# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Kim Dunbar' _publ_contact_author_email DUNBAR@MAIL.CHEM.TAMU.EDU _publ_section_title ; Magnetic Molecules Based on W(V) and Mo(V) Octacyanometallates with Ni(II) tmphen Units: A New Class of Trigonal Bipyramidal Cluster and Confirmation of SMM Behavior for the Pentadecanuclear Molecule [NiII{NiII(tmphen)(MeOH)}8{?-CN}30{WV(CN)3}6]. ; loop_ _publ_author_name 'K Dunbar' 'Matthew Hilfiger' 'Andrey V Prosvirin' 'Wolfgang Wernsdorfer' 'Hanhua Zhao.' # Attachment 'comp1-Ni3W2.cif' data_c:\comp1.cif _database_code_depnum_ccdc_archive 'CCDC 694537' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C120 H132 N28 Ni3 O10 W2' _chemical_formula_weight 2670.37 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 31.859(6) _cell_length_b 16.435(3) _cell_length_c 28.926(6) _cell_angle_alpha 90.00 _cell_angle_beta 116.12(3) _cell_angle_gamma 90.00 _cell_volume 13599(5) _cell_formula_units_Z 3 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.978 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4080 _exptl_absorpt_coefficient_mu 1.616 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS v2.03 (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD area-detector' _diffrn_measurement_method 'profile data from \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 117802 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 27.57 _reflns_number_total 30969 _reflns_number_gt 24826 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2000)' _computing_cell_refinement 'SMART V5.625 (Bruker, 2000)' _computing_data_reduction 'SAINT V6.32 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _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^)+(0.0844P)^2^+102.3046P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 30969 _refine_ls_number_parameters 1495 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1741 _refine_ls_wR_factor_gt 0.1630 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.168 _refine_ls_shift/su_mean 0.002 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 W1 W 0.328462(8) 0.700492(14) 0.723800(9) 0.01602(7) Uani 1 1 d . . . W2 W 0.204644(8) 0.338242(15) 0.552039(9) 0.01838(7) Uani 1 1 d . . . Ni1 Ni 0.32219(3) 0.38356(5) 0.74823(3) 0.01555(15) Uani 1 1 d . . . Ni2 Ni 0.33579(3) 0.54823(5) 0.56601(3) 0.01634(15) Uani 1 1 d . . . Ni3 Ni 0.15555(3) 0.63295(5) 0.58688(3) 0.01999(17) Uani 1 1 d . . . N2 N 0.33859(17) 0.5874(3) 0.6345(2) 0.0180(10) Uani 1 1 d . . . C13 C 0.1525(3) 0.2501(5) 0.5083(3) 0.0384(18) Uani 1 1 d . . . N9 N 0.28466(18) 0.3815(3) 0.6694(2) 0.0187(10) Uani 1 1 d . . . N3 N 0.22322(19) 0.6508(3) 0.6367(2) 0.0220(11) Uani 1 1 d . . . N19 N 0.34907(17) 0.3759(3) 0.82818(19) 0.0187(10) Uani 1 1 d . . . N1 N 0.32647(18) 0.5064(3) 0.7505(2) 0.0213(11) Uani 1 1 d . . . N11 N 0.16816(18) 0.5097(3) 0.5824(2) 0.0211(11) Uani 1 1 d . . . N23 N 0.32895(18) 0.5284(3) 0.4915(2) 0.0196(10) Uani 1 1 d . . . N26 N 0.1431(2) 0.7601(4) 0.5819(3) 0.0339(14) Uani 1 1 d . . . N25 N 0.16365(19) 0.6635(4) 0.5210(2) 0.0255(12) Uani 1 1 d . . . N22 N 0.40068(18) 0.6034(3) 0.5875(2) 0.0192(10) Uani 1 1 d . . . N21 N 0.38059(18) 0.4485(3) 0.5945(2) 0.0195(10) Uani 1 1 d . . . C50 C 0.4014(2) 0.3067(4) 0.6101(2) 0.0249(14) Uani 1 1 d . . . N10 N 0.27672(17) 0.4806(3) 0.5489(2) 0.0211(11) Uani 1 1 d . . . C18 C 0.4613(2) 0.4101(4) 0.7525(2) 0.0246(14) Uani 1 1 d . . . N24 N 0.30026(18) 0.6539(3) 0.5290(2) 0.0188(10) Uani 1 1 d . . . C3 C 0.2596(2) 0.6669(3) 0.6670(2) 0.0175(12) Uani 1 1 d . . . N20 N 0.26059(18) 0.3825(3) 0.7571(2) 0.0188(10) Uani 1 1 d . . . C11 C 0.1795(2) 0.4476(4) 0.5733(2) 0.0197(12) Uani 1 1 d . . . C25 C 0.2945(2) 0.1199(4) 0.7232(3) 0.0254(14) Uani 1 1 d . . . C14 C 0.1752(2) 0.2922(4) 0.6014(3) 0.0273(14) Uani 1 1 d . . . C68 C 0.3099(2) 0.5979(4) 0.4108(3) 0.0255(14) Uani 1 1 d . . . C5 C 0.2827(2) 0.8053(4) 0.7087(3) 0.0326(17) Uani 1 1 d . . . C26 C 0.2907(2) 0.2039(4) 0.7313(3) 0.0221(13) Uani 1 1 d . . . H26 H 0.2617 0.2233 0.7288 0.027 Uiso 1 1 calc R . . C56 C 0.4917(2) 0.6575(4) 0.6120(2) 0.0259(14) Uani 1 1 d . . . N17 N 0.38725(17) 0.3696(3) 0.74816(19) 0.0183(10) Uani 1 1 d . . . C42 C 0.2171(2) 0.3938(4) 0.7227(2) 0.0214(12) Uani 1 1 d . . . H42 H 0.2119 0.4111 0.6893 0.026 Uiso 1 1 calc R . . N18 N 0.32458(18) 0.2571(3) 0.7419(2) 0.0178(10) Uani 1 1 d . . . C7 C 0.2964(2) 0.6882(4) 0.7756(3) 0.0278(15) Uani 1 1 d . . . C9 C 0.2576(2) 0.3652(4) 0.6286(2) 0.0194(12) Uani 1 1 d . . . C21 C 0.4000(2) 0.2906(4) 0.7488(2) 0.0199(12) Uani 1 1 d . . . C49 C 0.3697(2) 0.3714(4) 0.5984(2) 0.0223(13) Uani 1 1 d . . . H49 H 0.3386 0.3596 0.5928 0.027 Uiso 1 1 calc R . . C106 C 0.1599(2) 0.6110(5) 0.6954(3) 0.0313(16) Uani 1 1 d . . . H106 H 0.1929 0.6124 0.7082 0.038 Uiso 1 1 calc R . . N7 N 0.2786(3) 0.6796(5) 0.8016(3) 0.0463(19) Uani 1 1 d . . . C55 C 0.4830(2) 0.5736(4) 0.6137(2) 0.0238(13) Uani 1 1 d . . . C69 C 0.3135(2) 0.5954(4) 0.4611(2) 0.0204(12) Uani 1 1 d . . . N8 N 0.4390(2) 0.6425(4) 0.7748(3) 0.0320(14) Uani 1 1 d . . . C33 C 0.3932(2) 0.3825(4) 0.8643(2) 0.0225(13) Uani 1 1 d . . . H33 H 0.4166 0.3963 0.8536 0.027 Uiso 1 1 calc R . . C70 C 0.2985(2) 0.6631(4) 0.4812(2) 0.0206(12) Uani 1 1 d . . . N4 N 0.3609(2) 0.8230(4) 0.6549(2) 0.0310(13) Uani 1 1 d . . . C67 C 0.3203(2) 0.5270(4) 0.3900(3) 0.0274(14) Uani 1 1 d . . . C71 C 0.2818(2) 0.7346(4) 0.4524(3) 0.0245(13) Uani 1 1 d . . . C35 C 0.3744(3) 0.3461(4) 0.9329(3) 0.0281(15) Uani 1 1 d . . . C59 C 0.5067(2) 0.4311(5) 0.6282(3) 0.0284(15) Uani 1 1 d . . . H59 H 0.5307 0.3916 0.6365 0.034 Uiso 1 1 calc R . . C27 C 0.4532(2) 0.1816(4) 0.7520(3) 0.0277(15) Uani 1 1 d . . . H27 H 0.4832 0.1644 0.7564 0.033 Uiso 1 1 calc R . . C6 C 0.3677(2) 0.7857(4) 0.7838(3) 0.0255(14) Uani 1 1 d . . . C22 C 0.3657(2) 0.2300(4) 0.7440(2) 0.0200(12) Uani 1 1 d . . . C53 C 0.4255(2) 0.4646(4) 0.6042(2) 0.0199(12) Uani 1 1 d . . . C34 C 0.4071(2) 0.3704(4) 0.9168(3) 0.0269(14) Uani 1 1 d . . . C10 C 0.2501(2) 0.4322(4) 0.5473(2) 0.0188(12) Uani 1 1 d . . . C38 C 0.2682(2) 0.3607(4) 0.8058(2) 0.0204(12) Uani 1 1 d . . . C72 C 0.2661(2) 0.7991(4) 0.4735(3) 0.0262(14) Uani 1 1 d . . . C8 C 0.4005(2) 0.6646(4) 0.7577(3) 0.0228(13) Uani 1 1 d . . . C2 C 0.3366(2) 0.6266(4) 0.6658(2) 0.0183(12) Uani 1 1 d . . . C81 C 0.1758(2) 0.6157(4) 0.4923(3) 0.0259(14) Uani 1 1 d . . . H81 H 0.1885 0.5638 0.5056 0.031 Uiso 1 1 calc R . . C41 C 0.1779(2) 0.3819(5) 0.7322(3) 0.0292(15) Uani 1 1 d . . . C28 C 0.4203(2) 0.1251(4) 0.7452(3) 0.0263(14) Uani 1 1 d . . . H28 H 0.4274 0.0692 0.7438 0.032 Uiso 1 1 calc R . . C58 C 0.4110(2) 0.6812(4) 0.5884(2) 0.0223(13) Uani 1 1 d . . . H58 H 0.3863 0.7193 0.5803 0.027 Uiso 1 1 calc R . . N28 N 0.13460(18) 0.6166(4) 0.6447(2) 0.0244(12) Uani 1 1 d . . . C73 C 0.2673(2) 0.7883(4) 0.5215(3) 0.0258(14) Uani 1 1 d . . . C54 C 0.4369(2) 0.5499(4) 0.6016(2) 0.0222(13) Uani 1 1 d . . . C17 C 0.4166(2) 0.4266(4) 0.7485(2) 0.0214(13) Uani 1 1 d . . . H17 H 0.4070 0.4818 0.7458 0.026 Uiso 1 1 calc R . . C20 C 0.4441(2) 0.2675(4) 0.7529(2) 0.0221(13) Uani 1 1 d . . . C65 C 0.3384(2) 0.4628(4) 0.4714(3) 0.0245(13) Uani 1 1 d . . . H65 H 0.3491 0.4158 0.4925 0.029 Uiso 1 1 calc R . . C4 C 0.3498(2) 0.7816(4) 0.6793(3) 0.0230(13) Uani 1 1 d . . . C23 C 0.3744(2) 0.1476(4) 0.7398(2) 0.0224(13) Uani 1 1 d . . . N14 N 0.1605(3) 0.2641(4) 0.6275(3) 0.0413(16) Uani 1 1 d . . . N27 N 0.08395(19) 0.6161(4) 0.5428(2) 0.0287(13) Uani 1 1 d . . . C62 C 0.4808(3) 0.2534(5) 0.6273(3) 0.0373(18) Uani 1 1 d . . . H62A H 0.4869 0.2264 0.6599 0.056 Uiso 1 1 calc R . . H62B H 0.5101 0.2747 0.6289 0.056 Uiso 1 1 calc R . . H62C H 0.4673 0.2142 0.5990 0.056 Uiso 1 1 calc R . . C39 C 0.2313(2) 0.3453(4) 0.8188(3) 0.0272(14) Uani 1 1 d . . . C1 C 0.32736(19) 0.5751(4) 0.7433(2) 0.0171(12) Uani 1 1 d . . . C74 C 0.2848(2) 0.7141(4) 0.5474(3) 0.0233(13) Uani 1 1 d . . . H74 H 0.2854 0.7071 0.5803 0.028 Uiso 1 1 calc R . . C19 C 0.4761(2) 0.3300(5) 0.7561(3) 0.0264(14) Uani 1 1 d . . . C80 C 0.2520(3) 0.8526(4) 0.5482(3) 0.0326(16) Uani 1 1 d . . . H80A H 0.2753 0.8963 0.5604 0.049 Uiso 1 1 calc R . . H80B H 0.2491 0.8282 0.5776 0.049 Uiso 1 1 calc R . . H80C H 0.2217 0.8748 0.5240 0.049 Uiso 1 1 calc R . . C36 C 0.3268(3) 0.3404(4) 0.8959(3) 0.0257(14) Uani 1 1 d . . . C61 C 0.3840(3) 0.2220(4) 0.6122(3) 0.0311(16) Uani 1 1 d . . . H61A H 0.3885 0.1872 0.5872 0.047 Uiso 1 1 calc R . . H5 H 0.3507 0.2241 0.6038 0.047 Uiso 1 1 calc R . . H61C H 0.4015 0.1995 0.6468 0.047 Uiso 1 1 calc R . . C43 C 0.2888(3) 0.3184(5) 0.9072(3) 0.0360(17) Uani 1 1 d . . . H43 H 0.2954 0.3017 0.9411 0.043 Uiso 1 1 calc R . . C51 C 0.4470(2) 0.3225(4) 0.6183(2) 0.0257(14) Uani 1 1 d . . . C15 C 0.2424(3) 0.2267(5) 0.5829(3) 0.0342(16) Uani 1 1 d . . . C16 C 0.2294(4) 0.2968(5) 0.4979(3) 0.043(2) Uani 1 1 d . . . C45 C 0.4575(3) 0.3825(5) 0.9542(3) 0.0368(18) Uani 1 1 d . . . H45A H 0.4593 0.4169 0.9828 0.055 Uiso 1 1 calc R . . H45B H 0.4740 0.4090 0.9367 0.055 Uiso 1 1 calc R . . H45C H 0.4719 0.3297 0.9677 0.055 Uiso 1 1 calc R . . C102 C 0.0873(2) 0.6124(5) 0.6274(3) 0.0302(16) Uani 1 1 d . . . C97 C 0.0599(2) 0.6140(5) 0.4926(3) 0.0342(17) Uani 1 1 d . . . H97 H 0.0766 0.6148 0.4723 0.041 Uiso 1 1 calc R . . C82 C 0.1712(2) 0.6372(5) 0.4430(3) 0.0320(16) Uani 1 1 d . . . C88 C 0.1216(4) 0.9258(6) 0.5586(5) 0.064(3) Uani 1 1 d . . . C37 C 0.3160(2) 0.3579(4) 0.8438(2) 0.0203(12) Uani 1 1 d . . . C66 C 0.3337(3) 0.4581(4) 0.4206(3) 0.0278(14) Uani 1 1 d . . . C52 C 0.4599(2) 0.4043(4) 0.6169(2) 0.0226(13) Uani 1 1 d . . . C40 C 0.1851(2) 0.3540(5) 0.7800(3) 0.0334(17) Uani 1 1 d . . . C78 C 0.3171(3) 0.5274(5) 0.3367(3) 0.0404(19) Uani 1 1 d . . . H78A H 0.3430 0.5591 0.3365 0.061 Uiso 1 1 calc R . . H78B H 0.2874 0.5521 0.3129 0.061 Uiso 1 1 calc R . . H78C H 0.3187 0.4715 0.3259 0.061 Uiso 1 1 calc R . . C79 C 0.2465(3) 0.8776(5) 0.4436(3) 0.0378(18) Uani 1 1 d . . . H79A H 0.2125 0.8725 0.4235 0.057 Uiso 1 1 calc R . . H79B H 0.2608 0.8876 0.4203 0.057 Uiso 1 1 calc R . . H79C H 0.2535 0.9231 0.4678 0.057 Uiso 1 1 calc R . . N16 N 0.2430(4) 0.2769(6) 0.4700(4) 0.073(3) Uani 1 1 d . . . C60 C 0.5172(2) 0.5100(5) 0.6271(3) 0.0268(14) Uani 1 1 d . . . H60 H 0.5486 0.5244 0.6357 0.032 Uiso 1 1 calc R . . C103 C 0.0657(3) 0.6068(6) 0.6594(3) 0.041(2) Uani 1 1 d . . . C108 C 0.0153(3) 0.6055(7) 0.6358(4) 0.055(3) Uani 1 1 d . . . H108 H -0.0002 0.6033 0.6573 0.066 Uiso 1 1 calc R . . C77 C 0.3441(3) 0.3774(5) 0.4028(3) 0.044(2) Uani 1 1 d . . . H77A H 0.3164 0.3587 0.3725 0.066 Uiso 1 1 calc R . . H77B H 0.3523 0.3372 0.4305 0.066 Uiso 1 1 calc R . . H77C H 0.3703 0.3838 0.3940 0.066 Uiso 1 1 calc R . . C46 C 0.3892(3) 0.3269(5) 0.9890(3) 0.0382(18) Uani 1 1 d . . . H46A H 0.4156 0.2889 1.0012 0.057 Uiso 1 1 calc R . . H46B H 0.3630 0.3022 0.9929 0.057 Uiso 1 1 calc R . . H46C H 0.3986 0.3772 1.0092 0.057 Uiso 1 1 calc R . . C44 C 0.2436(3) 0.3209(5) 0.8706(3) 0.0398(19) Uani 1 1 d . . . H44 H 0.2195 0.3059 0.8798 0.048 Uiso 1 1 calc R . . C30 C 0.5250(2) 0.3111(5) 0.7635(3) 0.0370(18) Uani 1 1 d . . . H30A H 0.5262 0.3142 0.7302 0.055 Uiso 1 1 calc R . . H30B H 0.5337 0.2562 0.7777 0.055 Uiso 1 1 calc R . . H30C H 0.5468 0.3507 0.7873 0.055 Uiso 1 1 calc R . . C32 C 0.2516(3) 0.0673(5) 0.7059(3) 0.0352(17) Uani 1 1 d . . . H32A H 0.2414 0.0515 0.6699 0.053 Uiso 1 1 calc R . . H32B H 0.2265 0.0978 0.7091 0.053 Uiso 1 1 calc R . . H32C H 0.2589 0.0185 0.7275 0.053 Uiso 1 1 calc R . . C85 C 0.1474(2) 0.7387(5) 0.5025(3) 0.0333(16) Uani 1 1 d . . . C75 C 0.2953(3) 0.6731(5) 0.3834(3) 0.0310(16) Uani 1 1 d . . . H75 H 0.2950 0.6779 0.3505 0.037 Uiso 1 1 calc R . . C24 C 0.3376(3) 0.0898(4) 0.7293(3) 0.0264(14) Uani 1 1 d . . . N6 N 0.3890(2) 0.8321(4) 0.8162(3) 0.0331(14) Uani 1 1 d . . . C86 C 0.1378(3) 0.7916(5) 0.5361(3) 0.0375(18) Uani 1 1 d . . . C57 C 0.4556(2) 0.7120(4) 0.6003(3) 0.0269(14) Uani 1 1 d . . . C107 C -0.0102(3) 0.6073(7) 0.5846(4) 0.053(3) Uani 1 1 d . . . H107 H -0.0433 0.6054 0.5708 0.063 Uiso 1 1 calc R . . C105 C 0.1420(3) 0.6034(5) 0.7312(3) 0.0368(18) Uani 1 1 d . . . C100 C 0.0112(2) 0.6119(6) 0.5501(3) 0.042(2) Uani 1 1 d . . . C98 C 0.0108(3) 0.6107(6) 0.4669(3) 0.042(2) Uani 1 1 d . . . C47 C 0.1442(3) 0.3369(7) 0.7918(4) 0.052(3) Uani 1 1 d . . . H47A H 0.1328 0.3881 0.7995 0.079 Uiso 1 1 calc R . . H47B H 0.1543 0.3007 0.8217 0.079 Uiso 1 1 calc R . . H47C H 0.1191 0.3108 0.7620 0.079 Uiso 1 1 calc R . . N13 N 0.1240(3) 0.2020(5) 0.4846(3) 0.054(2) Uani 1 1 d . . . C93 C 0.1872(3) 0.5769(6) 0.4142(3) 0.041(2) Uani 1 1 d . . . H93A H 0.1598 0.5512 0.3868 0.062 Uiso 1 1 calc R . . H93B H 0.2068 0.5351 0.4381 0.062 Uiso 1 1 calc R . . H93C H 0.2052 0.6055 0.3992 0.062 Uiso 1 1 calc R . . C101 C 0.0604(2) 0.6142(5) 0.5726(3) 0.0320(16) Uani 1 1 d . . . C29 C 0.4917(2) 0.4805(5) 0.7519(3) 0.0312(16) Uani 1 1 d . . . H29A H 0.5205 0.4811 0.7842 0.047 Uiso 1 1 calc R . . H29B H 0.4748 0.5318 0.7483 0.047 Uiso 1 1 calc R . . H29C H 0.4995 0.4742 0.7229 0.047 Uiso 1 1 calc R . . C90 C 0.1386(3) 0.8099(5) 0.6147(4) 0.046(2) Uani 1 1 d . . . H90 H 0.1424 0.7881 0.6467 0.055 Uiso 1 1 calc R . . C92 C 0.1180(4) 0.8981(7) 0.4718(4) 0.063(3) Uani 1 1 d . . . H92 H 0.1076 0.9519 0.4607 0.075 Uiso 1 1 calc R . . C76 C 0.2818(3) 0.7378(4) 0.4027(3) 0.0299(15) Uani 1 1 d . . . H76 H 0.2722 0.7863 0.3830 0.036 Uiso 1 1 calc R . . C83 C 0.1529(3) 0.7124(6) 0.4230(3) 0.042(2) Uani 1 1 d . . . C87 C 0.1253(4) 0.8734(6) 0.5225(5) 0.057(3) Uani 1 1 d . . . C89 C 0.1286(4) 0.8938(6) 0.6060(5) 0.058(3) Uani 1 1 d . . . C12 C 0.1567(2) 0.3976(4) 0.4818(3) 0.0238(13) Uani 1 1 d . . . C48 C 0.1299(2) 0.3969(6) 0.6890(3) 0.0384(19) Uani 1 1 d . . . H48A H 0.1137 0.3449 0.6771 0.058 Uiso 1 1 calc R . . H48B H 0.1330 0.4239 0.6604 0.058 Uiso 1 1 calc R . . H48C H 0.1120 0.4317 0.7013 0.058 Uiso 1 1 calc R . . C94 C 0.1459(3) 0.7359(7) 0.3703(3) 0.056(3) Uani 1 1 d . . . H94A H 0.1733 0.7661 0.3726 0.083 Uiso 1 1 calc R . . H94B H 0.1180 0.7704 0.3542 0.083 Uiso 1 1 calc R . . H94C H 0.1417 0.6869 0.3495 0.083 Uiso 1 1 calc R . . O9 O 0.3908(2) 0.9727(4) 0.6280(3) 0.0508(16) Uani 1 1 d . . . O6 O 0.5588(2) 0.3719(5) 1.0667(2) 0.0562(17) Uani 1 1 d . . . N12 N 0.1307(2) 0.4299(4) 0.4451(2) 0.0349(14) Uani 1 1 d . . . O4 O 0.4513(3) 0.3417(4) 0.4986(3) 0.0617(19) Uani 1 1 d . . . O5 O 0.4417(3) 0.4846(5) 1.0807(3) 0.064(2) Uani 1 1 d . . . N5 N 0.2569(2) 0.8583(4) 0.7014(4) 0.052(2) Uani 1 1 d . . . C117 C 0.3078(3) 1.0480(5) 0.5762(4) 0.0382(19) Uani 1 1 d . . . H7C H 0.3413 1.0361 0.5911 0.057 Uiso 1 1 calc R . . H7A H 0.2907 0.9985 0.5763 0.057 Uiso 1 1 calc R . . H7B H 0.3020 1.0902 0.5967 0.057 Uiso 1 1 calc R . . O7 O 0.5367(3) 0.2256(5) 1.0232(3) 0.071(2) Uani 1 1 d . . . C63 C 0.5399(3) 0.6877(5) 0.6217(3) 0.0337(17) Uani 1 1 d . . . H63A H 0.5421 0.6911 0.5890 0.051 Uiso 1 1 calc R . . H63B H 0.5637 0.6498 0.6448 0.051 Uiso 1 1 calc R . . H63C H 0.5452 0.7417 0.6377 0.051 Uiso 1 1 calc R . . N15 N 0.2629(3) 0.1674(4) 0.6003(3) 0.0468(18) Uani 1 1 d . . . O3 O 0.4094(3) 0.5498(5) 0.9912(3) 0.074(2) Uani 1 1 d . . . C64 C 0.4609(3) 0.8029(5) 0.5983(3) 0.0361(17) Uani 1 1 d . . . H64A H 0.4865 0.8214 0.6306 0.054 Uiso 1 1 calc R . . H64B H 0.4318 0.8296 0.5936 0.054 Uiso 1 1 calc R . . H64C H 0.4679 0.8167 0.5695 0.054 Uiso 1 1 calc R . . C31 C 0.3444(3) 0.0012(5) 0.7219(4) 0.0408(19) Uani 1 1 d . . . H31A H 0.3706 -0.0201 0.7529 0.061 Uiso 1 1 calc R . . H31B H 0.3513 -0.0054 0.6923 0.061 Uiso 1 1 calc R . . H31C H 0.3159 -0.0289 0.7158 0.061 Uiso 1 1 calc R . . C84 C 0.1412(3) 0.7651(6) 0.4536(3) 0.0416(19) Uani 1 1 d . . . C104 C 0.0938(3) 0.6023(6) 0.7133(3) 0.044(2) Uani 1 1 d . . . C99 C -0.0136(2) 0.6112(6) 0.4957(3) 0.044(2) Uani 1 1 d . . . C112 C 0.1750(3) 0.5945(7) 0.7874(3) 0.050(2) Uani 1 1 d . . . H11D H 0.1732 0.6430 0.8061 0.075 Uiso 1 1 calc R . . H11E H 0.2070 0.5882 0.7913 0.075 Uiso 1 1 calc R . . H11F H 0.1664 0.5464 0.8013 0.075 Uiso 1 1 calc R . . O1 O 0.1312(4) 0.4903(7) 0.8698(4) 0.103(3) Uani 1 1 d . . . C114 C 0.4591(4) 0.4250(6) 0.4920(4) 0.053(2) Uani 1 1 d . . . H4C H 0.4862 0.4446 0.5227 0.080 Uiso 1 1 calc R . . H4B H 0.4314 0.4568 0.4871 0.080 Uiso 1 1 calc R . . H4A H 0.4651 0.4310 0.4618 0.080 Uiso 1 1 calc R . . C91 C 0.1253(3) 0.8478(6) 0.4400(4) 0.053(3) Uani 1 1 d . . . H91 H 0.1199 0.8672 0.4069 0.064 Uiso 1 1 calc R . . C116 C 0.5095(4) 0.5306(6) 0.8838(4) 0.063(3) Uani 1 1 d . . . H6A H 0.4929 0.5506 0.9030 0.094 Uiso 1 1 calc R . . H6B H 0.4950 0.4800 0.8661 0.094 Uiso 1 1 calc R . . H6C H 0.5080 0.5715 0.8584 0.094 Uiso 1 1 calc R . . C111 C 0.0726(4) 0.5952(8) 0.7501(4) 0.065(3) Uani 1 1 d . . . H11M H 0.0962 0.5755 0.7834 0.097 Uiso 1 1 calc R . . H11N H 0.0464 0.5567 0.7364 0.097 Uiso 1 1 calc R . . H11O H 0.0613 0.6486 0.7546 0.097 Uiso 1 1 calc R . . C110 C -0.0668(3) 0.6102(8) 0.4701(4) 0.061(3) Uani 1 1 d . . . H11P H -0.0785 0.6613 0.4775 0.092 Uiso 1 1 calc R . . H11Q H -0.0779 0.5645 0.4836 0.092 Uiso 1 1 calc R . . H11R H -0.0783 0.6041 0.4328 0.092 Uiso 1 1 calc R . . C109 C -0.0129(3) 0.6101(7) 0.4090(3) 0.055(3) Uani 1 1 d . . . H10A H -0.0337 0.5629 0.3969 0.083 Uiso 1 1 calc R . . H10B H 0.0108 0.6070 0.3961 0.083 Uiso 1 1 calc R . . H10C H -0.0311 0.6601 0.3964 0.083 Uiso 1 1 calc R . . C119 C 0.4219(4) 0.6784(7) 0.4595(4) 0.064(3) Uani 1 1 d . . . H8C H 0.4285 0.6275 0.4791 0.097 Uiso 1 1 calc R . . H8A H 0.4106 0.6662 0.4228 0.097 Uiso 1 1 calc R . . H8B H 0.3979 0.7090 0.4648 0.097 Uiso 1 1 calc R . . O8 O 0.2929(5) 0.0748(9) 0.5268(7) 0.172(7) Uani 1 1 d . . . C120 C 0.4050(5) 0.6258(9) 0.8832(4) 0.084(4) Uani 1 1 d . . . H5C H 0.3822 0.6686 0.8791 0.127 Uiso 1 1 calc R . . H5A H 0.3895 0.5726 0.8769 0.127 Uiso 1 1 calc R . . H5B H 0.4178 0.6346 0.8584 0.127 Uiso 1 1 calc R . . C113 C 0.1648(5) 0.4476(8) 0.9127(5) 0.080(4) Uani 1 1 d . . . H1A H 0.1941 0.4438 0.9095 0.120 Uiso 1 1 calc R . . H1B H 0.1531 0.3928 0.9137 0.120 Uiso 1 1 calc R . . H1C H 0.1703 0.4767 0.9444 0.120 Uiso 1 1 calc R . . O2 O -0.0615(6) 0.6950(10) 0.6941(5) 0.154(6) Uani 1 1 d . . . C96 C 0.1260(6) 0.9445(8) 0.6471(6) 0.090(4) Uani 1 1 d . . . H96A H 0.1461 0.9924 0.6533 0.135 Uiso 1 1 calc R . . H96B H 0.1365 0.9125 0.6789 0.135 Uiso 1 1 calc R . . H96C H 0.0936 0.9620 0.6364 0.135 Uiso 1 1 calc R . . C115 C 0.3653(5) 0.5798(12) 0.9802(7) 0.114(6) Uani 1 1 d . . . H3C H 0.3598 0.5753 1.0109 0.171 Uiso 1 1 calc R . . H3A H 0.3416 0.5483 0.9521 0.171 Uiso 1 1 calc R . . H3B H 0.3634 0.6370 0.9700 0.171 Uiso 1 1 calc R . . C95 C 0.1101(6) 1.0157(7) 0.5461(7) 0.099(5) Uani 1 1 d . . . H95A H 0.0916 1.0352 0.5634 0.149 Uiso 1 1 calc R . . H95B H 0.0921 1.0225 0.5088 0.149 Uiso 1 1 calc R . . H95C H 0.1392 1.0471 0.5582 0.149 Uiso 1 1 calc R . . C118 C -0.0819(7) 0.7369(12) 0.6471(6) 0.122(7) Uani 1 1 d . . . H2A H -0.0698 0.7927 0.6521 0.184 Uiso 1 1 calc R . . H2B H -0.1159 0.7381 0.6346 0.184 Uiso 1 1 calc R . . H2C H -0.0742 0.7091 0.6219 0.184 Uiso 1 1 calc R . . O10 O -0.0719(5) 0.5392(10) 0.6652(6) 0.155(5) Uiso 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 W1 0.01330(11) 0.01446(12) 0.01924(12) -0.00274(9) 0.00618(9) -0.00223(8) W2 0.01929(12) 0.01916(13) 0.01631(12) -0.00279(9) 0.00748(9) -0.00045(9) Ni1 0.0139(3) 0.0170(4) 0.0149(4) 0.0029(3) 0.0055(3) 0.0006(3) Ni2 0.0160(3) 0.0187(4) 0.0161(4) 0.0038(3) 0.0086(3) 0.0034(3) Ni3 0.0127(3) 0.0239(4) 0.0206(4) -0.0033(3) 0.0048(3) 0.0019(3) N2 0.018(2) 0.018(2) 0.019(3) 0.003(2) 0.010(2) 0.004(2) C13 0.037(4) 0.039(4) 0.030(4) -0.010(3) 0.006(3) -0.015(3) N9 0.019(2) 0.020(3) 0.018(3) 0.004(2) 0.010(2) 0.002(2) N3 0.021(3) 0.024(3) 0.021(3) -0.003(2) 0.009(2) 0.001(2) N19 0.017(2) 0.020(3) 0.016(2) 0.005(2) 0.005(2) 0.002(2) N1 0.017(2) 0.029(3) 0.019(3) 0.000(2) 0.010(2) -0.001(2) N11 0.016(2) 0.026(3) 0.020(3) -0.003(2) 0.006(2) -0.001(2) N23 0.020(2) 0.022(3) 0.019(3) 0.002(2) 0.011(2) 0.002(2) N26 0.031(3) 0.029(3) 0.041(4) -0.002(3) 0.015(3) 0.006(3) N25 0.017(2) 0.030(3) 0.024(3) 0.005(2) 0.004(2) 0.002(2) N22 0.017(2) 0.023(3) 0.018(3) 0.001(2) 0.008(2) 0.003(2) N21 0.019(2) 0.022(3) 0.018(3) 0.004(2) 0.008(2) 0.004(2) C50 0.030(3) 0.025(3) 0.015(3) 0.004(2) 0.006(3) 0.009(3) N10 0.015(2) 0.032(3) 0.016(3) 0.006(2) 0.006(2) 0.004(2) C18 0.024(3) 0.036(4) 0.017(3) -0.005(3) 0.012(3) -0.003(3) N24 0.019(2) 0.022(3) 0.016(2) 0.004(2) 0.008(2) 0.003(2) C3 0.020(3) 0.012(3) 0.020(3) -0.002(2) 0.008(2) -0.001(2) N20 0.020(2) 0.017(2) 0.020(3) 0.002(2) 0.010(2) 0.001(2) C11 0.012(3) 0.029(3) 0.016(3) -0.003(2) 0.005(2) 0.000(2) C25 0.030(3) 0.022(3) 0.026(3) 0.004(3) 0.014(3) -0.002(3) C14 0.028(3) 0.032(4) 0.025(3) -0.004(3) 0.015(3) -0.010(3) C68 0.026(3) 0.028(3) 0.021(3) 0.002(3) 0.010(3) -0.004(3) C5 0.014(3) 0.020(3) 0.056(5) -0.012(3) 0.009(3) -0.009(3) C26 0.021(3) 0.019(3) 0.027(3) 0.006(2) 0.011(3) 0.002(2) C56 0.024(3) 0.039(4) 0.016(3) -0.005(3) 0.010(3) -0.008(3) N17 0.015(2) 0.022(3) 0.017(2) 0.002(2) 0.007(2) 0.001(2) C42 0.022(3) 0.020(3) 0.021(3) 0.002(2) 0.009(3) 0.003(2) N18 0.020(2) 0.013(2) 0.019(2) 0.0025(19) 0.007(2) -0.0005(19) C7 0.029(3) 0.028(4) 0.029(4) -0.016(3) 0.015(3) -0.011(3) C9 0.016(3) 0.028(3) 0.016(3) 0.001(2) 0.009(2) -0.001(2) C21 0.020(3) 0.025(3) 0.015(3) 0.000(2) 0.008(2) 0.003(2) C49 0.027(3) 0.023(3) 0.015(3) 0.002(2) 0.009(3) 0.004(3) C106 0.022(3) 0.042(4) 0.032(4) -0.010(3) 0.013(3) -0.003(3) N7 0.062(5) 0.048(4) 0.047(4) -0.027(3) 0.040(4) -0.023(4) C55 0.019(3) 0.039(4) 0.014(3) -0.002(3) 0.007(2) -0.005(3) C69 0.019(3) 0.024(3) 0.018(3) 0.001(2) 0.007(2) -0.002(2) N8 0.020(3) 0.027(3) 0.041(4) -0.009(3) 0.007(3) -0.002(2) C33 0.023(3) 0.021(3) 0.020(3) -0.002(2) 0.006(3) 0.003(2) C70 0.022(3) 0.018(3) 0.020(3) 0.005(2) 0.008(2) 0.001(2) N4 0.029(3) 0.025(3) 0.035(3) 0.008(3) 0.010(3) 0.002(2) C67 0.032(4) 0.031(4) 0.023(3) -0.002(3) 0.015(3) -0.004(3) C71 0.028(3) 0.020(3) 0.023(3) 0.006(3) 0.009(3) 0.000(3) C35 0.039(4) 0.026(3) 0.016(3) 0.004(3) 0.010(3) 0.006(3) C59 0.021(3) 0.043(4) 0.021(3) 0.001(3) 0.009(3) 0.012(3) C27 0.026(3) 0.032(4) 0.026(3) 0.002(3) 0.013(3) 0.012(3) C6 0.019(3) 0.024(3) 0.031(4) -0.003(3) 0.010(3) -0.003(3) C22 0.019(3) 0.023(3) 0.015(3) 0.004(2) 0.005(2) 0.004(2) C53 0.021(3) 0.024(3) 0.017(3) 0.003(2) 0.010(2) 0.008(2) C34 0.028(3) 0.026(3) 0.021(3) 0.000(3) 0.005(3) 0.010(3) C10 0.017(3) 0.025(3) 0.011(3) -0.001(2) 0.004(2) 0.002(2) C38 0.020(3) 0.022(3) 0.019(3) 0.002(2) 0.009(2) -0.001(2) C72 0.025(3) 0.020(3) 0.028(3) 0.006(3) 0.007(3) 0.002(3) C8 0.020(3) 0.021(3) 0.027(3) -0.004(3) 0.009(3) -0.002(2) C2 0.014(3) 0.023(3) 0.019(3) 0.005(2) 0.008(2) -0.001(2) C81 0.020(3) 0.031(4) 0.027(3) 0.000(3) 0.010(3) 0.000(3) C41 0.019(3) 0.039(4) 0.029(4) -0.012(3) 0.009(3) -0.008(3) C28 0.030(3) 0.024(3) 0.025(3) 0.005(3) 0.011(3) 0.011(3) C58 0.023(3) 0.025(3) 0.022(3) 0.003(2) 0.013(3) 0.000(3) N28 0.017(2) 0.028(3) 0.029(3) -0.008(2) 0.011(2) -0.003(2) C73 0.025(3) 0.023(3) 0.029(4) 0.000(3) 0.013(3) 0.005(3) C54 0.022(3) 0.030(3) 0.017(3) 0.001(2) 0.011(3) 0.003(3) C17 0.022(3) 0.024(3) 0.020(3) -0.004(2) 0.011(3) -0.004(3) C20 0.021(3) 0.027(3) 0.016(3) 0.000(2) 0.007(2) 0.004(3) C65 0.032(3) 0.021(3) 0.023(3) 0.002(2) 0.013(3) 0.001(3) C4 0.018(3) 0.020(3) 0.027(3) 0.005(3) 0.007(3) 0.002(2) C23 0.025(3) 0.022(3) 0.019(3) 0.005(2) 0.008(3) 0.007(3) N14 0.046(4) 0.040(4) 0.044(4) -0.011(3) 0.026(3) -0.014(3) N27 0.015(2) 0.039(3) 0.029(3) -0.007(3) 0.007(2) 0.003(2) C62 0.040(4) 0.033(4) 0.035(4) 0.004(3) 0.013(3) 0.020(3) C39 0.027(3) 0.032(4) 0.024(3) -0.004(3) 0.013(3) -0.012(3) C1 0.011(2) 0.025(3) 0.015(3) -0.003(2) 0.006(2) -0.002(2) C74 0.022(3) 0.030(3) 0.019(3) 0.004(3) 0.009(3) 0.006(3) C19 0.024(3) 0.038(4) 0.018(3) -0.007(3) 0.010(3) -0.001(3) C80 0.037(4) 0.027(4) 0.034(4) 0.000(3) 0.016(3) 0.012(3) C36 0.033(4) 0.024(3) 0.018(3) 0.001(3) 0.009(3) -0.001(3) C61 0.043(4) 0.020(3) 0.023(3) 0.002(3) 0.008(3) 0.004(3) C43 0.044(4) 0.044(4) 0.024(4) 0.002(3) 0.019(3) -0.009(4) C51 0.028(3) 0.031(4) 0.015(3) 0.001(3) 0.006(3) 0.010(3) C15 0.044(4) 0.029(4) 0.032(4) 0.002(3) 0.019(3) 0.004(3) C16 0.072(6) 0.030(4) 0.041(5) -0.003(3) 0.039(5) 0.014(4) C45 0.026(3) 0.053(5) 0.024(4) -0.006(3) 0.003(3) 0.007(3) C102 0.018(3) 0.039(4) 0.035(4) -0.013(3) 0.013(3) -0.001(3) C97 0.015(3) 0.053(5) 0.029(4) -0.003(3) 0.004(3) 0.003(3) C82 0.024(3) 0.047(5) 0.022(3) 0.004(3) 0.008(3) -0.003(3) C88 0.077(7) 0.040(5) 0.096(9) 0.008(5) 0.057(7) 0.015(5) C37 0.023(3) 0.021(3) 0.018(3) 0.004(2) 0.009(2) 0.000(2) C66 0.037(4) 0.023(3) 0.031(4) -0.003(3) 0.022(3) 0.000(3) C52 0.020(3) 0.032(4) 0.014(3) 0.000(2) 0.005(2) 0.007(3) C40 0.023(3) 0.048(5) 0.033(4) -0.010(3) 0.016(3) -0.012(3) C78 0.069(6) 0.037(4) 0.025(4) -0.001(3) 0.030(4) -0.001(4) C79 0.052(5) 0.025(4) 0.036(4) 0.011(3) 0.020(4) 0.012(3) N16 0.125(9) 0.055(5) 0.078(7) 0.002(5) 0.081(7) 0.024(6) C60 0.013(3) 0.042(4) 0.024(3) 0.000(3) 0.007(2) 0.000(3) C103 0.027(4) 0.059(5) 0.041(5) -0.014(4) 0.019(3) -0.005(4) C108 0.028(4) 0.092(8) 0.057(6) -0.022(5) 0.030(4) -0.003(4) C77 0.066(6) 0.036(4) 0.034(4) -0.005(3) 0.025(4) 0.009(4) C46 0.051(5) 0.043(5) 0.017(3) 0.006(3) 0.013(3) 0.008(4) C44 0.043(4) 0.052(5) 0.035(4) 0.002(4) 0.027(4) -0.012(4) C30 0.020(3) 0.049(5) 0.044(5) -0.009(4) 0.016(3) 0.002(3) C32 0.033(4) 0.023(4) 0.045(4) 0.002(3) 0.013(3) -0.004(3) C85 0.025(3) 0.037(4) 0.037(4) 0.010(3) 0.012(3) 0.010(3) C75 0.039(4) 0.035(4) 0.017(3) 0.006(3) 0.010(3) -0.001(3) C24 0.035(4) 0.019(3) 0.028(4) 0.008(3) 0.016(3) 0.005(3) N6 0.020(3) 0.033(3) 0.041(4) -0.013(3) 0.008(3) -0.008(2) C86 0.031(4) 0.036(4) 0.045(5) 0.008(4) 0.017(4) 0.008(3) C57 0.032(4) 0.031(4) 0.024(3) -0.003(3) 0.018(3) -0.007(3) C107 0.017(3) 0.086(7) 0.055(6) -0.021(5) 0.016(4) -0.005(4) C105 0.037(4) 0.048(5) 0.031(4) -0.013(3) 0.020(3) -0.010(4) C100 0.016(3) 0.062(6) 0.043(5) -0.014(4) 0.010(3) -0.001(3) C98 0.019(3) 0.060(6) 0.031(4) -0.007(4) -0.002(3) 0.001(3) C47 0.027(4) 0.094(8) 0.042(5) -0.009(5) 0.021(4) -0.017(4) N13 0.063(5) 0.041(4) 0.040(4) -0.010(3) 0.005(4) -0.020(4) C93 0.041(4) 0.061(6) 0.029(4) -0.008(4) 0.022(4) -0.015(4) C101 0.019(3) 0.038(4) 0.041(4) -0.013(3) 0.015(3) 0.002(3) C29 0.025(3) 0.034(4) 0.040(4) -0.012(3) 0.020(3) -0.011(3) C90 0.048(5) 0.036(4) 0.058(6) -0.005(4) 0.028(4) 0.005(4) C92 0.061(6) 0.050(6) 0.075(7) 0.038(5) 0.029(6) 0.025(5) C76 0.043(4) 0.022(3) 0.024(3) 0.010(3) 0.014(3) 0.003(3) C83 0.030(4) 0.060(6) 0.032(4) 0.014(4) 0.010(3) 0.004(4) C87 0.063(6) 0.039(5) 0.081(7) 0.019(5) 0.041(6) 0.026(5) C89 0.066(6) 0.037(5) 0.081(8) -0.006(5) 0.042(6) 0.009(5) C12 0.022(3) 0.026(3) 0.021(3) -0.003(3) 0.008(3) -0.004(3) C48 0.017(3) 0.057(5) 0.039(4) -0.010(4) 0.010(3) -0.002(3) C94 0.047(5) 0.079(7) 0.035(5) 0.022(5) 0.013(4) 0.006(5) O9 0.049(4) 0.044(4) 0.069(4) 0.015(3) 0.036(3) 0.000(3) O6 0.047(4) 0.073(5) 0.040(4) 0.002(3) 0.011(3) 0.013(3) N12 0.028(3) 0.039(4) 0.027(3) 0.002(3) 0.002(3) -0.005(3) O4 0.072(5) 0.060(5) 0.057(4) -0.008(3) 0.033(4) -0.029(4) O5 0.061(4) 0.082(5) 0.057(4) -0.012(4) 0.034(4) 0.007(4) N5 0.027(3) 0.025(3) 0.098(7) -0.017(4) 0.022(4) -0.002(3) C117 0.040(4) 0.020(4) 0.059(5) 0.010(4) 0.025(4) 0.011(3) O7 0.053(4) 0.071(5) 0.061(5) -0.005(4) 0.000(4) 0.021(4) C63 0.027(3) 0.047(5) 0.034(4) -0.007(3) 0.020(3) -0.011(3) N15 0.065(5) 0.028(4) 0.044(4) 0.010(3) 0.021(4) 0.014(3) O3 0.065(5) 0.084(6) 0.078(5) 0.017(5) 0.035(4) 0.024(4) C64 0.043(4) 0.034(4) 0.041(4) -0.002(3) 0.026(4) -0.008(3) C31 0.051(5) 0.022(4) 0.056(5) -0.004(3) 0.030(4) 0.004(3) C84 0.030(4) 0.049(5) 0.037(4) 0.015(4) 0.008(3) 0.008(4) C104 0.038(4) 0.067(6) 0.034(4) -0.014(4) 0.023(4) -0.008(4) C99 0.015(3) 0.062(6) 0.043(5) -0.013(4) 0.003(3) 0.001(3) C112 0.047(5) 0.076(7) 0.032(4) -0.010(4) 0.021(4) -0.017(5) O1 0.137(9) 0.099(7) 0.061(5) -0.007(5) 0.033(6) 0.037(7) C114 0.059(6) 0.059(6) 0.046(5) -0.007(5) 0.028(5) -0.012(5) C91 0.050(5) 0.057(6) 0.050(6) 0.030(5) 0.020(5) 0.027(5) C116 0.080(8) 0.046(6) 0.062(7) 0.000(5) 0.031(6) 0.012(5) C111 0.045(5) 0.110(10) 0.055(6) -0.018(6) 0.036(5) -0.013(6) C110 0.017(4) 0.097(9) 0.060(6) -0.013(6) 0.008(4) 0.005(4) C109 0.031(4) 0.088(8) 0.031(5) -0.007(5) -0.001(4) 0.001(5) C119 0.053(6) 0.077(8) 0.053(6) -0.006(5) 0.014(5) -0.031(6) O8 0.108(10) 0.133(11) 0.261(19) -0.132(13) 0.068(11) -0.018(8) C120 0.102(10) 0.084(9) 0.038(6) 0.009(6) 0.005(6) 0.011(8) C113 0.074(8) 0.068(8) 0.089(9) -0.019(7) 0.028(7) -0.002(6) O2 0.207(16) 0.166(14) 0.095(9) 0.016(9) 0.073(10) 0.049(11) C96 0.129(13) 0.048(7) 0.110(11) -0.023(7) 0.067(10) 0.002(7) C115 0.056(8) 0.166(17) 0.121(13) 0.071(12) 0.040(8) 0.029(9) C95 0.145(14) 0.042(6) 0.145(14) 0.031(8) 0.095(12) 0.042(8) C118 0.160(17) 0.145(16) 0.091(11) 0.007(11) 0.081(12) 0.059(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C1 2.140(6) . ? W1 C8 2.145(6) . ? W1 C6 2.151(7) . ? W1 C3 2.154(6) . ? W1 C4 2.160(7) . ? W1 C7 2.164(7) . ? W1 C5 2.173(7) . ? W1 C2 2.177(6) . ? W2 C13 2.146(7) . ? W2 C16 2.149(8) . ? W2 C15 2.158(8) . ? W2 C9 2.159(6) . ? W2 C14 2.161(7) . ? W2 C10 2.162(6) . ? W2 C12 2.163(7) . ? W2 C11 2.164(6) . ? Ni1 N1 2.022(6) . ? Ni1 N9 2.057(5) . ? Ni1 N17 2.086(5) . ? Ni1 N19 2.087(5) . ? Ni1 N20 2.088(5) . ? Ni1 N18 2.090(5) . ? Ni2 N2 2.047(5) . ? Ni2 N10 2.050(5) . ? Ni2 N22 2.086(5) . ? Ni2 N21 2.090(5) . ? Ni2 N24 2.092(5) . ? Ni2 N23 2.095(5) . ? Ni3 N3 2.019(5) . ? Ni3 N28 2.073(6) . ? Ni3 N11 2.080(6) . ? Ni3 N27 2.084(6) . ? Ni3 N25 2.094(6) . ? Ni3 N26 2.120(6) . ? N2 C2 1.136(8) . ? C13 N13 1.172(10) . ? N9 C9 1.144(8) . ? N3 C3 1.135(8) . ? N19 C33 1.338(8) . ? N19 C37 1.349(8) . ? N1 C1 1.152(8) . ? N11 C11 1.152(8) . ? N23 C65 1.321(8) . ? N23 C69 1.359(8) . ? N26 C90 1.308(11) . ? N26 C86 1.361(11) . ? N25 C81 1.319(9) . ? N25 C85 1.356(9) . ? N22 C58 1.318(8) . ? N22 C54 1.363(8) . ? N21 C49 1.331(8) . ? N21 C53 1.358(8) . ? C50 C51 1.390(10) . ? C50 C49 1.403(9) . ? C50 C61 1.509(10) . ? N10 C10 1.149(8) . ? C18 C19 1.386(10) . ? C18 C17 1.401(9) . ? C18 C29 1.515(10) . ? N24 C74 1.317(8) . ? N24 C70 1.367(8) . ? N20 C42 1.314(8) . ? N20 C38 1.368(8) . ? C25 C24 1.397(10) . ? C25 C26 1.414(9) . ? C25 C32 1.504(10) . ? C14 N14 1.147(9) . ? C68 C69 1.410(9) . ? C68 C67 1.416(10) . ? C68 C75 1.431(10) . ? C5 N5 1.152(10) . ? C26 N18 1.316(8) . ? C56 C57 1.379(10) . ? C56 C55 1.411(10) . ? C56 C63 1.518(9) . ? N17 C17 1.323(8) . ? N17 C21 1.357(8) . ? C42 C41 1.407(9) . ? N18 C22 1.358(8) . ? C7 N7 1.132(10) . ? C21 C20 1.408(9) . ? C21 C22 1.440(9) . ? C106 N28 1.329(9) . ? C106 C105 1.390(10) . ? C55 C54 1.405(9) . ? C55 C60 1.434(10) . ? C69 C70 1.431(9) . ? N8 C8 1.160(9) . ? C33 C34 1.395(9) . ? C70 C71 1.403(9) . ? N4 C4 1.142(9) . ? C67 C66 1.383(10) . ? C67 C78 1.500(9) . ? C71 C72 1.420(10) . ? C71 C76 1.438(9) . ? C35 C34 1.374(11) . ? C35 C36 1.422(10) . ? C35 C46 1.510(9) . ? C59 C60 1.344(11) . ? C59 C52 1.447(9) . ? C27 C28 1.348(10) . ? C27 C20 1.443(9) . ? C6 N6 1.166(9) . ? C22 C23 1.399(9) . ? C53 C52 1.402(8) . ? C53 C54 1.458(9) . ? C34 C45 1.502(10) . ? C38 C39 1.404(9) . ? C38 C37 1.434(9) . ? C72 C73 1.383(10) . ? C72 C79 1.525(9) . ? C81 C82 1.411(10) . ? C41 C40 1.377(11) . ? C41 C48 1.509(10) . ? C28 C23 1.450(9) . ? C58 C57 1.401(9) . ? N28 C102 1.364(8) . ? C73 C74 1.411(9) . ? C73 C80 1.512(9) . ? C20 C19 1.421(10) . ? C65 C66 1.412(9) . ? C23 C24 1.433(10) . ? N27 C97 1.311(9) . ? N27 C101 1.370(9) . ? C62 C51 1.505(9) . ? C39 C40 1.412(10) . ? C39 C44 1.431(10) . ? C19 C30 1.509(9) . ? C36 C37 1.421(9) . ? C36 C43 1.430(10) . ? C43 C44 1.362(12) . ? C51 C52 1.411(10) . ? C15 N15 1.158(10) . ? C16 N16 1.122(11) . ? C102 C103 1.381(11) . ? C102 C101 1.431(11) . ? C97 C98 1.406(9) . ? C82 C83 1.380(12) . ? C82 C93 1.519(11) . ? C88 C89 1.393(16) . ? C88 C87 1.398(15) . ? C88 C95 1.527(14) . ? C66 C77 1.512(10) . ? C40 C47 1.510(10) . ? C103 C104 1.417(12) . ? C103 C108 1.440(11) . ? C108 C107 1.340(13) . ? C85 C84 1.406(11) . ? C85 C86 1.436(11) . ? C75 C76 1.355(11) . ? C24 C31 1.502(10) . ? C86 C87 1.409(12) . ? C57 C64 1.508(10) . ? C107 C100 1.438(12) . ? C105 C104 1.387(11) . ? C105 C112 1.506(12) . ? C100 C101 1.410(9) . ? C100 C99 1.415(12) . ? C98 C99 1.367(12) . ? C98 C109 1.502(11) . ? C90 C89 1.413(13) . ? C92 C91 1.331(15) . ? C92 C87 1.436(15) . ? C83 C84 1.403(13) . ? C83 C94 1.491(11) . ? C89 C96 1.484(15) . ? C12 N12 1.149(9) . ? O6 C120 1.401(12) 3_667 ? O4 C114 1.419(12) . ? O5 C116 1.457(13) 3_667 ? C117 O8 1.37(2) 1_565 ? O7 C119 1.418(11) 2_646 ? O3 C115 1.386(14) . ? C84 C91 1.443(12) . ? C104 C111 1.495(11) . ? C99 C110 1.523(10) . ? O1 C113 1.415(15) . ? C116 O5 1.457(13) 3_667 ? C119 O7 1.418(11) 2_656 ? O8 C117 1.37(2) 1_545 ? C120 O6 1.401(12) 3_667 ? O2 C118 1.401(19) . ? 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 C1 W1 C8 75.7(2) . . ? C1 W1 C6 119.0(2) . . ? C8 W1 C6 71.6(2) . . ? C1 W1 C3 79.9(2) . . ? C8 W1 C3 143.5(2) . . ? C6 W1 C3 144.8(2) . . ? C1 W1 C4 142.8(2) . . ? C8 W1 C4 83.6(2) . . ? C6 W1 C4 81.7(3) . . ? C3 W1 C4 100.7(2) . . ? C1 W1 C7 70.1(2) . . ? C8 W1 C7 113.3(3) . . ? C6 W1 C7 77.6(3) . . ? C3 W1 C7 82.6(2) . . ? C4 W1 C7 147.0(3) . . ? C1 W1 C5 136.7(2) . . ? C8 W1 C5 143.0(2) . . ? C6 W1 C5 75.3(3) . . ? C3 W1 C5 71.5(2) . . ? C4 W1 C5 75.6(3) . . ? C7 W1 C5 74.5(3) . . ? C1 W1 C2 71.8(2) . . ? C8 W1 C2 74.5(2) . . ? C6 W1 C2 139.6(2) . . ? C3 W1 C2 72.3(2) . . ? C4 W1 C2 73.1(2) . . ? C7 W1 C2 137.3(2) . . ? C5 W1 C2 125.7(3) . . ? C13 W2 C16 78.1(4) . . ? C13 W2 C15 79.4(3) . . ? C16 W2 C15 73.5(3) . . ? C13 W2 C9 142.7(3) . . ? C16 W2 C9 116.2(3) . . ? C15 W2 C9 73.1(3) . . ? C13 W2 C14 72.8(3) . . ? C16 W2 C14 140.8(3) . . ? C15 W2 C14 75.8(3) . . ? C9 W2 C14 76.4(2) . . ? C13 W2 C10 144.1(3) . . ? C16 W2 C10 73.1(3) . . ? C15 W2 C10 111.5(3) . . ? C9 W2 C10 71.1(2) . . ? C14 W2 C10 142.2(2) . . ? C13 W2 C12 73.0(3) . . ? C16 W2 C12 78.1(3) . . ? C15 W2 C12 143.7(3) . . ? C9 W2 C12 141.3(2) . . ? C14 W2 C12 116.4(3) . . ? C10 W2 C12 80.4(2) . . ? C13 W2 C11 116.2(3) . . ? C16 W2 C11 140.3(3) . . ? C15 W2 C11 142.8(3) . . ? C9 W2 C11 75.9(2) . . ? C14 W2 C11 77.3(3) . . ? C10 W2 C11 76.5(2) . . ? C12 W2 C11 72.2(2) . . ? N1 Ni1 N9 92.9(2) . . ? N1 Ni1 N17 93.3(2) . . ? N9 Ni1 N17 95.2(2) . . ? N1 Ni1 N19 92.0(2) . . ? N9 Ni1 N19 169.3(2) . . ? N17 Ni1 N19 94.1(2) . . ? N1 Ni1 N20 93.3(2) . . ? N9 Ni1 N20 91.0(2) . . ? N17 Ni1 N20 170.8(2) . . ? N19 Ni1 N20 79.2(2) . . ? N1 Ni1 N18 172.1(2) . . ? N9 Ni1 N18 84.9(2) . . ? N17 Ni1 N18 79.4(2) . . ? N19 Ni1 N18 91.4(2) . . ? N20 Ni1 N18 94.3(2) . . ? N2 Ni2 N10 92.8(2) . . ? N2 Ni2 N22 87.7(2) . . ? N10 Ni2 N22 172.6(2) . . ? N2 Ni2 N21 97.7(2) . . ? N10 Ni2 N21 93.7(2) . . ? N22 Ni2 N21 78.9(2) . . ? N2 Ni2 N24 91.0(2) . . ? N10 Ni2 N24 95.4(2) . . ? N22 Ni2 N24 91.9(2) . . ? N21 Ni2 N24 167.1(2) . . ? N2 Ni2 N23 170.1(2) . . ? N10 Ni2 N23 90.0(2) . . ? N22 Ni2 N23 90.8(2) . . ? N21 Ni2 N23 91.6(2) . . ? N24 Ni2 N23 79.3(2) . . ? N3 Ni3 N28 93.7(2) . . ? N3 Ni3 N11 90.6(2) . . ? N28 Ni3 N11 93.7(2) . . ? N3 Ni3 N27 173.3(2) . . ? N28 Ni3 N27 79.8(2) . . ? N11 Ni3 N27 91.2(2) . . ? N3 Ni3 N25 95.4(2) . . ? N28 Ni3 N25 167.9(2) . . ? N11 Ni3 N25 94.1(2) . . ? N27 Ni3 N25 90.9(2) . . ? N3 Ni3 N26 90.8(2) . . ? N28 Ni3 N26 93.8(2) . . ? N11 Ni3 N26 172.3(2) . . ? N27 Ni3 N26 88.1(2) . . ? N25 Ni3 N26 78.2(2) . . ? C2 N2 Ni2 162.9(5) . . ? N13 C13 W2 179.7(9) . . ? C9 N9 Ni1 162.3(5) . . ? C3 N3 Ni3 172.8(5) . . ? C33 N19 C37 117.6(5) . . ? C33 N19 Ni1 129.7(4) . . ? C37 N19 Ni1 112.6(4) . . ? C1 N1 Ni1 168.5(5) . . ? C11 N11 Ni3 165.1(5) . . ? C65 N23 C69 117.7(6) . . ? C65 N23 Ni2 129.7(4) . . ? C69 N23 Ni2 112.5(4) . . ? C90 N26 C86 117.5(7) . . ? C90 N26 Ni3 130.1(6) . . ? C86 N26 Ni3 112.4(5) . . ? C81 N25 C85 117.4(6) . . ? C81 N25 Ni3 128.2(5) . . ? C85 N25 Ni3 113.6(5) . . ? C58 N22 C54 116.7(6) . . ? C58 N22 Ni2 129.3(4) . . ? C54 N22 Ni2 114.0(4) . . ? C49 N21 C53 117.3(5) . . ? C49 N21 Ni2 128.4(4) . . ? C53 N21 Ni2 113.8(4) . . ? C51 C50 C49 119.1(7) . . ? C51 C50 C61 122.7(6) . . ? C49 C50 C61 118.1(6) . . ? C10 N10 Ni2 165.6(5) . . ? C19 C18 C17 119.4(6) . . ? C19 C18 C29 121.8(6) . . ? C17 C18 C29 118.8(6) . . ? C74 N24 C70 118.0(5) . . ? C74 N24 Ni2 129.1(4) . . ? C70 N24 Ni2 112.4(4) . . ? N3 C3 W1 178.6(6) . . ? C42 N20 C38 117.7(5) . . ? C42 N20 Ni1 129.8(4) . . ? C38 N20 Ni1 112.2(4) . . ? N11 C11 W2 173.7(6) . . ? C24 C25 C26 118.4(6) . . ? C24 C25 C32 122.6(6) . . ? C26 C25 C32 119.0(6) . . ? N14 C14 W2 176.6(7) . . ? C69 C68 C67 119.1(6) . . ? C69 C68 C75 117.0(6) . . ? C67 C68 C75 123.8(6) . . ? N5 C5 W1 176.4(7) . . ? N18 C26 C25 124.5(6) . . ? C57 C56 C55 119.1(6) . . ? C57 C56 C63 120.1(7) . . ? C55 C56 C63 120.8(7) . . ? C17 N17 C21 118.1(5) . . ? C17 N17 Ni1 128.5(4) . . ? C21 N17 Ni1 113.4(4) . . ? N20 C42 C41 124.4(6) . . ? C26 N18 C22 117.9(5) . . ? C26 N18 Ni1 128.5(4) . . ? C22 N18 Ni1 113.2(4) . . ? N7 C7 W1 177.5(6) . . ? N9 C9 W2 177.7(6) . . ? N17 C21 C20 122.8(6) . . ? N17 C21 C22 116.7(5) . . ? C20 C21 C22 120.5(6) . . ? N21 C49 C50 123.8(6) . . ? N28 C106 C105 125.4(7) . . ? C54 C55 C56 117.5(6) . . ? C54 C55 C60 116.8(6) . . ? C56 C55 C60 125.7(6) . . ? N23 C69 C68 122.1(6) . . ? N23 C69 C70 117.2(6) . . ? C68 C69 C70 120.5(6) . . ? N19 C33 C34 124.0(6) . . ? N24 C70 C71 122.0(6) . . ? N24 C70 C69 116.9(5) . . ? C71 C70 C69 121.1(6) . . ? C66 C67 C68 117.8(6) . . ? C66 C67 C78 121.6(7) . . ? C68 C67 C78 120.6(7) . . ? C70 C71 C72 118.9(6) . . ? C70 C71 C76 117.2(6) . . ? C72 C71 C76 123.9(6) . . ? C34 C35 C36 118.8(6) . . ? C34 C35 C46 120.0(7) . . ? C36 C35 C46 121.2(7) . . ? C60 C59 C52 122.0(6) . . ? C28 C27 C20 121.9(6) . . ? N6 C6 W1 179.8(7) . . ? N18 C22 C23 122.5(6) . . ? N18 C22 C21 117.0(6) . . ? C23 C22 C21 120.4(6) . . ? N21 C53 C52 123.2(6) . . ? N21 C53 C54 116.2(5) . . ? C52 C53 C54 120.7(6) . . ? C35 C34 C33 119.0(6) . . ? C35 C34 C45 121.5(6) . . ? C33 C34 C45 119.5(7) . . ? N10 C10 W2 174.2(5) . . ? N20 C38 C39 122.2(6) . . ? N20 C38 C37 116.4(5) . . ? C39 C38 C37 121.3(6) . . ? C73 C72 C71 118.4(6) . . ? C73 C72 C79 120.1(7) . . ? C71 C72 C79 121.5(6) . . ? N8 C8 W1 177.3(6) . . ? N2 C2 W1 176.8(5) . . ? N25 C81 C82 123.9(7) . . ? C40 C41 C42 118.2(6) . . ? C40 C41 C48 123.2(7) . . ? C42 C41 C48 118.6(7) . . ? C27 C28 C23 121.4(6) . . ? N22 C58 C57 124.8(6) . . ? C106 N28 C102 115.9(6) . . ? C106 N28 Ni3 130.2(5) . . ? C102 N28 Ni3 113.9(5) . . ? C72 C73 C74 118.4(6) . . ? C72 C73 C80 123.4(6) . . ? C74 C73 C80 118.2(6) . . ? N22 C54 C55 123.4(6) . . ? N22 C54 C53 115.9(6) . . ? C55 C54 C53 120.7(6) . . ? N17 C17 C18 123.5(6) . . ? C21 C20 C19 118.0(6) . . ? C21 C20 C27 117.6(6) . . ? C19 C20 C27 124.4(6) . . ? N23 C65 C66 124.2(6) . . ? N4 C4 W1 178.4(6) . . ? C22 C23 C24 119.1(6) . . ? C22 C23 C28 117.9(6) . . ? C24 C23 C28 123.0(6) . . ? C97 N27 C101 118.8(6) . . ? C97 N27 Ni3 129.1(5) . . ? C101 N27 Ni3 111.9(5) . . ? C38 C39 C40 118.2(6) . . ? C38 C39 C44 117.2(7) . . ? C40 C39 C44 124.6(7) . . ? N1 C1 W1 175.4(5) . . ? N24 C74 C73 124.3(6) . . ? C18 C19 C20 118.1(6) . . ? C18 C19 C30 120.2(7) . . ? C20 C19 C30 121.8(7) . . ? C37 C36 C35 117.7(6) . . ? C37 C36 C43 117.2(6) . . ? C35 C36 C43 125.1(6) . . ? C44 C43 C36 121.9(7) . . ? C50 C51 C52 117.9(6) . . ? C50 C51 C62 120.1(7) . . ? C52 C51 C62 121.9(7) . . ? N15 C15 W2 178.8(7) . . ? N16 C16 W2 178.2(10) . . ? N28 C102 C103 123.6(7) . . ? N28 C102 C101 115.6(6) . . ? C103 C102 C101 120.8(6) . . ? N27 C97 C98 124.0(7) . . ? C83 C82 C81 119.0(7) . . ? C83 C82 C93 122.3(7) . . ? C81 C82 C93 118.6(7) . . ? C89 C88 C87 118.3(9) . . ? C89 C88 C95 121.0(11) . . ? C87 C88 C95 120.7(11) . . ? N19 C37 C36 122.6(6) . . ? N19 C37 C38 117.3(5) . . ? C36 C37 C38 120.1(6) . . ? C67 C66 C65 118.9(6) . . ? C67 C66 C77 123.6(7) . . ? C65 C66 C77 117.6(6) . . ? C53 C52 C51 118.6(6) . . ? C53 C52 C59 116.9(6) . . ? C51 C52 C59 124.5(6) . . ? C41 C40 C39 119.0(6) . . ? C41 C40 C47 120.7(7) . . ? C39 C40 C47 120.2(7) . . ? C59 C60 C55 122.9(6) . . ? C102 C103 C104 118.7(7) . . ? C102 C103 C108 117.7(8) . . ? C104 C103 C108 123.6(8) . . ? C107 C108 C103 122.1(8) . . ? C43 C44 C39 121.9(7) . . ? N25 C85 C84 122.6(8) . . ? N25 C85 C86 116.2(7) . . ? C84 C85 C86 121.2(7) . . ? C76 C75 C68 122.3(7) . . ? C25 C24 C23 117.3(6) . . ? C25 C24 C31 121.4(7) . . ? C23 C24 C31 121.2(6) . . ? N26 C86 C87 122.3(8) . . ? N26 C86 C85 117.3(7) . . ? C87 C86 C85 120.4(8) . . ? C56 C57 C58 118.3(6) . . ? C56 C57 C64 123.8(6) . . ? C58 C57 C64 117.9(7) . . ? C108 C107 C100 121.8(7) . . ? C104 C105 C106 118.2(7) . . ? C104 C105 C112 122.3(7) . . ? C106 C105 C112 119.4(7) . . ? C101 C100 C99 118.4(7) . . ? C101 C100 C107 116.8(8) . . ? C99 C100 C107 124.7(7) . . ? C99 C98 C97 118.4(7) . . ? C99 C98 C109 122.6(7) . . ? C97 C98 C109 119.0(8) . . ? N27 C101 C100 121.1(7) . . ? N27 C101 C102 118.0(6) . . ? C100 C101 C102 120.9(7) . . ? N26 C90 C89 124.7(9) . . ? C91 C92 C87 122.1(9) . . ? C75 C76 C71 121.6(6) . . ? C82 C83 C84 117.9(7) . . ? C82 C83 C94 120.5(9) . . ? C84 C83 C94 121.6(8) . . ? C88 C87 C86 119.0(10) . . ? C88 C87 C92 124.0(9) . . ? C86 C87 C92 117.0(9) . . ? C88 C89 C90 118.1(9) . . ? C88 C89 C96 122.4(10) . . ? C90 C89 C96 119.5(11) . . ? N12 C12 W2 178.6(7) . . ? C83 C84 C85 119.0(8) . . ? C83 C84 C91 124.7(8) . . ? C85 C84 C91 116.2(9) . . ? C105 C104 C103 118.0(7) . . ? C105 C104 C111 120.5(8) . . ? C103 C104 C111 121.4(8) . . ? C98 C99 C100 119.3(7) . . ? C98 C99 C110 120.9(8) . . ? C100 C99 C110 119.7(8) . . ? C92 C91 C84 122.9(9) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 3.439 _refine_diff_density_min -1.283 _refine_diff_density_rms 0.189 # Attachment 'comp2-Ni3Mo2.cif' data_c:\comp2.cif _database_code_depnum_ccdc_archive 'CCDC 694538' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C162.67 H159.20 Mo2.67 N44 Ni4 O10.67' _chemical_formula_weight 3391.89 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 31.229(6) _cell_length_b 16.302(3) _cell_length_c 28.862(6) _cell_angle_alpha 90.00 _cell_angle_beta 114.73(3) _cell_angle_gamma 90.00 _cell_volume 13346(5) _cell_formula_units_Z 3 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5258 _exptl_absorpt_coefficient_mu 0.662 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS v2.03 (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method 'profile data from \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 151444 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 28.61 _reflns_number_total 32249 _reflns_number_gt 20136 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2000)' _computing_cell_refinement 'SMART V5.625 (Bruker, 2000)' _computing_data_reduction 'SAINT V6.32 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _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^)+(0.1472P)^2^+44.2021P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 32249 _refine_ls_number_parameters 1496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1363 _refine_ls_R_factor_gt 0.0822 _refine_ls_wR_factor_ref 0.2895 _refine_ls_wR_factor_gt 0.2315 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 2.668 _refine_ls_shift/su_mean 0.050 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 Mo1 Mo 0.330182(15) 0.69009(3) 0.732968(19) 0.03612(13) Uani 1 1 d . . . Mo2 Mo 0.20709(2) 0.33230(4) 0.55469(2) 0.05789(18) Uani 1 1 d . . . Ni1 Ni 0.31775(2) 0.36988(4) 0.75097(3) 0.03418(16) Uani 1 1 d . . . Ni2 Ni 0.34102(2) 0.54450(5) 0.57440(3) 0.03858(18) Uani 1 1 d . . . Ni3 Ni 0.15709(3) 0.62706(6) 0.59547(3) 0.0528(2) Uani 1 1 d . . . N1 N 0.32178(16) 0.4937(3) 0.75097(17) 0.0379(10) Uani 1 1 d . . . N2 N 0.34462(17) 0.5847(3) 0.64288(19) 0.0437(11) Uani 1 1 d . . . N3 N 0.22521(16) 0.6432(3) 0.64506(18) 0.0458(11) Uani 1 1 d . . . N4 N 0.3665(2) 0.8185(3) 0.6680(3) 0.0666(17) Uani 1 1 d . . . N5 N 0.2561(3) 0.8446(4) 0.7112(5) 0.129(4) Uani 1 1 d . . . N6 N 0.3877(2) 0.8189(4) 0.8265(3) 0.0706(18) Uani 1 1 d . . . N7 N 0.2817(3) 0.6625(5) 0.8128(3) 0.085(2) Uani 1 1 d . . . N8 N 0.4391(2) 0.6248(4) 0.7908(4) 0.094(3) Uani 1 1 d . . . N9 N 0.28343(16) 0.3656(3) 0.67285(18) 0.0401(10) Uani 1 1 d . . . N10 N 0.27909(16) 0.4830(4) 0.55740(17) 0.0460(12) Uani 1 1 d . . . N11 N 0.16887(16) 0.5033(4) 0.58690(19) 0.0546(14) Uani 1 1 d . . . N12 N 0.1395(2) 0.4254(7) 0.4468(3) 0.107(3) Uani 1 1 d . . . N13 N 0.1298(4) 0.1986(9) 0.4797(5) 0.172(6) Uani 1 1 d . . . N14 N 0.1489(4) 0.2571(7) 0.6168(5) 0.139(5) Uani 1 1 d . . . N15 N 0.2553(5) 0.1536(6) 0.5997(4) 0.133(4) Uani 1 1 d . . . N16 N 0.2694(3) 0.2781(6) 0.4921(3) 0.102(3) Uani 1 1 d . . . N17 N 0.25434(16) 0.3730(3) 0.75879(18) 0.0391(10) Uani 1 1 d . . . N18 N 0.34283(17) 0.3700(3) 0.83076(17) 0.0384(10) Uani 1 1 d . . . N19 N 0.32013(16) 0.2429(3) 0.74592(17) 0.0379(10) Uani 1 1 d . . . N20 N 0.38409(16) 0.3551(3) 0.75098(17) 0.0379(10) Uani 1 1 d . . . N21 N 0.38200(16) 0.4398(3) 0.60131(18) 0.0409(10) Uani 1 1 d . . . N22 N 0.40832(18) 0.5916(3) 0.59430(19) 0.0454(11) Uani 1 1 d . . . N23 N 0.33468(17) 0.5217(3) 0.50059(19) 0.0450(11) Uani 1 1 d . . . N24 N 0.3103(2) 0.6534(4) 0.5379(2) 0.0545(14) Uani 1 1 d . . . N25 N 0.16796(19) 0.6620(5) 0.5319(2) 0.0634(17) Uani 1 1 d . . . N26 N 0.14600(19) 0.7552(4) 0.5949(2) 0.0627(16) Uani 1 1 d . . . N27 N 0.08509(18) 0.6144(5) 0.5529(2) 0.0676(18) Uani 1 1 d . . . N28 N 0.13521(18) 0.6068(4) 0.6532(2) 0.0534(13) Uani 1 1 d . . . N29 N 0.1984(13) 0.1616(10) 0.7868(10) 0.35(2) Uani 1 1 d . . . N30 N 0.1438(8) 0.4807(10) 0.8933(6) 0.211(9) Uani 1 1 d . . . N31 N 0.1912(7) 0.5508(9) 0.3064(5) 0.181(7) Uani 1 1 d . . . N32 N 0.5308(5) 0.6314(19) 0.5022(5) 0.316(17) Uani 1 1 d . . . N33 N 0.4051(7) 0.8859(17) 0.4852(7) 0.259(12) Uani 1 1 d . . . C1 C 0.32428(17) 0.5626(3) 0.74552(18) 0.0330(10) Uani 1 1 d . . . C2 C 0.34167(18) 0.6215(3) 0.6754(2) 0.0366(11) Uani 1 1 d . . . C3 C 0.26166(18) 0.6601(3) 0.6753(2) 0.0368(11) Uani 1 1 d . . . C4 C 0.3542(2) 0.7754(4) 0.6915(3) 0.0509(15) Uani 1 1 d . . . C5 C 0.2829(3) 0.7931(4) 0.7192(4) 0.080(3) Uani 1 1 d . . . C6 C 0.3678(2) 0.7759(4) 0.7929(3) 0.0509(15) Uani 1 1 d . . . C7 C 0.2992(3) 0.6728(4) 0.7853(3) 0.0601(19) Uani 1 1 d . . . C8 C 0.4019(2) 0.6494(4) 0.7713(3) 0.0610(19) Uani 1 1 d . . . C9 C 0.2576(2) 0.3531(3) 0.6317(2) 0.0415(12) Uani 1 1 d . . . C10 C 0.2527(2) 0.4323(5) 0.5542(2) 0.0483(15) Uani 1 1 d . . . C11 C 0.1801(2) 0.4420(5) 0.5768(2) 0.0515(16) Uani 1 1 d . . . C12 C 0.1636(2) 0.3915(7) 0.4841(3) 0.075(3) Uani 1 1 d . . . C13 C 0.1562(3) 0.2462(8) 0.5051(4) 0.109(4) Uani 1 1 d . . . C14 C 0.1684(3) 0.2849(6) 0.5947(4) 0.089(3) Uani 1 1 d . . . C15 C 0.2388(4) 0.2163(6) 0.5842(4) 0.088(3) Uani 1 1 d . . . C16 C 0.2464(3) 0.2950(6) 0.5125(3) 0.076(2) Uani 1 1 d . . . C17 C 0.2863(2) 0.1894(3) 0.7370(2) 0.0445(13) Uani 1 1 d . . . H17 H 0.2577 0.2082 0.7374 0.053 Uiso 1 1 calc R . . C18 C 0.2898(3) 0.1062(4) 0.7270(3) 0.0580(17) Uani 1 1 d . . . C19 C 0.3315(3) 0.0762(4) 0.7291(4) 0.073(2) Uani 1 1 d . . . C20 C 0.3695(3) 0.1329(4) 0.7390(3) 0.0539(16) Uani 1 1 d . . . C21 C 0.3616(2) 0.2156(3) 0.7456(2) 0.0411(12) Uani 1 1 d . . . C22 C 0.39599(19) 0.2763(3) 0.7494(2) 0.0393(11) Uani 1 1 d . . . C23 C 0.4400(2) 0.2529(4) 0.7508(2) 0.0468(14) Uani 1 1 d . . . C24 C 0.4725(2) 0.3162(4) 0.7536(2) 0.0501(15) Uani 1 1 d . . . C25 C 0.4585(2) 0.3957(4) 0.7522(2) 0.0484(14) Uani 1 1 d . . . C26 C 0.4144(2) 0.4128(4) 0.7514(2) 0.0437(13) Uani 1 1 d . . . H26 H 0.4056 0.4686 0.7511 0.052 Uiso 1 1 calc R . . C27 C 0.4155(3) 0.1114(4) 0.7425(3) 0.066(2) Uani 1 1 d . . . H27 H 0.4223 0.0551 0.7401 0.080 Uiso 1 1 calc R . . C28 C 0.4486(3) 0.1666(5) 0.7489(3) 0.0614(18) Uani 1 1 d . . . H28 H 0.4787 0.1488 0.7523 0.074 Uiso 1 1 calc R . . C29 C 0.2452(4) 0.0543(5) 0.7123(4) 0.087(3) Uani 1 1 d . . . H29A H 0.2310 0.0450 0.6754 0.130 Uiso 1 1 calc R . . H29B H 0.2228 0.0831 0.7221 0.130 Uiso 1 1 calc R . . H29C H 0.2534 0.0014 0.7301 0.130 Uiso 1 1 calc R . . C30 C 0.3392(5) -0.0121(5) 0.7210(6) 0.135(6) Uani 1 1 d . . . H30A H 0.3141 -0.0310 0.6889 0.202 Uiso 1 1 calc R . . H30B H 0.3386 -0.0448 0.7493 0.202 Uiso 1 1 calc R . . H30C H 0.3698 -0.0186 0.7196 0.202 Uiso 1 1 calc R . . C31 C 0.5211(2) 0.2976(6) 0.7581(3) 0.073(2) Uani 1 1 d . . . H31A H 0.5257 0.3240 0.7300 0.110 Uiso 1 1 calc R . . H31B H 0.5249 0.2382 0.7566 0.110 Uiso 1 1 calc R . . H31C H 0.5445 0.3186 0.7907 0.110 Uiso 1 1 calc R . . C32 C 0.4898(3) 0.4657(5) 0.7532(3) 0.071(2) Uani 1 1 d . . . H32A H 0.5192 0.4626 0.7842 0.106 Uiso 1 1 calc R . . H32B H 0.4738 0.5176 0.7527 0.106 Uiso 1 1 calc R . . H32C H 0.4969 0.4627 0.7232 0.106 Uiso 1 1 calc R . . C33 C 0.2109(2) 0.3800(4) 0.7228(3) 0.0461(13) Uani 1 1 d . . . H33 H 0.2071 0.3872 0.6886 0.055 Uiso 1 1 calc R . . C34 C 0.1704(2) 0.3774(4) 0.7319(3) 0.0516(15) Uani 1 1 d . . . C35 C 0.1755(2) 0.3649(5) 0.7810(3) 0.0617(18) Uani 1 1 d . . . C36 C 0.2216(2) 0.3598(5) 0.8204(3) 0.0581(17) Uani 1 1 d . . . C37 C 0.2601(2) 0.3654(3) 0.8079(2) 0.0437(13) Uani 1 1 d . . . C38 C 0.3072(2) 0.3640(3) 0.8460(2) 0.0416(12) Uani 1 1 d . . . C39 C 0.3162(3) 0.3580(5) 0.8980(3) 0.0582(17) Uani 1 1 d . . . C40 C 0.3633(3) 0.3617(6) 0.9347(3) 0.069(2) Uani 1 1 d . . . C41 C 0.3989(2) 0.3737(5) 0.9187(2) 0.0563(16) Uani 1 1 d . . . C42 C 0.3863(2) 0.3751(4) 0.8662(2) 0.0468(13) Uani 1 1 d . . . H42 H 0.4110 0.3801 0.8553 0.056 Uiso 1 1 calc R . . C43 C 0.2318(3) 0.3506(7) 0.8738(3) 0.084(3) Uani 1 1 d . . . H43 H 0.2064 0.3445 0.8834 0.101 Uiso 1 1 calc R . . C44 C 0.2753(3) 0.3507(7) 0.9094(3) 0.086(3) Uani 1 1 d . . . H44 H 0.2801 0.3456 0.9440 0.103 Uiso 1 1 calc R . . C45 C 0.1227(2) 0.3871(5) 0.6869(3) 0.068(2) Uani 1 1 d . . . H45A H 0.1079 0.3331 0.6767 0.102 Uiso 1 1 calc R . . H45B H 0.1271 0.4120 0.6582 0.102 Uiso 1 1 calc R . . H45C H 0.1025 0.4224 0.6967 0.102 Uiso 1 1 calc R . . C46 C 0.1325(3) 0.3547(7) 0.7928(4) 0.091(3) Uani 1 1 d . . . H46A H 0.1037 0.3567 0.7610 0.137 Uiso 1 1 calc R . . H46B H 0.1318 0.3991 0.8154 0.137 Uiso 1 1 calc R . . H46C H 0.1343 0.3017 0.8096 0.137 Uiso 1 1 calc R . . C47 C 0.3750(4) 0.3531(9) 0.9913(3) 0.117(4) Uani 1 1 d . . . H47A H 0.4063 0.3282 1.0088 0.175 Uiso 1 1 calc R . . H47B H 0.3514 0.3181 0.9956 0.175 Uiso 1 1 calc R . . H47C H 0.3749 0.4074 1.0058 0.175 Uiso 1 1 calc R . . C48 C 0.4496(3) 0.3843(7) 0.9555(3) 0.084(3) Uani 1 1 d . . . H48A H 0.4520 0.4273 0.9801 0.126 Uiso 1 1 calc R . . H48B H 0.4682 0.3999 0.9367 0.126 Uiso 1 1 calc R . . H48C H 0.4616 0.3325 0.9735 0.126 Uiso 1 1 calc R . . C49 C 0.3685(2) 0.3642(4) 0.6044(2) 0.0510(15) Uani 1 1 d . . . H49 H 0.3372 0.3568 0.6012 0.061 Uiso 1 1 calc R . . C50 C 0.3962(3) 0.2940(4) 0.6119(2) 0.065(2) Uani 1 1 d . . . C51 C 0.4423(3) 0.3054(5) 0.6184(2) 0.072(3) Uani 1 1 d . . . C52 C 0.4592(2) 0.3853(5) 0.6187(2) 0.060(2) Uani 1 1 d . . . C53 C 0.4277(2) 0.4513(4) 0.6089(2) 0.0442(13) Uani 1 1 d . . . C54 C 0.4421(2) 0.5338(4) 0.6065(2) 0.0473(14) Uani 1 1 d . . . C55 C 0.4889(2) 0.5530(6) 0.6167(2) 0.069(2) Uani 1 1 d . . . C56 C 0.5002(3) 0.6386(7) 0.6155(3) 0.085(3) Uani 1 1 d . . . C57 C 0.4660(4) 0.6968(6) 0.6054(3) 0.077(3) Uani 1 1 d . . . C58 C 0.4210(3) 0.6691(5) 0.5951(3) 0.0613(18) Uani 1 1 d . . . H58 H 0.3972 0.7095 0.5880 0.074 Uiso 1 1 calc R . . C59 C 0.5069(3) 0.4059(8) 0.6280(3) 0.089(3) Uani 1 1 d . . . H59 H 0.5291 0.3628 0.6341 0.107 Uiso 1 1 calc R . . C60 C 0.5214(2) 0.4848(8) 0.6286(3) 0.088(3) Uani 1 1 d . . . H60 H 0.5538 0.4953 0.6370 0.106 Uiso 1 1 calc R . . C61 C 0.3746(4) 0.2131(5) 0.6133(3) 0.097(3) Uani 1 1 d . . . H61A H 0.3630 0.1876 0.5795 0.145 Uiso 1 1 calc R . . H61B H 0.3483 0.2210 0.6229 0.145 Uiso 1 1 calc R . . H61C H 0.3983 0.1774 0.6383 0.145 Uiso 1 1 calc R . . C62 C 0.4734(4) 0.2319(7) 0.6233(4) 0.118(5) Uani 1 1 d . . . H62A H 0.4590 0.1828 0.6303 0.177 Uiso 1 1 calc R . . H62B H 0.5045 0.2409 0.6514 0.177 Uiso 1 1 calc R . . H62C H 0.4770 0.2244 0.5914 0.177 Uiso 1 1 calc R . . C63 C 0.5518(4) 0.6575(10) 0.6253(4) 0.132(6) Uani 1 1 d . . . H63A H 0.5571 0.6416 0.5954 0.198 Uiso 1 1 calc R . . H63B H 0.5732 0.6265 0.6551 0.198 Uiso 1 1 calc R . . H63C H 0.5579 0.7163 0.6316 0.198 Uiso 1 1 calc R . . C64 C 0.4748(5) 0.7870(7) 0.6044(4) 0.121(5) Uani 1 1 d . . . H64A H 0.5030 0.8021 0.6348 0.182 Uiso 1 1 calc R . . H64B H 0.4476 0.8175 0.6040 0.182 Uiso 1 1 calc R . . H64C H 0.4795 0.8003 0.5738 0.182 Uiso 1 1 calc R . . C65 C 0.3408(2) 0.4532(4) 0.4804(2) 0.0508(15) Uani 1 1 d . . . H65 H 0.3485 0.4054 0.5011 0.061 Uiso 1 1 calc R . . C66 C 0.3369(2) 0.4455(5) 0.4301(3) 0.0583(17) Uani 1 1 d . . . C67 C 0.3277(3) 0.5161(5) 0.4005(3) 0.0620(18) Uani 1 1 d . . . C68 C 0.3204(3) 0.5906(5) 0.4208(3) 0.0608(18) Uani 1 1 d . . . C69 C 0.3231(2) 0.5896(4) 0.4709(2) 0.0504(15) Uani 1 1 d . . . C70 C 0.3109(3) 0.6616(5) 0.4915(3) 0.0585(17) Uani 1 1 d . . . C71 C 0.2992(3) 0.7355(5) 0.4639(3) 0.077(2) Uani 1 1 d . . . C72 C 0.2853(4) 0.8030(6) 0.4850(4) 0.092(3) Uani 1 1 d . . . C73 C 0.2837(3) 0.7934(6) 0.5317(4) 0.084(3) Uani 1 1 d . . . C74 C 0.2960(3) 0.7163(5) 0.5557(3) 0.069(2) Uani 1 1 d . . . H74 H 0.2938 0.7095 0.5873 0.083 Uiso 1 1 calc R . . C75 C 0.3425(3) 0.3623(6) 0.4124(3) 0.074(2) Uani 1 1 d . . . H75A H 0.3184 0.3536 0.3777 0.110 Uiso 1 1 calc R . . H75B H 0.3389 0.3210 0.4352 0.110 Uiso 1 1 calc R . . H75C H 0.3739 0.3573 0.4127 0.110 Uiso 1 1 calc R . . C76 C 0.3242(4) 0.5144(7) 0.3464(3) 0.088(3) Uani 1 1 d . . . H76A H 0.3347 0.4609 0.3396 0.131 Uiso 1 1 calc R . . H76B H 0.3442 0.5576 0.3424 0.131 Uiso 1 1 calc R . . H76C H 0.2914 0.5237 0.3222 0.131 Uiso 1 1 calc R . . C77 C 0.2762(6) 0.8856(7) 0.4581(5) 0.134(5) Uani 1 1 d . . . H77A H 0.2456 0.9069 0.4545 0.201 Uiso 1 1 calc R . . H77B H 0.2759 0.8789 0.4242 0.201 Uiso 1 1 calc R . . H77C H 0.3012 0.9241 0.4781 0.201 Uiso 1 1 calc R . . C78 C 0.2691(5) 0.8613(6) 0.5585(4) 0.108(4) Uani 1 1 d . . . H78A H 0.2944 0.9019 0.5722 0.162 Uiso 1 1 calc R . . H78B H 0.2631 0.8376 0.5865 0.162 Uiso 1 1 calc R . . H78C H 0.2403 0.8879 0.5341 0.162 Uiso 1 1 calc R . . C79 C 0.1810(2) 0.6164(6) 0.5026(2) 0.067(2) Uani 1 1 d . . . H79 H 0.1903 0.5616 0.5131 0.080 Uiso 1 1 calc R . . C80 C 0.1820(3) 0.6433(7) 0.4565(3) 0.084(3) Uani 1 1 d . . . C81 C 0.1668(4) 0.7208(9) 0.4404(3) 0.105(4) Uani 1 1 d . . . C82 C 0.1551(4) 0.7728(8) 0.4720(4) 0.109(4) Uani 1 1 d . . . C83 C 0.1566(3) 0.7421(6) 0.5181(3) 0.076(2) Uani 1 1 d . . . C84 C 0.1459(3) 0.7924(6) 0.5522(3) 0.081(3) Uani 1 1 d . . . C85 C 0.1358(4) 0.8761(8) 0.5421(4) 0.113(4) Uani 1 1 d . . . C86 C 0.1275(4) 0.9238(7) 0.5784(4) 0.108(4) Uani 1 1 d . . . C87 C 0.1291(3) 0.8869(6) 0.6221(4) 0.084(3) Uani 1 1 d . . . C88 C 0.1378(3) 0.8023(5) 0.6276(3) 0.068(2) Uani 1 1 d . . . H88 H 0.1378 0.7768 0.6572 0.082 Uiso 1 1 calc R . . C89 C 0.1442(6) 0.8610(10) 0.4634(6) 0.155(7) Uani 1 1 d . . . H89 H 0.1448 0.8863 0.4341 0.186 Uiso 1 1 calc R . . C90 C 0.1333(6) 0.9069(10) 0.4958(5) 0.159(7) Uani 1 1 d . . . H90 H 0.1235 0.9621 0.4868 0.191 Uiso 1 1 calc R . . C91 C 0.1973(3) 0.5845(8) 0.4265(3) 0.093(3) Uani 1 1 d . . . H91A H 0.1694 0.5617 0.3985 0.140 Uiso 1 1 calc R . . H91B H 0.2155 0.5400 0.4488 0.140 Uiso 1 1 calc R . . H91C H 0.2168 0.6133 0.4126 0.140 Uiso 1 1 calc R . . C92 C 0.1644(5) 0.7519(10) 0.3891(4) 0.138(6) Uani 1 1 d . . . H92A H 0.1600 0.7053 0.3661 0.207 Uiso 1 1 calc R . . H92B H 0.1938 0.7803 0.3946 0.207 Uiso 1 1 calc R . . H92C H 0.1378 0.7899 0.3738 0.207 Uiso 1 1 calc R . . C93 C 0.1202(7) 1.0177(8) 0.5717(6) 0.159(7) Uani 1 1 d . . . H93A H 0.0975 1.0298 0.5368 0.239 Uiso 1 1 calc R . . H93B H 0.1504 1.0442 0.5783 0.239 Uiso 1 1 calc R . . H93C H 0.1082 1.0384 0.5958 0.239 Uiso 1 1 calc R . . C94 C 0.1210(4) 0.9317(7) 0.6631(4) 0.102(3) Uani 1 1 d . . . H94A H 0.1504 0.9584 0.6861 0.154 Uiso 1 1 calc R . . H94B H 0.1110 0.8928 0.6824 0.154 Uiso 1 1 calc R . . H94C H 0.0965 0.9733 0.6476 0.154 Uiso 1 1 calc R . . C95 C 0.0605(2) 0.6175(7) 0.5022(3) 0.084(3) Uani 1 1 d . . . H95 H 0.0775 0.6226 0.4817 0.101 Uiso 1 1 calc R . . C96 C 0.0116(3) 0.6136(7) 0.4777(3) 0.090(3) Uani 1 1 d . . . C97 C -0.0133(3) 0.6079(7) 0.5076(4) 0.093(3) Uani 1 1 d . . . C98 C 0.0108(2) 0.6059(6) 0.5607(3) 0.077(2) Uani 1 1 d . . . C99 C 0.0606(2) 0.6083(6) 0.5816(3) 0.066(2) Uani 1 1 d . . . C100 C 0.0877(2) 0.6052(5) 0.6362(3) 0.0588(17) Uani 1 1 d . . . C101 C 0.0647(3) 0.5988(6) 0.6684(3) 0.071(2) Uani 1 1 d . . . C102 C 0.0930(3) 0.5935(5) 0.7219(3) 0.072(2) Uani 1 1 d . . . C103 C 0.1415(3) 0.5930(5) 0.7390(3) 0.0600(17) Uani 1 1 d . . . C104 C 0.1605(2) 0.6008(5) 0.7029(2) 0.0554(16) Uani 1 1 d . . . H104 H 0.1939 0.6019 0.7151 0.066 Uiso 1 1 calc R . . C105 C -0.0110(3) 0.6007(7) 0.5939(5) 0.099(3) Uani 1 1 d . . . H105 H -0.0444 0.5990 0.5805 0.119 Uiso 1 1 calc R . . C106 C 0.0149(3) 0.5980(7) 0.6455(4) 0.091(3) Uani 1 1 d . . . H106 H -0.0014 0.5955 0.6670 0.110 Uiso 1 1 calc R . . C107 C -0.0117(3) 0.6173(8) 0.4200(3) 0.105(4) Uani 1 1 d . . . H10G H -0.0343 0.5722 0.4068 0.158 Uiso 1 1 calc R . . H10H H 0.0124 0.6125 0.4067 0.158 Uiso 1 1 calc R . . H10I H -0.0282 0.6698 0.4091 0.158 Uiso 1 1 calc R . . C108 C -0.0671(3) 0.6067(10) 0.4818(5) 0.143(6) Uani 1 1 d . . . H10D H -0.0792 0.6615 0.4835 0.214 Uiso 1 1 calc R . . H10E H -0.0790 0.5673 0.4992 0.214 Uiso 1 1 calc R . . H10F H -0.0776 0.5906 0.4460 0.214 Uiso 1 1 calc R . . C109 C 0.0707(4) 0.5887(8) 0.7599(4) 0.107(4) Uani 1 1 d . . . H10A H 0.0948 0.5726 0.7935 0.161 Uiso 1 1 calc R . . H10B H 0.0454 0.5478 0.7483 0.161 Uiso 1 1 calc R . . H10C H 0.0578 0.6424 0.7625 0.161 Uiso 1 1 calc R . . C110 C 0.1752(3) 0.5848(6) 0.7946(3) 0.081(3) Uani 1 1 d . . . H11A H 0.1721 0.6327 0.8135 0.122 Uiso 1 1 calc R . . H11B H 0.2076 0.5813 0.7977 0.122 Uiso 1 1 calc R . . H11C H 0.1677 0.5349 0.8088 0.122 Uiso 1 1 calc R . . C111 C 0.2017(8) 0.1451(9) 0.8262(8) 0.172(8) Uani 1 1 d . . . C112 C 0.2057(5) 0.1249(9) 0.8755(5) 0.131(5) Uani 1 1 d . . . H11G H 0.1742 0.1235 0.8753 0.197 Uiso 1 1 calc R . . H11H H 0.2250 0.1663 0.9000 0.197 Uiso 1 1 calc R . . H11I H 0.2206 0.0710 0.8854 0.197 Uiso 1 1 calc R . . C113 C 0.1726(9) 0.4548(9) 0.9327(7) 0.161(8) Uani 1 1 d . . . C114 C 0.2111(8) 0.4297(8) 0.9843(7) 0.194(10) Uani 1 1 d . . . H11M H 0.2390 0.4643 0.9922 0.291 Uiso 1 1 calc R . . H11N H 0.2196 0.3721 0.9831 0.291 Uiso 1 1 calc R . . H11O H 0.1996 0.4367 1.0108 0.291 Uiso 1 1 calc R . . C115 C 0.1901(4) 0.8050(7) 0.7751(4) 0.103(3) Uani 1 1 d . . . H11D H 0.1975 0.8056 0.7453 0.154 Uiso 1 1 calc R . . H11E H 0.1585 0.7821 0.7655 0.154 Uiso 1 1 calc R . . H11F H 0.2133 0.7713 0.8021 0.154 Uiso 1 1 calc R . . C116 C 0.1914(5) 0.6173(9) 0.2924(4) 0.111(4) Uani 1 1 d . . . C117 C 0.4408(5) 0.6170(18) 0.4677(5) 0.252(15) Uani 1 1 d . . . H11J H 0.4273 0.6654 0.4767 0.377 Uiso 1 1 calc R . . H11K H 0.4333 0.5679 0.4825 0.377 Uiso 1 1 calc R . . H11L H 0.4276 0.6115 0.4305 0.377 Uiso 1 1 calc R . . C118 C 0.5083(6) 0.3738(19) 0.5124(5) 0.258(15) Uani 1 1 d . . . C119 C 0.4055(7) 0.8896(11) 0.4430(8) 0.161(7) Uani 1 1 d . . . C120 C 0.4085(8) 0.6124(13) 0.8978(7) 0.207(10) Uani 1 1 d . . . H11P H 0.4164 0.6681 0.8913 0.311 Uiso 1 1 calc R . . H11Q H 0.3782 0.5962 0.8707 0.311 Uiso 1 1 calc R . . H11R H 0.4331 0.5743 0.8986 0.311 Uiso 1 1 calc R . . C163 C 0.3102(3) 0.6690(6) 0.3950(3) 0.079(3) Uani 1 1 d . . . H163 H 0.3091 0.6727 0.3616 0.095 Uiso 1 1 calc R . . C211 C 0.3024(3) 0.7365(5) 0.4167(3) 0.085(3) Uani 1 1 d . . . H211 H 0.2988 0.7874 0.3994 0.102 Uiso 1 1 calc R . . O5 O 0.1131(3) 0.1633(5) 0.6747(3) 0.223(6) Uiso 1 1 d R . . O2 O 0.4843(3) 0.5027(5) 0.8732(3) 0.257(8) Uiso 1 1 d R . . O4 O 0.3898(7) -0.0364(12) 0.6161(7) 0.269(8) Uiso 1 1 d . . . O1 O 0.3075(8) 0.4490(14) 1.0508(9) 0.316(10) Uiso 1 1 d . . . O3 O 0.4460(10) 0.9953(18) 0.5943(11) 0.361(13) Uiso 1 1 d . . . O6 O 0.0007(9) 0.4035(16) 0.7103(9) 0.332(11) Uiso 1 1 d . . . O8 O 0.0745(15) 0.568(3) 0.3361(16) 0.51(2) Uiso 1 1 d . . . O7 O -0.0642(9) 0.6364(16) 0.7147(10) 0.348(12) Uiso 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 Mo1 0.0283(2) 0.0275(2) 0.0559(3) -0.00619(19) 0.0210(2) -0.00556(16) Mo2 0.0437(3) 0.0808(4) 0.0458(3) -0.0244(3) 0.0155(2) -0.0217(3) Ni1 0.0355(3) 0.0296(3) 0.0394(4) 0.0041(3) 0.0175(3) 0.0031(3) Ni2 0.0364(4) 0.0454(4) 0.0412(4) 0.0106(3) 0.0234(3) 0.0097(3) Ni3 0.0276(3) 0.0934(7) 0.0348(4) 0.0010(4) 0.0104(3) 0.0076(4) N1 0.042(2) 0.033(2) 0.040(2) 0.0028(18) 0.018(2) -0.0005(18) N2 0.042(3) 0.047(3) 0.052(3) 0.010(2) 0.029(2) 0.008(2) N3 0.033(2) 0.066(3) 0.038(2) 0.007(2) 0.015(2) 0.006(2) N4 0.053(3) 0.046(3) 0.104(5) 0.021(3) 0.036(3) 0.001(2) N5 0.065(4) 0.042(4) 0.288(14) -0.018(6) 0.083(7) 0.001(3) N6 0.052(3) 0.071(4) 0.095(5) -0.036(4) 0.037(3) -0.020(3) N7 0.096(5) 0.091(5) 0.098(5) -0.054(4) 0.069(5) -0.044(4) N8 0.033(3) 0.069(4) 0.146(7) -0.051(4) 0.002(4) -0.007(3) N9 0.041(2) 0.036(2) 0.042(3) 0.0040(19) 0.016(2) -0.0031(19) N10 0.033(2) 0.072(3) 0.033(2) 0.010(2) 0.0135(19) 0.003(2) N11 0.027(2) 0.096(5) 0.037(3) -0.009(3) 0.009(2) -0.002(3) N12 0.050(4) 0.214(11) 0.045(4) -0.019(5) 0.008(3) 0.001(5) N13 0.107(8) 0.195(13) 0.167(11) -0.096(10) 0.013(7) -0.065(8) N14 0.167(10) 0.126(8) 0.186(11) -0.064(8) 0.133(9) -0.085(8) N15 0.183(12) 0.077(6) 0.124(9) -0.018(6) 0.051(8) -0.028(7) N16 0.116(7) 0.111(7) 0.095(6) -0.024(5) 0.059(5) 0.018(5) N17 0.038(2) 0.032(2) 0.047(3) 0.0063(19) 0.018(2) 0.0035(18) N18 0.047(3) 0.028(2) 0.040(2) 0.0029(18) 0.018(2) 0.0066(18) N19 0.043(2) 0.029(2) 0.041(2) 0.0067(18) 0.017(2) 0.0038(18) N20 0.036(2) 0.041(2) 0.038(2) 0.0003(19) 0.0163(19) 0.0011(18) N21 0.036(2) 0.044(3) 0.039(2) 0.001(2) 0.0125(19) 0.0084(19) N22 0.052(3) 0.049(3) 0.049(3) -0.006(2) 0.034(2) -0.008(2) N23 0.042(3) 0.057(3) 0.044(3) 0.012(2) 0.027(2) 0.007(2) N24 0.060(3) 0.060(3) 0.056(3) 0.022(3) 0.037(3) 0.023(3) N25 0.040(3) 0.110(5) 0.041(3) 0.017(3) 0.017(2) 0.023(3) N26 0.044(3) 0.097(5) 0.047(3) 0.016(3) 0.018(2) 0.023(3) N27 0.028(2) 0.119(5) 0.046(3) -0.015(3) 0.006(2) 0.008(3) N28 0.039(3) 0.079(4) 0.048(3) -0.011(3) 0.024(2) -0.006(2) N29 0.83(6) 0.115(11) 0.39(3) 0.022(14) 0.53(4) 0.04(2) N30 0.38(3) 0.170(14) 0.102(9) 0.011(9) 0.118(14) 0.035(15) N31 0.33(2) 0.128(10) 0.127(10) 0.017(8) 0.135(13) 0.012(12) N32 0.093(8) 0.78(5) 0.087(8) -0.119(16) 0.050(7) -0.126(17) N33 0.209(19) 0.41(4) 0.124(13) -0.046(17) 0.037(13) -0.10(2) C1 0.030(2) 0.039(3) 0.028(2) -0.002(2) 0.0108(19) -0.004(2) C2 0.033(2) 0.033(3) 0.050(3) 0.007(2) 0.022(2) 0.001(2) C3 0.031(3) 0.045(3) 0.038(3) 0.005(2) 0.019(2) 0.007(2) C4 0.040(3) 0.031(3) 0.080(4) 0.012(3) 0.025(3) 0.001(2) C5 0.048(4) 0.035(3) 0.160(9) -0.022(4) 0.047(5) -0.007(3) C6 0.044(3) 0.042(3) 0.076(4) -0.018(3) 0.034(3) -0.010(3) C7 0.061(4) 0.057(4) 0.082(5) -0.040(4) 0.049(4) -0.024(3) C8 0.030(3) 0.044(3) 0.098(5) -0.027(3) 0.016(3) -0.014(2) C9 0.044(3) 0.038(3) 0.045(3) -0.004(2) 0.021(3) -0.010(2) C10 0.034(3) 0.083(5) 0.026(3) 0.000(3) 0.010(2) 0.007(3) C11 0.028(3) 0.094(5) 0.028(3) -0.013(3) 0.008(2) -0.017(3) C12 0.040(3) 0.142(8) 0.042(4) -0.023(4) 0.015(3) -0.008(4) C13 0.069(6) 0.126(9) 0.111(8) -0.059(7) 0.017(5) -0.031(6) C14 0.082(6) 0.096(7) 0.110(7) -0.038(6) 0.063(6) -0.049(5) C15 0.110(7) 0.068(6) 0.081(6) -0.024(5) 0.035(5) -0.032(5) C16 0.074(5) 0.097(6) 0.056(4) -0.018(4) 0.027(4) 0.001(5) C17 0.052(3) 0.032(3) 0.053(3) 0.007(2) 0.026(3) 0.003(2) C18 0.073(4) 0.034(3) 0.075(5) 0.001(3) 0.039(4) -0.005(3) C19 0.103(6) 0.033(3) 0.107(6) 0.002(4) 0.069(5) 0.009(4) C20 0.070(4) 0.037(3) 0.066(4) 0.015(3) 0.041(4) 0.015(3) C21 0.048(3) 0.035(3) 0.043(3) 0.011(2) 0.023(3) 0.011(2) C22 0.041(3) 0.042(3) 0.035(3) 0.003(2) 0.016(2) 0.010(2) C23 0.041(3) 0.063(4) 0.034(3) 0.012(3) 0.014(2) 0.018(3) C24 0.035(3) 0.078(5) 0.038(3) 0.002(3) 0.015(2) 0.005(3) C25 0.040(3) 0.068(4) 0.038(3) -0.012(3) 0.017(2) -0.009(3) C26 0.041(3) 0.048(3) 0.047(3) -0.010(3) 0.024(3) -0.008(2) C27 0.089(5) 0.045(4) 0.083(5) 0.021(3) 0.054(5) 0.034(4) C28 0.057(4) 0.063(4) 0.071(5) 0.020(4) 0.033(4) 0.030(3) C29 0.105(7) 0.043(4) 0.132(8) -0.009(5) 0.069(6) -0.022(4) C30 0.178(12) 0.038(4) 0.264(17) -0.018(7) 0.166(13) 0.002(6) C31 0.039(3) 0.105(6) 0.078(5) 0.008(5) 0.026(3) 0.013(4) C32 0.060(4) 0.100(6) 0.070(5) -0.025(4) 0.044(4) -0.029(4) C33 0.041(3) 0.043(3) 0.055(3) 0.004(3) 0.021(3) 0.000(2) C34 0.041(3) 0.052(4) 0.059(4) -0.005(3) 0.019(3) -0.005(3) C35 0.047(4) 0.075(5) 0.071(5) -0.004(4) 0.032(3) -0.009(3) C36 0.054(4) 0.068(4) 0.060(4) -0.003(3) 0.032(3) -0.014(3) C37 0.052(3) 0.037(3) 0.049(3) 0.002(2) 0.028(3) -0.002(2) C38 0.051(3) 0.034(3) 0.044(3) 0.002(2) 0.023(3) -0.002(2) C39 0.059(4) 0.075(5) 0.047(4) 0.006(3) 0.028(3) 0.000(3) C40 0.070(5) 0.098(6) 0.038(3) 0.002(4) 0.021(3) 0.005(4) C41 0.051(4) 0.069(4) 0.044(3) -0.001(3) 0.015(3) 0.012(3) C42 0.045(3) 0.045(3) 0.048(3) 0.004(3) 0.018(3) 0.012(2) C43 0.066(5) 0.133(8) 0.063(5) 0.004(5) 0.038(4) -0.021(5) C44 0.081(6) 0.140(8) 0.051(4) 0.003(5) 0.041(4) -0.024(6) C45 0.041(3) 0.079(5) 0.078(5) 0.000(4) 0.020(3) -0.003(3) C46 0.054(4) 0.136(9) 0.096(7) -0.012(6) 0.043(5) -0.028(5) C47 0.088(7) 0.218(14) 0.044(4) 0.003(6) 0.026(4) -0.011(8) C48 0.065(5) 0.132(8) 0.045(4) -0.008(4) 0.014(4) 0.017(5) C49 0.054(4) 0.046(3) 0.041(3) 0.001(3) 0.009(3) 0.002(3) C50 0.090(6) 0.047(4) 0.034(3) 0.000(3) 0.001(3) 0.010(4) C51 0.085(6) 0.069(5) 0.034(3) -0.007(3) -0.003(3) 0.047(4) C52 0.049(3) 0.081(5) 0.034(3) -0.015(3) 0.002(3) 0.033(3) C53 0.040(3) 0.057(4) 0.035(3) -0.008(2) 0.014(2) 0.013(3) C54 0.037(3) 0.072(4) 0.040(3) -0.016(3) 0.022(2) -0.008(3) C55 0.036(3) 0.135(7) 0.040(3) -0.030(4) 0.022(3) -0.016(4) C56 0.076(5) 0.151(9) 0.042(4) -0.039(5) 0.039(4) -0.070(6) C57 0.093(6) 0.095(6) 0.054(4) -0.023(4) 0.042(4) -0.044(5) C58 0.084(5) 0.061(4) 0.054(4) -0.007(3) 0.043(4) -0.020(4) C59 0.043(4) 0.162(10) 0.048(4) -0.035(5) 0.006(3) 0.045(5) C60 0.032(3) 0.178(11) 0.050(4) -0.041(6) 0.012(3) 0.001(5) C61 0.152(9) 0.046(4) 0.055(5) 0.002(4) 0.008(5) 0.009(5) C62 0.134(9) 0.101(7) 0.078(6) -0.009(5) 0.004(6) 0.085(7) C63 0.090(7) 0.255(16) 0.073(6) -0.061(8) 0.055(5) -0.105(9) C64 0.171(11) 0.123(9) 0.074(6) -0.017(6) 0.056(7) -0.097(9) C65 0.044(3) 0.069(4) 0.046(3) 0.007(3) 0.026(3) 0.006(3) C66 0.050(4) 0.086(5) 0.050(4) -0.003(3) 0.033(3) -0.004(3) C67 0.059(4) 0.093(5) 0.048(4) 0.003(4) 0.035(3) -0.008(4) C68 0.060(4) 0.086(5) 0.049(4) 0.017(4) 0.035(3) 0.004(4) C69 0.044(3) 0.068(4) 0.048(3) 0.012(3) 0.029(3) 0.003(3) C70 0.066(4) 0.062(4) 0.057(4) 0.023(3) 0.035(3) 0.014(3) C71 0.097(6) 0.076(5) 0.068(5) 0.036(4) 0.045(5) 0.026(5) C72 0.134(9) 0.074(6) 0.078(6) 0.041(5) 0.054(6) 0.046(6) C73 0.094(6) 0.081(6) 0.083(6) 0.034(5) 0.044(5) 0.045(5) C74 0.087(5) 0.068(5) 0.064(4) 0.028(4) 0.044(4) 0.040(4) C75 0.076(5) 0.102(6) 0.057(4) -0.005(4) 0.042(4) 0.004(4) C76 0.110(7) 0.115(8) 0.059(5) 0.009(5) 0.056(5) 0.008(6) C77 0.225(16) 0.079(7) 0.110(9) 0.057(6) 0.083(10) 0.058(8) C78 0.149(10) 0.084(7) 0.098(7) 0.033(6) 0.058(7) 0.068(7) C79 0.041(3) 0.116(7) 0.040(3) 0.007(4) 0.014(3) 0.014(4) C80 0.062(5) 0.149(9) 0.044(4) 0.019(5) 0.028(4) 0.035(5) C81 0.089(6) 0.177(11) 0.056(5) 0.051(6) 0.036(5) 0.057(7) C82 0.104(7) 0.163(11) 0.073(6) 0.060(7) 0.048(5) 0.076(7) C83 0.067(5) 0.114(7) 0.051(4) 0.031(4) 0.030(4) 0.039(5) C84 0.073(5) 0.114(7) 0.060(4) 0.039(5) 0.034(4) 0.049(5) C85 0.130(9) 0.128(9) 0.101(8) 0.059(7) 0.068(7) 0.077(8) C86 0.128(9) 0.108(8) 0.111(8) 0.053(7) 0.072(7) 0.064(7) C87 0.087(6) 0.093(6) 0.078(6) 0.019(5) 0.039(5) 0.037(5) C88 0.060(4) 0.089(6) 0.060(4) 0.015(4) 0.029(4) 0.020(4) C89 0.210(16) 0.165(13) 0.135(11) 0.098(10) 0.117(12) 0.109(12) C90 0.238(17) 0.164(13) 0.127(10) 0.086(10) 0.127(12) 0.138(13) C91 0.070(5) 0.166(10) 0.052(4) 0.002(5) 0.034(4) 0.026(6) C92 0.151(11) 0.208(15) 0.083(7) 0.074(9) 0.076(7) 0.088(10) C93 0.248(19) 0.118(10) 0.159(13) 0.079(9) 0.132(14) 0.098(12) C94 0.134(9) 0.089(7) 0.098(7) 0.006(6) 0.062(7) 0.024(6) C95 0.037(4) 0.144(9) 0.062(5) -0.021(5) 0.012(3) 0.012(4) C96 0.040(4) 0.134(8) 0.074(5) -0.024(5) 0.003(4) 0.012(4) C97 0.029(3) 0.131(8) 0.100(7) -0.038(6) 0.010(4) -0.004(4) C98 0.030(3) 0.108(7) 0.088(6) -0.029(5) 0.020(3) -0.008(4) C99 0.031(3) 0.101(6) 0.063(4) -0.014(4) 0.018(3) -0.003(3) C100 0.038(3) 0.080(5) 0.064(4) -0.020(4) 0.027(3) -0.006(3) C101 0.056(4) 0.090(6) 0.084(5) -0.019(4) 0.046(4) -0.013(4) C102 0.077(5) 0.081(5) 0.081(5) -0.021(4) 0.055(5) -0.022(4) C103 0.071(4) 0.062(4) 0.061(4) -0.016(3) 0.041(4) -0.016(3) C104 0.048(3) 0.075(5) 0.045(3) -0.008(3) 0.021(3) -0.009(3) C105 0.043(4) 0.131(9) 0.135(9) -0.036(7) 0.049(5) -0.016(5) C106 0.056(5) 0.127(8) 0.112(8) -0.028(6) 0.056(5) -0.016(5) C107 0.050(5) 0.167(11) 0.065(5) -0.021(6) -0.009(4) 0.019(6) C108 0.029(4) 0.227(16) 0.144(11) -0.070(11) 0.008(5) 0.003(6) C109 0.106(8) 0.150(10) 0.103(7) -0.025(7) 0.081(7) -0.027(7) C110 0.103(7) 0.098(6) 0.051(4) -0.017(4) 0.039(4) -0.041(5) C111 0.30(2) 0.100(10) 0.227(19) -0.019(11) 0.22(2) -0.021(12) C112 0.149(12) 0.146(12) 0.122(10) -0.011(9) 0.081(10) -0.026(9) C113 0.30(3) 0.102(10) 0.132(13) 0.006(9) 0.144(16) -0.001(12) C114 0.39(3) 0.074(8) 0.178(16) 0.015(9) 0.18(2) -0.019(13) C115 0.100(8) 0.123(9) 0.091(7) -0.008(7) 0.045(6) 0.007(7) C116 0.155(11) 0.118(10) 0.082(7) 0.012(7) 0.071(8) 0.003(8) C117 0.083(8) 0.60(5) 0.098(9) -0.121(17) 0.060(8) -0.095(16) C118 0.112(11) 0.62(5) 0.060(7) -0.086(14) 0.049(8) -0.100(19) C119 0.168(16) 0.143(13) 0.134(14) -0.021(12) 0.026(13) -0.037(11) C120 0.27(3) 0.20(2) 0.149(16) 0.100(15) 0.085(17) 0.070(18) C163 0.088(6) 0.110(7) 0.049(4) 0.034(4) 0.036(4) -0.001(5) C211 0.115(7) 0.085(6) 0.068(5) 0.040(5) 0.053(5) 0.022(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C7 2.125(7) . ? Mo1 C1 2.131(5) . ? Mo1 C3 2.147(6) . ? Mo1 C8 2.146(7) . ? Mo1 C2 2.155(6) . ? Mo1 C6 2.152(6) . ? Mo1 C5 2.160(7) . ? Mo1 C4 2.161(6) . ? Mo2 C14 2.136(9) . ? Mo2 C9 2.147(6) . ? Mo2 C12 2.147(9) . ? Mo2 C16 2.147(9) . ? Mo2 C15 2.139(12) . ? Mo2 C13 2.155(9) . ? Mo2 C10 2.170(7) . ? Mo2 C11 2.183(8) . ? Ni1 N1 2.023(5) . ? Ni1 N9 2.053(5) . ? Ni1 N19 2.078(4) . ? Ni1 N20 2.085(4) . ? Ni1 N17 2.086(5) . ? Ni1 N18 2.099(5) . ? Ni2 N2 2.041(5) . ? Ni2 N10 2.047(5) . ? Ni2 N21 2.079(5) . ? Ni2 N22 2.080(5) . ? Ni2 N24 2.081(5) . ? Ni2 N23 2.089(5) . ? Ni3 N3 2.024(5) . ? Ni3 N28 2.075(5) . ? Ni3 N27 2.073(5) . ? Ni3 N25 2.081(6) . ? Ni3 N11 2.084(7) . ? Ni3 N26 2.116(7) . ? N1 C1 1.141(7) . ? N2 C2 1.148(7) . ? N3 C3 1.141(7) . ? N4 C4 1.151(8) . ? N5 C5 1.139(10) . ? N6 C6 1.145(8) . ? N7 C7 1.151(9) . ? N8 C8 1.131(9) . ? N9 C9 1.140(7) . ? N10 C10 1.143(8) . ? N11 C11 1.136(9) . ? N12 C12 1.164(12) . ? N13 C13 1.147(12) . ? N14 C14 1.143(11) . ? N15 C15 1.149(14) . ? N16 C16 1.139(11) . ? N17 C33 1.323(7) . ? N17 C37 1.356(7) . ? N18 C42 1.317(8) . ? N18 C38 1.359(7) . ? N19 C17 1.310(7) . ? N19 C21 1.373(7) . ? N20 C26 1.330(7) . ? N20 C22 1.344(7) . ? N21 C49 1.318(8) . ? N21 C53 1.362(7) . ? N22 C58 1.322(9) . ? N22 C54 1.346(8) . ? N23 C65 1.310(8) . ? N23 C69 1.355(8) . ? N24 C74 1.306(9) . ? N24 C70 1.355(8) . ? N25 C79 1.309(10) . ? N25 C83 1.368(11) . ? N26 C88 1.324(10) . ? N26 C84 1.371(9) . ? N27 C95 1.339(10) . ? N27 C99 1.345(9) . ? N28 C104 1.321(8) . ? N28 C100 1.355(8) . ? N29 C111 1.13(2) . ? N30 C113 1.19(2) . ? N31 C116 1.158(16) . ? N32 C118 1.116(18) 3_666 ? N33 C119 1.22(2) . ? C17 C18 1.401(9) . ? C18 C19 1.368(11) . ? C18 C29 1.530(11) . ? C19 C20 1.436(11) . ? C19 C30 1.494(11) . ? C20 C21 1.398(8) . ? C20 C27 1.439(10) . ? C21 C22 1.430(8) . ? C22 C23 1.410(8) . ? C23 C24 1.426(9) . ? C23 C28 1.438(10) . ? C24 C25 1.363(10) . ? C24 C31 1.499(8) . ? C25 C26 1.396(8) . ? C25 C32 1.495(9) . ? C27 C28 1.325(11) . ? C33 C34 1.398(9) . ? C34 C35 1.373(10) . ? C34 C45 1.520(10) . ? C35 C36 1.415(10) . ? C35 C46 1.526(10) . ? C36 C37 1.396(9) . ? C36 C43 1.444(11) . ? C37 C38 1.422(9) . ? C38 C39 1.410(9) . ? C39 C40 1.409(11) . ? C39 C44 1.452(10) . ? C40 C41 1.385(11) . ? C40 C47 1.523(11) . ? C41 C42 1.397(9) . ? C41 C48 1.502(10) . ? C43 C44 1.317(12) . ? C49 C50 1.397(10) . ? C50 C51 1.384(13) . ? C50 C61 1.489(12) . ? C51 C52 1.405(12) . ? C51 C62 1.510(10) . ? C52 C53 1.405(8) . ? C52 C59 1.439(12) . ? C53 C54 1.429(9) . ? C54 C55 1.402(8) . ? C55 C56 1.444(14) . ? C55 C60 1.447(14) . ? C56 C57 1.366(14) . ? C56 C63 1.547(11) . ? C57 C58 1.383(11) . ? C57 C64 1.499(14) . ? C59 C60 1.362(15) . ? C65 C66 1.411(9) . ? C66 C67 1.389(11) . ? C66 C75 1.485(11) . ? C67 C68 1.409(11) . ? C67 C76 1.520(10) . ? C68 C69 1.412(9) . ? C68 C163 1.445(11) . ? C69 C70 1.436(10) . ? C70 C71 1.406(10) . ? C71 C211 1.407(10) . ? C71 C72 1.411(13) . ? C72 C73 1.379(12) . ? C72 C77 1.521(11) . ? C73 C74 1.410(10) . ? C73 C78 1.525(13) . ? C79 C80 1.416(10) . ? C80 C81 1.362(15) . ? C80 C91 1.496(12) . ? C81 C82 1.399(15) . ? C81 C92 1.537(12) . ? C82 C83 1.406(11) . ? C82 C89 1.475(18) . ? C83 C84 1.423(12) . ? C84 C85 1.404(14) . ? C85 C86 1.413(15) . ? C85 C90 1.399(14) . ? C86 C87 1.380(13) . ? C86 C93 1.548(16) . ? C87 C88 1.402(12) . ? C87 C94 1.499(13) . ? C89 C90 1.348(18) . ? C95 C96 1.389(10) . ? C96 C97 1.385(14) . ? C96 C107 1.514(12) . ? C97 C98 1.397(13) . ? C97 C108 1.527(10) . ? C98 C99 1.415(9) . ? C98 C105 1.390(13) . ? C99 C100 1.444(10) . ? C100 C101 1.395(10) . ? C101 C106 1.415(11) . ? C101 C102 1.425(12) . ? C102 C103 1.385(11) . ? C102 C109 1.526(11) . ? C103 C104 1.403(9) . ? C103 C110 1.513(11) . ? C105 C106 1.367(14) . ? C111 C112 1.41(2) . ? C113 C114 1.53(3) . ? C115 C116 1.356(17) 4_576 ? C116 C115 1.356(17) 4_575 ? C117 C118 1.45(2) 3_666 ? C118 N32 1.116(18) 3_666 ? C118 C117 1.45(2) 3_666 ? C119 C120 1.35(3) 4_575 ? C120 C119 1.35(3) 4_576 ? C163 C211 1.340(12) . ? O4 O3 2.16(3) 1_545 ? O3 O4 2.16(3) 1_565 ? O6 O8 2.21(4) 3_566 ? O8 O6 2.21(4) 3_566 ? 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 C7 Mo1 C1 69.7(2) . . ? C7 Mo1 C3 85.3(2) . . ? C1 Mo1 C3 77.3(2) . . ? C7 Mo1 C8 106.2(3) . . ? C1 Mo1 C8 75.9(2) . . ? C3 Mo1 C8 144.7(2) . . ? C7 Mo1 C2 138.7(2) . . ? C1 Mo1 C2 71.28(19) . . ? C3 Mo1 C2 73.6(2) . . ? C8 Mo1 C2 76.3(2) . . ? C7 Mo1 C6 76.8(2) . . ? C1 Mo1 C6 123.6(2) . . ? C3 Mo1 C6 143.4(2) . . ? C8 Mo1 C6 71.7(2) . . ? C2 Mo1 C6 138.3(2) . . ? C7 Mo1 C5 75.8(4) . . ? C1 Mo1 C5 133.5(2) . . ? C3 Mo1 C5 69.6(3) . . ? C8 Mo1 C5 145.1(3) . . ? C2 Mo1 C5 125.7(3) . . ? C6 Mo1 C5 75.2(3) . . ? C7 Mo1 C4 147.6(3) . . ? C1 Mo1 C4 142.7(2) . . ? C3 Mo1 C4 100.5(2) . . ? C8 Mo1 C4 87.5(3) . . ? C2 Mo1 C4 72.5(2) . . ? C6 Mo1 C4 80.1(3) . . ? C5 Mo1 C4 76.5(3) . . ? C14 Mo2 C9 80.5(3) . . ? C14 Mo2 C12 113.5(4) . . ? C9 Mo2 C12 144.1(3) . . ? C14 Mo2 C16 142.3(4) . . ? C9 Mo2 C16 106.6(3) . . ? C12 Mo2 C16 82.7(3) . . ? C14 Mo2 C15 74.8(4) . . ? C9 Mo2 C15 73.1(3) . . ? C12 Mo2 C15 141.2(3) . . ? C16 Mo2 C15 72.3(4) . . ? C14 Mo2 C13 72.3(4) . . ? C9 Mo2 C13 144.0(4) . . ? C12 Mo2 C13 70.4(5) . . ? C16 Mo2 C13 82.9(4) . . ? C15 Mo2 C13 77.2(4) . . ? C14 Mo2 C10 142.9(3) . . ? C9 Mo2 C10 71.8(2) . . ? C12 Mo2 C10 79.2(3) . . ? C16 Mo2 C10 71.1(3) . . ? C15 Mo2 C10 118.1(3) . . ? C13 Mo2 C10 142.1(4) . . ? C14 Mo2 C11 76.3(3) . . ? C9 Mo2 C11 77.0(2) . . ? C12 Mo2 C11 75.0(3) . . ? C16 Mo2 C11 141.3(3) . . ? C15 Mo2 C11 141.2(3) . . ? C13 Mo2 C11 117.4(3) . . ? C10 Mo2 C11 73.8(2) . . ? N1 Ni1 N9 92.19(18) . . ? N1 Ni1 N19 171.85(18) . . ? N9 Ni1 N19 84.62(18) . . ? N1 Ni1 N20 93.06(18) . . ? N9 Ni1 N20 93.34(19) . . ? N19 Ni1 N20 79.67(18) . . ? N1 Ni1 N17 92.14(18) . . ? N9 Ni1 N17 92.10(19) . . ? N19 Ni1 N17 95.47(18) . . ? N20 Ni1 N17 172.32(18) . . ? N1 Ni1 N18 90.25(17) . . ? N9 Ni1 N18 171.27(19) . . ? N19 Ni1 N18 94.02(17) . . ? N20 Ni1 N18 94.90(18) . . ? N17 Ni1 N18 79.43(19) . . ? N2 Ni2 N10 93.06(19) . . ? N2 Ni2 N21 97.25(19) . . ? N10 Ni2 N21 93.4(2) . . ? N2 Ni2 N22 88.51(19) . . ? N10 Ni2 N22 172.3(2) . . ? N21 Ni2 N22 78.9(2) . . ? N2 Ni2 N24 92.5(2) . . ? N10 Ni2 N24 96.2(2) . . ? N21 Ni2 N24 166.0(2) . . ? N22 Ni2 N24 91.3(2) . . ? N2 Ni2 N23 171.3(2) . . ? N10 Ni2 N23 89.51(19) . . ? N21 Ni2 N23 90.89(19) . . ? N22 Ni2 N23 90.06(19) . . ? N24 Ni2 N23 79.0(2) . . ? N3 Ni3 N28 93.1(2) . . ? N3 Ni3 N27 172.2(2) . . ? N28 Ni3 N27 79.6(2) . . ? N3 Ni3 N25 94.4(2) . . ? N28 Ni3 N25 169.1(2) . . ? N27 Ni3 N25 92.4(2) . . ? N3 Ni3 N11 91.4(2) . . ? N28 Ni3 N11 94.3(2) . . ? N27 Ni3 N11 92.0(2) . . ? N25 Ni3 N11 93.3(2) . . ? N3 Ni3 N26 89.8(2) . . ? N28 Ni3 N26 93.2(2) . . ? N27 Ni3 N26 87.7(3) . . ? N25 Ni3 N26 79.0(3) . . ? N11 Ni3 N26 172.3(2) . . ? C1 N1 Ni1 171.9(4) . . ? C2 N2 Ni2 165.4(5) . . ? C3 N3 Ni3 171.7(5) . . ? C9 N9 Ni1 165.2(4) . . ? C10 N10 Ni2 161.7(5) . . ? C11 N11 Ni3 166.0(5) . . ? C33 N17 C37 118.2(5) . . ? C33 N17 Ni1 128.7(4) . . ? C37 N17 Ni1 113.2(4) . . ? C42 N18 C38 118.1(5) . . ? C42 N18 Ni1 130.0(4) . . ? C38 N18 Ni1 112.0(4) . . ? C17 N19 C21 117.9(5) . . ? C17 N19 Ni1 128.9(4) . . ? C21 N19 Ni1 112.6(4) . . ? C26 N20 C22 118.1(5) . . ? C26 N20 Ni1 128.4(4) . . ? C22 N20 Ni1 113.5(4) . . ? C49 N21 C53 117.5(5) . . ? C49 N21 Ni2 128.9(4) . . ? C53 N21 Ni2 112.7(4) . . ? C58 N22 C54 117.9(6) . . ? C58 N22 Ni2 128.2(5) . . ? C54 N22 Ni2 113.8(4) . . ? C65 N23 C69 117.7(5) . . ? C65 N23 Ni2 129.6(4) . . ? C69 N23 Ni2 112.7(4) . . ? C74 N24 C70 117.3(6) . . ? C74 N24 Ni2 129.2(5) . . ? C70 N24 Ni2 113.0(4) . . ? C79 N25 C83 117.9(6) . . ? C79 N25 Ni3 128.5(6) . . ? C83 N25 Ni3 113.4(5) . . ? C88 N26 C84 117.1(7) . . ? C88 N26 Ni3 130.3(5) . . ? C84 N26 Ni3 112.5(6) . . ? C95 N27 C99 117.4(6) . . ? C95 N27 Ni3 128.9(5) . . ? C99 N27 Ni3 113.5(4) . . ? C104 N28 C100 117.3(6) . . ? C104 N28 Ni3 129.5(4) . . ? C100 N28 Ni3 113.0(5) . . ? N1 C1 Mo1 177.5(5) . . ? N2 C2 Mo1 175.5(5) . . ? N3 C3 Mo1 179.0(5) . . ? N4 C4 Mo1 177.3(6) . . ? N5 C5 Mo1 176.5(6) . . ? N6 C6 Mo1 176.8(7) . . ? N7 C7 Mo1 178.5(6) . . ? N8 C8 Mo1 177.2(6) . . ? N9 C9 Mo2 177.8(5) . . ? N10 C10 Mo2 175.0(5) . . ? N11 C11 Mo2 173.4(6) . . ? N12 C12 Mo2 177.6(8) . . ? N13 C13 Mo2 178.0(15) . . ? N14 C14 Mo2 177.3(12) . . ? N15 C15 Mo2 179.1(12) . . ? N16 C16 Mo2 175.8(9) . . ? N19 C17 C18 124.0(6) . . ? C19 C18 C17 119.5(6) . . ? C19 C18 C29 123.6(7) . . ? C17 C18 C29 116.9(7) . . ? C18 C19 C20 118.1(6) . . ? C18 C19 C30 123.3(8) . . ? C20 C19 C30 118.6(8) . . ? C21 C20 C19 118.0(6) . . ? C21 C20 C27 117.0(6) . . ? C19 C20 C27 125.0(6) . . ? N19 C21 C20 122.4(6) . . ? N19 C21 C22 117.1(5) . . ? C20 C21 C22 120.4(5) . . ? N20 C22 C23 122.5(6) . . ? N20 C22 C21 117.0(5) . . ? C23 C22 C21 120.5(5) . . ? C22 C23 C24 118.0(6) . . ? C22 C23 C28 117.3(6) . . ? C24 C23 C28 124.7(6) . . ? C25 C24 C23 118.3(5) . . ? C25 C24 C31 119.7(7) . . ? C23 C24 C31 122.0(7) . . ? C24 C25 C26 119.5(6) . . ? C24 C25 C32 121.8(6) . . ? C26 C25 C32 118.7(6) . . ? N20 C26 C25 123.5(6) . . ? C28 C27 C20 122.7(6) . . ? C27 C28 C23 121.5(6) . . ? N17 C33 C34 124.1(6) . . ? C35 C34 C33 118.4(6) . . ? C35 C34 C45 123.2(6) . . ? C33 C34 C45 118.4(6) . . ? C34 C35 C36 118.4(6) . . ? C34 C35 C46 120.9(7) . . ? C36 C35 C46 120.6(7) . . ? C37 C36 C35 119.1(6) . . ? C37 C36 C43 116.9(7) . . ? C35 C36 C43 124.0(7) . . ? N17 C37 C36 121.6(6) . . ? N17 C37 C38 116.8(5) . . ? C36 C37 C38 121.6(6) . . ? N18 C38 C39 121.6(6) . . ? N18 C38 C37 118.1(5) . . ? C39 C38 C37 120.3(6) . . ? C40 C39 C38 118.6(6) . . ? C40 C39 C44 124.9(7) . . ? C38 C39 C44 116.5(7) . . ? C41 C40 C39 119.0(6) . . ? C41 C40 C47 120.3(7) . . ? C39 C40 C47 120.7(7) . . ? C40 C41 C42 117.6(6) . . ? C40 C41 C48 122.4(6) . . ? C42 C41 C48 119.9(7) . . ? N18 C42 C41 124.9(6) . . ? C44 C43 C36 122.0(7) . . ? C43 C44 C39 122.7(7) . . ? N21 C49 C50 125.5(7) . . ? C51 C50 C49 117.0(7) . . ? C51 C50 C61 124.9(8) . . ? C49 C50 C61 118.1(8) . . ? C50 C51 C52 119.5(6) . . ? C50 C51 C62 119.9(9) . . ? C52 C51 C62 120.6(9) . . ? C53 C52 C51 118.6(7) . . ? C53 C52 C59 116.4(8) . . ? C51 C52 C59 125.0(7) . . ? N21 C53 C52 121.7(6) . . ? N21 C53 C54 116.9(5) . . ? C52 C53 C54 121.4(6) . . ? N22 C54 C55 122.2(7) . . ? N22 C54 C53 116.3(5) . . ? C55 C54 C53 121.5(7) . . ? C54 C55 C56 117.0(8) . . ? C54 C55 C60 116.4(8) . . ? C56 C55 C60 126.5(8) . . ? C57 C56 C55 119.9(7) . . ? C57 C56 C63 124.3(10) . . ? C55 C56 C63 115.7(11) . . ? C58 C57 C56 116.9(8) . . ? C58 C57 C64 119.6(11) . . ? C56 C57 C64 123.5(9) . . ? N22 C58 C57 125.9(8) . . ? C60 C59 C52 122.4(7) . . ? C59 C60 C55 121.8(7) . . ? N23 C65 C66 124.6(6) . . ? C67 C66 C65 117.7(7) . . ? C67 C66 C75 124.7(6) . . ? C65 C66 C75 117.6(7) . . ? C66 C67 C68 119.2(6) . . ? C66 C67 C76 121.6(8) . . ? C68 C67 C76 119.2(7) . . ? C69 C68 C67 117.7(7) . . ? C69 C68 C163 116.4(7) . . ? C67 C68 C163 126.0(7) . . ? N23 C69 C68 122.9(6) . . ? N23 C69 C70 116.9(5) . . ? C68 C69 C70 120.1(6) . . ? N24 C70 C71 122.5(7) . . ? N24 C70 C69 116.4(6) . . ? C71 C70 C69 121.1(6) . . ? C211 C71 C70 116.8(8) . . ? C211 C71 C72 124.6(7) . . ? C70 C71 C72 118.6(7) . . ? C73 C72 C71 118.5(7) . . ? C73 C72 C77 121.6(9) . . ? C71 C72 C77 119.7(8) . . ? C72 C73 C74 117.8(8) . . ? C72 C73 C78 123.8(8) . . ? C74 C73 C78 118.4(8) . . ? N24 C74 C73 125.2(7) . . ? N25 C79 C80 124.5(9) . . ? C81 C80 C79 117.7(8) . . ? C81 C80 C91 123.2(8) . . ? C79 C80 C91 119.0(9) . . ? C80 C81 C82 119.3(8) . . ? C80 C81 C92 120.2(10) . . ? C82 C81 C92 120.5(11) . . ? C81 C82 C83 119.2(10) . . ? C81 C82 C89 125.9(9) . . ? C83 C82 C89 114.7(10) . . ? N25 C83 C82 121.0(8) . . ? N25 C83 C84 117.3(7) . . ? C82 C83 C84 121.8(9) . . ? N26 C84 C85 122.3(8) . . ? N26 C84 C83 116.9(8) . . ? C85 C84 C83 120.9(8) . . ? C86 C85 C90 123.9(11) . . ? C86 C85 C84 118.3(9) . . ? C90 C85 C84 117.8(11) . . ? C87 C86 C85 119.4(10) . . ? C87 C86 C93 119.5(11) . . ? C85 C86 C93 121.0(10) . . ? C86 C87 C88 117.6(9) . . ? C86 C87 C94 123.8(9) . . ? C88 C87 C94 118.6(8) . . ? N26 C88 C87 125.1(8) . . ? C90 C89 C82 122.2(10) . . ? C89 C90 C85 122.3(12) . . ? N27 C95 C96 124.1(8) . . ? C97 C96 C95 118.0(8) . . ? C97 C96 C107 123.4(8) . . ? C95 C96 C107 118.6(9) . . ? C96 C97 C98 120.0(7) . . ? C96 C97 C108 119.2(10) . . ? C98 C97 C108 120.8(9) . . ? C97 C98 C99 117.2(8) . . ? C97 C98 C105 124.4(7) . . ? C99 C98 C105 118.4(8) . . ? N27 C99 C98 123.1(7) . . ? N27 C99 C100 116.7(5) . . ? C98 C99 C100 120.1(7) . . ? N28 C100 C101 123.3(7) . . ? N28 C100 C99 116.6(6) . . ? C101 C100 C99 120.1(6) . . ? C100 C101 C106 117.5(8) . . ? C100 C101 C102 118.0(7) . . ? C106 C101 C102 124.5(7) . . ? C103 C102 C101 118.4(6) . . ? C103 C102 C109 120.2(8) . . ? C101 C102 C109 121.4(8) . . ? C102 C103 C104 118.3(7) . . ? C102 C103 C110 123.4(7) . . ? C104 C103 C110 118.3(7) . . ? N28 C104 C103 124.6(6) . . ? C106 C105 C98 121.2(7) . . ? C105 C106 C101 122.7(8) . . ? N29 C111 C112 180(2) . . ? N30 C113 C114 174.7(19) . . ? N31 C116 C115 178(2) . 4_575 ? N32 C118 C117 178(3) 3_666 3_666 ? N33 C119 C120 175(3) . 4_575 ? C211 C163 C68 121.9(7) . . ? C163 C211 C71 123.0(7) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 28.61 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 3.141 _refine_diff_density_min -2.182 _refine_diff_density_rms 0.143 # Attachment 'comp3-Ni9W6.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 694539' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H58 N22 Ni3 O6 W2' _chemical_formula_weight 1679.07 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 32.270(5) _cell_length_b 32.270(5) _cell_length_c 21.161(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 19084(5) _cell_formula_units_Z 9 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block' _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7452 _exptl_absorpt_coefficient_mu 3.406 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5731 _exptl_absorpt_correction_T_max 0.6802 _exptl_absorpt_process_details 'SADABS v2.03 (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method 'profile data from \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48537 _diffrn_reflns_av_R_equivalents 0.1186 _diffrn_reflns_av_sigmaI/netI 0.1256 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 27.61 _reflns_number_total 9650 _reflns_number_gt 4057 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2000)' _computing_cell_refinement 'SMART V5.625 (Bruker, 2000)' _computing_data_reduction 'SAINT V6.32 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _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^)+(0.1913P)^2^+118.1420P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9650 _refine_ls_number_parameters 404 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.2077 _refine_ls_R_factor_gt 0.0915 _refine_ls_wR_factor_ref 0.3493 _refine_ls_wR_factor_gt 0.2516 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 4.743 _refine_ls_shift/su_mean 0.068 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 W1 W 0.18716(2) 0.64496(2) 0.30767(4) 0.0716(3) Uani 1 1 d . . . Ni1 Ni 0.3333 0.6667 0.1667 0.0418(9) Uani 1 6 d S . . N1 N 0.3390(3) 0.6180(4) 0.2208(5) 0.044(2) Uani 1 1 d . . . C1 C 0.2466(5) 0.6560(4) 0.2500(6) 0.048(3) Uani 1 1 d . . . Ni2 Ni 0.30464(7) 0.83142(7) 0.26853(11) 0.0679(6) Uani 1 1 d . . . O2 O 0.3058(4) 0.8492(4) 0.3650(6) 0.071(3) Uani 1 1 d . . . N2 N 0.2590(5) 0.7616(4) 0.2909(7) 0.067(3) Uani 1 1 d . . . C2 C 0.2327(6) 0.7203(6) 0.2997(9) 0.069(4) Uani 1 1 d . . . Ni3 Ni 0.3333 0.6667 0.4514(2) 0.132(2) Uani 1 3 d S . . N3 N 0.2746(7) 0.6560(7) 0.3991(8) 0.099(5) Uani 1 1 d . . . C3 C 0.2425(8) 0.6516(7) 0.3669(9) 0.087(6) Uani 1 1 d . . . N4 N 0.3631(5) 0.8235(5) 0.2838(7) 0.076(4) Uani 1 1 d . . . C4 C 0.1646(5) 0.6377(5) 0.2132(10) 0.064(4) Uani 1 1 d . . . N5 N 0.3039(5) 0.8157(4) 0.1743(9) 0.076(4) Uani 1 1 d . . . C5 C 0.1805(6) 0.5768(6) 0.2938(9) 0.076(5) Uani 1 1 d . . . O6 O 0.3264(12) 0.7159(10) 0.5124(10) 0.247(15) Uani 1 1 d . . . N6 N 0.1197(6) 0.6961(7) 0.3016(9) 0.110(6) Uani 1 1 d . . . C6 C 0.1431(7) 0.6777(7) 0.3030(9) 0.083(5) Uani 1 1 d . . . O7 O 0.3439(10) 0.9375(8) 0.4029(12) 0.226(14) Uani 1 1 d D . . N7 N 0.1663(12) 0.6564(12) 0.4578(12) 0.204(16) Uani 1 1 d . . . C7 C 0.1754(10) 0.6544(10) 0.4070(11) 0.130(11) Uani 1 1 d . . . N8 N 0.0722(9) 0.5613(8) 0.325(2) 0.26(2) Uani 1 1 d . . . C8 C 0.1124(12) 0.5891(10) 0.3153(18) 0.171(15) Uani 1 1 d . . . N9 N 0.3446(5) 0.9038(4) 0.2520(7) 0.068(3) Uani 1 1 d . . . C9 C 0.3905(7) 0.9324(8) 0.2542(10) 0.095(6) Uani 1 1 d . . . H9 H 0.4099 0.9181 0.2590 0.114 Uiso 1 1 calc R . . N10 N 0.2509(4) 0.8465(4) 0.2547(6) 0.060(3) Uani 1 1 d . . . C10 C 0.4139(7) 0.9818(7) 0.2501(10) 0.090(6) Uani 1 1 d . . . N11 N 0.3650(14) 1.0252(13) 0.402(3) 0.34(3) Uiso 1 1 d D . . C11 C 0.3885(7) 1.0051(6) 0.2381(9) 0.086(5) Uani 1 1 d . . . C12 C 0.3360(7) 0.9739(6) 0.2350(9) 0.081(5) Uani 1 1 d . . . C13 C 0.3181(6) 0.9254(6) 0.2450(7) 0.066(4) Uani 1 1 d . . . C14 C 0.2667(6) 0.8940(6) 0.2449(8) 0.072(4) Uani 1 1 d . . . C15 C 0.2361(7) 0.9124(6) 0.2369(9) 0.076(5) Uani 1 1 d . . . C16 C 0.1858(6) 0.8795(6) 0.2390(8) 0.067(4) Uani 1 1 d . . . C17 C 0.1699(6) 0.8318(6) 0.2480(8) 0.069(4) Uani 1 1 d . . . C18 C 0.2052(6) 0.8178(6) 0.2561(8) 0.069(4) Uani 1 1 d . . . H18 H 0.1942 0.7848 0.2631 0.082 Uiso 1 1 calc R . . C19 C 0.3039(8) 0.9906(6) 0.2281(10) 0.095(6) Uani 1 1 d . . . H19 H 0.3165 1.0241 0.2240 0.113 Uiso 1 1 calc R . . C20 C 0.2582(7) 0.9632(6) 0.2269(9) 0.082(5) Uani 1 1 d . . . H20 H 0.2385 0.9768 0.2193 0.099 Uiso 1 1 calc R . . C21 C 0.4697(7) 1.0123(9) 0.2574(14) 0.132(9) Uani 1 1 d . . . H21A H 0.4820 1.0415 0.2319 0.198 Uiso 1 1 calc R . . H21B H 0.4842 0.9936 0.2431 0.198 Uiso 1 1 calc R . . H21C H 0.4779 1.0211 0.3019 0.198 Uiso 1 1 calc R . . C22 C 0.4098(7) 1.0572(6) 0.2295(10) 0.094(6) Uani 1 1 d . . . H22A H 0.4448 1.0723 0.2285 0.142 Uiso 1 1 calc R . . H22B H 0.4003 1.0704 0.2647 0.142 Uiso 1 1 calc R . . H22C H 0.3985 1.0635 0.1897 0.142 Uiso 1 1 calc R . . C23 C 0.1481(7) 0.8945(7) 0.2344(11) 0.097(6) Uani 1 1 d . . . H23A H 0.1549 0.9155 0.1978 0.146 Uiso 1 1 calc R . . H23B H 0.1486 0.9115 0.2729 0.146 Uiso 1 1 calc R . . H23C H 0.1165 0.8660 0.2294 0.146 Uiso 1 1 calc R . . C24 C 0.1194(6) 0.7961(7) 0.2533(11) 0.091(6) Uani 1 1 d . . . H24A H 0.1084 0.7961 0.2965 0.137 Uiso 1 1 calc R . . H24B H 0.1148 0.7644 0.2433 0.137 Uiso 1 1 calc R . . H24C H 0.1009 0.8039 0.2236 0.137 Uiso 1 1 calc R . . C25 C 0.3164(8) 0.8256(10) 0.4121(15) 0.133(9) Uani 1 1 d . . . H25A H 0.3193 0.7995 0.3932 0.199 Uiso 1 1 calc R . . H25B H 0.2906 0.8126 0.4435 0.199 Uiso 1 1 calc R . . H25C H 0.3466 0.8483 0.4326 0.199 Uiso 1 1 calc R . . C26 C 0.3315(16) 0.9735(12) 0.406(2) 1.08(8) Uani 1 1 d D . . H26 H 0.2986 0.9635 0.4112 1.292 Uiso 1 1 calc R . . C27 C 0.4168(13) 1.054(2) 0.413(6) 2.0(3) Uani 1 1 d D . . H27A H 0.4290 1.0327 0.4261 2.929 Uiso 1 1 calc R . . H27B H 0.4234 1.0776 0.4458 2.929 Uiso 1 1 calc R . . H27C H 0.4326 1.0701 0.3735 2.929 Uiso 1 1 calc R . . C28 C 0.3339(12) 1.0458(15) 0.3913(14) 0.29(4) Uani 1 1 d D . . H28A H 0.3523 1.0805 0.3980 0.435 Uiso 1 1 calc R . . H28B H 0.3069 1.0315 0.4208 0.435 Uiso 1 1 calc R . . H28C H 0.3219 1.0391 0.3479 0.435 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 W1 0.0759(5) 0.0554(4) 0.0837(6) 0.0084(3) 0.0333(4) 0.0330(3) Ni1 0.0428(12) 0.0428(12) 0.040(2) 0.000 0.000 0.0214(6) N1 0.035(5) 0.051(6) 0.050(6) -0.002(5) -0.005(4) 0.023(5) C1 0.057(8) 0.041(7) 0.044(7) 0.002(5) 0.006(6) 0.023(6) Ni2 0.0600(11) 0.0557(11) 0.0971(16) 0.0024(10) 0.0097(10) 0.0357(9) O2 0.058(6) 0.067(6) 0.091(8) 0.012(6) 0.001(5) 0.035(5) N2 0.065(8) 0.053(7) 0.091(10) -0.005(6) 0.005(7) 0.036(7) C2 0.074(10) 0.057(9) 0.090(12) -0.002(8) 0.017(9) 0.043(8) Ni3 0.179(4) 0.179(4) 0.039(2) 0.000 0.000 0.0895(18) N3 0.118(14) 0.129(14) 0.051(9) -0.013(9) 0.006(9) 0.062(12) C3 0.093(13) 0.107(14) 0.052(11) 0.004(10) 0.043(10) 0.044(12) N4 0.058(8) 0.087(10) 0.085(10) -0.003(8) 0.003(7) 0.038(7) C4 0.046(8) 0.055(9) 0.091(13) -0.002(8) 0.014(8) 0.025(7) N5 0.070(9) 0.045(7) 0.111(13) 0.015(8) 0.008(8) 0.027(6) C5 0.062(9) 0.055(9) 0.116(15) 0.028(9) 0.026(9) 0.033(8) O6 0.37(4) 0.24(3) 0.087(14) -0.070(16) -0.021(19) 0.13(3) N6 0.098(12) 0.130(15) 0.125(16) 0.008(11) 0.041(11) 0.074(12) C6 0.076(11) 0.086(12) 0.083(13) 0.007(10) 0.027(10) 0.039(10) O7 0.26(3) 0.123(16) 0.16(2) -0.073(15) 0.023(18) -0.004(17) N7 0.32(4) 0.34(4) 0.104(18) 0.06(2) 0.09(2) 0.28(4) C7 0.23(3) 0.19(3) 0.077(14) 0.051(15) 0.074(16) 0.19(3) N8 0.119(18) 0.091(15) 0.51(6) -0.08(2) 0.15(3) 0.002(14) C8 0.15(2) 0.097(18) 0.26(4) -0.01(2) 0.11(3) 0.051(18) N9 0.063(8) 0.056(7) 0.082(10) 0.012(6) 0.018(7) 0.029(6) C9 0.081(13) 0.103(15) 0.112(17) 0.009(12) 0.011(11) 0.053(12) N10 0.053(7) 0.058(7) 0.076(9) -0.002(6) 0.002(6) 0.034(6) C10 0.077(12) 0.081(12) 0.111(16) 0.017(11) 0.017(11) 0.039(10) C11 0.108(15) 0.065(10) 0.083(13) -0.020(9) -0.005(11) 0.041(11) C12 0.100(14) 0.070(11) 0.080(13) 0.008(9) 0.015(10) 0.048(11) C13 0.071(10) 0.075(10) 0.055(9) 0.008(7) 0.016(7) 0.038(8) C14 0.071(10) 0.077(11) 0.078(12) -0.003(9) -0.004(8) 0.045(9) C15 0.098(13) 0.066(10) 0.074(12) 0.002(8) 0.011(9) 0.050(10) C16 0.075(10) 0.077(11) 0.071(11) -0.011(8) -0.014(8) 0.054(9) C17 0.064(9) 0.093(12) 0.059(10) -0.016(8) -0.003(7) 0.048(9) C18 0.070(10) 0.077(10) 0.068(11) -0.002(8) 0.002(8) 0.044(9) C19 0.114(16) 0.058(10) 0.114(17) -0.009(10) 0.015(13) 0.045(11) C20 0.087(13) 0.070(11) 0.104(15) 0.011(10) 0.025(11) 0.049(10) C21 0.077(14) 0.107(17) 0.18(3) -0.021(17) -0.002(15) 0.023(13) C22 0.105(14) 0.062(10) 0.094(14) 0.014(9) 0.016(11) 0.025(10) C23 0.107(15) 0.084(13) 0.117(17) -0.003(11) -0.018(12) 0.060(12) C24 0.067(11) 0.085(12) 0.130(17) -0.038(12) -0.021(11) 0.044(10) C25 0.087(15) 0.14(2) 0.18(3) 0.014(19) 0.003(16) 0.061(15) C26 1.5(2) 0.26(4) 0.21(5) -0.17(4) 0.41(9) -0.510 C27 0.5(2) 2.0(7) 1.8(6) -1.0(3) 0.8(3) -0.557 C28 0.13(3) 0.44(7) 0.08(2) -0.02(3) -0.006(19) -0.02(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 W1 C3 2.10(3) . ? W1 C4 2.10(2) . ? W1 C5 2.121(16) . ? W1 C2 2.128(16) . ? W1 C1 2.146(14) . ? W1 C6 2.16(2) . ? W1 C8 2.18(3) . ? W1 C7 2.18(2) . ? Ni1 N1 2.024(11) 3_565 ? Ni1 N1 2.024(11) 2_665 ? Ni1 N1 2.024(11) 13_565 ? Ni1 N1 2.024(11) 14_455 ? Ni1 N1 2.024(11) 15 ? Ni1 N1 2.024(11) . ? N1 C1 1.156(16) 2_665 ? C1 N1 1.156(16) 3_565 ? Ni2 N2 2.038(13) . ? Ni2 N10 2.043(11) . ? Ni2 N4 2.053(14) . ? Ni2 N5 2.056(19) . ? Ni2 N9 2.057(12) . ? Ni2 O2 2.116(12) . ? O2 C25 1.40(3) . ? N2 C2 1.182(19) . ? Ni3 N3 2.07(2) . ? Ni3 N3 2.07(2) 3_565 ? Ni3 N3 2.07(2) 2_665 ? Ni3 O6 2.14(3) . ? Ni3 O6 2.14(3) 2_665 ? Ni3 O6 2.14(3) 3_565 ? N3 C3 1.19(2) . ? N4 C5 1.16(2) 3_565 ? C4 N5 1.18(2) 15 ? N5 C4 1.18(2) 14_455 ? C5 N4 1.16(2) 2_665 ? N6 C6 1.17(2) . ? O7 C26 1.41(2) . ? N7 C7 1.12(3) . ? N8 C8 1.17(3) . ? N9 C9 1.30(2) . ? N9 C13 1.355(19) . ? C9 C10 1.38(3) . ? N10 C18 1.290(19) . ? N10 C14 1.37(2) . ? C10 C11 1.38(3) . ? C10 C21 1.57(3) . ? N11 C27 1.466(14) . ? N11 C26 1.469(18) . ? N11 C28 1.474(19) . ? C11 C12 1.48(3) . ? C11 C22 1.48(2) . ? C12 C13 1.39(2) . ? C12 C19 1.39(3) . ? C13 C14 1.45(2) . ? C14 C15 1.40(2) . ? C15 C16 1.43(2) . ? C15 C20 1.44(2) . ? C16 C17 1.37(2) . ? C16 C23 1.52(2) . ? C17 C18 1.43(2) . ? C17 C24 1.45(2) . ? C19 C20 1.29(3) . ? 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 C3 W1 C4 143.9(6) . . ? C3 W1 C5 80.1(7) . . ? C4 W1 C5 84.5(7) . . ? C3 W1 C2 82.2(7) . . ? C4 W1 C2 93.1(6) . . ? C5 W1 C2 145.9(6) . . ? C3 W1 C1 71.3(5) . . ? C4 W1 C1 73.1(5) . . ? C5 W1 C1 73.3(5) . . ? C2 W1 C1 73.5(5) . . ? C3 W1 C6 135.4(7) . . ? C4 W1 C6 74.6(6) . . ? C5 W1 C6 138.8(7) . . ? C2 W1 C6 71.6(6) . . ? C1 W1 C6 130.2(6) . . ? C3 W1 C8 124.9(12) . . ? C4 W1 C8 78.4(12) . . ? C5 W1 C8 69.9(7) . . ? C2 W1 C8 142.9(9) . . ? C1 W1 C8 135.0(8) . . ? C6 W1 C8 71.4(9) . . ? C3 W1 C7 67.1(8) . . ? C4 W1 C7 148.9(8) . . ? C5 W1 C7 110.1(8) . . ? C2 W1 C7 89.2(9) . . ? C1 W1 C7 136.7(8) . . ? C6 W1 C7 76.8(7) . . ? C8 W1 C7 81.2(12) . . ? N1 Ni1 N1 91.1(4) 3_565 2_665 ? N1 Ni1 N1 88.9(4) 3_565 13_565 ? N1 Ni1 N1 88.9(4) 2_665 13_565 ? N1 Ni1 N1 88.9(4) 3_565 14_455 ? N1 Ni1 N1 179.996(2) 2_665 14_455 ? N1 Ni1 N1 91.1(4) 13_565 14_455 ? N1 Ni1 N1 180.0(5) 3_565 15 ? N1 Ni1 N1 88.9(4) 2_665 15 ? N1 Ni1 N1 91.1(4) 13_565 15 ? N1 Ni1 N1 91.1(4) 14_455 15 ? N1 Ni1 N1 91.1(4) 3_565 . ? N1 Ni1 N1 91.1(4) 2_665 . ? N1 Ni1 N1 179.996(2) 13_565 . ? N1 Ni1 N1 88.9(4) 14_455 . ? N1 Ni1 N1 88.9(4) 15 . ? C1 N1 Ni1 176.9(10) 2_665 . ? N1 C1 W1 177.2(12) 3_565 . ? N2 Ni2 N10 93.7(5) . . ? N2 Ni2 N4 91.6(5) . . ? N10 Ni2 N4 174.3(5) . . ? N2 Ni2 N5 92.3(5) . . ? N10 Ni2 N5 90.8(5) . . ? N4 Ni2 N5 91.2(6) . . ? N2 Ni2 N9 172.5(5) . . ? N10 Ni2 N9 80.3(5) . . ? N4 Ni2 N9 94.3(6) . . ? N5 Ni2 N9 92.3(5) . . ? N2 Ni2 O2 88.9(5) . . ? N10 Ni2 O2 88.5(5) . . ? N4 Ni2 O2 89.4(5) . . ? N5 Ni2 O2 178.7(4) . . ? N9 Ni2 O2 86.5(5) . . ? C25 O2 Ni2 121.0(14) . . ? C2 N2 Ni2 175.4(14) . . ? N2 C2 W1 175.1(14) . . ? N3 Ni3 N3 94.1(6) . 3_565 ? N3 Ni3 N3 94.1(6) . 2_665 ? N3 Ni3 N3 94.1(6) 3_565 2_665 ? N3 Ni3 O6 91.0(10) . . ? N3 Ni3 O6 87.3(10) 3_565 . ? N3 Ni3 O6 174.6(10) 2_665 . ? N3 Ni3 O6 87.3(10) . 2_665 ? N3 Ni3 O6 174.6(10) 3_565 2_665 ? N3 Ni3 O6 91.0(10) 2_665 2_665 ? O6 Ni3 O6 87.5(12) . 2_665 ? N3 Ni3 O6 174.6(10) . 3_565 ? N3 Ni3 O6 91.0(10) 3_565 3_565 ? N3 Ni3 O6 87.3(10) 2_665 3_565 ? O6 Ni3 O6 87.5(12) . 3_565 ? O6 Ni3 O6 87.5(12) 2_665 3_565 ? C3 N3 Ni3 176.7(18) . . ? N3 C3 W1 178.2(17) . . ? C5 N4 Ni2 178.4(15) 3_565 . ? N5 C4 W1 174.8(15) 15 . ? C4 N5 Ni2 178.4(13) 14_455 . ? N4 C5 W1 177.3(18) 2_665 . ? N6 C6 W1 179(2) . . ? N7 C7 W1 175(3) . . ? N8 C8 W1 173(3) . . ? C9 N9 C13 115.3(14) . . ? C9 N9 Ni2 130.3(12) . . ? C13 N9 Ni2 113.9(10) . . ? N9 C9 C10 126.0(18) . . ? C18 N10 C14 117.4(13) . . ? C18 N10 Ni2 128.9(10) . . ? C14 N10 Ni2 113.7(10) . . ? C11 C10 C9 120.5(18) . . ? C11 C10 C21 118.8(18) . . ? C9 C10 C21 120.6(19) . . ? C27 N11 C26 132(2) . . ? C27 N11 C28 124(2) . . ? C26 N11 C28 104(3) . . ? C10 C11 C12 115.3(16) . . ? C10 C11 C22 125.3(19) . . ? C12 C11 C22 119.4(18) . . ? C13 C12 C19 118.9(18) . . ? C13 C12 C11 116.7(16) . . ? C19 C12 C11 124.2(17) . . ? N9 C13 C12 125.8(15) . . ? N9 C13 C14 115.8(14) . . ? C12 C13 C14 118.3(15) . . ? N10 C14 C15 123.3(15) . . ? N10 C14 C13 116.2(13) . . ? C15 C14 C13 120.5(15) . . ? C14 C15 C16 117.6(15) . . ? C14 C15 C20 116.7(17) . . ? C16 C15 C20 125.7(16) . . ? C17 C16 C15 119.1(14) . . ? C17 C16 C23 117.2(16) . . ? C15 C16 C23 123.7(15) . . ? C16 C17 C18 117.4(15) . . ? C16 C17 C24 122.7(15) . . ? C18 C17 C24 119.8(16) . . ? N10 C18 C17 125.2(16) . . ? C20 C19 C12 123.7(18) . . ? C19 C20 C15 121.7(17) . . ? O7 C26 N11 126(3) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.947 _refine_diff_density_min -1.210 _refine_diff_density_rms 0.241 # Attachment 'comp4-Ni9Mo6.cif' data_c:\comp4.cif _database_code_depnum_ccdc_archive 'CCDC 694540' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H57 Mo2 N22 Ni3 O6' _chemical_formula_weight 1502.25 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 32.214(5) _cell_length_b 32.214(5) _cell_length_c 21.074(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 18939(5) _cell_formula_units_Z 9 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6867 _exptl_absorpt_coefficient_mu 0.999 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS v2.03 (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method 'profile data from \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 73793 _diffrn_reflns_av_R_equivalents 0.1367 _diffrn_reflns_av_sigmaI/netI 0.1301 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.76 _reflns_number_total 10423 _reflns_number_gt 3548 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2000)' _computing_cell_refinement 'SMART V5.625 (Bruker, 2000)' _computing_data_reduction 'SAINT V6.32 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _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^)+(0.2000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10423 _refine_ls_number_parameters 409 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2684 _refine_ls_R_factor_gt 0.1192 _refine_ls_wR_factor_ref 0.4215 _refine_ls_wR_factor_gt 0.3394 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 1.216 _refine_ls_shift/su_mean 0.061 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 Mo1 Mo 0.02088(3) 0.14603(4) 0.14101(5) 0.0837(5) Uani 1 1 d . . . Ni1 Ni -0.16599(5) 0.02738(5) 0.10311(8) 0.0810(5) Uani 1 1 d . . . O1 O -0.1846(3) 0.0254(3) 0.2005(4) 0.090(2) Uani 1 1 d . . . N1 N -0.0969(4) 0.0722(3) 0.1265(5) 0.085(3) Uani 1 1 d . . . C1 C -0.0572(5) 0.0970(4) 0.1341(6) 0.084(3) Uani 1 1 d . . . Ni2 Ni 0.0000 0.0000 0.0000 0.0583(8) Uani 1 6 d S . . O2 O -0.0073(8) -0.0522(9) 0.3541(10) 0.310(12) Uani 1 1 d . . . N2 N 0.0054(3) 0.0539(3) 0.0552(4) 0.0609(19) Uani 1 1 d . . . C2 C 0.0106(3) 0.0862(4) 0.0840(5) 0.063(2) Uani 1 1 d . . . Ni3 Ni 0.0000 0.0000 0.28536(14) 0.1390(14) Uani 1 3 d S . . N3 N 0.0100(5) 0.0584(6) 0.2313(6) 0.121(5) Uani 1 1 d . . . C3 C 0.0143(5) 0.0906(6) 0.1997(8) 0.119(6) Uani 1 1 d . . . N4 N -0.1578(3) -0.0314(4) 0.1196(5) 0.094(3) Uani 1 1 d . . . C4 C 0.0896(4) 0.1533(4) 0.1288(6) 0.081(3) Uani 1 1 d . . . O5 O -0.4069(17) -0.0569(9) -0.1024(13) 0.85(7) Uani 1 1 d D . . N5 N -0.1507(3) 0.0281(4) 0.0081(6) 0.090(3) Uani 1 1 d . . . C5 C 0.0262(4) 0.1681(4) 0.0455(8) 0.084(3) Uani 1 1 d . . . N6 N 0.1042(6) 0.2574(6) 0.1597(14) 0.280(16) Uani 1 1 d . . . C6 C 0.0755(6) 0.2194(7) 0.1504(13) 0.188(10) Uani 1 1 d . . . N7 N -0.0317(5) 0.2103(4) 0.1370(6) 0.115(4) Uani 1 1 d . . . C7 C -0.0138(5) 0.1899(5) 0.1381(6) 0.091(4) Uani 1 1 d . . . N8 N 0.0155(9) 0.1726(10) 0.2877(9) 0.266(14) Uani 1 1 d . . . C8 C 0.0162(7) 0.1614(8) 0.2374(9) 0.164(8) Uani 1 1 d . . . N9 N -0.2389(3) -0.0138(3) 0.0866(5) 0.084(3) Uani 1 1 d . . . C9 C -0.2675(5) -0.0598(4) 0.0881(6) 0.095(4) Uani 1 1 d . . . H9 H -0.2538 -0.0797 0.0937 0.114 Uiso 1 1 calc R . . N10 N -0.1805(3) 0.0819(3) 0.0893(4) 0.078(2) Uani 1 1 d . . . C10 C -0.3174(5) -0.0817(5) 0.0819(6) 0.095(4) Uani 1 1 d . . . N11 N -0.3302(7) 0.0238(8) -0.1049(6) 0.168(6) Uani 1 1 d . . . C11 C -0.3392(4) -0.0561(5) 0.0716(6) 0.095(4) Uani 1 1 d . . . C12 C -0.3099(4) -0.0057(5) 0.0686(5) 0.086(3) Uani 1 1 d . . . C13 C -0.2611(4) 0.0126(4) 0.0792(5) 0.084(3) Uani 1 1 d . . . C14 C -0.2282(5) 0.0663(4) 0.0800(5) 0.085(3) Uani 1 1 d . . . C15 C -0.2469(5) 0.0962(5) 0.0735(6) 0.093(4) Uani 1 1 d . . . C16 C -0.2147(4) 0.1458(4) 0.0729(6) 0.082(3) Uani 1 1 d . . . C17 C -0.1671(5) 0.1616(4) 0.0814(5) 0.085(3) Uani 1 1 d . . . C18 C -0.1514(4) 0.1278(4) 0.0888(5) 0.080(3) Uani 1 1 d . . . H18 H -0.1180 0.1393 0.0936 0.097 Uiso 1 1 calc R . . C19 C -0.3264(5) 0.0277(6) 0.0608(7) 0.110(4) Uani 1 1 d . . . H19 H -0.3597 0.0158 0.0545 0.132 Uiso 1 1 calc R . . C20 C -0.2972(5) 0.0748(5) 0.0620(7) 0.102(4) Uani 1 1 d . . . H20 H -0.3102 0.0951 0.0548 0.122 Uiso 1 1 calc R . . C21 C -0.3446(6) -0.1342(7) 0.0883(9) 0.158(7) Uani 1 1 d . . . H21A H -0.3727 -0.1473 0.0603 0.237 Uiso 1 1 calc R . . H21B H -0.3552 -0.1427 0.1324 0.237 Uiso 1 1 calc R . . H21C H -0.3242 -0.1474 0.0764 0.237 Uiso 1 1 calc R . . C22 C -0.3918(5) -0.0787(6) 0.0637(8) 0.136(6) Uani 1 1 d . . . H22A H -0.4079 -0.1070 0.0911 0.205 Uiso 1 1 calc R . . H22B H -0.4004 -0.0884 0.0193 0.205 Uiso 1 1 calc R . . H22C H -0.4021 -0.0557 0.0753 0.205 Uiso 1 1 calc R . . C23 C -0.2307(5) 0.1820(5) 0.0626(9) 0.131(5) Uani 1 1 d . . . H23A H -0.2628 0.1697 0.0805 0.196 Uiso 1 1 calc R . . H23B H -0.2314 0.1876 0.0170 0.196 Uiso 1 1 calc R . . H23C H -0.2082 0.2121 0.0836 0.196 Uiso 1 1 calc R . . C24 C -0.1279(5) 0.2165(4) 0.0845(6) 0.104(4) Uani 1 1 d . . . H24A H -0.1302 0.2328 0.0466 0.156 Uiso 1 1 calc R . . H24B H -0.0960 0.2199 0.0865 0.156 Uiso 1 1 calc R . . H24C H -0.1331 0.2309 0.1224 0.156 Uiso 1 1 calc R . . C25 C -0.1620(8) 0.0140(7) 0.2505(11) 0.178(8) Uani 1 1 d . . . H25A H -0.1757 -0.0208 0.2526 0.268 Uiso 1 1 calc R . . H25B H -0.1674 0.0256 0.2910 0.268 Uiso 1 1 calc R . . H25C H -0.1275 0.0294 0.2423 0.268 Uiso 1 1 calc R . . C26 C -0.3568(16) -0.0296(12) -0.0982(17) 0.36(3) Uani 1 1 d D . . H26 H -0.3392 -0.0455 -0.0909 0.433 Uiso 1 1 calc R . . C27 C -0.3621(12) 0.0452(14) -0.1001(11) 0.31(2) Uani 1 1 d . . . H27A H -0.3945 0.0216 -0.1140 0.469 Uiso 1 1 calc R . . H27B H -0.3495 0.0737 -0.1271 0.469 Uiso 1 1 calc R . . H27C H -0.3631 0.0542 -0.0559 0.469 Uiso 1 1 calc R . . C28 C -0.2731(8) 0.0544(8) -0.1110(13) 0.208(10) Uani 1 1 d . . . H28A H -0.2597 0.0745 -0.0732 0.312 Uiso 1 1 calc R . . H28B H -0.2644 0.0749 -0.1488 0.312 Uiso 1 1 calc R . . H28C H -0.2602 0.0327 -0.1149 0.312 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 Mo1 0.0684(7) 0.0903(8) 0.0945(8) -0.0325(6) -0.0084(5) 0.0413(6) Ni1 0.0672(9) 0.0726(9) 0.1126(13) -0.0092(8) -0.0026(8) 0.0420(8) O1 0.092(5) 0.075(5) 0.110(6) 0.001(4) -0.006(5) 0.046(4) N1 0.067(6) 0.077(6) 0.115(8) -0.015(5) -0.020(5) 0.040(5) C1 0.079(8) 0.089(8) 0.097(9) -0.028(7) -0.017(7) 0.051(7) Ni2 0.0589(11) 0.0589(11) 0.0571(17) 0.000 0.000 0.0294(5) O2 0.34(2) 0.41(3) 0.28(2) 0.23(2) 0.071(18) 0.26(3) N2 0.059(5) 0.054(5) 0.060(5) -0.002(4) -0.008(4) 0.021(4) C2 0.051(5) 0.066(6) 0.075(7) -0.004(5) 0.002(5) 0.033(5) Ni3 0.180(2) 0.180(2) 0.0564(18) 0.000 0.000 0.0902(11) N3 0.124(10) 0.149(13) 0.072(8) -0.018(7) 0.017(7) 0.055(10) C3 0.086(9) 0.135(14) 0.114(13) -0.067(11) 0.010(9) 0.037(10) N4 0.086(7) 0.088(7) 0.122(8) -0.010(6) -0.001(6) 0.054(6) C4 0.060(7) 0.082(8) 0.099(9) -0.008(6) -0.011(6) 0.034(6) O5 2.0(2) 0.25(3) 0.38(4) -0.18(3) -0.67(8) 0.62(7) N5 0.072(6) 0.088(7) 0.125(9) -0.016(7) -0.013(6) 0.050(6) C5 0.070(7) 0.060(7) 0.122(11) 0.000(7) 0.016(7) 0.033(6) N6 0.093(10) 0.142(14) 0.55(4) -0.18(2) 0.041(16) 0.015(10) C6 0.096(12) 0.130(15) 0.32(3) -0.125(17) -0.019(14) 0.045(11) N7 0.129(10) 0.084(7) 0.153(11) -0.004(7) 0.022(8) 0.069(8) C7 0.091(9) 0.084(8) 0.099(9) -0.027(7) -0.017(7) 0.043(7) N8 0.44(4) 0.44(3) 0.135(14) -0.106(18) -0.095(18) 0.39(3) C8 0.202(18) 0.26(2) 0.116(13) -0.109(14) -0.064(12) 0.179(18) N9 0.069(6) 0.079(7) 0.113(8) -0.013(5) -0.015(5) 0.042(5) C9 0.101(10) 0.071(8) 0.102(9) -0.002(7) -0.012(7) 0.034(7) N10 0.059(5) 0.076(6) 0.101(7) -0.004(5) 0.002(5) 0.036(5) C10 0.096(10) 0.069(8) 0.096(9) -0.009(7) 0.004(7) 0.024(8) N11 0.200(18) 0.223(19) 0.080(9) -0.013(10) -0.024(10) 0.105(15) C11 0.073(8) 0.105(10) 0.104(10) -0.028(8) -0.003(7) 0.041(8) C12 0.071(8) 0.114(10) 0.084(8) -0.021(7) -0.011(6) 0.054(8) C13 0.081(8) 0.091(8) 0.077(7) -0.015(6) 0.001(6) 0.040(7) C14 0.103(9) 0.084(8) 0.081(8) -0.006(6) 0.001(7) 0.056(7) C15 0.099(9) 0.122(11) 0.090(9) -0.005(7) 0.011(7) 0.080(9) C16 0.073(7) 0.083(8) 0.108(9) 0.009(6) 0.014(6) 0.052(7) C17 0.111(10) 0.077(7) 0.082(8) 0.003(6) 0.005(7) 0.060(7) C18 0.083(8) 0.076(8) 0.093(8) -0.011(6) -0.007(6) 0.047(7) C19 0.076(8) 0.144(13) 0.122(11) -0.004(10) 0.009(8) 0.063(10) C20 0.087(9) 0.109(11) 0.130(12) -0.012(9) 0.013(8) 0.064(9) C21 0.121(13) 0.21(2) 0.142(15) 0.034(14) 0.001(11) 0.085(15) C22 0.084(10) 0.135(13) 0.164(15) -0.047(11) 0.004(9) 0.035(9) C23 0.116(11) 0.114(11) 0.193(17) 0.009(11) -0.003(10) 0.081(10) C24 0.106(10) 0.081(8) 0.121(11) -0.011(7) 0.010(8) 0.045(8) C25 0.23(2) 0.154(17) 0.20(2) -0.033(15) 0.009(18) 0.136(18) C26 0.66(8) 0.16(3) 0.23(4) -0.07(2) 0.08(4) 0.18(4) C27 0.39(4) 0.65(7) 0.124(18) -0.13(3) -0.08(2) 0.43(5) C28 0.17(2) 0.16(2) 0.29(3) -0.025(18) 0.037(19) 0.082(17) _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 Mo1 C3 2.09(2) . ? Mo1 C4 2.121(12) . ? Mo1 C5 2.113(16) . ? Mo1 C8 2.114(17) . ? Mo1 C6 2.137(19) . ? Mo1 C2 2.151(11) . ? Mo1 C7 2.197(14) . ? Mo1 C1 2.208(13) . ? Ni1 N1 2.017(10) . ? Ni1 N10 2.051(9) . ? Ni1 N5 2.060(13) . ? Ni1 N9 2.068(9) . ? Ni1 N4 2.069(11) . ? Ni1 O1 2.130(9) . ? O1 C25 1.43(2) . ? N1 C1 1.130(13) . ? Ni2 N2 2.023(9) 2 ? Ni2 N2 2.023(9) 12 ? Ni2 N2 2.023(9) . ? Ni2 N2 2.023(9) 11 ? Ni2 N2 2.023(9) 10 ? Ni2 N2 2.023(9) 3 ? O2 Ni3 2.142(13) . ? N2 C2 1.143(11) . ? Ni3 N3 2.083(16) 2 ? Ni3 N3 2.083(16) . ? Ni3 N3 2.083(16) 3 ? Ni3 O2 2.142(13) 3 ? Ni3 O2 2.142(13) 2 ? N3 C3 1.18(2) . ? N4 C4 1.137(13) 2 ? C4 N4 1.137(13) 3 ? O5 C26 1.40(2) . ? N5 C5 1.172(15) 12 ? C5 N5 1.172(15) 11 ? N6 C6 1.122(19) . ? N7 C7 1.069(14) . ? N8 C8 1.122(19) . ? N9 C9 1.296(14) . ? N9 C13 1.366(14) . ? C9 C10 1.403(17) . ? N10 C18 1.296(13) . ? N10 C14 1.371(14) . ? C10 C11 1.341(18) . ? C10 C21 1.47(2) . ? N11 C26 1.50(3) . ? N11 C27 1.50(2) . ? N11 C28 1.60(2) . ? C11 C12 1.412(18) . ? C11 C22 1.483(17) . ? C12 C13 1.395(15) . ? C12 C19 1.430(18) . ? C13 C14 1.510(16) . ? C14 C15 1.376(15) . ? C15 C16 1.404(16) . ? C15 C20 1.430(17) . ? C16 C17 1.366(15) . ? C16 C23 1.505(15) . ? C17 C18 1.422(14) . ? C17 C24 1.578(16) . ? C19 C20 1.326(17) . ? 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 C3 Mo1 C4 79.7(5) . . ? C3 Mo1 C5 143.7(5) . . ? C4 Mo1 C5 86.6(4) . . ? C3 Mo1 C8 69.2(7) . . ? C4 Mo1 C8 106.5(6) . . ? C5 Mo1 C8 147.1(7) . . ? C3 Mo1 C6 124.4(8) . . ? C4 Mo1 C6 69.6(5) . . ? C5 Mo1 C6 80.4(8) . . ? C8 Mo1 C6 76.5(9) . . ? C3 Mo1 C2 70.2(4) . . ? C4 Mo1 C2 73.5(4) . . ? C5 Mo1 C2 73.7(4) . . ? C8 Mo1 C2 138.6(7) . . ? C6 Mo1 C2 135.7(6) . . ? C3 Mo1 C7 134.2(5) . . ? C4 Mo1 C7 139.8(5) . . ? C5 Mo1 C7 74.9(5) . . ? C8 Mo1 C7 76.0(6) . . ? C6 Mo1 C7 72.2(6) . . ? C2 Mo1 C7 131.3(4) . . ? C3 Mo1 C1 80.5(5) . . ? C4 Mo1 C1 145.5(4) . . ? C5 Mo1 C1 92.9(4) . . ? C8 Mo1 C1 92.4(6) . . ? C6 Mo1 C1 144.2(6) . . ? C2 Mo1 C1 73.4(4) . . ? C7 Mo1 C1 72.1(4) . . ? N1 Ni1 N10 93.7(4) . . ? N1 Ni1 N5 93.3(4) . . ? N10 Ni1 N5 90.5(4) . . ? N1 Ni1 N9 173.0(4) . . ? N10 Ni1 N9 81.6(4) . . ? N5 Ni1 N9 91.9(4) . . ? N1 Ni1 N4 90.8(4) . . ? N10 Ni1 N4 174.8(4) . . ? N5 Ni1 N4 92.0(4) . . ? N9 Ni1 N4 93.8(4) . . ? N1 Ni1 O1 88.8(4) . . ? N10 Ni1 O1 88.9(3) . . ? N5 Ni1 O1 177.8(3) . . ? N9 Ni1 O1 86.0(4) . . ? N4 Ni1 O1 88.5(4) . . ? C25 O1 Ni1 123.1(10) . . ? C1 N1 Ni1 173.8(10) . . ? N1 C1 Mo1 175.6(11) . . ? N2 Ni2 N2 89.8(3) 2 12 ? N2 Ni2 N2 90.2(3) 2 . ? N2 Ni2 N2 89.8(3) 12 . ? N2 Ni2 N2 180.0(10) 2 11 ? N2 Ni2 N2 90.2(3) 12 11 ? N2 Ni2 N2 89.8(3) . 11 ? N2 Ni2 N2 89.8(3) 2 10 ? N2 Ni2 N2 90.2(3) 12 10 ? N2 Ni2 N2 180.0(6) . 10 ? N2 Ni2 N2 90.2(3) 11 10 ? N2 Ni2 N2 90.2(3) 2 3 ? N2 Ni2 N2 180.0(5) 12 3 ? N2 Ni2 N2 90.2(3) . 3 ? N2 Ni2 N2 89.8(3) 11 3 ? N2 Ni2 N2 89.8(3) 10 3 ? C2 N2 Ni2 175.8(8) . . ? N2 C2 Mo1 178.1(9) . . ? N3 Ni3 N3 92.9(5) 2 . ? N3 Ni3 N3 92.9(5) 2 3 ? N3 Ni3 N3 92.9(5) . 3 ? N3 Ni3 O2 92.6(7) 2 3 ? N3 Ni3 O2 94.5(8) . 3 ? N3 Ni3 O2 170.5(9) 3 3 ? N3 Ni3 O2 170.5(9) 2 2 ? N3 Ni3 O2 92.6(7) . 2 ? N3 Ni3 O2 94.5(8) 3 2 ? O2 Ni3 O2 79.3(12) 3 2 ? N3 Ni3 O2 94.5(8) 2 . ? N3 Ni3 O2 170.5(9) . . ? N3 Ni3 O2 92.6(7) 3 . ? O2 Ni3 O2 79.3(12) 3 . ? O2 Ni3 O2 79.3(12) 2 . ? C3 N3 Ni3 177.9(17) . . ? N3 C3 Mo1 178.0(15) . . ? C4 N4 Ni1 179.9(13) 2 . ? N4 C4 Mo1 177.1(11) 3 . ? C5 N5 Ni1 176.2(10) 12 . ? N5 C5 Mo1 177.8(12) 11 . ? N6 C6 Mo1 175(3) . . ? N7 C7 Mo1 178.3(13) . . ? N8 C8 Mo1 176(3) . . ? C9 N9 C13 114.8(10) . . ? C9 N9 Ni1 131.2(9) . . ? C13 N9 Ni1 113.6(8) . . ? N9 C9 C10 123.6(12) . . ? C18 N10 C14 117.2(10) . . ? C18 N10 Ni1 129.2(7) . . ? C14 N10 Ni1 113.5(7) . . ? C11 C10 C9 121.8(12) . . ? C11 C10 C21 121.8(14) . . ? C9 C10 C21 116.4(13) . . ? C26 N11 C27 113(3) . . ? C26 N11 C28 123(2) . . ? C27 N11 C28 124(2) . . ? C10 C11 C12 117.4(11) . . ? C10 C11 C22 122.5(14) . . ? C12 C11 C22 120.1(13) . . ? C13 C12 C11 116.2(11) . . ? C13 C12 C19 117.8(12) . . ? C11 C12 C19 125.8(12) . . ? N9 C13 C12 126.0(11) . . ? N9 C13 C14 115.1(10) . . ? C12 C13 C14 118.9(11) . . ? C15 C14 N10 124.0(11) . . ? C15 C14 C13 119.9(12) . . ? N10 C14 C13 116.0(10) . . ? C14 C15 C16 117.8(11) . . ? C14 C15 C20 117.8(13) . . ? C16 C15 C20 124.1(11) . . ? C17 C16 C15 118.4(10) . . ? C17 C16 C23 119.0(11) . . ? C15 C16 C23 122.6(11) . . ? C16 C17 C18 119.5(11) . . ? C16 C17 C24 123.0(10) . . ? C18 C17 C24 117.5(11) . . ? N10 C18 C17 122.9(11) . . ? C20 C19 C12 122.7(12) . . ? C19 C20 C15 122.7(13) . . ? O5 C26 N11 122(3) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 28.76 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 1.724 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.164