data_Yan # SUBMISSION DETAILS _publ_contact_author_name 'Prof. Chun-Hua Yan' _publ_contact_author_address ; State Key Lab of Rare Earth Materials Chemistry and Applications & PKU-HKU Joint Lab on Rare Earth Materials and Bioinorganic Chemistry, College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, China ; _publ_contact_author_email chyan@chem.pku.edu.cn _publ_contact_author_phone '86-(10)-62754179' _publ_contact_author_fax '86-(10)-62754179' _publ_requested_journal 'Inorg. Chem.' _publ_section_title ; Lanthanide-transition heterometallic extended structures with novel orthogonal metalloligand as building blocks ; ## Crystallographic Data of Complex 1 data_Ni _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H63 Cl2 N19 Ni2 O17' _chemical_formula_weight 1594.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.84600(10) _cell_length_b 23.6352(2) _cell_length_c 20.8378(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.4531(4) _cell_angle_gamma 90.00 _cell_volume 7047.41(10) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 89052 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description 'block' _exptl_crystal_colour 'brownish red' _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3296 _exptl_absorpt_coefficient_mu 0.694 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 0.941 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 101437 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16049 _reflns_number_gt 10889 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16049 _refine_ls_number_parameters 801 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1411 _refine_ls_R_factor_gt 0.1034 _refine_ls_wR_factor_ref 0.3556 _refine_ls_wR_factor_gt 0.3262 _refine_ls_goodness_of_fit_ref 1.375 _refine_ls_restrained_S_all 18268.521 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.1(6) 0.4(3) 0.5(4) 0(3) Uani 1 1 d . . . Ni2 Ni -0.4(6) 0.6(4) 0.0(4) 0(3) Uani 1 1 d . . . C1 C 0(5) 0(3) 1(4) 0(17) Uani 1 1 d . . . H1A H -0.0856 0.3301 0.4721 0.047 Uiso 1 1 calc R . . C2 C 0(6) 0(4) 1(5) 0(20) Uani 1 1 d . . . H2A H -0.1800 0.3312 0.5436 0.059 Uiso 1 1 calc R . . C3 C 0(6) 0(3) 1(5) 0(20) Uani 1 1 d . . . H3A H -0.1540 0.3984 0.6279 0.060 Uiso 1 1 calc R . . C4 C 0(5) 0(3) 1(4) 0(17) Uani 1 1 d . . . H4A H -0.0329 0.4646 0.6369 0.050 Uiso 1 1 calc R . . C5 C 0(5) 0(3) 1(3) 0(14) Uani 1 1 d . . . C6 C 0(5) 0(3) 1(3) 0(15) Uani 1 1 d . . . H6A H 0.1039 0.5014 0.5927 0.042 Uiso 1 1 calc R . . C7 C 0(5) 0(3) 0(3) 0(16) Uani 1 1 d . . . C8 C 0(5) 1(4) 0(4) 0(18) Uani 1 1 d . . . C9 C 0(6) 1(4) 0(4) 0(20) Uani 1 1 d . . . H9A H 0.3224 0.5761 0.5182 0.059 Uiso 1 1 calc R . . C10 C 0(7) 1(4) 0(5) 0(26) Uani 1 1 d . . . H10A H 0.4475 0.6255 0.5011 0.076 Uiso 1 1 calc R . . C11 C 0(7) 1(5) 0(5) 0(29) Uani 1 1 d . . . H11A H 0.4887 0.5067 0.3799 0.081 Uiso 1 1 calc R . . C12 C 0(6) 0(4) 0(4) 0(21) Uani 1 1 d . . . H12A H 0.3644 0.4554 0.3961 0.064 Uiso 1 1 calc R . . C13 C 0(5) 0(3) 1(4) 0(18) Uani 1 1 d . . . H13A H 0.2589 0.3738 0.5898 0.051 Uiso 1 1 calc R . . C14 C 0(6) 0(4) 1(4) 0(20) Uani 1 1 d . . . H14A H 0.3326 0.2952 0.6456 0.058 Uiso 1 1 calc R . . C15 C 0(6) 0(3) 1(4) 0(19) Uani 1 1 d . . . H15A H 0.2893 0.2070 0.6044 0.054 Uiso 1 1 calc R . . C16 C 0(5) 0(3) 1(4) 0(16) Uani 1 1 d . . . H16A H 0.1776 0.1973 0.5038 0.045 Uiso 1 1 calc R . . C17 C 0(5) 0(3) 0(3) 0(15) Uani 1 1 d . . . C18 C 0(5) 0(3) 0(3) 0(15) Uani 1 1 d . . . H18A H 0.0657 0.2469 0.4001 0.038 Uiso 1 1 calc R . . C19 C 0(5) 0(3) 0(3) 0(14) Uani 1 1 d . . . C20 C 0(5) 0(3) 0(3) 0(14) Uani 1 1 d . . . C21 C 0(6) 0(3) 0(4) 0(19) Uani 1 1 d . . . H21A H -0.0797 0.3285 0.2159 0.054 Uiso 1 1 calc R . . C22 C 0(5) 0(3) 0(4) 0(17) Uani 1 1 d . . . H22A H -0.1736 0.3506 0.1150 0.047 Uiso 1 1 calc R . . C23 C 0(6) 0(3) 0(4) 0(18) Uani 1 1 d . . . H23A H -0.2125 0.5042 0.1770 0.052 Uiso 1 1 calc R . . C24 C 0(5) 0(3) 0(4) 0(16) Uani 1 1 d . . . H24A H -0.1119 0.4849 0.2788 0.046 Uiso 1 1 calc R . . C25 C -1(5) 1(4) 0(4) 0(19) Uani 1 1 d . . . H25A H -0.6234 0.6698 0.0083 0.055 Uiso 1 1 calc R . . C26 C -1(6) 1(4) 0(5) 0(24) Uani 1 1 d . . . H26A H -0.7143 0.6417 0.0762 0.069 Uiso 1 1 calc R . . C27 C -1(5) 1(4) 0(5) 0(21) Uani 1 1 d . . . H27A H -0.6781 0.5606 0.1399 0.060 Uiso 1 1 calc R . . C28 C -1(5) 1(3) 0(4) 0(17) Uani 1 1 d . . . H28A H -0.5482 0.5071 0.1325 0.050 Uiso 1 1 calc R . . C29 C -1(5) 1(3) 0(3) 0(15) Uani 1 1 d . . . C30 C 0(4) 1(3) 0(3) 0(14) Uani 1 1 d . . . H30A H -0.4056 0.4978 0.0834 0.035 Uiso 1 1 calc R . . C31 C 0(5) 1(3) 0(3) 0(15) Uani 1 1 d . . . C32 C 0(5) 1(3) 0(4) 0(15) Uani 1 1 d . . . C33 C 0(5) 0(3) 0(4) 0(17) Uani 1 1 d . . . H33A H -0.1782 0.4674 -0.0153 0.048 Uiso 1 1 calc R . . C34 C 0(6) 0(4) 0(4) 0(20) Uani 1 1 d . . . H34A H -0.0565 0.4399 -0.0564 0.060 Uiso 1 1 calc R . . C35 C 0(6) 1(4) 0(5) 0(23) Uani 1 1 d . . . H35A H -0.0311 0.5951 -0.1206 0.067 Uiso 1 1 calc R . . C36 C 0(5) 1(4) 0(4) 0(18) Uani 1 1 d . . . H36A H -0.1607 0.6241 -0.0862 0.053 Uiso 1 1 calc R . . C37 C 0(5) 1(3) 0(4) 0(17) Uani 1 1 d . . . H37A H -0.2926 0.6580 0.1238 0.050 Uiso 1 1 calc R . . C38 C 0(6) 1(4) 0(4) 0(20) Uani 1 1 d . . . H38A H -0.2325 0.7373 0.1799 0.058 Uiso 1 1 calc R . . C39 C 0(5) 1(3) 0(4) 0(18) Uani 1 1 d . . . H39A H -0.2764 0.8258 0.1322 0.052 Uiso 1 1 calc R . . C40 C 0(5) 1(3) 0(4) 0(17) Uani 1 1 d . . . H40A H -0.3841 0.8309 0.0304 0.048 Uiso 1 1 calc R . . C41 C 0(5) 1(3) 0(4) 0(16) Uani 1 1 d . . . C42 C 0(5) 1(3) 0(4) 0(16) Uani 1 1 d . . . H42A H -0.4914 0.7771 -0.0717 0.045 Uiso 1 1 calc R . . C43 C -1(5) 1(3) 0(3) 0(15) Uani 1 1 d . . . C44 C -1(5) 1(3) 0(3) 0(15) Uani 1 1 d . . . C45 C -1(5) 1(3) 0(4) 0(18) Uani 1 1 d . . . H45A H -0.6785 0.6953 -0.2386 0.051 Uiso 1 1 calc R . . C46 C -1(5) 1(3) 0(4) 0(17) Uani 1 1 d . . . H46A H -0.7673 0.6723 -0.3436 0.049 Uiso 1 1 calc R . . C47 C -1(6) 1(3) 0(4) 0(19) Uani 1 1 d . . . H47A H -0.6610 0.5186 -0.3262 0.054 Uiso 1 1 calc R . . C48 C -1(6) 1(3) 0(4) 0(18) Uani 1 1 d . . . H48A H -0.5817 0.5375 -0.2164 0.053 Uiso 1 1 calc R . . C49 C 0(10) 0(7) 0(7) 0(37) Uani 1 1 d . . . C50 C 0(9) 0(7) 0(9) 0(58) Uani 1 1 d . . . H50A H 0.1072 0.1825 0.1778 0.185 Uiso 1 1 calc R . . H50B H 0.0423 0.2142 0.1167 0.185 Uiso 1 1 calc R . . H50C H 0.0116 0.2077 0.1827 0.185 Uiso 1 1 calc R . . N1 N 0(4) 0(2) 1(3) 0(12) Uani 1 1 d . . . N2 N 0(4) 0(2) 1(3) 0(12) Uani 1 1 d . . . N3 N 0(4) 0(2) 1(3) 0(13) Uani 1 1 d . . . H3B H 0.2280 0.5218 0.5408 0.041 Uiso 1 1 calc R . . N4 N 0(5) 1(4) 0(5) 0(23) Uani 1 1 d . . . N5 N 0(4) 0(2) 1(3) 0(13) Uani 1 1 d . . . N6 N 0(4) 0(2) 0(3) 0(12) Uani 1 1 d . . . N7 N 0(4) 0(2) 0(3) 0(13) Uani 1 1 d . . . N8 N 0(4) 0(2) 0(3) 0(12) Uani 1 1 d . . . N9 N -1(4) 1(2) 0(3) 0(13) Uani 1 1 d . . . N10 N 0(4) 1(2) 0(3) 0(12) Uani 1 1 d . . . N11 N 0(4) 1(2) 0(3) 0(12) Uani 1 1 d . . . H11B H -0.2734 0.5063 0.0326 0.036 Uiso 1 1 calc R . . N12 N 0(4) 1(3) 0(3) 0(17) Uani 1 1 d . . . N13 N 0(4) 1(2) 0(3) 0(13) Uani 1 1 d . . . N14 N 0(4) 1(2) 0(3) 0(13) Uani 1 1 d . . . N15 N -1(4) 1(2) 0(3) 0(14) Uani 1 1 d . . . N16 N -1(4) 1(3) 0(3) 0(13) Uani 1 1 d . . . N17 N 0(10) 0(7) 0(6) 0(45) Uani 1 1 d . . . O1 O 0(3) 0(2) 0(2) 0(11) Uani 1 1 d . . . O2 O 1(6) 1(4) 0(5) 0(29) Uani 1 1 d . . . O3 O 0(3) 0.4(19) 0(2) 0(11) Uani 1 1 d . . . O4 O 0(4) 0(2) 0(2) 0(12) Uani 1 1 d . . . O5 O 0(3) 1(2) 0(3) 0(11) Uani 1 1 d . . . O6 O 0(4) 0(4) 0(4) 0(20) Uani 1 1 d . . . O7 O -1(3) 1(2) 0(2) 0(11) Uani 1 1 d . . . O8 O -1(4) 1(2) 0(3) 0(13) Uani 1 1 d . . . Cl1 Cl 0(4) 0.1(11) 0.2(13) 0(20) Uani 1 1 d D . . O9 O 0(6) 0(4) 0(5) 0(25) Uiso 1 1 d D . . O10 O 0(6) 0(4) 0(4) 0(23) Uiso 1 1 d D . . O11 O 0(5) 0(3) 0(4) 0(19) Uiso 1 1 d D . . O12 O 0(12) 0(8) 0(9) 0(64) Uiso 1 1 d D . . Cl2 Cl -0.1(18) 0.2(11) 0.5(14) 0(8) Uani 1 1 d D . . O16 O 0(6) 0(4) 0(4) 0(24) Uiso 1 1 d D . . O15 O 0(10) 0(6) 0(7) 0(47) Uiso 1 1 d D . . O14 O 0(10) 0(6) 1(7) 0(49) Uiso 1 1 d D . . O13 O 0(10) 0(6) 1(7) 0(47) Uiso 1 1 d D . . C59 C 0(14) 0(9) 1(11) 0(61) Uiso 1 1 d . . . H59A H 0.4565 0.1210 0.8097 0.165 Uiso 1 1 calc R . . O17 O 1(14) 0(8) 1(10) 0(69) Uiso 1 1 d . . . N19 N 0(12) 0(8) 1(9) 0(54) Uiso 1 1 d . . . C51 C 0(20) 0(11) 0(15) 0(98) Uiso 1 1 d . . . N18 N 0(9) 0(5) 0(7) 0(38) Uiso 1 1 d . . . C60 C 0(19) 0(12) 1(14) 0(114) Uiso 1 1 d . . . H60A H 0.3920 0.2305 0.7153 0.316 Uiso 1 1 calc R . . H60B H 0.3487 0.1773 0.7408 0.316 Uiso 1 1 calc R . . H60C H 0.4335 0.1702 0.7100 0.316 Uiso 1 1 calc R . . C61 C 1(18) 0(12) 1(14) 0(107) Uiso 1 1 d . . . H61A H 0.5564 0.2444 0.8758 0.309 Uiso 1 1 calc R . . H61B H 0.4785 0.2805 0.8277 0.309 Uiso 1 1 calc R . . H61C H 0.5642 0.2589 0.8041 0.309 Uiso 1 1 calc R . . C53 C 0(10) 0(7) 0(8) 0(142) Uiso 1 1 d G . . H53A H -0.3461 0.1474 0.2776 0.294 Uiso 1 1 calc R . . C54 C 0(10) 0(6) 0(5) 0(79) Uiso 1 1 d G . . H54A H -0.2014 0.1846 0.3322 0.196 Uiso 1 1 calc R . . C55 C 0(7) 0(5) 0(6) 0(53) Uiso 1 1 d G . . H55A H -0.1113 0.2294 0.2719 0.148 Uiso 1 1 calc R . . C56 C 0(8) 0(5) 0(6) 0(51) Uiso 1 1 d G . . H56A H -0.1659 0.2368 0.1571 0.143 Uiso 1 1 calc R . . C57 C 0(8) 0(5) 0(5) 0(58) Uiso 1 1 d G . . H57A H -0.3105 0.1995 0.1025 0.157 Uiso 1 1 calc R . . C58 C 0(7) 0(6) 0(8) 0(71) Uiso 1 1 d G . . H58A H -0.4007 0.1548 0.1628 0.181 Uiso 1 1 calc R . . C63 C 0(10) 0(12) 1(9) 0(80) Uiso 1 1 d G . . H63A H 0.0940 0.0382 0.7715 0.201 Uiso 1 1 calc R . . C62 C 0(16) 0(9) 1(11) 0(236) Uiso 1 1 d G . . H62A H 0.1659 0.1234 0.7605 0.410 Uiso 1 1 calc R . . C66 C 0(16) 0(8) 1(11) 0(226) Uiso 1 1 d G . . H66A H 0.3135 0.1238 0.7423 0.398 Uiso 1 1 calc R . . C64 C 0(10) 0(11) 1(8) 0(77) Uiso 1 1 d G . . H64A H 0.3890 0.0391 0.7352 0.194 Uiso 1 1 calc R . . C67 C 0(15) 0(8) 1(11) 0(258) Uiso 1 1 d G . . H67A H 0.3170 -0.0461 0.7462 0.434 Uiso 1 1 calc R . . C65 C 0(15) 0(9) 1(11) 0(209) Uiso 1 1 d G . . H65A H 0.1695 -0.0466 0.7644 0.383 Uiso 1 1 calc R . . C52 C 0(53) 0(29) 0(36) 1(428) Uiso 1 1 d . . . H52A H -0.0587 0.1381 0.2494 0.780 Uiso 1 1 calc R . . H52B H -0.0829 0.0884 0.2918 0.780 Uiso 1 1 calc R . . H52C H -0.0171 0.0777 0.2454 0.780 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0(5) 0(5) 0(5) 0(3) 0(4) 0(3) Ni2 0(5) 0(5) 0(5) 0(3) 0(4) 0(3) C1 0(41) 0(38) 0(40) 0(32) 0(33) 0(31) C2 0(46) 0(42) 0(55) 0(39) 0(41) 0(35) C3 0(48) 0(48) 0(54) 0(40) 0(42) 0(36) C4 0(45) 0(37) 0(44) 0(32) 0(36) 0(32) C5 0(35) 0(34) 0(34) 0(28) 0(28) 0(27) C6 0(38) 0(34) 0(36) 0(28) 0(30) 0(29) C7 0(35) 0(39) 0(36) 0(30) 0(29) 0(29) C8 0(38) 0(47) 0(43) 0(36) 0(32) 0(33) C9 0(47) 0(47) 0(50) 0(39) 0(39) 0(38) C10 0(54) 0(62) 0(66) 0(51) 0(49) 0(46) C11 0(56) 0(84) 0(57) 0(56) 0(45) 0(55) C12 0(48) 0(58) 0(47) 0(43) 0(38) 0(42) C13 0(43) 0(41) 0(39) 0(32) 0(33) 0(33) C14 0(46) 0(50) 0(42) 0(36) 0(35) 0(38) C15 0(47) 0(43) 0(41) 0(34) 0(35) 0(36) C16 0(41) 0(36) 0(39) 0(30) 0(33) 0(31) C17 0(37) 0(34) 0(35) 0(28) 0(29) 0(28) C18 0(38) 0(31) 0(35) 0(26) 0(29) 0(27) C19 0(35) 0(34) 0(33) 0(27) 0(27) 0(27) C20 0(35) 0(33) 0(35) 0(27) 0(28) 0(26) C21 0(48) 0(39) 0(42) 0(32) 0(36) 0(34) C22 0(44) 0(35) 0(37) 0(29) 0(33) 0(31) C23 0(46) 0(34) 0(44) 0(31) 0(36) 0(31) C24 0(41) 0(36) 0(38) 0(30) 0(32) 0(30) C25 0(40) 0(48) 0(47) 0(38) 0(34) 0(33) C26 0(43) 0(62) 0(63) 0(51) 0(42) 0(40) C27 0(42) 0(57) 0(51) 0(43) 0(38) 0(38) C28 0(39) 0(43) 0(44) 0(35) 0(33) 0(32) C29 0(35) 0(37) 0(35) 0(28) 0(28) 0(27) C30 0(32) 0(34) 0(32) 0(26) 0(26) 0(26) C31 0(36) 0(36) 0(34) 0(28) 0(28) 0(29) C32 0(36) 0(39) 0(36) 0(30) 0(29) 0(29) C33 0(38) 0(45) 0(39) 0(34) 0(31) 0(32) C34 0(43) 0(52) 0(49) 0(40) 0(37) 0(38) C35 0(49) 0(64) 0(52) 0(45) 0(41) 0(44) C36 0(43) 0(44) 0(43) 0(36) 0(35) 0(35) C37 0(41) 0(41) 0(40) 0(32) 0(32) 0(33) C38 0(49) 0(51) 0(39) 0(36) 0(35) 0(39) C39 0(43) 0(42) 0(45) 0(35) 0(35) 0(33) C40 0(40) 0(38) 0(43) 0(32) 0(34) 0(31) C41 0(39) 0(37) 0(40) 0(30) 0(32) 0(29) C42 0(40) 0(36) 0(39) 0(30) 0(31) 0(30) C43 0(36) 0(38) 0(36) 0(30) 0(29) 0(29) C44 0(36) 0(38) 0(35) 0(29) 0(28) 0(29) C45 0(45) 0(40) 0(39) 0(32) 0(34) 0(33) C46 0(42) 0(39) 0(39) 0(31) 0(32) 0(32) C47 0(50) 0(36) 0(42) 0(32) 0(37) 0(34) C48 0(47) 0(40) 0(41) 0(32) 0(35) 0(34) C49 0(93) 0(112) 0(75) 0(74) 0(68) 0(82) C50 0(84) 0(145) 0(138) 0(111) 0(84) 0(89) N1 0(31) 0(28) 0(29) 0(23) 0(24) 0(23) N2 0(28) 0(28) 0(29) 0(22) 0(23) 0(22) N3 0(31) 0(29) 0(32) 0(25) 0(25) 0(24) N4 0(43) 0(62) 0(56) 0(48) 0(40) 0(41) N5 0(31) 0(30) 0(30) 0(24) 0(25) 0(24) N6 0(30) 0(29) 0(28) 0(23) 0(24) 0(23) N7 0(30) 0(29) 0(30) 0(24) 0(24) 0(23) N8 0(29) 0(30) 0(29) 0(24) 0(23) 0(23) N9 0(30) 0(32) 0(30) 0(25) 0(24) 0(24) N10 0(28) 0(28) 0(28) 0(23) 0(23) 0(22) N11 0(28) 0(29) 0(29) 0(23) 0(23) 0(23) N12 0(34) 0(48) 0(39) 0(35) 0(30) 0(32) N13 0(32) 0(31) 0(29) 0(24) 0(25) 0(25) N14 0(30) 0(31) 0(30) 0(24) 0(24) 0(24) N15 0(34) 0(31) 0(32) 0(25) 0(26) 0(26) N16 0(32) 0(34) 0(30) 0(25) 0(24) 0(25) N17 0(98) 0(141) 0(74) 0(82) 0(66) 0(92) O1 0(28) 0(28) 0(26) 0(22) 0(22) 0(22) O2 0(51) 0(72) 0(67) 0(56) 0(48) 0(49) O3 0(28) 0(23) 0(25) 0(19) 0(21) 0(19) O4 0(29) 0(29) 0(27) 0(22) 0(22) 0(23) O5 0(28) 0(25) 0(28) 0(22) 0(23) 0(21) O6 0(37) 0(57) 0(47) 0(43) 0(34) 0(38) O7 0(28) 0(27) 0(25) 0(20) 0(21) 0(21) O8 0(32) 0(31) 0(28) 0(24) 0(24) 0(25) Cl1 0(57) 0(14) 0(14) 0(11) 0(23) 0(21) Cl2 0(15) 0(14) 0(18) 0(12) 0(13) 0(12) _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 N6 2(10) . ? Ni1 N2 2(10) . ? Ni1 N5 2(10) . ? Ni1 O3 2(10) . ? Ni1 N1 2(10) . ? Ni1 O1 2(10) . ? Ni2 N14 2(10) . ? Ni2 N10 2(10) . ? Ni2 N9 2(10) . ? Ni2 O7 2(10) . ? Ni2 N13 2(10) . ? Ni2 O5 2(10) . ? C1 N1 1(10) . ? C1 C2 1(10) . ? C1 H1A 0.9300 . ? C2 C3 1(10) . ? C2 H2A 0.9300 . ? C3 C4 1(10) . ? C3 H3A 0.9300 . ? C4 C5 1(10) . ? C4 H4A 0.9300 . ? C5 N1 1(10) . ? C5 C6 1(10) . ? C6 N2 1(10) . ? C6 H6A 0.9300 . ? C7 O1 1(10) . ? C7 N3 1(10) . ? C7 C8 1(10) . ? C8 C12 1(10) . ? C8 C9 1(10) . ? C9 C10 1(10) . ? C9 H9A 0.9300 . ? C10 N4 1(10) . ? C10 H10A 0.9300 . ? C11 N4 1(10) . ? C11 C12 1(10) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 N5 1(10) . ? C13 C14 1(10) . ? C13 H13A 0.9300 . ? C14 C15 1(10) . ? C14 H14A 0.9300 . ? C15 C16 1(10) . ? C15 H15A 0.9300 . ? C16 C17 1(10) . ? C16 H16A 0.9300 . ? C17 N5 1(10) . ? C17 C18 1(10) . ? C18 N6 1(10) . ? C18 H18A 0.9300 . ? C19 O3 1(10) . ? C19 N7 1(10) . ? C19 C20 1(10) . ? C20 C21 1(10) . ? C20 C24 1(10) . ? C21 C22 1(10) . ? C21 H21A 0.9300 . ? C22 N8 1(10) . ? C22 H22A 0.9300 . ? C23 N8 1(10) . ? C23 C24 1(10) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 N9 1(10) . ? C25 C26 1(10) . ? C25 H25A 0.9300 . ? C26 C27 1(10) . ? C26 H26A 0.9300 . ? C27 C28 1(10) . ? C27 H27A 0.9300 . ? C28 C29 1(10) . ? C28 H28A 0.9300 . ? C29 N9 1(10) . ? C29 C30 1(10) . ? C30 N10 1(10) . ? C30 H30A 0.9300 . ? C31 O5 1(10) . ? C31 N11 1(10) . ? C31 C32 1(10) . ? C32 C36 1(10) . ? C32 C33 1(10) . ? C33 C34 1(10) . ? C33 H33A 0.9300 . ? C34 N12 1(10) . ? C34 H34A 0.9300 . ? C35 N12 1(10) . ? C35 C36 1(10) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C37 C38 1(10) . ? C37 N13 1(10) . ? C37 H37A 0.9300 . ? C38 C39 1(10) . ? C38 H38A 0.9300 . ? C39 C40 1(10) . ? C39 H39A 0.9300 . ? C40 C41 1(10) . ? C40 H40A 0.9300 . ? C41 N13 1(10) . ? C41 C42 1(10) . ? C42 N14 1(10) . ? C42 H42A 0.9300 . ? C43 O7 1(10) . ? C43 N15 1(10) . ? C43 C44 2(10) . ? C44 C48 1(10) . ? C44 C45 1(10) . ? C45 C46 1(10) . ? C45 H45A 0.9300 . ? C46 N16 1(10) . ? C46 H46A 0.9300 . ? C47 N16 1(10) . ? C47 C48 1(10) . ? C47 H47A 0.9300 . ? C48 H48A 0.9300 . ? C49 N17 1(10) . ? C49 C50 1(10) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? N2 N3 1(10) . ? N3 H3B 0.8600 . ? N4 O2 1(10) . ? N6 N7 1(10) . ? N8 O4 1(10) . ? N10 N11 1(10) . ? N11 H11B 0.8600 . ? N12 O6 1(10) . ? N14 N15 1(10) . ? N16 O8 1(10) . ? Cl1 O9 1(10) . ? Cl1 O10 1(10) . ? Cl1 O11 1(10) . ? Cl1 O12 2(10) . ? Cl2 O13 1(10) . ? Cl2 O16 1(10) . ? Cl2 O15 1(10) . ? Cl2 O14 1(10) . ? C59 O17 1(10) . ? C59 N19 1(10) . ? C59 H59A 0.9300 . ? N19 C61 1(10) . ? N19 C60 2(10) . ? C51 N18 1(10) . ? C51 C52 2(10) . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C53 C54 1.4(6) . ? C53 C58 1.4(2) . ? C53 H53A 0.9300 . ? C54 C55 1.4(5) . ? C54 H54A 0.9300 . ? C55 C56 1.4(2) . ? C55 H55A 0.9300 . ? C56 C57 1.4(3) . ? C56 H56A 0.9300 . ? C57 C58 1.4(2) . ? C57 H57A 0.9300 . ? C58 H58A 0.9300 . ? C63 C62 1(2) . ? C63 C65 1.4(3) . ? C63 H63A 0.9300 . ? C62 C66 1.4(10) . ? C62 H62A 0.9300 . ? C66 C64 1.4(3) . ? C66 H66A 0.9300 . ? C64 C67 1.4(14) . ? C64 H64A 0.9300 . ? C67 C65 1.4(8) . ? C67 H67A 0.9300 . ? C65 H65A 0.9300 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? 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 N6 Ni1 N2 176(10) . . ? N6 Ni1 N5 79(10) . . ? N2 Ni1 N5 98(10) . . ? N6 Ni1 O3 76(10) . . ? N2 Ni1 O3 106(10) . . ? N5 Ni1 O3 155(10) . . ? N6 Ni1 N1 100(10) . . ? N2 Ni1 N1 77(10) . . ? N5 Ni1 N1 92(10) . . ? O3 Ni1 N1 96(10) . . ? N6 Ni1 O1 108(10) . . ? N2 Ni1 O1 75(10) . . ? N5 Ni1 O1 91(10) . . ? O3 Ni1 O1 92(10) . . ? N1 Ni1 O1 152(10) . . ? N14 Ni2 N10 177(10) . . ? N14 Ni2 N9 103(10) . . ? N10 Ni2 N9 78(10) . . ? N14 Ni2 O7 77(10) . . ? N10 Ni2 O7 100(10) . . ? N9 Ni2 O7 94(10) . . ? N14 Ni2 N13 78(10) . . ? N10 Ni2 N13 105(10) . . ? N9 Ni2 N13 94(10) . . ? O7 Ni2 N13 155(10) . . ? N14 Ni2 O5 104(10) . . ? N10 Ni2 O5 75(10) . . ? N9 Ni2 O5 153(10) . . ? O7 Ni2 O5 90(10) . . ? N13 Ni2 O5 93(10) . . ? N1 C1 C2 123(10) . . ? N1 C1 H1A 118.6 . . ? C2 C1 H1A 118.6 . . ? C3 C2 C1 119(10) . . ? C3 C2 H2A 120.5 . . ? C1 C2 H2A 120.5 . . ? C2 C3 C4 119(10) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C5 C4 C3 118(10) . . ? C5 C4 H4A 120.9 . . ? C3 C4 H4A 120.9 . . ? N1 C5 C4 123(10) . . ? N1 C5 C6 115(10) . . ? C4 C5 C6 122(10) . . ? N2 C6 C5 115(10) . . ? N2 C6 H6A 122.7 . . ? C5 C6 H6A 122.7 . . ? O1 C7 N3 120(10) . . ? O1 C7 C8 122(10) . . ? N3 C7 C8 118(10) . . ? C12 C8 C9 117(10) . . ? C12 C8 C7 120(10) . . ? C9 C8 C7 123(10) . . ? C10 C9 C8 121(10) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? N4 C10 C9 120(10) . . ? N4 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? N4 C11 C12 121(10) . . ? N4 C11 H11A 119.2 . . ? C12 C11 H11A 119.3 . . ? C8 C12 C11 121(10) . . ? C8 C12 H12A 119.5 . . ? C11 C12 H12A 119.5 . . ? N5 C13 C14 122(10) . . ? N5 C13 H13A 119.0 . . ? C14 C13 H13A 119.0 . . ? C15 C14 C13 120(10) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? C14 C15 C16 120(10) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? C15 C16 C17 118(10) . . ? C15 C16 H16A 120.9 . . ? C17 C16 H16A 120.9 . . ? N5 C17 C16 121(10) . . ? N5 C17 C18 116(10) . . ? C16 C17 C18 123(10) . . ? N6 C18 C17 115(10) . . ? N6 C18 H18A 122.6 . . ? C17 C18 H18A 122.6 . . ? O3 C19 N7 126(10) . . ? O3 C19 C20 120(10) . . ? N7 C19 C20 114(10) . . ? C21 C20 C24 117(10) . . ? C21 C20 C19 122(10) . . ? C24 C20 C19 121(10) . . ? C22 C21 C20 121(10) . . ? C22 C21 H21A 119.4 . . ? C20 C21 H21A 119.4 . . ? C21 C22 N8 122(10) . . ? C21 C22 H22A 119.2 . . ? N8 C22 H22A 119.2 . . ? N8 C23 C24 121(10) . . ? N8 C23 H23A 119.6 . . ? C24 C23 H23A 119.6 . . ? C23 C24 C20 121(10) . . ? C23 C24 H24A 119.7 . . ? C20 C24 H24A 119.7 . . ? N9 C25 C26 121(10) . . ? N9 C25 H25A 119.3 . . ? C26 C25 H25A 119.3 . . ? C27 C26 C25 121(10) . . ? C27 C26 H26A 119.6 . . ? C25 C26 H26A 119.6 . . ? C26 C27 C28 118(10) . . ? C26 C27 H27A 120.8 . . ? C28 C27 H27A 120.8 . . ? C27 C28 C29 118(10) . . ? C27 C28 H28A 120.8 . . ? C29 C28 H28A 120.8 . . ? N9 C29 C28 122(10) . . ? N9 C29 C30 116(10) . . ? C28 C29 C30 122(10) . . ? N10 C30 C29 115(10) . . ? N10 C30 H30A 122.6 . . ? C29 C30 H30A 122.6 . . ? O5 C31 N11 121(10) . . ? O5 C31 C32 120(10) . . ? N11 C31 C32 119(10) . . ? C36 C32 C33 119(10) . . ? C36 C32 C31 118(10) . . ? C33 C32 C31 123(10) . . ? C34 C33 C32 119(10) . . ? C34 C33 H33A 120.3 . . ? C32 C33 H33A 120.3 . . ? C33 C34 N12 121(10) . . ? C33 C34 H34A 119.3 . . ? N12 C34 H34A 119.3 . . ? N12 C35 C36 121(10) . . ? N12 C35 H35A 119.6 . . ? C36 C35 H35A 119.6 . . ? C32 C36 C35 120(10) . . ? C32 C36 H36A 120.2 . . ? C35 C36 H36A 120.2 . . ? C38 C37 N13 123(10) . . ? C38 C37 H37A 118.3 . . ? N13 C37 H37A 118.3 . . ? C37 C38 C39 119(10) . . ? C37 C38 H38A 120.3 . . ? C39 C38 H38A 120.3 . . ? C40 C39 C38 119(10) . . ? C40 C39 H39A 120.5 . . ? C38 C39 H39A 120.5 . . ? C39 C40 C41 120(10) . . ? C39 C40 H40A 120.0 . . ? C41 C40 H40A 120.0 . . ? N13 C41 C40 121(10) . . ? N13 C41 C42 114(10) . . ? C40 C41 C42 124(10) . . ? N14 C42 C41 116(10) . . ? N14 C42 H42A 121.8 . . ? C41 C42 H42A 121.8 . . ? O7 C43 N15 128(10) . . ? O7 C43 C44 118(10) . . ? N15 C43 C44 114(10) . . ? C48 C44 C45 119(10) . . ? C48 C44 C43 121(10) . . ? C45 C44 C43 120(10) . . ? C46 C45 C44 119(10) . . ? C46 C45 H45A 120.3 . . ? C44 C45 H45A 120.3 . . ? N16 C46 C45 120(10) . . ? N16 C46 H46A 119.8 . . ? C45 C46 H46A 119.8 . . ? N16 C47 C48 119(10) . . ? N16 C47 H47A 120.4 . . ? C48 C47 H47A 120.4 . . ? C44 C48 C47 121(10) . . ? C44 C48 H48A 119.6 . . ? C47 C48 H48A 119.6 . . ? N17 C49 C50 177(10) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C1 N1 C5 118(10) . . ? C1 N1 Ni1 129(10) . . ? C5 N1 Ni1 113(10) . . ? C6 N2 N3 122(10) . . ? C6 N2 Ni1 120(10) . . ? N3 N2 Ni1 118(10) . . ? C7 N3 N2 114(10) . . ? C7 N3 H3B 122.8 . . ? N2 N3 H3B 122.8 . . ? O2 N4 C11 123(10) . . ? O2 N4 C10 117(10) . . ? C11 N4 C10 120(10) . . ? C13 N5 C17 119(10) . . ? C13 N5 Ni1 130(10) . . ? C17 N5 Ni1 111(10) . . ? C18 N6 N7 122(10) . . ? C18 N6 Ni1 118(10) . . ? N7 N6 Ni1 120(10) . . ? C19 N7 N6 108(10) . . ? O4 N8 C23 121(10) . . ? O4 N8 C22 120(10) . . ? C23 N8 C22 119(10) . . ? C25 N9 C29 119(10) . . ? C25 N9 Ni2 128(10) . . ? C29 N9 Ni2 113(10) . . ? C30 N10 N11 124(10) . . ? C30 N10 Ni2 119(10) . . ? N11 N10 Ni2 118(10) . . ? C31 N11 N10 114(10) . . ? C31 N11 H11B 123.0 . . ? N10 N11 H11B 123.0 . . ? O6 N12 C35 120(10) . . ? O6 N12 C34 121(10) . . ? C35 N12 C34 120(10) . . ? C37 N13 C41 117(10) . . ? C37 N13 Ni2 131(10) . . ? C41 N13 Ni2 112(10) . . ? C42 N14 N15 123(10) . . ? C42 N14 Ni2 119(10) . . ? N15 N14 Ni2 118(10) . . ? C43 N15 N14 109(10) . . ? C47 N16 O8 120(10) . . ? C47 N16 C46 121(10) . . ? O8 N16 C46 118(10) . . ? C7 O1 Ni1 113(10) . . ? C19 O3 Ni1 110(10) . . ? C31 O5 Ni2 112(10) . . ? C43 O7 Ni2 109(10) . . ? O9 Cl1 O10 120(10) . . ? O9 Cl1 O11 121(10) . . ? O10 Cl1 O11 118(10) . . ? O9 Cl1 O12 90(10) . . ? O10 Cl1 O12 99(10) . . ? O11 Cl1 O12 92(10) . . ? O13 Cl2 O16 114(10) . . ? O13 Cl2 O15 114(10) . . ? O16 Cl2 O15 114(10) . . ? O13 Cl2 O14 112(10) . . ? O16 Cl2 O14 106(10) . . ? O15 Cl2 O14 95(10) . . ? O17 C59 N19 126(10) . . ? O17 C59 H59A 116.8 . . ? N19 C59 H59A 116.8 . . ? C59 N19 C61 126(10) . . ? C59 N19 C60 107(10) . . ? C61 N19 C60 126(10) . . ? N18 C51 C52 156(10) . . ? N19 C60 H60A 109.5 . . ? N19 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? N19 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N19 C61 H61A 109.5 . . ? N19 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N19 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C54 C53 C58 120(10) . . ? C54 C53 H53A 120.0 . . ? C58 C53 H53A 120.0 . . ? C53 C54 C55 120(10) . . ? C53 C54 H54A 120.0 . . ? C55 C54 H54A 120.0 . . ? C56 C55 C54 120(10) . . ? C56 C55 H55A 120.0 . . ? C54 C55 H55A 120.0 . . ? C57 C56 C55 120(10) . . ? C57 C56 H56A 120.0 . . ? C55 C56 H56A 120.0 . . ? C56 C57 C58 120(10) . . ? C56 C57 H57A 120.0 . . ? C58 C57 H57A 120.0 . . ? C57 C58 C53 120(10) . . ? C57 C58 H58A 120.0 . . ? C53 C58 H58A 120.0 . . ? C62 C63 C65 120(10) . . ? C62 C63 H63A 120.0 . . ? C65 C63 H63A 120.0 . . ? C66 C62 C63 120(10) . . ? C66 C62 H62A 120.0 . . ? C63 C62 H62A 120.0 . . ? C62 C66 C64 120(10) . . ? C62 C66 H66A 120.0 . . ? C64 C66 H66A 120.0 . . ? C67 C64 C66 120(10) . . ? C67 C64 H64A 120.0 . . ? C66 C64 H64A 120.0 . . ? C64 C67 C65 120(10) . . ? C64 C67 H67A 120.0 . . ? C65 C67 H67A 120.0 . . ? C67 C65 C63 120(10) . . ? C67 C65 H65A 120.0 . . ? C63 C65 H65A 120.0 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.3 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.701 _refine_diff_density_min -1.637 _refine_diff_density_rms 0.155 #===END ## Crystallographic Data of Complex 2 data_GdNi _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H40.50 Cl2 Gd0.50 N12 Ni O15' _chemical_formula_weight 1077.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Gd' 'Gd' -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 13.7063(4) _cell_length_b 12.4103(4) _cell_length_c 30.2541(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.781(2) _cell_angle_gamma 90.00 _cell_volume 5140.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 46208 _cell_measurement_theta_min 3.40 _cell_measurement_theta_max 27.53 _exptl_crystal_description 'block' _exptl_crystal_colour 'brownish red' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2194 _exptl_absorpt_coefficient_mu 1.185 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.642 _exptl_absorpt_correction_T_max 0.802 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44981 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 27.53 _reflns_number_total 11631 _reflns_number_gt 8145 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1227P)^2^+14.3446P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0036(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11631 _refine_ls_number_parameters 613 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.1168 _refine_ls_R_factor_gt 0.0814 _refine_ls_wR_factor_ref 0.2470 _refine_ls_wR_factor_gt 0.2173 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.5000 -0.25730(4) -0.2500 0.04823(19) Uani 1 2 d S . . Ni1 Ni 0.86481(6) 0.19717(7) -0.02357(3) 0.0467(2) Uani 1 1 d . . . C1 C 0.9125(5) 0.3991(6) 0.0364(2) 0.0561(16) Uani 1 1 d . . . H1A H 0.9404 0.3520 0.0573 0.067 Uiso 1 1 calc R . . C2 C 0.9074(6) 0.5072(7) 0.0469(3) 0.0639(18) Uani 1 1 d . . . H2A H 0.9303 0.5324 0.0744 0.077 Uiso 1 1 calc R . . C3 C 0.8680(7) 0.5759(6) 0.0158(3) 0.073(2) Uani 1 1 d . . . H3A H 0.8635 0.6490 0.0222 0.088 Uiso 1 1 calc R . . C4 C 0.8342(7) 0.5377(6) -0.0258(3) 0.075(2) Uani 1 1 d . . . H4A H 0.8084 0.5845 -0.0474 0.090 Uiso 1 1 calc R . . C5 C 0.8404(5) 0.4285(6) -0.0336(2) 0.0574(17) Uani 1 1 d . . . C6 C 0.8027(6) 0.3775(6) -0.0746(3) 0.066(2) Uani 1 1 d . . . H6A H 0.7782 0.4175 -0.0987 0.079 Uiso 1 1 calc R . . C7 C 0.7806(5) 0.1137(6) -0.1023(2) 0.0502(15) Uani 1 1 d . . . C8 C 0.7425(5) 0.0383(6) -0.1373(2) 0.0574(17) Uani 1 1 d . . . C9 C 0.6964(9) 0.0775(9) -0.1763(3) 0.098(4) Uani 1 1 d . . . H9A H 0.6862 0.1512 -0.1797 0.118 Uiso 1 1 calc R . . C10 C 0.6664(9) 0.0090(9) -0.2089(3) 0.099(4) Uani 1 1 d . . . H10A H 0.6375 0.0360 -0.2351 0.119 Uiso 1 1 calc R . . C11 C 0.7186(5) -0.1378(7) -0.1659(2) 0.0615(17) Uani 1 1 d . . . H11A H 0.7247 -0.2120 -0.1623 0.074 Uiso 1 1 calc R . . C12 C 0.7506(5) -0.0700(7) -0.1328(2) 0.0609(18) Uani 1 1 d . . . H12A H 0.7786 -0.0985 -0.1067 0.073 Uiso 1 1 calc R . . C13 C 1.0491(6) 0.1958(7) -0.0800(2) 0.0643(19) Uani 1 1 d . . . H13A H 1.0096 0.2232 -0.1033 0.077 Uiso 1 1 calc R . . C14 C 1.1464(7) 0.1771(7) -0.0869(3) 0.070(2) Uani 1 1 d . . . H14A H 1.1717 0.1905 -0.1143 0.084 Uiso 1 1 calc R . . C15 C 1.2048(6) 0.1386(6) -0.0527(3) 0.0659(19) Uani 1 1 d . . . H15A H 1.2711 0.1282 -0.0564 0.079 Uiso 1 1 calc R . . C16 C 1.1660(5) 0.1150(6) -0.0125(3) 0.0588(17) Uani 1 1 d . . . H16A H 1.2048 0.0870 0.0109 0.071 Uiso 1 1 calc R . . C17 C 1.0674(5) 0.1345(5) -0.0082(2) 0.0486(14) Uani 1 1 d . . . C18 C 1.0173(5) 0.1128(5) 0.0327(2) 0.0496(14) Uani 1 1 d . . . H18A H 1.0500 0.0868 0.0582 0.060 Uiso 1 1 calc R . . C19 C 0.7782(5) 0.1469(6) 0.0552(2) 0.0514(15) Uani 1 1 d . . . C20 C 0.7070(5) 0.1434(6) 0.0908(2) 0.0571(16) Uani 1 1 d . . . C21 C 0.7291(7) 0.1019(9) 0.1315(3) 0.083(3) Uani 1 1 d . . . H21A H 0.7905 0.0724 0.1379 0.100 Uiso 1 1 calc R . . C22 C 0.6598(8) 0.1032(10) 0.1639(3) 0.096(3) Uani 1 1 d . . . H22A H 0.6751 0.0742 0.1917 0.115 Uiso 1 1 calc R . . C23 C 0.5491(7) 0.1815(13) 0.1162(3) 0.106(4) Uani 1 1 d . . . H23A H 0.4861 0.2071 0.1102 0.128 Uiso 1 1 calc R . . C24 C 0.6146(7) 0.1830(11) 0.0831(3) 0.093(3) Uani 1 1 d . . . H24A H 0.5960 0.2111 0.0555 0.112 Uiso 1 1 calc R . . N1 N 0.8792(4) 0.3590(5) -0.00244(19) 0.0541(13) Uani 1 1 d . . . N2 N 0.8056(5) 0.2757(4) -0.07532(19) 0.0531(13) Uani 1 1 d . . . N3 N 0.7695(5) 0.2177(5) -0.11131(18) 0.0594(15) Uani 1 1 d . . . H3B H 0.7442 0.2442 -0.1355 0.071 Uiso 0.50 1 calc PR . . N4 N 0.6779(4) -0.0972(6) -0.20376(19) 0.0624(16) Uani 1 1 d . . . N5 N 1.0097(4) 0.1763(4) -0.04177(17) 0.0486(12) Uani 1 1 d . . . N6 N 0.9256(4) 0.1320(4) 0.03079(16) 0.0467(11) Uani 1 1 d . . . N7 N 0.8684(4) 0.1188(5) 0.06675(16) 0.0488(12) Uani 1 1 d . . . N8 N 0.5732(5) 0.1453(7) 0.1553(2) 0.0701(18) Uani 1 1 d . . . O1 O 0.8174(3) 0.0720(4) -0.06671(13) 0.0499(10) Uani 1 1 d . . . O2 O 0.6470(4) -0.1646(5) -0.23596(16) 0.0684(14) Uani 1 1 d . . . O3 O 0.7472(3) 0.1805(4) 0.01720(14) 0.0563(11) Uani 1 1 d . . . O4 O 0.5076(4) 0.1494(6) 0.18616(17) 0.0765(16) Uani 1 1 d . . . C25 C 0.2891(9) -0.3589(11) -0.2179(5) 0.114(4) Uani 1 1 d . . . H25A H 0.2684 -0.3409 -0.2466 0.137 Uiso 1 1 calc R . . C26 C 0.2523(16) -0.4336(17) -0.1501(5) 0.191(10) Uani 1 1 d . . . H26A H 0.3194 -0.4146 -0.1435 0.286 Uiso 1 1 calc R . . H26B H 0.2445 -0.5100 -0.1470 0.286 Uiso 1 1 calc R . . H26C H 0.2115 -0.3970 -0.1300 0.286 Uiso 1 1 calc R . . C27 C 0.1274(14) -0.427(2) -0.2079(7) 0.224(12) Uani 1 1 d . . . H27A H 0.1159 -0.4022 -0.2377 0.336 Uiso 1 1 calc R . . H27B H 0.0834 -0.3911 -0.1890 0.336 Uiso 1 1 calc R . . H27C H 0.1167 -0.5033 -0.2067 0.336 Uiso 1 1 calc R . . C28 C 0.5561(10) -0.4655(15) -0.1809(6) 0.282(19) Uani 1 1 d D . . H28 H 0.5128 -0.4458 -0.1596 0.339 Uiso 1 1 calc R . . C29 C 0.6638(19) -0.577(2) -0.1990(7) 0.232(11) Uiso 1 1 d D . . H29A H 0.6596 -0.5448 -0.2278 0.348 Uiso 1 1 calc R . . H29B H 0.6753 -0.6530 -0.2017 0.348 Uiso 1 1 calc R . . H29C H 0.7167 -0.5448 -0.1817 0.348 Uiso 1 1 calc R . . C30 C 0.558(3) -0.593(4) -0.1364(9) 0.36(2) Uiso 1 1 d D . . H30A H 0.4919 -0.5738 -0.1305 0.547 Uiso 1 1 calc R . . H30B H 0.6019 -0.5573 -0.1154 0.547 Uiso 1 1 calc R . . H30C H 0.5660 -0.6693 -0.1339 0.547 Uiso 1 1 calc R . . N9 N 0.2257(9) -0.4034(10) -0.1934(4) 0.127(4) Uani 1 1 d . . . N10 N 0.5777(12) -0.5605(13) -0.1784(8) 0.330(19) Uani 1 1 d D . . O5 O 0.3748(4) -0.3384(5) -0.20638(19) 0.0712(14) Uani 1 1 d . . . O6 O 0.5768(5) -0.3897(6) -0.2044(2) 0.099(2) Uani 1 1 d D . . Cl1 Cl 0.1110(3) 0.3596(3) 0.14039(11) 0.1198(11) Uani 1 1 d D . . O7 O 0.1092(9) 0.3227(12) 0.1843(3) 0.194(6) Uani 1 1 d D . . O8 O 0.0860(12) 0.2794(9) 0.1080(4) 0.204(8) Uani 1 1 d D . . O9 O 0.2121(6) 0.3878(9) 0.1330(4) 0.157(4) Uani 1 1 d D . . O10 O 0.0557(8) 0.4545(9) 0.1319(3) 0.163(4) Uani 1 1 d D . . Cl2 Cl 1.3413(7) -0.8021(7) -0.1801(2) 0.241(4) Uani 1 1 d D . . O11 O 1.4119(16) -0.8330(18) -0.2089(7) 0.47(3) Uani 1 1 d D . . O12 O 1.3705(16) -0.822(2) -0.1357(4) 0.561(14) Uani 1 1 d D . . O13 O 1.2539(12) -0.8679(15) -0.1901(5) 0.263(10) Uani 1 1 d D . . O14 O 1.3131(18) -0.6923(13) -0.1862(9) 0.337(15) Uani 1 1 d D . . C39 C 0.011(2) 0.092(3) 0.2168(11) 0.235(14) Uani 0.50 1 d PDU . . C37 C 0.081(2) 0.140(3) 0.2814(13) 0.203(17) Uani 0.50 1 d PDU . . C38 C 0.167(3) -0.002(3) 0.2529(15) 0.242(15) Uani 0.50 1 d PDU . . H38A H 0.1744 -0.0462 0.2274 0.363 Uiso 0.50 1 calc PR . . H38B H 0.1527 -0.0461 0.2778 0.363 Uiso 0.50 1 calc PR . . H38C H 0.2260 0.0378 0.2593 0.363 Uiso 0.50 1 calc PR . . O17 O -0.007(2) 0.049(3) 0.1799(11) 0.257(14) Uani 0.50 1 d PDU . . N13 N 0.0879(19) 0.072(3) 0.2443(10) 0.225(13) Uani 0.50 1 d PDU . . N11 N 0.6004(13) 0.9222(17) -0.0252(5) 0.175(6) Uiso 1 1 d . . . C32 C 0.5851(14) 1.008(2) -0.0379(6) 0.157(6) Uiso 1 1 d . . . C31 C 0.5514(19) 1.119(2) -0.0562(8) 0.211(10) Uiso 1 1 d . . . H31A H 0.5998 1.1722 -0.0483 0.317 Uiso 1 1 calc R . . H31B H 0.4906 1.1382 -0.0439 0.317 Uiso 1 1 calc R . . H31C H 0.5427 1.1149 -0.0879 0.317 Uiso 1 1 calc R . . C34 C 0.614(3) 0.477(4) 0.0147(12) 0.239(17) Uani 0.50 1 d PDU . . H34A H 0.6038 0.4533 -0.0154 0.359 Uiso 0.50 1 calc PR . . H34B H 0.5605 0.4538 0.0316 0.359 Uiso 0.50 1 calc PR . . H34C H 0.6738 0.4470 0.0271 0.359 Uiso 0.50 1 calc PR . . N12 N 0.620(2) 0.591(4) 0.0157(9) 0.238(15) Uani 0.50 1 d PDU . . C35 C 0.639(3) 0.633(4) 0.0584(12) 0.249(17) Uani 0.50 1 d PDU . . H35A H 0.6431 0.7097 0.0570 0.373 Uiso 0.50 1 calc PR . . H35B H 0.6989 0.6036 0.0707 0.373 Uiso 0.50 1 calc PR . . H35C H 0.5863 0.6129 0.0769 0.373 Uiso 0.50 1 calc PR . . C36 C 0.611(2) 0.665(3) -0.0152(12) 0.264(16) Uani 0.50 1 d PDU . . H36 H 0.6118 0.7365 -0.0065 0.316 Uiso 0.50 1 calc PR . . O16 O 0.603(2) 0.645(4) -0.0552(10) 0.276(16) Uani 0.50 1 d PDU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0511(3) 0.0493(3) 0.0445(3) 0.000 0.00387(17) 0.000 Ni1 0.0503(5) 0.0448(5) 0.0439(4) -0.0040(3) -0.0084(3) 0.0003(3) C1 0.068(4) 0.044(4) 0.055(4) -0.008(3) -0.009(3) -0.002(3) C2 0.064(4) 0.059(4) 0.068(4) -0.014(4) -0.006(3) -0.005(4) C3 0.089(6) 0.039(4) 0.090(6) -0.018(4) -0.013(4) 0.000(4) C4 0.096(6) 0.040(4) 0.087(5) 0.001(4) -0.021(5) 0.001(4) C5 0.067(4) 0.038(3) 0.065(4) -0.002(3) -0.015(3) 0.002(3) C6 0.090(6) 0.045(4) 0.062(4) 0.002(3) -0.016(4) 0.002(4) C7 0.051(3) 0.051(4) 0.048(3) -0.011(3) -0.005(3) -0.001(3) C8 0.063(4) 0.060(4) 0.048(3) -0.005(3) -0.010(3) -0.002(3) C9 0.152(10) 0.072(6) 0.066(5) -0.007(4) -0.046(6) 0.004(6) C10 0.144(10) 0.081(7) 0.067(5) -0.010(5) -0.047(6) 0.008(6) C11 0.059(4) 0.061(4) 0.064(4) -0.010(3) -0.005(3) 0.001(3) C12 0.057(4) 0.063(5) 0.060(4) -0.009(3) -0.016(3) 0.002(3) C13 0.077(5) 0.065(5) 0.050(4) -0.013(3) -0.001(3) -0.012(4) C14 0.079(5) 0.060(5) 0.073(5) -0.011(4) 0.018(4) -0.014(4) C15 0.063(4) 0.054(4) 0.082(5) -0.009(4) 0.013(4) -0.001(3) C16 0.055(4) 0.044(4) 0.077(5) -0.009(3) -0.002(3) 0.004(3) C17 0.054(4) 0.035(3) 0.056(3) -0.005(3) -0.001(3) -0.004(3) C18 0.054(4) 0.044(3) 0.050(3) -0.004(3) -0.010(3) 0.002(3) C19 0.053(4) 0.052(4) 0.048(3) -0.013(3) -0.003(3) -0.006(3) C20 0.057(4) 0.063(4) 0.050(4) -0.012(3) 0.003(3) -0.005(3) C21 0.074(5) 0.114(8) 0.064(5) 0.010(5) 0.019(4) 0.043(5) C22 0.092(7) 0.130(9) 0.067(5) 0.017(5) 0.025(4) 0.044(6) C23 0.056(5) 0.205(14) 0.058(5) -0.001(6) 0.004(4) 0.011(7) C24 0.062(5) 0.154(11) 0.062(5) 0.006(6) -0.004(4) 0.012(6) N1 0.057(3) 0.043(3) 0.061(3) -0.002(2) -0.011(2) 0.001(2) N2 0.067(4) 0.040(3) 0.051(3) -0.004(2) -0.011(2) 0.002(2) N3 0.078(4) 0.055(3) 0.044(3) -0.003(2) -0.017(3) 0.002(3) N4 0.056(3) 0.081(5) 0.050(3) -0.016(3) -0.003(2) -0.004(3) N5 0.049(3) 0.046(3) 0.050(3) -0.007(2) -0.004(2) -0.003(2) N6 0.054(3) 0.038(3) 0.046(3) -0.006(2) -0.007(2) -0.001(2) N7 0.055(3) 0.049(3) 0.042(3) -0.006(2) 0.001(2) 0.003(2) N8 0.061(4) 0.094(5) 0.055(3) -0.021(3) 0.006(3) -0.002(4) O1 0.058(3) 0.048(2) 0.043(2) -0.0057(18) -0.0135(18) 0.000(2) O2 0.063(3) 0.085(4) 0.057(3) -0.028(3) 0.001(2) -0.015(3) O3 0.048(2) 0.074(3) 0.046(2) 0.000(2) -0.0019(18) 0.002(2) O4 0.068(3) 0.106(5) 0.056(3) -0.025(3) 0.014(2) -0.004(3) C25 0.091(8) 0.125(11) 0.130(10) 0.040(8) 0.035(7) -0.002(7) C26 0.26(2) 0.184(18) 0.138(13) -0.007(12) 0.098(14) -0.111(17) C27 0.125(14) 0.30(3) 0.25(2) 0.02(2) 0.071(14) -0.078(17) C28 0.148(14) 0.37(3) 0.35(3) 0.28(3) 0.153(18) 0.18(2) N9 0.125(8) 0.126(9) 0.135(9) -0.007(7) 0.068(7) -0.040(7) N10 0.123(12) 0.34(3) 0.52(4) 0.35(3) -0.081(18) -0.056(15) O5 0.072(4) 0.066(3) 0.078(3) 0.015(3) 0.021(3) -0.001(3) O6 0.085(4) 0.098(5) 0.115(5) 0.054(4) 0.026(4) 0.031(4) Cl1 0.109(2) 0.142(3) 0.106(2) 0.031(2) -0.0148(16) 0.033(2) O7 0.201(12) 0.268(17) 0.115(8) 0.075(9) 0.018(7) 0.071(12) O8 0.303(19) 0.119(8) 0.176(11) 0.006(8) -0.127(13) -0.022(10) O9 0.108(7) 0.160(10) 0.201(10) 0.054(8) -0.022(7) 0.024(7) O10 0.145(8) 0.188(12) 0.155(9) 0.035(8) 0.007(7) 0.067(8) Cl2 0.346(10) 0.235(7) 0.150(4) -0.070(5) 0.112(6) -0.152(8) O11 0.63(5) 0.40(4) 0.43(3) -0.27(3) 0.39(4) -0.30(4) O12 0.54(3) 1.03(6) 0.121(12) -0.12(2) 0.089(18) -0.549 O13 0.31(2) 0.29(2) 0.197(14) -0.061(14) 0.027(13) -0.162(19) O14 0.38(4) 0.19(2) 0.44(4) -0.10(2) 0.05(3) 0.03(2) C39 0.122(17) 0.23(3) 0.34(4) 0.02(3) -0.10(2) -0.020(19) C37 0.12(2) 0.23(4) 0.25(4) 0.06(3) -0.07(2) -0.07(2) C38 0.15(2) 0.28(3) 0.29(3) 0.00(3) -0.08(2) -0.07(2) O17 0.127(16) 0.25(3) 0.39(4) 0.00(3) -0.10(2) -0.011(18) N13 0.115(17) 0.26(3) 0.29(3) 0.01(2) -0.08(2) -0.069(18) C34 0.21(2) 0.37(4) 0.145(19) 0.03(3) -0.006(18) 0.17(3) N12 0.199(19) 0.36(4) 0.151(17) 0.02(3) -0.012(16) 0.14(3) C35 0.20(2) 0.37(4) 0.17(2) 0.00(3) -0.04(2) 0.13(3) C36 0.19(2) 0.38(4) 0.21(3) 0.06(3) -0.09(2) 0.10(3) O16 0.19(2) 0.39(4) 0.24(3) 0.07(3) -0.09(2) 0.11(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O2 2.342(5) . ? Gd1 O2 2.342(5) 2_654 ? Gd1 O4 2.356(5) 3_655 ? Gd1 O4 2.356(5) 4 ? Gd1 O6 2.361(6) 2_654 ? Gd1 O6 2.361(6) . ? Gd1 O5 2.433(5) 2_654 ? Gd1 O5 2.433(5) . ? Ni1 N6 1.980(5) . ? Ni1 N2 1.984(6) . ? Ni1 O3 2.087(5) . ? Ni1 N5 2.103(5) . ? Ni1 O1 2.112(4) . ? Ni1 N1 2.114(6) . ? C1 N1 1.336(8) . ? C1 C2 1.381(10) . ? C1 H1A 0.9300 . ? C2 C3 1.362(12) . ? C2 H2A 0.9300 . ? C3 C4 1.401(11) . ? C3 H3A 0.9300 . ? C4 C5 1.380(10) . ? C4 H4A 0.9300 . ? C5 N1 1.367(9) . ? C5 C6 1.464(10) . ? C6 N2 1.265(9) . ? C6 H6A 0.9300 . ? C7 O1 1.276(8) . ? C7 N3 1.326(9) . ? C7 C8 1.489(9) . ? C8 C12 1.355(11) . ? C8 C9 1.397(11) . ? C9 C10 1.352(13) . ? C9 H9A 0.9300 . ? C10 N4 1.336(13) . ? C10 H10A 0.9300 . ? C11 N4 1.348(10) . ? C11 C12 1.364(10) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 N5 1.323(9) . ? C13 C14 1.380(12) . ? C13 H13A 0.9300 . ? C14 C15 1.363(12) . ? C14 H14A 0.9300 . ? C15 C16 1.383(11) . ? C15 H15A 0.9300 . ? C16 C17 1.386(10) . ? C16 H16A 0.9300 . ? C17 N5 1.360(8) . ? C17 C18 1.468(9) . ? C18 N6 1.278(8) . ? C18 H18A 0.9300 . ? C19 O3 1.277(8) . ? C19 N7 1.316(8) . ? C19 C20 1.488(10) . ? C20 C21 1.355(11) . ? C20 C24 1.368(12) . ? C21 C22 1.398(12) . ? C21 H21A 0.9300 . ? C22 N8 1.310(11) . ? C22 H22A 0.9300 . ? C23 N8 1.294(12) . ? C23 C24 1.376(13) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? N2 N3 1.377(8) . ? N3 H3B 0.8600 . ? N4 O2 1.337(7) . ? N6 N7 1.381(8) . ? N8 O4 1.329(8) . ? O4 Gd1 2.356(5) 3_655 ? C25 O5 1.235(14) . ? C25 N9 1.293(14) . ? C25 H25A 0.9300 . ? C26 N9 1.39(2) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 N9 1.43(2) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 N10 1.217(15) . ? C28 O6 1.220(13) . ? C28 H28 0.9300 . ? C29 N10 1.376(16) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 N10 1.371(17) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? Cl1 O7 1.406(9) . ? Cl1 O10 1.417(9) . ? Cl1 O8 1.427(10) . ? Cl1 O9 1.457(10) . ? Cl2 O11 1.388(13) . ? Cl2 O12 1.404(14) . ? Cl2 O14 1.426(15) . ? Cl2 O13 1.470(12) . ? C39 O17 1.255(19) . ? C39 N13 1.334(19) . ? C39 C37 1.40(5) 2 ? C39 N13 1.85(6) 2 ? C37 C39 1.40(5) 2 ? C37 N13 1.408(19) . ? C38 N13 1.433(18) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? N13 C39 1.85(6) 2 ? N11 C32 1.15(2) . ? C32 C31 1.55(3) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C34 N12 1.417(19) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? N12 C36 1.31(2) . ? N12 C35 1.404(18) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 O16 1.232(19) . ? C36 H36 0.9300 . ? 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 O2 Gd1 O2 121.1(3) . 2_654 ? O2 Gd1 O4 69.16(18) . 3_655 ? O2 Gd1 O4 78.3(2) 2_654 3_655 ? O2 Gd1 O4 78.3(2) . 4 ? O2 Gd1 O4 69.16(18) 2_654 4 ? O4 Gd1 O4 110.8(3) 3_655 4 ? O2 Gd1 O6 143.5(2) . 2_654 ? O2 Gd1 O6 83.1(3) 2_654 2_654 ? O4 Gd1 O6 147.0(2) 3_655 2_654 ? O4 Gd1 O6 87.3(3) 4 2_654 ? O2 Gd1 O6 83.1(3) . . ? O2 Gd1 O6 143.5(2) 2_654 . ? O4 Gd1 O6 87.3(3) 3_655 . ? O4 Gd1 O6 147.0(2) 4 . ? O6 Gd1 O6 91.8(4) 2_654 . ? O2 Gd1 O5 71.21(19) . 2_654 ? O2 Gd1 O5 136.75(19) 2_654 2_654 ? O4 Gd1 O5 137.7(2) 3_655 2_654 ? O4 Gd1 O5 74.3(2) 4 2_654 ? O6 Gd1 O5 72.6(2) 2_654 2_654 ? O6 Gd1 O5 73.9(2) . 2_654 ? O2 Gd1 O5 136.75(19) . . ? O2 Gd1 O5 71.21(19) 2_654 . ? O4 Gd1 O5 74.3(2) 3_655 . ? O4 Gd1 O5 137.7(2) 4 . ? O6 Gd1 O5 73.9(2) 2_654 . ? O6 Gd1 O5 72.6(2) . . ? O5 Gd1 O5 131.2(3) 2_654 . ? N6 Ni1 N2 174.7(2) . . ? N6 Ni1 O3 77.0(2) . . ? N2 Ni1 O3 102.5(2) . . ? N6 Ni1 N5 78.6(2) . . ? N2 Ni1 N5 102.1(2) . . ? O3 Ni1 N5 155.4(2) . . ? N6 Ni1 O1 108.49(19) . . ? N2 Ni1 O1 76.8(2) . . ? O3 Ni1 O1 93.95(19) . . ? N5 Ni1 O1 90.79(19) . . ? N6 Ni1 N1 96.2(2) . . ? N2 Ni1 N1 78.5(2) . . ? O3 Ni1 N1 88.8(2) . . ? N5 Ni1 N1 96.9(2) . . ? O1 Ni1 N1 155.2(2) . . ? N1 C1 C2 123.0(7) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C3 C2 C1 118.2(7) . . ? C3 C2 H2A 120.9 . . ? C1 C2 H2A 120.9 . . ? C2 C3 C4 120.7(7) . . ? C2 C3 H3A 119.6 . . ? C4 C3 H3A 119.6 . . ? C5 C4 C3 117.8(7) . . ? C5 C4 H4A 121.1 . . ? C3 C4 H4A 121.1 . . ? N1 C5 C4 121.7(7) . . ? N1 C5 C6 115.0(6) . . ? C4 C5 C6 123.2(7) . . ? N2 C6 C5 115.8(7) . . ? N2 C6 H6A 122.1 . . ? C5 C6 H6A 122.1 . . ? O1 C7 N3 127.3(6) . . ? O1 C7 C8 117.1(6) . . ? N3 C7 C8 115.6(6) . . ? C12 C8 C9 117.5(7) . . ? C12 C8 C7 121.8(6) . . ? C9 C8 C7 120.7(7) . . ? C10 C9 C8 120.5(9) . . ? C10 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? N4 C10 C9 120.3(8) . . ? N4 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? N4 C11 C12 119.9(8) . . ? N4 C11 H11A 120.1 . . ? C12 C11 H11A 120.1 . . ? C8 C12 C11 121.1(7) . . ? C8 C12 H12A 119.4 . . ? C11 C12 H12A 119.4 . . ? N5 C13 C14 122.5(8) . . ? N5 C13 H13A 118.7 . . ? C14 C13 H13A 118.7 . . ? C15 C14 C13 118.8(8) . . ? C15 C14 H14A 120.6 . . ? C13 C14 H14A 120.6 . . ? C14 C15 C16 120.3(8) . . ? C14 C15 H15A 119.8 . . ? C16 C15 H15A 119.8 . . ? C15 C16 C17 117.7(7) . . ? C15 C16 H16A 121.2 . . ? C17 C16 H16A 121.2 . . ? N5 C17 C16 122.0(6) . . ? N5 C17 C18 114.9(6) . . ? C16 C17 C18 123.1(6) . . ? N6 C18 C17 115.3(6) . . ? N6 C18 H18A 122.4 . . ? C17 C18 H18A 122.4 . . ? O3 C19 N7 126.3(6) . . ? O3 C19 C20 117.5(6) . . ? N7 C19 C20 116.2(6) . . ? C21 C20 C24 117.1(7) . . ? C21 C20 C19 122.9(7) . . ? C24 C20 C19 120.0(7) . . ? C20 C21 C22 120.2(8) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? N8 C22 C21 120.2(8) . . ? N8 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? N8 C23 C24 121.5(9) . . ? N8 C23 H23A 119.2 . . ? C24 C23 H23A 119.2 . . ? C20 C24 C23 120.2(9) . . ? C20 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C1 N1 C5 118.5(6) . . ? C1 N1 Ni1 130.0(5) . . ? C5 N1 Ni1 111.3(4) . . ? C6 N2 N3 121.7(6) . . ? C6 N2 Ni1 119.3(5) . . ? N3 N2 Ni1 119.0(4) . . ? C7 N3 N2 108.2(5) . . ? C7 N3 H3B 125.9 . . ? N2 N3 H3B 125.9 . . ? C10 N4 O2 120.1(6) . . ? C10 N4 C11 120.7(7) . . ? O2 N4 C11 119.3(7) . . ? C13 N5 C17 118.5(6) . . ? C13 N5 Ni1 129.5(5) . . ? C17 N5 Ni1 111.9(4) . . ? C18 N6 N7 122.5(5) . . ? C18 N6 Ni1 119.1(5) . . ? N7 N6 Ni1 118.1(4) . . ? C19 N7 N6 108.8(5) . . ? C23 N8 C22 120.7(7) . . ? C23 N8 O4 118.6(7) . . ? C22 N8 O4 120.8(7) . . ? C7 O1 Ni1 108.6(4) . . ? N4 O2 Gd1 132.7(4) . . ? C19 O3 Ni1 109.4(4) . . ? N8 O4 Gd1 131.1(5) . 3_655 ? O5 C25 N9 125.7(13) . . ? O5 C25 H25A 117.2 . . ? N9 C25 H25A 117.2 . . ? N9 C26 H26A 109.5 . . ? N9 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N9 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N9 C27 H27A 109.5 . . ? N9 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N9 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N10 C28 O6 136.1(16) . . ? N10 C28 H28 111.9 . . ? O6 C28 H28 111.9 . . ? N10 C29 H29A 109.5 . . ? N10 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N10 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N10 C30 H30A 109.5 . . ? N10 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N10 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C25 N9 C26 120.0(14) . . ? C25 N9 C27 124.2(15) . . ? C26 N9 C27 115.8(13) . . ? C28 N10 C30 106(3) . . ? C28 N10 C29 109.1(17) . . ? C30 N10 C29 126.0(19) . . ? C25 O5 Gd1 128.2(7) . . ? C28 O6 Gd1 140.1(8) . . ? O7 Cl1 O10 114.1(7) . . ? O7 Cl1 O8 114.0(8) . . ? O10 Cl1 O8 110.3(6) . . ? O7 Cl1 O9 106.5(7) . . ? O10 Cl1 O9 106.1(7) . . ? O8 Cl1 O9 105.1(8) . . ? O11 Cl2 O12 112.1(14) . . ? O11 Cl2 O14 112.1(12) . . ? O12 Cl2 O14 110.9(11) . . ? O11 Cl2 O13 107.6(10) . . ? O12 Cl2 O13 107.0(10) . . ? O14 Cl2 O13 107.0(12) . . ? O17 C39 N13 126(3) . . ? O17 C39 C37 94(3) . 2 ? N13 C39 C37 138(3) . 2 ? O17 C39 N13 113(2) . 2 ? N13 C39 N13 99(2) . 2 ? C37 C39 N13 48.9(17) 2 2 ? C39 C37 N13 83(3) 2 . ? N13 C38 H38A 109.5 . . ? N13 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N13 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C39 N13 C37 108(3) . . ? C39 N13 C38 143(3) . . ? C37 N13 C38 108.2(17) . . ? C39 N13 C39 78(3) . 2 ? C37 N13 C39 48.6(18) . 2 ? C38 N13 C39 122(3) . 2 ? N11 C32 C31 173(2) . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N12 C34 H34A 109.5 . . ? N12 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N12 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 N12 C35 114(3) . . ? C36 N12 C34 133(3) . . ? C35 N12 C34 113(2) . . ? N12 C35 H35A 109.5 . . ? N12 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N12 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O16 C36 N12 124(3) . . ? O16 C36 H36 117.8 . . ? N12 C36 H36 117.8 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.244 _refine_diff_density_min -1.122 _refine_diff_density_rms 0.125 #===END # Crystallographic Data of Complex 3 data_TbNi _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H41 Cl2 N12 Ni O15 Tb0.50' _chemical_formula_weight 1078.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tb' 'Tb' -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 13.7842(3) _cell_length_b 12.4662(4) _cell_length_c 30.2055(11) _cell_angle_alpha 90.00 _cell_angle_beta 92.7503(18) _cell_angle_gamma 90.00 _cell_volume 5184.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 14059 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 25.028 _exptl_crystal_description 'block' _exptl_crystal_colour 'brownish red' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2198 _exptl_absorpt_coefficient_mu 1.217 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.670 _exptl_absorpt_correction_T_max 0.731 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40890 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 25.05 _reflns_number_total 9089 _reflns_number_gt 6975 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1276P)^2^+16.2038P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9089 _refine_ls_number_parameters 613 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.1013 _refine_ls_R_factor_gt 0.0783 _refine_ls_wR_factor_ref 0.2376 _refine_ls_wR_factor_gt 0.2200 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.5000 -0.25235(4) -0.2500 0.0511(2) Uani 1 2 d S . . Ni1 Ni 0.86393(7) 0.19802(8) -0.02263(3) 0.0536(3) Uani 1 1 d . . . C1 C 0.9123(6) 0.3994(7) 0.0377(3) 0.071(2) Uani 1 1 d . . . H1A H 0.9386 0.3533 0.0593 0.085 Uiso 1 1 calc R . . C2 C 0.9086(7) 0.5088(8) 0.0472(3) 0.075(2) Uani 1 1 d . . . H2A H 0.9328 0.5351 0.0743 0.089 Uiso 1 1 calc R . . C3 C 0.8695(7) 0.5749(7) 0.0164(3) 0.080(3) Uani 1 1 d . . . H3A H 0.8650 0.6476 0.0228 0.096 Uiso 1 1 calc R . . C4 C 0.8358(8) 0.5388(8) -0.0244(4) 0.086(3) Uani 1 1 d . . . H4A H 0.8093 0.5861 -0.0455 0.103 Uiso 1 1 calc R . . C5 C 0.8423(7) 0.4300(7) -0.0334(3) 0.068(2) Uani 1 1 d . . . C6 C 0.8040(7) 0.3795(7) -0.0742(3) 0.071(2) Uani 1 1 d . . . H6A H 0.7804 0.4192 -0.0985 0.085 Uiso 1 1 calc R . . C7 C 0.7774(5) 0.1147(7) -0.1013(2) 0.0567(19) Uani 1 1 d . . . C8 C 0.7403(6) 0.0408(7) -0.1364(3) 0.060(2) Uani 1 1 d . . . C9 C 0.6945(9) 0.0783(9) -0.1747(3) 0.098(4) Uani 1 1 d . . . H9A H 0.6845 0.1517 -0.1781 0.117 Uiso 1 1 calc R . . C10 C 0.6634(9) 0.0107(9) -0.2079(3) 0.095(3) Uani 1 1 d . . . H10A H 0.6344 0.0381 -0.2339 0.115 Uiso 1 1 calc R . . C11 C 0.7164(6) -0.1357(7) -0.1649(3) 0.064(2) Uani 1 1 d . . . H11A H 0.7235 -0.2094 -0.1615 0.077 Uiso 1 1 calc R . . C12 C 0.7473(5) -0.0675(7) -0.1321(3) 0.062(2) Uani 1 1 d . . . H12A H 0.7743 -0.0959 -0.1058 0.074 Uiso 1 1 calc R . . C13 C 1.0466(7) 0.1958(8) -0.0793(3) 0.068(2) Uani 1 1 d . . . H13A H 1.0068 0.2239 -0.1022 0.082 Uiso 1 1 calc R . . C14 C 1.1422(8) 0.1769(8) -0.0871(3) 0.078(3) Uani 1 1 d . . . H14A H 1.1664 0.1908 -0.1148 0.093 Uiso 1 1 calc R . . C15 C 1.2017(7) 0.1369(7) -0.0530(3) 0.071(2) Uani 1 1 d . . . H15A H 1.2673 0.1251 -0.0571 0.085 Uiso 1 1 calc R . . C16 C 1.1633(6) 0.1149(6) -0.0133(3) 0.065(2) Uani 1 1 d . . . H16A H 1.2019 0.0871 0.0101 0.078 Uiso 1 1 calc R . . C17 C 1.0647(6) 0.1348(6) -0.0084(3) 0.0551(18) Uani 1 1 d . . . C18 C 1.0162(5) 0.1121(6) 0.0332(2) 0.0521(17) Uani 1 1 d . . . H18A H 1.0494 0.0862 0.0585 0.063 Uiso 1 1 calc R . . C19 C 0.7794(6) 0.1498(7) 0.0563(2) 0.0585(19) Uani 1 1 d . . . C20 C 0.7087(6) 0.1427(7) 0.0921(3) 0.065(2) Uani 1 1 d . . . C21 C 0.7301(7) 0.0990(9) 0.1321(3) 0.077(3) Uani 1 1 d . . . H21A H 0.7907 0.0680 0.1380 0.092 Uiso 1 1 calc R . . C22 C 0.6623(7) 0.0997(10) 0.1648(3) 0.088(3) Uani 1 1 d . . . H22A H 0.6775 0.0690 0.1923 0.105 Uiso 1 1 calc R . . C23 C 0.5506(8) 0.1833(14) 0.1173(3) 0.114(5) Uani 1 1 d . . . H23A H 0.4887 0.2114 0.1119 0.137 Uiso 1 1 calc R . . C24 C 0.6154(8) 0.1826(14) 0.0845(4) 0.116(5) Uani 1 1 d . . . H24A H 0.5967 0.2093 0.0566 0.139 Uiso 1 1 calc R . . N1 N 0.8792(5) 0.3570(5) -0.0018(2) 0.0566(16) Uani 1 1 d . . . N2 N 0.8053(5) 0.2752(5) -0.0744(2) 0.0585(16) Uani 1 1 d . . . N3 N 0.7683(5) 0.2182(5) -0.1100(2) 0.0622(17) Uani 1 1 d . . . H3B H 0.7433 0.2452 -0.1342 0.075 Uiso 0.50 1 calc PR . . N4 N 0.6748(5) -0.0940(7) -0.2030(2) 0.0684(19) Uani 1 1 d . . . N5 N 1.0081(5) 0.1764(5) -0.04125(19) 0.0542(15) Uani 1 1 d . . . N6 N 0.9248(4) 0.1310(5) 0.03160(19) 0.0496(14) Uani 1 1 d . . . N7 N 0.8691(5) 0.1183(5) 0.0676(2) 0.0540(15) Uani 1 1 d . . . N8 N 0.5758(5) 0.1443(7) 0.1564(2) 0.072(2) Uani 1 1 d . . . O1 O 0.8155(4) 0.0745(4) -0.06582(16) 0.0553(12) Uani 1 1 d . . . O2 O 0.6459(4) -0.1598(6) -0.23542(19) 0.0764(17) Uani 1 1 d . . . O3 O 0.7477(4) 0.1819(5) 0.01848(17) 0.0673(15) Uani 1 1 d . . . O4 O 0.5100(4) 0.1446(6) 0.1870(2) 0.0804(19) Uani 1 1 d . . . C25 C 0.2885(10) -0.3428(13) -0.2157(5) 0.129(5) Uani 1 1 d . . . H25 H 0.2655 -0.3130 -0.2424 0.154 Uiso 1 1 calc R . . C26 C 0.2574(17) -0.4287(18) -0.1493(5) 0.206(11) Uani 1 1 d . . . H26A H 0.3264 -0.4192 -0.1457 0.308 Uiso 1 1 calc R . . H26B H 0.2420 -0.5035 -0.1468 0.308 Uiso 1 1 calc R . . H26C H 0.2260 -0.3892 -0.1268 0.308 Uiso 1 1 calc R . . C27 C 0.1276(16) -0.393(3) -0.2012(9) 0.34(2) Uani 1 1 d . . . H27A H 0.1125 -0.3649 -0.2303 0.505 Uiso 1 1 calc R . . H27B H 0.0955 -0.3516 -0.1796 0.505 Uiso 1 1 calc R . . H27C H 0.1057 -0.4665 -0.2000 0.505 Uiso 1 1 calc R . . C28 C 0.5550(14) -0.4580(18) -0.1826(8) 0.52(5) Uani 1 1 d D . . H28 H 0.5076 -0.4394 -0.1631 0.623 Uiso 1 1 calc R . . C29 C 0.663(2) -0.567(3) -0.1990(9) 0.280(15) Uiso 1 1 d D . . H29A H 0.6639 -0.5201 -0.2240 0.420 Uiso 1 1 calc R . . H29B H 0.6676 -0.6403 -0.2088 0.420 Uiso 1 1 calc R . . H29C H 0.7161 -0.5512 -0.1786 0.420 Uiso 1 1 calc R . . C30 C 0.559(2) -0.602(3) -0.1383(9) 0.323(19) Uiso 1 1 d D . . H30A H 0.4967 -0.5805 -0.1289 0.485 Uiso 1 1 calc R . . H30B H 0.6085 -0.5803 -0.1166 0.485 Uiso 1 1 calc R . . H30C H 0.5609 -0.6784 -0.1418 0.485 Uiso 1 1 calc R . . N9 N 0.2240(9) -0.3899(11) -0.1926(5) 0.146(5) Uani 1 1 d . . . N10 N 0.5763(11) -0.5539(15) -0.1781(7) 0.328(19) Uani 1 1 d D . . O5 O 0.3743(5) -0.3326(5) -0.2073(2) 0.0722(16) Uani 1 1 d . . . O6 O 0.5758(5) -0.3828(6) -0.2038(3) 0.099(2) Uani 1 1 d D . . Cl1 Cl 0.1136(3) 0.3575(3) 0.14055(12) 0.1200(11) Uani 1 1 d D . . O7 O 0.1114(10) 0.3241(13) 0.1854(3) 0.220(7) Uani 1 1 d D . . O8 O 0.0884(12) 0.2759(8) 0.1099(4) 0.207(8) Uani 1 1 d D . . O9 O 0.2137(6) 0.3863(9) 0.1332(4) 0.162(4) Uani 1 1 d D . . O10 O 0.0573(8) 0.4516(9) 0.1315(4) 0.165(5) Uani 1 1 d D . . Cl2 Cl 1.3358(8) -0.7946(7) -0.1818(2) 0.262(5) Uani 1 1 d D . . O11 O 1.4081(17) -0.8260(18) -0.2097(8) 0.48(3) Uani 1 1 d D . . O12 O 1.3701(18) -0.813(2) -0.1372(5) 0.566(14) Uani 1 1 d D . . O13 O 1.2525(13) -0.8614(16) -0.1915(6) 0.292(11) Uani 1 1 d D . . O14 O 1.311(2) -0.6856(12) -0.1857(10) 0.41(2) Uani 1 1 d D . . C39 C 0.027(2) 0.071(3) 0.2080(10) 0.254(14) Uani 0.50 1 d PDU . . H39 H -0.0200 0.1188 0.2168 0.305 Uiso 0.50 1 calc PR . . C37 C 0.082(3) 0.140(4) 0.2736(16) 0.25(2) Uani 0.50 1 d PDU . . C38 C 0.174(3) -0.004(3) 0.2532(15) 0.252(16) Uani 0.50 1 d PDU . . H38A H 0.1919 -0.0494 0.2293 0.378 Uiso 0.50 1 calc PR . . H38B H 0.1520 -0.0472 0.2771 0.378 Uiso 0.50 1 calc PR . . H38C H 0.2284 0.0382 0.2634 0.378 Uiso 0.50 1 calc PR . . O17 O 0.003(2) 0.034(3) 0.1716(9) 0.235(12) Uani 0.50 1 d PDU . . N13 N 0.096(2) 0.066(3) 0.2377(9) 0.244(14) Uani 0.50 1 d PDU . . N11 N 0.5991(15) 0.920(2) -0.0231(7) 0.204(7) Uiso 1 1 d . . . C32 C 0.5866(17) 1.011(2) -0.0297(8) 0.193(9) Uiso 1 1 d . . . C31 C 0.552(2) 1.106(2) -0.0557(9) 0.237(11) Uiso 1 1 d . . . H31A H 0.5583 1.1695 -0.0376 0.355 Uiso 1 1 calc R . . H31B H 0.4846 1.0965 -0.0649 0.355 Uiso 1 1 calc R . . H31C H 0.5896 1.1143 -0.0813 0.355 Uiso 1 1 calc R . . C34 C 0.617(2) 0.467(2) 0.0131(11) 0.169(11) Uani 0.50 1 d PDU . . H34A H 0.6043 0.4412 -0.0165 0.254 Uiso 0.50 1 calc PR . . H34B H 0.5641 0.4468 0.0311 0.254 Uiso 0.50 1 calc PR . . H34C H 0.6762 0.4371 0.0253 0.254 Uiso 0.50 1 calc PR . . N12 N 0.6244(16) 0.581(2) 0.0124(7) 0.168(9) Uani 0.50 1 d PDU . . C35 C 0.644(2) 0.623(3) 0.0558(10) 0.182(11) Uani 0.50 1 d PDU . . H35A H 0.6490 0.6994 0.0542 0.273 Uiso 0.50 1 calc PR . . H35B H 0.7037 0.5934 0.0680 0.273 Uiso 0.50 1 calc PR . . H35C H 0.5919 0.6038 0.0744 0.273 Uiso 0.50 1 calc PR . . C36 C 0.6130(19) 0.647(3) -0.0213(10) 0.177(11) Uani 0.50 1 d PDU . . H36A H 0.6174 0.7202 -0.0159 0.213 Uiso 0.50 1 calc PR . . O16 O 0.5964(17) 0.615(2) -0.0600(8) 0.185(10) Uani 0.50 1 d PDU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.0550(3) 0.0547(3) 0.0436(3) 0.000 0.0035(2) 0.000 Ni1 0.0602(6) 0.0535(6) 0.0459(5) -0.0044(4) -0.0106(4) 0.0061(5) C1 0.076(6) 0.068(6) 0.067(5) -0.012(4) -0.013(4) 0.012(4) C2 0.077(6) 0.067(6) 0.079(6) -0.027(5) -0.002(5) 0.003(5) C3 0.093(7) 0.043(4) 0.102(7) -0.024(5) -0.024(6) 0.009(4) C4 0.099(7) 0.055(5) 0.100(7) 0.000(5) -0.027(6) 0.019(5) C5 0.079(6) 0.050(5) 0.073(6) -0.003(4) -0.020(4) 0.007(4) C6 0.093(6) 0.049(5) 0.069(5) -0.004(4) -0.019(5) 0.011(4) C7 0.055(4) 0.065(5) 0.049(4) -0.004(4) -0.007(3) 0.001(4) C8 0.063(5) 0.065(5) 0.052(4) -0.002(4) -0.009(4) 0.005(4) C9 0.140(10) 0.080(7) 0.069(6) -0.012(5) -0.045(6) 0.021(7) C10 0.134(9) 0.076(7) 0.071(6) -0.010(5) -0.043(6) -0.003(6) C11 0.062(5) 0.066(5) 0.062(5) -0.010(4) -0.007(4) 0.001(4) C12 0.051(4) 0.067(5) 0.065(5) 0.000(4) -0.012(4) 0.003(4) C13 0.086(6) 0.068(5) 0.051(5) -0.009(4) -0.002(4) -0.004(5) C14 0.094(7) 0.076(6) 0.064(6) -0.014(5) 0.018(5) -0.016(5) C15 0.075(6) 0.061(5) 0.078(6) -0.009(5) 0.014(5) 0.001(4) C16 0.061(5) 0.052(5) 0.082(6) -0.009(4) -0.003(4) 0.006(4) C17 0.068(5) 0.042(4) 0.055(4) -0.003(3) 0.002(4) 0.002(3) C18 0.060(4) 0.050(4) 0.046(4) -0.003(3) -0.005(3) 0.005(3) C19 0.066(5) 0.062(5) 0.047(4) -0.009(4) 0.001(4) 0.005(4) C20 0.065(5) 0.077(6) 0.055(5) -0.017(4) 0.003(4) 0.011(4) C21 0.069(5) 0.097(7) 0.064(5) -0.002(5) 0.013(4) 0.020(5) C22 0.073(6) 0.115(9) 0.075(6) -0.004(6) 0.011(5) 0.024(6) C23 0.069(6) 0.211(15) 0.062(6) -0.023(8) 0.001(5) 0.035(8) C24 0.072(6) 0.210(15) 0.065(6) -0.001(8) -0.006(5) 0.036(8) N1 0.072(4) 0.040(3) 0.056(4) 0.000(3) -0.020(3) 0.001(3) N2 0.071(4) 0.051(4) 0.052(4) -0.009(3) -0.012(3) 0.001(3) N3 0.080(5) 0.055(4) 0.049(4) -0.007(3) -0.019(3) 0.004(3) N4 0.056(4) 0.088(6) 0.060(4) -0.017(4) -0.004(3) -0.007(4) N5 0.066(4) 0.052(4) 0.044(3) -0.007(3) -0.003(3) 0.001(3) N6 0.059(4) 0.041(3) 0.047(3) -0.006(3) -0.006(3) 0.005(3) N7 0.060(4) 0.054(4) 0.048(3) -0.007(3) 0.002(3) 0.010(3) N8 0.066(4) 0.088(5) 0.062(4) -0.030(4) 0.005(3) 0.005(4) O1 0.064(3) 0.052(3) 0.048(3) -0.001(2) -0.012(2) 0.003(2) O2 0.062(3) 0.102(5) 0.064(3) -0.032(3) -0.006(3) -0.008(3) O3 0.061(3) 0.090(4) 0.050(3) -0.001(3) -0.006(2) 0.015(3) O4 0.063(3) 0.111(5) 0.069(4) -0.036(4) 0.016(3) -0.003(3) C25 0.091(9) 0.161(14) 0.138(12) 0.060(10) 0.040(8) -0.003(9) C26 0.29(3) 0.23(2) 0.101(12) 0.012(13) 0.075(14) -0.13(2) C27 0.139(18) 0.60(7) 0.28(3) 0.11(4) 0.08(2) -0.10(3) C28 0.23(3) 0.92(11) 0.42(5) 0.48(7) 0.21(3) 0.36(5) N9 0.117(9) 0.158(12) 0.169(12) 0.016(10) 0.072(9) -0.035(8) N10 0.092(10) 0.59(5) 0.29(2) 0.30(3) -0.042(13) 0.014(18) O5 0.072(4) 0.076(4) 0.070(4) 0.010(3) 0.018(3) 0.000(3) O6 0.100(5) 0.101(5) 0.100(5) 0.057(4) 0.027(4) 0.035(4) Cl1 0.108(2) 0.145(3) 0.105(2) 0.025(2) -0.0155(18) 0.027(2) O7 0.222(14) 0.32(2) 0.117(8) 0.101(11) 0.024(8) 0.099(14) O8 0.296(19) 0.114(8) 0.197(13) 0.008(8) -0.136(14) -0.030(9) O9 0.099(7) 0.183(11) 0.200(11) 0.059(9) -0.023(7) 0.011(7) O10 0.151(9) 0.194(12) 0.150(9) 0.032(8) 0.003(7) 0.077(9) Cl2 0.416(13) 0.229(7) 0.148(5) -0.053(5) 0.101(6) -0.178(9) O11 0.75(6) 0.29(3) 0.45(4) -0.17(3) 0.46(5) -0.21(4) O12 0.71(4) 0.88(5) 0.109(13) -0.12(2) 0.09(2) -0.549 O13 0.33(3) 0.29(2) 0.26(2) -0.088(18) 0.049(17) -0.15(2) O14 0.68(6) 0.141(17) 0.42(4) -0.05(2) 0.05(4) -0.03(3) C39 0.20(2) 0.30(3) 0.25(3) -0.02(2) -0.11(2) -0.05(2) C37 0.14(2) 0.32(5) 0.29(4) 0.06(4) -0.09(3) -0.09(3) C38 0.15(2) 0.35(4) 0.25(3) 0.00(3) -0.10(2) -0.08(2) O17 0.171(19) 0.29(3) 0.23(3) -0.05(2) -0.111(19) -0.03(2) N13 0.133(18) 0.33(4) 0.26(3) 0.00(2) -0.09(2) -0.08(2) C34 0.155(18) 0.19(2) 0.16(2) 0.01(2) -0.024(16) 0.09(2) N12 0.144(14) 0.21(2) 0.153(17) -0.005(18) -0.023(14) 0.073(17) C35 0.143(19) 0.22(3) 0.17(2) -0.02(2) -0.040(18) 0.06(2) C36 0.137(17) 0.21(2) 0.18(2) 0.05(2) -0.02(2) 0.022(18) O16 0.146(16) 0.22(2) 0.19(2) 0.08(2) -0.008(17) 0.030(15) _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 Tb1 O4 2.338(6) 3_655 ? Tb1 O4 2.338(6) 4 ? Tb1 O2 2.342(6) . ? Tb1 O2 2.342(6) 2_654 ? Tb1 O6 2.355(7) . ? Tb1 O6 2.355(7) 2_654 ? Tb1 O5 2.426(6) . ? Tb1 O5 2.426(6) 2_654 ? Ni1 N2 1.976(7) . ? Ni1 N6 1.989(6) . ? Ni1 O3 2.083(6) . ? Ni1 N1 2.087(6) . ? Ni1 O1 2.106(5) . ? Ni1 N5 2.108(6) . ? C1 N1 1.363(10) . ? C1 C2 1.394(12) . ? C1 H1A 0.9300 . ? C2 C3 1.338(13) . ? C2 H2A 0.9300 . ? C3 C4 1.370(13) . ? C3 H3A 0.9300 . ? C4 C5 1.387(12) . ? C4 H4A 0.9300 . ? C5 N1 1.396(10) . ? C5 C6 1.462(12) . ? C6 N2 1.300(10) . ? C6 H6A 0.9300 . ? C7 O1 1.273(9) . ? C7 N3 1.321(10) . ? C7 C8 1.479(11) . ? C8 C12 1.359(12) . ? C8 C9 1.373(12) . ? C9 C10 1.363(13) . ? C9 H9A 0.9300 . ? C10 N4 1.321(13) . ? C10 H10A 0.9300 . ? C11 C12 1.359(11) . ? C11 N4 1.362(11) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 N5 1.311(10) . ? C13 C14 1.371(13) . ? C13 H13A 0.9300 . ? C14 C15 1.379(13) . ? C14 H14A 0.9300 . ? C15 C16 1.364(12) . ? C15 H15A 0.9300 . ? C16 C17 1.397(11) . ? C16 H16A 0.9300 . ? C17 N5 1.337(10) . ? C17 C18 1.477(11) . ? C18 N6 1.279(9) . ? C18 H18A 0.9300 . ? C19 O3 1.268(9) . ? C19 N7 1.327(10) . ? C19 C20 1.492(11) . ? C20 C21 1.346(12) . ? C20 C24 1.389(13) . ? C21 C22 1.391(13) . ? C21 H21A 0.9300 . ? C22 N8 1.329(12) . ? C22 H22A 0.9300 . ? C23 N8 1.309(14) . ? C23 C24 1.366(15) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? N2 N3 1.368(9) . ? N3 H3B 0.8600 . ? N4 O2 1.324(9) . ? N6 N7 1.370(9) . ? N8 O4 1.325(9) . ? O4 Tb1 2.338(6) 3_655 ? C25 O5 1.204(14) . ? C25 N9 1.297(15) . ? C25 H25 0.9300 . ? C26 N9 1.45(2) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 N9 1.34(2) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 O6 1.177(16) . ? C28 N10 1.237(17) . ? C28 H28 0.9300 . ? C29 N10 1.382(17) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 N10 1.373(17) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? Cl1 O8 1.408(10) . ? Cl1 O7 1.419(9) . ? Cl1 O10 1.426(9) . ? Cl1 O9 1.454(9) . ? Cl2 O11 1.393(13) . ? Cl2 O14 1.404(15) . ? Cl2 O12 1.423(14) . ? Cl2 O13 1.437(13) . ? C39 O17 1.224(19) . ? C39 N13 1.275(19) . ? C39 C37 1.85(6) 2 ? C39 H39 0.9300 . ? C37 N13 1.441(19) . ? C37 C39 1.85(6) 2 ? C38 N13 1.443(19) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? N11 C32 1.17(3) . ? C32 C31 1.49(3) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C34 N12 1.416(19) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? N12 C36 1.314(19) . ? N12 C35 1.425(18) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 O16 1.245(19) . ? C36 H36A 0.9300 . ? 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 O4 Tb1 O4 109.9(4) 3_655 4 ? O4 Tb1 O2 69.4(2) 3_655 . ? O4 Tb1 O2 77.7(2) 4 . ? O4 Tb1 O2 77.7(2) 3_655 2_654 ? O4 Tb1 O2 69.4(2) 4 2_654 ? O2 Tb1 O2 121.0(3) . 2_654 ? O4 Tb1 O6 87.5(3) 3_655 . ? O4 Tb1 O6 146.9(2) 4 . ? O2 Tb1 O6 82.9(3) . . ? O2 Tb1 O6 143.5(2) 2_654 . ? O4 Tb1 O6 146.9(2) 3_655 2_654 ? O4 Tb1 O6 87.5(3) 4 2_654 ? O2 Tb1 O6 143.5(2) . 2_654 ? O2 Tb1 O6 82.9(3) 2_654 2_654 ? O6 Tb1 O6 92.6(4) . 2_654 ? O4 Tb1 O5 74.5(2) 3_655 . ? O4 Tb1 O5 137.8(2) 4 . ? O2 Tb1 O5 137.1(2) . . ? O2 Tb1 O5 71.0(2) 2_654 . ? O6 Tb1 O5 73.0(2) . . ? O6 Tb1 O5 73.9(2) 2_654 . ? O4 Tb1 O5 137.8(2) 3_655 2_654 ? O4 Tb1 O5 74.5(2) 4 2_654 ? O2 Tb1 O5 71.0(2) . 2_654 ? O2 Tb1 O5 137.1(2) 2_654 2_654 ? O6 Tb1 O5 73.9(2) . 2_654 ? O6 Tb1 O5 73.0(2) 2_654 2_654 ? O5 Tb1 O5 131.3(3) . 2_654 ? N2 Ni1 N6 175.7(2) . . ? N2 Ni1 O3 102.8(3) . . ? N6 Ni1 O3 77.0(2) . . ? N2 Ni1 N1 78.9(2) . . ? N6 Ni1 N1 96.8(2) . . ? O3 Ni1 N1 88.9(3) . . ? N2 Ni1 O1 76.1(2) . . ? N6 Ni1 O1 108.2(2) . . ? O3 Ni1 O1 93.9(2) . . ? N1 Ni1 O1 154.9(2) . . ? N2 Ni1 N5 101.9(3) . . ? N6 Ni1 N5 78.5(2) . . ? O3 Ni1 N5 155.3(2) . . ? N1 Ni1 N5 96.8(3) . . ? O1 Ni1 N5 90.9(2) . . ? N1 C1 C2 123.1(8) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C3 C2 C1 118.5(8) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C2 C3 C4 122.1(8) . . ? C2 C3 H3A 119.0 . . ? C4 C3 H3A 119.0 . . ? C3 C4 C5 118.3(9) . . ? C3 C4 H4A 120.9 . . ? C5 C4 H4A 120.9 . . ? C4 C5 N1 121.9(8) . . ? C4 C5 C6 124.2(8) . . ? N1 C5 C6 113.6(7) . . ? N2 C6 C5 115.4(8) . . ? N2 C6 H6A 122.3 . . ? C5 C6 H6A 122.3 . . ? O1 C7 N3 125.7(7) . . ? O1 C7 C8 118.3(7) . . ? N3 C7 C8 116.0(7) . . ? C12 C8 C9 116.6(8) . . ? C12 C8 C7 121.9(7) . . ? C9 C8 C7 121.5(8) . . ? C10 C9 C8 121.6(10) . . ? C10 C9 H9A 119.2 . . ? C8 C9 H9A 119.2 . . ? N4 C10 C9 119.8(9) . . ? N4 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? C12 C11 N4 118.8(8) . . ? C12 C11 H11A 120.6 . . ? N4 C11 H11A 120.6 . . ? C11 C12 C8 122.1(8) . . ? C11 C12 H12A 118.9 . . ? C8 C12 H12A 118.9 . . ? N5 C13 C14 123.5(9) . . ? N5 C13 H13A 118.2 . . ? C14 C13 H13A 118.2 . . ? C13 C14 C15 118.4(9) . . ? C13 C14 H14A 120.8 . . ? C15 C14 H14A 120.8 . . ? C16 C15 C14 119.3(9) . . ? C16 C15 H15A 120.4 . . ? C14 C15 H15A 120.4 . . ? C15 C16 C17 118.6(8) . . ? C15 C16 H16A 120.7 . . ? C17 C16 H16A 120.7 . . ? N5 C17 C16 121.8(7) . . ? N5 C17 C18 115.7(7) . . ? C16 C17 C18 122.5(7) . . ? N6 C18 C17 114.7(7) . . ? N6 C18 H18A 122.6 . . ? C17 C18 H18A 122.6 . . ? O3 C19 N7 127.0(7) . . ? O3 C19 C20 117.6(7) . . ? N7 C19 C20 115.4(7) . . ? C21 C20 C24 117.1(9) . . ? C21 C20 C19 123.5(7) . . ? C24 C20 C19 119.4(9) . . ? C20 C21 C22 120.6(9) . . ? C20 C21 H21A 119.7 . . ? C22 C21 H21A 119.7 . . ? N8 C22 C21 119.7(10) . . ? N8 C22 H22A 120.1 . . ? C21 C22 H22A 120.1 . . ? N8 C23 C24 119.9(10) . . ? N8 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C23 C24 C20 121.0(10) . . ? C23 C24 H24A 119.5 . . ? C20 C24 H24A 119.5 . . ? C1 N1 C5 116.1(7) . . ? C1 N1 Ni1 131.1(6) . . ? C5 N1 Ni1 112.6(5) . . ? C6 N2 N3 121.2(7) . . ? C6 N2 Ni1 119.3(6) . . ? N3 N2 Ni1 119.5(5) . . ? C7 N3 N2 108.8(6) . . ? C7 N3 H3B 125.6 . . ? N2 N3 H3B 125.6 . . ? C10 N4 O2 119.9(8) . . ? C10 N4 C11 121.0(8) . . ? O2 N4 C11 119.2(8) . . ? C13 N5 C17 118.4(7) . . ? C13 N5 Ni1 129.5(6) . . ? C17 N5 Ni1 112.0(5) . . ? C18 N6 N7 122.5(6) . . ? C18 N6 Ni1 118.9(5) . . ? N7 N6 Ni1 118.1(4) . . ? C19 N7 N6 108.2(6) . . ? C23 N8 O4 117.8(8) . . ? C23 N8 C22 121.5(8) . . ? O4 N8 C22 120.5(8) . . ? C7 O1 Ni1 109.8(5) . . ? N4 O2 Tb1 132.0(5) . . ? C19 O3 Ni1 109.0(5) . . ? N8 O4 Tb1 129.6(5) . 3_655 ? O5 C25 N9 128.7(15) . . ? O5 C25 H25 115.7 . . ? N9 C25 H25 115.7 . . ? N9 C26 H26A 109.5 . . ? N9 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N9 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N9 C27 H27A 109.5 . . ? N9 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N9 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O6 C28 N10 140(2) . . ? O6 C28 H28 110.0 . . ? N10 C28 H28 110.0 . . ? N10 C29 H29A 109.5 . . ? N10 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N10 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N10 C30 H30A 109.5 . . ? N10 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N10 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C25 N9 C27 127.5(19) . . ? C25 N9 C26 116.1(15) . . ? C27 N9 C26 115.7(15) . . ? C28 N10 C30 118(2) . . ? C28 N10 C29 106(2) . . ? C30 N10 C29 122.2(17) . . ? C25 O5 Tb1 130.5(7) . . ? C28 O6 Tb1 139.4(11) . . ? O8 Cl1 O7 113.6(9) . . ? O8 Cl1 O10 110.7(7) . . ? O7 Cl1 O10 112.8(8) . . ? O8 Cl1 O9 106.4(9) . . ? O7 Cl1 O9 106.4(7) . . ? O10 Cl1 O9 106.3(7) . . ? O11 Cl2 O14 113.4(12) . . ? O11 Cl2 O12 108.3(15) . . ? O14 Cl2 O12 107.5(11) . . ? O11 Cl2 O13 107.5(11) . . ? O14 Cl2 O13 110.9(14) . . ? O12 Cl2 O13 109.2(11) . . ? O17 C39 N13 141(4) . . ? O17 C39 C37 105(3) . 2 ? N13 C39 C37 114(3) . 2 ? O17 C39 H39 109.5 . . ? N13 C39 H39 109.5 . . ? C37 C39 H39 12.1 2 . ? N13 C37 C39 94(3) . 2 ? N13 C38 H38A 109.5 . . ? N13 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N13 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C39 N13 C37 112(3) . . ? C39 N13 C38 140(3) . . ? C37 N13 C38 105.3(16) . . ? N11 C32 C31 155(3) . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N12 C34 H34A 109.5 . . ? N12 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N12 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 N12 C34 129(2) . . ? C36 N12 C35 119(3) . . ? C34 N12 C35 111.4(18) . . ? N12 C35 H35A 109.5 . . ? N12 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N12 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O16 C36 N12 123(3) . . ? O16 C36 H36A 118.7 . . ? N12 C36 H36A 118.7 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.419 _refine_diff_density_min -0.792 _refine_diff_density_rms 0.125 #===END # Crystallographic Data of Complex 4 data_DyNi _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H92 Cl3 Dy N25 Ni2 O25' _chemical_formula_weight 2190.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Dy' 'Dy' -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6146(4) _cell_length_b 13.8847(5) _cell_length_c 30.3707(12) _cell_angle_alpha 91.9936(18) _cell_angle_beta 91.837(2) _cell_angle_gamma 91.4112(12) _cell_volume 5311.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 49192 _cell_measurement_theta_min 3.40 _cell_measurement_theta_max 25.05 _exptl_crystal_description 'block' _exptl_crystal_colour 'brownish red' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 1.199 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.667 _exptl_absorpt_correction_T_max 0.936 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49192 _diffrn_reflns_av_R_equivalents 0.0891 _diffrn_reflns_av_sigmaI/netI 0.0989 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 25.05 _reflns_number_total 17658 _reflns_number_gt 11346 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1667P)^2^+35.1770P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17658 _refine_ls_number_parameters 1109 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1696 _refine_ls_R_factor_gt 0.1160 _refine_ls_wR_factor_ref 0.3362 _refine_ls_wR_factor_gt 0.3012 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 1.22887(6) 1.00696(4) 1.255332(18) 0.0561(3) Uani 1 1 d . . . Ni1 Ni 0.79651(13) 1.36681(10) 1.47550(5) 0.0483(4) Uani 1 1 d . . . Ni2 Ni 0.80857(13) 0.63411(11) 1.01902(5) 0.0525(4) Uani 1 1 d . . . C1 C 0.7960(11) 1.5533(11) 1.4212(4) 0.064(4) Uani 1 1 d . . . H1A H 0.7641 1.5159 1.3982 0.076 Uiso 1 1 calc R . . C2 C 0.8172(13) 1.6512(11) 1.4150(5) 0.077(4) Uani 1 1 d . . . H2A H 0.8028 1.6782 1.3879 0.093 Uiso 1 1 calc R . . C3 C 0.8598(12) 1.7067(10) 1.4498(5) 0.071(4) Uani 1 1 d . . . H3A H 0.8711 1.7726 1.4470 0.085 Uiso 1 1 calc R . . C4 C 0.8861(11) 1.6637(9) 1.4893(5) 0.061(3) Uani 1 1 d . . . H4A H 0.9165 1.7001 1.5129 0.073 Uiso 1 1 calc R . . C5 C 0.8660(10) 1.5655(8) 1.4928(4) 0.048(3) Uani 1 1 d . . . C6 C 0.8925(10) 1.5145(9) 1.5314(4) 0.052(3) Uani 1 1 d . . . H6A H 0.9249 1.5446 1.5564 0.063 Uiso 1 1 calc R . . C7 C 0.8510(11) 1.2769(9) 1.5523(4) 0.054(3) Uani 1 1 d . . . C8 C 0.8652(12) 1.2017(9) 1.5875(4) 0.058(3) Uani 1 1 d . . . C9 C 0.9152(15) 1.2207(11) 1.6251(5) 0.089(6) Uani 1 1 d . . . H9A H 0.9477 1.2810 1.6304 0.107 Uiso 1 1 calc R . . C10 C 0.9208(17) 1.1503(11) 1.6582(5) 0.099(6) Uani 1 1 d . . . H10A H 0.9605 1.1623 1.6843 0.119 Uiso 1 1 calc R . . C11 C 0.8229(17) 1.0477(10) 1.6116(5) 0.096(6) Uani 1 1 d . . . H11A H 0.7937 0.9862 1.6057 0.115 Uiso 1 1 calc R . . C12 C 0.8186(15) 1.1124(10) 1.5810(5) 0.081(5) Uani 1 1 d . . . H12A H 0.7829 1.0970 1.5543 0.098 Uiso 1 1 calc R . . C13 C 0.6033(11) 1.4104(9) 1.5345(4) 0.058(3) Uani 1 1 d . . . H13A H 0.6528 1.4348 1.5556 0.069 Uiso 1 1 calc R . . C14 C 0.4957(14) 1.4077(10) 1.5439(5) 0.076(4) Uani 1 1 d . . . H14A H 0.4723 1.4288 1.5712 0.091 Uiso 1 1 calc R . . C15 C 0.4260(12) 1.3730(11) 1.5114(5) 0.072(4) Uani 1 1 d . . . H15A H 0.3539 1.3686 1.5170 0.086 Uiso 1 1 calc R . . C16 C 0.4607(13) 1.3445(11) 1.4708(5) 0.072(4) Uani 1 1 d . . . H16A H 0.4130 1.3248 1.4481 0.087 Uiso 1 1 calc R . . C17 C 0.5681(11) 1.3460(9) 1.4647(4) 0.055(3) Uani 1 1 d . . . C18 C 0.6131(12) 1.3131(10) 1.4236(4) 0.064(4) Uani 1 1 d . . . H18A H 0.5702 1.2942 1.3992 0.077 Uiso 1 1 calc R . . C19 C 0.8742(11) 1.2837(8) 1.3981(4) 0.054(3) Uani 1 1 d . . . C20 C 0.9446(12) 1.2458(8) 1.3635(4) 0.056(3) Uani 1 1 d . . . C21 C 0.9054(14) 1.1941(13) 1.3265(5) 0.087(5) Uani 1 1 d . . . H21A H 0.8326 1.1840 1.3226 0.105 Uiso 1 1 calc R . . C22 C 0.9704(15) 1.1581(14) 1.2961(6) 0.097(6) Uani 1 1 d . . . H22A H 0.9423 1.1211 1.2722 0.117 Uiso 1 1 calc R . . C23 C 1.1152(12) 1.2221(9) 1.3362(4) 0.060(4) Uani 1 1 d . . . H23A H 1.1883 1.2313 1.3395 0.072 Uiso 1 1 calc R . . C24 C 1.0546(12) 1.2554(8) 1.3674(4) 0.058(3) Uani 1 1 d . . . H24A H 1.0857 1.2860 1.3924 0.069 Uiso 1 1 calc R . . C25 C 0.6157(14) 0.5834(11) 0.9550(5) 0.075(4) Uani 1 1 d . . . H25A H 0.6633 0.5584 0.9351 0.090 Uiso 1 1 calc R . . C26 C 0.5032(16) 0.5871(12) 0.9433(6) 0.086(5) Uani 1 1 d . . . H26A H 0.4785 0.5685 0.9151 0.103 Uiso 1 1 calc R . . C27 C 0.4352(16) 0.6175(13) 0.9737(7) 0.094(6) Uani 1 1 d . . . H27A H 0.3629 0.6182 0.9669 0.113 Uiso 1 1 calc R . . C28 C 0.4726(15) 0.6468(12) 1.0138(6) 0.090(5) Uani 1 1 d . . . H28A H 0.4258 0.6689 1.0347 0.108 Uiso 1 1 calc R . . C29 C 0.5808(13) 0.6445(10) 1.0246(5) 0.067(4) Uani 1 1 d . . . C30 C 0.6229(14) 0.6809(12) 1.0656(5) 0.080(5) Uani 1 1 d . . . H30A H 0.5800 0.6999 1.0885 0.096 Uiso 1 1 calc R . . C31 C 0.8845(11) 0.7174(8) 1.0999(4) 0.049(3) Uani 1 1 d . . . C32 C 0.9484(14) 0.7569(9) 1.1377(4) 0.065(4) Uani 1 1 d . . . C33 C 1.0595(14) 0.7561(10) 1.1358(5) 0.071(4) Uani 1 1 d . . . H33A H 1.0919 0.7313 1.1109 0.086 Uiso 1 1 calc R . . C34 C 1.1207(14) 0.7937(10) 1.1722(5) 0.076(4) Uani 1 1 d . . . H34A H 1.1942 0.7944 1.1706 0.091 Uiso 1 1 calc R . . C35 C 0.977(2) 0.8279(12) 1.2102(5) 0.094(6) Uani 1 1 d . . . H35A H 0.9470 0.8534 1.2355 0.113 Uiso 1 1 calc R . . C36 C 0.9075(16) 0.7920(12) 1.1762(5) 0.086(5) Uani 1 1 d . . . H36A H 0.8346 0.7919 1.1797 0.103 Uiso 1 1 calc R . . C37 C 0.8127(12) 0.4520(11) 1.0759(5) 0.070(4) Uani 1 1 d . . . H37A H 0.7871 0.4905 1.0986 0.084 Uiso 1 1 calc R . . C38 C 0.8312(14) 0.3568(12) 1.0829(6) 0.083(5) Uani 1 1 d . . . H38A H 0.8212 0.3320 1.1106 0.100 Uiso 1 1 calc R . . C39 C 0.8637(12) 0.2994(11) 1.0499(5) 0.069(4) Uani 1 1 d . . . H39A H 0.8752 0.2346 1.0544 0.083 Uiso 1 1 calc R . . C40 C 0.8801(12) 0.3370(9) 1.0094(5) 0.066(4) Uani 1 1 d . . . H40A H 0.9012 0.2979 0.9859 0.079 Uiso 1 1 calc R . . C41 C 0.8642(11) 0.4361(9) 1.0041(4) 0.058(3) Uani 1 1 d . . . C42 C 0.8883(10) 0.4856(9) 0.9637(4) 0.052(3) Uani 1 1 d . . . H42A H 0.9123 0.4536 0.9386 0.062 Uiso 1 1 calc R . . C43 C 0.8599(11) 0.7201(9) 0.9416(4) 0.055(3) Uani 1 1 d . . . C44 C 0.8721(10) 0.7915(9) 0.9061(4) 0.051(3) Uani 1 1 d . . . C45 C 0.9109(12) 0.7687(10) 0.8663(4) 0.068(4) Uani 1 1 d . . . H45A H 0.9380 0.7078 0.8611 0.082 Uiso 1 1 calc R . . C46 C 0.9109(15) 0.8348(11) 0.8330(4) 0.083(5) Uani 1 1 d . . . H46A H 0.9345 0.8166 0.8053 0.099 Uiso 1 1 calc R . . C47 C 0.8409(14) 0.9507(10) 0.8794(4) 0.075(4) Uani 1 1 d . . . H47A H 0.8177 1.0132 0.8841 0.090 Uiso 1 1 calc R . . C48 C 0.8374(14) 0.8853(10) 0.9130(5) 0.073(4) Uani 1 1 d . . . H48A H 0.8118 0.9042 0.9403 0.088 Uiso 1 1 calc R . . C49 C 1.3309(15) 1.2184(11) 1.2262(6) 0.087(5) Uani 1 1 d . . . H49A H 1.3185 1.2368 1.2553 0.104 Uiso 1 1 calc R . . C50 C 1.399(2) 1.2578(17) 1.1567(7) 0.136(9) Uani 1 1 d . . . H50A H 1.3721 1.1942 1.1486 0.203 Uiso 1 1 calc R . . H50B H 1.4748 1.2599 1.1543 0.203 Uiso 1 1 calc R . . H50C H 1.3682 1.3034 1.1373 0.203 Uiso 1 1 calc R . . C51 C 1.406(3) 1.3775(18) 1.2173(9) 0.197(16) Uani 1 1 d . . . H51A H 1.3835 1.3868 1.2471 0.295 Uiso 1 1 calc R . . H51B H 1.3740 1.4248 1.1991 0.295 Uiso 1 1 calc R . . H51C H 1.4816 1.3841 1.2167 0.295 Uiso 1 1 calc R . . C52 C 1.3346(19) 0.8028(14) 1.2873(6) 0.107(6) Uani 1 1 d . . . H52 H 1.3144 0.7838 1.2585 0.128 Uiso 1 1 calc R . . C53 C 1.415(3) 0.765(3) 1.3546(8) 0.217(19) Uani 1 1 d . . . H53A H 1.3944 0.8293 1.3621 0.325 Uiso 1 1 calc R . . H53B H 1.4912 0.7614 1.3574 0.325 Uiso 1 1 calc R . . H53C H 1.3832 0.7207 1.3741 0.325 Uiso 1 1 calc R . . C54 C 1.406(3) 0.6423(19) 1.2922(10) 0.215(18) Uani 1 1 d . . . H54A H 1.3771 0.6346 1.2626 0.323 Uiso 1 1 calc R . . H54B H 1.3749 0.5943 1.3102 0.323 Uiso 1 1 calc R . . H54C H 1.4815 0.6349 1.2920 0.323 Uiso 1 1 calc R . . C55 C 1.427(3) 1.071(2) 1.3267(11) 0.23(2) Uani 1 1 d . . . H55 H 1.3961 1.0427 1.3506 0.276 Uiso 1 1 calc R . . C56 C 1.583(2) 1.0657(19) 1.3715(10) 0.182(14) Uani 1 1 d . . . H56A H 1.5436 1.0475 1.3966 0.273 Uiso 1 1 calc R . . H56B H 1.6217 1.1249 1.3784 0.273 Uiso 1 1 calc R . . H56C H 1.6315 1.0160 1.3641 0.273 Uiso 1 1 calc R . . C57 C 1.574(6) 1.114(9) 1.2966(16) 0.68(7) Uani 1 1 d . . . H57A H 1.5256 1.1229 1.2723 1.015 Uiso 1 1 calc R . . H57B H 1.6250 1.0664 1.2883 1.015 Uiso 1 1 calc R . . H57C H 1.6107 1.1734 1.3047 1.015 Uiso 1 1 calc R . . C58 C 1.407(3) 0.937(3) 1.1873(10) 0.197(18) Uani 1 1 d . . . H58 H 1.3734 0.9568 1.1615 0.237 Uiso 1 1 calc R . . C59 C 1.548(6) 0.837(7) 1.207(2) 0.53(7) Uani 1 1 d . . . H59A H 1.5049 0.8253 1.2312 0.790 Uiso 1 1 calc R . . H59B H 1.6192 0.8543 1.2169 0.790 Uiso 1 1 calc R . . H59C H 1.5498 0.7794 1.1880 0.790 Uiso 1 1 calc R . . C60 C 1.579(4) 0.940(4) 1.1410(16) 0.30(2) Uiso 1 1 d . . . H60A H 1.5477 0.9873 1.1228 0.452 Uiso 1 1 calc R . . H60B H 1.5882 0.8815 1.1237 0.452 Uiso 1 1 calc R . . H60C H 1.6466 0.9633 1.1527 0.452 Uiso 1 1 calc R . . N1 N 0.8196(8) 1.5129(7) 1.4582(3) 0.054(3) Uani 1 1 d . . . N2 N 0.8684(8) 1.4239(7) 1.5293(3) 0.051(2) Uani 1 1 d . . . N3 N 0.8879(9) 1.3647(7) 1.5643(3) 0.055(3) Uani 1 1 d . . . N4 N 0.8690(11) 1.0696(8) 1.6509(4) 0.073(3) Uani 1 1 d . . . N5 N 0.6338(10) 1.3800(8) 1.4975(4) 0.074(4) Uani 1 1 d . . . N6 N 0.7150(10) 1.3113(8) 1.4225(3) 0.062(3) Uani 1 1 d . . . N7 N 0.7695(9) 1.2749(7) 1.3880(3) 0.057(3) Uani 1 1 d . . . N8 N 1.0747(11) 1.1752(7) 1.3000(3) 0.064(3) Uani 1 1 d . . . N9 N 0.6480(10) 0.6156(8) 0.9938(4) 0.069(3) Uani 1 1 d . . . N10 N 0.7281(10) 0.6860(8) 1.0692(4) 0.065(3) Uani 1 1 d . . . N11 N 0.7811(11) 0.7214(8) 1.1065(3) 0.069(3) Uani 1 1 d . . . N12 N 1.0789(13) 0.8280(8) 1.2087(4) 0.071(4) Uani 1 1 d . . . N13 N 0.8303(8) 0.4900(7) 1.0376(3) 0.052(3) Uani 1 1 d . . . N14 N 0.8738(8) 0.5752(7) 0.9657(3) 0.053(3) Uani 1 1 d . . . N15 N 0.8865(8) 0.6344(7) 0.9301(3) 0.052(3) Uani 1 1 d . . . N16 N 0.8778(11) 0.9230(8) 0.8402(3) 0.066(3) Uani 1 1 d . . . N17 N 1.513(2) 1.0784(14) 1.3359(9) 0.166(11) Uani 1 1 d . . . N18 N 1.3819(16) 0.7405(13) 1.3104(6) 0.129(6) Uani 1 1 d . . . N19 N 1.5033(19) 0.9178(15) 1.1804(8) 0.146(9) Uani 1 1 d . . . N20 N 1.3725(14) 1.2816(11) 1.2008(5) 0.110(6) Uani 1 1 d . . . O1 O 0.8115(8) 1.2479(6) 1.5152(2) 0.061(2) Uani 1 1 d . . . O2 O 0.8708(10) 1.0041(7) 1.6817(3) 0.083(3) Uani 1 1 d . . . O3 O 0.9155(7) 1.3218(6) 1.4334(3) 0.054(2) Uani 1 1 d . . . O4 O 1.1354(9) 1.1475(6) 1.2677(3) 0.074(3) Uani 1 1 d . . . O5 O 0.9251(7) 0.6849(6) 1.0660(2) 0.055(2) Uani 1 1 d . . . O6 O 1.1340(10) 0.8613(7) 1.2425(3) 0.084(3) Uani 1 1 d . . . O7 O 0.8291(7) 0.7498(6) 0.9785(3) 0.058(2) Uani 1 1 d . . . O8 O 0.8775(9) 0.9877(6) 0.8092(3) 0.070(3) Uani 1 1 d . . . O9 O 1.3068(8) 1.1344(7) 1.2132(3) 0.067(3) Uani 1 1 d . . . O10 O 1.3138(8) 0.8836(8) 1.2991(3) 0.073(3) Uani 1 1 d . . . O11 O 1.3593(11) 1.0813(8) 1.3022(4) 0.105(4) Uani 1 1 d . . . O12 O 1.3579(12) 0.9364(9) 1.2109(5) 0.108(5) Uani 1 1 d . . . Cl1 Cl 1.6612(5) 1.6029(4) 0.63946(16) 0.1023(15) Uani 1 1 d D . . O13 O 1.6190(12) 1.6976(9) 0.6420(5) 0.153(6) Uani 1 1 d D . . O14 O 1.7346(11) 1.5968(13) 0.6053(4) 0.153(7) Uani 1 1 d D . . O15 O 1.5793(12) 1.5359(10) 0.6303(4) 0.151(7) Uani 1 1 d D . . O16 O 1.7123(15) 1.5911(12) 0.6810(4) 0.179(8) Uani 1 1 d D . . Cl2 Cl 0.6467(5) 0.3668(4) 0.85993(18) 0.1121(16) Uani 1 1 d D . . O17 O 0.5684(19) 0.4357(16) 0.8646(7) 0.258(15) Uani 1 1 d D . . O18 O 0.6784(14) 0.3514(14) 0.8170(4) 0.171(7) Uani 1 1 d D . . O19 O 0.600(2) 0.2765(16) 0.8737(8) 0.555(18) Uani 1 1 d D . . O20 O 0.7321(13) 0.3879(19) 0.8895(6) 0.249(15) Uani 1 1 d D . . Cl3 Cl 1.2125(10) 1.1328(9) 1.6800(3) 0.203(4) Uani 1 1 d D . . O21 O 1.184(3) 1.109(3) 1.6345(6) 0.56(5) Uani 1 1 d D . . O22 O 1.190(2) 1.0547(17) 1.7056(10) 0.37(3) Uani 1 1 d D . . O23 O 1.144(2) 1.2119(16) 1.6916(10) 0.274(17) Uani 1 1 d D . . O24 O 1.3168(15) 1.166(2) 1.6820(12) 0.38(3) Uani 1 1 d D . . C67 C 1.277(3) 0.825(2) 0.8146(10) 0.37(5) Uani 1 1 d G . . H67A H 1.3156 0.7765 0.8017 0.447 Uiso 1 1 calc R . . C68 C 1.218(3) 0.886(2) 0.7884(8) 1.03(16) Uani 1 1 d G . . H68A H 1.2178 0.8778 0.7578 1.231 Uiso 1 1 calc R . . C69 C 1.160(2) 0.959(2) 0.8077(12) 0.44(7) Uani 1 1 d G . . H69A H 1.1206 0.9994 0.7902 0.530 Uiso 1 1 calc R . . C70 C 1.160(2) 0.971(2) 0.8534(12) 0.58(10) Uani 1 1 d G . . H70A H 1.1211 1.0197 0.8663 0.698 Uiso 1 1 calc R . . C71 C 1.219(2) 0.910(2) 0.8796(8) 0.29(3) Uani 1 1 d G . . H71A H 1.2190 0.9184 0.9102 0.345 Uiso 1 1 calc R . . C72 C 1.277(2) 0.8374(18) 0.8603(9) 0.23(2) Uani 1 1 d G . . H72A H 1.3162 0.7968 0.8778 0.273 Uiso 1 1 calc R . . C61 C 0.8561(17) 1.551(2) 1.7932(9) 0.152(18) Uiso 0.50 1 d PG . . H61A H 0.7829 1.5411 1.7912 0.182 Uiso 0.50 1 calc PR . . C62 C 0.905(2) 1.6188(18) 1.7674(8) 0.097(11) Uiso 0.50 1 d PG . . H62A H 0.8639 1.6544 1.7480 0.117 Uiso 0.50 1 calc PR . . C63 C 1.014(2) 1.6335(18) 1.7704(9) 0.130(15) Uiso 0.50 1 d PG . . H63A H 1.0465 1.6789 1.7531 0.156 Uiso 0.50 1 calc PR . . C64 C 1.0749(17) 1.580(2) 1.7992(10) 0.146(18) Uiso 0.50 1 d PG . . H64A H 1.1481 1.5902 1.8012 0.175 Uiso 0.50 1 calc PR . . C65 C 1.026(2) 1.5125(18) 1.8250(8) 0.108(12) Uiso 0.50 1 d PG . . H65A H 1.0671 1.4769 1.8443 0.130 Uiso 0.50 1 calc PR . . C66 C 0.917(2) 1.4978(17) 1.8220(8) 0.092(10) Uiso 0.50 1 d PG . . H66A H 0.8845 1.4524 1.8393 0.110 Uiso 0.50 1 calc PR . . N22 N 0.887(2) 1.0537(18) 1.4413(8) 0.168(8) Uiso 1 1 d . . . C76 C 1.0693(17) 1.1035(14) 1.4714(6) 0.101(6) Uiso 1 1 d . . . H76A H 1.0783 1.1700 1.4808 0.151 Uiso 1 1 calc R . . H76B H 1.1160 1.0895 1.4478 0.151 Uiso 1 1 calc R . . H76C H 1.0857 1.0634 1.4957 0.151 Uiso 1 1 calc R . . C75 C 1.379(4) 1.157(4) 1.5627(16) 0.29(2) Uiso 1 1 d . . . H75A H 1.4392 1.1586 1.5831 0.435 Uiso 1 1 calc R . . H75B H 1.3267 1.1117 1.5721 0.435 Uiso 1 1 calc R . . H75C H 1.3498 1.2199 1.5617 0.435 Uiso 1 1 calc R . . C80 C 0.347(3) 0.488(3) 0.8226(11) 0.179(12) Uiso 1 1 d . . . N23 N 0.350(3) 0.572(3) 0.8376(11) 0.228(13) Uiso 1 1 d . . . C79 C 0.357(3) 0.385(3) 0.8054(12) 0.217(15) Uiso 1 1 d . . . H79A H 0.3044 0.3714 0.7825 0.325 Uiso 1 1 calc R . . H79B H 0.3470 0.3421 0.8290 0.325 Uiso 1 1 calc R . . H79C H 0.4265 0.3770 0.7940 0.325 Uiso 1 1 calc R . . C74 C 1.529(2) 1.117(2) 1.5121(9) 0.155(9) Uiso 1 1 d . . . H74A H 1.5474 1.0998 1.4825 0.232 Uiso 1 1 calc R . . H74B H 1.5530 1.0690 1.5317 0.232 Uiso 1 1 calc R . . H74C H 1.5622 1.1783 1.5207 0.232 Uiso 1 1 calc R . . N21 N 1.417(2) 1.1244(17) 1.5142(8) 0.154(8) Uiso 1 1 d . . . C83 C 0.964(3) 1.501(2) 1.6559(9) 0.172(11) Uiso 1 1 d . . . H83A H 1.0324 1.5108 1.6438 0.257 Uiso 1 1 calc R . . H83B H 0.9398 1.5607 1.6683 0.257 Uiso 1 1 calc R . . H83C H 0.9145 1.4778 1.6329 0.257 Uiso 1 1 calc R . . O25 O 1.397(3) 1.095(2) 1.4358(11) 0.262(13) Uiso 1 1 d . . . C84 C 0.971(3) 1.425(2) 1.6925(11) 0.170(11) Uiso 1 1 d . . . C73 C 1.348(3) 1.114(2) 1.4745(11) 0.177(12) Uiso 1 1 d . . . H73 H 1.2748 1.1197 1.4757 0.212 Uiso 1 1 calc R . . N25 N 0.891(4) 1.386(3) 1.7166(14) 0.286(18) Uiso 1 1 d . . . N24 N 0.911(4) 0.952(3) 1.0365(15) 0.304(19) Uiso 1 1 d . . . C82 C 1.025(4) 0.913(3) 1.0250(14) 0.211(15) Uiso 1 1 d . . . C81 C 1.104(4) 0.921(3) 1.0057(14) 0.238(19) Uiso 1 1 d . . . H81A H 1.1515 0.8715 1.0139 0.356 Uiso 1 1 calc R . . H81B H 1.1370 0.9832 1.0127 0.356 Uiso 1 1 calc R . . H81C H 1.0880 0.9155 0.9746 0.356 Uiso 1 1 calc R . . C77 C 0.983(2) 1.0886(17) 1.4593(8) 0.123(7) 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 Dy1 0.0765(5) 0.0509(4) 0.0407(3) 0.0089(2) -0.0012(3) -0.0078(3) Ni1 0.0553(10) 0.0460(8) 0.0431(8) 0.0002(6) 0.0028(7) -0.0066(7) Ni2 0.0579(11) 0.0557(9) 0.0436(8) 0.0073(7) -0.0033(7) -0.0064(8) C1 0.055(9) 0.079(9) 0.058(8) 0.010(7) 0.005(6) 0.000(7) C2 0.083(12) 0.075(10) 0.077(10) 0.034(8) 0.017(8) -0.005(9) C3 0.069(10) 0.048(7) 0.096(11) 0.012(7) -0.001(8) 0.000(7) C4 0.057(9) 0.049(7) 0.078(9) 0.012(6) 0.010(7) -0.014(6) C5 0.049(8) 0.042(6) 0.052(7) 0.002(5) 0.012(5) 0.002(5) C6 0.059(8) 0.052(7) 0.046(6) -0.004(5) 0.005(5) -0.014(6) C7 0.074(9) 0.049(7) 0.040(6) 0.005(5) 0.008(6) 0.002(6) C8 0.085(10) 0.046(7) 0.044(6) 0.009(5) 0.006(6) -0.009(7) C9 0.132(15) 0.064(9) 0.071(9) 0.038(7) -0.020(9) -0.041(10) C10 0.161(18) 0.067(10) 0.067(9) 0.023(8) -0.022(10) -0.035(11) C11 0.18(2) 0.046(8) 0.058(9) 0.002(7) 0.018(10) -0.026(10) C12 0.124(15) 0.066(9) 0.053(8) 0.011(7) -0.005(8) -0.025(9) C13 0.053(9) 0.067(8) 0.052(7) -0.002(6) 0.007(6) -0.019(7) C14 0.087(13) 0.061(9) 0.080(10) -0.012(7) 0.024(9) -0.008(8) C15 0.047(9) 0.072(9) 0.097(11) -0.003(8) 0.013(8) -0.005(7) C16 0.066(11) 0.070(9) 0.081(10) -0.007(8) -0.001(8) -0.005(8) C17 0.052(9) 0.056(7) 0.058(7) 0.000(6) 0.010(6) 0.005(6) C18 0.052(10) 0.071(9) 0.068(9) -0.010(7) -0.004(7) -0.015(7) C19 0.066(9) 0.045(7) 0.049(7) -0.002(5) -0.004(6) -0.013(6) C20 0.076(10) 0.043(7) 0.048(7) 0.003(5) 0.008(6) -0.012(7) C21 0.075(11) 0.126(14) 0.058(8) -0.029(9) 0.005(8) -0.014(10) C22 0.080(13) 0.128(15) 0.080(11) -0.042(10) 0.017(9) -0.030(12) C23 0.083(10) 0.047(7) 0.052(7) 0.001(6) 0.024(7) -0.007(7) C24 0.088(11) 0.038(6) 0.048(7) -0.001(5) -0.002(7) 0.002(7) C25 0.093(12) 0.068(9) 0.063(9) 0.008(7) -0.012(8) -0.018(8) C26 0.092(14) 0.074(10) 0.089(12) 0.015(9) -0.026(10) -0.028(10) C27 0.082(14) 0.088(12) 0.111(15) 0.030(11) -0.027(12) -0.013(10) C28 0.084(13) 0.090(12) 0.095(12) 0.024(9) -0.016(10) -0.014(10) C29 0.064(10) 0.064(9) 0.073(9) 0.015(7) 0.003(8) -0.005(8) C30 0.078(13) 0.085(11) 0.079(10) 0.012(8) 0.018(9) -0.004(9) C31 0.051(9) 0.048(7) 0.048(7) 0.004(5) -0.003(6) 0.000(6) C32 0.103(13) 0.046(7) 0.045(7) 0.006(5) 0.007(7) -0.013(7) C33 0.094(13) 0.063(9) 0.057(8) 0.001(6) -0.007(8) -0.006(8) C34 0.094(12) 0.062(9) 0.070(9) -0.002(7) -0.016(8) -0.007(8) C35 0.16(2) 0.076(11) 0.043(8) -0.015(7) -0.013(10) -0.004(12) C36 0.109(14) 0.090(11) 0.059(9) -0.011(8) -0.008(9) 0.013(10) C37 0.063(10) 0.083(10) 0.062(8) 0.017(7) -0.010(7) -0.013(8) C38 0.083(12) 0.077(11) 0.091(11) 0.043(9) -0.014(9) 0.006(9) C39 0.069(10) 0.061(8) 0.077(10) 0.019(8) -0.007(8) 0.002(7) C40 0.076(10) 0.043(7) 0.079(9) 0.008(6) 0.000(7) -0.003(7) C41 0.058(9) 0.058(8) 0.057(7) 0.002(6) -0.010(6) -0.009(7) C42 0.053(8) 0.046(7) 0.057(7) 0.009(5) 0.000(6) 0.001(6) C43 0.067(9) 0.052(8) 0.046(7) 0.000(6) -0.001(6) -0.002(6) C44 0.057(8) 0.058(8) 0.038(6) 0.011(5) -0.005(5) -0.008(6) C45 0.084(11) 0.063(8) 0.060(8) 0.018(6) -0.003(7) 0.021(8) C46 0.138(16) 0.067(10) 0.044(7) 0.009(7) 0.009(8) 0.001(10) C47 0.122(14) 0.051(8) 0.051(8) 0.005(6) -0.004(8) 0.004(8) C48 0.108(13) 0.050(8) 0.062(8) 0.007(6) 0.003(8) -0.003(8) C49 0.113(14) 0.059(9) 0.088(11) 0.024(8) 0.005(10) -0.016(9) C50 0.15(2) 0.16(2) 0.101(15) 0.055(14) 0.004(14) -0.053(17) C51 0.31(4) 0.13(2) 0.14(2) 0.043(17) 0.04(2) -0.11(2) C52 0.16(2) 0.078(12) 0.089(12) 0.023(10) -0.005(12) 0.017(13) C53 0.20(3) 0.36(5) 0.097(17) 0.08(2) 0.000(18) 0.14(3) C54 0.34(5) 0.12(2) 0.19(3) 0.07(2) 0.05(3) 0.09(3) C55 0.28(4) 0.16(2) 0.24(3) 0.13(2) -0.19(3) -0.16(3) C56 0.18(3) 0.13(2) 0.22(3) -0.03(2) -0.10(3) -0.011(19) C57 0.44(8) 1.4(2) 0.13(4) 0.09(8) -0.02(5) -0.513 C58 0.20(4) 0.27(4) 0.13(2) 0.03(2) 0.08(2) 0.17(3) C59 0.43(11) 0.70(16) 0.46(10) 0.27(11) -0.23(9) 0.09(10) N1 0.054(7) 0.057(6) 0.053(6) 0.008(5) 0.016(5) -0.004(5) N2 0.056(7) 0.052(6) 0.045(5) 0.003(4) 0.014(5) -0.003(5) N3 0.073(8) 0.045(6) 0.048(5) 0.012(4) 0.003(5) -0.006(5) N4 0.108(10) 0.057(7) 0.055(7) 0.020(5) 0.018(6) -0.007(7) N5 0.087(9) 0.073(8) 0.056(7) -0.016(6) -0.006(6) -0.034(7) N6 0.087(10) 0.063(7) 0.034(5) 0.011(5) -0.020(5) -0.017(6) N7 0.073(8) 0.059(6) 0.039(5) -0.001(5) 0.001(5) -0.010(6) N8 0.098(10) 0.043(6) 0.053(6) 0.005(5) 0.023(6) -0.009(6) N9 0.082(9) 0.058(7) 0.066(7) 0.016(6) -0.014(7) -0.008(6) N10 0.070(9) 0.061(7) 0.063(7) 0.011(5) -0.001(6) -0.004(6) N11 0.090(10) 0.070(7) 0.044(6) -0.009(5) -0.005(6) -0.002(7) N12 0.099(11) 0.054(7) 0.058(7) 0.009(5) -0.019(7) -0.023(7) N13 0.053(7) 0.055(6) 0.048(6) 0.016(5) -0.005(5) -0.007(5) N14 0.058(7) 0.055(6) 0.047(5) 0.015(5) -0.011(5) -0.012(5) N15 0.059(7) 0.053(6) 0.042(5) 0.002(4) -0.001(5) -0.007(5) N16 0.104(10) 0.053(7) 0.041(6) 0.004(5) -0.009(6) -0.006(6) N17 0.143(19) 0.105(14) 0.24(3) -0.005(15) -0.12(2) 0.000(13) N18 0.149(17) 0.110(13) 0.131(15) 0.055(11) -0.010(12) 0.039(12) N19 0.124(17) 0.116(14) 0.20(2) -0.033(14) 0.068(16) -0.040(13) N20 0.143(15) 0.097(11) 0.091(10) 0.031(8) 0.007(9) -0.052(10) O1 0.087(7) 0.056(5) 0.039(4) 0.006(4) 0.000(4) -0.013(5) O2 0.129(10) 0.064(6) 0.058(5) 0.026(5) 0.012(6) 0.002(6) O3 0.067(6) 0.048(5) 0.047(4) -0.003(4) -0.004(4) 0.001(4) O4 0.126(9) 0.050(5) 0.048(5) 0.006(4) 0.024(5) 0.005(5) O5 0.071(6) 0.055(5) 0.039(4) 0.003(4) -0.002(4) -0.010(4) O6 0.141(10) 0.059(6) 0.050(5) 0.011(4) -0.030(6) -0.029(6) O7 0.077(7) 0.048(5) 0.049(5) 0.010(4) 0.001(4) 0.000(4) O8 0.106(8) 0.056(5) 0.047(5) 0.017(4) -0.018(5) -0.010(5) O9 0.076(7) 0.069(6) 0.057(5) 0.022(4) 0.009(4) -0.008(5) O10 0.077(7) 0.068(7) 0.075(6) 0.015(5) -0.009(5) 0.013(5) O11 0.129(11) 0.080(7) 0.102(8) 0.026(6) -0.055(8) -0.039(7) O12 0.119(12) 0.092(8) 0.117(11) 0.017(7) 0.063(9) 0.018(8) Cl1 0.116(4) 0.100(3) 0.087(3) -0.005(2) -0.020(3) -0.029(3) O13 0.136(14) 0.127(13) 0.189(17) -0.060(12) -0.006(12) -0.003(11) O14 0.113(13) 0.213(19) 0.129(13) -0.050(12) -0.011(10) 0.016(12) O15 0.199(17) 0.133(12) 0.115(11) 0.008(9) -0.023(11) -0.082(12) O16 0.26(2) 0.146(14) 0.121(12) 0.020(10) -0.076(14) -0.035(14) Cl2 0.117(4) 0.118(4) 0.101(4) -0.006(3) 0.013(3) 0.007(3) O17 0.38(4) 0.19(2) 0.20(2) -0.067(18) -0.05(2) 0.14(3) O18 0.189(19) 0.217(19) 0.109(12) -0.030(12) 0.046(12) 0.025(15) O19 0.71(5) 0.55(4) 0.38(5) -0.23(3) 0.36(5) -0.521 O20 0.127(16) 0.43(4) 0.182(19) -0.10(2) 0.011(14) -0.09(2) Cl3 0.233(12) 0.218(10) 0.164(8) 0.041(7) 0.048(7) 0.006(9) O21 0.58(9) 1.01(14) 0.12(2) 0.15(4) 0.11(4) 0.34(9) O22 0.34(4) 0.25(3) 0.53(6) 0.26(4) -0.13(4) -0.12(3) O23 0.26(3) 0.18(2) 0.38(4) -0.03(2) 0.14(3) 0.03(2) O24 0.23(3) 0.36(4) 0.55(7) 0.15(4) 0.14(4) -0.16(3) C67 0.80(16) 0.23(5) 0.10(2) 0.06(3) -0.08(5) 0.02(6) C68 0.34(7) 1.6(3) 1.1(3) -1.0(3) 0.35(11) -0.555 C69 0.17(4) 0.90(18) 0.22(5) -0.26(8) 0.04(4) -0.24(7) C70 0.29(7) 0.32(7) 1.1(2) 0.46(12) -0.43(12) -0.21(6) C71 0.31(7) 0.18(4) 0.37(6) -0.03(4) 0.23(6) -0.09(4) C72 0.16(3) 0.12(3) 0.40(7) 0.11(3) 0.02(4) -0.01(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O2 2.328(10) 2_778 ? Dy1 O4 2.330(10) . ? Dy1 O11 2.336(11) . ? Dy1 O6 2.339(9) . ? Dy1 O8 2.345(8) 2_777 ? Dy1 O12 2.358(14) . ? Dy1 O9 2.425(8) . ? Dy1 O10 2.450(10) . ? Ni1 N2 1.976(10) . ? Ni1 N6 2.002(10) . ? Ni1 O1 2.088(8) . ? Ni1 O3 2.095(9) . ? Ni1 N1 2.128(10) . ? Ni1 N5 2.189(14) . ? Ni2 N10 1.983(12) . ? Ni2 N14 1.999(11) . ? Ni2 O7 2.073(8) . ? Ni2 O5 2.107(8) . ? Ni2 N13 2.120(10) . ? Ni2 N9 2.149(12) . ? C1 N1 1.305(16) . ? C1 C2 1.40(2) . ? C1 H1A 0.9300 . ? C2 C3 1.37(2) . ? C2 H2A 0.9300 . ? C3 C4 1.394(19) . ? C3 H3A 0.9300 . ? C4 C5 1.389(16) . ? C4 H4A 0.9300 . ? C5 N1 1.366(15) . ? C5 C6 1.425(17) . ? C6 N2 1.285(14) . ? C6 H6A 0.9300 . ? C7 O1 1.265(14) . ? C7 N3 1.329(15) . ? C7 C8 1.530(16) . ? C8 C9 1.301(19) . ? C8 C12 1.365(18) . ? C9 C10 1.428(19) . ? C9 H9A 0.9300 . ? C10 N4 1.293(18) . ? C10 H10A 0.9300 . ? C11 C12 1.32(2) . ? C11 N4 1.333(19) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 N5 1.260(16) . ? C13 C14 1.40(2) . ? C13 H13A 0.9300 . ? C14 C15 1.37(2) . ? C14 H14A 0.9300 . ? C15 C16 1.37(2) . ? C15 H15A 0.9300 . ? C16 C17 1.37(2) . ? C16 H16A 0.9300 . ? C17 N5 1.342(16) . ? C17 C18 1.452(18) . ? C18 N6 1.289(18) . ? C18 H18A 0.9300 . ? C19 O3 1.269(13) . ? C19 N7 1.348(17) . ? C19 C20 1.490(18) . ? C20 C24 1.39(2) . ? C20 C21 1.382(18) . ? C21 C22 1.35(2) . ? C21 H21A 0.9300 . ? C22 N8 1.33(2) . ? C22 H22A 0.9300 . ? C23 C24 1.313(18) . ? C23 N8 1.338(16) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 N9 1.296(17) . ? C25 C26 1.45(2) . ? C25 H25A 0.9300 . ? C26 C27 1.34(3) . ? C26 H26A 0.9300 . ? C27 C28 1.34(2) . ? C27 H27A 0.9300 . ? C28 C29 1.39(2) . ? C28 H28A 0.9300 . ? C29 N9 1.341(19) . ? C29 C30 1.41(2) . ? C30 N10 1.33(2) . ? C30 H30A 0.9300 . ? C31 O5 1.241(14) . ? C31 N11 1.328(17) . ? C31 C32 1.464(18) . ? C32 C36 1.37(2) . ? C32 C33 1.41(2) . ? C33 C34 1.407(19) . ? C33 H33A 0.9300 . ? C34 N12 1.320(19) . ? C34 H34A 0.9300 . ? C35 N12 1.29(2) . ? C35 C36 1.40(2) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C37 N13 1.318(16) . ? C37 C38 1.37(2) . ? C37 H37A 0.9300 . ? C38 C39 1.34(2) . ? C38 H38A 0.9300 . ? C39 C40 1.372(19) . ? C39 H39A 0.9300 . ? C40 C41 1.409(18) . ? C40 H40A 0.9300 . ? C41 N13 1.328(16) . ? C41 C42 1.465(17) . ? C42 N14 1.262(15) . ? C42 H42A 0.9300 . ? C43 O7 1.256(14) . ? C43 N15 1.284(16) . ? C43 C44 1.499(16) . ? C44 C45 1.348(18) . ? C44 C48 1.396(19) . ? C45 C46 1.390(18) . ? C45 H45A 0.9300 . ? C46 N16 1.316(18) . ? C46 H46A 0.9300 . ? C47 N16 1.339(17) . ? C47 C48 1.391(18) . ? C47 H47A 0.9300 . ? C48 H48A 0.9300 . ? C49 O9 1.246(17) . ? C49 N20 1.300(19) . ? C49 H49A 0.9300 . ? C50 N20 1.42(2) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 N20 1.45(3) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 O10 1.20(2) . ? C52 N18 1.28(2) . ? C52 H52 0.9300 . ? C53 N18 1.42(3) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 N18 1.50(3) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 N17 1.11(4) . ? C55 O11 1.13(3) . ? C55 H55 0.9300 . ? C56 N17 1.39(3) . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 N17 1.53(5) . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 O12 0.96(3) . ? C58 N19 1.27(3) . ? C58 H58 0.9300 . ? C59 N19 1.51(6) . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 N19 1.59(5) . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? N2 N3 1.384(13) . ? N4 O2 1.328(13) . ? N6 N7 1.362(15) . ? N8 O4 1.317(14) . ? N10 N11 1.368(15) . ? N12 O6 1.288(14) . ? N14 N15 1.392(13) . ? N16 O8 1.323(13) . ? O2 Dy1 2.328(10) 2_778 ? O8 Dy1 2.345(8) 2_777 ? Cl1 O15 1.388(11) . ? Cl1 O14 1.414(12) . ? Cl1 O16 1.414(11) . ? Cl1 O13 1.431(12) . ? Cl2 O18 1.386(11) . ? Cl2 O20 1.398(13) . ? Cl2 O17 1.400(14) . ? Cl2 O19 1.454(15) . ? Cl3 O24 1.382(16) . ? Cl3 O22 1.385(15) . ? Cl3 O21 1.440(17) . ? Cl3 O23 1.453(15) . ? C67 C68 1.3900 . ? C67 C72 1.3900 . ? C67 H67A 0.9300 . ? C68 C69 1.3900 . ? C68 H68A 0.9300 . ? C69 C70 1.3900 . ? C69 H69A 0.9300 . ? C70 C71 1.3900 . ? C70 H70A 0.9300 . ? C71 C72 1.3900 . ? C71 H71A 0.9300 . ? C72 H72A 0.9300 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C61 H61A 0.9300 . ? C62 C63 1.3900 . ? C62 H62A 0.9300 . ? C63 C64 1.3900 . ? C63 H63A 0.9300 . ? C64 C65 1.3900 . ? C64 H64A 0.9300 . ? C65 C66 1.3900 . ? C65 H65A 0.9300 . ? C66 H66A 0.9300 . ? N22 C77 1.38(3) . ? C76 C77 1.15(3) . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C75 N21 1.62(5) . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C80 N23 1.23(4) . ? C80 C79 1.51(4) . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? C74 N21 1.42(3) . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? N21 C73 1.47(4) . ? C83 C84 1.56(4) . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? O25 C73 1.36(4) . ? C84 N25 1.37(5) . ? C73 H73 0.9300 . ? N24 C82 1.60(6) . ? C82 C81 1.17(5) . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? 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 O2 Dy1 O4 69.3(3) 2_778 . ? O2 Dy1 O11 85.5(5) 2_778 . ? O4 Dy1 O11 84.9(5) . . ? O2 Dy1 O6 77.3(4) 2_778 . ? O4 Dy1 O6 118.8(4) . . ? O11 Dy1 O6 142.0(4) . . ? O2 Dy1 O8 112.5(4) 2_778 2_777 ? O4 Dy1 O8 78.1(3) . 2_777 ? O11 Dy1 O8 148.2(4) . 2_777 ? O6 Dy1 O8 69.5(3) . 2_777 ? O2 Dy1 O12 146.8(4) 2_778 . ? O4 Dy1 O12 143.4(4) . . ? O11 Dy1 O12 91.7(6) . . ? O6 Dy1 O12 85.1(5) . . ? O8 Dy1 O12 86.5(5) 2_777 . ? O2 Dy1 O9 137.0(3) 2_778 . ? O4 Dy1 O9 71.2(3) . . ? O11 Dy1 O9 74.5(4) . . ? O6 Dy1 O9 138.7(3) . . ? O8 Dy1 O9 74.6(3) 2_777 . ? O12 Dy1 O9 72.8(4) . . ? O2 Dy1 O10 74.6(4) 2_778 . ? O4 Dy1 O10 137.9(3) . . ? O11 Dy1 O10 71.2(4) . . ? O6 Dy1 O10 71.7(4) . . ? O8 Dy1 O10 137.3(3) 2_777 . ? O12 Dy1 O10 73.3(4) . . ? O9 Dy1 O10 130.2(4) . . ? N2 Ni1 N6 176.4(5) . . ? N2 Ni1 O1 77.6(4) . . ? N6 Ni1 O1 102.6(4) . . ? N2 Ni1 O3 107.0(4) . . ? N6 Ni1 O3 76.6(5) . . ? O1 Ni1 O3 93.4(3) . . ? N2 Ni1 N1 78.2(4) . . ? N6 Ni1 N1 101.7(4) . . ? O1 Ni1 N1 155.7(4) . . ? O3 Ni1 N1 91.5(4) . . ? N2 Ni1 N5 97.0(4) . . ? N6 Ni1 N5 79.5(5) . . ? O1 Ni1 N5 88.3(4) . . ? O3 Ni1 N5 155.8(4) . . ? N1 Ni1 N5 96.9(4) . . ? N10 Ni2 N14 173.4(5) . . ? N10 Ni2 O7 104.9(4) . . ? N14 Ni2 O7 76.5(4) . . ? N10 Ni2 O5 75.0(4) . . ? N14 Ni2 O5 111.5(4) . . ? O7 Ni2 O5 94.1(3) . . ? N10 Ni2 N13 101.2(4) . . ? N14 Ni2 N13 77.8(4) . . ? O7 Ni2 N13 153.9(4) . . ? O5 Ni2 N13 91.1(3) . . ? N10 Ni2 N9 78.6(5) . . ? N14 Ni2 N9 95.0(5) . . ? O7 Ni2 N9 89.4(4) . . ? O5 Ni2 N9 153.4(4) . . ? N13 Ni2 N9 97.3(4) . . ? N1 C1 C2 121.9(14) . . ? N1 C1 H1A 119.1 . . ? C2 C1 H1A 119.1 . . ? C3 C2 C1 118.6(13) . . ? C3 C2 H2A 120.7 . . ? C1 C2 H2A 120.7 . . ? C2 C3 C4 119.6(13) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 118.9(13) . . ? C5 C4 H4A 120.6 . . ? C3 C4 H4A 120.6 . . ? N1 C5 C4 120.2(11) . . ? N1 C5 C6 116.7(10) . . ? C4 C5 C6 123.1(11) . . ? N2 C6 C5 115.3(10) . . ? N2 C6 H6A 122.4 . . ? C5 C6 H6A 122.4 . . ? O1 C7 N3 128.1(11) . . ? O1 C7 C8 117.3(10) . . ? N3 C7 C8 114.5(10) . . ? C9 C8 C12 117.7(12) . . ? C9 C8 C7 122.8(11) . . ? C12 C8 C7 119.4(12) . . ? C8 C9 C10 121.0(13) . . ? C8 C9 H9A 119.5 . . ? C10 C9 H9A 119.5 . . ? N4 C10 C9 117.9(14) . . ? N4 C10 H10A 121.1 . . ? C9 C10 H10A 121.1 . . ? C12 C11 N4 120.4(13) . . ? C12 C11 H11A 119.8 . . ? N4 C11 H11A 119.8 . . ? C11 C12 C8 121.5(14) . . ? C11 C12 H12A 119.3 . . ? C8 C12 H12A 119.3 . . ? N5 C13 C14 120.5(13) . . ? N5 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C15 C14 C13 117.5(14) . . ? C15 C14 H14A 121.3 . . ? C13 C14 H14A 121.3 . . ? C14 C15 C16 120.9(15) . . ? C14 C15 H15A 119.5 . . ? C16 C15 H15A 119.5 . . ? C15 C16 C17 118.0(14) . . ? C15 C16 H16A 121.0 . . ? C17 C16 H16A 121.0 . . ? N5 C17 C16 119.1(13) . . ? N5 C17 C18 118.7(13) . . ? C16 C17 C18 122.2(13) . . ? N6 C18 C17 117.0(12) . . ? N6 C18 H18A 121.5 . . ? C17 C18 H18A 121.5 . . ? O3 C19 N7 126.0(12) . . ? O3 C19 C20 119.2(12) . . ? N7 C19 C20 114.8(10) . . ? C24 C20 C21 115.5(13) . . ? C24 C20 C19 122.2(11) . . ? C21 C20 C19 122.2(13) . . ? C22 C21 C20 121.5(16) . . ? C22 C21 H21A 119.2 . . ? C20 C21 H21A 119.2 . . ? N8 C22 C21 120.3(14) . . ? N8 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C24 C23 N8 121.9(14) . . ? C24 C23 H23A 119.0 . . ? N8 C23 H23A 119.0 . . ? C23 C24 C20 121.2(12) . . ? C23 C24 H24A 119.4 . . ? C20 C24 H24A 119.4 . . ? N9 C25 C26 118.4(16) . . ? N9 C25 H25A 120.8 . . ? C26 C25 H25A 120.8 . . ? C27 C26 C25 119.6(16) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C28 C27 C26 119.4(18) . . ? C28 C27 H27A 120.3 . . ? C26 C27 H27A 120.3 . . ? C27 C28 C29 120.9(19) . . ? C27 C28 H28A 119.6 . . ? C29 C28 H28A 119.6 . . ? N9 C29 C28 119.1(15) . . ? N9 C29 C30 118.7(14) . . ? C28 C29 C30 121.9(16) . . ? N10 C30 C29 115.3(14) . . ? N10 C30 H30A 122.4 . . ? C29 C30 H30A 122.4 . . ? O5 C31 N11 125.5(11) . . ? O5 C31 C32 122.2(13) . . ? N11 C31 C32 112.3(12) . . ? C36 C32 C33 116.7(14) . . ? C36 C32 C31 124.5(16) . . ? C33 C32 C31 118.7(13) . . ? C32 C33 C34 118.6(15) . . ? C32 C33 H33A 120.7 . . ? C34 C33 H33A 120.7 . . ? N12 C34 C33 123.2(17) . . ? N12 C34 H34A 118.4 . . ? C33 C34 H34A 118.4 . . ? N12 C35 C36 124.4(17) . . ? N12 C35 H35A 117.8 . . ? C36 C35 H35A 117.8 . . ? C32 C36 C35 119.4(19) . . ? C32 C36 H36A 120.3 . . ? C35 C36 H36A 120.3 . . ? N13 C37 C38 121.4(16) . . ? N13 C37 H37A 119.3 . . ? C38 C37 H37A 119.3 . . ? C39 C38 C37 120.0(15) . . ? C39 C38 H38A 120.0 . . ? C37 C38 H38A 120.0 . . ? C38 C39 C40 119.6(14) . . ? C38 C39 H39A 120.2 . . ? C40 C39 H39A 120.2 . . ? C39 C40 C41 118.5(14) . . ? C39 C40 H40A 120.7 . . ? C41 C40 H40A 120.7 . . ? N13 C41 C40 119.9(12) . . ? N13 C41 C42 116.9(11) . . ? C40 C41 C42 123.2(13) . . ? N14 C42 C41 114.4(12) . . ? N14 C42 H42A 122.8 . . ? C41 C42 H42A 122.8 . . ? O7 C43 N15 128.0(11) . . ? O7 C43 C44 118.4(11) . . ? N15 C43 C44 113.6(11) . . ? C45 C44 C48 117.3(11) . . ? C45 C44 C43 123.2(12) . . ? C48 C44 C43 119.4(11) . . ? C44 C45 C46 121.0(14) . . ? C44 C45 H45A 119.5 . . ? C46 C45 H45A 119.5 . . ? N16 C46 C45 120.7(13) . . ? N16 C46 H46A 119.6 . . ? C45 C46 H46A 119.6 . . ? N16 C47 C48 119.5(13) . . ? N16 C47 H47A 120.3 . . ? C48 C47 H47A 120.3 . . ? C47 C48 C44 120.4(13) . . ? C47 C48 H48A 119.8 . . ? C44 C48 H48A 119.8 . . ? O9 C49 N20 122.8(17) . . ? O9 C49 H49A 118.6 . . ? N20 C49 H49A 118.6 . . ? N20 C50 H50A 109.5 . . ? N20 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N20 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N20 C51 H51A 109.5 . . ? N20 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N20 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O10 C52 N18 126(2) . . ? O10 C52 H52 116.8 . . ? N18 C52 H52 116.8 . . ? N18 C53 H53A 109.5 . . ? N18 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N18 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N18 C54 H54A 109.5 . . ? N18 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N18 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N17 C55 O11 150(4) . . ? N17 C55 H55 105.1 . . ? O11 C55 H55 105.1 . . ? N17 C56 H56A 109.5 . . ? N17 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N17 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N17 C57 H57A 109.5 . . ? N17 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N17 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? O12 C58 N19 139(4) . . ? O12 C58 H58 110.4 . . ? N19 C58 H58 110.4 . . ? N19 C59 H59A 109.5 . . ? N19 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? N19 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N19 C60 H60A 109.5 . . ? N19 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? N19 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C1 N1 C5 120.8(11) . . ? C1 N1 Ni1 129.0(9) . . ? C5 N1 Ni1 110.2(7) . . ? C6 N2 N3 122.2(10) . . ? C6 N2 Ni1 119.5(8) . . ? N3 N2 Ni1 118.2(7) . . ? C7 N3 N2 107.5(9) . . ? C10 N4 O2 118.9(13) . . ? C10 N4 C11 121.0(12) . . ? O2 N4 C11 119.7(12) . . ? C13 N5 C17 123.9(14) . . ? C13 N5 Ni1 128.2(10) . . ? C17 N5 Ni1 107.8(9) . . ? C18 N6 N7 124.3(10) . . ? C18 N6 Ni1 116.8(10) . . ? N7 N6 Ni1 118.9(9) . . ? C19 N7 N6 108.5(10) . . ? O4 N8 C22 119.1(12) . . ? O4 N8 C23 121.5(13) . . ? C22 N8 C23 119.4(12) . . ? C25 N9 C29 122.4(14) . . ? C25 N9 Ni2 127.9(12) . . ? C29 N9 Ni2 109.7(9) . . ? C30 N10 N11 122.4(13) . . ? C30 N10 Ni2 117.6(10) . . ? N11 N10 Ni2 119.9(10) . . ? C31 N11 N10 108.1(11) . . ? O6 N12 C35 118.5(15) . . ? O6 N12 C34 123.9(16) . . ? C35 N12 C34 117.6(13) . . ? C37 N13 C41 120.6(12) . . ? C37 N13 Ni2 128.2(10) . . ? C41 N13 Ni2 111.1(8) . . ? C42 N14 N15 123.3(11) . . ? C42 N14 Ni2 119.3(8) . . ? N15 N14 Ni2 116.7(8) . . ? C43 N15 N14 108.6(10) . . ? C46 N16 O8 122.1(11) . . ? C46 N16 C47 121.1(11) . . ? O8 N16 C47 116.8(11) . . ? C55 N17 C56 141(4) . . ? C55 N17 C57 110(4) . . ? C56 N17 C57 110(4) . . ? C52 N18 C53 120(2) . . ? C52 N18 C54 122(2) . . ? C53 N18 C54 118(2) . . ? C58 N19 C59 116(4) . . ? C58 N19 C60 133(3) . . ? C59 N19 C60 109(4) . . ? C49 N20 C50 122.1(17) . . ? C49 N20 C51 121.8(17) . . ? C50 N20 C51 115.8(16) . . ? C7 O1 Ni1 108.2(7) . . ? N4 O2 Dy1 129.7(9) . 2_778 ? C19 O3 Ni1 110.1(8) . . ? N8 O4 Dy1 131.8(7) . . ? C31 O5 Ni2 111.4(8) . . ? N12 O6 Dy1 131.4(7) . . ? C43 O7 Ni2 109.6(8) . . ? N16 O8 Dy1 129.4(7) . 2_777 ? C49 O9 Dy1 127.7(9) . . ? C52 O10 Dy1 127.6(11) . . ? C55 O11 Dy1 146.5(16) . . ? C58 O12 Dy1 153(2) . . ? O15 Cl1 O14 108.8(8) . . ? O15 Cl1 O16 113.0(9) . . ? O14 Cl1 O16 110.8(10) . . ? O15 Cl1 O13 109.4(9) . . ? O14 Cl1 O13 109.9(10) . . ? O16 Cl1 O13 105.0(9) . . ? O18 Cl2 O20 112.6(10) . . ? O18 Cl2 O17 114.3(11) . . ? O20 Cl2 O17 110.4(11) . . ? O18 Cl2 O19 107.0(11) . . ? O20 Cl2 O19 105.9(13) . . ? O17 Cl2 O19 106.0(12) . . ? O24 Cl3 O22 115.4(14) . . ? O24 Cl3 O21 108.0(13) . . ? O22 Cl3 O21 110.0(15) . . ? O24 Cl3 O23 108.9(14) . . ? O22 Cl3 O23 109.9(14) . . ? O21 Cl3 O23 104.1(14) . . ? C68 C67 C72 120.0 . . ? C68 C67 H67A 120.0 . . ? C72 C67 H67A 120.0 . . ? C67 C68 C69 120.0 . . ? C67 C68 H68A 120.0 . . ? C69 C68 H68A 120.0 . . ? C68 C69 C70 120.0 . . ? C68 C69 H69A 120.0 . . ? C70 C69 H69A 120.0 . . ? C69 C70 C71 120.0 . . ? C69 C70 H70A 120.0 . . ? C71 C70 H70A 120.0 . . ? C72 C71 C70 120.0 . . ? C72 C71 H71A 120.0 . . ? C70 C71 H71A 120.0 . . ? C71 C72 C67 120.0 . . ? C71 C72 H72A 120.0 . . ? C67 C72 H72A 120.0 . . ? C62 C61 C66 120.00(5) . . ? C62 C61 H61A 120.0 . . ? C66 C61 H61A 120.0 . . ? C63 C62 C61 120.0 . . ? C63 C62 H62A 120.0 . . ? C61 C62 H62A 120.0 . . ? C62 C63 C64 120.0 . . ? C62 C63 H63A 120.0 . . ? C64 C63 H63A 120.0 . . ? C65 C64 C63 120.00(6) . . ? C65 C64 H64A 120.0 . . ? C63 C64 H64A 120.0 . . ? C64 C65 C66 120.0 . . ? C64 C65 H65A 120.0 . . ? C66 C65 H65A 120.0 . . ? C65 C66 C61 120.0 . . ? C65 C66 H66A 120.0 . . ? C61 C66 H66A 120.0 . . ? C77 C76 H76A 109.5 . . ? C77 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C77 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? N21 C75 H75A 109.5 . . ? N21 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? N21 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? N23 C80 C79 174(4) . . ? C80 C79 H79A 109.5 . . ? C80 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C80 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? N21 C74 H74A 109.5 . . ? N21 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? N21 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C74 N21 C73 122(3) . . ? C74 N21 C75 113(3) . . ? C73 N21 C75 125(3) . . ? C84 C83 H83A 109.5 . . ? C84 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C84 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? N25 C84 C83 129(4) . . ? O25 C73 N21 116(3) . . ? O25 C73 H73 121.9 . . ? N21 C73 H73 121.9 . . ? C81 C82 N24 149(5) . . ? C82 C81 H81A 109.5 . . ? C82 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C82 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C76 C77 N22 168(3) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 4.308 _refine_diff_density_min -1.519 _refine_diff_density_rms 0.170 #===END