# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'M. Albrecht' 'Sabrina Dehn' 'Roland Frohlich' 'Gerhard Raabe' _publ_contact_author_name M.Albrecht _publ_contact_author_address ; Institut fur Organische Chemie RWTH-Aachen Landoltweg 1 Aachen D-52074 GERMANY ; _publ_contact_author_email MARKUS.ALBRECHT@OC.RWTH-AACHEN.DE _publ_requested_journal 'Chemical Communications' _publ_section_title ; Structural diversity in the assembly of enantiopure helicate type nickel(II) complexes with bis(?-diketonate) ligands ; data_fro2892 _database_code_depnum_ccdc_archive 'CCDC 277819' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H54 Br4 Cl2 N2 Ni3 O16' _chemical_formula_weight 1637.73 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.030(2) _cell_length_b 19.345(2) _cell_length_c 14.077(2) _cell_angle_alpha 90.00 _cell_angle_beta 118.43(1) _cell_angle_gamma 90.00 _cell_volume 3359.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 3.355 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3864 _exptl_absorpt_correction_T_max 0.8502 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32419 _diffrn_reflns_av_R_equivalents 0.074 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.30 _reflns_number_total 12426 _reflns_number_gt 8619 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinwoski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+6.0617P] 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 riding _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 0.024(12) _refine_ls_number_reflns 12426 _refine_ls_number_parameters 831 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1011 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1592 _refine_ls_wR_factor_gt 0.1387 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.44658(9) 0.49880(5) 0.21977(9) 0.0450(3) Uani 1 1 d . A . Ni2 Ni 0.61745(10) 0.51811(6) 0.14508(10) 0.0428(2) Uani 1 1 d . A . Ni3 Ni 0.78916(9) 0.54257(5) 0.07339(9) 0.0457(3) Uani 1 1 d . A . O11 O 0.4327(5) 0.5381(3) 0.3437(5) 0.0485(15) Uani 1 1 d . . . C12 C 0.5110(8) 0.5568(4) 0.4324(8) 0.048(2) Uani 1 1 d . . . C13 C 0.6187(8) 0.5645(5) 0.4519(7) 0.050(2) Uani 1 1 d . . . H13 H 0.6701 0.5793 0.5223 0.060 Uiso 1 1 calc R . . C14 C 0.6565(7) 0.5531(4) 0.3806(7) 0.044(2) Uani 1 1 d . . . O15 O 0.6034(5) 0.5280(3) 0.2844(5) 0.0453(14) Uani 1 1 d . . . C16 C 0.7721(7) 0.5725(5) 0.4085(7) 0.048(2) Uani 1 1 d . A . H16 H 0.8075 0.5323 0.3931 0.058 Uiso 1 1 calc R . . O17 O 0.8357(6) 0.5929(4) 0.5181(5) 0.0644(18) Uani 1 1 d . A . C18 C 0.8695(13) 0.6621(8) 0.5215(11) 0.095(5) Uani 1 1 d . . . C19A C 0.775(4) 0.7034(18) 0.547(3) 0.068(12) Uani 0.37(5) 1 d P A 1 H19A H 0.7866 0.7534 0.5503 0.102 Uiso 0.37(5) 1 calc PR A 1 H19B H 0.7817 0.6872 0.6160 0.102 Uiso 0.37(5) 1 calc PR A 1 H19C H 0.7016 0.6929 0.4889 0.102 Uiso 0.37(5) 1 calc PR A 1 C20A C 0.968(3) 0.688(3) 0.600(3) 0.108(18) Uani 0.37(5) 1 d P A 1 H20A H 0.9623 0.7380 0.6071 0.162 Uiso 0.37(5) 1 calc PR A 1 H20B H 1.0244 0.6787 0.5788 0.162 Uiso 0.37(5) 1 calc PR A 1 H20C H 0.9882 0.6655 0.6693 0.162 Uiso 0.37(5) 1 calc PR A 1 C19B C 0.874(6) 0.7003(19) 0.600(4) 0.19(3) Uani 0.63(5) 1 d P A 2 H19D H 0.8401 0.7453 0.5715 0.281 Uiso 0.63(5) 1 calc PR A 2 H19E H 0.9494 0.7070 0.6547 0.281 Uiso 0.63(5) 1 calc PR A 2 H19F H 0.8344 0.6771 0.6330 0.281 Uiso 0.63(5) 1 calc PR A 2 C20B C 1.007(2) 0.642(2) 0.570(3) 0.15(2) Uani 0.63(5) 1 d P A 2 H20D H 1.0435 0.6820 0.5584 0.223 Uiso 0.63(5) 1 calc PR A 2 H20E H 1.0132 0.6021 0.5312 0.223 Uiso 0.63(5) 1 calc PR A 2 H20F H 1.0401 0.6320 0.6473 0.223 Uiso 0.63(5) 1 calc PR A 2 O21 O 0.8404(6) 0.6855(3) 0.4208(6) 0.0605(18) Uani 1 1 d . A . C22 C 0.7748(8) 0.6362(4) 0.3424(8) 0.050(2) Uani 1 1 d . . . H22 H 0.6998 0.6550 0.2995 0.060 Uiso 1 1 calc R A . C23 C 0.8202(7) 0.6170(4) 0.2654(7) 0.045(2) Uani 1 1 d . A . O24 O 0.7577(5) 0.5762(3) 0.1903(5) 0.0464(14) Uani 1 1 d . . . C25 C 0.9166(7) 0.6432(5) 0.2813(7) 0.049(2) Uani 1 1 d . . . H25 H 0.9478 0.6791 0.3331 0.058 Uiso 1 1 calc R A . C26 C 0.9746(7) 0.6212(4) 0.2269(8) 0.047(2) Uani 1 1 d . A . O27 O 0.9401(5) 0.5782(3) 0.1515(5) 0.0511(16) Uani 1 1 d . . . C31 C 0.4804(8) 0.5742(4) 0.5181(8) 0.043(2) Uani 1 1 d . . . C32 C 0.5549(8) 0.5844(5) 0.6249(8) 0.052(2) Uani 1 1 d . . . H32 H 0.6301 0.5806 0.6469 0.062 Uiso 1 1 calc R . . C33 C 0.5216(9) 0.6001(5) 0.7013(8) 0.061(3) Uani 1 1 d . . . H33 H 0.5739 0.6070 0.7748 0.073 Uiso 1 1 calc R . . C34 C 0.4149(10) 0.6056(5) 0.6709(9) 0.057(3) Uani 1 1 d . . . C35 C 0.3387(9) 0.5940(5) 0.5640(8) 0.057(2) Uani 1 1 d . . . H35 H 0.2635 0.5969 0.5425 0.069 Uiso 1 1 calc R . . C36 C 0.3721(8) 0.5781(5) 0.4887(8) 0.054(2) Uani 1 1 d . . . H36 H 0.3196 0.5698 0.4157 0.065 Uiso 1 1 calc R . . Br1 Br 0.36839(11) 0.62850(6) 0.77220(9) 0.0721(3) Uani 1 1 d . . . C41 C 1.0810(7) 0.6516(4) 0.2536(8) 0.046(2) Uani 1 1 d . . . C42 C 1.1302(7) 0.7065(4) 0.3255(8) 0.050(2) Uani 1 1 d . A . H42 H 1.0937 0.7263 0.3611 0.061 Uiso 1 1 calc R . . C43 C 1.2277(8) 0.7325(5) 0.3463(9) 0.054(2) Uani 1 1 d . . . H43 H 1.2589 0.7698 0.3953 0.064 Uiso 1 1 calc R A . C44 C 1.2812(8) 0.7039(5) 0.2949(8) 0.054(3) Uani 1 1 d . A . C45 C 1.2370(8) 0.6495(5) 0.2228(8) 0.050(2) Uani 1 1 d . . . H45 H 1.2738 0.6309 0.1868 0.061 Uiso 1 1 calc R A . C46 C 1.1397(7) 0.6235(5) 0.2047(7) 0.046(2) Uani 1 1 d . A . H46 H 1.1103 0.5851 0.1574 0.055 Uiso 1 1 calc R . . Br2 Br 1.41588(9) 0.74142(6) 0.31924(10) 0.0673(3) Uani 1 1 d . . . O51 O 0.2944(5) 0.4641(3) 0.1485(5) 0.0532(16) Uani 1 1 d . . . C52 C 0.2489(7) 0.4359(5) 0.0589(8) 0.048(2) Uani 1 1 d . . . C53 C 0.2884(8) 0.4342(5) -0.0178(9) 0.057(2) Uani 1 1 d . . . H53 H 0.2388 0.4218 -0.0901 0.068 Uiso 1 1 calc R . . C54 C 0.3916(8) 0.4490(5) 0.0053(8) 0.050(2) Uani 1 1 d . A . O55 O 0.4735(5) 0.4632(3) 0.0989(5) 0.0480(15) Uani 1 1 d . . . C56 C 0.4199(8) 0.4536(5) -0.0862(8) 0.054(2) Uani 1 1 d . . . H56 H 0.4333 0.5031 -0.0968 0.064 Uiso 1 1 calc R A . O57 O 0.3349(6) 0.4272(4) -0.1849(6) 0.074(2) Uani 1 1 d . A . C58 C 0.3728(10) 0.3769(6) -0.2288(9) 0.071(3) Uani 1 1 d . . . C59 C 0.3846(13) 0.4100(10) -0.3205(10) 0.123(6) Uani 1 1 d . A . H59A H 0.3129 0.4230 -0.3786 0.185 Uiso 1 1 calc R . . H59B H 0.4185 0.3771 -0.3481 0.185 Uiso 1 1 calc R . . H59C H 0.4301 0.4514 -0.2938 0.185 Uiso 1 1 calc R . . C60A C 0.312(2) 0.3125(14) -0.275(4) 0.108(11) Uani 0.68(9) 1 d P A 1 H60A H 0.3285 0.2792 -0.2164 0.162 Uiso 0.68(9) 1 calc PR A 1 H60B H 0.3340 0.2930 -0.3258 0.162 Uiso 0.68(9) 1 calc PR A 1 H60C H 0.2345 0.3223 -0.3123 0.162 Uiso 0.68(9) 1 calc PR A 1 C60B C 0.302(5) 0.309(3) -0.199(13) 0.13(5) Uani 0.32(9) 1 d P A 2 H60D H 0.2251 0.3211 -0.2299 0.197 Uiso 0.32(9) 1 calc PR A 2 H60E H 0.3333 0.3040 -0.1205 0.197 Uiso 0.32(9) 1 calc PR A 2 H60F H 0.3093 0.2655 -0.2302 0.197 Uiso 0.32(9) 1 calc PR A 2 O61 O 0.4799(6) 0.3580(3) -0.1473(6) 0.0642(18) Uani 1 1 d . A . C62 C 0.5198(8) 0.4111(5) -0.0641(8) 0.053(2) Uani 1 1 d . A . H62 H 0.5468 0.3880 0.0078 0.064 Uiso 1 1 calc R . . C63 C 0.6089(7) 0.4537(4) -0.0617(7) 0.046(2) Uani 1 1 d . . . O64 O 0.6363(4) 0.5052(3) 0.0063(5) 0.0426(13) Uani 1 1 d . A . C65 C 0.6554(8) 0.4379(5) -0.1261(9) 0.057(2) Uani 1 1 d . A . H65 H 0.6209 0.4029 -0.1788 0.068 Uiso 1 1 calc R . . C66 C 0.7484(8) 0.4682(4) -0.1219(8) 0.050(2) Uani 1 1 d . . . O67 O 0.8101(5) 0.5077(4) -0.0497(5) 0.0565(16) Uani 1 1 d . A . C71 C 0.1421(7) 0.4019(5) 0.0282(8) 0.051(2) Uani 1 1 d . . . C72 C 0.0979(8) 0.3507(5) -0.0504(8) 0.056(3) Uani 1 1 d . . . H72 H 0.1312 0.3398 -0.0936 0.067 Uiso 1 1 calc R . . C73 C 0.0060(8) 0.3155(5) -0.0660(10) 0.063(3) Uani 1 1 d . . . H73 H -0.0225 0.2794 -0.1178 0.076 Uiso 1 1 calc R . . C74 C -0.0439(8) 0.3330(5) -0.0059(9) 0.059(3) Uani 1 1 d . . . C75 C -0.0051(8) 0.3844(5) 0.0699(9) 0.060(3) Uani 1 1 d . . . H75 H -0.0415 0.3962 0.1099 0.071 Uiso 1 1 calc R . . C76 C 0.0888(8) 0.4191(5) 0.0872(9) 0.056(3) Uani 1 1 d . . . H76 H 0.1169 0.4549 0.1398 0.067 Uiso 1 1 calc R . . Br3 Br -0.16770(11) 0.28412(6) -0.02528(13) 0.0854(4) Uani 1 1 d . . . C81 C 0.7758(9) 0.4531(5) -0.2104(9) 0.056(2) Uani 1 1 d . A . C82 C 0.6990(9) 0.4260(5) -0.3104(8) 0.058(3) Uani 1 1 d . . . H82 H 0.6274 0.4166 -0.3230 0.070 Uiso 1 1 calc R A . C83 C 0.7260(9) 0.4133(5) -0.3882(8) 0.060(3) Uani 1 1 d . A . H83 H 0.6734 0.3969 -0.4569 0.072 Uiso 1 1 calc R . . C84 C 0.8326(10) 0.4246(5) -0.3665(9) 0.064(3) Uani 1 1 d . . . C85 C 0.9099(10) 0.4525(6) -0.2695(10) 0.070(3) Uani 1 1 d . A . H85 H 0.9818 0.4608 -0.2567 0.085 Uiso 1 1 calc R . . C86 C 0.8798(9) 0.4680(6) -0.1927(9) 0.067(3) Uani 1 1 d . . . H86 H 0.9304 0.4890 -0.1268 0.080 Uiso 1 1 calc R A . Br4 Br 0.87427(14) 0.39905(7) -0.47223(11) 0.0906(4) Uani 1 1 d . A . N91 N 0.4887(6) 0.4041(4) 0.3035(6) 0.0499(18) Uani 1 1 d . . . C92 C 0.4336(8) 0.3822(5) 0.3537(8) 0.055(2) Uani 1 1 d . A . H92 H 0.3800 0.4120 0.3542 0.065 Uiso 1 1 calc R . . C93 C 0.4497(9) 0.3198(5) 0.4039(9) 0.061(3) Uani 1 1 d . . . H93 H 0.4085 0.3068 0.4385 0.073 Uiso 1 1 calc R A . C94 C 0.5277(9) 0.2751(5) 0.4037(9) 0.062(3) Uani 1 1 d . A . H94 H 0.5403 0.2310 0.4370 0.075 Uiso 1 1 calc R . . C95 C 0.5859(9) 0.2972(5) 0.3535(9) 0.058(3) Uani 1 1 d . . . H95 H 0.6401 0.2685 0.3522 0.070 Uiso 1 1 calc R A . C96 C 0.5649(8) 0.3614(4) 0.3052(8) 0.052(2) Uani 1 1 d . A . H96 H 0.6063 0.3760 0.2716 0.062 Uiso 1 1 calc R . . N101 N 0.7451(6) 0.6377(4) -0.0098(6) 0.0484(18) Uani 1 1 d . . . C102 C 0.6644(8) 0.6766(5) -0.0144(8) 0.058(3) Uani 1 1 d . A . H102 H 0.6261 0.6609 0.0218 0.070 Uiso 1 1 calc R . . C103 C 0.6339(9) 0.7385(6) -0.0695(10) 0.073(3) Uani 1 1 d . . . H103 H 0.5781 0.7657 -0.0682 0.087 Uiso 1 1 calc R A . C104 C 0.6842(11) 0.7599(6) -0.1247(10) 0.077(3) Uani 1 1 d . A . H104 H 0.6628 0.8015 -0.1654 0.092 Uiso 1 1 calc R . . C105 C 0.7678(11) 0.7203(6) -0.1217(10) 0.079(3) Uani 1 1 d . . . H105 H 0.8054 0.7343 -0.1594 0.095 Uiso 1 1 calc R A . C106 C 0.7950(9) 0.6603(5) -0.0628(9) 0.067(3) Uani 1 1 d . A . H106 H 0.8529 0.6335 -0.0601 0.080 Uiso 1 1 calc R . . O111 O 0.3996(5) 0.5909(3) 0.1357(5) 0.0499(15) Uani 1 1 d . . . O112 O 0.5296(5) 0.6031(3) 0.0875(5) 0.0477(15) Uani 1 1 d . . . C113 C 0.4463(8) 0.6223(5) 0.0918(7) 0.047(2) Uani 1 1 d . A . C114 C 0.3981(9) 0.6899(5) 0.0402(9) 0.061(3) Uani 1 1 d . . . H11A H 0.4183 0.7254 0.0961 0.092 Uiso 1 1 calc R A . H11B H 0.3190 0.6857 0.0004 0.092 Uiso 1 1 calc R . . H11C H 0.4254 0.7029 -0.0098 0.092 Uiso 1 1 calc R . . O121 O 0.7068(5) 0.4327(3) 0.2028(5) 0.0491(15) Uani 1 1 d . . . O122 O 0.8399(5) 0.4499(3) 0.1597(5) 0.0523(16) Uani 1 1 d . . . C123 C 0.7916(8) 0.4153(5) 0.1994(8) 0.050(2) Uani 1 1 d . A . C124 C 0.8424(10) 0.3473(6) 0.2513(11) 0.072(3) Uani 1 1 d . . . H12A H 0.8571 0.3200 0.2011 0.108 Uiso 1 1 calc R A . H12B H 0.7926 0.3218 0.2691 0.108 Uiso 1 1 calc R . . H12C H 0.9104 0.3560 0.3175 0.108 Uiso 1 1 calc R . . C1 C 1.0963(13) 0.4687(8) -0.6515(13) 0.106(5) Uani 1 1 d . . . H1A H 1.1394 0.5077 -0.6563 0.127 Uiso 1 1 calc R . . H1B H 1.0286 0.4654 -0.7210 0.127 Uiso 1 1 calc R . . Cl1 Cl 1.1703(4) 0.3916(3) -0.6280(4) 0.1476(17) Uani 1 1 d . . . Cl2 Cl 1.0652(5) 0.4838(3) -0.5475(5) 0.1553(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0439(7) 0.0464(6) 0.0503(7) -0.0084(5) 0.0270(6) -0.0045(5) Ni2 0.0413(5) 0.0416(5) 0.0503(6) -0.0052(4) 0.0257(5) -0.0011(4) Ni3 0.0431(6) 0.0465(6) 0.0517(7) -0.0061(5) 0.0260(6) -0.0031(5) O11 0.052(4) 0.049(3) 0.049(4) -0.005(3) 0.028(3) 0.001(3) C12 0.063(6) 0.034(4) 0.054(6) -0.003(4) 0.034(5) 0.000(4) C13 0.050(6) 0.054(5) 0.044(5) -0.003(4) 0.021(5) -0.010(4) C14 0.048(5) 0.037(4) 0.045(5) -0.003(4) 0.019(5) -0.004(4) O15 0.035(3) 0.051(3) 0.051(4) -0.008(3) 0.022(3) -0.011(3) C16 0.044(5) 0.059(5) 0.044(5) 0.001(4) 0.021(4) 0.009(4) O17 0.059(4) 0.077(4) 0.048(4) -0.014(3) 0.018(3) -0.012(4) C18 0.114(12) 0.110(10) 0.064(9) -0.041(7) 0.045(9) -0.057(9) C19A 0.10(3) 0.065(18) 0.06(2) -0.040(16) 0.05(2) -0.010(18) C20A 0.07(3) 0.18(5) 0.06(3) -0.03(3) 0.02(2) 0.03(3) C19B 0.35(10) 0.15(3) 0.12(3) -0.06(3) 0.16(5) -0.08(5) C20B 0.068(19) 0.20(4) 0.11(2) 0.02(2) -0.012(17) -0.03(2) O21 0.067(5) 0.060(4) 0.067(5) -0.026(3) 0.041(4) -0.022(3) C22 0.049(5) 0.042(5) 0.067(6) -0.015(4) 0.034(5) -0.013(4) C23 0.048(5) 0.036(4) 0.058(6) -0.002(4) 0.031(5) -0.003(4) O24 0.046(4) 0.047(3) 0.049(4) -0.005(3) 0.025(3) -0.011(3) C25 0.039(5) 0.054(5) 0.053(6) -0.010(4) 0.022(5) -0.006(4) C26 0.049(5) 0.037(4) 0.054(6) 0.002(4) 0.023(5) 0.000(4) O27 0.047(4) 0.044(3) 0.064(4) -0.012(3) 0.028(3) -0.012(3) C31 0.052(6) 0.033(4) 0.056(6) 0.001(4) 0.035(5) 0.006(4) C32 0.052(6) 0.057(6) 0.050(6) -0.010(5) 0.027(5) 0.000(4) C33 0.068(7) 0.069(6) 0.044(6) -0.004(5) 0.024(6) -0.004(5) C34 0.073(8) 0.055(6) 0.061(7) 0.000(5) 0.046(6) 0.002(5) C35 0.056(6) 0.073(6) 0.051(6) -0.003(5) 0.033(6) -0.005(5) C36 0.058(7) 0.061(6) 0.047(6) -0.002(5) 0.029(5) 0.000(5) Br1 0.0974(9) 0.0727(7) 0.0689(7) -0.0020(6) 0.0580(7) 0.0015(6) C41 0.037(5) 0.046(5) 0.058(6) 0.002(4) 0.024(5) -0.001(4) C42 0.049(6) 0.045(5) 0.072(7) -0.007(5) 0.041(5) 0.005(4) C43 0.049(6) 0.048(5) 0.071(7) -0.007(5) 0.035(5) -0.010(4) C44 0.045(6) 0.057(6) 0.061(7) 0.002(5) 0.026(5) -0.015(5) C45 0.055(6) 0.048(5) 0.055(6) 0.003(4) 0.032(5) 0.002(4) C46 0.045(5) 0.045(5) 0.047(5) 0.000(4) 0.022(5) -0.002(4) Br2 0.0520(6) 0.0776(7) 0.0818(8) -0.0170(6) 0.0395(6) -0.0185(5) O51 0.048(4) 0.063(4) 0.052(4) -0.013(3) 0.028(4) -0.010(3) C52 0.039(5) 0.050(5) 0.057(6) -0.006(5) 0.025(5) -0.003(4) C53 0.048(6) 0.064(6) 0.064(7) -0.015(5) 0.031(5) -0.007(5) C54 0.056(6) 0.053(5) 0.048(6) -0.005(4) 0.030(5) 0.001(4) O55 0.051(4) 0.052(3) 0.046(4) -0.005(3) 0.028(3) -0.003(3) C56 0.050(6) 0.051(5) 0.056(6) -0.010(4) 0.022(5) -0.002(4) O57 0.054(4) 0.110(6) 0.053(4) -0.021(4) 0.020(4) 0.001(4) C58 0.076(8) 0.072(7) 0.057(7) -0.023(6) 0.025(7) -0.018(6) C59 0.131(13) 0.180(17) 0.054(8) 0.016(10) 0.041(9) 0.035(12) C60A 0.102(18) 0.100(16) 0.09(2) -0.008(14) 0.016(15) -0.043(13) C60B 0.09(4) 0.08(3) 0.18(10) -0.03(4) 0.02(5) -0.04(3) O61 0.074(5) 0.052(4) 0.067(5) -0.013(3) 0.034(4) -0.004(3) C62 0.053(6) 0.058(5) 0.053(6) -0.006(4) 0.029(5) -0.007(4) C63 0.041(5) 0.043(5) 0.054(6) 0.000(4) 0.024(5) -0.004(4) O64 0.042(3) 0.038(3) 0.051(3) -0.002(3) 0.025(3) -0.001(3) C65 0.052(6) 0.062(6) 0.066(7) -0.013(5) 0.035(5) -0.001(5) C66 0.054(6) 0.043(5) 0.056(6) -0.010(5) 0.030(5) 0.002(4) O67 0.053(4) 0.067(4) 0.057(4) -0.011(4) 0.033(3) -0.001(3) C71 0.038(5) 0.052(5) 0.067(6) -0.004(5) 0.028(5) 0.000(4) C72 0.048(6) 0.056(6) 0.070(7) -0.015(5) 0.034(5) -0.015(5) C73 0.042(6) 0.061(6) 0.076(7) -0.017(5) 0.020(6) -0.006(5) C74 0.054(6) 0.044(5) 0.079(7) -0.013(5) 0.032(6) -0.004(5) C75 0.060(7) 0.058(6) 0.074(7) -0.018(5) 0.043(6) -0.008(5) C76 0.046(6) 0.051(5) 0.074(7) -0.024(5) 0.031(5) -0.017(4) Br3 0.0699(8) 0.0869(8) 0.1137(11) -0.0318(7) 0.0552(8) -0.0349(6) C81 0.063(7) 0.050(5) 0.067(7) -0.004(5) 0.042(6) -0.001(5) C82 0.070(7) 0.052(5) 0.055(6) -0.012(5) 0.032(6) -0.003(5) C83 0.084(8) 0.054(5) 0.048(6) -0.006(4) 0.037(6) -0.006(5) C84 0.098(9) 0.047(5) 0.067(8) 0.006(5) 0.055(7) 0.007(6) C85 0.074(8) 0.083(8) 0.073(8) -0.001(6) 0.050(7) -0.001(6) C86 0.065(7) 0.084(7) 0.069(7) -0.007(6) 0.047(6) -0.008(6) Br4 0.1343(12) 0.0879(8) 0.0853(9) 0.0024(7) 0.0811(10) 0.0127(8) N91 0.056(5) 0.050(4) 0.049(5) -0.001(4) 0.030(4) -0.005(4) C92 0.055(6) 0.055(5) 0.058(6) -0.013(5) 0.030(5) -0.011(5) C93 0.074(7) 0.055(6) 0.059(7) 0.005(5) 0.036(6) -0.007(5) C94 0.082(8) 0.041(5) 0.071(7) -0.005(5) 0.041(6) -0.010(5) C95 0.064(7) 0.046(5) 0.070(7) -0.005(5) 0.037(6) 0.003(5) C96 0.062(6) 0.046(5) 0.066(7) -0.012(5) 0.045(6) 0.000(4) N101 0.052(5) 0.047(4) 0.050(5) -0.003(3) 0.027(4) -0.011(4) C102 0.046(6) 0.061(6) 0.057(6) 0.001(5) 0.015(5) -0.005(5) C103 0.069(7) 0.059(6) 0.082(8) 0.010(6) 0.029(7) 0.003(6) C104 0.083(8) 0.062(7) 0.079(8) 0.008(6) 0.033(7) -0.008(6) C105 0.088(9) 0.081(8) 0.072(8) 0.003(6) 0.042(7) -0.018(7) C106 0.056(7) 0.063(6) 0.075(8) 0.012(6) 0.026(6) -0.004(5) O111 0.054(4) 0.046(3) 0.058(4) 0.003(3) 0.033(4) 0.007(3) O112 0.044(4) 0.045(3) 0.063(4) -0.002(3) 0.033(3) 0.002(3) C113 0.055(6) 0.047(5) 0.048(5) -0.004(4) 0.031(5) -0.003(4) C114 0.060(7) 0.051(5) 0.076(7) 0.001(5) 0.036(6) 0.004(5) O121 0.042(4) 0.057(4) 0.052(4) 0.001(3) 0.025(3) 0.001(3) O122 0.048(4) 0.057(4) 0.058(4) -0.002(3) 0.030(4) 0.001(3) C123 0.054(6) 0.043(5) 0.053(6) -0.006(4) 0.027(5) -0.003(4) C124 0.070(7) 0.067(7) 0.100(9) 0.022(6) 0.059(7) 0.020(6) C1 0.096(11) 0.112(11) 0.111(12) 0.025(9) 0.050(10) -0.002(9) Cl1 0.140(4) 0.162(4) 0.137(4) 0.031(3) 0.062(3) 0.044(3) Cl2 0.146(4) 0.178(5) 0.145(4) 0.006(4) 0.072(4) 0.024(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 Ni1 O51 1.994(6) . ? Ni1 O11 1.996(6) . ? Ni1 O15 2.021(6) . ? Ni1 O55 2.031(6) . ? Ni1 O111 2.067(6) . ? Ni1 N91 2.105(7) . ? Ni2 O112 1.982(6) . ? Ni2 O121 1.998(6) . ? Ni2 O15 2.071(6) . ? Ni2 O24 2.086(6) . ? Ni2 O55 2.094(6) . ? Ni2 O64 2.107(6) . ? Ni3 O27 1.988(6) . ? Ni3 O24 2.004(6) . ? Ni3 O67 2.007(6) . ? Ni3 O64 2.021(6) . ? Ni3 O122 2.091(7) . ? Ni3 N101 2.109(8) . ? O11 C12 1.261(11) . ? C12 C13 1.408(13) . ? C12 C31 1.499(12) . ? C13 C14 1.360(12) . ? C14 O15 1.289(10) . ? C14 C16 1.523(12) . ? C16 O17 1.422(11) . ? C16 C22 1.554(13) . ? O17 C18 1.414(15) . ? C18 C19B 1.31(3) . ? C18 O21 1.352(15) . ? C18 C20A 1.39(4) . ? C18 C19A 1.73(4) . ? C18 C20B 1.75(4) . ? O21 C22 1.418(10) . ? C22 C23 1.541(12) . ? C23 O24 1.275(10) . ? C23 C25 1.359(12) . ? C25 C26 1.423(12) . ? C26 O27 1.250(10) . ? C26 C41 1.476(12) . ? C31 C36 1.373(13) . ? C31 C32 1.377(13) . ? C32 C33 1.396(13) . ? C33 C34 1.350(15) . ? C34 C35 1.388(14) . ? C34 Br1 1.883(9) . ? C35 C36 1.382(13) . ? C41 C42 1.403(13) . ? C41 C46 1.410(12) . ? C42 C43 1.351(12) . ? C43 C44 1.383(13) . ? C44 C45 1.386(14) . ? C44 Br2 1.897(9) . ? C45 C46 1.360(13) . ? O51 C52 1.237(11) . ? C52 C53 1.429(13) . ? C52 C71 1.499(12) . ? C53 C54 1.355(13) . ? C54 O55 1.299(11) . ? C54 C56 1.520(13) . ? C56 O57 1.428(12) . ? C56 C62 1.525(13) . ? O57 C58 1.386(13) . ? C58 O61 1.437(14) . ? C58 C60A 1.47(3) . ? C58 C59 1.519(18) . ? C58 C60B 1.81(11) . ? O61 C62 1.454(11) . ? C62 C63 1.484(12) . ? C63 O64 1.308(10) . ? C63 C65 1.379(13) . ? C65 C66 1.406(13) . ? C66 O67 1.236(11) . ? C66 C81 1.496(13) . ? C71 C72 1.393(13) . ? C71 C76 1.398(13) . ? C72 C73 1.381(13) . ? C73 C74 1.372(14) . ? C74 C75 1.368(14) . ? C74 Br3 1.880(10) . ? C75 C76 1.393(13) . ? C81 C86 1.388(14) . ? C81 C82 1.406(14) . ? C82 C83 1.341(13) . ? C83 C84 1.393(15) . ? C84 C85 1.387(16) . ? C84 Br4 1.905(10) . ? C85 C86 1.368(14) . ? N91 C92 1.340(11) . ? N91 C96 1.343(11) . ? C92 C93 1.363(14) . ? C93 C94 1.395(15) . ? C94 C95 1.378(14) . ? C95 C96 1.377(13) . ? N101 C106 1.317(12) . ? N101 C102 1.336(12) . ? C102 C103 1.380(15) . ? C103 C104 1.339(16) . ? C104 C105 1.385(17) . ? C105 C106 1.370(16) . ? O111 C113 1.251(10) . ? O112 C113 1.254(10) . ? C113 C114 1.492(14) . ? O121 C123 1.259(11) . ? O122 C123 1.258(11) . ? C123 C124 1.509(14) . ? C1 Cl2 1.741(16) . ? C1 Cl1 1.755(16) . ? 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 O51 Ni1 O11 92.4(3) . . ? O51 Ni1 O15 175.1(2) . . ? O11 Ni1 O15 92.2(2) . . ? O51 Ni1 O55 92.6(3) . . ? O11 Ni1 O55 174.9(3) . . ? O15 Ni1 O55 82.9(2) . . ? O51 Ni1 O111 91.7(3) . . ? O11 Ni1 O111 92.0(2) . . ? O15 Ni1 O111 89.9(2) . . ? O55 Ni1 O111 87.1(2) . . ? O51 Ni1 N91 86.4(3) . . ? O11 Ni1 N91 87.7(3) . . ? O15 Ni1 N91 92.1(3) . . ? O55 Ni1 N91 93.4(3) . . ? O111 Ni1 N91 178.0(3) . . ? O112 Ni2 O121 179.6(3) . . ? O112 Ni2 O15 89.4(2) . . ? O121 Ni2 O15 90.9(2) . . ? O112 Ni2 O24 89.4(2) . . ? O121 Ni2 O24 90.2(2) . . ? O15 Ni2 O24 99.3(2) . . ? O112 Ni2 O55 88.5(2) . . ? O121 Ni2 O55 91.8(2) . . ? O15 Ni2 O55 80.1(2) . . ? O24 Ni2 O55 177.9(3) . . ? O112 Ni2 O64 92.7(2) . . ? O121 Ni2 O64 87.0(2) . . ? O15 Ni2 O64 177.9(3) . . ? O24 Ni2 O64 80.2(2) . . ? O55 Ni2 O64 100.4(2) . . ? O27 Ni3 O24 91.5(3) . . ? O27 Ni3 O67 92.2(3) . . ? O24 Ni3 O67 176.2(3) . . ? O27 Ni3 O64 175.1(3) . . ? O24 Ni3 O64 84.3(2) . . ? O67 Ni3 O64 92.0(2) . . ? O27 Ni3 O122 89.9(3) . . ? O24 Ni3 O122 87.1(2) . . ? O67 Ni3 O122 93.7(3) . . ? O64 Ni3 O122 87.5(2) . . ? O27 Ni3 N101 87.6(3) . . ? O24 Ni3 N101 93.0(3) . . ? O67 Ni3 N101 86.5(3) . . ? O64 Ni3 N101 95.0(3) . . ? O122 Ni3 N101 177.4(3) . . ? C12 O11 Ni1 125.0(6) . . ? O11 C12 C13 124.9(8) . . ? O11 C12 C31 114.3(8) . . ? C13 C12 C31 120.7(9) . . ? C14 C13 C12 126.7(9) . . ? O15 C14 C13 127.1(8) . . ? O15 C14 C16 112.1(7) . . ? C13 C14 C16 120.8(8) . . ? C14 O15 Ni1 122.6(5) . . ? C14 O15 Ni2 139.6(5) . . ? Ni1 O15 Ni2 97.0(3) . . ? O17 C16 C14 112.9(7) . . ? O17 C16 C22 104.4(7) . . ? C14 C16 C22 111.6(7) . . ? C18 O17 C16 109.1(8) . . ? C19B C18 O21 125(2) . . ? C19B C18 C20A 60(3) . . ? O21 C18 C20A 114(3) . . ? C19B C18 O17 116.3(19) . . ? O21 C18 O17 110.6(9) . . ? C20A C18 O17 124(3) . . ? C19B C18 C19A 45(3) . . ? O21 C18 C19A 100.6(18) . . ? C20A C18 C19A 104(2) . . ? O17 C18 C19A 99.5(15) . . ? C19B C18 C20B 101(3) . . ? O21 C18 C20B 102.0(15) . . ? C20A C18 C20B 43.4(19) . . ? O17 C18 C20B 95.4(17) . . ? C19A C18 C20B 146.3(19) . . ? C18 O21 C22 110.6(8) . . ? O21 C22 C23 112.2(7) . . ? O21 C22 C16 105.0(7) . . ? C23 C22 C16 111.5(7) . . ? O24 C23 C25 127.2(8) . . ? O24 C23 C22 112.4(7) . . ? C25 C23 C22 120.5(8) . . ? C23 O24 Ni3 123.3(5) . . ? C23 O24 Ni2 139.7(5) . . ? Ni3 O24 Ni2 96.8(3) . . ? C23 C25 C26 125.5(8) . . ? O27 C26 C25 124.5(8) . . ? O27 C26 C41 114.6(8) . . ? C25 C26 C41 120.8(8) . . ? C26 O27 Ni3 125.5(6) . . ? C36 C31 C32 118.5(8) . . ? C36 C31 C12 118.0(9) . . ? C32 C31 C12 123.4(8) . . ? C31 C32 C33 120.9(9) . . ? C34 C33 C32 120.0(10) . . ? C33 C34 C35 119.8(9) . . ? C33 C34 Br1 120.6(9) . . ? C35 C34 Br1 119.6(8) . . ? C36 C35 C34 120.0(10) . . ? C31 C36 C35 120.8(10) . . ? C42 C41 C46 116.3(8) . . ? C42 C41 C26 125.2(8) . . ? C46 C41 C26 118.5(8) . . ? C43 C42 C41 122.5(8) . . ? C42 C43 C44 118.9(9) . . ? C43 C44 C45 121.4(9) . . ? C43 C44 Br2 119.6(7) . . ? C45 C44 Br2 118.9(7) . . ? C46 C45 C44 118.5(9) . . ? C45 C46 C41 122.2(9) . . ? C52 O51 Ni1 124.8(6) . . ? O51 C52 C53 125.7(8) . . ? O51 C52 C71 116.5(8) . . ? C53 C52 C71 117.8(9) . . ? C54 C53 C52 124.6(9) . . ? O55 C54 C53 128.0(8) . . ? O55 C54 C56 112.7(8) . . ? C53 C54 C56 119.2(9) . . ? C54 O55 Ni1 119.6(5) . . ? C54 O55 Ni2 132.7(6) . . ? Ni1 O55 Ni2 96.0(3) . . ? O57 C56 C54 111.7(8) . . ? O57 C56 C62 105.4(7) . . ? C54 C56 C62 112.4(8) . . ? C58 O57 C56 111.4(8) . . ? O57 C58 O61 107.5(8) . . ? O57 C58 C60A 122(2) . . ? O61 C58 C60A 107.4(14) . . ? O57 C58 C59 107.7(11) . . ? O61 C58 C59 106.9(10) . . ? C60A C58 C59 105(2) . . ? O57 C58 C60B 92(4) . . ? O61 C58 C60B 96(3) . . ? C60A C58 C60B 39(3) . . ? C59 C58 C60B 143(5) . . ? C58 O61 C62 108.6(7) . . ? O61 C62 C63 114.0(7) . . ? O61 C62 C56 104.6(7) . . ? C63 C62 C56 112.8(8) . . ? O64 C63 C65 125.7(8) . . ? O64 C63 C62 113.0(7) . . ? C65 C63 C62 121.3(8) . . ? C63 O64 Ni3 119.4(5) . . ? C63 O64 Ni2 130.3(5) . . ? Ni3 O64 Ni2 95.6(2) . . ? C63 C65 C66 127.0(9) . . ? O67 C66 C65 124.3(8) . . ? O67 C66 C81 116.6(9) . . ? C65 C66 C81 119.1(9) . . ? C66 O67 Ni3 125.8(6) . . ? C72 C71 C76 118.7(8) . . ? C72 C71 C52 123.1(8) . . ? C76 C71 C52 118.0(8) . . ? C73 C72 C71 120.4(9) . . ? C74 C73 C72 119.5(10) . . ? C75 C74 C73 122.0(9) . . ? C75 C74 Br3 118.4(8) . . ? C73 C74 Br3 119.5(8) . . ? C74 C75 C76 118.6(9) . . ? C75 C76 C71 120.7(9) . . ? C86 C81 C82 119.7(9) . . ? C86 C81 C66 118.4(10) . . ? C82 C81 C66 121.9(9) . . ? C83 C82 C81 120.4(10) . . ? C82 C83 C84 118.9(10) . . ? C85 C84 C83 122.1(9) . . ? C85 C84 Br4 118.9(9) . . ? C83 C84 Br4 119.0(8) . . ? C86 C85 C84 118.2(11) . . ? C85 C86 C81 120.5(11) . . ? C92 N91 C96 116.7(8) . . ? C92 N91 Ni1 119.5(7) . . ? C96 N91 Ni1 123.7(6) . . ? N91 C92 C93 123.9(10) . . ? C92 C93 C94 119.0(10) . . ? C95 C94 C93 117.8(9) . . ? C96 C95 C94 119.5(9) . . ? N91 C96 C95 123.0(9) . . ? C106 N101 C102 116.9(9) . . ? C106 N101 Ni3 120.7(7) . . ? C102 N101 Ni3 122.4(6) . . ? N101 C102 C103 123.1(10) . . ? C104 C103 C102 119.1(12) . . ? C103 C104 C105 118.9(11) . . ? C106 C105 C104 118.4(11) . . ? N101 C106 C105 123.6(11) . . ? C113 O111 Ni1 127.0(6) . . ? C113 O112 Ni2 129.6(6) . . ? O111 C113 O112 126.8(9) . . ? O111 C113 C114 116.3(8) . . ? O112 C113 C114 116.9(8) . . ? C123 O121 Ni2 128.8(6) . . ? C123 O122 Ni3 127.4(6) . . ? O122 C123 O121 126.5(8) . . ? O122 C123 C124 116.7(9) . . ? O121 C123 C124 116.8(9) . . ? Cl2 C1 Cl1 110.3(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O51 Ni1 O11 C12 164.9(7) . . . . ? O15 Ni1 O11 C12 -13.4(7) . . . . ? O55 Ni1 O11 C12 -24(3) . . . . ? O111 Ni1 O11 C12 -103.4(7) . . . . ? N91 Ni1 O11 C12 78.6(7) . . . . ? Ni1 O11 C12 C13 11.8(12) . . . . ? Ni1 O11 C12 C31 -170.9(5) . . . . ? O11 C12 C13 C14 -0.4(15) . . . . ? C31 C12 C13 C14 -177.5(8) . . . . ? C12 C13 C14 O15 -5.8(15) . . . . ? C12 C13 C14 C16 172.0(8) . . . . ? C13 C14 O15 Ni1 -0.7(12) . . . . ? C16 C14 O15 Ni1 -178.6(5) . . . . ? C13 C14 O15 Ni2 166.2(7) . . . . ? C16 C14 O15 Ni2 -11.7(12) . . . . ? O51 Ni1 O15 C14 -151(3) . . . . ? O11 Ni1 O15 C14 7.9(6) . . . . ? O55 Ni1 O15 C14 -173.0(6) . . . . ? O111 Ni1 O15 C14 99.9(6) . . . . ? N91 Ni1 O15 C14 -79.9(6) . . . . ? O51 Ni1 O15 Ni2 37(3) . . . . ? O11 Ni1 O15 Ni2 -163.5(2) . . . . ? O55 Ni1 O15 Ni2 15.5(2) . . . . ? O111 Ni1 O15 Ni2 -71.6(2) . . . . ? N91 Ni1 O15 Ni2 108.7(3) . . . . ? O112 Ni2 O15 C14 -95.5(8) . . . . ? O121 Ni2 O15 C14 84.3(8) . . . . ? O24 Ni2 O15 C14 -6.1(9) . . . . ? O55 Ni2 O15 C14 176.0(9) . . . . ? O64 Ni2 O15 C14 72(7) . . . . ? O112 Ni2 O15 Ni1 73.5(3) . . . . ? O121 Ni2 O15 Ni1 -106.8(3) . . . . ? O24 Ni2 O15 Ni1 162.8(2) . . . . ? O55 Ni2 O15 Ni1 -15.1(2) . . . . ? O64 Ni2 O15 Ni1 -119(7) . . . . ? O15 C14 C16 O17 -173.3(7) . . . . ? C13 C14 C16 O17 8.6(12) . . . . ? O15 C14 C16 C22 69.5(9) . . . . ? C13 C14 C16 C22 -108.6(9) . . . . ? C14 C16 O17 C18 -118.4(10) . . . . ? C22 C16 O17 C18 3.0(11) . . . . ? C16 O17 C18 C19B 144(4) . . . . ? C16 O17 C18 O21 -5.9(14) . . . . ? C16 O17 C18 C20A -146(2) . . . . ? C16 O17 C18 C19A 99.3(17) . . . . ? C16 O17 C18 C20B -111.0(16) . . . . ? C19B C18 O21 C22 -140(4) . . . . ? C20A C18 O21 C22 151(3) . . . . ? O17 C18 O21 C22 6.5(14) . . . . ? C19A C18 O21 C22 -98.1(15) . . . . ? C20B C18 O21 C22 107.0(18) . . . . ? C18 O21 C22 C23 -125.6(10) . . . . ? C18 O21 C22 C16 -4.3(11) . . . . ? O17 C16 C22 O21 0.7(9) . . . . ? C14 C16 C22 O21 122.9(7) . . . . ? O17 C16 C22 C23 122.4(8) . . . . ? C14 C16 C22 C23 -115.3(8) . . . . ? O21 C22 C23 O24 -175.6(7) . . . . ? C16 C22 C23 O24 66.9(10) . . . . ? O21 C22 C23 C25 4.3(12) . . . . ? C16 C22 C23 C25 -113.2(9) . . . . ? C25 C23 O24 Ni3 -1.5(12) . . . . ? C22 C23 O24 Ni3 178.4(5) . . . . ? C25 C23 O24 Ni2 172.2(7) . . . . ? C22 C23 O24 Ni2 -7.9(12) . . . . ? O27 Ni3 O24 C23 11.8(7) . . . . ? O67 Ni3 O24 C23 -157(4) . . . . ? O64 Ni3 O24 C23 -170.6(7) . . . . ? O122 Ni3 O24 C23 101.6(7) . . . . ? N101 Ni3 O24 C23 -75.8(7) . . . . ? O27 Ni3 O24 Ni2 -164.1(3) . . . . ? O67 Ni3 O24 Ni2 27(4) . . . . ? O64 Ni3 O24 Ni2 13.5(2) . . . . ? O122 Ni3 O24 Ni2 -74.3(3) . . . . ? N101 Ni3 O24 Ni2 108.2(3) . . . . ? O112 Ni2 O24 C23 79.4(9) . . . . ? O121 Ni2 O24 C23 -100.9(9) . . . . ? O15 Ni2 O24 C23 -9.9(9) . . . . ? O55 Ni2 O24 C23 66(8) . . . . ? O64 Ni2 O24 C23 172.2(9) . . . . ? O112 Ni2 O24 Ni3 -105.9(3) . . . . ? O121 Ni2 O24 Ni3 73.9(3) . . . . ? O15 Ni2 O24 Ni3 164.8(2) . . . . ? O55 Ni2 O24 Ni3 -120(7) . . . . ? O64 Ni2 O24 Ni3 -13.1(2) . . . . ? O24 C23 C25 C26 -10.6(15) . . . . ? C22 C23 C25 C26 169.5(9) . . . . ? C23 C25 C26 O27 5.4(15) . . . . ? C23 C25 C26 C41 -177.7(9) . . . . ? C25 C26 O27 Ni3 11.0(12) . . . . ? C41 C26 O27 Ni3 -166.1(6) . . . . ? O24 Ni3 O27 C26 -16.5(7) . . . . ? O67 Ni3 O27 C26 162.7(7) . . . . ? O64 Ni3 O27 C26 -46(3) . . . . ? O122 Ni3 O27 C26 -103.6(7) . . . . ? N101 Ni3 O27 C26 76.3(7) . . . . ? O11 C12 C31 C36 -9.4(11) . . . . ? C13 C12 C31 C36 168.1(9) . . . . ? O11 C12 C31 C32 168.8(8) . . . . ? C13 C12 C31 C32 -13.8(13) . . . . ? C36 C31 C32 C33 -1.6(14) . . . . ? C12 C31 C32 C33 -179.7(8) . . . . ? C31 C32 C33 C34 -0.1(15) . . . . ? C32 C33 C34 C35 1.5(15) . . . . ? C32 C33 C34 Br1 -178.8(7) . . . . ? C33 C34 C35 C36 -1.2(15) . . . . ? Br1 C34 C35 C36 179.1(7) . . . . ? C32 C31 C36 C35 1.9(14) . . . . ? C12 C31 C36 C35 -179.9(8) . . . . ? C34 C35 C36 C31 -0.5(15) . . . . ? O27 C26 C41 C42 171.9(9) . . . . ? C25 C26 C41 C42 -5.2(14) . . . . ? O27 C26 C41 C46 -8.7(12) . . . . ? C25 C26 C41 C46 174.1(8) . . . . ? C46 C41 C42 C43 1.1(14) . . . . ? C26 C41 C42 C43 -179.5(9) . . . . ? C41 C42 C43 C44 -0.1(15) . . . . ? C42 C43 C44 C45 0.2(15) . . . . ? C42 C43 C44 Br2 178.0(8) . . . . ? C43 C44 C45 C46 -1.3(15) . . . . ? Br2 C44 C45 C46 -179.1(7) . . . . ? C44 C45 C46 C41 2.4(14) . . . . ? C42 C41 C46 C45 -2.3(13) . . . . ? C26 C41 C46 C45 178.3(8) . . . . ? O11 Ni1 O51 C52 175.8(7) . . . . ? O15 Ni1 O51 C52 -25(4) . . . . ? O55 Ni1 O51 C52 -3.4(8) . . . . ? O111 Ni1 O51 C52 83.8(7) . . . . ? N91 Ni1 O51 C52 -96.6(7) . . . . ? Ni1 O51 C52 C53 -12.1(14) . . . . ? Ni1 O51 C52 C71 169.1(6) . . . . ? O51 C52 C53 C54 16.0(17) . . . . ? C71 C52 C53 C54 -165.3(9) . . . . ? C52 C53 C54 O55 4.2(17) . . . . ? C52 C53 C54 C56 -172.7(9) . . . . ? C53 C54 O55 Ni1 -22.1(13) . . . . ? C56 C54 O55 Ni1 155.0(6) . . . . ? C53 C54 O55 Ni2 -155.5(8) . . . . ? C56 C54 O55 Ni2 21.5(11) . . . . ? O51 Ni1 O55 C54 19.0(7) . . . . ? O11 Ni1 O55 C54 -152(3) . . . . ? O15 Ni1 O55 C54 -162.9(7) . . . . ? O111 Ni1 O55 C54 -72.6(6) . . . . ? N91 Ni1 O55 C54 105.5(7) . . . . ? O51 Ni1 O55 Ni2 166.5(3) . . . . ? O11 Ni1 O55 Ni2 -4(3) . . . . ? O15 Ni1 O55 Ni2 -15.3(2) . . . . ? O111 Ni1 O55 Ni2 75.0(3) . . . . ? N91 Ni1 O55 Ni2 -107.0(3) . . . . ? O112 Ni2 O55 C54 66.0(8) . . . . ? O121 Ni2 O55 C54 -113.8(8) . . . . ? O15 Ni2 O55 C54 155.6(8) . . . . ? O24 Ni2 O55 C54 80(7) . . . . ? O64 Ni2 O55 C54 -26.5(8) . . . . ? O112 Ni2 O55 Ni1 -74.6(3) . . . . ? O121 Ni2 O55 Ni1 105.6(3) . . . . ? O15 Ni2 O55 Ni1 15.0(2) . . . . ? O24 Ni2 O55 Ni1 -61(7) . . . . ? O64 Ni2 O55 Ni1 -167.1(2) . . . . ? O55 C54 C56 O57 170.5(8) . . . . ? C53 C54 C56 O57 -12.2(12) . . . . ? O55 C54 C56 C62 52.3(10) . . . . ? C53 C54 C56 C62 -130.4(9) . . . . ? C54 C56 O57 C58 -126.2(9) . . . . ? C62 C56 O57 C58 -3.9(11) . . . . ? C56 O57 C58 O61 12.6(11) . . . . ? C56 O57 C58 C60A 137(2) . . . . ? C56 O57 C58 C59 -102.2(11) . . . . ? C56 O57 C58 C60B 110(4) . . . . ? O57 C58 O61 C62 -16.5(11) . . . . ? C60A C58 O61 C62 -149(3) . . . . ? C59 C58 O61 C62 98.8(11) . . . . ? C60B C58 O61 C62 -111(5) . . . . ? C58 O61 C62 C63 -109.9(9) . . . . ? C58 O61 C62 C56 13.7(10) . . . . ? O57 C56 C62 O61 -6.1(10) . . . . ? C54 C56 C62 O61 115.8(8) . . . . ? O57 C56 C62 C63 118.3(9) . . . . ? C54 C56 C62 C63 -119.8(9) . . . . ? O61 C62 C63 O64 173.6(7) . . . . ? C56 C62 C63 O64 54.5(11) . . . . ? O61 C62 C63 C65 -6.7(13) . . . . ? C56 C62 C63 C65 -125.8(10) . . . . ? C65 C63 O64 Ni3 -27.1(12) . . . . ? C62 C63 O64 Ni3 152.6(6) . . . . ? C65 C63 O64 Ni2 -155.8(8) . . . . ? C62 C63 O64 Ni2 23.9(11) . . . . ? O27 Ni3 O64 C63 -127(3) . . . . ? O24 Ni3 O64 C63 -156.6(6) . . . . ? O67 Ni3 O64 C63 24.2(6) . . . . ? O122 Ni3 O64 C63 -69.3(6) . . . . ? N101 Ni3 O64 C63 110.9(6) . . . . ? O27 Ni3 O64 Ni2 16(3) . . . . ? O24 Ni3 O64 Ni2 -13.3(2) . . . . ? O67 Ni3 O64 Ni2 167.5(2) . . . . ? O122 Ni3 O64 Ni2 74.0(2) . . . . ? N101 Ni3 O64 Ni2 -105.8(3) . . . . ? O112 Ni2 O64 C63 -121.1(7) . . . . ? O121 Ni2 O64 C63 59.1(7) . . . . ? O15 Ni2 O64 C63 72(7) . . . . ? O24 Ni2 O64 C63 149.9(7) . . . . ? O55 Ni2 O64 C63 -32.2(7) . . . . ? O112 Ni2 O64 Ni3 101.9(2) . . . . ? O121 Ni2 O64 Ni3 -77.8(2) . . . . ? O15 Ni2 O64 Ni3 -65(7) . . . . ? O24 Ni2 O64 Ni3 12.9(2) . . . . ? O55 Ni2 O64 Ni3 -169.1(2) . . . . ? O64 C63 C65 C66 8.4(17) . . . . ? C62 C63 C65 C66 -171.3(9) . . . . ? C63 C65 C66 O67 9.7(17) . . . . ? C63 C65 C66 C81 -169.5(10) . . . . ? C65 C66 O67 Ni3 -3.7(14) . . . . ? C81 C66 O67 Ni3 175.5(6) . . . . ? O27 Ni3 O67 C66 167.3(8) . . . . ? O24 Ni3 O67 C66 -24(4) . . . . ? O64 Ni3 O67 C66 -10.4(8) . . . . ? O122 Ni3 O67 C66 77.3(8) . . . . ? N101 Ni3 O67 C66 -105.3(8) . . . . ? O51 C52 C71 C72 -158.9(9) . . . . ? C53 C52 C71 C72 22.3(14) . . . . ? O51 C52 C71 C76 16.2(13) . . . . ? C53 C52 C71 C76 -162.7(9) . . . . ? C76 C71 C72 C73 -2.9(15) . . . . ? C52 C71 C72 C73 172.1(10) . . . . ? C71 C72 C73 C74 2.3(16) . . . . ? C72 C73 C74 C75 -0.3(17) . . . . ? C72 C73 C74 Br3 -178.9(8) . . . . ? C73 C74 C75 C76 -0.9(17) . . . . ? Br3 C74 C75 C76 177.7(8) . . . . ? C74 C75 C76 C71 0.2(16) . . . . ? C72 C71 C76 C75 1.7(15) . . . . ? C52 C71 C76 C75 -173.6(9) . . . . ? O67 C66 C81 C86 17.0(13) . . . . ? C65 C66 C81 C86 -163.7(10) . . . . ? O67 C66 C81 C82 -161.7(9) . . . . ? C65 C66 C81 C82 17.6(14) . . . . ? C86 C81 C82 C83 1.1(15) . . . . ? C66 C81 C82 C83 179.8(9) . . . . ? C81 C82 C83 C84 2.8(15) . . . . ? C82 C83 C84 C85 -4.0(15) . . . . ? C82 C83 C84 Br4 174.6(7) . . . . ? C83 C84 C85 C86 1.3(16) . . . . ? Br4 C84 C85 C86 -177.4(8) . . . . ? C84 C85 C86 C81 2.7(17) . . . . ? C82 C81 C86 C85 -3.9(16) . . . . ? C66 C81 C86 C85 177.4(10) . . . . ? O51 Ni1 N91 C92 -50.0(7) . . . . ? O11 Ni1 N91 C92 42.5(7) . . . . ? O15 Ni1 N91 C92 134.6(7) . . . . ? O55 Ni1 N91 C92 -142.4(7) . . . . ? O111 Ni1 N91 C92 -39(8) . . . . ? O51 Ni1 N91 C96 126.1(7) . . . . ? O11 Ni1 N91 C96 -141.3(7) . . . . ? O15 Ni1 N91 C96 -49.2(7) . . . . ? O55 Ni1 N91 C96 33.7(8) . . . . ? O111 Ni1 N91 C96 137(7) . . . . ? C96 N91 C92 C93 -0.9(14) . . . . ? Ni1 N91 C92 C93 175.5(8) . . . . ? N91 C92 C93 C94 -0.2(16) . . . . ? C92 C93 C94 C95 0.9(16) . . . . ? C93 C94 C95 C96 -0.5(16) . . . . ? C92 N91 C96 C95 1.3(14) . . . . ? Ni1 N91 C96 C95 -174.9(8) . . . . ? C94 C95 C96 N91 -0.6(16) . . . . ? O27 Ni3 N101 C106 55.0(8) . . . . ? O24 Ni3 N101 C106 146.3(8) . . . . ? O67 Ni3 N101 C106 -37.4(8) . . . . ? O64 Ni3 N101 C106 -129.2(8) . . . . ? O122 Ni3 N101 C106 56(6) . . . . ? O27 Ni3 N101 C102 -127.2(7) . . . . ? O24 Ni3 N101 C102 -35.8(7) . . . . ? O67 Ni3 N101 C102 140.4(7) . . . . ? O64 Ni3 N101 C102 48.7(7) . . . . ? O122 Ni3 N101 C102 -126(6) . . . . ? C106 N101 C102 C103 -1.4(15) . . . . ? Ni3 N101 C102 C103 -179.3(8) . . . . ? N101 C102 C103 C104 2.8(17) . . . . ? C102 C103 C104 C105 -2.3(18) . . . . ? C103 C104 C105 C106 0.7(18) . . . . ? C102 N101 C106 C105 -0.4(16) . . . . ? Ni3 N101 C106 C105 177.5(9) . . . . ? C104 C105 C106 N101 0.8(18) . . . . ? O51 Ni1 O111 C113 -137.1(7) . . . . ? O11 Ni1 O111 C113 130.5(7) . . . . ? O15 Ni1 O111 C113 38.3(7) . . . . ? O55 Ni1 O111 C113 -44.5(7) . . . . ? N91 Ni1 O111 C113 -148(7) . . . . ? O121 Ni2 O112 C113 -176(100) . . . . ? O15 Ni2 O112 C113 -41.5(8) . . . . ? O24 Ni2 O112 C113 -140.9(8) . . . . ? O55 Ni2 O112 C113 38.6(8) . . . . ? O64 Ni2 O112 C113 138.9(8) . . . . ? Ni1 O111 C113 O112 2.1(14) . . . . ? Ni1 O111 C113 C114 -177.3(6) . . . . ? Ni2 O112 C113 O111 0.6(14) . . . . ? Ni2 O112 C113 C114 180.0(6) . . . . ? O112 Ni2 O121 C123 -3(48) . . . . ? O15 Ni2 O121 C123 -136.8(8) . . . . ? O24 Ni2 O121 C123 -37.5(8) . . . . ? O55 Ni2 O121 C123 143.0(8) . . . . ? O64 Ni2 O121 C123 42.7(8) . . . . ? O27 Ni3 O122 C123 138.9(8) . . . . ? O24 Ni3 O122 C123 47.4(8) . . . . ? O67 Ni3 O122 C123 -128.8(8) . . . . ? O64 Ni3 O122 C123 -37.0(8) . . . . ? N101 Ni3 O122 C123 138(6) . . . . ? Ni3 O122 C123 O121 -6.4(14) . . . . ? Ni3 O122 C123 C124 175.8(7) . . . . ? Ni2 O121 C123 O122 1.6(14) . . . . ? Ni2 O121 C123 C124 179.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.802 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.097