# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Frieder Jaekle' _publ_contact_author_address ; Chemistry Department Rutgers University 73 Warren Street Newark NJ 07102 UNITED STATES OF AMERICA ; _publ_contact_author_email FJAEKLE@ANDROMEDA.RUTGERS.EDU _publ_section_title ; Lewis Acidity Enhancement of Organoboranes via Oxidation of Appended Ferrocene Moieties ; loop_ _publ_author_name 'Frieder Jaekle' 'Rolfe H. Herber' 'Israel Nowik' 'Krishnan Venkatasubbaiah' data_1+pf6 _database_code_depnum_ccdc_archive 'CCDC 635884' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H28 B2 Cl6 F6 Fe2 P' _chemical_formula_sum 'C34 H28 B2 Cl6 F6 Fe2 P' _chemical_formula_weight 927.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' B B 0.0090 0.0039 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.5711(3) _cell_length_b 25.9704(4) _cell_length_c 15.3244(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.0530(10) _cell_angle_gamma 90.00 _cell_volume 7277.5(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8190 _cell_measurement_theta_min 3.39 _cell_measurement_theta_max 69.24 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3720 _exptl_absorpt_coefficient_mu 11.374 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1632 _exptl_absorpt_correction_T_max 0.5486 _exptl_absorpt_process_details '(SADABS; Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 CCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44369 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 64.99 _reflns_number_total 11958 _reflns_number_gt 9474 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT-Plus (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2000)' _computing_publication_material SHELXTL _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^)+(0.0618P)^2^+21.4637P] 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_number_reflns 11958 _refine_ls_number_parameters 919 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1335 _refine_ls_wR_factor_gt 0.1220 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.009 _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 B1 B 0.6970(3) 0.64119(18) 0.2168(3) 0.0139(10) Uani 1 1 d . . . B2 B 0.8123(3) 0.69715(18) 0.3558(3) 0.0160(10) Uani 1 1 d . . . B3 B 0.1953(3) 0.64610(18) 0.2035(3) 0.0152(10) Uani 1 1 d . . . B4 B 0.3071(3) 0.70285(18) 0.3469(3) 0.0139(10) Uani 1 1 d . . . C1 C 0.8944(3) 0.61017(19) 0.2125(3) 0.0300(12) Uani 1 1 d . . . H1 H 0.8836 0.6427 0.1778 0.036 Uiso 1 1 calc R . . C2 C 0.9433(3) 0.60510(19) 0.2935(3) 0.0296(11) Uani 1 1 d . . . H2 H 0.9734 0.6333 0.3261 0.035 Uiso 1 1 calc R . . C3 C 0.9434(3) 0.55262(18) 0.3195(3) 0.0255(10) Uani 1 1 d . . . H3 H 0.9735 0.5374 0.3739 0.031 Uiso 1 1 calc R . . C4 C 0.8942(3) 0.52558(18) 0.2549(3) 0.0265(11) Uani 1 1 d . . . H4 H 0.8837 0.4878 0.2553 0.032 Uiso 1 1 calc R . . C5 C 0.8634(3) 0.5610(2) 0.1884(3) 0.0300(11) Uani 1 1 d . . . H5 H 0.8275 0.5528 0.1336 0.036 Uiso 1 1 calc R . . C6 C 0.7877(2) 0.64082(16) 0.3699(3) 0.0143(9) Uani 1 1 d . . . C7 C 0.8184(2) 0.60322(17) 0.4351(3) 0.0184(9) Uani 1 1 d . . . H7 H 0.8565 0.6101 0.4885 0.022 Uiso 1 1 calc R . . C8 C 0.7852(2) 0.55498(17) 0.4110(3) 0.0213(10) Uani 1 1 d . . . H8 H 0.7964 0.5219 0.4438 0.026 Uiso 1 1 calc R . . C9 C 0.7336(2) 0.56176(16) 0.3318(3) 0.0177(9) Uani 1 1 d . . . H9 H 0.7026 0.5339 0.2993 0.021 Uiso 1 1 calc R . . C10 C 0.7345(2) 0.61445(15) 0.3044(3) 0.0151(9) Uani 1 1 d . . . C11 C 0.6521(3) 0.73381(17) 0.3931(3) 0.0222(10) Uani 1 1 d . . . H11 H 0.6816 0.7146 0.4437 0.027 Uiso 1 1 calc R . . C12 C 0.6573(2) 0.78729(17) 0.3749(3) 0.0222(10) Uani 1 1 d . . . H12 H 0.6906 0.8125 0.4111 0.027 Uiso 1 1 calc R . . C13 C 0.6063(3) 0.79867(18) 0.2967(3) 0.0257(10) Uani 1 1 d . . . H13 H 0.5972 0.8334 0.2687 0.031 Uiso 1 1 calc R . . C14 C 0.5696(3) 0.75261(19) 0.2665(3) 0.0271(11) Uani 1 1 d . . . H14 H 0.5304 0.7489 0.2131 0.032 Uiso 1 1 calc R . . C15 C 0.5980(3) 0.71270(18) 0.3261(3) 0.0264(11) Uani 1 1 d . . . H15 H 0.5830 0.6757 0.3209 0.032 Uiso 1 1 calc R . . C16 C 0.7829(2) 0.72040(15) 0.2651(3) 0.0147(9) Uani 1 1 d . . . C17 C 0.7778(2) 0.77453(16) 0.2440(3) 0.0179(9) Uani 1 1 d . . . H17 H 0.8072 0.8024 0.2784 0.021 Uiso 1 1 calc R . . C18 C 0.7233(2) 0.78211(16) 0.1689(3) 0.0206(10) Uani 1 1 d . . . H18 H 0.7073 0.8162 0.1418 0.025 Uiso 1 1 calc R . . C19 C 0.6925(2) 0.73379(16) 0.1406(3) 0.0195(9) Uani 1 1 d . . . H19 H 0.6518 0.7280 0.0895 0.023 Uiso 1 1 calc R . . C20 C 0.7284(2) 0.69440(16) 0.1988(3) 0.0163(9) Uani 1 1 d . . . C21 C 0.8662(2) 0.72720(16) 0.4277(3) 0.0168(9) Uani 1 1 d . . . C22 C 0.8588(2) 0.72832(17) 0.5168(3) 0.0211(10) Uani 1 1 d . . . H22 H 0.8212 0.7086 0.5356 0.025 Uiso 1 1 calc R . . C23 C 0.9051(3) 0.75761(18) 0.5786(3) 0.0260(11) Uani 1 1 d . . . H23 H 0.8976 0.7590 0.6384 0.031 Uiso 1 1 calc R . . C24 C 0.9623(3) 0.78481(18) 0.5531(3) 0.0288(11) Uani 1 1 d . . . H24 H 0.9942 0.8046 0.5953 0.035 Uiso 1 1 calc R . . C25 C 0.9726(3) 0.78302(18) 0.4659(3) 0.0271(11) Uani 1 1 d . . . H25 H 1.0125 0.8008 0.4485 0.032 Uiso 1 1 calc R . . C26 C 0.9248(2) 0.75539(16) 0.4041(3) 0.0214(10) Uani 1 1 d . . . H26 H 0.9315 0.7554 0.3441 0.026 Uiso 1 1 calc R . . C27 C 0.6347(2) 0.61491(15) 0.1508(3) 0.0166(9) Uani 1 1 d . . . C28 C 0.5805(2) 0.58383(16) 0.1777(3) 0.0195(9) Uani 1 1 d . . . H28 H 0.5812 0.5784 0.2392 0.023 Uiso 1 1 calc R . . C29 C 0.5262(2) 0.56091(17) 0.1167(3) 0.0246(10) Uani 1 1 d . . . H29 H 0.4900 0.5403 0.1365 0.029 Uiso 1 1 calc R . . C30 C 0.5247(3) 0.56808(18) 0.0258(3) 0.0276(11) Uani 1 1 d . . . H30 H 0.4873 0.5526 -0.0162 0.033 Uiso 1 1 calc R . . C31 C 0.5778(3) 0.59773(17) -0.0024(3) 0.0244(10) Uani 1 1 d . . . H31 H 0.5776 0.6021 -0.0640 0.029 Uiso 1 1 calc R . . C32 C 0.6316(2) 0.62116(17) 0.0589(3) 0.0206(9) Uani 1 1 d . . . H32 H 0.6673 0.6420 0.0385 0.025 Uiso 1 1 calc R . . C33 C 0.3888(3) 0.60119(19) 0.2242(4) 0.0322(12) Uani 1 1 d . . . H33 H 0.3810 0.6307 0.1817 0.039 Uiso 1 1 calc R . . C34 C 0.4329(3) 0.6020(2) 0.3083(4) 0.0344(12) Uani 1 1 d . . . H34 H 0.4625 0.6319 0.3358 0.041 Uiso 1 1 calc R . . C35 C 0.4293(3) 0.55228(19) 0.3470(3) 0.0280(11) Uani 1 1 d . . . H35 H 0.4560 0.5410 0.4063 0.034 Uiso 1 1 calc R . . C36 C 0.3831(3) 0.52142(17) 0.2855(3) 0.0237(10) Uani 1 1 d . . . H36 H 0.3709 0.4844 0.2937 0.028 Uiso 1 1 calc R . . C37 C 0.3570(3) 0.55214(19) 0.2092(3) 0.0276(11) Uani 1 1 d . . . H37 H 0.3236 0.5405 0.1544 0.033 Uiso 1 1 calc R . . C38 C 0.2751(2) 0.64868(16) 0.3645(3) 0.0164(9) Uani 1 1 d . . . C39 C 0.2944(2) 0.61372(17) 0.4370(3) 0.0205(9) Uani 1 1 d . . . H39 H 0.3284 0.6214 0.4936 0.025 Uiso 1 1 calc R . . C40 C 0.2580(2) 0.56643(17) 0.4152(3) 0.0205(9) Uani 1 1 d . . . H40 H 0.2625 0.5350 0.4533 0.025 Uiso 1 1 calc R . . C41 C 0.2155(2) 0.57080(16) 0.3299(3) 0.0188(9) Uani 1 1 d . . . H41 H 0.1842 0.5430 0.2978 0.023 Uiso 1 1 calc R . . C42 C 0.2245(2) 0.62162(16) 0.2966(3) 0.0150(9) Uani 1 1 d . . . C43 C 0.1470(3) 0.73741(19) 0.3737(3) 0.0289(11) Uani 1 1 d . . . H43 H 0.1706 0.7137 0.4216 0.035 Uiso 1 1 calc R . . C44 C 0.1633(3) 0.79018(19) 0.3655(3) 0.0259(10) Uani 1 1 d . . . H44 H 0.2000 0.8105 0.4074 0.031 Uiso 1 1 calc R . . C45 C 0.1175(3) 0.80967(18) 0.2885(3) 0.0242(10) Uani 1 1 d . . . H45 H 0.1163 0.8460 0.2667 0.029 Uiso 1 1 calc R . . C46 C 0.0736(2) 0.76876(19) 0.2487(3) 0.0269(11) Uani 1 1 d . . . H46 H 0.0360 0.7708 0.1934 0.032 Uiso 1 1 calc R . . C47 C 0.0921(3) 0.72410(19) 0.3017(3) 0.0288(11) Uani 1 1 d . . . H47 H 0.0702 0.6891 0.2895 0.035 Uiso 1 1 calc R . . C48 C 0.2835(2) 0.72374(15) 0.2532(3) 0.0148(9) Uani 1 1 d . . . C49 C 0.2819(2) 0.77792(16) 0.2308(3) 0.0169(9) Uani 1 1 d . . . H49 H 0.3125 0.8053 0.2650 0.020 Uiso 1 1 calc R . . C50 C 0.2280(2) 0.78601(16) 0.1551(3) 0.0184(9) Uani 1 1 d . . . H50 H 0.2137 0.8202 0.1273 0.022 Uiso 1 1 calc R . . C51 C 0.1954(2) 0.73783(16) 0.1268(3) 0.0167(9) Uani 1 1 d . . . H51 H 0.1548 0.7325 0.0754 0.020 Uiso 1 1 calc R . . C52 C 0.2288(2) 0.69828(16) 0.1868(3) 0.0149(9) Uani 1 1 d . . . C53 C 0.3605(2) 0.73346(15) 0.4185(3) 0.0159(9) Uani 1 1 d . . . C54 C 0.3498(2) 0.73896(16) 0.5059(3) 0.0191(9) Uani 1 1 d . . . H54 H 0.3094 0.7222 0.5239 0.023 Uiso 1 1 calc R . . C55 C 0.3963(3) 0.76818(16) 0.5673(3) 0.0220(10) Uani 1 1 d . . . H55 H 0.3868 0.7720 0.6258 0.026 Uiso 1 1 calc R . . C56 C 0.4573(3) 0.79197(17) 0.5428(3) 0.0238(10) Uani 1 1 d . . . H56 H 0.4893 0.8121 0.5845 0.029 Uiso 1 1 calc R . . C57 C 0.4705(3) 0.78604(18) 0.4572(3) 0.0242(10) Uani 1 1 d . . . H57 H 0.5126 0.8012 0.4406 0.029 Uiso 1 1 calc R . . C58 C 0.4222(2) 0.75786(17) 0.3956(3) 0.0204(9) Uani 1 1 d . . . H58 H 0.4311 0.7550 0.3366 0.024 Uiso 1 1 calc R . . C59 C 0.1361(2) 0.61933(15) 0.1326(3) 0.0152(9) Uani 1 1 d . . . C60 C 0.0773(2) 0.59096(16) 0.1551(3) 0.0192(9) Uani 1 1 d . . . H60 H 0.0728 0.5874 0.2156 0.023 Uiso 1 1 calc R . . C61 C 0.0259(2) 0.56808(17) 0.0899(3) 0.0207(10) Uani 1 1 d . . . H61 H -0.0136 0.5494 0.1064 0.025 Uiso 1 1 calc R . . C62 C 0.0316(2) 0.57206(16) 0.0020(3) 0.0212(10) Uani 1 1 d . . . H62 H -0.0039 0.5562 -0.0419 0.025 Uiso 1 1 calc R . . C63 C 0.0895(3) 0.59938(17) -0.0226(3) 0.0219(10) Uani 1 1 d . . . H63 H 0.0942 0.6020 -0.0832 0.026 Uiso 1 1 calc R . . C64 C 0.1406(2) 0.62285(16) 0.0428(3) 0.0169(9) Uani 1 1 d . . . H64 H 0.1796 0.6418 0.0257 0.020 Uiso 1 1 calc R . . C65 C 0.2736(3) 0.5685(2) 0.9086(4) 0.0416(14) Uani 1 1 d . . . H65 H 0.2296 0.5659 0.9378 0.050 Uiso 1 1 calc R . . C66 C 0.4564(3) 0.58485(17) 0.6766(3) 0.0247(10) Uani 1 1 d . . . H66 H 0.5041 0.5837 0.6549 0.030 Uiso 1 1 calc R . . C67 C 0.7709(4) 0.5724(2) 0.9349(5) 0.0572(18) Uani 1 1 d . . . H67 H 0.7374 0.5688 0.9790 0.069 Uiso 1 1 calc R . . C68 C 0.9151(3) 0.58373(19) 0.6962(3) 0.0295(11) Uani 1 1 d . . . H68 H 0.9434 0.5833 0.6464 0.035 Uiso 1 1 calc R . . Cl1 Cl 0.32214(8) 0.51082(5) 0.92355(11) 0.0497(4) Uani 1 1 d . . . Cl2 Cl 0.32812(8) 0.62031(5) 0.95522(10) 0.0460(4) Uani 1 1 d . . . Cl3 Cl 0.24429(9) 0.57983(5) 0.79111(11) 0.0531(4) Uani 1 1 d . . . Cl4 Cl 0.47353(14) 0.57255(8) 0.79008(11) 0.0905(8) Uani 1 1 d . . . Cl5 Cl 0.39973(7) 0.53652(4) 0.62109(8) 0.0327(3) Uani 1 1 d . . . Cl6 Cl 0.41959(9) 0.64574(5) 0.65510(11) 0.0555(4) Uani 1 1 d . . . Cl7 Cl 0.82345(8) 0.51582(5) 0.94158(9) 0.0401(3) Uani 1 1 d . . . Cl8 Cl 0.82787(7) 0.62628(5) 0.96859(8) 0.0373(3) Uani 1 1 d . . . Cl9 Cl 0.71692(8) 0.58188(5) 0.83442(10) 0.0492(4) Uani 1 1 d . . . Cl10 Cl 0.93769(7) 0.52880(5) 0.76228(8) 0.0357(3) Uani 1 1 d . . . Cl11 Cl 0.93978(8) 0.63867(5) 0.76212(13) 0.0579(4) Uani 1 1 d . . . Cl12 Cl 0.82127(7) 0.58394(6) 0.65260(8) 0.0427(3) Uani 1 1 d . . . F1 F 0.54767(15) 0.55491(11) 0.53273(18) 0.0356(7) Uani 1 1 d . . . F2 F 0.68042(15) 0.63099(10) 0.51850(17) 0.0289(6) Uani 1 1 d . . . F3 F 0.62864(15) 0.59936(10) 0.63126(16) 0.0299(6) Uani 1 1 d . . . F4 F 0.66786(16) 0.54544(10) 0.53294(18) 0.0324(6) Uani 1 1 d . . . F5 F 0.59805(15) 0.58733(10) 0.41949(16) 0.0278(6) Uani 1 1 d . . . F6 F 0.55926(17) 0.64104(12) 0.5171(2) 0.0428(8) Uani 1 1 d . . . F7 F 0.92415(18) 0.08263(15) 0.8565(2) 0.0522(9) Uani 1 1 d . . . F8 F 0.90998(17) 0.11010(14) 1.0567(2) 0.0466(8) Uani 1 1 d . . . F9 F 0.91702(19) 0.03682(12) 0.9810(3) 0.0546(9) Uani 1 1 d . . . F10 F 0.82965(15) 0.09456(12) 0.9285(2) 0.0410(7) Uani 1 1 d . . . F11 F 0.91709(18) 0.15545(12) 0.9331(2) 0.0493(8) Uani 1 1 d . . . F12 F 1.00421(15) 0.09712(12) 0.98359(19) 0.0363(7) Uani 1 1 d . . . Fe1 Fe 0.83812(4) 0.58308(2) 0.31021(4) 0.01424(16) Uani 1 1 d . . . Fe2 Fe 0.68040(4) 0.74597(2) 0.26932(4) 0.01380(15) Uani 1 1 d . . . Fe3 Fe 0.32529(4) 0.58499(2) 0.32096(4) 0.01520(16) Uani 1 1 d . . . Fe4 Fe 0.18273(4) 0.75203(2) 0.25563(4) 0.01398(16) Uani 1 1 d . . . P1 P 0.61323(6) 0.59343(4) 0.52482(7) 0.0183(2) Uani 1 1 d . . . P2 P 0.91641(7) 0.09614(4) 0.95716(8) 0.0234(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.014(3) 0.015(2) 0.016(2) -0.0017(18) 0.0087(18) 0.0020(19) B2 0.014(3) 0.016(2) 0.020(2) -0.0017(19) 0.0084(19) 0.002(2) B3 0.013(3) 0.014(2) 0.019(2) 0.0014(19) 0.0063(18) 0.0050(19) B4 0.010(2) 0.014(2) 0.020(2) 0.0009(18) 0.0082(18) 0.0010(19) C1 0.035(3) 0.025(3) 0.037(3) 0.007(2) 0.028(2) 0.008(2) C2 0.024(3) 0.026(3) 0.043(3) -0.011(2) 0.020(2) -0.009(2) C3 0.019(3) 0.029(3) 0.029(3) -0.004(2) 0.0081(19) 0.006(2) C4 0.028(3) 0.019(2) 0.033(3) -0.006(2) 0.009(2) 0.005(2) C5 0.027(3) 0.041(3) 0.024(3) -0.005(2) 0.013(2) 0.004(2) C6 0.014(2) 0.018(2) 0.013(2) 0.0035(16) 0.0089(15) -0.0008(17) C7 0.019(2) 0.020(2) 0.016(2) 0.0028(17) 0.0058(17) 0.0009(18) C8 0.022(2) 0.020(2) 0.024(2) 0.0069(18) 0.0109(18) 0.0014(19) C9 0.017(2) 0.014(2) 0.024(2) 0.0041(17) 0.0093(17) -0.0023(18) C10 0.014(2) 0.012(2) 0.021(2) -0.0003(16) 0.0080(16) -0.0011(17) C11 0.026(3) 0.023(2) 0.021(2) -0.0008(18) 0.0111(18) 0.005(2) C12 0.022(3) 0.020(2) 0.025(2) -0.0033(18) 0.0081(18) 0.0010(19) C13 0.025(3) 0.025(3) 0.028(3) 0.0004(19) 0.0093(19) 0.008(2) C14 0.018(2) 0.036(3) 0.028(3) -0.006(2) 0.0063(19) 0.003(2) C15 0.027(3) 0.020(2) 0.036(3) -0.007(2) 0.017(2) -0.002(2) C16 0.016(2) 0.012(2) 0.018(2) 0.0006(16) 0.0064(16) 0.0030(17) C17 0.017(2) 0.012(2) 0.026(2) 0.0022(17) 0.0077(17) -0.0019(17) C18 0.024(3) 0.014(2) 0.025(2) 0.0038(18) 0.0079(18) -0.0002(18) C19 0.022(2) 0.019(2) 0.019(2) 0.0025(17) 0.0057(17) 0.0024(19) C20 0.018(2) 0.017(2) 0.015(2) 0.0008(16) 0.0048(16) 0.0036(18) C21 0.015(2) 0.013(2) 0.021(2) -0.0004(17) 0.0011(17) 0.0011(17) C22 0.020(2) 0.019(2) 0.025(2) 0.0006(18) 0.0047(18) 0.0000(19) C23 0.030(3) 0.026(3) 0.020(2) -0.0038(19) -0.0003(19) 0.002(2) C24 0.030(3) 0.018(2) 0.032(3) -0.004(2) -0.011(2) -0.004(2) C25 0.023(3) 0.019(2) 0.038(3) 0.003(2) 0.000(2) -0.004(2) C26 0.021(2) 0.016(2) 0.027(2) 0.0026(18) 0.0039(18) -0.0015(19) C27 0.017(2) 0.011(2) 0.022(2) -0.0024(16) 0.0027(17) 0.0051(17) C28 0.020(2) 0.016(2) 0.023(2) -0.0035(17) 0.0054(17) 0.0010(18) C29 0.016(2) 0.019(2) 0.041(3) -0.009(2) 0.0090(19) -0.0024(19) C30 0.025(3) 0.023(2) 0.032(3) -0.011(2) -0.004(2) 0.005(2) C31 0.029(3) 0.022(2) 0.019(2) -0.0028(18) -0.0030(19) 0.005(2) C32 0.024(3) 0.018(2) 0.020(2) -0.0013(17) 0.0026(18) 0.0022(19) C33 0.034(3) 0.026(3) 0.043(3) 0.012(2) 0.025(2) 0.011(2) C34 0.022(3) 0.027(3) 0.057(4) -0.010(2) 0.016(2) -0.006(2) C35 0.019(3) 0.028(3) 0.035(3) -0.002(2) 0.0024(19) 0.008(2) C36 0.026(3) 0.018(2) 0.028(2) 0.0007(18) 0.0053(19) 0.005(2) C37 0.027(3) 0.031(3) 0.027(3) 0.000(2) 0.010(2) 0.009(2) C38 0.017(2) 0.017(2) 0.016(2) 0.0015(16) 0.0054(16) 0.0018(18) C39 0.024(3) 0.021(2) 0.017(2) 0.0021(17) 0.0052(17) 0.0036(19) C40 0.020(2) 0.017(2) 0.025(2) 0.0079(18) 0.0065(18) 0.0000(18) C41 0.018(2) 0.017(2) 0.023(2) 0.0035(17) 0.0070(17) -0.0042(18) C42 0.012(2) 0.014(2) 0.021(2) 0.0017(16) 0.0077(16) 0.0014(17) C43 0.034(3) 0.029(3) 0.030(3) 0.007(2) 0.023(2) 0.011(2) C44 0.023(3) 0.033(3) 0.023(2) -0.007(2) 0.0061(18) 0.004(2) C45 0.024(3) 0.020(2) 0.030(3) -0.0018(19) 0.0105(19) 0.007(2) C46 0.015(2) 0.037(3) 0.030(3) -0.008(2) 0.0081(19) 0.006(2) C47 0.025(3) 0.025(3) 0.043(3) -0.007(2) 0.023(2) -0.003(2) C48 0.016(2) 0.012(2) 0.019(2) 0.0007(16) 0.0097(16) 0.0006(17) C49 0.017(2) 0.011(2) 0.025(2) 0.0006(17) 0.0100(17) -0.0007(17) C50 0.022(2) 0.014(2) 0.021(2) 0.0030(17) 0.0087(17) 0.0030(18) C51 0.019(2) 0.016(2) 0.016(2) 0.0003(16) 0.0049(16) 0.0010(18) C52 0.017(2) 0.015(2) 0.014(2) 0.0023(16) 0.0073(16) 0.0022(17) C53 0.017(2) 0.011(2) 0.021(2) 0.0013(16) 0.0060(17) 0.0024(17) C54 0.020(2) 0.016(2) 0.022(2) 0.0019(17) 0.0061(17) -0.0009(18) C55 0.032(3) 0.015(2) 0.018(2) 0.0001(17) 0.0042(18) 0.000(2) C56 0.025(3) 0.018(2) 0.025(2) -0.0015(18) -0.0044(18) 0.001(2) C57 0.018(2) 0.024(2) 0.030(3) -0.0014(19) 0.0047(18) -0.004(2) C58 0.019(2) 0.020(2) 0.023(2) 0.0024(18) 0.0061(18) 0.0003(19) C59 0.013(2) 0.009(2) 0.025(2) 0.0022(16) 0.0052(17) 0.0062(16) C60 0.020(2) 0.014(2) 0.025(2) 0.0025(17) 0.0069(18) 0.0011(18) C61 0.012(2) 0.018(2) 0.033(3) -0.0018(18) 0.0044(18) 0.0012(18) C62 0.019(2) 0.013(2) 0.029(3) -0.0034(18) -0.0023(18) 0.0043(18) C63 0.030(3) 0.018(2) 0.017(2) -0.0004(17) 0.0035(18) 0.002(2) C64 0.018(2) 0.012(2) 0.021(2) 0.0012(16) 0.0066(17) 0.0021(17) C65 0.031(3) 0.025(3) 0.070(4) 0.002(3) 0.012(3) 0.003(2) C66 0.024(3) 0.022(2) 0.027(2) -0.0019(19) 0.0021(19) -0.002(2) C67 0.068(5) 0.032(3) 0.064(4) -0.005(3) -0.009(3) 0.010(3) C68 0.024(3) 0.033(3) 0.032(3) 0.010(2) 0.006(2) 0.002(2) Cl1 0.0506(9) 0.0210(6) 0.0810(11) 0.0076(6) 0.0214(7) 0.0057(6) Cl2 0.0371(8) 0.0228(6) 0.0720(10) -0.0059(6) -0.0076(6) -0.0017(6) Cl3 0.0495(9) 0.0273(7) 0.0732(10) -0.0002(6) -0.0153(7) -0.0042(6) Cl4 0.145(2) 0.0796(13) 0.0297(8) 0.0191(8) -0.0325(10) -0.0414(13) Cl5 0.0377(7) 0.0232(6) 0.0361(7) -0.0027(5) 0.0030(5) -0.0090(5) Cl6 0.0621(10) 0.0219(7) 0.0685(10) -0.0145(6) -0.0268(7) 0.0133(6) Cl7 0.0461(8) 0.0288(7) 0.0481(8) 0.0038(5) 0.0158(6) 0.0168(6) Cl8 0.0354(7) 0.0292(6) 0.0427(7) 0.0055(5) -0.0062(5) -0.0077(5) Cl9 0.0504(9) 0.0310(7) 0.0573(9) -0.0091(6) -0.0153(7) 0.0037(6) Cl10 0.0357(7) 0.0237(6) 0.0461(7) 0.0045(5) 0.0029(5) 0.0066(5) Cl11 0.0363(8) 0.0211(7) 0.1141(14) -0.0090(7) 0.0071(8) -0.0026(6) Cl12 0.0238(7) 0.0756(10) 0.0273(6) 0.0122(6) 0.0009(5) 0.0043(6) F1 0.0326(17) 0.0444(18) 0.0312(15) -0.0055(13) 0.0093(12) -0.0211(14) F2 0.0365(17) 0.0217(14) 0.0299(15) -0.0037(11) 0.0099(11) -0.0124(12) F3 0.0421(18) 0.0287(15) 0.0193(14) -0.0017(11) 0.0063(11) -0.0116(13) F4 0.0378(17) 0.0190(14) 0.0399(16) 0.0028(11) 0.0053(12) 0.0074(12) F5 0.0292(15) 0.0348(15) 0.0192(13) -0.0007(11) 0.0041(10) -0.0060(12) F6 0.046(2) 0.0395(18) 0.0466(18) 0.0061(14) 0.0182(14) 0.0240(15) F7 0.0385(19) 0.086(3) 0.0321(17) -0.0172(16) 0.0064(13) -0.0092(18) F8 0.0395(19) 0.069(2) 0.0335(17) -0.0129(15) 0.0124(13) -0.0003(16) F9 0.051(2) 0.0262(17) 0.081(3) 0.0104(16) -0.0015(17) -0.0005(15) F10 0.0191(16) 0.0516(19) 0.0517(19) 0.0087(15) 0.0047(13) -0.0001(14) F11 0.043(2) 0.0300(17) 0.070(2) 0.0136(15) -0.0041(16) -0.0033(15) F12 0.0220(16) 0.0455(18) 0.0394(17) 0.0028(13) 0.0000(12) 0.0008(13) Fe1 0.0148(4) 0.0102(3) 0.0183(3) 0.0017(2) 0.0047(3) 0.0011(3) Fe2 0.0150(4) 0.0099(3) 0.0168(3) 0.0002(2) 0.0035(2) 0.0009(3) Fe3 0.0154(4) 0.0107(3) 0.0192(4) 0.0021(3) 0.0022(3) 0.0002(3) Fe4 0.0148(4) 0.0111(3) 0.0171(3) -0.0002(2) 0.0057(2) 0.0012(3) P1 0.0207(6) 0.0144(5) 0.0196(6) 0.0001(4) 0.0032(4) -0.0017(4) P2 0.0209(6) 0.0223(6) 0.0263(6) 0.0010(5) 0.0019(5) 0.0014(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 B1 C20 1.543(6) . ? B1 C27 1.556(6) . ? B1 C10 1.562(6) . ? B2 C16 1.528(6) . ? B2 C6 1.559(6) . ? B2 C21 1.561(6) . ? B3 C52 1.531(6) . ? B3 C59 1.567(6) . ? B3 C42 1.570(6) . ? B4 C48 1.525(6) . ? B4 C53 1.563(6) . ? B4 C38 1.568(6) . ? C1 C2 1.410(8) . ? C1 C5 1.422(7) . ? C1 Fe1 2.092(4) . ? C2 C3 1.420(7) . ? C2 Fe1 2.094(5) . ? C3 C4 1.412(7) . ? C3 Fe1 2.091(5) . ? C4 C5 1.417(7) . ? C4 Fe1 2.084(4) . ? C5 Fe1 2.082(5) . ? C6 C7 1.441(6) . ? C6 C10 1.452(6) . ? C6 Fe1 2.065(4) . ? C7 C8 1.416(6) . ? C7 Fe1 2.077(4) . ? C8 C9 1.420(6) . ? C8 Fe1 2.100(4) . ? C9 C10 1.432(6) . ? C9 Fe1 2.099(4) . ? C10 Fe1 2.078(4) . ? C11 C15 1.416(7) . ? C11 C12 1.423(6) . ? C11 Fe2 2.079(4) . ? C12 C13 1.423(7) . ? C12 Fe2 2.047(4) . ? C13 C14 1.414(7) . ? C13 Fe2 2.036(5) . ? C14 C15 1.421(7) . ? C14 Fe2 2.058(5) . ? C15 Fe2 2.076(5) . ? C16 C17 1.442(6) . ? C16 C20 1.466(6) . ? C16 Fe2 2.028(4) . ? C17 C18 1.407(6) . ? C17 Fe2 2.054(4) . ? C18 C19 1.415(6) . ? C18 Fe2 2.077(4) . ? C19 C20 1.442(6) . ? C19 Fe2 2.048(4) . ? C20 Fe2 2.023(4) . ? C21 C22 1.397(6) . ? C21 C26 1.410(6) . ? C22 C23 1.390(6) . ? C23 C24 1.387(7) . ? C24 C25 1.383(7) . ? C25 C26 1.381(7) . ? C27 C28 1.407(6) . ? C27 C32 1.408(6) . ? C28 C29 1.384(6) . ? C29 C30 1.401(7) . ? C30 C31 1.380(7) . ? C31 C32 1.387(6) . ? C33 C34 1.402(8) . ? C33 C37 1.406(7) . ? C33 Fe3 2.092(5) . ? C34 C35 1.428(7) . ? C34 Fe3 2.089(5) . ? C35 C36 1.409(7) . ? C35 Fe3 2.084(5) . ? C36 C37 1.428(7) . ? C36 Fe3 2.092(4) . ? C37 Fe3 2.087(5) . ? C38 C39 1.431(6) . ? C38 C42 1.455(6) . ? C38 Fe3 2.065(4) . ? C39 C40 1.413(6) . ? C39 Fe3 2.098(4) . ? C40 C41 1.409(6) . ? C40 Fe3 2.123(4) . ? C41 C42 1.435(6) . ? C41 Fe3 2.100(4) . ? C42 Fe3 2.074(4) . ? C43 C47 1.408(7) . ? C43 C44 1.414(7) . ? C43 Fe4 2.068(4) . ? C44 C45 1.422(7) . ? C44 Fe4 2.039(4) . ? C45 C46 1.411(7) . ? C45 Fe4 2.044(4) . ? C46 C47 1.423(7) . ? C46 Fe4 2.057(5) . ? C47 Fe4 2.067(5) . ? C48 C49 1.447(6) . ? C48 C52 1.465(6) . ? C48 Fe4 2.017(4) . ? C49 C50 1.409(6) . ? C49 Fe4 2.057(4) . ? C50 C51 1.425(6) . ? C50 Fe4 2.076(4) . ? C51 C52 1.444(6) . ? C51 Fe4 2.061(4) . ? C52 Fe4 2.026(4) . ? C53 C54 1.395(6) . ? C53 C58 1.406(6) . ? C54 C55 1.387(6) . ? C55 C56 1.397(7) . ? C56 C57 1.384(7) . ? C57 C58 1.391(6) . ? C59 C64 1.396(6) . ? C59 C60 1.409(6) . ? C60 C61 1.388(6) . ? C61 C62 1.373(7) . ? C62 C63 1.395(7) . ? C63 C64 1.394(6) . ? C65 Cl1 1.743(5) . ? C65 Cl2 1.758(6) . ? C65 Cl3 1.812(6) . ? C66 Cl6 1.731(5) . ? C66 Cl4 1.742(5) . ? C66 Cl5 1.759(5) . ? C67 Cl9 1.702(7) . ? C67 Cl7 1.758(6) . ? C67 Cl8 1.775(7) . ? C68 Cl12 1.755(5) . ? C68 Cl10 1.757(5) . ? C68 Cl11 1.762(5) . ? F1 P1 1.597(3) . ? F2 P1 1.600(3) . ? F3 P1 1.614(3) . ? F4 P1 1.598(3) . ? F5 P1 1.597(3) . ? F6 P1 1.583(3) . ? F7 P2 1.612(3) . ? F8 P2 1.593(3) . ? F9 P2 1.583(3) . ? F10 P2 1.595(3) . ? F11 P2 1.584(3) . ? F12 P2 1.610(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 B1 C27 122.6(4) . . ? C20 B1 C10 115.2(4) . . ? C27 B1 C10 122.2(4) . . ? C16 B2 C6 115.5(4) . . ? C16 B2 C21 121.9(4) . . ? C6 B2 C21 122.6(4) . . ? C52 B3 C59 122.2(4) . . ? C52 B3 C42 115.1(4) . . ? C59 B3 C42 122.7(4) . . ? C48 B4 C53 121.5(4) . . ? C48 B4 C38 115.2(4) . . ? C53 B4 C38 123.3(4) . . ? C2 C1 C5 108.3(4) . . ? C2 C1 Fe1 70.4(3) . . ? C5 C1 Fe1 69.7(3) . . ? C1 C2 C3 107.8(4) . . ? C1 C2 Fe1 70.2(3) . . ? C3 C2 Fe1 70.0(3) . . ? C4 C3 C2 108.2(4) . . ? C4 C3 Fe1 70.0(3) . . ? C2 C3 Fe1 70.3(3) . . ? C3 C4 C5 108.2(4) . . ? C3 C4 Fe1 70.5(3) . . ? C5 C4 Fe1 70.1(3) . . ? C4 C5 C1 107.6(4) . . ? C4 C5 Fe1 70.2(3) . . ? C1 C5 Fe1 70.4(3) . . ? C7 C6 C10 107.4(4) . . ? C7 C6 B2 129.9(4) . . ? C10 C6 B2 121.8(4) . . ? C7 C6 Fe1 70.1(2) . . ? C10 C6 Fe1 70.0(2) . . ? B2 C6 Fe1 116.9(3) . . ? C8 C7 C6 108.5(4) . . ? C8 C7 Fe1 71.1(2) . . ? C6 C7 Fe1 69.2(2) . . ? C7 C8 C9 108.2(4) . . ? C7 C8 Fe1 69.3(2) . . ? C9 C8 Fe1 70.2(2) . . ? C8 C9 C10 109.2(4) . . ? C8 C9 Fe1 70.3(2) . . ? C10 C9 Fe1 69.1(2) . . ? C9 C10 C6 106.8(4) . . ? C9 C10 B1 130.6(4) . . ? C6 C10 B1 122.1(4) . . ? C9 C10 Fe1 70.8(2) . . ? C6 C10 Fe1 69.0(2) . . ? B1 C10 Fe1 118.7(3) . . ? C15 C11 C12 107.4(4) . . ? C15 C11 Fe2 70.0(3) . . ? C12 C11 Fe2 68.6(2) . . ? C13 C12 C11 108.0(4) . . ? C13 C12 Fe2 69.2(3) . . ? C11 C12 Fe2 71.0(2) . . ? C14 C13 C12 108.2(4) . . ? C14 C13 Fe2 70.6(3) . . ? C12 C13 Fe2 70.0(3) . . ? C13 C14 C15 107.6(4) . . ? C13 C14 Fe2 69.0(3) . . ? C15 C14 Fe2 70.6(3) . . ? C11 C15 C14 108.7(4) . . ? C11 C15 Fe2 70.2(3) . . ? C14 C15 Fe2 69.2(3) . . ? C17 C16 C20 106.5(4) . . ? C17 C16 B2 126.1(4) . . ? C20 C16 B2 122.8(4) . . ? C17 C16 Fe2 70.3(2) . . ? C20 C16 Fe2 68.6(2) . . ? B2 C16 Fe2 106.8(3) . . ? C18 C17 C16 109.2(4) . . ? C18 C17 Fe2 71.0(3) . . ? C16 C17 Fe2 68.4(2) . . ? C17 C18 C19 108.7(4) . . ? C17 C18 Fe2 69.2(2) . . ? C19 C18 Fe2 68.8(2) . . ? C18 C19 C20 108.7(4) . . ? C18 C19 Fe2 71.0(2) . . ? C20 C19 Fe2 68.3(2) . . ? C19 C20 C16 106.9(4) . . ? C19 C20 B1 126.7(4) . . ? C16 C20 B1 121.7(4) . . ? C19 C20 Fe2 70.2(2) . . ? C16 C20 Fe2 68.9(2) . . ? B1 C20 Fe2 106.4(3) . . ? C22 C21 C26 116.9(4) . . ? C22 C21 B2 122.6(4) . . ? C26 C21 B2 120.5(4) . . ? C23 C22 C21 121.5(4) . . ? C24 C23 C22 120.0(4) . . ? C25 C24 C23 119.8(4) . . ? C26 C25 C24 119.9(4) . . ? C25 C26 C21 121.8(4) . . ? C28 C27 C32 117.0(4) . . ? C28 C27 B1 123.4(4) . . ? C32 C27 B1 119.6(4) . . ? C29 C28 C27 121.5(4) . . ? C28 C29 C30 120.0(4) . . ? C31 C30 C29 119.6(4) . . ? C30 C31 C32 120.2(4) . . ? C31 C32 C27 121.7(4) . . ? C34 C33 C37 109.0(4) . . ? C34 C33 Fe3 70.3(3) . . ? C37 C33 Fe3 70.1(3) . . ? C33 C34 C35 107.8(4) . . ? C33 C34 Fe3 70.5(3) . . ? C35 C34 Fe3 69.8(3) . . ? C36 C35 C34 107.7(4) . . ? C36 C35 Fe3 70.6(3) . . ? C34 C35 Fe3 70.2(3) . . ? C35 C36 C37 108.0(4) . . ? C35 C36 Fe3 70.0(3) . . ? C37 C36 Fe3 69.8(3) . . ? C33 C37 C36 107.5(4) . . ? C33 C37 Fe3 70.5(3) . . ? C36 C37 Fe3 70.2(3) . . ? C39 C38 C42 106.9(4) . . ? C39 C38 B4 130.6(4) . . ? C42 C38 B4 121.8(4) . . ? C39 C38 Fe3 71.1(2) . . ? C42 C38 Fe3 69.8(2) . . ? B4 C38 Fe3 117.2(3) . . ? C40 C39 C38 108.9(4) . . ? C40 C39 Fe3 71.4(2) . . ? C38 C39 Fe3 68.7(2) . . ? C41 C40 C39 108.5(4) . . ? C41 C40 Fe3 69.6(2) . . ? C39 C40 Fe3 69.5(2) . . ? C40 C41 C42 108.8(4) . . ? C40 C41 Fe3 71.4(3) . . ? C42 C41 Fe3 68.9(2) . . ? C41 C42 C38 107.0(4) . . ? C41 C42 B3 130.7(4) . . ? C38 C42 B3 122.1(4) . . ? C41 C42 Fe3 70.8(2) . . ? C38 C42 Fe3 69.1(2) . . ? B3 C42 Fe3 120.5(3) . . ? C47 C43 C44 107.8(4) . . ? C47 C43 Fe4 70.0(3) . . ? C44 C43 Fe4 68.8(3) . . ? C43 C44 C45 108.1(4) . . ? C43 C44 Fe4 70.9(3) . . ? C45 C44 Fe4 69.8(3) . . ? C46 C45 C44 107.9(4) . . ? C46 C45 Fe4 70.4(3) . . ? C44 C45 Fe4 69.5(3) . . ? C45 C46 C47 107.6(4) . . ? C45 C46 Fe4 69.3(3) . . ? C47 C46 Fe4 70.2(3) . . ? C43 C47 C46 108.5(4) . . ? C43 C47 Fe4 70.1(3) . . ? C46 C47 Fe4 69.5(3) . . ? C49 C48 C52 106.9(4) . . ? C49 C48 B4 124.0(4) . . ? C52 C48 B4 122.9(4) . . ? C49 C48 Fe4 70.7(2) . . ? C52 C48 Fe4 69.1(2) . . ? B4 C48 Fe4 103.1(3) . . ? C50 C49 C48 108.8(4) . . ? C50 C49 Fe4 70.8(2) . . ? C48 C49 Fe4 67.7(2) . . ? C49 C50 C51 108.8(4) . . ? C49 C50 Fe4 69.4(2) . . ? C51 C50 Fe4 69.3(2) . . ? C50 C51 C52 108.6(4) . . ? C50 C51 Fe4 70.4(2) . . ? C52 C51 Fe4 68.0(2) . . ? C51 C52 C48 106.9(3) . . ? C51 C52 B3 126.4(4) . . ? C48 C52 B3 122.4(4) . . ? C51 C52 Fe4 70.6(2) . . ? C48 C52 Fe4 68.4(2) . . ? B3 C52 Fe4 107.6(3) . . ? C54 C53 C58 116.9(4) . . ? C54 C53 B4 123.2(4) . . ? C58 C53 B4 119.9(4) . . ? C55 C54 C53 122.1(4) . . ? C54 C55 C56 119.8(4) . . ? C57 C56 C55 119.4(4) . . ? C56 C57 C58 120.1(4) . . ? C57 C58 C53 121.6(4) . . ? C64 C59 C60 117.2(4) . . ? C64 C59 B3 120.0(4) . . ? C60 C59 B3 122.8(4) . . ? C61 C60 C59 120.8(4) . . ? C62 C61 C60 120.8(4) . . ? C61 C62 C63 119.9(4) . . ? C64 C63 C62 119.2(4) . . ? C63 C64 C59 122.0(4) . . ? Cl1 C65 Cl2 110.9(3) . . ? Cl1 C65 Cl3 109.2(3) . . ? Cl2 C65 Cl3 109.4(3) . . ? Cl6 C66 Cl4 110.8(3) . . ? Cl6 C66 Cl5 112.1(3) . . ? Cl4 C66 Cl5 110.0(3) . . ? Cl9 C67 Cl7 114.0(4) . . ? Cl9 C67 Cl8 112.1(4) . . ? Cl7 C67 Cl8 110.2(4) . . ? Cl12 C68 Cl10 110.1(3) . . ? Cl12 C68 Cl11 110.9(3) . . ? Cl10 C68 Cl11 108.4(3) . . ? C6 Fe1 C7 40.72(16) . . ? C6 Fe1 C10 41.03(16) . . ? C7 Fe1 C10 68.27(17) . . ? C6 Fe1 C5 141.96(18) . . ? C7 Fe1 C5 176.79(19) . . ? C10 Fe1 C5 114.92(18) . . ? C6 Fe1 C4 176.88(18) . . ? C7 Fe1 C4 137.43(18) . . ? C10 Fe1 C4 142.07(18) . . ? C5 Fe1 C4 39.8(2) . . ? C6 Fe1 C3 137.38(18) . . ? C7 Fe1 C3 110.22(18) . . ? C10 Fe1 C3 178.35(18) . . ? C5 Fe1 C3 66.60(19) . . ? C4 Fe1 C3 39.52(19) . . ? C6 Fe1 C1 113.28(17) . . ? C7 Fe1 C1 139.93(19) . . ? C10 Fe1 C1 114.35(18) . . ? C5 Fe1 C1 39.8(2) . . ? C4 Fe1 C1 66.54(19) . . ? C3 Fe1 C1 66.29(19) . . ? C6 Fe1 C2 111.18(17) . . ? C7 Fe1 C2 111.25(19) . . ? C10 Fe1 C2 139.89(18) . . ? C5 Fe1 C2 66.7(2) . . ? C4 Fe1 C2 66.57(19) . . ? C3 Fe1 C2 39.7(2) . . ? C1 Fe1 C2 39.4(2) . . ? C6 Fe1 C9 67.55(16) . . ? C7 Fe1 C9 66.72(17) . . ? C10 Fe1 C9 40.10(16) . . ? C5 Fe1 C9 115.32(19) . . ? C4 Fe1 C9 114.64(18) . . ? C3 Fe1 C9 140.25(18) . . ? C1 Fe1 C9 142.43(19) . . ? C2 Fe1 C9 177.95(19) . . ? C6 Fe1 C8 67.64(16) . . ? C7 Fe1 C8 39.63(17) . . ? C10 Fe1 C8 67.60(17) . . ? C5 Fe1 C8 140.42(19) . . ? C4 Fe1 C8 112.43(18) . . ? C3 Fe1 C8 111.74(18) . . ? C1 Fe1 C8 177.9(2) . . ? C2 Fe1 C8 138.7(2) . . ? C9 Fe1 C8 39.52(17) . . ? C20 Fe2 C16 42.44(17) . . ? C20 Fe2 C13 158.77(18) . . ? C16 Fe2 C13 154.02(18) . . ? C20 Fe2 C12 160.25(18) . . ? C16 Fe2 C12 121.60(18) . . ? C13 Fe2 C12 40.77(19) . . ? C20 Fe2 C19 41.49(17) . . ? C16 Fe2 C19 69.93(17) . . ? C13 Fe2 C19 119.62(18) . . ? C12 Fe2 C19 156.18(18) . . ? C20 Fe2 C17 69.71(17) . . ? C16 Fe2 C17 41.37(16) . . ? C13 Fe2 C17 116.47(18) . . ? C12 Fe2 C17 105.82(18) . . ? C19 Fe2 C17 68.00(18) . . ? C20 Fe2 C14 125.23(18) . . ? C16 Fe2 C14 165.37(18) . . ? C13 Fe2 C14 40.40(19) . . ? C12 Fe2 C14 68.06(19) . . ? C19 Fe2 C14 105.68(19) . . ? C17 Fe2 C14 151.19(18) . . ? C20 Fe2 C15 111.98(17) . . ? C16 Fe2 C15 129.94(18) . . ? C13 Fe2 C15 67.60(19) . . ? C12 Fe2 C15 67.41(18) . . ? C19 Fe2 C15 123.51(19) . . ? C17 Fe2 C15 165.35(19) . . ? C14 Fe2 C15 40.2(2) . . ? C20 Fe2 C18 68.99(17) . . ? C16 Fe2 C18 68.92(17) . . ? C13 Fe2 C18 102.12(18) . . ? C12 Fe2 C18 120.59(18) . . ? C19 Fe2 C18 40.12(17) . . ? C17 Fe2 C18 39.83(17) . . ? C14 Fe2 C18 117.28(19) . . ? C15 Fe2 C18 154.82(19) . . ? C20 Fe2 C11 126.28(17) . . ? C16 Fe2 C11 111.58(17) . . ? C13 Fe2 C11 68.05(18) . . ? C12 Fe2 C11 40.35(18) . . ? C19 Fe2 C11 160.54(18) . . ? C17 Fe2 C11 126.76(18) . . ? C14 Fe2 C11 67.72(19) . . ? C15 Fe2 C11 39.84(19) . . ? C18 Fe2 C11 159.34(18) . . ? C38 Fe3 C42 41.14(16) . . ? C38 Fe3 C35 136.05(18) . . ? C42 Fe3 C35 176.73(18) . . ? C38 Fe3 C37 143.10(17) . . ? C42 Fe3 C37 114.50(18) . . ? C35 Fe3 C37 66.79(19) . . ? C38 Fe3 C34 110.68(18) . . ? C42 Fe3 C34 137.22(19) . . ? C35 Fe3 C34 40.0(2) . . ? C37 Fe3 C34 66.4(2) . . ? C38 Fe3 C36 175.36(18) . . ? C42 Fe3 C36 143.41(18) . . ? C35 Fe3 C36 39.44(19) . . ? C37 Fe3 C36 39.96(18) . . ? C34 Fe3 C36 66.46(19) . . ? C38 Fe3 C33 114.17(18) . . ? C42 Fe3 C33 112.50(18) . . ? C35 Fe3 C33 66.4(2) . . ? C37 Fe3 C33 39.3(2) . . ? C34 Fe3 C33 39.2(2) . . ? C36 Fe3 C33 66.19(19) . . ? C38 Fe3 C39 40.20(16) . . ? C42 Fe3 C39 67.52(17) . . ? C35 Fe3 C39 111.35(18) . . ? C37 Fe3 C39 176.59(18) . . ? C34 Fe3 C39 114.25(19) . . ? C36 Fe3 C39 136.83(17) . . ? C33 Fe3 C39 143.2(2) . . ? C38 Fe3 C41 67.77(17) . . ? C42 Fe3 C41 40.21(16) . . ? C35 Fe3 C41 142.58(18) . . ? C37 Fe3 C41 113.43(19) . . ? C34 Fe3 C41 177.3(2) . . ? C36 Fe3 C41 115.24(18) . . ? C33 Fe3 C41 139.0(2) . . ? C39 Fe3 C41 66.12(17) . . ? C38 Fe3 C40 67.06(16) . . ? C42 Fe3 C40 66.85(16) . . ? C35 Fe3 C40 114.40(19) . . ? C37 Fe3 C40 138.47(19) . . ? C34 Fe3 C40 142.9(2) . . ? C36 Fe3 C40 112.77(18) . . ? C33 Fe3 C40 177.5(2) . . ? C39 Fe3 C40 39.12(17) . . ? C41 Fe3 C40 38.98(17) . . ? C48 Fe4 C52 42.47(17) . . ? C48 Fe4 C44 119.36(18) . . ? C52 Fe4 C44 156.32(18) . . ? C48 Fe4 C45 149.69(18) . . ? C52 Fe4 C45 162.77(18) . . ? C44 Fe4 C45 40.77(19) . . ? C48 Fe4 C49 41.60(16) . . ? C52 Fe4 C49 69.90(16) . . ? C44 Fe4 C49 106.65(18) . . ? C45 Fe4 C49 113.24(18) . . ? C48 Fe4 C46 170.04(18) . . ? C52 Fe4 C46 128.31(18) . . ? C44 Fe4 C46 68.02(19) . . ? C45 Fe4 C46 40.26(19) . . ? C49 Fe4 C46 145.79(18) . . ? C48 Fe4 C51 69.89(17) . . ? C52 Fe4 C51 41.37(16) . . ? C44 Fe4 C51 160.67(18) . . ? C45 Fe4 C51 122.60(18) . . ? C49 Fe4 C51 68.06(17) . . ? C46 Fe4 C51 105.32(18) . . ? C48 Fe4 C47 133.79(18) . . ? C52 Fe4 C47 112.25(18) . . ? C44 Fe4 C47 67.48(19) . . ? C45 Fe4 C47 67.64(19) . . ? C49 Fe4 C47 170.54(19) . . ? C46 Fe4 C47 40.4(2) . . ? C51 Fe4 C47 119.99(19) . . ? C48 Fe4 C43 112.94(18) . . ? C52 Fe4 C43 123.90(17) . . ? C44 Fe4 C43 40.3(2) . . ? C45 Fe4 C43 67.91(19) . . ? C49 Fe4 C43 131.0(2) . . ? C46 Fe4 C43 67.7(2) . . ? C51 Fe4 C43 155.85(19) . . ? C47 Fe4 C43 39.8(2) . . ? C48 Fe4 C50 69.13(17) . . ? C52 Fe4 C50 69.17(16) . . ? C44 Fe4 C50 123.97(18) . . ? C45 Fe4 C50 101.89(18) . . ? C49 Fe4 C50 39.86(17) . . ? C46 Fe4 C50 113.26(18) . . ? C51 Fe4 C50 40.28(17) . . ? C47 Fe4 C50 149.5(2) . . ? C43 Fe4 C50 163.82(19) . . ? F6 P1 F1 90.78(18) . . ? F6 P1 F5 90.26(16) . . ? F1 P1 F5 90.69(15) . . ? F6 P1 F4 179.8(2) . . ? F1 P1 F4 89.29(16) . . ? F5 P1 F4 89.94(15) . . ? F6 P1 F2 90.56(17) . . ? F1 P1 F2 178.45(17) . . ? F5 P1 F2 90.08(14) . . ? F4 P1 F2 89.37(15) . . ? F6 P1 F3 89.94(16) . . ? F1 P1 F3 89.20(14) . . ? F5 P1 F3 179.77(18) . . ? F4 P1 F3 89.86(15) . . ? F2 P1 F3 90.03(14) . . ? F9 P2 F11 179.1(2) . . ? F9 P2 F8 90.0(2) . . ? F11 P2 F8 90.4(2) . . ? F9 P2 F10 90.27(18) . . ? F11 P2 F10 90.55(17) . . ? F8 P2 F10 91.64(17) . . ? F9 P2 F12 89.50(18) . . ? F11 P2 F12 89.67(17) . . ? F8 P2 F12 89.85(16) . . ? F10 P2 F12 178.49(18) . . ? F9 P2 F7 90.6(2) . . ? F11 P2 F7 89.1(2) . . ? F8 P2 F7 179.0(2) . . ? F10 P2 F7 89.16(17) . . ? F12 P2 F7 89.35(17) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 64.99 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.644 _refine_diff_density_min -0.897 _refine_diff_density_rms 0.097 #===END data_22+(i3)2 _database_code_depnum_ccdc_archive 'CCDC 635885' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H38 B2 Fe2 I6 N4' _chemical_formula_sum 'C40 H38 B2 Fe2 I6 N4' _chemical_formula_weight 1469.46 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' B B 0.0090 0.0039 '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' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7183(9) _cell_length_b 8.9579(7) _cell_length_c 21.3539(15) _cell_angle_alpha 90.00 _cell_angle_beta 92.612(4) _cell_angle_gamma 90.00 _cell_volume 2239.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5280 _cell_measurement_theta_min 4.14 _cell_measurement_theta_max 67.36 _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 37.924 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.0334 _exptl_absorpt_correction_T_max 0.0645 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 CCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14152 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 67.74 _reflns_number_total 3956 _reflns_number_gt 3712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT-Plus (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2000)' _computing_publication_material SHELXTL _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^)+(0.0911P)^2^+1.1316P] 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_number_reflns 3956 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1193 _refine_ls_wR_factor_gt 0.1172 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.005 _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 B1 B 0.6314(5) 0.5572(7) 1.0148(2) 0.0320(11) Uani 1 1 d . . . C1 C 0.5425(5) 0.5408(6) 0.8248(2) 0.0410(12) Uani 1 1 d . . . H1 H 0.5740 0.4398 0.8356 0.049 Uiso 1 1 calc R . . C2 C 0.6055(5) 0.6760(7) 0.8237(2) 0.0424(13) Uani 1 1 d . . . H2 H 0.6893 0.6871 0.8334 0.051 Uiso 1 1 calc R . . C3 C 0.5293(5) 0.7914(7) 0.8036(2) 0.0403(12) Uani 1 1 d . . . H3 H 0.5495 0.8988 0.7976 0.048 Uiso 1 1 calc R . . C4 C 0.4208(5) 0.7273(7) 0.7925(2) 0.0407(12) Uani 1 1 d . . . H4 H 0.3500 0.7823 0.7783 0.049 Uiso 1 1 calc R . . C5 C 0.4275(5) 0.5740(7) 0.8056(2) 0.0399(12) Uani 1 1 d . . . H5 H 0.3631 0.5008 0.8015 0.048 Uiso 1 1 calc R . . C6 C 0.5315(4) 0.6586(6) 0.9831(2) 0.0318(10) Uani 1 1 d . . . C7 C 0.5361(5) 0.8119(6) 0.9647(2) 0.0348(11) Uani 1 1 d . . . H7 H 0.6062 0.8757 0.9670 0.042 Uiso 1 1 calc R . . C8 C 0.4263(5) 0.8607(6) 0.9445(2) 0.0363(11) Uani 1 1 d . . . H8 H 0.4045 0.9644 0.9313 0.044 Uiso 1 1 calc R . . C9 C 0.3506(5) 0.7353(6) 0.9487(2) 0.0352(11) Uani 1 1 d . . . H9 H 0.2668 0.7360 0.9377 0.042 Uiso 1 1 calc R . . C10 C 0.4142(4) 0.6114(6) 0.9731(2) 0.0310(10) Uani 1 1 d . . . C11 C 0.6881(4) 0.6322(6) 1.0777(2) 0.0322(10) Uani 1 1 d . . . C12 C 0.6291(4) 0.7444(6) 1.1103(2) 0.0337(10) Uani 1 1 d . . . H12 H 0.5559 0.7760 1.0945 0.040 Uiso 1 1 calc R . . C13 C 0.6762(5) 0.8090(6) 1.1649(2) 0.0354(11) Uani 1 1 d . . . H13 H 0.6350 0.8840 1.1858 0.043 Uiso 1 1 calc R . . C14 C 0.7824(5) 0.7650(6) 1.1891(2) 0.0378(11) Uani 1 1 d . . . H14 H 0.8151 0.8112 1.2257 0.045 Uiso 1 1 calc R . . C15 C 0.8409(5) 0.6523(7) 1.1593(3) 0.0406(12) Uani 1 1 d . . . H15 H 0.9126 0.6188 1.1765 0.049 Uiso 1 1 calc R . . C16 C 0.7944(4) 0.5879(7) 1.1038(2) 0.0363(11) Uani 1 1 d . . . H16 H 0.8361 0.5125 1.0835 0.044 Uiso 1 1 calc R . . C17 C 0.8008(5) 0.5183(6) 0.9338(2) 0.0362(11) Uani 1 1 d . . . C18 C 0.8910(5) 0.4971(7) 0.8898(3) 0.0432(12) Uani 1 1 d . . . H18A H 0.9273 0.5933 0.8816 0.065 Uiso 1 1 calc R . . H18B H 0.8583 0.4561 0.8505 0.065 Uiso 1 1 calc R . . H18C H 0.9483 0.4278 0.9078 0.065 Uiso 1 1 calc R . . C19 C 0.9436(6) 0.8120(9) 0.0122(3) 0.0568(17) Uani 1 1 d . . . C20 C 0.8619(6) 0.9303(9) 0.0311(3) 0.0573(17) Uani 1 1 d . . . H20A H 0.8343 0.9860 -0.0061 0.086 Uiso 1 1 calc R . . H20B H 0.9008 0.9987 0.0608 0.086 Uiso 1 1 calc R . . H20C H 0.7971 0.8837 0.0510 0.086 Uiso 1 1 calc R . . Fe1 Fe 0.47835(7) 0.69340(9) 0.88719(3) 0.0312(2) Uani 1 1 d . . . I1 I 0.69285(3) 1.14554(4) 0.878471(15) 0.03655(15) Uani 1 1 d . . . I2 I 0.89186(3) 0.97120(4) 0.839289(13) 0.03446(14) Uani 1 1 d . . . I3 I 1.08535(3) 0.80167(4) 0.801166(17) 0.04357(15) Uani 1 1 d . . . N1 N 0.7312(4) 0.5396(5) 0.96701(18) 0.0328(9) Uani 1 1 d . . . N2 N 1.0091(7) 0.7245(7) -0.0044(3) 0.0663(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.035(3) 0.037(3) 0.025(2) -0.002(2) 0.008(2) 0.001(2) C1 0.059(3) 0.038(3) 0.027(2) 0.000(2) 0.013(2) 0.011(3) C2 0.045(3) 0.057(3) 0.025(2) 0.002(2) 0.007(2) -0.003(3) C3 0.056(3) 0.041(3) 0.024(2) 0.001(2) 0.005(2) -0.009(3) C4 0.056(3) 0.043(3) 0.024(2) 0.001(2) 0.006(2) 0.004(3) C5 0.056(3) 0.040(3) 0.025(2) -0.002(2) 0.011(2) -0.006(3) C6 0.037(2) 0.038(3) 0.021(2) -0.0026(19) 0.0050(18) -0.004(2) C7 0.049(3) 0.031(3) 0.025(2) -0.0006(19) 0.008(2) -0.002(2) C8 0.051(3) 0.032(3) 0.027(2) -0.0035(19) 0.007(2) 0.003(2) C9 0.045(3) 0.037(3) 0.023(2) -0.002(2) 0.0036(19) 0.005(2) C10 0.034(2) 0.039(3) 0.0208(19) -0.0012(19) 0.0093(17) 0.001(2) C11 0.041(3) 0.032(3) 0.024(2) 0.0022(19) 0.0083(19) -0.002(2) C12 0.039(2) 0.034(3) 0.029(2) 0.003(2) 0.0055(19) 0.002(2) C13 0.046(3) 0.031(3) 0.030(2) 0.001(2) 0.011(2) 0.003(2) C14 0.046(3) 0.041(3) 0.026(2) -0.001(2) 0.005(2) -0.010(2) C15 0.036(3) 0.052(3) 0.034(3) 0.000(2) 0.002(2) 0.002(2) C16 0.038(2) 0.043(3) 0.029(2) -0.002(2) 0.0059(19) 0.004(2) C17 0.042(3) 0.039(3) 0.028(2) -0.001(2) 0.004(2) -0.001(2) C18 0.041(3) 0.052(3) 0.038(3) -0.002(2) 0.013(2) -0.001(3) C19 0.063(4) 0.061(4) 0.047(3) 0.011(3) 0.000(3) -0.015(4) C20 0.051(3) 0.077(5) 0.045(3) 0.009(3) 0.007(3) -0.018(3) Fe1 0.0404(4) 0.0309(4) 0.0227(3) 0.0010(3) 0.0052(3) -0.0002(3) I1 0.0393(2) 0.0360(2) 0.0349(2) -0.00012(12) 0.00760(14) 0.00279(13) I2 0.0386(2) 0.0356(2) 0.0295(2) -0.00047(12) 0.00509(14) 0.00090(13) I3 0.0426(2) 0.0459(3) 0.0427(2) -0.00297(15) 0.00754(16) 0.00725(15) N1 0.036(2) 0.037(2) 0.0252(19) -0.0006(17) 0.0050(17) -0.0021(18) N2 0.092(5) 0.051(3) 0.055(3) -0.003(3) -0.009(3) 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N1 1.594(6) . ? B1 C6 1.607(8) . ? B1 C11 1.617(7) . ? B1 C10 1.626(8) 3_667 ? C1 C2 1.419(9) . ? C1 C5 1.422(8) . ? C1 Fe1 2.073(5) . ? C2 C3 1.420(9) . ? C2 Fe1 2.064(6) . ? C3 C4 1.405(9) . ? C3 Fe1 2.100(5) . ? C4 C5 1.403(8) . ? C4 Fe1 2.125(5) . ? C5 Fe1 2.107(5) . ? C6 C7 1.430(7) . ? C6 C10 1.445(7) . ? C6 Fe1 2.137(5) . ? C7 C8 1.407(8) . ? C7 Fe1 2.054(5) . ? C8 C9 1.436(8) . ? C8 Fe1 2.045(5) . ? C9 C10 1.423(7) . ? C9 Fe1 2.070(5) . ? C10 B1 1.626(8) 3_667 ? C10 Fe1 2.144(5) . ? C11 C16 1.398(8) . ? C11 C12 1.420(7) . ? C12 C13 1.393(8) . ? C13 C14 1.382(8) . ? C14 C15 1.390(8) . ? C15 C16 1.405(8) . ? C17 N1 1.122(7) . ? C17 C18 1.458(7) . ? C19 N2 1.163(10) . ? C19 C20 1.496(11) . ? I1 I2 2.9590(4) . ? I2 I3 2.8772(5) . ? 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 B1 C6 109.1(4) . . ? N1 B1 C11 106.7(4) . . ? C6 B1 C11 112.3(4) . . ? N1 B1 C10 105.4(4) . 3_667 ? C6 B1 C10 110.7(4) . 3_667 ? C11 B1 C10 112.3(4) . 3_667 ? C2 C1 C5 107.7(5) . . ? C2 C1 Fe1 69.6(3) . . ? C5 C1 Fe1 71.4(3) . . ? C1 C2 C3 107.8(5) . . ? C1 C2 Fe1 70.3(3) . . ? C3 C2 Fe1 71.4(3) . . ? C4 C3 C2 107.7(5) . . ? C4 C3 Fe1 71.5(3) . . ? C2 C3 Fe1 68.7(3) . . ? C5 C4 C3 109.0(5) . . ? C5 C4 Fe1 69.9(3) . . ? C3 C4 Fe1 69.6(3) . . ? C4 C5 C1 107.8(5) . . ? C4 C5 Fe1 71.3(3) . . ? C1 C5 Fe1 68.8(3) . . ? C7 C6 C10 106.7(5) . . ? C7 C6 B1 128.6(5) . . ? C10 C6 B1 124.5(5) . . ? C7 C6 Fe1 67.0(3) . . ? C10 C6 Fe1 70.5(3) . . ? B1 C6 Fe1 131.4(3) . . ? C8 C7 C6 109.7(5) . . ? C8 C7 Fe1 69.6(3) . . ? C6 C7 Fe1 73.2(3) . . ? C7 C8 C9 107.2(5) . . ? C7 C8 Fe1 70.3(3) . . ? C9 C8 Fe1 70.5(3) . . ? C10 C9 C8 108.6(5) . . ? C10 C9 Fe1 73.1(3) . . ? C8 C9 Fe1 68.6(3) . . ? C9 C10 C6 107.7(5) . . ? C9 C10 B1 127.8(5) . 3_667 ? C6 C10 B1 124.4(5) . 3_667 ? C9 C10 Fe1 67.5(3) . . ? C6 C10 Fe1 70.0(3) . . ? B1 C10 Fe1 125.7(3) 3_667 . ? C16 C11 C12 116.8(5) . . ? C16 C11 B1 122.5(5) . . ? C12 C11 B1 120.7(5) . . ? C13 C12 C11 121.4(5) . . ? C14 C13 C12 120.6(5) . . ? C13 C14 C15 119.4(5) . . ? C14 C15 C16 120.2(5) . . ? C11 C16 C15 121.6(5) . . ? N1 C17 C18 177.6(6) . . ? N2 C19 C20 177.0(7) . . ? C8 Fe1 C7 40.2(2) . . ? C8 Fe1 C2 133.8(2) . . ? C7 Fe1 C2 110.3(2) . . ? C8 Fe1 C9 40.9(2) . . ? C7 Fe1 C9 67.4(2) . . ? C2 Fe1 C9 173.8(2) . . ? C8 Fe1 C1 173.8(2) . . ? C7 Fe1 C1 137.9(2) . . ? C2 Fe1 C1 40.1(2) . . ? C9 Fe1 C1 145.2(2) . . ? C8 Fe1 C3 107.8(2) . . ? C7 Fe1 C3 111.9(2) . . ? C2 Fe1 C3 39.9(2) . . ? C9 Fe1 C3 134.8(2) . . ? C1 Fe1 C3 66.7(2) . . ? C8 Fe1 C5 141.8(2) . . ? C7 Fe1 C5 177.0(2) . . ? C2 Fe1 C5 66.7(2) . . ? C9 Fe1 C5 115.5(2) . . ? C1 Fe1 C5 39.8(2) . . ? C3 Fe1 C5 65.8(2) . . ? C8 Fe1 C4 112.0(2) . . ? C7 Fe1 C4 140.5(2) . . ? C2 Fe1 C4 66.0(2) . . ? C9 Fe1 C4 111.8(2) . . ? C1 Fe1 C4 65.9(2) . . ? C3 Fe1 C4 38.9(2) . . ? C5 Fe1 C4 38.7(2) . . ? C8 Fe1 C6 67.4(2) . . ? C7 Fe1 C6 39.8(2) . . ? C2 Fe1 C6 115.5(2) . . ? C9 Fe1 C6 66.8(2) . . ? C1 Fe1 C6 114.9(2) . . ? C3 Fe1 C6 142.6(2) . . ? C5 Fe1 C6 141.1(2) . . ? C4 Fe1 C6 178.5(2) . . ? C8 Fe1 C10 67.3(2) . . ? C7 Fe1 C10 66.6(2) . . ? C2 Fe1 C10 145.8(2) . . ? C9 Fe1 C10 39.4(2) . . ? C1 Fe1 C10 118.4(2) . . ? C3 Fe1 C10 174.2(2) . . ? C5 Fe1 C10 115.9(2) . . ? C4 Fe1 C10 139.0(2) . . ? C6 Fe1 C10 39.46(19) . . ? I3 I2 I1 179.988(19) . . ? C17 N1 B1 175.9(5) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 67.74 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.940 _refine_diff_density_min -0.700 _refine_diff_density_rms 0.253 #===END