# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Tong-Bu Lu' _publ_contact_author_email LUTONGBU@MAIL.SYSU.EDU.CN _publ_section_title ; Constructions of 1D helical chains with left-handed/right-handed helicity: a correlation between the helicity of 1D chains and the chirality of building blocks ; loop_ _publ_author_name 'Tong-Bu Lu' 'Xiao-Long Feng' 'Long Jiang' 'Xiao-Dan Zheng' # Attachment '\D-2.cif' data_\D-2 _database_code_depnum_ccdc_archive 'CCDC 722169' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H79 Cl N18 Ni2 O5' _chemical_formula_weight 1057.09 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.1505(2) _cell_length_b 28.7597(7) _cell_length_c 10.2680(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.507(2) _cell_angle_gamma 90.00 _cell_volume 2616.03(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1822 _cell_measurement_theta_min 3.1827 _cell_measurement_theta_max 54.1392 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.830 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7379 _exptl_absorpt_correction_T_max 0.7830 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Gemini S Ultra' _diffrn_measurement_method '\w and \p scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13238 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0690 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7867 _reflns_number_gt 6694 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _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^)+(0.0458P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(13) _refine_ls_number_reflns 7867 _refine_ls_number_parameters 3 _refine_ls_number_restraints 209 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 1.036 _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 C1 C -0.2572(5) 0.52812(17) 0.0292(5) 0.0242(11) Uani 1 1 d . . . H1A H -0.2364 0.5045 -0.0312 0.029 Uiso 1 1 calc R . . H1B H -0.3658 0.5311 0.0130 0.029 Uiso 1 1 calc R . . C2 C -0.1916(5) 0.51320(18) 0.1726(5) 0.0260(11) Uani 1 1 d . . . H2A H -0.2174 0.5358 0.2335 0.031 Uiso 1 1 calc R . . H2B H -0.2336 0.4834 0.1885 0.031 Uiso 1 1 calc R . . C3 C 0.0474(5) 0.49901(18) 0.3422(4) 0.0263(11) Uani 1 1 d . . . H3 H 0.0275 0.5249 0.3973 0.032 Uiso 1 1 calc R . . C4 C -0.0166(6) 0.4550(2) 0.3868(5) 0.0425(15) Uani 1 1 d . . . H4A H -0.1248 0.4570 0.3646 0.064 Uiso 1 1 calc R . . H4B H 0.0210 0.4514 0.4823 0.064 Uiso 1 1 calc R . . H4C H 0.0133 0.4288 0.3419 0.064 Uiso 1 1 calc R . . C5 C 0.2194(5) 0.49361(18) 0.3652(5) 0.0301(12) Uani 1 1 d . . . H5A H 0.2574 0.4792 0.4526 0.036 Uiso 1 1 calc R . . H5B H 0.2371 0.4719 0.2986 0.036 Uiso 1 1 calc R . . C6 C 0.3146(5) 0.53641(17) 0.3604(4) 0.0237(10) Uani 1 1 d . . . C7 C 0.2907(5) 0.5737(2) 0.4601(4) 0.0314(11) Uani 1 1 d . . . H7A H 0.3545 0.5999 0.4567 0.047 Uiso 1 1 calc R . . H7B H 0.3155 0.5610 0.5495 0.047 Uiso 1 1 calc R . . H7C H 0.1870 0.5834 0.4367 0.047 Uiso 1 1 calc R . . C8 C 0.4838(5) 0.5225(2) 0.4031(5) 0.0398(14) Uani 1 1 d . . . H8A H 0.5011 0.4967 0.3496 0.060 Uiso 1 1 calc R . . H8B H 0.5102 0.5138 0.4964 0.060 Uiso 1 1 calc R . . H8C H 0.5448 0.5483 0.3899 0.060 Uiso 1 1 calc R . . C9 C 0.3358(5) 0.5310(2) 0.1259(5) 0.0342(13) Uani 1 1 d . . . H9A H 0.3135 0.4982 0.1315 0.041 Uiso 1 1 calc R . . H9B H 0.4447 0.5346 0.1486 0.041 Uiso 1 1 calc R . . C10 C 0.2703(5) 0.5480(2) -0.0161(5) 0.0337(13) Uani 1 1 d . . . H10A H 0.2972 0.5803 -0.0237 0.040 Uiso 1 1 calc R . . H10B H 0.3110 0.5299 -0.0786 0.040 Uiso 1 1 calc R . . C11 C 0.0310(5) 0.5620(2) -0.1847(5) 0.0366(10) Uani 1 1 d U . . H11 H 0.0523 0.5954 -0.1841 0.044 Uiso 1 1 calc R . . C12 C 0.0896(7) 0.5398(3) -0.2949(6) 0.0547(13) Uani 1 1 d U . . H12A H 0.1963 0.5451 -0.2780 0.082 Uiso 1 1 calc R . . H12B H 0.0394 0.5532 -0.3800 0.082 Uiso 1 1 calc R . . H12C H 0.0703 0.5070 -0.2968 0.082 Uiso 1 1 calc R . . C13 C -0.1404(5) 0.55560(19) -0.2197(5) 0.0354(10) Uani 1 1 d U . . H13A H -0.1785 0.5615 -0.3152 0.042 Uiso 1 1 calc R . . H13B H -0.1606 0.5232 -0.2048 0.042 Uiso 1 1 calc R . . C14 C -0.2316(5) 0.58481(17) -0.1461(4) 0.0290(12) Uani 1 1 d . . . C15 C -0.2033(7) 0.6363(2) -0.1581(6) 0.0493(16) Uani 1 1 d . . . H15A H -0.2649 0.6536 -0.1121 0.074 Uiso 1 1 calc R . . H15B H -0.2283 0.6450 -0.2513 0.074 Uiso 1 1 calc R . . H15C H -0.0988 0.6430 -0.1185 0.074 Uiso 1 1 calc R . . C16 C -0.4015(5) 0.5765(2) -0.2106(5) 0.0439(15) Uani 1 1 d . . . H16A H -0.4210 0.5437 -0.2186 0.066 Uiso 1 1 calc R . . H16B H -0.4287 0.5906 -0.2982 0.066 Uiso 1 1 calc R . . H16C H -0.4601 0.5902 -0.1550 0.066 Uiso 1 1 calc R . . C17 C 0.7119(5) 0.8228(2) 0.5913(5) 0.0334(13) Uani 1 1 d . . . H17A H 0.6752 0.8519 0.6188 0.040 Uiso 1 1 calc R . . H17B H 0.8139 0.8277 0.5828 0.040 Uiso 1 1 calc R . . C18 C 0.7122(5) 0.7862(2) 0.6956(5) 0.0302(13) Uani 1 1 d . . . H18A H 0.7499 0.7572 0.6684 0.036 Uiso 1 1 calc R . . H18B H 0.7789 0.7956 0.7807 0.036 Uiso 1 1 calc R . . C19 C 0.5459(5) 0.73964(18) 0.8026(4) 0.0274(11) Uani 1 1 d . . . H19 H 0.5663 0.7108 0.7595 0.033 Uiso 1 1 calc R . . C20 C 0.6589(6) 0.74336(19) 0.9414(5) 0.0409(14) Uani 1 1 d . . . H20A H 0.7601 0.7416 0.9307 0.061 Uiso 1 1 calc R . . H20B H 0.6423 0.7183 0.9976 0.061 Uiso 1 1 calc R . . H20C H 0.6449 0.7725 0.9823 0.061 Uiso 1 1 calc R . . C21 C 0.3870(6) 0.73640(18) 0.8267(4) 0.0303(12) Uani 1 1 d . . . H21A H 0.3919 0.7150 0.9006 0.036 Uiso 1 1 calc R . . H21B H 0.3617 0.7667 0.8562 0.036 Uiso 1 1 calc R . . C22 C 0.2563(5) 0.72098(18) 0.7094(5) 0.0260(11) Uani 1 1 d . . . C23 C 0.2845(6) 0.67379(19) 0.6551(5) 0.0352(13) Uani 1 1 d . . . H23A H 0.1945 0.6634 0.5919 0.053 Uiso 1 1 calc R . . H23B H 0.3115 0.6520 0.7280 0.053 Uiso 1 1 calc R . . H23C H 0.3652 0.6761 0.6111 0.053 Uiso 1 1 calc R . . C24 C 0.1130(6) 0.7174(2) 0.7615(6) 0.0430(14) Uani 1 1 d . . . H24A H 0.0278 0.7108 0.6879 0.064 Uiso 1 1 calc R . . H24B H 0.0967 0.7463 0.8024 0.064 Uiso 1 1 calc R . . H24C H 0.1251 0.6929 0.8269 0.064 Uiso 1 1 calc R . . C25 C 0.1688(5) 0.80046(18) 0.6224(5) 0.0292(12) Uani 1 1 d . . . H25A H 0.2279 0.8134 0.7064 0.035 Uiso 1 1 calc R . . H25B H 0.0669 0.7953 0.6310 0.035 Uiso 1 1 calc R . . C26 C 0.1658(5) 0.83375(18) 0.5110(5) 0.0266(11) Uani 1 1 d . . . H26A H 0.1069 0.8208 0.4270 0.032 Uiso 1 1 calc R . . H26B H 0.1183 0.8625 0.5278 0.032 Uiso 1 1 calc R . . C27 C 0.3250(5) 0.87103(17) 0.3788(4) 0.0246(11) Uani 1 1 d . . . H27 H 0.2833 0.8517 0.2996 0.030 Uiso 1 1 calc R . . C28 C 0.2305(6) 0.91527(19) 0.3653(5) 0.0369(13) Uani 1 1 d . . . H28A H 0.1268 0.9073 0.3575 0.055 Uiso 1 1 calc R . . H28B H 0.2386 0.9320 0.2866 0.055 Uiso 1 1 calc R . . H28C H 0.2666 0.9344 0.4435 0.055 Uiso 1 1 calc R . . C29 C 0.4879(5) 0.88343(18) 0.3779(5) 0.0297(12) Uani 1 1 d . . . H29A H 0.5341 0.8979 0.4636 0.036 Uiso 1 1 calc R . . H29B H 0.4829 0.9069 0.3092 0.036 Uiso 1 1 calc R . . C30 C 0.5962(5) 0.84524(18) 0.3544(5) 0.0265(11) Uani 1 1 d . . . C31 C 0.5368(6) 0.8209(2) 0.2197(5) 0.0356(13) Uani 1 1 d . . . H31A H 0.6112 0.7994 0.2051 0.053 Uiso 1 1 calc R . . H31B H 0.5161 0.8436 0.1489 0.053 Uiso 1 1 calc R . . H31C H 0.4457 0.8045 0.2203 0.053 Uiso 1 1 calc R . . C32 C 0.7453(6) 0.8681(2) 0.3546(6) 0.0441(15) Uani 1 1 d . . . H32A H 0.7773 0.8871 0.4335 0.066 Uiso 1 1 calc R . . H32B H 0.7333 0.8871 0.2758 0.066 Uiso 1 1 calc R . . H32C H 0.8197 0.8445 0.3548 0.066 Uiso 1 1 calc R . . C33 C 0.1406(6) 0.67561(19) 0.0992(5) 0.0313(10) Uani 1 1 d U . . C34 C 0.2216(6) 0.73957(18) 0.2286(5) 0.0305(10) Uani 1 1 d U . . C35 C -0.0671(6) 0.6374(2) 0.3282(5) 0.0410(12) Uani 1 1 d U . . C36 C -0.1126(7) 0.7103(3) 0.3958(6) 0.0527(15) Uani 1 1 d U . . C37 C 0.5246(6) 0.6833(2) 0.4049(6) 0.0406(11) Uani 1 1 d U . . C38 C 0.5536(6) 0.6443(2) 0.2125(7) 0.0469(13) Uani 1 1 d U . . Cl1 Cl 0.50710(14) 0.90021(4) 0.85848(12) 0.0320(3) Uani 1 1 d . . . N1 N -0.1925(4) 0.57305(15) 0.0008(3) 0.0213(8) Uani 1 1 d . . . H1C H -0.2389 0.5951 0.0399 0.026 Uiso 1 1 calc R . . N2 N -0.0251(4) 0.50946(13) 0.1984(3) 0.0195(9) Uani 1 1 d . . . H2C H -0.0044 0.4854 0.1481 0.023 Uiso 1 1 calc R . . N3 N 0.2729(4) 0.55722(13) 0.2228(3) 0.0204(9) Uani 1 1 d . . . H3A H 0.3203 0.5853 0.2314 0.025 Uiso 1 1 calc R . . N4 N 0.1041(4) 0.54305(15) -0.0491(4) 0.0228(9) Uani 1 1 d . . . H4D H 0.0832 0.5121 -0.0508 0.027 Uiso 1 1 calc R . . N5 N 0.2358(4) 0.75573(14) 0.5950(4) 0.0232(9) Uani 1 1 d . . . H5C H 0.1664 0.7427 0.5252 0.028 Uiso 1 1 calc R . . N6 N 0.3209(4) 0.84335(13) 0.5001(4) 0.0205(8) Uani 1 1 d . . . H6A H 0.3692 0.8599 0.5740 0.025 Uiso 1 1 calc R . . N7 N 0.6145(4) 0.80812(14) 0.4609(4) 0.0230(9) Uani 1 1 d . . . H7D H 0.6650 0.7845 0.4323 0.028 Uiso 1 1 calc R . . N8 N 0.5571(4) 0.77897(15) 0.7130(3) 0.0245(9) Uani 1 1 d . . . H8D H 0.5306 0.8052 0.7511 0.029 Uiso 1 1 calc R . . N9 N 0.1188(4) 0.63737(15) 0.0720(4) 0.0269(9) Uani 1 1 d U . . N10 N 0.1569(6) 0.72037(17) 0.1137(4) 0.0478(11) Uani 1 1 d U . . N11 N 0.2782(4) 0.76090(13) 0.3230(4) 0.0245(9) Uani 1 1 d U . . N12 N -0.0328(4) 0.60855(15) 0.2671(4) 0.0289(9) Uani 1 1 d U . . N13 N -0.1176(6) 0.6643(2) 0.4131(5) 0.0602(12) Uani 1 1 d U . . N14 N -0.1236(6) 0.7494(2) 0.3926(6) 0.0650(15) Uani 1 1 d U . . N15 N 0.5261(4) 0.71131(15) 0.4856(4) 0.0293(9) Uani 1 1 d U . . N16 N 0.4877(6) 0.6506(2) 0.3118(5) 0.0574(12) Uani 1 1 d U . . N17 N 0.5837(5) 0.6358(2) 0.1155(5) 0.0545(15) Uani 1 1 d . . . Ni1 Ni 0.03974(6) 0.571812(19) 0.11857(5) 0.01527(13) Uani 1 1 d . . . Ni2 Ni 0.42274(6) 0.77582(2) 0.51242(5) 0.01820(14) Uani 1 1 d . . . O1 O 0.5076(5) 0.93151(15) 0.9662(4) 0.0614(12) Uani 1 1 d . . . O2 O 0.4135(7) 0.9165(2) 0.7397(5) 0.104(2) Uani 1 1 d . . . O3 O 0.4570(7) 0.85568(17) 0.8858(5) 0.0915(18) Uani 1 1 d . . . O4 O 0.6526(5) 0.8956(3) 0.8400(7) 0.126(3) Uani 1 1 d . . . O5 O 0.0046(5) 0.44647(15) -0.0230(4) 0.0499(11) Uani 1 1 d . . . C41 C 0.0478(6) 0.4088(2) -0.0517(5) 0.0379(13) Uani 1 1 d . . . H41 H 0.1334 0.4085 -0.0851 0.046 Uiso 1 1 calc R . . C40 C -0.1469(7) 0.3660(3) 0.0132(7) 0.0595(18) Uani 1 1 d . . . H40A H -0.1732 0.3967 0.0360 0.089 Uiso 1 1 calc R . . H40B H -0.1255 0.3468 0.0921 0.089 Uiso 1 1 calc R . . H40C H -0.2295 0.3529 -0.0534 0.089 Uiso 1 1 calc R . . C39 C 0.0428(7) 0.3258(2) -0.0805(6) 0.0544(17) Uani 1 1 d . . . H39A H 0.1296 0.3326 -0.1139 0.082 Uiso 1 1 calc R . . H39B H -0.0333 0.3113 -0.1502 0.082 Uiso 1 1 calc R . . H39C H 0.0712 0.3052 -0.0049 0.082 Uiso 1 1 calc R . . N18 N -0.0156(5) 0.36830(16) -0.0397(4) 0.0358(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.018(2) 0.026(3) 0.028(2) -0.004(2) 0.006(2) -0.003(2) C2 0.020(2) 0.031(3) 0.029(3) 0.003(2) 0.012(2) -0.005(2) C3 0.032(3) 0.029(3) 0.020(2) 0.003(2) 0.010(2) -0.004(2) C4 0.044(3) 0.054(4) 0.028(3) 0.021(3) 0.005(2) -0.008(3) C5 0.037(3) 0.029(3) 0.020(2) 0.004(2) -0.001(2) -0.002(2) C6 0.023(2) 0.024(3) 0.024(2) 0.002(2) 0.0053(19) 0.000(2) C7 0.033(2) 0.033(3) 0.024(2) -0.005(3) -0.0005(19) -0.001(3) C8 0.030(3) 0.041(4) 0.041(3) -0.001(3) -0.005(2) 0.001(2) C9 0.019(2) 0.047(4) 0.037(3) -0.003(3) 0.008(2) 0.006(2) C10 0.028(3) 0.046(4) 0.035(3) -0.006(3) 0.022(2) 0.000(2) C11 0.0381(14) 0.0416(17) 0.0302(14) 0.0000(13) 0.0088(12) -0.0043(13) C12 0.0543(18) 0.067(2) 0.0471(19) -0.0058(16) 0.0202(15) -0.0004(17) C13 0.0380(14) 0.0382(17) 0.0286(15) 0.0001(14) 0.0059(12) -0.0039(14) C14 0.032(3) 0.027(3) 0.022(2) 0.002(2) -0.005(2) 0.000(2) C15 0.068(4) 0.038(4) 0.031(3) 0.009(3) -0.006(3) -0.002(3) C16 0.033(3) 0.058(4) 0.031(3) 0.002(3) -0.008(2) -0.004(3) C17 0.016(2) 0.039(4) 0.044(3) -0.011(3) 0.007(2) -0.002(2) C18 0.018(2) 0.047(4) 0.024(2) -0.005(2) 0.0016(19) -0.003(2) C19 0.038(3) 0.024(3) 0.015(2) -0.001(2) -0.002(2) 0.007(2) C20 0.056(3) 0.028(3) 0.028(3) -0.001(2) -0.009(3) 0.003(3) C21 0.049(3) 0.025(3) 0.016(2) 0.000(2) 0.007(2) -0.005(2) C22 0.031(3) 0.028(3) 0.022(2) 0.001(2) 0.011(2) -0.008(2) C23 0.047(3) 0.029(3) 0.031(3) -0.003(2) 0.010(2) -0.007(2) C24 0.049(3) 0.045(4) 0.039(3) 0.004(3) 0.018(3) -0.005(3) C25 0.023(2) 0.039(3) 0.031(3) 0.004(2) 0.016(2) 0.005(2) C26 0.024(2) 0.031(3) 0.025(2) 0.001(2) 0.007(2) 0.010(2) C27 0.029(2) 0.022(3) 0.022(2) -0.002(2) 0.0033(19) 0.005(2) C28 0.050(3) 0.027(3) 0.036(3) 0.009(2) 0.016(3) 0.015(3) C29 0.032(3) 0.025(3) 0.032(3) 0.006(2) 0.008(2) -0.005(2) C30 0.026(2) 0.027(3) 0.030(3) -0.002(2) 0.015(2) 0.000(2) C31 0.034(3) 0.047(4) 0.031(3) 0.006(3) 0.017(2) 0.001(3) C32 0.034(3) 0.056(4) 0.047(3) 0.007(3) 0.019(3) -0.009(3) C33 0.047(2) 0.025(2) 0.0174(18) 0.0013(17) -0.0004(18) -0.004(2) C34 0.044(2) 0.022(2) 0.0222(18) 0.0026(16) 0.0018(18) -0.0037(19) C35 0.047(2) 0.042(2) 0.032(2) -0.0092(19) 0.0044(19) 0.014(2) C36 0.047(3) 0.049(2) 0.059(3) -0.027(3) 0.009(2) 0.005(3) C37 0.051(2) 0.037(2) 0.041(2) -0.0044(18) 0.025(2) -0.005(2) C38 0.049(3) 0.045(3) 0.057(3) -0.015(2) 0.032(2) -0.017(2) Cl1 0.0426(7) 0.0249(7) 0.0286(6) -0.0029(5) 0.0090(5) -0.0007(6) N1 0.0230(17) 0.021(2) 0.0204(17) -0.0057(19) 0.0058(14) 0.0025(19) N2 0.0220(19) 0.021(2) 0.0172(18) -0.0034(16) 0.0077(16) -0.0008(16) N3 0.0182(17) 0.018(2) 0.0243(19) -0.0042(15) 0.0037(15) -0.0038(15) N4 0.023(2) 0.027(2) 0.0220(19) -0.0014(17) 0.0125(16) -0.0035(17) N5 0.024(2) 0.026(2) 0.0196(19) -0.0011(17) 0.0059(16) -0.0032(17) N6 0.0215(19) 0.021(2) 0.0188(18) -0.0032(16) 0.0038(15) 0.0027(16) N7 0.0202(19) 0.028(3) 0.022(2) -0.0049(18) 0.0086(17) -0.0025(17) N8 0.0216(18) 0.025(2) 0.0245(18) -0.0004(19) 0.0017(15) 0.0056(19) N9 0.0327(19) 0.0213(19) 0.0231(17) 0.0002(16) 0.0001(15) -0.0048(17) N10 0.075(2) 0.0278(19) 0.0282(18) -0.0009(17) -0.0104(19) -0.006(2) N11 0.0320(18) 0.020(2) 0.0210(17) -0.0043(14) 0.0051(15) -0.0029(16) N12 0.032(2) 0.031(2) 0.0232(18) -0.0052(16) 0.0048(16) 0.0043(17) N13 0.073(2) 0.058(2) 0.050(2) -0.015(2) 0.016(2) 0.014(2) N14 0.058(3) 0.053(3) 0.089(3) -0.023(3) 0.028(3) -0.005(3) N15 0.033(2) 0.028(2) 0.0268(19) -0.0023(16) 0.0090(17) -0.0021(17) N16 0.066(2) 0.055(2) 0.060(2) -0.0174(19) 0.0319(19) -0.014(2) N17 0.043(3) 0.068(4) 0.053(3) -0.026(3) 0.013(2) 0.011(3) Ni1 0.0176(3) 0.0145(3) 0.0144(2) -0.0026(3) 0.0054(2) -0.0006(3) Ni2 0.0190(3) 0.0182(3) 0.0173(3) -0.0040(3) 0.0043(2) 0.0021(3) O1 0.104(3) 0.038(3) 0.047(2) -0.023(2) 0.030(2) -0.011(2) O2 0.169(6) 0.068(4) 0.048(3) -0.007(3) -0.022(3) 0.030(4) O3 0.179(6) 0.036(3) 0.078(3) -0.015(3) 0.067(4) -0.032(3) O4 0.056(3) 0.183(7) 0.152(6) -0.087(5) 0.049(4) -0.024(4) O5 0.063(3) 0.030(2) 0.060(3) -0.019(2) 0.020(2) -0.003(2) C41 0.039(3) 0.035(4) 0.041(3) -0.010(3) 0.013(2) -0.005(3) C40 0.063(4) 0.071(5) 0.052(4) -0.004(4) 0.030(3) -0.019(4) C39 0.073(4) 0.031(4) 0.049(4) -0.002(3) -0.003(3) 0.011(3) N18 0.036(2) 0.032(3) 0.037(2) -0.004(2) 0.0035(19) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.480(6) . ? C1 C2 1.507(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.484(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.490(5) . ? C3 C4 1.512(7) . ? C3 C5 1.540(6) . ? C3 H3 0.9800 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.516(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N3 1.493(6) . ? C6 C7 1.535(7) . ? C6 C8 1.553(6) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 N3 1.476(6) . ? C9 C10 1.511(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N4 1.480(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N4 1.489(6) . ? C11 C12 1.510(8) . ? C11 C13 1.529(7) . ? C11 H11 0.9800 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.513(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N1 1.500(6) . ? C14 C15 1.514(7) . ? C14 C16 1.547(6) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N7 1.472(6) . ? C17 C18 1.502(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N8 1.489(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 N8 1.477(6) . ? C19 C21 1.537(7) . ? C19 C20 1.541(6) . ? C19 H19 0.9800 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.535(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.513(7) . ? C22 N5 1.517(6) . ? C22 C24 1.539(7) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N5 1.482(6) . ? C25 C26 1.486(7) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N6 1.477(6) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 N6 1.487(6) . ? C27 C28 1.525(6) . ? C27 C29 1.534(6) . ? C27 H27 0.9800 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.539(7) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 N7 1.508(6) . ? C30 C32 1.514(7) . ? C30 C31 1.523(7) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 N9 1.140(6) . ? C33 N10 1.300(7) . ? C34 N11 1.154(6) . ? C34 N10 1.303(6) . ? C35 N12 1.131(7) . ? C35 N13 1.332(7) . ? C36 N14 1.131(8) . ? C36 N13 1.336(8) . ? C37 N15 1.153(7) . ? C37 N16 1.324(7) . ? C38 N17 1.124(7) . ? C38 N16 1.320(8) . ? Cl1 O2 1.385(5) . ? Cl1 O4 1.397(5) . ? Cl1 O3 1.412(5) . ? Cl1 O1 1.425(4) . ? N1 Ni1 2.166(3) . ? N1 H1C 0.9100 . ? N2 Ni1 2.117(4) . ? N2 H2C 0.9100 . ? N3 Ni1 2.175(3) . ? N3 H3A 0.9100 . ? N4 Ni1 2.122(4) . ? N4 H4D 0.9100 . ? N5 Ni2 2.169(4) . ? N5 H5C 0.9100 . ? N6 Ni2 2.144(4) . ? N6 H6A 0.9100 . ? N7 Ni2 2.165(4) . ? N7 H7D 0.9100 . ? N8 Ni2 2.120(3) . ? N8 H8D 0.9100 . ? N9 Ni1 2.117(4) . ? N11 Ni2 2.104(3) . ? N12 Ni1 2.095(4) . ? N15 Ni2 2.131(4) . ? O5 C41 1.214(6) . ? C41 N18 1.321(7) . ? C41 H41 0.9300 . ? C40 N18 1.438(7) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C39 N18 1.437(7) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.1(4) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C1 109.5(4) . . ? N2 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? N2 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C4 111.0(4) . . ? N2 C3 C5 110.9(4) . . ? C4 C3 C5 109.1(4) . . ? N2 C3 H3 108.6 . . ? C4 C3 H3 108.6 . . ? C5 C3 H3 108.6 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C3 119.1(4) . . ? C6 C5 H5A 107.5 . . ? C3 C5 H5A 107.5 . . ? C6 C5 H5B 107.5 . . ? C3 C5 H5B 107.5 . . ? H5A C5 H5B 107.0 . . ? N3 C6 C5 110.1(3) . . ? N3 C6 C7 107.8(4) . . ? C5 C6 C7 111.4(4) . . ? N3 C6 C8 111.8(4) . . ? C5 C6 C8 108.8(4) . . ? C7 C6 C8 106.9(4) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C10 111.0(4) . . ? N3 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? N3 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N4 C10 C9 109.1(4) . . ? N4 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? N4 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? N4 C11 C12 112.6(5) . . ? N4 C11 C13 111.7(4) . . ? C12 C11 C13 108.0(4) . . ? N4 C11 H11 108.1 . . ? C12 C11 H11 108.1 . . ? C13 C11 H11 108.1 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C11 118.5(4) . . ? C14 C13 H13A 107.7 . . ? C11 C13 H13A 107.7 . . ? C14 C13 H13B 107.7 . . ? C11 C13 H13B 107.7 . . ? H13A C13 H13B 107.1 . . ? N1 C14 C13 110.8(4) . . ? N1 C14 C15 107.4(4) . . ? C13 C14 C15 112.1(5) . . ? N1 C14 C16 110.9(4) . . ? C13 C14 C16 108.8(4) . . ? C15 C14 C16 106.8(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N7 C17 C18 109.9(4) . . ? N7 C17 H17A 109.7 . . ? C18 C17 H17A 109.7 . . ? N7 C17 H17B 109.7 . . ? C18 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? N8 C18 C17 110.6(4) . . ? N8 C18 H18A 109.5 . . ? C17 C18 H18A 109.5 . . ? N8 C18 H18B 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? N8 C19 C21 111.2(4) . . ? N8 C19 C20 112.8(4) . . ? C21 C19 C20 107.3(4) . . ? N8 C19 H19 108.5 . . ? C21 C19 H19 108.5 . . ? C20 C19 H19 108.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C19 118.2(4) . . ? C22 C21 H21A 107.7 . . ? C19 C21 H21A 107.7 . . ? C22 C21 H21B 107.7 . . ? C19 C21 H21B 107.7 . . ? H21A C21 H21B 107.1 . . ? C23 C22 N5 107.8(4) . . ? C23 C22 C21 112.1(4) . . ? N5 C22 C21 109.8(4) . . ? C23 C22 C24 107.9(4) . . ? N5 C22 C24 111.3(4) . . ? C21 C22 C24 108.1(4) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 C26 110.0(4) . . ? N5 C25 H25A 109.7 . . ? C26 C25 H25A 109.7 . . ? N5 C25 H25B 109.7 . . ? C26 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? N6 C26 C25 110.2(4) . . ? N6 C26 H26A 109.6 . . ? C25 C26 H26A 109.6 . . ? N6 C26 H26B 109.6 . . ? C25 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? N6 C27 C28 112.9(4) . . ? N6 C27 C29 111.0(3) . . ? C28 C27 C29 109.6(4) . . ? N6 C27 H27 107.7 . . ? C28 C27 H27 107.7 . . ? C29 C27 H27 107.7 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 C30 120.0(4) . . ? C27 C29 H29A 107.3 . . ? C30 C29 H29A 107.3 . . ? C27 C29 H29B 107.3 . . ? C30 C29 H29B 107.3 . . ? H29A C29 H29B 106.9 . . ? N7 C30 C32 111.7(4) . . ? N7 C30 C31 106.5(4) . . ? C32 C30 C31 108.5(4) . . ? N7 C30 C29 110.5(4) . . ? C32 C30 C29 107.8(4) . . ? C31 C30 C29 111.9(4) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N9 C33 N10 172.5(5) . . ? N11 C34 N10 172.8(6) . . ? N12 C35 N13 168.4(7) . . ? N14 C36 N13 169.6(8) . . ? N15 C37 N16 166.1(6) . . ? N17 C38 N16 166.9(7) . . ? O2 Cl1 O4 108.2(5) . . ? O2 Cl1 O3 108.8(4) . . ? O4 Cl1 O3 108.0(4) . . ? O2 Cl1 O1 110.5(3) . . ? O4 Cl1 O1 110.3(3) . . ? O3 Cl1 O1 110.9(3) . . ? C1 N1 C14 112.9(3) . . ? C1 N1 Ni1 105.1(3) . . ? C14 N1 Ni1 121.3(3) . . ? C1 N1 H1C 105.5 . . ? C14 N1 H1C 105.5 . . ? Ni1 N1 H1C 105.5 . . ? C2 N2 C3 111.9(3) . . ? C2 N2 Ni1 104.2(3) . . ? C3 N2 Ni1 117.1(3) . . ? C2 N2 H2C 107.7 . . ? C3 N2 H2C 107.7 . . ? Ni1 N2 H2C 107.7 . . ? C9 N3 C6 112.5(4) . . ? C9 N3 Ni1 105.5(3) . . ? C6 N3 Ni1 122.0(3) . . ? C9 N3 H3A 105.1 . . ? C6 N3 H3A 105.1 . . ? Ni1 N3 H3A 105.1 . . ? C10 N4 C11 112.0(4) . . ? C10 N4 Ni1 104.8(3) . . ? C11 N4 Ni1 117.7(3) . . ? C10 N4 H4D 107.3 . . ? C11 N4 H4D 107.3 . . ? Ni1 N4 H4D 107.3 . . ? C25 N5 C22 113.7(4) . . ? C25 N5 Ni2 104.3(3) . . ? C22 N5 Ni2 121.4(3) . . ? C25 N5 H5C 105.4 . . ? C22 N5 H5C 105.4 . . ? Ni2 N5 H5C 105.4 . . ? C26 N6 C27 113.0(3) . . ? C26 N6 Ni2 103.8(3) . . ? C27 N6 Ni2 115.6(3) . . ? C26 N6 H6A 108.1 . . ? C27 N6 H6A 108.1 . . ? Ni2 N6 H6A 108.1 . . ? C17 N7 C30 112.9(4) . . ? C17 N7 Ni2 104.1(3) . . ? C30 N7 Ni2 122.1(3) . . ? C17 N7 H7D 105.5 . . ? C30 N7 H7D 105.5 . . ? Ni2 N7 H7D 105.5 . . ? C19 N8 C18 113.4(4) . . ? C19 N8 Ni2 117.3(3) . . ? C18 N8 Ni2 103.1(3) . . ? C19 N8 H8D 107.5 . . ? C18 N8 H8D 107.5 . . ? Ni2 N8 H8D 107.5 . . ? C33 N9 Ni1 148.5(4) . . ? C33 N10 C34 122.4(5) . . ? C34 N11 Ni2 158.5(4) . . ? C35 N12 Ni1 163.0(5) . . ? C35 N13 C36 117.4(6) . . ? C37 N15 Ni2 140.8(4) . . ? C38 N16 C37 125.0(6) . . ? N12 Ni1 N9 84.47(17) . . ? N12 Ni1 N2 88.55(16) . . ? N9 Ni1 N2 170.63(14) . . ? N12 Ni1 N4 171.90(16) . . ? N9 Ni1 N4 89.08(16) . . ? N2 Ni1 N4 98.37(15) . . ? N12 Ni1 N1 87.28(14) . . ? N9 Ni1 N1 101.67(15) . . ? N2 Ni1 N1 84.20(15) . . ? N4 Ni1 N1 89.23(13) . . ? N12 Ni1 N3 100.94(14) . . ? N9 Ni1 N3 86.25(14) . . ? N2 Ni1 N3 88.95(13) . . ? N4 Ni1 N3 83.48(13) . . ? N1 Ni1 N3 169.18(15) . . ? N11 Ni2 N8 169.78(16) . . ? N11 Ni2 N15 84.24(15) . . ? N8 Ni2 N15 89.70(15) . . ? N11 Ni2 N6 88.11(14) . . ? N8 Ni2 N6 98.98(15) . . ? N15 Ni2 N6 168.88(15) . . ? N11 Ni2 N7 102.83(15) . . ? N8 Ni2 N7 84.88(14) . . ? N15 Ni2 N7 85.93(16) . . ? N6 Ni2 N7 87.92(15) . . ? N11 Ni2 N5 86.13(14) . . ? N8 Ni2 N5 87.34(14) . . ? N15 Ni2 N5 103.74(16) . . ? N6 Ni2 N5 83.72(15) . . ? N7 Ni2 N5 167.56(14) . . ? O5 C41 N18 125.9(5) . . ? O5 C41 H41 117.0 . . ? N18 C41 H41 117.0 . . ? N18 C40 H40A 109.5 . . ? N18 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N18 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N18 C39 H39A 109.5 . . ? N18 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N18 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 N18 C39 121.2(5) . . ? C41 N18 C40 120.3(5) . . ? C39 N18 C40 118.5(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -58.1(5) . . . . ? N2 C3 C5 C6 71.9(5) . . . . ? C4 C3 C5 C6 -165.4(4) . . . . ? C3 C5 C6 N3 -63.8(5) . . . . ? C3 C5 C6 C7 55.8(5) . . . . ? C3 C5 C6 C8 173.4(4) . . . . ? N3 C9 C10 N4 -58.1(6) . . . . ? N4 C11 C13 C14 71.1(6) . . . . ? C12 C11 C13 C14 -164.6(5) . . . . ? C11 C13 C14 N1 -64.7(6) . . . . ? C11 C13 C14 C15 55.3(6) . . . . ? C11 C13 C14 C16 173.1(5) . . . . ? N7 C17 C18 N8 -60.9(5) . . . . ? N8 C19 C21 C22 70.3(5) . . . . ? C20 C19 C21 C22 -165.9(4) . . . . ? C19 C21 C22 C23 57.5(6) . . . . ? C19 C21 C22 N5 -62.3(6) . . . . ? C19 C21 C22 C24 176.3(4) . . . . ? N5 C25 C26 N6 -61.5(5) . . . . ? N6 C27 C29 C30 70.0(5) . . . . ? C28 C27 C29 C30 -164.6(4) . . . . ? C27 C29 C30 N7 -59.5(5) . . . . ? C27 C29 C30 C32 178.2(4) . . . . ? C27 C29 C30 C31 59.0(6) . . . . ? C2 C1 N1 C14 169.1(4) . . . . ? C2 C1 N1 Ni1 34.9(4) . . . . ? C13 C14 N1 C1 -74.8(5) . . . . ? C15 C14 N1 C1 162.5(4) . . . . ? C16 C14 N1 C1 46.1(5) . . . . ? C13 C14 N1 Ni1 51.2(5) . . . . ? C15 C14 N1 Ni1 -71.6(5) . . . . ? C16 C14 N1 Ni1 172.0(4) . . . . ? C1 C2 N2 C3 174.8(4) . . . . ? C1 C2 N2 Ni1 47.3(4) . . . . ? C4 C3 N2 C2 56.5(6) . . . . ? C5 C3 N2 C2 178.0(4) . . . . ? C4 C3 N2 Ni1 176.7(3) . . . . ? C5 C3 N2 Ni1 -61.8(5) . . . . ? C10 C9 N3 C6 170.4(4) . . . . ? C10 C9 N3 Ni1 35.1(5) . . . . ? C5 C6 N3 C9 -76.7(5) . . . . ? C7 C6 N3 C9 161.5(4) . . . . ? C8 C6 N3 C9 44.3(5) . . . . ? C5 C6 N3 Ni1 50.2(5) . . . . ? C7 C6 N3 Ni1 -71.6(4) . . . . ? C8 C6 N3 Ni1 171.2(3) . . . . ? C9 C10 N4 C11 176.3(4) . . . . ? C9 C10 N4 Ni1 47.6(5) . . . . ? C12 C11 N4 C10 56.7(6) . . . . ? C13 C11 N4 C10 178.4(4) . . . . ? C12 C11 N4 Ni1 178.2(4) . . . . ? C13 C11 N4 Ni1 -60.1(5) . . . . ? C26 C25 N5 C22 174.9(4) . . . . ? C26 C25 N5 Ni2 40.5(4) . . . . ? C23 C22 N5 C25 165.0(4) . . . . ? C21 C22 N5 C25 -72.6(5) . . . . ? C24 C22 N5 C25 46.9(5) . . . . ? C23 C22 N5 Ni2 -69.3(4) . . . . ? C21 C22 N5 Ni2 53.1(5) . . . . ? C24 C22 N5 Ni2 172.7(3) . . . . ? C25 C26 N6 C27 171.8(4) . . . . ? C25 C26 N6 Ni2 45.8(4) . . . . ? C28 C27 N6 C26 51.9(5) . . . . ? C29 C27 N6 C26 175.4(4) . . . . ? C28 C27 N6 Ni2 171.2(3) . . . . ? C29 C27 N6 Ni2 -65.3(4) . . . . ? C18 C17 N7 C30 174.2(4) . . . . ? C18 C17 N7 Ni2 39.7(4) . . . . ? C32 C30 N7 C17 44.6(6) . . . . ? C31 C30 N7 C17 162.8(4) . . . . ? C29 C30 N7 C17 -75.5(5) . . . . ? C32 C30 N7 Ni2 169.9(3) . . . . ? C31 C30 N7 Ni2 -71.9(4) . . . . ? C29 C30 N7 Ni2 49.8(5) . . . . ? C21 C19 N8 C18 175.1(4) . . . . ? C20 C19 N8 C18 54.4(6) . . . . ? C21 C19 N8 Ni2 -64.7(4) . . . . ? C20 C19 N8 Ni2 174.6(3) . . . . ? C17 C18 N8 C19 173.3(4) . . . . ? C17 C18 N8 Ni2 45.4(4) . . . . ? N10 C33 N9 Ni1 -133(4) . . . . ? N9 C33 N10 C34 -180(100) . . . . ? N11 C34 N10 C33 172(5) . . . . ? N10 C34 N11 Ni2 -147(4) . . . . ? N13 C35 N12 Ni1 168.2(19) . . . . ? N12 C35 N13 C36 -174(3) . . . . ? N14 C36 N13 C35 162(4) . . . . ? N16 C37 N15 Ni2 -58(3) . . . . ? N17 C38 N16 C37 -150(3) . . . . ? N15 C37 N16 C38 149(2) . . . . ? C35 N12 Ni1 N9 17.2(14) . . . . ? C35 N12 Ni1 N2 -169.0(14) . . . . ? C35 N12 Ni1 N4 -20(2) . . . . ? C35 N12 Ni1 N1 -84.8(14) . . . . ? C35 N12 Ni1 N3 102.3(14) . . . . ? C33 N9 Ni1 N12 7.9(7) . . . . ? C33 N9 Ni1 N2 -34.2(14) . . . . ? C33 N9 Ni1 N4 -177.0(7) . . . . ? C33 N9 Ni1 N1 94.0(7) . . . . ? C33 N9 Ni1 N3 -93.5(7) . . . . ? C2 N2 Ni1 N12 65.7(3) . . . . ? C3 N2 Ni1 N12 -58.5(3) . . . . ? C2 N2 Ni1 N9 107.5(9) . . . . ? C3 N2 Ni1 N9 -16.7(11) . . . . ? C2 N2 Ni1 N4 -110.1(3) . . . . ? C3 N2 Ni1 N4 125.7(3) . . . . ? C2 N2 Ni1 N1 -21.7(3) . . . . ? C3 N2 Ni1 N1 -145.9(3) . . . . ? C2 N2 Ni1 N3 166.6(3) . . . . ? C3 N2 Ni1 N3 42.4(3) . . . . ? C10 N4 Ni1 N12 101.6(11) . . . . ? C11 N4 Ni1 N12 -23.6(13) . . . . ? C10 N4 Ni1 N9 64.3(3) . . . . ? C11 N4 Ni1 N9 -60.9(3) . . . . ? C10 N4 Ni1 N2 -110.0(3) . . . . ? C11 N4 Ni1 N2 124.8(3) . . . . ? C10 N4 Ni1 N1 166.0(3) . . . . ? C11 N4 Ni1 N1 40.8(3) . . . . ? C10 N4 Ni1 N3 -22.0(3) . . . . ? C11 N4 Ni1 N3 -147.2(3) . . . . ? C1 N1 Ni1 N12 -95.6(3) . . . . ? C14 N1 Ni1 N12 135.0(4) . . . . ? C1 N1 Ni1 N9 -179.4(3) . . . . ? C14 N1 Ni1 N9 51.2(4) . . . . ? C1 N1 Ni1 N2 -6.8(3) . . . . ? C14 N1 Ni1 N2 -136.2(4) . . . . ? C1 N1 Ni1 N4 91.7(3) . . . . ? C14 N1 Ni1 N4 -37.7(4) . . . . ? C1 N1 Ni1 N3 44.2(9) . . . . ? C14 N1 Ni1 N3 -85.2(9) . . . . ? C9 N3 Ni1 N12 180.0(3) . . . . ? C6 N3 Ni1 N12 50.1(3) . . . . ? C9 N3 Ni1 N9 -96.4(3) . . . . ? C6 N3 Ni1 N9 133.7(3) . . . . ? C9 N3 Ni1 N2 91.7(3) . . . . ? C6 N3 Ni1 N2 -38.3(3) . . . . ? C9 N3 Ni1 N4 -6.9(3) . . . . ? C6 N3 Ni1 N4 -136.8(3) . . . . ? C9 N3 Ni1 N1 41.0(9) . . . . ? C6 N3 Ni1 N1 -88.9(8) . . . . ? C34 N11 Ni2 N8 -42.4(17) . . . . ? C34 N11 Ni2 N15 11.5(11) . . . . ? C34 N11 Ni2 N6 -176.6(12) . . . . ? C34 N11 Ni2 N7 96.0(11) . . . . ? C34 N11 Ni2 N5 -92.8(11) . . . . ? C19 N8 Ni2 N11 -3.7(10) . . . . ? C18 N8 Ni2 N11 121.7(8) . . . . ? C19 N8 Ni2 N15 -57.2(3) . . . . ? C18 N8 Ni2 N15 68.3(3) . . . . ? C19 N8 Ni2 N6 129.8(3) . . . . ? C18 N8 Ni2 N6 -104.8(3) . . . . ? C19 N8 Ni2 N7 -143.1(3) . . . . ? C18 N8 Ni2 N7 -17.7(3) . . . . ? C19 N8 Ni2 N5 46.6(3) . . . . ? C18 N8 Ni2 N5 172.0(3) . . . . ? C37 N15 Ni2 N11 9.4(7) . . . . ? C37 N15 Ni2 N8 -178.9(7) . . . . ? C37 N15 Ni2 N6 -37.4(12) . . . . ? C37 N15 Ni2 N7 -94.0(7) . . . . ? C37 N15 Ni2 N5 93.9(7) . . . . ? C26 N6 Ni2 N11 68.6(3) . . . . ? C27 N6 Ni2 N11 -55.6(3) . . . . ? C26 N6 Ni2 N8 -104.0(3) . . . . ? C27 N6 Ni2 N8 131.8(3) . . . . ? C26 N6 Ni2 N15 115.1(8) . . . . ? C27 N6 Ni2 N15 -9.1(9) . . . . ? C26 N6 Ni2 N7 171.6(3) . . . . ? C27 N6 Ni2 N7 47.3(3) . . . . ? C26 N6 Ni2 N5 -17.7(3) . . . . ? C27 N6 Ni2 N5 -141.9(3) . . . . ? C17 N7 Ni2 N11 175.1(3) . . . . ? C30 N7 Ni2 N11 45.9(4) . . . . ? C17 N7 Ni2 N8 -11.7(3) . . . . ? C30 N7 Ni2 N8 -140.9(4) . . . . ? C17 N7 Ni2 N15 -101.7(3) . . . . ? C30 N7 Ni2 N15 129.1(4) . . . . ? C17 N7 Ni2 N6 87.5(3) . . . . ? C30 N7 Ni2 N6 -41.7(3) . . . . ? C17 N7 Ni2 N5 39.8(8) . . . . ? C30 N7 Ni2 N5 -89.4(7) . . . . ? C25 N5 Ni2 N11 -100.4(3) . . . . ? C22 N5 Ni2 N11 129.7(3) . . . . ? C25 N5 Ni2 N8 87.4(3) . . . . ? C22 N5 Ni2 N8 -42.5(3) . . . . ? C25 N5 Ni2 N15 176.5(3) . . . . ? C22 N5 Ni2 N15 46.6(3) . . . . ? C25 N5 Ni2 N6 -11.9(3) . . . . ? C22 N5 Ni2 N6 -141.8(3) . . . . ? C25 N5 Ni2 N7 36.2(8) . . . . ? C22 N5 Ni2 N7 -93.8(7) . . . . ? O5 C41 N18 C39 178.1(5) . . . . ? O5 C41 N18 C40 -0.9(8) . . . . ? 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 N1 H1C N17 0.91 2.29 3.170(6) 162.7 1_455 N2 H2C O5 0.91 2.10 2.972(5) 159.3 . N4 H4D O5 0.91 2.06 2.956(6) 166.1 . N6 H6A O2 0.91 2.32 3.187(6) 159.7 . N7 H7D N14 0.91 2.31 3.150(7) 154.0 1_655 N8 H8D O3 0.91 2.22 3.109(7) 164.4 . _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.725 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.065 # Attachment '\L-2.cif' data_\L-2 _database_code_depnum_ccdc_archive 'CCDC 722170' # start Validation Reply Form _vrf_PLAT023_\L-2 ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 61.44 Deg. RESPONSE: The low data completeness of \L-2 is due to the defect of CrysAlis CCD, Gemini S Ultra (Oxford Diffraction Ltd.) when using Cu radiation. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H79 Cl N18 Ni2 O5' _chemical_formula_weight 1057.09 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.15950(10) _cell_length_b 28.7807(3) _cell_length_c 10.26460(10) _cell_angle_alpha 90.00 _cell_angle_beta 104.5420(10) _cell_angle_gamma 90.00 _cell_volume 2619.23(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1296 _cell_measurement_theta_min 2.8327 _cell_measurement_theta_max 62.3152 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.843 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5188 _exptl_absorpt_correction_T_max 0.5815 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0855 _diffrn_measurement_device_type 'Gemini S Ultra' _diffrn_measurement_method '\w and \p scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9801 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 61.12 _reflns_number_total 6609 _reflns_number_gt 6040 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _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^)+(0.0485P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.014(17) _refine_ls_number_reflns 6609 _refine_ls_number_parameters 616 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 1.024 _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 C1 C 0.2885(4) 0.75275(16) 0.4064(4) 0.0359(10) Uani 1 1 d . . . H1A H 0.1844 0.7474 0.4146 0.043 Uiso 1 1 calc R . . H1B H 0.3265 0.7233 0.3778 0.043 Uiso 1 1 calc R . . C2 C 0.2877(4) 0.78946(16) 0.3034(4) 0.0359(10) Uani 1 1 d . . . H2A H 0.2198 0.7801 0.2163 0.043 Uiso 1 1 calc R . . H2B H 0.2498 0.8190 0.3319 0.043 Uiso 1 1 calc R . . C3 C 0.4551(5) 0.83569(15) 0.1968(4) 0.0323(9) Uani 1 1 d . . . H3 H 0.4343 0.8651 0.2408 0.039 Uiso 1 1 calc R . . C4 C 0.3411(5) 0.83195(16) 0.0587(4) 0.0438(11) Uani 1 1 d . . . H4A H 0.3542 0.8021 0.0172 0.066 Uiso 1 1 calc R . . H4B H 0.3582 0.8573 0.0006 0.066 Uiso 1 1 calc R . . H4C H 0.2384 0.8341 0.0704 0.066 Uiso 1 1 calc R . . C5 C 0.6130(5) 0.83901(15) 0.1737(4) 0.0353(9) Uani 1 1 d . . . H5A H 0.6079 0.8609 0.0984 0.042 Uiso 1 1 calc R . . H5B H 0.6384 0.8081 0.1430 0.042 Uiso 1 1 calc R . . C6 C 0.7449(5) 0.85411(15) 0.2901(4) 0.0326(9) Uani 1 1 d . . . C7 C 0.7166(5) 0.90174(15) 0.3453(4) 0.0401(10) Uani 1 1 d . . . H7A H 0.6324 0.8995 0.3880 0.060 Uiso 1 1 calc R . . H7B H 0.6918 0.9242 0.2714 0.060 Uiso 1 1 calc R . . H7C H 0.8075 0.9119 0.4119 0.060 Uiso 1 1 calc R . . C8 C 0.8876(5) 0.85780(17) 0.2392(4) 0.0449(11) Uani 1 1 d . . . H8A H 0.8770 0.8835 0.1749 0.067 Uiso 1 1 calc R . . H8B H 0.9028 0.8287 0.1948 0.067 Uiso 1 1 calc R . . H8C H 0.9747 0.8635 0.3154 0.067 Uiso 1 1 calc R . . C9 C 0.8317(5) 0.77515(15) 0.3783(4) 0.0352(10) Uani 1 1 d . . . H9A H 0.9358 0.7806 0.3703 0.042 Uiso 1 1 calc R . . H9B H 0.7721 0.7621 0.2920 0.042 Uiso 1 1 calc R . . C10 C 0.8343(4) 0.74127(15) 0.4892(4) 0.0318(9) Uani 1 1 d . . . H10A H 0.8821 0.7119 0.4711 0.038 Uiso 1 1 calc R . . H10B H 0.8946 0.7541 0.5754 0.038 Uiso 1 1 calc R . . C11 C 0.6746(4) 0.70454(14) 0.6207(4) 0.0304(9) Uani 1 1 d . . . H11 H 0.7170 0.7243 0.7015 0.036 Uiso 1 1 calc R . . C12 C 0.7691(5) 0.65991(15) 0.6343(5) 0.0428(11) Uani 1 1 d . . . H12A H 0.7348 0.6410 0.5529 0.064 Uiso 1 1 calc R . . H12B H 0.7572 0.6422 0.7126 0.064 Uiso 1 1 calc R . . H12C H 0.8755 0.6680 0.6462 0.064 Uiso 1 1 calc R . . C13 C 0.5125(5) 0.69174(15) 0.6213(4) 0.0351(10) Uani 1 1 d . . . H13A H 0.5177 0.6678 0.6918 0.042 Uiso 1 1 calc R . . H13B H 0.4656 0.6769 0.5339 0.042 Uiso 1 1 calc R . . C14 C 0.4046(4) 0.73026(15) 0.6446(4) 0.0313(9) Uani 1 1 d . . . C15 C 0.4632(5) 0.75410(18) 0.7800(4) 0.0407(10) Uani 1 1 d . . . H15A H 0.5587 0.7697 0.7819 0.061 Uiso 1 1 calc R . . H15B H 0.4794 0.7309 0.8521 0.061 Uiso 1 1 calc R . . H15C H 0.3892 0.7770 0.7933 0.061 Uiso 1 1 calc R . . C16 C 0.2551(5) 0.70698(18) 0.6454(5) 0.0501(12) Uani 1 1 d . . . H16A H 0.1789 0.7308 0.6459 0.075 Uiso 1 1 calc R . . H16B H 0.2684 0.6876 0.7260 0.075 Uiso 1 1 calc R . . H16C H 0.2221 0.6876 0.5649 0.075 Uiso 1 1 calc R . . C17 C 1.2581(4) 1.04740(15) 0.9711(4) 0.0307(9) Uani 1 1 d . . . H17A H 1.3690 1.0445 0.9879 0.037 Uiso 1 1 calc R . . H17B H 1.2363 1.0714 1.0328 0.037 Uiso 1 1 calc R . . C18 C 1.1921(4) 1.06209(15) 0.8272(4) 0.0313(9) Uani 1 1 d . . . H18A H 1.2349 1.0924 0.8104 0.038 Uiso 1 1 calc R . . H18B H 1.2179 1.0389 0.7652 0.038 Uiso 1 1 calc R . . C19 C 0.9532(4) 1.07665(14) 0.6589(4) 0.0293(9) Uani 1 1 d . . . H19 H 0.9740 1.0503 0.6025 0.035 Uiso 1 1 calc R . . C20 C 1.0153(5) 1.12103(18) 0.6126(4) 0.0459(12) Uani 1 1 d . . . H20A H 0.9900 1.1475 0.6627 0.069 Uiso 1 1 calc R . . H20B H 0.9708 1.1255 0.5161 0.069 Uiso 1 1 calc R . . H20C H 1.1252 1.1186 0.6291 0.069 Uiso 1 1 calc R . . C21 C 0.7803(4) 1.08175(14) 0.6345(4) 0.0334(9) Uani 1 1 d . . . H21A H 0.7612 1.1039 0.7020 0.040 Uiso 1 1 calc R . . H21B H 0.7419 1.0963 0.5450 0.040 Uiso 1 1 calc R . . C22 C 0.6852(4) 1.03863(14) 0.6390(4) 0.0296(9) Uani 1 1 d . . . C23 C 0.7091(4) 1.00188(17) 0.5410(4) 0.0362(9) Uani 1 1 d . . . H23A H 0.8155 0.9927 0.5636 0.054 Uiso 1 1 calc R . . H23B H 0.6809 1.0144 0.4494 0.054 Uiso 1 1 calc R . . H23C H 0.6464 0.9747 0.5467 0.054 Uiso 1 1 calc R . . C24 C 0.5167(5) 1.05279(17) 0.5971(5) 0.0439(11) Uani 1 1 d . . . H24A H 0.4542 1.0264 0.6100 0.066 Uiso 1 1 calc R . . H24B H 0.4896 1.0620 0.5021 0.066 Uiso 1 1 calc R . . H24C H 0.4997 1.0789 0.6526 0.066 Uiso 1 1 calc R . . C25 C 0.6660(5) 1.04431(16) 0.8752(4) 0.0367(10) Uani 1 1 d . . . H25A H 0.5548 1.0411 0.8521 0.044 Uiso 1 1 calc R . . H25B H 0.6905 1.0776 0.8700 0.044 Uiso 1 1 calc R . . C26 C 0.7306(4) 1.02699(17) 1.0157(4) 0.0376(10) Uani 1 1 d . . . H26A H 0.6884 1.0450 1.0799 0.045 Uiso 1 1 calc R . . H26B H 0.7040 0.9939 1.0222 0.045 Uiso 1 1 calc R . . C27 C 0.9705(5) 1.01254(19) 1.1854(4) 0.0433(11) Uani 1 1 d U . . H27 H 0.9484 0.9785 1.1843 0.052 Uiso 1 1 calc R . . C28 C 0.9104(7) 1.0354(3) 1.2964(5) 0.0758(16) Uani 1 1 d U . . H28A H 0.9259 1.0691 1.2949 0.114 Uiso 1 1 calc R . . H28B H 0.9644 1.0230 1.3842 0.114 Uiso 1 1 calc R . . H28C H 0.8024 1.0289 1.2811 0.114 Uiso 1 1 calc R . . C29 C 1.1413(5) 1.01932(17) 1.2200(4) 0.0405(11) Uani 1 1 d . . . H29A H 1.1612 1.0524 1.2049 0.049 Uiso 1 1 calc R . . H29B H 1.1807 1.0132 1.3174 0.049 Uiso 1 1 calc R . . C30 C 1.2322(4) 0.99046(14) 1.1458(4) 0.0339(10) Uani 1 1 d . . . C31 C 1.2048(6) 0.93814(17) 1.1569(4) 0.0514(13) Uani 1 1 d . . . H31A H 1.1000 0.9308 1.1112 0.077 Uiso 1 1 calc R . . H31B H 1.2243 0.9294 1.2520 0.077 Uiso 1 1 calc R . . H31C H 1.2728 0.9208 1.1147 0.077 Uiso 1 1 calc R . . C32 C 1.4013(4) 0.99892(19) 1.2104(4) 0.0477(11) Uani 1 1 d . . . H32A H 1.4615 0.9846 1.1546 0.072 Uiso 1 1 calc R . . H32B H 1.4287 0.9851 1.3006 0.072 Uiso 1 1 calc R . . H32C H 1.4211 1.0324 1.2171 0.072 Uiso 1 1 calc R . . C33 C 0.7782(5) 0.83570(14) 0.7709(4) 0.0327(9) Uani 1 1 d U . . C34 C 0.8599(5) 0.89928(15) 0.9012(4) 0.0355(10) Uani 1 1 d U . . C35 C 0.4767(6) 0.89209(16) 0.5952(5) 0.0444(11) Uani 1 1 d . . . C36 C 0.4482(5) 0.93056(17) 0.7877(5) 0.0492(12) Uani 1 1 d . . . C37 C 1.0670(5) 0.93798(17) 0.6708(4) 0.0451(11) Uani 1 1 d U . . C38 C 1.1143(5) 0.8648(2) 0.6058(6) 0.0621(16) Uani 1 1 d U . . Cl1 Cl 0.49310(11) 0.67508(3) 0.14124(9) 0.0346(2) Uani 1 1 d . . . N1 N 0.3857(4) 0.76708(11) 0.5385(3) 0.0291(7) Uani 1 1 d . . . H1C H 0.3341 0.7911 0.5678 0.035 Uiso 1 1 calc R . . N2 N 0.4436(3) 0.79611(12) 0.2876(3) 0.0270(7) Uani 1 1 d . . . H2C H 0.4703 0.7692 0.2489 0.032 Uiso 1 1 calc R . . N3 N 0.7645(3) 0.81964(11) 0.4055(3) 0.0277(7) Uani 1 1 d . . . H3A H 0.8351 0.8330 0.4769 0.033 Uiso 1 1 calc R . . N4 N 0.6792(3) 0.73186(11) 0.4994(3) 0.0247(7) Uani 1 1 d . . . H4D H 0.6298 0.7150 0.4239 0.030 Uiso 1 1 calc R . . N5 N 1.1930(3) 1.00221(12) 0.9982(3) 0.0268(6) Uani 1 1 d . . . H5C H 1.2405 0.9798 0.9581 0.032 Uiso 1 1 calc R . . N6 N 1.0254(3) 1.06593(11) 0.8021(3) 0.0248(7) Uani 1 1 d . . . H6A H 1.0047 1.0904 0.8539 0.030 Uiso 1 1 calc R . . N7 N 0.7277(3) 1.01766(11) 0.7770(3) 0.0268(7) Uani 1 1 d . . . H7D H 0.6792 0.9890 0.7687 0.032 Uiso 1 1 calc R . . N8 N 0.8973(3) 1.03236(12) 1.0493(3) 0.0278(7) Uani 1 1 d . . . H8D H 0.9187 1.0640 1.0517 0.033 Uiso 1 1 calc R . . N9 N 0.7227(4) 0.81443(11) 0.6772(3) 0.0293(7) Uani 1 1 d . . . N10 N 0.8436(6) 0.85461(13) 0.8864(4) 0.0613(12) Uani 1 1 d U . . N11 N 0.8813(4) 0.93791(12) 0.9281(3) 0.0326(8) Uani 1 1 d . . . N12 N 0.4746(4) 0.86395(12) 0.5149(3) 0.0324(8) Uani 1 1 d . . . N13 N 0.5125(6) 0.92466(17) 0.6880(5) 0.0733(15) Uani 1 1 d . . . N14 N 0.4170(5) 0.93937(17) 0.8838(5) 0.0604(12) Uani 1 1 d . . . N15 N 1.0334(4) 0.96671(12) 0.7324(3) 0.0333(8) Uani 1 1 d . . . N16 N 1.1180(6) 0.91150(19) 0.5879(5) 0.0770(14) Uani 1 1 d U . . N17 N 1.1239(6) 0.82580(17) 0.6080(6) 0.0772(16) Uani 1 1 d . . . Ni1 Ni 0.57766(6) 0.79952(2) 0.48734(5) 0.02300(15) Uani 1 1 d . . . Ni2 Ni 0.96050(6) 1.00347(2) 0.88144(5) 0.02057(14) Uani 1 1 d . . . O1 O 0.5870(6) 0.65800(16) 0.2615(4) 0.1023(18) Uani 1 1 d . . . O2 O 0.3473(5) 0.6795(2) 0.1600(6) 0.124(2) Uani 1 1 d . . . O3 O 0.5427(6) 0.71956(13) 0.1159(4) 0.0926(16) Uani 1 1 d . . . O4 O 0.4922(5) 0.64379(12) 0.0338(3) 0.0654(10) Uani 1 1 d . . . O5 O 0.9943(4) 1.12863(11) 1.0229(3) 0.0510(8) Uani 1 1 d . . . C39 C 0.9571(6) 1.24977(17) 1.0790(5) 0.0585(14) Uani 1 1 d . . . H39A H 0.8691 1.2432 1.1141 0.088 Uiso 1 1 calc R . . H39B H 0.9273 1.2702 1.0005 0.088 Uiso 1 1 calc R . . H39C H 1.0350 1.2650 1.1489 0.088 Uiso 1 1 calc R . . C40 C 1.1467(6) 1.2095(2) 0.9865(6) 0.0637(15) Uani 1 1 d . . . H40A H 1.1752 1.1782 0.9645 0.096 Uiso 1 1 calc R . . H40B H 1.2305 1.2235 1.0537 0.096 Uiso 1 1 calc R . . H40C H 1.1236 1.2286 0.9050 0.096 Uiso 1 1 calc R . . C41 C 0.9507(5) 1.16670(15) 1.0524(4) 0.0394(10) Uani 1 1 d . . . H41A H 0.8635 1.1673 1.0866 0.047 Uiso 1 1 calc R . . N18 N 1.0157(4) 1.20679(12) 1.0400(3) 0.0384(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.022(2) 0.049(3) 0.035(2) -0.011(2) 0.0047(16) -0.0041(19) C2 0.028(2) 0.046(3) 0.030(2) -0.0064(19) 0.0005(16) 0.0002(19) C3 0.040(2) 0.032(2) 0.022(2) -0.0014(17) 0.0000(16) 0.0023(18) C4 0.055(3) 0.039(3) 0.029(2) -0.0015(19) -0.0054(19) 0.004(2) C5 0.050(2) 0.034(2) 0.023(2) 0.0005(17) 0.0100(17) -0.0019(19) C6 0.041(2) 0.032(2) 0.027(2) 0.0028(17) 0.0115(17) -0.0080(19) C7 0.050(3) 0.033(2) 0.037(3) 0.000(2) 0.0105(19) -0.007(2) C8 0.055(3) 0.051(3) 0.034(2) 0.006(2) 0.020(2) -0.008(2) C9 0.030(2) 0.043(2) 0.037(2) 0.0013(19) 0.0185(18) 0.0065(19) C10 0.026(2) 0.034(2) 0.036(2) 0.0010(18) 0.0095(16) 0.0121(18) C11 0.035(2) 0.030(2) 0.026(2) 0.0002(17) 0.0081(16) 0.0047(18) C12 0.050(3) 0.034(2) 0.045(3) 0.008(2) 0.013(2) 0.012(2) C13 0.041(2) 0.032(2) 0.034(2) 0.0024(18) 0.0119(18) -0.0045(18) C14 0.031(2) 0.037(2) 0.029(2) 0.0006(18) 0.0133(16) -0.0022(18) C15 0.044(2) 0.052(3) 0.031(2) -0.001(2) 0.0173(18) -0.001(2) C16 0.043(3) 0.056(3) 0.057(3) 0.004(2) 0.024(2) -0.006(2) C17 0.026(2) 0.037(2) 0.030(2) -0.0001(18) 0.0085(16) -0.0059(17) C18 0.023(2) 0.035(2) 0.037(2) 0.0041(18) 0.0098(16) -0.0021(17) C19 0.035(2) 0.032(2) 0.023(2) 0.0063(17) 0.0107(16) -0.0034(17) C20 0.045(3) 0.053(3) 0.038(3) 0.022(2) 0.007(2) -0.010(2) C21 0.037(2) 0.034(2) 0.027(2) 0.0053(17) 0.0021(16) -0.0006(18) C22 0.027(2) 0.031(2) 0.029(2) 0.0017(17) 0.0032(15) 0.0023(17) C23 0.037(2) 0.039(2) 0.029(2) -0.002(2) 0.0004(15) 0.000(2) C24 0.034(2) 0.046(3) 0.046(3) 0.002(2) 0.0002(19) 0.004(2) C25 0.028(2) 0.047(3) 0.038(2) -0.004(2) 0.0132(17) 0.0080(19) C26 0.033(2) 0.048(3) 0.038(2) -0.005(2) 0.0205(18) -0.003(2) C27 0.045(2) 0.064(3) 0.0234(19) -0.0007(19) 0.0131(16) -0.007(2) C28 0.070(3) 0.121(4) 0.045(3) -0.011(3) 0.031(2) 0.000(3) C29 0.044(2) 0.054(3) 0.020(2) -0.0035(18) 0.0027(16) -0.011(2) C30 0.032(2) 0.035(2) 0.029(2) -0.0006(18) -0.0029(16) -0.0036(18) C31 0.068(3) 0.041(3) 0.034(2) 0.013(2) -0.007(2) 0.001(2) C32 0.037(2) 0.059(3) 0.037(2) -0.001(2) -0.0105(17) 0.000(2) C33 0.051(2) 0.0190(19) 0.024(2) 0.0040(17) 0.0022(18) 0.0002(18) C34 0.054(3) 0.031(3) 0.0182(19) -0.0002(17) 0.0019(17) -0.003(2) C35 0.066(3) 0.030(2) 0.049(3) -0.001(2) 0.036(2) -0.002(2) C36 0.047(3) 0.048(3) 0.062(3) -0.024(3) 0.032(2) -0.016(2) C37 0.052(3) 0.048(3) 0.032(2) -0.011(2) 0.0032(19) 0.024(2) C38 0.037(3) 0.063(4) 0.078(4) -0.044(3) -0.001(2) 0.015(2) Cl1 0.0442(6) 0.0291(5) 0.0308(5) -0.0019(4) 0.0102(4) -0.0004(4) N1 0.0268(17) 0.0325(19) 0.0281(18) -0.0046(15) 0.0073(13) -0.0001(14) N2 0.0270(16) 0.0282(17) 0.0256(16) -0.0036(15) 0.0063(12) 0.0030(15) N3 0.0277(17) 0.0316(18) 0.0239(17) -0.0003(14) 0.0065(12) -0.0005(14) N4 0.0245(16) 0.0291(17) 0.0208(16) -0.0021(13) 0.0061(12) 0.0007(13) N5 0.0304(16) 0.0275(16) 0.0219(15) -0.0037(15) 0.0054(12) 0.0024(15) N6 0.0236(16) 0.0293(18) 0.0226(16) -0.0011(14) 0.0078(13) -0.0021(14) N7 0.0225(15) 0.0281(18) 0.0299(17) -0.0003(13) 0.0070(12) -0.0017(13) N8 0.0290(18) 0.0320(18) 0.0261(17) -0.0020(14) 0.0141(13) -0.0041(14) N9 0.0345(17) 0.0251(17) 0.0283(18) -0.0041(15) 0.0082(14) -0.0006(14) N10 0.112(3) 0.0247(19) 0.029(2) -0.0029(15) -0.017(2) -0.006(2) N11 0.0378(19) 0.027(2) 0.0291(18) -0.0004(15) 0.0015(14) -0.0061(15) N12 0.0369(19) 0.034(2) 0.0279(18) -0.0018(17) 0.0114(14) 0.0018(15) N13 0.093(4) 0.059(3) 0.086(3) -0.034(3) 0.058(3) -0.031(3) N14 0.052(3) 0.072(3) 0.059(3) -0.026(2) 0.016(2) 0.007(2) N15 0.0331(19) 0.037(2) 0.0283(18) -0.0059(16) 0.0049(14) 0.0052(16) N16 0.101(3) 0.073(3) 0.058(3) -0.022(2) 0.022(2) 0.027(3) N17 0.068(3) 0.047(3) 0.129(5) -0.045(3) 0.049(3) -0.011(2) Ni1 0.0246(3) 0.0231(3) 0.0213(3) -0.0036(3) 0.0058(2) 0.0019(3) Ni2 0.0231(3) 0.0202(3) 0.0192(3) -0.0027(3) 0.0068(2) -0.0004(3) O1 0.157(5) 0.068(3) 0.057(2) 0.000(2) -0.020(3) 0.032(3) O2 0.060(3) 0.171(6) 0.152(5) -0.083(4) 0.045(3) -0.017(3) O3 0.180(5) 0.040(2) 0.081(3) -0.015(2) 0.075(3) -0.030(3) O4 0.109(3) 0.042(2) 0.050(2) -0.0221(16) 0.027(2) -0.012(2) O5 0.068(2) 0.0298(17) 0.059(2) -0.0158(15) 0.0229(17) -0.0013(16) C39 0.077(4) 0.032(3) 0.059(3) -0.005(2) 0.001(3) 0.006(3) C40 0.060(3) 0.075(4) 0.061(3) -0.003(3) 0.024(3) -0.022(3) C41 0.038(2) 0.039(3) 0.043(3) -0.008(2) 0.0142(18) -0.003(2) N18 0.041(2) 0.032(2) 0.040(2) -0.0029(15) 0.0058(15) -0.0036(16) _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 C1 N1 1.481(5) . ? C1 C2 1.494(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.489(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N2 1.492(5) . ? C3 C5 1.526(6) . ? C3 C4 1.539(5) . ? C3 H3 1.0000 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.533(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N3 1.521(5) . ? C6 C8 1.529(6) . ? C6 C7 1.530(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N3 1.478(5) . ? C9 C10 1.494(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N4 1.475(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N4 1.483(5) . ? C11 C13 1.531(5) . ? C11 C12 1.535(6) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.544(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N1 1.498(5) . ? C14 C15 1.522(6) . ? C14 C16 1.526(6) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 N5 1.486(5) . ? C17 C18 1.509(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N6 1.488(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 N6 1.485(5) . ? C19 C20 1.522(6) . ? C19 C21 1.548(6) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.523(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N7 1.498(5) . ? C22 C23 1.513(6) . ? C22 C24 1.549(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N7 1.487(5) . ? C25 C26 1.500(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 N8 1.487(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 N8 1.502(5) . ? C27 C29 1.528(6) . ? C27 C28 1.533(7) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.511(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 N5 1.505(5) . ? C30 C31 1.536(6) . ? C30 C32 1.544(5) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 N9 1.146(5) . ? C33 N10 1.305(6) . ? C34 N11 1.151(5) . ? C34 N10 1.299(6) . ? C35 N12 1.152(5) . ? C35 N13 1.318(7) . ? C36 N14 1.122(6) . ? C36 N13 1.315(7) . ? C37 N15 1.130(5) . ? C37 N16 1.313(6) . ? C38 N17 1.127(8) . ? C38 N16 1.357(8) . ? Cl1 O2 1.402(4) . ? Cl1 O1 1.404(4) . ? Cl1 O3 1.404(4) . ? Cl1 O4 1.422(3) . ? N1 Ni1 2.169(3) . ? N1 H1C 0.9300 . ? N2 Ni1 2.111(3) . ? N2 H2C 0.9300 . ? N3 Ni1 2.166(3) . ? N3 H3A 0.9300 . ? N4 Ni1 2.148(3) . ? N4 H4D 0.9300 . ? N5 Ni2 2.166(3) . ? N5 H5C 0.9300 . ? N6 Ni2 2.119(3) . ? N6 H6A 0.9300 . ? N7 Ni2 2.172(3) . ? N7 H7D 0.9300 . ? N8 Ni2 2.121(3) . ? N8 H8D 0.9300 . ? N9 Ni1 2.109(3) . ? N11 Ni2 2.119(3) . ? N12 Ni1 2.132(4) . ? N15 Ni2 2.102(3) . ? O5 C41 1.230(5) . ? C39 N18 1.445(6) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 N18 1.442(6) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 N18 1.319(6) . ? C41 H41A 0.9500 . ? 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 N1 C1 C2 110.2(3) . . ? N1 C1 H1A 109.6 . . ? C2 C1 H1A 109.6 . . ? N1 C1 H1B 109.6 . . ? C2 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? N2 C2 C1 109.5(3) . . ? N2 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? N2 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C5 111.3(3) . . ? N2 C3 C4 112.6(3) . . ? C5 C3 C4 108.1(3) . . ? N2 C3 H3 108.2 . . ? C5 C3 H3 108.2 . . ? C4 C3 H3 108.2 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 C6 119.2(3) . . ? C3 C5 H5A 107.5 . . ? C6 C5 H5A 107.5 . . ? C3 C5 H5B 107.5 . . ? C6 C5 H5B 107.5 . . ? H5A C5 H5B 107.0 . . ? N3 C6 C8 111.6(3) . . ? N3 C6 C7 107.1(3) . . ? C8 C6 C7 107.7(3) . . ? N3 C6 C5 109.7(3) . . ? C8 C6 C5 109.1(3) . . ? C7 C6 C5 111.6(4) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C10 110.4(3) . . ? N3 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? N3 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? N4 C10 C9 110.0(3) . . ? N4 C10 H10A 109.7 . . ? C9 C10 H10A 109.7 . . ? N4 C10 H10B 109.7 . . ? C9 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? N4 C11 C13 111.3(3) . . ? N4 C11 C12 112.7(3) . . ? C13 C11 C12 108.9(3) . . ? N4 C11 H11 107.9 . . ? C13 C11 H11 107.9 . . ? C12 C11 H11 107.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 C14 119.2(3) . . ? C11 C13 H13A 107.5 . . ? C14 C13 H13A 107.5 . . ? C11 C13 H13B 107.5 . . ? C14 C13 H13B 107.5 . . ? H13A C13 H13B 107.0 . . ? N1 C14 C15 107.2(4) . . ? N1 C14 C16 112.0(3) . . ? C15 C14 C16 107.7(3) . . ? N1 C14 C13 110.9(3) . . ? C15 C14 C13 111.9(3) . . ? C16 C14 C13 107.2(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 C18 110.3(3) . . ? N5 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? N5 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? N6 C18 C17 109.4(3) . . ? N6 C18 H18A 109.8 . . ? C17 C18 H18A 109.8 . . ? N6 C18 H18B 109.8 . . ? C17 C18 H18B 109.8 . . ? H18A C18 H18B 108.2 . . ? N6 C19 C20 112.0(3) . . ? N6 C19 C21 111.3(3) . . ? C20 C19 C21 108.5(3) . . ? N6 C19 H19 108.3 . . ? C20 C19 H19 108.3 . . ? C21 C19 H19 108.3 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C19 119.2(3) . . ? C22 C21 H21A 107.5 . . ? C19 C21 H21A 107.5 . . ? C22 C21 H21B 107.5 . . ? C19 C21 H21B 107.5 . . ? H21A C21 H21B 107.0 . . ? N7 C22 C23 107.5(3) . . ? N7 C22 C21 110.0(3) . . ? C23 C22 C21 111.7(3) . . ? N7 C22 C24 111.9(3) . . ? C23 C22 C24 107.4(3) . . ? C21 C22 C24 108.3(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N7 C25 C26 110.8(3) . . ? N7 C25 H25A 109.5 . . ? C26 C25 H25A 109.5 . . ? N7 C25 H25B 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? N8 C26 C25 108.9(3) . . ? N8 C26 H26A 109.9 . . ? C25 C26 H26A 109.9 . . ? N8 C26 H26B 109.9 . . ? C25 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? N8 C27 C29 111.1(3) . . ? N8 C27 C28 111.6(4) . . ? C29 C27 C28 108.1(4) . . ? N8 C27 H27 108.7 . . ? C29 C27 H27 108.7 . . ? C28 C27 H27 108.7 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C27 118.3(3) . . ? C30 C29 H29A 107.7 . . ? C27 C29 H29A 107.7 . . ? C30 C29 H29B 107.7 . . ? C27 C29 H29B 107.7 . . ? H29A C29 H29B 107.1 . . ? N5 C30 C29 111.2(3) . . ? N5 C30 C31 107.1(3) . . ? C29 C30 C31 112.4(4) . . ? N5 C30 C32 110.9(3) . . ? C29 C30 C32 108.5(3) . . ? C31 C30 C32 106.7(4) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N9 C33 N10 172.3(4) . . ? N11 C34 N10 172.9(4) . . ? N12 C35 N13 166.7(5) . . ? N14 C36 N13 167.5(6) . . ? N15 C37 N16 168.3(6) . . ? N17 C38 N16 170.1(7) . . ? O2 Cl1 O1 107.8(4) . . ? O2 Cl1 O3 107.8(4) . . ? O1 Cl1 O3 109.1(3) . . ? O2 Cl1 O4 110.1(3) . . ? O1 Cl1 O4 110.1(3) . . ? O3 Cl1 O4 111.9(2) . . ? C1 N1 C14 113.7(3) . . ? C1 N1 Ni1 103.6(2) . . ? C14 N1 Ni1 121.9(2) . . ? C1 N1 H1C 105.5 . . ? C14 N1 H1C 105.5 . . ? Ni1 N1 H1C 105.5 . . ? C2 N2 C3 112.7(3) . . ? C2 N2 Ni1 103.9(2) . . ? C3 N2 Ni1 117.1(2) . . ? C2 N2 H2C 107.6 . . ? C3 N2 H2C 107.6 . . ? Ni1 N2 H2C 107.6 . . ? C9 N3 C6 113.0(3) . . ? C9 N3 Ni1 104.4(2) . . ? C6 N3 Ni1 121.8(2) . . ? C9 N3 H3A 105.5 . . ? C6 N3 H3A 105.5 . . ? Ni1 N3 H3A 105.5 . . ? C10 N4 C11 112.8(3) . . ? C10 N4 Ni1 103.9(2) . . ? C11 N4 Ni1 115.2(2) . . ? C10 N4 H4D 108.2 . . ? C11 N4 H4D 108.2 . . ? Ni1 N4 H4D 108.2 . . ? C17 N5 C30 112.3(3) . . ? C17 N5 Ni2 105.5(2) . . ? C30 N5 Ni2 120.9(2) . . ? C17 N5 H5C 105.7 . . ? C30 N5 H5C 105.7 . . ? Ni2 N5 H5C 105.7 . . ? C19 N6 C18 111.7(3) . . ? C19 N6 Ni2 117.3(2) . . ? C18 N6 Ni2 104.2(2) . . ? C19 N6 H6A 107.8 . . ? C18 N6 H6A 107.8 . . ? Ni2 N6 H6A 107.8 . . ? C25 N7 C22 112.4(3) . . ? C25 N7 Ni2 104.8(2) . . ? C22 N7 Ni2 122.1(2) . . ? C25 N7 H7D 105.4 . . ? C22 N7 H7D 105.4 . . ? Ni2 N7 H7D 105.4 . . ? C26 N8 C27 111.6(3) . . ? C26 N8 Ni2 104.2(2) . . ? C27 N8 Ni2 117.2(3) . . ? C26 N8 H8D 107.8 . . ? C27 N8 H8D 107.8 . . ? Ni2 N8 H8D 107.8 . . ? C33 N9 Ni1 158.2(3) . . ? C34 N10 C33 122.2(4) . . ? C34 N11 Ni2 148.6(3) . . ? C35 N12 Ni1 141.1(3) . . ? C36 N13 C35 125.2(4) . . ? C37 N15 Ni2 163.1(4) . . ? C37 N16 C38 117.5(5) . . ? N9 Ni1 N2 170.01(13) . . ? N9 Ni1 N12 84.11(13) . . ? N2 Ni1 N12 90.02(13) . . ? N9 Ni1 N4 88.18(12) . . ? N2 Ni1 N4 98.72(12) . . ? N12 Ni1 N4 168.73(12) . . ? N9 Ni1 N3 85.90(12) . . ? N2 Ni1 N3 87.67(11) . . ? N12 Ni1 N3 103.77(13) . . ? N4 Ni1 N3 83.80(12) . . ? N9 Ni1 N1 102.99(12) . . ? N2 Ni1 N1 84.59(11) . . ? N12 Ni1 N1 85.95(13) . . ? N4 Ni1 N1 87.80(12) . . ? N3 Ni1 N1 167.59(12) . . ? N15 Ni2 N11 84.59(14) . . ? N15 Ni2 N6 88.64(13) . . ? N11 Ni2 N6 170.80(12) . . ? N15 Ni2 N8 171.96(13) . . ? N11 Ni2 N8 89.23(13) . . ? N6 Ni2 N8 98.04(12) . . ? N15 Ni2 N5 86.93(12) . . ? N11 Ni2 N5 101.82(13) . . ? N6 Ni2 N5 83.98(12) . . ? N8 Ni2 N5 89.32(12) . . ? N15 Ni2 N7 100.80(12) . . ? N11 Ni2 N7 85.97(12) . . ? N6 Ni2 N7 89.21(11) . . ? N8 Ni2 N7 83.85(12) . . ? N5 Ni2 N7 169.60(12) . . ? N18 C39 H39A 109.5 . . ? N18 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N18 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N18 C40 H40A 109.5 . . ? N18 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N18 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O5 C41 N18 125.0(4) . . ? O5 C41 H41A 117.5 . . ? N18 C41 H41A 117.5 . . ? C41 N18 C40 121.5(4) . . ? C41 N18 C39 120.9(4) . . ? C40 N18 C39 117.5(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 61.4(4) . . . . ? N2 C3 C5 C6 -69.7(5) . . . . ? C4 C3 C5 C6 166.2(4) . . . . ? C3 C5 C6 N3 61.2(5) . . . . ? C3 C5 C6 C8 -176.3(4) . . . . ? C3 C5 C6 C7 -57.4(5) . . . . ? N3 C9 C10 N4 60.9(4) . . . . ? N4 C11 C13 C14 -70.3(4) . . . . ? C12 C11 C13 C14 164.8(3) . . . . ? C11 C13 C14 N1 59.6(4) . . . . ? C11 C13 C14 C15 -59.9(5) . . . . ? C11 C13 C14 C16 -177.8(4) . . . . ? N5 C17 C18 N6 58.6(4) . . . . ? N6 C19 C21 C22 -71.3(4) . . . . ? C20 C19 C21 C22 165.0(4) . . . . ? C19 C21 C22 N7 63.2(4) . . . . ? C19 C21 C22 C23 -56.1(4) . . . . ? C19 C21 C22 C24 -174.3(3) . . . . ? N7 C25 C26 N8 59.7(5) . . . . ? N8 C27 C29 C30 -71.8(5) . . . . ? C28 C27 C29 C30 165.5(4) . . . . ? C27 C29 C30 N5 64.9(5) . . . . ? C27 C29 C30 C31 -55.1(5) . . . . ? C27 C29 C30 C32 -172.9(4) . . . . ? C2 C1 N1 C14 -174.5(3) . . . . ? C2 C1 N1 Ni1 -40.1(4) . . . . ? C15 C14 N1 C1 -162.8(3) . . . . ? C16 C14 N1 C1 -44.9(4) . . . . ? C13 C14 N1 C1 74.8(4) . . . . ? C15 C14 N1 Ni1 72.0(4) . . . . ? C16 C14 N1 Ni1 -170.0(3) . . . . ? C13 C14 N1 Ni1 -50.3(4) . . . . ? C1 C2 N2 C3 -174.0(3) . . . . ? C1 C2 N2 Ni1 -46.2(4) . . . . ? C5 C3 N2 C2 -175.3(3) . . . . ? C4 C3 N2 C2 -53.7(4) . . . . ? C5 C3 N2 Ni1 64.2(4) . . . . ? C4 C3 N2 Ni1 -174.2(3) . . . . ? C10 C9 N3 C6 -174.6(3) . . . . ? C10 C9 N3 Ni1 -40.2(4) . . . . ? C8 C6 N3 C9 -47.2(4) . . . . ? C7 C6 N3 C9 -164.8(3) . . . . ? C5 C6 N3 C9 73.9(4) . . . . ? C8 C6 N3 Ni1 -172.8(3) . . . . ? C7 C6 N3 Ni1 69.7(4) . . . . ? C5 C6 N3 Ni1 -51.7(4) . . . . ? C9 C10 N4 C11 -170.8(3) . . . . ? C9 C10 N4 Ni1 -45.3(3) . . . . ? C13 C11 N4 C10 -174.9(3) . . . . ? C12 C11 N4 C10 -52.3(4) . . . . ? C13 C11 N4 Ni1 66.0(4) . . . . ? C12 C11 N4 Ni1 -171.4(3) . . . . ? C18 C17 N5 C30 -169.1(3) . . . . ? C18 C17 N5 Ni2 -35.5(3) . . . . ? C29 C30 N5 C17 74.8(4) . . . . ? C31 C30 N5 C17 -162.1(4) . . . . ? C32 C30 N5 C17 -46.0(4) . . . . ? C29 C30 N5 Ni2 -50.8(4) . . . . ? C31 C30 N5 Ni2 72.3(4) . . . . ? C32 C30 N5 Ni2 -171.6(3) . . . . ? C20 C19 N6 C18 -56.9(5) . . . . ? C21 C19 N6 C18 -178.6(3) . . . . ? C20 C19 N6 Ni2 -177.1(3) . . . . ? C21 C19 N6 Ni2 61.2(4) . . . . ? C17 C18 N6 C19 -175.5(3) . . . . ? C17 C18 N6 Ni2 -47.9(3) . . . . ? C26 C25 N7 C22 -170.9(3) . . . . ? C26 C25 N7 Ni2 -36.2(4) . . . . ? C23 C22 N7 C25 -162.3(3) . . . . ? C21 C22 N7 C25 75.8(4) . . . . ? C24 C22 N7 C25 -44.6(4) . . . . ? C23 C22 N7 Ni2 71.9(3) . . . . ? C21 C22 N7 Ni2 -50.0(4) . . . . ? C24 C22 N7 Ni2 -170.4(3) . . . . ? C25 C26 N8 C27 -176.0(4) . . . . ? C25 C26 N8 Ni2 -48.5(4) . . . . ? C29 C27 N8 C26 -178.7(4) . . . . ? C28 C27 N8 C26 -58.0(5) . . . . ? C29 C27 N8 Ni2 61.3(4) . . . . ? C28 C27 N8 Ni2 -178.0(3) . . . . ? N13 C35 N12 Ni1 56(2) . . . . ? N14 C36 N13 C35 156(3) . . . . ? N12 C35 N13 C36 -147(2) . . . . ? N16 C37 N15 Ni2 -165.2(18) . . . . ? N15 C37 N16 C38 170(2) . . . . ? N17 C38 N16 C37 -168(3) . . . . ? C33 N9 Ni1 N12 -10.9(9) . . . . ? C33 N9 Ni1 N4 177.3(9) . . . . ? C33 N9 Ni1 N3 93.4(9) . . . . ? C33 N9 Ni1 N1 -95.3(9) . . . . ? C2 N2 Ni1 N12 -67.5(3) . . . . ? C3 N2 Ni1 N12 57.5(3) . . . . ? C2 N2 Ni1 N4 105.3(3) . . . . ? C3 N2 Ni1 N4 -129.6(3) . . . . ? C2 N2 Ni1 N3 -171.3(3) . . . . ? C3 N2 Ni1 N3 -46.3(3) . . . . ? C2 N2 Ni1 N1 18.4(2) . . . . ? C3 N2 Ni1 N1 143.4(3) . . . . ? C35 N12 Ni1 N9 -8.6(5) . . . . ? C35 N12 Ni1 N2 179.4(5) . . . . ? C35 N12 Ni1 N4 38.4(10) . . . . ? C35 N12 Ni1 N3 -92.9(5) . . . . ? C35 N12 Ni1 N1 94.9(5) . . . . ? C10 N4 Ni1 N9 -68.3(2) . . . . ? C11 N4 Ni1 N9 55.6(2) . . . . ? C10 N4 Ni1 N2 104.4(2) . . . . ? C11 N4 Ni1 N2 -131.7(2) . . . . ? C10 N4 Ni1 N12 -115.1(6) . . . . ? C11 N4 Ni1 N12 8.8(8) . . . . ? C10 N4 Ni1 N3 17.8(2) . . . . ? C11 N4 Ni1 N3 141.7(3) . . . . ? C10 N4 Ni1 N1 -171.4(2) . . . . ? C11 N4 Ni1 N1 -47.5(2) . . . . ? C9 N3 Ni1 N9 100.3(2) . . . . ? C6 N3 Ni1 N9 -130.3(3) . . . . ? C9 N3 Ni1 N2 -87.3(2) . . . . ? C6 N3 Ni1 N2 42.0(3) . . . . ? C9 N3 Ni1 N12 -176.8(2) . . . . ? C6 N3 Ni1 N12 -47.4(3) . . . . ? C9 N3 Ni1 N4 11.7(2) . . . . ? C6 N3 Ni1 N4 141.1(3) . . . . ? C9 N3 Ni1 N1 -35.9(7) . . . . ? C6 N3 Ni1 N1 93.4(6) . . . . ? C1 N1 Ni1 N9 -175.3(2) . . . . ? C14 N1 Ni1 N9 -45.7(3) . . . . ? C1 N1 Ni1 N2 11.3(3) . . . . ? C14 N1 Ni1 N2 140.9(3) . . . . ? C1 N1 Ni1 N12 101.7(3) . . . . ? C14 N1 Ni1 N12 -128.7(3) . . . . ? C1 N1 Ni1 N4 -87.7(2) . . . . ? C14 N1 Ni1 N4 41.9(3) . . . . ? C1 N1 Ni1 N3 -40.4(7) . . . . ? C14 N1 Ni1 N3 89.2(6) . . . . ? C37 N15 Ni2 N11 -16.1(12) . . . . ? C37 N15 Ni2 N6 170.2(12) . . . . ? C37 N15 Ni2 N8 23.9(18) . . . . ? C37 N15 Ni2 N5 86.1(12) . . . . ? C37 N15 Ni2 N7 -100.9(12) . . . . ? C34 N11 Ni2 N15 -7.3(6) . . . . ? C34 N11 Ni2 N6 35.5(12) . . . . ? C34 N11 Ni2 N8 177.9(6) . . . . ? C34 N11 Ni2 N5 -93.0(6) . . . . ? C34 N11 Ni2 N7 94.0(6) . . . . ? C19 N6 Ni2 N15 58.7(3) . . . . ? C18 N6 Ni2 N15 -65.3(2) . . . . ? C19 N6 Ni2 N11 16.2(9) . . . . ? C19 N6 Ni2 N8 -125.8(2) . . . . ? C18 N6 Ni2 N8 110.2(2) . . . . ? C19 N6 Ni2 N5 145.8(3) . . . . ? C18 N6 Ni2 N5 21.8(2) . . . . ? C19 N6 Ni2 N7 -42.1(3) . . . . ? C18 N6 Ni2 N7 -166.1(2) . . . . ? C26 N8 Ni2 N11 -63.9(3) . . . . ? C27 N8 Ni2 N11 60.0(3) . . . . ? C26 N8 Ni2 N6 110.5(3) . . . . ? C27 N8 Ni2 N6 -125.6(3) . . . . ? C26 N8 Ni2 N5 -165.7(3) . . . . ? C27 N8 Ni2 N5 -41.8(3) . . . . ? C26 N8 Ni2 N7 22.1(3) . . . . ? C27 N8 Ni2 N7 146.0(3) . . . . ? C17 N5 Ni2 N15 96.1(2) . . . . ? C30 N5 Ni2 N15 -135.2(3) . . . . ? C17 N5 Ni2 N11 180.0(2) . . . . ? C30 N5 Ni2 N11 -51.4(3) . . . . ? C17 N5 Ni2 N6 7.2(2) . . . . ? C30 N5 Ni2 N6 135.9(3) . . . . ? C17 N5 Ni2 N8 -91.0(2) . . . . ? C30 N5 Ni2 N8 37.7(3) . . . . ? C17 N5 Ni2 N7 -42.2(7) . . . . ? C30 N5 Ni2 N7 86.5(7) . . . . ? C25 N7 Ni2 N15 -179.5(3) . . . . ? C22 N7 Ni2 N15 -50.4(3) . . . . ? C25 N7 Ni2 N11 96.8(3) . . . . ? C22 N7 Ni2 N11 -134.1(3) . . . . ? C25 N7 Ni2 N6 -91.0(3) . . . . ? C22 N7 Ni2 N6 38.1(3) . . . . ? C25 N7 Ni2 N8 7.1(2) . . . . ? C22 N7 Ni2 N8 136.2(3) . . . . ? C25 N7 Ni2 N5 -42.0(8) . . . . ? C22 N7 Ni2 N5 87.1(7) . . . . ? O5 C41 N18 C40 1.3(7) . . . . ? O5 C41 N18 C39 -179.2(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 N1 H1C N17 0.93 2.30 3.158(6) 154.0 1_455 N2 H2C O3 0.93 2.19 3.097(5) 164.1 . N4 H4D O1 0.93 2.30 3.187(5) 159.2 . N5 H5C N14 0.93 2.27 3.173(5) 162.6 1_655 N6 H6A O5 0.93 2.08 2.967(4) 159.6 . N8 H8D O5 0.93 2.03 2.943(5) 165.8 . _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 61.12 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.698 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.049 # Attachment '3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 722171' # start Validation Reply Form _vrf_PLAT432_3 ; PROBLEM: Short Inter X...Y Contact N11 .. C30 .. 2.46 Ang. RESPONSE: The acetonitrile molecule is disordered. ; _vrf_CELLZ01_3 ; PROBLEM: H atoms missing from atom site list. Is this intentional. RESPONSE: The hydrogen atoms of disordered acetonitrile molecule were not added. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H111 Cl2 N25 Ni3 O8' _chemical_formula_weight 1533.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.084(3) _cell_length_b 15.471(2) _cell_length_c 21.887(3) _cell_angle_alpha 90.00 _cell_angle_beta 120.605(5) _cell_angle_gamma 90.00 _cell_volume 7601.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2240 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 21.24 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 0.871 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7111 _exptl_absorpt_correction_T_max 0.7503 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17340 _diffrn_reflns_av_R_equivalents 0.1235 _diffrn_reflns_av_sigmaI/netI 0.1780 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6491 _reflns_number_gt 2899 _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^)+(0.1346P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6491 _refine_ls_number_parameters 524 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1910 _refine_ls_R_factor_gt 0.0799 _refine_ls_wR_factor_ref 0.2598 _refine_ls_wR_factor_gt 0.1914 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.969 _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 N10 N 0.9168(4) 0.5953(6) 0.2550(5) 0.0719(18) Uani 0.70 1 d PDU A 1 C27 C 0.9621(6) 0.6166(11) 0.2597(8) 0.074(2) Uani 0.70 1 d PDU . 1 N10' N 0.9168(4) 0.5953(6) 0.2550(5) 0.0719(18) Uani 0.30 1 d PDU A 2 C27' C 0.9415(16) 0.598(3) 0.2249(19) 0.074(2) Uani 0.30 1 d PDU A 2 N11 N 0.9872(6) 0.6469(14) 0.2264(11) 0.074(3) Uani 0.35 1 d PDU . 1 N11' N 0.9683(19) 0.618(3) 0.1920(18) 0.074(2) Uani 0.15 1 d PDU . . N12 N 0.9696(9) 0.4849(13) 0.0519(8) 0.094(5) Uani 0.50 1 d PDU . . C28 C 0.9553(13) 0.4555(18) 0.0881(13) 0.104(4) Uani 0.50 1 d PDU . . N13 N 0.9434(9) 0.4256(14) 0.1343(9) 0.105(4) Uani 0.50 1 d PDU . . C29 C 0.9732(13) 0.3818(19) 0.1924(8) 0.109(4) Uani 0.50 1 d PDU . . N14 N 1.0000 0.3585(12) 0.2500 0.119(4) Uani 1 2 d SDU . . N15 N 0.9536(14) 0.6746(19) 0.0744(16) 0.088(9) Uani 0.35 1 d PDU B 1 C30 C 0.9703(15) 0.7238(19) 0.1193(17) 0.061(9) Uani 0.35 1 d PDU B 1 C31 C 0.9924(16) 0.7907(19) 0.1738(17) 0.072(10) Uani 0.35 1 d PDU B 1 C31' C 0.942(7) 0.679(7) 0.034(6) 0.16(6) Uani 0.15 1 d PDU C 2 C30' C 0.968(3) 0.742(4) 0.091(4) 0.05(2) Uani 0.15 1 d PDU C 2 N15' N 0.989(3) 0.785(4) 0.140(3) 0.07(2) Uani 0.15 1 d PDU C 2 C1 C 0.7489(5) 0.6867(7) 0.2553(5) 0.057(3) Uani 1 1 d . . . H1A H 0.7329 0.6329 0.2638 0.069 Uiso 1 1 calc R . . H1B H 0.7398 0.7349 0.2781 0.069 Uiso 1 1 calc R . . C2 C 0.7194(4) 0.7024(6) 0.1795(5) 0.052(3) Uani 1 1 d . . . H2A H 0.7330 0.7583 0.1708 0.062 Uiso 1 1 calc R . . H2B H 0.6758 0.7062 0.1598 0.062 Uiso 1 1 calc R . . C3 C 0.7095(5) 0.6506(6) 0.0665(5) 0.061(3) Uani 1 1 d . . . H3 H 0.7347 0.6978 0.0644 0.073 Uiso 1 1 calc R . . C4 C 0.6447(5) 0.6817(9) 0.0246(6) 0.086(4) Uani 1 1 d . . . H4A H 0.6189 0.6393 0.0292 0.128 Uiso 1 1 calc R . . H4B H 0.6324 0.6881 -0.0256 0.128 Uiso 1 1 calc R . . H4C H 0.6413 0.7375 0.0433 0.128 Uiso 1 1 calc R . . C5 C 0.7176(5) 0.5736(7) 0.0316(5) 0.063(3) Uani 1 1 d . . . H5A H 0.6929 0.5828 -0.0203 0.075 Uiso 1 1 calc R . . H5B H 0.7004 0.5235 0.0431 0.075 Uiso 1 1 calc R . . C6 C 0.7796(5) 0.5471(6) 0.0476(5) 0.058(3) Uani 1 1 d . . . C7 C 0.7731(6) 0.4742(7) -0.0007(6) 0.083(4) Uani 1 1 d . . . H7A H 0.8127 0.4549 0.0102 0.124 Uiso 1 1 calc R . . H7B H 0.7504 0.4939 -0.0501 0.124 Uiso 1 1 calc R . . H7C H 0.7521 0.4262 0.0062 0.124 Uiso 1 1 calc R . . C8 C 0.8120(6) 0.6217(8) 0.0335(6) 0.082(4) Uani 1 1 d . . . H8A H 0.8267 0.6637 0.0724 0.123 Uiso 1 1 calc R . . H8B H 0.7841 0.6503 -0.0113 0.123 Uiso 1 1 calc R . . H8C H 0.8456 0.5983 0.0306 0.123 Uiso 1 1 calc R . . C9 C 0.8029(5) 0.4420(7) 0.1422(6) 0.064(3) Uani 1 1 d . . . H9A H 0.8114 0.3957 0.1174 0.077 Uiso 1 1 calc R . . H9B H 0.7597 0.4402 0.1254 0.077 Uiso 1 1 calc R . . C10 C 0.8373(5) 0.4250(6) 0.2203(6) 0.058(3) Uani 1 1 d . . . H10A H 0.8806 0.4260 0.2376 0.070 Uiso 1 1 calc R . . H10B H 0.8271 0.3672 0.2304 0.070 Uiso 1 1 calc R . . C11 C 0.8622(5) 0.4906(6) 0.3350(6) 0.064(3) Uani 1 1 d . . . H11 H 0.9030 0.5093 0.3469 0.077 Uiso 1 1 calc R . . C12 C 0.8665(7) 0.4015(7) 0.3676(7) 0.094(4) Uani 1 1 d . . . H12A H 0.8283 0.3870 0.3634 0.141 Uiso 1 1 calc R . . H12B H 0.8977 0.4024 0.4178 0.141 Uiso 1 1 calc R . . H12C H 0.8763 0.3582 0.3425 0.141 Uiso 1 1 calc R . . C13 C 0.8385(6) 0.5545(7) 0.3693(5) 0.070(3) Uani 1 1 d . . . H13A H 0.7956 0.5425 0.3489 0.084 Uiso 1 1 calc R . . H13B H 0.8585 0.5407 0.4206 0.084 Uiso 1 1 calc R . . C14 C 0.8453(5) 0.6501(7) 0.3625(5) 0.063(3) Uani 1 1 d . . . C15 C 0.8225(6) 0.7008(8) 0.4057(6) 0.087(4) Uani 1 1 d . . . H15A H 0.8266 0.7630 0.4008 0.131 Uiso 1 1 calc R . . H15B H 0.8461 0.6845 0.4558 0.131 Uiso 1 1 calc R . . H15C H 0.7805 0.6868 0.3875 0.131 Uiso 1 1 calc R . . C16 C 0.9137(6) 0.6725(7) 0.3940(6) 0.080(4) Uani 1 1 d . . . H16A H 0.9289 0.6400 0.3681 0.120 Uiso 1 1 calc R . . H16B H 0.9363 0.6567 0.4444 0.120 Uiso 1 1 calc R . . H16C H 0.9181 0.7346 0.3889 0.120 Uiso 1 1 calc R . . C17 C 0.9334(4) 1.1720(6) 0.3031(4) 0.039(2) Uani 1 1 d . . . H17A H 0.9573 1.2258 0.3170 0.047 Uiso 1 1 calc R . . H17B H 0.9090 1.1719 0.3260 0.047 Uiso 1 1 calc R . . C18 C 0.8934(4) 1.1694(5) 0.2238(4) 0.040(2) Uani 1 1 d . . . H18A H 0.8685 1.1166 0.2098 0.048 Uiso 1 1 calc R . . H18B H 0.8666 1.2203 0.2077 0.048 Uiso 1 1 calc R . . C19 C 0.8944(4) 1.1537(6) 0.1125(4) 0.039(2) Uani 1 1 d . . . H19 H 0.8795 1.0928 0.1047 0.047 Uiso 1 1 calc R . . C20 C 0.8409(4) 1.2146(6) 0.0745(5) 0.051(3) Uani 1 1 d . . . H20A H 0.8174 1.2124 0.0979 0.077 Uiso 1 1 calc R . . H20B H 0.8161 1.1965 0.0249 0.077 Uiso 1 1 calc R . . H20C H 0.8551 1.2737 0.0762 0.077 Uiso 1 1 calc R . . C21 C 1.0181(4) 1.1003(5) 0.4054(4) 0.036(2) Uani 1 1 d . . . C22 C 1.0678(4) 1.1655(6) 0.4213(4) 0.044(2) Uani 1 1 d . . . H22A H 1.0492 1.2234 0.4076 0.053 Uiso 1 1 calc R . . H22B H 1.0950 1.1664 0.4734 0.053 Uiso 1 1 calc R . . C23 C 1.0442(4) 1.0090(6) 0.4275(5) 0.048(2) Uani 1 1 d . . . H23A H 1.0123 0.9682 0.4183 0.072 Uiso 1 1 calc R . . H23B H 1.0742 1.0085 0.4782 0.072 Uiso 1 1 calc R . . H23C H 1.0628 0.9919 0.4001 0.072 Uiso 1 1 calc R . . C24 C 0.9900(4) 1.1256(6) 0.4500(5) 0.051(3) Uani 1 1 d . . . H24A H 0.9761 1.1855 0.4396 0.077 Uiso 1 1 calc R . . H24B H 1.0199 1.1199 0.5006 0.077 Uiso 1 1 calc R . . H24C H 0.9563 1.0873 0.4383 0.077 Uiso 1 1 calc R . . C25 C 0.8487(4) 0.8040(6) 0.1712(5) 0.048(2) Uani 1 1 d . . . C26 C 0.8979(4) 0.9314(6) 0.1865(4) 0.038(2) Uani 1 1 d . . . N1 N 0.8152(4) 0.6786(5) 0.2888(4) 0.052(2) Uani 1 1 d . A . H1C H 0.8290 0.7343 0.2898 0.062 Uiso 1 1 calc R . . N2 N 0.7321(3) 0.6331(4) 0.1434(4) 0.0450(19) Uani 1 1 d . A . H2C H 0.7126 0.5838 0.1456 0.054 Uiso 1 1 calc R . . N3 N 0.8175(4) 0.5256(5) 0.1241(4) 0.054(2) Uani 1 1 d . A . H3A H 0.8560 0.5200 0.1322 0.064 Uiso 1 1 calc R . . N4 N 0.8227(4) 0.4927(5) 0.2576(4) 0.054(2) Uani 1 1 d . A . H4D H 0.7838 0.4836 0.2474 0.065 Uiso 1 1 calc R . . N5 N 0.9737(3) 1.0963(4) 0.3279(3) 0.0311(16) Uani 1 1 d . . . H5C H 0.9496 1.0491 0.3221 0.037 Uiso 1 1 calc R . . N6 N 0.9305(3) 1.1699(4) 0.1902(3) 0.0316(16) Uani 1 1 d . . . H6A H 0.9476 1.2244 0.1969 0.038 Uiso 1 1 calc R . . N7 N 0.8379(4) 0.7334(5) 0.1771(4) 0.053(2) Uani 1 1 d . A . N8 N 0.8517(4) 0.8826(5) 0.1559(4) 0.062(2) Uani 1 1 d . . . N9 N 0.9349(3) 0.9818(4) 0.2074(3) 0.0317(16) Uani 1 1 d . . . Ni1 Ni 0.82490(5) 0.61014(7) 0.20869(6) 0.0412(4) Uani 1 1 d . . . Ni2 Ni 1.0000 1.07966(8) 0.2500 0.0253(4) Uani 1 2 d S . . Cl1 Cl 0.84598(10) 0.93696(14) 0.32388(12) 0.0441(6) Uani 1 1 d . . . O1 O 0.8976(3) 0.8953(5) 0.3335(4) 0.075(2) Uani 1 1 d . . . O2 O 0.8415(4) 1.0192(4) 0.2942(5) 0.095(3) Uani 1 1 d . . . O3 O 0.8481(4) 0.9472(6) 0.3903(4) 0.089(3) Uani 1 1 d . . . O4 O 0.7953(4) 0.8886(6) 0.2779(4) 0.091(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N10 0.072(3) 0.072(3) 0.077(3) -0.004(2) 0.0419(19) -0.003(2) C27 0.071(3) 0.076(3) 0.078(3) -0.003(2) 0.040(2) -0.003(2) N10' 0.072(3) 0.072(3) 0.077(3) -0.004(2) 0.0419(19) -0.003(2) C27' 0.072(3) 0.075(3) 0.077(3) -0.003(3) 0.040(2) -0.002(3) N11 0.072(3) 0.075(4) 0.076(3) -0.001(3) 0.040(3) -0.002(3) N11' 0.072(3) 0.076(4) 0.076(3) -0.001(3) 0.040(2) -0.002(3) N12 0.096(6) 0.093(6) 0.092(6) -0.008(4) 0.046(4) 0.003(4) C28 0.104(5) 0.104(5) 0.106(5) -0.006(3) 0.055(3) 0.000(4) N13 0.107(5) 0.106(5) 0.107(5) -0.006(3) 0.057(3) -0.003(3) C29 0.110(5) 0.109(5) 0.109(5) -0.005(3) 0.057(3) 0.001(3) N14 0.121(5) 0.116(5) 0.116(5) 0.000 0.057(4) 0.000 N15 0.081(12) 0.102(13) 0.089(12) -0.006(9) 0.051(10) 0.008(9) C30 0.053(12) 0.056(13) 0.070(12) 0.001(9) 0.026(9) -0.010(9) C31 0.075(14) 0.064(13) 0.069(13) 0.008(9) 0.031(10) 0.005(9) C31' 0.16(6) 0.16(6) 0.16(6) 0.000(10) 0.08(3) 0.000(10) C30' 0.05(2) 0.05(2) 0.05(2) 0.002(10) 0.027(13) -0.005(10) N15' 0.07(2) 0.07(2) 0.07(2) -0.002(10) 0.039(14) 0.004(10) C1 0.075(8) 0.050(6) 0.086(8) -0.027(5) 0.070(7) -0.023(5) C2 0.058(7) 0.033(6) 0.084(8) 0.003(5) 0.051(6) 0.004(4) C3 0.082(9) 0.047(6) 0.065(7) -0.001(5) 0.047(7) -0.020(6) C4 0.054(8) 0.085(9) 0.097(9) 0.020(7) 0.023(7) -0.011(7) C5 0.086(8) 0.060(7) 0.070(7) -0.020(5) 0.060(7) -0.026(6) C6 0.088(8) 0.053(6) 0.062(7) -0.028(5) 0.059(7) -0.027(6) C7 0.127(11) 0.065(8) 0.100(9) -0.039(7) 0.090(9) -0.042(7) C8 0.115(11) 0.075(9) 0.097(9) -0.022(7) 0.084(9) -0.036(7) C9 0.077(8) 0.046(7) 0.097(9) -0.028(6) 0.064(8) -0.016(5) C10 0.082(8) 0.020(5) 0.099(9) -0.019(5) 0.066(7) -0.005(5) C11 0.077(8) 0.045(7) 0.071(8) 0.011(5) 0.040(7) -0.011(5) C12 0.141(13) 0.041(7) 0.108(10) 0.004(6) 0.069(10) -0.015(7) C13 0.119(10) 0.054(7) 0.057(7) -0.008(5) 0.059(7) -0.023(6) C14 0.107(9) 0.044(6) 0.059(7) -0.020(5) 0.056(7) -0.029(6) C15 0.161(13) 0.069(8) 0.071(7) -0.021(6) 0.088(9) -0.034(8) C16 0.124(11) 0.040(7) 0.081(8) -0.006(6) 0.056(8) -0.025(7) C17 0.047(6) 0.042(5) 0.043(5) 0.000(4) 0.034(5) -0.003(4) C18 0.043(6) 0.034(5) 0.062(6) 0.010(4) 0.041(5) 0.013(4) C19 0.039(5) 0.042(5) 0.041(5) 0.009(4) 0.025(5) 0.011(4) C20 0.047(6) 0.056(7) 0.057(6) 0.018(5) 0.031(5) 0.018(5) C21 0.036(5) 0.038(5) 0.040(5) 0.001(4) 0.024(5) -0.007(4) C22 0.048(6) 0.058(6) 0.043(5) -0.009(4) 0.035(5) -0.008(5) C23 0.053(6) 0.054(6) 0.046(6) 0.002(5) 0.031(5) -0.006(5) C24 0.068(7) 0.065(7) 0.048(6) -0.005(5) 0.049(6) -0.004(5) C25 0.068(7) 0.029(6) 0.062(6) -0.006(5) 0.045(6) -0.017(5) C26 0.044(6) 0.033(5) 0.037(5) -0.002(4) 0.021(5) -0.014(5) N1 0.076(6) 0.037(5) 0.058(5) -0.006(4) 0.045(5) -0.004(4) N2 0.065(5) 0.025(4) 0.057(5) -0.013(3) 0.040(5) -0.015(4) N3 0.060(5) 0.040(5) 0.091(7) -0.005(4) 0.060(5) -0.006(4) N4 0.055(5) 0.033(5) 0.086(7) -0.011(4) 0.044(5) -0.013(4) N5 0.034(4) 0.028(4) 0.041(4) -0.002(3) 0.026(4) -0.005(3) N6 0.042(4) 0.028(4) 0.044(4) 0.006(3) 0.035(4) 0.003(3) N7 0.068(6) 0.046(5) 0.064(5) -0.005(4) 0.047(5) -0.008(4) N8 0.065(6) 0.043(5) 0.048(5) -0.002(4) 0.006(5) -0.027(4) N9 0.034(4) 0.024(4) 0.041(4) -0.003(3) 0.022(4) 0.000(3) Ni1 0.0540(8) 0.0251(6) 0.0677(8) -0.0111(5) 0.0479(7) -0.0092(5) Ni2 0.0322(9) 0.0190(8) 0.0350(9) 0.000 0.0247(8) 0.000 Cl1 0.0481(15) 0.0328(13) 0.0699(16) -0.0058(11) 0.0435(14) -0.0005(10) O1 0.056(5) 0.086(6) 0.103(6) 0.017(4) 0.055(5) 0.035(4) O2 0.128(7) 0.027(4) 0.154(7) 0.026(4) 0.089(6) 0.017(4) O3 0.110(7) 0.111(7) 0.076(5) -0.025(5) 0.071(5) -0.002(5) O4 0.070(6) 0.102(7) 0.104(6) -0.050(5) 0.047(5) -0.038(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N12 C28 1.129(9) . ? C28 N13 1.283(9) . ? N13 C29 1.295(9) . ? C29 N14 1.144(9) . ? N14 C29 1.144(9) 2_755 ? N15 C30 1.140(8) . ? C30 C31 1.458(8) . ? C1 C2 1.449(13) . ? C1 N1 1.501(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.467(11) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C5 1.486(14) . ? C3 N2 1.497(11) . ? C3 C4 1.534(15) . ? C3 H3 1.0000 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.527(14) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N3 1.486(12) . ? C6 C7 1.495(13) . ? C6 C8 1.552(14) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N3 1.461(12) . ? C9 C10 1.495(14) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N4 1.493(11) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N4 1.467(12) . ? C11 C12 1.530(14) . ? C11 C13 1.548(15) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.505(14) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N1 1.459(12) . ? C14 C15 1.558(14) . ? C14 C16 1.591(16) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 N5 1.479(10) . ? C17 C18 1.504(11) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N6 1.486(9) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 N6 1.485(10) . ? C19 C22 1.518(11) 2_755 ? C19 C20 1.531(11) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 N5 1.491(10) . ? C21 C23 1.536(12) . ? C21 C22 1.535(11) . ? C21 C24 1.540(11) . ? C22 C19 1.518(11) 2_755 ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N7 1.152(11) . ? C25 N8 1.274(12) . ? C26 N9 1.139(10) . ? C26 N8 1.285(11) . ? N1 Ni1 2.170(7) . ? N1 H1C 0.9300 . ? N2 Ni1 2.123(8) . ? N2 H2C 0.9300 . ? N3 Ni1 2.193(8) . ? N3 H3A 0.9300 . ? N4 Ni1 2.125(8) . ? N4 H4D 0.9300 . ? N5 Ni2 2.152(6) . ? N5 H5C 0.9300 . ? N6 Ni2 2.128(6) . ? N6 H6A 0.9300 . ? N7 Ni1 2.114(8) . ? N9 Ni2 2.106(7) . ? Ni2 N9 2.106(7) 2_755 ? Ni2 N6 2.128(6) 2_755 ? Ni2 N5 2.152(6) 2_755 ? Cl1 O4 1.401(7) . ? Cl1 O2 1.406(7) . ? Cl1 O1 1.408(6) . ? Cl1 O3 1.435(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 C27 N10 Ni1 149.8(10) . . ? N12 C28 N13 174(3) . . ? C28 N13 C29 134(3) . . ? N14 C29 N13 166(3) . . ? C29 N14 C29 143(4) . 2_755 ? N15 C30 C31 176(4) . . ? N15' C30' C31' 173(8) . . ? C2 C1 N1 112.4(7) . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1B 109.1 . . ? N1 C1 H1B 109.1 . . ? H1A C1 H1B 107.9 . . ? C1 C2 N2 111.1(8) . . ? C1 C2 H2A 109.4 . . ? N2 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? N2 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C5 C3 N2 110.8(8) . . ? C5 C3 C4 110.1(9) . . ? N2 C3 C4 114.3(9) . . ? C5 C3 H3 107.1 . . ? N2 C3 H3 107.1 . . ? C4 C3 H3 107.1 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 C6 120.5(9) . . ? C3 C5 H5A 107.2 . . ? C6 C5 H5A 107.2 . . ? C3 C5 H5B 107.2 . . ? C6 C5 H5B 107.2 . . ? H5A C5 H5B 106.8 . . ? N3 C6 C7 113.5(10) . . ? N3 C6 C5 109.8(7) . . ? C7 C6 C5 108.4(9) . . ? N3 C6 C8 105.8(9) . . ? C7 C6 C8 107.3(8) . . ? C5 C6 C8 112.0(10) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C10 112.2(8) . . ? N3 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? N3 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 N4 109.3(8) . . ? C9 C10 H10A 109.8 . . ? N4 C10 H10A 109.8 . . ? C9 C10 H10B 109.8 . . ? N4 C10 H10B 109.8 . . ? H10A C10 H10B 108.3 . . ? N4 C11 C12 113.6(9) . . ? N4 C11 C13 109.1(9) . . ? C12 C11 C13 107.5(9) . . ? N4 C11 H11 108.9 . . ? C12 C11 H11 108.9 . . ? C13 C11 H11 108.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C11 118.9(8) . . ? C14 C13 H13A 107.6 . . ? C11 C13 H13A 107.6 . . ? C14 C13 H13B 107.6 . . ? C11 C13 H13B 107.6 . . ? H13A C13 H13B 107.0 . . ? N1 C14 C13 112.4(8) . . ? N1 C14 C15 111.2(10) . . ? C13 C14 C15 109.6(8) . . ? N1 C14 C16 105.4(8) . . ? C13 C14 C16 109.5(10) . . ? C15 C14 C16 108.5(8) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 C18 110.4(6) . . ? N5 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? N5 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? N6 C18 C17 109.1(6) . . ? N6 C18 H18A 109.9 . . ? C17 C18 H18A 109.9 . . ? N6 C18 H18B 109.9 . . ? C17 C18 H18B 109.9 . . ? H18A C18 H18B 108.3 . . ? N6 C19 C22 110.3(7) . 2_755 ? N6 C19 C20 113.0(7) . . ? C22 C19 C20 107.4(7) 2_755 . ? N6 C19 H19 108.7 . . ? C22 C19 H19 108.7 2_755 . ? C20 C19 H19 108.7 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N5 C21 C23 106.5(6) . . ? N5 C21 C22 111.3(6) . . ? C23 C21 C22 110.2(7) . . ? N5 C21 C24 112.8(7) . . ? C23 C21 C24 108.1(7) . . ? C22 C21 C24 107.9(7) . . ? C19 C22 C21 119.6(7) 2_755 . ? C19 C22 H22A 107.4 2_755 . ? C21 C22 H22A 107.4 . . ? C19 C22 H22B 107.4 2_755 . ? C21 C22 H22B 107.4 . . ? H22A C22 H22B 107.0 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N7 C25 N8 170.4(11) . . ? N9 C26 N8 171.8(10) . . ? C14 N1 C1 113.8(8) . . ? C14 N1 Ni1 121.9(6) . . ? C1 N1 Ni1 103.1(5) . . ? C14 N1 H1C 105.6 . . ? C1 N1 H1C 105.6 . . ? Ni1 N1 H1C 105.6 . . ? C2 N2 C3 113.9(7) . . ? C2 N2 Ni1 104.6(5) . . ? C3 N2 Ni1 116.6(6) . . ? C2 N2 H2C 107.1 . . ? C3 N2 H2C 107.1 . . ? Ni1 N2 H2C 107.1 . . ? C9 N3 C6 112.8(8) . . ? C9 N3 Ni1 102.8(5) . . ? C6 N3 Ni1 122.7(6) . . ? C9 N3 H3A 105.7 . . ? C6 N3 H3A 105.7 . . ? Ni1 N3 H3A 105.7 . . ? C11 N4 C10 113.0(8) . . ? C11 N4 Ni1 114.6(5) . . ? C10 N4 Ni1 104.1(6) . . ? C11 N4 H4D 108.3 . . ? C10 N4 H4D 108.3 . . ? Ni1 N4 H4D 108.3 . . ? C17 N5 C21 112.3(6) . . ? C17 N5 Ni2 105.0(4) . . ? C21 N5 Ni2 122.0(5) . . ? C17 N5 H5C 105.4 . . ? C21 N5 H5C 105.4 . . ? Ni2 N5 H5C 105.4 . . ? C19 N6 C18 111.8(6) . . ? C19 N6 Ni2 116.0(5) . . ? C18 N6 Ni2 105.0(4) . . ? C19 N6 H6A 107.9 . . ? C18 N6 H6A 107.9 . . ? Ni2 N6 H6A 107.9 . . ? C25 N7 Ni1 169.0(7) . . ? C25 N8 C26 126.3(9) . . ? C26 N9 Ni2 175.5(7) . . ? N10 Ni1 N7 85.5(3) . . ? N10 Ni1 N2 168.5(3) . . ? N7 Ni1 N2 87.0(3) . . ? N10 Ni1 N4 88.9(3) . . ? N7 Ni1 N4 170.5(3) . . ? N2 Ni1 N4 99.6(3) . . ? N10 Ni1 N1 103.8(3) . . ? N7 Ni1 N1 85.9(3) . . ? N2 Ni1 N1 84.3(3) . . ? N4 Ni1 N1 88.0(3) . . ? N10 Ni1 N3 86.0(3) . . ? N7 Ni1 N3 102.8(3) . . ? N2 Ni1 N3 87.2(3) . . ? N4 Ni1 N3 84.4(3) . . ? N1 Ni1 N3 167.5(3) . . ? N9 Ni2 N9 88.0(3) . 2_755 ? N9 Ni2 N6 170.4(2) . 2_755 ? N9 Ni2 N6 87.5(2) 2_755 2_755 ? N9 Ni2 N6 87.5(2) . . ? N9 Ni2 N6 170.4(2) 2_755 . ? N6 Ni2 N6 98.1(4) 2_755 . ? N9 Ni2 N5 104.3(2) . 2_755 ? N9 Ni2 N5 85.7(2) 2_755 2_755 ? N6 Ni2 N5 83.9(2) 2_755 2_755 ? N6 Ni2 N5 87.1(2) . 2_755 ? N9 Ni2 N5 85.7(2) . . ? N9 Ni2 N5 104.3(2) 2_755 . ? N6 Ni2 N5 87.1(2) 2_755 . ? N6 Ni2 N5 83.9(2) . . ? N5 Ni2 N5 166.2(3) 2_755 . ? O4 Cl1 O2 109.0(6) . . ? O4 Cl1 O1 110.1(5) . . ? O2 Cl1 O1 109.4(5) . . ? O4 Cl1 O3 108.8(5) . . ? O2 Cl1 O3 108.6(5) . . ? O1 Cl1 O3 110.9(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ni1 N10 C27 N11 98(13) . . . 2_755 ? Ni1 N10 C27 N11 -32(5) . . . . ? N12 C28 N13 C29 -53(38) . . . . ? C28 N13 C29 N14 106(13) . . . . ? N13 C29 N14 C29 -14(13) . . . 2_755 ? N1 C1 C2 N2 58.1(10) . . . . ? N2 C3 C5 C6 -71.9(11) . . . . ? C4 C3 C5 C6 160.6(9) . . . . ? C3 C5 C6 N3 61.6(12) . . . . ? C3 C5 C6 C7 -173.9(9) . . . . ? C3 C5 C6 C8 -55.6(13) . . . . ? N3 C9 C10 N4 61.1(11) . . . . ? N4 C11 C13 C14 -72.8(12) . . . . ? C12 C11 C13 C14 163.6(11) . . . . ? C11 C13 C14 N1 59.8(14) . . . . ? C11 C13 C14 C15 -175.9(10) . . . . ? C11 C13 C14 C16 -57.0(12) . . . . ? N5 C17 C18 N6 -59.5(8) . . . . ? N5 C21 C22 C19 -58.9(10) . . . 2_755 ? C23 C21 C22 C19 58.9(10) . . . 2_755 ? C24 C21 C22 C19 176.8(8) . . . 2_755 ? C13 C14 N1 C1 77.2(11) . . . . ? C15 C14 N1 C1 -46.1(10) . . . . ? C16 C14 N1 C1 -163.5(8) . . . . ? C13 C14 N1 Ni1 -47.1(12) . . . . ? C15 C14 N1 Ni1 -170.5(7) . . . . ? C16 C14 N1 Ni1 72.1(9) . . . . ? C2 C1 N1 C14 -171.3(8) . . . . ? C2 C1 N1 Ni1 -37.3(8) . . . . ? C1 C2 N2 C3 -172.5(8) . . . . ? C1 C2 N2 Ni1 -44.1(8) . . . . ? C5 C3 N2 C2 -173.3(8) . . . . ? C4 C3 N2 C2 -48.1(11) . . . . ? C5 C3 N2 Ni1 64.7(9) . . . . ? C4 C3 N2 Ni1 -170.2(7) . . . . ? C10 C9 N3 C6 -174.6(8) . . . . ? C10 C9 N3 Ni1 -40.4(9) . . . . ? C7 C6 N3 C9 -46.5(11) . . . . ? C5 C6 N3 C9 75.1(9) . . . . ? C8 C6 N3 C9 -163.9(8) . . . . ? C7 C6 N3 Ni1 -170.3(7) . . . . ? C5 C6 N3 Ni1 -48.8(9) . . . . ? C8 C6 N3 Ni1 72.3(9) . . . . ? C12 C11 N4 C10 -52.7(12) . . . . ? C13 C11 N4 C10 -172.6(8) . . . . ? C12 C11 N4 Ni1 -171.8(8) . . . . ? C13 C11 N4 Ni1 68.3(9) . . . . ? C9 C10 N4 C11 -169.6(8) . . . . ? C9 C10 N4 Ni1 -44.6(9) . . . . ? C18 C17 N5 C21 174.7(6) . . . . ? C18 C17 N5 Ni2 40.0(7) . . . . ? C23 C21 N5 C17 164.3(6) . . . . ? C22 C21 N5 C17 -75.6(8) . . . . ? C24 C21 N5 C17 45.9(9) . . . . ? C23 C21 N5 Ni2 -69.9(7) . . . . ? C22 C21 N5 Ni2 50.2(8) . . . . ? C24 C21 N5 Ni2 171.7(5) . . . . ? C22 C19 N6 C18 173.1(6) 2_755 . . . ? C20 C19 N6 C18 52.8(9) . . . . ? C22 C19 N6 Ni2 -66.6(7) 2_755 . . . ? C20 C19 N6 Ni2 173.2(6) . . . . ? C17 C18 N6 C19 171.1(6) . . . . ? C17 C18 N6 Ni2 44.5(7) . . . . ? N8 C25 N7 Ni1 -130(5) . . . . ? N7 C25 N8 C26 -177(6) . . . . ? N9 C26 N8 C25 174(6) . . . . ? N8 C26 N9 Ni2 80(12) . . . . ? C27 N10 Ni1 N7 -18(2) . . . . ? C27 N10 Ni1 N2 31(3) . . . . ? C27 N10 Ni1 N4 169(2) . . . . ? C27 N10 Ni1 N1 -103(2) . . . . ? C27 N10 Ni1 N3 85(2) . . . . ? C25 N7 Ni1 N10 -75(4) . . . . ? C25 N7 Ni1 N2 114(4) . . . . ? C25 N7 Ni1 N4 -21(5) . . . . ? C25 N7 Ni1 N1 29(4) . . . . ? C25 N7 Ni1 N3 -160(4) . . . . ? C2 N2 Ni1 N10 -117.8(15) . . . . ? C3 N2 Ni1 N10 9.0(18) . . . . ? C2 N2 Ni1 N7 -68.6(5) . . . . ? C3 N2 Ni1 N7 58.2(6) . . . . ? C2 N2 Ni1 N4 104.5(5) . . . . ? C3 N2 Ni1 N4 -128.6(6) . . . . ? C2 N2 Ni1 N1 17.5(5) . . . . ? C3 N2 Ni1 N1 144.4(6) . . . . ? C2 N2 Ni1 N3 -171.6(5) . . . . ? C3 N2 Ni1 N3 -44.8(6) . . . . ? C11 N4 Ni1 N10 55.6(7) . . . . ? C10 N4 Ni1 N10 -68.3(6) . . . . ? C11 N4 Ni1 N7 2(2) . . . . ? C10 N4 Ni1 N7 -122.2(18) . . . . ? C11 N4 Ni1 N2 -132.1(7) . . . . ? C10 N4 Ni1 N2 103.9(6) . . . . ? C11 N4 Ni1 N1 -48.3(7) . . . . ? C10 N4 Ni1 N1 -172.2(6) . . . . ? C11 N4 Ni1 N3 141.7(7) . . . . ? C10 N4 Ni1 N3 17.7(6) . . . . ? C14 N1 Ni1 N10 -49.6(8) . . . . ? C1 N1 Ni1 N10 -178.7(6) . . . . ? C14 N1 Ni1 N7 -133.9(7) . . . . ? C1 N1 Ni1 N7 97.0(6) . . . . ? C14 N1 Ni1 N2 138.7(7) . . . . ? C1 N1 Ni1 N2 9.6(5) . . . . ? C14 N1 Ni1 N4 38.8(7) . . . . ? C1 N1 Ni1 N4 -90.3(6) . . . . ? C14 N1 Ni1 N3 91.6(16) . . . . ? C1 N1 Ni1 N3 -37.5(16) . . . . ? C9 N3 Ni1 N10 100.7(7) . . . . ? C6 N3 Ni1 N10 -131.0(7) . . . . ? C9 N3 Ni1 N7 -174.8(6) . . . . ? C6 N3 Ni1 N7 -46.6(7) . . . . ? C9 N3 Ni1 N2 -88.6(6) . . . . ? C6 N3 Ni1 N2 39.7(7) . . . . ? C9 N3 Ni1 N4 11.4(6) . . . . ? C6 N3 Ni1 N4 139.7(7) . . . . ? C9 N3 Ni1 N1 -41.7(17) . . . . ? C6 N3 Ni1 N1 86.6(15) . . . . ? C26 N9 Ni2 N9 128(9) . . . 2_755 ? C26 N9 Ni2 N6 65(10) . . . 2_755 ? C26 N9 Ni2 N6 -61(9) . . . . ? C26 N9 Ni2 N5 -147(9) . . . 2_755 ? C26 N9 Ni2 N5 23(9) . . . . ? C19 N6 Ni2 N9 -55.6(5) . . . . ? C18 N6 Ni2 N9 68.4(5) . . . . ? C19 N6 Ni2 N9 7.1(17) . . . 2_755 ? C18 N6 Ni2 N9 131.1(14) . . . 2_755 ? C19 N6 Ni2 N6 132.3(6) . . . 2_755 ? C18 N6 Ni2 N6 -103.8(5) . . . 2_755 ? C19 N6 Ni2 N5 48.8(5) . . . 2_755 ? C18 N6 Ni2 N5 172.8(5) . . . 2_755 ? C19 N6 Ni2 N5 -141.6(5) . . . . ? C18 N6 Ni2 N5 -17.6(5) . . . . ? C17 N5 Ni2 N9 -99.8(5) . . . . ? C21 N5 Ni2 N9 131.2(6) . . . . ? C17 N5 Ni2 N9 173.3(5) . . . 2_755 ? C21 N5 Ni2 N9 44.3(6) . . . 2_755 ? C17 N5 Ni2 N6 86.6(5) . . . 2_755 ? C21 N5 Ni2 N6 -42.4(6) . . . 2_755 ? C17 N5 Ni2 N6 -11.8(5) . . . . ? C21 N5 Ni2 N6 -140.9(6) . . . . ? C17 N5 Ni2 N5 37.5(5) . . . 2_755 ? C21 N5 Ni2 N5 -91.5(5) . . . 2_755 ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.173 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.118 # Attachment 'R-1.cif' data_R-1 _database_code_depnum_ccdc_archive 'CCDC 722172' # start Validation Reply Form _vrf_PLAT023_R-1 ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 61.44 Deg. RESPONSE: The low data completeness of R-1 is due to the defect of CrysAlis CCD, Gemini S Ultra (Oxford Diffraction Ltd.) when using Cu radiation. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H36 N10 Ni' _chemical_formula_weight 475.30 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.40860(10) _cell_length_b 18.7270(2) _cell_length_c 8.89430(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.8180(10) _cell_angle_gamma 90.00 _cell_volume 1181.22(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2711 _cell_measurement_theta_min 2.4654 _cell_measurement_theta_max 62.5332 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 1.407 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6616 _exptl_absorpt_correction_T_max 0.8493 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0855 _diffrn_measurement_device_type 'Gemini S Ultra' _diffrn_measurement_method '\w and \p scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6707 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 6.24 _diffrn_reflns_theta_max 61.44 _reflns_number_total 3152 _reflns_number_gt 3032 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.038(17) _refine_ls_number_reflns 3152 _refine_ls_number_parameters 285 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0217 _refine_ls_R_factor_gt 0.0204 _refine_ls_wR_factor_ref 0.0500 _refine_ls_wR_factor_gt 0.0496 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.13590(4) 0.249450(16) 0.27638(3) 0.01661(9) Uani 1 1 d . . . N5 N -0.0403(2) 0.28845(9) 0.06972(19) 0.0221(4) Uani 1 1 d U . . C10 C 0.3845(2) 0.24835(14) 0.0764(2) 0.0256(4) Uani 1 1 d . . . H10A H 0.5078 0.2566 0.0570 0.031 Uiso 1 1 calc R . . H10B H 0.2839 0.2616 -0.0198 0.031 Uiso 1 1 calc R . . N1 N 0.1669(2) 0.33909(8) 0.43685(18) 0.0179(3) Uani 1 1 d . . . H1C H 0.0541 0.3415 0.4626 0.021 Uiso 1 1 calc R . . N8 N -0.1106(2) 0.22340(9) 0.33946(19) 0.0235(4) Uani 1 1 d U . . C17 C -0.1371(3) 0.30474(11) -0.0536(2) 0.0212(4) Uani 1 1 d U . . N9 N -0.2814(2) 0.18400(10) 0.5245(2) 0.0282(4) Uani 1 1 d U . . C18 C -0.1962(3) 0.34659(12) -0.3016(3) 0.0249(5) Uani 1 1 d U . . C3 C 0.2346(3) 0.11705(10) 0.4965(2) 0.0206(4) Uani 1 1 d . . . H3 H 0.0953 0.1153 0.4802 0.025 Uiso 1 1 calc R . . C14 C 0.2030(3) 0.41366(11) 0.3902(2) 0.0220(5) Uani 1 1 d . . . C19 C -0.1864(2) 0.20518(11) 0.4299(2) 0.0205(4) Uani 1 1 d U . . N6 N -0.2579(2) 0.32349(10) -0.18515(19) 0.0300(4) Uani 1 1 d U . . C16 C 0.2502(3) 0.46466(12) 0.5317(3) 0.0314(5) Uani 1 1 d . . . H16A H 0.1525 0.4611 0.5857 0.047 Uiso 1 1 calc R . . H16B H 0.2557 0.5138 0.4952 0.047 Uiso 1 1 calc R . . H16C H 0.3726 0.4516 0.6044 0.047 Uiso 1 1 calc R . . C2 C 0.2822(2) 0.23793(11) 0.6164(2) 0.0203(5) Uani 1 1 d . . . H2A H 0.3820 0.2229 0.7115 0.024 Uiso 1 1 calc R . . H2B H 0.1586 0.2318 0.6369 0.024 Uiso 1 1 calc R . . N2 N 0.2898(2) 0.19312(9) 0.48150(18) 0.0178(3) Uani 1 1 d . . . H2C H 0.4150 0.1925 0.4806 0.021 Uiso 1 1 calc R . . N7 N -0.1604(3) 0.36863(11) -0.4106(2) 0.0384(5) Uani 1 1 d U . . C1 C 0.3097(3) 0.31528(11) 0.5815(2) 0.0225(4) Uani 1 1 d . . . H1A H 0.3006 0.3451 0.6710 0.027 Uiso 1 1 calc R . . H1B H 0.4372 0.3218 0.5692 0.027 Uiso 1 1 calc R . . C5 C 0.2803(3) 0.07158(11) 0.3691(2) 0.0245(5) Uani 1 1 d . . . H5A H 0.2689 0.0208 0.3963 0.029 Uiso 1 1 calc R . . H5B H 0.4144 0.0799 0.3759 0.029 Uiso 1 1 calc R . . C4 C 0.3330(3) 0.08588(12) 0.6582(2) 0.0269(5) Uani 1 1 d . . . H4A H 0.4692 0.0938 0.6830 0.040 Uiso 1 1 calc R . . H4B H 0.3077 0.0345 0.6579 0.040 Uiso 1 1 calc R . . H4C H 0.2851 0.1093 0.7375 0.040 Uiso 1 1 calc R . . N10 N -0.1049(3) 0.14334(11) 0.7923(2) 0.0407(5) Uani 1 1 d U . . C20 C -0.1824(3) 0.16326(12) 0.6666(3) 0.0258(5) Uani 1 1 d U . . N3 N 0.1822(2) 0.15682(9) 0.14328(18) 0.0212(4) Uani 1 1 d . . . H3A H 0.0926 0.1606 0.0457 0.025 Uiso 1 1 calc R . . C15 C 0.0208(3) 0.44057(12) 0.2743(3) 0.0287(5) Uani 1 1 d . . . H15A H -0.0149 0.4088 0.1829 0.043 Uiso 1 1 calc R . . H15B H 0.0402 0.4890 0.2403 0.043 Uiso 1 1 calc R . . H15C H -0.0800 0.4411 0.3255 0.043 Uiso 1 1 calc R . . C13 C 0.3670(3) 0.41517(11) 0.3173(2) 0.0249(5) Uani 1 1 d . . . H13A H 0.3871 0.4655 0.2923 0.030 Uiso 1 1 calc R . . H13B H 0.4818 0.3996 0.3990 0.030 Uiso 1 1 calc R . . C9 C 0.3659(3) 0.17087(11) 0.1135(2) 0.0257(5) Uani 1 1 d . . . H9A H 0.3765 0.1412 0.0244 0.031 Uiso 1 1 calc R . . H9B H 0.4697 0.1574 0.2073 0.031 Uiso 1 1 calc R . . C7 C -0.0445(3) 0.06754(12) 0.1724(3) 0.0333(5) Uani 1 1 d . . . H7A H -0.0957 0.1039 0.2280 0.050 Uiso 1 1 calc R . . H7B H -0.0606 0.0202 0.2134 0.050 Uiso 1 1 calc R . . H7C H -0.1116 0.0695 0.0600 0.050 Uiso 1 1 calc R . . N4 N 0.3694(2) 0.29327(9) 0.20957(18) 0.0200(4) Uani 1 1 d . . . H4D H 0.4781 0.2867 0.2926 0.024 Uiso 1 1 calc R . . C11 C 0.3525(3) 0.37087(11) 0.1698(2) 0.0238(4) Uani 1 1 d . . . H11 H 0.2255 0.3794 0.0936 0.029 Uiso 1 1 calc R . . C8 C 0.2391(4) 0.02714(13) 0.0997(3) 0.0386(6) Uani 1 1 d . . . H8A H 0.1866 0.0379 -0.0123 0.058 Uiso 1 1 calc R . . H8B H 0.2009 -0.0210 0.1210 0.058 Uiso 1 1 calc R . . H8C H 0.3770 0.0298 0.1287 0.058 Uiso 1 1 calc R . . C12 C 0.5027(3) 0.39657(13) 0.0944(3) 0.0381(6) Uani 1 1 d . . . H12A H 0.6284 0.3863 0.1651 0.057 Uiso 1 1 calc R . . H12B H 0.4892 0.4481 0.0755 0.057 Uiso 1 1 calc R . . H12C H 0.4865 0.3717 -0.0056 0.057 Uiso 1 1 calc R . . C6 C 0.1649(3) 0.08172(11) 0.1968(2) 0.0259(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01700(14) 0.01841(16) 0.01339(16) 0.00107(15) 0.00277(11) -0.00088(15) N5 0.0208(8) 0.0250(9) 0.0191(9) 0.0029(7) 0.0034(7) -0.0027(7) C10 0.0268(9) 0.0312(11) 0.0219(9) 0.0007(12) 0.0117(7) -0.0004(12) N1 0.0176(8) 0.0172(9) 0.0182(8) 0.0021(7) 0.0043(7) 0.0003(7) N8 0.0189(7) 0.0277(9) 0.0212(8) 0.0024(7) 0.0015(7) -0.0028(6) C17 0.0182(9) 0.0231(10) 0.0230(10) -0.0021(8) 0.0069(8) -0.0013(8) N9 0.0212(8) 0.0395(11) 0.0236(9) 0.0052(8) 0.0061(7) -0.0019(7) C18 0.0220(10) 0.0267(12) 0.0227(11) -0.0002(9) 0.0014(9) 0.0043(9) C3 0.0223(10) 0.0190(11) 0.0192(10) 0.0036(9) 0.0042(8) 0.0005(8) C14 0.0244(11) 0.0181(11) 0.0224(11) -0.0012(9) 0.0049(9) -0.0021(9) C19 0.0140(9) 0.0222(11) 0.0219(10) -0.0006(8) -0.0002(8) -0.0001(7) N6 0.0217(8) 0.0449(11) 0.0203(9) 0.0070(8) 0.0011(7) 0.0020(8) C16 0.0381(12) 0.0226(12) 0.0331(13) -0.0057(10) 0.0099(10) -0.0028(10) C2 0.0199(8) 0.0262(14) 0.0131(9) 0.0005(9) 0.0020(7) 0.0002(9) N2 0.0178(8) 0.0194(9) 0.0165(8) 0.0001(7) 0.0054(7) -0.0006(6) N7 0.0399(11) 0.0490(13) 0.0293(11) 0.0090(9) 0.0148(9) 0.0086(9) C1 0.0233(10) 0.0232(12) 0.0180(10) -0.0006(9) 0.0012(8) 0.0001(8) C5 0.0327(12) 0.0166(11) 0.0230(11) 0.0020(9) 0.0061(10) 0.0048(9) C4 0.0310(11) 0.0255(12) 0.0220(11) 0.0079(9) 0.0041(9) 0.0040(9) N10 0.0486(11) 0.0461(13) 0.0267(11) 0.0049(9) 0.0098(9) 0.0014(10) C20 0.0263(10) 0.0264(11) 0.0272(11) -0.0030(9) 0.0120(9) -0.0031(9) N3 0.0248(8) 0.0216(9) 0.0157(9) 0.0005(7) 0.0036(7) -0.0012(7) C15 0.0286(11) 0.0225(11) 0.0316(13) 0.0033(10) 0.0035(10) 0.0042(9) C13 0.0247(11) 0.0210(11) 0.0278(12) 0.0016(9) 0.0055(9) -0.0043(9) C9 0.0256(10) 0.0272(12) 0.0256(11) -0.0060(9) 0.0093(9) -0.0004(9) C7 0.0429(13) 0.0287(13) 0.0246(12) 0.0004(9) 0.0038(10) -0.0147(10) N4 0.0191(8) 0.0219(10) 0.0182(8) -0.0002(7) 0.0042(7) 0.0005(7) C11 0.0221(10) 0.0227(11) 0.0256(11) 0.0049(9) 0.0054(9) -0.0039(9) C8 0.0622(15) 0.0256(13) 0.0279(12) -0.0063(10) 0.0129(11) 0.0005(11) C12 0.0445(13) 0.0334(14) 0.0429(15) 0.0000(11) 0.0228(12) -0.0108(11) C6 0.0367(11) 0.0203(11) 0.0199(11) 0.0000(8) 0.0071(9) -0.0015(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N5 2.0561(16) . ? Ni1 N8 2.1166(16) . ? Ni1 N2 2.1301(16) . ? Ni1 N4 2.1480(15) . ? Ni1 N1 2.1721(16) . ? Ni1 N3 2.1825(16) . ? N5 C17 1.164(3) . ? C10 N4 1.483(3) . ? C10 C9 1.503(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? N1 C1 1.478(2) . ? N1 C14 1.503(3) . ? N1 H1C 0.9300 . ? N8 C19 1.158(2) . ? C17 N6 1.299(3) . ? N9 C19 1.305(3) . ? N9 C20 1.323(3) . ? C18 N7 1.154(3) . ? C18 N6 1.320(3) . ? C3 N2 1.499(3) . ? C3 C4 1.528(3) . ? C3 C5 1.531(3) . ? C3 H3 1.0000 . ? C14 C15 1.528(3) . ? C14 C13 1.534(3) . ? C14 C16 1.537(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C2 N2 1.479(3) . ? C2 C1 1.508(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N2 H2C 0.9300 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C5 C6 1.536(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? N10 C20 1.161(3) . ? N3 C9 1.483(2) . ? N3 C6 1.502(3) . ? N3 H3A 0.9300 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C13 C11 1.529(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C7 C6 1.526(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? N4 C11 1.492(3) . ? N4 H4D 0.9300 . ? C11 C12 1.534(3) . ? C11 H11 1.0000 . ? C8 C6 1.538(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 N5 Ni1 N8 86.88(6) . . ? N5 Ni1 N2 170.27(7) . . ? N8 Ni1 N2 87.01(6) . . ? N5 Ni1 N4 88.33(6) . . ? N8 Ni1 N4 170.75(6) . . ? N2 Ni1 N4 98.73(6) . . ? N5 Ni1 N1 103.42(6) . . ? N8 Ni1 N1 86.53(6) . . ? N2 Ni1 N1 83.76(6) . . ? N4 Ni1 N1 86.90(6) . . ? N5 Ni1 N3 87.49(6) . . ? N8 Ni1 N3 104.10(6) . . ? N2 Ni1 N3 86.66(6) . . ? N4 Ni1 N3 83.57(6) . . ? N1 Ni1 N3 165.31(6) . . ? C17 N5 Ni1 173.76(16) . . ? N4 C10 C9 109.84(15) . . ? N4 C10 H10A 109.7 . . ? C9 C10 H10A 109.7 . . ? N4 C10 H10B 109.7 . . ? C9 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? C1 N1 C14 112.41(14) . . ? C1 N1 Ni1 104.60(12) . . ? C14 N1 Ni1 122.03(12) . . ? C1 N1 H1C 105.5 . . ? C14 N1 H1C 105.5 . . ? Ni1 N1 H1C 105.5 . . ? C19 N8 Ni1 151.80(14) . . ? N5 C17 N6 174.6(2) . . ? C19 N9 C20 116.88(17) . . ? N7 C18 N6 173.3(2) . . ? N2 C3 C4 112.27(16) . . ? N2 C3 C5 109.78(16) . . ? C4 C3 C5 109.67(16) . . ? N2 C3 H3 108.3 . . ? C4 C3 H3 108.3 . . ? C5 C3 H3 108.3 . . ? N1 C14 C15 107.45(15) . . ? N1 C14 C13 111.07(16) . . ? C15 C14 C13 111.23(17) . . ? N1 C14 C16 111.58(16) . . ? C15 C14 C16 107.15(18) . . ? C13 C14 C16 108.31(17) . . ? N8 C19 N9 176.4(2) . . ? C17 N6 C18 119.40(17) . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C2 C1 109.81(15) . . ? N2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 N2 C3 113.06(15) . . ? C2 N2 Ni1 106.11(11) . . ? C3 N2 Ni1 117.05(11) . . ? C2 N2 H2C 106.7 . . ? C3 N2 H2C 106.7 . . ? Ni1 N2 H2C 106.7 . . ? N1 C1 C2 111.33(15) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C3 C5 C6 119.41(17) . . ? C3 C5 H5A 107.5 . . ? C6 C5 H5A 107.5 . . ? C3 C5 H5B 107.5 . . ? C6 C5 H5B 107.5 . . ? H5A C5 H5B 107.0 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N10 C20 N9 176.1(2) . . ? C9 N3 C6 112.92(15) . . ? C9 N3 Ni1 104.61(12) . . ? C6 N3 Ni1 122.08(12) . . ? C9 N3 H3A 105.3 . . ? C6 N3 H3A 105.3 . . ? Ni1 N3 H3A 105.3 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C13 C14 119.01(16) . . ? C11 C13 H13A 107.6 . . ? C14 C13 H13A 107.6 . . ? C11 C13 H13B 107.6 . . ? C14 C13 H13B 107.6 . . ? H13A C13 H13B 107.0 . . ? N3 C9 C10 110.94(16) . . ? N3 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.0 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C10 N4 C11 112.55(16) . . ? C10 N4 Ni1 104.90(12) . . ? C11 N4 Ni1 114.74(11) . . ? C10 N4 H4D 108.1 . . ? C11 N4 H4D 108.1 . . ? Ni1 N4 H4D 108.1 . . ? N4 C11 C13 110.15(16) . . ? N4 C11 C12 112.80(17) . . ? C13 C11 C12 108.97(17) . . ? N4 C11 H11 108.3 . . ? C13 C11 H11 108.3 . . ? C12 C11 H11 108.3 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C6 C7 107.11(16) . . ? N3 C6 C5 110.98(16) . . ? C7 C6 C5 111.72(18) . . ? N3 C6 C8 111.54(17) . . ? C7 C6 C8 108.55(18) . . ? C5 C6 C8 106.97(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N8 Ni1 N5 C17 -101.0(14) . . . . ? N2 Ni1 N5 C17 -49.8(16) . . . . ? N4 Ni1 N5 C17 86.9(14) . . . . ? N1 Ni1 N5 C17 173.3(14) . . . . ? N3 Ni1 N5 C17 3.3(14) . . . . ? N5 Ni1 N1 C1 -173.93(11) . . . . ? N8 Ni1 N1 C1 100.12(12) . . . . ? N2 Ni1 N1 C1 12.75(11) . . . . ? N4 Ni1 N1 C1 -86.39(12) . . . . ? N3 Ni1 N1 C1 -36.9(3) . . . . ? N5 Ni1 N1 C14 -45.06(14) . . . . ? N8 Ni1 N1 C14 -131.02(14) . . . . ? N2 Ni1 N1 C14 141.61(14) . . . . ? N4 Ni1 N1 C14 42.47(13) . . . . ? N3 Ni1 N1 C14 92.0(3) . . . . ? N5 Ni1 N8 C19 -169.3(3) . . . . ? N2 Ni1 N8 C19 18.3(3) . . . . ? N4 Ni1 N8 C19 -110.4(5) . . . . ? N1 Ni1 N8 C19 -65.6(3) . . . . ? N3 Ni1 N8 C19 104.1(3) . . . . ? Ni1 N5 C17 N6 121(2) . . . . ? C1 N1 C14 C15 -162.77(16) . . . . ? Ni1 N1 C14 C15 71.82(19) . . . . ? C1 N1 C14 C13 75.4(2) . . . . ? Ni1 N1 C14 C13 -50.04(19) . . . . ? C1 N1 C14 C16 -45.6(2) . . . . ? Ni1 N1 C14 C16 -171.00(13) . . . . ? Ni1 N8 C19 N9 -167(3) . . . . ? C20 N9 C19 N8 161(3) . . . . ? N5 C17 N6 C18 162(2) . . . . ? N7 C18 N6 C17 -171(2) . . . . ? C1 C2 N2 C3 -171.25(14) . . . . ? C1 C2 N2 Ni1 -41.64(15) . . . . ? C4 C3 N2 C2 -47.4(2) . . . . ? C5 C3 N2 C2 -169.70(14) . . . . ? C4 C3 N2 Ni1 -171.22(12) . . . . ? C5 C3 N2 Ni1 66.52(17) . . . . ? N5 Ni1 N2 C2 -122.4(4) . . . . ? N8 Ni1 N2 C2 -71.26(11) . . . . ? N4 Ni1 N2 C2 101.45(11) . . . . ? N1 Ni1 N2 C2 15.57(11) . . . . ? N3 Ni1 N2 C2 -175.58(12) . . . . ? N5 Ni1 N2 C3 4.8(5) . . . . ? N8 Ni1 N2 C3 56.00(13) . . . . ? N4 Ni1 N2 C3 -131.30(13) . . . . ? N1 Ni1 N2 C3 142.82(13) . . . . ? N3 Ni1 N2 C3 -48.33(13) . . . . ? C14 N1 C1 C2 -174.11(15) . . . . ? Ni1 N1 C1 C2 -39.67(17) . . . . ? N2 C2 C1 N1 57.34(19) . . . . ? N2 C3 C5 C6 -69.7(2) . . . . ? C4 C3 C5 C6 166.55(18) . . . . ? C19 N9 C20 N10 -165(4) . . . . ? N5 Ni1 N3 C9 99.91(12) . . . . ? N8 Ni1 N3 C9 -173.94(11) . . . . ? N2 Ni1 N3 C9 -87.87(12) . . . . ? N4 Ni1 N3 C9 11.31(11) . . . . ? N1 Ni1 N3 C9 -38.6(3) . . . . ? N5 Ni1 N3 C6 -130.42(14) . . . . ? N8 Ni1 N3 C6 -44.27(14) . . . . ? N2 Ni1 N3 C6 41.80(13) . . . . ? N4 Ni1 N3 C6 140.99(14) . . . . ? N1 Ni1 N3 C6 91.1(3) . . . . ? N1 C14 C13 C11 59.4(2) . . . . ? C15 C14 C13 C11 -60.3(2) . . . . ? C16 C14 C13 C11 -177.75(18) . . . . ? C6 N3 C9 C10 -174.20(15) . . . . ? Ni1 N3 C9 C10 -39.27(17) . . . . ? N4 C10 C9 N3 59.31(19) . . . . ? C9 C10 N4 C11 -169.86(14) . . . . ? C9 C10 N4 Ni1 -44.45(16) . . . . ? N5 Ni1 N4 C10 -70.03(12) . . . . ? N8 Ni1 N4 C10 -128.8(4) . . . . ? N2 Ni1 N4 C10 103.24(12) . . . . ? N1 Ni1 N4 C10 -173.56(13) . . . . ? N3 Ni1 N4 C10 17.63(12) . . . . ? N5 Ni1 N4 C11 53.99(13) . . . . ? N8 Ni1 N4 C11 -4.8(5) . . . . ? N2 Ni1 N4 C11 -132.74(12) . . . . ? N1 Ni1 N4 C11 -49.54(12) . . . . ? N3 Ni1 N4 C11 141.65(13) . . . . ? C10 N4 C11 C13 -171.61(14) . . . . ? Ni1 N4 C11 C13 68.53(16) . . . . ? C10 N4 C11 C12 -49.6(2) . . . . ? Ni1 N4 C11 C12 -169.46(13) . . . . ? C14 C13 C11 N4 -71.3(2) . . . . ? C14 C13 C11 C12 164.43(18) . . . . ? C9 N3 C6 C7 -162.22(16) . . . . ? Ni1 N3 C6 C7 71.75(18) . . . . ? C9 N3 C6 C5 75.6(2) . . . . ? Ni1 N3 C6 C5 -50.4(2) . . . . ? C9 N3 C6 C8 -43.6(2) . . . . ? Ni1 N3 C6 C8 -169.61(14) . . . . ? C3 C5 C6 N3 60.2(2) . . . . ? C3 C5 C6 C7 -59.3(3) . . . . ? C3 C5 C6 C8 -177.97(19) . . . . ? 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 N1 H1C N7 0.93 2.26 3.151(2) 161.4 1_556 N2 H2C N9 0.93 2.17 3.093(2) 169.0 1_655 N3 H3A N10 0.93 2.33 3.239(3) 166.3 1_554 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 61.44 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.120 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.037 # Attachment 'S-1.cif' data_S-1 _database_code_depnum_ccdc_archive 'CCDC 722173' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H36 N10 Ni' _chemical_formula_weight 475.30 _chemical_absolute_configuration ad 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.459(2) _cell_length_b 18.836(6) _cell_length_c 8.948(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.989(5) _cell_angle_gamma 90.00 _cell_volume 1202.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1893 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7206 _exptl_absorpt_correction_T_max 0.7999 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 5117 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3360 _reflns_number_gt 2705 _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^)+(0.0775P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 3360 _refine_ls_number_parameters 286 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0672 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1296 _refine_ls_wR_factor_gt 0.1099 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 C1 C 0.1874(9) 0.8196(3) 0.4183(7) 0.0255(14) Uani 1 1 d . . . H1A H 0.0614 0.8133 0.4321 0.031 Uiso 1 1 calc R . . H1B H 0.1945 0.7901 0.3286 0.031 Uiso 1 1 calc R . . C2 C 0.2171(8) 0.8976(3) 0.3850(6) 0.0209(14) Uani 1 1 d . . . H2A H 0.3405 0.9035 0.3659 0.025 Uiso 1 1 calc R . . H2B H 0.1188 0.9130 0.2899 0.025 Uiso 1 1 calc R . . C3 C 0.2641(8) 1.0176(3) 0.5038(6) 0.0208(12) Uani 1 1 d . . . H3 H 0.4025 1.0192 0.5199 0.025 Uiso 1 1 calc R . . C4 C 0.1655(9) 1.0493(3) 0.3415(7) 0.0298(14) Uani 1 1 d . . . H4A H 0.2108 1.0254 0.2622 0.045 Uiso 1 1 calc R . . H4B H 0.1932 1.1001 0.3417 0.045 Uiso 1 1 calc R . . H4C H 0.0298 1.0424 0.3175 0.045 Uiso 1 1 calc R . . C5 C 0.2198(10) 1.0635(3) 0.6319(7) 0.0293(16) Uani 1 1 d . . . H5A H 0.2318 1.1139 0.6050 0.035 Uiso 1 1 calc R . . H5B H 0.0867 1.0555 0.6257 0.035 Uiso 1 1 calc R . . C6 C 0.3362(10) 1.0530(3) 0.8034(7) 0.0326(16) Uani 1 1 d . . . C7 C 0.5422(10) 1.0676(4) 0.8280(7) 0.0349(16) Uani 1 1 d . . . H7A H 0.6096 1.0641 0.9395 0.052 Uiso 1 1 calc R . . H7B H 0.5576 1.1155 0.7907 0.052 Uiso 1 1 calc R . . H7C H 0.5928 1.0328 0.7697 0.052 Uiso 1 1 calc R . . C8 C 0.2603(12) 1.1068(4) 0.9008(8) 0.0429(18) Uani 1 1 d . . . H8A H 0.1258 1.0989 0.8827 0.064 Uiso 1 1 calc R . . H8B H 0.2810 1.1552 0.8694 0.064 Uiso 1 1 calc R . . H8C H 0.3260 1.1003 1.0120 0.064 Uiso 1 1 calc R . . C9 C 0.1361(8) 0.9639(3) 0.8863(7) 0.0260(13) Uani 1 1 d . . . H9A H 0.0333 0.9773 0.7924 0.031 Uiso 1 1 calc R . . H9B H 0.1252 0.9936 0.9745 0.031 Uiso 1 1 calc R . . C10 C 0.1162(7) 0.8856(4) 0.9240(5) 0.0267(11) Uani 1 1 d . . . H10A H 0.2153 0.8723 1.0204 0.032 Uiso 1 1 calc R . . H10B H -0.0072 0.8773 0.9416 0.032 Uiso 1 1 calc R . . C11 C 0.1489(8) 0.7632(3) 0.8303(7) 0.0245(13) Uani 1 1 d . . . H11 H 0.2747 0.7542 0.9064 0.029 Uiso 1 1 calc R . . C12 C -0.0032(12) 0.7386(4) 0.9043(9) 0.047(2) Uani 1 1 d . . . H12A H 0.0187 0.7607 1.0072 0.070 Uiso 1 1 calc R . . H12B H 0.0022 0.6868 0.9160 0.070 Uiso 1 1 calc R . . H12C H -0.1270 0.7525 0.8368 0.070 Uiso 1 1 calc R . . C13 C 0.1333(8) 0.7200(3) 0.6818(7) 0.0262(14) Uani 1 1 d . . . H13A H 0.1127 0.6698 0.7053 0.031 Uiso 1 1 calc R . . H13B H 0.0188 0.7360 0.6013 0.031 Uiso 1 1 calc R . . C14 C 0.2939(9) 0.7215(3) 0.6084(7) 0.0239(14) Uani 1 1 d . . . C15 C 0.4801(8) 0.6945(3) 0.7240(7) 0.0278(14) Uani 1 1 d . . . H15A H 0.5768 0.6915 0.6700 0.042 Uiso 1 1 calc R . . H15B H 0.4601 0.6474 0.7629 0.042 Uiso 1 1 calc R . . H15C H 0.5209 0.7276 0.8120 0.042 Uiso 1 1 calc R . . C16 C 0.2463(10) 0.6709(4) 0.4670(8) 0.0366(16) Uani 1 1 d . . . H16A H 0.1308 0.6868 0.3899 0.055 Uiso 1 1 calc R . . H16B H 0.2284 0.6227 0.5017 0.055 Uiso 1 1 calc R . . H16C H 0.3492 0.6709 0.4196 0.055 Uiso 1 1 calc R . . C17 C 0.6866(8) 0.9296(3) 0.5704(6) 0.0233(13) Uani 1 1 d . . . C18 C 0.6857(11) 0.9714(4) 0.3351(8) 0.0298(16) Uani 1 1 d . . . C19 C 0.6357(9) 0.8297(3) 1.0525(7) 0.0268(14) Uani 1 1 d . . . C20 C 0.6943(11) 0.7879(4) 1.3005(8) 0.0275(17) Uani 1 1 d . . . N9 N 0.7605(7) 0.8105(3) 1.1851(5) 0.0349(14) Uani 1 1 d . . . N1 N 0.3331(7) 0.7962(3) 0.5621(5) 0.0203(11) Uani 1 1 d . . . H1C H 0.4446 0.7936 0.5357 0.024 Uiso 1 1 calc R . . N2 N 0.2093(7) 0.9420(3) 0.5182(5) 0.0196(10) Uani 1 1 d . . . H2C H 0.0850 0.9425 0.5190 0.024 Uiso 1 1 calc R . . N3 N 0.3178(7) 0.9777(3) 0.8579(5) 0.0259(12) Uani 1 1 d . . . H3A H 0.4068 0.9739 0.9551 0.031 Uiso 1 1 calc R . . N4 N 0.1331(6) 0.8416(2) 0.7913(5) 0.0192(10) Uani 1 1 d . . . H4D H 0.0249 0.8483 0.7087 0.023 Uiso 1 1 calc R . . N5 N 0.6106(7) 0.9119(3) 0.6608(5) 0.0253(11) Uani 1 1 d . . . N6 N 0.7825(7) 0.9508(3) 0.4757(6) 0.0305(13) Uani 1 1 d . . . N7 N 0.6045(10) 0.9914(3) 0.2081(7) 0.0499(17) Uani 1 1 d . . . N8 N 0.5412(7) 0.8463(3) 0.9301(5) 0.0238(11) Uani 1 1 d . . . N10 N 0.6598(9) 0.7663(4) 1.4096(6) 0.0462(16) Uani 1 1 d . . . Ni1 Ni 0.36457(9) 0.88542(3) 0.72357(6) 0.01768(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.034(4) 0.021(3) 0.019(3) -0.003(2) 0.004(3) 0.000(3) C2 0.021(3) 0.023(4) 0.017(2) 0.007(3) 0.0020(19) -0.001(3) C3 0.021(3) 0.018(3) 0.023(3) 0.006(2) 0.006(2) 0.001(2) C4 0.036(4) 0.024(3) 0.028(3) 0.009(3) 0.007(3) 0.006(3) C5 0.042(4) 0.016(3) 0.028(3) 0.001(3) 0.007(3) 0.000(3) C6 0.060(5) 0.016(3) 0.021(3) -0.002(2) 0.011(3) -0.007(3) C7 0.046(4) 0.029(4) 0.027(3) 0.000(3) 0.007(3) -0.016(3) C8 0.076(6) 0.025(4) 0.026(3) -0.004(3) 0.013(3) -0.002(4) C9 0.027(3) 0.022(3) 0.031(3) -0.002(3) 0.011(3) 0.002(3) C10 0.026(3) 0.032(3) 0.026(2) -0.003(4) 0.013(2) 0.001(4) C11 0.023(3) 0.019(3) 0.030(3) 0.005(3) 0.006(2) -0.007(3) C12 0.071(6) 0.030(4) 0.051(4) 0.003(3) 0.035(4) -0.018(4) C13 0.022(4) 0.020(3) 0.035(3) -0.002(3) 0.006(3) -0.003(3) C14 0.031(4) 0.013(3) 0.026(3) -0.002(3) 0.006(3) -0.003(3) C15 0.026(4) 0.025(3) 0.031(4) -0.001(3) 0.006(3) 0.006(3) C16 0.051(5) 0.024(3) 0.036(4) -0.013(3) 0.013(3) -0.004(3) C17 0.024(3) 0.024(3) 0.018(3) 0.001(2) 0.001(2) -0.002(3) C18 0.046(4) 0.023(4) 0.027(4) -0.004(3) 0.020(3) -0.008(3) C19 0.037(4) 0.021(3) 0.025(3) -0.002(3) 0.015(3) -0.002(3) C20 0.035(4) 0.025(4) 0.019(3) -0.002(3) 0.002(3) 0.003(3) N9 0.035(3) 0.051(4) 0.017(2) 0.008(2) 0.005(2) 0.001(3) N1 0.028(3) 0.014(3) 0.021(2) -0.001(2) 0.011(2) 0.002(2) N2 0.024(3) 0.018(2) 0.019(2) 0.002(2) 0.010(2) 0.003(2) N3 0.045(3) 0.017(3) 0.014(2) 0.0011(19) 0.007(2) 0.000(2) N4 0.017(3) 0.019(3) 0.023(2) 0.002(2) 0.0062(19) -0.003(2) N5 0.023(3) 0.030(3) 0.021(2) 0.003(2) 0.002(2) -0.001(2) N6 0.019(3) 0.045(4) 0.028(3) 0.009(2) 0.007(2) -0.003(2) N7 0.081(5) 0.043(4) 0.027(3) 0.008(3) 0.018(3) 0.002(4) N8 0.025(3) 0.024(3) 0.020(3) 0.006(2) 0.002(2) -0.003(2) N10 0.068(5) 0.048(4) 0.029(3) 0.012(3) 0.024(3) 0.014(3) Ni1 0.0235(4) 0.0163(3) 0.0132(3) 0.0015(4) 0.0053(2) -0.0004(4) _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 C1 N1 1.488(7) . ? C1 C2 1.528(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.471(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N2 1.498(8) . ? C3 C4 1.543(8) . ? C3 C5 1.546(9) . ? C3 H3 1.0000 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.539(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.512(10) . ? C6 N3 1.519(8) . ? C6 C8 1.547(9) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N3 1.474(8) . ? C9 C10 1.531(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N4 1.482(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N4 1.514(7) . ? C11 C13 1.534(9) . ? C11 C12 1.543(9) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.526(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N1 1.519(8) . ? C14 C16 1.540(8) . ? C14 C15 1.556(8) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 N5 1.164(7) . ? C17 N6 1.320(8) . ? C18 N7 1.182(9) . ? C18 N6 1.313(9) . ? C19 N8 1.159(8) . ? C19 N9 1.327(8) . ? C20 N10 1.154(8) . ? C20 N9 1.338(9) . ? N1 Ni1 2.184(5) . ? N1 H1C 0.9300 . ? N2 Ni1 2.147(5) . ? N2 H2C 0.9300 . ? N3 Ni1 2.199(5) . ? N3 H3A 0.9300 . ? N4 Ni1 2.154(4) . ? N4 H4D 0.9300 . ? N5 Ni1 2.129(5) . ? N8 Ni1 2.067(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 N1 C1 C2 110.0(5) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? N2 C2 C1 110.3(4) . . ? N2 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? N2 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? N2 C3 C4 112.4(5) . . ? N2 C3 C5 110.2(5) . . ? C4 C3 C5 109.6(5) . . ? N2 C3 H3 108.2 . . ? C4 C3 H3 108.2 . . ? C5 C3 H3 108.2 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C3 119.1(5) . . ? C6 C5 H5A 107.5 . . ? C3 C5 H5A 107.5 . . ? C6 C5 H5B 107.5 . . ? C3 C5 H5B 107.5 . . ? H5A C5 H5B 107.0 . . ? C7 C6 N3 107.9(5) . . ? C7 C6 C5 112.0(5) . . ? N3 C6 C5 111.3(5) . . ? C7 C6 C8 108.8(6) . . ? N3 C6 C8 110.3(5) . . ? C5 C6 C8 106.5(6) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C10 111.2(5) . . ? N3 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? N3 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N4 C10 C9 109.0(4) . . ? N4 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? N4 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? N4 C11 C13 109.7(5) . . ? N4 C11 C12 112.0(5) . . ? C13 C11 C12 109.4(5) . . ? N4 C11 H11 108.5 . . ? C13 C11 H11 108.5 . . ? C12 C11 H11 108.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C11 119.5(5) . . ? C14 C13 H13A 107.4 . . ? C11 C13 H13A 107.4 . . ? C14 C13 H13B 107.4 . . ? C11 C13 H13B 107.4 . . ? H13A C13 H13B 107.0 . . ? N1 C14 C13 111.9(5) . . ? N1 C14 C16 111.5(5) . . ? C13 C14 C16 108.7(5) . . ? N1 C14 C15 106.2(5) . . ? C13 C14 C15 111.6(5) . . ? C16 C14 C15 106.9(5) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 N6 176.2(6) . . ? N7 C18 N6 177.4(8) . . ? N8 C19 N9 173.1(7) . . ? N10 C20 N9 171.6(8) . . ? C19 N9 C20 117.1(6) . . ? C1 N1 C14 111.1(5) . . ? C1 N1 Ni1 104.7(4) . . ? C14 N1 Ni1 121.6(3) . . ? C1 N1 H1C 106.1 . . ? C14 N1 H1C 106.1 . . ? Ni1 N1 H1C 106.1 . . ? C2 N2 C3 113.2(4) . . ? C2 N2 Ni1 105.8(3) . . ? C3 N2 Ni1 116.9(4) . . ? C2 N2 H2C 106.8 . . ? C3 N2 H2C 106.8 . . ? Ni1 N2 H2C 106.8 . . ? C9 N3 C6 113.2(5) . . ? C9 N3 Ni1 104.8(3) . . ? C6 N3 Ni1 121.3(3) . . ? C9 N3 H3A 105.4 . . ? C6 N3 H3A 105.4 . . ? Ni1 N3 H3A 105.4 . . ? C10 N4 C11 112.3(5) . . ? C10 N4 Ni1 105.9(4) . . ? C11 N4 Ni1 115.0(3) . . ? C10 N4 H4D 107.8 . . ? C11 N4 H4D 107.8 . . ? Ni1 N4 H4D 107.8 . . ? C17 N5 Ni1 152.0(5) . . ? C18 N6 C17 117.1(5) . . ? C19 N8 Ni1 173.8(5) . . ? N8 Ni1 N5 86.89(19) . . ? N8 Ni1 N2 170.3(2) . . ? N5 Ni1 N2 87.07(18) . . ? N8 Ni1 N4 88.06(19) . . ? N5 Ni1 N4 170.85(18) . . ? N2 Ni1 N4 98.90(18) . . ? N8 Ni1 N1 103.58(19) . . ? N5 Ni1 N1 86.57(19) . . ? N2 Ni1 N1 83.62(18) . . ? N4 Ni1 N1 87.22(18) . . ? N8 Ni1 N3 87.38(19) . . ? N5 Ni1 N3 104.21(19) . . ? N2 Ni1 N3 86.75(18) . . ? N4 Ni1 N3 83.16(18) . . ? N1 Ni1 N3 165.18(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -58.6(6) . . . . ? N2 C3 C5 C6 69.5(7) . . . . ? C4 C3 C5 C6 -166.3(6) . . . . ? C3 C5 C6 C7 60.3(8) . . . . ? C3 C5 C6 N3 -60.5(8) . . . . ? C3 C5 C6 C8 179.2(6) . . . . ? N3 C9 C10 N4 -59.0(6) . . . . ? N4 C11 C13 C14 71.1(7) . . . . ? C12 C11 C13 C14 -165.6(6) . . . . ? C11 C13 C14 N1 -59.4(7) . . . . ? C11 C13 C14 C16 177.1(5) . . . . ? C11 C13 C14 C15 59.5(7) . . . . ? N8 C19 N9 C20 -167(5) . . . . ? N10 C20 N9 C19 173(5) . . . . ? C2 C1 N1 C14 173.5(5) . . . . ? C2 C1 N1 Ni1 40.4(5) . . . . ? C13 C14 N1 C1 -75.1(6) . . . . ? C16 C14 N1 C1 46.8(7) . . . . ? C15 C14 N1 C1 162.9(5) . . . . ? C13 C14 N1 Ni1 48.9(6) . . . . ? C16 C14 N1 Ni1 170.8(4) . . . . ? C15 C14 N1 Ni1 -73.1(6) . . . . ? C1 C2 N2 C3 171.8(5) . . . . ? C1 C2 N2 Ni1 42.5(5) . . . . ? C4 C3 N2 C2 47.6(6) . . . . ? C5 C3 N2 C2 170.2(5) . . . . ? C4 C3 N2 Ni1 171.0(4) . . . . ? C5 C3 N2 Ni1 -66.4(6) . . . . ? C10 C9 N3 C6 174.0(4) . . . . ? C10 C9 N3 Ni1 39.7(5) . . . . ? C7 C6 N3 C9 162.2(5) . . . . ? C5 C6 N3 C9 -74.6(6) . . . . ? C8 C6 N3 C9 43.5(7) . . . . ? C7 C6 N3 Ni1 -72.0(5) . . . . ? C5 C6 N3 Ni1 51.3(7) . . . . ? C8 C6 N3 Ni1 169.3(4) . . . . ? C9 C10 N4 C11 170.0(4) . . . . ? C9 C10 N4 Ni1 43.7(5) . . . . ? C13 C11 N4 C10 170.7(4) . . . . ? C12 C11 N4 C10 49.0(6) . . . . ? C13 C11 N4 Ni1 -68.0(5) . . . . ? C12 C11 N4 Ni1 170.2(4) . . . . ? N6 C17 N5 Ni1 162(10) . . . . ? N7 C18 N6 C17 158(18) . . . . ? N5 C17 N6 C18 -154(10) . . . . ? N9 C19 N8 Ni1 -125(5) . . . . ? C19 N8 Ni1 N5 108(5) . . . . ? C19 N8 Ni1 N2 57(5) . . . . ? C19 N8 Ni1 N4 -79(5) . . . . ? C19 N8 Ni1 N1 -166(4) . . . . ? C19 N8 Ni1 N3 4(5) . . . . ? C17 N5 Ni1 N8 167.7(10) . . . . ? C17 N5 Ni1 N2 -19.9(10) . . . . ? C17 N5 Ni1 N4 111.1(14) . . . . ? C17 N5 Ni1 N1 63.8(10) . . . . ? C17 N5 Ni1 N3 -105.8(10) . . . . ? C2 N2 Ni1 N8 122.9(12) . . . . ? C3 N2 Ni1 N8 -4.3(14) . . . . ? C2 N2 Ni1 N5 71.3(4) . . . . ? C3 N2 Ni1 N5 -55.8(4) . . . . ? C2 N2 Ni1 N4 -101.7(3) . . . . ? C3 N2 Ni1 N4 131.1(4) . . . . ? C2 N2 Ni1 N1 -15.5(3) . . . . ? C3 N2 Ni1 N1 -142.7(4) . . . . ? C2 N2 Ni1 N3 175.7(4) . . . . ? C3 N2 Ni1 N3 48.6(4) . . . . ? C10 N4 Ni1 N8 70.1(4) . . . . ? C11 N4 Ni1 N8 -54.5(4) . . . . ? C10 N4 Ni1 N5 126.6(11) . . . . ? C11 N4 Ni1 N5 1.9(13) . . . . ? C10 N4 Ni1 N2 -103.1(4) . . . . ? C11 N4 Ni1 N2 132.3(4) . . . . ? C10 N4 Ni1 N1 173.8(4) . . . . ? C11 N4 Ni1 N1 49.2(4) . . . . ? C10 N4 Ni1 N3 -17.5(4) . . . . ? C11 N4 Ni1 N3 -142.1(4) . . . . ? C1 N1 Ni1 N8 173.0(4) . . . . ? C14 N1 Ni1 N8 46.1(5) . . . . ? C1 N1 Ni1 N5 -101.1(4) . . . . ? C14 N1 Ni1 N5 132.1(4) . . . . ? C1 N1 Ni1 N2 -13.6(4) . . . . ? C14 N1 Ni1 N2 -140.5(4) . . . . ? C1 N1 Ni1 N4 85.6(4) . . . . ? C14 N1 Ni1 N4 -41.2(4) . . . . ? C1 N1 Ni1 N3 36.2(9) . . . . ? C14 N1 Ni1 N3 -90.7(8) . . . . ? C9 N3 Ni1 N8 -100.3(4) . . . . ? C6 N3 Ni1 N8 130.1(5) . . . . ? C9 N3 Ni1 N5 173.6(3) . . . . ? C6 N3 Ni1 N5 44.0(5) . . . . ? C9 N3 Ni1 N2 87.4(4) . . . . ? C6 N3 Ni1 N2 -42.2(5) . . . . ? C9 N3 Ni1 N4 -12.0(3) . . . . ? C6 N3 Ni1 N4 -141.6(5) . . . . ? C9 N3 Ni1 N1 37.9(9) . . . . ? C6 N3 Ni1 N1 -91.7(8) . . . . ? 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 N3 H3A N7 0.93 2.34 3.247(8) 166.3 1_556 N2 H2C N6 0.93 2.18 3.099(7) 169.2 1_455 N1 H1C N10 0.93 2.27 3.172(8) 162.0 1_554 _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.981 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.126