# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Sally Brooker' _publ_contact_author_email Sbrooker@chemistry.otago.ac.nz _publ_author_name 'Sally Brooker' data_wag161 _database_code_depnum_ccdc_archive 'CCDC 842529' #TrackingRef 'wag161.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H58.50 Cl4 N13.50 Ni2 O16' _chemical_formula_weight 1375.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 14.1623(12) _cell_length_b 11.1055(8) _cell_length_c 19.3952(17) _cell_angle_alpha 90.00 _cell_angle_beta 91.551(5) _cell_angle_gamma 90.00 _cell_volume 3049.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 92(2) _cell_measurement_reflns_used 6343 _cell_measurement_theta_min 2.573 _cell_measurement_theta_max 24.241 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1422 _exptl_absorpt_coefficient_mu 0.870 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7224 _exptl_absorpt_correction_T_max 0.9578 _exptl_absorpt_process_details 'SCALE (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 92(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 Kappa Apex II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54058 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 26.41 _reflns_number_total 12458 _reflns_number_gt 10611 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All non-H ANIS. All H's calc and ride. Cl4 perchlorate twirling about the Cl4-O41 bond; CL42-CL44:CL45-Cl47 0.5:0.5 occupancy. Restrained by EADP to have equal opp ADPs and by SAME to have CL1-O14 perchlorate geom. Racemic twin 0.11(1). One full occup and one half occup MeCN of solvation. ; _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^)+(0.0596P)^2^+1.5924P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.112(12) _refine_ls_number_reflns 12458 _refine_ls_number_parameters 811 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.1143 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.05228(3) 0.72943(5) 0.90939(3) 0.02127(13) Uani 1 1 d . . . Ni2 Ni 0.02258(3) 0.78336(4) 0.57253(3) 0.02056(13) Uani 1 1 d . . . N11 N 0.0546(2) 0.6939(3) 0.79741(18) 0.0198(7) Uani 1 1 d . . . N12 N 0.1396(3) 0.5770(3) 0.90655(18) 0.0225(8) Uani 1 1 d . . . N13 N 0.0437(3) 0.7204(4) 1.0152(2) 0.0290(9) Uani 1 1 d . . . N14 N 0.1640(3) 0.8568(3) 0.91475(18) 0.0205(8) Uani 1 1 d . . . N15 N 0.0129(3) 0.7103(3) 0.67833(17) 0.0194(7) Uani 1 1 d . . . N16 N -0.0614(3) 0.6299(3) 0.55896(19) 0.0229(8) Uani 1 1 d . . . N17 N 0.0374(3) 0.8098(3) 0.4669(2) 0.0242(8) Uani 1 1 d . . . N18 N -0.0921(3) 0.9063(3) 0.57582(19) 0.0226(8) Uani 1 1 d . . . C1 C 0.0668(3) 0.5738(4) 0.7888(2) 0.0198(9) Uani 1 1 d . . . C2 C 0.0458(3) 0.5185(4) 0.7266(2) 0.0229(9) Uani 1 1 d . . . H2 H 0.0520 0.4338 0.7215 0.028 Uiso 1 1 calc R . . C3 C 0.0158(3) 0.5894(4) 0.6723(2) 0.0202(9) Uani 1 1 d . . . C4 C 0.0286(3) 0.7589(4) 0.7414(2) 0.0198(9) Uani 1 1 d . . . C5 C 0.0114(3) 0.8896(4) 0.7483(2) 0.0263(10) Uani 1 1 d . . . C6 C 0.0825(4) 0.9718(4) 0.7577(2) 0.0338(11) Uani 1 1 d . . . H6 H 0.1464 0.9457 0.7608 0.041 Uiso 1 1 calc R . . C7 C 0.0609(5) 1.0945(4) 0.7627(3) 0.0468(15) Uani 1 1 d . . . H7 H 0.1103 1.1520 0.7675 0.056 Uiso 1 1 calc R . . C8 C -0.0323(5) 1.1321(5) 0.7607(3) 0.0535(18) Uani 1 1 d . . . H8 H -0.0466 1.2153 0.7652 0.064 Uiso 1 1 calc R . . C9 C -0.1053(5) 1.0492(5) 0.7523(3) 0.0463(15) Uani 1 1 d . . . H9 H -0.1692 1.0752 0.7515 0.056 Uiso 1 1 calc R . . C10 C -0.0839(4) 0.9290(4) 0.7451(2) 0.0321(11) Uani 1 1 d . . . H10 H -0.1332 0.8721 0.7380 0.038 Uiso 1 1 calc R . . C11 C 0.0970(3) 0.5005(4) 0.8507(2) 0.0244(9) Uani 1 1 d . . . H11A H 0.0416 0.4575 0.8686 0.029 Uiso 1 1 calc R . . H11B H 0.1437 0.4395 0.8367 0.029 Uiso 1 1 calc R . . C12 C 0.1468(3) 0.5038(4) 0.9717(2) 0.0307(11) Uani 1 1 d . . . H12A H 0.1990 0.5366 1.0010 0.037 Uiso 1 1 calc R . . H12B H 0.1638 0.4202 0.9594 0.037 Uiso 1 1 calc R . . C13 C 0.0581(4) 0.5009(4) 1.0134(2) 0.0331(11) Uani 1 1 d . . . H13A H 0.0034 0.4831 0.9822 0.040 Uiso 1 1 calc R . . H13B H 0.0634 0.4347 1.0475 0.040 Uiso 1 1 calc R . . C14 C 0.0403(3) 0.6147(5) 1.0501(2) 0.0339(12) Uani 1 1 d . . . C15 C 0.0193(4) 0.6154(6) 1.1209(3) 0.0426(14) Uani 1 1 d . . . H15 H 0.0139 0.5410 1.1446 0.051 Uiso 1 1 calc R . . C16 C 0.0066(4) 0.7216(6) 1.1565(3) 0.0489(16) Uani 1 1 d . . . H16 H -0.0064 0.7213 1.2043 0.059 Uiso 1 1 calc R . . C17 C 0.0133(4) 0.8282(6) 1.1202(3) 0.0413(13) Uani 1 1 d . . . H17 H 0.0051 0.9030 1.1431 0.050 Uiso 1 1 calc R . . C18 C 0.0319(3) 0.8260(5) 1.0507(2) 0.0334(11) Uani 1 1 d . . . H18 H 0.0367 0.9001 1.0266 0.040 Uiso 1 1 calc R . . C22 C 0.2382(3) 0.6074(4) 0.8842(2) 0.0231(9) Uani 1 1 d . . . H22A H 0.2347 0.6386 0.8364 0.028 Uiso 1 1 calc R . . H22B H 0.2766 0.5329 0.8842 0.028 Uiso 1 1 calc R . . C23 C 0.2872(3) 0.7005(4) 0.9306(2) 0.0243(10) Uani 1 1 d . . . H23A H 0.2748 0.6801 0.9792 0.029 Uiso 1 1 calc R . . H23B H 0.3562 0.6942 0.9244 0.029 Uiso 1 1 calc R . . C24 C 0.2581(3) 0.8290(4) 0.9181(2) 0.0222(9) Uani 1 1 d . . . C25 C 0.3275(3) 0.9160(4) 0.9122(2) 0.0233(9) Uani 1 1 d . . . H25 H 0.3921 0.8929 0.9135 0.028 Uiso 1 1 calc R . . C26 C 0.3039(3) 1.0358(4) 0.9046(2) 0.0268(10) Uani 1 1 d . . . H26 H 0.3510 1.0956 0.8992 0.032 Uiso 1 1 calc R . . C27 C 0.2091(3) 1.0657(4) 0.9050(2) 0.0254(10) Uani 1 1 d . . . H27 H 0.1897 1.1474 0.9022 0.030 Uiso 1 1 calc R . . C28 C 0.1432(3) 0.9746(4) 0.9096(2) 0.0240(10) Uani 1 1 d . . . H28 H 0.0784 0.9968 0.9091 0.029 Uiso 1 1 calc R . . C31 C -0.0149(3) 0.5358(4) 0.6041(2) 0.0237(9) Uani 1 1 d . . . H31A H 0.0407 0.5025 0.5808 0.028 Uiso 1 1 calc R . . H31B H -0.0598 0.4691 0.6118 0.028 Uiso 1 1 calc R . . C32 C -0.0676(3) 0.5800(4) 0.4866(2) 0.0285(10) Uani 1 1 d . . . H32A H -0.1194 0.6216 0.4609 0.034 Uiso 1 1 calc R . . H32B H -0.0843 0.4935 0.4890 0.034 Uiso 1 1 calc R . . C33 C 0.0221(4) 0.5926(4) 0.4466(2) 0.0314(11) Uani 1 1 d . . . H33A H 0.0758 0.5645 0.4761 0.038 Uiso 1 1 calc R . . H33B H 0.0178 0.5388 0.4060 0.038 Uiso 1 1 calc R . . C34 C 0.0434(3) 0.7177(4) 0.4223(2) 0.0248(10) Uani 1 1 d . . . C35 C 0.0671(4) 0.7391(5) 0.3534(3) 0.0308(11) Uani 1 1 d . . . H35 H 0.0716 0.6736 0.3221 0.037 Uiso 1 1 calc R . . C36 C 0.0836(4) 0.8539(5) 0.3313(3) 0.0363(12) Uani 1 1 d . . . H36 H 0.1016 0.8686 0.2852 0.044 Uiso 1 1 calc R . . C37 C 0.0738(3) 0.9481(4) 0.3769(2) 0.0309(11) Uani 1 1 d . . . H37 H 0.0823 1.0290 0.3623 0.037 Uiso 1 1 calc R . . C38 C 0.0514(3) 0.9230(4) 0.4438(2) 0.0254(10) Uani 1 1 d . . . H38 H 0.0455 0.9880 0.4753 0.030 Uiso 1 1 calc R . . C42 C -0.1583(3) 0.6478(4) 0.5847(2) 0.0271(10) Uani 1 1 d . . . H42A H -0.1540 0.6626 0.6350 0.033 Uiso 1 1 calc R . . H42B H -0.1947 0.5725 0.5772 0.033 Uiso 1 1 calc R . . C43 C -0.2122(4) 0.7509(4) 0.5506(3) 0.0271(10) Uani 1 1 d . . . H43A H -0.2056 0.7431 0.5001 0.033 Uiso 1 1 calc R . . H43B H -0.2799 0.7403 0.5603 0.033 Uiso 1 1 calc R . . C44 C -0.1849(3) 0.8766(4) 0.5705(2) 0.0231(9) Uani 1 1 d . . . C45 C -0.2553(3) 0.9613(4) 0.5792(2) 0.0285(10) Uani 1 1 d . . . H45 H -0.3197 0.9371 0.5782 0.034 Uiso 1 1 calc R . . C46 C -0.2317(3) 1.0826(4) 0.5894(2) 0.0295(10) Uani 1 1 d . . . H46 H -0.2792 1.1421 0.5946 0.035 Uiso 1 1 calc R . . C47 C -0.1370(3) 1.1128(4) 0.5917(2) 0.0268(10) Uani 1 1 d . . . H47 H -0.1183 1.1945 0.5971 0.032 Uiso 1 1 calc R . . C48 C -0.0711(3) 1.0251(4) 0.5861(2) 0.0244(10) Uani 1 1 d . . . H48 H -0.0064 1.0476 0.5895 0.029 Uiso 1 1 calc R . . N70 N 0.1232(3) 0.9147(3) 0.5970(2) 0.0273(9) Uani 1 1 d . . . C70 C 0.1826(4) 0.9804(4) 0.6083(3) 0.0347(11) Uani 1 1 d . . . C71 C 0.2583(5) 1.0679(6) 0.6243(4) 0.0645(19) Uani 1 1 d . . . H71A H 0.2393 1.1476 0.6073 0.077 Uiso 1 1 calc R . . H71B H 0.3163 1.0429 0.6019 0.077 Uiso 1 1 calc R . . H71C H 0.2696 1.0714 0.6743 0.077 Uiso 1 1 calc R . . N80 N 0.1521(3) 0.6760(3) 0.57436(19) 0.0252(8) Uani 1 1 d . . . C80 C 0.2172(3) 0.6207(4) 0.5889(2) 0.0271(10) Uani 1 1 d . . . C81 C 0.2989(3) 0.5456(4) 0.6087(3) 0.0358(12) Uani 1 1 d . . . H81A H 0.2875 0.5064 0.6530 0.043 Uiso 1 1 calc R . . H81B H 0.3555 0.5961 0.6130 0.043 Uiso 1 1 calc R . . H81C H 0.3083 0.4840 0.5733 0.043 Uiso 1 1 calc R . . N60 N -0.0765(3) 0.6172(4) 0.9011(2) 0.0307(9) Uani 1 1 d . . . C60 C -0.1429(4) 0.5625(5) 0.8941(3) 0.0343(11) Uani 1 1 d . . . C61 C -0.2274(4) 0.4854(6) 0.8879(3) 0.0520(16) Uani 1 1 d . . . H61A H -0.2081 0.4014 0.8822 0.062 Uiso 1 1 calc R . . H61B H -0.2660 0.5106 0.8477 0.062 Uiso 1 1 calc R . . H61C H -0.2644 0.4932 0.9296 0.062 Uiso 1 1 calc R . . N50 N -0.0507(3) 0.8622(4) 0.90590(19) 0.0262(9) Uani 1 1 d . . . C50 C -0.1134(4) 0.9229(5) 0.9091(3) 0.0352(11) Uani 1 1 d . . . C51 C -0.1964(4) 1.0026(6) 0.9125(3) 0.0508(15) Uani 1 1 d . . . H51A H -0.2329 0.9982 0.8689 0.061 Uiso 1 1 calc R . . H51B H -0.1754 1.0856 0.9205 0.061 Uiso 1 1 calc R . . H51C H -0.2361 0.9769 0.9504 0.061 Uiso 1 1 calc R . . Cl1 Cl -0.18476(8) 0.68240(9) 0.28514(5) 0.0267(2) Uani 1 1 d D . . O11 O -0.1476(3) 0.7976(3) 0.26620(18) 0.0354(8) Uani 1 1 d D . . O12 O -0.1155(3) 0.5897(3) 0.2750(2) 0.0442(9) Uani 1 1 d D . . O13 O -0.2685(3) 0.6559(4) 0.24385(18) 0.0441(9) Uani 1 1 d D . . O14 O -0.2085(2) 0.6855(3) 0.35733(16) 0.0309(7) Uani 1 1 d D . . Cl2 Cl -0.23969(9) 0.38294(11) 0.69640(7) 0.0372(3) Uani 1 1 d . . . O21 O -0.1480(3) 0.4073(5) 0.7220(2) 0.0724(15) Uani 1 1 d . . . O22 O -0.2394(3) 0.3699(3) 0.62273(18) 0.0388(8) Uani 1 1 d . . . O23 O -0.3019(4) 0.4787(5) 0.7135(3) 0.0852(18) Uani 1 1 d . . . O24 O -0.2737(3) 0.2753(4) 0.7278(2) 0.0631(13) Uani 1 1 d . . . Cl3 Cl -0.03712(10) 1.19855(11) 1.03524(9) 0.0489(4) Uani 1 1 d . . . O31 O 0.0451(4) 1.1964(6) 0.9947(3) 0.100(2) Uani 1 1 d . . . O32 O -0.1103(3) 1.2645(4) 0.9994(3) 0.0610(12) Uani 1 1 d . . . O33 O -0.0686(5) 1.0787(4) 1.0454(4) 0.117(3) Uani 1 1 d . . . O34 O -0.0146(3) 1.2551(4) 1.0995(2) 0.0569(11) Uani 1 1 d . . . Cl4 Cl 0.10979(11) 0.27339(10) 0.48650(9) 0.0504(4) Uani 1 1 d D . . O41 O 0.1596(3) 0.3739(3) 0.5140(2) 0.0463(10) Uani 1 1 d D A . O42 O 0.1516(14) 0.2713(13) 0.4151(7) 0.149(5) Uani 0.50 1 d PD A 1 O43 O 0.1303(8) 0.1581(8) 0.5063(7) 0.075(3) Uani 0.50 1 d PD A 1 O44 O 0.0122(7) 0.2917(10) 0.4850(10) 0.110(5) Uani 0.50 1 d PD A 1 O45 O 0.0444(8) 0.2999(8) 0.4343(6) 0.075(3) Uani 0.50 1 d PD A 2 O46 O 0.0607(14) 0.2357(13) 0.5510(8) 0.149(5) Uani 0.50 1 d PD A 2 O47 O 0.1723(8) 0.1778(10) 0.4774(9) 0.110(5) Uani 0.50 1 d PD A 2 N90 N 0.2710(5) 0.7686(5) 0.7303(3) 0.0606(15) Uani 1 1 d . . . C90 C 0.3347(5) 0.8261(6) 0.7346(3) 0.0552(16) Uani 1 1 d . . . C91 C 0.4155(5) 0.9090(7) 0.7424(4) 0.074(2) Uani 1 1 d . . . H91A H 0.3936 0.9921 0.7362 0.089 Uiso 1 1 calc R . . H91B H 0.4622 0.8902 0.7076 0.089 Uiso 1 1 calc R . . H91C H 0.4444 0.8998 0.7886 0.089 Uiso 1 1 calc R . . N100 N -0.3234(7) 0.8270(14) 0.7573(6) 0.077(4) Uani 0.50 1 d P . . C100 C -0.3736(9) 0.7529(14) 0.7604(7) 0.056(4) Uani 0.50 1 d P . . C101 C -0.4442(8) 0.6571(10) 0.7671(6) 0.047(3) Uani 0.50 1 d P . . H10A H -0.4175 0.5805 0.7519 0.056 Uiso 0.50 1 calc PR . . H10B H -0.5002 0.6766 0.7386 0.056 Uiso 0.50 1 calc PR . . H10C H -0.4619 0.6503 0.8155 0.056 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0194(3) 0.0249(3) 0.0194(3) 0.0022(2) -0.0022(2) -0.0007(2) Ni2 0.0211(3) 0.0196(2) 0.0208(3) -0.0009(2) -0.0051(2) -0.0009(2) N11 0.0172(19) 0.0206(17) 0.0215(18) 0.0024(13) -0.0023(15) -0.0004(14) N12 0.024(2) 0.0232(18) 0.0204(19) 0.0042(14) -0.0041(15) -0.0019(15) N13 0.020(2) 0.043(2) 0.024(2) 0.0039(17) 0.0016(17) -0.0028(17) N14 0.021(2) 0.0224(18) 0.0179(18) -0.0001(13) -0.0011(15) 0.0023(15) N15 0.0195(19) 0.0212(17) 0.0173(17) 0.0004(13) -0.0007(14) 0.0011(14) N16 0.026(2) 0.0179(16) 0.0248(19) 0.0025(14) -0.0087(16) -0.0011(15) N17 0.018(2) 0.0279(19) 0.027(2) 0.0037(16) -0.0059(16) -0.0024(16) N18 0.025(2) 0.0205(17) 0.0218(19) 0.0006(14) -0.0038(16) -0.0020(15) C1 0.015(2) 0.023(2) 0.021(2) 0.0050(16) -0.0029(17) -0.0048(16) C2 0.025(2) 0.016(2) 0.027(2) 0.0006(17) -0.0057(19) -0.0018(16) C3 0.018(2) 0.0180(19) 0.025(2) -0.0015(16) -0.0026(17) 0.0031(16) C4 0.018(2) 0.023(2) 0.0180(18) 0.0015(14) -0.0034(16) -0.0022(16) C5 0.034(3) 0.028(2) 0.017(2) -0.0006(17) -0.0038(19) 0.002(2) C6 0.047(3) 0.029(2) 0.025(2) 0.0012(19) -0.004(2) -0.007(2) C7 0.086(5) 0.026(2) 0.027(3) 0.000(2) -0.013(3) -0.013(3) C8 0.108(6) 0.026(2) 0.026(3) -0.001(2) -0.006(3) 0.020(3) C9 0.065(4) 0.045(3) 0.028(3) -0.001(2) -0.007(3) 0.026(3) C10 0.037(3) 0.033(2) 0.025(2) 0.0013(19) -0.007(2) 0.012(2) C11 0.027(2) 0.0209(19) 0.025(2) 0.0047(17) -0.0076(19) -0.0004(17) C12 0.035(3) 0.029(2) 0.027(2) 0.0145(19) -0.008(2) -0.005(2) C13 0.035(3) 0.036(3) 0.028(2) 0.0132(19) -0.004(2) -0.009(2) C14 0.019(2) 0.055(3) 0.027(3) 0.014(2) -0.005(2) -0.006(2) C15 0.022(3) 0.076(4) 0.029(3) 0.023(3) -0.004(2) -0.012(3) C16 0.026(3) 0.095(5) 0.026(3) -0.001(3) 0.000(2) 0.001(3) C17 0.026(3) 0.069(4) 0.028(3) -0.007(3) 0.000(2) 0.005(3) C18 0.026(3) 0.047(3) 0.028(3) -0.005(2) 0.003(2) 0.002(2) C22 0.021(2) 0.021(2) 0.028(2) 0.0026(17) -0.0024(19) 0.0032(17) C23 0.020(2) 0.023(2) 0.030(3) 0.0012(18) -0.004(2) -0.0001(17) C24 0.024(2) 0.025(2) 0.017(2) -0.0033(16) -0.0031(18) 0.0030(18) C25 0.017(2) 0.030(2) 0.023(2) 0.0005(17) -0.0015(18) 0.0001(18) C26 0.024(2) 0.030(2) 0.027(2) 0.0006(18) -0.0025(19) -0.0061(19) C27 0.026(3) 0.020(2) 0.030(2) -0.0034(17) -0.0033(19) 0.0025(17) C28 0.022(2) 0.023(2) 0.028(2) -0.0051(17) -0.0014(19) 0.0032(18) C31 0.026(2) 0.022(2) 0.023(2) 0.0004(16) -0.0082(19) -0.0018(17) C32 0.039(3) 0.020(2) 0.026(2) -0.0021(17) -0.012(2) -0.0027(19) C33 0.042(3) 0.027(2) 0.025(2) -0.0021(18) -0.009(2) 0.004(2) C34 0.021(2) 0.029(2) 0.024(3) -0.0032(17) -0.005(2) 0.0025(19) C35 0.026(3) 0.042(3) 0.024(3) -0.008(2) 0.000(2) 0.003(2) C36 0.027(3) 0.056(3) 0.027(3) 0.001(2) 0.003(2) 0.001(2) C37 0.024(3) 0.038(3) 0.031(3) 0.006(2) 0.001(2) -0.003(2) C38 0.015(2) 0.031(2) 0.030(2) 0.0003(18) -0.0018(19) -0.0010(18) C42 0.027(3) 0.019(2) 0.034(3) -0.0003(18) -0.008(2) -0.0031(18) C43 0.025(3) 0.023(2) 0.033(3) -0.0005(18) -0.010(2) 0.0004(19) C44 0.022(2) 0.022(2) 0.024(2) 0.0039(17) -0.0035(19) 0.0002(17) C45 0.025(3) 0.029(2) 0.031(3) -0.0027(18) -0.005(2) 0.0032(19) C46 0.030(3) 0.034(2) 0.024(2) -0.0029(19) -0.002(2) 0.010(2) C47 0.037(3) 0.022(2) 0.021(2) -0.0008(16) -0.004(2) 0.0012(19) C48 0.028(3) 0.022(2) 0.023(2) -0.0020(16) -0.0009(19) -0.0055(18) N70 0.025(2) 0.0271(19) 0.029(2) 0.0011(16) -0.0070(17) -0.0066(17) C70 0.032(3) 0.039(3) 0.033(3) -0.003(2) -0.001(2) -0.004(2) C71 0.055(4) 0.075(4) 0.062(4) 0.001(3) -0.011(3) -0.039(4) N80 0.025(2) 0.0275(19) 0.023(2) -0.0018(15) -0.0041(17) 0.0032(17) C80 0.028(3) 0.029(2) 0.024(2) -0.0003(18) 0.002(2) -0.005(2) C81 0.030(3) 0.029(2) 0.048(3) 0.008(2) -0.008(2) -0.004(2) N60 0.026(2) 0.034(2) 0.032(2) 0.0036(17) -0.0010(18) -0.0060(18) C60 0.031(3) 0.044(3) 0.028(3) -0.003(2) 0.006(2) -0.002(2) C61 0.028(3) 0.071(4) 0.058(4) -0.028(3) 0.012(3) -0.022(3) N50 0.022(2) 0.034(2) 0.023(2) -0.0013(15) -0.0012(16) 0.0011(18) C50 0.033(3) 0.042(3) 0.031(3) 0.001(2) 0.001(2) 0.003(2) C51 0.028(3) 0.062(4) 0.062(4) -0.002(3) 0.002(3) 0.019(3) Cl1 0.0277(6) 0.0258(5) 0.0264(6) 0.0005(4) -0.0019(5) 0.0002(4) O11 0.046(2) 0.0270(17) 0.0339(19) 0.0084(14) 0.0066(17) 0.0009(15) O12 0.043(2) 0.0320(19) 0.059(2) 0.0002(17) 0.0123(19) 0.0074(16) O13 0.034(2) 0.065(2) 0.033(2) -0.0009(17) -0.0107(16) -0.0117(18) O14 0.044(2) 0.0280(16) 0.0211(16) 0.0015(12) -0.0003(15) -0.0038(15) Cl2 0.0327(7) 0.0414(6) 0.0373(7) 0.0019(5) -0.0018(5) 0.0009(5) O21 0.044(3) 0.115(4) 0.057(3) 0.018(3) -0.016(2) -0.029(3) O22 0.049(2) 0.0352(18) 0.0321(19) 0.0032(14) 0.0022(17) -0.0013(16) O23 0.089(4) 0.085(4) 0.080(4) -0.043(3) -0.026(3) 0.041(3) O24 0.052(3) 0.086(3) 0.052(3) 0.027(2) 0.006(2) -0.018(2) Cl3 0.0363(8) 0.0308(6) 0.0796(11) -0.0127(6) -0.0007(7) 0.0042(5) O31 0.040(3) 0.147(6) 0.113(5) -0.066(4) 0.013(3) 0.014(3) O32 0.053(3) 0.051(2) 0.078(3) -0.004(2) -0.009(2) 0.017(2) O33 0.152(6) 0.027(2) 0.170(6) 0.005(3) -0.052(5) -0.024(3) O34 0.070(3) 0.040(2) 0.060(3) -0.0007(19) 0.000(2) -0.004(2) Cl4 0.0470(9) 0.0229(6) 0.0803(11) 0.0040(6) -0.0142(8) -0.0028(5) O41 0.046(2) 0.0331(18) 0.059(2) -0.0052(16) -0.0108(19) -0.0026(16) O42 0.205(14) 0.103(8) 0.144(10) 0.018(7) 0.079(10) -0.052(8) O43 0.061(6) 0.036(3) 0.124(7) 0.002(4) -0.050(5) -0.012(4) O44 0.054(6) 0.043(5) 0.229(15) -0.008(7) -0.050(8) 0.008(4) O45 0.061(6) 0.036(3) 0.124(7) 0.002(4) -0.050(5) -0.012(4) O46 0.205(14) 0.103(8) 0.144(10) 0.018(7) 0.079(10) -0.052(8) O47 0.054(6) 0.043(5) 0.229(15) -0.008(7) -0.050(8) 0.008(4) N90 0.070(4) 0.057(3) 0.054(3) 0.000(2) -0.001(3) -0.016(3) C90 0.062(5) 0.065(4) 0.039(3) 0.000(3) 0.005(3) 0.002(4) C91 0.072(5) 0.073(5) 0.075(5) -0.017(4) -0.006(4) -0.005(4) N100 0.021(5) 0.134(11) 0.076(8) -0.044(8) 0.027(5) -0.034(7) C100 0.037(7) 0.080(9) 0.052(8) -0.026(7) -0.004(6) 0.021(7) C101 0.052(7) 0.045(6) 0.043(6) -0.008(5) -0.017(5) 0.030(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N13 2.062(4) . y Ni1 N50 2.074(4) . y Ni1 N12 2.098(4) . y Ni1 N14 2.123(4) . y Ni1 N11 2.208(4) . y Ni1 N60 2.212(4) . y Ni2 N70 2.084(4) . y Ni2 N17 2.086(4) . y Ni2 N16 2.091(3) . y Ni2 N18 2.123(4) . y Ni2 N80 2.188(4) . y Ni2 N15 2.214(3) . y N11 C4 1.348(6) . ? N11 C1 1.356(5) . ? N12 C11 1.491(5) . ? N12 C12 1.503(5) . ? N12 C22 1.511(6) . ? N13 C14 1.356(6) . ? N13 C18 1.371(6) . ? N14 C28 1.345(5) . ? N14 C24 1.367(6) . ? N15 C3 1.348(5) . ? N15 C4 1.350(6) . ? N16 C42 1.487(6) . ? N16 C31 1.504(5) . ? N16 C32 1.510(6) . ? N17 C34 1.344(6) . ? N17 C38 1.351(6) . ? N18 C44 1.356(6) . ? N18 C48 1.366(5) . ? C1 C2 1.380(6) . ? C1 C11 1.503(5) . ? C2 C3 1.373(6) . ? C2 H2 0.9500 . ? C3 C31 1.504(6) . ? C4 C5 1.478(6) . ? C5 C6 1.368(7) . ? C5 C10 1.418(7) . ? C6 C7 1.401(7) . ? C6 H6 0.9500 . ? C7 C8 1.385(9) . ? C7 H7 0.9500 . ? C8 C9 1.390(9) . ? C8 H8 0.9500 . ? C9 C10 1.377(7) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.513(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.476(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.413(7) . ? C15 C16 1.381(9) . ? C15 H15 0.9500 . ? C16 C17 1.382(9) . ? C16 H16 0.9500 . ? C17 C18 1.381(7) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C22 C23 1.525(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.503(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.386(6) . ? C25 C26 1.378(6) . ? C25 H25 0.9500 . ? C26 C27 1.383(6) . ? C26 H26 0.9500 . ? C27 C28 1.380(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.513(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.500(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.407(7) . ? C35 C36 1.367(7) . ? C35 H35 0.9500 . ? C36 C37 1.380(7) . ? C36 H36 0.9500 . ? C37 C38 1.373(6) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C42 C43 1.517(6) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.497(6) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.384(6) . ? C45 C46 1.402(7) . ? C45 H45 0.9500 . ? C46 C47 1.381(7) . ? C46 H46 0.9500 . ? C47 C48 1.357(6) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? N70 C70 1.130(6) . ? C70 C71 1.474(7) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? N80 C80 1.137(6) . ? C80 C81 1.469(7) . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? N60 C60 1.124(6) . ? C60 C61 1.474(7) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? N50 C50 1.118(6) . ? C50 C51 1.474(7) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? Cl1 O11 1.435(3) . ? Cl1 O12 1.439(4) . ? Cl1 O13 1.443(3) . ? Cl1 O14 1.449(3) . ? Cl2 O21 1.404(4) . ? Cl2 O23 1.426(5) . ? Cl2 O24 1.431(4) . ? Cl2 O22 1.436(4) . ? Cl3 O33 1.419(5) . ? Cl3 O31 1.423(6) . ? Cl3 O34 1.424(5) . ? Cl3 O32 1.433(4) . ? Cl4 O43 1.365(9) . ? Cl4 O45 1.385(8) . ? Cl4 O47 1.397(10) . ? Cl4 O44 1.397(10) . ? Cl4 O41 1.417(4) . ? Cl4 O46 1.506(11) . ? Cl4 O42 1.521(11) . ? N90 C90 1.106(8) . ? C90 C91 1.473(10) . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? N100 C100 1.090(18) . ? C100 C101 1.47(2) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N13 Ni1 N50 90.39(16) . . y N13 Ni1 N12 92.15(15) . . y N50 Ni1 N12 170.88(14) . . y N13 Ni1 N14 92.71(15) . . y N50 Ni1 N14 92.92(13) . . y N12 Ni1 N14 95.71(14) . . y N13 Ni1 N11 166.71(14) . . y N50 Ni1 N11 97.13(14) . . y N12 Ni1 N11 78.79(13) . . y N14 Ni1 N11 97.81(13) . . y N13 Ni1 N60 88.53(16) . . y N50 Ni1 N60 79.64(15) . . y N12 Ni1 N60 91.67(15) . . y N14 Ni1 N60 172.46(15) . . y N11 Ni1 N60 82.09(14) . . y N70 Ni2 N17 92.24(15) . . y N70 Ni2 N16 169.06(14) . . y N17 Ni2 N16 93.63(14) . . y N70 Ni2 N18 93.54(14) . . y N17 Ni2 N18 92.08(15) . . y N16 Ni2 N18 95.46(14) . . y N70 Ni2 N80 79.03(15) . . y N17 Ni2 N80 89.19(14) . . y N16 Ni2 N80 91.83(15) . . y N18 Ni2 N80 172.51(14) . . y N70 Ni2 N15 95.97(14) . . y N17 Ni2 N15 166.45(13) . . y N16 Ni2 N15 76.62(13) . . y N18 Ni2 N15 98.13(14) . . y N80 Ni2 N15 81.84(13) . . y C4 N11 C1 117.4(4) . . ? C4 N11 Ni1 133.3(3) . . y C1 N11 Ni1 107.5(3) . . ? C11 N12 C12 108.6(3) . . ? C11 N12 C22 106.1(3) . . ? C12 N12 C22 108.6(3) . . ? C11 N12 Ni1 104.6(2) . . ? C12 N12 Ni1 116.2(3) . . ? C22 N12 Ni1 112.1(2) . . ? C14 N13 C18 118.9(5) . . ? C14 N13 Ni1 122.8(3) . . ? C18 N13 Ni1 118.0(3) . . ? C28 N14 C24 115.8(4) . . ? C28 N14 Ni1 118.9(3) . . ? C24 N14 Ni1 125.2(3) . . ? C3 N15 C4 118.2(4) . . ? C3 N15 Ni2 106.4(3) . . ? C4 N15 Ni2 132.8(3) . . y C42 N16 C31 106.9(3) . . ? C42 N16 C32 109.3(3) . . ? C31 N16 C32 107.5(3) . . ? C42 N16 Ni2 112.1(3) . . ? C31 N16 Ni2 104.8(2) . . ? C32 N16 Ni2 115.8(3) . . ? C34 N17 C38 118.9(4) . . ? C34 N17 Ni2 122.3(3) . . ? C38 N17 Ni2 118.4(3) . . ? C44 N18 C48 116.9(4) . . ? C44 N18 Ni2 125.6(3) . . ? C48 N18 Ni2 117.5(3) . . ? N11 C1 C2 121.4(4) . . ? N11 C1 C11 118.0(4) . . ? C2 C1 C11 120.5(4) . . ? C3 C2 C1 118.0(4) . . ? C3 C2 H2 121.0 . . ? C1 C2 H2 121.0 . . ? N15 C3 C2 121.0(4) . . ? N15 C3 C31 117.5(4) . . ? C2 C3 C31 121.6(4) . . ? N11 C4 N15 123.4(4) . . ? N11 C4 C5 119.7(4) . . ? N15 C4 C5 116.8(4) . . ? C6 C5 C10 119.7(4) . . ? C6 C5 C4 123.0(4) . . ? C10 C5 C4 117.3(4) . . ? C5 C6 C7 119.8(5) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C8 C7 C6 120.1(5) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 120.5(5) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 119.3(5) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C5 120.5(5) . . ? C9 C10 H10 119.8 . . ? C5 C10 H10 119.8 . . ? N12 C11 C1 111.8(3) . . ? N12 C11 H11A 109.2 . . ? C1 C11 H11A 109.2 . . ? N12 C11 H11B 109.2 . . ? C1 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N12 C12 C13 115.0(4) . . ? N12 C12 H12A 108.5 . . ? C13 C12 H12A 108.5 . . ? N12 C12 H12B 108.5 . . ? C13 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? C14 C13 C12 113.2(4) . . ? C14 C13 H13A 108.9 . . ? C12 C13 H13A 108.9 . . ? C14 C13 H13B 108.9 . . ? C12 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? N13 C14 C15 119.4(5) . . ? N13 C14 C13 119.5(4) . . ? C15 C14 C13 121.1(5) . . ? C16 C15 C14 121.6(5) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C15 C16 C17 117.7(5) . . ? C15 C16 H16 121.1 . . ? C17 C16 H16 121.1 . . ? C18 C17 C16 119.9(6) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? N13 C18 C17 122.3(5) . . ? N13 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? N12 C22 C23 113.1(4) . . ? N12 C22 H22A 109.0 . . ? C23 C22 H22A 109.0 . . ? N12 C22 H22B 109.0 . . ? C23 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C24 C23 C22 115.5(4) . . ? C24 C23 H23A 108.4 . . ? C22 C23 H23A 108.4 . . ? C24 C23 H23B 108.4 . . ? C22 C23 H23B 108.4 . . ? H23A C23 H23B 107.5 . . ? N14 C24 C25 122.1(4) . . ? N14 C24 C23 119.0(4) . . ? C25 C24 C23 118.9(4) . . ? C26 C25 C24 120.7(4) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 117.7(4) . . ? C25 C26 H26 121.2 . . ? C27 C26 H26 121.2 . . ? C28 C27 C26 118.8(4) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? N14 C28 C27 124.8(4) . . ? N14 C28 H28 117.6 . . ? C27 C28 H28 117.6 . . ? N16 C31 C3 110.4(3) . . ? N16 C31 H31A 109.6 . . ? C3 C31 H31A 109.6 . . ? N16 C31 H31B 109.6 . . ? C3 C31 H31B 109.6 . . ? H31A C31 H31B 108.1 . . ? N16 C32 C33 114.4(4) . . ? N16 C32 H32A 108.7 . . ? C33 C32 H32A 108.7 . . ? N16 C32 H32B 108.7 . . ? C33 C32 H32B 108.7 . . ? H32A C32 H32B 107.6 . . ? C34 C33 C32 115.2(4) . . ? C34 C33 H33A 108.5 . . ? C32 C33 H33A 108.5 . . ? C34 C33 H33B 108.5 . . ? C32 C33 H33B 108.5 . . ? H33A C33 H33B 107.5 . . ? N17 C34 C35 120.2(4) . . ? N17 C34 C33 119.0(4) . . ? C35 C34 C33 120.7(4) . . ? C36 C35 C34 120.2(4) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C37 119.0(5) . . ? C35 C36 H36 120.5 . . ? C37 C36 H36 120.5 . . ? C38 C37 C36 118.8(5) . . ? C38 C37 H37 120.6 . . ? C36 C37 H37 120.6 . . ? N17 C38 C37 122.8(4) . . ? N17 C38 H38 118.6 . . ? C37 C38 H38 118.6 . . ? N16 C42 C43 114.4(4) . . ? N16 C42 H42A 108.7 . . ? C43 C42 H42A 108.7 . . ? N16 C42 H42B 108.7 . . ? C43 C42 H42B 108.7 . . ? H42A C42 H42B 107.6 . . ? C44 C43 C42 117.9(4) . . ? C44 C43 H43A 107.8 . . ? C42 C43 H43A 107.8 . . ? C44 C43 H43B 107.8 . . ? C42 C43 H43B 107.8 . . ? H43A C43 H43B 107.2 . . ? N18 C44 C45 121.7(4) . . ? N18 C44 C43 119.3(4) . . ? C45 C44 C43 118.9(4) . . ? C44 C45 C46 120.0(4) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C47 C46 C45 117.8(4) . . ? C47 C46 H46 121.1 . . ? C45 C46 H46 121.1 . . ? C48 C47 C46 119.5(4) . . ? C48 C47 H47 120.2 . . ? C46 C47 H47 120.2 . . ? C47 C48 N18 123.9(4) . . ? C47 C48 H48 118.0 . . ? N18 C48 H48 118.0 . . ? C70 N70 Ni2 174.9(4) . . ? N70 C70 C71 178.4(6) . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C80 N80 Ni2 166.5(4) . . ? N80 C80 C81 177.8(5) . . ? C80 C81 H81A 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C80 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C60 N60 Ni1 176.8(4) . . ? N60 C60 C61 176.5(6) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C50 N50 Ni1 170.4(4) . . ? N50 C50 C51 179.3(6) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O11 Cl1 O12 110.3(2) . . ? O11 Cl1 O13 109.9(2) . . ? O12 Cl1 O13 109.3(2) . . ? O11 Cl1 O14 108.8(2) . . ? O12 Cl1 O14 109.0(2) . . ? O13 Cl1 O14 109.4(2) . . ? O21 Cl2 O23 110.2(3) . . ? O21 Cl2 O24 109.2(3) . . ? O23 Cl2 O24 107.9(4) . . ? O21 Cl2 O22 110.1(3) . . ? O23 Cl2 O22 109.0(3) . . ? O24 Cl2 O22 110.4(3) . . ? O33 Cl3 O31 109.0(4) . . ? O33 Cl3 O34 110.8(4) . . ? O31 Cl3 O34 108.9(3) . . ? O33 Cl3 O32 108.8(3) . . ? O31 Cl3 O32 109.4(4) . . ? O34 Cl3 O32 109.9(3) . . ? O43 Cl4 O45 122.5(6) . . ? O43 Cl4 O47 36.1(7) . . ? O45 Cl4 O47 118.9(8) . . ? O43 Cl4 O44 110.2(7) . . ? O45 Cl4 O44 46.5(7) . . ? O47 Cl4 O44 137.6(7) . . ? O43 Cl4 O41 122.2(4) . . ? O45 Cl4 O41 115.1(4) . . ? O47 Cl4 O41 109.6(5) . . ? O44 Cl4 O41 112.0(5) . . ? O43 Cl4 O46 66.7(8) . . ? O45 Cl4 O46 110.6(9) . . ? O47 Cl4 O46 101.6(10) . . ? O44 Cl4 O46 65.1(9) . . ? O41 Cl4 O46 98.2(6) . . ? O43 Cl4 O42 99.0(8) . . ? O45 Cl4 O42 66.8(9) . . ? O47 Cl4 O42 67.0(10) . . ? O44 Cl4 O42 113.1(10) . . ? O41 Cl4 O42 98.8(6) . . ? O46 Cl4 O42 162.0(8) . . ? N90 C90 C91 176.2(8) . . ? C90 C91 H91A 109.5 . . ? C90 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C90 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? N100 C100 C101 176.9(14) . . ? C100 C101 H10A 109.5 . . ? C100 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C100 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N13 Ni1 N11 C4 146.0(6) . . . . ? N50 Ni1 N11 C4 22.0(4) . . . . ? N12 Ni1 N11 C4 -166.3(4) . . . . ? N14 Ni1 N11 C4 -72.0(4) . . . . ? N60 Ni1 N11 C4 100.4(4) . . . . ? N13 Ni1 N11 C1 -18.4(8) . . . . ? N50 Ni1 N11 C1 -142.4(3) . . . . ? N12 Ni1 N11 C1 29.3(3) . . . . ? N14 Ni1 N11 C1 123.6(3) . . . . ? N60 Ni1 N11 C1 -64.0(3) . . . . ? N13 Ni1 N12 C11 132.4(3) . . . . ? N14 Ni1 N12 C11 -134.6(3) . . . . ? N11 Ni1 N12 C11 -37.8(3) . . . . ? N60 Ni1 N12 C11 43.8(3) . . . . ? N13 Ni1 N12 C12 12.7(3) . . . . ? N14 Ni1 N12 C12 105.7(3) . . . . ? N11 Ni1 N12 C12 -157.4(3) . . . . ? N60 Ni1 N12 C12 -75.8(3) . . . . ? N13 Ni1 N12 C22 -113.0(3) . . . . ? N14 Ni1 N12 C22 -20.1(3) . . . . ? N11 Ni1 N12 C22 76.8(3) . . . . ? N60 Ni1 N12 C22 158.4(3) . . . . ? N50 Ni1 N13 C14 134.9(4) . . . . ? N12 Ni1 N13 C14 -36.3(4) . . . . ? N14 Ni1 N13 C14 -132.1(4) . . . . ? N11 Ni1 N13 C14 10.3(9) . . . . ? N60 Ni1 N13 C14 55.3(4) . . . . ? N50 Ni1 N13 C18 -38.6(4) . . . . ? N12 Ni1 N13 C18 150.1(4) . . . . ? N14 Ni1 N13 C18 54.3(4) . . . . ? N11 Ni1 N13 C18 -163.3(5) . . . . ? N60 Ni1 N13 C18 -118.3(4) . . . . ? N13 Ni1 N14 C28 -95.2(3) . . . . ? N50 Ni1 N14 C28 -4.7(3) . . . . ? N12 Ni1 N14 C28 172.3(3) . . . . ? N11 Ni1 N14 C28 92.9(3) . . . . ? N13 Ni1 N14 C24 89.8(4) . . . . ? N50 Ni1 N14 C24 -179.6(3) . . . . ? N12 Ni1 N14 C24 -2.6(4) . . . . ? N11 Ni1 N14 C24 -82.0(3) . . . . ? N70 Ni2 N15 C3 -134.2(3) . . . . ? N17 Ni2 N15 C3 -7.2(7) . . . . ? N16 Ni2 N15 C3 37.6(3) . . . . ? N18 Ni2 N15 C3 131.3(3) . . . . ? N80 Ni2 N15 C3 -56.2(3) . . . . ? N70 Ni2 N15 C4 26.6(4) . . . . ? N17 Ni2 N15 C4 153.6(5) . . . . ? N16 Ni2 N15 C4 -161.6(4) . . . . ? N18 Ni2 N15 C4 -67.8(4) . . . . ? N80 Ni2 N15 C4 104.6(4) . . . . ? N70 Ni2 N16 C42 121.7(8) . . . . ? N17 Ni2 N16 C42 -116.0(3) . . . . ? N18 Ni2 N16 C42 -23.5(3) . . . . ? N80 Ni2 N16 C42 154.7(3) . . . . ? N15 Ni2 N16 C42 73.5(3) . . . . ? N70 Ni2 N16 C31 6.1(10) . . . . ? N17 Ni2 N16 C31 128.4(3) . . . . ? N18 Ni2 N16 C31 -139.1(3) . . . . ? N80 Ni2 N16 C31 39.1(3) . . . . ? N15 Ni2 N16 C31 -42.1(3) . . . . ? N70 Ni2 N16 C32 -112.0(8) . . . . ? N17 Ni2 N16 C32 10.3(3) . . . . ? N18 Ni2 N16 C32 102.7(3) . . . . ? N80 Ni2 N16 C32 -79.0(3) . . . . ? N15 Ni2 N16 C32 -160.2(3) . . . . ? N70 Ni2 N17 C34 135.7(4) . . . . ? N16 Ni2 N17 C34 -35.1(4) . . . . ? N18 Ni2 N17 C34 -130.7(4) . . . . ? N80 Ni2 N17 C34 56.7(4) . . . . ? N15 Ni2 N17 C34 8.3(8) . . . . ? N70 Ni2 N17 C38 -37.2(3) . . . . ? N16 Ni2 N17 C38 152.0(3) . . . . ? N18 Ni2 N17 C38 56.4(3) . . . . ? N80 Ni2 N17 C38 -116.2(3) . . . . ? N15 Ni2 N17 C38 -164.6(5) . . . . ? N70 Ni2 N18 C44 -173.3(4) . . . . ? N17 Ni2 N18 C44 94.4(4) . . . . ? N16 Ni2 N18 C44 0.5(4) . . . . ? N15 Ni2 N18 C44 -76.7(4) . . . . ? N70 Ni2 N18 C48 4.8(3) . . . . ? N17 Ni2 N18 C48 -87.6(3) . . . . ? N16 Ni2 N18 C48 178.6(3) . . . . ? N15 Ni2 N18 C48 101.3(3) . . . . ? C4 N11 C1 C2 -5.3(6) . . . . ? Ni1 N11 C1 C2 162.0(3) . . . . ? C4 N11 C1 C11 179.3(4) . . . . ? Ni1 N11 C1 C11 -13.5(4) . . . . ? N11 C1 C2 C3 2.7(7) . . . . ? C11 C1 C2 C3 178.0(4) . . . . ? C4 N15 C3 C2 -8.4(6) . . . . ? Ni2 N15 C3 C2 155.7(4) . . . . ? C4 N15 C3 C31 171.7(4) . . . . ? Ni2 N15 C3 C31 -24.1(5) . . . . ? C1 C2 C3 N15 4.4(7) . . . . ? C1 C2 C3 C31 -175.8(4) . . . . ? C1 N11 C4 N15 1.0(7) . . . . ? Ni1 N11 C4 N15 -162.2(3) . . . . ? C1 N11 C4 C5 178.1(4) . . . . ? Ni1 N11 C4 C5 14.8(7) . . . . ? C3 N15 C4 N11 5.8(7) . . . . ? Ni2 N15 C4 N11 -153.3(3) . . . . ? C3 N15 C4 C5 -171.3(4) . . . . ? Ni2 N15 C4 C5 29.6(6) . . . . ? N11 C4 C5 C6 73.7(6) . . . . ? N15 C4 C5 C6 -109.1(5) . . . . ? N11 C4 C5 C10 -105.9(5) . . . . ? N15 C4 C5 C10 71.3(6) . . . . ? C10 C5 C6 C7 -1.3(7) . . . . ? C4 C5 C6 C7 179.0(4) . . . . ? C5 C6 C7 C8 2.4(8) . . . . ? C6 C7 C8 C9 -1.4(8) . . . . ? C7 C8 C9 C10 -0.7(8) . . . . ? C8 C9 C10 C5 1.8(7) . . . . ? C6 C5 C10 C9 -0.8(7) . . . . ? C4 C5 C10 C9 178.9(4) . . . . ? C12 N12 C11 C1 166.9(4) . . . . ? C22 N12 C11 C1 -76.5(4) . . . . ? Ni1 N12 C11 C1 42.2(4) . . . . ? N11 C1 C11 N12 -19.2(6) . . . . ? C2 C1 C11 N12 165.3(4) . . . . ? C11 N12 C12 C13 -84.4(5) . . . . ? C22 N12 C12 C13 160.6(4) . . . . ? Ni1 N12 C12 C13 33.1(5) . . . . ? N12 C12 C13 C14 -73.7(5) . . . . ? C18 N13 C14 C15 3.6(7) . . . . ? Ni1 N13 C14 C15 -169.9(3) . . . . ? C18 N13 C14 C13 -176.7(4) . . . . ? Ni1 N13 C14 C13 9.8(6) . . . . ? C12 C13 C14 N13 49.3(6) . . . . ? C12 C13 C14 C15 -130.9(5) . . . . ? N13 C14 C15 C16 -3.1(7) . . . . ? C13 C14 C15 C16 177.2(5) . . . . ? C14 C15 C16 C17 1.1(8) . . . . ? C15 C16 C17 C18 0.2(8) . . . . ? C14 N13 C18 C17 -2.3(7) . . . . ? Ni1 N13 C18 C17 171.5(4) . . . . ? C16 C17 C18 N13 0.4(8) . . . . ? C11 N12 C22 C23 171.6(3) . . . . ? C12 N12 C22 C23 -71.7(4) . . . . ? Ni1 N12 C22 C23 58.0(4) . . . . ? N12 C22 C23 C24 -78.7(5) . . . . ? C28 N14 C24 C25 -3.9(6) . . . . ? Ni1 N14 C24 C25 171.2(3) . . . . ? C28 N14 C24 C23 174.4(4) . . . . ? Ni1 N14 C24 C23 -10.5(5) . . . . ? C22 C23 C24 N14 49.6(6) . . . . ? C22 C23 C24 C25 -132.1(4) . . . . ? N14 C24 C25 C26 1.8(6) . . . . ? C23 C24 C25 C26 -176.4(4) . . . . ? C24 C25 C26 C27 1.8(6) . . . . ? C25 C26 C27 C28 -3.1(7) . . . . ? C24 N14 C28 C27 2.5(6) . . . . ? Ni1 N14 C28 C27 -172.9(4) . . . . ? C26 C27 C28 N14 1.0(7) . . . . ? C42 N16 C31 C3 -77.0(4) . . . . ? C32 N16 C31 C3 165.8(4) . . . . ? Ni2 N16 C31 C3 42.2(4) . . . . ? N15 C3 C31 N16 -11.0(6) . . . . ? C2 C3 C31 N16 169.2(4) . . . . ? C42 N16 C32 C33 162.4(3) . . . . ? C31 N16 C32 C33 -82.0(4) . . . . ? Ni2 N16 C32 C33 34.7(4) . . . . ? N16 C32 C33 C34 -73.7(5) . . . . ? C38 N17 C34 C35 2.2(6) . . . . ? Ni2 N17 C34 C35 -170.7(3) . . . . ? C38 N17 C34 C33 -176.3(4) . . . . ? Ni2 N17 C34 C33 10.8(6) . . . . ? C32 C33 C34 N17 47.5(6) . . . . ? C32 C33 C34 C35 -131.0(4) . . . . ? N17 C34 C35 C36 -0.4(7) . . . . ? C33 C34 C35 C36 178.1(5) . . . . ? C34 C35 C36 C37 -2.0(7) . . . . ? C35 C36 C37 C38 2.6(7) . . . . ? C34 N17 C38 C37 -1.6(6) . . . . ? Ni2 N17 C38 C37 171.5(3) . . . . ? C36 C37 C38 N17 -0.8(7) . . . . ? C31 N16 C42 C43 173.0(3) . . . . ? C32 N16 C42 C43 -71.0(4) . . . . ? Ni2 N16 C42 C43 58.7(4) . . . . ? N16 C42 C43 C44 -74.4(6) . . . . ? C48 N18 C44 C45 -3.8(6) . . . . ? Ni2 N18 C44 C45 174.3(3) . . . . ? C48 N18 C44 C43 172.5(4) . . . . ? Ni2 N18 C44 C43 -9.5(6) . . . . ? C42 C43 C44 N18 44.1(7) . . . . ? C42 C43 C44 C45 -139.6(5) . . . . ? N18 C44 C45 C46 4.1(7) . . . . ? C43 C44 C45 C46 -172.1(4) . . . . ? C44 C45 C46 C47 -1.2(7) . . . . ? C45 C46 C47 C48 -1.9(7) . . . . ? C46 C47 C48 N18 2.3(7) . . . . ? C44 N18 C48 C47 0.5(6) . . . . ? Ni2 N18 C48 C47 -177.7(3) . . . . ? N17 Ni2 N70 C70 -67(4) . . . . ? N16 Ni2 N70 C70 55(5) . . . . ? N18 Ni2 N70 C70 -159(4) . . . . ? N80 Ni2 N70 C70 22(4) . . . . ? N15 Ni2 N70 C70 102(4) . . . . ? Ni2 N70 C70 C71 -164(18) . . . . ? N70 Ni2 N80 C80 80.6(15) . . . . ? N17 Ni2 N80 C80 173.1(15) . . . . ? N16 Ni2 N80 C80 -93.3(15) . . . . ? N18 Ni2 N80 C80 73(2) . . . . ? N15 Ni2 N80 C80 -17.1(15) . . . . ? Ni2 N80 C80 C81 64(14) . . . . ? N13 Ni1 N60 C60 154(8) . . . . ? N50 Ni1 N60 C60 63(8) . . . . ? N12 Ni1 N60 C60 -114(8) . . . . ? N14 Ni1 N60 C60 54(8) . . . . ? N11 Ni1 N60 C60 -36(8) . . . . ? Ni1 N60 C60 C61 158(6) . . . . ? N13 Ni1 N50 C50 -53(2) . . . . ? N12 Ni1 N50 C50 53(3) . . . . ? N14 Ni1 N50 C50 -145(2) . . . . ? N11 Ni1 N50 C50 116(2) . . . . ? N60 Ni1 N50 C50 36(2) . . . . ? Ni1 N50 C50 C51 -101(60) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.698 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.079 # Attachment 'wag164r.cif' data_wag164r _database_code_depnum_ccdc_archive 'CCDC 842530' #TrackingRef 'wag164r.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H71 Cl4 Mn2 N13 O19' _chemical_formula_weight 1457.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 23.512(3) _cell_length_b 21.394(3) _cell_length_c 13.4375(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6759.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 91(2) _cell_measurement_reflns_used 3830 _cell_measurement_theta_min 2.575 _cell_measurement_theta_max 21.36 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3024 _exptl_absorpt_coefficient_mu 0.609 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8384 _exptl_absorpt_correction_T_max 0.9416 _exptl_absorpt_process_details 'SCALE (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 91(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65095 _diffrn_reflns_av_R_equivalents 0.1470 _diffrn_reflns_av_sigmaI/netI 0.0972 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.575 _diffrn_reflns_theta_max 21.36 _reflns_number_total 6804 _reflns_number_gt 3782 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+49.7631P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0026(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6804 _refine_ls_number_parameters 478 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1746 _refine_ls_R_factor_gt 0.0966 _refine_ls_wR_factor_ref 0.2464 _refine_ls_wR_factor_gt 0.2135 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.11767(4) 0.59296(6) 0.77736(8) 0.0359(4) Uani 1 1 d . . . N11 N 0.0971(2) 0.6942(3) 0.7269(4) 0.0314(14) Uani 1 1 d . . . C1 C 0.0684(3) 0.6945(4) 0.6391(5) 0.0334(18) Uani 1 1 d . . . C2 C 0.0528(4) 0.7500 0.5948(7) 0.029(2) Uani 1 2 d S . . H2 H 0.0316 0.7500 0.5347 0.035 Uiso 1 2 calc SR . . C4 C 0.1092(3) 0.7500 0.7672(7) 0.026(2) Uani 1 2 d S . . C5 C 0.1375(4) 0.7500 0.8678(7) 0.029(2) Uani 1 2 d S . . C6 C 0.1060(4) 0.7500 0.9517(7) 0.042(3) Uani 1 2 d S . . H6 H 0.0656 0.7500 0.9470 0.050 Uiso 1 2 calc SR . . C7 C 0.1313(5) 0.7500 1.0437(9) 0.057(4) Uani 1 2 d S . . H7 H 0.1080 0.7500 1.1015 0.069 Uiso 1 2 calc SR . . C8 C 0.1877(5) 0.7500 1.0539(8) 0.046(3) Uani 1 2 d S . . H8 H 0.2045 0.7500 1.1182 0.055 Uiso 1 2 calc SR . . C9 C 0.2205(5) 0.7500 0.9721(10) 0.069(4) Uani 1 2 d SU . . H9 H 0.2607 0.7500 0.9789 0.082 Uiso 1 2 calc SR . . C10 C 0.1960(5) 0.7500 0.8752(10) 0.082(5) Uani 1 2 d SU . . H10 H 0.2193 0.7500 0.8174 0.098 Uiso 1 2 calc SR . . C11 C 0.0551(3) 0.6331(4) 0.5920(5) 0.040(2) Uani 1 1 d . . . H11A H 0.0212 0.6378 0.5490 0.048 Uiso 1 1 calc R . . H11B H 0.0874 0.6203 0.5492 0.048 Uiso 1 1 calc R . . N12 N 0.0443(2) 0.5838(3) 0.6664(4) 0.0389(16) Uani 1 1 d . . . C12 C 0.0405(3) 0.5234(4) 0.6120(6) 0.051(2) Uani 1 1 d . . . H12A H 0.0219 0.5313 0.5471 0.061 Uiso 1 1 calc R . . H12B H 0.0155 0.4951 0.6502 0.061 Uiso 1 1 calc R . . C13 C 0.0972(4) 0.4893(5) 0.5924(6) 0.053(2) Uani 1 1 d . . . H13A H 0.0915 0.4584 0.5384 0.064 Uiso 1 1 calc R . . H13B H 0.1257 0.5200 0.5694 0.064 Uiso 1 1 calc R . . C14 C 0.1198(3) 0.4563(4) 0.6819(6) 0.0418(19) Uani 1 1 d . . . C15 C 0.1307(3) 0.3932(5) 0.6793(7) 0.057(3) Uani 1 1 d . . . H15 H 0.1226 0.3703 0.6204 0.068 Uiso 1 1 calc R . . C16 C 0.1532(4) 0.3620(4) 0.7612(7) 0.055(2) Uani 1 1 d . . . H16 H 0.1611 0.3185 0.7582 0.066 Uiso 1 1 calc R . . C17 C 0.1639(3) 0.3958(4) 0.8475(7) 0.047(2) Uani 1 1 d . . . H17 H 0.1792 0.3764 0.9052 0.057 Uiso 1 1 calc R . . C18 C 0.1515(3) 0.4593(4) 0.8459(6) 0.042(2) Uani 1 1 d . . . H18 H 0.1580 0.4828 0.9048 0.050 Uiso 1 1 calc R . . N13 N 0.1307(2) 0.4895(3) 0.7656(5) 0.0360(15) Uani 1 1 d . . . C22 C -0.0109(3) 0.5968(5) 0.7146(5) 0.049(2) Uani 1 1 d . . . H22A H -0.0416 0.5910 0.6650 0.058 Uiso 1 1 calc R . . H22B H -0.0116 0.6411 0.7358 0.058 Uiso 1 1 calc R . . C23 C -0.0237(4) 0.5556(5) 0.8049(6) 0.057(3) Uani 1 1 d . . . H23A H -0.0655 0.5534 0.8129 0.068 Uiso 1 1 calc R . . H23B H -0.0102 0.5128 0.7898 0.068 Uiso 1 1 calc R . . C24 C 0.0015(3) 0.5748(4) 0.9033(6) 0.0353(18) Uani 1 1 d . . . C25 C -0.0322(3) 0.5771(4) 0.9859(6) 0.041(2) Uani 1 1 d . . . H25 H -0.0717 0.5687 0.9804 0.049 Uiso 1 1 calc R . . C26 C -0.0090(3) 0.5914(4) 1.0771(6) 0.046(2) Uani 1 1 d . . . H26 H -0.0325 0.5936 1.1345 0.056 Uiso 1 1 calc R . . C27 C 0.0483(3) 0.6026(4) 1.0841(6) 0.051(2) Uani 1 1 d . . . H27 H 0.0658 0.6105 1.1466 0.061 Uiso 1 1 calc R . . C28 C 0.0798(3) 0.6019(4) 0.9974(5) 0.042(2) Uani 1 1 d . . . H28 H 0.1191 0.6118 1.0015 0.050 Uiso 1 1 calc R . . N14 N 0.0580(2) 0.5879(3) 0.9070(4) 0.0331(14) Uani 1 1 d . . . O40 O 0.1802(2) 0.6039(3) 0.6534(4) 0.0489(15) Uani 1 1 d . . . H40X H 0.1831 0.5771 0.6095 0.059 Uiso 1 1 d . . . H40Y H 0.1855 0.6373 0.6285 0.059 Uiso 1 1 d . . . N50 N 0.1947(3) 0.5991(4) 0.8705(5) 0.056(2) Uani 1 1 d . . . C50 C 0.2395(4) 0.6023(6) 0.8942(6) 0.069(3) Uani 1 1 d . . . C51 C 0.2998(4) 0.6031(6) 0.9253(9) 0.096(4) Uani 1 1 d . . . H51A H 0.3139 0.6462 0.9247 0.115 Uiso 1 1 calc R . . H51B H 0.3224 0.5778 0.8790 0.115 Uiso 1 1 calc R . . H51C H 0.3032 0.5859 0.9926 0.115 Uiso 1 1 calc R . . Cl1 Cl 0.10495(9) 0.2500 0.48427(19) 0.0360(7) Uani 1 2 d S . . O11 O 0.0701(2) 0.3047(3) 0.4870(5) 0.0651(19) Uani 1 1 d . . . O12 O 0.1431(3) 0.2500 0.5675(5) 0.0367(18) Uani 1 2 d S . . O13 O 0.1382(4) 0.2500 0.3952(6) 0.078(3) Uani 1 2 d S . . Cl2 Cl 0.29332(9) 0.49229(15) 0.62713(17) 0.0698(8) Uani 1 1 d . . . O21 O 0.3440(3) 0.5163(5) 0.5938(5) 0.101(3) Uani 1 1 d . . . O22 O 0.2985(3) 0.4230(4) 0.6284(5) 0.091(2) Uani 1 1 d . . . O23 O 0.2773(4) 0.5136(4) 0.7210(6) 0.105(3) Uani 1 1 d . . . O24 O 0.2479(3) 0.5090(4) 0.5591(7) 0.104(3) Uani 1 1 d . . . Cl3 Cl 0.23808(12) 0.7500 0.5426(2) 0.0562(9) Uani 1 2 d S . . O31 O 0.2679(6) 0.7500 0.4609(11) 0.156(7) Uani 1 2 d S . . O32 O 0.1826(5) 0.766(2) 0.5279(10) 0.120(19) Uani 0.50 1 d P . . O33 O 0.2481(10) 0.7867(11) 0.6303(15) 0.116(8) Uani 0.50 1 d P . . O34 O 0.2606(10) 0.6901(9) 0.5682(16) 0.101(7) Uani 0.50 1 d P . . N60 N 0.4158(4) 0.4379(5) 0.8519(6) 0.087(3) Uani 1 1 d D . . C60 C 0.3700(4) 0.4222(5) 0.8582(6) 0.065(3) Uani 1 1 d D . . C61 C 0.3122(4) 0.4000(6) 0.8700(7) 0.076(3) Uani 1 1 d D . . H61A H 0.3118 0.3637 0.9144 0.091 Uiso 1 1 calc R . . H61B H 0.2968 0.3881 0.8049 0.091 Uiso 1 1 calc R . . H61C H 0.2887 0.4334 0.8986 0.091 Uiso 1 1 calc R . . N70 N 0.0223(5) 0.256(3) 0.1754(8) 0.054(8) Uani 0.50 1 d PD A -1 C70 C 0.0675(5) 0.2729(7) 0.1693(11) 0.043(5) Uani 0.50 1 d PD A -1 C71 C 0.1249(7) 0.2960(12) 0.1609(16) 0.092(8) Uani 0.50 1 d PD A -1 H71A H 0.1262 0.3399 0.1816 0.111 Uiso 0.50 1 calc PR A -1 H71B H 0.1376 0.2925 0.0917 0.111 Uiso 0.50 1 calc PR A -1 H71C H 0.1501 0.2713 0.2038 0.111 Uiso 0.50 1 calc PR A -1 C80 C -0.1014(9) 0.2500 0.6858(13) 0.141(9) Uani 1 2 d S . . H80A H -0.1154 0.2899 0.7119 0.169 Uiso 0.50 1 calc PR . . H80B H -0.1154 0.2157 0.7274 0.169 Uiso 0.50 1 calc PR . . H80C H -0.1150 0.2444 0.6174 0.169 Uiso 0.50 1 calc PR . . C81 C -0.0382(6) 0.2500 0.6865(9) 0.082(5) Uani 1 2 d S . . H81A H -0.0238 0.2125 0.6514 0.099 Uiso 0.50 1 calc PR . . H81B H -0.0238 0.2875 0.6514 0.099 Uiso 0.50 1 calc PR . . O82 O -0.0189(4) 0.2500 0.7855(6) 0.071(3) Uani 1 2 d S . . C83 C 0.0379(6) 0.2500 0.7926(11) 0.085(5) Uani 1 2 d S . . H83A H 0.0532 0.2874 0.7586 0.102 Uiso 0.50 1 calc PR . . H83B H 0.0532 0.2126 0.7586 0.102 Uiso 0.50 1 calc PR . . C84 C 0.0579(6) 0.2500 0.9015(10) 0.070(4) Uani 1 2 d S . . H84A H 0.0312 0.2744 0.9419 0.084 Uiso 0.50 1 calc PR . . H84B H 0.0958 0.2687 0.9057 0.084 Uiso 0.50 1 calc PR . . H84C H 0.0593 0.2069 0.9262 0.084 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0280(6) 0.0503(8) 0.0295(6) -0.0029(6) -0.0033(5) -0.0127(5) N11 0.021(3) 0.052(4) 0.022(3) 0.000(3) -0.002(2) -0.007(3) C1 0.020(3) 0.059(5) 0.022(4) 0.003(4) 0.005(3) -0.006(3) C2 0.016(4) 0.054(7) 0.017(5) 0.000 -0.002(4) 0.000 C4 0.009(4) 0.047(7) 0.021(5) 0.000 0.004(4) 0.000 C5 0.018(5) 0.037(7) 0.031(6) 0.000 -0.010(4) 0.000 C6 0.028(5) 0.077(9) 0.021(5) 0.000 -0.007(4) 0.000 C7 0.051(8) 0.090(11) 0.032(6) 0.000 -0.015(5) 0.000 C8 0.057(8) 0.047(8) 0.032(6) 0.000 -0.023(6) 0.000 C9 0.024(6) 0.125(14) 0.057(8) 0.000 -0.024(6) 0.000 C10 0.025(6) 0.181(18) 0.041(7) 0.000 -0.010(5) 0.000 C11 0.031(4) 0.070(6) 0.020(4) -0.010(4) -0.002(3) -0.012(4) N12 0.035(3) 0.051(5) 0.030(3) -0.004(3) -0.006(3) -0.017(3) C12 0.049(5) 0.063(6) 0.041(5) -0.007(4) -0.012(4) -0.025(4) C13 0.054(5) 0.072(7) 0.033(4) -0.011(4) -0.001(4) -0.015(5) C14 0.038(4) 0.043(5) 0.044(5) -0.012(4) 0.010(4) -0.014(4) C15 0.044(5) 0.078(8) 0.048(5) -0.018(5) 0.010(4) -0.020(5) C16 0.046(5) 0.045(6) 0.075(7) -0.017(5) 0.023(5) -0.007(4) C17 0.029(4) 0.055(6) 0.058(5) -0.005(5) 0.006(4) -0.004(4) C18 0.019(4) 0.060(6) 0.046(5) -0.014(4) 0.002(3) -0.005(4) N13 0.025(3) 0.043(4) 0.040(4) -0.010(3) 0.003(3) -0.011(3) C22 0.025(4) 0.087(7) 0.034(4) 0.002(5) -0.008(3) -0.025(4) C23 0.051(5) 0.080(7) 0.039(5) -0.006(5) -0.004(4) -0.038(5) C24 0.033(4) 0.034(5) 0.039(4) 0.001(3) 0.002(3) -0.008(3) C25 0.035(4) 0.045(5) 0.044(5) -0.002(4) 0.000(3) -0.001(4) C26 0.042(4) 0.058(6) 0.039(5) -0.008(4) 0.006(3) 0.008(4) C27 0.048(5) 0.076(7) 0.029(4) -0.010(4) -0.007(4) 0.003(5) C28 0.033(4) 0.057(6) 0.035(4) -0.006(4) -0.005(3) 0.000(4) N14 0.035(3) 0.036(4) 0.029(3) -0.004(3) -0.007(3) -0.003(3) O40 0.046(3) 0.056(4) 0.044(3) -0.007(3) 0.008(2) -0.009(3) N50 0.034(4) 0.091(6) 0.042(4) 0.000(4) -0.010(3) -0.029(4) C50 0.050(6) 0.116(9) 0.040(5) 0.004(6) -0.008(4) -0.032(6) C51 0.049(6) 0.132(11) 0.106(9) 0.029(8) -0.026(6) -0.044(7) Cl1 0.0204(11) 0.0500(18) 0.0376(14) 0.000 -0.0037(10) 0.000 O11 0.038(3) 0.050(4) 0.107(5) -0.006(4) -0.030(3) 0.015(3) O12 0.024(3) 0.055(5) 0.031(4) 0.000 -0.008(3) 0.000 O13 0.054(5) 0.146(10) 0.035(5) 0.000 0.010(4) 0.000 Cl2 0.0359(11) 0.125(3) 0.0484(13) 0.0149(15) 0.0105(10) 0.0157(13) O21 0.038(4) 0.192(9) 0.071(5) 0.004(5) 0.004(3) -0.017(5) O22 0.114(6) 0.090(6) 0.069(5) 0.002(4) 0.012(4) 0.032(5) O23 0.118(7) 0.115(7) 0.081(5) -0.009(5) 0.064(5) 0.024(5) O24 0.052(4) 0.118(7) 0.142(7) 0.006(6) -0.029(4) 0.009(4) Cl3 0.0341(15) 0.076(3) 0.058(2) 0.000 0.0062(14) 0.000 O31 0.110(11) 0.242(19) 0.116(11) 0.000 0.075(9) 0.000 O32 0.041(6) 0.23(6) 0.087(9) 0.049(19) 0.000(6) 0.053(17) O33 0.116(16) 0.13(2) 0.105(16) -0.057(13) -0.051(13) 0.074(14) O34 0.138(17) 0.060(12) 0.105(17) 0.002(12) -0.034(15) 0.008(11) N60 0.069(6) 0.144(9) 0.048(5) 0.023(5) -0.009(4) -0.052(6) C60 0.060(6) 0.099(9) 0.037(5) 0.012(5) -0.010(4) -0.027(6) C61 0.052(6) 0.125(10) 0.051(6) 0.003(6) 0.004(4) -0.026(6) N70 0.032(6) 0.09(2) 0.045(6) 0.013(18) 0.008(5) -0.027(17) C70 0.030(8) 0.065(15) 0.033(8) 0.003(7) 0.009(6) 0.008(7) C71 0.033(10) 0.17(2) 0.078(14) -0.008(15) 0.013(9) -0.012(12) C80 0.117(17) 0.25(3) 0.051(10) 0.000 -0.011(11) 0.000 C81 0.061(9) 0.161(17) 0.025(7) 0.000 0.004(6) 0.000 O82 0.064(6) 0.103(8) 0.046(5) 0.000 -0.005(5) 0.000 C83 0.043(8) 0.146(16) 0.067(10) 0.000 0.002(7) 0.000 C84 0.060(9) 0.090(12) 0.059(9) 0.000 -0.012(7) 0.000 _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 Mn1 N50 2.206(6) . y Mn1 O40 2.234(5) . y Mn1 N13 2.239(6) . y Mn1 N14 2.240(6) . y Mn1 N12 2.289(6) . y Mn1 N11 2.321(6) . y N11 C4 1.342(7) . ? N11 C1 1.358(8) . ? C1 C2 1.379(9) . ? C1 C11 1.491(11) . ? C2 C1 1.379(9) 7_575 ? C2 H2 0.9500 . ? C4 N11 1.342(7) 7_575 ? C4 C5 1.507(13) . ? C5 C6 1.350(14) . ? C5 C10 1.379(14) . ? C6 C7 1.372(14) . ? C6 H6 0.9500 . ? C7 C8 1.335(16) . ? C7 H7 0.9500 . ? C8 C9 1.342(17) . ? C8 H8 0.9500 . ? C9 C10 1.422(16) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 N12 1.476(10) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? N12 C22 1.478(9) . ? N12 C12 1.487(10) . ? C12 C13 1.541(12) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.492(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N13 1.354(9) . ? C14 C15 1.376(12) . ? C15 C16 1.390(13) . ? C15 H15 0.9500 . ? C16 C17 1.390(12) . ? C16 H16 0.9500 . ? C17 C18 1.388(12) . ? C17 H17 0.9500 . ? C18 N13 1.349(10) . ? C18 H18 0.9500 . ? C22 C23 1.530(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.505(10) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N14 1.358(9) . ? C24 C25 1.364(10) . ? C25 C26 1.375(10) . ? C25 H25 0.9500 . ? C26 C27 1.373(11) . ? C26 H26 0.9500 . ? C27 C28 1.380(10) . ? C27 H27 0.9500 . ? C28 N14 1.353(9) . ? C28 H28 0.9500 . ? O40 H40X 0.8256 . ? O40 H40Y 0.7982 . ? N50 C50 1.102(10) . ? C50 C51 1.479(12) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? Cl1 O11 1.429(6) 7_565 ? Cl1 O11 1.429(6) . ? Cl1 O13 1.429(8) . ? Cl1 O12 1.433(7) . ? Cl2 O21 1.373(7) . ? Cl2 O23 1.394(7) . ? Cl2 O24 1.450(7) . ? Cl2 O22 1.488(8) . ? Cl3 O31 1.302(12) . ? Cl3 O32 1.363(16) 7_575 ? Cl3 O32 1.363(16) . ? Cl3 O34 1.43(2) . ? Cl3 O34 1.43(2) 7_575 ? Cl3 O33 1.437(19) . ? Cl3 O33 1.437(19) 7_575 ? O32 O32 0.69(10) 7_575 ? O33 O34 1.01(3) 7_575 ? O33 O33 1.57(5) 7_575 ? O34 O33 1.01(3) 7_575 ? N60 C60 1.131(10) . ? C60 C61 1.449(11) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? N70 C70 1.128(19) . ? C70 C71 1.443(16) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C80 C81 1.48(2) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 O82 1.406(14) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? O82 C83 1.339(15) . ? C83 C84 1.536(18) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N50 Mn1 O40 82.9(2) . . y N50 Mn1 N13 89.2(3) . . y O40 Mn1 N13 87.8(2) . . y N50 Mn1 N14 94.4(2) . . y O40 Mn1 N14 175.8(2) . . y N13 Mn1 N14 95.3(2) . . y N50 Mn1 N12 173.6(2) . . y O40 Mn1 N12 91.1(2) . . y N13 Mn1 N12 88.4(2) . . y N14 Mn1 N12 91.7(2) . . y N50 Mn1 N11 106.4(3) . . y O40 Mn1 N11 79.7(2) . . y N13 Mn1 N11 158.5(2) . . y N14 Mn1 N11 98.1(2) . . y N12 Mn1 N11 74.5(2) . . y C4 N11 C1 116.9(7) . . ? C4 N11 Mn1 131.9(5) . . ? C1 N11 Mn1 111.2(5) . . ? N11 C1 C2 120.7(7) . . ? N11 C1 C11 118.0(7) . . ? C2 C1 C11 121.3(6) . . ? C1 C2 C1 119.0(9) 7_575 . ? C1 C2 H2 120.5 7_575 . ? C1 C2 H2 120.5 . . ? N11 C4 N11 125.7(8) . 7_575 ? N11 C4 C5 117.1(4) . . ? N11 C4 C5 117.1(4) 7_575 . ? C6 C5 C10 119.2(10) . . ? C6 C5 C4 120.4(8) . . ? C10 C5 C4 120.4(9) . . ? C5 C6 C7 120.9(10) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C8 C7 C6 121.7(12) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C7 C8 C9 119.0(11) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? C8 C9 C10 121.2(11) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C5 C10 C9 118.0(11) . . ? C5 C10 H10 121.0 . . ? C9 C10 H10 121.0 . . ? N12 C11 C1 112.2(6) . . ? N12 C11 H11A 109.2 . . ? C1 C11 H11A 109.2 . . ? N12 C11 H11B 109.2 . . ? C1 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C11 N12 C22 108.3(6) . . ? C11 N12 C12 107.3(6) . . ? C22 N12 C12 109.1(6) . . ? C11 N12 Mn1 104.5(4) . . ? C22 N12 Mn1 111.1(4) . . ? C12 N12 Mn1 116.1(5) . . ? N12 C12 C13 116.4(6) . . ? N12 C12 H12A 108.2 . . ? C13 C12 H12A 108.2 . . ? N12 C12 H12B 108.2 . . ? C13 C12 H12B 108.2 . . ? H12A C12 H12B 107.3 . . ? C14 C13 C12 113.3(7) . . ? C14 C13 H13A 108.9 . . ? C12 C13 H13A 108.9 . . ? C14 C13 H13B 108.9 . . ? C12 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? N13 C14 C15 120.1(8) . . ? N13 C14 C13 119.3(8) . . ? C15 C14 C13 120.6(8) . . ? C14 C15 C16 121.4(8) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C17 C16 C15 118.7(9) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? C18 C17 C16 117.2(9) . . ? C18 C17 H17 121.4 . . ? C16 C17 H17 121.4 . . ? N13 C18 C17 123.9(8) . . ? N13 C18 H18 118.0 . . ? C17 C18 H18 118.0 . . ? C18 N13 C14 118.7(7) . . ? C18 N13 Mn1 117.9(5) . . ? C14 N13 Mn1 123.4(6) . . ? N12 C22 C23 114.3(7) . . ? N12 C22 H22A 108.7 . . ? C23 C22 H22A 108.7 . . ? N12 C22 H22B 108.7 . . ? C23 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? C24 C23 C22 117.5(7) . . ? C24 C23 H23A 107.9 . . ? C22 C23 H23A 107.9 . . ? C24 C23 H23B 107.9 . . ? C22 C23 H23B 107.9 . . ? H23A C23 H23B 107.2 . . ? N14 C24 C25 122.0(7) . . ? N14 C24 C23 118.2(6) . . ? C25 C24 C23 119.8(7) . . ? C24 C25 C26 120.3(7) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C27 C26 C25 119.2(7) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 117.9(7) . . ? C26 C27 H27 121.1 . . ? C28 C27 H27 121.1 . . ? N14 C28 C27 123.8(7) . . ? N14 C28 H28 118.1 . . ? C27 C28 H28 118.1 . . ? C28 N14 C24 116.7(6) . . ? C28 N14 Mn1 116.7(5) . . ? C24 N14 Mn1 126.5(5) . . ? Mn1 O40 H40X 120.9 . . ? Mn1 O40 H40Y 120.6 . . ? H40X O40 H40Y 108.0 . . ? C50 N50 Mn1 162.3(7) . . ? N50 C50 C51 177.1(13) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O11 Cl1 O11 109.9(5) 7_565 . ? O11 Cl1 O13 109.6(4) 7_565 . ? O11 Cl1 O13 109.6(4) . . ? O11 Cl1 O12 109.8(3) 7_565 . ? O11 Cl1 O12 109.8(3) . . ? O13 Cl1 O12 108.2(5) . . ? O21 Cl2 O23 114.1(5) . . ? O21 Cl2 O24 109.9(5) . . ? O23 Cl2 O24 106.9(5) . . ? O21 Cl2 O22 107.8(5) . . ? O23 Cl2 O22 109.7(5) . . ? O24 Cl2 O22 108.2(5) . . ? O31 Cl3 O32 113.1(10) . 7_575 ? O31 Cl3 O32 113.1(10) . . ? O32 Cl3 O32 29(4) 7_575 . ? O31 Cl3 O34 90.2(10) . . ? O32 Cl3 O34 99(2) 7_575 . ? O32 Cl3 O34 128(2) . . ? O31 Cl3 O34 90.2(10) . 7_575 ? O32 Cl3 O34 128(2) 7_575 7_575 ? O32 Cl3 O34 99(2) . 7_575 ? O34 Cl3 O34 127.4(18) . 7_575 ? O31 Cl3 O33 127.1(12) . . ? O32 Cl3 O33 114.4(15) 7_575 . ? O32 Cl3 O33 98.0(16) . . ? O34 Cl3 O33 103.4(14) . . ? O34 Cl3 O33 41.4(10) 7_575 . ? O31 Cl3 O33 127.1(12) . 7_575 ? O32 Cl3 O33 98.0(16) 7_575 7_575 ? O32 Cl3 O33 114.4(15) . 7_575 ? O34 Cl3 O33 41.4(10) . 7_575 ? O34 Cl3 O33 103.3(14) 7_575 7_575 ? O33 Cl3 O33 66.3(19) . 7_575 ? O32 O32 Cl3 75(2) 7_575 . ? O34 O33 Cl3 68.8(18) 7_575 . ? O34 O33 O33 119(2) 7_575 7_575 ? Cl3 O33 O33 56.9(10) . 7_575 ? O33 O34 Cl3 70(2) 7_575 . ? N60 C60 C61 177.3(11) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N70 C70 C71 179(3) . . ? C81 C80 H80A 109.5 . . ? C81 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C81 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? O82 C81 C80 109.3(12) . . ? O82 C81 H81A 109.8 . . ? C80 C81 H81A 109.8 . . ? O82 C81 H81B 109.8 . . ? C80 C81 H81B 109.8 . . ? H81A C81 H81B 108.3 . . ? C83 O82 C81 113.0(11) . . ? O82 C83 C84 111.9(12) . . ? O82 C83 H83A 109.2 . . ? C84 C83 H83A 109.2 . . ? O82 C83 H83B 109.2 . . ? C84 C83 H83B 109.2 . . ? H83A C83 H83B 107.9 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N50 Mn1 N11 C4 -25.4(7) . . . . ? O40 Mn1 N11 C4 -104.8(6) . . . . ? N13 Mn1 N11 C4 -160.3(6) . . . . ? N14 Mn1 N11 C4 71.7(6) . . . . ? N12 Mn1 N11 C4 161.2(7) . . . . ? N50 Mn1 N11 C1 153.1(4) . . . . ? O40 Mn1 N11 C1 73.7(4) . . . . ? N13 Mn1 N11 C1 18.2(8) . . . . ? N14 Mn1 N11 C1 -109.9(4) . . . . ? N12 Mn1 N11 C1 -20.4(4) . . . . ? C4 N11 C1 C2 -0.2(10) . . . . ? Mn1 N11 C1 C2 -178.9(6) . . . . ? C4 N11 C1 C11 179.1(6) . . . . ? Mn1 N11 C1 C11 0.4(7) . . . . ? N11 C1 C2 C1 2.4(13) . . . 7_575 ? C11 C1 C2 C1 -177.0(5) . . . 7_575 ? C1 N11 C4 N11 -2.1(12) . . . 7_575 ? Mn1 N11 C4 N11 176.3(4) . . . 7_575 ? C1 N11 C4 C5 176.1(7) . . . . ? Mn1 N11 C4 C5 -5.5(10) . . . . ? N11 C4 C5 C6 -89.2(6) . . . . ? N11 C4 C5 C6 89.2(6) 7_575 . . . ? N11 C4 C5 C10 90.8(6) . . . . ? N11 C4 C5 C10 -90.8(6) 7_575 . . . ? C10 C5 C6 C7 0.000(3) . . . . ? C4 C5 C6 C7 180.000(2) . . . . ? C5 C6 C7 C8 0.000(3) . . . . ? C6 C7 C8 C9 0.000(4) . . . . ? C7 C8 C9 C10 0.000(3) . . . . ? C6 C5 C10 C9 0.000(3) . . . . ? C4 C5 C10 C9 180.000(2) . . . . ? C8 C9 C10 C5 0.000(3) . . . . ? N11 C1 C11 N12 33.3(8) . . . . ? C2 C1 C11 N12 -147.3(7) . . . . ? C1 C11 N12 C22 71.0(7) . . . . ? C1 C11 N12 C12 -171.3(6) . . . . ? C1 C11 N12 Mn1 -47.5(6) . . . . ? O40 Mn1 N12 C11 -43.8(5) . . . . ? N13 Mn1 N12 C11 -131.6(5) . . . . ? N14 Mn1 N12 C11 133.1(5) . . . . ? N11 Mn1 N12 C11 35.2(4) . . . . ? O40 Mn1 N12 C22 -160.4(5) . . . . ? N13 Mn1 N12 C22 111.8(5) . . . . ? N14 Mn1 N12 C22 16.5(5) . . . . ? N11 Mn1 N12 C22 -81.4(5) . . . . ? O40 Mn1 N12 C12 74.2(5) . . . . ? N13 Mn1 N12 C12 -13.6(5) . . . . ? N14 Mn1 N12 C12 -108.9(5) . . . . ? N11 Mn1 N12 C12 153.2(5) . . . . ? C11 N12 C12 C13 86.1(8) . . . . ? C22 N12 C12 C13 -156.7(7) . . . . ? Mn1 N12 C12 C13 -30.3(9) . . . . ? N12 C12 C13 C14 77.2(9) . . . . ? C12 C13 C14 N13 -58.4(10) . . . . ? C12 C13 C14 C15 122.9(8) . . . . ? N13 C14 C15 C16 -0.5(12) . . . . ? C13 C14 C15 C16 178.2(7) . . . . ? C14 C15 C16 C17 1.0(12) . . . . ? C15 C16 C17 C18 -0.3(11) . . . . ? C16 C17 C18 N13 -1.1(11) . . . . ? C17 C18 N13 C14 1.7(10) . . . . ? C17 C18 N13 Mn1 -177.1(5) . . . . ? C15 C14 N13 C18 -0.9(10) . . . . ? C13 C14 N13 C18 -179.6(6) . . . . ? C15 C14 N13 Mn1 177.8(5) . . . . ? C13 C14 N13 Mn1 -0.9(9) . . . . ? N50 Mn1 N13 C18 35.9(5) . . . . ? O40 Mn1 N13 C18 118.8(5) . . . . ? N14 Mn1 N13 C18 -58.4(5) . . . . ? N12 Mn1 N13 C18 -150.0(5) . . . . ? N11 Mn1 N13 C18 173.1(5) . . . . ? N50 Mn1 N13 C14 -142.8(5) . . . . ? O40 Mn1 N13 C14 -59.9(5) . . . . ? N14 Mn1 N13 C14 122.9(5) . . . . ? N12 Mn1 N13 C14 31.3(5) . . . . ? N11 Mn1 N13 C14 -5.6(9) . . . . ? C11 N12 C22 C23 -170.8(6) . . . . ? C12 N12 C22 C23 72.7(8) . . . . ? Mn1 N12 C22 C23 -56.6(8) . . . . ? N12 C22 C23 C24 83.0(10) . . . . ? C22 C23 C24 N14 -50.2(12) . . . . ? C22 C23 C24 C25 131.4(8) . . . . ? N14 C24 C25 C26 -1.7(12) . . . . ? C23 C24 C25 C26 176.6(8) . . . . ? C24 C25 C26 C27 -0.9(13) . . . . ? C25 C26 C27 C28 3.2(13) . . . . ? C26 C27 C28 N14 -3.3(14) . . . . ? C27 C28 N14 C24 0.9(12) . . . . ? C27 C28 N14 Mn1 178.2(7) . . . . ? C25 C24 N14 C28 1.7(11) . . . . ? C23 C24 N14 C28 -176.6(7) . . . . ? C25 C24 N14 Mn1 -175.4(6) . . . . ? C23 C24 N14 Mn1 6.3(10) . . . . ? N50 Mn1 N14 C28 12.6(6) . . . . ? N13 Mn1 N14 C28 102.2(6) . . . . ? N12 Mn1 N14 C28 -169.2(6) . . . . ? N11 Mn1 N14 C28 -94.7(6) . . . . ? N50 Mn1 N14 C24 -170.4(6) . . . . ? N13 Mn1 N14 C24 -80.8(6) . . . . ? N12 Mn1 N14 C24 7.8(6) . . . . ? N11 Mn1 N14 C24 82.4(6) . . . . ? O40 Mn1 N50 C50 -5(3) . . . . ? N13 Mn1 N50 C50 83(3) . . . . ? N14 Mn1 N50 C50 179(3) . . . . ? N11 Mn1 N50 C50 -82(3) . . . . ? O31 Cl3 O32 O32 96.4(10) . . . 7_575 ? O34 Cl3 O32 O32 -13.5(12) . . . 7_575 ? O34 Cl3 O32 O32 -169.3(10) 7_575 . . 7_575 ? O33 Cl3 O32 O32 -127.4(12) . . . 7_575 ? O33 Cl3 O32 O32 -59.8(13) 7_575 . . 7_575 ? O31 Cl3 O33 O34 32(2) . . . 7_575 ? O32 Cl3 O33 O34 -120(3) 7_575 . . 7_575 ? O32 Cl3 O33 O34 -95(3) . . . 7_575 ? O34 Cl3 O33 O34 132(3) . . . 7_575 ? O33 Cl3 O33 O34 151.4(17) 7_575 . . 7_575 ? O31 Cl3 O33 O33 -119.6(11) . . . 7_575 ? O32 Cl3 O33 O33 88(2) 7_575 . . 7_575 ? O32 Cl3 O33 O33 113.3(19) . . . 7_575 ? O31 Cl3 O34 O33 155(2) . . . 7_575 ? O32 Cl3 O34 O33 -91(2) 7_575 . . 7_575 ? O32 Cl3 O34 O33 -85(2) . . . 7_575 ? O33 Cl3 O34 O33 26.7(18) . . . 7_575 ? C80 C81 O82 C83 180.000(2) . . . . ? C81 O82 C83 C84 180.000(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O40 H40X O24 0.83 2.21 2.875(10) 137.1 . O40 H40Y O34 0.80 2.25 2.88(3) 136.4 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.026 _refine_diff_density_min -0.803 _refine_diff_density_rms 0.143 # Attachment 'wag271.cif' data_wag271 _database_code_depnum_ccdc_archive 'CCDC 842531' #TrackingRef 'wag271.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82.40 H93.60 B4 Co4 F20 N16 O2.40' _chemical_formula_weight 2005.49 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.8889(13) _cell_length_b 22.663(2) _cell_length_c 26.145(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.529(4) _cell_angle_gamma 90.00 _cell_volume 8612.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 91(2) _cell_measurement_reflns_used 9336 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 26.37 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4109 _exptl_absorpt_coefficient_mu 0.859 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7251 _exptl_absorpt_correction_T_max 0.9190 _exptl_absorpt_process_details 'SCALE (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 91(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 95755 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 26.48 _reflns_number_total 8840 _reflns_number_gt 8070 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. [Co(II)4(LEt)2)(F)4](BF4)4.2.4MeOH Half of this in the asym unit and the other half generated by center of inversion. All non-H anis One MeOH(O50, c50) with full occup. and another MeOH(o60 c60) of 0.2 occup.are found and the latter is samed to O50. All H calc and ride except that on MeOH O atom which was inserted using HFIX 147 which optimizes OH angle to td;torsion angle chosen to maximize e density.One BF4 is ordered.The other BF4 is disordered and split into two parts B2:f21-f24 and B21:f25-f28 with site occup.0.8:0.2, respectively. H-bonds are present between MeOH(O50) and F21, f23 and f25; also between MeOH (O50) and MeOH (O60). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+14.8939P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8840 _refine_ls_number_parameters 638 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0994 _refine_ls_wR_factor_gt 0.0964 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.776468(18) 0.257886(12) -0.144316(11) 0.01872(8) Uani 1 1 d . . . Co2 Co 0.764091(19) 0.367234(12) 0.097820(11) 0.01951(8) Uani 1 1 d . . . N11 N 0.74513(11) 0.32236(7) -0.07796(7) 0.0175(3) Uani 1 1 d . . . C1 C 0.65959(14) 0.34319(9) -0.09666(8) 0.0182(4) Uani 1 1 d . . . C2 C 0.61010(14) 0.37115(9) -0.06479(8) 0.0190(4) Uani 1 1 d . . . H2 H 0.5513 0.3878 -0.0788 0.023 Uiso 1 1 calc R . . C3 C 0.64896(14) 0.37409(9) -0.01203(8) 0.0192(4) Uani 1 1 d . . . N15 N 0.73491(11) 0.35329(7) 0.00797(7) 0.0181(3) Uani 1 1 d . . . C4 C 0.78093(13) 0.33082(8) -0.02660(8) 0.0166(4) Uani 1 1 d . . . C5 C 0.88061(13) 0.31765(9) -0.00778(8) 0.0181(4) Uani 1 1 d . . . C6 C 0.91015(15) 0.27194(10) 0.02656(9) 0.0272(5) Uani 1 1 d . . . H6 H 0.8664 0.2482 0.0387 0.033 Uiso 1 1 calc R . . C7 C 1.00351(17) 0.26032(11) 0.04355(11) 0.0345(6) Uani 1 1 d . . . H7 H 1.0235 0.2281 0.0664 0.041 Uiso 1 1 calc R . . C8 C 1.06712(15) 0.29572(12) 0.02711(10) 0.0329(5) Uani 1 1 d . . . H8 H 1.1310 0.2878 0.0385 0.040 Uiso 1 1 calc R . . C9 C 1.03808(16) 0.34265(13) -0.00586(10) 0.0351(6) Uani 1 1 d . . . H9 H 1.0821 0.3679 -0.0160 0.042 Uiso 1 1 calc R . . C10 C 0.94467(15) 0.35314(11) -0.02431(9) 0.0294(5) Uani 1 1 d . . . H10 H 0.9248 0.3845 -0.0482 0.035 Uiso 1 1 calc R . . C11 C 0.61919(14) 0.33602(10) -0.15375(8) 0.0223(4) Uani 1 1 d . . . H11A H 0.5763 0.3021 -0.1587 0.027 Uiso 1 1 calc R . . H11B H 0.5830 0.3717 -0.1667 0.027 Uiso 1 1 calc R . . N12 N 0.68884(12) 0.32645(8) -0.18562(7) 0.0207(4) Uani 1 1 d . . . C12 C 0.63701(16) 0.31346(11) -0.24020(8) 0.0269(5) Uani 1 1 d . . . H12A H 0.6712 0.3299 -0.2654 0.032 Uiso 1 1 calc R . . H12B H 0.5763 0.3332 -0.2463 0.032 Uiso 1 1 calc R . . C13 C 0.62273(16) 0.24741(11) -0.25027(9) 0.0292(5) Uani 1 1 d . . . H13A H 0.6073 0.2282 -0.2193 0.035 Uiso 1 1 calc R . . H13B H 0.5710 0.2409 -0.2807 0.035 Uiso 1 1 calc R . . C14 C 0.70918(16) 0.22111(10) -0.26108(9) 0.0264(5) Uani 1 1 d . . . C15 C 0.71463(19) 0.20316(12) -0.31125(10) 0.0361(6) Uani 1 1 d . . . H15 H 0.6619 0.2051 -0.3391 0.043 Uiso 1 1 calc R . . C16 C 0.7968(2) 0.18260(13) -0.32026(11) 0.0443(7) Uani 1 1 d . . . H16 H 0.8015 0.1700 -0.3543 0.053 Uiso 1 1 calc R . . C17 C 0.8719(2) 0.18063(12) -0.27910(11) 0.0407(6) Uani 1 1 d . . . H17 H 0.9294 0.1665 -0.2842 0.049 Uiso 1 1 calc R . . C18 C 0.86295(17) 0.19955(11) -0.23011(10) 0.0316(5) Uani 1 1 d . . . H18 H 0.9155 0.1984 -0.2020 0.038 Uiso 1 1 calc R . . N13 N 0.78296(13) 0.21947(8) -0.22060(7) 0.0249(4) Uani 1 1 d . . . C22 C 0.74293(15) 0.38164(10) -0.18657(9) 0.0253(5) Uani 1 1 d . . . H22A H 0.7643 0.3961 -0.1502 0.030 Uiso 1 1 calc R . . H22B H 0.7022 0.4122 -0.2064 0.030 Uiso 1 1 calc R . . C23 C 0.82629(16) 0.37350(11) -0.21130(9) 0.0300(5) Uani 1 1 d . . . H23A H 0.8075 0.3481 -0.2426 0.036 Uiso 1 1 calc R . . H23B H 0.8427 0.4125 -0.2236 0.036 Uiso 1 1 calc R . . C24 C 0.91143(16) 0.34727(10) -0.17738(9) 0.0260(5) Uani 1 1 d . . . C25 C 0.99709(18) 0.36971(12) -0.17983(10) 0.0354(6) Uani 1 1 d . . . H25 H 1.0012 0.4040 -0.2001 0.042 Uiso 1 1 calc R . . C26 C 1.07650(17) 0.34254(13) -0.15307(11) 0.0382(6) Uani 1 1 d . . . H26 H 1.1353 0.3572 -0.1553 0.046 Uiso 1 1 calc R . . C27 C 1.06842(16) 0.29356(12) -0.12298(11) 0.0350(6) Uani 1 1 d . . . H27 H 1.1216 0.2733 -0.1046 0.042 Uiso 1 1 calc R . . C28 C 0.98133(15) 0.27457(11) -0.12005(10) 0.0294(5) Uani 1 1 d . . . H28 H 0.9760 0.2419 -0.0981 0.035 Uiso 1 1 calc R . . N14 N 0.90370(12) 0.30026(8) -0.14686(7) 0.0237(4) Uani 1 1 d . . . C31 C 0.59912(14) 0.40398(10) 0.02508(8) 0.0223(4) Uani 1 1 d . . . H31A H 0.5539 0.4323 0.0054 0.027 Uiso 1 1 calc R . . H31B H 0.5651 0.3741 0.0410 0.027 Uiso 1 1 calc R . . N16 N 0.66435(12) 0.43561(8) 0.06697(7) 0.0217(4) Uani 1 1 d . . . C32 C 0.61001(17) 0.46188(11) 0.10363(9) 0.0287(5) Uani 1 1 d . . . H32A H 0.5457 0.4680 0.0843 0.034 Uiso 1 1 calc R . . H32B H 0.6361 0.5010 0.1155 0.034 Uiso 1 1 calc R . . C33 C 0.60974(17) 0.42366(11) 0.15136(9) 0.0312(5) Uani 1 1 d . . . H33A H 0.5603 0.4371 0.1685 0.037 Uiso 1 1 calc R . . H33B H 0.5966 0.3823 0.1401 0.037 Uiso 1 1 calc R . . C34 C 0.70028(19) 0.42644(11) 0.18989(9) 0.0322(5) Uani 1 1 d . . . C35 C 0.7098(2) 0.45382(12) 0.23852(10) 0.0436(7) Uani 1 1 d . . . H35 H 0.6577 0.4704 0.2486 0.052 Uiso 1 1 calc R . . C36 C 0.7952(2) 0.45683(13) 0.27187(11) 0.0501(8) Uani 1 1 d . . . H36 H 0.8024 0.4755 0.3050 0.060 Uiso 1 1 calc R . . C37 C 0.8701(2) 0.43245(12) 0.25664(10) 0.0442(7) Uani 1 1 d . . . H37 H 0.9297 0.4340 0.2789 0.053 Uiso 1 1 calc R . . C38 C 0.85620(19) 0.40582(11) 0.20836(9) 0.0351(6) Uani 1 1 d . . . H38 H 0.9076 0.3886 0.1980 0.042 Uiso 1 1 calc R . . N17 N 0.77396(14) 0.40281(9) 0.17509(7) 0.0285(4) Uani 1 1 d . . . C42 C 0.70790(16) 0.48472(10) 0.04299(9) 0.0262(5) Uani 1 1 d . . . H42A H 0.6615 0.5160 0.0314 0.031 Uiso 1 1 calc R . . H42B H 0.7277 0.4697 0.0116 0.031 Uiso 1 1 calc R . . C43 C 0.79079(17) 0.51155(10) 0.08047(10) 0.0304(5) Uani 1 1 d . . . H43A H 0.7999 0.5521 0.0685 0.037 Uiso 1 1 calc R . . H43B H 0.7761 0.5148 0.1155 0.037 Uiso 1 1 calc R . . C44 C 0.88032(16) 0.47851(10) 0.08616(9) 0.0271(5) Uani 1 1 d . . . C45 C 0.96077(19) 0.50885(12) 0.08472(11) 0.0405(6) Uani 1 1 d . . . H45 H 0.9585 0.5501 0.0781 0.049 Uiso 1 1 calc R . . C46 C 1.04385(18) 0.47967(13) 0.09279(11) 0.0418(6) Uani 1 1 d . . . H46 H 1.0987 0.5004 0.0914 0.050 Uiso 1 1 calc R . . C47 C 1.04596(17) 0.41981(12) 0.10299(9) 0.0324(5) Uani 1 1 d . . . H47 H 1.1023 0.3986 0.1096 0.039 Uiso 1 1 calc R . . C48 C 0.96386(15) 0.39172(10) 0.10329(9) 0.0262(5) Uani 1 1 d . . . H48 H 0.9652 0.3505 0.1100 0.031 Uiso 1 1 calc R . . N18 N 0.88203(13) 0.41942(8) 0.09468(7) 0.0231(4) Uani 1 1 d . . . F1 F 0.66683(8) 0.20676(5) -0.13055(5) 0.0223(3) Uani 1 1 d . . . F2 F 0.83909(8) 0.19227(5) -0.09971(5) 0.0228(3) Uani 1 1 d . . . O50 O 0.4091(2) 0.35106(12) 0.07788(11) 0.0731(8) Uani 1 1 d D . . H50X H 0.4028 0.3866 0.0855 0.088 Uiso 1 1 calc R . . C50 C 0.3431(4) 0.33649(18) 0.03141(16) 0.0838(14) Uani 1 1 d D . . H50A H 0.3451 0.2940 0.0249 0.101 Uiso 1 1 calc R . . H50B H 0.3573 0.3581 0.0017 0.101 Uiso 1 1 calc R . . H50C H 0.2814 0.3474 0.0357 0.101 Uiso 1 1 calc R . . O60 O 0.5000 0.4742(3) 0.2500 0.084(4) Uani 0.40 2 d SPD . . H60X H 0.4633 0.4619 0.2231 0.101 Uiso 0.20 1 calc PR . . C60 C 0.5000 0.5350(5) 0.2500 0.142(11) Uani 0.40 2 d SPD . . H60A H 0.4478 0.5494 0.2234 0.170 Uiso 0.20 1 calc PR . . H60B H 0.5575 0.5494 0.2421 0.170 Uiso 0.20 1 calc PR . . H60C H 0.4946 0.5494 0.2845 0.170 Uiso 0.20 1 calc PR . . B1 B 0.65342(18) 0.64092(13) 0.12339(11) 0.0306(6) Uani 1 1 d D . . F11 F 0.58613(10) 0.66982(8) 0.14320(6) 0.0422(4) Uani 1 1 d D . . F12 F 0.71068(11) 0.60800(8) 0.16254(6) 0.0449(4) Uani 1 1 d D . . F13 F 0.70626(12) 0.68331(8) 0.10441(8) 0.0578(5) Uani 1 1 d D . . F14 F 0.61260(10) 0.60469(7) 0.08267(6) 0.0378(3) Uani 1 1 d D . . B2 B 0.3154(6) 0.4878(3) 0.1064(3) 0.0529(19) Uani 0.80 1 d PD A 1 F21 F 0.3762(3) 0.4773(3) 0.0743(3) 0.0478(11) Uani 0.80 1 d PD A 1 F22 F 0.2504(5) 0.5291(3) 0.0824(3) 0.0564(17) Uani 0.80 1 d PD A 1 F23 F 0.2698(2) 0.43671(13) 0.11325(18) 0.0909(11) Uani 0.80 1 d PD A 1 F24 F 0.3663(3) 0.50881(15) 0.15335(11) 0.0956(11) Uani 0.80 1 d PD A 1 B21 B 0.2876(13) 0.4836(8) 0.0907(7) 0.040(8) Uani 0.20 1 d PD B 2 F25 F 0.3762(14) 0.4823(14) 0.0838(12) 0.083(10) Uani 0.20 1 d PD B 2 F26 F 0.2453(18) 0.5375(8) 0.0767(7) 0.026(4) Uani 0.20 1 d PD B 2 F27 F 0.2358(6) 0.4398(4) 0.0625(5) 0.066(3) Uani 0.20 1 d PD B 2 F28 F 0.2851(9) 0.4801(6) 0.1428(4) 0.071(3) Uani 0.20 1 d PD B 2 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 Co1 0.01555(14) 0.02104(15) 0.01963(15) 0.00081(11) 0.00397(11) 0.00005(10) Co2 0.01979(15) 0.01877(15) 0.01890(15) -0.00039(11) 0.00184(11) -0.00085(11) N11 0.0159(8) 0.0179(8) 0.0185(8) 0.0015(7) 0.0034(7) 0.0000(6) C1 0.0173(9) 0.0165(9) 0.0200(10) 0.0029(8) 0.0026(8) -0.0009(7) C2 0.0157(9) 0.0182(10) 0.0222(10) 0.0009(8) 0.0022(8) 0.0010(7) C3 0.0174(10) 0.0180(10) 0.0221(10) 0.0002(8) 0.0040(8) -0.0008(8) N15 0.0154(8) 0.0184(8) 0.0201(9) -0.0004(7) 0.0030(7) 0.0002(6) C4 0.0168(9) 0.0139(9) 0.0194(10) 0.0022(7) 0.0043(8) -0.0018(7) C5 0.0153(9) 0.0212(10) 0.0176(10) -0.0032(8) 0.0030(8) -0.0013(8) C6 0.0213(11) 0.0231(11) 0.0356(13) 0.0044(9) 0.0022(9) -0.0028(9) C7 0.0265(12) 0.0286(12) 0.0422(14) 0.0035(11) -0.0059(11) 0.0059(10) C8 0.0143(10) 0.0461(15) 0.0360(13) -0.0062(11) 0.0002(9) 0.0023(10) C9 0.0187(11) 0.0553(17) 0.0320(13) 0.0056(11) 0.0070(10) -0.0078(11) C10 0.0218(11) 0.0392(13) 0.0262(12) 0.0100(10) 0.0034(9) -0.0036(10) C11 0.0181(10) 0.0302(11) 0.0182(10) 0.0001(8) 0.0033(8) 0.0035(8) N12 0.0203(9) 0.0262(9) 0.0154(8) 0.0004(7) 0.0033(7) 0.0019(7) C12 0.0256(11) 0.0373(13) 0.0161(10) 0.0020(9) 0.0010(9) 0.0045(9) C13 0.0242(11) 0.0412(14) 0.0210(11) -0.0036(10) 0.0025(9) -0.0059(10) C14 0.0321(12) 0.0249(11) 0.0234(11) -0.0030(9) 0.0089(9) -0.0067(9) C15 0.0459(15) 0.0372(14) 0.0260(12) -0.0065(10) 0.0096(11) -0.0072(11) C16 0.0604(18) 0.0444(16) 0.0345(14) -0.0123(12) 0.0245(14) -0.0070(13) C17 0.0422(15) 0.0408(15) 0.0470(16) -0.0097(12) 0.0267(13) -0.0020(12) C18 0.0304(12) 0.0322(13) 0.0359(13) -0.0037(10) 0.0151(10) -0.0023(10) N13 0.0255(9) 0.0261(10) 0.0251(10) -0.0021(8) 0.0103(8) -0.0023(8) C22 0.0266(11) 0.0253(11) 0.0244(11) 0.0047(9) 0.0060(9) 0.0026(9) C23 0.0304(12) 0.0356(13) 0.0258(12) 0.0076(10) 0.0098(10) -0.0020(10) C24 0.0275(11) 0.0302(12) 0.0226(11) -0.0030(9) 0.0101(9) -0.0033(9) C25 0.0336(13) 0.0419(15) 0.0336(13) -0.0003(11) 0.0139(11) -0.0098(11) C26 0.0251(12) 0.0513(16) 0.0413(14) -0.0075(12) 0.0141(11) -0.0110(11) C27 0.0201(11) 0.0422(14) 0.0426(14) -0.0083(11) 0.0069(10) 0.0008(10) C28 0.0204(11) 0.0303(12) 0.0367(13) -0.0017(10) 0.0044(9) 0.0007(9) N14 0.0186(9) 0.0273(10) 0.0258(9) -0.0030(8) 0.0059(7) -0.0013(7) C31 0.0180(10) 0.0279(11) 0.0208(10) -0.0008(8) 0.0038(8) 0.0048(8) N16 0.0248(9) 0.0217(9) 0.0190(9) -0.0030(7) 0.0055(7) 0.0039(7) C32 0.0309(12) 0.0312(12) 0.0254(11) -0.0046(9) 0.0091(10) 0.0076(10) C33 0.0373(13) 0.0342(13) 0.0255(12) -0.0050(10) 0.0140(10) -0.0002(10) C34 0.0508(15) 0.0258(12) 0.0213(11) 0.0000(9) 0.0107(10) -0.0038(11) C35 0.0659(19) 0.0381(15) 0.0271(13) -0.0050(11) 0.0108(13) 0.0043(13) C36 0.083(2) 0.0398(16) 0.0226(13) -0.0073(11) 0.0013(14) -0.0014(15) C37 0.0634(19) 0.0363(14) 0.0252(13) -0.0012(11) -0.0072(12) -0.0074(13) C38 0.0460(15) 0.0304(13) 0.0253(12) 0.0018(10) -0.0004(11) -0.0058(11) N17 0.0389(11) 0.0242(10) 0.0210(9) -0.0011(7) 0.0038(8) -0.0040(8) C42 0.0332(12) 0.0203(11) 0.0259(11) 0.0024(9) 0.0081(9) 0.0041(9) C43 0.0361(13) 0.0198(11) 0.0352(13) -0.0011(9) 0.0075(10) -0.0010(9) C44 0.0327(12) 0.0243(11) 0.0240(11) -0.0015(9) 0.0052(9) -0.0026(9) C45 0.0423(15) 0.0286(13) 0.0504(16) 0.0075(12) 0.0097(12) -0.0103(11) C46 0.0320(13) 0.0443(16) 0.0495(16) 0.0036(13) 0.0096(12) -0.0129(12) C47 0.0263(12) 0.0410(14) 0.0280(12) -0.0029(10) 0.0019(10) -0.0047(10) C48 0.0255(11) 0.0282(12) 0.0226(11) -0.0024(9) 0.0001(9) -0.0025(9) N18 0.0258(9) 0.0214(9) 0.0210(9) -0.0019(7) 0.0023(7) -0.0045(7) F1 0.0214(6) 0.0219(6) 0.0233(6) 0.0024(5) 0.0041(5) -0.0020(5) F2 0.0185(6) 0.0230(6) 0.0255(6) 0.0023(5) 0.0018(5) -0.0010(5) O50 0.0783(18) 0.0663(16) 0.0818(19) 0.0187(14) 0.0333(15) 0.0259(14) C50 0.137(4) 0.058(2) 0.062(2) -0.0042(19) 0.036(3) 0.016(3) O60 0.074(7) 0.044(5) 0.166(11) 0.000 0.095(7) 0.000 C60 0.032(7) 0.057(9) 0.33(3) 0.000 0.024(12) 0.000 B1 0.0244(13) 0.0353(15) 0.0301(14) -0.0059(11) 0.0012(11) 0.0060(11) F11 0.0350(8) 0.0600(10) 0.0295(8) -0.0077(7) 0.0025(6) 0.0194(7) F12 0.0385(8) 0.0565(10) 0.0359(8) 0.0023(7) -0.0005(7) 0.0176(7) F13 0.0435(10) 0.0556(11) 0.0735(13) 0.0059(9) 0.0110(9) -0.0122(8) F14 0.0394(8) 0.0376(8) 0.0344(8) -0.0107(6) 0.0033(6) 0.0040(6) B2 0.096(5) 0.030(3) 0.039(3) 0.001(2) 0.031(4) -0.003(3) F21 0.040(2) 0.065(2) 0.0402(17) 0.0135(15) 0.0130(13) 0.0117(17) F22 0.051(3) 0.042(3) 0.083(4) -0.004(2) 0.029(2) -0.009(2) F23 0.110(3) 0.0440(16) 0.143(3) 0.025(2) 0.080(3) 0.0033(16) F24 0.146(3) 0.085(2) 0.0464(15) -0.0101(14) 0.0007(18) 0.046(2) B21 0.079(17) 0.015(9) 0.041(14) 0.016(9) 0.047(13) 0.012(10) F25 0.046(11) 0.13(2) 0.080(18) 0.013(12) 0.025(10) -0.025(10) F26 0.053(9) 0.013(5) 0.022(5) -0.001(4) 0.027(5) -0.002(5) F27 0.050(5) 0.031(5) 0.129(10) -0.031(6) 0.045(6) -0.014(4) F28 0.102(9) 0.078(8) 0.046(6) 0.014(5) 0.043(6) 0.015(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 F2 1.9922(12) . y Co1 F1 2.0955(12) . y Co1 N14 2.1377(18) . y Co1 N12 2.1614(18) . y Co1 N13 2.1975(18) . y Co1 N11 2.3904(17) . y Co2 F2 2.0529(12) 7_655 y Co2 F1 2.0545(12) 7_655 y Co2 N18 2.1336(18) . y Co2 N17 2.1504(19) . y Co2 N16 2.1767(18) . y Co2 N15 2.3159(17) . y N11 C4 1.346(3) . ? N11 C1 1.347(3) . ? C1 C2 1.380(3) . ? C1 C11 1.492(3) . ? C2 C3 1.377(3) . ? C2 H2 0.9500 . ? C3 N15 1.358(3) . ? C3 C31 1.504(3) . ? N15 C4 1.347(3) . ? C4 C5 1.489(3) . ? C5 C6 1.379(3) . ? C5 C10 1.387(3) . ? C6 C7 1.390(3) . ? C6 H6 0.9500 . ? C7 C8 1.379(4) . ? C7 H7 0.9500 . ? C8 C9 1.378(4) . ? C8 H8 0.9500 . ? C9 C10 1.390(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 N12 1.481(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? N12 C22 1.491(3) . ? N12 C12 1.497(3) . ? C12 C13 1.527(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.500(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N13 1.350(3) . ? C14 C15 1.392(3) . ? C15 C16 1.376(4) . ? C15 H15 0.9500 . ? C16 C17 1.375(4) . ? C16 H16 0.9500 . ? C17 C18 1.384(4) . ? C17 H17 0.9500 . ? C18 N13 1.346(3) . ? C18 H18 0.9500 . ? C22 C23 1.530(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.503(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N14 1.351(3) . ? C24 C25 1.387(3) . ? C25 C26 1.381(4) . ? C25 H25 0.9500 . ? C26 C27 1.381(4) . ? C26 H26 0.9500 . ? C27 C28 1.384(3) . ? C27 H27 0.9500 . ? C28 N14 1.347(3) . ? C28 H28 0.9500 . ? C31 N16 1.481(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? N16 C42 1.493(3) . ? N16 C32 1.505(3) . ? C32 C33 1.520(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.499(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 N17 1.351(3) . ? C34 C35 1.394(3) . ? C35 C36 1.378(4) . ? C35 H35 0.9500 . ? C36 C37 1.379(5) . ? C36 H36 0.9500 . ? C37 C38 1.374(4) . ? C37 H37 0.9500 . ? C38 N17 1.341(3) . ? C38 H38 0.9500 . ? C42 C43 1.526(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.508(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 N18 1.357(3) . ? C44 C45 1.389(3) . ? C45 C46 1.378(4) . ? C45 H45 0.9500 . ? C46 C47 1.382(4) . ? C46 H46 0.9500 . ? C47 C48 1.380(3) . ? C47 H47 0.9500 . ? C48 N18 1.346(3) . ? C48 H48 0.9500 . ? F1 Co2 2.0545(12) 7_655 ? F2 Co2 2.0529(12) 7_655 ? O50 C50 1.426(5) . ? O50 H50X 0.8400 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? O60 C60 1.377(10) . ? O60 H60X 0.8400 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? B1 F14 1.377(3) . ? B1 F11 1.388(3) . ? B1 F12 1.397(3) . ? B1 F13 1.399(3) . ? B2 F23 1.372(8) . ? B2 F24 1.381(8) . ? B2 F21 1.383(8) . ? B2 F22 1.393(8) . ? B21 F25 1.370(15) . ? B21 F27 1.370(15) . ? B21 F28 1.375(15) . ? B21 F26 1.386(15) . ? 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 F2 Co1 F1 76.70(5) . . y F2 Co1 N14 92.76(6) . . y F1 Co1 N14 169.20(6) . . y F2 Co1 N12 169.81(6) . . y F1 Co1 N12 94.30(6) . . y N14 Co1 N12 95.99(7) . . y F2 Co1 N13 97.38(6) . . y F1 Co1 N13 97.24(6) . . y N14 Co1 N13 86.33(7) . . y N12 Co1 N13 88.40(7) . . y F2 Co1 N11 99.88(5) . . y F1 Co1 N11 86.06(5) . . y N14 Co1 N11 93.54(6) . . y N12 Co1 N11 74.42(6) . . y N13 Co1 N11 162.72(7) . . y F2 Co2 F1 76.31(5) 7_655 7_655 y F2 Co2 N18 172.57(6) 7_655 . y F1 Co2 N18 97.28(6) 7_655 . y F2 Co2 N17 97.05(6) 7_655 . y F1 Co2 N17 89.35(6) 7_655 . y N18 Co2 N17 86.52(7) . . y F2 Co2 N16 91.30(6) 7_655 . y F1 Co2 N16 167.21(6) 7_655 . y N18 Co2 N16 95.29(7) . . y N17 Co2 N16 89.04(7) . . y F2 Co2 N15 87.60(5) 7_655 . y F1 Co2 N15 106.14(5) 7_655 . y N18 Co2 N15 90.66(6) . . y N17 Co2 N15 164.49(7) . . y N16 Co2 N15 76.02(6) . . y C4 N11 C1 116.79(17) . . ? C4 N11 Co1 135.51(13) . . ? C1 N11 Co1 105.59(13) . . ? N11 C1 C2 121.89(19) . . ? N11 C1 C11 117.99(18) . . ? C2 C1 C11 120.11(18) . . ? C3 C2 C1 117.63(19) . . ? C3 C2 H2 121.2 . . ? C1 C2 H2 121.2 . . ? N15 C3 C2 121.69(19) . . ? N15 C3 C31 117.61(18) . . ? C2 C3 C31 120.60(18) . . ? C4 N15 C3 116.54(17) . . ? C4 N15 Co2 136.17(14) . . ? C3 N15 Co2 107.28(13) . . ? N11 C4 N15 125.03(18) . . ? N11 C4 C5 116.85(17) . . ? N15 C4 C5 118.00(17) . . ? C6 C5 C10 119.7(2) . . ? C6 C5 C4 121.34(19) . . ? C10 C5 C4 118.97(19) . . ? C5 C6 C7 120.4(2) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C8 C7 C6 119.8(2) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C9 C8 C7 120.0(2) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 120.2(2) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C5 C10 C9 119.8(2) . . ? C5 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? N12 C11 C1 113.54(17) . . ? N12 C11 H11A 108.9 . . ? C1 C11 H11A 108.9 . . ? N12 C11 H11B 108.9 . . ? C1 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C11 N12 C22 109.48(17) . . ? C11 N12 C12 106.62(16) . . ? C22 N12 C12 108.53(17) . . ? C11 N12 Co1 104.16(12) . . ? C22 N12 Co1 109.99(13) . . ? C12 N12 Co1 117.73(14) . . ? N12 C12 C13 112.40(18) . . ? N12 C12 H12A 109.1 . . ? C13 C12 H12A 109.1 . . ? N12 C12 H12B 109.1 . . ? C13 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C12 109.22(19) . . ? C14 C13 H13A 109.8 . . ? C12 C13 H13A 109.8 . . ? C14 C13 H13B 109.8 . . ? C12 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? N13 C14 C15 121.8(2) . . ? N13 C14 C13 116.67(19) . . ? C15 C14 C13 121.4(2) . . ? C16 C15 C14 119.7(3) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C17 C16 C15 118.7(2) . . ? C17 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? C16 C17 C18 119.3(2) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? N13 C18 C17 122.8(2) . . ? N13 C18 H18 118.6 . . ? C17 C18 H18 118.6 . . ? C18 N13 C14 117.8(2) . . ? C18 N13 Co1 121.02(16) . . ? C14 N13 Co1 120.79(15) . . ? N12 C22 C23 113.37(19) . . ? N12 C22 H22A 108.9 . . ? C23 C22 H22A 108.9 . . ? N12 C22 H22B 108.9 . . ? C23 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C24 C23 C22 117.13(19) . . ? C24 C23 H23A 108.0 . . ? C22 C23 H23A 108.0 . . ? C24 C23 H23B 108.0 . . ? C22 C23 H23B 108.0 . . ? H23A C23 H23B 107.3 . . ? N14 C24 C25 120.9(2) . . ? N14 C24 C23 119.44(19) . . ? C25 C24 C23 119.6(2) . . ? C26 C25 C24 120.5(2) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C27 C26 C25 118.4(2) . . ? C27 C26 H26 120.8 . . ? C25 C26 H26 120.8 . . ? C26 C27 C28 118.7(2) . . ? C26 C27 H27 120.7 . . ? C28 C27 H27 120.7 . . ? N14 C28 C27 123.0(2) . . ? N14 C28 H28 118.5 . . ? C27 C28 H28 118.5 . . ? C28 N14 C24 118.35(19) . . ? C28 N14 Co1 117.11(16) . . ? C24 N14 Co1 124.22(15) . . ? N16 C31 C3 111.02(17) . . ? N16 C31 H31A 109.4 . . ? C3 C31 H31A 109.4 . . ? N16 C31 H31B 109.4 . . ? C3 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C31 N16 C42 108.98(17) . . ? C31 N16 C32 107.79(17) . . ? C42 N16 C32 108.36(17) . . ? C31 N16 Co2 102.39(12) . . ? C42 N16 Co2 111.27(13) . . ? C32 N16 Co2 117.62(13) . . ? N16 C32 C33 113.26(19) . . ? N16 C32 H32A 108.9 . . ? C33 C32 H32A 108.9 . . ? N16 C32 H32B 108.9 . . ? C33 C32 H32B 108.9 . . ? H32A C32 H32B 107.7 . . ? C34 C33 C32 111.5(2) . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33B 109.3 . . ? C32 C33 H33B 109.3 . . ? H33A C33 H33B 108.0 . . ? N17 C34 C35 120.6(3) . . ? N17 C34 C33 117.3(2) . . ? C35 C34 C33 122.0(2) . . ? C36 C35 C34 119.8(3) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 119.4(3) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? C38 C37 C36 118.1(3) . . ? C38 C37 H37 120.9 . . ? C36 C37 H37 120.9 . . ? N17 C38 C37 123.6(3) . . ? N17 C38 H38 118.2 . . ? C37 C38 H38 118.2 . . ? C38 N17 C34 118.6(2) . . ? C38 N17 Co2 119.68(17) . . ? C34 N17 Co2 121.57(16) . . ? N16 C42 C43 113.08(18) . . ? N16 C42 H42A 109.0 . . ? C43 C42 H42A 109.0 . . ? N16 C42 H42B 109.0 . . ? C43 C42 H42B 109.0 . . ? H42A C42 H42B 107.8 . . ? C44 C43 C42 116.10(19) . . ? C44 C43 H43A 108.3 . . ? C42 C43 H43A 108.3 . . ? C44 C43 H43B 108.3 . . ? C42 C43 H43B 108.3 . . ? H43A C43 H43B 107.4 . . ? N18 C44 C45 120.5(2) . . ? N18 C44 C43 119.4(2) . . ? C45 C44 C43 120.0(2) . . ? C46 C45 C44 120.6(2) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C45 C46 C47 118.9(2) . . ? C45 C46 H46 120.6 . . ? C47 C46 H46 120.6 . . ? C48 C47 C46 118.1(2) . . ? C48 C47 H47 120.9 . . ? C46 C47 H47 120.9 . . ? N18 C48 C47 123.7(2) . . ? N18 C48 H48 118.2 . . ? C47 C48 H48 118.2 . . ? C48 N18 C44 118.2(2) . . ? C48 N18 Co2 117.24(15) . . ? C44 N18 Co2 124.55(16) . . ? Co2 F1 Co1 100.64(5) 7_655 . ? Co1 F2 Co2 104.29(5) . 7_655 ? C50 O50 H50X 109.5 . . ? O50 C50 H50A 109.5 . . ? O50 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? O50 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C60 O60 H60X 109.5 . . ? O60 C60 H60A 109.5 . . ? O60 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? O60 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? F14 B1 F11 109.7(2) . . ? F14 B1 F12 110.2(2) . . ? F11 B1 F12 110.7(2) . . ? F14 B1 F13 108.8(2) . . ? F11 B1 F13 108.4(2) . . ? F12 B1 F13 109.0(2) . . ? F23 B2 F24 111.5(5) . . ? F23 B2 F21 110.0(6) . . ? F24 B2 F21 107.0(7) . . ? F23 B2 F22 108.1(7) . . ? F24 B2 F22 111.2(6) . . ? F21 B2 F22 108.9(6) . . ? F25 B21 F27 111.1(17) . . ? F25 B21 F28 111.2(19) . . ? F27 B21 F28 111.0(13) . . ? F25 B21 F26 112.4(18) . . ? F27 B21 F26 109.1(16) . . ? F28 B21 F26 101.7(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F2 Co1 N11 C4 23.39(19) . . . . ? F1 Co1 N11 C4 99.15(18) . . . . ? N14 Co1 N11 C4 -70.04(19) . . . . ? N12 Co1 N11 C4 -165.3(2) . . . . ? N13 Co1 N11 C4 -159.1(2) . . . . ? F2 Co1 N11 C1 -138.78(12) . . . . ? F1 Co1 N11 C1 -63.03(12) . . . . ? N14 Co1 N11 C1 127.79(13) . . . . ? N12 Co1 N11 C1 32.55(13) . . . . ? N13 Co1 N11 C1 38.8(3) . . . . ? C4 N11 C1 C2 -0.9(3) . . . . ? Co1 N11 C1 C2 165.18(16) . . . . ? C4 N11 C1 C11 178.25(18) . . . . ? Co1 N11 C1 C11 -15.7(2) . . . . ? N11 C1 C2 C3 -3.8(3) . . . . ? C11 C1 C2 C3 177.03(19) . . . . ? C1 C2 C3 N15 3.6(3) . . . . ? C1 C2 C3 C31 179.89(19) . . . . ? C2 C3 N15 C4 1.4(3) . . . . ? C31 C3 N15 C4 -175.03(18) . . . . ? C2 C3 N15 Co2 -178.71(16) . . . . ? C31 C3 N15 Co2 4.8(2) . . . . ? F2 Co2 N15 C4 -114.81(19) 7_655 . . . ? F1 Co2 N15 C4 -39.8(2) 7_655 . . . ? N18 Co2 N15 C4 58.0(2) . . . . ? N17 Co2 N15 C4 137.3(3) . . . . ? N16 Co2 N15 C4 153.3(2) . . . . ? F2 Co2 N15 C3 65.35(13) 7_655 . . . ? F1 Co2 N15 C3 140.35(12) 7_655 . . . ? N18 Co2 N15 C3 -121.87(14) . . . . ? N17 Co2 N15 C3 -42.6(3) . . . . ? N16 Co2 N15 C3 -26.59(13) . . . . ? C1 N11 C4 N15 6.6(3) . . . . ? Co1 N11 C4 N15 -154.15(15) . . . . ? C1 N11 C4 C5 -169.45(17) . . . . ? Co1 N11 C4 C5 29.8(3) . . . . ? C3 N15 C4 N11 -6.8(3) . . . . ? Co2 N15 C4 N11 173.38(14) . . . . ? C3 N15 C4 C5 169.17(17) . . . . ? Co2 N15 C4 C5 -10.7(3) . . . . ? N11 C4 C5 C6 -113.9(2) . . . . ? N15 C4 C5 C6 69.8(3) . . . . ? N11 C4 C5 C10 67.7(3) . . . . ? N15 C4 C5 C10 -108.6(2) . . . . ? C10 C5 C6 C7 -1.7(3) . . . . ? C4 C5 C6 C7 179.9(2) . . . . ? C5 C6 C7 C8 1.8(4) . . . . ? C6 C7 C8 C9 0.3(4) . . . . ? C7 C8 C9 C10 -2.5(4) . . . . ? C6 C5 C10 C9 -0.5(4) . . . . ? C4 C5 C10 C9 178.0(2) . . . . ? C8 C9 C10 C5 2.6(4) . . . . ? N11 C1 C11 N12 -20.7(3) . . . . ? C2 C1 C11 N12 158.43(19) . . . . ? C1 C11 N12 C22 -69.0(2) . . . . ? C1 C11 N12 C12 173.78(18) . . . . ? C1 C11 N12 Co1 48.6(2) . . . . ? F2 Co1 N12 C11 15.9(4) . . . . ? F1 Co1 N12 C11 43.54(13) . . . . ? N14 Co1 N12 C11 -133.18(13) . . . . ? N13 Co1 N12 C11 140.69(13) . . . . ? N11 Co1 N12 C11 -41.16(12) . . . . ? F2 Co1 N12 C22 133.2(3) . . . . ? F1 Co1 N12 C22 160.78(13) . . . . ? N14 Co1 N12 C22 -15.94(14) . . . . ? N13 Co1 N12 C22 -102.07(14) . . . . ? N11 Co1 N12 C22 76.08(13) . . . . ? F2 Co1 N12 C12 -101.9(3) . . . . ? F1 Co1 N12 C12 -74.24(15) . . . . ? N14 Co1 N12 C12 109.05(15) . . . . ? N13 Co1 N12 C12 22.91(15) . . . . ? N11 Co1 N12 C12 -158.93(16) . . . . ? C11 N12 C12 C13 -92.8(2) . . . . ? C22 N12 C12 C13 149.34(18) . . . . ? Co1 N12 C12 C13 23.6(2) . . . . ? N12 C12 C13 C14 -79.9(2) . . . . ? C12 C13 C14 N13 68.1(3) . . . . ? C12 C13 C14 C15 -107.5(2) . . . . ? N13 C14 C15 C16 0.6(4) . . . . ? C13 C14 C15 C16 176.0(2) . . . . ? C14 C15 C16 C17 -0.3(4) . . . . ? C15 C16 C17 C18 -0.3(4) . . . . ? C16 C17 C18 N13 0.7(4) . . . . ? C17 C18 N13 C14 -0.4(4) . . . . ? C17 C18 N13 Co1 -173.2(2) . . . . ? C15 C14 N13 C18 -0.3(3) . . . . ? C13 C14 N13 C18 -175.9(2) . . . . ? C15 C14 N13 Co1 172.61(18) . . . . ? C13 C14 N13 Co1 -3.0(3) . . . . ? F2 Co1 N13 C18 -51.52(18) . . . . ? F1 Co1 N13 C18 -128.96(17) . . . . ? N14 Co1 N13 C18 40.80(18) . . . . ? N12 Co1 N13 C18 136.91(18) . . . . ? N11 Co1 N13 C18 130.9(2) . . . . ? F2 Co1 N13 C14 135.85(17) . . . . ? F1 Co1 N13 C14 58.41(17) . . . . ? N14 Co1 N13 C14 -131.83(18) . . . . ? N12 Co1 N13 C14 -35.72(17) . . . . ? N11 Co1 N13 C14 -41.7(3) . . . . ? C11 N12 C22 C23 171.01(18) . . . . ? C12 N12 C22 C23 -73.0(2) . . . . ? Co1 N12 C22 C23 57.1(2) . . . . ? N12 C22 C23 C24 -80.6(3) . . . . ? C22 C23 C24 N14 43.8(3) . . . . ? C22 C23 C24 C25 -139.5(2) . . . . ? N14 C24 C25 C26 3.3(4) . . . . ? C23 C24 C25 C26 -173.4(2) . . . . ? C24 C25 C26 C27 -1.5(4) . . . . ? C25 C26 C27 C28 -1.3(4) . . . . ? C26 C27 C28 N14 2.7(4) . . . . ? C27 C28 N14 C24 -1.0(3) . . . . ? C27 C28 N14 Co1 172.70(19) . . . . ? C25 C24 N14 C28 -2.0(3) . . . . ? C23 C24 N14 C28 174.7(2) . . . . ? C25 C24 N14 Co1 -175.19(17) . . . . ? C23 C24 N14 Co1 1.5(3) . . . . ? F2 Co1 N14 C28 -1.09(17) . . . . ? F1 Co1 N14 C28 11.4(4) . . . . ? N12 Co1 N14 C28 173.69(17) . . . . ? N13 Co1 N14 C28 -98.31(17) . . . . ? N11 Co1 N14 C28 99.00(17) . . . . ? F2 Co1 N14 C24 172.21(17) . . . . ? F1 Co1 N14 C24 -175.3(3) . . . . ? N12 Co1 N14 C24 -13.01(18) . . . . ? N13 Co1 N14 C24 74.98(18) . . . . ? N11 Co1 N14 C24 -87.70(17) . . . . ? N15 C3 C31 N16 32.8(3) . . . . ? C2 C3 C31 N16 -143.64(19) . . . . ? C3 C31 N16 C42 65.1(2) . . . . ? C3 C31 N16 C32 -177.51(17) . . . . ? C3 C31 N16 Co2 -52.83(18) . . . . ? F2 Co2 N16 C31 -45.95(12) 7_655 . . . ? F1 Co2 N16 C31 -60.1(3) 7_655 . . . ? N18 Co2 N16 C31 130.61(12) . . . . ? N17 Co2 N16 C31 -142.98(13) . . . . ? N15 Co2 N16 C31 41.25(12) . . . . ? F2 Co2 N16 C42 -162.24(13) 7_655 . . . ? F1 Co2 N16 C42 -176.4(2) 7_655 . . . ? N18 Co2 N16 C42 14.32(14) . . . . ? N17 Co2 N16 C42 100.74(14) . . . . ? N15 Co2 N16 C42 -75.04(13) . . . . ? F2 Co2 N16 C32 71.95(16) 7_655 . . . ? F1 Co2 N16 C32 57.8(3) 7_655 . . . ? N18 Co2 N16 C32 -111.49(16) . . . . ? N17 Co2 N16 C32 -25.08(16) . . . . ? N15 Co2 N16 C32 159.15(17) . . . . ? C31 N16 C32 C33 96.1(2) . . . . ? C42 N16 C32 C33 -146.1(2) . . . . ? Co2 N16 C32 C33 -18.9(3) . . . . ? N16 C32 C33 C34 74.5(3) . . . . ? C32 C33 C34 N17 -66.9(3) . . . . ? C32 C33 C34 C35 111.0(3) . . . . ? N17 C34 C35 C36 0.0(4) . . . . ? C33 C34 C35 C36 -177.9(3) . . . . ? C34 C35 C36 C37 -0.2(4) . . . . ? C35 C36 C37 C38 -0.1(4) . . . . ? C36 C37 C38 N17 0.7(4) . . . . ? C37 C38 N17 C34 -1.0(4) . . . . ? C37 C38 N17 Co2 174.1(2) . . . . ? C35 C34 N17 C38 0.6(3) . . . . ? C33 C34 N17 C38 178.6(2) . . . . ? C35 C34 N17 Co2 -174.42(19) . . . . ? C33 C34 N17 Co2 3.6(3) . . . . ? F2 Co2 N17 C38 128.76(17) 7_655 . . . ? F1 Co2 N17 C38 52.64(18) 7_655 . . . ? N18 Co2 N17 C38 -44.70(18) . . . . ? N16 Co2 N17 C38 -140.06(18) . . . . ? N15 Co2 N17 C38 -124.5(3) . . . . ? F2 Co2 N17 C34 -56.29(18) 7_655 . . . ? F1 Co2 N17 C34 -132.41(18) 7_655 . . . ? N18 Co2 N17 C34 130.26(18) . . . . ? N16 Co2 N17 C34 34.90(18) . . . . ? N15 Co2 N17 C34 50.4(4) . . . . ? C31 N16 C42 C43 -167.45(18) . . . . ? C32 N16 C42 C43 75.5(2) . . . . ? Co2 N16 C42 C43 -55.3(2) . . . . ? N16 C42 C43 C44 81.0(3) . . . . ? C42 C43 C44 N18 -48.3(3) . . . . ? C42 C43 C44 C45 134.2(2) . . . . ? N18 C44 C45 C46 -1.1(4) . . . . ? C43 C44 C45 C46 176.4(2) . . . . ? C44 C45 C46 C47 -0.8(4) . . . . ? C45 C46 C47 C48 1.6(4) . . . . ? C46 C47 C48 N18 -0.6(4) . . . . ? C47 C48 N18 C44 -1.3(3) . . . . ? C47 C48 N18 Co2 -179.37(18) . . . . ? C45 C44 N18 C48 2.1(3) . . . . ? C43 C44 N18 C48 -175.4(2) . . . . ? C45 C44 N18 Co2 -179.95(18) . . . . ? C43 C44 N18 Co2 2.6(3) . . . . ? F2 Co2 N18 C48 -17.9(6) 7_655 . . . ? F1 Co2 N18 C48 12.19(16) 7_655 . . . ? N17 Co2 N18 C48 101.09(16) . . . . ? N16 Co2 N18 C48 -170.20(16) . . . . ? N15 Co2 N18 C48 -94.17(16) . . . . ? F2 Co2 N18 C44 164.2(4) 7_655 . . . ? F1 Co2 N18 C44 -165.79(17) 7_655 . . . ? N17 Co2 N18 C44 -76.89(18) . . . . ? N16 Co2 N18 C44 11.82(18) . . . . ? N15 Co2 N18 C44 87.85(18) . . . . ? F2 Co1 F1 Co2 -10.92(5) . . . 7_655 ? N14 Co1 F1 Co2 -23.8(3) . . . 7_655 ? N12 Co1 F1 Co2 173.91(6) . . . 7_655 ? N13 Co1 F1 Co2 84.99(7) . . . 7_655 ? N11 Co1 F1 Co2 -112.06(6) . . . 7_655 ? F1 Co1 F2 Co2 11.09(5) . . . 7_655 ? N14 Co1 F2 Co2 -171.30(7) . . . 7_655 ? N12 Co1 F2 Co2 39.5(4) . . . 7_655 ? N13 Co1 F2 Co2 -84.65(7) . . . 7_655 ? N11 Co1 F2 Co2 94.61(6) . . . 7_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O50 H50X F21 0.84 2.10 2.902(7) 158.7 . O50 H50X F23 0.84 2.52 3.123(4) 129.4 . O50 H50X F25 0.84 2.20 3.02(3) 165.4 . O60 H60X F24 0.84 2.32 2.963(4) 133.3 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.791 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.063 # Attachment 'wag273.cif' data_wag273 _database_code_depnum_ccdc_archive 'CCDC 842532' #TrackingRef 'wag273.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H94 B4 F20 N16 O3 Zn4' _chemical_formula_weight 2036.45 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7624(6) _cell_length_b 12.1889(7) _cell_length_c 17.1948(11) _cell_angle_alpha 70.585(3) _cell_angle_beta 73.815(3) _cell_angle_gamma 69.180(3) _cell_volume 2136.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 91(2) _cell_measurement_reflns_used 9493 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 26.39 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1042 _exptl_absorpt_coefficient_mu 1.212 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7935 _exptl_absorpt_correction_T_max 0.9308 _exptl_absorpt_process_details 'SCALE (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 91(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39976 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.39 _reflns_number_total 8759 _reflns_number_gt 6992 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. [Zn(II)4(LEt)2)(F)4](BF4)4.2MeOH.H2O Half of this in the asym unit. Other half of complex generated by center of inversion. All non-H ANIS except for two disordered O atoms of water, each of 0.25 occup. All BF4 are ordered. One MeOH with full occup. All H calc and ride except that on MeOH O atom which was inserted using HFIX 147 and those on water O atom which were found from the map, HIMP'ed to 0.85A, and AFIX 01'ed with U(H)=1.2U(O). H-bonds are present between MeOH and F21; also weak H-bonds between 0.25 waters (O60; O61) and F23. The residual e density occurs in the same region of space as the two 0.25 occup water molecules and their symmetry generated equivalents (Q2 is just +0.58). NB. only one of these 4 0.25 occup water molecules is present at any one time. ; _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^)+(0.0408P)^2^+2.6777P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8759 _refine_ls_number_parameters 587 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0965 _refine_ls_wR_factor_gt 0.0893 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.77201(3) 0.11115(3) 0.277462(18) 0.01302(9) Uani 1 1 d . . . Zn2 Zn 0.49979(3) -0.27344(3) 0.746266(18) 0.01273(8) Uani 1 1 d . . . N11 N 0.68479(19) -0.04889(19) 0.43258(13) 0.0127(4) Uani 1 1 d . . . C1 C 0.6774(2) -0.2496(2) 0.45439(16) 0.0144(5) Uani 1 1 d . . . H1 H 0.6907 -0.3163 0.4327 0.017 Uiso 1 1 calc R . . C2 C 0.7028(2) -0.1435(2) 0.40302(16) 0.0125(5) Uani 1 1 d . . . C3 C 0.6317(2) -0.2552(2) 0.53873(16) 0.0137(5) Uani 1 1 d . . . N15 N 0.61114(19) -0.16105(19) 0.56984(13) 0.0127(4) Uani 1 1 d . . . C4 C 0.6385(2) -0.0610(2) 0.51518(16) 0.0122(5) Uani 1 1 d . . . C5 C 0.6202(2) 0.0419(2) 0.55003(16) 0.0131(5) Uani 1 1 d . . . C6 C 0.6457(2) 0.1486(2) 0.49767(17) 0.0153(5) Uani 1 1 d . . . H6 H 0.6719 0.1568 0.4391 0.018 Uiso 1 1 calc R . . C7 C 0.6334(3) 0.2429(3) 0.53014(17) 0.0187(6) Uani 1 1 d . . . H7 H 0.6519 0.3148 0.4939 0.022 Uiso 1 1 calc R . . C8 C 0.5940(3) 0.2325(2) 0.61542(17) 0.0190(6) Uani 1 1 d . . . H8 H 0.5861 0.2970 0.6378 0.023 Uiso 1 1 calc R . . C9 C 0.5663(3) 0.1274(3) 0.66803(18) 0.0192(6) Uani 1 1 d . . . H9 H 0.5384 0.1203 0.7264 0.023 Uiso 1 1 calc R . . C10 C 0.5792(2) 0.0328(2) 0.63550(17) 0.0157(5) Uani 1 1 d . . . H10 H 0.5600 -0.0388 0.6718 0.019 Uiso 1 1 calc R . . C11 C 0.7541(2) -0.1364(2) 0.31106(16) 0.0142(5) Uani 1 1 d . . . H11A H 0.7888 -0.2200 0.3038 0.017 Uiso 1 1 calc R . . H11B H 0.6854 -0.0936 0.2794 0.017 Uiso 1 1 calc R . . N12 N 0.85213(19) -0.07286(19) 0.27417(13) 0.0128(4) Uani 1 1 d . . . C12 C 0.9000(2) -0.0842(2) 0.18503(16) 0.0164(6) Uani 1 1 d . . . H12A H 0.8966 -0.1632 0.1831 0.020 Uiso 1 1 calc R . . H12B H 0.9880 -0.0853 0.1695 0.020 Uiso 1 1 calc R . . C13 C 0.8296(2) 0.0170(2) 0.11926(17) 0.0167(6) Uani 1 1 d . . . H13A H 0.8442 -0.0123 0.0691 0.020 Uiso 1 1 calc R . . H13B H 0.7398 0.0363 0.1424 0.020 Uiso 1 1 calc R . . C14 C 0.8690(2) 0.1303(2) 0.09392(17) 0.0162(6) Uani 1 1 d . . . C15 C 0.9246(2) 0.1763(3) 0.01236(18) 0.0213(6) Uani 1 1 d . . . H15 H 0.9370 0.1372 -0.0300 0.026 Uiso 1 1 calc R . . C16 C 0.9615(3) 0.2795(3) -0.00656(19) 0.0266(7) Uani 1 1 d . . . H16 H 1.0012 0.3109 -0.0617 0.032 Uiso 1 1 calc R . . C17 C 0.9398(3) 0.3360(3) 0.05576(19) 0.0248(7) Uani 1 1 d . . . H17 H 0.9638 0.4073 0.0441 0.030 Uiso 1 1 calc R . . C18 C 0.8829(2) 0.2878(3) 0.13505(18) 0.0204(6) Uani 1 1 d . . . H18 H 0.8671 0.3277 0.1776 0.024 Uiso 1 1 calc R . . N13 N 0.84852(19) 0.1859(2) 0.15457(14) 0.0154(5) Uani 1 1 d . . . C22 C 0.9568(2) -0.1399(2) 0.32102(17) 0.0169(6) Uani 1 1 d . . . H22A H 0.9993 -0.2189 0.3071 0.020 Uiso 1 1 calc R . . H22B H 0.9230 -0.1568 0.3819 0.020 Uiso 1 1 calc R . . C23 C 1.0513(2) -0.0709(3) 0.30165(17) 0.0188(6) Uani 1 1 d . . . H23A H 1.1295 -0.1300 0.3178 0.023 Uiso 1 1 calc R . . H23B H 1.0682 -0.0359 0.2402 0.023 Uiso 1 1 calc R . . C24 C 1.0161(2) 0.0292(3) 0.34355(16) 0.0169(6) Uani 1 1 d . . . C25 C 1.0955(3) 0.0341(3) 0.38798(18) 0.0215(6) Uani 1 1 d . . . H25 H 1.1696 -0.0301 0.3961 0.026 Uiso 1 1 calc R . . C26 C 1.0668(3) 0.1324(3) 0.42040(18) 0.0254(7) Uani 1 1 d . . . H26 H 1.1205 0.1362 0.4511 0.030 Uiso 1 1 calc R . . C27 C 0.9594(3) 0.2245(3) 0.40759(19) 0.0242(6) Uani 1 1 d . . . H27 H 0.9389 0.2942 0.4277 0.029 Uiso 1 1 calc R . . C28 C 0.8818(2) 0.2137(2) 0.36478(17) 0.0174(6) Uani 1 1 d . . . H28 H 0.8070 0.2770 0.3567 0.021 Uiso 1 1 calc R . . N14 N 0.90726(19) 0.1179(2) 0.33429(13) 0.0149(5) Uani 1 1 d . . . C31 C 0.6055(2) -0.3707(2) 0.59649(16) 0.0143(5) Uani 1 1 d . . . H31A H 0.5181 -0.3640 0.5997 0.017 Uiso 1 1 calc R . . H31B H 0.6576 -0.4389 0.5715 0.017 Uiso 1 1 calc R . . N16 N 0.62808(19) -0.40091(19) 0.68343(13) 0.0134(5) Uani 1 1 d . . . C32 C 0.6111(2) -0.5250(2) 0.72811(17) 0.0157(5) Uani 1 1 d . . . H32A H 0.6573 -0.5611 0.7751 0.019 Uiso 1 1 calc R . . H32B H 0.6488 -0.5772 0.6887 0.019 Uiso 1 1 calc R . . C33 C 0.4773(2) -0.5276(2) 0.76281(17) 0.0169(6) Uani 1 1 d . . . H33A H 0.4245 -0.4683 0.7223 0.020 Uiso 1 1 calc R . . H33B H 0.4721 -0.6093 0.7688 0.020 Uiso 1 1 calc R . . C34 C 0.4282(2) -0.4980(2) 0.84637(17) 0.0174(6) Uani 1 1 d . . . C35 C 0.3777(3) -0.5758(3) 0.91577(18) 0.0222(6) Uani 1 1 d . . . H35 H 0.3728 -0.6496 0.9113 0.027 Uiso 1 1 calc R . . C36 C 0.3344(3) -0.5448(3) 0.99152(18) 0.0256(7) Uani 1 1 d . . . H36 H 0.2982 -0.5965 1.0392 0.031 Uiso 1 1 calc R . . C37 C 0.3443(3) -0.4382(3) 0.99726(17) 0.0219(6) Uani 1 1 d . . . H37 H 0.3158 -0.4157 1.0488 0.026 Uiso 1 1 calc R . . C38 C 0.3965(2) -0.3655(2) 0.92655(17) 0.0173(6) Uani 1 1 d . . . H38 H 0.4038 -0.2923 0.9302 0.021 Uiso 1 1 calc R . . N17 N 0.43758(19) -0.3941(2) 0.85228(13) 0.0152(5) Uani 1 1 d . . . C42 C 0.7605(2) -0.4104(2) 0.67881(17) 0.0157(5) Uani 1 1 d . . . H42A H 0.7797 -0.3378 0.6370 0.019 Uiso 1 1 calc R . . H42B H 0.8143 -0.4824 0.6584 0.019 Uiso 1 1 calc R . . C43 C 0.7921(2) -0.4210(2) 0.76176(17) 0.0172(6) Uani 1 1 d . . . H43A H 0.7548 -0.4808 0.8063 0.021 Uiso 1 1 calc R . . H43B H 0.8830 -0.4542 0.7575 0.021 Uiso 1 1 calc R . . C44 C 0.7511(2) -0.3062(2) 0.78896(16) 0.0157(6) Uani 1 1 d . . . C45 C 0.8342(3) -0.2708(3) 0.81256(17) 0.0195(6) Uani 1 1 d . . . H45 H 0.9190 -0.3164 0.8072 0.023 Uiso 1 1 calc R . . C46 C 0.7941(3) -0.1699(3) 0.84374(18) 0.0225(6) Uani 1 1 d . . . H46 H 0.8508 -0.1455 0.8595 0.027 Uiso 1 1 calc R . . C47 C 0.6702(3) -0.1051(3) 0.85157(17) 0.0205(6) Uani 1 1 d . . . H47 H 0.6396 -0.0363 0.8739 0.025 Uiso 1 1 calc R . . C48 C 0.5918(3) -0.1428(3) 0.82600(16) 0.0185(6) Uani 1 1 d . . . H48 H 0.5068 -0.0978 0.8309 0.022 Uiso 1 1 calc R . . N18 N 0.6302(2) -0.2403(2) 0.79453(13) 0.0156(5) Uani 1 1 d . . . F1 F 0.64700(13) 0.25752(13) 0.30783(9) 0.0152(3) Uani 1 1 d . . . F2 F 0.61334(13) 0.11352(13) 0.24756(9) 0.0156(3) Uani 1 1 d . . . O50 O 0.6261(2) 0.8812(2) 0.14796(14) 0.0363(6) Uani 1 1 d . . . H50X H 0.6569 0.8076 0.1712 0.044 Uiso 1 1 calc R . . C50 C 0.6349(3) 0.8956(3) 0.06212(19) 0.0305(7) Uani 1 1 d . . . H50A H 0.6187 0.9821 0.0326 0.037 Uiso 1 1 calc R . . H50B H 0.5740 0.8638 0.0548 0.037 Uiso 1 1 calc R . . H50C H 0.7183 0.8510 0.0391 0.037 Uiso 1 1 calc R . . O60 O 0.9428(9) 0.4759(9) 0.4814(6) 0.039(2) Uiso 0.25 1 d P A 1 H60X H 0.9410 0.5096 0.4297 0.047 Uiso 0.25 1 d P B 1 H60Y H 0.8739 0.4611 0.5049 0.047 Uiso 0.25 1 d P C 1 O61 O 0.9976(9) 0.4581(7) 0.5046(6) 0.028(2) Uiso 0.25 1 d P . 2 H61X H 1.0325 0.4866 0.5282 0.034 Uiso 0.25 1 d P D 2 H61Y H 1.0452 0.3877 0.5033 0.034 Uiso 0.25 1 d P E 2 B1 B 0.2752(3) 0.8199(3) 0.1181(2) 0.0227(7) Uani 1 1 d . . . F11 F 0.34037(18) 0.80976(16) 0.17717(13) 0.0376(5) Uani 1 1 d . . . F12 F 0.35655(18) 0.79889(18) 0.04499(13) 0.0414(5) Uani 1 1 d . . . F13 F 0.20679(17) 0.73650(16) 0.14956(12) 0.0339(4) Uani 1 1 d . . . F14 F 0.19408(15) 0.93767(14) 0.09914(10) 0.0237(4) Uani 1 1 d . . . B2 B 0.8247(4) 0.5489(4) 0.2790(3) 0.0398(10) Uani 1 1 d . . . F21 F 0.7533(3) 0.6510(2) 0.2318(2) 0.0879(11) Uani 1 1 d . . . F22 F 0.7487(2) 0.5014(3) 0.35070(19) 0.0740(8) Uani 1 1 d . . . F23 F 0.91057(19) 0.57751(19) 0.30514(16) 0.0536(6) Uani 1 1 d . . . F24 F 0.8859(2) 0.46317(18) 0.23461(14) 0.0502(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01086(15) 0.01583(17) 0.01393(16) -0.00589(12) -0.00258(11) -0.00355(12) Zn2 0.01161(16) 0.01399(16) 0.01343(16) -0.00434(12) -0.00269(12) -0.00365(12) N11 0.0118(11) 0.0149(11) 0.0126(11) -0.0053(9) -0.0030(8) -0.0031(9) C1 0.0139(13) 0.0167(14) 0.0149(13) -0.0073(11) -0.0028(10) -0.0039(11) C2 0.0082(12) 0.0154(13) 0.0151(13) -0.0063(10) -0.0025(10) -0.0024(10) C3 0.0099(12) 0.0160(13) 0.0154(13) -0.0035(11) -0.0036(10) -0.0037(10) N15 0.0096(10) 0.0164(11) 0.0130(11) -0.0050(9) -0.0016(8) -0.0040(9) C4 0.0064(12) 0.0157(13) 0.0150(13) -0.0048(10) -0.0040(10) -0.0015(10) C5 0.0083(12) 0.0169(13) 0.0160(13) -0.0075(11) -0.0039(10) -0.0018(10) C6 0.0143(13) 0.0192(14) 0.0135(13) -0.0057(11) -0.0019(10) -0.0052(11) C7 0.0200(14) 0.0189(14) 0.0193(15) -0.0054(11) -0.0031(11) -0.0081(11) C8 0.0207(14) 0.0191(14) 0.0224(15) -0.0119(12) -0.0046(11) -0.0052(11) C9 0.0195(14) 0.0247(15) 0.0180(14) -0.0107(12) -0.0017(11) -0.0084(12) C10 0.0139(13) 0.0183(14) 0.0166(14) -0.0056(11) -0.0002(10) -0.0075(11) C11 0.0150(13) 0.0157(13) 0.0137(13) -0.0063(10) 0.0002(10) -0.0061(11) N12 0.0107(10) 0.0167(11) 0.0094(11) -0.0043(9) 0.0000(8) -0.0029(9) C12 0.0168(14) 0.0177(14) 0.0138(14) -0.0077(11) 0.0017(10) -0.0042(11) C13 0.0143(13) 0.0224(15) 0.0153(14) -0.0099(11) -0.0014(10) -0.0038(11) C14 0.0092(13) 0.0192(14) 0.0177(14) -0.0057(11) -0.0041(10) 0.0008(10) C15 0.0162(14) 0.0255(16) 0.0179(15) -0.0052(12) -0.0031(11) -0.0013(12) C16 0.0201(15) 0.0313(17) 0.0202(16) 0.0030(13) -0.0009(12) -0.0088(13) C17 0.0212(15) 0.0229(16) 0.0296(17) 0.0010(13) -0.0070(13) -0.0109(12) C18 0.0150(14) 0.0220(15) 0.0255(16) -0.0050(12) -0.0064(11) -0.0059(11) N13 0.0113(11) 0.0189(12) 0.0161(12) -0.0048(9) -0.0026(9) -0.0043(9) C22 0.0142(13) 0.0175(14) 0.0165(14) -0.0058(11) -0.0037(11) 0.0002(11) C23 0.0116(13) 0.0255(15) 0.0185(14) -0.0081(12) -0.0021(11) -0.0028(11) C24 0.0136(13) 0.0237(15) 0.0134(13) -0.0032(11) -0.0002(10) -0.0084(11) C25 0.0125(13) 0.0293(16) 0.0214(15) -0.0056(12) -0.0046(11) -0.0045(12) C26 0.0218(15) 0.0382(18) 0.0225(16) -0.0088(14) -0.0069(12) -0.0132(13) C27 0.0239(16) 0.0301(17) 0.0268(16) -0.0145(13) -0.0043(12) -0.0111(13) C28 0.0160(14) 0.0192(14) 0.0183(14) -0.0052(11) -0.0024(11) -0.0068(11) N14 0.0130(11) 0.0182(12) 0.0138(11) -0.0027(9) -0.0032(9) -0.0053(9) C31 0.0167(13) 0.0164(13) 0.0127(13) -0.0064(11) -0.0024(10) -0.0060(11) N16 0.0137(11) 0.0149(11) 0.0120(11) -0.0031(9) -0.0018(9) -0.0055(9) C32 0.0188(14) 0.0119(13) 0.0162(14) -0.0033(11) -0.0033(11) -0.0046(11) C33 0.0199(14) 0.0141(13) 0.0187(14) -0.0031(11) -0.0041(11) -0.0078(11) C34 0.0142(13) 0.0172(14) 0.0191(14) -0.0020(11) -0.0059(11) -0.0028(11) C35 0.0240(15) 0.0184(15) 0.0222(15) -0.0005(12) -0.0023(12) -0.0098(12) C36 0.0250(16) 0.0284(17) 0.0176(15) 0.0026(12) -0.0005(12) -0.0116(13) C37 0.0185(14) 0.0307(17) 0.0133(14) -0.0038(12) -0.0030(11) -0.0050(12) C38 0.0153(13) 0.0191(14) 0.0174(14) -0.0054(11) -0.0069(11) -0.0013(11) N17 0.0124(11) 0.0180(12) 0.0145(11) -0.0035(9) -0.0037(9) -0.0033(9) C42 0.0107(13) 0.0169(14) 0.0183(14) -0.0057(11) -0.0009(10) -0.0030(10) C43 0.0141(13) 0.0195(14) 0.0175(14) -0.0048(11) -0.0049(11) -0.0027(11) C44 0.0161(13) 0.0207(14) 0.0097(13) 0.0014(11) -0.0032(10) -0.0088(11) C45 0.0163(14) 0.0250(15) 0.0176(14) -0.0012(12) -0.0044(11) -0.0096(12) C46 0.0249(16) 0.0306(17) 0.0189(15) -0.0038(12) -0.0060(12) -0.0171(13) C47 0.0271(16) 0.0230(15) 0.0161(14) -0.0060(12) -0.0058(12) -0.0106(12) C48 0.0210(14) 0.0218(15) 0.0142(14) -0.0047(11) -0.0046(11) -0.0070(12) N18 0.0159(11) 0.0194(12) 0.0122(11) -0.0028(9) -0.0042(9) -0.0059(9) F1 0.0136(7) 0.0167(8) 0.0170(8) -0.0070(6) -0.0042(6) -0.0029(6) F2 0.0121(7) 0.0170(8) 0.0204(8) -0.0082(6) -0.0038(6) -0.0035(6) O50 0.0471(15) 0.0353(13) 0.0272(13) -0.0083(10) -0.0058(11) -0.0133(12) C50 0.0384(19) 0.0312(18) 0.0260(17) -0.0082(14) -0.0053(14) -0.0148(15) B1 0.0202(17) 0.0224(17) 0.0273(19) -0.0093(14) -0.0043(14) -0.0057(14) F11 0.0414(11) 0.0309(10) 0.0501(12) -0.0092(9) -0.0281(10) -0.0077(9) F12 0.0326(11) 0.0435(12) 0.0487(13) -0.0302(10) 0.0064(9) -0.0056(9) F13 0.0342(10) 0.0247(10) 0.0446(12) 0.0035(8) -0.0186(9) -0.0136(8) F14 0.0229(9) 0.0198(9) 0.0240(9) -0.0048(7) -0.0018(7) -0.0038(7) B2 0.040(2) 0.025(2) 0.062(3) -0.021(2) -0.025(2) 0.0017(17) F21 0.118(2) 0.0286(13) 0.144(3) -0.0211(15) -0.103(2) 0.0068(14) F22 0.0566(16) 0.0767(19) 0.095(2) -0.0489(17) 0.0040(15) -0.0163(14) F23 0.0381(12) 0.0422(13) 0.0973(19) -0.0408(13) -0.0302(12) 0.0034(10) F24 0.0643(15) 0.0341(12) 0.0619(15) -0.0267(11) -0.0154(12) -0.0095(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 F1 1.9860(15) . y Zn1 F2 2.0581(14) . y Zn1 N13 2.085(2) . y Zn1 N12 2.115(2) . y Zn1 N14 2.123(2) . y Zn2 F2 1.9485(15) 2_656 y Zn2 N17 2.064(2) . y Zn2 N16 2.097(2) . y Zn2 F1 2.1027(14) 2_656 y Zn2 N18 2.139(2) . y N11 C2 1.338(3) . ? N11 C4 1.350(3) . ? C1 C2 1.382(4) . ? C1 C3 1.387(4) . ? C1 H1 0.9500 . ? C2 C11 1.512(4) . ? C3 N15 1.342(3) . ? C3 C31 1.507(4) . ? N15 C4 1.350(3) . ? C4 C5 1.488(3) . ? C5 C10 1.392(4) . ? C5 C6 1.393(4) . ? C6 C7 1.384(4) . ? C6 H6 0.9500 . ? C7 C8 1.386(4) . ? C7 H7 0.9500 . ? C8 C9 1.389(4) . ? C8 H8 0.9500 . ? C9 C10 1.387(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 N12 1.493(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? N12 C22 1.495(3) . ? N12 C12 1.513(3) . ? C12 C13 1.534(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.502(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N13 1.349(3) . ? C14 C15 1.391(4) . ? C15 C16 1.383(4) . ? C15 H15 0.9500 . ? C16 C17 1.379(4) . ? C16 H16 0.9500 . ? C17 C18 1.375(4) . ? C17 H17 0.9500 . ? C18 N13 1.350(3) . ? C18 H18 0.9500 . ? C22 C23 1.524(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.496(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N14 1.360(3) . ? C24 C25 1.388(4) . ? C25 C26 1.383(4) . ? C25 H25 0.9500 . ? C26 C27 1.373(4) . ? C26 H26 0.9500 . ? C27 C28 1.385(4) . ? C27 H27 0.9500 . ? C28 N14 1.340(3) . ? C28 H28 0.9500 . ? C31 N16 1.492(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? N16 C42 1.501(3) . ? N16 C32 1.508(3) . ? C32 C33 1.528(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.504(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 N17 1.347(3) . ? C34 C35 1.389(4) . ? C35 C36 1.385(4) . ? C35 H35 0.9500 . ? C36 C37 1.383(4) . ? C36 H36 0.9500 . ? C37 C38 1.376(4) . ? C37 H37 0.9500 . ? C38 N17 1.349(3) . ? C38 H38 0.9500 . ? C42 C43 1.526(4) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.497(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 N18 1.357(3) . ? C44 C45 1.393(4) . ? C45 C46 1.380(4) . ? C45 H45 0.9500 . ? C46 C47 1.382(4) . ? C46 H46 0.9500 . ? C47 C48 1.384(4) . ? C47 H47 0.9500 . ? C48 N18 1.348(4) . ? C48 H48 0.9500 . ? F1 Zn2 2.1028(14) 2_656 ? F2 Zn2 1.9485(15) 2_656 ? O50 C50 1.406(4) . ? O50 H50X 0.8400 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? O60 H60X 0.8483 . ? O60 H60Y 0.8524 . ? O60 H61Y 1.3462 . ? O61 O61 1.000(15) 2_766 ? O61 H60X 1.4625 . ? O61 H60Y 1.4412 . ? O61 H61X 0.8614 . ? O61 H61Y 0.8455 . ? B1 F11 1.386(4) . ? B1 F12 1.389(4) . ? B1 F13 1.395(4) . ? B1 F14 1.402(4) . ? B2 F21 1.371(4) . ? B2 F24 1.371(5) . ? B2 F22 1.391(5) . ? B2 F23 1.398(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Zn1 F2 76.30(6) . . y F1 Zn1 N13 101.20(7) . . y F2 Zn1 N13 94.92(7) . . y F1 Zn1 N12 158.54(7) . . y F2 Zn1 N12 90.26(7) . . y N13 Zn1 N12 96.50(8) . . y F1 Zn1 N14 93.95(7) . . y F2 Zn1 N14 166.54(7) . . y N13 Zn1 N14 96.09(8) . . y N12 Zn1 N14 96.15(8) . . y F2 Zn2 N17 105.57(8) 2_656 . y F2 Zn2 N16 154.24(7) 2_656 . y N17 Zn2 N16 97.96(8) . . y F2 Zn2 F1 76.06(6) 2_656 2_656 y N17 Zn2 F1 89.75(7) . 2_656 y N16 Zn2 F1 93.97(7) . 2_656 y F2 Zn2 N18 90.04(7) 2_656 . y N17 Zn2 N18 98.62(8) . . y N16 Zn2 N18 96.75(8) . . y F1 Zn2 N18 165.33(7) 2_656 . y C2 N11 C4 116.8(2) . . ? C2 C1 C3 117.6(2) . . ? C2 C1 H1 121.2 . . ? C3 C1 H1 121.2 . . ? N11 C2 C1 122.0(2) . . ? N11 C2 C11 119.7(2) . . ? C1 C2 C11 118.3(2) . . ? N15 C3 C1 121.7(2) . . ? N15 C3 C31 119.6(2) . . ? C1 C3 C31 118.7(2) . . ? C3 N15 C4 116.7(2) . . ? N11 C4 N15 125.2(2) . . ? N11 C4 C5 117.9(2) . . ? N15 C4 C5 116.9(2) . . ? C10 C5 C6 118.8(2) . . ? C10 C5 C4 120.8(2) . . ? C6 C5 C4 120.4(2) . . ? C7 C6 C5 120.7(2) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 120.2(3) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C9 119.6(3) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 120.2(3) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C5 120.5(3) . . ? C9 C10 H10 119.7 . . ? C5 C10 H10 119.7 . . ? N12 C11 C2 114.3(2) . . ? N12 C11 H11A 108.7 . . ? C2 C11 H11A 108.7 . . ? N12 C11 H11B 108.7 . . ? C2 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C11 N12 C22 108.3(2) . . ? C11 N12 C12 106.87(19) . . ? C22 N12 C12 107.31(19) . . ? C11 N12 Zn1 108.47(15) . . ? C22 N12 Zn1 114.25(16) . . ? C12 N12 Zn1 111.37(15) . . ? N12 C12 C13 115.1(2) . . ? N12 C12 H12A 108.5 . . ? C13 C12 H12A 108.5 . . ? N12 C12 H12B 108.5 . . ? C13 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? C14 C13 C12 112.1(2) . . ? C14 C13 H13A 109.2 . . ? C12 C13 H13A 109.2 . . ? C14 C13 H13B 109.2 . . ? C12 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? N13 C14 C15 121.0(3) . . ? N13 C14 C13 116.6(2) . . ? C15 C14 C13 122.3(2) . . ? C16 C15 C14 119.5(3) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C17 C16 C15 119.0(3) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C18 C17 C16 119.1(3) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? N13 C18 C17 122.3(3) . . ? N13 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? C14 N13 C18 118.9(2) . . ? C14 N13 Zn1 120.34(18) . . ? C18 N13 Zn1 120.68(19) . . ? N12 C22 C23 113.5(2) . . ? N12 C22 H22A 108.9 . . ? C23 C22 H22A 108.9 . . ? N12 C22 H22B 108.9 . . ? C23 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C24 C23 C22 116.3(2) . . ? C24 C23 H23A 108.2 . . ? C22 C23 H23A 108.2 . . ? C24 C23 H23B 108.2 . . ? C22 C23 H23B 108.2 . . ? H23A C23 H23B 107.4 . . ? N14 C24 C25 120.7(3) . . ? N14 C24 C23 118.7(2) . . ? C25 C24 C23 120.6(2) . . ? C26 C25 C24 120.0(3) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C27 C26 C25 119.0(3) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? C26 C27 C28 118.7(3) . . ? C26 C27 H27 120.7 . . ? C28 C27 H27 120.7 . . ? N14 C28 C27 123.0(3) . . ? N14 C28 H28 118.5 . . ? C27 C28 H28 118.5 . . ? C28 N14 C24 118.5(2) . . ? C28 N14 Zn1 117.80(17) . . ? C24 N14 Zn1 123.68(18) . . ? N16 C31 C3 115.1(2) . . ? N16 C31 H31A 108.5 . . ? C3 C31 H31A 108.5 . . ? N16 C31 H31B 108.5 . . ? C3 C31 H31B 108.5 . . ? H31A C31 H31B 107.5 . . ? C31 N16 C42 108.7(2) . . ? C31 N16 C32 107.19(19) . . ? C42 N16 C32 107.39(19) . . ? C31 N16 Zn2 110.15(16) . . ? C42 N16 Zn2 113.86(16) . . ? C32 N16 Zn2 109.34(15) . . ? N16 C32 C33 115.4(2) . . ? N16 C32 H32A 108.4 . . ? C33 C32 H32A 108.4 . . ? N16 C32 H32B 108.4 . . ? C33 C32 H32B 108.4 . . ? H32A C32 H32B 107.5 . . ? C34 C33 C32 112.7(2) . . ? C34 C33 H33A 109.0 . . ? C32 C33 H33A 109.0 . . ? C34 C33 H33B 109.0 . . ? C32 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? N17 C34 C35 120.8(3) . . ? N17 C34 C33 117.6(2) . . ? C35 C34 C33 121.6(2) . . ? C36 C35 C34 119.4(3) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C37 C36 C35 119.5(3) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C38 C37 C36 118.4(3) . . ? C38 C37 H37 120.8 . . ? C36 C37 H37 120.8 . . ? N17 C38 C37 122.5(3) . . ? N17 C38 H38 118.7 . . ? C37 C38 H38 118.7 . . ? C34 N17 C38 119.3(2) . . ? C34 N17 Zn2 120.01(18) . . ? C38 N17 Zn2 120.47(18) . . ? N16 C42 C43 114.6(2) . . ? N16 C42 H42A 108.6 . . ? C43 C42 H42A 108.6 . . ? N16 C42 H42B 108.6 . . ? C43 C42 H42B 108.6 . . ? H42A C42 H42B 107.6 . . ? C44 C43 C42 116.4(2) . . ? C44 C43 H43A 108.2 . . ? C42 C43 H43A 108.2 . . ? C44 C43 H43B 108.2 . . ? C42 C43 H43B 108.2 . . ? H43A C43 H43B 107.3 . . ? N18 C44 C45 120.4(3) . . ? N18 C44 C43 118.8(2) . . ? C45 C44 C43 120.7(2) . . ? C46 C45 C44 120.5(3) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C45 C46 C47 118.9(3) . . ? C45 C46 H46 120.6 . . ? C47 C46 H46 120.6 . . ? C46 C47 C48 118.3(3) . . ? C46 C47 H47 120.8 . . ? C48 C47 H47 120.8 . . ? N18 C48 C47 123.3(3) . . ? N18 C48 H48 118.4 . . ? C47 C48 H48 118.4 . . ? C48 N18 C44 118.5(2) . . ? C48 N18 Zn2 117.87(17) . . ? C44 N18 Zn2 123.40(18) . . ? Zn1 F1 Zn2 101.26(6) . 2_656 ? Zn2 F2 Zn1 104.17(6) 2_656 . ? C50 O50 H50X 109.5 . . ? O50 C50 H50A 109.5 . . ? O50 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? O50 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? H60X O60 H60Y 108.3 . . ? H60X O60 H61Y 118.7 . . ? H60Y O60 H61Y 116.6 . . ? O61 O61 H60X 85.4 2_766 . ? O61 O61 H60Y 110.7 2_766 . ? H60X O61 H60Y 56.7 . . ? O61 O61 H61X 47.9 2_766 . ? H60X O61 H61X 132.7 . . ? H60Y O61 H61X 137.5 . . ? O61 O61 H61Y 139.5 2_766 . ? H60X O61 H61Y 108.3 . . ? H60Y O61 H61Y 108.5 . . ? H61X O61 H61Y 105.2 . . ? F11 B1 F12 109.9(3) . . ? F11 B1 F13 110.0(3) . . ? F12 B1 F13 109.9(3) . . ? F11 B1 F14 109.5(2) . . ? F12 B1 F14 108.6(3) . . ? F13 B1 F14 109.0(2) . . ? F21 B2 F24 111.0(3) . . ? F21 B2 F22 108.8(4) . . ? F24 B2 F22 109.6(3) . . ? F21 B2 F23 110.7(3) . . ? F24 B2 F23 109.3(3) . . ? F22 B2 F23 107.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N11 C2 C1 -1.0(3) . . . . ? C4 N11 C2 C11 179.9(2) . . . . ? C3 C1 C2 N11 0.1(4) . . . . ? C3 C1 C2 C11 179.3(2) . . . . ? C2 C1 C3 N15 0.8(4) . . . . ? C2 C1 C3 C31 -178.8(2) . . . . ? C1 C3 N15 C4 -0.8(3) . . . . ? C31 C3 N15 C4 178.8(2) . . . . ? C2 N11 C4 N15 1.0(3) . . . . ? C2 N11 C4 C5 178.7(2) . . . . ? C3 N15 C4 N11 -0.2(3) . . . . ? C3 N15 C4 C5 -177.8(2) . . . . ? N11 C4 C5 C10 -176.5(2) . . . . ? N15 C4 C5 C10 1.4(3) . . . . ? N11 C4 C5 C6 2.5(3) . . . . ? N15 C4 C5 C6 -179.7(2) . . . . ? C10 C5 C6 C7 1.5(4) . . . . ? C4 C5 C6 C7 -177.5(2) . . . . ? C5 C6 C7 C8 -0.7(4) . . . . ? C6 C7 C8 C9 -0.4(4) . . . . ? C7 C8 C9 C10 0.7(4) . . . . ? C8 C9 C10 C5 0.1(4) . . . . ? C6 C5 C10 C9 -1.2(4) . . . . ? C4 C5 C10 C9 177.8(2) . . . . ? N11 C2 C11 N12 38.6(3) . . . . ? C1 C2 C11 N12 -140.6(2) . . . . ? C2 C11 N12 C22 59.8(3) . . . . ? C2 C11 N12 C12 175.1(2) . . . . ? C2 C11 N12 Zn1 -64.7(2) . . . . ? F1 Zn1 N12 C11 12.0(3) . . . . ? F2 Zn1 N12 C11 -38.48(15) . . . . ? N13 Zn1 N12 C11 -133.46(15) . . . . ? N14 Zn1 N12 C11 129.66(15) . . . . ? F1 Zn1 N12 C22 -108.9(2) . . . . ? F2 Zn1 N12 C22 -159.38(17) . . . . ? N13 Zn1 N12 C22 105.64(17) . . . . ? N14 Zn1 N12 C22 8.77(18) . . . . ? F1 Zn1 N12 C12 129.37(19) . . . . ? F2 Zn1 N12 C12 78.85(16) . . . . ? N13 Zn1 N12 C12 -16.13(16) . . . . ? N14 Zn1 N12 C12 -113.01(16) . . . . ? C11 N12 C12 C13 88.4(3) . . . . ? C22 N12 C12 C13 -155.6(2) . . . . ? Zn1 N12 C12 C13 -29.9(3) . . . . ? N12 C12 C13 C14 80.3(3) . . . . ? C12 C13 C14 N13 -62.6(3) . . . . ? C12 C13 C14 C15 117.1(3) . . . . ? N13 C14 C15 C16 1.3(4) . . . . ? C13 C14 C15 C16 -178.4(3) . . . . ? C14 C15 C16 C17 -1.4(4) . . . . ? C15 C16 C17 C18 0.5(4) . . . . ? C16 C17 C18 N13 0.8(4) . . . . ? C15 C14 N13 C18 0.0(4) . . . . ? C13 C14 N13 C18 179.7(2) . . . . ? C15 C14 N13 Zn1 -177.40(19) . . . . ? C13 C14 N13 Zn1 2.3(3) . . . . ? C17 C18 N13 C14 -1.0(4) . . . . ? C17 C18 N13 Zn1 176.4(2) . . . . ? F1 Zn1 N13 C14 -135.33(18) . . . . ? F2 Zn1 N13 C14 -58.35(19) . . . . ? N12 Zn1 N13 C14 32.47(19) . . . . ? N14 Zn1 N13 C14 129.40(19) . . . . ? F1 Zn1 N13 C18 47.3(2) . . . . ? F2 Zn1 N13 C18 124.3(2) . . . . ? N12 Zn1 N13 C18 -144.8(2) . . . . ? N14 Zn1 N13 C18 -47.9(2) . . . . ? C11 N12 C22 C23 -168.4(2) . . . . ? C12 N12 C22 C23 76.6(3) . . . . ? Zn1 N12 C22 C23 -47.4(3) . . . . ? N12 C22 C23 C24 78.0(3) . . . . ? C22 C23 C24 N14 -54.3(3) . . . . ? C22 C23 C24 C25 128.5(3) . . . . ? N14 C24 C25 C26 -2.7(4) . . . . ? C23 C24 C25 C26 174.5(3) . . . . ? C24 C25 C26 C27 -0.3(4) . . . . ? C25 C26 C27 C28 2.0(4) . . . . ? C26 C27 C28 N14 -0.8(4) . . . . ? C27 C28 N14 C24 -2.1(4) . . . . ? C27 C28 N14 Zn1 176.0(2) . . . . ? C25 C24 N14 C28 3.8(4) . . . . ? C23 C24 N14 C28 -173.4(2) . . . . ? C25 C24 N14 Zn1 -174.16(19) . . . . ? C23 C24 N14 Zn1 8.6(3) . . . . ? F1 Zn1 N14 C28 -5.8(2) . . . . ? F2 Zn1 N14 C28 -48.8(4) . . . . ? N13 Zn1 N14 C28 95.9(2) . . . . ? N12 Zn1 N14 C28 -166.86(19) . . . . ? F1 Zn1 N14 C24 172.2(2) . . . . ? F2 Zn1 N14 C24 129.2(3) . . . . ? N13 Zn1 N14 C24 -86.1(2) . . . . ? N12 Zn1 N14 C24 11.1(2) . . . . ? N15 C3 C31 N16 -33.4(3) . . . . ? C1 C3 C31 N16 146.2(2) . . . . ? C3 C31 N16 C42 -57.9(3) . . . . ? C3 C31 N16 C32 -173.7(2) . . . . ? C3 C31 N16 Zn2 67.5(2) . . . . ? F2 Zn2 N16 C31 -28.1(3) 2_656 . . . ? N17 Zn2 N16 C31 127.90(16) . . . . ? F1 Zn2 N16 C31 37.60(16) 2_656 . . . ? N18 Zn2 N16 C31 -132.37(16) . . . . ? F2 Zn2 N16 C42 94.3(2) 2_656 . . . ? N17 Zn2 N16 C42 -109.74(17) . . . . ? F1 Zn2 N16 C42 159.96(16) 2_656 . . . ? N18 Zn2 N16 C42 -10.02(17) . . . . ? F2 Zn2 N16 C32 -145.60(16) 2_656 . . . ? N17 Zn2 N16 C32 10.36(16) . . . . ? F1 Zn2 N16 C32 -79.94(15) 2_656 . . . ? N18 Zn2 N16 C32 110.09(16) . . . . ? C31 N16 C32 C33 -81.2(3) . . . . ? C42 N16 C32 C33 162.2(2) . . . . ? Zn2 N16 C32 C33 38.2(2) . . . . ? N16 C32 C33 C34 -82.3(3) . . . . ? C32 C33 C34 N17 53.3(3) . . . . ? C32 C33 C34 C35 -125.3(3) . . . . ? N17 C34 C35 C36 1.2(4) . . . . ? C33 C34 C35 C36 179.6(3) . . . . ? C34 C35 C36 C37 -1.2(4) . . . . ? C35 C36 C37 C38 0.5(4) . . . . ? C36 C37 C38 N17 0.2(4) . . . . ? C35 C34 N17 C38 -0.4(4) . . . . ? C33 C34 N17 C38 -178.9(2) . . . . ? C35 C34 N17 Zn2 -175.0(2) . . . . ? C33 C34 N17 Zn2 6.5(3) . . . . ? C37 C38 N17 C34 -0.3(4) . . . . ? C37 C38 N17 Zn2 174.3(2) . . . . ? F2 Zn2 N17 C34 134.43(19) 2_656 . . . ? N16 Zn2 N17 C34 -35.0(2) . . . . ? F1 Zn2 N17 C34 58.99(19) 2_656 . . . ? N18 Zn2 N17 C34 -133.10(19) . . . . ? F2 Zn2 N17 C38 -40.11(19) 2_656 . . . ? N16 Zn2 N17 C38 150.48(18) . . . . ? F1 Zn2 N17 C38 -115.55(18) 2_656 . . . ? N18 Zn2 N17 C38 52.36(19) . . . . ? C31 N16 C42 C43 170.7(2) . . . . ? C32 N16 C42 C43 -73.6(3) . . . . ? Zn2 N16 C42 C43 47.6(3) . . . . ? N16 C42 C43 C44 -77.0(3) . . . . ? C42 C43 C44 N18 54.3(3) . . . . ? C42 C43 C44 C45 -129.2(3) . . . . ? N18 C44 C45 C46 1.5(4) . . . . ? C43 C44 C45 C46 -175.0(3) . . . . ? C44 C45 C46 C47 0.3(4) . . . . ? C45 C46 C47 C48 -1.4(4) . . . . ? C46 C47 C48 N18 0.6(4) . . . . ? C47 C48 N18 C44 1.2(4) . . . . ? C47 C48 N18 Zn2 -173.6(2) . . . . ? C45 C44 N18 C48 -2.3(4) . . . . ? C43 C44 N18 C48 174.3(2) . . . . ? C45 C44 N18 Zn2 172.26(19) . . . . ? C43 C44 N18 Zn2 -11.2(3) . . . . ? F2 Zn2 N18 C48 11.20(19) 2_656 . . . ? N17 Zn2 N18 C48 -94.6(2) . . . . ? N16 Zn2 N18 C48 166.30(19) . . . . ? F1 Zn2 N18 C48 29.6(4) 2_656 . . . ? F2 Zn2 N18 C44 -163.4(2) 2_656 . . . ? N17 Zn2 N18 C44 90.9(2) . . . . ? N16 Zn2 N18 C44 -8.3(2) . . . . ? F1 Zn2 N18 C44 -145.0(2) 2_656 . . . ? F2 Zn1 F1 Zn2 -10.88(6) . . . 2_656 ? N13 Zn1 F1 Zn2 81.50(8) . . . 2_656 ? N12 Zn1 F1 Zn2 -63.5(2) . . . 2_656 ? N14 Zn1 F1 Zn2 178.52(7) . . . 2_656 ? F1 Zn1 F2 Zn2 11.90(6) . . . 2_656 ? N13 Zn1 F2 Zn2 -88.45(8) . . . 2_656 ? N12 Zn1 F2 Zn2 175.00(8) . . . 2_656 ? N14 Zn1 F2 Zn2 56.4(3) . . . 2_656 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O50 H50X F21 0.84 1.95 2.778(3) 166.9 . O60 H60X F23 0.85 2.11 2.945(10) 169.2 . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.49 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.187 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.079 # Attachment 'wag284.cif' data_wag284 _database_code_depnum_ccdc_archive 'CCDC 842533' #TrackingRef 'wag284.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H100 B4 F20 N16 Ni4 O4' _chemical_formula_weight 2055.88 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7366(8) _cell_length_b 14.6440(8) _cell_length_c 15.0144(8) _cell_angle_alpha 68.536(2) _cell_angle_beta 71.171(2) _cell_angle_gamma 70.824(2) _cell_volume 2207.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 92(2) _cell_measurement_reflns_used 7600 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 26.47 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1060 _exptl_absorpt_coefficient_mu 0.943 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7524 _exptl_absorpt_correction_T_max 0.8953 _exptl_absorpt_process_details 'SCALE (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 92(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41031 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 26.51 _reflns_number_total 9099 _reflns_number_gt 8184 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. [Ni(II)4(LEt)2)(F)4](BF4)4.4MeOH Half of this in the asym unit and the other half generated by a center of inversion. All non-H anis. All H calc.and ride. Two disordered MeOH each split into two parts (o50,c50:051,c51) and (O60,C60:O61,C61) with 0.65:0.35 and 0.70:0.30 occup. respectively. Two disordered BF4. One is split into two parts sharing a common F = F11/F15 (EXYZ, EADP): B1,F11-F14 and B11,F15-F18 with 0.85:0.15 occup. respect.). B11,F15-F18 is SAME'd to the well behaved B1,F11-F14. The other BF4 is split into two overlapping parts B2,F21-F24 and B21,F25-F28 of 0.6:0.4 occup. respectively. Both parts also SAME'd to B1,F11-F14. H-bonds are present. i.e. MeOH(O51) with F18, MeOH(o60) with F22, and MeOH(o61) with F26, also between MeOH (O50) and MeOH (O60). ; _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^)+(0.0282P)^2^+1.3926P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9099 _refine_ls_number_parameters 722 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.461522(17) 0.141938(14) 0.245979(13) 0.01447(6) Uani 1 1 d . . . Ni2 Ni 0.755519(17) -0.219532(14) 0.587641(14) 0.01372(6) Uani 1 1 d . . . N11 N 0.71371(11) -0.08494(9) 0.45494(9) 0.0165(3) Uani 1 1 d . . . C1 C 0.79096(14) -0.02621(12) 0.43704(12) 0.0202(3) Uani 1 1 d . . . C2 C 0.78230(15) 0.06661(13) 0.36669(13) 0.0237(4) Uani 1 1 d . . . H2 H 0.8398 0.1060 0.3518 0.028 Uiso 1 1 calc R . . C3 C 0.68717(14) 0.10040(12) 0.31852(11) 0.0189(3) Uani 1 1 d . . . N15 N 0.60907(11) 0.04295(9) 0.33535(9) 0.0160(3) Uani 1 1 d . . . C4 C 0.63062(13) -0.05061(11) 0.39879(11) 0.0154(3) Uani 1 1 d . . . C5 C 0.57182(15) -0.12587(11) 0.39749(11) 0.0179(3) Uani 1 1 d . . . C6 C 0.63728(19) -0.18468(13) 0.33366(13) 0.0306(4) Uani 1 1 d . . . H6 H 0.7151 -0.1745 0.2916 0.037 Uiso 1 1 calc R . . C7 C 0.5887(3) -0.25761(14) 0.33178(16) 0.0451(6) Uani 1 1 d . . . H7 H 0.6324 -0.2970 0.2876 0.054 Uiso 1 1 calc R . . C8 C 0.4767(3) -0.27354(14) 0.39386(18) 0.0484(7) Uani 1 1 d . . . H8 H 0.4445 -0.3248 0.3930 0.058 Uiso 1 1 calc R . . C9 C 0.4115(2) -0.21591(15) 0.45690(16) 0.0397(5) Uani 1 1 d . . . H9 H 0.3343 -0.2270 0.4994 0.048 Uiso 1 1 calc R . . C10 C 0.45933(17) -0.14101(13) 0.45806(13) 0.0260(4) Uani 1 1 d . . . H10 H 0.4140 -0.1003 0.5009 0.031 Uiso 1 1 calc R . . C11 C 0.89383(15) -0.07008(13) 0.49034(13) 0.0262(4) Uani 1 1 d . . . H11B H 0.9667 -0.0426 0.4489 0.031 Uiso 1 1 calc R . . H11A H 0.8667 -0.0507 0.5519 0.031 Uiso 1 1 calc R . . N12 N 0.92903(12) -0.18191(11) 0.51379(10) 0.0249(3) Uani 1 1 d . . . C12 C 1.02641(16) -0.22107(15) 0.57177(14) 0.0344(5) Uani 1 1 d . . . H12B H 1.0791 -0.1723 0.5480 0.041 Uiso 1 1 calc R . . H12A H 1.0799 -0.2857 0.5601 0.041 Uiso 1 1 calc R . . C13 C 0.97252(16) -0.23806(13) 0.68184(14) 0.0277(4) Uani 1 1 d . . . H13B H 1.0366 -0.2416 0.7134 0.033 Uiso 1 1 calc R . . H13A H 0.9023 -0.1802 0.6929 0.033 Uiso 1 1 calc R . . C14 C 0.92838(14) -0.33384(12) 0.72805(12) 0.0189(3) Uani 1 1 d . . . C15 C 0.98331(15) -0.41459(13) 0.79754(12) 0.0236(3) Uani 1 1 d . . . H15 H 1.0493 -0.4096 0.8177 0.028 Uiso 1 1 calc R . . C16 C 0.94141(17) -0.50185(13) 0.83691(13) 0.0277(4) Uani 1 1 d . . . H16 H 0.9781 -0.5575 0.8845 0.033 Uiso 1 1 calc R . . C17 C 0.84514(17) -0.50746(13) 0.80628(13) 0.0258(4) Uani 1 1 d . . . H17 H 0.8142 -0.5666 0.8324 0.031 Uiso 1 1 calc R . . C18 C 0.79534(15) -0.42459(12) 0.73661(12) 0.0198(3) Uani 1 1 d . . . H18 H 0.7296 -0.4284 0.7153 0.024 Uiso 1 1 calc R . . N13 N 0.83489(12) -0.33893(9) 0.69744(9) 0.0165(3) Uani 1 1 d . . . C22 C 0.98288(17) -0.20965(14) 0.41968(14) 0.0360(5) Uani 1 1 d . . . H22B H 1.0649 -0.1933 0.3899 0.043 Uiso 1 1 calc R . . H22A H 0.9286 -0.1678 0.3735 0.043 Uiso 1 1 calc R . . C23 C 0.99822(18) -0.32030(15) 0.43179(15) 0.0423(5) Uani 1 1 d . . . H23B H 1.0546 -0.3354 0.3711 0.051 Uiso 1 1 calc R . . H23A H 1.0406 -0.3610 0.4862 0.051 Uiso 1 1 calc R . . C24 C 0.88451(19) -0.35668(14) 0.45203(13) 0.0341(5) Uani 1 1 d . . . C25 C 0.8891(3) -0.42787(17) 0.40936(16) 0.0531(7) Uani 1 1 d . . . H25 H 0.9612 -0.4472 0.3621 0.064 Uiso 1 1 calc R . . C26 C 0.7905(3) -0.47078(16) 0.43466(18) 0.0570(8) Uani 1 1 d . . . H26 H 0.7939 -0.5196 0.4056 0.068 Uiso 1 1 calc R . . C27 C 0.6867(2) -0.44115(13) 0.50322(16) 0.0416(6) Uani 1 1 d . . . H27 H 0.6185 -0.4714 0.5247 0.050 Uiso 1 1 calc R . . C28 C 0.68381(18) -0.36635(12) 0.54014(13) 0.0268(4) Uani 1 1 d . . . H28 H 0.6104 -0.3434 0.5845 0.032 Uiso 1 1 calc R . . N14 N 0.78020(13) -0.32452(10) 0.51607(10) 0.0218(3) Uani 1 1 d . . . C31 C 0.67407(15) 0.19943(12) 0.23932(12) 0.0228(4) Uani 1 1 d . . . H31A H 0.6164 0.2535 0.2681 0.027 Uiso 1 1 calc R . . H31B H 0.7557 0.2167 0.2097 0.027 Uiso 1 1 calc R . . N16 N 0.62603(12) 0.19296(10) 0.16232(10) 0.0225(3) Uani 1 1 d . . . C32 C 0.61142(16) 0.29468(13) 0.08747(13) 0.0289(4) Uani 1 1 d . . . H32A H 0.6283 0.2859 0.0217 0.035 Uiso 1 1 calc R . . H32B H 0.6732 0.3282 0.0857 0.035 Uiso 1 1 calc R . . C33 C 0.48184(15) 0.36210(13) 0.10974(13) 0.0263(4) Uani 1 1 d . . . H33A H 0.4564 0.3575 0.1806 0.032 Uiso 1 1 calc R . . H33B H 0.4832 0.4332 0.0718 0.032 Uiso 1 1 calc R . . C34 C 0.38936(15) 0.33147(12) 0.08372(12) 0.0229(4) Uani 1 1 d . . . C35 C 0.33711(17) 0.38970(14) 0.00332(13) 0.0311(4) Uani 1 1 d . . . H35 H 0.3591 0.4515 -0.0369 0.037 Uiso 1 1 calc R . . C36 C 0.25340(18) 0.35755(14) -0.01787(13) 0.0329(4) Uani 1 1 d . . . H36 H 0.2180 0.3964 -0.0730 0.039 Uiso 1 1 calc R . . C37 C 0.22173(18) 0.26793(13) 0.04223(13) 0.0286(4) Uani 1 1 d . . . H37 H 0.1624 0.2450 0.0306 0.034 Uiso 1 1 calc R . . C38 C 0.27863(16) 0.21242(12) 0.11986(12) 0.0230(3) Uani 1 1 d . . . H38 H 0.2581 0.1502 0.1605 0.028 Uiso 1 1 calc R . . N17 N 0.36158(12) 0.24247(10) 0.14040(9) 0.0190(3) Uani 1 1 d . . . C42 C 0.72038(16) 0.11779(14) 0.11293(13) 0.0319(4) Uani 1 1 d . . . H42A H 0.7515 0.0569 0.1638 0.038 Uiso 1 1 calc R . . H42B H 0.7915 0.1474 0.0708 0.038 Uiso 1 1 calc R . . C43 C 0.66930(18) 0.08696(15) 0.05074(13) 0.0357(5) Uani 1 1 d . . . H43A H 0.6211 0.1489 0.0113 0.043 Uiso 1 1 calc R . . H43B H 0.7402 0.0573 0.0041 0.043 Uiso 1 1 calc R . . C44 C 0.58844(18) 0.01340(13) 0.10372(12) 0.0303(4) Uani 1 1 d . . . C45 C 0.6062(2) -0.06716(15) 0.06911(14) 0.0407(5) Uani 1 1 d . . . H45 H 0.6759 -0.0807 0.0177 0.049 Uiso 1 1 calc R . . C46 C 0.5232(2) -0.12736(14) 0.10894(14) 0.0423(6) Uani 1 1 d . . . H46 H 0.5352 -0.1827 0.0854 0.051 Uiso 1 1 calc R . . C47 C 0.4216(2) -0.10654(13) 0.18396(14) 0.0333(4) Uani 1 1 d . . . H47 H 0.3601 -0.1444 0.2102 0.040 Uiso 1 1 calc R . . C48 C 0.41283(17) -0.02885(12) 0.21931(12) 0.0241(4) Uani 1 1 d . . . H48 H 0.3463 -0.0167 0.2732 0.029 Uiso 1 1 calc R . . N18 N 0.49389(13) 0.03039(10) 0.18107(10) 0.0216(3) Uani 1 1 d . . . F1 F 0.30167(8) 0.11176(6) 0.34096(6) 0.01624(18) Uani 1 1 d . . . F2 F 0.41547(8) 0.23281(6) 0.33362(6) 0.01586(18) Uani 1 1 d . . . B1 B 0.6771(3) 0.4344(3) 0.2681(3) 0.0344(9) Uani 0.85 1 d PD A 1 F11 F 0.73779(11) 0.36291(10) 0.33890(9) 0.0478(3) Uani 0.85 1 d PD A 1 F12 F 0.55746(17) 0.42349(17) 0.28943(16) 0.0513(6) Uani 0.85 1 d PD A 1 F13 F 0.74138(14) 0.41598(10) 0.17732(10) 0.0404(3) Uani 0.85 1 d PD A 1 F14 F 0.6765(3) 0.5309(2) 0.2616(3) 0.0514(9) Uani 0.85 1 d PD A 1 B11 B 0.6563(15) 0.4496(12) 0.2965(11) 0.049(10) Uani 0.15 1 d PD B 2 F15 F 0.73779(11) 0.36291(10) 0.33890(9) 0.0478(3) Uani 0.15 1 d PD B 2 F16 F 0.5659(8) 0.4786(7) 0.3731(7) 0.061(3) Uani 0.15 1 d PD B 2 F17 F 0.7192(14) 0.5251(14) 0.2478(12) 0.037(4) Uani 0.15 1 d PD B 2 F18 F 0.5978(16) 0.4397(8) 0.2342(11) 0.082(6) Uani 0.15 1 d PD B 2 B2 B 0.0463(4) 1.0390(3) 0.1933(3) 0.0259(8) Uani 0.60 1 d PD C 1 F21 F 0.0861(15) 1.0165(14) 0.2780(8) 0.0323(15) Uani 0.60 1 d PD C 1 F22 F -0.0329(3) 0.97749(19) 0.2107(2) 0.0324(6) Uani 0.60 1 d PD C 1 F23 F 0.1448(4) 1.0265(3) 0.1164(3) 0.0457(9) Uani 0.60 1 d PD C 1 F24 F -0.02123(17) 1.14004(13) 0.17005(14) 0.0351(4) Uani 0.60 1 d PD C 1 B21 B 0.0958(6) 0.9967(5) 0.1898(4) 0.0246(12) Uani 0.40 1 d PD D 2 F25 F 0.099(2) 1.004(2) 0.2788(11) 0.041(4) Uani 0.40 1 d PD D 2 F26 F -0.0266(5) 1.0231(5) 0.1827(4) 0.0593(15) Uani 0.40 1 d PD D 2 F27 F 0.1628(6) 1.0597(4) 0.1128(4) 0.0382(12) Uani 0.40 1 d PD D 2 F28 F 0.1468(3) 0.8981(2) 0.1859(2) 0.0371(7) Uani 0.40 1 d PD D 2 O50 O 0.3055(3) 0.70080(19) 0.14798(17) 0.0512(6) Uani 0.65 1 d P E 1 H50 H 0.2297 0.7268 0.1657 0.061 Uiso 0.65 1 calc PR E 1 C50 C 0.3514(7) 0.6440(5) 0.2281(5) 0.045(2) Uani 0.65 1 d P E 1 H50A H 0.4372 0.6479 0.2153 0.054 Uiso 0.65 1 calc PR E 1 H50B H 0.3491 0.5736 0.2428 0.054 Uiso 0.65 1 calc PR E 1 H50C H 0.3011 0.6692 0.2843 0.054 Uiso 0.65 1 calc PR E 1 O51 O 0.3947(4) 0.5793(3) 0.1761(4) 0.0434(10) Uani 0.35 1 d P F 2 H51 H 0.4580 0.5387 0.1947 0.052 Uiso 0.35 1 calc PR F 2 C51 C 0.3456(17) 0.6487(12) 0.2282(15) 0.095(9) Uani 0.35 1 d P F 2 H51A H 0.2826 0.7037 0.1979 0.114 Uiso 0.35 1 calc PR F 2 H51B H 0.4116 0.6762 0.2278 0.114 Uiso 0.35 1 calc PR F 2 H51C H 0.3075 0.6159 0.2962 0.114 Uiso 0.35 1 calc PR F 2 O60 O 0.0531(3) 0.7906(2) 0.1722(2) 0.0799(9) Uani 0.70 1 d P G 1 H60 H 0.0417 0.8472 0.1799 0.096 Uiso 0.70 1 calc PR G 1 C60 C -0.0193(5) 0.7991(6) 0.1121(6) 0.0613(16) Uani 0.70 1 d P G 1 H60A H -0.0922 0.7726 0.1522 0.074 Uiso 0.70 1 calc PR G 1 H60B H 0.0288 0.7604 0.0653 0.074 Uiso 0.70 1 calc PR G 1 H60C H -0.0460 0.8703 0.0762 0.074 Uiso 0.70 1 calc PR G 1 O61 O -0.1066(6) 0.8570(6) 0.1959(4) 0.0663(19) Uani 0.30 1 d P H 2 H61 H -0.0670 0.9014 0.1796 0.080 Uiso 0.30 1 calc PR H 2 C61 C -0.0724(10) 0.8119(15) 0.1214(13) 0.055(3) Uani 0.30 1 d P H 2 H61A H -0.0090 0.8416 0.0678 0.066 Uiso 0.30 1 calc PR H 2 H61B H -0.1451 0.8231 0.0967 0.066 Uiso 0.30 1 calc PR H 2 H61C H -0.0389 0.7392 0.1472 0.066 Uiso 0.30 1 calc PR H 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01594(10) 0.01365(10) 0.01164(10) -0.00331(7) -0.00278(7) -0.00155(7) Ni2 0.01278(10) 0.01249(10) 0.01468(10) -0.00372(7) -0.00280(7) -0.00213(7) N11 0.0134(6) 0.0159(6) 0.0157(6) -0.0030(5) -0.0007(5) -0.0022(5) C1 0.0126(7) 0.0213(8) 0.0201(8) -0.0010(6) -0.0017(6) -0.0035(6) C2 0.0142(7) 0.0223(8) 0.0276(9) 0.0023(7) -0.0037(6) -0.0072(6) C3 0.0136(7) 0.0175(8) 0.0185(8) -0.0014(6) 0.0005(6) -0.0031(6) N15 0.0143(6) 0.0155(6) 0.0138(6) -0.0039(5) -0.0001(5) -0.0015(5) C4 0.0134(7) 0.0158(7) 0.0127(7) -0.0060(6) 0.0016(5) -0.0003(6) C5 0.0270(8) 0.0114(7) 0.0159(7) -0.0028(6) -0.0111(6) -0.0005(6) C6 0.0446(11) 0.0213(9) 0.0242(9) -0.0115(7) -0.0181(8) 0.0098(8) C7 0.0873(18) 0.0176(9) 0.0416(12) -0.0149(8) -0.0465(13) 0.0114(10) C8 0.098(2) 0.0147(9) 0.0559(14) 0.0023(9) -0.0615(15) -0.0143(10) C9 0.0561(13) 0.0335(11) 0.0410(11) 0.0037(9) -0.0266(10) -0.0266(10) C10 0.0333(10) 0.0251(9) 0.0252(9) -0.0073(7) -0.0082(7) -0.0127(7) C11 0.0160(8) 0.0239(8) 0.0304(9) 0.0069(7) -0.0076(7) -0.0088(6) N12 0.0138(6) 0.0239(7) 0.0242(7) 0.0043(6) -0.0038(5) -0.0016(5) C12 0.0148(8) 0.0336(10) 0.0402(11) 0.0117(8) -0.0115(8) -0.0077(7) C13 0.0236(9) 0.0226(9) 0.0376(10) 0.0020(7) -0.0174(8) -0.0085(7) C14 0.0157(7) 0.0188(8) 0.0201(8) -0.0057(6) -0.0042(6) -0.0016(6) C15 0.0204(8) 0.0248(8) 0.0250(8) -0.0048(7) -0.0095(7) -0.0031(7) C16 0.0306(9) 0.0222(8) 0.0253(9) 0.0008(7) -0.0126(7) -0.0024(7) C17 0.0329(9) 0.0177(8) 0.0263(9) -0.0012(7) -0.0101(7) -0.0081(7) C18 0.0226(8) 0.0175(7) 0.0208(8) -0.0068(6) -0.0057(6) -0.0045(6) N13 0.0162(6) 0.0157(6) 0.0167(6) -0.0054(5) -0.0030(5) -0.0028(5) C22 0.0189(9) 0.0348(10) 0.0254(9) 0.0040(8) 0.0043(7) 0.0063(7) C23 0.0312(10) 0.0362(11) 0.0275(10) -0.0037(8) 0.0058(8) 0.0138(8) C24 0.0455(11) 0.0229(9) 0.0185(8) -0.0065(7) -0.0111(8) 0.0156(8) C25 0.0805(18) 0.0343(12) 0.0309(11) -0.0217(9) -0.0265(12) 0.0306(12) C26 0.105(2) 0.0240(10) 0.0542(14) -0.0248(10) -0.0599(15) 0.0253(12) C27 0.0735(15) 0.0148(8) 0.0506(13) -0.0091(8) -0.0483(12) 0.0048(9) C28 0.0423(10) 0.0150(8) 0.0274(9) -0.0050(7) -0.0229(8) 0.0011(7) N14 0.0300(8) 0.0154(6) 0.0170(7) -0.0053(5) -0.0096(6) 0.0031(6) C31 0.0156(8) 0.0204(8) 0.0249(8) 0.0045(7) -0.0052(6) -0.0068(6) N16 0.0190(7) 0.0215(7) 0.0160(6) 0.0025(5) -0.0018(5) -0.0022(5) C32 0.0218(8) 0.0275(9) 0.0224(9) 0.0087(7) -0.0030(7) -0.0070(7) C33 0.0235(8) 0.0189(8) 0.0263(9) 0.0049(7) -0.0055(7) -0.0053(7) C34 0.0206(8) 0.0204(8) 0.0177(8) -0.0017(6) -0.0019(6) 0.0009(6) C35 0.0281(9) 0.0282(9) 0.0222(9) 0.0048(7) -0.0060(7) -0.0014(7) C36 0.0350(10) 0.0338(10) 0.0195(8) -0.0025(7) -0.0133(7) 0.0058(8) C37 0.0355(10) 0.0259(9) 0.0253(9) -0.0129(7) -0.0156(8) 0.0062(7) C38 0.0323(9) 0.0176(8) 0.0200(8) -0.0091(6) -0.0104(7) 0.0014(7) N17 0.0224(7) 0.0170(6) 0.0138(6) -0.0054(5) -0.0038(5) 0.0011(5) C42 0.0204(8) 0.0338(10) 0.0194(8) 0.0003(7) 0.0047(7) 0.0034(7) C43 0.0370(11) 0.0359(10) 0.0147(8) -0.0065(7) 0.0019(7) 0.0072(8) C44 0.0390(10) 0.0256(9) 0.0149(8) -0.0068(7) -0.0093(7) 0.0107(8) C45 0.0612(14) 0.0285(10) 0.0195(9) -0.0130(8) -0.0139(9) 0.0167(10) C46 0.0782(16) 0.0205(9) 0.0281(10) -0.0145(8) -0.0309(11) 0.0152(10) C47 0.0582(13) 0.0165(8) 0.0301(10) -0.0067(7) -0.0284(9) 0.0029(8) C48 0.0351(9) 0.0162(8) 0.0204(8) -0.0058(6) -0.0145(7) 0.0030(7) N18 0.0292(7) 0.0174(7) 0.0148(6) -0.0054(5) -0.0090(6) 0.0033(6) F1 0.0180(4) 0.0153(4) 0.0178(4) -0.0067(3) -0.0049(3) -0.0040(3) F2 0.0153(4) 0.0150(4) 0.0177(4) -0.0051(3) -0.0030(3) -0.0046(3) B1 0.0328(16) 0.0296(17) 0.0393(19) 0.0104(17) -0.0210(16) -0.0161(13) F11 0.0398(7) 0.0483(7) 0.0398(7) 0.0141(6) -0.0184(5) -0.0123(6) F12 0.0280(8) 0.0462(11) 0.0736(14) -0.0038(11) -0.0165(9) -0.0119(7) F13 0.0460(8) 0.0380(8) 0.0377(8) 0.0030(6) -0.0174(6) -0.0189(6) F14 0.072(2) 0.0348(12) 0.0563(18) -0.0042(10) -0.0270(16) -0.0220(14) B11 0.062(17) 0.035(12) 0.064(19) -0.029(12) -0.026(13) 0.000(9) F15 0.0398(7) 0.0483(7) 0.0398(7) 0.0141(6) -0.0184(5) -0.0123(6) F16 0.039(5) 0.043(5) 0.076(7) -0.021(5) 0.025(5) -0.012(4) F17 0.042(9) 0.051(7) 0.012(4) -0.001(4) -0.007(5) -0.013(6) F18 0.151(16) 0.020(5) 0.118(12) -0.012(7) -0.111(12) -0.008(7) B2 0.021(2) 0.031(2) 0.0256(19) -0.0098(17) -0.0016(17) -0.0084(18) F21 0.033(2) 0.036(2) 0.032(3) -0.0094(17) -0.0092(17) -0.0121(17) F22 0.0293(12) 0.0330(13) 0.0387(16) -0.0123(11) -0.0083(11) -0.0097(11) F23 0.0333(15) 0.066(3) 0.0387(17) -0.0288(19) 0.0096(12) -0.0151(16) F24 0.0310(10) 0.0295(9) 0.0410(11) -0.0078(8) -0.0073(8) -0.0060(8) B21 0.018(3) 0.030(3) 0.023(3) -0.012(3) 0.003(2) -0.004(3) F25 0.053(9) 0.053(9) 0.023(4) -0.008(3) -0.006(4) -0.028(7) F26 0.021(2) 0.105(5) 0.050(3) -0.033(3) -0.006(2) -0.003(3) F27 0.050(3) 0.039(3) 0.0257(18) -0.0085(18) 0.0020(16) -0.0222(18) F28 0.0388(16) 0.0273(14) 0.0440(16) -0.0166(12) 0.0046(13) -0.0134(12) O50 0.0722(18) 0.0432(14) 0.0344(13) -0.0007(11) -0.0217(12) -0.0115(13) C50 0.060(4) 0.038(4) 0.045(3) 0.002(3) -0.025(3) -0.026(4) O51 0.034(2) 0.049(3) 0.056(3) -0.026(2) -0.016(2) -0.0029(19) C51 0.113(13) 0.065(10) 0.148(16) -0.075(9) -0.109(11) 0.054(7) O60 0.098(2) 0.0499(16) 0.088(2) -0.0240(16) -0.0475(19) 0.0165(16) C60 0.067(4) 0.059(3) 0.072(3) -0.033(2) -0.012(4) -0.020(4) O61 0.071(4) 0.107(5) 0.047(3) -0.021(3) 0.003(3) -0.072(4) C61 0.046(7) 0.081(10) 0.052(6) -0.027(5) -0.011(7) -0.024(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 F1 2.0262(9) . y Ni1 F2 2.0358(9) . y Ni1 N18 2.0691(14) . y Ni1 N17 2.1010(13) . y Ni1 N16 2.1353(14) . y Ni1 N15 2.3083(13) . y Ni2 F2 2.0049(9) 2_656 y Ni2 F1 2.0416(9) 2_656 y Ni2 N14 2.0780(14) . y Ni2 N13 2.1106(13) . y Ni2 N12 2.1242(14) . y Ni2 N11 2.2841(12) . y N11 C4 1.3464(19) . ? N11 C1 1.349(2) . ? C1 C2 1.379(2) . ? C1 C11 1.500(2) . ? C2 C3 1.382(2) . ? C2 H2 0.9500 . ? C3 N15 1.347(2) . ? C3 C31 1.500(2) . ? N15 C4 1.3495(19) . ? C4 C5 1.488(2) . ? C5 C10 1.374(2) . ? C5 C6 1.394(2) . ? C6 C7 1.378(3) . ? C6 H6 0.9500 . ? C7 C8 1.379(4) . ? C7 H7 0.9500 . ? C8 C9 1.374(3) . ? C8 H8 0.9500 . ? C9 C10 1.394(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 N12 1.485(2) . ? C11 H11B 0.9900 . ? C11 H11A 0.9900 . ? N12 C22 1.495(2) . ? N12 C12 1.496(2) . ? C12 C13 1.523(3) . ? C12 H12B 0.9900 . ? C12 H12A 0.9900 . ? C13 C14 1.500(2) . ? C13 H13B 0.9900 . ? C13 H13A 0.9900 . ? C14 N13 1.351(2) . ? C14 C15 1.390(2) . ? C15 C16 1.377(2) . ? C15 H15 0.9500 . ? C16 C17 1.385(3) . ? C16 H16 0.9500 . ? C17 C18 1.381(2) . ? C17 H17 0.9500 . ? C18 N13 1.342(2) . ? C18 H18 0.9500 . ? C22 C23 1.518(3) . ? C22 H22B 0.9900 . ? C22 H22A 0.9900 . ? C23 C24 1.498(3) . ? C23 H23B 0.9900 . ? C23 H23A 0.9900 . ? C24 N14 1.356(2) . ? C24 C25 1.389(3) . ? C25 C26 1.377(4) . ? C25 H25 0.9500 . ? C26 C27 1.379(4) . ? C26 H26 0.9500 . ? C27 C28 1.384(2) . ? C27 H27 0.9500 . ? C28 N14 1.347(2) . ? C28 H28 0.9500 . ? C31 N16 1.483(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? N16 C32 1.498(2) . ? N16 C42 1.502(2) . ? C32 C33 1.525(2) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.501(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 N17 1.348(2) . ? C34 C35 1.393(2) . ? C35 C36 1.380(3) . ? C35 H35 0.9500 . ? C36 C37 1.383(3) . ? C36 H36 0.9500 . ? C37 C38 1.385(2) . ? C37 H37 0.9500 . ? C38 N17 1.346(2) . ? C38 H38 0.9500 . ? C42 C43 1.511(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.500(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 N18 1.357(2) . ? C44 C45 1.387(3) . ? C45 C46 1.373(3) . ? C45 H45 0.9500 . ? C46 C47 1.389(3) . ? C46 H46 0.9500 . ? C47 C48 1.384(2) . ? C47 H47 0.9500 . ? C48 N18 1.346(2) . ? C48 H48 0.9500 . ? F1 Ni2 2.0416(9) 2_656 ? F2 Ni2 2.0049(9) 2_656 ? B1 F12 1.386(4) . ? B1 F11 1.385(3) . ? B1 F14 1.379(5) . ? B1 F13 1.403(5) . ? B11 F17 1.378(15) . ? B11 F16 1.380(14) . ? B11 F18 1.395(14) . ? B2 F23 1.364(6) . ? B2 F21 1.384(8) . ? B2 F22 1.402(5) . ? B2 F24 1.403(5) . ? B21 F27 1.384(7) . ? B21 F28 1.385(7) . ? B21 F25 1.392(11) . ? B21 F26 1.388(7) . ? O50 C50 1.349(7) . ? O50 H50 0.8400 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? O51 C51 1.373(17) . ? O51 H51 0.8400 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? O60 C60 1.376(7) . ? O60 H60 0.8400 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? O61 C61 1.388(18) . ? O61 H61 0.8400 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Ni1 F2 76.01(3) . . y F1 Ni1 N18 94.91(5) . . y F2 Ni1 N18 169.03(5) . . y F1 Ni1 N17 90.04(4) . . y F2 Ni1 N17 97.41(4) . . y N18 Ni1 N17 88.62(5) . . y F1 Ni1 N16 168.68(5) . . y F2 Ni1 N16 92.68(5) . . y N18 Ni1 N16 96.27(6) . . y N17 Ni1 N16 91.92(5) . . y F1 Ni1 N15 102.87(4) . . y F2 Ni1 N15 85.46(4) . . y N18 Ni1 N15 90.69(5) . . y N17 Ni1 N15 167.08(5) . . y N16 Ni1 N15 75.33(5) . . y F2 Ni2 F1 76.35(3) 2_656 2_656 y F2 Ni2 N14 94.68(5) 2_656 . y F1 Ni2 N14 169.72(5) 2_656 . y F2 Ni2 N13 90.99(4) 2_656 . y F1 Ni2 N13 96.90(4) 2_656 . y N14 Ni2 N13 88.16(5) . . y F2 Ni2 N12 169.36(5) 2_656 . y F1 Ni2 N12 93.06(5) 2_656 . y N14 Ni2 N12 95.78(6) . . y N13 Ni2 N12 91.32(5) . . y F2 Ni2 N11 101.64(4) 2_656 . y F1 Ni2 N11 83.85(4) 2_656 . y N14 Ni2 N11 93.22(5) . . y N13 Ni2 N11 167.12(5) . . y N12 Ni2 N11 75.80(5) . . y C4 N11 C1 117.11(13) . . ? C4 N11 Ni2 136.29(10) . . ? C1 N11 Ni2 106.45(10) . . ? N11 C1 C2 121.45(15) . . ? N11 C1 C11 117.09(14) . . ? C2 C1 C11 121.23(15) . . ? C1 C2 C3 117.78(15) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? N15 C3 C2 121.59(14) . . ? N15 C3 C31 117.55(14) . . ? C2 C3 C31 120.67(14) . . ? C3 N15 C4 116.93(13) . . ? C3 N15 Ni1 106.33(9) . . ? C4 N15 Ni1 136.68(11) . . ? N11 C4 N15 124.48(14) . . ? N11 C4 C5 116.84(13) . . ? N15 C4 C5 118.15(13) . . ? C10 C5 C6 119.80(16) . . ? C10 C5 C4 122.75(14) . . ? C6 C5 C4 117.42(16) . . ? C7 C6 C5 119.7(2) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C8 120.19(19) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 120.48(19) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 119.6(2) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C5 C10 C9 120.22(18) . . ? C5 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? N12 C11 C1 110.44(14) . . ? N12 C11 H11B 109.6 . . ? C1 C11 H11B 109.6 . . ? N12 C11 H11A 109.6 . . ? C1 C11 H11A 109.6 . . ? H11B C11 H11A 108.1 . . ? C11 N12 C22 108.69(13) . . ? C11 N12 C12 107.70(14) . . ? C22 N12 C12 108.84(14) . . ? C11 N12 Ni2 101.95(9) . . ? C22 N12 Ni2 112.16(12) . . ? C12 N12 Ni2 116.95(10) . . ? N12 C12 C13 112.97(14) . . ? N12 C12 H12B 109.0 . . ? C13 C12 H12B 109.0 . . ? N12 C12 H12A 109.0 . . ? C13 C12 H12A 109.0 . . ? H12B C12 H12A 107.8 . . ? C14 C13 C12 111.24(16) . . ? C14 C13 H13B 109.4 . . ? C12 C13 H13B 109.4 . . ? C14 C13 H13A 109.4 . . ? C12 C13 H13A 109.4 . . ? H13B C13 H13A 108.0 . . ? N13 C14 C15 121.56(15) . . ? N13 C14 C13 117.01(13) . . ? C15 C14 C13 121.41(15) . . ? C16 C15 C14 119.57(16) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 119.21(15) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 C16 118.15(16) . . ? C18 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? N13 C18 C17 123.50(15) . . ? N13 C18 H18 118.3 . . ? C17 C18 H18 118.3 . . ? C18 N13 C14 118.01(13) . . ? C18 N13 Ni2 119.85(10) . . ? C14 N13 Ni2 122.10(10) . . ? N12 C22 C23 113.92(15) . . ? N12 C22 H22B 108.8 . . ? C23 C22 H22B 108.8 . . ? N12 C22 H22A 108.8 . . ? C23 C22 H22A 108.8 . . ? H22B C22 H22A 107.7 . . ? C24 C23 C22 118.37(15) . . ? C24 C23 H23B 107.7 . . ? C22 C23 H23B 107.7 . . ? C24 C23 H23A 107.7 . . ? C22 C23 H23A 107.7 . . ? H23B C23 H23A 107.1 . . ? N14 C24 C25 120.4(2) . . ? N14 C24 C23 119.95(17) . . ? C25 C24 C23 119.6(2) . . ? C26 C25 C24 120.9(2) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C25 C26 C27 118.43(19) . . ? C25 C26 H26 120.8 . . ? C27 C26 H26 120.8 . . ? C26 C27 C28 118.6(2) . . ? C26 C27 H27 120.7 . . ? C28 C27 H27 120.7 . . ? N14 C28 C27 123.11(19) . . ? N14 C28 H28 118.4 . . ? C27 C28 H28 118.4 . . ? C28 N14 C24 118.38(16) . . ? C28 N14 Ni2 115.44(11) . . ? C24 N14 Ni2 126.11(14) . . ? N16 C31 C3 110.02(14) . . ? N16 C31 H31A 109.7 . . ? C3 C31 H31A 109.7 . . ? N16 C31 H31B 109.7 . . ? C3 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? C31 N16 C32 107.33(14) . . ? C31 N16 C42 108.86(13) . . ? C32 N16 C42 108.26(13) . . ? C31 N16 Ni1 102.22(9) . . ? C32 N16 Ni1 117.43(10) . . ? C42 N16 Ni1 112.23(11) . . ? N16 C32 C33 112.26(13) . . ? N16 C32 H32A 109.2 . . ? C33 C32 H32A 109.2 . . ? N16 C32 H32B 109.2 . . ? C33 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C34 C33 C32 111.20(15) . . ? C34 C33 H33A 109.4 . . ? C32 C33 H33A 109.4 . . ? C34 C33 H33B 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? N17 C34 C35 121.01(17) . . ? N17 C34 C33 116.67(14) . . ? C35 C34 C33 122.30(16) . . ? C36 C35 C34 119.93(17) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 119.05(16) . . ? C35 C36 H36 120.5 . . ? C37 C36 H36 120.5 . . ? C36 C37 C38 118.32(18) . . ? C36 C37 H37 120.8 . . ? C38 C37 H37 120.8 . . ? N17 C38 C37 123.08(16) . . ? N17 C38 H38 118.5 . . ? C37 C38 H38 118.5 . . ? C38 N17 C34 118.56(14) . . ? C38 N17 Ni1 119.35(11) . . ? C34 N17 Ni1 121.54(11) . . ? N16 C42 C43 113.01(15) . . ? N16 C42 H42A 109.0 . . ? C43 C42 H42A 109.0 . . ? N16 C42 H42B 109.0 . . ? C43 C42 H42B 109.0 . . ? H42A C42 H42B 107.8 . . ? C44 C43 C42 117.15(15) . . ? C44 C43 H43A 108.0 . . ? C42 C43 H43A 108.0 . . ? C44 C43 H43B 108.0 . . ? C42 C43 H43B 108.0 . . ? H43A C43 H43B 107.3 . . ? N18 C44 C45 120.88(19) . . ? N18 C44 C43 119.37(16) . . ? C45 C44 C43 119.62(17) . . ? C46 C45 C44 120.16(19) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C47 119.29(18) . . ? C45 C46 H46 120.4 . . ? C47 C46 H46 120.4 . . ? C48 C47 C46 117.8(2) . . ? C48 C47 H47 121.1 . . ? C46 C47 H47 121.1 . . ? N18 C48 C47 123.25(17) . . ? N18 C48 H48 118.4 . . ? C47 C48 H48 118.4 . . ? C48 N18 C44 118.33(15) . . ? C48 N18 Ni1 116.30(11) . . ? C44 N18 Ni1 125.37(13) . . ? Ni1 F1 Ni2 102.68(4) . 2_656 ? Ni2 F2 Ni1 103.64(4) 2_656 . ? F12 B1 F11 109.5(3) . . ? F12 B1 F14 110.9(3) . . ? F11 B1 F14 111.2(3) . . ? F12 B1 F13 108.7(3) . . ? F11 B1 F13 107.7(3) . . ? F14 B1 F13 108.7(3) . . ? F17 B11 F16 107.2(12) . . ? F17 B11 F18 110.4(14) . . ? F16 B11 F18 108.0(14) . . ? F23 B2 F21 110.7(8) . . ? F23 B2 F22 111.1(4) . . ? F21 B2 F22 109.1(8) . . ? F23 B2 F24 108.6(3) . . ? F21 B2 F24 109.1(8) . . ? F22 B2 F24 108.0(4) . . ? F27 B21 F28 109.2(5) . . ? F27 B21 F25 109.6(12) . . ? F28 B21 F25 110.0(12) . . ? F27 B21 F26 110.6(6) . . ? F28 B21 F26 108.1(5) . . ? F25 B21 F26 109.3(11) . . ? C51 O51 H51 109.5 . . ? O51 C51 H51A 109.5 . . ? O51 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O51 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C61 O61 H61 109.5 . . ? O61 C61 H61A 109.5 . . ? O61 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? O61 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F2 Ni2 N11 C4 -38.06(15) 2_656 . . . ? F1 Ni2 N11 C4 -112.72(14) 2_656 . . . ? N14 Ni2 N11 C4 57.39(15) . . . . ? N13 Ni2 N11 C4 153.22(19) . . . . ? N12 Ni2 N11 C4 152.54(15) . . . . ? F2 Ni2 N11 C1 137.19(10) 2_656 . . . ? F1 Ni2 N11 C1 62.53(10) 2_656 . . . ? N14 Ni2 N11 C1 -127.36(10) . . . . ? N13 Ni2 N11 C1 -31.5(3) . . . . ? N12 Ni2 N11 C1 -32.21(10) . . . . ? C4 N11 C1 C2 2.3(2) . . . . ? Ni2 N11 C1 C2 -174.04(13) . . . . ? C4 N11 C1 C11 -172.35(14) . . . . ? Ni2 N11 C1 C11 11.34(17) . . . . ? N11 C1 C2 C3 3.5(3) . . . . ? C11 C1 C2 C3 177.91(16) . . . . ? C1 C2 C3 N15 -3.5(2) . . . . ? C1 C2 C3 C31 -178.41(15) . . . . ? C2 C3 N15 C4 -2.3(2) . . . . ? C31 C3 N15 C4 172.76(14) . . . . ? C2 C3 N15 Ni1 175.27(13) . . . . ? C31 C3 N15 Ni1 -9.63(16) . . . . ? F1 Ni1 N15 C3 -137.36(9) . . . . ? F2 Ni1 N15 C3 -62.84(10) . . . . ? N18 Ni1 N15 C3 127.44(10) . . . . ? N17 Ni1 N15 C3 40.6(3) . . . . ? N16 Ni1 N15 C3 31.13(10) . . . . ? F1 Ni1 N15 C4 39.53(15) . . . . ? F2 Ni1 N15 C4 114.05(14) . . . . ? N18 Ni1 N15 C4 -55.67(15) . . . . ? N17 Ni1 N15 C4 -142.5(2) . . . . ? N16 Ni1 N15 C4 -151.97(15) . . . . ? C1 N11 C4 N15 -8.8(2) . . . . ? Ni2 N11 C4 N15 166.04(11) . . . . ? C1 N11 C4 C5 162.63(14) . . . . ? Ni2 N11 C4 C5 -22.5(2) . . . . ? C3 N15 C4 N11 8.9(2) . . . . ? Ni1 N15 C4 N11 -167.80(11) . . . . ? C3 N15 C4 C5 -162.50(14) . . . . ? Ni1 N15 C4 C5 20.8(2) . . . . ? N11 C4 C5 C10 94.91(18) . . . . ? N15 C4 C5 C10 -93.06(18) . . . . ? N11 C4 C5 C6 -83.05(18) . . . . ? N15 C4 C5 C6 88.97(17) . . . . ? C10 C5 C6 C7 0.0(2) . . . . ? C4 C5 C6 C7 178.02(15) . . . . ? C5 C6 C7 C8 -1.0(3) . . . . ? C6 C7 C8 C9 1.1(3) . . . . ? C7 C8 C9 C10 -0.2(3) . . . . ? C6 C5 C10 C9 1.0(2) . . . . ? C4 C5 C10 C9 -176.95(15) . . . . ? C8 C9 C10 C5 -0.9(3) . . . . ? N11 C1 C11 N12 27.7(2) . . . . ? C2 C1 C11 N12 -146.93(16) . . . . ? C1 C11 N12 C22 65.47(17) . . . . ? C1 C11 N12 C12 -176.76(14) . . . . ? C1 C11 N12 Ni2 -53.12(15) . . . . ? F2 Ni2 N12 C11 -33.0(3) 2_656 . . . ? F1 Ni2 N12 C11 -38.57(11) 2_656 . . . ? N14 Ni2 N12 C11 136.16(11) . . . . ? N13 Ni2 N12 C11 -135.55(11) . . . . ? N11 Ni2 N12 C11 44.30(10) . . . . ? F2 Ni2 N12 C22 -149.1(2) 2_656 . . . ? F1 Ni2 N12 C22 -154.67(10) 2_656 . . . ? N14 Ni2 N12 C22 20.06(11) . . . . ? N13 Ni2 N12 C22 108.35(11) . . . . ? N11 Ni2 N12 C22 -71.80(11) . . . . ? F2 Ni2 N12 C12 84.1(3) 2_656 . . . ? F1 Ni2 N12 C12 78.58(13) 2_656 . . . ? N14 Ni2 N12 C12 -106.69(14) . . . . ? N13 Ni2 N12 C12 -18.40(14) . . . . ? N11 Ni2 N12 C12 161.45(14) . . . . ? C11 N12 C12 C13 86.88(18) . . . . ? C22 N12 C12 C13 -155.45(16) . . . . ? Ni2 N12 C12 C13 -27.1(2) . . . . ? N12 C12 C13 C14 77.65(19) . . . . ? C12 C13 C14 N13 -63.04(19) . . . . ? C12 C13 C14 C15 115.47(17) . . . . ? N13 C14 C15 C16 -0.4(3) . . . . ? C13 C14 C15 C16 -178.86(16) . . . . ? C14 C15 C16 C17 0.1(3) . . . . ? C15 C16 C17 C18 0.3(3) . . . . ? C16 C17 C18 N13 -0.3(3) . . . . ? C17 C18 N13 C14 0.0(2) . . . . ? C17 C18 N13 Ni2 177.75(13) . . . . ? C15 C14 N13 C18 0.4(2) . . . . ? C13 C14 N13 C18 178.90(14) . . . . ? C15 C14 N13 Ni2 -177.33(12) . . . . ? C13 C14 N13 Ni2 1.18(19) . . . . ? F2 Ni2 N13 C18 46.44(12) 2_656 . . . ? F1 Ni2 N13 C18 122.81(11) 2_656 . . . ? N14 Ni2 N13 C18 -48.21(12) . . . . ? N12 Ni2 N13 C18 -143.95(12) . . . . ? N11 Ni2 N13 C18 -144.6(2) . . . . ? F2 Ni2 N13 C14 -135.88(12) 2_656 . . . ? F1 Ni2 N13 C14 -59.51(12) 2_656 . . . ? N14 Ni2 N13 C14 129.47(12) . . . . ? N12 Ni2 N13 C14 33.73(12) . . . . ? N11 Ni2 N13 C14 33.1(3) . . . . ? C11 N12 C22 C23 -168.05(15) . . . . ? C12 N12 C22 C23 74.9(2) . . . . ? Ni2 N12 C22 C23 -56.10(18) . . . . ? N12 C22 C23 C24 73.2(2) . . . . ? C22 C23 C24 N14 -41.7(2) . . . . ? C22 C23 C24 C25 142.12(19) . . . . ? N14 C24 C25 C26 -3.2(3) . . . . ? C23 C24 C25 C26 173.00(18) . . . . ? C24 C25 C26 C27 0.2(3) . . . . ? C25 C26 C27 C28 3.0(3) . . . . ? C26 C27 C28 N14 -3.5(3) . . . . ? C27 C28 N14 C24 0.6(2) . . . . ? C27 C28 N14 Ni2 -176.73(13) . . . . ? C25 C24 N14 C28 2.8(2) . . . . ? C23 C24 N14 C28 -173.42(15) . . . . ? C25 C24 N14 Ni2 179.74(13) . . . . ? C23 C24 N14 Ni2 3.6(2) . . . . ? F2 Ni2 N14 C28 0.45(11) 2_656 . . . ? F1 Ni2 N14 C28 -28.5(3) 2_656 . . . ? N13 Ni2 N14 C28 91.30(11) . . . . ? N12 Ni2 N14 C28 -177.56(11) . . . . ? N11 Ni2 N14 C28 -101.52(11) . . . . ? F2 Ni2 N14 C24 -176.61(13) 2_656 . . . ? F1 Ni2 N14 C24 154.5(2) 2_656 . . . ? N13 Ni2 N14 C24 -85.76(13) . . . . ? N12 Ni2 N14 C24 5.38(14) . . . . ? N11 Ni2 N14 C24 81.42(13) . . . . ? N15 C3 C31 N16 -29.49(19) . . . . ? C2 C3 C31 N16 145.65(15) . . . . ? C3 C31 N16 C32 178.27(13) . . . . ? C3 C31 N16 C42 -64.76(16) . . . . ? C3 C31 N16 Ni1 54.12(13) . . . . ? F1 Ni1 N16 C31 37.9(3) . . . . ? F2 Ni1 N16 C31 40.29(9) . . . . ? N18 Ni1 N16 C31 -133.38(10) . . . . ? N17 Ni1 N16 C31 137.80(10) . . . . ? N15 Ni1 N16 C31 -44.31(9) . . . . ? F1 Ni1 N16 C32 -79.2(3) . . . . ? F2 Ni1 N16 C32 -76.83(13) . . . . ? N18 Ni1 N16 C32 109.50(13) . . . . ? N17 Ni1 N16 C32 20.68(13) . . . . ? N15 Ni1 N16 C32 -161.43(14) . . . . ? F1 Ni1 N16 C42 154.42(19) . . . . ? F2 Ni1 N16 C42 156.76(11) . . . . ? N18 Ni1 N16 C42 -16.90(11) . . . . ? N17 Ni1 N16 C42 -105.72(11) . . . . ? N15 Ni1 N16 C42 72.16(11) . . . . ? C31 N16 C32 C33 -91.83(17) . . . . ? C42 N16 C32 C33 150.80(16) . . . . ? Ni1 N16 C32 C33 22.5(2) . . . . ? N16 C32 C33 C34 -75.98(19) . . . . ? C32 C33 C34 N17 69.51(19) . . . . ? C32 C33 C34 C35 -108.45(18) . . . . ? N17 C34 C35 C36 1.5(3) . . . . ? C33 C34 C35 C36 179.38(17) . . . . ? C34 C35 C36 C37 0.7(3) . . . . ? C35 C36 C37 C38 -1.9(3) . . . . ? C36 C37 C38 N17 1.1(3) . . . . ? C37 C38 N17 C34 1.0(2) . . . . ? C37 C38 N17 Ni1 -170.66(13) . . . . ? C35 C34 N17 C38 -2.3(2) . . . . ? C33 C34 N17 C38 179.68(14) . . . . ? C35 C34 N17 Ni1 169.15(13) . . . . ? C33 C34 N17 Ni1 -8.84(19) . . . . ? F1 Ni1 N17 C38 -49.18(12) . . . . ? F2 Ni1 N17 C38 -125.08(11) . . . . ? N18 Ni1 N17 C38 45.73(12) . . . . ? N16 Ni1 N17 C38 141.96(12) . . . . ? N15 Ni1 N17 C38 132.8(2) . . . . ? F1 Ni1 N17 C34 139.40(12) . . . . ? F2 Ni1 N17 C34 63.51(12) . . . . ? N18 Ni1 N17 C34 -125.68(12) . . . . ? N16 Ni1 N17 C34 -29.45(13) . . . . ? N15 Ni1 N17 C34 -38.6(3) . . . . ? C31 N16 C42 C43 166.32(14) . . . . ? C32 N16 C42 C43 -77.31(18) . . . . ? Ni1 N16 C42 C43 53.91(16) . . . . ? N16 C42 C43 C44 -76.8(2) . . . . ? C42 C43 C44 N18 49.1(2) . . . . ? C42 C43 C44 C45 -135.15(18) . . . . ? N18 C44 C45 C46 4.1(3) . . . . ? C43 C44 C45 C46 -171.61(17) . . . . ? C44 C45 C46 C47 0.1(3) . . . . ? C45 C46 C47 C48 -3.8(3) . . . . ? C46 C47 C48 N18 3.7(2) . . . . ? C47 C48 N18 C44 0.4(2) . . . . ? C47 C48 N18 Ni1 179.84(12) . . . . ? C45 C44 N18 C48 -4.3(2) . . . . ? C43 C44 N18 C48 171.43(15) . . . . ? C45 C44 N18 Ni1 176.28(12) . . . . ? C43 C44 N18 Ni1 -8.0(2) . . . . ? F1 Ni1 N18 C48 -3.36(11) . . . . ? F2 Ni1 N18 C48 30.3(3) . . . . ? N17 Ni1 N18 C48 -93.29(11) . . . . ? N16 Ni1 N18 C48 174.93(11) . . . . ? N15 Ni1 N18 C48 99.61(11) . . . . ? F1 Ni1 N18 C44 176.06(12) . . . . ? F2 Ni1 N18 C44 -150.2(2) . . . . ? N17 Ni1 N18 C44 86.14(13) . . . . ? N16 Ni1 N18 C44 -5.64(13) . . . . ? N15 Ni1 N18 C44 -80.96(13) . . . . ? F2 Ni1 F1 Ni2 8.71(3) . . . 2_656 ? N18 Ni1 F1 Ni2 -177.54(4) . . . 2_656 ? N17 Ni1 F1 Ni2 -88.92(5) . . . 2_656 ? N16 Ni1 F1 Ni2 11.1(2) . . . 2_656 ? N15 Ni1 F1 Ni2 90.63(5) . . . 2_656 ? F1 Ni1 F2 Ni2 -8.90(3) . . . 2_656 ? N18 Ni1 F2 Ni2 -43.6(2) . . . 2_656 ? N17 Ni1 F2 Ni2 79.28(5) . . . 2_656 ? N16 Ni1 F2 Ni2 171.57(5) . . . 2_656 ? N15 Ni1 F2 Ni2 -113.38(4) . . . 2_656 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O50 H50 O60 0.84 1.96 2.780(4) 165.1 . O60 H60 F22 0.84 1.98 2.795(4) 164.3 . O51 H51 F18 0.84 1.89 2.730(14) 175.6 . O61 H61 F26 0.84 2.01 2.805(9) 157.6 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.51 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.582 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.049 # Attachment 'wag586.cif' data_wag586 _database_code_depnum_ccdc_archive 'CCDC 842534' #TrackingRef 'wag586.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42.20 H46.90 B4 F16 N8.30 O0.40 Zn2' _chemical_formula_weight 1154.76 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.889(4) _cell_length_b 17.062(8) _cell_length_c 18.513(8) _cell_angle_alpha 64.89(2) _cell_angle_beta 78.41(2) _cell_angle_gamma 89.91(2) _cell_volume 2479.7(19) _cell_formula_units_Z 2 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used 3449 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 22.18 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1171 _exptl_absorpt_coefficient_mu 1.070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6743 _exptl_absorpt_correction_T_max 0.9193 _exptl_absorpt_process_details 'SCALE (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(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 Kappa Apex II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27717 _diffrn_reflns_av_R_equivalents 0.0790 _diffrn_reflns_av_sigmaI/netI 0.0994 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.59 _reflns_number_total 9621 _reflns_number_gt 5969 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Entire complex in the assym unit: [Zn2 LEt (BF4)2] (BF4)2 .(0.4Et2O) .(0.3MeCN) One of the tetrafluoroborate anions is disordered and was modelled by splitting it into two complete parts with B4-F41-F44 and B41-F45-F48 with 0.70:0.30 occupancy. Both parts were restrained to have similar geometry to the well behaved B1-F11-F14 anion by the SAME instruction, and SIMU B41 was used with default esds. A region of overlapping disordered solvent molecules was modelled as two 0.20 occupancy Et2O molecules and one 0.3 occupancy MeCN. The two EtO molecules were restrained using SADI to have similar bond lengths. DFIX and DANg were employed to help restrain the geometry of the 0.3 occupancy MeCN. All non-hydrogen atoms were modelled anisotropically except for these disordered solvent molecules. Two of the carbon atoms of the pyridine ring are split into two parts (C26 and C27) vs (C126 and C127), with 0.50 occupancies, due to a 'flap' type disorder of this ring, hinged at N14 and C24. All H atoms are in calculated positions and ride on the attached non-H atom. OMIT 0 0 1 was employed as this reflection was behind the beamstop. ; _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^)+(0.0866P)^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 9621 _refine_ls_number_parameters 754 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.1051 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1717 _refine_ls_wR_factor_gt 0.1445 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.048 _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 Zn1 Zn 0.53561(6) 0.20675(4) 0.24114(3) 0.02794(17) Uani 1 1 d . . . Zn2 Zn 0.74560(6) -0.20072(4) 0.36400(3) 0.02614(17) Uani 1 1 d . . . C1 C 0.7376(6) 0.0964(3) 0.3516(3) 0.0296(11) Uani 1 1 d . . . C2 C 0.8172(6) 0.0333(3) 0.3974(3) 0.0321(12) Uani 1 1 d . . . H2 H 0.8703 0.0421 0.4334 0.038 Uiso 1 1 calc R . . C3 C 0.8189(5) -0.0437(3) 0.3902(3) 0.0263(11) Uani 1 1 d . . . C4 C 0.6718(5) 0.0091(3) 0.2944(3) 0.0233(10) Uani 1 1 d . . . N11 N 0.6600(4) 0.0854(2) 0.3000(2) 0.0253(9) Uani 1 1 d . . . N15 N 0.7462(4) -0.0563(2) 0.3386(2) 0.0216(8) Uani 1 1 d . . . C5 C 0.6041(5) 0.0010(3) 0.2300(3) 0.0217(10) Uani 1 1 d . . . C6 C 0.7007(6) 0.0122(3) 0.1579(3) 0.0331(12) Uani 1 1 d . . . H6 H 0.8090 0.0224 0.1505 0.040 Uiso 1 1 calc R . . C7 C 0.6401(6) 0.0085(4) 0.0954(3) 0.0373(13) Uani 1 1 d . . . H7 H 0.7062 0.0164 0.0452 0.045 Uiso 1 1 calc R . . C8 C 0.4816(6) -0.0069(3) 0.1077(3) 0.0342(12) Uani 1 1 d . . . H8 H 0.4394 -0.0096 0.0654 0.041 Uiso 1 1 calc R . . C9 C 0.3857(6) -0.0182(3) 0.1795(3) 0.0294(11) Uani 1 1 d . . . H9 H 0.2774 -0.0286 0.1869 0.035 Uiso 1 1 calc R . . C10 C 0.4455(5) -0.0146(3) 0.2416(3) 0.0257(10) Uani 1 1 d . . . H10 H 0.3789 -0.0228 0.2918 0.031 Uiso 1 1 calc R . . C11 C 0.7322(6) 0.1828(3) 0.3546(3) 0.0335(12) Uani 1 1 d . . . H11A H 0.6451 0.1793 0.3990 0.040 Uiso 1 1 calc R . . H11B H 0.8286 0.1967 0.3676 0.040 Uiso 1 1 calc R . . N12 N 0.7137(5) 0.2536(3) 0.2760(2) 0.0284(9) Uani 1 1 d . . . C12 C 0.8560(6) 0.2679(4) 0.2103(3) 0.0393(13) Uani 1 1 d . . . H12A H 0.8799 0.2111 0.2105 0.047 Uiso 1 1 calc R . . H12B H 0.9438 0.2902 0.2240 0.047 Uiso 1 1 calc R . . C13 C 0.8429(6) 0.3305(4) 0.1248(3) 0.0415(14) Uani 1 1 d . . . H13A H 0.9487 0.3521 0.0911 0.050 Uiso 1 1 calc R . . H13B H 0.7928 0.3810 0.1283 0.050 Uiso 1 1 calc R . . C14 C 0.7548(6) 0.2967(3) 0.0792(3) 0.0354(12) Uani 1 1 d . . . C15 C 0.8012(7) 0.3271(4) -0.0045(3) 0.0441(14) Uani 1 1 d . . . H15 H 0.8875 0.3692 -0.0337 0.053 Uiso 1 1 calc R . . C16 C 0.7234(7) 0.2969(4) -0.0459(3) 0.0509(16) Uani 1 1 d . . . H16 H 0.7555 0.3172 -0.1035 0.061 Uiso 1 1 calc R . . C17 C 0.5966(7) 0.2360(4) -0.0019(3) 0.0474(15) Uani 1 1 d . . . H17 H 0.5399 0.2139 -0.0288 0.057 Uiso 1 1 calc R . . C18 C 0.5552(7) 0.2085(4) 0.0809(3) 0.0414(14) Uani 1 1 d . . . H18 H 0.4690 0.1665 0.1109 0.050 Uiso 1 1 calc R . . N13 N 0.6304(5) 0.2379(3) 0.1220(2) 0.0326(10) Uani 1 1 d . . . C22 C 0.6960(6) 0.3354(3) 0.2882(3) 0.0392(13) Uani 1 1 d . . . H22A H 0.7337 0.3865 0.2352 0.047 Uiso 1 1 calc R . . H22B H 0.7601 0.3355 0.3262 0.047 Uiso 1 1 calc R . . C23 C 0.5299(7) 0.3428(3) 0.3224(3) 0.0411(14) Uani 1 1 d . . . H23A H 0.4839 0.2853 0.3663 0.049 Uiso 1 1 calc R . . H23B H 0.5277 0.3839 0.3475 0.049 Uiso 1 1 calc R . . C24 C 0.4333(7) 0.3728(3) 0.2605(4) 0.0427(14) Uani 1 1 d . B . C25 C 0.3531(10) 0.4458(4) 0.2460(5) 0.078(2) Uani 1 1 d . . . H25 H 0.3392 0.4731 0.2819 0.094 Uiso 1 1 calc R A 1 C26 C 0.292(4) 0.478(2) 0.1729(19) 0.097(12) Uani 0.50 1 d P B 1 H26 H 0.2468 0.5314 0.1563 0.116 Uiso 0.50 1 calc PR B 1 C126 C 0.234(3) 0.465(2) 0.2044(17) 0.063(7) Uani 0.50 1 d P B 2 H126 H 0.189(14) 0.537(9) 0.174(8) 0.075 Uiso 0.50 1 d P C 2 C27 C 0.297(3) 0.4331(17) 0.1284(16) 0.091(8) Uani 0.50 1 d P B 1 H27 H 0.2721 0.4571 0.0761 0.109 Uiso 0.50 1 calc PR B 1 C127 C 0.225(2) 0.4161(12) 0.1599(12) 0.047(4) Uani 0.50 1 d P B 2 H127 H 0.1471 0.4237 0.1295 0.057 Uiso 0.50 1 calc PR B 2 C28 C 0.3403(9) 0.3518(4) 0.1619(5) 0.075(2) Uani 1 1 d . . . H28 H 0.3093 0.3109 0.1441 0.089 Uiso 1 1 calc R B 1 N14 N 0.4242(5) 0.3259(3) 0.2187(3) 0.0423(12) Uani 1 1 d . B . C31 C 0.9002(6) -0.1162(3) 0.4407(3) 0.0285(11) Uani 1 1 d . . . H31A H 0.9973 -0.0918 0.4449 0.034 Uiso 1 1 calc R . . H31B H 0.8349 -0.1461 0.4967 0.034 Uiso 1 1 calc R . . N16 N 0.9364(4) -0.1802(3) 0.4078(2) 0.0262(9) Uani 1 1 d . . . C32 C 1.0672(5) -0.1413(3) 0.3338(3) 0.0286(11) Uani 1 1 d . . . H32A H 1.1626 -0.1352 0.3516 0.034 Uiso 1 1 calc R . . H32B H 1.0450 -0.0823 0.2977 0.034 Uiso 1 1 calc R . . C33 C 1.0949(5) -0.1951(3) 0.2852(3) 0.0331(12) Uani 1 1 d . . . H33A H 1.2041 -0.1822 0.2552 0.040 Uiso 1 1 calc R . . H33B H 1.0804 -0.2572 0.3246 0.040 Uiso 1 1 calc R . . C34 C 0.9970(6) -0.1828(3) 0.2249(3) 0.0324(12) Uani 1 1 d . . . C35 C 1.0643(7) -0.1700(4) 0.1460(3) 0.0456(14) Uani 1 1 d . . . H35 H 1.1734 -0.1644 0.1282 0.055 Uiso 1 1 calc R . . C36 C 0.9701(7) -0.1654(4) 0.0932(3) 0.0495(16) Uani 1 1 d . . . H36 H 1.0145 -0.1573 0.0390 0.059 Uiso 1 1 calc R . . C37 C 0.8116(7) -0.1727(4) 0.1194(3) 0.0434(14) Uani 1 1 d . . . H37 H 0.7450 -0.1703 0.0844 0.052 Uiso 1 1 calc R . . C38 C 0.7543(6) -0.1834(3) 0.1977(3) 0.0349(12) Uani 1 1 d . . . H38 H 0.6455 -0.1871 0.2157 0.042 Uiso 1 1 calc R . . N17 N 0.8414(5) -0.1889(3) 0.2505(2) 0.0310(10) Uani 1 1 d . . . C42 C 0.9870(6) -0.2573(3) 0.4716(3) 0.0337(12) Uani 1 1 d . . . H42A H 1.0469 -0.2374 0.5013 0.040 Uiso 1 1 calc R . . H42B H 1.0560 -0.2873 0.4446 0.040 Uiso 1 1 calc R . . C43 C 0.8534(6) -0.3211(3) 0.5323(3) 0.0377(13) Uani 1 1 d . . . H43A H 0.8878 -0.3581 0.5828 0.045 Uiso 1 1 calc R . . H43B H 0.7698 -0.2885 0.5469 0.045 Uiso 1 1 calc R . . C44 C 0.7910(6) -0.3783(3) 0.4995(3) 0.0376(13) Uani 1 1 d . . . C45 C 0.7858(7) -0.4695(4) 0.5390(4) 0.0529(16) Uani 1 1 d . . . H45 H 0.8214 -0.4971 0.5882 0.063 Uiso 1 1 calc R . . C46 C 0.7295(8) -0.5180(4) 0.5063(4) 0.0639(19) Uani 1 1 d . . . H46 H 0.7233 -0.5796 0.5332 0.077 Uiso 1 1 calc R . . C47 C 0.6821(8) -0.4775(4) 0.4349(5) 0.066(2) Uani 1 1 d . . . H47 H 0.6439 -0.5104 0.4109 0.080 Uiso 1 1 calc R . . C48 C 0.6905(7) -0.3875(4) 0.3978(4) 0.0524(16) Uani 1 1 d . . . H48 H 0.6577 -0.3596 0.3478 0.063 Uiso 1 1 calc R . . N18 N 0.7423(5) -0.3383(3) 0.4290(3) 0.0348(10) Uani 1 1 d . . . B1 B 0.3831(8) 0.6694(4) 0.2556(4) 0.0428(16) Uani 1 1 d D . . F11 F 0.3735(4) 0.6955(2) 0.31872(19) 0.0463(8) Uani 1 1 d D . . F12 F 0.4270(4) 0.7405(3) 0.1823(2) 0.0650(10) Uani 1 1 d D . . F13 F 0.4955(4) 0.6102(3) 0.2656(3) 0.0742(12) Uani 1 1 d D . . F14 F 0.2445(4) 0.6291(2) 0.2627(2) 0.0514(9) Uani 1 1 d D . . B2 B 0.4396(7) -0.2152(4) 0.4540(3) 0.0303(13) Uani 1 1 d . . . F21 F 0.3367(3) -0.1528(2) 0.44958(18) 0.0465(8) Uani 1 1 d . . . F22 F 0.3610(3) -0.2967(2) 0.50284(17) 0.0465(8) Uani 1 1 d . . . F23 F 0.5601(3) -0.20244(19) 0.48840(16) 0.0352(7) Uani 1 1 d . . . F24 F 0.5155(3) -0.2068(2) 0.37339(19) 0.0461(8) Uani 1 1 d . . . B3 B 0.2491(7) 0.1247(4) 0.3554(4) 0.0338(14) Uani 1 1 d . . . F31 F 0.1848(4) 0.0402(2) 0.40041(19) 0.0489(8) Uani 1 1 d . . . F32 F 0.1325(4) 0.1812(2) 0.3535(2) 0.0533(9) Uani 1 1 d . . . F33 F 0.3633(4) 0.1442(2) 0.38873(19) 0.0505(9) Uani 1 1 d . . . F34 F 0.3266(4) 0.1422(2) 0.27173(19) 0.0515(9) Uani 1 1 d . . . B4 B 0.1031(19) 0.1390(9) 0.1216(10) 0.041(8) Uani 0.60 1 d PD D 1 F41 F -0.0089(18) 0.1893(10) 0.0840(10) 0.060(4) Uani 0.60 1 d PD D 1 F42 F 0.1887(17) 0.1159(12) 0.0684(9) 0.174(9) Uani 0.60 1 d PD D 1 F43 F 0.1819(10) 0.1925(6) 0.1445(5) 0.067(2) Uani 0.60 1 d PD D 1 F44 F 0.0377(8) 0.0669(6) 0.1888(5) 0.085(3) Uani 0.60 1 d PD D 1 B41 B 0.116(2) 0.1480(14) 0.1118(12) 0.053(14) Uani 0.40 1 d PD E 2 F45 F 0.1094(17) 0.0965(10) 0.1954(7) 0.086(4) Uani 0.40 1 d PD E 2 F46 F -0.023(3) 0.1579(16) 0.0937(19) 0.078(8) Uani 0.40 1 d PD E 2 F47 F 0.172(2) 0.2323(12) 0.0950(11) 0.165(9) Uani 0.40 1 d PD E 2 F48 F 0.2233(13) 0.1253(9) 0.0642(7) 0.037(3) Uani 0.40 1 d PD E 2 O50 O 0.8269(18) 0.5467(9) 0.1683(9) 0.021(4) Uiso 0.20 1 d PD F 1 C50 C 0.929(3) 0.5082(14) 0.2885(14) 0.022(5) Uiso 0.20 1 d PD F 1 H50A H 0.8395 0.4662 0.3232 0.027 Uiso 0.20 1 calc PR F 1 H50B H 0.9681 0.5335 0.3204 0.027 Uiso 0.20 1 calc PR F 1 H50C H 1.0096 0.4787 0.2684 0.027 Uiso 0.20 1 calc PR F 1 C51 C 0.881(2) 0.5786(11) 0.2176(12) 0.007(4) Uiso 0.20 1 d PD F 1 H51A H 0.7986 0.6079 0.2383 0.008 Uiso 0.20 1 calc PR F 1 H51B H 0.9699 0.6223 0.1843 0.008 Uiso 0.20 1 calc PR F 1 C52 C 0.761(3) 0.6088(12) 0.1104(12) 0.017(5) Uiso 0.20 1 d PD F 1 H52A H 0.8323 0.6626 0.0801 0.021 Uiso 0.20 1 calc PR F 1 H52B H 0.6642 0.6230 0.1375 0.021 Uiso 0.20 1 calc PR F 1 C53 C 0.727(3) 0.5750(18) 0.0520(16) 0.036(6) Uiso 0.20 1 d PD F 1 H53A H 0.8084 0.5390 0.0431 0.043 Uiso 0.20 1 calc PR F 1 H53B H 0.7240 0.6240 -0.0002 0.043 Uiso 0.20 1 calc PR F 1 H53C H 0.6275 0.5399 0.0750 0.043 Uiso 0.20 1 calc PR F 1 O60 O 0.803(2) 0.5584(12) 0.1370(13) 0.037(5) Uiso 0.20 1 d PD G 2 C61 C 0.846(3) 0.5911(16) 0.1876(16) 0.035(7) Uiso 0.20 1 d PD G 2 H61A H 0.7508 0.6060 0.2158 0.043 Uiso 0.20 1 calc PR G 2 H61B H 0.9112 0.6463 0.1522 0.043 Uiso 0.20 1 calc PR G 2 C62 C 0.703(4) 0.6045(19) 0.090(2) 0.055(9) Uiso 0.20 1 d PD G 2 H62A H 0.7580 0.6596 0.0458 0.066 Uiso 0.20 1 calc PR G 2 H62B H 0.6173 0.6190 0.1239 0.066 Uiso 0.20 1 calc PR G 2 C63 C 0.639(3) 0.5546(18) 0.0528(16) 0.036(6) Uiso 0.20 1 d PD G 2 H63A H 0.7225 0.5301 0.0282 0.043 Uiso 0.20 1 calc PR G 2 H63B H 0.5875 0.5931 0.0105 0.043 Uiso 0.20 1 calc PR G 2 H63C H 0.5642 0.5075 0.0952 0.043 Uiso 0.20 1 calc PR G 2 N70 N 0.8661(17) 0.5323(9) 0.1066(9) 0.042(4) Uiso 0.30 1 d PD H 3 C70 C 0.786(2) 0.5810(11) 0.0811(12) 0.038(4) Uiso 0.30 1 d PD H 3 C71 C 0.675(2) 0.6439(14) 0.0708(15) 0.061(6) Uiso 0.30 1 d PD H 3 H71A H 0.5867 0.6253 0.0553 0.073 Uiso 0.30 1 calc PR H 3 H71B H 0.7222 0.7006 0.0277 0.073 Uiso 0.30 1 calc PR H 3 H71C H 0.6388 0.6487 0.1222 0.073 Uiso 0.30 1 calc PR H 3 C60 C 0.927(4) 0.538(2) 0.250(2) 0.055(9) Uiso 0.20 1 d PD G 2 H60A H 0.8675 0.4815 0.2836 0.066 Uiso 0.20 1 calc PR G 2 H60B H 0.9386 0.5674 0.2840 0.066 Uiso 0.20 1 calc PR G 2 H60C H 1.0286 0.5300 0.2232 0.066 Uiso 0.20 1 calc PR G 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0282(3) 0.0317(3) 0.0247(3) -0.0128(3) -0.0062(2) -0.0036(2) Zn2 0.0209(3) 0.0327(3) 0.0248(3) -0.0106(3) -0.0090(2) -0.0016(2) C1 0.035(3) 0.031(3) 0.026(3) -0.016(2) -0.007(2) -0.002(2) C2 0.031(3) 0.044(3) 0.032(3) -0.021(3) -0.017(2) 0.001(2) C3 0.021(2) 0.036(3) 0.021(2) -0.011(2) -0.006(2) -0.003(2) C4 0.021(2) 0.033(3) 0.019(2) -0.013(2) -0.006(2) -0.001(2) N11 0.026(2) 0.034(2) 0.025(2) -0.0186(19) -0.0114(18) 0.0002(18) N15 0.021(2) 0.029(2) 0.019(2) -0.0116(17) -0.0098(16) 0.0014(16) C5 0.022(2) 0.025(2) 0.023(2) -0.012(2) -0.011(2) 0.0002(19) C6 0.021(3) 0.055(3) 0.032(3) -0.026(3) -0.010(2) 0.004(2) C7 0.037(3) 0.054(4) 0.029(3) -0.023(3) -0.012(2) 0.009(3) C8 0.042(3) 0.043(3) 0.029(3) -0.020(3) -0.022(2) 0.005(2) C9 0.028(3) 0.034(3) 0.028(3) -0.013(2) -0.013(2) -0.003(2) C10 0.024(2) 0.029(3) 0.023(2) -0.010(2) -0.006(2) -0.001(2) C11 0.040(3) 0.033(3) 0.032(3) -0.014(2) -0.017(2) 0.005(2) N12 0.035(2) 0.032(2) 0.021(2) -0.0144(19) -0.0066(18) -0.0007(18) C12 0.031(3) 0.052(4) 0.039(3) -0.025(3) -0.001(2) -0.009(3) C13 0.037(3) 0.050(3) 0.034(3) -0.020(3) 0.004(2) -0.015(3) C14 0.041(3) 0.036(3) 0.029(3) -0.015(2) -0.003(2) -0.003(2) C15 0.052(4) 0.043(3) 0.024(3) -0.007(3) 0.004(3) -0.012(3) C16 0.075(5) 0.054(4) 0.022(3) -0.017(3) -0.004(3) -0.004(3) C17 0.077(4) 0.042(3) 0.024(3) -0.012(3) -0.017(3) -0.006(3) C18 0.052(4) 0.039(3) 0.032(3) -0.012(3) -0.013(3) -0.012(3) N13 0.040(3) 0.034(2) 0.024(2) -0.013(2) -0.0059(19) -0.004(2) C22 0.053(4) 0.038(3) 0.038(3) -0.026(3) -0.011(3) -0.003(3) C23 0.058(4) 0.033(3) 0.037(3) -0.023(3) -0.005(3) -0.002(3) C24 0.056(4) 0.027(3) 0.046(3) -0.015(3) -0.016(3) 0.003(3) C25 0.118(7) 0.047(4) 0.095(6) -0.041(4) -0.054(6) 0.036(4) C26 0.15(3) 0.057(19) 0.11(3) -0.046(19) -0.07(2) 0.08(2) C126 0.079(15) 0.043(10) 0.065(15) -0.021(10) -0.020(11) 0.007(10) C27 0.11(2) 0.079(17) 0.09(2) -0.020(15) -0.070(16) 0.034(16) C127 0.046(10) 0.032(8) 0.063(12) -0.018(8) -0.015(8) 0.004(7) C28 0.106(6) 0.039(4) 0.105(6) -0.033(4) -0.075(5) 0.021(4) N14 0.054(3) 0.031(3) 0.047(3) -0.017(2) -0.022(2) 0.005(2) C31 0.031(3) 0.035(3) 0.024(3) -0.012(2) -0.016(2) 0.001(2) N16 0.021(2) 0.032(2) 0.024(2) -0.0081(19) -0.0098(17) -0.0018(17) C32 0.017(2) 0.037(3) 0.031(3) -0.013(2) -0.006(2) -0.003(2) C33 0.023(3) 0.039(3) 0.032(3) -0.012(2) -0.004(2) 0.000(2) C34 0.033(3) 0.032(3) 0.033(3) -0.016(2) -0.005(2) 0.003(2) C35 0.044(3) 0.053(4) 0.041(3) -0.026(3) -0.001(3) 0.002(3) C36 0.063(4) 0.059(4) 0.027(3) -0.020(3) -0.009(3) 0.006(3) C37 0.054(4) 0.049(4) 0.036(3) -0.022(3) -0.020(3) 0.006(3) C38 0.034(3) 0.044(3) 0.034(3) -0.023(3) -0.009(2) 0.001(2) N17 0.030(2) 0.035(2) 0.031(2) -0.016(2) -0.0084(19) 0.0013(19) C42 0.028(3) 0.036(3) 0.036(3) -0.009(2) -0.021(2) 0.003(2) C43 0.036(3) 0.039(3) 0.031(3) -0.004(3) -0.017(2) 0.006(2) C44 0.022(3) 0.038(3) 0.038(3) -0.002(3) -0.006(2) -0.003(2) C45 0.045(4) 0.042(4) 0.056(4) -0.003(3) -0.021(3) -0.003(3) C46 0.068(5) 0.031(3) 0.082(5) -0.007(4) -0.032(4) -0.002(3) C47 0.073(5) 0.038(4) 0.098(6) -0.023(4) -0.051(4) -0.002(3) C48 0.063(4) 0.038(3) 0.062(4) -0.017(3) -0.037(3) 0.003(3) N18 0.030(2) 0.031(2) 0.040(3) -0.008(2) -0.016(2) -0.0027(19) B1 0.044(4) 0.047(4) 0.054(4) -0.031(4) -0.026(3) 0.009(3) F11 0.053(2) 0.056(2) 0.050(2) -0.0334(17) -0.0294(17) 0.0097(16) F12 0.067(3) 0.080(3) 0.045(2) -0.022(2) -0.0188(19) -0.014(2) F13 0.064(2) 0.096(3) 0.115(3) -0.080(3) -0.055(2) 0.042(2) F14 0.0469(19) 0.055(2) 0.068(2) -0.0336(19) -0.0302(18) 0.0004(16) B2 0.030(3) 0.040(4) 0.023(3) -0.014(3) -0.009(2) 0.000(3) F21 0.0423(18) 0.067(2) 0.0419(19) -0.0310(17) -0.0174(15) 0.0208(16) F22 0.0460(19) 0.048(2) 0.0335(17) -0.0087(15) -0.0046(15) -0.0184(15) F23 0.0282(15) 0.0500(19) 0.0283(15) -0.0157(14) -0.0110(13) -0.0068(13) F24 0.0402(18) 0.053(2) 0.0451(19) -0.0218(16) -0.0076(15) 0.0019(15) B3 0.024(3) 0.045(4) 0.032(3) -0.017(3) -0.003(3) -0.002(3) F31 0.0447(19) 0.051(2) 0.0400(18) -0.0117(16) -0.0052(15) -0.0158(16) F32 0.0417(19) 0.071(2) 0.056(2) -0.0382(19) -0.0058(16) 0.0151(17) F33 0.048(2) 0.068(2) 0.047(2) -0.0332(18) -0.0160(16) -0.0048(17) F34 0.053(2) 0.053(2) 0.047(2) -0.0261(17) -0.0005(16) -0.0010(16) B4 0.031(11) 0.058(13) 0.040(12) -0.032(10) 0.006(9) 0.008(9) F41 0.056(6) 0.093(9) 0.060(5) -0.049(6) -0.039(4) 0.037(5) F42 0.198(15) 0.33(2) 0.113(11) -0.165(13) -0.124(10) 0.214(14) F43 0.065(5) 0.088(6) 0.055(5) -0.032(5) -0.027(4) -0.017(4) F44 0.044(4) 0.077(6) 0.083(6) 0.021(4) -0.031(4) -0.033(4) B41 0.05(2) 0.07(2) 0.031(17) -0.009(15) -0.031(15) -0.017(17) F45 0.101(11) 0.115(13) 0.033(6) -0.026(7) -0.006(7) 0.044(9) F46 0.054(9) 0.122(19) 0.129(18) -0.105(17) -0.060(11) 0.052(11) F47 0.106(13) 0.24(2) 0.129(16) -0.073(16) -0.001(13) -0.105(15) F48 0.018(4) 0.067(7) 0.016(5) -0.009(5) -0.001(4) 0.006(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 Zn1 F34 2.010(3) . y Zn1 N13 2.030(4) . y Zn1 N12 2.101(4) . y Zn1 N14 2.175(4) . y Zn1 N11 2.294(4) . y Zn2 F24 2.016(3) . y Zn2 N17 2.026(4) . y Zn2 N16 2.109(4) . y Zn2 N18 2.133(4) . y Zn2 N15 2.304(4) . y C1 N11 1.357(6) . ? C1 C2 1.357(7) . ? C1 C11 1.499(6) . ? C2 C3 1.374(7) . ? C2 H2 0.9500 . ? C3 N15 1.343(5) . ? C3 C31 1.488(6) . ? C4 N15 1.339(6) . ? C4 N11 1.350(6) . ? C4 C5 1.494(6) . ? C5 C6 1.372(6) . ? C5 C10 1.391(6) . ? C6 C7 1.394(6) . ? C6 H6 0.9500 . ? C7 C8 1.388(7) . ? C7 H7 0.9500 . ? C8 C9 1.363(7) . ? C8 H8 0.9500 . ? C9 C10 1.384(6) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 N12 1.486(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? N12 C12 1.506(6) . ? N12 C22 1.509(6) . ? C12 C13 1.516(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.529(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N13 1.354(6) . ? C14 C15 1.380(7) . ? C15 C16 1.371(8) . ? C15 H15 0.9500 . ? C16 C17 1.389(8) . ? C16 H16 0.9500 . ? C17 C18 1.368(7) . ? C17 H17 0.9500 . ? C18 N13 1.344(6) . ? C18 H18 0.9500 . ? C22 C23 1.513(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.487(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N14 1.340(7) . ? C24 C25 1.386(8) . ? C25 C126 1.39(4) . ? C25 C26 1.45(4) . ? C25 H25 0.9500 . ? C26 C27 1.33(4) . ? C26 H26 0.9500 . ? C26 H126 1.37(13) . ? C126 C127 1.41(4) . ? C126 H126 1.21(13) . ? C27 C28 1.35(3) . ? C27 H27 0.9500 . ? C127 C28 1.50(2) . ? C127 H127 0.9500 . ? C28 N14 1.333(7) . ? C28 H28 0.9500 . ? C31 N16 1.468(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? N16 C42 1.490(6) . ? N16 C32 1.503(6) . ? C32 C33 1.525(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.495(7) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 N17 1.358(6) . ? C34 C35 1.386(7) . ? C35 C36 1.388(8) . ? C35 H35 0.9500 . ? C36 C37 1.382(8) . ? C36 H36 0.9500 . ? C37 C38 1.368(7) . ? C37 H37 0.9500 . ? C38 N17 1.337(6) . ? C38 H38 0.9500 . ? C42 C43 1.513(7) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.505(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 N18 1.353(6) . ? C44 C45 1.407(8) . ? C45 C46 1.359(8) . ? C45 H45 0.9500 . ? C46 C47 1.360(9) . ? C46 H46 0.9500 . ? C47 C48 1.386(8) . ? C47 H47 0.9500 . ? C48 N18 1.329(7) . ? C48 H48 0.9500 . ? B1 F12 1.363(7) . ? B1 F14 1.367(7) . ? B1 F13 1.402(7) . ? B1 F11 1.404(7) . ? B2 F22 1.387(6) . ? B2 F21 1.389(6) . ? B2 F23 1.411(6) . ? B2 F24 1.456(6) . ? B3 F31 1.375(7) . ? B3 F33 1.396(6) . ? B3 F32 1.409(7) . ? B3 F34 1.464(7) . ? B4 F42 1.315(14) . ? B4 F44 1.346(16) . ? B4 F43 1.399(13) . ? B4 F41 1.408(15) . ? B41 F48 1.334(18) . ? B41 F46 1.342(17) . ? B41 F47 1.404(16) . ? B41 F45 1.408(18) . ? O50 C52 1.380(17) . ? O50 C51 1.399(17) . ? C50 C51 1.49(2) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.50(2) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? O60 C62 1.38(2) . ? O60 C61 1.387(18) . ? C61 C60 1.45(2) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.47(2) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? N70 C70 1.106(9) . ? C70 C71 1.439(9) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F34 Zn1 N13 108.98(15) . . y F34 Zn1 N12 149.31(14) . . y N13 Zn1 N12 101.59(16) . . y F34 Zn1 N14 88.87(16) . . y N13 Zn1 N14 96.04(17) . . y N12 Zn1 N14 90.66(16) . . y F34 Zn1 N11 95.48(14) . . y N13 Zn1 N11 98.60(15) . . y N12 Zn1 N11 76.95(14) . . y N14 Zn1 N11 162.43(15) . . y F24 Zn2 N17 106.03(15) . . y F24 Zn2 N16 149.08(14) . . y N17 Zn2 N16 103.63(16) . . y F24 Zn2 N18 92.69(15) . . y N17 Zn2 N18 98.18(17) . . y N16 Zn2 N18 91.59(15) . . y F24 Zn2 N15 89.50(13) . . y N17 Zn2 N15 100.20(15) . . y N16 Zn2 N15 76.76(14) . . y N18 Zn2 N15 160.12(15) . . y N11 C1 C2 122.0(4) . . ? N11 C1 C11 116.3(4) . . ? C2 C1 C11 121.7(4) . . ? C1 C2 C3 118.3(4) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? N15 C3 C2 121.3(4) . . ? N15 C3 C31 118.0(4) . . ? C2 C3 C31 120.7(4) . . ? N15 C4 N11 125.0(4) . . ? N15 C4 C5 118.6(4) . . ? N11 C4 C5 116.3(4) . . ? C4 N11 C1 116.0(4) . . ? C4 N11 Zn1 134.8(3) . . ? C1 N11 Zn1 109.2(3) . . ? C4 N15 C3 117.2(4) . . ? C4 N15 Zn2 133.3(3) . . ? C3 N15 Zn2 108.5(3) . . ? C6 C5 C10 120.4(4) . . ? C6 C5 C4 118.7(4) . . ? C10 C5 C4 120.8(4) . . ? C5 C6 C7 120.0(4) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C8 C7 C6 119.1(5) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? C9 C8 C7 120.9(4) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 120.2(4) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C5 119.5(4) . . ? C9 C10 H10 120.3 . . ? C5 C10 H10 120.3 . . ? N12 C11 C1 112.1(4) . . ? N12 C11 H11A 109.2 . . ? C1 C11 H11A 109.2 . . ? N12 C11 H11B 109.2 . . ? C1 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C11 N12 C12 109.7(4) . . ? C11 N12 C22 107.5(4) . . ? C12 N12 C22 108.8(4) . . ? C11 N12 Zn1 106.4(3) . . ? C12 N12 Zn1 105.5(3) . . ? C22 N12 Zn1 118.7(3) . . ? N12 C12 C13 114.6(4) . . ? N12 C12 H12A 108.6 . . ? C13 C12 H12A 108.6 . . ? N12 C12 H12B 108.6 . . ? C13 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? C12 C13 C14 117.9(4) . . ? C12 C13 H13A 107.8 . . ? C14 C13 H13A 107.8 . . ? C12 C13 H13B 107.8 . . ? C14 C13 H13B 107.8 . . ? H13A C13 H13B 107.2 . . ? N13 C14 C15 120.9(5) . . ? N13 C14 C13 119.1(4) . . ? C15 C14 C13 120.0(5) . . ? C16 C15 C14 120.4(5) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 118.7(5) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? C18 C17 C16 118.5(5) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? N13 C18 C17 123.3(5) . . ? N13 C18 H18 118.3 . . ? C17 C18 H18 118.3 . . ? C18 N13 C14 118.2(4) . . ? C18 N13 Zn1 118.7(4) . . ? C14 N13 Zn1 122.4(3) . . ? N12 C22 C23 111.9(4) . . ? N12 C22 H22A 109.2 . . ? C23 C22 H22A 109.2 . . ? N12 C22 H22B 109.2 . . ? C23 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C24 C23 C22 113.9(5) . . ? C24 C23 H23A 108.8 . . ? C22 C23 H23A 108.8 . . ? C24 C23 H23B 108.8 . . ? C22 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? N14 C24 C25 120.2(6) . . ? N14 C24 C23 117.5(5) . . ? C25 C24 C23 122.3(5) . . ? C24 C25 C126 124.5(15) . . ? C24 C25 C26 115.8(13) . . ? C126 C25 C26 26.5(15) . . ? C24 C25 H25 122.1 . . ? C126 C25 H25 108.0 . . ? C26 C25 H25 122.1 . . ? C27 C26 C25 121(2) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C27 C26 H126 125(6) . . ? C25 C26 H126 110(6) . . ? H26 C26 H126 20.9 . . ? C25 C126 C127 114(2) . . ? C25 C126 H126 125(6) . . ? C127 C126 H126 114(6) . . ? C26 C27 C28 116(2) . . ? C26 C27 H27 122.0 . . ? C28 C27 H27 122.0 . . ? C126 C127 C28 118(2) . . ? C126 C127 H127 120.8 . . ? C28 C127 H127 120.8 . . ? N14 C28 C27 123.4(13) . . ? N14 C28 C127 120.6(10) . . ? C27 C28 C127 29.5(11) . . ? N14 C28 H28 118.3 . . ? C27 C28 H28 118.3 . . ? C127 C28 H28 112.4 . . ? C28 N14 C24 119.0(5) . . ? C28 N14 Zn1 117.9(4) . . ? C24 N14 Zn1 123.1(4) . . ? N16 C31 C3 113.5(4) . . ? N16 C31 H31A 108.9 . . ? C3 C31 H31A 108.9 . . ? N16 C31 H31B 108.9 . . ? C3 C31 H31B 108.9 . . ? H31A C31 H31B 107.7 . . ? C31 N16 C42 107.9(4) . . ? C31 N16 C32 108.9(4) . . ? C42 N16 C32 108.8(4) . . ? C31 N16 Zn2 108.0(3) . . ? C42 N16 Zn2 117.6(3) . . ? C32 N16 Zn2 105.5(3) . . ? N16 C32 C33 113.4(4) . . ? N16 C32 H32A 108.9 . . ? C33 C32 H32A 108.9 . . ? N16 C32 H32B 108.9 . . ? C33 C32 H32B 108.9 . . ? H32A C32 H32B 107.7 . . ? C34 C33 C32 117.6(4) . . ? C34 C33 H33A 107.9 . . ? C32 C33 H33A 107.9 . . ? C34 C33 H33B 107.9 . . ? C32 C33 H33B 107.9 . . ? H33A C33 H33B 107.2 . . ? N17 C34 C35 121.0(5) . . ? N17 C34 C33 118.6(4) . . ? C35 C34 C33 120.2(5) . . ? C34 C35 C36 119.0(5) . . ? C34 C35 H35 120.5 . . ? C36 C35 H35 120.5 . . ? C37 C36 C35 120.0(5) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C38 C37 C36 117.4(5) . . ? C38 C37 H37 121.3 . . ? C36 C37 H37 121.3 . . ? N17 C38 C37 124.3(5) . . ? N17 C38 H38 117.9 . . ? C37 C38 H38 117.9 . . ? C38 N17 C34 118.3(4) . . ? C38 N17 Zn2 121.2(3) . . ? C34 N17 Zn2 120.5(3) . . ? N16 C42 C43 112.8(4) . . ? N16 C42 H42A 109.0 . . ? C43 C42 H42A 109.0 . . ? N16 C42 H42B 109.0 . . ? C43 C42 H42B 109.0 . . ? H42A C42 H42B 107.8 . . ? C44 C43 C42 112.6(4) . . ? C44 C43 H43A 109.1 . . ? C42 C43 H43A 109.1 . . ? C44 C43 H43B 109.1 . . ? C42 C43 H43B 109.1 . . ? H43A C43 H43B 107.8 . . ? N18 C44 C45 120.7(5) . . ? N18 C44 C43 117.2(4) . . ? C45 C44 C43 122.1(5) . . ? C46 C45 C44 119.6(6) . . ? C46 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C45 C46 C47 119.5(6) . . ? C45 C46 H46 120.3 . . ? C47 C46 H46 120.3 . . ? C46 C47 C48 119.0(6) . . ? C46 C47 H47 120.5 . . ? C48 C47 H47 120.5 . . ? N18 C48 C47 123.0(6) . . ? N18 C48 H48 118.5 . . ? C47 C48 H48 118.5 . . ? C48 N18 C44 118.2(5) . . ? C48 N18 Zn2 118.0(4) . . ? C44 N18 Zn2 123.8(3) . . ? F12 B1 F14 111.6(5) . . ? F12 B1 F13 110.5(6) . . ? F14 B1 F13 109.5(5) . . ? F12 B1 F11 108.9(5) . . ? F14 B1 F11 109.9(5) . . ? F13 B1 F11 106.3(5) . . ? F22 B2 F21 108.6(4) . . ? F22 B2 F23 109.9(4) . . ? F21 B2 F23 109.5(4) . . ? F22 B2 F24 111.9(4) . . ? F21 B2 F24 112.0(4) . . ? F23 B2 F24 104.9(4) . . ? B2 F24 Zn2 108.7(3) . . ? F31 B3 F33 111.7(5) . . ? F31 B3 F32 109.0(4) . . ? F33 B3 F32 109.0(5) . . ? F31 B3 F34 112.5(5) . . ? F33 B3 F34 104.9(4) . . ? F32 B3 F34 109.6(4) . . ? B3 F34 Zn1 110.6(3) . . ? F42 B4 F44 108.9(12) . . ? F42 B4 F43 114.8(15) . . ? F44 B4 F43 109.1(12) . . ? F42 B4 F41 107.7(14) . . ? F44 B4 F41 111.5(13) . . ? F43 B4 F41 104.9(10) . . ? F48 B41 F46 116.6(18) . . ? F48 B41 F47 103.6(17) . . ? F46 B41 F47 104.0(18) . . ? F48 B41 F45 112.0(16) . . ? F46 B41 F45 113(2) . . ? F47 B41 F45 106.4(15) . . ? C52 O50 C51 112.3(15) . . ? O50 C51 C50 112.2(15) . . ? O50 C51 H51A 109.2 . . ? C50 C51 H51A 109.2 . . ? O50 C51 H51B 109.2 . . ? C50 C51 H51B 109.2 . . ? H51A C51 H51B 107.9 . . ? O50 C52 C53 109.6(19) . . ? O50 C52 H52A 109.8 . . ? C53 C52 H52A 109.7 . . ? O50 C52 H52B 109.8 . . ? C53 C52 H52B 109.8 . . ? H52A C52 H52B 108.2 . . ? C62 O60 C61 116(2) . . ? O60 C61 C60 119(2) . . ? O60 C61 H61A 107.5 . . ? C60 C61 H61A 107.5 . . ? O60 C61 H61B 107.5 . . ? C60 C61 H61B 107.5 . . ? H61A C61 H61B 107.0 . . ? O60 C62 C63 112(2) . . ? O60 C62 H62A 109.3 . . ? C63 C62 H62A 109.3 . . ? O60 C62 H62B 109.3 . . ? C63 C62 H62B 109.3 . . ? H62A C62 H62B 108.0 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N70 C70 C71 164(2) . . ? C61 C60 H60A 109.5 . . ? C61 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C61 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 26.59 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 1.147 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.097