# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name R.M.Haak A.M.Castilla M.M.Belmonte E.C.Escudero-Adan ; J.Benet-Buchholz ; A.W.Kleij _publ_contact_author_name 'Arjan W. Kleij' _publ_contact_author_email akleij@ICIQ.ES data_rmh023_0m _database_code_depnum_ccdc_archive 'CCDC 790314' #TrackingRef '- RMH023_0mX.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H38 N2 O5 S Zn' _chemical_formula_weight 604.05 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.0153(5) _cell_length_b 22.6939(9) _cell_length_c 11.5963(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.7870(10) _cell_angle_gamma 90.00 _cell_volume 2884.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8839 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 37.92 _exptl_crystal_description Block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.966 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7605 _exptl_absorpt_correction_T_max 0.9533 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 43905 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0846 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 38.16 _reflns_number_total 20308 _reflns_number_gt 18282 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _chemical_absolute_configuration ad _refine_ls_abs_structure_Flack 0.000(5) _refine_ls_number_reflns 20308 _refine_ls_number_parameters 711 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0517 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1216 _refine_ls_wR_factor_gt 0.1172 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 Zn1 Zn 0.173147(17) 0.801249(8) 0.985238(17) 0.01285(4) Uani 1 1 d . . . Zn1A Zn 0.336881(17) 0.568105(9) 0.020394(17) 0.01358(4) Uani 1 1 d . . . O1A O 0.28679(13) 0.53153(8) 0.16505(12) 0.0190(3) Uani 1 1 d . . . O2A O 0.19674(13) 0.54041(7) -0.08419(12) 0.0184(2) Uani 1 1 d . . . N1A N 0.46044(13) 0.62118(7) 0.12069(13) 0.0146(2) Uani 1 1 d . . . N2A N 0.34670(14) 0.64324(7) -0.08796(13) 0.0146(2) Uani 1 1 d . . . O3A O 0.19890(14) 0.46570(8) 0.32456(13) 0.0229(3) Uani 1 1 d . . . O4A O 0.02106(14) 0.47880(7) -0.19309(12) 0.0204(3) Uani 1 1 d . . . C1A C 0.33213(15) 0.54042(9) 0.27217(15) 0.0156(3) Uani 1 1 d . . . C19A C 0.20660(16) 0.60641(9) -0.24703(15) 0.0155(3) Uani 1 1 d . . . C18A C 0.29466(16) 0.64770(9) -0.19122(15) 0.0151(3) Uani 1 1 d . . . H18A H 0.3154 0.6809 -0.2353 0.018 Uiso 1 1 calc R . . C3A C 0.32940(17) 0.51366(10) 0.47857(17) 0.0197(3) Uani 1 1 d . . . H3A H 0.2959 0.4905 0.5359 0.024 Uiso 1 1 calc R . . C13A C 0.60608(16) 0.70740(9) 0.11327(17) 0.0175(3) Uani 1 1 d . . . H13A H 0.6707 0.6874 0.1645 0.021 Uiso 1 1 calc R . . H13B H 0.5572 0.7317 0.1623 0.021 Uiso 1 1 calc R . . C16A C 0.48289(18) 0.73140(9) -0.12164(17) 0.0188(3) Uani 1 1 d . . . H16A H 0.5305 0.7077 -0.1729 0.023 Uiso 1 1 calc R . . H16B H 0.4176 0.7521 -0.1707 0.023 Uiso 1 1 calc R . . C9A C 0.46977(17) 0.56484(13) 0.63979(16) 0.0231(4) Uani 1 1 d . . . H9A1 H 0.4559 0.6063 0.6614 0.028 Uiso 1 1 calc R . . H9A2 H 0.4241 0.5393 0.6896 0.028 Uiso 1 1 calc R . . C6A C 0.42447(16) 0.58204(9) 0.30986(15) 0.0157(3) Uani 1 1 d . . . C17A C 0.42581(15) 0.69057(8) -0.03633(15) 0.0143(3) Uani 1 1 d . . . H17A H 0.3747 0.7157 0.0105 0.017 Uiso 1 1 calc R . . C24A C 0.16163(16) 0.55709(8) -0.18923(15) 0.0152(3) Uani 1 1 d . . . C2A C 0.28713(16) 0.50570(9) 0.36318(16) 0.0168(3) Uani 1 1 d . . . C28A C -0.0817(2) 0.44780(11) -0.2466(2) 0.0248(4) Uani 1 1 d . . . H28A H -0.0608 0.4299 -0.3189 0.037 Uiso 1 1 calc R . . H28B H -0.1498 0.4753 -0.2636 0.037 Uiso 1 1 calc R . . H28C H -0.1054 0.4169 -0.1942 0.037 Uiso 1 1 calc R . . C23A C 0.06480(16) 0.52450(9) -0.25382(16) 0.0162(3) Uani 1 1 d . . . C26A C -0.1115(2) 0.60613(14) -0.5667(2) 0.0299(5) Uani 1 1 d . . . H26A H -0.1494 0.6376 -0.5298 0.036 Uiso 1 1 calc R . . C4A C 0.42124(17) 0.55536(10) 0.51329(16) 0.0188(3) Uani 1 1 d . . . C5A C 0.46691(17) 0.58849(10) 0.42835(16) 0.0188(3) Uani 1 1 d . . . H5A H 0.5289 0.6166 0.4499 0.023 Uiso 1 1 calc R . . C7A C 0.48192(15) 0.62098(9) 0.23225(16) 0.0161(3) Uani 1 1 d . . . H7A H 0.5399 0.6485 0.2662 0.019 Uiso 1 1 calc R . . C22A C 0.02145(17) 0.53931(10) -0.36590(16) 0.0185(3) Uani 1 1 d . . . H22A H -0.0422 0.5166 -0.4055 0.022 Uiso 1 1 calc R . . C14A C 0.66451(18) 0.74702(10) 0.02709(19) 0.0219(3) Uani 1 1 d . . . H14A H 0.7150 0.7775 0.0699 0.026 Uiso 1 1 calc R . . H14B H 0.7184 0.7231 -0.0178 0.026 Uiso 1 1 calc R . . C20A C 0.16081(17) 0.62030(10) -0.36269(16) 0.0183(3) Uani 1 1 d . . . H20A H 0.1940 0.6532 -0.3995 0.022 Uiso 1 1 calc R . . C12A C 0.52476(15) 0.66168(8) 0.04894(15) 0.0144(3) Uani 1 1 d . . . H12A H 0.5774 0.6373 0.0022 0.017 Uiso 1 1 calc R . . C15A C 0.56646(18) 0.77651(9) -0.05535(18) 0.0205(3) Uani 1 1 d . . . H15A H 0.6059 0.8011 -0.1114 0.025 Uiso 1 1 calc R . . H15B H 0.5168 0.8027 -0.0106 0.025 Uiso 1 1 calc R . . C21A C 0.07043(17) 0.58798(10) -0.42318(16) 0.0190(3) Uani 1 1 d . . . C8A C 0.1478(2) 0.43082(12) 0.4098(2) 0.0264(4) Uani 1 1 d . . . H8A1 H 0.1136 0.4567 0.4660 0.040 Uiso 1 1 calc R . . H8A2 H 0.2115 0.4060 0.4499 0.040 Uiso 1 1 calc R . . H8A3 H 0.0830 0.4058 0.3721 0.040 Uiso 1 1 calc R . . C27A C -0.1829(2) 0.56974(19) -0.6313(2) 0.0382(7) Uani 1 1 d . . . H27A H -0.1484 0.5378 -0.6696 0.046 Uiso 1 1 calc R . . H27B H -0.2687 0.5755 -0.6394 0.046 Uiso 1 1 calc R . . C11A C 0.6884(2) 0.59161(15) 0.6886(2) 0.0324(5) Uani 1 1 d . . . H11A H 0.6668 0.6319 0.6955 0.039 Uiso 1 1 calc R . . H11B H 0.7716 0.5800 0.7012 0.039 Uiso 1 1 calc R . . C10A C 0.6020(2) 0.55128(13) 0.66119(19) 0.0272(4) Uani 1 1 d . . . H10A H 0.6266 0.5114 0.6550 0.033 Uiso 1 1 calc R . . C25A C 0.02430(19) 0.60171(12) -0.54724(17) 0.0235(4) Uani 1 1 d . . . H25A H 0.0604 0.6394 -0.5698 0.028 Uiso 1 1 calc R . . H25B H 0.0522 0.5705 -0.5980 0.028 Uiso 1 1 calc R . . O1SA O 0.47102(14) 0.51472(8) -0.03407(14) 0.0227(3) Uani 1 1 d . . . S1SA S 0.56970(5) 0.49037(3) 0.05499(6) 0.02718(11) Uani 1 1 d . . . C1SA C 0.6831(2) 0.46291(13) -0.0316(4) 0.0462(8) Uani 1 1 d . . . H1S1 H 0.7223 0.4960 -0.0674 0.069 Uiso 1 1 calc R . . H1S2 H 0.6444 0.4370 -0.0922 0.069 Uiso 1 1 calc R . . H1S3 H 0.7445 0.4406 0.0176 0.069 Uiso 1 1 calc R . . O1SB O 0.03464(13) 0.85845(7) 1.01449(13) 0.0206(3) Uani 1 1 d . . . S1SB S -0.04916(4) 0.88390(2) 0.91367(4) 0.01955(8) Uani 1 1 d . . . O2B O 0.22037(12) 0.84168(7) 0.84084(12) 0.0178(2) Uani 1 1 d . . . O1B O 0.31998(12) 0.82426(7) 1.08650(12) 0.0176(2) Uani 1 1 d . . . O4B O 0.30256(15) 0.90947(9) 0.68023(14) 0.0266(3) Uani 1 1 d . . . O3B O 0.50946(14) 0.88002(8) 1.18901(13) 0.0220(3) Uani 1 1 d . . . C6B C 0.31059(16) 0.75821(9) 1.25008(15) 0.0156(3) Uani 1 1 d . . . C7B C 0.20750(15) 0.72362(9) 1.20217(15) 0.0153(3) Uani 1 1 d . . . H7B H 0.1887 0.6891 1.2432 0.018 Uiso 1 1 calc R . . C2B C 0.46128(17) 0.83587(9) 1.25166(16) 0.0178(3) Uani 1 1 d . . . C1B C 0.35879(15) 0.80643(9) 1.19068(15) 0.0150(3) Uani 1 1 d . . . C5B C 0.35935(18) 0.74293(10) 1.36389(17) 0.0203(3) Uani 1 1 d . . . H5B H 0.3258 0.7103 1.4010 0.024 Uiso 1 1 calc R . . C3B C 0.50490(18) 0.82093(10) 1.36410(18) 0.0208(3) Uani 1 1 d . . . H3B H 0.5705 0.8428 1.4027 0.025 Uiso 1 1 calc R . . C4B C 0.4537(2) 0.77390(12) 1.42231(19) 0.0243(4) Uani 1 1 d . . . C8B C 0.6086(2) 0.91243(12) 1.2430(2) 0.0305(5) Uani 1 1 d . . . H8B1 H 0.6789 0.8862 1.2598 0.046 Uiso 1 1 calc R . . H8B2 H 0.5859 0.9294 1.3155 0.046 Uiso 1 1 calc R . . H8B3 H 0.6299 0.9441 1.1913 0.046 Uiso 1 1 calc R . . C9B C 0.4973(3) 0.76060(17) 1.5487(2) 0.0397(7) Uani 1 1 d . . . H9B1 H 0.4654 0.7913 1.5982 0.048 Uiso 1 1 calc R . . H9B2 H 0.4626 0.7224 1.5701 0.048 Uiso 1 1 calc R . . C10B C 0.6299(3) 0.75810(19) 1.5729(3) 0.0439(7) Uani 1 1 d . . . H10B H 0.6728 0.7282 1.5365 0.053 Uiso 1 1 calc R . . N2B N 0.08240(13) 0.73636(7) 0.88170(13) 0.0135(2) Uani 1 1 d . . . N1B N 0.13902(13) 0.73566(7) 1.10866(13) 0.0141(2) Uani 1 1 d . . . C16B C -0.06834(17) 0.65160(9) 0.88675(16) 0.0178(3) Uani 1 1 d . . . H16C H -0.0548 0.6391 0.8073 0.021 Uiso 1 1 calc R . . H16D H -0.1387 0.6790 0.8812 0.021 Uiso 1 1 calc R . . C13B C 0.00925(17) 0.64447(9) 1.13898(16) 0.0174(3) Uani 1 1 d . . . H13C H 0.0799 0.6175 1.1391 0.021 Uiso 1 1 calc R . . H13D H -0.0003 0.6554 1.2202 0.021 Uiso 1 1 calc R . . C15B C -0.0970(2) 0.59772(10) 0.95827(18) 0.0228(4) Uani 1 1 d . . . H15C H -0.0322 0.5678 0.9536 0.027 Uiso 1 1 calc R . . H15D H -0.1751 0.5802 0.9250 0.027 Uiso 1 1 calc R . . C14B C -0.10618(17) 0.61337(10) 1.08571(17) 0.0203(3) Uani 1 1 d . . . H14C H -0.1775 0.6394 1.0914 0.024 Uiso 1 1 calc R . . H14D H -0.1189 0.5769 1.1299 0.024 Uiso 1 1 calc R . . C12B C 0.03239(15) 0.69990(8) 1.06928(15) 0.0141(3) Uani 1 1 d . . . H12B H -0.0412 0.7257 1.0697 0.017 Uiso 1 1 calc R . . C17B C 0.04506(15) 0.68322(8) 0.94237(14) 0.0138(3) Uani 1 1 d . . . H17B H 0.1141 0.6546 0.9435 0.017 Uiso 1 1 calc R . . C24 C 0.17773(15) 0.83140(8) 0.73344(15) 0.0146(3) Uani 1 1 d . . . C22 C 0.17773(16) 0.85801(9) 0.52655(16) 0.0176(3) Uani 1 1 d . . . H22 H 0.2084 0.8820 0.4689 0.021 Uiso 1 1 calc R . . C25 C 0.04560(16) 0.80206(10) 0.36709(15) 0.0180(3) Uani 1 1 d . . . H25C H 0.0915 0.8270 0.3165 0.022 Uiso 1 1 calc R . . H25D H 0.0612 0.7603 0.3484 0.022 Uiso 1 1 calc R . . C19 C 0.09350(16) 0.78642(8) 0.69695(15) 0.0145(3) Uani 1 1 d . . . C23 C 0.21861(17) 0.86736(10) 0.64181(17) 0.0181(3) Uani 1 1 d . . . C20 C 0.05115(16) 0.77923(9) 0.57819(16) 0.0167(3) Uani 1 1 d . . . H20 H -0.0074 0.7494 0.5571 0.020 Uiso 1 1 calc R . . C21 C 0.09146(16) 0.81369(9) 0.49261(15) 0.0157(3) Uani 1 1 d . . . C18 C 0.05250(16) 0.74139(8) 0.77184(15) 0.0150(3) Uani 1 1 d . . . H18 H -0.0019 0.7126 0.7367 0.018 Uiso 1 1 calc R . . C27 C -0.1715(2) 0.77299(16) 0.3145(2) 0.0337(5) Uani 1 1 d . . . H27C H -0.1467 0.7331 0.3093 0.040 Uiso 1 1 calc R . . H27D H -0.2553 0.7831 0.2998 0.040 Uiso 1 1 calc R . . C28 C 0.3598(2) 0.94116(13) 0.5942(2) 0.0296(5) Uani 1 1 d . . . H28D H 0.2993 0.9661 0.5497 0.044 Uiso 1 1 calc R . . H28E H 0.3944 0.9132 0.5419 0.044 Uiso 1 1 calc R . . H28F H 0.4251 0.9659 0.6319 0.044 Uiso 1 1 calc R . . C26 C -0.08882(19) 0.81471(11) 0.34250(18) 0.0233(4) Uani 1 1 d . . . H26 H -0.1158 0.8543 0.3472 0.028 Uiso 1 1 calc R . . C1SB C 0.0072(2) 0.95614(11) 0.8893(2) 0.0275(4) Uani 1 1 d . . . H1S4 H 0.0814 0.9533 0.8496 0.041 Uiso 1 1 calc R . . H1S5 H 0.0259 0.9762 0.9638 0.041 Uiso 1 1 calc R . . H1S6 H -0.0549 0.9786 0.8412 0.041 Uiso 1 1 calc R . . C2SB C -0.18308(19) 0.90614(11) 0.9769(2) 0.0272(4) Uani 1 1 d . . . H2S1 H -0.1598 0.9300 1.0460 0.041 Uiso 1 1 calc R . . H2S2 H -0.2276 0.8712 0.9988 0.041 Uiso 1 1 calc R . . H2S3 H -0.2353 0.9294 0.9206 0.041 Uiso 1 1 calc R . . C2SA C 0.5132(2) 0.42150(12) 0.0974(2) 0.0302(5) Uani 1 1 d . . . H2S4 H 0.4875 0.3980 0.0283 0.045 Uiso 1 1 calc R . . H2S5 H 0.4434 0.4278 0.1420 0.045 Uiso 1 1 calc R . . H2S6 H 0.5776 0.4005 0.1454 0.045 Uiso 1 1 calc R . . C11 C 0.6952(3) 0.7966(3) 1.6455(3) 0.0664(15) Uani 1 1 d . . . H11C H 0.6543 0.8269 1.6830 0.080 Uiso 1 1 calc R . . H11D H 0.7814 0.7931 1.6584 0.080 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01637(8) 0.01196(8) 0.01008(8) 0.00029(6) 0.00061(6) -0.00014(6) Zn1A 0.01713(8) 0.01217(9) 0.01106(8) 0.00071(6) -0.00047(6) 0.00011(6) O1A 0.0224(6) 0.0228(7) 0.0114(5) 0.0009(5) -0.0009(4) -0.0057(5) O2A 0.0239(6) 0.0175(6) 0.0126(6) 0.0035(5) -0.0040(4) -0.0035(5) N1A 0.0180(5) 0.0131(6) 0.0127(6) 0.0013(5) 0.0016(4) -0.0008(4) N2A 0.0173(5) 0.0132(6) 0.0131(6) 0.0005(5) 0.0000(4) 0.0003(4) O3A 0.0262(6) 0.0268(8) 0.0152(6) 0.0045(5) 0.0002(5) -0.0103(6) O4A 0.0275(6) 0.0179(6) 0.0146(6) 0.0018(5) -0.0034(5) -0.0058(5) C1A 0.0168(6) 0.0191(8) 0.0106(7) 0.0014(6) 0.0000(5) -0.0006(5) C19A 0.0175(6) 0.0174(7) 0.0117(7) 0.0000(5) 0.0019(5) -0.0006(5) C18A 0.0181(6) 0.0151(7) 0.0124(7) 0.0022(5) 0.0024(5) 0.0003(5) C3A 0.0191(7) 0.0275(10) 0.0124(7) 0.0032(7) 0.0014(5) -0.0003(6) C13A 0.0182(6) 0.0170(7) 0.0175(8) 0.0001(6) 0.0022(6) -0.0023(5) C16A 0.0228(7) 0.0164(8) 0.0172(8) 0.0027(6) 0.0023(6) -0.0021(6) C9A 0.0233(7) 0.0337(11) 0.0122(7) 0.0000(8) 0.0022(6) -0.0021(8) C6A 0.0177(6) 0.0179(7) 0.0113(7) 0.0006(5) 0.0009(5) -0.0018(5) C17A 0.0165(6) 0.0127(6) 0.0138(7) 0.0004(5) 0.0015(5) 0.0002(5) C24A 0.0197(6) 0.0140(7) 0.0115(6) 0.0002(5) -0.0007(5) -0.0005(5) C2A 0.0185(7) 0.0194(8) 0.0124(7) 0.0022(6) 0.0004(5) -0.0007(6) C28A 0.0286(9) 0.0221(9) 0.0218(9) 0.0012(7) -0.0071(7) -0.0075(7) C23A 0.0215(7) 0.0154(7) 0.0114(7) -0.0010(5) 0.0000(5) -0.0012(5) C26A 0.0306(10) 0.0398(14) 0.0186(9) 0.0091(9) -0.0003(7) 0.0069(9) C4A 0.0201(7) 0.0254(9) 0.0106(7) 0.0010(6) 0.0006(5) -0.0022(6) C5A 0.0186(7) 0.0250(9) 0.0125(7) -0.0004(6) 0.0000(5) -0.0033(6) C7A 0.0174(6) 0.0161(7) 0.0145(7) -0.0010(6) -0.0003(5) -0.0013(5) C22A 0.0213(7) 0.0211(8) 0.0126(7) -0.0005(6) -0.0003(5) -0.0002(6) C14A 0.0207(7) 0.0217(9) 0.0236(9) 0.0007(7) 0.0035(6) -0.0062(6) C20A 0.0208(7) 0.0227(8) 0.0116(7) 0.0022(6) 0.0023(5) -0.0009(6) C12A 0.0158(6) 0.0128(6) 0.0147(7) -0.0005(5) 0.0021(5) 0.0003(5) C15A 0.0259(8) 0.0161(8) 0.0202(8) 0.0008(6) 0.0053(6) -0.0033(6) C21A 0.0235(7) 0.0244(9) 0.0090(6) 0.0018(6) 0.0016(5) 0.0003(6) C8A 0.0331(10) 0.0277(11) 0.0190(9) 0.0023(8) 0.0049(7) -0.0109(8) C27A 0.0289(10) 0.061(2) 0.0234(10) 0.0131(13) -0.0042(8) -0.0079(12) C11A 0.0260(9) 0.0473(16) 0.0230(10) -0.0016(10) -0.0019(7) -0.0065(10) C10A 0.0293(9) 0.0335(12) 0.0179(9) -0.0033(8) -0.0018(7) 0.0043(8) C25A 0.0259(8) 0.0340(11) 0.0105(7) 0.0031(7) 0.0014(6) -0.0019(8) O1SA 0.0255(6) 0.0188(7) 0.0234(7) -0.0007(5) 0.0001(5) 0.0083(5) S1SA 0.0221(2) 0.0147(2) 0.0420(3) -0.0066(2) -0.01045(19) 0.00258(16) C1SA 0.0180(8) 0.0243(12) 0.097(3) -0.0179(14) 0.0105(12) -0.0036(8) O1SB 0.0254(6) 0.0204(7) 0.0157(6) -0.0003(5) 0.0009(5) 0.0076(5) S1SB 0.02306(19) 0.01538(19) 0.0192(2) -0.00179(15) -0.00307(15) 0.00268(15) O2B 0.0228(6) 0.0197(6) 0.0104(5) 0.0015(5) -0.0011(4) -0.0055(5) O1B 0.0212(5) 0.0187(6) 0.0122(5) 0.0015(5) -0.0013(4) -0.0031(5) O4B 0.0310(7) 0.0318(9) 0.0162(7) 0.0059(6) -0.0027(5) -0.0178(7) O3B 0.0258(6) 0.0221(7) 0.0169(6) 0.0013(5) -0.0031(5) -0.0082(5) C6B 0.0188(6) 0.0169(7) 0.0110(7) 0.0011(5) 0.0013(5) 0.0020(5) C7B 0.0175(6) 0.0178(7) 0.0113(7) 0.0007(6) 0.0038(5) 0.0013(5) C2B 0.0206(7) 0.0189(8) 0.0135(7) 0.0005(6) -0.0004(5) -0.0005(6) C1B 0.0173(6) 0.0162(7) 0.0113(6) -0.0002(5) 0.0008(5) 0.0012(5) C5B 0.0239(8) 0.0212(9) 0.0152(8) 0.0029(6) -0.0008(6) -0.0004(6) C3B 0.0248(8) 0.0205(8) 0.0158(8) 0.0005(6) -0.0052(6) -0.0020(6) C4B 0.0265(8) 0.0282(11) 0.0169(8) 0.0047(7) -0.0048(6) -0.0020(7) C8B 0.0342(10) 0.0234(11) 0.0306(12) 0.0068(8) -0.0130(9) -0.0097(8) C9B 0.0463(14) 0.0488(18) 0.0211(11) 0.0129(11) -0.0111(10) -0.0112(13) C10B 0.0426(14) 0.055(2) 0.0323(14) 0.0144(14) -0.0050(11) 0.0016(14) N2B 0.0172(5) 0.0134(6) 0.0102(5) 0.0012(4) 0.0026(4) -0.0011(4) N1B 0.0175(5) 0.0136(6) 0.0114(6) -0.0001(5) 0.0023(4) 0.0001(4) C16B 0.0214(7) 0.0194(8) 0.0126(7) 0.0014(6) 0.0016(5) -0.0060(6) C13B 0.0221(7) 0.0174(8) 0.0132(7) 0.0024(6) 0.0040(6) -0.0012(6) C15B 0.0320(9) 0.0193(8) 0.0176(8) -0.0009(6) 0.0052(7) -0.0107(7) C14B 0.0224(7) 0.0219(8) 0.0174(8) 0.0023(6) 0.0055(6) -0.0052(6) C12B 0.0170(6) 0.0147(6) 0.0110(6) 0.0004(5) 0.0034(5) -0.0001(5) C17B 0.0176(6) 0.0126(6) 0.0115(6) 0.0010(5) 0.0031(5) -0.0005(5) C24 0.0171(6) 0.0145(7) 0.0120(7) 0.0018(5) 0.0009(5) -0.0018(5) C22 0.0192(7) 0.0200(8) 0.0133(7) 0.0046(6) 0.0007(5) -0.0027(6) C25 0.0232(7) 0.0202(8) 0.0105(6) 0.0003(6) 0.0013(5) 0.0015(7) C19 0.0182(6) 0.0155(7) 0.0096(6) 0.0009(5) 0.0007(5) -0.0023(5) C23 0.0196(7) 0.0203(8) 0.0142(7) 0.0036(6) 0.0004(5) -0.0044(6) C20 0.0207(7) 0.0177(8) 0.0115(7) 0.0010(6) 0.0001(5) -0.0029(6) C21 0.0182(6) 0.0187(8) 0.0101(6) 0.0012(5) 0.0014(5) 0.0000(5) C18 0.0188(6) 0.0146(7) 0.0119(7) 0.0002(5) 0.0024(5) -0.0030(5) C27 0.0258(9) 0.0468(17) 0.0275(11) -0.0084(11) -0.0021(8) -0.0031(10) C28 0.0312(10) 0.0343(12) 0.0232(10) 0.0079(9) 0.0029(8) -0.0144(9) C26 0.0246(8) 0.0292(11) 0.0156(8) -0.0036(7) -0.0004(6) 0.0025(7) C1SB 0.0290(9) 0.0214(10) 0.0300(11) 0.0069(8) -0.0077(8) -0.0038(7) C2SB 0.0200(8) 0.0238(10) 0.0372(12) -0.0040(9) 0.0000(7) 0.0036(7) C2SA 0.0352(11) 0.0213(10) 0.0307(12) 0.0030(8) -0.0130(9) 0.0034(8) C11 0.0521(17) 0.114(4) 0.0290(14) 0.020(2) -0.0164(12) -0.040(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 Zn1 O1B 1.9709(14) . ? Zn1 O2B 2.0229(14) . ? Zn1 O1SB 2.0573(15) . ? Zn1 N2B 2.0898(16) . ? Zn1 N1B 2.1246(15) . ? Zn1A O2A 1.9675(14) . ? Zn1A O1A 1.9985(14) . ? Zn1A O1SA 2.0586(15) . ? Zn1A N1A 2.0825(16) . ? Zn1A N2A 2.1273(16) . ? O1A C1A 1.307(2) . ? O2A C24A 1.297(2) . ? N1A C7A 1.291(2) . ? N1A C12A 1.469(2) . ? N2A C18A 1.278(2) . ? N2A C17A 1.472(2) . ? O3A C2A 1.372(3) . ? O3A C8A 1.426(3) . ? O4A C23A 1.368(2) . ? O4A C28A 1.421(3) . ? C1A C6A 1.424(3) . ? C1A C2A 1.444(3) . ? C19A C24A 1.419(3) . ? C19A C20A 1.420(3) . ? C19A C18A 1.453(3) . ? C3A C2A 1.384(3) . ? C3A C4A 1.414(3) . ? C13A C12A 1.517(3) . ? C13A C14A 1.533(3) . ? C16A C15A 1.531(3) . ? C16A C17A 1.536(2) . ? C9A C10A 1.484(3) . ? C9A C4A 1.525(3) . ? C6A C5A 1.414(3) . ? C6A C7A 1.451(3) . ? C17A C12A 1.542(2) . ? C24A C23A 1.444(3) . ? C23A C22A 1.380(3) . ? C26A C27A 1.320(4) . ? C26A C25A 1.493(3) . ? C4A C5A 1.374(3) . ? C22A C21A 1.423(3) . ? C14A C15A 1.523(3) . ? C20A C21A 1.371(3) . ? C21A C25A 1.509(3) . ? C11A C10A 1.336(4) . ? O1SA S1SA 1.5255(17) . ? S1SA C2SA 1.770(3) . ? S1SA C1SA 1.791(3) . ? O1SB S1SB 1.5281(16) . ? S1SB C2SB 1.785(2) . ? S1SB C1SB 1.785(2) . ? O2B C24 1.307(2) . ? O1B C1B 1.305(2) . ? O4B C23 1.373(3) . ? O4B C28 1.427(3) . ? O3B C2B 1.375(3) . ? O3B C8B 1.410(3) . ? C6B C5B 1.417(3) . ? C6B C1B 1.424(3) . ? C6B C7B 1.445(3) . ? C7B N1B 1.286(2) . ? C2B C3B 1.385(3) . ? C2B C1B 1.435(3) . ? C5B C4B 1.375(3) . ? C3B C4B 1.410(3) . ? C4B C9B 1.526(3) . ? C9B C10B 1.460(4) . ? C10B C11 1.366(6) . ? N2B C18 1.288(2) . ? N2B C17B 1.475(2) . ? N1B C12B 1.462(2) . ? C16B C17B 1.526(3) . ? C16B C15B 1.528(3) . ? C13B C14B 1.529(3) . ? C13B C12B 1.530(3) . ? C15B C14B 1.533(3) . ? C12B C17B 1.540(2) . ? C24 C19 1.415(3) . ? C24 C23 1.447(3) . ? C22 C23 1.383(3) . ? C22 C21 1.412(3) . ? C25 C26 1.507(3) . ? C25 C21 1.515(3) . ? C19 C20 1.418(2) . ? C19 C18 1.443(2) . ? C20 C21 1.372(3) . ? C27 C26 1.331(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1B Zn1 O2B 96.25(6) . . ? O1B Zn1 O1SB 108.20(6) . . ? O2B Zn1 O1SB 96.15(6) . . ? O1B Zn1 N2B 147.70(6) . . ? O2B Zn1 N2B 89.55(6) . . ? O1SB Zn1 N2B 102.69(6) . . ? O1B Zn1 N1B 88.54(6) . . ? O2B Zn1 N1B 162.39(6) . . ? O1SB Zn1 N1B 98.42(6) . . ? N2B Zn1 N1B 77.67(6) . . ? O2A Zn1A O1A 96.82(6) . . ? O2A Zn1A O1SA 99.54(7) . . ? O1A Zn1A O1SA 106.29(7) . . ? O2A Zn1A N1A 163.13(6) . . ? O1A Zn1A N1A 89.52(6) . . ? O1SA Zn1A N1A 93.60(6) . . ? O2A Zn1A N2A 88.59(6) . . ? O1A Zn1A N2A 149.71(6) . . ? O1SA Zn1A N2A 102.10(6) . . ? N1A Zn1A N2A 78.29(6) . . ? C1A O1A Zn1A 128.48(13) . . ? C24A O2A Zn1A 128.83(12) . . ? C7A N1A C12A 121.30(15) . . ? C7A N1A Zn1A 126.93(12) . . ? C12A N1A Zn1A 111.77(11) . . ? C18A N2A C17A 120.96(16) . . ? C18A N2A Zn1A 124.89(13) . . ? C17A N2A Zn1A 114.07(11) . . ? C2A O3A C8A 117.23(17) . . ? C23A O4A C28A 117.18(16) . . ? O1A C1A C6A 125.92(17) . . ? O1A C1A C2A 118.94(17) . . ? C6A C1A C2A 115.13(16) . . ? C24A C19A C20A 120.89(17) . . ? C24A C19A C18A 123.19(16) . . ? C20A C19A C18A 115.80(17) . . ? N2A C18A C19A 125.62(17) . . ? C2A C3A C4A 121.62(18) . . ? C12A C13A C14A 110.27(16) . . ? C15A C16A C17A 110.15(16) . . ? C10A C9A C4A 111.98(17) . . ? C5A C6A C1A 121.53(17) . . ? C5A C6A C7A 114.68(17) . . ? C1A C6A C7A 123.79(16) . . ? N2A C17A C16A 116.25(15) . . ? N2A C17A C12A 107.57(14) . . ? C16A C17A C12A 111.15(14) . . ? O2A C24A C19A 126.05(17) . . ? O2A C24A C23A 118.20(16) . . ? C19A C24A C23A 115.71(16) . . ? O3A C2A C3A 124.09(17) . . ? O3A C2A C1A 113.99(16) . . ? C3A C2A C1A 121.91(18) . . ? O4A C23A C22A 124.26(17) . . ? O4A C23A C24A 113.66(16) . . ? C22A C23A C24A 122.08(17) . . ? C27A C26A C25A 125.0(3) . . ? C5A C4A C3A 117.73(18) . . ? C5A C4A C9A 119.61(18) . . ? C3A C4A C9A 122.67(18) . . ? C4A C5A C6A 122.06(18) . . ? N1A C7A C6A 125.18(17) . . ? C23A C22A C21A 121.15(18) . . ? C15A C14A C13A 110.43(15) . . ? C21A C20A C19A 122.34(19) . . ? N1A C12A C13A 116.36(15) . . ? N1A C12A C17A 106.20(13) . . ? C13A C12A C17A 111.64(15) . . ? C14A C15A C16A 111.95(17) . . ? C20A C21A C22A 117.79(17) . . ? C20A C21A C25A 122.31(19) . . ? C22A C21A C25A 119.88(19) . . ? C11A C10A C9A 124.2(3) . . ? C26A C25A C21A 113.21(17) . . ? S1SA O1SA Zn1A 119.34(9) . . ? O1SA S1SA C2SA 105.18(11) . . ? O1SA S1SA C1SA 103.66(15) . . ? C2SA S1SA C1SA 97.64(14) . . ? S1SB O1SB Zn1 120.87(9) . . ? O1SB S1SB C2SB 104.66(11) . . ? O1SB S1SB C1SB 105.98(10) . . ? C2SB S1SB C1SB 96.90(12) . . ? C24 O2B Zn1 127.60(12) . . ? C1B O1B Zn1 129.95(12) . . ? C23 O4B C28 117.04(18) . . ? C2B O3B C8B 117.93(17) . . ? C5B C6B C1B 120.92(17) . . ? C5B C6B C7B 115.77(17) . . ? C1B C6B C7B 123.26(16) . . ? N1B C7B C6B 125.46(18) . . ? O3B C2B C3B 124.04(18) . . ? O3B C2B C1B 113.90(16) . . ? C3B C2B C1B 122.06(18) . . ? O1B C1B C6B 125.67(16) . . ? O1B C1B C2B 118.68(17) . . ? C6B C1B C2B 115.62(16) . . ? C4B C5B C6B 122.0(2) . . ? C2B C3B C4B 121.20(19) . . ? C5B C4B C3B 118.01(19) . . ? C5B C4B C9B 121.4(2) . . ? C3B C4B C9B 120.5(2) . . ? C10B C9B C4B 113.9(2) . . ? C11 C10B C9B 123.2(4) . . ? C18 N2B C17B 119.22(15) . . ? C18 N2B Zn1 124.43(12) . . ? C17B N2B Zn1 116.25(11) . . ? C7B N1B C12B 121.98(16) . . ? C7B N1B Zn1 126.03(13) . . ? C12B N1B Zn1 111.69(11) . . ? C17B C16B C15B 110.61(16) . . ? C14B C13B C12B 110.00(16) . . ? C16B C15B C14B 112.04(17) . . ? C13B C14B C15B 111.31(15) . . ? N1B C12B C13B 117.55(15) . . ? N1B C12B C17B 106.71(13) . . ? C13B C12B C17B 109.80(15) . . ? N2B C17B C16B 116.01(15) . . ? N2B C17B C12B 108.14(14) . . ? C16B C17B C12B 111.74(13) . . ? O2B C24 C19 125.13(16) . . ? O2B C24 C23 119.37(17) . . ? C19 C24 C23 115.49(16) . . ? C23 C22 C21 121.53(17) . . ? C26 C25 C21 112.00(15) . . ? C24 C19 C20 120.99(16) . . ? C24 C19 C18 124.51(16) . . ? C20 C19 C18 114.26(16) . . ? O4B C23 C22 124.29(17) . . ? O4B C23 C24 113.81(17) . . ? C22 C23 C24 121.87(18) . . ? C21 C20 C19 122.55(17) . . ? C20 C21 C22 117.52(16) . . ? C20 C21 C25 119.66(17) . . ? C22 C21 C25 122.80(16) . . ? N2B C18 C19 126.42(16) . . ? C27 C26 C25 123.1(2) . . ? 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 O2A Zn1A O1A C1A -168.66(17) . . . . ? O1SA Zn1A O1A C1A 89.28(18) . . . . ? N1A Zn1A O1A C1A -4.33(17) . . . . ? N2A Zn1A O1A C1A -69.7(2) . . . . ? O1A Zn1A O2A C24A 167.00(17) . . . . ? O1SA Zn1A O2A C24A -85.14(17) . . . . ? N1A Zn1A O2A C24A 55.6(3) . . . . ? N2A Zn1A O2A C24A 16.90(17) . . . . ? O2A Zn1A N1A C7A 114.0(2) . . . . ? O1A Zn1A N1A C7A 1.57(16) . . . . ? O1SA Zn1A N1A C7A -104.73(16) . . . . ? N2A Zn1A N1A C7A 153.65(16) . . . . ? O2A Zn1A N1A C12A -65.7(2) . . . . ? O1A Zn1A N1A C12A -178.13(12) . . . . ? O1SA Zn1A N1A C12A 75.57(12) . . . . ? N2A Zn1A N1A C12A -26.05(11) . . . . ? O2A Zn1A N2A C18A -16.10(15) . . . . ? O1A Zn1A N2A C18A -117.26(16) . . . . ? O1SA Zn1A N2A C18A 83.35(15) . . . . ? N1A Zn1A N2A C18A 174.57(16) . . . . ? O2A Zn1A N2A C17A 167.02(12) . . . . ? O1A Zn1A N2A C17A 65.86(16) . . . . ? O1SA Zn1A N2A C17A -93.53(12) . . . . ? N1A Zn1A N2A C17A -2.31(11) . . . . ? Zn1A O1A C1A C6A 4.3(3) . . . . ? Zn1A O1A C1A C2A -175.56(14) . . . . ? C17A N2A C18A C19A -174.17(16) . . . . ? Zn1A N2A C18A C19A 9.2(3) . . . . ? C24A C19A C18A N2A 4.1(3) . . . . ? C20A C19A C18A N2A -179.89(18) . . . . ? O1A C1A C6A C5A 179.62(19) . . . . ? C2A C1A C6A C5A -0.5(3) . . . . ? O1A C1A C6A C7A -0.1(3) . . . . ? C2A C1A C6A C7A 179.78(17) . . . . ? C18A N2A C17A C16A -23.6(2) . . . . ? Zn1A N2A C17A C16A 153.41(12) . . . . ? C18A N2A C17A C12A -148.92(16) . . . . ? Zn1A N2A C17A C12A 28.10(15) . . . . ? C15A C16A C17A N2A -177.67(15) . . . . ? C15A C16A C17A C12A -54.2(2) . . . . ? Zn1A O2A C24A C19A -10.5(3) . . . . ? Zn1A O2A C24A C23A 171.91(13) . . . . ? C20A C19A C24A O2A 179.99(18) . . . . ? C18A C19A C24A O2A -4.2(3) . . . . ? C20A C19A C24A C23A -2.4(3) . . . . ? C18A C19A C24A C23A 173.41(16) . . . . ? C8A O3A C2A C3A 0.5(3) . . . . ? C8A O3A C2A C1A -178.43(19) . . . . ? C4A C3A C2A O3A 179.6(2) . . . . ? C4A C3A C2A C1A -1.5(3) . . . . ? O1A C1A C2A O3A 0.3(3) . . . . ? C6A C1A C2A O3A -179.59(17) . . . . ? O1A C1A C2A C3A -178.70(19) . . . . ? C6A C1A C2A C3A 1.4(3) . . . . ? C28A O4A C23A C22A -5.0(3) . . . . ? C28A O4A C23A C24A 174.47(18) . . . . ? O2A C24A C23A O4A 0.3(2) . . . . ? C19A C24A C23A O4A -177.55(16) . . . . ? O2A C24A C23A C22A 179.74(18) . . . . ? C19A C24A C23A C22A 1.9(3) . . . . ? C2A C3A C4A C5A 0.6(3) . . . . ? C2A C3A C4A C9A -179.8(2) . . . . ? C10A C9A C4A C5A -62.2(3) . . . . ? C10A C9A C4A C3A 118.2(2) . . . . ? C3A C4A C5A C6A 0.3(3) . . . . ? C9A C4A C5A C6A -179.32(19) . . . . ? C1A C6A C5A C4A -0.3(3) . . . . ? C7A C6A C5A C4A 179.41(19) . . . . ? C12A N1A C7A C6A -178.96(17) . . . . ? Zn1A N1A C7A C6A 1.4(3) . . . . ? C5A C6A C7A N1A 177.39(18) . . . . ? C1A C6A C7A N1A -2.9(3) . . . . ? O4A C23A C22A C21A 179.19(18) . . . . ? C24A C23A C22A C21A -0.2(3) . . . . ? C12A C13A C14A C15A 57.3(2) . . . . ? C24A C19A C20A C21A 1.2(3) . . . . ? C18A C19A C20A C21A -174.87(18) . . . . ? C7A N1A C12A C13A -6.7(2) . . . . ? Zn1A N1A C12A C13A 173.03(12) . . . . ? C7A N1A C12A C17A -131.63(17) . . . . ? Zn1A N1A C12A C17A 48.09(15) . . . . ? C14A C13A C12A N1A -178.80(15) . . . . ? C14A C13A C12A C17A -56.68(19) . . . . ? N2A C17A C12A N1A -48.21(17) . . . . ? C16A C17A C12A N1A -176.53(15) . . . . ? N2A C17A C12A C13A -176.01(13) . . . . ? C16A C17A C12A C13A 55.68(19) . . . . ? C13A C14A C15A C16A -57.6(2) . . . . ? C17A C16A C15A C14A 55.9(2) . . . . ? C19A C20A C21A C22A 0.6(3) . . . . ? C19A C20A C21A C25A -178.22(19) . . . . ? C23A C22A C21A C20A -1.1(3) . . . . ? C23A C22A C21A C25A 177.76(19) . . . . ? C4A C9A C10A C11A 112.0(3) . . . . ? C27A C26A C25A C21A -114.3(3) . . . . ? C20A C21A C25A C26A -129.6(2) . . . . ? C22A C21A C25A C26A 51.6(3) . . . . ? O2A Zn1A O1SA S1SA -142.45(11) . . . . ? O1A Zn1A O1SA S1SA -42.39(13) . . . . ? N1A Zn1A O1SA S1SA 48.16(12) . . . . ? N2A Zn1A O1SA S1SA 126.95(11) . . . . ? Zn1A O1SA S1SA C2SA 91.56(14) . . . . ? Zn1A O1SA S1SA C1SA -166.45(12) . . . . ? O1B Zn1 O1SB S1SB 136.51(10) . . . . ? O2B Zn1 O1SB S1SB 37.84(12) . . . . ? N2B Zn1 O1SB S1SB -53.08(12) . . . . ? N1B Zn1 O1SB S1SB -132.25(11) . . . . ? Zn1 O1SB S1SB C2SB 158.69(11) . . . . ? Zn1 O1SB S1SB C1SB -99.54(13) . . . . ? O1B Zn1 O2B C24 160.64(16) . . . . ? O1SB Zn1 O2B C24 -90.23(17) . . . . ? N2B Zn1 O2B C24 12.49(16) . . . . ? N1B Zn1 O2B C24 55.5(3) . . . . ? O2B Zn1 O1B C1B -169.69(17) . . . . ? O1SB Zn1 O1B C1B 91.71(17) . . . . ? N2B Zn1 O1B C1B -70.6(2) . . . . ? N1B Zn1 O1B C1B -6.68(17) . . . . ? C5B C6B C7B N1B 168.99(18) . . . . ? C1B C6B C7B N1B -8.4(3) . . . . ? C8B O3B C2B C3B -0.6(3) . . . . ? C8B O3B C2B C1B 178.4(2) . . . . ? Zn1 O1B C1B C6B 10.0(3) . . . . ? Zn1 O1B C1B C2B -172.11(13) . . . . ? C5B C6B C1B O1B -179.50(18) . . . . ? C7B C6B C1B O1B -2.2(3) . . . . ? C5B C6B C1B C2B 2.5(3) . . . . ? C7B C6B C1B C2B 179.83(17) . . . . ? O3B C2B C1B O1B -1.5(3) . . . . ? C3B C2B C1B O1B 177.55(19) . . . . ? O3B C2B C1B C6B 176.56(16) . . . . ? C3B C2B C1B C6B -4.3(3) . . . . ? C1B C6B C5B C4B 0.6(3) . . . . ? C7B C6B C5B C4B -176.9(2) . . . . ? O3B C2B C3B C4B -178.0(2) . . . . ? C1B C2B C3B C4B 3.0(3) . . . . ? C6B C5B C4B C3B -2.1(3) . . . . ? C6B C5B C4B C9B 174.2(2) . . . . ? C2B C3B C4B C5B 0.3(3) . . . . ? C2B C3B C4B C9B -176.0(2) . . . . ? C5B C4B C9B C10B 135.4(3) . . . . ? C3B C4B C9B C10B -48.4(4) . . . . ? C4B C9B C10B C11 116.3(4) . . . . ? O1B Zn1 N2B C18 -117.03(16) . . . . ? O2B Zn1 N2B C18 -16.01(15) . . . . ? O1SB Zn1 N2B C18 80.20(15) . . . . ? N1B Zn1 N2B C18 176.20(15) . . . . ? O1B Zn1 N2B C17B 66.67(15) . . . . ? O2B Zn1 N2B C17B 167.70(12) . . . . ? O1SB Zn1 N2B C17B -96.10(12) . . . . ? N1B Zn1 N2B C17B -0.10(11) . . . . ? C6B C7B N1B C12B -176.75(16) . . . . ? C6B C7B N1B Zn1 10.1(3) . . . . ? O1B Zn1 N1B C7B -3.11(16) . . . . ? O2B Zn1 N1B C7B 103.2(2) . . . . ? O1SB Zn1 N1B C7B -111.29(15) . . . . ? N2B Zn1 N1B C7B 147.47(16) . . . . ? O1B Zn1 N1B C12B -176.83(11) . . . . ? O2B Zn1 N1B C12B -70.6(2) . . . . ? O1SB Zn1 N1B C12B 74.99(12) . . . . ? N2B Zn1 N1B C12B -26.26(11) . . . . ? C17B C16B C15B C14B 53.4(2) . . . . ? C12B C13B C14B C15B 57.2(2) . . . . ? C16B C15B C14B C13B -55.0(2) . . . . ? C7B N1B C12B C13B -4.2(2) . . . . ? Zn1 N1B C12B C13B 169.84(12) . . . . ? C7B N1B C12B C17B -127.93(17) . . . . ? Zn1 N1B C12B C17B 46.09(15) . . . . ? C14B C13B C12B N1B 179.45(14) . . . . ? C14B C13B C12B C17B -58.36(19) . . . . ? C18 N2B C17B C16B -25.7(2) . . . . ? Zn1 N2B C17B C16B 150.85(12) . . . . ? C18 N2B C17B C12B -152.06(16) . . . . ? Zn1 N2B C17B C12B 24.44(16) . . . . ? C15B C16B C17B N2B -179.78(15) . . . . ? C15B C16B C17B C12B -55.2(2) . . . . ? N1B C12B C17B N2B -44.60(18) . . . . ? C13B C12B C17B N2B -173.02(14) . . . . ? N1B C12B C17B C16B -173.47(15) . . . . ? C13B C12B C17B C16B 58.12(19) . . . . ? Zn1 O2B C24 C19 -4.1(3) . . . . ? Zn1 O2B C24 C23 176.74(14) . . . . ? O2B C24 C19 C20 179.11(18) . . . . ? C23 C24 C19 C20 -1.7(3) . . . . ? O2B C24 C19 C18 -7.0(3) . . . . ? C23 C24 C19 C18 172.24(17) . . . . ? C28 O4B C23 C22 -6.7(3) . . . . ? C28 O4B C23 C24 171.5(2) . . . . ? C21 C22 C23 O4B 179.7(2) . . . . ? C21 C22 C23 C24 1.6(3) . . . . ? O2B C24 C23 O4B 0.9(3) . . . . ? C19 C24 C23 O4B -178.39(18) . . . . ? O2B C24 C23 C22 179.19(19) . . . . ? C19 C24 C23 C22 -0.1(3) . . . . ? C24 C19 C20 C21 2.0(3) . . . . ? C18 C19 C20 C21 -172.46(18) . . . . ? C19 C20 C21 C22 -0.5(3) . . . . ? C19 C20 C21 C25 177.80(17) . . . . ? C23 C22 C21 C20 -1.3(3) . . . . ? C23 C22 C21 C25 -179.53(19) . . . . ? C26 C25 C21 C20 66.3(3) . . . . ? C26 C25 C21 C22 -115.4(2) . . . . ? C17B N2B C18 C19 -171.95(16) . . . . ? Zn1 N2B C18 C19 11.9(3) . . . . ? C24 C19 C18 N2B 2.4(3) . . . . ? C20 C19 C18 N2B 176.64(18) . . . . ? C21 C25 C26 C27 -113.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.941 _refine_diff_density_min -1.425 _refine_diff_density_rms 0.103 # Attachment 'RMH157-P1X.cif' data_rmh157-p1 _database_code_depnum_ccdc_archive 'CCDC 790315' #TrackingRef 'RMH157-P1X.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H42 N2 Ni O7' _chemical_formula_weight 601.37 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.3200(4) _cell_length_b 13.9529(8) _cell_length_c 14.0274(8) _cell_angle_alpha 112.3410(10) _cell_angle_beta 100.392(2) _cell_angle_gamma 94.466(2) _cell_volume 1462.16(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9841 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 36.26 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 0.712 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 43064 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 36.39 _reflns_number_total 22969 _reflns_number_gt 20303 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0651P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _chemical_absolute_configuration ad _refine_ls_abs_structure_Flack 0.016(6) _refine_ls_number_reflns 22969 _refine_ls_number_parameters 766 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.1063 _refine_ls_wR_factor_gt 0.1018 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 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 C1A C 0.32011(14) 0.13219(7) 0.99606(8) 0.0161(2) Uani 1 1 d . . . C2A C 0.28998(15) 0.22887(8) 1.06951(9) 0.0191(2) Uani 1 1 d . . . C3A C 0.22341(15) 0.23319(8) 1.15394(8) 0.0194(2) Uani 1 1 d . . . H3A H 0.2054 0.2989 1.2018 0.023 Uiso 1 1 calc R . . C4A C 0.18142(15) 0.14119(8) 1.17060(9) 0.0202(2) Uani 1 1 d . . . C5A C 0.20886(15) 0.04786(8) 1.10050(9) 0.0206(2) Uani 1 1 d . . . H5A H 0.1820 -0.0143 1.1109 0.025 Uiso 1 1 calc R . . C6A C 0.27616(14) 0.04119(8) 1.01278(8) 0.0164(2) Uani 1 1 d . . . C7A C 0.28623(14) -0.06084(7) 0.93741(9) 0.0179(2) Uani 1 1 d . . . H7A H 0.2517 -0.1196 0.9515 0.021 Uiso 1 1 calc R . . C8A C 0.2987(2) 0.41284(9) 1.11460(11) 0.0371(3) Uani 1 1 d . . . H8A1 H 0.1808 0.4067 1.1153 0.056 Uiso 1 1 calc R . . H8A2 H 0.3269 0.4660 1.0879 0.056 Uiso 1 1 calc R . . H8A3 H 0.3649 0.4336 1.1866 0.056 Uiso 1 1 calc R . . C9A C 0.10530(17) 0.14863(9) 1.26350(10) 0.0253(2) Uani 1 1 d . . . H9A1 H -0.0107 0.1602 1.2478 0.030 Uiso 1 1 calc R . . H9A2 H 0.1032 0.0809 1.2712 0.030 Uiso 1 1 calc R . . C10A C 0.19563(18) 0.23438(10) 1.36574(10) 0.0265(3) Uani 1 1 d . . . H10A H 0.3091 0.2327 1.3902 0.032 Uiso 1 1 calc R . . C11A C 0.12937(19) 0.31358(10) 1.42586(10) 0.0284(3) Uani 1 1 d . . . H11A H 0.0162 0.3180 1.4042 0.034 Uiso 1 1 calc R . . H11B H 0.1954 0.3653 1.4902 0.034 Uiso 1 1 calc R . . C12A C 0.32393(13) -0.18821(7) 0.77272(9) 0.01898(19) Uani 1 1 d . . . H12A H 0.2218 -0.2027 0.7162 0.023 Uiso 1 1 calc R . . C13A C 0.31461(16) -0.27510(8) 0.81347(10) 0.0242(3) Uani 1 1 d . . . H13A H 0.2165 -0.2746 0.8443 0.029 Uiso 1 1 calc R . . H13B H 0.4147 -0.2633 0.8694 0.029 Uiso 1 1 calc R . . C14A C 0.30226(17) -0.38086(8) 0.72136(12) 0.0306(3) Uani 1 1 d . . . H14A H 0.1967 -0.3950 0.6690 0.037 Uiso 1 1 calc R . . H14B H 0.3017 -0.4372 0.7480 0.037 Uiso 1 1 calc R . . C15A C 0.44665(17) -0.38255(8) 0.66732(11) 0.0305(3) Uani 1 1 d . . . H15A H 0.4305 -0.4503 0.6054 0.037 Uiso 1 1 calc R . . H15B H 0.5509 -0.3773 0.7173 0.037 Uiso 1 1 calc R . . C16A C 0.46221(17) -0.29231(8) 0.63060(11) 0.0261(3) Uani 1 1 d . . . H16A H 0.5629 -0.2920 0.6024 0.031 Uiso 1 1 calc R . . H16B H 0.3651 -0.3023 0.5734 0.031 Uiso 1 1 calc R . . C17A C 0.47220(13) -0.18804(7) 0.72377(8) 0.01869(19) Uani 1 1 d . . . H17A H 0.5735 -0.1793 0.7789 0.022 Uiso 1 1 calc R . . C18A C 0.53449(14) -0.09022(8) 0.62215(9) 0.0184(2) Uani 1 1 d . . . H18A H 0.5612 -0.1537 0.5758 0.022 Uiso 1 1 calc R . . C19A C 0.55819(14) 0.00012(8) 0.59738(8) 0.0172(2) Uani 1 1 d . . . C20A C 0.61199(15) -0.01164(9) 0.50372(9) 0.0209(2) Uani 1 1 d . . . H20A H 0.6316 -0.0786 0.4596 0.025 Uiso 1 1 calc R . . C21A C 0.63638(16) 0.07100(9) 0.47527(9) 0.0214(2) Uani 1 1 d . . . C22A C 0.60512(15) 0.17051(8) 0.54130(8) 0.0185(2) Uani 1 1 d . . . H22A H 0.6178 0.2281 0.5215 0.022 Uiso 1 1 calc R . . C23A C 0.55620(14) 0.18427(7) 0.63452(8) 0.0162(2) Uani 1 1 d . . . C24A C 0.53205(13) 0.09886(7) 0.66586(8) 0.0148(2) Uani 1 1 d . . . C25A C 0.70186(17) 0.06175(10) 0.37857(9) 0.0262(3) Uani 1 1 d . . . H25A H 0.8107 0.1075 0.4015 0.031 Uiso 1 1 calc R . . H25B H 0.7187 -0.0115 0.3415 0.031 Uiso 1 1 calc R . . C26A C 0.58681(18) 0.09195(10) 0.30323(9) 0.0260(3) Uani 1 1 d . . . H26A H 0.4810 0.0497 0.2699 0.031 Uiso 1 1 calc R . . C27A C 0.62219(18) 0.17302(10) 0.27995(11) 0.0299(3) Uani 1 1 d . . . H27A H 0.7269 0.2170 0.3118 0.036 Uiso 1 1 calc R . . H27B H 0.5430 0.1875 0.2314 0.036 Uiso 1 1 calc R . . C28A C 0.53430(16) 0.36424(8) 0.67508(10) 0.0224(2) Uani 1 1 d . . . H28A H 0.6422 0.3787 0.6603 0.034 Uiso 1 1 calc R . . H28B H 0.5157 0.4263 0.7327 0.034 Uiso 1 1 calc R . . H28C H 0.4469 0.3473 0.6114 0.034 Uiso 1 1 calc R . . N1A N 0.33853(12) -0.07907(6) 0.85183(7) 0.01683(17) Uani 1 1 d . . . N2A N 0.48016(12) -0.09244(6) 0.70179(7) 0.01700(18) Uani 1 1 d . . . Ni1A Ni 0.422553(11) 0.019601(7) 0.806481(8) 0.01460(3) Uani 1 1 d . . . O1A O 0.38259(11) 0.13372(6) 0.91666(6) 0.01844(17) Uani 1 1 d . . . O2A O 0.48922(11) 0.11828(5) 0.75654(6) 0.01767(16) Uani 1 1 d . . . O3A O 0.53152(11) 0.27782(6) 0.70532(6) 0.01928(17) Uani 1 1 d . . . O4A O 0.33320(13) 0.31307(6) 1.04684(7) 0.02509(19) Uani 1 1 d . . . C1B C -0.10175(14) 0.86185(8) 0.79870(8) 0.0149(2) Uani 1 1 d . . . C2B C -0.13123(14) 0.77665(8) 0.83036(8) 0.0151(2) Uani 1 1 d . . . C3B C -0.18871(15) 0.78971(8) 0.91936(9) 0.0181(2) Uani 1 1 d . . . H3B H -0.2054 0.7317 0.9382 0.022 Uiso 1 1 calc R . . C4B C -0.22354(15) 0.88800(8) 0.98341(9) 0.0190(2) Uani 1 1 d . . . C5B C -0.19223(15) 0.97210(8) 0.95685(9) 0.0173(2) Uani 1 1 d . . . H5B H -0.2137 1.0389 0.9999 0.021 Uiso 1 1 calc R . . C6B C -0.12882(14) 0.96083(8) 0.86674(8) 0.0145(2) Uani 1 1 d . . . C7B C -0.08063(14) 1.05435(7) 0.85130(9) 0.0154(2) Uani 1 1 d . . . H7B H -0.0960 1.1196 0.9013 0.019 Uiso 1 1 calc R . . C8B C -0.10668(17) 0.59667(8) 0.79308(10) 0.0220(2) Uani 1 1 d . . . H8B1 H -0.0225 0.6147 0.8584 0.033 Uiso 1 1 calc R . . H8B2 H -0.0850 0.5344 0.7372 0.033 Uiso 1 1 calc R . . H8B3 H -0.2165 0.5820 0.8054 0.033 Uiso 1 1 calc R . . C9B C -0.29366(18) 0.89741(10) 1.07891(10) 0.0260(3) Uani 1 1 d . . . H9B1 H -0.3189 0.9692 1.1126 0.031 Uiso 1 1 calc R . . H9B2 H -0.3982 0.8474 1.0555 0.031 Uiso 1 1 calc R . . C10B C -0.17274(18) 0.87480(10) 1.15831(10) 0.0253(3) Uani 1 1 d . . . H10B H -0.0737 0.9239 1.1942 0.030 Uiso 1 1 calc R . . C11B C -0.19257(19) 0.79294(11) 1.18215(11) 0.0284(3) Uani 1 1 d . . . H11C H -0.2898 0.7419 1.1481 0.034 Uiso 1 1 calc R . . H11D H -0.1096 0.7848 1.2334 0.034 Uiso 1 1 calc R . . C12B C 0.05164(13) 1.15637(7) 0.77232(8) 0.01674(18) Uani 1 1 d . . . H12B H 0.1747 1.1668 0.7968 0.020 Uiso 1 1 calc R . . C13B C -0.00812(17) 1.25505(8) 0.83959(10) 0.0222(2) Uani 1 1 d . . . H13C H 0.0206 1.2661 0.9150 0.027 Uiso 1 1 calc R . . H13D H -0.1299 1.2477 0.8173 0.027 Uiso 1 1 calc R . . C14B C 0.07624(18) 1.34865(8) 0.82482(10) 0.0263(2) Uani 1 1 d . . . H14C H 0.0351 1.4130 0.8657 0.032 Uiso 1 1 calc R . . H14D H 0.1971 1.3589 0.8532 0.032 Uiso 1 1 calc R . . C15B C 0.04320(16) 1.33232(8) 0.70855(10) 0.0253(2) Uani 1 1 d . . . H15C H 0.1046 1.3925 0.7022 0.030 Uiso 1 1 calc R . . H15D H -0.0764 1.3300 0.6823 0.030 Uiso 1 1 calc R . . C16B C 0.09613(16) 1.23042(8) 0.64014(10) 0.0211(2) Uani 1 1 d . . . H16C H 0.0645 1.2188 0.5646 0.025 Uiso 1 1 calc R . . H16D H 0.2179 1.2357 0.6601 0.025 Uiso 1 1 calc R . . C17B C 0.01230(13) 1.13904(7) 0.65645(8) 0.01659(17) Uani 1 1 d . . . H17B H -0.1101 1.1342 0.6333 0.020 Uiso 1 1 calc R . . C18B C 0.11593(14) 1.01667(8) 0.51643(9) 0.0165(2) Uani 1 1 d . . . H18B H 0.1383 1.0742 0.4977 0.020 Uiso 1 1 calc R . . C19B C 0.15078(15) 0.91671(8) 0.44986(9) 0.0166(2) Uani 1 1 d . . . C20B C 0.22275(16) 0.91173(8) 0.36459(9) 0.0187(2) Uani 1 1 d . . . H20B H 0.2486 0.9740 0.3541 0.022 Uiso 1 1 calc R . . C21B C 0.25629(15) 0.81775(9) 0.29608(9) 0.0193(2) Uani 1 1 d . . . C22B C 0.21699(15) 0.72657(9) 0.31385(9) 0.0193(2) Uani 1 1 d . . . H22B H 0.2392 0.6613 0.2678 0.023 Uiso 1 1 calc R . . C23B C 0.14687(15) 0.73065(8) 0.39704(9) 0.0175(2) Uani 1 1 d . . . C24B C 0.11135(15) 0.82704(8) 0.46935(9) 0.0159(2) Uani 1 1 d . . . C25B C 0.33634(18) 0.81205(10) 0.20565(10) 0.0252(3) Uani 1 1 d . . . H25C H 0.3446 0.8814 0.2013 0.030 Uiso 1 1 calc R . . H25D H 0.4502 0.7971 0.2212 0.030 Uiso 1 1 calc R . . C26B C 0.24405(18) 0.73007(10) 0.10034(10) 0.0236(3) Uani 1 1 d . . . H26B H 0.1319 0.7350 0.0763 0.028 Uiso 1 1 calc R . . C27B C 0.3058(2) 0.65152(10) 0.03815(11) 0.0271(3) Uani 1 1 d . . . H27C H 0.4174 0.6437 0.0592 0.033 Uiso 1 1 calc R . . H27D H 0.2385 0.6029 -0.0275 0.033 Uiso 1 1 calc R . . C28B C 0.1424(3) 0.54751(11) 0.35403(13) 0.0438(4) Uani 1 1 d . . . H28D H 0.0832 0.5269 0.2804 0.066 Uiso 1 1 calc R . . H28E H 0.1087 0.4941 0.3791 0.066 Uiso 1 1 calc R . . H28F H 0.2619 0.5540 0.3584 0.066 Uiso 1 1 calc R . . N1B N -0.01758(12) 1.05512(6) 0.77343(7) 0.01452(17) Uani 1 1 d . . . N2B N 0.05648(12) 1.03466(6) 0.59983(7) 0.01569(17) Uani 1 1 d . . . Ni1B Ni 0.008172(11) 0.939607(7) 0.657789(8) 0.01292(3) Uani 1 1 d . . . O1B O -0.05145(10) 0.84229(6) 0.71104(6) 0.01488(16) Uani 1 1 d . . . O2B O 0.04467(11) 0.82434(6) 0.54587(6) 0.01733(17) Uani 1 1 d . . . O3B O -0.10101(11) 0.68253(6) 0.76133(7) 0.01841(17) Uani 1 1 d . . . O4B O 0.10400(14) 0.64539(6) 0.41805(7) 0.0267(2) Uani 1 1 d . . . O1C O 0.7550(3) 0.42605(11) 0.50028(14) 0.0739(5) Uani 1 1 d . . . H1C H 0.8332 0.4674 0.4994 0.111 Uiso 1 1 calc R . . C1C C 0.6089(3) 0.42413(17) 0.4281(2) 0.0680(8) Uani 1 1 d . . . H1C1 H 0.5702 0.4919 0.4548 0.102 Uiso 1 1 calc R . . H1C2 H 0.5226 0.3683 0.4209 0.102 Uiso 1 1 calc R . . H1C3 H 0.6335 0.4109 0.3588 0.102 Uiso 1 1 calc R . . O1D O 0.84083(17) 0.29219(10) 0.04711(10) 0.0526(3) Uani 1 1 d . . . H1D H 0.7693 0.3061 0.0059 0.079 Uiso 1 1 calc R . . C1D C 0.7776(2) 0.29072(16) 0.13155(13) 0.0489(4) Uani 1 1 d . . . H1D1 H 0.8635 0.2792 0.1820 0.073 Uiso 1 1 calc R . . H1D2 H 0.6830 0.2339 0.1056 0.073 Uiso 1 1 calc R . . H1D3 H 0.7415 0.3580 0.1667 0.073 Uiso 1 1 calc R . . C1E C 0.8287(3) 0.53871(14) 0.03282(19) 0.0542(5) Uani 1 1 d . . . H1E1 H 0.8914 0.6097 0.0596 0.081 Uiso 1 1 calc R . . H1E2 H 0.8892 0.4883 -0.0107 0.081 Uiso 1 1 calc R . . H1E3 H 0.8143 0.5214 0.0926 0.081 Uiso 1 1 calc R . . O1E O 0.6738(2) 0.53407(11) -0.02834(17) 0.0747(6) Uani 1 1 d . . . H1E H 0.6152 0.4760 -0.0441 0.112 Uiso 1 1 calc R . . C1F C 0.6707(4) 0.6765(2) 0.3355(2) 0.0366(6) Uani 0.568(3) 1 d PDU A 1 H1F1 H 0.6744 0.7510 0.3492 0.055 Uiso 0.568(3) 1 calc PR A 1 H1F2 H 0.6050 0.6337 0.2638 0.055 Uiso 0.568(3) 1 calc PR A 1 H1F3 H 0.7834 0.6600 0.3419 0.055 Uiso 0.568(3) 1 calc PR A 1 O1F O 0.5981(3) 0.6547(2) 0.40909(19) 0.0632(7) Uani 0.568(3) 1 d PDU A 1 H1F H 0.6407 0.6073 0.4224 0.095 Uiso 0.568(3) 1 calc PRD A 1 C1F' C 0.6621(9) 0.6398(4) 0.3251(4) 0.0661(14) Uani 0.432(3) 1 d PDU A 2 H1F4 H 0.5737 0.6478 0.2734 0.099 Uiso 0.432(3) 1 calc PR A 2 H1F5 H 0.6305 0.5752 0.3342 0.099 Uiso 0.432(3) 1 calc PR A 2 H1F6 H 0.7646 0.6361 0.2997 0.099 Uiso 0.432(3) 1 calc PR A 2 O1F' O 0.6876(11) 0.7284(5) 0.4248(5) 0.160(3) Uani 0.432(3) 1 d PDU A 2 H1F' H 0.7142 0.7088 0.4744 0.240 Uiso 0.432(3) 1 calc PR A 2 O1W O 0.56022(13) 0.32584(7) 0.92444(7) 0.0291(2) Uani 1 1 d DU . . H11W H 0.5113(9) 0.2899(3) 0.9515(4) 0.035 Uiso 1 1 d D . . H12W H 0.4816(7) 0.3473(5) 0.8940(6) 0.035 Uiso 1 1 d D . . O2W O 0.8843(2) 0.62935(10) 0.54359(9) 0.0528(4) Uani 1 1 d DU . . H21W H 0.9685(6) 0.6011(5) 0.5555(8) 0.063 Uiso 1 1 d D . . H22W H 0.8872(12) 0.6791(7) 0.6029(5) 0.063 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1A 0.0172(4) 0.0145(3) 0.0173(4) 0.0076(3) 0.0034(3) 0.0023(3) C2A 0.0232(5) 0.0179(3) 0.0205(4) 0.0119(3) 0.0061(3) 0.0034(3) C3A 0.0209(5) 0.0201(4) 0.0186(4) 0.0089(3) 0.0057(3) 0.0025(3) C4A 0.0195(5) 0.0233(4) 0.0206(4) 0.0125(3) 0.0046(3) 0.0007(3) C5A 0.0207(5) 0.0232(4) 0.0210(4) 0.0142(3) 0.0027(3) -0.0011(3) C6A 0.0158(4) 0.0180(3) 0.0172(3) 0.0096(3) 0.0027(3) 0.0013(3) C7A 0.0159(4) 0.0157(3) 0.0238(4) 0.0107(3) 0.0034(3) 0.0010(3) C8A 0.0720(9) 0.0149(4) 0.0323(5) 0.0087(4) 0.0293(5) 0.0145(5) C9A 0.0270(5) 0.0277(4) 0.0269(4) 0.0151(3) 0.0118(4) 0.0015(4) C10A 0.0262(5) 0.0341(5) 0.0218(4) 0.0145(4) 0.0054(4) 0.0024(4) C11A 0.0321(6) 0.0277(5) 0.0267(5) 0.0116(4) 0.0092(4) 0.0029(4) C12A 0.0161(4) 0.0112(3) 0.0267(4) 0.0062(3) 0.0018(3) 0.0005(3) C13A 0.0206(5) 0.0143(3) 0.0382(5) 0.0112(3) 0.0075(4) 0.0015(3) C14A 0.0259(5) 0.0125(3) 0.0506(7) 0.0094(4) 0.0105(5) 0.0004(3) C15A 0.0312(6) 0.0133(3) 0.0476(6) 0.0101(4) 0.0139(5) 0.0061(4) C16A 0.0301(6) 0.0127(3) 0.0347(5) 0.0074(3) 0.0093(4) 0.0047(4) C17A 0.0168(4) 0.0115(3) 0.0272(4) 0.0080(3) 0.0033(3) 0.0023(3) C18A 0.0199(4) 0.0132(3) 0.0177(4) 0.0024(3) 0.0014(3) 0.0038(3) C19A 0.0193(4) 0.0137(3) 0.0163(4) 0.0040(3) 0.0029(3) 0.0037(3) C20A 0.0238(5) 0.0195(4) 0.0163(4) 0.0031(3) 0.0043(3) 0.0077(3) C21A 0.0257(5) 0.0225(4) 0.0151(4) 0.0057(3) 0.0051(3) 0.0074(4) C22A 0.0224(4) 0.0188(3) 0.0152(3) 0.0072(3) 0.0045(3) 0.0067(3) C23A 0.0191(4) 0.0126(3) 0.0160(4) 0.0048(3) 0.0039(3) 0.0034(3) C24A 0.0154(4) 0.0125(3) 0.0160(3) 0.0051(3) 0.0027(3) 0.0038(3) C25A 0.0341(5) 0.0292(4) 0.0191(4) 0.0090(3) 0.0126(4) 0.0145(4) C26A 0.0300(6) 0.0272(5) 0.0163(4) 0.0058(4) 0.0022(4) 0.0017(4) C27A 0.0268(6) 0.0374(5) 0.0345(5) 0.0225(4) 0.0105(4) 0.0058(4) C28A 0.0272(5) 0.0154(3) 0.0288(4) 0.0118(3) 0.0096(4) 0.0051(3) N1A 0.0147(4) 0.0133(3) 0.0222(3) 0.0076(2) 0.0029(3) 0.0015(2) N2A 0.0168(4) 0.0114(3) 0.0212(3) 0.0058(2) 0.0020(3) 0.0031(2) Ni1A 0.01639(6) 0.01001(4) 0.01711(5) 0.00514(4) 0.00355(4) 0.00271(4) O1A 0.0244(4) 0.0140(2) 0.0191(3) 0.0074(2) 0.0082(3) 0.0046(2) O2A 0.0245(4) 0.0131(2) 0.0173(3) 0.0063(2) 0.0083(2) 0.0050(2) O3A 0.0272(4) 0.0128(2) 0.0188(3) 0.0062(2) 0.0074(3) 0.0051(3) O4A 0.0430(5) 0.0128(3) 0.0235(3) 0.0067(2) 0.0175(3) 0.0071(3) C1B 0.0149(4) 0.0129(3) 0.0162(4) 0.0050(3) 0.0044(3) 0.0009(3) C2B 0.0162(4) 0.0129(3) 0.0156(4) 0.0048(3) 0.0041(3) 0.0036(3) C3B 0.0196(4) 0.0184(4) 0.0194(4) 0.0092(3) 0.0080(3) 0.0032(3) C4B 0.0227(5) 0.0178(4) 0.0180(4) 0.0070(3) 0.0083(3) 0.0048(3) C5B 0.0200(5) 0.0147(4) 0.0169(4) 0.0052(3) 0.0061(3) 0.0034(3) C6B 0.0150(4) 0.0127(3) 0.0147(4) 0.0042(3) 0.0037(3) 0.0028(3) C7B 0.0172(4) 0.0109(3) 0.0169(4) 0.0043(3) 0.0036(3) 0.0022(3) C8B 0.0277(5) 0.0149(4) 0.0282(5) 0.0116(3) 0.0105(4) 0.0058(4) C9B 0.0353(6) 0.0260(4) 0.0240(4) 0.0126(4) 0.0162(4) 0.0109(4) C10B 0.0320(6) 0.0231(5) 0.0175(4) 0.0051(4) 0.0081(4) -0.0043(4) C11B 0.0244(6) 0.0347(5) 0.0290(5) 0.0154(4) 0.0079(4) 0.0028(5) C12B 0.0162(4) 0.0116(3) 0.0217(4) 0.0063(3) 0.0038(3) 0.0010(3) C13B 0.0279(5) 0.0122(4) 0.0249(5) 0.0034(3) 0.0106(4) 0.0039(3) C14B 0.0346(6) 0.0124(3) 0.0302(5) 0.0056(3) 0.0110(4) 0.0004(4) C15B 0.0312(5) 0.0140(3) 0.0352(5) 0.0120(3) 0.0124(4) 0.0062(3) C16B 0.0272(5) 0.0132(3) 0.0270(4) 0.0108(3) 0.0096(4) 0.0033(3) C17B 0.0174(4) 0.0121(3) 0.0203(4) 0.0064(3) 0.0042(3) 0.0036(3) C18B 0.0183(4) 0.0124(3) 0.0192(4) 0.0070(3) 0.0040(3) 0.0022(3) C19B 0.0171(5) 0.0136(3) 0.0189(4) 0.0065(3) 0.0040(3) 0.0015(3) C20B 0.0201(5) 0.0157(4) 0.0194(4) 0.0054(3) 0.0072(4) 0.0002(3) C21B 0.0179(5) 0.0205(4) 0.0184(4) 0.0064(3) 0.0061(3) 0.0001(4) C22B 0.0226(5) 0.0180(4) 0.0180(4) 0.0057(3) 0.0084(3) 0.0055(3) C23B 0.0222(5) 0.0129(3) 0.0177(4) 0.0047(3) 0.0081(3) 0.0044(3) C24B 0.0177(4) 0.0141(3) 0.0162(4) 0.0058(3) 0.0045(3) 0.0029(3) C25B 0.0289(6) 0.0226(5) 0.0207(5) 0.0041(4) 0.0111(4) -0.0036(4) C26B 0.0280(6) 0.0252(4) 0.0204(4) 0.0105(4) 0.0090(4) 0.0046(4) C27B 0.0326(7) 0.0247(5) 0.0216(5) 0.0073(4) 0.0062(4) 0.0010(5) C28B 0.0888(11) 0.0200(5) 0.0358(6) 0.0135(4) 0.0358(7) 0.0214(6) N1B 0.0155(4) 0.0104(3) 0.0170(3) 0.0051(2) 0.0031(3) 0.0022(2) N2B 0.0158(4) 0.0115(3) 0.0204(3) 0.0067(2) 0.0045(3) 0.0032(2) Ni1B 0.01480(5) 0.00955(4) 0.01499(5) 0.00503(4) 0.00438(4) 0.00244(4) O1B 0.0186(3) 0.0113(3) 0.0160(3) 0.0054(2) 0.0069(2) 0.0033(2) O2B 0.0239(4) 0.0129(3) 0.0172(3) 0.0062(2) 0.0091(3) 0.0039(3) O3B 0.0264(4) 0.0115(3) 0.0213(3) 0.0077(2) 0.0112(3) 0.0064(3) O4B 0.0473(5) 0.0148(3) 0.0268(4) 0.0114(3) 0.0202(3) 0.0112(3) O1C 0.0996(14) 0.0522(7) 0.0741(8) 0.0352(6) 0.0181(9) -0.0118(8) C1C 0.0518(12) 0.0399(10) 0.0843(15) -0.0074(10) 0.0277(11) -0.0100(9) O1D 0.0543(6) 0.0816(6) 0.0552(5) 0.0489(4) 0.0342(4) 0.0369(5) C1D 0.0403(8) 0.0805(9) 0.0453(6) 0.0402(6) 0.0209(5) 0.0154(7) C1E 0.0612(11) 0.0305(7) 0.0725(11) 0.0138(7) 0.0370(9) 0.0013(7) O1E 0.0681(11) 0.0311(6) 0.1179(14) 0.0314(7) 0.0059(10) -0.0030(6) C1F 0.0404(13) 0.0451(12) 0.0327(10) 0.0222(9) 0.0139(9) 0.0072(10) O1F 0.0365(11) 0.1182(15) 0.0745(11) 0.0736(10) 0.0252(8) 0.0243(10) C1F' 0.071(3) 0.067(2) 0.078(2) 0.0508(17) 0.014(2) 0.001(2) O1F' 0.146(4) 0.165(4) 0.165(4) 0.058(3) 0.032(3) 0.057(3) O1W 0.0385(5) 0.0220(3) 0.0226(4) 0.0051(3) 0.0089(3) -0.0036(3) O2W 0.0782(9) 0.0384(6) 0.0310(5) 0.0019(4) 0.0261(5) -0.0213(6) _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 C1A O1A 1.3178(15) . ? C1A C6A 1.4092(16) . ? C1A C2A 1.4259(14) . ? C2A O4A 1.3675(15) . ? C2A C3A 1.3787(17) . ? C3A C4A 1.4185(17) . ? C4A C5A 1.3669(15) . ? C4A C9A 1.5217(18) . ? C5A C6A 1.4163(17) . ? C6A C7A 1.4345(14) . ? C7A N1A 1.2917(16) . ? C8A O4A 1.4418(15) . ? C9A C10A 1.4899(16) . ? C10A C11A 1.3380(19) . ? C12A N1A 1.4843(12) . ? C12A C17A 1.5164(16) . ? C12A C13A 1.5268(17) . ? C13A C14A 1.5286(16) . ? C14A C15A 1.529(2) . ? C15A C16A 1.5360(19) . ? C16A C17A 1.5258(14) . ? C17A N2A 1.4783(14) . ? C18A N2A 1.2882(17) . ? C18A C19A 1.4378(17) . ? C19A C24A 1.4085(13) . ? C19A C20A 1.4188(18) . ? C20A C21A 1.3686(18) . ? C21A C22A 1.4208(15) . ? C21A C25A 1.5158(18) . ? C22A C23A 1.3877(16) . ? C23A O3A 1.3646(12) . ? C23A C24A 1.4306(16) . ? C24A O2A 1.3172(14) . ? C25A C26A 1.4990(19) . ? C26A C27A 1.318(2) . ? C28A O3A 1.4221(15) . ? N1A Ni1A 1.8615(10) . ? N2A Ni1A 1.8589(9) . ? Ni1A O1A 1.8525(8) . ? Ni1A O2A 1.8570(9) . ? C1B O1B 1.3076(14) . ? C1B C6B 1.4117(14) . ? C1B C2B 1.4373(16) . ? C2B C3B 1.3699(17) . ? C2B O3B 1.3777(12) . ? C3B C4B 1.4111(15) . ? C4B C5B 1.3795(17) . ? C4B C9B 1.5206(19) . ? C5B C6B 1.4154(17) . ? C6B C7B 1.4405(16) . ? C7B N1B 1.2974(16) . ? C8B O3B 1.4284(15) . ? C9B C10B 1.505(2) . ? C10B C11B 1.313(2) . ? C12B N1B 1.4903(13) . ? C12B C17B 1.5180(15) . ? C12B C13B 1.5237(15) . ? C13B C14B 1.5352(18) . ? C14B C15B 1.5276(18) . ? C15B C16B 1.5327(15) . ? C16B C17B 1.5183(16) . ? C17B N2B 1.4819(12) . ? C18B N2B 1.2965(16) . ? C18B C19B 1.4393(14) . ? C19B C24B 1.4058(17) . ? C19B C20B 1.4127(18) . ? C20B C21B 1.3844(16) . ? C21B C22B 1.4119(18) . ? C21B C25B 1.5150(19) . ? C22B C23B 1.3804(18) . ? C23B O4B 1.3666(15) . ? C23B C24B 1.4346(15) . ? C24B O2B 1.3053(15) . ? C25B C26B 1.4999(17) . ? C26B C27B 1.3222(19) . ? C28B O4B 1.4189(17) . ? N1B Ni1B 1.8618(8) . ? N2B Ni1B 1.8538(10) . ? Ni1B O1B 1.8567(9) . ? Ni1B O2B 1.8633(8) . ? O1C C1C 1.427(3) . ? O1D C1D 1.386(2) . ? C1E O1E 1.395(3) . ? C1F O1F 1.399(3) . ? C1F' O1F' 1.438(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A C1A C6A 124.86(9) . . ? O1A C1A C2A 118.18(10) . . ? C6A C1A C2A 116.94(11) . . ? O4A C2A C3A 125.18(9) . . ? O4A C2A C1A 113.39(10) . . ? C3A C2A C1A 121.44(10) . . ? C2A C3A C4A 121.08(10) . . ? C5A C4A C3A 118.12(11) . . ? C5A C4A C9A 122.23(11) . . ? C3A C4A C9A 119.64(10) . . ? C4A C5A C6A 121.91(11) . . ? C1A C6A C5A 120.50(9) . . ? C1A C6A C7A 120.97(10) . . ? C5A C6A C7A 118.36(10) . . ? N1A C7A C6A 125.15(10) . . ? C10A C9A C4A 113.61(11) . . ? C11A C10A C9A 125.10(13) . . ? N1A C12A C17A 105.21(8) . . ? N1A C12A C13A 116.67(10) . . ? C17A C12A C13A 110.96(9) . . ? C12A C13A C14A 108.94(11) . . ? C13A C14A C15A 111.53(10) . . ? C14A C15A C16A 112.17(10) . . ? C17A C16A C15A 109.51(11) . . ? N2A C17A C12A 105.35(8) . . ? N2A C17A C16A 116.99(10) . . ? C12A C17A C16A 111.11(9) . . ? N2A C18A C19A 125.63(9) . . ? C24A C19A C20A 120.60(11) . . ? C24A C19A C18A 120.70(11) . . ? C20A C19A C18A 118.68(9) . . ? C21A C20A C19A 121.68(10) . . ? C20A C21A C22A 118.64(11) . . ? C20A C21A C25A 122.68(10) . . ? C22A C21A C25A 118.64(11) . . ? C23A C22A C21A 120.58(11) . . ? O3A C23A C22A 124.67(10) . . ? O3A C23A C24A 113.95(10) . . ? C22A C23A C24A 121.35(9) . . ? O2A C24A C19A 124.92(10) . . ? O2A C24A C23A 117.99(8) . . ? C19A C24A C23A 117.09(10) . . ? C26A C25A C21A 112.38(11) . . ? C27A C26A C25A 124.58(13) . . ? C7A N1A C12A 120.55(9) . . ? C7A N1A Ni1A 127.17(7) . . ? C12A N1A Ni1A 112.13(8) . . ? C18A N2A C17A 120.88(9) . . ? C18A N2A Ni1A 126.74(8) . . ? C17A N2A Ni1A 112.16(7) . . ? O1A Ni1A O2A 84.82(4) . . ? O1A Ni1A N2A 175.44(4) . . ? O2A Ni1A N2A 94.68(4) . . ? O1A Ni1A N1A 94.47(4) . . ? O2A Ni1A N1A 175.47(4) . . ? N2A Ni1A N1A 86.38(4) . . ? C1A O1A Ni1A 127.15(7) . . ? C24A O2A Ni1A 126.50(6) . . ? C23A O3A C28A 117.64(9) . . ? C2A O4A C8A 116.61(10) . . ? O1B C1B C6B 125.50(11) . . ? O1B C1B C2B 118.21(9) . . ? C6B C1B C2B 116.29(10) . . ? C3B C2B O3B 124.57(10) . . ? C3B C2B C1B 121.93(9) . . ? O3B C2B C1B 113.47(10) . . ? C2B C3B C4B 120.98(11) . . ? C5B C4B C3B 118.53(11) . . ? C5B C4B C9B 122.51(10) . . ? C3B C4B C9B 118.97(11) . . ? C4B C5B C6B 121.33(10) . . ? C1B C6B C5B 120.81(10) . . ? C1B C6B C7B 121.00(11) . . ? C5B C6B C7B 118.01(9) . . ? N1B C7B C6B 124.17(9) . . ? C10B C9B C4B 110.96(12) . . ? C11B C10B C9B 125.53(13) . . ? N1B C12B C17B 104.89(7) . . ? N1B C12B C13B 117.23(10) . . ? C17B C12B C13B 111.05(9) . . ? C12B C13B C14B 108.21(10) . . ? C15B C14B C13B 111.93(9) . . ? C14B C15B C16B 111.62(10) . . ? C17B C16B C15B 109.39(10) . . ? N2B C17B C12B 104.96(8) . . ? N2B C17B C16B 116.47(9) . . ? C12B C17B C16B 111.33(8) . . ? N2B C18B C19B 125.39(11) . . ? C24B C19B C20B 121.64(10) . . ? C24B C19B C18B 120.21(11) . . ? C20B C19B C18B 118.14(10) . . ? C21B C20B C19B 121.19(11) . . ? C20B C21B C22B 118.15(12) . . ? C20B C21B C25B 121.53(12) . . ? C22B C21B C25B 120.31(10) . . ? C23B C22B C21B 121.10(10) . . ? O4B C23B C22B 124.15(10) . . ? O4B C23B C24B 113.98(11) . . ? C22B C23B C24B 121.87(11) . . ? O2B C24B C19B 125.78(10) . . ? O2B C24B C23B 118.16(10) . . ? C19B C24B C23B 116.05(11) . . ? C26B C25B C21B 113.71(11) . . ? C27B C26B C25B 125.43(13) . . ? C7B N1B C12B 120.38(8) . . ? C7B N1B Ni1B 127.35(7) . . ? C12B N1B Ni1B 112.21(7) . . ? C18B N2B C17B 120.15(9) . . ? C18B N2B Ni1B 126.90(7) . . ? C17B N2B Ni1B 112.89(7) . . ? N2B Ni1B O1B 176.92(4) . . ? N2B Ni1B N1B 86.08(4) . . ? O1B Ni1B N1B 94.60(4) . . ? N2B Ni1B O2B 94.37(4) . . ? O1B Ni1B O2B 85.10(4) . . ? N1B Ni1B O2B 177.11(4) . . ? C1B O1B Ni1B 126.54(7) . . ? C24B O2B Ni1B 126.41(7) . . ? C2B O3B C8B 117.27(9) . . ? C23B O4B C28B 117.98(12) . . ? 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 O1A C1A C2A O4A -0.55(15) . . . . ? C6A C1A C2A O4A -178.91(10) . . . . ? O1A C1A C2A C3A 179.39(10) . . . . ? C6A C1A C2A C3A 1.03(16) . . . . ? O4A C2A C3A C4A 179.58(11) . . . . ? C1A C2A C3A C4A -0.35(18) . . . . ? C2A C3A C4A C5A 0.02(17) . . . . ? C2A C3A C4A C9A -178.90(11) . . . . ? C3A C4A C5A C6A -0.41(17) . . . . ? C9A C4A C5A C6A 178.48(11) . . . . ? O1A C1A C6A C5A -179.64(10) . . . . ? C2A C1A C6A C5A -1.40(16) . . . . ? O1A C1A C6A C7A -4.54(17) . . . . ? C2A C1A C6A C7A 173.70(10) . . . . ? C4A C5A C6A C1A 1.14(17) . . . . ? C4A C5A C6A C7A -174.09(11) . . . . ? C1A C6A C7A N1A 1.97(17) . . . . ? C5A C6A C7A N1A 177.18(11) . . . . ? C5A C4A C9A C10A 132.94(12) . . . . ? C3A C4A C9A C10A -48.19(16) . . . . ? C4A C9A C10A C11A 121.53(16) . . . . ? N1A C12A C13A C14A -179.31(10) . . . . ? C17A C12A C13A C14A -58.86(12) . . . . ? C12A C13A C14A C15A 56.23(14) . . . . ? C13A C14A C15A C16A -55.15(15) . . . . ? C14A C15A C16A C17A 54.03(14) . . . . ? N1A C12A C17A N2A -45.21(10) . . . . ? C13A C12A C17A N2A -172.24(8) . . . . ? N1A C12A C17A C16A -172.84(9) . . . . ? C13A C12A C17A C16A 60.13(12) . . . . ? C15A C16A C17A N2A -177.35(10) . . . . ? C15A C16A C17A C12A -56.34(13) . . . . ? N2A C18A C19A C24A 4.24(17) . . . . ? N2A C18A C19A C20A -177.13(11) . . . . ? C24A C19A C20A C21A -1.61(17) . . . . ? C18A C19A C20A C21A 179.75(11) . . . . ? C19A C20A C21A C22A -0.61(17) . . . . ? C19A C20A C21A C25A 176.90(11) . . . . ? C20A C21A C22A C23A 2.13(17) . . . . ? C25A C21A C22A C23A -175.48(11) . . . . ? C21A C22A C23A O3A 176.56(10) . . . . ? C21A C22A C23A C24A -1.46(17) . . . . ? C20A C19A C24A O2A -176.92(10) . . . . ? C18A C19A C24A O2A 1.69(17) . . . . ? C20A C19A C24A C23A 2.23(15) . . . . ? C18A C19A C24A C23A -179.16(10) . . . . ? O3A C23A C24A O2A 0.27(14) . . . . ? C22A C23A C24A O2A 178.49(10) . . . . ? O3A C23A C24A C19A -178.94(9) . . . . ? C22A C23A C24A C19A -0.73(15) . . . . ? C20A C21A C25A C26A 122.93(13) . . . . ? C22A C21A C25A C26A -59.56(14) . . . . ? C21A C25A C26A C27A 115.38(15) . . . . ? C6A C7A N1A C12A -172.24(10) . . . . ? C6A C7A N1A Ni1A 3.00(17) . . . . ? C17A C12A N1A C7A -147.92(10) . . . . ? C13A C12A N1A C7A -24.46(15) . . . . ? C17A C12A N1A Ni1A 36.17(10) . . . . ? C13A C12A N1A Ni1A 159.63(8) . . . . ? C19A C18A N2A C17A -175.53(10) . . . . ? C19A C18A N2A Ni1A -1.36(17) . . . . ? C12A C17A N2A C18A -147.91(10) . . . . ? C16A C17A N2A C18A -23.93(15) . . . . ? C12A C17A N2A Ni1A 37.13(9) . . . . ? C16A C17A N2A Ni1A 161.11(8) . . . . ? C18A N2A Ni1A O1A -88.0(6) . . . . ? C17A N2A Ni1A O1A 86.6(6) . . . . ? C18A N2A Ni1A O2A -4.52(10) . . . . ? C17A N2A Ni1A O2A 170.08(7) . . . . ? C18A N2A Ni1A N1A 171.06(10) . . . . ? C17A N2A Ni1A N1A -14.33(7) . . . . ? C7A N1A Ni1A O1A -4.34(10) . . . . ? C12A N1A Ni1A O1A 171.24(7) . . . . ? C7A N1A Ni1A O2A -85.1(5) . . . . ? C12A N1A Ni1A O2A 90.5(5) . . . . ? C7A N1A Ni1A N2A 171.17(10) . . . . ? C12A N1A Ni1A N2A -13.25(7) . . . . ? C6A C1A O1A Ni1A 1.94(16) . . . . ? C2A C1A O1A Ni1A -176.28(8) . . . . ? O2A Ni1A O1A C1A 177.44(9) . . . . ? N2A Ni1A O1A C1A -98.7(6) . . . . ? N1A Ni1A O1A C1A 1.93(9) . . . . ? C19A C24A O2A Ni1A -9.90(15) . . . . ? C23A C24A O2A Ni1A 170.95(7) . . . . ? O1A Ni1A O2A C24A -174.59(9) . . . . ? N2A Ni1A O2A C24A 9.97(9) . . . . ? N1A Ni1A O2A C24A -93.4(5) . . . . ? C22A C23A O3A C28A 8.88(16) . . . . ? C24A C23A O3A C28A -172.97(10) . . . . ? C3A C2A O4A C8A -2.94(17) . . . . ? C1A C2A O4A C8A 176.99(11) . . . . ? O1B C1B C2B C3B -178.04(11) . . . . ? C6B C1B C2B C3B 2.51(16) . . . . ? O1B C1B C2B O3B 0.08(14) . . . . ? C6B C1B C2B O3B -179.37(10) . . . . ? O3B C2B C3B C4B -177.11(11) . . . . ? C1B C2B C3B C4B 0.80(18) . . . . ? C2B C3B C4B C5B -2.54(18) . . . . ? C2B C3B C4B C9B 177.56(11) . . . . ? C3B C4B C5B C6B 0.89(18) . . . . ? C9B C4B C5B C6B -179.21(11) . . . . ? O1B C1B C6B C5B 176.48(11) . . . . ? C2B C1B C6B C5B -4.11(16) . . . . ? O1B C1B C6B C7B -8.48(17) . . . . ? C2B C1B C6B C7B 170.92(10) . . . . ? C4B C5B C6B C1B 2.53(17) . . . . ? C4B C5B C6B C7B -172.66(11) . . . . ? C1B C6B C7B N1B 3.28(17) . . . . ? C5B C6B C7B N1B 178.46(11) . . . . ? C5B C4B C9B C10B -116.75(13) . . . . ? C3B C4B C9B C10B 63.15(15) . . . . ? C4B C9B C10B C11B -112.02(16) . . . . ? N1B C12B C13B C14B -178.97(10) . . . . ? C17B C12B C13B C14B -58.45(12) . . . . ? C12B C13B C14B C15B 56.53(14) . . . . ? C13B C14B C15B C16B -55.90(14) . . . . ? C14B C15B C16B C17B 54.59(13) . . . . ? N1B C12B C17B N2B -45.18(10) . . . . ? C13B C12B C17B N2B -172.75(9) . . . . ? N1B C12B C17B C16B -172.02(9) . . . . ? C13B C12B C17B C16B 60.41(12) . . . . ? C15B C16B C17B N2B -177.11(9) . . . . ? C15B C16B C17B C12B -56.84(12) . . . . ? N2B C18B C19B C24B 3.79(18) . . . . ? N2B C18B C19B C20B -177.09(11) . . . . ? C24B C19B C20B C21B 0.49(18) . . . . ? C18B C19B C20B C21B -178.61(11) . . . . ? C19B C20B C21B C22B -0.18(18) . . . . ? C19B C20B C21B C25B -178.86(12) . . . . ? C20B C21B C22B C23B 0.08(18) . . . . ? C25B C21B C22B C23B 178.78(11) . . . . ? C21B C22B C23B O4B 179.20(11) . . . . ? C21B C22B C23B C24B -0.29(18) . . . . ? C20B C19B C24B O2B -179.90(11) . . . . ? C18B C19B C24B O2B -0.81(18) . . . . ? C20B C19B C24B C23B -0.66(17) . . . . ? C18B C19B C24B C23B 178.43(11) . . . . ? O4B C23B C24B O2B 0.33(16) . . . . ? C22B C23B C24B O2B 179.86(11) . . . . ? O4B C23B C24B C19B -178.97(10) . . . . ? C22B C23B C24B C19B 0.56(17) . . . . ? C20B C21B C25B C26B -128.20(13) . . . . ? C22B C21B C25B C26B 53.14(17) . . . . ? C21B C25B C26B C27B -122.19(16) . . . . ? C6B C7B N1B C12B -170.89(10) . . . . ? C6B C7B N1B Ni1B 6.20(17) . . . . ? C17B C12B N1B C7B -145.36(10) . . . . ? C13B C12B N1B C7B -21.66(15) . . . . ? C17B C12B N1B Ni1B 37.14(9) . . . . ? C13B C12B N1B Ni1B 160.84(8) . . . . ? C19B C18B N2B C17B -174.66(10) . . . . ? C19B C18B N2B Ni1B 2.35(17) . . . . ? C12B C17B N2B C18B -145.88(10) . . . . ? C16B C17B N2B C18B -22.26(14) . . . . ? C12B C17B N2B Ni1B 36.71(9) . . . . ? C16B C17B N2B Ni1B 160.34(8) . . . . ? C18B N2B Ni1B O1B -87.8(7) . . . . ? C17B N2B Ni1B O1B 89.4(7) . . . . ? C18B N2B Ni1B N1B 169.24(10) . . . . ? C17B N2B Ni1B N1B -13.56(7) . . . . ? C18B N2B Ni1B O2B -7.89(10) . . . . ? C17B N2B Ni1B O2B 169.30(7) . . . . ? C7B N1B Ni1B N2B 168.44(10) . . . . ? C12B N1B Ni1B N2B -14.27(7) . . . . ? C7B N1B Ni1B O1B -8.55(10) . . . . ? C12B N1B Ni1B O1B 168.74(7) . . . . ? C7B N1B Ni1B O2B -92.5(9) . . . . ? C12B N1B Ni1B O2B 84.7(9) . . . . ? C6B C1B O1B Ni1B 3.70(16) . . . . ? C2B C1B O1B Ni1B -175.69(7) . . . . ? N2B Ni1B O1B C1B -99.0(7) . . . . ? N1B Ni1B O1B C1B 3.70(9) . . . . ? O2B Ni1B O1B C1B -179.18(9) . . . . ? C19B C24B O2B Ni1B -7.94(17) . . . . ? C23B C24B O2B Ni1B 172.83(8) . . . . ? N2B Ni1B O2B C24B 10.59(10) . . . . ? O1B Ni1B O2B C24B -172.45(10) . . . . ? N1B Ni1B O2B C24B -88.2(9) . . . . ? C3B C2B O3B C8B -9.67(16) . . . . ? C1B C2B O3B C8B 172.27(10) . . . . ? C22B C23B O4B C28B 3.73(19) . . . . ? C24B C23B O4B C28B -176.75(13) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 36.39 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.931 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.124