# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c078 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H43 Cl2 Gd N4 Ni3 O15' _chemical_formula_weight 1164.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6729(7) _cell_length_b 10.7918(7) _cell_length_c 18.8925(13) _cell_angle_alpha 87.7800(10) _cell_angle_beta 75.7830(10) _cell_angle_gamma 87.9550(10) _cell_volume 2107.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9988 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 28.10 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.835 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1166 _exptl_absorpt_coefficient_mu 3.072 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5260 _exptl_absorpt_correction_T_max 0.7094 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27486 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_unetI/netI 0.0420 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9652 _reflns_number_gt 8685 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H atoms of the water were located from different map and refined with restraints in bond lengths and thermal parameters ; _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^)+(0.0441P)^2^+7.5348P] 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 9652 _refine_ls_number_parameters 552 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1086 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.13535(2) 0.492234(19) 0.215084(12) 0.01924(7) Uani 1 1 d . . . Ni1 Ni 0.20617(6) 0.78764(5) 0.14393(3) 0.01828(12) Uani 1 1 d . . . Ni2 Ni -0.05126(6) 0.77729(5) 0.24962(3) 0.02114(13) Uani 1 1 d . . . Ni3 Ni 0.20059(6) 0.72963(5) 0.30806(3) 0.01939(13) Uani 1 1 d . . . N1 N 0.3867(4) 0.8571(3) 0.1274(2) 0.0209(8) Uani 1 1 d . . . N2 N 0.2398(4) 0.6970(3) 0.0453(2) 0.0204(8) Uani 1 1 d . . . N3 N 0.3201(4) 0.8760(4) 0.3070(2) 0.0227(8) Uani 1 1 d . . . N4 N 0.0886(4) 0.7578(4) 0.4133(2) 0.0243(8) Uani 1 1 d . . . O1 O 0.2849(3) 0.6561(3) 0.20356(16) 0.0194(6) Uani 1 1 d . . . O2 O 0.0518(3) 0.6733(3) 0.16239(16) 0.0194(6) Uani 1 1 d . . . O3 O 0.1242(3) 0.8540(3) 0.24748(17) 0.0207(6) Uani 1 1 d . . . O4 O 0.0384(3) 0.6326(3) 0.30556(16) 0.0214(6) Uani 1 1 d . . . O5 O 0.1179(3) 0.9323(3) 0.10211(17) 0.0252(7) Uani 1 1 d . . . O6 O -0.0806(3) 0.9207(3) 0.17795(19) 0.0260(7) Uani 1 1 d . . . O7 O 0.3060(3) 0.6012(3) 0.35157(18) 0.0264(7) Uani 1 1 d . . . O8 O 0.2527(4) 0.4323(3) 0.30153(18) 0.0280(7) Uani 1 1 d . . . O9 O 0.3149(3) 0.3883(4) 0.1292(2) 0.0328(8) Uani 1 1 d . . . O10 O 0.1270(3) 0.4073(3) 0.10093(18) 0.0264(7) Uani 1 1 d . . . O11 O -0.0932(3) 0.4361(3) 0.23703(19) 0.0269(7) Uani 1 1 d . . . O12 O 0.0446(3) 0.2948(3) 0.2621(2) 0.0303(8) Uani 1 1 d . . . O13 O -0.1406(4) 0.8630(3) 0.3404(2) 0.0332(8) Uani 1 1 d . . . O14 O -0.3149(4) 0.7460(4) 0.3803(2) 0.0394(9) Uani 1 1 d . . . C1 C 0.4247(5) 0.9701(5) 0.1009(3) 0.0303(11) Uani 1 1 d . . . H1 H 0.3658 1.0247 0.0841 0.036 Uiso 1 1 calc R . . C2 C 0.5481(6) 1.0087(5) 0.0975(3) 0.0421(14) Uani 1 1 d . . . H2 H 0.5737 1.0889 0.0780 0.050 Uiso 1 1 calc R . . C3 C 0.6333(6) 0.9316(6) 0.1223(3) 0.0414(14) Uani 1 1 d . . . H3 H 0.7180 0.9578 0.1207 0.050 Uiso 1 1 calc R . . C4 C 0.5944(5) 0.8151(5) 0.1497(3) 0.0289(10) Uani 1 1 d . . . H4 H 0.6522 0.7597 0.1670 0.035 Uiso 1 1 calc R . . C5 C 0.4710(5) 0.7802(4) 0.1515(2) 0.0225(9) Uani 1 1 d . . . C6 C 0.4215(4) 0.6537(4) 0.1798(3) 0.0224(9) Uani 1 1 d . . . H6A H 0.4495 0.5932 0.1406 0.027 Uiso 1 1 calc R . . H6B H 0.4590 0.6264 0.2210 0.027 Uiso 1 1 calc R . . C7 C 0.3481(5) 0.6858(4) -0.0077(2) 0.0230(9) Uani 1 1 d . . . H7 H 0.4272 0.7090 0.0019 0.028 Uiso 1 1 calc R . . C8 C 0.3504(5) 0.6419(4) -0.0760(3) 0.0253(10) Uani 1 1 d . . . H8 H 0.4293 0.6331 -0.1122 0.030 Uiso 1 1 calc R . . C9 C 0.2339(5) 0.6111(4) -0.0900(3) 0.0258(10) Uani 1 1 d . . . H9 H 0.2312 0.5839 -0.1368 0.031 Uiso 1 1 calc R . . C10 C 0.1226(5) 0.6205(4) -0.0355(3) 0.0237(9) Uani 1 1 d . . . H10 H 0.0422 0.5989 -0.0440 0.028 Uiso 1 1 calc R . . C11 C 0.1286(4) 0.6620(4) 0.0324(2) 0.0202(9) Uani 1 1 d . . . C12 C 0.0109(4) 0.6682(4) 0.0967(2) 0.0223(9) Uani 1 1 d . . . H12A H -0.0430 0.7428 0.0911 0.027 Uiso 1 1 calc R . . H12B H -0.0419 0.5941 0.0982 0.027 Uiso 1 1 calc R . . C13 C 0.4342(5) 0.8759(5) 0.3250(3) 0.0291(11) Uani 1 1 d . . . H13 H 0.4695 0.7993 0.3388 0.035 Uiso 1 1 calc R . . C14 C 0.5027(6) 0.9830(5) 0.3241(4) 0.0423(14) Uani 1 1 d . . . H14 H 0.5834 0.9808 0.3370 0.051 Uiso 1 1 calc R . . C15 C 0.4497(6) 1.0926(5) 0.3037(4) 0.0473(16) Uani 1 1 d . . . H15 H 0.4950 1.1673 0.3018 0.057 Uiso 1 1 calc R . . C16 C 0.3309(6) 1.0956(5) 0.2859(3) 0.0358(12) Uani 1 1 d . . . H16A H 0.2930 1.1716 0.2732 0.043 Uiso 1 1 calc R . . C17 C 0.2691(5) 0.9836(4) 0.2874(2) 0.0241(10) Uani 1 1 d . . . C18 C 0.1411(5) 0.9758(4) 0.2667(3) 0.0242(10) Uani 1 1 d . . . H18A H 0.0695 1.0001 0.3085 0.029 Uiso 1 1 calc R . . H18B H 0.1396 1.0339 0.2250 0.029 Uiso 1 1 calc R . . C19 C 0.1114(5) 0.8345(5) 0.4633(3) 0.0274(10) Uani 1 1 d . . . H19 H 0.1757 0.8951 0.4482 0.033 Uiso 1 1 calc R . . C20 C 0.0438(6) 0.8276(5) 0.5362(3) 0.0325(11) Uani 1 1 d . . . H20 H 0.0611 0.8831 0.5703 0.039 Uiso 1 1 calc R . . C21 C -0.0487(6) 0.7389(5) 0.5584(3) 0.0347(12) Uani 1 1 d . . . H21 H -0.0949 0.7312 0.6081 0.042 Uiso 1 1 calc R . . C22 C -0.0732(5) 0.6612(5) 0.5068(3) 0.0310(11) Uani 1 1 d . . . H22 H -0.1373 0.6000 0.5206 0.037 Uiso 1 1 calc R . . C23 C -0.0022(5) 0.6741(4) 0.4344(3) 0.0265(10) Uani 1 1 d . . . C24 C -0.0271(5) 0.5913(4) 0.3765(2) 0.0262(10) Uani 1 1 d . . . H24A H 0.0021 0.5054 0.3855 0.031 Uiso 1 1 calc R . . H24B H -0.1212 0.5908 0.3799 0.031 Uiso 1 1 calc R . . C25 C 0.0030(5) 0.9710(4) 0.1277(3) 0.0256(10) Uani 1 1 d . . . C26 C -0.0351(6) 1.0914(5) 0.0937(3) 0.0361(12) Uani 1 1 d . . . H26A H -0.1267 1.1109 0.1150 0.054 Uiso 1 1 calc R . . H26B H -0.0209 1.0827 0.0409 0.054 Uiso 1 1 calc R . . H26C H 0.0176 1.1583 0.1033 0.054 Uiso 1 1 calc R . . C27 C 0.3186(5) 0.4876(4) 0.3368(3) 0.0294(11) Uani 1 1 d . . . C28 C 0.4213(9) 0.4126(6) 0.3631(5) 0.069(3) Uani 1 1 d . . . H28A H 0.3861 0.3331 0.3844 0.103 Uiso 1 1 calc R . . H28B H 0.4490 0.4585 0.4001 0.103 Uiso 1 1 calc R . . H28C H 0.4956 0.3974 0.3218 0.103 Uiso 1 1 calc R . . C29 C 0.2424(5) 0.3678(4) 0.0878(3) 0.0239(9) Uani 1 1 d . . . C30 C 0.2940(6) 0.2971(6) 0.0189(3) 0.0405(14) Uani 1 1 d . . . H30A H 0.2217 0.2644 0.0025 0.061 Uiso 1 1 calc R . . H30B H 0.3504 0.2282 0.0286 0.061 Uiso 1 1 calc R . . H30C H 0.3435 0.3527 -0.0192 0.061 Uiso 1 1 calc R . . C31 C -0.0681(5) 0.3261(5) 0.2575(3) 0.0271(10) Uani 1 1 d . . . C32 C -0.1751(5) 0.2347(5) 0.2777(3) 0.0360(12) Uani 1 1 d . . . H32A H -0.1380 0.1501 0.2742 0.054 Uiso 1 1 calc R . . H32B H -0.2319 0.2463 0.2442 0.054 Uiso 1 1 calc R . . H32C H -0.2251 0.2482 0.3279 0.054 Uiso 1 1 calc R . . C33 C -0.2401(5) 0.8280(5) 0.3878(3) 0.0338(12) Uani 1 1 d . . . C34 C -0.2680(7) 0.8921(7) 0.4604(4) 0.0511(16) Uani 1 1 d . . . H34A H -0.3296 0.9616 0.4600 0.077 Uiso 1 1 calc R . . H34B H -0.1874 0.9234 0.4681 0.077 Uiso 1 1 calc R . . H34C H -0.3049 0.8328 0.5000 0.077 Uiso 1 1 calc R . . C1S C 0.4088(6) 0.6748(6) 0.4887(3) 0.0402(13) Uani 1 1 d . . . H1S1 H 0.4996 0.6454 0.4708 0.048 Uiso 1 1 calc R . . H1S2 H 0.3729 0.6935 0.4457 0.048 Uiso 1 1 calc R . . Cl1 Cl 0.40364(17) 0.80982(15) 0.53846(10) 0.0528(4) Uani 1 1 d . . . Cl2 Cl 0.31842(17) 0.55743(17) 0.54419(10) 0.0548(4) Uani 1 1 d . . . O1W O -0.2115(3) 0.6742(3) 0.2485(2) 0.0289(7) Uani 1 1 d D . . H1W H -0.188(5) 0.5976(17) 0.246(3) 0.035 Uiso 1 1 d D . . H2W H -0.258(5) 0.684(4) 0.2917(13) 0.035 Uiso 1 1 d 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 Gd1 0.02462(12) 0.01621(11) 0.01779(11) 0.00045(8) -0.00713(8) -0.00021(8) Ni1 0.0230(3) 0.0167(3) 0.0164(3) 0.0023(2) -0.0074(2) -0.0027(2) Ni2 0.0231(3) 0.0158(3) 0.0274(3) 0.0006(2) -0.0122(2) 0.0002(2) Ni3 0.0278(3) 0.0156(3) 0.0152(3) 0.0004(2) -0.0066(2) 0.0010(2) N1 0.028(2) 0.0187(18) 0.0176(18) -0.0001(14) -0.0077(15) -0.0055(15) N2 0.0230(19) 0.0217(19) 0.0162(17) 0.0035(14) -0.0044(15) -0.0029(15) N3 0.032(2) 0.0202(19) 0.0177(18) -0.0035(14) -0.0089(16) 0.0013(16) N4 0.035(2) 0.0199(19) 0.0171(18) 0.0015(15) -0.0058(16) 0.0020(16) O1 0.0223(16) 0.0193(15) 0.0167(14) 0.0008(12) -0.0050(12) 0.0003(12) O2 0.0247(16) 0.0178(15) 0.0169(15) 0.0007(11) -0.0076(12) -0.0022(12) O3 0.0274(17) 0.0143(14) 0.0215(15) 0.0005(12) -0.0083(13) 0.0009(12) O4 0.0299(17) 0.0185(15) 0.0150(14) 0.0011(12) -0.0040(13) -0.0001(13) O5 0.0331(19) 0.0230(16) 0.0213(16) 0.0040(13) -0.0106(14) -0.0021(14) O6 0.0290(18) 0.0196(16) 0.0310(18) 0.0033(13) -0.0115(15) 0.0017(13) O7 0.040(2) 0.0210(16) 0.0216(16) -0.0023(13) -0.0144(15) 0.0055(14) O8 0.046(2) 0.0176(16) 0.0251(17) 0.0008(13) -0.0186(16) 0.0004(14) O9 0.0235(18) 0.045(2) 0.0323(19) -0.0109(16) -0.0100(15) 0.0007(15) O10 0.0264(18) 0.0302(18) 0.0239(17) -0.0058(14) -0.0083(14) 0.0035(14) O11 0.0281(18) 0.0218(17) 0.0299(18) -0.0034(13) -0.0048(14) -0.0009(13) O12 0.033(2) 0.0264(18) 0.0327(19) 0.0045(14) -0.0110(16) -0.0037(15) O13 0.034(2) 0.0305(19) 0.0332(19) -0.0006(15) -0.0046(16) -0.0003(15) O14 0.036(2) 0.041(2) 0.037(2) -0.0043(17) 0.0011(17) -0.0020(17) C1 0.041(3) 0.023(2) 0.028(3) 0.0036(19) -0.011(2) -0.009(2) C2 0.048(3) 0.032(3) 0.046(3) 0.002(2) -0.009(3) -0.020(3) C3 0.038(3) 0.044(3) 0.044(3) -0.006(3) -0.011(3) -0.015(3) C4 0.026(2) 0.036(3) 0.026(2) -0.007(2) -0.008(2) -0.004(2) C5 0.029(2) 0.024(2) 0.015(2) -0.0032(17) -0.0059(18) -0.0016(18) C6 0.021(2) 0.024(2) 0.023(2) 0.0002(17) -0.0068(18) -0.0004(17) C7 0.024(2) 0.024(2) 0.022(2) 0.0039(17) -0.0077(18) -0.0027(18) C8 0.029(2) 0.024(2) 0.022(2) 0.0002(18) -0.0036(19) -0.0002(19) C9 0.036(3) 0.025(2) 0.017(2) -0.0003(17) -0.0076(19) -0.003(2) C10 0.031(2) 0.018(2) 0.025(2) 0.0000(17) -0.012(2) -0.0012(18) C11 0.027(2) 0.017(2) 0.018(2) 0.0038(16) -0.0083(18) 0.0003(17) C12 0.025(2) 0.024(2) 0.020(2) -0.0009(17) -0.0087(18) -0.0009(18) C13 0.039(3) 0.026(2) 0.026(2) -0.0070(19) -0.014(2) 0.002(2) C14 0.044(3) 0.036(3) 0.056(4) -0.015(3) -0.027(3) -0.002(3) C15 0.055(4) 0.027(3) 0.069(4) -0.012(3) -0.030(3) -0.009(3) C16 0.048(3) 0.019(2) 0.044(3) -0.006(2) -0.018(3) 0.001(2) C17 0.037(3) 0.018(2) 0.020(2) -0.0076(17) -0.0095(19) 0.0026(19) C18 0.034(3) 0.015(2) 0.025(2) -0.0044(17) -0.008(2) 0.0010(18) C19 0.038(3) 0.023(2) 0.021(2) -0.0021(18) -0.007(2) 0.002(2) C20 0.048(3) 0.030(3) 0.020(2) -0.005(2) -0.008(2) 0.004(2) C21 0.053(3) 0.030(3) 0.020(2) 0.000(2) -0.007(2) 0.004(2) C22 0.041(3) 0.027(3) 0.022(2) 0.0020(19) -0.001(2) -0.004(2) C23 0.036(3) 0.021(2) 0.021(2) 0.0001(18) -0.006(2) 0.0035(19) C24 0.036(3) 0.022(2) 0.018(2) 0.0025(17) -0.0025(19) -0.0051(19) C25 0.037(3) 0.018(2) 0.026(2) 0.0010(18) -0.017(2) 0.0002(19) C26 0.047(3) 0.024(3) 0.041(3) 0.011(2) -0.020(3) -0.001(2) C27 0.043(3) 0.022(2) 0.027(2) -0.0014(19) -0.017(2) 0.005(2) C28 0.107(6) 0.036(3) 0.090(6) -0.029(4) -0.077(5) 0.034(4) C29 0.025(2) 0.023(2) 0.024(2) -0.0023(18) -0.0072(19) -0.0010(18) C30 0.033(3) 0.057(4) 0.032(3) -0.020(3) -0.009(2) 0.004(3) C31 0.034(3) 0.028(2) 0.018(2) -0.0020(18) -0.0035(19) -0.007(2) C32 0.037(3) 0.035(3) 0.035(3) 0.001(2) -0.006(2) -0.012(2) C33 0.031(3) 0.033(3) 0.035(3) 0.000(2) -0.007(2) 0.006(2) C34 0.052(4) 0.052(4) 0.045(4) -0.017(3) -0.003(3) 0.000(3) C1S 0.048(3) 0.044(3) 0.030(3) 0.006(2) -0.011(3) -0.012(3) Cl1 0.0588(10) 0.0419(8) 0.0550(10) -0.0082(7) -0.0076(8) -0.0017(7) Cl2 0.0551(10) 0.0555(10) 0.0546(10) 0.0084(8) -0.0138(8) -0.0206(8) O1W 0.0277(18) 0.0273(18) 0.0301(18) 0.0003(14) -0.0041(15) -0.0007(14) _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 O4 2.347(3) . ? Gd1 O8 2.349(3) . ? Gd1 O1 2.392(3) . ? Gd1 O10 2.398(3) . ? Gd1 O2 2.401(3) . ? Gd1 O12 2.418(3) . ? Gd1 O9 2.455(4) . ? Gd1 O11 2.466(3) . ? Gd1 Ni3 3.3482(6) . ? Gd1 Ni1 3.4470(6) . ? Gd1 Ni2 3.5967(6) . ? Ni1 O5 2.028(3) . ? Ni1 N1 2.039(4) . ? Ni1 O2 2.047(3) . ? Ni1 O1 2.060(3) . ? Ni1 O3 2.080(3) . ? Ni1 N2 2.084(4) . ? Ni1 Ni2 2.9763(8) . ? Ni1 Ni3 3.1259(8) . ? Ni2 O13 1.990(4) . ? Ni2 O3 2.065(3) . ? Ni2 O1W 2.078(4) . ? Ni2 O6 2.083(3) . ? Ni2 O2 2.086(3) . ? Ni2 O4 2.176(3) . ? Ni2 Ni3 3.1660(8) . ? Ni3 O3 2.009(3) . ? Ni3 O7 2.029(3) . ? Ni3 N3 2.062(4) . ? Ni3 O4 2.065(3) . ? Ni3 N4 2.081(4) . ? Ni3 O1 2.129(3) . ? N1 C1 1.339(6) . ? N1 C5 1.351(6) . ? N2 C7 1.335(6) . ? N2 C11 1.339(6) . ? N3 C13 1.342(6) . ? N3 C17 1.343(6) . ? N4 C23 1.326(6) . ? N4 C19 1.351(6) . ? O1 C6 1.416(5) . ? O2 C12 1.416(5) . ? O3 C18 1.407(5) . ? O4 C24 1.414(5) . ? O5 C25 1.265(6) . ? O6 C25 1.253(6) . ? O7 C27 1.263(6) . ? O8 C27 1.258(6) . ? O9 C29 1.257(6) . ? O10 C29 1.258(6) . ? O11 C31 1.274(6) . ? O12 C31 1.260(6) . ? O13 C33 1.268(6) . ? O14 C33 1.248(7) . ? C1 C2 1.382(8) . ? C2 C3 1.364(9) . ? C3 C4 1.379(8) . ? C4 C5 1.375(7) . ? C5 C6 1.512(6) . ? C7 C8 1.387(7) . ? C8 C9 1.386(7) . ? C9 C10 1.370(7) . ? C10 C11 1.392(6) . ? C11 C12 1.519(6) . ? C13 C14 1.388(8) . ? C14 C15 1.374(9) . ? C15 C16 1.389(8) . ? C16 C17 1.394(7) . ? C17 C18 1.516(7) . ? C19 C20 1.389(7) . ? C20 C21 1.378(8) . ? C21 C22 1.387(7) . ? C22 C23 1.397(7) . ? C23 C24 1.516(7) . ? C25 C26 1.514(6) . ? C27 C28 1.510(8) . ? C29 C30 1.508(7) . ? C31 C32 1.504(7) . ? C33 C34 1.519(8) . ? C1S Cl1 1.757(6) . ? C1S Cl2 1.767(6) . ? 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 Gd1 O8 81.95(11) . . ? O4 Gd1 O1 74.43(11) . . ? O8 Gd1 O1 77.33(11) . . ? O4 Gd1 O10 145.36(11) . . ? O8 Gd1 O10 132.17(11) . . ? O1 Gd1 O10 113.98(11) . . ? O4 Gd1 O2 69.10(10) . . ? O8 Gd1 O2 141.48(11) . . ? O1 Gd1 O2 70.93(10) . . ? O10 Gd1 O2 81.77(11) . . ? O4 Gd1 O12 104.33(11) . . ? O8 Gd1 O12 77.08(12) . . ? O1 Gd1 O12 154.29(11) . . ? O10 Gd1 O12 82.04(12) . . ? O2 Gd1 O12 133.44(11) . . ? O4 Gd1 O9 156.03(12) . . ? O8 Gd1 O9 83.83(12) . . ? O1 Gd1 O9 83.70(11) . . ? O10 Gd1 O9 53.87(11) . . ? O2 Gd1 O9 113.07(12) . . ? O12 Gd1 O9 91.10(13) . . ? O4 Gd1 O11 79.46(11) . . ? O8 Gd1 O11 119.55(12) . . ? O1 Gd1 O11 146.47(11) . . ? O10 Gd1 O11 77.51(11) . . ? O2 Gd1 O11 80.39(11) . . ? O12 Gd1 O11 53.54(12) . . ? O9 Gd1 O11 124.45(11) . . ? O4 Gd1 Ni3 37.59(8) . . ? O8 Gd1 Ni3 66.63(8) . . ? O1 Gd1 Ni3 39.29(7) . . ? O10 Gd1 Ni3 149.41(8) . . ? O2 Gd1 Ni3 74.99(7) . . ? O12 Gd1 Ni3 128.49(9) . . ? O9 Gd1 Ni3 118.58(8) . . ? O11 Gd1 Ni3 116.96(8) . . ? O4 Gd1 Ni1 72.26(7) . . ? O8 Gd1 Ni1 112.20(8) . . ? O1 Gd1 Ni1 35.90(7) . . ? O10 Gd1 Ni1 94.96(8) . . ? O2 Gd1 Ni1 35.61(7) . . ? O12 Gd1 Ni1 169.01(9) . . ? O9 Gd1 Ni1 95.66(9) . . ? O11 Gd1 Ni1 115.52(8) . . ? Ni3 Gd1 Ni1 54.754(14) . . ? O4 Gd1 Ni2 35.69(7) . . ? O8 Gd1 Ni2 115.62(8) . . ? O1 Gd1 Ni2 72.76(7) . . ? O10 Gd1 Ni2 112.02(8) . . ? O2 Gd1 Ni2 33.81(7) . . ? O12 Gd1 Ni2 121.47(9) . . ? O9 Gd1 Ni2 144.17(9) . . ? O11 Gd1 Ni2 73.76(8) . . ? Ni3 Gd1 Ni2 54.099(14) . . ? Ni1 Gd1 Ni2 49.935(14) . . ? O5 Ni1 N1 99.19(14) . . ? O5 Ni1 O2 95.54(13) . . ? N1 Ni1 O2 164.40(14) . . ? O5 Ni1 O1 169.95(13) . . ? N1 Ni1 O1 81.16(14) . . ? O2 Ni1 O1 85.24(12) . . ? O5 Ni1 O3 88.15(13) . . ? N1 Ni1 O3 99.39(14) . . ? O2 Ni1 O3 86.15(12) . . ? O1 Ni1 O3 81.90(12) . . ? O5 Ni1 N2 90.83(14) . . ? N1 Ni1 N2 96.32(15) . . ? O2 Ni1 N2 78.27(13) . . ? O1 Ni1 N2 99.13(13) . . ? O3 Ni1 N2 164.21(14) . . ? O5 Ni1 Ni2 81.59(10) . . ? N1 Ni1 Ni2 143.29(11) . . ? O2 Ni1 Ni2 44.44(9) . . ? O1 Ni1 Ni2 92.12(9) . . ? O3 Ni1 Ni2 43.91(9) . . ? N2 Ni1 Ni2 120.39(11) . . ? O5 Ni1 Ni3 127.42(10) . . ? N1 Ni1 Ni3 90.24(10) . . ? O2 Ni1 Ni3 84.85(8) . . ? O1 Ni1 Ni3 42.60(8) . . ? O3 Ni1 Ni3 39.31(8) . . ? N2 Ni1 Ni3 139.63(10) . . ? Ni2 Ni1 Ni3 62.450(19) . . ? O5 Ni1 Gd1 138.62(10) . . ? N1 Ni1 Gd1 122.07(11) . . ? O2 Ni1 Gd1 43.09(8) . . ? O1 Ni1 Gd1 42.90(9) . . ? O3 Ni1 Gd1 88.14(8) . . ? N2 Ni1 Gd1 82.23(10) . . ? Ni2 Ni1 Gd1 67.644(16) . . ? Ni3 Ni1 Gd1 61.014(14) . . ? O13 Ni2 O3 92.84(14) . . ? O13 Ni2 O1W 93.39(15) . . ? O3 Ni2 O1W 171.04(13) . . ? O13 Ni2 O6 95.75(14) . . ? O3 Ni2 O6 87.64(13) . . ? O1W Ni2 O6 98.12(14) . . ? O13 Ni2 O2 173.27(14) . . ? O3 Ni2 O2 85.54(12) . . ? O1W Ni2 O2 87.53(13) . . ? O6 Ni2 O2 90.72(13) . . ? O13 Ni2 O4 94.91(14) . . ? O3 Ni2 O4 78.51(12) . . ? O1W Ni2 O4 94.55(13) . . ? O6 Ni2 O4 162.90(13) . . ? O2 Ni2 O4 78.37(12) . . ? O13 Ni2 Ni1 136.43(11) . . ? O3 Ni2 Ni1 44.32(9) . . ? O1W Ni2 Ni1 130.12(10) . . ? O6 Ni2 Ni1 78.07(10) . . ? O2 Ni2 Ni1 43.40(9) . . ? O4 Ni2 Ni1 84.99(9) . . ? O13 Ni2 Ni3 91.46(11) . . ? O3 Ni2 Ni3 38.37(8) . . ? O1W Ni2 Ni3 134.95(10) . . ? O6 Ni2 Ni3 125.88(10) . . ? O2 Ni2 Ni3 83.21(9) . . ? O4 Ni2 Ni3 40.40(9) . . ? Ni1 Ni2 Ni3 61.092(19) . . ? O13 Ni2 Gd1 133.52(11) . . ? O3 Ni2 Gd1 84.38(8) . . ? O1W Ni2 Gd1 86.67(10) . . ? O6 Ni2 Gd1 130.31(10) . . ? O2 Ni2 Gd1 39.84(8) . . ? O4 Ni2 Gd1 39.00(8) . . ? Ni1 Ni2 Gd1 62.420(16) . . ? Ni3 Ni2 Gd1 58.942(14) . . ? O3 Ni3 O7 168.90(14) . . ? O3 Ni3 N3 80.38(14) . . ? O7 Ni3 N3 96.41(15) . . ? O3 Ni3 O4 82.42(13) . . ? O7 Ni3 O4 102.18(13) . . ? N3 Ni3 O4 160.46(14) . . ? O3 Ni3 N4 102.90(14) . . ? O7 Ni3 N4 87.92(14) . . ? N3 Ni3 N4 95.16(15) . . ? O4 Ni3 N4 79.69(14) . . ? O3 Ni3 O1 81.91(12) . . ? O7 Ni3 O1 88.29(12) . . ? N3 Ni3 O1 100.46(14) . . ? O4 Ni3 O1 86.18(12) . . ? N4 Ni3 O1 164.24(14) . . ? O3 Ni3 Ni1 41.00(9) . . ? O7 Ni3 Ni1 128.93(10) . . ? N3 Ni3 Ni1 90.04(11) . . ? O4 Ni3 Ni1 82.98(8) . . ? N4 Ni3 Ni1 141.98(11) . . ? O1 Ni3 Ni1 40.91(8) . . ? O3 Ni3 Ni2 39.65(9) . . ? O7 Ni3 Ni2 145.01(10) . . ? N3 Ni3 Ni2 118.58(11) . . ? O4 Ni3 Ni2 43.06(9) . . ? N4 Ni3 Ni2 88.62(12) . . ? O1 Ni3 Ni2 85.74(9) . . ? Ni1 Ni3 Ni2 56.458(18) . . ? O3 Ni3 Gd1 92.13(9) . . ? O7 Ni3 Gd1 84.58(9) . . ? N3 Ni3 Gd1 145.79(11) . . ? O4 Ni3 Gd1 43.88(9) . . ? N4 Ni3 Gd1 119.03(11) . . ? O1 Ni3 Gd1 45.34(8) . . ? Ni1 Ni3 Gd1 64.233(15) . . ? Ni2 Ni3 Gd1 66.959(16) . . ? C1 N1 C5 118.9(4) . . ? C1 N1 Ni1 127.2(4) . . ? C5 N1 Ni1 113.7(3) . . ? C7 N2 C11 118.5(4) . . ? C7 N2 Ni1 130.0(3) . . ? C11 N2 Ni1 110.8(3) . . ? C13 N3 C17 119.3(4) . . ? C13 N3 Ni3 128.8(3) . . ? C17 N3 Ni3 111.9(3) . . ? C23 N4 C19 118.9(4) . . ? C23 N4 Ni3 112.3(3) . . ? C19 N4 Ni3 127.8(3) . . ? C6 O1 Ni1 110.3(3) . . ? C6 O1 Ni3 117.4(3) . . ? Ni1 O1 Ni3 96.49(12) . . ? C6 O1 Gd1 130.2(3) . . ? Ni1 O1 Gd1 101.21(12) . . ? Ni3 O1 Gd1 95.38(12) . . ? C12 O2 Ni1 108.1(3) . . ? C12 O2 Ni2 121.5(3) . . ? Ni1 O2 Ni2 92.15(12) . . ? C12 O2 Gd1 121.5(3) . . ? Ni1 O2 Gd1 101.30(12) . . ? Ni2 O2 Gd1 106.35(12) . . ? C18 O3 Ni3 110.9(3) . . ? C18 O3 Ni2 125.3(3) . . ? Ni3 O3 Ni2 101.98(13) . . ? C18 O3 Ni1 122.6(3) . . ? Ni3 O3 Ni1 99.69(13) . . ? Ni2 O3 Ni1 91.77(12) . . ? C24 O4 Ni3 111.1(3) . . ? C24 O4 Ni2 119.2(3) . . ? Ni3 O4 Ni2 96.54(12) . . ? C24 O4 Gd1 121.5(3) . . ? Ni3 O4 Gd1 98.52(13) . . ? Ni2 O4 Gd1 105.30(12) . . ? C25 O5 Ni1 125.4(3) . . ? C25 O6 Ni2 127.2(3) . . ? C27 O7 Ni3 125.6(3) . . ? C27 O8 Gd1 135.2(3) . . ? C29 O9 Gd1 90.7(3) . . ? C29 O10 Gd1 93.3(3) . . ? C31 O11 Gd1 91.6(3) . . ? C31 O12 Gd1 94.2(3) . . ? C33 O13 Ni2 127.2(4) . . ? N1 C1 C2 121.2(5) . . ? C3 C2 C1 120.0(5) . . ? C2 C3 C4 119.0(5) . . ? C5 C4 C3 119.1(5) . . ? N1 C5 C4 121.8(4) . . ? N1 C5 C6 115.8(4) . . ? C4 C5 C6 122.4(4) . . ? O1 C6 C5 111.2(4) . . ? N2 C7 C8 123.1(4) . . ? C9 C8 C7 118.0(4) . . ? C10 C9 C8 119.3(4) . . ? C9 C10 C11 119.4(4) . . ? N2 C11 C10 121.6(4) . . ? N2 C11 C12 115.8(4) . . ? C10 C11 C12 122.5(4) . . ? O2 C12 C11 109.4(4) . . ? N3 C13 C14 122.6(5) . . ? C15 C14 C13 117.6(5) . . ? C14 C15 C16 121.0(5) . . ? C15 C16 C17 117.8(5) . . ? N3 C17 C16 121.7(5) . . ? N3 C17 C18 116.1(4) . . ? C16 C17 C18 122.2(4) . . ? O3 C18 C17 109.8(4) . . ? N4 C19 C20 122.1(5) . . ? C21 C20 C19 118.9(5) . . ? C20 C21 C22 118.9(5) . . ? C21 C22 C23 119.0(5) . . ? N4 C23 C22 122.1(5) . . ? N4 C23 C24 117.5(4) . . ? C22 C23 C24 120.4(4) . . ? O4 C24 C23 111.4(4) . . ? O6 C25 O5 126.9(4) . . ? O6 C25 C26 117.6(5) . . ? O5 C25 C26 115.6(5) . . ? O8 C27 O7 125.2(5) . . ? O8 C27 C28 117.5(5) . . ? O7 C27 C28 117.3(5) . . ? O9 C29 O10 121.9(4) . . ? O9 C29 C30 120.2(4) . . ? O10 C29 C30 117.9(4) . . ? O12 C31 O11 120.5(4) . . ? O12 C31 C32 120.3(5) . . ? O11 C31 C32 119.2(5) . . ? O14 C33 O13 126.1(5) . . ? O14 C33 C34 117.9(5) . . ? O13 C33 C34 115.9(5) . . ? Cl1 C1S Cl2 110.3(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H2W O14 0.855(10) 1.78(2) 2.600(5) 160(6) . O1W H1W O11 0.855(10) 1.974(17) 2.814(5) 167(6) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.759 _refine_diff_density_min -1.115 _refine_diff_density_rms 0.147 _shelx_res_file ; TITL C078 in P-1 CELL 0.71073 10.6729 10.7918 18.8925 87.780 75.783 87.955 ZERR 2.00 0.0007 0.0007 0.0013 0.001 0.001 0.001 LATT 1 SFAC C H N O Ni Gd Cl UNIT 70 86 8 30 6 2 4 OMIT -1.00 55.00 L.S. 10 ACTA BOND FMAP 2 PLAN 20 SIZE 0.24 0.20 0.12 DFIX 0.85 0.01 O1W H1W O1W H2W HTAB O1W O11 HTAB O1W O14 dfix 1.4 0.02 H1W H2W HTAB BIND Ni1 Ni2 BIND Ni1 Ni3 BIND Ni2 Ni3 BIND Ni1 Gd1 BIND Ni2 Gd1 BIND Ni3 Gd1 FREE Gd1 C31 FREE C29 Gd1 WGHT 0.044100 7.560600 FVAR 0.082040 TEMP -173 Gd1 6 0.135351 0.492234 0.215084 11.000000 0.024620 0.016210 = 0.017790 0.000450 -0.007130 -0.000210 Ni1 5 0.206173 0.787639 0.143934 11.000000 0.023020 0.016740 = 0.016350 0.002350 -0.007400 -0.002660 Ni2 5 -0.051258 0.777293 0.249622 11.000000 0.023120 0.015820 = 0.027440 0.000610 -0.012160 0.000190 Ni3 5 0.200589 0.729627 0.308059 11.000000 0.027810 0.015640 = 0.015230 0.000390 -0.006580 0.000990 N1 3 0.386655 0.857065 0.127418 11.000000 0.027780 0.018730 = 0.017610 -0.000050 -0.007680 -0.005530 N2 3 0.239837 0.697030 0.045325 11.000000 0.023050 0.021680 = 0.016240 0.003470 -0.004410 -0.002930 N3 3 0.320083 0.876020 0.307038 11.000000 0.031710 0.020230 = 0.017660 -0.003490 -0.008890 0.001330 N4 3 0.088629 0.757753 0.413346 11.000000 0.035130 0.019890 = 0.017130 0.001460 -0.005790 0.001980 O1 4 0.284856 0.656082 0.203561 11.000000 0.022290 0.019260 = 0.016670 0.000750 -0.005040 0.000290 O2 4 0.051778 0.673320 0.162389 11.000000 0.024680 0.017820 = 0.016920 0.000720 -0.007590 -0.002240 O3 4 0.124218 0.853982 0.247485 11.000000 0.027420 0.014310 = 0.021510 0.000530 -0.008320 0.000860 O4 4 0.038447 0.632631 0.305561 11.000000 0.029930 0.018480 = 0.014950 0.001060 -0.003990 -0.000080 O5 4 0.117887 0.932277 0.102110 11.000000 0.033140 0.023030 = 0.021330 0.004050 -0.010560 -0.002140 O6 4 -0.080604 0.920654 0.177946 11.000000 0.028980 0.019610 = 0.031030 0.003330 -0.011460 0.001710 O7 4 0.305965 0.601224 0.351568 11.000000 0.039970 0.021040 = 0.021580 -0.002340 -0.014410 0.005500 O8 4 0.252702 0.432317 0.301534 11.000000 0.046320 0.017590 = 0.025080 0.000780 -0.018600 0.000420 O9 4 0.314908 0.388270 0.129176 11.000000 0.023500 0.044790 = 0.032340 -0.010880 -0.009990 0.000730 O10 4 0.127021 0.407294 0.100935 11.000000 0.026390 0.030160 = 0.023900 -0.005760 -0.008320 0.003540 O11 4 -0.093214 0.436083 0.237026 11.000000 0.028100 0.021850 = 0.029870 -0.003440 -0.004770 -0.000930 O12 4 0.044607 0.294782 0.262079 11.000000 0.033260 0.026420 = 0.032660 0.004460 -0.011050 -0.003740 O13 4 -0.140589 0.863026 0.340380 11.000000 0.034000 0.030520 = 0.033190 -0.000570 -0.004560 -0.000340 O14 4 -0.314934 0.745958 0.380322 11.000000 0.035620 0.041060 = 0.036630 -0.004310 0.001140 -0.002000 C1 1 0.424711 0.970082 0.100890 11.000000 0.040880 0.023340 = 0.028150 0.003580 -0.010680 -0.008860 AFIX 43 H1 2 0.365754 1.024748 0.084051 11.000000 -1.200000 AFIX 0 C2 1 0.548109 1.008732 0.097537 11.000000 0.047980 0.032360 = 0.045630 0.002360 -0.008930 -0.019540 AFIX 43 H2 2 0.573657 1.088942 0.078002 11.000000 -1.200000 AFIX 0 C3 1 0.633263 0.931645 0.122295 11.000000 0.037680 0.043940 = 0.044350 -0.005880 -0.010790 -0.015030 AFIX 43 H3 2 0.717984 0.957826 0.120695 11.000000 -1.200000 AFIX 0 C4 1 0.594435 0.815118 0.149682 11.000000 0.026130 0.036270 = 0.025750 -0.006920 -0.008030 -0.003820 AFIX 43 H4 2 0.652173 0.759727 0.167047 11.000000 -1.200000 AFIX 0 C5 1 0.471029 0.780242 0.151502 11.000000 0.029470 0.024000 = 0.014520 -0.003220 -0.005940 -0.001570 C6 1 0.421474 0.653747 0.179783 11.000000 0.021230 0.023540 = 0.023010 0.000240 -0.006810 -0.000370 AFIX 23 H6A 2 0.449533 0.593192 0.140572 11.000000 -1.200000 H6B 2 0.459029 0.626407 0.220968 11.000000 -1.200000 AFIX 0 C7 1 0.348083 0.685787 -0.007683 11.000000 0.023760 0.024310 = 0.021920 0.003910 -0.007660 -0.002670 AFIX 43 H7 2 0.427247 0.708970 0.001868 11.000000 -1.200000 AFIX 0 C8 1 0.350352 0.641866 -0.076004 11.000000 0.028660 0.024310 = 0.021570 0.000150 -0.003640 -0.000210 AFIX 43 H8 2 0.429332 0.633093 -0.112154 11.000000 -1.200000 AFIX 0 C9 1 0.233877 0.611137 -0.089970 11.000000 0.035970 0.024880 = 0.017270 -0.000270 -0.007620 -0.002770 AFIX 43 H9 2 0.231224 0.583886 -0.136783 11.000000 -1.200000 AFIX 0 C10 1 0.122618 0.620499 -0.035518 11.000000 0.030960 0.018110 = 0.024780 -0.000010 -0.012360 -0.001150 AFIX 43 H10 2 0.042186 0.598869 -0.044045 11.000000 -1.200000 AFIX 0 C11 1 0.128559 0.662008 0.032420 11.000000 0.026610 0.017260 = 0.017720 0.003840 -0.008300 0.000290 C12 1 0.010908 0.668216 0.096704 11.000000 0.024850 0.023930 = 0.019910 -0.000870 -0.008700 -0.000860 AFIX 23 H12A 2 -0.043015 0.742776 0.091107 11.000000 -1.200000 H12B 2 -0.041915 0.594142 0.098229 11.000000 -1.200000 AFIX 0 C13 1 0.434203 0.875851 0.324958 11.000000 0.039490 0.025560 = 0.025570 -0.007020 -0.013870 0.001670 AFIX 43 H13 2 0.469500 0.799295 0.338816 11.000000 -1.200000 AFIX 0 C14 1 0.502729 0.983025 0.324059 11.000000 0.043990 0.036000 = 0.055700 -0.015400 -0.026530 -0.002480 AFIX 43 H14 2 0.583353 0.980764 0.337018 11.000000 -1.200000 AFIX 0 C15 1 0.449702 1.092555 0.303739 11.000000 0.055410 0.026910 = 0.068790 -0.012450 -0.030010 -0.009300 AFIX 43 H15 2 0.495016 1.167277 0.301838 11.000000 -1.200000 AFIX 0 C16 1 0.330876 1.095624 0.285944 11.000000 0.048070 0.018970 = 0.044100 -0.006290 -0.017950 0.001080 AFIX 43 H16A 2 0.292953 1.171567 0.273190 11.000000 -1.200000 AFIX 0 C17 1 0.269080 0.983599 0.287414 11.000000 0.036650 0.017580 = 0.019730 -0.007600 -0.009480 0.002590 C18 1 0.141094 0.975833 0.266733 11.000000 0.033920 0.014670 = 0.024540 -0.004420 -0.007810 0.001040 AFIX 23 H18A 2 0.069476 1.000098 0.308464 11.000000 -1.200000 H18B 2 0.139564 1.033852 0.225041 11.000000 -1.200000 AFIX 0 C19 1 0.111378 0.834483 0.463346 11.000000 0.038150 0.023330 = 0.020620 -0.002130 -0.007000 0.002360 AFIX 43 H19 2 0.175667 0.895149 0.448177 11.000000 -1.200000 AFIX 0 C20 1 0.043810 0.827559 0.536230 11.000000 0.047560 0.029830 = 0.020110 -0.005180 -0.008210 0.003570 AFIX 43 H20 2 0.061105 0.883063 0.570270 11.000000 -1.200000 AFIX 0 C21 1 -0.048679 0.738919 0.558360 11.000000 0.052670 0.029730 = 0.020430 0.000060 -0.007390 0.003960 AFIX 43 H21 2 -0.094919 0.731168 0.608094 11.000000 -1.200000 AFIX 0 C22 1 -0.073171 0.661184 0.506833 11.000000 0.040810 0.027160 = 0.021560 0.001990 -0.001130 -0.003640 AFIX 43 H22 2 -0.137263 0.600045 0.520626 11.000000 -1.200000 AFIX 0 C23 1 -0.002207 0.674115 0.434355 11.000000 0.035840 0.021160 = 0.021360 0.000110 -0.005720 0.003520 C24 1 -0.027134 0.591331 0.376501 11.000000 0.035560 0.022470 = 0.018500 0.002520 -0.002480 -0.005070 AFIX 23 H24A 2 0.002054 0.505354 0.385511 11.000000 -1.200000 H24B 2 -0.121161 0.590801 0.379884 11.000000 -1.200000 AFIX 0 C25 1 0.003004 0.970955 0.127738 11.000000 0.037280 0.017930 = 0.026470 0.001030 -0.017380 0.000240 C26 1 -0.035120 1.091356 0.093738 11.000000 0.046900 0.023990 = 0.041240 0.010680 -0.019920 -0.000840 AFIX 137 H26A 2 -0.126690 1.110949 0.115029 11.000000 -1.500000 H26B 2 -0.020916 1.082702 0.040891 11.000000 -1.500000 H26C 2 0.017569 1.158348 0.103286 11.000000 -1.500000 AFIX 0 C27 1 0.318576 0.487614 0.336751 11.000000 0.043110 0.022470 = 0.026750 -0.001410 -0.017250 0.005170 C28 1 0.421344 0.412556 0.363066 11.000000 0.107190 0.035980 = 0.089790 -0.028610 -0.077320 0.033820 AFIX 137 H28A 2 0.386114 0.333131 0.384408 11.000000 -1.500000 H28B 2 0.449010 0.458457 0.400084 11.000000 -1.500000 H28C 2 0.495612 0.397360 0.321786 11.000000 -1.500000 AFIX 0 C29 1 0.242450 0.367815 0.087783 11.000000 0.024710 0.023180 = 0.024460 -0.002320 -0.007170 -0.000970 C30 1 0.294017 0.297091 0.018900 11.000000 0.033280 0.057340 = 0.032340 -0.019610 -0.008860 0.004380 AFIX 137 H30A 2 0.221719 0.264398 0.002543 11.000000 -1.500000 H30B 2 0.350391 0.228206 0.028643 11.000000 -1.500000 H30C 2 0.343452 0.352709 -0.019249 11.000000 -1.500000 AFIX 0 C31 1 -0.068053 0.326135 0.257521 11.000000 0.034460 0.028380 = 0.017570 -0.001990 -0.003500 -0.007350 C32 1 -0.175102 0.234742 0.277721 11.000000 0.037180 0.034830 = 0.035240 0.001300 -0.006410 -0.011980 AFIX 137 H32A 2 -0.138035 0.150146 0.274246 11.000000 -1.500000 H32B 2 -0.231894 0.246286 0.244221 11.000000 -1.500000 H32C 2 -0.225149 0.248228 0.327860 11.000000 -1.500000 AFIX 0 C33 1 -0.240138 0.828034 0.387773 11.000000 0.031490 0.033140 = 0.035400 -0.000440 -0.006820 0.006000 C34 1 -0.267998 0.892146 0.460411 11.000000 0.051960 0.052470 = 0.045050 -0.016950 -0.002690 0.000430 AFIX 137 H34A 2 -0.329589 0.961554 0.459955 11.000000 -1.500000 H34B 2 -0.187432 0.923387 0.468130 11.000000 -1.500000 H34C 2 -0.304939 0.832846 0.499997 11.000000 -1.500000 AFIX 0 C1S 1 0.408798 0.674760 0.488663 11.000000 0.047790 0.043710 = 0.030060 0.005780 -0.011190 -0.011960 AFIX 23 H1S1 2 0.499646 0.645367 0.470840 11.000000 -1.200000 H1S2 2 0.372946 0.693523 0.445713 11.000000 -1.200000 AFIX 0 Cl1 7 0.403644 0.809822 0.538461 11.000000 0.058850 0.041930 = 0.055010 -0.008200 -0.007630 -0.001670 Cl2 7 0.318420 0.557433 0.544193 11.000000 0.055130 0.055490 = 0.054630 0.008430 -0.013800 -0.020560 O1W 4 -0.211465 0.674184 0.248479 11.000000 0.027700 0.027270 = 0.030110 0.000310 -0.004130 -0.000660 H1W 2 -0.187605 0.597630 0.245787 11.000000 -1.200000 H2W 2 -0.258296 0.684085 0.291695 11.000000 -1.200000 Q1 1 -0.082800 0.764400 0.284600 11.000000 0.050000 2.76 Q2 1 0.203100 0.529000 0.229500 11.000000 0.050000 2.52 Q3 1 -0.015700 0.786200 0.245100 11.000000 0.050000 1.73 Q4 1 -0.070300 0.767200 0.230700 11.000000 0.050000 1.64 Q5 1 0.194900 0.500200 0.169200 11.000000 0.050000 1.11 Q6 1 0.074600 0.493900 0.264900 11.000000 0.050000 1.01 Q7 1 0.047600 0.478700 0.224200 11.000000 0.050000 0.98 Q8 1 0.262700 0.760900 0.313100 11.000000 0.050000 0.95 Q9 1 0.137500 0.780100 0.147000 11.000000 0.050000 0.93 Q10 1 0.057500 0.448700 0.224800 11.000000 0.050000 0.91 Q11 1 0.079800 0.485200 0.180000 11.000000 0.050000 0.88 Q12 1 0.129200 0.727700 0.322700 11.000000 0.050000 0.77 Q13 1 0.215100 0.443500 0.203000 11.000000 0.050000 0.74 Q14 1 0.136000 0.562200 0.179900 11.000000 0.050000 0.73 Q15 1 0.145000 0.423000 0.180800 11.000000 0.050000 0.71 Q16 1 0.228100 0.792700 0.167800 11.000000 0.050000 0.67 Q17 1 0.264600 0.782900 0.118700 11.000000 0.050000 0.67 Q18 1 0.141200 0.430600 0.253600 11.000000 0.050000 0.64 Q19 1 0.321400 0.655100 0.534300 11.000000 0.050000 0.63 Q20 1 0.116700 0.301100 0.130400 11.000000 0.050000 0.59 HKLF 4 END ; _database_code_depnum_ccdc_archive 'CCDC 955198' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c088 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H43 Cl1.25 N4 Ni3 O15.50 Tb' _chemical_formula_weight 1147.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.4649(9) _cell_length_b 18.8485(14) _cell_length_c 19.7796(15) _cell_angle_alpha 90.00 _cell_angle_beta 99.7320(10) _cell_angle_gamma 90.00 _cell_volume 4212.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6483 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.77 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2301 _exptl_absorpt_coefficient_mu 3.130 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3324 _exptl_absorpt_correction_T_max 0.4312 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29548 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_unetI/netI 0.0518 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9667 _reflns_number_gt 7970 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The solvents were refined as two partially occupied dichloromethane and one partially occupied water. ; _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^)+(0.0614P)^2^+4.3634P] 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 9667 _refine_ls_number_parameters 574 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1161 _refine_ls_wR_factor_gt 0.1106 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.002 _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 C2S C 0.403(3) 0.9651(19) 0.4038(17) 0.040(8) Uiso 0.20 1 d P A 2 H2S1 H 0.4236 0.9898 0.3632 0.048 Uiso 0.20 1 calc PR A 2 H2S2 H 0.3762 1.0007 0.4345 0.048 Uiso 0.20 1 calc PR A 2 Cl4 Cl 0.2885(9) 0.8998(5) 0.3777(5) 0.047(2) Uiso 0.20 1 d P A 2 Cl3 Cl 0.5294(7) 0.9176(4) 0.4481(4) 0.0464(17) Uiso 0.20 1 d P A 2 O3W O 0.6885(12) 1.0470(9) 0.6334(7) 0.069(5) Uani 0.40 1 d P B -1 C1S C 0.3979(12) 1.0021(8) 0.4078(7) 0.031(3) Uani 0.40 1 d P C -1 H1S1 H 0.3318 1.0362 0.4057 0.038 Uiso 0.40 1 calc PR C -1 H1S2 H 0.4464 1.0164 0.3732 0.038 Uiso 0.40 1 calc PR C -1 Cl1 Cl 0.488(2) 1.0052(17) 0.4919(12) 0.053(3) Uani 0.40 1 d P C -1 Cl2 Cl 0.3410(5) 0.9172(3) 0.3886(2) 0.0521(11) Uani 0.40 1 d P C -1 Tb1 Tb 0.865846(18) 0.813329(11) 0.666307(11) 0.02135(8) Uani 1 1 d . . . Ni1 Ni 1.03266(5) 0.74594(3) 0.54931(3) 0.01659(12) Uani 1 1 d . . . Ni2 Ni 1.01869(5) 0.64891(3) 0.66435(3) 0.01646(12) Uani 1 1 d . . . Ni3 Ni 0.78246(5) 0.68326(3) 0.55898(3) 0.01625(12) Uani 1 1 d . . . O1 O 0.8625(3) 0.78226(15) 0.54864(15) 0.0191(6) Uani 1 1 d . . . O2 O 1.0468(3) 0.75735(15) 0.65323(15) 0.0176(6) Uani 1 1 d . . . O3 O 0.9516(2) 0.64988(14) 0.56113(14) 0.0144(6) Uani 1 1 d . . . O4 O 0.8416(3) 0.69128(14) 0.66405(15) 0.0189(6) Uani 1 1 d . . . O5 O 1.1881(3) 0.69293(15) 0.55083(15) 0.0197(6) Uani 1 1 d . . . O6 O 1.1848(2) 0.62489(15) 0.64442(15) 0.0190(6) Uani 1 1 d . . . O7 O 0.6188(3) 0.72798(15) 0.54777(16) 0.0212(6) Uani 1 1 d . . . O8 O 0.6667(3) 0.81546(18) 0.6233(2) 0.0380(9) Uani 1 1 d . . . O9 O 0.8626(4) 0.93031(19) 0.6132(2) 0.0494(11) Uani 1 1 d . . . O10 O 0.9836(3) 0.91432(16) 0.70929(16) 0.0250(7) Uani 1 1 d . . . O11 O 0.9579(3) 0.77891(17) 0.78542(16) 0.0252(7) Uani 1 1 d . . . O12 O 0.7732(3) 0.81588(19) 0.7683(2) 0.0378(9) Uani 1 1 d . . . O13 O 0.9724(3) 0.54643(16) 0.67164(16) 0.0235(7) Uani 1 1 d . . . O14 O 1.0152(4) 0.5291(2) 0.7842(2) 0.0481(11) Uani 1 1 d . . . N1 N 0.9824(3) 0.7581(2) 0.44674(19) 0.0229(8) Uani 1 1 d . . . N2 N 1.1252(3) 0.84180(19) 0.5653(2) 0.0228(8) Uani 1 1 d . . . N3 N 0.7696(3) 0.64636(18) 0.46012(17) 0.0163(7) Uani 1 1 d . . . N4 N 0.7106(3) 0.59100(18) 0.59286(18) 0.0184(7) Uani 1 1 d . . . C1 C 1.0412(4) 0.7371(3) 0.3968(2) 0.0280(10) Uani 1 1 d . . . H1 H 1.1106 0.7092 0.4089 0.034 Uiso 1 1 calc R . . C2 C 1.0049(5) 0.7543(3) 0.3285(3) 0.0339(12) Uani 1 1 d . . . H2 H 1.0491 0.7394 0.2945 0.041 Uiso 1 1 calc R . . C3 C 0.9033(5) 0.7934(3) 0.3112(3) 0.0362(13) Uani 1 1 d . . . H3 H 0.8757 0.8058 0.2647 0.043 Uiso 1 1 calc R . . C4 C 0.8412(5) 0.8146(3) 0.3618(3) 0.0323(12) Uani 1 1 d . . . H4 H 0.7706 0.8416 0.3503 0.039 Uiso 1 1 calc R . . C5 C 0.8827(4) 0.7963(2) 0.4299(2) 0.0252(10) Uani 1 1 d . . . C6 C 0.8221(4) 0.8199(2) 0.4874(2) 0.0243(10) Uani 1 1 d . . . H6A H 0.8365 0.8712 0.4955 0.029 Uiso 1 1 calc R . . H6B H 0.7358 0.8127 0.4740 0.029 Uiso 1 1 calc R . . C7 C 1.1409(4) 0.8920(3) 0.5190(3) 0.0287(11) Uani 1 1 d . . . H7 H 1.1024 0.8866 0.4728 0.034 Uiso 1 1 calc R . . C8 C 1.2109(4) 0.9508(2) 0.5364(3) 0.0317(11) Uani 1 1 d . . . H8 H 1.2190 0.9858 0.5029 0.038 Uiso 1 1 calc R . . C9 C 1.2687(4) 0.9581(2) 0.6026(3) 0.0302(11) Uani 1 1 d . . . H9 H 1.3190 0.9976 0.6156 0.036 Uiso 1 1 calc R . . C10 C 1.2520(4) 0.9063(2) 0.6508(2) 0.0234(10) Uani 1 1 d . . . H10 H 1.2900 0.9104 0.6972 0.028 Uiso 1 1 calc R . . C11 C 1.1794(4) 0.8489(2) 0.6299(2) 0.0187(9) Uani 1 1 d . . . C12 C 1.1563(4) 0.7905(2) 0.6784(2) 0.0191(9) Uani 1 1 d . . . H12A H 1.2208 0.7551 0.6828 0.023 Uiso 1 1 calc R . . H12B H 1.1544 0.8107 0.7245 0.023 Uiso 1 1 calc R . . C13 C 0.6786(4) 0.6531(2) 0.4082(2) 0.0205(9) Uani 1 1 d . . . H13 H 0.6197 0.6877 0.4115 0.025 Uiso 1 1 calc R . . C14 C 0.6676(4) 0.6114(2) 0.3499(2) 0.0247(10) Uani 1 1 d . . . H14 H 0.6029 0.6178 0.3135 0.030 Uiso 1 1 calc R . . C15 C 0.7533(4) 0.5599(2) 0.3457(2) 0.0247(10) Uani 1 1 d . . . H15 H 0.7465 0.5293 0.3071 0.030 Uiso 1 1 calc R . . C16 C 0.8478(4) 0.5542(2) 0.3984(2) 0.0195(9) Uani 1 1 d . . . H16 H 0.9082 0.5202 0.3961 0.023 Uiso 1 1 calc R . . C17 C 0.8545(4) 0.5984(2) 0.4550(2) 0.0164(8) Uani 1 1 d . . . C18 C 0.9539(4) 0.5933(2) 0.5156(2) 0.0183(8) Uani 1 1 d . . . H18A H 0.9470 0.5481 0.5401 0.022 Uiso 1 1 calc R . . H18B H 1.0306 0.5932 0.4990 0.022 Uiso 1 1 calc R . . C19 C 0.6600(4) 0.5362(2) 0.5551(2) 0.0213(9) Uani 1 1 d . . . H19 H 0.6589 0.5366 0.5070 0.026 Uiso 1 1 calc R . . C20 C 0.6099(4) 0.4800(2) 0.5837(3) 0.0271(10) Uani 1 1 d . . . H20 H 0.5742 0.4424 0.5556 0.033 Uiso 1 1 calc R . . C21 C 0.6120(4) 0.4785(2) 0.6535(3) 0.0278(10) Uani 1 1 d . . . H21 H 0.5781 0.4399 0.6742 0.033 Uiso 1 1 calc R . . C22 C 0.6641(4) 0.5340(3) 0.6927(3) 0.0276(10) Uani 1 1 d . . . H22 H 0.6667 0.5343 0.7409 0.033 Uiso 1 1 calc R . . C23 C 0.7127(4) 0.5893(2) 0.6609(2) 0.0205(9) Uani 1 1 d . . . C24 C 0.7664(4) 0.6530(2) 0.7011(2) 0.0237(10) Uani 1 1 d . . . H24A H 0.7024 0.6846 0.7111 0.028 Uiso 1 1 calc R . . H24B H 0.8125 0.6370 0.7454 0.028 Uiso 1 1 calc R . . C25 C 1.2307(4) 0.6469(2) 0.5952(2) 0.0196(9) Uani 1 1 d . . . C26 C 1.3504(4) 0.6155(3) 0.5877(3) 0.0319(11) Uani 1 1 d . . . H26A H 1.4009 0.6129 0.6328 0.048 Uiso 1 1 calc R . . H26B H 1.3882 0.6457 0.5573 0.048 Uiso 1 1 calc R . . H26C H 1.3391 0.5678 0.5681 0.048 Uiso 1 1 calc R . . C27 C 0.5933(4) 0.7810(2) 0.5808(3) 0.0265(10) Uani 1 1 d . . . C28 C 0.4663(5) 0.8058(3) 0.5699(3) 0.0427(14) Uani 1 1 d . . . H28A H 0.4437 0.8170 0.6143 0.064 Uiso 1 1 calc R . . H28B H 0.4148 0.7683 0.5473 0.064 Uiso 1 1 calc R . . H28C H 0.4580 0.8483 0.5410 0.064 Uiso 1 1 calc R . . C29 C 0.9441(4) 0.9527(2) 0.6591(2) 0.0229(9) Uani 1 1 d . . . C30 C 0.9939(5) 1.0252(3) 0.6529(3) 0.0338(12) Uani 1 1 d . . . H30A H 1.0485 1.0369 0.6951 0.051 Uiso 1 1 calc R . . H30B H 0.9293 1.0599 0.6457 0.051 Uiso 1 1 calc R . . H30C H 1.0364 1.0264 0.6139 0.051 Uiso 1 1 calc R . . C31 C 0.8603(5) 0.7908(3) 0.8071(3) 0.0327(12) Uani 1 1 d . . . C32 C 0.8527(6) 0.7735(4) 0.8805(3) 0.060(2) Uani 1 1 d . . . H32A H 0.8239 0.8151 0.9025 0.090 Uiso 1 1 calc R . . H32B H 0.9313 0.7604 0.9050 0.090 Uiso 1 1 calc R . . H32C H 0.7979 0.7338 0.8819 0.090 Uiso 1 1 calc R . . C33 C 0.9787(4) 0.5083(2) 0.7246(2) 0.0251(10) Uani 1 1 d . . . C34 C 0.9394(5) 0.4326(3) 0.7147(3) 0.0343(12) Uani 1 1 d . . . H34A H 1.0080 0.4012 0.7260 0.051 Uiso 1 1 calc R . . H34B H 0.9024 0.4252 0.6668 0.051 Uiso 1 1 calc R . . H34C H 0.8820 0.4220 0.7448 0.051 Uiso 1 1 calc R . . O1W O 1.0792(3) 0.65849(17) 0.76697(16) 0.0247(7) Uani 1 1 d D . . H1W H 1.032(4) 0.690(2) 0.779(3) 0.030 Uiso 1 1 d D . . H2W H 1.060(4) 0.6187(14) 0.783(2) 0.030 Uiso 1 1 d 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 O3W 0.057(8) 0.096(13) 0.052(8) 0.012(8) 0.008(6) 0.034(9) C1S 0.036(8) 0.026(8) 0.034(7) -0.009(6) 0.013(6) -0.007(6) Cl1 0.044(9) 0.071(8) 0.046(10) 0.000(6) 0.015(6) -0.023(6) Cl2 0.074(4) 0.042(3) 0.045(3) -0.013(2) 0.023(2) -0.016(3) Tb1 0.01693(12) 0.01436(12) 0.03151(14) -0.00638(8) 0.00049(9) 0.00115(8) Ni1 0.0144(3) 0.0139(3) 0.0201(3) 0.0004(2) -0.0009(2) -0.0006(2) Ni2 0.0130(3) 0.0113(3) 0.0231(3) -0.0045(2) -0.0028(2) 0.0014(2) Ni3 0.0132(3) 0.0116(3) 0.0231(3) -0.00186(19) 0.0005(2) 0.00046(19) O1 0.0159(15) 0.0135(14) 0.0258(16) 0.0045(12) -0.0027(12) 0.0016(11) O2 0.0157(14) 0.0146(14) 0.0213(16) -0.0022(11) -0.0001(12) -0.0007(11) O3 0.0149(14) 0.0100(14) 0.0170(14) -0.0023(10) -0.0005(11) 0.0010(11) O4 0.0190(15) 0.0120(15) 0.0264(17) -0.0043(11) 0.0056(13) -0.0031(11) O5 0.0160(15) 0.0185(16) 0.0242(16) 0.0017(12) 0.0024(12) 0.0012(12) O6 0.0151(14) 0.0180(15) 0.0238(16) -0.0003(12) 0.0028(12) 0.0032(12) O7 0.0155(15) 0.0156(15) 0.0321(18) -0.0019(12) 0.0029(13) 0.0020(12) O8 0.0211(18) 0.031(2) 0.058(3) -0.0242(17) -0.0030(17) 0.0046(15) O9 0.064(3) 0.0218(19) 0.049(2) 0.0002(16) -0.029(2) -0.0001(18) O10 0.0314(18) 0.0196(16) 0.0227(17) 0.0009(12) 0.0006(14) -0.0050(14) O11 0.0215(17) 0.0251(17) 0.0308(18) -0.0053(13) 0.0096(14) -0.0048(13) O12 0.0245(19) 0.035(2) 0.054(3) -0.0114(17) 0.0101(18) 0.0040(15) O13 0.0235(16) 0.0193(16) 0.0281(18) -0.0003(13) 0.0059(13) -0.0018(13) O14 0.075(3) 0.030(2) 0.034(2) 0.0100(16) -0.006(2) -0.012(2) N1 0.024(2) 0.021(2) 0.021(2) 0.0035(15) -0.0021(15) -0.0058(15) N2 0.0201(19) 0.0138(18) 0.033(2) 0.0018(15) -0.0006(16) -0.0044(15) N3 0.0140(17) 0.0129(17) 0.0207(18) 0.0029(13) -0.0007(14) -0.0015(13) N4 0.0143(17) 0.0169(18) 0.0229(19) -0.0024(14) 0.0006(14) -0.0002(14) C1 0.030(3) 0.025(3) 0.028(3) -0.0018(19) 0.003(2) -0.008(2) C2 0.047(3) 0.029(3) 0.025(3) 0.000(2) 0.004(2) -0.017(2) C3 0.050(3) 0.029(3) 0.025(3) 0.007(2) -0.009(2) -0.024(2) C4 0.035(3) 0.023(3) 0.034(3) 0.0053(19) -0.006(2) -0.013(2) C5 0.027(2) 0.015(2) 0.030(3) 0.0045(18) -0.0047(19) -0.0095(18) C6 0.020(2) 0.017(2) 0.032(3) 0.0103(18) -0.0077(19) -0.0011(17) C7 0.023(2) 0.024(2) 0.036(3) 0.009(2) -0.002(2) -0.0062(19) C8 0.028(3) 0.018(2) 0.050(3) 0.009(2) 0.008(2) -0.0035(19) C9 0.025(2) 0.016(2) 0.052(3) -0.006(2) 0.013(2) -0.0072(18) C10 0.017(2) 0.023(2) 0.030(3) -0.0097(18) 0.0049(18) -0.0051(17) C11 0.014(2) 0.013(2) 0.030(2) -0.0039(16) 0.0054(17) 0.0025(16) C12 0.018(2) 0.015(2) 0.023(2) -0.0040(16) -0.0013(17) 0.0003(16) C13 0.019(2) 0.015(2) 0.027(2) 0.0067(17) 0.0010(18) -0.0016(16) C14 0.025(2) 0.025(2) 0.021(2) 0.0070(18) -0.0066(18) -0.0069(19) C15 0.031(3) 0.024(2) 0.017(2) 0.0014(17) 0.0006(19) -0.0051(19) C16 0.021(2) 0.017(2) 0.020(2) -0.0001(16) 0.0016(17) 0.0000(17) C17 0.019(2) 0.0113(19) 0.019(2) 0.0013(15) 0.0029(16) -0.0038(15) C18 0.019(2) 0.0117(19) 0.023(2) -0.0020(16) -0.0001(17) 0.0036(16) C19 0.019(2) 0.019(2) 0.025(2) -0.0028(17) -0.0009(17) -0.0018(17) C20 0.022(2) 0.019(2) 0.037(3) 0.0005(19) -0.001(2) -0.0070(18) C21 0.022(2) 0.021(2) 0.039(3) 0.006(2) 0.002(2) -0.0045(18) C22 0.024(2) 0.028(3) 0.030(3) 0.0011(19) 0.002(2) -0.003(2) C23 0.0112(19) 0.023(2) 0.027(2) -0.0005(17) 0.0023(17) -0.0007(17) C24 0.022(2) 0.026(2) 0.024(2) -0.0058(18) 0.0068(18) -0.0048(19) C25 0.016(2) 0.017(2) 0.026(2) -0.0063(17) 0.0024(17) -0.0017(16) C26 0.025(2) 0.027(3) 0.046(3) 0.004(2) 0.012(2) 0.009(2) C27 0.015(2) 0.021(2) 0.042(3) -0.001(2) 0.002(2) 0.0032(18) C28 0.018(3) 0.034(3) 0.074(4) -0.013(3) 0.001(3) 0.007(2) C29 0.024(2) 0.017(2) 0.026(2) -0.0036(17) 0.0007(18) 0.0057(18) C30 0.041(3) 0.024(3) 0.035(3) -0.002(2) 0.002(2) -0.003(2) C31 0.031(3) 0.031(3) 0.039(3) -0.014(2) 0.013(2) -0.010(2) C32 0.040(3) 0.114(6) 0.030(3) -0.014(3) 0.017(3) -0.023(4) C33 0.019(2) 0.022(2) 0.033(3) 0.0041(19) 0.0025(19) -0.0004(18) C34 0.030(3) 0.023(3) 0.049(3) 0.007(2) 0.004(2) -0.003(2) O1W 0.0245(17) 0.0212(17) 0.0279(18) -0.0015(13) 0.0032(14) 0.0008(14) _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 C2S Cl3 1.80(3) . ? C2S Cl4 1.81(4) . ? C1S Cl2 1.746(14) . ? C1S Cl1 1.80(2) . ? Tb1 O8 2.299(3) . ? Tb1 O4 2.317(3) . ? Tb1 O2 2.380(3) . ? Tb1 O1 2.394(3) . ? Tb1 O10 2.405(3) . ? Tb1 O12 2.434(4) . ? Tb1 O9 2.440(4) . ? Tb1 O11 2.499(3) . ? Tb1 Ni3 3.2780(6) . ? Tb1 Ni1 3.4818(6) . ? Tb1 Ni2 3.5636(6) . ? Ni1 N1 2.026(4) . ? Ni1 O5 2.039(3) . ? Ni1 O2 2.046(3) . ? Ni1 O1 2.066(3) . ? Ni1 O3 2.066(3) . ? Ni1 N2 2.092(4) . ? Ni1 Ni2 2.9447(8) . ? Ni1 Ni3 3.1379(8) . ? Ni2 O13 2.015(3) . ? Ni2 O1W 2.039(3) . ? Ni2 O3 2.056(3) . ? Ni2 O6 2.060(3) . ? Ni2 O2 2.087(3) . ? Ni2 O4 2.181(3) . ? Ni2 Ni3 3.1921(8) . ? Ni3 O3 2.033(3) . ? Ni3 O7 2.035(3) . ? Ni3 N3 2.057(3) . ? Ni3 O4 2.080(3) . ? Ni3 N4 2.083(4) . ? Ni3 O1 2.105(3) . ? O1 C6 1.413(5) . ? O2 C12 1.416(5) . ? O3 C18 1.398(5) . ? O4 C24 1.419(5) . ? O5 C25 1.272(5) . ? O6 C25 1.253(5) . ? O7 C27 1.255(5) . ? O8 C27 1.263(6) . ? O9 C29 1.262(6) . ? O10 C29 1.250(5) . ? O11 C31 1.283(6) . ? O12 C31 1.245(7) . ? O13 C33 1.263(6) . ? O14 C33 1.246(6) . ? N1 C5 1.345(6) . ? N1 C1 1.346(6) . ? N2 C11 1.329(6) . ? N2 C7 1.350(6) . ? N3 C13 1.341(5) . ? N3 C17 1.345(5) . ? N4 C23 1.343(6) . ? N4 C19 1.346(5) . ? C1 C2 1.383(7) . ? C2 C3 1.372(8) . ? C3 C4 1.383(8) . ? C4 C5 1.393(7) . ? C5 C6 1.496(7) . ? C7 C8 1.377(6) . ? C8 C9 1.372(7) . ? C9 C10 1.400(7) . ? C10 C11 1.385(6) . ? C11 C12 1.513(6) . ? C13 C14 1.382(6) . ? C14 C15 1.393(7) . ? C15 C16 1.375(6) . ? C16 C17 1.386(6) . ? C17 C18 1.511(6) . ? C19 C20 1.372(6) . ? C20 C21 1.377(7) . ? C21 C22 1.377(7) . ? C22 C23 1.382(6) . ? C23 C24 1.512(6) . ? C25 C26 1.524(6) . ? C27 C28 1.510(6) . ? C29 C30 1.493(7) . ? C31 C32 1.505(8) . ? C33 C34 1.498(7) . ? 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 Cl3 C2S Cl4 106.7(18) . . ? Cl2 C1S Cl1 111.4(13) . . ? O8 Tb1 O4 84.36(12) . . ? O8 Tb1 O2 142.84(11) . . ? O4 Tb1 O2 70.23(10) . . ? O8 Tb1 O1 78.01(12) . . ? O4 Tb1 O1 75.89(10) . . ? O2 Tb1 O1 69.94(10) . . ? O8 Tb1 O10 125.49(11) . . ? O4 Tb1 O10 148.35(11) . . ? O2 Tb1 O10 86.65(11) . . ? O1 Tb1 O10 116.95(10) . . ? O8 Tb1 O12 76.20(14) . . ? O4 Tb1 O12 88.16(11) . . ? O2 Tb1 O12 127.53(11) . . ? O1 Tb1 O12 150.82(12) . . ? O10 Tb1 O12 89.37(11) . . ? O8 Tb1 O9 83.27(14) . . ? O4 Tb1 O9 153.62(12) . . ? O2 Tb1 O9 107.68(13) . . ? O1 Tb1 O9 78.79(12) . . ? O10 Tb1 O9 53.40(11) . . ? O12 Tb1 O9 111.24(14) . . ? O8 Tb1 O11 126.05(13) . . ? O4 Tb1 O11 77.91(10) . . ? O2 Tb1 O11 75.56(10) . . ? O1 Tb1 O11 142.00(10) . . ? O10 Tb1 O11 75.51(10) . . ? O12 Tb1 O11 52.95(11) . . ? O9 Tb1 O11 127.88(11) . . ? O8 Tb1 Ni3 67.07(8) . . ? O4 Tb1 Ni3 39.10(7) . . ? O2 Tb1 Ni3 76.24(7) . . ? O1 Tb1 Ni3 39.86(7) . . ? O10 Tb1 Ni3 154.95(8) . . ? O12 Tb1 Ni3 115.54(9) . . ? O9 Tb1 Ni3 114.54(9) . . ? O11 Tb1 Ni3 116.54(7) . . ? O8 Tb1 Ni1 112.52(9) . . ? O4 Tb1 Ni1 72.70(7) . . ? O2 Tb1 Ni1 34.84(7) . . ? O1 Tb1 Ni1 35.41(7) . . ? O10 Tb1 Ni1 100.66(8) . . ? O12 Tb1 Ni1 157.48(9) . . ? O9 Tb1 Ni1 90.76(11) . . ? O11 Tb1 Ni1 109.89(7) . . ? Ni3 Tb1 Ni1 55.218(14) . . ? O8 Tb1 Ni2 118.08(8) . . ? O4 Tb1 Ni2 36.28(7) . . ? O2 Tb1 Ni2 34.32(7) . . ? O1 Tb1 Ni2 72.78(7) . . ? O10 Tb1 Ni2 116.39(8) . . ? O12 Tb1 Ni2 108.08(9) . . ? O9 Tb1 Ni2 138.83(11) . . ? O11 Tb1 Ni2 69.79(7) . . ? Ni3 Tb1 Ni2 55.435(13) . . ? Ni1 Tb1 Ni2 49.395(13) . . ? N1 Ni1 O5 99.78(14) . . ? N1 Ni1 O2 162.76(14) . . ? O5 Ni1 O2 96.67(12) . . ? N1 Ni1 O1 81.25(14) . . ? O5 Ni1 O1 170.01(12) . . ? O2 Ni1 O1 83.44(12) . . ? N1 Ni1 O3 98.92(13) . . ? O5 Ni1 O3 88.72(11) . . ? O2 Ni1 O3 86.51(11) . . ? O1 Ni1 O3 81.31(11) . . ? N1 Ni1 N2 96.02(15) . . ? O5 Ni1 N2 90.06(13) . . ? O2 Ni1 N2 78.78(13) . . ? O1 Ni1 N2 99.74(13) . . ? O3 Ni1 N2 165.00(13) . . ? N1 Ni1 Ni2 143.18(11) . . ? O5 Ni1 Ni2 81.13(8) . . ? O2 Ni1 Ni2 45.11(8) . . ? O1 Ni1 Ni2 92.07(8) . . ? O3 Ni1 Ni2 44.29(8) . . ? N2 Ni1 Ni2 120.80(11) . . ? N1 Ni1 Ni3 89.75(11) . . ? O5 Ni1 Ni3 128.35(8) . . ? O2 Ni1 Ni3 84.04(8) . . ? O1 Ni1 Ni3 41.67(8) . . ? O3 Ni1 Ni3 39.65(8) . . ? N2 Ni1 Ni3 139.60(11) . . ? Ni2 Ni1 Ni3 63.216(18) . . ? N1 Ni1 Tb1 121.96(11) . . ? O5 Ni1 Tb1 138.24(9) . . ? O2 Ni1 Tb1 41.65(8) . . ? O1 Ni1 Tb1 42.18(8) . . ? O3 Ni1 Tb1 86.36(8) . . ? N2 Ni1 Tb1 84.62(11) . . ? Ni2 Ni1 Tb1 66.749(16) . . ? Ni3 Ni1 Tb1 59.091(14) . . ? O13 Ni2 O1W 93.62(13) . . ? O13 Ni2 O3 91.19(12) . . ? O1W Ni2 O3 174.09(12) . . ? O13 Ni2 O6 93.80(12) . . ? O1W Ni2 O6 92.28(12) . . ? O3 Ni2 O6 90.84(11) . . ? O13 Ni2 O2 173.66(12) . . ? O1W Ni2 O2 89.17(12) . . ? O3 Ni2 O2 85.70(11) . . ? O6 Ni2 O2 91.77(12) . . ? O13 Ni2 O4 95.45(12) . . ? O1W Ni2 O4 97.49(12) . . ? O3 Ni2 O4 78.60(11) . . ? O6 Ni2 O4 166.08(11) . . ? O2 Ni2 O4 78.53(11) . . ? O13 Ni2 Ni1 134.43(9) . . ? O1W Ni2 Ni1 131.33(10) . . ? O3 Ni2 Ni1 44.55(8) . . ? O6 Ni2 Ni1 79.38(8) . . ? O2 Ni2 Ni1 44.00(8) . . ? O4 Ni2 Ni1 86.71(8) . . ? O13 Ni2 Ni3 92.09(9) . . ? O1W Ni2 Ni3 137.77(9) . . ? O3 Ni2 Ni3 38.41(8) . . ? O6 Ni2 Ni3 129.02(8) . . ? O2 Ni2 Ni3 82.04(8) . . ? O4 Ni2 Ni3 40.29(8) . . ? Ni1 Ni2 Ni3 61.347(18) . . ? O13 Ni2 Tb1 134.19(9) . . ? O1W Ni2 Tb1 89.85(9) . . ? O3 Ni2 Tb1 84.32(8) . . ? O6 Ni2 Tb1 131.73(8) . . ? O2 Ni2 Tb1 40.02(8) . . ? O4 Ni2 Tb1 38.95(7) . . ? Ni1 Ni2 Tb1 63.856(15) . . ? Ni3 Ni2 Tb1 57.739(13) . . ? O3 Ni3 O7 171.75(12) . . ? O3 Ni3 N3 80.20(12) . . ? O7 Ni3 N3 96.89(13) . . ? O3 Ni3 O4 81.54(11) . . ? O7 Ni3 O4 102.57(12) . . ? N3 Ni3 O4 158.96(13) . . ? O3 Ni3 N4 99.38(12) . . ? O7 Ni3 N4 88.46(13) . . ? N3 Ni3 N4 93.15(13) . . ? O4 Ni3 N4 79.58(13) . . ? O3 Ni3 O1 81.16(11) . . ? O7 Ni3 O1 91.79(12) . . ? N3 Ni3 O1 99.77(12) . . ? O4 Ni3 O1 87.64(11) . . ? N4 Ni3 O1 166.95(13) . . ? O3 Ni3 Ni1 40.44(8) . . ? O7 Ni3 Ni1 132.31(9) . . ? N3 Ni3 Ni1 89.34(10) . . ? O4 Ni3 Ni1 83.49(8) . . ? N4 Ni3 Ni1 138.54(10) . . ? O1 Ni3 Ni1 40.73(8) . . ? O3 Ni3 Ni2 38.95(8) . . ? O7 Ni3 Ni2 145.11(9) . . ? N3 Ni3 Ni2 117.93(10) . . ? O4 Ni3 Ni2 42.69(8) . . ? N4 Ni3 Ni2 87.64(10) . . ? O1 Ni3 Ni2 84.70(8) . . ? Ni1 Ni3 Ni2 55.437(17) . . ? O3 Ni3 Tb1 92.59(8) . . ? O7 Ni3 Tb1 85.61(9) . . ? N3 Ni3 Tb1 146.57(9) . . ? O4 Ni3 Tb1 44.63(8) . . ? N4 Ni3 Tb1 120.26(10) . . ? O1 Ni3 Tb1 46.81(8) . . ? Ni1 Ni3 Tb1 65.691(15) . . ? Ni2 Ni3 Tb1 66.826(15) . . ? C6 O1 Ni1 110.1(3) . . ? C6 O1 Ni3 116.3(3) . . ? Ni1 O1 Ni3 97.60(12) . . ? C6 O1 Tb1 131.4(3) . . ? Ni1 O1 Tb1 102.41(12) . . ? Ni3 O1 Tb1 93.33(11) . . ? C12 O2 Ni1 108.4(2) . . ? C12 O2 Ni2 122.6(2) . . ? Ni1 O2 Ni2 90.89(11) . . ? C12 O2 Tb1 120.2(2) . . ? Ni1 O2 Tb1 103.50(12) . . ? Ni2 O2 Tb1 105.66(12) . . ? C18 O3 Ni3 110.1(2) . . ? C18 O3 Ni2 126.0(2) . . ? Ni3 O3 Ni2 102.64(12) . . ? C18 O3 Ni1 122.5(2) . . ? Ni3 O3 Ni1 99.91(12) . . ? Ni2 O3 Ni1 91.16(11) . . ? C24 O4 Ni3 110.8(2) . . ? C24 O4 Ni2 117.3(3) . . ? Ni3 O4 Ni2 97.02(12) . . ? C24 O4 Tb1 125.2(2) . . ? Ni3 O4 Tb1 96.27(11) . . ? Ni2 O4 Tb1 104.77(12) . . ? C25 O5 Ni1 125.3(3) . . ? C25 O6 Ni2 126.8(3) . . ? C27 O7 Ni3 124.3(3) . . ? C27 O8 Tb1 138.2(3) . . ? C29 O9 Tb1 92.1(3) . . ? C29 O10 Tb1 94.1(3) . . ? C31 O11 Tb1 91.0(3) . . ? C31 O12 Tb1 95.0(3) . . ? C33 O13 Ni2 128.8(3) . . ? C5 N1 C1 119.0(4) . . ? C5 N1 Ni1 113.3(3) . . ? C1 N1 Ni1 127.5(3) . . ? C11 N2 C7 119.2(4) . . ? C11 N2 Ni1 112.0(3) . . ? C7 N2 Ni1 128.7(3) . . ? C13 N3 C17 119.0(4) . . ? C13 N3 Ni3 128.2(3) . . ? C17 N3 Ni3 111.3(3) . . ? C23 N4 C19 118.1(4) . . ? C23 N4 Ni3 113.6(3) . . ? C19 N4 Ni3 128.2(3) . . ? N1 C1 C2 122.8(5) . . ? C3 C2 C1 118.2(5) . . ? C2 C3 C4 119.6(5) . . ? C3 C4 C5 119.6(5) . . ? N1 C5 C4 120.7(5) . . ? N1 C5 C6 117.0(4) . . ? C4 C5 C6 122.3(5) . . ? O1 C6 C5 112.1(4) . . ? N2 C7 C8 122.2(5) . . ? C9 C8 C7 119.1(4) . . ? C8 C9 C10 118.7(4) . . ? C11 C10 C9 119.1(4) . . ? N2 C11 C10 121.7(4) . . ? N2 C11 C12 115.7(4) . . ? C10 C11 C12 122.6(4) . . ? O2 C12 C11 109.7(3) . . ? N3 C13 C14 122.3(4) . . ? C13 C14 C15 118.6(4) . . ? C16 C15 C14 118.9(4) . . ? C15 C16 C17 119.6(4) . . ? N3 C17 C16 121.5(4) . . ? N3 C17 C18 116.2(3) . . ? C16 C17 C18 122.3(4) . . ? O3 C18 C17 111.7(3) . . ? N4 C19 C20 122.4(4) . . ? C19 C20 C21 119.4(4) . . ? C22 C21 C20 118.8(4) . . ? C21 C22 C23 119.1(5) . . ? N4 C23 C22 122.2(4) . . ? N4 C23 C24 116.4(4) . . ? C22 C23 C24 121.3(4) . . ? O4 C24 C23 111.2(3) . . ? O6 C25 O5 126.8(4) . . ? O6 C25 C26 116.8(4) . . ? O5 C25 C26 116.4(4) . . ? O7 C27 O8 124.6(4) . . ? O7 C27 C28 118.4(4) . . ? O8 C27 C28 117.0(4) . . ? O10 C29 O9 120.2(4) . . ? O10 C29 C30 120.2(4) . . ? O9 C29 C30 119.6(4) . . ? O12 C31 O11 120.9(5) . . ? O12 C31 C32 120.4(5) . . ? O11 C31 C32 118.7(5) . . ? O14 C33 O13 124.7(4) . . ? O14 C33 C34 118.0(4) . . ? O13 C33 C34 117.3(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W O11 0.859(10) 1.90(2) 2.719(5) 160(5) . O1W H2W O14 0.855(10) 1.76(2) 2.585(5) 160(5) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.190 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.149 _shelx_res_file ; TITL C088 in P2(1)/n CELL 0.71073 11.4649 18.8485 19.7796 90.000 99.732 90.000 ZERR 4.00 0.0009 0.0014 0.0015 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O Ni Tb Cl UNIT 140 172 16 62 12 4 5 OMIT -1.00 55.00 L.S. 6 ACTA BOND FMAP 2 PLAN 20 DFIX 0.85 0.01 O1W H1W O1W H2W HTAB HTAB O1W O11 HTAB O1W O14 SIZE 0.20 0.16 0.14 BIND Ni1 Ni2 BIND Ni1 Ni3 BIND Ni2 Ni3 BIND Ni1 Tb1 BIND Ni2 Tb1 BIND Ni3 Tb1 FREE Tb1 C29 FREE Tb1 C31 TEMP -173 WGHT 0.061400 4.363400 FVAR 0.05295 0.77946 PART 2 C2S 1 0.403214 0.965060 0.403814 10.20000 0.03983 AFIX 23 H2S1 2 0.423643 0.989799 0.363234 10.20000 -1.20000 H2S2 2 0.376157 1.000713 0.434508 10.20000 -1.20000 AFIX 0 CL4 7 0.288478 0.899773 0.377674 10.20000 0.04720 CL3 7 0.529444 0.917591 0.448144 10.20000 0.04638 PART -1 O3W 4 0.688527 1.047027 0.633351 10.40000 0.05711 0.09612 = 0.05187 0.01241 0.00805 0.03396 C1S 1 0.397946 1.002083 0.407824 10.40000 0.03649 0.02625 = 0.03373 -0.00851 0.01304 -0.00670 AFIX 23 H1S1 2 0.331824 1.036235 0.405707 10.40000 -1.20000 H1S2 2 0.446377 1.016388 0.373151 10.40000 -1.20000 AFIX 0 CL1 7 0.487560 1.005168 0.491864 10.40000 0.04430 0.07069 = 0.04637 0.00004 0.01514 -0.02347 CL2 7 0.341007 0.917202 0.388562 10.40000 0.07401 0.04154 = 0.04538 -0.01347 0.02309 -0.01590 PART 0 TB1 6 0.865846 0.813329 0.666307 11.00000 0.01693 0.01436 = 0.03151 -0.00638 0.00049 0.00115 NI1 5 1.032660 0.745936 0.549309 11.00000 0.01444 0.01392 = 0.02006 0.00039 -0.00090 -0.00062 NI2 5 1.018687 0.648909 0.664350 11.00000 0.01299 0.01125 = 0.02310 -0.00449 -0.00281 0.00137 NI3 5 0.782455 0.683258 0.558981 11.00000 0.01317 0.01156 = 0.02311 -0.00186 0.00048 0.00046 O1 4 0.862479 0.782264 0.548642 11.00000 0.01593 0.01346 = 0.02580 0.00453 -0.00274 0.00161 O2 4 1.046768 0.757353 0.653229 11.00000 0.01566 0.01459 = 0.02128 -0.00216 -0.00015 -0.00067 O3 4 0.951623 0.649877 0.561129 11.00000 0.01493 0.01004 = 0.01701 -0.00234 -0.00046 0.00099 O4 4 0.841591 0.691282 0.664048 11.00000 0.01898 0.01199 = 0.02640 -0.00435 0.00564 -0.00310 O5 4 1.188134 0.692928 0.550834 11.00000 0.01598 0.01854 = 0.02423 0.00169 0.00242 0.00115 O6 4 1.184823 0.624892 0.644421 11.00000 0.01514 0.01798 = 0.02378 -0.00025 0.00280 0.00321 O7 4 0.618780 0.727977 0.547766 11.00000 0.01549 0.01560 = 0.03214 -0.00193 0.00294 0.00205 O8 4 0.666673 0.815455 0.623254 11.00000 0.02106 0.03136 = 0.05806 -0.02420 -0.00300 0.00459 O9 4 0.862616 0.930306 0.613158 11.00000 0.06407 0.02181 = 0.04887 0.00015 -0.02923 -0.00010 O10 4 0.983639 0.914317 0.709294 11.00000 0.03138 0.01959 = 0.02266 0.00088 0.00061 -0.00502 O11 4 0.957859 0.778910 0.785417 11.00000 0.02150 0.02510 = 0.03078 -0.00529 0.00962 -0.00478 O12 4 0.773231 0.815876 0.768301 11.00000 0.02450 0.03544 = 0.05450 -0.01143 0.01006 0.00399 O13 4 0.972395 0.546425 0.671637 11.00000 0.02355 0.01932 = 0.02815 -0.00026 0.00585 -0.00183 O14 4 1.015211 0.529127 0.784196 11.00000 0.07458 0.03005 = 0.03433 0.01000 -0.00597 -0.01159 N1 3 0.982438 0.758074 0.446744 11.00000 0.02396 0.02117 = 0.02141 0.00354 -0.00214 -0.00576 N2 3 1.125249 0.841797 0.565294 11.00000 0.02007 0.01377 = 0.03277 0.00180 -0.00064 -0.00435 N3 3 0.769641 0.646362 0.460121 11.00000 0.01401 0.01293 = 0.02070 0.00295 -0.00070 -0.00152 N4 3 0.710555 0.590997 0.592862 11.00000 0.01430 0.01693 = 0.02295 -0.00240 0.00057 -0.00019 C1 1 1.041214 0.737071 0.396775 11.00000 0.03049 0.02477 = 0.02792 -0.00175 0.00251 -0.00846 AFIX 43 H1 2 1.110649 0.709218 0.408949 11.00000 -1.20000 AFIX 0 C2 1 1.004889 0.754285 0.328498 11.00000 0.04695 0.02910 = 0.02481 -0.00041 0.00357 -0.01673 AFIX 43 H2 2 1.049103 0.739445 0.294505 11.00000 -1.20000 AFIX 0 C3 1 0.903278 0.793373 0.311172 11.00000 0.04967 0.02902 = 0.02480 0.00681 -0.00868 -0.02437 AFIX 43 H3 2 0.875727 0.805759 0.264657 11.00000 -1.20000 AFIX 0 C4 1 0.841210 0.814631 0.361849 11.00000 0.03540 0.02312 = 0.03415 0.00532 -0.00609 -0.01254 AFIX 43 H4 2 0.770647 0.841600 0.350322 11.00000 -1.20000 AFIX 0 C5 1 0.882709 0.796289 0.429870 11.00000 0.02744 0.01505 = 0.02993 0.00449 -0.00465 -0.00946 C6 1 0.822141 0.819855 0.487356 11.00000 0.01991 0.01735 = 0.03159 0.01032 -0.00766 -0.00109 AFIX 23 H6A 2 0.836483 0.871180 0.495535 11.00000 -1.20000 H6B 2 0.735764 0.812730 0.473994 11.00000 -1.20000 AFIX 0 C7 1 1.140923 0.892018 0.518980 11.00000 0.02291 0.02429 = 0.03641 0.00871 -0.00194 -0.00618 AFIX 43 H7 2 1.102386 0.886605 0.472830 11.00000 -1.20000 AFIX 0 C8 1 1.210854 0.950802 0.536363 11.00000 0.02755 0.01756 = 0.05036 0.00890 0.00806 -0.00355 AFIX 43 H8 2 1.218974 0.985823 0.502930 11.00000 -1.20000 AFIX 0 C9 1 1.268674 0.958119 0.602646 11.00000 0.02480 0.01600 = 0.05215 -0.00605 0.01287 -0.00717 AFIX 43 H9 2 1.319028 0.997594 0.615594 11.00000 -1.20000 AFIX 0 C10 1 1.252024 0.906290 0.650809 11.00000 0.01714 0.02274 = 0.03049 -0.00972 0.00492 -0.00508 AFIX 43 H10 2 1.289996 0.910422 0.697199 11.00000 -1.20000 AFIX 0 C11 1 1.179388 0.848896 0.629856 11.00000 0.01365 0.01336 = 0.02962 -0.00395 0.00543 0.00246 C12 1 1.156323 0.790525 0.678447 11.00000 0.01809 0.01462 = 0.02281 -0.00405 -0.00133 0.00034 AFIX 23 H12A 2 1.220845 0.755055 0.682769 11.00000 -1.20000 H12B 2 1.154431 0.810720 0.724453 11.00000 -1.20000 AFIX 0 C13 1 0.678642 0.653091 0.408168 11.00000 0.01861 0.01504 = 0.02699 0.00666 0.00099 -0.00165 AFIX 43 H13 2 0.619687 0.687725 0.411513 11.00000 -1.20000 AFIX 0 C14 1 0.667559 0.611426 0.349914 11.00000 0.02457 0.02503 = 0.02084 0.00697 -0.00664 -0.00686 AFIX 43 H14 2 0.602855 0.617759 0.313508 11.00000 -1.20000 AFIX 0 C15 1 0.753269 0.559943 0.345703 11.00000 0.03100 0.02442 = 0.01743 0.00144 0.00056 -0.00513 AFIX 43 H15 2 0.746503 0.529318 0.307090 11.00000 -1.20000 AFIX 0 C16 1 0.847820 0.554232 0.398406 11.00000 0.02066 0.01665 = 0.02047 -0.00005 0.00161 -0.00003 AFIX 43 H16 2 0.908184 0.520241 0.396052 11.00000 -1.20000 AFIX 0 C17 1 0.854508 0.598384 0.454997 11.00000 0.01904 0.01133 = 0.01867 0.00126 0.00288 -0.00379 C18 1 0.953894 0.593336 0.515606 11.00000 0.01944 0.01167 = 0.02264 -0.00195 -0.00014 0.00356 AFIX 23 H18A 2 0.947031 0.548093 0.540055 11.00000 -1.20000 H18B 2 1.030649 0.593185 0.498994 11.00000 -1.20000 AFIX 0 C19 1 0.659979 0.536234 0.555141 11.00000 0.01905 0.01881 = 0.02459 -0.00278 -0.00090 -0.00180 AFIX 43 H19 2 0.658909 0.536553 0.507012 11.00000 -1.20000 AFIX 0 C20 1 0.609938 0.479993 0.583683 11.00000 0.02240 0.01947 = 0.03747 0.00048 -0.00072 -0.00695 AFIX 43 H20 2 0.574163 0.442400 0.555565 11.00000 -1.20000 AFIX 0 C21 1 0.612045 0.478533 0.653465 11.00000 0.02239 0.02077 = 0.03901 0.00568 0.00207 -0.00452 AFIX 43 H21 2 0.578149 0.439928 0.674195 11.00000 -1.20000 AFIX 0 C22 1 0.664149 0.534015 0.692669 11.00000 0.02397 0.02841 = 0.02975 0.00111 0.00229 -0.00326 AFIX 43 H22 2 0.666660 0.534277 0.740922 11.00000 -1.20000 AFIX 0 C23 1 0.712741 0.589311 0.660939 11.00000 0.01121 0.02259 = 0.02730 -0.00054 0.00230 -0.00072 C24 1 0.766439 0.652987 0.701118 11.00000 0.02215 0.02583 = 0.02421 -0.00584 0.00683 -0.00484 AFIX 23 H24A 2 0.702447 0.684557 0.711083 11.00000 -1.20000 H24B 2 0.812492 0.636997 0.745389 11.00000 -1.20000 AFIX 0 C25 1 1.230735 0.646869 0.595203 11.00000 0.01602 0.01674 = 0.02570 -0.00631 0.00237 -0.00168 C26 1 1.350443 0.615509 0.587692 11.00000 0.02474 0.02665 = 0.04639 0.00435 0.01170 0.00905 AFIX 137 H26A 2 1.400940 0.612926 0.632845 11.00000 -1.50000 H26B 2 1.388235 0.645687 0.557312 11.00000 -1.50000 H26C 2 1.339108 0.567753 0.568089 11.00000 -1.50000 AFIX 0 C27 1 0.593340 0.780989 0.580848 11.00000 0.01521 0.02102 = 0.04230 -0.00113 0.00189 0.00315 C28 1 0.466302 0.805841 0.569910 11.00000 0.01848 0.03372 = 0.07379 -0.01261 0.00134 0.00711 AFIX 137 H28A 2 0.443677 0.817034 0.614318 11.00000 -1.50000 H28B 2 0.414797 0.768263 0.547348 11.00000 -1.50000 H28C 2 0.458001 0.848350 0.540964 11.00000 -1.50000 AFIX 0 C29 1 0.944133 0.952742 0.659139 11.00000 0.02431 0.01706 = 0.02603 -0.00362 0.00072 0.00573 C30 1 0.993866 1.025210 0.652935 11.00000 0.04079 0.02441 = 0.03461 -0.00150 0.00205 -0.00277 AFIX 137 H30A 2 1.048503 1.036879 0.695124 11.00000 -1.50000 H30B 2 0.929314 1.059918 0.645660 11.00000 -1.50000 H30C 2 1.036423 1.026394 0.613948 11.00000 -1.50000 AFIX 0 C31 1 0.860285 0.790768 0.807077 11.00000 0.03088 0.03099 = 0.03881 -0.01384 0.01314 -0.01024 C32 1 0.852686 0.773504 0.880511 11.00000 0.03951 0.11393 = 0.03008 -0.01362 0.01687 -0.02269 AFIX 137 H32A 2 0.823915 0.815097 0.902465 11.00000 -1.50000 H32B 2 0.931278 0.760363 0.905007 11.00000 -1.50000 H32C 2 0.797917 0.733812 0.881870 11.00000 -1.50000 AFIX 0 C33 1 0.978685 0.508293 0.724606 11.00000 0.01949 0.02212 = 0.03316 0.00410 0.00254 -0.00041 C34 1 0.939358 0.432643 0.714683 11.00000 0.02975 0.02303 = 0.04924 0.00660 0.00396 -0.00254 AFIX 137 H34A 2 1.007976 0.401208 0.725962 11.00000 -1.50000 H34B 2 0.902399 0.425248 0.666797 11.00000 -1.50000 H34C 2 0.881977 0.421995 0.744799 11.00000 -1.50000 AFIX 0 O1W 4 1.079226 0.658486 0.766968 11.00000 0.02454 0.02121 = 0.02788 -0.00148 0.00320 0.00084 H1W 2 1.032110 0.689843 0.778788 11.00000 -1.20000 H2W 2 1.059688 0.618668 0.782553 11.00000 -1.20000 HKLF 4 REM C088 in P2(1)/n REM R1 = 0.0449 for 7970 Fo > 4sig(Fo) and 0.0560 for all 9667 data REM 574 parameters refined using 2 restraints END WGHT 0.0614 2.9731 REM Highest difference peak 3.190, deepest hole -0.695, 1-sigma level 0.149 Q1 1 1.0004 0.6392 0.7002 11.00000 0.05 3.19 Q2 1 0.8667 0.8077 0.6218 11.00000 0.05 2.22 Q3 1 0.8637 0.8145 0.7156 11.00000 0.05 2.05 Q4 1 1.0540 0.6511 0.6725 11.00000 0.05 1.27 Q5 1 0.9414 0.8144 0.7082 11.00000 0.05 1.02 Q6 1 1.0534 0.7429 0.5163 11.00000 0.05 1.00 Q7 1 0.7573 0.6798 0.5950 11.00000 0.05 0.95 Q8 1 0.7829 0.6809 0.5129 11.00000 0.05 0.91 Q9 1 1.0188 0.7425 0.5944 11.00000 0.05 0.81 Q10 1 0.8380 0.8562 0.6583 11.00000 0.05 0.71 Q11 1 0.5203 0.9422 0.4687 11.00000 0.05 0.66 Q12 1 0.6847 0.8192 0.5806 11.00000 0.05 0.61 Q13 1 1.2739 0.9205 0.6274 11.00000 0.05 0.59 Q14 1 0.9789 0.7423 0.5332 11.00000 0.05 0.58 Q15 1 1.0055 0.7486 0.4231 11.00000 0.05 0.57 Q16 1 0.9048 0.5222 0.6575 11.00000 0.05 0.57 Q17 1 1.0169 0.6538 0.6077 11.00000 0.05 0.54 Q18 1 0.5318 0.8937 0.4260 11.00000 0.05 0.54 Q19 1 1.0221 0.7433 0.3512 11.00000 0.05 0.53 Q20 1 0.6696 0.6013 0.6455 11.00000 0.05 0.52 ; #===END _database_code_depnum_ccdc_archive 'CCDC 955199' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c065 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H43 Cl2 Dy N4 Ni3 O15' _chemical_formula_weight 1169.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6814(17) _cell_length_b 10.7905(17) _cell_length_c 18.848(3) _cell_angle_alpha 87.685(3) _cell_angle_beta 75.725(3) _cell_angle_gamma 88.381(3) _cell_volume 2103.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 980 _cell_measurement_theta_min 3.27 _cell_measurement_theta_max 27.50 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1170 _exptl_absorpt_coefficient_mu 3.277 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3540 _exptl_absorpt_correction_T_max 0.4397 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27418 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_unetI/netI 0.0276 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9612 _reflns_number_gt 9011 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H atoms of the water were located from different map and refined with restraints in bond lengths. ; _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^)+(0.0465P)^2^+7.5333P] 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 9612 _refine_ls_number_parameters 554 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.1003 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.134957(18) 0.494302(16) 0.215402(10) 0.02018(7) Uani 1 1 d . . . Ni1 Ni 0.20964(5) 0.78780(5) 0.14303(3) 0.01903(11) Uani 1 1 d . . . Ni2 Ni -0.04770(5) 0.77701(5) 0.24879(3) 0.02157(11) Uani 1 1 d . . . Ni3 Ni 0.20273(5) 0.72962(5) 0.30774(3) 0.01976(11) Uani 1 1 d . . . N1 N 0.3912(3) 0.8557(3) 0.12691(18) 0.0222(7) Uani 1 1 d . . . N2 N 0.2422(3) 0.6971(3) 0.04412(18) 0.0222(7) Uani 1 1 d . . . N3 N 0.3237(4) 0.8760(3) 0.30629(18) 0.0229(7) Uani 1 1 d . . . N4 N 0.0908(4) 0.7574(3) 0.41335(19) 0.0238(7) Uani 1 1 d . . . O1 O 0.2853(3) 0.6554(3) 0.20323(15) 0.0203(5) Uani 1 1 d . . . O2 O 0.0542(3) 0.6734(3) 0.16195(15) 0.0203(5) Uani 1 1 d . . . O3 O 0.1278(3) 0.8542(2) 0.24659(15) 0.0210(6) Uani 1 1 d . . . O4 O 0.0407(3) 0.6318(3) 0.30513(15) 0.0221(6) Uani 1 1 d . . . O5 O 0.1236(3) 0.9332(3) 0.10082(16) 0.0257(6) Uani 1 1 d . . . O6 O -0.0758(3) 0.9209(3) 0.17694(17) 0.0269(6) Uani 1 1 d . . . O7 O 0.3065(3) 0.6006(3) 0.35183(16) 0.0262(6) Uani 1 1 d . . . O8 O 0.2496(3) 0.4338(3) 0.30136(17) 0.0280(6) Uani 1 1 d . . . O9 O 0.3129(3) 0.3915(3) 0.13113(18) 0.0326(7) Uani 1 1 d . . . O10 O 0.1254(3) 0.4106(3) 0.10233(17) 0.0276(6) Uani 1 1 d . . . O11 O -0.0915(3) 0.4382(3) 0.23701(18) 0.0292(7) Uani 1 1 d . . . O12 O 0.0463(3) 0.2964(3) 0.26071(18) 0.0297(7) Uani 1 1 d . . . O13 O -0.1369(3) 0.8632(3) 0.33973(18) 0.0317(7) Uani 1 1 d . . . O14 O -0.3125(3) 0.7466(3) 0.3798(2) 0.0389(8) Uani 1 1 d . . . C1 C 0.4330(5) 0.9680(4) 0.0995(2) 0.0303(9) Uani 1 1 d . . . H1 H 0.3759 1.0231 0.0818 0.036 Uiso 1 1 calc R . . C2 C 0.5568(6) 1.0057(5) 0.0964(3) 0.0427(12) Uani 1 1 d . . . H2 H 0.5839 1.0859 0.0770 0.051 Uiso 1 1 calc R . . C3 C 0.6403(5) 0.9266(5) 0.1215(3) 0.0411(12) Uani 1 1 d . . . H3 H 0.7256 0.9515 0.1201 0.049 Uiso 1 1 calc R . . C4 C 0.5986(4) 0.8103(5) 0.1488(2) 0.0301(9) Uani 1 1 d . . . H4 H 0.6549 0.7537 0.1661 0.036 Uiso 1 1 calc R . . C5 C 0.4739(4) 0.7774(4) 0.1507(2) 0.0234(8) Uani 1 1 d . . . C6 C 0.4216(4) 0.6514(4) 0.1793(2) 0.0225(8) Uani 1 1 d . . . H6A H 0.4482 0.5908 0.1401 0.027 Uiso 1 1 calc R . . H6B H 0.4586 0.6233 0.2206 0.027 Uiso 1 1 calc R . . C7 C 0.3503(4) 0.6866(4) -0.0093(2) 0.0249(8) Uani 1 1 d . . . H7 H 0.4294 0.7110 0.0000 0.030 Uiso 1 1 calc R . . C8 C 0.3525(4) 0.6420(4) -0.0777(2) 0.0275(9) Uani 1 1 d . . . H8 H 0.4315 0.6329 -0.1138 0.033 Uiso 1 1 calc R . . C9 C 0.2358(5) 0.6111(4) -0.0914(2) 0.0273(9) Uani 1 1 d . . . H9 H 0.2329 0.5836 -0.1382 0.033 Uiso 1 1 calc R . . C10 C 0.1239(4) 0.6207(4) -0.0366(2) 0.0244(8) Uani 1 1 d . . . H10 H 0.0433 0.5994 -0.0452 0.029 Uiso 1 1 calc R . . C11 C 0.1302(4) 0.6618(4) 0.0314(2) 0.0221(8) Uani 1 1 d . . . C12 C 0.0133(4) 0.6684(4) 0.0955(2) 0.0229(8) Uani 1 1 d . . . H12A H -0.0397 0.7431 0.0897 0.028 Uiso 1 1 calc R . . H12B H -0.0404 0.5945 0.0972 0.028 Uiso 1 1 calc R . . C13 C 0.4389(5) 0.8762(4) 0.3237(2) 0.0287(9) Uani 1 1 d . . . H13 H 0.4741 0.7999 0.3378 0.034 Uiso 1 1 calc R . . C14 C 0.5077(5) 0.9835(5) 0.3219(3) 0.0402(12) Uani 1 1 d . . . H14 H 0.5890 0.9812 0.3340 0.048 Uiso 1 1 calc R . . C15 C 0.4554(6) 1.0933(5) 0.3021(3) 0.0453(13) Uani 1 1 d . . . H15 H 0.5006 1.1683 0.3006 0.054 Uiso 1 1 calc R . . C16 C 0.3369(5) 1.0952(4) 0.2843(3) 0.0351(10) Uani 1 1 d . . . H16A H 0.2999 1.1709 0.2709 0.042 Uiso 1 1 calc R . . C17 C 0.2735(4) 0.9841(4) 0.2864(2) 0.0242(8) Uani 1 1 d . . . C18 C 0.1454(4) 0.9761(4) 0.2662(2) 0.0248(8) Uani 1 1 d . . . H18A H 0.0742 0.9995 0.3084 0.030 Uiso 1 1 calc R . . H18B H 0.1435 1.0347 0.2247 0.030 Uiso 1 1 calc R . . C19 C 0.1130(5) 0.8343(4) 0.4636(2) 0.0280(9) Uani 1 1 d . . . H19 H 0.1774 0.8954 0.4484 0.034 Uiso 1 1 calc R . . C20 C 0.0456(5) 0.8273(4) 0.5361(2) 0.0323(10) Uani 1 1 d . . . H20 H 0.0630 0.8829 0.5702 0.039 Uiso 1 1 calc R . . C21 C -0.0471(5) 0.7386(4) 0.5584(2) 0.0333(10) Uani 1 1 d . . . H21 H -0.0928 0.7305 0.6084 0.040 Uiso 1 1 calc R . . C22 C -0.0734(5) 0.6606(4) 0.5068(2) 0.0316(10) Uani 1 1 d . . . H22 H -0.1386 0.6000 0.5208 0.038 Uiso 1 1 calc R . . C23 C -0.0017(5) 0.6736(4) 0.4340(2) 0.0269(9) Uani 1 1 d . . . C24 C -0.0262(5) 0.5906(4) 0.3762(2) 0.0260(9) Uani 1 1 d . . . H24A H 0.0021 0.5047 0.3856 0.031 Uiso 1 1 calc R . . H24B H -0.1200 0.5900 0.3791 0.031 Uiso 1 1 calc R . . C25 C 0.0082(5) 0.9719(4) 0.1265(2) 0.0272(9) Uani 1 1 d . . . C26 C -0.0283(5) 1.0926(4) 0.0925(3) 0.0370(11) Uani 1 1 d . . . H26A H -0.1201 1.1115 0.1130 0.056 Uiso 1 1 calc R . . H26B H -0.0122 1.0850 0.0394 0.056 Uiso 1 1 calc R . . H26C H 0.0238 1.1596 0.1031 0.056 Uiso 1 1 calc R . . C27 C 0.3161(5) 0.4871(4) 0.3370(2) 0.0284(9) Uani 1 1 d . . . C28 C 0.4145(7) 0.4098(5) 0.3648(4) 0.0590(19) Uani 1 1 d . . . H28A H 0.3779 0.3291 0.3834 0.089 Uiso 1 1 calc R . . H28B H 0.4383 0.4525 0.4044 0.089 Uiso 1 1 calc R . . H28C H 0.4916 0.3973 0.3248 0.089 Uiso 1 1 calc R . . C29 C 0.2405(4) 0.3708(4) 0.0893(2) 0.0248(8) Uani 1 1 d . . . C30 C 0.2918(5) 0.3013(6) 0.0203(3) 0.0408(12) Uani 1 1 d . . . H30A H 0.2195 0.2739 0.0018 0.061 Uiso 1 1 calc R . . H30B H 0.3427 0.2289 0.0308 0.061 Uiso 1 1 calc R . . H30C H 0.3468 0.3558 -0.0166 0.061 Uiso 1 1 calc R . . C31 C -0.0663(5) 0.3278(4) 0.2567(2) 0.0270(9) Uani 1 1 d . . . C32 C -0.1733(5) 0.2349(5) 0.2768(3) 0.0357(10) Uani 1 1 d . . . H32A H -0.1359 0.1511 0.2785 0.054 Uiso 1 1 calc R . . H32B H -0.2242 0.2398 0.2400 0.054 Uiso 1 1 calc R . . H32C H -0.2293 0.2533 0.3249 0.054 Uiso 1 1 calc R . . C33 C -0.2367(5) 0.8282(4) 0.3875(3) 0.0336(10) Uani 1 1 d . . . C34 C -0.2643(6) 0.8920(6) 0.4607(3) 0.0482(14) Uani 1 1 d . . . H34A H -0.3245 0.9620 0.4600 0.072 Uiso 1 1 calc R . . H34B H -0.1834 0.9222 0.4687 0.072 Uiso 1 1 calc R . . H34C H -0.3027 0.8327 0.5003 0.072 Uiso 1 1 calc R . . C1S C 0.4089(5) 0.6750(5) 0.4889(3) 0.0378(11) Uani 1 1 d . . . H1S1 H 0.3712 0.6934 0.4465 0.045 Uiso 1 1 calc R . . H1S2 H 0.4993 0.6460 0.4700 0.045 Uiso 1 1 calc R . . Cl1 Cl 0.40619(15) 0.81091(13) 0.53850(9) 0.0498(3) Uani 1 1 d . . . Cl2 Cl 0.31998(15) 0.55775(14) 0.54579(8) 0.0513(3) Uani 1 1 d . . . O1W O -0.2088(3) 0.6744(3) 0.24801(18) 0.0287(6) Uani 1 1 d D . . H1W H -0.197(6) 0.5963(13) 0.250(4) 0.049(18) Uiso 1 1 d D . . H2W H -0.257(7) 0.672(9) 0.291(2) 0.10(3) Uiso 1 1 d 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 0.02563(11) 0.01760(10) 0.01828(10) 0.00056(6) -0.00732(7) -0.00131(7) Ni1 0.0242(3) 0.0171(2) 0.0173(2) 0.00274(18) -0.00804(19) -0.00334(19) Ni2 0.0231(3) 0.0155(2) 0.0289(3) -0.00093(19) -0.0119(2) -0.00022(19) Ni3 0.0277(3) 0.0163(2) 0.0159(2) 0.00076(17) -0.00692(19) -0.00011(19) N1 0.0292(18) 0.0215(16) 0.0171(15) 0.0004(12) -0.0071(13) -0.0065(13) N2 0.0258(17) 0.0227(17) 0.0191(16) 0.0020(13) -0.0074(13) -0.0028(13) N3 0.0318(18) 0.0214(16) 0.0163(15) -0.0034(12) -0.0073(14) 0.0007(14) N4 0.0335(19) 0.0194(16) 0.0188(16) 0.0007(13) -0.0070(14) 0.0012(14) O1 0.0224(14) 0.0204(13) 0.0180(13) 0.0013(10) -0.0054(11) -0.0004(11) O2 0.0246(14) 0.0193(13) 0.0180(13) 0.0004(10) -0.0073(11) -0.0027(11) O3 0.0276(14) 0.0151(13) 0.0216(13) 0.0005(10) -0.0086(11) -0.0006(11) O4 0.0282(15) 0.0206(14) 0.0162(13) 0.0020(10) -0.0033(11) -0.0027(11) O5 0.0318(16) 0.0226(14) 0.0245(15) 0.0039(11) -0.0110(12) -0.0025(12) O6 0.0310(16) 0.0212(14) 0.0300(16) 0.0049(12) -0.0115(13) -0.0008(12) O7 0.0388(17) 0.0206(14) 0.0223(14) -0.0015(11) -0.0140(13) 0.0044(12) O8 0.0442(18) 0.0179(14) 0.0261(15) 0.0011(11) -0.0170(14) -0.0004(12) O9 0.0279(16) 0.0398(18) 0.0324(17) -0.0086(14) -0.0108(13) -0.0001(14) O10 0.0276(15) 0.0310(16) 0.0254(15) -0.0047(12) -0.0085(12) 0.0008(12) O11 0.0319(16) 0.0235(15) 0.0319(16) -0.0024(12) -0.0067(13) -0.0034(12) O12 0.0345(17) 0.0235(15) 0.0328(17) 0.0040(12) -0.0120(14) -0.0045(13) O13 0.0313(17) 0.0313(17) 0.0317(17) -0.0019(13) -0.0059(14) -0.0007(13) O14 0.0346(18) 0.0403(19) 0.0369(19) -0.0036(15) 0.0015(15) -0.0035(15) C1 0.040(3) 0.025(2) 0.027(2) 0.0039(17) -0.0100(19) -0.0091(18) C2 0.048(3) 0.032(3) 0.049(3) 0.001(2) -0.011(2) -0.021(2) C3 0.035(3) 0.040(3) 0.051(3) -0.004(2) -0.014(2) -0.016(2) C4 0.030(2) 0.037(2) 0.026(2) -0.0080(18) -0.0100(18) -0.0047(18) C5 0.029(2) 0.026(2) 0.0153(17) -0.0028(15) -0.0059(15) -0.0041(16) C6 0.0212(19) 0.024(2) 0.0219(19) 0.0006(15) -0.0051(15) -0.0008(15) C7 0.027(2) 0.026(2) 0.023(2) 0.0009(16) -0.0083(16) -0.0034(16) C8 0.031(2) 0.028(2) 0.022(2) 0.0000(16) -0.0034(17) -0.0043(17) C9 0.040(2) 0.023(2) 0.0201(19) -0.0004(15) -0.0103(17) -0.0042(17) C10 0.033(2) 0.0183(18) 0.026(2) 0.0012(15) -0.0135(17) -0.0037(16) C11 0.028(2) 0.0187(18) 0.0203(18) 0.0019(14) -0.0085(16) -0.0012(15) C12 0.0233(19) 0.025(2) 0.0215(19) 0.0003(15) -0.0073(15) -0.0039(15) C13 0.038(2) 0.028(2) 0.025(2) -0.0056(17) -0.0154(18) -0.0012(18) C14 0.043(3) 0.035(3) 0.050(3) -0.012(2) -0.023(2) -0.002(2) C15 0.053(3) 0.027(2) 0.064(4) -0.012(2) -0.028(3) -0.008(2) C16 0.045(3) 0.020(2) 0.043(3) -0.0066(18) -0.016(2) 0.0003(19) C17 0.035(2) 0.0195(19) 0.0186(18) -0.0042(14) -0.0075(16) 0.0010(16) C18 0.032(2) 0.0164(18) 0.027(2) -0.0019(15) -0.0088(17) -0.0007(16) C19 0.037(2) 0.023(2) 0.023(2) -0.0031(16) -0.0074(18) -0.0002(17) C20 0.047(3) 0.030(2) 0.020(2) -0.0056(17) -0.0079(19) 0.005(2) C21 0.048(3) 0.031(2) 0.0173(19) -0.0002(17) -0.0031(19) 0.002(2) C22 0.044(3) 0.026(2) 0.021(2) 0.0018(16) -0.0013(18) -0.0036(19) C23 0.038(2) 0.0200(19) 0.022(2) 0.0000(15) -0.0064(17) 0.0014(17) C24 0.036(2) 0.022(2) 0.0176(18) 0.0038(15) -0.0019(16) -0.0052(17) C25 0.038(2) 0.0198(19) 0.029(2) 0.0030(16) -0.0182(19) -0.0007(17) C26 0.045(3) 0.025(2) 0.043(3) 0.013(2) -0.017(2) 0.001(2) C27 0.042(3) 0.023(2) 0.023(2) -0.0014(16) -0.0162(18) 0.0056(18) C28 0.090(5) 0.034(3) 0.076(4) -0.023(3) -0.063(4) 0.027(3) C29 0.029(2) 0.0215(19) 0.025(2) -0.0034(16) -0.0083(17) -0.0011(16) C30 0.031(2) 0.054(3) 0.038(3) -0.020(2) -0.007(2) 0.006(2) C31 0.036(2) 0.025(2) 0.0192(19) -0.0006(15) -0.0037(17) -0.0062(17) C32 0.038(3) 0.032(2) 0.038(3) 0.002(2) -0.009(2) -0.014(2) C33 0.036(2) 0.029(2) 0.034(2) -0.0013(19) -0.008(2) 0.0041(19) C34 0.051(3) 0.048(3) 0.042(3) -0.013(2) -0.001(3) 0.001(3) C1S 0.047(3) 0.037(3) 0.032(2) 0.001(2) -0.012(2) -0.011(2) Cl1 0.0542(8) 0.0400(7) 0.0531(8) -0.0082(6) -0.0082(6) -0.0010(6) Cl2 0.0514(8) 0.0511(8) 0.0510(8) 0.0072(6) -0.0110(6) -0.0194(6) O1W 0.0275(16) 0.0283(16) 0.0306(17) 0.0013(13) -0.0078(13) -0.0025(13) _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 O4 2.313(3) . ? Dy1 O8 2.323(3) . ? Dy1 O1 2.365(3) . ? Dy1 O10 2.374(3) . ? Dy1 O2 2.381(3) . ? Dy1 O12 2.399(3) . ? Dy1 O9 2.429(3) . ? Dy1 O11 2.442(3) . ? Dy1 Ni3 3.3291(6) . ? Dy1 Ni1 3.4328(7) . ? Dy1 Ni2 3.5668(7) . ? Ni1 O5 2.029(3) . ? Ni1 N1 2.040(4) . ? Ni1 O2 2.049(3) . ? Ni1 O1 2.059(3) . ? Ni1 O3 2.079(3) . ? Ni1 N2 2.089(3) . ? Ni1 Ni2 2.9731(8) . ? Ni1 Ni3 3.1255(8) . ? Ni2 O13 1.996(3) . ? Ni2 O3 2.063(3) . ? Ni2 O1W 2.076(3) . ? Ni2 O2 2.077(3) . ? Ni2 O6 2.083(3) . ? Ni2 O4 2.180(3) . ? Ni2 Ni3 3.1614(8) . ? Ni3 O3 2.011(3) . ? Ni3 O7 2.032(3) . ? Ni3 N3 2.064(4) . ? Ni3 O4 2.065(3) . ? Ni3 N4 2.082(4) . ? Ni3 O1 2.129(3) . ? N1 C1 1.342(5) . ? N1 C5 1.348(6) . ? N2 C7 1.337(6) . ? N2 C11 1.344(5) . ? N3 C17 1.347(5) . ? N3 C13 1.350(6) . ? N4 C23 1.333(6) . ? N4 C19 1.352(5) . ? O1 C6 1.414(5) . ? O2 C12 1.427(5) . ? O3 C18 1.411(5) . ? O4 C24 1.413(5) . ? O5 C25 1.273(6) . ? O6 C25 1.255(6) . ? O7 C27 1.264(5) . ? O8 C27 1.256(5) . ? O9 C29 1.262(5) . ? O10 C29 1.259(5) . ? O11 C31 1.275(5) . ? O12 C31 1.260(6) . ? O13 C33 1.269(6) . ? O14 C33 1.249(6) . ? C1 C2 1.381(7) . ? C2 C3 1.372(8) . ? C3 C4 1.381(7) . ? C4 C5 1.380(6) . ? C5 C6 1.512(6) . ? C7 C8 1.388(6) . ? C8 C9 1.387(6) . ? C9 C10 1.377(6) . ? C10 C11 1.391(6) . ? C11 C12 1.511(6) . ? C13 C14 1.383(7) . ? C14 C15 1.372(8) . ? C15 C16 1.387(8) . ? C16 C17 1.388(6) . ? C17 C18 1.514(6) . ? C19 C20 1.380(6) . ? C20 C21 1.375(7) . ? C21 C22 1.395(7) . ? C22 C23 1.400(6) . ? C23 C24 1.514(6) . ? C25 C26 1.512(6) . ? C27 C28 1.504(7) . ? C29 C30 1.503(6) . ? C31 C32 1.508(6) . ? C33 C34 1.525(7) . ? C1S Cl2 1.763(5) . ? C1S Cl1 1.767(5) . ? 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 Dy1 O8 81.78(11) . . ? O4 Dy1 O1 74.93(10) . . ? O8 Dy1 O1 77.59(10) . . ? O4 Dy1 O10 145.43(10) . . ? O8 Dy1 O10 132.18(11) . . ? O1 Dy1 O10 113.85(10) . . ? O4 Dy1 O2 69.80(10) . . ? O8 Dy1 O2 142.07(10) . . ? O1 Dy1 O2 71.25(10) . . ? O10 Dy1 O2 81.31(10) . . ? O4 Dy1 O12 105.15(11) . . ? O8 Dy1 O12 76.72(11) . . ? O1 Dy1 O12 154.00(10) . . ? O10 Dy1 O12 81.26(11) . . ? O2 Dy1 O12 133.92(10) . . ? O4 Dy1 O9 155.62(11) . . ? O8 Dy1 O9 83.35(11) . . ? O1 Dy1 O9 83.07(10) . . ? O10 Dy1 O9 54.57(11) . . ? O2 Dy1 O9 113.06(11) . . ? O12 Dy1 O9 90.02(12) . . ? O4 Dy1 O11 79.64(10) . . ? O8 Dy1 O11 119.31(11) . . ? O1 Dy1 O11 147.00(10) . . ? O10 Dy1 O11 77.16(11) . . ? O2 Dy1 O11 80.49(10) . . ? O12 Dy1 O11 54.12(11) . . ? O9 Dy1 O11 124.63(11) . . ? O4 Dy1 Ni3 37.79(7) . . ? O8 Dy1 Ni3 66.72(7) . . ? O1 Dy1 Ni3 39.53(7) . . ? O10 Dy1 Ni3 149.49(8) . . ? O2 Dy1 Ni3 75.47(7) . . ? O12 Dy1 Ni3 129.22(8) . . ? O9 Dy1 Ni3 118.04(8) . . ? O11 Dy1 Ni3 117.33(7) . . ? O4 Dy1 Ni1 72.89(7) . . ? O8 Dy1 Ni1 112.54(8) . . ? O1 Dy1 Ni1 35.98(7) . . ? O10 Dy1 Ni1 94.74(8) . . ? O2 Dy1 Ni1 35.82(7) . . ? O12 Dy1 Ni1 169.73(8) . . ? O9 Dy1 Ni1 95.37(9) . . ? O11 Dy1 Ni1 115.84(8) . . ? Ni3 Dy1 Ni1 55.036(15) . . ? O4 Dy1 Ni2 36.17(7) . . ? O8 Dy1 Ni2 115.96(8) . . ? O1 Dy1 Ni2 73.17(7) . . ? O10 Dy1 Ni2 111.72(8) . . ? O2 Dy1 Ni2 34.03(7) . . ? O12 Dy1 Ni2 122.53(8) . . ? O9 Dy1 Ni2 144.26(9) . . ? O11 Dy1 Ni2 73.88(7) . . ? Ni3 Dy1 Ni2 54.441(15) . . ? Ni1 Dy1 Ni2 50.226(15) . . ? O5 Ni1 N1 99.43(13) . . ? O5 Ni1 O2 95.92(12) . . ? N1 Ni1 O2 163.86(13) . . ? O5 Ni1 O1 169.87(12) . . ? N1 Ni1 O1 81.15(13) . . ? O2 Ni1 O1 84.62(11) . . ? O5 Ni1 O3 88.00(12) . . ? N1 Ni1 O3 99.42(12) . . ? O2 Ni1 O3 86.01(11) . . ? O1 Ni1 O3 81.94(11) . . ? O5 Ni1 N2 90.85(13) . . ? N1 Ni1 N2 96.52(14) . . ? O2 Ni1 N2 78.23(12) . . ? O1 Ni1 N2 99.15(12) . . ? O3 Ni1 N2 164.00(13) . . ? O5 Ni1 Ni2 81.84(9) . . ? N1 Ni1 Ni2 143.34(10) . . ? O2 Ni1 Ni2 44.27(8) . . ? O1 Ni1 Ni2 91.66(8) . . ? O3 Ni1 Ni2 43.92(8) . . ? N2 Ni1 Ni2 120.14(10) . . ? O5 Ni1 Ni3 127.33(9) . . ? N1 Ni1 Ni3 89.94(9) . . ? O2 Ni1 Ni3 84.67(8) . . ? O1 Ni1 Ni3 42.58(8) . . ? O3 Ni1 Ni3 39.38(8) . . ? N2 Ni1 Ni3 139.69(10) . . ? Ni2 Ni1 Ni3 62.387(18) . . ? O5 Ni1 Dy1 138.77(9) . . ? N1 Ni1 Dy1 121.71(10) . . ? O2 Ni1 Dy1 42.86(8) . . ? O1 Ni1 Dy1 42.46(8) . . ? O3 Ni1 Dy1 87.88(8) . . ? N2 Ni1 Dy1 82.48(9) . . ? Ni2 Ni1 Dy1 67.226(15) . . ? Ni3 Ni1 Dy1 60.796(13) . . ? O13 Ni2 O3 92.76(12) . . ? O13 Ni2 O1W 93.20(14) . . ? O3 Ni2 O1W 171.39(12) . . ? O13 Ni2 O2 173.37(13) . . ? O3 Ni2 O2 85.70(11) . . ? O1W Ni2 O2 87.68(12) . . ? O13 Ni2 O6 95.41(13) . . ? O3 Ni2 O6 87.45(12) . . ? O1W Ni2 O6 98.17(13) . . ? O2 Ni2 O6 90.97(12) . . ? O13 Ni2 O4 95.15(12) . . ? O3 Ni2 O4 78.73(11) . . ? O1W Ni2 O4 94.54(12) . . ? O2 Ni2 O4 78.23(11) . . ? O6 Ni2 O4 162.97(12) . . ? O13 Ni2 Ni1 136.37(10) . . ? O3 Ni2 Ni1 44.35(8) . . ? O1W Ni2 Ni1 130.36(10) . . ? O2 Ni2 Ni1 43.52(8) . . ? O6 Ni2 Ni1 78.14(9) . . ? O4 Ni2 Ni1 85.00(8) . . ? O13 Ni2 Ni3 91.47(10) . . ? O3 Ni2 Ni3 38.52(8) . . ? O1W Ni2 Ni3 135.02(9) . . ? O2 Ni2 Ni3 83.30(8) . . ? O6 Ni2 Ni3 125.85(9) . . ? O4 Ni2 Ni3 40.48(8) . . ? Ni1 Ni2 Ni3 61.17(2) . . ? O13 Ni2 Dy1 133.55(10) . . ? O3 Ni2 Dy1 84.54(8) . . ? O1W Ni2 Dy1 86.85(9) . . ? O2 Ni2 Dy1 39.91(8) . . ? O6 Ni2 Dy1 130.61(9) . . ? O4 Ni2 Dy1 38.78(7) . . ? Ni1 Ni2 Dy1 62.547(15) . . ? Ni3 Ni2 Dy1 58.946(14) . . ? O3 Ni3 O7 168.95(12) . . ? O3 Ni3 N3 80.33(13) . . ? O7 Ni3 N3 96.55(14) . . ? O3 Ni3 O4 82.69(12) . . ? O7 Ni3 O4 101.76(12) . . ? N3 Ni3 O4 160.83(13) . . ? O3 Ni3 N4 103.04(13) . . ? O7 Ni3 N4 87.77(13) . . ? N3 Ni3 N4 95.34(14) . . ? O4 Ni3 N4 79.87(13) . . ? O3 Ni3 O1 81.84(11) . . ? O7 Ni3 O1 88.39(11) . . ? N3 Ni3 O1 100.77(12) . . ? O4 Ni3 O1 85.49(11) . . ? N4 Ni3 O1 163.76(13) . . ? O3 Ni3 Ni1 40.99(8) . . ? O7 Ni3 Ni1 128.95(9) . . ? N3 Ni3 Ni1 89.91(10) . . ? O4 Ni3 Ni1 83.02(8) . . ? N4 Ni3 Ni1 142.09(10) . . ? O1 Ni3 Ni1 40.87(7) . . ? O3 Ni3 Ni2 39.72(8) . . ? O7 Ni3 Ni2 144.81(9) . . ? N3 Ni3 Ni2 118.63(10) . . ? O4 Ni3 Ni2 43.27(8) . . ? N4 Ni3 Ni2 88.75(10) . . ? O1 Ni3 Ni2 85.34(8) . . ? Ni1 Ni3 Ni2 56.444(17) . . ? O3 Ni3 Dy1 91.93(8) . . ? O7 Ni3 Dy1 84.71(8) . . ? N3 Ni3 Dy1 145.78(10) . . ? O4 Ni3 Dy1 43.37(8) . . ? N4 Ni3 Dy1 118.87(10) . . ? O1 Ni3 Dy1 45.01(8) . . ? Ni1 Ni3 Dy1 64.168(15) . . ? Ni2 Ni3 Dy1 66.613(15) . . ? C1 N1 C5 118.6(4) . . ? C1 N1 Ni1 127.7(3) . . ? C5 N1 Ni1 113.6(3) . . ? C7 N2 C11 118.6(4) . . ? C7 N2 Ni1 129.8(3) . . ? C11 N2 Ni1 110.9(3) . . ? C17 N3 C13 119.0(4) . . ? C17 N3 Ni3 111.9(3) . . ? C13 N3 Ni3 129.1(3) . . ? C23 N4 C19 119.0(4) . . ? C23 N4 Ni3 112.0(3) . . ? C19 N4 Ni3 128.1(3) . . ? C6 O1 Ni1 110.3(2) . . ? C6 O1 Ni3 117.4(2) . . ? Ni1 O1 Ni3 96.55(12) . . ? C6 O1 Dy1 129.9(2) . . ? Ni1 O1 Dy1 101.56(11) . . ? Ni3 O1 Dy1 95.45(11) . . ? C12 O2 Ni1 107.9(2) . . ? C12 O2 Ni2 121.4(2) . . ? Ni1 O2 Ni2 92.21(11) . . ? C12 O2 Dy1 121.8(2) . . ? Ni1 O2 Dy1 101.32(11) . . ? Ni2 O2 Dy1 106.06(11) . . ? C18 O3 Ni3 110.7(2) . . ? C18 O3 Ni2 125.4(3) . . ? Ni3 O3 Ni2 101.76(12) . . ? C18 O3 Ni1 123.0(2) . . ? Ni3 O3 Ni1 99.64(12) . . ? Ni2 O3 Ni1 91.73(11) . . ? C24 O4 Ni3 111.4(2) . . ? C24 O4 Ni2 118.8(3) . . ? Ni3 O4 Ni2 96.25(11) . . ? C24 O4 Dy1 121.9(2) . . ? Ni3 O4 Dy1 98.84(12) . . ? Ni2 O4 Dy1 105.04(11) . . ? C25 O5 Ni1 125.1(3) . . ? C25 O6 Ni2 127.4(3) . . ? C27 O7 Ni3 124.8(3) . . ? C27 O8 Dy1 135.9(3) . . ? C29 O9 Dy1 90.5(3) . . ? C29 O10 Dy1 93.1(2) . . ? C31 O11 Dy1 91.4(3) . . ? C31 O12 Dy1 93.8(3) . . ? C33 O13 Ni2 127.3(3) . . ? N1 C1 C2 121.9(5) . . ? C3 C2 C1 119.6(5) . . ? C2 C3 C4 118.9(5) . . ? C5 C4 C3 119.2(5) . . ? N1 C5 C4 121.9(4) . . ? N1 C5 C6 115.9(4) . . ? C4 C5 C6 122.2(4) . . ? O1 C6 C5 111.2(3) . . ? N2 C7 C8 123.2(4) . . ? C9 C8 C7 117.8(4) . . ? C10 C9 C8 119.5(4) . . ? C9 C10 C11 119.3(4) . . ? N2 C11 C10 121.5(4) . . ? N2 C11 C12 115.9(3) . . ? C10 C11 C12 122.6(4) . . ? O2 C12 C11 109.5(3) . . ? N3 C13 C14 122.4(4) . . ? C15 C14 C13 118.3(5) . . ? C14 C15 C16 120.3(5) . . ? C15 C16 C17 118.6(5) . . ? N3 C17 C16 121.5(4) . . ? N3 C17 C18 115.9(4) . . ? C16 C17 C18 122.6(4) . . ? O3 C18 C17 109.9(3) . . ? N4 C19 C20 122.4(4) . . ? C21 C20 C19 119.0(4) . . ? C20 C21 C22 119.3(4) . . ? C21 C22 C23 118.5(4) . . ? N4 C23 C22 121.7(4) . . ? N4 C23 C24 117.7(4) . . ? C22 C23 C24 120.5(4) . . ? O4 C24 C23 111.3(3) . . ? O6 C25 O5 126.7(4) . . ? O6 C25 C26 117.9(4) . . ? O5 C25 C26 115.4(4) . . ? O8 C27 O7 125.2(4) . . ? O8 C27 C28 117.6(4) . . ? O7 C27 C28 117.2(4) . . ? O10 C29 O9 121.7(4) . . ? O10 C29 C30 117.9(4) . . ? O9 C29 C30 120.3(4) . . ? O12 C31 O11 120.6(4) . . ? O12 C31 C32 119.9(4) . . ? O11 C31 C32 119.4(4) . . ? O14 C33 O13 125.8(5) . . ? O14 C33 C34 118.0(5) . . ? O13 C33 C34 116.2(5) . . ? Cl2 C1S Cl1 110.2(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W O11 0.850(10) 2.01(3) 2.800(5) 155(6) . O1W H2W O14 0.850(10) 1.84(5) 2.599(5) 148(9) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.040 _refine_diff_density_min -0.886 _refine_diff_density_rms 0.144 _shelx_res_file ; TITL C065 in P-1 CELL 0.71073 10.6814 10.7905 18.8478 87.685 75.725 88.381 ZERR 2.00 0.0017 0.0017 0.0030 0.003 0.003 0.003 LATT 1 SFAC C H N O Ni Dy Cl UNIT 70 86 8 30 6 2 4 omit 1 0 0 omit 0 0 1 OMIT -1.00 55.00 L.S. 10 ACTA BOND FMAP 2 PLAN 20 BIND Ni1 Ni2 BIND Ni1 Ni3 BIND Ni2 Ni3 BIND Ni1 Dy1 BIND Ni2 Dy1 BIND Ni3 Dy1 FREE Dy1 C29 FREE Dy1 C31 SIZE 0.40 0.36 0.30 DFIX 0.85 0.01 O1W H1W O1W H2W HTAB O1W O11 HTAB O1W O14 HTAB TEMP -173 WGHT 0.046500 7.533300 FVAR 0.08318 DY1 6 0.134957 0.494302 0.215402 11.00000 0.02563 0.01760 = 0.01828 0.00056 -0.00732 -0.00131 NI1 5 0.209639 0.787801 0.143034 11.00000 0.02415 0.01712 = 0.01728 0.00274 -0.00804 -0.00334 NI2 5 -0.047701 0.777014 0.248788 11.00000 0.02314 0.01554 = 0.02893 -0.00093 -0.01191 -0.00022 NI3 5 0.202733 0.729622 0.307740 11.00000 0.02773 0.01635 = 0.01589 0.00076 -0.00692 -0.00011 N1 3 0.391230 0.855719 0.126905 11.00000 0.02917 0.02149 = 0.01706 0.00039 -0.00715 -0.00653 N2 3 0.242171 0.697102 0.044117 11.00000 0.02580 0.02270 = 0.01909 0.00199 -0.00742 -0.00277 N3 3 0.323731 0.876023 0.306288 11.00000 0.03177 0.02143 = 0.01627 -0.00341 -0.00735 0.00074 N4 3 0.090753 0.757403 0.413349 11.00000 0.03352 0.01936 = 0.01877 0.00068 -0.00704 0.00124 O1 4 0.285277 0.655362 0.203226 11.00000 0.02240 0.02040 = 0.01800 0.00132 -0.00536 -0.00040 O2 4 0.054170 0.673387 0.161952 11.00000 0.02464 0.01927 = 0.01799 0.00044 -0.00732 -0.00265 O3 4 0.127810 0.854218 0.246590 11.00000 0.02764 0.01511 = 0.02163 0.00051 -0.00858 -0.00065 O4 4 0.040700 0.631762 0.305127 11.00000 0.02820 0.02064 = 0.01616 0.00200 -0.00327 -0.00273 O5 4 0.123585 0.933222 0.100819 11.00000 0.03177 0.02258 = 0.02454 0.00388 -0.01104 -0.00251 O6 4 -0.075781 0.920934 0.176935 11.00000 0.03100 0.02116 = 0.03005 0.00486 -0.01151 -0.00077 O7 4 0.306476 0.600641 0.351831 11.00000 0.03879 0.02062 = 0.02225 -0.00154 -0.01395 0.00438 O8 4 0.249594 0.433762 0.301355 11.00000 0.04415 0.01794 = 0.02612 0.00113 -0.01699 -0.00042 O9 4 0.312857 0.391481 0.131132 11.00000 0.02790 0.03981 = 0.03243 -0.00862 -0.01082 -0.00013 O10 4 0.125398 0.410557 0.102333 11.00000 0.02756 0.03103 = 0.02539 -0.00466 -0.00847 0.00082 O11 4 -0.091538 0.438203 0.237009 11.00000 0.03187 0.02350 = 0.03187 -0.00242 -0.00666 -0.00336 O12 4 0.046307 0.296396 0.260708 11.00000 0.03451 0.02352 = 0.03281 0.00398 -0.01202 -0.00447 O13 4 -0.136948 0.863232 0.339729 11.00000 0.03128 0.03130 = 0.03169 -0.00187 -0.00595 -0.00070 O14 4 -0.312479 0.746613 0.379796 11.00000 0.03456 0.04029 = 0.03686 -0.00363 0.00145 -0.00351 C1 1 0.433028 0.968010 0.099507 11.00000 0.03979 0.02521 = 0.02703 0.00389 -0.01000 -0.00914 AFIX 43 H1 2 0.375867 1.023121 0.081756 11.00000 -1.20000 AFIX 0 C2 1 0.556783 1.005710 0.096388 11.00000 0.04846 0.03156 = 0.04871 0.00128 -0.01120 -0.02113 AFIX 43 H2 2 0.583874 1.085894 0.076984 11.00000 -1.20000 AFIX 0 C3 1 0.640348 0.926630 0.121489 11.00000 0.03543 0.03956 = 0.05128 -0.00450 -0.01398 -0.01629 AFIX 43 H3 2 0.725555 0.951489 0.120104 11.00000 -1.20000 AFIX 0 C4 1 0.598560 0.810304 0.148800 11.00000 0.02952 0.03668 = 0.02647 -0.00795 -0.01001 -0.00470 AFIX 43 H4 2 0.654948 0.753651 0.166086 11.00000 -1.20000 AFIX 0 C5 1 0.473903 0.777356 0.150678 11.00000 0.02914 0.02627 = 0.01531 -0.00280 -0.00589 -0.00409 C6 1 0.421583 0.651395 0.179311 11.00000 0.02124 0.02408 = 0.02194 0.00059 -0.00515 -0.00085 AFIX 23 H6A 2 0.448237 0.590759 0.140100 11.00000 -1.20000 H6B 2 0.458606 0.623295 0.220607 11.00000 -1.20000 AFIX 0 C7 1 0.350290 0.686650 -0.009310 11.00000 0.02653 0.02648 = 0.02297 0.00086 -0.00833 -0.00337 AFIX 43 H7 2 0.429392 0.710957 -0.000023 11.00000 -1.20000 AFIX 0 C8 1 0.352547 0.642019 -0.077660 11.00000 0.03102 0.02786 = 0.02226 0.00003 -0.00339 -0.00426 AFIX 43 H8 2 0.431459 0.632930 -0.113848 11.00000 -1.20000 AFIX 0 C9 1 0.235773 0.611138 -0.091366 11.00000 0.04025 0.02321 = 0.02010 -0.00038 -0.01034 -0.00423 AFIX 43 H9 2 0.232949 0.583586 -0.138175 11.00000 -1.20000 AFIX 0 C10 1 0.123903 0.620712 -0.036601 11.00000 0.03256 0.01829 = 0.02570 0.00115 -0.01348 -0.00367 AFIX 43 H10 2 0.043322 0.599443 -0.045185 11.00000 -1.20000 AFIX 0 C11 1 0.130197 0.661850 0.031393 11.00000 0.02846 0.01872 = 0.02032 0.00194 -0.00847 -0.00120 C12 1 0.013277 0.668395 0.095544 11.00000 0.02329 0.02509 = 0.02153 0.00027 -0.00732 -0.00395 AFIX 23 H12A 2 -0.039712 0.743117 0.089734 11.00000 -1.20000 H12B 2 -0.040403 0.594510 0.097246 11.00000 -1.20000 AFIX 0 C13 1 0.438942 0.876212 0.323733 11.00000 0.03794 0.02796 = 0.02464 -0.00556 -0.01545 -0.00118 AFIX 43 H13 2 0.474059 0.799918 0.337784 11.00000 -1.20000 AFIX 0 C14 1 0.507665 0.983469 0.321883 11.00000 0.04251 0.03545 = 0.04957 -0.01185 -0.02267 -0.00247 AFIX 43 H14 2 0.588955 0.981213 0.333980 11.00000 -1.20000 AFIX 0 C15 1 0.455421 1.093283 0.302120 11.00000 0.05299 0.02666 = 0.06450 -0.01238 -0.02767 -0.00817 AFIX 43 H15 2 0.500622 1.168287 0.300638 11.00000 -1.20000 AFIX 0 C16 1 0.336911 1.095182 0.284304 11.00000 0.04507 0.02015 = 0.04305 -0.00663 -0.01581 0.00025 AFIX 43 H16A 2 0.299893 1.170942 0.270923 11.00000 -1.20000 AFIX 0 C17 1 0.273539 0.984079 0.286438 11.00000 0.03506 0.01952 = 0.01863 -0.00423 -0.00748 0.00095 C18 1 0.145358 0.976115 0.266245 11.00000 0.03204 0.01644 = 0.02682 -0.00194 -0.00878 -0.00072 AFIX 23 H18A 2 0.074206 0.999533 0.308390 11.00000 -1.20000 H18B 2 0.143531 1.034716 0.224703 11.00000 -1.20000 AFIX 0 C19 1 0.113036 0.834343 0.463584 11.00000 0.03748 0.02325 = 0.02349 -0.00308 -0.00741 -0.00023 AFIX 43 H19 2 0.177413 0.895420 0.448377 11.00000 -1.20000 AFIX 0 C20 1 0.045618 0.827318 0.536142 11.00000 0.04709 0.03013 = 0.01953 -0.00561 -0.00791 0.00457 AFIX 43 H20 2 0.063007 0.882932 0.570185 11.00000 -1.20000 AFIX 0 C21 1 -0.047105 0.738599 0.558409 11.00000 0.04846 0.03130 = 0.01735 -0.00018 -0.00310 0.00206 AFIX 43 H21 2 -0.092785 0.730480 0.608398 11.00000 -1.20000 AFIX 0 C22 1 -0.073437 0.660596 0.506836 11.00000 0.04397 0.02629 = 0.02084 0.00181 -0.00127 -0.00358 AFIX 43 H22 2 -0.138605 0.600020 0.520793 11.00000 -1.20000 AFIX 0 C23 1 -0.001697 0.673561 0.434049 11.00000 0.03838 0.01996 = 0.02157 0.00002 -0.00640 0.00140 C24 1 -0.026178 0.590640 0.376152 11.00000 0.03583 0.02204 = 0.01764 0.00378 -0.00190 -0.00517 AFIX 23 H24A 2 0.002123 0.504717 0.385603 11.00000 -1.20000 H24B 2 -0.119990 0.590032 0.379100 11.00000 -1.20000 AFIX 0 C25 1 0.008224 0.971905 0.126516 11.00000 0.03808 0.01982 = 0.02873 0.00303 -0.01823 -0.00066 C26 1 -0.028259 1.092609 0.092519 11.00000 0.04526 0.02506 = 0.04264 0.01312 -0.01667 0.00065 AFIX 137 H26A 2 -0.120051 1.111471 0.113036 11.00000 -1.50000 H26B 2 -0.012178 1.085015 0.039377 11.00000 -1.50000 H26C 2 0.023807 1.159580 0.103106 11.00000 -1.50000 AFIX 0 C27 1 0.316110 0.487076 0.337014 11.00000 0.04225 0.02342 = 0.02345 -0.00142 -0.01616 0.00559 C28 1 0.414537 0.409778 0.364808 11.00000 0.09018 0.03365 = 0.07584 -0.02322 -0.06309 0.02660 AFIX 137 H28A 2 0.377872 0.329143 0.383425 11.00000 -1.50000 H28B 2 0.438320 0.452508 0.404353 11.00000 -1.50000 H28C 2 0.491554 0.397320 0.324754 11.00000 -1.50000 AFIX 0 C29 1 0.240489 0.370816 0.089305 11.00000 0.02862 0.02148 = 0.02549 -0.00338 -0.00829 -0.00113 C30 1 0.291846 0.301304 0.020326 11.00000 0.03145 0.05372 = 0.03771 -0.02042 -0.00715 0.00577 AFIX 137 H30A 2 0.219545 0.273851 0.001797 11.00000 -1.50000 H30B 2 0.342671 0.228916 0.030812 11.00000 -1.50000 H30C 2 0.346817 0.355807 -0.016623 11.00000 -1.50000 AFIX 0 C31 1 -0.066339 0.327785 0.256740 11.00000 0.03571 0.02488 = 0.01922 -0.00063 -0.00367 -0.00615 C32 1 -0.173317 0.234863 0.276785 11.00000 0.03774 0.03234 = 0.03758 0.00244 -0.00919 -0.01377 AFIX 137 H32A 2 -0.135933 0.151127 0.278465 11.00000 -1.50000 H32B 2 -0.224210 0.239833 0.239997 11.00000 -1.50000 H32C 2 -0.229314 0.253255 0.324918 11.00000 -1.50000 AFIX 0 C33 1 -0.236671 0.828208 0.387520 11.00000 0.03649 0.02945 = 0.03392 -0.00128 -0.00760 0.00414 C34 1 -0.264294 0.891984 0.460690 11.00000 0.05113 0.04760 = 0.04155 -0.01313 -0.00121 0.00057 AFIX 137 H34A 2 -0.324492 0.962023 0.460049 11.00000 -1.50000 H34B 2 -0.183424 0.922244 0.468743 11.00000 -1.50000 H34C 2 -0.302711 0.832654 0.500286 11.00000 -1.50000 AFIX 0 C1S 1 0.408903 0.674998 0.488900 11.00000 0.04653 0.03691 = 0.03185 0.00137 -0.01240 -0.01110 AFIX 23 H1S1 2 0.371228 0.693405 0.446536 11.00000 -1.20000 H1S2 2 0.499337 0.645997 0.470007 11.00000 -1.20000 AFIX 0 CL1 7 0.406191 0.810912 0.538503 11.00000 0.05420 0.03999 = 0.05312 -0.00820 -0.00823 -0.00097 CL2 7 0.319982 0.557752 0.545786 11.00000 0.05142 0.05106 = 0.05099 0.00721 -0.01101 -0.01935 O1W 4 -0.208793 0.674391 0.248014 11.00000 0.02754 0.02827 = 0.03062 0.00130 -0.00775 -0.00254 H1W 2 -0.196688 0.596341 0.250428 11.00000 0.04929 H2W 2 -0.256980 0.671804 0.291249 11.00000 0.09615 HKLF 4 REM C065 in P-1 REM R1 = 0.0382 for 9011 Fo > 4sig(Fo) and 0.0406 for all 9612 data REM 554 parameters refined using 2 restraints END WGHT 0.0465 7.5326 REM Highest difference peak 3.040, deepest hole -0.886, 1-sigma level 0.144 Q1 1 0.1936 0.5333 0.2238 11.00000 0.05 3.04 Q2 1 -0.0737 0.7620 0.2827 11.00000 0.05 2.84 Q3 1 -0.0599 0.8191 0.2503 11.00000 0.05 1.74 Q4 1 -0.0775 0.7779 0.2365 11.00000 0.05 1.62 Q5 1 0.0569 0.4534 0.2289 11.00000 0.05 1.44 Q6 1 0.0813 0.5560 0.2269 11.00000 0.05 1.33 Q7 1 0.2046 0.4377 0.2021 11.00000 0.05 1.07 Q8 1 0.2571 0.7620 0.3111 11.00000 0.05 0.87 Q9 1 0.1418 0.7898 0.1511 11.00000 0.05 0.81 Q10 1 0.2696 0.4566 0.1345 11.00000 0.05 0.81 Q11 1 0.1428 0.7516 0.3199 11.00000 0.05 0.70 Q12 1 0.1608 0.7772 0.3154 11.00000 0.05 0.66 Q13 1 0.2436 0.8138 0.1341 11.00000 0.05 0.61 Q14 1 0.2382 0.7612 0.1322 11.00000 0.05 0.59 Q15 1 0.2813 0.6444 -0.0862 11.00000 0.05 0.55 Q16 1 0.0401 0.3841 0.2622 11.00000 0.05 0.54 Q17 1 0.1147 0.3174 0.1289 11.00000 0.05 0.54 Q18 1 0.3522 0.6527 -0.0398 11.00000 0.05 0.53 Q19 1 0.2638 0.3379 0.0559 11.00000 0.05 0.53 Q20 1 0.1833 0.6220 -0.0623 11.00000 0.05 0.53 ; _database_code_depnum_ccdc_archive 'CCDC 955200' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c073 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H43 Cl2 Ho N4 Ni3 O15' _chemical_formula_weight 1171.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7144(6) _cell_length_b 10.7830(6) _cell_length_c 18.7998(10) _cell_angle_alpha 87.5680(10) _cell_angle_beta 75.6680(10) _cell_angle_gamma 89.1670(10) _cell_volume 2102.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4013 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 24.29 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.851 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 3.383 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6136 _exptl_absorpt_correction_T_max 0.7284 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27451 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_unetI/netI 0.0742 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9620 _reflns_number_gt 7937 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H atoms of the water were located from different map and refined with restraints in bond lengths. ; _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^)+(0.0477P)^2^+1.4570P] 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 9620 _refine_ls_number_parameters 554 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1148 _refine_ls_wR_factor_gt 0.1094 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 Ho1 Ho 0.13507(2) 0.49460(2) 0.215347(13) 0.01498(8) Uani 1 1 d . . . Ni1 Ni 0.21500(7) 0.78791(6) 0.14189(4) 0.01585(16) Uani 1 1 d . . . Ni2 Ni -0.04244(7) 0.77718(6) 0.24724(4) 0.01699(16) Uani 1 1 d . . . Ni3 Ni 0.20551(7) 0.72907(6) 0.30744(4) 0.01582(16) Uani 1 1 d . . . N1 N 0.3982(4) 0.8548(4) 0.1260(2) 0.0175(10) Uani 1 1 d . . . N2 N 0.2461(4) 0.6979(4) 0.0427(2) 0.0183(10) Uani 1 1 d . . . N3 N 0.3275(4) 0.8769(4) 0.3056(2) 0.0188(10) Uani 1 1 d . . . N4 N 0.0935(4) 0.7571(4) 0.4130(2) 0.0189(10) Uani 1 1 d . . . O1 O 0.2865(3) 0.6546(3) 0.20250(19) 0.0162(8) Uani 1 1 d . . . O2 O 0.0577(3) 0.6736(3) 0.16089(19) 0.0149(8) Uani 1 1 d . . . O3 O 0.1329(4) 0.8541(3) 0.2456(2) 0.0166(8) Uani 1 1 d . . . O4 O 0.0425(4) 0.6317(3) 0.3042(2) 0.0174(8) Uani 1 1 d . . . O5 O 0.1318(4) 0.9340(4) 0.0993(2) 0.0226(9) Uani 1 1 d . . . O6 O -0.0683(4) 0.9212(4) 0.1749(2) 0.0239(9) Uani 1 1 d . . . O7 O 0.3068(4) 0.5995(3) 0.3522(2) 0.0201(8) Uani 1 1 d . . . O8 O 0.2474(4) 0.4329(3) 0.3015(2) 0.0210(9) Uani 1 1 d . . . O9 O 0.3107(4) 0.3935(4) 0.1320(2) 0.0275(10) Uani 1 1 d . . . O10 O 0.1242(4) 0.4114(4) 0.1027(2) 0.0217(9) Uani 1 1 d . . . O11 O -0.0902(4) 0.4371(4) 0.2376(2) 0.0244(9) Uani 1 1 d . . . O12 O 0.0471(4) 0.2962(4) 0.2597(2) 0.0252(9) Uani 1 1 d . . . O13 O -0.1316(4) 0.8625(4) 0.3382(2) 0.0260(9) Uani 1 1 d . . . O14 O -0.3089(4) 0.7466(4) 0.3787(2) 0.0350(11) Uani 1 1 d . . . C1 C 0.4426(6) 0.9663(5) 0.0983(3) 0.0262(13) Uani 1 1 d . . . H1 H 0.3876 1.0223 0.0801 0.031 Uiso 1 1 calc R . . C2 C 0.5684(7) 1.0022(6) 0.0958(4) 0.0376(17) Uani 1 1 d . . . H2 H 0.5984 1.0819 0.0760 0.045 Uiso 1 1 calc R . . C3 C 0.6479(6) 0.9223(6) 0.1221(4) 0.0319(15) Uani 1 1 d . . . H3 H 0.7331 0.9463 0.1215 0.038 Uiso 1 1 calc R . . C4 C 0.6028(5) 0.8062(6) 0.1493(3) 0.0228(13) Uani 1 1 d . . . H4 H 0.6572 0.7485 0.1669 0.027 Uiso 1 1 calc R . . C5 C 0.4779(6) 0.7750(5) 0.1508(3) 0.0200(12) Uani 1 1 d . . . C6 C 0.4228(5) 0.6493(5) 0.1794(3) 0.0179(11) Uani 1 1 d . . . H6A H 0.4489 0.5887 0.1403 0.021 Uiso 1 1 calc R . . H6B H 0.4580 0.6207 0.2213 0.021 Uiso 1 1 calc R . . C7 C 0.3535(6) 0.6872(5) -0.0106(3) 0.0214(12) Uani 1 1 d . . . H7 H 0.4326 0.7115 -0.0012 0.026 Uiso 1 1 calc R . . C8 C 0.3562(6) 0.6426(5) -0.0790(3) 0.0244(13) Uani 1 1 d . . . H8 H 0.4351 0.6335 -0.1150 0.029 Uiso 1 1 calc R . . C9 C 0.2396(6) 0.6116(5) -0.0931(3) 0.0234(13) Uani 1 1 d . . . H9 H 0.2368 0.5838 -0.1399 0.028 Uiso 1 1 calc R . . C10 C 0.1282(6) 0.6215(5) -0.0385(3) 0.0194(12) Uani 1 1 d . . . H10 H 0.0476 0.6006 -0.0472 0.023 Uiso 1 1 calc R . . C11 C 0.1346(6) 0.6627(5) 0.0300(3) 0.0193(12) Uani 1 1 d . . . C12 C 0.0173(5) 0.6690(5) 0.0940(3) 0.0181(11) Uani 1 1 d . . . H12A H -0.0342 0.7438 0.0879 0.022 Uiso 1 1 calc R . . H12B H -0.0372 0.5951 0.0956 0.022 Uiso 1 1 calc R . . C13 C 0.4427(6) 0.8758(6) 0.3227(3) 0.0229(13) Uani 1 1 d . . . H13 H 0.4768 0.7989 0.3360 0.028 Uiso 1 1 calc R . . C14 C 0.5129(6) 0.9833(6) 0.3215(4) 0.0301(15) Uani 1 1 d . . . H14 H 0.5935 0.9810 0.3341 0.036 Uiso 1 1 calc R . . C15 C 0.4620(7) 1.0936(6) 0.3016(4) 0.0393(17) Uani 1 1 d . . . H15 H 0.5082 1.1687 0.2999 0.047 Uiso 1 1 calc R . . C16 C 0.3434(6) 1.0954(6) 0.2841(4) 0.0298(14) Uani 1 1 d . . . H16A H 0.3070 1.1715 0.2713 0.036 Uiso 1 1 calc R . . C17 C 0.2795(5) 0.9845(5) 0.2855(3) 0.0199(12) Uani 1 1 d . . . C18 C 0.1517(6) 0.9751(5) 0.2654(3) 0.0211(12) Uani 1 1 d . . . H18A H 0.0809 0.9977 0.3077 0.025 Uiso 1 1 calc R . . H18B H 0.1501 1.0341 0.2238 0.025 Uiso 1 1 calc R . . C19 C 0.1165(6) 0.8330(5) 0.4637(3) 0.0226(12) Uani 1 1 d . . . H19 H 0.1827 0.8933 0.4490 0.027 Uiso 1 1 calc R . . C20 C 0.0471(6) 0.8257(6) 0.5361(3) 0.0258(13) Uani 1 1 d . . . H20 H 0.0642 0.8817 0.5702 0.031 Uiso 1 1 calc R . . C21 C -0.0465(6) 0.7376(6) 0.5586(3) 0.0265(14) Uani 1 1 d . . . H21 H -0.0928 0.7295 0.6086 0.032 Uiso 1 1 calc R . . C22 C -0.0725(6) 0.6603(5) 0.5070(3) 0.0250(13) Uani 1 1 d . . . H22 H -0.1385 0.5997 0.5207 0.030 Uiso 1 1 calc R . . C23 C 0.0004(6) 0.6735(5) 0.4345(3) 0.0202(12) Uani 1 1 d . . . C24 C -0.0254(5) 0.5899(5) 0.3756(3) 0.0192(12) Uani 1 1 d . . . H24A H 0.0013 0.5038 0.3852 0.023 Uiso 1 1 calc R . . H24B H -0.1189 0.5895 0.3785 0.023 Uiso 1 1 calc R . . C25 C 0.0172(6) 0.9725(5) 0.1246(3) 0.0219(12) Uani 1 1 d . . . C26 C -0.0173(7) 1.0929(6) 0.0904(4) 0.0340(16) Uani 1 1 d . . . H26A H -0.1104 1.1069 0.1067 0.051 Uiso 1 1 calc R . . H26B H 0.0077 1.0887 0.0367 0.051 Uiso 1 1 calc R . . H26C H 0.0283 1.1613 0.1054 0.051 Uiso 1 1 calc R . . C27 C 0.3136(6) 0.4862(5) 0.3376(3) 0.0211(12) Uani 1 1 d . . . C28 C 0.4114(7) 0.4084(7) 0.3665(4) 0.0438(19) Uani 1 1 d . . . H28A H 0.3791 0.3235 0.3782 0.066 Uiso 1 1 calc R . . H28B H 0.4248 0.4445 0.4110 0.066 Uiso 1 1 calc R . . H28C H 0.4932 0.4069 0.3290 0.066 Uiso 1 1 calc R . . C29 C 0.2391(5) 0.3722(5) 0.0892(3) 0.0207(12) Uani 1 1 d . . . C30 C 0.2917(6) 0.3045(7) 0.0203(3) 0.0339(16) Uani 1 1 d . . . H30A H 0.2207 0.2802 -0.0004 0.051 Uiso 1 1 calc R . . H30B H 0.3382 0.2301 0.0315 0.051 Uiso 1 1 calc R . . H30C H 0.3508 0.3588 -0.0154 0.051 Uiso 1 1 calc R . . C31 C -0.0663(6) 0.3264(6) 0.2562(3) 0.0226(13) Uani 1 1 d . . . C32 C -0.1727(6) 0.2331(6) 0.2760(4) 0.0312(15) Uani 1 1 d . . . H32A H -0.1377 0.1522 0.2871 0.047 Uiso 1 1 calc R . . H32B H -0.2125 0.2265 0.2347 0.047 Uiso 1 1 calc R . . H32C H -0.2376 0.2597 0.3192 0.047 Uiso 1 1 calc R . . C33 C -0.2303(6) 0.8277(6) 0.3859(4) 0.0280(14) Uani 1 1 d . . . C34 C -0.2582(7) 0.8922(7) 0.4592(4) 0.0400(17) Uani 1 1 d . . . H34A H -0.3139 0.9645 0.4571 0.060 Uiso 1 1 calc R . . H34B H -0.1771 0.9193 0.4686 0.060 Uiso 1 1 calc R . . H34C H -0.3016 0.8342 0.4988 0.060 Uiso 1 1 calc R . . C1S C 0.4111(6) 0.6768(6) 0.4887(3) 0.0285(14) Uani 1 1 d . . . H1S1 H 0.5010 0.6485 0.4695 0.034 Uiso 1 1 calc R . . H1S2 H 0.3727 0.6938 0.4465 0.034 Uiso 1 1 calc R . . Cl1 Cl 0.40978(19) 0.81342(17) 0.53711(11) 0.0451(4) Uani 1 1 d . . . Cl2 Cl 0.32220(18) 0.55900(18) 0.54761(10) 0.0458(5) Uani 1 1 d . . . O1W O -0.2044(4) 0.6741(4) 0.2468(2) 0.0227(9) Uani 1 1 d D . . H1W H -0.191(7) 0.5969(18) 0.253(4) 0.05(2) Uiso 1 1 d D . . H2W H -0.237(7) 0.672(7) 0.2930(9) 0.05(3) Uiso 1 1 d 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 Ho1 0.02001(14) 0.01356(13) 0.01327(13) -0.00032(9) -0.00772(10) -0.00124(9) Ni1 0.0211(4) 0.0146(3) 0.0143(3) 0.0021(3) -0.0094(3) -0.0029(3) Ni2 0.0198(4) 0.0131(3) 0.0218(4) 0.0004(3) -0.0122(3) -0.0009(3) Ni3 0.0225(4) 0.0138(3) 0.0130(3) 0.0001(3) -0.0081(3) -0.0007(3) N1 0.022(2) 0.016(2) 0.016(2) 0.0001(18) -0.0069(19) -0.0053(19) N2 0.022(2) 0.018(2) 0.017(2) 0.0025(19) -0.010(2) -0.0019(19) N3 0.028(3) 0.016(2) 0.015(2) -0.0036(18) -0.009(2) -0.004(2) N4 0.025(3) 0.018(2) 0.013(2) 0.0029(18) -0.005(2) 0.002(2) O1 0.0172(19) 0.0173(19) 0.0156(19) 0.0016(15) -0.0071(15) 0.0008(15) O2 0.0181(19) 0.0148(19) 0.0141(18) 0.0008(15) -0.0085(15) -0.0011(15) O3 0.022(2) 0.0126(18) 0.0173(19) -0.0002(15) -0.0091(16) -0.0016(15) O4 0.022(2) 0.0161(19) 0.0145(19) -0.0015(15) -0.0044(16) -0.0012(15) O5 0.031(2) 0.021(2) 0.019(2) 0.0041(16) -0.0133(18) -0.0035(18) O6 0.025(2) 0.022(2) 0.029(2) 0.0034(18) -0.0154(19) -0.0016(17) O7 0.030(2) 0.018(2) 0.0151(19) -0.0015(16) -0.0108(17) 0.0013(17) O8 0.034(2) 0.016(2) 0.017(2) 0.0018(16) -0.0139(18) 0.0017(17) O9 0.027(2) 0.032(2) 0.028(2) -0.0099(19) -0.0125(19) -0.0006(19) O10 0.025(2) 0.025(2) 0.019(2) -0.0031(17) -0.0112(17) 0.0005(17) O11 0.026(2) 0.018(2) 0.030(2) -0.0042(17) -0.0070(18) -0.0033(17) O12 0.027(2) 0.022(2) 0.028(2) 0.0038(18) -0.0115(19) -0.0061(18) O13 0.026(2) 0.023(2) 0.029(2) -0.0006(18) -0.0063(19) -0.0014(18) O14 0.029(2) 0.038(3) 0.034(3) -0.004(2) -0.002(2) -0.003(2) C1 0.033(3) 0.022(3) 0.025(3) 0.002(2) -0.010(3) -0.004(3) C2 0.041(4) 0.030(4) 0.041(4) 0.007(3) -0.009(3) -0.019(3) C3 0.026(3) 0.032(4) 0.040(4) -0.005(3) -0.012(3) -0.010(3) C4 0.019(3) 0.032(3) 0.020(3) -0.006(2) -0.008(2) -0.005(2) C5 0.026(3) 0.026(3) 0.009(3) -0.004(2) -0.006(2) -0.002(2) C6 0.016(3) 0.021(3) 0.019(3) 0.000(2) -0.008(2) 0.000(2) C7 0.027(3) 0.019(3) 0.022(3) 0.006(2) -0.013(2) -0.003(2) C8 0.029(3) 0.024(3) 0.019(3) 0.001(2) -0.005(3) -0.005(3) C9 0.035(3) 0.024(3) 0.013(3) -0.002(2) -0.008(2) -0.004(3) C10 0.027(3) 0.016(3) 0.021(3) 0.003(2) -0.017(2) -0.003(2) C11 0.029(3) 0.014(3) 0.019(3) 0.002(2) -0.014(2) -0.003(2) C12 0.021(3) 0.020(3) 0.017(3) 0.000(2) -0.012(2) 0.000(2) C13 0.027(3) 0.028(3) 0.018(3) -0.006(2) -0.012(2) -0.002(3) C14 0.028(3) 0.031(4) 0.037(4) -0.012(3) -0.018(3) 0.001(3) C15 0.039(4) 0.029(4) 0.054(5) -0.011(3) -0.019(4) -0.005(3) C16 0.037(4) 0.017(3) 0.038(4) -0.007(3) -0.013(3) -0.003(3) C17 0.024(3) 0.017(3) 0.020(3) -0.005(2) -0.007(2) 0.000(2) C18 0.031(3) 0.014(3) 0.020(3) -0.001(2) -0.011(3) 0.002(2) C19 0.028(3) 0.020(3) 0.021(3) -0.002(2) -0.007(2) 0.004(2) C20 0.035(4) 0.029(3) 0.015(3) -0.004(2) -0.009(3) 0.003(3) C21 0.039(4) 0.026(3) 0.015(3) -0.004(2) -0.007(3) 0.002(3) C22 0.036(4) 0.018(3) 0.020(3) 0.000(2) -0.005(3) -0.001(3) C23 0.029(3) 0.016(3) 0.015(3) 0.001(2) -0.005(2) 0.003(2) C24 0.022(3) 0.019(3) 0.016(3) 0.000(2) -0.005(2) -0.002(2) C25 0.030(3) 0.014(3) 0.027(3) 0.001(2) -0.017(3) -0.001(2) C26 0.046(4) 0.023(3) 0.037(4) 0.006(3) -0.018(3) 0.003(3) C27 0.030(3) 0.020(3) 0.017(3) 0.002(2) -0.013(2) 0.001(2) C28 0.060(5) 0.035(4) 0.052(5) -0.016(3) -0.042(4) 0.020(4) C29 0.021(3) 0.019(3) 0.022(3) 0.001(2) -0.005(2) -0.002(2) C30 0.026(3) 0.048(4) 0.029(4) -0.009(3) -0.009(3) 0.005(3) C31 0.026(3) 0.029(3) 0.013(3) -0.002(2) -0.005(2) -0.006(3) C32 0.028(3) 0.033(4) 0.032(4) 0.003(3) -0.007(3) -0.014(3) C33 0.027(3) 0.027(3) 0.033(4) -0.007(3) -0.011(3) 0.008(3) C34 0.041(4) 0.038(4) 0.040(4) -0.018(3) -0.007(3) 0.005(3) C1S 0.035(4) 0.031(3) 0.022(3) 0.002(3) -0.011(3) -0.006(3) Cl1 0.0487(11) 0.0349(10) 0.0509(11) -0.0109(8) -0.0096(9) -0.0004(8) Cl2 0.0450(11) 0.0485(11) 0.0447(11) 0.0066(9) -0.0129(9) -0.0182(9) O1W 0.023(2) 0.023(2) 0.024(2) 0.0012(18) -0.0100(19) -0.0007(18) _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 Ho1 O4 2.304(4) . ? Ho1 O8 2.315(4) . ? Ho1 O1 2.349(4) . ? Ho1 O10 2.364(4) . ? Ho1 O2 2.380(3) . ? Ho1 O12 2.383(4) . ? Ho1 O9 2.411(4) . ? Ho1 O11 2.430(4) . ? Ho1 Ni3 3.3216(7) . ? Ho1 Ni1 3.4302(7) . ? Ho1 Ni2 3.5614(7) . ? Ni1 O5 2.031(4) . ? Ni1 N1 2.048(4) . ? Ni1 O2 2.052(4) . ? Ni1 O1 2.053(4) . ? Ni1 O3 2.083(4) . ? Ni1 N2 2.089(5) . ? Ni1 Ni2 2.9714(10) . ? Ni1 Ni3 3.1268(9) . ? Ni2 O13 1.996(4) . ? Ni2 O3 2.057(4) . ? Ni2 O2 2.072(4) . ? Ni2 O1W 2.076(4) . ? Ni2 O6 2.082(4) . ? Ni2 O4 2.176(4) . ? Ni2 Ni3 3.1632(10) . ? Ni3 O3 2.014(4) . ? Ni3 O7 2.036(4) . ? Ni3 O4 2.065(4) . ? Ni3 N3 2.070(4) . ? Ni3 N4 2.082(4) . ? Ni3 O1 2.135(4) . ? N1 C1 1.336(7) . ? N1 C5 1.352(7) . ? N2 C7 1.333(7) . ? N2 C11 1.338(7) . ? N3 C17 1.340(7) . ? N3 C13 1.350(7) . ? N4 C23 1.330(7) . ? N4 C19 1.351(7) . ? O1 C6 1.418(6) . ? O2 C12 1.431(6) . ? O3 C18 1.403(6) . ? O4 C24 1.418(6) . ? O5 C25 1.272(7) . ? O6 C25 1.257(7) . ? O7 C27 1.260(6) . ? O8 C27 1.257(7) . ? O9 C29 1.271(7) . ? O10 C29 1.264(7) . ? O11 C31 1.270(7) . ? O12 C31 1.270(7) . ? O13 C33 1.255(7) . ? O14 C33 1.257(7) . ? C1 C2 1.396(9) . ? C2 C3 1.365(9) . ? C3 C4 1.380(8) . ? C4 C5 1.379(8) . ? C5 C6 1.509(8) . ? C7 C8 1.385(8) . ? C8 C9 1.388(8) . ? C9 C10 1.374(8) . ? C10 C11 1.397(7) . ? C11 C12 1.512(8) . ? C13 C14 1.388(8) . ? C14 C15 1.376(9) . ? C15 C16 1.389(9) . ? C16 C17 1.383(8) . ? C17 C18 1.514(8) . ? C19 C20 1.379(8) . ? C20 C21 1.368(9) . ? C21 C22 1.387(8) . ? C22 C23 1.396(8) . ? C23 C24 1.535(8) . ? C25 C26 1.506(8) . ? C27 C28 1.521(8) . ? C29 C30 1.494(8) . ? C31 C32 1.497(8) . ? C33 C34 1.531(9) . ? C1S Cl1 1.763(6) . ? C1S Cl2 1.772(6) . ? 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 Ho1 O8 82.24(13) . . ? O4 Ho1 O1 75.16(13) . . ? O8 Ho1 O1 77.98(13) . . ? O4 Ho1 O10 145.06(13) . . ? O8 Ho1 O10 132.04(13) . . ? O1 Ho1 O10 113.76(13) . . ? O4 Ho1 O2 69.74(12) . . ? O8 Ho1 O2 142.49(12) . . ? O1 Ho1 O2 71.23(12) . . ? O10 Ho1 O2 81.11(13) . . ? O4 Ho1 O12 106.06(13) . . ? O8 Ho1 O12 76.25(13) . . ? O1 Ho1 O12 153.74(13) . . ? O10 Ho1 O12 80.71(14) . . ? O2 Ho1 O12 134.47(13) . . ? O4 Ho1 O9 155.46(13) . . ? O8 Ho1 O9 83.10(14) . . ? O1 Ho1 O9 82.60(13) . . ? O10 Ho1 O9 54.96(13) . . ? O2 Ho1 O9 112.85(13) . . ? O12 Ho1 O9 89.36(14) . . ? O4 Ho1 O11 79.59(13) . . ? O8 Ho1 O11 118.67(14) . . ? O1 Ho1 O11 147.47(13) . . ? O10 Ho1 O11 77.16(13) . . ? O2 Ho1 O11 81.03(13) . . ? O12 Ho1 O11 54.32(14) . . ? O9 Ho1 O11 124.84(13) . . ? O4 Ho1 Ni3 37.90(9) . . ? O8 Ho1 Ni3 66.96(9) . . ? O1 Ho1 Ni3 39.78(9) . . ? O10 Ho1 Ni3 149.63(10) . . ? O2 Ho1 Ni3 75.66(8) . . ? O12 Ho1 Ni3 129.64(10) . . ? O9 Ho1 Ni3 117.73(10) . . ? O11 Ho1 Ni3 117.43(9) . . ? O4 Ho1 Ni1 72.90(9) . . ? O8 Ho1 Ni1 112.76(9) . . ? O1 Ho1 Ni1 35.81(9) . . ? O10 Ho1 Ni1 94.74(10) . . ? O2 Ho1 Ni1 35.95(9) . . ? O12 Ho1 Ni1 170.37(10) . . ? O9 Ho1 Ni1 94.99(10) . . ? O11 Ho1 Ni1 116.49(10) . . ? Ni3 Ho1 Ni1 55.146(17) . . ? O4 Ho1 Ni2 36.13(9) . . ? O8 Ho1 Ni2 116.37(9) . . ? O1 Ho1 Ni2 73.22(9) . . ? O10 Ho1 Ni2 111.46(9) . . ? O2 Ho1 Ni2 33.99(8) . . ? O12 Ho1 Ni2 123.53(10) . . ? O9 Ho1 Ni2 143.93(10) . . ? O11 Ho1 Ni2 74.29(9) . . ? Ni3 Ho1 Ni2 54.583(17) . . ? Ni1 Ho1 Ni2 50.258(17) . . ? O5 Ni1 N1 99.78(17) . . ? O5 Ni1 O2 95.90(15) . . ? N1 Ni1 O2 163.55(16) . . ? O5 Ni1 O1 169.83(15) . . ? N1 Ni1 O1 81.19(16) . . ? O2 Ni1 O1 84.27(14) . . ? O5 Ni1 O3 87.75(15) . . ? N1 Ni1 O3 99.74(16) . . ? O2 Ni1 O3 85.77(14) . . ? O1 Ni1 O3 82.12(14) . . ? O5 Ni1 N2 90.78(16) . . ? N1 Ni1 N2 96.55(18) . . ? O2 Ni1 N2 78.19(16) . . ? O1 Ni1 N2 99.19(16) . . ? O3 Ni1 N2 163.66(17) . . ? O5 Ni1 Ni2 81.67(12) . . ? N1 Ni1 Ni2 143.53(13) . . ? O2 Ni1 Ni2 44.17(10) . . ? O1 Ni1 Ni2 91.54(10) . . ? O3 Ni1 Ni2 43.79(10) . . ? N2 Ni1 Ni2 119.92(13) . . ? O5 Ni1 Ni3 127.14(11) . . ? N1 Ni1 Ni3 89.86(12) . . ? O2 Ni1 Ni3 84.61(10) . . ? O1 Ni1 Ni3 42.71(10) . . ? O3 Ni1 Ni3 39.44(10) . . ? N2 Ni1 Ni3 139.90(13) . . ? Ni2 Ni1 Ni3 62.43(2) . . ? O5 Ni1 Ho1 138.78(11) . . ? N1 Ni1 Ho1 121.37(13) . . ? O2 Ni1 Ho1 42.90(10) . . ? O1 Ni1 Ho1 42.03(10) . . ? O3 Ni1 Ho1 87.68(10) . . ? N2 Ni1 Ho1 82.72(12) . . ? Ni2 Ni1 Ho1 67.161(19) . . ? Ni3 Ni1 Ho1 60.664(17) . . ? O13 Ni2 O3 92.90(16) . . ? O13 Ni2 O2 173.22(15) . . ? O3 Ni2 O2 85.93(14) . . ? O13 Ni2 O1W 92.79(17) . . ? O3 Ni2 O1W 171.29(16) . . ? O2 Ni2 O1W 87.64(16) . . ? O13 Ni2 O6 95.48(16) . . ? O3 Ni2 O6 87.78(15) . . ? O2 Ni2 O6 91.15(15) . . ? O1W Ni2 O6 98.23(16) . . ? O13 Ni2 O4 95.08(15) . . ? O3 Ni2 O4 78.69(14) . . ? O2 Ni2 O4 78.14(14) . . ? O1W Ni2 O4 94.24(15) . . ? O6 Ni2 O4 163.22(15) . . ? O13 Ni2 Ni1 136.66(12) . . ? O3 Ni2 Ni1 44.47(10) . . ? O2 Ni2 Ni1 43.65(10) . . ? O1W Ni2 Ni1 130.50(12) . . ? O6 Ni2 Ni1 78.42(12) . . ? O4 Ni2 Ni1 84.96(10) . . ? O13 Ni2 Ni3 91.56(12) . . ? O3 Ni2 Ni3 38.52(10) . . ? O2 Ni2 Ni3 83.36(10) . . ? O1W Ni2 Ni3 134.68(12) . . ? O6 Ni2 Ni3 126.18(11) . . ? O4 Ni2 Ni3 40.45(10) . . ? Ni1 Ni2 Ni3 61.19(2) . . ? O13 Ni2 Ho1 133.30(12) . . ? O3 Ni2 Ho1 84.56(10) . . ? O2 Ni2 Ho1 39.96(10) . . ? O1W Ni2 Ho1 86.74(12) . . ? O6 Ni2 Ho1 130.85(12) . . ? O4 Ni2 Ho1 38.63(9) . . ? Ni1 Ni2 Ho1 62.580(19) . . ? Ni3 Ni2 Ho1 58.846(17) . . ? O3 Ni3 O7 169.00(15) . . ? O3 Ni3 O4 82.35(15) . . ? O7 Ni3 O4 101.99(15) . . ? O3 Ni3 N3 79.93(17) . . ? O7 Ni3 N3 97.05(17) . . ? O4 Ni3 N3 160.15(17) . . ? O3 Ni3 N4 102.83(16) . . ? O7 Ni3 N4 87.94(16) . . ? O4 Ni3 N4 80.10(17) . . ? N3 Ni3 N4 95.16(18) . . ? O3 Ni3 O1 81.75(14) . . ? O7 Ni3 O1 88.52(14) . . ? O4 Ni3 O1 85.02(14) . . ? N3 Ni3 O1 101.13(16) . . ? N4 Ni3 O1 163.64(17) . . ? O3 Ni3 Ni1 41.07(10) . . ? O7 Ni3 Ni1 128.88(11) . . ? O4 Ni3 Ni1 82.83(10) . . ? N3 Ni3 Ni1 89.60(13) . . ? N4 Ni3 Ni1 142.03(13) . . ? O1 Ni3 Ni1 40.71(10) . . ? O3 Ni3 Ni2 39.51(10) . . ? O7 Ni3 Ni2 144.90(11) . . ? O4 Ni3 Ni2 43.13(10) . . ? N3 Ni3 Ni2 118.05(13) . . ? N4 Ni3 Ni2 88.81(13) . . ? O1 Ni3 Ni2 84.93(10) . . ? Ni1 Ni3 Ni2 56.38(2) . . ? O3 Ni3 Ho1 91.87(10) . . ? O7 Ni3 Ho1 84.73(10) . . ? O4 Ni3 Ho1 43.28(10) . . ? N3 Ni3 Ho1 145.87(13) . . ? N4 Ni3 Ho1 118.96(13) . . ? O1 Ni3 Ho1 44.76(10) . . ? Ni1 Ni3 Ho1 64.191(18) . . ? Ni2 Ni3 Ho1 66.570(19) . . ? C1 N1 C5 118.9(5) . . ? C1 N1 Ni1 127.8(4) . . ? C5 N1 Ni1 113.1(4) . . ? C7 N2 C11 118.5(5) . . ? C7 N2 Ni1 129.8(4) . . ? C11 N2 Ni1 111.0(4) . . ? C17 N3 C13 119.5(5) . . ? C17 N3 Ni3 112.4(4) . . ? C13 N3 Ni3 128.2(4) . . ? C23 N4 C19 118.1(5) . . ? C23 N4 Ni3 112.4(4) . . ? C19 N4 Ni3 128.5(4) . . ? C6 O1 Ni1 110.7(3) . . ? C6 O1 Ni3 116.8(3) . . ? Ni1 O1 Ni3 96.58(15) . . ? C6 O1 Ho1 129.5(3) . . ? Ni1 O1 Ho1 102.16(15) . . ? Ni3 O1 Ho1 95.47(14) . . ? C12 O2 Ni1 107.9(3) . . ? C12 O2 Ni2 121.3(3) . . ? Ni1 O2 Ni2 92.19(14) . . ? C12 O2 Ho1 122.0(3) . . ? Ni1 O2 Ho1 101.15(14) . . ? Ni2 O2 Ho1 106.05(14) . . ? C18 O3 Ni3 110.5(3) . . ? C18 O3 Ni2 125.3(3) . . ? Ni3 O3 Ni2 101.97(16) . . ? C18 O3 Ni1 123.2(3) . . ? Ni3 O3 Ni1 99.49(15) . . ? Ni2 O3 Ni1 91.74(14) . . ? C24 O4 Ni3 111.2(3) . . ? C24 O4 Ni2 118.9(3) . . ? Ni3 O4 Ni2 96.42(15) . . ? C24 O4 Ho1 121.6(3) . . ? Ni3 O4 Ho1 98.82(15) . . ? Ni2 O4 Ho1 105.25(15) . . ? C25 O5 Ni1 125.2(4) . . ? C25 O6 Ni2 126.9(4) . . ? C27 O7 Ni3 124.4(3) . . ? C27 O8 Ho1 135.7(3) . . ? C29 O9 Ho1 90.9(3) . . ? C29 O10 Ho1 93.3(3) . . ? C31 O11 Ho1 91.8(3) . . ? C31 O12 Ho1 93.9(3) . . ? C33 O13 Ni2 127.9(4) . . ? N1 C1 C2 121.3(6) . . ? C3 C2 C1 119.7(6) . . ? C2 C3 C4 119.1(6) . . ? C5 C4 C3 119.2(6) . . ? N1 C5 C4 121.9(5) . . ? N1 C5 C6 116.3(5) . . ? C4 C5 C6 121.9(5) . . ? O1 C6 C5 111.0(4) . . ? N2 C7 C8 123.6(5) . . ? C7 C8 C9 117.7(6) . . ? C10 C9 C8 119.3(5) . . ? C9 C10 C11 119.4(5) . . ? N2 C11 C10 121.5(5) . . ? N2 C11 C12 116.2(5) . . ? C10 C11 C12 122.3(5) . . ? O2 C12 C11 109.3(4) . . ? N3 C13 C14 122.2(6) . . ? C15 C14 C13 117.9(6) . . ? C14 C15 C16 120.2(6) . . ? C17 C16 C15 118.8(6) . . ? N3 C17 C16 121.4(5) . . ? N3 C17 C18 115.3(5) . . ? C16 C17 C18 123.3(5) . . ? O3 C18 C17 110.4(4) . . ? N4 C19 C20 122.2(6) . . ? C21 C20 C19 119.7(6) . . ? C20 C21 C22 118.8(5) . . ? C21 C22 C23 118.5(6) . . ? N4 C23 C22 122.7(5) . . ? N4 C23 C24 117.1(5) . . ? C22 C23 C24 120.2(5) . . ? O4 C24 C23 111.3(4) . . ? O6 C25 O5 126.9(5) . . ? O6 C25 C26 117.5(5) . . ? O5 C25 C26 115.6(5) . . ? O8 C27 O7 125.8(5) . . ? O8 C27 C28 117.8(5) . . ? O7 C27 C28 116.5(5) . . ? O10 C29 O9 120.7(5) . . ? O10 C29 C30 119.0(5) . . ? O9 C29 C30 120.2(5) . . ? O11 C31 O12 119.8(5) . . ? O11 C31 C32 119.8(5) . . ? O12 C31 C32 120.4(6) . . ? O13 C33 O14 126.2(6) . . ? O13 C33 C34 116.6(6) . . ? O14 C33 C34 117.2(6) . . ? Cl1 C1S Cl2 110.0(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H2W O14 0.851(10) 1.82(4) 2.604(6) 152(8) . O1W H1W O11 0.851(10) 2.02(3) 2.811(6) 155(7) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.387 _refine_diff_density_min -1.221 _refine_diff_density_rms 0.174 _shelx_res_file ; TITL C073 in P-1 CELL 0.71073 10.7144 10.7830 18.7998 87.568 75.668 89.167 ZERR 2.00 0.0006 0.0006 0.0010 0.001 0.001 0.001 LATT 1 SFAC C H N O Ni Ho Cl UNIT 70 86 8 30 6 2 4 OMIT 0 0 1 OMIT 0 0 2 OMIT 0 1 0 OMIT 1 0 1 OMIT -1.00 55.00 L.S. 10 ACTA BOND FMAP 2 PLAN 20 BIND Ni1 Ni2 BIND Ni1 Ni3 BIND Ni2 Ni3 BIND Ni1 Ho1 BIND Ni2 Ho1 BIND Ni3 Ho1 FREE Ho1 C29 FREE Ho1 C31 HTAB HTAB O1W O14 HTAB O1W O11 DFIX 0.85 0.01 O1W H1W O1W H2W SIZE 0.16 0.10 0.10 TEMP -173 WGHT 0.047700 1.457000 FVAR 0.08146 HO1 6 0.135068 0.494598 0.215347 11.00000 0.02001 0.01356 = 0.01327 -0.00032 -0.00772 -0.00124 NI1 5 0.215002 0.787913 0.141894 11.00000 0.02114 0.01459 = 0.01433 0.00206 -0.00941 -0.00292 NI2 5 -0.042435 0.777183 0.247243 11.00000 0.01977 0.01310 = 0.02176 0.00039 -0.01219 -0.00090 NI3 5 0.205508 0.729069 0.307441 11.00000 0.02247 0.01384 = 0.01305 0.00012 -0.00806 -0.00065 N1 3 0.398214 0.854781 0.125984 11.00000 0.02201 0.01611 = 0.01552 0.00014 -0.00688 -0.00533 N2 3 0.246073 0.697935 0.042717 11.00000 0.02226 0.01846 = 0.01670 0.00248 -0.00983 -0.00189 N3 3 0.327463 0.876929 0.305649 11.00000 0.02750 0.01607 = 0.01503 -0.00361 -0.00852 -0.00398 N4 3 0.093543 0.757147 0.413042 11.00000 0.02547 0.01771 = 0.01327 0.00289 -0.00493 0.00217 O1 4 0.286539 0.654569 0.202498 11.00000 0.01717 0.01734 = 0.01559 0.00164 -0.00715 0.00083 O2 4 0.057734 0.673562 0.160889 11.00000 0.01811 0.01484 = 0.01408 0.00079 -0.00852 -0.00110 O3 4 0.132887 0.854052 0.245646 11.00000 0.02214 0.01257 = 0.01731 -0.00018 -0.00909 -0.00156 O4 4 0.042548 0.631737 0.304248 11.00000 0.02179 0.01607 = 0.01446 -0.00152 -0.00437 -0.00122 O5 4 0.131799 0.934045 0.099272 11.00000 0.03125 0.02103 = 0.01901 0.00411 -0.01328 -0.00349 O6 4 -0.068279 0.921153 0.174864 11.00000 0.02477 0.02238 = 0.02890 0.00339 -0.01543 -0.00164 O7 4 0.306761 0.599502 0.352235 11.00000 0.02977 0.01827 = 0.01510 -0.00148 -0.01085 0.00132 O8 4 0.247351 0.432939 0.301462 11.00000 0.03384 0.01619 = 0.01687 0.00180 -0.01393 0.00173 O9 4 0.310749 0.393532 0.131955 11.00000 0.02655 0.03178 = 0.02788 -0.00988 -0.01252 -0.00060 O10 4 0.124238 0.411383 0.102703 11.00000 0.02533 0.02458 = 0.01853 -0.00311 -0.01120 0.00049 O11 4 -0.090167 0.437081 0.237573 11.00000 0.02561 0.01848 = 0.02970 -0.00418 -0.00697 -0.00335 O12 4 0.047100 0.296166 0.259724 11.00000 0.02733 0.02245 = 0.02819 0.00375 -0.01152 -0.00609 O13 4 -0.131560 0.862479 0.338231 11.00000 0.02631 0.02257 = 0.02891 -0.00061 -0.00631 -0.00140 O14 4 -0.308898 0.746591 0.378697 11.00000 0.02944 0.03842 = 0.03403 -0.00357 -0.00157 -0.00280 C1 1 0.442649 0.966339 0.098349 11.00000 0.03302 0.02150 = 0.02529 0.00183 -0.00977 -0.00419 AFIX 43 H1 2 0.387627 1.022314 0.080058 11.00000 -1.20000 AFIX 0 C2 1 0.568356 1.002238 0.095832 11.00000 0.04083 0.03037 = 0.04103 0.00680 -0.00945 -0.01914 AFIX 43 H2 2 0.598396 1.081908 0.075956 11.00000 -1.20000 AFIX 0 C3 1 0.647906 0.922339 0.122059 11.00000 0.02648 0.03179 = 0.04000 -0.00463 -0.01198 -0.00954 AFIX 43 H3 2 0.733105 0.946318 0.121540 11.00000 -1.20000 AFIX 0 C4 1 0.602834 0.806208 0.149349 11.00000 0.01876 0.03194 = 0.01966 -0.00597 -0.00763 -0.00510 AFIX 43 H4 2 0.657216 0.748543 0.166914 11.00000 -1.20000 AFIX 0 C5 1 0.477901 0.774951 0.150794 11.00000 0.02623 0.02637 = 0.00855 -0.00394 -0.00593 -0.00237 C6 1 0.422840 0.649338 0.179411 11.00000 0.01573 0.02076 = 0.01928 -0.00033 -0.00832 0.00041 AFIX 23 H6A 2 0.448872 0.588710 0.140288 11.00000 -1.20000 H6B 2 0.458025 0.620723 0.221289 11.00000 -1.20000 AFIX 0 C7 1 0.353523 0.687198 -0.010600 11.00000 0.02678 0.01902 = 0.02159 0.00575 -0.01306 -0.00297 AFIX 43 H7 2 0.432595 0.711473 -0.001166 11.00000 -1.20000 AFIX 0 C8 1 0.356189 0.642589 -0.078996 11.00000 0.02935 0.02392 = 0.01920 0.00099 -0.00462 -0.00539 AFIX 43 H8 2 0.435092 0.633522 -0.115010 11.00000 -1.20000 AFIX 0 C9 1 0.239563 0.611611 -0.093060 11.00000 0.03489 0.02438 = 0.01259 -0.00167 -0.00841 -0.00373 AFIX 43 H9 2 0.236764 0.583844 -0.139924 11.00000 -1.20000 AFIX 0 C10 1 0.128221 0.621534 -0.038484 11.00000 0.02680 0.01620 = 0.02086 0.00280 -0.01701 -0.00279 AFIX 43 H10 2 0.047628 0.600608 -0.047217 11.00000 -1.20000 AFIX 0 C11 1 0.134633 0.662704 0.030006 11.00000 0.02915 0.01449 = 0.01852 0.00164 -0.01392 -0.00295 C12 1 0.017340 0.668985 0.093988 11.00000 0.02083 0.02008 = 0.01722 -0.00047 -0.01197 -0.00044 AFIX 23 H12A 2 -0.034199 0.743837 0.087886 11.00000 -1.20000 H12B 2 -0.037217 0.595088 0.095628 11.00000 -1.20000 AFIX 0 C13 1 0.442696 0.875829 0.322721 11.00000 0.02731 0.02761 = 0.01759 -0.00632 -0.01160 -0.00202 AFIX 43 H13 2 0.476835 0.798912 0.335972 11.00000 -1.20000 AFIX 0 C14 1 0.512898 0.983347 0.321549 11.00000 0.02831 0.03126 = 0.03697 -0.01206 -0.01802 0.00080 AFIX 43 H14 2 0.593539 0.980955 0.334092 11.00000 -1.20000 AFIX 0 C15 1 0.462016 1.093571 0.301643 11.00000 0.03924 0.02915 = 0.05448 -0.01138 -0.01901 -0.00519 AFIX 43 H15 2 0.508154 1.168663 0.299909 11.00000 -1.20000 AFIX 0 C16 1 0.343448 1.095427 0.284077 11.00000 0.03660 0.01718 = 0.03802 -0.00678 -0.01272 -0.00270 AFIX 43 H16A 2 0.306983 1.171452 0.271328 11.00000 -1.20000 AFIX 0 C17 1 0.279496 0.984525 0.285497 11.00000 0.02431 0.01668 = 0.01977 -0.00461 -0.00673 -0.00023 C18 1 0.151676 0.975120 0.265356 11.00000 0.03114 0.01403 = 0.02028 -0.00058 -0.01050 0.00205 AFIX 23 H18A 2 0.080930 0.997727 0.307701 11.00000 -1.20000 H18B 2 0.150079 1.034111 0.223775 11.00000 -1.20000 AFIX 0 C19 1 0.116540 0.832989 0.463724 11.00000 0.02751 0.01967 = 0.02116 -0.00234 -0.00710 0.00385 AFIX 43 H19 2 0.182683 0.893284 0.449027 11.00000 -1.20000 AFIX 0 C20 1 0.047122 0.825730 0.536106 11.00000 0.03540 0.02889 = 0.01485 -0.00420 -0.00938 0.00345 AFIX 43 H20 2 0.064228 0.881693 0.570190 11.00000 -1.20000 AFIX 0 C21 1 -0.046457 0.737594 0.558590 11.00000 0.03923 0.02556 = 0.01506 -0.00363 -0.00677 0.00194 AFIX 43 H21 2 -0.092768 0.729502 0.608646 11.00000 -1.20000 AFIX 0 C22 1 -0.072518 0.660265 0.507011 11.00000 0.03603 0.01823 = 0.01973 0.00036 -0.00524 -0.00099 AFIX 43 H22 2 -0.138514 0.599652 0.520710 11.00000 -1.20000 AFIX 0 C23 1 0.000406 0.673506 0.434520 11.00000 0.02902 0.01577 = 0.01526 0.00116 -0.00488 0.00321 C24 1 -0.025409 0.589937 0.375649 11.00000 0.02243 0.01913 = 0.01602 0.00049 -0.00465 -0.00213 AFIX 23 H24A 2 0.001336 0.503832 0.385213 11.00000 -1.20000 H24B 2 -0.118905 0.589531 0.378477 11.00000 -1.20000 AFIX 0 C25 1 0.017231 0.972519 0.124593 11.00000 0.03029 0.01401 = 0.02650 0.00112 -0.01717 -0.00058 C26 1 -0.017319 1.092868 0.090356 11.00000 0.04572 0.02285 = 0.03685 0.00614 -0.01822 0.00343 AFIX 137 H26A 2 -0.110440 1.106879 0.106668 11.00000 -1.50000 H26B 2 0.007725 1.088697 0.036718 11.00000 -1.50000 H26C 2 0.028277 1.161334 0.105406 11.00000 -1.50000 AFIX 0 C27 1 0.313648 0.486240 0.337617 11.00000 0.03043 0.01974 = 0.01650 0.00165 -0.01267 0.00140 C28 1 0.411387 0.408374 0.366506 11.00000 0.05975 0.03463 = 0.05249 -0.01640 -0.04181 0.02029 AFIX 137 H28A 2 0.379089 0.323479 0.378162 11.00000 -1.50000 H28B 2 0.424836 0.444534 0.410967 11.00000 -1.50000 H28C 2 0.493203 0.406942 0.328999 11.00000 -1.50000 AFIX 0 C29 1 0.239129 0.372154 0.089160 11.00000 0.02062 0.01876 = 0.02249 0.00120 -0.00530 -0.00208 C30 1 0.291730 0.304482 0.020307 11.00000 0.02562 0.04848 = 0.02920 -0.00914 -0.00905 0.00528 AFIX 137 H30A 2 0.220702 0.280152 -0.000388 11.00000 -1.50000 H30B 2 0.338167 0.230149 0.031518 11.00000 -1.50000 H30C 2 0.350819 0.358759 -0.015366 11.00000 -1.50000 AFIX 0 C31 1 -0.066263 0.326365 0.256215 11.00000 0.02606 0.02904 = 0.01324 -0.00221 -0.00512 -0.00572 C32 1 -0.172720 0.233137 0.276008 11.00000 0.02773 0.03318 = 0.03228 0.00278 -0.00662 -0.01449 AFIX 137 H32A 2 -0.137673 0.152158 0.287066 11.00000 -1.50000 H32B 2 -0.212540 0.226493 0.234685 11.00000 -1.50000 H32C 2 -0.237629 0.259737 0.319230 11.00000 -1.50000 AFIX 0 C33 1 -0.230298 0.827742 0.385900 11.00000 0.02673 0.02675 = 0.03265 -0.00660 -0.01078 0.00772 C34 1 -0.258225 0.892238 0.459193 11.00000 0.04129 0.03819 = 0.03997 -0.01849 -0.00667 0.00488 AFIX 137 H34A 2 -0.313904 0.964509 0.457074 11.00000 -1.50000 H34B 2 -0.177081 0.919323 0.468605 11.00000 -1.50000 H34C 2 -0.301570 0.834174 0.498827 11.00000 -1.50000 AFIX 0 C1S 1 0.411088 0.676757 0.488708 11.00000 0.03492 0.03075 = 0.02212 0.00187 -0.01129 -0.00555 AFIX 23 H1S1 2 0.501003 0.648496 0.469470 11.00000 -1.20000 H1S2 2 0.372723 0.693804 0.446476 11.00000 -1.20000 AFIX 0 CL1 7 0.409782 0.813424 0.537115 11.00000 0.04869 0.03493 = 0.05094 -0.01085 -0.00960 -0.00040 CL2 7 0.322197 0.559004 0.547613 11.00000 0.04500 0.04853 = 0.04471 0.00655 -0.01293 -0.01815 O1W 4 -0.204376 0.674110 0.246767 11.00000 0.02314 0.02257 = 0.02439 0.00118 -0.01002 -0.00074 H1W 2 -0.191385 0.596902 0.253470 11.00000 0.04529 H2W 2 -0.236751 0.672110 0.292961 11.00000 0.05418 HKLF 4 REM C073 in P-1 REM R1 = 0.0510 for 7937 Fo > 4sig(Fo) and 0.0649 for all 9620 data REM 554 parameters refined using 2 restraints END WGHT 0.0465 1.6776 REM Highest difference peak 2.387, deepest hole -1.221, 1-sigma level 0.174 Q1 1 0.1958 0.5396 0.2284 11.00000 0.05 2.39 Q2 1 0.0814 0.5650 0.2403 11.00000 0.05 1.75 Q3 1 0.0573 0.4523 0.2514 11.00000 0.05 1.59 Q4 1 0.2059 0.5283 0.1751 11.00000 0.05 1.55 Q5 1 0.1807 0.4242 0.1980 11.00000 0.05 1.54 Q6 1 -0.0696 0.7667 0.2859 11.00000 0.05 1.52 Q7 1 0.0740 0.4521 0.1924 11.00000 0.05 1.33 Q8 1 -0.0852 0.8339 0.2588 11.00000 0.05 1.31 Q9 1 -0.0976 0.7472 0.2734 11.00000 0.05 1.31 Q10 1 -0.0823 0.7371 0.2349 11.00000 0.05 1.19 Q11 1 -0.0035 0.8003 0.2426 11.00000 0.05 1.05 Q12 1 -0.0020 0.7369 0.2472 11.00000 0.05 0.95 Q13 1 0.0402 0.5153 0.2161 11.00000 0.05 0.92 Q14 1 0.2511 0.7722 0.3275 11.00000 0.05 0.92 Q15 1 0.1528 0.7640 0.1769 11.00000 0.05 0.89 Q16 1 0.1697 0.8591 0.1580 11.00000 0.05 0.88 Q17 1 0.2605 0.7262 0.1286 11.00000 0.05 0.84 Q18 1 0.1440 0.7089 0.3404 11.00000 0.05 0.81 Q19 1 0.1615 0.4342 0.2503 11.00000 0.05 0.80 Q20 1 0.1624 0.7576 0.1230 11.00000 0.05 0.77 ; _database_code_depnum_ccdc_archive 'CCDC 955201' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c066 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H43 Cl2 N4 Ni3 O15 Y' _chemical_formula_weight 1095.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7085(7) _cell_length_b 10.7725(7) _cell_length_c 18.7974(13) _cell_angle_alpha 87.5570(10) _cell_angle_beta 75.6550(10) _cell_angle_gamma 89.1680(10) _cell_volume 2098.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8248 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 27.47 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 2.893 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3907 _exptl_absorpt_correction_T_max 0.4773 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26715 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_unetI/netI 0.0468 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9593 _reflns_number_gt 7653 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0568P)^2^+1.0220P] 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 9593 _refine_ls_number_parameters 554 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.13518(3) 0.49432(3) 0.215457(16) 0.01566(8) Uani 1 1 d . . . Ni1 Ni 0.21514(4) 0.78765(4) 0.14185(2) 0.01560(10) Uani 1 1 d . . . Ni2 Ni -0.04152(4) 0.77669(4) 0.24654(2) 0.01795(10) Uani 1 1 d . . . Ni3 Ni 0.20565(4) 0.72878(4) 0.30738(2) 0.01546(10) Uani 1 1 d . . . N1 N 0.3984(3) 0.8537(2) 0.12618(14) 0.0177(5) Uani 1 1 d . . . N2 N 0.2458(3) 0.6977(2) 0.04264(14) 0.0190(6) Uani 1 1 d . . . N3 N 0.3285(3) 0.8755(2) 0.30537(14) 0.0181(6) Uani 1 1 d . . . N4 N 0.0933(3) 0.7568(2) 0.41290(14) 0.0192(6) Uani 1 1 d . . . O1 O 0.2869(2) 0.65404(19) 0.20254(11) 0.0163(4) Uani 1 1 d . . . O2 O 0.0586(2) 0.67253(19) 0.16070(11) 0.0162(4) Uani 1 1 d . . . O3 O 0.1333(2) 0.85354(19) 0.24557(11) 0.0172(4) Uani 1 1 d . . . O4 O 0.0429(2) 0.63058(19) 0.30439(11) 0.0163(4) Uani 1 1 d . . . O5 O 0.1320(2) 0.9337(2) 0.09930(12) 0.0220(5) Uani 1 1 d . . . O6 O -0.0675(2) 0.9202(2) 0.17440(13) 0.0227(5) Uani 1 1 d . . . O7 O 0.3067(2) 0.5995(2) 0.35221(12) 0.0209(5) Uani 1 1 d . . . O8 O 0.2475(2) 0.4329(2) 0.30141(12) 0.0225(5) Uani 1 1 d . . . O9 O 0.3100(2) 0.3932(2) 0.13207(13) 0.0265(5) Uani 1 1 d . . . O10 O 0.1246(2) 0.4119(2) 0.10279(12) 0.0221(5) Uani 1 1 d . . . O11 O -0.0903(2) 0.4370(2) 0.23763(13) 0.0237(5) Uani 1 1 d . . . O12 O 0.0469(2) 0.2959(2) 0.25978(13) 0.0250(5) Uani 1 1 d . . . O13 O -0.1314(2) 0.8623(2) 0.33809(13) 0.0267(5) Uani 1 1 d . . . O14 O -0.3090(2) 0.7464(2) 0.37854(14) 0.0324(6) Uani 1 1 d . . . C1 C 0.4440(4) 0.9659(3) 0.09851(19) 0.0267(8) Uani 1 1 d . . . H1 H 0.3886 1.0222 0.0806 0.032 Uiso 1 1 calc R . . C2 C 0.5685(4) 1.0024(4) 0.0951(2) 0.0357(9) Uani 1 1 d . . . H2 H 0.5982 1.0822 0.0751 0.043 Uiso 1 1 calc R . . C3 C 0.6483(4) 0.9222(4) 0.1209(2) 0.0340(9) Uani 1 1 d . . . H3 H 0.7339 0.9462 0.1197 0.041 Uiso 1 1 calc R . . C4 C 0.6038(3) 0.8060(3) 0.14886(18) 0.0225(7) Uani 1 1 d . . . H4 H 0.6583 0.7487 0.1667 0.027 Uiso 1 1 calc R . . C5 C 0.4780(3) 0.7745(3) 0.15038(16) 0.0180(6) Uani 1 1 d . . . C6 C 0.4223(3) 0.6489(3) 0.17923(18) 0.0195(7) Uani 1 1 d . . . H6A H 0.4479 0.5881 0.1401 0.023 Uiso 1 1 calc R . . H6B H 0.4578 0.6201 0.2210 0.023 Uiso 1 1 calc R . . C7 C 0.3539(3) 0.6868(3) -0.01093(18) 0.0228(7) Uani 1 1 d . . . H7 H 0.4332 0.7105 -0.0015 0.027 Uiso 1 1 calc R . . C8 C 0.3558(3) 0.6429(3) -0.07911(18) 0.0238(7) Uani 1 1 d . . . H8 H 0.4346 0.6343 -0.1154 0.029 Uiso 1 1 calc R . . C9 C 0.2386(3) 0.6115(3) -0.09304(18) 0.0237(7) Uani 1 1 d . . . H9 H 0.2357 0.5835 -0.1398 0.028 Uiso 1 1 calc R . . C10 C 0.1266(3) 0.6215(3) -0.03824(18) 0.0214(7) Uani 1 1 d . . . H10 H 0.0458 0.6010 -0.0469 0.026 Uiso 1 1 calc R . . C11 C 0.1340(3) 0.6621(3) 0.02982(17) 0.0172(6) Uani 1 1 d . . . C12 C 0.0179(3) 0.6685(3) 0.09438(17) 0.0191(7) Uani 1 1 d . . . H12A H -0.0336 0.7436 0.0886 0.023 Uiso 1 1 calc R . . H12B H -0.0371 0.5948 0.0962 0.023 Uiso 1 1 calc R . . C13 C 0.4432(3) 0.8761(3) 0.32292(18) 0.0231(7) Uani 1 1 d . . . H13 H 0.4773 0.7998 0.3373 0.028 Uiso 1 1 calc R . . C14 C 0.5126(4) 0.9829(3) 0.3208(2) 0.0318(9) Uani 1 1 d . . . H14 H 0.5939 0.9803 0.3327 0.038 Uiso 1 1 calc R . . C15 C 0.4625(4) 1.0937(4) 0.3012(2) 0.0374(9) Uani 1 1 d . . . H15 H 0.5088 1.1687 0.2997 0.045 Uiso 1 1 calc R . . C16 C 0.3443(4) 1.0957(3) 0.2836(2) 0.0304(8) Uani 1 1 d . . . H16A H 0.3080 1.1717 0.2706 0.037 Uiso 1 1 calc R . . C17 C 0.2803(3) 0.9841(3) 0.28550(17) 0.0194(7) Uani 1 1 d . . . C18 C 0.1525(3) 0.9759(3) 0.26504(18) 0.0212(7) Uani 1 1 d . . . H18A H 0.0816 0.9993 0.3072 0.025 Uiso 1 1 calc R . . H18B H 0.1517 1.0347 0.2232 0.025 Uiso 1 1 calc R . . C19 C 0.1161(3) 0.8331(3) 0.46356(18) 0.0233(7) Uani 1 1 d . . . H19 H 0.1819 0.8938 0.4487 0.028 Uiso 1 1 calc R . . C20 C 0.0472(4) 0.8258(3) 0.53612(18) 0.0266(8) Uani 1 1 d . . . H20 H 0.0650 0.8813 0.5703 0.032 Uiso 1 1 calc R . . C21 C -0.0476(4) 0.7376(3) 0.55851(18) 0.0268(8) Uani 1 1 d . . . H21 H -0.0950 0.7300 0.6084 0.032 Uiso 1 1 calc R . . C22 C -0.0724(3) 0.6601(3) 0.50676(18) 0.0242(7) Uani 1 1 d . . . H22 H -0.1379 0.5989 0.5208 0.029 Uiso 1 1 calc R . . C23 C -0.0009(3) 0.6724(3) 0.43412(17) 0.0205(7) Uani 1 1 d . . . C24 C -0.0251(3) 0.5895(3) 0.37609(17) 0.0215(7) Uani 1 1 d . . . H24A H 0.0021 0.5036 0.3860 0.026 Uiso 1 1 calc R . . H24B H -0.1186 0.5884 0.3788 0.026 Uiso 1 1 calc R . . C25 C 0.0182(3) 0.9717(3) 0.12401(18) 0.0228(7) Uani 1 1 d . . . C26 C -0.0171(4) 1.0927(3) 0.0902(2) 0.0328(9) Uani 1 1 d . . . H26A H -0.1110 1.1032 0.1035 0.049 Uiso 1 1 calc R . . H26B H 0.0139 1.0916 0.0366 0.049 Uiso 1 1 calc R . . H26C H 0.0230 1.1618 0.1084 0.049 Uiso 1 1 calc R . . C27 C 0.3131(3) 0.4862(3) 0.33803(18) 0.0228(7) Uani 1 1 d . . . C28 C 0.4093(5) 0.4078(4) 0.3668(2) 0.0457(12) Uani 1 1 d . . . H28A H 0.3760 0.3232 0.3786 0.069 Uiso 1 1 calc R . . H28B H 0.4231 0.4438 0.4113 0.069 Uiso 1 1 calc R . . H28C H 0.4911 0.4055 0.3294 0.069 Uiso 1 1 calc R . . C29 C 0.2394(3) 0.3732(3) 0.08917(18) 0.0215(7) Uani 1 1 d . . . C30 C 0.2909(4) 0.3049(4) 0.0201(2) 0.0356(9) Uani 1 1 d . . . H30A H 0.2209 0.2904 -0.0036 0.053 Uiso 1 1 calc R . . H30B H 0.3272 0.2250 0.0321 0.053 Uiso 1 1 calc R . . H30C H 0.3583 0.3545 -0.0134 0.053 Uiso 1 1 calc R . . C31 C -0.0657(3) 0.3256(3) 0.25656(17) 0.0231(7) Uani 1 1 d . . . C32 C -0.1712(4) 0.2311(4) 0.2753(2) 0.0332(9) Uani 1 1 d . . . H32A H -0.1335 0.1475 0.2740 0.050 Uiso 1 1 calc R . . H32B H -0.2238 0.2391 0.2394 0.050 Uiso 1 1 calc R . . H32C H -0.2254 0.2448 0.3246 0.050 Uiso 1 1 calc R . . C33 C -0.2308(4) 0.8284(3) 0.3859(2) 0.0289(8) Uani 1 1 d . . . C34 C -0.2593(4) 0.8932(4) 0.4576(2) 0.0406(10) Uani 1 1 d . . . H34A H -0.2980 0.9747 0.4515 0.061 Uiso 1 1 calc R . . H34B H -0.1790 0.9041 0.4728 0.061 Uiso 1 1 calc R . . H34C H -0.3193 0.8430 0.4954 0.061 Uiso 1 1 calc R . . C1S C 0.4106(4) 0.6768(3) 0.4888(2) 0.0315(8) Uani 1 1 d . . . H1S1 H 0.5006 0.6487 0.4693 0.038 Uiso 1 1 calc R . . H1S2 H 0.3717 0.6938 0.4468 0.038 Uiso 1 1 calc R . . Cl1 Cl 0.40986(11) 0.81358(10) 0.53698(6) 0.0447(3) Uani 1 1 d . . . Cl2 Cl 0.32259(11) 0.55864(11) 0.54771(6) 0.0459(3) Uani 1 1 d . . . O1W O -0.2040(2) 0.6731(2) 0.24701(14) 0.0244(5) Uani 1 1 d D . . H1W H -0.181(5) 0.5983(18) 0.253(3) 0.062(16) Uiso 1 1 d D . . H2W H -0.239(5) 0.678(5) 0.2929(8) 0.067(17) Uiso 1 1 d 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 Y1 0.01966(16) 0.01518(16) 0.01360(15) 0.00119(11) -0.00706(12) -0.00220(12) Ni1 0.0197(2) 0.0160(2) 0.01323(19) 0.00303(15) -0.00850(16) -0.00376(16) Ni2 0.0202(2) 0.0160(2) 0.0202(2) 0.00147(16) -0.01010(17) -0.00178(16) Ni3 0.0208(2) 0.0148(2) 0.01221(19) 0.00123(15) -0.00697(16) -0.00150(16) N1 0.0239(14) 0.0174(13) 0.0134(12) 0.0009(10) -0.0076(11) -0.0047(11) N2 0.0238(14) 0.0191(14) 0.0161(13) 0.0037(11) -0.0095(11) -0.0036(11) N3 0.0247(14) 0.0187(14) 0.0121(12) -0.0014(10) -0.0066(11) -0.0020(11) N4 0.0243(14) 0.0175(14) 0.0163(13) -0.0004(11) -0.0058(11) 0.0008(11) O1 0.0163(11) 0.0187(11) 0.0150(10) 0.0022(8) -0.0062(9) -0.0023(9) O2 0.0198(11) 0.0171(11) 0.0144(10) 0.0011(8) -0.0094(9) -0.0032(9) O3 0.0222(11) 0.0145(11) 0.0166(11) 0.0012(8) -0.0082(9) -0.0024(9) O4 0.0208(11) 0.0162(11) 0.0115(10) 0.0023(8) -0.0039(9) -0.0021(9) O5 0.0283(13) 0.0200(12) 0.0209(12) 0.0050(9) -0.0131(10) -0.0035(10) O6 0.0239(12) 0.0214(12) 0.0256(12) 0.0042(10) -0.0122(10) -0.0007(10) O7 0.0312(13) 0.0187(12) 0.0166(11) 0.0003(9) -0.0133(10) 0.0018(10) O8 0.0345(13) 0.0184(12) 0.0191(11) 0.0015(9) -0.0152(10) -0.0035(10) O9 0.0203(12) 0.0350(14) 0.0266(13) -0.0079(11) -0.0091(10) -0.0012(10) O10 0.0223(12) 0.0275(13) 0.0184(11) -0.0040(9) -0.0084(10) 0.0001(10) O11 0.0253(13) 0.0214(12) 0.0240(12) -0.0015(10) -0.0047(10) -0.0052(10) O12 0.0293(13) 0.0230(12) 0.0246(12) 0.0050(10) -0.0110(10) -0.0050(10) O13 0.0229(13) 0.0278(13) 0.0287(13) -0.0001(10) -0.0053(11) 0.0001(10) O14 0.0259(13) 0.0352(15) 0.0340(14) -0.0039(12) -0.0029(11) -0.0031(11) C1 0.035(2) 0.0232(18) 0.0236(18) 0.0041(14) -0.0104(15) -0.0072(15) C2 0.039(2) 0.0248(19) 0.043(2) 0.0047(17) -0.0088(18) -0.0192(17) C3 0.028(2) 0.036(2) 0.039(2) -0.0031(17) -0.0114(17) -0.0138(17) C4 0.0205(17) 0.0290(18) 0.0191(16) -0.0034(14) -0.0064(13) -0.0041(14) C5 0.0236(16) 0.0221(16) 0.0096(14) -0.0015(12) -0.0064(12) -0.0035(13) C6 0.0165(15) 0.0219(17) 0.0207(16) 0.0026(13) -0.0066(13) -0.0020(13) C7 0.0244(17) 0.0249(18) 0.0209(17) 0.0027(13) -0.0092(14) -0.0026(14) C8 0.0296(18) 0.0232(17) 0.0174(16) 0.0022(13) -0.0041(14) -0.0028(14) C9 0.038(2) 0.0206(17) 0.0149(15) 0.0000(13) -0.0104(14) -0.0038(15) C10 0.0263(17) 0.0191(16) 0.0232(17) 0.0010(13) -0.0148(14) -0.0016(13) C11 0.0229(16) 0.0151(15) 0.0161(15) 0.0045(12) -0.0101(13) -0.0013(12) C12 0.0216(16) 0.0219(17) 0.0169(15) 0.0005(12) -0.0106(13) -0.0025(13) C13 0.0260(18) 0.0246(18) 0.0223(17) -0.0048(14) -0.0125(14) 0.0017(14) C14 0.031(2) 0.030(2) 0.042(2) -0.0100(17) -0.0219(18) -0.0015(16) C15 0.042(2) 0.026(2) 0.051(3) -0.0107(18) -0.023(2) -0.0051(17) C16 0.040(2) 0.0192(17) 0.036(2) -0.0046(15) -0.0162(18) -0.0008(15) C17 0.0258(17) 0.0189(16) 0.0156(15) -0.0057(12) -0.0083(13) 0.0001(13) C18 0.0268(18) 0.0158(16) 0.0230(17) -0.0003(13) -0.0100(14) -0.0002(13) C19 0.0306(19) 0.0209(17) 0.0190(16) 0.0002(13) -0.0070(14) -0.0022(14) C20 0.039(2) 0.0236(18) 0.0185(16) -0.0056(14) -0.0092(15) 0.0013(15) C21 0.034(2) 0.0305(19) 0.0133(16) 0.0010(14) -0.0022(14) 0.0022(16) C22 0.0317(19) 0.0196(17) 0.0194(17) 0.0016(13) -0.0033(14) -0.0027(14) C23 0.0253(17) 0.0184(16) 0.0183(16) 0.0009(13) -0.0067(13) 0.0006(13) C24 0.0285(18) 0.0206(17) 0.0142(15) 0.0013(13) -0.0029(13) -0.0042(14) C25 0.0321(19) 0.0189(17) 0.0234(17) 0.0019(13) -0.0186(15) -0.0056(14) C26 0.040(2) 0.0217(18) 0.040(2) 0.0101(16) -0.0186(18) 0.0003(16) C27 0.0284(18) 0.0242(18) 0.0189(16) -0.0014(13) -0.0118(14) 0.0029(14) C28 0.068(3) 0.031(2) 0.056(3) -0.017(2) -0.048(2) 0.019(2) C29 0.0241(18) 0.0208(17) 0.0202(16) 0.0007(13) -0.0069(14) -0.0047(14) C30 0.0261(19) 0.051(3) 0.032(2) -0.0192(18) -0.0082(16) 0.0021(17) C31 0.0287(19) 0.0271(18) 0.0125(15) -0.0006(13) -0.0028(13) -0.0082(15) C32 0.034(2) 0.035(2) 0.029(2) 0.0022(16) -0.0041(16) -0.0127(17) C33 0.030(2) 0.0272(19) 0.031(2) -0.0013(15) -0.0121(16) 0.0063(16) C34 0.040(2) 0.040(2) 0.038(2) -0.0107(19) -0.0016(19) -0.0018(19) C1S 0.039(2) 0.034(2) 0.0235(18) 0.0006(16) -0.0106(16) -0.0061(17) Cl1 0.0473(6) 0.0373(6) 0.0483(6) -0.0097(5) -0.0085(5) -0.0008(5) Cl2 0.0445(6) 0.0497(6) 0.0428(6) 0.0069(5) -0.0099(5) -0.0188(5) O1W 0.0245(13) 0.0250(14) 0.0253(13) 0.0015(11) -0.0094(11) -0.0017(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O4 2.297(2) . ? Y1 O8 2.312(2) . ? Y1 O1 2.347(2) . ? Y1 O10 2.360(2) . ? Y1 O2 2.371(2) . ? Y1 O12 2.381(2) . ? Y1 O9 2.404(2) . ? Y1 O11 2.430(2) . ? Y1 Ni3 3.3178(5) . ? Y1 Ni1 3.4279(5) . ? Y1 Ni2 3.5512(5) . ? Ni1 O5 2.028(2) . ? Ni1 N1 2.044(3) . ? Ni1 O2 2.050(2) . ? Ni1 O1 2.056(2) . ? Ni1 O3 2.080(2) . ? Ni1 N2 2.089(3) . ? Ni1 Ni2 2.9580(6) . ? Ni1 Ni3 3.1259(6) . ? Ni2 O13 2.007(2) . ? Ni2 O3 2.054(2) . ? Ni2 O2 2.068(2) . ? Ni2 O6 2.074(2) . ? Ni2 O1W 2.078(2) . ? Ni2 O4 2.186(2) . ? Ni2 Ni3 3.1607(6) . ? Ni3 O3 2.010(2) . ? Ni3 O7 2.032(2) . ? Ni3 N3 2.065(3) . ? Ni3 O4 2.066(2) . ? Ni3 N4 2.081(3) . ? Ni3 O1 2.134(2) . ? N1 C5 1.342(4) . ? N1 C1 1.345(4) . ? N2 C7 1.341(4) . ? N2 C11 1.342(4) . ? N3 C17 1.347(4) . ? N3 C13 1.349(4) . ? N4 C23 1.342(4) . ? N4 C19 1.353(4) . ? O1 C6 1.408(4) . ? O2 C12 1.422(4) . ? O3 C18 1.414(4) . ? O4 C24 1.419(4) . ? O5 C25 1.261(4) . ? O6 C25 1.259(4) . ? O7 C27 1.258(4) . ? O8 C27 1.258(4) . ? O9 C29 1.261(4) . ? O10 C29 1.260(4) . ? O11 C31 1.280(4) . ? O12 C31 1.258(4) . ? O13 C33 1.258(4) . ? O14 C33 1.261(4) . ? C1 C2 1.381(5) . ? C2 C3 1.364(6) . ? C3 C4 1.381(5) . ? C4 C5 1.387(4) . ? C5 C6 1.511(4) . ? C7 C8 1.380(5) . ? C8 C9 1.394(5) . ? C9 C10 1.380(5) . ? C10 C11 1.391(4) . ? C11 C12 1.510(4) . ? C13 C14 1.372(5) . ? C14 C15 1.375(5) . ? C15 C16 1.384(5) . ? C16 C17 1.387(5) . ? C17 C18 1.516(4) . ? C19 C20 1.380(5) . ? C20 C21 1.376(5) . ? C21 C22 1.385(5) . ? C22 C23 1.392(4) . ? C23 C24 1.511(4) . ? C25 C26 1.510(5) . ? C27 C28 1.509(5) . ? C29 C30 1.499(5) . ? C31 C32 1.498(5) . ? C33 C34 1.506(5) . ? C1S Cl1 1.761(4) . ? C1S Cl2 1.770(4) . ? 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 Y1 O8 82.08(8) . . ? O4 Y1 O1 75.35(7) . . ? O8 Y1 O1 77.87(7) . . ? O4 Y1 O10 145.11(8) . . ? O8 Y1 O10 132.18(8) . . ? O1 Y1 O10 113.56(8) . . ? O4 Y1 O2 70.17(7) . . ? O8 Y1 O2 142.57(7) . . ? O1 Y1 O2 71.28(7) . . ? O10 Y1 O2 80.74(8) . . ? O4 Y1 O12 105.86(8) . . ? O8 Y1 O12 76.38(8) . . ? O1 Y1 O12 153.75(8) . . ? O10 Y1 O12 80.89(8) . . ? O2 Y1 O12 134.44(8) . . ? O4 Y1 O9 155.66(8) . . ? O8 Y1 O9 83.23(8) . . ? O1 Y1 O9 82.66(8) . . ? O10 Y1 O9 54.79(8) . . ? O2 Y1 O9 112.57(8) . . ? O12 Y1 O9 89.31(8) . . ? O4 Y1 O11 79.53(7) . . ? O8 Y1 O11 118.78(8) . . ? O1 Y1 O11 147.50(8) . . ? O10 Y1 O11 77.24(8) . . ? O2 Y1 O11 81.05(7) . . ? O12 Y1 O11 54.32(8) . . ? O9 Y1 O11 124.69(8) . . ? O4 Y1 Ni3 37.96(5) . . ? O8 Y1 Ni3 66.93(6) . . ? O1 Y1 Ni3 39.82(5) . . ? O10 Y1 Ni3 149.41(6) . . ? O2 Y1 Ni3 75.80(5) . . ? O12 Y1 Ni3 129.69(6) . . ? O9 Y1 Ni3 117.89(6) . . ? O11 Y1 Ni3 117.42(6) . . ? O4 Y1 Ni1 73.14(5) . . ? O8 Y1 Ni1 112.75(6) . . ? O1 Y1 Ni1 35.90(5) . . ? O10 Y1 Ni1 94.48(6) . . ? O2 Y1 Ni1 35.87(5) . . ? O12 Y1 Ni1 170.27(6) . . ? O9 Y1 Ni1 95.02(6) . . ? O11 Y1 Ni1 116.41(6) . . ? Ni3 Y1 Ni1 55.182(11) . . ? O4 Y1 Ni2 36.52(5) . . ? O8 Y1 Ni2 116.52(6) . . ? O1 Y1 Ni2 73.25(5) . . ? O10 Y1 Ni2 111.15(6) . . ? O2 Y1 Ni2 34.02(5) . . ? O12 Y1 Ni2 123.62(6) . . ? O9 Y1 Ni2 143.74(6) . . ? O11 Y1 Ni2 74.29(6) . . ? Ni3 Y1 Ni2 54.664(11) . . ? Ni1 Y1 Ni2 50.115(11) . . ? O5 Ni1 N1 100.06(10) . . ? O5 Ni1 O2 96.14(9) . . ? N1 Ni1 O2 163.00(10) . . ? O5 Ni1 O1 169.83(9) . . ? N1 Ni1 O1 80.89(9) . . ? O2 Ni1 O1 84.08(8) . . ? O5 Ni1 O3 87.85(9) . . ? N1 Ni1 O3 99.69(9) . . ? O2 Ni1 O3 85.98(8) . . ? O1 Ni1 O3 82.02(8) . . ? O5 Ni1 N2 90.67(10) . . ? N1 Ni1 N2 96.65(10) . . ? O2 Ni1 N2 77.94(9) . . ? O1 Ni1 N2 99.29(9) . . ? O3 Ni1 N2 163.60(10) . . ? O5 Ni1 Ni2 81.63(7) . . ? N1 Ni1 Ni2 143.64(7) . . ? O2 Ni1 Ni2 44.31(6) . . ? O1 Ni1 Ni2 91.60(6) . . ? O3 Ni1 Ni2 43.95(6) . . ? N2 Ni1 Ni2 119.70(7) . . ? O5 Ni1 Ni3 127.13(7) . . ? N1 Ni1 Ni3 89.68(7) . . ? O2 Ni1 Ni3 84.61(6) . . ? O1 Ni1 Ni3 42.72(6) . . ? O3 Ni1 Ni3 39.33(6) . . ? N2 Ni1 Ni3 139.98(7) . . ? Ni2 Ni1 Ni3 62.528(13) . . ? O5 Ni1 Y1 138.78(7) . . ? N1 Ni1 Y1 121.09(7) . . ? O2 Ni1 Y1 42.67(6) . . ? O1 Ni1 Y1 42.03(6) . . ? O3 Ni1 Y1 87.58(6) . . ? N2 Ni1 Y1 82.79(7) . . ? Ni2 Ni1 Y1 67.106(12) . . ? Ni3 Ni1 Y1 60.619(11) . . ? O13 Ni2 O3 92.71(9) . . ? O13 Ni2 O2 172.92(9) . . ? O3 Ni2 O2 86.20(8) . . ? O13 Ni2 O6 95.52(10) . . ? O3 Ni2 O6 88.03(9) . . ? O2 Ni2 O6 91.44(9) . . ? O13 Ni2 O1W 92.35(10) . . ? O3 Ni2 O1W 171.30(9) . . ? O2 Ni2 O1W 87.92(9) . . ? O6 Ni2 O1W 98.52(9) . . ? O13 Ni2 O4 94.74(9) . . ? O3 Ni2 O4 78.73(8) . . ? O2 Ni2 O4 78.18(8) . . ? O6 Ni2 O4 163.60(9) . . ? O1W Ni2 O4 93.80(9) . . ? O13 Ni2 Ni1 136.65(7) . . ? O3 Ni2 Ni1 44.67(6) . . ? O2 Ni2 Ni1 43.83(6) . . ? O6 Ni2 Ni1 78.50(7) . . ? O1W Ni2 Ni1 130.97(7) . . ? O4 Ni2 Ni1 85.26(6) . . ? O13 Ni2 Ni3 91.36(7) . . ? O3 Ni2 Ni3 38.44(6) . . ? O2 Ni2 Ni3 83.43(6) . . ? O6 Ni2 Ni3 126.35(6) . . ? O1W Ni2 Ni3 134.34(7) . . ? O4 Ni2 Ni3 40.54(6) . . ? Ni1 Ni2 Ni3 61.338(13) . . ? O13 Ni2 Y1 133.04(7) . . ? O3 Ni2 Y1 84.67(6) . . ? O2 Ni2 Y1 39.90(6) . . ? O6 Ni2 Y1 131.09(7) . . ? O1W Ni2 Y1 86.71(7) . . ? O4 Ni2 Y1 38.71(5) . . ? Ni1 Ni2 Y1 62.779(12) . . ? Ni3 Ni2 Y1 58.907(11) . . ? O3 Ni3 O7 168.98(9) . . ? O3 Ni3 N3 80.21(9) . . ? O7 Ni3 N3 96.67(10) . . ? O3 Ni3 O4 82.62(8) . . ? O7 Ni3 O4 101.77(9) . . ? N3 Ni3 O4 160.81(10) . . ? O3 Ni3 N4 102.83(10) . . ? O7 Ni3 N4 87.95(10) . . ? N3 Ni3 N4 95.50(10) . . ? O4 Ni3 N4 79.99(9) . . ? O3 Ni3 O1 81.76(8) . . ? O7 Ni3 O1 88.51(8) . . ? N3 Ni3 O1 100.87(9) . . ? O4 Ni3 O1 85.02(8) . . ? N4 Ni3 O1 163.54(9) . . ? O3 Ni3 Ni1 40.99(6) . . ? O7 Ni3 Ni1 128.95(6) . . ? N3 Ni3 Ni1 89.62(7) . . ? O4 Ni3 Ni1 82.97(6) . . ? N4 Ni3 Ni1 141.93(7) . . ? O1 Ni3 Ni1 40.80(6) . . ? O3 Ni3 Ni2 39.44(6) . . ? O7 Ni3 Ni2 144.96(7) . . ? N3 Ni3 Ni2 118.37(7) . . ? O4 Ni3 Ni2 43.45(6) . . ? N4 Ni3 Ni2 88.94(7) . . ? O1 Ni3 Ni2 84.77(6) . . ? Ni1 Ni3 Ni2 56.133(12) . . ? O3 Ni3 Y1 91.84(6) . . ? O7 Ni3 Y1 84.80(6) . . ? N3 Ni3 Y1 145.64(7) . . ? O4 Ni3 Y1 43.15(6) . . ? N4 Ni3 Y1 118.86(8) . . ? O1 Ni3 Y1 44.77(6) . . ? Ni1 Ni3 Y1 64.198(12) . . ? Ni2 Ni3 Y1 66.429(12) . . ? C5 N1 C1 118.3(3) . . ? C5 N1 Ni1 113.7(2) . . ? C1 N1 Ni1 128.0(2) . . ? C7 N2 C11 118.4(3) . . ? C7 N2 Ni1 129.7(2) . . ? C11 N2 Ni1 111.3(2) . . ? C17 N3 C13 118.6(3) . . ? C17 N3 Ni3 112.2(2) . . ? C13 N3 Ni3 129.2(2) . . ? C23 N4 C19 118.5(3) . . ? C23 N4 Ni3 112.2(2) . . ? C19 N4 Ni3 128.4(2) . . ? C6 O1 Ni1 110.52(17) . . ? C6 O1 Ni3 117.11(18) . . ? Ni1 O1 Ni3 96.49(9) . . ? C6 O1 Y1 129.59(18) . . ? Ni1 O1 Y1 102.07(8) . . ? Ni3 O1 Y1 95.41(8) . . ? C12 O2 Ni1 107.93(17) . . ? C12 O2 Ni2 120.78(18) . . ? Ni1 O2 Ni2 91.86(8) . . ? C12 O2 Y1 122.48(18) . . ? Ni1 O2 Y1 101.46(8) . . ? Ni2 O2 Y1 106.09(8) . . ? C18 O3 Ni3 110.67(18) . . ? C18 O3 Ni2 125.52(19) . . ? Ni3 O3 Ni2 102.12(9) . . ? C18 O3 Ni1 122.84(19) . . ? Ni3 O3 Ni1 99.68(9) . . ? Ni2 O3 Ni1 91.38(8) . . ? C24 O4 Ni3 111.02(18) . . ? C24 O4 Ni2 119.14(19) . . ? Ni3 O4 Ni2 96.01(8) . . ? C24 O4 Y1 122.15(18) . . ? Ni3 O4 Y1 98.89(8) . . ? Ni2 O4 Y1 104.77(8) . . ? C25 O5 Ni1 125.4(2) . . ? C25 O6 Ni2 126.9(2) . . ? C27 O7 Ni3 124.4(2) . . ? C27 O8 Y1 135.9(2) . . ? C29 O9 Y1 91.1(2) . . ? C29 O10 Y1 93.21(19) . . ? C31 O11 Y1 91.43(19) . . ? C31 O12 Y1 94.3(2) . . ? C33 O13 Ni2 128.3(2) . . ? N1 C1 C2 122.3(3) . . ? C3 C2 C1 119.1(3) . . ? C2 C3 C4 119.5(3) . . ? C3 C4 C5 118.7(3) . . ? N1 C5 C4 122.1(3) . . ? N1 C5 C6 115.9(3) . . ? C4 C5 C6 122.1(3) . . ? O1 C6 C5 111.3(3) . . ? N2 C7 C8 123.3(3) . . ? C7 C8 C9 117.9(3) . . ? C10 C9 C8 119.4(3) . . ? C9 C10 C11 118.9(3) . . ? N2 C11 C10 122.0(3) . . ? N2 C11 C12 115.4(3) . . ? C10 C11 C12 122.6(3) . . ? O2 C12 C11 109.8(2) . . ? N3 C13 C14 122.4(3) . . ? C13 C14 C15 118.8(3) . . ? C14 C15 C16 119.9(3) . . ? C15 C16 C17 118.4(3) . . ? N3 C17 C16 121.9(3) . . ? N3 C17 C18 115.6(3) . . ? C16 C17 C18 122.4(3) . . ? O3 C18 C17 109.9(3) . . ? N4 C19 C20 122.3(3) . . ? C21 C20 C19 119.4(3) . . ? C20 C21 C22 118.6(3) . . ? C21 C22 C23 119.6(3) . . ? N4 C23 C22 121.5(3) . . ? N4 C23 C24 117.3(3) . . ? C22 C23 C24 121.2(3) . . ? O4 C24 C23 111.8(3) . . ? O6 C25 O5 126.7(3) . . ? O6 C25 C26 117.2(3) . . ? O5 C25 C26 116.1(3) . . ? O8 C27 O7 125.8(3) . . ? O8 C27 C28 117.3(3) . . ? O7 C27 C28 117.0(3) . . ? O10 C29 O9 120.8(3) . . ? O10 C29 C30 118.5(3) . . ? O9 C29 C30 120.7(3) . . ? O12 C31 O11 119.9(3) . . ? O12 C31 C32 120.2(3) . . ? O11 C31 C32 119.9(3) . . ? O13 C33 O14 125.7(3) . . ? O13 C33 C34 116.8(3) . . ? O14 C33 C34 117.5(3) . . ? Cl1 C1S Cl2 110.3(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H2W O14 0.853(10) 1.78(2) 2.600(4) 160(5) . O1W H1W O11 0.850(10) 1.977(19) 2.798(3) 162(5) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.322 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.117 _shelx_res_file ; TITL C066 in P-1 CELL 0.71073 10.7085 10.7725 18.7974 87.557 75.655 89.168 ZERR 2.00 0.0007 0.0007 0.0013 0.001 0.001 0.001 LATT 1 SFAC C H N O Ni Y Cl UNIT 70 86 8 30 6 2 4 OMIT -1.00 55.00 L.S. 10 ACTA BOND FMAP 2 PLAN 20 BIND Ni1 Ni2 BIND Ni1 Ni3 BIND Ni2 Ni3 BIND Ni1 Y1 BIND Ni2 Y1 BIND Ni3 Y1 FREE Y1 C29 FREE Y1 C31 HTAB HTAB O1W O14 HTAB O1W O11 DFIX 0.85 0.01 O1W H1W O1W H2W SIZE 0.40 0.36 0.30 TEMP -173 WGHT 0.056800 1.022000 FVAR 0.09385 Y1 6 0.135181 0.494323 0.215457 11.00000 0.01966 0.01518 = 0.01360 0.00119 -0.00706 -0.00220 NI1 5 0.215139 0.787647 0.141851 11.00000 0.01973 0.01595 = 0.01323 0.00303 -0.00850 -0.00376 NI2 5 -0.041520 0.776693 0.246536 11.00000 0.02021 0.01602 = 0.02019 0.00147 -0.01010 -0.00178 NI3 5 0.205645 0.728781 0.307383 11.00000 0.02077 0.01480 = 0.01221 0.00123 -0.00697 -0.00150 N1 3 0.398376 0.853712 0.126177 11.00000 0.02385 0.01740 = 0.01338 0.00093 -0.00761 -0.00466 N2 3 0.245796 0.697732 0.042642 11.00000 0.02382 0.01912 = 0.01611 0.00374 -0.00953 -0.00361 N3 3 0.328542 0.875550 0.305368 11.00000 0.02467 0.01867 = 0.01214 -0.00142 -0.00664 -0.00197 N4 3 0.093261 0.756828 0.412896 11.00000 0.02430 0.01746 = 0.01633 -0.00039 -0.00584 0.00084 O1 4 0.286885 0.654035 0.202539 11.00000 0.01630 0.01870 = 0.01503 0.00221 -0.00622 -0.00232 O2 4 0.058642 0.672528 0.160703 11.00000 0.01976 0.01707 = 0.01444 0.00108 -0.00940 -0.00321 O3 4 0.133309 0.853539 0.245572 11.00000 0.02216 0.01452 = 0.01661 0.00122 -0.00822 -0.00235 O4 4 0.042873 0.630580 0.304393 11.00000 0.02079 0.01619 = 0.01153 0.00234 -0.00386 -0.00215 O5 4 0.131985 0.933669 0.099297 11.00000 0.02830 0.01998 = 0.02090 0.00505 -0.01310 -0.00353 O6 4 -0.067488 0.920244 0.174401 11.00000 0.02394 0.02145 = 0.02556 0.00419 -0.01222 -0.00069 O7 4 0.306700 0.599539 0.352212 11.00000 0.03123 0.01872 = 0.01655 0.00034 -0.01330 0.00184 O8 4 0.247496 0.432855 0.301408 11.00000 0.03451 0.01841 = 0.01908 0.00155 -0.01523 -0.00349 O9 4 0.309996 0.393164 0.132068 11.00000 0.02032 0.03495 = 0.02664 -0.00790 -0.00911 -0.00123 O10 4 0.124576 0.411895 0.102786 11.00000 0.02226 0.02754 = 0.01844 -0.00398 -0.00842 0.00014 O11 4 -0.090263 0.436988 0.237632 11.00000 0.02526 0.02135 = 0.02401 -0.00145 -0.00474 -0.00522 O12 4 0.046947 0.295929 0.259783 11.00000 0.02930 0.02302 = 0.02463 0.00497 -0.01103 -0.00497 O13 4 -0.131444 0.862283 0.338087 11.00000 0.02290 0.02777 = 0.02867 -0.00014 -0.00530 0.00006 O14 4 -0.308994 0.746399 0.378538 11.00000 0.02595 0.03523 = 0.03404 -0.00393 -0.00295 -0.00308 C1 1 0.443988 0.965948 0.098507 11.00000 0.03466 0.02321 = 0.02361 0.00407 -0.01039 -0.00717 AFIX 43 H1 2 0.388581 1.022163 0.080641 11.00000 -1.20000 AFIX 0 C2 1 0.568517 1.002403 0.095137 11.00000 0.03864 0.02481 = 0.04310 0.00474 -0.00881 -0.01917 AFIX 43 H2 2 0.598155 1.082204 0.075117 11.00000 -1.20000 AFIX 0 C3 1 0.648345 0.922243 0.120949 11.00000 0.02820 0.03647 = 0.03950 -0.00308 -0.01140 -0.01381 AFIX 43 H3 2 0.733904 0.946175 0.119743 11.00000 -1.20000 AFIX 0 C4 1 0.603840 0.806006 0.148856 11.00000 0.02048 0.02896 = 0.01915 -0.00336 -0.00642 -0.00413 AFIX 43 H4 2 0.658347 0.748706 0.166663 11.00000 -1.20000 AFIX 0 C5 1 0.478028 0.774541 0.150383 11.00000 0.02362 0.02208 = 0.00956 -0.00154 -0.00635 -0.00345 C6 1 0.422314 0.648855 0.179233 11.00000 0.01654 0.02195 = 0.02068 0.00259 -0.00662 -0.00196 AFIX 23 H6A 2 0.447941 0.588121 0.140105 11.00000 -1.20000 H6B 2 0.457813 0.620070 0.220979 11.00000 -1.20000 AFIX 0 C7 1 0.353943 0.686812 -0.010932 11.00000 0.02438 0.02494 = 0.02087 0.00271 -0.00922 -0.00255 AFIX 43 H7 2 0.433249 0.710486 -0.001497 11.00000 -1.20000 AFIX 0 C8 1 0.355839 0.642903 -0.079106 11.00000 0.02957 0.02323 = 0.01738 0.00218 -0.00407 -0.00281 AFIX 43 H8 2 0.434569 0.634341 -0.115382 11.00000 -1.20000 AFIX 0 C9 1 0.238570 0.611523 -0.093037 11.00000 0.03787 0.02056 = 0.01486 -0.00001 -0.01039 -0.00379 AFIX 43 H9 2 0.235747 0.583487 -0.139848 11.00000 -1.20000 AFIX 0 C10 1 0.126634 0.621536 -0.038245 11.00000 0.02629 0.01913 = 0.02321 0.00101 -0.01479 -0.00159 AFIX 43 H10 2 0.045804 0.601025 -0.046873 11.00000 -1.20000 AFIX 0 C11 1 0.134050 0.662142 0.029819 11.00000 0.02288 0.01511 = 0.01605 0.00454 -0.01015 -0.00131 C12 1 0.017894 0.668495 0.094384 11.00000 0.02159 0.02188 = 0.01691 0.00046 -0.01062 -0.00246 AFIX 23 H12A 2 -0.033640 0.743610 0.088639 11.00000 -1.20000 H12B 2 -0.037088 0.594761 0.096191 11.00000 -1.20000 AFIX 0 C13 1 0.443241 0.876095 0.322923 11.00000 0.02601 0.02463 = 0.02228 -0.00481 -0.01246 0.00171 AFIX 43 H13 2 0.477252 0.799778 0.337283 11.00000 -1.20000 AFIX 0 C14 1 0.512601 0.982890 0.320795 11.00000 0.03067 0.02989 = 0.04242 -0.01004 -0.02186 -0.00145 AFIX 43 H14 2 0.593856 0.980320 0.332657 11.00000 -1.20000 AFIX 0 C15 1 0.462454 1.093684 0.301197 11.00000 0.04196 0.02645 = 0.05111 -0.01073 -0.02346 -0.00511 AFIX 43 H15 2 0.508781 1.168679 0.299730 11.00000 -1.20000 AFIX 0 C16 1 0.344332 1.095705 0.283612 11.00000 0.03965 0.01919 = 0.03637 -0.00465 -0.01621 -0.00085 AFIX 43 H16A 2 0.307961 1.171674 0.270569 11.00000 -1.20000 AFIX 0 C17 1 0.280324 0.984094 0.285496 11.00000 0.02581 0.01893 = 0.01559 -0.00569 -0.00835 0.00013 C18 1 0.152454 0.975930 0.265043 11.00000 0.02685 0.01580 = 0.02295 -0.00033 -0.00997 -0.00018 AFIX 23 H18A 2 0.081567 0.999253 0.307175 11.00000 -1.20000 H18B 2 0.151713 1.034680 0.223188 11.00000 -1.20000 AFIX 0 C19 1 0.116114 0.833131 0.463560 11.00000 0.03056 0.02088 = 0.01901 0.00023 -0.00703 -0.00218 AFIX 43 H19 2 0.181905 0.893844 0.448673 11.00000 -1.20000 AFIX 0 C20 1 0.047175 0.825838 0.536121 11.00000 0.03915 0.02363 = 0.01849 -0.00562 -0.00917 0.00126 AFIX 43 H20 2 0.065006 0.881262 0.570299 11.00000 -1.20000 AFIX 0 C21 1 -0.047586 0.737603 0.558513 11.00000 0.03431 0.03052 = 0.01331 0.00101 -0.00216 0.00219 AFIX 43 H21 2 -0.094964 0.729997 0.608404 11.00000 -1.20000 AFIX 0 C22 1 -0.072429 0.660106 0.506764 11.00000 0.03171 0.01963 = 0.01941 0.00159 -0.00331 -0.00267 AFIX 43 H22 2 -0.137903 0.598919 0.520763 11.00000 -1.20000 AFIX 0 C23 1 -0.000928 0.672364 0.434118 11.00000 0.02532 0.01837 = 0.01834 0.00091 -0.00673 0.00055 C24 1 -0.025066 0.589483 0.376087 11.00000 0.02845 0.02061 = 0.01425 0.00129 -0.00291 -0.00420 AFIX 23 H24A 2 0.002109 0.503570 0.385977 11.00000 -1.20000 H24B 2 -0.118552 0.588351 0.378779 11.00000 -1.20000 AFIX 0 C25 1 0.018173 0.971683 0.124007 11.00000 0.03209 0.01890 = 0.02339 0.00192 -0.01859 -0.00559 C26 1 -0.017088 1.092703 0.090156 11.00000 0.04020 0.02168 = 0.04003 0.01005 -0.01864 0.00034 AFIX 137 H26A 2 -0.110963 1.103193 0.103512 11.00000 -1.50000 H26B 2 0.013860 1.091620 0.036560 11.00000 -1.50000 H26C 2 0.022958 1.161822 0.108432 11.00000 -1.50000 AFIX 0 C27 1 0.313140 0.486172 0.338025 11.00000 0.02842 0.02421 = 0.01888 -0.00139 -0.01181 0.00295 C28 1 0.409257 0.407799 0.366849 11.00000 0.06751 0.03124 = 0.05618 -0.01691 -0.04757 0.01922 AFIX 137 H28A 2 0.375978 0.323160 0.378608 11.00000 -1.50000 H28B 2 0.423068 0.443803 0.411281 11.00000 -1.50000 H28C 2 0.491135 0.405543 0.329372 11.00000 -1.50000 AFIX 0 C29 1 0.239382 0.373219 0.089173 11.00000 0.02414 0.02079 = 0.02021 0.00068 -0.00692 -0.00472 C30 1 0.290899 0.304888 0.020110 11.00000 0.02610 0.05070 = 0.03210 -0.01922 -0.00819 0.00209 AFIX 137 H30A 2 0.220885 0.290449 -0.003624 11.00000 -1.50000 H30B 2 0.327197 0.224989 0.032149 11.00000 -1.50000 H30C 2 0.358303 0.354549 -0.013354 11.00000 -1.50000 AFIX 0 C31 1 -0.065671 0.325554 0.256562 11.00000 0.02871 0.02710 = 0.01249 -0.00056 -0.00276 -0.00824 C32 1 -0.171225 0.231081 0.275265 11.00000 0.03352 0.03495 = 0.02927 0.00216 -0.00406 -0.01274 AFIX 137 H32A 2 -0.133501 0.147530 0.274036 11.00000 -1.50000 H32B 2 -0.223831 0.239080 0.239423 11.00000 -1.50000 H32C 2 -0.225412 0.244813 0.324574 11.00000 -1.50000 AFIX 0 C33 1 -0.230758 0.828358 0.385922 11.00000 0.03039 0.02717 = 0.03136 -0.00135 -0.01213 0.00635 C34 1 -0.259259 0.893185 0.457637 11.00000 0.04029 0.04050 = 0.03767 -0.01071 -0.00155 -0.00182 AFIX 137 H34A 2 -0.297994 0.974654 0.451456 11.00000 -1.50000 H34B 2 -0.178988 0.904091 0.472762 11.00000 -1.50000 H34C 2 -0.319340 0.842991 0.495357 11.00000 -1.50000 AFIX 0 C1S 1 0.410627 0.676793 0.488837 11.00000 0.03879 0.03393 = 0.02347 0.00059 -0.01062 -0.00607 AFIX 23 H1S1 2 0.500564 0.648680 0.469258 11.00000 -1.20000 H1S2 2 0.371701 0.693806 0.446809 11.00000 -1.20000 AFIX 0 CL1 7 0.409857 0.813577 0.536975 11.00000 0.04730 0.03735 = 0.04831 -0.00965 -0.00847 -0.00075 CL2 7 0.322591 0.558637 0.547713 11.00000 0.04451 0.04965 = 0.04275 0.00693 -0.00993 -0.01879 O1W 4 -0.204006 0.673148 0.247012 11.00000 0.02451 0.02495 = 0.02534 0.00154 -0.00937 -0.00169 H1W 2 -0.181369 0.598291 0.253239 11.00000 0.06191 H2W 2 -0.238602 0.678412 0.292855 11.00000 0.06706 HKLF 4 REM C066 in P-1 REM R1 = 0.0402 for 7653 Fo > 4sig(Fo) and 0.0569 for all 9593 data REM 554 parameters refined using 2 restraints END WGHT 0.0570 1.0003 REM Highest difference peak 1.322, deepest hole -0.783, 1-sigma level 0.117 Q1 1 0.1962 0.5398 0.2250 11.00000 0.05 1.32 Q2 1 -0.1151 0.7625 0.2664 11.00000 0.05 0.99 Q3 1 0.1409 0.7857 0.1567 11.00000 0.05 0.92 Q4 1 0.2033 0.8644 0.1436 11.00000 0.05 0.86 Q5 1 0.1296 0.7243 0.3240 11.00000 0.05 0.86 Q6 1 0.1097 0.5727 0.2271 11.00000 0.05 0.78 Q7 1 0.0548 0.4808 0.2343 11.00000 0.05 0.73 Q8 1 -0.0943 0.8324 0.2609 11.00000 0.05 0.70 Q9 1 0.2040 0.8008 0.3024 11.00000 0.05 0.67 Q10 1 -0.0477 0.8414 0.2498 11.00000 0.05 0.66 Q11 1 0.1989 0.7202 0.1518 11.00000 0.05 0.65 Q12 1 0.1536 0.4138 0.2129 11.00000 0.05 0.64 Q13 1 0.3754 0.8865 0.3166 11.00000 0.05 0.54 Q14 1 0.2255 0.6595 0.3019 11.00000 0.05 0.54 Q15 1 0.3138 0.8669 0.1403 11.00000 0.05 0.53 Q16 1 -0.0159 0.7049 0.2434 11.00000 0.05 0.52 Q17 1 0.0216 0.3910 0.2579 11.00000 0.05 0.51 Q18 1 0.3211 0.8191 0.1242 11.00000 0.05 0.50 Q19 1 0.3344 0.6535 0.1974 11.00000 0.05 0.49 Q20 1 -0.3381 0.8896 0.4670 11.00000 0.05 0.48 ; _database_code_depnum_ccdc_archive 'CCDC 955202'