# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Efthymiou, Constantinos' 'Georgopoulou, Anastasia' 'Papatriantafyllopoulou, Constantina' 'Terzis, Aris' 'Raptopoulou, Catherine' 'Escuer, A.' 'Perlepes, Spyros' _publ_contact_author_name 'Perlepes, Spyros' _publ_contact_author_email perlepes@patreas.upatras.gr _publ_section_title ; Initial employment of di-2-pyridyl ketone as a route to nickel(II)/lanthanide(III) clusters: triangular Ni2Ln complexes ; # Attachment '- peng37a.cif' data_peng37a _database_code_depnum_ccdc_archive 'CCDC 778581' #TrackingRef '- peng37a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54.60 H63.80 Cl2 N9 Ni2 O22.30 Tb' _chemical_formula_weight 1550.19 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' Ni Ni 0.3393 1.1124 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.998(5) _cell_length_b 12.117(5) _cell_length_c 26.990(10) _cell_angle_alpha 81.400(10) _cell_angle_beta 89.580(10) _cell_angle_gamma 63.280(10) _cell_volume 3457(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.5 _cell_measurement_theta_max 11.0 _exptl_crystal_description parallelepiped' _exptl_crystal_colour green _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 1.704 _exptl_absorpt_correction_type 'psi-scan empirical' _exptl_absorpt_correction_T_min 0.797 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _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 'Crystal Logic Dual Goniometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.8 _diffrn_reflns_number 12750 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.01 _reflns_number_total 12129 _reflns_number_gt 9795 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0966P)^2^+4.8786P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12129 _refine_ls_number_parameters 817 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1663 _refine_ls_wR_factor_gt 0.1526 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.076 _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 Tb Tb 0.43046(2) 0.11192(3) 0.697164(11) 0.03928(12) Uani 1 1 d . . . Ni1 Ni 0.21868(6) 0.07885(7) 0.77714(3) 0.03817(19) Uani 1 1 d . . . Ni2 Ni 0.50241(7) -0.10663(7) 0.80302(3) 0.03973(19) Uani 1 1 d . . . O1 O 0.3990(4) 0.0867(4) 0.78521(16) 0.0408(9) Uani 1 1 d . . . N1 N 0.1639(5) 0.2510(5) 0.8005(2) 0.0456(12) Uani 1 1 d . . . N2 N 0.4511(5) -0.0549(5) 0.8735(2) 0.0473(12) Uani 1 1 d . . . O11 O 0.3409(3) -0.1001(4) 0.77276(16) 0.0400(9) Uani 1 1 d . . . N11 N 0.1942(5) -0.0173(6) 0.8439(2) 0.0486(13) Uani 1 1 d . . . N12 N 0.5369(5) -0.2909(5) 0.8235(2) 0.0513(13) Uani 1 1 d . . . O21 O 0.5560(3) -0.0929(4) 0.73118(16) 0.0400(9) Uani 1 1 d . . . N21 N 0.6882(5) -0.1350(6) 0.8142(2) 0.0529(14) Uani 1 1 d . . . N22 N 0.6391(5) 0.0036(5) 0.6549(2) 0.0535(14) Uani 1 1 d . . . O31 O 0.2296(4) 0.1560(4) 0.70616(16) 0.0402(9) Uani 1 1 d . . . N31 N 0.0504(5) 0.1099(5) 0.7431(2) 0.0437(12) Uani 1 1 d . . . N32 N 0.3416(5) 0.0169(5) 0.6394(2) 0.0504(13) Uani 1 1 d . . . O41 O 0.5512(5) 0.2192(6) 0.7112(2) 0.0716(16) Uani 1 1 d . . . O42 O 0.3549(5) 0.3278(4) 0.7180(2) 0.0598(12) Uani 1 1 d . . . O1W O 0.3840(5) 0.2428(5) 0.6174(2) 0.0666(14) Uani 1 1 d . . . C1 C 0.0474(7) 0.3498(7) 0.7923(3) 0.0609(19) Uani 1 1 d . . . H1 H -0.0181 0.3388 0.7796 0.079 Uiso 1 1 calc R . . C2 C 0.0254(8) 0.4648(8) 0.8023(4) 0.079(3) Uani 1 1 d . . . H2 H -0.0551 0.5307 0.7970 0.103 Uiso 1 1 calc R . . C3 C 0.1200(9) 0.4837(8) 0.8199(4) 0.084(3) Uani 1 1 d . . . H3 H 0.1050 0.5618 0.8269 0.109 Uiso 1 1 calc R . . C4 C 0.2399(8) 0.3839(8) 0.8274(3) 0.068(2) Uani 1 1 d . . . H4 H 0.3067 0.3948 0.8388 0.088 Uiso 1 1 calc R . . C5 C 0.2581(6) 0.2692(6) 0.8176(3) 0.0470(14) Uani 1 1 d . . . C6 C 0.3870(6) 0.1538(6) 0.8245(2) 0.0443(14) Uani 1 1 d . . . O2 O 0.4772(5) 0.1982(5) 0.8237(2) 0.0632(13) Uani 1 1 d . . . H2O H 0.5393 0.1470 0.8416 0.082 Uiso 1 1 calc R . . C7 C 0.4003(6) 0.0683(7) 0.8748(2) 0.0461(14) Uani 1 1 d . . . C8 C 0.3601(7) 0.1175(8) 0.9189(3) 0.0614(19) Uani 1 1 d . . . H8 H 0.3262 0.2032 0.9190 0.080 Uiso 1 1 calc R . . C9 C 0.3722(8) 0.0351(10) 0.9626(3) 0.073(2) Uani 1 1 d . . . H9 H 0.3453 0.0655 0.9924 0.095 Uiso 1 1 calc R . . C10 C 0.4239(8) -0.0910(9) 0.9618(3) 0.072(2) Uani 1 1 d . . . H10 H 0.4322 -0.1473 0.9907 0.094 Uiso 1 1 calc R . . C11 C 0.4639(7) -0.1328(8) 0.9161(3) 0.0578(18) Uani 1 1 d . . . H11 H 0.5008 -0.2184 0.9154 0.075 Uiso 1 1 calc R . . C21 C 0.1311(7) 0.0323(8) 0.8827(3) 0.0604(18) Uani 1 1 d . . . H21 H 0.0990 0.1180 0.8825 0.079 Uiso 1 1 calc R . . C22 C 0.1127(8) -0.0422(11) 0.9238(3) 0.078(3) Uani 1 1 d . . . H22 H 0.0681 -0.0063 0.9502 0.101 Uiso 1 1 calc R . . C23 C 0.1616(10) -0.1693(11) 0.9242(3) 0.083(3) Uani 1 1 d . . . H23 H 0.1512 -0.2205 0.9512 0.108 Uiso 1 1 calc R . . C24 C 0.2250(7) -0.2188(8) 0.8849(3) 0.0630(19) Uani 1 1 d . . . H24 H 0.2578 -0.3043 0.8846 0.082 Uiso 1 1 calc R . . C25 C 0.2409(6) -0.1427(7) 0.8455(3) 0.0487(15) Uani 1 1 d . . . C26 C 0.3140(6) -0.1898(6) 0.7991(3) 0.0453(14) Uani 1 1 d . . . O12 O 0.2317(4) -0.2181(4) 0.77150(19) 0.0522(11) Uani 1 1 d . . . C27 C 0.4364(6) -0.3091(7) 0.8161(3) 0.0548(17) Uani 1 1 d . . . C28 C 0.4452(8) -0.4297(7) 0.8232(4) 0.073(2) Uani 1 1 d . . . H28 H 0.3757 -0.4412 0.8163 0.095 Uiso 1 1 calc R . . C29 C 0.5571(10) -0.5309(8) 0.8404(5) 0.093(3) Uani 1 1 d . . . H29 H 0.5637 -0.6112 0.8462 0.121 Uiso 1 1 calc R . . C30 C 0.6595(9) -0.5118(8) 0.8490(4) 0.084(3) Uani 1 1 d . . . H30 H 0.7362 -0.5797 0.8604 0.109 Uiso 1 1 calc R . . C31 C 0.6485(7) -0.3915(7) 0.8408(3) 0.068(2) Uani 1 1 d . . . H31 H 0.7178 -0.3790 0.8470 0.088 Uiso 1 1 calc R . . C32 C 0.2712(8) -0.2486(8) 0.7226(3) 0.0635(19) Uani 1 1 d . . . H32A H 0.3516 -0.3225 0.7261 0.083 Uiso 1 1 calc R . . H32B H 0.2800 -0.1798 0.7026 0.083 Uiso 1 1 calc R . . C33 C 0.1775(10) -0.2718(13) 0.6979(4) 0.100(4) Uani 1 1 d . . . H33A H 0.2022 -0.2909 0.6651 0.130 Uiso 1 1 calc R . . H33B H 0.0981 -0.1985 0.6949 0.130 Uiso 1 1 calc R . . H33C H 0.1707 -0.3411 0.7175 0.130 Uiso 1 1 calc R . . C41 C 0.7436(7) -0.1345(10) 0.8567(3) 0.074(2) Uani 1 1 d . . . H41 H 0.6981 -0.1196 0.8851 0.096 Uiso 1 1 calc R . . C42 C 0.8658(8) -0.1552(10) 0.8598(4) 0.081(3) Uani 1 1 d . . . H42 H 0.9030 -0.1570 0.8902 0.105 Uiso 1 1 calc R . . C43 C 0.9321(7) -0.1730(8) 0.8182(4) 0.070(2) Uani 1 1 d . . . H43 H 1.0145 -0.1858 0.8195 0.090 Uiso 1 1 calc R . . C44 C 0.8749(6) -0.1715(7) 0.7744(3) 0.0581(18) Uani 1 1 d . . . H44 H 0.9181 -0.1825 0.7453 0.076 Uiso 1 1 calc R . . C45 C 0.7526(5) -0.1538(6) 0.7732(3) 0.0447(14) Uani 1 1 d . . . C46 C 0.6814(5) -0.1589(6) 0.7273(3) 0.0437(14) Uani 1 1 d . . . O22 O 0.7218(4) -0.2922(4) 0.73173(19) 0.0499(11) Uani 1 1 d . . . C47 C 0.7196(6) -0.1105(6) 0.6776(3) 0.0498(15) Uani 1 1 d . . . C48 C 0.8308(7) -0.1819(8) 0.6568(3) 0.066(2) Uani 1 1 d . . . H48 H 0.8833 -0.2631 0.6725 0.086 Uiso 1 1 calc R . . C49 C 0.8627(8) -0.1329(9) 0.6136(4) 0.077(2) Uani 1 1 d . . . H49 H 0.9376 -0.1790 0.5997 0.101 Uiso 1 1 calc R . . C50 C 0.7814(9) -0.0132(10) 0.5908(4) 0.081(3) Uani 1 1 d . . . H50 H 0.8003 0.0232 0.5612 0.105 Uiso 1 1 calc R . . C51 C 0.6724(8) 0.0509(8) 0.6125(3) 0.072(2) Uani 1 1 d . . . H51 H 0.6183 0.1317 0.5970 0.093 Uiso 1 1 calc R . . C52 C 0.6517(7) -0.3247(7) 0.6989(4) 0.064(2) Uani 1 1 d . . . H52A H 0.6602 -0.2966 0.6641 0.084 Uiso 1 1 calc R . . H52B H 0.5638 -0.2851 0.7054 0.084 Uiso 1 1 calc R . . C53 C 0.7029(11) -0.4649(9) 0.7088(5) 0.092(3) Uani 1 1 d . . . H53A H 0.6495 -0.4885 0.6915 0.120 Uiso 1 1 calc R . . H53B H 0.7065 -0.4930 0.7442 0.120 Uiso 1 1 calc R . . H53C H 0.7855 -0.5027 0.6971 0.120 Uiso 1 1 calc R . . C61 C -0.0472(6) 0.1048(7) 0.7667(3) 0.0561(17) Uani 1 1 d . . . H61 H -0.0357 0.0716 0.8007 0.073 Uiso 1 1 calc R . . C62 C -0.1628(7) 0.1469(8) 0.7425(3) 0.069(2) Uani 1 1 d . . . H62 H -0.2289 0.1441 0.7600 0.089 Uiso 1 1 calc R . . C63 C -0.1786(7) 0.1921(9) 0.6930(4) 0.076(2) Uani 1 1 d . . . H63 H -0.2563 0.2211 0.6761 0.099 Uiso 1 1 calc R . . C64 C -0.0791(7) 0.1957(8) 0.6669(3) 0.066(2) Uani 1 1 d . . . H64 H -0.0883 0.2250 0.6326 0.085 Uiso 1 1 calc R . . C65 C 0.0349(6) 0.1534(7) 0.6944(3) 0.0505(16) Uani 1 1 d . . . C66 C 0.1491(6) 0.1601(6) 0.6701(2) 0.0427(13) Uani 1 1 d . . . O32 O 0.1062(4) 0.2710(4) 0.63297(17) 0.0504(11) Uani 1 1 d . B . C67 C 0.2171(6) 0.0572(6) 0.6383(3) 0.0475(15) Uani 1 1 d . . . C68 C 0.1567(8) 0.0145(8) 0.6078(3) 0.069(2) Uani 1 1 d . . . H68 H 0.0704 0.0445 0.6073 0.089 Uiso 1 1 calc R . . C69 C 0.2286(12) -0.0750(11) 0.5778(4) 0.100(4) Uani 1 1 d . . . H69 H 0.1908 -0.1062 0.5576 0.130 Uiso 1 1 calc R . . C70 C 0.3526(10) -0.1144(9) 0.5790(4) 0.085(3) Uani 1 1 d . . . H70 H 0.4021 -0.1736 0.5596 0.111 Uiso 1 1 calc R . . C71 C 0.4059(8) -0.0657(8) 0.6093(3) 0.070(2) Uani 1 1 d . . . H71 H 0.4916 -0.0920 0.6088 0.091 Uiso 1 1 calc R . . C72 C 0.0556(9) 0.3849(7) 0.6536(3) 0.070(2) Uani 1 1 d . . . H72A H 0.1232 0.3950 0.6684 0.091 Uiso 1 1 calc R A 1 H72B H 0.0017 0.3803 0.6799 0.091 Uiso 1 1 calc R A 1 C73 C -0.020(3) 0.499(4) 0.6126(15) 0.140(17) Uani 0.50 1 d P B 1 C73A C 0.042(3) 0.4863(18) 0.6109(14) 0.110(13) Uani 0.50 1 d P B 2 N41 N 0.4632(7) 0.3186(7) 0.7206(3) 0.0677(18) Uani 1 1 d . . . O43 O 0.4795(8) 0.4047(7) 0.7322(3) 0.102(2) Uani 1 1 d . . . Cl1 Cl 0.2555(2) 0.8600(3) 0.07855(10) 0.0871(7) Uani 1 1 d . . . O51 O 0.2070(11) 0.8469(10) 0.1253(4) 0.161(5) Uani 1 1 d . . . O52 O 0.3745(9) 0.8581(13) 0.0876(4) 0.164(5) Uani 1 1 d . . . O53 O 0.1793(9) 0.9746(10) 0.0474(3) 0.142(4) Uani 1 1 d . . . O54 O 0.2802(15) 0.7627(11) 0.0505(4) 0.181(5) Uani 1 1 d . . . Cl2 Cl 0.1215(5) 0.7307(5) 0.49774(15) 0.1474(16) Uani 1 1 d . . . O55 O 0.1402(16) 0.6926(15) 0.5492(5) 0.205(6) Uani 1 1 d . . . O56 O 0.216(3) 0.754(2) 0.4752(8) 0.324(14) Uani 1 1 d . . . O57 O 0.064(3) 0.690(3) 0.4718(9) 0.400(19) Uani 1 1 d . . . O58 O 0.028(3) 0.865(2) 0.4969(14) 0.47(3) Uani 1 1 d . . . O1E O 0.2326(9) 0.2487(9) 0.5429(4) 0.128(3) Uiso 1 1 d D . . C1E C 0.228(3) 0.262(3) 0.4947(9) 0.257(13) Uiso 1 1 d D . . C2E C 0.317(3) 0.264(3) 0.4737(10) 0.238(12) Uiso 1 1 d D . . O2E O 0.6369(16) 0.5249(16) 0.4046(6) 0.107(5) Uiso 0.50 1 d PD . . C3E C 0.553(4) 0.488(4) 0.4071(19) 0.211(19) Uiso 0.50 1 d PD . . C4E C 0.460(3) 0.551(4) 0.4245(14) 0.160(13) Uiso 0.50 1 d PD . . O3E O 0.961(3) 0.704(3) 0.0125(10) 0.147(9) Uiso 0.40 1 d PD . . C5E C 1.014(3) 0.649(3) 0.0533(11) 0.103(8) Uiso 0.40 1 d PD . . C6E C 1.060(6) 0.538(4) 0.063(2) 0.22(3) Uiso 0.40 1 d PD . . O4E O 0.754(3) 0.504(3) 0.0596(12) 0.195(13) Uiso 0.40 1 d PD . . C7E C 0.667(2) 0.577(2) 0.0291(9) 0.076(6) Uiso 0.40 1 d PD . . C8E C 0.645(5) 0.542(5) -0.0068(16) 0.19(2) Uiso 0.40 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb 0.02793(16) 0.03706(17) 0.05136(19) -0.00749(12) 0.00240(11) -0.01336(12) Ni1 0.0260(4) 0.0380(4) 0.0482(4) -0.0072(3) 0.0002(3) -0.0124(3) Ni2 0.0265(4) 0.0393(4) 0.0507(4) -0.0057(3) -0.0007(3) -0.0131(3) O1 0.031(2) 0.037(2) 0.053(2) -0.0105(18) -0.0009(17) -0.0131(17) N1 0.034(3) 0.044(3) 0.053(3) -0.014(2) 0.003(2) -0.011(2) N2 0.034(3) 0.054(3) 0.051(3) -0.004(3) -0.001(2) -0.019(2) O11 0.0256(19) 0.037(2) 0.056(2) -0.0043(18) 0.0014(17) -0.0137(17) N11 0.033(3) 0.058(3) 0.050(3) -0.004(3) 0.002(2) -0.019(2) N12 0.033(3) 0.045(3) 0.067(4) -0.003(3) -0.005(2) -0.012(2) O21 0.0248(19) 0.040(2) 0.052(2) -0.0084(18) -0.0005(17) -0.0118(17) N21 0.030(3) 0.068(4) 0.063(3) -0.019(3) 0.005(2) -0.021(3) N22 0.043(3) 0.049(3) 0.067(4) -0.013(3) 0.012(3) -0.018(3) O31 0.029(2) 0.040(2) 0.053(2) -0.0112(18) 0.0035(17) -0.0157(17) N31 0.031(2) 0.041(3) 0.057(3) -0.004(2) -0.002(2) -0.016(2) N32 0.044(3) 0.046(3) 0.057(3) -0.016(3) 0.000(2) -0.015(2) O41 0.048(3) 0.081(4) 0.106(4) -0.040(3) 0.021(3) -0.040(3) O42 0.055(3) 0.044(3) 0.080(3) -0.013(2) 0.004(3) -0.021(2) O1W 0.065(3) 0.062(3) 0.067(3) 0.000(3) -0.002(3) -0.027(3) C1 0.036(3) 0.055(4) 0.079(5) -0.018(4) 0.001(3) -0.008(3) C2 0.058(5) 0.049(4) 0.106(7) -0.023(4) 0.009(5) 0.000(4) C3 0.072(6) 0.051(5) 0.124(8) -0.035(5) 0.005(5) -0.017(4) C4 0.065(5) 0.056(4) 0.089(6) -0.023(4) 0.004(4) -0.029(4) C5 0.045(4) 0.040(3) 0.055(4) -0.014(3) 0.006(3) -0.017(3) C6 0.038(3) 0.045(3) 0.053(4) -0.014(3) -0.003(3) -0.019(3) O2 0.056(3) 0.069(3) 0.079(4) -0.012(3) -0.004(3) -0.040(3) C7 0.036(3) 0.062(4) 0.045(3) -0.014(3) -0.001(3) -0.024(3) C8 0.052(4) 0.082(5) 0.059(4) -0.028(4) 0.009(3) -0.033(4) C9 0.069(5) 0.108(7) 0.050(4) -0.023(5) 0.003(4) -0.044(5) C10 0.062(5) 0.091(7) 0.056(5) 0.003(4) 0.001(4) -0.032(5) C11 0.049(4) 0.068(5) 0.053(4) 0.001(3) -0.006(3) -0.027(4) C21 0.043(4) 0.073(5) 0.060(4) -0.012(4) 0.004(3) -0.022(4) C22 0.058(5) 0.122(8) 0.056(5) -0.014(5) 0.015(4) -0.043(5) C23 0.087(7) 0.106(8) 0.065(5) 0.005(5) 0.003(5) -0.057(6) C24 0.059(4) 0.075(5) 0.064(5) 0.002(4) 0.003(4) -0.041(4) C25 0.035(3) 0.058(4) 0.056(4) 0.001(3) -0.011(3) -0.027(3) C26 0.036(3) 0.038(3) 0.062(4) -0.003(3) -0.003(3) -0.018(3) O12 0.040(2) 0.056(3) 0.069(3) -0.008(2) -0.002(2) -0.029(2) C27 0.043(4) 0.047(4) 0.072(5) 0.000(3) -0.005(3) -0.021(3) C28 0.060(5) 0.047(4) 0.109(7) 0.004(4) -0.008(5) -0.026(4) C29 0.076(6) 0.048(5) 0.145(10) 0.016(5) -0.015(6) -0.027(4) C30 0.064(5) 0.050(5) 0.108(7) 0.014(5) -0.006(5) -0.008(4) C31 0.046(4) 0.052(4) 0.088(6) 0.005(4) -0.008(4) -0.011(3) C32 0.064(5) 0.067(5) 0.076(5) -0.024(4) 0.013(4) -0.040(4) C33 0.090(7) 0.156(11) 0.093(7) -0.051(7) 0.016(6) -0.081(8) C41 0.045(4) 0.107(7) 0.072(5) -0.031(5) -0.003(4) -0.031(4) C42 0.043(4) 0.107(7) 0.098(7) -0.039(6) -0.007(4) -0.033(5) C43 0.036(4) 0.067(5) 0.109(7) -0.022(5) -0.008(4) -0.024(4) C44 0.031(3) 0.047(4) 0.093(6) -0.011(4) 0.003(3) -0.015(3) C45 0.030(3) 0.035(3) 0.065(4) -0.008(3) -0.003(3) -0.012(2) C46 0.031(3) 0.034(3) 0.064(4) -0.012(3) 0.006(3) -0.012(2) O22 0.035(2) 0.035(2) 0.076(3) -0.013(2) -0.001(2) -0.0123(18) C47 0.033(3) 0.049(4) 0.066(4) -0.012(3) 0.007(3) -0.016(3) C48 0.044(4) 0.063(5) 0.087(6) -0.030(4) 0.024(4) -0.016(4) C49 0.050(4) 0.089(6) 0.089(6) -0.026(5) 0.030(4) -0.024(4) C50 0.082(6) 0.096(7) 0.074(6) -0.020(5) 0.030(5) -0.048(6) C51 0.065(5) 0.065(5) 0.080(6) -0.007(4) 0.025(4) -0.027(4) C52 0.050(4) 0.050(4) 0.095(6) -0.027(4) 0.004(4) -0.020(3) C53 0.100(8) 0.061(5) 0.125(9) -0.033(5) 0.001(6) -0.040(5) C61 0.036(3) 0.065(4) 0.065(4) 0.004(3) -0.001(3) -0.025(3) C62 0.039(4) 0.078(5) 0.090(6) 0.007(4) -0.006(4) -0.033(4) C63 0.034(4) 0.091(6) 0.101(7) -0.003(5) -0.016(4) -0.032(4) C64 0.037(4) 0.082(5) 0.073(5) 0.002(4) -0.015(3) -0.027(4) C65 0.035(3) 0.057(4) 0.060(4) -0.006(3) -0.008(3) -0.022(3) C66 0.034(3) 0.043(3) 0.046(3) 0.003(3) -0.008(2) -0.015(3) O32 0.044(2) 0.044(2) 0.054(3) 0.001(2) -0.003(2) -0.015(2) C67 0.046(4) 0.045(3) 0.053(4) -0.005(3) -0.003(3) -0.023(3) C68 0.065(5) 0.079(5) 0.070(5) -0.019(4) -0.010(4) -0.037(4) C69 0.119(9) 0.100(8) 0.097(8) -0.043(6) -0.014(7) -0.056(7) C70 0.089(7) 0.076(6) 0.088(7) -0.043(5) 0.006(5) -0.026(5) C71 0.061(5) 0.067(5) 0.076(5) -0.029(4) 0.004(4) -0.017(4) C72 0.074(5) 0.047(4) 0.072(5) -0.008(4) 0.010(4) -0.014(4) C73 0.11(3) 0.12(3) 0.092(19) -0.004(16) 0.016(19) 0.03(2) C73A 0.13(3) 0.016(7) 0.13(2) -0.001(9) 0.05(2) 0.009(11) N41 0.076(5) 0.073(4) 0.079(4) -0.020(4) 0.011(4) -0.054(4) O43 0.136(6) 0.096(5) 0.128(6) -0.046(4) 0.021(5) -0.090(5) Cl1 0.0792(15) 0.0936(17) 0.0763(14) -0.0030(12) -0.0023(12) -0.0317(13) O51 0.191(11) 0.131(8) 0.107(6) 0.014(6) 0.055(7) -0.037(7) O52 0.103(7) 0.278(15) 0.118(7) 0.006(8) -0.028(5) -0.104(9) O53 0.125(7) 0.136(8) 0.104(6) 0.026(6) -0.005(5) -0.021(6) O54 0.312(18) 0.134(9) 0.124(8) -0.049(7) 0.033(9) -0.118(11) Cl2 0.190(5) 0.181(4) 0.094(2) -0.003(2) -0.020(3) -0.110(4) O55 0.262(17) 0.210(14) 0.120(9) 0.023(9) -0.014(10) -0.100(13) O56 0.42(3) 0.26(2) 0.31(2) -0.052(18) 0.23(2) -0.17(2) O57 0.60(5) 0.40(3) 0.33(3) -0.03(2) -0.22(3) -0.34(3) O58 0.37(4) 0.184(19) 0.64(5) -0.09(3) -0.30(4) 0.07(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb O31 2.241(4) . ? Tb O21 2.291(4) . ? Tb O1W 2.379(5) . ? Tb O1 2.399(4) . ? Tb O41 2.404(5) . ? Tb O42 2.505(5) . ? Tb N32 2.562(6) . ? Tb N22 2.596(6) . ? Tb N41 2.862(7) . ? Tb Ni2 3.4115(13) . ? Tb Ni1 3.4429(13) . ? Ni1 O11 2.020(4) . ? Ni1 O31 2.033(4) . ? Ni1 N31 2.074(5) . ? Ni1 N1 2.083(5) . ? Ni1 N11 2.089(6) . ? Ni1 O1 2.222(4) . ? Ni2 O21 2.045(4) . ? Ni2 N12 2.066(6) . ? Ni2 O11 2.072(4) . ? Ni2 O1 2.078(4) . ? Ni2 N2 2.094(6) . ? Ni2 N21 2.113(5) . ? O1 C6 1.398(7) . ? N1 C5 1.342(8) . ? N1 C1 1.362(8) . ? N2 C11 1.336(9) . ? N2 C7 1.342(9) . ? O11 C26 1.369(7) . ? N11 C21 1.342(9) . ? N11 C25 1.356(9) . ? N12 C27 1.340(9) . ? N12 C31 1.367(9) . ? O21 C46 1.361(7) . ? N21 C41 1.332(9) . ? N21 C45 1.333(9) . ? N22 C47 1.332(9) . ? N22 C51 1.342(10) . ? O31 C66 1.357(7) . ? N31 C65 1.322(9) . ? N31 C61 1.350(8) . ? N32 C71 1.340(9) . ? N32 C67 1.346(9) . ? O41 N41 1.254(9) . ? O42 N41 1.255(8) . ? C1 C2 1.365(12) . ? C1 H1 0.9300 . ? C2 C3 1.357(13) . ? C2 H2 0.9300 . ? C3 C4 1.393(12) . ? C3 H3 0.9300 . ? C4 C5 1.373(10) . ? C4 H4 0.9300 . ? C5 C6 1.537(9) . ? C6 O2 1.409(8) . ? C6 C7 1.542(9) . ? O2 H2O 0.8200 . ? C7 C8 1.396(10) . ? C8 C9 1.389(12) . ? C8 H8 0.9300 . ? C9 C10 1.371(13) . ? C9 H9 0.9300 . ? C10 C11 1.401(12) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C21 C22 1.402(12) . ? C21 H21 0.9300 . ? C22 C23 1.377(15) . ? C22 H22 0.9300 . ? C23 C24 1.355(13) . ? C23 H23 0.9300 . ? C24 C25 1.371(10) . ? C24 H24 0.9300 . ? C25 C26 1.551(10) . ? C26 O12 1.428(7) . ? C26 C27 1.536(9) . ? O12 C32 1.443(9) . ? C27 C28 1.401(10) . ? C28 C29 1.371(12) . ? C28 H28 0.9300 . ? C29 C30 1.375(14) . ? C29 H29 0.9300 . ? C30 C31 1.387(12) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.463(11) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C41 C42 1.373(11) . ? C41 H41 0.9300 . ? C42 C43 1.359(13) . ? C42 H42 0.9300 . ? C43 C44 1.365(11) . ? C43 H43 0.9300 . ? C44 C45 1.383(9) . ? C44 H44 0.9300 . ? C45 C46 1.535(9) . ? C46 O22 1.449(7) . ? C46 C47 1.533(10) . ? O22 C52 1.435(9) . ? C47 C48 1.394(9) . ? C48 C49 1.361(12) . ? C48 H48 0.9300 . ? C49 C50 1.380(14) . ? C49 H49 0.9300 . ? C50 C51 1.367(12) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 C53 1.505(12) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C61 C62 1.375(10) . ? C61 H61 0.9300 . ? C62 C63 1.347(12) . ? C62 H62 0.9300 . ? C63 C64 1.395(11) . ? C63 H63 0.9300 . ? C64 C65 1.399(9) . ? C64 H64 0.9300 . ? C65 C66 1.545(9) . ? C66 O32 1.434(7) . ? C66 C67 1.533(9) . ? O32 C72 1.433(9) . ? C67 C68 1.394(10) . ? C68 C69 1.409(14) . ? C68 H68 0.9300 . ? C69 C70 1.341(15) . ? C69 H69 0.9300 . ? C70 C71 1.386(12) . ? C70 H70 0.9300 . ? C71 H71 0.9300 . ? C72 C73A 1.50(3) . ? C72 C73 1.55(4) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? N41 O43 1.226(8) . ? Cl1 O51 1.404(9) . ? Cl1 O53 1.411(9) . ? Cl1 O54 1.416(10) . ? Cl1 O52 1.440(9) . ? Cl2 O57 1.278(14) . ? Cl2 O55 1.382(12) . ? Cl2 O56 1.40(2) . ? Cl2 O58 1.50(2) . ? O1E C1E 1.28(2) . ? C1E C2E 1.22(3) . ? O2E C3E 1.27(2) . ? C3E C4E 1.17(3) . ? O3E C5E 1.21(2) . ? C5E C6E 1.19(3) . ? O4E C7E 1.23(2) . ? C7E C8E 1.19(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O31 Tb O21 109.49(15) . . ? O31 Tb O1W 92.80(17) . . ? O21 Tb O1W 138.24(17) . . ? O31 Tb O1 71.57(14) . . ? O21 Tb O1 72.15(14) . . ? O1W Tb O1 149.60(17) . . ? O31 Tb O41 133.22(17) . . ? O21 Tb O41 104.50(19) . . ? O1W Tb O41 82.1(2) . . ? O1 Tb O41 89.91(18) . . ? O31 Tb O42 81.86(16) . . ? O21 Tb O42 140.17(16) . . ? O1W Tb O42 75.96(19) . . ? O1 Tb O42 76.10(16) . . ? O41 Tb O42 51.69(18) . . ? O31 Tb N32 65.01(16) . . ? O21 Tb N32 83.88(17) . . ? O1W Tb N32 74.0(2) . . ? O1 Tb N32 118.83(17) . . ? O41 Tb N32 151.2(2) . . ? O42 Tb N32 133.35(18) . . ? O31 Tb N22 151.23(18) . . ? O21 Tb N22 64.65(17) . . ? O1W Tb N22 78.71(19) . . ? O1 Tb N22 126.94(17) . . ? O41 Tb N22 73.32(19) . . ? O42 Tb N22 121.54(18) . . ? N32 Tb N22 86.22(19) . . ? O31 Tb N41 107.62(18) . . ? O21 Tb N41 124.01(19) . . ? O1W Tb N41 78.3(2) . . ? O1 Tb N41 81.81(17) . . ? O41 Tb N41 25.73(19) . . ? O42 Tb N41 25.97(19) . . ? N32 Tb N41 150.8(2) . . ? N22 Tb N41 97.6(2) . . ? O31 Tb Ni2 87.32(11) . . ? O21 Tb Ni2 35.64(10) . . ? O1W Tb Ni2 172.46(14) . . ? O1 Tb Ni2 36.98(10) . . ? O41 Tb Ni2 103.31(16) . . ? O42 Tb Ni2 111.49(13) . . ? N32 Tb Ni2 99.30(14) . . ? N22 Tb Ni2 97.63(14) . . ? N41 Tb Ni2 108.82(15) . . ? O31 Tb Ni1 34.34(11) . . ? O21 Tb Ni1 83.72(10) . . ? O1W Tb Ni1 126.78(14) . . ? O1 Tb Ni1 39.90(10) . . ? O41 Tb Ni1 124.72(14) . . ? O42 Tb Ni1 87.16(12) . . ? N32 Tb Ni1 83.19(14) . . ? N22 Tb Ni1 147.54(13) . . ? N41 Tb Ni1 106.53(14) . . ? Ni2 Tb Ni1 54.39(3) . . ? O11 Ni1 O31 97.50(17) . . ? O11 Ni1 N31 106.20(19) . . ? O31 Ni1 N31 78.93(19) . . ? O11 Ni1 N1 153.95(19) . . ? O31 Ni1 N1 90.0(2) . . ? N31 Ni1 N1 99.7(2) . . ? O11 Ni1 N11 78.3(2) . . ? O31 Ni1 N11 169.9(2) . . ? N31 Ni1 N11 93.4(2) . . ? N1 Ni1 N11 97.8(2) . . ? O11 Ni1 O1 79.43(15) . . ? O31 Ni1 O1 79.22(16) . . ? N31 Ni1 O1 157.97(19) . . ? N1 Ni1 O1 77.50(18) . . ? N11 Ni1 O1 108.67(18) . . ? O11 Ni1 Tb 76.96(12) . . ? O31 Ni1 Tb 38.45(11) . . ? N31 Ni1 Tb 115.67(16) . . ? N1 Ni1 Tb 94.36(15) . . ? N11 Ni1 Tb 146.05(15) . . ? O1 Ni1 Tb 43.84(11) . . ? O21 Ni2 N12 105.5(2) . . ? O21 Ni2 O11 87.17(16) . . ? N12 Ni2 O11 79.23(19) . . ? O21 Ni2 O1 84.15(17) . . ? N12 Ni2 O1 158.07(19) . . ? O11 Ni2 O1 81.72(16) . . ? O21 Ni2 N2 157.7(2) . . ? N12 Ni2 N2 96.0(2) . . ? O11 Ni2 N2 102.75(19) . . ? O1 Ni2 N2 77.7(2) . . ? O21 Ni2 N21 77.5(2) . . ? N12 Ni2 N21 97.4(2) . . ? O11 Ni2 N21 162.9(2) . . ? O1 Ni2 N21 103.9(2) . . ? N2 Ni2 N21 94.3(2) . . ? O21 Ni2 Tb 40.74(11) . . ? N12 Ni2 Tb 139.11(17) . . ? O11 Ni2 Tb 77.19(12) . . ? O1 Ni2 Tb 43.99(12) . . ? N2 Ni2 Tb 121.52(16) . . ? N21 Ni2 Tb 95.51(18) . . ? C6 O1 Ni2 116.0(4) . . ? C6 O1 Ni1 105.7(3) . . ? Ni2 O1 Ni1 93.47(16) . . ? C6 O1 Tb 136.7(4) . . ? Ni2 O1 Tb 99.03(16) . . ? Ni1 O1 Tb 96.26(15) . . ? C5 N1 C1 118.8(6) . . ? C5 N1 Ni1 114.7(4) . . ? C1 N1 Ni1 125.5(5) . . ? C11 N2 C7 118.4(6) . . ? C11 N2 Ni2 126.0(5) . . ? C7 N2 Ni2 115.6(4) . . ? C26 O11 Ni1 115.6(4) . . ? C26 O11 Ni2 111.2(4) . . ? Ni1 O11 Ni2 99.91(18) . . ? C21 N11 C25 118.1(6) . . ? C21 N11 Ni1 127.2(5) . . ? C25 N11 Ni1 114.6(5) . . ? C27 N12 C31 119.3(6) . . ? C27 N12 Ni2 113.3(4) . . ? C31 N12 Ni2 127.3(5) . . ? C46 O21 Ni2 113.8(4) . . ? C46 O21 Tb 126.9(4) . . ? Ni2 O21 Tb 103.62(17) . . ? C41 N21 C45 118.9(6) . . ? C41 N21 Ni2 126.9(5) . . ? C45 N21 Ni2 114.1(4) . . ? C47 N22 C51 117.5(6) . . ? C47 N22 Tb 116.2(4) . . ? C51 N22 Tb 126.3(5) . . ? C66 O31 Ni1 116.8(4) . . ? C66 O31 Tb 125.6(4) . . ? Ni1 O31 Tb 107.21(18) . . ? C65 N31 C61 118.5(6) . . ? C65 N31 Ni1 114.7(4) . . ? C61 N31 Ni1 126.3(5) . . ? C71 N32 C67 117.2(6) . . ? C71 N32 Tb 126.6(5) . . ? C67 N32 Tb 116.2(4) . . ? N41 O41 Tb 98.0(4) . . ? N41 O42 Tb 93.1(4) . . ? N1 C1 C2 121.1(7) . . ? N1 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C3 C2 C1 120.5(8) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 118.8(8) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 119.0(8) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? N1 C5 C4 121.8(6) . . ? N1 C5 C6 115.4(5) . . ? C4 C5 C6 122.8(6) . . ? O1 C6 O2 111.2(5) . . ? O1 C6 C5 108.9(5) . . ? O2 C6 C5 106.9(5) . . ? O1 C6 C7 109.0(5) . . ? O2 C6 C7 110.3(5) . . ? C5 C6 C7 110.5(5) . . ? C6 O2 H2O 109.5 . . ? N2 C7 C8 122.4(7) . . ? N2 C7 C6 116.1(5) . . ? C8 C7 C6 121.5(7) . . ? C9 C8 C7 118.2(8) . . ? C9 C8 H8 120.9 . . ? C7 C8 H8 120.9 . . ? C10 C9 C8 120.0(8) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 118.1(8) . . ? C9 C10 H10 120.9 . . ? C11 C10 H10 120.9 . . ? N2 C11 C10 122.8(8) . . ? N2 C11 H11 118.6 . . ? C10 C11 H11 118.6 . . ? N11 C21 C22 121.5(8) . . ? N11 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C23 C22 C21 119.1(8) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C24 C23 C22 119.2(9) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C23 C24 C25 120.0(9) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? N11 C25 C24 122.3(7) . . ? N11 C25 C26 113.5(6) . . ? C24 C25 C26 124.2(7) . . ? O11 C26 O12 113.3(5) . . ? O11 C26 C27 109.3(5) . . ? O12 C26 C27 110.1(5) . . ? O11 C26 C25 110.6(5) . . ? O12 C26 C25 103.4(5) . . ? C27 C26 C25 109.9(6) . . ? C26 O12 C32 114.4(5) . . ? N12 C27 C28 121.2(7) . . ? N12 C27 C26 115.4(6) . . ? C28 C27 C26 123.4(6) . . ? C29 C28 C27 119.6(8) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 119.1(8) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C29 C30 C31 120.0(8) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? N12 C31 C30 120.7(8) . . ? N12 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? O12 C32 C33 108.8(7) . . ? O12 C32 H32A 109.9 . . ? C33 C32 H32A 109.9 . . ? O12 C32 H32B 109.9 . . ? C33 C32 H32B 109.9 . . ? H32A C32 H32B 108.3 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N21 C41 C42 122.1(8) . . ? N21 C41 H41 119.0 . . ? C42 C41 H41 119.0 . . ? C43 C42 C41 119.6(8) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C42 C43 C44 118.5(7) . . ? C42 C43 H43 120.7 . . ? C44 C43 H43 120.7 . . ? C43 C44 C45 120.0(8) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? N21 C45 C44 120.9(7) . . ? N21 C45 C46 114.3(5) . . ? C44 C45 C46 124.8(7) . . ? O21 C46 O22 112.4(5) . . ? O21 C46 C47 110.4(5) . . ? O22 C46 C47 110.0(5) . . ? O21 C46 C45 109.7(5) . . ? O22 C46 C45 101.4(5) . . ? C47 C46 C45 112.6(5) . . ? C52 O22 C46 114.2(5) . . ? N22 C47 C48 121.7(7) . . ? N22 C47 C46 116.1(5) . . ? C48 C47 C46 122.3(7) . . ? C49 C48 C47 120.0(8) . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C48 C49 C50 118.4(8) . . ? C48 C49 H49 120.8 . . ? C50 C49 H49 120.8 . . ? C51 C50 C49 118.7(9) . . ? C51 C50 H50 120.6 . . ? C49 C50 H50 120.6 . . ? N22 C51 C50 123.6(9) . . ? N22 C51 H51 118.2 . . ? C50 C51 H51 118.2 . . ? O22 C52 C53 107.6(7) . . ? O22 C52 H52A 110.2 . . ? C53 C52 H52A 110.2 . . ? O22 C52 H52B 110.2 . . ? C53 C52 H52B 110.2 . . ? H52A C52 H52B 108.5 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N31 C61 C62 122.6(7) . . ? N31 C61 H61 118.7 . . ? C62 C61 H61 118.7 . . ? C63 C62 C61 118.7(7) . . ? C63 C62 H62 120.7 . . ? C61 C62 H62 120.7 . . ? C62 C63 C64 120.5(7) . . ? C62 C63 H63 119.8 . . ? C64 C63 H63 119.8 . . ? C63 C64 C65 117.3(8) . . ? C63 C64 H64 121.3 . . ? C65 C64 H64 121.3 . . ? N31 C65 C64 122.4(7) . . ? N31 C65 C66 115.8(5) . . ? C64 C65 C66 121.8(6) . . ? O31 C66 O32 112.7(5) . . ? O31 C66 C67 110.3(5) . . ? O32 C66 C67 101.6(5) . . ? O31 C66 C65 109.7(5) . . ? O32 C66 C65 109.0(5) . . ? C67 C66 C65 113.5(5) . . ? C72 O32 C66 113.9(5) . . ? N32 C67 C68 122.0(7) . . ? N32 C67 C66 113.9(5) . . ? C68 C67 C66 124.0(6) . . ? C67 C68 C69 118.9(8) . . ? C67 C68 H68 120.6 . . ? C69 C68 H68 120.6 . . ? C70 C69 C68 118.8(9) . . ? C70 C69 H69 120.6 . . ? C68 C69 H69 120.6 . . ? C69 C70 C71 119.2(9) . . ? C69 C70 H70 120.4 . . ? C71 C70 H70 120.4 . . ? N32 C71 C70 124.0(8) . . ? N32 C71 H71 118.0 . . ? C70 C71 H71 118.0 . . ? O32 C72 C73A 105.8(13) . . ? O32 C72 C73 111.0(18) . . ? C73A C72 C73 26(2) . . ? O32 C72 H72A 109.4 . . ? C73A C72 H72A 88.4 . . ? C73 C72 H72A 109.4 . . ? O32 C72 H72B 109.4 . . ? C73A C72 H72B 132.6 . . ? C73 C72 H72B 109.4 . . ? H72A C72 H72B 108.0 . . ? O43 N41 O41 122.8(7) . . ? O43 N41 O42 120.0(8) . . ? O41 N41 O42 117.2(6) . . ? O43 N41 Tb 177.8(7) . . ? O41 N41 Tb 56.3(3) . . ? O42 N41 Tb 61.0(3) . . ? O51 Cl1 O53 112.9(6) . . ? O51 Cl1 O54 115.4(8) . . ? O53 Cl1 O54 107.7(7) . . ? O51 Cl1 O52 107.7(7) . . ? O53 Cl1 O52 107.1(7) . . ? O54 Cl1 O52 105.4(9) . . ? O57 Cl2 O55 119.3(15) . . ? O57 Cl2 O56 117.5(18) . . ? O55 Cl2 O56 115.0(14) . . ? O57 Cl2 O58 102.8(18) . . ? O55 Cl2 O58 98.6(16) . . ? O56 Cl2 O58 97.3(19) . . ? C2E C1E O1E 117(3) . . ? C4E C3E O2E 117(3) . . ? C6E C5E O3E 121(3) . . ? C8E C7E O4E 120(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.046 _refine_diff_density_min -1.907 _refine_diff_density_rms 0.137 # Attachment '- peng50.cif' data_peng50 _database_code_depnum_ccdc_archive 'CCDC 778582' #TrackingRef '- peng50.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54.60 H63.80 Cl2 Gd N9 Ni2 O22.30' _chemical_formula_weight 1548.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.981(6) _cell_length_b 12.089(6) _cell_length_c 26.960(10) _cell_angle_alpha 81.34(2) _cell_angle_beta 89.48(2) _cell_angle_gamma 63.37(2) _cell_volume 3443(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11 _cell_measurement_theta_max 27 _exptl_crystal_description parallelepiped _exptl_crystal_colour green-blue _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1574 _exptl_absorpt_coefficient_mu 8.148 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'P21 Nicolet upgraded by Crystal Logic' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.6 _diffrn_reflns_number 10211 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 58.44 _reflns_number_total 9671 _reflns_number_gt 8556 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1475P)^2^+3.4543P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0035(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9671 _refine_ls_number_parameters 824 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.1989 _refine_ls_wR_factor_gt 0.1865 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Gd Gd 0.43255(3) 0.11181(4) 0.696921(14) 0.0507(2) Uani 1 1 d . . . Ni1 Ni 0.21993(10) 0.07757(10) 0.77717(4) 0.0491(3) Uani 1 1 d . . . Ni2 Ni 0.50363(10) -0.10792(11) 0.80306(4) 0.0505(3) Uani 1 1 d . . . O1 O 0.4003(4) 0.0849(4) 0.78569(17) 0.0501(10) Uani 1 1 d . . . N1 N 0.1649(6) 0.2494(6) 0.8002(2) 0.0565(14) Uani 1 1 d . . . N2 N 0.4521(6) -0.0563(6) 0.8739(2) 0.0567(14) Uani 1 1 d . . . O11 O 0.3420(4) -0.1007(4) 0.77273(17) 0.0495(10) Uani 1 1 d . . . N11 N 0.1963(5) -0.0204(6) 0.8442(2) 0.0592(15) Uani 1 1 d . . . N12 N 0.5384(6) -0.2928(6) 0.8231(2) 0.0603(15) Uani 1 1 d . . . O21 O 0.5584(4) -0.0955(4) 0.73085(18) 0.0529(11) Uani 1 1 d . . . N21 N 0.6874(6) -0.1356(6) 0.8142(2) 0.0628(16) Uani 1 1 d . . . N22 N 0.6406(6) 0.0030(6) 0.6555(2) 0.0647(16) Uani 1 1 d . . . O31 O 0.2301(4) 0.1555(4) 0.70600(17) 0.0507(10) Uani 1 1 d . . . N31 N 0.0521(6) 0.1082(6) 0.7435(2) 0.0566(14) Uani 1 1 d . . . N32 N 0.3427(6) 0.0168(6) 0.6389(2) 0.0597(15) Uani 1 1 d . . . O41 O 0.5517(6) 0.2231(7) 0.7103(3) 0.0824(18) Uani 1 1 d . . . O42 O 0.3545(6) 0.3291(5) 0.7168(2) 0.0724(15) Uani 1 1 d . . . OW1 O 0.3886(6) 0.2428(6) 0.6163(2) 0.0798(16) Uani 1 1 d . . . C1 C 0.0510(8) 0.3464(9) 0.7932(3) 0.071(2) Uani 1 1 d . . . H1 H -0.0147 0.3339 0.7816 0.093 Uiso 1 1 calc R . . C2 C 0.0261(10) 0.4624(9) 0.8020(4) 0.090(3) Uani 1 1 d . . . H2 H -0.0546 0.5280 0.7963 0.117 Uiso 1 1 calc R . . C3 C 0.1229(10) 0.4813(9) 0.8197(5) 0.093(3) Uani 1 1 d . . . H3 H 0.1084 0.5601 0.8259 0.120 Uiso 1 1 calc R . . C4 C 0.2399(9) 0.3834(8) 0.8280(4) 0.079(2) Uani 1 1 d . . . H4 H 0.3059 0.3941 0.8405 0.103 Uiso 1 1 calc R . . C5 C 0.2596(7) 0.2674(7) 0.8175(3) 0.0596(18) Uani 1 1 d . . . C6 C 0.3882(7) 0.1513(7) 0.8245(3) 0.0552(16) Uani 1 1 d . . . O2 O 0.4795(5) 0.1955(6) 0.8244(2) 0.0705(14) Uani 1 1 d . . . C7 C 0.4020(7) 0.0658(8) 0.8747(3) 0.0583(18) Uani 1 1 d . . . C8 C 0.3626(9) 0.1136(10) 0.9194(3) 0.079(2) Uani 1 1 d . . . H8 H 0.3293 0.1994 0.9195 0.103 Uiso 1 1 calc R . . C9 C 0.3732(9) 0.0342(11) 0.9629(3) 0.082(3) Uani 1 1 d . . . H9 H 0.3451 0.0649 0.9926 0.107 Uiso 1 1 calc R . . C10 C 0.4270(9) -0.0935(11) 0.9615(3) 0.082(3) Uani 1 1 d . . . H10 H 0.4376 -0.1504 0.9906 0.107 Uiso 1 1 calc R . . C11 C 0.4643(8) -0.1345(9) 0.9168(3) 0.070(2) Uani 1 1 d . . . H11 H 0.4995 -0.2202 0.9161 0.091 Uiso 1 1 calc R . . C21 C 0.1306(8) 0.0316(9) 0.8828(3) 0.070(2) Uani 1 1 d . . . H21 H 0.0965 0.1179 0.8817 0.091 Uiso 1 1 calc R . . C22 C 0.1131(10) -0.0415(13) 0.9240(3) 0.093(3) Uani 1 1 d . . . H22 H 0.0689 -0.0049 0.9505 0.121 Uiso 1 1 calc R . . C23 C 0.1629(10) -0.1712(12) 0.9252(4) 0.091(3) Uani 1 1 d . . . H23 H 0.1533 -0.2226 0.9525 0.118 Uiso 1 1 calc R . . C24 C 0.2265(8) -0.2202(9) 0.8847(3) 0.076(2) Uani 1 1 d . . . H24 H 0.2592 -0.3058 0.8843 0.099 Uiso 1 1 calc R . . C25 C 0.2421(7) -0.1437(7) 0.8451(3) 0.0581(17) Uani 1 1 d . . . C26 C 0.3159(7) -0.1912(7) 0.7991(3) 0.0597(18) Uani 1 1 d . . . O12 O 0.2323(5) -0.2189(5) 0.7717(2) 0.0618(12) Uani 1 1 d . . . C27 C 0.4379(7) -0.3103(7) 0.8157(3) 0.0621(19) Uani 1 1 d . . . C28 C 0.4450(10) -0.4294(8) 0.8225(4) 0.086(3) Uani 1 1 d . . . H28 H 0.3749 -0.4401 0.8156 0.112 Uiso 1 1 calc R . . C29 C 0.5573(11) -0.5314(10) 0.8394(5) 0.109(4) Uani 1 1 d . . . H29 H 0.5636 -0.6119 0.8445 0.141 Uiso 1 1 calc R . . C30 C 0.6604(10) -0.5132(9) 0.8488(5) 0.093(3) Uani 1 1 d . . . H30 H 0.7368 -0.5807 0.8607 0.120 Uiso 1 1 calc R . . C31 C 0.6473(8) -0.3925(9) 0.8400(4) 0.078(2) Uani 1 1 d . . . H31 H 0.7167 -0.3797 0.8460 0.101 Uiso 1 1 calc R . . C32 C 0.2719(8) -0.2482(9) 0.7227(3) 0.073(2) Uani 1 1 d . . . H32A H 0.3526 -0.3218 0.7259 0.095 Uiso 1 1 calc R . . H32B H 0.2799 -0.1786 0.7028 0.095 Uiso 1 1 calc R . . C33 C 0.1768(12) -0.2721(14) 0.6983(5) 0.109(4) Uani 1 1 d . . . H33A H 0.2024 -0.2942 0.6659 0.141 Uiso 1 1 calc R . . H33B H 0.0980 -0.1978 0.6944 0.141 Uiso 1 1 calc R . . H33C H 0.1682 -0.3397 0.7187 0.141 Uiso 1 1 calc R . . C41 C 0.7441(9) -0.1349(10) 0.8579(4) 0.087(3) Uani 1 1 d . . . H41 H 0.6988 -0.1197 0.8864 0.113 Uiso 1 1 calc R . . C42 C 0.8669(9) -0.1562(11) 0.8603(4) 0.093(3) Uani 1 1 d . . . H42 H 0.9045 -0.1576 0.8906 0.121 Uiso 1 1 calc R . . C43 C 0.9341(8) -0.1753(9) 0.8185(4) 0.079(2) Uani 1 1 d . . . H43 H 1.0171 -0.1896 0.8200 0.103 Uiso 1 1 calc R . . C44 C 0.8770(7) -0.1729(8) 0.7742(4) 0.067(2) Uani 1 1 d . . . H44 H 0.9199 -0.1832 0.7450 0.088 Uiso 1 1 calc R . . C45 C 0.7530(7) -0.1548(6) 0.7736(3) 0.0545(16) Uani 1 1 d . . . C46 C 0.6837(6) -0.1605(6) 0.7279(3) 0.0520(16) Uani 1 1 d . . . O22 O 0.7235(5) -0.2933(5) 0.7318(2) 0.0614(13) Uani 1 1 d . . . C47 C 0.7226(7) -0.1127(7) 0.6776(3) 0.0594(18) Uani 1 1 d . . . C48 C 0.8339(8) -0.1846(9) 0.6575(4) 0.075(2) Uani 1 1 d . . . H48 H 0.8863 -0.2656 0.6735 0.097 Uiso 1 1 calc R . . C49 C 0.8660(10) -0.1353(11) 0.6139(4) 0.087(3) Uani 1 1 d . . . H49 H 0.9407 -0.1826 0.6002 0.114 Uiso 1 1 calc R . . C50 C 0.7882(11) -0.0161(11) 0.5906(4) 0.094(3) Uani 1 1 d . . . H50 H 0.8095 0.0198 0.5614 0.122 Uiso 1 1 calc R . . C51 C 0.6748(9) 0.0503(9) 0.6122(4) 0.079(2) Uani 1 1 d . . . H51 H 0.6204 0.1305 0.5961 0.103 Uiso 1 1 calc R . . C52 C 0.6531(9) -0.3273(9) 0.6992(4) 0.076(2) Uani 1 1 d . . . H52A H 0.6601 -0.2984 0.6643 0.11(4) Uiso 1 1 calc R . . H52B H 0.5653 -0.2891 0.7061 0.12(4) Uiso 1 1 calc R . . C53 C 0.7060(12) -0.4672(10) 0.7089(5) 0.096(3) Uani 1 1 d . . . H53A H 0.7095 -0.4957 0.7443 0.09(4) Uiso 1 1 calc R . . H53B H 0.7887 -0.5037 0.6972 0.16(6) Uiso 1 1 calc R . . H53C H 0.6536 -0.4919 0.6914 0.18(7) Uiso 1 1 calc R . . C61 C -0.0464(8) 0.1056(8) 0.7670(3) 0.069(2) Uani 1 1 d . . . H61 H -0.0363 0.0764 0.8014 0.090 Uiso 1 1 calc R . . C62 C -0.1608(8) 0.1440(9) 0.7428(4) 0.078(2) Uani 1 1 d . . . H62 H -0.2263 0.1391 0.7601 0.101 Uiso 1 1 calc R . . C63 C -0.1763(8) 0.1899(9) 0.6921(4) 0.081(3) Uani 1 1 d . . . H63 H -0.2531 0.2176 0.6747 0.106 Uiso 1 1 calc R . . C64 C -0.0781(8) 0.1945(10) 0.6677(3) 0.077(2) Uani 1 1 d . . . H64 H -0.0875 0.2257 0.6335 0.100 Uiso 1 1 calc R . . C65 C 0.0361(6) 0.1525(7) 0.6941(3) 0.0564(17) Uani 1 1 d . . . C66 C 0.1494(7) 0.1579(7) 0.6702(3) 0.0549(16) Uani 1 1 d . . . O32 O 0.1072(5) 0.2701(5) 0.63296(19) 0.0620(12) Uani 1 1 d . B . C67 C 0.2181(8) 0.0549(7) 0.6379(3) 0.0611(18) Uani 1 1 d . . . C68 C 0.1576(10) 0.0146(9) 0.6082(4) 0.082(3) Uani 1 1 d . . . H68 H 0.0712 0.0455 0.6077 0.107 Uiso 1 1 calc R . . C69 C 0.2285(13) -0.0741(11) 0.5785(4) 0.101(3) Uani 1 1 d . . . H69 H 0.1907 -0.1070 0.5591 0.132 Uiso 1 1 calc R . . C70 C 0.3515(12) -0.1113(10) 0.5783(4) 0.096(3) Uani 1 1 d . . . H70 H 0.4000 -0.1682 0.5578 0.124 Uiso 1 1 calc R . . C71 C 0.4064(9) -0.0639(9) 0.6090(4) 0.081(3) Uani 1 1 d . . . H71 H 0.4922 -0.0903 0.6084 0.105 Uiso 1 1 calc R . . C72 C 0.0561(10) 0.3849(8) 0.6532(4) 0.084(3) Uani 1 1 d . . . H72A H 0.1237 0.3945 0.6684 0.11(4) Uiso 1 1 calc R A 1 H72B H 0.0013 0.3807 0.6794 0.09(3) Uiso 1 1 calc R A 1 C73 C -0.017(4) 0.498(4) 0.6131(14) 0.16(2) Uani 0.50 1 d P B 1 C73A C 0.042(5) 0.484(2) 0.6104(19) 0.16(2) Uani 0.50 1 d P B 2 N41 N 0.4625(8) 0.3221(8) 0.7200(3) 0.079(2) Uani 1 1 d . . . O43 O 0.4777(9) 0.4095(9) 0.7311(4) 0.122(3) Uani 1 1 d . . . Cl1 Cl 0.2541(3) 0.8619(3) 0.07882(9) 0.0949(7) Uani 1 1 d . . . O51 O 0.2033(11) 0.8484(11) 0.1248(4) 0.158(4) Uani 1 1 d . . . O52 O 0.3724(10) 0.8618(16) 0.0879(4) 0.180(6) Uani 1 1 d . . . O53 O 0.1767(10) 0.9769(11) 0.0481(4) 0.150(4) Uani 1 1 d . . . O54 O 0.2778(17) 0.7634(12) 0.0516(5) 0.189(6) Uani 1 1 d . . . Cl2 Cl 0.1240(6) 0.7306(5) 0.49735(14) 0.1547(17) Uani 1 1 d . . . O55 O 0.1430(17) 0.6908(17) 0.5474(5) 0.214(7) Uani 1 1 d . . . O56 O 0.218(3) 0.751(3) 0.4767(10) 0.349(17) Uani 1 1 d . . . O57 O 0.070(4) 0.686(3) 0.4708(10) 0.40(2) Uani 1 1 d . . . O58 O 0.030(3) 0.869(2) 0.4975(11) 0.37(2) Uani 1 1 d . . . O1E O 0.2319(10) 0.2475(11) 0.5426(5) 0.140(3) Uiso 1 1 d D . . C1E C 0.222(3) 0.277(4) 0.4947(11) 0.292(17) Uiso 1 1 d D . . C2E C 0.321(4) 0.256(4) 0.4749(13) 0.281(16) Uiso 1 1 d D . . O2E O 0.6338(19) 0.5230(19) 0.4054(8) 0.129(6) Uiso 0.50 1 d PD . . C3E C 0.557(4) 0.477(4) 0.407(2) 0.199(18) Uiso 0.50 1 d PD . . C4E C 0.455(3) 0.543(4) 0.4184(16) 0.161(13) Uiso 0.50 1 d PD . . O3E O 0.957(3) 0.710(3) 0.0136(13) 0.173(12) Uiso 0.40 1 d PD . . C5E C 1.016(4) 0.652(4) 0.0539(14) 0.127(11) Uiso 0.40 1 d PD . . C6E C 1.063(6) 0.539(4) 0.063(2) 0.22(3) Uiso 0.40 1 d PD . . O4E O 0.750(3) 0.505(4) 0.0634(13) 0.196(14) Uiso 0.40 1 d PD . . C7E C 0.669(3) 0.576(2) 0.0295(10) 0.087(7) Uiso 0.40 1 d PD . . C8E C 0.601(6) 0.540(6) 0.012(2) 0.24(3) Uiso 0.40 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd 0.0502(3) 0.0508(3) 0.0490(3) -0.00862(17) 0.00517(17) -0.0210(2) Ni1 0.0464(6) 0.0516(6) 0.0457(6) -0.0089(5) 0.0026(5) -0.0188(5) Ni2 0.0469(6) 0.0531(7) 0.0480(6) -0.0068(5) 0.0014(5) -0.0199(5) O1 0.054(3) 0.049(3) 0.047(2) -0.010(2) 0.005(2) -0.023(2) N1 0.052(3) 0.052(3) 0.058(3) -0.018(3) 0.009(3) -0.013(3) N2 0.053(3) 0.062(4) 0.050(3) -0.006(3) 0.003(3) -0.022(3) O11 0.050(2) 0.049(3) 0.048(2) -0.001(2) 0.003(2) -0.024(2) N11 0.048(3) 0.075(4) 0.047(3) -0.006(3) 0.006(3) -0.023(3) N12 0.050(3) 0.052(3) 0.064(4) 0.000(3) 0.002(3) -0.013(3) O21 0.046(2) 0.051(3) 0.056(3) -0.010(2) 0.005(2) -0.017(2) N21 0.061(4) 0.071(4) 0.057(4) -0.021(3) 0.004(3) -0.028(3) N22 0.067(4) 0.070(4) 0.058(4) -0.012(3) 0.017(3) -0.032(3) O31 0.052(3) 0.052(3) 0.046(2) -0.010(2) 0.002(2) -0.022(2) N31 0.055(3) 0.055(3) 0.055(4) 0.000(3) -0.002(3) -0.024(3) N32 0.065(4) 0.060(4) 0.056(4) -0.015(3) -0.008(3) -0.027(3) O41 0.069(4) 0.095(5) 0.110(5) -0.040(4) 0.022(3) -0.054(4) O42 0.074(4) 0.054(3) 0.086(4) -0.017(3) 0.007(3) -0.024(3) OW1 0.089(4) 0.081(4) 0.063(3) 0.004(3) 0.002(3) -0.038(3) C1 0.071(5) 0.073(6) 0.068(5) -0.019(4) 0.008(4) -0.027(5) C2 0.078(6) 0.061(5) 0.112(8) -0.026(5) 0.019(6) -0.010(5) C3 0.099(7) 0.056(5) 0.120(9) -0.029(5) 0.017(6) -0.028(5) C4 0.079(6) 0.067(5) 0.094(7) -0.026(5) 0.007(5) -0.032(5) C5 0.066(5) 0.062(4) 0.052(4) -0.020(3) 0.009(3) -0.027(4) C6 0.060(4) 0.065(4) 0.047(4) -0.016(3) 0.007(3) -0.032(4) O2 0.071(3) 0.081(4) 0.077(4) -0.019(3) 0.006(3) -0.048(3) C7 0.054(4) 0.076(5) 0.046(4) -0.017(4) 0.000(3) -0.028(4) C8 0.078(6) 0.096(7) 0.064(5) -0.028(5) 0.005(4) -0.036(5) C9 0.086(6) 0.123(9) 0.043(4) -0.019(5) 0.004(4) -0.050(6) C10 0.077(6) 0.107(8) 0.048(5) 0.004(5) -0.004(4) -0.033(5) C11 0.073(5) 0.082(6) 0.050(4) 0.007(4) -0.008(4) -0.036(4) C21 0.060(4) 0.088(6) 0.061(5) -0.020(4) 0.008(4) -0.031(4) C22 0.089(7) 0.154(11) 0.047(5) -0.011(6) 0.014(4) -0.065(7) C23 0.099(7) 0.113(9) 0.070(6) 0.005(6) 0.001(5) -0.061(7) C24 0.078(5) 0.082(6) 0.063(5) 0.015(4) 0.001(4) -0.040(5) C25 0.055(4) 0.064(5) 0.056(4) -0.004(3) 0.001(3) -0.029(4) C26 0.060(4) 0.059(4) 0.060(4) -0.004(3) -0.007(3) -0.028(4) O12 0.061(3) 0.062(3) 0.069(3) -0.012(3) 0.003(2) -0.034(3) C27 0.053(4) 0.057(4) 0.071(5) -0.004(4) 0.003(4) -0.022(3) C28 0.088(6) 0.059(5) 0.108(8) 0.011(5) -0.002(5) -0.037(5) C29 0.094(8) 0.063(6) 0.148(11) 0.017(6) -0.003(7) -0.028(6) C30 0.077(6) 0.064(6) 0.110(8) 0.016(5) -0.006(6) -0.018(5) C31 0.064(5) 0.076(6) 0.077(6) 0.003(5) -0.006(4) -0.022(4) C32 0.072(5) 0.081(6) 0.079(6) -0.024(5) 0.015(4) -0.042(5) C33 0.109(8) 0.161(12) 0.097(8) -0.050(8) 0.013(6) -0.088(9) C41 0.067(5) 0.105(7) 0.081(6) -0.031(6) -0.008(5) -0.028(5) C42 0.061(5) 0.125(8) 0.104(8) -0.048(7) -0.012(5) -0.044(5) C43 0.057(5) 0.077(6) 0.107(7) -0.020(5) -0.003(5) -0.032(4) C44 0.046(4) 0.065(5) 0.087(6) -0.009(4) 0.005(4) -0.022(4) C45 0.053(4) 0.046(4) 0.064(4) -0.010(3) 0.003(3) -0.021(3) C46 0.044(4) 0.046(4) 0.056(4) -0.011(3) 0.006(3) -0.011(3) O22 0.054(3) 0.046(3) 0.080(4) -0.019(2) 0.005(2) -0.017(2) C47 0.057(4) 0.057(4) 0.065(5) -0.017(4) 0.014(4) -0.024(4) C48 0.071(5) 0.073(5) 0.079(6) -0.027(4) 0.026(4) -0.028(4) C49 0.082(6) 0.097(7) 0.081(6) -0.026(6) 0.034(5) -0.035(6) C50 0.102(8) 0.107(8) 0.080(6) -0.028(6) 0.043(6) -0.052(7) C51 0.085(6) 0.075(6) 0.070(5) -0.007(4) 0.019(5) -0.031(5) C52 0.079(6) 0.075(6) 0.083(6) -0.029(5) 0.004(5) -0.039(5) C53 0.103(8) 0.071(6) 0.127(10) -0.029(6) 0.001(7) -0.046(6) C61 0.066(5) 0.073(5) 0.069(5) -0.002(4) 0.001(4) -0.035(4) C62 0.056(5) 0.090(6) 0.091(6) 0.001(5) -0.003(4) -0.041(5) C63 0.056(5) 0.090(6) 0.098(7) 0.008(5) -0.012(4) -0.040(5) C64 0.065(5) 0.095(6) 0.065(5) 0.000(5) -0.013(4) -0.035(5) C65 0.045(4) 0.061(4) 0.060(4) -0.007(3) -0.003(3) -0.023(3) C66 0.051(4) 0.056(4) 0.055(4) -0.008(3) -0.004(3) -0.021(3) O32 0.069(3) 0.057(3) 0.051(3) -0.002(2) -0.001(2) -0.022(2) C67 0.073(5) 0.061(4) 0.055(4) -0.014(3) -0.002(4) -0.033(4) C68 0.091(6) 0.083(6) 0.077(6) -0.021(5) -0.008(5) -0.041(5) C69 0.129(10) 0.100(8) 0.090(7) -0.050(6) -0.003(7) -0.055(7) C70 0.103(8) 0.086(7) 0.092(7) -0.043(6) 0.010(6) -0.028(6) C71 0.072(5) 0.080(6) 0.086(6) -0.047(5) 0.002(5) -0.020(5) C72 0.093(7) 0.054(5) 0.078(6) -0.007(4) 0.021(5) -0.011(5) C73 0.15(3) 0.14(3) 0.073(17) -0.007(17) 0.00(2) 0.02(2) C73A 0.20(5) 0.023(10) 0.20(4) -0.014(13) 0.11(3) -0.002(16) N41 0.086(5) 0.089(6) 0.081(5) -0.017(4) 0.015(4) -0.055(5) O43 0.158(8) 0.124(6) 0.141(7) -0.053(6) 0.031(6) -0.105(6) Cl1 0.0992(17) 0.1030(18) 0.0723(14) -0.0052(13) 0.0012(12) -0.0393(14) O51 0.174(10) 0.151(9) 0.101(6) 0.014(6) 0.056(6) -0.043(7) O52 0.126(8) 0.313(17) 0.120(8) -0.001(9) -0.020(6) -0.127(10) O53 0.146(8) 0.145(8) 0.102(6) 0.033(6) 0.003(6) -0.030(7) O54 0.310(18) 0.152(10) 0.133(9) -0.048(8) 0.043(10) -0.123(11) Cl2 0.213(5) 0.188(4) 0.086(2) -0.005(2) -0.014(3) -0.116(4) O55 0.269(19) 0.243(17) 0.123(10) 0.019(10) -0.020(10) -0.124(15) O56 0.47(4) 0.34(3) 0.33(3) -0.13(2) 0.28(3) -0.25(3) O57 0.62(5) 0.49(4) 0.27(2) -0.06(3) -0.14(3) -0.40(4) O58 0.40(4) 0.176(18) 0.38(4) -0.06(2) -0.14(3) 0.01(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd O31 2.258(5) . ? Gd O21 2.310(5) . ? Gd OW1 2.398(6) . ? Gd O1 2.417(5) . ? Gd O41 2.420(5) . ? Gd O42 2.505(5) . ? Gd N32 2.571(6) . ? Gd N22 2.578(6) . ? Gd N41 2.877(8) . ? Gd Ni2 3.4201(18) . ? Gd Ni1 3.4521(17) . ? Ni1 O11 2.011(5) . ? Ni1 O31 2.035(5) . ? Ni1 N31 2.066(6) . ? Ni1 N1 2.070(6) . ? Ni1 N11 2.096(6) . ? Ni1 O1 2.217(5) . ? Ni2 O21 2.054(5) . ? Ni2 N12 2.065(6) . ? Ni2 O1 2.069(5) . ? Ni2 O11 2.070(5) . ? Ni2 N21 2.090(7) . ? Ni2 N2 2.100(6) . ? O1 C6 1.382(8) . ? N1 C1 1.334(11) . ? N1 C5 1.346(10) . ? N2 C7 1.325(11) . ? N2 C11 1.343(10) . ? O11 C26 1.367(9) . ? N11 C25 1.334(10) . ? N11 C21 1.356(10) . ? N12 C27 1.335(10) . ? N12 C31 1.341(10) . ? O21 C46 1.355(8) . ? N21 C45 1.329(10) . ? N21 C41 1.368(11) . ? N22 C47 1.344(10) . ? N22 C51 1.362(11) . ? O31 C66 1.361(8) . ? N31 C65 1.339(10) . ? N31 C61 1.345(10) . ? N32 C71 1.319(10) . ? N32 C67 1.349(10) . ? O41 N41 1.260(10) . ? O42 N41 1.261(9) . ? C1 C2 1.356(14) . ? C1 H1 0.9300 . ? C2 C3 1.380(15) . ? C2 H2 0.9300 . ? C3 C4 1.362(14) . ? C3 H3 0.9300 . ? C4 C5 1.387(12) . ? C4 H4 0.9300 . ? C5 C6 1.538(11) . ? C6 O2 1.416(9) . ? C6 C7 1.535(11) . ? C7 C8 1.401(12) . ? C8 C9 1.366(14) . ? C8 H8 0.9300 . ? C9 C10 1.387(15) . ? C9 H9 0.9300 . ? C10 C11 1.369(13) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C21 C22 1.386(14) . ? C21 H21 0.9300 . ? C22 C23 1.400(17) . ? C22 H22 0.9300 . ? C23 C24 1.377(15) . ? C23 H23 0.9300 . ? C24 C25 1.373(11) . ? C24 H24 0.9300 . ? C25 C26 1.546(11) . ? C26 O12 1.431(9) . ? C26 C27 1.530(11) . ? O12 C32 1.440(10) . ? C27 C28 1.387(12) . ? C28 C29 1.376(14) . ? C28 H28 0.9300 . ? C29 C30 1.380(16) . ? C29 H29 0.9300 . ? C30 C31 1.380(14) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.477(13) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C41 C42 1.376(13) . ? C41 H41 0.9300 . ? C42 C43 1.368(15) . ? C42 H42 0.9300 . ? C43 C44 1.372(13) . ? C43 H43 0.9300 . ? C44 C45 1.401(11) . ? C44 H44 0.9300 . ? C45 C46 1.519(10) . ? C46 O22 1.442(9) . ? C46 C47 1.544(11) . ? O22 C52 1.446(10) . ? C47 C48 1.385(11) . ? C48 C49 1.368(14) . ? C48 H48 0.9300 . ? C49 C50 1.370(16) . ? C49 H49 0.9300 . ? C50 C51 1.406(13) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 C53 1.496(14) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C61 C62 1.370(12) . ? C61 H61 0.9300 . ? C62 C63 1.376(14) . ? C62 H62 0.9300 . ? C63 C64 1.361(13) . ? C63 H63 0.9300 . ? C64 C65 1.387(11) . ? C64 H64 0.9300 . ? C65 C66 1.522(10) . ? C66 O32 1.445(9) . ? C66 C67 1.542(11) . ? O32 C72 1.435(10) . ? C67 C68 1.360(12) . ? C68 C69 1.394(14) . ? C68 H68 0.9300 . ? C69 C70 1.334(16) . ? C69 H69 0.9300 . ? C70 C71 1.392(14) . ? C70 H70 0.9300 . ? C71 H71 0.9300 . ? C72 C73A 1.48(4) . ? C72 C73 1.52(4) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? N41 O43 1.228(10) . ? Cl1 O51 1.396(9) . ? Cl1 O53 1.410(10) . ? Cl1 O54 1.412(12) . ? Cl1 O52 1.440(10) . ? Cl2 O57 1.291(17) . ? Cl2 O55 1.347(13) . ? Cl2 O56 1.35(2) . ? Cl2 O58 1.54(2) . ? O1E C1E 1.28(3) . ? C1E C2E 1.23(3) . ? O2E C3E 1.27(3) . ? C3E C4E 1.19(3) . ? O3E C5E 1.23(3) . ? C5E C6E 1.20(3) . ? O4E C7E 1.24(3) . ? C7E C8E 1.21(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O31 Gd O21 109.16(17) . . ? O31 Gd OW1 93.51(19) . . ? O21 Gd OW1 137.5(2) . . ? O31 Gd O1 71.43(16) . . ? O21 Gd O1 72.09(16) . . ? OW1 Gd O1 150.4(2) . . ? O31 Gd O41 132.8(2) . . ? O21 Gd O41 105.8(2) . . ? OW1 Gd O41 81.0(2) . . ? O1 Gd O41 90.7(2) . . ? O31 Gd O42 81.50(18) . . ? O21 Gd O42 141.32(19) . . ? OW1 Gd O42 75.7(2) . . ? O1 Gd O42 76.94(18) . . ? O41 Gd O42 51.6(2) . . ? O31 Gd N32 64.72(19) . . ? O21 Gd N32 83.62(19) . . ? OW1 Gd N32 74.1(2) . . ? O1 Gd N32 118.38(19) . . ? O41 Gd N32 150.9(2) . . ? O42 Gd N32 132.4(2) . . ? O31 Gd N22 151.2(2) . . ? O21 Gd N22 64.24(19) . . ? OW1 Gd N22 78.5(2) . . ? O1 Gd N22 126.51(19) . . ? O41 Gd N22 73.7(2) . . ? O42 Gd N22 122.0(2) . . ? N32 Gd N22 86.5(2) . . ? O31 Gd N41 107.2(2) . . ? O21 Gd N41 125.1(2) . . ? OW1 Gd N41 77.9(2) . . ? O1 Gd N41 82.36(19) . . ? O41 Gd N41 25.7(2) . . ? O42 Gd N41 25.9(2) . . ? N32 Gd N41 150.1(2) . . ? N22 Gd N41 98.2(2) . . ? O31 Gd Ni2 87.12(12) . . ? O21 Gd Ni2 35.82(12) . . ? OW1 Gd Ni2 172.15(16) . . ? O1 Gd Ni2 36.69(11) . . ? O41 Gd Ni2 104.26(18) . . ? O42 Gd Ni2 112.13(15) . . ? N32 Gd Ni2 99.22(15) . . ? N22 Gd Ni2 97.27(16) . . ? N41 Gd Ni2 109.35(17) . . ? O31 Gd Ni1 34.32(12) . . ? O21 Gd Ni1 83.58(12) . . ? OW1 Gd Ni1 127.49(16) . . ? O1 Gd Ni1 39.68(11) . . ? O41 Gd Ni1 124.91(16) . . ? O42 Gd Ni1 87.22(15) . . ? N32 Gd Ni1 83.00(16) . . ? N22 Gd Ni1 147.06(15) . . ? N41 Gd Ni1 106.40(16) . . ? Ni2 Gd Ni1 54.22(4) . . ? O11 Ni1 O31 97.63(19) . . ? O11 Ni1 N31 106.3(2) . . ? O31 Ni1 N31 78.8(2) . . ? O11 Ni1 N1 154.1(2) . . ? O31 Ni1 N1 89.7(2) . . ? N31 Ni1 N1 99.5(2) . . ? O11 Ni1 N11 78.0(2) . . ? O31 Ni1 N11 169.7(2) . . ? N31 Ni1 N11 93.4(2) . . ? N1 Ni1 N11 98.3(3) . . ? O11 Ni1 O1 79.19(18) . . ? O31 Ni1 O1 79.86(18) . . ? N31 Ni1 O1 158.5(2) . . ? N1 Ni1 O1 77.7(2) . . ? N11 Ni1 O1 108.1(2) . . ? O11 Ni1 Gd 76.97(13) . . ? O31 Ni1 Gd 38.74(13) . . ? N31 Ni1 Gd 115.88(17) . . ? N1 Ni1 Gd 94.20(18) . . ? N11 Ni1 Gd 145.72(17) . . ? O1 Ni1 Gd 44.12(12) . . ? O21 Ni2 N12 104.8(2) . . ? O21 Ni2 O1 84.91(19) . . ? N12 Ni2 O1 158.1(2) . . ? O21 Ni2 O11 87.11(18) . . ? N12 Ni2 O11 79.5(2) . . ? O1 Ni2 O11 81.44(18) . . ? O21 Ni2 N21 77.5(2) . . ? N12 Ni2 N21 97.4(3) . . ? O1 Ni2 N21 104.0(2) . . ? O11 Ni2 N21 163.1(2) . . ? O21 Ni2 N2 158.2(2) . . ? N12 Ni2 N2 96.2(3) . . ? O1 Ni2 N2 77.5(2) . . ? O11 Ni2 N2 102.7(2) . . ? N21 Ni2 N2 94.2(2) . . ? O21 Ni2 Gd 41.16(13) . . ? N12 Ni2 Gd 138.94(19) . . ? O1 Ni2 Gd 44.27(13) . . ? O11 Ni2 Gd 77.15(13) . . ? N21 Ni2 Gd 95.4(2) . . ? N2 Ni2 Gd 121.55(18) . . ? C6 O1 Ni2 116.2(4) . . ? C6 O1 Ni1 105.8(4) . . ? Ni2 O1 Ni1 93.82(18) . . ? C6 O1 Gd 136.3(4) . . ? Ni2 O1 Gd 99.04(18) . . ? Ni1 O1 Gd 96.20(17) . . ? C1 N1 C5 118.2(7) . . ? C1 N1 Ni1 126.6(6) . . ? C5 N1 Ni1 114.5(5) . . ? C7 N2 C11 118.8(7) . . ? C7 N2 Ni2 115.0(5) . . ? C11 N2 Ni2 126.2(6) . . ? C26 O11 Ni1 115.9(4) . . ? C26 O11 Ni2 110.7(4) . . ? Ni1 O11 Ni2 100.2(2) . . ? C25 N11 C21 119.4(7) . . ? C25 N11 Ni1 114.3(5) . . ? C21 N11 Ni1 126.0(6) . . ? C27 N12 C31 119.0(7) . . ? C27 N12 Ni2 112.9(5) . . ? C31 N12 Ni2 128.1(6) . . ? C46 O21 Ni2 113.1(4) . . ? C46 O21 Gd 126.8(4) . . ? Ni2 O21 Gd 103.02(19) . . ? C45 N21 C41 118.4(7) . . ? C45 N21 Ni2 114.6(5) . . ? C41 N21 Ni2 127.0(6) . . ? C47 N22 C51 116.3(7) . . ? C47 N22 Gd 117.5(5) . . ? C51 N22 Gd 126.2(6) . . ? C66 O31 Ni1 116.3(4) . . ? C66 O31 Gd 126.0(4) . . ? Ni1 O31 Gd 106.9(2) . . ? C65 N31 C61 118.0(7) . . ? C65 N31 Ni1 114.7(5) . . ? C61 N31 Ni1 126.5(5) . . ? C71 N32 C67 116.7(7) . . ? C71 N32 Gd 126.2(6) . . ? C67 N32 Gd 117.1(5) . . ? N41 O41 Gd 97.9(5) . . ? N41 O42 Gd 93.7(5) . . ? N1 C1 C2 123.3(9) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 118.6(9) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 119.4(9) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 119.1(9) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 121.3(8) . . ? N1 C5 C6 115.3(6) . . ? C4 C5 C6 123.4(7) . . ? O1 C6 O2 111.6(6) . . ? O1 C6 C7 109.0(6) . . ? O2 C6 C7 109.4(6) . . ? O1 C6 C5 108.9(6) . . ? O2 C6 C5 106.9(6) . . ? C7 C6 C5 111.1(6) . . ? N2 C7 C8 121.1(8) . . ? N2 C7 C6 116.8(6) . . ? C8 C7 C6 122.1(8) . . ? C9 C8 C7 120.1(10) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 118.1(8) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? C11 C10 C9 119.1(9) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? N2 C11 C10 122.8(9) . . ? N2 C11 H11 118.6 . . ? C10 C11 H11 118.6 . . ? N11 C21 C22 121.2(10) . . ? N11 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C21 C22 C23 119.2(10) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C24 C23 C22 117.9(9) . . ? C24 C23 H23 121.0 . . ? C22 C23 H23 121.0 . . ? C25 C24 C23 120.5(10) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? N11 C25 C24 121.7(8) . . ? N11 C25 C26 114.3(6) . . ? C24 C25 C26 124.0(8) . . ? O11 C26 O12 113.3(6) . . ? O11 C26 C27 109.6(6) . . ? O12 C26 C27 110.4(6) . . ? O11 C26 C25 110.2(6) . . ? O12 C26 C25 102.5(6) . . ? C27 C26 C25 110.7(6) . . ? C26 O12 C32 113.5(6) . . ? N12 C27 C28 121.6(8) . . ? N12 C27 C26 115.7(7) . . ? C28 C27 C26 122.7(7) . . ? C29 C28 C27 119.1(10) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C28 C29 C30 119.4(10) . . ? C28 C29 H29 120.3 . . ? C30 C29 H29 120.3 . . ? C31 C30 C29 118.4(9) . . ? C31 C30 H30 120.8 . . ? C29 C30 H30 120.8 . . ? N12 C31 C30 122.5(9) . . ? N12 C31 H31 118.8 . . ? C30 C31 H31 118.8 . . ? O12 C32 C33 107.9(7) . . ? O12 C32 H32A 110.1 . . ? C33 C32 H32A 110.1 . . ? O12 C32 H32B 110.1 . . ? C33 C32 H32B 110.1 . . ? H32A C32 H32B 108.4 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N21 C41 C42 121.1(10) . . ? N21 C41 H41 119.4 . . ? C42 C41 H41 119.4 . . ? C43 C42 C41 120.3(9) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 118.9(8) . . ? C42 C43 H43 120.6 . . ? C44 C43 H43 120.6 . . ? C43 C44 C45 119.0(8) . . ? C43 C44 H44 120.5 . . ? C45 C44 H44 120.5 . . ? N21 C45 C44 122.2(7) . . ? N21 C45 C46 114.2(6) . . ? C44 C45 C46 123.6(7) . . ? O21 C46 O22 111.9(6) . . ? O21 C46 C45 110.4(6) . . ? O22 C46 C45 102.1(5) . . ? O21 C46 C47 109.9(6) . . ? O22 C46 C47 109.1(6) . . ? C45 C46 C47 113.2(6) . . ? C46 O22 C52 115.1(6) . . ? N22 C47 C48 123.3(8) . . ? N22 C47 C46 114.8(6) . . ? C48 C47 C46 121.9(7) . . ? C49 C48 C47 119.3(9) . . ? C49 C48 H48 120.4 . . ? C47 C48 H48 120.4 . . ? C48 C49 C50 120.0(9) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C49 C50 C51 117.7(9) . . ? C49 C50 H50 121.1 . . ? C51 C50 H50 121.1 . . ? N22 C51 C50 123.3(9) . . ? N22 C51 H51 118.3 . . ? C50 C51 H51 118.3 . . ? O22 C52 C53 107.6(8) . . ? O22 C52 H52A 110.2 . . ? C53 C52 H52A 110.2 . . ? O22 C52 H52B 110.2 . . ? C53 C52 H52B 110.2 . . ? H52A C52 H52B 108.5 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N31 C61 C62 123.2(8) . . ? N31 C61 H61 118.4 . . ? C62 C61 H61 118.4 . . ? C61 C62 C63 118.3(8) . . ? C61 C62 H62 120.9 . . ? C63 C62 H62 120.9 . . ? C64 C63 C62 119.4(8) . . ? C64 C63 H63 120.3 . . ? C62 C63 H63 120.3 . . ? C63 C64 C65 119.7(9) . . ? C63 C64 H64 120.2 . . ? C65 C64 H64 120.2 . . ? N31 C65 C64 121.4(7) . . ? N31 C65 C66 115.4(6) . . ? C64 C65 C66 123.1(7) . . ? O31 C66 O32 111.3(6) . . ? O31 C66 C65 110.2(6) . . ? O32 C66 C65 108.8(6) . . ? O31 C66 C67 110.5(6) . . ? O32 C66 C67 101.5(6) . . ? C65 C66 C67 114.2(6) . . ? C72 O32 C66 114.6(6) . . ? N32 C67 C68 123.5(8) . . ? N32 C67 C66 113.2(6) . . ? C68 C67 C66 123.1(8) . . ? C67 C68 C69 118.3(10) . . ? C67 C68 H68 120.9 . . ? C69 C68 H68 120.9 . . ? C70 C69 C68 119.1(9) . . ? C70 C69 H69 120.5 . . ? C68 C69 H69 120.5 . . ? C69 C70 C71 119.3(9) . . ? C69 C70 H70 120.4 . . ? C71 C70 H70 120.4 . . ? N32 C71 C70 123.2(9) . . ? N32 C71 H71 118.4 . . ? C70 C71 H71 118.4 . . ? O32 C72 C73A 105.4(16) . . ? O32 C72 C73 111.9(19) . . ? C73A C72 C73 25(3) . . ? O32 C72 H72A 109.2 . . ? C73A C72 H72A 90.1 . . ? C73 C72 H72A 109.2 . . ? O32 C72 H72B 109.2 . . ? C73A C72 H72B 132.2 . . ? C73 C72 H72B 109.2 . . ? H72A C72 H72B 107.9 . . ? O43 N41 O41 122.6(8) . . ? O43 N41 O42 120.8(9) . . ? O41 N41 O42 116.6(7) . . ? O43 N41 Gd 178.0(8) . . ? O41 N41 Gd 56.4(4) . . ? O42 N41 Gd 60.3(4) . . ? O51 Cl1 O53 111.6(7) . . ? O51 Cl1 O54 113.4(8) . . ? O53 Cl1 O54 108.8(8) . . ? O51 Cl1 O52 109.0(8) . . ? O53 Cl1 O52 107.0(8) . . ? O54 Cl1 O52 106.7(10) . . ? O57 Cl2 O55 118.8(16) . . ? O57 Cl2 O56 117(2) . . ? O55 Cl2 O56 113.6(17) . . ? O57 Cl2 O58 106(2) . . ? O55 Cl2 O58 98.8(14) . . ? O56 Cl2 O58 97.3(18) . . ? C2E C1E O1E 115(3) . . ? C4E C3E O2E 115(3) . . ? C6E C5E O3E 123(4) . . ? C8E C7E O4E 120(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 58.44 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.625 _refine_diff_density_min -1.122 _refine_diff_density_rms 0.131 # Attachment '- peng63a1.cif' data_peng63a1 _database_code_depnum_ccdc_archive 'CCDC 778583' #TrackingRef '- peng63a1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C109.20 H129.60 Cl2 N23 Ni4 O52.60 Y3' _chemical_formula_weight 3178.43 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 12.0779(5) _cell_length_b 22.1582(5) _cell_length_c 53.202(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.0670(10) _cell_angle_gamma 90.00 _cell_volume 14202.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 24202 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 27.61 _exptl_crystal_description parallelepiped _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6518 _exptl_absorpt_coefficient_mu 1.860 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.257 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'CrystalClear, Rigaku MSC, 2005' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Rigaku R-AXIS SPIDER IPDS' _diffrn_measurement_method '\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31118 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.0716 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -60 _diffrn_reflns_limit_l_max 60 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 24.00 _reflns_number_total 10442 _reflns_number_gt 7731 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Rigaku MSC, 2005' _computing_cell_refinement 'CrystalClear, Rigaku MSC, 2005' _computing_data_reduction 'CrystalClear, Rigaku MSC, 2005' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+114.0602P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10442 _refine_ls_number_parameters 857 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1088 _refine_ls_R_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.1870 _refine_ls_wR_factor_gt 0.1708 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.73215(5) 0.16361(3) 0.094428(13) 0.0452(2) Uani 1 1 d . . . Ni1 Ni 0.97531(7) 0.15680(5) 0.132468(17) 0.0471(3) Uani 1 1 d . . . Ni2 Ni 0.79669(7) 0.24879(4) 0.148269(16) 0.0413(2) Uani 1 1 d . . . OW1 O 0.6876(4) 0.1161(3) 0.05558(10) 0.0648(15) Uani 1 1 d . . . O1 O 0.7247(3) 0.2557(2) 0.11215(8) 0.0429(11) Uani 1 1 d . . . O21 O 0.9082(4) 0.1382(2) 0.09737(9) 0.0480(12) Uani 1 1 d . . . O41 O 0.9462(3) 0.2446(2) 0.13238(9) 0.0475(12) Uani 1 1 d . . . O61 O 0.7923(4) 0.1563(2) 0.13868(8) 0.0441(11) Uani 1 1 d . . . O3 O 0.5666(4) 0.1152(3) 0.10479(12) 0.0733(17) Uani 1 1 d . . . O4 O 0.7060(5) 0.0560(3) 0.10451(11) 0.0670(15) Uani 1 1 d . . . N1 N 0.5764(5) 0.2304(3) 0.07528(11) 0.0514(15) Uani 1 1 d . . . N2 N 0.6321(4) 0.2731(3) 0.15523(11) 0.0477(15) Uani 1 1 d . . . N21 N 0.8468(5) 0.2154(3) 0.06195(12) 0.0585(17) Uani 1 1 d . . . N22 N 1.1173(5) 0.1494(3) 0.11312(13) 0.0585(17) Uani 1 1 d . . . N41 N 0.8630(5) 0.3320(3) 0.15888(11) 0.0497(15) Uani 1 1 d . . . N42 N 1.0619(5) 0.1840(3) 0.16630(12) 0.0562(17) Uani 1 1 d . . . N61 N 0.9507(5) 0.0695(3) 0.14386(12) 0.0526(16) Uani 1 1 d . . . N62 N 0.8310(5) 0.2051(3) 0.18312(10) 0.0489(15) Uani 1 1 d . . . O5 O 0.5461(7) 0.0210(4) 0.11470(15) 0.109(3) Uani 1 1 d . . . O2 O 0.6654(4) 0.3559(2) 0.11319(9) 0.0506(12) Uani 1 1 d . . . O22 O 0.9551(4) 0.0902(3) 0.06067(10) 0.0648(15) Uani 1 1 d . . . O42 O 1.1167(4) 0.2950(3) 0.13057(10) 0.0591(14) Uani 1 1 d . . . O62 O 0.6727(4) 0.0920(2) 0.15939(10) 0.0607(14) Uani 1 1 d . . . N3 N 0.6055(6) 0.0613(4) 0.10855(14) 0.0683(19) Uani 1 1 d . . . C1 C 0.5093(7) 0.2190(5) 0.05441(16) 0.073(3) Uani 1 1 d . . . H1 H 0.5155 0.1808 0.0466 0.095 Uiso 1 1 calc R . . C2 C 0.4331(7) 0.2590(5) 0.04381(17) 0.075(3) Uani 1 1 d . . . H2 H 0.3871 0.2484 0.0292 0.097 Uiso 1 1 calc R . . C3 C 0.4247(7) 0.3139(5) 0.05459(16) 0.069(2) Uani 1 1 d . . . H3 H 0.3739 0.3429 0.0474 0.090 Uiso 1 1 calc R . . C4 C 0.4914(6) 0.3282(4) 0.07656(16) 0.062(2) Uani 1 1 d . . . H4 H 0.4868 0.3665 0.0844 0.080 Uiso 1 1 calc R . . C5 C 0.5646(5) 0.2840(3) 0.08639(13) 0.0440(17) Uani 1 1 d . . . C6 C 0.6350(5) 0.2939(3) 0.11095(13) 0.0428(16) Uani 1 1 d . . . C7 C 0.5687(5) 0.2842(3) 0.13404(13) 0.0410(16) Uani 1 1 d . . . C8 C 0.4556(6) 0.2898(4) 0.13413(15) 0.055(2) Uani 1 1 d . . . H8 H 0.4117 0.2973 0.1189 0.072 Uiso 1 1 calc R . . C9 C 0.4064(6) 0.2844(4) 0.15689(17) 0.067(2) Uani 1 1 d . . . H9 H 0.3280 0.2869 0.1573 0.088 Uiso 1 1 calc R . . C10 C 0.4708(6) 0.2755(4) 0.17857(17) 0.068(2) Uani 1 1 d . . . H10 H 0.4388 0.2726 0.1943 0.088 Uiso 1 1 calc R . . C11 C 0.5822(7) 0.2708(4) 0.17704(15) 0.062(2) Uani 1 1 d . . . H11 H 0.6275 0.2656 0.1922 0.081 Uiso 1 1 calc R . . C12 C 0.7478(7) 0.3755(4) 0.09692(17) 0.061(2) Uani 1 1 d . . . H12A H 0.7225 0.3682 0.0791 0.080 Uiso 1 1 calc R . . H12B H 0.8182 0.3534 0.1008 0.080 Uiso 1 1 calc R . . C13 C 0.7640(9) 0.4418(5) 0.1017(2) 0.103(4) Uani 1 1 d . . . H13A H 0.8298 0.4556 0.0936 0.133 Uiso 1 1 calc R . . H13B H 0.7740 0.4490 0.1199 0.133 Uiso 1 1 calc R . . H13C H 0.6986 0.4639 0.0947 0.133 Uiso 1 1 calc R . . C21 C 0.8142(8) 0.2598(5) 0.04639(18) 0.082(3) Uani 1 1 d . . . H21 H 0.7397 0.2733 0.0467 0.106 Uiso 1 1 calc R . . C22 C 0.8798(10) 0.2875(6) 0.0299(2) 0.098(4) Uani 1 1 d . . . H22 H 0.8530 0.3201 0.0196 0.128 Uiso 1 1 calc R . . C23 C 0.9852(11) 0.2664(6) 0.0291(2) 0.101(4) Uani 1 1 d . . . H23 H 1.0335 0.2840 0.0178 0.131 Uiso 1 1 calc R . . C24 C 1.0226(8) 0.2190(5) 0.04468(18) 0.082(3) Uani 1 1 d . . . H24 H 1.0960 0.2039 0.0441 0.106 Uiso 1 1 calc R . . C25 C 0.9507(6) 0.1940(4) 0.06121(14) 0.056(2) Uani 1 1 d . . . C26 C 0.9768(6) 0.1399(4) 0.07777(14) 0.0522(19) Uani 1 1 d . . . C27 C 1.0990(6) 0.1371(4) 0.08864(16) 0.059(2) Uani 1 1 d . . . C28 C 1.1846(7) 0.1215(5) 0.07367(19) 0.084(3) Uani 1 1 d . . . H28 H 1.1698 0.1123 0.0563 0.110 Uiso 1 1 calc R . . C29 C 1.2907(7) 0.1196(6) 0.0846(2) 0.097(4) Uani 1 1 d . . . H29 H 1.3503 0.1074 0.0750 0.126 Uiso 1 1 calc R . . C30 C 1.3102(7) 0.1353(6) 0.1092(2) 0.096(4) Uani 1 1 d . . . H30 H 1.3840 0.1366 0.1166 0.125 Uiso 1 1 calc R . . C31 C 1.2234(6) 0.1491(5) 0.12301(18) 0.075(3) Uani 1 1 d . . . H31 H 1.2378 0.1590 0.1403 0.097 Uiso 1 1 calc R . . C32 C 0.9612(10) 0.0319(5) 0.0720(2) 0.093(3) Uani 1 1 d . . . H32A H 0.9364 0.0343 0.0893 0.121 Uiso 1 1 calc R . . H32B H 1.0391 0.0176 0.0731 0.121 Uiso 1 1 calc R . . C33 C 0.8926(16) -0.0102(5) 0.0575(3) 0.186(9) Uani 1 1 d . . . H33A H 0.8700 -0.0429 0.0685 0.242 Uiso 1 1 calc R . . H33B H 0.9344 -0.0271 0.0440 0.242 Uiso 1 1 calc R . . H33C H 0.8265 0.0106 0.0501 0.242 Uiso 1 1 calc R . . C41 C 0.8121(7) 0.3803(4) 0.16855(17) 0.069(2) Uani 1 1 d . . . H41 H 0.7365 0.3769 0.1722 0.089 Uiso 1 1 calc R . . C42 C 0.8658(9) 0.4335(5) 0.1732(2) 0.090(3) Uani 1 1 d . . . H42 H 0.8279 0.4669 0.1797 0.117 Uiso 1 1 calc R . . C43 C 0.9763(9) 0.4381(5) 0.1683(2) 0.099(4) Uani 1 1 d . . . H43 H 1.0150 0.4750 0.1714 0.129 Uiso 1 1 calc R . . C44 C 1.0293(8) 0.3899(4) 0.1590(2) 0.083(3) Uani 1 1 d . . . H44 H 1.1055 0.3928 0.1559 0.107 Uiso 1 1 calc R . . C45 C 0.9724(6) 0.3370(4) 0.15422(15) 0.0556(19) Uani 1 1 d . . . C46 C 1.0252(6) 0.2793(4) 0.14545(14) 0.0515(19) Uani 1 1 d . . . C47 C 1.0812(5) 0.2434(4) 0.16737(14) 0.056(2) Uani 1 1 d . . . C48 C 1.1471(6) 0.2700(4) 0.18694(15) 0.063(2) Uani 1 1 d . . . H48 H 1.1578 0.3124 0.1878 0.082 Uiso 1 1 calc R . . C49 C 1.1972(7) 0.2306(6) 0.20538(16) 0.079(3) Uani 1 1 d . . . H49 H 1.2441 0.2465 0.2189 0.103 Uiso 1 1 calc R . . C50 C 1.1786(8) 0.1711(5) 0.20383(17) 0.076(3) Uani 1 1 d . . . H50 H 1.2126 0.1447 0.2161 0.099 Uiso 1 1 calc R . . C51 C 1.1104(7) 0.1485(4) 0.18444(15) 0.069(2) Uani 1 1 d . . . H51 H 1.0968 0.1062 0.1838 0.090 Uiso 1 1 calc R . . C52 C 1.0833(7) 0.3197(5) 0.10595(17) 0.078(3) Uani 1 1 d . . . H52A H 1.0437 0.3584 0.1078 0.101 Uiso 1 1 calc R . . H52B H 1.0327 0.2913 0.0965 0.101 Uiso 1 1 calc R . . C53 C 1.1853(9) 0.3295(8) 0.0922(2) 0.151(7) Uani 1 1 d . . . H53A H 1.1642 0.3408 0.0747 0.197 Uiso 1 1 calc R . . H53B H 1.2291 0.2922 0.0925 0.197 Uiso 1 1 calc R . . H53C H 1.2297 0.3619 0.1004 0.197 Uiso 1 1 calc R . . C61 C 1.0187(7) 0.0235(4) 0.13999(16) 0.068(2) Uani 1 1 d . . . H61 H 1.0887 0.0316 0.1336 0.088 Uiso 1 1 calc R . . C62 C 0.9906(9) -0.0355(5) 0.1449(2) 0.083(3) Uani 1 1 d . . . H62 H 1.0391 -0.0678 0.1415 0.107 Uiso 1 1 calc R . . C63 C 0.8903(10) -0.0462(4) 0.15482(19) 0.084(3) Uani 1 1 d . . . H63 H 0.8700 -0.0862 0.1589 0.109 Uiso 1 1 calc R . . C64 C 0.8194(8) 0.0008(4) 0.15882(18) 0.072(2) Uani 1 1 d . . . H64 H 0.7493 -0.0061 0.1653 0.093 Uiso 1 1 calc R . . C65 C 0.8536(6) 0.0585(3) 0.15304(14) 0.0490(18) Uani 1 1 d . . . C66 C 0.7832(6) 0.1151(4) 0.15783(13) 0.0504(18) Uani 1 1 d . . . C67 C 0.8203(6) 0.1448(4) 0.18319(13) 0.0488(18) Uani 1 1 d . . . C68 C 0.8393(7) 0.1109(4) 0.20509(15) 0.067(2) Uani 1 1 d . . . H68 H 0.8305 0.0683 0.2046 0.087 Uiso 1 1 calc R . . C69 C 0.8708(8) 0.1394(5) 0.22750(16) 0.076(3) Uani 1 1 d . . . H69 H 0.8859 0.1170 0.2426 0.099 Uiso 1 1 calc R . . C70 C 0.8796(8) 0.2009(5) 0.22726(15) 0.076(3) Uani 1 1 d . . . H70 H 0.9001 0.2219 0.2425 0.099 Uiso 1 1 calc R . . C71 C 0.8592(6) 0.2329(4) 0.20525(14) 0.061(2) Uani 1 1 d . . . H71 H 0.8652 0.2756 0.2056 0.079 Uiso 1 1 calc R . . C72 C 0.5891(7) 0.1328(4) 0.1661(2) 0.079(3) Uani 1 1 d . . . H72A H 0.5754 0.1631 0.1526 0.103 Uiso 1 1 calc R . . H72B H 0.6148 0.1544 0.1818 0.103 Uiso 1 1 calc R . . C73 C 0.4842(8) 0.1003(5) 0.1702(2) 0.104(4) Uani 1 1 d . . . H73A H 0.4249 0.1297 0.1723 0.135 Uiso 1 1 calc R . . H73B H 0.4945 0.0753 0.1853 0.135 Uiso 1 1 calc R . . H73C H 0.4640 0.0747 0.1556 0.135 Uiso 1 1 calc R . . Y2 Y 0.5000 0.41849(6) 0.2500 0.0793(4) Uani 1 2 d S . . N11 N 0.2991(11) 0.4197(5) 0.21642(17) 0.098(3) Uani 1 1 d . . . N12 N 0.6076(10) 0.4796(8) 0.2127(2) 0.123(4) Uani 1 1 d . . . O11 O 0.3223(11) 0.4568(6) 0.2327(3) 0.223(8) Uani 1 1 d . . . O12 O 0.3724(9) 0.3816(5) 0.21625(17) 0.132(3) Uani 1 1 d . . . O13 O 0.2162(7) 0.4206(4) 0.20289(16) 0.124(3) Uani 1 1 d . . . O14 O 0.5487(8) 0.5075(4) 0.22699(18) 0.128(3) Uani 1 1 d . . . O15 O 0.6121(10) 0.4244(6) 0.2153(2) 0.158(4) Uani 1 1 d . . . O16 O 0.6613(9) 0.5071(6) 0.1977(2) 0.173(5) Uani 1 1 d . . . N13 N 0.5000 0.2998(11) 0.2500 0.143(6) Uiso 1 2 d S . . O17 O 0.5770(11) 0.3163(6) 0.2387(2) 0.188(5) Uiso 1 1 d . . . O18 O 0.5000 0.242(3) 0.2500 0.49(3) Uiso 1 2 d S . . Cl Cl 0.2789(3) 0.11532(18) 0.00224(5) 0.1023(9) Uani 1 1 d . . . O6 O 0.2113(17) 0.1607(12) 0.0074(3) 0.349(15) Uani 1 1 d . . . O7 O 0.263(2) 0.0598(10) 0.0104(5) 0.372(15) Uani 1 1 d . . . O8 O 0.2809(10) 0.1128(7) -0.02314(17) 0.203(6) Uani 1 1 d . . . O9 O 0.3765(14) 0.1258(6) 0.0137(3) 0.263(9) Uani 1 1 d . . . O1E O 0.8201(18) 0.1185(10) 0.0155(4) 0.171(7) Uiso 0.60 1 d P . . C1E C 0.875(3) 0.1044(18) -0.0072(8) 0.181(13) Uiso 0.60 1 d P . . C2E C 0.866(3) 0.0724(19) -0.0229(7) 0.193(14) Uiso 0.60 1 d P . . O2E O 0.5071(9) 0.0488(6) 0.0455(2) 0.104(3) Uiso 0.70 1 d P . . C3E C 0.530(3) -0.0058(18) 0.0401(6) 0.205(13) Uiso 0.70 1 d P . . C4E C 0.481(3) -0.0480(18) 0.0486(7) 0.219(14) Uiso 0.70 1 d P . . O2W O 0.7644(17) 0.0790(10) 0.0072(4) 0.188(7) Uiso 0.70 1 d P . . O3W O 0.0000 0.367(3) 0.2500 0.24(3) Uiso 0.40 2 d SP . . O4W O -0.073(4) 0.387(2) 0.2410(9) 0.197(17) Uiso 0.30 1 d P . . O5W O 0.561(3) 0.084(2) 0.2527(9) 0.200(18) Uiso 0.30 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 Y1 0.0338(4) 0.0550(4) 0.0465(4) -0.0042(3) 0.0013(3) 0.0083(3) Ni1 0.0341(5) 0.0584(6) 0.0486(5) -0.0030(5) 0.0003(4) 0.0105(4) Ni2 0.0308(4) 0.0492(5) 0.0435(5) -0.0040(4) -0.0007(3) 0.0032(4) OW1 0.062(3) 0.075(4) 0.057(3) -0.016(3) -0.001(3) 0.007(3) O1 0.031(2) 0.054(3) 0.044(2) -0.003(2) 0.0011(19) 0.010(2) O21 0.034(2) 0.061(3) 0.050(3) 0.000(2) 0.004(2) 0.002(2) O41 0.028(2) 0.060(3) 0.054(3) -0.008(3) 0.000(2) -0.003(2) O61 0.044(3) 0.046(3) 0.042(2) -0.002(2) -0.001(2) 0.011(2) O3 0.040(3) 0.090(5) 0.092(4) 0.009(4) 0.012(3) -0.002(3) O4 0.058(4) 0.069(4) 0.073(4) -0.004(3) 0.005(3) 0.000(3) N1 0.042(3) 0.058(4) 0.052(4) -0.005(3) -0.007(3) 0.009(3) N2 0.034(3) 0.059(4) 0.050(3) -0.006(3) 0.004(3) 0.002(3) N21 0.051(4) 0.074(5) 0.051(4) 0.006(4) 0.012(3) 0.002(3) N22 0.039(3) 0.069(5) 0.068(4) -0.004(4) 0.002(3) 0.004(3) N41 0.042(3) 0.055(4) 0.051(3) -0.008(3) -0.002(3) -0.002(3) N42 0.044(4) 0.071(5) 0.054(4) 0.003(3) -0.002(3) 0.006(3) N61 0.049(4) 0.049(4) 0.058(4) 0.000(3) -0.003(3) 0.017(3) N62 0.037(3) 0.066(4) 0.043(3) -0.007(3) 0.001(3) 0.004(3) O5 0.106(6) 0.101(6) 0.120(6) 0.010(5) 0.009(5) -0.058(5) O2 0.038(3) 0.056(3) 0.057(3) -0.003(2) 0.004(2) 0.006(2) O22 0.061(3) 0.070(4) 0.063(3) -0.020(3) -0.001(3) 0.022(3) O42 0.033(3) 0.077(4) 0.067(3) 0.007(3) 0.003(2) -0.004(3) O62 0.055(3) 0.055(3) 0.073(3) -0.007(3) 0.010(3) 0.002(3) N3 0.063(5) 0.075(6) 0.066(4) -0.010(4) 0.000(4) -0.010(4) C1 0.057(5) 0.088(7) 0.070(5) -0.014(5) -0.021(4) 0.012(5) C2 0.061(5) 0.089(7) 0.072(6) 0.008(5) -0.018(4) 0.008(5) C3 0.059(5) 0.082(7) 0.064(5) 0.011(5) -0.014(4) 0.025(5) C4 0.053(5) 0.061(5) 0.070(5) -0.008(4) -0.010(4) 0.019(4) C5 0.034(4) 0.047(4) 0.050(4) -0.002(3) 0.002(3) 0.005(3) C6 0.034(4) 0.037(4) 0.057(4) -0.003(3) 0.001(3) 0.009(3) C7 0.034(4) 0.037(4) 0.053(4) -0.006(3) 0.008(3) 0.006(3) C8 0.034(4) 0.063(5) 0.068(5) -0.001(4) -0.001(3) 0.003(4) C9 0.037(4) 0.087(7) 0.080(6) -0.003(5) 0.017(4) 0.003(4) C10 0.046(5) 0.089(7) 0.071(5) -0.017(5) 0.022(4) -0.001(4) C11 0.055(5) 0.081(6) 0.052(4) -0.010(4) 0.008(4) 0.000(4) C12 0.055(5) 0.049(5) 0.082(6) 0.004(4) 0.019(4) -0.003(4) C13 0.099(8) 0.080(8) 0.133(10) 0.014(7) 0.034(7) -0.021(6) C21 0.079(6) 0.092(8) 0.076(6) 0.025(6) 0.016(5) 0.008(6) C22 0.106(9) 0.106(9) 0.086(7) 0.031(7) 0.029(6) 0.017(7) C23 0.107(9) 0.118(10) 0.081(7) 0.024(7) 0.031(6) -0.010(8) C24 0.064(6) 0.109(8) 0.076(6) 0.000(6) 0.027(5) -0.011(6) C25 0.049(4) 0.068(5) 0.053(4) -0.007(4) 0.011(4) -0.006(4) C26 0.033(4) 0.068(5) 0.057(4) -0.008(4) 0.012(3) 0.003(4) C27 0.037(4) 0.068(6) 0.073(5) -0.002(4) 0.015(4) 0.010(4) C28 0.048(5) 0.124(9) 0.084(6) -0.016(6) 0.023(5) 0.023(5) C29 0.042(5) 0.156(12) 0.095(8) -0.021(8) 0.022(5) 0.010(6) C30 0.035(5) 0.141(11) 0.113(9) 0.000(8) 0.009(5) 0.016(5) C31 0.032(4) 0.112(8) 0.079(6) -0.004(6) -0.003(4) 0.013(5) C32 0.113(9) 0.085(8) 0.078(6) -0.024(6) -0.014(6) 0.042(7) C33 0.27(2) 0.040(7) 0.225(18) -0.017(9) -0.116(16) 0.023(9) C41 0.061(5) 0.060(6) 0.084(6) -0.023(5) 0.001(5) 0.006(4) C42 0.088(7) 0.060(6) 0.122(9) -0.032(6) 0.006(7) -0.005(5) C43 0.086(8) 0.065(7) 0.145(10) -0.030(7) -0.005(7) -0.014(6) C44 0.057(5) 0.064(6) 0.126(8) -0.013(6) -0.001(5) -0.016(5) C45 0.044(4) 0.058(5) 0.063(5) -0.005(4) -0.002(4) -0.004(4) C46 0.034(4) 0.067(5) 0.053(4) -0.005(4) -0.002(3) -0.008(4) C47 0.025(3) 0.092(7) 0.051(4) -0.011(4) 0.006(3) 0.004(4) C48 0.043(4) 0.084(6) 0.060(5) -0.002(5) 0.001(4) -0.008(4) C49 0.040(5) 0.144(11) 0.052(5) 0.006(6) -0.006(4) -0.008(6) C50 0.061(6) 0.100(8) 0.064(6) 0.011(6) -0.007(4) -0.003(6) C51 0.065(5) 0.081(7) 0.060(5) 0.004(5) -0.008(4) 0.022(5) C52 0.044(5) 0.115(9) 0.074(6) 0.036(6) 0.003(4) -0.003(5) C53 0.058(6) 0.29(2) 0.110(9) 0.090(11) 0.011(6) -0.019(9) C61 0.059(5) 0.072(6) 0.073(5) -0.006(5) 0.000(4) 0.029(5) C62 0.089(7) 0.060(6) 0.098(7) -0.010(6) 0.004(6) 0.029(6) C63 0.112(8) 0.049(6) 0.093(7) 0.014(5) 0.020(6) 0.024(6) C64 0.074(6) 0.056(6) 0.085(6) 0.007(5) 0.010(5) 0.010(5) C65 0.051(4) 0.039(4) 0.056(4) -0.001(3) 0.003(4) 0.014(3) C66 0.048(4) 0.057(5) 0.046(4) 0.000(4) -0.001(3) 0.011(4) C67 0.045(4) 0.053(5) 0.047(4) 0.004(3) 0.000(3) 0.003(3) C68 0.072(6) 0.075(6) 0.053(5) 0.010(4) 0.005(4) 0.009(5) C69 0.091(7) 0.089(8) 0.046(5) 0.011(5) -0.004(4) 0.014(6) C70 0.083(7) 0.106(9) 0.038(4) 0.001(5) -0.009(4) 0.008(6) C71 0.049(4) 0.086(6) 0.049(4) -0.014(4) 0.000(3) 0.003(4) C72 0.064(6) 0.071(6) 0.103(7) 0.007(6) 0.018(5) 0.005(5) C73 0.076(7) 0.098(9) 0.143(10) 0.002(8) 0.043(7) -0.005(6) Y2 0.1190(12) 0.0541(8) 0.0609(7) 0.000 -0.0196(7) 0.000 N11 0.145(10) 0.077(7) 0.069(6) -0.001(5) -0.020(6) -0.004(7) N12 0.106(8) 0.164(13) 0.101(8) 0.045(9) 0.028(6) 0.057(9) O11 0.220(13) 0.199(13) 0.227(13) -0.112(11) -0.144(11) 0.097(10) O12 0.161(9) 0.113(7) 0.114(7) -0.044(6) -0.043(6) 0.014(7) O13 0.114(7) 0.152(9) 0.100(6) 0.011(5) -0.042(5) -0.030(6) O14 0.148(8) 0.108(7) 0.133(7) 0.054(6) 0.049(6) 0.044(6) O15 0.170(10) 0.119(9) 0.195(11) -0.031(8) 0.078(8) 0.026(8) O16 0.126(8) 0.231(14) 0.170(10) 0.070(10) 0.058(7) 0.051(8) Cl 0.098(2) 0.132(3) 0.0754(17) -0.0067(18) -0.0034(15) 0.005(2) O6 0.33(2) 0.55(4) 0.174(13) -0.031(17) 0.037(13) 0.31(3) O7 0.40(3) 0.223(19) 0.49(4) 0.15(2) 0.00(3) -0.15(2) O8 0.185(11) 0.337(18) 0.083(6) -0.014(9) -0.016(6) 0.112(11) O9 0.287(16) 0.145(11) 0.320(18) -0.026(11) -0.234(15) 0.010(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O21 2.195(4) . ? Y1 O1 2.251(5) . ? Y1 OW1 2.347(5) . ? Y1 O3 2.368(6) . ? Y1 O61 2.419(4) . ? Y1 O4 2.469(6) . ? Y1 N1 2.549(6) . ? Y1 N21 2.562(6) . ? Y1 N3 2.865(8) . ? Y1 Ni1 3.4498(11) . ? Y1 Ni2 3.4725(11) . ? Ni1 O41 1.978(5) . ? Ni1 O21 2.025(5) . ? Ni1 N61 2.055(7) . ? Ni1 N22 2.068(6) . ? Ni1 N42 2.105(6) . ? Ni1 O61 2.258(5) . ? Ni2 O41 2.050(4) . ? Ni2 O1 2.058(4) . ? Ni2 N41 2.073(6) . ? Ni2 N62 2.106(6) . ? Ni2 O61 2.111(5) . ? Ni2 N2 2.118(6) . ? O1 C6 1.373(7) . ? O21 C26 1.378(8) . ? O41 C46 1.375(8) . ? O61 C66 1.379(9) . ? O3 N3 1.294(10) . ? O4 N3 1.254(9) . ? N1 C5 1.338(9) . ? N1 C1 1.351(10) . ? N2 C7 1.339(9) . ? N2 C11 1.346(9) . ? N21 C21 1.327(11) . ? N21 C25 1.344(10) . ? N22 C27 1.333(10) . ? N22 C31 1.350(10) . ? N41 C41 1.353(10) . ? N41 C45 1.366(9) . ? N42 C47 1.337(11) . ? N42 C51 1.347(10) . ? N61 C65 1.324(9) . ? N61 C61 1.334(10) . ? N62 C67 1.343(10) . ? N62 C71 1.350(9) . ? O5 N3 1.206(9) . ? O2 C6 1.423(8) . ? O2 C12 1.432(9) . ? O22 C32 1.427(12) . ? O22 C26 1.440(9) . ? O42 C46 1.447(8) . ? O42 C52 1.450(9) . ? O62 C72 1.420(10) . ? O62 C66 1.438(9) . ? C1 C2 1.370(12) . ? C1 H1 0.9500 . ? C2 C3 1.353(13) . ? C2 H2 0.9500 . ? C3 C4 1.407(11) . ? C3 H3 0.9500 . ? C4 C5 1.395(10) . ? C4 H4 0.9500 . ? C5 C6 1.524(9) . ? C6 C7 1.529(9) . ? C7 C8 1.372(9) . ? C8 C9 1.391(11) . ? C8 H8 0.9500 . ? C9 C10 1.360(12) . ? C9 H9 0.9500 . ? C10 C11 1.357(11) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.501(13) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 C22 1.368(13) . ? C21 H21 0.9500 . ? C22 C23 1.360(15) . ? C22 H22 0.9500 . ? C23 C24 1.393(15) . ? C23 H23 0.9500 . ? C24 C25 1.394(11) . ? C24 H24 0.9500 . ? C25 C26 1.509(11) . ? C26 C27 1.548(10) . ? C27 C28 1.393(11) . ? C28 C29 1.370(13) . ? C28 H28 0.9500 . ? C29 C30 1.356(14) . ? C29 H29 0.9500 . ? C30 C31 1.359(12) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.436(16) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C41 C42 1.359(13) . ? C41 H41 0.9500 . ? C42 C43 1.381(14) . ? C42 H42 0.9500 . ? C43 C44 1.356(14) . ? C43 H43 0.9500 . ? C44 C45 1.375(12) . ? C44 H44 0.9500 . ? C45 C46 1.517(11) . ? C46 C47 1.529(11) . ? C47 C48 1.394(11) . ? C48 C49 1.415(13) . ? C48 H48 0.9500 . ? C49 C50 1.339(14) . ? C49 H49 0.9500 . ? C50 C51 1.368(12) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C53 1.493(12) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C61 C62 1.380(13) . ? C61 H61 0.9500 . ? C62 C63 1.376(14) . ? C62 H62 0.9500 . ? C63 C64 1.375(12) . ? C63 H63 0.9500 . ? C64 C65 1.386(12) . ? C64 H64 0.9500 . ? C65 C66 1.546(10) . ? C66 C67 1.539(10) . ? C67 C68 1.391(10) . ? C68 C69 1.379(12) . ? C68 H68 0.9500 . ? C69 C70 1.368(14) . ? C69 H69 0.9500 . ? C70 C71 1.375(12) . ? C70 H70 0.9500 . ? C71 H71 0.9500 . ? C72 C73 1.486(13) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? Y2 O15 2.370(11) . ? Y2 O15 2.370(11) 6_656 ? Y2 O14 2.416(8) . ? Y2 O14 2.416(8) 6_656 ? Y2 O12 2.424(8) . ? Y2 O12 2.424(8) 6_656 ? Y2 O11 2.427(10) 6_656 ? Y2 O11 2.427(10) . ? Y2 O17 2.537(14) . ? Y2 O17 2.537(14) 6_656 ? Y2 N13 2.63(2) . ? Y2 N12 2.797(13) . ? N11 O13 1.191(12) . ? N11 O11 1.213(12) . ? N11 O12 1.225(12) . ? N12 O16 1.226(14) . ? N12 O15 1.231(15) . ? N12 O14 1.242(13) . ? N13 O17 1.200(14) . ? N13 O17 1.200(14) 6_656 ? N13 O18 1.28(6) . ? Cl O9 1.309(11) . ? Cl O7 1.322(17) . ? Cl O6 1.335(15) . ? Cl O8 1.353(9) . ? O1E O2W 1.17(2) . ? O1E C1E 1.46(4) . ? C1E C2E 1.09(4) . ? C1E O2W 1.68(4) . ? O2E C3E 1.28(4) . ? C3E C4E 1.21(4) . ? O3W O4W 1.07(5) 6_556 ? O3W O4W 1.07(5) . ? O5W O5W 1.49(8) 6_656 ? 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 O21 Y1 O1 105.68(17) . . ? O21 Y1 OW1 96.21(18) . . ? O1 Y1 OW1 139.57(19) . . ? O21 Y1 O3 134.2(2) . . ? O1 Y1 O3 104.7(2) . . ? OW1 Y1 O3 81.8(2) . . ? O21 Y1 O61 72.00(16) . . ? O1 Y1 O61 70.79(16) . . ? OW1 Y1 O61 149.44(19) . . ? O3 Y1 O61 86.77(19) . . ? O21 Y1 O4 82.80(19) . . ? O1 Y1 O4 140.74(18) . . ? OW1 Y1 O4 74.5(2) . . ? O3 Y1 O4 52.3(2) . . ? O61 Y1 O4 76.03(18) . . ? O21 Y1 N1 149.49(19) . . ? O1 Y1 N1 65.84(17) . . ? OW1 Y1 N1 77.98(19) . . ? O3 Y1 N1 75.2(2) . . ? O61 Y1 N1 126.14(17) . . ? O4 Y1 N1 123.1(2) . . ? O21 Y1 N21 66.15(19) . . ? O1 Y1 N21 85.2(2) . . ? OW1 Y1 N21 73.0(2) . . ? O3 Y1 N21 150.0(2) . . ? O61 Y1 N21 123.15(19) . . ? O4 Y1 N21 131.5(2) . . ? N1 Y1 N21 83.6(2) . . ? O21 Y1 N3 108.1(2) . . ? O1 Y1 N3 124.68(19) . . ? OW1 Y1 N3 77.5(2) . . ? O3 Y1 N3 26.5(2) . . ? O61 Y1 N3 79.70(18) . . ? O4 Y1 N3 25.84(19) . . ? N1 Y1 N3 99.9(2) . . ? N21 Y1 N3 148.9(2) . . ? O21 Y1 Ni1 33.56(12) . . ? O1 Y1 Ni1 81.47(11) . . ? OW1 Y1 Ni1 129.01(13) . . ? O3 Y1 Ni1 122.77(16) . . ? O61 Y1 Ni1 40.70(11) . . ? O4 Y1 Ni1 86.96(14) . . ? N1 Y1 Ni1 146.44(14) . . ? N21 Y1 Ni1 86.38(15) . . ? N3 Y1 Ni1 105.06(16) . . ? O21 Y1 Ni2 85.47(13) . . ? O1 Y1 Ni2 34.46(11) . . ? OW1 Y1 Ni2 173.68(15) . . ? O3 Y1 Ni2 101.42(16) . . ? O61 Y1 Ni2 36.79(11) . . ? O4 Y1 Ni2 111.74(14) . . ? N1 Y1 Ni2 97.48(14) . . ? N21 Y1 Ni2 102.26(16) . . ? N3 Y1 Ni2 107.85(14) . . ? Ni1 Y1 Ni2 53.69(2) . . ? O41 Ni1 O21 98.0(2) . . ? O41 Ni1 N61 153.8(2) . . ? O21 Ni1 N61 91.3(2) . . ? O41 Ni1 N22 103.3(2) . . ? O21 Ni1 N22 79.4(2) . . ? N61 Ni1 N22 102.4(3) . . ? O41 Ni1 N42 78.3(2) . . ? O21 Ni1 N42 171.6(2) . . ? N61 Ni1 N42 95.2(3) . . ? N22 Ni1 N42 94.0(3) . . ? O41 Ni1 O61 80.16(17) . . ? O21 Ni1 O61 78.57(17) . . ? N61 Ni1 O61 77.8(2) . . ? N22 Ni1 O61 158.0(2) . . ? N42 Ni1 O61 108.0(2) . . ? O41 Ni1 Y1 79.15(13) . . ? O21 Ni1 Y1 36.81(13) . . ? N61 Ni1 Y1 94.53(17) . . ? N22 Ni1 Y1 114.39(19) . . ? N42 Ni1 Y1 147.14(18) . . ? O61 Ni1 Y1 44.32(11) . . ? O41 Ni2 O1 86.82(17) . . ? O41 Ni2 N41 79.5(2) . . ? O1 Ni2 N41 108.5(2) . . ? O41 Ni2 N62 102.6(2) . . ? O1 Ni2 N62 154.1(2) . . ? N41 Ni2 N62 96.9(2) . . ? O41 Ni2 O61 82.22(19) . . ? O1 Ni2 O61 81.04(18) . . ? N41 Ni2 O61 158.7(2) . . ? N62 Ni2 O61 76.5(2) . . ? O41 Ni2 N2 161.6(2) . . ? O1 Ni2 N2 78.72(19) . . ? N41 Ni2 N2 94.3(2) . . ? N62 Ni2 N2 95.3(2) . . ? O61 Ni2 N2 106.4(2) . . ? O41 Ni2 Y1 77.77(13) . . ? O1 Ni2 Y1 38.25(13) . . ? N41 Ni2 Y1 140.17(17) . . ? N62 Ni2 Y1 119.68(18) . . ? O61 Ni2 Y1 43.34(12) . . ? N2 Ni2 Y1 97.12(16) . . ? C6 O1 Ni2 111.6(4) . . ? C6 O1 Y1 126.5(4) . . ? Ni2 O1 Y1 107.3(2) . . ? C26 O21 Ni1 118.0(4) . . ? C26 O21 Y1 124.8(4) . . ? Ni1 O21 Y1 109.6(2) . . ? C46 O41 Ni1 115.6(4) . . ? C46 O41 Ni2 111.5(4) . . ? Ni1 O41 Ni2 101.8(2) . . ? C66 O61 Ni2 117.8(4) . . ? C66 O61 Ni1 104.0(4) . . ? Ni2 O61 Ni1 91.31(18) . . ? C66 O61 Y1 136.8(4) . . ? Ni2 O61 Y1 99.87(18) . . ? Ni1 O61 Y1 94.99(16) . . ? N3 O3 Y1 98.7(5) . . ? N3 O4 Y1 95.0(5) . . ? C5 N1 C1 116.9(7) . . ? C5 N1 Y1 115.9(4) . . ? C1 N1 Y1 127.0(6) . . ? C7 N2 C11 118.0(6) . . ? C7 N2 Ni2 112.8(4) . . ? C11 N2 Ni2 128.6(5) . . ? C21 N21 C25 118.6(7) . . ? C21 N21 Y1 127.0(6) . . ? C25 N21 Y1 114.3(5) . . ? C27 N22 C31 117.8(7) . . ? C27 N22 Ni1 114.6(5) . . ? C31 N22 Ni1 127.1(6) . . ? C41 N41 C45 118.5(7) . . ? C41 N41 Ni2 129.0(5) . . ? C45 N41 Ni2 112.4(5) . . ? C47 N42 C51 118.7(7) . . ? C47 N42 Ni1 113.1(5) . . ? C51 N42 Ni1 127.6(6) . . ? C65 N61 C61 119.2(7) . . ? C65 N61 Ni1 115.6(5) . . ? C61 N61 Ni1 124.7(6) . . ? C67 N62 C71 117.9(7) . . ? C67 N62 Ni2 116.5(5) . . ? C71 N62 Ni2 125.5(6) . . ? C6 O2 C12 115.3(5) . . ? C32 O22 C26 115.1(6) . . ? C46 O42 C52 114.2(5) . . ? C72 O62 C66 117.9(6) . . ? O5 N3 O4 125.4(9) . . ? O5 N3 O3 120.7(8) . . ? O4 N3 O3 113.9(7) . . ? O5 N3 Y1 175.4(7) . . ? O4 N3 Y1 59.2(4) . . ? O3 N3 Y1 54.8(4) . . ? N1 C1 C2 124.3(9) . . ? N1 C1 H1 117.8 . . ? C2 C1 H1 117.8 . . ? C3 C2 C1 118.4(8) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 119.9(8) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 117.7(8) . . ? C5 C4 H4 121.2 . . ? C3 C4 H4 121.2 . . ? N1 C5 C4 122.7(7) . . ? N1 C5 C6 115.9(6) . . ? C4 C5 C6 121.4(7) . . ? O1 C6 O2 113.2(5) . . ? O1 C6 C5 109.9(5) . . ? O2 C6 C5 109.6(6) . . ? O1 C6 C7 109.4(5) . . ? O2 C6 C7 102.5(5) . . ? C5 C6 C7 112.1(5) . . ? N2 C7 C8 121.6(6) . . ? N2 C7 C6 113.7(5) . . ? C8 C7 C6 124.6(6) . . ? C7 C8 C9 118.8(7) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C10 C9 C8 119.8(7) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 118.1(8) . . ? C11 C10 H10 121.0 . . ? C9 C10 H10 121.0 . . ? N2 C11 C10 123.7(8) . . ? N2 C11 H11 118.2 . . ? C10 C11 H11 118.2 . . ? O2 C12 C13 106.4(7) . . ? O2 C12 H12A 110.4 . . ? C13 C12 H12A 110.4 . . ? O2 C12 H12B 110.4 . . ? C13 C12 H12B 110.4 . . ? H12A C12 H12B 108.6 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N21 C21 C22 125.0(10) . . ? N21 C21 H21 117.5 . . ? C22 C21 H21 117.5 . . ? C23 C22 C21 116.8(11) . . ? C23 C22 H22 121.6 . . ? C21 C22 H22 121.6 . . ? C22 C23 C24 120.4(10) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C25 118.9(10) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? N21 C25 C24 120.2(9) . . ? N21 C25 C26 114.9(6) . . ? C24 C25 C26 124.7(8) . . ? O21 C26 O22 111.4(6) . . ? O21 C26 C25 110.6(6) . . ? O22 C26 C25 102.6(6) . . ? O21 C26 C27 109.0(6) . . ? O22 C26 C27 109.4(6) . . ? C25 C26 C27 113.9(6) . . ? N22 C27 C28 122.1(8) . . ? N22 C27 C26 116.4(6) . . ? C28 C27 C26 121.5(8) . . ? C29 C28 C27 118.3(9) . . ? C29 C28 H28 120.8 . . ? C27 C28 H28 120.8 . . ? C30 C29 C28 119.7(9) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 119.5(9) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? N22 C31 C30 122.5(9) . . ? N22 C31 H31 118.8 . . ? C30 C31 H31 118.8 . . ? O22 C32 C33 110.5(9) . . ? O22 C32 H32A 109.6 . . ? C33 C32 H32A 109.6 . . ? O22 C32 H32B 109.6 . . ? C33 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N41 C41 C42 122.0(9) . . ? N41 C41 H41 119.0 . . ? C42 C41 H41 119.0 . . ? C41 C42 C43 119.1(10) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C44 C43 C42 119.7(9) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 119.9(9) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? N41 C45 C44 120.7(8) . . ? N41 C45 C46 114.9(7) . . ? C44 C45 C46 124.2(7) . . ? O41 C46 O42 112.8(6) . . ? O41 C46 C45 109.5(6) . . ? O42 C46 C45 108.7(6) . . ? O41 C46 C47 110.5(7) . . ? O42 C46 C47 103.2(5) . . ? C45 C46 C47 112.1(6) . . ? N42 C47 C48 122.3(8) . . ? N42 C47 C46 114.4(6) . . ? C48 C47 C46 123.3(9) . . ? C47 C48 C49 116.8(9) . . ? C47 C48 H48 121.6 . . ? C49 C48 H48 121.6 . . ? C50 C49 C48 120.1(9) . . ? C50 C49 H49 119.9 . . ? C48 C49 H49 119.9 . . ? C49 C50 C51 119.8(9) . . ? C49 C50 H50 120.1 . . ? C51 C50 H50 120.1 . . ? N42 C51 C50 122.2(10) . . ? N42 C51 H51 118.9 . . ? C50 C51 H51 118.9 . . ? O42 C52 C53 108.1(7) . . ? O42 C52 H52A 110.1 . . ? C53 C52 H52A 110.1 . . ? O42 C52 H52B 110.1 . . ? C53 C52 H52B 110.1 . . ? H52A C52 H52B 108.4 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N61 C61 C62 122.2(9) . . ? N61 C61 H61 118.9 . . ? C62 C61 H61 118.9 . . ? C63 C62 C61 118.0(9) . . ? C63 C62 H62 121.0 . . ? C61 C62 H62 121.0 . . ? C64 C63 C62 120.3(9) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.9 . . ? C63 C64 C65 117.8(9) . . ? C63 C64 H64 121.1 . . ? C65 C64 H64 121.1 . . ? N61 C65 C64 122.4(7) . . ? N61 C65 C66 115.1(7) . . ? C64 C65 C66 122.4(7) . . ? O61 C66 O62 113.7(6) . . ? O61 C66 C67 109.3(6) . . ? O62 C66 C67 108.4(6) . . ? O61 C66 C65 110.0(6) . . ? O62 C66 C65 104.1(6) . . ? C67 C66 C65 111.2(6) . . ? N62 C67 C68 122.0(7) . . ? N62 C67 C66 116.4(6) . . ? C68 C67 C66 121.6(7) . . ? C69 C68 C67 119.7(9) . . ? C69 C68 H68 120.1 . . ? C67 C68 H68 120.1 . . ? C70 C69 C68 117.7(8) . . ? C70 C69 H69 121.1 . . ? C68 C69 H69 121.1 . . ? C69 C70 C71 120.8(9) . . ? C69 C70 H70 119.6 . . ? C71 C70 H70 119.6 . . ? N62 C71 C70 121.8(9) . . ? N62 C71 H71 119.1 . . ? C70 C71 H71 119.1 . . ? O62 C72 C73 110.9(8) . . ? O62 C72 H72A 109.5 . . ? C73 C72 H72A 109.5 . . ? O62 C72 H72B 109.5 . . ? C73 C72 H72B 109.5 . . ? H72A C72 H72B 108.0 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? O15 Y2 O15 173.7(6) . 6_656 ? O15 Y2 O14 52.2(4) . . ? O15 Y2 O14 121.5(4) 6_656 . ? O15 Y2 O14 121.5(4) . 6_656 ? O15 Y2 O14 52.2(4) 6_656 6_656 ? O14 Y2 O14 70.6(5) . 6_656 ? O15 Y2 O12 79.0(4) . . ? O15 Y2 O12 103.2(4) 6_656 . ? O14 Y2 O12 93.7(4) . . ? O14 Y2 O12 119.1(4) 6_656 . ? O15 Y2 O12 103.2(4) . 6_656 ? O15 Y2 O12 79.0(4) 6_656 6_656 ? O14 Y2 O12 119.1(4) . 6_656 ? O14 Y2 O12 93.7(4) 6_656 6_656 ? O12 Y2 O12 140.5(5) . 6_656 ? O15 Y2 O11 74.8(5) . 6_656 ? O15 Y2 O11 102.9(5) 6_656 6_656 ? O14 Y2 O11 70.5(4) . 6_656 ? O14 Y2 O11 76.3(5) 6_656 6_656 ? O12 Y2 O11 153.8(5) . 6_656 ? O12 Y2 O11 48.6(3) 6_656 6_656 ? O15 Y2 O11 102.9(5) . . ? O15 Y2 O11 74.8(5) 6_656 . ? O14 Y2 O11 76.3(5) . . ? O14 Y2 O11 70.5(4) 6_656 . ? O12 Y2 O11 48.6(3) . . ? O12 Y2 O11 153.8(5) 6_656 . ? O11 Y2 O11 139.0(7) 6_656 . ? O15 Y2 O17 68.0(4) . . ? O15 Y2 O17 118.3(4) 6_656 . ? O14 Y2 O17 120.1(4) . . ? O14 Y2 O17 162.8(4) 6_656 . ? O12 Y2 O17 75.4(4) . . ? O12 Y2 O17 69.5(4) 6_656 . ? O11 Y2 O17 94.2(5) 6_656 . ? O11 Y2 O17 123.5(4) . . ? O15 Y2 O17 118.3(4) . 6_656 ? O15 Y2 O17 68.0(4) 6_656 6_656 ? O14 Y2 O17 162.8(4) . 6_656 ? O14 Y2 O17 120.1(4) 6_656 6_656 ? O12 Y2 O17 69.5(4) . 6_656 ? O12 Y2 O17 75.4(4) 6_656 6_656 ? O11 Y2 O17 123.5(4) 6_656 6_656 ? O11 Y2 O17 94.2(5) . 6_656 ? O17 Y2 O17 53.6(6) . 6_656 ? O15 Y2 N13 93.2(3) . . ? O15 Y2 N13 93.2(3) 6_656 . ? O14 Y2 N13 144.7(2) . . ? O14 Y2 N13 144.7(2) 6_656 . ? O12 Y2 N13 70.3(3) . . ? O12 Y2 N13 70.3(3) 6_656 . ? O11 Y2 N13 110.5(3) 6_656 . ? O11 Y2 N13 110.5(3) . . ? O17 Y2 N13 26.8(3) . . ? O17 Y2 N13 26.8(3) 6_656 . ? O15 Y2 N12 25.9(3) . . ? O15 Y2 N12 147.8(5) 6_656 . ? O14 Y2 N12 26.3(3) . . ? O14 Y2 N12 96.1(5) 6_656 . ? O12 Y2 N12 86.6(4) . . ? O12 Y2 N12 112.7(3) 6_656 . ? O11 Y2 N12 70.0(4) 6_656 . ? O11 Y2 N12 90.2(5) . . ? O17 Y2 N12 93.9(5) . . ? O17 Y2 N12 142.8(5) 6_656 . ? N13 Y2 N12 118.9(3) . . ? O13 N11 O11 124.2(13) . . ? O13 N11 O12 125.8(11) . . ? O11 N11 O12 110.0(11) . . ? O13 N11 Y2 179.1(10) . . ? O11 N11 Y2 55.0(7) . . ? O12 N11 Y2 55.0(6) . . ? O16 N12 O15 123.1(15) . . ? O16 N12 O14 120.1(16) . . ? O15 N12 O14 116.7(13) . . ? O16 N12 Y2 175.1(11) . . ? O15 N12 Y2 57.3(7) . . ? O14 N12 Y2 59.5(7) . . ? N11 O11 Y2 100.8(9) . . ? N11 O12 Y2 100.6(7) . . ? N12 O14 Y2 94.2(8) . . ? N12 O15 Y2 96.8(8) . . ? O17 N13 O17 145(3) . 6_656 ? O17 N13 O18 107.7(14) . . ? O17 N13 O18 107.7(14) 6_656 . ? O17 N13 Y2 72.3(14) . . ? O17 N13 Y2 72.3(14) 6_656 . ? O18 N13 Y2 180.000(8) . . ? N13 O17 Y2 80.9(15) . . ? O9 Cl O7 99.0(12) . . ? O9 Cl O6 108.3(13) . . ? O7 Cl O6 121.9(17) . . ? O9 Cl O8 113.2(11) . . ? O7 Cl O8 107.6(15) . . ? O6 Cl O8 106.9(9) . . ? O2W O1E C1E 79(2) . . ? C2E C1E O1E 138(4) . . ? C2E C1E O2W 95(4) . . ? O1E C1E O2W 43.0(14) . . ? C4E C3E O2E 122(4) . . ? O1E O2W C1E 58.0(18) . . ? O4W O3W O4W 132(10) 6_556 . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.860 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.086 # start Validation Reply Form _vrf_PLAT029_peng63a1 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.93 RESPONSE: The data used for the refinement were cut off at 2theta=48 deg because the data at higher 2theta values were more than 50% unobserved. Moreover, some reflections were omitted as most disagreable. However, the ratio of the reflections used to the number of parameters refined is more than 10 to 1, in agreement with the crystallographic criteria. ; _vrf_PLAT241_peng63a1 ; PROBLEM: Check High Ueq as Compared to Neighbors for O11 RESPONSE: This is probably a false alert due to the smaller thermal motion of the neighboring atoms. ; _vrf_PLAT242_peng63a1 ; PROBLEM: Check Low Ueq as Compared to Neighbors for Y2 RESPONSE: This is probably a false alert due to the larger thermal motion of the neighboring atoms. ; _vrf_PLAT430_peng63a1 ; PROBLEM: Short Inter D...A Contact O4W .. O4W .. 1.95 Ang. RESPONSE: Solvate water and EtOH molecules were refined with occupation factor less than one; thus there is no contradiction regarding the short intermolecular distance above. ; # end Validation Reply Form