# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_peen31a _database_code_depnum_ccdc_archive 'CCDC 896963' #TrackingRef 'Dalton Perlepes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43.20 H51 Ce Cl2 N12 Ni O15.80' _chemical_formula_weight 1260.89 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' Ce Ce -1.8482 9.6596 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 15.7565(2) _cell_length_b 26.1310(4) _cell_length_c 26.5276(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.6630(10) _cell_angle_gamma 90.00 _cell_volume 10516.7(3) _cell_formula_units_Z 8 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 61500 _cell_measurement_theta_min 6.52 _cell_measurement_theta_max 72.08 _exptl_crystal_description parallelepiped _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5125 _exptl_absorpt_coefficient_mu 8.652 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.431 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'CrystalClear, Rigaku MSC, 2005' _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 71053 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.0721 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 6.56 _diffrn_reflns_theta_max 65.00 _reflns_number_total 17408 _reflns_number_gt 14453 _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0931P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17408 _refine_ls_number_parameters 1401 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0673 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1580 _refine_ls_wR_factor_gt 0.1493 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.004 _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 Ni1 Ni 0.19839(4) 0.59536(3) 0.40715(3) 0.02489(18) Uani 1 1 d . . . Ce1 Ce 0.214777(16) 0.446505(11) 0.427474(10) 0.02563(7) Uani 1 1 d . . . N1 N 0.2665(2) 0.63180(14) 0.35987(13) 0.0265(9) Uani 1 1 d . . . N2 N 0.1914(2) 0.54246(14) 0.34887(14) 0.0277(9) Uani 1 1 d . . . N11 N 0.2397(2) 0.64672(14) 0.46878(13) 0.0265(9) Uani 1 1 d . . . N12 N 0.3059(2) 0.55950(14) 0.45423(14) 0.0276(9) Uani 1 1 d . . . N21 N 0.0782(2) 0.63032(15) 0.37122(13) 0.0288(9) Uani 1 1 d . . . N22 N 0.1113(2) 0.55286(14) 0.43496(13) 0.0264(9) Uani 1 1 d . . . N31 N 0.1237(2) 0.37687(15) 0.47060(14) 0.0310(10) Uani 1 1 d . . . N32 N 0.0418(2) 0.43072(15) 0.38756(15) 0.0356(10) Uani 1 1 d . . . N41 N 0.3473(2) 0.38725(15) 0.48332(14) 0.0303(9) Uani 1 1 d . . . N42 N 0.2813(2) 0.45963(15) 0.53119(15) 0.0313(10) Uani 1 1 d . . . N51 N 0.2012(2) 0.37037(15) 0.35544(14) 0.0318(10) Uani 1 1 d . . . N52 N 0.3274(2) 0.44012(15) 0.36608(14) 0.0299(9) Uani 1 1 d . . . O1 O 0.15420(18) 0.49522(12) 0.34769(11) 0.0316(8) Uani 1 1 d . . . O11 O 0.33028(17) 0.51119(12) 0.44454(11) 0.0280(7) Uani 1 1 d . . . O21 O 0.13552(18) 0.51047(11) 0.46537(11) 0.0286(7) Uani 1 1 d . . . O31 O -0.0009(2) 0.45931(15) 0.34458(14) 0.0516(11) Uani 1 1 d . . . H31O H 0.0341 0.4811 0.3382 0.067 Uiso 1 1 calc R . . O41 O 0.2485(2) 0.49915(12) 0.55557(12) 0.0366(8) Uani 1 1 d . . . O51 O 0.39404(19) 0.47586(12) 0.37252(12) 0.0363(8) Uani 1 1 d . . . C1 C 0.3067(3) 0.67733(19) 0.36710(17) 0.0328(12) Uani 1 1 d . . . H1 H 0.2988 0.6982 0.3948 0.046 Uiso 1 1 calc R . . C2 C 0.3589(3) 0.6960 0.33702(18) 0.0384(13) Uani 1 1 d . . . H2 H 0.3864 0.7285 0.3437 0.054 Uiso 1 1 calc R . . C3 C 0.3692(3) 0.6651(2) 0.29657(18) 0.0426(14) Uani 1 1 d . . . H3 H 0.4061 0.6758 0.2755 0.060 Uiso 1 1 calc R . . C4 C 0.3261(3) 0.6195(2) 0.28729(19) 0.0376(13) Uani 1 1 d . . . H4 H 0.3312 0.5986 0.2589 0.053 Uiso 1 1 calc R . . C5 C 0.2749(3) 0.60349(18) 0.31932(16) 0.0280(11) Uani 1 1 d . . . C6 C 0.2278(3) 0.55397(18) 0.31191(17) 0.0277(11) Uani 1 1 d . . . C7 C 0.2237(3) 0.5209(2) 0.26514(18) 0.0414(13) Uani 1 1 d . . . H7A H 0.1854 0.4914 0.2655 0.062 Uiso 1 1 calc R . . H7B H 0.2831 0.5088 0.2663 0.062 Uiso 1 1 calc R . . H7C H 0.2001 0.5408 0.2331 0.062 Uiso 1 1 calc R . . C11 C 0.2036(3) 0.69221(19) 0.47603(19) 0.0345(12) Uani 1 1 d . . . H11 H 0.1510 0.7027 0.4511 0.048 Uiso 1 1 calc R . . C12 C 0.2395(3) 0.7245(2) 0.5182(2) 0.0451(14) Uani 1 1 d . . . H12 H 0.2122 0.7561 0.5220 0.063 Uiso 1 1 calc R . . C13 C 0.3154(3) 0.7093(2) 0.55404(19) 0.0449(14) Uani 1 1 d . . . H13 H 0.3409 0.7300 0.5836 0.063 Uiso 1 1 calc R . . C14 C 0.3545(3) 0.6639(2) 0.54695(19) 0.0413(13) Uani 1 1 d . . . H14 H 0.4083 0.6537 0.5710 0.058 Uiso 1 1 calc R . . C15 C 0.3157(3) 0.63299(18) 0.50491(16) 0.0286(11) Uani 1 1 d . . . C16 C 0.3514(3) 0.58293(18) 0.49560(16) 0.0282(11) Uani 1 1 d . . . C17 C 0.4316(3) 0.56032(19) 0.53308(18) 0.0373(13) Uani 1 1 d . . . H17A H 0.4453 0.5273 0.5196 0.056 Uiso 1 1 calc R . . H17B H 0.4202 0.5552 0.5673 0.056 Uiso 1 1 calc R . . H17C H 0.4816 0.5836 0.5369 0.056 Uiso 1 1 calc R . . C21 C 0.0639(3) 0.66999(19) 0.33762(17) 0.0327(12) Uani 1 1 d . . . H21 H 0.1133 0.6866 0.3308 0.046 Uiso 1 1 calc R . . C22 C -0.0198(3) 0.68757(19) 0.31263(17) 0.0365(13) Uani 1 1 d . . . H22 H -0.0278 0.7155 0.2889 0.051 Uiso 1 1 calc R . . C23 C -0.0910(3) 0.66358(19) 0.32289(18) 0.0364(13) Uani 1 1 d . . . H23 H -0.1492 0.6742 0.3056 0.051 Uiso 1 1 calc R . . C24 C -0.0771(3) 0.62387(19) 0.35856(17) 0.0331(12) Uani 1 1 d . . . H24 H -0.1258 0.6080 0.3670 0.046 Uiso 1 1 calc R . . C25 C 0.0086(3) 0.60695(17) 0.38230(16) 0.0268(11) Uani 1 1 d . . . C26 C 0.0283(3) 0.56437(18) 0.41852(16) 0.0268(11) Uani 1 1 d . . . C27 C -0.0431(3) 0.5352(2) 0.43318(19) 0.0396(13) Uani 1 1 d . . . H27A H -0.0177 0.5054 0.4542 0.059 Uiso 1 1 calc R . . H27B H -0.0868 0.5239 0.4014 0.059 Uiso 1 1 calc R . . H27C H -0.0716 0.5574 0.4536 0.059 Uiso 1 1 calc R . . C31 C 0.1633(3) 0.34745(19) 0.51272(19) 0.0388(13) Uani 1 1 d . . . H31 H 0.2257 0.3489 0.5252 0.054 Uiso 1 1 calc R . . C32 C 0.1197(3) 0.3162(2) 0.53812(19) 0.0422(14) Uani 1 1 d . . . H32 H 0.1512 0.2964 0.5671 0.059 Uiso 1 1 calc R . . C33 C 0.0304(3) 0.3139(2) 0.5215(2) 0.0431(14) Uani 1 1 d . . . H33 H -0.0017 0.2927 0.5390 0.060 Uiso 1 1 calc R . . C34 C -0.0130(3) 0.3426(2) 0.4786(2) 0.0431(14) Uani 1 1 d . . . H34 H -0.0754 0.3414 0.4662 0.060 Uiso 1 1 calc R . . C35 C 0.0350(3) 0.37339(19) 0.45377(18) 0.0331(12) Uani 1 1 d . . . C36 C -0.0108(3) 0.4041(2) 0.4072(2) 0.0407(13) Uani 1 1 d . . . C37 C -0.1076(3) 0.4018 0.3854(2) 0.0596(18) Uani 1 1 d . . . H37A H -0.1252 0.4232 0.3540 0.089 Uiso 1 1 calc R . . H37B H -0.1363 0.4143 0.4116 0.089 Uiso 1 1 calc R . . H37C H -0.1256 0.3663 0.3763 0.089 Uiso 1 1 calc R . . C41 C 0.3764(3) 0.34878(18) 0.45989(18) 0.0329(12) Uani 1 1 d . . . H41 H 0.3476 0.3423 0.4241 0.046 Uiso 1 1 calc R . . C42 C 0.4467(3) 0.31735(19) 0.48467(19) 0.0371(13) Uani 1 1 d . . . H42 H 0.4652 0.2898 0.4667 0.052 Uiso 1 1 calc R . . C43 C 0.4885(3) 0.3280(2) 0.5367(2) 0.0452(14) Uani 1 1 d . . . H43 H 0.5374 0.3079 0.5551 0.063 Uiso 1 1 calc R . . C44 C 0.4591(3) 0.3677(2) 0.56170(19) 0.0399(13) Uani 1 1 d . . . H44 H 0.4878 0.3752 0.5973 0.056 Uiso 1 1 calc R . . C45 C 0.3879(3) 0.39643(18) 0.53495(17) 0.0308(12) Uani 1 1 d . . . C46 C 0.3518(3) 0.43780(19) 0.56064(18) 0.0313(12) Uani 1 1 d . . . C47 C 0.3966(3) 0.45338(19) 0.61547(18) 0.0392(13) Uani 1 1 d . . . H47A H 0.3647 0.4820 0.6256 0.059 Uiso 1 1 calc R . . H47B H 0.4572 0.4639 0.6177 0.059 Uiso 1 1 calc R . . H47C H 0.3975 0.4244 0.6391 0.059 Uiso 1 1 calc R . . C51 C 0.1366(3) 0.3357(2) 0.34831(19) 0.0419(14) Uani 1 1 d . . . H51 H 0.1039 0.3339 0.3736 0.059 Uiso 1 1 calc R . . C52 C 0.1144(4) 0.3023(3) 0.3063(2) 0.071(2) Uani 1 1 d . . . H52 H 0.0696 0.2774 0.3037 0.100 Uiso 1 1 calc R . . C53 C 0.1590(4) 0.3061(3) 0.2685(3) 0.083(2) Uani 1 1 d . . . H53 H 0.1433 0.2849 0.2383 0.116 Uiso 1 1 calc R . . C54 C 0.2274(4) 0.3413(2) 0.2747(2) 0.0582(17) Uani 1 1 d . . . H54 H 0.2600 0.3436 0.2495 0.082 Uiso 1 1 calc R . . C55 C 0.2473(3) 0.3732(2) 0.31878(18) 0.0391(13) Uani 1 1 d . . . C56 C 0.3201(3) 0.41071(19) 0.32723(18) 0.0327(12) Uani 1 1 d . . . C57 C 0.3778(3) 0.4122(2) 0.2907(2) 0.0467(14) Uani 1 1 d . . . H57A H 0.4218 0.4395 0.3016 0.070 Uiso 1 1 calc R . . H57B H 0.3417 0.4190 0.2551 0.070 Uiso 1 1 calc R . . H57C H 0.4078 0.3793 0.2917 0.070 Uiso 1 1 calc R . . Ni2 Ni 0.27634(5) 0.60517(3) 0.09944(3) 0.02834(19) Uani 1 1 d . . . Ce2 Ce 0.289679(16) 0.458813(11) 0.063836(10) 0.02746(7) Uani 1 1 d . . . N61 N 0.2402(2) 0.66169(15) 0.04193(15) 0.0331(10) Uani 1 1 d . . . N62 N 0.3297(2) 0.57796(15) 0.04215(15) 0.0305(10) Uani 1 1 d . . . N71 N 0.3861(2) 0.64499(15) 0.14359(14) 0.0318(10) Uani 1 1 d . . . N72 N 0.3399(2) 0.54955(15) 0.15070(14) 0.0277(9) Uani 1 1 d . . . N81 N 0.1915(2) 0.63137(15) 0.14284(14) 0.0309(9) Uani 1 1 d . . . N82 N 0.1687(2) 0.55906(15) 0.07298(14) 0.0291(9) Uani 1 1 d . . . N91 N 0.3626(2) 0.41053(16) -0.00451(14) 0.0331(10) Uani 1 1 d . . . N92 N 0.2342(2) 0.47806(15) -0.03862(15) 0.0328(10) Uani 1 1 d . . . N101 N 0.1668(2) 0.38433(15) 0.02389(15) 0.0337(10) Uani 1 1 d . . . N102 N 0.1672(3) 0.43208(16) 0.11230(16) 0.0367(10) Uani 1 1 d . . . O61 O 0.37062(18) 0.53210(12) 0.04513(12) 0.0304(8) Uani 1 1 d . . . O71 O 0.31157(19) 0.50038(12) 0.14947(11) 0.0334(8) Uani 1 1 d . . . O81 O 0.16667(18) 0.51957(12) 0.03937(12) 0.0320(8) Uani 1 1 d . . . O91 O 0.1678(2) 0.51383(13) -0.05658(12) 0.0392(9) Uani 1 1 d . . . O95 O 0.1695(2) 0.45641(13) 0.15900(14) 0.0465(10) Uani 1 1 d . . . C61 C 0.1963(3) 0.70540(19) 0.0432(2) 0.0365(13) Uani 1 1 d . . . H61 H 0.1815 0.7138 0.0746 0.051 Uiso 1 1 calc R . . C62 C 0.1712(4) 0.7388(2) 0.0017(2) 0.0579(17) Uani 1 1 d . . . H62 H 0.1402 0.7694 0.0045 0.081 Uiso 1 1 calc R . . C63 C 0.1924(4) 0.7265(3) -0.0438(3) 0.076(2) Uani 1 1 d . . . H63 H 0.1737 0.7479 -0.0737 0.107 Uiso 1 1 calc R . . C64 C 0.2416(4) 0.6823(2) -0.0458(2) 0.0569(17) Uani 1 1 d . . . H64 H 0.2591 0.6741 -0.0764 0.080 Uiso 1 1 calc R . . C65 C 0.2639(3) 0.6511(2) -0.0027(2) 0.0376(13) Uani 1 1 d . . . C66 C 0.3147(3) 0.60321(18) -0.00188(17) 0.0305(12) Uani 1 1 d . . . C67 C 0.3419(3) 0.5860(2) -0.04874(18) 0.0396(13) Uani 1 1 d . . . H67A H 0.3831 0.5573 -0.0391 0.059 Uiso 1 1 calc R . . H67B H 0.3708 0.6144 -0.0618 0.059 Uiso 1 1 calc R . . H67C H 0.2898 0.5752 -0.0761 0.059 Uiso 1 1 calc R . . C71 C 0.4066(3) 0.6935(2) 0.1390(2) 0.0395(13) Uani 1 1 d . . . H71 H 0.3664 0.7142 0.1143 0.055 Uiso 1 1 calc R . . C72 C 0.4833(3) 0.7152(2) 0.1685(2) 0.0450(14) Uani 1 1 d . . . H72 H 0.4952 0.7505 0.1647 0.063 Uiso 1 1 calc R . . C73 C 0.5429(3) 0.6847(2) 0.2039(2) 0.0479(15) Uani 1 1 d . . . H73 H 0.5977 0.6984 0.2237 0.067 Uiso 1 1 calc R . . C74 C 0.5219(3) 0.6341(2) 0.21010(18) 0.0401(13) Uani 1 1 d . . . H74 H 0.5609 0.6129 0.2350 0.056 Uiso 1 1 calc R . . C75 C 0.4432(3) 0.61490(19) 0.17946(16) 0.0306(12) Uani 1 1 d . . . C76 C 0.4149(3) 0.56091(19) 0.18332(17) 0.0288(11) Uani 1 1 d . . . C77 C 0.4712(3) 0.5240(2) 0.22186(19) 0.0441(14) Uani 1 1 d . . . C81 C 0.2060(3) 0.66800(19) 0.17904(18) 0.0342(12) Uani 1 1 d . . . H81 H 0.2602 0.6861 0.1864 0.048 Uiso 1 1 calc R . . C82 C 0.1455(3) 0.6810(2) 0.20655(18) 0.0392(13) Uani 1 1 d . . . H82 H 0.1584 0.7071 0.2324 0.055 Uiso 1 1 calc R . . C83 C 0.0675(3) 0.6554(2) 0.19557(19) 0.0398(13) Uani 1 1 d . . . H83 H 0.0252 0.6632 0.2140 0.056 Uiso 1 1 calc R . . C84 C 0.0503(3) 0.6178(2) 0.15700(19) 0.0392(13) Uani 1 1 d . . . H84 H -0.0044 0.6001 0.1484 0.055 Uiso 1 1 calc R . . C85 C 0.1138(3) 0.60629(19) 0.13122(19) 0.0327(12) Uani 1 1 d . . . C86 C 0.1013(3) 0.56567(18) 0.09172(17) 0.0291(11) Uani 1 1 d . . . C87 C 0.0193(3) 0.5343(2) 0.0764(2) 0.0421(14) Uani 1 1 d . . . H87A H 0.0243 0.5091 0.0500 0.063 Uiso 1 1 calc R . . H87B H -0.0313 0.5566 0.0619 0.063 Uiso 1 1 calc R . . H87C H 0.0111 0.5165 0.1073 0.063 Uiso 1 1 calc R . . C91 C 0.4263(3) 0.3758(2) 0.0116(2) 0.0391(13) Uani 1 1 d . . . H91 H 0.4433 0.3673 0.0478 0.055 Uiso 1 1 calc R . . C92 C 0.4689(3) 0.3517(2) -0.0205(2) 0.0448(14) Uani 1 1 d . . . H92 H 0.5135 0.3271 -0.0070 0.063 Uiso 1 1 calc R . . C93 C 0.4448(3) 0.3645(2) -0.0731(2) 0.0521(16) Uani 1 1 d . . . H93 H 0.4732 0.3488 -0.0965 0.073 Uiso 1 1 calc R . . C94 C 0.3797(3) 0.3998(2) -0.0911(2) 0.0451(14) Uani 1 1 d . . . H94 H 0.3629 0.4090 -0.1271 0.063 Uiso 1 1 calc R . . C95 C 0.3382(3) 0.42224(19) -0.05652(18) 0.0348(12) Uani 1 1 d . . . C96 C 0.2662(3) 0.4592(2) -0.0744(2) 0.0395(14) Uani 1 1 d . . . C97 C 0.2348(4) 0.4730(2) -0.13106(19) 0.0596(18) Uani 1 1 d . . . H97A H 0.1961 0.5029 -0.1352 0.089 Uiso 1 1 calc R . . H97B H 0.2021 0.4441 -0.1507 0.089 Uiso 1 1 calc R . . H97C H 0.2855 0.4809 -0.1444 0.089 Uiso 1 1 calc R . . C101 C 0.1669(3) 0.35809(19) -0.01958(18) 0.0372(13) Uani 1 1 d . . . H101 H 0.2162 0.3619 -0.0335 0.052 Uiso 1 1 calc R . . C102 C 0.0999(3) 0.3259(2) -0.0452(2) 0.0452(14) Uani 1 1 d . . . H102 H 0.1033 0.3082 -0.0759 0.063 Uiso 1 1 calc R . . C103 C 0.0284(4) 0.3199(2) -0.0259(2) 0.0548(17) Uani 1 1 d . . . H103 H -0.0189 0.2980 -0.0428 0.077 Uiso 1 1 calc R . . C104 C 0.0264(3) 0.3460(2) 0.0184(2) 0.0511(16) Uani 1 1 d . . . H104 H -0.0231 0.3426 0.0322 0.072 Uiso 1 1 calc R . . C105 C 0.0970(3) 0.3780(2) 0.0439(2) 0.0382(13) Uani 1 1 d . . . C106 C 0.0989(3) 0.4040(2) 0.0936(2) 0.0386(13) Uani 1 1 d . . . C107 C 0.0267(4) 0.3967(2) 0.1200(2) 0.0620(18) Uani 1 1 d . . . H10A H 0.0435 0.4132 0.1545 0.093 Uiso 1 1 calc R . . H10B H 0.0174 0.3601 0.1242 0.093 Uiso 1 1 calc R . . H10C H -0.0278 0.4122 0.0986 0.093 Uiso 1 1 calc R . . N111 N 0.3614(3) 0.37813(16) 0.12660(15) 0.0362(10) Uani 1 1 d . . . N112 N 0.4630(2) 0.45535(16) 0.11077(16) 0.0347(10) Uani 1 1 d . . . O96 O 0.51656(19) 0.49501(13) 0.10196(13) 0.0412(9) Uani 1 1 d . . . C111 C 0.3102(4) 0.3405(2) 0.13558(19) 0.0420(14) Uani 1 1 d . . . H111 H 0.2506 0.3388 0.1153 0.059 Uiso 1 1 calc R . . C112 C 0.3421(4) 0.3032(2) 0.1743(2) 0.0472(15) Uani 1 1 d . . . H112 H 0.3049 0.2765 0.1801 0.066 Uiso 1 1 calc R . . C113 C 0.4278(4) 0.3063(2) 0.2035(2) 0.0563(17) Uani 1 1 d . . . H113 H 0.4504 0.2817 0.2300 0.079 Uiso 1 1 calc R . . C114 C 0.4813(4) 0.3445(2) 0.1948(2) 0.0487(15) Uani 1 1 d . . . H114 H 0.5409 0.3467 0.2151 0.068 Uiso 1 1 calc R . . C115 C 0.4471(3) 0.3803(2) 0.15562(18) 0.0376(13) Uani 1 1 d . . . C116 C 0.5037(3) 0.4224(2) 0.14463(17) 0.0342(12) Uani 1 1 d . . . C117 C 0.5994(3) 0.4240(2) 0.1717(2) 0.0511(16) Uani 1 1 d . . . H11A H 0.6272 0.4520 0.1573 0.077 Uiso 1 1 calc R . . H11B H 0.6266 0.3914 0.1665 0.077 Uiso 1 1 calc R . . H11C H 0.6076 0.4297 0.2092 0.077 Uiso 1 1 calc R . . Cl1 Cl 0.41601(9) 0.25620(6) 0.35428(5) 0.0507(4) Uani 1 1 d . . . O121 O 0.3432(3) 0.25122(18) 0.37612(17) 0.0760(14) Uani 1 1 d . . . O122 O 0.4879(3) 0.22763(18) 0.38502(18) 0.0869(15) Uani 1 1 d . . . O123 O 0.3925(3) 0.2389(2) 0.30105(16) 0.0930(16) Uani 1 1 d . . . O124 O 0.4433(3) 0.30835(18) 0.3564(2) 0.0858(15) Uani 1 1 d . . . Cl2 Cl 0.59451(10) 0.26310(6) 0.11737(6) 0.0539(4) Uani 1 1 d . . . O131 O 0.6503(4) 0.2940 0.1552(3) 0.176(3) Uani 1 1 d . . . O132 O 0.5395(5) 0.2342(3) 0.1408(3) 0.114(3) Uani 0.811(6) 1 d P . . O133 O 0.6456(4) 0.2323(2) 0.0958(3) 0.094(2) Uani 0.811(6) 1 d P . . O134 O 0.5516(5) 0.2998 0.0878(3) 0.142(3) Uani 0.811(6) 1 d P . . O32A O 0.6128(16) 0.2194(9) 0.1406(9) 0.063(7) Uiso 0.189(6) 1 d P . . O33A O 0.6222(17) 0.2616(11) 0.0624(10) 0.077(8) Uiso 0.189(6) 1 d P . . O34A O 0.4966(13) 0.2623(8) 0.0935(8) 0.052(6) Uiso 0.189(6) 1 d P . . Cl3 Cl 0.66118(8) 0.69461(5) 0.35013(5) 0.0390(3) Uani 1 1 d . . . O141 O 0.5704(2) 0.68256(18) 0.32990(14) 0.0673(13) Uani 1 1 d . . . O142 O 0.6776(3) 0.71982(17) 0.40018(14) 0.0667(12) Uani 1 1 d . . . O143 O 0.7112(3) 0.64818(15) 0.35770(18) 0.0726(13) Uani 1 1 d . . . O144 O 0.6901(2) 0.72652(15) 0.31431(15) 0.0575(11) Uani 1 1 d . . . Cl4 Cl 0.78801(8) 0.68805(5) 0.17613(5) 0.0416(3) Uani 1 1 d . . . O151 O 0.7450(3) 0.65239(17) 0.19974(15) 0.0751(14) Uani 1 1 d . . . O152 O 0.8276(3) 0.72744(16) 0.21275(16) 0.0724(14) Uani 1 1 d . . . O153 O 0.7282(4) 0.7102 0.1329(2) 0.142(3) Uani 1 1 d . . . O154 O 0.8526(4) 0.6633(3) 0.1593(3) 0.152(3) Uani 1 1 d . . . O1M O 0.7417(7) 0.5388(5) 0.2776(4) 0.244(5) Uani 1 1 d . . . C1M C 0.7728(8) 0.4898(5) 0.2857(6) 0.168(6) Uani 1 1 d . . . O2M O 0.6466(8) 0.3960(6) 0.3384(5) 0.121(5) Uani 0.50 1 d P . . C2M C 0.6228(11) 0.4404(7) 0.3022(5) 0.083(5) Uani 0.50 1 d P . . O3M O 0.9647(5) 0.5415(4) 0.2479(4) 0.088(3) Uani 0.50 1 d P . . C3M C 0.9742(10) 0.4964(7) 0.2225(6) 0.123(8) Uani 0.50 1 d P . . O4M O 0.8833(8) 0.4547(4) 0.2277(5) 0.074(3) Uiso 0.40 1 d P . . C4M C 0.9055(14) 0.3980(8) 0.2199(8) 0.089(6) Uiso 0.40 1 d P . . O1W O 0.6801(10) 0.4080(7) 0.3049(5) 0.152(6) Uani 0.50 1 d P . . O2W O 0.7157(10) 0.3178(6) 0.2645(7) 0.157(7) Uani 0.40 1 d P . . O3W O 0.8506(19) 0.3853(11) 0.2224(11) 0.169(11) Uiso 0.30 1 d P . . H41O H 0.2050 0.5124 0.5246 0.078 Uiso 1 1 d . . . H51O H 0.3804 0.4957 0.3923 0.063 Uiso 1 1 d . . . H91O H 0.1505 0.5215 -0.0281 0.053 Uiso 1 1 d . . . H95O H 0.2199 0.4768 0.1664 0.057 Uiso 1 1 d . . . H96O H 0.4750 0.5147 0.0792 0.051 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0159(4) 0.0327(5) 0.0261(4) 0.0004(3) 0.0057(3) 0.0012(3) Ce1 0.01652(14) 0.03221(17) 0.02794(14) -0.00061(11) 0.00563(10) -0.00178(11) N1 0.0162(19) 0.032(2) 0.030(2) 0.0002(17) 0.0034(15) -0.0008(17) N2 0.016(2) 0.035(2) 0.029(2) 0.0047(17) 0.0011(16) 0.0024(17) N11 0.0212(19) 0.039(2) 0.0238(18) 0.0017(17) 0.0130(15) -0.0015(18) N12 0.022(2) 0.032(2) 0.030(2) 0.0017(17) 0.0090(16) 0.0000(17) N21 0.022(2) 0.033(2) 0.031(2) -0.0016(18) 0.0078(16) -0.0006(18) N22 0.022(2) 0.035(2) 0.0219(19) -0.0025(16) 0.0055(15) 0.0029(17) N31 0.017(2) 0.040(3) 0.038(2) -0.0105(19) 0.0086(16) -0.0059(18) N32 0.022(2) 0.038(3) 0.040(2) -0.002(2) -0.0025(17) 0.0018(19) N41 0.018(2) 0.040(3) 0.034(2) 0.0039(19) 0.0086(16) -0.0009(18) N42 0.024(2) 0.037(3) 0.035(2) 0.0020(18) 0.0112(17) -0.0014(18) N51 0.023(2) 0.039(3) 0.033(2) -0.0064(19) 0.0085(16) 0.0006(19) N52 0.020(2) 0.035(2) 0.036(2) 0.0041(18) 0.0092(16) 0.0054(18) O1 0.0268(17) 0.032(2) 0.0319(17) -0.0019(15) 0.0011(13) -0.0062(15) O11 0.0182(16) 0.0317(19) 0.0357(17) -0.0001(15) 0.0098(13) -0.0002(14) O21 0.0274(17) 0.0295(19) 0.0292(16) 0.0077(14) 0.0081(13) 0.0051(14) O31 0.031(2) 0.067(3) 0.049(2) 0.011(2) -0.0019(17) -0.0080(18) O41 0.0338(18) 0.041(2) 0.0352(18) -0.0062(16) 0.0094(14) 0.0017(16) O51 0.0246(18) 0.042(2) 0.047(2) -0.0012(17) 0.0177(15) -0.0039(16) C1 0.020(2) 0.047(3) 0.033(3) 0.004(2) 0.0091(19) 0.000(2) C2 0.029(3) 0.048(3) 0.037(3) 0.007(2) 0.006(2) -0.009(2) C3 0.025(3) 0.070(4) 0.036(3) 0.017(3) 0.012(2) 0.005(3) C4 0.023(3) 0.051(4) 0.041(3) 0.003(3) 0.013(2) -0.001(2) C5 0.017(2) 0.041(3) 0.027(2) 0.005(2) 0.0074(18) 0.009(2) C6 0.016(2) 0.041(3) 0.024(2) 0.001(2) 0.0022(18) 0.003(2) C7 0.046(3) 0.048(4) 0.033(3) -0.005(2) 0.014(2) 0.007(3) C11 0.028(3) 0.037(3) 0.042(3) 0.000(2) 0.016(2) 0.002(2) C12 0.048(3) 0.039(3) 0.053(3) -0.008(3) 0.019(3) 0.000(3) C13 0.047(3) 0.046(4) 0.039(3) -0.010(3) 0.008(2) -0.001(3) C14 0.037(3) 0.045(4) 0.039(3) -0.008(3) 0.006(2) -0.006(3) C15 0.021(2) 0.038(3) 0.026(2) 0.001(2) 0.0053(18) -0.007(2) C16 0.021(2) 0.036(3) 0.028(2) 0.002(2) 0.0066(18) -0.007(2) C17 0.021(3) 0.047(3) 0.036(3) 0.006(2) -0.006(2) -0.002(2) C21 0.027(3) 0.040(3) 0.031(2) 0.003(2) 0.008(2) 0.004(2) C22 0.040(3) 0.039(3) 0.027(2) 0.003(2) 0.004(2) 0.013(2) C23 0.026(3) 0.046(3) 0.034(3) -0.004(2) 0.002(2) 0.010(2) C24 0.019(2) 0.042(3) 0.037(3) -0.005(2) 0.004(2) 0.003(2) C25 0.022(2) 0.037(3) 0.020(2) -0.006(2) 0.0041(17) 0.001(2) C26 0.017(2) 0.037(3) 0.028(2) -0.006(2) 0.0071(18) 0.000(2) C27 0.023(3) 0.054(4) 0.044(3) 0.006(3) 0.014(2) -0.002(2) C31 0.027(3) 0.046(3) 0.043(3) -0.001(3) 0.007(2) -0.002(2) C32 0.037(3) 0.050(4) 0.041(3) 0.001(3) 0.013(2) -0.003(3) C33 0.039(3) 0.050(4) 0.046(3) 0.000(3) 0.021(2) -0.010(3) C34 0.028(3) 0.050(4) 0.053(3) -0.009(3) 0.013(2) -0.010(3) C35 0.025(3) 0.038(3) 0.035(3) -0.008(2) 0.007(2) -0.006(2) C36 0.023(3) 0.049(4) 0.048(3) -0.008(3) 0.007(2) -0.005(2) C37 0.028(3) 0.072(5) 0.071(4) 0.011(3) 0.001(3) -0.013(3) C41 0.033(3) 0.034(3) 0.033(3) 0.005(2) 0.010(2) -0.001(2) C42 0.029(3) 0.039(3) 0.042(3) 0.005(2) 0.007(2) 0.003(2) C43 0.030(3) 0.051(4) 0.050(3) 0.004(3) 0.002(2) 0.013(3) C44 0.029(3) 0.052(4) 0.034(3) 0.005(3) 0.000(2) 0.000(3) C45 0.023(3) 0.037(3) 0.033(2) 0.006(2) 0.0085(19) -0.010(2) C46 0.020(3) 0.038(3) 0.036(3) 0.008(2) 0.007(2) -0.001(2) C47 0.039(3) 0.046(3) 0.030(3) 0.001(2) 0.004(2) -0.001(2) C51 0.034(3) 0.055(4) 0.038(3) -0.011(3) 0.012(2) -0.009(3) C52 0.064(4) 0.080(5) 0.074(4) -0.040(4) 0.028(3) -0.040(4) C53 0.086(5) 0.108(6) 0.063(4) -0.048(4) 0.034(4) -0.038(4) C54 0.062(4) 0.071(5) 0.047(3) -0.022(3) 0.025(3) -0.015(3) C55 0.043(3) 0.044(3) 0.031(3) -0.001(2) 0.011(2) -0.002(3) C56 0.032(3) 0.037(3) 0.031(3) 0.004(2) 0.012(2) 0.010(2) C57 0.046(3) 0.052(4) 0.053(3) 0.004(3) 0.031(3) 0.011(3) Ni2 0.0179(4) 0.0344(5) 0.0315(4) -0.0059(4) 0.0046(3) -0.0019(3) Ce2 0.02130(15) 0.03260(18) 0.02845(14) -0.00414(11) 0.00666(11) -0.00223(11) N61 0.023(2) 0.034(3) 0.039(2) -0.0056(19) 0.0041(17) -0.0021(19) N62 0.017(2) 0.034(3) 0.040(2) -0.0040(19) 0.0068(16) -0.0006(18) N71 0.027(2) 0.038(3) 0.032(2) -0.0107(19) 0.0096(17) -0.0012(19) N72 0.022(2) 0.034(2) 0.029(2) -0.0079(17) 0.0085(16) -0.0068(17) N81 0.021(2) 0.037(3) 0.033(2) -0.0001(19) 0.0054(16) -0.0007(18) N82 0.019(2) 0.036(2) 0.030(2) -0.0019(18) 0.0027(16) 0.0014(17) N91 0.030(2) 0.041(3) 0.028(2) -0.0057(19) 0.0081(17) -0.008(2) N92 0.024(2) 0.038(3) 0.035(2) -0.0061(19) 0.0059(17) -0.0089(19) N101 0.029(2) 0.033(3) 0.041(2) -0.0057(19) 0.0123(18) -0.0083(19) N102 0.033(2) 0.040(3) 0.042(2) -0.006(2) 0.0194(19) -0.004(2) O61 0.0244(17) 0.0297(19) 0.0362(18) -0.0060(15) 0.0070(14) -0.0024(15) O71 0.0311(18) 0.040(2) 0.0302(17) -0.0075(15) 0.0100(14) -0.0048(16) O81 0.0244(17) 0.035(2) 0.0358(18) -0.0088(15) 0.0061(14) -0.0063(15) O91 0.0260(18) 0.049(2) 0.0393(19) -0.0017(17) 0.0029(15) -0.0027(17) O95 0.051(2) 0.052(2) 0.046(2) -0.0170(18) 0.0298(18) -0.0142(19) C61 0.026(3) 0.032(3) 0.051(3) 0.002(2) 0.009(2) 0.003(2) C62 0.066(4) 0.034(4) 0.084(5) 0.014(3) 0.039(3) 0.009(3) C63 0.100(5) 0.062(5) 0.083(5) 0.040(4) 0.052(4) 0.031(4) C64 0.068(4) 0.053(4) 0.061(4) 0.021(3) 0.036(3) 0.016(3) C65 0.030(3) 0.038(3) 0.046(3) 0.002(3) 0.013(2) -0.001(2) C66 0.026(3) 0.034(3) 0.031(3) 0.000(2) 0.009(2) -0.006(2) C67 0.038(3) 0.049(4) 0.034(3) -0.006(2) 0.014(2) -0.006(3) C71 0.025(3) 0.035(3) 0.060(3) -0.014(3) 0.013(2) -0.009(2) C72 0.036(3) 0.040(3) 0.060(3) -0.021(3) 0.015(3) -0.010(3) C73 0.031(3) 0.068(4) 0.046(3) -0.022(3) 0.014(2) -0.019(3) C74 0.032(3) 0.054(4) 0.033(3) -0.006(3) 0.007(2) -0.009(3) C75 0.027(3) 0.046(3) 0.021(2) -0.007(2) 0.0098(19) -0.006(2) C76 0.019(2) 0.043(3) 0.023(2) -0.006(2) 0.0046(18) 0.001(2) C77 0.036(3) 0.059(4) 0.030(3) 0.011(3) -0.003(2) 0.010(3) C81 0.029(3) 0.035(3) 0.036(3) -0.007(2) 0.003(2) 0.006(2) C82 0.041(3) 0.045(3) 0.029(3) -0.008(2) 0.005(2) 0.014(3) C83 0.036(3) 0.046(4) 0.041(3) -0.001(3) 0.019(2) 0.010(3) C84 0.027(3) 0.047(4) 0.045(3) 0.002(3) 0.014(2) 0.007(2) C85 0.022(3) 0.036(3) 0.040(3) 0.001(2) 0.009(2) 0.000(2) C86 0.017(2) 0.033(3) 0.034(3) -0.001(2) 0.0018(19) 0.001(2) C87 0.026(3) 0.049(4) 0.051(3) -0.008(3) 0.010(2) -0.005(3) C91 0.032(3) 0.046(3) 0.038(3) -0.015(3) 0.008(2) -0.002(3) C92 0.032(3) 0.055(4) 0.049(3) -0.013(3) 0.012(2) -0.003(3) C93 0.046(3) 0.067(4) 0.051(3) -0.023(3) 0.027(3) -0.007(3) C94 0.053(3) 0.050(4) 0.040(3) -0.012(3) 0.025(3) -0.007(3) C95 0.034(3) 0.036(3) 0.035(3) -0.005(2) 0.012(2) -0.014(2) C96 0.036(3) 0.041(3) 0.038(3) -0.008(2) 0.002(2) -0.009(3) C97 0.085(5) 0.070(4) 0.024(3) -0.006(3) 0.015(3) -0.002(4) C101 0.038(3) 0.035(3) 0.038(3) -0.005(2) 0.008(2) 0.003(2) C102 0.035(3) 0.051(4) 0.045(3) -0.006(3) 0.003(2) -0.010(3) C103 0.044(3) 0.054(4) 0.059(4) -0.017(3) 0.002(3) -0.019(3) C104 0.036(3) 0.053(4) 0.065(4) -0.002(3) 0.014(3) -0.008(3) C105 0.033(3) 0.034(3) 0.047(3) 0.002(2) 0.010(2) 0.003(2) C106 0.038(3) 0.035(3) 0.049(3) -0.005(3) 0.022(2) -0.006(2) C107 0.053(4) 0.058(4) 0.089(5) -0.016(4) 0.043(3) -0.018(3) N111 0.036(2) 0.038(3) 0.035(2) 0.0003(19) 0.0109(18) 0.007(2) N112 0.022(2) 0.043(3) 0.038(2) -0.003(2) 0.0076(18) -0.0006(19) O96 0.0237(18) 0.048(2) 0.048(2) 0.0051(18) 0.0036(15) -0.0039(16) C111 0.046(3) 0.047(4) 0.041(3) -0.002(3) 0.024(2) 0.002(3) C112 0.059(4) 0.045(4) 0.045(3) 0.004(3) 0.026(3) -0.001(3) C113 0.066(4) 0.059(4) 0.049(3) 0.018(3) 0.024(3) 0.019(3) C114 0.045(3) 0.061(4) 0.041(3) 0.009(3) 0.013(3) 0.005(3) C115 0.036(3) 0.050(4) 0.029(3) 0.000(2) 0.014(2) 0.009(3) C116 0.023(3) 0.052(4) 0.026(2) -0.003(2) 0.0032(19) 0.006(2) C117 0.032(3) 0.068(4) 0.049(3) 0.006(3) 0.003(2) 0.008(3) Cl1 0.0564(9) 0.0548(10) 0.0445(7) 0.0078(7) 0.0197(6) 0.0110(7) O121 0.070(3) 0.103(4) 0.071(3) -0.008(3) 0.046(2) -0.010(3) O122 0.088(3) 0.095(4) 0.080(3) 0.031(3) 0.028(3) 0.048(3) O123 0.121(4) 0.118(4) 0.047(3) -0.012(3) 0.035(3) 0.000(3) O124 0.084(3) 0.067(3) 0.108(4) 0.024(3) 0.030(3) -0.001(3) Cl2 0.0490(9) 0.0454(9) 0.0678(9) 0.0026(8) 0.0167(7) 0.0054(7) O131 0.106(4) 0.161(6) 0.258(8) -0.146(6) 0.043(5) -0.029(4) O132 0.156(7) 0.083(5) 0.136(6) 0.014(5) 0.097(5) -0.017(5) O133 0.066(4) 0.072(4) 0.156(7) -0.027(5) 0.051(4) 0.019(3) O134 0.163(7) 0.145(7) 0.136(6) 0.098(5) 0.072(5) 0.117(6) Cl3 0.0299(7) 0.0483(8) 0.0375(6) -0.0027(6) 0.0066(5) -0.0033(6) O141 0.026(2) 0.120(4) 0.051(2) 0.012(2) 0.0021(17) -0.017(2) O142 0.077(3) 0.082(3) 0.036(2) -0.018(2) 0.0063(19) -0.002(2) O143 0.056(3) 0.052(3) 0.110(4) 0.002(3) 0.022(3) 0.012(2) O144 0.060(3) 0.060(3) 0.057(2) 0.001(2) 0.025(2) -0.022(2) Cl4 0.0311(7) 0.0492(9) 0.0420(7) 0.0096(6) 0.0055(5) -0.0039(6) O151 0.078(3) 0.091(4) 0.061(3) 0.005(2) 0.027(2) -0.042(3) O152 0.074(3) 0.056(3) 0.061(3) 0.015(2) -0.027(2) -0.016(2) O153 0.170(5) 0.077(4) 0.106(4) 0.042(3) -0.091(4) -0.035(4) O154 0.110(4) 0.192(7) 0.193(6) -0.054(5) 0.107(4) 0.004(5) O1M 0.239(11) 0.340(15) 0.199(9) -0.023(10) 0.137(8) -0.057(10) C1M 0.155(9) 0.134(10) 0.254(14) 0.119(10) 0.121(9) 0.055(8) O2M 0.112(9) 0.190(14) 0.075(7) 0.032(8) 0.048(7) -0.011(9) C2M 0.089(12) 0.105(13) 0.043(8) 0.007(8) -0.004(8) 0.022(10) O3M 0.050(6) 0.152(10) 0.060(6) 0.032(6) 0.009(5) 0.010(6) C3M 0.099(12) 0.172(17) 0.069(9) -0.076(11) -0.029(8) 0.091(12) O1W 0.138(12) 0.199(16) 0.076(9) 0.025(10) -0.044(8) 0.019(12) O2W 0.102(10) 0.140(14) 0.183(16) 0.013(12) -0.038(10) 0.061(10) _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 Ni1 N12 2.041(4) . ? Ni1 N22 2.051(4) . ? Ni1 N2 2.055(4) . ? Ni1 N11 2.079(4) . ? Ni1 N21 2.087(4) . ? Ni1 N1 2.088(4) . ? Ce1 O1 2.433(3) . ? Ce1 O11 2.435(3) . ? Ce1 O21 2.458(3) . ? Ce1 N32 2.676(4) . ? Ce1 N42 2.689(4) . ? Ce1 N41 2.698(4) . ? Ce1 N52 2.718(4) . ? Ce1 N51 2.727(4) . ? Ce1 N31 2.750(4) . ? N1 C1 1.337(5) . ? N1 C5 1.341(5) . ? N2 C6 1.298(5) . ? N2 O1 1.364(4) . ? N11 C11 1.354(5) . ? N11 C15 1.365(5) . ? N12 C16 1.291(5) . ? N12 O11 1.364(4) . ? N21 C21 1.346(5) . ? N21 C25 1.354(5) . ? N22 C26 1.297(5) . ? N22 O21 1.363(4) . ? N31 C35 1.351(5) . ? N31 C31 1.361(6) . ? N32 C36 1.294(6) . ? N32 O31 1.377(5) . ? N41 C41 1.327(5) . ? N41 C45 1.367(5) . ? N42 C46 1.304(5) . ? N42 O41 1.391(5) . ? N51 C51 1.337(6) . ? N51 C55 1.364(6) . ? N52 C56 1.266(6) . ? N52 O51 1.381(4) . ? O31 H31O 0.8400 . ? O41 H41O 0.9793 . ? O51 H51O 0.8058 . ? C1 C2 1.380(6) . ? C1 H1 0.9500 . ? C2 C3 1.387(6) . ? C2 H2 0.9500 . ? C3 C4 1.362(7) . ? C3 H3 0.9500 . ? C4 C5 1.385(6) . ? C4 H4 0.9500 . ? C5 C6 1.478(6) . ? C6 C7 1.499(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C11 C12 1.393(6) . ? C11 H11 0.9500 . ? C12 C13 1.371(6) . ? C12 H12 0.9500 . ? C13 C14 1.373(7) . ? C13 H13 0.9500 . ? C14 C15 1.378(6) . ? C14 H14 0.9500 . ? C15 C16 1.470(6) . ? C16 C17 1.502(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C21 C22 1.385(6) . ? C21 H21 0.9500 . ? C22 C23 1.375(6) . ? C22 H22 0.9500 . ? C23 C24 1.381(6) . ? C23 H23 0.9500 . ? C24 C25 1.399(5) . ? C24 H24 0.9500 . ? C25 C26 1.448(6) . ? C26 C27 1.494(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C31 C32 1.357(6) . ? C31 H31 0.9500 . ? C32 C33 1.357(6) . ? C32 H32 0.9500 . ? C33 C34 1.381(7) . ? C33 H33 0.9500 . ? C34 C35 1.386(6) . ? C34 H34 0.9500 . ? C35 C36 1.488(6) . ? C36 C37 1.479(6) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C41 C42 1.393(6) . ? C41 H41 0.9500 . ? C42 C43 1.388(6) . ? C42 H42 0.9500 . ? C43 C44 1.376(7) . ? C43 H43 0.9500 . ? C44 C45 1.378(6) . ? C44 H44 0.9500 . ? C45 C46 1.472(6) . ? C46 C47 1.492(6) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C51 C52 1.384(7) . ? C51 H51 0.9500 . ? C52 C53 1.376(8) . ? C52 H52 0.9500 . ? C53 C54 1.391(8) . ? C53 H53 0.9500 . ? C54 C55 1.400(7) . ? C54 H54 0.9500 . ? C55 C56 1.479(7) . ? C56 C57 1.498(6) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? Ni2 N82 2.044(4) . ? Ni2 N62 2.052(4) . ? Ni2 N72 2.056(4) . ? Ni2 N71 2.086(4) . ? Ni2 N61 2.089(4) . ? Ni2 N81 2.100(4) . ? Ce2 O61 2.425(3) . ? Ce2 O81 2.453(3) . ? Ce2 O71 2.457(3) . ? Ce2 N92 2.669(4) . ? Ce2 N112 2.680(4) . ? Ce2 N102 2.684(4) . ? Ce2 N91 2.706(4) . ? Ce2 N111 2.735(4) . ? Ce2 N101 2.748(4) . ? N61 C61 1.341(6) . ? N61 C65 1.362(6) . ? N62 C66 1.306(6) . ? N62 O61 1.353(4) . ? N71 C71 1.320(6) . ? N71 C75 1.368(5) . ? N72 C76 1.297(5) . ? N72 O71 1.357(4) . ? N81 C81 1.331(6) . ? N81 C85 1.349(5) . ? N82 C86 1.300(6) . ? N82 O81 1.358(4) . ? N91 C91 1.335(6) . ? N91 C95 1.363(6) . ? N92 C96 1.287(6) . ? N92 O91 1.388(5) . ? N101 C101 1.342(6) . ? N101 C105 1.353(6) . ? N102 C106 1.287(6) . ? N102 O95 1.384(5) . ? O91 H91O 0.8929 . ? O95 H95O 0.9327 . ? C61 C62 1.375(7) . ? C61 H61 0.9500 . ? C62 C63 1.374(8) . ? C62 H62 0.9500 . ? C63 C64 1.401(8) . ? C63 H63 0.9500 . ? C64 C65 1.372(7) . ? C64 H64 0.9500 . ? C65 C66 1.482(7) . ? C66 C67 1.489(6) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C71 C72 1.373(6) . ? C71 H71 0.9500 . ? C72 C73 1.388(7) . ? C72 H72 0.9500 . ? C73 C74 1.384(7) . ? C73 H73 0.9500 . ? C74 C75 1.380(6) . ? C74 H74 0.9500 . ? C75 C76 1.492(6) . ? C76 C77 1.507(6) . ? C81 C82 1.389(6) . ? C81 H81 0.9500 . ? C82 C83 1.360(7) . ? C82 H82 0.9500 . ? C83 C84 1.392(7) . ? C83 H83 0.9500 . ? C84 C85 1.389(6) . ? C84 H84 0.9500 . ? C85 C86 1.467(6) . ? C86 C87 1.491(6) . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C91 C92 1.371(7) . ? C91 H91 0.9500 . ? C92 C93 1.385(7) . ? C92 H92 0.9500 . ? C93 C94 1.366(7) . ? C93 H93 0.9500 . ? C94 C95 1.392(7) . ? C94 H94 0.9500 . ? C95 C96 1.467(7) . ? C96 C97 1.494(7) . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C101 C102 1.377(6) . ? C101 H101 0.9500 . ? C102 C103 1.368(7) . ? C102 H102 0.9500 . ? C103 C104 1.366(7) . ? C103 H103 0.9500 . ? C104 C105 1.410(7) . ? C104 H104 0.9500 . ? C105 C106 1.475(7) . ? C106 C107 1.500(7) . ? C107 H10A 0.9800 . ? C107 H10B 0.9800 . ? C107 H10C 0.9800 . ? N111 C111 1.334(6) . ? N111 C115 1.364(6) . ? N112 C116 1.283(6) . ? N112 O96 1.395(5) . ? O96 H96O 0.9196 . ? C111 C112 1.406(7) . ? C111 H111 0.9500 . ? C112 C113 1.366(7) . ? C112 H112 0.9500 . ? C113 C114 1.365(7) . ? C113 H113 0.9500 . ? C114 C115 1.393(7) . ? C114 H114 0.9500 . ? C115 C116 1.494(7) . ? C116 C117 1.486(6) . ? C117 H11A 0.9800 . ? C117 H11B 0.9800 . ? C117 H11C 0.9800 . ? Cl1 O122 1.416(4) . ? Cl1 O121 1.424(4) . ? Cl1 O124 1.426(5) . ? Cl1 O123 1.433(4) . ? Cl2 O32A 1.29(2) . ? Cl2 O134 1.306(4) . ? Cl2 O133 1.368(5) . ? Cl2 O131 1.399(5) . ? Cl2 O132 1.414(6) . ? Cl2 O34A 1.50(2) . ? Cl2 O33A 1.63(3) . ? O132 O32A 1.22(2) . ? O132 O34A 1.45(2) . ? O133 O33A 1.15(3) . ? O133 O32A 1.46(3) . ? O134 O34A 1.34(2) . ? O134 O33A 1.76(3) . ? Cl3 O141 1.420(3) . ? Cl3 O144 1.428(4) . ? Cl3 O143 1.431(4) . ? Cl3 O142 1.442(4) . ? Cl4 O154 1.379(5) . ? Cl4 O151 1.396(4) . ? Cl4 O153 1.398(4) . ? Cl4 O152 1.437(4) . ? O1M C1M 1.369(13) . ? O2M O1W 1.191(17) . ? O2M C2M 1.488(19) . ? C2M O1W 1.227(19) . ? O3M C3M 1.386(16) . ? C3M O4M 1.84(2) . ? O4M C4M 1.55(2) . ? C4M O3W 0.95(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 N12 Ni1 N22 93.26(15) . . ? N12 Ni1 N2 91.05(14) . . ? N22 Ni1 N2 90.09(15) . . ? N12 Ni1 N11 77.48(15) . . ? N22 Ni1 N11 99.46(13) . . ? N2 Ni1 N11 165.39(14) . . ? N12 Ni1 N21 168.95(15) . . ? N22 Ni1 N21 77.78(14) . . ? N2 Ni1 N21 95.37(14) . . ? N11 Ni1 N21 97.43(14) . . ? N12 Ni1 N1 95.75(14) . . ? N22 Ni1 N1 164.89(14) . . ? N2 Ni1 N1 77.67(15) . . ? N11 Ni1 N1 94.32(14) . . ? N21 Ni1 N1 94.40(14) . . ? O1 Ce1 O11 84.06(10) . . ? O1 Ce1 O21 82.92(10) . . ? O11 Ce1 O21 83.61(10) . . ? O1 Ce1 N32 67.54(11) . . ? O11 Ce1 N32 144.18(11) . . ? O21 Ce1 N32 72.01(11) . . ? O1 Ce1 N42 140.93(11) . . ? O11 Ce1 N42 69.87(10) . . ? O21 Ce1 N42 66.14(10) . . ? N32 Ce1 N42 119.91(12) . . ? O1 Ce1 N41 147.30(11) . . ? O11 Ce1 N41 82.39(10) . . ? O21 Ce1 N41 124.67(10) . . ? N32 Ce1 N41 133.09(12) . . ? N42 Ce1 N41 58.75(12) . . ? O1 Ce1 N52 71.16(10) . . ? O11 Ce1 N52 65.04(11) . . ? O21 Ce1 N52 140.59(11) . . ? N32 Ce1 N52 120.87(12) . . ? N42 Ce1 N52 118.94(11) . . ? N41 Ce1 N52 76.14(11) . . ? O1 Ce1 N51 80.44(11) . . ? O11 Ce1 N51 123.38(11) . . ? O21 Ce1 N51 146.13(10) . . ? N32 Ce1 N51 74.40(11) . . ? N42 Ce1 N51 138.20(11) . . ? N41 Ce1 N51 82.47(11) . . ? N52 Ce1 N51 58.39(11) . . ? O1 Ce1 N31 125.57(10) . . ? O11 Ce1 N31 146.05(10) . . ? O21 Ce1 N31 84.27(11) . . ? N32 Ce1 N31 58.18(12) . . ? N42 Ce1 N31 76.22(11) . . ? N41 Ce1 N31 78.76(11) . . ? N52 Ce1 N31 134.97(11) . . ? N51 Ce1 N31 81.81(11) . . ? C1 N1 C5 117.4(4) . . ? C1 N1 Ni1 128.3(3) . . ? C5 N1 Ni1 114.1(3) . . ? C6 N2 O1 117.9(4) . . ? C6 N2 Ni1 117.9(3) . . ? O1 N2 Ni1 124.2(3) . . ? C11 N11 C15 117.0(4) . . ? C11 N11 Ni1 128.6(3) . . ? C15 N11 Ni1 114.3(3) . . ? C16 N12 O11 118.7(4) . . ? C16 N12 Ni1 118.7(3) . . ? O11 N12 Ni1 122.6(2) . . ? C21 N21 C25 119.4(4) . . ? C21 N21 Ni1 127.4(3) . . ? C25 N21 Ni1 113.0(3) . . ? C26 N22 O21 118.9(4) . . ? C26 N22 Ni1 117.7(3) . . ? O21 N22 Ni1 123.1(2) . . ? C35 N31 C31 115.9(4) . . ? C35 N31 Ce1 121.1(3) . . ? C31 N31 Ce1 122.7(3) . . ? C36 N32 O31 113.6(4) . . ? C36 N32 Ce1 128.2(3) . . ? O31 N32 Ce1 117.5(3) . . ? C41 N41 C45 118.3(4) . . ? C41 N41 Ce1 119.4(3) . . ? C45 N41 Ce1 122.2(3) . . ? C46 N42 O41 114.2(4) . . ? C46 N42 Ce1 126.2(3) . . ? O41 N42 Ce1 118.7(2) . . ? C51 N51 C55 117.9(4) . . ? C51 N51 Ce1 120.4(3) . . ? C55 N51 Ce1 120.3(3) . . ? C56 N52 O51 114.2(4) . . ? C56 N52 Ce1 126.5(3) . . ? O51 N52 Ce1 118.8(3) . . ? N2 O1 Ce1 112.9(2) . . ? N12 O11 Ce1 116.3(2) . . ? N22 O21 Ce1 113.7(2) . . ? N32 O31 H31O 109.5 . . ? N42 O41 H41O 97.9 . . ? N52 O51 H51O 100.9 . . ? N1 C1 C2 124.3(4) . . ? N1 C1 H1 117.8 . . ? C2 C1 H1 117.8 . . ? C1 C2 C3 117.1(3) . . ? C1 C2 H2 121.5 . . ? C3 C2 H2 121.5 . . ? C4 C3 C2 119.5(4) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 119.9(5) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 121.7(5) . . ? N1 C5 C6 115.8(4) . . ? C4 C5 C6 122.5(4) . . ? N2 C6 C5 114.3(4) . . ? N2 C6 C7 124.2(4) . . ? C5 C6 C7 121.5(4) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N11 C11 C12 123.4(4) . . ? N11 C11 H11 118.3 . . ? C12 C11 H11 118.3 . . ? C13 C12 C11 118.1(5) . . ? C13 C12 H12 121.0 . . ? C11 C12 H12 121.0 . . ? C12 C13 C14 119.7(5) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C15 120.0(5) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? N11 C15 C14 121.8(5) . . ? N11 C15 C16 114.7(4) . . ? C14 C15 C16 123.4(4) . . ? N12 C16 C15 114.5(4) . . ? N12 C16 C17 123.4(4) . . ? C15 C16 C17 122.0(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N21 C21 C22 122.6(4) . . ? N21 C21 H21 118.7 . . ? C22 C21 H21 118.7 . . ? C23 C22 C21 118.5(5) . . ? C23 C22 H22 120.8 . . ? C21 C22 H22 120.8 . . ? C22 C23 C24 119.4(4) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C23 C24 C25 120.1(5) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? N21 C25 C24 120.0(4) . . ? N21 C25 C26 116.7(4) . . ? C24 C25 C26 123.4(4) . . ? N22 C26 C25 114.7(4) . . ? N22 C26 C27 123.8(4) . . ? C25 C26 C27 121.5(4) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C32 C31 N31 124.5(4) . . ? C32 C31 H31 117.8 . . ? N31 C31 H31 117.8 . . ? C31 C32 C33 119.0(5) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C32 C33 C34 118.8(5) . . ? C32 C33 H33 120.6 . . ? C34 C33 H33 120.6 . . ? C33 C34 C35 119.7(5) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? N31 C35 C34 122.1(4) . . ? N31 C35 C36 117.7(4) . . ? C34 C35 C36 120.2(4) . . ? N32 C36 C37 124.8(5) . . ? N32 C36 C35 113.8(4) . . ? C37 C36 C35 121.3(5) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N41 C41 C42 123.8(4) . . ? N41 C41 H41 118.1 . . ? C42 C41 H41 118.1 . . ? C43 C42 C41 117.0(5) . . ? C43 C42 H42 121.5 . . ? C41 C42 H42 121.5 . . ? C44 C43 C42 119.9(5) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 119.8(5) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? N41 C45 C44 121.1(5) . . ? N41 C45 C46 117.2(4) . . ? C44 C45 C46 121.7(4) . . ? N42 C46 C45 114.6(4) . . ? N42 C46 C47 124.6(5) . . ? C45 C46 C47 120.7(4) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N51 C51 C52 123.9(5) . . ? N51 C51 H51 118.0 . . ? C52 C51 H51 118.0 . . ? C53 C52 C51 118.3(6) . . ? C53 C52 H52 120.8 . . ? C51 C52 H52 120.8 . . ? C52 C53 C54 119.5(6) . . ? C52 C53 H53 120.3 . . ? C54 C53 H53 120.3 . . ? C53 C54 C55 119.0(6) . . ? C53 C54 H54 120.5 . . ? C55 C54 H54 120.5 . . ? N51 C55 C54 121.3(5) . . ? N51 C55 C56 117.9(4) . . ? C54 C55 C56 120.8(5) . . ? N52 C56 C55 115.0(4) . . ? N52 C56 C57 124.9(5) . . ? C55 C56 C57 120.1(4) . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N82 Ni2 N62 90.52(15) . . ? N82 Ni2 N72 91.20(15) . . ? N62 Ni2 N72 91.22(15) . . ? N82 Ni2 N71 166.43(16) . . ? N62 Ni2 N71 98.36(14) . . ? N72 Ni2 N71 78.43(15) . . ? N82 Ni2 N61 97.40(14) . . ? N62 Ni2 N61 77.85(16) . . ? N72 Ni2 N61 166.09(15) . . ? N71 Ni2 N61 94.51(15) . . ? N82 Ni2 N81 77.81(15) . . ? N62 Ni2 N81 165.32(14) . . ? N72 Ni2 N81 97.82(15) . . ? N71 Ni2 N81 94.78(14) . . ? N61 Ni2 N81 94.68(15) . . ? O61 Ce2 O81 81.74(10) . . ? O61 Ce2 O71 83.67(10) . . ? O81 Ce2 O71 82.08(10) . . ? O61 Ce2 N92 71.85(11) . . ? O81 Ce2 N92 65.82(11) . . ? O71 Ce2 N92 141.63(11) . . ? O61 Ce2 N112 66.14(11) . . ? O81 Ce2 N112 141.08(11) . . ? O71 Ce2 N112 73.40(11) . . ? N92 Ce2 N112 119.48(12) . . ? O61 Ce2 N102 142.12(11) . . ? O81 Ce2 N102 71.12(11) . . ? O71 Ce2 N102 67.16(11) . . ? N92 Ce2 N102 117.18(12) . . ? N112 Ce2 N102 122.88(12) . . ? O61 Ce2 N91 83.64(11) . . ? O81 Ce2 N91 124.91(11) . . ? O71 Ce2 N91 147.84(10) . . ? N92 Ce2 N91 59.14(12) . . ? N112 Ce2 N91 74.45(11) . . ? N102 Ce2 N91 133.60(12) . . ? O61 Ce2 N111 125.43(11) . . ? O81 Ce2 N111 145.80(11) . . ? O71 Ce2 N111 81.15(11) . . ? N92 Ce2 N111 137.16(12) . . ? N112 Ce2 N111 59.29(12) . . ? N102 Ce2 N111 74.92(12) . . ? N91 Ce2 N111 82.42(12) . . ? O61 Ce2 N101 146.62(11) . . ? O81 Ce2 N101 86.11(11) . . ? O71 Ce2 N101 125.31(11) . . ? N92 Ce2 N101 74.80(11) . . ? N112 Ce2 N101 132.75(12) . . ? N102 Ce2 N101 58.50(12) . . ? N91 Ce2 N101 78.10(11) . . ? N111 Ce2 N101 79.69(12) . . ? C61 N61 C65 117.3(4) . . ? C61 N61 Ni2 128.7(3) . . ? C65 N61 Ni2 113.9(3) . . ? C66 N62 O61 117.9(4) . . ? C66 N62 Ni2 118.4(3) . . ? O61 N62 Ni2 123.2(3) . . ? C71 N71 C75 118.9(4) . . ? C71 N71 Ni2 127.8(3) . . ? C75 N71 Ni2 113.2(3) . . ? C76 N72 O71 117.8(4) . . ? C76 N72 Ni2 118.2(3) . . ? O71 N72 Ni2 123.7(2) . . ? C81 N81 C85 118.8(4) . . ? C81 N81 Ni2 128.3(3) . . ? C85 N81 Ni2 112.9(3) . . ? C86 N82 O81 118.3(4) . . ? C86 N82 Ni2 118.5(3) . . ? O81 N82 Ni2 123.0(3) . . ? C91 N91 C95 117.3(4) . . ? C91 N91 Ce2 121.4(3) . . ? C95 N91 Ce2 121.3(3) . . ? C96 N92 O91 114.5(4) . . ? C96 N92 Ce2 126.4(3) . . ? O91 N92 Ce2 119.1(3) . . ? C101 N101 C105 117.7(4) . . ? C101 N101 Ce2 121.9(3) . . ? C105 N101 Ce2 119.8(3) . . ? C106 N102 O95 115.1(4) . . ? C106 N102 Ce2 126.7(3) . . ? O95 N102 Ce2 117.5(3) . . ? N62 O61 Ce2 116.3(2) . . ? N72 O71 Ce2 113.8(2) . . ? N82 O81 Ce2 116.1(2) . . ? N92 O91 H91O 103.7 . . ? N102 O95 H95O 105.4 . . ? N61 C61 C62 124.0(5) . . ? N61 C61 H61 118.0 . . ? C62 C61 H61 118.0 . . ? C63 C62 C61 118.0(6) . . ? C63 C62 H62 121.0 . . ? C61 C62 H62 121.0 . . ? C62 C63 C64 119.6(6) . . ? C62 C63 H63 120.2 . . ? C64 C63 H63 120.2 . . ? C65 C64 C63 118.6(6) . . ? C65 C64 H64 120.7 . . ? C63 C64 H64 120.7 . . ? N61 C65 C64 122.3(5) . . ? N61 C65 C66 115.7(4) . . ? C64 C65 C66 122.0(5) . . ? N62 C66 C65 113.9(4) . . ? N62 C66 C67 124.8(5) . . ? C65 C66 C67 121.2(4) . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N71 C71 C72 123.0(5) . . ? N71 C71 H71 118.5 . . ? C72 C71 H71 118.5 . . ? C71 C72 C73 118.6(5) . . ? C71 C72 H72 120.7 . . ? C73 C72 H72 120.7 . . ? C74 C73 C72 119.3(5) . . ? C74 C73 H73 120.4 . . ? C72 C73 H73 120.4 . . ? C75 C74 C73 118.9(5) . . ? C75 C74 H74 120.5 . . ? C73 C74 H74 120.5 . . ? N71 C75 C74 121.2(5) . . ? N71 C75 C76 116.0(4) . . ? C74 C75 C76 122.8(4) . . ? N72 C76 C75 114.0(4) . . ? N72 C76 C77 124.8(5) . . ? C75 C76 C77 121.3(4) . . ? N81 C81 C82 123.2(5) . . ? N81 C81 H81 118.4 . . ? C82 C81 H81 118.4 . . ? C83 C82 C81 118.4(5) . . ? C83 C82 H82 120.8 . . ? C81 C82 H82 120.8 . . ? C82 C83 C84 119.3(5) . . ? C82 C83 H83 120.3 . . ? C84 C83 H83 120.3 . . ? C85 C84 C83 119.5(5) . . ? C85 C84 H84 120.3 . . ? C83 C84 H84 120.3 . . ? N81 C85 C84 120.8(5) . . ? N81 C85 C86 116.9(4) . . ? C84 C85 C86 122.2(4) . . ? N82 C86 C85 113.8(4) . . ? N82 C86 C87 124.0(4) . . ? C85 C86 C87 122.1(4) . . ? C86 C87 H87A 109.5 . . ? C86 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C86 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? N91 C91 C92 124.4(5) . . ? N91 C91 H91 117.8 . . ? C92 C91 H91 117.8 . . ? C91 C92 C93 118.0(5) . . ? C91 C92 H92 121.0 . . ? C93 C92 H92 121.0 . . ? C94 C93 C92 119.4(5) . . ? C94 C93 H93 120.3 . . ? C92 C93 H93 120.3 . . ? C93 C94 C95 119.7(5) . . ? C93 C94 H94 120.1 . . ? C95 C94 H94 120.1 . . ? N91 C95 C94 121.2(5) . . ? N91 C95 C96 117.2(5) . . ? C94 C95 C96 121.6(5) . . ? N92 C96 C95 115.9(5) . . ? N92 C96 C97 124.0(5) . . ? C95 C96 C97 120.1(5) . . ? C96 C97 H97A 109.5 . . ? C96 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C96 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? N101 C101 C102 123.8(5) . . ? N101 C101 H101 118.1 . . ? C102 C101 H101 118.1 . . ? C103 C102 C101 119.0(5) . . ? C103 C102 H102 120.5 . . ? C101 C102 H102 120.5 . . ? C104 C103 C102 118.5(5) . . ? C104 C103 H103 120.8 . . ? C102 C103 H103 120.8 . . ? C103 C104 C105 120.7(5) . . ? C103 C104 H104 119.7 . . ? C105 C104 H104 119.7 . . ? N101 C105 C104 120.2(5) . . ? N101 C105 C106 118.1(4) . . ? C104 C105 C106 121.6(5) . . ? N102 C106 C105 114.8(5) . . ? N102 C106 C107 123.5(5) . . ? C105 C106 C107 121.6(5) . . ? C106 C107 H10A 109.5 . . ? C106 C107 H10B 109.5 . . ? H10A C107 H10B 109.5 . . ? C106 C107 H10C 109.5 . . ? H10A C107 H10C 109.5 . . ? H10B C107 H10C 109.5 . . ? C111 N111 C115 119.0(4) . . ? C111 N111 Ce2 120.5(3) . . ? C115 N111 Ce2 119.7(3) . . ? C116 N112 O96 113.9(4) . . ? C116 N112 Ce2 127.0(3) . . ? O96 N112 Ce2 118.9(3) . . ? N112 O96 H96O 99.8 . . ? N111 C111 C112 121.8(5) . . ? N111 C111 H111 119.1 . . ? C112 C111 H111 119.1 . . ? C113 C112 C111 118.4(5) . . ? C113 C112 H112 120.8 . . ? C111 C112 H112 120.8 . . ? C114 C113 C112 120.6(5) . . ? C114 C113 H113 119.7 . . ? C112 C113 H113 119.7 . . ? C113 C114 C115 119.0(5) . . ? C113 C114 H114 120.5 . . ? C115 C114 H114 120.5 . . ? N111 C115 C114 121.2(5) . . ? N111 C115 C116 118.2(4) . . ? C114 C115 C116 120.6(5) . . ? N112 C116 C117 124.7(5) . . ? N112 C116 C115 114.8(4) . . ? C117 C116 C115 120.5(4) . . ? C116 C117 H11A 109.5 . . ? C116 C117 H11B 109.5 . . ? H11A C117 H11B 109.5 . . ? C116 C117 H11C 109.5 . . ? H11A C117 H11C 109.5 . . ? H11B C117 H11C 109.5 . . ? O122 Cl1 O121 108.9(3) . . ? O122 Cl1 O124 107.2(3) . . ? O121 Cl1 O124 109.8(3) . . ? O122 Cl1 O123 110.8(3) . . ? O121 Cl1 O123 110.5(3) . . ? O124 Cl1 O123 109.6(3) . . ? O32A Cl2 O134 161.4(11) . . ? O32A Cl2 O133 66.4(12) . . ? O134 Cl2 O133 116.6(5) . . ? O32A Cl2 O131 98.8(10) . . ? O134 Cl2 O131 97.5(3) . . ? O133 Cl2 O131 108.2(4) . . ? O32A Cl2 O132 53.4(11) . . ? O134 Cl2 O132 112.1(5) . . ? O133 Cl2 O132 111.8(4) . . ? O131 Cl2 O132 109.5(4) . . ? O32A Cl2 O34A 105.1(14) . . ? O134 Cl2 O34A 56.7(8) . . ? O133 Cl2 O34A 118.0(8) . . ? O131 Cl2 O34A 133.3(8) . . ? O132 Cl2 O34A 59.7(8) . . ? O32A Cl2 O33A 109.0(15) . . ? O134 Cl2 O33A 72.6(10) . . ? O133 Cl2 O33A 44.1(9) . . ? O131 Cl2 O33A 112.8(9) . . ? O132 Cl2 O33A 136.4(9) . . ? O34A Cl2 O33A 96.6(12) . . ? O32A O132 Cl2 58.2(12) . . ? O32A O132 O34A 112.1(15) . . ? Cl2 O132 O34A 63.2(9) . . ? O33A O133 Cl2 80.2(14) . . ? O33A O133 O32A 132.1(18) . . ? Cl2 O133 O32A 54.4(10) . . ? Cl2 O134 O34A 69.0(9) . . ? Cl2 O134 O33A 62.3(9) . . ? O34A O134 O33A 97.1(13) . . ? O132 O32A Cl2 68.4(13) . . ? O132 O32A O133 118.3(18) . . ? Cl2 O32A O133 59.3(11) . . ? O133 O33A Cl2 55.7(12) . . ? O133 O33A O134 100.7(18) . . ? Cl2 O33A O134 45.1(7) . . ? O134 O34A O132 107.5(14) . . ? O134 O34A Cl2 54.3(8) . . ? O132 O34A Cl2 57.1(8) . . ? O141 Cl3 O144 110.3(2) . . ? O141 Cl3 O143 109.0(3) . . ? O144 Cl3 O143 109.0(3) . . ? O141 Cl3 O142 111.2(3) . . ? O144 Cl3 O142 109.6(2) . . ? O143 Cl3 O142 107.6(3) . . ? O154 Cl4 O151 108.8(4) . . ? O154 Cl4 O153 108.7(4) . . ? O151 Cl4 O153 110.0(3) . . ? O154 Cl4 O152 109.4(3) . . ? O151 Cl4 O152 110.4(3) . . ? O153 Cl4 O152 109.41(19) . . ? O1W O2M C2M 53.1(11) . . ? O1W C2M O2M 50.9(10) . . ? O3M C3M O4M 106.1(11) . . ? C4M O4M C3M 110.4(12) . . ? O3W C4M O4M 95(3) . . ? O2M O1W C2M 76.0(16) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.595 _refine_diff_density_min -1.871 _refine_diff_density_rms 0.117 data_peen6_a _database_code_depnum_ccdc_archive 'CCDC 896964' #TrackingRef 'Dalton Perlepes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43.20 H51 Cl2 Dy N12 Ni O15.80' _chemical_formula_weight 1283.27 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' Dy Dy -9.8046 9.8477 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 15.7617(3) _cell_length_b 26.1482(5) _cell_length_c 26.3339(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.3070(10) _cell_angle_gamma 90.00 _cell_volume 10468.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 64200 _cell_measurement_theta_min 6.56 _cell_measurement_theta_max 72.16 _exptl_crystal_description parallelepiped _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5189 _exptl_absorpt_coefficient_mu 9.609 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.315 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'CrystalClear, Rigaku MSC, 2005' _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _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 '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 83045 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 6.56 _diffrn_reflns_theta_max 65.00 _reflns_number_total 16722 _reflns_number_gt 12500 _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1317P)^2^+21.7723P] 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 16722 _refine_ls_number_parameters 1322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1008 _refine_ls_R_factor_gt 0.0798 _refine_ls_wR_factor_ref 0.2336 _refine_ls_wR_factor_gt 0.2123 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.004 _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 Ni1 Ni 0.19895(8) 0.59484(5) 0.40856(5) 0.0384(3) Uani 1 1 d . . . Dy1 Dy 0.21730(3) 0.447074(17) 0.42702(2) 0.04056(13) Uani 1 1 d . . . N1 N 0.2703(4) 0.6332(2) 0.3631(3) 0.0407(16) Uani 1 1 d . . . N2 N 0.2003(4) 0.5425(2) 0.3510(3) 0.0386(16) Uani 1 1 d . . . N11 N 0.2391(4) 0.6462(2) 0.4718(3) 0.0410(16) Uani 1 1 d . . . N12 N 0.3033(4) 0.5589(2) 0.4575(3) 0.0405(16) Uani 1 1 d . . . N21 N 0.0797(4) 0.6298(2) 0.3723(3) 0.0409(16) Uani 1 1 d . . . N22 N 0.1115(4) 0.5503(2) 0.4336(3) 0.0395(16) Uani 1 1 d . . . N31 N 0.1314(4) 0.3796(2) 0.4691(3) 0.0443(17) Uani 1 1 d . . . N32 N 0.0518(5) 0.4329(2) 0.3844(3) 0.0440(17) Uani 1 1 d . . . N41 N 0.3442(4) 0.3883(2) 0.4785(3) 0.0418(16) Uani 1 1 d . . . N42 N 0.2761(5) 0.4587(3) 0.5281(3) 0.0483(18) Uani 1 1 d . . . N51 N 0.2033(4) 0.3743(2) 0.3571(3) 0.0448(17) Uani 1 1 d . . . N52 N 0.3285(4) 0.4432(2) 0.3703(3) 0.0428(17) Uani 1 1 d . . . O1 O 0.1654(3) 0.49464(18) 0.3504(2) 0.0406(13) Uani 1 1 d . . . O11 O 0.3268(3) 0.50990(18) 0.4479(2) 0.0405(13) Uani 1 1 d . . . O21 O 0.1368(3) 0.50641(17) 0.4623(2) 0.0384(12) Uani 1 1 d . . . O31 O 0.0109(4) 0.4597(3) 0.3395(3) 0.0629(18) Uani 1 1 d . . . H31O H 0.0477 0.4787 0.3309 0.082 Uiso 1 1 calc R . . O41 O 0.2432(4) 0.4968(2) 0.5524(2) 0.0507(15) Uani 1 1 d . . . O51 O 0.3984(4) 0.4777(2) 0.3787(3) 0.0524(15) Uani 1 1 d . . . C1 C 0.3080(5) 0.6790(3) 0.3706(4) 0.047(2) Uani 1 1 d . . . H1 H 0.2986 0.6996 0.3983 0.066 Uiso 1 1 calc R . . C2 C 0.3601(6) 0.6985(3) 0.3403(4) 0.049(2) Uani 1 1 d . . . H2 H 0.3877 0.7310 0.3480 0.069 Uiso 1 1 calc R . . C3 C 0.3711(5) 0.6700(3) 0.2990(4) 0.047(2) Uani 1 1 d . . . H3 H 0.4065 0.6823 0.2775 0.066 Uiso 1 1 calc R . . C4 C 0.3298(5) 0.6227(3) 0.2889(4) 0.048(2) Uani 1 1 d . . . H4 H 0.3366 0.6025 0.2603 0.067 Uiso 1 1 calc R . . C5 C 0.2787(5) 0.6054(3) 0.3208(3) 0.0396(19) Uani 1 1 d . . . C6 C 0.2332(5) 0.5556(3) 0.3136(3) 0.0399(19) Uani 1 1 d . . . C7 C 0.2309(6) 0.5235(3) 0.2656(4) 0.053(2) Uani 1 1 d . . . H7A H 0.1991 0.4916 0.2674 0.080 Uiso 1 1 calc R . . H7B H 0.2911 0.5156 0.2645 0.080 Uiso 1 1 calc R . . H7C H 0.2009 0.5424 0.2338 0.080 Uiso 1 1 calc R . . C11 C 0.2007(6) 0.6918(3) 0.4774(4) 0.051(2) Uani 1 1 d . . . H11 H 0.1478 0.7013 0.4523 0.071 Uiso 1 1 calc R . . C12 C 0.2378(7) 0.7250(3) 0.5194(4) 0.060(3) Uani 1 1 d . . . H12 H 0.2097 0.7564 0.5233 0.084 Uiso 1 1 calc R . . C13 C 0.3161(8) 0.7112(4) 0.5551(4) 0.072(3) Uani 1 1 d . . . H13 H 0.3434 0.7332 0.5834 0.101 Uiso 1 1 calc R . . C14 C 0.3539(7) 0.6643(4) 0.5485(4) 0.063(3) Uani 1 1 d . . . H14 H 0.4077 0.6543 0.5725 0.088 Uiso 1 1 calc R . . C15 C 0.3145(5) 0.6329(3) 0.5080(3) 0.0407(19) Uani 1 1 d . . . C16 C 0.3500(6) 0.5819(3) 0.4987(3) 0.042(2) Uani 1 1 d . . . C17 C 0.4289(6) 0.5605(3) 0.5362(4) 0.049(2) Uani 1 1 d . . . H17A H 0.4313 0.5235 0.5306 0.074 Uiso 1 1 calc R . . H17B H 0.4258 0.5671 0.5723 0.074 Uiso 1 1 calc R . . H17C H 0.4818 0.5766 0.5306 0.074 Uiso 1 1 calc R . . C21 C 0.0651(6) 0.6695(3) 0.3395(3) 0.045(2) Uani 1 1 d . . . H21 H 0.1143 0.6864 0.3327 0.064 Uiso 1 1 calc R . . C22 C -0.0187(6) 0.6874(3) 0.3148(3) 0.046(2) Uani 1 1 d . . . H22 H -0.0260 0.7158 0.2914 0.065 Uiso 1 1 calc R . . C23 C -0.0897(6) 0.6640(3) 0.3243(4) 0.048(2) Uani 1 1 d . . . H23 H -0.1477 0.6755 0.3078 0.068 Uiso 1 1 calc R . . C24 C -0.0752(6) 0.6229(3) 0.3587(3) 0.046(2) Uani 1 1 d . . . H24 H -0.1238 0.6060 0.3663 0.064 Uiso 1 1 calc R . . C25 C 0.0100(5) 0.6061(3) 0.3822(3) 0.0416(19) Uani 1 1 d . . . C26 C 0.0289(5) 0.5616(3) 0.4167(4) 0.043(2) Uani 1 1 d . . . C27 C -0.0442(6) 0.5314(3) 0.4308(4) 0.055(2) Uani 1 1 d . . . H27A H -0.0184 0.5041 0.4556 0.082 Uiso 1 1 calc R . . H27B H -0.0825 0.5164 0.3988 0.082 Uiso 1 1 calc R . . H27C H -0.0786 0.5543 0.4471 0.082 Uiso 1 1 calc R . . C31 C 0.1684(6) 0.3503(3) 0.5104(4) 0.049(2) Uani 1 1 d . . . H31 H 0.2306 0.3519 0.5231 0.069 Uiso 1 1 calc R . . C32 C 0.1254(6) 0.3183(3) 0.5363(4) 0.056(2) Uani 1 1 d . . . H32 H 0.1567 0.2983 0.5654 0.079 Uiso 1 1 calc R . . C33 C 0.0352(6) 0.3160(3) 0.5187(4) 0.055(2) Uani 1 1 d . . . H33 H 0.0024 0.2948 0.5359 0.077 Uiso 1 1 calc R . . C34 C -0.0072(6) 0.3452(3) 0.4752(4) 0.053(2) Uani 1 1 d . . . H34 H -0.0694 0.3443 0.4621 0.074 Uiso 1 1 calc R . . C35 C 0.0430(6) 0.3756(3) 0.4514(4) 0.047(2) Uani 1 1 d . . . C36 C 0.0003(6) 0.4055(3) 0.4038(4) 0.053(2) Uani 1 1 d . . . C37 C -0.0991(6) 0.4033(4) 0.3797(4) 0.067(3) Uani 1 1 d . . . H37A H -0.1151 0.4254 0.3485 0.100 Uiso 1 1 calc R . . H37B H -0.1294 0.4151 0.4056 0.100 Uiso 1 1 calc R . . H37C H -0.1166 0.3680 0.3694 0.100 Uiso 1 1 calc R . . C41 C 0.3738(6) 0.3492(3) 0.4548(4) 0.048(2) Uani 1 1 d . . . H41 H 0.3449 0.3424 0.4190 0.068 Uiso 1 1 calc R . . C42 C 0.4445(6) 0.3182(3) 0.4799(4) 0.058(3) Uani 1 1 d . . . H42 H 0.4640 0.2911 0.4617 0.081 Uiso 1 1 calc R . . C43 C 0.4846(6) 0.3284(4) 0.5316(5) 0.063(3) Uani 1 1 d . . . H43 H 0.5326 0.3077 0.5497 0.088 Uiso 1 1 calc R . . C44 C 0.4571(6) 0.3682(3) 0.5582(4) 0.061(3) Uani 1 1 d . . . H44 H 0.4859 0.3755 0.5939 0.085 Uiso 1 1 calc R . . C45 C 0.3844(6) 0.3973(3) 0.5300(4) 0.046(2) Uani 1 1 d . . . C46 C 0.3480(6) 0.4376(3) 0.5570(4) 0.047(2) Uani 1 1 d . . . C47 C 0.3931(7) 0.4524(3) 0.6133(4) 0.059(3) Uani 1 1 d . . . H47A H 0.3586 0.4788 0.6251 0.088 Uiso 1 1 calc R . . H47B H 0.4521 0.4656 0.6152 0.088 Uiso 1 1 calc R . . H47C H 0.3979 0.4222 0.6360 0.088 Uiso 1 1 calc R . . C51 C 0.1380(6) 0.3382(3) 0.3489(4) 0.055(2) Uani 1 1 d . . . H51 H 0.1064 0.3338 0.3748 0.077 Uiso 1 1 calc R . . C52 C 0.1167(7) 0.3081(4) 0.3046(4) 0.067(3) Uani 1 1 d . . . H52 H 0.0720 0.2829 0.3007 0.094 Uiso 1 1 calc R . . C53 C 0.1592(8) 0.3139(4) 0.2660(5) 0.082(4) Uani 1 1 d . . . H53 H 0.1424 0.2944 0.2345 0.115 Uiso 1 1 calc R . . C54 C 0.2278(7) 0.3491(4) 0.2738(4) 0.068(3) Uani 1 1 d . . . H54 H 0.2599 0.3529 0.2481 0.095 Uiso 1 1 calc R . . C55 C 0.2490(6) 0.3785(3) 0.3192(4) 0.050(2) Uani 1 1 d . . . C56 C 0.3220(6) 0.4147(3) 0.3303(4) 0.048(2) Uani 1 1 d . . . C57 C 0.3814(7) 0.4172(3) 0.2929(4) 0.060(3) Uani 1 1 d . . . H57A H 0.4286 0.4421 0.3062 0.089 Uiso 1 1 calc R . . H57B H 0.3467 0.4277 0.2579 0.089 Uiso 1 1 calc R . . H57C H 0.4071 0.3834 0.2906 0.089 Uiso 1 1 calc R . . Ni2 Ni 0.27605(9) 0.60537(5) 0.09806(6) 0.0426(3) Uani 1 1 d . . . Dy2 Dy 0.29016(3) 0.460309(17) 0.06343(2) 0.04214(14) Uani 1 1 d . . . N61 N 0.2364(4) 0.6617(2) 0.0398(3) 0.0437(17) Uani 1 1 d . . . N62 N 0.3225(4) 0.5776(2) 0.0384(3) 0.0406(16) Uani 1 1 d . . . N71 N 0.3858(4) 0.6461(2) 0.1403(3) 0.0470(18) Uani 1 1 d . . . N72 N 0.3443(5) 0.5508(2) 0.1484(3) 0.0417(17) Uani 1 1 d . . . N81 N 0.1950(4) 0.6317(2) 0.1433(3) 0.0441(17) Uani 1 1 d . . . N82 N 0.1704(5) 0.5573(2) 0.0759(3) 0.0443(17) Uani 1 1 d . . . N91 N 0.3617(4) 0.4122(2) -0.0016(3) 0.0452(17) Uani 1 1 d . . . N92 N 0.2326(5) 0.4782(2) -0.0362(3) 0.0479(18) Uani 1 1 d . . . N101 N 0.1724(5) 0.3887(2) 0.0250(3) 0.0470(18) Uani 1 1 d . . . N102 N 0.1766(5) 0.4344(2) 0.1137(3) 0.0494(18) Uani 1 1 d . . . O61 O 0.3621(3) 0.53087(18) 0.0408(2) 0.0436(14) Uani 1 1 d . . . O71 O 0.3197(3) 0.50073(18) 0.1463(2) 0.0394(13) Uani 1 1 d . . . O81 O 0.1703(3) 0.51680(18) 0.0441(2) 0.0435(13) Uani 1 1 d . . . O91 O 0.1636(4) 0.5129(2) -0.0533(3) 0.0539(16) Uani 1 1 d . . . O101 O 0.1830(4) 0.4576(2) 0.1633(3) 0.0587(17) Uani 1 1 d . . . C61 C 0.1940(6) 0.7050(3) 0.0429(4) 0.051(2) Uani 1 1 d . . . H61 H 0.1819 0.7137 0.0753 0.071 Uiso 1 1 calc R . . C62 C 0.1665(7) 0.7383(4) 0.0001(5) 0.072(3) Uani 1 1 d . . . H62 H 0.1350 0.7686 0.0031 0.101 Uiso 1 1 calc R . . C63 C 0.1859(9) 0.7263(5) -0.0455(6) 0.099(4) Uani 1 1 d . . . H63 H 0.1662 0.7479 -0.0753 0.139 Uiso 1 1 calc R . . C64 C 0.2345(8) 0.6825(4) -0.0493(5) 0.076(3) Uani 1 1 d . . . H64 H 0.2506 0.6744 -0.0807 0.107 Uiso 1 1 calc R . . C65 C 0.2588(6) 0.6508(3) -0.0046(4) 0.055(2) Uani 1 1 d . . . C66 C 0.3087(5) 0.6028(3) -0.0059(3) 0.041(2) Uani 1 1 d . . . C67 C 0.3353(6) 0.5866(3) -0.0537(4) 0.053(2) Uani 1 1 d . . . H67A H 0.3674 0.5541 -0.0466 0.079 Uiso 1 1 calc R . . H67B H 0.3733 0.6127 -0.0627 0.079 Uiso 1 1 calc R . . H67C H 0.2828 0.5821 -0.0831 0.079 Uiso 1 1 calc R . . C71 C 0.4047(6) 0.6948(3) 0.1347(4) 0.048(2) Uani 1 1 d . . . H71 H 0.3647 0.7148 0.1089 0.068 Uiso 1 1 calc R . . C72 C 0.4803(6) 0.7176(3) 0.1648(4) 0.058(3) Uani 1 1 d . . . H72 H 0.4913 0.7529 0.1605 0.081 Uiso 1 1 calc R . . C73 C 0.5385(6) 0.6892(3) 0.2007(4) 0.060(3) Uani 1 1 d . . . H73 H 0.5918 0.7040 0.2209 0.084 Uiso 1 1 calc R . . C74 C 0.5199(6) 0.6382(3) 0.2077(4) 0.054(2) Uani 1 1 d . . . H74 H 0.5601 0.6178 0.2329 0.075 Uiso 1 1 calc R . . C75 C 0.4419(6) 0.6175(3) 0.1776(3) 0.044(2) Uani 1 1 d . . . C76 C 0.4175(5) 0.5642(3) 0.1813(3) 0.0391(19) Uani 1 1 d . . . C77 C 0.4762(6) 0.5284(3) 0.2205(4) 0.056(2) Uani 1 1 d . . . C81 C 0.2093(6) 0.6691(3) 0.1793(4) 0.047(2) Uani 1 1 d . . . H81 H 0.2636 0.6871 0.1862 0.066 Uiso 1 1 calc R . . C82 C 0.1493(7) 0.6832(3) 0.2070(4) 0.058(3) Uani 1 1 d . . . H82 H 0.1624 0.7100 0.2322 0.082 Uiso 1 1 calc R . . C83 C 0.0719(6) 0.6578(3) 0.1974(4) 0.051(2) Uani 1 1 d . . . H83 H 0.0295 0.6664 0.2158 0.072 Uiso 1 1 calc R . . C84 C 0.0553(6) 0.6186(3) 0.1599(4) 0.054(2) Uani 1 1 d . . . H84 H 0.0015 0.6003 0.1529 0.076 Uiso 1 1 calc R . . C85 C 0.1159(5) 0.6067(3) 0.1336(4) 0.043(2) Uani 1 1 d . . . C86 C 0.1042(6) 0.5643(3) 0.0952(4) 0.045(2) Uani 1 1 d . . . C87 C 0.0225(6) 0.5336(3) 0.0816(4) 0.056(2) Uani 1 1 d . . . H87A H 0.0269 0.5072 0.0561 0.085 Uiso 1 1 calc R . . H87B H -0.0277 0.5560 0.0663 0.085 Uiso 1 1 calc R . . H87C H 0.0141 0.5175 0.1135 0.085 Uiso 1 1 calc R . . C91 C 0.4268(5) 0.3782(3) 0.0149(4) 0.046(2) Uani 1 1 d . . . H91 H 0.4449 0.3701 0.0513 0.064 Uiso 1 1 calc R . . C92 C 0.4694(6) 0.3542(4) -0.0187(4) 0.057(3) Uani 1 1 d . . . H92 H 0.5147 0.3297 -0.0062 0.080 Uiso 1 1 calc R . . C93 C 0.4418(7) 0.3680(4) -0.0722(4) 0.064(3) Uani 1 1 d . . . H93 H 0.4694 0.3529 -0.0965 0.090 Uiso 1 1 calc R . . C94 C 0.3777(7) 0.4020(3) -0.0892(4) 0.055(2) Uani 1 1 d . . . H94 H 0.3600 0.4113 -0.1253 0.077 Uiso 1 1 calc R . . C95 C 0.3367(6) 0.4239(3) -0.0538(4) 0.050(2) Uani 1 1 d . . . C96 C 0.2635(6) 0.4598(3) -0.0723(4) 0.046(2) Uani 1 1 d . . . C97 C 0.2281(8) 0.4726(4) -0.1294(4) 0.073(3) Uani 1 1 d . . . H97A H 0.1794 0.4969 -0.1337 0.109 Uiso 1 1 calc R . . H97B H 0.2070 0.4413 -0.1493 0.109 Uiso 1 1 calc R . . H97C H 0.2748 0.4879 -0.1427 0.109 Uiso 1 1 calc R . . C101 C 0.1693(6) 0.3619(3) -0.0191(4) 0.051(2) Uani 1 1 d . . . H101 H 0.2178 0.3654 -0.0338 0.072 Uiso 1 1 calc R . . C102 C 0.1030(7) 0.3303(3) -0.0445(4) 0.060(3) Uani 1 1 d . . . H102 H 0.1055 0.3126 -0.0755 0.084 Uiso 1 1 calc R . . C103 C 0.0322(7) 0.3250(4) -0.0234(4) 0.066(3) Uani 1 1 d . . . H103 H -0.0159 0.3037 -0.0401 0.092 Uiso 1 1 calc R . . C104 C 0.0318(6) 0.3508(4) 0.0216(4) 0.063(3) Uani 1 1 d . . . H104 H -0.0168 0.3474 0.0364 0.088 Uiso 1 1 calc R . . C105 C 0.1032(6) 0.3822(3) 0.0461(4) 0.053(2) Uani 1 1 d . . . C106 C 0.1090(6) 0.4076(3) 0.0967(4) 0.050(2) Uani 1 1 d . . . C107 C 0.0383(7) 0.4000(4) 0.1247(4) 0.070(3) Uani 1 1 d . . . H10A H 0.0554 0.4170 0.1591 0.105 Uiso 1 1 calc R . . H10B H 0.0304 0.3633 0.1298 0.105 Uiso 1 1 calc R . . H10C H -0.0170 0.4146 0.1036 0.105 Uiso 1 1 calc R . . N111 N 0.3583(5) 0.3828(3) 0.1239(3) 0.0463(17) Uani 1 1 d . . . N112 N 0.4568(5) 0.4582(2) 0.1067(3) 0.0423(17) Uani 1 1 d . . . O111 O 0.5104(4) 0.4978(2) 0.0965(3) 0.0558(16) Uani 1 1 d . . . C111 C 0.3090(7) 0.3428(3) 0.1334(4) 0.055(2) Uani 1 1 d . . . H111 H 0.2498 0.3403 0.1128 0.077 Uiso 1 1 calc R . . C112 C 0.3393(8) 0.3067(3) 0.1703(4) 0.064(3) Uani 1 1 d . . . H112 H 0.3026 0.2791 0.1747 0.089 Uiso 1 1 calc R . . C113 C 0.4242(8) 0.3103(4) 0.2016(4) 0.067(3) Uani 1 1 d . . . H113 H 0.4467 0.2862 0.2289 0.093 Uiso 1 1 calc R . . C114 C 0.4758(7) 0.3500(4) 0.1919(4) 0.064(3) Uani 1 1 d . . . H114 H 0.5352 0.3529 0.2120 0.090 Uiso 1 1 calc R . . C115 C 0.4418(6) 0.3848(3) 0.1538(4) 0.050(2) Uani 1 1 d . . . C116 C 0.4988(6) 0.4268(3) 0.1415(4) 0.049(2) Uani 1 1 d . . . C117 C 0.5924(6) 0.4293(4) 0.1681(4) 0.066(3) Uani 1 1 d . . . H11A H 0.6176 0.4604 0.1574 0.098 Uiso 1 1 calc R . . H11B H 0.6222 0.3993 0.1585 0.098 Uiso 1 1 calc R . . H11C H 0.6004 0.4297 0.2063 0.098 Uiso 1 1 calc R . . Cl1 Cl 0.41542(19) 0.25622(9) 0.35014(11) 0.0675(7) Uani 1 1 d . . . O121 O 0.3427(6) 0.2519(3) 0.3722(3) 0.095(3) Uani 1 1 d . . . O122 O 0.4875(6) 0.2283(3) 0.3820(3) 0.097(3) Uani 1 1 d . . . O123 O 0.3943(6) 0.2369(4) 0.2966(3) 0.103(3) Uani 1 1 d . . . O124 O 0.4416(6) 0.3092(3) 0.3515(4) 0.101(3) Uani 1 1 d . . . Cl2 Cl 0.59268(18) 0.26342(9) 0.11652(12) 0.0691(7) Uani 1 1 d . . . O131 O 0.6477(8) 0.3002(4) 0.1495(5) 0.162(5) Uani 1 1 d . . . O132 O 0.5407(11) 0.2362(5) 0.1444(6) 0.132(6) Uani 0.79(2) 1 d P . . O133 O 0.6439(9) 0.2308(5) 0.0961(8) 0.144(8) Uani 0.79(2) 1 d P . . O134 O 0.5411(14) 0.2957(7) 0.0849(6) 0.175(9) Uani 0.79(2) 1 d P . . O32A O 0.613(3) 0.2201(13) 0.1412(14) 0.067(13) Uiso 0.21(2) 1 d P . . O33A O 0.613(3) 0.2630(17) 0.0601(15) 0.079(14) Uiso 0.21(2) 1 d P . . O34A O 0.495(3) 0.264(2) 0.096(2) 0.102(17) Uiso 0.21(2) 1 d P . . Cl3 Cl 0.66093(15) 0.69371(8) 0.35052(9) 0.0524(5) Uani 1 1 d . . . O141 O 0.5704(4) 0.6788(3) 0.3305(3) 0.074(2) Uani 1 1 d . . . O142 O 0.6747(5) 0.7195(3) 0.4002(3) 0.077(2) Uani 1 1 d . . . O143 O 0.7144(5) 0.6483(2) 0.3587(3) 0.077(2) Uani 1 1 d . . . O144 O 0.6874(5) 0.7269(2) 0.3137(3) 0.072(2) Uani 1 1 d . . . Cl4 Cl 0.79057(15) 0.68701(8) 0.17721(10) 0.0539(5) Uani 1 1 d . . . O151 O 0.7407(5) 0.6535(3) 0.2000(3) 0.090(3) Uani 1 1 d . . . O152 O 0.8263(5) 0.7267(2) 0.2138(3) 0.080(2) Uani 1 1 d . . . O153 O 0.7380(7) 0.7096(3) 0.1314(4) 0.133(4) Uani 1 1 d . . . O154 O 0.8598(6) 0.6601(4) 0.1654(5) 0.140(4) Uani 1 1 d . . . O1M O 0.7417 0.5388 0.2776 0.245 Uani 1 1 d . . . C1M C 0.7728 0.4898 0.2857 0.168 Uani 1 1 d . . . O2M O 0.6466 0.3960 0.3384 0.121 Uani 0.50 1 d P . . C2M C 0.6228 0.4404 0.3022 0.083 Uani 0.50 1 d P . . O3M O 0.9647 0.5415 0.2479 0.088 Uani 0.50 1 d P . . C3M C 0.9742 0.4964 0.2225 0.123 Uani 0.50 1 d P . . O4M O 0.8833 0.4547 0.2277 0.074 Uiso 0.40 1 d P . . C4M C 0.9055 0.3980 0.2199 0.089 Uiso 0.40 1 d P . . O1W O 0.6801 0.4080 0.3049 0.152 Uani 0.50 1 d P . . O2W O 0.7157 0.3178 0.2645 0.156 Uani 0.40 1 d P . . O3W O 0.8506 0.3853 0.2224 0.169 Uiso 0.30 1 d P . . H41O H 0.2050 0.5124 0.5246 0.078 Uiso 1 1 d . . . H51O H 0.3804 0.4957 0.3923 0.063 Uiso 1 1 d . . . H91O H 0.1505 0.5215 -0.0281 0.053 Uiso 1 1 d . . . H95O H 0.2199 0.4768 0.1664 0.057 Uiso 1 1 d . . . H96O H 0.4750 0.5147 0.0792 0.051 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0359(7) 0.0265(6) 0.0585(9) 0.0012(6) 0.0226(6) 0.0007(5) Dy1 0.0381(3) 0.0252(2) 0.0635(3) 0.0019(2) 0.0225(2) -0.00139(19) N1 0.035(4) 0.029(3) 0.063(5) 0.003(3) 0.024(3) -0.005(3) N2 0.039(4) 0.021(3) 0.063(5) 0.002(3) 0.026(3) 0.001(3) N11 0.043(4) 0.028(3) 0.061(4) -0.005(3) 0.028(4) -0.003(3) N12 0.042(4) 0.026(3) 0.063(5) -0.006(3) 0.031(4) -0.007(3) N21 0.041(4) 0.029(3) 0.060(4) 0.000(3) 0.025(3) 0.004(3) N22 0.036(4) 0.031(3) 0.056(4) 0.001(3) 0.020(3) 0.001(3) N31 0.040(4) 0.030(3) 0.066(5) 0.000(3) 0.020(4) -0.005(3) N32 0.045(4) 0.036(4) 0.055(4) 0.002(3) 0.020(4) 0.001(3) N41 0.033(4) 0.029(3) 0.065(5) 0.008(3) 0.015(3) 0.000(3) N42 0.046(4) 0.035(4) 0.072(5) 0.000(3) 0.030(4) -0.003(3) N51 0.036(4) 0.032(3) 0.071(5) -0.003(3) 0.023(4) -0.004(3) N52 0.032(4) 0.024(3) 0.080(5) 0.005(3) 0.030(4) 0.002(3) O1 0.038(3) 0.022(2) 0.065(4) 0.004(2) 0.019(3) -0.002(2) O11 0.042(3) 0.022(2) 0.064(4) 0.000(2) 0.026(3) -0.004(2) O21 0.041(3) 0.024(2) 0.055(3) 0.004(2) 0.023(3) 0.005(2) O31 0.047(4) 0.063(4) 0.075(5) 0.016(3) 0.010(3) -0.013(3) O41 0.058(4) 0.034(3) 0.064(4) -0.006(3) 0.023(3) -0.001(3) O51 0.052(4) 0.035(3) 0.082(4) -0.001(3) 0.040(3) -0.005(3) C1 0.044(5) 0.033(4) 0.066(6) -0.003(4) 0.020(4) 0.001(4) C2 0.050(5) 0.037(4) 0.066(6) 0.008(4) 0.024(5) -0.012(4) C3 0.040(5) 0.045(5) 0.061(6) 0.011(4) 0.022(4) -0.002(4) C4 0.049(5) 0.035(4) 0.070(6) 0.003(4) 0.032(5) 0.002(4) C5 0.034(4) 0.035(4) 0.057(5) 0.009(4) 0.026(4) 0.009(3) C6 0.038(5) 0.029(4) 0.057(5) 0.000(3) 0.019(4) 0.004(3) C7 0.069(6) 0.034(4) 0.063(6) -0.002(4) 0.027(5) 0.003(4) C11 0.057(6) 0.032(4) 0.078(6) 0.002(4) 0.046(5) 0.004(4) C12 0.071(7) 0.036(5) 0.082(7) -0.017(5) 0.035(6) 0.002(5) C13 0.091(8) 0.052(6) 0.080(8) -0.018(5) 0.034(7) 0.004(6) C14 0.078(7) 0.050(6) 0.059(6) -0.013(5) 0.018(5) 0.000(5) C15 0.036(5) 0.029(4) 0.061(5) 0.002(4) 0.021(4) -0.004(3) C16 0.046(5) 0.035(4) 0.048(5) -0.003(4) 0.017(4) -0.005(4) C17 0.048(5) 0.038(5) 0.058(6) 0.000(4) 0.009(4) 0.001(4) C21 0.046(5) 0.033(4) 0.064(6) 0.000(4) 0.027(4) 0.004(4) C22 0.047(5) 0.035(4) 0.063(6) 0.009(4) 0.026(4) 0.016(4) C23 0.039(5) 0.041(5) 0.070(6) -0.006(4) 0.024(5) 0.011(4) C24 0.043(5) 0.035(4) 0.066(6) -0.006(4) 0.025(4) 0.001(4) C25 0.042(5) 0.029(4) 0.058(5) 0.000(4) 0.021(4) 0.002(4) C26 0.030(5) 0.038(4) 0.067(6) -0.002(4) 0.023(4) -0.009(4) C27 0.041(5) 0.047(5) 0.087(7) 0.015(5) 0.036(5) -0.001(4) C31 0.052(5) 0.030(4) 0.072(6) -0.006(4) 0.029(5) -0.009(4) C32 0.059(6) 0.035(5) 0.086(7) 0.008(4) 0.038(5) -0.001(4) C33 0.055(6) 0.035(5) 0.086(7) -0.010(4) 0.036(5) -0.013(4) C34 0.045(5) 0.039(5) 0.078(7) 0.000(4) 0.023(5) -0.005(4) C35 0.052(6) 0.027(4) 0.071(6) -0.003(4) 0.030(5) -0.011(4) C36 0.050(6) 0.028(4) 0.086(7) -0.005(4) 0.027(5) -0.013(4) C37 0.036(5) 0.055(6) 0.100(8) 0.016(5) 0.002(5) -0.015(4) C41 0.046(5) 0.034(4) 0.072(6) 0.010(4) 0.027(5) 0.002(4) C42 0.047(6) 0.039(5) 0.089(8) 0.005(5) 0.021(5) 0.002(4) C43 0.046(6) 0.046(5) 0.098(8) 0.008(5) 0.020(6) 0.006(4) C44 0.060(6) 0.047(5) 0.076(7) 0.007(5) 0.017(5) -0.006(5) C45 0.048(5) 0.030(4) 0.070(6) 0.015(4) 0.030(5) 0.001(4) C46 0.047(5) 0.036(4) 0.063(6) 0.007(4) 0.021(5) -0.006(4) C47 0.069(7) 0.047(5) 0.064(7) 0.002(4) 0.024(5) -0.002(5) C51 0.051(6) 0.039(5) 0.073(6) -0.013(4) 0.015(5) 0.000(4) C52 0.070(7) 0.058(6) 0.085(8) -0.011(5) 0.039(6) -0.010(5) C53 0.097(9) 0.068(7) 0.086(8) -0.040(6) 0.033(7) -0.007(7) C54 0.093(8) 0.045(5) 0.074(7) -0.009(5) 0.038(6) 0.002(5) C55 0.056(6) 0.034(4) 0.063(6) -0.001(4) 0.021(5) 0.002(4) C56 0.047(5) 0.032(4) 0.072(6) 0.013(4) 0.029(5) 0.009(4) C57 0.069(7) 0.038(5) 0.087(7) 0.009(5) 0.048(6) 0.012(5) Ni2 0.0406(8) 0.0252(6) 0.0668(9) -0.0034(6) 0.0226(7) -0.0010(6) Dy2 0.0432(3) 0.0250(2) 0.0649(3) -0.0029(2) 0.0259(3) -0.00160(19) N61 0.033(4) 0.031(3) 0.069(5) 0.000(3) 0.017(4) -0.004(3) N62 0.032(4) 0.024(3) 0.070(5) 0.003(3) 0.021(3) 0.001(3) N71 0.039(4) 0.030(3) 0.079(5) -0.005(3) 0.028(4) 0.000(3) N72 0.053(5) 0.020(3) 0.063(5) -0.006(3) 0.034(4) -0.002(3) N81 0.035(4) 0.035(4) 0.067(5) 0.002(3) 0.021(3) 0.003(3) N82 0.040(4) 0.032(4) 0.066(5) -0.004(3) 0.023(4) 0.003(3) N91 0.045(4) 0.032(3) 0.066(5) -0.007(3) 0.028(4) -0.002(3) N92 0.042(4) 0.029(3) 0.075(5) 0.002(3) 0.018(4) -0.002(3) N101 0.054(5) 0.027(3) 0.064(5) 0.002(3) 0.020(4) -0.005(3) N102 0.045(4) 0.033(4) 0.081(5) -0.010(3) 0.035(4) -0.003(3) O61 0.042(3) 0.026(3) 0.068(4) 0.001(2) 0.023(3) 0.000(2) O71 0.048(3) 0.027(3) 0.049(3) -0.002(2) 0.023(3) -0.004(2) O81 0.041(3) 0.026(3) 0.066(4) -0.008(2) 0.019(3) -0.002(2) O91 0.045(4) 0.041(3) 0.080(4) 0.002(3) 0.026(3) 0.003(3) O101 0.076(5) 0.041(3) 0.073(4) -0.019(3) 0.046(4) -0.014(3) C61 0.052(5) 0.022(4) 0.087(7) -0.002(4) 0.032(5) 0.004(4) C62 0.080(8) 0.038(5) 0.117(9) 0.010(6) 0.060(7) 0.020(5) C63 0.124(11) 0.066(8) 0.131(11) 0.050(8) 0.076(10) 0.039(8) C64 0.115(9) 0.046(6) 0.086(8) 0.022(5) 0.057(7) 0.015(6) C65 0.052(6) 0.031(4) 0.094(8) -0.002(4) 0.037(5) 0.001(4) C66 0.039(5) 0.022(4) 0.066(6) -0.003(4) 0.023(4) -0.003(3) C67 0.061(6) 0.040(5) 0.063(6) 0.004(4) 0.027(5) 0.010(4) C71 0.043(5) 0.028(4) 0.079(6) -0.004(4) 0.026(5) 0.000(4) C72 0.054(6) 0.030(4) 0.091(7) -0.016(5) 0.020(5) -0.007(4) C73 0.051(6) 0.045(5) 0.089(7) -0.005(5) 0.028(5) -0.014(5) C74 0.047(5) 0.046(5) 0.076(7) -0.009(5) 0.031(5) -0.008(4) C75 0.045(5) 0.037(4) 0.056(5) -0.004(4) 0.022(4) -0.003(4) C76 0.034(5) 0.037(4) 0.052(5) -0.007(4) 0.022(4) -0.009(4) C77 0.062(6) 0.043(5) 0.064(6) 0.004(4) 0.017(5) 0.007(4) C81 0.043(5) 0.033(4) 0.070(6) -0.002(4) 0.023(5) 0.006(4) C82 0.063(6) 0.040(5) 0.070(7) -0.008(4) 0.014(5) 0.010(5) C83 0.057(6) 0.039(5) 0.068(6) 0.003(4) 0.036(5) 0.012(4) C84 0.040(5) 0.044(5) 0.083(7) 0.001(5) 0.024(5) 0.007(4) C85 0.034(5) 0.031(4) 0.072(6) 0.002(4) 0.026(4) 0.009(4) C86 0.039(5) 0.028(4) 0.071(6) -0.003(4) 0.020(5) 0.002(4) C87 0.043(5) 0.049(5) 0.084(7) -0.007(5) 0.027(5) -0.011(4) C91 0.038(5) 0.034(4) 0.066(6) -0.004(4) 0.017(4) -0.002(4) C92 0.046(6) 0.047(5) 0.087(8) -0.009(5) 0.033(5) -0.004(4) C93 0.061(7) 0.059(6) 0.091(8) -0.016(6) 0.052(6) -0.018(5) C94 0.067(7) 0.043(5) 0.066(6) -0.002(4) 0.037(5) -0.004(5) C95 0.057(6) 0.034(4) 0.067(6) -0.004(4) 0.031(5) -0.012(4) C96 0.053(6) 0.032(4) 0.063(6) -0.005(4) 0.030(5) -0.008(4) C97 0.101(9) 0.055(6) 0.067(7) 0.002(5) 0.032(6) 0.010(6) C101 0.056(6) 0.033(4) 0.067(6) -0.004(4) 0.022(5) -0.007(4) C102 0.070(7) 0.035(5) 0.080(7) -0.007(4) 0.027(6) -0.008(5) C103 0.060(6) 0.052(6) 0.089(8) -0.020(5) 0.027(6) -0.025(5) C104 0.047(6) 0.053(6) 0.095(8) -0.006(5) 0.031(6) -0.009(5) C105 0.045(5) 0.030(4) 0.094(7) 0.001(4) 0.034(5) -0.005(4) C106 0.044(5) 0.032(4) 0.082(7) 0.006(4) 0.032(5) -0.004(4) C107 0.075(7) 0.052(6) 0.100(8) -0.013(5) 0.054(7) -0.013(5) N111 0.054(5) 0.038(4) 0.057(5) 0.003(3) 0.031(4) 0.008(3) N112 0.049(4) 0.029(3) 0.057(4) 0.001(3) 0.027(4) -0.001(3) O111 0.047(4) 0.040(3) 0.081(4) 0.005(3) 0.017(3) -0.003(3) C111 0.071(7) 0.030(4) 0.075(7) 0.001(4) 0.038(5) 0.001(4) C112 0.090(8) 0.033(5) 0.090(8) 0.005(5) 0.063(7) 0.008(5) C113 0.079(8) 0.056(6) 0.081(8) 0.022(5) 0.050(7) 0.024(6) C114 0.065(7) 0.054(6) 0.079(7) 0.015(5) 0.029(6) 0.016(5) C115 0.052(6) 0.035(4) 0.073(6) -0.001(4) 0.034(5) 0.011(4) C116 0.045(5) 0.041(5) 0.069(6) -0.001(4) 0.029(5) 0.005(4) C117 0.054(6) 0.068(7) 0.081(7) 0.016(6) 0.029(6) 0.006(5) Cl1 0.0834(19) 0.0443(12) 0.0851(19) 0.0113(12) 0.0406(15) 0.0129(12) O121 0.098(6) 0.102(6) 0.107(6) -0.014(5) 0.067(5) -0.011(5) O122 0.122(7) 0.080(5) 0.092(6) 0.025(5) 0.034(5) 0.046(5) O123 0.132(8) 0.105(7) 0.087(6) -0.015(5) 0.058(6) -0.013(6) O124 0.119(7) 0.046(4) 0.150(8) 0.012(5) 0.060(6) 0.006(4) Cl2 0.0717(17) 0.0401(12) 0.101(2) -0.0013(12) 0.0318(15) 0.0080(12) O131 0.157(10) 0.128(9) 0.224(13) -0.105(9) 0.090(10) -0.069(8) O132 0.162(15) 0.091(9) 0.177(14) 0.036(9) 0.103(11) 0.007(9) O133 0.115(10) 0.102(10) 0.25(2) -0.061(13) 0.111(12) 0.011(8) O134 0.23(2) 0.162(15) 0.144(13) 0.097(12) 0.064(13) 0.118(15) Cl3 0.0510(13) 0.0381(10) 0.0729(15) 0.0012(10) 0.0246(11) -0.0017(9) O141 0.047(4) 0.090(5) 0.085(5) 0.005(4) 0.017(4) -0.006(4) O142 0.096(6) 0.063(4) 0.078(5) -0.016(4) 0.037(4) -0.001(4) O143 0.065(5) 0.048(4) 0.123(6) 0.002(4) 0.032(4) 0.013(3) O144 0.093(5) 0.052(4) 0.081(5) 0.007(3) 0.042(4) -0.022(4) Cl4 0.0515(13) 0.0388(11) 0.0766(16) 0.0051(10) 0.0262(12) -0.0028(10) O151 0.103(6) 0.091(6) 0.091(6) -0.004(4) 0.051(5) -0.044(5) O152 0.109(6) 0.043(4) 0.075(5) 0.002(3) 0.003(4) -0.005(4) O153 0.162(9) 0.065(5) 0.123(7) 0.039(5) -0.049(7) -0.015(6) O154 0.077(6) 0.154(10) 0.214(11) -0.061(9) 0.083(7) 0.009(6) O1M 0.240 0.340 0.199 -0.024 0.137 -0.057 C1M 0.155 0.134 0.254 0.119 0.121 0.055 O2M 0.112 0.190 0.075 0.032 0.048 -0.011 C2M 0.089 0.105 0.043 0.007 -0.004 0.022 O3M 0.050 0.152 0.060 0.032 0.009 0.010 C3M 0.099 0.172 0.068 -0.076 -0.029 0.091 O1W 0.138 0.199 0.076 0.025 -0.044 0.019 O2W 0.102 0.140 0.184 0.013 -0.038 0.061 _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 Ni1 N12 2.032(7) . ? Ni1 N22 2.041(7) . ? Ni1 N2 2.047(7) . ? Ni1 N21 2.081(7) . ? Ni1 N1 2.102(6) . ? Ni1 N11 2.103(7) . ? Dy1 O1 2.328(5) . ? Dy1 O11 2.340(5) . ? Dy1 O21 2.346(5) . ? Dy1 N32 2.579(7) . ? Dy1 N52 2.588(7) . ? Dy1 N42 2.595(8) . ? Dy1 N41 2.601(6) . ? Dy1 N51 2.617(7) . ? Dy1 N31 2.638(7) . ? N1 C1 1.329(10) . ? N1 C5 1.365(10) . ? N2 C6 1.273(10) . ? N2 O1 1.365(7) . ? N11 C15 1.358(10) . ? N11 C11 1.362(10) . ? N12 C16 1.289(10) . ? N12 O11 1.375(7) . ? N21 C21 1.330(10) . ? N21 C25 1.346(10) . ? N22 C26 1.294(10) . ? N22 O21 1.375(7) . ? N31 C31 1.333(10) . ? N31 C35 1.351(10) . ? N32 C36 1.285(10) . ? N32 O31 1.378(9) . ? N41 C41 1.344(10) . ? N41 C45 1.358(11) . ? N42 C46 1.309(11) . ? N42 O41 1.359(8) . ? N51 C51 1.372(10) . ? N51 C55 1.379(11) . ? N52 C56 1.271(11) . ? N52 O51 1.396(8) . ? O31 H31O 0.8400 . ? O41 H41O 0.9117 . ? O51 H51O 0.6949 . ? C1 C2 1.385(11) . ? C1 H1 0.9500 . ? C2 C3 1.366(12) . ? C2 H2 0.9500 . ? C3 C4 1.389(11) . ? C3 H3 0.9500 . ? C4 C5 1.386(11) . ? C4 H4 0.9500 . ? C5 C6 1.473(10) . ? C6 C7 1.511(11) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C11 C12 1.408(12) . ? C11 H11 0.9500 . ? C12 C13 1.388(14) . ? C12 H12 0.9500 . ? C13 C14 1.394(13) . ? C13 H13 0.9500 . ? C14 C15 1.360(12) . ? C14 H14 0.9500 . ? C15 C16 1.490(11) . ? C16 C17 1.480(11) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C21 C22 1.390(11) . ? C21 H21 0.9500 . ? C22 C23 1.356(11) . ? C22 H22 0.9500 . ? C23 C24 1.385(12) . ? C23 H23 0.9500 . ? C24 C25 1.394(11) . ? C24 H24 0.9500 . ? C25 C26 1.457(11) . ? C26 C27 1.521(11) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C31 C32 1.369(11) . ? C31 H31 0.9500 . ? C32 C33 1.375(12) . ? C32 H32 0.9500 . ? C33 C34 1.394(12) . ? C33 H33 0.9500 . ? C34 C35 1.382(11) . ? C34 H34 0.9500 . ? C35 C36 1.481(12) . ? C36 C37 1.529(12) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C41 C42 1.396(12) . ? C41 H41 0.9500 . ? C42 C43 1.368(14) . ? C42 H42 0.9500 . ? C43 C44 1.387(13) . ? C43 H43 0.9500 . ? C44 C45 1.412(12) . ? C44 H44 0.9500 . ? C45 C46 1.468(12) . ? C46 C47 1.516(13) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C51 C52 1.375(13) . ? C51 H51 0.9500 . ? C52 C53 1.364(14) . ? C52 H52 0.9500 . ? C53 C54 1.393(14) . ? C53 H53 0.9500 . ? C54 C55 1.387(13) . ? C54 H54 0.9500 . ? C55 C56 1.459(12) . ? C56 C57 1.530(12) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? Ni2 N62 2.034(7) . ? Ni2 N82 2.044(7) . ? Ni2 N72 2.049(7) . ? Ni2 N81 2.082(7) . ? Ni2 N71 2.085(7) . ? Ni2 N61 2.100(7) . ? Dy2 O61 2.324(5) . ? Dy2 O81 2.346(5) . ? Dy2 O71 2.358(5) . ? Dy2 N112 2.573(7) . ? Dy2 N102 2.582(7) . ? Dy2 N92 2.583(8) . ? Dy2 N91 2.608(7) . ? Dy2 N111 2.626(7) . ? Dy2 N101 2.644(7) . ? N61 C61 1.329(10) . ? N61 C65 1.338(11) . ? N62 C66 1.308(10) . ? N62 O61 1.366(7) . ? N71 C71 1.325(10) . ? N71 C75 1.359(10) . ? N72 C76 1.295(10) . ? N72 O71 1.362(7) . ? N81 C81 1.338(10) . ? N81 C85 1.370(10) . ? N82 C86 1.288(11) . ? N82 O81 1.351(8) . ? N91 C91 1.341(10) . ? N91 C95 1.361(11) . ? N92 C96 1.273(11) . ? N92 O91 1.397(8) . ? N101 C101 1.344(11) . ? N101 C105 1.359(11) . ? N102 C106 1.255(10) . ? N102 O101 1.421(9) . ? O91 H91O 0.7783 . ? O101 H95O 0.7563 . ? C61 C62 1.399(13) . ? C61 H61 0.9500 . ? C62 C63 1.353(16) . ? C62 H62 0.9500 . ? C63 C64 1.396(15) . ? C63 H63 0.9500 . ? C64 C65 1.406(13) . ? C64 H64 0.9500 . ? C65 C66 1.489(11) . ? C66 C67 1.487(12) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C71 C72 1.381(12) . ? C71 H71 0.9500 . ? C72 C73 1.352(13) . ? C72 H72 0.9500 . ? C73 C74 1.387(12) . ? C73 H73 0.9500 . ? C74 C75 1.386(12) . ? C74 H74 0.9500 . ? C75 C76 1.454(11) . ? C76 C77 1.514(12) . ? C81 C82 1.389(12) . ? C81 H81 0.9500 . ? C82 C83 1.353(12) . ? C82 H82 0.9500 . ? C83 C84 1.399(12) . ? C83 H83 0.9500 . ? C84 C85 1.355(12) . ? C84 H84 0.9500 . ? C85 C86 1.481(11) . ? C86 C87 1.478(11) . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C91 C92 1.394(12) . ? C91 H91 0.9500 . ? C92 C93 1.406(14) . ? C92 H92 0.9500 . ? C93 C94 1.333(13) . ? C93 H93 0.9500 . ? C94 C95 1.388(12) . ? C94 H94 0.9500 . ? C95 C96 1.467(12) . ? C96 C97 1.497(13) . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C101 C102 1.361(12) . ? C101 H101 0.9500 . ? C102 C103 1.379(13) . ? C102 H102 0.9500 . ? C103 C104 1.364(13) . ? C103 H103 0.9500 . ? C104 C105 1.406(12) . ? C104 H104 0.9500 . ? C105 C106 1.471(13) . ? C106 C107 1.503(12) . ? C107 H10A 0.9800 . ? C107 H10B 0.9800 . ? C107 H10C 0.9800 . ? N111 C115 1.345(11) . ? N111 C111 1.363(11) . ? N112 C116 1.276(11) . ? N112 O111 1.407(8) . ? O111 H96O 0.7617 . ? C111 C112 1.351(13) . ? C111 H111 0.9500 . ? C112 C113 1.376(15) . ? C112 H112 0.9500 . ? C113 C114 1.384(14) . ? C113 H113 0.9500 . ? C114 C115 1.355(12) . ? C114 H114 0.9500 . ? C115 C116 1.508(12) . ? C116 C117 1.459(13) . ? C117 H11A 0.9800 . ? C117 H11B 0.9800 . ? C117 H11C 0.9800 . ? Cl1 O121 1.421(8) . ? Cl1 O122 1.422(8) . ? Cl1 O124 1.443(8) . ? Cl1 O123 1.450(8) . ? Cl2 O32A 1.30(3) . ? Cl2 O134 1.307(11) . ? Cl2 O133 1.377(11) . ? Cl2 O131 1.426(9) . ? Cl2 O132 1.427(13) . ? Cl2 O34A 1.48(5) . ? Cl2 O33A 1.60(4) . ? O132 O32A 1.24(4) . ? O132 O34A 1.48(5) . ? O133 O33A 1.26(4) . ? O133 O32A 1.42(4) . ? O134 O34A 1.18(5) . ? O134 O33A 1.69(4) . ? Cl3 O142 1.436(7) . ? Cl3 O141 1.439(7) . ? Cl3 O143 1.439(7) . ? Cl3 O144 1.441(6) . ? Cl4 O154 1.400(8) . ? Cl4 O153 1.402(8) . ? Cl4 O151 1.412(7) . ? Cl4 O152 1.427(7) . ? O1M C1M 1.3700 . ? O2M O1W 1.1827 . ? O2M C2M 1.4864 . ? C2M O1W 1.2278 . ? O3M C3M 1.3842 . ? C3M O4M 1.8347 . ? O4M C4M 1.5501 . ? C4M O3W 0.9454 . ? 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 N12 Ni1 N22 91.9(3) . . ? N12 Ni1 N2 89.7(3) . . ? N22 Ni1 N2 89.9(3) . . ? N12 Ni1 N21 167.4(3) . . ? N22 Ni1 N21 78.1(3) . . ? N2 Ni1 N21 97.9(3) . . ? N12 Ni1 N1 96.7(3) . . ? N22 Ni1 N1 164.7(3) . . ? N2 Ni1 N1 77.6(3) . . ? N21 Ni1 N1 94.8(3) . . ? N12 Ni1 N11 76.7(3) . . ? N22 Ni1 N11 101.3(3) . . ? N2 Ni1 N11 162.5(3) . . ? N21 Ni1 N11 97.5(3) . . ? N1 Ni1 N11 93.0(3) . . ? O1 Dy1 O11 84.08(18) . . ? O1 Dy1 O21 83.53(18) . . ? O11 Dy1 O21 83.39(17) . . ? O1 Dy1 N32 67.4(2) . . ? O11 Dy1 N32 143.22(19) . . ? O21 Dy1 N32 71.16(19) . . ? O1 Dy1 N52 69.93(19) . . ? O11 Dy1 N52 66.0(2) . . ? O21 Dy1 N52 140.75(18) . . ? N32 Dy1 N52 120.3(2) . . ? O1 Dy1 N42 140.83(19) . . ? O11 Dy1 N42 68.6(2) . . ? O21 Dy1 N42 66.4(2) . . ? N32 Dy1 N42 120.7(2) . . ? N52 Dy1 N42 118.9(2) . . ? O1 Dy1 N41 144.4(2) . . ? O11 Dy1 N41 82.79(18) . . ? O21 Dy1 N41 127.3(2) . . ? N32 Dy1 N41 133.8(2) . . ? N52 Dy1 N41 74.5(2) . . ? N42 Dy1 N41 61.1(2) . . ? O1 Dy1 N51 80.4(2) . . ? O11 Dy1 N51 126.6(2) . . ? O21 Dy1 N51 143.69(19) . . ? N32 Dy1 N51 72.6(2) . . ? N52 Dy1 N51 60.6(2) . . ? N42 Dy1 N51 138.5(2) . . ? N41 Dy1 N51 81.3(2) . . ? O1 Dy1 N31 128.3(2) . . ? O11 Dy1 N31 143.0(2) . . ? O21 Dy1 N31 83.39(19) . . ? N32 Dy1 N31 61.0(2) . . ? N52 Dy1 N31 135.8(2) . . ? N42 Dy1 N31 74.5(2) . . ? N41 Dy1 N31 78.2(2) . . ? N51 Dy1 N31 81.5(2) . . ? C1 N1 C5 117.8(7) . . ? C1 N1 Ni1 129.1(6) . . ? C5 N1 Ni1 113.1(5) . . ? C6 N2 O1 118.8(6) . . ? C6 N2 Ni1 118.6(5) . . ? O1 N2 Ni1 122.6(5) . . ? C15 N11 C11 118.7(7) . . ? C15 N11 Ni1 114.7(5) . . ? C11 N11 Ni1 126.5(6) . . ? C16 N12 O11 117.9(7) . . ? C16 N12 Ni1 120.3(5) . . ? O11 N12 Ni1 121.8(5) . . ? C21 N21 C25 118.3(7) . . ? C21 N21 Ni1 128.4(6) . . ? C25 N21 Ni1 113.2(5) . . ? C26 N22 O21 119.9(6) . . ? C26 N22 Ni1 117.6(5) . . ? O21 N22 Ni1 122.1(5) . . ? C31 N31 C35 115.1(7) . . ? C31 N31 Dy1 124.4(5) . . ? C35 N31 Dy1 120.3(5) . . ? C36 N32 O31 114.9(7) . . ? C36 N32 Dy1 125.4(6) . . ? O31 N32 Dy1 119.4(5) . . ? C41 N41 C45 117.9(7) . . ? C41 N41 Dy1 121.3(6) . . ? C45 N41 Dy1 120.7(5) . . ? C46 N42 O41 114.5(7) . . ? C46 N42 Dy1 124.5(6) . . ? O41 N42 Dy1 119.5(5) . . ? C51 N51 C55 117.1(8) . . ? C51 N51 Dy1 122.1(6) . . ? C55 N51 Dy1 119.2(5) . . ? C56 N52 O51 113.4(7) . . ? C56 N52 Dy1 125.6(6) . . ? O51 N52 Dy1 120.6(5) . . ? N2 O1 Dy1 115.6(4) . . ? N12 O11 Dy1 118.7(4) . . ? N22 O21 Dy1 116.3(4) . . ? N32 O31 H31O 109.5 . . ? N42 O41 H41O 101.7 . . ? N52 O51 H51O 96.2 . . ? N1 C1 C2 123.8(8) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C3 C2 C1 118.4(8) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 119.1(8) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 119.6(8) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N1 C5 C4 121.1(7) . . ? N1 C5 C6 115.3(7) . . ? C4 C5 C6 123.5(8) . . ? N2 C6 C5 114.9(7) . . ? N2 C6 C7 124.8(7) . . ? C5 C6 C7 120.2(8) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N11 C11 C12 121.4(9) . . ? N11 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C13 C12 C11 118.8(9) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C12 C13 C14 118.6(10) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? C15 C14 C13 120.5(10) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? N11 C15 C14 122.0(8) . . ? N11 C15 C16 114.2(7) . . ? C14 C15 C16 123.8(8) . . ? N12 C16 C17 125.3(7) . . ? N12 C16 C15 113.7(7) . . ? C17 C16 C15 121.0(7) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N21 C21 C22 123.3(8) . . ? N21 C21 H21 118.4 . . ? C22 C21 H21 118.4 . . ? C23 C22 C21 119.3(8) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C22 C23 C24 118.0(8) . . ? C22 C23 H23 121.0 . . ? C24 C23 H23 121.0 . . ? C23 C24 C25 120.6(8) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? N21 C25 C24 120.6(7) . . ? N21 C25 C26 116.4(7) . . ? C24 C25 C26 122.9(8) . . ? N22 C26 C25 114.7(7) . . ? N22 C26 C27 123.8(8) . . ? C25 C26 C27 121.5(7) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N31 C31 C32 126.3(9) . . ? N31 C31 H31 116.8 . . ? C32 C31 H31 116.8 . . ? C31 C32 C33 117.5(9) . . ? C31 C32 H32 121.2 . . ? C33 C32 H32 121.2 . . ? C32 C33 C34 118.8(9) . . ? C32 C33 H33 120.6 . . ? C34 C33 H33 120.6 . . ? C35 C34 C33 118.7(9) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? N31 C35 C34 123.4(9) . . ? N31 C35 C36 116.6(7) . . ? C34 C35 C36 120.0(8) . . ? N32 C36 C35 115.9(8) . . ? N32 C36 C37 122.9(9) . . ? C35 C36 C37 121.2(8) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N41 C41 C42 123.6(9) . . ? N41 C41 H41 118.2 . . ? C42 C41 H41 118.2 . . ? C43 C42 C41 117.4(9) . . ? C43 C42 H42 121.3 . . ? C41 C42 H42 121.3 . . ? C42 C43 C44 121.6(9) . . ? C42 C43 H43 119.2 . . ? C44 C43 H43 119.2 . . ? C43 C44 C45 117.3(9) . . ? C43 C44 H44 121.4 . . ? C45 C44 H44 121.4 . . ? N41 C45 C44 122.1(8) . . ? N41 C45 C46 117.9(8) . . ? C44 C45 C46 119.9(9) . . ? N42 C46 C45 114.3(8) . . ? N42 C46 C47 124.8(8) . . ? C45 C46 C47 120.9(8) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N51 C51 C52 122.1(10) . . ? N51 C51 H51 119.0 . . ? C52 C51 H51 119.0 . . ? C53 C52 C51 120.7(10) . . ? C53 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? C52 C53 C54 118.7(10) . . ? C52 C53 H53 120.6 . . ? C54 C53 H53 120.6 . . ? C55 C54 C53 119.5(10) . . ? C55 C54 H54 120.2 . . ? C53 C54 H54 120.2 . . ? N51 C55 C54 121.8(9) . . ? N51 C55 C56 116.2(8) . . ? C54 C55 C56 122.0(9) . . ? N52 C56 C55 115.6(8) . . ? N52 C56 C57 125.4(8) . . ? C55 C56 C57 118.9(8) . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N62 Ni2 N82 89.6(3) . . ? N62 Ni2 N72 90.9(3) . . ? N82 Ni2 N72 90.3(3) . . ? N62 Ni2 N81 163.9(3) . . ? N82 Ni2 N81 77.9(3) . . ? N72 Ni2 N81 99.0(3) . . ? N62 Ni2 N71 100.2(3) . . ? N82 Ni2 N71 164.7(3) . . ? N72 Ni2 N71 77.9(3) . . ? N81 Ni2 N71 94.2(3) . . ? N62 Ni2 N61 77.6(3) . . ? N82 Ni2 N61 99.2(3) . . ? N72 Ni2 N61 164.9(3) . . ? N81 Ni2 N61 94.4(3) . . ? N71 Ni2 N61 94.4(3) . . ? O61 Dy2 O81 82.20(18) . . ? O61 Dy2 O71 83.72(19) . . ? O81 Dy2 O71 82.52(18) . . ? O61 Dy2 N112 67.69(19) . . ? O81 Dy2 N112 141.20(18) . . ? O71 Dy2 N112 70.8(2) . . ? O61 Dy2 N102 142.27(19) . . ? O81 Dy2 N102 69.4(2) . . ? O71 Dy2 N102 68.7(2) . . ? N112 Dy2 N102 122.1(2) . . ? O61 Dy2 N92 70.2(2) . . ? O81 Dy2 N92 67.6(2) . . ? O71 Dy2 N92 142.18(19) . . ? N112 Dy2 N92 119.8(2) . . ? N102 Dy2 N92 117.6(2) . . ? O61 Dy2 N91 83.7(2) . . ? O81 Dy2 N91 128.6(2) . . ? O71 Dy2 N91 144.1(2) . . ? N112 Dy2 N91 73.3(2) . . ? N102 Dy2 N91 133.5(2) . . ? N92 Dy2 N91 61.1(2) . . ? O61 Dy2 N111 128.3(2) . . ? O81 Dy2 N111 142.6(2) . . ? O71 Dy2 N111 80.56(19) . . ? N112 Dy2 N111 60.6(2) . . ? N102 Dy2 N111 73.4(2) . . ? N92 Dy2 N111 137.1(2) . . ? N91 Dy2 N111 81.2(2) . . ? O61 Dy2 N101 143.6(2) . . ? O81 Dy2 N101 85.37(19) . . ? O71 Dy2 N101 128.3(2) . . ? N112 Dy2 N101 133.3(2) . . ? N102 Dy2 N101 59.9(2) . . ? N92 Dy2 N101 73.5(2) . . ? N91 Dy2 N101 77.8(2) . . ? N111 Dy2 N101 79.5(2) . . ? C61 N61 C65 119.2(8) . . ? C61 N61 Ni2 127.6(7) . . ? C65 N61 Ni2 113.2(5) . . ? C66 N62 O61 117.2(7) . . ? C66 N62 Ni2 120.1(5) . . ? O61 N62 Ni2 122.5(5) . . ? C71 N71 C75 119.2(7) . . ? C71 N71 Ni2 127.6(6) . . ? C75 N71 Ni2 113.2(5) . . ? C76 N72 O71 118.8(7) . . ? C76 N72 Ni2 117.8(5) . . ? O71 N72 Ni2 123.3(5) . . ? C81 N81 C85 117.2(7) . . ? C81 N81 Ni2 129.2(6) . . ? C85 N81 Ni2 113.6(5) . . ? C86 N82 O81 119.1(7) . . ? C86 N82 Ni2 119.0(6) . . ? O81 N82 Ni2 121.8(5) . . ? C91 N91 C95 117.9(8) . . ? C91 N91 Dy2 122.3(6) . . ? C95 N91 Dy2 119.7(5) . . ? C96 N92 O91 115.1(7) . . ? C96 N92 Dy2 126.2(6) . . ? O91 N92 Dy2 118.6(5) . . ? C101 N101 C105 116.0(8) . . ? C101 N101 Dy2 124.2(6) . . ? C105 N101 Dy2 119.3(6) . . ? C106 N102 O101 114.4(7) . . ? C106 N102 Dy2 127.0(7) . . ? O101 N102 Dy2 118.0(5) . . ? N62 O61 Dy2 118.3(4) . . ? N72 O71 Dy2 116.9(4) . . ? N82 O81 Dy2 119.3(4) . . ? N92 O91 H91O 105.9 . . ? N102 O101 H95O 104.3 . . ? N61 C61 C62 122.3(9) . . ? N61 C61 H61 118.9 . . ? C62 C61 H61 118.9 . . ? C63 C62 C61 118.5(9) . . ? C63 C62 H62 120.8 . . ? C61 C62 H62 120.8 . . ? C62 C63 C64 120.7(11) . . ? C62 C63 H63 119.7 . . ? C64 C63 H63 119.7 . . ? C63 C64 C65 117.2(10) . . ? C63 C64 H64 121.4 . . ? C65 C64 H64 121.4 . . ? N61 C65 C64 122.0(8) . . ? N61 C65 C66 117.6(8) . . ? C64 C65 C66 120.4(9) . . ? N62 C66 C67 126.4(7) . . ? N62 C66 C65 111.6(8) . . ? C67 C66 C65 121.9(8) . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N71 C71 C72 122.4(9) . . ? N71 C71 H71 118.8 . . ? C72 C71 H71 118.8 . . ? C73 C72 C71 119.2(8) . . ? C73 C72 H72 120.4 . . ? C71 C72 H72 120.4 . . ? C72 C73 C74 119.6(9) . . ? C72 C73 H73 120.2 . . ? C74 C73 H73 120.2 . . ? C75 C74 C73 119.0(9) . . ? C75 C74 H74 120.5 . . ? C73 C74 H74 120.5 . . ? N71 C75 C74 120.5(8) . . ? N71 C75 C76 116.3(7) . . ? C74 C75 C76 123.1(8) . . ? N72 C76 C75 114.8(8) . . ? N72 C76 C77 124.3(7) . . ? C75 C76 C77 120.9(7) . . ? N81 C81 C82 123.7(8) . . ? N81 C81 H81 118.2 . . ? C82 C81 H81 118.2 . . ? C83 C82 C81 118.5(9) . . ? C83 C82 H82 120.7 . . ? C81 C82 H82 120.7 . . ? C82 C83 C84 118.8(9) . . ? C82 C83 H83 120.6 . . ? C84 C83 H83 120.6 . . ? C85 C84 C83 120.2(9) . . ? C85 C84 H84 119.9 . . ? C83 C84 H84 119.9 . . ? C84 C85 N81 121.6(8) . . ? C84 C85 C86 123.0(8) . . ? N81 C85 C86 115.4(7) . . ? N82 C86 C87 125.0(8) . . ? N82 C86 C85 114.0(7) . . ? C87 C86 C85 121.0(8) . . ? C86 C87 H87A 109.5 . . ? C86 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C86 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? N91 C91 C92 123.4(9) . . ? N91 C91 H91 118.3 . . ? C92 C91 H91 118.3 . . ? C91 C92 C93 116.5(9) . . ? C91 C92 H92 121.8 . . ? C93 C92 H92 121.8 . . ? C94 C93 C92 120.9(9) . . ? C94 C93 H93 119.5 . . ? C92 C93 H93 119.5 . . ? C93 C94 C95 119.7(10) . . ? C93 C94 H94 120.1 . . ? C95 C94 H94 120.1 . . ? N91 C95 C94 121.6(9) . . ? N91 C95 C96 118.1(8) . . ? C94 C95 C96 120.3(9) . . ? N92 C96 C95 114.6(8) . . ? N92 C96 C97 123.5(9) . . ? C95 C96 C97 121.9(8) . . ? C96 C97 H97A 109.5 . . ? C96 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C96 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? N101 C101 C102 126.1(9) . . ? N101 C101 H101 117.0 . . ? C102 C101 H101 117.0 . . ? C101 C102 C103 117.4(9) . . ? C101 C102 H102 121.3 . . ? C103 C102 H102 121.3 . . ? C104 C103 C102 119.4(9) . . ? C104 C103 H103 120.3 . . ? C102 C103 H103 120.3 . . ? C103 C104 C105 120.0(9) . . ? C103 C104 H104 120.0 . . ? C105 C104 H104 120.0 . . ? N101 C105 C104 121.1(9) . . ? N101 C105 C106 116.8(8) . . ? C104 C105 C106 122.0(9) . . ? N102 C106 C105 114.8(8) . . ? N102 C106 C107 124.7(9) . . ? C105 C106 C107 120.5(8) . . ? C106 C107 H10A 109.5 . . ? C106 C107 H10B 109.5 . . ? H10A C107 H10B 109.5 . . ? C106 C107 H10C 109.5 . . ? H10A C107 H10C 109.5 . . ? H10B C107 H10C 109.5 . . ? C115 N111 C111 116.1(8) . . ? C115 N111 Dy2 120.3(5) . . ? C111 N111 Dy2 122.8(6) . . ? C116 N112 O111 112.8(7) . . ? C116 N112 Dy2 127.4(6) . . ? O111 N112 Dy2 119.5(4) . . ? N112 O111 H96O 99.2 . . ? C112 C111 N111 123.9(10) . . ? C112 C111 H111 118.0 . . ? N111 C111 H111 118.0 . . ? C111 C112 C113 119.1(10) . . ? C111 C112 H112 120.5 . . ? C113 C112 H112 120.5 . . ? C112 C113 C114 117.8(10) . . ? C112 C113 H113 121.1 . . ? C114 C113 H113 121.1 . . ? C115 C114 C113 120.3(10) . . ? C115 C114 H114 119.9 . . ? C113 C114 H114 119.9 . . ? N111 C115 C114 122.8(9) . . ? N111 C115 C116 116.8(8) . . ? C114 C115 C116 120.4(9) . . ? N112 C116 C117 125.7(8) . . ? N112 C116 C115 113.4(8) . . ? C117 C116 C115 120.9(8) . . ? C116 C117 H11A 109.5 . . ? C116 C117 H11B 109.5 . . ? H11A C117 H11B 109.5 . . ? C116 C117 H11C 109.5 . . ? H11A C117 H11C 109.5 . . ? H11B C117 H11C 109.5 . . ? O121 Cl1 O122 108.8(5) . . ? O121 Cl1 O124 108.8(5) . . ? O122 Cl1 O124 107.4(6) . . ? O121 Cl1 O123 111.5(5) . . ? O122 Cl1 O123 109.7(5) . . ? O124 Cl1 O123 110.4(6) . . ? O32A Cl2 O134 155.3(19) . . ? O32A Cl2 O133 64.2(18) . . ? O134 Cl2 O133 118.7(11) . . ? O32A Cl2 O131 104.5(16) . . ? O134 Cl2 O131 97.5(12) . . ? O133 Cl2 O131 109.3(8) . . ? O32A Cl2 O132 53.7(18) . . ? O134 Cl2 O132 107.7(11) . . ? O133 Cl2 O132 111.5(9) . . ? O131 Cl2 O132 111.2(9) . . ? O32A Cl2 O34A 107(3) . . ? O134 Cl2 O34A 49.6(19) . . ? O133 Cl2 O34A 121.6(19) . . ? O131 Cl2 O34A 127.9(19) . . ? O132 Cl2 O34A 61(2) . . ? O32A Cl2 O33A 112(2) . . ? O134 Cl2 O33A 70.0(16) . . ? O133 Cl2 O33A 49.4(14) . . ? O131 Cl2 O33A 109.3(15) . . ? O132 Cl2 O33A 139.3(15) . . ? O34A Cl2 O33A 96(2) . . ? O32A O132 Cl2 58.0(17) . . ? O32A O132 O34A 111(3) . . ? Cl2 O132 O34A 61(2) . . ? O33A O133 Cl2 74.6(19) . . ? O33A O133 O32A 128(3) . . ? Cl2 O133 O32A 55.4(15) . . ? O34A O134 Cl2 73(3) . . ? O34A O134 O33A 105(3) . . ? Cl2 O134 O33A 63.2(15) . . ? O132 O32A Cl2 68(2) . . ? O132 O32A O133 121(3) . . ? Cl2 O32A O133 60.4(16) . . ? O133 O33A Cl2 55.9(16) . . ? O133 O33A O134 102(3) . . ? Cl2 O33A O134 46.7(12) . . ? O134 O34A O132 112(4) . . ? O134 O34A Cl2 57(2) . . ? O132 O34A Cl2 57.6(19) . . ? O142 Cl3 O141 110.9(5) . . ? O142 Cl3 O143 108.0(5) . . ? O141 Cl3 O143 108.5(4) . . ? O142 Cl3 O144 109.2(4) . . ? O141 Cl3 O144 110.6(4) . . ? O143 Cl3 O144 109.6(5) . . ? O154 Cl4 O153 109.8(8) . . ? O154 Cl4 O151 109.7(6) . . ? O153 Cl4 O151 111.1(6) . . ? O154 Cl4 O152 108.9(6) . . ? O153 Cl4 O152 108.2(5) . . ? O151 Cl4 O152 109.1(5) . . ? O1W O2M C2M 53.3 . . ? O1W C2M O2M 50.6 . . ? O3M C3M O4M 106.4 . . ? C4M O4M C3M 110.5 . . ? O3W C4M O4M 94.9 . . ? O2M O1W C2M 76.1 . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 1.950 _refine_diff_density_min -3.324 _refine_diff_density_rms 0.136 # start Validation Reply Form _vrf_PLAT029_I ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.939 RESPONSE: The crystals showed poor diffraction ability, especially at higher two-theta values. Repeating efforts to improve the quality of the crystals were unsuccessful. However, the compound is isostructural to the NiCe compound (also reported in the same article) thus we decided to proceed with the data collection in order to establish the gross structure of the complex. Full data to 143 deg (for Cu-radiation) were collected but only those to 130 deg were used in the refinement. ; data_peen30a1 _database_code_depnum_ccdc_archive 'CCDC 896965' #TrackingRef 'Dalton Perlepes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H56 Cl La N18 Ni2 O30' _chemical_formula_weight 1608.85 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' Cl Cl 0.3639 0.7018 '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' La La -1.4094 9.0376 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 13.4798(2) _cell_length_b 13.4798(5) _cell_length_c 30.0050(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4721.62(19) _cell_formula_units_Z 3 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 16653 _cell_measurement_theta_min 6.57 _cell_measurement_theta_max 71.86 _exptl_crystal_description parallelepiped _exptl_crystal_colour orange _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.697 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 7.134 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.531 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'CrystalClear, Rigaku MSC, 2005' _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 15636 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 7.02 _diffrn_reflns_theta_max 64.98 _reflns_number_total 1776 _reflns_number_gt 1776 _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^)+(0.0427P)^2^+13.6585P] 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 1776 _refine_ls_number_parameters 179 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0281 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0730 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.105 _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 Ni Ni 0.0000 0.0000 0.29932(2) 0.0119(2) Uani 1 3 d S . . O1 O -0.20525(17) -0.12344(19) 0.36663(7) 0.0224(5) Uani 1 1 d . . . N1 N -0.14133(19) -0.13164(19) 0.33218(7) 0.0145(5) Uani 1 1 d . . . N2 N -0.0323(2) -0.1442(2) 0.26278(8) 0.0167(5) Uani 1 1 d . . . C1 C -0.2998(3) -0.3302(3) 0.32972(11) 0.0272(7) Uani 1 1 d . . . H1A H -0.3513 -0.3656 0.3043 0.038 Uiso 1 1 calc R . . H1B H -0.3358 -0.3033 0.3513 0.038 Uiso 1 1 calc R . . H1C H -0.2848 -0.3867 0.3440 0.038 Uiso 1 1 calc R . . C2 C -0.1898(2) -0.2313(2) 0.31392(9) 0.0158(6) Uani 1 1 d . . . C3 C -0.1279(2) -0.2419(2) 0.27527(9) 0.0167(6) Uani 1 1 d . . . C4 C -0.1634(3) -0.3440(3) 0.25297(11) 0.0251(7) Uani 1 1 d . . . C5 C -0.0984(3) -0.3470(3) 0.21777(12) 0.0321(8) Uani 1 1 d . . . C6 C -0.0010(3) -0.2487(3) 0.20567(12) 0.0327(8) Uani 1 1 d . . . C7 C 0.0294(3) -0.1491(3) 0.22885(11) 0.0262(7) Uani 1 1 d . . . La La 0.0000 0.0000 0.5000 0.01086(14) Uani 1 6 d S . . O2 O -0.07604(18) 0.14892(17) 0.48288(7) 0.0240(5) Uani 1 1 d . . . O3 O -0.1789(2) 0.1367(2) 0.42528(9) 0.0389(6) Uani 1 1 d . . . O4 O -0.10674(18) 0.02478(18) 0.43204(6) 0.0226(5) Uani 1 1 d . . . N3 N -0.1222(2) 0.1056(2) 0.44637(8) 0.0201(5) Uani 1 1 d . . . Cl Cl 0.6667 0.3333 0.3333 0.0613(7) Uani 1 6 d SD . . O51 O 0.6317(14) 0.2336(11) 0.3502(6) 0.052(2) Uani 0.17 1 d PD A -1 O52 O 0.5931(15) 0.3593(19) 0.3045(7) 0.052(2) Uani 0.17 1 d PD A -1 O53 O 0.7763(17) 0.379(3) 0.3048(9) 0.052(2) Uani 0.17 1 d PD B -1 O54 O 0.725(2) 0.437(2) 0.3653(11) 0.052(2) Uani 0.17 1 d PD C -1 C1M C 0.0000 0.0000 0.1279(5) 0.115(4) Uiso 1 3 d S . . O1N O 0.0516(7) 0.0894(7) 0.1264(3) 0.048(2) Uiso 0.33 1 d P . . H1O H -0.164(3) -0.064(3) 0.3807(11) 0.018(8) Uiso 1 1 d . . . H4 H -0.223(3) -0.409(3) 0.2617(12) 0.028(10) Uiso 1 1 d . . . H5 H -0.114(3) -0.409(4) 0.2033(13) 0.042(11) Uiso 1 1 d . . . H6 H 0.049(3) -0.246(3) 0.1808(13) 0.034(10) Uiso 1 1 d . . . H7 H 0.099(3) -0.078(3) 0.2207(12) 0.028(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0111(3) 0.0111(3) 0.0136(4) 0.000 0.000 0.00556(13) O1 0.0152(11) 0.0265(12) 0.0187(10) -0.0070(9) 0.0038(8) 0.0055(9) N1 0.0127(11) 0.0168(12) 0.0136(11) -0.0003(9) -0.0006(9) 0.0071(10) N2 0.0167(12) 0.0175(12) 0.0189(12) -0.0034(9) -0.0009(9) 0.0107(10) C1 0.0229(16) 0.0190(16) 0.0296(17) 0.0006(12) 0.0021(13) 0.0029(13) C2 0.0138(14) 0.0152(14) 0.0173(14) 0.0021(11) -0.0041(11) 0.0065(12) C3 0.0178(14) 0.0158(14) 0.0192(14) -0.0013(11) -0.0071(11) 0.0105(12) C4 0.0295(18) 0.0160(16) 0.0293(17) -0.0042(12) -0.0079(13) 0.0110(15) C5 0.046(2) 0.0273(18) 0.0340(18) -0.0142(15) -0.0095(15) 0.0268(17) C6 0.037(2) 0.038(2) 0.0318(18) -0.0104(15) 0.0016(15) 0.0252(17) C7 0.0234(17) 0.0286(17) 0.0272(16) -0.0058(13) 0.0042(13) 0.0135(15) La 0.01269(16) 0.01269(16) 0.00719(19) 0.000 0.000 0.00635(8) O2 0.0280(11) 0.0195(11) 0.0222(11) -0.0048(8) -0.0094(9) 0.0102(9) O3 0.0440(15) 0.0425(15) 0.0427(14) -0.0031(11) -0.0211(11) 0.0310(13) O4 0.0296(12) 0.0277(11) 0.0167(10) -0.0032(8) -0.0037(8) 0.0190(10) N3 0.0192(13) 0.0188(13) 0.0215(13) 0.0028(10) -0.0021(10) 0.0090(11) Cl 0.0690(11) 0.0690(11) 0.0460(14) 0.000 0.000 0.0345(6) O51 0.020(5) 0.052(7) 0.073(5) -0.026(6) -0.020(5) 0.011(5) O52 0.020(5) 0.052(7) 0.073(5) -0.026(6) -0.020(5) 0.011(5) O53 0.020(5) 0.052(7) 0.073(5) -0.026(6) -0.020(5) 0.011(5) O54 0.020(5) 0.052(7) 0.073(5) -0.026(6) -0.020(5) 0.011(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni N2 2.079(2) . ? Ni N2 2.079(2) 2 ? Ni N2 2.079(2) 3 ? Ni N1 2.090(2) 3 ? Ni N1 2.090(2) 2 ? Ni N1 2.090(2) . ? O1 N1 1.385(3) . ? O1 H1O 0.82(4) . ? N1 C2 1.286(4) . ? N2 C7 1.337(4) . ? N2 C3 1.356(4) . ? C1 C2 1.492(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.477(4) . ? C3 C4 1.383(4) . ? C4 C5 1.386(5) . ? C4 H4 0.88(4) . ? C5 C6 1.369(5) . ? C5 H5 0.88(4) . ? C6 C7 1.380(5) . ? C6 H6 1.00(4) . ? C7 H7 0.98(4) . ? La O4 2.6116(19) 11_556 ? La O4 2.6116(19) . ? La O4 2.6116(19) 2 ? La O4 2.612(2) 3 ? La O4 2.6116(19) 10_556 ? La O4 2.6116(19) 12_556 ? La O2 2.721(2) 11_556 ? La O2 2.721(2) 3 ? La O2 2.721(2) 2 ? La O2 2.721(2) 10_556 ? La O2 2.721(2) 12_556 ? La O2 2.721(2) . ? O2 N3 1.251(3) . ? O3 N3 1.216(3) . ? O4 N3 1.282(3) . ? Cl O51 1.286(14) 16_655 ? Cl O51 1.286(14) 2_655 ? Cl O51 1.286(14) . ? Cl O51 1.286(14) 17 ? Cl O51 1.286(14) 3_665 ? Cl O51 1.286(14) 18_545 ? Cl O52 1.484(15) 17 ? Cl O52 1.484(15) 18_545 ? Cl O52 1.484(15) 2_655 ? Cl O52 1.484(15) 3_665 ? Cl O52 1.484(15) . ? Cl O52 1.484(15) 16_655 ? C1M O1N 1.049(8) 2 ? C1M O1N 1.049(8) . ? C1M O1N 1.049(8) 3 ? O1N O1N 1.815(14) 2 ? O1N O1N 1.815(14) 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 N2 Ni N2 94.75(9) . 2 ? N2 Ni N2 94.75(9) . 3 ? N2 Ni N2 94.75(9) 2 3 ? N2 Ni N1 171.53(9) . 3 ? N2 Ni N1 88.73(9) 2 3 ? N2 Ni N1 77.25(9) 3 3 ? N2 Ni N1 88.73(9) . 2 ? N2 Ni N1 77.25(9) 2 2 ? N2 Ni N1 171.53(9) 3 2 ? N1 Ni N1 99.57(8) 3 2 ? N2 Ni N1 77.25(9) . . ? N2 Ni N1 171.53(9) 2 . ? N2 Ni N1 88.73(9) 3 . ? N1 Ni N1 99.57(8) 3 . ? N1 Ni N1 99.57(8) 2 . ? N1 O1 H1O 108(2) . . ? C2 N1 O1 113.0(2) . . ? C2 N1 Ni 117.20(18) . . ? O1 N1 Ni 128.57(17) . . ? C7 N2 C3 118.3(3) . . ? C7 N2 Ni 127.1(2) . . ? C3 N2 Ni 114.56(18) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 114.8(2) . . ? N1 C2 C1 123.8(3) . . ? C3 C2 C1 121.3(3) . . ? N2 C3 C4 121.4(3) . . ? N2 C3 C2 115.5(2) . . ? C4 C3 C2 123.1(3) . . ? C3 C4 C5 119.2(3) . . ? C3 C4 H4 122(2) . . ? C5 C4 H4 119(2) . . ? C6 C5 C4 119.3(3) . . ? C6 C5 H5 117(3) . . ? C4 C5 H5 124(3) . . ? C5 C6 C7 118.8(3) . . ? C5 C6 H6 123(2) . . ? C7 C6 H6 118(2) . . ? N2 C7 C6 122.9(3) . . ? N2 C7 H7 117(2) . . ? C6 C7 H7 120(2) . . ? O4 La O4 114.48(7) 11_556 . ? O4 La O4 180.0 11_556 2 ? O4 La O4 65.52(7) . 2 ? O4 La O4 114.48(7) 11_556 3 ? O4 La O4 65.52(7) . 3 ? O4 La O4 65.52(7) 2 3 ? O4 La O4 65.52(7) 11_556 10_556 ? O4 La O4 180.00(5) . 10_556 ? O4 La O4 114.48(7) 2 10_556 ? O4 La O4 114.48(7) 3 10_556 ? O4 La O4 65.52(7) 11_556 12_556 ? O4 La O4 114.48(7) . 12_556 ? O4 La O4 114.48(7) 2 12_556 ? O4 La O4 180.0 3 12_556 ? O4 La O4 65.52(7) 10_556 12_556 ? O4 La O2 47.41(6) 11_556 11_556 ? O4 La O2 98.71(7) . 11_556 ? O4 La O2 132.59(6) 2 11_556 ? O4 La O2 67.29(6) 3 11_556 ? O4 La O2 81.29(7) 10_556 11_556 ? O4 La O2 112.71(6) 12_556 11_556 ? O4 La O2 98.71(7) 11_556 3 ? O4 La O2 112.71(6) . 3 ? O4 La O2 81.29(7) 2 3 ? O4 La O2 47.41(6) 3 3 ? O4 La O2 67.29(6) 10_556 3 ? O4 La O2 132.59(6) 12_556 3 ? O2 La O2 63.48(3) 11_556 3 ? O4 La O2 132.59(6) 11_556 2 ? O4 La O2 81.29(7) . 2 ? O4 La O2 47.41(6) 2 2 ? O4 La O2 112.71(6) 3 2 ? O4 La O2 98.71(7) 10_556 2 ? O4 La O2 67.29(6) 12_556 2 ? O2 La O2 180.0 11_556 2 ? O2 La O2 116.52(3) 3 2 ? O4 La O2 112.71(6) 11_556 10_556 ? O4 La O2 132.59(6) . 10_556 ? O4 La O2 67.29(6) 2 10_556 ? O4 La O2 98.71(7) 3 10_556 ? O4 La O2 47.41(6) 10_556 10_556 ? O4 La O2 81.29(7) 12_556 10_556 ? O2 La O2 116.52(3) 11_556 10_556 ? O2 La O2 63.48(3) 3 10_556 ? O2 La O2 63.48(3) 2 10_556 ? O4 La O2 81.29(7) 11_556 12_556 ? O4 La O2 67.29(6) . 12_556 ? O4 La O2 98.71(7) 2 12_556 ? O4 La O2 132.59(6) 3 12_556 ? O4 La O2 112.71(6) 10_556 12_556 ? O4 La O2 47.41(6) 12_556 12_556 ? O2 La O2 116.52(3) 11_556 12_556 ? O2 La O2 180.0 3 12_556 ? O2 La O2 63.48(3) 2 12_556 ? O2 La O2 116.52(3) 10_556 12_556 ? O4 La O2 67.29(6) 11_556 . ? O4 La O2 47.41(6) . . ? O4 La O2 112.71(6) 2 . ? O4 La O2 81.29(7) 3 . ? O4 La O2 132.59(6) 10_556 . ? O4 La O2 98.71(7) 12_556 . ? O2 La O2 63.48(3) 11_556 . ? O2 La O2 116.52(3) 3 . ? O2 La O2 116.52(3) 2 . ? O2 La O2 180.00(9) 10_556 . ? O2 La O2 63.48(3) 12_556 . ? N3 O2 La 95.97(15) . . ? N3 O4 La 100.43(15) . . ? O3 N3 O2 123.1(3) . . ? O3 N3 O4 121.0(2) . . ? O2 N3 O4 115.9(2) . . ? O51 Cl O51 74.5(9) 16_655 2_655 ? O51 Cl O51 179.996(4) 16_655 . ? O51 Cl O51 105.5(9) 2_655 . ? O51 Cl O51 105.5(9) 16_655 17 ? O51 Cl O51 179.996(4) 2_655 17 ? O51 Cl O51 74.5(9) . 17 ? O51 Cl O51 74.5(9) 16_655 3_665 ? O51 Cl O51 105.5(9) 2_655 3_665 ? O51 Cl O51 105.5(9) . 3_665 ? O51 Cl O51 74.5(9) 17 3_665 ? O51 Cl O51 105.4(9) 16_655 18_545 ? O51 Cl O51 74.5(9) 2_655 18_545 ? O51 Cl O51 74.5(9) . 18_545 ? O51 Cl O51 105.4(9) 17 18_545 ? O51 Cl O51 179.998(8) 3_665 18_545 ? O51 Cl O52 59.1(11) 16_655 17 ? O51 Cl O52 57.5(9) 2_655 17 ? O51 Cl O52 120.9(11) . 17 ? O51 Cl O52 122.5(9) 17 17 ? O51 Cl O52 48.3(10) 3_665 17 ? O51 Cl O52 131.7(10) 18_545 17 ? O51 Cl O52 131.7(10) 16_655 18_545 ? O51 Cl O52 120.9(11) 2_655 18_545 ? O51 Cl O52 48.3(10) . 18_545 ? O51 Cl O52 59.1(11) 17 18_545 ? O51 Cl O52 57.5(9) 3_665 18_545 ? O51 Cl O52 122.5(9) 18_545 18_545 ? O52 Cl O52 89.5(12) 17 18_545 ? O51 Cl O52 120.9(11) 16_655 2_655 ? O51 Cl O52 122.5(9) 2_655 2_655 ? O51 Cl O52 59.1(11) . 2_655 ? O51 Cl O52 57.5(9) 17 2_655 ? O51 Cl O52 131.7(10) 3_665 2_655 ? O51 Cl O52 48.3(10) 18_545 2_655 ? O52 Cl O52 179.998(5) 17 2_655 ? O52 Cl O52 90.5(12) 18_545 2_655 ? O51 Cl O52 48.3(10) 16_655 3_665 ? O51 Cl O52 59.1(11) 2_655 3_665 ? O51 Cl O52 131.7(10) . 3_665 ? O51 Cl O52 120.9(11) 17 3_665 ? O51 Cl O52 122.5(9) 3_665 3_665 ? O51 Cl O52 57.5(9) 18_545 3_665 ? O52 Cl O52 90.5(12) 17 3_665 ? O52 Cl O52 179.997(5) 18_545 3_665 ? O52 Cl O52 89.5(12) 2_655 3_665 ? O51 Cl O52 57.5(9) 16_655 . ? O51 Cl O52 131.7(10) 2_655 . ? O51 Cl O52 122.5(10) . . ? O51 Cl O52 48.3(10) 17 . ? O51 Cl O52 59.1(11) 3_665 . ? O51 Cl O52 120.9(11) 18_545 . ? O52 Cl O52 90.5(12) 17 . ? O52 Cl O52 90.5(12) 18_545 . ? O52 Cl O52 89.5(12) 2_655 . ? O52 Cl O52 89.5(12) 3_665 . ? O51 Cl O52 122.5(10) 16_655 16_655 ? O51 Cl O52 48.3(10) 2_655 16_655 ? O51 Cl O52 57.5(9) . 16_655 ? O51 Cl O52 131.7(10) 17 16_655 ? O51 Cl O52 120.9(11) 3_665 16_655 ? O51 Cl O52 59.1(11) 18_545 16_655 ? O52 Cl O52 89.5(12) 17 16_655 ? O52 Cl O52 89.5(12) 18_545 16_655 ? O52 Cl O52 90.5(12) 2_655 16_655 ? O52 Cl O52 90.5(12) 3_665 16_655 ? O52 Cl O52 179.996(8) . 16_655 ? O1N C1M O1N 119.81(17) 2 . ? O1N C1M O1N 119.81(17) 2 3 ? O1N C1M O1N 119.81(17) . 3 ? C1M O1N O1N 30.10(9) . 2 ? C1M O1N O1N 30.10(8) . 3 ? O1N O1N O1N 60.000(1) 2 3 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 64.98 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.680 _refine_diff_density_min -0.973 _refine_diff_density_rms 0.095 #===END