani 1 1 d . . . Gd1 Gd 0.58098(2) 0.727098(17) 0.259264(12) 0.02225(6) Uani 1 1 d . . . N1 N 0.9535(4) 1.0422(3) 0.3278(2) 0.0317(11) Uani 1 1 d . . . N2 N 0.7398(5) 1.3016(5) 0.3563(3) 0.0798(18) Uani 1 1 d . . . N3 N 0.7553(5) 1.3864(4) 0.1433(3) 0.0532(14) Uani 1 1 d . . . N4 N 1.1485(5) 1.3796(4) 0.4071(2) 0.0442(13) Uani 1 1 d . . . N5 N 1.1648(4) 1.4801(3) 0.2002(2) 0.0366(12) Uani 1 1 d . . . N6 N 1.2719(4) 1.2060(4) 0.2439(2) 0.0421(13) Uani 1 1 d . . . N7 N 0.9694(5) 1.1564(4) 0.0622(2) 0.0509(15) Uani 1 1 d . . . N8 N 0.6495(5) 1.0674(4) 0.1775(3) 0.0665(16) Uani 1 1 d . . . C1 C 0.9517(5) 1.1158(4) 0.2980(3) 0.0293(13) Uani 1 1 d . . . C2 C 0.8150(5) 1.2860(5) 0.3171(3) 0.0483(16) Uani 1 1 d . . . C3 C 0.8233(5) 1.3406(4) 0.1771(3) 0.0354(14) Uani 1 1 d . . . C4 C 1.0822(5) 1.3376(4) 0.3484(3) 0.0307(12) Uani 1 1 d . . . C5 C 1.0933(5) 1.4011(4) 0.2126(2) 0.0267(12) Uani 1 1 d . . . C6 C 1.1630(5) 1.2223(4) 0.2417(3) 0.0306(13) Uani 1 1 d . . . C7 C 0.9637(5) 1.1924(4) 0.1230(3) 0.0318(13) Uani 1 1 d . . . C8 C 0.7517(5) 1.1337(4) 0.1962(3) 0.0463(15) Uani 1 1 d . . . C9 C -0.0593(5) 0.5758(4) 0.4011(3) 0.0401(14) Uani 1 1 d . . . H9A H -0.1476 0.5809 0.3698 0.060 Uiso 1 1 calc R . . H9B H -0.0479 0.6148 0.4526 0.060 Uiso 1 1 calc R . . H9C H -0.0644 0.4997 0.4041 0.060 Uiso 1 1 calc R . . C10 C 0.0661(5) 0.6248(4) 0.3654(3) 0.0342(13) Uani 1 1 d . . . C11 C 0.2045(5) 0.6510(5) 0.4094(3) 0.0435(15) Uani 1 1 d . A . H11 H 0.2113 0.6371 0.4608 0.052 Uiso 1 1 calc R . . C12 C 0.3330(5) 0.6953(4) 0.3853(3) 0.0353(13) Uani 1 1 d . . . C13 C 0.4679(5) 0.7338(5) 0.4423(3) 0.0420(15) Uani 1 1 d . A . C14 C 0.4700(6) 0.7401(6) 0.5199(3) 0.071(2) Uani 1 1 d . . . H14 H 0.3831 0.7178 0.5388 0.085 Uiso 1 1 calc R A . C15 C 0.5969(6) 0.7783(7) 0.5696(3) 0.072(2) Uani 1 1 d . A . H15 H 0.5995 0.7837 0.6233 0.087 Uiso 1 1 calc R . . C16 C 0.7193(5) 0.8085(5) 0.5411(3) 0.0436(16) Uani 1 1 d . . . H16 H 0.8088 0.8370 0.5747 0.052 Uiso 1 1 calc R A . C17 C 0.7130(5) 0.7974(4) 0.4615(2) 0.0279(12) Uani 1 1 d . A . C18 C 0.8447(5) 0.8237(3) 0.4261(2) 0.0197(11) Uani 1 1 d . . . C19 C 0.9771(5) 0.8630(3) 0.4717(2) 0.0242(12) Uani 1 1 d . A . H19 H 0.9785 0.8745 0.5252 0.029 Uiso 1 1 calc R . . C20 C 1.1107(5) 0.8882(3) 0.4485(2) 0.0260(12) Uani 1 1 d . . . C21 C 1.2435(5) 0.9171(4) 0.5092(3) 0.0401(16) Uani 1 1 d . A . H21A H 1.2479 0.8543 0.5349 0.060 Uiso 1 1 calc R . . H21B H 1.2407 0.9772 0.5466 0.060 Uiso 1 1 calc R . . H21C H 1.3284 0.9388 0.4855 0.060 Uiso 1 1 calc R . . C22 C -0.0936(5) 0.6158(4) 0.0241(3) 0.0389(15) Uani 1 1 d . . . H22A H -0.1604 0.5567 0.0413 0.058 Uiso 1 1 calc R . . H22B H -0.0714 0.5897 -0.0249 0.058 Uiso 1 1 calc R . . H22C H -0.1375 0.6754 0.0179 0.058 Uiso 1 1 calc RD . . C23 C 0.0418(5) 0.6550(4) 0.0824(3) 0.0282(12) Uani 1 1 d . . . C24 C 0.1740(5) 0.6871(4) 0.0581(3) 0.0269(12) Uani 1 1 d . A . H24 H 0.1729 0.6782 0.0046 0.032 Uiso 1 1 calc R . . C25 C 0.3055(5) 0.7306(3) 0.1054(2) 0.0240(12) Uani 1 1 d . . . C26 C 0.4339(5) 0.7798(5) 0.0725(3) 0.0429(13) Uani 1 1 d U A . C27 C 0.4207(6) 0.8178(5) 0.0027(3) 0.0608(12) Uani 1 1 d U . . H27 H 0.3290 0.8099 -0.0270 0.073 Uiso 1 1 calc R A . C28 C 0.5435(7) 0.8669(6) -0.0223(4) 0.0753(13) Uani 1 1 d U A . H28 H 0.5383 0.8937 -0.0699 0.090 Uiso 1 1 calc R . . C29 C 0.6762(7) 0.8772(6) 0.0232(3) 0.0717(13) Uani 1 1 d U . . H29 H 0.7624 0.9093 0.0062 0.086 Uiso 1 1 calc R A . C30 C 0.6810(6) 0.8404(5) 0.0928(3) 0.0530(14) Uani 1 1 d U A . C31 C 0.8183(5) 0.8595(4) 0.1462(2) 0.0303(13) Uani 1 1 d . . . C32 C 0.9442(5) 0.9009(4) 0.1217(2) 0.0278(12) Uani 1 1 d . A . H32 H 0.9379 0.9190 0.0713 0.033 Uiso 1 1 calc R . . C33 C 1.0844(5) 0.9192(3) 0.1658(3) 0.0265(12) Uani 1 1 d . . . C34 C 1.2106(5) 0.9663(4) 0.1298(2) 0.0289(12) Uani 1 1 d . A . H34A H 1.2273 1.0449 0.1343 0.043 Uiso 1 1 calc R . . H34B H 1.1911 0.9352 0.0757 0.043 Uiso 1 1 calc R . . H34C H 1.2957 0.9494 0.1559 0.043 Uiso 1 1 calc R . . N9 N 0.5880(4) 0.7627(3) 0.4123(2) 0.0268(10) Uani 1 1 d . A . N10 N 0.5621(4) 0.7928(3) 0.1184(2) 0.0252(10) Uani 1 1 d . A . O1 O 0.0396(3) 0.6414(3) 0.29628(18) 0.0359(9) Uani 1 1 d . . . O2 O 0.3460(3) 0.7086(3) 0.31506(16) 0.0300(9) Uani 1 1 d . A . O3 O 0.8194(3) 0.8017(2) 0.35180(15) 0.0219(8) Uani 1 1 d . A . O4 O 1.1255(3) 0.8847(3) 0.37936(17) 0.0321(9) Uani 1 1 d . A . O5 O 0.0256(3) 0.6586(3) 0.15161(18) 0.0297(9) Uani 1 1 d . . . O6 O 0.3292(3) 0.7368(2) 0.17858(16) 0.0242(8) Uani 1 1 d . A . O7 O 0.8045(3) 0.8346(3) 0.21425(16) 0.0316(9) Uani 1 1 d . A . O8 O 1.1106(3) 0.9012(3) 0.23419(17) 0.0319(9) Uani 1 1 d . A . O9 O 0.4417(3) 0.5678(3) 0.17081(18) 0.0322(9) Uani 1 1 d . A . H9D H 0.3703 0.5310 0.1909 0.048 Uiso 1 1 d RD . . H9E H 0.4966 0.5253 0.1605 0.048 Uiso 1 1 d R . . O10 O 0.5614(4) 0.5697(3) 0.32334(19) 0.0407(10) Uani 1 1 d . A . H10A H 0.5115 0.5117 0.2918 0.061 Uiso 1 1 d RD . . H10B H 0.5184 0.5767 0.3625 0.061 Uiso 1 1 d R . . O11 O 0.7336(3) 0.6172(3) 0.2083(2) 0.0441(11) Uani 1 1 d . A . H11A H 0.8191 0.6440 0.1961 0.066 Uiso 1 1 d R . . H11B H 0.7107 0.5454 0.1996 0.066 Uiso 1 1 d R . . O12 O 0.5797(3) 0.9125(2) 0.28266(18) 0.0322(9) Uani 0.50 1 d P A 1 O17 O 0.3945(7) 1.0076(6) 0.3302(4) 0.056(3) Uani 0.50 1 d PD B 1 H17A H 0.3667(14) 0.986(5) 0.2790(7) 0.067 Uiso 0.50 1 d PD C 1 H17B H 0.3067(13) 0.983(5) 0.3419(7) 0.067 Uiso 0.50 1 d PD D 1 O12' O 0.5797(3) 0.9125(2) 0.28266(18) 0.0322(9) Uani 0.50 1 d PD A 2 C35 C 0.4839(11) 0.9645(8) 0.3212(6) 0.058(4) Uani 0.50 1 d PD A 2 H35A H 0.5135 1.0427 0.3205 0.087 Uiso 0.50 1 calc PR A 2 H35B H 0.4906 0.9503 0.3743 0.087 Uiso 0.50 1 calc PR A 2 H35C H 0.3848 0.9346 0.2942 0.087 Uiso 0.50 1 calc PR A 2 O13 O 0.6269(5) 0.5191(4) 0.4655(2) 0.0930(16) Uani 1 1 d DU . . H13B H 0.7119(12) 0.5084(14) 0.4755(11) 0.112 Uiso 1 1 d D . . H13A H 0.6307(15) 0.5731(13) 0.5002(10) 0.112 Uiso 1 1 d D . . O15 O 0.5204(5) 0.3785(4) 0.2422(3) 0.0844(16) Uani 1 1 d U . . H15A H 0.4417 0.3297 0.2484 0.101 Uiso 1 1 d RD . . H15B H 0.5945 0.3612 0.2619 0.101 Uiso 1 1 d R . . O16 O 0.5114(8) 0.4480(6) 0.0607(4) 0.159(3) Uani 1 1 d DU . . H16A H 0.5959 0.4582 0.0679 0.191 Uiso 1 1 d R . . C36 C 0.4259(13) 0.3431(11) 0.0756(7) 0.278(5) Uani 1 1 d DU . . H36A H 0.3239 0.3401 0.0650 0.417 Uiso 1 1 calc R . . H36B H 0.4535 0.3353 0.1292 0.417 Uiso 1 1 calc RD . . H36C H 0.4436 0.2844 0.0425 0.417 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01533(9) 0.03530(9) 0.02208(9) 0.01374(7) 0.00067(7) 0.00103(7) Cu1 0.0174(3) 0.0352(3) 0.0173(2) 0.0073(2) 0.0009(2) -0.0030(2) Cu2 0.0156(3) 0.0465(3) 0.0223(3) 0.0076(2) 0.0033(2) 0.0106(2) Gd1 0.02096(11) 0.02506(10) 0.02064(11) 0.00570(8) 0.00496(9) 0.00447(9) N1 0.027(2) 0.036(2) 0.024(2) 0.0080(17) -0.0027(17) -0.0037(18) N2 0.047(3) 0.154(5) 0.069(3) 0.061(3) 0.035(2) 0.051(3) N3 0.033(2) 0.071(3) 0.061(3) 0.040(2) 0.007(2) 0.013(2) N4 0.045(2) 0.063(3) 0.027(2) -0.003(2) -0.002(2) 0.028(2) N5 0.029(2) 0.037(2) 0.041(2) 0.0077(18) 0.0090(18) 0.0019(18) N6 0.028(2) 0.060(3) 0.034(2) -0.005(2) 0.0004(19) 0.013(2) N7 0.063(3) 0.052(3) 0.024(2) 0.001(2) -0.006(2) 0.001(2) N8 0.038(3) 0.073(3) 0.074(3) 0.051(2) -0.015(2) -0.014(2) C1 0.018(2) 0.042(3) 0.024(2) 0.010(2) -0.0011(19) 0.002(2) C2 0.023(2) 0.088(3) 0.047(3) 0.041(3) 0.011(2) 0.022(2) C3 0.024(2) 0.043(3) 0.035(3) 0.015(2) 0.004(2) 0.001(2) C4 0.027(2) 0.046(2) 0.028(2) 0.015(2) 0.0084(19) 0.019(2) C5 0.020(2) 0.044(3) 0.014(2) 0.0055(19) 0.0027(17) 0.005(2) C6 0.032(3) 0.036(2) 0.017(2) -0.0006(19) -0.001(2) 0.001(2) C7 0.028(3) 0.031(2) 0.026(2) 0.011(2) -0.007(2) -0.006(2) C8 0.025(3) 0.054(3) 0.049(3) 0.037(2) -0.008(2) -0.013(2) C9 0.033(3) 0.056(3) 0.043(3) 0.017(2) 0.018(2) 0.023(2) C10 0.029(2) 0.048(3) 0.030(3) 0.010(2) 0.009(2) 0.016(2) C11 0.034(3) 0.080(3) 0.029(3) 0.020(2) 0.013(2) 0.028(2) C12 0.020(2) 0.064(3) 0.032(3) 0.014(2) 0.0063(19) 0.026(2) C13 0.021(2) 0.087(4) 0.025(2) 0.012(2) 0.008(2) 0.022(2) C14 0.033(3) 0.171(6) 0.022(3) 0.025(3) 0.016(2) 0.045(3) C15 0.041(3) 0.175(6) 0.014(2) 0.020(3) 0.010(2) 0.050(4) C16 0.029(3) 0.084(4) 0.018(2) 0.002(2) -0.004(2) 0.023(3) C17 0.028(2) 0.040(2) 0.021(2) 0.0056(19) 0.0042(19) 0.0190(19) C18 0.023(2) 0.0220(19) 0.0131(19) 0.0041(16) 0.0001(17) 0.0065(17) C19 0.029(2) 0.029(2) 0.012(2) -0.0019(17) 0.0004(18) 0.0071(19) C20 0.030(2) 0.022(2) 0.023(2) 0.0036(18) 0.0003(19) 0.0033(19) C21 0.034(3) 0.044(3) 0.029(3) 0.003(2) -0.003(2) -0.005(2) C22 0.027(3) 0.048(3) 0.033(3) 0.004(2) -0.005(2) 0.001(2) C23 0.024(2) 0.031(2) 0.030(2) 0.0118(19) 0.0007(19) 0.0086(19) C24 0.019(2) 0.035(2) 0.026(2) 0.0073(19) 0.0013(19) 0.0066(19) C25 0.024(2) 0.028(2) 0.019(2) 0.0035(18) 0.0018(18) 0.0070(18) C26 0.020(2) 0.073(2) 0.028(2) 0.0211(19) -0.0015(18) -0.004(2) C27 0.0351(19) 0.094(2) 0.0389(18) 0.0324(18) -0.0073(17) -0.0094(19) C28 0.050(2) 0.113(2) 0.0456(19) 0.0409(19) -0.0044(18) -0.014(2) C29 0.046(2) 0.109(2) 0.0432(19) 0.0400(18) -0.0023(18) -0.014(2) C30 0.034(2) 0.086(2) 0.032(2) 0.0344(19) 0.0012(18) -0.005(2) C31 0.026(2) 0.041(2) 0.019(2) 0.0106(19) 0.0022(19) -0.001(2) C32 0.028(2) 0.034(2) 0.020(2) 0.0091(18) 0.0069(19) 0.003(2) C33 0.028(2) 0.026(2) 0.027(2) 0.0040(18) 0.0119(19) 0.0050(19) C34 0.026(2) 0.036(2) 0.025(2) 0.0076(19) 0.0137(19) 0.002(2) N9 0.030(2) 0.0363(19) 0.0178(18) 0.0048(15) 0.0026(16) 0.0169(16) N10 0.0190(18) 0.0344(19) 0.0166(17) 0.0059(15) 0.0020(15) -0.0031(16) O1 0.0199(15) 0.062(2) 0.0310(17) 0.0068(16) 0.0118(13) 0.0158(15) O2 0.0203(15) 0.0548(19) 0.0183(15) 0.0105(14) 0.0039(12) 0.0142(14) O3 0.0216(15) 0.0280(15) 0.0109(14) 0.0023(12) -0.0013(12) 0.0000(12) O4 0.0200(16) 0.0490(18) 0.0218(16) 0.0127(14) -0.0020(13) -0.0001(14) O5 0.0165(15) 0.0414(17) 0.0329(17) 0.0090(14) 0.0025(13) 0.0109(13) O6 0.0173(14) 0.0359(15) 0.0198(15) 0.0103(12) 0.0035(12) 0.0056(13) O7 0.0219(16) 0.0483(18) 0.0197(15) 0.0150(14) 0.0041(13) -0.0036(15) O8 0.0247(16) 0.0449(18) 0.0231(16) 0.0107(14) 0.0067(13) 0.0007(15) O9 0.0201(16) 0.0338(17) 0.0403(19) 0.0000(15) 0.0047(14) 0.0054(14) O10 0.044(2) 0.0388(18) 0.0387(19) 0.0126(15) 0.0047(16) 0.0079(16) O11 0.0204(17) 0.047(2) 0.059(2) -0.0118(18) 0.0078(17) 0.0072(15) O12 0.0374(18) 0.0248(15) 0.0351(18) 0.0033(14) 0.0124(15) 0.0066(14) O17 0.022(3) 0.056(4) 0.088(6) -0.017(4) 0.016(4) 0.016(3) O12' 0.0374(18) 0.0248(15) 0.0351(18) 0.0033(14) 0.0124(15) 0.0066(14) C35 0.054(7) 0.047(6) 0.047(7) 0.016(5) -0.019(6) -0.022(6) O13 0.058(3) 0.122(3) 0.071(2) 0.068(2) -0.021(2) -0.029(2) O15 0.062(2) 0.055(2) 0.147(4) 0.013(3) 0.047(3) 0.020(2) O16 0.131(4) 0.154(4) 0.191(5) -0.038(4) 0.036(4) 0.058(4) C36 0.271(7) 0.279(7) 0.278(7) 0.022(6) 0.040(6) 0.076(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C3 2.164(5) . ? W1 C4 2.166(4) . ? W1 C5 2.167(5) . ? W1 C1 2.169(5) . ? W1 C7 2.169(5) . ? W1 C2 2.173(6) . ? W1 C6 2.174(6) . ? W1 C8 2.180(5) . ? Cu1 O8 1.918(3) . ? Cu1 O7 1.925(3) . ? Cu1 O3 1.932(3) . ? Cu1 O4 1.935(3) . ? Cu1 N1 2.324(4) . ? Cu2 O6 1.909(3) . ? Cu2 O1 1.908(3) . ? Cu2 O5 1.912(3) . ? Cu2 O2 1.925(3) . ? Gd1 O12 2.391(3) . ? Gd1 O10 2.414(3) . ? Gd1 O9 2.424(3) . ? Gd1 O11 2.507(4) . ? Gd1 O3 2.554(3) . ? Gd1 O7 2.566(3) . ? Gd1 O2 2.608(3) . ? Gd1 O6 2.708(3) . ? Gd1 N9 2.714(4) . ? Gd1 N10 2.734(4) . ? N1 C1 1.140(6) . ? N2 C2 1.127(8) . ? N3 C3 1.145(7) . ? N4 C4 1.149(6) . ? N5 C5 1.146(6) . ? N6 C6 1.135(7) . ? N7 C7 1.152(6) . ? N8 C8 1.122(6) . ? C9 C10 1.496(7) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 O1 1.276(6) . ? C10 C11 1.404(7) . ? C11 C12 1.395(7) . ? C11 H11 0.9500 . ? C12 O2 1.304(6) . ? C12 C13 1.483(6) . ? C13 N9 1.347(6) . ? C13 C14 1.379(7) . ? C14 C15 1.362(7) . ? C14 H14 0.9500 . ? C15 C16 1.355(8) . ? C15 H15 0.9500 . ? C16 C17 1.406(7) . ? C16 H16 0.9500 . ? C17 N9 1.342(5) . ? C17 C18 1.498(6) . ? C18 O3 1.303(5) . ? C18 C19 1.370(6) . ? C19 C20 1.401(7) . ? C19 H19 0.9500 . ? C20 O4 1.263(5) . ? C20 C21 1.506(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.500(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 O5 1.268(6) . ? C23 C24 1.403(7) . ? C24 C25 1.381(6) . ? C24 H24 0.9500 . ? C25 O6 1.285(5) . ? C25 C26 1.491(7) . ? C26 N10 1.358(6) . ? C26 C27 1.387(8) . ? C27 C28 1.371(9) . ? C27 H27 0.9500 . ? C28 C29 1.396(9) . ? C28 H28 0.9500 . ? C29 C30 1.375(8) . ? C29 H29 0.9500 . ? C30 N10 1.341(6) . ? C30 C31 1.480(7) . ? C31 O7 1.307(5) . ? C31 C32 1.369(7) . ? C32 C33 1.431(6) . ? C32 H32 0.9500 . ? C33 O8 1.269(5) . ? C33 C34 1.499(6) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O9 H9D 0.8866 . ? O9 H9E 0.8846 . ? O10 H10A 0.8749 . ? O10 H10B 0.8772 . ? O11 H11A 0.8901 . ? O11 H11B 0.8891 . ? O17 H17A 0.908(13) . ? O17 H17B 0.902(14) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? O13 H13B 0.874(12) . ? O13 H13A 0.874(14) . ? O15 H15A 0.8935 . ? O15 H15B 0.8506 . ? O16 C36 1.475(12) . ? O16 H16A 0.7937 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 W1 C4 116.90(19) . . ? C3 W1 C5 71.33(18) . . ? C4 W1 C5 75.41(17) . . ? C3 W1 C1 144.33(17) . . ? C4 W1 C1 81.06(17) . . ? C5 W1 C1 144.21(17) . . ? C3 W1 C7 80.46(19) . . ? C4 W1 C7 144.84(18) . . ? C5 W1 C7 82.85(16) . . ? C1 W1 C7 102.58(18) . . ? C3 W1 C2 76.1(2) . . ? C4 W1 C2 70.23(18) . . ? C5 W1 C2 113.3(2) . . ? C1 W1 C2 82.6(2) . . ? C7 W1 C2 144.77(18) . . ? C3 W1 C6 139.41(18) . . ? C4 W1 C6 74.73(18) . . ? C5 W1 C6 75.17(18) . . ? C1 W1 C6 72.83(18) . . ? C7 W1 C6 73.17(18) . . ? C2 W1 C6 139.72(18) . . ? C3 W1 C8 75.40(19) . . ? C4 W1 C8 138.03(19) . . ? C5 W1 C8 141.91(18) . . ? C1 W1 C8 71.61(18) . . ? C7 W1 C8 73.75(19) . . ? C2 W1 C8 75.1(2) . . ? C6 W1 C8 123.7(2) . . ? O8 Cu1 O7 96.24(13) . . ? O8 Cu1 O3 168.73(14) . . ? O7 Cu1 O3 81.84(12) . . ? O8 Cu1 O4 85.31(13) . . ? O7 Cu1 O4 175.10(14) . . ? O3 Cu1 O4 95.73(12) . . ? O8 Cu1 N1 96.12(14) . . ? O7 Cu1 N1 92.32(14) . . ? O3 Cu1 N1 95.05(14) . . ? O4 Cu1 N1 92.14(14) . . ? O6 Cu2 O1 172.99(14) . . ? O6 Cu2 O5 96.04(13) . . ? O1 Cu2 O5 85.97(14) . . ? O6 Cu2 O2 81.05(12) . . ? O1 Cu2 O2 96.75(13) . . ? O5 Cu2 O2 176.71(14) . . ? O12 Gd1 O10 140.54(12) . . ? O12 Gd1 O9 136.34(11) . . ? O10 Gd1 O9 70.75(11) . . ? O12 Gd1 O11 138.82(11) . . ? O10 Gd1 O11 71.18(13) . . ? O9 Gd1 O11 67.29(11) . . ? O12 Gd1 O3 80.84(10) . . ? O10 Gd1 O3 84.24(10) . . ? O9 Gd1 O3 141.74(11) . . ? O11 Gd1 O3 77.59(10) . . ? O12 Gd1 O7 74.48(11) . . ? O10 Gd1 O7 126.61(12) . . ? O9 Gd1 O7 114.25(10) . . ? O11 Gd1 O7 64.36(11) . . ? O3 Gd1 O7 59.14(9) . . ? O12 Gd1 O2 79.16(11) . . ? O10 Gd1 O2 75.96(12) . . ? O9 Gd1 O2 84.40(10) . . ? O11 Gd1 O2 142.02(11) . . ? O3 Gd1 O2 117.75(9) . . ? O7 Gd1 O2 153.61(11) . . ? O12 Gd1 O6 74.63(10) . . ? O10 Gd1 O6 113.77(10) . . ? O9 Gd1 O6 62.74(10) . . ? O11 Gd1 O6 123.01(10) . . ? O3 Gd1 O6 155.39(9) . . ? O7 Gd1 O6 114.56(9) . . ? O2 Gd1 O6 55.84(9) . . ? O12 Gd1 N9 76.53(11) . . ? O10 Gd1 N9 64.46(11) . . ? O9 Gd1 N9 126.93(11) . . ? O11 Gd1 N9 119.39(12) . . ? O3 Gd1 N9 59.35(10) . . ? O7 Gd1 N9 114.73(10) . . ? O2 Gd1 N9 58.81(10) . . ? O6 Gd1 N9 111.83(10) . . ? O12 Gd1 N10 75.06(11) . . ? O10 Gd1 N10 143.32(11) . . ? O9 Gd1 N10 74.76(11) . . ? O11 Gd1 N10 84.43(12) . . ? O3 Gd1 N10 117.46(9) . . ? O7 Gd1 N10 59.03(10) . . ? O2 Gd1 N10 112.92(11) . . ? O6 Gd1 N10 57.89(10) . . ? N9 Gd1 N10 151.50(12) . . ? C1 N1 Cu1 137.9(4) . . ? N1 C1 W1 177.7(5) . . ? N2 C2 W1 178.6(5) . . ? N3 C3 W1 178.6(5) . . ? N4 C4 W1 178.7(4) . . ? N5 C5 W1 178.0(4) . . ? N6 C6 W1 179.2(4) . . ? N7 C7 W1 177.8(5) . . ? N8 C8 W1 175.5(5) . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C10 C11 123.9(5) . . ? O1 C10 C9 117.2(4) . . ? C11 C10 C9 118.9(4) . . ? C12 C11 C10 126.6(5) . . ? C12 C11 H11 116.7 . . ? C10 C11 H11 116.7 . . ? O2 C12 C11 125.1(4) . . ? O2 C12 C13 115.3(4) . . ? C11 C12 C13 119.5(4) . . ? N9 C13 C14 122.6(4) . . ? N9 C13 C12 114.8(4) . . ? C14 C13 C12 122.5(5) . . ? C15 C14 C13 119.9(5) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 118.7(5) . . ? C16 C15 H15 120.7 . . ? C14 C15 H15 120.7 . . ? C15 C16 C17 119.6(4) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? N9 C17 C16 121.9(4) . . ? N9 C17 C18 115.7(4) . . ? C16 C17 C18 122.4(4) . . ? O3 C18 C19 126.0(4) . . ? O3 C18 C17 114.0(3) . . ? C19 C18 C17 120.0(4) . . ? C18 C19 C20 127.5(4) . . ? C18 C19 H19 116.3 . . ? C20 C19 H19 116.3 . . ? O4 C20 C19 123.5(4) . . ? O4 C20 C21 118.3(4) . . ? C19 C20 C21 118.2(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 C23 C24 124.9(4) . . ? O5 C23 C22 115.6(4) . . ? C24 C23 C22 119.6(4) . . ? C25 C24 C23 125.6(4) . . ? C25 C24 H24 117.2 . . ? C23 C24 H24 117.2 . . ? O6 C25 C24 125.6(4) . . ? O6 C25 C26 114.3(4) . . ? C24 C25 C26 120.0(4) . . ? N10 C26 C27 123.1(5) . . ? N10 C26 C25 115.3(4) . . ? C27 C26 C25 121.4(5) . . ? C28 C27 C26 118.2(5) . . ? C28 C27 H27 120.9 . . ? C26 C27 H27 120.9 . . ? C27 C28 C29 119.2(6) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C30 C29 C28 119.4(6) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? N10 C30 C29 122.3(5) . . ? N10 C30 C31 116.3(4) . . ? C29 C30 C31 121.2(5) . . ? O7 C31 C32 126.5(4) . . ? O7 C31 C30 114.3(4) . . ? C32 C31 C30 119.2(4) . . ? C31 C32 C33 125.2(4) . . ? C31 C32 H32 117.4 . . ? C33 C32 H32 117.4 . . ? O8 C33 C32 125.0(4) . . ? O8 C33 C34 117.1(4) . . ? C32 C33 C34 117.9(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C17 N9 C13 117.2(4) . . ? C17 N9 Gd1 121.0(3) . . ? C13 N9 Gd1 121.3(3) . . ? C30 N10 C26 117.7(4) . . ? C30 N10 Gd1 120.4(3) . . ? C26 N10 Gd1 121.9(3) . . ? C10 O1 Cu2 124.2(3) . . ? C12 O2 Cu2 122.1(3) . . ? C12 O2 Gd1 125.4(3) . . ? Cu2 O2 Gd1 110.85(13) . . ? C18 O3 Cu1 118.7(2) . . ? C18 O3 Gd1 129.7(3) . . ? Cu1 O3 Gd1 109.37(11) . . ? C20 O4 Cu1 122.7(3) . . ? C23 O5 Cu2 122.6(3) . . ? C25 O6 Cu2 122.4(3) . . ? C25 O6 Gd1 122.9(3) . . ? Cu2 O6 Gd1 107.46(12) . . ? C31 O7 Cu1 121.8(3) . . ? C31 O7 Gd1 128.8(3) . . ? Cu1 O7 Gd1 109.15(13) . . ? C33 O8 Cu1 123.5(3) . . ? Gd1 O9 H9D 110.3 . . ? Gd1 O9 H9E 110.1 . . ? H9D O9 H9E 108.7 . . ? Gd1 O10 H10A 109.9 . . ? Gd1 O10 H10B 109.7 . . ? H10A O10 H10B 109.1 . . ? Gd1 O11 H11A 125.4 . . ? Gd1 O11 H11B 125.2 . . ? H11A O11 H11B 109.4 . . ? H17A O17 H17B 95.6(14) . . ? H17A C35 H35A 75.6 . . ? H17A C35 H35B 124.7 . . ? H35A C35 H35B 109.5 . . ? H17A C35 H35C 33.9 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? H13B O13 H13A 103.7(12) . . ? H15A O15 H15B 109.6 . . ? C36 O16 H16A 116.8 . . ? O16 C36 H36A 109.5 . . ? O16 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O16 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.463 _refine_diff_density_min -1.389 _refine_diff_density_rms 0.165 data_3 _database_code_depnum_ccdc_archive 'CCDC 919825' #TrackingRef '3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71 H80 Cu4 N20 O31 Tb2 W2' _chemical_formula_weight 2649.25 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7851(9) _cell_length_b 12.9070(12) _cell_length_c 17.8866(17) _cell_angle_alpha 95.7140(10) _cell_angle_beta 98.4760(10) _cell_angle_gamma 104.8130(10) _cell_volume 2137.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1983 _cell_measurement_theta_min 2.02 _cell_measurement_theta_max 24.86 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 5.379 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4799 _exptl_absorpt_correction_T_max 0.5415 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex2 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15153 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_unetI/netI 0.0511 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7465 _reflns_number_gt 5862 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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 thermal parameters of C28, c29, C30,c27, c26, O13, o15, C36, and O16 were restrained. Also some O--H and H...H distances are restrained. ; _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^)+(0.0324P)^2^+11.8918P] 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 7465 _refine_ls_number_parameters 616 _refine_ls_number_restraints 103 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0897 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.027 _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 W1 W 0.95433(2) 1.254632(17) 0.239245(10) 0.02618(5) Uani 1 1 d . . . Cu1 Cu 0.96789(6) 0.86586(5) 0.29601(3) 0.02630(16) Uani 1 1 d . . . Cu2 Cu 0.18220(6) 0.68030(5) 0.23497(3) 0.02749(16) Uani 1 1 d . . . Tb1 Tb 0.58295(2) 0.726582(18) 0.259952(12) 0.02051(6) Uani 1 1 d . . . N1 N 0.9530(4) 1.0413(3) 0.3277(2) 0.0320(12) Uani 1 1 d . . . N2 N 0.7408(5) 1.3010(6) 0.3576(3) 0.087(2) Uani 1 1 d . . . N3 N 0.7561(5) 1.3883(4) 0.1433(3) 0.0512(15) Uani 1 1 d . . . N4 N 1.1477(5) 1.3806(4) 0.4067(2) 0.0432(13) Uani 1 1 d . . . N5 N 1.1653(4) 1.4791(4) 0.2001(2) 0.0343(12) Uani 1 1 d . . . N6 N 1.2701(5) 1.2053(4) 0.2438(3) 0.0449(14) Uani 1 1 d . . . N7 N 0.9691(6) 1.1584(4) 0.0636(2) 0.0512(16) Uani 1 1 d . . . N8 N 0.6455(5) 1.0657(5) 0.1762(3) 0.0791(19) Uani 1 1 d . . . C1 C 0.9505(5) 1.1159(4) 0.2986(3) 0.0302(14) Uani 1 1 d . . . C2 C 0.8127(6) 1.2846(6) 0.3168(3) 0.0598(18) Uani 1 1 d . . . C3 C 0.8226(5) 1.3415(4) 0.1770(3) 0.0358(15) Uani 1 1 d . . . C4 C 1.0829(5) 1.3374(4) 0.3476(3) 0.0303(13) Uani 1 1 d . . . C5 C 1.0930(5) 1.4006(4) 0.2122(3) 0.0280(14) Uani 1 1 d . . . C6 C 1.1612(5) 1.2225(4) 0.2423(3) 0.0313(14) Uani 1 1 d . . . C7 C 0.9644(5) 1.1935(4) 0.1241(3) 0.0343(15) Uani 1 1 d . . . C8 C 0.7496(6) 1.1334(5) 0.1966(3) 0.0539(18) Uani 1 1 d . . . C9 C -0.0578(5) 0.5769(5) 0.4023(3) 0.0392(15) Uani 1 1 d . . . H9A H -0.1435 0.5940 0.3771 0.059 Uiso 1 1 calc R . . H9B H -0.0369 0.6072 0.4565 0.059 Uiso 1 1 calc R . . H9C H -0.0748 0.4981 0.3974 0.059 Uiso 1 1 calc R . . C10 C 0.0665(5) 0.6243(5) 0.3659(3) 0.0351(14) Uani 1 1 d . . . C11 C 0.2058(5) 0.6501(5) 0.4088(3) 0.0442(16) Uani 1 1 d . A . H11 H 0.2130 0.6357 0.4601 0.053 Uiso 1 1 calc R . . C12 C 0.3333(5) 0.6937(5) 0.3853(3) 0.0359(14) Uani 1 1 d . . . C13 C 0.4706(5) 0.7324(5) 0.4415(3) 0.0424(16) Uani 1 1 d . A . C14 C 0.4706(6) 0.7393(7) 0.5191(3) 0.077(3) Uani 1 1 d . . . H14 H 0.3830 0.7175 0.5376 0.092 Uiso 1 1 calc R A . C15 C 0.5985(6) 0.7781(6) 0.5690(3) 0.0591(19) Uani 1 1 d U A . H15 H 0.6012 0.7847 0.6226 0.071 Uiso 1 1 calc R . . C16 C 0.7230(6) 0.8071(5) 0.5399(3) 0.0474(17) Uani 1 1 d . . . H16 H 0.8132 0.8343 0.5732 0.057 Uiso 1 1 calc R A . C17 C 0.7160(5) 0.7966(4) 0.4614(2) 0.0243(12) Uani 1 1 d . A . C18 C 0.8460(5) 0.8218(4) 0.4262(2) 0.0225(12) Uani 1 1 d . . . C19 C 0.9805(5) 0.8627(4) 0.4712(3) 0.0289(14) Uani 1 1 d . A . H19 H 0.9831 0.8753 0.5247 0.035 Uiso 1 1 calc R . . C20 C 1.1124(5) 0.8875(4) 0.4472(3) 0.0308(14) Uani 1 1 d . . . C21 C 1.2462(5) 0.9182(5) 0.5078(3) 0.0399(16) Uani 1 1 d . A . H21A H 1.2570 0.8540 0.5303 0.060 Uiso 1 1 calc R . . H21B H 1.2382 0.9731 0.5477 0.060 Uiso 1 1 calc R . . H21C H 1.3302 0.9475 0.4848 0.060 Uiso 1 1 calc R . . C22 C -0.0951(5) 0.6146(5) 0.0249(3) 0.0377(16) Uani 1 1 d . . . H22A H -0.1542 0.5472 0.0373 0.057 Uiso 1 1 calc R . . H22B H -0.0712 0.6012 -0.0259 0.057 Uiso 1 1 calc R . . H22C H -0.1484 0.6693 0.0251 0.057 Uiso 1 1 calc RD . . C23 C 0.0405(5) 0.6545(4) 0.0830(3) 0.0277(13) Uani 1 1 d . . . C24 C 0.1732(5) 0.6876(4) 0.0591(3) 0.0260(13) Uani 1 1 d . A . H24 H 0.1721 0.6791 0.0056 0.031 Uiso 1 1 calc R . . C25 C 0.3056(5) 0.7315(4) 0.1062(3) 0.0224(12) Uani 1 1 d . . . C26 C 0.4324(5) 0.7791(5) 0.0734(3) 0.0397(13) Uani 1 1 d U A . C27 C 0.4189(7) 0.8158(5) 0.0037(3) 0.0581(12) Uani 1 1 d U . . H27 H 0.3268 0.8083 -0.0256 0.070 Uiso 1 1 calc R A . C28 C 0.5422(8) 0.8635(6) -0.0225(4) 0.0744(13) Uani 1 1 d U A . H28 H 0.5364 0.8889 -0.0707 0.089 Uiso 1 1 calc R . . C29 C 0.6759(8) 0.8743(6) 0.0224(4) 0.0717(13) Uani 1 1 d U . . H29 H 0.7621 0.9045 0.0045 0.086 Uiso 1 1 calc R A . C30 C 0.6806(6) 0.8404(5) 0.0933(3) 0.0528(13) Uani 1 1 d U A . C31 C 0.8184(5) 0.8587(4) 0.1457(3) 0.0316(14) Uani 1 1 d . . . C32 C 0.9459(5) 0.9011(4) 0.1223(3) 0.0301(14) Uani 1 1 d . A . H32 H 0.9401 0.9184 0.0717 0.036 Uiso 1 1 calc R . . C33 C 1.0845(5) 0.9214(4) 0.1658(3) 0.0247(13) Uani 1 1 d . . . C34 C 1.2113(5) 0.9676(4) 0.1288(3) 0.0289(14) Uani 1 1 d . A . H34A H 1.2258 1.0458 0.1302 0.043 Uiso 1 1 calc R . . H34B H 1.1930 0.9329 0.0756 0.043 Uiso 1 1 calc R . . H34C H 1.2977 0.9540 0.1566 0.043 Uiso 1 1 calc R . . N9 N 0.5900(4) 0.7619(3) 0.4122(2) 0.0264(11) Uani 1 1 d . A . N10 N 0.5616(4) 0.7923(3) 0.1188(2) 0.0240(11) Uani 1 1 d . A . O1 O 0.0397(3) 0.6398(3) 0.29644(19) 0.0374(10) Uani 1 1 d . . . O2 O 0.3472(3) 0.7071(3) 0.31463(17) 0.0308(9) Uani 1 1 d . A . O3 O 0.8208(3) 0.8006(2) 0.35147(16) 0.0200(8) Uani 1 1 d . A . O4 O 1.1277(3) 0.8842(3) 0.37811(18) 0.0365(10) Uani 1 1 d . A . O5 O 0.0243(3) 0.6585(3) 0.15222(18) 0.0318(10) Uani 1 1 d . . . O6 O 0.3290(3) 0.7382(3) 0.17934(16) 0.0234(9) Uani 1 1 d . A . O7 O 0.8048(3) 0.8342(3) 0.21416(17) 0.0292(10) Uani 1 1 d . A . O8 O 1.1128(3) 0.9032(3) 0.23395(17) 0.0301(10) Uani 1 1 d . A . O9 O 0.4429(3) 0.5716(3) 0.17277(18) 0.0304(9) Uani 1 1 d . A . H9D H 0.4108 0.5182 0.1977 0.046 Uiso 1 1 d R . . H9E H 0.4973 0.5523 0.1425 0.046 Uiso 1 1 d R . . O10 O 0.5619(4) 0.5710(3) 0.3234(2) 0.0388(11) Uani 1 1 d . A . H10A H 0.4793 0.5240 0.3054 0.058 Uiso 1 1 d R . . H10B H 0.5684 0.5899 0.3725 0.058 Uiso 1 1 d R . . O11 O 0.7342(3) 0.6182(3) 0.2092(2) 0.0399(11) Uani 1 1 d . A . H11A H 0.8184 0.6450 0.1955 0.060 Uiso 1 1 d R . . H11B H 0.7126 0.5463 0.2019 0.060 Uiso 1 1 d R . . O12 O 0.5839(3) 0.9098(3) 0.28350(18) 0.0296(9) Uani 0.50 1 d P A 1 O17 O 0.3986(6) 1.0071(5) 0.3308(4) 0.039(2) Uani 0.50 1 d PD B 1 H17A H 0.3643(16) 1.006(2) 0.2808(7) 0.047 Uiso 0.50 1 d PD C 1 H17B H 0.3167(15) 0.963(2) 0.3404(9) 0.047 Uiso 0.50 1 d PD D 1 O12' O 0.5839(3) 0.9098(3) 0.28350(18) 0.0296(9) Uani 0.50 1 d PD A 2 C35 C 0.4819(13) 0.9606(12) 0.3206(8) 0.084(4) Uani 0.50 1 d PDU A 2 H35A H 0.5106 1.0390 0.3202 0.127 Uiso 0.50 1 calc PR A 2 H35B H 0.4857 0.9458 0.3735 0.127 Uiso 0.50 1 calc PR A 2 H35C H 0.3838 0.9298 0.2921 0.127 Uiso 0.50 1 calc PR A 2 O13 O 0.6266(5) 0.5198(4) 0.4653(2) 0.0802(15) Uani 1 1 d DU . . H13B H 0.7028(13) 0.4990(12) 0.4818(11) 0.096 Uiso 1 1 d D . . H13A H 0.6311(15) 0.5747(13) 0.4996(10) 0.096 Uiso 1 1 d D . . O15 O 0.5220(5) 0.3789(4) 0.2450(3) 0.0756(15) Uani 1 1 d U . . H15A H 0.4433 0.3301 0.2512 0.091 Uiso 1 1 d R . . H15B H 0.5961 0.3615 0.2646 0.091 Uiso 1 1 d R . . O16 O 0.5091(6) 0.4464(5) 0.0639(4) 0.118(2) Uani 1 1 d DU . . H16A H 0.5936 0.4565 0.0712 0.142 Uiso 1 1 d R . . C36 C 0.4166(14) 0.3416(10) 0.0797(8) 0.248(5) Uani 1 1 d DU . . H36A H 0.3154 0.3413 0.0685 0.372 Uiso 1 1 calc R . . H36B H 0.4423 0.3341 0.1335 0.372 Uiso 1 1 calc R . . H36C H 0.4317 0.2811 0.0474 0.372 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01714(9) 0.03640(11) 0.02248(9) 0.01634(8) 0.00020(7) 0.00018(8) Cu1 0.0204(3) 0.0350(3) 0.0181(3) 0.0092(2) 0.0004(2) -0.0022(3) Cu2 0.0183(2) 0.0453(4) 0.0209(3) 0.0066(3) 0.0045(2) 0.0112(2) Tb1 0.02197(10) 0.02068(12) 0.01893(10) 0.00533(9) 0.00509(8) 0.00423(9) N1 0.037(2) 0.030(2) 0.023(2) 0.0060(18) -0.0031(18) 0.0033(19) N2 0.056(3) 0.171(5) 0.076(3) 0.082(3) 0.047(2) 0.061(3) N3 0.030(2) 0.060(3) 0.066(3) 0.038(2) 0.002(2) 0.008(2) N4 0.048(2) 0.059(3) 0.029(2) 0.007(2) 0.003(2) 0.029(2) N5 0.028(2) 0.035(2) 0.035(2) 0.0095(19) 0.0060(18) -0.0016(19) N6 0.030(2) 0.063(3) 0.037(2) -0.007(2) 0.001(2) 0.015(2) N7 0.068(3) 0.048(3) 0.026(2) 0.010(2) -0.005(2) 0.002(3) N8 0.038(3) 0.082(4) 0.093(4) 0.063(3) -0.025(3) -0.027(3) C1 0.021(2) 0.039(3) 0.023(2) 0.007(2) -0.0015(19) -0.003(2) C2 0.038(3) 0.108(4) 0.052(3) 0.061(3) 0.019(2) 0.030(3) C3 0.022(2) 0.043(3) 0.040(3) 0.025(2) 0.006(2) -0.004(2) C4 0.030(2) 0.046(3) 0.024(2) 0.011(2) 0.009(2) 0.021(2) C5 0.016(2) 0.038(3) 0.027(2) 0.008(2) 0.0061(19) -0.002(2) C6 0.031(3) 0.041(3) 0.015(2) 0.004(2) 0.000(2) 0.001(2) C7 0.034(3) 0.035(3) 0.025(2) 0.016(2) -0.006(2) -0.004(2) C8 0.034(3) 0.067(4) 0.050(3) 0.048(3) -0.009(2) -0.011(3) C9 0.033(2) 0.055(3) 0.042(3) 0.018(3) 0.020(2) 0.021(2) C10 0.035(2) 0.055(3) 0.025(2) 0.007(2) 0.011(2) 0.025(2) C11 0.041(3) 0.085(4) 0.022(2) 0.024(2) 0.015(2) 0.034(3) C12 0.031(2) 0.064(3) 0.025(2) 0.017(2) 0.014(2) 0.026(2) C13 0.033(2) 0.085(4) 0.019(2) 0.013(3) 0.010(2) 0.028(3) C14 0.027(3) 0.187(7) 0.030(3) 0.026(4) 0.012(2) 0.044(4) C15 0.046(3) 0.119(4) 0.020(2) 0.008(3) 0.009(2) 0.035(3) C16 0.043(3) 0.087(4) 0.018(2) 0.010(3) 0.000(2) 0.032(3) C17 0.027(2) 0.031(3) 0.017(2) 0.0041(19) 0.0041(18) 0.013(2) C18 0.035(2) 0.018(2) 0.017(2) 0.0053(18) 0.0012(19) 0.0127(19) C19 0.037(3) 0.031(3) 0.015(2) 0.003(2) 0.001(2) 0.006(2) C20 0.030(3) 0.027(3) 0.028(3) 0.009(2) -0.004(2) -0.002(2) C21 0.031(3) 0.049(3) 0.032(3) 0.007(3) -0.002(2) 0.001(3) C22 0.024(2) 0.048(3) 0.032(3) 0.011(2) -0.004(2) -0.003(2) C23 0.029(2) 0.025(3) 0.028(2) 0.009(2) -0.002(2) 0.008(2) C24 0.023(2) 0.030(3) 0.024(2) 0.007(2) 0.0020(19) 0.005(2) C25 0.026(2) 0.017(2) 0.024(2) 0.0056(18) -0.0003(19) 0.0068(19) C26 0.031(2) 0.056(2) 0.028(2) 0.0226(19) -0.0006(18) 0.001(2) C27 0.0462(18) 0.075(2) 0.0447(18) 0.0272(17) 0.0015(16) -0.0009(17) C28 0.0608(19) 0.094(2) 0.0562(19) 0.0349(18) 0.0011(17) -0.0048(18) C29 0.0565(19) 0.091(2) 0.0555(19) 0.0333(18) 0.0021(17) -0.0048(18) C30 0.042(2) 0.070(2) 0.042(2) 0.0294(19) 0.0056(18) -0.0002(19) C31 0.032(3) 0.040(3) 0.016(2) 0.006(2) 0.002(2) -0.001(2) C32 0.027(2) 0.039(3) 0.021(2) 0.015(2) 0.0051(19) -0.001(2) C33 0.026(2) 0.021(2) 0.026(2) 0.004(2) 0.0111(19) 0.000(2) C34 0.025(2) 0.035(3) 0.025(2) 0.005(2) 0.0106(19) 0.002(2) N9 0.0310(19) 0.041(2) 0.0146(18) 0.0091(16) 0.0066(15) 0.0187(17) N10 0.0234(19) 0.028(2) 0.0155(18) 0.0076(16) 0.0020(15) -0.0019(17) O1 0.0262(16) 0.061(2) 0.0286(18) 0.0076(17) 0.0114(14) 0.0148(16) O2 0.0227(15) 0.053(2) 0.0192(16) 0.0078(15) 0.0024(13) 0.0149(15) O3 0.0226(15) 0.0174(16) 0.0188(15) 0.0082(12) 0.0032(12) 0.0015(13) O4 0.0263(17) 0.052(2) 0.0257(17) 0.0123(16) -0.0005(14) 0.0017(17) O5 0.0194(15) 0.047(2) 0.0307(17) 0.0134(15) 0.0016(14) 0.0109(15) O6 0.0170(14) 0.0288(18) 0.0207(15) 0.0062(13) 0.0015(12) -0.0001(13) O7 0.0223(16) 0.040(2) 0.0166(15) 0.0095(14) 0.0005(13) -0.0067(15) O8 0.0198(15) 0.045(2) 0.0222(16) 0.0083(15) 0.0050(13) 0.0010(15) O9 0.0294(16) 0.0317(18) 0.0328(18) 0.0026(15) 0.0086(14) 0.0122(14) O10 0.041(2) 0.032(2) 0.0365(19) 0.0106(16) 0.0017(16) -0.0003(17) O11 0.0231(16) 0.046(2) 0.048(2) -0.0098(18) 0.0087(16) 0.0116(16) O12 0.0392(18) 0.0181(17) 0.0322(18) 0.0014(14) 0.0081(15) 0.0091(14) O17 0.010(3) 0.023(4) 0.078(5) -0.017(4) 0.012(3) -0.001(3) O12' 0.0392(18) 0.0181(17) 0.0322(18) 0.0014(14) 0.0081(15) 0.0091(14) C35 0.085(7) 0.077(7) 0.076(6) 0.019(5) -0.001(5) 0.001(5) O13 0.063(2) 0.096(3) 0.062(2) 0.047(2) -0.0105(19) -0.013(2) O15 0.070(2) 0.061(2) 0.105(3) 0.010(2) 0.035(2) 0.0232(19) O16 0.081(3) 0.122(4) 0.149(4) -0.032(3) 0.025(3) 0.041(3) C36 0.240(7) 0.248(7) 0.247(7) 0.019(6) 0.030(6) 0.065(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C7 2.156(5) . ? W1 C4 2.159(4) . ? W1 C6 2.161(6) . ? W1 C1 2.166(5) . ? W1 C5 2.167(5) . ? W1 C2 2.174(7) . ? W1 C3 2.174(6) . ? W1 C8 2.181(5) . ? Cu1 O8 1.923(3) . ? Cu1 O7 1.928(3) . ? Cu1 O4 1.929(3) . ? Cu1 O3 1.932(3) . ? Cu1 N1 2.326(4) . ? Cu2 O1 1.903(3) . ? Cu2 O6 1.906(3) . ? Cu2 O5 1.918(3) . ? Cu2 O2 1.922(3) . ? Tb1 O12 2.357(3) . ? Tb1 O9 2.379(3) . ? Tb1 O10 2.383(4) . ? Tb1 O11 2.484(4) . ? Tb1 O3 2.537(3) . ? Tb1 O7 2.554(3) . ? Tb1 O2 2.599(3) . ? Tb1 N9 2.704(4) . ? Tb1 O6 2.730(3) . ? Tb1 N10 2.739(4) . ? N1 C1 1.143(7) . ? N2 C2 1.127(8) . ? N3 C3 1.143(7) . ? N4 C4 1.155(6) . ? N5 C5 1.138(6) . ? N6 C6 1.140(7) . ? N7 C7 1.142(7) . ? N8 C8 1.142(7) . ? C9 C10 1.486(7) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 O1 1.278(6) . ? C10 C11 1.402(7) . ? C11 C12 1.376(7) . ? C11 H11 0.9500 . ? C12 O2 1.314(6) . ? C12 C13 1.492(6) . ? C13 N9 1.333(6) . ? C13 C14 1.382(7) . ? C14 C15 1.369(7) . ? C14 H14 0.9500 . ? C15 C16 1.374(8) . ? C15 H15 0.9500 . ? C16 C17 1.386(7) . ? C16 H16 0.9500 . ? C17 N9 1.347(5) . ? C17 C18 1.480(7) . ? C18 O3 1.310(5) . ? C18 C19 1.381(6) . ? C19 C20 1.390(7) . ? C19 H19 0.9500 . ? C20 O4 1.264(6) . ? C20 C21 1.508(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.498(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 O5 1.268(6) . ? C23 C24 1.403(7) . ? C24 C25 1.384(6) . ? C24 H24 0.9500 . ? C25 O6 1.286(5) . ? C25 C26 1.468(7) . ? C26 N10 1.358(6) . ? C26 C27 1.378(8) . ? C27 C28 1.378(9) . ? C27 H27 0.9500 . ? C28 C29 1.397(9) . ? C28 H28 0.9500 . ? C29 C30 1.380(9) . ? C29 H29 0.9500 . ? C30 N10 1.338(7) . ? C30 C31 1.475(7) . ? C31 O7 1.311(6) . ? C31 C32 1.372(7) . ? C32 C33 1.407(6) . ? C32 H32 0.9500 . ? C33 O8 1.269(6) . ? C33 C34 1.508(7) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O9 H9D 0.8738 . ? O9 H9E 0.8747 . ? O10 H10A 0.8715 . ? O10 H10B 0.8751 . ? O11 H11A 0.8880 . ? O11 H11B 0.8889 . ? O17 H17A 0.905(13) . ? O17 H17B 0.905(14) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? O13 H13B 0.876(13) . ? O13 H13A 0.879(14) . ? O15 H15A 0.8905 . ? O15 H15B 0.8498 . ? O16 C36 1.501(12) . ? O16 H16A 0.7919 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 W1 C4 143.84(19) . . ? C7 W1 C6 72.95(18) . . ? C4 W1 C6 74.16(18) . . ? C7 W1 C1 103.0(2) . . ? C4 W1 C1 81.03(18) . . ? C6 W1 C1 72.83(19) . . ? C7 W1 C5 82.16(18) . . ? C4 W1 C5 75.20(18) . . ? C6 W1 C5 75.0(2) . . ? C1 W1 C5 144.10(18) . . ? C7 W1 C2 145.0(2) . . ? C4 W1 C2 71.0(2) . . ? C6 W1 C2 139.71(19) . . ? C1 W1 C2 82.3(2) . . ? C5 W1 C2 113.9(2) . . ? C7 W1 C3 80.7(2) . . ? C4 W1 C3 116.8(2) . . ? C6 W1 C3 139.27(19) . . ? C1 W1 C3 144.71(18) . . ? C5 W1 C3 71.05(18) . . ? C2 W1 C3 76.2(2) . . ? C7 W1 C8 74.4(2) . . ? C4 W1 C8 138.5(2) . . ? C6 W1 C8 123.9(2) . . ? C1 W1 C8 71.81(19) . . ? C5 W1 C8 141.79(19) . . ? C2 W1 C8 74.6(2) . . ? C3 W1 C8 75.7(2) . . ? O8 Cu1 O7 96.51(13) . . ? O8 Cu1 O4 84.93(14) . . ? O7 Cu1 O4 175.03(16) . . ? O8 Cu1 O3 169.20(14) . . ? O7 Cu1 O3 81.74(13) . . ? O4 Cu1 O3 95.95(13) . . ? O8 Cu1 N1 96.00(15) . . ? O7 Cu1 N1 92.03(14) . . ? O4 Cu1 N1 92.55(15) . . ? O3 Cu1 N1 94.72(14) . . ? O1 Cu2 O6 173.12(15) . . ? O1 Cu2 O5 85.79(14) . . ? O6 Cu2 O5 96.13(13) . . ? O1 Cu2 O2 97.22(14) . . ? O6 Cu2 O2 80.75(13) . . ? O5 Cu2 O2 176.79(15) . . ? O12 Tb1 O9 135.90(11) . . ? O12 Tb1 O10 140.19(12) . . ? O9 Tb1 O10 71.31(11) . . ? O12 Tb1 O11 138.50(12) . . ? O9 Tb1 O11 68.03(11) . . ? O10 Tb1 O11 71.66(13) . . ? O12 Tb1 O3 80.50(10) . . ? O9 Tb1 O3 142.50(11) . . ? O10 Tb1 O3 84.43(10) . . ? O11 Tb1 O3 77.52(10) . . ? O12 Tb1 O7 74.15(12) . . ? O9 Tb1 O7 114.24(11) . . ? O10 Tb1 O7 127.31(12) . . ? O11 Tb1 O7 64.38(12) . . ? O3 Tb1 O7 59.49(9) . . ? O12 Tb1 O2 79.51(11) . . ? O9 Tb1 O2 83.55(11) . . ? O10 Tb1 O2 75.69(12) . . ? O11 Tb1 O2 141.99(12) . . ? O3 Tb1 O2 118.29(9) . . ? O7 Tb1 O2 153.58(12) . . ? O12 Tb1 N9 76.25(12) . . ? O9 Tb1 N9 127.09(12) . . ? O10 Tb1 N9 64.38(12) . . ? O11 Tb1 N9 119.62(12) . . ? O3 Tb1 N9 59.50(10) . . ? O7 Tb1 N9 115.09(10) . . ? O2 Tb1 N9 59.16(10) . . ? O12 Tb1 O6 74.54(10) . . ? O9 Tb1 O6 62.38(11) . . ? O10 Tb1 O6 113.83(11) . . ? O11 Tb1 O6 123.34(10) . . ? O3 Tb1 O6 154.97(10) . . ? O7 Tb1 O6 113.97(10) . . ? O2 Tb1 O6 55.40(9) . . ? N9 Tb1 O6 111.50(11) . . ? O12 Tb1 N10 75.28(12) . . ? O9 Tb1 N10 74.08(11) . . ? O10 Tb1 N10 143.32(12) . . ? O11 Tb1 N10 84.54(12) . . ? O3 Tb1 N10 117.83(10) . . ? O7 Tb1 N10 59.04(10) . . ? O2 Tb1 N10 112.18(11) . . ? N9 Tb1 N10 151.38(12) . . ? O6 Tb1 N10 57.44(10) . . ? C1 N1 Cu1 138.6(4) . . ? N1 C1 W1 176.6(5) . . ? N2 C2 W1 179.1(6) . . ? N3 C3 W1 178.2(5) . . ? N4 C4 W1 177.7(4) . . ? N5 C5 W1 177.8(5) . . ? N6 C6 W1 179.8(5) . . ? N7 C7 W1 178.2(5) . . ? N8 C8 W1 176.1(6) . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C10 C11 123.4(5) . . ? O1 C10 C9 117.6(4) . . ? C11 C10 C9 119.1(5) . . ? C12 C11 C10 127.6(5) . . ? C12 C11 H11 116.2 . . ? C10 C11 H11 116.2 . . ? O2 C12 C11 125.3(4) . . ? O2 C12 C13 114.2(4) . . ? C11 C12 C13 120.5(4) . . ? N9 C13 C14 123.1(4) . . ? N9 C13 C12 116.0(4) . . ? C14 C13 C12 120.9(5) . . ? C15 C14 C13 119.1(5) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C14 C15 C16 118.6(5) . . ? C14 C15 H15 120.7 . . ? C16 C15 H15 120.7 . . ? C15 C16 C17 119.4(5) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? N9 C17 C16 122.1(4) . . ? N9 C17 C18 115.6(4) . . ? C16 C17 C18 122.3(4) . . ? O3 C18 C19 125.1(4) . . ? O3 C18 C17 114.5(4) . . ? C19 C18 C17 120.4(4) . . ? C18 C19 C20 127.4(4) . . ? C18 C19 H19 116.3 . . ? C20 C19 H19 116.3 . . ? O4 C20 C19 124.4(4) . . ? O4 C20 C21 117.9(5) . . ? C19 C20 C21 117.6(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 C23 C24 124.6(4) . . ? O5 C23 C22 115.6(4) . . ? C24 C23 C22 119.8(4) . . ? C25 C24 C23 126.1(4) . . ? C25 C24 H24 117.0 . . ? C23 C24 H24 117.0 . . ? O6 C25 C24 125.2(4) . . ? O6 C25 C26 114.6(4) . . ? C24 C25 C26 120.1(4) . . ? N10 C26 C27 122.8(5) . . ? N10 C26 C25 115.8(4) . . ? C27 C26 C25 121.2(5) . . ? C26 C27 C28 118.4(6) . . ? C26 C27 H27 120.8 . . ? C28 C27 H27 120.8 . . ? C27 C28 C29 119.3(7) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C30 C29 C28 118.9(7) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? N10 C30 C29 122.3(5) . . ? N10 C30 C31 116.7(5) . . ? C29 C30 C31 121.0(5) . . ? O7 C31 C32 125.6(4) . . ? O7 C31 C30 114.0(4) . . ? C32 C31 C30 120.4(5) . . ? C31 C32 C33 126.4(4) . . ? C31 C32 H32 116.8 . . ? C33 C32 H32 116.8 . . ? O8 C33 C32 125.5(4) . . ? O8 C33 C34 116.5(4) . . ? C32 C33 C34 118.0(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C13 N9 C17 117.5(4) . . ? C13 N9 Tb1 121.0(3) . . ? C17 N9 Tb1 120.9(3) . . ? C30 N10 C26 118.2(4) . . ? C30 N10 Tb1 119.9(3) . . ? C26 N10 Tb1 121.8(3) . . ? C10 O1 Cu2 124.3(3) . . ? C12 O2 Cu2 121.3(3) . . ? C12 O2 Tb1 125.4(3) . . ? Cu2 O2 Tb1 111.82(14) . . ? C18 O3 Cu1 119.0(3) . . ? C18 O3 Tb1 129.4(3) . . ? Cu1 O3 Tb1 109.39(12) . . ? C20 O4 Cu1 122.1(3) . . ? C23 O5 Cu2 122.4(3) . . ? C25 O6 Cu2 122.5(3) . . ? C25 O6 Tb1 122.3(3) . . ? Cu2 O6 Tb1 107.22(13) . . ? C31 O7 Cu1 121.7(3) . . ? C31 O7 Tb1 129.1(3) . . ? Cu1 O7 Tb1 108.90(13) . . ? C33 O8 Cu1 122.7(3) . . ? Tb1 O9 H9D 110.0 . . ? Tb1 O9 H9E 108.6 . . ? H9D O9 H9E 109.0 . . ? Tb1 O10 H10A 109.8 . . ? Tb1 O10 H10B 109.6 . . ? H10A O10 H10B 109.4 . . ? Tb1 O11 H11A 125.5 . . ? Tb1 O11 H11B 125.3 . . ? H11A O11 H11B 109.2 . . ? H17A O17 H17B 95.4(13) . . ? H17A C35 H35A 65.1 . . ? H17A C35 H35B 121.8 . . ? H35A C35 H35B 109.5 . . ? H17A C35 H35C 44.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? H13B O13 H13A 103.7(13) . . ? H15A O15 H15B 109.6 . . ? C36 O16 H16A 118.9 . . ? O16 C36 H36A 109.5 . . ? O16 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O16 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.634 _refine_diff_density_min -1.386 _refine_diff_density_rms 0.157 data_4 _database_code_depnum_ccdc_archive 'CCDC 919826' #TrackingRef '4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71 H80 Cu4 Dy2 N20 O31 W2' _chemical_formula_weight 2656.41 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' Cu Cu 0.3201 1.2651 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7940(13) _cell_length_b 12.8961(17) _cell_length_c 17.868(2) _cell_angle_alpha 95.573(2) _cell_angle_beta 98.348(2) _cell_angle_gamma 104.862(2) _cell_volume 2136.8(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2691 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 24.59 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.064 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1290 _exptl_absorpt_coefficient_mu 5.475 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4563 _exptl_absorpt_correction_T_max 0.5145 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex2 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14896 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_unetI/netI 0.0628 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7443 _reflns_number_gt 6064 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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 thermal parameters of C28, c29, C30,c27, c26, O13, o15, C36, and O16 were restrained. Also some O--H and H...H distances are restrained. ; _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^)+(0.0323P)^2^+8.6476P] 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 7443 _refine_ls_number_parameters 616 _refine_ls_number_restraints 97 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.173 _refine_ls_shift/su_max 0.008 _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 W1 W 0.95555(2) 1.255387(17) 0.238716(11) 0.02755(6) Uani 1 1 d . . . Cu1 Cu 0.96768(6) 0.86639(5) 0.29649(3) 0.02705(16) Uani 1 1 d . . . Cu2 Cu 0.18315(6) 0.68061(5) 0.23592(3) 0.02908(17) Uani 1 1 d . . . Dy1 Dy 0.58415(2) 0.727776(18) 0.261248(12) 0.02202(6) Uani 1 1 d . . . N1 N 0.9533(5) 1.0418(4) 0.3278(2) 0.0347(13) Uani 1 1 d . . . N2 N 0.7424(6) 1.3018(6) 0.3575(3) 0.089(2) Uani 1 1 d . . . N3 N 0.7566(5) 1.3887(4) 0.1430(3) 0.0564(16) Uani 1 1 d . . . N4 N 1.1499(5) 1.3805(4) 0.4049(3) 0.0481(15) Uani 1 1 d . . . N5 N 1.1667(4) 1.4809(4) 0.1985(2) 0.0342(13) Uani 1 1 d . . . N6 N 1.2720(5) 1.2086(4) 0.2423(3) 0.0431(15) Uani 1 1 d . . . N7 N 0.9691(6) 1.1580(4) 0.0628(3) 0.0528(17) Uani 1 1 d . . . N8 N 0.6467(6) 1.0656(5) 0.1777(3) 0.0741(19) Uani 1 1 d . . . C1 C 0.9526(5) 1.1159(5) 0.2981(3) 0.0329(15) Uani 1 1 d . . . C2 C 0.8145(6) 1.2837(5) 0.3159(4) 0.0514(18) Uani 1 1 d . . . C3 C 0.8257(6) 1.3415(5) 0.1763(3) 0.0433(17) Uani 1 1 d . . . C4 C 1.0816(5) 1.3372(5) 0.3467(3) 0.0335(15) Uani 1 1 d . . . C5 C 1.0937(5) 1.4037(5) 0.2124(3) 0.0324(15) Uani 1 1 d . . . C6 C 1.1615(5) 1.2237(5) 0.2406(3) 0.0311(14) Uani 1 1 d . . . C7 C 0.9622(6) 1.1941(5) 0.1239(3) 0.0400(17) Uani 1 1 d . . . C8 C 0.7520(6) 1.1343(5) 0.1967(3) 0.0505(18) Uani 1 1 d . . . C9 C -0.0579(5) 0.5757(5) 0.4039(3) 0.0403(16) Uani 1 1 d . . . H9A H -0.1435 0.5925 0.3784 0.060 Uiso 1 1 calc R . . H9B H -0.0383 0.6054 0.4582 0.060 Uiso 1 1 calc R . . H9C H -0.0741 0.4969 0.3988 0.060 Uiso 1 1 calc R . . C10 C 0.0681(5) 0.6249(5) 0.3678(3) 0.0348(15) Uani 1 1 d . . . C11 C 0.2060(5) 0.6498(5) 0.4100(3) 0.0451(17) Uani 1 1 d . A . H11 H 0.2135 0.6339 0.4610 0.054 Uiso 1 1 calc R . . C12 C 0.3337(5) 0.6952(5) 0.3861(3) 0.0384(16) Uani 1 1 d . . . C13 C 0.4706(5) 0.7325(5) 0.4425(3) 0.0434(17) Uani 1 1 d . A . C14 C 0.4715(6) 0.7410(8) 0.5208(3) 0.079(3) Uani 1 1 d . . . H14 H 0.3844 0.7182 0.5397 0.095 Uiso 1 1 calc R A . C15 C 0.5989(6) 0.7826(8) 0.5702(3) 0.082(3) Uani 1 1 d . A . H15 H 0.6013 0.7924 0.6238 0.098 Uiso 1 1 calc R . . C16 C 0.7222(6) 0.8098(6) 0.5411(3) 0.0474(19) Uani 1 1 d . . . H16 H 0.8124 0.8365 0.5743 0.057 Uiso 1 1 calc R A . C17 C 0.7149(5) 0.7981(4) 0.4621(3) 0.0291(14) Uani 1 1 d . A . C18 C 0.8451(5) 0.8240(4) 0.4266(3) 0.0248(13) Uani 1 1 d . . . C19 C 0.9781(5) 0.8634(4) 0.4715(3) 0.0272(14) Uani 1 1 d . A . H19 H 0.9802 0.8760 0.5250 0.033 Uiso 1 1 calc R . . C20 C 1.1109(5) 0.8872(4) 0.4478(3) 0.0295(14) Uani 1 1 d . . . C21 C 1.2443(6) 0.9173(5) 0.5080(3) 0.0429(18) Uani 1 1 d . A . H21A H 1.2487 0.8552 0.5348 0.064 Uiso 1 1 calc R . . H21B H 1.2421 0.9784 0.5446 0.064 Uiso 1 1 calc R . . H21C H 1.3290 0.9381 0.4838 0.064 Uiso 1 1 calc R . . C22 C -0.0942(5) 0.6140(5) 0.0252(3) 0.0427(17) Uani 1 1 d . . . H22A H -0.1536 0.5464 0.0374 0.064 Uiso 1 1 calc R . . H22B H -0.0681 0.6008 -0.0250 0.064 Uiso 1 1 calc R . . H22C H -0.1481 0.6684 0.0245 0.064 Uiso 1 1 calc RD . . C23 C 0.0398(5) 0.6547(4) 0.0848(3) 0.0281(14) Uani 1 1 d . . . C24 C 0.1743(5) 0.6866(4) 0.0597(3) 0.0310(14) Uani 1 1 d . A . H24 H 0.1739 0.6760 0.0063 0.037 Uiso 1 1 calc R . . C25 C 0.3042(5) 0.7314(4) 0.1069(3) 0.0252(13) Uani 1 1 d . . . C26 C 0.4338(6) 0.7794(5) 0.0740(3) 0.0455(14) Uani 1 1 d U A . C27 C 0.4209(7) 0.8159(6) 0.0040(4) 0.0622(12) Uani 1 1 d U . . H27 H 0.3292 0.8067 -0.0260 0.075 Uiso 1 1 calc R A . C28 C 0.5439(8) 0.8656(7) -0.0211(4) 0.0773(13) Uani 1 1 d U A . H28 H 0.5380 0.8906 -0.0695 0.093 Uiso 1 1 calc R . . C29 C 0.6767(8) 0.8796(7) 0.0241(4) 0.0741(13) Uani 1 1 d U . . H29 H 0.7629 0.9137 0.0075 0.089 Uiso 1 1 calc R A . C30 C 0.6793(7) 0.8424(6) 0.0937(3) 0.0567(14) Uani 1 1 d U A . C31 C 0.8176(6) 0.8605(5) 0.1467(3) 0.0347(15) Uani 1 1 d . . . C32 C 0.9450(5) 0.9026(4) 0.1227(3) 0.0273(14) Uani 1 1 d . A . H32 H 0.9391 0.9212 0.0724 0.033 Uiso 1 1 calc R . . C33 C 1.0844(5) 0.9208(4) 0.1658(3) 0.0257(13) Uani 1 1 d . . . C34 C 1.2108(5) 0.9678(4) 0.1291(3) 0.0294(14) Uani 1 1 d . A . H34A H 1.2226 1.0455 0.1289 0.044 Uiso 1 1 calc R . . H34B H 1.1945 0.9317 0.0764 0.044 Uiso 1 1 calc R . . H34C H 1.2977 0.9566 0.1580 0.044 Uiso 1 1 calc R . . N9 N 0.5901(4) 0.7634(4) 0.4127(2) 0.0319(12) Uani 1 1 d . A . N10 N 0.5618(4) 0.7930(3) 0.1197(2) 0.0251(11) Uani 1 1 d . A . O1 O 0.0409(3) 0.6392(3) 0.2974(2) 0.0380(11) Uani 1 1 d . . . O2 O 0.3478(3) 0.7072(3) 0.31514(18) 0.0297(9) Uani 1 1 d . A . O3 O 0.8205(3) 0.8012(3) 0.35174(17) 0.0232(9) Uani 1 1 d . A . O4 O 1.1274(4) 0.8836(3) 0.3782(2) 0.0389(11) Uani 1 1 d . A . O5 O 0.0243(3) 0.6599(3) 0.15314(19) 0.0326(10) Uani 1 1 d . . . O6 O 0.3290(3) 0.7395(3) 0.18009(17) 0.0266(9) Uani 1 1 d . A . O7 O 0.8047(3) 0.8362(3) 0.21550(17) 0.0304(10) Uani 1 1 d . A . O8 O 1.1121(3) 0.9034(3) 0.23433(18) 0.0322(10) Uani 1 1 d . A . O9 O 0.4476(3) 0.5737(3) 0.1745(2) 0.0321(10) Uani 1 1 d . A . H9D H 0.3641 0.5497 0.1875 0.048 Uiso 1 1 d R . . H9E H 0.4928 0.5235 0.1758 0.048 Uiso 1 1 d R . . O10 O 0.5660(4) 0.5741(3) 0.3254(2) 0.0395(11) Uani 1 1 d . A . H10A H 0.5214 0.5162 0.2930 0.059 Uiso 1 1 d R . . H10B H 0.5181 0.5793 0.3624 0.059 Uiso 1 1 d R . . O11 O 0.7350(4) 0.6201(3) 0.2114(2) 0.0429(12) Uani 1 1 d . A . H11A H 0.8275 0.6450 0.2093 0.064 Uiso 1 1 d R . . H11B H 0.7051 0.5501 0.1926 0.064 Uiso 1 1 d R . . O12 O 0.5824(4) 0.9098(3) 0.28346(19) 0.0314(10) Uani 0.50 1 d P A 1 O17 O 0.3999(7) 1.0072(8) 0.3286(5) 0.072(3) Uani 0.50 1 d PD B 1 H17A H 0.3711(13) 0.973(3) 0.2795(9) 0.086 Uiso 0.50 1 d PD C 1 H17B H 0.3094(12) 0.998(4) 0.3385(10) 0.086 Uiso 0.50 1 d PD D 1 O12' O 0.5824(4) 0.9098(3) 0.28346(19) 0.0314(10) Uani 0.50 1 d PD A 2 C35 C 0.4855(11) 0.9594(9) 0.3223(6) 0.047(3) Uani 0.50 1 d PDU A 2 H35A H 0.5139 1.0379 0.3221 0.070 Uiso 0.50 1 calc PR A 2 H35B H 0.4924 0.9441 0.3752 0.070 Uiso 0.50 1 calc PR A 2 H35C H 0.3865 0.9288 0.2954 0.070 Uiso 0.50 1 calc PR A 2 O13 O 0.6272(5) 0.5209(4) 0.4660(3) 0.0818(15) Uani 1 1 d DU . . H13B H 0.7045(13) 0.5013(12) 0.4818(11) 0.098 Uiso 1 1 d D . . H13A H 0.6311(15) 0.5758(13) 0.5005(10) 0.098 Uiso 1 1 d D . . O15 O 0.5255(5) 0.3818(4) 0.2477(3) 0.0786(15) Uani 1 1 d U . . H15A H 0.4468 0.3330 0.2538 0.094 Uiso 1 1 d R . . H15B H 0.5996 0.3645 0.2673 0.094 Uiso 1 1 d R . . O16 O 0.5124(7) 0.4512(5) 0.0660(4) 0.129(2) Uani 1 1 d DU . . H16A H 0.5969 0.4613 0.0733 0.155 Uiso 1 1 d R . . C36 C 0.4167(14) 0.3467(10) 0.0805(8) 0.220(5) Uani 1 1 d DU . . H36A H 0.3163 0.3480 0.0690 0.330 Uiso 1 1 calc R . . H36B H 0.4405 0.3376 0.1342 0.330 Uiso 1 1 calc R . . H36C H 0.4307 0.2861 0.0478 0.330 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01655(9) 0.03795(12) 0.02569(10) 0.01809(9) -0.00029(7) 0.00033(8) Cu1 0.0193(3) 0.0359(3) 0.0189(3) 0.0097(3) -0.0009(2) -0.0048(3) Cu2 0.0176(3) 0.0487(4) 0.0234(3) 0.0094(3) 0.0034(2) 0.0121(3) Dy1 0.02218(11) 0.02146(11) 0.02202(11) 0.00619(9) 0.00513(9) 0.00349(9) N1 0.029(2) 0.039(3) 0.030(2) 0.016(2) -0.0058(18) 0.002(2) N2 0.056(3) 0.174(6) 0.076(3) 0.075(3) 0.044(2) 0.061(3) N3 0.031(2) 0.073(3) 0.071(3) 0.049(3) 0.006(2) 0.013(2) N4 0.054(3) 0.068(3) 0.032(3) 0.010(2) 0.008(2) 0.033(2) N5 0.024(2) 0.036(3) 0.038(2) 0.009(2) 0.0050(18) -0.0024(19) N6 0.027(2) 0.058(3) 0.038(3) -0.005(2) 0.002(2) 0.007(2) N7 0.063(3) 0.050(3) 0.032(3) 0.009(2) -0.003(2) -0.004(3) N8 0.036(3) 0.073(3) 0.094(4) 0.058(3) -0.022(3) -0.020(3) C1 0.024(2) 0.043(3) 0.029(3) 0.013(2) 0.000(2) 0.004(2) C2 0.028(3) 0.078(4) 0.063(3) 0.048(3) 0.013(3) 0.025(3) C3 0.030(3) 0.052(4) 0.044(3) 0.026(3) 0.004(2) -0.003(3) C4 0.032(2) 0.054(3) 0.021(2) 0.007(2) 0.003(2) 0.022(2) C5 0.024(2) 0.042(3) 0.027(3) 0.010(2) 0.000(2) 0.002(2) C6 0.020(2) 0.045(3) 0.027(3) 0.009(2) 0.005(2) 0.004(2) C7 0.033(3) 0.045(3) 0.031(3) 0.021(3) -0.009(2) -0.005(3) C8 0.028(3) 0.069(4) 0.046(3) 0.038(3) -0.010(2) -0.004(3) C9 0.029(3) 0.056(3) 0.043(3) 0.016(3) 0.014(2) 0.019(2) C10 0.028(2) 0.050(3) 0.032(3) 0.005(2) 0.012(2) 0.015(2) C11 0.029(2) 0.091(4) 0.029(3) 0.023(3) 0.011(2) 0.032(3) C12 0.031(3) 0.067(4) 0.025(3) 0.017(2) 0.008(2) 0.021(3) C13 0.026(2) 0.087(4) 0.024(3) 0.012(3) 0.006(2) 0.026(3) C14 0.026(3) 0.196(8) 0.025(3) 0.028(4) 0.010(2) 0.038(4) C15 0.037(3) 0.198(8) 0.019(3) 0.014(4) 0.005(2) 0.047(4) C16 0.030(3) 0.093(5) 0.020(3) 0.007(3) -0.002(2) 0.023(3) C17 0.033(2) 0.041(3) 0.019(2) 0.007(2) 0.0078(19) 0.019(2) C18 0.036(2) 0.020(2) 0.021(2) 0.0103(19) 0.004(2) 0.011(2) C19 0.033(3) 0.025(3) 0.017(2) 0.001(2) -0.001(2) 0.000(2) C20 0.031(3) 0.023(3) 0.029(3) 0.007(2) -0.007(2) 0.002(2) C21 0.029(3) 0.048(4) 0.038(3) 0.008(3) -0.006(2) -0.008(3) C22 0.025(3) 0.054(4) 0.040(3) 0.014(3) -0.008(2) 0.000(3) C23 0.026(2) 0.019(2) 0.036(3) 0.009(2) -0.004(2) 0.005(2) C24 0.028(3) 0.033(3) 0.026(3) 0.010(2) -0.006(2) 0.002(2) C25 0.025(2) 0.026(2) 0.028(2) 0.012(2) 0.0053(19) 0.011(2) C26 0.029(2) 0.068(3) 0.032(2) 0.027(2) -0.0022(19) -0.004(2) C27 0.0466(19) 0.082(2) 0.0483(18) 0.0302(17) 0.0002(17) -0.0022(17) C28 0.0608(19) 0.097(2) 0.0615(19) 0.0355(18) 0.0018(18) -0.0051(18) C29 0.0591(19) 0.094(2) 0.0569(19) 0.0326(18) 0.0037(17) -0.0054(18) C30 0.047(2) 0.075(2) 0.041(2) 0.0258(19) 0.0068(18) -0.0019(19) C31 0.031(3) 0.037(3) 0.027(3) 0.010(2) -0.003(2) -0.005(2) C32 0.029(2) 0.032(3) 0.015(2) 0.006(2) 0.0018(19) 0.000(2) C33 0.024(2) 0.025(3) 0.025(2) 0.003(2) 0.0089(19) 0.002(2) C34 0.019(2) 0.039(3) 0.027(2) 0.004(2) 0.0100(19) 0.001(2) N9 0.029(2) 0.058(3) 0.019(2) 0.0127(19) 0.0049(16) 0.0260(19) N10 0.025(2) 0.028(2) 0.0139(18) 0.0040(17) -0.0012(16) -0.0058(18) O1 0.0221(16) 0.066(3) 0.0295(19) 0.0095(18) 0.0077(14) 0.0148(17) O2 0.0188(15) 0.058(2) 0.0165(16) 0.0059(15) 0.0023(12) 0.0184(15) O3 0.0252(16) 0.0214(17) 0.0183(16) 0.0055(13) 0.0033(13) -0.0027(14) O4 0.0256(18) 0.055(2) 0.0281(18) 0.0166(17) -0.0016(15) -0.0041(17) O5 0.0199(16) 0.051(2) 0.0300(18) 0.0128(16) 0.0033(14) 0.0124(15) O6 0.0211(15) 0.0389(19) 0.0189(16) 0.0130(14) -0.0005(13) 0.0053(14) O7 0.0197(16) 0.046(2) 0.0180(16) 0.0138(15) -0.0028(13) -0.0040(16) O8 0.0218(16) 0.046(2) 0.0232(17) 0.0088(16) 0.0009(14) -0.0006(16) O9 0.0159(15) 0.0306(19) 0.047(2) 0.0029(17) 0.0030(15) 0.0037(14) O10 0.042(2) 0.031(2) 0.043(2) 0.0123(17) 0.0026(17) 0.0062(17) O11 0.0176(16) 0.046(2) 0.059(2) -0.014(2) 0.0026(17) 0.0065(16) O12 0.0437(19) 0.0195(17) 0.0297(18) 0.0060(15) 0.0067(16) 0.0052(15) O17 0.022(4) 0.069(6) 0.106(8) -0.030(6) 0.002(5) 0.001(4) O12' 0.0437(19) 0.0195(17) 0.0297(18) 0.0060(15) 0.0067(16) 0.0052(15) C35 0.048(5) 0.045(5) 0.042(5) 0.006(4) -0.003(4) 0.011(4) O13 0.061(2) 0.096(3) 0.069(2) 0.048(2) -0.009(2) -0.015(2) O15 0.072(2) 0.063(2) 0.108(3) 0.010(2) 0.032(2) 0.024(2) O16 0.100(4) 0.124(4) 0.166(5) -0.025(4) 0.031(4) 0.048(3) C36 0.212(7) 0.221(7) 0.223(7) 0.016(6) 0.027(6) 0.063(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C7 2.142(6) . ? W1 C4 2.146(5) . ? W1 C6 2.155(5) . ? W1 C3 2.156(6) . ? W1 C2 2.158(7) . ? W1 C8 2.172(5) . ? W1 C1 2.172(6) . ? W1 C5 2.177(5) . ? Cu1 O8 1.917(3) . ? Cu1 O7 1.922(3) . ? Cu1 O3 1.926(3) . ? Cu1 O4 1.929(3) . ? Cu1 N1 2.322(5) . ? Cu2 O1 1.899(4) . ? Cu2 O6 1.902(3) . ? Cu2 O2 1.918(3) . ? Cu2 O5 1.929(3) . ? Dy1 O12 2.347(3) . ? Dy1 O9 2.361(3) . ? Dy1 O10 2.364(4) . ? Dy1 O11 2.470(4) . ? Dy1 O3 2.522(3) . ? Dy1 O7 2.545(3) . ? Dy1 O2 2.596(3) . ? Dy1 N9 2.691(4) . ? Dy1 N10 2.737(4) . ? Dy1 O6 2.748(3) . ? N1 C1 1.138(7) . ? N2 C2 1.144(9) . ? N3 C3 1.160(8) . ? N4 C4 1.155(6) . ? N5 C5 1.140(7) . ? N6 C6 1.144(7) . ? N7 C7 1.163(7) . ? N8 C8 1.156(7) . ? C9 C10 1.501(7) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 O1 1.289(6) . ? C10 C11 1.389(7) . ? C11 C12 1.384(7) . ? C11 H11 0.9500 . ? C12 O2 1.315(6) . ? C12 C13 1.492(7) . ? C13 N9 1.340(7) . ? C13 C14 1.391(8) . ? C14 C15 1.367(8) . ? C14 H14 0.9500 . ? C15 C16 1.361(8) . ? C15 H15 0.9500 . ? C16 C17 1.394(7) . ? C16 H16 0.9500 . ? C17 N9 1.342(6) . ? C17 C18 1.482(7) . ? C18 O3 1.315(5) . ? C18 C19 1.370(6) . ? C19 C20 1.395(7) . ? C19 H19 0.9500 . ? C20 O4 1.275(6) . ? C20 C21 1.505(7) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.504(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 O5 1.250(6) . ? C23 C24 1.426(7) . ? C24 C25 1.371(6) . ? C24 H24 0.9500 . ? C25 O6 1.283(6) . ? C25 C26 1.492(7) . ? C26 N10 1.353(6) . ? C26 C27 1.378(9) . ? C27 C28 1.371(10) . ? C27 H27 0.9500 . ? C28 C29 1.387(10) . ? C28 H28 0.9500 . ? C29 C30 1.376(10) . ? C29 H29 0.9500 . ? C30 N10 1.335(7) . ? C30 C31 1.485(8) . ? C31 O7 1.314(6) . ? C31 C32 1.374(7) . ? C32 C33 1.416(7) . ? C32 H32 0.9500 . ? C33 O8 1.270(6) . ? C33 C34 1.503(7) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O9 H9D 0.8706 . ? O9 H9E 0.8729 . ? O10 H10A 0.8706 . ? O10 H10B 0.8723 . ? O11 H11A 0.8879 . ? O11 H11B 0.8887 . ? O17 H17A 0.914(15) . ? O17 H17B 0.909(13) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? O13 H13B 0.876(13) . ? O13 H13A 0.881(14) . ? O15 H15A 0.8899 . ? O15 H15B 0.8507 . ? O16 C36 1.501(12) . ? O16 H16A 0.7929 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 W1 C4 145.1(2) . . ? C7 W1 C6 73.3(2) . . ? C4 W1 C6 74.8(2) . . ? C7 W1 C3 79.8(2) . . ? C4 W1 C3 116.9(2) . . ? C6 W1 C3 138.5(2) . . ? C7 W1 C2 144.0(2) . . ? C4 W1 C2 70.7(2) . . ? C6 W1 C2 140.1(2) . . ? C3 W1 C2 76.9(2) . . ? C7 W1 C8 73.6(2) . . ? C4 W1 C8 138.0(2) . . ? C6 W1 C8 123.8(2) . . ? C3 W1 C8 75.8(2) . . ? C2 W1 C8 74.3(2) . . ? C7 W1 C1 102.8(2) . . ? C4 W1 C1 80.9(2) . . ? C6 W1 C1 72.9(2) . . ? C3 W1 C1 145.1(2) . . ? C2 W1 C1 82.2(2) . . ? C8 W1 C1 71.8(2) . . ? C7 W1 C5 83.4(2) . . ? C4 W1 C5 75.0(2) . . ? C6 W1 C5 75.3(2) . . ? C3 W1 C5 70.6(2) . . ? C2 W1 C5 113.5(2) . . ? C8 W1 C5 142.1(2) . . ? C1 W1 C5 144.09(19) . . ? O8 Cu1 O7 96.79(14) . . ? O8 Cu1 O3 169.09(15) . . ? O7 Cu1 O3 81.37(13) . . ? O8 Cu1 O4 84.81(14) . . ? O7 Cu1 O4 175.14(17) . . ? O3 Cu1 O4 96.19(14) . . ? O8 Cu1 N1 95.99(16) . . ? O7 Cu1 N1 91.46(15) . . ? O3 Cu1 N1 94.81(15) . . ? O4 Cu1 N1 92.94(16) . . ? O1 Cu2 O6 173.09(17) . . ? O1 Cu2 O2 97.34(14) . . ? O6 Cu2 O2 80.84(13) . . ? O1 Cu2 O5 85.65(15) . . ? O6 Cu2 O5 96.01(14) . . ? O2 Cu2 O5 176.66(15) . . ? O12 Dy1 O9 135.56(12) . . ? O12 Dy1 O10 140.25(13) . . ? O9 Dy1 O10 71.89(12) . . ? O12 Dy1 O11 138.85(12) . . ? O9 Dy1 O11 67.63(12) . . ? O10 Dy1 O11 71.32(14) . . ? O12 Dy1 O3 81.26(11) . . ? O9 Dy1 O3 141.93(12) . . ? O10 Dy1 O3 83.77(11) . . ? O11 Dy1 O3 77.15(11) . . ? O12 Dy1 O7 74.13(12) . . ? O9 Dy1 O7 113.96(11) . . ? O10 Dy1 O7 127.05(13) . . ? O11 Dy1 O7 64.74(13) . . ? O3 Dy1 O7 59.36(10) . . ? O12 Dy1 O2 79.44(12) . . ? O9 Dy1 O2 83.70(11) . . ? O10 Dy1 O2 76.06(13) . . ? O11 Dy1 O2 141.71(12) . . ? O3 Dy1 O2 118.87(10) . . ? O7 Dy1 O2 153.48(12) . . ? O12 Dy1 N9 76.38(13) . . ? O9 Dy1 N9 127.51(13) . . ? O10 Dy1 N9 64.28(14) . . ? O11 Dy1 N9 119.61(13) . . ? O3 Dy1 N9 59.78(11) . . ? O7 Dy1 N9 114.98(11) . . ? O2 Dy1 N9 59.42(11) . . ? O12 Dy1 N10 75.03(12) . . ? O9 Dy1 N10 73.68(12) . . ? O10 Dy1 N10 143.54(12) . . ? O11 Dy1 N10 84.83(14) . . ? O3 Dy1 N10 118.03(10) . . ? O7 Dy1 N10 59.27(10) . . ? O2 Dy1 N10 111.72(11) . . ? N9 Dy1 N10 151.25(14) . . ? O12 Dy1 O6 73.87(11) . . ? O9 Dy1 O6 62.81(11) . . ? O10 Dy1 O6 114.52(11) . . ? O11 Dy1 O6 123.56(11) . . ? O3 Dy1 O6 155.07(11) . . ? O7 Dy1 O6 113.79(10) . . ? O2 Dy1 O6 55.14(10) . . ? N9 Dy1 O6 111.34(11) . . ? N10 Dy1 O6 57.15(11) . . ? C1 N1 Cu1 137.8(4) . . ? N1 C1 W1 178.0(5) . . ? N2 C2 W1 178.0(6) . . ? N3 C3 W1 179.4(5) . . ? N4 C4 W1 179.4(6) . . ? N5 C5 W1 179.5(6) . . ? N6 C6 W1 178.8(5) . . ? N7 C7 W1 177.1(6) . . ? N8 C8 W1 175.4(6) . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C10 C11 123.5(5) . . ? O1 C10 C9 116.9(4) . . ? C11 C10 C9 119.5(5) . . ? C12 C11 C10 127.4(5) . . ? C12 C11 H11 116.3 . . ? C10 C11 H11 116.3 . . ? O2 C12 C11 125.2(4) . . ? O2 C12 C13 114.7(4) . . ? C11 C12 C13 120.1(5) . . ? N9 C13 C14 122.8(5) . . ? N9 C13 C12 115.5(4) . . ? C14 C13 C12 121.5(5) . . ? C15 C14 C13 119.3(6) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C16 C15 C14 118.7(6) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C15 C16 C17 119.3(5) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? N9 C17 C16 122.7(5) . . ? N9 C17 C18 115.1(4) . . ? C16 C17 C18 122.2(4) . . ? O3 C18 C19 125.1(5) . . ? O3 C18 C17 114.6(4) . . ? C19 C18 C17 120.2(4) . . ? C18 C19 C20 127.5(5) . . ? C18 C19 H19 116.2 . . ? C20 C19 H19 116.2 . . ? O4 C20 C19 124.4(4) . . ? O4 C20 C21 117.4(5) . . ? C19 C20 C21 118.2(5) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 C23 C24 124.7(4) . . ? O5 C23 C22 117.0(5) . . ? C24 C23 C22 118.2(5) . . ? C25 C24 C23 124.9(5) . . ? C25 C24 H24 117.6 . . ? C23 C24 H24 117.6 . . ? O6 C25 C24 126.6(5) . . ? O6 C25 C26 113.4(4) . . ? C24 C25 C26 119.9(5) . . ? N10 C26 C27 123.1(5) . . ? N10 C26 C25 115.8(5) . . ? C27 C26 C25 120.9(5) . . ? C28 C27 C26 118.3(6) . . ? C28 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? C27 C28 C29 120.0(7) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 117.8(7) . . ? C30 C29 H29 121.1 . . ? C28 C29 H29 121.1 . . ? N10 C30 C29 123.8(6) . . ? N10 C30 C31 115.8(5) . . ? C29 C30 C31 120.3(6) . . ? O7 C31 C32 125.3(4) . . ? O7 C31 C30 114.6(5) . . ? C32 C31 C30 120.1(5) . . ? C31 C32 C33 126.3(5) . . ? C31 C32 H32 116.9 . . ? C33 C32 H32 116.9 . . ? O8 C33 C32 125.3(4) . . ? O8 C33 C34 116.6(4) . . ? C32 C33 C34 118.1(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C13 N9 C17 116.9(4) . . ? C13 N9 Dy1 121.2(3) . . ? C17 N9 Dy1 121.2(3) . . ? C30 N10 C26 117.1(5) . . ? C30 N10 Dy1 120.4(3) . . ? C26 N10 Dy1 122.5(3) . . ? C10 O1 Cu2 124.2(3) . . ? C12 O2 Cu2 121.2(3) . . ? C12 O2 Dy1 125.3(3) . . ? Cu2 O2 Dy1 112.33(14) . . ? C18 O3 Cu1 118.7(3) . . ? C18 O3 Dy1 129.1(3) . . ? Cu1 O3 Dy1 109.71(13) . . ? C20 O4 Cu1 121.4(3) . . ? C23 O5 Cu2 122.3(3) . . ? C25 O6 Cu2 121.8(3) . . ? C25 O6 Dy1 122.8(3) . . ? Cu2 O6 Dy1 106.87(13) . . ? C31 O7 Cu1 121.9(3) . . ? C31 O7 Dy1 128.7(3) . . ? Cu1 O7 Dy1 108.98(14) . . ? C33 O8 Cu1 122.9(3) . . ? Dy1 O9 H9D 109.5 . . ? Dy1 O9 H9E 109.1 . . ? H9D O9 H9E 109.6 . . ? Dy1 O10 H10A 109.0 . . ? Dy1 O10 H10B 109.5 . . ? H10A O10 H10B 109.7 . . ? Dy1 O11 H11A 125.6 . . ? Dy1 O11 H11B 125.3 . . ? H11A O11 H11B 109.1 . . ? H17A O17 H17B 94.7(13) . . ? H17A C35 H35A 78.8 . . ? H17A C35 H35B 126.0 . . ? H35A C35 H35B 109.5 . . ? H17A C35 H35C 31.0 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? H13B O13 H13A 103.8(13) . . ? H15A O15 H15B 109.7 . . ? C36 O16 H16A 120.3 . . ? O16 C36 H36A 109.5 . . ? O16 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O16 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.918 _refine_diff_density_min -1.649 _refine_diff_density_rms 0.175