# Electronic Supplementary Material (ESI) for Chemical Communications # 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_nb3_195_0m #TrackingRef 'web_deposit_cif_file_0_Lise-MarieChamoreau_1349269842.nb3_195_0m - publi.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H52 Cu2 Mo2 N20 O16 Tb2, 2(C30 H22 N6 Ni), 2(Cl O4), 20(H2 O)' _chemical_formula_sum 'C112 H136 Cl2 Cu2 Gd0 Mo2 N32 Ni2 O44 Tb2' _chemical_formula_weight 3459.65 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 '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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d d' _symmetry_space_group_name_Hall '-F 2uv 2vw' _symmetry_Int_Tables_number 70 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+1/4, z' 'x, -y+1/4, -z+1/4' '-x+1/4, y, -z+1/4' 'x, y+1/2, z+1/2' '-x+1/4, -y+3/4, z+1/2' 'x, -y+3/4, -z+3/4' '-x+1/4, y+1/2, -z+3/4' 'x+1/2, y, z+1/2' '-x+3/4, -y+1/4, z+1/2' 'x+1/2, -y+1/4, -z+3/4' '-x+3/4, y, -z+3/4' 'x+1/2, y+1/2, z' '-x+3/4, -y+3/4, z' 'x+1/2, -y+3/4, -z+1/4' '-x+3/4, y+1/2, -z+1/4' '-x, -y, -z' 'x-1/4, y-1/4, -z' '-x, y-1/4, z-1/4' 'x-1/4, -y, z-1/4' '-x, -y+1/2, -z+1/2' 'x-1/4, y+1/4, -z+1/2' '-x, y+1/4, z+1/4' 'x-1/4, -y+1/2, z+1/4' '-x+1/2, -y, -z+1/2' 'x+1/4, y-1/4, -z+1/2' '-x+1/2, y-1/4, z+1/4' 'x+1/4, -y, z+1/4' '-x+1/2, -y+1/2, -z' 'x+1/4, y+1/4, -z' '-x+1/2, y+1/4, z-1/4' 'x+1/4, -y+1/2, z-1/4' _cell_length_a 23.0051(4) _cell_length_b 29.8285(6) _cell_length_c 42.2334(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 28980.9(9) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9910 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 32 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13968 _exptl_absorpt_coefficient_mu 1.797 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9302 _exptl_absorpt_correction_T_max 0.9481 _exptl_absorpt_process_details ; SADABS, Bruker AXS Inc., Madison, Wisconsin, USA. ; _diffrn_ambient_temperature 200(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83991 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0144 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 62 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 32.02 _reflns_number_total 12598 _reflns_number_gt 9693 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SUPERFLIP (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND. Crystal Impact GbR, Bonn, Germany' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+471.7736P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12598 _refine_ls_number_parameters 425 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1210 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.950310(14) 0.1250 0.1250 0.01456(7) Uani 1 2 d S . . Tb1 Tb 1.1250 0.1250 0.031764(4) 0.01661(6) Uani 1 2 d S . . Cu1 Cu 1.1250 0.1250 -0.047679(13) 0.02627(12) Uani 1 2 d S . . O1 O 1.10549(12) 0.08539(8) -0.01385(5) 0.0250(5) Uani 1 1 d . . . O2 O 1.10135(12) 0.04269(8) 0.03774(6) 0.0260(5) Uani 1 1 d . . . N1 N 1.06127(13) 0.11998(11) 0.07625(7) 0.0267(6) Uani 1 1 d . . . N2 N 0.99782(16) 0.22931(11) 0.11837(8) 0.0344(7) Uani 1 1 d . . . N3 N 0.83980(15) 0.05867(12) 0.10624(8) 0.0332(7) Uani 1 1 d . . . N4 N 0.91488(15) 0.15518(12) 0.05183(7) 0.0322(6) Uani 1 1 d . . . N5 N 1.10025(16) 0.08481(12) -0.08047(7) 0.0327(7) Uani 1 1 d . . . C1 C 1.02240(14) 0.12001(11) 0.09375(7) 0.0214(6) Uani 1 1 d . . . C2 C 0.98159(14) 0.19320(11) 0.12150(8) 0.0234(6) Uani 1 1 d . . . C3 C 0.87769(14) 0.08205(11) 0.11320(7) 0.0223(6) Uani 1 1 d . . . C4 C 0.92399(14) 0.14417(11) 0.07759(7) 0.0225(6) Uani 1 1 d . . . C5 C 1.1016(2) 0.01894(14) 0.06755(9) 0.0395(9) Uani 1 1 d . . . H5A H 1.0623 0.0079 0.0721 0.059 Uiso 1 1 calc R . . H5B H 1.1141 0.0392 0.0845 0.059 Uiso 1 1 calc R . . H5C H 1.1285 -0.0065 0.0663 0.059 Uiso 1 1 calc R . . C6 C 1.08699(15) 0.01777(11) 0.01098(8) 0.0250(6) Uani 1 1 d . . . C7 C 1.07064(19) -0.02663(13) 0.01069(10) 0.0341(8) Uani 1 1 d . . . H7 H 1.0670 -0.0428 0.0300 0.041 Uiso 1 1 calc R . . C8 C 1.0595(2) -0.04761(14) -0.01813(12) 0.0408(9) Uani 1 1 d . . . H8 H 1.0487 -0.0784 -0.0185 0.049 Uiso 1 1 calc R . . C9 C 1.06393(19) -0.02414(14) -0.04608(10) 0.0371(9) Uani 1 1 d . . . H9 H 1.0559 -0.0389 -0.0655 0.045 Uiso 1 1 calc R . . C10 C 1.08013(16) 0.02134(13) -0.04629(9) 0.0293(7) Uani 1 1 d . . . C11 C 1.09124(14) 0.04258(11) -0.01710(8) 0.0232(6) Uani 1 1 d . . . C12 C 1.08414(18) 0.04432(15) -0.07671(9) 0.0335(8) Uani 1 1 d . . . H12 H 1.0740 0.0278 -0.0951 0.040 Uiso 1 1 calc R . . C13 C 1.1002(2) 0.10777(18) -0.11126(9) 0.0421(10) Uani 1 1 d . . . H13A H 1.0625 0.1230 -0.1147 0.051 Uiso 1 1 calc R . . H13B H 1.1060 0.0858 -0.1285 0.051 Uiso 1 1 calc R . . Ni2 Ni 0.8750 0.3750 0.010743(14) 0.02142(12) Uani 1 2 d S . . N6 N 0.84076(14) 0.33293(10) 0.04616(7) 0.0287(6) Uani 1 1 d . . . N7 N 0.93399(14) 0.32606(10) 0.01229(7) 0.0273(6) Uani 1 1 d . . . N8 N 0.93313(14) 0.39499(12) -0.02470(8) 0.0316(6) Uani 1 1 d . . . C14 C 0.79236(19) 0.33898(15) 0.06264(10) 0.0373(8) Uani 1 1 d . . . H14 H 0.7687 0.3642 0.0578 0.045 Uiso 1 1 calc R . . C15 C 0.7747(2) 0.31017(17) 0.08657(11) 0.0459(11) Uani 1 1 d . . . H15 H 0.7397 0.3154 0.0979 0.055 Uiso 1 1 calc R . . C16 C 0.8091(2) 0.27389(17) 0.09347(11) 0.0469(11) Uani 1 1 d . . . H16 H 0.7982 0.2538 0.1099 0.056 Uiso 1 1 calc R . . C17 C 0.8593(2) 0.26665(15) 0.07656(10) 0.0407(9) Uani 1 1 d . . . H17 H 0.8832 0.2414 0.0809 0.049 Uiso 1 1 calc R . . C18 C 0.87451(17) 0.29689(12) 0.05297(9) 0.0295(7) Uani 1 1 d . . . C19 C 0.92786(17) 0.29346(12) 0.03388(9) 0.0303(7) Uani 1 1 d . . . C20 C 0.9704(2) 0.26047(15) 0.03690(13) 0.0453(11) Uani 1 1 d . . . H20 H 0.9666 0.2373 0.0522 0.054 Uiso 1 1 calc R . . C21 C 1.0174(2) 0.26226(17) 0.01743(15) 0.0524(13) Uani 1 1 d . . . H21 H 1.0463 0.2396 0.0189 0.063 Uiso 1 1 calc R . . C22 C 1.02404(19) 0.29665(16) -0.00461(13) 0.0447(10) Uani 1 1 d . . . H22 H 1.0574 0.2982 -0.0178 0.054 Uiso 1 1 calc R . . C23 C 0.98041(16) 0.32864(13) -0.00668(9) 0.0302(7) Uani 1 1 d . . . C24 C 0.97891(17) 0.36692(15) -0.02865(10) 0.0338(8) Uani 1 1 d . . . C25 C 1.0191(2) 0.37359(19) -0.05243(14) 0.0516(12) Uani 1 1 d . . . H25 H 1.0509 0.3535 -0.0548 0.062 Uiso 1 1 calc R . . C26 C 1.0131(3) 0.4092(2) -0.07261(15) 0.0645(16) Uani 1 1 d . . . H26 H 1.0409 0.4144 -0.0888 0.077 Uiso 1 1 calc R . . C27 C 0.9661(3) 0.4372(2) -0.06907(15) 0.0620(15) Uani 1 1 d . . . H27 H 0.9606 0.4617 -0.0832 0.074 Uiso 1 1 calc R . . C28 C 0.9268(2) 0.42953(17) -0.04472(12) 0.0445(10) Uani 1 1 d . . . H28 H 0.8946 0.4492 -0.0422 0.053 Uiso 1 1 calc R . . O1W O 1.21819(11) 0.09657(10) 0.01707(6) 0.0301(5) Uani 1 1 d . . . H1A H 1.2306 0.0903 -0.0010 0.045 Uiso 1 1 d R . . H1B H 1.2506 0.0945 0.0266 0.045 Uiso 1 1 d R . . O2W O 1.02176(16) 0.16412(13) -0.04525(8) 0.0477(8) Uani 1 1 d . . . H2A H 1.0003 0.1499 -0.0584 0.071 Uiso 1 1 d R . . H2B H 1.0210 0.1858 -0.0581 0.071 Uiso 1 1 d R . . Cl1 Cl 0.6250 0.2822(7) 0.1250 0.357(8) Uiso 1 2 d SD . . O4 O 0.6237(10) 0.2863(9) 0.0893(4) 0.370 Uiso 1 1 d D . . O3 O 0.5817(9) 0.2466(7) 0.1158(5) 0.343(11) Uiso 1 1 d D . . O3W O 0.7648(2) -0.00339(16) 0.07410(11) 0.0715(13) Uani 1 1 d . . . O5WA O 1.0234(5) 0.3209(4) 0.1074(3) 0.082(3) Uiso 0.50 1 d P . . O5WB O 1.0633(4) 0.3083(3) 0.11795(19) 0.0530(17) Uiso 0.50 1 d P . . O6WA O 1.0000 0.5000 0.0000 0.153(5) Uiso 1 2 d S . . O7WA O 1.0466(5) 0.3517(4) 0.1739(3) 0.086(3) Uiso 0.50 1 d P . . O7WB O 1.0520(5) 0.3778(4) 0.1589(3) 0.081(3) Uiso 0.50 1 d P . . O8W O 0.6604(4) 0.3934(3) 0.0589(2) 0.071(2) Uiso 0.50 1 d P . . O9W O 0.6534(7) 0.3127(5) 0.0120(3) 0.231(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01448(14) 0.01712(14) 0.01210(13) -0.00005(11) 0.000 0.000 Tb1 0.01847(9) 0.01790(9) 0.01345(9) 0.000 0.000 0.00049(7) Cu1 0.0371(3) 0.0283(3) 0.0134(2) 0.000 0.000 -0.0045(2) O1 0.0344(12) 0.0232(11) 0.0175(9) -0.0024(8) -0.0019(9) -0.0048(10) O2 0.0359(13) 0.0220(11) 0.0201(10) -0.0003(8) 0.0001(9) -0.0012(10) N1 0.0218(12) 0.0381(16) 0.0203(12) 0.0030(11) 0.0025(10) 0.0052(11) N2 0.0395(18) 0.0272(15) 0.0366(17) 0.0009(12) 0.0018(14) -0.0043(13) N3 0.0318(16) 0.0360(17) 0.0319(15) 0.0015(13) -0.0036(12) -0.0094(13) N4 0.0377(17) 0.0350(16) 0.0238(13) 0.0034(12) -0.0037(12) 0.0025(13) N5 0.0380(17) 0.0422(18) 0.0178(12) -0.0054(12) -0.0026(11) -0.0001(14) C1 0.0206(13) 0.0272(15) 0.0166(12) 0.0006(10) 0.0003(10) 0.0029(11) C2 0.0230(14) 0.0247(14) 0.0223(13) 0.0001(11) -0.0002(11) 0.0004(11) C3 0.0234(14) 0.0256(14) 0.0180(12) -0.0001(11) -0.0022(11) 0.0003(12) C4 0.0232(14) 0.0243(14) 0.0201(13) 0.0006(11) 0.0000(11) -0.0003(11) C5 0.063(3) 0.0290(18) 0.0263(16) 0.0075(14) 0.0009(17) 0.0029(18) C6 0.0266(15) 0.0215(14) 0.0270(15) -0.0042(11) 0.0024(12) 0.0016(12) C7 0.040(2) 0.0220(15) 0.040(2) -0.0026(14) 0.0074(16) -0.0013(14) C8 0.044(2) 0.0265(18) 0.051(2) -0.0130(17) 0.0058(19) -0.0070(16) C9 0.038(2) 0.0334(19) 0.040(2) -0.0186(16) 0.0035(16) -0.0054(16) C10 0.0292(16) 0.0316(17) 0.0271(15) -0.0125(13) 0.0000(13) -0.0007(13) C11 0.0222(13) 0.0238(14) 0.0238(13) -0.0061(11) -0.0003(11) 0.0004(11) C12 0.0358(19) 0.042(2) 0.0224(15) -0.0115(14) -0.0024(13) -0.0003(16) C13 0.050(3) 0.060(3) 0.0167(15) 0.0006(16) -0.0044(15) 0.001(2) Ni2 0.0203(3) 0.0202(3) 0.0238(3) 0.000 0.000 0.0038(2) N6 0.0318(15) 0.0258(14) 0.0286(14) 0.0026(11) 0.0004(11) 0.0033(12) N7 0.0271(14) 0.0246(13) 0.0304(14) -0.0037(11) -0.0014(11) 0.0038(11) N8 0.0290(15) 0.0327(16) 0.0332(15) 0.0008(13) 0.0051(12) 0.0015(12) C14 0.040(2) 0.036(2) 0.0359(19) 0.0050(16) 0.0100(16) 0.0022(16) C15 0.049(3) 0.049(3) 0.040(2) 0.0055(19) 0.0142(19) -0.007(2) C16 0.063(3) 0.042(2) 0.036(2) 0.0099(18) 0.003(2) -0.009(2) C17 0.055(3) 0.0314(19) 0.035(2) 0.0092(16) -0.0070(18) -0.0020(18) C18 0.0368(18) 0.0228(15) 0.0289(15) 0.0002(12) -0.0051(14) 0.0013(14) C19 0.0322(17) 0.0230(15) 0.0357(18) -0.0009(13) -0.0084(14) 0.0035(13) C20 0.041(2) 0.0280(19) 0.067(3) 0.0042(19) -0.008(2) 0.0095(17) C21 0.038(2) 0.034(2) 0.085(4) 0.002(2) 0.002(2) 0.0133(19) C22 0.0282(19) 0.040(2) 0.066(3) -0.010(2) 0.0040(19) 0.0097(17) C23 0.0249(16) 0.0286(16) 0.0370(18) -0.0078(14) 0.0002(13) 0.0031(13) C24 0.0261(17) 0.039(2) 0.0359(18) -0.0063(15) 0.0059(14) -0.0004(14) C25 0.040(2) 0.059(3) 0.056(3) -0.002(2) 0.021(2) 0.001(2) C26 0.060(3) 0.075(4) 0.058(3) 0.014(3) 0.029(3) -0.003(3) C27 0.062(3) 0.065(4) 0.059(3) 0.023(3) 0.016(3) -0.007(3) C28 0.043(2) 0.043(2) 0.047(2) 0.0124(19) 0.0090(19) 0.0006(19) O1W 0.0251(12) 0.0411(15) 0.0241(11) -0.0071(10) 0.0002(9) 0.0076(11) O2W 0.0495(19) 0.061(2) 0.0324(15) 0.0108(14) -0.0094(13) -0.0037(16) O3W 0.070(3) 0.077(3) 0.067(3) -0.027(2) 0.001(2) -0.027(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Mo1 C1 2.125(3) 3 ? Mo1 C1 2.125(3) . ? Mo1 C2 2.163(3) . ? Mo1 C2 2.163(3) 3 ? Mo1 C3 2.163(3) . ? Mo1 C3 2.163(3) 3 ? Mo1 C4 2.168(3) . ? Mo1 C4 2.168(3) 3 ? Tb1 O1 2.304(2) . ? Tb1 O1 2.304(2) 2_755 ? Tb1 O1W 2.388(3) 2_755 ? Tb1 O1W 2.388(3) . ? Tb1 N1 2.388(3) . ? Tb1 N1 2.388(3) 2_755 ? Tb1 O2 2.527(2) 2_755 ? Tb1 O2 2.527(2) . ? Tb1 Cu1 3.3551(6) . ? Cu1 O1 1.907(2) 2_755 ? Cu1 O1 1.907(2) . ? Cu1 N5 1.918(3) . ? Cu1 N5 1.918(3) 2_755 ? O1 C11 1.326(4) . ? O2 C6 1.393(4) . ? O2 C5 1.444(4) . ? N1 C1 1.160(4) . ? N2 C2 1.148(5) . ? N3 C3 1.155(5) . ? N4 C4 1.156(4) . ? N5 C12 1.273(6) . ? N5 C13 1.470(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.377(5) . ? C6 C11 1.401(5) . ? C7 C8 1.393(6) . ? C7 H7 0.9500 . ? C8 C9 1.376(7) . ? C8 H8 0.9500 . ? C9 C10 1.407(6) . ? C9 H9 0.9500 . ? C10 C11 1.410(5) . ? C10 C12 1.459(6) . ? C12 H12 0.9500 . ? C13 C13 1.536(10) 2_755 ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? Ni2 N7 1.994(3) 14_655 ? Ni2 N7 1.994(3) . ? Ni2 N8 2.094(3) 14_655 ? Ni2 N8 2.094(3) . ? Ni2 N6 2.105(3) 14_655 ? Ni2 N6 2.105(3) . ? N6 C14 1.325(5) . ? N6 C18 1.357(5) . ? N7 C23 1.337(5) . ? N7 C19 1.340(5) . ? N8 C28 1.341(6) . ? N8 C24 1.356(5) . ? C14 C15 1.388(6) . ? C14 H14 0.9500 . ? C15 C16 1.371(7) . ? C15 H15 0.9500 . ? C16 C17 1.376(7) . ? C16 H16 0.9500 . ? C17 C18 1.389(6) . ? C17 H17 0.9500 . ? C18 C19 1.472(6) . ? C19 C20 1.393(5) . ? C20 C21 1.360(8) . ? C20 H20 0.9500 . ? C21 C22 1.394(8) . ? C21 H21 0.9500 . ? C22 C23 1.387(6) . ? C22 H22 0.9500 . ? C23 C24 1.472(6) . ? C24 C25 1.380(6) . ? C25 C26 1.368(8) . ? C25 H25 0.9500 . ? C26 C27 1.375(9) . ? C26 H26 0.9500 . ? C27 C28 1.389(7) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? O1W H1A 0.8359 . ? O1W H1B 0.8490 . ? O2W H2A 0.8551 . ? O2W H2B 0.8456 . ? Cl1 O3 1.505(15) . ? Cl1 O3 1.505(15) 4_655 ? O5WA O5WB 1.090(12) . ? O7WA O7WB 1.012(14) . ? 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 C1 Mo1 C1 77.38(17) 3 . ? C1 Mo1 C2 73.56(12) 3 . ? C1 Mo1 C2 76.33(12) . . ? C1 Mo1 C2 76.33(12) 3 3 ? C1 Mo1 C2 73.56(12) . 3 ? C2 Mo1 C2 141.14(18) . 3 ? C1 Mo1 C3 141.93(12) 3 . ? C1 Mo1 C3 114.71(12) . . ? C2 Mo1 C3 142.95(12) . . ? C2 Mo1 C3 73.48(12) 3 . ? C1 Mo1 C3 114.71(12) 3 3 ? C1 Mo1 C3 141.93(12) . 3 ? C2 Mo1 C3 73.48(12) . 3 ? C2 Mo1 C3 142.95(12) 3 3 ? C3 Mo1 C3 78.90(18) . 3 ? C1 Mo1 C4 140.63(12) 3 . ? C1 Mo1 C4 70.30(12) . . ? C2 Mo1 C4 77.40(12) . . ? C2 Mo1 C4 113.83(12) 3 . ? C3 Mo1 C4 74.20(12) . . ? C3 Mo1 C4 80.85(12) 3 . ? C1 Mo1 C4 70.30(12) 3 3 ? C1 Mo1 C4 140.63(12) . 3 ? C2 Mo1 C4 113.83(12) . 3 ? C2 Mo1 C4 77.40(12) 3 3 ? C3 Mo1 C4 80.85(12) . 3 ? C3 Mo1 C4 74.20(12) 3 3 ? C4 Mo1 C4 147.57(17) . 3 ? O1 Tb1 O1 66.53(12) . 2_755 ? O1 Tb1 O1W 77.87(10) . 2_755 ? O1 Tb1 O1W 77.02(9) 2_755 2_755 ? O1 Tb1 O1W 77.02(9) . . ? O1 Tb1 O1W 77.87(10) 2_755 . ? O1W Tb1 O1W 149.86(12) 2_755 . ? O1 Tb1 N1 120.41(10) . . ? O1 Tb1 N1 144.06(10) 2_755 . ? O1W Tb1 N1 71.06(9) 2_755 . ? O1W Tb1 N1 137.19(10) . . ? O1 Tb1 N1 144.06(10) . 2_755 ? O1 Tb1 N1 120.41(10) 2_755 2_755 ? O1W Tb1 N1 137.19(10) 2_755 2_755 ? O1W Tb1 N1 71.06(9) . 2_755 ? N1 Tb1 N1 76.23(15) . 2_755 ? O1 Tb1 O2 128.58(8) . 2_755 ? O1 Tb1 O2 62.84(8) 2_755 2_755 ? O1W Tb1 O2 82.78(9) 2_755 2_755 ? O1W Tb1 O2 100.23(9) . 2_755 ? N1 Tb1 O2 96.57(10) . 2_755 ? N1 Tb1 O2 74.24(10) 2_755 2_755 ? O1 Tb1 O2 62.84(8) . . ? O1 Tb1 O2 128.58(8) 2_755 . ? O1W Tb1 O2 100.23(9) 2_755 . ? O1W Tb1 O2 82.78(9) . . ? N1 Tb1 O2 74.24(10) . . ? N1 Tb1 O2 96.57(10) 2_755 . ? O2 Tb1 O2 168.53(11) 2_755 . ? O1 Tb1 Cu1 33.26(6) . . ? O1 Tb1 Cu1 33.26(6) 2_755 . ? O1W Tb1 Cu1 74.93(6) 2_755 . ? O1W Tb1 Cu1 74.93(6) . . ? N1 Tb1 Cu1 141.89(7) . . ? N1 Tb1 Cu1 141.89(7) 2_755 . ? O2 Tb1 Cu1 95.73(5) 2_755 . ? O2 Tb1 Cu1 95.73(5) . . ? O1 Cu1 O1 83.00(14) 2_755 . ? O1 Cu1 N5 176.14(13) 2_755 . ? O1 Cu1 N5 94.80(13) . . ? O1 Cu1 N5 94.80(13) 2_755 2_755 ? O1 Cu1 N5 176.14(13) . 2_755 ? N5 Cu1 N5 87.6(2) . 2_755 ? O1 Cu1 Tb1 41.50(7) 2_755 . ? O1 Cu1 Tb1 41.50(7) . . ? N5 Cu1 Tb1 136.22(10) . . ? N5 Cu1 Tb1 136.22(10) 2_755 . ? C11 O1 Cu1 125.3(2) . . ? C11 O1 Tb1 128.9(2) . . ? Cu1 O1 Tb1 105.24(11) . . ? C6 O2 C5 116.5(3) . . ? C6 O2 Tb1 119.2(2) . . ? C5 O2 Tb1 124.2(2) . . ? C1 N1 Tb1 167.0(3) . . ? C12 N5 C13 123.5(3) . . ? C12 N5 Cu1 126.1(3) . . ? C13 N5 Cu1 110.4(3) . . ? N1 C1 Mo1 175.9(3) . . ? N2 C2 Mo1 177.3(3) . . ? N3 C3 Mo1 178.2(3) . . ? N4 C4 Mo1 174.2(3) . . ? O2 C5 H5A 109.5 . . ? O2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 O2 125.8(3) . . ? C7 C6 C11 121.3(3) . . ? O2 C6 C11 112.9(3) . . ? C6 C7 C8 119.4(4) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C9 C8 C7 120.5(4) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 121.0(4) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C9 C10 C11 118.4(4) . . ? C9 C10 C12 118.4(3) . . ? C11 C10 C12 123.2(3) . . ? O1 C11 C6 116.0(3) . . ? O1 C11 C10 124.6(3) . . ? C6 C11 C10 119.4(3) . . ? N5 C12 C10 125.0(3) . . ? N5 C12 H12 117.5 . . ? C10 C12 H12 117.5 . . ? N5 C13 C13 108.1(3) . 2_755 ? N5 C13 H13A 110.1 . . ? C13 C13 H13A 110.1 2_755 . ? N5 C13 H13B 110.1 . . ? C13 C13 H13B 110.1 2_755 . ? H13A C13 H13B 108.4 . . ? N7 Ni2 N7 176.25(18) 14_655 . ? N7 Ni2 N8 78.30(13) 14_655 14_655 ? N7 Ni2 N8 104.45(13) . 14_655 ? N7 Ni2 N8 104.45(13) 14_655 . ? N7 Ni2 N8 78.30(13) . . ? N8 Ni2 N8 88.73(19) 14_655 . ? N7 Ni2 N6 78.17(13) 14_655 14_655 ? N7 Ni2 N6 99.12(12) . 14_655 ? N8 Ni2 N6 156.43(13) 14_655 14_655 ? N8 Ni2 N6 95.70(13) . 14_655 ? N7 Ni2 N6 99.12(12) 14_655 . ? N7 Ni2 N6 78.17(13) . . ? N8 Ni2 N6 95.70(13) 14_655 . ? N8 Ni2 N6 156.43(13) . . ? N6 Ni2 N6 89.46(18) 14_655 . ? C14 N6 C18 118.5(3) . . ? C14 N6 Ni2 127.3(3) . . ? C18 N6 Ni2 114.1(3) . . ? C23 N7 C19 122.2(3) . . ? C23 N7 Ni2 118.8(3) . . ? C19 N7 Ni2 118.8(3) . . ? C28 N8 C24 118.8(4) . . ? C28 N8 Ni2 126.9(3) . . ? C24 N8 Ni2 114.1(3) . . ? N6 C14 C15 123.0(4) . . ? N6 C14 H14 118.5 . . ? C15 C14 H14 118.5 . . ? C16 C15 C14 118.4(4) . . ? C16 C15 H15 120.8 . . ? C14 C15 H15 120.8 . . ? C15 C16 C17 119.8(4) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C18 118.8(4) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? N6 C18 C17 121.5(4) . . ? N6 C18 C19 114.6(3) . . ? C17 C18 C19 123.9(4) . . ? N7 C19 C20 120.0(4) . . ? N7 C19 C18 114.2(3) . . ? C20 C19 C18 125.8(4) . . ? C21 C20 C19 118.4(5) . . ? C21 C20 H20 120.8 . . ? C19 C20 H20 120.8 . . ? C20 C21 C22 121.3(4) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C23 C22 C21 118.0(4) . . ? C23 C22 H22 121.0 . . ? C21 C22 H22 121.0 . . ? N7 C23 C22 120.0(4) . . ? N7 C23 C24 113.8(3) . . ? C22 C23 C24 126.2(4) . . ? N8 C24 C25 121.4(4) . . ? N8 C24 C23 114.8(3) . . ? C25 C24 C23 123.7(4) . . ? C26 C25 C24 119.8(5) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 118.9(5) . . ? C25 C26 H26 120.5 . . ? C27 C26 H26 120.5 . . ? C26 C27 C28 119.5(5) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? N8 C28 C27 121.5(5) . . ? N8 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? Tb1 O1W H1A 128.6 . . ? Tb1 O1W H1B 133.6 . . ? H1A O1W H1B 96.7 . . ? H2A O2W H2B 87.2 . . ? O3 Cl1 O3 90(2) . 4_655 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 32.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.451 _refine_diff_density_min -1.563 _refine_diff_density_rms 0.160 _database_code_depnum_ccdc_archive 'CCDC 904312' ####################################################################### # # 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_nb4_11_0m #TrackingRef 'web_deposit_cif_file_1_Lise-MarieChamoreau_1349269842.nb4_11_0m - publi.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H52 Cu2 N20 O16 Tb2 W2, 2(C30 H22 N6 Ni), 2(Cl O4), 20 (H2 O)' _chemical_formula_sum 'C112 H136 Cl2 Cu2 N32 Ni2 O44 Tb2 W2' _chemical_formula_weight 3635.47 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d d' _symmetry_space_group_name_Hall '-F 2uv 2vw' _symmetry_Int_Tables_number 70 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+1/4, z' 'x, -y+1/4, -z+1/4' '-x+1/4, y, -z+1/4' 'x, y+1/2, z+1/2' '-x+1/4, -y+3/4, z+1/2' 'x, -y+3/4, -z+3/4' '-x+1/4, y+1/2, -z+3/4' 'x+1/2, y, z+1/2' '-x+3/4, -y+1/4, z+1/2' 'x+1/2, -y+1/4, -z+3/4' '-x+3/4, y, -z+3/4' 'x+1/2, y+1/2, z' '-x+3/4, -y+3/4, z' 'x+1/2, -y+3/4, -z+1/4' '-x+3/4, y+1/2, -z+1/4' '-x, -y, -z' 'x-1/4, y-1/4, -z' '-x, y-1/4, z-1/4' 'x-1/4, -y, z-1/4' '-x, -y+1/2, -z+1/2' 'x-1/4, y+1/4, -z+1/2' '-x, y+1/4, z+1/4' 'x-1/4, -y+1/2, z+1/4' '-x+1/2, -y, -z+1/2' 'x+1/4, y-1/4, -z+1/2' '-x+1/2, y-1/4, z+1/4' 'x+1/4, -y, z+1/4' '-x+1/2, -y+1/2, -z' 'x+1/4, y+1/4, -z' '-x+1/2, y+1/4, z-1/4' 'x+1/4, -y+1/2, z-1/4' _cell_length_a 23.0007(7) _cell_length_b 29.7883(9) _cell_length_c 42.1077(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 28850.2(15) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9764 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 32 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14480 _exptl_absorpt_coefficient_mu 3.225 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.672 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details ; SADABS, Bruker AXS Inc., Madison, Wisconsin, USA. ; _diffrn_ambient_temperature 200(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 85990 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -62 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 32.02 _reflns_number_total 12546 _reflns_number_gt 8871 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND. Crystal Impact GbR, Bonn, Germany' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+381.0761P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12546 _refine_ls_number_parameters 453 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0846 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.003 _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 0.949650(7) 0.1250 0.1250 0.01661(4) Uani 1 2 d S . . Tb1 Tb 1.1250 0.1250 0.031766(4) 0.01799(5) Uani 1 2 d S . . Cu1 Cu 1.1250 0.1250 -0.047854(13) 0.02960(13) Uani 1 2 d S . . O1 O 1.10581(12) 0.08527(8) -0.01394(5) 0.0275(5) Uani 1 1 d . . . O2 O 1.10130(12) 0.04245(8) 0.03788(6) 0.0274(5) Uani 1 1 d . . . N1 N 1.06084(13) 0.11991(11) 0.07623(7) 0.0281(6) Uani 1 1 d . . . N2 N 0.99751(16) 0.22961(11) 0.11777(8) 0.0352(7) Uani 1 1 d . . . N3 N 0.83981(15) 0.05800(12) 0.10613(8) 0.0348(7) Uani 1 1 d . . . N4 N 0.91254(15) 0.15520(11) 0.05173(7) 0.0341(7) Uani 1 1 d . . . N5 N 1.10036(16) 0.08490(12) -0.08074(7) 0.0349(7) Uani 1 1 d . . . C1 C 1.02212(14) 0.11966(11) 0.09362(7) 0.0226(6) Uani 1 1 d . . . C2 C 0.98112(15) 0.19327(11) 0.12106(8) 0.0243(6) Uani 1 1 d . . . C3 C 0.87719(15) 0.08155(11) 0.11310(7) 0.0237(6) Uani 1 1 d . . . C4 C 0.92274(15) 0.14424(11) 0.07751(8) 0.0239(6) Uani 1 1 d . . . C5 C 1.1016(2) 0.01864(14) 0.06776(9) 0.0410(9) Uani 1 1 d . . . H5A H 1.0622 0.0084 0.0727 0.062 Uiso 1 1 calc R . . H5B H 1.1154 0.0387 0.0846 0.062 Uiso 1 1 calc R . . H5C H 1.1276 -0.0074 0.0662 0.062 Uiso 1 1 calc R . . C6 C 1.08672(16) 0.01764(11) 0.01103(8) 0.0262(6) Uani 1 1 d . . . C7 C 1.07042(18) -0.02692(12) 0.01073(10) 0.0350(8) Uani 1 1 d . . . H7 H 1.0673 -0.0433 0.0300 0.042 Uiso 1 1 calc R . . C8 C 1.0587(2) -0.04757(14) -0.01802(11) 0.0417(10) Uani 1 1 d . . . H8 H 1.0472 -0.0782 -0.0184 0.050 Uiso 1 1 calc R . . C9 C 1.06340(19) -0.02420(14) -0.04605(10) 0.0392(9) Uani 1 1 d . . . H9 H 1.0554 -0.0391 -0.0655 0.047 Uiso 1 1 calc R . . C10 C 1.07984(16) 0.02116(13) -0.04648(9) 0.0303(7) Uani 1 1 d . . . C11 C 1.09102(15) 0.04238(11) -0.01714(8) 0.0248(6) Uani 1 1 d . . . C12 C 1.08418(18) 0.04420(15) -0.07698(9) 0.0370(9) Uani 1 1 d . . . H12 H 1.0742 0.0276 -0.0955 0.044 Uiso 1 1 calc R . . C13 C 1.1008(2) 0.10787(18) -0.11156(9) 0.0480(11) Uani 1 1 d . . . H13A H 1.0630 0.1229 -0.1152 0.058 Uiso 1 1 calc R . . H13B H 1.1070 0.0858 -0.1288 0.058 Uiso 1 1 calc R . . Ni2 Ni 0.8750 0.3750 0.009711(16) 0.02870(13) Uani 1 2 d S . . N6 N 0.84052(16) 0.33257(11) 0.04520(8) 0.0361(7) Uani 1 1 d . . . N7 N 0.93406(14) 0.32623(11) 0.01139(8) 0.0326(7) Uani 1 1 d . . . N8 N 0.93238(16) 0.39526(13) -0.02593(10) 0.0431(8) Uani 1 1 d . . . C14 C 0.7917(2) 0.33812(16) 0.06138(12) 0.0482(11) Uani 1 1 d . . . H14 H 0.7674 0.3629 0.0562 0.058 Uiso 1 1 calc R . . C15 C 0.7743(3) 0.30963(19) 0.08550(13) 0.0596(14) Uani 1 1 d . . . H15 H 0.7394 0.3150 0.0969 0.072 Uiso 1 1 calc R . . C16 C 0.8084(3) 0.2738(2) 0.09239(13) 0.0610(14) Uani 1 1 d . . . H16 H 0.7970 0.2535 0.1087 0.073 Uiso 1 1 calc R . . C17 C 0.8589(2) 0.26660(16) 0.07617(12) 0.0479(11) Uani 1 1 d . . . H17 H 0.8828 0.2415 0.0810 0.058 Uiso 1 1 calc R . . C18 C 0.87487(19) 0.29671(13) 0.05229(10) 0.0357(8) Uani 1 1 d . . . C19 C 0.92800(18) 0.29380(13) 0.03343(10) 0.0345(8) Uani 1 1 d . . . C20 C 0.9707(2) 0.26091(15) 0.03693(13) 0.0486(11) Uani 1 1 d . . . H20 H 0.9669 0.2376 0.0522 0.058 Uiso 1 1 calc R . . C21 C 1.0183(2) 0.26344(17) 0.01747(16) 0.0589(14) Uani 1 1 d . . . H21 H 1.0480 0.2415 0.0195 0.071 Uiso 1 1 calc R . . C22 C 1.0246(2) 0.29677(17) -0.00493(14) 0.0508(12) Uani 1 1 d . . . H22 H 1.0579 0.2980 -0.0182 0.061 Uiso 1 1 calc R . . C23 C 0.98030(17) 0.32875(14) -0.00744(11) 0.0374(9) Uani 1 1 d . . . C24 C 0.97854(18) 0.36655(16) -0.03003(11) 0.0424(10) Uani 1 1 d . . . C25 C 1.0174(3) 0.3727(2) -0.05433(15) 0.0617(15) Uani 1 1 d . . . H25 H 1.0499 0.3533 -0.0566 0.074 Uiso 1 1 calc R . . C26 C 1.0091(3) 0.4067(3) -0.07498(18) 0.089(2) Uani 1 1 d . . . H26 H 1.0353 0.4107 -0.0922 0.107 Uiso 1 1 calc R . . C27 C 0.9632(3) 0.4357(3) -0.0715(2) 0.095(3) Uani 1 1 d . . . H27 H 0.9572 0.4596 -0.0860 0.114 Uiso 1 1 calc R . . C28 C 0.9257(3) 0.4289(2) -0.04600(15) 0.0692(18) Uani 1 1 d . . . H28 H 0.8942 0.4491 -0.0430 0.083 Uiso 1 1 calc R . . Cl1 Cl 0.6224(4) 0.2762(3) 0.11390(16) 0.147(2) Uiso 0.50 1 d PD . . O3 O 0.5771(6) 0.2485(5) 0.1177(3) 0.231(5) Uiso 1 1 d . . . O4 O 0.6250 0.3186(7) 0.1250 0.220(7) Uiso 1 2 d S . . O5 O 0.6184(10) 0.2746(9) 0.0798(4) 0.224(10) Uiso 0.50 1 d PD . . O1W O 1.21819(11) 0.09631(9) 0.01705(6) 0.0317(5) Uani 1 1 d . . . H1A H 1.2306 0.0901 -0.0010 0.048 Uiso 1 1 d R . . H1B H 1.2506 0.0943 0.0266 0.048 Uiso 1 1 d R . . O2W O 1.02017(17) 0.16310(13) -0.04540(8) 0.0567(9) Uani 1 1 d . . . H2A H 0.9988 0.1488 -0.0585 0.085 Uiso 1 1 d R . . H2B H 1.0194 0.1848 -0.0583 0.085 Uiso 1 1 d R . . O3W O 0.7639(2) -0.00506(15) 0.07511(11) 0.0773(13) Uani 1 1 d . . . O4WA O 0.9445(3) 0.1255(3) -0.0915(2) 0.0569(19) Uani 0.50 1 d P . . O4WB O 0.9489(6) 0.1026(5) -0.0758(3) 0.111(5) Uani 0.50 1 d P . . O5WA O 0.9780(3) 0.07221(19) -0.14163(17) 0.0651(16) Uani 0.70 1 d P . . O5WB O 0.9404(8) 0.0614(5) -0.1333(4) 0.068(4) Uani 0.30 1 d P . . O6WA O 0.8425(8) 0.1226(6) -0.0651(4) 0.135(6) Uiso 0.50 1 d P . . O6WB O 0.8444(4) 0.0988(4) -0.0585(2) 0.071(2) Uiso 0.50 1 d P . . O7W O 0.8548(5) 0.1668(4) -0.0089(3) 0.192(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01783(8) 0.01822(7) 0.01378(7) -0.00063(6) 0.000 0.000 Tb1 0.02112(9) 0.01845(9) 0.01439(8) 0.000 0.000 0.00025(7) Cu1 0.0424(3) 0.0318(3) 0.0146(2) 0.000 0.000 -0.0065(3) O1 0.0403(14) 0.0236(11) 0.0186(10) -0.0029(9) -0.0005(10) -0.0058(10) O2 0.0375(14) 0.0229(11) 0.0219(11) -0.0006(9) 0.0016(10) -0.0010(10) N1 0.0249(13) 0.0377(17) 0.0218(13) 0.0030(12) 0.0022(10) 0.0053(12) N2 0.0407(18) 0.0271(15) 0.0377(17) 0.0007(12) 0.0003(14) -0.0054(13) N3 0.0322(16) 0.0381(17) 0.0341(16) 0.0009(13) -0.0034(13) -0.0090(14) N4 0.0402(18) 0.0366(17) 0.0256(14) 0.0038(12) -0.0024(13) 0.0018(14) N5 0.0388(18) 0.0465(19) 0.0195(13) -0.0048(13) -0.0025(12) -0.0050(15) C1 0.0242(14) 0.0258(15) 0.0178(13) 0.0005(11) -0.0002(11) 0.0049(12) C2 0.0257(15) 0.0240(14) 0.0232(15) -0.0011(11) -0.0004(12) 0.0004(12) C3 0.0257(14) 0.0252(14) 0.0201(13) 0.0007(11) -0.0006(12) 0.0005(13) C4 0.0233(15) 0.0249(15) 0.0235(14) -0.0016(12) 0.0011(12) 0.0013(12) C5 0.067(3) 0.0295(18) 0.0270(18) 0.0058(14) 0.0018(18) 0.0024(19) C6 0.0276(16) 0.0222(14) 0.0288(16) -0.0037(12) 0.0021(13) 0.0019(12) C7 0.041(2) 0.0215(16) 0.042(2) -0.0026(14) 0.0054(17) -0.0023(15) C8 0.047(2) 0.0263(18) 0.052(2) -0.0131(17) 0.007(2) -0.0073(17) C9 0.039(2) 0.038(2) 0.040(2) -0.0197(17) 0.0032(17) -0.0056(17) C10 0.0287(17) 0.0334(18) 0.0289(17) -0.0130(14) 0.0019(13) -0.0019(14) C11 0.0223(15) 0.0258(15) 0.0263(15) -0.0068(12) 0.0013(12) 0.0001(12) C12 0.039(2) 0.048(2) 0.0243(16) -0.0134(16) -0.0008(15) -0.0034(18) C13 0.065(3) 0.060(3) 0.0196(17) -0.0029(18) -0.0071(18) -0.010(2) Ni2 0.0240(3) 0.0276(3) 0.0346(3) 0.000 0.000 0.0077(2) N6 0.0392(18) 0.0290(16) 0.0403(18) 0.0027(13) -0.0017(14) 0.0069(13) N7 0.0274(15) 0.0312(16) 0.0391(17) -0.0074(13) -0.0023(13) 0.0060(12) N8 0.0338(18) 0.046(2) 0.050(2) 0.0038(17) 0.0078(16) 0.0053(16) C14 0.047(3) 0.042(2) 0.056(3) 0.010(2) 0.014(2) 0.004(2) C15 0.070(4) 0.057(3) 0.053(3) 0.013(2) 0.022(3) 0.002(3) C16 0.077(4) 0.057(3) 0.050(3) 0.017(2) 0.010(3) -0.003(3) C17 0.061(3) 0.037(2) 0.046(2) 0.0114(19) -0.008(2) 0.005(2) C18 0.041(2) 0.0280(17) 0.0376(19) 0.0009(14) -0.0067(17) 0.0057(16) C19 0.0342(19) 0.0269(17) 0.042(2) -0.0027(15) -0.0096(16) 0.0057(15) C20 0.041(2) 0.033(2) 0.072(3) 0.004(2) -0.008(2) 0.0105(18) C21 0.042(3) 0.039(2) 0.096(4) -0.004(3) -0.002(3) 0.015(2) C22 0.031(2) 0.047(3) 0.074(3) -0.009(2) 0.004(2) 0.0089(19) C23 0.0259(18) 0.037(2) 0.050(2) -0.0091(17) -0.0027(16) 0.0036(15) C24 0.0267(18) 0.051(3) 0.049(2) -0.0088(19) 0.0089(17) 0.0012(17) C25 0.050(3) 0.069(4) 0.066(3) 0.004(3) 0.029(3) 0.005(3) C26 0.078(5) 0.104(6) 0.086(5) 0.031(4) 0.047(4) 0.012(4) C27 0.083(5) 0.099(6) 0.102(6) 0.056(5) 0.039(4) 0.011(4) C28 0.055(3) 0.075(4) 0.078(4) 0.033(3) 0.022(3) 0.013(3) O1W 0.0280(13) 0.0422(15) 0.0250(12) -0.0073(11) 0.0009(10) 0.0078(11) O2W 0.071(2) 0.065(2) 0.0342(16) 0.0103(15) -0.0136(16) -0.0151(19) O3W 0.075(3) 0.080(3) 0.077(3) -0.033(2) 0.006(2) -0.030(2) O4WA 0.055(4) 0.060(5) 0.057(5) -0.005(4) -0.003(4) -0.005(4) O4WB 0.146(12) 0.114(10) 0.072(7) 0.019(7) -0.011(7) -0.055(9) O5WA 0.078(4) 0.034(3) 0.083(4) -0.004(3) -0.008(4) 0.003(3) O5WB 0.086(11) 0.036(7) 0.083(11) -0.007(6) -0.020(9) 0.023(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 2.133(3) 3 ? W1 C1 2.133(3) . ? W1 C2 2.165(3) 3 ? W1 C2 2.165(3) . ? W1 C3 2.169(3) . ? W1 C3 2.169(3) 3 ? W1 C4 2.170(3) 3 ? W1 C4 2.170(3) . ? Tb1 O1 2.302(2) . ? Tb1 O1 2.302(2) 2_755 ? Tb1 N1 2.389(3) 2_755 ? Tb1 N1 2.389(3) . ? Tb1 O1W 2.389(3) . ? Tb1 O1W 2.389(3) 2_755 ? Tb1 O2 2.532(2) . ? Tb1 O2 2.532(2) 2_755 ? Tb1 Cu1 3.3526(6) . ? Cu1 O1 1.906(2) 2_755 ? Cu1 O1 1.906(2) . ? Cu1 N5 1.915(3) . ? Cu1 N5 1.915(3) 2_755 ? O1 C11 1.329(4) . ? O2 C6 1.392(4) . ? O2 C5 1.444(4) . ? N1 C1 1.153(4) . ? N2 C2 1.154(5) . ? N3 C3 1.148(5) . ? N4 C4 1.157(4) . ? N5 C12 1.278(5) . ? N5 C13 1.467(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.379(5) . ? C6 C11 1.400(5) . ? C7 C8 1.384(6) . ? C7 H7 0.9500 . ? C8 C9 1.375(7) . ? C8 H8 0.9500 . ? C9 C10 1.403(6) . ? C9 H9 0.9500 . ? C10 C11 1.411(5) . ? C10 C12 1.459(6) . ? C12 H12 0.9500 . ? C13 C13 1.511(10) 2_755 ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? Ni2 N7 1.990(3) . ? Ni2 N7 1.990(3) 14_655 ? Ni2 N8 2.088(4) . ? Ni2 N8 2.088(4) 14_655 ? Ni2 N6 2.112(4) 14_655 ? Ni2 N6 2.112(4) . ? N6 C14 1.324(6) . ? N6 C18 1.362(5) . ? N7 C23 1.329(5) . ? N7 C19 1.347(5) . ? N8 C28 1.319(7) . ? N8 C24 1.374(6) . ? C14 C15 1.383(7) . ? C14 H14 0.9500 . ? C15 C16 1.356(8) . ? C15 H15 0.9500 . ? C16 C17 1.365(8) . ? C16 H16 0.9500 . ? C17 C18 1.397(6) . ? C17 H17 0.9500 . ? C18 C19 1.460(6) . ? C19 C20 1.395(6) . ? C20 C21 1.369(8) . ? C20 H20 0.9500 . ? C21 C22 1.377(8) . ? C21 H21 0.9500 . ? C22 C23 1.398(6) . ? C22 H22 0.9500 . ? C23 C24 1.475(7) . ? C24 C25 1.372(6) . ? C25 C26 1.349(9) . ? C25 H25 0.9500 . ? C26 C27 1.370(10) . ? C26 H26 0.9500 . ? C27 C28 1.392(8) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? Cl1 Cl1 0.943(14) 4_655 ? Cl1 O3 1.339(14) . ? Cl1 O4 1.349(17) . ? Cl1 O5 1.440(16) . ? Cl1 O3 1.622(15) 4_655 ? O3 Cl1 1.622(15) 4_655 ? O4 Cl1 1.349(17) 4_655 ? O1W H1A 0.8337 . ? O1W H1B 0.8483 . ? O2W H2A 0.8537 . ? O2W H2B 0.8439 . ? O4WA O4WB 0.956(13) . ? O5WA O5WB 0.988(18) . ? O6WA O6WB 0.765(16) . ? 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 C1 W1 C1 77.21(17) 3 . ? C1 W1 C2 76.19(12) 3 3 ? C1 W1 C2 73.51(12) . 3 ? C1 W1 C2 73.51(12) 3 . ? C1 W1 C2 76.19(12) . . ? C2 W1 C2 140.93(18) 3 . ? C1 W1 C3 142.01(12) 3 . ? C1 W1 C3 114.39(12) . . ? C2 W1 C3 73.39(13) 3 . ? C2 W1 C3 143.11(12) . . ? C1 W1 C3 114.39(12) 3 3 ? C1 W1 C3 142.01(12) . 3 ? C2 W1 C3 143.11(12) 3 3 ? C2 W1 C3 73.39(12) . 3 ? C3 W1 C3 79.57(18) . 3 ? C1 W1 C4 70.84(12) 3 3 ? C1 W1 C4 140.71(12) . 3 ? C2 W1 C4 77.10(12) 3 3 ? C2 W1 C4 114.45(12) . 3 ? C3 W1 C4 80.58(12) . 3 ? C3 W1 C4 74.07(12) 3 3 ? C1 W1 C4 140.71(12) 3 . ? C1 W1 C4 70.84(12) . . ? C2 W1 C4 114.45(12) 3 . ? C2 W1 C4 77.10(12) . . ? C3 W1 C4 74.07(12) . . ? C3 W1 C4 80.58(12) 3 . ? C4 W1 C4 146.87(18) 3 . ? O1 Tb1 O1 66.55(12) . 2_755 ? O1 Tb1 N1 143.74(10) . 2_755 ? O1 Tb1 N1 120.28(10) 2_755 2_755 ? O1 Tb1 N1 120.28(10) . . ? O1 Tb1 N1 143.74(10) 2_755 . ? N1 Tb1 N1 76.79(15) 2_755 . ? O1 Tb1 O1W 76.78(9) . . ? O1 Tb1 O1W 78.18(10) 2_755 . ? N1 Tb1 O1W 70.83(9) 2_755 . ? N1 Tb1 O1W 137.29(10) . . ? O1 Tb1 O1W 78.18(10) . 2_755 ? O1 Tb1 O1W 76.78(9) 2_755 2_755 ? N1 Tb1 O1W 137.29(10) 2_755 2_755 ? N1 Tb1 O1W 70.83(9) . 2_755 ? O1W Tb1 O1W 149.94(12) . 2_755 ? O1 Tb1 O2 62.90(8) . . ? O1 Tb1 O2 128.72(8) 2_755 . ? N1 Tb1 O2 96.60(10) 2_755 . ? N1 Tb1 O2 74.07(10) . . ? O1W Tb1 O2 82.65(9) . . ? O1W Tb1 O2 100.41(9) 2_755 . ? O1 Tb1 O2 128.72(8) . 2_755 ? O1 Tb1 O2 62.90(8) 2_755 2_755 ? N1 Tb1 O2 74.07(10) 2_755 2_755 ? N1 Tb1 O2 96.60(10) . 2_755 ? O1W Tb1 O2 100.41(9) . 2_755 ? O1W Tb1 O2 82.65(9) 2_755 2_755 ? O2 Tb1 O2 168.32(11) . 2_755 ? O1 Tb1 Cu1 33.27(6) . . ? O1 Tb1 Cu1 33.27(6) 2_755 . ? N1 Tb1 Cu1 141.61(7) 2_755 . ? N1 Tb1 Cu1 141.61(7) . . ? O1W Tb1 Cu1 74.97(6) . . ? O1W Tb1 Cu1 74.97(6) 2_755 . ? O2 Tb1 Cu1 95.84(5) . . ? O2 Tb1 Cu1 95.84(5) 2_755 . ? O1 Cu1 O1 82.98(14) 2_755 . ? O1 Cu1 N5 176.01(14) 2_755 . ? O1 Cu1 N5 94.93(12) . . ? O1 Cu1 N5 94.93(12) 2_755 2_755 ? O1 Cu1 N5 176.01(14) . 2_755 ? N5 Cu1 N5 87.4(2) . 2_755 ? O1 Cu1 Tb1 41.49(7) 2_755 . ? O1 Cu1 Tb1 41.49(7) . . ? N5 Cu1 Tb1 136.32(10) . . ? N5 Cu1 Tb1 136.32(10) 2_755 . ? C11 O1 Cu1 125.5(2) . . ? C11 O1 Tb1 128.9(2) . . ? Cu1 O1 Tb1 105.24(11) . . ? C6 O2 C5 116.6(3) . . ? C6 O2 Tb1 119.0(2) . . ? C5 O2 Tb1 124.4(2) . . ? C1 N1 Tb1 167.3(3) . . ? C12 N5 C13 123.6(3) . . ? C12 N5 Cu1 126.0(3) . . ? C13 N5 Cu1 110.3(3) . . ? N1 C1 W1 175.3(3) . . ? N2 C2 W1 177.5(3) . . ? N3 C3 W1 178.0(3) . . ? N4 C4 W1 175.1(3) . . ? O2 C5 H5A 109.5 . . ? O2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 O2 125.7(3) . . ? C7 C6 C11 121.2(3) . . ? O2 C6 C11 113.1(3) . . ? C6 C7 C8 119.3(4) . . ? C6 C7 H7 120.4 . . ? C8 C7 H7 120.4 . . ? C9 C8 C7 120.7(4) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 121.3(4) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C9 C10 C11 118.0(4) . . ? C9 C10 C12 118.8(3) . . ? C11 C10 C12 123.2(3) . . ? O1 C11 C6 116.0(3) . . ? O1 C11 C10 124.5(3) . . ? C6 C11 C10 119.5(3) . . ? N5 C12 C10 125.1(3) . . ? N5 C12 H12 117.4 . . ? C10 C12 H12 117.4 . . ? N5 C13 C13 108.7(3) . 2_755 ? N5 C13 H13A 110.0 . . ? C13 C13 H13A 110.0 2_755 . ? N5 C13 H13B 110.0 . . ? C13 C13 H13B 110.0 2_755 . ? H13A C13 H13B 108.3 . . ? N7 Ni2 N7 175.9(2) . 14_655 ? N7 Ni2 N8 78.76(15) . . ? N7 Ni2 N8 104.23(14) 14_655 . ? N7 Ni2 N8 104.23(14) . 14_655 ? N7 Ni2 N8 78.76(15) 14_655 14_655 ? N8 Ni2 N8 88.1(2) . 14_655 ? N7 Ni2 N6 98.94(13) . 14_655 ? N7 Ni2 N6 78.13(14) 14_655 14_655 ? N8 Ni2 N6 95.64(15) . 14_655 ? N8 Ni2 N6 156.81(14) 14_655 14_655 ? N7 Ni2 N6 78.13(14) . . ? N7 Ni2 N6 98.94(13) 14_655 . ? N8 Ni2 N6 156.81(14) . . ? N8 Ni2 N6 95.64(15) 14_655 . ? N6 Ni2 N6 89.9(2) 14_655 . ? C14 N6 C18 118.5(4) . . ? C14 N6 Ni2 127.5(3) . . ? C18 N6 Ni2 114.0(3) . . ? C23 N7 C19 122.3(3) . . ? C23 N7 Ni2 118.9(3) . . ? C19 N7 Ni2 118.5(3) . . ? C28 N8 C24 118.8(4) . . ? C28 N8 Ni2 127.3(3) . . ? C24 N8 Ni2 113.5(3) . . ? N6 C14 C15 123.2(5) . . ? N6 C14 H14 118.4 . . ? C15 C14 H14 118.4 . . ? C16 C15 C14 118.2(5) . . ? C16 C15 H15 120.9 . . ? C14 C15 H15 120.9 . . ? C15 C16 C17 120.6(5) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C18 118.9(4) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? N6 C18 C17 120.6(4) . . ? N6 C18 C19 114.4(4) . . ? C17 C18 C19 125.0(4) . . ? N7 C19 C20 120.2(4) . . ? N7 C19 C18 114.8(3) . . ? C20 C19 C18 125.0(4) . . ? C21 C20 C19 117.4(5) . . ? C21 C20 H20 121.3 . . ? C19 C20 H20 121.3 . . ? C22 C21 C20 122.3(4) . . ? C22 C21 H21 118.9 . . ? C20 C21 H21 118.9 . . ? C21 C22 C23 117.8(5) . . ? C21 C22 H22 121.1 . . ? C23 C22 H22 121.1 . . ? N7 C23 C22 120.0(4) . . ? N7 C23 C24 114.0(3) . . ? C22 C23 C24 126.1(4) . . ? C25 C24 N8 120.9(5) . . ? C25 C24 C23 124.5(4) . . ? N8 C24 C23 114.6(4) . . ? C26 C25 C24 119.3(5) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C25 C26 C27 120.8(6) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C26 C27 C28 118.0(6) . . ? C26 C27 H27 121.0 . . ? C28 C27 H27 121.0 . . ? N8 C28 C27 122.1(6) . . ? N8 C28 H28 118.9 . . ? C27 C28 H28 118.9 . . ? Cl1 Cl1 O3 88.9(10) 4_655 . ? Cl1 Cl1 O4 69.5(4) 4_655 . ? O3 Cl1 O4 124.8(9) . . ? Cl1 Cl1 O5 175.7(16) 4_655 . ? O3 Cl1 O5 92.9(12) . . ? O4 Cl1 O5 112.4(12) . . ? Cl1 Cl1 O3 55.6(7) 4_655 4_655 ? O3 Cl1 O3 100.7(11) . 4_655 ? O4 Cl1 O3 106.2(7) . 4_655 ? O5 Cl1 O3 120.2(12) . 4_655 ? Cl1 O3 Cl1 35.5(7) . 4_655 ? Cl1 O4 Cl1 40.9(9) 4_655 . ? Tb1 O1W H1A 128.6 . . ? Tb1 O1W H1B 133.7 . . ? H1A O1W H1B 96.6 . . ? H2A O2W H2B 87.2 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 32.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.947 _refine_diff_density_min -1.723 _refine_diff_density_rms 0.136 _database_code_depnum_ccdc_archive 'CCDC 904313' ####################################################################### # # 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_nb4_90_0m #TrackingRef 'web_deposit_cif_file_2_Lise-MarieChamoreau_1349269842.nb4_90_0m - publi.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H52 Cu2 N20 O16 Tb2 Mo2, 2(C30 H22 N6 Ru), 2(N O3), 24 (H2 O)' _chemical_formula_sum 'C112 H144 Cl0 Cu2 Mo2 N34 O46 Ru2 Tb2' _chemical_formula_weight 3541.55 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d d' _symmetry_space_group_name_Hall '-F 2uv 2vw' _symmetry_Int_Tables_number 70 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+1/4, z' 'x, -y+1/4, -z+1/4' '-x+1/4, y, -z+1/4' 'x, y+1/2, z+1/2' '-x+1/4, -y+3/4, z+1/2' 'x, -y+3/4, -z+3/4' '-x+1/4, y+1/2, -z+3/4' 'x+1/2, y, z+1/2' '-x+3/4, -y+1/4, z+1/2' 'x+1/2, -y+1/4, -z+3/4' '-x+3/4, y, -z+3/4' 'x+1/2, y+1/2, z' '-x+3/4, -y+3/4, z' 'x+1/2, -y+3/4, -z+1/4' '-x+3/4, y+1/2, -z+1/4' '-x, -y, -z' 'x-1/4, y-1/4, -z' '-x, y-1/4, z-1/4' 'x-1/4, -y, z-1/4' '-x, -y+1/2, -z+1/2' 'x-1/4, y+1/4, -z+1/2' '-x, y+1/4, z+1/4' 'x-1/4, -y+1/2, z+1/4' '-x+1/2, -y, -z+1/2' 'x+1/4, y-1/4, -z+1/2' '-x+1/2, y-1/4, z+1/4' 'x+1/4, -y, z+1/4' '-x+1/2, -y+1/2, -z' 'x+1/4, y+1/4, -z' '-x+1/2, y+1/4, z-1/4' 'x+1/4, -y+1/2, z-1/4' _cell_length_a 22.9246(7) _cell_length_b 29.8958(9) _cell_length_c 41.9514(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 28751.4(16) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9939 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 29.93 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14256 _exptl_absorpt_coefficient_mu 1.725 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.672 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details ; SADABS, Bruker AXS Inc., Madison, Wisconsin, USA. ; _diffrn_ambient_temperature 200(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55017 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -58 _diffrn_reflns_limit_l_max 58 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 29.97 _reflns_number_total 10367 _reflns_number_gt 7462 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SUPERFLIP (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND. Crystal Impact GbR, Bonn, Germany' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Geometry of NO3 anion was restrained. 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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+409.0241P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10367 _refine_ls_number_parameters 441 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0618 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.948493(16) 0.1250 0.1250 0.01448(8) Uani 1 2 d S . . Tb1 Tb 1.1250 0.1250 0.031575(5) 0.01770(6) Uani 1 2 d S . . Cu1 Cu 1.1250 0.1250 -0.048422(14) 0.02655(14) Uani 1 2 d S . . O1 O 1.10584(12) 0.08539(8) -0.01441(6) 0.0243(5) Uani 1 1 d . . . O2 O 1.10167(12) 0.04258(8) 0.03776(6) 0.0241(5) Uani 1 1 d . . . N1 N 1.06029(14) 0.11953(11) 0.07628(7) 0.0257(6) Uani 1 1 d . . . N2 N 0.99705(16) 0.22901(11) 0.11724(8) 0.0330(8) Uani 1 1 d . . . N3 N 0.83833(15) 0.05822(11) 0.10599(8) 0.0295(7) Uani 1 1 d . . . N4 N 0.91105(16) 0.15517(11) 0.05152(8) 0.0305(7) Uani 1 1 d . . . N5 N 1.10037(16) 0.08483(13) -0.08134(8) 0.0327(8) Uani 1 1 d . . . C1 C 1.02133(15) 0.11934(11) 0.09352(8) 0.0200(6) Uani 1 1 d . . . C2 C 0.98018(16) 0.19312(12) 0.12069(8) 0.0220(7) Uani 1 1 d . . . C3 C 0.87600(17) 0.08150(11) 0.11300(8) 0.0215(6) Uani 1 1 d . . . C4 C 0.92127(16) 0.14414(12) 0.07720(8) 0.0214(7) Uani 1 1 d . . . C5 C 1.1031(2) 0.01887(14) 0.06781(10) 0.0374(10) Uani 1 1 d . . . H5A H 1.0637 0.0088 0.0733 0.056 Uiso 1 1 calc R . . H5B H 1.1176 0.0389 0.0846 0.056 Uiso 1 1 calc R . . H5C H 1.1290 -0.0071 0.0660 0.056 Uiso 1 1 calc R . . C6 C 1.08709(16) 0.01785(12) 0.01067(9) 0.0232(7) Uani 1 1 d . . . C7 C 1.07046(19) -0.02654(13) 0.01061(11) 0.0326(9) Uani 1 1 d . . . H7 H 1.0673 -0.0428 0.0300 0.039 Uiso 1 1 calc R . . C8 C 1.0583(2) -0.04714(14) -0.01863(12) 0.0388(10) Uani 1 1 d . . . H8 H 1.0465 -0.0776 -0.0191 0.047 Uiso 1 1 calc R . . C9 C 1.06335(19) -0.02388(15) -0.04657(11) 0.0366(10) Uani 1 1 d . . . H9 H 1.0554 -0.0386 -0.0662 0.044 Uiso 1 1 calc R . . C10 C 1.08000(17) 0.02128(13) -0.04693(9) 0.0280(8) Uani 1 1 d . . . C11 C 1.09117(16) 0.04261(12) -0.01753(8) 0.0215(7) Uani 1 1 d . . . C12 C 1.08382(18) 0.04427(15) -0.07767(9) 0.0330(9) Uani 1 1 d . . . H12 H 1.0733 0.0279 -0.0962 0.040 Uiso 1 1 calc R . . C13 C 1.1005(2) 0.10783(18) -0.11215(10) 0.0442(11) Uani 1 1 d . . . H13A H 1.0626 0.1229 -0.1156 0.053 Uiso 1 1 calc R . . H13B H 1.1066 0.0860 -0.1296 0.053 Uiso 1 1 calc R . . Ru1 Ru 0.8750 0.3750 0.009529(10) 0.02419(9) Uani 1 2 d S . . N6 N 0.84116(15) 0.33369(11) 0.04438(8) 0.0298(7) Uani 1 1 d . . . N7 N 0.93477(14) 0.32699(11) 0.01087(8) 0.0300(7) Uani 1 1 d . . . N8 N 0.93002(16) 0.39598(14) -0.02614(9) 0.0373(8) Uani 1 1 d . . . C14 C 0.7918(2) 0.33931(16) 0.06109(11) 0.0402(10) Uani 1 1 d . . . H14 H 0.7680 0.3645 0.0565 0.048 Uiso 1 1 calc R . . C15 C 0.7739(3) 0.31004(18) 0.08479(12) 0.0519(13) Uani 1 1 d . . . H15 H 0.7384 0.3151 0.0959 0.062 Uiso 1 1 calc R . . C16 C 0.8078(3) 0.27390(19) 0.09192(13) 0.0561(15) Uani 1 1 d . . . H16 H 0.7964 0.2537 0.1082 0.067 Uiso 1 1 calc R . . C17 C 0.8580(3) 0.26707(16) 0.07548(12) 0.0466(12) Uani 1 1 d . . . H17 H 0.8817 0.2419 0.0802 0.056 Uiso 1 1 calc R . . C18 C 0.8752(2) 0.29722(13) 0.05136(10) 0.0342(9) Uani 1 1 d . . . C19 C 0.9284(2) 0.29357(13) 0.03258(11) 0.0347(9) Uani 1 1 d . . . C20 C 0.9707(2) 0.26051(16) 0.03467(15) 0.0509(14) Uani 1 1 d . . . H20 H 0.9670 0.2368 0.0496 0.061 Uiso 1 1 calc R . . C21 C 1.0176(2) 0.26289(18) 0.01470(18) 0.0633(18) Uani 1 1 d . . . H21 H 1.0468 0.2404 0.0160 0.076 Uiso 1 1 calc R . . C22 C 1.0241(2) 0.29654(18) -0.00699(15) 0.0523(14) Uani 1 1 d . . . H22 H 1.0572 0.2976 -0.0206 0.063 Uiso 1 1 calc R . . C23 C 0.98077(19) 0.32954(15) -0.00877(12) 0.0376(10) Uani 1 1 d . . . C24 C 0.97719(19) 0.36753(17) -0.03066(12) 0.0417(11) Uani 1 1 d . . . C25 C 1.0159(3) 0.3744(2) -0.05526(15) 0.0608(15) Uani 1 1 d . . . H25 H 1.0487 0.3553 -0.0578 0.073 Uiso 1 1 calc R . . C26 C 1.0070(3) 0.4089(3) -0.07599(17) 0.079(2) Uani 1 1 d . . . H26 H 1.0334 0.4137 -0.0931 0.095 Uiso 1 1 calc R . . C27 C 0.9597(3) 0.4369(3) -0.07205(17) 0.080(2) Uani 1 1 d . . . H27 H 0.9529 0.4607 -0.0866 0.096 Uiso 1 1 calc R . . C28 C 0.9221(2) 0.4297(2) -0.04636(14) 0.0542(14) Uani 1 1 d . . . H28 H 0.8900 0.4493 -0.0433 0.065 Uiso 1 1 calc R . . O1W O 1.21868(12) 0.09671(10) 0.01675(6) 0.0304(6) Uani 1 1 d . . . H1A H 1.2291(6) 0.09795(11) 0.0016(8) 0.046 Uiso 1 1 d R . . H1B H 1.2433(12) 0.09425(16) 0.0268(5) 0.046 Uiso 1 1 d R . . O2W O 1.02065(17) 0.16192(13) -0.04620(8) 0.0516(10) Uani 1 1 d . . . H2A H 1.0153(3) 0.1873(13) -0.0507(3) 0.077 Uiso 1 1 d R . . H2B H 0.9949(14) 0.1440(9) -0.0526(3) 0.077 Uiso 1 1 d R . . O3W O 0.7636(2) -0.00803(17) 0.07667(12) 0.0866(18) Uani 1 1 d . . . H3A H 0.7898(18) 0.0097(13) 0.0823(4) 0.130 Uiso 1 1 d R . . H3B H 0.735(2) 0.0089(12) 0.0814(4) 0.130 Uiso 1 1 d R . . N9 N 0.6197(10) 0.2782(7) 0.1044(4) 0.164(9) Uiso 0.50 1 d PD . . O5 O 0.6036(7) 0.2728(5) 0.0696(3) 0.145(6) Uiso 0.50 1 d PD . . O3 O 0.6250 0.3112(6) 0.1250 0.226(7) Uiso 1 2 d SD . . O4 O 0.5898(9) 0.2540(6) 0.1233(5) 0.200(9) Uiso 0.50 1 d PD . . O4WA O 0.9433(3) 0.1259(3) -0.09149(18) 0.0478(16) Uiso 0.50 1 d P . . O4WB O 0.9500(6) 0.1025(5) -0.0785(3) 0.106(4) Uiso 0.50 1 d P . . O5WA O 0.9774(3) 0.0712(2) -0.14237(16) 0.0405(15) Uiso 0.50 1 d P . . O5WB O 0.9424(5) 0.0606(3) -0.1346(2) 0.076(3) Uiso 0.50 1 d P . . O6WA O 0.6589(5) 0.3988(4) 0.0558(3) 0.065(3) Uiso 0.50 1 d P . . O6WB O 0.6613(7) 0.3827(5) 0.0633(4) 0.108(5) Uiso 0.50 1 d P . . O7W O 0.8501(4) 0.1743(4) -0.0088(2) 0.158(3) Uiso 1 1 d . . . O8WA O 0.7500 0.2500 0.0000 0.169(5) Uiso 1 2 d S . . O8WB O 0.6747(14) 0.2925(11) 0.0042(8) 0.277(14) Uiso 0.50 1 d P . . 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 Mo1 0.01548(17) 0.01470(17) 0.01326(15) -0.00068(14) 0.000 0.000 Tb1 0.02088(11) 0.01704(11) 0.01518(10) 0.000 0.000 -0.00009(9) Cu1 0.0382(4) 0.0273(3) 0.0141(2) 0.000 0.000 -0.0073(3) O1 0.0376(14) 0.0189(12) 0.0165(11) -0.0027(9) -0.0008(10) -0.0071(11) O2 0.0344(14) 0.0175(12) 0.0204(12) 0.0000(9) 0.0001(10) -0.0007(11) N1 0.0245(15) 0.0319(18) 0.0209(13) 0.0024(12) 0.0019(12) 0.0050(13) N2 0.0377(19) 0.0241(17) 0.0371(19) -0.0002(13) 0.0020(15) -0.0036(14) N3 0.0276(17) 0.0277(17) 0.0330(17) 0.0003(13) -0.0023(14) -0.0058(13) N4 0.0357(19) 0.0291(17) 0.0269(16) 0.0004(13) -0.0039(14) 0.0015(14) N5 0.0382(19) 0.041(2) 0.0190(15) -0.0055(13) -0.0001(14) -0.0061(16) C1 0.0231(16) 0.0204(17) 0.0165(14) 0.0023(12) -0.0030(12) 0.0024(13) C2 0.0226(16) 0.0221(16) 0.0214(17) -0.0004(13) -0.0008(13) 0.0010(13) C3 0.0247(16) 0.0220(16) 0.0177(13) 0.0005(12) -0.0005(14) 0.0020(15) C4 0.0221(17) 0.0190(16) 0.0230(16) -0.0031(13) -0.0001(13) -0.0015(13) C5 0.061(3) 0.026(2) 0.0255(19) 0.0068(15) 0.0004(19) 0.0030(19) C6 0.0255(17) 0.0188(16) 0.0255(17) -0.0043(13) 0.0019(14) 0.0003(14) C7 0.040(2) 0.0178(17) 0.040(2) -0.0027(15) 0.0071(18) -0.0016(16) C8 0.042(2) 0.0217(19) 0.053(3) -0.0119(18) 0.007(2) -0.0067(18) C9 0.036(2) 0.033(2) 0.041(2) -0.0192(18) 0.0035(19) -0.0059(18) C10 0.0282(19) 0.029(2) 0.0268(18) -0.0118(15) 0.0018(15) -0.0023(16) C11 0.0218(16) 0.0193(16) 0.0235(16) -0.0051(13) -0.0001(13) -0.0010(13) C12 0.033(2) 0.044(2) 0.0227(17) -0.0141(16) -0.0010(15) -0.0036(18) C13 0.056(3) 0.061(3) 0.0162(17) 0.0005(19) -0.0052(18) -0.008(2) Ru1 0.01896(18) 0.0248(2) 0.02881(19) 0.000 0.000 0.00666(17) N6 0.0353(19) 0.0235(16) 0.0306(17) 0.0009(13) -0.0033(14) 0.0052(14) N7 0.0238(16) 0.0283(17) 0.0379(18) -0.0124(14) -0.0065(14) 0.0039(13) N8 0.0286(18) 0.044(2) 0.039(2) -0.0011(17) 0.0044(15) 0.0004(16) C14 0.044(3) 0.034(2) 0.043(2) 0.0061(19) 0.008(2) 0.0009(19) C15 0.064(4) 0.046(3) 0.045(3) 0.009(2) 0.014(3) -0.003(3) C16 0.080(4) 0.049(3) 0.040(3) 0.014(2) 0.003(3) -0.008(3) C17 0.066(3) 0.028(2) 0.046(3) 0.0086(19) -0.017(2) 0.003(2) C18 0.042(2) 0.0225(18) 0.038(2) -0.0027(15) -0.014(2) 0.0060(18) C19 0.036(2) 0.0217(19) 0.046(2) -0.0060(17) -0.0162(19) 0.0070(17) C20 0.043(3) 0.024(2) 0.085(4) -0.003(2) -0.018(3) 0.012(2) C21 0.037(3) 0.032(3) 0.121(6) -0.013(3) -0.008(3) 0.014(2) C22 0.029(2) 0.046(3) 0.081(4) -0.021(3) 0.006(2) 0.006(2) C23 0.025(2) 0.036(2) 0.052(3) -0.017(2) -0.0006(19) 0.0005(17) C24 0.025(2) 0.052(3) 0.049(3) -0.017(2) 0.0095(18) -0.0074(19) C25 0.044(3) 0.070(4) 0.068(4) -0.011(3) 0.027(3) -0.007(3) C26 0.061(4) 0.105(6) 0.072(4) 0.003(4) 0.039(4) -0.008(4) C27 0.074(5) 0.095(5) 0.071(4) 0.032(4) 0.026(4) -0.010(4) C28 0.042(3) 0.063(4) 0.058(3) 0.019(3) 0.015(2) -0.002(3) O1W 0.0281(14) 0.0407(16) 0.0225(12) -0.0048(11) 0.0016(11) 0.0080(12) O2W 0.063(2) 0.054(2) 0.0382(18) 0.0095(16) -0.0133(17) -0.0116(18) O3W 0.071(3) 0.090(4) 0.099(4) -0.051(3) 0.008(3) -0.033(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Mo1 C1 2.136(3) 3 ? Mo1 C1 2.136(3) . ? Mo1 C3 2.169(4) . ? Mo1 C3 2.169(4) 3 ? Mo1 C2 2.170(4) . ? Mo1 C2 2.170(4) 3 ? Mo1 C4 2.177(4) 3 ? Mo1 C4 2.177(4) . ? Tb1 O1 2.306(2) 2_755 ? Tb1 O1 2.306(2) . ? Tb1 O1W 2.390(3) 2_755 ? Tb1 O1W 2.390(3) . ? Tb1 N1 2.397(3) 2_755 ? Tb1 N1 2.397(3) . ? Tb1 O2 2.535(2) 2_755 ? Tb1 O2 2.535(2) . ? Tb1 Cu1 3.3560(6) . ? Cu1 O1 1.906(3) 2_755 ? Cu1 O1 1.906(3) . ? Cu1 N5 1.915(3) 2_755 ? Cu1 N5 1.915(3) . ? O1 C11 1.329(4) . ? O2 C6 1.396(4) . ? O2 C5 1.447(4) . ? N1 C1 1.149(5) . ? N2 C2 1.150(5) . ? N3 C3 1.147(5) . ? N4 C4 1.151(5) . ? N5 C12 1.280(6) . ? N5 C13 1.464(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.381(5) . ? C6 C11 1.399(5) . ? C7 C8 1.401(6) . ? C7 H7 0.9500 . ? C8 C9 1.368(7) . ? C8 H8 0.9500 . ? C9 C10 1.403(6) . ? C9 H9 0.9500 . ? C10 C11 1.412(5) . ? C10 C12 1.464(6) . ? C12 H12 0.9500 . ? C13 C13 1.521(10) 2_755 ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? Ru1 N7 1.985(3) 14_655 ? Ru1 N7 1.985(3) . ? Ru1 N8 2.055(4) . ? Ru1 N8 2.055(4) 14_655 ? Ru1 N6 2.065(3) 14_655 ? Ru1 N6 2.065(3) . ? N6 C14 1.342(6) . ? N6 C18 1.372(5) . ? N7 C23 1.341(6) . ? N7 C19 1.360(6) . ? N8 C28 1.329(6) . ? N8 C24 1.389(6) . ? C14 C15 1.387(6) . ? C14 H14 0.9500 . ? C15 C16 1.365(8) . ? C15 H15 0.9500 . ? C16 C17 1.357(8) . ? C16 H16 0.9500 . ? C17 C18 1.412(6) . ? C17 H17 0.9500 . ? C18 C19 1.456(7) . ? C19 C20 1.387(6) . ? C20 C21 1.366(9) . ? C20 H20 0.9500 . ? C21 C22 1.364(9) . ? C21 H21 0.9500 . ? C22 C23 1.401(7) . ? C22 H22 0.9500 . ? C23 C24 1.463(7) . ? C24 C25 1.377(7) . ? C25 C26 1.364(10) . ? C25 H25 0.9500 . ? C26 C27 1.378(10) . ? C26 H26 0.9500 . ? C27 C28 1.397(8) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? O1W H1A 0.6815 . ? O1W H1B 0.7074 . ? O2W H2A 0.7914 . ? O2W H2B 0.8408 . ? O3W H3A 0.8351 . ? O3W H3B 0.8503 . ? N9 O4 1.274(16) . ? N9 O3 1.316(15) . ? N9 O4 1.506(16) 4_655 ? N9 O5 1.516(15) . ? O3 N9 1.316(15) 4_655 ? O4 N9 1.506(16) 4_655 ? O4 O4 1.62(4) 4_655 ? O4WA O4WB 0.901(13) . ? O5WA O5WB 0.922(10) . ? O6WA O6WB 0.577(17) . ? O7W O8WB 1.16(3) 29_655 ? O8WB O7W 1.16(3) 29_655 ? 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 C1 Mo1 C1 77.13(18) 3 . ? C1 Mo1 C3 142.19(13) 3 . ? C1 Mo1 C3 114.07(13) . . ? C1 Mo1 C3 114.07(13) 3 3 ? C1 Mo1 C3 142.19(13) . 3 ? C3 Mo1 C3 80.01(19) . 3 ? C1 Mo1 C2 73.46(13) 3 . ? C1 Mo1 C2 76.18(13) . . ? C3 Mo1 C2 143.11(13) . . ? C3 Mo1 C2 73.33(13) 3 . ? C1 Mo1 C2 76.18(13) 3 3 ? C1 Mo1 C2 73.46(13) . 3 ? C3 Mo1 C2 73.33(13) . 3 ? C3 Mo1 C2 143.11(13) 3 3 ? C2 Mo1 C2 140.88(19) . 3 ? C1 Mo1 C4 71.06(13) 3 3 ? C1 Mo1 C4 140.62(13) . 3 ? C3 Mo1 C4 80.60(13) . 3 ? C3 Mo1 C4 73.99(13) 3 3 ? C2 Mo1 C4 114.81(13) . 3 ? C2 Mo1 C4 76.85(13) 3 3 ? C1 Mo1 C4 140.62(13) 3 . ? C1 Mo1 C4 71.06(13) . . ? C3 Mo1 C4 73.99(13) . . ? C3 Mo1 C4 80.60(13) 3 . ? C2 Mo1 C4 76.85(13) . . ? C2 Mo1 C4 114.81(13) 3 . ? C4 Mo1 C4 146.68(19) 3 . ? O1 Tb1 O1 66.43(12) 2_755 . ? O1 Tb1 O1W 76.81(10) 2_755 2_755 ? O1 Tb1 O1W 78.05(10) . 2_755 ? O1 Tb1 O1W 78.05(10) 2_755 . ? O1 Tb1 O1W 76.81(10) . . ? O1W Tb1 O1W 149.84(13) 2_755 . ? O1 Tb1 N1 120.11(10) 2_755 2_755 ? O1 Tb1 N1 143.85(10) . 2_755 ? O1W Tb1 N1 137.35(10) 2_755 2_755 ? O1W Tb1 N1 70.83(10) . 2_755 ? O1 Tb1 N1 143.85(10) 2_755 . ? O1 Tb1 N1 120.11(10) . . ? O1W Tb1 N1 70.83(10) 2_755 . ? O1W Tb1 N1 137.35(10) . . ? N1 Tb1 N1 77.03(15) 2_755 . ? O1 Tb1 O2 63.01(8) 2_755 2_755 ? O1 Tb1 O2 128.69(8) . 2_755 ? O1W Tb1 O2 82.66(10) 2_755 2_755 ? O1W Tb1 O2 100.43(9) . 2_755 ? N1 Tb1 O2 73.92(10) 2_755 2_755 ? N1 Tb1 O2 96.71(10) . 2_755 ? O1 Tb1 O2 128.69(8) 2_755 . ? O1 Tb1 O2 63.01(8) . . ? O1W Tb1 O2 100.43(9) 2_755 . ? O1W Tb1 O2 82.66(10) . . ? N1 Tb1 O2 96.71(10) 2_755 . ? N1 Tb1 O2 73.92(10) . . ? O2 Tb1 O2 168.26(11) 2_755 . ? O1 Tb1 Cu1 33.22(6) 2_755 . ? O1 Tb1 Cu1 33.22(6) . . ? O1W Tb1 Cu1 74.92(6) 2_755 . ? O1W Tb1 Cu1 74.92(6) . . ? N1 Tb1 Cu1 141.48(8) 2_755 . ? N1 Tb1 Cu1 141.48(8) . . ? O2 Tb1 Cu1 95.87(6) 2_755 . ? O2 Tb1 Cu1 95.87(6) . . ? O1 Cu1 O1 83.02(15) 2_755 . ? O1 Cu1 N5 94.72(13) 2_755 2_755 ? O1 Cu1 N5 175.97(14) . 2_755 ? O1 Cu1 N5 175.97(14) 2_755 . ? O1 Cu1 N5 94.72(13) . . ? N5 Cu1 N5 87.7(2) 2_755 . ? O1 Cu1 Tb1 41.51(7) 2_755 . ? O1 Cu1 Tb1 41.51(7) . . ? N5 Cu1 Tb1 136.14(11) 2_755 . ? N5 Cu1 Tb1 136.14(11) . . ? C11 O1 Cu1 125.6(2) . . ? C11 O1 Tb1 128.7(2) . . ? Cu1 O1 Tb1 105.27(11) . . ? C6 O2 C5 117.1(3) . . ? C6 O2 Tb1 118.8(2) . . ? C5 O2 Tb1 124.1(2) . . ? C1 N1 Tb1 166.9(3) . . ? C12 N5 C13 123.5(4) . . ? C12 N5 Cu1 126.5(3) . . ? C13 N5 Cu1 110.0(3) . . ? N1 C1 Mo1 175.1(3) . . ? N2 C2 Mo1 177.6(3) . . ? N3 C3 Mo1 178.4(3) . . ? N4 C4 Mo1 175.0(3) . . ? O2 C5 H5A 109.5 . . ? O2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 O2 125.2(3) . . ? C7 C6 C11 121.7(4) . . ? O2 C6 C11 113.1(3) . . ? C6 C7 C8 118.6(4) . . ? C6 C7 H7 120.7 . . ? C8 C7 H7 120.7 . . ? C9 C8 C7 120.7(4) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 121.4(4) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C9 C10 C11 118.3(4) . . ? C9 C10 C12 118.5(4) . . ? C11 C10 C12 123.1(3) . . ? O1 C11 C6 116.3(3) . . ? O1 C11 C10 124.5(3) . . ? C6 C11 C10 119.2(3) . . ? N5 C12 C10 124.6(3) . . ? N5 C12 H12 117.7 . . ? C10 C12 H12 117.7 . . ? N5 C13 C13 108.6(3) . 2_755 ? N5 C13 H13A 110.0 . . ? C13 C13 H13A 110.0 2_755 . ? N5 C13 H13B 110.0 . . ? C13 C13 H13B 110.0 2_755 . ? H13A C13 H13B 108.4 . . ? N7 Ru1 N7 176.7(2) 14_655 . ? N7 Ru1 N8 102.92(14) 14_655 . ? N7 Ru1 N8 79.50(16) . . ? N7 Ru1 N8 79.50(16) 14_655 14_655 ? N7 Ru1 N8 102.92(14) . 14_655 ? N8 Ru1 N8 86.5(2) . 14_655 ? N7 Ru1 N6 78.86(14) 14_655 14_655 ? N7 Ru1 N6 98.80(13) . 14_655 ? N8 Ru1 N6 95.88(15) . 14_655 ? N8 Ru1 N6 158.21(15) 14_655 14_655 ? N7 Ru1 N6 98.80(13) 14_655 . ? N7 Ru1 N6 78.86(14) . . ? N8 Ru1 N6 158.21(15) . . ? N8 Ru1 N6 95.88(15) 14_655 . ? N6 Ru1 N6 89.86(19) 14_655 . ? C14 N6 C18 117.9(4) . . ? C14 N6 Ru1 127.7(3) . . ? C18 N6 Ru1 114.3(3) . . ? C23 N7 C19 122.5(4) . . ? C23 N7 Ru1 119.0(3) . . ? C19 N7 Ru1 118.4(3) . . ? C28 N8 C24 118.9(4) . . ? C28 N8 Ru1 127.7(3) . . ? C24 N8 Ru1 113.0(3) . . ? N6 C14 C15 123.1(5) . . ? N6 C14 H14 118.5 . . ? C15 C14 H14 118.5 . . ? C16 C15 C14 119.2(5) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 C15 119.4(5) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 120.3(5) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? N6 C18 C17 120.1(4) . . ? N6 C18 C19 114.9(4) . . ? C17 C18 C19 125.0(4) . . ? N7 C19 C20 119.4(5) . . ? N7 C19 C18 113.4(3) . . ? C20 C19 C18 127.2(5) . . ? C21 C20 C19 118.3(5) . . ? C21 C20 H20 120.8 . . ? C19 C20 H20 120.8 . . ? C22 C21 C20 122.2(5) . . ? C22 C21 H21 118.9 . . ? C20 C21 H21 118.9 . . ? C21 C22 C23 118.6(5) . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? N7 C23 C22 119.0(5) . . ? N7 C23 C24 112.7(4) . . ? C22 C23 C24 128.3(5) . . ? C25 C24 N8 120.8(5) . . ? C25 C24 C23 123.4(5) . . ? N8 C24 C23 115.7(4) . . ? C26 C25 C24 119.6(6) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 120.0(6) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C28 119.0(6) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? N8 C28 C27 121.6(6) . . ? N8 C28 H28 119.2 . . ? C27 C28 H28 119.2 . . ? Tb1 O1W H1A 122.7 . . ? Tb1 O1W H1B 126.7 . . ? H1A O1W H1B 106.4 . . ? H2A O2W H2B 115.2 . . ? H3A O3W H3B 96.4 . . ? O4 N9 O3 94.0(15) . . ? O4 N9 O4 71(2) . 4_655 ? O3 N9 O4 84.1(12) . 4_655 ? O4 N9 O5 113.9(19) . . ? O3 N9 O5 137.3(16) . . ? O4 N9 O5 134.2(19) 4_655 . ? N9 O3 N9 82.9(18) . 4_655 ? N9 O4 N9 77.2(16) . 4_655 ? N9 O4 O4 61.3(14) . 4_655 ? N9 O4 O4 47.9(10) 4_655 4_655 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 29.97 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.592 _refine_diff_density_min -1.065 _refine_diff_density_rms 0.118 _database_code_depnum_ccdc_archive 'CCDC 904314' ####################################################################### # # 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_nb6-148 #TrackingRef 'web_deposit_cif_file_0_GeoffreyGontard_1364478012.nb6-148-publi.cif' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C52 H52 Cu2 N20 O16 Tb2 W2, 2(C30 H22 N6 Os), 2(N O3), 18(H2 O)' _chemical_formula_sum 'C112 H140 Cu2 N34 O40 Os2 Tb2 W2' _chemical_formula_weight 3795.75 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.6030 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d d' _symmetry_space_group_name_Hall '-F 2uv 2vw' _symmetry_Int_Tables_number 70 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+1/4, z' 'x, -y+1/4, -z+1/4' '-x+1/4, y, -z+1/4' 'x, y+1/2, z+1/2' '-x+1/4, -y+3/4, z+1/2' 'x, -y+3/4, -z+3/4' '-x+1/4, y+1/2, -z+3/4' 'x+1/2, y, z+1/2' '-x+3/4, -y+1/4, z+1/2' 'x+1/2, -y+1/4, -z+3/4' '-x+3/4, y, -z+3/4' 'x+1/2, y+1/2, z' '-x+3/4, -y+3/4, z' 'x+1/2, -y+3/4, -z+1/4' '-x+3/4, y+1/2, -z+1/4' '-x, -y, -z' 'x-1/4, y-1/4, -z' '-x, y-1/4, z-1/4' 'x-1/4, -y, z-1/4' '-x, -y+1/2, -z+1/2' 'x-1/4, y+1/4, -z+1/2' '-x, y+1/4, z+1/4' 'x-1/4, -y+1/2, z+1/4' '-x+1/2, -y, -z+1/2' 'x+1/4, y-1/4, -z+1/2' '-x+1/2, y-1/4, z+1/4' 'x+1/4, -y, z+1/4' '-x+1/2, -y+1/2, -z' 'x+1/4, y+1/4, -z' '-x+1/2, y+1/4, z-1/4' 'x+1/4, -y+1/2, z-1/4' _cell_length_a 22.8937(7) _cell_length_b 29.8563(10) _cell_length_c 41.8842(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 28628.7(16) _cell_formula_units_Z 8 _cell_measurement_temperature 200(1) _cell_measurement_reflns_used 9921 _cell_measurement_theta_min 4.49 _cell_measurement_theta_max 63.94 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14576 _exptl_absorpt_coefficient_mu 4.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2522 _exptl_absorpt_correction_T_max 0.3385 _exptl_absorpt_process_details ; SADABS, Bruker AXS Inc., Madison, Wisconsin, USA. ; _diffrn_ambient_temperature 200(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'curved graphite' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 68209 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 62 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 32.02 _reflns_number_total 12436 _reflns_number_gt 8673 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SUPERFLIP (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+407.0836P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 12436 _refine_ls_number_parameters 453 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.1226 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 1.1250 0.1250 0.031492(6) 0.01855(6) Uani 1 2 d S . . Os1 Os 0.8750 0.3750 0.009768(6) 0.02934(7) Uani 1 2 d S . . W1 W 0.948589(9) 0.1250 0.1250 0.01777(6) Uani 1 2 d S . . Cu1 Cu 1.1250 0.1250 -0.048499(18) 0.03002(16) Uani 1 2 d S . . O1 O 1.10576(16) 0.08536(11) -0.01439(7) 0.0294(7) Uani 1 1 d . . . O2 O 1.10167(16) 0.04255(11) 0.03775(8) 0.0288(7) Uani 1 1 d . . . O3 O 0.8750 0.5543(9) -0.1250 0.245(11) Uiso 1 2 d SD . . O4 O 0.8384(11) 0.5040(9) -0.1204(6) 0.195(11) Uiso 0.50 1 d PD . . O5 O 0.8560(10) 0.5233(8) -0.0726(5) 0.167(8) Uiso 0.50 1 d PD . . O1W O 1.21880(15) 0.09706(13) 0.01664(8) 0.0339(8) Uani 1 1 d . . . H1A H 1.2313 0.0908 -0.0014 0.041 Uiso 1 1 d R . . H1B H 1.2512 0.0950 0.0262 0.041 Uiso 1 1 d R . . O2W O 1.0204(2) 0.16210(17) -0.04633(10) 0.0585(13) Uani 1 1 d . . . H2A H 0.9990 0.1478 -0.0595 0.070 Uiso 1 1 d R . . H2B H 1.0196 0.1838 -0.0592 0.070 Uiso 1 1 d R . . O3W O 0.7638(3) -0.0081(2) 0.07712(15) 0.091(2) Uani 1 1 d . . . H3A H 0.7878 0.0178 0.0799 0.109 Uiso 1 1 d R . . H3B H 0.7292 0.0088 0.0795 0.109 Uiso 1 1 d R . . O4WA O 0.9435(4) 0.1248(4) -0.0904(2) 0.079(3) Uani 0.70 1 d P A 1 O5WA O 0.9764(4) 0.0712(2) -0.1416(2) 0.067(2) Uani 0.70 1 d P B 1 O6WA O 0.8410(5) 0.1030(4) -0.0567(3) 0.091(3) Uiso 0.70 1 d P C 1 O4WB O 0.9531(9) 0.0985(6) -0.0766(4) 0.064(5) Uani 0.30 1 d P D 2 O5WB O 0.9390(9) 0.0598(6) -0.1334(5) 0.064(5) Uani 0.30 1 d P E 2 O6WB O 0.8379(12) 0.1242(9) -0.0652(6) 0.090(7) Uiso 0.30 1 d P F 2 O7W O 0.8490(6) 0.1764(4) -0.0087(3) 0.079(3) Uiso 0.50 1 d P . . N1 N 1.06065(17) 0.11966(14) 0.07624(9) 0.0287(8) Uani 1 1 d . . . N2 N 0.9972(2) 0.22928(15) 0.11733(11) 0.0362(9) Uani 1 1 d . . . N3 N 0.83828(19) 0.05810(15) 0.10581(10) 0.0343(9) Uani 1 1 d . . . N4 N 0.91103(19) 0.15543(15) 0.05145(10) 0.0334(9) Uani 1 1 d . . . N5 N 1.1002(2) 0.08497(17) -0.08147(10) 0.0378(10) Uani 1 1 d . . . N6 N 0.8415(2) 0.33331(15) 0.04471(11) 0.0366(9) Uani 1 1 d . . . N7 N 0.93474(18) 0.32670(16) 0.01102(11) 0.0366(10) Uani 1 1 d . . . N8 N 0.9303(2) 0.3957(2) -0.02578(13) 0.0454(12) Uani 1 1 d . . . N9 N 0.8629(10) 0.5303(9) -0.1024(5) 0.204(15) Uiso 0.50 1 d PD . . C1 C 1.02141(18) 0.11939(15) 0.09348(10) 0.0238(8) Uani 1 1 d . . . C2 C 0.98043(19) 0.19292(16) 0.12085(11) 0.0259(8) Uani 1 1 d . . . C3 C 0.87573(19) 0.08143(15) 0.11306(10) 0.0241(7) Uani 1 1 d . . . C4 C 0.92137(18) 0.14434(16) 0.07718(11) 0.0259(8) Uani 1 1 d . . . C5 C 1.1036(3) 0.01890(19) 0.06784(13) 0.0415(12) Uani 1 1 d . . . H5A H 1.0653 0.0081 0.0730 0.062 Uiso 1 1 calc R . . H5B H 1.1169 0.0388 0.0843 0.062 Uiso 1 1 calc R . . H5C H 1.1301 -0.0060 0.0662 0.062 Uiso 1 1 calc R . . C6 C 1.0871(2) 0.01780(16) 0.01076(11) 0.0273(9) Uani 1 1 d . . . C7 C 1.0706(2) -0.02658(18) 0.01046(13) 0.0364(11) Uani 1 1 d . . . H7 H 1.0676 -0.0425 0.0295 0.044 Uiso 1 1 calc R . . C8 C 1.0584(3) -0.04727(19) -0.01818(15) 0.0434(13) Uani 1 1 d . . . H8 H 1.0469 -0.0771 -0.0184 0.052 Uiso 1 1 calc R . . C9 C 1.0631(2) -0.02398(19) -0.04668(14) 0.0405(12) Uani 1 1 d . . . H9 H 1.0551 -0.0385 -0.0658 0.049 Uiso 1 1 calc R . . C10 C 1.0799(2) 0.02142(18) -0.04692(12) 0.0328(10) Uani 1 1 d . . . C11 C 1.09126(19) 0.04256(15) -0.01766(11) 0.0257(8) Uani 1 1 d . . . C12 C 1.0835(2) 0.0441(2) -0.07775(12) 0.0376(12) Uani 1 1 d . . . H12 H 1.0731 0.0280 -0.0959 0.045 Uiso 1 1 calc R . . C13 C 1.1007(3) 0.1078(2) -0.11221(13) 0.0478(14) Uani 1 1 d . . . H13A H 1.0634 0.1225 -0.1158 0.057 Uiso 1 1 calc R . . H13B H 1.1068 0.0863 -0.1292 0.057 Uiso 1 1 calc R . . C14 C 0.7916(3) 0.3390(2) 0.06123(15) 0.0473(14) Uani 1 1 d . . . H14 H 0.7681 0.3635 0.0565 0.057 Uiso 1 1 calc R . . C15 C 0.7738(4) 0.3100(3) 0.08491(17) 0.0615(19) Uani 1 1 d . . . H15 H 0.7393 0.3151 0.0960 0.074 Uiso 1 1 calc R . . C16 C 0.8075(4) 0.2740(3) 0.09179(18) 0.064(2) Uani 1 1 d . . . H16 H 0.7959 0.2539 0.1076 0.077 Uiso 1 1 calc R . . C17 C 0.8584(3) 0.2670(2) 0.07563(17) 0.0539(16) Uani 1 1 d . . . H17 H 0.8817 0.2424 0.0805 0.065 Uiso 1 1 calc R . . C18 C 0.8754(2) 0.29673(18) 0.05185(13) 0.0379(11) Uani 1 1 d . . . C19 C 0.9285(2) 0.29323(18) 0.03293(15) 0.0403(13) Uani 1 1 d . . . C20 C 0.9705(3) 0.2599(2) 0.0352(2) 0.0555(17) Uani 1 1 d . . . H20 H 0.9666 0.2365 0.0497 0.067 Uiso 1 1 calc R . . C21 C 1.0186(3) 0.2628(2) 0.0151(2) 0.070(2) Uani 1 1 d . . . H21 H 1.0478 0.2412 0.0165 0.084 Uiso 1 1 calc R . . C22 C 1.0242(3) 0.2964(2) -0.0067(2) 0.0574(19) Uani 1 1 d . . . H22 H 1.0566 0.2974 -0.0201 0.069 Uiso 1 1 calc R . . C23 C 0.9812(2) 0.3293(2) -0.00884(16) 0.0424(13) Uani 1 1 d . . . C24 C 0.9779(2) 0.3670(2) -0.03022(16) 0.0469(15) Uani 1 1 d . . . C25 C 1.0173(3) 0.3746(3) -0.0552(2) 0.072(2) Uani 1 1 d . . . H25 H 1.0495 0.3560 -0.0579 0.086 Uiso 1 1 calc R . . C26 C 1.0082(4) 0.4094(4) -0.0753(2) 0.086(3) Uani 1 1 d . . . H26 H 1.0339 0.4145 -0.0922 0.104 Uiso 1 1 calc R . . C27 C 0.9607(4) 0.4374(4) -0.0710(3) 0.099(4) Uani 1 1 d . . . H27 H 0.9541 0.4611 -0.0850 0.119 Uiso 1 1 calc R . . C28 C 0.9229(3) 0.4300(3) -0.0455(2) 0.069(2) Uani 1 1 d . . . H28 H 0.8918 0.4495 -0.0423 0.083 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 Tb1 0.02229(11) 0.01918(12) 0.01417(11) 0.000 0.000 -0.00018(10) Os1 0.02422(11) 0.03191(13) 0.03188(13) 0.000 0.000 0.00871(10) W1 0.01948(9) 0.01964(10) 0.01418(9) -0.00060(9) 0.000 0.000 Cu1 0.0443(4) 0.0315(4) 0.0142(3) 0.000 0.000 -0.0079(4) O1 0.0454(18) 0.0243(16) 0.0184(14) -0.0035(12) -0.0004(13) -0.0062(14) O2 0.0405(17) 0.0237(16) 0.0223(15) 0.0006(12) 0.0012(13) -0.0015(13) O1W 0.0299(16) 0.045(2) 0.0267(16) -0.0067(15) 0.0008(13) 0.0074(15) O2W 0.073(3) 0.065(3) 0.037(2) 0.012(2) -0.019(2) -0.017(3) O3W 0.078(4) 0.095(5) 0.100(5) -0.054(4) 0.009(3) -0.031(3) O4WA 0.075(6) 0.096(7) 0.066(6) -0.019(5) -0.009(4) 0.004(5) O5WA 0.081(6) 0.034(4) 0.086(6) -0.006(4) -0.018(5) 0.006(4) O4WB 0.091(13) 0.048(10) 0.053(10) 0.011(8) -0.011(9) -0.025(9) O5WB 0.066(11) 0.049(10) 0.077(13) -0.014(9) -0.022(10) 0.025(9) N1 0.0262(16) 0.037(2) 0.0228(17) 0.0035(16) 0.0012(13) 0.0040(15) N2 0.046(2) 0.024(2) 0.038(2) 0.0010(17) 0.0027(18) -0.0054(17) N3 0.038(2) 0.034(2) 0.031(2) 0.0004(17) -0.0037(17) -0.0057(17) N4 0.040(2) 0.035(2) 0.0248(19) 0.0039(17) -0.0033(16) 0.0026(18) N5 0.044(2) 0.050(3) 0.0195(18) -0.0065(18) -0.0016(17) -0.007(2) N6 0.044(2) 0.032(2) 0.034(2) 0.0012(18) -0.0042(18) 0.0091(18) N7 0.0302(19) 0.035(2) 0.044(3) -0.0128(19) -0.0079(17) 0.0084(17) N8 0.028(2) 0.059(3) 0.048(3) 0.001(2) 0.0037(19) 0.003(2) C1 0.0265(18) 0.028(2) 0.0171(17) 0.0014(15) -0.0021(14) 0.0030(15) C2 0.0260(18) 0.026(2) 0.026(2) 0.0004(17) -0.0005(15) 0.0014(15) C3 0.0269(17) 0.0263(19) 0.0190(17) -0.0003(15) -0.0012(16) 0.0009(17) C4 0.0245(18) 0.029(2) 0.024(2) -0.0022(17) -0.0014(15) 0.0021(16) C5 0.065(3) 0.030(3) 0.030(3) 0.007(2) 0.001(2) 0.001(2) C6 0.029(2) 0.023(2) 0.030(2) -0.0043(17) 0.0034(16) 0.0009(16) C7 0.044(3) 0.026(2) 0.039(3) -0.002(2) 0.005(2) -0.003(2) C8 0.049(3) 0.026(2) 0.055(3) -0.014(2) 0.009(3) -0.007(2) C9 0.043(3) 0.035(3) 0.043(3) -0.020(2) 0.004(2) -0.005(2) C10 0.035(2) 0.033(3) 0.030(2) -0.012(2) 0.0002(18) -0.0048(19) C11 0.0270(19) 0.025(2) 0.025(2) -0.0043(17) 0.0007(16) -0.0030(16) C12 0.040(3) 0.048(3) 0.025(2) -0.015(2) 0.0002(19) -0.007(2) C13 0.067(4) 0.058(4) 0.019(2) -0.006(2) -0.003(2) -0.017(3) C14 0.053(3) 0.039(3) 0.050(3) 0.005(3) 0.012(3) 0.002(3) C15 0.078(5) 0.052(4) 0.055(4) 0.012(3) 0.024(4) -0.001(4) C16 0.092(6) 0.052(4) 0.048(4) 0.015(3) 0.004(4) -0.002(4) C17 0.077(5) 0.033(3) 0.052(4) 0.007(3) -0.016(3) 0.003(3) C18 0.047(3) 0.029(2) 0.038(3) -0.001(2) -0.013(2) 0.007(2) C19 0.042(3) 0.028(2) 0.052(3) -0.010(2) -0.018(2) 0.010(2) C20 0.044(3) 0.035(3) 0.087(5) -0.006(3) -0.015(3) 0.011(3) C21 0.042(3) 0.037(3) 0.130(8) -0.014(4) -0.007(4) 0.013(3) C22 0.033(3) 0.050(4) 0.089(5) -0.022(4) 0.003(3) 0.008(3) C23 0.028(2) 0.039(3) 0.060(4) -0.015(3) -0.002(2) 0.005(2) C24 0.026(2) 0.062(4) 0.052(3) -0.015(3) 0.010(2) -0.002(2) C25 0.044(3) 0.098(7) 0.073(5) -0.006(5) 0.023(3) -0.001(4) C26 0.061(5) 0.117(8) 0.082(6) 0.021(6) 0.040(4) 0.003(5) C27 0.080(6) 0.113(9) 0.105(8) 0.056(7) 0.030(6) 0.003(6) C28 0.055(4) 0.078(5) 0.073(5) 0.036(4) 0.022(4) 0.007(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Tb1 O1 2.299(3) 2_755 ? Tb1 O1 2.299(3) . ? Tb1 O1W 2.386(3) 2_755 ? Tb1 O1W 2.386(3) . ? Tb1 N1 2.389(4) . ? Tb1 N1 2.389(4) 2_755 ? Tb1 O2 2.533(3) 2_755 ? Tb1 O2 2.533(3) . ? Tb1 Cu1 3.3504(8) . ? Os1 N7 1.988(4) 14_655 ? Os1 N7 1.988(4) . ? Os1 N8 2.050(5) 14_655 ? Os1 N8 2.050(5) . ? Os1 N6 2.069(5) 14_655 ? Os1 N6 2.069(5) . ? W1 C1 2.133(4) . ? W1 C1 2.133(4) 3 ? W1 C2 2.162(5) . ? W1 C2 2.162(5) 3 ? W1 C3 2.174(4) 3 ? W1 C3 2.174(4) . ? W1 C4 2.176(4) . ? W1 C4 2.176(4) 3 ? Cu1 O1 1.907(3) 2_755 ? Cu1 O1 1.907(3) . ? Cu1 N5 1.912(4) 2_755 ? Cu1 N5 1.912(4) . ? O1 C11 1.327(5) . ? O2 C6 1.391(6) . ? O2 C5 1.445(6) . ? O3 N9 1.218(17) 12_654 ? O3 N9 1.218(17) . ? O3 O4 1.73(3) . ? O3 O4 1.73(3) 12_654 ? O4 N9 1.224(18) . ? O5 N9 1.277(16) . ? N1 C1 1.152(6) . ? N2 C2 1.161(6) . ? N3 C3 1.145(6) . ? N4 C4 1.152(6) . ? N5 C12 1.287(7) . ? N5 C13 1.457(7) . ? N6 C14 1.346(7) . ? N6 C18 1.373(6) . ? N7 C23 1.352(7) . ? N7 C19 1.364(8) . ? N8 C28 1.328(9) . ? N8 C24 1.399(8) . ? C6 C7 1.378(7) . ? C6 C11 1.405(7) . ? C7 C8 1.378(8) . ? C8 C9 1.385(9) . ? C9 C10 1.409(7) . ? C10 C11 1.403(6) . ? C10 C12 1.461(8) . ? C13 C13 1.515(12) 2_755 ? C14 C15 1.378(9) . ? C15 C16 1.355(11) . ? C16 C17 1.364(11) . ? C17 C18 1.390(9) . ? C18 C19 1.454(9) . ? C19 C20 1.388(8) . ? C20 C21 1.391(11) . ? C21 C22 1.361(11) . ? C22 C23 1.393(8) . ? C23 C24 1.440(9) . ? C24 C25 1.399(9) . ? C25 C26 1.355(13) . ? C26 C27 1.384(13) . ? C27 C28 1.390(11) . ? 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 O1 Tb1 O1 66.61(16) 2_755 . ? O1 Tb1 O1W 76.97(13) 2_755 2_755 ? O1 Tb1 O1W 77.86(13) . 2_755 ? O1 Tb1 O1W 77.86(13) 2_755 . ? O1 Tb1 O1W 76.97(13) . . ? O1W Tb1 O1W 149.77(17) 2_755 . ? O1 Tb1 N1 143.90(13) 2_755 . ? O1 Tb1 N1 120.21(13) . . ? O1W Tb1 N1 70.91(12) 2_755 . ? O1W Tb1 N1 137.40(13) . . ? O1 Tb1 N1 120.21(13) 2_755 2_755 ? O1 Tb1 N1 143.90(13) . 2_755 ? O1W Tb1 N1 137.40(13) 2_755 2_755 ? O1W Tb1 N1 70.91(12) . 2_755 ? N1 Tb1 N1 76.66(19) . 2_755 ? O1 Tb1 O2 62.99(11) 2_755 2_755 ? O1 Tb1 O2 128.84(11) . 2_755 ? O1W Tb1 O2 82.93(12) 2_755 2_755 ? O1W Tb1 O2 100.19(12) . 2_755 ? N1 Tb1 O2 96.53(13) . 2_755 ? N1 Tb1 O2 73.98(13) 2_755 2_755 ? O1 Tb1 O2 128.84(11) 2_755 . ? O1 Tb1 O2 62.99(11) . . ? O1W Tb1 O2 100.19(12) 2_755 . ? O1W Tb1 O2 82.93(12) . . ? N1 Tb1 O2 73.98(13) . . ? N1 Tb1 O2 96.53(13) 2_755 . ? O2 Tb1 O2 168.12(14) 2_755 . ? O1 Tb1 Cu1 33.31(8) 2_755 . ? O1 Tb1 Cu1 33.31(8) . . ? O1W Tb1 Cu1 74.89(8) 2_755 . ? O1W Tb1 Cu1 74.89(8) . . ? N1 Tb1 Cu1 141.67(9) . . ? N1 Tb1 Cu1 141.67(9) 2_755 . ? O2 Tb1 Cu1 95.94(7) 2_755 . ? O2 Tb1 Cu1 95.94(7) . . ? N7 Os1 N7 177.0(3) 14_655 . ? N7 Os1 N8 79.2(2) 14_655 14_655 ? N7 Os1 N8 103.03(19) . 14_655 ? N7 Os1 N8 103.03(19) 14_655 . ? N7 Os1 N8 79.2(2) . . ? N8 Os1 N8 86.8(3) 14_655 . ? N7 Os1 N6 78.46(19) 14_655 14_655 ? N7 Os1 N6 99.36(17) . 14_655 ? N8 Os1 N6 157.6(2) 14_655 14_655 ? N8 Os1 N6 96.0(2) . 14_655 ? N7 Os1 N6 99.36(17) 14_655 . ? N7 Os1 N6 78.46(19) . . ? N8 Os1 N6 96.0(2) 14_655 . ? N8 Os1 N6 157.6(2) . . ? N6 Os1 N6 89.9(3) 14_655 . ? C1 W1 C1 77.2(2) . 3 ? C1 W1 C2 76.14(17) . . ? C1 W1 C2 73.30(17) 3 . ? C1 W1 C2 73.30(17) . 3 ? C1 W1 C2 76.14(17) 3 3 ? C2 W1 C2 140.6(2) . 3 ? C1 W1 C3 142.10(16) . 3 ? C1 W1 C3 114.23(16) 3 3 ? C2 W1 C3 73.49(16) . 3 ? C2 W1 C3 143.29(16) 3 3 ? C1 W1 C3 114.23(16) . . ? C1 W1 C3 142.10(16) 3 . ? C2 W1 C3 143.29(16) . . ? C2 W1 C3 73.49(16) 3 . ? C3 W1 C3 79.8(2) 3 . ? C1 W1 C4 71.03(16) . . ? C1 W1 C4 140.61(16) 3 . ? C2 W1 C4 76.92(17) . . ? C2 W1 C4 114.81(17) 3 . ? C3 W1 C4 80.39(16) 3 . ? C3 W1 C4 74.17(16) . . ? C1 W1 C4 140.61(16) . 3 ? C1 W1 C4 71.03(16) 3 3 ? C2 W1 C4 114.81(17) . 3 ? C2 W1 C4 76.92(17) 3 3 ? C3 W1 C4 74.17(16) 3 3 ? C3 W1 C4 80.39(16) . 3 ? C4 W1 C4 146.7(2) . 3 ? O1 Cu1 O1 82.94(19) 2_755 . ? O1 Cu1 N5 94.86(17) 2_755 2_755 ? O1 Cu1 N5 175.93(18) . 2_755 ? O1 Cu1 N5 175.93(18) 2_755 . ? O1 Cu1 N5 94.86(17) . . ? N5 Cu1 N5 87.5(3) 2_755 . ? O1 Cu1 Tb1 41.47(10) 2_755 . ? O1 Cu1 Tb1 41.47(10) . . ? N5 Cu1 Tb1 136.24(14) 2_755 . ? N5 Cu1 Tb1 136.24(14) . . ? C11 O1 Cu1 125.3(3) . . ? C11 O1 Tb1 129.0(3) . . ? Cu1 O1 Tb1 105.22(14) . . ? C6 O2 C5 117.2(4) . . ? C6 O2 Tb1 118.9(3) . . ? C5 O2 Tb1 123.9(3) . . ? N9 O3 N9 108(3) 12_654 . ? N9 O3 O4 71.7(18) 12_654 . ? N9 O3 O4 45.1(12) . . ? N9 O3 O4 45.1(12) 12_654 12_654 ? N9 O3 O4 71.7(18) . 12_654 ? O4 O3 O4 60(2) . 12_654 ? N9 O4 O3 44.8(12) . . ? C1 N1 Tb1 166.5(3) . . ? C12 N5 C13 123.5(4) . . ? C12 N5 Cu1 126.3(4) . . ? C13 N5 Cu1 110.1(4) . . ? C14 N6 C18 117.9(5) . . ? C14 N6 Os1 127.0(4) . . ? C18 N6 Os1 115.0(4) . . ? C23 N7 C19 122.5(5) . . ? C23 N7 Os1 118.9(4) . . ? C19 N7 Os1 118.5(4) . . ? C28 N8 C24 119.3(6) . . ? C28 N8 Os1 127.3(4) . . ? C24 N8 Os1 113.1(4) . . ? O3 N9 O4 90(2) . . ? O3 N9 O5 152(3) . . ? O4 N9 O5 116(2) . . ? N1 C1 W1 175.1(4) . . ? N2 C2 W1 177.3(4) . . ? N3 C3 W1 177.7(4) . . ? N4 C4 W1 175.1(4) . . ? C7 C6 O2 125.7(5) . . ? C7 C6 C11 121.1(4) . . ? O2 C6 C11 113.1(4) . . ? C8 C7 C6 119.6(5) . . ? C7 C8 C9 120.6(5) . . ? C8 C9 C10 120.7(5) . . ? C11 C10 C9 118.5(5) . . ? C11 C10 C12 123.5(5) . . ? C9 C10 C12 118.0(5) . . ? O1 C11 C10 124.7(4) . . ? O1 C11 C6 115.9(4) . . ? C10 C11 C6 119.4(4) . . ? N5 C12 C10 124.3(4) . . ? N5 C13 C13 108.8(4) . 2_755 ? N6 C14 C15 122.8(6) . . ? C16 C15 C14 118.9(7) . . ? C15 C16 C17 120.1(7) . . ? C16 C17 C18 119.9(6) . . ? N6 C18 C17 120.3(6) . . ? N6 C18 C19 114.3(5) . . ? C17 C18 C19 125.4(5) . . ? N7 C19 C20 120.0(6) . . ? N7 C19 C18 113.7(4) . . ? C20 C19 C18 126.3(6) . . ? C19 C20 C21 117.5(7) . . ? C22 C21 C20 121.8(6) . . ? C21 C22 C23 119.8(7) . . ? N7 C23 C22 118.4(6) . . ? N7 C23 C24 112.7(5) . . ? C22 C23 C24 128.9(6) . . ? N8 C24 C25 120.1(7) . . ? N8 C24 C23 115.9(5) . . ? C25 C24 C23 123.9(6) . . ? C26 C25 C24 119.5(8) . . ? C25 C26 C27 120.1(7) . . ? C26 C27 C28 119.6(9) . . ? N8 C28 C27 121.4(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 32.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.193 _refine_diff_density_min -3.124 _refine_diff_density_rms 0.182 _database_code_depnum_ccdc_archive 'CCDC 931580'