# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Richard Winpenny' _publ_contact_author_address ; University of Manchester Manchester UK ; _publ_contact_author_email RICHARD.WINPENNY@MANCHESTER.AC.UK _publ_section_title ; Influencing The Nuclearity and Constitution of Heterometallic Rings Via Templates ; loop_ _publ_author_name 'R. Winpenny' 'Andrei S. Batsanov' 'Finn Krebs Larsen' 'Chris Muryn' 'Jacob Overgaard' ; S.J.Teat ; 'Grigore A. Timco' data_gt216_iso2 _database_code_depnum_ccdc_archive 'CCDC 231872' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'insert name here' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H194 Cr9 F12 N Ni O37' _chemical_formula_weight 2853.35 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 31.133(5) _cell_length_b 17.213(5) _cell_length_c 32.873(5) _cell_angle_alpha 90.000(10) _cell_angle_beta 112.940(10) _cell_angle_gamma 90.000(10) _cell_volume 16223(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5988 _exptl_absorpt_coefficient_mu 0.764 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 17127 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 26.37 _reflns_number_total 17127 _reflns_number_gt 14267 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.1599P)^2^+287.8094P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(4) _refine_ls_number_reflns 17127 _refine_ls_number_parameters 932 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.1322 _refine_ls_R_factor_gt 0.1068 _refine_ls_wR_factor_ref 0.3125 _refine_ls_wR_factor_gt 0.2945 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.00359(6) 0.59505(17) 0.26208(6) 0.0220(4) Uani 1 1 d . . . Cr2 Cr 0.11328(7) 0.56728(18) 0.33429(7) 0.0302(5) Uani 1 1 d . . . Cr3 Cr 0.18600(8) 0.41344(19) 0.37013(9) 0.0390(6) Uani 1 1 d . . . Cr4 Cr 0.17763(8) 0.21700(18) 0.36267(8) 0.0348(5) Uani 1 1 d . . . Cr5 Cr 0.09528(6) 0.09143(17) 0.29882(6) 0.0186(4) Uani 1 1 d . . . Ni6 Ni 0.00122(6) 0.04467(16) 0.23393(6) 0.0306(4) Uani 1 1 d . . . Cr7 Cr -0.10863(6) 0.07459(17) 0.16269(7) 0.0249(4) Uani 1 1 d . . . Cr8 Cr -0.18272(8) 0.22722(19) 0.13628(9) 0.0404(6) Uani 1 1 d . . . Cr9 Cr -0.17506(7) 0.42328(18) 0.14019(8) 0.0324(5) Uani 1 1 d . . . Cr10 Cr -0.09089(6) 0.54846(17) 0.19983(6) 0.0204(4) Uani 1 1 d . . . F1 F 0.0504(2) 0.5355(5) 0.3066(2) 0.0279(15) Uani 1 1 d . . . F2 F 0.1339(2) 0.4665(5) 0.3264(2) 0.0277(16) Uani 1 1 d . . . F3 F 0.1515(2) 0.3194(5) 0.3612(2) 0.0291(16) Uani 1 1 d . . . F4 F 0.1283(2) 0.1917(4) 0.3087(3) 0.0272(16) Uani 1 1 d . . . F5 F 0.0364(2) 0.1439(5) 0.2634(2) 0.0260(15) Uani 1 1 d . . . F6 F 0.0553(3) 0.0022(5) 0.2838(3) 0.0338(18) Uani 1 1 d . . . F7 F -0.0458(2) 0.1086(5) 0.1893(3) 0.0279(16) Uani 1 1 d . . . F8 F -0.1284(2) 0.1782(4) 0.1737(2) 0.0235(15) Uani 1 1 d . . . F9 F -0.1475(2) 0.3235(5) 0.1411(2) 0.0277(15) Uani 1 1 d . . . F10 F -0.1223(2) 0.4516(5) 0.1923(2) 0.0250(15) Uani 1 1 d . . . F11 F -0.0304(2) 0.5035(4) 0.2349(3) 0.0270(16) Uani 1 1 d . . . F12 F -0.0504(2) 0.6390(4) 0.2147(2) 0.0255(15) Uani 1 1 d . . . O1 O 0.0401(3) 0.5962(7) 0.2249(3) 0.031(2) Uani 1 1 d . . . O2 O 0.1133(3) 0.6004(6) 0.2771(3) 0.035(2) Uani 1 1 d . . . O3 O 0.0297(3) 0.6964(5) 0.2860(4) 0.037(2) Uani 1 1 d . . . O4 O 0.0938(3) 0.6694(7) 0.3441(4) 0.043(3) Uani 1 1 d . . . O5 O 0.1125(4) 0.5379(7) 0.3912(3) 0.042(2) Uani 1 1 d . . . O6 O 0.1642(5) 0.4409(6) 0.4163(4) 0.064(4) Uani 1 1 d . . . O7 O 0.1763(4) 0.6075(7) 0.3607(4) 0.043(3) Uani 1 1 d . . . O8 O 0.2238(3) 0.5070(8) 0.3783(6) 0.070(5) Uani 1 1 d . . . O9 O 0.2078(5) 0.3860(8) 0.3255(6) 0.073(5) Uani 1 1 d . . . O10 O 0.2133(3) 0.2571(6) 0.3294(4) 0.041(2) Uani 1 1 d . . . O11 O 0.2397(5) 0.3684(8) 0.4171(6) 0.101(7) Uani 1 1 d . . . O12 O 0.2285(4) 0.2417(7) 0.4184(4) 0.061(4) Uani 1 1 d . . . O13 O 0.1448(4) 0.1783(7) 0.3972(3) 0.045(3) Uani 1 1 d . . . O14 O 0.0838(3) 0.1068(7) 0.3531(3) 0.038(2) Uani 1 1 d . . . O15 O 0.2090(4) 0.1205(7) 0.3661(4) 0.0422(15) Uiso 1 1 d . . . O16 O 0.1519(4) 0.0325(7) 0.3328(3) 0.0422(15) Uiso 1 1 d . . . O17 O 0.1089(3) 0.0760(6) 0.2462(3) 0.034(2) Uani 1 1 d . . . O18 O 0.0382(3) 0.0396(6) 0.1968(3) 0.033(2) Uani 1 1 d . . . O19 O -0.0358(3) 0.0483(6) 0.2706(3) 0.034(2) Uani 1 1 d . . . O20 O -0.1089(3) 0.0396(7) 0.2184(3) 0.035(2) Uani 1 1 d . . . O21 O -0.0261(3) -0.0554(6) 0.2084(4) 0.040(2) Uani 1 1 d . . . O22 O -0.0910(3) -0.0262(6) 0.1488(3) 0.035(2) Uani 1 1 d . . . O23 O -0.1134(4) 0.1121(7) 0.1043(3) 0.041(2) Uani 1 1 d . . . O24 O -0.1718(5) 0.1966(8) 0.0849(4) 0.057(3) Uani 1 1 d . . . O25 O -0.1741(3) 0.0386(7) 0.1367(4) 0.041(3) Uani 1 1 d . . . O26 O -0.2204(4) 0.1359(8) 0.1339(6) 0.070(4) Uani 1 1 d . . . O27 O -0.1969(4) 0.2603(6) 0.1874(5) 0.051(3) Uani 1 1 d . . . O28 O -0.2066(3) 0.3875(6) 0.1772(4) 0.044(3) Uani 1 1 d . . . O29 O -0.2409(4) 0.2753(7) 0.0957(6) 0.080(5) Uani 1 1 d . . . O30 O -0.2280(4) 0.3993(6) 0.0856(4) 0.062(4) Uani 1 1 d . . . O31 O -0.1439(4) 0.4652(7) 0.1028(3) 0.045(3) Uani 1 1 d . . . O32 O -0.0823(3) 0.5340(7) 0.1443(3) 0.036(2) Uani 1 1 d . . . O33 O -0.2049(3) 0.5257(5) 0.1408(4) 0.043(3) Uani 1 1 d . . . O34 O -0.1473(3) 0.6096(5) 0.1681(3) 0.0290(19) Uani 1 1 d . . . O35 O -0.1029(3) 0.5674(6) 0.2542(3) 0.031(2) Uani 1 1 d . . . O36 O -0.0310(3) 0.6002(6) 0.3005(3) 0.032(2) Uani 1 1 d . . . N1 N 0.0215(8) 0.2910(9) 0.2325(6) 0.079(6) Uani 1 1 d . . . H1 H 0.0287 0.2419 0.2432 0.095 Uiso 1 1 calc R . . C1 C 0.0839(5) 0.6034(9) 0.2373(4) 0.035(3) Uiso 1 1 d . . . C2 C 0.1030(4) 0.6234(8) 0.2030(4) 0.047(4) Uiso 1 1 d D . . C3 C 0.0718(7) 0.5896(14) 0.1586(6) 0.113(6) Uiso 1 1 d D . . H3A H 0.0840 0.6027 0.1369 0.170 Uiso 1 1 calc R . . H3B H 0.0409 0.6105 0.1500 0.170 Uiso 1 1 calc R . . H3C H 0.0706 0.5341 0.1610 0.170 Uiso 1 1 calc R . . C4 C 0.1041(8) 0.7113(8) 0.1993(8) 0.113(6) Uiso 1 1 d D . . H4A H 0.1155 0.7251 0.1770 0.170 Uiso 1 1 calc R . . H4B H 0.1244 0.7327 0.2272 0.170 Uiso 1 1 calc R . . H4C H 0.0732 0.7318 0.1915 0.170 Uiso 1 1 calc R . . C5 C 0.1520(5) 0.5915(14) 0.2163(8) 0.113(6) Uiso 1 1 d D . . H5A H 0.1635 0.6039 0.1938 0.170 Uiso 1 1 calc R . . H5B H 0.1515 0.5362 0.2195 0.170 Uiso 1 1 calc R . . H5C H 0.1720 0.6144 0.2438 0.170 Uiso 1 1 calc R . . C6 C 0.0632(5) 0.7154(10) 0.3198(5) 0.039(3) Uiso 1 1 d . . . C7 C 0.0706(3) 0.8019(7) 0.3292(3) 0.050(4) Uiso 1 1 d D . . C8 C 0.0241(3) 0.8421(10) 0.3185(4) 0.052(2) Uiso 1 1 d D . . H8A H 0.0291 0.8967 0.3243 0.079 Uiso 1 1 calc R . . H8B H 0.0090 0.8207 0.3365 0.079 Uiso 1 1 calc R . . H8C H 0.0047 0.8342 0.2879 0.079 Uiso 1 1 calc R . . C9 C 0.0938(4) 0.8330(10) 0.2996(4) 0.052(2) Uiso 1 1 d D . . H9A H 0.0990 0.8878 0.3045 0.079 Uiso 1 1 calc R . . H9B H 0.0739 0.8239 0.2693 0.079 Uiso 1 1 calc R . . H9C H 0.1231 0.8071 0.3064 0.079 Uiso 1 1 calc R . . C10 C 0.1019(4) 0.8161(10) 0.3772(3) 0.052(2) Uiso 1 1 d D . . H10A H 0.1063 0.8709 0.3824 0.079 Uiso 1 1 calc R . . H10B H 0.1316 0.7916 0.3837 0.079 Uiso 1 1 calc R . . H10C H 0.0877 0.7947 0.3959 0.079 Uiso 1 1 calc R . . C11 C 0.1332(6) 0.4876(11) 0.4186(6) 0.048(4) Uiso 1 1 d . . . C12 C 0.1219(6) 0.4781(10) 0.4604(5) 0.056(4) Uiso 1 1 d D . . C13 C 0.0692(6) 0.475(2) 0.4451(12) 0.198(12) Uiso 1 1 d D . . H13A H 0.0573 0.4320 0.4252 0.297 Uiso 1 1 calc R . . H13B H 0.0560 0.5224 0.4301 0.297 Uiso 1 1 calc R . . H13C H 0.0611 0.4685 0.4702 0.297 Uiso 1 1 calc R . . C14 C 0.1402(12) 0.5520(14) 0.4863(13) 0.198(12) Uiso 1 1 d D . . H14A H 0.1264 0.5961 0.4680 0.297 Uiso 1 1 calc R . . H14B H 0.1735 0.5542 0.4955 0.297 Uiso 1 1 calc R . . H14C H 0.1324 0.5527 0.5118 0.297 Uiso 1 1 calc R . . C15 C 0.1434(12) 0.4081(15) 0.4891(13) 0.198(12) Uiso 1 1 d D . . H15A H 0.1308 0.3614 0.4729 0.297 Uiso 1 1 calc R . . H15B H 0.1364 0.4097 0.5151 0.297 Uiso 1 1 calc R . . H15C H 0.1766 0.4090 0.4976 0.297 Uiso 1 1 calc R . . C16 C 0.2153(5) 0.5768(10) 0.3717(5) 0.039(3) Uiso 1 1 d . . . C17 C 0.2568(4) 0.6301(7) 0.3804(4) 0.048(4) Uiso 1 1 d D . . C18 C 0.2424(7) 0.7146(9) 0.3712(6) 0.073(3) Uiso 1 1 d D . . H18A H 0.2218 0.7205 0.3408 0.110 Uiso 1 1 calc R . . H18B H 0.2696 0.7462 0.3773 0.110 Uiso 1 1 calc R . . H18C H 0.2266 0.7307 0.3898 0.110 Uiso 1 1 calc R . . C19 C 0.2796(6) 0.6038(11) 0.3494(5) 0.073(3) Uiso 1 1 d D . . H19A H 0.2577 0.6085 0.3194 0.110 Uiso 1 1 calc R . . H19B H 0.2891 0.5505 0.3555 0.110 Uiso 1 1 calc R . . H19C H 0.3064 0.6356 0.3539 0.110 Uiso 1 1 calc R . . C20 C 0.2908(6) 0.6209(12) 0.4279(4) 0.073(3) Uiso 1 1 d D . . H20A H 0.3000 0.5675 0.4334 0.110 Uiso 1 1 calc R . . H20B H 0.2761 0.6369 0.4473 0.110 Uiso 1 1 calc R . . H20C H 0.3178 0.6526 0.4329 0.110 Uiso 1 1 calc R . . C21 C 0.2177(6) 0.3186(12) 0.3140(6) 0.055(4) Uiso 1 1 d . . . C22 C 0.2332(9) 0.3148(17) 0.2766(8) 0.100(8) Uiso 1 1 d D . . C23 C 0.2346(17) 0.387(2) 0.2504(16) 0.27(2) Uiso 1 1 d D . . H23A H 0.2055 0.4141 0.2419 0.408 Uiso 1 1 calc R . . H23B H 0.2396 0.3717 0.2244 0.408 Uiso 1 1 calc R . . H23C H 0.2596 0.4200 0.2683 0.408 Uiso 1 1 calc R . . C24 C 0.2817(11) 0.280(3) 0.2971(16) 0.27(2) Uiso 1 1 d D . . H24A H 0.3012 0.3125 0.3208 0.408 Uiso 1 1 calc R . . H24B H 0.2948 0.2761 0.2751 0.408 Uiso 1 1 calc R . . H24C H 0.2799 0.2291 0.3083 0.408 Uiso 1 1 calc R . . C25 C 0.2001(14) 0.256(2) 0.2458(16) 0.27(2) Uiso 1 1 d D . . H25A H 0.1700 0.2790 0.2308 0.408 Uiso 1 1 calc R . . H25B H 0.1973 0.2118 0.2626 0.408 Uiso 1 1 calc R . . H25C H 0.2121 0.2388 0.2244 0.408 Uiso 1 1 calc R . . C26 C 0.2485(5) 0.3038(9) 0.4355(5) 0.039(3) Uiso 1 1 d . . . C27 C 0.2904(4) 0.2965(7) 0.4776(4) 0.055(4) Uiso 1 1 d D . . C28 C 0.3102(7) 0.3749(8) 0.4969(7) 0.080(3) Uiso 1 1 d D . . H28A H 0.3356 0.3676 0.5250 0.120 Uiso 1 1 calc R . . H28B H 0.2863 0.4054 0.5009 0.120 Uiso 1 1 calc R . . H28C H 0.3213 0.4014 0.4772 0.120 Uiso 1 1 calc R . . C29 C 0.3280(6) 0.2484(10) 0.4709(7) 0.080(3) Uiso 1 1 d D . . H29A H 0.3537 0.2417 0.4988 0.120 Uiso 1 1 calc R . . H29B H 0.3384 0.2746 0.4507 0.120 Uiso 1 1 calc R . . H29C H 0.3155 0.1985 0.4591 0.120 Uiso 1 1 calc R . . C30 C 0.2735(7) 0.2544(10) 0.5093(6) 0.080(3) Uiso 1 1 d D . . H30A H 0.2989 0.2483 0.5373 0.120 Uiso 1 1 calc R . . H30B H 0.2616 0.2042 0.4974 0.120 Uiso 1 1 calc R . . H30C H 0.2491 0.2841 0.5130 0.120 Uiso 1 1 calc R . . C31 C 0.1087(5) 0.1368(10) 0.3893(5) 0.036(3) Uiso 1 1 d . . . C32 C 0.0957(5) 0.1151(9) 0.4290(5) 0.055(4) Uiso 1 1 d D . . C33 C 0.0981(9) 0.1845(12) 0.4583(9) 0.132(7) Uiso 1 1 d D . . H33A H 0.1297 0.2030 0.4714 0.198 Uiso 1 1 calc R . . H33B H 0.0879 0.1692 0.4812 0.198 Uiso 1 1 calc R . . H33C H 0.0783 0.2251 0.4409 0.198 Uiso 1 1 calc R . . C34 C 0.1335(7) 0.0572(13) 0.4545(9) 0.132(7) Uiso 1 1 d D . . H34A H 0.1636 0.0801 0.4613 0.198 Uiso 1 1 calc R . . H34B H 0.1305 0.0113 0.4370 0.198 Uiso 1 1 calc R . . H34C H 0.1302 0.0435 0.4815 0.198 Uiso 1 1 calc R . . C35 C 0.0483(6) 0.0766(15) 0.4153(9) 0.132(7) Uiso 1 1 d D . . H35A H 0.0460 0.0347 0.3953 0.198 Uiso 1 1 calc R . . H35B H 0.0243 0.1141 0.4010 0.198 Uiso 1 1 calc R . . H35C H 0.0445 0.0567 0.4410 0.198 Uiso 1 1 calc R . . C36 C 0.1921(5) 0.0511(11) 0.3509(5) 0.0422(15) Uiso 1 1 d . . . C37 C 0.2300(4) -0.0127(8) 0.3667(4) 0.045(3) Uiso 1 1 d D . . C38 C 0.2789(6) 0.0173(16) 0.3760(7) 0.106(5) Uiso 1 1 d D . . H38A H 0.2881 0.0527 0.4005 0.159 Uiso 1 1 calc R . . H38B H 0.2791 0.0437 0.3504 0.159 Uiso 1 1 calc R . . H38C H 0.3003 -0.0256 0.3831 0.159 Uiso 1 1 calc R . . C39 C 0.2295(9) -0.0509(15) 0.4082(6) 0.106(5) Uiso 1 1 d D . . H39A H 0.1991 -0.0720 0.4022 0.159 Uiso 1 1 calc R . . H39B H 0.2369 -0.0129 0.4313 0.159 Uiso 1 1 calc R . . H39C H 0.2522 -0.0919 0.4173 0.159 Uiso 1 1 calc R . . C40 C 0.2166(9) -0.0725(14) 0.3298(6) 0.106(5) Uiso 1 1 d D . . H40A H 0.1858 -0.0917 0.3240 0.159 Uiso 1 1 calc R . . H40B H 0.2384 -0.1148 0.3385 0.159 Uiso 1 1 calc R . . H40C H 0.2172 -0.0488 0.3036 0.159 Uiso 1 1 calc R . . C41 C 0.0810(5) 0.0483(10) 0.2093(5) 0.038(3) Uiso 1 1 d . . . C42 C 0.1040(5) 0.0151(9) 0.1783(5) 0.066(5) Uiso 1 1 d D . . C43 C 0.1528(6) 0.0483(14) 0.1923(7) 0.110(5) Uiso 1 1 d D . . H43A H 0.1709 0.0341 0.2224 0.165 Uiso 1 1 calc R . . H43B H 0.1511 0.1039 0.1898 0.165 Uiso 1 1 calc R . . H43C H 0.1673 0.0280 0.1735 0.165 Uiso 1 1 calc R . . C44 C 0.1072(8) -0.0723(10) 0.1855(8) 0.110(5) Uiso 1 1 d D . . H44A H 0.0765 -0.0932 0.1784 0.165 Uiso 1 1 calc R . . H44B H 0.1263 -0.0832 0.2159 0.165 Uiso 1 1 calc R . . H44C H 0.1208 -0.0957 0.1669 0.165 Uiso 1 1 calc R . . C45 C 0.0766(7) 0.0321(15) 0.1297(6) 0.110(5) Uiso 1 1 d D . . H45A H 0.0454 0.0123 0.1209 0.165 Uiso 1 1 calc R . . H45B H 0.0915 0.0075 0.1124 0.165 Uiso 1 1 calc R . . H45C H 0.0754 0.0872 0.1249 0.165 Uiso 1 1 calc R . . C46 C -0.0803(4) 0.0393(9) 0.2578(4) 0.031(3) Uiso 1 1 d . . . C47 C -0.0984(5) 0.0148(9) 0.2926(4) 0.056(4) Uiso 1 1 d D . . C48 C -0.0635(6) 0.0295(13) 0.3394(6) 0.101(5) Uiso 1 1 d D . . H48A H -0.0360 -0.0011 0.3449 0.152 Uiso 1 1 calc R . . H48B H -0.0771 0.0155 0.3599 0.152 Uiso 1 1 calc R . . H48C H -0.0552 0.0836 0.3428 0.152 Uiso 1 1 calc R . . C49 C -0.1082(8) -0.0719(9) 0.2864(8) 0.101(5) Uiso 1 1 d D . . H49A H -0.0796 -0.0993 0.2921 0.152 Uiso 1 1 calc R . . H49B H -0.1296 -0.0818 0.2567 0.152 Uiso 1 1 calc R . . H49C H -0.1217 -0.0893 0.3066 0.152 Uiso 1 1 calc R . . C50 C -0.1434(6) 0.0578(13) 0.2850(7) 0.101(5) Uiso 1 1 d D . . H50A H -0.1653 0.0490 0.2553 0.152 Uiso 1 1 calc R . . H50B H -0.1372 0.1124 0.2896 0.152 Uiso 1 1 calc R . . H50C H -0.1563 0.0391 0.3054 0.152 Uiso 1 1 calc R . . C51 C -0.0595(4) -0.0726(9) 0.1725(4) 0.031(3) Uiso 1 1 d . . . C52 C -0.0669(4) -0.1572(7) 0.1591(3) 0.043(3) Uiso 1 1 d D . . C53 C -0.0205(4) -0.1988(12) 0.1725(5) 0.063(3) Uiso 1 1 d D . . H53A H -0.0043 -0.1966 0.2040 0.094 Uiso 1 1 calc R . . H53B H -0.0020 -0.1741 0.1587 0.094 Uiso 1 1 calc R . . H53C H -0.0258 -0.2521 0.1632 0.094 Uiso 1 1 calc R . . C54 C -0.0952(5) -0.1932(11) 0.1828(5) 0.063(3) Uiso 1 1 d D . . H54A H -0.0781 -0.1896 0.2142 0.094 Uiso 1 1 calc R . . H54B H -0.1012 -0.2468 0.1745 0.094 Uiso 1 1 calc R . . H54C H -0.1243 -0.1660 0.1749 0.094 Uiso 1 1 calc R . . C55 C -0.0938(5) -0.1640(11) 0.1096(3) 0.063(3) Uiso 1 1 d D . . H55A H -0.0760 -0.1409 0.0945 0.094 Uiso 1 1 calc R . . H55B H -0.1231 -0.1376 0.1013 0.094 Uiso 1 1 calc R . . H55C H -0.0992 -0.2179 0.1016 0.094 Uiso 1 1 calc R . . C56 C -0.1422(7) 0.1571(14) 0.0775(6) 0.060(5) Uiso 1 1 d . . . C57 C -0.1580(5) 0.1463(9) 0.0270(5) 0.083(6) Uiso 1 1 d D . . C58 C -0.1203(6) 0.1033(12) 0.0176(8) 0.094(4) Uiso 1 1 d D . . H58A H -0.1165 0.0523 0.0302 0.141 Uiso 1 1 calc R . . H58B H -0.0915 0.1314 0.0303 0.141 Uiso 1 1 calc R . . H58C H -0.1292 0.0992 -0.0138 0.141 Uiso 1 1 calc R . . C59 C -0.2033(6) 0.1006(12) 0.0081(8) 0.094(4) Uiso 1 1 d D . . H59A H -0.2270 0.1273 0.0144 0.141 Uiso 1 1 calc R . . H59B H -0.1986 0.0498 0.0211 0.141 Uiso 1 1 calc R . . H59C H -0.2128 0.0958 -0.0234 0.141 Uiso 1 1 calc R . . C60 C -0.1652(7) 0.2261(9) 0.0058(8) 0.094(4) Uiso 1 1 d D . . H60A H -0.1885 0.2537 0.0124 0.141 Uiso 1 1 calc R . . H60B H -0.1752 0.2207 -0.0256 0.141 Uiso 1 1 calc R . . H60C H -0.1364 0.2545 0.0172 0.141 Uiso 1 1 calc R . . C61 C -0.2123(5) 0.0659(10) 0.1304(5) 0.039(3) Uiso 1 1 d . A . C62 C -0.2527(4) 0.0087(8) 0.1220(4) 0.046(4) Uiso 1 1 d D . . C63 C -0.2784(10) 0.032(2) 0.1509(8) 0.069(4) Uiso 0.505(18) 1 d PD A 1 H63A H -0.3042 -0.0023 0.1457 0.103 Uiso 0.505(18) 1 calc PR A 1 H63B H -0.2897 0.0844 0.1439 0.103 Uiso 0.505(18) 1 calc PR A 1 H63C H -0.2575 0.0294 0.1814 0.103 Uiso 0.505(18) 1 calc PR A 1 C64 C -0.2344(12) -0.0735(12) 0.1332(10) 0.069(4) Uiso 0.505(18) 1 d PD A 1 H64A H -0.2601 -0.1087 0.1271 0.103 Uiso 0.505(18) 1 calc PR A 1 H64B H -0.2144 -0.0764 0.1640 0.103 Uiso 0.505(18) 1 calc PR A 1 H64C H -0.2171 -0.0875 0.1157 0.103 Uiso 0.505(18) 1 calc PR A 1 C65 C -0.2853(10) 0.013(2) 0.0738(5) 0.069(4) Uiso 0.505(18) 1 d PD A 1 H65A H -0.3107 -0.0223 0.0681 0.103 Uiso 0.505(18) 1 calc PR A 1 H65B H -0.2685 -0.0001 0.0556 0.103 Uiso 0.505(18) 1 calc PR A 1 H65C H -0.2973 0.0652 0.0670 0.103 Uiso 0.505(18) 1 calc PR A 1 C63A C -0.2994(8) 0.0501(18) 0.1011(9) 0.069(4) Uiso 0.495(18) 1 d PD A 2 H63D H -0.3005 0.0786 0.0757 0.103 Uiso 0.495(18) 1 calc PR A 2 H63E H -0.3032 0.0853 0.1222 0.103 Uiso 0.495(18) 1 calc PR A 2 H63F H -0.3242 0.0125 0.0924 0.103 Uiso 0.495(18) 1 calc PR A 2 C64A C -0.2493(12) -0.0527(16) 0.0901(8) 0.069(4) Uiso 0.495(18) 1 d PD A 2 H64D H -0.2497 -0.0279 0.0638 0.103 Uiso 0.495(18) 1 calc PR A 2 H64E H -0.2754 -0.0875 0.0825 0.103 Uiso 0.495(18) 1 calc PR A 2 H64F H -0.2208 -0.0813 0.1037 0.103 Uiso 0.495(18) 1 calc PR A 2 C65A C -0.2495(11) -0.0302(18) 0.1645(7) 0.069(4) Uiso 0.495(18) 1 d PD A 2 H65D H -0.2753 -0.0652 0.1583 0.103 Uiso 0.495(18) 1 calc PR A 2 H65E H -0.2504 0.0086 0.1851 0.103 Uiso 0.495(18) 1 calc PR A 2 H65F H -0.2208 -0.0587 0.1769 0.103 Uiso 0.495(18) 1 calc PR A 2 C66 C -0.2076(5) 0.3242(10) 0.1977(5) 0.044(3) Uiso 1 1 d . . . C67 C -0.2244(4) 0.3312(8) 0.2363(4) 0.056(4) Uiso 1 1 d D . . C68 C -0.2769(5) 0.3408(13) 0.2156(7) 0.098(4) Uiso 1 1 d D . . H68A H -0.2845 0.3877 0.1984 0.147 Uiso 1 1 calc R . . H68B H -0.2889 0.3437 0.2383 0.147 Uiso 1 1 calc R . . H68C H -0.2906 0.2972 0.1968 0.147 Uiso 1 1 calc R . . C69 C -0.2027(7) 0.4008(10) 0.2654(7) 0.098(4) Uiso 1 1 d D . . H69A H -0.1694 0.3950 0.2782 0.147 Uiso 1 1 calc R . . H69B H -0.2142 0.4042 0.2885 0.147 Uiso 1 1 calc R . . H69C H -0.2107 0.4473 0.2479 0.147 Uiso 1 1 calc R . . C70 C -0.2121(8) 0.2577(9) 0.2639(7) 0.098(4) Uiso 1 1 d D . . H70A H -0.1789 0.2503 0.2755 0.147 Uiso 1 1 calc R . . H70B H -0.2271 0.2140 0.2457 0.147 Uiso 1 1 calc R . . H70C H -0.2224 0.2621 0.2877 0.147 Uiso 1 1 calc R . . C71 C -0.2533(7) 0.3398(13) 0.0773(6) 0.062(5) Uiso 1 1 d . . . C72 C -0.3023(8) 0.3428(16) 0.0420(8) 0.128(11) Uiso 1 1 d D . . C73 C -0.3281(14) 0.2661(16) 0.0306(13) 0.178(10) Uiso 1 1 d D . . H73A H -0.3587 0.2743 0.0082 0.267 Uiso 1 1 calc R . . H73B H -0.3309 0.2449 0.0566 0.267 Uiso 1 1 calc R . . H73C H -0.3112 0.2304 0.0200 0.267 Uiso 1 1 calc R . . C74 C -0.3314(14) 0.4021(19) 0.0540(12) 0.178(10) Uiso 1 1 d D . . H74A H -0.3618 0.4054 0.0307 0.267 Uiso 1 1 calc R . . H74B H -0.3164 0.4520 0.0582 0.267 Uiso 1 1 calc R . . H74C H -0.3344 0.3866 0.0809 0.267 Uiso 1 1 calc R . . C75 C -0.2927(14) 0.372(2) 0.0028(12) 0.178(10) Uiso 1 1 d D . . H75A H -0.3217 0.3787 -0.0220 0.267 Uiso 1 1 calc R . . H75B H -0.2740 0.3343 -0.0045 0.267 Uiso 1 1 calc R . . H75C H -0.2764 0.4203 0.0101 0.267 Uiso 1 1 calc R . . C76 C -0.1087(5) 0.5073(10) 0.1077(5) 0.037(3) Uiso 1 1 d . . . C77 C -0.1023(5) 0.5275(8) 0.0664(4) 0.054(4) Uiso 1 1 d D . . C78 C -0.1238(7) 0.4692(11) 0.0294(7) 0.100(5) Uiso 1 1 d D . . H78A H -0.1181 0.4853 0.0040 0.149 Uiso 1 1 calc R . . H78B H -0.1568 0.4664 0.0218 0.149 Uiso 1 1 calc R . . H78C H -0.1101 0.4190 0.0389 0.149 Uiso 1 1 calc R . . C79 C -0.1259(7) 0.6058(10) 0.0523(8) 0.100(5) Uiso 1 1 d D . . H79A H -0.1227 0.6224 0.0257 0.149 Uiso 1 1 calc R . . H79B H -0.1115 0.6432 0.0752 0.149 Uiso 1 1 calc R . . H79C H -0.1584 0.6013 0.0469 0.149 Uiso 1 1 calc R . . C80 C -0.0506(4) 0.5350(13) 0.0770(8) 0.100(5) Uiso 1 1 d D . . H80A H -0.0459 0.5479 0.0507 0.149 Uiso 1 1 calc R . . H80B H -0.0354 0.4866 0.0886 0.149 Uiso 1 1 calc R . . H80C H -0.0377 0.5752 0.0986 0.149 Uiso 1 1 calc R . . C81 C -0.1903(5) 0.5907(10) 0.1486(5) 0.035(3) Uiso 1 1 d . . . C82 C -0.2242(3) 0.6598(6) 0.1404(3) 0.032(3) Uiso 1 1 d D . . C83 C -0.2735(4) 0.6292(9) 0.1260(4) 0.048(2) Uiso 1 1 d D . . H83A H -0.2948 0.6721 0.1200 0.072 Uiso 1 1 calc R . . H83B H -0.2760 0.5979 0.1492 0.072 Uiso 1 1 calc R . . H83C H -0.2810 0.5984 0.0998 0.072 Uiso 1 1 calc R . . C84 C -0.2193(5) 0.7056(9) 0.1029(4) 0.048(2) Uiso 1 1 d D . . H84A H -0.2400 0.7495 0.0959 0.072 Uiso 1 1 calc R . . H84B H -0.2272 0.6729 0.0773 0.072 Uiso 1 1 calc R . . H84C H -0.1878 0.7235 0.1117 0.072 Uiso 1 1 calc R . . C85 C -0.2129(5) 0.7121(8) 0.1803(3) 0.048(2) Uiso 1 1 d D . . H85A H -0.2347 0.7544 0.1731 0.072 Uiso 1 1 calc R . . H85B H -0.1818 0.7322 0.1888 0.072 Uiso 1 1 calc R . . H85C H -0.2149 0.6828 0.2043 0.072 Uiso 1 1 calc R . . C86 C -0.0741(4) 0.5922(9) 0.2910(4) 0.033(3) Uiso 1 1 d . . . C87 C -0.0921(4) 0.6164(8) 0.3254(4) 0.057(4) Uiso 1 1 d D . . C88 C -0.1388(5) 0.5812(11) 0.3193(6) 0.082(4) Uiso 1 1 d D . . H88A H -0.1478 0.5986 0.3426 0.123 Uiso 1 1 calc R . . H88B H -0.1364 0.5256 0.3200 0.123 Uiso 1 1 calc R . . H88C H -0.1619 0.5973 0.2913 0.123 Uiso 1 1 calc R . . C89 C -0.0960(6) 0.7043(8) 0.3230(7) 0.082(4) Uiso 1 1 d D . . H89A H -0.1067 0.7227 0.3450 0.123 Uiso 1 1 calc R . . H89B H -0.1178 0.7194 0.2942 0.123 Uiso 1 1 calc R . . H89C H -0.0660 0.7264 0.3282 0.123 Uiso 1 1 calc R . . C90 C -0.0557(5) 0.5924(11) 0.3698(5) 0.082(4) Uiso 1 1 d D . . H90A H -0.0657 0.6076 0.3928 0.123 Uiso 1 1 calc R . . H90B H -0.0266 0.6175 0.3743 0.123 Uiso 1 1 calc R . . H90C H -0.0516 0.5371 0.3704 0.123 Uiso 1 1 calc R . . C100 C -0.0069(9) 0.2785(15) 0.1864(8) 0.082(6) Uiso 1 1 d . . . H100 H -0.0293 0.2370 0.1839 0.099 Uiso 1 1 calc R . . C101 C -0.0322(6) 0.3460(11) 0.1600(5) 0.054(4) Uiso 1 1 d . . . H10D H -0.0515 0.3708 0.1734 0.065 Uiso 1 1 calc R . . H10E H -0.0108 0.3840 0.1567 0.065 Uiso 1 1 calc R . . C102 C -0.0606(8) 0.3103(15) 0.1178(7) 0.082(6) Uiso 1 1 d . . . H10F H -0.0834 0.3481 0.1002 0.099 Uiso 1 1 calc R . . H10G H -0.0776 0.2671 0.1233 0.099 Uiso 1 1 calc R . . C103 C -0.0335(9) 0.2805(17) 0.0904(9) 0.096(7) Uiso 1 1 d . . . H10H H -0.0156 0.3217 0.0844 0.115 Uiso 1 1 calc R . . H10I H -0.0543 0.2578 0.0628 0.115 Uiso 1 1 calc R . . C104 C -0.0010(8) 0.2176(15) 0.1221(8) 0.084(6) Uiso 1 1 d . . . H10J H -0.0205 0.1767 0.1261 0.100 Uiso 1 1 calc R . . H10K H 0.0179 0.1947 0.1077 0.100 Uiso 1 1 calc R . . C105 C 0.0314(9) 0.2464(17) 0.1676(8) 0.090(7) Uiso 1 1 d . . . H10L H 0.0517 0.2877 0.1655 0.109 Uiso 1 1 calc R . . H10M H 0.0502 0.2047 0.1856 0.109 Uiso 1 1 calc R . . C106 C -0.0029(4) 0.3243(9) 0.2606(4) 0.033(3) Uiso 1 1 d . . . H106 H -0.0120 0.3776 0.2505 0.040 Uiso 1 1 calc R . . C107 C 0.0286(8) 0.3281(15) 0.3098(7) 0.075(5) Uiso 1 1 d . . . H10N H 0.0538 0.3646 0.3144 0.090 Uiso 1 1 calc R . . H10O H 0.0422 0.2774 0.3199 0.090 Uiso 1 1 calc R . . C108 C -0.0019(12) 0.356(2) 0.3380(12) 0.133(12) Uiso 1 1 d . . . H10P H 0.0159 0.3448 0.3690 0.160 Uiso 1 1 calc R . . H10Q H -0.0065 0.4114 0.3349 0.160 Uiso 1 1 calc R . . C109 C -0.0468(14) 0.319(3) 0.3249(13) 0.149(14) Uiso 1 1 d . . . H10R H -0.0423 0.2658 0.3360 0.179 Uiso 1 1 calc R . . H10S H -0.0650 0.3459 0.3386 0.179 Uiso 1 1 calc R . . C110 C -0.0725(9) 0.3167(18) 0.2788(9) 0.094(7) Uiso 1 1 d . . . H11A H -0.0810 0.3695 0.2684 0.113 Uiso 1 1 calc R . . H11B H -0.1011 0.2880 0.2728 0.113 Uiso 1 1 calc R . . C111 C -0.0463(7) 0.2799(13) 0.2529(7) 0.069(5) Uiso 1 1 d . . . H11C H -0.0386 0.2265 0.2622 0.083 Uiso 1 1 calc R . . H11D H -0.0660 0.2800 0.2216 0.083 Uiso 1 1 calc R . . C112 C 0.0726(10) 0.3317(18) 0.2458(9) 0.099(8) Uiso 1 1 d . . . H11E H 0.0872 0.3381 0.2776 0.119 Uiso 1 1 calc R . . H11F H 0.0924 0.2984 0.2368 0.119 Uiso 1 1 calc R . . C113 C 0.0686(8) 0.3983(14) 0.2270(8) 0.079(6) Uiso 1 1 d . . . H11G H 0.0990 0.4180 0.2317 0.118 Uiso 1 1 calc R . . H11H H 0.0531 0.4337 0.2394 0.118 Uiso 1 1 calc R . . H11I H 0.0506 0.3929 0.1959 0.118 Uiso 1 1 calc R . . O115 O -0.0400(14) 0.300(3) 0.4468(15) 0.253(18) Uiso 1 1 d D . . C116 C -0.0625(15) 0.384(3) 0.4385(16) 0.19(2) Uiso 1 1 d D . . H116 H -0.0486 0.4325 0.4483 0.231 Uiso 1 1 calc R . . C117 C -0.1156(16) 0.364(2) 0.4088(14) 0.172(17) Uiso 1 1 d D . . H117 H -0.1412 0.3969 0.3973 0.206 Uiso 1 1 calc R . . C114 C -0.0683(15) 0.221(3) 0.4316(16) 0.21(2) Uiso 1 1 d D . . H114 H -0.0618 0.1678 0.4365 0.255 Uiso 1 1 calc R . . C115 C -0.1127(15) 0.272(2) 0.4044(13) 0.147(14) Uiso 1 1 d D . . H115 H -0.1388 0.2469 0.3844 0.177 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0168(8) 0.0134(9) 0.0293(9) 0.0035(8) 0.0020(7) 0.0011(7) Cr2 0.0204(9) 0.0206(11) 0.0393(11) 0.0050(9) 0.0006(8) -0.0001(8) Cr3 0.0247(10) 0.0173(11) 0.0522(14) 0.0022(10) -0.0098(9) 0.0024(8) Cr4 0.0307(11) 0.0159(11) 0.0391(12) 0.0017(9) -0.0066(9) 0.0036(9) Cr5 0.0152(7) 0.0117(9) 0.0242(8) 0.0017(7) 0.0027(6) 0.0033(7) Ni6 0.0258(7) 0.0205(9) 0.0391(9) -0.0001(7) 0.0056(6) -0.0006(7) Cr7 0.0233(9) 0.0115(9) 0.0324(10) 0.0002(8) 0.0028(7) 0.0022(7) Cr8 0.0242(10) 0.0119(11) 0.0602(15) -0.0028(10) -0.0107(9) 0.0016(8) Cr9 0.0278(10) 0.0129(11) 0.0381(12) -0.0010(9) -0.0072(8) 0.0009(8) Cr10 0.0167(8) 0.0128(9) 0.0268(9) 0.0000(8) 0.0032(7) 0.0012(7) F1 0.027(3) 0.019(4) 0.031(4) 0.002(3) 0.003(3) 0.000(3) F2 0.030(4) 0.020(4) 0.037(4) 0.001(3) 0.017(3) -0.001(3) F3 0.022(3) 0.023(4) 0.030(4) 0.002(3) -0.003(3) -0.001(3) F4 0.026(3) 0.009(3) 0.041(4) -0.002(3) 0.007(3) -0.001(3) F5 0.022(3) 0.018(4) 0.033(4) 0.002(3) 0.006(3) -0.001(3) F6 0.033(4) 0.026(4) 0.039(4) 0.009(4) 0.011(3) 0.008(3) F7 0.015(3) 0.018(4) 0.045(4) 0.003(3) 0.005(3) 0.002(3) F8 0.015(3) 0.015(3) 0.031(4) 0.003(3) -0.001(3) -0.001(3) F9 0.032(4) 0.008(3) 0.033(4) -0.002(3) 0.001(3) 0.001(3) F10 0.017(3) 0.027(4) 0.025(3) 0.002(3) 0.002(3) 0.002(3) F11 0.018(3) 0.009(3) 0.049(4) 0.000(3) 0.008(3) 0.001(2) F12 0.023(3) 0.013(4) 0.038(4) 0.004(3) 0.009(3) 0.004(3) O1 0.025(4) 0.037(6) 0.028(4) -0.005(4) 0.007(3) -0.007(4) O2 0.028(4) 0.027(5) 0.050(5) 0.015(4) 0.016(4) 0.002(4) O3 0.029(4) 0.007(4) 0.057(6) 0.002(4) -0.003(4) -0.004(3) O4 0.028(5) 0.022(5) 0.055(6) 0.001(5) -0.008(4) 0.010(4) O5 0.047(6) 0.037(6) 0.033(5) -0.006(5) 0.004(4) 0.006(5) O6 0.124(11) 0.013(5) 0.033(5) 0.001(4) 0.007(6) 0.025(6) O7 0.035(5) 0.023(6) 0.056(6) 0.002(5) 0.002(5) -0.007(4) O8 0.015(4) 0.026(6) 0.134(12) 0.012(7) -0.009(6) 0.002(4) O9 0.067(8) 0.034(7) 0.147(14) 0.026(8) 0.073(9) 0.014(6) O10 0.030(5) 0.026(5) 0.063(7) -0.006(5) 0.014(5) -0.002(4) O11 0.076(9) 0.016(6) 0.114(12) -0.002(7) -0.067(9) -0.007(6) O12 0.062(7) 0.026(6) 0.049(7) -0.006(5) -0.027(5) 0.007(5) O13 0.061(7) 0.021(5) 0.039(6) -0.002(5) 0.006(5) -0.018(5) O14 0.033(5) 0.041(7) 0.033(5) 0.002(5) 0.007(4) -0.012(5) O17 0.033(4) 0.026(5) 0.044(5) -0.007(4) 0.014(4) -0.006(4) O18 0.029(4) 0.027(5) 0.035(5) -0.007(4) 0.004(4) -0.004(4) O19 0.035(5) 0.029(5) 0.031(4) 0.012(4) 0.005(4) 0.000(4) O20 0.019(4) 0.037(6) 0.046(5) 0.012(5) 0.009(4) 0.005(4) O21 0.023(4) 0.028(6) 0.049(6) 0.000(5) -0.007(4) 0.002(4) O22 0.037(5) 0.020(5) 0.043(5) -0.013(4) 0.009(4) 0.001(4) O23 0.046(6) 0.037(6) 0.032(5) 0.002(4) 0.006(4) -0.003(5) O24 0.067(7) 0.045(8) 0.033(5) -0.005(5) -0.009(5) 0.002(6) O25 0.024(4) 0.021(5) 0.054(6) 0.000(5) -0.009(4) 0.010(4) O26 0.039(6) 0.025(6) 0.113(11) -0.003(7) -0.006(6) -0.001(5) O27 0.041(6) 0.018(5) 0.105(9) -0.005(5) 0.040(6) -0.005(4) O28 0.025(5) 0.022(5) 0.075(7) -0.015(5) 0.010(5) -0.006(4) O29 0.037(6) 0.019(6) 0.124(12) -0.002(7) -0.034(7) 0.004(5) O30 0.056(7) 0.011(5) 0.066(7) 0.005(5) -0.033(6) -0.004(5) O31 0.056(6) 0.036(6) 0.023(5) 0.010(5) -0.006(4) 0.002(5) O32 0.036(5) 0.044(7) 0.022(4) -0.003(4) 0.006(4) 0.004(5) O33 0.024(4) 0.011(4) 0.060(6) -0.004(4) -0.021(4) 0.000(3) O34 0.016(3) 0.002(3) 0.051(5) -0.003(3) -0.007(3) 0.002(3) O35 0.023(4) 0.029(5) 0.039(5) -0.004(4) 0.012(4) 0.000(4) O36 0.027(4) 0.032(5) 0.029(4) -0.004(4) 0.002(3) 0.003(4) N1 0.147(17) 0.030(7) 0.079(11) 0.021(7) 0.065(12) 0.032(9) _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 Cr1 F1 1.912(7) . ? Cr1 F11 1.914(8) . ? Cr1 F12 1.944(7) . ? Cr1 O36 1.955(9) . ? Cr1 O3 1.955(9) . ? Cr1 O1 1.967(8) . ? Cr1 Cr10 2.965(3) . ? Cr2 F1 1.889(7) . ? Cr2 F2 1.902(8) . ? Cr2 O4 1.927(11) . ? Cr2 O7 1.938(10) . ? Cr2 O5 1.947(11) . ? Cr2 O2 1.966(9) . ? Cr3 F3 1.901(8) . ? Cr3 O9 1.901(15) . ? Cr3 F2 1.926(8) . ? Cr3 O11 1.942(12) . ? Cr3 O6 1.947(14) . ? Cr3 O8 1.950(12) . ? Cr4 F4 1.890(8) . ? Cr4 O15 1.909(12) . ? Cr4 O13 1.921(11) . ? Cr4 F3 1.934(9) . ? Cr4 O12 1.945(11) . ? Cr4 O10 1.965(11) . ? Cr5 F6 1.917(9) . ? Cr5 O17 1.954(9) . ? Cr5 O16 1.961(11) . ? Cr5 F5 1.966(7) . ? Cr5 F4 1.969(7) . ? Cr5 O14 1.971(10) . ? Cr5 Ni6 2.984(2) . ? Ni6 F7 1.958(7) . ? Ni6 O21 1.959(11) . ? Ni6 O19 1.968(9) . ? Ni6 F6 1.976(8) . ? Ni6 O18 1.978(9) . ? Ni6 F5 2.056(8) . ? Cr7 F7 1.898(7) . ? Cr7 O22 1.928(10) . ? Cr7 O20 1.930(10) . ? Cr7 F8 1.965(8) . ? Cr7 O23 1.975(10) . ? Cr7 O25 1.978(10) . ? Cr8 F8 1.860(7) . ? Cr8 O24 1.920(13) . ? Cr8 O26 1.944(13) . ? Cr8 F9 1.959(8) . ? Cr8 O29 1.966(11) . ? Cr8 O27 1.981(13) . ? Cr9 F9 1.914(8) . ? Cr9 F10 1.918(7) . ? Cr9 O28 1.936(12) . ? Cr9 O30 1.950(10) . ? Cr9 O31 1.975(12) . ? Cr9 O33 1.996(10) . ? Cr10 F10 1.898(8) . ? Cr10 F12 1.944(8) . ? Cr10 F11 1.945(7) . ? Cr10 O34 1.962(8) . ? Cr10 O32 1.962(9) . ? Cr10 O35 1.992(9) . ? O1 C1 1.269(15) . ? O2 C1 1.272(16) . ? O3 C6 1.236(18) . ? O4 C6 1.256(18) . ? O5 C11 1.23(2) . ? O6 C11 1.28(2) . ? O7 C16 1.242(19) . ? O8 C16 1.23(2) . ? O9 C21 1.29(2) . ? O10 C21 1.20(2) . ? O11 C26 1.24(2) . ? O12 C26 1.255(19) . ? O13 C31 1.268(18) . ? O14 C31 1.251(18) . ? O15 C36 1.32(2) . ? O16 C36 1.203(19) . ? O17 C41 1.277(17) . ? O18 C41 1.242(16) . ? O19 C46 1.290(15) . ? O20 C46 1.254(16) . ? O21 C51 1.267(16) . ? O22 C51 1.270(17) . ? O23 C56 1.25(2) . ? O24 C56 1.24(2) . ? O25 C61 1.219(18) . ? O26 C61 1.24(2) . ? O27 C66 1.23(2) . ? O28 C66 1.29(2) . ? O29 C71 1.25(2) . ? O30 C71 1.26(2) . ? O31 C76 1.269(19) . ? O32 C76 1.250(18) . ? O33 C81 1.197(19) . ? O34 C81 1.283(16) . ? O35 C86 1.266(16) . ? O36 C86 1.262(15) . ? N1 C100 1.44(3) . ? N1 C106 1.52(2) . ? N1 C112 1.64(3) . ? N1 H1 0.9100 . ? C1 C2 1.504(18) . ? C2 C5 1.517(6) . ? C2 C3 1.518(6) . ? C2 C4 1.520(6) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.52(2) . ? C7 C10 1.515(6) . ? C7 C9 1.517(6) . ? C7 C8 1.518(6) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.55(2) . ? C12 C14 1.515(6) . ? C12 C13 1.516(6) . ? C12 C15 1.516(6) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.516(19) . ? C17 C20 1.513(6) . ? C17 C18 1.518(6) . ? C17 C19 1.520(6) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.49(3) . ? C22 C24 1.518(6) . ? C22 C25 1.519(6) . ? C22 C23 1.520(6) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.492(18) . ? C27 C28 1.517(6) . ? C27 C29 1.517(6) . ? C27 C30 1.520(6) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.553(19) . ? C32 C35 1.518(6) . ? C32 C34 1.520(6) . ? C32 C33 1.520(6) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.55(2) . ? C37 C40 1.519(6) . ? C37 C38 1.519(6) . ? C37 C39 1.521(6) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.565(19) . ? C42 C45 1.518(6) . ? C42 C43 1.519(6) . ? C42 C44 1.520(6) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 C47 1.517(18) . ? C47 C50 1.516(6) . ? C47 C48 1.519(6) . ? C47 C49 1.522(6) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 C52 1.513(18) . ? C52 C55 1.517(6) . ? C52 C53 1.517(6) . ? C52 C54 1.519(6) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 C57 1.55(2) . ? C57 C58 1.517(6) . ? C57 C60 1.517(6) . ? C57 C59 1.520(6) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 C62 1.54(2) . ? C62 C65 1.514(6) . ? C62 C63 1.516(6) . ? C62 C65A 1.517(6) . ? C62 C64 1.517(6) . ? C62 C64A 1.521(6) . ? C62 C63A 1.522(6) . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C63A H63D 0.9600 . ? C63A H63E 0.9600 . ? C63A H63F 0.9600 . ? C64A H64D 0.9600 . ? C64A H64E 0.9600 . ? C64A H64F 0.9600 . ? C65A H65D 0.9600 . ? C65A H65E 0.9600 . ? C65A H65F 0.9600 . ? C66 C67 1.556(19) . ? C67 C68 1.515(6) . ? C67 C70 1.515(6) . ? C67 C69 1.518(6) . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 C72 1.51(3) . ? C72 C75 1.516(6) . ? C72 C74 1.516(6) . ? C72 C73 1.517(6) . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C76 C77 1.487(19) . ? C77 C80 1.514(6) . ? C77 C78 1.517(6) . ? C77 C79 1.518(6) . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? C80 H80A 0.9600 . ? C80 H80B 0.9600 . ? C80 H80C 0.9600 . ? C81 C82 1.541(18) . ? C82 C83 1.515(6) . ? C82 C85 1.515(6) . ? C82 C84 1.521(6) . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C84 H84A 0.9600 . ? C84 H84B 0.9600 . ? C84 H84C 0.9600 . ? C85 H85A 0.9600 . ? C85 H85B 0.9600 . ? C85 H85C 0.9600 . ? C86 C87 1.503(17) . ? C87 C88 1.515(6) . ? C87 C90 1.516(6) . ? C87 C89 1.518(6) . ? C88 H88A 0.9600 . ? C88 H88B 0.9600 . ? C88 H88C 0.9600 . ? C89 H89A 0.9600 . ? C89 H89B 0.9600 . ? C89 H89C 0.9600 . ? C90 H90A 0.9600 . ? C90 H90B 0.9600 . ? C90 H90C 0.9600 . ? C100 C101 1.48(3) . ? C100 C105 1.64(3) . ? C100 H100 0.9800 . ? C101 C102 1.46(3) . ? C101 H10D 0.9700 . ? C101 H10E 0.9700 . ? C102 C103 1.54(3) . ? C102 H10F 0.9700 . ? C102 H10G 0.9700 . ? C103 C104 1.57(3) . ? C103 H10H 0.9700 . ? C103 H10I 0.9700 . ? C104 C105 1.52(3) . ? C104 H10J 0.9700 . ? C104 H10K 0.9700 . ? C105 H10L 0.9700 . ? C105 H10M 0.9700 . ? C106 C111 1.49(2) . ? C106 C107 1.53(2) . ? C106 H106 0.9800 . ? C107 C108 1.64(4) . ? C107 H10N 0.9700 . ? C107 H10O 0.9700 . ? C108 C109 1.44(5) . ? C108 H10P 0.9700 . ? C108 H10Q 0.9700 . ? C109 C110 1.41(4) . ? C109 H10R 0.9700 . ? C109 H10S 0.9700 . ? C110 C111 1.53(3) . ? C110 H11A 0.9700 . ? C110 H11B 0.9700 . ? C111 H11C 0.9700 . ? C111 H11D 0.9700 . ? C112 C113 1.29(4) . ? C112 H11E 0.9700 . ? C112 H11F 0.9700 . ? C113 H11G 0.9600 . ? C113 H11H 0.9600 . ? C113 H11I 0.9600 . ? O115 C114 1.59(2) . ? O115 C116 1.59(2) . ? C116 C117 1.60(2) . ? C116 H116 0.9300 . ? C117 C115 1.59(2) . ? C117 H117 0.9300 . ? C114 C115 1.59(2) . ? C114 H114 0.9300 . ? C115 H115 0.9300 . ? 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 Cr1 F11 91.9(3) . . ? F1 Cr1 F12 170.0(3) . . ? F11 Cr1 F12 78.4(3) . . ? F1 Cr1 O36 88.7(4) . . ? F11 Cr1 O36 89.7(4) . . ? F12 Cr1 O36 88.7(3) . . ? F1 Cr1 O3 95.5(4) . . ? F11 Cr1 O3 171.7(3) . . ? F12 Cr1 O3 94.0(4) . . ? O36 Cr1 O3 87.0(5) . . ? F1 Cr1 O1 91.7(4) . . ? F11 Cr1 O1 93.8(4) . . ? F12 Cr1 O1 91.5(4) . . ? O36 Cr1 O1 176.4(5) . . ? O3 Cr1 O1 89.5(5) . . ? F1 Cr1 Cr10 129.7(2) . . ? F11 Cr1 Cr10 40.2(2) . . ? F12 Cr1 Cr10 40.3(2) . . ? O36 Cr1 Cr10 79.0(3) . . ? O3 Cr1 Cr10 131.6(3) . . ? O1 Cr1 Cr10 103.4(3) . . ? F1 Cr2 F2 90.7(3) . . ? F1 Cr2 O4 90.5(4) . . ? F2 Cr2 O4 178.2(4) . . ? F1 Cr2 O7 175.7(4) . . ? F2 Cr2 O7 92.9(4) . . ? O4 Cr2 O7 86.0(5) . . ? F1 Cr2 O5 89.3(4) . . ? F2 Cr2 O5 91.4(4) . . ? O4 Cr2 O5 87.3(5) . . ? O7 Cr2 O5 93.0(5) . . ? F1 Cr2 O2 90.6(4) . . ? F2 Cr2 O2 90.5(4) . . ? O4 Cr2 O2 90.8(5) . . ? O7 Cr2 O2 87.0(4) . . ? O5 Cr2 O2 178.1(5) . . ? F3 Cr3 O9 91.1(5) . . ? F3 Cr3 F2 91.6(3) . . ? O9 Cr3 F2 89.5(5) . . ? F3 Cr3 O11 92.5(5) . . ? O9 Cr3 O11 93.4(8) . . ? F2 Cr3 O11 175.0(5) . . ? F3 Cr3 O6 88.8(5) . . ? O9 Cr3 O6 179.4(6) . . ? F2 Cr3 O6 91.1(4) . . ? O11 Cr3 O6 86.0(8) . . ? F3 Cr3 O8 176.9(5) . . ? O9 Cr3 O8 86.2(7) . . ? F2 Cr3 O8 90.0(4) . . ? O11 Cr3 O8 86.2(5) . . ? O6 Cr3 O8 93.9(7) . . ? F4 Cr4 O15 93.8(4) . . ? F4 Cr4 O13 92.8(4) . . ? O15 Cr4 O13 92.4(5) . . ? F4 Cr4 F3 90.4(3) . . ? O15 Cr4 F3 174.6(4) . . ? O13 Cr4 F3 90.9(4) . . ? F4 Cr4 O12 179.3(5) . . ? O15 Cr4 O12 85.6(5) . . ? O13 Cr4 O12 86.8(6) . . ? F3 Cr4 O12 90.3(4) . . ? F4 Cr4 O10 89.3(4) . . ? O15 Cr4 O10 87.2(5) . . ? O13 Cr4 O10 177.8(5) . . ? F3 Cr4 O10 89.4(4) . . ? O12 Cr4 O10 91.0(6) . . ? F6 Cr5 O17 90.4(4) . . ? F6 Cr5 O16 94.7(4) . . ? O17 Cr5 O16 88.6(4) . . ? F6 Cr5 F5 81.6(3) . . ? O17 Cr5 F5 90.7(4) . . ? O16 Cr5 F5 176.2(4) . . ? F6 Cr5 F4 171.6(3) . . ? O17 Cr5 F4 89.2(4) . . ? O16 Cr5 F4 93.7(4) . . ? F5 Cr5 F4 90.1(3) . . ? F6 Cr5 O14 90.7(4) . . ? O17 Cr5 O14 178.1(4) . . ? O16 Cr5 O14 89.7(4) . . ? F5 Cr5 O14 91.0(4) . . ? F4 Cr5 O14 90.0(4) . . ? F6 Cr5 Ni6 40.7(2) . . ? O17 Cr5 Ni6 79.8(3) . . ? O16 Cr5 Ni6 132.9(4) . . ? F5 Cr5 Ni6 43.3(2) . . ? F4 Cr5 Ni6 131.1(2) . . ? O14 Cr5 Ni6 102.1(3) . . ? F7 Ni6 O21 95.7(4) . . ? F7 Ni6 O19 89.8(3) . . ? O21 Ni6 O19 91.7(5) . . ? F7 Ni6 F6 167.5(4) . . ? O21 Ni6 F6 96.7(4) . . ? O19 Ni6 F6 91.0(4) . . ? F7 Ni6 O18 90.4(4) . . ? O21 Ni6 O18 87.6(5) . . ? O19 Ni6 O18 179.2(5) . . ? F6 Ni6 O18 89.0(4) . . ? F7 Ni6 F5 89.5(3) . . ? O21 Ni6 F5 174.1(4) . . ? O19 Ni6 F5 91.0(4) . . ? F6 Ni6 F5 78.0(3) . . ? O18 Ni6 F5 89.8(4) . . ? F7 Ni6 Cr5 128.5(2) . . ? O21 Ni6 Cr5 133.2(3) . . ? O19 Ni6 Cr5 101.5(3) . . ? F6 Ni6 Cr5 39.2(3) . . ? O18 Ni6 Cr5 78.9(3) . . ? F5 Ni6 Cr5 41.0(2) . . ? F7 Cr7 O22 92.8(4) . . ? F7 Cr7 O20 92.5(4) . . ? O22 Cr7 O20 92.9(5) . . ? F7 Cr7 F8 88.7(3) . . ? O22 Cr7 F8 177.1(4) . . ? O20 Cr7 F8 89.5(4) . . ? F7 Cr7 O23 91.1(4) . . ? O22 Cr7 O23 89.1(5) . . ? O20 Cr7 O23 175.7(4) . . ? F8 Cr7 O23 88.4(4) . . ? F7 Cr7 O25 178.4(4) . . ? O22 Cr7 O25 87.5(4) . . ? O20 Cr7 O25 85.9(4) . . ? F8 Cr7 O25 91.1(4) . . ? O23 Cr7 O25 90.4(5) . . ? F8 Cr8 O24 91.7(4) . . ? F8 Cr8 O26 92.2(4) . . ? O24 Cr8 O26 93.1(7) . . ? F8 Cr8 F9 89.8(3) . . ? O24 Cr8 F9 91.0(5) . . ? O26 Cr8 F9 175.4(6) . . ? F8 Cr8 O29 177.9(5) . . ? O24 Cr8 O29 87.2(7) . . ? O26 Cr8 O29 86.1(5) . . ? F9 Cr8 O29 92.1(5) . . ? F8 Cr8 O27 90.9(4) . . ? O24 Cr8 O27 177.3(5) . . ? O26 Cr8 O27 86.3(6) . . ? F9 Cr8 O27 89.5(4) . . ? O29 Cr8 O27 90.2(7) . . ? F9 Cr9 F10 89.6(3) . . ? F9 Cr9 O28 92.2(4) . . ? F10 Cr9 O28 89.3(4) . . ? F9 Cr9 O30 92.1(4) . . ? F10 Cr9 O30 176.9(5) . . ? O28 Cr9 O30 93.3(6) . . ? F9 Cr9 O31 90.7(4) . . ? F10 Cr9 O31 90.3(4) . . ? O28 Cr9 O31 177.1(5) . . ? O30 Cr9 O31 87.1(6) . . ? F9 Cr9 O33 177.8(5) . . ? F10 Cr9 O33 90.4(3) . . ? O28 Cr9 O33 85.6(5) . . ? O30 Cr9 O33 88.0(4) . . ? O31 Cr9 O33 91.5(5) . . ? F10 Cr10 F12 170.8(3) . . ? F10 Cr10 F11 93.3(3) . . ? F12 Cr10 F11 77.7(3) . . ? F10 Cr10 O34 95.4(3) . . ? F12 Cr10 O34 93.6(3) . . ? F11 Cr10 O34 170.9(3) . . ? F10 Cr10 O32 91.0(4) . . ? F12 Cr10 O32 91.5(4) . . ? F11 Cr10 O32 92.9(4) . . ? O34 Cr10 O32 89.5(4) . . ? F10 Cr10 O35 89.6(4) . . ? F12 Cr10 O35 88.4(4) . . ? F11 Cr10 O35 90.6(3) . . ? O34 Cr10 O35 86.9(4) . . ? O32 Cr10 O35 176.4(4) . . ? F10 Cr10 Cr1 130.5(2) . . ? F12 Cr10 Cr1 40.3(2) . . ? F11 Cr10 Cr1 39.4(2) . . ? O34 Cr10 Cr1 131.5(2) . . ? O32 Cr10 Cr1 102.6(3) . . ? O35 Cr10 Cr1 79.6(3) . . ? Cr2 F1 Cr1 123.4(4) . . ? Cr2 F2 Cr3 124.2(4) . . ? Cr3 F3 Cr4 124.4(4) . . ? Cr4 F4 Cr5 122.5(4) . . ? Cr5 F5 Ni6 95.8(3) . . ? Cr5 F6 Ni6 100.1(4) . . ? Cr7 F7 Ni6 120.4(4) . . ? Cr8 F8 Cr7 124.0(4) . . ? Cr9 F9 Cr8 121.7(4) . . ? Cr10 F10 Cr9 123.9(4) . . ? Cr1 F11 Cr10 100.4(3) . . ? Cr1 F12 Cr10 99.4(3) . . ? C1 O1 Cr1 127.6(8) . . ? C1 O2 Cr2 136.6(9) . . ? C6 O3 Cr1 132.2(10) . . ? C6 O4 Cr2 132.7(10) . . ? C11 O5 Cr2 133.2(11) . . ? C11 O6 Cr3 134.2(11) . . ? C16 O7 Cr2 133.2(11) . . ? C16 O8 Cr3 134.8(10) . . ? C21 O9 Cr3 130.1(12) . . ? C21 O10 Cr4 136.4(11) . . ? C26 O11 Cr3 134.5(11) . . ? C26 O12 Cr4 133.5(11) . . ? C31 O13 Cr4 135.0(10) . . ? C31 O14 Cr5 130.7(9) . . ? C36 O15 Cr4 130.1(10) . . ? C36 O16 Cr5 132.5(13) . . ? C41 O17 Cr5 126.0(8) . . ? C41 O18 Ni6 126.8(9) . . ? C46 O19 Ni6 127.4(8) . . ? C46 O20 Cr7 136.0(9) . . ? C51 O21 Ni6 131.7(10) . . ? C51 O22 Cr7 130.0(9) . . ? C56 O23 Cr7 130.4(12) . . ? C56 O24 Cr8 136.1(12) . . ? C61 O25 Cr7 136.5(11) . . ? C61 O26 Cr8 130.2(12) . . ? C66 O27 Cr8 131.5(12) . . ? C66 O28 Cr9 136.1(10) . . ? C71 O29 Cr8 136.9(13) . . ? C71 O30 Cr9 127.3(12) . . ? C76 O31 Cr9 137.6(10) . . ? C76 O32 Cr10 131.7(10) . . ? C81 O33 Cr9 133.5(10) . . ? C81 O34 Cr10 132.4(9) . . ? C86 O35 Cr10 126.9(8) . . ? C86 O36 Cr1 129.5(8) . . ? C100 N1 C106 116.7(17) . . ? C100 N1 C112 118.5(18) . . ? C106 N1 C112 110.0(16) . . ? C100 N1 H1 103.0 . . ? C106 N1 H1 103.0 . . ? C112 N1 H1 103.0 . . ? O1 C1 O2 125.4(12) . . ? O1 C1 C2 118.1(12) . . ? O2 C1 C2 116.3(11) . . ? C1 C2 C5 110.4(13) . . ? C1 C2 C3 109.9(13) . . ? C5 C2 C3 109.5(5) . . ? C1 C2 C4 108.4(14) . . ? C5 C2 C4 109.3(5) . . ? C3 C2 C4 109.4(5) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 124.7(15) . . ? O3 C6 C7 116.8(13) . . ? O4 C6 C7 118.1(12) . . ? C10 C7 C9 109.7(5) . . ? C10 C7 C8 109.7(5) . . ? C9 C7 C8 109.8(5) . . ? C10 C7 C6 110.8(11) . . ? C9 C7 C6 106.7(11) . . ? C8 C7 C6 110.1(11) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O5 C11 O6 126.1(15) . . ? O5 C11 C12 119.0(15) . . ? O6 C11 C12 114.9(15) . . ? C14 C12 C13 109.8(5) . . ? C14 C12 C15 109.8(5) . . ? C13 C12 C15 109.7(5) . . ? C14 C12 C11 104(2) . . ? C13 C12 C11 107.4(18) . . ? C15 C12 C11 116(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O8 C16 O7 125.7(15) . . ? O8 C16 C17 116.7(13) . . ? O7 C16 C17 117.5(14) . . ? C20 C17 C16 109.5(12) . . ? C20 C17 C18 109.8(5) . . ? C16 C17 C18 112.2(12) . . ? C20 C17 C19 109.8(5) . . ? C16 C17 C19 106.2(12) . . ? C18 C17 C19 109.3(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O10 C21 O9 126.0(16) . . ? O10 C21 C22 115.7(19) . . ? O9 C21 C22 118.1(19) . . ? C21 C22 C24 104(2) . . ? C21 C22 C25 103(3) . . ? C24 C22 C25 109.3(5) . . ? C21 C22 C23 122(3) . . ? C24 C22 C23 109.3(5) . . ? C25 C22 C23 109.3(5) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O11 C26 O12 124.6(13) . . ? O11 C26 C27 118.2(13) . . ? O12 C26 C27 116.5(13) . . ? C26 C27 C28 112.3(12) . . ? C26 C27 C29 110.8(12) . . ? C28 C27 C29 109.6(5) . . ? C26 C27 C30 105.3(12) . . ? C28 C27 C30 109.3(5) . . ? C29 C27 C30 109.3(5) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O14 C31 O13 126.8(13) . . ? O14 C31 C32 115.5(13) . . ? O13 C31 C32 117.5(13) . . ? C35 C32 C34 109.3(5) . . ? C35 C32 C33 109.4(5) . . ? C34 C32 C33 109.2(5) . . ? C35 C32 C31 113.5(15) . . ? C34 C32 C31 103.0(15) . . ? C33 C32 C31 112.3(15) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O16 C36 O15 127.8(16) . . ? O16 C36 C37 119.2(16) . . ? O15 C36 C37 112.1(13) . . ? C40 C37 C38 109.5(5) . . ? C40 C37 C39 109.2(5) . . ? C38 C37 C39 109.0(5) . . ? C40 C37 C36 106.1(14) . . ? C38 C37 C36 113.5(15) . . ? C39 C37 C36 109.6(14) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O18 C41 O17 127.2(13) . . ? O18 C41 C42 116.4(13) . . ? O17 C41 C42 116.1(12) . . ? C45 C42 C43 109.4(5) . . ? C45 C42 C44 109.4(5) . . ? C43 C42 C44 109.2(5) . . ? C45 C42 C41 113.8(14) . . ? C43 C42 C41 108.8(14) . . ? C44 C42 C41 106.2(15) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O20 C46 O19 125.1(11) . . ? O20 C46 C47 117.3(11) . . ? O19 C46 C47 117.0(11) . . ? C50 C47 C46 109.3(13) . . ? C50 C47 C48 109.6(5) . . ? C46 C47 C48 112.8(13) . . ? C50 C47 C49 109.3(5) . . ? C46 C47 C49 106.7(14) . . ? C48 C47 C49 109.0(5) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O21 C51 O22 125.7(13) . . ? O21 C51 C52 118.2(12) . . ? O22 C51 C52 115.6(11) . . ? C51 C52 C55 110.2(11) . . ? C51 C52 C53 110.5(11) . . ? C55 C52 C53 109.8(5) . . ? C51 C52 C54 107.3(11) . . ? C55 C52 C54 109.4(5) . . ? C53 C52 C54 109.6(5) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O24 C56 O23 125.7(18) . . ? O24 C56 C57 109.0(16) . . ? O23 C56 C57 121.5(18) . . ? C58 C57 C60 109.6(5) . . ? C58 C57 C59 109.4(5) . . ? C60 C57 C59 109.5(5) . . ? C58 C57 C56 109.2(14) . . ? C60 C57 C56 108.2(15) . . ? C59 C57 C56 110.9(14) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O25 C61 O26 125.2(16) . . ? O25 C61 C62 117.4(15) . . ? O26 C61 C62 117.1(14) . . ? C65 C62 C63 109.9(5) . . ? C65 C62 C65A 139.8(18) . . ? C63 C62 C65A 53.3(14) . . ? C65 C62 C64 109.8(5) . . ? C63 C62 C64 109.6(5) . . ? C65A C62 C64 58.6(14) . . ? C65 C62 C64A 60.8(14) . . ? C63 C62 C64A 144.4(19) . . ? C65A C62 C64A 109.3(5) . . ? C64 C62 C64A 53.1(14) . . ? C65 C62 C63A 51.1(13) . . ? C63 C62 C63A 60.8(13) . . ? C65A C62 C63A 109.3(5) . . ? C64 C62 C63A 138.5(19) . . ? C64A C62 C63A 109.0(5) . . ? C65 C62 C61 108.8(16) . . ? C63 C62 C61 108.1(16) . . ? C65A C62 C61 111.2(16) . . ? C64 C62 C61 110.5(17) . . ? C64A C62 C61 107.3(16) . . ? C63A C62 C61 110.7(16) . . ? 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 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C62 C65 H65A 109.5 . . ? C62 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C62 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C62 C63A H63D 109.5 . . ? C62 C63A H63E 109.5 . . ? H63D C63A H63E 109.5 . . ? C62 C63A H63F 109.5 . . ? H63D C63A H63F 109.5 . . ? H63E C63A H63F 109.5 . . ? C62 C64A H64D 109.5 . . ? C62 C64A H64E 109.5 . . ? H64D C64A H64E 109.5 . . ? C62 C64A H64F 109.5 . . ? H64D C64A H64F 109.5 . . ? H64E C64A H64F 109.5 . . ? C62 C65A H65D 109.5 . . ? C62 C65A H65E 109.5 . . ? H65D C65A H65E 109.5 . . ? C62 C65A H65F 109.5 . . ? H65D C65A H65F 109.5 . . ? H65E C65A H65F 109.5 . . ? O27 C66 O28 123.0(14) . . ? O27 C66 C67 120.4(14) . . ? O28 C66 C67 116.6(14) . . ? C68 C67 C70 109.8(5) . . ? C68 C67 C69 109.6(5) . . ? C70 C67 C69 109.7(5) . . ? C68 C67 C66 106.7(12) . . ? C70 C67 C66 109.5(14) . . ? C69 C67 C66 111.5(14) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C67 C70 H70A 109.5 . . ? C67 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C67 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? O29 C71 O30 124.8(17) . . ? O29 C71 C72 115.4(19) . . ? O30 C71 C72 119.8(19) . . ? C71 C72 C75 101(2) . . ? C71 C72 C74 110(2) . . ? C75 C72 C74 109.6(5) . . ? C71 C72 C73 116(2) . . ? C75 C72 C73 109.7(5) . . ? C74 C72 C73 109.7(5) . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C72 C74 H74A 109.5 . . ? C72 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C72 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C72 C75 H75A 109.5 . . ? C72 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C72 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? O32 C76 O31 122.9(13) . . ? O32 C76 C77 121.3(14) . . ? O31 C76 C77 115.7(13) . . ? C76 C77 C80 108.5(13) . . ? C76 C77 C78 113.8(14) . . ? C80 C77 C78 109.8(5) . . ? C76 C77 C79 105.4(13) . . ? C80 C77 C79 109.8(5) . . ? C78 C77 C79 109.4(5) . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C77 C79 H79A 109.5 . . ? C77 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C77 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C77 C80 H80A 109.5 . . ? C77 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C77 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? O33 C81 O34 125.5(14) . . ? O33 C81 C82 120.6(12) . . ? O34 C81 C82 113.6(13) . . ? C83 C82 C85 109.9(5) . . ? C83 C82 C84 109.6(5) . . ? C85 C82 C84 109.3(5) . . ? C83 C82 C81 109.1(10) . . ? C85 C82 C81 113.3(10) . . ? C84 C82 C81 105.4(9) . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C82 C84 H84A 109.5 . . ? C82 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C82 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C82 C85 H85A 109.5 . . ? C82 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C82 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? O36 C86 O35 124.3(11) . . ? O36 C86 C87 117.1(11) . . ? O35 C86 C87 118.6(11) . . ? C86 C87 C88 114.2(12) . . ? C86 C87 C90 106.9(12) . . ? C88 C87 C90 109.8(5) . . ? C86 C87 C89 106.4(13) . . ? C88 C87 C89 109.7(5) . . ? C90 C87 C89 109.6(5) . . ? C87 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C87 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C87 C89 H89A 109.5 . . ? C87 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C87 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C87 C90 H90A 109.5 . . ? C87 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C87 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? N1 C100 C101 118(2) . . ? N1 C100 C105 102.2(18) . . ? C101 C100 C105 110.1(19) . . ? N1 C100 H100 108.8 . . ? C101 C100 H100 108.8 . . ? C105 C100 H100 108.8 . . ? C102 C101 C100 102.4(18) . . ? C102 C101 H10D 111.3 . . ? C100 C101 H10D 111.3 . . ? C102 C101 H10E 111.3 . . ? C100 C101 H10E 111.3 . . ? H10D C101 H10E 109.2 . . ? C101 C102 C103 115.4(19) . . ? C101 C102 H10F 108.4 . . ? C103 C102 H10F 108.4 . . ? C101 C102 H10G 108.4 . . ? C103 C102 H10G 108.4 . . ? H10F C102 H10G 107.5 . . ? C102 C103 C104 102(2) . . ? C102 C103 H10H 111.4 . . ? C104 C103 H10H 111.4 . . ? C102 C103 H10I 111.4 . . ? C104 C103 H10I 111.4 . . ? H10H C103 H10I 109.3 . . ? C105 C104 C103 116(2) . . ? C105 C104 H10J 108.3 . . ? C103 C104 H10J 108.3 . . ? C105 C104 H10K 108.3 . . ? C103 C104 H10K 108.3 . . ? H10J C104 H10K 107.4 . . ? C104 C105 C100 100.3(19) . . ? C104 C105 H10L 111.7 . . ? C100 C105 H10L 111.7 . . ? C104 C105 H10M 111.7 . . ? C100 C105 H10M 111.7 . . ? H10L C105 H10M 109.5 . . ? C111 C106 N1 109.9(14) . . ? C111 C106 C107 111.5(14) . . ? N1 C106 C107 113.1(14) . . ? C111 C106 H106 107.3 . . ? N1 C106 H106 107.3 . . ? C107 C106 H106 107.3 . . ? C106 C107 C108 109.7(19) . . ? C106 C107 H10N 109.7 . . ? C108 C107 H10N 109.7 . . ? C106 C107 H10O 109.7 . . ? C108 C107 H10O 109.7 . . ? H10N C107 H10O 108.2 . . ? C109 C108 C107 114(3) . . ? C109 C108 H10P 108.7 . . ? C107 C108 H10P 108.7 . . ? C109 C108 H10Q 108.7 . . ? C107 C108 H10Q 108.7 . . ? H10P C108 H10Q 107.6 . . ? C110 C109 C108 114(3) . . ? C110 C109 H10R 108.7 . . ? C108 C109 H10R 108.7 . . ? C110 C109 H10S 108.7 . . ? C108 C109 H10S 108.7 . . ? H10R C109 H10S 107.6 . . ? C109 C110 C111 114(3) . . ? C109 C110 H11A 108.7 . . ? C111 C110 H11A 108.7 . . ? C109 C110 H11B 108.7 . . ? C111 C110 H11B 108.7 . . ? H11A C110 H11B 107.6 . . ? C106 C111 C110 109.8(18) . . ? C106 C111 H11C 109.7 . . ? C110 C111 H11C 109.7 . . ? C106 C111 H11D 109.7 . . ? C110 C111 H11D 109.7 . . ? H11C C111 H11D 108.2 . . ? C113 C112 N1 111(2) . . ? C113 C112 H11E 109.5 . . ? N1 C112 H11E 109.5 . . ? C113 C112 H11F 109.6 . . ? N1 C112 H11F 109.6 . . ? H11E C112 H11F 108.1 . . ? C112 C113 H11G 109.5 . . ? C112 C113 H11H 109.5 . . ? H11G C113 H11H 109.5 . . ? C112 C113 H11I 109.5 . . ? H11G C113 H11I 109.5 . . ? H11H C113 H11I 109.5 . . ? C114 O115 C116 125(4) . . ? O115 C116 C117 101(3) . . ? O115 C116 H116 129.6 . . ? C117 C116 H116 129.7 . . ? C115 C117 C116 101(4) . . ? C115 C117 H117 129.5 . . ? C116 C117 H117 129.4 . . ? C115 C114 O115 87(3) . . ? C115 C114 H114 136.4 . . ? O115 C114 H114 136.4 . . ? C117 C115 C114 125(4) . . ? C117 C115 H115 117.6 . . ? C114 C115 H115 117.7 . . ? 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 F6 Cr5 Ni6 F7 176.2(5) . . . . ? O17 Cr5 Ni6 F7 -81.0(4) . . . . ? O16 Cr5 Ni6 F7 -159.4(5) . . . . ? F5 Cr5 Ni6 F7 21.1(4) . . . . ? F4 Cr5 Ni6 F7 -1.2(4) . . . . ? O14 Cr5 Ni6 F7 99.6(5) . . . . ? F6 Cr5 Ni6 O21 -26.3(6) . . . . ? O17 Cr5 Ni6 O21 76.5(6) . . . . ? O16 Cr5 Ni6 O21 -1.9(6) . . . . ? F5 Cr5 Ni6 O21 178.6(6) . . . . ? F4 Cr5 Ni6 O21 156.2(6) . . . . ? O14 Cr5 Ni6 O21 -103.0(6) . . . . ? F6 Cr5 Ni6 O19 77.1(5) . . . . ? O17 Cr5 Ni6 O19 179.9(4) . . . . ? O16 Cr5 Ni6 O19 101.5(5) . . . . ? F5 Cr5 Ni6 O19 -78.0(4) . . . . ? F4 Cr5 Ni6 O19 -100.3(4) . . . . ? O14 Cr5 Ni6 O19 0.5(5) . . . . ? O17 Cr5 Ni6 F6 102.8(5) . . . . ? O16 Cr5 Ni6 F6 24.3(6) . . . . ? F5 Cr5 Ni6 F6 -155.1(5) . . . . ? F4 Cr5 Ni6 F6 -177.5(5) . . . . ? O14 Cr5 Ni6 F6 -76.7(5) . . . . ? F6 Cr5 Ni6 O18 -102.2(5) . . . . ? O17 Cr5 Ni6 O18 0.5(5) . . . . ? O16 Cr5 Ni6 O18 -77.9(5) . . . . ? F5 Cr5 Ni6 O18 102.7(5) . . . . ? F4 Cr5 Ni6 O18 80.3(4) . . . . ? O14 Cr5 Ni6 O18 -178.9(5) . . . . ? F6 Cr5 Ni6 F5 155.1(5) . . . . ? O17 Cr5 Ni6 F5 -102.1(4) . . . . ? O16 Cr5 Ni6 F5 179.5(5) . . . . ? F4 Cr5 Ni6 F5 -22.3(4) . . . . ? O14 Cr5 Ni6 F5 78.4(5) . . . . ? F1 Cr1 Cr10 F10 -0.4(4) . . . . ? F11 Cr1 Cr10 F10 23.4(5) . . . . ? F12 Cr1 Cr10 F10 179.5(4) . . . . ? O36 Cr1 Cr10 F10 -79.4(4) . . . . ? O3 Cr1 Cr10 F10 -155.3(5) . . . . ? O1 Cr1 Cr10 F10 103.2(4) . . . . ? F1 Cr1 Cr10 F12 -179.9(5) . . . . ? F11 Cr1 Cr10 F12 -156.1(5) . . . . ? O36 Cr1 Cr10 F12 101.1(5) . . . . ? O3 Cr1 Cr10 F12 25.2(6) . . . . ? O1 Cr1 Cr10 F12 -76.2(5) . . . . ? F1 Cr1 Cr10 F11 -23.8(5) . . . . ? F12 Cr1 Cr10 F11 156.1(5) . . . . ? O36 Cr1 Cr10 F11 -102.8(5) . . . . ? O3 Cr1 Cr10 F11 -178.6(6) . . . . ? O1 Cr1 Cr10 F11 79.9(5) . . . . ? F1 Cr1 Cr10 O34 156.4(5) . . . . ? F11 Cr1 Cr10 O34 -179.8(5) . . . . ? F12 Cr1 Cr10 O34 -23.7(5) . . . . ? O36 Cr1 Cr10 O34 77.4(5) . . . . ? O3 Cr1 Cr10 O34 1.6(6) . . . . ? O1 Cr1 Cr10 O34 -99.9(5) . . . . ? F1 Cr1 Cr10 O32 -102.8(5) . . . . ? F11 Cr1 Cr10 O32 -79.0(5) . . . . ? F12 Cr1 Cr10 O32 77.1(5) . . . . ? O36 Cr1 Cr10 O32 178.2(5) . . . . ? O3 Cr1 Cr10 O32 102.4(6) . . . . ? O1 Cr1 Cr10 O32 0.9(5) . . . . ? F1 Cr1 Cr10 O35 80.1(4) . . . . ? F11 Cr1 Cr10 O35 103.9(5) . . . . ? F12 Cr1 Cr10 O35 -100.0(5) . . . . ? O36 Cr1 Cr10 O35 1.1(4) . . . . ? O3 Cr1 Cr10 O35 -74.8(6) . . . . ? O1 Cr1 Cr10 O35 -176.2(5) . . . . ? F2 Cr2 F1 Cr1 -133.6(5) . . . . ? O4 Cr2 F1 Cr1 47.7(6) . . . . ? O7 Cr2 F1 Cr1 12(6) . . . . ? O5 Cr2 F1 Cr1 135.0(6) . . . . ? O2 Cr2 F1 Cr1 -43.1(5) . . . . ? F11 Cr1 F1 Cr2 150.4(5) . . . . ? F12 Cr1 F1 Cr2 165.1(17) . . . . ? O36 Cr1 F1 Cr2 -120.0(5) . . . . ? O3 Cr1 F1 Cr2 -33.2(6) . . . . ? O1 Cr1 F1 Cr2 56.5(5) . . . . ? Cr10 Cr1 F1 Cr2 165.5(3) . . . . ? F1 Cr2 F2 Cr3 -139.4(5) . . . . ? O4 Cr2 F2 Cr3 -7(14) . . . . ? O7 Cr2 F2 Cr3 43.0(5) . . . . ? O5 Cr2 F2 Cr3 -50.1(5) . . . . ? O2 Cr2 F2 Cr3 130.0(5) . . . . ? F3 Cr3 F2 Cr2 134.8(5) . . . . ? O9 Cr3 F2 Cr2 -134.2(6) . . . . ? O11 Cr3 F2 Cr2 -8(8) . . . . ? O6 Cr3 F2 Cr2 45.9(6) . . . . ? O8 Cr3 F2 Cr2 -48.0(7) . . . . ? O9 Cr3 F3 Cr4 53.5(6) . . . . ? F2 Cr3 F3 Cr4 143.1(5) . . . . ? O11 Cr3 F3 Cr4 -40.0(8) . . . . ? O6 Cr3 F3 Cr4 -125.9(6) . . . . ? O8 Cr3 F3 Cr4 24(10) . . . . ? F4 Cr4 F3 Cr3 -131.1(5) . . . . ? O15 Cr4 F3 Cr3 9(5) . . . . ? O13 Cr4 F3 Cr3 136.1(5) . . . . ? O12 Cr4 F3 Cr3 49.3(7) . . . . ? O10 Cr4 F3 Cr3 -41.8(5) . . . . ? O15 Cr4 F4 Cr5 47.7(5) . . . . ? O13 Cr4 F4 Cr5 -44.9(6) . . . . ? F3 Cr4 F4 Cr5 -135.8(5) . . . . ? O12 Cr4 F4 Cr5 15(45) . . . . ? O10 Cr4 F4 Cr5 134.9(5) . . . . ? F6 Cr5 F4 Cr4 147(2) . . . . ? O17 Cr5 F4 Cr4 -125.7(5) . . . . ? O16 Cr5 F4 Cr4 -37.1(5) . . . . ? F5 Cr5 F4 Cr4 143.6(5) . . . . ? O14 Cr5 F4 Cr4 52.5(5) . . . . ? Ni6 Cr5 F4 Cr4 158.7(3) . . . . ? F6 Cr5 F5 Ni6 -16.1(3) . . . . ? O17 Cr5 F5 Ni6 74.2(4) . . . . ? O16 Cr5 F5 Ni6 -6(6) . . . . ? F4 Cr5 F5 Ni6 163.4(3) . . . . ? O14 Cr5 F5 Ni6 -106.6(4) . . . . ? F7 Ni6 F5 Cr5 -163.6(3) . . . . ? O21 Ni6 F5 Cr5 -10(4) . . . . ? O19 Ni6 F5 Cr5 106.6(4) . . . . ? F6 Ni6 F5 Cr5 15.8(3) . . . . ? O18 Ni6 F5 Cr5 -73.2(4) . . . . ? O17 Cr5 F6 Ni6 -73.7(4) . . . . ? O16 Cr5 F6 Ni6 -162.4(4) . . . . ? F5 Cr5 F6 Ni6 16.9(3) . . . . ? F4 Cr5 F6 Ni6 13(3) . . . . ? O14 Cr5 F6 Ni6 107.9(4) . . . . ? F7 Ni6 F6 Cr5 -13.6(17) . . . . ? O21 Ni6 F6 Cr5 161.0(4) . . . . ? O19 Ni6 F6 Cr5 -107.2(4) . . . . ? O18 Ni6 F6 Cr5 73.6(4) . . . . ? F5 Ni6 F6 Cr5 -16.4(3) . . . . ? O22 Cr7 F7 Ni6 -50.2(5) . . . . ? O20 Cr7 F7 Ni6 42.9(5) . . . . ? F8 Cr7 F7 Ni6 132.3(5) . . . . ? O23 Cr7 F7 Ni6 -139.4(5) . . . . ? O25 Cr7 F7 Ni6 51(15) . . . . ? O21 Ni6 F7 Cr7 33.3(5) . . . . ? O19 Ni6 F7 Cr7 -58.4(5) . . . . ? F6 Ni6 F7 Cr7 -152.0(13) . . . . ? O18 Ni6 F7 Cr7 120.9(5) . . . . ? F5 Ni6 F7 Cr7 -149.3(5) . . . . ? Cr5 Ni6 F7 Cr7 -163.0(3) . . . . ? O24 Cr8 F8 Cr7 -43.3(6) . . . . ? O26 Cr8 F8 Cr7 49.8(7) . . . . ? F9 Cr8 F8 Cr7 -134.3(4) . . . . ? O29 Cr8 F8 Cr7 17(18) . . . . ? O27 Cr8 F8 Cr7 136.2(5) . . . . ? F7 Cr7 F8 Cr8 145.8(5) . . . . ? O22 Cr7 F8 Cr8 25(8) . . . . ? O20 Cr7 F8 Cr8 -121.7(5) . . . . ? O23 Cr7 F8 Cr8 54.6(5) . . . . ? O25 Cr7 F8 Cr8 -35.8(5) . . . . ? F10 Cr9 F9 Cr8 130.2(5) . . . . ? O28 Cr9 F9 Cr8 40.9(5) . . . . ? O30 Cr9 F9 Cr8 -52.5(6) . . . . ? O31 Cr9 F9 Cr8 -139.6(5) . . . . ? O33 Cr9 F9 Cr8 41(10) . . . . ? F8 Cr8 F9 Cr9 -146.0(4) . . . . ? O24 Cr8 F9 Cr9 122.3(5) . . . . ? O26 Cr8 F9 Cr9 -31(6) . . . . ? O29 Cr8 F9 Cr9 35.1(7) . . . . ? O27 Cr8 F9 Cr9 -55.1(5) . . . . ? F12 Cr10 F10 Cr9 -159.0(18) . . . . ? F11 Cr10 F10 Cr9 -146.5(5) . . . . ? O34 Cr10 F10 Cr9 36.1(5) . . . . ? O32 Cr10 F10 Cr9 -53.6(5) . . . . ? O35 Cr10 F10 Cr9 122.9(5) . . . . ? Cr1 Cr10 F10 Cr9 -161.1(3) . . . . ? F9 Cr9 F10 Cr10 134.9(5) . . . . ? O28 Cr9 F10 Cr10 -132.9(5) . . . . ? O30 Cr9 F10 Cr10 12(10) . . . . ? O31 Cr9 F10 Cr10 44.2(5) . . . . ? O33 Cr9 F10 Cr10 -47.3(5) . . . . ? F1 Cr1 F11 Cr10 161.9(3) . . . . ? F12 Cr1 F11 Cr10 -15.5(3) . . . . ? O36 Cr1 F11 Cr10 73.2(4) . . . . ? O3 Cr1 F11 Cr10 7(3) . . . . ? O1 Cr1 F11 Cr10 -106.3(4) . . . . ? F10 Cr10 F11 Cr1 -162.4(3) . . . . ? F12 Cr10 F11 Cr1 15.5(3) . . . . ? O34 Cr10 F11 Cr1 1(3) . . . . ? O32 Cr10 F11 Cr1 106.4(4) . . . . ? O35 Cr10 F11 Cr1 -72.7(4) . . . . ? F1 Cr1 F12 Cr10 0(2) . . . . ? F11 Cr1 F12 Cr10 15.5(3) . . . . ? O36 Cr1 F12 Cr10 -74.5(4) . . . . ? O3 Cr1 F12 Cr10 -161.4(4) . . . . ? O1 Cr1 F12 Cr10 109.1(4) . . . . ? F10 Cr10 F12 Cr1 -2(2) . . . . ? F11 Cr10 F12 Cr1 -15.3(3) . . . . ? O34 Cr10 F12 Cr1 162.5(4) . . . . ? O32 Cr10 F12 Cr1 -107.9(4) . . . . ? O35 Cr10 F12 Cr1 75.7(4) . . . . ? F1 Cr1 O1 C1 -39.1(13) . . . . ? F11 Cr1 O1 C1 -131.2(13) . . . . ? F12 Cr1 O1 C1 150.4(13) . . . . ? O36 Cr1 O1 C1 57(7) . . . . ? O3 Cr1 O1 C1 56.4(13) . . . . ? Cr10 Cr1 O1 C1 -170.7(12) . . . . ? F1 Cr2 O2 C1 2.4(15) . . . . ? F2 Cr2 O2 C1 93.1(15) . . . . ? O4 Cr2 O2 C1 -88.1(15) . . . . ? O7 Cr2 O2 C1 -174.1(15) . . . . ? O5 Cr2 O2 C1 -85(14) . . . . ? F1 Cr1 O3 C6 -4.1(14) . . . . ? F11 Cr1 O3 C6 151(3) . . . . ? F12 Cr1 O3 C6 172.8(14) . . . . ? O36 Cr1 O3 C6 84.3(14) . . . . ? O1 Cr1 O3 C6 -95.7(14) . . . . ? Cr10 Cr1 O3 C6 156.8(12) . . . . ? F1 Cr2 O4 C6 -45.5(14) . . . . ? F2 Cr2 O4 C6 -178(100) . . . . ? O7 Cr2 O4 C6 132.0(15) . . . . ? O5 Cr2 O4 C6 -134.8(15) . . . . ? O2 Cr2 O4 C6 45.1(14) . . . . ? F1 Cr2 O5 C11 114.7(16) . . . . ? F2 Cr2 O5 C11 24.1(16) . . . . ? O4 Cr2 O5 C11 -154.7(16) . . . . ? O7 Cr2 O5 C11 -68.9(16) . . . . ? O2 Cr2 O5 C11 -158(13) . . . . ? F3 Cr3 O6 C11 -103.2(18) . . . . ? O9 Cr3 O6 C11 172(100) . . . . ? F2 Cr3 O6 C11 -11.7(18) . . . . ? O11 Cr3 O6 C11 164.2(18) . . . . ? O8 Cr3 O6 C11 78.4(18) . . . . ? F1 Cr2 O7 C16 -151(5) . . . . ? F2 Cr2 O7 C16 -5.4(15) . . . . ? O4 Cr2 O7 C16 173.3(15) . . . . ? O5 Cr2 O7 C16 86.2(15) . . . . ? O2 Cr2 O7 C16 -95.7(15) . . . . ? F3 Cr3 O8 C16 142(8) . . . . ? O9 Cr3 O8 C16 112(2) . . . . ? F2 Cr3 O8 C16 23(2) . . . . ? O11 Cr3 O8 C16 -154(2) . . . . ? O6 Cr3 O8 C16 -68(2) . . . . ? F3 Cr3 O9 C21 -33.6(18) . . . . ? F2 Cr3 O9 C21 -125.2(18) . . . . ? O11 Cr3 O9 C21 58.9(19) . . . . ? O6 Cr3 O9 C21 51(68) . . . . ? O8 Cr3 O9 C21 144.8(18) . . . . ? F4 Cr4 O10 C21 90.1(17) . . . . ? O15 Cr4 O10 C21 -176.1(17) . . . . ? O13 Cr4 O10 C21 -97(13) . . . . ? F3 Cr4 O10 C21 -0.3(17) . . . . ? O12 Cr4 O10 C21 -90.5(17) . . . . ? F3 Cr3 O11 C26 -2(2) . . . . ? O9 Cr3 O11 C26 -93(2) . . . . ? F2 Cr3 O11 C26 141(6) . . . . ? O6 Cr3 O11 C26 87(2) . . . . ? O8 Cr3 O11 C26 -179(2) . . . . ? F4 Cr4 O12 C26 -179(100) . . . . ? O15 Cr4 O12 C26 148.1(18) . . . . ? O13 Cr4 O12 C26 -119.3(18) . . . . ? F3 Cr4 O12 C26 -28.4(17) . . . . ? O10 Cr4 O12 C26 60.9(18) . . . . ? F4 Cr4 O13 C31 13.3(15) . . . . ? O15 Cr4 O13 C31 -80.6(15) . . . . ? F3 Cr4 O13 C31 103.7(15) . . . . ? O12 Cr4 O13 C31 -166.1(16) . . . . ? O10 Cr4 O13 C31 -159(13) . . . . ? F6 Cr5 O14 C31 151.8(14) . . . . ? O17 Cr5 O14 C31 28(15) . . . . ? O16 Cr5 O14 C31 57.1(14) . . . . ? F5 Cr5 O14 C31 -126.6(14) . . . . ? F4 Cr5 O14 C31 -36.5(14) . . . . ? Ni6 Cr5 O14 C31 -168.8(13) . . . . ? F4 Cr4 O15 C36 -29.4(13) . . . . ? O13 Cr4 O15 C36 63.6(13) . . . . ? F3 Cr4 O15 C36 -169(4) . . . . ? O12 Cr4 O15 C36 150.2(14) . . . . ? O10 Cr4 O15 C36 -118.5(13) . . . . ? F6 Cr5 O16 C36 176.1(14) . . . . ? O17 Cr5 O16 C36 85.8(14) . . . . ? F5 Cr5 O16 C36 166(5) . . . . ? F4 Cr5 O16 C36 -3.3(14) . . . . ? O14 Cr5 O16 C36 -93.3(14) . . . . ? Ni6 Cr5 O16 C36 160.4(12) . . . . ? F6 Cr5 O17 C41 32.6(13) . . . . ? O16 Cr5 O17 C41 127.2(13) . . . . ? F5 Cr5 O17 C41 -49.0(13) . . . . ? F4 Cr5 O17 C41 -139.1(13) . . . . ? O14 Cr5 O17 C41 157(13) . . . . ? Ni6 Cr5 O17 C41 -6.9(12) . . . . ? F7 Ni6 O18 C41 135.1(13) . . . . ? O21 Ni6 O18 C41 -129.1(13) . . . . ? O19 Ni6 O18 C41 -120(30) . . . . ? F6 Ni6 O18 C41 -32.3(13) . . . . ? F5 Ni6 O18 C41 45.6(13) . . . . ? Cr5 Ni6 O18 C41 5.8(13) . . . . ? F7 Ni6 O19 C46 44.3(12) . . . . ? O21 Ni6 O19 C46 -51.5(12) . . . . ? F6 Ni6 O19 C46 -148.3(12) . . . . ? O18 Ni6 O19 C46 -61(30) . . . . ? F5 Ni6 O19 C46 133.8(12) . . . . ? Cr5 Ni6 O19 C46 173.7(11) . . . . ? F7 Cr7 O20 C46 1.4(15) . . . . ? O22 Cr7 O20 C46 94.4(15) . . . . ? F8 Cr7 O20 C46 -87.2(15) . . . . ? O23 Cr7 O20 C46 -147(6) . . . . ? O25 Cr7 O20 C46 -178.4(15) . . . . ? F7 Ni6 O21 C51 7.5(13) . . . . ? O19 Ni6 O21 C51 97.4(13) . . . . ? F6 Ni6 O21 C51 -171.4(13) . . . . ? O18 Ni6 O21 C51 -82.7(13) . . . . ? F5 Ni6 O21 C51 -146(4) . . . . ? Cr5 Ni6 O21 C51 -155.0(10) . . . . ? F7 Cr7 O22 C51 45.9(12) . . . . ? O20 Cr7 O22 C51 -46.8(12) . . . . ? F8 Cr7 O22 C51 167(7) . . . . ? O23 Cr7 O22 C51 137.0(12) . . . . ? O25 Cr7 O22 C51 -132.6(12) . . . . ? F7 Cr7 O23 C56 -126.1(17) . . . . ? O22 Cr7 O23 C56 141.1(17) . . . . ? O20 Cr7 O23 C56 23(7) . . . . ? F8 Cr7 O23 C56 -37.4(17) . . . . ? O25 Cr7 O23 C56 53.7(17) . . . . ? F8 Cr8 O24 C56 3(2) . . . . ? O26 Cr8 O24 C56 -89(2) . . . . ? F9 Cr8 O24 C56 93(2) . . . . ? O29 Cr8 O24 C56 -175(2) . . . . ? O27 Cr8 O24 C56 -166(11) . . . . ? F7 Cr7 O25 C61 79(15) . . . . ? O22 Cr7 O25 C61 -179.6(16) . . . . ? O20 Cr7 O25 C61 87.3(16) . . . . ? F8 Cr7 O25 C61 -2.1(16) . . . . ? O23 Cr7 O25 C61 -90.5(16) . . . . ? F8 Cr8 O26 C61 -42.1(18) . . . . ? O24 Cr8 O26 C61 49.8(18) . . . . ? F9 Cr8 O26 C61 -157(5) . . . . ? O29 Cr8 O26 C61 136.8(19) . . . . ? O27 Cr8 O26 C61 -132.8(18) . . . . ? F8 Cr8 O27 C66 130.5(14) . . . . ? O24 Cr8 O27 C66 -60(12) . . . . ? O26 Cr8 O27 C66 -137.4(15) . . . . ? F9 Cr8 O27 C66 40.7(14) . . . . ? O29 Cr8 O27 C66 -51.4(15) . . . . ? F9 Cr9 O28 C66 4.1(15) . . . . ? F10 Cr9 O28 C66 -85.4(15) . . . . ? O30 Cr9 O28 C66 96.3(15) . . . . ? O31 Cr9 O28 C66 -167(8) . . . . ? O33 Cr9 O28 C66 -175.9(15) . . . . ? F8 Cr8 O29 C71 -148(16) . . . . ? O24 Cr8 O29 C71 -88(2) . . . . ? O26 Cr8 O29 C71 178(2) . . . . ? F9 Cr8 O29 C71 3(2) . . . . ? O27 Cr8 O29 C71 92(2) . . . . ? F9 Cr9 O30 C71 49.9(18) . . . . ? F10 Cr9 O30 C71 172(9) . . . . ? O28 Cr9 O30 C71 -42.5(18) . . . . ? O31 Cr9 O30 C71 140.5(18) . . . . ? O33 Cr9 O30 C71 -127.9(18) . . . . ? F9 Cr9 O31 C76 -102.1(16) . . . . ? F10 Cr9 O31 C76 -12.6(16) . . . . ? O28 Cr9 O31 C76 69(9) . . . . ? O30 Cr9 O31 C76 165.8(16) . . . . ? O33 Cr9 O31 C76 77.8(16) . . . . ? F10 Cr10 O32 C76 40.0(15) . . . . ? F12 Cr10 O32 C76 -148.9(14) . . . . ? F11 Cr10 O32 C76 133.4(14) . . . . ? O34 Cr10 O32 C76 -55.3(15) . . . . ? O35 Cr10 O32 C76 -60(8) . . . . ? Cr1 Cr10 O32 C76 172.0(14) . . . . ? F9 Cr9 O33 C81 129(9) . . . . ? F10 Cr9 O33 C81 40.0(15) . . . . ? O28 Cr9 O33 C81 129.3(15) . . . . ? O30 Cr9 O33 C81 -137.3(16) . . . . ? O31 Cr9 O33 C81 -50.3(15) . . . . ? F10 Cr10 O34 C81 -0.9(13) . . . . ? F12 Cr10 O34 C81 -178.5(12) . . . . ? F11 Cr10 O34 C81 -164(2) . . . . ? O32 Cr10 O34 C81 90.1(13) . . . . ? O35 Cr10 O34 C81 -90.2(13) . . . . ? Cr1 Cr10 O34 C81 -163.4(10) . . . . ? F10 Cr10 O35 C86 134.6(12) . . . . ? F12 Cr10 O35 C86 -36.4(12) . . . . ? F11 Cr10 O35 C86 41.3(12) . . . . ? O34 Cr10 O35 C86 -130.0(12) . . . . ? O32 Cr10 O35 C86 -125(7) . . . . ? Cr1 Cr10 O35 C86 3.2(12) . . . . ? F1 Cr1 O36 C86 -137.1(13) . . . . ? F11 Cr1 O36 C86 -45.1(13) . . . . ? F12 Cr1 O36 C86 33.3(13) . . . . ? O3 Cr1 O36 C86 127.3(13) . . . . ? O1 Cr1 O36 C86 127(6) . . . . ? Cr10 Cr1 O36 C86 -6.2(12) . . . . ? Cr1 O1 C1 O2 11(2) . . . . ? Cr1 O1 C1 C2 -164.4(10) . . . . ? Cr2 O2 C1 O1 14(3) . . . . ? Cr2 O2 C1 C2 -171.3(10) . . . . ? O1 C1 C2 C5 -151.7(14) . . . . ? O2 C1 C2 C5 32.9(17) . . . . ? O1 C1 C2 C3 -30.9(18) . . . . ? O2 C1 C2 C3 153.7(14) . . . . ? O1 C1 C2 C4 88.6(16) . . . . ? O2 C1 C2 C4 -86.8(16) . . . . ? Cr1 O3 C6 O4 12(2) . . . . ? Cr1 O3 C6 C7 -175.2(9) . . . . ? Cr2 O4 C6 O3 20(2) . . . . ? Cr2 O4 C6 C7 -152.5(10) . . . . ? O3 C6 C7 C10 161.9(11) . . . . ? O4 C6 C7 C10 -25.0(16) . . . . ? O3 C6 C7 C9 -78.7(14) . . . . ? O4 C6 C7 C9 94.4(13) . . . . ? O3 C6 C7 C8 40.4(15) . . . . ? O4 C6 C7 C8 -146.5(12) . . . . ? Cr2 O5 C11 O6 3(3) . . . . ? Cr2 O5 C11 C12 -177.1(11) . . . . ? Cr3 O6 C11 O5 -11(3) . . . . ? Cr3 O6 C11 C12 168.9(12) . . . . ? O5 C11 C12 C14 -68(2) . . . . ? O6 C11 C12 C14 112(2) . . . . ? O5 C11 C12 C13 49(2) . . . . ? O6 C11 C12 C13 -131.6(19) . . . . ? O5 C11 C12 C15 171.6(19) . . . . ? O6 C11 C12 C15 -9(2) . . . . ? Cr3 O8 C16 O7 8(3) . . . . ? Cr3 O8 C16 C17 -176.1(13) . . . . ? Cr2 O7 C16 O8 -19(3) . . . . ? Cr2 O7 C16 C17 164.3(10) . . . . ? O8 C16 C17 C20 -57.9(18) . . . . ? O7 C16 C17 C20 118.7(14) . . . . ? O8 C16 C17 C18 179.9(15) . . . . ? O7 C16 C17 C18 -3.5(17) . . . . ? O8 C16 C17 C19 60.5(17) . . . . ? O7 C16 C17 C19 -122.9(13) . . . . ? Cr4 O10 C21 O9 20(3) . . . . ? Cr4 O10 C21 C22 -155.9(15) . . . . ? Cr3 O9 C21 O10 3(3) . . . . ? Cr3 O9 C21 C22 178.6(15) . . . . ? O10 C21 C22 C24 -64(2) . . . . ? O9 C21 C22 C24 120(2) . . . . ? O10 C21 C22 C25 50(2) . . . . ? O9 C21 C22 C25 -126(2) . . . . ? O10 C21 C22 C23 173(2) . . . . ? O9 C21 C22 C23 -4(3) . . . . ? Cr3 O11 C26 O12 24(3) . . . . ? Cr3 O11 C26 C27 -166.4(15) . . . . ? Cr4 O12 C26 O11 -3(3) . . . . ? Cr4 O12 C26 C27 -173.4(11) . . . . ? O11 C26 C27 C28 13(2) . . . . ? O12 C26 C27 C28 -176.6(13) . . . . ? O11 C26 C27 C29 -110.2(18) . . . . ? O12 C26 C27 C29 60.5(16) . . . . ? O11 C26 C27 C30 131.6(17) . . . . ? O12 C26 C27 C30 -57.7(16) . . . . ? Cr5 O14 C31 O13 14(3) . . . . ? Cr5 O14 C31 C32 -160.6(10) . . . . ? Cr4 O13 C31 O14 2(3) . . . . ? Cr4 O13 C31 C32 176.5(11) . . . . ? O14 C31 C32 C35 -13.7(19) . . . . ? O13 C31 C32 C35 170.8(14) . . . . ? O14 C31 C32 C34 104.4(15) . . . . ? O13 C31 C32 C34 -71.1(17) . . . . ? O14 C31 C32 C33 -138.3(15) . . . . ? O13 C31 C32 C33 46.1(18) . . . . ? Cr5 O16 C36 O15 25(3) . . . . ? Cr5 O16 C36 C37 -167.2(9) . . . . ? Cr4 O15 C36 O16 -4(3) . . . . ? Cr4 O15 C36 C37 -172.5(8) . . . . ? O16 C36 C37 C40 42.4(17) . . . . ? O15 C36 C37 C40 -148.0(13) . . . . ? O16 C36 C37 C38 162.6(14) . . . . ? O15 C36 C37 C38 -27.8(16) . . . . ? O16 C36 C37 C39 -75.3(17) . . . . ? O15 C36 C37 C39 94.3(14) . . . . ? Ni6 O18 C41 O17 -14(2) . . . . ? Ni6 O18 C41 C42 160.3(10) . . . . ? Cr5 O17 C41 O18 15(2) . . . . ? Cr5 O17 C41 C42 -159.6(10) . . . . ? O18 C41 C42 C45 43.5(19) . . . . ? O17 C41 C42 C45 -141.7(14) . . . . ? O18 C41 C42 C43 165.7(14) . . . . ? O17 C41 C42 C43 -19.4(17) . . . . ? O18 C41 C42 C44 -76.9(16) . . . . ? O17 C41 C42 C44 97.9(15) . . . . ? Cr7 O20 C46 O19 -18(2) . . . . ? Cr7 O20 C46 C47 171.7(10) . . . . ? Ni6 O19 C46 O20 -13(2) . . . . ? Ni6 O19 C46 C47 157.8(10) . . . . ? O20 C46 C47 C50 -48.1(16) . . . . ? O19 C46 C47 C50 140.7(13) . . . . ? O20 C46 C47 C48 -170.3(13) . . . . ? O19 C46 C47 C48 18.5(17) . . . . ? O20 C46 C47 C49 70.1(15) . . . . ? O19 C46 C47 C49 -101.1(15) . . . . ? Ni6 O21 C51 O22 -19(2) . . . . ? Ni6 O21 C51 C52 170.1(9) . . . . ? Cr7 O22 C51 O21 -15(2) . . . . ? Cr7 O22 C51 C52 156.3(9) . . . . ? O21 C51 C52 C55 -157.5(11) . . . . ? O22 C51 C52 C55 30.4(14) . . . . ? O21 C51 C52 C53 -36.1(14) . . . . ? O22 C51 C52 C53 151.9(11) . . . . ? O21 C51 C52 C54 83.4(13) . . . . ? O22 C51 C52 C54 -88.6(12) . . . . ? Cr8 O24 C56 O23 14(3) . . . . ? Cr8 O24 C56 C57 172.3(12) . . . . ? Cr7 O23 C56 O24 10(3) . . . . ? Cr7 O23 C56 C57 -145.7(13) . . . . ? O24 C56 C57 C58 175.8(15) . . . . ? O23 C56 C57 C58 -25(2) . . . . ? O24 C56 C57 C60 56.5(18) . . . . ? O23 C56 C57 C60 -144.3(17) . . . . ? O24 C56 C57 C59 -63.5(19) . . . . ? O23 C56 C57 C59 95.6(19) . . . . ? Cr7 O25 C61 O26 12(3) . . . . ? Cr7 O25 C61 C62 -161.3(11) . . . . ? Cr8 O26 C61 O25 16(3) . . . . ? Cr8 O26 C61 C62 -170.4(11) . . . . ? O25 C61 C62 C65 -107.9(17) . . . . ? O26 C61 C62 C65 77.8(19) . . . . ? O25 C61 C62 C63 132.7(16) . . . . ? O26 C61 C62 C63 -42(2) . . . . ? O25 C61 C62 C65A 75.9(18) . . . . ? O26 C61 C62 C65A -98.3(19) . . . . ? O25 C61 C62 C64 12.7(19) . . . . ? O26 C61 C62 C64 -161.5(18) . . . . ? O25 C61 C62 C64A -43.6(18) . . . . ? O26 C61 C62 C64A 142.1(18) . . . . ? O25 C61 C62 C63A -162.5(15) . . . . ? O26 C61 C62 C63A 23(2) . . . . ? Cr8 O27 C66 O28 -8(2) . . . . ? Cr8 O27 C66 C67 170.5(9) . . . . ? Cr9 O28 C66 O27 -22(2) . . . . ? Cr9 O28 C66 C67 159.1(10) . . . . ? O27 C66 C67 C68 -103.2(16) . . . . ? O28 C66 C67 C68 75.6(15) . . . . ? O27 C66 C67 C70 15.7(18) . . . . ? O28 C66 C67 C70 -165.6(13) . . . . ? O27 C66 C67 C69 137.2(15) . . . . ? O28 C66 C67 C69 -44.0(16) . . . . ? Cr8 O29 C71 O30 -9(4) . . . . ? Cr8 O29 C71 C72 169.8(17) . . . . ? Cr9 O30 C71 O29 -25(3) . . . . ? Cr9 O30 C71 C72 156.8(15) . . . . ? O29 C71 C72 C75 -124(2) . . . . ? O30 C71 C72 C75 55(2) . . . . ? O29 C71 C72 C74 120(2) . . . . ? O30 C71 C72 C74 -61(2) . . . . ? O29 C71 C72 C73 -5(3) . . . . ? O30 C71 C72 C73 173.2(19) . . . . ? Cr10 O32 C76 O31 -19(2) . . . . ? Cr10 O32 C76 C77 157.4(11) . . . . ? Cr9 O31 C76 O32 1(3) . . . . ? Cr9 O31 C76 C77 -175.3(11) . . . . ? O32 C76 C77 C80 35.4(18) . . . . ? O31 C76 C77 C80 -148.3(14) . . . . ? O32 C76 C77 C78 157.9(14) . . . . ? O31 C76 C77 C78 -25.8(18) . . . . ? O32 C76 C77 C79 -82.2(16) . . . . ? O31 C76 C77 C79 94.1(15) . . . . ? Cr9 O33 C81 O34 -15(3) . . . . ? Cr9 O33 C81 C82 172.3(8) . . . . ? Cr10 O34 C81 O33 -10(2) . . . . ? Cr10 O34 C81 C82 162.6(8) . . . . ? O33 C81 C82 C83 4.6(16) . . . . ? O34 C81 C82 C83 -168.5(10) . . . . ? O33 C81 C82 C85 127.4(13) . . . . ? O34 C81 C82 C85 -45.7(13) . . . . ? O33 C81 C82 C84 -113.0(14) . . . . ? O34 C81 C82 C84 73.8(12) . . . . ? Cr1 O36 C86 O35 11(2) . . . . ? Cr1 O36 C86 C87 -167.0(9) . . . . ? Cr10 O35 C86 O36 -9(2) . . . . ? Cr10 O35 C86 C87 169.0(9) . . . . ? O36 C86 C87 C88 -160.2(12) . . . . ? O35 C86 C87 C88 21.8(17) . . . . ? O36 C86 C87 C90 -38.6(16) . . . . ? O35 C86 C87 C90 143.4(13) . . . . ? O36 C86 C87 C89 78.6(15) . . . . ? O35 C86 C87 C89 -99.4(14) . . . . ? C106 N1 C100 C101 57(3) . . . . ? C112 N1 C100 C101 -78(3) . . . . ? C106 N1 C100 C105 177.8(16) . . . . ? C112 N1 C100 C105 43(3) . . . . ? N1 C100 C101 C102 -174(2) . . . . ? C105 C100 C101 C102 70(2) . . . . ? C100 C101 C102 C103 -70(2) . . . . ? C101 C102 C103 C104 61(3) . . . . ? C102 C103 C104 C105 -58(3) . . . . ? C103 C104 C105 C100 61(3) . . . . ? N1 C100 C105 C104 168.2(19) . . . . ? C101 C100 C105 C104 -66(2) . . . . ? C100 N1 C106 C111 49(2) . . . . ? C112 N1 C106 C111 -172.2(16) . . . . ? C100 N1 C106 C107 174.3(18) . . . . ? C112 N1 C106 C107 -47(2) . . . . ? C111 C106 C107 C108 -49(3) . . . . ? N1 C106 C107 C108 -174(2) . . . . ? C106 C107 C108 C109 44(4) . . . . ? C107 C108 C109 C110 -46(5) . . . . ? C108 C109 C110 C111 55(5) . . . . ? N1 C106 C111 C110 -176.3(17) . . . . ? C107 C106 C111 C110 57(2) . . . . ? C109 C110 C111 C106 -60(3) . . . . ? C100 N1 C112 C113 57(3) . . . . ? C106 N1 C112 C113 -81(2) . . . . ? C114 O115 C116 C117 -5(6) . . . . ? O115 C116 C117 C115 -2(4) . . . . ? C116 O115 C114 C115 9(5) . . . . ? C116 C117 C115 C114 10(6) . . . . ? O115 C114 C115 C117 -11(5) . . . . ? 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 N1 H1 F5 0.91 1.79 2.701(16) 173.7 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.601 _refine_diff_density_min -0.875 _refine_diff_density_rms 0.174 data_orepw174absc _database_code_depnum_ccdc_archive 'CCDC 268355' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H190 Cr8 F12 N4 Ni2 O39' _chemical_formula_weight 2882.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr .3209 .6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni .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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.328(2) _cell_length_b 17.410(2) _cell_length_c 23.585(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.734(9) _cell_angle_gamma 90.00 _cell_volume 7581.2(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4561 _cell_measurement_theta_min 2.5152 _cell_measurement_theta_max 32.1203 _exptl_crystal_description prismatic _exptl_crystal_colour Green _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2968 _exptl_absorpt_coefficient_mu 0.872 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.6953 _exptl_absorpt_correction_T_max 0.8878 _exptl_absorpt_process_details ? _exptl_special_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38547 _diffrn_reflns_av_R_equivalents 0.0959 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 23.26 _reflns_number_total 10863 _reflns_number_gt 7771 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Due to poor data quality disordered carbons and central disordered amine have been left isotropic. No hydrogens have been placed on any atoms. Ni atoms are on symmetry site and averaged with Cr atoms. Large electron residue of 3.57 is 0.07 A from Cr7. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10863 _refine_ls_number_parameters 742 _refine_ls_number_restraints 232 _refine_ls_R_factor_all 0.1699 _refine_ls_R_factor_gt 0.1450 _refine_ls_wR_factor_ref 0.4447 _refine_ls_wR_factor_gt 0.3957 _refine_ls_goodness_of_fit_ref 1.814 _refine_ls_restrained_S_all 1.798 _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 0.97138(7) 0.23734(8) 0.88693(6) 0.0430(5) Uani 0.50 1 d P . . Ni2 Ni 0.86616(7) 0.23576(8) 0.94420(6) 0.0433(5) Uani 0.50 1 d P . . Cr1 Cr 0.97138(7) 0.23734(8) 0.88693(6) 0.0430(5) Uani 0.50 1 d P . . Cr2 Cr 0.86616(7) 0.23576(8) 0.94420(6) 0.0433(5) Uani 0.50 1 d P . . Cr3 Cr 0.78874(8) 0.16531(9) 1.03360(8) 0.0499(5) Uani 1 1 d . . . Cr5 Cr 0.90587(9) -0.15450(9) 1.15482(8) 0.0527(5) Uani 1 1 d . . . Cr4 Cr 0.79272(8) -0.00179(9) 1.10785(7) 0.0508(5) Uani 1 1 d . . . F1 F 0.8694(3) 0.1703(3) 1.0143(2) 0.0445(12) Uani 1 1 d . . . F2 F 0.8041(2) 0.0552(3) 1.0441(2) 0.0401(11) Uani 1 1 d . . . F3 F 0.8843(2) -0.0491(3) 1.1269(2) 0.0402(11) Uani 1 1 d . . . F4 F 0.9357(2) 0.1653(3) 0.9320(2) 0.0424(12) Uani 1 1 d . . . F5 F 0.8826(3) 0.2904(3) 0.8787(2) 0.0524(13) Uani 1 1 d . . . F6 F 1.0566(3) 0.1721(3) 0.9061(2) 0.0445(12) Uani 1 1 d . . . O1 O 0.8003(4) 0.3143(4) 0.9509(3) 0.0616(19) Uani 1 1 d . . . O2 O 0.7750(4) 0.2749(4) 1.0292(4) 0.070(2) Uani 1 1 d . . . O3 O 0.7834(4) 0.1727(4) 0.8862(3) 0.0579(17) Uani 1 1 d . . . O4 O 0.7254(3) 0.1485(4) 0.9468(4) 0.0590(18) Uani 1 1 d . . . O5 O 0.8546(5) 0.1788(5) 1.1224(4) 0.070(2) Uani 1 1 d . A . O6 O 0.8399(4) 0.0757(5) 1.1697(3) 0.067(2) Uani 1 1 d . A . O7 O 0.7052(4) 0.1595(4) 1.0530(4) 0.066(2) Uani 1 1 d . . . O8 O 0.6979(4) 0.0404(5) 1.0853(4) 0.075(2) Uani 1 1 d . . . O9 O 0.7773(5) -0.0592(5) 1.1725(5) 0.083(3) Uani 1 1 d . B . O10 O 0.8714(5) -0.1358(5) 1.2204(4) 0.078(2) Uani 1 1 d . B . O11 O 0.7466(3) -0.0846(5) 1.0464(4) 0.068(2) Uani 1 1 d . . . O12 O 0.8116(4) -0.1865(4) 1.0946(4) 0.065(2) Uani 1 1 d . . . O13 O 1.0010(4) -0.1200(5) 1.2158(3) 0.069(2) Uani 1 1 d . . . O14 O 0.9181(3) 0.1837(4) 0.8069(3) 0.0572(17) Uani 1 1 d . . . O15 O 1.0289(3) 0.2886(4) 0.9679(3) 0.0502(16) Uani 1 1 d . . . O16 O 0.9483(4) 0.2925(4) 1.0089(3) 0.0502(16) Uani 1 1 d . . . O17 O 1.0023(4) 0.3189(4) 0.8461(3) 0.0593(18) Uani 1 1 d . . . O18 O 0.9222(5) -0.2581(5) 1.1845(4) 0.078(2) Uani 1 1 d . . . C1 C 0.7737(6) 0.3234(6) 0.9880(5) 0.056(2) Uani 1 1 d . . . C2 C 0.7369(6) 0.3996(7) 0.9875(6) 0.066(3) Uani 1 1 d . . . C3 C 0.6584(8) 0.3947(10) 0.9342(9) 0.110(5) Uani 1 1 d . . . C4 C 0.7746(9) 0.4625(8) 0.9707(7) 0.091(4) Uani 1 1 d . . . C5 C 0.7315(13) 0.4131(9) 1.0500(9) 0.129(8) Uani 1 1 d . . . C6 C 0.7301(5) 0.1475(6) 0.8948(5) 0.052(2) Uani 1 1 d . . . C7 C 0.6678(6) 0.1075(8) 0.8421(6) 0.082(4) Uani 1 1 d . . . C8 C 0.6018(7) 0.1567(10) 0.8250(10) 0.128(7) Uani 1 1 d . . . C9 C 0.6519(11) 0.0283(10) 0.8676(9) 0.132(7) Uani 1 1 d . . . C10 C 0.6899(11) 0.0897(10) 0.7881(7) 0.116(6) Uani 1 1 d . . . C11 C 0.8683(5) 0.1409(8) 1.1695(5) 0.063(3) Uani 1 1 d . . . C12 C 0.9343(17) 0.1600(17) 1.2341(16) 0.13(2) Uiso 0.38(2) 1 d PD A 1 C13 C 0.922(2) 0.236(2) 1.256(2) 0.101(11) Uiso 0.38(2) 1 d PDU A 1 C14 C 1.0038(18) 0.1614(19) 1.2276(18) 0.085(10) Uiso 0.38(2) 1 d PDU A 1 C15 C 0.939(3) 0.101(2) 1.281(3) 0.140(12) Uiso 0.38(2) 1 d PDU A 1 C12A C 0.9177(10) 0.1696(9) 1.2352(8) 0.069(6) Uiso 0.62(2) 1 d PD A 2 C13A C 0.9235(13) 0.2536(10) 1.2284(13) 0.093(7) Uiso 0.62(2) 1 d PDU A 2 C14A C 0.9905(15) 0.1345(16) 1.2556(16) 0.136(9) Uiso 0.62(2) 1 d PDU A 2 C15A C 0.8902(16) 0.1549(15) 1.2834(13) 0.125(10) Uiso 0.62(2) 1 d PDU A 2 C16 C 0.6718(5) 0.1046(6) 1.0649(5) 0.051(2) Uani 1 1 d . . . C17 C 0.5936(6) 0.1230(6) 1.0565(6) 0.061(3) Uani 1 1 d . . . C18 C 0.5933(9) 0.1996(10) 1.0882(12) 0.143(9) Uani 1 1 d . . . C19 C 0.5670(8) 0.0574(10) 1.0850(8) 0.098(5) Uani 1 1 d . . . C20 C 0.5483(7) 0.1200(14) 0.9858(8) 0.131(7) Uani 1 1 d . . . C21 C 0.8193(7) -0.1017(7) 1.2178(6) 0.069(3) Uani 1 1 d . . . C22 C 0.8300(18) -0.1105(16) 1.2903(18) 0.130(19) Uiso 0.37(3) 1 d PD B 1 C23 C 0.7817(19) -0.0393(14) 1.2909(16) 0.069(11) Uiso 0.37(3) 1 d PDU B 1 C24 C 0.9053(19) -0.110(3) 1.350(3) 0.19(3) Uiso 0.37(3) 1 d PDU B 1 C25 C 0.788(2) -0.1890(15) 1.2855(19) 0.072(11) Uiso 0.37(3) 1 d PDU B 1 C22A C 0.7960(8) -0.1149(7) 1.2701(7) 0.056(5) Uiso 0.63(3) 1 d PD B 2 C23A C 0.7321(12) -0.0599(12) 1.2661(11) 0.102(9) Uiso 0.63(3) 1 d PDU B 2 C24A C 0.8658(10) -0.1018(9) 1.3335(8) 0.068(6) Uiso 0.63(3) 1 d PDU B 2 C25A C 0.7712(12) -0.2022(10) 1.2634(14) 0.106(9) Uiso 0.63(3) 1 d PDU B 2 C26 C 0.7624(7) -0.1563(7) 1.0524(6) 0.064(3) Uani 1 1 d . C . C27 C 0.7123(7) -0.2078(8) 0.9982(7) 0.098(4) Uani 1 1 d D . . C28 C 0.7132(14) -0.2911(11) 1.0187(13) 0.111(10) Uiso 0.62(4) 1 d PDU C 1 C29 C 0.7509(14) -0.2013(16) 0.9549(13) 0.118(11) Uiso 0.62(4) 1 d PDU C 1 C30 C 0.6348(10) -0.1788(13) 0.9649(12) 0.098(9) Uiso 0.62(4) 1 d PDU C 1 C28A C 0.739(2) -0.2907(13) 1.003(2) 0.117(16) Uiso 0.38(4) 1 d PDU C 2 C29A C 0.703(3) -0.174(2) 0.9351(13) 0.119(18) Uiso 0.38(4) 1 d PDU C 2 C30A C 0.6391(17) -0.206(3) 1.003(2) 0.14(2) Uiso 0.38(4) 1 d PDU C 2 C31 C 1.0641(6) -0.1439(7) 1.2278(6) 0.063(3) Uani 1 1 d . . . C32 C 1.1233(7) -0.1158(7) 1.2900(5) 0.086(4) Uani 1 1 d D . . C33 C 1.091(3) -0.043(2) 1.304(3) 0.13(2) Uiso 0.28(2) 1 d PDU D 1 C34 C 1.191(2) -0.096(3) 1.281(4) 0.15(3) Uiso 0.28(2) 1 d PDU D 1 C35 C 1.142(4) -0.172(3) 1.344(3) 0.23(4) Uiso 0.28(2) 1 d PDU D 1 C33A C 1.1402(12) -0.0325(10) 1.2823(12) 0.121(9) Uiso 0.72(2) 1 d PDU D 2 C34A C 1.1924(10) -0.1630(10) 1.3100(9) 0.089(6) Uiso 0.72(2) 1 d PDU D 2 C35A C 1.0935(10) -0.1222(10) 1.3388(8) 0.085(6) Uiso 0.72(2) 1 d PDU D 2 C36 C 1.0078(5) 0.3075(5) 1.0085(4) 0.043(2) Uani 1 1 d . . . C37 C 1.0609(6) 0.3497(6) 1.0666(5) 0.060(3) Uani 1 1 d . . . C38 C 1.1142(10) 0.3963(10) 1.0474(10) 0.131(7) Uani 1 1 d . . . C39 C 1.1075(8) 0.2864(8) 1.1144(6) 0.089(4) Uani 1 1 d . . . C40 C 1.0201(10) 0.3969(11) 1.0963(8) 0.121(7) Uani 1 1 d . . . C41 C 1.0450(6) 0.3174(6) 0.8217(6) 0.064(3) Uani 1 1 d . . . C42 C 1.0580(9) 0.3906(8) 0.7919(9) 0.103(4) Uani 1 1 d U . . C43 C 1.0128(13) 0.3813(11) 0.7192(10) 0.137(6) Uani 1 1 d U . . C44 C 1.1369(11) 0.3988(11) 0.8110(14) 0.160(8) Uani 1 1 d U . . C45 C 1.0287(10) 0.4606(7) 0.8141(11) 0.120(6) Uani 1 1 d U . . N1 N 0.0603(7) 0.0351(7) 0.0819(6) 0.042(3) Uiso 0.50 1 d PDU E 1 C100 C 0.0417(13) 0.0985(12) 0.0449(12) 0.050(9) Uiso 0.50 1 d PDU E 1 N2 N 0.0794(8) 0.0978(8) 0.0091(7) 0.049(4) Uiso 0.50 1 d PDU E 1 C101 C 0.1276(9) 0.0392(9) 0.0317(8) 0.050(5) Uiso 0.50 1 d PDU E 1 C102 C 0.1143(10) -0.0010(11) 0.0728(9) 0.061(5) Uiso 0.50 1 d PDU E 1 C103 C 0.0277(13) 0.0128(13) 0.1230(11) 0.060(5) Uiso 0.50 1 d PDU E 1 N1A N 0.0895(7) 0.0375(7) 0.0652(6) 0.043(3) Uiso 0.50 1 d PDU F 2 C104 C 0.0649(10) -0.0007(11) 0.1024(9) 0.061(5) Uiso 0.50 1 d PDU F 2 N2A N 0.0070(10) 0.0365(10) 0.1043(9) 0.077(6) Uiso 0.50 1 d PDU F 2 C105 C -0.0073(9) 0.0935(9) 0.0613(7) 0.044(4) Uiso 0.50 1 d PDU F 2 C106 C 0.0381(12) 0.0911(14) 0.0353(12) 0.049(9) Uiso 0.50 1 d PDU F 2 C107 C 0.1504(11) 0.0150(13) 0.0533(11) 0.060(5) Uiso 0.50 1 d PDU F 2 C152 C 0.8180(12) 0.3753(15) 0.7475(11) 0.148(8) Uani 1 1 d . . . O50 O 0.6974(11) 0.3928(11) 0.6860(8) 0.236(11) Uani 1 1 d . . . C150 C 0.7436(12) 0.3668(10) 0.7327(8) 0.124(7) Uani 1 1 d . . . C151 C 0.7211(10) 0.3289(15) 0.7789(10) 0.145(8) Uani 1 1 d . . . O100 O 0.0000 0.0000 0.5000 0.39(3) Uiso 1 2 d S . . 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 0.0315(8) 0.0567(9) 0.0433(8) 0.0060(6) 0.0181(6) 0.0039(5) Ni2 0.0329(8) 0.0602(9) 0.0384(8) 0.0064(6) 0.0164(6) 0.0084(5) Cr1 0.0315(8) 0.0567(9) 0.0433(8) 0.0060(6) 0.0181(6) 0.0039(5) Cr2 0.0329(8) 0.0602(9) 0.0384(8) 0.0064(6) 0.0164(6) 0.0084(5) Cr3 0.0403(9) 0.0571(10) 0.0617(11) 0.0015(7) 0.0307(8) 0.0012(7) Cr5 0.0530(10) 0.0600(11) 0.0593(11) 0.0064(7) 0.0375(9) 0.0049(7) Cr4 0.0408(9) 0.0694(11) 0.0557(10) 0.0050(7) 0.0335(8) 0.0080(7) F1 0.037(3) 0.061(3) 0.044(3) 0.005(2) 0.025(2) 0.000(2) F2 0.032(2) 0.054(3) 0.039(3) -0.003(2) 0.019(2) 0.002(2) F3 0.037(3) 0.046(3) 0.045(3) -0.001(2) 0.023(2) -0.002(2) F4 0.035(3) 0.048(3) 0.050(3) 0.008(2) 0.023(2) 0.006(2) F5 0.045(3) 0.060(3) 0.050(3) 0.016(3) 0.019(3) 0.013(2) F6 0.037(3) 0.055(3) 0.044(3) 0.002(2) 0.021(2) 0.007(2) O1 0.051(4) 0.085(5) 0.053(4) 0.026(4) 0.026(4) 0.026(4) O2 0.077(5) 0.065(5) 0.095(6) 0.008(4) 0.062(5) 0.013(4) O3 0.037(4) 0.077(5) 0.056(4) 0.007(3) 0.015(3) 0.007(3) O4 0.037(4) 0.072(5) 0.071(5) 0.012(4) 0.026(4) 0.006(3) O5 0.090(6) 0.075(5) 0.066(5) -0.016(4) 0.053(5) -0.031(4) O6 0.074(5) 0.076(5) 0.048(4) -0.013(3) 0.023(4) -0.001(4) O7 0.053(4) 0.067(5) 0.091(6) 0.006(4) 0.044(4) 0.010(3) O8 0.062(5) 0.080(5) 0.112(7) 0.017(5) 0.065(5) 0.009(4) O9 0.085(6) 0.083(5) 0.127(8) 0.022(5) 0.088(6) 0.018(5) O10 0.106(7) 0.071(5) 0.088(6) 0.022(4) 0.073(6) 0.030(5) O11 0.033(4) 0.085(6) 0.073(5) 0.019(4) 0.009(4) -0.006(3) O12 0.042(4) 0.073(5) 0.084(5) -0.013(4) 0.029(4) 0.007(4) O13 0.078(6) 0.082(5) 0.037(4) 0.002(3) 0.015(4) 0.026(4) O14 0.043(4) 0.085(5) 0.051(4) -0.009(4) 0.028(3) 0.000(3) O15 0.038(3) 0.059(4) 0.059(4) -0.005(3) 0.025(3) -0.002(3) O16 0.052(4) 0.056(4) 0.043(3) 0.002(3) 0.020(3) 0.001(3) O17 0.056(4) 0.070(4) 0.070(5) 0.019(4) 0.044(4) 0.007(3) O18 0.091(6) 0.067(5) 0.102(6) 0.011(4) 0.066(6) 0.021(4) C1 0.057(6) 0.061(6) 0.059(6) -0.001(5) 0.034(6) 0.001(5) C2 0.057(6) 0.070(7) 0.079(8) 0.003(6) 0.038(6) 0.011(5) C3 0.061(8) 0.121(12) 0.141(14) 0.012(11) 0.035(9) 0.021(8) C4 0.111(11) 0.090(9) 0.091(9) 0.013(8) 0.062(9) 0.016(8) C5 0.23(2) 0.086(10) 0.138(14) 0.021(9) 0.143(16) 0.057(12) C6 0.037(5) 0.061(6) 0.052(6) -0.005(5) 0.012(5) 0.005(4) C7 0.051(7) 0.106(10) 0.071(8) -0.014(7) 0.007(6) 0.006(6) C8 0.043(7) 0.132(14) 0.153(16) 0.007(12) -0.013(9) 0.020(8) C9 0.145(16) 0.100(12) 0.128(14) -0.013(11) 0.034(13) -0.063(12) C10 0.139(15) 0.105(11) 0.059(8) -0.019(8) -0.002(9) -0.011(10) C11 0.032(5) 0.105(9) 0.051(6) -0.022(6) 0.017(5) -0.015(5) C16 0.042(5) 0.067(7) 0.054(6) -0.024(5) 0.030(5) -0.013(5) C17 0.050(6) 0.066(6) 0.082(7) -0.022(6) 0.042(6) -0.005(5) C18 0.098(11) 0.102(12) 0.26(3) -0.101(14) 0.112(15) -0.018(9) C19 0.067(8) 0.121(12) 0.132(13) -0.003(10) 0.068(9) -0.009(8) C20 0.038(7) 0.26(2) 0.097(11) 0.018(13) 0.029(8) 0.032(10) C21 0.079(8) 0.072(7) 0.081(8) 0.010(6) 0.058(7) 0.008(6) C26 0.063(7) 0.069(8) 0.064(7) -0.011(6) 0.029(6) -0.015(6) C27 0.086(10) 0.104(11) 0.108(11) -0.021(9) 0.044(9) -0.007(8) C31 0.048(6) 0.072(7) 0.064(7) 0.014(6) 0.019(6) 0.002(5) C32 0.099(10) 0.101(10) 0.043(6) 0.007(6) 0.016(7) 0.016(8) C36 0.036(5) 0.055(5) 0.040(5) -0.002(4) 0.018(4) 0.002(4) C37 0.048(6) 0.060(6) 0.063(6) -0.010(5) 0.015(5) -0.005(5) C38 0.118(14) 0.111(13) 0.169(19) -0.018(12) 0.066(14) -0.066(11) C39 0.093(10) 0.081(9) 0.057(7) -0.002(6) -0.002(7) 0.002(7) C40 0.110(12) 0.143(15) 0.110(12) -0.090(12) 0.045(10) -0.019(10) C41 0.058(7) 0.053(6) 0.075(7) 0.012(5) 0.023(6) 0.001(5) C42 0.122(10) 0.075(8) 0.163(11) 0.043(8) 0.108(10) 0.016(7) C43 0.193(16) 0.119(13) 0.146(10) 0.060(10) 0.117(11) 0.047(12) C44 0.120(10) 0.111(13) 0.30(2) 0.064(16) 0.141(13) -0.002(9) C45 0.142(13) 0.045(7) 0.213(17) 0.014(8) 0.114(14) 0.001(7) C152 0.109(15) 0.19(2) 0.131(17) 0.057(16) 0.040(14) 0.020(15) O50 0.24(2) 0.205(18) 0.125(12) 0.071(12) -0.054(13) 0.033(15) C150 0.129(16) 0.096(11) 0.090(11) 0.013(9) -0.009(12) -0.014(10) C151 0.081(12) 0.21(2) 0.127(15) 0.053(15) 0.026(11) 0.006(12) _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 F6 1.959(5) . ? Ni1 O17 1.961(7) . ? Ni1 F5 1.963(5) . ? Ni1 F4 1.969(5) . ? Ni1 O14 1.974(7) . ? Ni1 O15 1.985(7) . ? Ni1 Ni2 2.9696(17) . ? Ni2 F5 1.959(5) . ? Ni2 O1 1.967(7) . ? Ni2 F4 1.981(5) . ? Ni2 F1 1.986(5) . ? Ni2 O16 1.990(7) . ? Ni2 O3 1.995(7) . ? Cr3 F1 1.878(5) . ? Cr3 O2 1.924(7) . ? Cr3 O4 1.931(8) . ? Cr3 O7 1.936(7) . ? Cr3 F2 1.941(5) . ? Cr3 O5 1.972(8) . ? Cr5 F6 1.912(5) 3_757 ? Cr5 O18 1.912(8) . ? Cr5 O12 1.929(8) . ? Cr5 F3 1.937(5) . ? Cr5 O13 1.960(8) . ? Cr5 O10 1.975(8) . ? Cr4 F2 1.895(5) . ? Cr4 F3 1.910(5) . ? Cr4 O8 1.919(8) . ? Cr4 O6 1.922(7) . ? Cr4 O9 1.955(8) . ? Cr4 O11 1.981(8) . ? F6 Cr5 1.913(5) 3_757 ? O1 C1 1.213(12) . ? O2 C1 1.280(13) . ? O3 C6 1.261(12) . ? O4 C6 1.270(12) . ? O5 C11 1.219(14) . ? O6 C11 1.275(14) . ? O7 C16 1.272(12) . ? O8 C16 1.244(13) . ? O9 C21 1.287(15) . ? O10 C21 1.192(14) . ? O11 C26 1.281(14) . ? O12 C26 1.197(14) . ? O13 C31 1.263(13) . ? O14 C31 1.236(14) 3_757 ? O15 C36 1.247(10) . ? O16 C36 1.241(11) . ? O17 C41 1.226(13) . ? O18 C41 1.271(13) 3_757 ? C1 C2 1.521(15) . ? C2 C4 1.484(18) . ? C2 C5 1.540(19) . ? C2 C3 1.57(2) . ? C6 C7 1.521(15) . ? C7 C8 1.498(19) . ? C7 C10 1.55(2) . ? C7 C9 1.59(2) . ? C11 C12A 1.53(2) . ? C11 C12 1.59(3) . ? C12 C13 1.481(15) . ? C12 C14 1.483(15) . ? C12 C15 1.484(15) . ? C12A C13A 1.482(15) . ? C12A C14A 1.483(15) . ? C12A C15A 1.485(15) . ? C16 C17 1.550(13) . ? C17 C18 1.528(17) . ? C17 C20 1.53(2) . ? C17 C19 1.534(19) . ? C21 C22A 1.512(19) . ? C21 C22 1.64(4) . ? C22 C23 1.585(15) . ? C22 C25 1.586(15) . ? C22 C24 1.586(15) . ? C22A C23A 1.585(14) . ? C22A C25A 1.588(14) . ? C22A C24A 1.589(14) . ? C26 C27 1.546(18) . ? C27 C30 1.522(14) . ? C27 C28 1.527(14) . ? C27 C28A 1.527(15) . ? C27 C29 1.529(14) . ? C27 C29A 1.533(15) . ? C27 C30A 1.534(15) . ? C31 O14 1.236(14) 3_757 ? C31 C32 1.538(17) . ? C32 C35A 1.512(13) . ? C32 C35 1.515(15) . ? C32 C34 1.517(15) . ? C32 C33 1.518(15) . ? C32 C33A 1.519(14) . ? C32 C34A 1.521(13) . ? C36 C37 1.531(13) . ? C37 C40 1.530(18) . ? C37 C38 1.565(19) . ? C37 C39 1.578(17) . ? C41 O18 1.271(13) 3_757 ? C41 C42 1.530(16) . ? C42 C44 1.48(2) . ? C42 C45 1.54(2) . ? C42 C43 1.58(3) . ? N1 C102 1.358(11) . ? N1 C100 1.360(10) . ? N1 C103 1.44(2) . ? C100 N2 1.357(11) . ? N2 C101 1.360(11) . ? C101 C102 1.312(9) . ? N1A C104 1.355(11) . ? N1A C106 1.358(10) . ? N1A C107 1.43(2) . ? C104 N2A 1.358(11) . ? N2A C105 1.360(11) . ? C105 C106 1.304(9) . ? C152 C150 1.41(3) . ? O50 C150 1.20(2) . ? C150 C151 1.50(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F6 Ni1 O17 95.7(2) . . ? F6 Ni1 F5 169.4(2) . . ? O17 Ni1 F5 94.6(2) . . ? F6 Ni1 F4 89.8(2) . . ? O17 Ni1 F4 173.2(3) . . ? F5 Ni1 F4 79.7(2) . . ? F6 Ni1 O14 91.4(3) . . ? O17 Ni1 O14 91.9(3) . . ? F5 Ni1 O14 90.8(3) . . ? F4 Ni1 O14 92.1(3) . . ? F6 Ni1 O15 86.0(2) . . ? O17 Ni1 O15 88.0(3) . . ? F5 Ni1 O15 91.8(2) . . ? F4 Ni1 O15 88.2(2) . . ? O14 Ni1 O15 177.4(3) . . ? F6 Ni1 Ni2 128.69(15) . . ? O17 Ni1 Ni2 132.1(2) . . ? F5 Ni1 Ni2 40.73(15) . . ? F4 Ni1 Ni2 41.41(14) . . ? O14 Ni1 Ni2 102.68(19) . . ? O15 Ni1 Ni2 79.23(18) . . ? F5 Ni2 O1 94.2(3) . . ? F5 Ni2 F4 79.6(2) . . ? O1 Ni2 F4 173.5(3) . . ? F5 Ni2 F1 168.0(2) . . ? O1 Ni2 F1 96.8(2) . . ? F4 Ni2 F1 89.3(2) . . ? F5 Ni2 O16 89.9(2) . . ? O1 Ni2 O16 88.6(3) . . ? F4 Ni2 O16 89.9(2) . . ? F1 Ni2 O16 85.5(2) . . ? F5 Ni2 O3 95.7(3) . . ? O1 Ni2 O3 91.7(3) . . ? F4 Ni2 O3 90.4(2) . . ? F1 Ni2 O3 88.8(3) . . ? O16 Ni2 O3 174.3(3) . . ? F5 Ni2 Ni1 40.85(15) . . ? O1 Ni2 Ni1 132.4(2) . . ? F4 Ni2 Ni1 41.10(14) . . ? F1 Ni2 Ni1 127.21(15) . . ? O16 Ni2 Ni1 79.09(19) . . ? O3 Ni2 Ni1 104.8(2) . . ? F1 Cr3 O2 93.6(3) . . ? F1 Cr3 O4 90.7(3) . . ? O2 Cr3 O4 94.3(3) . . ? F1 Cr3 O7 179.5(3) . . ? O2 Cr3 O7 86.7(3) . . ? O4 Cr3 O7 88.9(3) . . ? F1 Cr3 F2 88.1(2) . . ? O2 Cr3 F2 176.1(3) . . ? O4 Cr3 F2 89.2(3) . . ? O7 Cr3 F2 91.7(3) . . ? F1 Cr3 O5 88.8(3) . . ? O2 Cr3 O5 87.6(4) . . ? O4 Cr3 O5 178.0(3) . . ? O7 Cr3 O5 91.6(3) . . ? F2 Cr3 O5 88.9(3) . . ? F6 Cr5 O18 93.5(3) 3_757 . ? F6 Cr5 O12 89.2(3) 3_757 . ? O18 Cr5 O12 87.9(4) . . ? F6 Cr5 F3 90.0(2) 3_757 . ? O18 Cr5 F3 176.1(3) . . ? O12 Cr5 F3 90.5(3) . . ? F6 Cr5 O13 91.1(3) 3_757 . ? O18 Cr5 O13 93.0(4) . . ? O12 Cr5 O13 178.9(3) . . ? F3 Cr5 O13 88.5(3) . . ? F6 Cr5 O10 177.6(3) 3_757 . ? O18 Cr5 O10 86.1(3) . . ? O12 Cr5 O10 93.2(4) . . ? F3 Cr5 O10 90.4(3) . . ? O13 Cr5 O10 86.5(4) . . ? F2 Cr4 F3 88.9(2) . . ? F2 Cr4 O8 91.3(3) . . ? F3 Cr4 O8 176.4(3) . . ? F2 Cr4 O6 92.7(3) . . ? F3 Cr4 O6 89.8(3) . . ? O8 Cr4 O6 93.8(4) . . ? F2 Cr4 O9 177.9(3) . . ? F3 Cr4 O9 93.1(3) . . ? O8 Cr4 O9 86.6(3) . . ? O6 Cr4 O9 87.7(4) . . ? F2 Cr4 O11 88.7(3) . . ? F3 Cr4 O11 88.5(3) . . ? O8 Cr4 O11 87.9(3) . . ? O6 Cr4 O11 177.8(3) . . ? O9 Cr4 O11 91.0(4) . . ? Cr3 F1 Ni2 120.0(3) . . ? Cr4 F2 Cr3 123.5(2) . . ? Cr4 F3 Cr5 123.2(2) . . ? Ni1 F4 Ni2 97.5(2) . . ? Ni2 F5 Ni1 98.4(2) . . ? Cr5 F6 Ni1 120.8(3) 3_757 . ? C1 O1 Ni2 132.2(7) . . ? C1 O2 Cr3 130.7(7) . . ? C6 O3 Ni2 128.1(7) . . ? C6 O4 Cr3 137.7(6) . . ? C11 O5 Cr3 134.3(7) . . ? C11 O6 Cr4 134.9(7) . . ? C16 O7 Cr3 133.9(6) . . ? C16 O8 Cr4 131.9(6) . . ? C21 O9 Cr4 132.4(7) . . ? C21 O10 Cr5 129.8(8) . . ? C26 O11 Cr4 127.4(7) . . ? C26 O12 Cr5 135.4(8) . . ? C31 O13 Cr5 131.4(8) . . ? C31 O14 Ni1 134.7(7) 3_757 . ? C36 O15 Ni1 127.2(6) . . ? C36 O16 Ni2 127.4(6) . . ? C41 O17 Ni1 130.6(7) . . ? C41 O18 Cr5 138.0(8) 3_757 . ? O1 C1 O2 126.0(10) . . ? O1 C1 C2 118.3(10) . . ? O2 C1 C2 115.7(9) . . ? C4 C2 C1 109.8(10) . . ? C4 C2 C5 113.2(12) . . ? C1 C2 C5 111.0(10) . . ? C4 C2 C3 107.0(12) . . ? C1 C2 C3 106.9(11) . . ? C5 C2 C3 108.7(13) . . ? O3 C6 O4 124.5(9) . . ? O3 C6 C7 120.4(10) . . ? O4 C6 C7 115.0(10) . . ? C8 C7 C6 107.7(12) . . ? C8 C7 C10 115.3(14) . . ? C6 C7 C10 109.6(11) . . ? C8 C7 C9 107.2(15) . . ? C6 C7 C9 108.6(11) . . ? C10 C7 C9 108.2(14) . . ? O5 C11 O6 123.5(9) . . ? O5 C11 C12A 123.2(12) . . ? O6 C11 C12A 113.1(11) . . ? O5 C11 C12 122.7(15) . . ? O6 C11 C12 112.7(14) . . ? C12A C11 C12 14.1(12) . . ? C13 C12 C14 109.0(11) . . ? C13 C12 C15 109.1(12) . . ? C14 C12 C15 108.9(11) . . ? C13 C12 C11 109(3) . . ? C14 C12 C11 111(2) . . ? C15 C12 C11 110(3) . . ? C13A C12A C14A 109.1(10) . . ? C13A C12A C15A 109.0(10) . . ? C14A C12A C15A 108.9(10) . . ? C13A C12A C11 105.1(16) . . ? C14A C12A C11 109.7(18) . . ? C15A C12A C11 114.9(17) . . ? O8 C16 O7 125.5(9) . . ? O8 C16 C17 119.0(9) . . ? O7 C16 C17 115.4(10) . . ? C18 C17 C20 116.0(15) . . ? C18 C17 C19 111.2(12) . . ? C20 C17 C19 106.8(12) . . ? C18 C17 C16 109.4(9) . . ? C20 C17 C16 104.5(9) . . ? C19 C17 C16 108.7(10) . . ? O10 C21 O9 126.6(11) . . ? O10 C21 C22A 117.2(12) . . ? O9 C21 C22A 116.0(10) . . ? O10 C21 C22 100.0(14) . . ? O9 C21 C22 132.3(13) . . ? C22A C21 C22 23.7(11) . . ? C23 C22 C25 111.2(10) . . ? C23 C22 C24 111.0(10) . . ? C25 C22 C24 110.9(10) . . ? C23 C22 C21 97(2) . . ? C25 C22 C21 100(2) . . ? C24 C22 C21 125(3) . . ? C21 C22A C23A 112.9(14) . . ? C21 C22A C25A 105.0(15) . . ? C23A C22A C25A 110.7(8) . . ? C21 C22A C24A 106.5(12) . . ? C23A C22A C24A 110.9(8) . . ? C25A C22A C24A 110.6(8) . . ? O12 C26 O11 127.1(10) . . ? O12 C26 C27 117.7(11) . . ? O11 C26 C27 115.1(11) . . ? C30 C27 C28 110.6(9) . . ? C30 C27 C28A 127(2) . . ? C28 C27 C28A 28.4(16) . . ? C30 C27 C29 109.9(9) . . ? C28 C27 C29 109.9(9) . . ? C28A C27 C29 81.9(16) . . ? C30 C27 C29A 71.9(17) . . ? C28 C27 C29A 131(2) . . ? C28A C27 C29A 109.5(10) . . ? C29 C27 C29A 38.5(15) . . ? C30 C27 C30A 37.3(16) . . ? C28 C27 C30A 83.2(17) . . ? C28A C27 C30A 109.5(10) . . ? C29 C27 C30A 146(2) . . ? C29A C27 C30A 108.9(10) . . ? C30 C27 C26 114.6(14) . . ? C28 C27 C26 111.9(15) . . ? C28A C27 C26 113.3(19) . . ? C29 C27 C26 99.5(15) . . ? C29A C27 C26 110.7(19) . . ? C30A C27 C26 105(2) . . ? O14 C31 O13 126.0(10) 3_757 . ? O14 C31 C32 118.8(9) 3_757 . ? O13 C31 C32 115.2(11) . . ? C35A C32 C35 50(2) . . ? C35A C32 C34 143(3) . . ? C35 C32 C34 109.9(11) . . ? C35A C32 C33 64(2) . . ? C35 C32 C33 109.8(11) . . ? C34 C32 C33 109.6(11) . . ? C35A C32 C33A 110.2(8) . . ? C35 C32 C33A 137(4) . . ? C34 C32 C33A 60(2) . . ? C33 C32 C33A 51(2) . . ? C35A C32 C34A 109.7(8) . . ? C35 C32 C34A 61(2) . . ? C34 C32 C34A 52(2) . . ? C33 C32 C34A 144(3) . . ? C33A C32 C34A 109.1(8) . . ? C35A C32 C31 107.4(12) . . ? C35 C32 C31 114(3) . . ? C34 C32 C31 110(3) . . ? C33 C32 C31 104(3) . . ? C33A C32 C31 108.4(13) . . ? C34A C32 C31 112.1(12) . . ? O16 C36 O15 126.8(9) . . ? O16 C36 C37 114.8(8) . . ? O15 C36 C37 118.3(8) . . ? C36 C37 C40 110.6(9) . . ? C36 C37 C38 107.7(11) . . ? C40 C37 C38 115.4(13) . . ? C36 C37 C39 106.9(9) . . ? C40 C37 C39 109.0(12) . . ? C38 C37 C39 106.8(12) . . ? O17 C41 O18 125.5(10) . 3_757 ? O17 C41 C42 119.3(10) . . ? O18 C41 C42 115.1(11) 3_757 . ? C44 C42 C41 108.4(13) . . ? C44 C42 C45 110.1(17) . . ? C41 C42 C45 109.7(12) . . ? C44 C42 C43 113.8(17) . . ? C41 C42 C43 106.2(14) . . ? C45 C42 C43 108.5(14) . . ? C102 N1 C100 107.4(11) . . ? C102 N1 C103 127.8(13) . . ? C100 N1 C103 124.7(13) . . ? N2 C100 N1 108.4(11) . . ? C100 N2 C101 105.3(11) . . ? C102 C101 N2 110.7(13) . . ? C101 C102 N1 107.5(12) . . ? C104 N1A C106 105.1(11) . . ? C104 N1A C107 125.3(13) . . ? C106 N1A C107 128.8(13) . . ? N1A C104 N2A 110.3(13) . . ? C104 N2A C105 104.0(12) . . ? C106 C105 N2A 110.7(13) . . ? C105 C106 N1A 108.7(12) . . ? O50 C150 C152 122(2) . . ? O50 C150 C151 118(2) . . ? C152 C150 C151 119.2(15) . . ? 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 F6 Ni1 Ni2 F5 -178.4(3) . . . . ? O17 Ni1 Ni2 F5 28.2(4) . . . . ? F4 Ni1 Ni2 F5 -154.7(4) . . . . ? O14 Ni1 Ni2 F5 -76.2(3) . . . . ? O15 Ni1 Ni2 F5 105.6(3) . . . . ? F6 Ni1 Ni2 O1 156.7(4) . . . . ? O17 Ni1 Ni2 O1 3.3(4) . . . . ? F5 Ni1 Ni2 O1 -24.9(4) . . . . ? F4 Ni1 Ni2 O1 -179.6(4) . . . . ? O14 Ni1 Ni2 O1 -101.1(4) . . . . ? O15 Ni1 Ni2 O1 80.7(4) . . . . ? F6 Ni1 Ni2 F4 -23.7(3) . . . . ? O17 Ni1 Ni2 F4 -177.0(4) . . . . ? F5 Ni1 Ni2 F4 154.7(4) . . . . ? O14 Ni1 Ni2 F4 78.5(3) . . . . ? O15 Ni1 Ni2 F4 -99.7(3) . . . . ? F6 Ni1 Ni2 F1 3.1(3) . . . . ? O17 Ni1 Ni2 F1 -150.2(4) . . . . ? F5 Ni1 Ni2 F1 -178.5(3) . . . . ? F4 Ni1 Ni2 F1 26.8(3) . . . . ? O14 Ni1 Ni2 F1 105.3(3) . . . . ? O15 Ni1 Ni2 F1 -72.9(3) . . . . ? F6 Ni1 Ni2 O16 78.8(3) . . . . ? O17 Ni1 Ni2 O16 -74.5(4) . . . . ? F5 Ni1 Ni2 O16 -102.7(3) . . . . ? F4 Ni1 Ni2 O16 102.6(3) . . . . ? O14 Ni1 Ni2 O16 -178.9(3) . . . . ? O15 Ni1 Ni2 O16 2.9(3) . . . . ? F6 Ni1 Ni2 O3 -96.9(3) . . . . ? O17 Ni1 Ni2 O3 109.8(4) . . . . ? F5 Ni1 Ni2 O3 81.6(3) . . . . ? F4 Ni1 Ni2 O3 -73.2(3) . . . . ? O14 Ni1 Ni2 O3 5.4(3) . . . . ? O15 Ni1 Ni2 O3 -172.8(3) . . . . ? O2 Cr3 F1 Ni2 -46.1(4) . . . . ? O4 Cr3 F1 Ni2 48.3(3) . . . . ? O7 Cr3 F1 Ni2 81(39) . . . . ? F2 Cr3 F1 Ni2 137.4(3) . . . . ? O5 Cr3 F1 Ni2 -133.7(4) . . . . ? F5 Ni2 F1 Cr3 -173.5(10) . . . . ? O1 Ni2 F1 Cr3 30.6(4) . . . . ? F4 Ni2 F1 Cr3 -151.4(3) . . . . ? O16 Ni2 F1 Cr3 118.7(3) . . . . ? O3 Ni2 F1 Cr3 -61.0(3) . . . . ? Ni1 Ni2 F1 Cr3 -168.67(17) . . . . ? F3 Cr4 F2 Cr3 -131.7(3) . . . . ? O8 Cr4 F2 Cr3 51.9(4) . . . . ? O6 Cr4 F2 Cr3 -42.0(4) . . . . ? O9 Cr4 F2 Cr3 57(9) . . . . ? O11 Cr4 F2 Cr3 139.7(3) . . . . ? F1 Cr3 F2 Cr4 140.6(3) . . . . ? O2 Cr3 F2 Cr4 26(4) . . . . ? O4 Cr3 F2 Cr4 -128.7(3) . . . . ? O7 Cr3 F2 Cr4 -39.8(4) . . . . ? O5 Cr3 F2 Cr4 51.8(3) . . . . ? F2 Cr4 F3 Cr5 -145.7(3) . . . . ? O8 Cr4 F3 Cr5 -52(5) . . . . ? O6 Cr4 F3 Cr5 121.6(4) . . . . ? O9 Cr4 F3 Cr5 34.0(4) . . . . ? O11 Cr4 F3 Cr5 -56.9(3) . . . . ? F6 Cr5 F3 Cr4 131.0(3) 3_757 . . . ? O18 Cr5 F3 Cr4 -25(5) . . . . ? O12 Cr5 F3 Cr4 41.8(4) . . . . ? O13 Cr5 F3 Cr4 -137.9(3) . . . . ? O10 Cr5 F3 Cr4 -51.4(4) . . . . ? F6 Ni1 F4 Ni2 161.7(2) . . . . ? O17 Ni1 F4 Ni2 19(2) . . . . ? F5 Ni1 F4 Ni2 -16.4(2) . . . . ? O14 Ni1 F4 Ni2 -106.9(3) . . . . ? O15 Ni1 F4 Ni2 75.7(2) . . . . ? F5 Ni2 F4 Ni1 16.5(2) . . . . ? O1 Ni2 F4 Ni1 2(3) . . . . ? F1 Ni2 F4 Ni1 -159.0(2) . . . . ? O16 Ni2 F4 Ni1 -73.4(2) . . . . ? O3 Ni2 F4 Ni1 112.3(3) . . . . ? O1 Ni2 F5 Ni1 161.8(3) . . . . ? F4 Ni2 F5 Ni1 -16.6(2) . . . . ? F1 Ni2 F5 Ni1 5.8(12) . . . . ? O16 Ni2 F5 Ni1 73.3(3) . . . . ? O3 Ni2 F5 Ni1 -106.0(3) . . . . ? F6 Ni1 F5 Ni2 6.6(14) . . . . ? O17 Ni1 F5 Ni2 -159.4(3) . . . . ? F4 Ni1 F5 Ni2 16.7(2) . . . . ? O14 Ni1 F5 Ni2 108.6(3) . . . . ? O15 Ni1 F5 Ni2 -71.2(3) . . . . ? O17 Ni1 F6 Cr5 -44.1(4) . . . 3_757 ? F5 Ni1 F6 Cr5 150.0(11) . . . 3_757 ? F4 Ni1 F6 Cr5 140.1(3) . . . 3_757 ? O14 Ni1 F6 Cr5 48.0(3) . . . 3_757 ? O15 Ni1 F6 Cr5 -131.7(3) . . . 3_757 ? Ni2 Ni1 F6 Cr5 155.49(18) . . . 3_757 ? F5 Ni2 O1 C1 -170.8(10) . . . . ? F4 Ni2 O1 C1 -157(2) . . . . ? F1 Ni2 O1 C1 4.3(10) . . . . ? O16 Ni2 O1 C1 -81.0(10) . . . . ? O3 Ni2 O1 C1 93.3(10) . . . . ? Ni1 Ni2 O1 C1 -154.8(9) . . . . ? F1 Cr3 O2 C1 47.3(10) . . . . ? O4 Cr3 O2 C1 -43.6(10) . . . . ? O7 Cr3 O2 C1 -132.3(10) . . . . ? F2 Cr3 O2 C1 162(4) . . . . ? O5 Cr3 O2 C1 135.9(10) . . . . ? F5 Ni2 O3 C6 -149.6(8) . . . . ? O1 Ni2 O3 C6 -55.2(8) . . . . ? F4 Ni2 O3 C6 130.9(8) . . . . ? F1 Ni2 O3 C6 41.5(8) . . . . ? O16 Ni2 O3 C6 38(3) . . . . ? Ni1 Ni2 O3 C6 169.9(8) . . . . ? F1 Cr3 O4 C6 -5.9(10) . . . . ? O2 Cr3 O4 C6 87.7(10) . . . . ? O7 Cr3 O4 C6 174.3(10) . . . . ? F2 Cr3 O4 C6 -94.0(10) . . . . ? O5 Cr3 O4 C6 -80(9) . . . . ? F1 Cr3 O5 C11 -121.3(11) . . . . ? O2 Cr3 O5 C11 145.1(11) . . . . ? O4 Cr3 O5 C11 -47(9) . . . . ? O7 Cr3 O5 C11 58.4(11) . . . . ? F2 Cr3 O5 C11 -33.2(11) . . . . ? F2 Cr4 O6 C11 0.1(10) . . . . ? F3 Cr4 O6 C11 89.1(10) . . . . ? O8 Cr4 O6 C11 -91.3(11) . . . . ? O9 Cr4 O6 C11 -177.8(11) . . . . ? O11 Cr4 O6 C11 129(8) . . . . ? F1 Cr3 O7 C16 54(39) . . . . ? O2 Cr3 O7 C16 -179.3(11) . . . . ? O4 Cr3 O7 C16 86.3(10) . . . . ? F2 Cr3 O7 C16 -2.8(10) . . . . ? O5 Cr3 O7 C16 -91.7(10) . . . . ? F2 Cr4 O8 C16 -33.9(10) . . . . ? F3 Cr4 O8 C16 -127(4) . . . . ? O6 Cr4 O8 C16 58.8(10) . . . . ? O9 Cr4 O8 C16 146.3(11) . . . . ? O11 Cr4 O8 C16 -122.6(10) . . . . ? F2 Cr4 O9 C21 -178(100) . . . . ? F3 Cr4 O9 C21 11.1(12) . . . . ? O8 Cr4 O9 C21 -172.5(12) . . . . ? O6 Cr4 O9 C21 -78.6(12) . . . . ? O11 Cr4 O9 C21 99.7(12) . . . . ? F6 Cr5 O10 C21 143(6) 3_757 . . . ? O18 Cr5 O10 C21 -135.4(12) . . . . ? O12 Cr5 O10 C21 -47.7(12) . . . . ? F3 Cr5 O10 C21 42.9(12) . . . . ? O13 Cr5 O10 C21 131.3(12) . . . . ? F2 Cr4 O11 C26 129.4(9) . . . . ? F3 Cr4 O11 C26 40.4(9) . . . . ? O8 Cr4 O11 C26 -139.3(9) . . . . ? O6 Cr4 O11 C26 0(9) . . . . ? O9 Cr4 O11 C26 -52.7(9) . . . . ? F6 Cr5 O12 C26 -83.0(11) 3_757 . . . ? O18 Cr5 O12 C26 -176.5(11) . . . . ? F3 Cr5 O12 C26 7.1(11) . . . . ? O13 Cr5 O12 C26 24(19) . . . . ? O10 Cr5 O12 C26 97.5(11) . . . . ? F6 Cr5 O13 C31 -38.7(10) 3_757 . . . ? O18 Cr5 O13 C31 54.9(10) . . . . ? O12 Cr5 O13 C31 -146(18) . . . . ? F3 Cr5 O13 C31 -128.7(10) . . . . ? O10 Cr5 O13 C31 140.8(10) . . . . ? F6 Ni1 O14 C31 -20.8(10) . . . 3_757 ? O17 Ni1 O14 C31 74.9(10) . . . 3_757 ? F5 Ni1 O14 C31 169.6(10) . . . 3_757 ? F4 Ni1 O14 C31 -110.6(10) . . . 3_757 ? O15 Ni1 O14 C31 -14(7) . . . 3_757 ? Ni2 Ni1 O14 C31 -151.1(10) . . . 3_757 ? F6 Ni1 O15 C36 -136.1(8) . . . . ? O17 Ni1 O15 C36 128.1(8) . . . . ? F5 Ni1 O15 C36 33.5(8) . . . . ? F4 Ni1 O15 C36 -46.2(8) . . . . ? O14 Ni1 O15 C36 -143(6) . . . . ? Ni2 Ni1 O15 C36 -5.5(7) . . . . ? F5 Ni2 O16 C36 -41.5(8) . . . . ? O1 Ni2 O16 C36 -135.6(8) . . . . ? F4 Ni2 O16 C36 38.1(7) . . . . ? F1 Ni2 O16 C36 127.4(8) . . . . ? O3 Ni2 O16 C36 131(3) . . . . ? Ni1 Ni2 O16 C36 -1.8(7) . . . . ? F6 Ni1 O17 C41 22.3(10) . . . . ? F5 Ni1 O17 C41 -160.3(10) . . . . ? F4 Ni1 O17 C41 165.0(19) . . . . ? O14 Ni1 O17 C41 -69.3(10) . . . . ? O15 Ni1 O17 C41 108.1(10) . . . . ? Ni2 Ni1 O17 C41 -178.3(9) . . . . ? F6 Cr5 O18 C41 10.8(13) 3_757 . . 3_757 ? O12 Cr5 O18 C41 99.8(13) . . . 3_757 ? F3 Cr5 O18 C41 167(4) . . . 3_757 ? O13 Cr5 O18 C41 -80.5(13) . . . 3_757 ? O10 Cr5 O18 C41 -166.8(13) . . . 3_757 ? Ni2 O1 C1 O2 -10.6(18) . . . . ? Ni2 O1 C1 C2 167.7(8) . . . . ? Cr3 O2 C1 O1 -21.8(17) . . . . ? Cr3 O2 C1 C2 159.9(8) . . . . ? O1 C1 C2 C4 -33.4(15) . . . . ? O2 C1 C2 C4 145.1(11) . . . . ? O1 C1 C2 C5 -159.3(13) . . . . ? O2 C1 C2 C5 19.1(16) . . . . ? O1 C1 C2 C3 82.3(13) . . . . ? O2 C1 C2 C3 -99.2(13) . . . . ? Ni2 O3 C6 O4 -11.1(14) . . . . ? Ni2 O3 C6 C7 173.3(7) . . . . ? Cr3 O4 C6 O3 -13.5(17) . . . . ? Cr3 O4 C6 C7 162.3(8) . . . . ? O3 C6 C7 C8 -114.2(14) . . . . ? O4 C6 C7 C8 69.9(16) . . . . ? O3 C6 C7 C10 12.0(16) . . . . ? O4 C6 C7 C10 -164.0(11) . . . . ? O3 C6 C7 C9 130.0(13) . . . . ? O4 C6 C7 C9 -45.9(15) . . . . ? Cr3 O5 C11 O6 2.2(18) . . . . ? Cr3 O5 C11 C12A -173.5(10) . . . . ? Cr3 O5 C11 C12 169.6(14) . . . . ? Cr4 O6 C11 O5 20.4(17) . . . . ? Cr4 O6 C11 C12A -163.5(9) . . . . ? Cr4 O6 C11 C12 -148.2(13) . . . . ? O5 C11 C12 C13 64(2) . . . . ? O6 C11 C12 C13 -127.4(16) . . . . ? C12A C11 C12 C13 -33(5) . . . . ? O5 C11 C12 C14 -56(2) . . . . ? O6 C11 C12 C14 112.3(17) . . . . ? C12A C11 C12 C14 -153(6) . . . . ? O5 C11 C12 C15 -176.8(17) . . . . ? O6 C11 C12 C15 -8.1(19) . . . . ? C12A C11 C12 C15 86(6) . . . . ? O5 C11 C12A C13A 16.1(17) . . . . ? O6 C11 C12A C13A -160.0(12) . . . . ? C12 C11 C12A C13A 109(6) . . . . ? O5 C11 C12A C14A -101.1(15) . . . . ? O6 C11 C12A C14A 82.8(13) . . . . ? C12 C11 C12A C14A -9(5) . . . . ? O5 C11 C12A C15A 135.9(14) . . . . ? O6 C11 C12A C15A -40.2(15) . . . . ? C12 C11 C12A C15A -132(6) . . . . ? Cr4 O8 C16 O7 1.2(17) . . . . ? Cr4 O8 C16 C17 -174.8(7) . . . . ? Cr3 O7 C16 O8 23.1(17) . . . . ? Cr3 O7 C16 C17 -160.7(7) . . . . ? O8 C16 C17 C18 129.2(14) . . . . ? O7 C16 C17 C18 -47.2(16) . . . . ? O8 C16 C17 C20 -106.0(14) . . . . ? O7 C16 C17 C20 77.5(13) . . . . ? O8 C16 C17 C19 7.7(14) . . . . ? O7 C16 C17 C19 -168.8(11) . . . . ? Cr5 O10 C21 O9 -10(2) . . . . ? Cr5 O10 C21 C22A 163.9(9) . . . . ? Cr5 O10 C21 C22 -178.8(13) . . . . ? Cr4 O9 C21 O10 -25(2) . . . . ? Cr4 O9 C21 C22A 160.3(9) . . . . ? Cr4 O9 C21 C22 139.2(17) . . . . ? O10 C21 C22 C23 158.1(14) . . . . ? O9 C21 C22 C23 -9(2) . . . . ? C22A C21 C22 C23 -63(2) . . . . ? O10 C21 C22 C25 -88.8(15) . . . . ? O9 C21 C22 C25 104(2) . . . . ? C22A C21 C22 C25 50(2) . . . . ? O10 C21 C22 C24 35.9(18) . . . . ? O9 C21 C22 C24 -132(2) . . . . ? C22A C21 C22 C24 175(3) . . . . ? O10 C21 C22A C23A 173.4(12) . . . . ? O9 C21 C22A C23A -11.8(15) . . . . ? C22 C21 C22A C23A 127(3) . . . . ? O10 C21 C22A C25A -65.9(15) . . . . ? O9 C21 C22A C25A 108.9(12) . . . . ? C22 C21 C22A C25A -113(3) . . . . ? O10 C21 C22A C24A 51.5(15) . . . . ? O9 C21 C22A C24A -133.7(11) . . . . ? C22 C21 C22A C24A 5(3) . . . . ? Cr5 O12 C26 O11 -25.9(19) . . . . ? Cr5 O12 C26 C27 153.0(8) . . . . ? Cr4 O11 C26 O12 -5.9(18) . . . . ? Cr4 O11 C26 C27 175.2(7) . . . . ? O12 C26 C27 C30 151.2(13) . . . . ? O11 C26 C27 C30 -29.8(16) . . . . ? O12 C26 C27 C28 24.3(16) . . . . ? O11 C26 C27 C28 -156.7(13) . . . . ? O12 C26 C27 C28A -6(2) . . . . ? O11 C26 C27 C28A 172.5(19) . . . . ? O12 C26 C27 C29 -91.7(14) . . . . ? O11 C26 C27 C29 87.3(14) . . . . ? O12 C26 C27 C29A -130(2) . . . . ? O11 C26 C27 C29A 49(2) . . . . ? O12 C26 C27 C30A 113(2) . . . . ? O11 C26 C27 C30A -68(2) . . . . ? Cr5 O13 C31 O14 18.8(18) . . . 3_757 ? Cr5 O13 C31 C32 -164.7(7) . . . . ? O14 C31 C32 C35A -139.8(11) 3_757 . . . ? O13 C31 C32 C35A 43.5(12) . . . . ? O14 C31 C32 C35 -87(3) 3_757 . . . ? O13 C31 C32 C35 97(3) . . . . ? O14 C31 C32 C34 37(3) 3_757 . . . ? O13 C31 C32 C34 -140(3) . . . . ? O14 C31 C32 C33 154(2) 3_757 . . . ? O13 C31 C32 C33 -23(3) . . . . ? O14 C31 C32 C33A 101.2(12) 3_757 . . . ? O13 C31 C32 C33A -75.5(12) . . . . ? O14 C31 C32 C34A -19.3(14) 3_757 . . . ? O13 C31 C32 C34A 164.0(10) . . . . ? Ni2 O16 C36 O15 -1.6(14) . . . . ? Ni2 O16 C36 C37 -177.9(6) . . . . ? Ni1 O15 C36 O16 6.4(14) . . . . ? Ni1 O15 C36 C37 -177.5(6) . . . . ? O16 C36 C37 C40 -27.3(14) . . . . ? O15 C36 C37 C40 156.1(12) . . . . ? O16 C36 C37 C38 -154.2(11) . . . . ? O15 C36 C37 C38 29.1(14) . . . . ? O16 C36 C37 C39 91.3(11) . . . . ? O15 C36 C37 C39 -85.3(12) . . . . ? Ni1 O17 C41 O18 3.0(18) . . . 3_757 ? Ni1 O17 C41 C42 178.9(10) . . . . ? O17 C41 C42 C44 135.6(16) . . . . ? O18 C41 C42 C44 -48(2) 3_757 . . . ? O17 C41 C42 C45 15(2) . . . . ? O18 C41 C42 C45 -168.4(14) 3_757 . . . ? O17 C41 C42 C43 -101.8(15) . . . . ? O18 C41 C42 C43 74.5(15) 3_757 . . . ? C102 N1 C100 N2 5(3) . . . . ? C103 N1 C100 N2 -175.2(19) . . . . ? N1 C100 N2 C101 -8(3) . . . . ? C100 N2 C101 C102 8(3) . . . . ? N2 C101 C102 N1 -5(2) . . . . ? C100 N1 C102 C101 0(3) . . . . ? C103 N1 C102 C101 -179.6(19) . . . . ? C106 N1A C104 N2A -11(3) . . . . ? C107 N1A C104 N2A 179.1(18) . . . . ? N1A C104 N2A C105 7(3) . . . . ? C104 N2A C105 C106 0(3) . . . . ? N2A C105 C106 N1A -7(3) . . . . ? C104 N1A C106 C105 11(3) . . . . ? C107 N1A C106 C105 -180(2) . . . . ? _diffrn_measured_fraction_theta_max .997 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full .997 _refine_diff_density_max 3.571 _refine_diff_density_min -.962 _refine_diff_density_rms .194 data_orepw110absc _database_code_depnum_ccdc_archive 'CCDC 268356' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C97 H182 Cd Cr8 F9 N O37' _chemical_formula_weight 2653.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr .3209 .6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 19.3987(8) _cell_length_b 22.2606(8) _cell_length_c 31.3094(14) _cell_angle_alpha 90.00 _cell_angle_beta 91.663(4) _cell_angle_gamma 90.00 _cell_volume 13514.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12178 _cell_measurement_theta_min 2.6600 _cell_measurement_theta_max 32.0613 _exptl_crystal_description Prismatic _exptl_crystal_colour Green _exptl_crystal_size_max 0.36479 _exptl_crystal_size_mid 0.22327 _exptl_crystal_size_min 0.14855 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5552 _exptl_absorpt_coefficient_mu 0.850 _exptl_absorpt_correction_T_min 0.54158 _exptl_absorpt_correction_T_max 0.79958 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_process_details ? _exptl_special_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.pre23_9 beta (release 18.06.2004 CrysAlis171 .NET) (compiled Jun 18 2004,12:34:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66991 _diffrn_reflns_av_R_equivalents 0.0822 _diffrn_reflns_av_sigmaI/netI 0.0749 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 23.26 _reflns_number_total 19356 _reflns_number_gt 12668 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Due to poor data quality and insufficient data to parameters. Disordered methly groups left isotopic. Hydrogens were not placed due to poor data. 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^)+(0.1877P)^2^+125.8955P] 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 SHELXL _refine_ls_extinction_coef 0.0008(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 19356 _refine_ls_number_parameters 1355 _refine_ls_number_restraints 1173 _refine_ls_R_factor_all 0.1590 _refine_ls_R_factor_gt 0.1228 _refine_ls_wR_factor_ref 0.3504 _refine_ls_wR_factor_gt 0.3179 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.023 _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 Cd9 Cd 0.21123(4) 0.78669(4) 0.02031(3) 0.0557(3) Uani 1 1 d . . . Cr1 Cr 0.14673(8) 0.87855(7) 0.10210(6) 0.0392(4) Uani 1 1 d . . . Cr2 Cr 0.37246(10) 0.75071(8) -0.02355(5) 0.0463(5) Uani 1 1 d . . . Cr3 Cr 0.53974(9) 0.71830(8) 0.00219(5) 0.0424(5) Uani 1 1 d . . . Cr4 Cr 0.63174(8) 0.73089(8) 0.09500(5) 0.0406(5) Uani 1 1 d . . . Cr5 Cr 0.62676(8) 0.81453(8) 0.18401(5) 0.0421(5) Uani 1 1 d . . . Cr6 Cr 0.51193(9) 0.86721(8) 0.25378(5) 0.0421(5) Uani 1 1 d . J . Cr7 Cr 0.34879(10) 0.91935(14) 0.25923(7) 0.0832(9) Uani 1 1 d D . . Cr8 Cr 0.19990(9) 0.91527(10) 0.20318(6) 0.0534(6) Uani 1 1 d . . . F1 F 0.2050(3) 0.8674(2) 0.15311(18) 0.0397(13) Uani 1 1 d . L . F2 F 0.2243(3) 0.8584(3) 0.07040(19) 0.0445(14) Uani 1 1 d . . . F3 F 0.3285(3) 0.7822(3) 0.02453(19) 0.0487(15) Uani 1 1 d . . . F4 F 0.4445(3) 0.7210(2) 0.01512(17) 0.0390(13) Uani 1 1 d . . . F5 F 0.5628(3) 0.7599(2) 0.05451(16) 0.0332(12) Uani 1 1 d . . . F6 F 0.5818(3) 0.7634(2) 0.14188(16) 0.0362(13) Uani 1 1 d . . . F7 F 0.5410(3) 0.8550(3) 0.19565(17) 0.0395(13) Uani 1 1 d . . . F8 F 0.4152(3) 0.8641(3) 0.23670(17) 0.0471(15) Uani 1 1 d . J . F9 F 0.2985(3) 0.9196(2) 0.20684(17) 0.0388(13) Uani 1 1 d . L . O1 O 0.1134(4) 0.7969(3) 0.1077(3) 0.0491(19) Uani 1 1 d . A . O2 O 0.1865(5) 0.7327(4) 0.0789(3) 0.067(2) Uani 1 1 d . A . O3 O 0.0891(4) 0.8927(3) 0.0517(3) 0.054(2) Uani 1 1 d . . . O4 O 0.1007(4) 0.8104(4) 0.0112(3) 0.068(3) Uani 1 1 d . . . O5 O 0.2141(5) 0.7001(4) -0.0152(3) 0.071(3) Uani 1 1 d . B . O6 O 0.3257(4) 0.6744(4) -0.0190(3) 0.054(2) Uani 1 1 d . B . O7 O 0.2332(4) 0.8422(4) -0.0379(3) 0.059(2) Uani 1 1 d . C . O8 O 0.3089(4) 0.7804(4) -0.0669(2) 0.056(2) Uani 1 1 d . C . O9 O 0.4256(4) 0.8263(3) -0.0291(2) 0.0460(18) Uani 1 1 d . D . O10 O 0.5360(4) 0.7951(3) -0.0278(2) 0.0440(18) Uani 1 1 d . D . O11 O 0.4225(5) 0.7180(4) -0.0733(2) 0.056(2) Uani 1 1 d . E . O12 O 0.5204(4) 0.6765(4) -0.0510(2) 0.055(2) Uani 1 1 d . E . O13 O 0.5466(4) 0.6405(3) 0.0314(2) 0.0466(18) Uani 1 1 d . . . O14 O 0.5808(4) 0.6565(3) 0.0997(2) 0.0433(17) Uani 1 1 d . . . O15 O 0.6372(4) 0.7157(4) -0.0123(3) 0.055(2) Uani 1 1 d . F . O16 O 0.6893(4) 0.6984(3) 0.0510(3) 0.0489(19) Uani 1 1 d . F . O17 O 0.6818(3) 0.8059(4) 0.0885(2) 0.0437(18) Uani 1 1 d . H . O18 O 0.6481(3) 0.8705(3) 0.1384(2) 0.0421(17) Uani 1 1 d . H . O19 O 0.7006(4) 0.6977(4) 0.1349(3) 0.052(2) Uani 1 1 d . I . O20 O 0.7152(4) 0.7750(4) 0.1796(3) 0.053(2) Uani 1 1 d . I . O21 O 0.6770(4) 0.8680(4) 0.2218(2) 0.054(2) Uani 1 1 d . J . O22 O 0.6066(4) 0.8776(4) 0.2760(2) 0.057(2) Uani 1 1 d . J . O23 O 0.6067(4) 0.7542(3) 0.2278(2) 0.0499(19) Uani 1 1 d . K . O24 O 0.5109(4) 0.7796(4) 0.2613(2) 0.054(2) Uani 1 1 d . J . O33 O 0.1963(6) 0.9866(4) 0.1683(3) 0.091(4) Uani 1 1 d . L . O34 O 0.1764(4) 0.9640(3) 0.1007(2) 0.0414(17) Uani 1 1 d . L . O35 O 0.1007(5) 0.9070(8) 0.2019(3) 0.127(6) Uani 1 1 d . L . O36 O 0.0661(3) 0.9027(3) 0.1358(3) 0.0486(19) Uani 1 1 d . L . C1 C 0.1353(7) 0.7459(5) 0.0994(5) 0.067(4) Uani 1 1 d U . . C2 C 0.0955(13) 0.6960(11) 0.1272(8) 0.071(7) Uiso 0.50 1 d PDU A 1 C3 C 0.070(2) 0.718(2) 0.1697(11) 0.131(15) Uiso 0.50 1 d PDU A 1 C4 C 0.035(2) 0.680(2) 0.0980(14) 0.17(2) Uiso 0.50 1 d PDU A 1 C5 C 0.1411(15) 0.6416(13) 0.1339(10) 0.085(9) Uiso 0.50 1 d PDU A 1 C2A C 0.0773(15) 0.6964(13) 0.1023(9) 0.090(9) Uiso 0.50 1 d PDU A 2 C3A C 0.0488(19) 0.7017(17) 0.1467(10) 0.109(12) Uiso 0.50 1 d PDU A 2 C4A C 0.020(2) 0.707(2) 0.0693(12) 0.18(2) Uiso 0.50 1 d PDU A 2 C5A C 0.107(3) 0.6342(19) 0.0962(14) 0.158(18) Uiso 0.50 1 d PDU A 2 C6 C 0.0690(6) 0.8572(6) 0.0225(4) 0.056(3) Uani 1 1 d U . . C7 C 0.0037(7) 0.8746(7) -0.0031(5) 0.075(3) Uani 1 1 d U . . C8 C 0.0214(9) 0.9293(8) -0.0321(5) 0.088(4) Uani 1 1 d U . . C9 C -0.0504(7) 0.8941(9) 0.0291(6) 0.095(5) Uani 1 1 d U . . C10 C -0.0210(9) 0.8227(8) -0.0317(7) 0.113(6) Uani 1 1 d U . . C11 C 0.2630(7) 0.6643(6) -0.0185(4) 0.064(4) Uani 1 1 d U . . C12 C 0.2405(10) 0.5922(10) -0.0167(7) 0.052(6) Uiso 0.50 1 d PDU B 1 C13 C 0.2530(17) 0.577(2) -0.0642(8) 0.123(14) Uiso 0.50 1 d PDU B 1 C14 C 0.1643(12) 0.5808(18) -0.0059(11) 0.108(12) Uiso 0.50 1 d PDU B 1 C15 C 0.2898(14) 0.5559(15) 0.0131(8) 0.085(9) Uiso 0.50 1 d PDU B 1 C12A C 0.2440(11) 0.6004(12) -0.0286(7) 0.080(10) Uiso 0.50 1 d PDU B 2 C13A C 0.2910(16) 0.5693(19) -0.0612(10) 0.110(12) Uiso 0.50 1 d PDU B 2 C14A C 0.1674(12) 0.5967(15) -0.0438(9) 0.084(9) Uiso 0.50 1 d PDU B 2 C15A C 0.2541(17) 0.572(2) 0.0163(9) 0.115(13) Uiso 0.50 1 d PDU B 2 C16 C 0.2601(7) 0.8181(6) -0.0689(4) 0.062(3) Uani 1 1 d U . . C17 C 0.2399(9) 0.8353(7) -0.1171(6) 0.048(5) Uiso 0.60 1 d PDU C 1 C18 C 0.1810(14) 0.8815(9) -0.1157(16) 0.081(16) Uiso 0.60 1 d PDU C 1 C19 C 0.2136(10) 0.7754(8) -0.1360(7) 0.064(6) Uiso 0.60 1 d PDU C 1 C20 C 0.3002(11) 0.8597(10) -0.1428(8) 0.079(7) Uiso 0.60 1 d PDU C 1 C17A C 0.2218(15) 0.8219(13) -0.1102(10) 0.072(9) Uiso 0.40 1 d PDU C 2 C18A C 0.189(2) 0.8846(13) -0.115(2) 0.08(2) Uiso 0.40 1 d PDU C 2 C19A C 0.1666(18) 0.7725(15) -0.1146(14) 0.092(12) Uiso 0.40 1 d PDU C 2 C20A C 0.2784(18) 0.8126(17) -0.1431(13) 0.101(13) Uiso 0.40 1 d PDU C 2 C21 C 0.4895(6) 0.8323(5) -0.0365(3) 0.043(3) Uani 1 1 d U . . C22 C 0.5200(10) 0.8923(8) -0.0552(5) 0.039(6) Uiso 0.50 1 d PDU D 1 C23 C 0.5809(13) 0.9177(15) -0.0279(9) 0.105(11) Uiso 0.50 1 d PDU D 1 C24 C 0.4604(12) 0.9381(12) -0.0590(8) 0.075(8) Uiso 0.50 1 d PDU D 1 C25 C 0.5438(15) 0.8726(15) -0.0998(8) 0.100(11) Uiso 0.50 1 d PDU D 1 C22A C 0.5020(9) 0.8901(8) -0.0609(5) 0.052(7) Uiso 0.50 1 d PDU D 2 C23A C 0.4941(11) 0.9412(10) -0.0279(7) 0.060(6) Uiso 0.50 1 d PDU D 2 C24A C 0.4508(11) 0.8987(12) -0.0992(7) 0.068(7) Uiso 0.50 1 d PDU D 2 C25A C 0.5771(10) 0.8863(11) -0.0762(7) 0.060(6) Uiso 0.50 1 d PDU D 2 C26 C 0.4747(7) 0.6881(5) -0.0799(4) 0.050(3) Uani 1 1 d U . . C27 C 0.4944(11) 0.6699(8) -0.1241(6) 0.052(7) Uiso 0.50 1 d PDU E 1 C28 C 0.5126(12) 0.7281(9) -0.1485(7) 0.053(6) Uiso 0.50 1 d PDU E 1 C29 C 0.4279(12) 0.6415(11) -0.1441(8) 0.056(7) Uiso 0.50 1 d PDU E 1 C30 C 0.5543(13) 0.6238(13) -0.1240(13) 0.059(13) Uiso 0.50 1 d PDU E 1 C27A C 0.4773(10) 0.6634(8) -0.1248(6) 0.052(7) Uiso 0.50 1 d PDU E 2 C28A C 0.4758(12) 0.7187(9) -0.1550(8) 0.056(6) Uiso 0.50 1 d PDU E 2 C29A C 0.4142(12) 0.6224(12) -0.1345(11) 0.079(10) Uiso 0.50 1 d PDU E 2 C30A C 0.5451(11) 0.6275(11) -0.1303(11) 0.039(9) Uiso 0.50 1 d PDU E 2 C31 C 0.6880(7) 0.7019(5) 0.0109(4) 0.054(3) Uani 1 1 d U . . C32 C 0.7593(14) 0.6927(12) -0.0083(9) 0.090(11) Uiso 0.50 1 d PDU F 1 C33 C 0.763(3) 0.7298(17) -0.0501(12) 0.127(18) Uiso 0.50 1 d PDU F 1 C34 C 0.753(2) 0.6244(14) -0.0181(13) 0.137(15) Uiso 0.50 1 d PDU F 1 C35 C 0.8221(15) 0.7056(13) 0.0222(9) 0.077(8) Uiso 0.50 1 d PDU F 1 C32A C 0.7510(12) 0.6862(9) -0.0147(7) 0.068(9) Uiso 0.50 1 d PDU F 2 C33A C 0.7697(16) 0.7446(11) -0.0390(9) 0.063(8) Uiso 0.50 1 d PDU F 2 C34A C 0.7330(19) 0.6343(12) -0.0462(10) 0.110(12) Uiso 0.50 1 d PDU F 2 C35A C 0.8102(15) 0.6679(13) 0.0172(9) 0.082(9) Uiso 0.50 1 d PDU F 2 C36 C 0.5544(6) 0.6242(5) 0.0702(4) 0.044(3) Uani 1 1 d U . . C37 C 0.5277(7) 0.5634(5) 0.0804(4) 0.055(3) Uani 1 1 d U . . C38 C 0.5620(8) 0.5185(6) 0.0490(5) 0.074(4) Uani 1 1 d U . . C39 C 0.4486(8) 0.5646(8) 0.0714(7) 0.103(5) Uani 1 1 d U . . C40 C 0.5489(11) 0.5458(6) 0.1278(5) 0.097(5) Uani 1 1 d U . . C41 C 0.6784(5) 0.8573(6) 0.1038(4) 0.045(3) Uani 1 1 d U . . C42 C 0.767(3) 0.934(2) 0.1011(14) 0.11(2) Uiso 0.20 1 d PDU G 1 C43 C 0.832(3) 0.975(4) 0.107(3) 0.17(4) Uiso 0.20 1 d PDU G 1 C44 C 0.700(3) 0.972(3) 0.103(2) 0.080(19) Uiso 0.20 1 d PDU G 1 C45 C 0.771(2) 0.8988(19) 0.0585(14) 0.031(10) Uiso 0.20 1 d PDU G 1 C42A C 0.7149(6) 0.9088(5) 0.0823(3) 0.043(3) Uiso 0.80 1 d PDU H 2 C43A C 0.7778(10) 0.9218(11) 0.1130(7) 0.116(9) Uiso 0.80 1 d PDU H 2 C44A C 0.6673(9) 0.9643(8) 0.0788(5) 0.076(5) Uiso 0.80 1 d PDU H 2 C45A C 0.7402(10) 0.8892(9) 0.0379(5) 0.091(6) Uiso 0.80 1 d PDU H 2 C46 C 0.7327(6) 0.7244(7) 0.1645(5) 0.058(3) Uani 1 1 d U . . C47 C 0.7992(14) 0.7007(10) 0.1875(7) 0.077(11) Uiso 0.50 1 d PDU I 1 C48 C 0.8277(14) 0.7377(11) 0.2252(7) 0.062(7) Uiso 0.50 1 d PDU I 1 C49 C 0.851(2) 0.6978(16) 0.1515(9) 0.097(13) Uiso 0.50 1 d PDU I 1 C50 C 0.7788(15) 0.6376(11) 0.2021(9) 0.074(8) Uiso 0.50 1 d PDU I 1 C47A C 0.7984(12) 0.6928(11) 0.1810(7) 0.061(8) Uiso 0.50 1 d PDU I 2 C48A C 0.806(2) 0.7094(17) 0.2284(9) 0.124(14) Uiso 0.50 1 d PDU I 2 C49A C 0.8580(19) 0.7185(16) 0.1557(10) 0.090(11) Uiso 0.50 1 d PDU I 2 C50A C 0.793(2) 0.6247(13) 0.1753(12) 0.120(13) Uiso 0.50 1 d PDU I 2 C51 C 0.6640(6) 0.8848(6) 0.2572(5) 0.060(3) Uani 1 1 d U . . C52 C 0.7114(16) 0.9127(14) 0.2952(10) 0.073(10) Uiso 0.35 1 d PDU J 1 C53 C 0.684(3) 0.9713(18) 0.3149(15) 0.089(15) Uiso 0.35 1 d PDU J 1 C54 C 0.774(2) 0.925(2) 0.2670(15) 0.114(16) Uiso 0.35 1 d PDU J 1 C55 C 0.728(2) 0.8653(16) 0.3299(13) 0.084(12) Uiso 0.35 1 d PDU J 1 C52A C 0.7192(8) 0.9237(7) 0.2820(5) 0.052(5) Uiso 0.65 1 d PDU J 2 C53A C 0.6877(19) 0.9526(13) 0.3219(9) 0.121(13) Uiso 0.65 1 d PDU J 2 C54A C 0.7483(11) 0.9721(9) 0.2521(7) 0.076(6) Uiso 0.65 1 d PDU J 2 C55A C 0.7743(15) 0.8765(12) 0.2947(9) 0.123(10) Uiso 0.65 1 d PDU J 2 C56 C 0.5542(6) 0.7435(6) 0.2495(4) 0.050(3) Uani 1 1 d U . . C57 C 0.5394(9) 0.6812(11) 0.2662(5) 0.043(7) Uiso 0.50 1 d PDU K 1 C58 C 0.6018(13) 0.640(2) 0.2564(9) 0.065(13) Uiso 0.50 1 d PDU K 1 C59 C 0.4736(11) 0.6596(12) 0.2414(7) 0.063(7) Uiso 0.50 1 d PDU K 1 C60 C 0.5273(11) 0.6837(11) 0.3149(6) 0.047(6) Uiso 0.50 1 d PDU K 1 C57A C 0.5426(10) 0.6737(12) 0.2579(7) 0.053(8) Uiso 0.50 1 d PDU K 2 C58A C 0.6127(15) 0.640(3) 0.2587(12) 0.10(2) Uiso 0.50 1 d PDU K 2 C59A C 0.4952(14) 0.6517(15) 0.2204(8) 0.083(9) Uiso 0.50 1 d PDU K 2 C60A C 0.5064(15) 0.6669(15) 0.3011(8) 0.075(8) Uiso 0.50 1 d PDU K 2 O25 O 0.4893(5) 0.8734(4) 0.3139(2) 0.058(2) Uani 1 1 d DU . . O26 O 0.3952(5) 0.9365(6) 0.3150(3) 0.043(3) Uani 0.60 1 d PDU L 1 C61 C 0.4437(6) 0.9053(7) 0.3314(4) 0.043(4) Uani 0.60 1 d PDU L 1 C62 C 0.4464(8) 0.9140(7) 0.3800(5) 0.054(5) Uiso 0.60 1 d PDU L 1 C63 C 0.3883(11) 0.9509(10) 0.3976(8) 0.077(7) Uiso 0.60 1 d PDU L 1 C64 C 0.5142(11) 0.9443(11) 0.3910(9) 0.097(9) Uiso 0.60 1 d PDU L 1 C65 C 0.4455(14) 0.8524(11) 0.4005(13) 0.136(13) Uiso 0.60 1 d PDU L 1 O26A O 0.3792(11) 0.8783(11) 0.3139(5) 0.078(6) Uani 0.40 1 d PDU L 2 C61A C 0.4350(7) 0.869(2) 0.3347(7) 0.077(7) Uani 0.40 1 d PDU L 2 C62A C 0.4577(15) 0.8604(14) 0.3817(8) 0.102(12) Uiso 0.40 1 d PDU L 2 C63A C 0.4101(17) 0.9013(18) 0.4056(13) 0.097(12) Uiso 0.40 1 d PDU L 2 C64A C 0.5294(15) 0.8646(17) 0.4014(12) 0.083(11) Uiso 0.40 1 d PDU L 2 C65A C 0.432(2) 0.7966(16) 0.385(2) 0.18(3) Uiso 0.40 1 d PDU L 2 O27 O 0.5108(4) 0.9536(4) 0.2447(2) 0.0481(18) Uani 1 1 d U . . O28 O 0.4044(4) 0.9884(4) 0.2388(4) 0.103(4) Uani 1 1 d DU L . C66 C 0.4666(6) 0.9936(5) 0.2407(4) 0.057(3) Uani 1 1 d DU L . C67 C 0.4951(6) 1.0565(5) 0.2316(3) 0.049(3) Uiso 0.85 1 d PDU L 1 C68 C 0.5093(9) 1.0821(10) 0.2772(5) 0.102(7) Uiso 0.85 1 d PDU L 1 C69 C 0.4435(9) 1.0983(9) 0.2071(5) 0.090(6) Uiso 0.85 1 d PDU L 1 C70 C 0.5637(9) 1.0541(10) 0.2075(5) 0.092(6) Uiso 0.85 1 d PDU L 1 C67A C 0.473(3) 1.0621(6) 0.2414(15) 0.056(14) Uiso 0.15 1 d PDU L 2 C68A C 0.479(4) 1.110(3) 0.2773(19) 0.07(2) Uiso 0.15 1 d PDU L 2 C69A C 0.405(3) 1.072(3) 0.2150(19) 0.043(16) Uiso 0.15 1 d PDU L 2 C70A C 0.535(3) 1.066(3) 0.212(2) 0.06(2) Uiso 0.15 1 d PDU L 2 O29 O 0.2957(4) 0.8549(6) 0.2786(3) 0.094(4) Uani 1 1 d U L . O30 O 0.2043(5) 0.8424(5) 0.2391(3) 0.073(3) Uani 1 1 d U L . C71 C 0.2453(8) 0.8250(5) 0.2663(4) 0.058(3) Uani 1 1 d U . . C72 C 0.2383(11) 0.7669(11) 0.2895(7) 0.081(10) Uiso 0.60 1 d PDU L 1 C73 C 0.1942(15) 0.7205(17) 0.2649(10) 0.133(13) Uiso 0.60 1 d PDU L 1 C74 C 0.3124(12) 0.7425(16) 0.2959(10) 0.106(10) Uiso 0.60 1 d PDU L 1 C75 C 0.2074(12) 0.7789(11) 0.3333(7) 0.075(7) Uiso 0.60 1 d PDU L 1 C72A C 0.2437(13) 0.7721(12) 0.2947(8) 0.056(10) Uiso 0.40 1 d PDU L 2 C73A C 0.1713(16) 0.753(2) 0.2790(12) 0.096(13) Uiso 0.40 1 d PDU L 2 C74A C 0.2963(18) 0.723(2) 0.2832(14) 0.109(16) Uiso 0.40 1 d PDU L 2 C75A C 0.2447(19) 0.7815(18) 0.3433(9) 0.081(11) Uiso 0.40 1 d PDU L 2 O32 O 0.1887(5) 0.9622(5) 0.2538(3) 0.083(3) Uani 1 1 d DU L . O31 O 0.2876(5) 0.9870(4) 0.2775(4) 0.059(3) Uani 0.70 1 d PDU L 1 C76 C 0.2260(6) 0.9915(7) 0.2769(6) 0.056(5) Uani 0.70 1 d PDU L 1 C77 C 0.1874(7) 1.0327(6) 0.3074(4) 0.058(4) Uiso 0.70 1 d PDU L 1 C78 C 0.2043(10) 1.0966(9) 0.2906(6) 0.083(6) Uiso 0.70 1 d PDU L 1 C79 C 0.2188(9) 1.0236(9) 0.3533(6) 0.071(5) Uiso 0.70 1 d PDU L 1 C80 C 0.1079(9) 1.0224(9) 0.3069(6) 0.080(6) Uiso 0.70 1 d PDU L 1 O31A O 0.2758(9) 0.9478(11) 0.2973(5) 0.039(5) Uani 0.30 1 d PDU L 2 C76A C 0.2277(16) 0.9771(17) 0.2830(10) 0.041(7) Uani 0.30 1 d PDU L 2 C77A C 0.2161(17) 1.0224(12) 0.3193(8) 0.048(8) Uiso 0.30 1 d PDU L 2 C78A C 0.143(2) 1.049(3) 0.3089(19) 0.13(2) Uiso 0.30 1 d PDU L 2 C79A C 0.270(3) 1.074(2) 0.322(2) 0.14(2) Uiso 0.30 1 d PDU L 2 C80A C 0.216(3) 0.987(2) 0.3622(13) 0.095(16) Uiso 0.30 1 d PDU L 2 C81 C 0.1915(5) 1.0001(5) 0.1296(3) 0.039(2) Uani 1 1 d U . . C82 C 0.2027(6) 1.0644(5) 0.1180(4) 0.050(2) Uani 1 1 d U L . C83 C 0.1383(7) 1.1002(6) 0.1341(5) 0.071(4) Uani 1 1 d U . . C84 C 0.2067(8) 1.0723(6) 0.0690(4) 0.069(3) Uani 1 1 d U . . C85 C 0.2673(8) 1.0868(7) 0.1415(6) 0.085(5) Uani 1 1 d U . . C86 C 0.0556(6) 0.9098(7) 0.1744(4) 0.060(3) Uani 1 1 d U . . C87 C -0.0151(11) 0.9305(8) 0.1880(5) 0.068(8) Uiso 0.55 1 d PDU L 1 C88 C -0.0448(13) 0.9778(9) 0.1560(7) 0.062(7) Uiso 0.55 1 d PDU L 1 C89 C -0.0151(13) 0.9542(11) 0.2346(6) 0.071(7) Uiso 0.55 1 d PDU L 1 C90 C -0.0551(15) 0.8701(10) 0.1839(8) 0.084(8) Uiso 0.55 1 d PDU L 1 C87A C -0.0212(10) 0.9120(9) 0.1850(6) 0.039(6) Uiso 0.45 1 d PD L 2 C88A C -0.044(2) 0.9770(10) 0.1730(10) 0.081(11) Uiso 0.45 1 d PD L 2 C89A C -0.026(2) 0.9013(15) 0.2339(7) 0.096(11) Uiso 0.45 1 d PD L 2 C90A C -0.0646(17) 0.8650(12) 0.1592(9) 0.076(9) Uiso 0.45 1 d PD L 2 N1 N 0.3594(4) 0.8322(5) 0.1018(3) 0.049(2) Uani 1 1 d . . . C100 C 0.3879(6) 0.7891(6) 0.1364(3) 0.052(3) Uani 1 1 d . . . C101 C 0.4150(7) 0.7357(6) 0.1161(4) 0.063(4) Uani 1 1 d . . . C102 C 0.3298(6) 0.7741(5) 0.1667(4) 0.053(3) Uani 1 1 d . . . C103 C 0.4024(6) 0.8900(5) 0.0945(4) 0.051(3) Uani 1 1 d . . . C104 C 0.4738(5) 0.8712(5) 0.0826(4) 0.049(3) Uani 1 1 d . . . C105 C 0.4046(7) 0.9294(5) 0.1344(4) 0.057(3) Uani 1 1 d . . . C106 C 0.3637(7) 0.9237(5) 0.0573(4) 0.054(3) Uani 1 1 d . . . O50 O 0.2061(8) 0.9626(6) 0.9916(4) 0.125(5) 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 Cd9 0.0459(5) 0.0519(6) 0.0686(6) -0.0154(4) -0.0080(4) 0.0065(4) Cr1 0.0241(8) 0.0346(9) 0.0587(11) -0.0032(8) -0.0038(7) 0.0008(7) Cr2 0.0559(11) 0.0463(11) 0.0364(10) -0.0113(8) -0.0059(8) 0.0007(9) Cr3 0.0491(11) 0.0390(10) 0.0399(10) -0.0007(7) 0.0119(8) 0.0066(8) Cr4 0.0299(9) 0.0436(10) 0.0488(10) 0.0115(8) 0.0103(7) 0.0041(7) Cr5 0.0274(9) 0.0547(11) 0.0439(10) 0.0106(8) -0.0048(7) -0.0065(8) Cr6 0.0383(10) 0.0535(11) 0.0340(9) 0.0083(8) -0.0053(7) -0.0085(8) Cr7 0.0273(10) 0.174(3) 0.0488(12) -0.0454(14) 0.0093(9) -0.0142(13) Cr8 0.0404(10) 0.0809(14) 0.0391(10) 0.0102(9) 0.0068(8) 0.0292(10) F1 0.029(3) 0.043(3) 0.048(3) 0.003(3) -0.004(2) 0.007(2) F2 0.036(3) 0.043(4) 0.054(4) -0.006(3) 0.001(3) 0.004(3) F3 0.050(4) 0.048(4) 0.048(4) -0.013(3) -0.003(3) 0.004(3) F4 0.039(3) 0.042(3) 0.036(3) -0.005(2) 0.003(2) -0.003(3) F5 0.032(3) 0.030(3) 0.038(3) 0.001(2) 0.008(2) 0.004(2) F6 0.029(3) 0.043(3) 0.037(3) 0.005(2) 0.003(2) -0.002(2) F7 0.030(3) 0.053(4) 0.036(3) 0.011(3) 0.002(2) -0.008(3) F8 0.034(3) 0.071(4) 0.036(3) 0.003(3) 0.000(2) -0.018(3) F9 0.032(3) 0.043(3) 0.042(3) -0.002(3) 0.013(2) -0.007(2) O1 0.036(4) 0.039(5) 0.072(5) -0.006(4) 0.003(4) -0.008(3) O2 0.073(6) 0.046(5) 0.083(6) -0.006(4) 0.016(5) 0.016(4) O3 0.039(4) 0.044(5) 0.077(6) -0.010(4) -0.021(4) 0.005(3) O4 0.043(5) 0.062(6) 0.098(7) -0.034(5) -0.016(4) 0.006(4) O5 0.051(5) 0.083(7) 0.079(6) -0.035(5) -0.012(4) 0.001(5) O6 0.038(5) 0.059(5) 0.063(5) -0.019(4) -0.006(4) 0.000(4) O7 0.060(5) 0.052(5) 0.065(5) -0.019(4) -0.009(4) 0.012(4) O8 0.058(5) 0.067(6) 0.044(4) -0.020(4) -0.012(4) 0.013(4) O9 0.060(5) 0.034(4) 0.044(4) 0.000(3) -0.001(4) 0.006(4) O10 0.053(5) 0.046(4) 0.034(4) 0.009(3) 0.017(3) 0.009(4) O11 0.071(6) 0.068(6) 0.030(4) -0.012(4) 0.001(4) 0.007(5) O12 0.075(6) 0.052(5) 0.039(4) -0.009(4) 0.016(4) -0.002(4) O13 0.056(5) 0.039(4) 0.046(5) 0.001(3) 0.014(4) 0.006(3) O14 0.043(4) 0.039(4) 0.049(4) 0.011(4) 0.008(3) 0.003(3) O15 0.059(5) 0.055(5) 0.052(5) 0.000(4) 0.026(4) 0.015(4) O16 0.039(4) 0.050(5) 0.058(5) 0.009(4) 0.017(4) 0.011(3) O17 0.029(4) 0.049(5) 0.053(5) 0.012(4) 0.007(3) -0.005(3) O18 0.028(4) 0.050(5) 0.049(4) 0.009(3) 0.001(3) -0.011(3) O19 0.038(4) 0.059(5) 0.059(5) 0.014(4) -0.001(4) 0.010(4) O20 0.028(4) 0.059(6) 0.070(5) 0.022(4) -0.006(4) 0.001(4) O21 0.041(4) 0.084(6) 0.037(5) -0.002(4) -0.004(3) -0.012(4) O22 0.051(5) 0.072(6) 0.046(5) 0.007(4) -0.024(4) -0.004(4) O23 0.040(4) 0.053(5) 0.056(5) 0.012(4) -0.011(4) -0.007(4) O24 0.052(5) 0.062(5) 0.047(5) 0.020(4) 0.006(4) 0.000(4) O33 0.169(11) 0.052(6) 0.049(6) -0.010(4) -0.036(6) 0.056(6) O34 0.047(4) 0.034(4) 0.043(4) 0.003(3) -0.004(3) -0.008(3) O35 0.032(5) 0.282(19) 0.067(7) -0.010(9) 0.006(5) 0.044(8) O36 0.024(4) 0.040(4) 0.081(6) -0.010(4) 0.002(4) 0.006(3) C1 0.063(8) 0.030(7) 0.107(10) -0.006(7) 0.007(8) -0.003(6) C6 0.028(5) 0.057(8) 0.083(8) -0.017(6) -0.009(5) -0.005(5) C7 0.057(7) 0.069(8) 0.098(10) -0.010(6) -0.024(6) 0.000(6) C8 0.085(11) 0.089(9) 0.089(10) 0.006(7) -0.003(7) 0.007(8) C9 0.040(7) 0.146(15) 0.100(10) 0.021(9) -0.007(6) 0.013(8) C10 0.079(11) 0.093(10) 0.160(16) -0.029(10) -0.082(10) -0.003(9) C11 0.057(8) 0.061(8) 0.074(9) -0.037(7) -0.011(6) 0.003(7) C16 0.069(8) 0.053(7) 0.064(8) -0.031(6) -0.020(6) 0.017(7) C21 0.054(7) 0.047(7) 0.028(5) 0.006(5) 0.008(5) -0.004(6) C26 0.067(8) 0.037(6) 0.046(7) 0.002(5) -0.003(6) 0.003(6) C31 0.057(8) 0.042(7) 0.065(8) 0.016(6) 0.024(6) 0.013(6) C36 0.050(6) 0.030(5) 0.052(7) 0.003(5) 0.022(5) 0.006(4) C37 0.073(7) 0.033(6) 0.060(6) 0.003(5) 0.014(6) 0.002(5) C38 0.094(9) 0.039(6) 0.090(9) -0.019(6) 0.023(8) -0.003(7) C39 0.055(6) 0.077(11) 0.177(17) 0.028(11) 0.028(8) -0.010(6) C40 0.186(16) 0.047(8) 0.059(7) 0.018(6) 0.005(8) -0.022(10) C41 0.026(5) 0.061(8) 0.048(7) 0.022(6) -0.003(5) -0.002(5) C46 0.027(6) 0.065(9) 0.082(9) 0.038(7) 0.008(6) 0.003(6) C51 0.032(6) 0.074(9) 0.074(9) 0.029(7) -0.024(6) -0.016(6) C56 0.046(7) 0.053(7) 0.050(7) 0.016(6) -0.011(6) -0.017(6) O25 0.069(5) 0.068(6) 0.037(4) 0.009(4) -0.005(4) 0.002(4) O26 0.025(5) 0.062(8) 0.044(7) -0.020(6) 0.008(5) -0.022(5) C61 0.026(7) 0.079(11) 0.024(8) 0.015(7) 0.008(6) -0.032(6) O26A 0.076(9) 0.095(15) 0.063(12) -0.003(12) 0.029(9) 0.006(13) C61A 0.095(12) 0.087(17) 0.052(15) 0.010(15) 0.019(9) -0.020(16) O27 0.029(4) 0.059(5) 0.056(5) 0.006(4) 0.000(3) -0.008(3) O28 0.030(4) 0.085(7) 0.195(12) -0.078(8) -0.001(6) -0.005(4) C66 0.031(5) 0.084(8) 0.057(7) -0.035(6) -0.007(5) 0.006(5) O29 0.031(4) 0.164(10) 0.086(7) 0.077(7) 0.002(4) -0.018(5) O30 0.059(5) 0.106(7) 0.054(5) 0.025(5) -0.001(4) -0.051(5) C71 0.079(8) 0.042(7) 0.053(7) 0.015(5) 0.023(5) -0.005(5) O32 0.076(6) 0.116(8) 0.057(5) -0.016(5) -0.012(4) 0.062(5) O31 0.061(6) 0.054(7) 0.063(7) 0.003(6) 0.023(6) -0.008(6) C76 0.067(7) 0.012(8) 0.090(11) 0.002(8) 0.044(8) -0.003(7) O31A 0.054(11) 0.049(13) 0.016(10) -0.003(9) 0.012(7) -0.006(9) C76A 0.065(13) 0.031(15) 0.030(12) 0.007(12) 0.029(9) 0.011(10) C81 0.042(6) 0.035(5) 0.039(6) -0.003(4) -0.002(5) 0.010(4) C82 0.053(6) 0.036(5) 0.060(6) -0.006(5) -0.005(5) 0.002(5) C83 0.067(7) 0.053(7) 0.093(9) 0.006(7) 0.011(7) 0.024(6) C84 0.085(10) 0.052(8) 0.069(6) 0.018(6) 0.013(6) 0.005(7) C85 0.064(7) 0.059(8) 0.131(12) -0.039(9) -0.020(8) -0.008(6) C86 0.029(6) 0.093(10) 0.059(8) 0.002(7) 0.010(6) 0.021(6) N1 0.035(5) 0.073(7) 0.041(5) 0.014(5) 0.008(4) 0.010(5) C100 0.059(7) 0.063(8) 0.036(6) 0.009(5) 0.011(5) 0.023(6) C101 0.066(8) 0.048(7) 0.076(9) 0.006(6) 0.036(7) 0.014(6) C102 0.052(7) 0.048(7) 0.061(7) 0.004(6) 0.021(6) -0.001(5) C103 0.046(7) 0.047(7) 0.059(7) -0.010(5) 0.004(5) 0.002(5) C104 0.034(6) 0.054(7) 0.058(7) -0.001(5) 0.005(5) 0.006(5) C105 0.071(8) 0.047(7) 0.054(7) -0.003(6) 0.006(6) -0.001(6) C106 0.074(8) 0.049(7) 0.040(6) 0.008(5) -0.009(6) -0.008(6) O50 0.171(14) 0.093(9) 0.112(10) 0.008(7) -0.001(9) -0.014(9) _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 Cd9 O4 2.219(8) . ? Cd9 O5 2.227(9) . ? Cd9 F2 2.247(6) . ? Cd9 O7 2.251(9) . ? Cd9 O2 2.256(9) . ? Cd9 F3 2.277(6) . ? Cr1 F2 1.881(6) . ? Cr1 O3 1.932(8) . ? Cr1 O1 1.939(7) . ? Cr1 F1 1.946(6) . ? Cr1 O36 1.986(7) . ? Cr1 O34 1.988(7) . ? Cr2 F3 1.887(6) . ? Cr2 O8 1.923(8) . ? Cr2 O6 1.933(8) . ? Cr2 F4 1.939(6) . ? Cr2 O9 1.983(8) . ? Cr2 O11 1.997(8) . ? Cr3 F4 1.904(6) . ? Cr3 F5 1.923(5) . ? Cr3 O12 1.935(8) . ? Cr3 O10 1.952(7) . ? Cr3 O15 1.958(8) . ? Cr3 O13 1.963(7) . ? Cr4 F6 1.924(5) . ? Cr4 F5 1.927(5) . ? Cr4 O14 1.937(7) . ? Cr4 O16 1.940(7) . ? Cr4 O17 1.945(7) . ? Cr4 O19 1.947(8) . ? Cr5 O21 1.923(8) . ? Cr5 F6 1.931(6) . ? Cr5 F7 1.936(6) . ? Cr5 O20 1.936(8) . ? Cr5 O18 1.948(7) . ? Cr5 O23 1.967(8) . ? Cr6 F8 1.938(6) . ? Cr6 F7 1.940(6) . ? Cr6 O27 1.945(8) . ? Cr6 O25 1.951(8) . ? Cr6 O22 1.959(8) . ? Cr6 O24 1.965(9) . ? Cr7 O29 1.878(10) . ? Cr7 F9 1.884(6) . ? Cr7 F8 1.929(7) . ? Cr7 O26 1.977(8) . ? Cr7 O31A 1.982(9) . ? Cr7 O28 1.994(8) . ? Cr7 O31 2.010(8) . ? Cr7 O26A 2.013(10) . ? Cr8 F1 1.901(6) . ? Cr8 O32 1.915(9) . ? Cr8 F9 1.916(5) . ? Cr8 O33 1.926(9) . ? Cr8 O35 1.931(10) . ? Cr8 O30 1.974(10) . ? O1 C1 1.242(14) . ? O2 C1 1.234(16) . ? O3 C6 1.261(14) . ? O4 C6 1.264(14) . ? O5 C11 1.247(15) . ? O6 C11 1.237(15) . ? O7 C16 1.239(15) . ? O8 C16 1.265(14) . ? O9 C21 1.274(13) . ? O10 C21 1.250(13) . ? O11 C26 1.233(14) . ? O12 C26 1.274(14) . ? O13 C36 1.270(13) . ? O14 C36 1.266(13) . ? O15 C31 1.247(15) . ? O16 C31 1.255(14) . ? O17 C41 1.243(14) . ? O18 C41 1.282(14) . ? O19 C46 1.252(16) . ? O20 C46 1.273(16) . ? O21 C51 1.205(16) . ? O22 C51 1.285(15) . ? O23 C56 1.263(14) . ? O24 C56 1.227(15) . ? O33 C81 1.252(13) . ? O34 C81 1.239(12) . ? O35 C86 1.210(16) . ? O36 C86 1.240(14) . ? C1 C2A 1.58(3) . ? C1 C2 1.62(3) . ? C2 C5 1.51(2) . ? C2 C4 1.52(2) . ? C2 C3 1.52(2) . ? C2A C5A 1.51(2) . ? C2A C3A 1.51(2) . ? C2A C4A 1.52(2) . ? C6 C7 1.531(18) . ? C7 C10 1.53(2) . ? C7 C9 1.54(2) . ? C7 C8 1.56(2) . ? C11 C12A 1.50(3) . ? C11 C12 1.66(3) . ? C12 C15 1.545(16) . ? C12 C14 1.547(16) . ? C12 C13 1.552(16) . ? C12A C15A 1.550(16) . ? C12A C14A 1.550(16) . ? C12A C13A 1.550(16) . ? C16 C17A 1.47(4) . ? C16 C17 1.59(2) . ? C17 C20 1.537(13) . ? C17 C18 1.538(13) . ? C17 C19 1.541(13) . ? C17A C18A 1.538(14) . ? C17A C19A 1.539(14) . ? C17A C20A 1.540(14) . ? C21 C22A 1.52(2) . ? C21 C22 1.58(2) . ? C22 C23 1.544(14) . ? C22 C24 1.545(14) . ? C22 C25 1.546(14) . ? C22A C24A 1.546(14) . ? C22A C23A 1.548(14) . ? C22A C25A 1.548(14) . ? C26 C27 1.50(2) . ? C26 C27A 1.51(2) . ? C27 C30 1.550(13) . ? C27 C29 1.551(13) . ? C27 C28 1.551(12) . ? C27A C29A 1.551(13) . ? C27A C28A 1.552(12) . ? C27A C30A 1.552(13) . ? C31 C32A 1.52(3) . ? C31 C32 1.54(3) . ? C32 C35 1.552(15) . ? C32 C33 1.553(15) . ? C32 C34 1.554(15) . ? C32A C34A 1.551(15) . ? C32A C33A 1.554(15) . ? C32A C35A 1.555(15) . ? C36 C37 1.488(15) . ? C37 C39 1.55(2) . ? C37 C38 1.563(17) . ? C37 C40 1.579(19) . ? C41 C42A 1.515(17) . ? C42 C44 1.551(15) . ? C42 C45 1.551(15) . ? C42 C43 1.552(15) . ? C42A C44A 1.544(14) . ? C42A C45A 1.551(14) . ? C42A C43A 1.558(14) . ? C46 C47A 1.53(3) . ? C46 C47 1.55(3) . ? C47 C49 1.529(15) . ? C47 C48 1.530(15) . ? C47 C50 1.531(15) . ? C47A C50A 1.530(15) . ? C47A C49A 1.530(15) . ? C47A C48A 1.534(15) . ? C51 C52A 1.57(2) . ? C51 C52 1.61(4) . ? C52 C55 1.542(16) . ? C52 C54 1.542(16) . ? C52 C53 1.545(16) . ? C52A C55A 1.542(16) . ? C52A C54A 1.543(15) . ? C52A C53A 1.548(16) . ? C56 C57 1.51(3) . ? C56 C57A 1.59(3) . ? C57 C59 1.550(13) . ? C57 C60 1.550(13) . ? C57 C58 1.551(13) . ? C57A C58A 1.548(13) . ? C57A C59A 1.549(13) . ? C57A C60A 1.550(13) . ? O25 C61A 1.259(11) . ? O25 C61 1.269(10) . ? O26 C61 1.267(10) . ? C61 C62 1.533(13) . ? C62 C64 1.508(17) . ? C62 C65 1.513(17) . ? C62 C63 1.513(17) . ? O26A C61A 1.264(11) . ? C61A C62A 1.535(14) . ? C62A C64A 1.507(17) . ? C62A C65A 1.509(17) . ? C62A C63A 1.511(17) . ? O27 C66 1.239(13) . ? O28 C66 1.210(13) . ? C66 C67A 1.530(14) . ? C66 C67 1.536(13) . ? C67 C70 1.551(14) . ? C67 C69 1.552(14) . ? C67 C68 1.555(14) . ? C67A C68A 1.548(15) . ? C67A C70A 1.548(15) . ? C67A C69A 1.548(15) . ? O29 C71 1.235(16) . ? O30 C71 1.212(16) . ? C71 C72A 1.48(3) . ? C71 C72 1.49(3) . ? C72 C73 1.534(15) . ? C72 C75 1.535(15) . ? C72 C74 1.543(15) . ? C72A C73A 1.535(15) . ? C72A C75A 1.535(15) . ? C72A C74A 1.539(15) . ? O32 C76 1.201(10) . ? O32 C76A 1.216(12) . ? O31 C76 1.199(11) . ? C76 C77 1.534(13) . ? C77 C78 1.555(14) . ? C77 C79 1.558(14) . ? C77 C80 1.559(14) . ? O31A C76A 1.212(12) . ? C76A C77A 1.541(14) . ? C77A C79A 1.560(15) . ? C77A C80A 1.561(15) . ? C77A C78A 1.562(15) . ? C81 C82 1.494(15) . ? C82 C85 1.517(18) . ? C82 C84 1.548(18) . ? C82 C83 1.578(17) . ? C86 C87 1.52(2) . ? C86 C87A 1.54(2) . ? C87 C89 1.552(14) . ? C87 C88 1.553(14) . ? C87 C90 1.556(14) . ? C87A C89A 1.554(14) . ? C87A C90A 1.555(14) . ? C87A C88A 1.556(14) . ? N1 C100 1.539(14) . ? N1 C103 1.554(15) . ? C100 C101 1.454(16) . ? C100 C102 1.529(16) . ? C103 C104 1.505(15) . ? C103 C105 1.525(17) . ? C103 C106 1.558(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cd9 O5 100.4(3) . . ? O4 Cd9 F2 90.6(3) . . ? O5 Cd9 F2 163.7(3) . . ? O4 Cd9 O7 88.3(3) . . ? O5 Cd9 O7 93.6(3) . . ? F2 Cd9 O7 98.9(3) . . ? O4 Cd9 O2 90.2(4) . . ? O5 Cd9 O2 87.4(3) . . ? F2 Cd9 O2 80.4(3) . . ? O7 Cd9 O2 178.4(3) . . ? O4 Cd9 F3 168.0(3) . . ? O5 Cd9 F3 87.2(3) . . ? F2 Cd9 F3 84.1(2) . . ? O7 Cd9 F3 81.9(3) . . ? O2 Cd9 F3 99.5(3) . . ? F2 Cr1 O3 93.5(3) . . ? F2 Cr1 O1 95.7(3) . . ? O3 Cr1 O1 92.2(3) . . ? F2 Cr1 F1 87.0(2) . . ? O3 Cr1 F1 178.0(3) . . ? O1 Cr1 F1 89.7(3) . . ? F2 Cr1 O36 178.0(3) . . ? O3 Cr1 O36 86.8(3) . . ? O1 Cr1 O36 86.3(3) . . ? F1 Cr1 O36 92.6(3) . . ? F2 Cr1 O34 88.8(3) . . ? O3 Cr1 O34 89.3(3) . . ? O1 Cr1 O34 175.2(3) . . ? F1 Cr1 O34 88.8(3) . . ? O36 Cr1 O34 89.2(3) . . ? F3 Cr2 O8 98.0(3) . . ? F3 Cr2 O6 92.5(3) . . ? O8 Cr2 O6 93.6(4) . . ? F3 Cr2 F4 87.9(3) . . ? O8 Cr2 F4 173.4(3) . . ? O6 Cr2 F4 89.1(3) . . ? F3 Cr2 O9 90.2(3) . . ? O8 Cr2 O9 88.4(3) . . ? O6 Cr2 O9 176.5(3) . . ? F4 Cr2 O9 88.7(3) . . ? F3 Cr2 O11 177.8(3) . . ? O8 Cr2 O11 83.8(3) . . ? O6 Cr2 O11 88.7(3) . . ? F4 Cr2 O11 90.3(3) . . ? O9 Cr2 O11 88.6(3) . . ? F4 Cr3 F5 90.4(2) . . ? F4 Cr3 O12 91.9(3) . . ? F5 Cr3 O12 177.7(3) . . ? F4 Cr3 O10 93.0(3) . . ? F5 Cr3 O10 89.6(3) . . ? O12 Cr3 O10 90.2(3) . . ? F4 Cr3 O15 178.9(3) . . ? F5 Cr3 O15 90.5(3) . . ? O12 Cr3 O15 87.2(4) . . ? O10 Cr3 O15 86.4(3) . . ? F4 Cr3 O13 88.9(3) . . ? F5 Cr3 O13 90.9(3) . . ? O12 Cr3 O13 89.2(3) . . ? O10 Cr3 O13 178.0(3) . . ? O15 Cr3 O13 91.7(3) . . ? F6 Cr4 F5 91.2(2) . . ? F6 Cr4 O14 89.7(3) . . ? F5 Cr4 O14 89.5(3) . . ? F6 Cr4 O16 175.0(3) . . ? F5 Cr4 O16 93.4(3) . . ? O14 Cr4 O16 92.3(3) . . ? F6 Cr4 O17 91.2(3) . . ? F5 Cr4 O17 89.0(3) . . ? O14 Cr4 O17 178.3(3) . . ? O16 Cr4 O17 86.9(3) . . ? F6 Cr4 O19 90.3(3) . . ? F5 Cr4 O19 177.2(3) . . ? O14 Cr4 O19 88.2(3) . . ? O16 Cr4 O19 85.2(3) . . ? O17 Cr4 O19 93.3(3) . . ? O21 Cr5 F6 174.6(3) . . ? O21 Cr5 F7 91.1(3) . . ? F6 Cr5 F7 91.7(2) . . ? O21 Cr5 O20 83.7(4) . . ? F6 Cr5 O20 93.9(3) . . ? F7 Cr5 O20 173.1(3) . . ? O21 Cr5 O18 86.6(3) . . ? F6 Cr5 O18 88.7(3) . . ? F7 Cr5 O18 92.4(3) . . ? O20 Cr5 O18 91.8(3) . . ? O21 Cr5 O23 95.8(3) . . ? F6 Cr5 O23 88.8(3) . . ? F7 Cr5 O23 89.9(3) . . ? O20 Cr5 O23 86.1(3) . . ? O18 Cr5 O23 176.6(3) . . ? F8 Cr6 F7 92.4(2) . . ? F8 Cr6 O27 89.3(3) . . ? F7 Cr6 O27 90.2(3) . . ? F8 Cr6 O25 91.5(3) . . ? F7 Cr6 O25 174.4(3) . . ? O27 Cr6 O25 94.0(3) . . ? F8 Cr6 O22 173.1(3) . . ? F7 Cr6 O22 93.2(3) . . ? O27 Cr6 O22 86.7(3) . . ? O25 Cr6 O22 83.3(4) . . ? F8 Cr6 O24 89.1(3) . . ? F7 Cr6 O24 88.8(3) . . ? O27 Cr6 O24 178.1(3) . . ? O25 Cr6 O24 87.2(3) . . ? O22 Cr6 O24 95.0(4) . . ? O29 Cr7 F9 90.5(4) . . ? O29 Cr7 F8 90.6(4) . . ? F9 Cr7 F8 91.0(2) . . ? O29 Cr7 O26 95.8(5) . . ? F9 Cr7 O26 168.2(4) . . ? F8 Cr7 O26 98.8(4) . . ? O29 Cr7 O31A 69.0(8) . . ? F9 Cr7 O31A 99.3(6) . . ? F8 Cr7 O31A 157.0(7) . . ? O26 Cr7 O31A 73.9(7) . . ? O29 Cr7 O28 179.4(5) . . ? F9 Cr7 O28 89.4(4) . . ? F8 Cr7 O28 90.0(3) . . ? O26 Cr7 O28 84.1(5) . . ? O31A Cr7 O28 110.4(8) . . ? O29 Cr7 O31 98.4(5) . . ? F9 Cr7 O31 87.2(4) . . ? F8 Cr7 O31 170.8(4) . . ? O26 Cr7 O31 82.1(5) . . ? O31A Cr7 O31 31.9(7) . . ? O28 Cr7 O31 81.0(4) . . ? O29 Cr7 O26A 61.8(8) . . ? F9 Cr7 O26A 150.8(8) . . ? F8 Cr7 O26A 80.8(7) . . ? O26 Cr7 O26A 39.0(8) . . ? O31A Cr7 O26A 80.3(9) . . ? O28 Cr7 O26A 118.3(8) . . ? O31 Cr7 O26A 105.0(7) . . ? F1 Cr8 O32 176.4(4) . . ? F1 Cr8 F9 90.1(2) . . ? O32 Cr8 F9 93.5(4) . . ? F1 Cr8 O33 89.8(3) . . ? O32 Cr8 O33 90.9(4) . . ? F9 Cr8 O33 90.7(4) . . ? F1 Cr8 O35 90.3(4) . . ? O32 Cr8 O35 86.1(5) . . ? F9 Cr8 O35 176.6(5) . . ? O33 Cr8 O35 92.7(6) . . ? F1 Cr8 O30 90.4(3) . . ? O32 Cr8 O30 88.9(4) . . ? F9 Cr8 O30 88.9(3) . . ? O33 Cr8 O30 179.6(5) . . ? O35 Cr8 O30 87.7(5) . . ? Cr8 F1 Cr1 124.2(3) . . ? Cr1 F2 Cd9 117.5(3) . . ? Cr2 F3 Cd9 116.4(3) . . ? Cr3 F4 Cr2 124.4(3) . . ? Cr3 F5 Cr4 122.6(3) . . ? Cr4 F6 Cr5 121.0(3) . . ? Cr5 F7 Cr6 121.1(3) . . ? Cr7 F8 Cr6 121.9(3) . . ? Cr7 F9 Cr8 122.9(3) . . ? C1 O1 Cr1 136.1(8) . . ? C1 O2 Cd9 119.3(9) . . ? C6 O3 Cr1 130.5(8) . . ? C6 O4 Cd9 129.4(7) . . ? C11 O5 Cd9 128.7(8) . . ? C11 O6 Cr2 128.6(9) . . ? C16 O7 Cd9 119.5(8) . . ? C16 O8 Cr2 136.7(8) . . ? C21 O9 Cr2 128.1(7) . . ? C21 O10 Cr3 134.6(7) . . ? C26 O11 Cr2 138.3(8) . . ? C26 O12 Cr3 128.8(8) . . ? C36 O13 Cr3 134.5(7) . . ? C36 O14 Cr4 128.7(7) . . ? C31 O15 Cr3 128.6(7) . . ? C31 O16 Cr4 133.7(7) . . ? C41 O17 Cr4 135.9(7) . . ? C41 O18 Cr5 125.9(7) . . ? C46 O19 Cr4 127.7(8) . . ? C46 O20 Cr5 132.6(8) . . ? C51 O21 Cr5 130.0(8) . . ? C51 O22 Cr6 131.9(8) . . ? C56 O23 Cr5 133.0(8) . . ? C56 O24 Cr6 127.1(7) . . ? C81 O33 Cr8 138.4(8) . . ? C81 O34 Cr1 131.8(7) . . ? C86 O35 Cr8 135.2(10) . . ? C86 O36 Cr1 134.9(7) . . ? O2 C1 O1 127.7(12) . . ? O2 C1 C2A 116.7(14) . . ? O1 C1 C2A 112.2(15) . . ? O2 C1 C2 121.2(13) . . ? O1 C1 C2 110.2(13) . . ? C2A C1 C2 30.6(12) . . ? C5 C2 C4 109.8(13) . . ? C5 C2 C3 109.8(13) . . ? C4 C2 C3 109.4(13) . . ? C5 C2 C1 110(2) . . ? C4 C2 C1 102(3) . . ? C3 C2 C1 115(2) . . ? C5A C2A C3A 109.8(13) . . ? C5A C2A C4A 109.5(13) . . ? C3A C2A C4A 109.3(13) . . ? C5A C2A C1 111(3) . . ? C3A C2A C1 106(2) . . ? C4A C2A C1 111(3) . . ? O3 C6 O4 125.2(11) . . ? O3 C6 C7 117.1(11) . . ? O4 C6 C7 117.6(11) . . ? C10 C7 C6 110.8(12) . . ? C10 C7 C9 112.9(15) . . ? C6 C7 C9 107.3(12) . . ? C10 C7 C8 108.6(15) . . ? C6 C7 C8 108.0(12) . . ? C9 C7 C8 109.1(13) . . ? O6 C11 O5 129.5(13) . . ? O6 C11 C12A 114.0(13) . . ? O5 C11 C12A 116.1(14) . . ? O6 C11 C12 115.8(12) . . ? O5 C11 C12 114.4(13) . . ? C12A C11 C12 14.1(11) . . ? C15 C12 C14 111.1(10) . . ? C15 C12 C13 110.7(9) . . ? C14 C12 C13 110.6(9) . . ? C15 C12 C11 111.4(17) . . ? C14 C12 C11 114.7(19) . . ? C13 C12 C11 98(2) . . ? C11 C12A C15A 100(2) . . ? C11 C12A C14A 110(2) . . ? C15A C12A C14A 110.6(10) . . ? C11 C12A C13A 115(2) . . ? C15A C12A C13A 110.7(10) . . ? C14A C12A C13A 110.6(10) . . ? O7 C16 O8 125.3(12) . . ? O7 C16 C17A 116.8(15) . . ? O8 C16 C17A 116.1(14) . . ? O7 C16 C17 122.8(11) . . ? O8 C16 C17 111.8(11) . . ? C17A C16 C17 18.7(12) . . ? C20 C17 C18 110.9(9) . . ? C20 C17 C19 110.7(8) . . ? C18 C17 C19 110.6(8) . . ? C20 C17 C16 114.2(16) . . ? C18 C17 C16 107(2) . . ? C19 C17 C16 102.9(14) . . ? C16 C17A C18A 110(3) . . ? C16 C17A C19A 112(3) . . ? C18A C17A C19A 110.9(9) . . ? C16 C17A C20A 103(3) . . ? C18A C17A C20A 110.6(9) . . ? C19A C17A C20A 110.5(9) . . ? O10 C21 O9 126.1(10) . . ? O10 C21 C22A 123.1(11) . . ? O9 C21 C22A 110.6(11) . . ? O10 C21 C22 111.3(11) . . ? O9 C21 C22 122.3(11) . . ? C22A C21 C22 14.4(9) . . ? C23 C22 C24 111.1(8) . . ? C23 C22 C25 111.1(8) . . ? C24 C22 C25 111.1(8) . . ? C23 C22 C21 113.2(18) . . ? C24 C22 C21 107.3(16) . . ? C25 C22 C21 102.6(17) . . ? C21 C22A C24A 112.7(16) . . ? C21 C22A C23A 105.5(14) . . ? C24A C22A C23A 110.6(8) . . ? C21 C22A C25A 105.9(14) . . ? C24A C22A C25A 110.8(8) . . ? C23A C22A C25A 111.0(8) . . ? O11 C26 O12 123.3(11) . . ? O11 C26 C27 122.1(12) . . ? O12 C26 C27 114.1(12) . . ? O11 C26 C27A 113.6(12) . . ? O12 C26 C27A 123.0(12) . . ? C27 C26 C27A 13.7(11) . . ? C26 C27 C30 112.8(18) . . ? C26 C27 C29 104.6(16) . . ? C30 C27 C29 110.2(9) . . ? C26 C27 C28 107.2(15) . . ? C30 C27 C28 111.8(17) . . ? C29 C27 C28 109.9(9) . . ? C26 C27A C29A 110.4(17) . . ? C26 C27A C28A 106.2(16) . . ? C29A C27A C28A 110.3(9) . . ? C26 C27A C30A 110.0(17) . . ? C29A C27A C30A 110.0(9) . . ? C28A C27A C30A 109.9(9) . . ? O15 C31 O16 126.2(10) . . ? O15 C31 C32A 112.4(12) . . ? O16 C31 C32A 121.3(13) . . ? O15 C31 C32 120.6(14) . . ? O16 C31 C32 112.9(14) . . ? C32A C31 C32 11.0(13) . . ? C31 C32 C35 116(2) . . ? C31 C32 C33 109(3) . . ? C35 C32 C33 111.3(10) . . ? C31 C32 C34 98(2) . . ? C35 C32 C34 111.1(10) . . ? C33 C32 C34 111.1(10) . . ? C31 C32A C34A 110(2) . . ? C31 C32A C33A 105.6(17) . . ? C34A C32A C33A 111.4(9) . . ? C31 C32A C35A 108.1(18) . . ? C34A C32A C35A 111.1(9) . . ? C33A C32A C35A 110.8(9) . . ? O14 C36 O13 124.8(10) . . ? O14 C36 C37 119.7(10) . . ? O13 C36 C37 115.5(11) . . ? C36 C37 C39 107.2(10) . . ? C36 C37 C38 106.9(10) . . ? C39 C37 C38 109.5(12) . . ? C36 C37 C40 110.1(11) . . ? C39 C37 C40 113.7(13) . . ? C38 C37 C40 109.2(12) . . ? O17 C41 O18 124.5(10) . . ? O17 C41 C42A 119.8(10) . . ? O18 C41 C42A 115.7(11) . . ? C44 C42 C45 110.7(10) . . ? C44 C42 C43 110.7(10) . . ? C45 C42 C43 110.6(11) . . ? C41 C42A C44A 110.6(11) . . ? C41 C42A C45A 110.4(12) . . ? C44A C42A C45A 111.4(8) . . ? C41 C42A C43A 103.6(14) . . ? C44A C42A C43A 110.6(8) . . ? C45A C42A C43A 110.1(8) . . ? O19 C46 O20 124.3(11) . . ? O19 C46 C47A 115.1(15) . . ? O20 C46 C47A 120.6(15) . . ? O19 C46 C47 124.9(14) . . ? O20 C46 C47 110.8(14) . . ? C47A C46 C47 10.0(13) . . ? C49 C47 C48 111.3(9) . . ? C49 C47 C50 111.1(9) . . ? C48 C47 C50 110.9(9) . . ? C49 C47 C46 103(2) . . ? C48 C47 C46 116.9(19) . . ? C50 C47 C46 103.4(18) . . ? C50A C47A C49A 111.1(9) . . ? C50A C47A C46 111(2) . . ? C49A C47A C46 107(2) . . ? C50A C47A C48A 110.8(9) . . ? C49A C47A C48A 110.7(9) . . ? C46 C47A C48A 106(2) . . ? O21 C51 O22 126.2(11) . . ? O21 C51 C52A 118.0(11) . . ? O22 C51 C52A 115.6(13) . . ? O21 C51 C52 132.1(14) . . ? O22 C51 C52 101.2(15) . . ? C52A C51 C52 18.3(12) . . ? C55 C52 C54 111.8(10) . . ? C55 C52 C53 111.4(10) . . ? C54 C52 C53 111.5(10) . . ? C55 C52 C51 111(3) . . ? C54 C52 C51 95(3) . . ? C53 C52 C51 115(3) . . ? C55A C52A C54A 111.6(9) . . ? C55A C52A C53A 111.2(9) . . ? C54A C52A C53A 111.1(9) . . ? C55A C52A C51 102.1(17) . . ? C54A C52A C51 110.0(14) . . ? C53A C52A C51 110.4(19) . . ? O24 C56 O23 127.6(11) . . ? O24 C56 C57 110.9(12) . . ? O23 C56 C57 121.4(13) . . ? O24 C56 C57A 119.1(12) . . ? O23 C56 C57A 113.1(13) . . ? C57 C56 C57A 11.3(11) . . ? C56 C57 C59 105.9(16) . . ? C56 C57 C60 109.9(16) . . ? C59 C57 C60 111.0(8) . . ? C56 C57 C58 108(2) . . ? C59 C57 C58 110.8(8) . . ? C60 C57 C58 110.8(8) . . ? C58A C57A C59A 111.2(9) . . ? C58A C57A C60A 111.0(8) . . ? C59A C57A C60A 110.9(8) . . ? C58A C57A C56 110(3) . . ? C59A C57A C56 105.5(19) . . ? C60A C57A C56 108.0(19) . . ? C61A O25 C61 38.3(19) . . ? C61A O25 Cr6 135.2(12) . . ? C61 O25 Cr6 129.4(8) . . ? C61 O26 Cr7 124.5(9) . . ? O26 C61 O25 130.6(12) . . ? O26 C61 C62 109.7(10) . . ? O25 C61 C62 119.6(10) . . ? C64 C62 C65 109.2(10) . . ? C64 C62 C63 109.0(10) . . ? C65 C62 C63 108.6(10) . . ? C64 C62 C61 106.8(16) . . ? C65 C62 C61 108(2) . . ? C63 C62 C61 115.3(14) . . ? C61A O26A Cr7 137.5(19) . . ? O25 C61A O26A 116(2) . . ? O25 C61A C62A 106.5(17) . . ? O26A C61A C62A 137.2(17) . . ? C64A C62A C65A 109.4(11) . . ? C64A C62A C63A 109.3(11) . . ? C65A C62A C63A 109.1(11) . . ? C64A C62A C61A 128(3) . . ? C65A C62A C61A 96(4) . . ? C63A C62A C61A 104(3) . . ? C66 O27 Cr6 136.8(7) . . ? C66 O28 Cr7 127.2(10) . . ? O28 C66 O27 128.5(11) . . ? O28 C66 C67A 100(2) . . ? O27 C66 C67A 131(2) . . ? O28 C66 C67 116.2(11) . . ? O27 C66 C67 114.9(9) . . ? C67A C66 C67 20.7(19) . . ? C66 C67 C70 112.1(11) . . ? C66 C67 C69 114.1(12) . . ? C70 C67 C69 109.3(8) . . ? C66 C67 C68 102.7(12) . . ? C70 C67 C68 109.2(8) . . ? C69 C67 C68 109.2(8) . . ? C66 C67A C68A 134(4) . . ? C66 C67A C70A 97(4) . . ? C68A C67A C70A 109.9(10) . . ? C66 C67A C69A 94(3) . . ? C68A C67A C69A 109.8(10) . . ? C70A C67A C69A 109.8(10) . . ? C71 O29 Cr7 138.4(9) . . ? C71 O30 Cr8 132.8(8) . . ? O30 C71 O29 123.0(11) . . ? O30 C71 C72A 130.8(16) . . ? O29 C71 C72A 105.8(15) . . ? O30 C71 C72 123.6(14) . . ? O29 C71 C72 113.4(14) . . ? C72A C71 C72 8.5(14) . . ? C71 C72 C73 113(2) . . ? C71 C72 C75 109.1(17) . . ? C73 C72 C75 109.9(10) . . ? C71 C72 C74 105.8(19) . . ? C73 C72 C74 109.4(10) . . ? C75 C72 C74 109.4(9) . . ? C71 C72A C73A 94(2) . . ? C71 C72A C75A 119(2) . . ? C73A C72A C75A 109.9(10) . . ? C71 C72A C74A 113(3) . . ? C73A C72A C74A 109.5(10) . . ? C75A C72A C74A 109.8(10) . . ? C76 O32 C76A 18(3) . . ? C76 O32 Cr8 135.5(10) . . ? C76A O32 Cr8 133.5(14) . . ? C76 O31 Cr7 130.9(10) . . ? O31 C76 O32 123.1(14) . . ? O31 C76 C77 123.0(11) . . ? O32 C76 C77 113.8(11) . . ? C76 C77 C78 103.0(14) . . ? C76 C77 C79 108.2(14) . . ? C78 C77 C79 110.5(8) . . ? C76 C77 C80 114.0(13) . . ? C78 C77 C80 110.4(8) . . ? C79 C77 C80 110.4(8) . . ? C76A O31A Cr7 120(2) . . ? O31A C76A O32 126(2) . . ? O31A C76A C77A 101.9(17) . . ? O32 C76A C77A 129(2) . . ? C76A C77A C79A 115(4) . . ? C76A C77A C80A 108(3) . . ? C79A C77A C80A 110.1(9) . . ? C76A C77A C78A 104(3) . . ? C79A C77A C78A 109.9(9) . . ? C80A C77A C78A 109.8(9) . . ? O34 C81 O33 124.2(10) . . ? O34 C81 C82 118.5(9) . . ? O33 C81 C82 117.3(10) . . ? C81 C82 C85 108.7(10) . . ? C81 C82 C84 111.1(9) . . ? C85 C82 C84 112.3(12) . . ? C81 C82 C83 106.5(10) . . ? C85 C82 C83 109.2(11) . . ? C84 C82 C83 108.8(10) . . ? O35 C86 O36 123.3(10) . . ? O35 C86 C87 117.1(13) . . ? O36 C86 C87 119.1(11) . . ? O35 C86 C87A 122.2(13) . . ? O36 C86 C87A 113.7(12) . . ? C87 C86 C87A 16.5(10) . . ? C86 C87 C89 113.1(16) . . ? C86 C87 C88 110.2(15) . . ? C89 C87 C88 111.4(9) . . ? C86 C87 C90 99.6(16) . . ? C89 C87 C90 111.0(9) . . ? C88 C87 C90 110.9(8) . . ? C86 C87A C89A 107.4(18) . . ? C86 C87A C90A 112.3(17) . . ? C89A C87A C90A 111.0(9) . . ? C86 C87A C88A 104.2(19) . . ? C89A C87A C88A 110.8(9) . . ? C90A C87A C88A 110.8(8) . . ? C100 N1 C103 116.0(9) . . ? C101 C100 C102 112.1(11) . . ? C101 C100 N1 109.2(10) . . ? C102 C100 N1 108.4(9) . . ? C104 C103 C105 111.0(10) . . ? C104 C103 N1 108.0(9) . . ? C105 C103 N1 110.9(9) . . ? C104 C103 C106 112.1(10) . . ? C105 C103 C106 109.7(10) . . ? N1 C103 C106 105.0(9) . . ? 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 O32 Cr8 F1 Cr1 56(6) . . . . ? F9 Cr8 F1 Cr1 -136.3(4) . . . . ? O33 Cr8 F1 Cr1 -45.6(5) . . . . ? O35 Cr8 F1 Cr1 47.1(6) . . . . ? O30 Cr8 F1 Cr1 134.8(4) . . . . ? F2 Cr1 F1 Cr8 143.1(4) . . . . ? O3 Cr1 F1 Cr8 39(9) . . . . ? O1 Cr1 F1 Cr8 -121.2(4) . . . . ? O36 Cr1 F1 Cr8 -35.0(4) . . . . ? O34 Cr1 F1 Cr8 54.2(4) . . . . ? O3 Cr1 F2 Cd9 -52.9(4) . . . . ? O1 Cr1 F2 Cd9 39.7(4) . . . . ? F1 Cr1 F2 Cd9 129.0(3) . . . . ? O36 Cr1 F2 Cd9 -152(9) . . . . ? O34 Cr1 F2 Cd9 -142.1(3) . . . . ? O4 Cd9 F2 Cr1 28.6(4) . . . . ? O5 Cd9 F2 Cr1 -103.7(10) . . . . ? O7 Cd9 F2 Cr1 117.0(3) . . . . ? O2 Cd9 F2 Cr1 -61.5(4) . . . . ? F3 Cd9 F2 Cr1 -162.2(3) . . . . ? O8 Cr2 F3 Cd9 33.9(4) . . . . ? O6 Cr2 F3 Cd9 -60.1(4) . . . . ? F4 Cr2 F3 Cd9 -149.1(3) . . . . ? O9 Cr2 F3 Cd9 122.2(3) . . . . ? O11 Cr2 F3 Cd9 177(100) . . . . ? O4 Cd9 F3 Cr2 -93.0(13) . . . . ? O5 Cd9 F3 Cr2 36.7(4) . . . . ? F2 Cd9 F3 Cr2 -157.2(3) . . . . ? O7 Cd9 F3 Cr2 -57.3(4) . . . . ? O2 Cd9 F3 Cr2 123.6(4) . . . . ? F5 Cr3 F4 Cr2 128.1(3) . . . . ? O12 Cr3 F4 Cr2 -51.8(4) . . . . ? O10 Cr3 F4 Cr2 38.5(4) . . . . ? O15 Cr3 F4 Cr2 -17(15) . . . . ? O13 Cr3 F4 Cr2 -141.0(4) . . . . ? F3 Cr2 F4 Cr3 -143.8(4) . . . . ? O8 Cr2 F4 Cr3 10(3) . . . . ? O6 Cr2 F4 Cr3 123.6(4) . . . . ? O9 Cr2 F4 Cr3 -53.6(4) . . . . ? O11 Cr2 F4 Cr3 34.9(4) . . . . ? F4 Cr3 F5 Cr4 128.6(3) . . . . ? O12 Cr3 F5 Cr4 -54(8) . . . . ? O10 Cr3 F5 Cr4 -138.4(3) . . . . ? O15 Cr3 F5 Cr4 -52.0(4) . . . . ? O13 Cr3 F5 Cr4 39.7(4) . . . . ? F6 Cr4 F5 Cr3 -147.5(3) . . . . ? O14 Cr4 F5 Cr3 -57.8(4) . . . . ? O16 Cr4 F5 Cr3 34.5(4) . . . . ? O17 Cr4 F5 Cr3 121.3(4) . . . . ? O19 Cr4 F5 Cr3 -26(6) . . . . ? F5 Cr4 F6 Cr5 -128.4(3) . . . . ? O14 Cr4 F6 Cr5 142.1(4) . . . . ? O16 Cr4 F6 Cr5 29(3) . . . . ? O17 Cr4 F6 Cr5 -39.4(4) . . . . ? O19 Cr4 F6 Cr5 53.9(4) . . . . ? O21 Cr5 F6 Cr4 31(4) . . . . ? F7 Cr5 F6 Cr4 152.3(3) . . . . ? O20 Cr5 F6 Cr4 -31.8(4) . . . . ? O18 Cr5 F6 Cr4 59.9(4) . . . . ? O23 Cr5 F6 Cr4 -117.8(4) . . . . ? O21 Cr5 F7 Cr6 -52.8(4) . . . . ? F6 Cr5 F7 Cr6 131.8(3) . . . . ? O20 Cr5 F7 Cr6 -12(3) . . . . ? O18 Cr5 F7 Cr6 -139.4(4) . . . . ? O23 Cr5 F7 Cr6 43.0(4) . . . . ? F8 Cr6 F7 Cr5 -150.0(3) . . . . ? O27 Cr6 F7 Cr5 120.7(4) . . . . ? O25 Cr6 F7 Cr5 -17(3) . . . . ? O22 Cr6 F7 Cr5 34.0(4) . . . . ? O24 Cr6 F7 Cr5 -60.9(4) . . . . ? O29 Cr7 F8 Cr6 -123.5(4) . . . . ? F9 Cr7 F8 Cr6 146.0(3) . . . . ? O26 Cr7 F8 Cr6 -27.5(5) . . . . ? O31A Cr7 F8 Cr6 -96.9(17) . . . . ? O28 Cr7 F8 Cr6 56.5(5) . . . . ? O31 Cr7 F8 Cr6 68(3) . . . . ? O26A Cr7 F8 Cr6 -62.2(8) . . . . ? F7 Cr6 F8 Cr7 -137.5(4) . . . . ? O27 Cr6 F8 Cr7 -47.4(4) . . . . ? O25 Cr6 F8 Cr7 46.6(4) . . . . ? O22 Cr6 F8 Cr7 7(3) . . . . ? O24 Cr6 F8 Cr7 133.8(4) . . . . ? O29 Cr7 F9 Cr8 46.3(5) . . . . ? F8 Cr7 F9 Cr8 136.9(4) . . . . ? O26 Cr7 F9 Cr8 -76.4(18) . . . . ? O31A Cr7 F9 Cr8 -22.4(8) . . . . ? O28 Cr7 F9 Cr8 -133.1(4) . . . . ? O31 Cr7 F9 Cr8 -52.1(5) . . . . ? O26A Cr7 F9 Cr8 64.3(13) . . . . ? F1 Cr8 F9 Cr7 -143.8(4) . . . . ? O32 Cr8 F9 Cr7 35.4(5) . . . . ? O33 Cr8 F9 Cr7 126.3(4) . . . . ? O35 Cr8 F9 Cr7 -48(8) . . . . ? O30 Cr8 F9 Cr7 -53.4(4) . . . . ? F2 Cr1 O1 C1 8.2(13) . . . . ? O3 Cr1 O1 C1 101.9(13) . . . . ? F1 Cr1 O1 C1 -78.7(13) . . . . ? O36 Cr1 O1 C1 -171.4(13) . . . . ? O34 Cr1 O1 C1 -150(4) . . . . ? O4 Cd9 O2 C1 -26.4(10) . . . . ? O5 Cd9 O2 C1 -126.7(10) . . . . ? F2 Cd9 O2 C1 64.2(10) . . . . ? O7 Cd9 O2 C1 -2(12) . . . . ? F3 Cd9 O2 C1 146.5(10) . . . . ? F2 Cr1 O3 C6 63.7(11) . . . . ? O1 Cr1 O3 C6 -32.2(11) . . . . ? F1 Cr1 O3 C6 168(8) . . . . ? O36 Cr1 O3 C6 -118.3(11) . . . . ? O34 Cr1 O3 C6 152.5(11) . . . . ? O5 Cd9 O4 C6 -175.7(12) . . . . ? F2 Cd9 O4 C6 16.5(12) . . . . ? O7 Cd9 O4 C6 -82.4(12) . . . . ? O2 Cd9 O4 C6 96.9(12) . . . . ? F3 Cd9 O4 C6 -47(2) . . . . ? O4 Cd9 O5 C11 -174.9(12) . . . . ? F2 Cd9 O5 C11 -43.7(19) . . . . ? O7 Cd9 O5 C11 96.1(13) . . . . ? O2 Cd9 O5 C11 -85.2(13) . . . . ? F3 Cd9 O5 C11 14.5(13) . . . . ? F3 Cr2 O6 C11 56.0(11) . . . . ? O8 Cr2 O6 C11 -42.1(11) . . . . ? F4 Cr2 O6 C11 143.9(10) . . . . ? O9 Cr2 O6 C11 -165(5) . . . . ? O11 Cr2 O6 C11 -125.8(11) . . . . ? O4 Cd9 O7 C16 -120.7(9) . . . . ? O5 Cd9 O7 C16 -20.4(9) . . . . ? F2 Cd9 O7 C16 149.0(9) . . . . ? O2 Cd9 O7 C16 -145(11) . . . . ? F3 Cd9 O7 C16 66.3(9) . . . . ? F3 Cr2 O8 C16 13.1(14) . . . . ? O6 Cr2 O8 C16 106.1(14) . . . . ? F4 Cr2 O8 C16 -140(2) . . . . ? O9 Cr2 O8 C16 -76.9(14) . . . . ? O11 Cr2 O8 C16 -165.6(14) . . . . ? F3 Cr2 O9 C21 136.4(8) . . . . ? O8 Cr2 O9 C21 -125.6(8) . . . . ? O6 Cr2 O9 C21 -2(6) . . . . ? F4 Cr2 O9 C21 48.5(8) . . . . ? O11 Cr2 O9 C21 -41.8(8) . . . . ? F4 Cr3 O10 C21 -1.3(10) . . . . ? F5 Cr3 O10 C21 -91.7(10) . . . . ? O12 Cr3 O10 C21 90.6(10) . . . . ? O15 Cr3 O10 C21 177.8(10) . . . . ? O13 Cr3 O10 C21 163(10) . . . . ? F3 Cr2 O11 C26 37(9) . . . . ? O8 Cr2 O11 C26 -178.9(13) . . . . ? O6 Cr2 O11 C26 -85.2(13) . . . . ? F4 Cr2 O11 C26 3.9(13) . . . . ? O9 Cr2 O11 C26 92.6(13) . . . . ? F4 Cr3 O12 C26 46.5(10) . . . . ? F5 Cr3 O12 C26 -131(7) . . . . ? O10 Cr3 O12 C26 -46.5(10) . . . . ? O15 Cr3 O12 C26 -132.8(10) . . . . ? O13 Cr3 O12 C26 135.4(10) . . . . ? F4 Cr3 O13 C36 -82.7(10) . . . . ? F5 Cr3 O13 C36 7.7(10) . . . . ? O12 Cr3 O13 C36 -174.6(10) . . . . ? O10 Cr3 O13 C36 113(10) . . . . ? O15 Cr3 O13 C36 98.2(10) . . . . ? F6 Cr4 O14 C36 137.1(9) . . . . ? F5 Cr4 O14 C36 46.0(9) . . . . ? O16 Cr4 O14 C36 -47.5(9) . . . . ? O17 Cr4 O14 C36 17(11) . . . . ? O19 Cr4 O14 C36 -132.6(9) . . . . ? F4 Cr3 O15 C31 -169(100) . . . . ? F5 Cr3 O15 C31 45.8(10) . . . . ? O12 Cr3 O15 C31 -134.3(10) . . . . ? O10 Cr3 O15 C31 135.4(10) . . . . ? O13 Cr3 O15 C31 -45.1(10) . . . . ? F6 Cr4 O16 C31 -148(3) . . . . ? F5 Cr4 O16 C31 8.8(11) . . . . ? O14 Cr4 O16 C31 98.4(11) . . . . ? O17 Cr4 O16 C31 -80.0(11) . . . . ? O19 Cr4 O16 C31 -173.6(11) . . . . ? F6 Cr4 O17 C41 -8.3(10) . . . . ? F5 Cr4 O17 C41 82.9(10) . . . . ? O14 Cr4 O17 C41 111(11) . . . . ? O16 Cr4 O17 C41 176.4(10) . . . . ? O19 Cr4 O17 C41 -98.7(10) . . . . ? O21 Cr5 O18 C41 124.6(8) . . . . ? F6 Cr5 O18 C41 -52.8(8) . . . . ? F7 Cr5 O18 C41 -144.4(8) . . . . ? O20 Cr5 O18 C41 41.0(8) . . . . ? O23 Cr5 O18 C41 -10(5) . . . . ? F6 Cr4 O19 C46 -51.2(9) . . . . ? F5 Cr4 O19 C46 -173(5) . . . . ? O14 Cr4 O19 C46 -140.9(10) . . . . ? O16 Cr4 O19 C46 126.6(10) . . . . ? O17 Cr4 O19 C46 40.0(10) . . . . ? O21 Cr5 O20 C46 167.3(11) . . . . ? F6 Cr5 O20 C46 -17.5(11) . . . . ? F7 Cr5 O20 C46 126(2) . . . . ? O18 Cr5 O20 C46 -106.3(10) . . . . ? O23 Cr5 O20 C46 71.0(10) . . . . ? F6 Cr5 O21 C51 167(3) . . . . ? F7 Cr5 O21 C51 45.7(11) . . . . ? O20 Cr5 O21 C51 -129.7(11) . . . . ? O18 Cr5 O21 C51 138.1(11) . . . . ? O23 Cr5 O21 C51 -44.3(11) . . . . ? F8 Cr6 O22 C51 -133(2) . . . . ? F7 Cr6 O22 C51 11.4(12) . . . . ? O27 Cr6 O22 C51 -78.6(11) . . . . ? O25 Cr6 O22 C51 -173.0(12) . . . . ? O24 Cr6 O22 C51 100.4(11) . . . . ? O21 Cr5 O23 C56 99.3(10) . . . . ? F6 Cr5 O23 C56 -83.4(10) . . . . ? F7 Cr5 O23 C56 8.2(10) . . . . ? O20 Cr5 O23 C56 -177.4(11) . . . . ? O18 Cr5 O23 C56 -126(5) . . . . ? F8 Cr6 O24 C56 135.6(9) . . . . ? F7 Cr6 O24 C56 43.2(9) . . . . ? O27 Cr6 O24 C56 100(11) . . . . ? O25 Cr6 O24 C56 -132.9(10) . . . . ? O22 Cr6 O24 C56 -49.9(10) . . . . ? F1 Cr8 O33 C81 7.1(15) . . . . ? O32 Cr8 O33 C81 -169.4(15) . . . . ? F9 Cr8 O33 C81 97.1(15) . . . . ? O35 Cr8 O33 C81 -83.2(15) . . . . ? O30 Cr8 O33 C81 125(68) . . . . ? F2 Cr1 O34 C81 -120.4(9) . . . . ? O3 Cr1 O34 C81 146.1(9) . . . . ? O1 Cr1 O34 C81 38(4) . . . . ? F1 Cr1 O34 C81 -33.4(9) . . . . ? O36 Cr1 O34 C81 59.3(9) . . . . ? F1 Cr8 O35 C86 -44.0(19) . . . . ? O32 Cr8 O35 C86 137(2) . . . . ? F9 Cr8 O35 C86 -140(7) . . . . ? O33 Cr8 O35 C86 45.8(19) . . . . ? O30 Cr8 O35 C86 -134.4(19) . . . . ? F2 Cr1 O36 C86 -77(9) . . . . ? O3 Cr1 O36 C86 -176.5(12) . . . . ? O1 Cr1 O36 C86 91.1(12) . . . . ? F1 Cr1 O36 C86 1.6(12) . . . . ? O34 Cr1 O36 C86 -87.2(12) . . . . ? Cd9 O2 C1 O1 -39(2) . . . . ? Cd9 O2 C1 C2A 118.2(15) . . . . ? Cd9 O2 C1 C2 152.9(13) . . . . ? Cr1 O1 C1 O2 -10(2) . . . . ? Cr1 O1 C1 C2A -167.9(13) . . . . ? Cr1 O1 C1 C2 159.3(11) . . . . ? O2 C1 C2 C5 17(2) . . . . ? O1 C1 C2 C5 -153.3(15) . . . . ? C2A C1 C2 C5 107(3) . . . . ? O2 C1 C2 C4 -100.0(19) . . . . ? O1 C1 C2 C4 90.1(16) . . . . ? C2A C1 C2 C4 -10(3) . . . . ? O2 C1 C2 C3 141.4(18) . . . . ? O1 C1 C2 C3 -28(2) . . . . ? C2A C1 C2 C3 -128(3) . . . . ? O2 C1 C2A C5A 24(2) . . . . ? O1 C1 C2A C5A -174.7(17) . . . . ? C2 C1 C2A C5A -82(3) . . . . ? O2 C1 C2A C3A 143.8(18) . . . . ? O1 C1 C2A C3A -55(2) . . . . ? C2 C1 C2A C3A 37(2) . . . . ? O2 C1 C2A C4A -97.6(19) . . . . ? O1 C1 C2A C4A 63(2) . . . . ? C2 C1 C2A C4A 156(3) . . . . ? Cr1 O3 C6 O4 -27(2) . . . . ? Cr1 O3 C6 C7 157.2(10) . . . . ? Cd9 O4 C6 O3 -22(2) . . . . ? Cd9 O4 C6 C7 154.1(10) . . . . ? O3 C6 C7 C10 -170.1(15) . . . . ? O4 C6 C7 C10 14(2) . . . . ? O3 C6 C7 C9 -46.4(17) . . . . ? O4 C6 C7 C9 137.5(14) . . . . ? O3 C6 C7 C8 71.1(17) . . . . ? O4 C6 C7 C8 -105.1(15) . . . . ? Cr2 O6 C11 O5 -10(2) . . . . ? Cr2 O6 C11 C12A 161.4(12) . . . . ? Cr2 O6 C11 C12 176.9(9) . . . . ? Cd9 O5 C11 O6 -32(2) . . . . ? Cd9 O5 C11 C12A 156.1(12) . . . . ? Cd9 O5 C11 C12 140.6(11) . . . . ? O6 C11 C12 C15 39.3(19) . . . . ? O5 C11 C12 C15 -134.4(15) . . . . ? C12A C11 C12 C15 125(5) . . . . ? O6 C11 C12 C14 166.7(14) . . . . ? O5 C11 C12 C14 -7.1(18) . . . . ? C12A C11 C12 C14 -108(5) . . . . ? O6 C11 C12 C13 -76.4(16) . . . . ? O5 C11 C12 C13 109.8(15) . . . . ? C12A C11 C12 C13 9(5) . . . . ? O6 C11 C12A C15A 84.7(16) . . . . ? O5 C11 C12A C15A -102.3(16) . . . . ? C12 C11 C12A C15A -16(5) . . . . ? O6 C11 C12A C14A -158.9(14) . . . . ? O5 C11 C12A C14A 14(2) . . . . ? C12 C11 C12A C14A 100(5) . . . . ? O6 C11 C12A C13A -34(2) . . . . ? O5 C11 C12A C13A 139.4(16) . . . . ? C12 C11 C12A C13A -134(5) . . . . ? Cd9 O7 C16 O8 -41.6(17) . . . . ? Cd9 O7 C16 C17A 122.4(16) . . . . ? Cd9 O7 C16 C17 142.9(11) . . . . ? Cr2 O8 C16 O7 -11(2) . . . . ? Cr2 O8 C16 C17A -175.3(14) . . . . ? Cr2 O8 C16 C17 164.8(9) . . . . ? O7 C16 C17 C20 119.8(15) . . . . ? O8 C16 C17 C20 -56.2(15) . . . . ? C17A C16 C17 C20 -164(5) . . . . ? O7 C16 C17 C18 -3.5(17) . . . . ? O8 C16 C17 C18 -179.5(12) . . . . ? C17A C16 C17 C18 73(4) . . . . ? O7 C16 C17 C19 -120.2(14) . . . . ? O8 C16 C17 C19 63.8(14) . . . . ? C17A C16 C17 C19 -43(4) . . . . ? O7 C16 C17A C18A 40(2) . . . . ? O8 C16 C17A C18A -154.5(17) . . . . ? C17 C16 C17A C18A -74(4) . . . . ? O7 C16 C17A C19A -83(2) . . . . ? O8 C16 C17A C19A 82(2) . . . . ? C17 C16 C17A C19A 163(5) . . . . ? O7 C16 C17A C20A 157.8(17) . . . . ? O8 C16 C17A C20A -37(2) . . . . ? C17 C16 C17A C20A 44(4) . . . . ? Cr3 O10 C21 O9 -4.8(17) . . . . ? Cr3 O10 C21 C22A 179.8(9) . . . . ? Cr3 O10 C21 C22 170.4(8) . . . . ? Cr2 O9 C21 O10 -26.2(15) . . . . ? Cr2 O9 C21 C22A 149.7(8) . . . . ? Cr2 O9 C21 C22 159.0(9) . . . . ? O10 C21 C22 C23 -49.3(14) . . . . ? O9 C21 C22 C23 126.2(14) . . . . ? C22A C21 C22 C23 164(4) . . . . ? O10 C21 C22 C24 -172.3(11) . . . . ? O9 C21 C22 C24 3.1(16) . . . . ? C22A C21 C22 C24 41(4) . . . . ? O10 C21 C22 C25 70.6(13) . . . . ? O9 C21 C22 C25 -114.0(13) . . . . ? C22A C21 C22 C25 -76(4) . . . . ? O10 C21 C22A C24A 128.8(12) . . . . ? O9 C21 C22A C24A -47.3(13) . . . . ? C22 C21 C22A C24A 166(4) . . . . ? O10 C21 C22A C23A -110.3(12) . . . . ? O9 C21 C22A C23A 73.6(12) . . . . ? C22 C21 C22A C23A -73(4) . . . . ? O10 C21 C22A C25A 7.4(15) . . . . ? O9 C21 C22A C25A -168.6(10) . . . . ? C22 C21 C22A C25A 45(4) . . . . ? Cr2 O11 C26 O12 -11(2) . . . . ? Cr2 O11 C26 C27 177.4(10) . . . . ? Cr2 O11 C26 C27A 165.1(10) . . . . ? Cr3 O12 C26 O11 -21.3(17) . . . . ? Cr3 O12 C26 C27 150.5(10) . . . . ? Cr3 O12 C26 C27A 162.5(10) . . . . ? O11 C26 C27 C30 -170.2(15) . . . . ? O12 C26 C27 C30 17.9(18) . . . . ? C27A C26 C27 C30 -115(5) . . . . ? O11 C26 C27 C29 -50.3(16) . . . . ? O12 C26 C27 C29 137.8(12) . . . . ? C27A C26 C27 C29 5(4) . . . . ? O11 C26 C27 C28 66.3(18) . . . . ? O12 C26 C27 C28 -105.6(14) . . . . ? C27A C26 C27 C28 121(5) . . . . ? O11 C26 C27A C29A -59.4(14) . . . . ? O12 C26 C27A C29A 117.2(14) . . . . ? C27 C26 C27A C29A 170(5) . . . . ? O11 C26 C27A C28A 60.1(15) . . . . ? O12 C26 C27A C28A -123.3(13) . . . . ? C27 C26 C27A C28A -71(5) . . . . ? O11 C26 C27A C30A 179.0(12) . . . . ? O12 C26 C27A C30A -4.4(17) . . . . ? C27 C26 C27A C30A 48(5) . . . . ? Cr3 O15 C31 O16 -15.6(19) . . . . ? Cr3 O15 C31 C32A 161.8(10) . . . . ? Cr3 O15 C31 C32 170.0(13) . . . . ? Cr4 O16 C31 O15 -20(2) . . . . ? Cr4 O16 C31 C32A 162.6(11) . . . . ? Cr4 O16 C31 C32 154.6(12) . . . . ? O15 C31 C32 C35 152.1(16) . . . . ? O16 C31 C32 C35 -23(2) . . . . ? C32A C31 C32 C35 -164(8) . . . . ? O15 C31 C32 C33 26(2) . . . . ? O16 C31 C32 C33 -149.3(15) . . . . ? C32A C31 C32 C33 69(7) . . . . ? O15 C31 C32 C34 -89.9(17) . . . . ? O16 C31 C32 C34 95.1(16) . . . . ? C32A C31 C32 C34 -46(7) . . . . ? O15 C31 C32A C34A -57.0(15) . . . . ? O16 C31 C32A C34A 120.6(15) . . . . ? C32 C31 C32A C34A 163(8) . . . . ? O15 C31 C32A C33A 63.1(16) . . . . ? O16 C31 C32A C33A -119.3(14) . . . . ? C32 C31 C32A C33A -77(7) . . . . ? O15 C31 C32A C35A -178.3(13) . . . . ? O16 C31 C32A C35A -0.7(18) . . . . ? C32 C31 C32A C35A 42(7) . . . . ? Cr4 O14 C36 O13 -12.7(15) . . . . ? Cr4 O14 C36 C37 169.6(7) . . . . ? Cr3 O13 C36 O14 -22.9(17) . . . . ? Cr3 O13 C36 C37 154.8(8) . . . . ? O14 C36 C37 C39 115.1(13) . . . . ? O13 C36 C37 C39 -62.8(14) . . . . ? O14 C36 C37 C38 -127.6(12) . . . . ? O13 C36 C37 C38 54.6(14) . . . . ? O14 C36 C37 C40 -9.1(16) . . . . ? O13 C36 C37 C40 173.0(11) . . . . ? Cr4 O17 C41 O18 19.2(16) . . . . ? Cr4 O17 C41 C42A -164.1(7) . . . . ? Cr5 O18 C41 O17 20.9(14) . . . . ? Cr5 O18 C41 C42A -155.9(7) . . . . ? O17 C41 C42A C44A 134.8(10) . . . . ? O18 C41 C42A C44A -48.2(12) . . . . ? O17 C41 C42A C45A 11.1(13) . . . . ? O18 C41 C42A C45A -171.9(9) . . . . ? O17 C41 C42A C43A -106.7(11) . . . . ? O18 C41 C42A C43A 70.3(11) . . . . ? Cr4 O19 C46 O20 16.2(17) . . . . ? Cr4 O19 C46 C47A -161.5(10) . . . . ? Cr4 O19 C46 C47 -163.6(11) . . . . ? Cr5 O20 C46 O19 28.4(17) . . . . ? Cr5 O20 C46 C47A -154.0(11) . . . . ? Cr5 O20 C46 C47 -151.8(10) . . . . ? O19 C46 C47 C49 62.3(16) . . . . ? O20 C46 C47 C49 -117.5(13) . . . . ? C47A C46 C47 C49 51(7) . . . . ? O19 C46 C47 C48 -175.5(13) . . . . ? O20 C46 C47 C48 4.7(17) . . . . ? C47A C46 C47 C48 173(8) . . . . ? O19 C46 C47 C50 -53.4(17) . . . . ? O20 C46 C47 C50 126.8(13) . . . . ? C47A C46 C47 C50 -64(7) . . . . ? O19 C46 C47A C50A -28.7(18) . . . . ? O20 C46 C47A C50A 153.6(15) . . . . ? C47 C46 C47A C50A 141(8) . . . . ? O19 C46 C47A C49A 92.7(16) . . . . ? O20 C46 C47A C49A -85.0(18) . . . . ? C47 C46 C47A C49A -97(8) . . . . ? O19 C46 C47A C48A -149.2(15) . . . . ? O20 C46 C47A C48A 33.0(18) . . . . ? C47 C46 C47A C48A 21(7) . . . . ? Cr5 O21 C51 O22 -11(2) . . . . ? Cr5 O21 C51 C52A 173.9(9) . . . . ? Cr5 O21 C51 C52 159.5(17) . . . . ? Cr6 O22 C51 O21 -26(2) . . . . ? Cr6 O22 C51 C52A 148.7(9) . . . . ? Cr6 O22 C51 C52 160.8(13) . . . . ? O21 C51 C52 C55 -102(2) . . . . ? O22 C51 C52 C55 70.0(19) . . . . ? C52A C51 C52 C55 -147(5) . . . . ? O21 C51 C52 C54 13(2) . . . . ? O22 C51 C52 C54 -174.3(16) . . . . ? C52A C51 C52 C54 -31(4) . . . . ? O21 C51 C52 C53 130(2) . . . . ? O22 C51 C52 C53 -58(2) . . . . ? C52A C51 C52 C53 85(4) . . . . ? O21 C51 C52A C55A -74.2(15) . . . . ? O22 C51 C52A C55A 110.5(13) . . . . ? C52 C51 C52A C55A 70(4) . . . . ? O21 C51 C52A C54A 44.5(16) . . . . ? O22 C51 C52A C54A -130.9(12) . . . . ? C52 C51 C52A C54A -171(4) . . . . ? O21 C51 C52A C53A 167.5(13) . . . . ? O22 C51 C52A C53A -7.9(15) . . . . ? C52 C51 C52A C53A -48(4) . . . . ? Cr6 O24 C56 O23 -4.6(17) . . . . ? Cr6 O24 C56 C57 172.9(8) . . . . ? Cr6 O24 C56 C57A -178.5(10) . . . . ? Cr5 O23 C56 O24 -30.0(18) . . . . ? Cr5 O23 C56 C57 152.7(10) . . . . ? Cr5 O23 C56 C57A 144.2(11) . . . . ? O24 C56 C57 C59 70.1(14) . . . . ? O23 C56 C57 C59 -112.2(13) . . . . ? C57A C56 C57 C59 -68(6) . . . . ? O24 C56 C57 C60 -49.9(14) . . . . ? O23 C56 C57 C60 127.9(13) . . . . ? C57A C56 C57 C60 172(7) . . . . ? O24 C56 C57 C58 -171.0(11) . . . . ? O23 C56 C57 C58 6.7(15) . . . . ? C57A C56 C57 C58 51(6) . . . . ? O24 C56 C57A C58A -156.2(14) . . . . ? O23 C56 C57A C58A 29.0(15) . . . . ? C57 C56 C57A C58A -111(6) . . . . ? O24 C56 C57A C59A 83.7(16) . . . . ? O23 C56 C57A C59A -91.0(14) . . . . ? C57 C56 C57A C59A 129(7) . . . . ? O24 C56 C57A C60A -35.0(18) . . . . ? O23 C56 C57A C60A 150.3(13) . . . . ? C57 C56 C57A C60A 10(6) . . . . ? F8 Cr6 O25 C61A 8(3) . . . . ? F7 Cr6 O25 C61A -125(4) . . . . ? O27 Cr6 O25 C61A 98(3) . . . . ? O22 Cr6 O25 C61A -176(3) . . . . ? O24 Cr6 O25 C61A -81(3) . . . . ? F8 Cr6 O25 C61 -43.7(12) . . . . ? F7 Cr6 O25 C61 -177(3) . . . . ? O27 Cr6 O25 C61 45.7(12) . . . . ? O22 Cr6 O25 C61 131.9(12) . . . . ? O24 Cr6 O25 C61 -132.8(12) . . . . ? O29 Cr7 O26 C61 75.9(13) . . . . ? F9 Cr7 O26 C61 -161.8(14) . . . . ? F8 Cr7 O26 C61 -15.6(13) . . . . ? O31A Cr7 O26 C61 142.0(15) . . . . ? O28 Cr7 O26 C61 -104.7(12) . . . . ? O31 Cr7 O26 C61 173.6(13) . . . . ? O26A Cr7 O26 C61 47.6(14) . . . . ? Cr7 O26 C61 O25 28(2) . . . . ? Cr7 O26 C61 C62 -156.4(10) . . . . ? C61A O25 C61 O26 -107(3) . . . . ? Cr6 O25 C61 O26 9(3) . . . . ? C61A O25 C61 C62 78(2) . . . . ? Cr6 O25 C61 C62 -165.7(10) . . . . ? O26 C61 C62 C64 -115.1(15) . . . . ? O25 C61 C62 C64 60.8(18) . . . . ? O26 C61 C62 C65 127.6(14) . . . . ? O25 C61 C62 C65 -56.5(18) . . . . ? O26 C61 C62 C63 6.1(19) . . . . ? O25 C61 C62 C63 -178.0(14) . . . . ? O29 Cr7 O26A C61A 152(4) . . . . ? F9 Cr7 O26A C61A 132(4) . . . . ? F8 Cr7 O26A C61A 57(4) . . . . ? O26 Cr7 O26A C61A -60(4) . . . . ? O31A Cr7 O26A C61A -136(4) . . . . ? O28 Cr7 O26A C61A -28(4) . . . . ? O31 Cr7 O26A C61A -116(4) . . . . ? C61 O25 C61A O26A 78(4) . . . . ? Cr6 O25 C61A O26A -23(6) . . . . ? C61 O25 C61A C62A -96(3) . . . . ? Cr6 O25 C61A C62A 163.5(15) . . . . ? Cr7 O26A C61A O25 -21(6) . . . . ? Cr7 O26A C61A C62A 151(3) . . . . ? O25 C61A C62A C64A 8(5) . . . . ? O26A C61A C62A C64A -164(4) . . . . ? O25 C61A C62A C65A -112(3) . . . . ? O26A C61A C62A C65A 76(6) . . . . ? O25 C61A C62A C63A 137(3) . . . . ? O26A C61A C62A C63A -35(6) . . . . ? F8 Cr6 O27 C66 16.5(11) . . . . ? F7 Cr6 O27 C66 108.9(11) . . . . ? O25 Cr6 O27 C66 -74.9(11) . . . . ? O22 Cr6 O27 C66 -157.9(11) . . . . ? O24 Cr6 O27 C66 52(11) . . . . ? O29 Cr7 O28 C66 143(99) . . . . ? F9 Cr7 O28 C66 -132.4(11) . . . . ? F8 Cr7 O28 C66 -41.4(11) . . . . ? O26 Cr7 O28 C66 57.5(11) . . . . ? O31A Cr7 O28 C66 127.8(12) . . . . ? O31 Cr7 O28 C66 140.4(12) . . . . ? O26A Cr7 O28 C66 38.1(14) . . . . ? Cr7 O28 C66 O27 21(2) . . . . ? Cr7 O28 C66 C67A -154(2) . . . . ? Cr7 O28 C66 C67 -167.2(8) . . . . ? Cr6 O27 C66 O28 -5(2) . . . . ? Cr6 O27 C66 C67A 168(2) . . . . ? Cr6 O27 C66 C67 -177.1(7) . . . . ? O28 C66 C67 C70 -144.3(11) . . . . ? O27 C66 C67 C70 28.8(13) . . . . ? C67A C66 C67 C70 175(5) . . . . ? O28 C66 C67 C69 -19.4(14) . . . . ? O27 C66 C67 C69 153.7(10) . . . . ? C67A C66 C67 C69 -61(5) . . . . ? O28 C66 C67 C68 98.7(12) . . . . ? O27 C66 C67 C68 -88.3(11) . . . . ? C67A C66 C67 C68 58(5) . . . . ? O28 C66 C67A C68A 93(4) . . . . ? O27 C66 C67A C68A -81(4) . . . . ? C67 C66 C67A C68A -124(7) . . . . ? O28 C66 C67A C70A -140(2) . . . . ? O27 C66 C67A C70A 46(3) . . . . ? C67 C66 C67A C70A 3(5) . . . . ? O28 C66 C67A C69A -30(2) . . . . ? O27 C66 C67A C69A 156(3) . . . . ? C67 C66 C67A C69A 113(6) . . . . ? F9 Cr7 O29 C71 -4.7(16) . . . . ? F8 Cr7 O29 C71 -95.7(16) . . . . ? O26 Cr7 O29 C71 165.4(16) . . . . ? O31A Cr7 O29 C71 95.1(17) . . . . ? O28 Cr7 O29 C71 80(49) . . . . ? O31 Cr7 O29 C71 82.5(17) . . . . ? O26A Cr7 O29 C71 -174.8(19) . . . . ? F1 Cr8 O30 C71 118.3(13) . . . . ? O32 Cr8 O30 C71 -65.3(13) . . . . ? F9 Cr8 O30 C71 28.2(13) . . . . ? O33 Cr8 O30 C71 1(69) . . . . ? O35 Cr8 O30 C71 -151.5(13) . . . . ? Cr8 O30 C71 O29 3(2) . . . . ? Cr8 O30 C71 C72A 174.8(15) . . . . ? Cr8 O30 C71 C72 -179.4(11) . . . . ? Cr7 O29 C71 O30 -20(2) . . . . ? Cr7 O29 C71 C72A 166.7(15) . . . . ? Cr7 O29 C71 C72 162.5(13) . . . . ? O30 C71 C72 C73 23(2) . . . . ? O29 C71 C72 C73 -159.0(14) . . . . ? C72A C71 C72 C73 173(10) . . . . ? O30 C71 C72 C75 -99.2(17) . . . . ? O29 C71 C72 C75 78.3(17) . . . . ? C72A C71 C72 C75 50(10) . . . . ? O30 C71 C72 C74 143.3(15) . . . . ? O29 C71 C72 C74 -39.3(17) . . . . ? C72A C71 C72 C74 -67(10) . . . . ? O30 C71 C72A C73A -4(2) . . . . ? O29 C71 C72A C73A 168.5(16) . . . . ? C72 C71 C72A C73A -38(10) . . . . ? O30 C71 C72A C75A -119(2) . . . . ? O29 C71 C72A C75A 53(2) . . . . ? C72 C71 C72A C75A -154(11) . . . . ? O30 C71 C72A C74A 109(2) . . . . ? O29 C71 C72A C74A -78.3(19) . . . . ? C72 C71 C72A C74A 75(10) . . . . ? F1 Cr8 O32 C76 177(100) . . . . ? F9 Cr8 O32 C76 9.6(19) . . . . ? O33 Cr8 O32 C76 -81.2(19) . . . . ? O35 Cr8 O32 C76 -173.8(19) . . . . ? O30 Cr8 O32 C76 98.4(19) . . . . ? F1 Cr8 O32 C76A 152(6) . . . . ? F9 Cr8 O32 C76A -15(3) . . . . ? O33 Cr8 O32 C76A -106(3) . . . . ? O35 Cr8 O32 C76A 161(4) . . . . ? O30 Cr8 O32 C76A 73(3) . . . . ? O29 Cr7 O31 C76 -38.8(19) . . . . ? F9 Cr7 O31 C76 51.3(19) . . . . ? F8 Cr7 O31 C76 130(3) . . . . ? O26 Cr7 O31 C76 -133.6(19) . . . . ? O31A Cr7 O31 C76 -61(2) . . . . ? O28 Cr7 O31 C76 141.2(19) . . . . ? O26A Cr7 O31 C76 -102(2) . . . . ? Cr7 O31 C76 O32 -22(3) . . . . ? Cr7 O31 C76 C77 154.2(12) . . . . ? C76A O32 C76 O31 75(6) . . . . ? Cr8 O32 C76 O31 -17(4) . . . . ? C76A O32 C76 C77 -102(7) . . . . ? Cr8 O32 C76 C77 166.0(10) . . . . ? O31 C76 C77 C78 71(2) . . . . ? O32 C76 C77 C78 -111.9(18) . . . . ? O31 C76 C77 C79 -46(2) . . . . ? O32 C76 C77 C79 131.1(17) . . . . ? O31 C76 C77 C80 -168.9(18) . . . . ? O32 C76 C77 C80 8(2) . . . . ? O29 Cr7 O31A C76A -111(3) . . . . ? F9 Cr7 O31A C76A -24(3) . . . . ? F8 Cr7 O31A C76A -140(2) . . . . ? O26 Cr7 O31A C76A 146(3) . . . . ? O28 Cr7 O31A C76A 69(3) . . . . ? O31 Cr7 O31A C76A 45(2) . . . . ? O26A Cr7 O31A C76A -174(3) . . . . ? Cr7 O31A C76A O32 55(6) . . . . ? Cr7 O31A C76A C77A -143(2) . . . . ? C76 O32 C76A O31A -138(11) . . . . ? Cr8 O32 C76A O31A -33(7) . . . . ? C76 O32 C76A C77A 65(4) . . . . ? Cr8 O32 C76A C77A 170(3) . . . . ? O31A C76A C77A C79A 76(4) . . . . ? O32 C76A C77A C79A -123(5) . . . . ? O31A C76A C77A C80A -47(4) . . . . ? O32 C76A C77A C80A 114(5) . . . . ? O31A C76A C77A C78A -164(3) . . . . ? O32 C76A C77A C78A -3(6) . . . . ? Cr1 O34 C81 O33 6.2(17) . . . . ? Cr1 O34 C81 C82 -171.8(7) . . . . ? Cr8 O33 C81 O34 12(2) . . . . ? Cr8 O33 C81 C82 -169.9(11) . . . . ? O34 C81 C82 C85 -135.0(11) . . . . ? O33 C81 C82 C85 46.9(15) . . . . ? O34 C81 C82 C84 -10.9(15) . . . . ? O33 C81 C82 C84 171.0(11) . . . . ? O34 C81 C82 C83 107.4(11) . . . . ? O33 C81 C82 C83 -70.7(14) . . . . ? Cr8 O35 C86 O36 21(3) . . . . ? Cr8 O35 C86 C87 -150.9(14) . . . . ? Cr8 O35 C86 C87A -168.9(14) . . . . ? Cr1 O36 C86 O35 6(2) . . . . ? Cr1 O36 C86 C87 178.7(9) . . . . ? Cr1 O36 C86 C87A -163.9(10) . . . . ? O35 C86 C87 C89 9(2) . . . . ? O36 C86 C87 C89 -164.0(12) . . . . ? C87A C86 C87 C89 121(4) . . . . ? O35 C86 C87 C88 134.2(16) . . . . ? O36 C86 C87 C88 -38.5(18) . . . . ? C87A C86 C87 C88 -113(4) . . . . ? O35 C86 C87 C90 -109.1(16) . . . . ? O36 C86 C87 C90 78.1(15) . . . . ? C87A C86 C87 C90 3(3) . . . . ? O35 C86 C87A C89A -8(2) . . . . ? O36 C86 C87A C89A 162.9(14) . . . . ? C87 C86 C87A C89A -84(4) . . . . ? O35 C86 C87A C90A -129.9(18) . . . . ? O36 C86 C87A C90A 40.5(18) . . . . ? C87 C86 C87A C90A 153(4) . . . . ? O35 C86 C87A C88A 110.1(19) . . . . ? O36 C86 C87A C88A -79.5(16) . . . . ? C87 C86 C87A C88A 33(3) . . . . ? C103 N1 C100 C101 -108.2(11) . . . . ? C103 N1 C100 C102 129.4(10) . . . . ? C100 N1 C103 C104 58.3(12) . . . . ? C100 N1 C103 C105 -63.5(12) . . . . ? C100 N1 C103 C106 178.1(9) . . . . ? _diffrn_measured_fraction_theta_max .997 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full .997 _refine_diff_density_max 1.911 _refine_diff_density_min -2.093 _refine_diff_density_rms .163 data_orepw15absmonoc _database_code_depnum_ccdc_archive 'CCDC 268357' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H200 Cr9 F12 N Ni O40' _chemical_formula_weight 2859.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr .3209 .6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni .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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 19.9340(12) _cell_length_b 16.0192(11) _cell_length_c 26.2060(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.054(5) _cell_angle_gamma 90.00 _cell_volume 8368.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 24323 _cell_measurement_theta_min 2.7385 _cell_measurement_theta_max 32.0824 _exptl_crystal_description Primatic _exptl_crystal_colour Green _exptl_crystal_size_max 0.32504 _exptl_crystal_size_mid 0.25396 _exptl_crystal_size_min 0.15622 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3004 _exptl_absorpt_coefficient_mu 0.742 _exptl_absorpt_correction_T_min 0.7945 _exptl_absorpt_correction_T_max 0.8929 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.pre23_9 beta (release 18.06.2004 CrysAlis171 .NET) (compiled Jun 18 2004,12:34:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39596 _diffrn_reflns_av_R_equivalents 0.1007 _diffrn_reflns_av_sigmaI/netI 0.0735 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 21.95 _reflns_number_total 10157 _reflns_number_gt 6912 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Limited data range hindered complete structure solution. Molecular formula is missing Nitrogen and Hydrogen. Amine group could not be modeled in any space group, position of N and Me group could not be determined. Due to poor modelling of amine it has been left isotropic. Solvent molecules have been left isotropic. Hydrogens not placed on any atom. Cr4 and Cr5 disordered with Ni1 and Ni2, unable to determine actual site due to symmetry. Formula doesn't match due to missing N, C and H. Solvent molecules not modeled due to poor quality of data. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10157 _refine_ls_number_parameters 996 _refine_ls_number_restraints 1318 _refine_ls_R_factor_all 0.1660 _refine_ls_R_factor_gt 0.1438 _refine_ls_wR_factor_ref 0.3912 _refine_ls_wR_factor_gt 0.3641 _refine_ls_goodness_of_fit_ref 1.474 _refine_ls_restrained_S_all 1.405 _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 0.72493(12) 0.51743(15) -0.05682(9) 0.0448(7) Uani 0.25 1 d P . . Ni2 Ni 0.72474(12) 0.52029(15) 0.05625(9) 0.0451(7) Uani 0.25 1 d P . . Cr5 Cr 0.72493(12) 0.51743(15) -0.05682(9) 0.0448(7) Uani 0.75 1 d P . . Cr4 Cr 0.72474(12) 0.52029(15) 0.05625(9) 0.0451(7) Uani 0.75 1 d P . . Cr1 Cr 0.65789(13) 0.52031(17) 0.17218(11) 0.0523(8) Uani 1 1 d . . . Cr2 Cr 0.50184(17) 0.49901(17) 0.22007(6) 0.0429(6) Uani 1 1 d . . . Cr3 Cr 0.34444(14) 0.49873(17) 0.17326(12) 0.0562(9) Uani 1 1 d . . . F1 F 0.7861(3) 0.4974(5) 0.0003(5) 0.0582(19) Uani 1 1 d . . . F2 F 0.6614(3) 0.5089(4) -0.0004(5) 0.0449(16) Uani 1 1 d . . . F3 F 0.6544(4) 0.5492(5) 0.1029(3) 0.043(2) Uani 1 1 d . . . F4 F 0.5671(4) 0.4776(4) 0.1689(3) 0.041(2) Uani 1 1 d . . . F5 F 0.4367(4) 0.5281(5) 0.1690(3) 0.045(2) Uani 1 1 d . . . F6 F 0.3476(4) 0.4592(5) 0.1040(3) 0.046(2) Uani 1 1 d . . . O1 O 0.7181(6) 0.3995(7) -0.0719(4) 0.065(3) Uani 1 1 d . . . O2 O 0.3209(6) 0.6138(7) 0.1518(4) 0.076(4) Uani 1 1 d . A . O3 O 0.7311(6) 0.6392(6) -0.0446(4) 0.063(3) Uani 1 1 d . B . O4 O 0.7326(5) 0.6415(7) 0.0412(4) 0.050(3) Uani 1 1 d . B . O5 O 0.7989(5) 0.5321(7) 0.1068(4) 0.052(3) Uani 1 1 d . C . O6 O 0.7497(5) 0.5675(8) 0.1790(4) 0.069(3) Uani 1 1 d . C . O7 O 0.7159(5) 0.4038(7) 0.0734(4) 0.054(3) Uani 1 1 d . D . O8 O 0.6914(6) 0.4109(7) 0.1568(4) 0.062(3) Uani 1 1 d . D . O9 O 0.6684(6) 0.4930(8) 0.2456(5) 0.081(4) Uani 1 1 d . E . O10 O 0.5646(6) 0.4703(9) 0.2736(4) 0.078(4) Uani 1 1 d . E . O11 O 0.6257(5) 0.6324(6) 0.1883(4) 0.062(3) Uani 1 1 d . F . O12 O 0.5291(5) 0.6144(6) 0.2263(5) 0.065(3) Uani 1 1 d . F . O13 O 0.4776(5) 0.3809(7) 0.2131(5) 0.069(3) Uani 1 1 d . G . O14 O 0.3647(6) 0.3884(6) 0.1965(4) 0.058(3) Uani 1 1 d . G . O15 O 0.4385(7) 0.5165(8) 0.2757(5) 0.068(4) Uani 1 1 d . H . O16 O 0.3408(6) 0.5372(9) 0.2432(4) 0.072(4) Uani 1 1 d . H . O17 O 0.2536(6) 0.4689(10) 0.1800(5) 0.093(5) Uani 1 1 d . . . O18 O 0.7953(6) 0.5313(8) -0.1039(5) 0.067(4) Uani 1 1 d . . . C1 C 0.2986(8) 0.6419(10) 0.1124(6) 0.070(4) Uani 1 1 d DU . . C2 C 0.2489(11) 0.7099(13) 0.1259(8) 0.084(5) Uani 0.35 1 d PDU A 1 C3 C 0.277(2) 0.7702(18) 0.1652(14) 0.087(6) Uani 0.35 1 d PDU A 1 C4 C 0.1846(13) 0.674(3) 0.1483(16) 0.098(7) Uani 0.35 1 d PDU A 1 C5 C 0.229(2) 0.761(2) 0.0795(13) 0.087(6) Uani 0.35 1 d PDU A 1 C2A C 0.2746(8) 0.7317(10) 0.1109(5) 0.082(4) Uani 0.65 1 d PDU A 2 C3A C 0.3078(12) 0.7847(11) 0.1518(8) 0.086(6) Uani 0.65 1 d PDU A 2 C4A C 0.1989(10) 0.7367(15) 0.1193(9) 0.100(5) Uani 0.65 1 d PDU A 2 C5A C 0.2887(14) 0.7730(13) 0.0598(8) 0.102(6) Uani 0.65 1 d PDU A 2 C6 C 0.7355(7) 0.6770(8) -0.0001(8) 0.062(3) Uani 1 1 d DU . . C7 C 0.7676(13) 0.7621(11) -0.0045(10) 0.068(4) Uani 0.40 1 d PDU B 1 C8 C 0.7307(18) 0.811(2) -0.0484(12) 0.064(6) Uani 0.40 1 d PDU B 1 C9 C 0.8437(14) 0.752(2) -0.0184(14) 0.078(6) Uani 0.40 1 d PDU B 1 C10 C 0.7603(19) 0.811(2) 0.0469(12) 0.070(6) Uani 0.40 1 d PDU B 1 C7A C 0.7409(8) 0.7716(8) -0.0003(8) 0.068(4) Uani 0.60 1 d PDU B 2 C8A C 0.6994(12) 0.8006(18) -0.0484(9) 0.070(6) Uani 0.60 1 d PDU B 2 C9A C 0.8167(10) 0.7973(18) -0.0079(10) 0.083(5) Uani 0.60 1 d PDU B 2 C10A C 0.7128(12) 0.8170(15) 0.0484(9) 0.068(5) Uani 0.60 1 d PDU B 2 C11 C 0.8012(7) 0.5545(11) 0.1540(7) 0.061(3) Uani 1 1 d DU . . C12 C 0.8710(7) 0.5786(10) 0.1722(6) 0.063(3) Uani 0.70 1 d PDU C 1 C13 C 0.9186(10) 0.6189(13) 0.1345(8) 0.067(4) Uani 0.70 1 d PDU C 1 C14 C 0.8956(12) 0.4930(12) 0.1873(10) 0.080(5) Uani 0.70 1 d PDU C 1 C15 C 0.8613(11) 0.6339(14) 0.2184(8) 0.080(4) Uani 0.70 1 d PDU C 1 C12A C 0.8667(10) 0.571(2) 0.1813(11) 0.066(4) Uani 0.30 1 d PDU C 2 C13A C 0.875(2) 0.664(2) 0.1788(18) 0.072(5) Uani 0.30 1 d PDU C 2 C14A C 0.917(2) 0.526(3) 0.1490(16) 0.066(5) Uani 0.30 1 d PDU C 2 C15A C 0.866(2) 0.539(3) 0.2353(14) 0.071(5) Uani 0.30 1 d PDU C 2 C16 C 0.7103(8) 0.3672(9) 0.1140(6) 0.071(4) Uani 1 1 d DU . . C17 C 0.7143(8) 0.2750(10) 0.1260(6) 0.072(4) Uani 0.60 1 d PDU D 1 C18 C 0.7718(13) 0.2650(15) 0.1676(9) 0.096(6) Uani 0.60 1 d PDU D 1 C19 C 0.7317(13) 0.2283(12) 0.0748(9) 0.084(6) Uani 0.60 1 d PDU D 1 C20 C 0.6432(12) 0.2491(14) 0.1481(10) 0.091(5) Uani 0.60 1 d PDU D 1 C17A C 0.6693(11) 0.2897(11) 0.1250(8) 0.081(4) Uani 0.40 1 d PDU D 2 C18A C 0.7092(19) 0.2380(16) 0.1665(12) 0.088(6) Uani 0.40 1 d PDU D 2 C19A C 0.662(2) 0.2409(16) 0.0728(13) 0.094(6) Uani 0.40 1 d PDU D 2 C20A C 0.5991(12) 0.321(2) 0.1459(15) 0.095(6) Uani 0.40 1 d PDU D 2 C21 C 0.6254(9) 0.4699(10) 0.2790(6) 0.050(3) Uani 1 1 d U . . C22 C 0.6544(10) 0.4451(12) 0.3285(9) 0.057(3) Uani 0.50 1 d PDU E 1 C23 C 0.7151(13) 0.3829(16) 0.3201(12) 0.069(5) Uani 0.50 1 d PDU E 1 C24 C 0.6007(14) 0.4091(17) 0.3674(12) 0.065(5) Uani 0.50 1 d PDU E 1 C25 C 0.6788(15) 0.5358(14) 0.3441(12) 0.068(5) Uani 0.50 1 d PDU E 1 C22A C 0.6542(10) 0.4542(11) 0.3316(9) 0.060(3) Uani 0.50 1 d PDU E 2 C23A C 0.7330(11) 0.4423(16) 0.3296(12) 0.061(3) Uani 0.50 1 d PDU E 2 C24A C 0.6171(13) 0.3745(14) 0.3536(12) 0.061(3) Uani 0.50 1 d PDU E 2 C25A C 0.6334(14) 0.5370(14) 0.3609(12) 0.061(3) Uani 0.50 1 d PDU E 2 C26 C 0.5774(8) 0.6610(9) 0.2100(5) 0.047(3) Uani 1 1 d U . . C27 C 0.5620(9) 0.7533(13) 0.2253(6) 0.059(3) Uani 0.60 1 d PDU F 1 C28 C 0.5650(12) 0.7516(16) 0.2814(7) 0.065(5) Uani 0.60 1 d PDU F 1 C29 C 0.4947(11) 0.7768(15) 0.2073(8) 0.067(4) Uani 0.60 1 d PDU F 1 C30 C 0.6142(11) 0.8071(16) 0.2036(8) 0.060(5) Uani 0.60 1 d PDU F 1 C27A C 0.5661(13) 0.7592(17) 0.2049(9) 0.059(3) Uani 0.40 1 d PDU F 2 C28A C 0.5456(17) 0.789(2) 0.2557(10) 0.059(3) Uani 0.40 1 d PDU F 2 C29A C 0.5129(16) 0.773(2) 0.1667(11) 0.059(3) Uani 0.40 1 d PDU F 2 C30A C 0.6300(15) 0.796(3) 0.1887(13) 0.059(3) Uani 0.40 1 d PDU F 2 C31 C 0.4222(11) 0.3469(9) 0.2080(6) 0.070(3) Uani 1 1 d DU . . C32 C 0.4181(10) 0.2580(10) 0.2257(6) 0.079(4) Uani 0.60 1 d PDU G 1 C33 C 0.4285(15) 0.2531(19) 0.2856(8) 0.095(6) Uani 0.60 1 d PDU G 1 C34 C 0.4750(13) 0.2077(17) 0.1972(10) 0.088(5) Uani 0.60 1 d PDU G 1 C35 C 0.3463(12) 0.2234(16) 0.2107(9) 0.079(5) Uani 0.60 1 d PDU G 1 C32A C 0.4106(15) 0.2544(10) 0.2113(9) 0.077(3) Uani 0.40 1 d PDU G 2 C33A C 0.3548(18) 0.245(2) 0.2540(12) 0.077(3) Uani 0.40 1 d PDU G 2 C34A C 0.4773(16) 0.209(2) 0.2283(13) 0.077(3) Uani 0.40 1 d PDU G 2 C35A C 0.3843(19) 0.218(2) 0.1588(11) 0.077(3) Uani 0.40 1 d PDU G 2 C36 C 0.3768(11) 0.5379(10) 0.2767(6) 0.057(3) Uani 1 1 d DU . . C37 C 0.3488(12) 0.5602(14) 0.3279(7) 0.063(3) Uani 0.40 1 d PDU H 1 C38 C 0.2768(15) 0.521(2) 0.3335(13) 0.071(6) Uani 0.40 1 d PDU H 1 C39 C 0.3433(18) 0.6579(15) 0.3271(12) 0.067(5) Uani 0.40 1 d PDU H 1 C40 C 0.3930(17) 0.533(2) 0.3745(12) 0.070(5) Uani 0.40 1 d PDU H 1 C37A C 0.3593(9) 0.5526(10) 0.3317(5) 0.066(3) Uani 0.60 1 d PDU H 2 C38A C 0.3567(12) 0.4686(12) 0.3627(9) 0.066(3) Uani 0.60 1 d PDU H 2 C39A C 0.2873(11) 0.5929(14) 0.3316(9) 0.066(3) Uani 0.60 1 d PDU H 2 C40A C 0.4095(11) 0.6137(14) 0.3589(9) 0.066(3) Uani 0.60 1 d PDU H 2 C41 C 0.7973(7) 0.5417(10) -0.1494(6) 0.068(4) Uani 1 1 d DU . . C42 C 0.8601(7) 0.5651(7) -0.1777(5) 0.083(4) Uani 1 1 d DU . . C43 C 0.9080(8) 0.6130(12) -0.1414(8) 0.111(6) Uani 1 1 d DU . . C44 C 0.8405(10) 0.6215(13) -0.2237(7) 0.131(6) Uani 1 1 d DU . . C45 C 0.8942(10) 0.4843(13) -0.1973(9) 0.124(6) Uani 1 1 d DU . . C50 C 0.5179(12) 0.5520(15) 0.0029(8) 0.137(8) Uiso 1 1 d D . . C51 C 0.4884(13) 0.5569(14) 0.0697(8) 0.114(7) Uiso 1 1 d D . . C52 C 0.4777(18) 0.6695(14) 0.0836(12) 0.180(13) Uiso 1 1 d D . . C53 C 0.490(3) 0.763(2) 0.0434(15) 0.186(19) Uiso 0.70 1 d PD . . C54 C 0.503(3) 0.709(3) -0.0184(18) 0.33(3) Uiso 1 1 d D . . C55 C 0.4641(14) 0.6116(16) -0.0415(10) 0.137(9) Uiso 1 1 d D . . O51 O 0.444(2) 0.529(2) 0.504(2) 0.36(2) Uiso 1 1 d . . . C54A C 0.5599(13) 0.6758(16) -0.0010(16) 0.013(6) Uiso 0.30 1 d P . . O52 O 0.500(5) -0.002(3) 0.104(2) 0.45(3) Uiso 1 1 d . . . C60 C 0.419(4) 0.019(3) 0.080(2) 0.30(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0249(13) 0.0726(17) 0.0370(15) -0.0007(11) 0.0025(14) 0.0035(11) Ni2 0.0264(13) 0.0723(16) 0.0368(15) -0.0013(11) 0.0037(14) 0.0048(11) Cr5 0.0249(13) 0.0726(17) 0.0370(15) -0.0007(11) 0.0025(14) 0.0035(11) Cr4 0.0264(13) 0.0723(16) 0.0368(15) -0.0013(11) 0.0037(14) 0.0048(11) Cr1 0.0314(15) 0.0860(18) 0.0395(16) -0.0004(13) 0.0072(14) 0.0119(13) Cr2 0.0395(11) 0.0566(13) 0.0326(10) 0.0006(12) 0.0038(17) -0.0025(9) Cr3 0.0345(16) 0.093(2) 0.0408(17) 0.0046(12) 0.0035(14) 0.0173(12) F1 0.014(3) 0.118(6) 0.042(4) 0.000(5) -0.004(6) 0.017(3) F2 0.022(3) 0.068(4) 0.046(4) -0.003(4) 0.017(6) 0.002(3) F3 0.018(4) 0.074(6) 0.038(5) 0.005(4) 0.004(4) 0.006(4) F4 0.033(5) 0.037(4) 0.052(6) 0.004(4) -0.003(4) 0.003(3) F5 0.045(5) 0.071(5) 0.019(4) 0.007(4) -0.005(4) 0.026(4) F6 0.054(5) 0.045(5) 0.039(5) 0.006(4) -0.004(4) 0.009(4) O1 0.081(9) 0.059(7) 0.055(7) -0.005(5) -0.005(6) 0.040(7) O2 0.096(10) 0.070(8) 0.061(8) -0.003(6) 0.024(7) 0.055(7) O3 0.070(8) 0.055(7) 0.063(7) -0.003(6) 0.014(6) -0.003(6) O4 0.036(6) 0.083(7) 0.032(6) -0.002(5) 0.013(5) -0.016(5) O5 0.018(5) 0.104(9) 0.033(7) -0.006(6) 0.002(5) 0.014(6) O6 0.040(7) 0.118(10) 0.050(7) -0.024(6) 0.025(5) -0.013(6) O7 0.035(6) 0.089(8) 0.039(6) -0.013(5) 0.011(5) 0.005(6) O8 0.060(7) 0.085(8) 0.041(6) 0.013(5) 0.004(5) 0.027(6) O9 0.043(8) 0.153(13) 0.048(8) 0.025(7) -0.018(6) -0.006(7) O10 0.050(8) 0.155(12) 0.030(7) 0.037(7) -0.031(6) -0.018(7) O11 0.056(7) 0.060(7) 0.069(7) -0.007(5) 0.038(6) -0.004(5) O12 0.035(6) 0.045(6) 0.115(9) -0.018(6) 0.003(6) 0.013(5) O13 0.033(6) 0.056(7) 0.119(10) 0.026(6) 0.001(6) 0.009(5) O14 0.058(7) 0.064(7) 0.053(6) 0.030(5) -0.012(5) -0.006(6) O15 0.060(9) 0.115(10) 0.029(7) 0.005(6) -0.004(6) 0.003(7) O16 0.027(6) 0.150(11) 0.039(7) 0.002(7) 0.012(6) 0.036(7) O17 0.040(8) 0.187(15) 0.051(8) 0.029(8) 0.017(6) 0.005(8) O18 0.045(8) 0.115(10) 0.040(7) 0.001(6) 0.004(6) 0.033(7) C1 0.078(9) 0.088(8) 0.042(8) -0.006(6) 0.010(7) 0.046(7) C2 0.094(10) 0.097(10) 0.059(9) -0.007(7) 0.016(7) 0.056(8) C3 0.109(15) 0.097(12) 0.056(11) -0.011(9) 0.015(11) 0.064(11) C4 0.095(12) 0.121(15) 0.080(15) -0.007(11) 0.029(11) 0.057(10) C5 0.100(13) 0.099(12) 0.062(10) -0.008(9) 0.010(9) 0.065(10) C2A 0.099(10) 0.092(9) 0.054(8) -0.008(6) 0.020(7) 0.054(8) C3A 0.113(13) 0.085(11) 0.060(10) -0.005(9) 0.018(10) 0.046(11) C4A 0.097(10) 0.113(12) 0.090(11) -0.008(10) 0.006(8) 0.069(9) C5A 0.144(15) 0.097(12) 0.064(9) 0.007(8) 0.011(10) 0.052(13) C6 0.065(8) 0.080(6) 0.040(6) -0.004(7) 0.006(8) -0.032(5) C7 0.070(9) 0.084(7) 0.051(6) -0.005(7) 0.007(9) -0.039(7) C8 0.077(14) 0.066(10) 0.048(8) -0.012(8) 0.007(11) -0.038(11) C9 0.068(10) 0.087(15) 0.080(14) -0.011(13) 0.009(10) -0.039(9) C10 0.082(14) 0.079(10) 0.047(7) -0.001(8) 0.008(11) -0.044(11) C7A 0.074(9) 0.080(6) 0.051(6) -0.002(7) 0.005(8) -0.040(7) C8A 0.087(13) 0.064(11) 0.058(7) -0.013(9) -0.006(11) -0.028(12) C9A 0.071(10) 0.094(11) 0.084(11) -0.009(11) 0.003(9) -0.041(8) C10A 0.084(13) 0.066(9) 0.054(7) -0.008(8) 0.006(10) -0.060(11) C11 0.025(5) 0.088(8) 0.071(8) -0.007(7) -0.021(6) -0.006(5) C12 0.029(6) 0.086(8) 0.074(8) 0.000(6) -0.023(6) -0.016(6) C13 0.031(8) 0.086(11) 0.085(10) 0.002(8) -0.016(7) -0.012(8) C14 0.045(9) 0.098(9) 0.098(11) 0.020(7) -0.044(8) -0.014(7) C15 0.040(9) 0.117(10) 0.082(9) -0.017(8) -0.016(7) -0.035(8) C12A 0.030(6) 0.091(8) 0.078(8) -0.002(7) -0.025(6) -0.016(7) C13A 0.038(10) 0.092(8) 0.085(12) 0.000(8) -0.029(10) -0.016(8) C14A 0.019(7) 0.096(11) 0.082(11) 0.001(10) -0.033(9) -0.012(9) C15A 0.032(12) 0.100(12) 0.080(9) 0.003(9) -0.031(7) -0.024(12) C16 0.081(9) 0.049(7) 0.084(9) 0.008(6) -0.008(8) 0.018(7) C17 0.084(9) 0.047(7) 0.085(9) 0.008(6) -0.013(8) 0.020(8) C18 0.109(12) 0.070(12) 0.108(12) 0.001(10) -0.036(11) 0.037(11) C19 0.104(14) 0.054(10) 0.093(11) 0.003(9) -0.009(10) 0.029(12) C20 0.101(10) 0.068(10) 0.104(12) 0.007(9) 0.002(9) -0.001(9) C17A 0.094(10) 0.056(8) 0.094(9) 0.012(7) -0.010(9) 0.010(7) C18A 0.109(12) 0.060(10) 0.096(11) 0.018(8) -0.006(11) 0.015(10) C19A 0.110(16) 0.066(12) 0.107(12) -0.001(10) -0.023(12) 0.010(12) C20A 0.087(11) 0.086(14) 0.113(15) 0.011(12) -0.005(11) 0.006(9) C21 0.043(7) 0.057(7) 0.050(6) 0.005(5) 0.006(5) 0.006(6) C22 0.057(7) 0.062(7) 0.053(7) 0.006(6) 0.002(6) 0.013(6) C23 0.061(10) 0.079(10) 0.068(11) 0.012(9) 0.001(8) 0.024(8) C24 0.074(10) 0.072(11) 0.048(9) 0.008(9) 0.009(8) 0.012(9) C25 0.065(11) 0.074(8) 0.064(10) -0.001(8) -0.014(9) 0.004(8) C22A 0.060(6) 0.067(6) 0.054(6) 0.007(5) -0.004(5) 0.012(5) C23A 0.060(6) 0.068(6) 0.055(6) 0.007(5) -0.005(5) 0.013(6) C24A 0.060(6) 0.067(6) 0.054(6) 0.008(5) -0.004(5) 0.013(6) C25A 0.060(6) 0.068(6) 0.054(6) 0.006(5) -0.004(5) 0.012(6) C26 0.057(7) 0.047(5) 0.039(6) 0.001(5) 0.009(6) -0.010(5) C27 0.074(7) 0.046(6) 0.058(8) -0.002(6) 0.009(7) -0.013(6) C28 0.085(12) 0.055(11) 0.057(8) -0.013(7) 0.019(8) -0.030(10) C29 0.076(8) 0.046(8) 0.080(10) 0.004(9) 0.017(8) 0.001(7) C30 0.078(9) 0.044(8) 0.059(10) 0.000(9) 0.017(9) -0.007(8) C27A 0.074(7) 0.043(5) 0.060(7) 0.001(5) 0.012(6) -0.007(5) C28A 0.074(7) 0.043(6) 0.061(7) 0.000(5) 0.013(6) -0.007(5) C29A 0.074(7) 0.042(6) 0.061(7) 0.001(6) 0.012(6) -0.007(5) C30A 0.074(7) 0.042(6) 0.061(8) 0.001(6) 0.013(6) -0.007(5) C31 0.102(9) 0.048(6) 0.060(8) -0.013(6) 0.015(7) -0.014(6) C32 0.110(9) 0.051(6) 0.076(8) -0.006(6) 0.004(7) -0.020(6) C33 0.130(14) 0.073(12) 0.081(8) 0.006(8) -0.014(9) -0.019(12) C34 0.110(10) 0.053(9) 0.100(11) -0.001(10) -0.005(10) -0.002(8) C35 0.109(9) 0.053(9) 0.074(10) -0.003(9) 0.002(9) -0.020(7) C32A 0.111(8) 0.048(6) 0.072(7) -0.008(6) 0.007(7) -0.018(6) C33A 0.111(9) 0.048(6) 0.072(7) -0.008(6) 0.007(7) -0.019(6) C34A 0.111(9) 0.048(6) 0.071(8) -0.008(6) 0.007(7) -0.018(6) C35A 0.111(9) 0.049(6) 0.072(7) -0.009(6) 0.006(7) -0.019(6) C36 0.075(8) 0.047(6) 0.048(6) -0.020(5) 0.019(6) 0.005(6) C37 0.082(8) 0.058(7) 0.048(6) -0.022(6) 0.021(6) 0.006(7) C38 0.089(10) 0.074(12) 0.050(12) -0.022(12) 0.028(8) -0.005(10) C39 0.088(14) 0.057(7) 0.055(12) -0.025(8) 0.020(12) 0.010(9) C40 0.092(11) 0.070(10) 0.048(7) -0.021(9) 0.021(8) 0.018(10) C37A 0.086(7) 0.063(6) 0.048(6) -0.023(5) 0.023(5) 0.007(5) C38A 0.086(7) 0.064(6) 0.048(6) -0.022(5) 0.024(6) 0.007(5) C39A 0.086(7) 0.064(6) 0.048(6) -0.023(5) 0.023(5) 0.007(5) C40A 0.086(7) 0.063(6) 0.048(6) -0.023(5) 0.023(6) 0.007(6) C41 0.031(7) 0.075(9) 0.098(11) 0.029(8) -0.001(7) 0.014(6) C42 0.037(7) 0.101(9) 0.111(10) 0.015(7) 0.007(6) 0.001(6) C43 0.050(10) 0.156(15) 0.128(13) -0.020(10) 0.022(8) -0.028(10) C44 0.071(12) 0.179(15) 0.143(13) 0.078(11) 0.014(9) -0.020(11) C45 0.076(12) 0.129(12) 0.167(17) -0.024(10) 0.045(11) 0.005(9) _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 O18 1.882(12) . ? Ni1 O1 1.935(11) . ? Ni1 F6 1.938(8) 3_665 ? Ni1 F2 1.953(9) . ? Ni1 F1 1.956(11) . ? Ni1 O3 1.981(10) . ? Ni1 Ni2 2.964(2) . ? Ni2 F3 1.917(7) . ? Ni2 O7 1.927(11) . ? Ni2 F1 1.946(10) . ? Ni2 F2 1.956(11) . ? Ni2 O4 1.987(11) . ? Ni2 O5 1.992(11) . ? Cr1 F3 1.876(8) . ? Cr1 O8 1.919(11) . ? Cr1 F4 1.936(8) . ? Cr1 O11 1.953(10) . ? Cr1 O9 1.984(13) . ? Cr1 O6 1.987(11) . ? Cr2 F4 1.900(8) . ? Cr2 F5 1.921(8) . ? Cr2 O10 1.933(10) . ? Cr2 O12 1.934(10) . ? Cr2 O15 1.951(13) . ? Cr2 O13 1.961(11) . ? Cr3 O17 1.881(12) . ? Cr3 F5 1.902(9) . ? Cr3 O14 1.912(10) . ? Cr3 F6 1.925(8) . ? Cr3 O16 1.934(12) . ? Cr3 O2 1.984(11) . ? F6 Cr5 1.938(8) 3_665 ? F6 Ni1 1.938(8) 3_665 ? O1 C1 1.295(17) 3_665 ? O2 C1 1.209(17) . ? O3 C6 1.32(2) . ? O4 C6 1.225(19) . ? O5 C11 1.288(18) . ? O6 C11 1.239(19) . ? O7 C16 1.220(17) . ? O8 C16 1.376(18) . ? O9 C21 1.279(18) . ? O10 C21 1.221(19) . ? O11 C26 1.208(17) . ? O12 C26 1.291(17) . ? O13 C31 1.24(2) . ? O14 C31 1.36(2) . ? O15 C36 1.28(2) . ? O16 C36 1.13(2) . ? O17 C41 1.304(19) 3_665 ? O18 C41 1.205(17) . ? C1 O1 1.295(17) 3_665 ? C1 C2 1.514(13) . ? C1 C2A 1.518(12) . ? C2 C5 1.521(15) . ? C2 C3 1.521(15) . ? C2 C4 1.524(15) . ? C2A C5A 1.519(15) . ? C2A C3A 1.519(15) . ? C2A C4A 1.526(15) . ? C6 C7 1.510(13) . ? C6 C7A 1.519(13) . ? C7 C10 1.567(13) . ? C7 C9 1.570(13) . ? C7 C8 1.572(13) . ? C7A C10A 1.572(13) . ? C7A C8A 1.577(13) . ? C7A C9A 1.579(13) . ? C11 C12A 1.512(13) . ? C11 C12 1.521(12) . ? C12 C14 1.509(14) . ? C12 C15 1.512(14) . ? C12 C13 1.515(14) . ? C12A C14A 1.502(14) . ? C12A C15A 1.503(14) . ? C12A C13A 1.503(14) . ? C16 C17 1.512(13) . ? C16 C17A 1.513(13) . ? C17 C19 1.577(16) . ? C17 C20 1.587(16) . ? C17 C18 1.588(16) . ? C17A C19A 1.582(16) . ? C17A C18A 1.582(16) . ? C17A C20A 1.587(16) . ? C21 C22 1.47(3) . ? C21 C22A 1.51(3) . ? C22 C23 1.584(14) . ? C22 C25 1.586(14) . ? C22 C24 1.587(14) . ? C22A C23A 1.583(14) . ? C22A C24A 1.585(14) . ? C22A C25A 1.588(14) . ? C26 C27 1.56(2) . ? C26 C27A 1.59(3) . ? C27 C30 1.467(14) . ? C27 C29 1.472(14) . ? C27 C28 1.472(14) . ? C27A C30A 1.470(14) . ? C27A C28A 1.472(14) . ? C27A C29A 1.473(14) . ? C31 C32 1.500(15) . ? C31 C32A 1.501(15) . ? C32 C34 1.579(16) . ? C32 C33 1.584(16) . ? C32 C35 1.586(16) . ? C32A C34A 1.582(16) . ? C32A C35A 1.583(16) . ? C32A C33A 1.587(16) . ? C36 C37 1.498(15) . ? C36 C37A 1.501(15) . ? C37 C39 1.568(15) . ? C37 C40 1.569(15) . ? C37 C38 1.570(15) . ? C37A C40A 1.571(14) . ? C37A C38A 1.572(15) . ? C37A C39A 1.573(14) . ? C41 O17 1.304(19) 3_665 ? C41 C42 1.504(14) . ? C42 C45 1.550(15) . ? C42 C43 1.550(15) . ? C42 C44 1.556(15) . ? C50 C50 1.82(5) 3_665 ? C50 C55 1.848(16) . ? C50 C51 1.849(16) . ? C51 C52 1.852(16) . ? C52 C53 1.849(17) . ? C53 C54 1.853(17) . ? C54 C54A 1.33(6) . ? C54 C55 1.852(17) . ? O52 C60 1.76(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O18 Ni1 O1 91.9(5) . . ? O18 Ni1 F6 96.6(4) . 3_665 ? O1 Ni1 F6 90.4(4) . 3_665 ? O18 Ni1 F2 171.5(5) . . ? O1 Ni1 F2 92.4(4) . . ? F6 Ni1 F2 90.7(4) 3_665 . ? O18 Ni1 F1 93.2(5) . . ? O1 Ni1 F1 92.3(4) . . ? F6 Ni1 F1 169.7(4) 3_665 . ? F2 Ni1 F1 79.2(4) . . ? O18 Ni1 O3 86.8(5) . . ? O1 Ni1 O3 177.5(5) . . ? F6 Ni1 O3 87.6(4) 3_665 . ? F2 Ni1 O3 89.2(4) . . ? F1 Ni1 O3 90.0(4) . . ? O18 Ni1 Ni2 130.9(4) . . ? O1 Ni1 Ni2 102.7(3) . . ? F6 Ni1 Ni2 129.3(3) 3_665 . ? F2 Ni1 Ni2 40.7(3) . . ? F1 Ni1 Ni2 40.4(3) . . ? O3 Ni1 Ni2 79.8(3) . . ? F3 Ni2 O7 91.1(4) . . ? F3 Ni2 F1 170.6(4) . . ? O7 Ni2 F1 92.9(4) . . ? F3 Ni2 F2 91.9(3) . . ? O7 Ni2 F2 91.6(4) . . ? F1 Ni2 F2 79.4(3) . . ? F3 Ni2 O4 87.0(4) . . ? O7 Ni2 O4 177.8(4) . . ? F1 Ni2 O4 89.1(4) . . ? F2 Ni2 O4 89.5(4) . . ? F3 Ni2 O5 95.5(3) . . ? O7 Ni2 O5 90.3(5) . . ? F1 Ni2 O5 93.0(4) . . ? F2 Ni2 O5 172.3(4) . . ? O4 Ni2 O5 88.9(4) . . ? F3 Ni2 Ni1 130.0(3) . . ? O7 Ni2 Ni1 102.6(3) . . ? F1 Ni2 Ni1 40.7(3) . . ? F2 Ni2 Ni1 40.7(2) . . ? O4 Ni2 Ni1 79.4(3) . . ? O5 Ni2 Ni1 131.6(3) . . ? F3 Cr1 O8 92.0(4) . . ? F3 Cr1 F4 90.6(4) . . ? O8 Cr1 F4 89.6(4) . . ? F3 Cr1 O11 88.3(4) . . ? O8 Cr1 O11 178.7(5) . . ? F4 Cr1 O11 91.6(4) . . ? F3 Cr1 O9 175.8(5) . . ? O8 Cr1 O9 88.0(5) . . ? F4 Cr1 O9 93.6(5) . . ? O11 Cr1 O9 91.5(5) . . ? F3 Cr1 O6 91.5(4) . . ? O8 Cr1 O6 92.6(5) . . ? F4 Cr1 O6 176.8(4) . . ? O11 Cr1 O6 86.1(5) . . ? O9 Cr1 O6 84.3(5) . . ? F4 Cr2 F5 90.9(2) . . ? F4 Cr2 O10 91.5(5) . . ? F5 Cr2 O10 177.6(5) . . ? F4 Cr2 O12 92.2(4) . . ? F5 Cr2 O12 90.9(4) . . ? O10 Cr2 O12 89.1(6) . . ? F4 Cr2 O15 176.1(5) . . ? F5 Cr2 O15 92.8(4) . . ? O10 Cr2 O15 84.9(4) . . ? O12 Cr2 O15 89.0(5) . . ? F4 Cr2 O13 86.0(4) . . ? F5 Cr2 O13 90.2(4) . . ? O10 Cr2 O13 89.8(5) . . ? O12 Cr2 O13 177.9(5) . . ? O15 Cr2 O13 92.8(5) . . ? O17 Cr3 F5 177.9(5) . . ? O17 Cr3 O14 86.4(5) . . ? F5 Cr3 O14 92.5(4) . . ? O17 Cr3 F6 92.2(5) . . ? F5 Cr3 F6 89.6(4) . . ? O14 Cr3 F6 89.4(4) . . ? O17 Cr3 O16 87.4(6) . . ? F5 Cr3 O16 90.8(5) . . ? O14 Cr3 O16 90.0(5) . . ? F6 Cr3 O16 179.3(5) . . ? O17 Cr3 O2 92.0(6) . . ? F5 Cr3 O2 89.0(5) . . ? O14 Cr3 O2 177.5(5) . . ? F6 Cr3 O2 92.6(4) . . ? O16 Cr3 O2 87.9(5) . . ? Ni2 F1 Ni1 98.8(2) . . ? Ni1 F2 Ni2 98.6(3) . . ? Cr1 F3 Ni2 122.1(4) . . ? Cr2 F4 Cr1 123.1(5) . . ? Cr3 F5 Cr2 123.5(4) . . ? Cr3 F6 Cr5 120.8(4) . 3_665 ? Cr3 F6 Ni1 120.8(4) . 3_665 ? Cr5 F6 Ni1 0.00(15) 3_665 3_665 ? C1 O1 Ni1 133.3(10) 3_665 . ? C1 O2 Cr3 132.5(11) . . ? C6 O3 Ni1 126.9(9) . . ? C6 O4 Ni2 129.3(9) . . ? C11 O5 Ni2 133.7(9) . . ? C11 O6 Cr1 130.7(10) . . ? C16 O7 Ni2 132.7(10) . . ? C16 O8 Cr1 137.0(9) . . ? C21 O9 Cr1 131.1(11) . . ? C21 O10 Cr2 136.7(11) . . ? C26 O11 Cr1 135.4(10) . . ? C26 O12 Cr2 137.2(10) . . ? C31 O13 Cr2 130.9(11) . . ? C31 O14 Cr3 134.5(10) . . ? C36 O15 Cr2 132.6(11) . . ? C36 O16 Cr3 135.4(11) . . ? C41 O17 Cr3 136.3(10) 3_665 . ? C41 O18 Ni1 133.6(11) . . ? O2 C1 O1 127.0(15) . 3_665 ? O2 C1 C2 108.0(12) . . ? O1 C1 C2 113.0(13) 3_665 . ? O2 C1 C2A 119.5(12) . . ? O1 C1 C2A 112.5(11) 3_665 . ? C2 C1 C2A 28.0(10) . . ? C1 C2 C5 111.9(9) . . ? C1 C2 C3 111.8(9) . . ? C5 C2 C3 107.2(10) . . ? C1 C2 C4 111.6(9) . . ? C5 C2 C4 106.9(10) . . ? C3 C2 C4 107.1(10) . . ? C1 C2A C5A 112.2(9) . . ? C1 C2A C3A 111.9(9) . . ? C5A C2A C3A 107.4(9) . . ? C1 C2A C4A 111.0(9) . . ? C5A C2A C4A 106.8(9) . . ? C3A C2A C4A 107.3(9) . . ? O4 C6 O3 124.4(11) . . ? O4 C6 C7 120.5(17) . . ? O3 C6 C7 112.0(17) . . ? O4 C6 C7A 118.1(16) . . ? O3 C6 C7A 117.4(16) . . ? C7 C6 C7A 21.5(12) . . ? C6 C7 C10 110(2) . . ? C6 C7 C9 110(2) . . ? C10 C7 C9 110.0(9) . . ? C6 C7 C8 108(2) . . ? C10 C7 C8 109.7(9) . . ? C9 C7 C8 109.5(9) . . ? C6 C7A C10A 115.7(16) . . ? C6 C7A C8A 105.0(17) . . ? C10A C7A C8A 109.0(8) . . ? C6 C7A C9A 109.2(15) . . ? C10A C7A C9A 108.9(8) . . ? C8A C7A C9A 108.9(8) . . ? O6 C11 O5 121.7(12) . . ? O6 C11 C12A 115.9(19) . . ? O5 C11 C12A 122.3(18) . . ? O6 C11 C12 123.4(15) . . ? O5 C11 C12 114.0(14) . . ? C12A C11 C12 10.7(14) . . ? C14 C12 C15 111.4(8) . . ? C14 C12 C13 110.7(8) . . ? C15 C12 C13 110.7(8) . . ? C14 C12 C11 98.6(14) . . ? C15 C12 C11 106.4(14) . . ? C13 C12 C11 118.4(15) . . ? C14A C12A C15A 112.2(9) . . ? C14A C12A C13A 112.5(9) . . ? C15A C12A C13A 112.3(9) . . ? C14A C12A C11 103(2) . . ? C15A C12A C11 112(3) . . ? C13A C12A C11 104(2) . . ? O7 C16 O8 119.4(13) . . ? O7 C16 C17 130.3(13) . . ? O8 C16 C17 109.9(11) . . ? O7 C16 C17A 127.7(14) . . ? O8 C16 C17A 96.5(13) . . ? C17 C16 C17A 35.8(9) . . ? C16 C17 C19 107.3(9) . . ? C16 C17 C20 106.5(9) . . ? C19 C17 C20 112.5(8) . . ? C16 C17 C18 106.3(9) . . ? C19 C17 C18 112.2(8) . . ? C20 C17 C18 111.6(8) . . ? C16 C17A C19A 106.9(9) . . ? C16 C17A C18A 106.8(9) . . ? C19A C17A C18A 112.4(9) . . ? C16 C17A C20A 106.3(9) . . ? C19A C17A C20A 112.0(9) . . ? C18A C17A C20A 112.0(9) . . ? O10 C21 O9 125.8(15) . . ? O10 C21 C22 119.4(15) . . ? O9 C21 C22 114.7(15) . . ? O10 C21 C22A 118.9(15) . . ? O9 C21 C22A 114.6(15) . . ? C22 C21 C22A 6.2(11) . . ? C21 C22 C23 110.2(18) . . ? C21 C22 C25 95.7(17) . . ? C23 C22 C25 112.2(9) . . ? C21 C22 C24 113.6(19) . . ? C23 C22 C24 112.2(9) . . ? C25 C22 C24 112.0(9) . . ? C21 C22A C23A 111.4(18) . . ? C21 C22A C24A 106.7(18) . . ? C23A C22A C24A 112.2(9) . . ? C21 C22A C25A 101.8(17) . . ? C23A C22A C25A 112.1(9) . . ? C24A C22A C25A 112.0(9) . . ? O11 C26 O12 122.1(13) . . ? O11 C26 C27 129.5(14) . . ? O12 C26 C27 108.3(13) . . ? O11 C26 C27A 116.6(14) . . ? O12 C26 C27A 119.4(15) . . ? C27 C26 C27A 20.0(10) . . ? C30 C27 C29 111.8(10) . . ? C30 C27 C28 111.8(10) . . ? C29 C27 C28 111.2(10) . . ? C30 C27 C26 108.4(16) . . ? C29 C27 C26 109.8(16) . . ? C28 C27 C26 103.4(16) . . ? C30A C27A C28A 111.6(11) . . ? C30A C27A C29A 111.4(10) . . ? C28A C27A C29A 111.3(11) . . ? C30A C27A C26 108(2) . . ? C28A C27A C26 106(2) . . ? C29A C27A C26 108(2) . . ? O13 C31 O14 124.0(13) . . ? O13 C31 C32 115.6(18) . . ? O14 C31 C32 119.2(17) . . ? O13 C31 C32A 124(2) . . ? O14 C31 C32A 111.5(18) . . ? C32 C31 C32A 15.7(12) . . ? C31 C32 C34 107.4(17) . . ? C31 C32 C33 110.3(17) . . ? C34 C32 C33 110.5(9) . . ? C31 C32 C35 107.7(16) . . ? C34 C32 C35 110.7(9) . . ? C33 C32 C35 110.2(9) . . ? C31 C32A C34A 110(2) . . ? C31 C32A C35A 111(2) . . ? C34A C32A C35A 110.5(9) . . ? C31 C32A C33A 104(2) . . ? C34A C32A C33A 110.2(9) . . ? C35A C32A C33A 110.1(9) . . ? O16 C36 O15 126.2(14) . . ? O16 C36 C37 117(2) . . ? O15 C36 C37 116.2(19) . . ? O16 C36 C37A 126.7(18) . . ? O15 C36 C37A 106.6(17) . . ? C37 C36 C37A 10.0(13) . . ? C36 C37 C39 104.5(18) . . ? C36 C37 C40 115(2) . . ? C39 C37 C40 109.4(9) . . ? C36 C37 C38 109(2) . . ? C39 C37 C38 109.4(9) . . ? C40 C37 C38 109.2(9) . . ? C36 C37A C40A 112.6(15) . . ? C36 C37A C38A 111.8(15) . . ? C40A C37A C38A 108.7(8) . . ? C36 C37A C39A 106.0(15) . . ? C40A C37A C39A 108.9(8) . . ? C38A C37A C39A 108.7(8) . . ? O18 C41 O17 124.4(14) . 3_665 ? O18 C41 C42 123.4(13) . . ? O17 C41 C42 112.1(11) 3_665 . ? C41 C42 C45 108.8(9) . . ? C41 C42 C43 109.5(9) . . ? C45 C42 C43 110.3(8) . . ? C41 C42 C44 108.6(8) . . ? C45 C42 C44 109.7(9) . . ? C43 C42 C44 110.0(8) . . ? C50 C50 C55 101.1(19) 3_665 . ? C50 C50 C51 89.7(16) 3_665 . ? C55 C50 C51 113.0(17) . . ? C50 C51 C52 105.3(16) . . ? C53 C52 C51 131(2) . . ? C52 C53 C54 98(3) . . ? C54A C54 C55 97(3) . . ? C54A C54 C53 91(4) . . ? C55 C54 C53 128(3) . . ? C50 C55 C54 89(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O18 Ni1 Ni2 F3 152.6(6) . . . . ? O1 Ni1 Ni2 F3 -103.5(5) . . . . ? F6 Ni1 Ni2 F3 -2.4(6) 3_665 . . . ? F2 Ni1 Ni2 F3 -24.8(4) . . . . ? F1 Ni1 Ni2 F3 178.1(5) . . . . ? O3 Ni1 Ni2 F3 76.0(5) . . . . ? O18 Ni1 Ni2 O7 -105.1(6) . . . . ? O1 Ni1 Ni2 O7 -1.2(6) . . . . ? F6 Ni1 Ni2 O7 99.9(4) 3_665 . . . ? F2 Ni1 Ni2 O7 77.4(4) . . . . ? F1 Ni1 Ni2 O7 -79.6(5) . . . . ? O3 Ni1 Ni2 O7 178.3(5) . . . . ? O18 Ni1 Ni2 F1 -25.5(6) . . . . ? O1 Ni1 Ni2 F1 78.4(5) . . . . ? F6 Ni1 Ni2 F1 179.5(5) 3_665 . . . ? F2 Ni1 Ni2 F1 157.1(5) . . . . ? O3 Ni1 Ni2 F1 -102.1(5) . . . . ? O18 Ni1 Ni2 F2 177.4(6) . . . . ? O1 Ni1 Ni2 F2 -78.7(5) . . . . ? F6 Ni1 Ni2 F2 22.4(4) 3_665 . . . ? F1 Ni1 Ni2 F2 -157.1(5) . . . . ? O3 Ni1 Ni2 F2 100.8(5) . . . . ? O18 Ni1 Ni2 O4 75.6(6) . . . . ? O1 Ni1 Ni2 O4 179.5(5) . . . . ? F6 Ni1 Ni2 O4 -79.4(4) 3_665 . . . ? F2 Ni1 Ni2 O4 -101.8(4) . . . . ? F1 Ni1 Ni2 O4 101.1(5) . . . . ? O3 Ni1 Ni2 O4 -1.0(6) . . . . ? O18 Ni1 Ni2 O5 -3.2(8) . . . . ? O1 Ni1 Ni2 O5 100.7(6) . . . . ? F6 Ni1 Ni2 O5 -158.3(6) 3_665 . . . ? F2 Ni1 Ni2 O5 179.3(6) . . . . ? F1 Ni1 Ni2 O5 22.3(6) . . . . ? O3 Ni1 Ni2 O5 -79.8(6) . . . . ? F3 Ni2 F1 Ni1 -9(2) . . . . ? O7 Ni2 F1 Ni1 106.0(4) . . . . ? F2 Ni2 F1 Ni1 15.0(3) . . . . ? O4 Ni2 F1 Ni1 -74.7(4) . . . . ? O5 Ni2 F1 Ni1 -163.5(4) . . . . ? O18 Ni1 F1 Ni2 161.0(5) . . . . ? O1 Ni1 F1 Ni2 -107.0(5) . . . . ? F6 Ni1 F1 Ni2 -2(2) 3_665 . . . ? F2 Ni1 F1 Ni2 -15.0(3) . . . . ? O3 Ni1 F1 Ni2 74.2(4) . . . . ? O18 Ni1 F2 Ni2 -13(3) . . . . ? O1 Ni1 F2 Ni2 106.8(4) . . . . ? F6 Ni1 F2 Ni2 -162.8(3) 3_665 . . . ? F1 Ni1 F2 Ni2 14.9(3) . . . . ? O3 Ni1 F2 Ni2 -75.2(4) . . . . ? F3 Ni2 F2 Ni1 161.2(3) . . . . ? O7 Ni2 F2 Ni1 -107.7(4) . . . . ? F1 Ni2 F2 Ni1 -15.0(3) . . . . ? O4 Ni2 F2 Ni1 74.2(4) . . . . ? O5 Ni2 F2 Ni1 -4(3) . . . . ? O8 Cr1 F3 Ni2 -42.1(6) . . . . ? F4 Cr1 F3 Ni2 -131.8(5) . . . . ? O11 Cr1 F3 Ni2 136.7(6) . . . . ? O9 Cr1 F3 Ni2 48(7) . . . . ? O6 Cr1 F3 Ni2 50.6(6) . . . . ? O7 Ni2 F3 Cr1 56.2(6) . . . . ? F1 Ni2 F3 Cr1 171(2) . . . . ? F2 Ni2 F3 Cr1 147.8(5) . . . . ? O4 Ni2 F3 Cr1 -122.8(6) . . . . ? O5 Ni2 F3 Cr1 -34.2(6) . . . . ? Ni1 Ni2 F3 Cr1 163.7(3) . . . . ? F5 Cr2 F4 Cr1 132.7(4) . . . . ? O10 Cr2 F4 Cr1 -47.5(6) . . . . ? O12 Cr2 F4 Cr1 41.7(6) . . . . ? O15 Cr2 F4 Cr1 -67(7) . . . . ? O13 Cr2 F4 Cr1 -137.2(5) . . . . ? F3 Cr1 F4 Cr2 -136.5(5) . . . . ? O8 Cr1 F4 Cr2 131.5(5) . . . . ? O11 Cr1 F4 Cr2 -48.2(5) . . . . ? O9 Cr1 F4 Cr2 43.5(6) . . . . ? O6 Cr1 F4 Cr2 -4(9) . . . . ? O17 Cr3 F5 Cr2 17(15) . . . . ? O14 Cr3 F5 Cr2 -42.6(6) . . . . ? F6 Cr3 F5 Cr2 -132.0(5) . . . . ? O16 Cr3 F5 Cr2 47.4(6) . . . . ? O2 Cr3 F5 Cr2 135.3(6) . . . . ? F4 Cr2 F5 Cr3 141.4(4) . . . . ? O10 Cr2 F5 Cr3 -35(13) . . . . ? O12 Cr2 F5 Cr3 -126.4(6) . . . . ? O15 Cr2 F5 Cr3 -37.4(6) . . . . ? O13 Cr2 F5 Cr3 55.4(6) . . . . ? O17 Cr3 F6 Cr5 43.0(6) . . . 3_665 ? F5 Cr3 F6 Cr5 -138.1(5) . . . 3_665 ? O14 Cr3 F6 Cr5 129.4(5) . . . 3_665 ? O16 Cr3 F6 Cr5 94(39) . . . 3_665 ? O2 Cr3 F6 Cr5 -49.2(6) . . . 3_665 ? O17 Cr3 F6 Ni1 43.0(6) . . . 3_665 ? F5 Cr3 F6 Ni1 -138.1(5) . . . 3_665 ? O14 Cr3 F6 Ni1 129.4(5) . . . 3_665 ? O16 Cr3 F6 Ni1 94(39) . . . 3_665 ? O2 Cr3 F6 Ni1 -49.2(6) . . . 3_665 ? O18 Ni1 O1 C1 -65.0(15) . . . 3_665 ? F6 Ni1 O1 C1 31.7(15) 3_665 . . 3_665 ? F2 Ni1 O1 C1 122.4(15) . . . 3_665 ? F1 Ni1 O1 C1 -158.3(15) . . . 3_665 ? O3 Ni1 O1 C1 -6(13) . . . 3_665 ? Ni2 Ni1 O1 C1 162.2(14) . . . 3_665 ? O17 Cr3 O2 C1 -74.2(16) . . . . ? F5 Cr3 O2 C1 107.7(16) . . . . ? O14 Cr3 O2 C1 -126(12) . . . . ? F6 Cr3 O2 C1 18.1(16) . . . . ? O16 Cr3 O2 C1 -161.5(16) . . . . ? O18 Ni1 O3 C6 -129.9(12) . . . . ? O1 Ni1 O3 C6 172(11) . . . . ? F6 Ni1 O3 C6 133.4(12) 3_665 . . . ? F2 Ni1 O3 C6 42.6(12) . . . . ? F1 Ni1 O3 C6 -36.6(12) . . . . ? Ni2 Ni1 O3 C6 2.7(11) . . . . ? F3 Ni2 O4 C6 -132.1(12) . . . . ? O7 Ni2 O4 C6 -161(11) . . . . ? F1 Ni2 O4 C6 39.4(12) . . . . ? F2 Ni2 O4 C6 -40.1(12) . . . . ? O5 Ni2 O4 C6 132.4(12) . . . . ? Ni1 Ni2 O4 C6 -0.4(11) . . . . ? F3 Ni2 O5 C11 -2.5(16) . . . . ? O7 Ni2 O5 C11 -93.6(16) . . . . ? F1 Ni2 O5 C11 173.5(15) . . . . ? F2 Ni2 O5 C11 162(2) . . . . ? O4 Ni2 O5 C11 84.4(16) . . . . ? Ni1 Ni2 O5 C11 159.2(14) . . . . ? F3 Cr1 O6 C11 -52.6(16) . . . . ? O8 Cr1 O6 C11 39.5(16) . . . . ? F4 Cr1 O6 C11 175(8) . . . . ? O11 Cr1 O6 C11 -140.9(16) . . . . ? O9 Cr1 O6 C11 127.2(17) . . . . ? F3 Ni2 O7 C16 -45.1(15) . . . . ? F1 Ni2 O7 C16 143.5(15) . . . . ? F2 Ni2 O7 C16 -137.0(14) . . . . ? O4 Ni2 O7 C16 -16(13) . . . . ? O5 Ni2 O7 C16 50.4(15) . . . . ? Ni1 Ni2 O7 C16 -176.6(14) . . . . ? F3 Cr1 O8 C16 3.2(16) . . . . ? F4 Cr1 O8 C16 93.8(16) . . . . ? O11 Cr1 O8 C16 -103(21) . . . . ? O9 Cr1 O8 C16 -172.6(16) . . . . ? O6 Cr1 O8 C16 -88.4(16) . . . . ? F3 Cr1 O9 C21 169(6) . . . . ? O8 Cr1 O9 C21 -100.3(15) . . . . ? F4 Cr1 O9 C21 -10.8(15) . . . . ? O11 Cr1 O9 C21 80.9(15) . . . . ? O6 Cr1 O9 C21 166.8(16) . . . . ? F4 Cr2 O10 C21 26(2) . . . . ? F5 Cr2 O10 C21 -158(12) . . . . ? O12 Cr2 O10 C21 -66.7(19) . . . . ? O15 Cr2 O10 C21 -155.7(19) . . . . ? O13 Cr2 O10 C21 111(2) . . . . ? F3 Cr1 O11 C26 120.2(16) . . . . ? O8 Cr1 O11 C26 -134(20) . . . . ? F4 Cr1 O11 C26 29.6(16) . . . . ? O9 Cr1 O11 C26 -64.0(16) . . . . ? O6 Cr1 O11 C26 -148.2(16) . . . . ? F4 Cr2 O12 C26 -9.4(16) . . . . ? F5 Cr2 O12 C26 -100.3(16) . . . . ? O10 Cr2 O12 C26 82.0(16) . . . . ? O15 Cr2 O12 C26 166.9(16) . . . . ? O13 Cr2 O12 C26 21(14) . . . . ? F4 Cr2 O13 C31 -131.6(16) . . . . ? F5 Cr2 O13 C31 -40.8(16) . . . . ? O10 Cr2 O13 C31 136.9(16) . . . . ? O12 Cr2 O13 C31 -163(12) . . . . ? O15 Cr2 O13 C31 52.0(16) . . . . ? O17 Cr3 O14 C31 -175.7(15) . . . . ? F5 Cr3 O14 C31 2.5(15) . . . . ? F6 Cr3 O14 C31 92.1(14) . . . . ? O16 Cr3 O14 C31 -88.3(15) . . . . ? O2 Cr3 O14 C31 -123(12) . . . . ? F4 Cr2 O15 C36 -160(6) . . . . ? F5 Cr2 O15 C36 1.0(16) . . . . ? O10 Cr2 O15 C36 -178.9(15) . . . . ? O12 Cr2 O15 C36 91.9(16) . . . . ? O13 Cr2 O15 C36 -89.3(16) . . . . ? O17 Cr3 O16 C36 145(2) . . . . ? F5 Cr3 O16 C36 -34(2) . . . . ? O14 Cr3 O16 C36 58(2) . . . . ? F6 Cr3 O16 C36 93(39) . . . . ? O2 Cr3 O16 C36 -123(2) . . . . ? F5 Cr3 O17 C41 -174(14) . . . 3_665 ? O14 Cr3 O17 C41 -114.4(18) . . . 3_665 ? F6 Cr3 O17 C41 -25.2(18) . . . 3_665 ? O16 Cr3 O17 C41 155.4(18) . . . 3_665 ? O2 Cr3 O17 C41 67.5(18) . . . 3_665 ? O1 Ni1 O18 C41 83.0(16) . . . . ? F6 Ni1 O18 C41 -7.6(16) 3_665 . . . ? F2 Ni1 O18 C41 -157(2) . . . . ? F1 Ni1 O18 C41 175.4(16) . . . . ? O3 Ni1 O18 C41 -94.8(17) . . . . ? Ni2 Ni1 O18 C41 -168.3(14) . . . . ? Cr3 O2 C1 O1 2(3) . . . 3_665 ? Cr3 O2 C1 C2 141.4(14) . . . . ? Cr3 O2 C1 C2A 169.4(9) . . . . ? O2 C1 C2 C5 168(2) . . . . ? O1 C1 C2 C5 -46.0(19) 3_665 . . . ? C2A C1 C2 C5 49(3) . . . . ? O2 C1 C2 C3 48(2) . . . . ? O1 C1 C2 C3 -166.3(19) 3_665 . . . ? C2A C1 C2 C3 -71(3) . . . . ? O2 C1 C2 C4 -72(2) . . . . ? O1 C1 C2 C4 73.8(19) 3_665 . . . ? C2A C1 C2 C4 169(3) . . . . ? O2 C1 C2A C5A 144.8(17) . . . . ? O1 C1 C2A C5A -45.9(15) 3_665 . . . ? C2 C1 C2A C5A -143(2) . . . . ? O2 C1 C2A C3A 24.1(17) . . . . ? O1 C1 C2A C3A -166.6(14) 3_665 . . . ? C2 C1 C2A C3A 96(2) . . . . ? O2 C1 C2A C4A -95.7(17) . . . . ? O1 C1 C2A C4A 73.5(14) 3_665 . . . ? C2 C1 C2A C4A -24(2) . . . . ? Ni2 O4 C6 O3 2.7(19) . . . . ? Ni2 O4 C6 C7 -156.0(15) . . . . ? Ni2 O4 C6 C7A 179.5(10) . . . . ? Ni1 O3 C6 O4 -4.1(19) . . . . ? Ni1 O3 C6 C7 156.1(14) . . . . ? Ni1 O3 C6 C7A 179.0(10) . . . . ? O4 C6 C7 C10 -29(2) . . . . ? O3 C6 C7 C10 170.0(16) . . . . ? C7A C6 C7 C10 61(4) . . . . ? O4 C6 C7 C9 92.3(19) . . . . ? O3 C6 C7 C9 -68.8(19) . . . . ? C7A C6 C7 C9 -178(5) . . . . ? O4 C6 C7 C8 -148.7(17) . . . . ? O3 C6 C7 C8 50.2(19) . . . . ? C7A C6 C7 C8 -59(4) . . . . ? O4 C6 C7A C10A -24.7(18) . . . . ? O3 C6 C7A C10A 152.4(14) . . . . ? C7 C6 C7A C10A -127(4) . . . . ? O4 C6 C7A C8A -144.9(14) . . . . ? O3 C6 C7A C8A 32.2(16) . . . . ? C7 C6 C7A C8A 113(4) . . . . ? O4 C6 C7A C9A 98.4(15) . . . . ? O3 C6 C7A C9A -84.5(15) . . . . ? C7 C6 C7A C9A -4(4) . . . . ? Cr1 O6 C11 O5 28(3) . . . . ? Cr1 O6 C11 C12A -155.0(17) . . . . ? Cr1 O6 C11 C12 -163.9(12) . . . . ? Ni2 O5 C11 O6 6(3) . . . . ? Ni2 O5 C11 C12A -170.3(17) . . . . ? Ni2 O5 C11 C12 -162.7(11) . . . . ? O6 C11 C12 C14 104.2(18) . . . . ? O5 C11 C12 C14 -86.8(16) . . . . ? C12A C11 C12 C14 56(8) . . . . ? O6 C11 C12 C15 -11(2) . . . . ? O5 C11 C12 C15 157.8(15) . . . . ? C12A C11 C12 C15 -59(8) . . . . ? O6 C11 C12 C13 -136.6(17) . . . . ? O5 C11 C12 C13 32(2) . . . . ? C12A C11 C12 C13 175(9) . . . . ? O6 C11 C12A C14A 163(2) . . . . ? O5 C11 C12A C14A -20(3) . . . . ? C12 C11 C12A C14A -61(8) . . . . ? O6 C11 C12A C15A 42(3) . . . . ? O5 C11 C12A C15A -141(2) . . . . ? C12 C11 C12A C15A 178(9) . . . . ? O6 C11 C12A C13A -79(2) . . . . ? O5 C11 C12A C13A 98(2) . . . . ? C12 C11 C12A C13A 57(8) . . . . ? Ni2 O7 C16 O8 18(2) . . . . ? Ni2 O7 C16 C17 -169.1(10) . . . . ? Ni2 O7 C16 C17A 144.4(13) . . . . ? Cr1 O8 C16 O7 10(3) . . . . ? Cr1 O8 C16 C17 -164.5(11) . . . . ? Cr1 O8 C16 C17A -130.3(14) . . . . ? O7 C16 C17 C19 3(2) . . . . ? O8 C16 C17 C19 176.5(13) . . . . ? C17A C16 C17 C19 103.8(18) . . . . ? O7 C16 C17 C20 -117.9(19) . . . . ? O8 C16 C17 C20 55.8(14) . . . . ? C17A C16 C17 C20 -16.8(17) . . . . ? O7 C16 C17 C18 122.9(19) . . . . ? O8 C16 C17 C18 -63.3(13) . . . . ? C17A C16 C17 C18 -136.0(18) . . . . ? O7 C16 C17A C19A 25.4(19) . . . . ? O8 C16 C17A C19A 160.9(14) . . . . ? C17 C16 C17A C19A -83.7(18) . . . . ? O7 C16 C17A C18A 146.0(19) . . . . ? O8 C16 C17A C18A -78.6(14) . . . . ? C17 C16 C17A C18A 36.9(18) . . . . ? O7 C16 C17A C20A -94.3(19) . . . . ? O8 C16 C17A C20A 41.2(14) . . . . ? C17 C16 C17A C20A 156.6(19) . . . . ? Cr2 O10 C21 O9 1(3) . . . . ? Cr2 O10 C21 C22 177.9(13) . . . . ? Cr2 O10 C21 C22A 170.8(14) . . . . ? Cr1 O9 C21 O10 -11(3) . . . . ? Cr1 O9 C21 C22 172.6(12) . . . . ? Cr1 O9 C21 C22A 179.5(11) . . . . ? O10 C21 C22 C23 135.0(17) . . . . ? O9 C21 C22 C23 -48.0(19) . . . . ? C22A C21 C22 C23 -139(12) . . . . ? O10 C21 C22 C25 -108.8(18) . . . . ? O9 C21 C22 C25 68.1(16) . . . . ? C22A C21 C22 C25 -22(11) . . . . ? O10 C21 C22 C24 8(2) . . . . ? O9 C21 C22 C24 -174.9(14) . . . . ? C22A C21 C22 C24 95(11) . . . . ? O10 C21 C22A C23A 171.3(15) . . . . ? O9 C21 C22A C23A -18.0(19) . . . . ? C22 C21 C22A C23A 74(11) . . . . ? O10 C21 C22A C24A 48.5(19) . . . . ? O9 C21 C22A C24A -140.8(15) . . . . ? C22 C21 C22A C24A -49(11) . . . . ? O10 C21 C22A C25A -69.0(18) . . . . ? O9 C21 C22A C25A 101.6(16) . . . . ? C22 C21 C22A C25A -166(12) . . . . ? Cr1 O11 C26 O12 -5(3) . . . . ? Cr1 O11 C26 C27 172.6(11) . . . . ? Cr1 O11 C26 C27A -169.0(13) . . . . ? Cr2 O12 C26 O11 -9(3) . . . . ? Cr2 O12 C26 C27 173.1(11) . . . . ? Cr2 O12 C26 C27A 154.8(13) . . . . ? O11 C26 C27 C30 7(2) . . . . ? O12 C26 C27 C30 -175.8(12) . . . . ? C27A C26 C27 C30 -49(4) . . . . ? O11 C26 C27 C29 129.1(18) . . . . ? O12 C26 C27 C29 -53.4(15) . . . . ? C27A C26 C27 C29 74(4) . . . . ? O11 C26 C27 C28 -112.2(18) . . . . ? O12 C26 C27 C28 65.4(15) . . . . ? C27A C26 C27 C28 -168(4) . . . . ? O11 C26 C27A C30A -18.7(19) . . . . ? O12 C26 C27A C30A 176.5(16) . . . . ? C27 C26 C27A C30A 116(4) . . . . ? O11 C26 C27A C28A -138.5(16) . . . . ? O12 C26 C27A C28A 57(2) . . . . ? C27 C26 C27A C28A -4(3) . . . . ? O11 C26 C27A C29A 101.8(18) . . . . ? O12 C26 C27A C29A -63(2) . . . . ? C27 C26 C27A C29A -123(4) . . . . ? Cr2 O13 C31 O14 13(3) . . . . ? Cr2 O13 C31 C32 -154.9(12) . . . . ? Cr2 O13 C31 C32A -170.0(13) . . . . ? Cr3 O14 C31 O13 13(3) . . . . ? Cr3 O14 C31 C32 179.9(11) . . . . ? Cr3 O14 C31 C32A -164.9(12) . . . . ? O13 C31 C32 C34 -55.0(18) . . . . ? O14 C31 C32 C34 136.6(15) . . . . ? C32A C31 C32 C34 73(5) . . . . ? O13 C31 C32 C33 65.5(19) . . . . ? O14 C31 C32 C33 -102.9(16) . . . . ? C32A C31 C32 C33 -167(6) . . . . ? O13 C31 C32 C35 -174.3(15) . . . . ? O14 C31 C32 C35 17.3(19) . . . . ? C32A C31 C32 C35 -47(5) . . . . ? O13 C31 C32A C34A 6(2) . . . . ? O14 C31 C32A C34A -176.2(15) . . . . ? C32 C31 C32A C34A -54(5) . . . . ? O13 C31 C32A C35A -117(2) . . . . ? O14 C31 C32A C35A 60.8(19) . . . . ? C32 C31 C32A C35A -177(6) . . . . ? O13 C31 C32A C33A 125(2) . . . . ? O14 C31 C32A C33A -58.0(18) . . . . ? C32 C31 C32A C33A 65(5) . . . . ? Cr3 O16 C36 O15 6(3) . . . . ? Cr3 O16 C36 C37 -169.0(14) . . . . ? Cr3 O16 C36 C37A -164.5(13) . . . . ? Cr2 O15 C36 O16 16(3) . . . . ? Cr2 O15 C36 C37 -168.9(13) . . . . ? Cr2 O15 C36 C37A -171.9(11) . . . . ? O16 C36 C37 C39 -79(2) . . . . ? O15 C36 C37 C39 105.0(18) . . . . ? C37A C36 C37 C39 122(7) . . . . ? O16 C36 C37 C40 160.8(18) . . . . ? O15 C36 C37 C40 -15(2) . . . . ? C37A C36 C37 C40 2(6) . . . . ? O16 C36 C37 C38 38(2) . . . . ? O15 C36 C37 C38 -138.0(17) . . . . ? C37A C36 C37 C38 -121(7) . . . . ? O16 C36 C37A C40A -135.8(19) . . . . ? O15 C36 C37A C40A 51.9(16) . . . . ? C37 C36 C37A C40A -112(7) . . . . ? O16 C36 C37A C38A 102(2) . . . . ? O15 C36 C37A C38A -70.8(16) . . . . ? C37 C36 C37A C38A 125(7) . . . . ? O16 C36 C37A C39A -17(2) . . . . ? O15 C36 C37A C39A 170.9(12) . . . . ? C37 C36 C37A C39A 7(7) . . . . ? Ni1 O18 C41 O17 -13(3) . . . 3_665 ? Ni1 O18 C41 C42 169.7(10) . . . . ? O18 C41 C42 C45 93.7(16) . . . . ? O17 C41 C42 C45 -83.9(14) 3_665 . . . ? O18 C41 C42 C43 -26.9(17) . . . . ? O17 C41 C42 C43 155.5(13) 3_665 . . . ? O18 C41 C42 C44 -147.0(16) . . . . ? O17 C41 C42 C44 35.4(14) 3_665 . . . ? C50 C50 C51 C52 -154(2) 3_665 . . . ? C55 C50 C51 C52 -52(2) . . . . ? C50 C51 C52 C53 1(4) . . . . ? C51 C52 C53 C54 9(5) . . . . ? C52 C53 C54 C54A -65(3) . . . . ? C52 C53 C54 C55 34(6) . . . . ? C50 C50 C55 C54 172(2) 3_665 . . . ? C51 C50 C55 C54 77(2) . . . . ? C54A C54 C55 C50 23(3) . . . . ? C53 C54 C55 C50 -74(5) . . . . ? _diffrn_measured_fraction_theta_max .995 _diffrn_reflns_theta_full 21.95 _diffrn_measured_fraction_theta_full .995 _refine_diff_density_max 2.049 _refine_diff_density_min -.835 _refine_diff_density_rms .196 data_orepw170pb3c1 _database_code_depnum_ccdc_archive 'CCDC 268358' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C91 H167 Cr8 F11 N4 Ni O37' _chemical_formula_weight 2590.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr .3209 .6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni .3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' _cell_length_a 36.0766(12) _cell_length_b 36.0766(12) _cell_length_c 19.0238(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 21442.7(13) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16478 _cell_measurement_theta_min 2.5728 _cell_measurement_theta_max 32.0865 _exptl_crystal_description Prismatic _exptl_crystal_colour Green _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8124 _exptl_absorpt_coefficient_mu 0.789 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.7637 _exptl_absorpt_correction_T_max 0.9057 _exptl_absorpt_process_details ? _exptl_special_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 92071 _diffrn_reflns_av_R_equivalents 0.1244 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 20.81 _reflns_number_total 7466 _reflns_number_gt 6093 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Data of very poor quality. All disordered oxygens are left isotrpic. All carbons left isotropic and hydrogens have not been placed. Ni position not determined due to high symmetry and averaged over all sites. Amine molecule left isotropic. 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^)+(0.1951P)^2^+150.5188P] 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 7466 _refine_ls_number_parameters 627 _refine_ls_number_restraints 536 _refine_ls_R_factor_all 0.1455 _refine_ls_R_factor_gt 0.1262 _refine_ls_wR_factor_ref 0.3512 _refine_ls_wR_factor_gt 0.3339 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.114 _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 Cr1 Cr 0.24723(7) 0.24723(7) 0.2500 0.0578(9) Uani 0.89 2 d SP . . Cr2 Cr 0.32488(7) 0.22766(6) 0.29587(15) 0.0706(8) Uani 0.89 1 d P . . Cr3 Cr 0.43176(6) 0.27971(6) 0.30857(12) 0.0548(7) Uani 0.89 1 d P . . Cr4 Cr 0.51133(6) 0.37742(6) 0.26580(10) 0.0419(6) Uani 0.89 1 d P . . Cr5 Cr 0.52191(5) 0.47138(6) 0.21282(9) 0.0369(6) Uani 0.89 1 d P . . Ni1 Ni 0.24723(7) 0.24723(7) 0.2500 0.0578(9) Uani 0.11 2 d SP . . Ni2 Ni 0.32488(7) 0.22766(6) 0.29587(15) 0.0706(8) Uani 0.11 1 d P . . Ni3 Ni 0.43176(6) 0.27971(6) 0.30857(12) 0.0548(7) Uani 0.11 1 d P . . Ni4 Ni 0.51133(6) 0.37742(6) 0.26580(10) 0.0419(6) Uani 0.11 1 d P . . Ni5 Ni 0.52191(5) 0.47138(6) 0.21282(9) 0.0369(6) Uani 0.11 1 d P . . F1 F 0.3039(2) 0.2671(2) 0.2903(3) 0.0545(18) Uani 1 1 d . A . F2 F 0.3810(2) 0.2737(2) 0.2657(3) 0.0508(18) Uani 1 1 d . A . F3 F 0.45587(18) 0.34076(18) 0.3021(3) 0.0365(15) Uani 1 1 d . A . F4 F 0.48964(18) 0.41019(18) 0.2223(3) 0.0352(15) Uani 1 1 d . A . F5 F 0.49691(19) 0.4643(2) 0.1248(3) 0.0437(16) Uani 1 1 d . A . F6 F 0.4734(2) 0.4734(2) 0.2500 0.034(2) Uani 1 2 d S A . O1 O 0.2367(7) 0.2760(7) 0.3410(10) 0.061(5) Uiso 0.50 1 d PU A 1 O2 O 0.3051(5) 0.2018(5) 0.2124(8) 0.044(4) Uiso 0.50 1 d PDU A 1 C1 C 0.2876(9) 0.2111(10) 0.1597(12) 0.047(9) Uiso 0.50 1 d PDU A 1 C2 C 0.2929(10) 0.1938(9) 0.0842(15) 0.110(11) Uiso 0.50 1 d PDU A 1 C3 C 0.2643(13) 0.2031(13) 0.033(2) 0.135(15) Uiso 0.50 1 d PDU A 1 C4 C 0.2744(13) 0.1448(10) 0.099(2) 0.137(16) Uiso 0.50 1 d PDU A 1 C5 C 0.3411(11) 0.2170(15) 0.060(3) 0.20(2) Uiso 0.50 1 d PDU A 1 O1A O 0.2206(6) 0.2545(6) 0.3243(9) 0.047(4) Uiso 0.50 1 d PU A 2 O2A O 0.3172(6) 0.2223(7) 0.1809(11) 0.069(5) Uiso 0.50 1 d PDU A 2 C1A C 0.2831(11) 0.2185(15) 0.1494(16) 0.075(12) Uiso 0.50 1 d PDU A 2 C2A C 0.2783(11) 0.1993(12) 0.0707(17) 0.132(13) Uiso 0.50 1 d PDU A 2 C3A C 0.2995(16) 0.2400(13) 0.022(2) 0.160(19) Uiso 0.50 1 d PDU A 2 C4A C 0.2284(12) 0.1700(17) 0.064(3) 0.23(3) Uiso 0.50 1 d PDU A 2 C5A C 0.3037(18) 0.1744(18) 0.064(3) 0.20(2) Uiso 0.50 1 d PDU A 2 O3 O 0.2235(5) 0.1961(6) 0.3185(10) 0.061(5) Uiso 0.50 1 d PDU A 1 O4 O 0.2723(6) 0.1768(6) 0.3067(12) 0.077(6) Uiso 0.50 1 d PDU A 1 C6 C 0.2368(8) 0.1736(8) 0.332(2) 0.076(11) Uiso 0.50 1 d PDU A 1 C7 C 0.2021(7) 0.1289(7) 0.3600(13) 0.073(9) Uiso 0.50 1 d PDU A 1 C8 C 0.1590(9) 0.1107(11) 0.3165(16) 0.099(11) Uiso 0.50 1 d PDU A 1 C9 C 0.1963(11) 0.1401(12) 0.4376(15) 0.120(13) Uiso 0.50 1 d PDU A 1 C10 C 0.2204(13) 0.0971(12) 0.358(2) 0.142(16) Uiso 0.50 1 d PDU A 1 O3A O 0.2225(4) 0.1858(5) 0.2730(8) 0.040(4) Uiso 0.50 1 d PDU A 2 O4A O 0.2699(5) 0.1868(5) 0.3514(8) 0.045(4) Uiso 0.50 1 d PDU A 2 C6A C 0.2339(6) 0.1696(7) 0.3151(15) 0.048(8) Uiso 0.50 1 d PDU A 2 C7A C 0.1981(8) 0.1246(8) 0.3393(15) 0.099(12) Uiso 0.50 1 d PDU A 2 C8A C 0.1551(10) 0.1241(13) 0.358(2) 0.125(14) Uiso 0.50 1 d PDU A 2 C9A C 0.2168(14) 0.1171(15) 0.410(2) 0.156(17) Uiso 0.50 1 d PDU A 2 C10A C 0.1916(15) 0.0909(13) 0.281(2) 0.159(18) Uiso 0.50 1 d PDU A 2 O5 O 0.3416(5) 0.1854(5) 0.3250(9) 0.042(4) Uiso 0.50 1 d PDU A 1 O6 O 0.4095(6) 0.2177(6) 0.2920(14) 0.085(7) Uiso 0.50 1 d PDU A 1 C11 C 0.3747(7) 0.1851(7) 0.312(2) 0.058(11) Uiso 0.50 1 d PDU A 1 C12 C 0.3755(6) 0.1433(6) 0.3108(12) 0.062(12) Uiso 0.50 1 d PDU A 1 C13 C 0.3959(10) 0.1426(12) 0.2403(13) 0.101(13) Uiso 0.50 1 d PDU A 1 C14 C 0.3293(7) 0.1061(9) 0.3161(17) 0.092(11) Uiso 0.50 1 d PDU A 1 C15 C 0.4027(9) 0.1425(9) 0.3724(13) 0.076(9) Uiso 0.50 1 d PDU A 1 O5A O 0.3492(6) 0.1876(7) 0.2754(12) 0.083(6) Uiso 0.50 1 d PDU A 2 O6A O 0.4120(4) 0.2208(4) 0.3310(8) 0.027(3) Uiso 0.50 1 d PDU A 2 C11A C 0.3798(7) 0.1880(6) 0.305(2) 0.052(10) Uiso 0.50 1 d PDU A 2 C12A C 0.3790(7) 0.1456(6) 0.3130(12) 0.058(12) Uiso 0.50 1 d PDU A 2 C13A C 0.3739(12) 0.1275(11) 0.2386(13) 0.087(10) Uiso 0.50 1 d PDU A 2 C14A C 0.3392(11) 0.1158(12) 0.357(2) 0.127(15) Uiso 0.50 1 d PDU A 2 C15A C 0.4202(9) 0.1521(10) 0.3473(17) 0.086(10) Uiso 0.50 1 d PDU A 2 O7 O 0.3437(5) 0.2551(6) 0.3997(9) 0.046(4) Uiso 0.50 1 d PDU A 1 O8 O 0.4129(5) 0.2742(6) 0.3952(9) 0.048(5) Uiso 0.50 1 d PDU A 1 C16 C 0.3811(9) 0.2705(12) 0.4268(11) 0.053(10) Uiso 0.50 1 d PDU A 1 C17 C 0.3869(11) 0.2874(10) 0.5061(14) 0.112(12) Uiso 0.50 1 d PDU A 1 C18 C 0.4057(16) 0.2642(15) 0.546(2) 0.16(2) Uiso 0.50 1 d PDU A 1 C19 C 0.3427(13) 0.2767(17) 0.532(3) 0.20(2) Uiso 0.50 1 d PDU A 1 C20 C 0.4175(15) 0.3357(11) 0.502(3) 0.164(19) Uiso 0.50 1 d PDU A 1 O7A O 0.3386(5) 0.2348(6) 0.3870(9) 0.048(5) Uiso 0.50 1 d PDU A 2 O8A O 0.4083(4) 0.2867(5) 0.4050(8) 0.029(4) Uiso 0.50 1 d PDU A 2 C16A C 0.3702(8) 0.2632(9) 0.4224(10) 0.035(8) Uiso 0.50 1 d PDU A 2 C17A C 0.3615(10) 0.2700(9) 0.5028(13) 0.083(9) Uiso 0.50 1 d PDU A 2 C18A C 0.3823(18) 0.2495(17) 0.545(2) 0.19(2) Uiso 0.50 1 d PDU A 2 C19A C 0.3129(11) 0.2468(15) 0.511(3) 0.17(2) Uiso 0.50 1 d PDU A 2 C20A C 0.3814(15) 0.3182(10) 0.513(2) 0.153(17) Uiso 0.50 1 d PDU A 2 O9 O 0.4488(6) 0.2804(6) 0.2000(12) 0.065(6) Uiso 0.50 1 d PDU A 1 O10 O 0.5052(6) 0.3453(5) 0.1878(10) 0.047(6) Uiso 0.50 1 d PDU A 1 C21 C 0.4803(8) 0.3088(7) 0.1666(10) 0.028(9) Uiso 0.50 1 d PDU A 1 C22 C 0.4861(6) 0.2932(6) 0.0962(9) 0.046(6) Uiso 0.50 1 d PDU A 1 C23 C 0.5348(6) 0.3157(9) 0.0810(16) 0.091(10) Uiso 0.50 1 d PDU A 1 C24 C 0.4639(9) 0.3066(8) 0.0393(13) 0.074(9) Uiso 0.50 1 d PDU A 1 C25 C 0.4658(8) 0.2436(6) 0.0974(14) 0.070(8) Uiso 0.50 1 d PDU A 1 O9A O 0.4575(4) 0.2759(4) 0.2258(8) 0.024(4) Uiso 0.50 1 d PDU A 2 O10A O 0.4916(5) 0.3408(4) 0.1760(8) 0.023(5) Uiso 0.50 1 d PDU A 2 C21A C 0.4726(9) 0.3011(6) 0.1736(10) 0.028(9) Uiso 0.50 1 d PDU A 2 C22A C 0.4668(7) 0.2789(6) 0.1042(10) 0.054(7) Uiso 0.50 1 d PDU A 2 C23A C 0.4903(9) 0.2527(9) 0.1088(15) 0.068(8) Uiso 0.50 1 d PDU A 2 C24A C 0.4886(9) 0.3127(8) 0.0445(13) 0.072(8) Uiso 0.50 1 d PDU A 2 C25A C 0.4177(8) 0.2511(11) 0.090(2) 0.126(14) Uiso 0.50 1 d PDU A 2 O11 O 0.4850(3) 0.2897(4) 0.3626(6) 0.028(3) Uiso 0.60 1 d PDU A 1 O12 O 0.5366(4) 0.3446(4) 0.3008(7) 0.031(3) Uiso 0.60 1 d PDU A 1 C26 C 0.5226(5) 0.3143(6) 0.3433(16) 0.040(8) Uiso 0.60 1 d PDU A 1 C27 C 0.5545(6) 0.3036(6) 0.3809(10) 0.066(9) Uiso 0.60 1 d PDU A 1 C28 C 0.5991(8) 0.3279(9) 0.3467(16) 0.132(12) Uiso 0.60 1 d PDU A 1 C29 C 0.5362(9) 0.2541(6) 0.3772(15) 0.090(10) Uiso 0.60 1 d PDU A 1 C30 C 0.5563(8) 0.3176(7) 0.4585(10) 0.077(7) Uiso 0.60 1 d PDU A 1 O11A O 0.4839(6) 0.2796(7) 0.3243(13) 0.061(6) Uiso 0.40 1 d PDU A 2 O12A O 0.5324(7) 0.3492(6) 0.3293(14) 0.057(7) Uiso 0.40 1 d PDU A 2 C26A C 0.5188(7) 0.3106(8) 0.343(2) 0.045(12) Uiso 0.40 1 d PDU A 2 C27A C 0.5551(7) 0.3026(8) 0.3687(14) 0.069(13) Uiso 0.40 1 d PDU A 2 C28A C 0.5847(8) 0.3061(9) 0.3067(13) 0.043(7) Uiso 0.40 1 d PDU A 2 C29A C 0.5361(13) 0.2583(10) 0.405(2) 0.091(15) Uiso 0.40 1 d PDU A 2 C30A C 0.5840(13) 0.3401(11) 0.4189(19) 0.101(13) Uiso 0.40 1 d PDU A 2 O13 O 0.5237(3) 0.4112(3) 0.3506(4) 0.066(3) Uani 1 1 d . A . O14 O 0.5449(2) 0.4775(2) 0.3099(4) 0.0386(19) Uani 1 1 d . A . O15 O 0.5683(3) 0.4134(3) 0.2288(5) 0.065(3) Uani 1 1 d . A . O16 O 0.5713(2) 0.4696(2) 0.1738(4) 0.044(2) Uani 1 1 d . A . O17 O 0.5568(2) 0.5334(3) 0.2056(4) 0.044(2) Uani 1 1 d . A . C31 C 0.5386(4) 0.4502(5) 0.3575(7) 0.051(3) Uani 1 1 d . . . C32 C 0.5474(5) 0.4662(4) 0.4347(7) 0.060(4) Uani 1 1 d . A . C33 C 0.5774(5) 0.4510(6) 0.4652(7) 0.082(5) Uani 1 1 d . . . C34 C 0.5058(4) 0.4463(4) 0.4739(7) 0.061(4) Uani 1 1 d . . . C35 C 0.5705(5) 0.5166(4) 0.4367(7) 0.073(4) Uani 1 1 d . . . C36 C 0.5867(4) 0.4472(5) 0.1926(7) 0.049(3) Uani 1 1 d . . . C37 C 0.6330(6) 0.4628(6) 0.1750(10) 0.043(7) Uiso 0.60 1 d PDU A 1 C38 C 0.6422(14) 0.4878(10) 0.1044(13) 0.127(16) Uiso 0.60 1 d PDU A 1 C39 C 0.6407(12) 0.4245(8) 0.1669(16) 0.122(11) Uiso 0.60 1 d PDU A 1 C40 C 0.6607(8) 0.4928(7) 0.2351(11) 0.071(7) Uiso 0.60 1 d PDU A 1 C37A C 0.6310(12) 0.4584(8) 0.1575(15) 0.080(15) Uiso 0.40 1 d PDU A 2 C38A C 0.6492(10) 0.5011(9) 0.1164(14) 0.028(7) Uiso 0.40 1 d PDU A 2 C39A C 0.6286(11) 0.4205(9) 0.1159(18) 0.067(10) Uiso 0.40 1 d PDU A 2 C40A C 0.6555(12) 0.4647(12) 0.2275(16) 0.077(11) Uiso 0.40 1 d PDU A 2 C41 C 0.5616(4) 0.5616(4) 0.2500 0.037(4) Uani 1 2 d SD . . C42 C 0.6036(5) 0.6036(5) 0.2500 0.047(4) Uani 1 2 d SD A . C43 C 0.6281(8) 0.6037(9) 0.1854(13) 0.079(9) Uiso 0.50 1 d PD A 1 C44 C 0.6283(7) 0.6032(8) 0.3145(13) 0.070(8) Uiso 0.50 1 d PD A 1 C45A C 0.6390(6) 0.5932(8) 0.2440(15) 0.069(8) Uiso 0.50 1 d PD A 2 N1 N 0.4180(7) 0.4014(7) 0.145(2) 0.044(15) Uiso 0.50 1 d PDU B 1 N2 N 0.3523(7) 0.3741(10) 0.1722(15) 0.076(9) Uiso 0.50 1 d PDU B 1 C70 C 0.3871(11) 0.4123(10) 0.149(2) 0.083(16) Uiso 0.50 1 d PDU B 1 C71 C 0.3603(11) 0.3408(9) 0.171(2) 0.083(10) Uiso 0.50 1 d PDU B 1 C72 C 0.4019(12) 0.3578(9) 0.146(2) 0.057(13) Uiso 0.50 1 d PDU B 1 N1A N 0.4163(6) 0.4018(7) 0.1338(19) 0.035(14) Uiso 0.50 1 d PD C 2 N2A N 0.3510(6) 0.3576(8) 0.1587(13) 0.053(7) Uiso 0.50 1 d PD C 2 C70A C 0.3808(6) 0.4012(8) 0.1582(14) 0.020(7) Uiso 0.50 1 d PD C 2 C71A C 0.3700(8) 0.3335(6) 0.1467(14) 0.042(7) Uiso 0.50 1 d PD C 2 C72A C 0.4133(11) 0.3622(10) 0.137(2) 0.067(15) Uiso 0.50 1 d PD C 2 O100 O 0.2778(10) 0.0000 0.2500 0.227(14) Uiso 1 2 d S . . O101 O 0.6667 0.3333 0.144(6) 0.67(6) Uiso 1.50 3 d SP . . O102 O 0.6667 0.3333 0.542(3) 0.42(3) Uiso 1.50 3 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0364(12) 0.0364(12) 0.093(2) 0.0136(8) -0.0136(8) 0.0125(13) Cr2 0.0457(13) 0.0360(12) 0.126(2) -0.0033(12) -0.0331(13) 0.0172(10) Cr3 0.0491(13) 0.0441(13) 0.0791(16) 0.0127(10) 0.0153(11) 0.0292(11) Cr4 0.0429(12) 0.0397(11) 0.0490(12) -0.0041(9) -0.0051(9) 0.0251(9) Cr5 0.0348(11) 0.0399(11) 0.0398(11) -0.0032(8) 0.0020(8) 0.0214(9) Ni1 0.0364(12) 0.0364(12) 0.093(2) 0.0136(8) -0.0136(8) 0.0125(13) Ni2 0.0457(13) 0.0360(12) 0.126(2) -0.0033(12) -0.0331(13) 0.0172(10) Ni3 0.0491(13) 0.0441(13) 0.0791(16) 0.0127(10) 0.0153(11) 0.0292(11) Ni4 0.0429(12) 0.0397(11) 0.0490(12) -0.0041(9) -0.0051(9) 0.0251(9) Ni5 0.0348(11) 0.0399(11) 0.0398(11) -0.0032(8) 0.0020(8) 0.0214(9) F1 0.058(4) 0.053(4) 0.055(4) -0.004(3) -0.010(3) 0.030(4) F2 0.060(4) 0.057(4) 0.041(4) -0.013(3) -0.008(3) 0.033(4) F3 0.045(4) 0.039(4) 0.034(3) -0.001(3) 0.000(3) 0.028(3) F4 0.038(3) 0.040(4) 0.031(3) -0.003(3) 0.001(3) 0.022(3) F5 0.045(4) 0.050(4) 0.038(4) 0.003(3) 0.002(3) 0.024(3) F6 0.035(4) 0.035(4) 0.036(5) -0.0030(19) 0.0030(19) 0.021(4) O13 0.105(8) 0.034(6) 0.045(5) -0.006(4) -0.027(5) 0.025(5) O14 0.040(5) 0.037(5) 0.040(5) -0.004(4) -0.007(4) 0.020(4) O15 0.044(5) 0.047(6) 0.105(8) 0.012(6) 0.003(5) 0.024(5) O16 0.038(5) 0.050(5) 0.046(5) -0.010(4) 0.000(4) 0.024(4) O17 0.034(4) 0.049(5) 0.049(5) -0.004(4) 0.004(4) 0.021(4) C31 0.035(7) 0.061(10) 0.051(9) -0.015(8) -0.011(6) 0.020(7) C32 0.073(10) 0.058(9) 0.046(8) -0.021(7) -0.023(7) 0.031(8) C33 0.105(13) 0.121(14) 0.054(9) -0.036(9) -0.037(9) 0.081(12) C34 0.056(9) 0.072(10) 0.044(8) 0.003(7) -0.001(7) 0.024(8) C35 0.100(12) 0.038(8) 0.064(9) -0.026(7) -0.023(8) 0.023(8) C36 0.045(8) 0.070(10) 0.047(8) -0.017(7) -0.007(6) 0.040(8) C41 0.034(7) 0.034(7) 0.048(11) -0.004(4) 0.004(4) 0.021(8) C42 0.044(8) 0.044(8) 0.065(12) 0.000(4) 0.000(4) 0.030(9) _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 Cr1 O1A 1.801(16) 4 ? Cr1 O1A 1.801(16) . ? Cr1 F1 1.954(7) . ? Cr1 F1 1.954(7) 4 ? Cr1 O3A 1.981(14) 4 ? Cr1 O3A 1.981(14) . ? Cr1 O3 2.062(18) 4 ? Cr1 O3 2.062(18) . ? Cr1 O1 2.15(2) . ? Cr1 O1 2.15(2) 4 ? Cr2 O7A 1.785(16) . ? Cr2 O2 1.798(15) . ? Cr2 O4 1.878(19) . ? Cr2 F1 1.920(7) . ? Cr2 F2 1.956(7) . ? Cr2 O5 1.978(14) . ? Cr2 O5A 2.07(2) . ? Cr2 O4A 2.074(16) . ? Cr2 O7 2.162(18) . ? Cr2 O2A 2.20(2) . ? Cr3 O8 1.756(17) . ? Cr3 O9A 1.867(13) . ? Cr3 O11A 1.91(2) . ? Cr3 F2 1.914(7) . ? Cr3 O6A 1.921(13) . ? Cr3 F3 1.925(6) . ? Cr3 O6 1.99(2) . ? Cr3 O11 2.044(11) . ? Cr3 O8A 2.087(17) . ? Cr3 O9 2.15(2) . ? Cr4 O10 1.827(17) . ? Cr4 F3 1.893(6) . ? Cr4 F4 1.903(6) . ? Cr4 O15 1.933(9) . ? Cr4 O13 1.935(9) . ? Cr4 O12 1.939(12) . ? Cr4 O12A 1.96(2) . ? Cr4 O10A 2.056(15) . ? Cr5 F5 1.858(6) . ? Cr5 F4 1.921(6) . ? Cr5 F6 1.922(4) . ? Cr5 O17 1.949(8) . ? Cr5 O16 1.960(8) . ? Cr5 O14 1.991(8) . ? F6 Ni5 1.922(4) 4 ? F6 Cr5 1.922(4) 4 ? O1 C1 1.19(3) 4 ? O2 C1 1.31(3) . ? C1 O1 1.19(3) 4 ? C1 C2 1.61(3) . ? C2 C4 1.572(19) . ? C2 C3 1.574(19) . ? C2 C5 1.575(19) . ? O1A C1A 1.18(3) 4 ? O2A C1A 1.31(3) . ? C1A O1A 1.18(3) 4 ? C1A C2A 1.62(3) . ? C2A C4A 1.572(19) . ? C2A C3A 1.573(19) . ? C2A C5A 1.575(19) . ? O3 C6 1.16(2) . ? O4 C6 1.32(2) . ? C6 C7 1.56(2) . ? C7 C9 1.572(19) . ? C7 C8 1.584(18) . ? C7 C10 1.586(19) . ? O3A C6A 1.179(19) . ? O4A C6A 1.32(2) . ? C6A C7A 1.56(2) . ? C7A C10A 1.577(19) . ? C7A C8A 1.583(19) . ? C7A C9A 1.583(19) . ? O5 C11 1.23(2) . ? O6 C11 1.27(2) . ? C11 C12 1.52(2) . ? C12 C14 1.534(17) . ? C12 C13 1.536(17) . ? C12 C15 1.538(16) . ? O5A C11A 1.23(2) . ? O6A C11A 1.27(2) . ? C11A C12A 1.52(2) . ? C12A C15A 1.531(16) . ? C12A C13A 1.532(17) . ? C12A C14A 1.537(17) . ? O7 C16 1.28(2) . ? O8 C16 1.24(2) . ? C16 C17 1.60(3) . ? C17 C18 1.516(17) . ? C17 C19 1.525(17) . ? C17 C20 1.531(17) . ? O7A C16A 1.28(2) . ? O8A C16A 1.25(2) . ? C16A C17A 1.60(3) . ? C17A C18A 1.523(17) . ? C17A C20A 1.525(17) . ? C17A C19A 1.529(17) . ? O9 C21 1.26(2) . ? O10 C21 1.233(19) . ? C21 C22 1.51(2) . ? C22 C23 1.552(16) . ? C22 C25 1.558(15) . ? C22 C24 1.560(15) . ? O9A C21A 1.27(2) . ? O10A C21A 1.242(18) . ? C21A C22A 1.50(2) . ? C22A C23A 1.557(16) . ? C22A C24A 1.560(16) . ? C22A C25A 1.562(16) . ? O11 C26 1.249(19) . ? O12 C26 1.245(18) . ? C26 C27 1.56(2) . ? C27 C28 1.541(15) . ? C27 C30 1.551(15) . ? C27 C29 1.566(14) . ? O11A C26A 1.25(2) . ? O12A C26A 1.25(2) . ? C26A C27A 1.55(2) . ? C27A C29A 1.547(15) . ? C27A C28A 1.552(16) . ? C27A C30A 1.555(16) . ? O13 C31 1.236(15) . ? O14 C31 1.272(15) . ? O15 C36 1.262(16) . ? O16 C36 1.242(14) . ? O17 C41 1.266(10) . ? C31 C32 1.551(17) . ? C32 C34 1.499(19) . ? C32 C33 1.551(19) . ? C32 C35 1.575(19) . ? C36 C37 1.51(2) . ? C36 C37A 1.59(4) . ? C37 C40 1.548(15) . ? C37 C39 1.551(15) . ? C37 C38 1.556(15) . ? C37A C39A 1.545(16) . ? C37A C38A 1.551(16) . ? C37A C40A 1.552(16) . ? C41 O17 1.266(10) 4 ? C41 C42 1.51(2) . ? C42 C45A 1.51(2) 4 ? C42 C45A 1.51(2) . ? C42 C43 1.51(2) 4 ? C42 C43 1.51(2) . ? C42 C44 1.52(2) . ? C42 C44 1.52(2) 4 ? C43 C44 1.55(4) 4 ? C44 C43 1.55(4) 4 ? N1 C70 1.36(2) . ? N1 C72 1.38(2) . ? N2 C71 1.37(3) . ? N2 C70 1.39(3) . ? C71 C72 1.39(3) . ? N1A C70A 1.356(19) . ? N1A C72A 1.38(2) . ? N2A C71A 1.37(3) . ? N2A C70A 1.39(3) . ? C71A C72A 1.39(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Cr1 O1A 157.7(12) 4 . ? O1A Cr1 F1 95.7(6) 4 . ? O1A Cr1 F1 100.1(6) . . ? O1A Cr1 F1 100.1(6) 4 4 ? O1A Cr1 F1 95.7(6) . 4 ? F1 Cr1 F1 90.1(4) . 4 ? O1A Cr1 O3A 90.9(7) 4 4 ? O1A Cr1 O3A 71.4(8) . 4 ? F1 Cr1 O3A 169.2(5) . 4 ? F1 Cr1 O3A 97.3(5) 4 4 ? O1A Cr1 O3A 71.4(7) 4 . ? O1A Cr1 O3A 90.8(7) . . ? F1 Cr1 O3A 97.3(5) . . ? F1 Cr1 O3A 169.2(5) 4 . ? O3A Cr1 O3A 76.6(8) 4 . ? O1A Cr1 O3 67.7(7) 4 4 ? O1A Cr1 O3 97.2(8) . 4 ? F1 Cr1 O3 162.7(6) . 4 ? F1 Cr1 O3 88.3(5) 4 4 ? O3A Cr1 O3 26.7(5) 4 4 ? O3A Cr1 O3 82.3(7) . 4 ? O1A Cr1 O3 97.2(8) 4 . ? O1A Cr1 O3 67.7(7) . . ? F1 Cr1 O3 88.3(5) . . ? F1 Cr1 O3 162.7(6) 4 . ? O3A Cr1 O3 82.3(7) 4 . ? O3A Cr1 O3 26.7(5) . . ? O3 Cr1 O3 98.2(10) 4 . ? O1A Cr1 O1 177.3(10) 4 . ? O1A Cr1 O1 20.0(7) . . ? F1 Cr1 O1 84.9(6) . . ? F1 Cr1 O1 82.6(6) 4 . ? O3A Cr1 O1 88.2(7) 4 . ? O3A Cr1 O1 105.9(7) . . ? O3 Cr1 O1 111.9(8) 4 . ? O3 Cr1 O1 80.1(8) . . ? O1A Cr1 O1 20.0(7) 4 4 ? O1A Cr1 O1 177.3(10) . 4 ? F1 Cr1 O1 82.6(6) . 4 ? F1 Cr1 O1 84.9(6) 4 4 ? O3A Cr1 O1 105.9(7) 4 4 ? O3A Cr1 O1 88.2(7) . 4 ? O3 Cr1 O1 80.1(8) 4 4 ? O3 Cr1 O1 111.9(8) . 4 ? O1 Cr1 O1 162.3(12) . 4 ? O7A Cr2 O2 160.2(8) . . ? O7A Cr2 O4 96.1(9) . . ? O2 Cr2 O4 69.2(9) . . ? O7A Cr2 F1 97.5(7) . . ? O2 Cr2 F1 97.7(5) . . ? O4 Cr2 F1 98.6(6) . . ? O7A Cr2 F2 93.9(5) . . ? O2 Cr2 F2 99.0(6) . . ? O4 Cr2 F2 166.7(7) . . ? F1 Cr2 F2 88.8(3) . . ? O7A Cr2 O5 70.7(8) . . ? O2 Cr2 O5 92.5(7) . . ? O4 Cr2 O5 76.5(7) . . ? F1 Cr2 O5 166.3(5) . . ? F2 Cr2 O5 98.7(5) . . ? O7A Cr2 O5A 95.7(9) . . ? O2 Cr2 O5A 70.7(7) . . ? O4 Cr2 O5A 85.0(8) . . ? F1 Cr2 O5A 165.9(7) . . ? F2 Cr2 O5A 85.2(6) . . ? O5 Cr2 O5A 27.8(6) . . ? O7A Cr2 O4A 72.9(6) . . ? O2 Cr2 O4A 95.2(7) . . ? O4 Cr2 O4A 27.1(7) . . ? F1 Cr2 O4A 87.9(5) . . ? F2 Cr2 O4A 165.8(5) . . ? O5 Cr2 O4A 82.0(6) . . ? O5A Cr2 O4A 100.8(8) . . ? O7A Cr2 O7 17.4(7) . . ? O2 Cr2 O7 175.4(7) . . ? O4 Cr2 O7 106.3(8) . . ? F1 Cr2 O7 82.0(5) . . ? F2 Cr2 O7 85.6(5) . . ? O5 Cr2 O7 87.1(7) . . ? O5A Cr2 O7 110.2(7) . . ? O4A Cr2 O7 80.2(6) . . ? O7A Cr2 O2A 172.3(7) . . ? O2 Cr2 O2A 22.7(6) . . ? O4 Cr2 O2A 90.1(9) . . ? F1 Cr2 O2A 86.1(6) . . ? F2 Cr2 O2A 79.3(6) . . ? O5 Cr2 O2A 106.5(7) . . ? O5A Cr2 O2A 80.2(8) . . ? O4A Cr2 O2A 114.2(7) . . ? O7 Cr2 O2A 161.0(7) . . ? O8 Cr3 O9A 164.1(8) . . ? O8 Cr3 O11A 100.3(10) . . ? O9A Cr3 O11A 66.7(9) . . ? O8 Cr3 F2 95.3(6) . . ? O9A Cr3 F2 96.6(5) . . ? O11A Cr3 F2 162.7(8) . . ? O8 Cr3 O6A 76.0(8) . . ? O9A Cr3 O6A 91.7(6) . . ? O11A Cr3 O6A 77.5(7) . . ? F2 Cr3 O6A 99.5(4) . . ? O8 Cr3 F3 96.7(7) . . ? O9A Cr3 F3 94.2(4) . . ? O11A Cr3 F3 97.5(6) . . ? F2 Cr3 F3 87.8(3) . . ? O6A Cr3 F3 170.0(5) . . ? O8 Cr3 O6 96.1(10) . . ? O9A Cr3 O6 73.7(7) . . ? O11A Cr3 O6 82.3(9) . . ? F2 Cr3 O6 88.8(7) . . ? O6A Cr3 O6 22.0(7) . . ? F3 Cr3 O6 167.0(7) . . ? O8 Cr3 O11 79.9(6) . . ? O9A Cr3 O11 88.8(6) . . ? O11A Cr3 O11 23.3(7) . . ? F2 Cr3 O11 173.9(4) . . ? O6A Cr3 O11 83.1(5) . . ? F3 Cr3 O11 89.0(4) . . ? O6 Cr3 O11 95.4(8) . . ? O8 Cr3 O8A 14.4(7) . . ? O9A Cr3 O8A 175.0(6) . . ? O11A Cr3 O8A 108.8(9) . . ? F2 Cr3 O8A 88.0(5) . . ? O6A Cr3 O8A 89.4(6) . . ? F3 Cr3 O8A 84.1(4) . . ? O6 Cr3 O8A 108.3(8) . . ? O11 Cr3 O8A 86.5(5) . . ? O8 Cr3 O9 174.0(7) . . ? O9A Cr3 O9 16.6(6) . . ? O11A Cr3 O9 82.7(10) . . ? F2 Cr3 O9 81.0(6) . . ? O6A Cr3 O9 99.9(7) . . ? F3 Cr3 O9 87.9(5) . . ? O6 Cr3 O9 79.2(9) . . ? O11 Cr3 O9 104.0(7) . . ? O8A Cr3 O9 166.7(8) . . ? O10 Cr4 F3 95.9(6) . . ? O10 Cr4 F4 94.8(7) . . ? F3 Cr4 F4 88.5(2) . . ? O10 Cr4 O15 83.2(6) . . ? F3 Cr4 O15 178.3(3) . . ? F4 Cr4 O15 93.1(3) . . ? O10 Cr4 O13 173.5(8) . . ? F3 Cr4 O13 88.1(4) . . ? F4 Cr4 O13 90.5(3) . . ? O15 Cr4 O13 92.7(4) . . ? O10 Cr4 O12 80.6(8) . . ? F3 Cr4 O12 95.9(4) . . ? F4 Cr4 O12 173.9(5) . . ? O15 Cr4 O12 82.5(4) . . ? O13 Cr4 O12 93.9(5) . . ? O10 Cr4 O12A 97.3(10) . . ? F3 Cr4 O12A 87.8(7) . . ? F4 Cr4 O12A 167.6(8) . . ? O15 Cr4 O12A 90.9(7) . . ? O13 Cr4 O12A 77.7(8) . . ? O12 Cr4 O12A 18.0(7) . . ? O10 Cr4 O10A 12.7(8) . . ? F3 Cr4 O10A 87.1(5) . . ? F4 Cr4 O10A 85.5(4) . . ? O15 Cr4 O10A 92.2(5) . . ? O13 Cr4 O10A 173.7(6) . . ? O12 Cr4 O10A 90.5(6) . . ? O12A Cr4 O10A 106.1(8) . . ? F5 Cr5 F4 87.3(3) . . ? F5 Cr5 F6 87.1(2) . . ? F4 Cr5 F6 88.3(3) . . ? F5 Cr5 O17 94.9(3) . . ? F4 Cr5 O17 177.3(3) . . ? F6 Cr5 O17 93.4(3) . . ? F5 Cr5 O16 92.3(3) . . ? F4 Cr5 O16 92.1(3) . . ? F6 Cr5 O16 179.3(3) . . ? O17 Cr5 O16 86.3(3) . . ? F5 Cr5 O14 176.2(3) . . ? F4 Cr5 O14 91.2(3) . . ? F6 Cr5 O14 89.5(2) . . ? O17 Cr5 O14 86.8(3) . . ? O16 Cr5 O14 91.2(3) . . ? Cr2 F1 Cr1 118.5(3) . . ? Cr3 F2 Cr2 119.8(3) . . ? Cr4 F3 Cr3 122.5(3) . . ? Cr4 F4 Cr5 123.6(3) . . ? Ni5 F6 Cr5 0.00(13) 4 4 ? Ni5 F6 Cr5 128.3(4) 4 . ? Cr5 F6 Cr5 128.3(4) 4 . ? C1 O1 Cr1 121.1(18) 4 . ? C1 O2 Cr2 131.2(15) . . ? O1 C1 O2 127(2) 4 . ? O1 C1 C2 116(2) 4 . ? O2 C1 C2 115(2) . . ? C4 C2 C3 113.5(14) . . ? C4 C2 C5 112.8(14) . . ? C3 C2 C5 111.9(14) . . ? C4 C2 C1 102(2) . . ? C3 C2 C1 105(2) . . ? C5 C2 C1 112(3) . . ? C1A O1A Cr1 137(2) 4 . ? C1A O2A Cr2 122.1(17) . . ? O1A C1A O2A 127(2) 4 . ? O1A C1A C2A 121(2) 4 . ? O2A C1A C2A 111(2) . . ? C4A C2A C3A 116(3) . . ? C4A C2A C5A 114(2) . . ? C3A C2A C5A 110(2) . . ? C4A C2A C1A 102(2) . . ? C3A C2A C1A 104(3) . . ? C5A C2A C1A 111(3) . . ? C6 O3 Cr1 129.5(17) . . ? C6 O4 Cr2 126.1(18) . . ? O3 C6 O4 125(2) . . ? O3 C6 C7 113.6(19) . . ? O4 C6 C7 117.4(18) . . ? C6 C7 C9 101(2) . . ? C6 C7 C8 111.6(19) . . ? C9 C7 C8 111.7(13) . . ? C6 C7 C10 109(2) . . ? C9 C7 C10 111.7(13) . . ? C8 C7 C10 111.2(12) . . ? C6A O3A Cr1 129.1(15) . . ? C6A O4A Cr2 115.7(14) . . ? O3A C6A O4A 128.9(18) . . ? O3A C6A C7A 113.9(17) . . ? O4A C6A C7A 116.3(17) . . ? C6A C7A C10A 109(2) . . ? C6A C7A C8A 112(2) . . ? C10A C7A C8A 112(2) . . ? C6A C7A C9A 103(2) . . ? C10A C7A C9A 112(2) . . ? C8A C7A C9A 108(2) . . ? C11 O5 Cr2 128.6(16) . . ? C11 O6 Cr3 130.4(18) . . ? O5 C11 O6 124.5(19) . . ? O5 C11 C12 120.9(18) . . ? O6 C11 C12 114.4(18) . . ? C11 C12 C14 108.4(17) . . ? C11 C12 C13 105.9(17) . . ? C14 C12 C13 111.3(12) . . ? C11 C12 C15 109.6(17) . . ? C14 C12 C15 110.9(12) . . ? C13 C12 C15 110.5(12) . . ? C11A O5A Cr2 126.6(19) . . ? C11A O6A Cr3 127.0(15) . . ? O5A C11A O6A 125.8(18) . . ? O5A C11A C12A 117.8(18) . . ? O6A C11A C12A 116.3(17) . . ? C11A C12A C15A 111.1(17) . . ? C11A C12A C13A 105.8(17) . . ? C15A C12A C13A 111.1(19) . . ? C11A C12A C14A 107.4(19) . . ? C15A C12A C14A 112(2) . . ? C13A C12A C14A 109(2) . . ? C16 O7 Cr2 126.1(13) . . ? C16 O8 Cr3 138.7(17) . . ? O8 C16 O7 124.5(18) . . ? O8 C16 C17 119(2) . . ? O7 C16 C17 117(2) . . ? C18 C17 C19 113.3(14) . . ? C18 C17 C20 112.9(14) . . ? C19 C17 C20 111.9(14) . . ? C18 C17 C16 106(2) . . ? C19 C17 C16 107(3) . . ? C20 C17 C16 105(2) . . ? C16A O7A Cr2 134.3(15) . . ? C16A O8A Cr3 121.9(13) . . ? O8A C16A O7A 129.9(17) . . ? O8A C16A C17A 113(2) . . ? O7A C16A C17A 117.5(19) . . ? C18A C17A C20A 115(2) . . ? C18A C17A C19A 113(2) . . ? C20A C17A C19A 112(2) . . ? C18A C17A C16A 105(2) . . ? C20A C17A C16A 106(2) . . ? C19A C17A C16A 106(3) . . ? C21 O9 Cr3 129.2(14) . . ? C21 O10 Cr4 137.4(15) . . ? O10 C21 O9 125.7(17) . . ? O10 C21 C22 121.8(18) . . ? O9 C21 C22 112.5(17) . . ? C21 C22 C23 107.6(17) . . ? C21 C22 C25 110.0(18) . . ? C23 C22 C25 111.1(12) . . ? C21 C22 C24 108.3(16) . . ? C23 C22 C24 109.4(12) . . ? C25 C22 C24 110.4(12) . . ? C21A O9A Cr3 131.2(13) . . ? C21A O10A Cr4 125.9(12) . . ? O10A C21A O9A 126.0(15) . . ? O10A C21A C22A 119.7(17) . . ? O9A C21A C22A 114.3(15) . . ? C21A C22A C23A 107.5(17) . . ? C21A C22A C24A 109.9(16) . . ? C23A C22A C24A 107.5(17) . . ? C21A C22A C25A 108(2) . . ? C23A C22A C25A 114.1(19) . . ? C24A C22A C25A 109.9(18) . . ? C26 O11 Cr3 124.7(12) . . ? C26 O12 Cr4 130.6(13) . . ? O12 C26 O11 129.4(14) . . ? O12 C26 C27 119.3(14) . . ? O11 C26 C27 111.4(13) . . ? C28 C27 C30 110.8(12) . . ? C28 C27 C26 110.9(17) . . ? C30 C27 C26 105.7(16) . . ? C28 C27 C29 110.8(12) . . ? C30 C27 C29 109.8(12) . . ? C26 C27 C29 108.7(15) . . ? C26A O11A Cr3 127(2) . . ? C26A O12A Cr4 132.1(19) . . ? O11A C26A O12A 126(2) . . ? O11A C26A C27A 119(2) . . ? O12A C26A C27A 112.0(18) . . ? C29A C27A C28A 111(2) . . ? C29A C27A C26A 110.4(19) . . ? C28A C27A C26A 111(2) . . ? C29A C27A C30A 113(2) . . ? C28A C27A C30A 105.2(19) . . ? C26A C27A C30A 106.7(19) . . ? C31 O13 Cr4 129.6(8) . . ? C31 O14 Cr5 132.2(7) . . ? C36 O15 Cr4 135.9(8) . . ? C36 O16 Cr5 128.6(8) . . ? C41 O17 Cr5 128.8(8) . . ? O13 C31 O14 127.8(11) . . ? O13 C31 C32 114.6(12) . . ? O14 C31 C32 117.4(12) . . ? C34 C32 C33 110.6(12) . . ? C34 C32 C31 108.9(10) . . ? C33 C32 C31 105.7(11) . . ? C34 C32 C35 111.5(12) . . ? C33 C32 C35 109.8(12) . . ? C31 C32 C35 110.1(11) . . ? O16 C36 O15 126.4(11) . . ? O16 C36 C37 117.7(14) . . ? O15 C36 C37 115.7(12) . . ? O16 C36 C37A 115.9(14) . . ? O15 C36 C37A 117.0(13) . . ? C37 C36 C37A 13.1(13) . . ? C36 C37 C40 107.8(16) . . ? C36 C37 C39 110.3(18) . . ? C40 C37 C39 110.8(12) . . ? C36 C37 C38 107(2) . . ? C40 C37 C38 110.9(13) . . ? C39 C37 C38 110.4(13) . . ? C39A C37A C38A 115(2) . . ? C39A C37A C40A 110(2) . . ? C38A C37A C40A 111(2) . . ? C39A C37A C36 113(2) . . ? C38A C37A C36 110(2) . . ? C40A C37A C36 96(2) . . ? O17 C41 O17 123.9(14) . 4 ? O17 C41 C42 118.1(7) . . ? O17 C41 C42 118.1(7) 4 . ? C45A C42 C45A 145(2) 4 . ? C45A C42 C41 107.5(11) 4 . ? C45A C42 C41 107.5(11) . . ? C45A C42 C43 51.1(15) 4 4 ? C45A C42 C43 116.9(16) . 4 ? C41 C42 C43 107.1(12) . 4 ? C45A C42 C43 116.9(16) 4 . ? C45A C42 C43 51.0(15) . . ? C41 C42 C43 107.1(12) . . ? C43 C42 C43 146(2) 4 . ? C45A C42 C44 110.0(16) 4 . ? C45A C42 C44 58.9(15) . . ? C41 C42 C44 106.8(11) . . ? C43 C42 C44 61.3(16) 4 . ? C43 C42 C44 108.1(17) . . ? C45A C42 C44 58.9(15) 4 4 ? C45A C42 C44 110.0(16) . 4 ? C41 C42 C44 106.8(11) . 4 ? C43 C42 C44 108.1(17) 4 4 ? C43 C42 C44 61.3(16) . 4 ? C44 C42 C44 146(2) . 4 ? C42 C43 C44 59.6(10) . 4 ? C42 C44 C43 59.1(10) . 4 ? C70 N1 C72 113(2) . . ? C71 N2 C70 112.3(19) . . ? N1 C70 N2 101(2) . . ? N2 C71 C72 106.1(19) . . ? N1 C72 C71 105(2) . . ? C70A N1A C72A 113(2) . . ? C71A N2A C70A 111.5(16) . . ? N1A C70A N2A 102.0(17) . . ? N2A C71A C72A 106.5(17) . . ? N1A C72A C71A 105(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7A Cr2 F1 Cr1 -127.9(6) . . . . ? O2 Cr2 F1 Cr1 39.4(7) . . . . ? O4 Cr2 F1 Cr1 -30.5(8) . . . . ? F2 Cr2 F1 Cr1 138.3(4) . . . . ? O5 Cr2 F1 Cr1 -98(2) . . . . ? O5A Cr2 F1 Cr1 73(2) . . . . ? O4A Cr2 F1 Cr1 -55.5(5) . . . . ? O7 Cr2 F1 Cr1 -135.9(6) . . . . ? O2A Cr2 F1 Cr1 58.9(6) . . . . ? O1A Cr1 F1 Cr2 -45.2(7) 4 . . . ? O1A Cr1 F1 Cr2 118.9(7) . . . . ? F1 Cr1 F1 Cr2 -145.4(5) 4 . . . ? O3A Cr1 F1 Cr2 82(3) 4 . . . ? O3A Cr1 F1 Cr2 26.7(6) . . . . ? O3 Cr1 F1 Cr2 -60.8(19) 4 . . . ? O3 Cr1 F1 Cr2 51.9(6) . . . . ? O1 Cr1 F1 Cr2 132.1(6) . . . . ? O1 Cr1 F1 Cr2 -60.5(7) 4 . . . ? O8 Cr3 F2 Cr2 -46.4(7) . . . . ? O9A Cr3 F2 Cr2 123.0(5) . . . . ? O11A Cr3 F2 Cr2 108(2) . . . . ? O6A Cr3 F2 Cr2 30.2(6) . . . . ? F3 Cr3 F2 Cr2 -143.0(4) . . . . ? O6 Cr3 F2 Cr2 49.6(7) . . . . ? O11 Cr3 F2 Cr2 -84(4) . . . . ? O8A Cr3 F2 Cr2 -58.8(5) . . . . ? O9 Cr3 F2 Cr2 128.8(6) . . . . ? O7A Cr2 F2 Cr3 41.9(7) . . . . ? O2 Cr2 F2 Cr3 -123.0(6) . . . . ? O4 Cr2 F2 Cr3 -97(3) . . . . ? F1 Cr2 F2 Cr3 139.4(4) . . . . ? O5 Cr2 F2 Cr3 -29.1(6) . . . . ? O5A Cr2 F2 Cr3 -53.5(7) . . . . ? O4A Cr2 F2 Cr3 63(2) . . . . ? O7 Cr2 F2 Cr3 57.3(5) . . . . ? O2A Cr2 F2 Cr3 -134.4(6) . . . . ? O10 Cr4 F3 Cr3 47.1(7) . . . . ? F4 Cr4 F3 Cr3 141.7(4) . . . . ? O15 Cr4 F3 Cr3 -11(12) . . . . ? O13 Cr4 F3 Cr3 -127.8(4) . . . . ? O12 Cr4 F3 Cr3 -34.0(5) . . . . ? O12A Cr4 F3 Cr3 -50.1(8) . . . . ? O10A Cr4 F3 Cr3 56.2(5) . . . . ? O8 Cr3 F3 Cr4 133.2(6) . . . . ? O9A Cr3 F3 Cr4 -35.3(6) . . . . ? O11A Cr3 F3 Cr4 31.8(8) . . . . ? F2 Cr3 F3 Cr4 -131.7(4) . . . . ? O6A Cr3 F3 Cr4 91(3) . . . . ? O6 Cr3 F3 Cr4 -56(3) . . . . ? O11 Cr3 F3 Cr4 53.5(5) . . . . ? O8A Cr3 F3 Cr4 140.0(5) . . . . ? O9 Cr3 F3 Cr4 -50.6(6) . . . . ? O10 Cr4 F4 Cr5 -120.3(6) . . . . ? F3 Cr4 F4 Cr5 143.9(3) . . . . ? O15 Cr4 F4 Cr5 -36.9(4) . . . . ? O13 Cr4 F4 Cr5 55.9(4) . . . . ? O12 Cr4 F4 Cr5 -80(4) . . . . ? O12A Cr4 F4 Cr5 72(3) . . . . ? O10A Cr4 F4 Cr5 -128.8(5) . . . . ? F5 Cr5 F4 Cr4 141.9(4) . . . . ? F6 Cr5 F4 Cr4 -130.9(3) . . . . ? O17 Cr5 F4 Cr4 -2(6) . . . . ? O16 Cr5 F4 Cr4 49.7(4) . . . . ? O14 Cr5 F4 Cr4 -41.5(4) . . . . ? F5 Cr5 F6 Ni5 -108.8(2) . . . 4 ? F4 Cr5 F6 Ni5 163.87(18) . . . 4 ? O17 Cr5 F6 Ni5 -14.0(2) . . . 4 ? O16 Cr5 F6 Ni5 -78(30) . . . 4 ? O14 Cr5 F6 Ni5 72.7(2) . . . 4 ? F5 Cr5 F6 Cr5 -108.8(2) . . . 4 ? F4 Cr5 F6 Cr5 163.87(18) . . . 4 ? O17 Cr5 F6 Cr5 -14.0(2) . . . 4 ? O16 Cr5 F6 Cr5 -78(30) . . . 4 ? O14 Cr5 F6 Cr5 72.7(2) . . . 4 ? O1A Cr1 O1 C1 -102(18) 4 . . 4 ? O1A Cr1 O1 C1 -65(3) . . . 4 ? F1 Cr1 O1 C1 156(2) . . . 4 ? F1 Cr1 O1 C1 65(2) 4 . . 4 ? O3A Cr1 O1 C1 -33(2) 4 . . 4 ? O3A Cr1 O1 C1 -108(2) . . . 4 ? O3 Cr1 O1 C1 -20(2) 4 . . 4 ? O3 Cr1 O1 C1 -115(2) . . . 4 ? O1 Cr1 O1 C1 110(2) 4 . . 4 ? O7A Cr2 O2 C1 149(3) . . . . ? O4 Cr2 O2 C1 105(2) . . . . ? F1 Cr2 O2 C1 9(2) . . . . ? F2 Cr2 O2 C1 -81(2) . . . . ? O5 Cr2 O2 C1 180(2) . . . . ? O5A Cr2 O2 C1 -163(3) . . . . ? O4A Cr2 O2 C1 98(2) . . . . ? O7 Cr2 O2 C1 95(9) . . . . ? O2A Cr2 O2 C1 -51(2) . . . . ? Cr2 O2 C1 O1 -10(5) . . . 4 ? Cr2 O2 C1 C2 154.6(17) . . . . ? O1 C1 C2 C4 -140(3) 4 . . . ? O2 C1 C2 C4 54(3) . . . . ? O1 C1 C2 C3 -21(3) 4 . . . ? O2 C1 C2 C3 172(2) . . . . ? O1 C1 C2 C5 100(3) 4 . . . ? O2 C1 C2 C5 -66(3) . . . . ? O1A Cr1 O1A C1A -145(4) 4 . . 4 ? F1 Cr1 O1A C1A 81(4) . . . 4 ? F1 Cr1 O1A C1A -10(4) 4 . . 4 ? O3A Cr1 O1A C1A -106(4) 4 . . 4 ? O3A Cr1 O1A C1A 179(4) . . . 4 ? O3 Cr1 O1A C1A -99(4) 4 . . 4 ? O3 Cr1 O1A C1A 165(4) . . . 4 ? O1 Cr1 O1A C1A 40(4) . . . 4 ? O1 Cr1 O1A C1A -112(19) 4 . . 4 ? O7A Cr2 O2A C1A -162(6) . . . . ? O2 Cr2 O2A C1A 77(3) . . . . ? O4 Cr2 O2A C1A 55(3) . . . . ? F1 Cr2 O2A C1A -44(3) . . . . ? F2 Cr2 O2A C1A -133(3) . . . . ? O5 Cr2 O2A C1A 131(3) . . . . ? O5A Cr2 O2A C1A 140(3) . . . . ? O4A Cr2 O2A C1A 42(3) . . . . ? O7 Cr2 O2A C1A -95(4) . . . . ? Cr2 O2A C1A O1A 6(6) . . . 4 ? Cr2 O2A C1A C2A -160.6(19) . . . . ? O1A C1A C2A C4A -24(5) 4 . . . ? O2A C1A C2A C4A 143(4) . . . . ? O1A C1A C2A C3A 97(4) 4 . . . ? O2A C1A C2A C3A -96(4) . . . . ? O1A C1A C2A C5A -146(4) 4 . . . ? O2A C1A C2A C5A 22(4) . . . . ? O1A Cr1 O3 C6 49(3) 4 . . . ? O1A Cr1 O3 C6 -148(3) . . . . ? F1 Cr1 O3 C6 -46(3) . . . . ? F1 Cr1 O3 C6 -131(3) 4 . . . ? O3A Cr1 O3 C6 139(3) 4 . . . ? O3A Cr1 O3 C6 64(3) . . . . ? O3 Cr1 O3 C6 118(3) 4 . . . ? O1 Cr1 O3 C6 -131(3) . . . . ? O1 Cr1 O3 C6 35(3) 4 . . . ? O7A Cr2 O4 C6 74(3) . . . . ? O2 Cr2 O4 C6 -120(3) . . . . ? F1 Cr2 O4 C6 -25(3) . . . . ? F2 Cr2 O4 C6 -148(3) . . . . ? O5 Cr2 O4 C6 142(3) . . . . ? O5A Cr2 O4 C6 169(3) . . . . ? O4A Cr2 O4 C6 43(2) . . . . ? O7 Cr2 O4 C6 60(3) . . . . ? O2A Cr2 O4 C6 -111(3) . . . . ? Cr1 O3 C6 O4 2(6) . . . . ? Cr1 O3 C6 C7 -155.6(17) . . . . ? Cr2 O4 C6 O3 44(5) . . . . ? Cr2 O4 C6 C7 -159.9(18) . . . . ? O3 C6 C7 C9 -77(3) . . . . ? O4 C6 C7 C9 124(3) . . . . ? O3 C6 C7 C8 42(4) . . . . ? O4 C6 C7 C8 -118(3) . . . . ? O3 C6 C7 C10 165(3) . . . . ? O4 C6 C7 C10 6(4) . . . . ? O1A Cr1 O3A C6A 113(2) 4 . . . ? O1A Cr1 O3A C6A -81(2) . . . . ? F1 Cr1 O3A C6A 20(2) . . . . ? F1 Cr1 O3A C6A 152(2) 4 . . . ? O3A Cr1 O3A C6A -151(3) 4 . . . ? O3 Cr1 O3A C6A -178(2) 4 . . . ? O3 Cr1 O3A C6A -52(2) . . . . ? O1 Cr1 O3A C6A -67(2) . . . . ? O1 Cr1 O3A C6A 102(2) 4 . . . ? O7A Cr2 O4A C6A 167.3(18) . . . . ? O2 Cr2 O4A C6A -28.7(17) . . . . ? O4 Cr2 O4A C6A -44.7(19) . . . . ? F1 Cr2 O4A C6A 68.8(16) . . . . ? F2 Cr2 O4A C6A 145.7(18) . . . . ? O5 Cr2 O4A C6A -120.5(17) . . . . ? O5A Cr2 O4A C6A -100.0(17) . . . . ? O7 Cr2 O4A C6A 151.1(17) . . . . ? O2A Cr2 O4A C6A -16.0(18) . . . . ? Cr1 O3A C6A O4A -11(4) . . . . ? Cr1 O3A C6A C7A 156.9(16) . . . . ? Cr2 O4A C6A O3A -42(4) . . . . ? Cr2 O4A C6A C7A 150.2(17) . . . . ? O3A C6A C7A C10A 78(3) . . . . ? O4A C6A C7A C10A -112(3) . . . . ? O3A C6A C7A C8A -47(3) . . . . ? O4A C6A C7A C8A 123(3) . . . . ? O3A C6A C7A C9A -163(3) . . . . ? O4A C6A C7A C9A 7(3) . . . . ? O7A Cr2 O5 C11 -106(3) . . . . ? O2 Cr2 O5 C11 84(3) . . . . ? O4 Cr2 O5 C11 152(3) . . . . ? F1 Cr2 O5 C11 -137(3) . . . . ? F2 Cr2 O5 C11 -15(3) . . . . ? O5A Cr2 O5 C11 47(3) . . . . ? O4A Cr2 O5 C11 179(3) . . . . ? O7 Cr2 O5 C11 -100(3) . . . . ? O2A Cr2 O5 C11 66(3) . . . . ? O8 Cr3 O6 C11 38(3) . . . . ? O9A Cr3 O6 C11 -155(3) . . . . ? O11A Cr3 O6 C11 137(3) . . . . ? F2 Cr3 O6 C11 -57(3) . . . . ? O6A Cr3 O6 C11 62(3) . . . . ? F3 Cr3 O6 C11 -133(3) . . . . ? O11 Cr3 O6 C11 118(3) . . . . ? O8A Cr3 O6 C11 30(3) . . . . ? O9 Cr3 O6 C11 -139(3) . . . . ? Cr2 O5 C11 O6 19(5) . . . . ? Cr2 O5 C11 C12 -154.0(17) . . . . ? Cr3 O6 C11 O5 26(6) . . . . ? Cr3 O6 C11 C12 -160.1(19) . . . . ? O5 C11 C12 C14 9(4) . . . . ? O6 C11 C12 C14 -165(3) . . . . ? O5 C11 C12 C13 129(3) . . . . ? O6 C11 C12 C13 -45(3) . . . . ? O5 C11 C12 C15 -112(3) . . . . ? O6 C11 C12 C15 74(3) . . . . ? O7A Cr2 O5A C11A -31(3) . . . . ? O2 Cr2 O5A C11A 164(3) . . . . ? O4 Cr2 O5A C11A -127(3) . . . . ? F1 Cr2 O5A C11A 128(3) . . . . ? F2 Cr2 O5A C11A 63(3) . . . . ? O5 Cr2 O5A C11A -56(3) . . . . ? O4A Cr2 O5A C11A -104(3) . . . . ? O7 Cr2 O5A C11A -21(3) . . . . ? O2A Cr2 O5A C11A 143(3) . . . . ? O8 Cr3 O6A C11A 112(2) . . . . ? O9A Cr3 O6A C11A -79(2) . . . . ? O11A Cr3 O6A C11A -144(3) . . . . ? F2 Cr3 O6A C11A 18(2) . . . . ? F3 Cr3 O6A C11A 155(3) . . . . ? O6 Cr3 O6A C11A -44(3) . . . . ? O11 Cr3 O6A C11A -167(2) . . . . ? O8A Cr3 O6A C11A 106(2) . . . . ? O9 Cr3 O6A C11A -64(2) . . . . ? Cr2 O5A C11A O6A -30(5) . . . . ? Cr2 O5A C11A C12A 148.1(19) . . . . ? Cr3 O6A C11A O5A -21(5) . . . . ? Cr3 O6A C11A C12A 160.9(15) . . . . ? O5A C11A C12A C15A 177(3) . . . . ? O6A C11A C12A C15A -4(4) . . . . ? O5A C11A C12A C13A 56(4) . . . . ? O6A C11A C12A C13A -125(3) . . . . ? O5A C11A C12A C14A -60(4) . . . . ? O6A C11A C12A C14A 118(3) . . . . ? O7A Cr2 O7 C16 79(3) . . . . ? O2 Cr2 O7 C16 144(8) . . . . ? O4 Cr2 O7 C16 135(2) . . . . ? F1 Cr2 O7 C16 -129(2) . . . . ? F2 Cr2 O7 C16 -39(2) . . . . ? O5 Cr2 O7 C16 60(2) . . . . ? O5A Cr2 O7 C16 44(2) . . . . ? O4A Cr2 O7 C16 142(2) . . . . ? O2A Cr2 O7 C16 -77(3) . . . . ? O9A Cr3 O8 C16 -143(3) . . . . ? O11A Cr3 O8 C16 -177(4) . . . . ? F2 Cr3 O8 C16 -5(4) . . . . ? O6A Cr3 O8 C16 -103(4) . . . . ? F3 Cr3 O8 C16 84(4) . . . . ? O6 Cr3 O8 C16 -94(4) . . . . ? O11 Cr3 O8 C16 172(4) . . . . ? O8A Cr3 O8 C16 55(4) . . . . ? O9 Cr3 O8 C16 -57(11) . . . . ? Cr3 O8 C16 O7 26(6) . . . . ? Cr3 O8 C16 C17 -152(2) . . . . ? Cr2 O7 C16 O8 5(5) . . . . ? Cr2 O7 C16 C17 -177.5(17) . . . . ? O8 C16 C17 C18 -56(4) . . . . ? O7 C16 C17 C18 126(3) . . . . ? O8 C16 C17 C19 -177(3) . . . . ? O7 C16 C17 C19 5(3) . . . . ? O8 C16 C17 C20 64(4) . . . . ? O7 C16 C17 C20 -114(3) . . . . ? O2 Cr2 O7A C16A 141(3) . . . . ? O4 Cr2 O7A C16A -179(3) . . . . ? F1 Cr2 O7A C16A -79(3) . . . . ? F2 Cr2 O7A C16A 10(3) . . . . ? O5 Cr2 O7A C16A 108(3) . . . . ? O5A Cr2 O7A C16A 96(3) . . . . ? O4A Cr2 O7A C16A -165(3) . . . . ? O7 Cr2 O7A C16A -52(3) . . . . ? O2A Cr2 O7A C16A 38(8) . . . . ? O8 Cr3 O8A C16A -77(3) . . . . ? O9A Cr3 O8A C16A -158(7) . . . . ? O11A Cr3 O8A C16A -132.3(19) . . . . ? F2 Cr3 O8A C16A 43.7(19) . . . . ? O6A Cr3 O8A C16A -55.8(19) . . . . ? F3 Cr3 O8A C16A 131.7(19) . . . . ? O6 Cr3 O8A C16A -44(2) . . . . ? O11 Cr3 O8A C16A -138.9(19) . . . . ? O9 Cr3 O8A C16A 78(3) . . . . ? Cr3 O8A C16A O7A -6(4) . . . . ? Cr3 O8A C16A C17A 171.4(15) . . . . ? Cr2 O7A C16A O8A -30(5) . . . . ? Cr2 O7A C16A C17A 152.7(18) . . . . ? O8A C16A C17A C18A -72(3) . . . . ? O7A C16A C17A C18A 106(3) . . . . ? O8A C16A C17A C20A 49(3) . . . . ? O7A C16A C17A C20A -132(3) . . . . ? O8A C16A C17A C19A 168(3) . . . . ? O7A C16A C17A C19A -14(3) . . . . ? O8 Cr3 O9 C21 174(8) . . . . ? O9A Cr3 O9 C21 -79(3) . . . . ? O11A Cr3 O9 C21 -65(2) . . . . ? F2 Cr3 O9 C21 121(2) . . . . ? O6A Cr3 O9 C21 -141(2) . . . . ? F3 Cr3 O9 C21 33(2) . . . . ? O6 Cr3 O9 C21 -148(2) . . . . ? O11 Cr3 O9 C21 -55(2) . . . . ? O8A Cr3 O9 C21 86(4) . . . . ? F3 Cr4 O10 C21 -14(3) . . . . ? F4 Cr4 O10 C21 -103(3) . . . . ? O15 Cr4 O10 C21 164(3) . . . . ? O13 Cr4 O10 C21 113(6) . . . . ? O12 Cr4 O10 C21 81(3) . . . . ? O12A Cr4 O10 C21 74(3) . . . . ? O10A Cr4 O10 C21 -61(4) . . . . ? Cr4 O10 C21 O9 -2(5) . . . . ? Cr4 O10 C21 C22 -179.8(17) . . . . ? Cr3 O9 C21 O10 -11(4) . . . . ? Cr3 O9 C21 C22 167.6(16) . . . . ? O10 C21 C22 C23 32(3) . . . . ? O9 C21 C22 C23 -146(2) . . . . ? O10 C21 C22 C25 153(3) . . . . ? O9 C21 C22 C25 -25(3) . . . . ? O10 C21 C22 C24 -86(3) . . . . ? O9 C21 C22 C24 96(2) . . . . ? O8 Cr3 O9A C21A -154(3) . . . . ? O11A Cr3 O9A C21A -117(2) . . . . ? F2 Cr3 O9A C21A 68(2) . . . . ? O6A Cr3 O9A C21A 167(2) . . . . ? F3 Cr3 O9A C21A -21(2) . . . . ? O6 Cr3 O9A C21A 155(2) . . . . ? O11 Cr3 O9A C21A -110(2) . . . . ? O8A Cr3 O9A C21A -90(8) . . . . ? O9 Cr3 O9A C21A 47(3) . . . . ? O10 Cr4 O10A C21A 86(4) . . . . ? F3 Cr4 O10A C21A -48(2) . . . . ? F4 Cr4 O10A C21A -136(2) . . . . ? O15 Cr4 O10A C21A 131(2) . . . . ? O13 Cr4 O10A C21A -87(5) . . . . ? O12 Cr4 O10A C21A 48(2) . . . . ? O12A Cr4 O10A C21A 39(2) . . . . ? Cr4 O10A C21A O9A 9(4) . . . . ? Cr4 O10A C21A C22A -169.7(16) . . . . ? Cr3 O9A C21A O10A 36(4) . . . . ? Cr3 O9A C21A C22A -145.7(15) . . . . ? O10A C21A C22A C23A 118(3) . . . . ? O9A C21A C22A C23A -60(3) . . . . ? O10A C21A C22A C24A 2(3) . . . . ? O9A C21A C22A C24A -177(2) . . . . ? O10A C21A C22A C25A -118(3) . . . . ? O9A C21A C22A C25A 63(3) . . . . ? O8 Cr3 O11 C26 -147(2) . . . . ? O9A Cr3 O11 C26 44.4(19) . . . . ? O11A Cr3 O11 C26 62(3) . . . . ? F2 Cr3 O11 C26 -109(4) . . . . ? O6A Cr3 O11 C26 136(2) . . . . ? F3 Cr3 O11 C26 -49.8(19) . . . . ? O6 Cr3 O11 C26 118(2) . . . . ? O8A Cr3 O11 C26 -134.0(19) . . . . ? O9 Cr3 O11 C26 38(2) . . . . ? O10 Cr4 O12 C26 -106(2) . . . . ? F3 Cr4 O12 C26 -11(2) . . . . ? F4 Cr4 O12 C26 -147(4) . . . . ? O15 Cr4 O12 C26 169(2) . . . . ? O13 Cr4 O12 C26 77(2) . . . . ? O12A Cr4 O12 C26 52(3) . . . . ? O10A Cr4 O12 C26 -98(2) . . . . ? Cr4 O12 C26 O11 20(5) . . . . ? Cr4 O12 C26 C27 -159.9(13) . . . . ? Cr3 O11 C26 O12 20(4) . . . . ? Cr3 O11 C26 C27 -161.0(12) . . . . ? O12 C26 C27 C28 -12(3) . . . . ? O11 C26 C27 C28 169(2) . . . . ? O12 C26 C27 C30 109(3) . . . . ? O11 C26 C27 C30 -71(2) . . . . ? O12 C26 C27 C29 -134(3) . . . . ? O11 C26 C27 C29 47(3) . . . . ? O8 Cr3 O11A C26A -81(3) . . . . ? O9A Cr3 O11A C26A 108(3) . . . . ? F2 Cr3 O11A C26A 124(3) . . . . ? O6A Cr3 O11A C26A -154(3) . . . . ? F3 Cr3 O11A C26A 17(3) . . . . ? O6 Cr3 O11A C26A -176(3) . . . . ? O11 Cr3 O11A C26A -52(3) . . . . ? O8A Cr3 O11A C26A -69(3) . . . . ? O9 Cr3 O11A C26A 104(3) . . . . ? O10 Cr4 O12A C26A -50(4) . . . . ? F3 Cr4 O12A C26A 46(4) . . . . ? F4 Cr4 O12A C26A 118(4) . . . . ? O15 Cr4 O12A C26A -133(4) . . . . ? O13 Cr4 O12A C26A 134(4) . . . . ? O12 Cr4 O12A C26A -72(4) . . . . ? O10A Cr4 O12A C26A -41(4) . . . . ? Cr3 O11A C26A O12A -32(7) . . . . ? Cr3 O11A C26A C27A 167(2) . . . . ? Cr4 O12A C26A O11A -8(7) . . . . ? Cr4 O12A C26A C27A 154(2) . . . . ? O11A C26A C27A C29A -32(5) . . . . ? O12A C26A C27A C29A 164(4) . . . . ? O11A C26A C27A C28A 91(4) . . . . ? O12A C26A C27A C28A -72(4) . . . . ? O11A C26A C27A C30A -155(4) . . . . ? O12A C26A C27A C30A 42(4) . . . . ? O10 Cr4 O13 C31 103(5) . . . . ? F3 Cr4 O13 C31 -129.0(12) . . . . ? F4 Cr4 O13 C31 -40.6(12) . . . . ? O15 Cr4 O13 C31 52.5(12) . . . . ? O12 Cr4 O13 C31 135.1(12) . . . . ? O12A Cr4 O13 C31 142.8(14) . . . . ? O10A Cr4 O13 C31 -90(4) . . . . ? F5 Cr5 O14 C31 64(5) . . . . ? F4 Cr5 O14 C31 -1.2(10) . . . . ? F6 Cr5 O14 C31 87.0(10) . . . . ? O17 Cr5 O14 C31 -179.5(10) . . . . ? O16 Cr5 O14 C31 -93.3(10) . . . . ? O10 Cr4 O15 C36 97.7(14) . . . . ? F3 Cr4 O15 C36 156(11) . . . . ? F4 Cr4 O15 C36 3.3(13) . . . . ? O13 Cr4 O15 C36 -87.3(13) . . . . ? O12 Cr4 O15 C36 179.1(13) . . . . ? O12A Cr4 O15 C36 -165.0(14) . . . . ? O10A Cr4 O15 C36 88.9(13) . . . . ? F5 Cr5 O16 C36 -128.8(10) . . . . ? F4 Cr5 O16 C36 -41.4(10) . . . . ? F6 Cr5 O16 C36 -159(30) . . . . ? O17 Cr5 O16 C36 136.4(10) . . . . ? O14 Cr5 O16 C36 49.8(10) . . . . ? F5 Cr5 O17 C41 132.1(7) . . . . ? F4 Cr5 O17 C41 -84(6) . . . . ? F6 Cr5 O17 C41 44.7(7) . . . . ? O16 Cr5 O17 C41 -135.9(8) . . . . ? O14 Cr5 O17 C41 -44.5(7) . . . . ? Cr4 O13 C31 O14 9(2) . . . . ? Cr4 O13 C31 C32 -175.4(9) . . . . ? Cr5 O14 C31 O13 18.0(19) . . . . ? Cr5 O14 C31 C32 -157.1(8) . . . . ? O13 C31 C32 C34 -63.1(15) . . . . ? O14 C31 C32 C34 112.7(13) . . . . ? O13 C31 C32 C33 55.8(15) . . . . ? O14 C31 C32 C33 -128.4(13) . . . . ? O13 C31 C32 C35 174.3(12) . . . . ? O14 C31 C32 C35 -10.0(16) . . . . ? Cr5 O16 C36 O15 19.1(18) . . . . ? Cr5 O16 C36 C37 -156.7(10) . . . . ? Cr5 O16 C36 C37A -171.2(13) . . . . ? Cr4 O15 C36 O16 6(2) . . . . ? Cr4 O15 C36 C37 -178.4(11) . . . . ? Cr4 O15 C36 C37A -163.9(14) . . . . ? O16 C36 C37 C40 87.3(15) . . . . ? O15 C36 C37 C40 -88.9(15) . . . . ? C37A C36 C37 C40 172(6) . . . . ? O16 C36 C37 C39 -151.6(14) . . . . ? O15 C36 C37 C39 32.1(18) . . . . ? C37A C36 C37 C39 -67(6) . . . . ? O16 C36 C37 C38 -31.8(17) . . . . ? O15 C36 C37 C38 152.0(14) . . . . ? C37A C36 C37 C38 53(6) . . . . ? O16 C36 C37A C39A -120.0(19) . . . . ? O15 C36 C37A C39A 51(2) . . . . ? C37 C36 C37A C39A 139(6) . . . . ? O16 C36 C37A C38A 10(2) . . . . ? O15 C36 C37A C38A -179.1(16) . . . . ? C37 C36 C37A C38A -91(6) . . . . ? O16 C36 C37A C40A 125.1(17) . . . . ? O15 C36 C37A C40A -64(2) . . . . ? C37 C36 C37A C40A 24(5) . . . . ? Cr5 O17 C41 O17 -28.7(5) . . . 4 ? Cr5 O17 C41 C42 151.3(5) . . . . ? O17 C41 C42 C45A 135.5(12) . . . 4 ? O17 C41 C42 C45A -44.5(12) 4 . . 4 ? O17 C41 C42 C45A -44.5(12) . . . . ? O17 C41 C42 C45A 135.5(12) 4 . . . ? O17 C41 C42 C43 -170.9(14) . . . 4 ? O17 C41 C42 C43 9.1(14) 4 . . 4 ? O17 C41 C42 C43 9.1(14) . . . . ? O17 C41 C42 C43 -170.9(14) 4 . . . ? O17 C41 C42 C44 -106.5(12) . . . . ? O17 C41 C42 C44 73.5(12) 4 . . . ? O17 C41 C42 C44 73.5(12) . . . 4 ? O17 C41 C42 C44 -106.5(12) 4 . . 4 ? C45A C42 C43 C44 -20.4(17) 4 . . 4 ? C45A C42 C43 C44 -161(2) . . . 4 ? C41 C42 C43 C44 100.2(11) . . . 4 ? C43 C42 C43 C44 -79.8(11) 4 . . 4 ? C44 C42 C43 C44 -145(2) . . . 4 ? C45A C42 C44 C43 15.7(16) 4 . . 4 ? C45A C42 C44 C43 158.7(19) . . . 4 ? C41 C42 C44 C43 -100.7(12) . . . 4 ? C43 C42 C44 C43 144(2) . . . 4 ? C44 C42 C44 C43 79.3(12) 4 . . 4 ? C72 N1 C70 N2 16(5) . . . . ? C71 N2 C70 N1 -9(4) . . . . ? C70 N2 C71 C72 0(4) . . . . ? C70 N1 C72 C71 -16(5) . . . . ? N2 C71 C72 N1 9(4) . . . . ? C72A N1A C70A N2A -16(4) . . . . ? C71A N2A C70A N1A 10(3) . . . . ? C70A N2A C71A C72A -1(3) . . . . ? C70A N1A C72A C71A 16(4) . . . . ? N2A C71A C72A N1A -9(4) . . . . ? _diffrn_measured_fraction_theta_max .995 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full .995 _refine_diff_density_max 1.295 _refine_diff_density_min -.592 _refine_diff_density_rms .142 data_gt275a04 _database_code_depnum_ccdc_archive 'CCDC 268359' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H186.50 Cr8 F12 N4 Ni2 O36.75' _chemical_formula_weight 2842.49 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' 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' Cr Cr 0.3209 0.6236 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5916(19) _cell_length_b 21.808(3) _cell_length_c 27.727(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.890(3) _cell_angle_gamma 90.00 _cell_volume 7596.2(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6341 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 21.15 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2977 _exptl_absorpt_coefficient_mu 0.868 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6863 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 23232 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.0915 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 21.16 _reflns_number_total 9060 _reflns_number_gt 6647 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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. The data were cut at 0.95 angstroms as above this the average I/sigma was less than 2 and therfore on average the data was unobserved. The diffraction pattern indicated the presences of a second set of reflections much weaker than first, however no sensible index of this second set was possible. Several different crystals were tried and this was the best. There are indication in the refinement that the crystal is twinned i.e. most disagreeable reflection list Fobs is greater than Fcalc, and K values larger when Fc/Fc(max) is small. Rotax was used to try and sort out the twinning but could not find a twin law. It is this twinning that have could the high R1 value, however, the clearly shows the metal ring and its interaction with the cation. All non-hydrogens were refined with anisotropic displacement parameters, except the two partially occupied water molecules. Dispalcement parameter restrains were use to model the pivalate ligands. All hydrogen were placed geometrically, however, the hydrogens on the waters could not be found or placed and so have been omitted from the refinement. ; _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^)+(0.1709P)^2^+145.4609P] 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 9060 _refine_ls_number_parameters 755 _refine_ls_number_restraints 409 _refine_ls_R_factor_all 0.1506 _refine_ls_R_factor_gt 0.1248 _refine_ls_wR_factor_ref 0.3729 _refine_ls_wR_factor_gt 0.3563 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.080 _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 Cr1 Cr -0.04869(17) 1.18217(9) -0.09465(7) 0.0330(8) Uani 0.68(3) 1 d P . 1 Ni1 Ni -0.04869(17) 1.18217(9) -0.09465(7) 0.0330(8) Uani 0.32(3) 1 d P . 2 Cr2 Cr -0.0458(2) 1.24421(10) 0.01732(8) 0.0401(7) Uani 1 1 d . . . Cr3 Cr 0.03301(19) 1.20426(10) 0.13184(8) 0.0364(6) Uani 1 1 d . . . Cr4 Cr 0.0574(2) 1.07122(10) 0.19536(8) 0.0392(7) Uani 1 1 d . . . Cr5 Cr 0.06453(15) 0.92103(8) 0.16534(7) 0.0340(7) Uani 0.32(3) 1 d P . 1 Ni5 Ni 0.06453(15) 0.92103(8) 0.16534(7) 0.0340(7) Uani 0.68(3) 1 d P . 2 F1 F 0.0050(6) 1.1853(3) -0.0269(2) 0.0367(19) Uani 1 1 d . . . F2 F -0.0358(6) 1.1854(3) 0.0685(3) 0.0392(19) Uani 1 1 d . . . F3 F 0.0751(6) 1.1198(3) 0.1383(3) 0.0397(19) Uani 1 1 d . . . F4 F 0.0117(6) 1.0062(3) 0.1532(3) 0.040(2) Uani 1 1 d . . . F5 F 0.0605(6) 0.9071(3) 0.0938(3) 0.039(2) Uani 1 1 d . . . F6 F 0.0974(6) 0.8312(4) 0.1610(3) 0.042(2) Uani 1 1 d . . . C1 C -0.1213(13) 0.9539(7) 0.0380(6) 0.048(4) Uani 1 1 d . . . H1 H -0.1160 0.9119 0.0467 0.057 Uiso 1 1 calc R . . N2 N -0.1080(11) 1.0009(6) 0.0670(4) 0.049(3) Uani 1 1 d . . . H2 H -0.0933 0.9977 0.0984 0.058 Uiso 1 1 calc R . . C3 C -0.1192(13) 1.0532(8) 0.0439(6) 0.054(4) Uani 1 1 d . . . H3 H -0.1123 1.0932 0.0574 0.065 Uiso 1 1 calc R . . C4 C -0.1434(12) 1.0379(8) -0.0048(6) 0.049(4) Uani 1 1 d . . . H4 H -0.1566 1.0652 -0.0312 0.059 Uiso 1 1 calc R . . N5 N -0.1439(10) 0.9766(6) -0.0063(5) 0.045(3) Uani 1 1 d . . . C6 C -0.1696(14) 0.9380(9) -0.0506(6) 0.066(5) Uani 1 1 d . . . H6A H -0.1592 0.8941 -0.0426 0.079 Uiso 1 1 calc R . . H6B H -0.1211 0.9488 -0.0760 0.079 Uiso 1 1 calc R . . C7 C -0.2834(13) 0.9489(9) -0.0692(6) 0.064(5) Uani 1 1 d . . . H7A H -0.2905 0.9923 -0.0793 0.076 Uiso 1 1 calc R . . H7B H -0.2983 0.9233 -0.0984 0.076 Uiso 1 1 calc R . . C8 C -0.3652(13) 0.9357(8) -0.0351(6) 0.053(4) Uani 1 1 d . . . H8A H -0.3529 0.9622 -0.0062 0.064 Uiso 1 1 calc R . . H8B H -0.3585 0.8925 -0.0244 0.064 Uiso 1 1 calc R . . C9 C -0.4769(16) 0.9466(10) -0.0574(7) 0.080(6) Uani 1 1 d . . . H9A H -0.5287 0.9372 -0.0337 0.120 Uiso 1 1 calc R . . H9B H -0.4898 0.9199 -0.0857 0.120 Uiso 1 1 calc R . . H9C H -0.4844 0.9896 -0.0674 0.120 Uiso 1 1 calc R . . O11 O -0.1956(8) 1.1893(4) -0.0755(3) 0.039(2) Uani 1 1 d U . . O12 O -0.1924(8) 1.2169(4) 0.0018(3) 0.045(2) Uani 1 1 d U . . C11 C -0.2381(12) 1.1998(7) -0.0369(6) 0.043(3) Uani 1 1 d U . . C12 C -0.3607(13) 1.1902(8) -0.0372(6) 0.054(3) Uani 1 1 d U . . C13 C -0.3983(14) 1.1975(8) 0.0143(6) 0.061(4) Uani 1 1 d U . . H13A H -0.4756 1.1916 0.0135 0.092 Uiso 1 1 calc R . . H13B H -0.3804 1.2387 0.0264 0.092 Uiso 1 1 calc R . . H13C H -0.3630 1.1668 0.0356 0.092 Uiso 1 1 calc R . . C14 C -0.3857(14) 1.1250(9) -0.0570(7) 0.066(4) Uani 1 1 d U . . H14A H -0.3601 1.1210 -0.0894 0.099 Uiso 1 1 calc R . . H14B H -0.4627 1.1180 -0.0585 0.099 Uiso 1 1 calc R . . H14C H -0.3501 1.0945 -0.0355 0.099 Uiso 1 1 calc R . . C15 C -0.4109(15) 1.2373(10) -0.0726(7) 0.070(5) Uani 1 1 d U . . H15A H -0.3833 1.2313 -0.1045 0.106 Uiso 1 1 calc R . . H15B H -0.3932 1.2787 -0.0610 0.106 Uiso 1 1 calc R . . H15C H -0.4884 1.2320 -0.0751 0.106 Uiso 1 1 calc R . . O21 O -0.0366(8) 1.2712(4) -0.1054(3) 0.044(2) Uani 1 1 d U . . O22 O -0.0579(9) 1.3094(4) -0.0300(4) 0.053(3) Uani 1 1 d U . . C21 C -0.0393(14) 1.3159(7) -0.0760(6) 0.051(3) Uani 1 1 d U . . C22 C -0.0248(15) 1.3816(7) -0.0912(6) 0.059(3) Uani 1 1 d U . . C23 C 0.0060(16) 1.3824(8) -0.1443(6) 0.068(4) Uani 1 1 d U . . H23A H 0.0160 1.4248 -0.1546 0.102 Uiso 1 1 calc R . . H23B H -0.0509 1.3633 -0.1651 0.102 Uiso 1 1 calc R . . H23C H 0.0723 1.3594 -0.1469 0.102 Uiso 1 1 calc R . . C24 C 0.0598(16) 1.4087(8) -0.0578(7) 0.070(5) Uani 1 1 d U . . H24A H 0.0721 1.4513 -0.0671 0.105 Uiso 1 1 calc R . . H24B H 0.1257 1.3852 -0.0597 0.105 Uiso 1 1 calc R . . H24C H 0.0375 1.4074 -0.0247 0.105 Uiso 1 1 calc R . . C25 C -0.1278(16) 1.4143(7) -0.0865(8) 0.070(5) Uani 1 1 d U . . H25A H -0.1206 1.4571 -0.0965 0.105 Uiso 1 1 calc R . . H25B H -0.1464 1.4129 -0.0528 0.105 Uiso 1 1 calc R . . H25C H -0.1839 1.3944 -0.1071 0.105 Uiso 1 1 calc R . . C31 C -0.0681(13) 1.3205(7) 0.1024(6) 0.049(4) Uani 1 1 d . . . O31 O -0.1043(9) 1.3046(5) 0.0609(4) 0.051(3) Uani 1 1 d . . . O32 O -0.0067(9) 1.2899(5) 0.1287(4) 0.053(3) Uani 1 1 d . . . C32 C -0.0997(15) 1.3856(7) 0.1202(7) 0.058(5) Uani 1 1 d . . . C33 C 0.0045(17) 1.4241(8) 0.1178(8) 0.076(6) Uani 1 1 d . . . H33A H 0.0222 1.4281 0.0840 0.114 Uiso 1 1 calc R . . H33B H 0.0630 1.4035 0.1364 0.114 Uiso 1 1 calc R . . H33C H -0.0063 1.4650 0.1314 0.114 Uiso 1 1 calc R . . C34 C -0.1293(17) 1.3789(9) 0.1719(6) 0.069(5) Uani 1 1 d . . . H34A H -0.1493 1.4191 0.1843 0.104 Uiso 1 1 calc R . . H34B H -0.0683 1.3628 0.1917 0.104 Uiso 1 1 calc R . . H34C H -0.1895 1.3506 0.1731 0.104 Uiso 1 1 calc R . . C35 C -0.1883(18) 1.4114(9) 0.0880(7) 0.080(6) Uani 1 1 d . . . H35A H -0.1653 1.4153 0.0551 0.120 Uiso 1 1 calc R . . H35B H -0.2079 1.4519 0.1000 0.120 Uiso 1 1 calc R . . H35C H -0.2500 1.3840 0.0879 0.120 Uiso 1 1 calc R . . O41 O 0.1011(8) 1.2710(4) 0.0329(3) 0.044(2) Uani 1 1 d U . . O42 O 0.1637(8) 1.2217(4) 0.1003(4) 0.048(2) Uani 1 1 d U . . C41 C 0.1770(12) 1.2543(6) 0.0639(6) 0.042(3) Uani 1 1 d U . . C42 C 0.2866(13) 1.2776(7) 0.0542(6) 0.049(3) Uani 1 1 d U . . C43 C 0.3702(14) 1.2500(8) 0.0884(7) 0.063(4) Uani 1 1 d U . . H43A H 0.4401 1.2659 0.0811 0.094 Uiso 1 1 calc R . . H43B H 0.3694 1.2053 0.0848 0.094 Uiso 1 1 calc R . . H43C H 0.3558 1.2608 0.1216 0.094 Uiso 1 1 calc R . . C44 C 0.3060(15) 1.2641(9) 0.0001(6) 0.063(4) Uani 1 1 d U . . H44A H 0.2499 1.2836 -0.0208 0.094 Uiso 1 1 calc R . . H44B H 0.3050 1.2197 -0.0054 0.094 Uiso 1 1 calc R . . H44C H 0.3754 1.2807 -0.0073 0.094 Uiso 1 1 calc R . . C45 C 0.2826(14) 1.3499(7) 0.0593(7) 0.061(4) Uani 1 1 d U . . H45A H 0.2272 1.3664 0.0364 0.092 Uiso 1 1 calc R . . H45B H 0.3517 1.3672 0.0523 0.092 Uiso 1 1 calc R . . H45C H 0.2665 1.3607 0.0923 0.092 Uiso 1 1 calc R . . O51 O 0.1094(9) 1.2236(4) 0.1936(3) 0.050(3) Uani 1 1 d U . . O52 O 0.1085(9) 1.1388(4) 0.2379(4) 0.051(3) Uani 1 1 d U . . C51 C 0.1329(13) 1.1935(7) 0.2300(5) 0.047(3) Uani 1 1 d U . . C52 C 0.2008(14) 1.2266(7) 0.2704(6) 0.054(3) Uani 1 1 d U . . C53 C 0.2150(16) 1.1885(8) 0.3147(6) 0.069(5) Uani 1 1 d U . . H53A H 0.2489 1.1496 0.3070 0.104 Uiso 1 1 calc R . . H53B H 0.1454 1.1803 0.3271 0.104 Uiso 1 1 calc R . . H53C H 0.2600 1.2104 0.3392 0.104 Uiso 1 1 calc R . . C54 C 0.1487(16) 1.2881(8) 0.2812(7) 0.067(5) Uani 1 1 d U . . H54A H 0.1393 1.3122 0.2514 0.101 Uiso 1 1 calc R . . H54B H 0.1942 1.3107 0.3051 0.101 Uiso 1 1 calc R . . H54C H 0.0791 1.2808 0.2940 0.101 Uiso 1 1 calc R . . C55 C 0.3106(15) 1.2364(9) 0.2501(7) 0.074(5) Uani 1 1 d U . . H55A H 0.3025 1.2620 0.2211 0.110 Uiso 1 1 calc R . . H55B H 0.3407 1.1966 0.2418 0.110 Uiso 1 1 calc R . . H55C H 0.3582 1.2567 0.2745 0.110 Uiso 1 1 calc R . . O61 O -0.1006(9) 1.1901(5) 0.1599(4) 0.053(3) Uani 1 1 d U . . O62 O -0.0915(9) 1.0978(5) 0.1968(4) 0.052(3) Uani 1 1 d U . . C61 C -0.1423(14) 1.1459(8) 0.1820(6) 0.054(3) Uani 1 1 d U . . C62 C -0.2578(15) 1.1484(10) 0.1916(7) 0.070(3) Uani 1 1 d U . . C63 C -0.2768(17) 1.1295(11) 0.2423(7) 0.082(5) Uani 1 1 d U . . H63A H -0.3532 1.1312 0.2469 0.123 Uiso 1 1 calc R . . H63B H -0.2386 1.1572 0.2652 0.123 Uiso 1 1 calc R . . H63C H -0.2510 1.0875 0.2478 0.123 Uiso 1 1 calc R . . C64 C -0.308(2) 1.2085(14) 0.1742(11) 0.118(7) Uani 1 1 d U . . H64A H -0.2918 1.2159 0.1407 0.177 Uiso 1 1 calc R . . H64B H -0.2799 1.2421 0.1947 0.177 Uiso 1 1 calc R . . H64C H -0.3856 1.2061 0.1761 0.177 Uiso 1 1 calc R . . C65 C -0.3169(19) 1.1017(14) 0.1561(9) 0.110(6) Uani 1 1 d U . . H65A H -0.3051 1.1130 0.1227 0.165 Uiso 1 1 calc R . . H65B H -0.3934 1.1026 0.1608 0.165 Uiso 1 1 calc R . . H65C H -0.2893 1.0603 0.1628 0.165 Uiso 1 1 calc R . . O71 O 0.0335(10) 1.0238(4) 0.2534(3) 0.053(3) Uani 1 1 d U . . O72 O 0.0655(8) 0.9254(4) 0.2371(3) 0.045(2) Uani 1 1 d U . . C71 C 0.0419(14) 0.9680(7) 0.2636(5) 0.049(3) Uani 1 1 d U . . C72 C 0.0180(16) 0.9537(8) 0.3170(6) 0.060(3) Uani 1 1 d U . . C73 C 0.0186(19) 0.8818(8) 0.3236(7) 0.080(5) Uani 1 1 d U . . H73A H -0.0360 0.8635 0.3012 0.121 Uiso 1 1 calc R . . H73B H 0.0035 0.8717 0.3569 0.121 Uiso 1 1 calc R . . H73C H 0.0887 0.8656 0.3169 0.121 Uiso 1 1 calc R . . C74 C -0.0925(18) 0.9791(10) 0.3255(7) 0.084(5) Uani 1 1 d U . . H74A H -0.1458 0.9589 0.3036 0.126 Uiso 1 1 calc R . . H74B H -0.0937 1.0234 0.3194 0.126 Uiso 1 1 calc R . . H74C H -0.1086 0.9714 0.3591 0.126 Uiso 1 1 calc R . . C75 C 0.1013(18) 0.9846(9) 0.3505(7) 0.075(5) Uani 1 1 d U . . H75A H 0.1716 0.9677 0.3450 0.112 Uiso 1 1 calc R . . H75B H 0.0853 0.9772 0.3841 0.112 Uiso 1 1 calc R . . H75C H 0.1010 1.0288 0.3441 0.112 Uiso 1 1 calc R . . O81 O 0.2043(8) 1.0438(4) 0.1962(4) 0.046(2) Uani 1 1 d U . . O82 O 0.2170(8) 0.9480(4) 0.1688(4) 0.047(2) Uani 1 1 d U . . C81 C 0.2555(12) 0.9959(7) 0.1888(6) 0.046(3) Uani 1 1 d U . . C82 C 0.3713(13) 0.9930(7) 0.2104(6) 0.051(3) Uani 1 1 d U . . C83 C 0.4179(15) 1.0583(8) 0.2108(7) 0.067(5) Uani 1 1 d U . . H83A H 0.3738 1.0855 0.2292 0.100 Uiso 1 1 calc R . . H83B H 0.4191 1.0733 0.1775 0.100 Uiso 1 1 calc R . . H83C H 0.4906 1.0576 0.2259 0.100 Uiso 1 1 calc R . . C84 C 0.4375(13) 0.9520(8) 0.1833(7) 0.057(4) Uani 1 1 d U . . H84A H 0.4078 0.9105 0.1833 0.086 Uiso 1 1 calc R . . H84B H 0.5101 0.9514 0.1985 0.086 Uiso 1 1 calc R . . H84C H 0.4390 0.9667 0.1499 0.086 Uiso 1 1 calc R . . C85 C 0.3607(14) 0.9714(8) 0.2623(6) 0.060(4) Uani 1 1 d U . . H85A H 0.3157 1.0001 0.2789 0.090 Uiso 1 1 calc R . . H85B H 0.4313 0.9696 0.2795 0.090 Uiso 1 1 calc R . . H85C H 0.3282 0.9305 0.2620 0.090 Uiso 1 1 calc R . . O91 O -0.0913(8) 0.8995(5) 0.1650(4) 0.046(2) Uani 1 1 d U . . O92 O -0.1007(8) 0.8243(4) 0.1111(3) 0.041(2) Uani 1 1 d U . . C91 C -0.1410(12) 0.8569(7) 0.1424(5) 0.043(3) Uani 1 1 d U . . C92 C -0.2551(13) 0.8444(8) 0.1539(6) 0.057(3) Uani 1 1 d U . . C93 C -0.2727(14) 0.8636(10) 0.2063(6) 0.067(4) Uani 1 1 d U . . H93A H -0.3466 0.8553 0.2132 0.101 Uiso 1 1 calc R . . H93B H -0.2579 0.9075 0.2103 0.101 Uiso 1 1 calc R . . H93C H -0.2247 0.8401 0.2287 0.101 Uiso 1 1 calc R . . C94 C -0.2804(16) 0.7770(9) 0.1465(8) 0.076(5) Uani 1 1 d U . . H94A H -0.3540 0.7691 0.1541 0.114 Uiso 1 1 calc R . . H94B H -0.2319 0.7523 0.1677 0.114 Uiso 1 1 calc R . . H94C H -0.2716 0.7659 0.1127 0.114 Uiso 1 1 calc R . . C95 C -0.3259(15) 0.8820(11) 0.1202(7) 0.078(5) Uani 1 1 d U . . H95A H -0.4003 0.8751 0.1270 0.117 Uiso 1 1 calc R . . H95B H -0.3153 0.8701 0.0868 0.117 Uiso 1 1 calc R . . H95C H -0.3085 0.9255 0.1248 0.117 Uiso 1 1 calc R . . O1W O 0.0000 1.0000 0.5000 0.060(17) Uiso 0.25 2 d SP . . O2W O 0.032(4) 0.923(3) 0.546(2) 0.083(16) Uiso 0.25 1 d P . . 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 Cr1 0.0464(14) 0.0254(12) 0.0254(12) 0.0027(8) -0.0110(9) -0.0002(9) Ni1 0.0464(14) 0.0254(12) 0.0254(12) 0.0027(8) -0.0110(9) -0.0002(9) Cr2 0.0584(16) 0.0260(13) 0.0335(13) 0.0007(10) -0.0154(11) -0.0015(10) Cr3 0.0551(15) 0.0228(12) 0.0298(13) -0.0021(9) -0.0083(11) 0.0002(10) Cr4 0.0593(16) 0.0263(12) 0.0300(13) 0.0024(10) -0.0124(11) -0.0004(11) Cr5 0.0473(13) 0.0241(11) 0.0287(12) -0.0008(8) -0.0118(9) -0.0028(8) Ni5 0.0473(13) 0.0241(11) 0.0287(12) -0.0008(8) -0.0118(9) -0.0028(8) F1 0.050(5) 0.040(4) 0.018(4) -0.002(3) -0.018(3) -0.001(4) F2 0.044(5) 0.026(4) 0.045(5) -0.004(3) -0.013(4) -0.003(3) F3 0.055(5) 0.026(4) 0.037(5) 0.001(3) -0.003(4) 0.001(3) F4 0.063(5) 0.025(4) 0.031(4) 0.005(3) -0.015(4) 0.006(4) F5 0.057(5) 0.030(4) 0.029(4) 0.009(3) -0.015(4) 0.001(4) F6 0.055(5) 0.040(5) 0.030(4) 0.008(3) -0.011(4) 0.002(4) C1 0.064(11) 0.030(8) 0.045(10) -0.014(7) -0.028(8) 0.006(7) N2 0.074(9) 0.035(8) 0.032(7) -0.003(6) -0.027(6) 0.004(6) C3 0.063(11) 0.047(11) 0.048(10) -0.015(8) -0.017(8) -0.016(8) C4 0.041(9) 0.051(11) 0.052(10) 0.008(8) -0.015(8) -0.007(7) N5 0.040(7) 0.049(9) 0.046(8) -0.013(6) -0.011(6) 0.007(6) C6 0.069(12) 0.077(13) 0.050(11) -0.025(9) -0.011(9) -0.002(10) C7 0.056(11) 0.078(13) 0.054(11) -0.026(9) -0.012(9) -0.020(9) C8 0.055(11) 0.057(11) 0.046(10) -0.004(8) -0.010(8) -0.013(8) C9 0.081(14) 0.091(16) 0.066(13) 0.017(11) -0.010(11) -0.029(12) O11 0.056(6) 0.034(5) 0.024(5) -0.006(4) -0.014(4) 0.000(4) O12 0.057(6) 0.040(5) 0.037(5) -0.009(4) -0.009(4) 0.002(4) C11 0.054(5) 0.039(5) 0.035(5) 0.002(5) -0.011(5) 0.003(5) C12 0.054(6) 0.057(7) 0.051(6) 0.004(6) -0.001(6) 0.001(6) C13 0.066(10) 0.060(10) 0.057(8) -0.002(7) 0.001(8) -0.006(8) C14 0.060(10) 0.073(9) 0.064(10) -0.013(8) -0.011(8) -0.005(8) C15 0.057(9) 0.087(11) 0.066(10) 0.019(9) -0.003(8) 0.012(9) O21 0.068(6) 0.028(5) 0.035(5) 0.012(4) -0.008(5) 0.002(4) O22 0.086(7) 0.029(5) 0.041(5) 0.004(4) -0.015(5) 0.000(5) C21 0.077(6) 0.029(5) 0.044(5) 0.009(5) -0.011(5) 0.000(5) C22 0.084(7) 0.032(6) 0.058(6) 0.012(5) -0.014(6) -0.004(6) C23 0.103(12) 0.035(9) 0.064(9) 0.001(7) -0.009(9) -0.022(8) C24 0.095(11) 0.035(8) 0.075(10) 0.006(8) -0.033(9) -0.014(8) C25 0.093(10) 0.026(8) 0.089(11) 0.015(8) -0.012(9) 0.007(7) C31 0.051(10) 0.031(9) 0.063(12) -0.011(8) 0.003(9) -0.006(8) O31 0.067(7) 0.039(6) 0.044(7) -0.002(5) -0.018(6) 0.007(5) O32 0.083(8) 0.030(6) 0.043(6) -0.003(5) -0.019(6) 0.011(6) C32 0.077(12) 0.031(9) 0.067(12) -0.011(8) 0.003(10) 0.011(8) C33 0.107(16) 0.034(10) 0.087(15) -0.001(9) 0.012(12) 0.006(10) C34 0.101(15) 0.053(11) 0.055(12) 0.002(9) 0.010(11) 0.010(10) C35 0.105(16) 0.061(13) 0.071(13) -0.013(10) -0.019(12) 0.027(11) O41 0.064(6) 0.029(5) 0.037(5) -0.001(4) -0.009(4) -0.010(4) O42 0.058(6) 0.031(5) 0.052(6) 0.006(4) -0.021(5) -0.005(4) C41 0.057(5) 0.027(5) 0.042(5) -0.002(5) -0.007(5) -0.003(5) C42 0.059(6) 0.036(6) 0.051(6) -0.001(5) -0.003(6) -0.002(5) C43 0.060(9) 0.058(9) 0.069(10) -0.011(8) -0.003(8) -0.003(8) C44 0.067(10) 0.065(10) 0.057(8) -0.009(8) 0.006(8) -0.008(8) C45 0.060(10) 0.035(7) 0.087(11) -0.005(7) -0.014(9) -0.011(7) O51 0.090(7) 0.028(5) 0.028(5) -0.005(4) -0.017(5) -0.002(5) O52 0.084(7) 0.030(5) 0.035(5) -0.006(4) -0.024(5) -0.004(5) C51 0.077(6) 0.029(5) 0.031(5) -0.006(4) -0.022(5) -0.003(5) C52 0.081(7) 0.039(6) 0.040(6) -0.017(5) -0.022(6) -0.004(6) C53 0.098(12) 0.056(9) 0.046(8) -0.009(7) -0.039(8) 0.007(9) C54 0.094(11) 0.045(8) 0.060(10) -0.009(7) -0.017(9) 0.010(8) C55 0.078(10) 0.075(11) 0.064(10) -0.032(9) -0.018(8) -0.019(9) O61 0.067(6) 0.044(6) 0.047(6) -0.001(4) -0.004(5) 0.009(5) O62 0.064(6) 0.036(5) 0.058(6) 0.001(5) 0.013(5) -0.003(5) C61 0.061(6) 0.047(6) 0.052(6) -0.005(5) 0.001(5) 0.000(5) C62 0.064(7) 0.081(8) 0.067(7) -0.005(7) 0.008(6) -0.001(6) C63 0.074(11) 0.105(13) 0.068(10) -0.011(9) 0.013(9) -0.008(10) C64 0.087(13) 0.133(13) 0.135(15) 0.022(12) 0.013(13) 0.036(11) C65 0.088(12) 0.156(15) 0.084(12) -0.022(12) 0.003(11) -0.035(12) O71 0.093(7) 0.031(5) 0.032(5) 0.000(4) -0.005(5) -0.001(5) O72 0.069(6) 0.034(5) 0.030(5) 0.003(4) -0.016(5) 0.002(5) C71 0.080(6) 0.035(5) 0.031(5) 0.004(4) -0.011(5) 0.000(5) C72 0.093(8) 0.049(6) 0.037(6) 0.007(5) -0.004(6) -0.007(6) C73 0.138(14) 0.052(9) 0.050(10) 0.004(8) -0.003(10) -0.016(9) C74 0.106(11) 0.087(12) 0.060(10) 0.009(10) 0.025(9) 0.000(10) C75 0.109(12) 0.067(10) 0.047(9) 0.002(8) -0.004(9) -0.015(9) O81 0.053(6) 0.029(5) 0.054(6) -0.002(4) -0.023(5) 0.000(4) O82 0.048(5) 0.030(5) 0.058(6) -0.002(4) -0.015(5) -0.002(4) C81 0.051(5) 0.029(5) 0.056(6) 0.001(5) -0.016(5) 0.000(4) C82 0.052(6) 0.037(6) 0.060(6) -0.007(5) -0.021(6) -0.006(5) C83 0.065(10) 0.045(8) 0.087(11) -0.004(8) -0.018(9) -0.015(7) C84 0.046(8) 0.047(8) 0.077(10) 0.005(8) -0.010(8) 0.001(7) C85 0.067(10) 0.050(9) 0.059(8) 0.009(7) -0.031(7) 0.004(8) O91 0.051(5) 0.041(5) 0.043(5) -0.006(4) -0.009(5) 0.005(4) O92 0.058(6) 0.032(5) 0.032(5) 0.001(4) -0.011(4) 0.000(4) C91 0.050(5) 0.041(6) 0.036(5) -0.008(5) -0.011(5) 0.000(5) C92 0.053(6) 0.064(7) 0.052(7) -0.009(6) 0.000(6) -0.001(6) C93 0.059(10) 0.087(11) 0.056(9) -0.005(8) 0.003(8) -0.007(9) C94 0.066(11) 0.082(10) 0.083(12) -0.023(9) 0.021(9) -0.023(9) C95 0.057(9) 0.102(12) 0.073(10) -0.002(10) -0.006(9) 0.010(9) _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 Cr1 F1 1.953(7) . ? Cr1 F5 1.953(7) 3_575 ? Cr1 F6 1.922(7) 3_575 ? Cr1 O11 1.965(10) . ? Cr1 O21 1.971(9) . ? Cr1 O92 1.971(10) 3_575 ? Cr2 F1 1.916(8) . ? Cr2 F2 1.911(8) . ? Cr2 O12 1.959(10) . ? Cr2 O22 1.934(10) . ? Cr2 O31 1.964(11) . ? Cr2 O41 1.960(10) . ? Cr3 F2 1.948(7) . ? Cr3 F3 1.922(7) . ? Cr3 O32 1.933(10) . ? Cr3 O42 1.953(11) . ? Cr3 O51 1.952(9) . ? Cr3 O61 1.926(12) . ? Cr4 F3 1.930(8) . ? Cr4 F4 1.903(7) . ? Cr4 O52 1.970(9) . ? Cr4 O62 1.965(11) . ? Cr4 O71 1.953(10) . ? Cr4 O81 1.943(10) . ? Cr5 F4 1.993(7) . ? Cr5 F5 2.003(7) . ? Cr5 F6 2.007(8) . ? Cr5 O72 1.991(9) . ? Cr5 O82 2.004(10) . ? Cr5 O91 2.017(10) . ? F5 Cr1 1.953(7) 3_575 ? F5 Ni1 1.953(7) 3_575 ? F6 Cr1 1.922(7) 3_575 ? F6 Ni1 1.922(7) 3_575 ? C1 N2 1.306(19) . ? C1 N5 1.34(2) . ? N2 C3 1.31(2) . ? C3 C4 1.41(2) . ? C4 N5 1.34(2) . ? N5 C6 1.51(2) . ? C6 C7 1.51(2) . ? C7 C8 1.47(2) . ? C8 C9 1.52(2) . ? O11 C11 1.250(18) . ? O12 C11 1.240(17) . ? C11 C12 1.56(2) . ? C12 C13 1.54(2) . ? C12 C14 1.55(2) . ? C12 C15 1.53(2) . ? O21 C21 1.275(19) . ? O22 C21 1.318(19) . ? C21 C22 1.51(2) . ? C22 C23 1.55(3) . ? C22 C24 1.49(2) . ? C22 C25 1.49(3) . ? C31 O31 1.259(19) . ? C31 O32 1.224(19) . ? C31 C32 1.56(2) . ? C32 C33 1.56(3) . ? C32 C34 1.51(2) . ? C32 C35 1.49(3) . ? O41 C41 1.293(18) . ? O42 C41 1.255(18) . ? C41 C42 1.51(2) . ? C42 C43 1.49(2) . ? C42 C44 1.56(2) . ? C42 C45 1.58(2) . ? O51 C51 1.223(17) . ? O52 C51 1.255(18) . ? C51 C52 1.54(2) . ? C52 C53 1.48(2) . ? C52 C54 1.53(2) . ? C52 C55 1.54(3) . ? O61 C61 1.27(2) . ? O62 C61 1.28(2) . ? C61 C62 1.50(2) . ? C62 C63 1.50(3) . ? C62 C64 1.52(3) . ? C62 C65 1.57(3) . ? O71 C71 1.251(18) . ? O72 C71 1.234(18) . ? C71 C72 1.56(2) . ? C72 C73 1.58(2) . ? C72 C74 1.53(3) . ? C72 C75 1.51(3) . ? O81 C81 1.251(18) . ? O82 C81 1.264(18) . ? C81 C82 1.54(2) . ? C82 C83 1.54(2) . ? C82 C84 1.46(2) . ? C82 C85 1.53(2) . ? O91 C91 1.261(17) . ? O92 Cr1 1.971(10) 3_575 ? O92 Ni1 1.971(10) 3_575 ? O92 C91 1.256(17) . ? C91 C92 1.52(2) . ? C92 C93 1.54(2) . ? C92 C94 1.52(3) . ? C92 C95 1.49(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Cr1 F5 92.6(3) . 3_575 ? F1 Cr1 F6 173.1(3) . 3_575 ? F1 Cr1 O11 90.4(3) . . ? F1 Cr1 O21 94.9(4) . . ? F1 Cr1 O92 87.3(4) . 3_575 ? F5 Cr1 F6 80.8(3) 3_575 3_575 ? F5 Cr1 O11 90.1(4) 3_575 . ? F5 Cr1 O21 171.9(4) 3_575 . ? F5 Cr1 O92 90.3(4) 3_575 3_575 ? F6 Cr1 O11 91.5(4) 3_575 . ? F6 Cr1 O21 91.6(4) 3_575 . ? F6 Cr1 O92 90.9(4) 3_575 3_575 ? O11 Cr1 O21 92.7(4) . . ? O11 Cr1 O92 177.7(4) . 3_575 ? O21 Cr1 O92 87.2(4) . 3_575 ? F1 Cr2 F2 91.0(3) . . ? F1 Cr2 O12 90.4(4) . . ? F1 Cr2 O22 94.1(4) . . ? F1 Cr2 O31 177.3(4) . . ? F1 Cr2 O41 89.5(4) . . ? F2 Cr2 O12 88.4(4) . . ? F2 Cr2 O22 174.7(4) . . ? F2 Cr2 O31 90.1(4) . . ? F2 Cr2 O41 91.3(4) . . ? O12 Cr2 O22 92.6(5) . . ? O12 Cr2 O31 87.2(4) . . ? O12 Cr2 O41 179.7(5) . . ? O22 Cr2 O31 84.8(5) . . ? O22 Cr2 O41 87.7(4) . . ? O31 Cr2 O41 93.0(4) . . ? F2 Cr3 F3 89.1(3) . . ? F2 Cr3 O32 93.8(4) . . ? F2 Cr3 O42 88.5(4) . . ? F2 Cr3 O51 176.8(4) . . ? F2 Cr3 O61 89.0(4) . . ? F3 Cr3 O32 177.1(4) . . ? F3 Cr3 O42 89.6(4) . . ? F3 Cr3 O51 90.5(4) . . ? F3 Cr3 O61 93.0(4) . . ? O32 Cr3 O42 90.9(5) . . ? O32 Cr3 O51 86.6(4) . . ? O32 Cr3 O61 86.7(5) . . ? O42 Cr3 O51 88.3(5) . . ? O42 Cr3 O61 176.5(4) . . ? O51 Cr3 O61 94.1(5) . . ? F3 Cr4 F4 87.2(3) . . ? F3 Cr4 O52 91.7(4) . . ? F3 Cr4 O62 91.0(4) . . ? F3 Cr4 O71 177.5(4) . . ? F3 Cr4 O81 90.9(4) . . ? F4 Cr4 O52 178.3(5) . . ? F4 Cr4 O62 89.1(4) . . ? F4 Cr4 O71 93.1(4) . . ? F4 Cr4 O81 91.5(4) . . ? O52 Cr4 O62 92.3(5) . . ? O52 Cr4 O71 88.0(4) . . ? O52 Cr4 O81 87.1(4) . . ? O62 Cr4 O71 86.5(5) . . ? O62 Cr4 O81 178.0(5) . . ? O71 Cr4 O81 91.5(5) . . ? F4 Cr5 F5 89.3(3) . . ? F4 Cr5 F6 165.2(3) . . ? F4 Cr5 O72 96.0(4) . . ? F4 Cr5 O82 92.4(4) . . ? F4 Cr5 O91 84.4(4) . . ? F5 Cr5 F6 77.5(3) . . ? F5 Cr5 O72 173.9(4) . . ? F5 Cr5 O82 93.0(4) . . ? F5 Cr5 O91 90.0(4) . . ? F6 Cr5 O72 96.8(4) . . ? F6 Cr5 O82 95.1(4) . . ? F6 Cr5 O91 88.7(4) . . ? O72 Cr5 O82 89.8(4) . . ? O72 Cr5 O91 87.5(4) . . ? O82 Cr5 O91 175.6(4) . . ? Cr1 F1 Cr2 122.0(4) . . ? Cr2 F2 Cr3 122.0(4) . . ? Cr3 F3 Cr4 123.8(4) . . ? Cr4 F4 Cr5 120.4(4) . . ? Cr1 F5 Ni1 0.00(12) 3_575 3_575 ? Cr1 F5 Cr5 97.8(3) 3_575 . ? Ni1 F5 Cr5 97.8(3) 3_575 . ? Cr1 F6 Ni1 0.00(16) 3_575 3_575 ? Cr1 F6 Cr5 98.7(3) 3_575 . ? Ni1 F6 Cr5 98.7(3) 3_575 . ? N2 C1 N5 106.7(13) . . ? C1 N2 C3 112.1(13) . . ? N2 C3 C4 105.7(14) . . ? C3 C4 N5 105.5(14) . . ? C1 N5 C4 109.9(12) . . ? C1 N5 C6 124.4(14) . . ? C4 N5 C6 125.7(14) . . ? N5 C6 C7 109.7(14) . . ? C6 C7 C8 116.0(16) . . ? C7 C8 C9 112.1(15) . . ? Cr1 O11 C11 135.4(9) . . ? Cr2 O12 C11 131.0(11) . . ? O11 C11 O12 126.6(15) . . ? O11 C11 C12 116.9(13) . . ? O12 C11 C12 116.5(14) . . ? C11 C12 C13 110.3(14) . . ? C11 C12 C14 107.6(14) . . ? C11 C12 C15 106.3(14) . . ? C13 C12 C14 110.7(14) . . ? C13 C12 C15 112.7(15) . . ? C14 C12 C15 108.9(15) . . ? Cr1 O21 C21 130.6(9) . . ? Cr2 O22 C21 136.4(10) . . ? O21 C21 O22 123.5(13) . . ? O21 C21 C22 122.6(15) . . ? O22 C21 C22 113.9(14) . . ? C21 C22 C23 108.6(14) . . ? C21 C22 C24 107.4(14) . . ? C21 C22 C25 107.9(15) . . ? C23 C22 C24 111.9(16) . . ? C23 C22 C25 110.7(15) . . ? C24 C22 C25 110.3(16) . . ? O31 C31 O32 124.7(14) . . ? O31 C31 C32 117.0(15) . . ? O32 C31 C32 118.2(15) . . ? Cr2 O31 C31 128.3(10) . . ? Cr3 O32 C31 134.8(10) . . ? C31 C32 C33 104.0(14) . . ? C31 C32 C34 107.2(14) . . ? C31 C32 C35 110.6(15) . . ? C33 C32 C34 110.7(16) . . ? C33 C32 C35 111.5(16) . . ? C34 C32 C35 112.4(17) . . ? Cr2 O41 C41 135.0(9) . . ? Cr3 O42 C41 129.3(10) . . ? O41 C41 O42 124.1(14) . . ? O41 C41 C42 115.5(13) . . ? O42 C41 C42 120.4(13) . . ? C41 C42 C43 111.4(14) . . ? C41 C42 C44 108.2(13) . . ? C41 C42 C45 106.5(13) . . ? C43 C42 C44 112.5(15) . . ? C43 C42 C45 111.6(14) . . ? C44 C42 C45 106.2(14) . . ? Cr3 O51 C51 133.2(10) . . ? Cr4 O52 C51 132.9(9) . . ? O51 C51 O52 127.3(13) . . ? O51 C51 C52 116.1(13) . . ? O52 C51 C52 116.5(13) . . ? C51 C52 C53 111.7(14) . . ? C51 C52 C54 109.2(14) . . ? C51 C52 C55 105.5(13) . . ? C53 C52 C54 110.9(15) . . ? C53 C52 C55 108.6(16) . . ? C54 C52 C55 110.8(15) . . ? Cr3 O61 C61 135.6(11) . . ? Cr4 O62 C61 133.7(11) . . ? O61 C61 O62 124.1(16) . . ? O61 C61 C62 119.6(16) . . ? O62 C61 C62 116.3(16) . . ? C61 C62 C63 112.1(17) . . ? C61 C62 C64 111.4(18) . . ? C61 C62 C65 106.9(16) . . ? C63 C62 C64 116.5(19) . . ? C63 C62 C65 108.0(18) . . ? C64 C62 C65 101(2) . . ? Cr4 O71 C71 133.3(10) . . ? Cr5 O72 C71 130.2(9) . . ? O71 C71 O72 128.2(14) . . ? O71 C71 C72 112.9(14) . . ? O72 C71 C72 118.9(13) . . ? C71 C72 C73 108.0(14) . . ? C71 C72 C74 108.0(14) . . ? C71 C72 C75 108.9(15) . . ? C73 C72 C74 109.8(16) . . ? C73 C72 C75 111.9(16) . . ? C74 C72 C75 110.1(17) . . ? Cr4 O81 C81 139.0(10) . . ? Cr5 O82 C81 126.9(10) . . ? O81 C81 O82 125.2(14) . . ? O81 C81 C82 117.1(13) . . ? O82 C81 C82 117.4(13) . . ? C81 C82 C83 108.4(13) . . ? C81 C82 C84 112.5(13) . . ? C81 C82 C85 103.7(14) . . ? C83 C82 C84 109.7(15) . . ? C83 C82 C85 109.7(14) . . ? C84 C82 C85 112.6(14) . . ? Cr5 O91 C91 128.6(10) . . ? Cr1 O92 Ni1 0.00(16) 3_575 3_575 ? Cr1 O92 C91 129.6(9) 3_575 . ? Ni1 O92 C91 129.6(9) 3_575 . ? O91 C91 O92 123.3(14) . . ? O91 C91 C92 118.2(14) . . ? O92 C91 C92 118.5(13) . . ? C91 C92 C93 110.4(14) . . ? C91 C92 C94 109.8(14) . . ? C91 C92 C95 107.7(15) . . ? C93 C92 C94 110.4(16) . . ? C93 C92 C95 108.9(16) . . ? C94 C92 C95 109.7(16) . . ? 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 N2 H2 F4 0.88 1.95 2.739(13) 148.0 . _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 21.16 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.506 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.158 data_GT14CT-03 _database_code_depnum_ccdc_archive 'CCDC 268360' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H162 Cr8 F12 Ni2 O36 2-,2(C13 H26 N 1+)' _chemical_formula_sum 'C116 H214 Cr8 F12 N2 Ni2 O36' _chemical_formula_weight 2974.31 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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 I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 26.003(3) _cell_length_b 19.882(2) _cell_length_c 31.266(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.99(1) _cell_angle_gamma 90.00 _cell_volume 15751(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5190 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 23.9 _exptl_crystal_description block _exptl_crystal_colour green-blue _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6272 _exptl_absorpt_coefficient_mu 0.840 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 3 sets of \w scans; each set at different \f angles and each scan (30 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.83 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 6000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number 0 _diffrn_reflns_number 72976 _diffrn_reflns_av_R_equivalents 0.0906 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13879 _reflns_number_gt 7993 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SMART version 5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXTL version 6.12 (Bruker, 2001)' _computing_structure_refinement 'SHELXTL version 6.12 (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL version 6.12 (Bruker, 2001)' _computing_publication_material 'SHELXTL version 6.12 (Bruker, 2001)' _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. The Cr and Ni atoms are sharing the sites Cr/Ni(4) and Cr/Ni(5) in the ratios of 0.6:0.4 and 0.4:0.6, respectively. 7 out of 9 independent t-Bu groups are disordered, by rotation around the O~2~C---CMe~3~ bond and simulatneous tilting of this bond. Thus, atoms C(2) to C(5) are disordered between positions A and B with the occupancies 0.55:0.45, C(7) to C(10) with the occupancies 0.5:0.5, C(17) to C(20) with 0.6:0.4, C(22) to C(27) with 0.67:0.33, C(32) to C(35) with 0.6:0.4, C(42) to C(45) with 0.33:0.67, respectively. The C(27) atom is disordered between two positions (A and B, 0.5:0.5), while C(28) to C(30) between three (A, B and C, 0.25:0.25:0.5). The intraannular [MeNH(cy-C~6~H~11~)~2~]^+^ cation is located at an inversion centre and disordered between two positions related via this centre (occupancies 0.5:0.5). Besides, its atom C(48) is disordered between positions A and B (occupancies 0.33:0.17). Between the molecules there are continuous channels, parallel to the [1 0 0] direction. The volume of the channels exceeds 2100 \%A^3^ or 13% of the total unit cell volume, and their width is sufficient for free motion of the second [MeNH(cy-C~6~H~11~)~2~]^+^ cation, whose position therefore could not be determined, difference Fourier maps revealing a continuous "stream" of diffuse electron density along the channel. Standard least squares refinement without any account of this cation gave R~1~=0.080 for observed data, R~2~=0.280 for all data. The present refinement used the SQUEEZE routine of the PLATON software package (A.L.Spek, Utrecht University, 1980-2002) to account for unassigned electron density (P. van der Sluis & A.L. Spek, Acta Cryst., 1990 A46, 194-201). ; _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^)+(0.1237P)^2^] 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 13879 _refine_ls_number_parameters 708 _refine_ls_number_restraints 284 _refine_ls_R_factor_all 0.1036 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.2081 _refine_ls_wR_factor_gt 0.1909 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.10226(4) 0.34029(4) 0.13144(3) 0.0629(3) Uani 1 1 d . . . Cr2 Cr 0.10934(3) 0.49262(4) 0.18035(2) 0.0448(2) Uani 1 1 d . . . Cr3 Cr 0.09139(3) 0.65445(4) 0.14758(2) 0.0482(2) Uani 1 1 d . . . Cr4 Cr 0.02267(3) 0.72786(4) 0.05561(2) 0.0484(2) Uani 0.60 1 d P . . Cr5 Cr -0.03833(3) 0.72769(3) -0.03763(2) 0.0543(2) Uani 0.40 1 d P . . Ni4 Ni 0.02267(3) 0.72786(4) 0.05561(2) 0.0484(2) Uani 0.40 1 d P . . Ni5 Ni -0.03833(3) 0.72769(3) -0.03763(2) 0.0543(2) Uani 0.60 1 d P . . F1 F 0.07528(10) 0.42987(13) 0.13716(8) 0.0507(7) Uani 1 1 d . . . F2 F 0.10387(9) 0.56107(13) 0.13646(7) 0.0442(6) Uani 1 1 d . . . F3 F 0.03384(10) 0.65482(13) 0.09779(8) 0.0486(6) Uani 1 1 d . . . F4 F -0.00127(11) 0.66391(14) 0.00767(9) 0.0583(8) Uani 1 1 d . . . F5 F 0.00638(13) 0.79100(16) 0.00555(11) 0.0727(9) Uani 1 1 d . . . F6 F -0.07846(12) 0.65354(14) -0.07004(9) 0.0614(8) Uani 1 1 d . . . O1 O 0.12796(17) 0.3298(2) 0.19524(13) 0.0786(13) Uani 1 1 d . A . O2 O 0.11453(15) 0.4260(2) 0.22657(11) 0.0637(10) Uani 1 1 d . A . O3 O 0.17141(15) 0.3789(2) 0.12783(13) 0.0726(11) Uani 1 1 d . B . O4 O 0.17880(13) 0.46865(19) 0.17126(12) 0.0575(9) Uani 1 1 d . B . O5 O 0.14531(14) 0.55254(19) 0.22718(10) 0.0594(9) Uani 1 1 d . . . O6 O 0.15037(14) 0.6539(2) 0.19944(12) 0.0655(10) Uani 1 1 d . . . O7 O 0.04055(14) 0.51784(18) 0.19026(12) 0.0576(9) Uani 1 1 d . C . O8 O 0.04201(14) 0.62934(18) 0.18432(11) 0.0558(9) Uani 1 1 d . C . O9 O 0.07992(16) 0.74737(18) 0.16174(11) 0.0643(10) Uani 1 1 d . D . O10 O 0.04357(16) 0.80141(18) 0.09978(12) 0.0686(11) Uani 1 1 d . D . O11 O 0.14157(13) 0.68045(19) 0.11299(11) 0.0583(9) Uani 1 1 d . E . O12 O 0.09640(15) 0.7217(2) 0.04886(12) 0.0721(11) Uani 1 1 d . E . O13 O -0.04983(13) 0.73865(18) 0.06376(11) 0.0581(9) Uani 1 1 d . I . O14 O -0.09544(14) 0.73956(17) -0.00590(11) 0.0591(9) Uani 1 1 d . I . O15 O -0.07276(17) 0.80374(18) -0.07672(13) 0.0733(11) Uani 1 1 d . . . O16 O -0.13294(19) 0.7486(2) -0.12681(14) 0.0873(14) Uani 1 1 d . . . O17 O 0.01706(15) 0.7179(2) -0.07187(11) 0.0684(11) Uani 1 1 d . J . O18 O -0.03434(17) 0.6951(2) -0.13785(11) 0.0741(12) Uani 1 1 d . . . C1 C 0.1265(2) 0.3658(3) 0.22840(18) 0.0638(15) Uani 1 1 d D . . C2A C 0.1313(4) 0.3352(4) 0.2744(3) 0.053(3) Uiso 0.55 1 d PD A 1 C3A C 0.1599(5) 0.2679(6) 0.2757(5) 0.103(4) Uiso 0.55 1 d PD A 1 H31 H 0.1391 0.2394 0.2527 0.154 Uiso 0.55 1 d PR A 1 H32 H 0.1624 0.2465 0.3044 0.154 Uiso 0.55 1 d PR A 1 H33 H 0.1954 0.2739 0.2705 0.154 Uiso 0.55 1 d PR A 1 C4A C 0.0787(4) 0.3241(6) 0.2838(4) 0.091(4) Uiso 0.55 1 d PD A 1 H41 H 0.0596 0.2930 0.2616 0.137 Uiso 0.55 1 d PR A 1 H42 H 0.0594 0.3667 0.2821 0.137 Uiso 0.55 1 d PR A 1 H43 H 0.0819 0.3044 0.3130 0.137 Uiso 0.55 1 d PR A 1 C5A C 0.1654(6) 0.3819(8) 0.3071(6) 0.123(9) Uiso 0.55 1 d PD A 1 H51 H 0.1999 0.3862 0.2997 0.184 Uiso 0.55 1 d PR A 1 H52 H 0.1700 0.3627 0.3366 0.184 Uiso 0.55 1 d PR A 1 H53 H 0.1489 0.4263 0.3063 0.184 Uiso 0.55 1 d PR A 1 C2B C 0.1531(5) 0.3311(5) 0.2706(4) 0.063(4) Uiso 0.45 1 d PD A 2 C3B C 0.1195(6) 0.2711(7) 0.2737(6) 0.099(5) Uiso 0.45 1 d PD A 2 H34 H 0.1199 0.2428 0.2482 0.149 Uiso 0.45 1 d PR A 2 H35 H 0.0830 0.2829 0.2741 0.149 Uiso 0.45 1 d PR A 2 H36 H 0.1355 0.2466 0.3006 0.149 Uiso 0.45 1 d PR A 2 C4B C 0.2087(5) 0.3105(8) 0.2722(5) 0.093(5) Uiso 0.45 1 d PD A 2 H44 H 0.2293 0.3509 0.2695 0.140 Uiso 0.45 1 d PR A 2 H45 H 0.2088 0.2804 0.2474 0.140 Uiso 0.45 1 d PR A 2 H46 H 0.2246 0.2873 0.2997 0.140 Uiso 0.45 1 d PR A 2 C5B C 0.1508(7) 0.3802(7) 0.3082(5) 0.074(5) Uiso 0.45 1 d PD A 2 H54 H 0.1675 0.3609 0.3368 0.111 Uiso 0.45 1 d PR A 2 H55 H 0.1136 0.3896 0.3073 0.111 Uiso 0.45 1 d PR A 2 H56 H 0.1688 0.4221 0.3037 0.111 Uiso 0.45 1 d PR A 2 C6 C 0.1958(2) 0.4266(3) 0.14858(18) 0.0606(14) Uani 1 1 d D . . C7A C 0.2572(4) 0.4359(6) 0.1541(5) 0.083(5) Uiso 0.50 1 d PD B 1 C8A C 0.2857(6) 0.4182(7) 0.2007(4) 0.100(5) Uiso 0.50 1 d PD B 1 H81 H 0.2775 0.3712 0.2059 0.150 Uiso 0.50 1 d PR B 1 H82 H 0.2745 0.4470 0.2224 0.150 Uiso 0.50 1 d PR B 1 H83 H 0.3238 0.4231 0.2034 0.150 Uiso 0.50 1 d PR B 1 C9A C 0.2760(6) 0.3883(7) 0.1223(5) 0.109(5) Uiso 0.50 1 d PD B 1 H91 H 0.2675 0.3416 0.1281 0.164 Uiso 0.50 1 d PR B 1 H92 H 0.3140 0.3925 0.1246 0.164 Uiso 0.50 1 d PR B 1 H93 H 0.2570 0.4010 0.0926 0.164 Uiso 0.50 1 d PR B 1 C10A C 0.2703(6) 0.5081(5) 0.1434(5) 0.096(5) Uiso 0.50 1 d PD B 1 H101 H 0.2593 0.5372 0.1650 0.144 Uiso 0.50 1 d PR B 1 H102 H 0.2519 0.5216 0.1137 0.144 Uiso 0.50 1 d PR B 1 H103 H 0.3085 0.5122 0.1463 0.144 Uiso 0.50 1 d PR B 1 C7B C 0.2512(5) 0.4339(6) 0.1395(5) 0.095(6) Uiso 0.50 1 d PD B 2 C8B C 0.2515(7) 0.4379(9) 0.0922(4) 0.135(7) Uiso 0.50 1 d PD B 2 H84 H 0.2343 0.3989 0.0759 0.203 Uiso 0.50 1 d PR B 2 H85 H 0.2880 0.4410 0.0887 0.203 Uiso 0.50 1 d PR B 2 H86 H 0.2324 0.4789 0.0808 0.203 Uiso 0.50 1 d PR B 2 C9B C 0.2773(7) 0.3689(7) 0.1598(6) 0.127(6) Uiso 0.50 1 d PD B 2 H94 H 0.2775 0.3639 0.1910 0.190 Uiso 0.50 1 d PR B 2 H95 H 0.3137 0.3689 0.1559 0.190 Uiso 0.50 1 d PR B 2 H96 H 0.2579 0.3314 0.1433 0.190 Uiso 0.50 1 d PR B 2 C10B C 0.2783(6) 0.4931(6) 0.1659(5) 0.089(4) Uiso 0.50 1 d PD B 2 H104 H 0.2768 0.4854 0.1966 0.134 Uiso 0.50 1 d PR B 2 H105 H 0.2602 0.5353 0.1556 0.134 Uiso 0.50 1 d PR B 2 H106 H 0.3152 0.4960 0.1637 0.134 Uiso 0.50 1 d PR B 2 C11 C 0.16301(19) 0.6108(3) 0.22829(16) 0.0530(13) Uani 1 1 d . . . C12 C 0.2037(3) 0.6316(3) 0.26942(19) 0.0773(18) Uani 1 1 d . . . C13 C 0.2528(3) 0.6549(4) 0.2559(3) 0.114(3) Uani 1 1 d . . . H131 H 0.2805 0.6682 0.2812 0.171 Uiso 1 1 d R . . H132 H 0.2436 0.6933 0.2360 0.171 Uiso 1 1 d R . . H133 H 0.2654 0.6178 0.2404 0.171 Uiso 1 1 d R . . C14 C 0.2188(4) 0.5718(5) 0.3000(2) 0.164(5) Uani 1 1 d . . . H141 H 0.2450 0.5853 0.3263 0.246 Uiso 1 1 d R . . H142 H 0.2337 0.5365 0.2845 0.246 Uiso 1 1 d R . . H143 H 0.1872 0.5547 0.3084 0.246 Uiso 1 1 d R . . C15 C 0.1814(3) 0.6886(5) 0.2899(2) 0.124(3) Uani 1 1 d . . . H151 H 0.2064 0.7028 0.3167 0.186 Uiso 1 1 d R . . H152 H 0.1483 0.6744 0.2972 0.186 Uiso 1 1 d R . . H153 H 0.1744 0.7263 0.2692 0.186 Uiso 1 1 d R . . C16 C 0.02381(19) 0.5758(3) 0.19530(15) 0.0517(12) Uani 1 1 d D . . C17A C -0.0258(4) 0.5864(5) 0.2131(4) 0.075(4) Uiso 0.60 1 d PD C 1 C18A C -0.0088(6) 0.6343(6) 0.2519(4) 0.122(5) Uiso 0.60 1 d PD C 1 H181 H 0.0198 0.6135 0.2737 0.183 Uiso 0.60 1 d PR C 1 H182 H -0.0384 0.6444 0.2654 0.183 Uiso 0.60 1 d PR C 1 H183 H 0.0039 0.6760 0.2411 0.183 Uiso 0.60 1 d PR C 1 C19A C -0.0427(5) 0.5214(6) 0.2318(4) 0.105(4) Uiso 0.60 1 d PD C 1 H191 H -0.0134 0.5025 0.2538 0.157 Uiso 0.60 1 d PR C 1 H192 H -0.0540 0.4890 0.2080 0.157 Uiso 0.60 1 d PR C 1 H193 H -0.0723 0.5311 0.2456 0.157 Uiso 0.60 1 d PR C 1 C20A C -0.0692(5) 0.6192(6) 0.1801(4) 0.111(4) Uiso 0.60 1 d PD C 1 H201 H -0.1003 0.6254 0.1925 0.166 Uiso 0.60 1 d PR C 1 H202 H -0.0782 0.5893 0.1545 0.166 Uiso 0.60 1 d PR C 1 H203 H -0.0577 0.6628 0.1711 0.166 Uiso 0.60 1 d PR C 1 C17B C -0.0178(5) 0.5751(7) 0.2238(5) 0.073(6) Uiso 0.40 1 d PD C 2 C18B C -0.0461(7) 0.6416(7) 0.2184(6) 0.100(6) Uiso 0.40 1 d PD C 2 H184 H -0.0622 0.6508 0.1875 0.150 Uiso 0.40 1 d PR C 2 H185 H -0.0206 0.6771 0.2300 0.150 Uiso 0.40 1 d PR C 2 H186 H -0.0737 0.6405 0.2352 0.150 Uiso 0.40 1 d PR C 2 C19B C -0.0590(6) 0.5190(7) 0.2066(6) 0.085(5) Uiso 0.40 1 d PD C 2 H194 H -0.0756 0.5284 0.1758 0.127 Uiso 0.40 1 d PR C 2 H195 H -0.0859 0.5190 0.2240 0.127 Uiso 0.40 1 d PR C 2 H196 H -0.0417 0.4749 0.2087 0.127 Uiso 0.40 1 d PR C 2 C20B C 0.0068(8) 0.5605(10) 0.2706(5) 0.130(8) Uiso 0.40 1 d PD C 2 H204 H 0.0246 0.5168 0.2725 0.195 Uiso 0.40 1 d PR C 2 H205 H -0.0201 0.5594 0.2881 0.195 Uiso 0.40 1 d PR C 2 H206 H 0.0328 0.5955 0.2821 0.195 Uiso 0.40 1 d PR C 2 C21 C 0.0614(2) 0.7990(3) 0.14014(17) 0.0534(13) Uani 1 1 d D . . C22A C 0.0689(4) 0.8666(4) 0.1643(3) 0.070(3) Uiso 0.67 1 d PD D 1 C23A C 0.1151(4) 0.9020(6) 0.1529(4) 0.118(4) Uiso 0.67 1 d PD D 1 H231 H 0.1216 0.9454 0.1680 0.177 Uiso 0.67 1 d PR D 1 H232 H 0.1104 0.9090 0.1212 0.177 Uiso 0.67 1 d PR D 1 H233 H 0.1453 0.8721 0.1634 0.177 Uiso 0.67 1 d PR D 1 C24A C 0.0160(5) 0.9035(7) 0.1484(4) 0.130(5) Uiso 0.67 1 d PD D 1 H241 H -0.0152 0.8823 0.1552 0.195 Uiso 0.67 1 d PR D 1 H242 H 0.0108 0.9085 0.1165 0.195 Uiso 0.67 1 d PR D 1 H243 H 0.0213 0.9480 0.1623 0.195 Uiso 0.67 1 d PR D 1 C25A C 0.0776(4) 0.8510(6) 0.2144(3) 0.084(3) Uiso 0.67 1 d PD D 1 H251 H 0.0446 0.8317 0.2190 0.126 Uiso 0.67 1 d PR D 1 H252 H 0.0856 0.8926 0.2315 0.126 Uiso 0.67 1 d PR D 1 H253 H 0.1064 0.8188 0.2239 0.126 Uiso 0.67 1 d PR D 1 C22B C 0.0512(6) 0.8579(7) 0.1702(4) 0.052(4) Uiso 0.33 1 d PD D 2 C23B C 0.0027(8) 0.8458(14) 0.1908(9) 0.155(12) Uiso 0.33 1 d PD D 2 H234 H -0.0020 0.8848 0.2088 0.233 Uiso 0.33 1 d PR D 2 H235 H -0.0044 0.8045 0.2057 0.233 Uiso 0.33 1 d PR D 2 H236 H -0.0219 0.8490 0.1622 0.233 Uiso 0.33 1 d PR D 2 C24B C 0.0412(9) 0.9225(10) 0.1423(6) 0.101(7) Uiso 0.33 1 d PD D 2 H244 H 0.0779 0.9214 0.1393 0.152 Uiso 0.33 1 d PR D 2 H245 H 0.0367 0.9594 0.1619 0.152 Uiso 0.33 1 d PR D 2 H246 H 0.0176 0.9295 0.1134 0.152 Uiso 0.33 1 d PR D 2 C25B C 0.0996(7) 0.8678(11) 0.2092(6) 0.093(7) Uiso 0.33 1 d PD D 2 H254 H 0.1357 0.8636 0.2050 0.140 Uiso 0.33 1 d PR D 2 H255 H 0.0904 0.8275 0.2238 0.140 Uiso 0.33 1 d PR D 2 H256 H 0.0971 0.9074 0.2272 0.140 Uiso 0.33 1 d PR D 2 C26 C 0.1383(2) 0.7061(3) 0.07590(19) 0.0698(16) Uani 1 1 d D . . C27A C 0.1901(4) 0.7006(6) 0.0605(3) 0.065(3) Uiso 0.50 1 d PD E 1 C28A C 0.1856(14) 0.6695(16) 0.0179(7) 0.126(8) Uiso 0.25 1 d PD E 1 H281 H 0.1780 0.6228 0.0244 0.189 Uiso 0.25 1 d PR E 1 H282 H 0.2194 0.6715 0.0090 0.189 Uiso 0.25 1 d PR E 1 H283 H 0.1575 0.6863 -0.0061 0.189 Uiso 0.25 1 d PR E 1 C29A C 0.2329(12) 0.6626(16) 0.0916(9) 0.126(8) Uiso 0.25 1 d PD E 1 H291 H 0.2352 0.6909 0.1177 0.189 Uiso 0.25 1 d PR E 1 H292 H 0.2666 0.6639 0.0826 0.189 Uiso 0.25 1 d PR E 1 H293 H 0.2250 0.6162 0.0985 0.189 Uiso 0.25 1 d PR E 1 C30A C 0.2103(14) 0.7698(10) 0.0607(12) 0.126(8) Uiso 0.25 1 d PD E 1 H301 H 0.2116 0.7955 0.0876 0.189 Uiso 0.25 1 d PR E 1 H302 H 0.1824 0.7878 0.0371 0.189 Uiso 0.25 1 d PR E 1 H303 H 0.2443 0.7735 0.0523 0.189 Uiso 0.25 1 d PR E 1 C27B C 0.1893(5) 0.7437(7) 0.0688(4) 0.091(4) Uiso 0.50 1 d PD E 2 C28B C 0.1854(6) 0.7590(7) 0.0211(4) 0.091(4) Uiso 0.50 1 d PD E 2 H284 H 0.1531 0.7845 0.0093 0.136 Uiso 0.50 1 d PR E 2 H285 H 0.1845 0.7166 0.0050 0.136 Uiso 0.50 1 d PR E 2 H286 H 0.2161 0.7854 0.0180 0.136 Uiso 0.50 1 d PR E 2 C29B C 0.2378(5) 0.7053(8) 0.0890(4) 0.087(4) Uiso 0.50 1 d PD E 2 H294 H 0.2394 0.6971 0.1202 0.131 Uiso 0.50 1 d PR E 2 H295 H 0.2686 0.7316 0.0859 0.131 Uiso 0.50 1 d PR E 2 H296 H 0.2377 0.6621 0.0738 0.131 Uiso 0.50 1 d PR E 2 C30B C 0.1993(7) 0.8139(8) 0.0911(5) 0.136(6) Uiso 0.50 1 d PD E 2 H304 H 0.1679 0.8407 0.0788 0.203 Uiso 0.50 1 d PR E 2 H305 H 0.2307 0.8372 0.0864 0.203 Uiso 0.50 1 d PR E 2 H306 H 0.2022 0.8077 0.1227 0.203 Uiso 0.50 1 d PR E 2 C28C C 0.1860(13) 0.7162(15) 0.0143(6) 0.103(10) Uiso 0.25 1 d PD F 3 H287 H 0.1661 0.7566 0.0060 0.154 Uiso 0.25 1 d PR F 3 H288 H 0.2200 0.7205 0.0073 0.154 Uiso 0.25 1 d PR F 3 H289 H 0.1675 0.6787 -0.0013 0.154 Uiso 0.25 1 d PR F 3 C29C C 0.2162(15) 0.6331(12) 0.0675(11) 0.165(18) Uiso 0.25 1 d PD G 3 H297 H 0.2480 0.6355 0.0568 0.247 Uiso 0.25 1 d PR G 3 H298 H 0.2250 0.6279 0.0988 0.247 Uiso 0.25 1 d PR G 3 H299 H 0.1955 0.5952 0.0544 0.247 Uiso 0.25 1 d PR G 3 C30C C 0.2262(10) 0.7472(13) 0.0890(8) 0.081(7) Uiso 0.25 1 d PD H 3 H307 H 0.2066 0.7881 0.0816 0.121 Uiso 0.25 1 d PR H 3 H308 H 0.2308 0.7385 0.1198 0.121 Uiso 0.25 1 d PR H 3 H309 H 0.2601 0.7517 0.0819 0.121 Uiso 0.25 1 d PR H 3 C31 C -0.0918(2) 0.7448(3) 0.03443(18) 0.0590(14) Uani 1 1 d D . . C32A C -0.1442(4) 0.7533(5) 0.0473(3) 0.071(3) Uiso 0.60 1 d PD I 1 C33A C -0.1709(5) 0.8184(6) 0.0240(4) 0.110(4) Uiso 0.60 1 d PD I 1 H331 H -0.2047 0.8255 0.0322 0.165 Uiso 0.60 1 d PR I 1 H332 H -0.1769 0.8148 -0.0080 0.165 Uiso 0.60 1 d PR I 1 H333 H -0.1473 0.8564 0.0342 0.165 Uiso 0.60 1 d PR I 1 C34A C -0.1812(4) 0.6951(5) 0.0308(4) 0.086(3) Uiso 0.60 1 d PD I 1 H341 H -0.2145 0.7031 0.0397 0.129 Uiso 0.60 1 d PR I 1 H342 H -0.1659 0.6525 0.0433 0.129 Uiso 0.60 1 d PR I 1 H343 H -0.1878 0.6931 -0.0013 0.129 Uiso 0.60 1 d PR I 1 C35A C -0.1378(6) 0.7633(7) 0.0966(4) 0.106(5) Uiso 0.60 1 d PD I 1 H351 H -0.1724 0.7699 0.1036 0.158 Uiso 0.60 1 d PR I 1 H352 H -0.1155 0.8026 0.1064 0.158 Uiso 0.60 1 d PR I 1 H353 H -0.1211 0.7230 0.1116 0.158 Uiso 0.60 1 d PR I 1 C32B C -0.1372(6) 0.7734(9) 0.0534(5) 0.093(7) Uiso 0.40 1 d PD I 2 C33B C -0.1897(10) 0.7631(14) 0.0209(7) 0.191(13) Uiso 0.40 1 d PD I 2 H334 H -0.1966 0.7173 0.0093 0.286 Uiso 0.40 1 d PR I 2 H335 H -0.1892 0.7942 -0.0032 0.286 Uiso 0.40 1 d PR I 2 H336 H -0.2176 0.7764 0.0357 0.286 Uiso 0.40 1 d PR I 2 C34B C -0.1282(9) 0.8471(8) 0.0662(7) 0.137(8) Uiso 0.40 1 d PD I 2 H344 H -0.1595 0.8617 0.0763 0.205 Uiso 0.40 1 d PR I 2 H345 H -0.1225 0.8773 0.0429 0.205 Uiso 0.40 1 d PR I 2 H346 H -0.0973 0.8482 0.0908 0.205 Uiso 0.40 1 d PR I 2 C35B C -0.1376(8) 0.7323(9) 0.0963(5) 0.089(6) Uiso 0.40 1 d PD I 2 H354 H -0.1447 0.6859 0.0861 0.134 Uiso 0.40 1 d PR I 2 H355 H -0.1662 0.7482 0.1094 0.134 Uiso 0.40 1 d PR I 2 H356 H -0.1041 0.7341 0.1182 0.134 Uiso 0.40 1 d PR I 2 C36 C -0.1127(3) 0.8009(3) -0.1073(2) 0.0806(19) Uani 1 1 d . . . C37 C -0.1428(4) 0.8660(4) -0.1213(3) 0.120(3) Uani 1 1 d . . . C38 C -0.1213(4) 0.9243(4) -0.0909(3) 0.150(4) Uani 1 1 d . . . H381 H -0.1214 0.9119 -0.0605 0.225 Uiso 1 1 d R . . H382 H -0.1440 0.9636 -0.0994 0.225 Uiso 1 1 d R . . H383 H -0.0852 0.9351 -0.0931 0.225 Uiso 1 1 d R . . C39 C -0.2002(4) 0.8551(5) -0.1133(4) 0.157(4) Uani 1 1 d . . . H391 H -0.1980 0.8494 -0.0818 0.235 Uiso 1 1 d R . . H392 H -0.2164 0.8151 -0.1290 0.235 Uiso 1 1 d R . . H393 H -0.2217 0.8947 -0.1239 0.235 Uiso 1 1 d R . . C40 C -0.1462(6) 0.8766(5) -0.1680(3) 0.217(7) Uani 1 1 d . . . H401 H -0.1613 0.8361 -0.1839 0.326 Uiso 1 1 d R . . H402 H -0.1111 0.8850 -0.1735 0.326 Uiso 1 1 d R . . H403 H -0.1692 0.9151 -0.1782 0.326 Uiso 1 1 d R . . C41 C 0.0097(3) 0.7080(3) -0.11242(19) 0.0723(17) Uani 1 1 d D . . C42A C 0.0625(7) 0.7126(11) -0.1282(6) 0.22(3) Uiso 0.33 1 d PD J 1 C43A C 0.1009(9) 0.6551(11) -0.1068(7) 0.113(8) Uiso 0.33 1 d PD J 1 H431 H 0.1077 0.6580 -0.0747 0.169 Uiso 0.33 1 d PR J 1 H432 H 0.1342 0.6594 -0.1162 0.169 Uiso 0.33 1 d PR J 1 H433 H 0.0846 0.6116 -0.1164 0.169 Uiso 0.33 1 d PR J 1 C44A C 0.0924(11) 0.7781(10) -0.1143(7) 0.133(10) Uiso 0.33 1 d PD J 1 H441 H 0.0980 0.7833 -0.0824 0.200 Uiso 0.33 1 d PR J 1 H442 H 0.0717 0.8162 -0.1289 0.200 Uiso 0.33 1 d PR J 1 H443 H 0.1266 0.7769 -0.1225 0.200 Uiso 0.33 1 d PR J 1 C45A C 0.0517(6) 0.7050(8) -0.1781(4) 0.057(4) Uiso 0.33 1 d PD J 1 H451 H 0.0853 0.7100 -0.1871 0.085 Uiso 0.33 1 d PR J 1 H452 H 0.0271 0.7399 -0.1922 0.085 Uiso 0.33 1 d PR J 1 H453 H 0.0368 0.6605 -0.1869 0.085 Uiso 0.33 1 d PR J 1 C42B C 0.0568(4) 0.7025(5) -0.1343(3) 0.081(4) Uiso 0.67 1 d PD J 2 C43B C 0.1088(4) 0.7200(6) -0.1031(4) 0.108(4) Uiso 0.67 1 d PD J 2 H434 H 0.1167 0.6881 -0.0787 0.163 Uiso 0.67 1 d PR J 2 H435 H 0.1061 0.7655 -0.0917 0.163 Uiso 0.67 1 d PR J 2 H436 H 0.1371 0.7188 -0.1192 0.163 Uiso 0.67 1 d PR J 2 C44B C 0.0439(6) 0.7512(7) -0.1717(5) 0.164(7) Uiso 0.67 1 d PD J 2 H444 H 0.0106 0.7382 -0.1916 0.246 Uiso 0.67 1 d PR J 2 H445 H 0.0723 0.7507 -0.1877 0.246 Uiso 0.67 1 d PR J 2 H446 H 0.0405 0.7965 -0.1604 0.246 Uiso 0.67 1 d PR J 2 C45B C 0.0591(7) 0.6304(7) -0.1521(6) 0.190(7) Uiso 0.67 1 d PD J 2 H454 H 0.0673 0.5981 -0.1279 0.285 Uiso 0.67 1 d PR J 2 H455 H 0.0866 0.6286 -0.1690 0.285 Uiso 0.67 1 d PR J 2 H456 H 0.0249 0.6192 -0.1713 0.285 Uiso 0.67 1 d PR J 2 N1 N -0.0236(4) 0.5214(5) 0.0195(3) 0.063(3) Uiso 0.50 1 d PD K -1 H1 H -0.0158 0.5671 0.0203 0.082 Uiso 0.50 1 calc PR K -1 C46 C 0.0188(3) 0.4894(6) 0.0011(3) 0.054(3) Uiso 0.50 1 d PD K -1 H460 H 0.0166 0.4397 0.0052 0.065 Uiso 0.50 1 d PR K -1 C47 C 0.0070(6) 0.5083(11) -0.0498(4) 0.127(4) Uiso 0.50 1 d PD K -1 H471 H -0.0278 0.4887 -0.0637 0.164 Uiso 0.50 1 d PR K -1 H472 H 0.0043 0.5577 -0.0537 0.164 Uiso 0.50 1 d PR K -1 C48A C 0.0483(5) 0.4762(10) -0.0729(4) 0.068(5) Uiso 0.33 1 d PD K -1 H481 H 0.0443 0.4268 -0.0760 0.089 Uiso 0.33 1 d PR K -1 H482 H 0.0418 0.4958 -0.1027 0.089 Uiso 0.33 1 d PR K -1 C48B C 0.0448(12) 0.5498(16) -0.0491(11) 0.060(8) Uiso 0.17 1 d P K -1 H483 H 0.0504 0.5787 -0.0238 0.079 Uiso 0.17 1 d PR K -1 H484 H 0.0367 0.5767 -0.0752 0.079 Uiso 0.17 1 d PR K -1 C49 C 0.1055(5) 0.4918(7) -0.0490(4) 0.092(4) Uiso 0.50 1 d PD K -1 H491 H 0.1129 0.5397 -0.0539 0.120 Uiso 0.50 1 d PR K -1 H492 H 0.1300 0.4643 -0.0619 0.120 Uiso 0.50 1 d PR K -1 C50 C 0.1164(5) 0.4791(9) 0.0017(4) 0.121(6) Uiso 0.50 1 d PD K -1 H501 H 0.1519 0.4967 0.0154 0.158 Uiso 0.50 1 d PR K -1 H502 H 0.1168 0.4300 0.0067 0.158 Uiso 0.50 1 d PR K -1 C51 C 0.0746(4) 0.5147(7) 0.0251(3) 0.073(3) Uiso 0.50 1 d PD K -1 H511 H 0.0817 0.5016 0.0564 0.095 Uiso 0.50 1 d PR K -1 H512 H 0.0764 0.5643 0.0233 0.095 Uiso 0.50 1 d PR K -1 C52 C -0.0744(5) 0.5178(6) -0.0029(5) 0.088(4) Uiso 0.50 1 d PD K -1 H520 H -0.0761 0.5380 -0.0325 0.106 Uiso 0.50 1 d PR K -1 C53 C -0.1086(5) 0.5608(7) 0.0214(5) 0.093(4) Uiso 0.50 1 d PD K -1 H531 H -0.0951 0.6076 0.0245 0.121 Uiso 0.50 1 d PR K -1 H532 H -0.1074 0.5426 0.0511 0.121 Uiso 0.50 1 d PR K -1 C54 C -0.1674(5) 0.5625(7) -0.0086(6) 0.137(7) Uiso 0.50 1 d PD K -1 H541 H -0.1902 0.5905 0.0056 0.179 Uiso 0.50 1 d PR K -1 H542 H -0.1684 0.5813 -0.0381 0.179 Uiso 0.50 1 d PR K -1 C55 C -0.1890(6) 0.4896(8) -0.0155(7) 0.157(8) Uiso 0.50 1 d PD K -1 H551 H -0.1875 0.4706 0.0140 0.205 Uiso 0.50 1 d PR K -1 H552 H -0.2262 0.4888 -0.0321 0.205 Uiso 0.50 1 d PR K -1 C56 C -0.1533(6) 0.4432(9) -0.0369(7) 0.189(10) Uiso 0.50 1 d PD K -1 H561 H -0.1557 0.4612 -0.0668 0.245 Uiso 0.50 1 d PR K -1 H562 H -0.1660 0.3962 -0.0396 0.245 Uiso 0.50 1 d PR K -1 C57 C -0.0949(6) 0.4450(7) -0.0093(6) 0.134(7) Uiso 0.50 1 d PD K -1 H571 H -0.0924 0.4234 0.0196 0.175 Uiso 0.50 1 d PR K -1 H572 H -0.0724 0.4193 -0.0252 0.175 Uiso 0.50 1 d PR K -1 C58 C -0.0175(9) 0.5024(10) 0.0659(4) 0.127(4) Uiso 0.50 1 d PD K -1 H581 H 0.0201 0.5093 0.0791 0.190 Uiso 0.50 1 d PR K -1 H582 H -0.0256 0.4543 0.0656 0.190 Uiso 0.50 1 d PR K -1 H583 H -0.0387 0.5263 0.0833 0.190 Uiso 0.50 1 d PR K -1 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 Cr1 0.0779(6) 0.0505(5) 0.0503(5) 0.0020(4) -0.0070(4) 0.0072(5) Cr2 0.0412(4) 0.0550(5) 0.0351(4) 0.0010(3) 0.0016(3) 0.0020(4) Cr3 0.0497(5) 0.0514(5) 0.0412(4) -0.0003(3) 0.0054(3) -0.0041(4) Cr4 0.0493(4) 0.0490(4) 0.0424(4) 0.0009(3) 0.0010(3) -0.0039(3) Cr5 0.0668(5) 0.0441(4) 0.0450(4) 0.0037(3) -0.0021(3) -0.0001(4) Ni4 0.0493(4) 0.0490(4) 0.0424(4) 0.0009(3) 0.0010(3) -0.0039(3) Ni5 0.0668(5) 0.0441(4) 0.0450(4) 0.0037(3) -0.0021(3) -0.0001(4) F1 0.0527(16) 0.0528(16) 0.0395(14) 0.0041(12) -0.0044(12) -0.0014(13) F2 0.0421(14) 0.0546(16) 0.0343(13) 0.0010(11) 0.0050(11) 0.0021(12) F3 0.0446(14) 0.0561(17) 0.0423(14) 0.0001(12) 0.0036(11) 0.0006(13) F4 0.0703(19) 0.0484(17) 0.0532(17) 0.0011(13) 0.0074(14) 0.0074(14) F5 0.083(2) 0.0514(18) 0.077(2) 0.0045(15) 0.0041(17) -0.0089(16) F6 0.077(2) 0.0523(17) 0.0481(16) -0.0021(13) -0.0008(14) -0.0036(15) O1 0.105(3) 0.059(2) 0.056(2) 0.011(2) -0.013(2) 0.013(2) O2 0.082(3) 0.065(3) 0.0407(19) 0.0043(18) 0.0062(18) 0.003(2) O3 0.067(3) 0.078(3) 0.068(3) -0.013(2) 0.005(2) 0.017(2) O4 0.046(2) 0.062(2) 0.063(2) -0.0003(19) 0.0098(17) 0.0065(18) O5 0.068(2) 0.066(2) 0.0373(18) 0.0042(16) -0.0029(16) -0.008(2) O6 0.067(2) 0.069(2) 0.050(2) 0.0003(19) -0.0089(18) -0.014(2) O7 0.057(2) 0.055(2) 0.067(2) 0.0042(18) 0.0264(18) 0.0004(18) O8 0.064(2) 0.059(2) 0.048(2) 0.0036(17) 0.0212(17) 0.0051(19) O9 0.090(3) 0.051(2) 0.050(2) -0.0048(17) 0.010(2) -0.005(2) O10 0.087(3) 0.054(2) 0.055(2) -0.0017(18) -0.007(2) -0.015(2) O11 0.048(2) 0.071(2) 0.054(2) 0.0091(18) 0.0064(16) -0.0067(18) O12 0.055(2) 0.107(3) 0.053(2) 0.014(2) 0.0093(19) -0.009(2) O13 0.051(2) 0.068(2) 0.051(2) -0.0058(17) 0.0022(17) 0.0062(18) O14 0.062(2) 0.058(2) 0.051(2) -0.0062(17) -0.0015(17) 0.0043(18) O15 0.091(3) 0.053(2) 0.064(2) 0.0114(19) -0.006(2) 0.005(2) O16 0.110(4) 0.058(3) 0.078(3) -0.002(2) -0.012(3) 0.024(3) O17 0.077(3) 0.083(3) 0.040(2) 0.0056(18) 0.0035(18) -0.006(2) O18 0.104(3) 0.074(3) 0.038(2) 0.0127(18) 0.004(2) -0.016(2) C1 0.067(4) 0.069(4) 0.046(3) 0.003(3) -0.008(3) 0.000(3) C6 0.054(3) 0.072(4) 0.054(3) 0.008(3) 0.008(3) 0.005(3) C11 0.044(3) 0.066(4) 0.046(3) -0.001(3) 0.005(2) -0.003(3) C12 0.082(4) 0.082(4) 0.055(3) -0.004(3) -0.012(3) -0.019(4) C13 0.062(4) 0.143(7) 0.122(7) -0.026(6) -0.009(4) -0.029(5) C14 0.201(10) 0.143(8) 0.090(6) 0.030(5) -0.092(6) -0.073(7) C15 0.101(6) 0.175(9) 0.082(5) -0.049(6) -0.008(4) -0.024(6) C16 0.044(3) 0.069(4) 0.042(3) -0.004(3) 0.010(2) -0.001(3) C21 0.056(3) 0.051(3) 0.053(3) -0.006(3) 0.013(3) -0.010(3) C26 0.055(3) 0.104(5) 0.055(4) 0.002(3) 0.021(3) -0.007(3) C31 0.063(4) 0.054(3) 0.057(4) -0.003(3) 0.006(3) 0.004(3) C36 0.107(5) 0.052(4) 0.070(4) 0.008(3) -0.009(4) 0.011(4) C37 0.149(8) 0.062(5) 0.115(7) 0.011(4) -0.041(6) 0.022(5) C38 0.205(11) 0.063(5) 0.152(8) 0.004(5) -0.026(7) 0.026(6) C39 0.143(9) 0.119(8) 0.177(11) -0.012(7) -0.027(8) 0.052(7) C40 0.39(2) 0.143(9) 0.103(7) 0.052(7) 0.027(10) 0.126(11) C41 0.081(4) 0.084(4) 0.049(3) 0.021(3) 0.009(3) -0.013(3) _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 Cr1 F6 1.884(3) 5_565 ? Cr1 F1 1.937(3) . ? Cr1 O18 1.953(4) 5_565 ? Cr1 O16 1.959(4) 5_565 ? Cr1 O1 1.967(4) . ? Cr1 O3 1.982(4) . ? Cr2 F1 1.904(3) . ? Cr2 F2 1.915(3) . ? Cr2 O2 1.942(4) . ? Cr2 O7 1.949(4) . ? Cr2 O4 1.949(4) . ? Cr2 O5 1.955(3) . ? Cr3 F3 1.901(3) . ? Cr3 F2 1.930(3) . ? Cr3 O9 1.938(4) . ? Cr3 O11 1.943(4) . ? Cr3 O6 1.966(3) . ? Cr3 O8 1.970(3) . ? Cr4 F3 1.939(3) . ? Cr4 F4 1.957(3) . ? Cr4 O13 1.970(4) . ? Cr4 F5 1.977(3) . ? Cr4 O12 1.979(4) . ? Cr4 O10 2.001(4) . ? Cr5 F6 1.953(3) . ? Cr5 O14 1.977(4) . ? Cr5 F4 1.982(3) . ? Cr5 O17 1.988(4) . ? Cr5 F5 2.013(3) . ? Cr5 O15 2.022(4) . ? F6 Cr1 1.884(3) 5_565 ? O1 C1 1.267(7) . ? O2 C1 1.235(7) . ? O3 C6 1.240(7) . ? O4 C6 1.240(6) . ? O5 C11 1.243(6) . ? O6 C11 1.235(6) . ? O7 C16 1.254(6) . ? O8 C16 1.245(6) . ? O9 C21 1.264(6) . ? O10 C21 1.244(6) . ? O11 C26 1.252(6) . ? O12 C26 1.258(7) . ? O13 C31 1.265(6) . ? O14 C31 1.248(6) . ? O15 C36 1.244(7) . ? O16 C36 1.260(7) . ? O16 Cr1 1.959(4) 5_565 ? O17 C41 1.255(7) . ? O18 C41 1.265(7) . ? O18 Cr1 1.953(4) 5_565 ? C1 C2B 1.512(12) . ? C1 C2A 1.539(10) . ? C2A C4A 1.478(11) . ? C2A C5A 1.513(11) . ? C2A C3A 1.527(11) . ? C2B C3B 1.494(12) . ? C2B C4B 1.495(12) . ? C2B C5B 1.537(12) . ? C6 C7B 1.537(13) . ? C6 C7A 1.577(12) . ? C7A C8A 1.521(12) . ? C7A C10A 1.528(12) . ? C7A C9A 1.530(12) . ? C7B C8B 1.484(12) . ? C7B C10B 1.518(12) . ? C7B C9B 1.529(13) . ? C11 C12 1.528(7) . ? C12 C15 1.483(10) . ? C12 C13 1.504(9) . ? C12 C14 1.521(9) . ? C16 C17A 1.531(10) . ? C16 C17B 1.550(13) . ? C17A C20A 1.496(11) . ? C17A C19A 1.524(11) . ? C17A C18A 1.526(11) . ? C17B C20B 1.488(13) . ? C17B C18B 1.506(13) . ? C17B C19B 1.556(13) . ? C21 C22A 1.532(9) . ? C21 C22B 1.560(13) . ? C22A C23A 1.502(11) . ? C22A C24A 1.541(11) . ? C22A C25A 1.563(10) . ? C22B C24B 1.541(13) . ? C22B C25B 1.556(13) . ? C22B C23B 1.560(14) . ? C26 C27A 1.533(11) . ? C26 C27B 1.581(14) . ? C27A C28A 1.450(17) . ? C27A C30A 1.473(18) . ? C27A C29A 1.507(17) . ? C27B C29B 1.488(14) . ? C27B C28B 1.503(14) . ? C27B C30B 1.556(15) . ? C31 C32A 1.513(10) . ? C31 C32B 1.542(14) . ? C32A C34A 1.519(11) . ? C32A C35A 1.526(11) . ? C32A C33A 1.568(11) . ? C32B C34B 1.522(14) . ? C32B C33B 1.523(14) . ? C32B C35B 1.570(13) . ? C36 C37 1.525(9) . ? C37 C40 1.460(12) . ? C37 C38 1.523(11) . ? C37 C39 1.583(13) . ? C41 C42B 1.534(10) . ? C41 C42A 1.562(19) . ? C42A C45A 1.528(15) . ? C42A C44A 1.529(15) . ? C42A C43A 1.566(15) . ? C42B C44B 1.498(11) . ? C42B C43B 1.518(11) . ? C42B C45B 1.544(12) . ? N1 C52 1.351(14) . ? N1 C58 1.473(9) . ? N1 C46 1.496(14) . ? C46 C51 1.559(11) . ? C46 C47 1.599(13) . ? C47 C48B 1.28(3) . ? C47 C48A 1.560(14) . ? C48A C49 1.537(12) . ? C48A C48B 1.65(4) . ? C48B C49 1.95(3) . ? C49 C50 1.567(13) . ? C50 C51 1.606(13) . ? C52 C57 1.539(13) . ? C52 C53 1.551(13) . ? C53 C54 1.605(13) . ? C54 C55 1.552(14) . ? C55 C56 1.562(14) . ? C56 C57 1.570(14) . ? 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 F6 Cr1 F1 89.51(12) 5_565 . ? F6 Cr1 O18 91.75(14) 5_565 5_565 ? F1 Cr1 O18 88.15(15) . 5_565 ? F6 Cr1 O16 91.68(16) 5_565 5_565 ? F1 Cr1 O16 177.26(17) . 5_565 ? O18 Cr1 O16 94.3(2) 5_565 5_565 ? F6 Cr1 O1 177.54(16) 5_565 . ? F1 Cr1 O1 92.94(14) . . ? O18 Cr1 O1 88.10(17) 5_565 . ? O16 Cr1 O1 85.88(18) 5_565 . ? F6 Cr1 O3 90.63(15) 5_565 . ? F1 Cr1 O3 90.05(14) . . ? O18 Cr1 O3 177.00(17) 5_565 . ? O16 Cr1 O3 87.47(19) 5_565 . ? O1 Cr1 O3 89.60(18) . . ? F1 Cr2 F2 90.56(11) . . ? F1 Cr2 O2 91.40(13) . . ? F2 Cr2 O2 177.65(14) . . ? F1 Cr2 O7 89.09(14) . . ? F2 Cr2 O7 90.46(13) . . ? O2 Cr2 O7 88.27(16) . . ? F1 Cr2 O4 92.01(14) . . ? F2 Cr2 O4 89.51(13) . . ? O2 Cr2 O4 91.73(16) . . ? O7 Cr2 O4 178.90(17) . . ? F1 Cr2 O5 176.55(13) . . ? F2 Cr2 O5 92.84(13) . . ? O2 Cr2 O5 85.22(15) . . ? O7 Cr2 O5 91.47(16) . . ? O4 Cr2 O5 87.43(16) . . ? F3 Cr3 F2 89.40(11) . . ? F3 Cr3 O9 92.87(14) . . ? F2 Cr3 O9 177.25(13) . . ? F3 Cr3 O11 92.68(13) . . ? F2 Cr3 O11 89.69(14) . . ? O9 Cr3 O11 91.75(16) . . ? F3 Cr3 O6 179.41(15) . . ? F2 Cr3 O6 90.68(14) . . ? O9 Cr3 O6 87.03(16) . . ? O11 Cr3 O6 87.90(15) . . ? F3 Cr3 O8 88.98(13) . . ? F2 Cr3 O8 91.10(13) . . ? O9 Cr3 O8 87.39(16) . . ? O11 Cr3 O8 178.16(15) . . ? O6 Cr3 O8 90.43(15) . . ? F3 Cr4 F4 90.44(11) . . ? F3 Cr4 O13 89.71(13) . . ? F4 Cr4 O13 91.20(13) . . ? F3 Cr4 F5 170.69(12) . . ? F4 Cr4 F5 80.30(13) . . ? O13 Cr4 F5 89.56(15) . . ? F3 Cr4 O12 91.46(14) . . ? F4 Cr4 O12 91.55(15) . . ? O13 Cr4 O12 177.01(17) . . ? F5 Cr4 O12 89.73(15) . . ? F3 Cr4 O10 95.86(13) . . ? F4 Cr4 O10 173.48(13) . . ? O13 Cr4 O10 87.17(16) . . ? F5 Cr4 O10 93.38(14) . . ? O12 Cr4 O10 89.97(17) . . ? F6 Cr5 O14 88.65(14) . . ? F6 Cr5 F4 90.29(12) . . ? O14 Cr5 F4 90.98(13) . . ? F6 Cr5 O17 90.81(15) . . ? O14 Cr5 O17 177.39(15) . . ? F4 Cr5 O17 91.57(14) . . ? F6 Cr5 F5 168.70(12) . . ? O14 Cr5 F5 88.54(14) . . ? F4 Cr5 F5 78.82(12) . . ? O17 Cr5 F5 92.47(15) . . ? F6 Cr5 O15 97.97(14) . . ? O14 Cr5 O15 86.19(16) . . ? F4 Cr5 O15 171.20(14) . . ? O17 Cr5 O15 91.36(17) . . ? F5 Cr5 O15 92.76(14) . . ? Cr2 F1 Cr1 123.18(13) . . ? Cr2 F2 Cr3 122.90(13) . . ? Cr3 F3 Cr4 121.98(14) . . ? Cr4 F4 Cr5 98.72(12) . . ? Cr4 F5 Cr5 97.04(13) . . ? Cr1 F6 Cr5 119.63(15) 5_565 . ? C1 O1 Cr1 134.7(4) . . ? C1 O2 Cr2 132.1(4) . . ? C6 O3 Cr1 129.1(4) . . ? C6 O4 Cr2 135.2(4) . . ? C11 O5 Cr2 134.4(3) . . ? C11 O6 Cr3 129.5(3) . . ? C16 O7 Cr2 127.8(3) . . ? C16 O8 Cr3 135.7(3) . . ? C21 O9 Cr3 135.4(3) . . ? C21 O10 Cr4 130.9(4) . . ? C26 O11 Cr3 135.2(3) . . ? C26 O12 Cr4 131.0(4) . . ? C31 O13 Cr4 127.8(4) . . ? C31 O14 Cr5 128.5(4) . . ? C36 O15 Cr5 127.6(4) . . ? C36 O16 Cr1 130.4(4) . 5_565 ? C41 O17 Cr5 126.6(4) . . ? C41 O18 Cr1 136.1(4) . 5_565 ? O2 C1 O1 124.2(5) . . ? O2 C1 C2B 122.9(6) . . ? O1 C1 C2B 111.4(6) . . ? O2 C1 C2A 113.2(6) . . ? O1 C1 C2A 122.0(6) . . ? C2B C1 C2A 23.0(5) . . ? C4A C2A C5A 112.5(9) . . ? C4A C2A C3A 109.3(8) . . ? C5A C2A C3A 108.1(9) . . ? C4A C2A C1 111.2(8) . . ? C5A C2A C1 107.6(10) . . ? C3A C2A C1 108.0(8) . . ? C3B C2B C4B 110.7(9) . . ? C3B C2B C1 105.1(10) . . ? C4B C2B C1 113.8(10) . . ? C3B C2B C5B 109.5(9) . . ? C4B C2B C5B 110.7(9) . . ? C1 C2B C5B 106.8(10) . . ? O4 C6 O3 127.5(5) . . ? O4 C6 C7B 120.8(7) . . ? O3 C6 C7B 111.5(7) . . ? O4 C6 C7A 110.0(7) . . ? O3 C6 C7A 122.2(7) . . ? C7B C6 C7A 16.5(7) . . ? C8A C7A C10A 110.1(10) . . ? C8A C7A C9A 108.8(9) . . ? C10A C7A C9A 108.6(9) . . ? C8A C7A C6 109.8(10) . . ? C10A C7A C6 110.8(10) . . ? C9A C7A C6 108.6(10) . . ? C8B C7B C10B 113.3(10) . . ? C8B C7B C9B 110.9(10) . . ? C10B C7B C9B 108.8(10) . . ? C8B C7B C6 113.9(12) . . ? C10B C7B C6 108.2(10) . . ? C9B C7B C6 101.0(11) . . ? O6 C11 O5 126.2(5) . . ? O6 C11 C12 116.5(5) . . ? O5 C11 C12 117.3(5) . . ? C15 C12 C13 109.0(6) . . ? C15 C12 C14 113.5(7) . . ? C13 C12 C14 107.5(7) . . ? C15 C12 C11 107.8(5) . . ? C13 C12 C11 108.5(5) . . ? C14 C12 C11 110.4(5) . . ? O8 C16 O7 125.9(5) . . ? O8 C16 C17A 112.7(6) . . ? O7 C16 C17A 121.2(6) . . ? O8 C16 C17B 121.7(7) . . ? O7 C16 C17B 111.8(7) . . ? C17A C16 C17B 15.6(7) . . ? C20A C17A C19A 113.3(9) . . ? C20A C17A C18A 108.4(9) . . ? C19A C17A C18A 106.4(8) . . ? C20A C17A C16 112.0(9) . . ? C19A C17A C16 111.2(9) . . ? C18A C17A C16 104.9(8) . . ? C20B C17B C18B 112.0(11) . . ? C20B C17B C16 111.5(13) . . ? C18B C17B C16 108.3(12) . . ? C20B C17B C19B 108.2(10) . . ? C18B C17B C19B 108.0(10) . . ? C16 C17B C19B 108.7(11) . . ? O10 C21 O9 125.7(5) . . ? O10 C21 C22A 116.4(5) . . ? O9 C21 C22A 117.3(5) . . ? O10 C21 C22B 120.5(7) . . ? O9 C21 C22B 112.6(6) . . ? C22A C21 C22B 20.9(6) . . ? C23A C22A C21 108.3(8) . . ? C23A C22A C24A 113.8(8) . . ? C21 C22A C24A 104.6(8) . . ? C23A C22A C25A 112.8(7) . . ? C21 C22A C25A 107.1(7) . . ? C24A C22A C25A 109.6(8) . . ? C24B C22B C25B 109.9(11) . . ? C24B C22B C21 108.4(12) . . ? C25B C22B C21 110.4(12) . . ? C24B C22B C23B 108.3(11) . . ? C25B C22B C23B 106.4(11) . . ? C21 C22B C23B 113.4(15) . . ? O11 C26 O12 126.3(5) . . ? O11 C26 C27A 112.4(6) . . ? O12 C26 C27A 119.6(6) . . ? O11 C26 C27B 115.9(6) . . ? O12 C26 C27B 114.6(6) . . ? C27A C26 C27B 33.4(5) . . ? C28A C27A C30A 110.9(14) . . ? C28A C27A C29A 105.9(13) . . ? C30A C27A C29A 104.7(12) . . ? C28A C27A C26 115.1(16) . . ? C30A C27A C26 105.8(16) . . ? C29A C27A C26 113.9(16) . . ? C29B C27B C28B 112.7(10) . . ? C29B C27B C30B 103.3(10) . . ? C28B C27B C30B 103.3(10) . . ? C29B C27B C26 110.9(10) . . ? C28B C27B C26 111.2(10) . . ? C30B C27B C26 115.0(11) . . ? O14 C31 O13 125.5(5) . . ? O14 C31 C32A 114.3(6) . . ? O13 C31 C32A 120.0(6) . . ? O14 C31 C32B 122.0(7) . . ? O13 C31 C32B 111.5(7) . . ? C32A C31 C32B 17.4(8) . . ? C31 C32A C34A 111.3(8) . . ? C31 C32A C35A 112.6(9) . . ? C34A C32A C35A 111.1(8) . . ? C31 C32A C33A 107.4(8) . . ? C34A C32A C33A 106.8(8) . . ? C35A C32A C33A 107.4(8) . . ? C34B C32B C33B 111.5(12) . . ? C34B C32B C31 111.7(14) . . ? C33B C32B C31 110.0(17) . . ? C34B C32B C35B 107.9(11) . . ? C33B C32B C35B 108.8(11) . . ? C31 C32B C35B 106.8(12) . . ? O15 C36 O16 126.5(6) . . ? O15 C36 C37 117.9(6) . . ? O16 C36 C37 115.4(6) . . ? C40 C37 C38 116.6(9) . . ? C40 C37 C36 108.7(8) . . ? C38 C37 C36 112.0(6) . . ? C40 C37 C39 109.3(9) . . ? C38 C37 C39 103.4(9) . . ? C36 C37 C39 106.3(7) . . ? O17 C41 O18 125.3(6) . . ? O17 C41 C42B 120.4(6) . . ? O18 C41 C42B 114.0(6) . . ? O17 C41 C42A 111.5(8) . . ? O18 C41 C42A 123.3(9) . . ? C42B C41 C42A 10.8(9) . . ? C45A C42A C44A 109.8(12) . . ? C45A C42A C41 110.2(13) . . ? C44A C42A C41 112.7(17) . . ? C45A C42A C43A 108.5(12) . . ? C44A C42A C43A 105.4(12) . . ? C41 C42A C43A 110.0(16) . . ? C44B C42B C43B 111.3(9) . . ? C44B C42B C41 104.0(9) . . ? C43B C42B C41 112.5(9) . . ? C44B C42B C45B 109.7(9) . . ? C43B C42B C45B 110.1(8) . . ? C41 C42B C45B 109.1(10) . . ? C52 N1 C58 112.1(13) . . ? C52 N1 C46 119.7(10) . . ? C58 N1 C46 110.0(11) . . ? N1 C46 C51 111.5(9) . . ? N1 C46 C47 106.9(8) . . ? C51 C46 C47 110.7(8) . . ? C48B C47 C48A 70.4(17) . . ? C48B C47 C46 99.1(18) . . ? C48A C47 C46 111.5(9) . . ? C49 C48A C47 112.7(9) . . ? C49 C48A C48B 75.4(13) . . ? C47 C48A C48B 46.9(13) . . ? C47 C48B C48A 62.7(16) . . ? C47 C48B C49 104(2) . . ? C48A C48B C49 49.6(10) . . ? C48A C49 C50 113.2(9) . . ? C48A C49 C48B 55.0(12) . . ? C50 C49 C48B 93.4(12) . . ? C49 C50 C51 113.8(9) . . ? C46 C51 C50 107.0(8) . . ? N1 C52 C57 112.8(11) . . ? N1 C52 C53 108.4(11) . . ? C57 C52 C53 111.2(10) . . ? C52 C53 C54 107.4(9) . . ? C55 C54 C53 109.2(10) . . ? C54 C55 C56 112.3(11) . . ? C55 C56 C57 110.2(11) . . ? C52 C57 C56 110.9(10) . . ? 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 N1 H1 F4 0.93 2.02 2.932(11) 167.4 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.737 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.084 data_orepw98absc _database_code_depnum_ccdc_archive 'CCDC 268361' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C107 H198 Cr9 F10 N Ni O40' _chemical_formula_weight 2855.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr .3209 .6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni .3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Cmca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 32.686(3) _cell_length_b 20.8976(19) _cell_length_c 22.154(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15132(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7167 _cell_measurement_theta_min 2.4846 _cell_measurement_theta_max 31.9523 _exptl_crystal_description prismatic _exptl_crystal_colour Green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6000 _exptl_absorpt_coefficient_mu 0.819 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.8801 _exptl_absorpt_correction_T_max 0.9197 _exptl_absorpt_process_details ? _exptl_special_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.pre23_9 beta (release 18.06.2004 CrysAlis171 .NET) (compiled Jun 18 2004,12:34:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18144 _diffrn_reflns_av_R_equivalents 0.0882 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 16.52 _reflns_number_total 2082 _reflns_number_gt 1941 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Limited data set with poor data to parameter ratio. Unable to determine Ni position, so averaged over all positions with Cr. All carbons left isotropic due lack of data. Unable to model amine due to high symmetry. N1 and C56 modelled with 0.25 occupancy due to four fold symmetry for these atoms while C54,C55,C57 with 0.5 to ensure correct chemical formula. Insufficient data to place hydrogens. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0005(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2082 _refine_ls_number_parameters 325 _refine_ls_number_restraints 328 _refine_ls_R_factor_all 0.1552 _refine_ls_R_factor_gt 0.1488 _refine_ls_wR_factor_ref 0.4272 _refine_ls_wR_factor_gt 0.4206 _refine_ls_goodness_of_fit_ref 2.082 _refine_ls_restrained_S_all 2.052 _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 0.63215(10) 0.37341(15) 0.07461(15) 0.062(2) Uani 0.10 1 d P . . Cr1 Cr 0.63215(10) 0.37341(15) 0.07461(15) 0.062(2) Uani 0.90 1 d P . . Cr2 Cr 0.54993(10) 0.29352(17) 0.11336(16) 0.071(2) Uani 0.90 1 d P . . Cr3 Cr 0.66467(15) 0.5000 0.0000 0.077(3) Uani 0.90 2 d SP . . Ni2 Ni 0.54993(10) 0.29352(17) 0.11336(16) 0.071(2) Uani 0.10 1 d P . . Ni3 Ni 0.66467(15) 0.5000 0.0000 0.077(3) Uani 0.10 2 d SP . . F1 F 0.5000 0.3380(7) 0.1125(6) 0.072(6) Uani 1 2 d S . . F2 F 0.5766(4) 0.3500(5) 0.0607(4) 0.072(4) Uani 1 1 d . . . F3 F 0.6241(3) 0.4594(5) 0.0493(4) 0.057(4) Uani 1 1 d . . . O1 O 0.7104(6) 0.4676(10) 0.0463(11) 0.150(7) Uani 1 1 d U A . O2 O 0.6889(7) 0.3894(10) 0.0977(9) 0.133(7) Uani 1 1 d U A . O3 O 0.6644(6) 0.4273(8) -0.0561(7) 0.113(6) Uani 1 1 d U B . O4 O 0.6460(6) 0.3475(7) -0.0062(9) 0.114(6) Uani 1 1 d U B . O5 O 0.6481(6) 0.2892(11) 0.1004(10) 0.141(7) Uani 1 1 d U C . O6 O 0.5975(7) 0.2342(9) 0.1204(10) 0.140(7) Uani 1 1 d U C . O7 O 0.6197(5) 0.4006(8) 0.1556(7) 0.089(5) Uani 1 1 d U D . O8 O 0.5672(5) 0.3420(8) 0.1831(6) 0.091(5) Uani 1 1 d U D . O9 O 0.5330(4) 0.2437(7) 0.0463(7) 0.091(5) Uani 1 1 d U . . O10 O 0.5310(7) 0.2263(9) 0.1689(9) 0.134(7) Uani 1 1 d U . . C1 C 0.7139(9) 0.4237(18) 0.0850(15) 0.117(7) Uiso 1 1 d DU . . C2 C 0.7558(8) 0.4172(12) 0.1204(11) 0.093(10) Uiso 0.60 1 d PDU A 1 C3 C 0.7873(12) 0.4061(18) 0.0728(15) 0.115(14) Uiso 0.60 1 d PDU A 1 C4 C 0.7546(12) 0.3630(14) 0.1644(16) 0.097(13) Uiso 0.60 1 d PDU A 1 C5 C 0.7625(13) 0.4795(15) 0.1517(16) 0.103(13) Uiso 0.60 1 d PDU A 1 C2A C 0.7605(8) 0.4256(18) 0.1047(18) 0.093(11) Uiso 0.40 1 d PDU A 2 C3A C 0.7912(15) 0.464(2) 0.070(2) 0.082(16) Uiso 0.40 1 d PDU A 2 C4A C 0.7715(19) 0.3563(19) 0.105(3) 0.118(17) Uiso 0.40 1 d PDU A 2 C5A C 0.7553(19) 0.451(3) 0.167(2) 0.114(18) Uiso 0.40 1 d PDU A 2 C6 C 0.6532(8) 0.3706(14) -0.0550(13) 0.100(7) Uiso 1 1 d DU . . C7 C 0.6561(7) 0.3226(12) -0.1104(12) 0.119(11) Uiso 0.60 1 d PDU B 1 C8 C 0.6969(10) 0.338(2) -0.1376(15) 0.135(16) Uiso 0.60 1 d PDU B 1 C9 C 0.6203(11) 0.3405(18) -0.1489(14) 0.104(13) Uiso 0.60 1 d PDU B 1 C10 C 0.6531(14) 0.2581(15) -0.0817(19) 0.140(16) Uiso 0.60 1 d PDU B 1 C7A C 0.6540(10) 0.3387(16) -0.1200(14) 0.118(12) Uiso 0.40 1 d PDU B 2 C8A C 0.658(2) 0.394(3) -0.1618(16) 0.14(2) Uiso 0.40 1 d PDU B 2 C9A C 0.6139(15) 0.304(3) -0.123(2) 0.13(2) Uiso 0.40 1 d PDU B 2 C10A C 0.6906(16) 0.296(2) -0.118(2) 0.117(18) Uiso 0.40 1 d PDU B 2 C11 C 0.6330(11) 0.2375(16) 0.1152(14) 0.120(8) Uiso 1 1 d DU . . C12 C 0.6649(8) 0.1834(13) 0.1325(11) 0.095(10) Uiso 0.70 1 d PDU C 1 C13 C 0.6917(10) 0.2067(16) 0.1835(14) 0.107(13) Uiso 0.70 1 d PDU C 1 C14 C 0.6900(11) 0.1672(19) 0.0775(14) 0.120(14) Uiso 0.70 1 d PDU C 1 C15 C 0.6390(10) 0.1273(15) 0.1521(15) 0.087(11) Uiso 0.70 1 d PDU C 1 C12A C 0.6503(18) 0.1667(17) 0.120(2) 0.098(12) Uiso 0.30 1 d PDU C 2 C13A C 0.677(2) 0.157(4) 0.065(3) 0.10(2) Uiso 0.30 1 d PDU C 2 C14A C 0.618(2) 0.115(4) 0.125(3) 0.10(2) Uiso 0.30 1 d PDU C 2 C15A C 0.676(2) 0.170(4) 0.176(3) 0.091(18) Uiso 0.30 1 d PDU C 2 C16 C 0.5933(9) 0.3838(12) 0.1923(10) 0.072(6) Uiso 1 1 d DU . . C17 C 0.5910(8) 0.4085(11) 0.2600(10) 0.071(8) Uiso 0.70 1 d PDU D 1 C18 C 0.6115(10) 0.3563(15) 0.2983(17) 0.104(13) Uiso 0.70 1 d PDU D 1 C19 C 0.5480(10) 0.4207(17) 0.2859(19) 0.141(15) Uiso 0.70 1 d PDU D 1 C20 C 0.6160(10) 0.4703(15) 0.2664(18) 0.116(12) Uiso 0.70 1 d PDU D 1 C17A C 0.6116(15) 0.425(2) 0.2463(19) 0.084(12) Uiso 0.30 1 d PDU D 2 C18A C 0.625(2) 0.380(3) 0.298(3) 0.09(2) Uiso 0.30 1 d PDU D 2 C19A C 0.5770(19) 0.468(3) 0.270(3) 0.107(18) Uiso 0.30 1 d PDU D 2 C20A C 0.6481(18) 0.468(3) 0.230(3) 0.09(2) Uiso 0.30 1 d PDU D 2 C21 C 0.5000 0.2323(16) 0.0189(13) 0.094(9) Uiso 1 2 d SDU . . C22 C 0.5000 0.2025(17) -0.0471(15) 0.162(14) Uiso 1 2 d SDU . . C23 C 0.5408(9) 0.1701(19) -0.0492(18) 0.29(2) Uiso 1 1 d DU . . C24 C 0.5000 0.261(2) -0.0860(16) 0.27(3) Uiso 1 2 d SDU . . C26 C 0.5000 0.212(2) 0.193(2) 0.122(11) Uiso 1 2 d SU . . C27 C 0.5000 0.150(2) 0.2319(19) 0.121(12) Uiso 1 2 d SU . . C28 C 0.5000 0.088(2) 0.189(2) 0.158(17) Uiso 1 2 d SU . . C29 C 0.4621(13) 0.1525(19) 0.2722(18) 0.188(15) Uiso 1 1 d . . . N1 N 0.537(9) 0.5000 0.0000 0.56(17) Uiso 0.50 2 d SP . . C54 C 0.462(2) 0.510(4) 0.084(3) 0.16(3) Uiso 0.50 1 d P . . C55 C 0.5000 0.532(2) 0.052(2) 0.132(15) Uiso 1 2 d S . . C56 C 0.5000 0.605(6) 0.055(5) 0.18(4) Uiso 0.50 2 d SP . . C57 C 0.461(2) 0.561(3) 0.059(3) 0.13(2) Uiso 0.50 1 d P . . 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 0.065(3) 0.058(3) 0.063(3) 0.0165(19) 0.012(2) -0.0197(19) Cr1 0.065(3) 0.058(3) 0.063(3) 0.0165(19) 0.012(2) -0.0197(19) Cr2 0.041(3) 0.088(4) 0.084(4) 0.015(2) 0.003(2) -0.021(2) Cr3 0.070(4) 0.064(4) 0.096(5) 0.051(3) 0.000 0.000 Ni2 0.041(3) 0.088(4) 0.084(4) 0.015(2) 0.003(2) -0.021(2) Ni3 0.070(4) 0.064(4) 0.096(5) 0.051(3) 0.000 0.000 F1 0.115(16) 0.043(10) 0.059(11) -0.025(8) 0.000 0.000 F2 0.092(10) 0.078(8) 0.047(7) -0.004(6) -0.002(7) -0.005(7) F3 0.074(8) 0.062(8) 0.036(7) -0.021(6) -0.001(6) -0.003(6) O1 0.096(12) 0.138(13) 0.217(16) 0.076(12) -0.019(12) -0.003(11) O2 0.114(14) 0.138(13) 0.147(13) 0.069(11) -0.019(11) 0.017(11) O3 0.147(13) 0.093(11) 0.100(11) 0.023(9) 0.081(10) 0.044(10) O4 0.149(12) 0.058(9) 0.135(13) -0.026(9) 0.063(11) -0.032(10) O5 0.091(11) 0.130(14) 0.202(16) 0.049(12) 0.026(12) 0.025(10) O6 0.123(14) 0.096(12) 0.202(16) 0.060(11) -0.031(12) -0.006(10) O7 0.084(10) 0.130(11) 0.052(9) 0.009(9) -0.013(8) -0.066(9) O8 0.075(10) 0.145(12) 0.053(9) 0.007(9) -0.002(8) -0.059(9) O9 0.040(10) 0.100(10) 0.134(12) -0.047(10) 0.033(9) -0.009(8) O10 0.116(13) 0.143(13) 0.143(14) 0.070(11) -0.036(12) -0.005(11) _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 F3 1.900(11) . ? Ni1 F2 1.905(12) . ? Ni1 O5 1.92(2) . ? Ni1 O4 1.925(18) . ? Ni1 O7 1.927(16) . ? Ni1 O2 1.95(2) . ? Cr2 F2 1.876(11) . ? Cr2 F1 1.878(8) . ? Cr2 O9 1.897(15) . ? Cr2 O8 1.932(15) . ? Cr2 O10 1.967(18) . ? Cr2 O6 2.00(2) . ? Cr3 F3 1.916(11) . ? Cr3 F3 1.916(11) 4_565 ? Cr3 O1 1.94(2) 4_565 ? Cr3 O1 1.94(2) . ? Cr3 O3 1.963(18) . ? Cr3 O3 1.963(18) 4_565 ? F1 Ni2 1.878(8) 12_655 ? F1 Cr2 1.878(8) 12_655 ? O1 C1 1.26(3) . ? O2 C1 1.12(3) . ? O3 C6 1.24(3) . ? O4 C6 1.21(3) . ? O5 C11 1.23(3) . ? O6 C11 1.17(3) . ? O7 C16 1.24(2) . ? O8 C16 1.24(3) . ? O9 C21 1.261(19) . ? O10 C26 1.18(3) . ? C1 C2 1.58(2) . ? C1 C2A 1.59(2) . ? C2 C3 1.492(18) . ? C2 C5 1.492(18) . ? C2 C4 1.494(18) . ? C2A C3A 1.492(18) . ? C2A C5A 1.492(18) . ? C2A C4A 1.493(18) . ? C6 C7A 1.59(2) . ? C6 C7 1.588(19) . ? C7 C10 1.49(2) . ? C7 C9 1.49(2) . ? C7 C8 1.50(2) . ? C7A C8A 1.49(2) . ? C7A C10A 1.49(2) . ? C7A C9A 1.50(2) . ? C11 C12 1.583(19) . ? C11 C12A 1.59(2) . ? C12 C15 1.509(19) . ? C12 C13 1.509(19) . ? C12 C14 1.509(19) . ? C12A C13A 1.51(2) . ? C12A C14A 1.51(2) . ? C12A C15A 1.51(2) . ? C16 C17 1.587(19) . ? C16 C17A 1.59(2) . ? C17 C20 1.54(2) . ? C17 C18 1.54(2) . ? C17 C19 1.54(2) . ? C17A C19A 1.54(2) . ? C17A C18A 1.54(2) . ? C17A C20A 1.54(2) . ? C21 O9 1.261(19) 12_655 ? C21 C22 1.59(2) . ? C22 C24 1.496(18) . ? C22 C23 1.496(18) . ? C22 C23 1.496(18) 12_655 ? C26 O10 1.18(3) 12_655 ? C26 C27 1.56(6) . ? C27 C29 1.53(4) 12_655 ? C27 C29 1.53(4) . ? C27 C28 1.61(6) . ? N1 C55 1.8(2) . ? N1 C55 1.8(2) 9_665 ? N1 C57 1.84(6) 9_665 ? N1 C57 1.84(6) 12_655 ? N1 C54 1.87(8) 12_655 ? N1 C54 1.87(8) 9_665 ? C54 C57 1.20(7) . ? C54 C55 1.51(8) . ? C54 N1 1.87(8) 9_665 ? C55 C57 1.44(7) 12_655 ? C55 C57 1.44(6) . ? C55 C54 1.51(8) 12_655 ? C55 C56 1.52(12) . ? C55 N1 1.8(2) 9_665 ? C56 C57 1.58(9) 12_655 ? C56 C57 1.58(9) . ? C57 N1 1.84(6) 9_665 ? 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 F3 Ni1 F2 93.6(5) . . ? F3 Ni1 O5 172.1(7) . . ? F2 Ni1 O5 94.2(8) . . ? F3 Ni1 O4 91.4(6) . . ? F2 Ni1 O4 90.0(6) . . ? O5 Ni1 O4 87.4(9) . . ? F3 Ni1 O7 88.1(6) . . ? F2 Ni1 O7 91.4(5) . . ? O5 Ni1 O7 92.9(8) . . ? O4 Ni1 O7 178.5(7) . . ? F3 Ni1 O2 92.6(6) . . ? F2 Ni1 O2 172.5(7) . . ? O5 Ni1 O2 79.7(9) . . ? O4 Ni1 O2 93.9(8) . . ? O7 Ni1 O2 84.7(8) . . ? F2 Cr2 F1 94.9(6) . . ? F2 Cr2 O9 89.6(6) . . ? F1 Cr2 O9 90.6(6) . . ? F2 Cr2 O8 91.8(5) . . ? F1 Cr2 O8 90.1(7) . . ? O9 Cr2 O8 178.3(7) . . ? F2 Cr2 O10 170.1(7) . . ? F1 Cr2 O10 95.0(8) . . ? O9 Cr2 O10 90.4(8) . . ? O8 Cr2 O10 88.0(8) . . ? F2 Cr2 O6 94.4(7) . . ? F1 Cr2 O6 170.3(7) . . ? O9 Cr2 O6 87.0(8) . . ? O8 Cr2 O6 92.1(8) . . ? O10 Cr2 O6 75.7(8) . . ? F3 Cr3 F3 92.5(7) . 4_565 ? F3 Cr3 O1 172.6(7) . 4_565 ? F3 Cr3 O1 94.4(7) 4_565 4_565 ? F3 Cr3 O1 94.4(7) . . ? F3 Cr3 O1 172.6(7) 4_565 . ? O1 Cr3 O1 78.9(13) 4_565 . ? F3 Cr3 O3 90.9(5) . . ? F3 Cr3 O3 88.8(6) 4_565 . ? O1 Cr3 O3 86.5(8) 4_565 . ? O1 Cr3 O3 93.9(9) . . ? F3 Cr3 O3 88.8(6) . 4_565 ? F3 Cr3 O3 90.9(5) 4_565 4_565 ? O1 Cr3 O3 93.9(9) 4_565 4_565 ? O1 Cr3 O3 86.5(8) . 4_565 ? O3 Cr3 O3 179.5(11) . 4_565 ? Cr2 F1 Ni2 120.7(8) . 12_655 ? Cr2 F1 Cr2 120.7(8) . 12_655 ? Ni2 F1 Cr2 0.0(3) 12_655 12_655 ? Cr2 F2 Ni1 120.2(6) . . ? Ni1 F3 Cr3 119.5(6) . . ? C1 O1 Cr3 133.1(19) . . ? C1 O2 Ni1 137(2) . . ? C6 O3 Cr3 136.7(18) . . ? C6 O4 Ni1 140.0(19) . . ? C11 O5 Ni1 141(2) . . ? C11 O6 Cr2 137(2) . . ? C16 O7 Ni1 132.5(14) . . ? C16 O8 Cr2 134.6(15) . . ? C21 O9 Cr2 136.9(17) . . ? C26 O10 Cr2 137(3) . . ? O2 C1 O1 125(3) . . ? O2 C1 C2 117(3) . . ? O1 C1 C2 118(3) . . ? O2 C1 C2A 130(4) . . ? O1 C1 C2A 105(3) . . ? C2 C1 C2A 15.2(18) . . ? C3 C2 C5 111.3(12) . . ? C3 C2 C4 111.2(12) . . ? C5 C2 C4 111.2(12) . . ? C3 C2 C1 105(3) . . ? C5 C2 C1 106(3) . . ? C4 C2 C1 111(3) . . ? C3A C2A C5A 111.3(13) . . ? C3A C2A C4A 111.2(13) . . ? C5A C2A C4A 111.3(13) . . ? C3A C2A C1 121(4) . . ? C5A C2A C1 99(4) . . ? C4A C2A C1 102(4) . . ? O4 C6 O3 117(3) . . ? O4 C6 C7A 130(2) . . ? O3 C6 C7A 112(2) . . ? O4 C6 C7 117(2) . . ? O3 C6 C7 125(2) . . ? C7A C6 C7 14.6(14) . . ? C10 C7 C9 114.7(12) . . ? C10 C7 C8 114.8(12) . . ? C9 C7 C8 114.5(12) . . ? C10 C7 C6 103.7(15) . . ? C9 C7 C6 103.7(15) . . ? C8 C7 C6 103.4(15) . . ? C8A C7A C10A 114.8(12) . . ? C8A C7A C9A 114.6(12) . . ? C10A C7A C9A 114.6(12) . . ? C8A C7A C6 103.6(15) . . ? C10A C7A C6 103.7(15) . . ? C9A C7A C6 103.5(15) . . ? O6 C11 O5 118(3) . . ? O6 C11 C12 126(3) . . ? O5 C11 C12 115(3) . . ? O6 C11 C12A 107(4) . . ? O5 C11 C12A 134(4) . . ? C12 C11 C12A 24(2) . . ? C15 C12 C13 111.2(13) . . ? C15 C12 C14 111.2(13) . . ? C13 C12 C14 111.1(13) . . ? C15 C12 C11 105(3) . . ? C13 C12 C11 109(3) . . ? C14 C12 C11 109(3) . . ? C13A C12A C14A 111.0(14) . . ? C13A C12A C15A 111.1(14) . . ? C14A C12A C15A 111.0(14) . . ? C13A C12A C11 106(5) . . ? C14A C12A C11 115(5) . . ? C15A C12A C11 102(4) . . ? O7 C16 O8 125(2) . . ? O7 C16 C17 124(2) . . ? O8 C16 C17 111(2) . . ? O7 C16 C17A 94(3) . . ? O8 C16 C17A 140(3) . . ? C17 C16 C17A 30(2) . . ? C20 C17 C18 108.3(13) . . ? C20 C17 C19 108.2(13) . . ? C18 C17 C19 108.0(13) . . ? C20 C17 C16 110(2) . . ? C18 C17 C16 106(2) . . ? C19 C17 C16 117(3) . . ? C19A C17A C18A 108.1(14) . . ? C19A C17A C20A 107.9(14) . . ? C18A C17A C20A 107.9(14) . . ? C19A C17A C16 107(4) . . ? C18A C17A C16 110(4) . . ? C20A C17A C16 116(4) . . ? O9 C21 O9 118(3) . 12_655 ? O9 C21 C22 121.1(13) . . ? O9 C21 C22 121.1(13) 12_655 . ? C24 C22 C23 110.6(13) . . ? C24 C22 C23 110.6(13) . 12_655 ? C23 C22 C23 126(3) . 12_655 ? C24 C22 C21 102.1(13) . . ? C23 C22 C21 101.9(13) . . ? C23 C22 C21 101.9(13) 12_655 . ? O10 C26 O10 118(5) . 12_655 ? O10 C26 C27 118(3) . . ? O10 C26 C27 118(3) 12_655 . ? C29 C27 C29 108(4) 12_655 . ? C29 C27 C26 107(3) 12_655 . ? C29 C27 C26 107(3) . . ? C29 C27 C28 112(3) 12_655 . ? C29 C27 C28 112(3) . . ? C26 C27 C28 110(4) . . ? C55 N1 C55 95(10) . 9_665 ? C55 N1 C57 138(10) . 9_665 ? C55 N1 C57 46(3) 9_665 9_665 ? C55 N1 C57 46(3) . 12_655 ? C55 N1 C57 138(10) 9_665 12_655 ? C57 N1 C57 176(10) 9_665 12_655 ? C55 N1 C54 48(3) . 12_655 ? C55 N1 C54 134(10) 9_665 12_655 ? C57 N1 C54 142(3) 9_665 12_655 ? C57 N1 C54 38(2) 12_655 12_655 ? C55 N1 C54 134(10) . 9_665 ? C55 N1 C54 48(3) 9_665 9_665 ? C57 N1 C54 38(2) 9_665 9_665 ? C57 N1 C54 142(3) 12_655 9_665 ? C54 N1 C54 178(10) 12_655 9_665 ? C57 C54 C55 63(5) . . ? C57 C54 N1 70(5) . 9_665 ? C55 C54 N1 64(9) . 9_665 ? C57 C55 C57 127(6) 12_655 . ? C57 C55 C54 48(3) 12_655 12_655 ? C57 C55 C54 146(5) . 12_655 ? C57 C55 C54 146(5) 12_655 . ? C57 C55 C54 48(3) . . ? C54 C55 C54 113(7) 12_655 . ? C57 C55 C56 64(3) 12_655 . ? C57 C55 C56 64(3) . . ? C54 C55 C56 107(4) 12_655 . ? C54 C55 C56 107(4) . . ? C57 C55 N1 68(7) 12_655 . ? C57 C55 N1 146(8) . . ? C54 C55 N1 68(6) 12_655 . ? C54 C55 N1 138(7) . . ? C56 C55 N1 113(4) . . ? C57 C55 N1 146(8) 12_655 9_665 ? C57 C55 N1 68(7) . 9_665 ? C54 C55 N1 138(7) 12_655 9_665 ? C54 C55 N1 68(6) . 9_665 ? C56 C55 N1 113(4) . 9_665 ? N1 C55 N1 85(10) . 9_665 ? C55 C56 C57 55(4) . 12_655 ? C55 C56 C57 55(4) . . ? C57 C56 C57 110(8) 12_655 . ? C54 C57 C55 69(5) . . ? C54 C57 C56 121(8) . . ? C55 C57 C56 60(5) . . ? C54 C57 N1 72(5) . 9_665 ? C55 C57 N1 66(9) . 9_665 ? C56 C57 N1 109(10) . 9_665 ? 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 Cr2 F1 Ni2 142.3(8) . . . 12_655 ? O9 Cr2 F1 Ni2 52.6(9) . . . 12_655 ? O8 Cr2 F1 Ni2 -125.8(9) . . . 12_655 ? O10 Cr2 F1 Ni2 -37.8(10) . . . 12_655 ? O6 Cr2 F1 Ni2 -23(5) . . . 12_655 ? F2 Cr2 F1 Cr2 142.3(8) . . . 12_655 ? O9 Cr2 F1 Cr2 52.6(9) . . . 12_655 ? O8 Cr2 F1 Cr2 -125.8(9) . . . 12_655 ? O10 Cr2 F1 Cr2 -37.8(10) . . . 12_655 ? O6 Cr2 F1 Cr2 -23(5) . . . 12_655 ? F1 Cr2 F2 Ni1 140.0(7) . . . . ? O9 Cr2 F2 Ni1 -129.4(7) . . . . ? O8 Cr2 F2 Ni1 49.7(8) . . . . ? O10 Cr2 F2 Ni1 -39(4) . . . . ? O6 Cr2 F2 Ni1 -42.5(9) . . . . ? F3 Ni1 F2 Cr2 -142.4(6) . . . . ? O5 Ni1 F2 Cr2 38.8(9) . . . . ? O4 Ni1 F2 Cr2 126.2(8) . . . . ? O7 Ni1 F2 Cr2 -54.2(8) . . . . ? O2 Ni1 F2 Cr2 4(6) . . . . ? F2 Ni1 F3 Cr3 -138.3(6) . . . . ? O5 Ni1 F3 Cr3 33(6) . . . . ? O4 Ni1 F3 Cr3 -48.2(8) . . . . ? O7 Ni1 F3 Cr3 130.3(7) . . . . ? O2 Ni1 F3 Cr3 45.8(8) . . . . ? F3 Cr3 F3 Ni1 139.5(7) 4_565 . . . ? O1 Cr3 F3 Ni1 -18(6) 4_565 . . . ? O1 Cr3 F3 Ni1 -43.3(9) . . . . ? O3 Cr3 F3 Ni1 50.7(7) . . . . ? O3 Cr3 F3 Ni1 -129.7(7) 4_565 . . . ? F3 Cr3 O1 C1 15(3) . . . . ? F3 Cr3 O1 C1 173(4) 4_565 . . . ? O1 Cr3 O1 C1 -161(4) 4_565 . . . ? O3 Cr3 O1 C1 -76(3) . . . . ? O3 Cr3 O1 C1 104(3) 4_565 . . . ? F3 Ni1 O2 C1 -25(4) . . . . ? F2 Ni1 O2 C1 -172(4) . . . . ? O5 Ni1 O2 C1 153(4) . . . . ? O4 Ni1 O2 C1 66(4) . . . . ? O7 Ni1 O2 C1 -113(4) . . . . ? F3 Cr3 O3 C6 -19(3) . . . . ? F3 Cr3 O3 C6 -111(3) 4_565 . . . ? O1 Cr3 O3 C6 154(3) 4_565 . . . ? O1 Cr3 O3 C6 76(3) . . . . ? O3 Cr3 O3 C6 -65(3) 4_565 . . . ? F3 Ni1 O4 C6 9(3) . . . . ? F2 Ni1 O4 C6 103(3) . . . . ? O5 Ni1 O4 C6 -163(3) . . . . ? O7 Ni1 O4 C6 -59(33) . . . . ? O2 Ni1 O4 C6 -83(3) . . . . ? F3 Ni1 O5 C11 177(4) . . . . ? F2 Ni1 O5 C11 -12(4) . . . . ? O4 Ni1 O5 C11 -102(4) . . . . ? O7 Ni1 O5 C11 80(4) . . . . ? O2 Ni1 O5 C11 164(4) . . . . ? F2 Cr2 O6 C11 25(4) . . . . ? F1 Cr2 O6 C11 -170(4) . . . . ? O9 Cr2 O6 C11 115(4) . . . . ? O8 Cr2 O6 C11 -67(4) . . . . ? O10 Cr2 O6 C11 -154(4) . . . . ? F3 Ni1 O7 C16 122(2) . . . . ? F2 Ni1 O7 C16 28(2) . . . . ? O5 Ni1 O7 C16 -66(2) . . . . ? O4 Ni1 O7 C16 -170(100) . . . . ? O2 Ni1 O7 C16 -145(2) . . . . ? F2 Cr2 O8 C16 -16(2) . . . . ? F1 Cr2 O8 C16 -111(2) . . . . ? O9 Cr2 O8 C16 135(21) . . . . ? O10 Cr2 O8 C16 154(2) . . . . ? O6 Cr2 O8 C16 79(2) . . . . ? F2 Cr2 O9 C21 -109(3) . . . . ? F1 Cr2 O9 C21 -14(3) . . . . ? O8 Cr2 O9 C21 101(22) . . . . ? O10 Cr2 O9 C21 81(3) . . . . ? O6 Cr2 O9 C21 157(3) . . . . ? F2 Cr2 O10 C26 -176(4) . . . . ? F1 Cr2 O10 C26 4(4) . . . . ? O9 Cr2 O10 C26 -86(4) . . . . ? O8 Cr2 O10 C26 94(4) . . . . ? O6 Cr2 O10 C26 -173(4) . . . . ? Ni1 O2 C1 O1 0(6) . . . . ? Ni1 O2 C1 C2 178.1(19) . . . . ? Ni1 O2 C1 C2A -173(2) . . . . ? Cr3 O1 C1 O2 6(5) . . . . ? Cr3 O1 C1 C2 -171.6(18) . . . . ? Cr3 O1 C1 C2A -179(2) . . . . ? O2 C1 C2 C3 122(3) . . . . ? O1 C1 C2 C3 -60(3) . . . . ? C2A C1 C2 C3 -32(6) . . . . ? O2 C1 C2 C5 -120(3) . . . . ? O1 C1 C2 C5 59(3) . . . . ? C2A C1 C2 C5 86(7) . . . . ? O2 C1 C2 C4 2(4) . . . . ? O1 C1 C2 C4 180(2) . . . . ? C2A C1 C2 C4 -153(7) . . . . ? O2 C1 C2A C3A 163(4) . . . . ? O1 C1 C2A C3A -12(4) . . . . ? C2 C1 C2A C3A -167(8) . . . . ? O2 C1 C2A C5A -75(4) . . . . ? O1 C1 C2A C5A 110(3) . . . . ? C2 C1 C2A C5A -45(6) . . . . ? O2 C1 C2A C4A 39(5) . . . . ? O1 C1 C2A C4A -136(3) . . . . ? C2 C1 C2A C4A 69(6) . . . . ? Ni1 O4 C6 O3 21(5) . . . . ? Ni1 O4 C6 C7A -164(2) . . . . ? Ni1 O4 C6 C7 -170.4(18) . . . . ? Cr3 O3 C6 O4 -15(4) . . . . ? Cr3 O3 C6 C7A 169.6(19) . . . . ? Cr3 O3 C6 C7 178.1(14) . . . . ? O4 C6 C7 C10 -6(3) . . . . ? O3 C6 C7 C10 161(3) . . . . ? C7A C6 C7 C10 -166(6) . . . . ? O4 C6 C7 C9 114(3) . . . . ? O3 C6 C7 C9 -79(3) . . . . ? C7A C6 C7 C9 -46(6) . . . . ? O4 C6 C7 C8 -126(2) . . . . ? O3 C6 C7 C8 41(3) . . . . ? C7A C6 C7 C8 74(6) . . . . ? O4 C6 C7A C8A 171(3) . . . . ? O3 C6 C7A C8A -14(3) . . . . ? C7 C6 C7A C8A -165(6) . . . . ? O4 C6 C7A C10A -69(3) . . . . ? O3 C6 C7A C10A 106(3) . . . . ? C7 C6 C7A C10A -45(6) . . . . ? O4 C6 C7A C9A 51(3) . . . . ? O3 C6 C7A C9A -134(3) . . . . ? C7 C6 C7A C9A 75(6) . . . . ? Cr2 O6 C11 O5 -2(6) . . . . ? Cr2 O6 C11 C12 170.9(18) . . . . ? Cr2 O6 C11 C12A -173(3) . . . . ? Ni1 O5 C11 O6 -7(6) . . . . ? Ni1 O5 C11 C12 180(2) . . . . ? Ni1 O5 C11 C12A 161(3) . . . . ? O6 C11 C12 C15 4(4) . . . . ? O5 C11 C12 C15 177(3) . . . . ? C12A C11 C12 C15 -38(6) . . . . ? O6 C11 C12 C13 -115(4) . . . . ? O5 C11 C12 C13 58(3) . . . . ? C12A C11 C12 C13 -157(6) . . . . ? O6 C11 C12 C14 123(3) . . . . ? O5 C11 C12 C14 -64(3) . . . . ? C12A C11 C12 C14 81(6) . . . . ? O6 C11 C12A C13A 127(3) . . . . ? O5 C11 C12A C13A -42(5) . . . . ? C12 C11 C12A C13A -87(6) . . . . ? O6 C11 C12A C14A 4(4) . . . . ? O5 C11 C12A C14A -165(4) . . . . ? C12 C11 C12A C14A 150(7) . . . . ? O6 C11 C12A C15A -116(3) . . . . ? O5 C11 C12A C15A 75(5) . . . . ? C12 C11 C12A C15A 29(5) . . . . ? Ni1 O7 C16 O8 0(4) . . . . ? Ni1 O7 C16 C17 174.0(15) . . . . ? Ni1 O7 C16 C17A 172(2) . . . . ? Cr2 O8 C16 O7 -9(4) . . . . ? Cr2 O8 C16 C17 176.6(15) . . . . ? Cr2 O8 C16 C17A -177(3) . . . . ? O7 C16 C17 C20 19(3) . . . . ? O8 C16 C17 C20 -166.6(19) . . . . ? C17A C16 C17 C20 22(4) . . . . ? O7 C16 C17 C18 -98(2) . . . . ? O8 C16 C17 C18 77(2) . . . . ? C17A C16 C17 C18 -95(4) . . . . ? O7 C16 C17 C19 142(2) . . . . ? O8 C16 C17 C19 -43(2) . . . . ? C17A C16 C17 C19 145(5) . . . . ? O7 C16 C17A C19A 125(3) . . . . ? O8 C16 C17A C19A -64(5) . . . . ? C17 C16 C17A C19A -52(4) . . . . ? O7 C16 C17A C18A -117(3) . . . . ? O8 C16 C17A C18A 53(5) . . . . ? C17 C16 C17A C18A 65(4) . . . . ? O7 C16 C17A C20A 5(3) . . . . ? O8 C16 C17A C20A 175(4) . . . . ? C17 C16 C17A C20A -172(6) . . . . ? Cr2 O9 C21 O9 -19(5) . . . 12_655 ? Cr2 O9 C21 C22 162.8(18) . . . . ? O9 C21 C22 C24 -91(3) . . . . ? O9 C21 C22 C24 91(3) 12_655 . . . ? O9 C21 C22 C23 23(3) . . . . ? O9 C21 C22 C23 -155(3) 12_655 . . . ? O9 C21 C22 C23 155(3) . . . 12_655 ? O9 C21 C22 C23 -23(3) 12_655 . . 12_655 ? Cr2 O10 C26 O10 27(8) . . . 12_655 ? Cr2 O10 C26 C27 177(2) . . . . ? O10 C26 C27 C29 47(5) . . . 12_655 ? O10 C26 C27 C29 -163(4) 12_655 . . 12_655 ? O10 C26 C27 C29 163(4) . . . . ? O10 C26 C27 C29 -47(5) 12_655 . . . ? O10 C26 C27 C28 -75(4) . . . . ? O10 C26 C27 C28 75(4) 12_655 . . . ? C57 C54 C55 C57 98(11) . . . 12_655 ? N1 C54 C55 C57 178(11) 9_665 . . 12_655 ? N1 C54 C55 C57 80(6) 9_665 . . . ? C57 C54 C55 C54 146(6) . . . 12_655 ? N1 C54 C55 C54 -134(7) 9_665 . . 12_655 ? C57 C54 C55 C56 29(7) . . . . ? N1 C54 C55 C56 109(6) 9_665 . . . ? C57 C54 C55 N1 -133(11) . . . . ? N1 C54 C55 N1 -53(14) 9_665 . . . ? C57 C54 C55 N1 -80(6) . . . 9_665 ? C55 N1 C55 C57 -160(4) 9_665 . . 12_655 ? C57 N1 C55 C57 178(8) 9_665 . . 12_655 ? C54 N1 C55 C57 52(4) 12_655 . . 12_655 ? C54 N1 C55 C57 -126(10) 9_665 . . 12_655 ? C55 N1 C55 C57 -35(10) 9_665 . . . ? C57 N1 C55 C57 -56(10) 9_665 . . . ? C57 N1 C55 C57 125(13) 12_655 . . . ? C54 N1 C55 C57 178(11) 12_655 . . . ? C54 N1 C55 C57 -1(19) 9_665 . . . ? C55 N1 C55 C54 148(4) 9_665 . . 12_655 ? C57 N1 C55 C54 126(7) 9_665 . . 12_655 ? C57 N1 C55 C54 -52(4) 12_655 . . 12_655 ? C54 N1 C55 C54 -179(11) 9_665 . . 12_655 ? C55 N1 C55 C54 48(9) 9_665 . . . ? C57 N1 C55 C54 27(16) 9_665 . . . ? C57 N1 C55 C54 -152(10) 12_655 . . . ? C54 N1 C55 C54 -100(12) 12_655 . . . ? C54 N1 C55 C54 82(8) 9_665 . . . ? C55 N1 C55 C56 -113(6) 9_665 . . . ? C57 N1 C55 C56 -135(6) 9_665 . . . ? C57 N1 C55 C56 47(6) 12_655 . . . ? C54 N1 C55 C56 99(6) 12_655 . . . ? C54 N1 C55 C56 -79(14) 9_665 . . . ? C55 N1 C55 N1 -0.002(3) 9_665 . . 9_665 ? C57 N1 C55 N1 -22(8) 9_665 . . 9_665 ? C57 N1 C55 N1 160(4) 12_655 . . 9_665 ? C54 N1 C55 N1 -148(4) 12_655 . . 9_665 ? C54 N1 C55 N1 34(10) 9_665 . . 9_665 ? C57 C55 C56 C57 168(8) . . . 12_655 ? C54 C55 C56 C57 24(5) 12_655 . . 12_655 ? C54 C55 C56 C57 144(6) . . . 12_655 ? N1 C55 C56 C57 -49(9) . . . 12_655 ? N1 C55 C56 C57 -143(10) 9_665 . . 12_655 ? C57 C55 C56 C57 -168(8) 12_655 . . . ? C54 C55 C56 C57 -144(6) 12_655 . . . ? C54 C55 C56 C57 -24(5) . . . . ? N1 C55 C56 C57 143(10) . . . . ? N1 C55 C56 C57 49(9) 9_665 . . . ? N1 C54 C57 C55 -70(10) 9_665 . . . ? C55 C54 C57 C56 -32(7) . . . . ? N1 C54 C57 C56 -102(12) 9_665 . . . ? C55 C54 C57 N1 70(10) . . . 9_665 ? C57 C55 C57 C54 -135(7) 12_655 . . . ? C54 C55 C57 C54 -67(11) 12_655 . . . ? C56 C55 C57 C54 -149(7) . . . . ? N1 C55 C57 C54 117(12) . . . . ? N1 C55 C57 C54 79(5) 9_665 . . . ? C57 C55 C57 C56 14(9) 12_655 . . . ? C54 C55 C57 C56 82(11) 12_655 . . . ? C54 C55 C57 C56 149(7) . . . . ? N1 C55 C57 C56 -94(12) . . . . ? N1 C55 C57 C56 -132(6) 9_665 . . . ? C57 C55 C57 N1 145(8) 12_655 . . 9_665 ? C54 C55 C57 N1 -146(10) 12_655 . . 9_665 ? C54 C55 C57 N1 -79(5) . . . 9_665 ? C56 C55 C57 N1 132(6) . . . 9_665 ? N1 C55 C57 N1 38(13) . . . 9_665 ? C55 C56 C57 C54 34(8) . . . . ? C57 C56 C57 C54 24(13) 12_655 . . . ? C57 C56 C57 C55 -10(7) 12_655 . . . ? C55 C56 C57 N1 -46(6) . . . 9_665 ? C57 C56 C57 N1 -56(11) 12_655 . . 9_665 ? _diffrn_measured_fraction_theta_max .991 _diffrn_reflns_theta_full 16.52 _diffrn_measured_fraction_theta_full .991 _refine_diff_density_max .804 _refine_diff_density_min -.644 _refine_diff_density_rms .162 data_orepw200absc _database_code_depnum_ccdc_archive 'CCDC 268362' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89 H159 Cr6 F8 N4 Ni2 O32' _chemical_formula_weight 2378.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr .3209 .6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni .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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 24.9758(6) _cell_length_b 16.6444(5) _cell_length_c 31.0706(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.149(2) _cell_angle_gamma 90.00 _cell_volume 12046.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 19468 _cell_measurement_theta_min 2.6041 _cell_measurement_theta_max 32.0816 _exptl_crystal_description Prismatic _exptl_crystal_colour Green _exptl_crystal_size_max 0.23345 _exptl_crystal_size_mid 0.18056 _exptl_crystal_size_min 0.10184 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5096 _exptl_absorpt_coefficient_mu 0.906 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.65200 _exptl_absorpt_correction_T_max 0.84486 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.pre23_9 beta (release 18.06.2004 CrysAlis171 .NET) (compiled Jun 18 2004,12:34:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 87256 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.0866 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 26.37 _reflns_number_total 24575 _reflns_number_gt 15713 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++) (compiled Nov 6 2003,09:43:27) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Solvent molecule is on a symmetry position and disordered and was left isotropic. Modelling of solvent involved only constraining all C-C bonds to be equal for both parts of the disorder. 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^)+(0.0901P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24575 _refine_ls_number_parameters 1509 _refine_ls_number_restraints 1113 _refine_ls_R_factor_all 0.0989 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1692 _refine_ls_wR_factor_gt 0.1525 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.027 _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 Cr1 Cr 0.32645(3) 0.28099(4) 0.69924(2) 0.01902(15) Uani 0.75 1 d P . . Cr2 Cr 0.34904(3) 0.34168(4) 0.60323(2) 0.01782(15) Uani 0.75 1 d P . . Cr3 Cr 0.33348(3) 0.51830(4) 0.54500(2) 0.01993(15) Uani 0.75 1 d P . . Cr4 Cr 0.24740(3) 0.68214(4) 0.53339(2) 0.02031(15) Uani 0.75 1 d P . . Cr5 Cr 0.17566(3) 0.76246(4) 0.59799(2) 0.01980(15) Uani 0.75 1 d P . . Cr6 Cr 0.12086(3) 0.67681(4) 0.67236(2) 0.01735(15) Uani 0.75 1 d P . . Cr7 Cr 0.15669(3) 0.51423(4) 0.74310(2) 0.01995(15) Uani 0.75 1 d P . . Cr8 Cr 0.22630(3) 0.33817(4) 0.74313(2) 0.02058(15) Uani 0.75 1 d P . . Ni1 Ni 0.32645(3) 0.28099(4) 0.69924(2) 0.01902(15) Uani 0.25 1 d P . . Ni2 Ni 0.34904(3) 0.34168(4) 0.60323(2) 0.01782(15) Uani 0.25 1 d P . . Ni3 Ni 0.33348(3) 0.51830(4) 0.54500(2) 0.01993(15) Uani 0.25 1 d P . . Ni4 Ni 0.24740(3) 0.68214(4) 0.53339(2) 0.02031(15) Uani 0.25 1 d P . . Ni5 Ni 0.17566(3) 0.76246(4) 0.59799(2) 0.01980(15) Uani 0.25 1 d P . . Ni6 Ni 0.12086(3) 0.67681(4) 0.67236(2) 0.01735(15) Uani 0.25 1 d P . . Ni7 Ni 0.15669(3) 0.51423(4) 0.74310(2) 0.01995(15) Uani 0.25 1 d P . . Ni8 Ni 0.22630(3) 0.33817(4) 0.74313(2) 0.02058(15) Uani 0.25 1 d P . . F1 F 0.33696(10) 0.36575(14) 0.66027(8) 0.0247(6) Uani 1 1 d . . . F2 F 0.30503(10) 0.43670(14) 0.57559(8) 0.0247(6) Uani 1 1 d . . . F3 F 0.29658(10) 0.59850(14) 0.57040(8) 0.0242(6) Uani 1 1 d . . . F4 F 0.19992(10) 0.67050(14) 0.57011(8) 0.0245(6) Uani 1 1 d . . . F5 F 0.18359(10) 0.69306(14) 0.64986(8) 0.0229(5) Uani 1 1 d . . . F6 F 0.14625(10) 0.56552(14) 0.68475(8) 0.0231(5) Uani 1 1 d . . . F7 F 0.21909(10) 0.45396(14) 0.73531(8) 0.0225(5) Uani 1 1 d . . . F8 F 0.25513(10) 0.33539(14) 0.69356(8) 0.0216(5) Uani 1 1 d . . . O1 O 0.28342(12) 0.21044(17) 0.64611(10) 0.0231(7) Uani 1 1 d . A . O2 O 0.27664(14) 0.27869(19) 0.58247(11) 0.0339(8) Uani 1 1 d . A . O3 O 0.39930(13) 0.23197(18) 0.70301(10) 0.0279(7) Uani 1 1 d . . . O4 O 0.39460(12) 0.24518(17) 0.62992(10) 0.0239(7) Uani 1 1 d . . . O5 O 0.35861(13) 0.31684(18) 0.54484(10) 0.0274(7) Uani 1 1 d . . . O6 O 0.37131(12) 0.43844(17) 0.51866(10) 0.0236(7) Uani 1 1 d . . . O7 O 0.42242(12) 0.40172(17) 0.62580(10) 0.0225(7) Uani 1 1 d . B . O8 O 0.40249(13) 0.52905(18) 0.60176(11) 0.0323(8) Uani 1 1 d . B . O9 O 0.26466(12) 0.50680(17) 0.48794(10) 0.0240(7) Uani 1 1 d . C . O10 O 0.20193(12) 0.60197(19) 0.48872(10) 0.0302(8) Uani 1 1 d . C . O11 O 0.36539(13) 0.60329(18) 0.51757(11) 0.0273(7) Uani 1 1 d . . . O12 O 0.29722(12) 0.69799(18) 0.49768(10) 0.0258(7) Uani 1 1 d . . . O13 O 0.19630(13) 0.76440(18) 0.49558(10) 0.0271(7) Uani 1 1 d . D . O14 O 0.16734(13) 0.83320(17) 0.54478(11) 0.0253(7) Uani 1 1 d . D . O15 O 0.29578(12) 0.76191(17) 0.57722(10) 0.0224(7) Uani 1 1 d . . . O16 O 0.25678(13) 0.79398(18) 0.62952(11) 0.0291(7) Uani 1 1 d . . . O17 O 0.09346(12) 0.73290(17) 0.56451(10) 0.0226(7) Uani 1 1 d . . . O18 O 0.07198(13) 0.64225(19) 0.60881(10) 0.0324(8) Uani 1 1 d . . . O19 O 0.15023(13) 0.85192(17) 0.62686(11) 0.0276(7) Uani 1 1 d . E . O20 O 0.09409(13) 0.78867(17) 0.65852(10) 0.0256(7) Uani 1 1 d . E . O21 O 0.05607(13) 0.65770(19) 0.69270(11) 0.0295(7) Uani 1 1 d . . . O22 O 0.09297(13) 0.57179(18) 0.75160(10) 0.0251(7) Uani 1 1 d . . . O23 O 0.17208(13) 0.71055(18) 0.73512(10) 0.0266(7) Uani 1 1 d . . . O24 O 0.21121(14) 0.59936(19) 0.77484(10) 0.0335(8) Uani 1 1 d . . . O25 O 0.10088(12) 0.43148(17) 0.70827(10) 0.0231(7) Uani 1 1 d . . . O26 O 0.14931(12) 0.32587(17) 0.69623(10) 0.0236(7) Uani 1 1 d . . . O27 O 0.16940(13) 0.46197(18) 0.80262(10) 0.0285(7) Uani 1 1 d . . . O28 O 0.19702(13) 0.33779(17) 0.79389(10) 0.0240(7) Uani 1 1 d . . . O29 O 0.23325(12) 0.22215(17) 0.75027(10) 0.0242(7) Uani 1 1 d . . . O30 O 0.31555(12) 0.19517(17) 0.73982(10) 0.0240(7) Uani 1 1 d . . . O31 O 0.30446(12) 0.35251(16) 0.79054(9) 0.0195(6) Uani 1 1 d . . . O32 O 0.36736(12) 0.34737(19) 0.75414(10) 0.0285(7) Uani 1 1 d . . . C1 C 0.26635(18) 0.2195(3) 0.60286(15) 0.0241(10) Uani 1 1 d D . . C2 C 0.2366(5) 0.1497(9) 0.5731(5) 0.0449(18) Uani 0.50 1 d PDU A 1 C3 C 0.2305(5) 0.0790(6) 0.6017(4) 0.053(3) Uani 0.50 1 d PDU A 1 H3A H 0.2678 0.0626 0.6223 0.079 Uiso 0.50 1 calc PR A 1 H3B H 0.2124 0.0351 0.5817 0.079 Uiso 0.50 1 calc PR A 1 H3C H 0.2074 0.0944 0.6192 0.079 Uiso 0.50 1 calc PR A 1 C4 C 0.2769(5) 0.1230(7) 0.5473(4) 0.061(2) Uani 0.50 1 d PDU A 1 H4A H 0.2824 0.1671 0.5294 0.092 Uiso 0.50 1 calc PR A 1 H4B H 0.2598 0.0787 0.5272 0.092 Uiso 0.50 1 calc PR A 1 H4C H 0.3133 0.1067 0.5694 0.092 Uiso 0.50 1 calc PR A 1 C5 C 0.1806(4) 0.1784(7) 0.5383(4) 0.072(3) Uani 0.50 1 d PDU A 1 H5A H 0.1581 0.2030 0.5541 0.109 Uiso 0.50 1 calc PR A 1 H5B H 0.1599 0.1337 0.5205 0.109 Uiso 0.50 1 calc PR A 1 H5C H 0.1880 0.2170 0.5182 0.109 Uiso 0.50 1 calc PR A 1 C2A C 0.2237(5) 0.1542(8) 0.5742(4) 0.0412(17) Uani 0.50 1 d PDU A 2 C3A C 0.2490(5) 0.0726(5) 0.5929(4) 0.049(3) Uani 0.50 1 d PDU A 2 H3A1 H 0.2223 0.0311 0.5773 0.074 Uiso 0.50 1 calc PR A 2 H3A2 H 0.2564 0.0702 0.6254 0.074 Uiso 0.50 1 calc PR A 2 H3A3 H 0.2842 0.0651 0.5876 0.074 Uiso 0.50 1 calc PR A 2 C4A C 0.2120(5) 0.1648(7) 0.5230(3) 0.053(2) Uani 0.50 1 d PDU A 2 H4A1 H 0.2472 0.1588 0.5174 0.080 Uiso 0.50 1 calc PR A 2 H4A2 H 0.1964 0.2173 0.5134 0.080 Uiso 0.50 1 calc PR A 2 H4A3 H 0.1850 0.1249 0.5058 0.080 Uiso 0.50 1 calc PR A 2 C5A C 0.1677(4) 0.1678(6) 0.5827(4) 0.050(2) Uani 0.50 1 d PDU A 2 H5A1 H 0.1545 0.2217 0.5741 0.075 Uiso 0.50 1 calc PR A 2 H5A2 H 0.1743 0.1598 0.6148 0.075 Uiso 0.50 1 calc PR A 2 H5A3 H 0.1392 0.1305 0.5646 0.075 Uiso 0.50 1 calc PR A 2 C6 C 0.41664(18) 0.2182(3) 0.67049(15) 0.0226(10) Uani 1 1 d . . . C7 C 0.4680(2) 0.1615(3) 0.68125(17) 0.0325(11) Uani 1 1 d . . . C8 C 0.4468(3) 0.0796(3) 0.6890(3) 0.076(2) Uani 1 1 d . . . H8A H 0.4307 0.0832 0.7127 0.114 Uiso 1 1 calc R . . H8B H 0.4783 0.0424 0.6984 0.114 Uiso 1 1 calc R . . H8C H 0.4179 0.0612 0.6609 0.114 Uiso 1 1 calc R . . C9 C 0.5146(2) 0.1892(4) 0.7246(2) 0.0559(17) Uani 1 1 d . . . H9A H 0.5281 0.2411 0.7195 0.084 Uiso 1 1 calc R . . H9B H 0.5458 0.1515 0.7329 0.084 Uiso 1 1 calc R . . H9C H 0.4998 0.1927 0.7490 0.084 Uiso 1 1 calc R . . C10 C 0.4894(3) 0.1604(5) 0.6417(2) 0.081(3) Uani 1 1 d . . . H10A H 0.4593 0.1418 0.6143 0.122 Uiso 1 1 calc R . . H10B H 0.5218 0.1250 0.6489 0.122 Uiso 1 1 calc R . . H10C H 0.5006 0.2136 0.6366 0.122 Uiso 1 1 calc R . . C11 C 0.37118(17) 0.3626(3) 0.51762(14) 0.0211(9) Uani 1 1 d . . . C12 C 0.38605(19) 0.3216(3) 0.47944(15) 0.0265(10) Uani 1 1 d . . . C13 C 0.3300(2) 0.2937(4) 0.44422(18) 0.0470(15) Uani 1 1 d . . . H13A H 0.3121 0.2562 0.4583 0.071 Uiso 1 1 calc R . . H13B H 0.3370 0.2682 0.4191 0.071 Uiso 1 1 calc R . . H13C H 0.3051 0.3391 0.4329 0.071 Uiso 1 1 calc R . . C14 C 0.4237(2) 0.2486(3) 0.49953(19) 0.0463(14) Uani 1 1 d . . . H14A H 0.4033 0.2117 0.5118 0.069 Uiso 1 1 calc R . . H14B H 0.4583 0.2656 0.5237 0.069 Uiso 1 1 calc R . . H14C H 0.4334 0.2225 0.4757 0.069 Uiso 1 1 calc R . . C15 C 0.4158(2) 0.3795(3) 0.45761(18) 0.0429(14) Uani 1 1 d . . . H15A H 0.4243 0.3526 0.4335 0.064 Uiso 1 1 calc R . . H15B H 0.4509 0.3980 0.4806 0.064 Uiso 1 1 calc R . . H15C H 0.3912 0.4246 0.4449 0.064 Uiso 1 1 calc R . . C16 C 0.43582(18) 0.4739(3) 0.62432(14) 0.0216(9) Uani 1 1 d . . . C17 C 0.4981(9) 0.4973(10) 0.6520(6) 0.0406(16) Uani 0.50 1 d PDU B 1 C18 C 0.5145(6) 0.4602(8) 0.7002(4) 0.057(3) Uani 0.50 1 d PDU B 1 H18A H 0.5533 0.4747 0.7184 0.086 Uiso 0.50 1 calc PR B 1 H18B H 0.5114 0.4028 0.6975 0.086 Uiso 0.50 1 calc PR B 1 H18C H 0.4892 0.4799 0.7147 0.086 Uiso 0.50 1 calc PR B 1 C19 C 0.5078(12) 0.5878(9) 0.6555(7) 0.043(3) Uani 0.50 1 d PDU B 1 H19A H 0.4853 0.6114 0.6716 0.064 Uiso 0.50 1 calc PR B 1 H19B H 0.4965 0.6103 0.6251 0.064 Uiso 0.50 1 calc PR B 1 H19C H 0.5477 0.5986 0.6721 0.064 Uiso 0.50 1 calc PR B 1 C20 C 0.5363(5) 0.4605(8) 0.6282(5) 0.058(2) Uani 0.50 1 d PDU B 1 H20A H 0.5239 0.4789 0.5969 0.087 Uiso 0.50 1 calc PR B 1 H20B H 0.5337 0.4030 0.6287 0.087 Uiso 0.50 1 calc PR B 1 H20C H 0.5754 0.4766 0.6443 0.087 Uiso 0.50 1 calc PR B 1 C17A C 0.4983(9) 0.4986(10) 0.6472(5) 0.0390(16) Uani 0.50 1 d PDU B 2 C18A C 0.5319(5) 0.4415(7) 0.6851(4) 0.049(2) Uani 0.50 1 d PDU B 2 H18D H 0.5150 0.4399 0.7084 0.073 Uiso 0.50 1 calc PR B 2 H18E H 0.5709 0.4596 0.6986 0.073 Uiso 0.50 1 calc PR B 2 H18F H 0.5311 0.3887 0.6725 0.073 Uiso 0.50 1 calc PR B 2 C19A C 0.5017(12) 0.5848(9) 0.6638(7) 0.044(3) Uani 0.50 1 d PDU B 2 H19D H 0.4912 0.6204 0.6378 0.066 Uiso 0.50 1 calc PR B 2 H19E H 0.5402 0.5964 0.6841 0.066 Uiso 0.50 1 calc PR B 2 H19F H 0.4759 0.5920 0.6801 0.066 Uiso 0.50 1 calc PR B 2 C20A C 0.5231(5) 0.4917(8) 0.6083(4) 0.048(2) Uani 0.50 1 d PDU B 2 H20D H 0.5200 0.4372 0.5976 0.071 Uiso 0.50 1 calc PR B 2 H20E H 0.5628 0.5074 0.6200 0.071 Uiso 0.50 1 calc PR B 2 H20F H 0.5020 0.5263 0.5831 0.071 Uiso 0.50 1 calc PR B 2 C21 C 0.21776(18) 0.5426(3) 0.47076(15) 0.0217(9) Uani 1 1 d . . . C22 C 0.1761(8) 0.5131(8) 0.4250(7) 0.0404(16) Uani 0.50 1 d PDU C 1 C23 C 0.1914(6) 0.5572(8) 0.3888(4) 0.064(3) Uani 0.50 1 d PDU C 1 H23A H 0.1929 0.6138 0.3950 0.097 Uiso 0.50 1 calc PR C 1 H23B H 0.1629 0.5467 0.3590 0.097 Uiso 0.50 1 calc PR C 1 H23C H 0.2282 0.5392 0.3894 0.097 Uiso 0.50 1 calc PR C 1 C24 C 0.1144(6) 0.5339(8) 0.4201(5) 0.054(2) Uani 0.50 1 d PDU C 1 H24A H 0.1089 0.5218 0.4485 0.080 Uiso 0.50 1 calc PR C 1 H24B H 0.0880 0.5029 0.3955 0.080 Uiso 0.50 1 calc PR C 1 H24C H 0.1076 0.5901 0.4134 0.080 Uiso 0.50 1 calc PR C 1 C25 C 0.1785(5) 0.4222(6) 0.4214(4) 0.047(2) Uani 0.50 1 d PDU C 1 H25A H 0.2132 0.4071 0.4169 0.071 Uiso 0.50 1 calc PR C 1 H25B H 0.1460 0.4038 0.3958 0.071 Uiso 0.50 1 calc PR C 1 H25C H 0.1778 0.3983 0.4493 0.071 Uiso 0.50 1 calc PR C 1 C22A C 0.1755(8) 0.5191(8) 0.4231(7) 0.0382(16) Uani 0.50 1 d PDU C 2 C23A C 0.1681(5) 0.5911(7) 0.3904(4) 0.048(2) Uani 0.50 1 d PDU C 2 H23D H 0.1491 0.6341 0.3998 0.072 Uiso 0.50 1 calc PR C 2 H23E H 0.1454 0.5753 0.3595 0.072 Uiso 0.50 1 calc PR C 2 H23F H 0.2051 0.6090 0.3915 0.072 Uiso 0.50 1 calc PR C 2 C24A C 0.1173(5) 0.5017(7) 0.4274(5) 0.044(2) Uani 0.50 1 d PDU C 2 H24D H 0.1202 0.4542 0.4456 0.065 Uiso 0.50 1 calc PR C 2 H24E H 0.0888 0.4937 0.3972 0.065 Uiso 0.50 1 calc PR C 2 H24F H 0.1064 0.5464 0.4420 0.065 Uiso 0.50 1 calc PR C 2 C25A C 0.1944(6) 0.4445(7) 0.4050(4) 0.056(3) Uani 0.50 1 d PDU C 2 H25D H 0.2270 0.4568 0.3968 0.083 Uiso 0.50 1 calc PR C 2 H25E H 0.1636 0.4254 0.3783 0.083 Uiso 0.50 1 calc PR C 2 H25F H 0.2046 0.4037 0.4285 0.083 Uiso 0.50 1 calc PR C 2 C26 C 0.34615(18) 0.6703(3) 0.50133(14) 0.0222(10) Uani 1 1 d . . . C27 C 0.3851(2) 0.7238(3) 0.48549(16) 0.0292(11) Uani 1 1 d . . . C28 C 0.4387(2) 0.7397(3) 0.52755(17) 0.0361(12) Uani 1 1 d . . . H28A H 0.4281 0.7652 0.5510 0.054 Uiso 1 1 calc R . . H28B H 0.4641 0.7742 0.5191 0.054 Uiso 1 1 calc R . . H28C H 0.4577 0.6898 0.5391 0.054 Uiso 1 1 calc R . . C29 C 0.3561(2) 0.8034(3) 0.46633(19) 0.0398(13) Uani 1 1 d . . . H29A H 0.3214 0.7934 0.4406 0.060 Uiso 1 1 calc R . . H29B H 0.3815 0.8356 0.4565 0.060 Uiso 1 1 calc R . . H29C H 0.3473 0.8315 0.4899 0.060 Uiso 1 1 calc R . . C30 C 0.4000(2) 0.6777(3) 0.44853(18) 0.0419(13) Uani 1 1 d . . . H30A H 0.4191 0.6284 0.4614 0.063 Uiso 1 1 calc R . . H30B H 0.4249 0.7099 0.4381 0.063 Uiso 1 1 calc R . . H30C H 0.3654 0.6659 0.4229 0.063 Uiso 1 1 calc R . . C31 C 0.17085(18) 0.8220(2) 0.50604(15) 0.0213(9) Uani 1 1 d . . . C32 C 0.1442(7) 0.8851(13) 0.4692(7) 0.0373(15) Uani 0.50 1 d PDU D 1 C33 C 0.0994(6) 0.9337(10) 0.4806(6) 0.048(2) Uani 0.50 1 d PDU D 1 H33A H 0.0659 0.9013 0.4755 0.071 Uiso 0.50 1 calc PR D 1 H33B H 0.0893 0.9804 0.4612 0.071 Uiso 0.50 1 calc PR D 1 H33C H 0.1149 0.9501 0.5124 0.071 Uiso 0.50 1 calc PR D 1 C34 C 0.1196(6) 0.8468(9) 0.4220(5) 0.048(3) Uani 0.50 1 d PDU D 1 H34A H 0.1499 0.8226 0.4144 0.071 Uiso 0.50 1 calc PR D 1 H34B H 0.1009 0.8871 0.3995 0.071 Uiso 0.50 1 calc PR D 1 H34C H 0.0922 0.8063 0.4221 0.071 Uiso 0.50 1 calc PR D 1 C35 C 0.1957(6) 0.9382(10) 0.4723(4) 0.050(3) Uani 0.50 1 d PDU D 1 H35A H 0.2122 0.9601 0.5028 0.074 Uiso 0.50 1 calc PR D 1 H35B H 0.1832 0.9811 0.4503 0.074 Uiso 0.50 1 calc PR D 1 H35C H 0.2240 0.9064 0.4657 0.074 Uiso 0.50 1 calc PR D 1 C32A C 0.1431(7) 0.8824(12) 0.4681(7) 0.0377(15) Uani 0.50 1 d PDU D 2 C33A C 0.1154(6) 0.9504(10) 0.4851(6) 0.049(3) Uani 0.50 1 d PDU D 2 H33D H 0.0872 0.9289 0.4963 0.073 Uiso 0.50 1 calc PR D 2 H33E H 0.0972 0.9869 0.4601 0.073 Uiso 0.50 1 calc PR D 2 H33F H 0.1442 0.9785 0.5096 0.073 Uiso 0.50 1 calc PR D 2 C34A C 0.0995(6) 0.8390(9) 0.4279(5) 0.050(3) Uani 0.50 1 d PDU D 2 H34D H 0.1176 0.7943 0.4190 0.075 Uiso 0.50 1 calc PR D 2 H34E H 0.0846 0.8753 0.4023 0.075 Uiso 0.50 1 calc PR D 2 H34F H 0.0688 0.8199 0.4367 0.075 Uiso 0.50 1 calc PR D 2 C35A C 0.1906(6) 0.9200(10) 0.4549(4) 0.051(2) Uani 0.50 1 d PDU D 2 H35D H 0.2187 0.9439 0.4816 0.076 Uiso 0.50 1 calc PR D 2 H35E H 0.1745 0.9605 0.4318 0.076 Uiso 0.50 1 calc PR D 2 H35F H 0.2086 0.8793 0.4428 0.076 Uiso 0.50 1 calc PR D 2 C36 C 0.29709(19) 0.7939(2) 0.61423(15) 0.0229(10) Uani 1 1 d . . . C37 C 0.3530(2) 0.8357(3) 0.64273(17) 0.0338(12) Uani 1 1 d . . . C38 C 0.3480(3) 0.8802(4) 0.6830(2) 0.067(2) Uani 1 1 d . . . H38A H 0.3162 0.9167 0.6724 0.100 Uiso 1 1 calc R . . H38B H 0.3827 0.9099 0.6982 0.100 Uiso 1 1 calc R . . H38C H 0.3421 0.8427 0.7043 0.100 Uiso 1 1 calc R . . C39 C 0.3694(2) 0.8942(3) 0.6111(2) 0.0482(15) Uani 1 1 d . . . H39A H 0.3398 0.9340 0.5994 0.072 Uiso 1 1 calc R . . H39B H 0.3735 0.8650 0.5858 0.072 Uiso 1 1 calc R . . H39C H 0.4050 0.9201 0.6284 0.072 Uiso 1 1 calc R . . C40 C 0.3990(2) 0.7704(4) 0.6585(2) 0.0554(17) Uani 1 1 d . . . H40A H 0.4353 0.7944 0.6759 0.083 Uiso 1 1 calc R . . H40B H 0.4016 0.7435 0.6320 0.083 Uiso 1 1 calc R . . H40C H 0.3889 0.7323 0.6775 0.083 Uiso 1 1 calc R . . C41 C 0.05950(19) 0.6868(2) 0.57379(14) 0.0218(9) Uani 1 1 d . . . C42 C -0.0024(2) 0.6824(3) 0.53983(16) 0.0309(11) Uani 1 1 d . . . C43 C -0.0424(2) 0.6988(4) 0.5666(2) 0.0565(17) Uani 1 1 d . . . H43A H -0.0346 0.6607 0.5913 0.085 Uiso 1 1 calc R . . H43B H -0.0816 0.6937 0.5462 0.085 Uiso 1 1 calc R . . H43C H -0.0358 0.7522 0.5791 0.085 Uiso 1 1 calc R . . C44 C -0.0124(3) 0.5965(3) 0.52058(19) 0.0502(15) Uani 1 1 d . . . H44A H 0.0131 0.5857 0.5045 0.075 Uiso 1 1 calc R . . H44B H -0.0514 0.5912 0.4997 0.075 Uiso 1 1 calc R . . H44C H -0.0053 0.5591 0.5455 0.075 Uiso 1 1 calc R . . C45 C -0.0132(2) 0.7427(3) 0.50072(18) 0.0458(15) Uani 1 1 d . . . H45A H -0.0101 0.7963 0.5128 0.069 Uiso 1 1 calc R . . H45B H -0.0510 0.7347 0.4782 0.069 Uiso 1 1 calc R . . H45C H 0.0147 0.7352 0.4864 0.069 Uiso 1 1 calc R . . C46 C 0.11273(19) 0.8505(3) 0.64507(16) 0.0268(10) Uani 1 1 d . . . C47 C 0.0871(8) 0.9284(16) 0.6535(7) 0.0420(19) Uani 0.50 1 d PDU E 1 C48 C 0.0223(6) 0.9250(10) 0.6332(5) 0.055(3) Uani 0.50 1 d PDU E 1 H48A H 0.0089 0.8828 0.6478 0.082 Uiso 0.50 1 calc PR E 1 H48B H 0.0100 0.9147 0.6007 0.082 Uiso 0.50 1 calc PR E 1 H48C H 0.0068 0.9754 0.6382 0.082 Uiso 0.50 1 calc PR E 1 C49 C 0.1216(7) 0.9969(14) 0.6469(7) 0.051(3) Uani 0.50 1 d PDU E 1 H49A H 0.1604 0.9921 0.6683 0.077 Uiso 0.50 1 calc PR E 1 H49B H 0.1055 1.0465 0.6524 0.077 Uiso 0.50 1 calc PR E 1 H49C H 0.1212 0.9963 0.6159 0.077 Uiso 0.50 1 calc PR E 1 C50 C 0.1013(6) 0.9342(13) 0.7074(6) 0.054(3) Uani 0.50 1 d PDU E 1 H50A H 0.0826 0.8911 0.7170 0.080 Uiso 0.50 1 calc PR E 1 H50B H 0.0879 0.9847 0.7146 0.080 Uiso 0.50 1 calc PR E 1 H50C H 0.1420 0.9303 0.7234 0.080 Uiso 0.50 1 calc PR E 1 C47A C 0.0841(8) 0.9303(16) 0.6481(7) 0.0394(19) Uani 0.50 1 d PDU E 2 C48A C 0.0233(7) 0.9279(11) 0.6128(5) 0.051(3) Uani 0.50 1 d PDU E 2 H48D H 0.0026 0.9743 0.6165 0.077 Uiso 0.50 1 calc PR E 2 H48E H 0.0044 0.8801 0.6172 0.077 Uiso 0.50 1 calc PR E 2 H48F H 0.0246 0.9278 0.5822 0.077 Uiso 0.50 1 calc PR E 2 C49A C 0.1101(7) 1.0031(15) 0.6347(7) 0.050(3) Uani 0.50 1 d PDU E 2 H49D H 0.1512 1.0007 0.6491 0.075 Uiso 0.50 1 calc PR E 2 H49E H 0.0963 1.0507 0.6448 0.075 Uiso 0.50 1 calc PR E 2 H49F H 0.0995 1.0046 0.6018 0.075 Uiso 0.50 1 calc PR E 2 C50A C 0.0803(6) 0.9390(12) 0.6965(5) 0.049(3) Uani 0.50 1 d PDU E 2 H50D H 0.1161 0.9232 0.7196 0.074 Uiso 0.50 1 calc PR E 2 H50E H 0.0501 0.9051 0.6985 0.074 Uiso 0.50 1 calc PR E 2 H50F H 0.0722 0.9939 0.7014 0.074 Uiso 0.50 1 calc PR E 2 C51 C 0.05456(18) 0.6185(3) 0.72662(15) 0.0222(10) Uani 1 1 d . . . C52 C 0.0007(2) 0.6273(3) 0.73871(16) 0.0309(11) Uani 1 1 d . . . C53 C 0.0166(2) 0.6205(3) 0.79073(16) 0.0333(12) Uani 1 1 d . . . H53A H 0.0420 0.6635 0.8057 0.050 Uiso 1 1 calc R . . H53B H 0.0353 0.5699 0.8012 0.050 Uiso 1 1 calc R . . H53C H -0.0176 0.6236 0.7980 0.050 Uiso 1 1 calc R . . C54 C -0.0384(3) 0.5589(5) 0.7147(2) 0.074(2) Uani 1 1 d . . . H54A H -0.0181 0.5089 0.7235 0.112 Uiso 1 1 calc R . . H54B H -0.0502 0.5656 0.6819 0.112 Uiso 1 1 calc R . . H54C H -0.0715 0.5586 0.7234 0.112 Uiso 1 1 calc R . . C55 C -0.0282(3) 0.7069(4) 0.7210(2) 0.063(2) Uani 1 1 d . . . H55A H -0.0615 0.7125 0.7292 0.094 Uiso 1 1 calc R . . H55B H -0.0394 0.7088 0.6880 0.094 Uiso 1 1 calc R . . H55C H -0.0019 0.7500 0.7345 0.094 Uiso 1 1 calc R . . C56 C 0.2061(2) 0.6745(3) 0.76980(16) 0.0279(11) Uani 1 1 d . . . C57 C 0.2423(2) 0.7258(3) 0.81039(18) 0.0424(14) Uani 1 1 d . . . C58 C 0.2152(3) 0.7173(4) 0.84714(19) 0.0611(18) Uani 1 1 d . . . H58A H 0.2356 0.7504 0.8732 0.092 Uiso 1 1 calc R . . H58B H 0.2171 0.6622 0.8567 0.092 Uiso 1 1 calc R . . H58C H 0.1758 0.7341 0.8345 0.092 Uiso 1 1 calc R . . C59 C 0.2411(3) 0.8127(4) 0.7971(2) 0.082(2) Uani 1 1 d . . . H59A H 0.2587 0.8187 0.7744 0.123 Uiso 1 1 calc R . . H59B H 0.2618 0.8441 0.8239 0.123 Uiso 1 1 calc R . . H59C H 0.2020 0.8310 0.7844 0.123 Uiso 1 1 calc R . . C60 C 0.3037(2) 0.6925(4) 0.8289(2) 0.0561(17) Uani 1 1 d . . . H60A H 0.3197 0.6949 0.8051 0.084 Uiso 1 1 calc R . . H60B H 0.3030 0.6378 0.8384 0.084 Uiso 1 1 calc R . . H60C H 0.3267 0.7241 0.8549 0.084 Uiso 1 1 calc R . . C61 C 0.10447(18) 0.3663(3) 0.68876(14) 0.0220(10) Uani 1 1 d . . . C62 C 0.04967(19) 0.3364(3) 0.65055(16) 0.0290(11) Uani 1 1 d . . . C63 C 0.0580(2) 0.2508(3) 0.6371(2) 0.0479(15) Uani 1 1 d . . . H63A H 0.0880 0.2497 0.6246 0.072 Uiso 1 1 calc R . . H63B H 0.0229 0.2317 0.6143 0.072 Uiso 1 1 calc R . . H63C H 0.0684 0.2169 0.6639 0.072 Uiso 1 1 calc R . . C64 C 0.0376(2) 0.3942(4) 0.60939(18) 0.0494(15) Uani 1 1 d . . . H64A H 0.0350 0.4482 0.6193 0.074 Uiso 1 1 calc R . . H64B H 0.0020 0.3797 0.5856 0.074 Uiso 1 1 calc R . . H64C H 0.0681 0.3907 0.5976 0.074 Uiso 1 1 calc R . . C65 C 0.0003(2) 0.3402(3) 0.66798(19) 0.0405(13) Uani 1 1 d . . . H65A H 0.0106 0.3120 0.6968 0.061 Uiso 1 1 calc R . . H65B H -0.0331 0.3156 0.6458 0.061 Uiso 1 1 calc R . . H65C H -0.0080 0.3953 0.6724 0.061 Uiso 1 1 calc R . . C66 C 0.18136(18) 0.3907(3) 0.81546(14) 0.0219(10) Uani 1 1 d . . . C67 C 0.17898(19) 0.3678(3) 0.86215(14) 0.0238(10) Uani 1 1 d . . . C68 C 0.1822(2) 0.2775(3) 0.86883(17) 0.0362(12) Uani 1 1 d . . . H68A H 0.1494 0.2529 0.8460 0.054 Uiso 1 1 calc R . . H68B H 0.1824 0.2649 0.8990 0.054 Uiso 1 1 calc R . . H68C H 0.2167 0.2576 0.8657 0.054 Uiso 1 1 calc R . . C69 C 0.1228(2) 0.4001(3) 0.86552(17) 0.0368(12) Uani 1 1 d . . . H69A H 0.1222 0.4577 0.8632 0.055 Uiso 1 1 calc R . . H69B H 0.1206 0.3848 0.8946 0.055 Uiso 1 1 calc R . . H69C H 0.0907 0.3782 0.8409 0.055 Uiso 1 1 calc R . . C70 C 0.2309(2) 0.4073(3) 0.89851(15) 0.0333(12) Uani 1 1 d . . . H70A H 0.2654 0.3885 0.8950 0.050 Uiso 1 1 calc R . . H70B H 0.2317 0.3936 0.9287 0.050 Uiso 1 1 calc R . . H70C H 0.2283 0.4646 0.8946 0.050 Uiso 1 1 calc R . . C71 C 0.27493(19) 0.1774(3) 0.75233(14) 0.0231(10) Uani 1 1 d . . . C72 C 0.2760(2) 0.0939(3) 0.77385(16) 0.0267(10) Uani 1 1 d . . . C73 C 0.3197(2) 0.1003(3) 0.82360(18) 0.0461(14) Uani 1 1 d . . . H73A H 0.3566 0.1148 0.8229 0.069 Uiso 1 1 calc R . . H73B H 0.3225 0.0495 0.8388 0.069 Uiso 1 1 calc R . . H73C H 0.3073 0.1406 0.8401 0.069 Uiso 1 1 calc R . . C74 C 0.2958(3) 0.0314(3) 0.7472(2) 0.0530(16) Uani 1 1 d . . . H74A H 0.2703 0.0312 0.7156 0.079 Uiso 1 1 calc R . . H74B H 0.2958 -0.0206 0.7605 0.079 Uiso 1 1 calc R . . H74C H 0.3339 0.0442 0.7488 0.079 Uiso 1 1 calc R . . C75 C 0.2176(2) 0.0729(3) 0.77565(19) 0.0414(13) Uani 1 1 d . . . H75A H 0.2081 0.1104 0.7953 0.062 Uiso 1 1 calc R . . H75B H 0.2187 0.0195 0.7877 0.062 Uiso 1 1 calc R . . H75C H 0.1890 0.0754 0.7451 0.062 Uiso 1 1 calc R . . C76 C 0.35423(18) 0.3580(2) 0.78955(14) 0.0197(9) Uani 1 1 d . . . C77 C 0.40299(19) 0.3764(3) 0.83463(15) 0.0272(10) Uani 1 1 d . . . C78 C 0.4313(3) 0.2945(4) 0.8523(2) 0.075(2) Uani 1 1 d . . . H78A H 0.4647 0.3024 0.8795 0.112 Uiso 1 1 calc R . . H78B H 0.4423 0.2695 0.8288 0.112 Uiso 1 1 calc R . . H78C H 0.4045 0.2606 0.8594 0.112 Uiso 1 1 calc R . . C79 C 0.3817(3) 0.4123(6) 0.8697(2) 0.092(3) Uani 1 1 d . . . H79A H 0.3624 0.4621 0.8582 0.138 Uiso 1 1 calc R . . H79B H 0.4137 0.4221 0.8978 0.138 Uiso 1 1 calc R . . H79C H 0.3555 0.3758 0.8757 0.138 Uiso 1 1 calc R . . C80 C 0.4476(2) 0.4290(4) 0.82643(19) 0.0541(16) Uani 1 1 d . . . H80A H 0.4311 0.4806 0.8153 0.081 Uiso 1 1 calc R . . H80B H 0.4603 0.4043 0.8039 0.081 Uiso 1 1 calc R . . H80C H 0.4796 0.4357 0.8548 0.081 Uiso 1 1 calc R . . N1 N 0.2025(2) 0.4118(3) 0.60186(17) 0.0587(14) Uani 1 1 d . . . H1 H 0.2249 0.3715 0.6125 0.070 Uiso 1 1 calc R . . N2 N 0.1517(3) 0.5020(3) 0.55545(18) 0.0625(15) Uani 1 1 d . . . C90 C 0.1831(2) 0.4342(4) 0.55819(18) 0.0441(14) Uani 1 1 d . . . H90 H 0.1897 0.4085 0.5340 0.053 Uiso 1 1 calc R . . C91 C 0.1834(2) 0.4588(3) 0.62710(16) 0.0286(11) Uani 1 1 d . . . H91 H 0.1901 0.4537 0.6584 0.034 Uiso 1 1 calc R . . C92 C 0.1527(2) 0.5145(3) 0.59890(15) 0.0280(11) Uani 1 1 d . . . H92 H 0.1342 0.5566 0.6075 0.034 Uiso 1 1 calc R . . N3 N 0.3417(3) 0.5177(3) 0.70828(18) 0.093(2) Uani 1 1 d . . . H3 H 0.3642 0.4772 0.7182 0.112 Uiso 1 1 calc R . . N4 N 0.2900(2) 0.6020(3) 0.66196(17) 0.0567(14) Uani 1 1 d . . . C95 C 0.3263(2) 0.5473(3) 0.66565(15) 0.0452(16) Uani 1 1 d . . . H95 H 0.3398 0.5306 0.6428 0.054 Uiso 1 1 calc R . . C96 C 0.3189(3) 0.5573(4) 0.7324(2) 0.0524(16) Uani 1 1 d . . . H96 H 0.3251 0.5525 0.7636 0.063 Uiso 1 1 calc R . . C97 C 0.2844(3) 0.6066(6) 0.7019(2) 0.101(4) Uani 1 1 d . . . H97 H 0.2588 0.6410 0.7081 0.121 Uiso 1 1 calc R . . C100 C 0.4045(8) 0.4874(16) 0.0053(7) 0.147(6) Uiso 0.51(2) 1 d PDU F 1 H10D H 0.3929 0.5217 -0.0214 0.221 Uiso 0.51(2) 1 calc PR F 1 H10E H 0.3746 0.4858 0.0179 0.221 Uiso 0.51(2) 1 calc PR F 1 H10F H 0.4113 0.4342 -0.0035 0.221 Uiso 0.51(2) 1 calc PR F 1 C101 C 0.4655(9) 0.5238(12) 0.0454(5) 0.088(4) Uiso 0.51(2) 1 d PDU F 1 H10G H 0.4846 0.4907 0.0723 0.105 Uiso 0.51(2) 1 calc PR F 1 H10H H 0.4674 0.5811 0.0516 0.105 Uiso 0.51(2) 1 calc PR F 1 C103 C 0.3715(11) 0.4725(16) 0.0012(8) 0.140(7) Uiso 0.49(2) 1 d PDU F 2 H10I H 0.3470 0.5187 -0.0080 0.211 Uiso 0.49(2) 1 calc PR F 2 H10J H 0.3574 0.4374 0.0193 0.211 Uiso 0.49(2) 1 calc PR F 2 H10K H 0.3718 0.4444 -0.0257 0.211 Uiso 0.49(2) 1 calc PR F 2 C104 C 0.4415(9) 0.5034(14) 0.0344(6) 0.095(4) Uiso 0.49(2) 1 d PDU F 2 H10L H 0.4430 0.5586 0.0447 0.114 Uiso 0.49(2) 1 calc PR F 2 H10M H 0.4598 0.4684 0.0605 0.114 Uiso 0.49(2) 1 calc PR F 2 C102 C 0.4691(3) 0.4923(5) -0.0077(3) 0.087(2) Uiso 1 1 d D . . H10N H 0.4593 0.4362 -0.0145 0.104 Uiso 1 1 calc R F 1 H10O H 0.4468 0.5259 -0.0335 0.104 Uiso 1 1 calc R F 1 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 Cr1 0.0213(3) 0.0190(3) 0.0170(3) 0.0009(3) 0.0071(3) 0.0048(3) Cr2 0.0193(3) 0.0179(3) 0.0165(3) 0.0002(2) 0.0067(3) 0.0016(3) Cr3 0.0199(3) 0.0198(4) 0.0188(3) 0.0013(3) 0.0054(3) 0.0034(3) Cr4 0.0204(3) 0.0200(4) 0.0204(3) -0.0002(3) 0.0071(3) 0.0023(3) Cr5 0.0211(3) 0.0171(3) 0.0236(4) 0.0012(3) 0.0109(3) 0.0016(3) Cr6 0.0195(3) 0.0155(3) 0.0178(3) 0.0012(2) 0.0076(3) 0.0028(3) Cr7 0.0220(3) 0.0200(4) 0.0179(3) 0.0017(3) 0.0073(3) 0.0046(3) Cr8 0.0209(3) 0.0208(4) 0.0194(3) 0.0004(3) 0.0065(3) 0.0043(3) Ni1 0.0213(3) 0.0190(3) 0.0170(3) 0.0009(3) 0.0071(3) 0.0048(3) Ni2 0.0193(3) 0.0179(3) 0.0165(3) 0.0002(2) 0.0067(3) 0.0016(3) Ni3 0.0199(3) 0.0198(4) 0.0188(3) 0.0013(3) 0.0054(3) 0.0034(3) Ni4 0.0204(3) 0.0200(4) 0.0204(3) -0.0002(3) 0.0071(3) 0.0023(3) Ni5 0.0211(3) 0.0171(3) 0.0236(4) 0.0012(3) 0.0109(3) 0.0016(3) Ni6 0.0195(3) 0.0155(3) 0.0178(3) 0.0012(2) 0.0076(3) 0.0028(3) Ni7 0.0220(3) 0.0200(4) 0.0179(3) 0.0017(3) 0.0073(3) 0.0046(3) Ni8 0.0209(3) 0.0208(4) 0.0194(3) 0.0004(3) 0.0065(3) 0.0043(3) F1 0.0238(13) 0.0268(14) 0.0219(13) -0.0026(10) 0.0063(11) 0.0045(11) F2 0.0216(13) 0.0301(14) 0.0199(13) 0.0007(10) 0.0046(11) 0.0010(11) F3 0.0252(13) 0.0243(14) 0.0193(13) -0.0013(10) 0.0034(11) 0.0016(11) F4 0.0289(14) 0.0203(13) 0.0264(14) -0.0039(10) 0.0124(12) -0.0047(11) F5 0.0203(13) 0.0243(14) 0.0244(13) 0.0011(10) 0.0086(11) 0.0012(10) F6 0.0258(13) 0.0223(13) 0.0203(13) 0.0002(10) 0.0073(11) 0.0015(11) F7 0.0223(13) 0.0186(13) 0.0265(14) -0.0006(10) 0.0088(11) 0.0011(10) F8 0.0209(13) 0.0264(14) 0.0170(12) 0.0014(10) 0.0065(10) 0.0041(10) O1 0.0247(16) 0.0207(16) 0.0237(17) -0.0038(12) 0.0083(14) -0.0036(13) O2 0.0361(19) 0.0304(19) 0.0257(18) 0.0046(14) -0.0004(15) -0.0107(15) O3 0.0330(18) 0.0285(18) 0.0215(17) 0.0007(13) 0.0091(15) 0.0114(14) O4 0.0263(17) 0.0225(17) 0.0230(17) 0.0001(13) 0.0091(14) 0.0074(13) O5 0.0392(19) 0.0240(17) 0.0217(16) -0.0027(13) 0.0142(15) 0.0028(15) O6 0.0263(17) 0.0236(18) 0.0237(16) 0.0010(13) 0.0124(14) 0.0042(13) O7 0.0183(15) 0.0220(17) 0.0241(16) -0.0007(12) 0.0039(13) -0.0007(13) O8 0.0257(17) 0.0231(18) 0.0353(19) -0.0012(14) -0.0043(15) -0.0016(14) O9 0.0243(16) 0.0228(17) 0.0221(16) 0.0006(13) 0.0050(14) 0.0045(13) O10 0.0179(16) 0.038(2) 0.0276(18) -0.0099(15) -0.0003(14) 0.0053(14) O11 0.0247(17) 0.0259(18) 0.0344(18) 0.0084(14) 0.0145(15) 0.0054(14) O12 0.0243(17) 0.0289(18) 0.0267(17) 0.0039(13) 0.0121(14) 0.0035(14) O13 0.0306(17) 0.0267(18) 0.0240(17) 0.0024(13) 0.0098(14) 0.0084(14) O14 0.0309(18) 0.0176(16) 0.0322(18) 0.0053(13) 0.0173(15) 0.0041(13) O15 0.0202(16) 0.0219(16) 0.0254(17) -0.0043(13) 0.0085(13) -0.0048(13) O16 0.0288(18) 0.0301(19) 0.0300(18) -0.0079(14) 0.0127(15) -0.0073(14) O17 0.0198(15) 0.0237(17) 0.0250(16) 0.0031(13) 0.0088(13) 0.0007(13) O18 0.0316(18) 0.0358(19) 0.0246(18) 0.0091(14) 0.0039(15) -0.0103(15) O19 0.0268(17) 0.0216(17) 0.0401(19) -0.0037(14) 0.0189(16) -0.0003(14) O20 0.0285(17) 0.0205(17) 0.0320(18) 0.0045(13) 0.0160(15) 0.0056(14) O21 0.0288(18) 0.0329(19) 0.0328(19) 0.0124(15) 0.0183(15) 0.0108(14) O22 0.0283(17) 0.0273(17) 0.0223(16) 0.0036(13) 0.0121(14) 0.0102(14) O23 0.0351(18) 0.0232(17) 0.0205(17) -0.0051(13) 0.0090(15) 0.0006(14) O24 0.0347(19) 0.0268(19) 0.0252(18) -0.0064(14) -0.0059(15) 0.0070(15) O25 0.0185(15) 0.0218(17) 0.0268(17) 0.0014(13) 0.0057(13) 0.0013(13) O26 0.0200(16) 0.0233(17) 0.0273(17) -0.0054(13) 0.0083(14) 0.0014(13) O27 0.0377(19) 0.0293(19) 0.0221(17) 0.0061(13) 0.0150(15) 0.0102(15) O28 0.0295(17) 0.0224(17) 0.0215(16) 0.0001(13) 0.0109(14) 0.0042(13) O29 0.0267(17) 0.0210(16) 0.0261(17) 0.0008(13) 0.0111(14) 0.0039(14) O30 0.0269(17) 0.0214(17) 0.0262(17) 0.0041(13) 0.0125(14) 0.0066(13) O31 0.0178(15) 0.0219(16) 0.0159(15) -0.0008(12) 0.0025(12) 0.0033(12) O32 0.0201(16) 0.046(2) 0.0194(17) -0.0046(14) 0.0072(14) -0.0001(15) C1 0.023(2) 0.025(3) 0.025(3) -0.0013(19) 0.009(2) 0.0012(19) C2 0.051(4) 0.038(3) 0.039(3) -0.013(3) 0.008(3) -0.014(3) C3 0.061(6) 0.039(4) 0.052(5) -0.014(3) 0.012(4) -0.026(4) C4 0.081(5) 0.054(6) 0.054(5) -0.027(4) 0.030(4) -0.021(5) C5 0.063(4) 0.056(5) 0.069(5) -0.010(4) -0.012(4) -0.011(4) C2A 0.046(4) 0.035(3) 0.039(3) -0.011(3) 0.011(3) -0.016(3) C3A 0.056(5) 0.035(4) 0.048(5) -0.014(3) 0.008(4) -0.013(4) C4A 0.067(5) 0.048(4) 0.038(3) -0.014(3) 0.010(3) -0.027(4) C5A 0.037(4) 0.052(5) 0.054(5) -0.005(5) 0.008(4) -0.016(4) C6 0.020(2) 0.019(2) 0.026(3) -0.0044(19) 0.006(2) -0.0009(18) C7 0.029(3) 0.031(3) 0.036(3) 0.003(2) 0.010(2) 0.011(2) C8 0.063(4) 0.028(3) 0.140(7) 0.000(4) 0.041(5) 0.015(3) C9 0.030(3) 0.062(4) 0.066(4) 0.002(3) 0.005(3) 0.012(3) C10 0.081(5) 0.122(6) 0.054(4) 0.031(4) 0.040(4) 0.076(5) C11 0.015(2) 0.027(3) 0.018(2) 0.0010(18) 0.0021(18) 0.0036(18) C12 0.024(2) 0.032(3) 0.027(3) -0.003(2) 0.014(2) 0.002(2) C13 0.040(3) 0.065(4) 0.038(3) -0.023(3) 0.016(3) -0.008(3) C14 0.055(4) 0.045(3) 0.048(3) 0.000(3) 0.030(3) 0.019(3) C15 0.057(4) 0.041(3) 0.044(3) -0.003(2) 0.034(3) -0.004(3) C16 0.018(2) 0.028(3) 0.019(2) -0.0038(18) 0.0075(19) 0.0041(19) C17 0.022(3) 0.032(3) 0.056(4) -0.004(3) 0.001(3) -0.003(3) C18 0.044(5) 0.044(5) 0.058(4) 0.003(4) -0.013(4) -0.009(4) C19 0.027(5) 0.033(3) 0.058(6) -0.007(3) 0.002(5) -0.006(4) C20 0.028(4) 0.050(5) 0.087(6) -0.017(4) 0.009(4) 0.005(4) C17A 0.021(3) 0.032(3) 0.054(4) -0.003(2) 0.002(3) -0.001(3) C18A 0.028(5) 0.041(4) 0.060(5) 0.003(4) -0.005(4) -0.003(4) C19A 0.027(5) 0.034(3) 0.060(6) -0.008(3) 0.003(4) -0.008(4) C20A 0.025(4) 0.052(5) 0.061(5) -0.006(4) 0.008(4) -0.002(4) C21 0.021(2) 0.021(2) 0.023(2) 0.0017(18) 0.0076(19) -0.0028(19) C22 0.042(3) 0.039(3) 0.030(3) -0.011(3) 0.000(3) -0.001(3) C23 0.075(5) 0.067(5) 0.036(4) -0.001(4) 0.002(4) -0.021(5) C24 0.038(3) 0.055(6) 0.046(5) -0.018(5) -0.011(4) 0.006(4) C25 0.044(5) 0.039(3) 0.042(5) -0.014(4) -0.004(4) -0.001(4) C22A 0.040(3) 0.039(3) 0.027(3) -0.008(2) 0.003(3) -0.001(3) C23A 0.048(5) 0.055(4) 0.031(4) 0.003(4) 0.003(4) -0.001(4) C24A 0.035(4) 0.042(6) 0.040(5) -0.001(4) -0.003(3) -0.005(4) C25A 0.050(5) 0.054(4) 0.042(5) -0.024(4) -0.008(4) 0.010(4) C26 0.020(2) 0.028(3) 0.018(2) -0.0040(18) 0.0070(19) 0.0000(19) C27 0.029(3) 0.032(3) 0.029(3) 0.004(2) 0.013(2) -0.002(2) C28 0.027(3) 0.041(3) 0.041(3) 0.000(2) 0.013(2) -0.005(2) C29 0.041(3) 0.035(3) 0.046(3) 0.010(2) 0.020(3) -0.005(2) C30 0.049(3) 0.046(3) 0.038(3) 0.000(2) 0.025(3) 0.001(3) C31 0.019(2) 0.017(2) 0.027(2) -0.0020(18) 0.0067(19) -0.0050(18) C32 0.045(3) 0.036(3) 0.027(3) 0.012(2) 0.008(3) 0.007(2) C33 0.051(5) 0.042(6) 0.039(5) 0.006(4) 0.004(5) 0.018(4) C34 0.054(6) 0.046(5) 0.033(4) 0.004(3) 0.004(4) 0.010(4) C35 0.060(4) 0.047(5) 0.036(5) 0.016(4) 0.011(4) -0.006(3) C32A 0.045(3) 0.035(3) 0.027(3) 0.010(2) 0.005(3) 0.008(2) C33A 0.052(5) 0.040(5) 0.041(5) 0.006(3) 0.001(4) 0.017(4) C34A 0.059(5) 0.043(5) 0.032(5) 0.006(3) -0.004(4) 0.007(4) C35A 0.063(4) 0.051(5) 0.036(6) 0.018(4) 0.015(4) 0.000(4) C36 0.024(2) 0.016(2) 0.027(3) 0.0015(18) 0.008(2) 0.0009(18) C37 0.023(2) 0.037(3) 0.038(3) -0.014(2) 0.007(2) -0.009(2) C38 0.068(4) 0.088(5) 0.046(4) -0.042(3) 0.024(3) -0.039(4) C39 0.046(3) 0.043(3) 0.060(4) -0.017(3) 0.025(3) -0.024(3) C40 0.030(3) 0.059(4) 0.059(4) -0.004(3) -0.005(3) -0.001(3) C41 0.027(2) 0.017(2) 0.019(2) -0.0004(18) 0.0060(19) -0.0018(19) C42 0.026(3) 0.028(3) 0.031(3) 0.004(2) 0.002(2) -0.004(2) C43 0.029(3) 0.068(4) 0.074(5) 0.008(3) 0.021(3) 0.000(3) C44 0.057(4) 0.038(3) 0.039(3) -0.002(2) -0.002(3) -0.020(3) C45 0.033(3) 0.045(3) 0.043(3) 0.020(3) -0.006(3) -0.004(3) C46 0.027(2) 0.025(3) 0.032(3) 0.000(2) 0.015(2) 0.002(2) C47 0.044(3) 0.029(3) 0.061(5) -0.002(4) 0.028(4) 0.013(3) C48 0.045(3) 0.037(5) 0.080(7) -0.009(6) 0.018(5) 0.012(3) C49 0.053(5) 0.023(5) 0.081(7) 0.003(5) 0.027(5) 0.013(4) C50 0.060(7) 0.044(5) 0.060(5) -0.005(5) 0.025(5) 0.021(6) C47A 0.040(3) 0.026(3) 0.061(5) -0.001(4) 0.028(3) 0.011(3) C48A 0.048(3) 0.036(4) 0.067(6) -0.009(6) 0.018(5) 0.016(3) C49A 0.058(5) 0.029(5) 0.071(6) 0.009(5) 0.032(5) 0.011(4) C50A 0.053(6) 0.043(5) 0.059(5) 0.004(5) 0.029(4) 0.016(6) C51 0.023(2) 0.023(2) 0.020(2) -0.0028(18) 0.007(2) 0.0027(19) C52 0.030(3) 0.044(3) 0.025(3) 0.003(2) 0.017(2) 0.006(2) C53 0.041(3) 0.037(3) 0.031(3) 0.005(2) 0.023(2) 0.010(2) C54 0.040(4) 0.131(7) 0.063(4) -0.039(4) 0.032(3) -0.034(4) C55 0.062(4) 0.091(5) 0.053(4) 0.032(3) 0.042(3) 0.052(4) C56 0.028(3) 0.030(3) 0.025(3) -0.006(2) 0.008(2) 0.002(2) C57 0.050(3) 0.029(3) 0.036(3) -0.012(2) 0.001(3) 0.000(3) C58 0.067(4) 0.077(5) 0.035(3) -0.021(3) 0.012(3) 0.013(4) C59 0.105(6) 0.040(4) 0.071(5) -0.017(3) -0.006(4) -0.017(4) C60 0.043(3) 0.071(4) 0.044(4) -0.030(3) 0.003(3) -0.012(3) C61 0.023(2) 0.024(2) 0.020(2) 0.0047(18) 0.0099(19) -0.006(2) C62 0.019(2) 0.034(3) 0.030(3) 0.000(2) 0.004(2) -0.004(2) C63 0.038(3) 0.044(3) 0.056(4) -0.019(3) 0.010(3) -0.012(3) C64 0.044(3) 0.060(4) 0.029(3) 0.004(3) -0.005(3) -0.012(3) C65 0.025(3) 0.045(3) 0.049(3) -0.003(3) 0.011(3) -0.006(2) C66 0.019(2) 0.029(3) 0.018(2) 0.0041(19) 0.0075(19) 0.0024(19) C67 0.025(2) 0.027(2) 0.018(2) 0.0025(18) 0.0049(19) 0.0018(19) C68 0.047(3) 0.032(3) 0.032(3) 0.012(2) 0.018(3) 0.003(2) C69 0.039(3) 0.043(3) 0.035(3) 0.005(2) 0.021(3) 0.004(2) C70 0.034(3) 0.047(3) 0.017(2) 0.000(2) 0.006(2) -0.001(2) C71 0.030(3) 0.022(2) 0.017(2) -0.0034(17) 0.007(2) 0.002(2) C72 0.030(3) 0.022(2) 0.029(3) 0.0032(19) 0.012(2) 0.004(2) C73 0.049(3) 0.041(3) 0.040(3) 0.018(3) 0.006(3) 0.002(3) C74 0.080(4) 0.022(3) 0.074(4) 0.003(3) 0.047(4) 0.006(3) C75 0.044(3) 0.031(3) 0.049(3) 0.008(2) 0.017(3) -0.006(2) C76 0.020(2) 0.015(2) 0.022(2) 0.0008(17) 0.0048(19) 0.0013(18) C77 0.023(2) 0.033(3) 0.021(2) -0.0017(19) 0.003(2) -0.005(2) C78 0.058(4) 0.063(4) 0.069(5) 0.030(4) -0.018(4) -0.005(3) C79 0.052(4) 0.177(9) 0.045(4) -0.058(5) 0.016(3) -0.025(5) C80 0.046(3) 0.070(4) 0.038(3) 0.003(3) 0.007(3) -0.022(3) N1 0.054(3) 0.060(3) 0.054(3) 0.002(3) 0.009(3) 0.030(3) N2 0.092(4) 0.049(3) 0.055(3) -0.008(2) 0.036(3) -0.023(3) C90 0.030(3) 0.073(4) 0.031(3) -0.018(3) 0.014(2) 0.004(3) C91 0.035(3) 0.030(3) 0.025(3) -0.002(2) 0.016(2) 0.005(2) C92 0.054(3) 0.015(2) 0.022(2) -0.0020(18) 0.022(2) 0.008(2) N3 0.174(7) 0.056(4) 0.039(3) 0.006(3) 0.025(4) 0.064(4) N4 0.066(3) 0.057(3) 0.041(3) 0.011(2) 0.012(3) 0.013(3) C95 0.069(4) 0.052(3) 0.011(2) 0.004(2) 0.009(2) 0.046(3) C96 0.056(4) 0.072(4) 0.036(3) 0.004(3) 0.025(3) -0.006(3) C97 0.096(6) 0.191(9) 0.028(3) 0.034(4) 0.036(4) 0.122(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 Cr1 F1 1.937(3) . ? Cr1 F8 1.949(2) . ? Cr1 O3 1.959(3) . ? Cr1 O32 1.979(3) . ? Cr1 O30 1.988(3) . ? Cr1 O1 1.995(3) . ? Cr2 F2 1.941(2) . ? Cr2 F1 1.944(2) . ? Cr2 O5 1.958(3) . ? Cr2 O4 1.970(3) . ? Cr2 O7 1.980(3) . ? Cr2 O2 1.986(3) . ? Cr3 F2 1.934(2) . ? Cr3 F3 1.944(2) . ? Cr3 O11 1.963(3) . ? Cr3 O6 1.971(3) . ? Cr3 O8 1.980(3) . ? Cr3 O9 1.984(3) . ? Cr4 F4 1.929(2) . ? Cr4 F3 1.936(2) . ? Cr4 O13 1.950(3) . ? Cr4 O12 1.961(3) . ? Cr4 O10 1.965(3) . ? Cr4 O15 1.972(3) . ? Cr5 F5 1.934(2) . ? Cr5 O19 1.959(3) . ? Cr5 F4 1.959(2) . ? Cr5 O16 1.977(3) . ? Cr5 O14 1.979(3) . ? Cr5 O17 2.000(3) . ? Cr6 F6 1.951(2) . ? Cr6 F5 1.951(2) . ? Cr6 O21 1.964(3) . ? Cr6 O20 1.972(3) . ? Cr6 O23 1.988(3) . ? Cr6 O18 1.995(3) . ? Cr7 F6 1.935(2) . ? Cr7 F7 1.940(2) . ? Cr7 O22 1.955(3) . ? Cr7 O27 1.963(3) . ? Cr7 O24 1.966(3) . ? Cr7 O25 1.981(3) . ? Cr8 F8 1.922(2) . ? Cr8 F7 1.943(2) . ? Cr8 O29 1.944(3) . ? Cr8 O26 1.960(3) . ? Cr8 O28 1.963(3) . ? Cr8 O31 1.991(3) . ? O1 C1 1.264(5) . ? O2 C1 1.247(5) . ? O3 C6 1.256(5) . ? O4 C6 1.262(5) . ? O5 C11 1.259(5) . ? O6 C11 1.263(5) . ? O7 C16 1.253(5) . ? O8 C16 1.267(5) . ? O9 C21 1.249(5) . ? O10 C21 1.266(5) . ? O11 C26 1.247(5) . ? O12 C26 1.272(5) . ? O13 C31 1.256(5) . ? O14 C31 1.252(5) . ? O15 C36 1.257(5) . ? O16 C36 1.259(5) . ? O17 C41 1.252(5) . ? O18 C41 1.260(5) . ? O19 C46 1.257(5) . ? O20 C46 1.262(5) . ? O21 C51 1.252(5) . ? O22 C51 1.261(5) . ? O23 C56 1.258(5) . ? O24 C56 1.262(5) . ? O25 C61 1.261(5) . ? O26 C61 1.254(5) . ? O27 C66 1.253(5) . ? O28 C66 1.251(5) . ? O29 C71 1.263(5) . ? O30 C71 1.246(5) . ? O31 C76 1.258(5) . ? O32 C76 1.269(5) . ? C1 C2 1.505(17) . ? C1 C2A 1.557(17) . ? C2 C5 1.504(12) . ? C2 C3 1.515(12) . ? C2 C4 1.560(11) . ? C2A C3A 1.521(12) . ? C2A C4A 1.522(12) . ? C2A C5A 1.529(11) . ? C6 C7 1.530(6) . ? C7 C9 1.500(7) . ? C7 C10 1.506(7) . ? C7 C8 1.513(8) . ? C11 C12 1.526(6) . ? C12 C13 1.507(6) . ? C12 C15 1.519(6) . ? C12 C14 1.526(7) . ? C16 C17A 1.52(2) . ? C16 C17 1.53(2) . ? C17 C19 1.523(12) . ? C17 C20 1.530(12) . ? C17 C18 1.532(12) . ? C17A C18A 1.511(12) . ? C17A C19A 1.516(12) . ? C17A C20A 1.549(12) . ? C21 C22 1.51(2) . ? C21 C22A 1.53(2) . ? C22 C23 1.502(12) . ? C22 C25 1.520(12) . ? C22 C24 1.533(12) . ? C22A C25A 1.507(12) . ? C22A C24A 1.536(12) . ? C22A C23A 1.538(12) . ? C26 C27 1.526(6) . ? C27 C28 1.519(6) . ? C27 C29 1.525(7) . ? C27 C30 1.534(6) . ? C31 C32A 1.51(3) . ? C31 C32 1.52(3) . ? C32 C34 1.511(12) . ? C32 C33 1.522(12) . ? C32 C35 1.535(12) . ? C32A C34A 1.512(12) . ? C32A C33A 1.518(12) . ? C32A C35A 1.523(13) . ? C36 C37 1.525(6) . ? C37 C38 1.498(7) . ? C37 C40 1.529(7) . ? C37 C39 1.540(7) . ? C41 C42 1.528(6) . ? C42 C45 1.524(6) . ? C42 C44 1.534(7) . ? C42 C43 1.536(7) . ? C46 C47 1.51(3) . ? C46 C47A 1.53(3) . ? C47 C49 1.487(12) . ? C47 C48 1.511(12) . ? C47 C50 1.586(12) . ? C47A C49A 1.503(12) . ? C47A C48A 1.519(12) . ? C47A C50A 1.550(12) . ? C51 C52 1.530(6) . ? C52 C54 1.510(8) . ? C52 C55 1.513(7) . ? C52 C53 1.523(6) . ? C56 C57 1.521(6) . ? C57 C59 1.502(8) . ? C57 C58 1.529(8) . ? C57 C60 1.534(8) . ? C61 C62 1.536(6) . ? C62 C65 1.518(6) . ? C62 C63 1.520(7) . ? C62 C64 1.540(7) . ? C66 C67 1.522(6) . ? C67 C68 1.515(6) . ? C67 C70 1.528(6) . ? C67 C69 1.541(6) . ? C71 C72 1.537(6) . ? C72 C74 1.520(7) . ? C72 C75 1.521(7) . ? C72 C73 1.541(7) . ? C76 C77 1.519(6) . ? C77 C79 1.499(7) . ? C77 C80 1.509(7) . ? C77 C78 1.542(7) . ? N1 C91 1.314(6) . ? N1 C90 1.319(7) . ? N2 C92 1.358(6) . ? N2 C90 1.359(7) . ? C91 C92 1.315(6) . ? N3 C96 1.277(7) . ? N3 C95 1.333(7) . ? N4 C95 1.259(6) . ? N4 C97 1.300(7) . ? C96 C97 1.313(8) . ? C100 C101 1.697(11) . ? C101 C102 1.767(11) . ? C103 C104 1.756(12) . ? C104 C102 1.694(11) . ? C102 C102 1.464(14) 3_665 ? 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 Cr1 F8 86.02(10) . . ? F1 Cr1 O3 90.49(12) . . ? F8 Cr1 O3 176.47(12) . . ? F1 Cr1 O32 89.30(12) . . ? F8 Cr1 O32 89.40(11) . . ? O3 Cr1 O32 90.08(13) . . ? F1 Cr1 O30 179.20(11) . . ? F8 Cr1 O30 93.51(11) . . ? O3 Cr1 O30 89.98(12) . . ? O32 Cr1 O30 90.04(13) . . ? F1 Cr1 O1 93.76(11) . . ? F8 Cr1 O1 89.81(11) . . ? O3 Cr1 O1 90.91(12) . . ? O32 Cr1 O1 176.77(13) . . ? O30 Cr1 O1 86.89(12) . . ? F2 Cr2 F1 89.20(10) . . ? F2 Cr2 O5 90.05(11) . . ? F1 Cr2 O5 178.19(12) . . ? F2 Cr2 O4 178.41(11) . . ? F1 Cr2 O4 92.31(11) . . ? O5 Cr2 O4 88.45(12) . . ? F2 Cr2 O7 92.83(11) . . ? F1 Cr2 O7 90.08(11) . . ? O5 Cr2 O7 91.60(13) . . ? O4 Cr2 O7 86.69(12) . . ? F2 Cr2 O2 89.00(12) . . ? F1 Cr2 O2 88.99(12) . . ? O5 Cr2 O2 89.35(14) . . ? O4 Cr2 O2 91.51(13) . . ? O7 Cr2 O2 177.93(13) . . ? F2 Cr3 F3 88.31(10) . . ? F2 Cr3 O11 176.59(12) . . ? F3 Cr3 O11 90.43(12) . . ? F2 Cr3 O6 92.67(11) . . ? F3 Cr3 O6 179.01(12) . . ? O11 Cr3 O6 88.59(12) . . ? F2 Cr3 O8 88.95(12) . . ? F3 Cr3 O8 87.94(12) . . ? O11 Cr3 O8 87.84(13) . . ? O6 Cr3 O8 92.13(13) . . ? F2 Cr3 O9 91.03(11) . . ? F3 Cr3 O9 92.54(11) . . ? O11 Cr3 O9 92.19(13) . . ? O6 Cr3 O9 87.40(12) . . ? O8 Cr3 O9 179.52(14) . . ? F4 Cr4 F3 88.28(10) . . ? F4 Cr4 O13 91.06(12) . . ? F3 Cr4 O13 178.55(12) . . ? F4 Cr4 O12 177.54(12) . . ? F3 Cr4 O12 92.11(11) . . ? O13 Cr4 O12 88.60(13) . . ? F4 Cr4 O10 91.58(12) . . ? F3 Cr4 O10 90.71(12) . . ? O13 Cr4 O10 88.02(13) . . ? O12 Cr4 O10 90.84(13) . . ? F4 Cr4 O15 90.77(11) . . ? F3 Cr4 O15 88.54(11) . . ? O13 Cr4 O15 92.76(13) . . ? O12 Cr4 O15 86.82(12) . . ? O10 Cr4 O15 177.51(13) . . ? F5 Cr5 O19 91.44(12) . . ? F5 Cr5 F4 86.95(10) . . ? O19 Cr5 F4 178.11(12) . . ? F5 Cr5 O16 88.12(12) . . ? O19 Cr5 O16 90.86(13) . . ? F4 Cr5 O16 90.08(12) . . ? F5 Cr5 O14 179.79(15) . . ? O19 Cr5 O14 88.66(13) . . ? F4 Cr5 O14 92.95(11) . . ? O16 Cr5 O14 92.07(13) . . ? F5 Cr5 O17 93.65(11) . . ? O19 Cr5 O17 89.06(12) . . ? F4 Cr5 O17 90.05(11) . . ? O16 Cr5 O17 178.23(13) . . ? O14 Cr5 O17 86.16(12) . . ? F6 Cr6 F5 87.50(10) . . ? F6 Cr6 O21 91.70(11) . . ? F5 Cr6 O21 177.59(12) . . ? F6 Cr6 O20 178.79(12) . . ? F5 Cr6 O20 92.52(11) . . ? O21 Cr6 O20 88.23(12) . . ? F6 Cr6 O23 91.51(11) . . ? F5 Cr6 O23 89.80(11) . . ? O21 Cr6 O23 92.49(13) . . ? O20 Cr6 O23 89.70(13) . . ? F6 Cr6 O18 87.75(12) . . ? F5 Cr6 O18 88.22(12) . . ? O21 Cr6 O18 89.48(13) . . ? O20 Cr6 O18 91.04(13) . . ? O23 Cr6 O18 177.92(13) . . ? F6 Cr7 F7 87.36(10) . . ? F6 Cr7 O22 93.98(11) . . ? F7 Cr7 O22 178.16(12) . . ? F6 Cr7 O27 178.53(12) . . ? F7 Cr7 O27 91.39(11) . . ? O22 Cr7 O27 87.29(12) . . ? F6 Cr7 O24 89.24(12) . . ? F7 Cr7 O24 89.60(12) . . ? O22 Cr7 O24 91.68(13) . . ? O27 Cr7 O24 89.98(14) . . ? F6 Cr7 O25 87.96(11) . . ? F7 Cr7 O25 90.62(11) . . ? O22 Cr7 O25 88.17(12) . . ? O27 Cr7 O25 92.83(13) . . ? O24 Cr7 O25 177.18(13) . . ? F8 Cr8 F7 88.19(10) . . ? F8 Cr8 O29 91.36(11) . . ? F7 Cr8 O29 179.41(11) . . ? F8 Cr8 O26 87.27(11) . . ? F7 Cr8 O26 89.36(11) . . ? O29 Cr8 O26 90.25(12) . . ? F8 Cr8 O28 178.43(11) . . ? F7 Cr8 O28 93.38(11) . . ? O29 Cr8 O28 87.08(12) . . ? O26 Cr8 O28 92.70(12) . . ? F8 Cr8 O31 92.58(11) . . ? F7 Cr8 O31 89.74(11) . . ? O29 Cr8 O31 90.65(12) . . ? O26 Cr8 O31 179.09(13) . . ? O28 Cr8 O31 87.48(12) . . ? Cr1 F1 Cr2 121.34(12) . . ? Cr3 F2 Cr2 122.69(12) . . ? Cr4 F3 Cr3 122.99(12) . . ? Cr4 F4 Cr5 122.48(12) . . ? Cr5 F5 Cr6 121.83(12) . . ? Cr7 F6 Cr6 121.88(12) . . ? Cr7 F7 Cr8 122.66(12) . . ? Cr8 F8 Cr1 122.22(12) . . ? C1 O1 Cr1 133.1(3) . . ? C1 O2 Cr2 125.6(3) . . ? C6 O3 Cr1 127.6(3) . . ? C6 O4 Cr2 133.5(3) . . ? C11 O5 Cr2 129.7(3) . . ? C11 O6 Cr3 133.4(3) . . ? C16 O7 Cr2 134.1(3) . . ? C16 O8 Cr3 127.9(3) . . ? C21 O9 Cr3 135.4(3) . . ? C21 O10 Cr4 130.4(3) . . ? C26 O11 Cr3 131.5(3) . . ? C26 O12 Cr4 133.3(3) . . ? C31 O13 Cr4 131.5(3) . . ? C31 O14 Cr5 133.8(3) . . ? C36 O15 Cr4 136.4(3) . . ? C36 O16 Cr5 129.0(3) . . ? C41 O17 Cr5 133.2(3) . . ? C41 O18 Cr6 123.9(3) . . ? C46 O19 Cr5 127.6(3) . . ? C46 O20 Cr6 134.9(3) . . ? C51 O21 Cr6 129.3(3) . . ? C51 O22 Cr7 134.0(3) . . ? C56 O23 Cr6 134.6(3) . . ? C56 O24 Cr7 129.2(3) . . ? C61 O25 Cr7 134.6(3) . . ? C61 O26 Cr8 130.7(3) . . ? C66 O27 Cr7 131.2(3) . . ? C66 O28 Cr8 135.0(3) . . ? C71 O29 Cr8 129.0(3) . . ? C71 O30 Cr1 133.0(3) . . ? C76 O31 Cr8 134.8(3) . . ? C76 O32 Cr1 127.6(3) . . ? O2 C1 O1 125.6(4) . . ? O2 C1 C2 116.4(6) . . ? O1 C1 C2 117.6(5) . . ? O2 C1 C2A 119.0(5) . . ? O1 C1 C2A 115.0(5) . . ? C2 C1 C2A 12.8(7) . . ? C5 C2 C1 108.7(9) . . ? C5 C2 C3 113.8(10) . . ? C1 C2 C3 111.8(10) . . ? C5 C2 C4 109.1(10) . . ? C1 C2 C4 105.6(9) . . ? C3 C2 C4 107.5(9) . . ? C3A C2A C4A 113.4(10) . . ? C3A C2A C5A 110.3(9) . . ? C4A C2A C5A 108.7(9) . . ? C3A C2A C1 107.5(9) . . ? C4A C2A C1 110.5(9) . . ? C5A C2A C1 106.1(9) . . ? O3 C6 O4 125.9(4) . . ? O3 C6 C7 116.2(4) . . ? O4 C6 C7 117.8(4) . . ? C9 C7 C10 110.3(5) . . ? C9 C7 C8 109.7(5) . . ? C10 C7 C8 111.5(5) . . ? C9 C7 C6 109.0(4) . . ? C10 C7 C6 110.2(4) . . ? C8 C7 C6 106.1(4) . . ? O5 C11 O6 125.9(4) . . ? O5 C11 C12 116.2(4) . . ? O6 C11 C12 117.9(4) . . ? C13 C12 C15 110.4(4) . . ? C13 C12 C11 106.2(4) . . ? C15 C12 C11 111.1(4) . . ? C13 C12 C14 109.0(4) . . ? C15 C12 C14 111.0(4) . . ? C11 C12 C14 109.0(4) . . ? O7 C16 O8 125.7(4) . . ? O7 C16 C17A 119.0(6) . . ? O8 C16 C17A 114.9(7) . . ? O7 C16 C17 117.0(7) . . ? O8 C16 C17 117.3(7) . . ? C17A C16 C17 5.8(10) . . ? C19 C17 C20 108.6(13) . . ? C19 C17 C16 113.3(15) . . ? C20 C17 C16 108.2(12) . . ? C19 C17 C18 110.4(13) . . ? C20 C17 C18 108.4(12) . . ? C16 C17 C18 107.9(12) . . ? C18A C17A C19A 112.5(14) . . ? C18A C17A C16 112.4(13) . . ? C19A C17A C16 109.7(15) . . ? C18A C17A C20A 107.2(11) . . ? C19A C17A C20A 110.3(13) . . ? C16 C17A C20A 104.4(12) . . ? O9 C21 O10 125.3(4) . . ? O9 C21 C22 118.0(6) . . ? O10 C21 C22 116.7(6) . . ? O9 C21 C22A 120.4(6) . . ? O10 C21 C22A 114.3(6) . . ? C22 C21 C22A 4.3(9) . . ? C23 C22 C21 105.7(11) . . ? C23 C22 C25 113.8(13) . . ? C21 C22 C25 111.1(12) . . ? C23 C22 C24 109.6(13) . . ? C21 C22 C24 110.2(13) . . ? C25 C22 C24 106.4(11) . . ? C25A C22A C21 111.9(11) . . ? C25A C22A C24A 108.1(12) . . ? C21 C22A C24A 107.9(12) . . ? C25A C22A C23A 112.1(12) . . ? C21 C22A C23A 108.5(11) . . ? C24A C22A C23A 108.2(12) . . ? O11 C26 O12 125.3(4) . . ? O11 C26 C27 117.0(4) . . ? O12 C26 C27 117.7(4) . . ? C28 C27 C29 109.3(4) . . ? C28 C27 C26 106.9(4) . . ? C29 C27 C26 111.4(4) . . ? C28 C27 C30 110.8(4) . . ? C29 C27 C30 110.6(4) . . ? C26 C27 C30 107.8(4) . . ? O14 C31 O13 125.4(4) . . ? O14 C31 C32A 118.6(7) . . ? O13 C31 C32A 115.9(7) . . ? O14 C31 C32 117.3(7) . . ? O13 C31 C32 117.2(7) . . ? C32A C31 C32 2.1(11) . . ? C34 C32 C31 110.8(13) . . ? C34 C32 C33 112.0(14) . . ? C31 C32 C33 110.5(14) . . ? C34 C32 C35 110.1(12) . . ? C31 C32 C35 102.7(13) . . ? C33 C32 C35 110.4(12) . . ? C34A C32A C31 108.5(13) . . ? C34A C32A C33A 111.1(13) . . ? C31 C32A C33A 111.3(14) . . ? C34A C32A C35A 111.8(13) . . ? C31 C32A C35A 107.6(13) . . ? C33A C32A C35A 106.6(13) . . ? O15 C36 O16 125.9(4) . . ? O15 C36 C37 116.2(4) . . ? O16 C36 C37 118.0(4) . . ? C38 C37 C36 112.2(4) . . ? C38 C37 C40 111.3(5) . . ? C36 C37 C40 106.6(4) . . ? C38 C37 C39 110.0(5) . . ? C36 C37 C39 108.5(4) . . ? C40 C37 C39 108.2(4) . . ? O17 C41 O18 125.6(4) . . ? O17 C41 C42 118.2(4) . . ? O18 C41 C42 116.2(4) . . ? C45 C42 C41 111.2(4) . . ? C45 C42 C44 110.2(4) . . ? C41 C42 C44 107.2(4) . . ? C45 C42 C43 110.6(4) . . ? C41 C42 C43 108.1(4) . . ? C44 C42 C43 109.3(4) . . ? O19 C46 O20 126.0(4) . . ? O19 C46 C47 119.6(8) . . ? O20 C46 C47 114.4(8) . . ? O19 C46 C47A 117.0(8) . . ? O20 C46 C47A 116.9(8) . . ? C47 C46 C47A 6.0(14) . . ? C49 C47 C46 109.3(13) . . ? C49 C47 C48 124.0(16) . . ? C46 C47 C48 110.7(15) . . ? C49 C47 C50 100.3(12) . . ? C46 C47 C50 106.7(15) . . ? C48 C47 C50 103.9(11) . . ? C49A C47A C48A 104.0(13) . . ? C49A C47A C46 115.2(14) . . ? C48A C47A C46 107.6(14) . . ? C49A C47A C50A 112.1(13) . . ? C48A C47A C50A 108.0(11) . . ? C46 C47A C50A 109.5(14) . . ? O21 C51 O22 126.3(4) . . ? O21 C51 C52 116.9(4) . . ? O22 C51 C52 116.7(4) . . ? C54 C52 C55 110.1(5) . . ? C54 C52 C53 110.0(4) . . ? C55 C52 C53 111.1(4) . . ? C54 C52 C51 105.9(4) . . ? C55 C52 C51 109.9(4) . . ? C53 C52 C51 109.7(4) . . ? O23 C56 O24 125.9(4) . . ? O23 C56 C57 117.3(4) . . ? O24 C56 C57 116.8(4) . . ? C59 C57 C56 111.4(5) . . ? C59 C57 C58 108.9(5) . . ? C56 C57 C58 106.1(4) . . ? C59 C57 C60 111.6(5) . . ? C56 C57 C60 108.9(4) . . ? C58 C57 C60 109.8(5) . . ? O26 C61 O25 125.9(4) . . ? O26 C61 C62 117.2(4) . . ? O25 C61 C62 116.9(4) . . ? C65 C62 C63 110.3(4) . . ? C65 C62 C61 108.9(4) . . ? C63 C62 C61 110.1(4) . . ? C65 C62 C64 109.2(4) . . ? C63 C62 C64 111.3(4) . . ? C61 C62 C64 107.0(4) . . ? O28 C66 O27 125.5(4) . . ? O28 C66 C67 117.5(4) . . ? O27 C66 C67 117.0(4) . . ? C68 C67 C66 111.2(4) . . ? C68 C67 C70 109.7(4) . . ? C66 C67 C70 106.4(4) . . ? C68 C67 C69 110.0(4) . . ? C66 C67 C69 109.1(4) . . ? C70 C67 C69 110.5(4) . . ? O30 C71 O29 126.3(4) . . ? O30 C71 C72 117.6(4) . . ? O29 C71 C72 116.1(4) . . ? C74 C72 C75 111.6(4) . . ? C74 C72 C71 109.8(4) . . ? C75 C72 C71 111.0(4) . . ? C74 C72 C73 109.9(4) . . ? C75 C72 C73 108.8(4) . . ? C71 C72 C73 105.6(4) . . ? O31 C76 O32 125.3(4) . . ? O31 C76 C77 117.6(4) . . ? O32 C76 C77 117.1(4) . . ? C79 C77 C80 111.6(5) . . ? C79 C77 C76 112.0(4) . . ? C80 C77 C76 110.9(4) . . ? C79 C77 C78 109.4(5) . . ? C80 C77 C78 107.6(5) . . ? C76 C77 C78 105.2(4) . . ? C91 N1 C90 111.6(5) . . ? C92 N2 C90 105.2(5) . . ? N1 C90 N2 106.8(5) . . ? N1 C91 C92 105.8(4) . . ? C91 C92 N2 110.5(4) . . ? C96 N3 C95 111.2(5) . . ? C95 N4 C97 106.1(5) . . ? N4 C95 N3 107.4(5) . . ? N3 C96 C97 102.4(5) . . ? N4 C97 C96 112.5(5) . . ? C100 C101 C102 62.7(8) . . ? C102 C104 C103 96.4(15) . . ? C102 C102 C104 113.6(11) 3_665 . ? C102 C102 C101 92.5(10) 3_665 . ? C104 C102 C101 22.1(7) . . ? 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 F8 Cr1 F1 Cr2 -124.85(14) . . . . ? O3 Cr1 F1 Cr2 55.63(15) . . . . ? O32 Cr1 F1 Cr2 145.70(15) . . . . ? O30 Cr1 F1 Cr2 -179(100) . . . . ? O1 Cr1 F1 Cr2 -35.31(15) . . . . ? F2 Cr2 F1 Cr1 144.41(14) . . . . ? O5 Cr2 F1 Cr1 79(4) . . . . ? O4 Cr2 F1 Cr1 -36.07(15) . . . . ? O7 Cr2 F1 Cr1 -122.76(15) . . . . ? O2 Cr2 F1 Cr1 55.40(15) . . . . ? F3 Cr3 F2 Cr2 -142.97(15) . . . . ? O11 Cr3 F2 Cr2 -74(2) . . . . ? O6 Cr3 F2 Cr2 37.08(16) . . . . ? O8 Cr3 F2 Cr2 -55.00(16) . . . . ? O9 Cr3 F2 Cr2 124.52(15) . . . . ? F1 Cr2 F2 Cr3 127.85(15) . . . . ? O5 Cr2 F2 Cr3 -53.80(16) . . . . ? O4 Cr2 F2 Cr3 -34(5) . . . . ? O7 Cr2 F2 Cr3 37.81(16) . . . . ? O2 Cr2 F2 Cr3 -143.15(16) . . . . ? F4 Cr4 F3 Cr3 143.05(15) . . . . ? O13 Cr4 F3 Cr3 80(5) . . . . ? O12 Cr4 F3 Cr3 -39.37(16) . . . . ? O10 Cr4 F3 Cr3 51.49(16) . . . . ? O15 Cr4 F3 Cr3 -126.13(16) . . . . ? F2 Cr3 F3 Cr4 -130.63(15) . . . . ? O11 Cr3 F3 Cr4 52.54(16) . . . . ? O6 Cr3 F3 Cr4 46(8) . . . . ? O8 Cr3 F3 Cr4 140.36(16) . . . . ? O9 Cr3 F3 Cr4 -39.67(16) . . . . ? F3 Cr4 F4 Cr5 130.37(15) . . . . ? O13 Cr4 F4 Cr5 -50.92(16) . . . . ? O12 Cr4 F4 Cr5 31(3) . . . . ? O10 Cr4 F4 Cr5 -138.96(16) . . . . ? O15 Cr4 F4 Cr5 41.85(16) . . . . ? F5 Cr5 F4 Cr4 -144.00(15) . . . . ? O19 Cr5 F4 Cr4 -176(59) . . . . ? O16 Cr5 F4 Cr4 -55.89(16) . . . . ? O14 Cr5 F4 Cr4 36.19(16) . . . . ? O17 Cr5 F4 Cr4 122.35(16) . . . . ? O19 Cr5 F5 Cr6 53.36(16) . . . . ? F4 Cr5 F5 Cr6 -125.65(15) . . . . ? O16 Cr5 F5 Cr6 144.17(15) . . . . ? O14 Cr5 F5 Cr6 -63(41) . . . . ? O17 Cr5 F5 Cr6 -35.79(16) . . . . ? F6 Cr6 F5 Cr5 143.55(14) . . . . ? O21 Cr6 F5 Cr5 73(3) . . . . ? O20 Cr6 F5 Cr5 -35.24(16) . . . . ? O23 Cr6 F5 Cr5 -124.93(15) . . . . ? O18 Cr6 F5 Cr5 55.73(16) . . . . ? F7 Cr7 F6 Cr6 -146.72(14) . . . . ? O22 Cr7 F6 Cr6 34.54(16) . . . . ? O27 Cr7 F6 Cr6 -115(5) . . . . ? O24 Cr7 F6 Cr6 -57.09(16) . . . . ? O25 Cr7 F6 Cr6 122.56(15) . . . . ? F5 Cr6 F6 Cr7 131.84(15) . . . . ? O21 Cr6 F6 Cr7 -50.43(16) . . . . ? O20 Cr6 F6 Cr7 -137(6) . . . . ? O23 Cr6 F6 Cr7 42.10(16) . . . . ? O18 Cr6 F6 Cr7 -139.84(16) . . . . ? F6 Cr7 F7 Cr8 -131.28(15) . . . . ? O22 Cr7 F7 Cr8 5(4) . . . . ? O27 Cr7 F7 Cr8 49.50(16) . . . . ? O24 Cr7 F7 Cr8 139.47(16) . . . . ? O25 Cr7 F7 Cr8 -43.35(15) . . . . ? F8 Cr8 F7 Cr7 143.85(15) . . . . ? O29 Cr8 F7 Cr7 104(11) . . . . ? O26 Cr8 F7 Cr7 56.56(15) . . . . ? O28 Cr8 F7 Cr7 -36.10(16) . . . . ? O31 Cr8 F7 Cr7 -123.56(15) . . . . ? F7 Cr8 F8 Cr1 128.79(14) . . . . ? O29 Cr8 F8 Cr1 -51.59(16) . . . . ? O26 Cr8 F8 Cr1 -141.77(15) . . . . ? O28 Cr8 F8 Cr1 -53(4) . . . . ? O31 Cr8 F8 Cr1 39.12(15) . . . . ? F1 Cr1 F8 Cr8 -145.40(15) . . . . ? O3 Cr1 F8 Cr8 -137.5(19) . . . . ? O32 Cr1 F8 Cr8 -56.05(16) . . . . ? O30 Cr1 F8 Cr8 33.95(16) . . . . ? O1 Cr1 F8 Cr8 120.82(15) . . . . ? F1 Cr1 O1 C1 -3.6(4) . . . . ? F8 Cr1 O1 C1 82.4(4) . . . . ? O3 Cr1 O1 C1 -94.1(4) . . . . ? O32 Cr1 O1 C1 158(2) . . . . ? O30 Cr1 O1 C1 175.9(4) . . . . ? F2 Cr2 O2 C1 -148.2(4) . . . . ? F1 Cr2 O2 C1 -59.0(4) . . . . ? O5 Cr2 O2 C1 121.7(4) . . . . ? O4 Cr2 O2 C1 33.3(4) . . . . ? O7 Cr2 O2 C1 4(4) . . . . ? F1 Cr1 O3 C6 -47.1(4) . . . . ? F8 Cr1 O3 C6 -55(2) . . . . ? O32 Cr1 O3 C6 -136.4(4) . . . . ? O30 Cr1 O3 C6 133.5(4) . . . . ? O1 Cr1 O3 C6 46.7(4) . . . . ? F2 Cr2 O4 C6 151(4) . . . . ? F1 Cr2 O4 C6 -11.8(4) . . . . ? O5 Cr2 O4 C6 169.8(4) . . . . ? O7 Cr2 O4 C6 78.1(4) . . . . ? O2 Cr2 O4 C6 -100.9(4) . . . . ? F2 Cr2 O5 C11 44.2(4) . . . . ? F1 Cr2 O5 C11 110(4) . . . . ? O4 Cr2 O5 C11 -135.3(4) . . . . ? O7 Cr2 O5 C11 -48.6(4) . . . . ? O2 Cr2 O5 C11 133.2(4) . . . . ? F2 Cr3 O6 C11 7.4(4) . . . . ? F3 Cr3 O6 C11 -170(57) . . . . ? O11 Cr3 O6 C11 -175.8(4) . . . . ? O8 Cr3 O6 C11 96.4(4) . . . . ? O9 Cr3 O6 C11 -83.6(4) . . . . ? F2 Cr2 O7 C16 1.9(4) . . . . ? F1 Cr2 O7 C16 -87.3(4) . . . . ? O5 Cr2 O7 C16 92.0(4) . . . . ? O4 Cr2 O7 C16 -179.6(4) . . . . ? O2 Cr2 O7 C16 -151(4) . . . . ? F2 Cr3 O8 C16 52.1(4) . . . . ? F3 Cr3 O8 C16 140.4(4) . . . . ? O11 Cr3 O8 C16 -129.0(4) . . . . ? O6 Cr3 O8 C16 -40.5(4) . . . . ? O9 Cr3 O8 C16 -36(20) . . . . ? F2 Cr3 O9 C21 96.4(4) . . . . ? F3 Cr3 O9 C21 8.0(4) . . . . ? O11 Cr3 O9 C21 -82.5(4) . . . . ? O6 Cr3 O9 C21 -171.0(4) . . . . ? O8 Cr3 O9 C21 -175(100) . . . . ? F4 Cr4 O10 C21 -133.2(4) . . . . ? F3 Cr4 O10 C21 -44.9(4) . . . . ? O13 Cr4 O10 C21 135.8(4) . . . . ? O12 Cr4 O10 C21 47.2(4) . . . . ? O15 Cr4 O10 C21 28(3) . . . . ? F2 Cr3 O11 C26 -102(2) . . . . ? F3 Cr3 O11 C26 -33.4(4) . . . . ? O6 Cr3 O11 C26 146.5(4) . . . . ? O8 Cr3 O11 C26 -121.3(4) . . . . ? O9 Cr3 O11 C26 59.1(4) . . . . ? F4 Cr4 O12 C26 92(3) . . . . ? F3 Cr4 O12 C26 -7.1(4) . . . . ? O13 Cr4 O12 C26 174.2(4) . . . . ? O10 Cr4 O12 C26 -97.8(4) . . . . ? O15 Cr4 O12 C26 81.4(4) . . . . ? F4 Cr4 O13 C31 41.0(4) . . . . ? F3 Cr4 O13 C31 104(5) . . . . ? O12 Cr4 O13 C31 -136.5(4) . . . . ? O10 Cr4 O13 C31 132.6(4) . . . . ? O15 Cr4 O13 C31 -49.8(4) . . . . ? F5 Cr5 O14 C31 -57(41) . . . . ? O19 Cr5 O14 C31 -173.1(4) . . . . ? F4 Cr5 O14 C31 5.9(4) . . . . ? O16 Cr5 O14 C31 96.1(4) . . . . ? O17 Cr5 O14 C31 -84.0(4) . . . . ? F4 Cr4 O15 C36 0.1(4) . . . . ? F3 Cr4 O15 C36 -88.1(4) . . . . ? O13 Cr4 O15 C36 91.2(4) . . . . ? O12 Cr4 O15 C36 179.7(4) . . . . ? O10 Cr4 O15 C36 -161(3) . . . . ? F5 Cr5 O16 C36 128.0(4) . . . . ? O19 Cr5 O16 C36 -140.5(4) . . . . ? F4 Cr5 O16 C36 41.1(4) . . . . ? O14 Cr5 O16 C36 -51.9(4) . . . . ? O17 Cr5 O16 C36 -53(4) . . . . ? F5 Cr5 O17 C41 0.4(4) . . . . ? O19 Cr5 O17 C41 -91.0(4) . . . . ? F4 Cr5 O17 C41 87.3(4) . . . . ? O16 Cr5 O17 C41 -178(100) . . . . ? O14 Cr5 O17 C41 -179.7(4) . . . . ? F6 Cr6 O18 C41 -149.3(4) . . . . ? F5 Cr6 O18 C41 -61.7(4) . . . . ? O21 Cr6 O18 C41 119.0(4) . . . . ? O20 Cr6 O18 C41 30.8(4) . . . . ? O23 Cr6 O18 C41 -80(4) . . . . ? F5 Cr5 O19 C46 -47.8(4) . . . . ? F4 Cr5 O19 C46 -16(4) . . . . ? O16 Cr5 O19 C46 -135.9(4) . . . . ? O14 Cr5 O19 C46 132.0(4) . . . . ? O17 Cr5 O19 C46 45.8(4) . . . . ? F6 Cr6 O20 C46 -97(6) . . . . ? F5 Cr6 O20 C46 -6.7(4) . . . . ? O21 Cr6 O20 C46 175.6(4) . . . . ? O23 Cr6 O20 C46 83.1(4) . . . . ? O18 Cr6 O20 C46 -95.0(4) . . . . ? F6 Cr6 O21 C51 42.1(4) . . . . ? F5 Cr6 O21 C51 113(3) . . . . ? O20 Cr6 O21 C51 -139.1(4) . . . . ? O23 Cr6 O21 C51 -49.5(4) . . . . ? O18 Cr6 O21 C51 129.8(4) . . . . ? F6 Cr7 O22 C51 7.0(4) . . . . ? F7 Cr7 O22 C51 -130(4) . . . . ? O27 Cr7 O22 C51 -173.7(4) . . . . ? O24 Cr7 O22 C51 96.4(4) . . . . ? O25 Cr7 O22 C51 -80.8(4) . . . . ? F6 Cr6 O23 C56 -2.1(4) . . . . ? F5 Cr6 O23 C56 -89.6(4) . . . . ? O21 Cr6 O23 C56 89.7(4) . . . . ? O20 Cr6 O23 C56 177.9(4) . . . . ? O18 Cr6 O23 C56 -71(4) . . . . ? F6 Cr7 O24 C56 48.0(4) . . . . ? F7 Cr7 O24 C56 135.4(4) . . . . ? O22 Cr7 O24 C56 -45.9(4) . . . . ? O27 Cr7 O24 C56 -133.2(4) . . . . ? O25 Cr7 O24 C56 41(3) . . . . ? F6 Cr7 O25 C61 87.0(4) . . . . ? F7 Cr7 O25 C61 -0.3(4) . . . . ? O22 Cr7 O25 C61 -178.9(4) . . . . ? O27 Cr7 O25 C61 -91.7(4) . . . . ? O24 Cr7 O25 C61 94(3) . . . . ? F8 Cr8 O26 C61 -127.7(4) . . . . ? F7 Cr8 O26 C61 -39.5(4) . . . . ? O29 Cr8 O26 C61 140.9(4) . . . . ? O28 Cr8 O26 C61 53.8(4) . . . . ? O31 Cr8 O26 C61 -47(8) . . . . ? F6 Cr7 O27 C66 -72(5) . . . . ? F7 Cr7 O27 C66 -40.1(4) . . . . ? O22 Cr7 O27 C66 138.6(4) . . . . ? O24 Cr7 O27 C66 -129.7(4) . . . . ? O25 Cr7 O27 C66 50.6(4) . . . . ? F8 Cr8 O28 C66 179(100) . . . . ? F7 Cr8 O28 C66 -2.6(4) . . . . ? O29 Cr8 O28 C66 177.8(4) . . . . ? O26 Cr8 O28 C66 -92.1(4) . . . . ? O31 Cr8 O28 C66 87.0(4) . . . . ? F8 Cr8 O29 C71 47.1(4) . . . . ? F7 Cr8 O29 C71 87(11) . . . . ? O26 Cr8 O29 C71 134.4(4) . . . . ? O28 Cr8 O29 C71 -133.0(4) . . . . ? O31 Cr8 O29 C71 -45.5(4) . . . . ? F1 Cr1 O30 C71 62(9) . . . . ? F8 Cr1 O30 C71 7.6(4) . . . . ? O3 Cr1 O30 C71 -173.0(4) . . . . ? O32 Cr1 O30 C71 97.0(4) . . . . ? O1 Cr1 O30 C71 -82.0(4) . . . . ? F8 Cr8 O31 C76 0.1(4) . . . . ? F7 Cr8 O31 C76 -88.1(4) . . . . ? O29 Cr8 O31 C76 91.5(4) . . . . ? O26 Cr8 O31 C76 -80(8) . . . . ? O28 Cr8 O31 C76 178.6(4) . . . . ? F1 Cr1 O32 C76 137.4(3) . . . . ? F8 Cr1 O32 C76 51.4(3) . . . . ? O3 Cr1 O32 C76 -132.1(4) . . . . ? O30 Cr1 O32 C76 -42.1(4) . . . . ? O1 Cr1 O32 C76 -24(2) . . . . ? Cr2 O2 C1 O1 35.2(6) . . . . ? Cr2 O2 C1 C2 -137.7(5) . . . . ? Cr2 O2 C1 C2A -151.9(5) . . . . ? Cr1 O1 C1 O2 4.6(7) . . . . ? Cr1 O1 C1 C2 177.5(5) . . . . ? Cr1 O1 C1 C2A -168.5(5) . . . . ? O2 C1 C2 C5 -58.0(10) . . . . ? O1 C1 C2 C5 128.5(8) . . . . ? C2A C1 C2 C5 47(3) . . . . ? O2 C1 C2 C3 175.5(7) . . . . ? O1 C1 C2 C3 2.0(10) . . . . ? C2A C1 C2 C3 -79(3) . . . . ? O2 C1 C2 C4 58.9(9) . . . . ? O1 C1 C2 C4 -114.6(7) . . . . ? C2A C1 C2 C4 164(4) . . . . ? O2 C1 C2A C3A 137.9(7) . . . . ? O1 C1 C2A C3A -48.5(9) . . . . ? C2 C1 C2A C3A 56(3) . . . . ? O2 C1 C2A C4A 13.6(10) . . . . ? O1 C1 C2A C4A -172.8(7) . . . . ? C2 C1 C2A C4A -68(3) . . . . ? O2 C1 C2A C5A -104.1(8) . . . . ? O1 C1 C2A C5A 69.6(8) . . . . ? C2 C1 C2A C5A 174(4) . . . . ? Cr1 O3 C6 O4 12.4(6) . . . . ? Cr1 O3 C6 C7 -165.6(3) . . . . ? Cr2 O4 C6 O3 26.2(7) . . . . ? Cr2 O4 C6 C7 -155.8(3) . . . . ? O3 C6 C7 C9 -50.5(6) . . . . ? O4 C6 C7 C9 131.4(5) . . . . ? O3 C6 C7 C10 -171.6(5) . . . . ? O4 C6 C7 C10 10.2(7) . . . . ? O3 C6 C7 C8 67.5(6) . . . . ? O4 C6 C7 C8 -110.6(5) . . . . ? Cr2 O5 C11 O6 -12.5(6) . . . . ? Cr2 O5 C11 C12 169.2(3) . . . . ? Cr3 O6 C11 O5 -21.6(6) . . . . ? Cr3 O6 C11 C12 156.8(3) . . . . ? O5 C11 C12 C13 75.6(5) . . . . ? O6 C11 C12 C13 -102.9(5) . . . . ? O5 C11 C12 C15 -164.3(4) . . . . ? O6 C11 C12 C15 17.2(6) . . . . ? O5 C11 C12 C14 -41.7(5) . . . . ? O6 C11 C12 C14 139.8(4) . . . . ? Cr2 O7 C16 O8 -8.1(7) . . . . ? Cr2 O7 C16 C17A 178.4(6) . . . . ? Cr2 O7 C16 C17 172.3(6) . . . . ? Cr3 O8 C16 O7 -26.9(6) . . . . ? Cr3 O8 C16 C17A 146.8(6) . . . . ? Cr3 O8 C16 C17 152.7(6) . . . . ? O7 C16 C17 C19 -169.3(9) . . . . ? O8 C16 C17 C19 11.0(13) . . . . ? C17A C16 C17 C19 78(10) . . . . ? O7 C16 C17 C20 70.3(11) . . . . ? O8 C16 C17 C20 -109.4(10) . . . . ? C17A C16 C17 C20 -42(10) . . . . ? O7 C16 C17 C18 -46.8(11) . . . . ? O8 C16 C17 C18 133.6(8) . . . . ? C17A C16 C17 C18 -159(11) . . . . ? O7 C16 C17A C18A -24.2(13) . . . . ? O8 C16 C17A C18A 161.6(8) . . . . ? C17 C16 C17A C18A 46(10) . . . . ? O7 C16 C17A C19A -150.1(9) . . . . ? O8 C16 C17A C19A 35.7(13) . . . . ? C17 C16 C17A C19A -80(10) . . . . ? O7 C16 C17A C20A 91.7(9) . . . . ? O8 C16 C17A C20A -82.5(9) . . . . ? C17 C16 C17A C20A 162(11) . . . . ? Cr3 O9 C21 O10 -0.3(7) . . . . ? Cr3 O9 C21 C22 180.0(6) . . . . ? Cr3 O9 C21 C22A 175.9(6) . . . . ? Cr4 O10 C21 O9 24.3(7) . . . . ? Cr4 O10 C21 C22 -156.0(6) . . . . ? Cr4 O10 C21 C22A -152.2(6) . . . . ? O9 C21 C22 C23 -88.2(10) . . . . ? O10 C21 C22 C23 92.1(10) . . . . ? C22A C21 C22 C23 37(13) . . . . ? O9 C21 C22 C25 35.8(12) . . . . ? O10 C21 C22 C25 -144.0(8) . . . . ? C22A C21 C22 C25 161(14) . . . . ? O9 C21 C22 C24 153.5(8) . . . . ? O10 C21 C22 C24 -26.2(12) . . . . ? C22A C21 C22 C24 -81(13) . . . . ? O9 C21 C22A C25A 7.7(12) . . . . ? O10 C21 C22A C25A -175.7(8) . . . . ? C22 C21 C22A C25A -49(13) . . . . ? O9 C21 C22A C24A 126.5(8) . . . . ? O10 C21 C22A C24A -56.9(10) . . . . ? C22 C21 C22A C24A 70(13) . . . . ? O9 C21 C22A C23A -116.5(9) . . . . ? O10 C21 C22A C23A 60.2(10) . . . . ? C22 C21 C22A C23A -173(14) . . . . ? Cr3 O11 C26 O12 -2.6(7) . . . . ? Cr3 O11 C26 C27 176.1(3) . . . . ? Cr4 O12 C26 O11 29.9(7) . . . . ? Cr4 O12 C26 C27 -148.9(3) . . . . ? O11 C26 C27 C28 -60.8(5) . . . . ? O12 C26 C27 C28 118.0(4) . . . . ? O11 C26 C27 C29 179.8(4) . . . . ? O12 C26 C27 C29 -1.3(6) . . . . ? O11 C26 C27 C30 58.3(5) . . . . ? O12 C26 C27 C30 -122.8(4) . . . . ? Cr5 O14 C31 O13 -20.8(7) . . . . ? Cr5 O14 C31 C32A 160.0(7) . . . . ? Cr5 O14 C31 C32 161.8(7) . . . . ? Cr4 O13 C31 O14 -10.0(7) . . . . ? Cr4 O13 C31 C32A 169.3(7) . . . . ? Cr4 O13 C31 C32 167.4(7) . . . . ? O14 C31 C32 C34 -145.9(8) . . . . ? O13 C31 C32 C34 36.5(12) . . . . ? C32A C31 C32 C34 -16(31) . . . . ? O14 C31 C32 C33 -21.1(13) . . . . ? O13 C31 C32 C33 161.2(8) . . . . ? C32A C31 C32 C33 109(32) . . . . ? O14 C31 C32 C35 96.6(9) . . . . ? O13 C31 C32 C35 -81.0(10) . . . . ? C32A C31 C32 C35 -134(32) . . . . ? O14 C31 C32A C34A -121.4(9) . . . . ? O13 C31 C32A C34A 59.2(12) . . . . ? C32 C31 C32A C34A -172(32) . . . . ? O14 C31 C32A C33A 1.1(13) . . . . ? O13 C31 C32A C33A -178.2(8) . . . . ? C32 C31 C32A C33A -50(31) . . . . ? O14 C31 C32A C35A 117.4(9) . . . . ? O13 C31 C32A C35A -61.9(11) . . . . ? C32 C31 C32A C35A 66(31) . . . . ? Cr4 O15 C36 O16 -16.3(7) . . . . ? Cr4 O15 C36 C37 163.5(3) . . . . ? Cr5 O16 C36 O15 -11.4(7) . . . . ? Cr5 O16 C36 C37 168.8(3) . . . . ? O15 C36 C37 C38 173.1(5) . . . . ? O16 C36 C37 C38 -7.1(7) . . . . ? O15 C36 C37 C40 -64.8(5) . . . . ? O16 C36 C37 C40 115.0(5) . . . . ? O15 C36 C37 C39 51.4(5) . . . . ? O16 C36 C37 C39 -128.7(4) . . . . ? Cr5 O17 C41 O18 -3.7(7) . . . . ? Cr5 O17 C41 C42 177.3(3) . . . . ? Cr6 O18 C41 O17 42.6(6) . . . . ? Cr6 O18 C41 C42 -138.4(3) . . . . ? O17 C41 C42 C45 -4.6(6) . . . . ? O18 C41 C42 C45 176.3(4) . . . . ? O17 C41 C42 C44 116.0(5) . . . . ? O18 C41 C42 C44 -63.1(5) . . . . ? O17 C41 C42 C43 -126.3(5) . . . . ? O18 C41 C42 C43 54.6(5) . . . . ? Cr5 O19 C46 O20 18.6(7) . . . . ? Cr5 O19 C46 C47 -162.9(9) . . . . ? Cr5 O19 C46 C47A -156.7(8) . . . . ? Cr6 O20 C46 O19 16.8(7) . . . . ? Cr6 O20 C46 C47 -161.8(8) . . . . ? Cr6 O20 C46 C47A -167.9(8) . . . . ? O19 C46 C47 C49 -12.1(14) . . . . ? O20 C46 C47 C49 166.5(9) . . . . ? C47A C46 C47 C49 -78(12) . . . . ? O19 C46 C47 C48 127.8(10) . . . . ? O20 C46 C47 C48 -53.6(14) . . . . ? C47A C46 C47 C48 62(12) . . . . ? O19 C46 C47 C50 -119.7(9) . . . . ? O20 C46 C47 C50 58.9(12) . . . . ? C47A C46 C47 C50 175(13) . . . . ? O19 C46 C47A C49A -8.2(15) . . . . ? O20 C46 C47A C49A 176.0(9) . . . . ? C47 C46 C47A C49A 109(12) . . . . ? O19 C46 C47A C48A 107.2(10) . . . . ? O20 C46 C47A C48A -68.6(13) . . . . ? C47 C46 C47A C48A -135(12) . . . . ? O19 C46 C47A C50A -135.7(9) . . . . ? O20 C46 C47A C50A 48.5(13) . . . . ? C47 C46 C47A C50A -18(11) . . . . ? Cr6 O21 C51 O22 -11.7(7) . . . . ? Cr6 O21 C51 C52 168.9(3) . . . . ? Cr7 O22 C51 O21 -20.6(7) . . . . ? Cr7 O22 C51 C52 158.8(3) . . . . ? O21 C51 C52 C54 94.3(5) . . . . ? O22 C51 C52 C54 -85.2(5) . . . . ? O21 C51 C52 C55 -24.6(6) . . . . ? O22 C51 C52 C55 155.9(5) . . . . ? O21 C51 C52 C53 -147.0(4) . . . . ? O22 C51 C52 C53 33.5(6) . . . . ? Cr6 O23 C56 O24 -9.2(8) . . . . ? Cr6 O23 C56 C57 174.0(3) . . . . ? Cr7 O24 C56 O23 -20.8(7) . . . . ? Cr7 O24 C56 C57 156.1(4) . . . . ? O23 C56 C57 C59 -13.9(7) . . . . ? O24 C56 C57 C59 169.0(5) . . . . ? O23 C56 C57 C58 104.5(5) . . . . ? O24 C56 C57 C58 -72.7(6) . . . . ? O23 C56 C57 C60 -137.5(5) . . . . ? O24 C56 C57 C60 45.4(6) . . . . ? Cr8 O26 C61 O25 7.6(6) . . . . ? Cr8 O26 C61 C62 -176.0(3) . . . . ? Cr7 O25 C61 O26 19.1(7) . . . . ? Cr7 O25 C61 C62 -157.3(3) . . . . ? O26 C61 C62 C65 135.0(4) . . . . ? O25 C61 C62 C65 -48.3(5) . . . . ? O26 C61 C62 C63 14.0(6) . . . . ? O25 C61 C62 C63 -169.3(4) . . . . ? O26 C61 C62 C64 -107.1(5) . . . . ? O25 C61 C62 C64 69.6(5) . . . . ? Cr8 O28 C66 O27 16.0(7) . . . . ? Cr8 O28 C66 C67 -161.3(3) . . . . ? Cr7 O27 C66 O28 12.1(7) . . . . ? Cr7 O27 C66 C67 -170.6(3) . . . . ? O28 C66 C67 C68 -14.2(6) . . . . ? O27 C66 C67 C68 168.3(4) . . . . ? O28 C66 C67 C70 105.1(4) . . . . ? O27 C66 C67 C70 -72.4(5) . . . . ? O28 C66 C67 C69 -135.7(4) . . . . ? O27 C66 C67 C69 46.8(5) . . . . ? Cr1 O30 C71 O29 -17.6(7) . . . . ? Cr1 O30 C71 C72 164.5(3) . . . . ? Cr8 O29 C71 O30 -17.7(6) . . . . ? Cr8 O29 C71 C72 160.3(3) . . . . ? O30 C71 C72 C74 -41.3(6) . . . . ? O29 C71 C72 C74 140.5(4) . . . . ? O30 C71 C72 C75 -165.2(4) . . . . ? O29 C71 C72 C75 16.7(6) . . . . ? O30 C71 C72 C73 77.1(5) . . . . ? O29 C71 C72 C73 -101.0(5) . . . . ? Cr8 O31 C76 O32 -7.3(7) . . . . ? Cr8 O31 C76 C77 174.6(3) . . . . ? Cr1 O32 C76 O31 -26.2(6) . . . . ? Cr1 O32 C76 C77 151.9(3) . . . . ? O31 C76 C77 C79 -19.5(7) . . . . ? O32 C76 C77 C79 162.3(5) . . . . ? O31 C76 C77 C80 -144.9(4) . . . . ? O32 C76 C77 C80 36.9(6) . . . . ? O31 C76 C77 C78 99.2(5) . . . . ? O32 C76 C77 C78 -79.0(5) . . . . ? C91 N1 C90 N2 3.0(7) . . . . ? C92 N2 C90 N1 -2.3(6) . . . . ? C90 N1 C91 C92 -2.4(7) . . . . ? N1 C91 C92 N2 0.9(6) . . . . ? C90 N2 C92 C91 0.9(6) . . . . ? C97 N4 C95 N3 1.2(9) . . . . ? C96 N3 C95 N4 -4.9(9) . . . . ? C95 N3 C96 C97 6.2(9) . . . . ? C95 N4 C97 C96 2.8(10) . . . . ? N3 C96 C97 N4 -5.6(10) . . . . ? C103 C104 C102 C102 -175.9(13) . . . 3_665 ? C103 C104 C102 C101 166(4) . . . . ? C100 C101 C102 C102 -176.2(14) . . . 3_665 ? C100 C101 C102 C104 -12(3) . . . . ? 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 N3 H3 F1 0.86 2.50 2.917(6) 110.4 . N1 H1 F8 0.86 2.43 2.960(5) 120.4 . _diffrn_measured_fraction_theta_max .997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full .997 _refine_diff_density_max 1.508 _refine_diff_density_min -.725 _refine_diff_density_rms .101