Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jorg Sundermeyer' _publ_contact_author_address ; Fachbereich Chemie Philipps-Universit\"at Marburg 35032 GERMANY ; _publ_contact_author_email JSU@CHEMIE.UNI-MARBURG.DE _publ_section_title ; A series of metal complexes with the non-innocent N,N'-bis(pentafluorophenyl)-o-phenylenediamido ligand: twisted geometry for tuning the electronic structure ; loop_ _publ_author_name 'Jorg Sundermeyer' 'Olaf Burghaus' 'Carole Duboc' 'Jan Fiedler' 'Klaus Harms' W.Kaim ; M.Khusniyarov ; 'Biprajit Sarkar' 'J.van Slageren' # Attachment 'dalton B714974C-Khusniyarov-Sundermeyer-corrected.cif' data_no_1 _database_code_depnum_ccdc_archive 'CCDC 662503' #data_analytical (mk01) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H8 F20 N4 Ni, C4H8O, 0.5(C4 H8 O)' _chemical_formula_sum 'C42 H20 F20 N4 Ni O1.50' _chemical_formula_weight 1043.33 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' F F 0.0171 0.0103 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 58.619(3) _cell_length_b 15.3293(6) _cell_length_c 8.6322(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.288(3) _cell_angle_gamma 90.00 _cell_volume 7694.1(6) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 35506 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 25 _exptl_crystal_description irregular _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.801 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4160 _exptl_absorpt_coefficient_mu 0.647 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.7725 _exptl_absorpt_correction_T_max 0.8979 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -26 3 0 0.1550 -17 11 5 0.1390 18 9 1 0.1830 -30 19 -15 0.2310 -18 -28 5 0.2080 22 1 4 0.1890 15 -2 -1 0.2350 27 4 5 0.1500 -29 10 -1 0.1280 -22 0 -1 0.1500 21 9 -1 0.2190 -17 -8 -1 0.0680 1 -21 -5 0.0900 _exptl_absorpt_process_details ; (see. N.W. Alcock (1970). Cryst. Computing, p271) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 IPDS-II _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 42093 _diffrn_reflns_av_R_equivalents 0.0998 _diffrn_reflns_av_sigmaI/netI 0.0567 _diffrn_reflns_limit_h_min -69 _diffrn_reflns_limit_h_max 69 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6746 _reflns_number_gt 4771 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0892P)^2^+5.0950P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00156(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6746 _refine_ls_number_parameters 687 _refine_ls_number_restraints 326 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1545 _refine_ls_wR_factor_gt 0.1413 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.035 _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 C1 C 0.38026(7) 0.4269(3) 0.6225(5) 0.0370(9) Uani 1 1 d . . . C2 C 0.38481(8) 0.5174(3) 0.6521(6) 0.0460(11) Uani 1 1 d . . . H2 H 0.3991 0.5351 0.7069 0.055 Uiso 1 1 calc R . . C3 C 0.36875(9) 0.5776(3) 0.6020(7) 0.0583(14) Uani 1 1 d . . . H3 H 0.3717 0.6375 0.6251 0.070 Uiso 1 1 calc R . . C4 C 0.34752(9) 0.5527(3) 0.5152(7) 0.0625(15) Uani 1 1 d . . . H4 H 0.3369 0.5962 0.4743 0.075 Uiso 1 1 calc R . . C5 C 0.34235(8) 0.4675(3) 0.4905(6) 0.0500(12) Uani 1 1 d . . . H5 H 0.3280 0.4513 0.4344 0.060 Uiso 1 1 calc R . . C6 C 0.35823(8) 0.4026(3) 0.5478(5) 0.0411(10) Uani 1 1 d . . . C7 C 0.41769(7) 0.3720(2) 0.7207(5) 0.0326(9) Uani 1 1 d . . . C8 C 0.42803(7) 0.3235(3) 0.8475(5) 0.0365(9) Uani 1 1 d . . . C9 C 0.45117(8) 0.3288(3) 0.9008(5) 0.0396(10) Uani 1 1 d . . . C10 C 0.46494(7) 0.3855(3) 0.8301(5) 0.0414(10) Uani 1 1 d . . . C11 C 0.45561(7) 0.4338(3) 0.7028(5) 0.0375(9) Uani 1 1 d . . . C12 C 0.43261(7) 0.4253(2) 0.6486(5) 0.0338(9) Uani 1 1 d . . . C13 C 0.33369(7) 0.2799(3) 0.4742(5) 0.0394(10) Uani 1 1 d . . . C14 C 0.31380(8) 0.2984(3) 0.5422(6) 0.0449(11) Uani 1 1 d . . . C15 C 0.29309(8) 0.2615(3) 0.4913(7) 0.0560(13) Uani 1 1 d . . . C16 C 0.29155(9) 0.2004(4) 0.3721(7) 0.0626(15) Uani 1 1 d . . . C17 C 0.31068(10) 0.1787(3) 0.3081(6) 0.0550(13) Uani 1 1 d . . . C18 C 0.33154(8) 0.2183(3) 0.3568(6) 0.0433(11) Uani 1 1 d . . . C19 C 0.38308(8) 0.0668(3) 0.6384(5) 0.0386(10) Uani 1 1 d . . . C20 C 0.37858(9) -0.0227(3) 0.6680(6) 0.0473(11) Uani 1 1 d . . . H20 H 0.3653 -0.0384 0.7145 0.057 Uiso 1 1 calc R . . C21 C 0.39302(9) -0.0845(3) 0.6303(6) 0.0518(12) Uani 1 1 d . . . H21 H 0.3900 -0.1438 0.6527 0.062 Uiso 1 1 calc R . . C22 C 0.41282(9) -0.0635(3) 0.5571(6) 0.0543(13) Uani 1 1 d . . . H22 H 0.4224 -0.1088 0.5266 0.065 Uiso 1 1 calc R . . C23 C 0.41810(8) 0.0216(3) 0.5307(6) 0.0473(11) Uani 1 1 d . . . H23 H 0.4316 0.0354 0.4850 0.057 Uiso 1 1 calc R . . C24 C 0.40352(8) 0.0889(3) 0.5715(5) 0.0387(10) Uani 1 1 d . . . C25 C 0.34908(8) 0.1300(3) 0.7234(5) 0.0414(10) Uani 1 1 d . . . C26 C 0.34409(9) 0.1840(3) 0.8437(6) 0.0478(11) Uani 1 1 d . . . C27 C 0.32255(10) 0.1901(3) 0.8897(6) 0.0542(13) Uani 1 1 d . . . C28 C 0.30494(9) 0.1402(4) 0.8175(7) 0.0595(14) Uani 1 1 d . . . C29 C 0.30896(8) 0.0859(3) 0.6982(7) 0.0539(13) Uani 1 1 d . . . C30 C 0.33069(8) 0.0810(3) 0.6498(6) 0.0443(11) Uani 1 1 d . . . C31 C 0.42542(7) 0.2101(2) 0.4932(5) 0.0357(9) Uani 1 1 d . . . C32 C 0.44776(8) 0.1971(3) 0.5670(5) 0.0388(10) Uani 1 1 d . . . C33 C 0.46657(8) 0.2383(3) 0.5181(6) 0.0443(10) Uani 1 1 d . . . C34 C 0.46335(8) 0.2975(3) 0.3967(5) 0.0424(10) Uani 1 1 d . . . C35 C 0.44153(8) 0.3143(3) 0.3245(5) 0.0393(10) Uani 1 1 d . . . C36 C 0.42315(7) 0.2708(2) 0.3713(5) 0.0350(9) Uani 1 1 d . . . F8 F 0.41506(5) 0.26899(16) 0.9206(3) 0.0490(6) Uani 1 1 d . . . F9 F 0.46057(5) 0.27820(19) 1.0184(3) 0.0542(7) Uani 1 1 d . . . F10 F 0.48723(4) 0.39284(19) 0.8839(3) 0.0556(7) Uani 1 1 d . . . F11 F 0.46904(4) 0.48550(17) 0.6292(3) 0.0519(7) Uani 1 1 d . . . F12 F 0.42482(4) 0.46831(15) 0.5160(3) 0.0441(6) Uani 1 1 d . . . F14 F 0.31480(5) 0.35366(19) 0.6641(3) 0.0582(7) Uani 1 1 d . . . F15 F 0.27443(6) 0.2808(3) 0.5597(5) 0.0839(11) Uani 1 1 d . . . F16 F 0.27131(6) 0.1619(3) 0.3226(5) 0.0889(12) Uani 1 1 d . . . F17 F 0.30972(6) 0.1167(2) 0.1963(4) 0.0737(10) Uani 1 1 d . . . F18 F 0.35000(5) 0.19525(18) 0.2897(3) 0.0569(7) Uani 1 1 d . . . F26 F 0.36075(5) 0.23509(17) 0.9183(3) 0.0566(7) Uani 1 1 d . . . F27 F 0.31861(6) 0.2473(2) 1.0017(4) 0.0720(9) Uani 1 1 d . . . F28 F 0.28383(6) 0.1463(3) 0.8583(5) 0.0847(11) Uani 1 1 d . . . F29 F 0.29167(5) 0.04073(19) 0.6164(5) 0.0729(10) Uani 1 1 d . . . F30 F 0.33355(5) 0.03204(17) 0.5233(3) 0.0548(7) Uani 1 1 d . . . F32 F 0.45133(5) 0.14484(17) 0.6934(3) 0.0498(6) Uani 1 1 d . . . F33 F 0.48756(5) 0.2236(2) 0.5928(4) 0.0598(8) Uani 1 1 d . . . F34 F 0.48135(5) 0.3393(2) 0.3498(3) 0.0595(8) Uani 1 1 d . . . F35 F 0.43807(5) 0.37423(16) 0.2118(3) 0.0477(6) Uani 1 1 d . . . F36 F 0.40208(4) 0.28924(16) 0.2984(3) 0.0447(6) Uani 1 1 d . . . N1 N 0.39445(6) 0.3585(2) 0.6629(4) 0.0354(8) Uani 1 1 d . . . N2 N 0.35548(6) 0.3146(2) 0.5309(4) 0.0386(8) Uani 1 1 d . . . N3 N 0.37070(6) 0.1377(2) 0.6704(4) 0.0394(8) Uani 1 1 d . . . N4 N 0.40552(6) 0.1762(2) 0.5467(4) 0.0367(8) Uani 1 1 d . . . Ni1 Ni 0.381684(9) 0.24658(3) 0.60671(6) 0.03446(18) Uani 1 1 d . . . O700 O 0.2701(5) 0.4546(16) 0.270(3) 0.242(8) Uani 0.50 1 d PDU A 2 C701 C 0.2871(5) 0.401(2) 0.203(3) 0.240(10) Uani 0.50 1 d PDU A 2 H70A H 0.2939 0.3571 0.2799 0.288 Uiso 0.50 1 calc PR A 2 H70B H 0.2996 0.4374 0.1708 0.288 Uiso 0.50 1 calc PR A 2 C702 C 0.2739(8) 0.355(2) 0.061(4) 0.247(10) Uani 0.50 1 d PDU A 2 H70C H 0.2842 0.3338 -0.0130 0.296 Uiso 0.50 1 calc PR A 2 H70D H 0.2641 0.3073 0.0910 0.296 Uiso 0.50 1 calc PR A 2 C703 C 0.2602(6) 0.435(2) 0.001(3) 0.231(9) Uani 0.50 1 d PDU A 2 H70I H 0.2677 0.4639 -0.0817 0.277 Uiso 0.50 1 calc PR A 2 H70J H 0.2445 0.4171 -0.0449 0.277 Uiso 0.50 1 calc PR A 2 C704 C 0.2587(7) 0.497(2) 0.133(4) 0.261(11) Uani 0.50 1 d PDU A 2 H70K H 0.2664 0.5525 0.1142 0.313 Uiso 0.50 1 calc PR A 2 H70L H 0.2425 0.5090 0.1454 0.313 Uiso 0.50 1 calc PR A 2 O800 O 0.4917(4) -0.0038(17) 0.383(4) 0.337(14) Uani 0.50 1 d PDU B -1 C801 C 0.5147(4) 0.034(2) 0.403(4) 0.290(15) Uani 0.50 1 d PDU B -1 H80A H 0.5263 -0.0132 0.4239 0.348 Uiso 0.50 1 calc PR B -1 H80B H 0.5163 0.0742 0.4928 0.348 Uiso 0.50 1 calc PR B -1 C802 C 0.5183(4) 0.083(2) 0.253(5) 0.276(14) Uani 0.50 1 d PDU B -1 H80C H 0.5292 0.1321 0.2740 0.331 Uiso 0.50 1 calc PR B -1 H80D H 0.5239 0.0434 0.1743 0.331 Uiso 0.50 1 calc PR B -1 C803 C 0.4936(4) 0.114(2) 0.200(4) 0.254(13) Uani 0.50 1 d PDU B -1 H80E H 0.4925 0.1782 0.2148 0.305 Uiso 0.50 1 calc PR B -1 H80F H 0.4890 0.1006 0.0887 0.305 Uiso 0.50 1 calc PR B -1 C804 C 0.4782(5) 0.066(2) 0.304(5) 0.287(14) Uani 0.50 1 d PDU B -1 H80G H 0.4729 0.1064 0.3809 0.344 Uiso 0.50 1 calc PR B -1 H80H H 0.4645 0.0417 0.2386 0.344 Uiso 0.50 1 calc PR B -1 O900 O 0.2872(5) 0.4502(19) 0.153(3) 0.269(9) Uani 0.50 1 d PDU C 1 C901 C 0.2773(8) 0.5028(19) 0.019(3) 0.281(11) Uani 0.50 1 d PDU C 1 H90A H 0.2877 0.5515 0.0002 0.338 Uiso 0.50 1 calc PR C 1 H90B H 0.2622 0.5268 0.0366 0.338 Uiso 0.50 1 calc PR C 1 C902 C 0.2750(7) 0.4387(19) -0.115(3) 0.276(11) Uani 0.50 1 d PDU C 1 H90C H 0.2900 0.4218 -0.1475 0.331 Uiso 0.50 1 calc PR C 1 H90D H 0.2645 0.4599 -0.2065 0.331 Uiso 0.50 1 calc PR C 1 C903 C 0.2642(8) 0.366(2) -0.025(4) 0.268(11) Uani 0.50 1 d PDU C 1 H90E H 0.2472 0.3689 -0.0465 0.322 Uiso 0.50 1 calc PR C 1 H90F H 0.2692 0.3083 -0.0599 0.322 Uiso 0.50 1 calc PR C 1 C904 C 0.2717(8) 0.377(3) 0.147(4) 0.257(10) Uani 0.50 1 d PDU C 1 H90G H 0.2585 0.3900 0.2034 0.309 Uiso 0.50 1 calc PR C 1 H90H H 0.2797 0.3245 0.1920 0.309 Uiso 0.50 1 calc PR C 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 C1 0.037(2) 0.029(2) 0.044(2) -0.0001(18) 0.0010(18) 0.0026(17) C2 0.044(3) 0.030(2) 0.061(3) -0.006(2) -0.009(2) 0.0018(18) C3 0.058(3) 0.027(2) 0.085(4) -0.005(2) -0.011(3) 0.002(2) C4 0.049(3) 0.034(2) 0.098(4) 0.005(3) -0.016(3) 0.005(2) C5 0.043(3) 0.034(2) 0.068(3) 0.000(2) -0.011(2) 0.0017(19) C6 0.042(2) 0.029(2) 0.051(3) -0.0013(19) 0.000(2) -0.0006(17) C7 0.037(2) 0.0216(18) 0.038(2) -0.0033(16) 0.0026(17) -0.0010(15) C8 0.040(2) 0.029(2) 0.039(2) 0.0016(17) 0.0025(18) -0.0005(17) C9 0.046(3) 0.043(2) 0.029(2) 0.0040(18) 0.0006(18) 0.0108(19) C10 0.032(2) 0.047(2) 0.044(3) -0.008(2) 0.0032(18) 0.0043(18) C11 0.038(2) 0.033(2) 0.043(2) -0.0013(18) 0.0109(18) -0.0005(17) C12 0.043(2) 0.0250(18) 0.032(2) -0.0030(16) 0.0004(17) 0.0017(16) C13 0.038(2) 0.0281(19) 0.049(3) 0.0008(18) -0.0050(19) -0.0024(17) C14 0.045(3) 0.038(2) 0.052(3) -0.002(2) 0.004(2) 0.0004(19) C15 0.039(3) 0.059(3) 0.069(3) 0.010(3) 0.000(2) -0.002(2) C16 0.042(3) 0.068(4) 0.075(4) 0.003(3) -0.006(3) -0.016(2) C17 0.066(3) 0.038(2) 0.057(3) -0.003(2) -0.008(2) -0.016(2) C18 0.046(3) 0.033(2) 0.049(3) -0.0010(19) -0.002(2) 0.0008(18) C19 0.048(3) 0.027(2) 0.038(2) -0.0005(17) -0.0037(19) -0.0018(18) C20 0.055(3) 0.029(2) 0.056(3) 0.008(2) -0.004(2) -0.007(2) C21 0.059(3) 0.025(2) 0.067(3) 0.003(2) -0.011(2) -0.002(2) C22 0.063(3) 0.028(2) 0.068(3) -0.008(2) -0.003(3) 0.008(2) C23 0.049(3) 0.033(2) 0.058(3) -0.002(2) 0.001(2) 0.0041(19) C24 0.050(3) 0.027(2) 0.037(2) 0.0004(17) -0.0011(19) 0.0004(17) C25 0.048(3) 0.028(2) 0.048(3) 0.0015(19) 0.005(2) -0.0022(18) C26 0.061(3) 0.035(2) 0.048(3) 0.004(2) 0.008(2) -0.006(2) C27 0.068(4) 0.042(2) 0.056(3) 0.006(2) 0.021(3) 0.000(2) C28 0.054(3) 0.051(3) 0.076(4) 0.012(3) 0.021(3) 0.003(2) C29 0.044(3) 0.040(2) 0.076(4) 0.014(2) 0.002(2) -0.011(2) C30 0.051(3) 0.029(2) 0.051(3) 0.003(2) 0.002(2) -0.0035(18) C31 0.041(2) 0.0247(18) 0.041(2) -0.0024(17) 0.0046(18) 0.0013(16) C32 0.047(3) 0.034(2) 0.035(2) 0.0012(18) 0.0053(18) 0.0034(18) C33 0.036(2) 0.048(3) 0.048(3) -0.003(2) 0.0017(19) 0.0041(19) C34 0.043(3) 0.044(2) 0.042(3) -0.007(2) 0.0094(19) -0.0063(19) C35 0.050(3) 0.033(2) 0.035(2) -0.0008(18) 0.0073(19) 0.0038(18) C36 0.041(2) 0.030(2) 0.033(2) -0.0027(16) -0.0002(17) 0.0032(16) F8 0.0524(16) 0.0422(14) 0.0522(16) 0.0168(11) 0.0051(12) -0.0016(11) F9 0.0579(17) 0.0606(16) 0.0419(15) 0.0110(12) -0.0021(12) 0.0196(13) F10 0.0342(14) 0.0714(18) 0.0591(17) -0.0030(14) -0.0021(12) 0.0034(12) F11 0.0406(15) 0.0481(15) 0.0686(18) 0.0064(13) 0.0129(13) -0.0056(11) F12 0.0509(15) 0.0379(13) 0.0424(14) 0.0093(11) 0.0019(11) 0.0008(11) F14 0.0556(17) 0.0573(17) 0.0635(18) -0.0135(14) 0.0145(14) 0.0050(13) F15 0.0405(18) 0.101(3) 0.113(3) -0.001(2) 0.0197(17) 0.0007(16) F16 0.055(2) 0.096(3) 0.107(3) 0.001(2) -0.0207(19) -0.0332(19) F17 0.096(3) 0.0529(18) 0.067(2) -0.0175(15) -0.0118(17) -0.0212(16) F18 0.0610(18) 0.0468(15) 0.0636(18) -0.0140(13) 0.0105(14) 0.0042(13) F26 0.0698(19) 0.0463(15) 0.0535(16) -0.0100(12) 0.0069(14) -0.0113(13) F27 0.094(3) 0.0607(18) 0.069(2) -0.0013(16) 0.0367(18) 0.0048(17) F28 0.060(2) 0.084(2) 0.116(3) 0.016(2) 0.036(2) -0.0002(18) F29 0.0488(18) 0.0484(17) 0.118(3) 0.0069(17) -0.0044(17) -0.0102(13) F30 0.0580(18) 0.0380(14) 0.0649(18) -0.0056(13) -0.0055(14) -0.0064(12) F32 0.0520(16) 0.0443(14) 0.0506(16) 0.0100(12) -0.0030(12) 0.0049(12) F33 0.0392(15) 0.0720(19) 0.0651(19) 0.0066(15) -0.0055(13) 0.0003(13) F34 0.0485(17) 0.0706(19) 0.0612(18) 0.0005(15) 0.0140(13) -0.0146(14) F35 0.0589(17) 0.0393(13) 0.0463(15) 0.0069(11) 0.0122(12) 0.0017(12) F36 0.0415(14) 0.0403(13) 0.0503(15) 0.0060(11) -0.0024(11) 0.0046(11) N1 0.0379(19) 0.0247(16) 0.042(2) 0.0022(14) -0.0013(15) 0.0001(14) N2 0.040(2) 0.0274(16) 0.047(2) -0.0006(15) -0.0005(15) -0.0019(14) N3 0.043(2) 0.0290(17) 0.045(2) 0.0003(15) 0.0034(16) -0.0023(15) N4 0.042(2) 0.0229(16) 0.044(2) 0.0013(14) 0.0024(15) -0.0016(14) Ni1 0.0358(3) 0.0220(3) 0.0450(3) 0.0006(2) 0.0028(2) -0.0011(2) O700 0.27(2) 0.211(18) 0.246(19) 0.046(13) 0.041(15) -0.030(14) C701 0.24(2) 0.20(2) 0.27(2) 0.048(17) 0.021(15) -0.024(15) C702 0.26(2) 0.228(19) 0.25(2) 0.040(15) 0.018(18) 0.017(16) C703 0.25(2) 0.21(2) 0.235(19) 0.074(16) 0.048(15) -0.006(16) C704 0.30(2) 0.19(2) 0.29(2) 0.048(16) 0.01(2) -0.001(17) O800 0.22(2) 0.31(3) 0.46(3) 0.07(2) -0.03(2) 0.01(2) C801 0.20(2) 0.27(3) 0.40(4) -0.01(3) 0.02(3) 0.04(2) C802 0.18(2) 0.27(3) 0.38(4) -0.04(3) 0.03(2) 0.05(2) C803 0.18(3) 0.21(2) 0.37(4) -0.03(2) 0.07(2) 0.07(2) C804 0.191(19) 0.25(3) 0.43(4) 0.01(3) 0.05(2) 0.05(2) O900 0.30(2) 0.25(2) 0.258(19) 0.037(16) 0.035(16) 0.011(16) C901 0.30(2) 0.250(19) 0.29(2) 0.042(16) 0.01(2) 0.035(19) C902 0.28(3) 0.27(2) 0.27(2) 0.044(18) 0.00(2) 0.02(2) C903 0.28(2) 0.25(2) 0.26(2) 0.044(19) -0.001(19) 0.041(18) C904 0.27(2) 0.230(19) 0.26(2) 0.020(16) 0.023(18) 0.032(16) _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 C1 N1 1.356(5) . ? C1 C6 1.418(6) . ? C1 C2 1.429(6) . ? C2 C3 1.350(6) . ? C2 H2 0.9500 . ? C3 C4 1.421(7) . ? C3 H3 0.9500 . ? C4 C5 1.352(7) . ? C4 H4 0.9500 . ? C5 C6 1.409(6) . ? C5 H5 0.9500 . ? C6 N2 1.365(5) . ? C7 C8 1.397(6) . ? C7 C12 1.399(6) . ? C7 N1 1.405(5) . ? C8 F8 1.340(5) . ? C8 C9 1.378(6) . ? C9 F9 1.340(5) . ? C9 C10 1.380(6) . ? C10 F10 1.335(5) . ? C10 C11 1.379(6) . ? C11 F11 1.334(5) . ? C11 C12 1.376(6) . ? C12 F12 1.350(5) . ? C13 C18 1.379(7) . ? C13 C14 1.399(7) . ? C13 N2 1.412(5) . ? C14 F14 1.346(5) . ? C14 C15 1.361(7) . ? C15 F15 1.340(6) . ? C15 C16 1.386(8) . ? C16 F16 1.345(6) . ? C16 C17 1.353(8) . ? C17 F17 1.351(6) . ? C17 C18 1.382(7) . ? C18 F18 1.338(6) . ? C19 N3 1.355(6) . ? C19 C20 1.426(6) . ? C19 C24 1.435(6) . ? C20 C21 1.338(7) . ? C20 H20 0.9500 . ? C21 C22 1.427(8) . ? C21 H21 0.9500 . ? C22 C23 1.366(7) . ? C22 H22 0.9500 . ? C23 C24 1.414(6) . ? C23 H23 0.9500 . ? C24 N4 1.362(5) . ? C25 C26 1.388(7) . ? C25 C30 1.400(6) . ? C25 N3 1.406(6) . ? C26 F26 1.350(6) . ? C26 C27 1.374(7) . ? C27 F27 1.346(6) . ? C27 C28 1.370(8) . ? C28 F28 1.332(6) . ? C28 C29 1.368(8) . ? C29 F29 1.350(6) . ? C29 C30 1.392(7) . ? C30 F30 1.353(5) . ? C31 C32 1.396(6) . ? C31 C36 1.399(6) . ? C31 N4 1.407(5) . ? C32 F32 1.349(5) . ? C32 C33 1.381(6) . ? C33 F33 1.334(5) . ? C33 C34 1.381(7) . ? C34 F34 1.341(5) . ? C34 C35 1.374(6) . ? C35 F35 1.334(5) . ? C35 C36 1.371(6) . ? C36 F36 1.343(5) . ? N1 Ni1 1.909(3) . ? N2 Ni1 1.902(4) . ? N3 Ni1 1.895(3) . ? N4 Ni1 1.889(4) . ? O700 C704 1.435(18) . ? O700 C701 1.469(19) . ? C701 C702 1.526(19) . ? C701 H70A 0.9900 . ? C701 H70B 0.9900 . ? C702 C703 1.520(18) . ? C702 H70C 0.9900 . ? C702 H70D 0.9900 . ? C703 C704 1.494(19) . ? C703 H70I 0.9900 . ? C703 H70J 0.9900 . ? C704 H70K 0.9900 . ? C704 H70L 0.9900 . ? O800 C804 1.4499(11) . ? O800 C801 1.4500(11) . ? C801 C802 1.5399(11) . ? C801 H80A 0.9900 . ? C801 H80B 0.9900 . ? C802 C803 1.5400(11) . ? C802 H80C 0.9900 . ? C802 H80D 0.9900 . ? C803 C804 1.5399(11) . ? C803 H80E 0.9900 . ? C803 H80F 0.9900 . ? C804 H80G 0.9900 . ? C804 H80H 0.9900 . ? O900 C904 1.434(19) . ? O900 C901 1.461(18) . ? C901 C902 1.514(18) . ? C901 H90A 0.9900 . ? C901 H90B 0.9900 . ? C902 C903 1.539(19) . ? C902 H90C 0.9900 . ? C902 H90D 0.9900 . ? C903 C904 1.504(19) . ? C903 H90E 0.9900 . ? C903 H90F 0.9900 . ? C904 H90G 0.9900 . ? C904 H90H 0.9900 . ? 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 N1 C1 C6 114.0(4) . . ? N1 C1 C2 127.6(4) . . ? C6 C1 C2 118.3(4) . . ? C3 C2 C1 120.0(4) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.9(4) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 120.4(4) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 120.1(4) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? N2 C6 C5 126.6(4) . . ? N2 C6 C1 113.4(4) . . ? C5 C6 C1 119.8(4) . . ? C8 C7 C12 115.2(4) . . ? C8 C7 N1 120.3(4) . . ? C12 C7 N1 124.1(4) . . ? F8 C8 C9 118.2(4) . . ? F8 C8 C7 119.0(4) . . ? C9 C8 C7 122.7(4) . . ? F9 C9 C8 120.7(4) . . ? F9 C9 C10 119.5(4) . . ? C8 C9 C10 119.7(4) . . ? F10 C10 C11 120.3(4) . . ? F10 C10 C9 120.0(4) . . ? C11 C10 C9 119.7(4) . . ? F11 C11 C12 120.5(4) . . ? F11 C11 C10 120.0(4) . . ? C12 C11 C10 119.5(4) . . ? F12 C12 C11 116.9(4) . . ? F12 C12 C7 120.0(4) . . ? C11 C12 C7 123.1(4) . . ? C18 C13 C14 116.4(4) . . ? C18 C13 N2 120.4(4) . . ? C14 C13 N2 122.9(4) . . ? F14 C14 C15 117.6(4) . . ? F14 C14 C13 120.0(4) . . ? C15 C14 C13 122.4(5) . . ? F15 C15 C14 120.7(5) . . ? F15 C15 C16 119.7(5) . . ? C14 C15 C16 119.5(5) . . ? F16 C16 C17 120.4(5) . . ? F16 C16 C15 120.3(5) . . ? C17 C16 C15 119.3(5) . . ? F17 C17 C16 120.2(5) . . ? F17 C17 C18 118.8(5) . . ? C16 C17 C18 121.0(5) . . ? F18 C18 C13 119.7(4) . . ? F18 C18 C17 119.0(4) . . ? C13 C18 C17 121.3(5) . . ? N3 C19 C20 128.3(4) . . ? N3 C19 C24 112.8(4) . . ? C20 C19 C24 118.8(4) . . ? C21 C20 C19 120.1(5) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 121.5(4) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? C23 C22 C21 120.3(4) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 119.9(5) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? N4 C24 C23 127.7(4) . . ? N4 C24 C19 112.9(4) . . ? C23 C24 C19 119.3(4) . . ? C26 C25 C30 115.9(4) . . ? C26 C25 N3 118.5(4) . . ? C30 C25 N3 124.9(4) . . ? F26 C26 C27 117.3(4) . . ? F26 C26 C25 119.6(4) . . ? C27 C26 C25 123.1(5) . . ? F27 C27 C28 120.2(5) . . ? F27 C27 C26 120.0(5) . . ? C28 C27 C26 119.8(5) . . ? F28 C28 C29 119.7(5) . . ? F28 C28 C27 120.8(5) . . ? C29 C28 C27 119.4(5) . . ? F29 C29 C28 121.1(5) . . ? F29 C29 C30 118.0(5) . . ? C28 C29 C30 120.7(5) . . ? F30 C30 C29 119.0(4) . . ? F30 C30 C25 119.8(4) . . ? C29 C30 C25 121.1(5) . . ? C32 C31 C36 115.6(4) . . ? C32 C31 N4 124.5(4) . . ? C36 C31 N4 119.3(4) . . ? F32 C32 C33 118.1(4) . . ? F32 C32 C31 119.6(4) . . ? C33 C32 C31 122.3(4) . . ? F33 C33 C34 120.4(4) . . ? F33 C33 C32 119.9(4) . . ? C34 C33 C32 119.6(4) . . ? F34 C34 C35 119.7(4) . . ? F34 C34 C33 120.5(4) . . ? C35 C34 C33 119.8(4) . . ? F35 C35 C36 119.8(4) . . ? F35 C35 C34 120.4(4) . . ? C36 C35 C34 119.8(4) . . ? F36 C36 C35 118.1(4) . . ? F36 C36 C31 119.1(4) . . ? C35 C36 C31 122.8(4) . . ? C1 N1 C7 120.8(3) . . ? C1 N1 Ni1 114.9(3) . . ? C7 N1 Ni1 123.6(2) . . ? C6 N2 C13 119.9(4) . . ? C6 N2 Ni1 115.2(3) . . ? C13 N2 Ni1 124.6(3) . . ? C19 N3 C25 121.8(4) . . ? C19 N3 Ni1 115.9(3) . . ? C25 N3 Ni1 121.5(3) . . ? C24 N4 C31 120.4(4) . . ? C24 N4 Ni1 115.9(3) . . ? C31 N4 Ni1 123.5(3) . . ? N4 Ni1 N3 82.35(15) . . ? N4 Ni1 N2 144.25(16) . . ? N3 Ni1 N2 107.04(15) . . ? N4 Ni1 N1 107.64(15) . . ? N3 Ni1 N1 148.66(15) . . ? N2 Ni1 N1 82.45(14) . . ? C704 O700 C701 101.3(19) . . ? O700 C701 C702 106(2) . . ? O700 C701 H70A 110.6 . . ? C702 C701 H70A 110.6 . . ? O700 C701 H70B 110.6 . . ? C702 C701 H70B 110.6 . . ? H70A C701 H70B 108.7 . . ? C703 C702 C701 95.8(17) . . ? C703 C702 H70C 112.6 . . ? C701 C702 H70C 112.6 . . ? C703 C702 H70D 112.6 . . ? C701 C702 H70D 112.6 . . ? H70C C702 H70D 110.1 . . ? C704 C703 C702 109.0(18) . . ? C704 C703 H70I 109.9 . . ? C702 C703 H70I 109.9 . . ? C704 C703 H70J 109.9 . . ? C702 C703 H70J 109.9 . . ? H70I C703 H70J 108.3 . . ? O700 C704 C703 106.2(17) . . ? O700 C704 H70K 110.5 . . ? C703 C704 H70K 110.5 . . ? O700 C704 H70L 110.5 . . ? C703 C704 H70L 110.5 . . ? H70K C704 H70L 108.7 . . ? C804 O800 C801 102.1(18) . . ? O800 C801 C802 108.5(15) . . ? O800 C801 H80A 110.0 . . ? C802 C801 H80A 110.0 . . ? O800 C801 H80B 110.0 . . ? C802 C801 H80B 110.0 . . ? H80A C801 H80B 108.4 . . ? C803 C802 C801 100.0(12) . . ? C803 C802 H80C 111.8 . . ? C801 C802 H80C 111.8 . . ? C803 C802 H80D 111.8 . . ? C801 C802 H80D 111.8 . . ? H80C C802 H80D 109.5 . . ? C804 C803 C802 106.2(11) . . ? C804 C803 H80E 110.5 . . ? C802 C803 H80E 110.5 . . ? C804 C803 H80F 110.5 . . ? C802 C803 H80F 110.5 . . ? H80E C803 H80F 108.7 . . ? O800 C804 C803 107.5(13) . . ? O800 C804 H80G 110.2 . . ? C803 C804 H80G 110.2 . . ? O800 C804 H80H 110.2 . . ? C803 C804 H80H 110.2 . . ? H80G C804 H80H 108.5 . . ? C904 O900 C901 103(2) . . ? O900 C901 C902 104(2) . . ? O900 C901 H90A 111.0 . . ? C902 C901 H90A 111.0 . . ? O900 C901 H90B 111.0 . . ? C902 C901 H90B 111.0 . . ? H90A C901 H90B 109.0 . . ? C901 C902 C903 94.9(19) . . ? C901 C902 H90C 112.8 . . ? C903 C902 H90C 112.8 . . ? C901 C902 H90D 112.8 . . ? C903 C902 H90D 112.8 . . ? H90C C902 H90D 110.2 . . ? C904 C903 C902 109.1(19) . . ? C904 C903 H90E 109.9 . . ? C902 C903 H90E 109.9 . . ? C904 C903 H90F 109.9 . . ? C902 C903 H90F 109.9 . . ? H90E C903 H90F 108.3 . . ? O900 C904 C903 103.3(19) . . ? O900 C904 H90G 111.1 . . ? C903 C904 H90G 111.1 . . ? O900 C904 H90H 111.1 . . ? C903 C904 H90H 111.1 . . ? H90G C904 H90H 109.1 . . ? 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 N1 C1 C2 C3 179.3(5) . . . . ? C6 C1 C2 C3 -3.4(7) . . . . ? C1 C2 C3 C4 -2.1(9) . . . . ? C2 C3 C4 C5 4.6(10) . . . . ? C3 C4 C5 C6 -1.4(9) . . . . ? C4 C5 C6 N2 -179.4(5) . . . . ? C4 C5 C6 C1 -4.1(8) . . . . ? N1 C1 C6 N2 0.1(6) . . . . ? C2 C1 C6 N2 -177.6(4) . . . . ? N1 C1 C6 C5 -175.8(4) . . . . ? C2 C1 C6 C5 6.5(7) . . . . ? C12 C7 C8 F8 -178.2(3) . . . . ? N1 C7 C8 F8 -5.2(6) . . . . ? C12 C7 C8 C9 1.4(6) . . . . ? N1 C7 C8 C9 174.4(4) . . . . ? F8 C8 C9 F9 2.6(6) . . . . ? C7 C8 C9 F9 -177.0(4) . . . . ? F8 C8 C9 C10 -178.8(4) . . . . ? C7 C8 C9 C10 1.6(6) . . . . ? F9 C9 C10 F10 -3.3(6) . . . . ? C8 C9 C10 F10 178.0(4) . . . . ? F9 C9 C10 C11 176.0(4) . . . . ? C8 C9 C10 C11 -2.6(6) . . . . ? F10 C10 C11 F11 2.6(6) . . . . ? C9 C10 C11 F11 -176.7(4) . . . . ? F10 C10 C11 C12 179.8(4) . . . . ? C9 C10 C11 C12 0.5(6) . . . . ? F11 C11 C12 F12 2.7(6) . . . . ? C10 C11 C12 F12 -174.5(4) . . . . ? F11 C11 C12 C7 180.0(4) . . . . ? C10 C11 C12 C7 2.8(6) . . . . ? C8 C7 C12 F12 173.6(3) . . . . ? N1 C7 C12 F12 0.9(6) . . . . ? C8 C7 C12 C11 -3.6(6) . . . . ? N1 C7 C12 C11 -176.3(4) . . . . ? C18 C13 C14 F14 175.8(4) . . . . ? N2 C13 C14 F14 2.2(6) . . . . ? C18 C13 C14 C15 -3.2(7) . . . . ? N2 C13 C14 C15 -176.9(4) . . . . ? F14 C14 C15 F15 0.8(7) . . . . ? C13 C14 C15 F15 179.9(4) . . . . ? F14 C14 C15 C16 -176.3(5) . . . . ? C13 C14 C15 C16 2.8(7) . . . . ? F15 C15 C16 F16 1.4(8) . . . . ? C14 C15 C16 F16 178.6(5) . . . . ? F15 C15 C16 C17 -177.3(5) . . . . ? C14 C15 C16 C17 -0.2(8) . . . . ? F16 C16 C17 F17 -1.5(8) . . . . ? C15 C16 C17 F17 177.2(5) . . . . ? F16 C16 C17 C18 179.4(5) . . . . ? C15 C16 C17 C18 -1.8(8) . . . . ? C14 C13 C18 F18 -177.9(4) . . . . ? N2 C13 C18 F18 -4.1(6) . . . . ? C14 C13 C18 C17 1.2(7) . . . . ? N2 C13 C18 C17 175.0(4) . . . . ? F17 C17 C18 F18 1.3(7) . . . . ? C16 C17 C18 F18 -179.6(5) . . . . ? F17 C17 C18 C13 -177.8(4) . . . . ? C16 C17 C18 C13 1.3(8) . . . . ? N3 C19 C20 C21 -179.0(5) . . . . ? C24 C19 C20 C21 -1.5(7) . . . . ? C19 C20 C21 C22 -1.4(8) . . . . ? C20 C21 C22 C23 3.2(8) . . . . ? C21 C22 C23 C24 -2.0(7) . . . . ? C22 C23 C24 N4 -176.5(5) . . . . ? C22 C23 C24 C19 -0.9(7) . . . . ? N3 C19 C24 N4 -3.2(5) . . . . ? C20 C19 C24 N4 178.9(4) . . . . ? N3 C19 C24 C23 -179.5(4) . . . . ? C20 C19 C24 C23 2.6(6) . . . . ? C30 C25 C26 F26 -178.4(4) . . . . ? N3 C25 C26 F26 -7.5(6) . . . . ? C30 C25 C26 C27 0.0(7) . . . . ? N3 C25 C26 C27 170.9(4) . . . . ? F26 C26 C27 F27 2.0(7) . . . . ? C25 C26 C27 F27 -176.4(4) . . . . ? F26 C26 C27 C28 179.6(4) . . . . ? C25 C26 C27 C28 1.2(8) . . . . ? F27 C27 C28 F28 -1.1(8) . . . . ? C26 C27 C28 F28 -178.7(5) . . . . ? F27 C27 C28 C29 176.5(4) . . . . ? C26 C27 C28 C29 -1.1(8) . . . . ? F28 C28 C29 F29 2.7(7) . . . . ? C27 C28 C29 F29 -174.9(5) . . . . ? F28 C28 C29 C30 177.6(4) . . . . ? C27 C28 C29 C30 0.0(8) . . . . ? F29 C29 C30 F30 0.4(6) . . . . ? C28 C29 C30 F30 -174.6(4) . . . . ? F29 C29 C30 C25 176.2(4) . . . . ? C28 C29 C30 C25 1.2(7) . . . . ? C26 C25 C30 F30 174.6(4) . . . . ? N3 C25 C30 F30 4.3(6) . . . . ? C26 C25 C30 C29 -1.1(6) . . . . ? N3 C25 C30 C29 -171.5(4) . . . . ? C36 C31 C32 F32 174.9(4) . . . . ? N4 C31 C32 F32 4.1(6) . . . . ? C36 C31 C32 C33 -3.1(6) . . . . ? N4 C31 C32 C33 -173.9(4) . . . . ? F32 C32 C33 F33 2.0(6) . . . . ? C31 C32 C33 F33 -180.0(4) . . . . ? F32 C32 C33 C34 -175.0(4) . . . . ? C31 C32 C33 C34 3.0(7) . . . . ? F33 C33 C34 F34 1.7(7) . . . . ? C32 C33 C34 F34 178.7(4) . . . . ? F33 C33 C34 C35 -177.6(4) . . . . ? C32 C33 C34 C35 -0.6(7) . . . . ? F34 C34 C35 F35 -2.3(6) . . . . ? C33 C34 C35 F35 177.0(4) . . . . ? F34 C34 C35 C36 179.3(4) . . . . ? C33 C34 C35 C36 -1.4(6) . . . . ? F35 C35 C36 F36 1.4(6) . . . . ? C34 C35 C36 F36 179.8(4) . . . . ? F35 C35 C36 C31 -177.2(4) . . . . ? C34 C35 C36 C31 1.3(6) . . . . ? C32 C31 C36 F36 -177.6(3) . . . . ? N4 C31 C36 F36 -6.2(6) . . . . ? C32 C31 C36 C35 1.0(6) . . . . ? N4 C31 C36 C35 172.3(4) . . . . ? C6 C1 N1 C7 172.3(4) . . . . ? C2 C1 N1 C7 -10.2(7) . . . . ? C6 C1 N1 Ni1 1.0(5) . . . . ? C2 C1 N1 Ni1 178.5(4) . . . . ? C8 C7 N1 C1 137.4(4) . . . . ? C12 C7 N1 C1 -50.2(6) . . . . ? C8 C7 N1 Ni1 -52.1(5) . . . . ? C12 C7 N1 Ni1 120.3(4) . . . . ? C5 C6 N2 C13 -11.4(7) . . . . ? C1 C6 N2 C13 173.1(4) . . . . ? C5 C6 N2 Ni1 174.4(4) . . . . ? C1 C6 N2 Ni1 -1.2(5) . . . . ? C18 C13 N2 C6 132.2(5) . . . . ? C14 C13 N2 C6 -54.4(6) . . . . ? C18 C13 N2 Ni1 -54.2(5) . . . . ? C14 C13 N2 Ni1 119.2(4) . . . . ? C20 C19 N3 C25 -8.1(7) . . . . ? C24 C19 N3 C25 174.3(4) . . . . ? C20 C19 N3 Ni1 -177.9(4) . . . . ? C24 C19 N3 Ni1 4.4(5) . . . . ? C26 C25 N3 C19 137.3(4) . . . . ? C30 C25 N3 C19 -52.6(6) . . . . ? C26 C25 N3 Ni1 -53.5(5) . . . . ? C30 C25 N3 Ni1 116.6(4) . . . . ? C23 C24 N4 C31 -9.1(7) . . . . ? C19 C24 N4 C31 175.0(4) . . . . ? C23 C24 N4 Ni1 176.5(4) . . . . ? C19 C24 N4 Ni1 0.6(5) . . . . ? C32 C31 N4 C24 -55.5(6) . . . . ? C36 C31 N4 C24 134.0(4) . . . . ? C32 C31 N4 Ni1 118.4(4) . . . . ? C36 C31 N4 Ni1 -52.1(5) . . . . ? C24 N4 Ni1 N3 1.4(3) . . . . ? C31 N4 Ni1 N3 -172.8(3) . . . . ? C24 N4 Ni1 N2 -107.2(3) . . . . ? C31 N4 Ni1 N2 78.6(4) . . . . ? C24 N4 Ni1 N1 150.9(3) . . . . ? C31 N4 Ni1 N1 -23.3(4) . . . . ? C19 N3 Ni1 N4 -3.3(3) . . . . ? C25 N3 Ni1 N4 -173.1(4) . . . . ? C19 N3 Ni1 N2 141.3(3) . . . . ? C25 N3 Ni1 N2 -28.5(4) . . . . ? C19 N3 Ni1 N1 -114.8(4) . . . . ? C25 N3 Ni1 N1 75.3(4) . . . . ? C6 N2 Ni1 N4 -108.5(4) . . . . ? C13 N2 Ni1 N4 77.6(4) . . . . ? C6 N2 Ni1 N3 150.7(3) . . . . ? C13 N2 Ni1 N3 -23.2(4) . . . . ? C6 N2 Ni1 N1 1.4(3) . . . . ? C13 N2 Ni1 N1 -172.6(4) . . . . ? C1 N1 Ni1 N4 143.5(3) . . . . ? C7 N1 Ni1 N4 -27.6(4) . . . . ? C1 N1 Ni1 N3 -111.9(4) . . . . ? C7 N1 Ni1 N3 77.1(4) . . . . ? C1 N1 Ni1 N2 -1.3(3) . . . . ? C7 N1 Ni1 N2 -172.3(3) . . . . ? C704 O700 C701 C702 -47(3) . . . . ? O700 C701 C702 C703 43(3) . . . . ? C701 C702 C703 C704 -24(4) . . . . ? C701 O700 C704 C703 29(4) . . . . ? C702 C703 C704 O700 -3(5) . . . . ? C804 O800 C801 C802 -41(4) . . . . ? O800 C801 C802 C803 32(4) . . . . ? C801 C802 C803 C804 -11(5) . . . . ? C801 O800 C804 C803 32(4) . . . . ? C802 C803 C804 O800 -13(5) . . . . ? C904 O900 C901 C902 -52(3) . . . . ? O900 C901 C902 C903 46(4) . . . . ? C901 C902 C903 C904 -26(5) . . . . ? C901 O900 C904 C903 33(4) . . . . ? C902 C903 C904 O900 -3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.064 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.082 #===END #data_mk2 data_no_2 _database_code_depnum_ccdc_archive 'CCDC 662504' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H8 F20 N4 Pd, 4(C4 H8 O)' _chemical_formula_sum 'C52 H40 F20 N4 O4 Pd' _chemical_formula_weight 1271.28 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' F F 0.0171 0.0103 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d d' _symmetry_space_group_name_Hall '-F 2uv 2vw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+1/4, z' 'x, -y+1/4, -z+1/4' '-x+1/4, y, -z+1/4' 'x, y+1/2, z+1/2' '-x+1/4, -y+3/4, z+1/2' 'x, -y+3/4, -z+3/4' '-x+1/4, y+1/2, -z+3/4' 'x+1/2, y, z+1/2' '-x+3/4, -y+1/4, z+1/2' 'x+1/2, -y+1/4, -z+3/4' '-x+3/4, y, -z+3/4' 'x+1/2, y+1/2, z' '-x+3/4, -y+3/4, z' 'x+1/2, -y+3/4, -z+1/4' '-x+3/4, y+1/2, -z+1/4' '-x, -y, -z' 'x-1/4, y-1/4, -z' '-x, y-1/4, z-1/4' 'x-1/4, -y, z-1/4' '-x, -y+1/2, -z+1/2' 'x-1/4, y+1/4, -z+1/2' '-x, y+1/4, z+1/4' 'x-1/4, -y+1/2, z+1/4' '-x+1/2, -y, -z+1/2' 'x+1/4, y-1/4, -z+1/2' '-x+1/2, y-1/4, z+1/4' 'x+1/4, -y, z+1/4' '-x+1/2, -y+1/2, -z' 'x+1/4, y+1/4, -z' '-x+1/2, y+1/4, z-1/4' 'x+1/4, -y+1/2, z-1/4' _cell_length_a 15.0923(14) _cell_length_b 19.2020(14) _cell_length_c 35.566(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10307.1(15) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9087 _cell_measurement_theta_min 26.18 _cell_measurement_theta_max 0 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5104 _exptl_absorpt_coefficient_mu 0.483 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8581 _exptl_absorpt_correction_T_max 1.1316 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'STOE IPDS-2' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16959 _diffrn_reflns_av_R_equivalents 0.1010 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2200 _reflns_number_gt 1643 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0583P)^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 SHELXL _refine_ls_extinction_coef 0.00016(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2200 _refine_ls_number_parameters 204 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1064 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.991 _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 C1 C -0.0496(2) 0.1562(2) 0.16596(10) 0.0372(10) Uani 1 1 d . . . C2 C -0.0697(3) 0.2229(2) 0.15577(11) 0.0405(10) Uani 1 1 d . . . C3 C -0.1565(3) 0.2459(3) 0.15294(12) 0.0445(11) Uani 1 1 d . . . C4 C -0.2237(3) 0.2001(3) 0.16142(12) 0.0480(11) Uani 1 1 d . . . C5 C -0.2055(2) 0.1337(3) 0.17154(12) 0.0478(11) Uani 1 1 d . . . C6 C -0.1183(2) 0.1112(2) 0.17399(10) 0.0398(9) Uani 1 1 d . . . C7 C 0.0783(2) 0.1323(2) 0.20284(10) 0.0377(9) Uani 1 1 d . . . C8 C 0.0343(3) 0.1419(2) 0.23719(11) 0.0472(12) Uani 1 1 d . . . H8 H -0.0268 0.1537 0.2374 0.057 Uiso 1 1 calc R . . C9 C 0.0792(3) 0.1342(3) 0.27025(11) 0.0530(12) Uani 1 1 d . . . H9 H 0.0492 0.1412 0.2934 0.064 Uiso 1 1 calc R . . F2 F -0.00503(15) 0.26901(14) 0.14816(8) 0.0554(7) Uani 1 1 d . . . F3 F -0.17490(18) 0.31096(16) 0.14274(8) 0.0647(8) Uani 1 1 d . . . F4 F -0.30834(15) 0.22185(17) 0.15864(9) 0.0714(9) Uani 1 1 d . . . F5 F -0.27116(16) 0.08837(17) 0.17888(9) 0.0685(8) Uani 1 1 d . . . F6 F -0.10185(15) 0.04558(15) 0.18440(8) 0.0558(7) Uani 1 1 d . . . N1 N 0.04111(18) 0.1338(2) 0.16802(9) 0.0399(8) Uani 1 1 d . . . Pd1 Pd 0.1250 0.1250 0.1250 0.0355(2) Uani 1 4 d S . . O100 O -0.1839(3) 0.1302(3) 0.25514(11) 0.0938(14) Uani 1 1 d D A . C101 C -0.1813(7) 0.0743(5) 0.2812(2) 0.119(3) Uani 1 1 d D . . H101 H -0.1205 0.0551 0.2828 0.143 Uiso 0.56(3) 1 calc PR A 1 H111 H -0.2217 0.0366 0.2730 0.143 Uiso 0.56(3) 1 calc PR A 1 H121 H -0.1324 0.0416 0.2754 0.143 Uiso 0.44(3) 1 d PR A 2 H131 H -0.2380 0.0484 0.2815 0.143 Uiso 0.44(3) 1 d PR A 2 C102 C -0.2084(19) 0.1009(10) 0.3172(5) 0.191(15) Uani 0.56(3) 1 d PD A 1 H10A H -0.1721 0.0815 0.3378 0.229 Uiso 0.56(3) 1 calc PR A 1 H10B H -0.2718 0.0913 0.3222 0.229 Uiso 0.56(3) 1 calc PR A 1 C103 C -0.1912(18) 0.1784(9) 0.3115(4) 0.195(16) Uani 0.56(3) 1 d PD A 1 H10C H -0.2286 0.2069 0.3285 0.234 Uiso 0.56(3) 1 calc PR A 1 H10D H -0.1281 0.1900 0.3159 0.234 Uiso 0.56(3) 1 calc PR A 1 C104 C -0.2156(6) 0.1886(5) 0.2725(2) 0.119(3) Uani 1 1 d D . . H104 H -0.2806 0.1923 0.2696 0.143 Uiso 0.56(3) 1 calc PR A 1 H114 H -0.1876 0.2311 0.2621 0.143 Uiso 0.56(3) 1 calc PR A 1 H124 H -0.2702 0.2052 0.2599 0.143 Uiso 0.44(3) 1 d PR A 2 H134 H -0.1709 0.2264 0.2718 0.143 Uiso 0.44(3) 1 d PR A 2 C112 C -0.1659(11) 0.1106(10) 0.3170(4) 0.077(7) Uani 0.44(3) 1 d PD A 2 H11A H -0.1049 0.1292 0.3189 0.092 Uiso 0.44(3) 1 calc PR A 2 H11B H -0.1789 0.0807 0.3390 0.092 Uiso 0.44(3) 1 calc PR A 2 C113 C -0.235(3) 0.1679(17) 0.3118(5) 0.25(3) Uani 0.44(3) 1 d PD A 2 H11C H -0.2957 0.1500 0.3147 0.301 Uiso 0.44(3) 1 calc PR A 2 H11D H -0.2250 0.2069 0.3296 0.301 Uiso 0.44(3) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0254(17) 0.054(3) 0.0324(19) -0.0020(18) 0.0005(14) 0.0050(17) C2 0.039(2) 0.041(3) 0.041(2) -0.0005(19) -0.0008(16) -0.0004(18) C3 0.041(2) 0.039(3) 0.054(2) -0.003(2) -0.0032(18) 0.0076(19) C4 0.0310(19) 0.059(4) 0.054(3) -0.006(2) 0.0003(18) 0.012(2) C5 0.0291(19) 0.058(4) 0.056(2) -0.002(2) 0.0078(16) -0.009(2) C6 0.0354(19) 0.044(3) 0.0399(18) 0.0023(17) 0.0019(16) 0.0006(19) C7 0.0327(18) 0.042(3) 0.0382(19) 0.0009(19) 0.0012(14) 0.0000(17) C8 0.0346(18) 0.065(4) 0.042(2) 0.000(2) 0.0053(16) 0.0072(19) C9 0.046(2) 0.078(4) 0.035(2) -0.005(2) 0.0069(16) 0.002(2) F2 0.0466(13) 0.0510(19) 0.0685(16) 0.0043(13) 0.0000(12) -0.0115(11) F3 0.0647(16) 0.048(2) 0.0819(19) -0.0042(15) -0.0141(14) 0.0122(13) F4 0.0320(12) 0.085(2) 0.097(2) -0.0101(18) -0.0050(13) 0.0164(13) F5 0.0346(13) 0.077(2) 0.093(2) 0.0077(16) 0.0089(13) -0.0134(13) F6 0.0468(14) 0.050(2) 0.0708(17) 0.0099(13) 0.0034(11) 0.0005(11) N1 0.0278(15) 0.052(3) 0.0404(17) 0.0006(16) -0.0012(12) 0.0025(15) Pd1 0.0242(3) 0.0519(5) 0.0304(3) 0.000 0.000 0.000 O100 0.102(3) 0.108(4) 0.072(2) 0.010(3) 0.027(2) 0.022(3) C101 0.162(8) 0.079(7) 0.116(7) 0.014(5) 0.031(6) -0.004(5) C102 0.21(3) 0.22(3) 0.147(17) 0.097(17) 0.141(18) 0.12(2) C103 0.25(3) 0.18(2) 0.149(18) -0.122(17) -0.141(19) 0.146(19) C104 0.152(7) 0.080(6) 0.124(7) 0.009(5) 0.032(6) 0.042(5) C112 0.065(9) 0.112(17) 0.054(8) 0.009(8) 0.026(7) 0.028(9) C113 0.31(5) 0.33(5) 0.108(18) 0.12(3) 0.11(2) 0.27(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.364(6) . ? C1 C6 1.379(6) . ? C1 N1 1.437(4) . ? C2 F2 1.345(5) . ? C2 C3 1.386(6) . ? C3 F3 1.330(5) . ? C3 C4 1.376(6) . ? C4 F4 1.348(5) . ? C4 C5 1.353(7) . ? C5 F5 1.345(5) . ? C5 C6 1.388(6) . ? C6 F6 1.337(5) . ? C7 N1 1.360(5) . ? C7 C8 1.402(5) . ? C7 C7 1.436(7) 2 ? C8 C9 1.365(6) . ? C8 H8 0.9500 . ? C9 C9 1.428(8) 2 ? C9 H9 0.9500 . ? N1 Pd1 1.993(3) . ? Pd1 N1 1.993(3) 2 ? Pd1 N1 1.993(3) 4 ? Pd1 N1 1.993(3) 3 ? O100 C104 1.366(8) . ? O100 C101 1.419(9) . ? C101 C102 1.438(16) . ? C101 C112 1.470(15) . ? C101 H101 0.9900 . ? C101 H111 0.9900 . ? C101 H121 0.9900 . ? C101 H131 0.9900 . ? C102 C103 1.52(2) . ? C102 H10A 0.9900 . ? C102 H10B 0.9900 . ? C103 C104 1.451(15) . ? C103 H10C 0.9900 . ? C103 H10D 0.9900 . ? C104 C113 1.483(17) . ? C104 H104 0.9900 . ? C104 H114 0.9900 . ? C104 H124 0.9900 . ? C104 H134 0.9900 . ? C112 C113 1.52(2) . ? C112 H11A 0.9900 . ? C112 H11B 0.9900 . ? C113 H11C 0.9900 . ? C113 H11D 0.9900 . ? 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 C2 C1 C6 118.4(4) . . ? C2 C1 N1 120.4(4) . . ? C6 C1 N1 121.1(4) . . ? F2 C2 C1 120.7(3) . . ? F2 C2 C3 117.4(4) . . ? C1 C2 C3 121.9(4) . . ? F3 C3 C4 120.4(4) . . ? F3 C3 C2 121.1(4) . . ? C4 C3 C2 118.5(4) . . ? F4 C4 C5 120.3(4) . . ? F4 C4 C3 119.0(4) . . ? C5 C4 C3 120.7(4) . . ? F5 C5 C4 120.8(4) . . ? F5 C5 C6 119.0(5) . . ? C4 C5 C6 120.2(4) . . ? F6 C6 C1 120.6(4) . . ? F6 C6 C5 119.1(4) . . ? C1 C6 C5 120.3(4) . . ? N1 C7 C8 126.5(3) . . ? N1 C7 C7 114.15(19) . 2 ? C8 C7 C7 119.3(2) . 2 ? C9 C8 C7 120.1(4) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C9 120.5(2) . 2 ? C8 C9 H9 119.8 . . ? C9 C9 H9 119.8 2 . ? C7 N1 C1 116.5(3) . . ? C7 N1 Pd1 115.8(2) . . ? C1 N1 Pd1 126.3(2) . . ? N1 Pd1 N1 101.13(16) 2 4 ? N1 Pd1 N1 170.3(2) 2 3 ? N1 Pd1 N1 79.71(16) 4 3 ? N1 Pd1 N1 79.71(16) 2 . ? N1 Pd1 N1 170.3(2) 4 . ? N1 Pd1 N1 101.13(16) 3 . ? C104 O100 C101 109.7(6) . . ? O100 C101 C102 107.7(10) . . ? O100 C101 C112 102.2(9) . . ? C102 C101 C112 26.6(11) . . ? O100 C101 H101 110.2 . . ? C102 C101 H101 110.2 . . ? C112 C101 H101 88.8 . . ? O100 C101 H111 110.2 . . ? C102 C101 H111 110.2 . . ? C112 C101 H111 134.2 . . ? H101 C101 H111 108.5 . . ? O100 C101 H121 111.3 . . ? C102 C101 H121 128.6 . . ? C112 C101 H121 111.3 . . ? H101 C101 H121 24.0 . . ? H111 C101 H121 86.3 . . ? O100 C101 H131 111.3 . . ? C102 C101 H131 85.4 . . ? C112 C101 H131 111.3 . . ? H101 C101 H131 127.9 . . ? H111 C101 H131 26.3 . . ? H121 C101 H131 109.2 . . ? C101 C102 C103 100.4(11) . . ? C101 C102 H10A 111.7 . . ? C103 C102 H10A 111.7 . . ? C101 C102 H10B 111.7 . . ? C103 C102 H10B 111.7 . . ? H10A C102 H10B 109.5 . . ? C104 C103 C102 102.4(12) . . ? C104 C103 H10C 111.3 . . ? C102 C103 H10C 111.3 . . ? C104 C103 H10D 111.3 . . ? C102 C103 H10D 111.3 . . ? H10C C103 H10D 109.2 . . ? O100 C104 C103 103.4(8) . . ? O100 C104 C113 105.8(11) . . ? C103 C104 C113 27(2) . . ? O100 C104 H104 111.1 . . ? C103 C104 H104 111.1 . . ? C113 C104 H104 85.7 . . ? O100 C104 H114 111.1 . . ? C103 C104 H114 111.1 . . ? C113 C104 H114 130.9 . . ? H104 C104 H114 109.0 . . ? O100 C104 H124 110.5 . . ? C103 C104 H124 133.4 . . ? C113 C104 H124 110.6 . . ? H104 C104 H124 26.5 . . ? H114 C104 H124 85.6 . . ? O100 C104 H134 110.6 . . ? C103 C104 H134 87.1 . . ? C113 C104 H134 110.6 . . ? H104 C104 H134 128.4 . . ? H114 C104 H134 25.4 . . ? H124 C104 H134 108.7 . . ? C101 C112 C113 97.5(15) . . ? C101 C112 H11A 112.3 . . ? C113 C112 H11A 112.3 . . ? C101 C112 H11B 112.3 . . ? C113 C112 H11B 112.3 . . ? H11A C112 H11B 109.9 . . ? C104 C113 C112 100.2(13) . . ? C104 C113 H11C 111.7 . . ? C112 C113 H11C 111.7 . . ? C104 C113 H11D 111.7 . . ? C112 C113 H11D 111.7 . . ? H11C C113 H11D 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 F2 179.1(3) . . . . ? N1 C1 C2 F2 -1.2(6) . . . . ? C6 C1 C2 C3 -0.7(6) . . . . ? N1 C1 C2 C3 179.0(4) . . . . ? F2 C2 C3 F3 0.6(6) . . . . ? C1 C2 C3 F3 -179.6(4) . . . . ? F2 C2 C3 C4 -178.5(4) . . . . ? C1 C2 C3 C4 1.3(6) . . . . ? F3 C3 C4 F4 1.1(6) . . . . ? C2 C3 C4 F4 -179.8(4) . . . . ? F3 C3 C4 C5 179.5(4) . . . . ? C2 C3 C4 C5 -1.3(7) . . . . ? F4 C4 C5 F5 0.2(7) . . . . ? C3 C4 C5 F5 -178.2(4) . . . . ? F4 C4 C5 C6 179.3(4) . . . . ? C3 C4 C5 C6 0.9(7) . . . . ? C2 C1 C6 F6 -179.4(3) . . . . ? N1 C1 C6 F6 0.9(6) . . . . ? C2 C1 C6 C5 0.2(6) . . . . ? N1 C1 C6 C5 -179.5(4) . . . . ? F5 C5 C6 F6 -1.5(6) . . . . ? C4 C5 C6 F6 179.3(4) . . . . ? F5 C5 C6 C1 178.8(4) . . . . ? C4 C5 C6 C1 -0.3(6) . . . . ? N1 C7 C8 C9 175.5(5) . . . . ? C7 C7 C8 C9 -3.0(8) 2 . . . ? C7 C8 C9 C9 -0.6(9) . . . 2 ? C8 C7 N1 C1 8.6(7) . . . . ? C7 C7 N1 C1 -172.8(5) 2 . . . ? C8 C7 N1 Pd1 175.7(4) . . . . ? C7 C7 N1 Pd1 -5.8(6) 2 . . . ? C2 C1 N1 C7 99.5(4) . . . . ? C6 C1 N1 C7 -80.8(5) . . . . ? C2 C1 N1 Pd1 -66.0(5) . . . . ? C6 C1 N1 Pd1 113.7(4) . . . . ? C7 N1 Pd1 N1 2.1(2) . . . 2 ? C1 N1 Pd1 N1 167.7(5) . . . 2 ? C7 N1 Pd1 N1 -93.7(3) . . . 4 ? C1 N1 Pd1 N1 71.9(4) . . . 4 ? C7 N1 Pd1 N1 172.3(4) . . . 3 ? C1 N1 Pd1 N1 -22.1(3) . . . 3 ? C104 O100 C101 C102 -3.3(17) . . . . ? C104 O100 C101 C112 -30.2(11) . . . . ? O100 C101 C102 C103 -21(2) . . . . ? C112 C101 C102 C103 61(2) . . . . ? C101 C102 C103 C104 37(2) . . . . ? C101 O100 C104 C103 27.4(15) . . . . ? C101 O100 C104 C113 0(2) . . . . ? C102 C103 C104 O100 -40(2) . . . . ? C102 C103 C104 C113 59(3) . . . . ? O100 C101 C112 C113 46(2) . . . . ? C102 C101 C112 C113 -59(2) . . . . ? O100 C104 C113 C112 29(3) . . . . ? C103 C104 C113 C112 -59(2) . . . . ? C101 C112 C113 C104 -46(3) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.622 _refine_diff_density_min -0.931 _refine_diff_density_rms 0.071 #===END data_no_3 _database_code_depnum_ccdc_archive 'CCDC 662505' #data_co44a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H8 Co F20 N4, C4 H8 O, 0.5(C4 H8 O)' _chemical_formula_sum 'C42 H20 Co F20 N4 O1.50' _chemical_formula_weight 1043.55 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' F F 0.0171 0.0103 '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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 59.292(3) _cell_length_b 15.3580(4) _cell_length_c 8.6688(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.952(3) _cell_angle_gamma 90.00 _cell_volume 7817.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 33737 _cell_measurement_theta_min 1.3 _cell_measurement_theta_max 25 _exptl_crystal_description plate _exptl_crystal_colour dark _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4152 _exptl_absorpt_coefficient_mu 0.579 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8324 _exptl_absorpt_correction_T_max 1.2798 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _diffrn_ambient_temperature 193(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 IPDS-II _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 48108 _diffrn_reflns_av_R_equivalents 0.1025 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -70 _diffrn_reflns_limit_h_max 70 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6890 _reflns_number_gt 4714 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.1' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0981P)^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 SHELXL _refine_ls_extinction_coef 0.00181(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6890 _refine_ls_number_parameters 686 _refine_ls_number_restraints 258 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1478 _refine_ls_wR_factor_gt 0.1378 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 1.019 _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 C1 C 0.38156(6) 0.4256(2) 0.6224(4) 0.0529(8) Uani 1 1 d . . . C2 C 0.38611(6) 0.5156(2) 0.6514(5) 0.0591(9) Uani 1 1 d . . . H2 H 0.4002 0.5333 0.7080 0.071 Uiso 1 1 calc R . . C3 C 0.37014(7) 0.5760(2) 0.5976(6) 0.0751(12) Uani 1 1 d . . . H3 H 0.3733 0.6360 0.6169 0.090 Uiso 1 1 calc R . . C4 C 0.34912(7) 0.5519(3) 0.5145(6) 0.0797(13) Uani 1 1 d . . . H4 H 0.3385 0.5954 0.4748 0.096 Uiso 1 1 calc R . . C5 C 0.34388(7) 0.4661(2) 0.4906(5) 0.0682(11) Uani 1 1 d . . . H5 H 0.3295 0.4500 0.4350 0.082 Uiso 1 1 calc R . . C6 C 0.35948(6) 0.4014(2) 0.5475(4) 0.0547(8) Uani 1 1 d . . . C7 C 0.41882(6) 0.3723(2) 0.7203(4) 0.0486(8) Uani 1 1 d . . . C8 C 0.42938(6) 0.3248(2) 0.8466(4) 0.0517(8) Uani 1 1 d . . . C9 C 0.45212(6) 0.3305(2) 0.8998(4) 0.0540(8) Uani 1 1 d . . . C10 C 0.46557(6) 0.3872(2) 0.8281(4) 0.0558(8) Uani 1 1 d . . . C11 C 0.45615(6) 0.4345(2) 0.7028(4) 0.0529(8) Uani 1 1 d . . . C12 C 0.43339(6) 0.4258(2) 0.6472(4) 0.0483(8) Uani 1 1 d . . . C13 C 0.33470(6) 0.2794(2) 0.4777(5) 0.0550(9) Uani 1 1 d . . . C14 C 0.31557(6) 0.2987(2) 0.5473(5) 0.0631(10) Uani 1 1 d . . . C15 C 0.29487(7) 0.2618(3) 0.4984(6) 0.0742(12) Uani 1 1 d . . . C16 C 0.29266(7) 0.2011(3) 0.3801(6) 0.0773(12) Uani 1 1 d . . . C17 C 0.31126(8) 0.1788(3) 0.3136(5) 0.0713(11) Uani 1 1 d . . . C18 C 0.33212(6) 0.2177(2) 0.3614(5) 0.0595(9) Uani 1 1 d . . . C19 C 0.38465(6) 0.0668(2) 0.6406(4) 0.0566(9) Uani 1 1 d . . . C20 C 0.38024(7) -0.0218(2) 0.6705(5) 0.0658(10) Uani 1 1 d . . . H20 H 0.3674 -0.0374 0.7187 0.079 Uiso 1 1 calc R . . C21 C 0.39449(8) -0.0845(2) 0.6300(5) 0.0732(12) Uani 1 1 d . . . H21 H 0.3913 -0.1439 0.6492 0.088 Uiso 1 1 calc R . . C22 C 0.41372(8) -0.0633(2) 0.5605(5) 0.0749(12) Uani 1 1 d . . . H22 H 0.4233 -0.1085 0.5327 0.090 Uiso 1 1 calc R . . C23 C 0.41886(7) 0.0215(2) 0.5319(5) 0.0642(10) Uani 1 1 d . . . H23 H 0.4320 0.0351 0.4851 0.077 Uiso 1 1 calc R . . C24 C 0.40449(6) 0.0889(2) 0.5724(4) 0.0559(9) Uani 1 1 d . . . C25 C 0.35086(7) 0.1286(2) 0.7259(4) 0.0583(9) Uani 1 1 d . . . C26 C 0.34611(7) 0.1826(3) 0.8472(5) 0.0639(10) Uani 1 1 d . . . C27 C 0.32476(8) 0.1880(3) 0.8929(5) 0.0750(11) Uani 1 1 d . . . C28 C 0.30755(8) 0.1380(3) 0.8176(6) 0.0788(12) Uani 1 1 d . . . C29 C 0.31129(7) 0.0849(3) 0.6987(6) 0.0740(12) Uani 1 1 d . . . C30 C 0.33255(7) 0.0805(2) 0.6526(5) 0.0641(10) Uani 1 1 d . . . C31 C 0.42616(6) 0.2105(2) 0.4924(4) 0.0515(8) Uani 1 1 d . . . C32 C 0.44830(6) 0.1975(2) 0.5670(4) 0.0564(9) Uani 1 1 d . . . C33 C 0.46668(6) 0.2389(2) 0.5185(5) 0.0590(9) Uani 1 1 d . . . C34 C 0.46355(6) 0.2976(2) 0.3972(4) 0.0590(9) Uani 1 1 d . . . C35 C 0.44200(6) 0.3134(2) 0.3242(4) 0.0544(8) Uani 1 1 d . . . C36 C 0.42379(6) 0.2701(2) 0.3715(4) 0.0522(8) Uani 1 1 d . . . F8 F 0.41664(4) 0.26950(13) 0.9199(3) 0.0640(5) Uani 1 1 d . . . F9 F 0.46158(4) 0.28079(15) 1.0180(2) 0.0679(6) Uani 1 1 d . . . F10 F 0.48770(3) 0.39570(15) 0.8838(3) 0.0700(6) Uani 1 1 d . . . F11 F 0.46911(4) 0.48709(14) 0.6285(3) 0.0670(6) Uani 1 1 d . . . F12 F 0.42531(3) 0.46835(12) 0.5154(2) 0.0586(5) Uani 1 1 d . . . F14 F 0.31709(4) 0.35401(16) 0.6685(3) 0.0781(7) Uani 1 1 d . . . F15 F 0.27676(4) 0.2830(2) 0.5680(4) 0.1054(9) Uani 1 1 d . . . F16 F 0.27255(5) 0.1634(2) 0.3328(4) 0.1114(11) Uani 1 1 d . . . F17 F 0.30989(5) 0.11736(17) 0.2022(3) 0.0956(9) Uani 1 1 d . . . F18 F 0.35021(4) 0.19326(15) 0.2939(3) 0.0746(6) Uani 1 1 d . . . F26 F 0.36258(4) 0.23372(14) 0.9205(3) 0.0726(6) Uani 1 1 d . . . F27 F 0.32093(5) 0.24450(18) 1.0036(3) 0.0934(8) Uani 1 1 d . . . F28 F 0.28651(5) 0.1443(2) 0.8595(4) 0.1083(10) Uani 1 1 d . . . F29 F 0.29398(4) 0.04045(16) 0.6176(4) 0.0921(8) Uani 1 1 d . . . F30 F 0.33539(4) 0.03189(14) 0.5259(3) 0.0751(6) Uani 1 1 d . . . F32 F 0.45206(4) 0.14576(14) 0.6926(3) 0.0672(6) Uani 1 1 d . . . F33 F 0.48767(4) 0.22431(17) 0.5937(3) 0.0781(7) Uani 1 1 d . . . F34 F 0.48128(4) 0.33890(16) 0.3515(3) 0.0738(6) Uani 1 1 d . . . F35 F 0.43825(4) 0.37346(13) 0.2117(2) 0.0631(5) Uani 1 1 d . . . F36 F 0.40287(3) 0.28861(13) 0.2986(2) 0.0607(5) Uani 1 1 d . . . N1 N 0.39579(5) 0.35769(18) 0.6628(3) 0.0515(7) Uani 1 1 d . . . N2 N 0.35669(5) 0.31332(18) 0.5316(4) 0.0546(7) Uani 1 1 d . . . N3 N 0.37227(5) 0.13721(19) 0.6732(4) 0.0578(7) Uani 1 1 d . . . N4 N 0.40648(5) 0.17614(17) 0.5444(4) 0.0545(7) Uani 1 1 d . . . Co1 Co 0.382878(8) 0.24608(3) 0.60635(6) 0.05174(18) Uani 1 1 d . . . O700 O 0.2740(5) 0.3515(14) 0.023(3) 0.295(10) Uani 0.50 1 d PDU A -2 C701 C 0.2599(6) 0.4228(19) -0.026(4) 0.271(13) Uani 0.50 1 d PDU A -2 H70I H 0.2438 0.4038 -0.0422 0.325 Uiso 0.50 1 calc PR A -2 H70J H 0.2638 0.4459 -0.1253 0.325 Uiso 0.50 1 calc PR A -2 C702 C 0.2630(5) 0.4894(16) 0.091(4) 0.257(12) Uani 0.50 1 d PDU A -2 H70K H 0.2482 0.5033 0.1261 0.309 Uiso 0.50 1 calc PR A -2 H70L H 0.2689 0.5430 0.0473 0.309 Uiso 0.50 1 calc PR A -2 C703 C 0.2791(6) 0.459(2) 0.224(4) 0.289(13) Uani 0.50 1 d PDU A -2 H70M H 0.2711 0.4442 0.3132 0.346 Uiso 0.50 1 calc PR A -2 H70N H 0.2908 0.5041 0.2564 0.346 Uiso 0.50 1 calc PR A -2 C704 C 0.2895(4) 0.3799(17) 0.160(4) 0.239(11) Uani 0.50 1 d PDU A -2 H70A H 0.3047 0.3942 0.1312 0.287 Uiso 0.50 1 calc PR A -2 H70B H 0.2914 0.3331 0.2396 0.287 Uiso 0.50 1 calc PR A -2 O800 O 0.4863(4) 0.0264(18) 0.396(3) 0.358(12) Uani 0.50 1 d PDU B -1 C801 C 0.5081(4) 0.0036(16) 0.349(4) 0.336(14) Uani 0.50 1 d PDU B -1 H80A H 0.5063 -0.0467 0.2770 0.404 Uiso 0.50 1 calc PR B -1 H80B H 0.5191 -0.0120 0.4411 0.404 Uiso 0.50 1 calc PR B -1 C802 C 0.5163(3) 0.0841(17) 0.267(4) 0.291(13) Uani 0.50 1 d PDU B -1 H80C H 0.5264 0.0675 0.1898 0.350 Uiso 0.50 1 calc PR B -1 H80D H 0.5245 0.1254 0.3430 0.350 Uiso 0.50 1 calc PR B -1 C803 C 0.4937(4) 0.1224(14) 0.188(4) 0.287(12) Uani 0.50 1 d PDU B -1 H80E H 0.4924 0.1186 0.0734 0.344 Uiso 0.50 1 calc PR B -1 H80F H 0.4920 0.1840 0.2185 0.344 Uiso 0.50 1 calc PR B -1 C804 C 0.4758(3) 0.064(2) 0.251(4) 0.304(13) Uani 0.50 1 d PDU B -1 H80G H 0.4624 0.0993 0.2679 0.364 Uiso 0.50 1 calc PR B -1 H80H H 0.4707 0.0177 0.1747 0.364 Uiso 0.50 1 calc PR B -1 O900 O 0.2633(3) 0.3769(18) 0.183(2) 0.264(8) Uani 0.50 1 d PDU C -1 C901 C 0.2844(2) 0.4050(12) 0.2469(17) 0.121(4) Uani 0.50 1 d PDU C -1 H90A H 0.2826 0.4516 0.3234 0.146 Uiso 0.50 1 calc PR C -1 H90B H 0.2927 0.3562 0.3036 0.146 Uiso 0.50 1 calc PR C -1 C902 C 0.2967(3) 0.4355(19) 0.1404(18) 0.165(7) Uani 0.50 1 d PDU C -1 H90C H 0.3089 0.3933 0.1267 0.198 Uiso 0.50 1 calc PR C -1 H90D H 0.3040 0.4909 0.1780 0.198 Uiso 0.50 1 calc PR C -1 C903 C 0.2827(4) 0.450(3) -0.009(2) 0.239(10) Uani 0.50 1 d PDU C -1 H90E H 0.2891 0.4208 -0.0949 0.287 Uiso 0.50 1 calc PR C -1 H90F H 0.2807 0.5129 -0.0324 0.287 Uiso 0.50 1 calc PR C -1 C904 C 0.2601(3) 0.408(3) 0.021(2) 0.223(10) Uani 0.50 1 d PDU C -1 H90G H 0.2476 0.4508 0.0049 0.268 Uiso 0.50 1 calc PR C -1 H90H H 0.2563 0.3584 -0.0511 0.268 Uiso 0.50 1 calc PR C -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 C1 0.057(2) 0.0400(17) 0.058(2) 0.0008(15) -0.0029(16) 0.0001(15) C2 0.060(2) 0.0417(18) 0.071(2) -0.0024(17) -0.0076(18) -0.0024(15) C3 0.074(3) 0.0380(19) 0.105(3) -0.006(2) -0.014(2) 0.0021(17) C4 0.073(3) 0.046(2) 0.111(4) 0.000(2) -0.021(2) 0.0069(18) C5 0.061(2) 0.0445(19) 0.092(3) -0.0038(19) -0.014(2) -0.0012(16) C6 0.057(2) 0.0411(17) 0.063(2) -0.0041(16) -0.0013(17) -0.0031(15) C7 0.0570(19) 0.0340(15) 0.052(2) -0.0030(14) -0.0008(15) 0.0000(14) C8 0.060(2) 0.0432(17) 0.050(2) 0.0021(15) -0.0001(16) -0.0012(15) C9 0.064(2) 0.052(2) 0.0448(19) 0.0036(16) 0.0006(16) 0.0121(16) C10 0.0522(19) 0.059(2) 0.055(2) -0.0063(17) 0.0021(16) 0.0054(16) C11 0.059(2) 0.0456(18) 0.054(2) -0.0041(16) 0.0080(16) 0.0003(15) C12 0.0579(19) 0.0401(16) 0.0449(19) -0.0015(14) -0.0002(15) 0.0012(14) C13 0.055(2) 0.0425(17) 0.064(2) 0.0007(16) -0.0036(17) -0.0013(14) C14 0.066(2) 0.053(2) 0.067(3) -0.0043(19) -0.0012(19) 0.0005(17) C15 0.057(2) 0.077(3) 0.086(3) 0.009(2) 0.000(2) -0.004(2) C16 0.061(2) 0.080(3) 0.085(3) 0.007(3) -0.010(2) -0.023(2) C17 0.090(3) 0.053(2) 0.064(3) -0.0031(19) -0.013(2) -0.015(2) C18 0.065(2) 0.0474(19) 0.062(2) -0.0023(17) -0.0038(18) -0.0034(17) C19 0.071(2) 0.0400(17) 0.054(2) 0.0027(15) -0.0070(18) -0.0041(16) C20 0.081(3) 0.0415(19) 0.069(3) 0.0059(18) -0.011(2) -0.0081(18) C21 0.088(3) 0.0385(19) 0.084(3) 0.0034(19) -0.020(2) -0.0036(19) C22 0.091(3) 0.042(2) 0.084(3) -0.008(2) -0.015(2) 0.010(2) C23 0.076(2) 0.048(2) 0.065(2) -0.0034(18) -0.0041(19) 0.0069(17) C24 0.069(2) 0.0391(17) 0.055(2) 0.0011(15) -0.0091(17) -0.0008(15) C25 0.069(2) 0.0426(18) 0.061(2) 0.0043(17) 0.0013(18) -0.0073(16) C26 0.073(2) 0.053(2) 0.065(2) 0.0067(19) 0.007(2) -0.0069(18) C27 0.094(3) 0.061(2) 0.070(3) 0.005(2) 0.013(2) -0.005(2) C28 0.076(3) 0.069(3) 0.093(3) 0.013(3) 0.019(2) 0.000(2) C29 0.066(3) 0.056(2) 0.094(3) 0.017(2) -0.007(2) -0.0149(19) C30 0.079(3) 0.0421(18) 0.068(3) 0.0034(18) -0.002(2) -0.0079(17) C31 0.061(2) 0.0381(16) 0.054(2) -0.0027(15) 0.0017(16) 0.0029(15) C32 0.070(2) 0.0458(19) 0.051(2) 0.0024(16) 0.0017(17) 0.0063(16) C33 0.056(2) 0.059(2) 0.059(2) -0.0039(18) -0.0021(17) 0.0075(17) C34 0.060(2) 0.060(2) 0.058(2) -0.0061(18) 0.0086(17) -0.0014(17) C35 0.070(2) 0.0443(18) 0.048(2) 0.0015(16) 0.0059(17) 0.0050(16) C36 0.056(2) 0.0444(18) 0.053(2) -0.0047(15) -0.0012(16) 0.0044(14) F8 0.0730(13) 0.0530(11) 0.0646(13) 0.0163(10) 0.0041(10) -0.0045(10) F9 0.0713(13) 0.0753(14) 0.0539(12) 0.0100(11) -0.0030(10) 0.0189(11) F10 0.0499(11) 0.0843(15) 0.0729(15) -0.0002(12) -0.0011(10) 0.0037(10) F11 0.0625(12) 0.0612(12) 0.0788(15) 0.0079(11) 0.0149(11) -0.0061(10) F12 0.0720(13) 0.0479(11) 0.0533(12) 0.0085(9) -0.0011(9) 0.0014(9) F14 0.0782(15) 0.0737(15) 0.0819(16) -0.0132(13) 0.0097(12) 0.0051(12) F15 0.0658(16) 0.122(2) 0.130(3) 0.004(2) 0.0197(16) -0.0001(15) F16 0.0820(18) 0.116(2) 0.125(2) 0.0074(19) -0.0244(16) -0.0431(16) F17 0.130(2) 0.0705(16) 0.0785(17) -0.0167(14) -0.0143(15) -0.0292(15) F18 0.0855(16) 0.0597(13) 0.0776(16) -0.0147(12) 0.0081(12) 0.0010(11) F26 0.0896(16) 0.0586(13) 0.0672(14) -0.0071(11) 0.0025(12) -0.0112(11) F27 0.119(2) 0.0825(18) 0.0851(19) -0.0021(15) 0.0358(16) 0.0009(15) F28 0.0878(19) 0.109(2) 0.134(3) 0.0184(19) 0.0352(18) -0.0052(16) F29 0.0733(15) 0.0642(14) 0.131(2) 0.0104(15) -0.0129(14) -0.0157(12) F30 0.0853(15) 0.0514(12) 0.0822(16) -0.0048(12) -0.0113(12) -0.0098(11) F32 0.0749(14) 0.0583(12) 0.0640(13) 0.0094(10) -0.0059(10) 0.0059(10) F33 0.0594(13) 0.0890(16) 0.0812(17) 0.0067(13) -0.0071(11) 0.0037(11) F34 0.0660(13) 0.0826(16) 0.0731(15) 0.0017(12) 0.0107(11) -0.0099(11) F35 0.0789(14) 0.0532(11) 0.0577(12) 0.0059(10) 0.0107(10) 0.0020(10) F36 0.0610(12) 0.0524(11) 0.0649(13) 0.0059(10) -0.0049(10) 0.0048(9) N1 0.0553(16) 0.0428(15) 0.0534(17) 0.0012(13) -0.0036(13) 0.0001(12) N2 0.0584(17) 0.0398(14) 0.0628(19) -0.0043(13) -0.0018(13) -0.0053(12) N3 0.0646(18) 0.0421(15) 0.0639(19) 0.0009(14) -0.0009(15) -0.0045(13) N4 0.0659(18) 0.0357(14) 0.0593(18) 0.0028(13) -0.0008(14) -0.0034(12) Co1 0.0565(3) 0.0346(3) 0.0618(3) 0.0012(2) 0.0000(2) -0.00194(19) O700 0.239(18) 0.231(17) 0.39(3) -0.035(16) -0.051(17) 0.076(15) C701 0.21(2) 0.23(2) 0.34(3) -0.012(19) -0.098(19) 0.041(17) C702 0.20(2) 0.183(18) 0.36(3) -0.001(18) -0.06(2) 0.062(15) C703 0.25(3) 0.23(2) 0.35(3) -0.010(18) -0.10(2) 0.000(18) C704 0.106(14) 0.194(19) 0.39(3) 0.080(19) -0.060(16) 0.019(12) O800 0.255(18) 0.37(3) 0.44(3) 0.02(2) 0.04(2) 0.038(19) C801 0.25(2) 0.27(2) 0.48(3) 0.04(2) 0.03(2) 0.10(2) C802 0.183(16) 0.22(3) 0.46(3) -0.06(2) 0.00(2) 0.031(17) C803 0.19(2) 0.182(18) 0.49(3) -0.01(2) 0.04(2) 0.057(18) C804 0.192(16) 0.26(3) 0.47(3) 0.02(3) 0.06(2) 0.061(19) O900 0.162(10) 0.38(2) 0.225(13) 0.124(15) -0.050(9) -0.067(13) C901 0.081(8) 0.143(13) 0.142(10) 0.019(9) 0.019(6) 0.027(8) C902 0.146(11) 0.223(19) 0.123(11) 0.022(12) 0.012(8) -0.032(13) C903 0.160(14) 0.37(3) 0.174(13) 0.062(17) -0.021(11) -0.066(17) C904 0.113(11) 0.41(3) 0.151(12) 0.039(17) 0.021(9) -0.015(16) _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 C1 N1 1.357(4) . ? C1 C2 1.423(5) . ? C1 C6 1.428(5) . ? C2 C3 1.362(5) . ? C2 H2 0.9500 . ? C3 C4 1.400(6) . ? C3 H3 0.9500 . ? C4 C5 1.364(5) . ? C4 H4 0.9500 . ? C5 C6 1.399(5) . ? C5 H5 0.9500 . ? C6 N2 1.368(4) . ? C7 C8 1.390(5) . ? C7 C12 1.405(5) . ? C7 N1 1.406(4) . ? C8 F8 1.353(4) . ? C8 C9 1.366(5) . ? C9 F9 1.338(4) . ? C9 C10 1.384(5) . ? C10 F10 1.341(4) . ? C10 C11 1.361(5) . ? C11 F11 1.339(4) . ? C11 C12 1.375(5) . ? C12 F12 1.346(4) . ? C13 C18 1.377(5) . ? C13 C14 1.389(5) . ? C13 N2 1.422(4) . ? C14 F14 1.344(4) . ? C14 C15 1.365(6) . ? C15 F15 1.342(5) . ? C15 C16 1.379(7) . ? C16 F16 1.338(5) . ? C16 C17 1.356(6) . ? C17 F17 1.345(5) . ? C17 C18 1.384(5) . ? C18 F18 1.344(4) . ? C19 N3 1.359(5) . ? C19 C20 1.417(5) . ? C19 C24 1.429(5) . ? C20 C21 1.358(6) . ? C20 H20 0.9500 . ? C21 C22 1.400(6) . ? C21 H21 0.9500 . ? C22 C23 1.369(6) . ? C22 H22 0.9500 . ? C23 C24 1.415(5) . ? C23 H23 0.9500 . ? C24 N4 1.370(4) . ? C25 C30 1.392(5) . ? C25 C26 1.399(6) . ? C25 N3 1.413(5) . ? C26 F26 1.342(4) . ? C26 C27 1.380(6) . ? C27 F27 1.337(5) . ? C27 C28 1.368(7) . ? C28 F28 1.350(5) . ? C28 C29 1.357(7) . ? C29 F29 1.347(5) . ? C29 C30 1.376(6) . ? C30 F30 1.358(5) . ? C31 C36 1.384(5) . ? C31 C32 1.395(5) . ? C31 N4 1.411(4) . ? C32 F32 1.341(4) . ? C32 C33 1.377(5) . ? C33 F33 1.342(4) . ? C33 C34 1.378(6) . ? C34 F34 1.334(4) . ? C34 C35 1.367(5) . ? C35 F35 1.338(4) . ? C35 C36 1.378(5) . ? C36 F36 1.342(4) . ? N1 Co1 1.913(3) . ? N2 Co1 1.903(3) . ? N3 Co1 1.905(3) . ? N4 Co1 1.900(3) . ? O700 C701 1.407(18) . ? O700 C704 1.467(18) . ? C701 C702 1.434(18) . ? C701 H70I 0.9900 . ? C701 H70J 0.9900 . ? C702 C703 1.462(18) . ? C702 H70K 0.9900 . ? C702 H70L 0.9900 . ? C703 C704 1.506(19) . ? C703 H70M 0.9900 . ? C703 H70N 0.9900 . ? C704 H70A 0.9900 . ? C704 H70B 0.9900 . ? O800 C801 1.4497(11) . ? O800 C804 1.4501(11) . ? C801 C802 1.5394(11) . ? C801 H80A 0.9900 . ? C801 H80B 0.9900 . ? C802 C803 1.5396(11) . ? C802 H80C 0.9900 . ? C802 H80D 0.9900 . ? C803 C804 1.5399(11) . ? C803 H80E 0.9900 . ? C803 H80F 0.9900 . ? C804 H80G 0.9900 . ? C804 H80H 0.9900 . ? O900 C901 1.363(15) . ? O900 C904 1.471(16) . ? C901 C902 1.338(15) . ? C901 H90A 0.9900 . ? C901 H90B 0.9900 . ? C902 C903 1.456(16) . ? C902 H90C 0.9900 . ? C902 H90D 0.9900 . ? C903 C904 1.540(18) . ? C903 H90E 0.9900 . ? C903 H90F 0.9900 . ? C904 H90G 0.9900 . ? C904 H90H 0.9900 . ? 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 N1 C1 C2 127.2(3) . . ? N1 C1 C6 114.5(3) . . ? C2 C1 C6 118.2(3) . . ? C3 C2 C1 119.7(3) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 121.5(4) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C5 C4 C3 120.1(4) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.4(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? N2 C6 C5 126.9(3) . . ? N2 C6 C1 113.2(3) . . ? C5 C6 C1 119.7(3) . . ? C8 C7 C12 115.1(3) . . ? C8 C7 N1 120.4(3) . . ? C12 C7 N1 124.1(3) . . ? F8 C8 C9 118.1(3) . . ? F8 C8 C7 118.6(3) . . ? C9 C8 C7 123.3(3) . . ? F9 C9 C8 120.8(3) . . ? F9 C9 C10 119.8(3) . . ? C8 C9 C10 119.5(3) . . ? F10 C10 C11 120.6(3) . . ? F10 C10 C9 119.7(3) . . ? C11 C10 C9 119.7(3) . . ? F11 C11 C10 120.4(3) . . ? F11 C11 C12 119.4(3) . . ? C10 C11 C12 120.1(3) . . ? F12 C12 C11 117.8(3) . . ? F12 C12 C7 119.9(3) . . ? C11 C12 C7 122.2(3) . . ? C18 C13 C14 116.8(3) . . ? C18 C13 N2 119.8(3) . . ? C14 C13 N2 123.1(3) . . ? F14 C14 C15 117.7(4) . . ? F14 C14 C13 120.3(3) . . ? C15 C14 C13 122.0(4) . . ? F15 C15 C14 120.0(4) . . ? F15 C15 C16 119.9(4) . . ? C14 C15 C16 120.0(4) . . ? F16 C16 C17 120.2(5) . . ? F16 C16 C15 120.6(5) . . ? C17 C16 C15 119.2(4) . . ? F17 C17 C16 120.7(4) . . ? F17 C17 C18 118.7(4) . . ? C16 C17 C18 120.6(4) . . ? F18 C18 C13 119.8(3) . . ? F18 C18 C17 118.9(4) . . ? C13 C18 C17 121.3(4) . . ? N3 C19 C20 127.5(4) . . ? N3 C19 C24 113.3(3) . . ? C20 C19 C24 119.2(3) . . ? C21 C20 C19 119.8(4) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C22 121.3(4) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C23 C22 C21 120.9(4) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 119.6(4) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? N4 C24 C23 127.0(4) . . ? N4 C24 C19 113.7(3) . . ? C23 C24 C19 119.2(3) . . ? C30 C25 C26 115.6(4) . . ? C30 C25 N3 125.5(4) . . ? C26 C25 N3 118.1(3) . . ? F26 C26 C27 117.7(4) . . ? F26 C26 C25 119.6(4) . . ? C27 C26 C25 122.6(4) . . ? F27 C27 C28 121.1(4) . . ? F27 C27 C26 119.9(4) . . ? C28 C27 C26 118.9(4) . . ? F28 C28 C29 120.1(4) . . ? F28 C28 C27 119.2(5) . . ? C29 C28 C27 120.7(4) . . ? F29 C29 C28 120.6(4) . . ? F29 C29 C30 119.1(4) . . ? C28 C29 C30 120.2(4) . . ? F30 C30 C29 118.9(4) . . ? F30 C30 C25 119.0(4) . . ? C29 C30 C25 121.9(4) . . ? C36 C31 C32 115.9(3) . . ? C36 C31 N4 119.2(3) . . ? C32 C31 N4 124.4(3) . . ? F32 C32 C33 118.2(3) . . ? F32 C32 C31 120.1(3) . . ? C33 C32 C31 121.7(3) . . ? F33 C33 C32 119.6(3) . . ? F33 C33 C34 119.9(4) . . ? C32 C33 C34 120.5(3) . . ? F34 C34 C35 120.2(3) . . ? F34 C34 C33 120.6(3) . . ? C35 C34 C33 119.2(3) . . ? F35 C35 C34 120.7(3) . . ? F35 C35 C36 119.4(3) . . ? C34 C35 C36 119.8(3) . . ? F36 C36 C35 118.0(3) . . ? F36 C36 C31 119.1(3) . . ? C35 C36 C31 122.9(3) . . ? C1 N1 C7 120.5(3) . . ? C1 N1 Co1 114.2(2) . . ? C7 N1 Co1 124.6(2) . . ? C6 N2 C13 119.3(3) . . ? C6 N2 Co1 114.9(2) . . ? C13 N2 Co1 125.5(2) . . ? C19 N3 C25 121.8(3) . . ? C19 N3 Co1 115.1(2) . . ? C25 N3 Co1 122.0(2) . . ? C24 N4 C31 121.2(3) . . ? C24 N4 Co1 114.7(2) . . ? C31 N4 Co1 123.6(2) . . ? N4 Co1 N2 144.02(13) . . ? N4 Co1 N3 82.93(12) . . ? N2 Co1 N3 106.96(13) . . ? N4 Co1 N1 107.14(12) . . ? N2 Co1 N1 83.08(11) . . ? N3 Co1 N1 147.78(13) . . ? C701 O700 C704 106.9(15) . . ? O700 C701 C702 109.5(16) . . ? O700 C701 H70I 109.8 . . ? C702 C701 H70I 109.8 . . ? O700 C701 H70J 109.8 . . ? C702 C701 H70J 109.8 . . ? H70I C701 H70J 108.2 . . ? C701 C702 C703 109.5(16) . . ? C701 C702 H70K 109.8 . . ? C703 C702 H70K 109.8 . . ? C701 C702 H70L 109.8 . . ? C703 C702 H70L 109.8 . . ? H70K C702 H70L 108.2 . . ? C702 C703 C704 103.1(16) . . ? C702 C703 H70M 111.1 . . ? C704 C703 H70M 111.1 . . ? C702 C703 H70N 111.1 . . ? C704 C703 H70N 111.1 . . ? H70M C703 H70N 109.1 . . ? O700 C704 C703 107.1(15) . . ? O700 C704 H70A 110.3 . . ? C703 C704 H70A 110.3 . . ? O700 C704 H70B 110.3 . . ? C703 C704 H70B 110.3 . . ? H70A C704 H70B 108.5 . . ? C801 O800 C804 98.1(15) . . ? O800 C801 C802 106.9(13) . . ? O800 C801 H80A 110.3 . . ? C802 C801 H80A 110.3 . . ? O800 C801 H80B 110.3 . . ? C802 C801 H80B 110.3 . . ? H80A C801 H80B 108.6 . . ? C801 C802 C803 101.3(11) . . ? C801 C802 H80C 111.5 . . ? C803 C802 H80C 111.5 . . ? C801 C802 H80D 111.5 . . ? C803 C802 H80D 111.5 . . ? H80C C802 H80D 109.3 . . ? C802 C803 C804 102.9(10) . . ? C802 C803 H80E 111.2 . . ? C804 C803 H80E 111.2 . . ? C802 C803 H80F 111.2 . . ? C804 C803 H80F 111.2 . . ? H80E C803 H80F 109.1 . . ? O800 C804 C803 107.8(13) . . ? O800 C804 H80G 110.1 . . ? C803 C804 H80G 110.1 . . ? O800 C804 H80H 110.1 . . ? C803 C804 H80H 110.1 . . ? H80G C804 H80H 108.5 . . ? C901 O900 C904 105.9(12) . . ? C902 C901 O900 112.9(14) . . ? C902 C901 H90A 109.0 . . ? O900 C901 H90A 109.0 . . ? C902 C901 H90B 109.0 . . ? O900 C901 H90B 109.0 . . ? H90A C901 H90B 107.8 . . ? C901 C902 C903 111.6(14) . . ? C901 C902 H90C 109.3 . . ? C903 C902 H90C 109.3 . . ? C901 C902 H90D 109.3 . . ? C903 C902 H90D 109.3 . . ? H90C C902 H90D 108.0 . . ? C902 C903 C904 100.8(13) . . ? C902 C903 H90E 111.6 . . ? C904 C903 H90E 111.6 . . ? C902 C903 H90F 111.6 . . ? C904 C903 H90F 111.6 . . ? H90E C903 H90F 109.4 . . ? O900 C904 C903 107.3(13) . . ? O900 C904 H90G 110.3 . . ? C903 C904 H90G 110.3 . . ? O900 C904 H90H 110.3 . . ? C903 C904 H90H 110.3 . . ? H90G C904 H90H 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 177.6(4) . . . . ? C6 C1 C2 C3 -4.8(6) . . . . ? C1 C2 C3 C4 0.4(7) . . . . ? C2 C3 C4 C5 2.4(8) . . . . ? C3 C4 C5 C6 -0.6(8) . . . . ? C4 C5 C6 N2 -179.5(4) . . . . ? C4 C5 C6 C1 -4.0(7) . . . . ? N1 C1 C6 N2 0.6(5) . . . . ? C2 C1 C6 N2 -177.3(3) . . . . ? N1 C1 C6 C5 -175.5(4) . . . . ? C2 C1 C6 C5 6.6(6) . . . . ? C12 C7 C8 F8 -177.8(3) . . . . ? N1 C7 C8 F8 -5.0(5) . . . . ? C12 C7 C8 C9 1.5(5) . . . . ? N1 C7 C8 C9 174.3(3) . . . . ? F8 C8 C9 F9 2.0(5) . . . . ? C7 C8 C9 F9 -177.3(3) . . . . ? F8 C8 C9 C10 -179.4(3) . . . . ? C7 C8 C9 C10 1.3(5) . . . . ? F9 C9 C10 F10 -4.0(5) . . . . ? C8 C9 C10 F10 177.3(3) . . . . ? F9 C9 C10 C11 176.6(3) . . . . ? C8 C9 C10 C11 -2.1(5) . . . . ? F10 C10 C11 F11 3.2(5) . . . . ? C9 C10 C11 F11 -177.4(3) . . . . ? F10 C10 C11 C12 -179.6(3) . . . . ? C9 C10 C11 C12 -0.2(5) . . . . ? F11 C11 C12 F12 2.7(5) . . . . ? C10 C11 C12 F12 -174.5(3) . . . . ? F11 C11 C12 C7 -179.5(3) . . . . ? C10 C11 C12 C7 3.3(5) . . . . ? C8 C7 C12 F12 174.0(3) . . . . ? N1 C7 C12 F12 1.5(5) . . . . ? C8 C7 C12 C11 -3.8(5) . . . . ? N1 C7 C12 C11 -176.3(3) . . . . ? C18 C13 C14 F14 175.6(3) . . . . ? N2 C13 C14 F14 2.1(5) . . . . ? C18 C13 C14 C15 -3.0(6) . . . . ? N2 C13 C14 C15 -176.5(4) . . . . ? F14 C14 C15 F15 2.0(6) . . . . ? C13 C14 C15 F15 -179.4(4) . . . . ? F14 C14 C15 C16 -176.5(4) . . . . ? C13 C14 C15 C16 2.2(6) . . . . ? F15 C15 C16 F16 0.5(7) . . . . ? C14 C15 C16 F16 179.0(4) . . . . ? F15 C15 C16 C17 -178.4(4) . . . . ? C14 C15 C16 C17 0.1(7) . . . . ? F16 C16 C17 F17 -1.6(6) . . . . ? C15 C16 C17 F17 177.3(4) . . . . ? F16 C16 C17 C18 179.8(4) . . . . ? C15 C16 C17 C18 -1.3(7) . . . . ? C14 C13 C18 F18 -177.2(3) . . . . ? N2 C13 C18 F18 -3.5(5) . . . . ? C14 C13 C18 C17 1.8(6) . . . . ? N2 C13 C18 C17 175.5(3) . . . . ? F17 C17 C18 F18 0.6(5) . . . . ? C16 C17 C18 F18 179.3(4) . . . . ? F17 C17 C18 C13 -178.3(4) . . . . ? C16 C17 C18 C13 0.4(6) . . . . ? N3 C19 C20 C21 180.0(4) . . . . ? C24 C19 C20 C21 -1.9(6) . . . . ? C19 C20 C21 C22 0.8(6) . . . . ? C20 C21 C22 C23 0.4(7) . . . . ? C21 C22 C23 C24 -0.3(6) . . . . ? C22 C23 C24 N4 -176.3(4) . . . . ? C22 C23 C24 C19 -0.9(6) . . . . ? N3 C19 C24 N4 -3.7(5) . . . . ? C20 C19 C24 N4 177.9(3) . . . . ? N3 C19 C24 C23 -179.7(3) . . . . ? C20 C19 C24 C23 2.0(5) . . . . ? C30 C25 C26 F26 -177.6(3) . . . . ? N3 C25 C26 F26 -7.0(5) . . . . ? C30 C25 C26 C27 0.3(6) . . . . ? N3 C25 C26 C27 170.9(4) . . . . ? F26 C26 C27 F27 1.8(6) . . . . ? C25 C26 C27 F27 -176.1(4) . . . . ? F26 C26 C27 C28 178.5(4) . . . . ? C25 C26 C27 C28 0.6(6) . . . . ? F27 C27 C28 F28 -2.0(6) . . . . ? C26 C27 C28 F28 -178.7(4) . . . . ? F27 C27 C28 C29 175.8(4) . . . . ? C26 C27 C28 C29 -0.8(7) . . . . ? F28 C28 C29 F29 2.5(6) . . . . ? C27 C28 C29 F29 -175.3(4) . . . . ? F28 C28 C29 C30 178.0(4) . . . . ? C27 C28 C29 C30 0.2(7) . . . . ? F29 C29 C30 F30 0.5(5) . . . . ? C28 C29 C30 F30 -175.0(4) . . . . ? F29 C29 C30 C25 176.3(3) . . . . ? C28 C29 C30 C25 0.8(6) . . . . ? C26 C25 C30 F30 174.8(3) . . . . ? N3 C25 C30 F30 5.1(5) . . . . ? C26 C25 C30 C29 -1.0(5) . . . . ? N3 C25 C30 C29 -170.8(4) . . . . ? C36 C31 C32 F32 175.1(3) . . . . ? N4 C31 C32 F32 3.5(5) . . . . ? C36 C31 C32 C33 -2.6(5) . . . . ? N4 C31 C32 C33 -174.2(3) . . . . ? F32 C32 C33 F33 2.4(5) . . . . ? C31 C32 C33 F33 -179.9(3) . . . . ? F32 C32 C33 C34 -175.3(3) . . . . ? C31 C32 C33 C34 2.4(5) . . . . ? F33 C33 C34 F34 1.3(5) . . . . ? C32 C33 C34 F34 178.9(3) . . . . ? F33 C33 C34 C35 -178.4(3) . . . . ? C32 C33 C34 C35 -0.7(6) . . . . ? F34 C34 C35 F35 -3.3(5) . . . . ? C33 C34 C35 F35 176.3(3) . . . . ? F34 C34 C35 C36 179.7(3) . . . . ? C33 C34 C35 C36 -0.7(5) . . . . ? F35 C35 C36 F36 1.9(5) . . . . ? C34 C35 C36 F36 178.9(3) . . . . ? F35 C35 C36 C31 -176.6(3) . . . . ? C34 C35 C36 C31 0.4(5) . . . . ? C32 C31 C36 F36 -177.3(3) . . . . ? N4 C31 C36 F36 -5.3(5) . . . . ? C32 C31 C36 C35 1.2(5) . . . . ? N4 C31 C36 C35 173.2(3) . . . . ? C2 C1 N1 C7 -10.0(6) . . . . ? C6 C1 N1 C7 172.4(3) . . . . ? C2 C1 N1 Co1 178.6(3) . . . . ? C6 C1 N1 Co1 1.0(4) . . . . ? C8 C7 N1 C1 137.3(3) . . . . ? C12 C7 N1 C1 -50.6(5) . . . . ? C8 C7 N1 Co1 -52.3(4) . . . . ? C12 C7 N1 Co1 119.9(3) . . . . ? C5 C6 N2 C13 -12.3(6) . . . . ? C1 C6 N2 C13 171.9(3) . . . . ? C5 C6 N2 Co1 173.9(3) . . . . ? C1 C6 N2 Co1 -1.8(4) . . . . ? C18 C13 N2 C6 132.5(4) . . . . ? C14 C13 N2 C6 -54.2(5) . . . . ? C18 C13 N2 Co1 -54.5(5) . . . . ? C14 C13 N2 Co1 118.8(3) . . . . ? C20 C19 N3 C25 -8.5(6) . . . . ? C24 C19 N3 C25 173.3(3) . . . . ? C20 C19 N3 Co1 -177.2(3) . . . . ? C24 C19 N3 Co1 4.6(4) . . . . ? C30 C25 N3 C19 -53.2(5) . . . . ? C26 C25 N3 C19 137.3(4) . . . . ? C30 C25 N3 Co1 114.8(4) . . . . ? C26 C25 N3 Co1 -54.7(4) . . . . ? C23 C24 N4 C31 -11.0(6) . . . . ? C19 C24 N4 C31 173.5(3) . . . . ? C23 C24 N4 Co1 176.7(3) . . . . ? C19 C24 N4 Co1 1.1(4) . . . . ? C36 C31 N4 C24 134.8(4) . . . . ? C32 C31 N4 C24 -53.9(5) . . . . ? C36 C31 N4 Co1 -53.5(4) . . . . ? C32 C31 N4 Co1 117.8(3) . . . . ? C24 N4 Co1 N2 -108.2(3) . . . . ? C31 N4 Co1 N2 79.7(3) . . . . ? C24 N4 Co1 N3 1.1(3) . . . . ? C31 N4 Co1 N3 -171.1(3) . . . . ? C24 N4 Co1 N1 149.7(2) . . . . ? C31 N4 Co1 N1 -22.4(3) . . . . ? C6 N2 Co1 N4 -107.9(3) . . . . ? C13 N2 Co1 N4 78.8(4) . . . . ? C6 N2 Co1 N3 150.5(3) . . . . ? C13 N2 Co1 N3 -22.8(3) . . . . ? C6 N2 Co1 N1 1.9(3) . . . . ? C13 N2 Co1 N1 -171.4(3) . . . . ? C19 N3 Co1 N4 -3.2(3) . . . . ? C25 N3 Co1 N4 -171.9(3) . . . . ? C19 N3 Co1 N2 141.4(3) . . . . ? C25 N3 Co1 N2 -27.3(3) . . . . ? C19 N3 Co1 N1 -114.3(3) . . . . ? C25 N3 Co1 N1 77.0(4) . . . . ? C1 N1 Co1 N4 143.1(3) . . . . ? C7 N1 Co1 N4 -27.9(3) . . . . ? C1 N1 Co1 N2 -1.6(3) . . . . ? C7 N1 Co1 N2 -172.6(3) . . . . ? C1 N1 Co1 N3 -112.6(3) . . . . ? C7 N1 Co1 N3 76.4(4) . . . . ? C704 O700 C701 C702 -10(5) . . . . ? O700 C701 C702 C703 -2(5) . . . . ? C701 C702 C703 C704 13(5) . . . . ? C701 O700 C704 C703 19(5) . . . . ? C702 C703 C704 O700 -19(5) . . . . ? C804 O800 C801 C802 48(3) . . . . ? O800 C801 C802 C803 -34(3) . . . . ? C801 C802 C803 C804 6(3) . . . . ? C801 O800 C804 C803 -43(3) . . . . ? C802 C803 C804 O800 23(3) . . . . ? C904 O900 C901 C902 -12(3) . . . . ? O900 C901 C902 C903 14(4) . . . . ? C901 C902 C903 C904 -9(4) . . . . ? C901 O900 C904 C903 5(4) . . . . ? C902 C903 C904 O900 2(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.593 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.085 #===END data_no_4 _database_code_depnum_ccdc_archive 'CCDC 662506' #data_khus01a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H8 Cu F20 N4, C4 H8 O, 0.5(C4 H8 O)' _chemical_formula_sum 'C42 H20 Cu F20 N4 O1.50' _chemical_formula_weight 1048.16 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' F F 0.0171 0.0103 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 59.219(3) _cell_length_b 15.3696(8) _cell_length_c 8.5864(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.394(4) _cell_angle_gamma 90.00 _cell_volume 7750.1(7) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 19977 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 24.9 _exptl_crystal_description plate _exptl_crystal_colour dark _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4168 _exptl_absorpt_coefficient_mu 0.705 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8963 _exptl_absorpt_correction_T_max 0.9922 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'STOE IPDS-II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 39236 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -69 _diffrn_reflns_limit_h_max 70 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 24.94 _reflns_number_total 6763 _reflns_number_gt 4464 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.1' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0582P)^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 6763 _refine_ls_number_parameters 685 _refine_ls_number_restraints 262 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0979 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.948 _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 C1 C 0.38096(6) 0.42638(18) 0.6225(4) 0.0412(8) Uani 1 1 d . . . C2 C 0.38566(6) 0.51657(19) 0.6501(4) 0.0491(9) Uani 1 1 d . . . H2 H 0.4000 0.5341 0.7034 0.059 Uiso 1 1 calc R . . C3 C 0.36973(7) 0.5772(2) 0.6006(5) 0.0629(11) Uani 1 1 d . . . H3 H 0.3728 0.6369 0.6227 0.076 Uiso 1 1 calc R . . C4 C 0.34852(7) 0.5529(2) 0.5165(5) 0.0686(12) Uani 1 1 d . . . H4 H 0.3380 0.5966 0.4758 0.082 Uiso 1 1 calc R . . C5 C 0.34305(6) 0.4679(2) 0.4936(5) 0.0552(10) Uani 1 1 d . . . H5 H 0.3285 0.4525 0.4414 0.066 Uiso 1 1 calc R . . C6 C 0.35882(6) 0.40203(19) 0.5466(4) 0.0433(8) Uani 1 1 d . . . C7 C 0.41824(5) 0.37321(18) 0.7208(3) 0.0358(7) Uani 1 1 d . . . C8 C 0.42861(6) 0.32386(19) 0.8477(4) 0.0389(7) Uani 1 1 d . . . C9 C 0.45154(6) 0.3286(2) 0.8986(3) 0.0415(8) Uani 1 1 d . . . C10 C 0.46504(6) 0.3849(2) 0.8276(4) 0.0432(8) Uani 1 1 d . . . C11 C 0.45554(6) 0.4336(2) 0.7013(4) 0.0406(7) Uani 1 1 d . . . C12 C 0.43289(6) 0.42578(18) 0.6478(3) 0.0385(7) Uani 1 1 d . . . C13 C 0.33394(6) 0.28205(19) 0.4749(4) 0.0403(8) Uani 1 1 d . . . C14 C 0.31455(6) 0.3014(2) 0.5449(4) 0.0470(8) Uani 1 1 d . . . C15 C 0.29376(6) 0.2642(3) 0.4970(5) 0.0586(10) Uani 1 1 d . . . C16 C 0.29176(7) 0.2032(3) 0.3788(5) 0.0615(11) Uani 1 1 d . . . C17 C 0.31039(7) 0.1803(2) 0.3116(4) 0.0548(10) Uani 1 1 d . . . C18 C 0.33125(6) 0.2191(2) 0.3581(4) 0.0445(8) Uani 1 1 d . . . C19 C 0.38374(6) 0.06615(19) 0.6392(4) 0.0425(8) Uani 1 1 d . . . C20 C 0.37905(7) -0.0234(2) 0.6668(4) 0.0516(9) Uani 1 1 d . . . H20 H 0.3658 -0.0392 0.7114 0.062 Uiso 1 1 calc R . . C21 C 0.39354(7) -0.0853(2) 0.6295(5) 0.0577(10) Uani 1 1 d . . . H21 H 0.3905 -0.1445 0.6498 0.069 Uiso 1 1 calc R . . C22 C 0.41309(7) -0.0639(2) 0.5613(5) 0.0590(10) Uani 1 1 d . . . H22 H 0.4227 -0.1092 0.5336 0.071 Uiso 1 1 calc R . . C23 C 0.41859(7) 0.0203(2) 0.5339(4) 0.0512(9) Uani 1 1 d . . . H23 H 0.4321 0.0335 0.4901 0.061 Uiso 1 1 calc R . . C24 C 0.40389(6) 0.08794(19) 0.5716(4) 0.0424(8) Uani 1 1 d . . . C25 C 0.34994(6) 0.12743(19) 0.7252(4) 0.0446(8) Uani 1 1 d . . . C26 C 0.34452(7) 0.1820(2) 0.8461(4) 0.0510(9) Uani 1 1 d . . . C27 C 0.32306(7) 0.1881(2) 0.8880(4) 0.0581(10) Uani 1 1 d . . . C28 C 0.30597(7) 0.1386(3) 0.8137(5) 0.0632(10) Uani 1 1 d . . . C29 C 0.31020(7) 0.0841(2) 0.6930(5) 0.0597(10) Uani 1 1 d . . . C30 C 0.33174(6) 0.0794(2) 0.6500(4) 0.0497(9) Uani 1 1 d . . . C31 C 0.42582(6) 0.20772(19) 0.4902(4) 0.0402(7) Uani 1 1 d . . . C32 C 0.44790(6) 0.1952(2) 0.5650(4) 0.0425(8) Uani 1 1 d . . . C33 C 0.46634(6) 0.2369(2) 0.5193(4) 0.0472(8) Uani 1 1 d . . . C34 C 0.46351(6) 0.2968(2) 0.3981(4) 0.0456(8) Uani 1 1 d . . . C35 C 0.44196(6) 0.3132(2) 0.3254(4) 0.0422(8) Uani 1 1 d . . . C36 C 0.42386(6) 0.26999(19) 0.3699(4) 0.0393(7) Uani 1 1 d . . . F8 F 0.41582(3) 0.26921(12) 0.9210(2) 0.0531(5) Uani 1 1 d . . . F9 F 0.46079(3) 0.27771(13) 1.0169(2) 0.0558(5) Uani 1 1 d . . . F10 F 0.48717(3) 0.39210(14) 0.8815(2) 0.0588(5) Uani 1 1 d . . . F11 F 0.46882(3) 0.48521(13) 0.6257(2) 0.0565(5) Uani 1 1 d . . . F12 F 0.42489(3) 0.46904(11) 0.5152(2) 0.0475(5) Uani 1 1 d . . . F14 F 0.31622(4) 0.35676(14) 0.6677(2) 0.0615(5) Uani 1 1 d . . . F15 F 0.27580(4) 0.28506(19) 0.5687(3) 0.0898(8) Uani 1 1 d . . . F16 F 0.27165(4) 0.16540(18) 0.3339(3) 0.0910(9) Uani 1 1 d . . . F17 F 0.30882(5) 0.11744(14) 0.2011(3) 0.0761(7) Uani 1 1 d . . . F18 F 0.34917(4) 0.19418(13) 0.2891(2) 0.0595(5) Uani 1 1 d . . . F26 F 0.36096(4) 0.23332(12) 0.9205(2) 0.0579(5) Uani 1 1 d . . . F27 F 0.31892(5) 0.24528(16) 0.9994(3) 0.0765(7) Uani 1 1 d . . . F28 F 0.28489(5) 0.14460(18) 0.8525(4) 0.0910(8) Uani 1 1 d . . . F29 F 0.29314(4) 0.03972(14) 0.6102(3) 0.0781(7) Uani 1 1 d . . . F30 F 0.33491(4) 0.03109(12) 0.5225(2) 0.0587(6) Uani 1 1 d . . . F32 F 0.45129(3) 0.14241(12) 0.6919(2) 0.0538(5) Uani 1 1 d . . . F33 F 0.48718(3) 0.22213(15) 0.5957(3) 0.0658(6) Uani 1 1 d . . . F34 F 0.48142(4) 0.33826(14) 0.3536(2) 0.0627(6) Uani 1 1 d . . . F35 F 0.43870(3) 0.37445(11) 0.2129(2) 0.0504(5) Uani 1 1 d . . . F36 F 0.40292(3) 0.28895(12) 0.2965(2) 0.0490(5) Uani 1 1 d . . . N1 N 0.39506(4) 0.35941(16) 0.6679(3) 0.0410(6) Uani 1 1 d . . . N2 N 0.35575(5) 0.31556(16) 0.5248(3) 0.0421(6) Uani 1 1 d . . . N3 N 0.37150(5) 0.13565(16) 0.6778(3) 0.0427(6) Uani 1 1 d . . . N4 N 0.40595(5) 0.17381(15) 0.5380(3) 0.0411(6) Uani 1 1 d . . . Cu1 Cu 0.382175(7) 0.24622(2) 0.60601(4) 0.03819(11) Uani 1 1 d . . . O700 O 0.2900(3) 0.3863(12) 0.164(3) 0.254(9) Uani 0.50 1 d PDU A 2 C701 C 0.2725(3) 0.3547(13) 0.056(3) 0.207(8) Uani 0.50 1 d PDU A 2 H70I H 0.2630 0.3123 0.1055 0.248 Uiso 0.50 1 calc PR A 2 H70J H 0.2785 0.3267 -0.0338 0.248 Uiso 0.50 1 calc PR A 2 C702 C 0.2594(3) 0.4347(11) 0.007(2) 0.167(6) Uani 0.50 1 d PDU A 2 H70K H 0.2432 0.4210 -0.0277 0.201 Uiso 0.50 1 calc PR A 2 H70L H 0.2658 0.4646 -0.0796 0.201 Uiso 0.50 1 calc PR A 2 C703 C 0.2620(4) 0.4895(15) 0.154(3) 0.251(10) Uani 0.50 1 d PDU A 2 H70M H 0.2476 0.4920 0.2011 0.301 Uiso 0.50 1 calc PR A 2 H70N H 0.2669 0.5494 0.1323 0.301 Uiso 0.50 1 calc PR A 2 C704 C 0.2807(3) 0.4409(17) 0.262(3) 0.255(10) Uani 0.50 1 d PDU A 2 H70O H 0.2922 0.4820 0.3134 0.307 Uiso 0.50 1 calc PR A 2 H70P H 0.2740 0.4079 0.3444 0.307 Uiso 0.50 1 calc PR A 2 O800 O 0.4926(4) 0.0011(14) 0.388(3) 0.372(12) Uani 0.50 1 d PDU B -1 C801 C 0.5154(4) 0.0368(18) 0.413(3) 0.305(12) Uani 0.50 1 d PDU B -1 H80A H 0.5268 -0.0097 0.4397 0.366 Uiso 0.50 1 calc PR B -1 H80B H 0.5168 0.0806 0.4979 0.366 Uiso 0.50 1 calc PR B -1 C802 C 0.5185(4) 0.0792(18) 0.254(4) 0.280(11) Uani 0.50 1 d PDU B -1 H80C H 0.5228 0.0356 0.1784 0.336 Uiso 0.50 1 calc PR B -1 H80D H 0.5302 0.1257 0.2675 0.336 Uiso 0.50 1 calc PR B -1 C803 C 0.4946(4) 0.1166(14) 0.202(3) 0.276(11) Uani 0.50 1 d PDU B -1 H80E H 0.4897 0.1043 0.0892 0.331 Uiso 0.50 1 calc PR B -1 H80F H 0.4944 0.1803 0.2185 0.331 Uiso 0.50 1 calc PR B -1 C804 C 0.4791(4) 0.0698(14) 0.306(3) 0.312(12) Uani 0.50 1 d PDU B -1 H80G H 0.4738 0.1111 0.3819 0.374 Uiso 0.50 1 calc PR B -1 H80H H 0.4656 0.0452 0.2404 0.374 Uiso 0.50 1 calc PR B -1 O900 O 0.2810(5) 0.4873(17) 0.000(3) 0.374(12) Uani 0.50 1 d PDU C 1 C901 C 0.2728(7) 0.4198(18) -0.095(3) 0.357(14) Uani 0.50 1 d PDU C 1 H90C H 0.2852 0.3836 -0.1258 0.428 Uiso 0.50 1 calc PR C 1 H90D H 0.2631 0.4410 -0.1899 0.428 Uiso 0.50 1 calc PR C 1 C902 C 0.2590(5) 0.371(3) 0.011(3) 0.321(14) Uani 0.50 1 d PDU C 1 H90E H 0.2602 0.3075 -0.0061 0.385 Uiso 0.50 1 calc PR C 1 H90F H 0.2428 0.3880 -0.0095 0.385 Uiso 0.50 1 calc PR C 1 C903 C 0.2688(5) 0.3945(18) 0.179(3) 0.299(13) Uani 0.50 1 d PDU C 1 H90G H 0.2731 0.3421 0.2431 0.359 Uiso 0.50 1 calc PR C 1 H90H H 0.2582 0.4305 0.2312 0.359 Uiso 0.50 1 calc PR C 1 C904 C 0.2901(5) 0.447(2) 0.146(3) 0.304(14) Uani 0.50 1 d PDU C 1 H90A H 0.2946 0.4907 0.2291 0.365 Uiso 0.50 1 calc PR C 1 H90B H 0.3032 0.4088 0.1336 0.365 Uiso 0.50 1 calc PR C 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 C1 0.0437(19) 0.0278(15) 0.0495(19) 0.0011(14) -0.0040(15) -0.0009(14) C2 0.047(2) 0.0295(16) 0.067(2) -0.0015(15) -0.0083(17) -0.0018(14) C3 0.061(2) 0.0275(16) 0.094(3) -0.0025(17) -0.017(2) 0.0004(16) C4 0.059(3) 0.0338(18) 0.104(3) 0.0022(19) -0.023(2) 0.0057(17) C5 0.047(2) 0.0371(18) 0.076(2) 0.0007(17) -0.0139(18) -0.0005(15) C6 0.044(2) 0.0307(16) 0.0518(19) -0.0005(14) -0.0051(16) -0.0002(13) C7 0.0398(18) 0.0271(14) 0.0387(16) -0.0011(12) -0.0019(14) -0.0004(12) C8 0.0452(19) 0.0306(15) 0.0411(17) 0.0014(13) 0.0062(15) 0.0001(13) C9 0.047(2) 0.0418(17) 0.0341(16) 0.0008(13) -0.0028(14) 0.0120(15) C10 0.0348(18) 0.0483(18) 0.0458(18) -0.0072(15) 0.0021(15) 0.0057(15) C11 0.0431(19) 0.0366(16) 0.0430(17) -0.0019(14) 0.0097(15) -0.0011(14) C12 0.048(2) 0.0302(15) 0.0360(16) -0.0018(12) -0.0008(14) 0.0035(13) C13 0.0398(19) 0.0304(15) 0.0475(19) 0.0011(13) -0.0069(15) -0.0023(13) C14 0.046(2) 0.0434(19) 0.050(2) -0.0051(15) -0.0009(16) 0.0007(15) C15 0.041(2) 0.064(2) 0.070(2) 0.0082(19) 0.0032(18) 0.0012(18) C16 0.048(2) 0.059(2) 0.073(3) 0.006(2) -0.011(2) -0.0165(18) C17 0.066(3) 0.0439(19) 0.050(2) -0.0028(16) -0.0093(19) -0.0121(18) C18 0.046(2) 0.0358(16) 0.0494(19) -0.0023(14) -0.0030(16) -0.0002(14) C19 0.050(2) 0.0331(16) 0.0415(18) 0.0024(13) -0.0068(16) -0.0047(15) C20 0.062(2) 0.0305(17) 0.059(2) 0.0074(15) -0.0083(18) -0.0076(16) C21 0.069(3) 0.0286(17) 0.069(2) 0.0012(16) -0.014(2) -0.0046(17) C22 0.069(3) 0.0317(18) 0.071(2) -0.0066(16) -0.009(2) 0.0081(17) C23 0.060(2) 0.0328(17) 0.058(2) -0.0027(15) -0.0019(18) 0.0059(15) C24 0.052(2) 0.0300(15) 0.0419(17) -0.0008(13) -0.0063(15) -0.0010(14) C25 0.053(2) 0.0319(16) 0.0482(19) 0.0047(14) 0.0032(16) -0.0065(14) C26 0.059(2) 0.0424(18) 0.051(2) 0.0053(16) 0.0054(18) -0.0084(17) C27 0.074(3) 0.046(2) 0.057(2) 0.0067(18) 0.019(2) -0.0012(19) C28 0.059(3) 0.052(2) 0.082(3) 0.014(2) 0.022(2) -0.0017(19) C29 0.047(2) 0.046(2) 0.083(3) 0.021(2) -0.006(2) -0.0115(17) C30 0.058(2) 0.0334(17) 0.055(2) 0.0053(15) -0.0041(17) -0.0060(15) C31 0.046(2) 0.0309(15) 0.0428(18) -0.0028(13) 0.0017(15) 0.0035(14) C32 0.050(2) 0.0367(17) 0.0393(17) 0.0006(13) 0.0008(15) 0.0055(15) C33 0.0410(19) 0.050(2) 0.0482(18) -0.0040(15) -0.0023(15) 0.0065(16) C34 0.042(2) 0.0488(19) 0.0472(19) -0.0072(15) 0.0122(16) -0.0057(15) C35 0.052(2) 0.0360(16) 0.0383(17) -0.0003(13) 0.0051(15) 0.0033(15) C36 0.0410(18) 0.0343(16) 0.0412(17) -0.0024(12) -0.0001(14) 0.0045(13) F8 0.0565(12) 0.0444(11) 0.0571(11) 0.0172(9) 0.0027(10) -0.0032(9) F9 0.0581(13) 0.0647(12) 0.0423(10) 0.0103(9) -0.0025(9) 0.0197(10) F10 0.0352(11) 0.0758(14) 0.0637(12) -0.0015(10) -0.0006(9) 0.0061(10) F11 0.0472(12) 0.0546(12) 0.0698(13) 0.0089(10) 0.0158(10) -0.0033(9) F12 0.0574(12) 0.0409(10) 0.0427(10) 0.0092(8) -0.0001(9) 0.0016(9) F14 0.0600(14) 0.0609(13) 0.0638(13) -0.0148(10) 0.0088(10) 0.0048(10) F15 0.0456(14) 0.113(2) 0.114(2) -0.0022(16) 0.0210(14) -0.0016(13) F16 0.0583(15) 0.0975(19) 0.109(2) 0.0056(15) -0.0194(14) -0.0367(14) F17 0.1026(19) 0.0530(13) 0.0665(14) -0.0162(11) -0.0128(13) -0.0236(12) F18 0.0638(14) 0.0499(11) 0.0652(13) -0.0169(10) 0.0095(11) 0.0022(10) F26 0.0690(14) 0.0484(12) 0.0552(11) -0.0080(9) 0.0035(10) -0.0104(10) F27 0.0945(18) 0.0707(14) 0.0701(14) 0.0005(13) 0.0329(13) 0.0059(14) F28 0.0662(17) 0.0877(18) 0.124(2) 0.0174(16) 0.0328(16) -0.0017(14) F29 0.0553(14) 0.0529(13) 0.119(2) 0.0111(13) -0.0171(13) -0.0133(11) F30 0.0660(14) 0.0404(10) 0.0652(13) -0.0067(10) -0.0091(11) -0.0063(9) F32 0.0574(13) 0.0493(11) 0.0511(11) 0.0105(9) -0.0062(9) 0.0048(9) F33 0.0420(12) 0.0799(15) 0.0709(14) 0.0074(11) -0.0107(10) 0.0004(10) F34 0.0511(13) 0.0745(14) 0.0635(13) 0.0011(11) 0.0110(10) -0.0138(11) F35 0.0617(13) 0.0423(10) 0.0486(10) 0.0074(8) 0.0121(9) 0.0011(9) F36 0.0438(11) 0.0435(10) 0.0573(11) 0.0104(8) -0.0027(9) 0.0042(8) N1 0.0404(16) 0.0319(13) 0.0478(15) 0.0019(11) -0.0047(12) 0.0007(11) N2 0.0424(16) 0.0308(13) 0.0512(16) -0.0021(11) -0.0008(12) -0.0044(11) N3 0.0490(18) 0.0320(13) 0.0461(15) 0.0005(11) 0.0026(13) -0.0026(12) N4 0.0465(16) 0.0268(13) 0.0482(15) 0.0033(11) -0.0001(12) -0.0008(11) Cu1 0.0399(2) 0.02551(17) 0.0477(2) 0.00127(17) 0.00003(15) -0.00189(16) O700 0.151(12) 0.226(17) 0.36(2) 0.005(14) -0.057(12) 0.021(10) C701 0.118(13) 0.169(14) 0.33(2) -0.033(14) -0.001(14) 0.013(11) C702 0.083(9) 0.178(14) 0.244(17) 0.056(12) 0.036(10) -0.019(9) C703 0.173(17) 0.162(15) 0.41(3) -0.057(16) 0.005(18) 0.001(12) C704 0.20(2) 0.25(2) 0.30(2) -0.024(15) -0.038(15) -0.066(15) O800 0.30(2) 0.30(2) 0.50(3) 0.11(2) -0.01(2) -0.034(18) C801 0.27(2) 0.24(3) 0.41(3) 0.04(2) 0.03(2) 0.004(19) C802 0.238(17) 0.22(3) 0.37(3) 0.00(2) 0.01(2) 0.02(2) C803 0.26(2) 0.191(18) 0.38(3) 0.005(17) 0.06(2) 0.07(2) C804 0.253(17) 0.21(2) 0.47(3) 0.01(2) 0.07(2) 0.04(2) O900 0.39(3) 0.41(3) 0.29(2) -0.003(18) -0.06(2) 0.00(2) C901 0.33(3) 0.47(3) 0.254(19) -0.05(2) -0.03(2) 0.01(3) C902 0.33(3) 0.39(3) 0.23(2) -0.06(2) -0.03(2) 0.04(2) C903 0.26(3) 0.35(3) 0.236(18) 0.022(17) -0.134(18) 0.09(2) C904 0.34(3) 0.31(3) 0.24(2) -0.060(19) -0.03(2) 0.06(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.351(4) . ? C1 C2 1.428(4) . ? C1 C6 1.437(4) . ? C2 C3 1.355(5) . ? C2 H2 0.9500 . ? C3 C4 1.415(5) . ? C3 H3 0.9500 . ? C4 C5 1.355(5) . ? C4 H4 0.9500 . ? C5 C6 1.412(5) . ? C5 H5 0.9500 . ? C6 N2 1.351(4) . ? C7 C12 1.392(4) . ? C7 C8 1.402(4) . ? C7 N1 1.406(4) . ? C8 F8 1.341(4) . ? C8 C9 1.374(5) . ? C9 F9 1.343(3) . ? C9 C10 1.373(5) . ? C10 F10 1.337(4) . ? C10 C11 1.377(4) . ? C11 F11 1.342(4) . ? C11 C12 1.366(4) . ? C12 F12 1.351(3) . ? C13 C18 1.388(5) . ? C13 C14 1.395(5) . ? C13 N2 1.406(4) . ? C14 F14 1.348(4) . ? C14 C15 1.372(5) . ? C15 F15 1.335(5) . ? C15 C16 1.376(6) . ? C16 F16 1.337(4) . ? C16 C17 1.355(6) . ? C17 F17 1.349(4) . ? C17 C18 1.383(5) . ? C18 F18 1.337(4) . ? C19 N3 1.356(4) . ? C19 C20 1.429(4) . ? C19 C24 1.432(5) . ? C20 C21 1.347(5) . ? C20 H20 0.9500 . ? C21 C22 1.402(6) . ? C21 H21 0.9500 . ? C22 C23 1.362(5) . ? C22 H22 0.9500 . ? C23 C24 1.420(5) . ? C23 H23 0.9500 . ? C24 N4 1.360(4) . ? C25 C30 1.394(5) . ? C25 N3 1.395(4) . ? C25 C26 1.404(5) . ? C26 F26 1.348(4) . ? C26 C27 1.368(5) . ? C27 F27 1.344(4) . ? C27 C28 1.358(6) . ? C28 F28 1.336(5) . ? C28 C29 1.380(6) . ? C29 F29 1.345(4) . ? C29 C30 1.375(5) . ? C30 F30 1.356(4) . ? C31 C32 1.394(4) . ? C31 N4 1.396(4) . ? C31 C36 1.402(4) . ? C32 F32 1.352(3) . ? C32 C33 1.367(5) . ? C33 F33 1.340(4) . ? C33 C34 1.383(5) . ? C34 F34 1.335(4) . ? C34 C35 1.370(5) . ? C35 F35 1.345(3) . ? C35 C36 1.356(5) . ? C36 F36 1.349(3) . ? N1 Cu1 1.946(2) . ? N2 Cu1 1.947(3) . ? N3 Cu1 1.941(3) . ? N4 Cu1 1.942(3) . ? O700 C704 1.356(17) . ? O700 C701 1.389(16) . ? C701 C702 1.487(16) . ? C701 H70I 0.9900 . ? C701 H70J 0.9900 . ? C702 C703 1.511(15) . ? C702 H70K 0.9900 . ? C702 H70L 0.9900 . ? C703 C704 1.542(18) . ? C703 H70M 0.9900 . ? C703 H70N 0.9900 . ? C704 H70O 0.9900 . ? C704 H70P 0.9900 . ? O800 C801 1.4496(11) . ? O800 C804 1.4496(11) . ? C801 C802 1.5398(11) . ? C801 H80A 0.9900 . ? C801 H80B 0.9900 . ? C802 C803 1.5399(11) . ? C802 H80C 0.9900 . ? C802 H80D 0.9900 . ? C803 C804 1.5400(11) . ? C803 H80E 0.9900 . ? C803 H80F 0.9900 . ? C804 H80G 0.9900 . ? C804 H80H 0.9900 . ? O900 C901 1.370(18) . ? O900 C904 1.436(19) . ? C901 C902 1.498(18) . ? C901 H90C 0.9900 . ? C901 H90D 0.9900 . ? C902 C903 1.527(17) . ? C902 H90E 0.9900 . ? C902 H90F 0.9900 . ? C903 C904 1.552(18) . ? C903 H90G 0.9900 . ? C903 H90H 0.9900 . ? C904 H90A 0.9900 . ? C904 H90B 0.9900 . ? 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 N1 C1 C2 126.3(3) . . ? N1 C1 C6 115.2(3) . . ? C2 C1 C6 118.4(3) . . ? C3 C2 C1 120.2(3) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 121.0(3) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 120.5(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.6(3) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? N2 C6 C5 126.1(3) . . ? N2 C6 C1 114.7(3) . . ? C5 C6 C1 119.1(3) . . ? C12 C7 C8 115.3(3) . . ? C12 C7 N1 125.5(3) . . ? C8 C7 N1 118.7(3) . . ? F8 C8 C9 118.6(3) . . ? F8 C8 C7 119.1(3) . . ? C9 C8 C7 122.3(3) . . ? F9 C9 C10 119.9(3) . . ? F9 C9 C8 120.0(3) . . ? C10 C9 C8 120.1(3) . . ? F10 C10 C9 119.9(3) . . ? F10 C10 C11 120.7(3) . . ? C9 C10 C11 119.3(3) . . ? F11 C11 C12 120.1(3) . . ? F11 C11 C10 119.8(3) . . ? C12 C11 C10 120.1(3) . . ? F12 C12 C11 117.6(3) . . ? F12 C12 C7 119.6(3) . . ? C11 C12 C7 122.8(3) . . ? C18 C13 C14 115.8(3) . . ? C18 C13 N2 119.4(3) . . ? C14 C13 N2 124.4(3) . . ? F14 C14 C15 118.1(3) . . ? F14 C14 C13 119.3(3) . . ? C15 C14 C13 122.6(3) . . ? F15 C15 C14 119.9(4) . . ? F15 C15 C16 120.4(4) . . ? C14 C15 C16 119.6(4) . . ? F16 C16 C17 120.6(4) . . ? F16 C16 C15 119.8(4) . . ? C17 C16 C15 119.5(3) . . ? F17 C17 C16 119.9(3) . . ? F17 C17 C18 119.3(4) . . ? C16 C17 C18 120.8(3) . . ? F18 C18 C17 118.7(3) . . ? F18 C18 C13 119.8(3) . . ? C17 C18 C13 121.6(3) . . ? N3 C19 C20 126.6(3) . . ? N3 C19 C24 114.5(3) . . ? C20 C19 C24 118.8(3) . . ? C21 C20 C19 119.8(4) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C22 121.3(3) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C23 C22 C21 121.5(4) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C22 C23 C24 119.3(4) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? N4 C24 C23 126.1(3) . . ? N4 C24 C19 114.5(3) . . ? C23 C24 C19 119.2(3) . . ? C30 C25 N3 126.5(3) . . ? C30 C25 C26 115.0(3) . . ? N3 C25 C26 117.8(3) . . ? F26 C26 C27 118.3(3) . . ? F26 C26 C25 118.7(3) . . ? C27 C26 C25 123.0(3) . . ? F27 C27 C28 120.5(4) . . ? F27 C27 C26 119.5(4) . . ? C28 C27 C26 120.0(4) . . ? F28 C28 C27 120.5(4) . . ? F28 C28 C29 119.6(4) . . ? C27 C28 C29 119.8(4) . . ? F29 C29 C30 119.4(4) . . ? F29 C29 C28 120.6(4) . . ? C30 C29 C28 119.9(4) . . ? F30 C30 C29 118.4(3) . . ? F30 C30 C25 119.0(3) . . ? C29 C30 C25 122.4(4) . . ? C32 C31 N4 126.1(3) . . ? C32 C31 C36 114.7(3) . . ? N4 C31 C36 118.6(3) . . ? F32 C32 C33 118.1(3) . . ? F32 C32 C31 119.2(3) . . ? C33 C32 C31 122.7(3) . . ? F33 C33 C32 120.0(3) . . ? F33 C33 C34 119.7(3) . . ? C32 C33 C34 120.3(3) . . ? F34 C34 C35 120.6(3) . . ? F34 C34 C33 120.6(3) . . ? C35 C34 C33 118.8(3) . . ? F35 C35 C36 119.9(3) . . ? F35 C35 C34 119.7(3) . . ? C36 C35 C34 120.3(3) . . ? F36 C36 C35 118.4(3) . . ? F36 C36 C31 118.4(3) . . ? C35 C36 C31 123.2(3) . . ? C1 N1 C7 121.3(2) . . ? C1 N1 Cu1 113.4(2) . . ? C7 N1 Cu1 123.74(19) . . ? C6 N2 C13 120.3(3) . . ? C6 N2 Cu1 113.7(2) . . ? C13 N2 Cu1 125.00(19) . . ? C19 N3 C25 122.6(3) . . ? C19 N3 Cu1 113.9(2) . . ? C25 N3 Cu1 121.3(2) . . ? C24 N4 C31 121.8(3) . . ? C24 N4 Cu1 113.9(2) . . ? C31 N4 Cu1 123.05(19) . . ? N3 Cu1 N4 82.65(11) . . ? N3 Cu1 N1 145.92(11) . . ? N4 Cu1 N1 108.70(11) . . ? N3 Cu1 N2 108.25(11) . . ? N4 Cu1 N2 141.84(11) . . ? N1 Cu1 N2 82.95(10) . . ? C704 O700 C701 107.4(18) . . ? O700 C701 C702 102.7(15) . . ? O700 C701 H70I 111.2 . . ? C702 C701 H70I 111.2 . . ? O700 C701 H70J 111.2 . . ? C702 C701 H70J 111.2 . . ? H70I C701 H70J 109.1 . . ? C701 C702 C703 103.1(15) . . ? C701 C702 H70K 111.1 . . ? C703 C702 H70K 111.1 . . ? C701 C702 H70L 111.1 . . ? C703 C702 H70L 111.1 . . ? H70K C702 H70L 109.1 . . ? C702 C703 C704 102.9(13) . . ? C702 C703 H70M 111.2 . . ? C704 C703 H70M 111.2 . . ? C702 C703 H70N 111.2 . . ? C704 C703 H70N 111.2 . . ? H70M C703 H70N 109.1 . . ? O700 C704 C703 104.2(16) . . ? O700 C704 H70O 110.9 . . ? C703 C704 H70O 110.9 . . ? O700 C704 H70P 110.9 . . ? C703 C704 H70P 110.9 . . ? H70O C704 H70P 108.9 . . ? C801 O800 C804 103.9(15) . . ? O800 C801 C802 104.1(13) . . ? O800 C801 H80A 110.9 . . ? C802 C801 H80A 110.9 . . ? O800 C801 H80B 110.9 . . ? C802 C801 H80B 110.9 . . ? H80A C801 H80B 109.0 . . ? C801 C802 C803 102.0(11) . . ? C801 C802 H80C 111.4 . . ? C803 C802 H80C 111.4 . . ? C801 C802 H80D 111.4 . . ? C803 C802 H80D 111.4 . . ? H80C C802 H80D 109.2 . . ? C802 C803 C804 104.5(10) . . ? C802 C803 H80E 110.9 . . ? C804 C803 H80E 110.9 . . ? C802 C803 H80F 110.9 . . ? C804 C803 H80F 110.9 . . ? H80E C803 H80F 108.9 . . ? O800 C804 C803 106.8(11) . . ? O800 C804 H80G 110.4 . . ? C803 C804 H80G 110.4 . . ? O800 C804 H80H 110.4 . . ? C803 C804 H80H 110.4 . . ? H80G C804 H80H 108.6 . . ? C901 O900 C904 105(2) . . ? O900 C901 C902 102(2) . . ? O900 C901 H90C 111.5 . . ? C902 C901 H90C 111.5 . . ? O900 C901 H90D 111.5 . . ? C902 C901 H90D 111.5 . . ? H90C C901 H90D 109.3 . . ? C901 C902 C903 106.3(17) . . ? C901 C902 H90E 110.5 . . ? C903 C902 H90E 110.5 . . ? C901 C902 H90F 110.5 . . ? C903 C902 H90F 110.5 . . ? H90E C902 H90F 108.7 . . ? C902 C903 C904 99.9(16) . . ? C902 C903 H90G 111.8 . . ? C904 C903 H90G 111.8 . . ? C902 C903 H90H 111.8 . . ? C904 C903 H90H 111.8 . . ? H90G C903 H90H 109.5 . . ? O900 C904 C903 99.3(18) . . ? O900 C904 H90A 111.9 . . ? C903 C904 H90A 111.9 . . ? O900 C904 H90B 111.9 . . ? C903 C904 H90B 111.9 . . ? H90A C904 H90B 109.6 . . ? 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 N1 C1 C2 C3 -178.7(4) . . . . ? C6 C1 C2 C3 -2.2(6) . . . . ? C1 C2 C3 C4 -2.1(7) . . . . ? C2 C3 C4 C5 4.8(7) . . . . ? C3 C4 C5 C6 -3.0(7) . . . . ? C4 C5 C6 N2 -176.9(4) . . . . ? C4 C5 C6 C1 -1.3(6) . . . . ? N1 C1 C6 N2 -3.1(5) . . . . ? C2 C1 C6 N2 180.0(3) . . . . ? N1 C1 C6 C5 -179.3(3) . . . . ? C2 C1 C6 C5 3.9(5) . . . . ? C12 C7 C8 F8 -177.7(3) . . . . ? N1 C7 C8 F8 -4.2(4) . . . . ? C12 C7 C8 C9 1.4(4) . . . . ? N1 C7 C8 C9 174.9(3) . . . . ? F8 C8 C9 F9 1.6(4) . . . . ? C7 C8 C9 F9 -177.6(3) . . . . ? F8 C8 C9 C10 -179.0(3) . . . . ? C7 C8 C9 C10 1.9(5) . . . . ? F9 C9 C10 F10 -3.3(5) . . . . ? C8 C9 C10 F10 177.2(3) . . . . ? F9 C9 C10 C11 176.7(3) . . . . ? C8 C9 C10 C11 -2.7(5) . . . . ? F10 C10 C11 F11 3.7(5) . . . . ? C9 C10 C11 F11 -176.3(3) . . . . ? F10 C10 C11 C12 -179.8(3) . . . . ? C9 C10 C11 C12 0.1(5) . . . . ? F11 C11 C12 F12 2.3(4) . . . . ? C10 C11 C12 F12 -174.2(3) . . . . ? F11 C11 C12 C7 179.9(3) . . . . ? C10 C11 C12 C7 3.4(5) . . . . ? C8 C7 C12 F12 173.5(3) . . . . ? N1 C7 C12 F12 0.5(4) . . . . ? C8 C7 C12 C11 -4.1(4) . . . . ? N1 C7 C12 C11 -177.0(3) . . . . ? C18 C13 C14 F14 174.7(3) . . . . ? N2 C13 C14 F14 1.0(5) . . . . ? C18 C13 C14 C15 -3.2(5) . . . . ? N2 C13 C14 C15 -176.9(3) . . . . ? F14 C14 C15 F15 1.9(5) . . . . ? C13 C14 C15 F15 179.9(3) . . . . ? F14 C14 C15 C16 -175.8(3) . . . . ? C13 C14 C15 C16 2.1(5) . . . . ? F15 C15 C16 F16 0.9(6) . . . . ? C14 C15 C16 F16 178.6(3) . . . . ? F15 C15 C16 C17 -177.4(4) . . . . ? C14 C15 C16 C17 0.3(6) . . . . ? F16 C16 C17 F17 -1.6(6) . . . . ? C15 C16 C17 F17 176.7(3) . . . . ? F16 C16 C17 C18 -179.8(3) . . . . ? C15 C16 C17 C18 -1.5(6) . . . . ? F17 C17 C18 F18 1.5(5) . . . . ? C16 C17 C18 F18 179.7(3) . . . . ? F17 C17 C18 C13 -177.9(3) . . . . ? C16 C17 C18 C13 0.3(5) . . . . ? C14 C13 C18 F18 -177.5(3) . . . . ? N2 C13 C18 F18 -3.4(5) . . . . ? C14 C13 C18 C17 2.0(5) . . . . ? N2 C13 C18 C17 176.0(3) . . . . ? N3 C19 C20 C21 -176.3(3) . . . . ? C24 C19 C20 C21 0.1(5) . . . . ? C19 C20 C21 C22 -1.0(5) . . . . ? C20 C21 C22 C23 1.8(6) . . . . ? C21 C22 C23 C24 -1.6(5) . . . . ? C22 C23 C24 N4 -173.5(3) . . . . ? C22 C23 C24 C19 0.7(5) . . . . ? N3 C19 C24 N4 -8.2(4) . . . . ? C20 C19 C24 N4 174.9(3) . . . . ? N3 C19 C24 C23 176.9(3) . . . . ? C20 C19 C24 C23 0.1(4) . . . . ? C30 C25 C26 F26 -177.3(3) . . . . ? N3 C25 C26 F26 -6.4(4) . . . . ? C30 C25 C26 C27 0.1(5) . . . . ? N3 C25 C26 C27 171.0(3) . . . . ? F26 C26 C27 F27 0.9(5) . . . . ? C25 C26 C27 F27 -176.5(3) . . . . ? F26 C26 C27 C28 178.8(3) . . . . ? C25 C26 C27 C28 1.4(6) . . . . ? F27 C27 C28 F28 -1.5(6) . . . . ? C26 C27 C28 F28 -179.3(3) . . . . ? F27 C27 C28 C29 176.0(3) . . . . ? C26 C27 C28 C29 -1.8(6) . . . . ? F28 C28 C29 F29 2.7(5) . . . . ? C27 C28 C29 F29 -174.9(3) . . . . ? F28 C28 C29 C30 178.3(3) . . . . ? C27 C28 C29 C30 0.8(6) . . . . ? F29 C29 C30 F30 1.2(5) . . . . ? C28 C29 C30 F30 -174.4(3) . . . . ? F29 C29 C30 C25 176.4(3) . . . . ? C28 C29 C30 C25 0.7(5) . . . . ? N3 C25 C30 F30 4.0(5) . . . . ? C26 C25 C30 F30 174.0(3) . . . . ? N3 C25 C30 C29 -171.2(3) . . . . ? C26 C25 C30 C29 -1.1(5) . . . . ? N4 C31 C32 F32 3.4(5) . . . . ? C36 C31 C32 F32 174.1(3) . . . . ? N4 C31 C32 C33 -173.9(3) . . . . ? C36 C31 C32 C33 -3.3(5) . . . . ? F32 C32 C33 F33 2.8(5) . . . . ? C31 C32 C33 F33 -179.9(3) . . . . ? F32 C32 C33 C34 -174.9(3) . . . . ? C31 C32 C33 C34 2.5(5) . . . . ? F33 C33 C34 F34 1.8(5) . . . . ? C32 C33 C34 F34 179.5(3) . . . . ? F33 C33 C34 C35 -177.7(3) . . . . ? C32 C33 C34 C35 0.0(5) . . . . ? F34 C34 C35 F35 -3.0(5) . . . . ? C33 C34 C35 F35 176.5(3) . . . . ? F34 C34 C35 C36 179.2(3) . . . . ? C33 C34 C35 C36 -1.3(5) . . . . ? F35 C35 C36 F36 1.3(4) . . . . ? C34 C35 C36 F36 179.2(3) . . . . ? F35 C35 C36 C31 -177.5(3) . . . . ? C34 C35 C36 C31 0.3(5) . . . . ? C32 C31 C36 F36 -176.9(3) . . . . ? N4 C31 C36 F36 -5.6(4) . . . . ? C32 C31 C36 C35 1.9(4) . . . . ? N4 C31 C36 C35 173.3(3) . . . . ? C2 C1 N1 C7 -13.5(5) . . . . ? C6 C1 N1 C7 169.9(3) . . . . ? C2 C1 N1 Cu1 -179.7(3) . . . . ? C6 C1 N1 Cu1 3.7(4) . . . . ? C12 C7 N1 C1 -46.7(5) . . . . ? C8 C7 N1 C1 140.6(3) . . . . ? C12 C7 N1 Cu1 118.0(3) . . . . ? C8 C7 N1 Cu1 -54.7(4) . . . . ? C5 C6 N2 C13 -14.2(5) . . . . ? C1 C6 N2 C13 170.0(3) . . . . ? C5 C6 N2 Cu1 176.8(3) . . . . ? C1 C6 N2 Cu1 1.0(4) . . . . ? C18 C13 N2 C6 135.8(3) . . . . ? C14 C13 N2 C6 -50.7(4) . . . . ? C18 C13 N2 Cu1 -56.6(4) . . . . ? C14 C13 N2 Cu1 117.0(3) . . . . ? C20 C19 N3 C25 -12.2(5) . . . . ? C24 C19 N3 C25 171.3(3) . . . . ? C20 C19 N3 Cu1 -175.6(3) . . . . ? C24 C19 N3 Cu1 7.8(3) . . . . ? C30 C25 N3 C19 -49.0(5) . . . . ? C26 C25 N3 C19 141.2(3) . . . . ? C30 C25 N3 Cu1 113.2(3) . . . . ? C26 C25 N3 Cu1 -56.5(4) . . . . ? C23 C24 N4 C31 -13.7(5) . . . . ? C19 C24 N4 C31 171.9(3) . . . . ? C23 C24 N4 Cu1 179.1(3) . . . . ? C19 C24 N4 Cu1 4.7(3) . . . . ? C32 C31 N4 C24 -50.4(4) . . . . ? C36 C31 N4 C24 139.3(3) . . . . ? C32 C31 N4 Cu1 115.6(3) . . . . ? C36 C31 N4 Cu1 -54.7(4) . . . . ? C19 N3 Cu1 N4 -4.2(2) . . . . ? C25 N3 Cu1 N4 -167.9(2) . . . . ? C19 N3 Cu1 N1 -116.9(2) . . . . ? C25 N3 Cu1 N1 79.4(3) . . . . ? C19 N3 Cu1 N2 138.2(2) . . . . ? C25 N3 Cu1 N2 -25.5(3) . . . . ? C24 N4 Cu1 N3 -0.4(2) . . . . ? C31 N4 Cu1 N3 -167.4(2) . . . . ? C24 N4 Cu1 N1 146.5(2) . . . . ? C31 N4 Cu1 N1 -20.5(3) . . . . ? C24 N4 Cu1 N2 -110.7(2) . . . . ? C31 N4 Cu1 N2 82.3(3) . . . . ? C1 N1 Cu1 N3 -114.8(3) . . . . ? C7 N1 Cu1 N3 79.4(3) . . . . ? C1 N1 Cu1 N4 140.2(2) . . . . ? C7 N1 Cu1 N4 -25.6(3) . . . . ? C1 N1 Cu1 N2 -2.5(2) . . . . ? C7 N1 Cu1 N2 -168.3(3) . . . . ? C6 N2 Cu1 N3 147.7(2) . . . . ? C13 N2 Cu1 N3 -20.7(3) . . . . ? C6 N2 Cu1 N4 -110.7(3) . . . . ? C13 N2 Cu1 N4 81.0(3) . . . . ? C6 N2 Cu1 N1 0.7(2) . . . . ? C13 N2 Cu1 N1 -167.6(3) . . . . ? C704 O700 C701 C702 46(3) . . . . ? O700 C701 C702 C703 -33(2) . . . . ? C701 C702 C703 C704 11(2) . . . . ? C701 O700 C704 C703 -39(3) . . . . ? C702 C703 C704 O700 15(3) . . . . ? C804 O800 C801 C802 -44(3) . . . . ? O800 C801 C802 C803 37(3) . . . . ? C801 C802 C803 C804 -16(3) . . . . ? C801 O800 C804 C803 33(3) . . . . ? C802 C803 C804 O800 -10(3) . . . . ? C904 O900 C901 C902 49(4) . . . . ? O900 C901 C902 C903 -24(4) . . . . ? C901 C902 C903 C904 -7(3) . . . . ? C901 O900 C904 C903 -54(3) . . . . ? C902 C903 C904 O900 34(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.94 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.360 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.055 #===END