Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Michael Hannon' _publ_contact_author_address ; School of Chemistry University of Birmingham Edgbaston Birmingham B15 2TT UNITED KINGDOM ; _publ_contact_author_email M.J.HANNON@BHAM.AC.UK _publ_section_title ; Aggregation of imine based metallo-supramolecular architectures through pi-pi interactions. ; loop_ _publ_author_name 'M. J. Hannon' 'Guy Clarkson' 'Benson M. Kariuki' 'Mirela Pascu' # Attachment 'mp4c_final.cif' data_mp4c _database_code_depnum_ccdc_archive 'CCDC 292897' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C107 H84 F24 N16 Ni2 P4' _chemical_formula_weight 2291.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 36.7531(15) _cell_length_b 37.8287(16) _cell_length_c 14.9350(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 20764.5(16) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5507 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 49.99 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9360 _exptl_absorpt_coefficient_mu 1.905 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4879 _exptl_absorpt_correction_T_max 0.9277 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 6000 CCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78865 _diffrn_reflns_av_R_equivalents 0.1847 _diffrn_reflns_av_sigmaI/netI 0.1238 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 49.99 _reflns_number_total 10392 _reflns_number_gt 5507 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINTPLUS _computing_data_reduction SAINTPLUS _computing_structure_solution SHELXTL _computing_structure_refinement SHELXTL _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0632P)^2^+102.3072P] 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 10392 _refine_ls_number_parameters 866 _refine_ls_number_restraints 441 _refine_ls_R_factor_all 0.1626 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.1962 _refine_ls_wR_factor_gt 0.1519 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.006 _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 0.8374(3) 0.5831(3) 0.8213(8) 0.065(3) Uiso 1 1 d U . . H1 H 0.8252 0.5643 0.8507 0.078 Uiso 1 1 calc R . . C2 C 0.8383(3) 0.5841(3) 0.7270(9) 0.080(4) Uiso 1 1 d U . . H2 H 0.8279 0.5654 0.6932 0.096 Uiso 1 1 calc R . . C3 C 0.8545(3) 0.6126(3) 0.6837(7) 0.057(3) Uiso 1 1 d U . . C4 C 0.8560(3) 0.6156(3) 0.5883(8) 0.069(3) Uiso 1 1 d U . . H4 H 0.8458 0.5977 0.5514 0.083 Uiso 1 1 calc R . . C5 C 0.8719(3) 0.6442(3) 0.5509(8) 0.061(3) Uiso 1 1 d U . . H5 H 0.8731 0.6460 0.4876 0.073 Uiso 1 1 calc R . . C6 C 0.8864(3) 0.6707(3) 0.6025(7) 0.059(3) Uiso 1 1 d U . . H6 H 0.8968 0.6907 0.5738 0.071 Uiso 1 1 calc R . . C7 C 0.8863(2) 0.6691(3) 0.6942(7) 0.048(3) Uiso 1 1 d U . . H7 H 0.8967 0.6878 0.7282 0.058 Uiso 1 1 calc R . . C8 C 0.8708(2) 0.6403(3) 0.7372(7) 0.041(3) Uiso 1 1 d U . . C9 C 0.8699(2) 0.6352(3) 0.8315(6) 0.036(3) Uiso 1 1 d U . . C10 C 0.8884(2) 0.6589(2) 0.8952(7) 0.033(2) Uiso 1 1 d U . . H10 H 0.8988 0.6805 0.8757 0.040 Uiso 1 1 calc R . . C11 C 0.9079(2) 0.6725(2) 1.0398(6) 0.037(3) Uiso 1 1 d U . . C12 C 0.9360(2) 0.6602(3) 1.0904(6) 0.044(3) Uiso 1 1 d U . . H12 H 0.9446 0.6367 1.0819 0.053 Uiso 1 1 calc R . . C13 C 0.9521(2) 0.6819(2) 1.1543(6) 0.040(3) Uiso 1 1 d U . . H13 H 0.9718 0.6730 1.1886 0.048 Uiso 1 1 calc R . . C14 C 0.9402(2) 0.7157(2) 1.1692(6) 0.033(2) Uiso 1 1 d U . . C15 C 0.9116(3) 0.7277(3) 1.1181(7) 0.058(3) Uiso 1 1 d U . . H15 H 0.9027 0.7510 1.1271 0.069 Uiso 1 1 calc R . . C16 C 0.8955(3) 0.7062(3) 1.0533(7) 0.060(3) Uiso 1 1 d U . . H16 H 0.8759 0.7150 1.0184 0.072 Uiso 1 1 calc R . . C17 C 0.9552(2) 0.7400(2) 1.2405(6) 0.032(2) Uiso 1 1 d U . . H17A H 0.9633 0.7622 1.2115 0.038 Uiso 1 1 calc R . . H17B H 0.9353 0.7461 1.2823 0.038 Uiso 1 1 calc R . . C18 C 0.9862(2) 0.7252(2) 1.2932(6) 0.033(2) Uiso 1 1 d U . . C19 C 0.9807(2) 0.7057(2) 1.3724(6) 0.039(3) Uiso 1 1 d U . . H19 H 0.9567 0.7028 1.3950 0.047 Uiso 1 1 calc R . . C20 C 1.0093(2) 0.6907(2) 1.4176(7) 0.042(3) Uiso 1 1 d U . . H20 H 1.0050 0.6773 1.4702 0.050 Uiso 1 1 calc R . . C21 C 1.0444(2) 0.6953(2) 1.3867(6) 0.033(2) Uiso 1 1 d U . . C22 C 1.0508(2) 0.7149(2) 1.3110(6) 0.034(2) Uiso 1 1 d U . . H22 H 1.0750 0.7186 1.2908 0.041 Uiso 1 1 calc R . . C23 C 1.0217(2) 0.7293(2) 1.2639(6) 0.034(2) Uiso 1 1 d U . . H23 H 1.0263 0.7423 1.2107 0.041 Uiso 1 1 calc R . . C24 C 1.0779(2) 0.6834(2) 1.5161(7) 0.033(2) Uiso 1 1 d U . . H24 H 1.0611 0.6981 1.5470 0.039 Uiso 1 1 calc R . . C25 C 1.1070(2) 0.6656(2) 1.5653(6) 0.032(2) Uiso 1 1 d U . . C26 C 1.1131(2) 0.6699(2) 1.6579(6) 0.039(3) Uiso 1 1 d U . . C27 C 1.0945(2) 0.6942(3) 1.7116(7) 0.046(3) Uiso 1 1 d U . . H27 H 1.0768 0.7093 1.6853 0.055 Uiso 1 1 calc R . . C28 C 1.1014(3) 0.6967(3) 1.8012(7) 0.058(3) Uiso 1 1 d U . . H28 H 1.0886 0.7132 1.8370 0.070 Uiso 1 1 calc R . . C29 C 1.1275(3) 0.6747(3) 1.8398(8) 0.061(3) Uiso 1 1 d U . . H29 H 1.1319 0.6764 1.9024 0.073 Uiso 1 1 calc R . . C30 C 1.1465(3) 0.6514(3) 1.7918(7) 0.062(3) Uiso 1 1 d U . . H30 H 1.1641 0.6369 1.8204 0.074 Uiso 1 1 calc R . . C31 C 1.1406(2) 0.6481(3) 1.6977(7) 0.047(3) Uiso 1 1 d U . . C32 C 1.1601(3) 0.6258(3) 1.6430(7) 0.054(3) Uiso 1 1 d U . . H32 H 1.1784 0.6112 1.6683 0.064 Uiso 1 1 calc R . . C33 C 1.1535(3) 0.6244(3) 1.5515(7) 0.051(3) Uiso 1 1 d U . . H33 H 1.1678 0.6091 1.5151 0.062 Uiso 1 1 calc R . . C34 C 0.7902(3) 0.6564(3) 0.9528(7) 0.051(3) Uiso 1 1 d U . . H34 H 0.7957 0.6498 0.8929 0.061 Uiso 1 1 calc R . . C35 C 0.7601(3) 0.6764(3) 0.9689(7) 0.056(3) Uiso 1 1 d U . . H35 H 0.7448 0.6829 0.9203 0.068 Uiso 1 1 calc R . . C36 C 0.7511(3) 0.6876(3) 1.0553(7) 0.049(3) Uiso 1 1 d U . . C37 C 0.7198(3) 0.7075(3) 1.0761(8) 0.067(3) Uiso 1 1 d U . . H37 H 0.7037 0.7143 1.0293 0.081 Uiso 1 1 calc R . . C38 C 0.7122(3) 0.7171(3) 1.1605(8) 0.062(3) Uiso 1 1 d U . . H38 H 0.6912 0.7308 1.1730 0.075 Uiso 1 1 calc R . . C39 C 0.7355(3) 0.7067(3) 1.2306(8) 0.063(3) Uiso 1 1 d U . . H39 H 0.7301 0.7136 1.2902 0.075 Uiso 1 1 calc R . . C40 C 0.7657(3) 0.6868(3) 1.2145(7) 0.054(3) Uiso 1 1 d U . . H40 H 0.7806 0.6795 1.2630 0.064 Uiso 1 1 calc R . . C41 C 0.7750(2) 0.6768(2) 1.1255(7) 0.042(3) Uiso 1 1 d U . . C42 C 0.8047(2) 0.6556(2) 1.1038(7) 0.038(3) Uiso 1 1 d U . . C43 C 0.8306(2) 0.6419(2) 1.1708(7) 0.040(3) Uiso 1 1 d U . . H43 H 0.8298 0.6504 1.2306 0.048 Uiso 1 1 calc R . . C44 C 0.8772(2) 0.6053(2) 1.2162(6) 0.028(2) Uiso 1 1 d U . . C45 C 0.8804(2) 0.5690(2) 1.2289(6) 0.041(3) Uiso 1 1 d U . . H45 H 0.8673 0.5533 1.1909 0.049 Uiso 1 1 calc R . . C46 C 0.9021(2) 0.5553(3) 1.2959(6) 0.040(3) Uiso 1 1 d U . . H46 H 0.9033 0.5305 1.3045 0.048 Uiso 1 1 calc R . . C47 C 0.9222(2) 0.5773(2) 1.3502(6) 0.034(2) Uiso 1 1 d U . . C48 C 0.9192(2) 0.6130(2) 1.3387(6) 0.040(3) Uiso 1 1 d U . . H48 H 0.9327 0.6285 1.3763 0.048 Uiso 1 1 calc R . . C49 C 0.8968(2) 0.6272(3) 1.2730(6) 0.039(3) Uiso 1 1 d U . . H49 H 0.8948 0.6521 1.2670 0.047 Uiso 1 1 calc R . . C50 C 0.9471(2) 0.5620(3) 1.4222(6) 0.046(3) Uiso 1 1 d U . . H50A H 0.9395 0.5713 1.4812 0.055 Uiso 1 1 calc R . . H50B H 0.9440 0.5360 1.4236 0.055 Uiso 1 1 calc R . . C51 C 0.9867(2) 0.5703(2) 1.4079(6) 0.036(3) Uiso 1 1 d U . . C52 C 1.0062(2) 0.5901(2) 1.4684(7) 0.044(3) Uiso 1 1 d U . . H52 H 0.9950 0.5977 1.5223 0.052 Uiso 1 1 calc R . . C53 C 1.0421(2) 0.5990(2) 1.4518(6) 0.042(3) Uiso 1 1 d U . . H53 H 1.0551 0.6130 1.4938 0.050 Uiso 1 1 calc R . . C54 C 1.0594(2) 0.5875(2) 1.3744(6) 0.035(2) Uiso 1 1 d U . . C55 C 1.0404(2) 0.5668(2) 1.3132(7) 0.042(3) Uiso 1 1 d U . . H55 H 1.0520 0.5584 1.2605 0.050 Uiso 1 1 calc R . . C56 C 1.0042(2) 0.5587(2) 1.3304(6) 0.041(3) Uiso 1 1 d U . . H56 H 0.9910 0.5448 1.2884 0.049 Uiso 1 1 calc R . . C57 C 1.1182(2) 0.5771(3) 1.3219(6) 0.040(3) Uiso 1 1 d U . . H57 H 1.1104 0.5540 1.3061 0.048 Uiso 1 1 calc R . . C58 C 1.1557(2) 0.5878(3) 1.3044(6) 0.034(2) Uiso 1 1 d U . . C59 C 1.1819(2) 0.5668(2) 1.2612(6) 0.041(3) Uiso 1 1 d U . . C60 C 1.1739(3) 0.5329(3) 1.2269(7) 0.056(3) Uiso 1 1 d U . . H60 H 1.1501 0.5234 1.2326 0.067 Uiso 1 1 calc R . . C61 C 1.2010(3) 0.5137(3) 1.1850(7) 0.067(3) Uiso 1 1 d U . . H61 H 1.1955 0.4908 1.1626 0.080 Uiso 1 1 calc R . . C62 C 1.2361(3) 0.5271(3) 1.1748(8) 0.068(3) Uiso 1 1 d U . . H62 H 1.2543 0.5135 1.1457 0.081 Uiso 1 1 calc R . . C63 C 1.2440(3) 0.5594(3) 1.2065(7) 0.054(3) Uiso 1 1 d U . . H63 H 1.2678 0.5686 1.1988 0.065 Uiso 1 1 calc R . . C64 C 1.2177(2) 0.5801(3) 1.2509(7) 0.042(3) Uiso 1 1 d U . . C65 C 1.2247(3) 0.6136(2) 1.2868(6) 0.044(3) Uiso 1 1 d U . . H65 H 1.2485 0.6234 1.2825 0.053 Uiso 1 1 calc R . . C66 C 1.1981(2) 0.6322(3) 1.3275(6) 0.045(3) Uiso 1 1 d U . . H66 H 1.2037 0.6548 1.3515 0.054 Uiso 1 1 calc R . . C67 C 0.7825(3) 0.5676(3) 1.0384(6) 0.047(3) Uiso 1 1 d U . . H67 H 0.7712 0.5901 1.0360 0.056 Uiso 1 1 calc R . . C68 C 0.7617(3) 0.5386(3) 1.0528(6) 0.047(3) Uiso 1 1 d U . . H68 H 0.7363 0.5411 1.0626 0.056 Uiso 1 1 calc R . . C69 C 0.7772(2) 0.5053(3) 1.0535(6) 0.042(3) Uiso 1 1 d U . . C70 C 0.7564(3) 0.4735(3) 1.0644(7) 0.054(3) Uiso 1 1 d U . . H70 H 0.7307 0.4747 1.0711 0.064 Uiso 1 1 calc R . . C71 C 0.7732(3) 0.4420(3) 1.0652(7) 0.066(3) Uiso 1 1 d U . . H71 H 0.7590 0.4211 1.0696 0.079 Uiso 1 1 calc R . . C72 C 0.8115(3) 0.4391(3) 1.0596(8) 0.077(4) Uiso 1 1 d U . . H72 H 0.8229 0.4166 1.0622 0.092 Uiso 1 1 calc R . . C73 C 0.8323(3) 0.4695(3) 1.0502(8) 0.071(4) Uiso 1 1 d U . . H73 H 0.8580 0.4680 1.0483 0.086 Uiso 1 1 calc R . . C74 C 0.8152(2) 0.5024(3) 1.0434(6) 0.043(3) Uiso 1 1 d U . . C75 C 0.8349(2) 0.5344(3) 1.0297(6) 0.038(3) Uiso 1 1 d U . . C76 C 0.8741(2) 0.5354(3) 1.0170(6) 0.038(3) Uiso 1 1 d U . . H76 H 0.8875 0.5140 1.0143 0.046 Uiso 1 1 calc R . . C77 C 0.9293(2) 0.5641(2) 1.0024(6) 0.032(2) Uiso 1 1 d U . . C78 C 0.9471(2) 0.5848(2) 0.9387(6) 0.040(3) Uiso 1 1 d U . . H78 H 0.9337 0.5993 0.8984 0.048 Uiso 1 1 calc R . . C79 C 0.9846(2) 0.5836(2) 0.9354(7) 0.045(3) Uiso 1 1 d U . . H79 H 0.9969 0.5972 0.8912 0.053 Uiso 1 1 calc R . . C80 C 1.0047(2) 0.5638(2) 0.9933(6) 0.038(3) Uiso 1 1 d U . . C81 C 0.9871(2) 0.5432(2) 1.0576(7) 0.044(3) Uiso 1 1 d U . . H81 H 1.0008 0.5292 1.0984 0.053 Uiso 1 1 calc R . . C82 C 0.9492(2) 0.5433(3) 1.0611(7) 0.046(3) Uiso 1 1 d U . . H82 H 0.9370 0.5291 1.1039 0.055 Uiso 1 1 calc R . . C83 C 1.0458(2) 0.5655(2) 0.9915(6) 0.042(3) Uiso 1 1 d U . . H83A H 1.0538 0.5705 0.9295 0.051 Uiso 1 1 calc R . . H83B H 1.0556 0.5420 1.0085 0.051 Uiso 1 1 calc R . . C84 C 1.0620(2) 0.5932(2) 1.0534(6) 0.039(3) Uiso 1 1 d U . . C85 C 1.0416(3) 0.6116(2) 1.1171(6) 0.044(3) Uiso 1 1 d U . . H85 H 1.0159 0.6086 1.1192 0.052 Uiso 1 1 calc R . . C86 C 1.0584(2) 0.6344(2) 1.1770(6) 0.036(3) Uiso 1 1 d U . . H86 H 1.0443 0.6460 1.2213 0.044 Uiso 1 1 calc R . . C87 C 1.0952(2) 0.6402(2) 1.1729(6) 0.033(2) Uiso 1 1 d U . . C88 C 1.1156(3) 0.6230(3) 1.1097(7) 0.051(3) Uiso 1 1 d U . . H88 H 1.1411 0.6271 1.1064 0.061 Uiso 1 1 calc R . . C89 C 1.0989(3) 0.5995(3) 1.0498(7) 0.056(3) Uiso 1 1 d U . . H89 H 1.1132 0.5877 1.0061 0.067 Uiso 1 1 calc R . . C90 C 1.1336(2) 0.6869(2) 1.2136(7) 0.033(2) Uiso 1 1 d U . . H90 H 1.1363 0.6918 1.1516 0.040 Uiso 1 1 calc R . . C91 C 1.1531(2) 0.7079(2) 1.2799(7) 0.030(2) Uiso 1 1 d U . . C92 C 1.1751(2) 0.7369(2) 1.2583(6) 0.034(2) Uiso 1 1 d U . . C93 C 1.1805(2) 0.7496(2) 1.1706(6) 0.040(3) Uiso 1 1 d U . . H93 H 1.1683 0.7387 1.1217 0.048 Uiso 1 1 calc R . . C94 C 1.2031(2) 0.7770(3) 1.1563(7) 0.052(3) Uiso 1 1 d U . . H94 H 1.2067 0.7851 1.0967 0.062 Uiso 1 1 calc R . . C95 C 1.2216(3) 0.7942(3) 1.2263(7) 0.051(3) Uiso 1 1 d U . . H95 H 1.2376 0.8133 1.2139 0.062 Uiso 1 1 calc R . . C96 C 1.2162(2) 0.7832(3) 1.3111(7) 0.047(3) Uiso 1 1 d U . . H96 H 1.2281 0.7951 1.3589 0.057 Uiso 1 1 calc R . . C97 C 1.1932(2) 0.7543(2) 1.3300(6) 0.040(3) Uiso 1 1 d U . . C98 C 1.1866(2) 0.7427(3) 1.4170(7) 0.048(3) Uiso 1 1 d U . . H98 H 1.1975 0.7545 1.4664 0.057 Uiso 1 1 calc R . . C99 C 1.1645(2) 0.7142(3) 1.4311(7) 0.044(3) Uiso 1 1 d U . . H99 H 1.1606 0.7064 1.4908 0.053 Uiso 1 1 calc R . . N1 N 0.8535(2) 0.6084(2) 0.8702(5) 0.043(2) Uani 1 1 d U . . N2 N 0.89015(18) 0.64970(19) 0.9767(5) 0.035(2) Uani 1 1 d U . . N3 N 1.07511(17) 0.67913(18) 1.4306(5) 0.032(2) Uani 1 1 d U . . N4 N 1.12710(18) 0.64439(19) 1.5133(5) 0.037(2) Uani 1 1 d U . . N5 N 0.81265(19) 0.6455(2) 1.0204(5) 0.040(2) Uani 1 1 d U . . N6 N 0.85388(18) 0.61870(19) 1.1486(5) 0.034(2) Uani 1 1 d U . . N7 N 1.09601(18) 0.59855(19) 1.3583(5) 0.033(2) Uani 1 1 d U . . N8 N 1.16389(17) 0.61979(19) 1.3354(5) 0.035(2) Uani 1 1 d U . . N9 N 0.81888(19) 0.5655(2) 1.0272(5) 0.039(2) Uani 1 1 d U . . N10 N 0.89072(18) 0.56482(19) 1.0096(5) 0.035(2) Uani 1 1 d U . . N11 N 1.11278(18) 0.66169(19) 1.2397(5) 0.034(2) Uani 1 1 d U . . N12 N 1.14773(17) 0.69653(19) 1.3635(5) 0.035(2) Uani 1 1 d U . . Ni1 Ni 0.85451(4) 0.60837(4) 1.00933(10) 0.0392(5) Uani 1 1 d . . . Ni2 Ni 1.11846(4) 0.64956(4) 1.37671(10) 0.0376(5) Uani 1 1 d . . . F1 F 0.68096(13) 0.32685(16) 0.4927(4) 0.0628(17) Uani 1 1 d U . . F2 F 0.73746(14) 0.30397(15) 0.4799(4) 0.0603(17) Uani 1 1 d U . . F3 F 0.70923(15) 0.32944(16) 0.3598(4) 0.0685(18) Uani 1 1 d U . . F4 F 0.70120(14) 0.37931(16) 0.4389(4) 0.0661(18) Uani 1 1 d U . . F5 F 0.72799(14) 0.35395(15) 0.5588(4) 0.0626(17) Uani 1 1 d U . . F6 F 0.75750(14) 0.35605(16) 0.4263(4) 0.0683(18) Uani 1 1 d U . . P1 P 0.71920(7) 0.34181(8) 0.45899(19) 0.0491(8) Uani 1 1 d U . . F7 F 0.83689(17) 0.45978(16) 0.5270(5) 0.086(2) Uani 1 1 d U . . F8 F 0.8287(2) 0.5137(2) 0.5826(5) 0.131(3) Uani 1 1 d U . . F9 F 0.86835(17) 0.53687(17) 0.4871(5) 0.086(2) Uani 1 1 d U . . F10 F 0.8744(3) 0.4842(2) 0.4274(7) 0.177(5) Uani 1 1 d U . . F11 F 0.8197(2) 0.5058(2) 0.4443(6) 0.131(3) Uani 1 1 d U . . F12 F 0.8833(2) 0.4925(2) 0.5751(7) 0.175(5) Uani 1 1 d U . . P2 P 0.85294(8) 0.49789(9) 0.5059(2) 0.0582(9) Uani 1 1 d U . . F13 F 0.98671(18) 0.60878(17) 0.7039(5) 0.095(2) Uani 1 1 d U . . F14 F 0.96604(15) 0.65523(19) 0.7806(4) 0.086(2) Uani 1 1 d U . . F15 F 1.00902(18) 0.68954(17) 0.7157(6) 0.113(3) Uani 1 1 d U . . F16 F 1.02874(14) 0.64295(15) 0.6365(4) 0.0622(17) Uani 1 1 d U . . F17 F 0.97030(17) 0.6579(2) 0.6308(5) 0.119(3) Uani 1 1 d U . . F18 F 1.02539(15) 0.64035(18) 0.7867(4) 0.076(2) Uani 1 1 d U . . P3 P 0.99704(7) 0.64922(9) 0.7088(2) 0.0557(9) Uani 1 1 d U . . F19 F 0.83074(13) 0.68529(13) 0.3796(3) 0.0494(15) Uani 1 1 d U . . F20 F 0.84678(15) 0.71656(15) 0.2562(4) 0.0630(17) Uani 1 1 d U . . F21 F 0.86709(15) 0.76109(14) 0.3425(4) 0.0642(17) Uani 1 1 d U . . F22 F 0.85153(14) 0.73000(14) 0.4669(3) 0.0527(16) Uani 1 1 d U . . F23 F 0.80958(14) 0.74060(14) 0.3600(4) 0.0637(17) Uani 1 1 d U . . F24 F 0.88830(13) 0.70550(15) 0.3641(4) 0.0648(18) Uani 1 1 d U . . P4 P 0.84909(7) 0.72348(8) 0.36121(19) 0.0460(8) Uani 1 1 d U . . C100 C 0.7216(4) 0.5872(4) 0.8178(11) 0.092(5) Uiso 1 1 d U . . C101 C 0.6952(3) 0.5919(3) 0.8901(9) 0.095(4) Uiso 1 1 d U . . H10A H 0.7076 0.6011 0.9433 0.143 Uiso 1 1 calc R . . H10B H 0.6840 0.5690 0.9044 0.143 Uiso 1 1 calc R . . H10C H 0.6763 0.6086 0.8711 0.143 Uiso 1 1 calc R . . N13 N 0.7407(4) 0.5882(5) 0.7654(10) 0.184(7) Uani 1 1 d U . . C102 C 0.9238(3) 0.5179(4) 0.7759(10) 0.074(4) Uiso 1 1 d U . . C103 C 0.9378(4) 0.5391(4) 0.7018(10) 0.110(5) Uiso 1 1 d U . . H10D H 0.9207 0.5583 0.6886 0.165 Uiso 1 1 calc R . . H10E H 0.9406 0.5241 0.6487 0.165 Uiso 1 1 calc R . . H10F H 0.9614 0.5490 0.7184 0.165 Uiso 1 1 calc R . . N14 N 0.9124(3) 0.5023(3) 0.8325(7) 0.089(3) Uani 1 1 d U . . C104 C 0.5547(3) 0.2839(4) 0.4807(9) 0.080(4) Uiso 1 1 d DU . . C105 C 0.5239(4) 0.3007(4) 0.5297(9) 0.115(5) Uiso 1 1 d DU . . H10G H 0.5100 0.2825 0.5615 0.172 Uiso 1 1 calc R . . H10H H 0.5080 0.3129 0.4870 0.172 Uiso 1 1 calc R . . H10I H 0.5335 0.3179 0.5729 0.172 Uiso 1 1 calc R . . N15 N 0.5787(3) 0.2716(3) 0.4506(7) 0.092(3) Uani 1 1 d DU . . C106 C 0.5841(5) 0.4555(5) 0.7420(13) 0.064(6) Uiso 0.693(13) 1 d PDU . . C107 C 0.5701(6) 0.4352(5) 0.8229(13) 0.081(7) Uiso 0.693(13) 1 d PDU . . H10J H 0.5905 0.4292 0.8624 0.122 Uiso 0.693(13) 1 calc PR . . H10K H 0.5582 0.4134 0.8027 0.122 Uiso 0.693(13) 1 calc PR . . H10L H 0.5525 0.4498 0.8555 0.122 Uiso 0.693(13) 1 calc PR . . N16 N 0.5939(4) 0.4713(4) 0.6886(9) 0.078(6) Uani 0.693(13) 1 d PDU . . C108 C 0.5598(8) 0.4583(9) 0.761(2) 0.068(13) Uiso 0.307(13) 1 d PDU . . C109 C 0.5808(11) 0.4284(10) 0.800(3) 0.071(15) Uiso 0.307(13) 1 d PDU . . H10M H 0.5711 0.4226 0.8590 0.107 Uiso 0.307(13) 1 calc PR . . H10N H 0.6065 0.4351 0.8051 0.107 Uiso 0.307(13) 1 calc PR . . H10O H 0.5788 0.4077 0.7605 0.107 Uiso 0.307(13) 1 calc PR . . N17 N 0.5411(8) 0.4789(6) 0.7372(19) 0.067(11) Uani 0.307(13) 1 d PDU . . 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 N1 0.058(5) 0.047(5) 0.025(5) -0.015(4) -0.014(4) -0.023(5) N2 0.047(5) 0.041(5) 0.017(5) 0.005(4) -0.004(4) 0.003(4) N3 0.029(4) 0.038(5) 0.030(6) 0.003(4) 0.000(4) -0.002(4) N4 0.029(4) 0.043(5) 0.039(5) 0.014(4) -0.017(4) -0.003(4) N5 0.041(5) 0.045(5) 0.033(6) 0.005(4) -0.004(4) 0.001(4) N6 0.033(4) 0.038(5) 0.031(5) 0.007(4) -0.008(4) -0.002(4) N7 0.032(4) 0.037(5) 0.031(5) 0.000(4) -0.008(4) -0.008(4) N8 0.023(4) 0.040(5) 0.041(5) 0.000(4) -0.002(4) -0.004(4) N9 0.036(5) 0.049(6) 0.033(5) 0.002(4) -0.002(4) -0.006(4) N10 0.037(4) 0.040(5) 0.028(5) 0.000(4) 0.003(4) -0.004(4) N11 0.029(4) 0.043(5) 0.030(5) -0.009(4) -0.004(4) -0.002(4) N12 0.027(4) 0.038(5) 0.038(6) -0.004(4) -0.009(4) -0.004(4) Ni1 0.0456(9) 0.0455(11) 0.0265(11) -0.0006(9) -0.0043(8) -0.0057(8) Ni2 0.0341(9) 0.0459(11) 0.0328(11) 0.0017(9) -0.0050(8) -0.0008(8) F1 0.047(3) 0.099(5) 0.042(4) 0.002(4) 0.014(3) -0.014(3) F2 0.069(4) 0.062(4) 0.049(4) 0.005(3) 0.010(3) 0.009(3) F3 0.072(4) 0.100(5) 0.033(4) 0.003(4) -0.004(3) -0.021(4) F4 0.059(4) 0.075(5) 0.064(4) 0.014(4) -0.015(3) 0.006(3) F5 0.070(4) 0.069(4) 0.049(4) -0.002(3) -0.013(3) 0.000(3) F6 0.047(4) 0.090(5) 0.068(4) 0.018(4) 0.003(3) -0.012(3) P1 0.0418(17) 0.073(2) 0.033(2) 0.0031(17) 0.0015(14) -0.0062(17) F7 0.095(5) 0.057(5) 0.105(6) 0.018(4) 0.004(4) 0.000(4) F8 0.155(7) 0.130(7) 0.109(7) -0.038(6) 0.071(6) -0.047(6) F9 0.093(5) 0.075(5) 0.092(5) 0.014(4) 0.017(4) -0.016(4) F10 0.233(11) 0.104(7) 0.192(10) -0.039(7) 0.160(9) -0.001(7) F11 0.127(7) 0.111(6) 0.156(8) 0.046(6) -0.064(6) -0.017(5) F12 0.133(7) 0.159(8) 0.233(11) 0.113(8) -0.117(8) -0.053(6) P2 0.0545(18) 0.072(3) 0.048(2) 0.0078(19) 0.0113(17) 0.0089(19) F13 0.112(5) 0.075(5) 0.098(6) -0.012(4) 0.025(4) -0.050(4) F14 0.054(4) 0.133(6) 0.071(5) -0.017(4) 0.017(3) 0.003(4) F15 0.096(5) 0.052(5) 0.191(9) -0.019(5) 0.027(5) 0.000(4) F16 0.063(4) 0.076(4) 0.047(4) 0.005(3) 0.007(3) -0.001(3) F17 0.059(4) 0.224(9) 0.074(5) 0.045(6) -0.006(4) 0.005(5) F18 0.061(4) 0.120(6) 0.048(4) 0.009(4) -0.004(3) -0.003(4) P3 0.0487(18) 0.070(3) 0.048(2) 0.0003(18) 0.0030(17) -0.0027(17) F19 0.053(3) 0.054(4) 0.041(4) 0.007(3) -0.004(3) -0.012(3) F20 0.089(4) 0.075(4) 0.024(4) -0.003(3) 0.007(3) -0.003(4) F21 0.085(4) 0.054(4) 0.054(4) 0.005(3) 0.007(3) -0.014(3) F22 0.060(3) 0.073(4) 0.025(4) -0.007(3) 0.001(3) -0.015(3) F23 0.056(4) 0.067(4) 0.068(4) -0.008(4) -0.011(3) 0.016(3) F24 0.040(3) 0.085(5) 0.069(5) -0.006(4) 0.005(3) 0.002(3) P4 0.0430(17) 0.057(2) 0.038(2) 0.0007(16) 0.0022(14) -0.0016(16) N13 0.125(12) 0.31(2) 0.115(13) -0.015(13) 0.029(10) 0.007(13) N14 0.120(9) 0.084(8) 0.061(8) -0.017(7) 0.006(7) -0.019(7) N15 0.122(9) 0.076(8) 0.079(8) 0.006(7) 0.014(7) 0.000(7) N16 0.140(14) 0.070(11) 0.025(10) -0.010(8) -0.041(9) -0.009(9) N17 0.12(3) 0.018(17) 0.07(2) -0.021(16) 0.001(19) -0.001(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.341(12) . ? C1 C2 1.409(15) . ? C2 C3 1.391(14) . ? C3 C4 1.431(14) . ? C3 C8 1.447(13) . ? C4 C5 1.350(13) . ? C5 C6 1.370(13) . ? C6 C7 1.371(13) . ? C7 C8 1.390(12) . ? C8 C9 1.422(12) . ? C9 N1 1.314(11) . ? C9 C10 1.472(12) . ? C10 N2 1.268(10) . ? C11 C12 1.362(12) . ? C11 C16 1.369(12) . ? C11 N2 1.434(11) . ? C12 C13 1.391(12) . ? C13 C14 1.371(11) . ? C14 C15 1.377(12) . ? C14 C17 1.510(11) . ? C15 C16 1.395(13) . ? C17 C18 1.496(11) . ? C18 C23 1.385(11) . ? C18 C19 1.409(12) . ? C19 C20 1.373(11) . ? C20 C21 1.380(11) . ? C21 C22 1.372(11) . ? C21 N3 1.442(10) . ? C22 C23 1.389(11) . ? C24 N3 1.291(10) . ? C24 C25 1.461(12) . ? C25 N4 1.339(11) . ? C25 C26 1.411(12) . ? C26 C27 1.399(12) . ? C26 C31 1.434(12) . ? C27 C28 1.366(13) . ? C28 C29 1.395(13) . ? C29 C30 1.334(13) . ? C30 C31 1.428(13) . ? C31 C32 1.375(12) . ? C32 C33 1.389(13) . ? C33 N4 1.358(11) . ? C34 C35 1.361(12) . ? C34 N5 1.368(11) . ? C35 C36 1.398(13) . ? C36 C37 1.409(13) . ? C36 C41 1.428(13) . ? C37 C38 1.342(14) . ? C38 C39 1.409(14) . ? C39 C40 1.361(12) . ? C40 C41 1.422(13) . ? C41 C42 1.395(12) . ? C42 N5 1.334(11) . ? C42 C43 1.473(12) . ? C43 N6 1.271(10) . ? C44 C49 1.387(11) . ? C44 C45 1.390(11) . ? C44 N6 1.420(10) . ? C45 C46 1.382(12) . ? C46 C47 1.375(11) . ? C47 C48 1.369(11) . ? C47 C50 1.525(12) . ? C48 C49 1.389(11) . ? C50 C51 1.505(12) . ? C51 C52 1.375(12) . ? C51 C56 1.396(12) . ? C52 C53 1.384(12) . ? C53 C54 1.389(12) . ? C54 C55 1.390(12) . ? C54 N7 1.429(10) . ? C55 C56 1.390(11) . ? C57 N7 1.274(10) . ? C57 C58 1.459(12) . ? C58 N8 1.329(10) . ? C58 C59 1.407(12) . ? C59 C60 1.411(12) . ? C59 C64 1.416(12) . ? C60 C61 1.381(13) . ? C61 C62 1.397(13) . ? C62 C63 1.343(13) . ? C63 C64 1.409(12) . ? C64 C65 1.401(12) . ? C65 C66 1.350(12) . ? C66 N8 1.346(10) . ? C67 N9 1.348(11) . ? C67 C68 1.354(12) . ? C68 C69 1.381(12) . ? C69 C74 1.411(12) . ? C69 C70 1.435(12) . ? C70 C71 1.342(13) . ? C71 C72 1.414(14) . ? C72 C73 1.389(14) . ? C73 C74 1.394(13) . ? C74 C75 1.425(12) . ? C75 N9 1.316(11) . ? C75 C76 1.454(12) . ? C76 N10 1.273(10) . ? C77 C82 1.388(12) . ? C77 C78 1.394(11) . ? C77 N10 1.421(10) . ? C78 C79 1.381(11) . ? C79 C80 1.363(12) . ? C80 C81 1.396(12) . ? C80 C83 1.510(12) . ? C81 C82 1.393(12) . ? C83 C84 1.521(12) . ? C84 C89 1.375(12) . ? C84 C85 1.398(12) . ? C85 C86 1.386(12) . ? C86 C87 1.371(11) . ? C87 C88 1.370(12) . ? C87 N11 1.441(11) . ? C88 C89 1.405(13) . ? C90 N11 1.283(10) . ? C90 C91 1.458(12) . ? C91 N12 1.336(11) . ? C91 C92 1.399(11) . ? C92 C93 1.409(12) . ? C92 C97 1.424(12) . ? C93 C94 1.347(12) . ? C94 C95 1.405(13) . ? C95 C96 1.348(12) . ? C96 C97 1.410(12) . ? C97 C98 1.393(12) . ? C98 C99 1.367(12) . ? C99 N12 1.358(11) . ? N1 Ni1 2.079(7) . ? N2 Ni1 2.097(7) . ? N3 Ni2 2.107(7) . ? N4 Ni2 2.073(7) . ? N5 Ni1 2.091(7) . ? N6 Ni1 2.116(7) . ? N7 Ni2 2.116(7) . ? N8 Ni2 2.106(7) . ? N9 Ni1 2.101(7) . ? N10 Ni1 2.118(7) . ? N11 Ni2 2.107(7) . ? N12 Ni2 2.086(7) . ? F1 P1 1.597(5) . ? F2 P1 1.612(6) . ? F3 P1 1.596(6) . ? F4 P1 1.594(6) . ? F5 P1 1.593(6) . ? F6 P1 1.584(6) . ? F7 P2 1.589(7) . ? F8 P2 1.569(8) . ? F9 P2 1.605(7) . ? F10 P2 1.507(8) . ? F11 P2 1.559(8) . ? F12 P2 1.535(8) . ? F13 P3 1.578(7) . ? F14 P3 1.581(6) . ? F15 P3 1.591(7) . ? F16 P3 1.607(6) . ? F17 P3 1.560(7) . ? F18 P3 1.597(6) . ? F19 P4 1.618(6) . ? F20 P4 1.593(6) . ? F21 P4 1.594(6) . ? F22 P4 1.601(6) . ? F23 P4 1.590(6) . ? F24 P4 1.594(6) . ? C100 N13 1.052(16) . ? C100 C101 1.464(17) . ? C102 N14 1.113(14) . ? C102 C103 1.459(17) . ? C104 N15 1.093(11) . ? C104 C105 1.490(14) . ? C106 N16 1.061(14) . ? C106 C107 1.521(17) . ? N16 C108 1.72(3) . ? C108 N17 1.094(12) . ? C108 C109 1.492(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 121.1(11) . . ? C3 C2 C1 119.6(12) . . ? C2 C3 C4 122.8(11) . . ? C2 C3 C8 118.8(11) . . ? C4 C3 C8 118.4(10) . . ? C5 C4 C3 119.5(12) . . ? C4 C5 C6 121.4(12) . . ? C5 C6 C7 122.0(11) . . ? C6 C7 C8 119.7(10) . . ? C7 C8 C9 124.9(9) . . ? C7 C8 C3 118.9(9) . . ? C9 C8 C3 116.1(9) . . ? N1 C9 C8 123.3(9) . . ? N1 C9 C10 113.4(9) . . ? C8 C9 C10 123.3(9) . . ? N2 C10 C9 118.6(9) . . ? C12 C11 C16 119.3(10) . . ? C12 C11 N2 120.2(8) . . ? C16 C11 N2 120.4(9) . . ? C11 C12 C13 120.0(9) . . ? C14 C13 C12 121.8(9) . . ? C13 C14 C15 117.4(9) . . ? C13 C14 C17 124.6(8) . . ? C15 C14 C17 118.0(8) . . ? C14 C15 C16 121.2(10) . . ? C11 C16 C15 120.2(10) . . ? C18 C17 C14 114.9(7) . . ? C23 C18 C19 117.4(8) . . ? C23 C18 C17 120.6(8) . . ? C19 C18 C17 121.9(8) . . ? C20 C19 C18 121.2(9) . . ? C19 C20 C21 120.0(9) . . ? C22 C21 C20 120.1(9) . . ? C22 C21 N3 118.1(8) . . ? C20 C21 N3 121.7(8) . . ? C21 C22 C23 119.9(8) . . ? C18 C23 C22 121.3(9) . . ? N3 C24 C25 119.8(9) . . ? N4 C25 C26 123.3(8) . . ? N4 C25 C24 112.9(8) . . ? C26 C25 C24 123.8(9) . . ? C27 C26 C25 124.1(9) . . ? C27 C26 C31 119.0(9) . . ? C25 C26 C31 116.9(9) . . ? C28 C27 C26 121.0(10) . . ? C27 C28 C29 119.5(11) . . ? C30 C29 C28 122.2(12) . . ? C29 C30 C31 120.4(11) . . ? C32 C31 C30 123.9(10) . . ? C32 C31 C26 118.2(10) . . ? C30 C31 C26 117.8(9) . . ? C31 C32 C33 121.2(10) . . ? N4 C33 C32 121.0(10) . . ? C35 C34 N5 121.8(10) . . ? C34 C35 C36 121.7(10) . . ? C35 C36 C37 124.0(10) . . ? C35 C36 C41 116.4(9) . . ? C37 C36 C41 119.6(10) . . ? C38 C37 C36 121.4(11) . . ? C37 C38 C39 119.7(11) . . ? C40 C39 C38 121.2(11) . . ? C39 C40 C41 120.5(10) . . ? C42 C41 C40 124.0(9) . . ? C42 C41 C36 118.4(9) . . ? C40 C41 C36 117.5(9) . . ? N5 C42 C41 123.5(9) . . ? N5 C42 C43 113.2(8) . . ? C41 C42 C43 123.3(10) . . ? N6 C43 C42 120.0(9) . . ? C49 C44 C45 117.7(9) . . ? C49 C44 N6 122.3(8) . . ? C45 C44 N6 120.0(8) . . ? C46 C45 C44 121.0(9) . . ? C47 C46 C45 120.8(9) . . ? C48 C47 C46 118.6(9) . . ? C48 C47 C50 120.8(8) . . ? C46 C47 C50 120.6(8) . . ? C47 C48 C49 121.2(9) . . ? C44 C49 C48 120.6(9) . . ? C51 C50 C47 113.6(8) . . ? C52 C51 C56 118.5(8) . . ? C52 C51 C50 121.8(9) . . ? C56 C51 C50 119.8(8) . . ? C51 C52 C53 120.8(9) . . ? C52 C53 C54 120.6(9) . . ? C53 C54 C55 119.5(8) . . ? C53 C54 N7 118.6(8) . . ? C55 C54 N7 121.8(8) . . ? C56 C55 C54 119.1(9) . . ? C55 C56 C51 121.5(9) . . ? N7 C57 C58 120.2(9) . . ? N8 C58 C59 121.3(8) . . ? N8 C58 C57 113.9(8) . . ? C59 C58 C57 124.8(9) . . ? C58 C59 C60 122.6(9) . . ? C58 C59 C64 118.9(9) . . ? C60 C59 C64 118.5(9) . . ? C61 C60 C59 119.5(10) . . ? C60 C61 C62 121.6(11) . . ? C63 C62 C61 119.4(11) . . ? C62 C63 C64 121.6(10) . . ? C65 C64 C63 123.7(9) . . ? C65 C64 C59 116.9(9) . . ? C63 C64 C59 119.4(9) . . ? C66 C65 C64 120.6(9) . . ? N8 C66 C65 122.4(9) . . ? N9 C67 C68 122.1(10) . . ? C67 C68 C69 120.5(9) . . ? C68 C69 C74 118.5(9) . . ? C68 C69 C70 123.2(9) . . ? C74 C69 C70 118.3(9) . . ? C71 C70 C69 120.1(10) . . ? C70 C71 C72 121.7(11) . . ? C73 C72 C71 119.2(12) . . ? C72 C73 C74 120.0(11) . . ? C73 C74 C69 120.4(10) . . ? C73 C74 C75 122.7(9) . . ? C69 C74 C75 116.8(9) . . ? N9 C75 C74 122.5(8) . . ? N9 C75 C76 114.6(9) . . ? C74 C75 C76 122.9(9) . . ? N10 C76 C75 120.6(9) . . ? C82 C77 C78 120.0(8) . . ? C82 C77 N10 119.3(8) . . ? C78 C77 N10 120.6(8) . . ? C79 C78 C77 118.3(9) . . ? C80 C79 C78 122.5(10) . . ? C79 C80 C81 119.5(9) . . ? C79 C80 C83 120.5(9) . . ? C81 C80 C83 119.9(8) . . ? C82 C81 C80 119.1(9) . . ? C77 C82 C81 120.5(9) . . ? C80 C83 C84 114.2(8) . . ? C89 C84 C85 118.1(9) . . ? C89 C84 C83 118.7(9) . . ? C85 C84 C83 123.1(8) . . ? C86 C85 C84 120.5(9) . . ? C87 C86 C85 120.7(9) . . ? C88 C87 C86 119.7(9) . . ? C88 C87 N11 119.9(8) . . ? C86 C87 N11 120.2(8) . . ? C87 C88 C89 119.9(9) . . ? C84 C89 C88 121.0(10) . . ? N11 C90 C91 119.4(9) . . ? N12 C91 C92 123.6(8) . . ? N12 C91 C90 112.7(8) . . ? C92 C91 C90 123.7(9) . . ? C91 C92 C93 124.2(9) . . ? C91 C92 C97 117.4(8) . . ? C93 C92 C97 118.4(8) . . ? C94 C93 C92 119.8(9) . . ? C93 C94 C95 122.4(10) . . ? C96 C95 C94 119.1(10) . . ? C95 C96 C97 120.9(10) . . ? C98 C97 C96 122.4(9) . . ? C98 C97 C92 118.3(9) . . ? C96 C97 C92 119.3(9) . . ? C99 C98 C97 119.8(10) . . ? N12 C99 C98 122.9(10) . . ? C9 N1 C1 120.9(9) . . ? C9 N1 Ni1 115.6(6) . . ? C1 N1 Ni1 123.5(7) . . ? C10 N2 C11 119.3(8) . . ? C10 N2 Ni1 113.3(6) . . ? C11 N2 Ni1 125.5(6) . . ? C24 N3 C21 117.3(7) . . ? C24 N3 Ni2 112.6(6) . . ? C21 N3 Ni2 130.0(6) . . ? C25 N4 C33 119.1(8) . . ? C25 N4 Ni2 115.4(6) . . ? C33 N4 Ni2 125.1(7) . . ? C42 N5 C34 118.2(8) . . ? C42 N5 Ni1 115.2(6) . . ? C34 N5 Ni1 126.1(7) . . ? C43 N6 C44 118.0(8) . . ? C43 N6 Ni1 113.1(6) . . ? C44 N6 Ni1 128.8(6) . . ? C57 N7 C54 119.2(8) . . ? C57 N7 Ni2 112.8(6) . . ? C54 N7 Ni2 127.8(6) . . ? C58 N8 C66 119.9(8) . . ? C58 N8 Ni2 114.1(5) . . ? C66 N8 Ni2 125.4(6) . . ? C75 N9 C67 119.4(8) . . ? C75 N9 Ni1 114.5(6) . . ? C67 N9 Ni1 126.1(7) . . ? C76 N10 C77 117.9(8) . . ? C76 N10 Ni1 112.2(6) . . ? C77 N10 Ni1 129.8(6) . . ? C90 N11 C87 118.4(8) . . ? C90 N11 Ni2 113.5(6) . . ? C87 N11 Ni2 126.4(6) . . ? C91 N12 C99 118.0(8) . . ? C91 N12 Ni2 116.1(6) . . ? C99 N12 Ni2 125.6(6) . . ? N1 Ni1 N5 93.7(3) . . ? N1 Ni1 N2 77.2(3) . . ? N5 Ni1 N2 88.6(3) . . ? N1 Ni1 N9 96.7(3) . . ? N5 Ni1 N9 92.9(3) . . ? N2 Ni1 N9 173.8(3) . . ? N1 Ni1 N6 169.2(3) . . ? N5 Ni1 N6 77.9(3) . . ? N2 Ni1 N6 95.6(3) . . ? N9 Ni1 N6 90.6(3) . . ? N1 Ni1 N10 90.8(3) . . ? N5 Ni1 N10 170.2(3) . . ? N2 Ni1 N10 100.8(3) . . ? N9 Ni1 N10 78.0(3) . . ? N6 Ni1 N10 98.6(3) . . ? N4 Ni2 N12 95.4(3) . . ? N4 Ni2 N8 96.7(3) . . ? N12 Ni2 N8 91.1(3) . . ? N4 Ni2 N3 77.9(3) . . ? N12 Ni2 N3 88.5(3) . . ? N8 Ni2 N3 174.4(3) . . ? N4 Ni2 N11 172.2(3) . . ? N12 Ni2 N11 76.9(3) . . ? N8 Ni2 N11 84.9(3) . . ? N3 Ni2 N11 100.4(3) . . ? N4 Ni2 N7 95.8(3) . . ? N12 Ni2 N7 164.8(3) . . ? N8 Ni2 N7 77.5(3) . . ? N3 Ni2 N7 103.8(3) . . ? N11 Ni2 N7 91.9(3) . . ? F6 P1 F5 90.6(3) . . ? F6 P1 F4 90.5(3) . . ? F5 P1 F4 90.2(3) . . ? F6 P1 F3 91.0(3) . . ? F5 P1 F3 178.4(3) . . ? F4 P1 F3 89.5(3) . . ? F6 P1 F1 179.0(4) . . ? F5 P1 F1 89.2(3) . . ? F4 P1 F1 90.5(3) . . ? F3 P1 F1 89.2(3) . . ? F6 P1 F2 89.6(3) . . ? F5 P1 F2 89.4(3) . . ? F4 P1 F2 179.7(4) . . ? F3 P1 F2 90.9(3) . . ? F1 P1 F2 89.5(3) . . ? F10 P2 F12 95.5(7) . . ? F10 P2 F11 91.0(6) . . ? F12 P2 F11 173.4(7) . . ? F10 P2 F8 175.7(6) . . ? F12 P2 F8 88.4(6) . . ? F11 P2 F8 85.0(5) . . ? F10 P2 F7 92.1(4) . . ? F12 P2 F7 90.9(4) . . ? F11 P2 F7 90.1(4) . . ? F8 P2 F7 89.5(4) . . ? F10 P2 F9 89.7(4) . . ? F12 P2 F9 89.0(4) . . ? F11 P2 F9 89.8(4) . . ? F8 P2 F9 88.8(4) . . ? F7 P2 F9 178.2(4) . . ? F17 P3 F13 91.0(5) . . ? F17 P3 F14 91.3(4) . . ? F13 P3 F14 89.9(4) . . ? F17 P3 F15 91.2(5) . . ? F13 P3 F15 177.6(4) . . ? F14 P3 F15 91.0(4) . . ? F17 P3 F18 178.3(4) . . ? F13 P3 F18 89.3(4) . . ? F14 P3 F18 90.4(3) . . ? F15 P3 F18 88.5(4) . . ? F17 P3 F16 89.1(4) . . ? F13 P3 F16 90.0(4) . . ? F14 P3 F16 179.5(4) . . ? F15 P3 F16 89.1(4) . . ? F18 P3 F16 89.2(3) . . ? F23 P4 F20 90.4(3) . . ? F23 P4 F21 90.8(3) . . ? F20 P4 F21 89.8(3) . . ? F23 P4 F24 178.5(4) . . ? F20 P4 F24 90.3(3) . . ? F21 P4 F24 90.6(3) . . ? F23 P4 F22 90.0(3) . . ? F20 P4 F22 179.4(4) . . ? F21 P4 F22 90.7(3) . . ? F24 P4 F22 89.3(3) . . ? F23 P4 F19 89.1(3) . . ? F20 P4 F19 89.9(3) . . ? F21 P4 F19 179.7(4) . . ? F24 P4 F19 89.5(3) . . ? F22 P4 F19 89.6(3) . . ? N13 C100 C101 171(2) . . ? N14 C102 C103 178.2(16) . . ? N15 C104 C105 174.6(16) . . ? N16 C106 C107 176(2) . . ? C106 N16 C108 28.7(14) . . ? N17 C108 C109 172(2) . . ? N17 C108 N16 93(2) . . ? C109 C108 N16 95(2) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 49.99 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.458 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.080 # Attachment 'mp5_1.cif' data_mp5 _database_code_depnum_ccdc_archive 'CCDC 292898' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C124.75 H102.75 B4 F16 Fe2 N17' _chemical_formula_weight 2298.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4072(12) _cell_length_b 20.3149(17) _cell_length_c 21.2381(19) _cell_angle_alpha 76.1860(10) _cell_angle_beta 87.9410(10) _cell_angle_gamma 87.5210(10) _cell_volume 5610.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 27.08 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2373 _exptl_absorpt_coefficient_mu 0.344 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8118 _exptl_absorpt_correction_T_max 0.9469 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique Set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(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 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 56615 _diffrn_reflns_av_R_equivalents 0.0719 _diffrn_reflns_av_sigmaI/netI 0.0959 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 19630 _reflns_number_gt 11393 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1078P)^2^+3.3111P] 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 19630 _refine_ls_number_parameters 1514 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.1413 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.2191 _refine_ls_wR_factor_gt 0.1846 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.041 _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 Fe1 Fe 0.46573(5) 0.93592(3) 0.25569(4) 0.0348(2) Uani 1 1 d . . . Fe2 Fe 0.90035(5) 0.45153(3) 0.22911(3) 0.03267(19) Uani 1 1 d . . . N101 N 0.4659(3) 0.98280(19) 0.3273(2) 0.0357(10) Uani 1 1 d . . . C102 C 0.3837(4) 1.0079(3) 0.3549(3) 0.0440(13) Uani 1 1 d . . . H10A H 0.3192 0.9990 0.3424 0.053 Uiso 1 1 calc R . . C103 C 0.3916(4) 1.0454(3) 0.3999(3) 0.0475(14) Uani 1 1 d . . . H10B H 0.3328 1.0628 0.4174 0.057 Uiso 1 1 calc R . . C104 C 0.4856(4) 1.0586(2) 0.4207(3) 0.0404(12) Uani 1 1 d . . . C105 C 0.4980(4) 1.0969(3) 0.4674(3) 0.0460(13) Uani 1 1 d . . . H10C H 0.4412 1.1169 0.4845 0.055 Uiso 1 1 calc R . . C106 C 0.5900(4) 1.1051(3) 0.4877(3) 0.0538(15) Uani 1 1 d . . . H10D H 0.5976 1.1307 0.5191 0.065 Uiso 1 1 calc R . . C107 C 0.6756(4) 1.0755(3) 0.4620(3) 0.0551(15) Uani 1 1 d . . . H10E H 0.7398 1.0812 0.4771 0.066 Uiso 1 1 calc R . . C108 C 0.6674(4) 1.0395(3) 0.4167(3) 0.0482(14) Uani 1 1 d . . . H10F H 0.7255 1.0205 0.4000 0.058 Uiso 1 1 calc R . . C109 C 0.5722(4) 1.0301(2) 0.3940(3) 0.0391(12) Uani 1 1 d . . . C110 C 0.5567(3) 0.9935(2) 0.3462(2) 0.0375(12) Uani 1 1 d . . . C111 C 0.6370(4) 0.9635(2) 0.3132(3) 0.0386(12) Uani 1 1 d . . . H11A H 0.7052 0.9688 0.3208 0.046 Uiso 1 1 calc R . . N112 N 0.6103(3) 0.92921(19) 0.27298(19) 0.0344(9) Uani 1 1 d . . . C113 C 0.6889(3) 0.9002(2) 0.2391(2) 0.0351(12) Uani 1 1 d . . . C114 C 0.7086(4) 0.8316(2) 0.2537(3) 0.0432(13) Uani 1 1 d . . . H11B H 0.6703 0.8027 0.2867 0.052 Uiso 1 1 calc R . . C115 C 0.7846(4) 0.8044(3) 0.2204(3) 0.0452(13) Uani 1 1 d . . . H11C H 0.7997 0.7570 0.2327 0.054 Uiso 1 1 calc R . . C116 C 0.8387(4) 0.8440(2) 0.1701(2) 0.0374(12) Uani 1 1 d . . . C117 C 0.8168(4) 0.9133(2) 0.1552(2) 0.0418(13) Uani 1 1 d . . . H11D H 0.8525 0.9418 0.1206 0.050 Uiso 1 1 calc R . . C118 C 0.7446(4) 0.9419(2) 0.1893(2) 0.0403(13) Uani 1 1 d . . . H11E H 0.7327 0.9897 0.1791 0.048 Uiso 1 1 calc R . . C119 C 0.9215(4) 0.8151(2) 0.1328(3) 0.0446(13) Uani 1 1 d . . . H11F H 0.9866 0.8238 0.1492 0.054 Uiso 1 1 calc R . . H11G H 0.9191 0.8394 0.0865 0.054 Uiso 1 1 calc R . . C120 C 0.9160(4) 0.7392(2) 0.1376(2) 0.0386(12) Uani 1 1 d . . . C121 C 0.8324(4) 0.7138(3) 0.1168(3) 0.0430(13) Uani 1 1 d . . . H12A H 0.7790 0.7439 0.0989 0.052 Uiso 1 1 calc R . . C122 C 0.8259(4) 0.6445(3) 0.1220(2) 0.0421(13) Uani 1 1 d . . . H12B H 0.7678 0.6274 0.1082 0.050 Uiso 1 1 calc R . . C123 C 0.9042(4) 0.6006(2) 0.1472(2) 0.0354(11) Uani 1 1 d . . . C124 C 0.9882(3) 0.6257(2) 0.1680(2) 0.0369(12) Uani 1 1 d . . . H12C H 1.0420 0.5957 0.1853 0.044 Uiso 1 1 calc R . . C125 C 0.9936(4) 0.6943(2) 0.1635(3) 0.0406(12) Uani 1 1 d . . . H12D H 1.0512 0.7112 0.1782 0.049 Uiso 1 1 calc R . . N126 N 0.8957(3) 0.52845(19) 0.15221(19) 0.0334(9) Uani 1 1 d . . . C127 C 0.8839(4) 0.5123(2) 0.0979(2) 0.0373(12) Uani 1 1 d . . . H12E H 0.8864 0.5451 0.0577 0.045 Uiso 1 1 calc R . . C128 C 0.8666(3) 0.4418(2) 0.1012(2) 0.0351(11) Uani 1 1 d . . . N129 N 0.8685(3) 0.4029(2) 0.1628(2) 0.0359(10) Uani 1 1 d . . . C130 C 0.8485(4) 0.3361(2) 0.1723(3) 0.0407(12) Uani 1 1 d . . . H13A H 0.8495 0.3084 0.2152 0.049 Uiso 1 1 calc R . . C131 C 0.8271(4) 0.3072(3) 0.1228(3) 0.0425(13) Uani 1 1 d . . . H13B H 0.8135 0.2603 0.1319 0.051 Uiso 1 1 calc R . . C132 C 0.8252(3) 0.3461(3) 0.0588(3) 0.0389(12) Uani 1 1 d . . . C133 C 0.8065(4) 0.3185(3) 0.0056(3) 0.0490(14) Uani 1 1 d . . . H13C H 0.7945 0.2715 0.0130 0.059 Uiso 1 1 calc R . . C134 C 0.8052(4) 0.3578(3) -0.0562(3) 0.0512(15) Uani 1 1 d . . . H13D H 0.7908 0.3383 -0.0912 0.061 Uiso 1 1 calc R . . C135 C 0.8252(4) 0.4271(3) -0.0680(3) 0.0550(15) Uani 1 1 d . . . H13E H 0.8239 0.4544 -0.1111 0.066 Uiso 1 1 calc R . . C136 C 0.8467(4) 0.4558(3) -0.0176(3) 0.0491(14) Uani 1 1 d . . . H13F H 0.8619 0.5024 -0.0262 0.059 Uiso 1 1 calc R . . C137 C 0.8463(3) 0.4160(2) 0.0467(2) 0.0368(12) Uani 1 1 d . . . N201 N 0.4996(3) 1.0197(2) 0.1892(2) 0.0406(11) Uani 1 1 d . . . C202 C 0.5035(4) 1.0834(3) 0.1979(3) 0.0537(15) Uani 1 1 d . . . H20A H 0.4773 1.0926 0.2372 0.064 Uiso 1 1 calc R . . C203 C 0.5441(5) 1.1352(3) 0.1516(3) 0.0630(18) Uani 1 1 d . . . H20B H 0.5455 1.1791 0.1597 0.076 Uiso 1 1 calc R . . C204 C 0.5838(5) 1.1245(3) 0.0923(3) 0.0624(18) Uani 1 1 d . . . C205 C 0.6291(6) 1.1762(4) 0.0427(4) 0.080(2) Uani 1 1 d . . . H20C H 0.6356 1.2202 0.0500 0.096 Uiso 1 1 calc R . . C206 C 0.6619(6) 1.1638(4) -0.0127(4) 0.078(2) Uani 1 1 d . . . H20D H 0.6892 1.1994 -0.0454 0.094 Uiso 1 1 calc R . . C207 C 0.6569(5) 1.0995(4) -0.0238(3) 0.071(2) Uani 1 1 d . . . H20E H 0.6822 1.0913 -0.0638 0.086 Uiso 1 1 calc R . . C208 C 0.6162(4) 1.0474(3) 0.0219(3) 0.0582(16) Uani 1 1 d . . . H20F H 0.6140 1.0035 0.0138 0.070 Uiso 1 1 calc R . . C209 C 0.5771(4) 1.0596(3) 0.0814(3) 0.0518(15) Uani 1 1 d . . . C210 C 0.5331(4) 1.0093(3) 0.1319(3) 0.0410(13) Uani 1 1 d . . . C211 C 0.5194(4) 0.9406(3) 0.1274(3) 0.0425(13) Uani 1 1 d . . . H21A H 0.5362 0.9266 0.0886 0.051 Uiso 1 1 calc R . . N212 N 0.4836(3) 0.89861(19) 0.1778(2) 0.0347(10) Uani 1 1 d . . . C213 C 0.4687(4) 0.8310(2) 0.1707(2) 0.0366(12) Uani 1 1 d . . . C214 C 0.5456(4) 0.7951(3) 0.1474(3) 0.0469(14) Uani 1 1 d . . . H21B H 0.6086 0.8149 0.1363 0.056 Uiso 1 1 calc R . . C215 C 0.5308(4) 0.7305(3) 0.1405(3) 0.0509(15) Uani 1 1 d . . . H21C H 0.5838 0.7063 0.1241 0.061 Uiso 1 1 calc R . . C216 C 0.4403(4) 0.7004(2) 0.1569(2) 0.0401(13) Uani 1 1 d . . . C217 C 0.3622(4) 0.7370(2) 0.1790(2) 0.0355(12) Uani 1 1 d . . . H21D H 0.2991 0.7171 0.1896 0.043 Uiso 1 1 calc R . . C218 C 0.3754(4) 0.8019(2) 0.1855(2) 0.0354(12) Uani 1 1 d . . . H21E H 0.3214 0.8268 0.2001 0.043 Uiso 1 1 calc R . . C219 C 0.4272(4) 0.6271(3) 0.1529(3) 0.0477(14) Uani 1 1 d . . . H21F H 0.3657 0.6098 0.1774 0.057 Uiso 1 1 calc R . . H21G H 0.4193 0.6257 0.1071 0.057 Uiso 1 1 calc R . . C220 C 0.5154(3) 0.5821(2) 0.1801(2) 0.0370(12) Uani 1 1 d . . . C221 C 0.5691(4) 0.5441(3) 0.1438(3) 0.0414(13) Uani 1 1 d . . . H22A H 0.5496 0.5463 0.1007 0.050 Uiso 1 1 calc R . . C222 C 0.6508(3) 0.5025(2) 0.1685(2) 0.0377(12) Uani 1 1 d . . . H22B H 0.6870 0.4769 0.1426 0.045 Uiso 1 1 calc R . . C223 C 0.6784(3) 0.4991(2) 0.2317(2) 0.0339(11) Uani 1 1 d . . . C224 C 0.6250(4) 0.5364(2) 0.2696(2) 0.0386(12) Uani 1 1 d . . . H22C H 0.6435 0.5339 0.3129 0.046 Uiso 1 1 calc R . . C225 C 0.5438(4) 0.5774(3) 0.2429(3) 0.0437(13) Uani 1 1 d . . . H22D H 0.5070 0.6029 0.2685 0.052 Uiso 1 1 calc R . . N226 N 0.7594(3) 0.45385(19) 0.25925(19) 0.0326(9) Uani 1 1 d . . . C227 C 0.7390(4) 0.4098(2) 0.3121(2) 0.0361(12) Uani 1 1 d . . . H22E H 0.6746 0.4091 0.3324 0.043 Uiso 1 1 calc R . . C228 C 0.8176(3) 0.3613(2) 0.3399(2) 0.0330(11) Uani 1 1 d . . . N229 N 0.9022(3) 0.36881(19) 0.30274(19) 0.0341(9) Uani 1 1 d . . . C230 C 0.9799(4) 0.3227(2) 0.3207(3) 0.0391(12) Uani 1 1 d . . . H23A H 1.0391 0.3265 0.2942 0.047 Uiso 1 1 calc R . . C231 C 0.9745(4) 0.2719(3) 0.3752(3) 0.0429(13) Uani 1 1 d . . . H23B H 1.0302 0.2411 0.3858 0.051 Uiso 1 1 calc R . . C232 C 0.8894(4) 0.2630(2) 0.4168(2) 0.0384(12) Uani 1 1 d . . . C233 C 0.8812(4) 0.2113(3) 0.4741(3) 0.0441(13) Uani 1 1 d . . . H23C H 0.9355 0.1798 0.4866 0.053 Uiso 1 1 calc R . . C234 C 0.7958(5) 0.2063(3) 0.5118(3) 0.0537(15) Uani 1 1 d . . . H23D H 0.7910 0.1712 0.5503 0.064 Uiso 1 1 calc R . . C235 C 0.7149(4) 0.2527(3) 0.4942(3) 0.0528(15) Uani 1 1 d . . . H23E H 0.6564 0.2492 0.5212 0.063 Uiso 1 1 calc R . . C236 C 0.7197(4) 0.3029(3) 0.4385(3) 0.0457(13) Uani 1 1 d . . . H23F H 0.6641 0.3335 0.4268 0.055 Uiso 1 1 calc R . . C237 C 0.8070(3) 0.3097(2) 0.3980(2) 0.0346(11) Uani 1 1 d . . . N301 N 0.3201(3) 0.9469(2) 0.2463(2) 0.0389(10) Uani 1 1 d . . . C302 C 0.2706(4) 1.0017(3) 0.2085(3) 0.0455(14) Uani 1 1 d . . . H30A H 0.3077 1.0370 0.1815 0.055 Uiso 1 1 calc R . . C303 C 0.1687(4) 1.0065(3) 0.2089(3) 0.0499(15) Uani 1 1 d . . . H30B H 0.1363 1.0451 0.1820 0.060 Uiso 1 1 calc R . . C304 C 0.1107(4) 0.9561(3) 0.2478(3) 0.0438(13) Uani 1 1 d . . . C305 C 0.0038(4) 0.9601(3) 0.2522(3) 0.0543(16) Uani 1 1 d . . . H30C H -0.0312 0.9988 0.2275 0.065 Uiso 1 1 calc R . . C306 C -0.0477(4) 0.9098(3) 0.2909(3) 0.0561(16) Uani 1 1 d . . . H30D H -0.1184 0.9143 0.2947 0.067 Uiso 1 1 calc R . . C307 C 0.0025(4) 0.8504(3) 0.3258(3) 0.0514(14) Uani 1 1 d . . . H30E H -0.0350 0.8146 0.3514 0.062 Uiso 1 1 calc R . . C308 C 0.1039(4) 0.8439(3) 0.3232(3) 0.0455(13) Uani 1 1 d . . . H30F H 0.1365 0.8037 0.3472 0.055 Uiso 1 1 calc R . . C309 C 0.1608(3) 0.8961(3) 0.2851(2) 0.0367(12) Uani 1 1 d . . . C310 C 0.2667(3) 0.8964(2) 0.2826(2) 0.0334(11) Uani 1 1 d . . . C311 C 0.3299(3) 0.8421(2) 0.3206(2) 0.0311(11) Uani 1 1 d . . . H31A H 0.3026 0.8024 0.3474 0.037 Uiso 1 1 calc R . . N312 N 0.4249(3) 0.85104(18) 0.31581(18) 0.0313(9) Uani 1 1 d . . . C313 C 0.4891(3) 0.7966(2) 0.3512(2) 0.0289(11) Uani 1 1 d . . . C314 C 0.5569(3) 0.8095(2) 0.3944(2) 0.0328(11) Uani 1 1 d . . . H31B H 0.5590 0.8536 0.4022 0.039 Uiso 1 1 calc R . . C315 C 0.6214(3) 0.7581(2) 0.4262(2) 0.0353(12) Uani 1 1 d . . . H31C H 0.6677 0.7674 0.4555 0.042 Uiso 1 1 calc R . . C316 C 0.6194(3) 0.6937(2) 0.4158(2) 0.0346(11) Uani 1 1 d . . . C317 C 0.5498(3) 0.6810(2) 0.3742(2) 0.0354(12) Uani 1 1 d . . . H31D H 0.5468 0.6364 0.3676 0.043 Uiso 1 1 calc R . . C318 C 0.4844(4) 0.7313(2) 0.3416(2) 0.0361(12) Uani 1 1 d . . . H31E H 0.4372 0.7215 0.3131 0.043 Uiso 1 1 calc R . . C319 C 0.6912(4) 0.6372(3) 0.4508(2) 0.0375(12) Uani 1 1 d . . . H31F H 0.7351 0.6565 0.4778 0.045 Uiso 1 1 calc R . . H31G H 0.6515 0.6022 0.4805 0.045 Uiso 1 1 calc R . . C320 C 0.7565(3) 0.6027(2) 0.4078(2) 0.0329(11) Uani 1 1 d . . . C321 C 0.7786(4) 0.6317(3) 0.3445(3) 0.0474(14) Uani 1 1 d . . . H32A H 0.7505 0.6755 0.3260 0.057 Uiso 1 1 calc R . . C322 C 0.8400(4) 0.6004(3) 0.3058(3) 0.0485(14) Uani 1 1 d . . . H32B H 0.8527 0.6224 0.2617 0.058 Uiso 1 1 calc R . . C323 C 0.8829(3) 0.5366(2) 0.3318(2) 0.0310(11) Uani 1 1 d . . . C324 C 0.8617(4) 0.5067(3) 0.3955(3) 0.0452(13) Uani 1 1 d . . . H32C H 0.8908 0.4633 0.4143 0.054 Uiso 1 1 calc R . . C325 C 0.7989(4) 0.5384(3) 0.4332(3) 0.0433(13) Uani 1 1 d . . . H32D H 0.7844 0.5160 0.4770 0.052 Uiso 1 1 calc R . . N326 N 0.9450(3) 0.50215(18) 0.29120(18) 0.0318(9) Uani 1 1 d . . . C327 C 1.0401(3) 0.4984(2) 0.2998(2) 0.0341(11) Uani 1 1 d . . . H32E H 1.0691 0.5172 0.3314 0.041 Uiso 1 1 calc R . . C328 C 1.1006(3) 0.4637(2) 0.2582(2) 0.0352(12) Uani 1 1 d . . . N329 N 1.0456(3) 0.4418(2) 0.21633(19) 0.0359(10) Uani 1 1 d . . . C330 C 1.0925(4) 0.4084(3) 0.1742(2) 0.0412(13) Uani 1 1 d . . . H33A H 1.0534 0.3933 0.1443 0.049 Uiso 1 1 calc R . . C331 C 1.1931(4) 0.3960(3) 0.1735(3) 0.0470(14) Uani 1 1 d . . . H33B H 1.2225 0.3724 0.1436 0.056 Uiso 1 1 calc R . . C332 C 1.2538(4) 0.4177(3) 0.2164(3) 0.0430(13) Uani 1 1 d . . . C333 C 1.3584(4) 0.4057(3) 0.2177(3) 0.0528(15) Uani 1 1 d . . . H33C H 1.3905 0.3814 0.1891 0.063 Uiso 1 1 calc R . . C334 C 1.4127(4) 0.4291(3) 0.2600(3) 0.0559(16) Uani 1 1 d . . . H33D H 1.4832 0.4215 0.2603 0.067 Uiso 1 1 calc R . . C335 C 1.3671(4) 0.4638(3) 0.3028(3) 0.0563(16) Uani 1 1 d . . . H33E H 1.4068 0.4796 0.3320 0.068 Uiso 1 1 calc R . . C336 C 1.2654(4) 0.4759(3) 0.3038(3) 0.0469(14) Uani 1 1 d . . . H33F H 1.2353 0.4993 0.3337 0.056 Uiso 1 1 calc R . . C337 C 1.2064(3) 0.4535(2) 0.2604(3) 0.0388(12) Uani 1 1 d . . . B10 B 1.1753(5) 0.1442(3) 0.5175(4) 0.0488(16) Uani 1 1 d . . . F11 F 1.1018(3) 0.1166(2) 0.4912(2) 0.1048(15) Uani 1 1 d . . . F12 F 1.1949(3) 0.1054(2) 0.5787(2) 0.0949(13) Uani 1 1 d . . . F13 F 1.2615(3) 0.14771(19) 0.48074(19) 0.0780(11) Uani 1 1 d . . . F14 F 1.1440(3) 0.20836(17) 0.52164(19) 0.0732(10) Uani 1 1 d . . . B20 B 0.7044(7) 0.8740(6) -0.0258(5) 0.102(3) Uani 1 1 d D . . F21 F 0.6546(8) 0.9315(6) -0.0589(4) 0.188(6) Uani 0.653(11) 1 d PDU A 1 F22 F 0.6650(17) 0.8126(10) -0.0310(12) 0.337(12) Uani 0.653(11) 1 d PDU A 1 F23 F 0.7812(8) 0.8811(5) -0.0672(5) 0.162(5) Uani 0.653(11) 1 d PD A 1 F24 F 0.7164(7) 0.8795(4) 0.0339(3) 0.129(4) Uani 0.653(11) 1 d PD A 1 F21A F 0.7941(15) 0.9014(13) -0.0139(16) 0.213(12) Uiso 0.347(11) 1 d PD A 2 F22A F 0.7128(14) 0.8033(7) -0.0133(9) 0.117(5) Uiso 0.347(11) 1 d PD A 2 F23A F 0.684(3) 0.893(2) -0.0914(10) 0.33(2) Uiso 0.347(11) 1 d PD A 2 F24A F 0.6130(10) 0.8832(8) 0.0007(8) 0.117(5) Uiso 0.347(11) 1 d PD A 2 B30 B 0.2217(7) 0.6391(4) 0.3334(5) 0.086(3) Uani 1 1 d D . . F31 F 0.3199(3) 0.62315(17) 0.31942(19) 0.0743(10) Uani 1 1 d D B . F32 F 0.2129(6) 0.7052(4) 0.3248(5) 0.0743(10) Uani 0.480(8) 1 d P B 1 F33 F 0.1731(13) 0.5961(8) 0.3721(10) 0.131(10) Uani 0.480(8) 1 d P B 1 F34 F 0.1806(5) 0.6312(4) 0.2659(5) 0.072(3) Uani 0.480(8) 1 d P B 1 F32A F 0.2263(5) 0.6934(4) 0.3700(4) 0.069(2) Uiso 0.520(8) 1 d PD B 2 F33A F 0.1744(11) 0.5884(8) 0.3792(7) 0.083(5) Uiso 0.520(8) 1 d PD B 2 F34A F 0.1649(10) 0.6647(8) 0.2846(7) 0.155(6) Uiso 0.520(8) 1 d PD B 2 B40 B 0.8364(6) 1.1306(4) 0.2277(5) 0.075(2) Uani 1 1 d . . . F41 F 0.7533(4) 1.1575(3) 0.1947(3) 0.159(2) Uani 1 1 d . . . F42 F 0.9128(5) 1.1244(3) 0.1858(3) 0.147(2) Uani 1 1 d . . . F43 F 0.8585(4) 1.1778(2) 0.2603(3) 0.1240(17) Uani 1 1 d . . . F44 F 0.8172(3) 1.0701(2) 0.2695(2) 0.1017(14) Uani 1 1 d . . . C21 C 0.4410(8) 0.5217(5) 0.4461(6) 0.095(2) Uani 0.75 1 d PD . . H21H H 0.3979 0.5347 0.4104 0.114 Uiso 0.75 1 calc PR . . C22 C 0.5272(8) 0.4679(5) 0.4433(5) 0.085(3) Uani 0.75 1 d PD . . H22I H 0.5429 0.4516 0.4056 0.102 Uiso 0.75 1 calc PR . . C23 C 0.5769(6) 0.4467(4) 0.4987(4) 0.095(2) Uani 0.75 1 d P . . H23J H 0.6250 0.4103 0.5024 0.114 Uiso 0.75 1 calc PR . . C31 C 0.9139(6) 1.0055(4) -0.0311(4) 0.075(4) Uani 0.50 1 d PR . . H31H H 0.8533 1.0087 -0.0536 0.090 Uiso 0.50 1 d PR . . C32 C 0.9235(9) 1.0494(7) 0.0111(7) 0.071(4) Uani 0.50 1 d P . . H32F H 0.8720 1.0811 0.0172 0.085 Uiso 0.50 1 calc PR . . C33 C 1.0120(9) 1.0431(7) 0.0424(6) 0.065(4) Uani 0.50 1 d P . . H33G H 1.0239 1.0708 0.0714 0.078 Uiso 0.50 1 calc PR . . C401 C 0.4957(8) 0.5893(6) -0.0577(6) 0.149(4) Uani 1 1 d U . . H40A H 0.4441 0.5645 -0.0698 0.178 Uiso 1 1 calc R . . C402 C 0.4795(8) 0.6543(6) -0.0543(7) 0.155(4) Uani 1 1 d U . . H40B H 0.4156 0.6754 -0.0645 0.186 Uiso 1 1 calc R . . C403 C 0.5526(7) 0.6907(5) -0.0366(5) 0.129(4) Uani 1 1 d U . . H40C H 0.5404 0.7367 -0.0348 0.154 Uiso 1 1 calc R . . C404 C 0.6427(6) 0.6595(5) -0.0219(4) 0.092(3) Uani 1 1 d . . . H40D H 0.6944 0.6846 -0.0103 0.111 Uiso 1 1 calc R . . C405 C 0.6617(6) 0.5953(5) -0.0230(4) 0.088(2) Uani 1 1 d . . . H40E H 0.7247 0.5741 -0.0100 0.106 Uiso 1 1 calc R . . C406 C 0.5894(8) 0.5595(6) -0.0430(5) 0.124(3) Uani 1 1 d . . . H40F H 0.6038 0.5144 -0.0469 0.149 Uiso 1 1 calc R . . N600 N 0.9155(4) 0.6440(3) -0.0376(3) 0.0629(14) Uani 1 1 d . . . C601 C 0.9355(4) 0.6986(4) -0.0390(3) 0.0564(16) Uani 1 1 d . . . C602 C 0.9609(5) 0.7691(3) -0.0407(3) 0.0729(19) Uani 1 1 d . . . H60A H 1.0077 0.7855 -0.0771 0.109 Uiso 1 1 calc R . . H60B H 0.9920 0.7705 0.0000 0.109 Uiso 1 1 calc R . . H60C H 0.9000 0.7982 -0.0461 0.109 Uiso 1 1 calc R . . C501 C 0.2355(16) 1.2137(7) 0.1832(7) 0.165(6) Uani 1 1 d U . . H50A H 0.2437 1.2275 0.1374 0.199 Uiso 1 1 calc R . . C502 C 0.1466(12) 1.1928(6) 0.2086(6) 0.148(5) Uani 1 1 d U . . H50B H 0.0931 1.1928 0.1804 0.178 Uiso 1 1 calc R . . C503 C 0.1312(8) 1.1721(5) 0.2718(5) 0.110(3) Uani 1 1 d U . . H50C H 0.0669 1.1579 0.2887 0.131 Uiso 1 1 calc R . . C504 C 0.2061(9) 1.1710(5) 0.3125(4) 0.110(3) Uani 1 1 d U . . H50D H 0.1951 1.1550 0.3579 0.132 Uiso 1 1 calc R . . C505 C 0.3006(9) 1.1935(5) 0.2880(7) 0.125(4) Uani 1 1 d U . . H50E H 0.3533 1.1932 0.3167 0.150 Uiso 1 1 calc R . . C506 C 0.3167(10) 1.2161(5) 0.2215(8) 0.137(4) Uani 1 1 d U . . H50F H 0.3794 1.2322 0.2032 0.164 Uiso 1 1 calc R . . N700 N 1.1475(4) -0.0320(3) 0.4108(3) 0.0725(16) Uani 1 1 d . . . C701 C 1.0731(5) -0.0044(3) 0.4080(3) 0.0589(16) Uani 1 1 d . . . C702 C 0.9752(5) 0.0313(3) 0.4067(3) 0.0732(19) Uani 1 1 d . . . H70A H 0.9242 -0.0011 0.4262 0.110 Uiso 1 1 calc R . . H70B H 0.9584 0.0526 0.3617 0.110 Uiso 1 1 calc R . . H70C H 0.9776 0.0663 0.4313 0.110 Uiso 1 1 calc R . . N800 N 0.5250(6) 0.6925(4) 0.5958(4) 0.118(3) Uani 1 1 d . . . C801 C 0.6083(7) 0.6948(4) 0.6017(3) 0.075(2) Uani 1 1 d . . . C802 C 0.7140(5) 0.6944(4) 0.6089(3) 0.080(2) Uani 1 1 d . . . H80A H 0.7282 0.6991 0.6525 0.120 Uiso 1 1 calc R . . H80B H 0.7420 0.7324 0.5766 0.120 Uiso 1 1 calc R . . H80C H 0.7440 0.6516 0.6025 0.120 Uiso 1 1 calc R . . N900 N 1.0809(5) 0.3993(3) 0.4373(3) 0.0782(18) Uani 1 1 d . . . C901 C 1.0466(5) 0.3722(4) 0.4863(4) 0.0626(18) Uani 1 1 d . . . C902 C 1.0028(5) 0.3385(4) 0.5490(4) 0.083(2) Uani 1 1 d . . . H90A H 1.0284 0.3579 0.5830 0.124 Uiso 1 1 calc R . . H90B H 1.0207 0.2899 0.5582 0.124 Uiso 1 1 calc R . . H90C H 0.9300 0.3449 0.5479 0.124 Uiso 1 1 calc R . . N10 N 0.6086(5) 0.3198(4) 0.2293(4) 0.117(3) Uani 1 1 d . . . C11 C 0.6155(5) 0.2704(4) 0.2666(4) 0.075(2) Uani 1 1 d . . . C12 C 0.6273(6) 0.2095(4) 0.3154(4) 0.096(2) Uani 1 1 d . . . H12F H 0.6025 0.1716 0.3000 0.144 Uiso 1 1 calc R . . H12G H 0.5895 0.2139 0.3546 0.144 Uiso 1 1 calc R . . H12H H 0.6982 0.2010 0.3253 0.144 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0329(4) 0.0270(4) 0.0447(5) -0.0082(3) -0.0112(3) 0.0044(3) Fe2 0.0326(4) 0.0308(4) 0.0365(4) -0.0126(3) -0.0031(3) 0.0059(3) N101 0.032(2) 0.027(2) 0.049(3) -0.011(2) -0.0075(19) 0.0051(17) C102 0.033(3) 0.039(3) 0.063(4) -0.019(3) -0.008(3) 0.006(2) C103 0.039(3) 0.043(3) 0.063(4) -0.020(3) 0.000(3) 0.014(2) C104 0.044(3) 0.030(3) 0.050(3) -0.014(2) -0.008(3) 0.005(2) C105 0.044(3) 0.042(3) 0.055(4) -0.020(3) 0.005(3) 0.003(2) C106 0.053(4) 0.055(4) 0.063(4) -0.032(3) -0.006(3) -0.001(3) C107 0.044(3) 0.057(4) 0.072(4) -0.031(3) -0.015(3) 0.004(3) C108 0.043(3) 0.043(3) 0.065(4) -0.025(3) -0.007(3) 0.008(2) C109 0.038(3) 0.030(3) 0.052(3) -0.014(2) -0.005(2) 0.004(2) C110 0.034(3) 0.032(3) 0.048(3) -0.011(2) -0.008(2) 0.006(2) C111 0.032(3) 0.033(3) 0.053(3) -0.015(3) -0.009(2) 0.004(2) N112 0.035(2) 0.026(2) 0.042(3) -0.0086(19) -0.0048(19) 0.0023(17) C113 0.027(2) 0.036(3) 0.044(3) -0.014(2) -0.009(2) 0.001(2) C114 0.044(3) 0.029(3) 0.054(3) -0.005(3) 0.008(3) -0.003(2) C115 0.048(3) 0.026(3) 0.060(4) -0.010(3) 0.004(3) 0.007(2) C116 0.042(3) 0.035(3) 0.037(3) -0.011(2) -0.006(2) 0.001(2) C117 0.054(3) 0.030(3) 0.038(3) -0.001(2) 0.002(3) -0.001(2) C118 0.047(3) 0.026(3) 0.047(3) -0.006(2) -0.010(3) 0.005(2) C119 0.051(3) 0.035(3) 0.050(3) -0.016(3) 0.010(3) -0.001(2) C120 0.045(3) 0.035(3) 0.038(3) -0.012(2) 0.009(2) 0.000(2) C121 0.046(3) 0.034(3) 0.049(3) -0.013(3) -0.005(3) 0.010(2) C122 0.042(3) 0.045(3) 0.041(3) -0.015(3) -0.009(2) 0.006(2) C123 0.043(3) 0.034(3) 0.031(3) -0.012(2) 0.005(2) 0.004(2) C124 0.034(3) 0.037(3) 0.039(3) -0.008(2) 0.003(2) 0.006(2) C125 0.038(3) 0.038(3) 0.048(3) -0.015(3) 0.003(2) -0.001(2) N126 0.036(2) 0.030(2) 0.035(2) -0.0120(19) -0.0016(18) 0.0061(17) C127 0.044(3) 0.038(3) 0.030(3) -0.011(2) -0.002(2) 0.008(2) C128 0.036(3) 0.036(3) 0.035(3) -0.013(2) 0.000(2) 0.008(2) N129 0.037(2) 0.034(2) 0.039(3) -0.014(2) -0.0045(19) 0.0082(18) C130 0.048(3) 0.031(3) 0.044(3) -0.011(2) -0.001(3) 0.000(2) C131 0.041(3) 0.041(3) 0.050(3) -0.021(3) 0.003(3) -0.003(2) C132 0.031(3) 0.043(3) 0.047(3) -0.020(3) -0.005(2) 0.002(2) C133 0.040(3) 0.055(4) 0.061(4) -0.029(3) -0.004(3) -0.004(3) C134 0.044(3) 0.070(4) 0.051(4) -0.036(3) -0.006(3) 0.002(3) C135 0.065(4) 0.061(4) 0.042(3) -0.018(3) -0.011(3) 0.009(3) C136 0.058(4) 0.048(3) 0.047(4) -0.023(3) -0.003(3) 0.007(3) C137 0.035(3) 0.038(3) 0.039(3) -0.013(2) 0.001(2) 0.006(2) N201 0.040(2) 0.029(2) 0.053(3) -0.007(2) -0.018(2) 0.0013(18) C202 0.062(4) 0.031(3) 0.067(4) -0.009(3) -0.014(3) 0.002(3) C203 0.074(4) 0.032(3) 0.082(5) -0.007(3) -0.021(4) -0.004(3) C204 0.071(4) 0.048(4) 0.063(4) 0.002(3) -0.030(4) -0.008(3) C205 0.102(6) 0.057(4) 0.073(5) 0.009(4) -0.021(4) -0.032(4) C206 0.097(5) 0.070(5) 0.057(5) 0.016(4) -0.031(4) -0.038(4) C207 0.075(5) 0.085(5) 0.047(4) 0.005(4) -0.017(3) -0.031(4) C208 0.057(4) 0.058(4) 0.053(4) 0.003(3) -0.017(3) -0.009(3) C209 0.052(3) 0.046(3) 0.054(4) 0.001(3) -0.027(3) -0.008(3) C210 0.040(3) 0.040(3) 0.039(3) 0.001(3) -0.018(2) -0.006(2) C211 0.044(3) 0.040(3) 0.042(3) -0.004(3) -0.014(3) -0.003(2) N212 0.034(2) 0.030(2) 0.040(3) -0.007(2) -0.0121(19) 0.0040(17) C213 0.045(3) 0.033(3) 0.032(3) -0.008(2) -0.013(2) 0.002(2) C214 0.034(3) 0.042(3) 0.063(4) -0.010(3) -0.008(3) 0.002(2) C215 0.041(3) 0.041(3) 0.073(4) -0.020(3) -0.012(3) 0.009(3) C216 0.042(3) 0.035(3) 0.043(3) -0.008(2) -0.019(2) 0.005(2) C217 0.039(3) 0.033(3) 0.035(3) -0.008(2) -0.010(2) -0.003(2) C218 0.041(3) 0.036(3) 0.029(3) -0.008(2) -0.008(2) 0.003(2) C219 0.048(3) 0.041(3) 0.058(4) -0.017(3) -0.022(3) 0.008(2) C220 0.037(3) 0.030(3) 0.047(3) -0.017(2) -0.015(2) 0.005(2) C221 0.043(3) 0.042(3) 0.041(3) -0.011(3) -0.015(2) 0.000(2) C222 0.036(3) 0.039(3) 0.040(3) -0.014(2) -0.001(2) 0.005(2) C223 0.031(3) 0.031(3) 0.039(3) -0.008(2) -0.001(2) -0.001(2) C224 0.041(3) 0.038(3) 0.039(3) -0.014(2) -0.008(2) 0.005(2) C225 0.041(3) 0.043(3) 0.053(4) -0.026(3) -0.009(3) 0.013(2) N226 0.032(2) 0.033(2) 0.035(2) -0.012(2) -0.0082(18) 0.0066(17) C227 0.032(3) 0.035(3) 0.042(3) -0.012(3) -0.003(2) 0.007(2) C228 0.034(3) 0.030(3) 0.038(3) -0.014(2) -0.002(2) 0.001(2) N229 0.035(2) 0.032(2) 0.038(2) -0.0141(19) -0.0019(19) 0.0046(18) C230 0.034(3) 0.033(3) 0.049(3) -0.008(3) -0.004(2) 0.008(2) C231 0.041(3) 0.037(3) 0.051(3) -0.011(3) -0.015(3) 0.014(2) C232 0.040(3) 0.035(3) 0.042(3) -0.013(2) -0.009(2) 0.002(2) C233 0.047(3) 0.034(3) 0.052(4) -0.010(3) -0.016(3) 0.008(2) C234 0.071(4) 0.043(3) 0.044(3) -0.004(3) -0.004(3) -0.002(3) C235 0.052(3) 0.048(3) 0.054(4) -0.007(3) 0.007(3) 0.001(3) C236 0.043(3) 0.040(3) 0.050(3) -0.005(3) 0.006(3) 0.004(2) C237 0.035(3) 0.027(3) 0.043(3) -0.012(2) -0.007(2) 0.000(2) N301 0.037(2) 0.032(2) 0.048(3) -0.007(2) -0.015(2) 0.0032(19) C302 0.042(3) 0.035(3) 0.056(4) -0.002(3) -0.017(3) 0.003(2) C303 0.046(3) 0.040(3) 0.063(4) -0.010(3) -0.025(3) 0.015(3) C304 0.040(3) 0.043(3) 0.051(3) -0.014(3) -0.016(3) 0.009(2) C305 0.038(3) 0.062(4) 0.064(4) -0.016(3) -0.020(3) 0.017(3) C306 0.030(3) 0.083(5) 0.058(4) -0.024(4) -0.008(3) 0.007(3) C307 0.040(3) 0.057(4) 0.055(4) -0.009(3) -0.003(3) -0.002(3) C308 0.038(3) 0.049(3) 0.050(3) -0.013(3) -0.011(3) 0.005(3) C309 0.036(3) 0.043(3) 0.035(3) -0.017(2) -0.010(2) 0.007(2) C310 0.035(3) 0.033(3) 0.036(3) -0.015(2) -0.009(2) 0.003(2) C311 0.032(3) 0.029(2) 0.033(3) -0.009(2) -0.005(2) 0.004(2) N312 0.033(2) 0.031(2) 0.032(2) -0.0113(18) -0.0092(18) 0.0060(17) C313 0.024(2) 0.030(3) 0.030(3) -0.002(2) -0.002(2) 0.0051(19) C314 0.036(3) 0.027(2) 0.037(3) -0.011(2) -0.005(2) 0.004(2) C315 0.034(3) 0.040(3) 0.034(3) -0.012(2) -0.008(2) 0.006(2) C316 0.035(3) 0.035(3) 0.033(3) -0.009(2) -0.002(2) 0.011(2) C317 0.040(3) 0.029(3) 0.039(3) -0.013(2) -0.009(2) 0.009(2) C318 0.039(3) 0.036(3) 0.036(3) -0.011(2) -0.011(2) 0.001(2) C319 0.040(3) 0.045(3) 0.028(3) -0.010(2) -0.006(2) 0.014(2) C320 0.034(3) 0.032(3) 0.034(3) -0.011(2) -0.010(2) 0.009(2) C321 0.059(3) 0.036(3) 0.043(3) -0.006(3) 0.003(3) 0.020(3) C322 0.062(4) 0.044(3) 0.035(3) -0.004(3) 0.005(3) 0.018(3) C323 0.030(2) 0.031(3) 0.035(3) -0.013(2) -0.004(2) 0.004(2) C324 0.059(3) 0.034(3) 0.040(3) -0.006(3) -0.004(3) 0.019(2) C325 0.054(3) 0.042(3) 0.033(3) -0.009(2) 0.000(2) 0.015(3) N326 0.031(2) 0.030(2) 0.034(2) -0.0095(18) -0.0040(18) 0.0056(17) C327 0.033(3) 0.034(3) 0.036(3) -0.009(2) -0.006(2) 0.003(2) C328 0.033(3) 0.028(3) 0.043(3) -0.007(2) -0.001(2) 0.005(2) N329 0.035(2) 0.034(2) 0.040(2) -0.013(2) -0.0009(19) 0.0042(18) C330 0.045(3) 0.041(3) 0.042(3) -0.018(3) -0.002(2) 0.006(2) C331 0.042(3) 0.053(3) 0.049(3) -0.019(3) 0.008(3) 0.008(3) C332 0.035(3) 0.037(3) 0.053(3) -0.006(3) 0.007(3) 0.004(2) C333 0.040(3) 0.048(3) 0.070(4) -0.017(3) 0.008(3) 0.006(3) C334 0.030(3) 0.046(3) 0.089(5) -0.012(3) 0.001(3) 0.006(3) C335 0.033(3) 0.052(4) 0.087(5) -0.022(3) -0.007(3) -0.003(3) C336 0.035(3) 0.043(3) 0.066(4) -0.020(3) -0.005(3) 0.002(2) C337 0.033(3) 0.032(3) 0.051(3) -0.011(3) 0.002(2) 0.003(2) B10 0.041(4) 0.046(4) 0.063(5) -0.020(4) 0.000(3) 0.002(3) F11 0.073(3) 0.102(3) 0.160(4) -0.066(3) -0.036(3) -0.005(2) F12 0.122(3) 0.083(3) 0.072(3) -0.008(2) -0.011(2) 0.027(2) F13 0.061(2) 0.081(3) 0.098(3) -0.037(2) 0.021(2) 0.0023(19) F14 0.066(2) 0.055(2) 0.099(3) -0.025(2) 0.004(2) 0.0147(17) B20 0.058(6) 0.134(10) 0.121(10) -0.041(8) -0.017(6) 0.005(6) F21 0.205(10) 0.261(12) 0.092(7) -0.051(8) -0.069(7) 0.158(9) F22 0.34(2) 0.33(2) 0.39(2) -0.169(19) -0.003(18) -0.088(17) F23 0.158(9) 0.159(9) 0.150(9) -0.019(7) 0.076(7) 0.041(7) F24 0.200(10) 0.131(7) 0.051(5) -0.001(4) -0.013(5) -0.054(6) B30 0.083(6) 0.039(4) 0.132(9) -0.015(5) -0.015(6) 0.009(4) F31 0.063(2) 0.060(2) 0.102(3) -0.024(2) 0.0018(19) 0.0014(16) F32 0.063(2) 0.060(2) 0.102(3) -0.024(2) 0.0018(19) 0.0014(16) F33 0.137(12) 0.080(9) 0.210(18) -0.107(10) 0.133(12) -0.085(8) F34 0.045(4) 0.052(5) 0.113(7) 0.000(5) -0.045(4) -0.005(4) B40 0.067(5) 0.053(5) 0.099(7) -0.006(5) -0.016(5) 0.015(4) F41 0.137(5) 0.129(5) 0.190(6) 0.011(4) -0.084(4) 0.007(4) F42 0.169(5) 0.111(4) 0.147(5) -0.014(4) 0.072(4) -0.003(4) F43 0.139(4) 0.083(3) 0.161(5) -0.048(3) -0.009(4) -0.014(3) F44 0.125(4) 0.058(3) 0.111(3) -0.002(3) 0.016(3) -0.002(2) C21 0.109(6) 0.059(5) 0.126(7) -0.032(4) -0.001(5) -0.028(4) C22 0.132(9) 0.065(6) 0.065(6) -0.025(5) -0.047(6) 0.002(6) C23 0.109(6) 0.059(5) 0.126(7) -0.032(4) -0.001(5) -0.028(4) C31 0.051(8) 0.087(10) 0.071(10) 0.021(8) -0.030(7) -0.016(8) C32 0.040(7) 0.069(9) 0.080(10) 0.033(8) -0.015(7) -0.017(6) C33 0.055(8) 0.067(8) 0.061(8) 0.012(7) -0.010(6) -0.023(7) C401 0.105(8) 0.151(10) 0.230(13) -0.125(10) -0.042(8) 0.029(7) C402 0.098(7) 0.139(9) 0.254(13) -0.100(10) -0.031(8) 0.025(7) C403 0.091(6) 0.127(8) 0.187(10) -0.071(8) -0.053(7) 0.021(6) C404 0.063(5) 0.124(8) 0.080(6) -0.008(5) -0.009(4) 0.021(5) C405 0.072(5) 0.115(7) 0.076(5) -0.022(5) -0.006(4) 0.026(5) C406 0.123(8) 0.134(9) 0.129(8) -0.063(7) -0.010(7) 0.040(7) N600 0.063(3) 0.074(4) 0.056(3) -0.025(3) 0.000(3) 0.005(3) C601 0.049(4) 0.075(5) 0.045(4) -0.016(4) 0.003(3) 0.014(3) C602 0.076(5) 0.065(4) 0.079(5) -0.023(4) 0.003(4) 0.009(4) C501 0.280(19) 0.112(9) 0.097(9) -0.008(7) 0.006(11) -0.026(11) C502 0.253(15) 0.107(8) 0.082(8) -0.008(6) -0.055(9) -0.025(9) C503 0.149(8) 0.092(6) 0.095(7) -0.035(6) -0.033(6) 0.016(6) C504 0.149(9) 0.108(7) 0.071(6) -0.025(5) -0.021(6) 0.057(7) C505 0.122(8) 0.105(8) 0.154(10) -0.048(8) -0.036(8) 0.052(7) C506 0.164(11) 0.073(6) 0.162(12) -0.015(8) 0.038(9) 0.030(7) N700 0.061(4) 0.085(4) 0.080(4) -0.038(3) -0.015(3) 0.010(3) C701 0.057(4) 0.061(4) 0.064(4) -0.023(3) -0.014(3) 0.002(3) C702 0.060(4) 0.074(5) 0.088(5) -0.025(4) -0.015(4) 0.007(3) N800 0.085(5) 0.151(7) 0.118(6) -0.034(5) -0.023(5) 0.027(5) C801 0.084(6) 0.080(5) 0.060(5) -0.016(4) -0.009(4) 0.013(4) C802 0.082(5) 0.088(5) 0.063(5) -0.003(4) -0.007(4) -0.009(4) N900 0.077(4) 0.082(4) 0.074(4) -0.018(4) -0.014(4) 0.013(3) C901 0.045(4) 0.068(5) 0.084(6) -0.036(4) -0.026(4) 0.015(3) C902 0.076(5) 0.094(6) 0.084(6) -0.033(5) 0.010(4) -0.010(4) N10 0.103(5) 0.083(5) 0.149(7) -0.006(5) 0.032(5) 0.029(4) C11 0.064(4) 0.066(5) 0.098(6) -0.029(5) 0.008(4) 0.004(4) C12 0.112(7) 0.074(5) 0.099(6) -0.016(5) 0.003(5) -0.008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N301 1.968(4) . ? Fe1 N312 1.971(4) . ? Fe1 N101 1.978(4) . ? Fe1 N112 1.978(4) . ? Fe1 N212 1.980(4) . ? Fe1 N201 1.992(4) . ? Fe2 N329 1.965(4) . ? Fe2 N129 1.971(4) . ? Fe2 N126 1.973(4) . ? Fe2 N226 1.975(4) . ? Fe2 N326 1.978(4) . ? Fe2 N229 2.004(4) . ? N101 C110 1.339(6) . ? N101 C102 1.366(6) . ? C102 C103 1.366(7) . ? C102 H10A 0.9500 . ? C103 C104 1.408(7) . ? C103 H10B 0.9500 . ? C104 C105 1.416(7) . ? C104 C109 1.434(7) . ? C105 C106 1.351(7) . ? C105 H10C 0.9500 . ? C106 C107 1.424(8) . ? C106 H10D 0.9500 . ? C107 C108 1.350(7) . ? C107 H10E 0.9500 . ? C108 C109 1.417(7) . ? C108 H10F 0.9500 . ? C109 C110 1.418(7) . ? C110 C111 1.453(7) . ? C111 N112 1.294(6) . ? C111 H11A 0.9500 . ? N112 C113 1.440(6) . ? C113 C114 1.369(7) . ? C113 C118 1.401(7) . ? C114 C115 1.390(7) . ? C114 H11B 0.9500 . ? C115 C116 1.379(7) . ? C115 H11C 0.9500 . ? C116 C117 1.388(7) . ? C116 C119 1.519(7) . ? C117 C118 1.378(7) . ? C117 H11D 0.9500 . ? C118 H11E 0.9500 . ? C119 C120 1.525(7) . ? C119 H11F 0.9900 . ? C119 H11G 0.9900 . ? C120 C121 1.382(7) . ? C120 C125 1.391(7) . ? C121 C122 1.391(7) . ? C121 H12A 0.9500 . ? C122 C123 1.385(7) . ? C122 H12B 0.9500 . ? C123 C124 1.384(7) . ? C123 N126 1.453(6) . ? C124 C125 1.380(7) . ? C124 H12C 0.9500 . ? C125 H12D 0.9500 . ? N126 C127 1.290(6) . ? C127 C128 1.445(7) . ? C127 H12E 0.9500 . ? C128 N129 1.358(6) . ? C128 C137 1.418(7) . ? N129 C130 1.361(6) . ? C130 C131 1.365(7) . ? C130 H13A 0.9500 . ? C131 C132 1.401(7) . ? C131 H13B 0.9500 . ? C132 C133 1.410(7) . ? C132 C137 1.419(7) . ? C133 C134 1.364(8) . ? C133 H13C 0.9500 . ? C134 C135 1.406(8) . ? C134 H13D 0.9500 . ? C135 C136 1.380(7) . ? C135 H13E 0.9500 . ? C136 C137 1.412(7) . ? C136 H13F 0.9500 . ? N201 C210 1.342(7) . ? N201 C202 1.354(6) . ? C202 C203 1.373(8) . ? C202 H20A 0.9500 . ? C203 C204 1.410(9) . ? C203 H20B 0.9500 . ? C204 C209 1.399(8) . ? C204 C205 1.437(9) . ? C205 C206 1.318(10) . ? C205 H20C 0.9500 . ? C206 C207 1.388(10) . ? C206 H20D 0.9500 . ? C207 C208 1.371(8) . ? C207 H20E 0.9500 . ? C208 C209 1.422(8) . ? C208 H20F 0.9500 . ? C209 C210 1.423(7) . ? C210 C211 1.443(7) . ? C211 N212 1.291(6) . ? C211 H21A 0.9500 . ? N212 C213 1.441(6) . ? C213 C214 1.381(7) . ? C213 C218 1.400(7) . ? C214 C215 1.379(7) . ? C214 H21B 0.9500 . ? C215 C216 1.378(7) . ? C215 H21C 0.9500 . ? C216 C217 1.390(7) . ? C216 C219 1.531(7) . ? C217 C218 1.377(6) . ? C217 H21D 0.9500 . ? C218 H21E 0.9500 . ? C219 C220 1.507(6) . ? C219 H21F 0.9900 . ? C219 H21G 0.9900 . ? C220 C225 1.379(7) . ? C220 C221 1.382(7) . ? C221 C222 1.392(7) . ? C221 H22A 0.9500 . ? C222 C223 1.391(7) . ? C222 H22B 0.9500 . ? C223 C224 1.393(7) . ? C223 N226 1.439(6) . ? C224 C225 1.393(6) . ? C224 H22C 0.9500 . ? C225 H22D 0.9500 . ? N226 C227 1.287(6) . ? C227 C228 1.453(6) . ? C227 H22E 0.9500 . ? C228 N229 1.350(6) . ? C228 C237 1.423(7) . ? N229 C230 1.371(6) . ? C230 C231 1.358(7) . ? C230 H23A 0.9500 . ? C231 C232 1.409(7) . ? C231 H23B 0.9500 . ? C232 C233 1.409(7) . ? C232 C237 1.428(6) . ? C233 C234 1.368(8) . ? C233 H23C 0.9500 . ? C234 C235 1.407(8) . ? C234 H23D 0.9500 . ? C235 C236 1.367(7) . ? C235 H23E 0.9500 . ? C236 C237 1.418(7) . ? C236 H23F 0.9500 . ? N301 C310 1.344(6) . ? N301 C302 1.368(6) . ? C302 C303 1.365(7) . ? C302 H30A 0.9500 . ? C303 C304 1.398(7) . ? C303 H30B 0.9500 . ? C304 C305 1.432(7) . ? C304 C309 1.439(7) . ? C305 C306 1.348(8) . ? C305 H30C 0.9500 . ? C306 C307 1.413(8) . ? C306 H30D 0.9500 . ? C307 C308 1.361(7) . ? C307 H30E 0.9500 . ? C308 C309 1.407(7) . ? C308 H30F 0.9500 . ? C309 C310 1.418(6) . ? C310 C311 1.459(6) . ? C311 N312 1.292(6) . ? C311 H31A 0.9500 . ? N312 C313 1.447(5) . ? C313 C314 1.391(6) . ? C313 C318 1.394(6) . ? C314 C315 1.386(6) . ? C314 H31B 0.9500 . ? C315 C316 1.379(6) . ? C315 H31C 0.9500 . ? C316 C317 1.382(6) . ? C316 C319 1.532(6) . ? C317 C318 1.386(6) . ? C317 H31D 0.9500 . ? C318 H31E 0.9500 . ? C319 C320 1.512(6) . ? C319 H31F 0.9900 . ? C319 H31G 0.9900 . ? C320 C321 1.360(7) . ? C320 C325 1.394(6) . ? C321 C322 1.382(7) . ? C321 H32A 0.9500 . ? C322 C323 1.392(7) . ? C322 H32B 0.9500 . ? C323 C324 1.368(7) . ? C323 N326 1.453(6) . ? C324 C325 1.384(7) . ? C324 H32C 0.9500 . ? C325 H32D 0.9500 . ? N326 C327 1.291(6) . ? C327 C328 1.460(7) . ? C327 H32E 0.9500 . ? C328 N329 1.340(6) . ? C328 C337 1.426(6) . ? N329 C330 1.366(6) . ? C330 C331 1.362(7) . ? C330 H33A 0.9500 . ? C331 C332 1.401(7) . ? C331 H33B 0.9500 . ? C332 C333 1.412(7) . ? C332 C337 1.431(7) . ? C333 C334 1.359(8) . ? C333 H33C 0.9500 . ? C334 C335 1.389(8) . ? C334 H33D 0.9500 . ? C335 C336 1.375(7) . ? C335 H33E 0.9500 . ? C336 C337 1.403(7) . ? C336 H33F 0.9500 . ? B10 F11 1.355(7) . ? B10 F13 1.366(7) . ? B10 F14 1.374(7) . ? B10 F12 1.377(8) . ? B20 F24 1.315(11) . ? B20 F23 1.320(11) . ? B20 F24A 1.355(13) . ? B20 F21 1.371(11) . ? B20 F23A 1.388(17) . ? B20 F22A 1.397(15) . ? B20 F21A 1.401(16) . ? B20 F22 1.406(14) . ? B30 F33 1.238(18) . ? B30 F34A 1.299(12) . ? B30 F32 1.310(11) . ? B30 F31 1.381(9) . ? B30 F33A 1.395(13) . ? B30 F32A 1.497(10) . ? B30 F34 1.600(14) . ? B40 F42 1.354(10) . ? B40 F43 1.356(10) . ? B40 F44 1.361(9) . ? B40 F41 1.362(9) . ? C21 C23 1.473(11) 2_666 ? C21 C22 1.567(12) . ? C21 H21H 0.9500 . ? C22 C23 1.344(11) . ? C22 H22I 0.9500 . ? C23 C21 1.473(11) 2_666 ? C23 H23J 0.9500 . ? C31 C32 1.420(17) . ? C31 C33 1.425(16) 2_775 ? C31 H31H 0.9500 . ? C32 C33 1.366(16) . ? C32 H32F 0.9500 . ? C33 C31 1.425(16) 2_775 ? C33 H33G 0.9500 . ? C401 C402 1.347(13) . ? C401 C406 1.383(13) . ? C401 H40A 0.9500 . ? C402 C403 1.368(12) . ? C402 H40B 0.9500 . ? C403 C404 1.351(11) . ? C403 H40C 0.9500 . ? C404 C405 1.324(11) . ? C404 H40D 0.9500 . ? C405 C406 1.373(12) . ? C405 H40E 0.9500 . ? C406 H40F 0.9500 . ? N600 C601 1.146(8) . ? C601 C602 1.479(9) . ? C602 H60A 0.9800 . ? C602 H60B 0.9800 . ? C602 H60C 0.9800 . ? C501 C502 1.335(17) . ? C501 C506 1.390(17) . ? C501 H50A 0.9500 . ? C502 C503 1.320(14) . ? C502 H50B 0.9500 . ? C503 C504 1.344(12) . ? C503 H50C 0.9500 . ? C504 C505 1.406(14) . ? C504 H50D 0.9500 . ? C505 C506 1.388(15) . ? C505 H50E 0.9500 . ? C506 H50F 0.9500 . ? N700 C701 1.118(7) . ? C701 C702 1.471(9) . ? C702 H70A 0.9800 . ? C702 H70B 0.9800 . ? C702 H70C 0.9800 . ? N800 C801 1.132(9) . ? C801 C802 1.430(10) . ? C802 H80A 0.9800 . ? C802 H80B 0.9800 . ? C802 H80C 0.9800 . ? N900 C901 1.144(8) . ? C901 C902 1.460(11) . ? C902 H90A 0.9800 . ? C902 H90B 0.9800 . ? C902 H90C 0.9800 . ? N10 C11 1.124(9) . ? C11 C12 1.418(11) . ? C12 H12F 0.9800 . ? C12 H12G 0.9800 . ? C12 H12H 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N301 Fe1 N312 80.61(16) . . ? N301 Fe1 N101 93.65(16) . . ? N312 Fe1 N101 91.33(16) . . ? N301 Fe1 N112 174.03(17) . . ? N312 Fe1 N112 98.98(15) . . ? N101 Fe1 N112 80.40(16) . . ? N301 Fe1 N212 92.60(16) . . ? N312 Fe1 N212 96.50(16) . . ? N101 Fe1 N212 170.69(17) . . ? N112 Fe1 N212 93.36(16) . . ? N301 Fe1 N201 96.19(16) . . ? N312 Fe1 N201 175.00(16) . . ? N101 Fe1 N201 92.72(17) . . ? N112 Fe1 N201 84.60(15) . . ? N212 Fe1 N201 79.74(18) . . ? N329 Fe2 N129 94.40(16) . . ? N329 Fe2 N126 89.91(16) . . ? N129 Fe2 N126 80.45(16) . . ? N329 Fe2 N226 169.25(16) . . ? N129 Fe2 N226 92.10(16) . . ? N126 Fe2 N226 99.62(16) . . ? N329 Fe2 N326 80.48(16) . . ? N129 Fe2 N326 174.43(16) . . ? N126 Fe2 N326 97.27(16) . . ? N226 Fe2 N326 93.29(15) . . ? N329 Fe2 N229 90.60(16) . . ? N129 Fe2 N229 95.13(16) . . ? N126 Fe2 N229 175.57(16) . . ? N226 Fe2 N229 80.29(16) . . ? N326 Fe2 N229 87.15(15) . . ? C110 N101 C102 119.1(4) . . ? C110 N101 Fe1 114.8(3) . . ? C102 N101 Fe1 126.0(3) . . ? N101 C102 C103 121.8(5) . . ? N101 C102 H10A 119.1 . . ? C103 C102 H10A 119.1 . . ? C102 C103 C104 121.0(5) . . ? C102 C103 H10B 119.5 . . ? C104 C103 H10B 119.5 . . ? C103 C104 C105 123.3(5) . . ? C103 C104 C109 117.5(5) . . ? C105 C104 C109 119.1(4) . . ? C106 C105 C104 120.5(5) . . ? C106 C105 H10C 119.7 . . ? C104 C105 H10C 119.7 . . ? C105 C106 C107 120.2(5) . . ? C105 C106 H10D 119.9 . . ? C107 C106 H10D 119.9 . . ? C108 C107 C106 121.3(5) . . ? C108 C107 H10E 119.4 . . ? C106 C107 H10E 119.4 . . ? C107 C108 C109 120.2(5) . . ? C107 C108 H10F 119.9 . . ? C109 C108 H10F 119.9 . . ? C108 C109 C110 124.0(5) . . ? C108 C109 C104 118.7(5) . . ? C110 C109 C104 117.4(4) . . ? N101 C110 C109 123.0(4) . . ? N101 C110 C111 113.1(4) . . ? C109 C110 C111 123.9(4) . . ? N112 C111 C110 116.3(4) . . ? N112 C111 H11A 121.9 . . ? C110 C111 H11A 121.9 . . ? C111 N112 C113 116.9(4) . . ? C111 N112 Fe1 114.6(3) . . ? C113 N112 Fe1 127.6(3) . . ? C114 C113 C118 119.2(5) . . ? C114 C113 N112 120.7(5) . . ? C118 C113 N112 120.1(4) . . ? C113 C114 C115 120.0(5) . . ? C113 C114 H11B 120.0 . . ? C115 C114 H11B 120.0 . . ? C116 C115 C114 122.0(5) . . ? C116 C115 H11C 119.0 . . ? C114 C115 H11C 119.0 . . ? C115 C116 C117 117.1(5) . . ? C115 C116 C119 122.8(4) . . ? C117 C116 C119 120.1(5) . . ? C118 C117 C116 122.0(5) . . ? C118 C117 H11D 119.0 . . ? C116 C117 H11D 119.0 . . ? C117 C118 C113 119.6(4) . . ? C117 C118 H11E 120.2 . . ? C113 C118 H11E 120.2 . . ? C116 C119 C120 114.3(4) . . ? C116 C119 H11F 108.7 . . ? C120 C119 H11F 108.7 . . ? C116 C119 H11G 108.7 . . ? C120 C119 H11G 108.7 . . ? H11F C119 H11G 107.6 . . ? C121 C120 C125 118.8(5) . . ? C121 C120 C119 120.1(5) . . ? C125 C120 C119 121.1(5) . . ? C120 C121 C122 120.5(5) . . ? C120 C121 H12A 119.7 . . ? C122 C121 H12A 119.7 . . ? C123 C122 C121 120.0(5) . . ? C123 C122 H12B 120.0 . . ? C121 C122 H12B 120.0 . . ? C124 C123 C122 119.8(5) . . ? C124 C123 N126 121.2(4) . . ? C122 C123 N126 119.0(4) . . ? C125 C124 C123 120.0(5) . . ? C125 C124 H12C 120.0 . . ? C123 C124 H12C 120.0 . . ? C124 C125 C120 120.9(5) . . ? C124 C125 H12D 119.5 . . ? C120 C125 H12D 119.5 . . ? C127 N126 C123 114.9(4) . . ? C127 N126 Fe2 115.1(3) . . ? C123 N126 Fe2 130.0(3) . . ? N126 C127 C128 116.7(5) . . ? N126 C127 H12E 121.6 . . ? C128 C127 H12E 121.6 . . ? N129 C128 C137 123.3(4) . . ? N129 C128 C127 112.5(4) . . ? C137 C128 C127 124.2(5) . . ? C128 N129 C130 117.8(4) . . ? C128 N129 Fe2 114.9(3) . . ? C130 N129 Fe2 127.3(4) . . ? N129 C130 C131 122.8(5) . . ? N129 C130 H13A 118.6 . . ? C131 C130 H13A 118.6 . . ? C130 C131 C132 120.5(5) . . ? C130 C131 H13B 119.7 . . ? C132 C131 H13B 119.7 . . ? C131 C132 C133 122.9(5) . . ? C131 C132 C137 118.5(5) . . ? C133 C132 C137 118.6(5) . . ? C134 C133 C132 121.5(5) . . ? C134 C133 H13C 119.2 . . ? C132 C133 H13C 119.2 . . ? C133 C134 C135 119.8(5) . . ? C133 C134 H13D 120.1 . . ? C135 C134 H13D 120.1 . . ? C136 C135 C134 120.6(6) . . ? C136 C135 H13E 119.7 . . ? C134 C135 H13E 119.7 . . ? C135 C136 C137 120.1(5) . . ? C135 C136 H13F 120.0 . . ? C137 C136 H13F 120.0 . . ? C136 C137 C128 123.5(5) . . ? C136 C137 C132 119.4(5) . . ? C128 C137 C132 117.1(5) . . ? C210 N201 C202 117.2(5) . . ? C210 N201 Fe1 115.0(3) . . ? C202 N201 Fe1 127.3(4) . . ? N201 C202 C203 122.0(6) . . ? N201 C202 H20A 119.0 . . ? C203 C202 H20A 119.0 . . ? C202 C203 C204 121.4(6) . . ? C202 C203 H20B 119.3 . . ? C204 C203 H20B 119.3 . . ? C209 C204 C203 117.5(6) . . ? C209 C204 C205 118.6(7) . . ? C203 C204 C205 123.9(6) . . ? C206 C205 C204 121.2(7) . . ? C206 C205 H20C 119.4 . . ? C204 C205 H20C 119.4 . . ? C205 C206 C207 120.7(7) . . ? C205 C206 H20D 119.6 . . ? C207 C206 H20D 119.6 . . ? C208 C207 C206 121.1(7) . . ? C208 C207 H20E 119.5 . . ? C206 C207 H20E 119.5 . . ? C207 C208 C209 119.7(6) . . ? C207 C208 H20F 120.2 . . ? C209 C208 H20F 120.2 . . ? C204 C209 C208 118.7(6) . . ? C204 C209 C210 117.1(6) . . ? C208 C209 C210 124.2(5) . . ? N201 C210 C209 124.6(5) . . ? N201 C210 C211 111.7(5) . . ? C209 C210 C211 123.7(5) . . ? N212 C211 C210 117.9(5) . . ? N212 C211 H21A 121.1 . . ? C210 C211 H21A 121.1 . . ? C211 N212 C213 116.0(4) . . ? C211 N212 Fe1 114.3(3) . . ? C213 N212 Fe1 129.6(3) . . ? C214 C213 C218 119.5(5) . . ? C214 C213 N212 120.2(4) . . ? C218 C213 N212 120.2(4) . . ? C215 C214 C213 120.0(5) . . ? C215 C214 H21B 120.0 . . ? C213 C214 H21B 120.0 . . ? C216 C215 C214 121.1(5) . . ? C216 C215 H21C 119.5 . . ? C214 C215 H21C 119.5 . . ? C215 C216 C217 119.0(5) . . ? C215 C216 C219 120.3(5) . . ? C217 C216 C219 120.6(5) . . ? C218 C217 C216 120.6(5) . . ? C218 C217 H21D 119.7 . . ? C216 C217 H21D 119.7 . . ? C217 C218 C213 119.8(5) . . ? C217 C218 H21E 120.1 . . ? C213 C218 H21E 120.1 . . ? C220 C219 C216 111.3(4) . . ? C220 C219 H21F 109.4 . . ? C216 C219 H21F 109.4 . . ? C220 C219 H21G 109.4 . . ? C216 C219 H21G 109.4 . . ? H21F C219 H21G 108.0 . . ? C225 C220 C221 118.2(4) . . ? C225 C220 C219 120.3(5) . . ? C221 C220 C219 121.4(5) . . ? C220 C221 C222 121.9(5) . . ? C220 C221 H22A 119.0 . . ? C222 C221 H22A 119.0 . . ? C223 C222 C221 118.7(5) . . ? C223 C222 H22B 120.6 . . ? C221 C222 H22B 120.6 . . ? C222 C223 C224 120.6(4) . . ? C222 C223 N226 119.6(4) . . ? C224 C223 N226 119.7(4) . . ? C223 C224 C225 118.7(5) . . ? C223 C224 H22C 120.7 . . ? C225 C224 H22C 120.7 . . ? C220 C225 C224 121.9(5) . . ? C220 C225 H22D 119.0 . . ? C224 C225 H22D 119.0 . . ? C227 N226 C223 116.2(4) . . ? C227 N226 Fe2 114.7(3) . . ? C223 N226 Fe2 129.1(3) . . ? N226 C227 C228 117.8(4) . . ? N226 C227 H22E 121.1 . . ? C228 C227 H22E 121.1 . . ? N229 C228 C237 123.2(4) . . ? N229 C228 C227 112.2(4) . . ? C237 C228 C227 124.6(4) . . ? C228 N229 C230 118.2(4) . . ? C228 N229 Fe2 114.2(3) . . ? C230 N229 Fe2 127.5(3) . . ? C231 C230 N229 121.7(5) . . ? C231 C230 H23A 119.2 . . ? N229 C230 H23A 119.2 . . ? C230 C231 C232 122.4(5) . . ? C230 C231 H23B 118.8 . . ? C232 C231 H23B 118.8 . . ? C231 C232 C233 124.1(5) . . ? C231 C232 C237 116.5(5) . . ? C233 C232 C237 119.4(5) . . ? C234 C233 C232 120.4(5) . . ? C234 C233 H23C 119.8 . . ? C232 C233 H23C 119.8 . . ? C233 C234 C235 120.5(5) . . ? C233 C234 H23D 119.7 . . ? C235 C234 H23D 119.7 . . ? C236 C235 C234 120.6(5) . . ? C236 C235 H23E 119.7 . . ? C234 C235 H23E 119.7 . . ? C235 C236 C237 120.5(5) . . ? C235 C236 H23F 119.7 . . ? C237 C236 H23F 119.7 . . ? C236 C237 C228 123.5(4) . . ? C236 C237 C232 118.5(5) . . ? C228 C237 C232 117.9(5) . . ? C310 N301 C302 118.9(4) . . ? C310 N301 Fe1 115.4(3) . . ? C302 N301 Fe1 125.7(3) . . ? C303 C302 N301 121.0(5) . . ? C303 C302 H30A 119.5 . . ? N301 C302 H30A 119.5 . . ? C302 C303 C304 121.7(5) . . ? C302 C303 H30B 119.1 . . ? C304 C303 H30B 119.1 . . ? C303 C304 C305 123.9(5) . . ? C303 C304 C309 118.3(5) . . ? C305 C304 C309 117.8(5) . . ? C306 C305 C304 121.0(5) . . ? C306 C305 H30C 119.5 . . ? C304 C305 H30C 119.5 . . ? C305 C306 C307 120.5(5) . . ? C305 C306 H30D 119.8 . . ? C307 C306 H30D 119.8 . . ? C308 C307 C306 120.9(5) . . ? C308 C307 H30E 119.5 . . ? C306 C307 H30E 119.5 . . ? C307 C308 C309 120.4(5) . . ? C307 C308 H30F 119.8 . . ? C309 C308 H30F 119.8 . . ? C308 C309 C310 124.9(4) . . ? C308 C309 C304 119.3(4) . . ? C310 C309 C304 115.7(5) . . ? N301 C310 C309 124.2(4) . . ? N301 C310 C311 112.4(4) . . ? C309 C310 C311 123.4(4) . . ? N312 C311 C310 116.4(4) . . ? N312 C311 H31A 121.8 . . ? C310 C311 H31A 121.8 . . ? C311 N312 C313 117.3(4) . . ? C311 N312 Fe1 115.1(3) . . ? C313 N312 Fe1 127.5(3) . . ? C314 C313 C318 119.6(4) . . ? C314 C313 N312 120.0(4) . . ? C318 C313 N312 120.4(4) . . ? C315 C314 C313 120.0(4) . . ? C315 C314 H31B 120.0 . . ? C313 C314 H31B 120.0 . . ? C316 C315 C314 121.0(4) . . ? C316 C315 H31C 119.5 . . ? C314 C315 H31C 119.5 . . ? C315 C316 C317 118.5(4) . . ? C315 C316 C319 120.8(4) . . ? C317 C316 C319 120.7(4) . . ? C316 C317 C318 121.9(4) . . ? C316 C317 H31D 119.1 . . ? C318 C317 H31D 119.1 . . ? C317 C318 C313 119.0(4) . . ? C317 C318 H31E 120.5 . . ? C313 C318 H31E 120.5 . . ? C320 C319 C316 116.0(4) . . ? C320 C319 H31F 108.3 . . ? C316 C319 H31F 108.3 . . ? C320 C319 H31G 108.3 . . ? C316 C319 H31G 108.3 . . ? H31F C319 H31G 107.4 . . ? C321 C320 C325 116.8(5) . . ? C321 C320 C319 123.5(4) . . ? C325 C320 C319 119.7(4) . . ? C320 C321 C322 123.1(5) . . ? C320 C321 H32A 118.4 . . ? C322 C321 H32A 118.4 . . ? C321 C322 C323 119.6(5) . . ? C321 C322 H32B 120.2 . . ? C323 C322 H32B 120.2 . . ? C324 C323 C322 118.1(5) . . ? C324 C323 N326 121.7(4) . . ? C322 C323 N326 120.2(4) . . ? C323 C324 C325 121.4(5) . . ? C323 C324 H32C 119.3 . . ? C325 C324 H32C 119.3 . . ? C324 C325 C320 120.9(5) . . ? C324 C325 H32D 119.5 . . ? C320 C325 H32D 119.5 . . ? C327 N326 C323 117.5(4) . . ? C327 N326 Fe2 114.7(3) . . ? C323 N326 Fe2 127.5(3) . . ? N326 C327 C328 116.3(4) . . ? N326 C327 H32E 121.9 . . ? C328 C327 H32E 121.9 . . ? N329 C328 C337 122.3(4) . . ? N329 C328 C327 112.5(4) . . ? C337 C328 C327 125.1(4) . . ? C328 N329 C330 119.0(4) . . ? C328 N329 Fe2 115.2(3) . . ? C330 N329 Fe2 125.4(3) . . ? C331 C330 N329 122.4(5) . . ? C331 C330 H33A 118.8 . . ? N329 C330 H33A 118.8 . . ? C330 C331 C332 120.9(5) . . ? C330 C331 H33B 119.6 . . ? C332 C331 H33B 119.6 . . ? C331 C332 C333 122.9(5) . . ? C331 C332 C337 117.6(4) . . ? C333 C332 C337 119.5(5) . . ? C334 C333 C332 119.6(5) . . ? C334 C333 H33C 120.2 . . ? C332 C333 H33C 120.2 . . ? C333 C334 C335 121.1(5) . . ? C333 C334 H33D 119.4 . . ? C335 C334 H33D 119.4 . . ? C336 C335 C334 121.2(5) . . ? C336 C335 H33E 119.4 . . ? C334 C335 H33E 119.4 . . ? C335 C336 C337 119.7(5) . . ? C335 C336 H33F 120.2 . . ? C337 C336 H33F 120.2 . . ? C336 C337 C328 123.3(5) . . ? C336 C337 C332 118.9(5) . . ? C328 C337 C332 117.8(5) . . ? F11 B10 F13 111.4(6) . . ? F11 B10 F14 108.6(5) . . ? F13 B10 F14 109.4(5) . . ? F11 B10 F12 109.9(6) . . ? F13 B10 F12 108.3(5) . . ? F14 B10 F12 109.2(5) . . ? F24 B20 F23 119.9(10) . . ? F24 B20 F24A 72.0(9) . . ? F23 B20 F24A 160.9(12) . . ? F24 B20 F21 108.2(9) . . ? F23 B20 F21 94.0(9) . . ? F24A B20 F21 67.2(9) . . ? F24 B20 F23A 160(2) . . ? F23 B20 F23A 62.4(16) . . ? F24A B20 F23A 101.0(18) . . ? F21 B20 F23A 52.2(17) . . ? F24 B20 F22A 97.4(11) . . ? F23 B20 F22A 92.2(11) . . ? F24A B20 F22A 101.3(12) . . ? F21 B20 F22A 145.9(12) . . ? F23A B20 F22A 102.9(19) . . ? F24 B20 F21A 63.7(13) . . ? F23 B20 F21A 57.6(12) . . ? F24A B20 F21A 127.2(16) . . ? F21 B20 F21A 100.3(14) . . ? F23A B20 F21A 110.3(19) . . ? F22A B20 F21A 111.2(14) . . ? F24 B20 F22 115.0(14) . . ? F23 B20 F22 102.9(13) . . ? F24A B20 F22 82.9(12) . . ? F21 B20 F22 115.3(13) . . ? F23A B20 F22 82.3(18) . . ? F22A B20 F22 31.0(13) . . ? F21A B20 F22 141.2(16) . . ? F33 B30 F34A 107.2(14) . . ? F33 B30 F32 127.1(11) . . ? F34A B30 F32 70.0(8) . . ? F33 B30 F31 118.4(11) . . ? F34A B30 F31 117.3(11) . . ? F32 B30 F31 107.6(7) . . ? F33 B30 F33A 4.7(15) . . ? F34A B30 F33A 111.6(11) . . ? F32 B30 F33A 129.4(11) . . ? F31 B30 F33A 114.1(9) . . ? F33 B30 F32A 101.2(11) . . ? F34A B30 F32A 105.4(9) . . ? F32 B30 F32A 39.0(5) . . ? F31 B30 F32A 105.4(6) . . ? F33A B30 F32A 101.1(10) . . ? F33 B30 F34 100.7(11) . . ? F34A B30 F34 33.4(7) . . ? F32 B30 F34 100.0(8) . . ? F31 B30 F34 94.9(7) . . ? F33A B30 F34 103.5(8) . . ? F32A B30 F34 138.0(7) . . ? F42 B40 F43 109.1(7) . . ? F42 B40 F44 111.5(7) . . ? F43 B40 F44 111.1(8) . . ? F42 B40 F41 110.3(8) . . ? F43 B40 F41 103.6(7) . . ? F44 B40 F41 110.8(7) . . ? C23 C21 C22 123.5(9) 2_666 . ? C23 C21 H21H 118.2 2_666 . ? C22 C21 H21H 118.2 . . ? C23 C22 C21 114.2(9) . . ? C23 C22 H22I 122.9 . . ? C21 C22 H22I 122.9 . . ? C22 C23 C21 121.8(9) . 2_666 ? C22 C23 H23J 119.1 . . ? C21 C23 H23J 119.1 2_666 . ? C32 C31 C33 125.2(9) . 2_775 ? C32 C31 H31H 117.5 . . ? C33 C31 H31H 117.3 2_775 . ? C33 C32 C31 115.5(13) . . ? C33 C32 H32F 122.3 . . ? C31 C32 H32F 122.3 . . ? C32 C33 C31 119.3(13) . 2_775 ? C32 C33 H33G 120.3 . . ? C31 C33 H33G 120.3 2_775 . ? C402 C401 C406 118.3(10) . . ? C402 C401 H40A 120.9 . . ? C406 C401 H40A 120.9 . . ? C401 C402 C403 121.8(10) . . ? C401 C402 H40B 119.1 . . ? C403 C402 H40B 119.1 . . ? C404 C403 C402 118.1(10) . . ? C404 C403 H40C 121.0 . . ? C402 C403 H40C 121.0 . . ? C405 C404 C403 122.4(9) . . ? C405 C404 H40D 118.8 . . ? C403 C404 H40D 118.8 . . ? C404 C405 C406 119.4(8) . . ? C404 C405 H40E 120.3 . . ? C406 C405 H40E 120.3 . . ? C405 C406 C401 119.9(10) . . ? C405 C406 H40F 120.0 . . ? C401 C406 H40F 120.0 . . ? N600 C601 C602 179.7(8) . . ? C601 C602 H60A 109.5 . . ? C601 C602 H60B 109.5 . . ? H60A C602 H60B 109.5 . . ? C601 C602 H60C 109.5 . . ? H60A C602 H60C 109.5 . . ? H60B C602 H60C 109.5 . . ? C502 C501 C506 122.4(14) . . ? C502 C501 H50A 118.8 . . ? C506 C501 H50A 118.8 . . ? C503 C502 C501 121.6(13) . . ? C503 C502 H50B 119.2 . . ? C501 C502 H50B 119.2 . . ? C502 C503 C504 120.2(12) . . ? C502 C503 H50C 119.9 . . ? C504 C503 H50C 119.9 . . ? C503 C504 C505 120.1(10) . . ? C503 C504 H50D 119.9 . . ? C505 C504 H50D 119.9 . . ? C506 C505 C504 119.8(11) . . ? C506 C505 H50E 120.1 . . ? C504 C505 H50E 120.1 . . ? C505 C506 C501 115.9(13) . . ? C505 C506 H50F 122.0 . . ? C501 C506 H50F 122.0 . . ? N700 C701 C702 178.0(7) . . ? C701 C702 H70A 109.5 . . ? C701 C702 H70B 109.5 . . ? H70A C702 H70B 109.5 . . ? C701 C702 H70C 109.5 . . ? H70A C702 H70C 109.5 . . ? H70B C702 H70C 109.5 . . ? N800 C801 C802 177.4(9) . . ? C801 C802 H80A 109.5 . . ? C801 C802 H80B 109.5 . . ? H80A C802 H80B 109.5 . . ? C801 C802 H80C 109.5 . . ? H80A C802 H80C 109.5 . . ? H80B C802 H80C 109.5 . . ? N900 C901 C902 179.4(8) . . ? C901 C902 H90A 109.5 . . ? C901 C902 H90B 109.5 . . ? H90A C902 H90B 109.5 . . ? C901 C902 H90C 109.5 . . ? H90A C902 H90C 109.5 . . ? H90B C902 H90C 109.5 . . ? N10 C11 C12 177.2(10) . . ? C11 C12 H12F 109.5 . . ? C11 C12 H12G 109.5 . . ? H12F C12 H12G 109.5 . . ? C11 C12 H12H 109.5 . . ? H12F C12 H12H 109.5 . . ? H12G C12 H12H 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.085 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.072 # Attachment 'mp6 2.cif' data_mp6 _database_code_depnum_ccdc_archive 'CCDC 292899' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69.50 H52 Ag2 F12 N8 O0.50 P2' _chemical_formula_weight 1512.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.620(4) _cell_length_b 11.942(5) _cell_length_c 13.638(5) _cell_angle_alpha 84.576(8) _cell_angle_beta 69.772(8) _cell_angle_gamma 85.742(9) _cell_volume 1766.1(12) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 3717 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 26.10 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 761 _exptl_absorpt_coefficient_mu 0.677 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8118 _exptl_absorpt_correction_T_max 0.9734 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique Set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(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 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 10961 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.1405 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 29.01 _reflns_number_total 7986 _reflns_number_gt 3817 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^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 7986 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1504 _refine_ls_R_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.1736 _refine_ls_wR_factor_gt 0.1424 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_restrained_S_all 0.917 _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 Ag1 Ag 0.82062(4) 0.25960(5) 0.71934(4) 0.0517(2) Uani 1 1 d . . . N1 N 0.8041(4) 0.3154(4) 0.8804(3) 0.0425(12) Uani 1 1 d . . . C2 C 0.8997(5) 0.3165(6) 0.9163(5) 0.0482(16) Uani 1 1 d . . . H2A H 0.9801 0.2999 0.8696 0.058 Uiso 1 1 calc R . . C3 C 0.8864(6) 0.3398(6) 1.0145(5) 0.0543(17) Uani 1 1 d . . . H3A H 0.9559 0.3401 1.0359 0.065 Uiso 1 1 calc R . . C4 C 0.7667(6) 0.3640(5) 1.0856(5) 0.0450(15) Uani 1 1 d . . . C5 C 0.7442(7) 0.3885(6) 1.1899(5) 0.0592(19) Uani 1 1 d . . . H5A H 0.8116 0.3903 1.2139 0.071 Uiso 1 1 calc R . . C6 C 0.6298(7) 0.4094(6) 1.2562(5) 0.064(2) Uani 1 1 d . . . H6A H 0.6172 0.4256 1.3261 0.077 Uiso 1 1 calc R . . C7 C 0.5305(7) 0.4072(6) 1.2225(5) 0.0592(18) Uani 1 1 d . . . H7A H 0.4501 0.4224 1.2698 0.071 Uiso 1 1 calc R . . C8 C 0.5463(6) 0.3832(5) 1.1218(4) 0.0475(16) Uani 1 1 d . . . H8A H 0.4770 0.3816 1.1002 0.057 Uiso 1 1 calc R . . C9 C 0.6650(5) 0.3612(4) 1.0511(4) 0.0337(13) Uani 1 1 d . . . C10 C 0.6910(5) 0.3364(5) 0.9454(4) 0.0367(13) Uani 1 1 d . . . C11 C 0.5917(5) 0.3347(5) 0.8998(4) 0.0374(14) Uani 1 1 d . . . H11A H 0.5103 0.3583 0.9394 0.045 Uiso 1 1 calc R . . N12 N 0.6145(4) 0.3020(4) 0.8089(3) 0.0349(11) Uani 1 1 d . . . C13 C 0.5174(5) 0.2981(4) 0.7681(4) 0.0326(13) Uani 1 1 d . . . C14 C 0.4007(5) 0.2695(5) 0.8288(4) 0.0409(14) Uani 1 1 d . . . H14A H 0.3798 0.2565 0.9026 0.049 Uiso 1 1 calc R . . C15 C 0.3130(5) 0.2594(5) 0.7822(4) 0.0457(16) Uani 1 1 d . . . H15A H 0.2327 0.2388 0.8250 0.055 Uiso 1 1 calc R . . C16 C 0.3398(5) 0.2785(5) 0.6753(5) 0.0376(13) Uani 1 1 d . . . C17 C 0.4573(5) 0.3098(5) 0.6152(4) 0.0391(14) Uani 1 1 d . . . H17A H 0.4772 0.3263 0.5419 0.047 Uiso 1 1 calc R . . C18 C 0.5462(5) 0.3176(5) 0.6601(4) 0.0386(14) Uani 1 1 d . . . H18A H 0.6271 0.3362 0.6172 0.046 Uiso 1 1 calc R . . C19 C 0.2457(5) 0.2640(5) 0.6245(5) 0.0434(15) Uani 1 1 d . . . H19A H 0.2815 0.2135 0.5669 0.052 Uiso 1 1 calc R . . H19B H 0.1739 0.2274 0.6768 0.052 Uiso 1 1 calc R . . C20 C 0.2033(5) 0.3736(5) 0.5813(4) 0.0354(13) Uani 1 1 d . . . C21 C 0.2289(5) 0.3977(5) 0.4751(4) 0.0391(14) Uani 1 1 d . . . H21A H 0.2750 0.3436 0.4284 0.047 Uiso 1 1 calc R . . C22 C 0.1898(5) 0.4978(5) 0.4343(4) 0.0371(14) Uani 1 1 d . . . H22A H 0.2074 0.5111 0.3609 0.045 Uiso 1 1 calc R . . C23 C 0.1245(5) 0.5788(5) 0.5016(4) 0.0342(13) Uani 1 1 d . . . C24 C 0.0995(5) 0.5564(5) 0.6096(4) 0.0419(15) Uani 1 1 d . . . H24A H 0.0565 0.6111 0.6570 0.050 Uiso 1 1 calc R . . C25 C 0.1375(5) 0.4553(5) 0.6461(4) 0.0425(15) Uani 1 1 d . . . H25A H 0.1178 0.4404 0.7196 0.051 Uiso 1 1 calc R . . N26 N 0.0883(4) 0.6807(4) 0.4555(3) 0.0337(11) Uani 1 1 d . . . C27 C 0.0065(5) 0.7480(5) 0.5083(4) 0.0346(13) Uani 1 1 d . . . H27A H -0.0316 0.7311 0.5815 0.042 Uiso 1 1 calc R . . C28 C -0.0305(5) 0.8514(5) 0.4589(4) 0.0363(14) Uani 1 1 d . . . N29 N 0.0407(4) 0.8804(4) 0.3605(4) 0.0432(12) Uani 1 1 d . . . C30 C 0.0087(6) 0.9756(6) 0.3108(5) 0.0494(16) Uani 1 1 d . . . H30A H 0.0603 0.9970 0.2416 0.059 Uiso 1 1 calc R . . C31 C -0.0931(6) 1.0412(5) 0.3550(5) 0.0496(16) Uani 1 1 d . . . H31A H -0.1118 1.1059 0.3161 0.059 Uiso 1 1 calc R . . C32 C -0.1713(5) 1.0141(5) 0.4581(5) 0.0422(15) Uani 1 1 d . . . C33 C -0.2790(6) 1.0764(6) 0.5087(6) 0.0610(19) Uani 1 1 d . . . H33A H -0.3021 1.1419 0.4734 0.073 Uiso 1 1 calc R . . C34 C -0.3507(7) 1.0440(6) 0.6079(7) 0.072(2) Uani 1 1 d . . . H34A H -0.4242 1.0866 0.6406 0.087 Uiso 1 1 calc R . . C35 C -0.3192(6) 0.9508(6) 0.6622(5) 0.0615(19) Uani 1 1 d . . . H35A H -0.3703 0.9302 0.7319 0.074 Uiso 1 1 calc R . . C36 C -0.2159(6) 0.8886(5) 0.6168(5) 0.0477(16) Uani 1 1 d . . . H36A H -0.1948 0.8245 0.6551 0.057 Uiso 1 1 calc R . . C37 C -0.1383(5) 0.9172(5) 0.5132(4) 0.0367(13) Uani 1 1 d . . . P10 P 0.18109(14) 0.32069(14) 0.13539(12) 0.0415(4) Uani 1 1 d . . . F11 F 0.0796(3) 0.2411(3) 0.2132(3) 0.0694(11) Uani 1 1 d . . . F12 F 0.2832(3) 0.4015(3) 0.0582(3) 0.0634(10) Uani 1 1 d . . . F13 F 0.1584(3) 0.2758(3) 0.0379(3) 0.0628(10) Uani 1 1 d . . . F14 F 0.2042(4) 0.3637(3) 0.2341(3) 0.0679(11) Uani 1 1 d . . . F15 F 0.0770(3) 0.4162(3) 0.1434(3) 0.0620(10) Uani 1 1 d . . . F16 F 0.2855(3) 0.2251(3) 0.1282(3) 0.0651(10) Uani 1 1 d . . . O100 O 0.344(2) 0.9513(19) 0.8874(16) 0.079(6) Uiso 0.25 1 d P A 1 C101 C 0.229(4) 0.977(3) 0.993(3) 0.080(7) Uiso 0.25 1 d P A 1 C201 C 0.3898(16) 0.952(2) 0.9628(17) 0.120(14) Uiso 0.25 1 d PG B 2 C202 C 0.4042(14) 0.944(2) 0.8581(15) 0.080(7) Uiso 0.25 1 d PG B 2 C203 C 0.3020(18) 0.9519(18) 0.8267(11) 0.061(7) Uiso 0.25 1 d PG B 2 C204 C 0.1852(15) 0.9669(17) 0.9000(14) 0.057(7) Uiso 0.25 1 d PG B 2 C205 C 0.1708(15) 0.9743(18) 1.0048(13) 0.066(10) Uiso 0.25 1 d PG B 2 C206 C 0.2730(19) 0.9667(19) 1.0362(12) 0.052(7) Uiso 0.25 1 d PG B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0403(3) 0.0738(4) 0.0356(3) -0.0098(2) -0.0068(2) 0.0087(2) N1 0.034(3) 0.058(3) 0.035(3) -0.008(2) -0.011(2) 0.000(2) C2 0.029(3) 0.076(5) 0.046(4) -0.006(3) -0.020(3) -0.002(3) C3 0.038(4) 0.073(5) 0.059(4) -0.005(4) -0.024(3) -0.008(3) C4 0.047(4) 0.051(4) 0.044(3) -0.008(3) -0.023(3) -0.005(3) C5 0.060(5) 0.080(5) 0.055(4) -0.017(4) -0.039(4) 0.000(4) C6 0.080(6) 0.071(5) 0.049(4) -0.022(4) -0.028(4) 0.006(4) C7 0.058(5) 0.070(5) 0.046(4) -0.017(3) -0.009(3) 0.001(4) C8 0.044(4) 0.057(4) 0.041(3) -0.009(3) -0.013(3) 0.000(3) C9 0.036(3) 0.032(3) 0.034(3) -0.001(2) -0.012(3) -0.006(2) C10 0.032(3) 0.042(4) 0.037(3) -0.003(3) -0.012(3) 0.001(3) C11 0.030(3) 0.048(4) 0.034(3) -0.006(3) -0.012(3) 0.006(3) N12 0.028(3) 0.043(3) 0.036(3) -0.001(2) -0.014(2) 0.001(2) C13 0.028(3) 0.035(3) 0.037(3) -0.004(3) -0.015(3) 0.002(2) C14 0.035(3) 0.055(4) 0.031(3) -0.001(3) -0.010(3) 0.001(3) C15 0.033(3) 0.061(4) 0.040(3) -0.005(3) -0.007(3) -0.009(3) C16 0.034(3) 0.033(3) 0.047(3) -0.002(3) -0.016(3) 0.003(3) C17 0.042(4) 0.045(4) 0.032(3) -0.004(3) -0.014(3) 0.002(3) C18 0.032(3) 0.049(4) 0.034(3) -0.003(3) -0.010(3) -0.003(3) C19 0.041(4) 0.048(4) 0.047(3) -0.005(3) -0.020(3) -0.010(3) C20 0.032(3) 0.036(3) 0.046(3) -0.007(3) -0.022(3) -0.004(2) C21 0.025(3) 0.043(4) 0.044(3) -0.014(3) -0.004(3) 0.000(3) C22 0.028(3) 0.045(4) 0.033(3) -0.010(3) -0.001(2) -0.002(3) C23 0.024(3) 0.040(4) 0.040(3) -0.004(3) -0.012(2) -0.006(2) C24 0.038(3) 0.056(4) 0.031(3) -0.014(3) -0.010(3) 0.011(3) C25 0.042(4) 0.060(4) 0.029(3) -0.009(3) -0.016(3) 0.004(3) N26 0.029(3) 0.041(3) 0.032(2) -0.006(2) -0.012(2) 0.000(2) C27 0.029(3) 0.043(4) 0.033(3) -0.008(3) -0.010(3) -0.004(3) C28 0.031(3) 0.046(4) 0.039(3) -0.013(3) -0.018(3) -0.002(3) N29 0.038(3) 0.051(3) 0.040(3) -0.003(2) -0.013(2) -0.004(2) C30 0.049(4) 0.058(4) 0.042(3) 0.002(3) -0.017(3) -0.006(3) C31 0.049(4) 0.041(4) 0.061(4) 0.004(3) -0.023(3) -0.001(3) C32 0.038(4) 0.035(4) 0.057(4) -0.004(3) -0.019(3) 0.000(3) C33 0.062(5) 0.042(4) 0.077(5) 0.002(4) -0.024(4) 0.011(3) C34 0.049(5) 0.054(5) 0.097(6) -0.011(4) -0.004(4) 0.015(4) C35 0.048(4) 0.061(5) 0.055(4) -0.005(4) 0.004(3) 0.017(3) C36 0.048(4) 0.041(4) 0.051(4) -0.009(3) -0.013(3) 0.006(3) C37 0.036(3) 0.037(3) 0.044(3) -0.008(3) -0.020(3) -0.001(3) P10 0.0381(9) 0.0485(10) 0.0364(8) -0.0079(7) -0.0103(7) 0.0007(7) F11 0.062(3) 0.075(3) 0.059(2) 0.005(2) -0.006(2) -0.014(2) F12 0.050(2) 0.067(3) 0.065(2) 0.003(2) -0.0096(19) -0.0085(19) F13 0.051(2) 0.090(3) 0.050(2) -0.024(2) -0.0163(18) 0.001(2) F14 0.082(3) 0.079(3) 0.055(2) -0.019(2) -0.037(2) 0.002(2) F15 0.048(2) 0.068(3) 0.066(2) -0.013(2) -0.0163(19) 0.0192(18) F16 0.063(3) 0.058(2) 0.076(3) -0.008(2) -0.028(2) 0.0159(19) _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 Ag1 N1 2.295(4) . ? Ag1 N29 2.304(5) 2_666 ? Ag1 N26 2.315(4) 2_666 ? Ag1 N12 2.324(4) . ? N1 C10 1.328(6) . ? N1 C2 1.362(7) . ? C2 C3 1.348(8) . ? C2 H2A 0.9500 . ? C3 C4 1.421(8) . ? C3 H3A 0.9500 . ? C4 C5 1.410(8) . ? C4 C9 1.418(8) . ? C5 C6 1.345(9) . ? C5 H5A 0.9500 . ? C6 C7 1.385(9) . ? C6 H6A 0.9500 . ? C7 C8 1.376(8) . ? C7 H7A 0.9500 . ? C8 C9 1.406(8) . ? C8 H8A 0.9500 . ? C9 C10 1.423(7) . ? C10 C11 1.489(8) . ? C11 N12 1.268(6) . ? C11 H11A 0.9500 . ? N12 C13 1.425(6) . ? C13 C14 1.371(7) . ? C13 C18 1.393(7) . ? C14 C15 1.392(8) . ? C14 H14A 0.9500 . ? C15 C16 1.382(8) . ? C15 H15A 0.9500 . ? C16 C17 1.385(7) . ? C16 C19 1.510(8) . ? C17 C18 1.383(7) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.504(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C25 1.378(8) . ? C20 C21 1.380(7) . ? C21 C22 1.383(8) . ? C21 H21A 0.9500 . ? C22 C23 1.389(7) . ? C22 H22A 0.9500 . ? C23 C24 1.403(7) . ? C23 N26 1.420(7) . ? C24 C25 1.363(8) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? N26 C27 1.262(6) . ? N26 Ag1 2.315(4) 2_666 ? C27 C28 1.458(8) . ? C27 H27A 0.9500 . ? C28 N29 1.339(7) . ? C28 C37 1.435(8) . ? N29 C30 1.363(8) . ? N29 Ag1 2.304(5) 2_666 ? C30 C31 1.354(9) . ? C30 H30A 0.9500 . ? C31 C32 1.408(8) . ? C31 H31A 0.9500 . ? C32 C33 1.399(9) . ? C32 C37 1.422(8) . ? C33 C34 1.358(9) . ? C33 H33A 0.9500 . ? C34 C35 1.376(10) . ? C34 H34A 0.9500 . ? C35 C36 1.347(8) . ? C35 H35A 0.9500 . ? C36 C37 1.414(8) . ? C36 H36A 0.9500 . ? P10 F15 1.583(4) . ? P10 F16 1.587(4) . ? P10 F13 1.589(4) . ? P10 F11 1.591(4) . ? P10 F14 1.597(4) . ? P10 F12 1.600(4) . ? O100 C101 1.62(4) . ? C201 C202 1.3900 . ? C201 C206 1.3900 . ? C202 C203 1.3900 . ? C203 C204 1.3900 . ? C204 C205 1.3900 . ? C205 C206 1.3900 . ? 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 Ag1 N29 122.38(17) . 2_666 ? N1 Ag1 N26 138.23(16) . 2_666 ? N29 Ag1 N26 72.09(17) 2_666 2_666 ? N1 Ag1 N12 72.14(16) . . ? N29 Ag1 N12 144.17(16) 2_666 . ? N26 Ag1 N12 121.14(16) 2_666 . ? C10 N1 C2 118.8(5) . . ? C10 N1 Ag1 116.3(3) . . ? C2 N1 Ag1 124.5(4) . . ? C3 C2 N1 123.5(6) . . ? C3 C2 H2A 118.2 . . ? N1 C2 H2A 118.2 . . ? C2 C3 C4 119.0(6) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C5 C4 C9 118.4(6) . . ? C5 C4 C3 122.8(6) . . ? C9 C4 C3 118.8(5) . . ? C6 C5 C4 121.7(6) . . ? C6 C5 H5A 119.2 . . ? C4 C5 H5A 119.2 . . ? C5 C6 C7 120.0(6) . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C8 C7 C6 121.2(6) . . ? C8 C7 H7A 119.4 . . ? C6 C7 H7A 119.4 . . ? C7 C8 C9 119.8(6) . . ? C7 C8 H8A 120.1 . . ? C9 C8 H8A 120.1 . . ? C8 C9 C4 118.9(5) . . ? C8 C9 C10 124.1(5) . . ? C4 C9 C10 117.0(5) . . ? N1 C10 C9 122.9(5) . . ? N1 C10 C11 115.5(5) . . ? C9 C10 C11 121.6(5) . . ? N12 C11 C10 120.9(5) . . ? N12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 N12 C13 119.9(5) . . ? C11 N12 Ag1 114.7(4) . . ? C13 N12 Ag1 125.4(3) . . ? C14 C13 C18 119.3(5) . . ? C14 C13 N12 123.2(5) . . ? C18 C13 N12 117.4(5) . . ? C13 C14 C15 119.9(5) . . ? C13 C14 H14A 120.1 . . ? C15 C14 H14A 120.1 . . ? C16 C15 C14 121.7(5) . . ? C16 C15 H15A 119.2 . . ? C14 C15 H15A 119.2 . . ? C15 C16 C17 117.7(5) . . ? C15 C16 C19 121.6(5) . . ? C17 C16 C19 120.7(5) . . ? C18 C17 C16 121.2(5) . . ? C18 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? C17 C18 C13 120.2(5) . . ? C17 C18 H18A 119.9 . . ? C13 C18 H18A 119.9 . . ? C20 C19 C16 112.9(5) . . ? C20 C19 H19A 109.0 . . ? C16 C19 H19A 109.0 . . ? C20 C19 H19B 109.0 . . ? C16 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C25 C20 C21 116.7(5) . . ? C25 C20 C19 121.5(5) . . ? C21 C20 C19 121.7(5) . . ? C20 C21 C22 122.4(5) . . ? C20 C21 H21A 118.8 . . ? C22 C21 H21A 118.8 . . ? C21 C22 C23 119.4(5) . . ? C21 C22 H22A 120.3 . . ? C23 C22 H22A 120.3 . . ? C22 C23 C24 118.9(5) . . ? C22 C23 N26 117.1(5) . . ? C24 C23 N26 124.0(5) . . ? C25 C24 C23 119.4(5) . . ? C25 C24 H24A 120.3 . . ? C23 C24 H24A 120.3 . . ? C24 C25 C20 123.1(5) . . ? C24 C25 H25A 118.4 . . ? C20 C25 H25A 118.4 . . ? C27 N26 C23 122.0(5) . . ? C27 N26 Ag1 114.8(4) . 2_666 ? C23 N26 Ag1 123.1(3) . 2_666 ? N26 C27 C28 121.1(5) . . ? N26 C27 H27A 119.5 . . ? C28 C27 H27A 119.5 . . ? N29 C28 C37 122.2(5) . . ? N29 C28 C27 116.5(5) . . ? C37 C28 C27 121.3(5) . . ? C28 N29 C30 118.4(5) . . ? C28 N29 Ag1 114.3(4) . 2_666 ? C30 N29 Ag1 125.6(4) . 2_666 ? C31 C30 N29 123.4(6) . . ? C31 C30 H30A 118.3 . . ? N29 C30 H30A 118.3 . . ? C30 C31 C32 120.4(6) . . ? C30 C31 H31A 119.8 . . ? C32 C31 H31A 119.8 . . ? C33 C32 C31 123.9(6) . . ? C33 C32 C37 118.5(6) . . ? C31 C32 C37 117.6(5) . . ? C34 C33 C32 120.5(7) . . ? C34 C33 H33A 119.8 . . ? C32 C33 H33A 119.8 . . ? C33 C34 C35 121.4(7) . . ? C33 C34 H34A 119.3 . . ? C35 C34 H34A 119.3 . . ? C36 C35 C34 120.1(6) . . ? C36 C35 H35A 119.9 . . ? C34 C35 H35A 119.9 . . ? C35 C36 C37 121.1(6) . . ? C35 C36 H36A 119.4 . . ? C37 C36 H36A 119.4 . . ? C36 C37 C32 118.3(5) . . ? C36 C37 C28 123.7(5) . . ? C32 C37 C28 117.9(5) . . ? F15 P10 F16 179.6(2) . . ? F15 P10 F13 90.3(2) . . ? F16 P10 F13 90.1(2) . . ? F15 P10 F11 88.6(2) . . ? F16 P10 F11 91.3(2) . . ? F13 P10 F11 90.3(2) . . ? F15 P10 F14 90.4(2) . . ? F16 P10 F14 89.2(2) . . ? F13 P10 F14 179.0(2) . . ? F11 P10 F14 89.1(2) . . ? F15 P10 F12 91.2(2) . . ? F16 P10 F12 88.9(2) . . ? F13 P10 F12 90.3(2) . . ? F11 P10 F12 179.4(2) . . ? F14 P10 F12 90.3(2) . . ? C202 C201 C206 120.0 . . ? C201 C202 C203 120.0 . . ? C204 C203 C202 120.0 . . ? C203 C204 C205 120.0 . . ? C206 C205 C204 120.0 . . ? C205 C206 C201 120.0 . . ? _diffrn_measured_fraction_theta_max 0.850 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.796 _refine_diff_density_min -0.394 _refine_diff_density_rms 0.101 # Attachment 'mp8 2.cif' data_mp8 _database_code_depnum_ccdc_archive 'CCDC 292900' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H66 B2 Cu2 F8 N14' _chemical_formula_weight 1500.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.176(3) _cell_length_b 14.973(5) _cell_length_c 15.005(4) _cell_angle_alpha 116.654(6) _cell_angle_beta 96.444(6) _cell_angle_gamma 94.840(4) _cell_volume 1809.7(9) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 1943 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 0.663 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8881 _exptl_absorpt_correction_T_max 0.9489 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique Set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(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 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 9041 _diffrn_reflns_av_R_equivalents 0.1341 _diffrn_reflns_av_sigmaI/netI 0.4524 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6179 _reflns_number_gt 1770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0992P)^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 0.014(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6179 _refine_ls_number_parameters 473 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2788 _refine_ls_R_factor_gt 0.1122 _refine_ls_wR_factor_ref 0.2836 _refine_ls_wR_factor_gt 0.2308 _refine_ls_goodness_of_fit_ref 0.839 _refine_ls_restrained_S_all 0.839 _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 Cu1 Cu 0.50797(19) 0.28334(11) 0.72386(11) 0.0446(6) Uani 1 1 d . . . N1 N 0.6710(11) 0.3290(7) 0.8461(6) 0.038(3) Uani 1 1 d . . . C2 C 0.7574(14) 0.2754(9) 0.8742(9) 0.046(3) Uani 1 1 d . . . H2A H 0.7455 0.2047 0.8305 0.055 Uiso 1 1 calc R . . C3 C 0.8578(16) 0.3120(10) 0.9574(8) 0.061(4) Uani 1 1 d . . . H3A H 0.9216 0.2697 0.9683 0.073 Uiso 1 1 calc R . . C4 C 0.8693(14) 0.4129(11) 1.0288(10) 0.053(4) Uani 1 1 d . . . C5 C 0.9744(14) 0.4567(10) 1.1251(9) 0.053(4) Uani 1 1 d . . . H5A H 1.0353 0.4158 1.1409 0.064 Uiso 1 1 calc R . . C6 C 0.9829(15) 0.5548(10) 1.1896(9) 0.055(4) Uani 1 1 d . . . H6A H 1.0510 0.5845 1.2515 0.066 Uiso 1 1 calc R . . C7 C 0.8858(14) 0.6164(10) 1.1642(9) 0.057(4) Uani 1 1 d . . . H7A H 0.8889 0.6853 1.2116 0.069 Uiso 1 1 calc R . . C8 C 0.7921(13) 0.5771(8) 1.0747(8) 0.040(3) Uani 1 1 d . . . H8A H 0.7343 0.6194 1.0588 0.048 Uiso 1 1 calc R . . C9 C 0.7796(13) 0.4732(8) 1.0044(8) 0.033(3) Uani 1 1 d . . . C10 C 0.6799(13) 0.4252(8) 0.9121(8) 0.035(3) Uani 1 1 d . . . C11 C 0.5829(13) 0.4821(9) 0.8756(8) 0.040(3) Uani 1 1 d . . . H11A H 0.5915 0.5535 0.9134 0.048 Uiso 1 1 calc R . . N12 N 0.4907(10) 0.4354(6) 0.7955(6) 0.031(2) Uani 1 1 d . . . C13 C 0.3975(13) 0.4825(8) 0.7552(8) 0.039(3) Uani 1 1 d . . . C14 C 0.3173(12) 0.4307(8) 0.6588(7) 0.037(3) Uani 1 1 d . . . H14A H 0.3243 0.3612 0.6198 0.044 Uiso 1 1 calc R . . C15 C 0.2264(13) 0.4763(9) 0.6162(8) 0.041(3) Uani 1 1 d . . . H15A H 0.1752 0.4383 0.5486 0.050 Uiso 1 1 calc R . . C16 C 0.2101(13) 0.5764(8) 0.6715(8) 0.035(3) Uani 1 1 d . . . C17 C 0.2840(13) 0.6323(8) 0.7732(8) 0.041(3) Uani 1 1 d . . . H17A H 0.2698 0.7001 0.8134 0.049 Uiso 1 1 calc R . . C18 C 0.3775(13) 0.5856(8) 0.8127(8) 0.039(3) Uani 1 1 d . . . H18A H 0.4298 0.6234 0.8800 0.047 Uiso 1 1 calc R . . C19 C 0.1158(12) 0.6293(9) 0.6294(8) 0.038(3) Uani 1 1 d . . . H19A H 0.0798 0.6847 0.6850 0.046 Uiso 1 1 calc R . . H19B H 0.0285 0.5812 0.5822 0.046 Uiso 1 1 calc R . . C20 C 0.2070(13) 0.6735(9) 0.5723(8) 0.035(3) Uani 1 1 d . . . C21 C 0.2215(13) 0.6179(9) 0.4736(9) 0.046(3) Uani 1 1 d . . . H21A H 0.1686 0.5512 0.4364 0.056 Uiso 1 1 calc R . . C22 C 0.3112(13) 0.6558(8) 0.4254(8) 0.041(3) Uani 1 1 d . . . H22A H 0.3148 0.6166 0.3556 0.049 Uiso 1 1 calc R . . C23 C 0.3940(13) 0.7497(9) 0.4791(8) 0.042(3) Uani 1 1 d . . . C24 C 0.3847(13) 0.8086(8) 0.5819(8) 0.040(3) Uani 1 1 d . . . H24A H 0.4396 0.8746 0.6202 0.048 Uiso 1 1 calc R . . C25 C 0.2931(14) 0.7671(10) 0.6247(9) 0.050(4) Uani 1 1 d . . . H25A H 0.2893 0.8053 0.6947 0.060 Uiso 1 1 calc R . . N26 N 0.4806(11) 0.7876(7) 0.4271(6) 0.039(3) Uani 1 1 d . . . C27 C 0.5737(14) 0.8655(9) 0.4741(8) 0.041(3) Uani 1 1 d . . . H27A H 0.5843 0.9029 0.5456 0.049 Uiso 1 1 calc R . . C28 C 0.6702(13) 0.9008(8) 0.4170(8) 0.040(3) Uani 1 1 d . . . N29 N 0.6475(10) 0.8377(7) 0.3202(6) 0.034(2) Uani 1 1 d . . . C30 C 0.7239(15) 0.8585(8) 0.2579(9) 0.053(4) Uani 1 1 d . . . H30A H 0.7075 0.8133 0.1875 0.064 Uiso 1 1 calc R . . C31 C 0.8305(14) 0.9497(10) 0.2990(10) 0.055(4) Uani 1 1 d . . . H31A H 0.8866 0.9629 0.2556 0.066 Uiso 1 1 calc R . . C32 C 0.8525(14) 1.0205(8) 0.4046(8) 0.039(3) Uani 1 1 d . . . C33 C 0.9550(13) 1.1093(10) 0.4445(10) 0.052(4) Uani 1 1 d . . . H33A H 1.0134 1.1234 0.4026 0.062 Uiso 1 1 calc R . . C34 C 0.9692(15) 1.1756(9) 0.5460(9) 0.053(4) Uani 1 1 d . . . H34A H 1.0368 1.2369 0.5739 0.063 Uiso 1 1 calc R . . C35 C 0.8853(14) 1.1542(11) 0.6090(10) 0.053(4) Uani 1 1 d . . . H35A H 0.9000 1.1997 0.6793 0.063 Uiso 1 1 calc R . . C36 C 0.7818(14) 1.0677(9) 0.5694(10) 0.049(4) Uani 1 1 d . . . H36A H 0.7206 1.0560 0.6113 0.059 Uiso 1 1 calc R . . C37 C 0.7673(13) 0.9958(9) 0.4651(9) 0.039(3) Uani 1 1 d . . . N200 N 0.6242(17) 1.0153(8) 0.7436(7) 0.075(5) Uani 1 1 d . . . C201 C 0.5786(19) 1.0333(10) 0.8085(15) 0.087(6) Uani 1 1 d . . . C202 C 0.526(2) 1.0388(15) 0.9142(12) 0.138(8) Uani 1 1 d . . . H20A H 0.4634 1.0914 0.9403 0.207 Uiso 1 1 calc R . . H20B H 0.6146 1.0547 0.9651 0.207 Uiso 1 1 calc R . . H20C H 0.4708 0.9733 0.8989 0.207 Uiso 1 1 calc R . . N300 N 1.2232(18) 1.2454(11) 0.3941(12) 0.119(6) Uani 1 1 d . . . C301 C 1.2898(19) 1.2963(12) 0.3716(12) 0.071(5) Uani 1 1 d . . . C302 C 1.3907(18) 1.3553(13) 0.3442(12) 0.092(5) Uani 1 1 d . . . H30B H 1.3533 1.3449 0.2759 0.138 Uiso 1 1 calc R . . H30C H 1.4887 1.3341 0.3458 0.138 Uiso 1 1 calc R . . H30D H 1.3986 1.4271 0.3923 0.138 Uiso 1 1 calc R . . B10 B 0.730(2) 0.7713(18) 0.9630(17) 0.078(6) Uani 1 1 d . . . F11 F 0.7771(12) 0.6923(8) 0.8939(8) 0.123(4) Uani 1 1 d . . . F12 F 0.8507(12) 0.8344(8) 1.0357(8) 0.143(4) Uani 1 1 d . . . F13 F 0.6609(11) 0.8247(7) 0.9156(7) 0.108(3) Uani 1 1 d . . . F14 F 0.6301(9) 0.7445(6) 1.0106(5) 0.077(2) Uani 1 1 d . . . N400 N 0.178(2) 0.8800(13) 0.8699(13) 0.115(6) Uani 1 1 d . . . C401 C 0.073(3) 0.9048(19) 0.8701(15) 0.120(9) Uani 1 1 d . . . C402 C -0.071(3) 0.9469(14) 0.8575(16) 0.141(8) Uani 1 1 d . . . H40F H -0.1128 0.9174 0.7855 0.211 Uiso 1 1 calc R . . H40E H -0.0492 1.0206 0.8860 0.211 Uiso 1 1 calc R . . H40D H -0.1426 0.9295 0.8931 0.211 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0803(13) 0.0244(9) 0.0285(8) 0.0133(7) 0.0018(8) 0.0078(8) N1 0.071(7) 0.022(5) 0.020(5) 0.013(5) -0.007(5) 0.010(6) C2 0.075(10) 0.027(7) 0.036(7) 0.014(6) 0.011(7) 0.016(7) C3 0.111(12) 0.054(9) 0.017(7) 0.012(7) 0.006(8) 0.041(9) C4 0.050(9) 0.060(10) 0.049(8) 0.025(8) 0.009(7) 0.004(8) C5 0.080(11) 0.046(9) 0.031(7) 0.017(7) 0.003(7) 0.007(8) C6 0.070(10) 0.037(8) 0.043(8) 0.008(7) 0.002(7) -0.003(8) C7 0.067(10) 0.050(9) 0.044(8) 0.020(8) -0.013(8) -0.012(8) C8 0.058(9) 0.021(7) 0.027(7) 0.006(6) -0.008(6) -0.012(6) C9 0.061(9) 0.026(7) 0.022(6) 0.020(6) 0.003(6) 0.008(7) C10 0.050(9) 0.017(6) 0.024(6) 0.000(5) 0.002(6) -0.007(6) C11 0.056(9) 0.025(7) 0.034(7) 0.011(6) -0.004(7) 0.014(7) N12 0.060(7) 0.014(5) 0.024(5) 0.014(4) -0.003(5) 0.005(5) C13 0.059(9) 0.028(7) 0.017(6) 0.000(6) 0.014(6) -0.011(7) C14 0.052(8) 0.014(6) 0.021(6) -0.011(5) 0.001(6) -0.002(6) C15 0.060(9) 0.044(8) 0.031(7) 0.023(6) 0.006(6) 0.027(7) C16 0.053(8) 0.030(7) 0.042(7) 0.034(7) 0.009(7) 0.009(7) C17 0.068(9) 0.016(6) 0.037(7) 0.009(6) 0.011(7) 0.010(7) C18 0.067(9) 0.021(7) 0.024(6) 0.008(6) 0.003(6) -0.003(7) C19 0.049(8) 0.036(7) 0.031(6) 0.015(6) 0.005(6) 0.016(7) C20 0.049(9) 0.041(8) 0.015(6) 0.016(6) -0.007(6) 0.005(7) C21 0.067(10) 0.033(7) 0.050(8) 0.030(7) 0.001(7) 0.008(7) C22 0.077(10) 0.015(6) 0.024(6) 0.004(5) 0.012(6) -0.005(7) C23 0.061(9) 0.043(8) 0.024(6) 0.022(6) -0.003(6) -0.006(7) C24 0.071(10) 0.013(6) 0.044(8) 0.019(6) 0.018(7) 0.006(6) C25 0.066(10) 0.052(9) 0.029(7) 0.023(7) -0.007(7) -0.008(8) N26 0.066(8) 0.022(6) 0.032(5) 0.017(5) -0.001(5) -0.001(6) C27 0.074(10) 0.030(8) 0.024(6) 0.017(6) 0.007(7) 0.012(8) C28 0.073(10) 0.010(6) 0.032(7) 0.014(5) -0.021(7) -0.009(7) N29 0.044(6) 0.036(6) 0.021(5) 0.016(5) -0.003(5) -0.002(5) C30 0.109(12) 0.011(6) 0.041(7) 0.013(6) 0.017(8) 0.009(8) C31 0.067(10) 0.048(9) 0.063(9) 0.034(8) 0.017(8) 0.015(8) C32 0.059(9) 0.017(7) 0.035(7) 0.010(6) -0.006(7) 0.002(7) C33 0.042(9) 0.063(10) 0.058(9) 0.034(8) 0.007(7) 0.015(8) C34 0.087(11) 0.020(7) 0.040(8) 0.008(6) 0.000(8) -0.005(7) C35 0.051(9) 0.063(10) 0.046(8) 0.030(8) -0.007(7) 0.009(8) C36 0.058(10) 0.040(8) 0.068(10) 0.044(8) 0.001(8) 0.004(8) C37 0.047(8) 0.046(8) 0.036(7) 0.028(7) 0.007(7) 0.018(7) N200 0.173(14) 0.044(7) 0.019(6) 0.015(6) 0.039(7) 0.033(8) C201 0.083(13) 0.021(8) 0.109(15) -0.010(10) 0.018(12) -0.009(8) C202 0.21(2) 0.156(19) 0.072(12) 0.074(13) 0.052(13) 0.012(17) N300 0.122(14) 0.064(11) 0.138(14) 0.029(10) 0.014(11) -0.036(10) C301 0.074(13) 0.046(10) 0.072(11) 0.014(9) -0.010(10) 0.000(10) C302 0.088(13) 0.107(14) 0.086(12) 0.046(12) 0.025(10) 0.020(12) B10 0.059(15) 0.072(15) 0.081(15) 0.024(14) 0.000(13) -0.013(13) F11 0.168(11) 0.086(8) 0.102(8) 0.024(7) 0.037(7) 0.042(7) F12 0.128(9) 0.111(9) 0.121(8) 0.012(7) -0.009(7) -0.039(8) F13 0.145(9) 0.096(8) 0.111(8) 0.065(7) 0.034(7) 0.041(7) F14 0.103(7) 0.055(5) 0.055(5) 0.015(4) 0.000(5) -0.002(5) N400 0.121(17) 0.096(12) 0.098(12) 0.009(10) 0.026(13) 0.058(13) C401 0.079(18) 0.13(2) 0.069(12) -0.023(13) 0.014(14) 0.005(16) C402 0.16(2) 0.073(14) 0.17(2) 0.040(15) 0.052(18) 0.007(15) _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 Cu1 N29 2.008(9) 2_666 ? Cu1 N1 2.039(9) . ? Cu1 N26 2.045(9) 2_666 ? Cu1 N12 2.066(8) . ? N1 C10 1.320(13) . ? N1 C2 1.337(14) . ? C2 C3 1.324(15) . ? C2 H2A 0.9500 . ? C3 C4 1.392(17) . ? C3 H3A 0.9500 . ? C4 C9 1.408(16) . ? C4 C5 1.476(16) . ? C5 C6 1.338(16) . ? C5 H5A 0.9500 . ? C6 C7 1.472(18) . ? C6 H6A 0.9500 . ? C7 C8 1.355(14) . ? C7 H7A 0.9500 . ? C8 C9 1.420(14) . ? C8 H8A 0.9500 . ? C9 C10 1.408(14) . ? C10 C11 1.502(15) . ? C11 N12 1.253(12) . ? C11 H11A 0.9500 . ? N12 C13 1.401(14) . ? C13 C14 1.376(13) . ? C13 C18 1.432(15) . ? C14 C15 1.392(15) . ? C14 H14A 0.9500 . ? C15 C16 1.381(15) . ? C15 H15A 0.9500 . ? C16 C17 1.419(15) . ? C16 C19 1.489(15) . ? C17 C18 1.391(15) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.565(14) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.364(15) . ? C20 C25 1.375(15) . ? C21 C22 1.395(14) . ? C21 H21A 0.9500 . ? C22 C23 1.367(14) . ? C22 H22A 0.9500 . ? C23 C24 1.409(14) . ? C23 N26 1.423(13) . ? C24 C25 1.378(14) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? N26 C27 1.244(13) . ? N26 Cu1 2.045(9) 2_666 ? C27 C28 1.514(15) . ? C27 H27A 0.9500 . ? C28 N29 1.308(13) . ? C28 C37 1.435(15) . ? N29 C30 1.355(13) . ? N29 Cu1 2.008(9) 2_666 ? C30 C31 1.444(16) . ? C30 H30A 0.9500 . ? C31 C32 1.436(16) . ? C31 H31A 0.9500 . ? C32 C33 1.399(15) . ? C32 C37 1.408(15) . ? C33 C34 1.378(16) . ? C33 H33A 0.9500 . ? C34 C35 1.408(16) . ? C34 H34A 0.9500 . ? C35 C36 1.382(16) . ? C35 H35A 0.9500 . ? C36 C37 1.430(16) . ? C36 H36A 0.9500 . ? N200 C201 1.035(17) . ? C201 C202 1.68(2) . ? C202 H20A 0.9800 . ? C202 H20B 0.9800 . ? C202 H20C 0.9800 . ? N300 C301 1.125(18) . ? C301 C302 1.44(2) . ? C302 H30B 0.9800 . ? C302 H30C 0.9800 . ? C302 H30D 0.9800 . ? B10 F11 1.32(2) . ? B10 F14 1.36(2) . ? B10 F12 1.39(2) . ? B10 F13 1.43(2) . ? N400 C401 1.06(2) . ? C401 C402 1.54(3) . ? C402 H40F 0.9800 . ? C402 H40E 0.9800 . ? C402 H40D 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N29 Cu1 N1 122.2(3) 2_666 . ? N29 Cu1 N26 80.9(4) 2_666 2_666 ? N1 Cu1 N26 129.8(4) . 2_666 ? N29 Cu1 N12 129.7(4) 2_666 . ? N1 Cu1 N12 81.0(4) . . ? N26 Cu1 N12 120.3(3) 2_666 . ? C10 N1 C2 116.0(10) . . ? C10 N1 Cu1 113.3(8) . . ? C2 N1 Cu1 130.3(8) . . ? C3 C2 N1 125.7(12) . . ? C3 C2 H2A 117.1 . . ? N1 C2 H2A 117.1 . . ? C2 C3 C4 119.5(13) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C3 C4 C9 117.3(12) . . ? C3 C4 C5 121.9(13) . . ? C9 C4 C5 120.8(12) . . ? C6 C5 C4 119.1(13) . . ? C6 C5 H5A 120.5 . . ? C4 C5 H5A 120.5 . . ? C5 C6 C7 119.5(13) . . ? C5 C6 H6A 120.2 . . ? C7 C6 H6A 120.2 . . ? C8 C7 C6 121.5(13) . . ? C8 C7 H7A 119.3 . . ? C6 C7 H7A 119.3 . . ? C7 C8 C9 120.6(12) . . ? C7 C8 H8A 119.7 . . ? C9 C8 H8A 119.7 . . ? C4 C9 C10 117.2(11) . . ? C4 C9 C8 118.5(11) . . ? C10 C9 C8 124.2(11) . . ? N1 C10 C9 123.9(11) . . ? N1 C10 C11 113.6(10) . . ? C9 C10 C11 122.2(10) . . ? N12 C11 C10 120.0(10) . . ? N12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C11 N12 C13 123.8(9) . . ? C11 N12 Cu1 111.5(8) . . ? C13 N12 Cu1 124.4(7) . . ? C14 C13 N12 121.3(11) . . ? C14 C13 C18 116.6(12) . . ? N12 C13 C18 122.0(10) . . ? C13 C14 C15 122.5(11) . . ? C13 C14 H14A 118.8 . . ? C15 C14 H14A 118.8 . . ? C16 C15 C14 120.4(11) . . ? C16 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C15 C16 C17 119.7(11) . . ? C15 C16 C19 122.7(11) . . ? C17 C16 C19 117.6(11) . . ? C18 C17 C16 118.6(11) . . ? C18 C17 H17A 120.7 . . ? C16 C17 H17A 120.7 . . ? C17 C18 C13 122.1(11) . . ? C17 C18 H18A 119.0 . . ? C13 C18 H18A 119.0 . . ? C16 C19 C20 110.1(9) . . ? C16 C19 H19A 109.6 . . ? C20 C19 H19A 109.6 . . ? C16 C19 H19B 109.6 . . ? C20 C19 H19B 109.6 . . ? H19A C19 H19B 108.1 . . ? C21 C20 C25 116.7(10) . . ? C21 C20 C19 122.7(10) . . ? C25 C20 C19 120.1(10) . . ? C20 C21 C22 122.2(11) . . ? C20 C21 H21A 118.9 . . ? C22 C21 H21A 118.9 . . ? C23 C22 C21 119.6(10) . . ? C23 C22 H22A 120.2 . . ? C21 C22 H22A 120.2 . . ? C22 C23 C24 119.8(10) . . ? C22 C23 N26 118.3(10) . . ? C24 C23 N26 121.7(10) . . ? C25 C24 C23 117.6(11) . . ? C25 C24 H24A 121.2 . . ? C23 C24 H24A 121.2 . . ? C20 C25 C24 123.9(11) . . ? C20 C25 H25A 118.1 . . ? C24 C25 H25A 118.1 . . ? C27 N26 C23 121.0(9) . . ? C27 N26 Cu1 111.9(7) . 2_666 ? C23 N26 Cu1 126.5(8) . 2_666 ? N26 C27 C28 119.8(10) . . ? N26 C27 H27A 120.1 . . ? C28 C27 H27A 120.1 . . ? N29 C28 C37 125.4(10) . . ? N29 C28 C27 112.1(9) . . ? C37 C28 C27 122.4(10) . . ? C28 N29 C30 119.6(10) . . ? C28 N29 Cu1 115.2(7) . 2_666 ? C30 N29 Cu1 125.2(7) . 2_666 ? N29 C30 C31 119.7(11) . . ? N29 C30 H30A 120.2 . . ? C31 C30 H30A 120.2 . . ? C32 C31 C30 120.8(11) . . ? C32 C31 H31A 119.6 . . ? C30 C31 H31A 119.6 . . ? C33 C32 C37 122.3(11) . . ? C33 C32 C31 120.9(11) . . ? C37 C32 C31 116.8(11) . . ? C34 C33 C32 118.4(11) . . ? C34 C33 H33A 120.8 . . ? C32 C33 H33A 120.8 . . ? C33 C34 C35 121.2(12) . . ? C33 C34 H34A 119.4 . . ? C35 C34 H34A 119.4 . . ? C36 C35 C34 120.5(12) . . ? C36 C35 H35A 119.7 . . ? C34 C35 H35A 119.7 . . ? C35 C36 C37 119.7(11) . . ? C35 C36 H36A 120.2 . . ? C37 C36 H36A 120.2 . . ? C32 C37 C36 117.8(11) . . ? C32 C37 C28 117.5(11) . . ? C36 C37 C28 124.7(10) . . ? N200 C201 C202 165(2) . . ? C201 C202 H20A 109.5 . . ? C201 C202 H20B 109.5 . . ? H20A C202 H20B 109.5 . . ? C201 C202 H20C 109.5 . . ? H20A C202 H20C 109.5 . . ? H20B C202 H20C 109.5 . . ? N300 C301 C302 172.8(19) . . ? C301 C302 H30B 109.5 . . ? C301 C302 H30C 109.5 . . ? H30B C302 H30C 109.5 . . ? C301 C302 H30D 109.5 . . ? H30B C302 H30D 109.5 . . ? H30C C302 H30D 109.5 . . ? F11 B10 F14 112.6(18) . . ? F11 B10 F12 108.9(18) . . ? F14 B10 F12 108.1(17) . . ? F11 B10 F13 109.1(17) . . ? F14 B10 F13 108.4(17) . . ? F12 B10 F13 109.7(17) . . ? N400 C401 C402 170(3) . . ? C401 C402 H40F 109.5 . . ? C401 C402 H40E 109.5 . . ? H40F C402 H40E 109.5 . . ? C401 C402 H40D 109.5 . . ? H40F C402 H40D 109.5 . . ? H40E C402 H40D 109.5 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.073 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.107