Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Way-Zen Lee' _publ_contact_author_email WZLEE@NTNU.EDU.TW _publ_section_title ; Dinickel Complexes of Disubstituted Benzoate Polydentate Ligands: Mimics for the Active Site of Urease ; _publ_contact_author 'Way-Zen Lee' loop_ _publ_author_name 'Way-Zen Lee.' 'Meng-Yu Ku.' 'Ting-Shen Kuo.' 'Huan-Sheng Tseng.' # Attachment '1.cif' data_5763 _database_code_depnum_ccdc_archive 'CCDC 667937' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H70 Cl3 N11 Ni2 O20' _chemical_formula_sum 'C49 H70 Cl3 N11 Ni2 O20' _chemical_formula_weight 1356.93 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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.4365(3) _cell_length_b 34.4541(8) _cell_length_c 14.4644(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.1670(10) _cell_angle_gamma 90.00 _cell_volume 6643.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 45898 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.35 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 0.761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7352 _exptl_absorpt_correction_T_max 0.8033 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50507 _diffrn_reflns_av_R_equivalents 0.0768 _diffrn_reflns_av_sigmaI/netI 0.0698 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.33 _reflns_number_total 12028 _reflns_number_gt 8155 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (O & M 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material 'SHELXTL, Bruker' _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. 3 SADI restraints were used because of the disorder of perchlorate anions. ; _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^)+(0.1105P)^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 12028 _refine_ls_number_parameters 767 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1844 _refine_ls_wR_factor_gt 0.1724 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0065(3) 0.16063(14) 0.1022(4) 0.0449(12) Uani 1 1 d . . . H1 H -0.0021 0.1530 0.0412 0.054 Uiso 1 1 calc R . . C2 C -0.0982(4) 0.16023(16) 0.1345(5) 0.0592(15) Uani 1 1 d . . . H2 H -0.1553 0.1526 0.0957 0.071 Uiso 1 1 calc R . . C3 C -0.1050(4) 0.17130(17) 0.2251(4) 0.0605(16) Uani 1 1 d . . . H3 H -0.1667 0.1711 0.2479 0.073 Uiso 1 1 calc R . . C4 C -0.0212(4) 0.18241(15) 0.2804(4) 0.0491(13) Uani 1 1 d . . . H4 H -0.0250 0.1899 0.3416 0.059 Uiso 1 1 calc R . . C5 C 0.0707(3) 0.18261(13) 0.2454(3) 0.0370(11) Uani 1 1 d . . . C6 C 0.1665(3) 0.19471(13) 0.3005(3) 0.0367(11) Uani 1 1 d . . . H6A H 0.1622 0.1906 0.3662 0.044 Uiso 1 1 calc R . . H6B H 0.1772 0.2222 0.2910 0.044 Uiso 1 1 calc R . . C7 C 0.3451(3) 0.19739(12) 0.2833(3) 0.0331(10) Uani 1 1 d . . . H7A H 0.4045 0.1819 0.2788 0.040 Uiso 1 1 calc R . . H7B H 0.3524 0.2099 0.3439 0.040 Uiso 1 1 calc R . . C8 C 0.3336(3) 0.22776(13) 0.2069(3) 0.0336(10) Uani 1 1 d . . . C9 C 0.3838(4) 0.26299(14) 0.2162(3) 0.0485(13) Uani 1 1 d . . . H9 H 0.4261 0.2690 0.2702 0.058 Uiso 1 1 calc R . . C10 C 0.3693(4) 0.28889(15) 0.1430(4) 0.0544(14) Uani 1 1 d . . . H10 H 0.4023 0.3127 0.1471 0.065 Uiso 1 1 calc R . . C11 C 0.3065(4) 0.27966(14) 0.0648(4) 0.0499(13) Uani 1 1 d . . . H11 H 0.2950 0.2973 0.0159 0.060 Uiso 1 1 calc R . . C12 C 0.2603(3) 0.24390(13) 0.0589(3) 0.0395(11) Uani 1 1 d . . . H12 H 0.2190 0.2374 0.0048 0.047 Uiso 1 1 calc R . . C13 C 0.2685(3) 0.13670(12) 0.3313(3) 0.0294(10) Uani 1 1 d . . . H13A H 0.2047 0.1233 0.3287 0.035 Uiso 1 1 calc R . . H13B H 0.2880 0.1446 0.3954 0.035 Uiso 1 1 calc R . . C14 C 0.3453(3) 0.10856(12) 0.3043(3) 0.0264(9) Uani 1 1 d . . . C15 C 0.3189(3) 0.07953(12) 0.2375(2) 0.0245(9) Uani 1 1 d . . . C16 C 0.2130(3) 0.07758(12) 0.1875(3) 0.0245(9) Uani 1 1 d . . . C17 C 0.3895(3) 0.05196(12) 0.2176(3) 0.0265(9) Uani 1 1 d . . . C18 C 0.4887(3) 0.05508(13) 0.2618(3) 0.0332(10) Uani 1 1 d . . . H18 H 0.5370 0.0376 0.2467 0.040 Uiso 1 1 calc R . . C19 C 0.5151(3) 0.08338(14) 0.3266(3) 0.0394(11) Uani 1 1 d . . . H19 H 0.5808 0.0850 0.3554 0.047 Uiso 1 1 calc R . . C20 C 0.4433(3) 0.10973(13) 0.3494(3) 0.0351(11) Uani 1 1 d . . . H20 H 0.4609 0.1283 0.3951 0.042 Uiso 1 1 calc R . . C21 C 0.3628(3) 0.01958(12) 0.1483(3) 0.0272(9) Uani 1 1 d . . . H21A H 0.3157 0.0295 0.0975 0.033 Uiso 1 1 calc R . . H21B H 0.4230 0.0117 0.1225 0.033 Uiso 1 1 calc R . . C22 C 0.2858(3) -0.04337(12) 0.1119(3) 0.0300(10) Uani 1 1 d . . . H22A H 0.3038 -0.0694 0.1332 0.036 Uiso 1 1 calc R . . H22B H 0.3220 -0.0377 0.0595 0.036 Uiso 1 1 calc R . . C23 C 0.1742(3) -0.04201(12) 0.0795(3) 0.0286(9) Uani 1 1 d . . . C24 C 0.1353(3) -0.05595(13) -0.0077(3) 0.0371(11) Uani 1 1 d . . . H24 H 0.1780 -0.0633 -0.0506 0.045 Uiso 1 1 calc R . . C25 C 0.0327(4) -0.05879(14) -0.0300(3) 0.0441(12) Uani 1 1 d . . . H25 H 0.0051 -0.0683 -0.0878 0.053 Uiso 1 1 calc R . . C26 C -0.0284(3) -0.04730(14) 0.0350(3) 0.0406(12) Uani 1 1 d . . . H26 H -0.0978 -0.0491 0.0220 0.049 Uiso 1 1 calc R . . C27 C 0.0155(3) -0.03309(13) 0.1200(3) 0.0383(11) Uani 1 1 d . . . H27 H -0.0260 -0.0250 0.1632 0.046 Uiso 1 1 calc R . . C28 C 0.3913(3) -0.03478(12) 0.2589(3) 0.0274(9) Uani 1 1 d . . . H28A H 0.4249 -0.0155 0.3005 0.033 Uiso 1 1 calc R . . H28B H 0.4416 -0.0479 0.2276 0.033 Uiso 1 1 calc R . . C29 C 0.3398(3) -0.06391(12) 0.3148(3) 0.0285(9) Uani 1 1 d . . . C30 C 0.3906(3) -0.09484(13) 0.3601(3) 0.0401(11) Uani 1 1 d . . . H30 H 0.4572 -0.0996 0.3527 0.048 Uiso 1 1 calc R . . C31 C 0.3407(4) -0.11862(15) 0.4166(4) 0.0476(13) Uani 1 1 d . . . H31 H 0.3736 -0.1393 0.4483 0.057 Uiso 1 1 calc R . . C32 C 0.2411(4) -0.11100(14) 0.4248(3) 0.0466(13) Uani 1 1 d . . . H32 H 0.2065 -0.1263 0.4632 0.056 Uiso 1 1 calc R . . C33 C 0.1936(3) -0.08049(13) 0.3756(3) 0.0357(10) Uani 1 1 d . . . H33 H 0.1261 -0.0760 0.3800 0.043 Uiso 1 1 calc R . . C34 C 0.1878(3) 0.13890(14) -0.0699(3) 0.0395(11) Uani 1 1 d . A . H34 H 0.2178 0.1159 -0.0475 0.047 Uiso 1 1 calc R . . C35 C 0.2114(14) 0.1169(6) -0.2241(17) 0.073(6) Uani 0.55 1 d P A 1 H35A H 0.1853 0.1233 -0.2871 0.110 Uiso 0.55 1 calc PR A 1 H35B H 0.1953 0.0904 -0.2117 0.110 Uiso 0.55 1 calc PR A 1 H35C H 0.2829 0.1201 -0.2158 0.110 Uiso 0.55 1 calc PR A 1 C35A C 0.1625(18) 0.1068(7) -0.226(2) 0.073(6) Uani 0.45 1 d P A 2 H35D H 0.1433 0.1151 -0.2887 0.110 Uiso 0.45 1 calc PR A 2 H35E H 0.1144 0.0884 -0.2083 0.110 Uiso 0.45 1 calc PR A 2 H35F H 0.2275 0.0949 -0.2207 0.110 Uiso 0.45 1 calc PR A 2 C36 C 0.1161(5) 0.17696(19) -0.1992(4) 0.080(2) Uani 1 1 d . A . H36A H 0.1049 0.1745 -0.2658 0.119 Uiso 1 1 calc R . . H36B H 0.1571 0.1993 -0.1827 0.119 Uiso 1 1 calc R . . H36C H 0.0529 0.1799 -0.1754 0.119 Uiso 1 1 calc R . . C37 C 0.4491(3) 0.14105(14) 0.1099(3) 0.0389(11) Uani 1 1 d . A . H37 H 0.4749 0.1564 0.1602 0.047 Uiso 1 1 calc R . . C38 C 0.6203(4) 0.1206(2) 0.1022(4) 0.0743(19) Uani 1 1 d . . . H38A H 0.6544 0.1034 0.0645 0.111 Uiso 1 1 calc R . . H38B H 0.6307 0.1121 0.1659 0.111 Uiso 1 1 calc R . . H38C H 0.6462 0.1464 0.0980 0.111 Uiso 1 1 calc R . . C39 C 0.4804(4) 0.0947(2) -0.0068(4) 0.083(2) Uani 1 1 d . . . H39A H 0.5377 0.0819 -0.0265 0.125 Uiso 1 1 calc R . . H39B H 0.4464 0.1092 -0.0578 0.125 Uiso 1 1 calc R . . H39C H 0.4356 0.0756 0.0133 0.125 Uiso 1 1 calc R . . C40 C 0.2579(3) 0.04173(13) 0.4349(3) 0.0302(10) Uani 1 1 d . . . H40 H 0.2019 0.0573 0.4192 0.036 Uiso 1 1 calc R . . C41 C 0.2908(5) 0.07744(18) 0.5807(4) 0.0666(12) Uani 1 1 d . . . H41A H 0.3389 0.0759 0.6356 0.100 Uiso 1 1 calc R . . H41B H 0.2245 0.0741 0.5976 0.100 Uiso 1 1 calc R . . H41C H 0.2957 0.1023 0.5518 0.100 Uiso 1 1 calc R . . C42 C 0.3994(4) 0.02288(19) 0.5439(4) 0.073(2) Uani 1 1 d . . . H42A H 0.4302 0.0306 0.6046 0.110 Uiso 1 1 calc R . . H42B H 0.4465 0.0260 0.4998 0.110 Uiso 1 1 calc R . . H42C H 0.3793 -0.0038 0.5455 0.110 Uiso 1 1 calc R . . C43 C 0.0082(3) 0.02851(14) 0.3194(3) 0.0380(11) Uani 1 1 d . . . H43 H 0.0272 0.0493 0.2845 0.046 Uiso 1 1 calc R . . C44 C -0.1131(5) 0.0008(2) 0.4105(5) 0.079(2) Uani 1 1 d . . . H44A H -0.1753 0.0086 0.4310 0.118 Uiso 1 1 calc R . . H44B H -0.0649 -0.0046 0.4637 0.118 Uiso 1 1 calc R . . H44C H -0.1237 -0.0221 0.3727 0.118 Uiso 1 1 calc R . . C45 C -0.1392(4) 0.06662(18) 0.3410(4) 0.0662(17) Uani 1 1 d . . . H45A H -0.1975 0.0636 0.3725 0.099 Uiso 1 1 calc R . . H45B H -0.1596 0.0700 0.2755 0.099 Uiso 1 1 calc R . . H45C H -0.1021 0.0890 0.3651 0.099 Uiso 1 1 calc R . . C46 C 0.3657(6) 0.1789(2) 0.5828(5) 0.0794(19) Uani 1 1 d . B . H46 H 0.3047 0.1681 0.5934 0.095 Uiso 1 1 calc R . . C47 C 0.4815(9) 0.2325(4) 0.5895(8) 0.0666(12) Uani 0.50 1 d P B 3 H47A H 0.5250 0.2128 0.5703 0.100 Uiso 0.50 1 calc PR B 3 H47B H 0.5023 0.2392 0.6534 0.100 Uiso 0.50 1 calc PR B 3 H47C H 0.4850 0.2551 0.5511 0.100 Uiso 0.50 1 calc PR B 3 C47A C 0.4423(10) 0.2391(4) 0.5461(8) 0.0666(12) Uani 0.50 1 d P B 4 H47D H 0.4143 0.2514 0.4891 0.100 Uiso 0.50 1 calc PR B 4 H47E H 0.4978 0.2231 0.5345 0.100 Uiso 0.50 1 calc PR B 4 H47F H 0.4651 0.2587 0.5912 0.100 Uiso 0.50 1 calc PR B 4 C48 C 0.2832(8) 0.2384(3) 0.6099(7) 0.0666(12) Uani 0.60 1 d P B 5 H48A H 0.2222 0.2257 0.5850 0.100 Uiso 0.60 1 calc PR B 5 H48B H 0.2825 0.2647 0.5877 0.100 Uiso 0.60 1 calc PR B 5 H48C H 0.2887 0.2384 0.6767 0.100 Uiso 0.60 1 calc PR B 5 C48A C 0.2832(12) 0.2417(5) 0.5570(10) 0.0666(12) Uani 0.40 1 d P B 6 H48D H 0.2238 0.2261 0.5548 0.080 Uiso 0.40 1 calc PR B 6 H48E H 0.2854 0.2540 0.4977 0.100 Uiso 0.40 1 calc PR B 6 H48F H 0.2824 0.2613 0.6043 0.100 Uiso 0.40 1 calc PR B 6 C49 C 0.3528(8) 0.3585(3) 0.3473(7) 0.133(4) Uani 1 1 d . . . H49A H 0.4015 0.3786 0.3638 0.200 Uiso 1 1 calc R . . H49B H 0.3209 0.3628 0.2850 0.200 Uiso 1 1 calc R . . H49C H 0.3856 0.3337 0.3507 0.200 Uiso 1 1 calc R . . N1 N 0.1149(2) -0.03045(10) 0.1428(2) 0.0293(8) Uani 1 1 d . . . N2 N 0.3178(2) -0.01535(10) 0.1887(2) 0.0257(8) Uani 1 1 d . . . N3 N 0.2419(2) -0.05706(10) 0.3215(2) 0.0304(8) Uani 1 1 d . . . N4 N -0.0757(3) 0.03188(12) 0.3561(3) 0.0414(10) Uani 1 1 d . . . N5 N 0.3111(3) 0.04723(11) 0.5163(2) 0.0337(9) Uani 1 1 d . . . N6 N 0.0775(3) 0.17184(10) 0.1565(2) 0.0331(9) Uani 1 1 d . . . N7 N 0.2542(2) 0.17210(10) 0.2727(2) 0.0282(8) Uani 1 1 d . . . N8 N 0.2732(3) 0.21829(10) 0.1291(2) 0.0313(8) Uani 1 1 d . . . N9 N 0.1664(4) 0.14256(13) -0.1595(3) 0.0590(13) Uani 1 1 d . . . N10 N 0.5128(3) 0.12045(12) 0.0691(3) 0.0416(10) Uani 1 1 d . . . N11 N 0.3718(4) 0.21714(16) 0.5789(4) 0.0787(16) Uani 1 1 d . . . O1 O 0.16152(19) 0.04753(8) 0.19852(18) 0.0277(6) Uani 1 1 d . . . O2 O 0.0651(2) -0.00042(9) 0.3277(2) 0.0350(7) Uani 1 1 d . . . O3 O 0.2781(2) 0.01697(9) 0.37770(19) 0.0328(7) Uani 1 1 d . . . O4 O 0.1799(2) 0.10505(8) 0.13675(18) 0.0294(7) Uani 1 1 d . . . O5 O 0.1712(2) 0.16377(8) -0.0121(2) 0.0341(7) Uani 1 1 d . . . O6 O 0.3572(2) 0.14180(9) 0.0871(2) 0.0375(7) Uani 1 1 d . . . O7 O 0.2221(6) 0.0060(2) 0.7931(5) 0.0821(10) Uani 0.595(6) 1 d PD C 5 O7A O 0.2671(9) -0.0185(3) 0.8176(7) 0.0821(10) Uani 0.405(6) 1 d PD C 6 O8 O 0.3710(4) 0.03451(15) 0.8022(3) 0.1034(18) Uani 1 1 d . C . O9 O 0.2694(3) 0.03662(14) 0.9216(3) 0.0821(10) Uani 1 1 d . C . O10 O 0.3933(8) -0.0058(3) 0.9195(6) 0.0821(10) Uani 0.532(10) 1 d PD C 7 O10A O 0.3465(10) -0.0232(3) 0.8912(7) 0.0821(10) Uani 0.468(10) 1 d PD C 8 O11 O -0.0548(3) 0.15138(13) 0.4816(3) 0.0672(12) Uani 1 1 d . . . O12 O 0.0686(3) 0.11116(15) 0.4332(3) 0.0869(10) Uani 1 1 d . . . O13 O 0.0297(3) 0.10653(15) 0.5832(3) 0.0869(10) Uani 1 1 d . . . O14 O 0.1157(3) 0.15944(13) 0.5365(3) 0.0916(15) Uani 1 1 d . . . O15 O 0.5953(4) 0.20604(19) 0.2322(3) 0.120(2) Uani 1 1 d . D . O16 O 0.6678(5) 0.16756(17) 0.3506(5) 0.149(3) Uani 1 1 d . D . O17 O 0.7316(3) 0.22695(13) 0.3343(3) 0.0757(12) Uani 1 1 d . D . O18 O 0.5772(10) 0.2269(3) 0.3771(9) 0.073(3) Uani 0.65 1 d PD D 13 O18A O 0.578(2) 0.2077(8) 0.3969(19) 0.111(11) Uani 0.35 1 d PD D 14 O19 O 0.4339(4) 0.15715(15) 0.5734(5) 0.1114(19) Uani 1 1 d . . . O20 O 0.2806(8) 0.3593(3) 0.4093(7) 0.186(3) Uani 1 1 d . . . H20A H 0.2679 0.3370 0.4241 0.279 Uiso 1 1 calc R . . Ni2 Ni 0.22120(4) 0.161643(15) 0.12700(3) 0.02567(16) Uani 1 1 d . A . Ni1 Ni 0.19160(4) -0.005038(15) 0.26005(3) 0.02500(16) Uani 1 1 d . . . Cl1 Cl 0.31372(10) 0.01338(4) 0.85814(8) 0.0470(3) Uani 1 1 d D . . Cl2 Cl 0.03885(9) 0.13233(4) 0.50982(8) 0.0460(3) Uani 1 1 d . . . Cl3 Cl 0.64269(10) 0.20574(5) 0.32533(10) 0.0606(4) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.033(3) 0.040(3) 0.060(3) 0.003(2) -0.001(2) 0.003(2) C2 0.028(3) 0.053(4) 0.097(5) 0.001(3) 0.011(3) 0.002(2) C3 0.034(3) 0.066(4) 0.086(4) 0.012(3) 0.025(3) 0.011(3) C4 0.047(3) 0.050(3) 0.054(3) 0.004(3) 0.024(3) 0.015(2) C5 0.042(3) 0.030(3) 0.040(3) 0.006(2) 0.010(2) 0.012(2) C6 0.048(3) 0.031(3) 0.034(2) -0.004(2) 0.012(2) 0.008(2) C7 0.037(2) 0.029(2) 0.032(2) -0.0066(19) -0.0011(19) -0.0052(19) C8 0.038(3) 0.027(2) 0.034(2) -0.002(2) -0.001(2) -0.0036(19) C9 0.061(3) 0.035(3) 0.045(3) 0.001(2) -0.009(2) -0.012(2) C10 0.067(4) 0.033(3) 0.059(3) 0.008(3) -0.008(3) -0.018(3) C11 0.065(4) 0.030(3) 0.051(3) 0.011(2) -0.004(3) -0.008(2) C12 0.047(3) 0.029(3) 0.040(3) 0.002(2) -0.002(2) -0.003(2) C13 0.036(2) 0.030(2) 0.023(2) -0.0001(18) 0.0051(18) 0.0023(19) C14 0.029(2) 0.024(2) 0.026(2) 0.0041(18) 0.0012(17) -0.0029(17) C15 0.022(2) 0.031(2) 0.019(2) 0.0042(17) -0.0005(16) -0.0059(17) C16 0.021(2) 0.027(2) 0.025(2) -0.0052(18) 0.0035(17) -0.0010(17) C17 0.025(2) 0.026(2) 0.028(2) 0.0030(18) 0.0011(17) -0.0018(17) C18 0.024(2) 0.031(3) 0.045(3) 0.000(2) 0.0052(19) 0.0021(18) C19 0.028(2) 0.039(3) 0.048(3) 0.000(2) -0.007(2) -0.007(2) C20 0.039(3) 0.032(3) 0.031(2) 0.002(2) -0.007(2) -0.005(2) C21 0.026(2) 0.029(2) 0.028(2) 0.0010(18) 0.0059(17) -0.0008(17) C22 0.026(2) 0.031(2) 0.033(2) -0.0113(19) 0.0015(18) -0.0038(18) C23 0.024(2) 0.024(2) 0.037(2) -0.0051(19) 0.0019(18) -0.0012(17) C24 0.038(3) 0.039(3) 0.034(3) -0.010(2) 0.000(2) 0.001(2) C25 0.044(3) 0.039(3) 0.046(3) -0.011(2) -0.010(2) -0.002(2) C26 0.028(2) 0.042(3) 0.047(3) -0.007(2) -0.010(2) -0.005(2) C27 0.024(2) 0.039(3) 0.052(3) -0.004(2) 0.005(2) 0.0004(19) C28 0.020(2) 0.031(2) 0.030(2) -0.0012(19) -0.0005(17) 0.0029(17) C29 0.030(2) 0.024(2) 0.032(2) -0.0025(18) 0.0037(18) -0.0010(17) C30 0.036(3) 0.031(3) 0.052(3) 0.004(2) 0.003(2) 0.006(2) C31 0.048(3) 0.035(3) 0.059(3) 0.013(2) 0.005(2) 0.004(2) C32 0.059(3) 0.037(3) 0.046(3) 0.006(2) 0.017(3) -0.004(2) C33 0.041(3) 0.028(3) 0.040(3) 0.000(2) 0.014(2) -0.004(2) C34 0.049(3) 0.037(3) 0.031(3) 0.001(2) -0.004(2) 0.008(2) C35 0.117(18) 0.042(10) 0.052(4) -0.016(7) -0.023(12) 0.023(9) C35A 0.117(18) 0.042(10) 0.052(4) -0.016(7) -0.023(12) 0.023(9) C36 0.123(6) 0.062(4) 0.047(3) 0.003(3) -0.014(3) 0.045(4) C37 0.034(3) 0.042(3) 0.041(3) -0.004(2) 0.004(2) -0.007(2) C38 0.033(3) 0.104(5) 0.086(4) -0.023(4) 0.009(3) 0.006(3) C39 0.059(4) 0.098(6) 0.094(5) -0.058(4) 0.017(3) -0.003(4) C40 0.033(2) 0.030(2) 0.027(2) 0.0050(19) 0.0022(19) 0.0003(19) C41 0.076(3) 0.064(3) 0.059(3) -0.019(3) 0.003(2) 0.004(2) C42 0.062(4) 0.083(5) 0.066(4) -0.032(3) -0.028(3) 0.038(3) C43 0.035(3) 0.041(3) 0.040(3) -0.010(2) 0.011(2) -0.006(2) C44 0.056(4) 0.110(6) 0.077(4) 0.010(4) 0.029(3) -0.006(4) C45 0.039(3) 0.069(4) 0.091(4) -0.026(3) 0.010(3) 0.014(3) C46 0.074(5) 0.068(5) 0.096(5) -0.001(4) 0.009(4) -0.014(4) C47 0.076(3) 0.064(3) 0.059(3) -0.019(3) 0.003(2) 0.004(2) C47A 0.076(3) 0.064(3) 0.059(3) -0.019(3) 0.003(2) 0.004(2) C48 0.076(3) 0.064(3) 0.059(3) -0.019(3) 0.003(2) 0.004(2) C48A 0.076(3) 0.064(3) 0.059(3) -0.019(3) 0.003(2) 0.004(2) C49 0.156(10) 0.133(9) 0.120(8) -0.023(6) 0.055(7) 0.016(7) N1 0.0246(19) 0.028(2) 0.035(2) -0.0023(16) 0.0018(15) -0.0008(15) N2 0.0243(18) 0.028(2) 0.0245(18) -0.0043(15) 0.0010(14) -0.0021(14) N3 0.0286(19) 0.030(2) 0.033(2) -0.0008(16) 0.0044(15) 0.0001(15) N4 0.030(2) 0.053(3) 0.043(2) -0.010(2) 0.0126(18) 0.0006(18) N5 0.034(2) 0.036(2) 0.030(2) -0.0034(17) 0.0003(16) 0.0074(16) N6 0.033(2) 0.031(2) 0.035(2) 0.0044(17) 0.0027(16) 0.0030(16) N7 0.0318(19) 0.025(2) 0.0287(19) -0.0018(15) 0.0052(15) 0.0012(15) N8 0.037(2) 0.026(2) 0.030(2) -0.0015(16) 0.0028(16) -0.0020(16) N9 0.098(4) 0.050(3) 0.025(2) -0.0067(19) -0.006(2) 0.028(3) N10 0.030(2) 0.049(3) 0.048(2) -0.003(2) 0.0119(18) 0.0025(18) N11 0.087(4) 0.050(3) 0.102(4) -0.017(3) 0.024(3) -0.013(3) O1 0.0211(14) 0.0266(16) 0.0350(16) 0.0018(13) 0.0015(12) -0.0012(12) O2 0.0312(17) 0.0329(18) 0.0430(18) 0.0024(14) 0.0134(14) 0.0030(13) O3 0.0317(16) 0.0364(18) 0.0302(16) -0.0042(14) 0.0035(13) -0.0022(13) O4 0.0270(15) 0.0265(17) 0.0328(16) 0.0039(13) -0.0041(12) -0.0033(12) O5 0.0403(18) 0.0304(18) 0.0309(16) -0.0009(14) 0.0015(13) 0.0009(13) O6 0.0325(18) 0.0405(19) 0.0401(18) 0.0002(15) 0.0065(14) 0.0007(14) O7 0.088(3) 0.093(3) 0.067(2) -0.0016(18) 0.0173(17) 0.0294(19) O7A 0.088(3) 0.093(3) 0.067(2) -0.0016(18) 0.0173(17) 0.0294(19) O8 0.097(4) 0.111(4) 0.116(4) 0.053(3) 0.068(3) 0.023(3) O9 0.088(3) 0.093(3) 0.067(2) -0.0016(18) 0.0173(17) 0.0294(19) O10 0.088(3) 0.093(3) 0.067(2) -0.0016(18) 0.0173(17) 0.0294(19) O10A 0.088(3) 0.093(3) 0.067(2) -0.0016(18) 0.0173(17) 0.0294(19) O11 0.052(2) 0.087(3) 0.067(3) 0.016(2) 0.0242(19) 0.030(2) O12 0.0585(19) 0.118(3) 0.085(2) 0.022(2) 0.0138(16) 0.0068(18) O13 0.0585(19) 0.118(3) 0.085(2) 0.022(2) 0.0138(16) 0.0068(18) O14 0.074(3) 0.082(4) 0.116(4) -0.018(3) 0.004(3) -0.033(3) O15 0.100(4) 0.173(6) 0.079(3) -0.046(3) -0.026(3) -0.009(4) O16 0.153(6) 0.073(4) 0.216(7) 0.027(4) 0.007(5) -0.031(4) O17 0.061(3) 0.084(3) 0.082(3) -0.019(2) 0.009(2) -0.025(2) O18 0.052(5) 0.106(9) 0.065(5) -0.016(6) 0.023(4) -0.003(6) O18A 0.100(14) 0.15(3) 0.098(18) -0.045(17) 0.054(13) -0.030(18) O19 0.071(3) 0.075(4) 0.187(6) -0.014(4) 0.012(3) 0.011(3) O20 0.210(9) 0.185(8) 0.166(7) 0.003(7) 0.034(6) -0.056(7) Ni2 0.0258(3) 0.0251(3) 0.0257(3) -0.0005(2) 0.0018(2) -0.0005(2) Ni1 0.0227(3) 0.0264(3) 0.0261(3) -0.0015(2) 0.0040(2) -0.0004(2) Cl1 0.0519(8) 0.0525(8) 0.0379(7) -0.0017(6) 0.0109(6) 0.0041(6) Cl2 0.0378(7) 0.0577(8) 0.0437(7) 0.0042(6) 0.0092(5) -0.0012(6) Cl3 0.0473(8) 0.0737(11) 0.0598(9) -0.0199(8) 0.0023(7) -0.0134(7) _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 N6 1.349(6) . ? C1 C2 1.372(7) . ? C1 H1 0.9300 . ? C2 C3 1.378(8) . ? C2 H2 0.9300 . ? C3 C4 1.353(8) . ? C3 H3 0.9300 . ? C4 C5 1.392(6) . ? C4 H4 0.9300 . ? C5 N6 1.352(5) . ? C5 C6 1.487(6) . ? C6 N7 1.509(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N7 1.492(5) . ? C7 C8 1.516(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N8 1.343(5) . ? C8 C9 1.387(6) . ? C9 C10 1.379(7) . ? C9 H9 0.9300 . ? C10 C11 1.362(7) . ? C10 H10 0.9300 . ? C11 C12 1.378(6) . ? C11 H11 0.9300 . ? C12 N8 1.340(5) . ? C12 H12 0.9300 . ? C13 N7 1.484(5) . ? C13 C14 1.502(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C20 1.395(6) . ? C14 C15 1.405(5) . ? C15 C17 1.398(5) . ? C15 C16 1.515(5) . ? C16 O4 1.245(5) . ? C16 O1 1.267(5) . ? C17 C18 1.409(5) . ? C17 C21 1.512(5) . ? C18 C19 1.369(6) . ? C18 H18 0.9300 . ? C19 C20 1.394(6) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 N2 1.498(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N2 1.494(5) . ? C22 C23 1.515(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N1 1.346(5) . ? C23 C24 1.390(6) . ? C24 C25 1.380(6) . ? C24 H24 0.9300 . ? C25 C26 1.382(7) . ? C25 H25 0.9300 . ? C26 C27 1.385(6) . ? C26 H26 0.9300 . ? C27 N1 1.338(5) . ? C27 H27 0.9300 . ? C28 N2 1.485(5) . ? C28 C29 1.510(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 N3 1.351(5) . ? C29 C30 1.385(6) . ? C30 C31 1.387(6) . ? C30 H30 0.9300 . ? C31 C32 1.383(7) . ? C31 H31 0.9300 . ? C32 C33 1.381(6) . ? C32 H32 0.9300 . ? C33 N3 1.347(5) . ? C33 H33 0.9300 . ? C34 O5 1.237(5) . ? C34 N9 1.297(5) . ? C34 H34 0.9300 . ? C35 N9 1.47(2) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C35A N9 1.56(3) . ? C35A H35D 0.9600 . ? C35A H35E 0.9600 . ? C35A H35F 0.9600 . ? C36 N9 1.447(7) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 O6 1.237(5) . ? C37 N10 1.308(6) . ? C37 H37 0.9300 . ? C38 N10 1.464(6) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 N10 1.436(6) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 O3 1.242(5) . ? C40 N5 1.312(5) . ? C40 H40 0.9300 . ? C41 N5 1.446(6) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 N5 1.468(6) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 O2 1.252(5) . ? C43 N4 1.310(5) . ? C43 H43 0.9300 . ? C44 N4 1.455(7) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 N4 1.471(6) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 O19 1.205(8) . ? C46 N11 1.321(8) . ? C46 H46 0.9300 . ? C47 N11 1.557(13) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C47A N11 1.345(14) . ? C47A H47D 0.9600 . ? C47A H47E 0.9600 . ? C47A H47F 0.9600 . ? C48 N11 1.513(11) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C48A N11 1.463(16) . ? C48A H48D 0.9600 . ? C48A H48E 0.9600 . ? C48A H48F 0.9600 . ? C49 O20 1.401(10) . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? N1 Ni1 2.066(3) . ? N2 Ni1 2.122(3) . ? N3 Ni1 2.076(3) . ? N6 Ni2 2.060(3) . ? N7 Ni2 2.130(3) . ? N8 Ni2 2.072(3) . ? O1 Ni1 2.036(3) . ? O2 Ni1 2.071(3) . ? O3 Ni1 2.080(3) . ? O4 Ni2 2.037(3) . ? O5 Ni2 2.041(3) . ? O6 Ni2 2.099(3) . ? O7 Cl1 1.475(7) . ? O7A Cl1 1.362(11) . ? O8 Cl1 1.391(4) . ? O9 Cl1 1.405(4) . ? O10 Cl1 1.459(8) . ? O10A Cl1 1.400(9) . ? O11 Cl2 1.433(4) . ? O12 Cl2 1.425(5) . ? O13 Cl2 1.401(4) . ? O14 Cl2 1.411(4) . ? O15 Cl3 1.416(5) . ? O16 Cl3 1.395(6) . ? O17 Cl3 1.392(4) . ? O18 Cl3 1.425(8) . ? O18A Cl3 1.431(14) . ? O20 H20A 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 C1 C2 121.7(5) . . ? N6 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C1 C2 C3 119.3(5) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 119.4(5) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 119.8(5) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N6 C5 C4 120.8(4) . . ? N6 C5 C6 115.5(4) . . ? C4 C5 C6 123.7(4) . . ? C5 C6 N7 111.4(3) . . ? C5 C6 H6A 109.3 . . ? N7 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? N7 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? N7 C7 C8 108.7(3) . . ? N7 C7 H7A 110.0 . . ? C8 C7 H7A 110.0 . . ? N7 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? H7A C7 H7B 108.3 . . ? N8 C8 C9 122.0(4) . . ? N8 C8 C7 116.1(4) . . ? C9 C8 C7 121.9(4) . . ? C10 C9 C8 118.1(4) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? C11 C10 C9 120.0(5) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 119.2(5) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? N8 C12 C11 121.9(4) . . ? N8 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? N7 C13 C14 115.3(3) . . ? N7 C13 H13A 108.5 . . ? C14 C13 H13A 108.5 . . ? N7 C13 H13B 108.5 . . ? C14 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? C20 C14 C15 119.0(4) . . ? C20 C14 C13 119.9(4) . . ? C15 C14 C13 121.0(3) . . ? C17 C15 C14 120.4(3) . . ? C17 C15 C16 119.5(3) . . ? C14 C15 C16 120.1(3) . . ? O4 C16 O1 122.3(3) . . ? O4 C16 C15 119.6(3) . . ? O1 C16 C15 118.1(3) . . ? C15 C17 C18 118.9(4) . . ? C15 C17 C21 121.8(3) . . ? C18 C17 C21 119.3(4) . . ? C19 C18 C17 121.0(4) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 119.9(4) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C19 C20 C14 120.8(4) . . ? C19 C20 H20 119.6 . . ? C14 C20 H20 119.6 . . ? N2 C21 C17 114.1(3) . . ? N2 C21 H21A 108.7 . . ? C17 C21 H21A 108.7 . . ? N2 C21 H21B 108.7 . . ? C17 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? N2 C22 C23 113.1(3) . . ? N2 C22 H22A 109.0 . . ? C23 C22 H22A 109.0 . . ? N2 C22 H22B 109.0 . . ? C23 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? N1 C23 C24 122.2(4) . . ? N1 C23 C22 116.5(3) . . ? C24 C23 C22 121.0(4) . . ? C25 C24 C23 119.2(4) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C24 C25 C26 118.8(4) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? C25 C26 C27 118.8(4) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? N1 C27 C26 123.0(4) . . ? N1 C27 H27 118.5 . . ? C26 C27 H27 118.5 . . ? N2 C28 C29 110.8(3) . . ? N2 C28 H28A 109.5 . . ? C29 C28 H28A 109.5 . . ? N2 C28 H28B 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? N3 C29 C30 121.8(4) . . ? N3 C29 C28 115.9(3) . . ? C30 C29 C28 122.2(4) . . ? C29 C30 C31 119.2(4) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C32 C31 C30 118.8(4) . . ? C32 C31 H31 120.6 . . ? C30 C31 H31 120.6 . . ? C33 C32 C31 119.4(4) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? N3 C33 C32 122.0(4) . . ? N3 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? O5 C34 N9 124.9(4) . . ? O5 C34 H34 117.6 . . ? N9 C34 H34 117.6 . . ? N9 C35 H35A 109.5 . . ? N9 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N9 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N9 C35A H35D 109.5 . . ? N9 C35A H35E 109.5 . . ? H35D C35A H35E 109.5 . . ? N9 C35A H35F 109.5 . . ? H35D C35A H35F 109.5 . . ? H35E C35A H35F 109.5 . . ? N9 C36 H36A 109.5 . . ? N9 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N9 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O6 C37 N10 125.3(4) . . ? O6 C37 H37 117.3 . . ? N10 C37 H37 117.3 . . ? N10 C38 H38A 109.5 . . ? N10 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N10 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N10 C39 H39A 109.5 . . ? N10 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N10 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O3 C40 N5 123.9(4) . . ? O3 C40 H40 118.0 . . ? N5 C40 H40 118.0 . . ? N5 C41 H41A 109.5 . . ? N5 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N5 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N5 C42 H42A 109.5 . . ? N5 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N5 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O2 C43 N4 125.3(5) . . ? O2 C43 H43 117.4 . . ? N4 C43 H43 117.4 . . ? N4 C44 H44A 109.5 . . ? N4 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N4 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N4 C45 H45A 109.5 . . ? N4 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N4 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O19 C46 N11 124.3(7) . . ? O19 C46 H46 117.8 . . ? N11 C46 H46 117.8 . . ? N11 C47 H47A 109.5 . . ? N11 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N11 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N11 C47A H47D 109.5 . . ? N11 C47A H47E 109.5 . . ? H47D C47A H47E 109.5 . . ? N11 C47A H47F 109.5 . . ? H47D C47A H47F 109.5 . . ? H47E C47A H47F 109.5 . . ? N11 C48 H48A 109.5 . . ? N11 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N11 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N11 C48A H48D 109.5 . . ? N11 C48A H48E 109.5 . . ? H48D C48A H48E 109.5 . . ? N11 C48A H48F 109.5 . . ? H48D C48A H48F 109.5 . . ? H48E C48A H48F 109.5 . . ? O20 C49 H49A 109.5 . . ? O20 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? O20 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C27 N1 C23 118.0(4) . . ? C27 N1 Ni1 127.7(3) . . ? C23 N1 Ni1 114.0(3) . . ? C28 N2 C22 108.8(3) . . ? C28 N2 C21 111.3(3) . . ? C22 N2 C21 108.8(3) . . ? C28 N2 Ni1 104.3(2) . . ? C22 N2 Ni1 107.2(2) . . ? C21 N2 Ni1 116.2(2) . . ? C33 N3 C29 118.8(4) . . ? C33 N3 Ni1 127.7(3) . . ? C29 N3 Ni1 112.8(3) . . ? C43 N4 C44 121.8(5) . . ? C43 N4 C45 121.7(4) . . ? C44 N4 C45 116.5(4) . . ? C40 N5 C41 123.9(4) . . ? C40 N5 C42 119.5(4) . . ? C41 N5 C42 116.5(4) . . ? C1 N6 C5 118.9(4) . . ? C1 N6 Ni2 124.6(3) . . ? C5 N6 Ni2 114.8(3) . . ? C13 N7 C7 112.0(3) . . ? C13 N7 C6 108.8(3) . . ? C7 N7 C6 109.1(3) . . ? C13 N7 Ni2 115.0(2) . . ? C7 N7 Ni2 105.5(2) . . ? C6 N7 Ni2 106.1(2) . . ? C12 N8 C8 118.8(4) . . ? C12 N8 Ni2 126.7(3) . . ? C8 N8 Ni2 114.1(3) . . ? C34 N9 C36 120.7(4) . . ? C34 N9 C35 121.3(10) . . ? C36 N9 C35 116.7(10) . . ? C34 N9 C35A 121.5(12) . . ? C36 N9 C35A 115.2(11) . . ? C35 N9 C35A 28.1(13) . . ? C37 N10 C39 121.8(4) . . ? C37 N10 C38 121.7(4) . . ? C39 N10 C38 116.4(4) . . ? C46 N11 C47A 128.8(8) . . ? C46 N11 C48A 122.2(9) . . ? C47A N11 C48A 100.7(10) . . ? C46 N11 C48 114.6(7) . . ? C47A N11 C48 116.5(8) . . ? C48A N11 C48 30.1(6) . . ? C46 N11 C47 113.5(7) . . ? C47A N11 C47 30.9(6) . . ? C48A N11 C47 124.0(9) . . ? C48 N11 C47 125.2(7) . . ? C16 O1 Ni1 134.5(3) . . ? C43 O2 Ni1 122.9(3) . . ? C40 O3 Ni1 130.5(3) . . ? C16 O4 Ni2 133.4(2) . . ? C34 O5 Ni2 125.2(3) . . ? C37 O6 Ni2 143.9(3) . . ? C49 O20 H20A 109.5 . . ? O4 Ni2 O5 92.50(11) . . ? O4 Ni2 N6 83.00(13) . . ? O5 Ni2 N6 89.80(13) . . ? O4 Ni2 N8 174.25(12) . . ? O5 Ni2 N8 92.84(12) . . ? N6 Ni2 N8 99.17(14) . . ? O4 Ni2 O6 87.80(12) . . ? O5 Ni2 O6 86.09(12) . . ? N6 Ni2 O6 169.75(13) . . ? N8 Ni2 O6 90.41(13) . . ? O4 Ni2 N7 96.80(12) . . ? O5 Ni2 N7 166.32(12) . . ? N6 Ni2 N7 81.42(13) . . ? N8 Ni2 N7 78.34(13) . . ? O6 Ni2 N7 104.23(12) . . ? O1 Ni1 N1 88.09(12) . . ? O1 Ni1 O2 90.47(11) . . ? N1 Ni1 O2 93.78(12) . . ? O1 Ni1 N3 172.47(12) . . ? N1 Ni1 N3 95.04(13) . . ? O2 Ni1 N3 96.14(12) . . ? O1 Ni1 O3 95.36(11) . . ? N1 Ni1 O3 175.16(13) . . ? O2 Ni1 O3 89.59(12) . . ? N3 Ni1 O3 81.13(12) . . ? O1 Ni1 N2 93.64(12) . . ? N1 Ni1 N2 82.93(12) . . ? O2 Ni1 N2 174.63(12) . . ? N3 Ni1 N2 79.99(13) . . ? O3 Ni1 N2 93.45(11) . . ? O7A Cl1 O8 115.5(5) . . ? O7A Cl1 O10A 61.8(7) . . ? O8 Cl1 O10A 119.8(5) . . ? O7A Cl1 O9 122.1(5) . . ? O8 Cl1 O9 113.1(3) . . ? O10A Cl1 O9 115.5(4) . . ? O7A Cl1 O10 99.1(7) . . ? O8 Cl1 O10 100.0(5) . . ? O10A Cl1 O10 37.7(5) . . ? O9 Cl1 O10 101.5(4) . . ? O7A Cl1 O7 44.3(5) . . ? O8 Cl1 O7 101.4(4) . . ? O10A Cl1 O7 105.4(7) . . ? O9 Cl1 O7 97.3(3) . . ? O10 Cl1 O7 143.1(6) . . ? O13 Cl2 O14 110.1(3) . . ? O13 Cl2 O12 108.9(3) . . ? O14 Cl2 O12 106.6(3) . . ? O13 Cl2 O11 110.4(2) . . ? O14 Cl2 O11 111.2(3) . . ? O12 Cl2 O11 109.6(2) . . ? O17 Cl3 O16 107.1(3) . . ? O17 Cl3 O15 111.3(3) . . ? O16 Cl3 O15 108.8(4) . . ? O17 Cl3 O18 105.1(6) . . ? O16 Cl3 O18 119.4(6) . . ? O15 Cl3 O18 105.2(7) . . ? O17 Cl3 O18A 119.8(14) . . ? O16 Cl3 O18A 90.1(11) . . ? O15 Cl3 O18A 116.6(15) . . ? O18 Cl3 O18A 29.3(12) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.812 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.111 # Attachment '2.cif' data_5780 _database_code_depnum_ccdc_archive 'CCDC 667938' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H36 N10 Ni2 O12' _chemical_formula_sum 'C35 H36 N10 Ni2 O12' _chemical_formula_weight 906.16 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' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6704(4) _cell_length_b 14.8713(6) _cell_length_c 15.0500(8) _cell_angle_alpha 81.222(2) _cell_angle_beta 82.826(2) _cell_angle_gamma 89.510(2) _cell_volume 1902.70(15) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 27775 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.35 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.868 _exptl_absorpt_correction_T_max 0.9553 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28591 _diffrn_reflns_av_R_equivalents 0.1140 _diffrn_reflns_av_sigmaI/netI 0.1170 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.28 _reflns_number_total 6865 _reflns_number_gt 3814 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (O & Mr 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material 'SHELXTL, Bruker' _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. 32 SADI restraints were used because of the disorder of a pyridyl side arm and a nitrate anion. ; _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^)+(0.1032P)^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 6865 _refine_ls_number_parameters 571 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.1394 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.1979 _refine_ls_wR_factor_gt 0.1682 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 0.19796(8) 0.39335(5) 0.14897(5) 0.0438(3) Uani 1 1 d . . . Ni2 Ni -0.02907(9) 0.76236(5) 0.22903(5) 0.0503(3) Uani 1 1 d D . . O3 O 0.3171(5) 0.2792(3) 0.0972(3) 0.0575(11) Uani 1 1 d . . . O2 O 0.2973(5) 0.4099(3) 0.0144(3) 0.0565(11) Uani 1 1 d . . . O4 O 0.4288(6) 0.3013(4) -0.0425(4) 0.0794(15) Uani 1 1 d . . . O1 O 0.0989(5) 0.5158(2) 0.1430(3) 0.0488(10) Uani 1 1 d . A . O5 O 0.0021(5) 0.6449(3) 0.1755(3) 0.0587(12) Uani 1 1 d . A . O6 O -0.0914(6) 0.6907(3) 0.3640(3) 0.0665(13) Uani 1 1 d . A . O7 O -0.2709(6) 0.7339(4) 0.2720(6) 0.108(2) Uani 1 1 d . A . O8 O -0.3377(7) 0.6697(5) 0.4186(5) 0.111(2) Uani 1 1 d . A . N1 N -0.0100(5) 0.3395(3) 0.1307(3) 0.0469(12) Uani 1 1 d . . . N2 N 0.1250(5) 0.3420(3) 0.2825(3) 0.0461(12) Uani 1 1 d . . . N3 N 0.3943(5) 0.4247(3) 0.2001(3) 0.0455(12) Uani 1 1 d . . . N4 N 0.3511(6) 0.3286(4) 0.0209(4) 0.0569(14) Uani 1 1 d . . . N5 N -0.2380(11) 0.6971(5) 0.3618(6) 0.099(2) Uani 1 1 d . . . N7 N 0.2053(6) 0.7910(3) 0.2261(4) 0.0560(14) Uani 1 1 d D A . N8 N -0.0441(6) 0.8795(3) 0.2877(4) 0.0548(14) Uani 1 1 d . A . N10 N 0.7298(11) 0.2062(6) 0.4610(5) 0.105(3) Uani 1 1 d . . . C1 C -0.0917(7) 0.3609(4) 0.0602(4) 0.0498(15) Uani 1 1 d . . . H1 H -0.0462 0.4005 0.0072 0.060 Uiso 1 1 d R . . C2 C -0.2412(7) 0.3273(4) 0.0620(5) 0.0540(16) Uani 1 1 d . . . H2 H -0.2960 0.3433 0.0103 0.065 Uiso 1 1 d R . . C3 C -0.3070(8) 0.2703(4) 0.1379(5) 0.0578(17) Uani 1 1 d . . . H3 H -0.4101 0.2463 0.1403 0.069 Uiso 1 1 d R . . C4 C -0.2241(7) 0.2494(4) 0.2100(5) 0.0566(17) Uani 1 1 d . . . H4 H -0.2699 0.2109 0.2637 0.068 Uiso 1 1 d R . . C5 C -0.0738(7) 0.2836(4) 0.2043(4) 0.0486(15) Uani 1 1 d . . . C6 C 0.0292(7) 0.2604(4) 0.2780(4) 0.0522(16) Uani 1 1 d . . . H6A H 0.0966 0.2109 0.2662 0.063 Uiso 1 1 d R . . H6B H -0.0334 0.2442 0.3355 0.063 Uiso 1 1 d R . . C7 C 0.2702(7) 0.3171(4) 0.3238(4) 0.0552(17) Uani 1 1 d . . . H7A H 0.2490 0.3136 0.3884 0.066 Uiso 1 1 d R . . H7B H 0.3035 0.2588 0.3092 0.066 Uiso 1 1 d R . . C8 C 0.3982(7) 0.3865(4) 0.2874(4) 0.0466(15) Uani 1 1 d . . . C9 C 0.5110(7) 0.4093(5) 0.3375(5) 0.0560(17) Uani 1 1 d . . . H9 H 0.5085 0.3801 0.3991 0.067 Uiso 1 1 d R . . C10 C 0.6227(8) 0.4726(5) 0.2972(5) 0.0629(19) Uani 1 1 d . . . H10 H 0.7006 0.4905 0.3313 0.075 Uiso 1 1 d R . . C11 C 0.6235(7) 0.5096(4) 0.2070(5) 0.0559(17) Uani 1 1 d . . . H11 H 0.7044 0.5515 0.1776 0.067 Uiso 1 1 d R . . C12 C 0.5058(7) 0.4854(4) 0.1619(4) 0.0545(16) Uani 1 1 d . . . H12 H 0.5037 0.5126 0.1000 0.065 Uiso 1 1 d R . . C13 C 0.0246(7) 0.4065(4) 0.3318(4) 0.0546(17) Uani 1 1 d . . . H13A H -0.0567 0.4282 0.2965 0.065 Uiso 1 1 d R . . H13B H -0.0202 0.3742 0.3893 0.065 Uiso 1 1 d R . . C14 C 0.1155(6) 0.4878(4) 0.3480(4) 0.0487(15) Uani 1 1 d . . . C15 C 0.1527(7) 0.5633(4) 0.2820(4) 0.0439(14) Uani 1 1 d . A . C16 C 0.0800(7) 0.5750(4) 0.1941(4) 0.0440(14) Uani 1 1 d . . . C17 C 0.2552(7) 0.6307(4) 0.2961(4) 0.0495(15) Uani 1 1 d . . . C18 C 0.3070(7) 0.7097(4) 0.2230(5) 0.0611(18) Uani 1 1 d . A . H18A H 0.3083 0.6895 0.1653 0.073 Uiso 1 1 d R . . H18B H 0.4105 0.7264 0.2311 0.073 Uiso 1 1 d R . . C19 C 0.3136(8) 0.6225(5) 0.3791(5) 0.0644(19) Uani 1 1 d . A . H19 H 0.3881 0.6656 0.3901 0.077 Uiso 1 1 d R . . C20 C 0.2670(9) 0.5511(5) 0.4465(5) 0.069(2) Uani 1 1 d . . . H20 H 0.3008 0.5482 0.5052 0.083 Uiso 1 1 d R A . C21 C 0.1690(8) 0.4855(5) 0.4314(5) 0.0589(17) Uani 1 1 d . A . H21 H 0.1379 0.4357 0.4786 0.071 Uiso 1 1 d R . . N6 N -0.0183(13) 0.8296(15) 0.1024(7) 0.056(3) Uani 0.660(6) 1 d PD A 3 C22 C -0.1331(12) 0.8330(7) 0.0486(7) 0.054(2) Uani 0.660(6) 1 d PD A 3 H22A H -0.2308 0.8080 0.0710 0.065 Uiso 0.660(6) 1 calc PR A 3 C23 C -0.1007(17) 0.8752(8) -0.0418(7) 0.073(4) Uani 0.660(6) 1 d PD A 3 H23A H -0.1781 0.8790 -0.0797 0.087 Uiso 0.660(6) 1 calc PR A 3 C24 C 0.0441(16) 0.9107(11) -0.0746(11) 0.080(5) Uani 0.660(6) 1 d PD A 3 H24A H 0.0661 0.9375 -0.1348 0.096 Uiso 0.660(6) 1 calc PR A 3 C25 C 0.1560(17) 0.9063(9) -0.0174(9) 0.077(4) Uani 0.660(6) 1 d PD A 3 H25A H 0.2545 0.9309 -0.0382 0.092 Uiso 0.660(6) 1 calc PR A 3 C26 C 0.1210(14) 0.8645(12) 0.0721(8) 0.052(3) Uani 0.660(6) 1 d PD A 3 C27 C 0.2349(12) 0.8626(8) 0.1406(7) 0.054(2) Uani 0.660(6) 1 d PD A 3 H27A H 0.2357 0.9222 0.1594 0.065 Uiso 0.660(6) 1 calc PR A 3 H27B H 0.3379 0.8529 0.1104 0.065 Uiso 0.660(6) 1 calc PR A 3 N6A N 0.042(3) 0.832(3) 0.1014(15) 0.056(3) Uani 0.340(6) 1 d PD A 4 C22A C -0.046(2) 0.8431(13) 0.0289(14) 0.054(2) Uani 0.340(6) 1 d PD A 4 H22B H -0.1464 0.8191 0.0381 0.065 Uiso 0.340(6) 1 calc PR A 4 C23A C 0.011(4) 0.889(3) -0.0572(19) 0.073(4) Uani 0.340(6) 1 d PD A 4 H23B H -0.0553 0.8999 -0.1016 0.087 Uiso 0.340(6) 1 calc PR A 4 C24A C 0.161(3) 0.9185(19) -0.0768(18) 0.080(5) Uani 0.340(6) 1 d PD A 4 H24B H 0.2004 0.9451 -0.1351 0.096 Uiso 0.340(6) 1 calc PR A 4 C25A C 0.253(3) 0.908(2) -0.0083(16) 0.077(4) Uani 0.340(6) 1 d PD A 4 H25B H 0.3549 0.9286 -0.0184 0.092 Uiso 0.340(6) 1 calc PR A 4 C26A C 0.188(3) 0.864(3) 0.0774(16) 0.052(3) Uani 0.340(6) 1 d PD A 4 C27A C 0.292(2) 0.8555(16) 0.1524(14) 0.054(2) Uani 0.340(6) 1 d PD A 4 H27C H 0.3931 0.8315 0.1327 0.065 Uiso 0.340(6) 1 calc PR A 4 H27D H 0.3069 0.9139 0.1717 0.065 Uiso 0.340(6) 1 calc PR A 4 C28 C 0.2151(8) 0.8301(5) 0.3098(5) 0.0656(19) Uani 1 1 d . . . H28A H 0.2078 0.7818 0.3604 0.079 Uiso 1 1 d R A . H28B H 0.3133 0.8610 0.3044 0.079 Uiso 1 1 d R . . C29 C 0.0836(8) 0.8977(4) 0.3226(4) 0.0525(16) Uani 1 1 d . A . C30 C 0.0960(9) 0.9703(5) 0.3692(5) 0.070(2) Uani 1 1 d . . . H30 H 0.1923 0.9812 0.3912 0.084 Uiso 1 1 d R A . C31 C -0.0326(9) 1.0247(5) 0.3804(5) 0.067(2) Uani 1 1 d . A . H31 H -0.0295 1.0750 0.4133 0.080 Uiso 1 1 d R . . C32 C -0.1628(9) 1.0073(5) 0.3456(5) 0.0655(19) Uani 1 1 d . . . H32 H -0.2519 1.0454 0.3535 0.079 Uiso 1 1 d R A . C33 C -0.1676(8) 0.9349(4) 0.2981(5) 0.0589(17) Uani 1 1 d . A . H33 H -0.2609 0.9234 0.2732 0.071 Uiso 1 1 d R . . C34 C 0.6117(12) 0.1729(5) 0.4826(5) 0.077(2) Uani 1 1 d . . . C35 C 0.4621(11) 0.1311(7) 0.5095(8) 0.121(4) Uani 1 1 d . . . H35A H 0.4215 0.1131 0.4583 0.145 Uiso 1 1 d R . . H35B H 0.3927 0.1735 0.5354 0.145 Uiso 1 1 d R . . H35C H 0.4720 0.0785 0.5540 0.145 Uiso 1 1 d R . . N9 N 0.4210(11) 0.0577(9) 0.2627(8) 0.070(3) Uani 0.660(6) 1 d PD A 1 O9 O 0.5024(12) -0.0014(7) 0.2337(11) 0.136(5) Uani 0.660(6) 1 d PD A 1 O10 O 0.4544(17) 0.1096(14) 0.3118(12) 0.166(7) Uani 0.660(6) 1 d PD A 1 O11 O 0.3179(15) 0.0897(10) 0.2203(10) 0.156(5) Uani 0.660(6) 1 d PD A 1 N9A N 0.473(3) 0.062(2) 0.2540(18) 0.070(3) Uani 0.340(6) 1 d PD A 2 O9A O 0.479(2) 0.0064(15) 0.3224(19) 0.136(5) Uani 0.340(6) 1 d PD A 2 O10A O 0.391(4) 0.127(3) 0.266(3) 0.166(7) Uani 0.340(6) 1 d PD A 2 O11A O 0.443(3) 0.0505(19) 0.1790(19) 0.156(5) Uani 0.340(6) 1 d PD A 2 O12 O 0.390(2) 0.0970(13) 0.8707(18) 0.233(11) Uani 0.50 1 d PD . . H12A H 0.4090 0.1493 0.8772 0.350 Uiso 0.50 1 calc PRD . . H12B H 0.3941 0.0931 0.8140 0.350 Uiso 0.50 1 d PRD . . O13 O 0.572(3) 0.9108(14) -0.0446(15) 0.225(10) Uani 0.50 1 d P . . H13C H 0.5641 0.8700 -0.0010 0.337 Uiso 0.50 1 calc PR . . H13D H 0.5490 0.8711 -0.0775 0.337 Uiso 0.50 1 d PR . . 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 0.0431(5) 0.0478(5) 0.0399(5) -0.0056(3) -0.0049(3) 0.0030(3) Ni2 0.0567(5) 0.0435(5) 0.0539(5) -0.0101(4) -0.0161(4) 0.0015(4) O3 0.052(3) 0.060(3) 0.060(3) -0.008(2) -0.007(2) 0.008(2) O2 0.057(3) 0.068(3) 0.044(3) -0.011(2) 0.001(2) -0.009(2) O4 0.072(3) 0.099(4) 0.072(3) -0.047(3) 0.014(3) 0.000(3) O1 0.067(3) 0.041(2) 0.040(2) -0.009(2) -0.013(2) 0.005(2) O5 0.079(3) 0.042(2) 0.060(3) -0.006(2) -0.032(2) 0.005(2) O6 0.053(3) 0.059(3) 0.089(4) 0.005(2) -0.031(3) -0.003(2) O7 0.056(3) 0.062(3) 0.220(8) -0.043(4) -0.043(4) 0.005(3) O8 0.080(4) 0.148(6) 0.094(5) 0.004(4) 0.001(4) -0.001(4) N1 0.050(3) 0.048(3) 0.041(3) -0.004(2) 0.001(2) -0.005(2) N2 0.043(3) 0.052(3) 0.041(3) -0.002(2) -0.002(2) 0.004(2) N3 0.036(3) 0.051(3) 0.051(3) -0.012(2) -0.003(2) 0.004(2) N4 0.049(3) 0.063(4) 0.062(4) -0.017(3) -0.007(3) -0.006(3) N5 0.113(7) 0.066(5) 0.104(6) 0.027(4) -0.012(6) 0.002(4) N7 0.063(3) 0.053(3) 0.052(3) -0.018(3) 0.003(3) -0.009(3) N8 0.064(4) 0.044(3) 0.058(4) -0.007(3) -0.013(3) -0.003(3) N10 0.118(6) 0.120(6) 0.071(5) -0.024(4) 0.018(5) -0.015(5) C1 0.052(4) 0.051(4) 0.045(4) -0.004(3) -0.008(3) 0.007(3) C2 0.044(4) 0.059(4) 0.065(5) -0.018(4) -0.021(3) 0.007(3) C3 0.049(4) 0.061(4) 0.064(5) -0.013(4) -0.008(4) 0.002(3) C4 0.055(4) 0.049(4) 0.062(5) -0.006(3) 0.003(4) -0.001(3) C5 0.044(4) 0.045(3) 0.057(4) -0.009(3) -0.003(3) 0.005(3) C6 0.052(4) 0.048(4) 0.054(4) 0.000(3) -0.006(3) 0.005(3) C7 0.049(4) 0.066(4) 0.048(4) -0.003(3) -0.005(3) 0.014(3) C8 0.048(4) 0.058(4) 0.034(4) -0.007(3) -0.008(3) 0.018(3) C9 0.051(4) 0.070(4) 0.049(4) -0.012(3) -0.013(3) 0.014(4) C10 0.047(4) 0.093(5) 0.059(5) -0.033(4) -0.019(3) 0.018(4) C11 0.040(4) 0.068(4) 0.065(5) -0.029(4) -0.004(3) 0.003(3) C12 0.055(4) 0.070(4) 0.041(4) -0.020(3) -0.005(3) -0.001(3) C13 0.055(4) 0.060(4) 0.043(4) 0.002(3) 0.005(3) 0.008(3) C14 0.038(3) 0.069(4) 0.039(4) -0.011(3) -0.002(3) 0.013(3) C15 0.042(3) 0.053(4) 0.039(3) -0.011(3) -0.006(3) 0.013(3) C16 0.045(3) 0.042(4) 0.043(4) 0.001(3) -0.009(3) -0.002(3) C17 0.041(3) 0.066(4) 0.046(4) -0.020(3) -0.009(3) 0.010(3) C18 0.048(4) 0.069(4) 0.070(5) -0.032(4) 0.002(3) -0.007(3) C19 0.054(4) 0.087(5) 0.065(5) -0.039(4) -0.023(4) 0.021(4) C20 0.083(5) 0.084(5) 0.048(4) -0.021(4) -0.022(4) 0.035(4) C21 0.058(4) 0.066(4) 0.051(4) -0.007(3) -0.004(3) 0.025(4) N6 0.081(10) 0.037(3) 0.057(4) -0.010(3) -0.037(6) 0.011(9) C22 0.045(6) 0.043(3) 0.074(5) -0.011(3) -0.004(4) -0.004(4) C23 0.128(13) 0.043(6) 0.052(7) -0.014(5) -0.023(9) 0.016(9) C24 0.120(13) 0.061(9) 0.050(7) 0.006(6) 0.005(10) 0.012(11) C25 0.102(13) 0.047(5) 0.071(7) -0.002(5) 0.019(9) -0.006(10) C26 0.051(10) 0.052(5) 0.053(5) -0.012(4) 0.005(7) 0.000(10) C27 0.045(6) 0.043(3) 0.074(5) -0.011(3) -0.004(4) -0.004(4) N6A 0.081(10) 0.037(3) 0.057(4) -0.010(3) -0.037(6) 0.011(9) C22A 0.045(6) 0.043(3) 0.074(5) -0.011(3) -0.004(4) -0.004(4) C23A 0.128(13) 0.043(6) 0.052(7) -0.014(5) -0.023(9) 0.016(9) C24A 0.120(13) 0.061(9) 0.050(7) 0.006(6) 0.005(10) 0.012(11) C25A 0.102(13) 0.047(5) 0.071(7) -0.002(5) 0.019(9) -0.006(10) C26A 0.051(10) 0.052(5) 0.053(5) -0.012(4) 0.005(7) 0.000(10) C27A 0.045(6) 0.043(3) 0.074(5) -0.011(3) -0.004(4) -0.004(4) C28 0.063(4) 0.066(4) 0.073(5) -0.030(4) -0.003(4) -0.012(4) C29 0.061(4) 0.051(4) 0.045(4) -0.010(3) -0.002(3) 0.007(3) C30 0.073(5) 0.065(4) 0.078(5) -0.031(4) -0.007(4) 0.000(4) C31 0.086(6) 0.057(4) 0.057(5) -0.017(3) 0.002(4) -0.003(4) C32 0.080(5) 0.055(4) 0.058(5) -0.008(4) 0.000(4) 0.012(4) C33 0.067(5) 0.044(4) 0.067(5) -0.011(3) -0.011(4) 0.005(3) C34 0.113(7) 0.066(5) 0.049(5) -0.012(4) 0.005(5) 0.010(5) C35 0.094(7) 0.110(8) 0.151(10) -0.022(7) 0.013(7) 0.004(6) N9 0.034(9) 0.085(5) 0.087(6) -0.021(5) 0.010(6) -0.021(7) O9 0.083(6) 0.087(6) 0.258(18) -0.064(10) -0.058(10) 0.046(5) O10 0.108(12) 0.212(13) 0.218(19) -0.152(15) -0.025(8) -0.011(9) O11 0.122(10) 0.153(10) 0.178(12) 0.043(9) -0.038(9) 0.031(8) N9A 0.034(9) 0.085(5) 0.087(6) -0.021(5) 0.010(6) -0.021(7) O9A 0.083(6) 0.087(6) 0.258(18) -0.064(10) -0.058(10) 0.046(5) O10A 0.108(12) 0.212(13) 0.218(19) -0.152(15) -0.025(8) -0.011(9) O11A 0.122(10) 0.153(10) 0.178(12) 0.043(9) -0.038(9) 0.031(8) O12 0.20(2) 0.163(17) 0.35(3) -0.060(19) -0.06(2) -0.024(15) O13 0.31(3) 0.193(19) 0.21(2) -0.075(17) -0.10(2) 0.026(19) _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 O1 2.001(4) . ? Ni1 N3 2.039(5) . ? Ni1 N1 2.045(5) . ? Ni1 N2 2.060(5) . ? Ni1 O2 2.079(4) . ? Ni1 O3 2.174(4) . ? Ni2 N6 2.003(8) . ? Ni2 O5 2.034(4) . ? Ni2 N6A 2.060(15) . ? Ni2 N8 2.066(5) . ? Ni2 N7 2.073(5) . ? Ni2 O7 2.141(5) . ? Ni2 O6 2.152(5) . ? O3 N4 1.267(7) . ? O2 N4 1.287(7) . ? O4 N4 1.217(7) . ? O1 C16 1.253(7) . ? O5 C16 1.250(7) . ? O6 N5 1.278(9) . ? O7 N5 1.441(10) . ? O8 N5 1.165(9) . ? N1 C5 1.340(7) . ? N1 C1 1.346(7) . ? N2 C6 1.491(7) . ? N2 C7 1.492(7) . ? N2 C13 1.507(8) . ? N3 C12 1.340(7) . ? N3 C8 1.355(7) . ? N7 C28 1.477(8) . ? N7 C27A 1.483(15) . ? N7 C18 1.492(8) . ? N7 C27 1.537(10) . ? N8 C29 1.331(8) . ? N8 C33 1.354(8) . ? N10 C34 1.129(10) . ? C1 C2 1.389(8) . ? C1 H1 0.9600 . ? C2 C3 1.377(9) . ? C2 H2 0.9600 . ? C3 C4 1.371(9) . ? C3 H3 0.9600 . ? C4 C5 1.391(8) . ? C4 H4 0.9601 . ? C5 C6 1.508(9) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C7 C8 1.513(8) . ? C7 H7A 0.9599 . ? C7 H7B 0.9601 . ? C8 C9 1.381(8) . ? C9 C10 1.374(9) . ? C9 H9 0.9600 . ? C10 C11 1.384(9) . ? C10 H10 0.9600 . ? C11 C12 1.373(8) . ? C11 H11 0.9600 . ? C12 H12 0.9600 . ? C13 C14 1.514(9) . ? C13 H13A 0.9598 . ? C13 H13B 0.9600 . ? C14 C21 1.388(9) . ? C14 C15 1.392(8) . ? C15 C17 1.402(8) . ? C15 C16 1.522(8) . ? C17 C19 1.394(9) . ? C17 C18 1.511(9) . ? C18 H18A 0.9600 . ? C18 H18B 0.9601 . ? C19 C20 1.377(10) . ? C19 H19 0.9600 . ? C20 C21 1.361(10) . ? C20 H20 0.9599 . ? C21 H21 0.9600 . ? N6 C26 1.319(12) . ? N6 C22 1.356(11) . ? C22 C23 1.404(12) . ? C22 H22A 0.9300 . ? C23 C24 1.370(14) . ? C23 H23A 0.9300 . ? C24 C25 1.369(14) . ? C24 H24A 0.9300 . ? C25 C26 1.392(12) . ? C25 H25A 0.9300 . ? C26 C27 1.511(13) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? N6A C26A 1.348(18) . ? N6A C22A 1.395(17) . ? C22A C23A 1.403(17) . ? C22A H22B 0.9300 . ? C23A C24A 1.358(18) . ? C23A H23B 0.9300 . ? C24A C25A 1.367(18) . ? C24A H24B 0.9300 . ? C25A C26A 1.402(16) . ? C25A H25B 0.9300 . ? C26A C27A 1.521(19) . ? C27A H27C 0.9700 . ? C27A H27D 0.9700 . ? C28 C29 1.527(9) . ? C28 H28A 0.9601 . ? C28 H28B 0.9600 . ? C29 C30 1.385(9) . ? C30 C31 1.380(10) . ? C30 H30 0.9600 . ? C31 C32 1.345(10) . ? C31 H31 0.9601 . ? C32 C33 1.384(9) . ? C32 H32 0.9599 . ? C33 H33 0.9601 . ? C34 C35 1.428(13) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? N9 O10 1.207(11) . ? N9 O11 1.214(11) . ? N9 O9 1.221(11) . ? N9A O10A 1.216(16) . ? N9A O9A 1.225(16) . ? N9A O11A 1.227(15) . ? O12 H12A 0.8200 . ? O12 H12B 0.8601 . ? O13 H13C 0.8200 . ? O13 H13D 0.8646 . ? 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 O1 Ni1 N3 97.79(18) . . ? O1 Ni1 N1 88.92(18) . . ? N3 Ni1 N1 164.48(19) . . ? O1 Ni1 N2 99.40(18) . . ? N3 Ni1 N2 82.91(19) . . ? N1 Ni1 N2 82.19(19) . . ? O1 Ni1 O2 96.28(18) . . ? N3 Ni1 O2 95.86(18) . . ? N1 Ni1 O2 97.30(17) . . ? N2 Ni1 O2 164.3(2) . . ? O1 Ni1 O3 156.84(17) . . ? N3 Ni1 O3 89.66(17) . . ? N1 Ni1 O3 89.54(17) . . ? N2 Ni1 O3 103.28(18) . . ? O2 Ni1 O3 61.02(18) . . ? N6 Ni2 O5 88.2(7) . . ? N6 Ni2 N6A 14.6(8) . . ? O5 Ni2 N6A 87.8(15) . . ? N6 Ni2 N8 93.9(7) . . ? O5 Ni2 N8 175.4(2) . . ? N6A Ni2 N8 93.3(15) . . ? N6 Ni2 N7 88.6(3) . . ? O5 Ni2 N7 95.92(19) . . ? N6A Ni2 N7 74.1(6) . . ? N8 Ni2 N7 80.1(2) . . ? N6 Ni2 O7 105.4(4) . . ? O5 Ni2 O7 92.70(19) . . ? N6A Ni2 O7 120.1(7) . . ? N8 Ni2 O7 90.7(2) . . ? N7 Ni2 O7 163.8(3) . . ? N6 Ni2 O6 168.2(3) . . ? O5 Ni2 O6 92.65(18) . . ? N6A Ni2 O6 177.1(6) . . ? N8 Ni2 O6 86.08(19) . . ? N7 Ni2 O6 103.00(19) . . ? O7 Ni2 O6 62.8(2) . . ? N4 O3 Ni1 89.8(4) . . ? N4 O2 Ni1 93.6(4) . . ? C16 O1 Ni1 135.5(4) . . ? C16 O5 Ni2 133.7(4) . . ? N5 O6 Ni2 95.1(4) . . ? N5 O7 Ni2 90.8(5) . . ? C5 N1 C1 119.2(5) . . ? C5 N1 Ni1 112.4(4) . . ? C1 N1 Ni1 128.0(4) . . ? C6 N2 C7 112.1(5) . . ? C6 N2 C13 108.3(4) . . ? C7 N2 C13 113.0(5) . . ? C6 N2 Ni1 104.3(3) . . ? C7 N2 Ni1 105.3(3) . . ? C13 N2 Ni1 113.5(4) . . ? C12 N3 C8 118.0(5) . . ? C12 N3 Ni1 127.9(4) . . ? C8 N3 Ni1 113.5(4) . . ? O4 N4 O3 122.7(6) . . ? O4 N4 O2 121.8(6) . . ? O3 N4 O2 115.6(5) . . ? O8 N5 O6 128.0(8) . . ? O8 N5 O7 121.0(9) . . ? O6 N5 O7 110.5(7) . . ? C28 N7 C27A 105.3(11) . . ? C28 N7 C18 110.7(5) . . ? C27A N7 C18 99.7(11) . . ? C28 N7 C27 112.2(7) . . ? C27A N7 C27 21.0(8) . . ? C18 N7 C27 113.4(6) . . ? C28 N7 Ni2 104.6(4) . . ? C27A N7 Ni2 122.4(9) . . ? C18 N7 Ni2 113.8(4) . . ? C27 N7 Ni2 101.4(5) . . ? C29 N8 C33 118.2(5) . . ? C29 N8 Ni2 113.5(4) . . ? C33 N8 Ni2 128.2(4) . . ? N1 C1 C2 121.6(6) . . ? N1 C1 H1 119.6 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 119.1(6) . . ? C3 C2 H2 121.3 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 119.1(6) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 119.6(6) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 121.3(6) . . ? N1 C5 C6 115.3(5) . . ? C4 C5 C6 123.4(6) . . ? N2 C6 C5 108.9(5) . . ? N2 C6 H6A 109.2 . . ? C5 C6 H6A 111.0 . . ? N2 C6 H6B 108.3 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 109.5 . . ? N2 C7 C8 111.0(5) . . ? N2 C7 H7A 109.2 . . ? C8 C7 H7A 109.6 . . ? N2 C7 H7B 108.5 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 109.5 . . ? N3 C8 C9 122.0(6) . . ? N3 C8 C7 114.2(5) . . ? C9 C8 C7 123.8(6) . . ? C10 C9 C8 118.8(6) . . ? C10 C9 H9 122.4 . . ? C8 C9 H9 118.7 . . ? C9 C10 C11 119.6(6) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 118.3(6) . . ? C12 C11 H11 121.5 . . ? C10 C11 H11 120.1 . . ? N3 C12 C11 123.0(6) . . ? N3 C12 H12 118.3 . . ? C11 C12 H12 118.7 . . ? N2 C13 C14 112.4(5) . . ? N2 C13 H13A 109.0 . . ? C14 C13 H13A 108.5 . . ? N2 C13 H13B 108.5 . . ? C14 C13 H13B 108.9 . . ? H13A C13 H13B 109.5 . . ? C21 C14 C15 118.3(6) . . ? C21 C14 C13 118.5(6) . . ? C15 C14 C13 123.1(5) . . ? C14 C15 C17 120.7(5) . . ? C14 C15 C16 120.4(5) . . ? C17 C15 C16 118.9(5) . . ? O5 C16 O1 122.1(5) . . ? O5 C16 C15 117.8(5) . . ? O1 C16 C15 120.1(5) . . ? C19 C17 C15 118.6(6) . . ? C19 C17 C18 119.6(6) . . ? C15 C17 C18 121.8(5) . . ? N7 C18 C17 113.5(5) . . ? N7 C18 H18A 109.4 . . ? C17 C18 H18A 108.1 . . ? N7 C18 H18B 108.9 . . ? C17 C18 H18B 107.4 . . ? H18A C18 H18B 109.5 . . ? C20 C19 C17 120.3(6) . . ? C20 C19 H19 118.7 . . ? C17 C19 H19 121.0 . . ? C21 C20 C19 120.4(7) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 120.2 . . ? C20 C21 C14 121.3(6) . . ? C20 C21 H21 119.8 . . ? C14 C21 H21 118.8 . . ? C26 N6 C22 121.9(9) . . ? C26 N6 Ni2 112.2(7) . . ? C22 N6 Ni2 125.6(7) . . ? N6 C22 C23 118.3(10) . . ? N6 C22 H22A 120.9 . . ? C23 C22 H22A 120.9 . . ? C24 C23 C22 120.5(12) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C25 C24 C23 119.1(13) . . ? C25 C24 H24A 120.4 . . ? C23 C24 H24A 120.4 . . ? C24 C25 C26 119.4(12) . . ? C24 C25 H25A 120.3 . . ? C26 C25 H25A 120.3 . . ? N6 C26 C25 120.9(11) . . ? N6 C26 C27 116.7(9) . . ? C25 C26 C27 122.3(11) . . ? C26 C27 N7 116.8(8) . . ? C26 C27 H27A 108.1 . . ? N7 C27 H27A 108.1 . . ? C26 C27 H27B 108.1 . . ? N7 C27 H27B 108.1 . . ? H27A C27 H27B 107.3 . . ? C26A N6A C22A 112.5(16) . . ? C26A N6A Ni2 121.6(16) . . ? C22A N6A Ni2 125.6(16) . . ? N6A C22A C23A 123(2) . . ? N6A C22A H22B 118.6 . . ? C23A C22A H22B 118.6 . . ? C24A C23A C22A 121(3) . . ? C24A C23A H23B 119.4 . . ? C22A C23A H23B 119.4 . . ? C23A C24A C25A 118(3) . . ? C23A C24A H24B 121.0 . . ? C25A C24A H24B 121.0 . . ? C24A C25A C26A 118(2) . . ? C24A C25A H25B 120.8 . . ? C26A C25A H25B 120.8 . . ? N6A C26A C25A 127(2) . . ? N6A C26A C27A 116.3(19) . . ? C25A C26A C27A 116.8(19) . . ? N7 C27A C26A 103.3(15) . . ? N7 C27A H27C 111.1 . . ? C26A C27A H27C 111.1 . . ? N7 C27A H27D 111.1 . . ? C26A C27A H27D 111.1 . . ? H27C C27A H27D 109.1 . . ? N7 C28 C29 109.7(6) . . ? N7 C28 H28A 109.1 . . ? C29 C28 H28A 110.4 . . ? N7 C28 H28B 108.8 . . ? C29 C28 H28B 109.4 . . ? H28A C28 H28B 109.5 . . ? N8 C29 C30 123.2(6) . . ? N8 C29 C28 114.4(5) . . ? C30 C29 C28 122.4(6) . . ? C31 C30 C29 117.4(7) . . ? C31 C30 H30 123.1 . . ? C29 C30 H30 119.5 . . ? C32 C31 C30 120.2(7) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 120.1 . . ? C31 C32 C33 119.9(7) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 120.2 . . ? N8 C33 C32 121.0(7) . . ? N8 C33 H33 119.7 . . ? C32 C33 H33 119.2 . . ? N10 C34 C35 179.6(11) . . ? C34 C35 H35A 110.5 . . ? C34 C35 H35B 109.2 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 108.6 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O10 N9 O11 109.8(14) . . ? O10 N9 O9 127.4(13) . . ? O11 N9 O9 118.8(13) . . ? O10A N9A O9A 114(3) . . ? O10A N9A O11A 100(3) . . ? O9A N9A O11A 130(3) . . ? H12A O12 H12B 110.1 . . ? H13C O13 H13D 88.3 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.28 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.859 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.152 # Attachment '3.cif' data_6281 _database_code_depnum_ccdc_archive 'CCDC 667939' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C57 H62 Cl3 N16 Ni2 O14.50' _chemical_formula_sum 'C57 H62 Cl3 N16 Ni2 O14.50' _chemical_formula_weight 1427.00 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 21.9140(7) _cell_length_b 26.5340(11) _cell_length_c 13.9360(5) _cell_angle_alpha 90.00 _cell_angle_beta 119.740(2) _cell_angle_gamma 90.00 _cell_volume 7036.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 20740 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.35 _exptl_crystal_description prism _exptl_crystal_colour 'light blue' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2956 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8227 _exptl_absorpt_correction_T_max 0.9467 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24273 _diffrn_reflns_av_R_equivalents 0.0896 _diffrn_reflns_av_sigmaI/netI 0.0872 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.38 _reflns_number_total 6434 _reflns_number_gt 3975 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (O & M 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material 'SHELXTL, Bruker' _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^)+(0.1382P)^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 6434 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1276 _refine_ls_R_factor_gt 0.0760 _refine_ls_wR_factor_ref 0.2356 _refine_ls_wR_factor_gt 0.1999 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 0.14915(3) 0.11930(3) 0.77974(5) 0.0369(3) Uani 1 1 d . . . C1 C 0.0000 0.2802(3) 0.7500 0.054(2) Uani 1 2 d S . . H1 H 0.0000 0.3152 0.7500 0.065 Uiso 1 2 calc SR . . C2 C 0.0088(3) 0.2542(2) 0.6725(5) 0.0484(14) Uani 1 1 d . . . H2 H 0.0138 0.2719 0.6193 0.058 Uiso 1 1 calc R . . C3 C 0.0105(3) 0.2018(2) 0.6725(4) 0.0380(12) Uani 1 1 d . . . C4 C 0.0000 0.1755(3) 0.7500 0.0336(16) Uani 1 2 d S . . C5 C 0.0000 0.1195(3) 0.7500 0.0374(17) Uani 1 2 d S . . C6 C 0.0212(3) 0.1748(2) 0.5875(4) 0.0413(13) Uani 1 1 d . . . H6A H -0.0069 0.1443 0.5659 0.050 Uiso 1 1 calc R . . H6B H 0.0039 0.1961 0.5225 0.050 Uiso 1 1 calc R . . C7 C 0.1385(3) 0.2065(2) 0.6381(4) 0.0466(14) Uani 1 1 d . . . H7A H 0.1279 0.2327 0.6763 0.056 Uiso 1 1 calc R . . H7B H 0.1284 0.2195 0.5666 0.056 Uiso 1 1 calc R . . C8 C 0.2141(3) 0.1915(2) 0.7043(4) 0.0478(14) Uani 1 1 d . . . C9 C 0.2673(4) 0.2622(3) 0.6499(6) 0.073(2) Uani 1 1 d . . . H9A H 0.2193 0.2721 0.6024 0.110 Uiso 1 1 calc R . . H9B H 0.2896 0.2566 0.6064 0.110 Uiso 1 1 calc R . . H9C H 0.2917 0.2884 0.7028 0.110 Uiso 1 1 calc R . . C10 C 0.3287(3) 0.1906(3) 0.7818(5) 0.0560(16) Uani 1 1 d . . . C11 C 0.3999(4) 0.2002(3) 0.8207(6) 0.075(2) Uani 1 1 d . . . H11 H 0.4145 0.2274 0.7951 0.090 Uiso 1 1 calc R . . C12 C 0.4463(4) 0.1680(4) 0.8973(7) 0.089(3) Uani 1 1 d . . . H12 H 0.4940 0.1728 0.9235 0.107 Uiso 1 1 calc R . . C13 C 0.4254(4) 0.1280(4) 0.9382(7) 0.088(3) Uani 1 1 d . . . H13 H 0.4594 0.1071 0.9916 0.106 Uiso 1 1 calc R . . C14 C 0.3545(3) 0.1182(3) 0.9010(6) 0.0685(19) Uani 1 1 d . . . H14 H 0.3404 0.0914 0.9288 0.082 Uiso 1 1 calc R . . C15 C 0.3060(3) 0.1502(3) 0.8207(5) 0.0536(16) Uani 1 1 d . . . C16 C 0.0959(3) 0.1280(2) 0.5364(4) 0.0422(13) Uani 1 1 d . . . H16A H 0.0528 0.1328 0.4667 0.051 Uiso 1 1 calc R . . H16B H 0.1350 0.1373 0.5260 0.051 Uiso 1 1 calc R . . C17 C 0.1023(3) 0.0751(2) 0.5698(4) 0.0402(13) Uani 1 1 d . . . C18 C 0.0448(3) 0.0357(2) 0.3798(4) 0.0493(15) Uani 1 1 d . . . H18A H 0.0387 0.0700 0.3549 0.074 Uiso 1 1 calc R . . H18B H -0.0003 0.0201 0.3521 0.074 Uiso 1 1 calc R . . H18C H 0.0714 0.0177 0.3529 0.074 Uiso 1 1 calc R . . C19 C 0.1007(3) -0.0083(2) 0.5644(4) 0.0386(13) Uani 1 1 d . . . C20 C 0.0933(3) -0.0587(2) 0.5376(5) 0.0481(14) Uani 1 1 d . . . H20 H 0.0715 -0.0692 0.4643 0.058 Uiso 1 1 calc R . . C21 C 0.1189(3) -0.0929(2) 0.6221(5) 0.0535(15) Uani 1 1 d . . . H21 H 0.1150 -0.1271 0.6060 0.064 Uiso 1 1 calc R . . C22 C 0.1515(3) -0.0770(2) 0.7345(5) 0.0507(15) Uani 1 1 d . . . H22 H 0.1679 -0.1009 0.7907 0.061 Uiso 1 1 calc R . . C23 C 0.1587(3) -0.0272(2) 0.7600(4) 0.0394(13) Uani 1 1 d . . . H23 H 0.1806 -0.0169 0.8334 0.047 Uiso 1 1 calc R . . C24 C 0.1329(3) 0.0085(2) 0.6748(4) 0.0378(12) Uani 1 1 d . . . C25 C 0.2333(4) 0.0558(3) 1.0002(6) 0.0664(19) Uani 1 1 d . . . C26 C 0.2711(4) 0.0238(3) 1.1050(6) 0.088(2) Uani 1 1 d . . . H26A H 0.2667 0.0395 1.1634 0.132 Uiso 1 1 calc R . . H26B H 0.3200 0.0210 1.1266 0.132 Uiso 1 1 calc R . . H26C H 0.2504 -0.0092 1.0909 0.132 Uiso 1 1 calc R . . C27 C 0.1632(3) 0.2117(3) 0.9377(5) 0.0548(16) Uani 1 1 d . . . C28 C 0.1696(4) 0.2528(3) 1.0111(6) 0.086(3) Uani 1 1 d . . . H28A H 0.2097 0.2471 1.0828 0.129 Uiso 1 1 calc R . . H28B H 0.1280 0.2544 1.0174 0.129 Uiso 1 1 calc R . . H28C H 0.1754 0.2840 0.9816 0.129 Uiso 1 1 calc R . . C29 C 0.3033(6) 0.1208(4) 0.5463(8) 0.099(3) Uani 1 1 d . . . C30 C 0.3754(6) 0.1252(5) 0.5750(11) 0.147(5) Uani 1 1 d . . . H30A H 0.3972 0.1518 0.6281 0.220 Uiso 1 1 calc R . . H30B H 0.3783 0.1328 0.5100 0.220 Uiso 1 1 calc R . . H30C H 0.3993 0.0940 0.6062 0.220 Uiso 1 1 calc R . . N1 N 0.1337(2) 0.06061(17) 0.6753(3) 0.0392(10) Uani 1 1 d . . . N2 N 0.0952(2) 0.16097(17) 0.6238(3) 0.0384(10) Uani 1 1 d . . . N3 N 0.2330(2) 0.15142(19) 0.7692(4) 0.0465(12) Uani 1 1 d . . . N4 N 0.0826(2) 0.03454(17) 0.5009(3) 0.0402(11) Uani 1 1 d . . . N5 N 0.2692(3) 0.2160(2) 0.7075(4) 0.0535(13) Uani 1 1 d . . . N6 N 0.2062(2) 0.07842(18) 0.9222(4) 0.0442(12) Uani 1 1 d . . . N7 N 0.1575(2) 0.17993(19) 0.8802(4) 0.0456(11) Uani 1 1 d . . . N8 N 0.2474(5) 0.1170(5) 0.5234(7) 0.146(4) Uani 1 1 d . . . O1 O 0.05530(17) 0.09607(13) 0.7679(3) 0.0376(8) Uani 1 1 d . . . Cl1 Cl 0.16167(13) 0.34840(9) 0.7548(3) 0.1087(9) Uani 1 1 d . . . O2 O 0.1860(4) 0.3003(3) 0.8029(6) 0.142(3) Uani 1 1 d . . . O3 O 0.1374(6) 0.3742(3) 0.8169(11) 0.190(5) Uani 1 1 d . . . O4 O 0.2143(5) 0.3753(4) 0.7510(11) 0.221(6) Uani 1 1 d . . . O5 O 0.1067(5) 0.3398(4) 0.6439(8) 0.209(6) Uani 1 1 d . . . Cl2 Cl 0.0000 0.19884(9) 0.2500 0.0620(6) Uani 1 2 d S . . O6 O -0.0420(3) 0.2290(2) 0.1574(4) 0.0895(16) Uani 1 1 d . . . O7 O -0.0425(4) 0.1695(3) 0.2745(6) 0.154(3) Uani 1 1 d . . . O8 O 0.0000 0.4647(19) 0.7500 0.31(2) Uiso 0.50 2 d SP . . 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 0.0351(4) 0.0442(5) 0.0295(4) -0.0045(3) 0.0146(3) -0.0029(3) C1 0.048(5) 0.028(4) 0.082(6) 0.000 0.028(5) 0.000 C2 0.037(3) 0.042(4) 0.063(3) 0.012(3) 0.022(3) 0.001(3) C3 0.030(3) 0.037(3) 0.036(3) 0.003(2) 0.007(2) 0.000(2) C4 0.026(3) 0.031(4) 0.034(4) 0.000 0.008(3) 0.000 C5 0.036(4) 0.047(5) 0.028(3) 0.000 0.014(3) 0.000 C6 0.038(3) 0.042(3) 0.035(3) 0.003(2) 0.012(2) -0.007(2) C7 0.049(3) 0.050(4) 0.043(3) -0.007(3) 0.024(3) -0.012(3) C8 0.055(4) 0.052(4) 0.041(3) -0.012(3) 0.027(3) -0.010(3) C9 0.073(5) 0.084(5) 0.077(4) -0.004(4) 0.048(4) -0.028(4) C10 0.044(3) 0.077(5) 0.049(3) -0.015(3) 0.024(3) -0.009(3) C11 0.050(4) 0.109(6) 0.077(5) -0.022(5) 0.040(4) -0.028(4) C12 0.045(4) 0.146(9) 0.076(5) -0.026(5) 0.030(4) -0.011(5) C13 0.049(4) 0.112(7) 0.082(5) -0.003(5) 0.016(4) 0.021(4) C14 0.048(4) 0.080(5) 0.071(4) -0.003(4) 0.025(3) 0.007(3) C15 0.040(3) 0.074(5) 0.049(3) -0.018(3) 0.024(3) -0.005(3) C16 0.047(3) 0.048(4) 0.030(3) -0.001(2) 0.019(2) -0.005(3) C17 0.041(3) 0.051(4) 0.031(3) -0.006(3) 0.020(2) -0.005(3) C18 0.051(3) 0.070(4) 0.026(3) -0.010(3) 0.018(2) -0.009(3) C19 0.034(3) 0.051(4) 0.036(3) -0.010(3) 0.020(2) -0.004(2) C20 0.048(3) 0.051(4) 0.043(3) -0.010(3) 0.020(3) -0.003(3) C21 0.050(3) 0.044(4) 0.061(4) -0.014(3) 0.024(3) -0.003(3) C22 0.045(3) 0.053(4) 0.052(3) -0.002(3) 0.023(3) 0.002(3) C23 0.036(3) 0.045(4) 0.035(3) -0.004(2) 0.016(2) 0.005(2) C24 0.036(3) 0.043(3) 0.037(3) -0.007(2) 0.020(2) -0.002(2) C25 0.059(4) 0.072(5) 0.073(5) -0.023(4) 0.036(4) -0.008(4) C26 0.085(6) 0.093(6) 0.069(5) 0.017(4) 0.026(4) 0.011(5) C27 0.036(3) 0.071(5) 0.052(3) -0.018(3) 0.017(3) -0.008(3) C28 0.052(4) 0.111(6) 0.079(5) -0.054(5) 0.021(4) -0.009(4) C29 0.102(7) 0.118(8) 0.091(6) 0.006(5) 0.059(6) 0.015(6) C30 0.101(8) 0.193(13) 0.171(12) -0.005(9) 0.087(9) -0.010(8) N1 0.042(2) 0.047(3) 0.027(2) -0.0060(19) 0.0152(18) -0.003(2) N2 0.039(2) 0.044(3) 0.030(2) -0.0025(19) 0.0155(18) -0.005(2) N3 0.041(3) 0.055(3) 0.042(2) -0.009(2) 0.020(2) -0.007(2) N4 0.043(2) 0.050(3) 0.029(2) -0.006(2) 0.0187(19) -0.008(2) N5 0.052(3) 0.065(3) 0.054(3) -0.015(3) 0.034(3) -0.021(3) N6 0.045(3) 0.053(3) 0.025(2) 0.001(2) 0.0098(19) 0.008(2) N7 0.041(3) 0.049(3) 0.041(2) -0.012(2) 0.017(2) -0.003(2) N8 0.100(7) 0.249(13) 0.103(6) -0.037(6) 0.061(6) 0.002(7) O1 0.0383(19) 0.038(2) 0.0417(19) 0.0002(16) 0.0234(16) -0.0016(17) Cl1 0.0827(15) 0.0704(15) 0.192(3) -0.0344(16) 0.0821(18) -0.0283(12) O2 0.133(6) 0.094(5) 0.143(6) -0.028(4) 0.025(5) 0.013(4) O3 0.211(10) 0.123(7) 0.338(14) -0.064(7) 0.215(11) -0.028(6) O4 0.177(9) 0.194(9) 0.377(16) -0.158(10) 0.202(11) -0.123(7) O5 0.143(7) 0.214(10) 0.165(8) 0.086(7) -0.003(6) -0.091(7) Cl2 0.0758(15) 0.0560(14) 0.0541(13) 0.000 0.0322(12) 0.000 O6 0.105(4) 0.088(4) 0.058(3) 0.015(3) 0.028(3) 0.003(3) O7 0.145(6) 0.164(7) 0.115(5) 0.052(5) 0.036(4) -0.075(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 Ni1 N1 2.042(4) . ? Ni1 N6 2.054(5) . ? Ni1 O1 2.074(3) . ? Ni1 N7 2.080(5) . ? Ni1 N3 2.095(5) . ? Ni1 N2 2.190(4) . ? C1 C2 1.373(7) . ? C1 C2 1.373(7) 2_556 ? C1 H1 0.9300 . ? C2 C3 1.392(8) . ? C2 H2 0.9300 . ? C3 C4 1.397(6) . ? C3 C6 1.499(7) . ? C4 C3 1.397(6) 2_556 ? C4 C5 1.484(10) . ? C5 O1 1.272(5) . ? C5 O1 1.272(5) 2_556 ? C6 N2 1.486(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N2 1.487(7) . ? C7 C8 1.497(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N3 1.324(7) . ? C8 N5 1.352(7) . ? C9 N5 1.455(8) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 N5 1.374(8) . ? C10 C11 1.397(9) . ? C10 C15 1.399(9) . ? C11 C12 1.352(11) . ? C11 H11 0.9300 . ? C12 C13 1.385(12) . ? C12 H12 0.9300 . ? C13 C14 1.398(10) . ? C13 H13 0.9300 . ? C14 C15 1.386(9) . ? C14 H14 0.9300 . ? C15 N3 1.392(7) . ? C16 C17 1.464(8) . ? C16 N2 1.505(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N1 1.334(6) . ? C17 N4 1.362(7) . ? C18 N4 1.466(6) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N4 1.373(7) . ? C19 C20 1.377(8) . ? C19 C24 1.409(7) . ? C20 C21 1.368(8) . ? C20 H20 0.9300 . ? C21 C22 1.425(8) . ? C21 H21 0.9300 . ? C22 C23 1.357(8) . ? C22 H22 0.9300 . ? C23 C24 1.400(7) . ? C23 H23 0.9300 . ? C24 N1 1.383(7) . ? C25 N6 1.119(8) . ? C25 C26 1.530(11) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 N7 1.127(7) . ? C27 C28 1.453(9) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 N8 1.107(12) . ? C29 C30 1.430(14) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? Cl1 O4 1.380(8) . ? Cl1 O3 1.400(9) . ? Cl1 O2 1.416(7) . ? Cl1 O5 1.430(9) . ? Cl2 O7 1.380(6) . ? Cl2 O7 1.380(6) 2 ? Cl2 O6 1.406(5) 2 ? Cl2 O6 1.406(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 Ni1 N6 95.30(17) . . ? N1 Ni1 O1 84.81(15) . . ? N6 Ni1 O1 91.39(16) . . ? N1 Ni1 N7 176.11(17) . . ? N6 Ni1 N7 87.12(18) . . ? O1 Ni1 N7 92.08(16) . . ? N1 Ni1 N3 95.81(17) . . ? N6 Ni1 N3 98.50(19) . . ? O1 Ni1 N3 169.99(17) . . ? N7 Ni1 N3 86.83(18) . . ? N1 Ni1 N2 81.99(16) . . ? N6 Ni1 N2 174.93(17) . . ? O1 Ni1 N2 92.62(14) . . ? N7 Ni1 N2 95.83(17) . . ? N3 Ni1 N2 77.60(17) . . ? C2 C1 C2 119.7(8) . 2_556 ? C2 C1 H1 120.1 . . ? C2 C1 H1 120.1 2_556 . ? C1 C2 C3 121.1(6) . . ? C1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C2 C3 C4 119.0(5) . . ? C2 C3 C6 119.4(5) . . ? C4 C3 C6 121.5(5) . . ? C3 C4 C3 120.1(7) 2_556 . ? C3 C4 C5 120.0(3) 2_556 . ? C3 C4 C5 120.0(3) . . ? O1 C5 O1 121.4(7) . 2_556 ? O1 C5 C4 119.3(3) . . ? O1 C5 C4 119.3(3) 2_556 . ? N2 C6 C3 115.0(4) . . ? N2 C6 H6A 108.5 . . ? C3 C6 H6A 108.5 . . ? N2 C6 H6B 108.5 . . ? C3 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? N2 C7 C8 107.7(5) . . ? N2 C7 H7A 110.2 . . ? C8 C7 H7A 110.2 . . ? N2 C7 H7B 110.2 . . ? C8 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? N3 C8 N5 113.1(5) . . ? N3 C8 C7 120.6(5) . . ? N5 C8 C7 126.2(6) . . ? N5 C9 H9A 109.5 . . ? N5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N5 C10 C11 131.5(7) . . ? N5 C10 C15 106.4(5) . . ? C11 C10 C15 122.1(7) . . ? C12 C11 C10 116.7(7) . . ? C12 C11 H11 121.7 . . ? C10 C11 H11 121.7 . . ? C11 C12 C13 122.4(7) . . ? C11 C12 H12 118.8 . . ? C13 C12 H12 118.8 . . ? C12 C13 C14 121.6(8) . . ? C12 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C15 C14 C13 116.8(7) . . ? C15 C14 H14 121.6 . . ? C13 C14 H14 121.6 . . ? C14 C15 N3 130.9(6) . . ? C14 C15 C10 120.4(6) . . ? N3 C15 C10 108.7(6) . . ? C17 C16 N2 109.8(4) . . ? C17 C16 H16A 109.7 . . ? N2 C16 H16A 109.7 . . ? C17 C16 H16B 109.7 . . ? N2 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? N1 C17 N4 111.1(5) . . ? N1 C17 C16 122.8(5) . . ? N4 C17 C16 125.9(4) . . ? N4 C18 H18A 109.5 . . ? N4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 C20 132.2(5) . . ? N4 C19 C24 105.7(4) . . ? C20 C19 C24 122.1(5) . . ? C21 C20 C19 117.9(5) . . ? C21 C20 H20 121.1 . . ? C19 C20 H20 121.1 . . ? C20 C21 C22 121.2(6) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C23 C22 C21 120.4(6) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 119.4(5) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? N1 C24 C23 132.3(4) . . ? N1 C24 C19 108.7(4) . . ? C23 C24 C19 119.0(5) . . ? N6 C25 C26 178.2(7) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N7 C27 C28 179.3(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 . . ? N8 C29 C30 179.3(14) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C17 N1 C24 106.4(4) . . ? C17 N1 Ni1 112.3(4) . . ? C24 N1 Ni1 139.8(3) . . ? C6 N2 C7 111.1(4) . . ? C6 N2 C16 108.4(4) . . ? C7 N2 C16 108.7(4) . . ? C6 N2 Ni1 115.0(3) . . ? C7 N2 Ni1 106.5(3) . . ? C16 N2 Ni1 107.0(3) . . ? C8 N3 C15 105.1(5) . . ? C8 N3 Ni1 112.8(4) . . ? C15 N3 Ni1 141.1(4) . . ? C17 N4 C19 108.0(4) . . ? C17 N4 C18 126.6(5) . . ? C19 N4 C18 125.3(4) . . ? C8 N5 C10 106.7(5) . . ? C8 N5 C9 127.3(6) . . ? C10 N5 C9 125.9(5) . . ? C25 N6 Ni1 175.4(5) . . ? C27 N7 Ni1 177.6(5) . . ? C5 O1 Ni1 132.9(4) . . ? O4 Cl1 O3 110.6(5) . . ? O4 Cl1 O2 111.0(7) . . ? O3 Cl1 O2 108.5(6) . . ? O4 Cl1 O5 108.3(7) . . ? O3 Cl1 O5 111.8(8) . . ? O2 Cl1 O5 106.5(5) . . ? O7 Cl2 O7 111.3(9) . 2 ? O7 Cl2 O6 108.0(4) . 2 ? O7 Cl2 O6 109.5(4) 2 2 ? O7 Cl2 O6 109.5(4) . . ? O7 Cl2 O6 108.0(4) 2 . ? O6 Cl2 O6 110.5(5) 2 . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.872 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.145 # Attachment '4.cif' data_5949 _database_code_depnum_ccdc_archive 'CCDC 667940' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H59 Cl3 N16 Ni2 O21' _chemical_formula_sum 'C40 H59 Cl3 N16 Ni2 O21' _chemical_formula_weight 1323.80 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 'C 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' _cell_length_a 13.6282(4) _cell_length_b 18.4465(5) _cell_length_c 22.9362(8) _cell_angle_alpha 90.00 _cell_angle_beta 101.0440(10) _cell_angle_gamma 90.00 _cell_volume 5659.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 19012 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.682 _exptl_crystal_description prism _exptl_crystal_colour 'pale blue' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2744 _exptl_absorpt_coefficient_mu 0.895 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.875 _exptl_absorpt_correction_T_max 0.9441 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16708 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.68 _reflns_number_total 9122 _reflns_number_gt 7763 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (O & M 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material 'SHELXTL, Bruker' _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. 5 SADI restraints were used because of the disorder of perchlorate anions. ; _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^)+(0.1046P)^2^+5.1798P] 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 0.268(18) _refine_ls_number_reflns 9122 _refine_ls_number_parameters 737 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1825 _refine_ls_wR_factor_gt 0.1547 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _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 0.9602(6) 0.2989(4) 0.3544(3) 0.0362(17) Uani 1 1 d . . . H1A H 1.0274 0.2932 0.3715 0.043 Uiso 1 1 calc R . . C2 C 0.8908(6) 0.2909(5) 0.3899(4) 0.046(2) Uani 1 1 d . . . H2A H 0.9096 0.2793 0.4299 0.055 Uiso 1 1 calc R . . C3 C 0.7898(7) 0.3009(5) 0.3631(4) 0.047(2) Uani 1 1 d . . . H3A H 0.7402 0.2969 0.3858 0.057 Uiso 1 1 calc R . . C4 C 0.7645(6) 0.3166(4) 0.3042(4) 0.0394(19) Uani 1 1 d . . . H4A H 0.6977 0.3222 0.2863 0.047 Uiso 1 1 calc R . . C5 C 0.8395(5) 0.3241(4) 0.2706(4) 0.0315(16) Uani 1 1 d . . . C6 C 0.8192(5) 0.3423(4) 0.2055(3) 0.0345(17) Uani 1 1 d . . . H6A H 0.7528 0.3256 0.1875 0.041 Uiso 1 1 calc R . . H6B H 0.8209 0.3945 0.2007 0.041 Uiso 1 1 calc R . . C7 C 0.9133(6) 0.3509(4) 0.1229(4) 0.0384(18) Uani 1 1 d . . . H7A H 0.9110 0.4024 0.1311 0.046 Uiso 1 1 calc R . . H7B H 0.8624 0.3403 0.0882 0.046 Uiso 1 1 calc R . . C8 C 1.0139(6) 0.3314(5) 0.1107(3) 0.0377(18) Uani 1 1 d . . . C9 C 1.0345(7) 0.3279(6) 0.0539(4) 0.054(2) Uani 1 1 d . . . H9A H 0.9847 0.3370 0.0209 0.065 Uiso 1 1 calc R . . C10 C 1.1307(8) 0.3108(6) 0.0471(4) 0.059(3) Uani 1 1 d . . . H10A H 1.1458 0.3089 0.0092 0.071 Uiso 1 1 calc R . . C11 C 1.2049(7) 0.2964(5) 0.0967(4) 0.050(2) Uani 1 1 d . . . H11A H 1.2695 0.2841 0.0928 0.060 Uiso 1 1 calc R . . C12 C 1.1791(6) 0.3012(4) 0.1521(4) 0.0375(18) Uani 1 1 d . . . H12A H 1.2278 0.2920 0.1856 0.045 Uiso 1 1 calc R . . C13 C 0.8625(6) 0.2337(4) 0.1543(3) 0.0361(18) Uani 1 1 d . . . H13A H 0.9175 0.2107 0.1401 0.043 Uiso 1 1 calc R . . H13B H 0.8067 0.2368 0.1211 0.043 Uiso 1 1 calc R . . C14 C 0.8326(5) 0.1864(4) 0.2018(3) 0.0327(16) Uani 1 1 d . . . C15 C 0.7319(5) 0.1813(4) 0.2050(4) 0.041(2) Uani 1 1 d . . . H15A H 0.6848 0.2042 0.1761 0.049 Uiso 1 1 calc R . . C16 C 0.7003(6) 0.1438(4) 0.2488(5) 0.048(2) Uani 1 1 d . . . H16A H 0.6329 0.1434 0.2512 0.058 Uiso 1 1 calc R . . C17 C 0.7694(6) 0.1061(5) 0.2903(4) 0.0437(19) Uani 1 1 d . . . H17A H 0.7484 0.0827 0.3217 0.052 Uiso 1 1 calc R . . C18 C 0.8689(5) 0.1028(4) 0.2855(3) 0.0318(16) Uani 1 1 d . . . C19 C 0.9011(5) 0.1464(4) 0.2417(3) 0.0290(15) Uani 1 1 d . . . C20 C 1.0113(5) 0.1477(3) 0.2388(3) 0.0250(15) Uani 1 1 d . . . C21 C 0.9380(5) 0.0545(4) 0.3279(3) 0.0314(16) Uani 1 1 d . . . H21A H 1.0023 0.0785 0.3389 0.038 Uiso 1 1 calc R . . H21B H 0.9109 0.0487 0.3638 0.038 Uiso 1 1 calc R . . C22 C 0.8785(6) 0.0039(4) 0.1257(3) 0.0344(17) Uani 1 1 d . . . H22A H 0.9303 0.0132 0.1056 0.041 Uiso 1 1 calc R . . C23 C 0.7823(6) 0.0120(6) 0.0955(4) 0.048(2) Uani 1 1 d . . . H23A H 0.7685 0.0263 0.0559 0.058 Uiso 1 1 calc R . . C24 C 0.7077(6) -0.0018(6) 0.1258(4) 0.050(2) Uani 1 1 d . . . H24A H 0.6413 0.0040 0.1071 0.060 Uiso 1 1 calc R . . C25 C 0.7299(5) -0.0242(5) 0.1836(4) 0.0400(19) Uani 1 1 d . . . H25A H 0.6789 -0.0348 0.2040 0.048 Uiso 1 1 calc R . . C26 C 0.8265(5) -0.0309(4) 0.2108(3) 0.0292(15) Uani 1 1 d . . . C27 C 0.8582(5) -0.0555(4) 0.2758(3) 0.0327(16) Uani 1 1 d . . . H27A H 0.8064 -0.0431 0.2978 0.039 Uiso 1 1 calc R . . H27B H 0.8668 -0.1077 0.2773 0.039 Uiso 1 1 calc R . . C28 C 1.0136(6) -0.0653(4) 0.3520(3) 0.0342(16) Uani 1 1 d . . . H28A H 1.0073 -0.1161 0.3411 0.041 Uiso 1 1 calc R . . H28B H 0.9895 -0.0586 0.3887 0.041 Uiso 1 1 calc R . . C29 C 1.1212(5) -0.0416(4) 0.3596(3) 0.0346(17) Uani 1 1 d . . . C30 C 1.1837(7) -0.0383(5) 0.4147(4) 0.050(2) Uani 1 1 d . . . H30A H 1.1601 -0.0500 0.4489 0.060 Uiso 1 1 calc R . . C31 C 1.2820(6) -0.0172(6) 0.4177(4) 0.053(2) Uani 1 1 d . . . H31A H 1.3255 -0.0157 0.4543 0.063 Uiso 1 1 calc R . . C32 C 1.3156(7) 0.0016(5) 0.3669(4) 0.047(2) Uani 1 1 d . . . H32A H 1.3810 0.0170 0.3684 0.056 Uiso 1 1 calc R . . C33 C 1.2491(5) -0.0029(4) 0.3135(3) 0.0340(17) Uani 1 1 d . . . H33A H 1.2711 0.0093 0.2789 0.041 Uiso 1 1 calc R . . C34 C 1.0148(6) 0.4814(4) 0.2627(4) 0.0350(17) Uani 1 1 d . . . C35 C 1.2255(5) 0.2936(4) 0.3293(3) 0.0320(16) Uani 1 1 d . . . C36 C 1.1719(6) 0.0119(4) 0.1420(3) 0.0364(18) Uani 1 1 d . . . C37 C 1.0056(5) -0.1784(4) 0.1947(3) 0.0309(16) Uani 1 1 d . . . C38 C 0.6311(7) 0.0671(7) -0.0360(4) 0.064(3) Uani 1 1 d . . . C39 C 0.8597(12) -0.1069(7) -0.0238(7) 0.094(4) Uani 1 1 d . . . C40 C 0.9848(13) 0.1328(8) 0.0175(6) 0.096(4) Uani 1 1 d . . . N1 N 1.0863(5) 0.3187(4) 0.1592(3) 0.0357(16) Uani 1 1 d . . . N2 N 0.8931(4) 0.3088(3) 0.1747(3) 0.0281(14) Uani 1 1 d . . . N3 N 0.9364(4) 0.3145(3) 0.2967(3) 0.0295(14) Uani 1 1 d . . . N4 N 1.0666(5) 0.4778(4) 0.3174(3) 0.0454(17) Uani 1 1 d . . . H4B H 1.1002 0.4394 0.3294 0.054 Uiso 1 1 calc R . . H4C H 1.0669 0.5140 0.3411 0.054 Uiso 1 1 calc R . . N5 N 0.9608(5) 0.5416(4) 0.2457(4) 0.0488(18) Uani 1 1 d . . . H5A H 0.9252 0.5445 0.2105 0.059 Uiso 1 1 calc R . . H5B H 0.9621 0.5772 0.2701 0.059 Uiso 1 1 calc R . . N6 N 1.2854(5) 0.3197(4) 0.3771(3) 0.0466(18) Uani 1 1 d . . . H6C H 1.2783 0.3636 0.3882 0.056 Uiso 1 1 calc R . . H6D H 1.3314 0.2927 0.3970 0.056 Uiso 1 1 calc R . . N7 N 1.2412(6) 0.2279(4) 0.3109(4) 0.062(2) Uani 1 1 d . . . H7C H 1.2053 0.2115 0.2787 0.075 Uiso 1 1 calc R . . H7D H 1.2873 0.2013 0.3312 0.075 Uiso 1 1 calc R . . N8 N 1.1546(4) -0.0242(3) 0.3095(3) 0.0292(14) Uani 1 1 d . . . N9 N 0.9541(4) -0.0194(3) 0.3036(3) 0.0255(13) Uani 1 1 d . . . N10 N 0.9017(4) -0.0166(3) 0.1823(3) 0.0281(14) Uani 1 1 d . . . N11 N 1.0203(6) -0.1670(4) 0.1402(3) 0.0461(17) Uani 1 1 d . . . H11B H 1.0485 -0.1276 0.1319 0.055 Uiso 1 1 calc R . . H11C H 1.0018 -0.1989 0.1130 0.055 Uiso 1 1 calc R . . N12 N 0.9610(6) -0.2411(4) 0.2057(4) 0.0547(19) Uani 1 1 d . . . H12B H 0.9504 -0.2499 0.2408 0.066 Uiso 1 1 calc R . . H12C H 0.9431 -0.2721 0.1777 0.066 Uiso 1 1 calc R . . N13 N 1.2146(6) -0.0127(4) 0.0982(3) 0.0503(19) Uani 1 1 d . . . H13C H 1.2068 -0.0572 0.0872 0.060 Uiso 1 1 calc R . . H13D H 1.2499 0.0159 0.0810 0.060 Uiso 1 1 calc R . . N14 N 1.1902(6) 0.0813(4) 0.1603(4) 0.0510(19) Uani 1 1 d . . . H14A H 1.1662 0.0977 0.1897 0.061 Uiso 1 1 calc R . . H14B H 1.2258 0.1089 0.1424 0.061 Uiso 1 1 calc R . . N15 N 0.6215(7) 0.1276(5) -0.0122(4) 0.068(2) Uani 1 1 d . . . H15B H 0.6606 0.1629 -0.0167 0.082 Uiso 1 1 calc R . . H15C H 0.5759 0.1337 0.0086 0.082 Uiso 1 1 calc R . . N16 N 0.5686(7) 0.0114(5) -0.0285(4) 0.073(3) Uani 1 1 d . . . H16B H 0.5232 0.0178 -0.0076 0.087 Uiso 1 1 calc R . . H16C H 0.5747 -0.0300 -0.0446 0.087 Uiso 1 1 calc R . . O1 O 1.0547(4) 0.2072(3) 0.2363(3) 0.0329(12) Uani 1 1 d . . . O2 O 1.1585(4) 0.3338(3) 0.3006(2) 0.0329(12) Uani 1 1 d . . . O3 O 1.0126(4) 0.4291(3) 0.2265(2) 0.0337(12) Uani 1 1 d . . . O4 O 1.0597(3) 0.0899(2) 0.2396(2) 0.0285(11) Uani 1 1 d . . . O5 O 1.1196(4) -0.0291(3) 0.1680(3) 0.0350(13) Uani 1 1 d . . . O6 O 1.0311(5) -0.1338(2) 0.2364(3) 0.0321(10) Uani 1 1 d . . . O7 O 0.6976(5) 0.0533(4) -0.0679(3) 0.0650(18) Uani 1 1 d . . . O8 O 0.5648(7) 0.2472(5) 0.3882(6) 0.110(3) Uani 1 1 d . . . O9 O 0.5758(6) 0.1221(4) 0.3941(3) 0.073(2) Uani 1 1 d . . . O10 O 0.4701(7) 0.1761(5) 0.3159(3) 0.077(2) Uani 1 1 d . . . O11 O 0.4332(6) 0.1835(5) 0.4094(3) 0.078(2) Uani 1 1 d . . . O12 O 0.3957(8) 0.1299(4) 0.1343(3) 0.084(3) Uani 1 1 d . . . O13 O 0.4514(8) 0.1914(5) 0.0596(4) 0.101(3) Uani 1 1 d . . . O14 O 0.4478(7) 0.0653(6) 0.0595(5) 0.104(3) Uani 1 1 d . . . O15 O 0.2993(6) 0.1249(5) 0.0417(4) 0.086(2) Uani 1 1 d . . . O16 O 0.2470(7) 0.2394(6) 0.4956(4) 0.098(3) Uani 1 1 d . A . O17 O 0.2366(11) 0.1176(7) 0.4901(5) 0.137(4) Uani 1 1 d D A . O18 O 0.0867(15) 0.1982(16) 0.4556(14) 0.098(3) Uani 0.45(3) 1 d PD A 1 O18A O 0.1177(18) 0.1759(13) 0.4344(8) 0.098(3) Uani 0.55(3) 1 d PD A 2 O19 O 0.1519(9) 0.1722(6) 0.5493(5) 0.114(4) Uani 1 1 d . A . O20 O 0.8639(7) -0.0277(6) -0.0398(4) 0.092(3) Uani 1 1 d . . . O21 O 1.0158(7) 0.0598(5) 0.0181(4) 0.094(3) Uani 1 1 d . . . Cl1 Cl 0.51273(14) 0.18211(10) 0.37709(9) 0.0383(4) Uani 1 1 d . . . Cl2 Cl 0.40002(17) 0.12891(13) 0.07296(10) 0.0509(6) Uani 1 1 d . . . Cl3 Cl 0.1757(2) 0.17846(14) 0.49201(11) 0.0621(6) Uani 1 1 d D . . Ni1 Ni 1.02953(6) 0.31683(4) 0.23635(4) 0.0256(2) Uani 1 1 d . . . Ni2 Ni 1.03995(6) -0.02045(4) 0.23612(4) 0.0244(2) 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 0.037(4) 0.033(4) 0.037(4) -0.006(3) 0.005(3) 0.001(3) C2 0.043(5) 0.051(6) 0.042(5) -0.006(4) 0.008(4) -0.008(4) C3 0.045(5) 0.049(5) 0.052(6) -0.003(4) 0.018(4) -0.003(4) C4 0.026(4) 0.035(5) 0.059(6) -0.004(4) 0.012(3) -0.001(3) C5 0.032(4) 0.018(3) 0.044(4) -0.002(3) 0.004(3) 0.004(3) C6 0.026(4) 0.035(4) 0.040(4) -0.002(3) 0.000(3) 0.003(3) C7 0.047(4) 0.035(4) 0.031(4) 0.007(3) 0.001(3) 0.002(4) C8 0.051(5) 0.037(4) 0.024(4) 0.000(3) 0.005(3) 0.002(4) C9 0.060(6) 0.072(7) 0.029(4) 0.004(4) 0.006(4) -0.005(5) C10 0.069(6) 0.072(7) 0.042(5) -0.002(5) 0.024(5) -0.004(5) C11 0.047(5) 0.051(6) 0.055(6) -0.003(4) 0.022(4) 0.000(4) C12 0.036(4) 0.030(4) 0.049(5) -0.003(3) 0.014(3) 0.001(3) C13 0.035(4) 0.028(4) 0.040(4) -0.008(3) -0.005(3) 0.005(3) C14 0.029(4) 0.024(4) 0.043(4) -0.009(3) 0.001(3) -0.002(3) C15 0.020(3) 0.030(4) 0.068(6) -0.005(4) -0.002(3) 0.000(3) C16 0.023(4) 0.032(5) 0.093(7) -0.004(4) 0.019(4) -0.002(3) C17 0.048(5) 0.033(4) 0.056(5) -0.009(4) 0.024(4) -0.005(4) C18 0.033(4) 0.028(4) 0.036(4) -0.008(3) 0.011(3) -0.004(3) C19 0.023(3) 0.024(4) 0.040(4) -0.008(3) 0.008(3) -0.005(3) C20 0.031(4) 0.017(3) 0.027(3) 0.001(3) 0.005(3) 0.000(3) C21 0.036(4) 0.030(4) 0.030(4) -0.008(3) 0.012(3) 0.001(3) C22 0.035(4) 0.040(4) 0.029(4) 0.003(3) 0.008(3) 0.007(3) C23 0.040(5) 0.071(7) 0.034(5) 0.002(4) 0.004(4) 0.012(4) C24 0.031(4) 0.067(6) 0.047(5) -0.001(4) -0.006(3) 0.006(4) C25 0.025(4) 0.044(5) 0.051(5) -0.005(4) 0.008(3) -0.007(3) C26 0.031(4) 0.027(4) 0.030(4) -0.004(3) 0.005(3) -0.009(3) C27 0.029(4) 0.030(4) 0.039(4) -0.003(3) 0.009(3) -0.008(3) C28 0.042(4) 0.035(4) 0.027(4) 0.007(3) 0.009(3) 0.000(3) C29 0.034(4) 0.041(5) 0.028(4) -0.001(3) 0.005(3) -0.004(3) C30 0.054(5) 0.060(6) 0.032(5) 0.004(4) 0.002(4) -0.004(4) C31 0.043(5) 0.066(7) 0.043(5) 0.004(4) -0.005(4) -0.004(4) C32 0.044(5) 0.053(6) 0.042(5) -0.002(4) 0.005(4) -0.004(4) C33 0.027(4) 0.036(4) 0.039(4) 0.006(3) 0.005(3) 0.007(3) C34 0.034(4) 0.030(4) 0.044(5) -0.005(3) 0.014(3) -0.006(3) C35 0.028(4) 0.035(4) 0.033(4) 0.007(3) 0.006(3) -0.003(3) C36 0.040(4) 0.033(5) 0.037(4) 0.003(3) 0.010(3) 0.007(4) C37 0.033(4) 0.022(4) 0.034(4) 0.001(3) -0.003(3) -0.001(3) C38 0.051(5) 0.097(9) 0.039(5) 0.017(6) 0.000(4) 0.003(6) C39 0.118(11) 0.063(8) 0.108(11) 0.006(7) 0.038(9) 0.008(8) C40 0.132(12) 0.079(10) 0.070(9) -0.001(7) 0.002(8) 0.019(9) N1 0.040(4) 0.036(4) 0.032(4) 0.001(3) 0.009(3) -0.003(3) N2 0.028(3) 0.021(3) 0.033(3) 0.000(3) 0.000(2) 0.001(2) N3 0.028(3) 0.025(3) 0.036(4) -0.002(3) 0.009(3) 0.000(3) N4 0.055(4) 0.031(4) 0.050(5) -0.012(3) 0.011(3) 0.001(3) N5 0.051(4) 0.029(4) 0.068(5) 0.000(3) 0.017(3) 0.008(3) N6 0.047(4) 0.048(4) 0.037(4) 0.005(3) -0.010(3) -0.002(3) N7 0.047(4) 0.042(5) 0.085(6) -0.012(4) -0.020(4) 0.015(4) N8 0.027(3) 0.027(3) 0.033(4) 0.001(3) 0.005(2) -0.002(3) N9 0.029(3) 0.022(3) 0.028(3) -0.004(2) 0.011(2) 0.000(2) N10 0.027(3) 0.025(3) 0.032(3) 0.000(3) 0.008(2) -0.001(2) N11 0.064(5) 0.034(4) 0.039(4) -0.004(3) 0.007(3) -0.010(3) N12 0.072(5) 0.029(4) 0.059(5) -0.005(3) 0.002(4) -0.014(4) N13 0.052(4) 0.053(5) 0.053(5) -0.004(4) 0.028(4) 0.003(4) N14 0.054(4) 0.037(4) 0.073(5) 0.003(4) 0.039(4) -0.009(3) N15 0.073(6) 0.056(6) 0.076(7) -0.006(5) 0.016(5) 0.011(5) N16 0.073(6) 0.072(7) 0.077(6) 0.000(5) 0.025(5) -0.011(5) O1 0.029(3) 0.022(3) 0.048(3) -0.001(2) 0.008(2) -0.002(2) O2 0.032(3) 0.027(3) 0.037(3) -0.001(2) -0.001(2) 0.002(2) O3 0.044(3) 0.022(3) 0.037(3) 0.002(2) 0.011(2) -0.001(2) O4 0.030(3) 0.019(2) 0.039(3) -0.001(2) 0.015(2) -0.002(2) O5 0.037(3) 0.030(3) 0.043(3) -0.002(2) 0.021(2) 0.002(2) O6 0.039(3) 0.023(2) 0.033(2) 0.002(3) 0.0025(19) -0.005(3) O7 0.073(5) 0.062(5) 0.059(4) 0.007(3) 0.010(3) -0.001(4) O8 0.077(5) 0.047(5) 0.205(11) -0.012(6) 0.021(6) -0.027(4) O9 0.081(5) 0.061(5) 0.074(5) 0.001(4) 0.005(4) 0.039(4) O10 0.113(7) 0.077(5) 0.041(4) -0.006(4) 0.012(4) 0.034(5) O11 0.068(5) 0.115(7) 0.058(5) 0.021(4) 0.030(4) 0.023(4) O12 0.143(8) 0.065(5) 0.045(4) -0.016(4) 0.019(4) -0.047(5) O13 0.140(8) 0.087(7) 0.085(6) -0.008(5) 0.044(6) -0.062(6) O14 0.085(6) 0.093(7) 0.137(8) -0.031(6) 0.030(6) 0.017(5) O15 0.075(5) 0.084(6) 0.092(6) -0.003(5) 0.001(4) -0.009(5) O16 0.097(6) 0.097(6) 0.095(6) 0.034(5) 0.007(4) -0.005(5) O17 0.180(12) 0.111(9) 0.107(9) -0.021(7) -0.001(8) 0.036(9) O18 0.097(6) 0.097(6) 0.095(6) 0.034(5) 0.007(4) -0.005(5) O18A 0.097(6) 0.097(6) 0.095(6) 0.034(5) 0.007(4) -0.005(5) O19 0.144(9) 0.115(8) 0.101(8) 0.013(6) 0.068(7) -0.001(7) O20 0.094(6) 0.093(7) 0.096(7) -0.003(5) 0.037(5) 0.001(5) O21 0.106(7) 0.091(7) 0.087(6) 0.007(5) 0.022(5) 0.007(6) Cl1 0.0401(10) 0.0324(10) 0.0426(11) -0.0019(8) 0.0082(8) 0.0018(8) Cl2 0.0579(13) 0.0528(14) 0.0455(12) -0.0117(10) 0.0189(10) -0.0131(11) Cl3 0.0773(17) 0.0529(15) 0.0536(14) 0.0148(11) 0.0063(12) 0.0030(13) Ni1 0.0248(4) 0.0219(4) 0.0292(4) -0.0001(5) 0.0031(3) 0.0005(4) Ni2 0.0245(4) 0.0216(4) 0.0278(4) 0.0005(4) 0.0066(3) -0.0002(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 N3 1.332(10) . ? C1 C2 1.368(12) . ? C1 H1A 0.9300 . ? C2 C3 1.408(13) . ? C2 H2A 0.9300 . ? C3 C4 1.360(12) . ? C3 H3A 0.9300 . ? C4 C5 1.399(11) . ? C4 H4A 0.9300 . ? C5 N3 1.353(10) . ? C5 C6 1.504(11) . ? C6 N2 1.472(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N2 1.490(10) . ? C7 C8 1.494(12) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N1 1.358(10) . ? C8 C9 1.387(12) . ? C9 C10 1.386(14) . ? C9 H9A 0.9300 . ? C10 C11 1.396(14) . ? C10 H10A 0.9300 . ? C11 C12 1.383(12) . ? C11 H11A 0.9300 . ? C12 N1 1.345(10) . ? C12 H12A 0.9300 . ? C13 N2 1.496(10) . ? C13 C14 1.510(11) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C19 1.389(11) . ? C14 C15 1.392(10) . ? C15 C16 1.357(13) . ? C15 H15A 0.9300 . ? C16 C17 1.391(13) . ? C16 H16A 0.9300 . ? C17 C18 1.383(11) . ? C17 H17A 0.9300 . ? C18 C19 1.419(10) . ? C18 C21 1.508(11) . ? C19 C20 1.516(9) . ? C20 O4 1.252(8) . ? C20 O1 1.254(8) . ? C21 N9 1.506(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N10 1.332(10) . ? C22 C23 1.368(11) . ? C22 H22A 0.9300 . ? C23 C24 1.362(13) . ? C23 H23A 0.9300 . ? C24 C25 1.365(12) . ? C24 H24A 0.9300 . ? C25 C26 1.351(10) . ? C25 H25A 0.9300 . ? C26 N10 1.343(9) . ? C26 C27 1.539(10) . ? C27 N9 1.496(9) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 N9 1.502(9) . ? C28 C29 1.508(10) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 N8 1.352(10) . ? C29 C30 1.383(11) . ? C30 C31 1.383(12) . ? C30 H30A 0.9300 . ? C31 C32 1.377(13) . ? C31 H31A 0.9300 . ? C32 C33 1.378(12) . ? C32 H32A 0.9300 . ? C33 N8 1.332(9) . ? C33 H33A 0.9300 . ? C34 O3 1.269(9) . ? C34 N4 1.318(11) . ? C34 N5 1.349(10) . ? C35 O2 1.260(9) . ? C35 N7 1.313(11) . ? C35 N6 1.325(10) . ? C36 O5 1.266(10) . ? C36 N13 1.333(10) . ? C36 N14 1.354(11) . ? C37 O6 1.259(9) . ? C37 N11 1.320(10) . ? C37 N12 1.353(10) . ? C38 N15 1.261(14) . ? C38 O7 1.297(12) . ? C38 N16 1.366(14) . ? C39 O20 1.511(16) . ? C40 O21 1.410(16) . ? N1 Ni1 2.062(7) . ? N2 Ni1 2.114(6) . ? N3 Ni1 2.050(6) . ? N4 H4B 0.8600 . ? N4 H4C 0.8600 . ? N5 H5A 0.8600 . ? N5 H5B 0.8600 . ? N6 H6C 0.8600 . ? N6 H6D 0.8600 . ? N7 H7C 0.8600 . ? N7 H7D 0.8600 . ? N8 Ni2 2.067(6) . ? N9 Ni2 2.112(6) . ? N10 Ni2 2.046(6) . ? N11 H11B 0.8600 . ? N11 H11C 0.8600 . ? N12 H12B 0.8600 . ? N12 H12C 0.8600 . ? N13 H13C 0.8600 . ? N13 H13D 0.8600 . ? N14 H14A 0.8600 . ? N14 H14B 0.8600 . ? N15 H15B 0.8600 . ? N15 H15C 0.8600 . ? N16 H16B 0.8600 . ? N16 H16C 0.8600 . ? O1 Ni1 2.050(5) . ? O2 Ni1 2.090(5) . ? O3 Ni1 2.091(5) . ? O4 Ni2 2.052(5) . ? O5 Ni2 2.071(5) . ? O6 Ni2 2.095(4) . ? O8 Cl1 1.393(8) . ? O9 Cl1 1.410(7) . ? O10 Cl1 1.416(8) . ? O11 Cl1 1.426(7) . ? O12 Cl2 1.419(8) . ? O13 Cl2 1.412(8) . ? O14 Cl2 1.405(9) . ? O15 Cl2 1.423(8) . ? O16 Cl3 1.478(10) . ? O17 Cl3 1.401(11) . ? O18 Cl3 1.383(14) . ? O18A Cl3 1.405(14) . ? O19 Cl3 1.416(9) . ? 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 N3 C1 C2 123.3(8) . . ? N3 C1 H1A 118.3 . . ? C2 C1 H1A 118.3 . . ? C1 C2 C3 117.2(8) . . ? C1 C2 H2A 121.4 . . ? C3 C2 H2A 121.4 . . ? C4 C3 C2 120.0(8) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 119.7(7) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? N3 C5 C4 119.8(7) . . ? N3 C5 C6 116.6(7) . . ? C4 C5 C6 123.6(7) . . ? N2 C6 C5 111.7(6) . . ? N2 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? N2 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? N2 C7 C8 109.8(6) . . ? N2 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? N2 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? N1 C8 C9 121.1(8) . . ? N1 C8 C7 116.0(7) . . ? C9 C8 C7 123.0(8) . . ? C10 C9 C8 118.9(9) . . ? C10 C9 H9A 120.6 . . ? C8 C9 H9A 120.6 . . ? C9 C10 C11 120.2(8) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C12 C11 C10 117.7(9) . . ? C12 C11 H11A 121.2 . . ? C10 C11 H11A 121.2 . . ? N1 C12 C11 122.6(8) . . ? N1 C12 H12A 118.7 . . ? C11 C12 H12A 118.7 . . ? N2 C13 C14 114.0(6) . . ? N2 C13 H13A 108.8 . . ? C14 C13 H13A 108.8 . . ? N2 C13 H13B 108.8 . . ? C14 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C19 C14 C15 118.3(7) . . ? C19 C14 C13 122.9(6) . . ? C15 C14 C13 118.8(7) . . ? C16 C15 C14 122.0(8) . . ? C16 C15 H15A 119.0 . . ? C14 C15 H15A 119.0 . . ? C15 C16 C17 119.5(7) . . ? C15 C16 H16A 120.3 . . ? C17 C16 H16A 120.3 . . ? C18 C17 C16 120.9(8) . . ? C18 C17 H17A 119.5 . . ? C16 C17 H17A 119.5 . . ? C17 C18 C19 118.2(7) . . ? C17 C18 C21 118.4(7) . . ? C19 C18 C21 123.4(6) . . ? C14 C19 C18 120.6(6) . . ? C14 C19 C20 120.5(6) . . ? C18 C19 C20 118.9(6) . . ? O4 C20 O1 119.7(6) . . ? O4 C20 C19 120.6(6) . . ? O1 C20 C19 119.7(6) . . ? N9 C21 C18 114.4(6) . . ? N9 C21 H21A 108.7 . . ? C18 C21 H21A 108.7 . . ? N9 C21 H21B 108.7 . . ? C18 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? N10 C22 C23 123.5(7) . . ? N10 C22 H22A 118.3 . . ? C23 C22 H22A 118.3 . . ? C24 C23 C22 117.2(8) . . ? C24 C23 H23A 121.4 . . ? C22 C23 H23A 121.4 . . ? C23 C24 C25 120.3(7) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C26 C25 C24 119.5(7) . . ? C26 C25 H25A 120.3 . . ? C24 C25 H25A 120.3 . . ? N10 C26 C25 121.6(7) . . ? N10 C26 C27 115.6(6) . . ? C25 C26 C27 122.9(6) . . ? N9 C27 C26 109.9(6) . . ? N9 C27 H27A 109.7 . . ? C26 C27 H27A 109.7 . . ? N9 C27 H27B 109.7 . . ? C26 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? N9 C28 C29 107.3(6) . . ? N9 C28 H28A 110.2 . . ? C29 C28 H28A 110.2 . . ? N9 C28 H28B 110.2 . . ? C29 C28 H28B 110.2 . . ? H28A C28 H28B 108.5 . . ? N8 C29 C30 121.1(7) . . ? N8 C29 C28 116.6(6) . . ? C30 C29 C28 122.2(7) . . ? C29 C30 C31 118.6(8) . . ? C29 C30 H30A 120.7 . . ? C31 C30 H30A 120.7 . . ? C32 C31 C30 120.2(8) . . ? C32 C31 H31A 119.9 . . ? C30 C31 H31A 119.9 . . ? C31 C32 C33 117.9(8) . . ? C31 C32 H32A 121.1 . . ? C33 C32 H32A 121.1 . . ? N8 C33 C32 122.8(7) . . ? N8 C33 H33A 118.6 . . ? C32 C33 H33A 118.6 . . ? O3 C34 N4 121.7(7) . . ? O3 C34 N5 119.6(8) . . ? N4 C34 N5 118.6(7) . . ? O2 C35 N7 121.5(7) . . ? O2 C35 N6 119.2(8) . . ? N7 C35 N6 119.2(7) . . ? O5 C36 N13 121.2(8) . . ? O5 C36 N14 120.4(7) . . ? N13 C36 N14 118.3(7) . . ? O6 C37 N11 123.0(7) . . ? O6 C37 N12 118.9(7) . . ? N11 C37 N12 118.0(7) . . ? N15 C38 O7 124.1(11) . . ? N15 C38 N16 119.5(10) . . ? O7 C38 N16 116.3(11) . . ? C12 N1 C8 119.5(7) . . ? C12 N1 Ni1 128.1(6) . . ? C8 N1 Ni1 111.9(5) . . ? C6 N2 C7 114.3(6) . . ? C6 N2 C13 111.3(6) . . ? C7 N2 C13 108.4(6) . . ? C6 N2 Ni1 104.1(4) . . ? C7 N2 Ni1 102.9(4) . . ? C13 N2 Ni1 115.6(4) . . ? C1 N3 C5 119.9(7) . . ? C1 N3 Ni1 127.7(5) . . ? C5 N3 Ni1 112.1(5) . . ? C34 N4 H4B 120.0 . . ? C34 N4 H4C 120.0 . . ? H4B N4 H4C 120.0 . . ? C34 N5 H5A 120.0 . . ? C34 N5 H5B 120.0 . . ? H5A N5 H5B 120.0 . . ? C35 N6 H6C 120.0 . . ? C35 N6 H6D 120.0 . . ? H6C N6 H6D 120.0 . . ? C35 N7 H7C 120.0 . . ? C35 N7 H7D 120.0 . . ? H7C N7 H7D 120.0 . . ? C33 N8 C29 119.3(6) . . ? C33 N8 Ni2 128.0(5) . . ? C29 N8 Ni2 112.0(5) . . ? C27 N9 C28 111.6(6) . . ? C27 N9 C21 112.6(6) . . ? C28 N9 C21 109.4(6) . . ? C27 N9 Ni2 104.2(4) . . ? C28 N9 Ni2 103.8(4) . . ? C21 N9 Ni2 114.8(4) . . ? C22 N10 C26 118.0(6) . . ? C22 N10 Ni2 128.2(5) . . ? C26 N10 Ni2 113.6(5) . . ? C37 N11 H11B 120.0 . . ? C37 N11 H11C 120.0 . . ? H11B N11 H11C 120.0 . . ? C37 N12 H12B 120.0 . . ? C37 N12 H12C 120.0 . . ? H12B N12 H12C 120.0 . . ? C36 N13 H13C 120.0 . . ? C36 N13 H13D 120.0 . . ? H13C N13 H13D 120.0 . . ? C36 N14 H14A 120.0 . . ? C36 N14 H14B 120.0 . . ? H14A N14 H14B 120.0 . . ? C38 N15 H15B 120.0 . . ? C38 N15 H15C 120.0 . . ? H15B N15 H15C 120.0 . . ? C38 N16 H16B 120.0 . . ? C38 N16 H16C 120.0 . . ? H16B N16 H16C 120.0 . . ? C20 O1 Ni1 141.6(4) . . ? C35 O2 Ni1 135.0(5) . . ? C34 O3 Ni1 133.9(5) . . ? C20 O4 Ni2 141.2(4) . . ? C36 O5 Ni2 137.1(5) . . ? C37 O6 Ni2 131.1(5) . . ? O8 Cl1 O9 111.3(6) . . ? O8 Cl1 O10 110.3(6) . . ? O9 Cl1 O10 109.0(5) . . ? O8 Cl1 O11 107.5(6) . . ? O9 Cl1 O11 110.8(5) . . ? O10 Cl1 O11 107.9(5) . . ? O14 Cl2 O13 111.3(7) . . ? O14 Cl2 O12 109.7(6) . . ? O13 Cl2 O12 108.7(5) . . ? O14 Cl2 O15 106.8(6) . . ? O13 Cl2 O15 113.8(6) . . ? O12 Cl2 O15 106.3(6) . . ? O18 Cl3 O17 130.4(17) . . ? O18 Cl3 O18A 33.9(12) . . ? O17 Cl3 O18A 100.0(13) . . ? O18 Cl3 O19 104.5(16) . . ? O17 Cl3 O19 101.9(7) . . ? O18A Cl3 O19 133.0(12) . . ? O18 Cl3 O16 109.0(11) . . ? O17 Cl3 O16 103.0(8) . . ? O18A Cl3 O16 108.9(9) . . ? O19 Cl3 O16 106.0(7) . . ? N3 Ni1 O1 96.0(2) . . ? N3 Ni1 N1 164.2(2) . . ? O1 Ni1 N1 85.7(2) . . ? N3 Ni1 O2 94.2(2) . . ? O1 Ni1 O2 91.7(2) . . ? N1 Ni1 O2 101.5(2) . . ? N3 Ni1 O3 91.4(2) . . ? O1 Ni1 O3 172.5(2) . . ? N1 Ni1 O3 86.7(2) . . ? O2 Ni1 O3 89.3(2) . . ? N3 Ni1 N2 82.6(3) . . ? O1 Ni1 N2 93.2(2) . . ? N1 Ni1 N2 81.6(3) . . ? O2 Ni1 N2 174.4(2) . . ? O3 Ni1 N2 86.1(2) . . ? N10 Ni2 O4 95.1(2) . . ? N10 Ni2 N8 163.2(2) . . ? O4 Ni2 N8 85.9(2) . . ? N10 Ni2 O5 95.9(2) . . ? O4 Ni2 O5 91.3(2) . . ? N8 Ni2 O5 100.8(2) . . ? N10 Ni2 O6 89.4(2) . . ? O4 Ni2 O6 175.6(2) . . ? N8 Ni2 O6 89.9(2) . . ? O5 Ni2 O6 87.9(2) . . ? N10 Ni2 N9 82.3(2) . . ? O4 Ni2 N9 92.8(2) . . ? N8 Ni2 N9 80.9(2) . . ? O5 Ni2 N9 175.6(2) . . ? O6 Ni2 N9 88.1(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.597 _refine_diff_density_min -0.817 _refine_diff_density_rms 0.170 # Attachment '5.cif' data_6393 _database_code_depnum_ccdc_archive 'CCDC 667941' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H59 Cl3 N18 Ni2 O18' _chemical_formula_sum 'C49 H59 Cl3 N18 Ni2 O18' _chemical_formula_weight 1411.91 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' 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 18.4897(4) _cell_length_b 15.2943(3) _cell_length_c 24.4927(6) _cell_angle_alpha 90.00 _cell_angle_beta 110.4140(10) _cell_angle_gamma 90.00 _cell_volume 6491.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 14793 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.35 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2920 _exptl_absorpt_coefficient_mu 0.783 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7348 _exptl_absorpt_correction_T_max 0.8722 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20967 _diffrn_reflns_av_R_equivalents 0.0966 _diffrn_reflns_av_sigmaI/netI 0.0805 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.34 _reflns_number_total 5903 _reflns_number_gt 4156 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (O & M 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material 'SHELXTL, Bruker' _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^)+(0.1610P)^2^+0.8501P] 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 5903 _refine_ls_number_parameters 412 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1078 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.2451 _refine_ls_wR_factor_gt 0.2235 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.16764(3) 0.04309(4) 0.24944(3) 0.0245(3) Uani 1 1 d . . . Cl1 Cl 0.48464(8) 0.11519(11) 0.11623(6) 0.0500(4) Uani 1 1 d . . . Cl2 Cl 0.2485(2) 0.3338(3) 0.46350(14) 0.0601(9) Uani 0.50 1 d P . . O1 O 0.06099(19) 0.0273(2) 0.25544(16) 0.0313(9) Uani 1 1 d . . . O2 O 0.1477(2) -0.0599(2) 0.19016(16) 0.0366(9) Uani 1 1 d . . . O3 O 0.28057(19) 0.0541(2) 0.24949(15) 0.0314(9) Uani 1 1 d . . . O4 O 0.5436(4) 0.0557(5) 0.1201(3) 0.116(3) Uani 1 1 d . . . O5 O 0.4794(5) 0.1753(6) 0.0719(3) 0.139(3) Uani 1 1 d . . . O6 O 0.5049(4) 0.1652(4) 0.1695(2) 0.0838(17) Uani 1 1 d . . . O7 O 0.4144(3) 0.0747(5) 0.1063(3) 0.092(2) Uani 1 1 d . . . O8 O 0.1779(7) 0.3703(8) 0.4248(4) 0.0779(16) Uani 0.50 1 d P . . O9 O 0.2805(7) 0.3712(8) 0.5197(4) 0.0779(16) Uani 0.50 1 d P . . O10 O 0.2324(7) 0.2387(8) 0.4745(4) 0.0779(16) Uani 0.50 1 d P . . O11 O 0.2797(7) 0.3314(8) 0.4262(4) 0.0779(16) Uani 0.50 1 d P . . N1 N 0.2139(2) -0.0202(3) 0.32884(19) 0.0299(10) Uani 1 1 d . . . N2 N 0.1969(2) 0.1526(3) 0.30766(18) 0.0281(10) Uani 1 1 d . . . N3 N 0.1311(2) 0.1420(3) 0.18971(18) 0.0289(10) Uani 1 1 d . . . N4 N 0.2990(3) -0.0087(3) 0.41931(18) 0.0381(11) Uani 1 1 d . . . N5 N 0.1221(3) 0.2864(3) 0.1772(2) 0.0361(11) Uani 1 1 d . . . N6 N 0.3854(3) 0.0689(4) 0.2246(2) 0.0527(14) Uani 1 1 d . . . H6A' H 0.4106 0.0924 0.2577 0.063 Uiso 1 1 calc R . . H6B' H 0.4074 0.0617 0.1991 0.063 Uiso 1 1 calc R . . N7 N 0.2775(3) 0.0081(4) 0.1614(2) 0.0595(16) Uani 1 1 d . . . H7A' H 0.2305 -0.0092 0.1519 0.071 Uiso 1 1 calc R . . H7B' H 0.3016 0.0022 0.1373 0.071 Uiso 1 1 calc R . . N8 N 0.1056(3) -0.1761(3) 0.1322(2) 0.0505(14) Uani 1 1 d . . . H8A' H 0.1426 -0.1707 0.1188 0.061 Uiso 1 1 calc R . . H8B' H 0.0725 -0.2176 0.1198 0.061 Uiso 1 1 calc R . . N9 N 0.0418(3) -0.1298(3) 0.1913(2) 0.0505(13) Uani 1 1 d . . . H9A' H 0.0367 -0.0940 0.2167 0.061 Uiso 1 1 calc R . . H9B' H 0.0093 -0.1717 0.1784 0.061 Uiso 1 1 calc R . . C1 C 0.2208(3) -0.1013(3) 0.3556(2) 0.0330(12) Uani 1 1 d . . . C2 C 0.1861(4) -0.1816(4) 0.3338(3) 0.0420(14) Uani 1 1 d . . . H2 H 0.1513 -0.1867 0.2959 0.050 Uiso 1 1 calc R . . C3 C 0.2052(4) -0.2523(4) 0.3706(3) 0.0571(18) Uani 1 1 d . . . H3 H 0.1817 -0.3060 0.3580 0.069 Uiso 1 1 calc R . . C4 C 0.2597(5) -0.2445(5) 0.4268(3) 0.066(2) Uani 1 1 d . . . H4 H 0.2715 -0.2937 0.4506 0.080 Uiso 1 1 calc R . . C5 C 0.2967(4) -0.1668(4) 0.4485(3) 0.0548(17) Uani 1 1 d . . . H5 H 0.3343 -0.1629 0.4854 0.066 Uiso 1 1 calc R . . C6 C 0.2746(3) -0.0956(4) 0.4122(2) 0.0425(14) Uani 1 1 d . . . C7 C 0.3584(5) 0.0263(5) 0.4712(3) 0.065(2) Uani 1 1 d . . . H7A H 0.3750 -0.0186 0.5004 0.097 Uiso 1 1 calc R . . H7B H 0.3377 0.0746 0.4861 0.097 Uiso 1 1 calc R . . H7C H 0.4016 0.0459 0.4613 0.097 Uiso 1 1 calc R . . C8 C 0.2608(3) 0.0317(3) 0.3687(2) 0.0296(12) Uani 1 1 d . . . C9 C 0.2681(3) 0.1280(3) 0.3566(2) 0.0348(12) Uani 1 1 d . . . H9A H 0.2730 0.1626 0.3909 0.042 Uiso 1 1 calc R . . H9B H 0.3133 0.1379 0.3460 0.042 Uiso 1 1 calc R . . C10 C 0.2116(3) 0.2273(3) 0.2742(2) 0.0295(11) Uani 1 1 d . . . H10A H 0.2640 0.2250 0.2742 0.035 Uiso 1 1 calc R . . H10B H 0.2045 0.2822 0.2915 0.035 Uiso 1 1 calc R . . C11 C 0.1552(3) 0.2200(3) 0.2133(2) 0.0305(12) Uani 1 1 d . . . C12 C 0.1326(4) 0.3800(4) 0.1881(3) 0.0473(15) Uani 1 1 d . . . H12A H 0.1018 0.4115 0.1541 0.071 Uiso 1 1 calc R . . H12B H 0.1860 0.3947 0.1973 0.071 Uiso 1 1 calc R . . H12C H 0.1168 0.3954 0.2203 0.071 Uiso 1 1 calc R . . C13 C 0.0699(3) 0.2487(4) 0.1264(3) 0.0413(14) Uani 1 1 d . . . C14 C 0.0181(4) 0.2870(5) 0.0762(3) 0.0550(18) Uani 1 1 d . . . H14 H 0.0145 0.3473 0.0710 0.066 Uiso 1 1 calc R . . C15 C -0.0276(4) 0.2291(5) 0.0347(3) 0.066(2) Uani 1 1 d . . . H15 H -0.0635 0.2509 0.0006 0.079 Uiso 1 1 calc R . . C16 C -0.0204(4) 0.1389(5) 0.0434(3) 0.063(2) Uani 1 1 d . . . H16 H -0.0518 0.1022 0.0145 0.076 Uiso 1 1 calc R . . C17 C 0.0312(4) 0.1020(4) 0.0929(2) 0.0471(16) Uani 1 1 d . . . H17 H 0.0353 0.0417 0.0979 0.057 Uiso 1 1 calc R . . C18 C 0.0766(3) 0.1584(3) 0.1348(2) 0.0332(12) Uani 1 1 d . . . C19 C 0.1343(3) 0.1711(4) 0.3319(2) 0.0342(12) Uani 1 1 d . . . H19A H 0.1547 0.2095 0.3653 0.041 Uiso 1 1 calc R . . H19B H 0.1197 0.1166 0.3456 0.041 Uiso 1 1 calc R . . C20 C 0.0627(3) 0.2128(3) 0.2888(2) 0.0330(12) Uani 1 1 d . . . C21 C 0.0601(3) 0.3049(4) 0.2901(3) 0.0445(15) Uani 1 1 d . . . H21 H 0.0991 0.3356 0.3181 0.053 Uiso 1 1 calc R . . C22 C 0.0000 0.3497(5) 0.2500 0.047(2) Uani 1 2 d S . . H22 H 0.0000 0.4105 0.2500 0.057 Uiso 1 2 calc SR . . C23 C 0.0000 0.1667(5) 0.2500 0.0295(16) Uani 1 2 d S . . C24 C 0.0000 0.0691(5) 0.2500 0.0293(16) Uani 1 2 d S . . C25 C 0.3125(3) 0.0437(3) 0.2126(2) 0.0326(12) Uani 1 1 d . . . C26 C 0.0995(3) -0.1205(3) 0.1720(2) 0.0341(13) 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 0.0245(4) 0.0234(4) 0.0259(4) -0.0017(3) 0.0091(3) -0.0011(3) Cl1 0.0406(8) 0.0689(11) 0.0391(9) 0.0107(7) 0.0121(6) -0.0025(8) Cl2 0.0554(19) 0.089(3) 0.0334(16) -0.0128(16) 0.0127(14) 0.0027(18) O1 0.0234(18) 0.0289(19) 0.044(2) 0.0012(16) 0.0144(16) -0.0001(15) O2 0.039(2) 0.030(2) 0.042(2) -0.0096(17) 0.0159(18) -0.0015(17) O3 0.0268(18) 0.039(2) 0.031(2) -0.0017(16) 0.0135(16) -0.0021(15) O4 0.093(5) 0.140(6) 0.121(6) 0.011(5) 0.045(4) 0.048(4) O5 0.160(7) 0.151(7) 0.080(5) 0.061(5) 0.012(4) -0.015(6) O6 0.101(4) 0.076(4) 0.064(3) -0.021(3) 0.016(3) -0.019(3) O7 0.075(4) 0.128(5) 0.082(4) -0.054(4) 0.040(3) -0.048(4) O8 0.103(4) 0.099(4) 0.042(3) -0.012(3) 0.038(3) -0.010(3) O9 0.103(4) 0.099(4) 0.042(3) -0.012(3) 0.038(3) -0.010(3) O10 0.103(4) 0.099(4) 0.042(3) -0.012(3) 0.038(3) -0.010(3) O11 0.103(4) 0.099(4) 0.042(3) -0.012(3) 0.038(3) -0.010(3) N1 0.028(2) 0.032(2) 0.031(2) 0.0020(19) 0.0126(19) 0.0034(19) N2 0.025(2) 0.030(2) 0.028(2) 0.0002(18) 0.0080(17) 0.0013(18) N3 0.029(2) 0.030(2) 0.027(2) -0.0009(18) 0.0098(18) 0.0006(19) N4 0.043(3) 0.042(3) 0.023(2) 0.004(2) 0.003(2) -0.007(2) N5 0.037(2) 0.031(2) 0.040(3) 0.006(2) 0.013(2) 0.000(2) N6 0.036(3) 0.085(4) 0.043(3) 0.016(3) 0.022(2) 0.008(3) N7 0.059(3) 0.092(4) 0.040(3) -0.022(3) 0.032(3) -0.013(3) N8 0.059(3) 0.043(3) 0.047(3) -0.018(2) 0.016(3) -0.010(3) N9 0.049(3) 0.048(3) 0.060(3) -0.019(3) 0.026(3) -0.017(2) C1 0.038(3) 0.029(3) 0.035(3) 0.004(2) 0.017(2) 0.003(2) C2 0.051(3) 0.040(3) 0.039(3) -0.003(3) 0.021(3) -0.004(3) C3 0.081(5) 0.043(4) 0.051(4) -0.002(3) 0.027(4) -0.010(4) C4 0.090(6) 0.045(4) 0.059(5) 0.019(3) 0.020(4) 0.003(4) C5 0.069(4) 0.059(4) 0.039(4) 0.013(3) 0.023(3) 0.000(4) C6 0.050(3) 0.050(4) 0.030(3) 0.004(3) 0.018(3) -0.005(3) C7 0.079(5) 0.073(5) 0.031(4) 0.000(3) 0.004(3) -0.024(4) C8 0.032(3) 0.029(3) 0.028(3) -0.002(2) 0.011(2) -0.002(2) C9 0.034(3) 0.038(3) 0.030(3) -0.005(2) 0.009(2) -0.004(2) C10 0.031(3) 0.024(2) 0.035(3) -0.001(2) 0.014(2) -0.002(2) C11 0.024(2) 0.027(3) 0.044(3) 0.000(2) 0.016(2) 0.004(2) C12 0.053(4) 0.033(3) 0.063(4) 0.010(3) 0.029(3) -0.002(3) C13 0.035(3) 0.039(3) 0.047(4) 0.010(3) 0.010(3) 0.002(3) C14 0.054(4) 0.057(4) 0.051(4) 0.023(3) 0.014(3) 0.006(3) C15 0.059(4) 0.077(5) 0.045(4) 0.018(4) -0.003(3) 0.005(4) C16 0.066(4) 0.068(5) 0.040(4) 0.005(3) -0.002(3) -0.010(4) C17 0.054(4) 0.048(4) 0.032(3) 0.005(3) 0.005(3) -0.011(3) C18 0.030(3) 0.038(3) 0.032(3) 0.001(2) 0.012(2) -0.004(2) C19 0.031(3) 0.032(3) 0.043(3) -0.009(2) 0.018(2) -0.005(2) C20 0.034(3) 0.030(3) 0.043(3) -0.005(2) 0.024(2) 0.002(2) C21 0.031(3) 0.033(3) 0.077(4) -0.018(3) 0.028(3) -0.005(2) C22 0.052(5) 0.021(4) 0.084(7) 0.000 0.042(5) 0.000 C23 0.030(4) 0.028(4) 0.040(4) 0.000 0.024(3) 0.000 C24 0.024(4) 0.038(4) 0.025(4) 0.000 0.006(3) 0.000 C25 0.034(3) 0.035(3) 0.031(3) 0.011(2) 0.015(2) 0.005(2) C26 0.040(3) 0.024(3) 0.032(3) -0.005(2) 0.005(2) 0.004(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 Ni1 O1 2.042(3) . ? Ni1 N3 2.048(4) . ? Ni1 N1 2.071(4) . ? Ni1 O2 2.085(4) . ? Ni1 O3 2.094(3) . ? Ni1 N2 2.144(4) . ? Cl1 O7 1.381(5) . ? Cl1 O4 1.398(6) . ? Cl1 O5 1.400(6) . ? Cl1 O6 1.444(5) . ? Cl2 O11 1.238(10) . ? Cl2 O9 1.417(10) . ? Cl2 O8 1.433(12) . ? Cl2 O10 1.528(13) . ? Cl2 O10 1.811(11) 7_556 ? O1 C24 1.262(5) . ? O2 C26 1.256(6) . ? O3 C25 1.250(6) . ? O9 O10 1.710(16) 7_556 ? O10 O10 1.238(18) 7_556 ? O10 O9 1.710(16) 7_556 ? O10 Cl2 1.811(11) 7_556 ? N1 C8 1.321(7) . ? N1 C1 1.389(7) . ? N2 C10 1.485(6) . ? N2 C9 1.487(6) . ? N2 C19 1.502(7) . ? N3 C11 1.333(7) . ? N3 C18 1.394(6) . ? N4 C8 1.343(7) . ? N4 C6 1.395(8) . ? N4 C7 1.461(7) . ? N5 C11 1.346(7) . ? N5 C13 1.407(7) . ? N5 C12 1.456(7) . ? N6 C25 1.334(7) . ? N6 H6A' 0.8600 . ? N6 H6B' 0.8600 . ? N7 C25 1.312(7) . ? N7 H7A' 0.8600 . ? N7 H7B' 0.8600 . ? N8 C26 1.329(7) . ? N8 H8A' 0.8600 . ? N8 H8B' 0.8600 . ? N9 C26 1.315(8) . ? N9 H9A' 0.8600 . ? N9 H9B' 0.8600 . ? C1 C6 1.399(8) . ? C1 C2 1.401(8) . ? C2 C3 1.373(9) . ? C2 H2 0.9300 . ? C3 C4 1.398(10) . ? C3 H3 0.9300 . ? C4 C5 1.382(10) . ? C4 H4 0.9300 . ? C5 C6 1.374(8) . ? C5 H5 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.517(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.496(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C18 1.395(8) . ? C13 C14 1.395(8) . ? C14 C15 1.390(10) . ? C14 H14 0.9300 . ? C15 C16 1.395(10) . ? C15 H15 0.9300 . ? C16 C17 1.376(8) . ? C16 H16 0.9300 . ? C17 C18 1.378(8) . ? C17 H17 0.9300 . ? C19 C20 1.516(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C23 1.405(6) . ? C20 C21 1.410(7) . ? C21 C22 1.381(7) . ? C21 H21 0.9300 . ? C22 C21 1.381(7) 2 ? C22 H22 0.9300 . ? C23 C20 1.405(6) 2 ? C23 C24 1.492(10) . ? C24 O1 1.262(5) 2 ? 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 O1 Ni1 N3 92.99(15) . . ? O1 Ni1 N1 88.31(15) . . ? N3 Ni1 N1 160.21(17) . . ? O1 Ni1 O2 91.18(15) . . ? N3 Ni1 O2 97.24(16) . . ? N1 Ni1 O2 102.47(16) . . ? O1 Ni1 O3 175.54(14) . . ? N3 Ni1 O3 91.23(15) . . ? N1 Ni1 O3 87.23(15) . . ? O2 Ni1 O3 89.73(14) . . ? O1 Ni1 N2 94.04(15) . . ? N3 Ni1 N2 80.90(16) . . ? N1 Ni1 N2 79.31(16) . . ? O2 Ni1 N2 174.54(16) . . ? O3 Ni1 N2 85.20(15) . . ? O7 Cl1 O4 112.5(5) . . ? O7 Cl1 O5 110.5(5) . . ? O4 Cl1 O5 108.7(6) . . ? O7 Cl1 O6 109.2(4) . . ? O4 Cl1 O6 109.5(4) . . ? O5 Cl1 O6 106.2(5) . . ? O11 Cl2 O9 125.8(7) . . ? O11 Cl2 O8 94.3(7) . . ? O9 Cl2 O8 117.4(7) . . ? O11 Cl2 O10 105.8(7) . . ? O9 Cl2 O10 104.7(6) . . ? O8 Cl2 O10 107.5(7) . . ? O11 Cl2 O10 126.5(7) . 7_556 ? O9 Cl2 O10 62.6(6) . 7_556 ? O8 Cl2 O10 131.2(6) . 7_556 ? O10 Cl2 O10 42.5(6) . 7_556 ? C24 O1 Ni1 141.5(4) . . ? C26 O2 Ni1 137.3(4) . . ? C25 O3 Ni1 135.3(3) . . ? Cl2 O9 O10 70.1(6) . 7_556 ? O10 O10 Cl2 81.1(11) 7_556 . ? O10 O10 O9 103.4(13) 7_556 7_556 ? Cl2 O10 O9 172.6(8) . 7_556 ? O10 O10 Cl2 56.4(9) 7_556 7_556 ? Cl2 O10 Cl2 137.5(6) . 7_556 ? O9 O10 Cl2 47.3(5) 7_556 7_556 ? C8 N1 C1 105.0(4) . . ? C8 N1 Ni1 111.3(3) . . ? C1 N1 Ni1 143.2(4) . . ? C10 N2 C9 111.0(4) . . ? C10 N2 C19 112.9(4) . . ? C9 N2 C19 108.5(4) . . ? C10 N2 Ni1 106.6(3) . . ? C9 N2 Ni1 106.6(3) . . ? C19 N2 Ni1 111.1(3) . . ? C11 N3 C18 106.1(4) . . ? C11 N3 Ni1 112.0(3) . . ? C18 N3 Ni1 140.4(3) . . ? C8 N4 C6 106.3(4) . . ? C8 N4 C7 128.9(5) . . ? C6 N4 C7 124.8(5) . . ? C11 N5 C13 106.6(4) . . ? C11 N5 C12 128.3(5) . . ? C13 N5 C12 124.9(5) . . ? C25 N6 H6A' 120.0 . . ? C25 N6 H6B' 120.0 . . ? H6A' N6 H6B' 120.0 . . ? C25 N7 H7A' 120.0 . . ? C25 N7 H7B' 120.0 . . ? H7A' N7 H7B' 120.0 . . ? C26 N8 H8A' 120.0 . . ? C26 N8 H8B' 120.0 . . ? H8A' N8 H8B' 120.0 . . ? C26 N9 H9A' 120.0 . . ? C26 N9 H9B' 120.0 . . ? H9A' N9 H9B' 120.0 . . ? N1 C1 C6 109.1(5) . . ? N1 C1 C2 130.5(5) . . ? C6 C1 C2 120.3(5) . . ? C3 C2 C1 117.5(6) . . ? C3 C2 H2 121.3 . . ? C1 C2 H2 121.3 . . ? C2 C3 C4 120.7(6) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 122.8(6) . . ? C5 C4 H4 118.6 . . ? C3 C4 H4 118.6 . . ? C6 C5 C4 115.9(6) . . ? C6 C5 H5 122.1 . . ? C4 C5 H5 122.1 . . ? C5 C6 N4 131.6(5) . . ? C5 C6 C1 122.7(6) . . ? N4 C6 C1 105.7(5) . . ? N4 C7 H7A 109.5 . . ? N4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 N4 113.8(4) . . ? N1 C8 C9 121.2(5) . . ? N4 C8 C9 125.0(5) . . ? N2 C9 C8 106.8(4) . . ? N2 C9 H9A 110.4 . . ? C8 C9 H9A 110.4 . . ? N2 C9 H9B 110.4 . . ? C8 C9 H9B 110.4 . . ? H9A C9 H9B 108.6 . . ? N2 C10 C11 107.1(4) . . ? N2 C10 H10A 110.3 . . ? C11 C10 H10A 110.3 . . ? N2 C10 H10B 110.3 . . ? C11 C10 H10B 110.3 . . ? H10A C10 H10B 108.5 . . ? N3 C11 N5 112.6(4) . . ? N3 C11 C10 120.7(4) . . ? N5 C11 C10 126.7(5) . . ? N5 C12 H12A 109.5 . . ? N5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 123.0(6) . . ? C18 C13 N5 106.1(5) . . ? C14 C13 N5 130.9(6) . . ? C15 C14 C13 115.5(6) . . ? C15 C14 H14 122.2 . . ? C13 C14 H14 122.2 . . ? C14 C15 C16 121.2(6) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C17 C16 C15 122.6(6) . . ? C17 C16 H16 118.7 . . ? C15 C16 H16 118.7 . . ? C16 C17 C18 117.0(6) . . ? C16 C17 H17 121.5 . . ? C18 C17 H17 121.5 . . ? C17 C18 N3 130.7(5) . . ? C17 C18 C13 120.7(5) . . ? N3 C18 C13 108.6(5) . . ? N2 C19 C20 114.2(4) . . ? N2 C19 H19A 108.7 . . ? C20 C19 H19A 108.7 . . ? N2 C19 H19B 108.7 . . ? C20 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C23 C20 C21 119.3(5) . . ? C23 C20 C19 125.0(5) . . ? C21 C20 C19 115.6(5) . . ? C22 C21 C20 120.3(6) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C21 120.5(7) . 2 ? C21 C22 H22 119.8 . . ? C21 C22 H22 119.8 2 . ? C20 C23 C20 119.8(7) . 2 ? C20 C23 C24 120.1(3) . . ? C20 C23 C24 120.1(3) 2 . ? O1 C24 O1 119.1(7) 2 . ? O1 C24 C23 120.4(3) 2 . ? O1 C24 C23 120.4(3) . . ? O3 C25 N7 123.0(5) . . ? O3 C25 N6 120.1(5) . . ? N7 C25 N6 117.0(5) . . ? O2 C26 N9 121.2(5) . . ? O2 C26 N8 120.1(6) . . ? N9 C26 N8 118.7(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.218 _refine_diff_density_min -1.357 _refine_diff_density_rms 0.191