data_cmt39 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H96 B2 Cl2 Fe2 N4 P2' _chemical_formula_weight 1067.51 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 10.3430(4) _cell_length_b 10.5536(4) _cell_length_c 14.0707(5) _cell_angle_alpha 87.428(2) _cell_angle_beta 83.364(2) _cell_angle_gamma 73.7360(10) _cell_volume 1464.43(9) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4224 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 41.06 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 1.0 _exptl_crystal_size_mid 0.93 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 574 _exptl_absorpt_coefficient_mu 0.678 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33050 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_sigmaI/netI 0.1019 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 42.82 _reflns_number_total 17197 _reflns_number_gt 10244 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17197 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0989 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.0905 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _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 Fe Fe 0.02042(2) 0.06764(2) 0.117289(15) 0.00965(4) Uani 1 1 d . . . P1 P 0.14104(4) -0.08839(4) 0.23499(3) 0.00944(7) Uani 1 1 d . . . P2 P -0.15054(4) 0.24686(4) 0.22987(3) 0.00901(6) Uani 1 1 d . . . Cl Cl -0.15807(3) 0.03455(4) 0.03915(2) 0.01414(7) Uani 1 1 d . . . C16 C -0.40169(16) 0.35854(16) 0.34783(12) 0.0198(3) Uani 1 1 d . . . H16A H -0.4745 0.3414 0.3931 0.030 Uiso 1 1 calc R . . H16B H -0.4407 0.4104 0.2933 0.030 Uiso 1 1 calc R . . H16C H -0.3520 0.4079 0.3797 0.030 Uiso 1 1 calc R . . N1 N 0.19098(11) 0.21245(12) 0.21051(8) 0.0097(2) Uani 1 1 d . . . C8 C 0.05461(15) -0.21957(15) 0.28140(10) 0.0135(3) Uani 1 1 d . . . C7 C 0.37575(16) -0.25071(17) 0.13041(11) 0.0192(3) Uani 1 1 d . . . H7A H 0.4748 -0.2837 0.1218 0.029 Uiso 1 1 calc R . . H7B H 0.3444 -0.1966 0.0747 0.029 Uiso 1 1 calc R . . H7C H 0.3365 -0.3255 0.1369 0.029 Uiso 1 1 calc R . . C14 C -0.38193(15) 0.15194(16) 0.25916(11) 0.0164(3) Uani 1 1 d . . . H14A H -0.3218 0.0652 0.2402 0.025 Uiso 1 1 calc R . . H14B H -0.4132 0.2025 0.2020 0.025 Uiso 1 1 calc R . . H14C H -0.4601 0.1405 0.3015 0.025 Uiso 1 1 calc R . . C11 C -0.09236(15) -0.16784(16) 0.25807(12) 0.0187(3) Uani 1 1 d . . . H11A H -0.1460 -0.2237 0.2902 0.028 Uiso 1 1 calc R . . H11B H -0.0948 -0.1698 0.1887 0.028 Uiso 1 1 calc R . . H11C H -0.1302 -0.0769 0.2804 0.028 Uiso 1 1 calc R . . C23 C 0.15630(15) 0.36933(15) 0.42143(10) 0.0137(3) Uani 1 1 d . . . H23 H 0.0898 0.4325 0.3899 0.016 Uiso 1 1 calc R . . N2 N 0.16250(12) 0.17269(12) 0.12623(8) 0.0106(2) Uani 1 1 d . . . C10 C 0.11519(17) -0.35043(15) 0.22800(12) 0.0196(3) Uani 1 1 d . . . H10A H 0.2059 -0.3927 0.2467 0.029 Uiso 1 1 calc R . . H10B H 0.1213 -0.3330 0.1589 0.029 Uiso 1 1 calc R . . H10C H 0.0570 -0.4090 0.2444 0.029 Uiso 1 1 calc R . . C12 C 0.11072(14) 0.03148(14) 0.33196(10) 0.0105(2) Uani 1 1 d . . . H12A H 0.0211 0.0339 0.3665 0.013 Uiso 1 1 calc R . . H12B H 0.1786 -0.0066 0.3771 0.013 Uiso 1 1 calc R . . C22 C 0.18896(13) 0.23622(14) 0.39469(10) 0.0101(2) Uani 1 1 d . . . C4 C 0.33126(14) -0.16667(15) 0.22105(10) 0.0129(3) Uani 1 1 d . . . C21 C -0.04087(13) 0.29059(14) 0.30922(10) 0.0101(2) Uani 1 1 d . . . H21A H -0.0313 0.3791 0.2897 0.012 Uiso 1 1 calc R . . H21B H -0.0876 0.2978 0.3751 0.012 Uiso 1 1 calc R . . C13 C -0.30444(14) 0.22687(15) 0.31226(10) 0.0126(3) Uani 1 1 d . . . B B 0.11254(15) 0.18865(16) 0.31218(11) 0.0093(3) Uani 1 1 d . . . C9 C 0.05451(17) -0.24411(16) 0.38953(11) 0.0187(3) Uani 1 1 d . . . H9A H 0.0102 -0.1613 0.4231 0.028 Uiso 1 1 calc R . . H9B H 0.1480 -0.2772 0.4053 0.028 Uiso 1 1 calc R . . H9C H 0.0052 -0.3095 0.4093 0.028 Uiso 1 1 calc R . . C6 C 0.38039(16) -0.24973(16) 0.30858(11) 0.0189(3) Uani 1 1 d . . . H6A H 0.3425 -0.3254 0.3152 0.028 Uiso 1 1 calc R . . H6B H 0.3506 -0.1957 0.3661 0.028 Uiso 1 1 calc R . . H6C H 0.4795 -0.2813 0.3005 0.028 Uiso 1 1 calc R . . C5 C 0.40396(15) -0.05721(16) 0.20911(12) 0.0179(3) Uani 1 1 d . . . H5A H 0.3784 -0.0010 0.2657 0.027 Uiso 1 1 calc R . . H5B H 0.3776 -0.0037 0.1521 0.027 Uiso 1 1 calc R . . H5C H 0.5022 -0.0972 0.2020 0.027 Uiso 1 1 calc R . . C25 C 0.31410(15) 0.32301(16) 0.54031(11) 0.0162(3) Uani 1 1 d . . . H25 H 0.3555 0.3518 0.5889 0.019 Uiso 1 1 calc R . . C15 C -0.25921(16) 0.14571(16) 0.40176(11) 0.0174(3) Uani 1 1 d . . . H15A H -0.2153 0.1944 0.4394 0.026 Uiso 1 1 calc R . . H15B H -0.1951 0.0610 0.3825 0.026 Uiso 1 1 calc R . . H15C H -0.3384 0.1299 0.4405 0.026 Uiso 1 1 calc R . . C17 C -0.21019(14) 0.39853(15) 0.15001(10) 0.0129(3) Uani 1 1 d . . . C20 C -0.09196(17) 0.39808(17) 0.07333(12) 0.0221(3) Uani 1 1 d . . . H20A H -0.0688 0.3167 0.0364 0.033 Uiso 1 1 calc R . . H20B H -0.0132 0.4028 0.1042 0.033 Uiso 1 1 calc R . . H20C H -0.1183 0.4745 0.0304 0.033 Uiso 1 1 calc R . . C27 C 0.28880(14) 0.14928(15) 0.44427(10) 0.0127(3) Uani 1 1 d . . . H27 H 0.3161 0.0585 0.4281 0.015 Uiso 1 1 calc R . . C24 C 0.21724(15) 0.41239(15) 0.49212(11) 0.0152(3) Uani 1 1 d . . . H24 H 0.1924 0.5034 0.5074 0.018 Uiso 1 1 calc R . . C18 C -0.24679(16) 0.53279(15) 0.20038(12) 0.0179(3) Uani 1 1 d . . . H18A H -0.2660 0.6043 0.1527 0.027 Uiso 1 1 calc R . . H18B H -0.1706 0.5386 0.2338 0.027 Uiso 1 1 calc R . . H18C H -0.3270 0.5407 0.2467 0.027 Uiso 1 1 calc R . . C19 C -0.32982(16) 0.38910(16) 0.09848(11) 0.0181(3) Uani 1 1 d . . . H19A H -0.3439 0.4550 0.0466 0.027 Uiso 1 1 calc R . . H19B H -0.4118 0.4056 0.1440 0.027 Uiso 1 1 calc R . . H19C H -0.3103 0.3006 0.0719 0.027 Uiso 1 1 calc R . . C26 C 0.34969(15) 0.19002(16) 0.51610(11) 0.0152(3) Uani 1 1 d . . . H26 H 0.4154 0.1272 0.5486 0.018 Uiso 1 1 calc R . . C1 C 0.28391(14) 0.27973(14) 0.19132(11) 0.0132(3) Uani 1 1 d . . . H1 H 0.3199 0.3190 0.2377 0.016 Uiso 1 1 calc R . . C2 C 0.31915(15) 0.28284(16) 0.09315(11) 0.0160(3) Uani 1 1 d . . . H2 H 0.3826 0.3231 0.0594 0.019 Uiso 1 1 calc R . . C3 C 0.24099(14) 0.21400(15) 0.05540(10) 0.0136(3) Uani 1 1 d . . . H3 H 0.2426 0.1983 -0.0107 0.016 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 Fe 0.01062(9) 0.00995(9) 0.00930(9) -0.00018(8) -0.00330(7) -0.00347(7) P1 0.01103(15) 0.00819(16) 0.00934(15) -0.00016(13) -0.00293(13) -0.00231(12) P2 0.00857(14) 0.00950(16) 0.00945(15) -0.00060(13) -0.00179(12) -0.00290(12) Cl 0.01175(14) 0.01933(17) 0.01188(14) -0.00447(14) -0.00272(12) -0.00395(12) C16 0.0177(7) 0.0177(8) 0.0216(8) -0.0032(7) 0.0052(6) -0.0037(6) N1 0.0094(5) 0.0101(5) 0.0099(5) -0.0002(4) -0.0018(4) -0.0028(4) C8 0.0187(6) 0.0101(6) 0.0132(6) 0.0011(5) -0.0028(5) -0.0061(5) C7 0.0182(7) 0.0191(8) 0.0165(7) -0.0051(6) -0.0028(6) 0.0024(6) C14 0.0130(6) 0.0180(7) 0.0204(7) -0.0004(6) -0.0027(6) -0.0074(5) C11 0.0189(7) 0.0154(7) 0.0245(8) 0.0022(6) -0.0056(6) -0.0082(6) C23 0.0176(6) 0.0115(6) 0.0137(6) 0.0018(5) -0.0058(5) -0.0053(5) N2 0.0113(5) 0.0119(5) 0.0093(5) -0.0009(5) -0.0011(4) -0.0044(4) C10 0.0274(8) 0.0116(7) 0.0215(8) -0.0006(6) -0.0054(7) -0.0072(6) C12 0.0122(6) 0.0097(6) 0.0099(6) -0.0015(5) -0.0015(5) -0.0032(5) C22 0.0107(5) 0.0112(6) 0.0090(5) 0.0005(5) -0.0014(5) -0.0039(5) C4 0.0116(6) 0.0122(6) 0.0128(6) -0.0019(5) -0.0028(5) 0.0008(5) C21 0.0102(5) 0.0100(6) 0.0108(6) -0.0008(5) -0.0024(5) -0.0035(5) C13 0.0110(6) 0.0134(6) 0.0138(6) -0.0014(5) 0.0007(5) -0.0047(5) B 0.0104(6) 0.0095(6) 0.0087(6) 0.0001(6) -0.0022(5) -0.0034(5) C9 0.0267(8) 0.0163(7) 0.0147(7) 0.0035(6) -0.0024(6) -0.0093(6) C6 0.0180(7) 0.0178(7) 0.0176(7) -0.0005(6) -0.0067(6) 0.0024(6) C5 0.0116(6) 0.0179(7) 0.0230(8) -0.0015(7) -0.0018(6) -0.0019(5) C25 0.0179(7) 0.0198(7) 0.0134(6) -0.0023(6) -0.0052(6) -0.0078(6) C15 0.0179(7) 0.0206(8) 0.0150(7) 0.0008(6) 0.0006(6) -0.0085(6) C17 0.0112(6) 0.0120(6) 0.0142(6) 0.0008(6) -0.0013(5) -0.0011(5) C20 0.0200(7) 0.0193(8) 0.0211(8) 0.0097(7) 0.0030(7) 0.0004(6) C27 0.0126(6) 0.0125(6) 0.0134(6) -0.0014(5) -0.0034(5) -0.0030(5) C24 0.0184(7) 0.0134(7) 0.0154(6) -0.0039(6) -0.0041(6) -0.0056(5) C18 0.0174(7) 0.0113(7) 0.0252(8) 0.0011(6) -0.0057(6) -0.0028(5) C19 0.0210(7) 0.0150(7) 0.0171(7) 0.0013(6) -0.0090(6) -0.0009(6) C26 0.0150(6) 0.0176(7) 0.0141(6) 0.0018(6) -0.0077(5) -0.0040(5) C1 0.0125(6) 0.0131(6) 0.0157(6) -0.0005(6) -0.0014(5) -0.0062(5) C2 0.0161(6) 0.0196(7) 0.0145(6) 0.0021(6) -0.0002(6) -0.0094(6) C3 0.0156(6) 0.0162(7) 0.0104(6) 0.0010(6) -0.0012(5) -0.0069(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 Fe N2 2.0910(11) . ? Fe Cl 2.3671(4) . ? Fe P1 2.4684(4) . ? Fe Cl 2.5815(4) 2 ? Fe P2 2.6385(4) . ? P1 C12 1.8423(13) . ? P1 C4 1.8992(14) . ? P1 C8 1.9024(14) . ? P2 C21 1.8381(13) . ? P2 C17 1.9107(16) . ? P2 C13 1.9136(14) . ? Cl Fe 2.5815(4) 2 ? C16 C13 1.535(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? N1 C1 1.3438(17) . ? N1 N2 1.3653(15) . ? N1 B 1.6067(19) . ? C8 C9 1.532(2) . ? C8 C11 1.533(2) . ? C8 C10 1.538(2) . ? C7 C4 1.537(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C14 C13 1.5402(18) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C23 C24 1.3925(19) . ? C23 C22 1.408(2) . ? C23 H23 0.9500 . ? N2 C3 1.3470(18) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C12 B 1.674(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C22 C27 1.405(2) . ? C22 B 1.6465(19) . ? C4 C6 1.530(2) . ? C4 C5 1.539(2) . ? C21 B 1.653(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C13 C15 1.534(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C25 C24 1.387(2) . ? C25 C26 1.395(2) . ? C25 H25 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C17 C19 1.533(2) . ? C17 C20 1.534(2) . ? C17 C18 1.543(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C27 C26 1.3931(19) . ? C27 H27 0.9500 . ? C24 H24 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C26 H26 0.9500 . ? C1 C2 1.389(2) . ? C1 H1 0.9500 . ? C2 C3 1.3879(19) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? 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 N2 Fe Cl 148.61(4) . . ? N2 Fe P1 86.69(4) . . ? Cl Fe P1 124.107(15) . . ? N2 Fe Cl 88.42(3) . 2 ? Cl Fe Cl 80.932(14) . 2 ? P1 Fe Cl 99.844(14) . 2 ? N2 Fe P2 87.30(3) . . ? Cl Fe P2 91.599(13) . . ? P1 Fe P2 101.578(14) . . ? Cl Fe P2 157.860(15) 2 . ? C12 P1 C4 104.98(6) . . ? C12 P1 C8 106.37(6) . . ? C4 P1 C8 108.43(7) . . ? C12 P1 Fe 96.34(5) . . ? C4 P1 Fe 123.62(5) . . ? C8 P1 Fe 114.48(5) . . ? C21 P2 C17 105.81(6) . . ? C21 P2 C13 105.19(6) . . ? C17 P2 C13 107.80(6) . . ? C21 P2 Fe 103.29(5) . . ? C17 P2 Fe 105.58(5) . . ? C13 P2 Fe 127.42(5) . . ? Fe Cl Fe 99.068(14) . 2 ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 N1 N2 108.68(11) . . ? C1 N1 B 128.38(11) . . ? N2 N1 B 122.77(10) . . ? C9 C8 C11 108.76(13) . . ? C9 C8 C10 110.02(13) . . ? C11 C8 C10 106.40(12) . . ? C9 C8 P1 113.43(10) . . ? C11 C8 P1 105.85(10) . . ? C10 C8 P1 111.99(10) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C24 C23 C22 122.86(14) . . ? C24 C23 H23 118.6 . . ? C22 C23 H23 118.6 . . ? C3 N2 N1 107.29(11) . . ? C3 N2 Fe 129.14(9) . . ? N1 N2 Fe 123.57(9) . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? B C12 P1 122.83(9) . . ? B C12 H12A 106.6 . . ? P1 C12 H12A 106.6 . . ? B C12 H12B 106.6 . . ? P1 C12 H12B 106.6 . . ? H12A C12 H12B 106.6 . . ? C27 C22 C23 115.01(12) . . ? C27 C22 B 123.54(12) . . ? C23 C22 B 121.45(13) . . ? C6 C4 C7 110.06(12) . . ? C6 C4 C5 107.04(12) . . ? C7 C4 C5 106.74(13) . . ? C6 C4 P1 112.51(10) . . ? C7 C4 P1 111.04(10) . . ? C5 C4 P1 109.20(10) . . ? B C21 P2 116.81(9) . . ? B C21 H21A 108.1 . . ? P2 C21 H21A 108.1 . . ? B C21 H21B 108.1 . . ? P2 C21 H21B 108.1 . . ? H21A C21 H21B 107.3 . . ? C15 C13 C16 106.46(12) . . ? C15 C13 C14 107.82(12) . . ? C16 C13 C14 109.25(12) . . ? C15 C13 P2 110.43(10) . . ? C16 C13 P2 113.44(10) . . ? C14 C13 P2 109.27(10) . . ? N1 B C22 106.80(10) . . ? N1 B C21 103.85(11) . . ? C22 B C21 109.51(11) . . ? N1 B C12 113.42(11) . . ? C22 B C12 110.19(11) . . ? C21 B C12 112.72(11) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C24 C25 C26 118.79(13) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C19 C17 C20 107.48(13) . . ? C19 C17 C18 109.41(12) . . ? C20 C17 C18 106.44(13) . . ? C19 C17 P2 110.94(10) . . ? C20 C17 P2 106.66(10) . . ? C18 C17 P2 115.49(11) . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C27 C22 123.03(14) . . ? C26 C27 H27 118.5 . . ? C22 C27 H27 118.5 . . ? C25 C24 C23 120.31(14) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C27 C26 C25 119.98(14) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? N1 C1 C2 109.37(12) . . ? N1 C1 H1 125.3 . . ? C2 C1 H1 125.3 . . ? C3 C2 C1 104.56(12) . . ? C3 C2 H2 127.7 . . ? C1 C2 H2 127.7 . . ? N2 C3 C2 110.09(12) . . ? N2 C3 H3 125.0 . . ? C2 C3 H3 125.0 . . ? _diffrn_measured_fraction_theta_max 0.802 _diffrn_reflns_theta_full 42.82 _diffrn_measured_fraction_theta_full 0.802 _refine_diff_density_max 0.915 _refine_diff_density_min -0.952 _refine_diff_density_rms 0.116 #===END data_cmt46 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H63 B1 Fe1 N3 P2' _chemical_formula_weight 678.44 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' 'P' 'P' 0.1023 0.0942 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.8828(9) _cell_length_b 20.2565(17) _cell_length_c 33.573(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.412(2) _cell_angle_gamma 90.00 _cell_volume 7379.1(11) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3176 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.88 _exptl_crystal_description block _exptl_crystal_colour purple-blac _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.15_exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2838 _exptl_absorpt_coefficient_mu 0.412 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17743 _diffrn_reflns_av_R_equivalents 0.0940 _diffrn_reflns_av_sigmaI/netI 0.1163 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 27.68 _reflns_number_total 5487 _reflns_number_gt 3057 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5487 _refine_ls_number_parameters 817 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1493 _refine_ls_R_factor_gt 0.0818 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.1083 _refine_ls_goodness_of_fit_ref 1.763 _refine_ls_restrained_S_all 1.763 _refine_ls_shift/su_max 1.424 _refine_ls_shift/su_mean 0.088 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 0.1505(11) 0.8732(6) 0.4182(3) 0.016(3) Uani 1 1 d . . . Fe1 Fe 0.32575(12) 0.99933(8) 0.38438(3) 0.0144(4) Uani 1 1 d . . . P1 P 0.3666(4) 0.8869(2) 0.36950(15) 0.0128(11) Uani 1 1 d . . . P2 P 0.1143(2) 1.00117(15) 0.37508(6) 0.0117(6) Uani 1 1 d . . . N1 N 0.2240(7) 0.9187(4) 0.4504(2) 0.0082(19) Uani 1 1 d . . . N2 N 0.2940(8) 0.9694(4) 0.4401(2) 0.019(2) Uani 1 1 d . . . N3 N 0.4057(9) 1.0589(5) 0.3673(2) 0.018(2) Uani 1 1 d . . . C1 C 0.442(5) 1.108(3) 0.3538(14) 0.005(9) Uani 1 1 d . . . C2 C 0.3970(11) 1.1770(5) 0.3569(3) 0.017(3) Uani 1 1 d . . . H2A H 0.3093 1.1757 0.3466 0.021 Uiso 1 1 calc R . . H2B H 0.3971 1.1860 0.3859 0.021 Uiso 1 1 calc R . . C3 C 0.447(5) 1.2360(19) 0.3398(13) 0.005(7) Uani 1 1 d . . . H3 H 0.4010 1.2761 0.3478 0.007 Uiso 1 1 calc R . . C4 C 0.441(3) 1.2292(19) 0.2914(8) 0.013(5) Uani 1 1 d . . . H4A H 0.4799 1.2680 0.2795 0.016 Uiso 1 1 calc R . . H4B H 0.3549 1.2256 0.2800 0.016 Uiso 1 1 calc R . . C5 C 0.5135(10) 1.1658(6) 0.2831(3) 0.027(3) Uani 1 1 d . . . H5 H 0.5077 1.1583 0.2536 0.033 Uiso 1 1 calc R . . C6 C 0.459(3) 1.1084(15) 0.3020(10) 0.020(7) Uani 1 1 d . . . H6A H 0.5087 1.0693 0.2961 0.024 Uiso 1 1 calc R . . H6B H 0.3757 1.1015 0.2884 0.024 Uiso 1 1 calc R . . C7 C 0.5990(9) 1.1183(5) 0.3626(3) 0.014(3) Uani 1 1 d . . . H7A H 0.6392 1.0778 0.3534 0.017 Uiso 1 1 calc R . . H7B H 0.6180 1.1211 0.3918 0.017 Uiso 1 1 calc R . . C8 C 0.6608(11) 1.1783(5) 0.3433(3) 0.024(3) Uani 1 1 d . . . H8 H 0.7495 1.1811 0.3535 0.029 Uiso 1 1 calc R . . C9 C 0.5931(9) 1.2419(5) 0.3542(3) 0.017(3) Uani 1 1 d . . . H9A H 0.6291 1.2802 0.3409 0.020 Uiso 1 1 calc R . . H9B H 0.6034 1.2490 0.3834 0.020 Uiso 1 1 calc R . . C10 C 0.6509(11) 1.1702(5) 0.2978(3) 0.036(3) Uani 1 1 d . . . H10A H 0.6895 1.2084 0.2852 0.043 Uiso 1 1 calc R . . H10B H 0.6944 1.1296 0.2903 0.043 Uiso 1 1 calc R . . C11 C 0.0722(16) 0.8227(9) 0.4409(4) 0.021(5) Uani 1 1 d . . . C12 C -0.0461(18) 0.8383(11) 0.4567(7) 0.017(6) Uani 1 1 d . . . H12 H -0.0752 0.8822 0.4526 0.020 Uiso 1 1 calc R . . C13 C -0.1169(10) 0.7984(6) 0.4761(3) 0.021(3) Uani 1 1 d . . . H13 H -0.1943 0.8142 0.4832 0.025 Uiso 1 1 calc R . . C14 C -0.082(3) 0.7332(12) 0.4865(7) 0.036(8) Uani 1 1 d . . . H14 H -0.1287 0.7052 0.5024 0.044 Uiso 1 1 calc R . . C15 C 0.028(2) 0.7143(9) 0.4707(5) 0.019(5) Uani 1 1 d . . . H15 H 0.0525 0.6695 0.4736 0.023 Uiso 1 1 calc R . . C16 C 0.1055(9) 0.7570(5) 0.4508(3) 0.015(3) Uani 1 1 d . . . H16 H 0.1829 0.7409 0.4438 0.017 Uiso 1 1 calc R . . C17 C 0.2605(9) 0.8349(5) 0.3975(2) 0.014(3) Uani 1 1 d . . . H17A H 0.2225 0.8015 0.3789 0.017 Uiso 1 1 calc R . . H17B H 0.3106 0.8108 0.4187 0.017 Uiso 1 1 calc R . . C18 C 0.5301(16) 0.8693(8) 0.3933(4) 0.030(5) Uani 1 1 d . . . C19 C 0.5457(10) 0.9045(5) 0.4335(3) 0.024(3) Uani 1 1 d . . . H19A H 0.4891 0.8853 0.4517 0.036 Uiso 1 1 calc R . . H19B H 0.5273 0.9515 0.4297 0.036 Uiso 1 1 calc R . . H19C H 0.6308 0.8993 0.4449 0.036 Uiso 1 1 calc R . . C20 C 0.5574(10) 0.7977(5) 0.4026(3) 0.026(3) Uani 1 1 d . . . H20A H 0.6311 0.7946 0.4212 0.039 Uiso 1 1 calc R . . H20B H 0.5715 0.7742 0.3779 0.039 Uiso 1 1 calc R . . H20C H 0.4872 0.7779 0.4148 0.039 Uiso 1 1 calc R . . C21 C 0.6295(15) 0.9023(9) 0.3688(5) 0.053(7) Uani 1 1 d . . . H21A H 0.7104 0.8990 0.3837 0.080 Uiso 1 1 calc R . . H21B H 0.6086 0.9489 0.3643 0.080 Uiso 1 1 calc R . . H21C H 0.6319 0.8798 0.3430 0.080 Uiso 1 1 calc R . . C22 C 0.3593(10) 0.8505(5) 0.3161(2) 0.014(3) Uani 1 1 d . . . C23 C 0.2263(10) 0.8312(5) 0.3042(2) 0.024(3) Uani 1 1 d . . . H23A H 0.1708 0.8643 0.3143 0.036 Uiso 1 1 calc R . . H23B H 0.2091 0.7880 0.3157 0.036 Uiso 1 1 calc R . . H23C H 0.2135 0.8289 0.2750 0.036 Uiso 1 1 calc R . . C24 C 0.4076(12) 0.9038(8) 0.2881(5) 0.030(4) Uani 1 1 d . . . H24A H 0.3952 0.8887 0.2603 0.045 Uiso 1 1 calc R . . H24B H 0.4956 0.9112 0.2950 0.045 Uiso 1 1 calc R . . H24C H 0.3624 0.9451 0.2912 0.045 Uiso 1 1 calc R . . C25 C 0.445(3) 0.7898(15) 0.3136(7) 0.011(6) Uani 1 1 d . . . H25A H 0.4238 0.7565 0.3330 0.016 Uiso 1 1 calc R . . H25B H 0.5312 0.8036 0.3195 0.016 Uiso 1 1 calc R . . H25C H 0.4356 0.7711 0.2866 0.016 Uiso 1 1 calc R . . C26 C 0.0640(9) 0.9166(4) 0.3846(3) 0.017(3) Uani 1 1 d . . . H26A H -0.0208 0.9185 0.3933 0.021 Uiso 1 1 calc R . . H26B H 0.0599 0.8921 0.3590 0.021 Uiso 1 1 calc R . . C27 C 0.036(4) 1.0634(18) 0.4101(8) 0.006(5) Uani 1 1 d . . . C28 C 0.0979(10) 1.1262(5) 0.4126(2) 0.020(3) Uani 1 1 d . . . H28A H 0.0811 1.1501 0.3874 0.030 Uiso 1 1 calc R . . H28B H 0.1868 1.1192 0.4175 0.030 Uiso 1 1 calc R . . H28C H 0.0679 1.1521 0.4345 0.030 Uiso 1 1 calc R . . C29 C -0.115(3) 1.0612(13) 0.3990(7) 0.032(7) Uani 1 1 d . . . H29A H -0.1569 1.0801 0.4211 0.049 Uiso 1 1 calc R . . H29B H -0.1411 1.0153 0.3947 0.049 Uiso 1 1 calc R . . H29C H -0.1353 1.0868 0.3747 0.049 Uiso 1 1 calc R . . C30 C 0.0435(10) 1.0310(5) 0.4544(3) 0.018(3) Uani 1 1 d . . . H30A H 0.1296 1.0298 0.4654 0.027 Uiso 1 1 calc R . . H30B H 0.0103 0.9860 0.4528 0.027 Uiso 1 1 calc R . . H30C H -0.0049 1.0577 0.4719 0.027 Uiso 1 1 calc R . . C31 C 0.0508(12) 1.0264(6) 0.3221(3) 0.022(4) Uani 1 1 d . . . C32 C 0.1367(8) 1.0026(5) 0.2923(2) 0.022(3) Uani 1 1 d . . . H32A H 0.1081 1.0185 0.2656 0.034 Uiso 1 1 calc R . . H32B H 0.1382 0.9542 0.2923 0.034 Uiso 1 1 calc R . . H32C H 0.2198 1.0194 0.2995 0.034 Uiso 1 1 calc R . . C33 C 0.0349(10) 1.1017(5) 0.3156(2) 0.023(3) Uani 1 1 d . . . H33A H 0.1148 1.1237 0.3208 0.034 Uiso 1 1 calc R . . H33B H -0.0233 1.1190 0.3339 0.034 Uiso 1 1 calc R . . H33C H 0.0033 1.1102 0.2879 0.034 Uiso 1 1 calc R . . C34 C -0.0769(14) 0.9936(10) 0.3127(5) 0.019(5) Uani 1 1 d . . . H34A H -0.1033 0.9997 0.2844 0.028 Uiso 1 1 calc R . . H34B H -0.1372 1.0139 0.3291 0.028 Uiso 1 1 calc R . . H34C H -0.0709 0.9463 0.3187 0.028 Uiso 1 1 calc R . . C35 C 0.2347(9) 0.9133(5) 0.4899(3) 0.013(3) Uani 1 1 d . . . H35 H 0.1938 0.8810 0.5046 0.016 Uiso 1 1 calc R . . C36 C 0.3134(10) 0.9611(5) 0.5070(3) 0.021(3) Uani 1 1 d . . . H36 H 0.3360 0.9689 0.5345 0.025 Uiso 1 1 calc R . . C37 C 0.3513(9) 0.9949(6) 0.4738(3) 0.023(3) Uani 1 1 d . . . H37 H 0.4085 1.0304 0.4748 0.028 Uiso 1 1 calc R . . B2 B 0.3094(11) 0.3708(5) 0.4190(3) 0.012(3) Uani 1 1 d . . . Fe2 Fe 0.11791(12) 0.49658(8) 0.38785(3) 0.0151(4) Uani 1 1 d . . . N4 N 0.2552(7) 0.4160(3) 0.45303(19) 0.0073(19) Uani 1 1 d . . . N5 N 0.1765(8) 0.4672(4) 0.4432(2) 0.017(2) Uani 1 1 d . . . N6 N 0.0299(8) 0.5572(4) 0.3711(2) 0.014(2) Uani 1 1 d . . . P3 P 0.3243(2) 0.49779(14) 0.37675(6) 0.0100(6) Uani 1 1 d . . . P4 P 0.0678(5) 0.3844(2) 0.37390(13) 0.0139(12) Uani 1 1 d . . . C38 C -0.024(5) 0.616(3) 0.3455(14) -0.001(8) Uani 1 1 d . . . C39 C -0.080(2) 0.5938(15) 0.3071(10) 0.018(6) Uani 1 1 d . . . H39A H -0.1329 0.5549 0.3107 0.022 Uiso 1 1 calc R . . H39B H -0.0151 0.5812 0.2894 0.022 Uiso 1 1 calc R . . C40 C -0.1571(11) 0.6504(6) 0.2883(3) 0.029(3) Uani 1 1 d . . . H40 H -0.1797 0.6416 0.2593 0.035 Uiso 1 1 calc R . . C41 C -0.073(4) 0.712(2) 0.2937(12) 0.066(14) Uani 1 1 d . . . H41A H -0.1166 0.7497 0.2805 0.079 Uiso 1 1 calc R . . H41B H 0.0017 0.7036 0.2791 0.079 Uiso 1 1 calc R . . C42 C -0.032(6) 0.732(2) 0.3343(15) 0.023(14) Uani 1 1 d . . . H42 H 0.0199 0.7727 0.3351 0.028 Uiso 1 1 calc R . . C43 C 0.0339(11) 0.6740(6) 0.3540(3) 0.020(3) Uani 1 1 d . . . H43A H 0.1185 0.6717 0.3451 0.024 Uiso 1 1 calc R . . H43B H 0.0406 0.6808 0.3833 0.024 Uiso 1 1 calc R . . C44 C -0.1627(10) 0.6209(5) 0.3743(3) 0.020(3) Uani 1 1 d . . . H44A H -0.2095 0.5790 0.3728 0.024 Uiso 1 1 calc R . . H44B H -0.1401 0.6317 0.4027 0.024 Uiso 1 1 calc R . . C45 C -0.2352(10) 0.6760(5) 0.3536(3) 0.023(3) Uani 1 1 d . . . H45 H -0.3124 0.6822 0.3675 0.028 Uiso 1 1 calc R . . C46 C -0.2714(10) 0.6616(5) 0.3105(3) 0.030(3) Uani 1 1 d . . . H46A H -0.3190 0.6991 0.2984 0.036 Uiso 1 1 calc R . . H46B H -0.3243 0.6218 0.3083 0.036 Uiso 1 1 calc R . . C47 C -0.1607(11) 0.7406(6) 0.3576(3) 0.029(3) Uani 1 1 d . . . H47A H -0.1401 0.7509 0.3861 0.034 Uiso 1 1 calc R . . H47B H -0.2102 0.7776 0.3455 0.034 Uiso 1 1 calc R . . C48 C 0.4048(17) 0.3186(7) 0.4439(4) 0.018(4) Uani 1 1 d . . . C49 C 0.5240(16) 0.3367(11) 0.4558(6) 0.011(6) Uani 1 1 d . . . H49 H 0.5525 0.3789 0.4483 0.014 Uiso 1 1 calc R . . C50 C 0.6059(10) 0.2945(6) 0.4789(3) 0.023(3) Uani 1 1 d . . . H50 H 0.6856 0.3092 0.4885 0.028 Uiso 1 1 calc R . . C51 C 0.5658(18) 0.2306(8) 0.4872(4) 0.023(5) Uani 1 1 d . . . H51 H 0.6200 0.1998 0.5008 0.028 Uiso 1 1 calc R . . C52 C 0.448(2) 0.2135(13) 0.4753(6) 0.011(5) Uani 1 1 d . . . H52 H 0.4191 0.1714 0.4827 0.013 Uiso 1 1 calc R . . C53 C 0.3699(9) 0.2542(6) 0.4535(3) 0.019(3) Uani 1 1 d . . . H53 H 0.2901 0.2387 0.4445 0.022 Uiso 1 1 calc R . . C54 C 0.3821(9) 0.4118(5) 0.3863(3) 0.019(3) Uani 1 1 d . . . H54A H 0.3754 0.3872 0.3607 0.023 Uiso 1 1 calc R . . H54B H 0.4705 0.4140 0.3956 0.023 Uiso 1 1 calc R . . C55 C 0.3612(11) 0.5200(7) 0.3232(3) 0.017(4) Uani 1 1 d . . . C56 C 0.2641(9) 0.4955(6) 0.2933(2) 0.041(3) Uani 1 1 d . . . H56A H 0.2891 0.5038 0.2663 0.062 Uiso 1 1 calc R . . H56B H 0.1866 0.5187 0.2969 0.062 Uiso 1 1 calc R . . H56C H 0.2525 0.4480 0.2971 0.062 Uiso 1 1 calc R . . C57 C 0.3697(10) 0.5978(5) 0.3167(3) 0.030(3) Uani 1 1 d . . . H57A H 0.3896 0.6069 0.2893 0.044 Uiso 1 1 calc R . . H57B H 0.4343 0.6161 0.3355 0.044 Uiso 1 1 calc R . . H57C H 0.2905 0.6181 0.3215 0.044 Uiso 1 1 calc R . . C58 C 0.4902(14) 0.4901(11) 0.3112(6) 0.026(6) Uani 1 1 d . . . H58A H 0.4824 0.4423 0.3077 0.038 Uiso 1 1 calc R . . H58B H 0.5545 0.4996 0.3325 0.038 Uiso 1 1 calc R . . H58C H 0.5124 0.5103 0.2863 0.038 Uiso 1 1 calc R . . C59 C 0.424(2) 0.5578(11) 0.4102(6) 0.013(5) Uani 1 1 d . . . C60 C 0.4337(10) 0.5292(5) 0.4551(2) 0.021(3) Uani 1 1 d . . . H60A H 0.4880 0.5575 0.4723 0.032 Uiso 1 1 calc R . . H60B H 0.4672 0.4843 0.4552 0.032 Uiso 1 1 calc R . . H60C H 0.3514 0.5284 0.4651 0.032 Uiso 1 1 calc R . . C61 C 0.3577(9) 0.6217(5) 0.4133(3) 0.022(3) Uani 1 1 d . . . H61A H 0.4034 0.6501 0.4329 0.033 Uiso 1 1 calc R . . H61B H 0.2751 0.6133 0.4219 0.033 Uiso 1 1 calc R . . H61C H 0.3509 0.6436 0.3873 0.033 Uiso 1 1 calc R . . C62 C 0.554(4) 0.558(2) 0.3981(7) 0.033(12) Uani 1 1 d . . . H62A H 0.5554 0.5782 0.3716 0.049 Uiso 1 1 calc R . . H62B H 0.5847 0.5130 0.3975 0.049 Uiso 1 1 calc R . . H62C H 0.6057 0.5842 0.4175 0.049 Uiso 1 1 calc R . . C63 C 0.1864(9) 0.3320(4) 0.4001(2) 0.014(2) Uani 1 1 d . . . H63A H 0.1486 0.3086 0.4220 0.017 Uiso 1 1 calc R . . H63B H 0.2123 0.2982 0.3812 0.017 Uiso 1 1 calc R . . C64 C -0.0806(13) 0.3666(5) 0.3981(3) 0.021(3) Uani 1 1 d . . . C65 C -0.0768(11) 0.4021(5) 0.4393(3) 0.028(3) Uani 1 1 d . . . H65A H -0.0656 0.4497 0.4355 0.042 Uiso 1 1 calc R . . H65B H -0.0080 0.3848 0.4568 0.042 Uiso 1 1 calc R . . H65C H -0.1543 0.3943 0.4516 0.042 Uiso 1 1 calc R . . C66 C -0.1953(13) 0.3958(10) 0.3751(6) 0.033(6) Uani 1 1 d . . . H66A H -0.2139 0.3707 0.3504 0.050 Uiso 1 1 calc R . . H66B H -0.1797 0.4421 0.3685 0.050 Uiso 1 1 calc R . . H66C H -0.2654 0.3933 0.3917 0.050 Uiso 1 1 calc R . . C67 C -0.1090(10) 0.2940(5) 0.4067(3) 0.023(3) Uani 1 1 d . . . H67A H -0.1805 0.2914 0.4227 0.034 Uiso 1 1 calc R . . H67B H -0.0375 0.2737 0.4215 0.034 Uiso 1 1 calc R . . H67C H -0.1269 0.2704 0.3814 0.034 Uiso 1 1 calc R . . C68 C 0.0462(9) 0.3510(5) 0.3214(3) 0.016(3) Uani 1 1 d . . . C69 C 0.1746(9) 0.3304(5) 0.3079(2) 0.016(3) Uani 1 1 d . . . H69A H 0.1671 0.3200 0.2793 0.024 Uiso 1 1 calc R . . H69B H 0.2044 0.2914 0.3230 0.024 Uiso 1 1 calc R . . H69C H 0.2330 0.3668 0.3129 0.024 Uiso 1 1 calc R . . C70 C -0.036(4) 0.2823(19) 0.3147(10) 0.081(13) Uani 1 1 d . . . H70A H -0.0341 0.2677 0.2869 0.122 Uiso 1 1 calc R . . H70B H -0.1212 0.2908 0.3206 0.122 Uiso 1 1 calc R . . H70C H -0.0006 0.2478 0.3325 0.122 Uiso 1 1 calc R . . C71 C -0.0137(12) 0.4047(9) 0.2929(5) 0.029(4) Uani 1 1 d . . . H71A H 0.0274 0.4471 0.2984 0.043 Uiso 1 1 calc R . . H71B H -0.1014 0.4088 0.2973 0.043 Uiso 1 1 calc R . . H71C H -0.0049 0.3920 0.2651 0.043 Uiso 1 1 calc R . . C72 C 0.2656(9) 0.4110(5) 0.4923(3) 0.014(3) Uani 1 1 d . . . H72 H 0.3148 0.3792 0.5070 0.017 Uiso 1 1 calc R . . C73 C 0.1936(9) 0.4594(6) 0.5095(3) 0.023(3) Uani 1 1 d . . . H73 H 0.1833 0.4665 0.5370 0.028 Uiso 1 1 calc R . . C74 C 0.1409(9) 0.4943(5) 0.4769(2) 0.014(2) Uani 1 1 d . . . H74 H 0.0882 0.5315 0.4783 0.017 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 B1 0.000(8) 0.016(8) 0.033(7) -0.001(6) 0.004(6) -0.006(6) Fe1 0.0192(10) 0.0081(9) 0.0157(7) 0.0029(7) -0.0001(6) 0.0001(9) P1 0.017(3) 0.011(2) 0.0123(18) -0.0003(16) 0.012(2) -0.006(2) P2 0.0149(17) 0.0060(16) 0.0135(12) -0.0019(14) -0.0033(12) 0.0024(16) N1 0.009(6) 0.005(5) 0.012(4) 0.003(4) 0.009(4) -0.006(4) N2 0.019(6) 0.019(6) 0.018(4) -0.006(4) 0.000(4) 0.006(4) N3 0.028(8) 0.012(6) 0.015(5) -0.002(5) -0.001(5) 0.001(5) C1 0.00(2) 0.02(2) 0.000(16) 0.005(15) 0.028(13) -0.019(14) C2 0.027(10) 0.013(9) 0.013(5) 0.002(5) 0.008(5) 0.003(6) C3 0.008(19) 0.000(15) 0.011(14) -0.002(9) 0.018(14) 0.007(9) C4 0.036(13) 0.006(13) 0.000(8) 0.017(8) 0.013(8) 0.017(8) C5 0.026(9) 0.018(8) 0.037(7) 0.000(6) 0.003(6) -0.001(7) C6 0.030(16) 0.009(16) 0.024(10) -0.004(10) 0.011(10) -0.017(9) C7 0.007(8) 0.018(7) 0.017(6) 0.004(5) 0.005(5) -0.004(6) C8 0.034(9) 0.008(7) 0.028(6) 0.003(5) -0.002(6) 0.004(6) C9 0.023(7) 0.006(7) 0.021(6) 0.001(5) -0.006(5) 0.004(6) C10 0.038(9) 0.028(8) 0.042(7) 0.007(6) 0.005(6) 0.013(7) C11 0.016(13) 0.033(10) 0.016(9) 0.000(8) 0.002(7) 0.011(8) C12 0.019(18) 0.005(9) 0.030(11) -0.003(8) 0.020(15) -0.016(13) C13 0.012(8) 0.031(9) 0.020(7) 0.009(7) 0.009(5) 0.003(6) C14 0.040(19) 0.047(19) 0.025(13) -0.012(9) 0.018(10) -0.003(11) C15 0.038(16) 0.010(9) 0.010(9) -0.002(7) 0.008(13) -0.006(12) C16 0.014(7) 0.015(7) 0.015(6) 0.003(6) 0.002(5) -0.005(6) C17 0.018(7) 0.015(7) 0.011(5) 0.012(5) 0.010(5) -0.010(5) C18 0.028(13) 0.051(12) 0.012(8) -0.002(8) 0.006(9) -0.006(9) C19 0.032(9) 0.015(7) 0.025(6) -0.006(5) -0.004(6) 0.003(6) C20 0.020(8) 0.025(8) 0.033(6) -0.003(6) 0.005(6) 0.011(6) C21 0.040(15) 0.032(12) 0.085(13) 0.019(9) -0.013(10) -0.020(10) C22 0.022(8) 0.019(7) 0.004(5) -0.004(5) 0.014(5) 0.002(5) C23 0.039(9) 0.023(7) 0.010(5) 0.001(5) 0.003(5) 0.003(6) C24 0.032(11) 0.034(9) 0.026(8) 0.012(7) 0.020(9) 0.009(9) C25 0.034(14) 0.001(11) 0.000(9) 0.007(8) 0.020(9) 0.009(9) C26 0.010(7) 0.019(7) 0.023(6) 0.028(5) 0.001(5) -0.010(5) C27 0.000(12) 0.010(10) 0.009(13) -0.023(9) 0.004(11) 0.015(7) C28 0.035(8) 0.021(8) 0.005(5) -0.003(5) 0.003(5) 0.003(6) C29 0.000(17) 0.049(12) 0.046(16) 0.002(11) -0.006(10) 0.024(10) C30 0.018(8) 0.016(7) 0.020(6) 0.005(5) -0.003(6) -0.007(6) C31 0.020(10) 0.027(9) 0.017(6) -0.006(6) -0.017(6) -0.001(6) C32 0.028(7) 0.025(7) 0.014(5) -0.007(6) 0.000(5) 0.005(7) C33 0.039(9) 0.016(7) 0.014(5) 0.004(5) 0.005(5) -0.022(6) C34 0.012(15) 0.027(12) 0.021(9) 0.021(8) 0.023(11) 0.012(12) C35 0.019(8) 0.007(6) 0.015(5) -0.003(4) 0.002(5) 0.003(5) C36 0.035(9) 0.027(9) 0.001(5) 0.002(5) 0.016(5) 0.011(6) C37 0.016(7) 0.024(7) 0.029(6) -0.029(6) -0.002(5) 0.020(6) B2 0.012(8) 0.009(8) 0.015(6) -0.005(5) 0.007(6) 0.020(6) Fe2 0.0190(10) 0.0111(9) 0.0147(7) 0.0012(7) -0.0008(6) 0.0005(9) N4 0.011(6) 0.007(5) 0.004(4) 0.004(3) 0.004(4) 0.004(4) N5 0.024(6) 0.019(6) 0.010(4) 0.001(4) 0.010(4) -0.006(4) N6 0.006(6) 0.018(6) 0.018(4) -0.010(4) 0.003(4) -0.004(5) P3 0.0155(17) 0.0040(15) 0.0109(12) 0.0007(13) 0.0037(11) 0.0014(16) P4 0.019(4) 0.010(3) 0.012(2) -0.005(2) 0.000(2) -0.001(2) C38 0.000(18) 0.000(11) 0.001(18) 0.013(12) 0.031(11) -0.020(11) C39 0.032(18) 0.000(12) 0.021(10) 0.003(8) -0.005(13) -0.008(10) C40 0.027(9) 0.044(10) 0.015(6) -0.013(6) -0.002(6) 0.030(7) C41 0.09(2) 0.05(3) 0.061(17) 0.051(15) 0.031(14) 0.036(19) C42 0.02(2) 0.05(2) 0.009(13) -0.005(10) 0.030(12) 0.005(12) C43 0.017(9) 0.026(9) 0.019(6) 0.007(6) 0.016(6) 0.012(7) C44 0.010(8) 0.017(8) 0.035(7) 0.004(6) 0.016(6) 0.005(6) C45 0.017(8) 0.021(7) 0.034(7) 0.013(5) 0.018(6) 0.008(6) C46 0.027(9) 0.019(7) 0.042(7) 0.001(6) -0.012(6) 0.006(6) C47 0.031(9) 0.029(9) 0.026(6) 0.010(6) 0.005(6) -0.016(7) C48 0.035(13) 0.000(10) 0.020(8) 0.002(6) 0.005(7) -0.007(7) C49 0.000(15) 0.017(11) 0.019(10) 0.016(7) 0.010(13) -0.020(13) C50 0.013(8) 0.027(8) 0.028(6) -0.001(6) -0.009(6) -0.003(6) C51 0.023(13) 0.027(12) 0.018(9) 0.009(7) 0.000(8) 0.024(8) C52 0.005(13) 0.019(13) 0.011(12) 0.005(9) 0.013(12) -0.001(12) C53 0.011(7) 0.032(8) 0.013(6) -0.017(6) -0.004(5) 0.004(6) C54 0.006(7) 0.025(7) 0.027(6) 0.030(5) 0.009(5) 0.020(5) C55 0.000(9) 0.034(10) 0.017(7) 0.011(6) -0.002(6) 0.000(6) C56 0.052(9) 0.051(8) 0.019(5) 0.016(6) -0.010(5) -0.024(8) C57 0.044(9) 0.025(8) 0.019(6) 0.011(5) -0.002(6) 0.017(6) C58 0.020(16) 0.042(12) 0.019(8) 0.000(7) 0.026(12) 0.035(14) C59 0.000(18) 0.019(10) 0.018(10) -0.017(7) -0.011(8) -0.005(9) C60 0.032(9) 0.017(7) 0.013(6) -0.001(5) 0.000(6) -0.005(6) C61 0.012(7) 0.032(8) 0.024(6) 0.005(6) 0.009(5) -0.023(6) C62 0.04(2) 0.042(17) 0.018(15) -0.021(13) -0.005(14) -0.012(13) C63 0.026(7) 0.006(6) 0.010(5) 0.002(4) 0.005(5) -0.003(5) C64 0.021(10) 0.023(8) 0.018(7) 0.006(6) -0.006(7) 0.006(6) C65 0.034(9) 0.022(8) 0.030(7) 0.012(5) 0.010(6) -0.006(6) C66 0.018(14) 0.053(12) 0.028(10) -0.006(8) -0.005(9) -0.010(11) C67 0.021(8) 0.015(7) 0.032(6) 0.003(5) -0.003(5) 0.003(5) C68 0.022(8) 0.016(7) 0.010(5) 0.004(5) 0.008(5) 0.000(5) C69 0.025(8) 0.024(7) 0.000(4) 0.003(4) 0.012(5) 0.002(6) C70 0.12(3) 0.05(2) 0.068(18) -0.038(15) -0.011(18) -0.02(2) C71 0.028(11) 0.047(10) 0.013(6) 0.003(6) 0.005(8) 0.010(10) C72 0.001(7) 0.013(7) 0.029(6) 0.003(5) 0.006(5) 0.000(5) C73 0.015(8) 0.041(9) 0.012(6) 0.006(6) -0.006(5) -0.001(6) C74 0.023(7) 0.008(7) 0.013(5) -0.007(5) 0.008(5) -0.015(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N1 1.588(12) . ? B1 C11 1.57(2) . ? B1 C17 1.627(14) . ? B1 C26 1.664(13) . ? Fe1 N3 1.618(10) . ? Fe1 N2 2.022(8) . ? Fe1 P2 2.299(3) . ? Fe1 P1 2.380(5) . ? P1 C17 1.871(10) . ? P1 C18 1.928(17) . ? P1 C22 1.935(10) . ? P2 C26 1.834(9) . ? P2 C27 1.96(3) . ? P2 C31 1.927(10) . ? N1 C35 1.328(10) . ? N1 N2 1.339(10) . ? N2 C37 1.351(10) . ? N3 C1 1.17(6) . ? C1 C2 1.49(7) . ? C1 C7 1.73(5) . ? C1 C6 1.76(5) . ? C2 C3 1.45(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.63(5) . ? C3 C9 1.63(5) . ? C3 H3 1.0000 . ? C4 C5 1.54(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.47(3) . ? C5 C10 1.541(14) . ? C5 H5 1.0000 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.553(14) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.541(13) . ? C8 C10 1.535(13) . ? C8 H8 1.0000 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.412(19) . ? C11 C12 1.46(3) . ? C12 C13 1.32(2) . ? C12 H12 0.9500 . ? C13 C14 1.41(3) . ? C13 H13 0.9500 . ? C14 C15 1.40(4) . ? C14 H14 0.9500 . ? C15 C16 1.41(2) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C20 1.506(17) . ? C18 C19 1.524(15) . ? C18 C21 1.560(18) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.523(13) . ? C22 C25 1.55(3) . ? C22 C24 1.549(17) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.44(4) . ? C27 C29 1.65(4) . ? C27 C30 1.62(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.501(15) . ? C31 C33 1.548(14) . ? C31 C34 1.55(2) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.386(13) . ? C35 H35 0.9500 . ? C36 C37 1.397(13) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? B2 N4 1.611(12) . ? B2 C54 1.630(14) . ? B2 C63 1.637(14) . ? B2 C48 1.662(19) . ? Fe2 N6 1.630(8) . ? Fe2 N5 2.009(7) . ? Fe2 P3 2.305(3) . ? Fe2 P4 2.375(4) . ? N4 C72 1.319(10) . ? N4 N5 1.369(10) . ? N5 C74 1.341(11) . ? N6 C38 1.56(7) . ? P3 C54 1.870(9) . ? P3 C59 1.93(2) . ? P3 C55 1.926(11) . ? P4 C63 1.841(10) . ? P4 C68 1.885(10) . ? P4 C64 1.898(13) . ? C38 C39 1.45(6) . ? C38 C43 1.36(6) . ? C38 C44 1.85(4) . ? C39 C40 1.53(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.55(4) . ? C40 C46 1.515(14) . ? C40 H40 1.0000 . ? C41 C42 1.46(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.50(4) . ? C42 C47 1.67(6) . ? C42 H42 1.0000 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.505(13) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.499(12) . ? C45 C47 1.541(14) . ? C45 H45 1.0000 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.38(3) . ? C48 C53 1.403(18) . ? C49 C50 1.42(2) . ? C49 H49 0.9500 . ? C50 C51 1.400(17) . ? C50 H50 0.9500 . ? C51 C52 1.36(4) . ? C51 H51 0.9500 . ? C52 C53 1.36(3) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.484(14) . ? C55 C57 1.593(15) . ? C55 C58 1.608(16) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C61 1.49(3) . ? C59 C62 1.49(5) . ? C59 C60 1.61(2) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C66 1.535(17) . ? C64 C67 1.536(13) . ? C64 C65 1.557(13) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C69 1.558(13) . ? C68 C71 1.558(16) . ? C68 C70 1.66(4) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.406(13) . ? C72 H72 0.9500 . ? C73 C74 1.389(12) . ? C73 H73 0.9500 . ? C74 H74 0.9500 . ? 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 C11 108.2(9) . . ? N1 B1 C17 102.6(8) . . ? C11 B1 C17 109.9(10) . . ? N1 B1 C26 112.6(8) . . ? C11 B1 C26 112.0(10) . . ? C17 B1 C26 111.0(8) . . ? N3 Fe1 N2 133.4(4) . . ? N3 Fe1 P2 120.0(3) . . ? N2 Fe1 P2 83.7(2) . . ? N3 Fe1 P1 121.6(3) . . ? N2 Fe1 P1 87.4(2) . . ? P2 Fe1 P1 100.85(16) . . ? C17 P1 C18 105.8(6) . . ? C17 P1 C22 105.6(5) . . ? C18 P1 C22 106.5(6) . . ? C17 P1 Fe1 107.5(4) . . ? C18 P1 Fe1 105.8(5) . . ? C22 P1 Fe1 124.4(4) . . ? C26 P2 C27 110.3(12) . . ? C26 P2 C31 108.5(5) . . ? C27 P2 C31 104.0(9) . . ? C26 P2 Fe1 105.7(3) . . ? C27 P2 Fe1 113.9(11) . . ? C31 P2 Fe1 114.4(4) . . ? C35 N1 N2 108.2(7) . . ? C35 N1 B1 129.2(8) . . ? N2 N1 B1 122.5(7) . . ? N1 N2 C37 108.3(8) . . ? N1 N2 Fe1 127.5(6) . . ? C37 N2 Fe1 124.0(8) . . ? C1 N3 Fe1 167(3) . . ? N3 C1 C2 131(4) . . ? N3 C1 C7 113(5) . . ? C2 C1 C7 102(3) . . ? N3 C1 C6 116(4) . . ? C2 C1 C6 97(3) . . ? C7 C1 C6 89(2) . . ? C3 C2 C1 128(3) . . ? C3 C2 H2A 105.9 . . ? C1 C2 H2A 104.1 . . ? C3 C2 H2B 105.5 . . ? C1 C2 H2B 105.6 . . ? H2A C2 H2B 106.2 . . ? C2 C3 C4 110(3) . . ? C2 C3 C9 109(2) . . ? C4 C3 C9 105(3) . . ? C2 C3 H3 110.9 . . ? C4 C3 H3 110.9 . . ? C9 C3 H3 110.7 . . ? C3 C4 C5 106(2) . . ? C3 C4 H4A 110.8 . . ? C5 C4 H4A 110.6 . . ? C3 C4 H4B 110.3 . . ? C5 C4 H4B 110.6 . . ? H4A C4 H4B 108.8 . . ? C6 C5 C4 111(2) . . ? C6 C5 C10 108.9(17) . . ? C4 C5 C10 112.9(15) . . ? C6 C5 H5 107.8 . . ? C4 C5 H5 108.3 . . ? C10 C5 H5 108.2 . . ? C5 C6 C1 120(3) . . ? C5 C6 H6A 107.3 . . ? C1 C6 H6A 107.7 . . ? C5 C6 H6B 107.8 . . ? C1 C6 H6B 106.1 . . ? H6A C6 H6B 106.9 . . ? C1 C7 C8 119(2) . . ? C1 C7 H7A 107.7 . . ? C8 C7 H7A 107.8 . . ? C1 C7 H7B 107.4 . . ? C8 C7 H7B 107.7 . . ? H7A C7 H7B 107.1 . . ? C9 C8 C10 109.1(8) . . ? C9 C8 C7 109.0(9) . . ? C10 C8 C7 109.3(8) . . ? C9 C8 H8 109.8 . . ? C10 C8 H8 109.8 . . ? C7 C8 H8 109.8 . . ? C8 C9 C3 110.0(16) . . ? C8 C9 H9A 109.7 . . ? C3 C9 H9A 110.0 . . ? C8 C9 H9B 109.6 . . ? C3 C9 H9B 109.4 . . ? H9A C9 H9B 108.2 . . ? C5 C10 C8 108.4(9) . . ? C5 C10 H10A 110.0 . . ? C8 C10 H10A 110.0 . . ? C5 C10 H10B 110.0 . . ? C8 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? C16 C11 C12 109.6(16) . . ? C16 C11 B1 126.3(12) . . ? C12 C11 B1 124.1(16) . . ? C13 C12 C11 127(2) . . ? C13 C12 H12 116.3 . . ? C11 C12 H12 116.3 . . ? C12 C13 C14 122.8(18) . . ? C12 C13 H13 118.7 . . ? C14 C13 H13 118.5 . . ? C15 C14 C13 112(2) . . ? C15 C14 H14 123.8 . . ? C13 C14 H14 123.8 . . ? C14 C15 C16 124.9(19) . . ? C14 C15 H15 117.5 . . ? C16 C15 H15 117.6 . . ? C11 C16 C15 122.5(14) . . ? C11 C16 H16 118.7 . . ? C15 C16 H16 118.8 . . ? B1 C17 P1 116.7(7) . . ? B1 C17 H17A 108.1 . . ? P1 C17 H17A 108.1 . . ? B1 C17 H17B 108.2 . . ? P1 C17 H17B 108.1 . . ? H17A C17 H17B 107.3 . . ? C20 C18 C19 105.1(10) . . ? C20 C18 C21 112.9(15) . . ? C19 C18 C21 103.4(12) . . ? C20 C18 P1 115.1(10) . . ? C19 C18 P1 108.5(11) . . ? C21 C18 P1 110.9(11) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.4 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.4 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.4 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C25 110.3(15) . . ? C23 C22 C24 112.3(8) . . ? C25 C22 C24 106.5(12) . . ? C23 C22 P1 108.1(6) . . ? C25 C22 P1 111.8(11) . . ? C24 C22 P1 107.8(8) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.4 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.4 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.4 . . ? C22 C25 H25B 109.6 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.4 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? B1 C26 P2 116.7(7) . . ? B1 C26 H26A 108.2 . . ? P2 C26 H26A 108.1 . . ? B1 C26 H26B 108.1 . . ? P2 C26 H26B 108.1 . . ? H26A C26 H26B 107.3 . . ? C28 C27 C29 119(2) . . ? C28 C27 C30 108.4(19) . . ? C29 C27 C30 100(2) . . ? C28 C27 P2 112(2) . . ? C29 C27 P2 108(2) . . ? C30 C27 P2 107.2(17) . . ? C27 C28 H28A 109.4 . . ? C27 C28 H28B 109.8 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.2 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.3 . . ? C27 C29 H29B 110.1 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.0 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.4 . . ? C27 C30 H30B 109.9 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.1 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C33 107.0(10) . . ? C32 C31 C34 108.7(10) . . ? C33 C31 C34 107.8(10) . . ? C32 C31 P2 109.4(8) . . ? C33 C31 P2 114.8(7) . . ? C34 C31 P2 109.0(9) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.4 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.4 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N1 C35 C36 111.1(9) . . ? N1 C35 H35 124.5 . . ? C36 C35 H35 124.4 . . ? C35 C36 C37 102.9(9) . . ? C35 C36 H36 128.6 . . ? C37 C36 H36 128.5 . . ? N2 C37 C36 109.5(10) . . ? N2 C37 H37 125.3 . . ? C36 C37 H37 125.2 . . ? N4 B2 C54 114.3(8) . . ? N4 B2 C63 102.4(8) . . ? C54 B2 C63 114.1(8) . . ? N4 B2 C48 104.7(8) . . ? C54 B2 C48 110.3(9) . . ? C63 B2 C48 110.5(9) . . ? N6 Fe2 N5 132.8(4) . . ? N6 Fe2 P3 119.4(3) . . ? N5 Fe2 P3 84.8(2) . . ? N6 Fe2 P4 122.1(3) . . ? N5 Fe2 P4 87.2(2) . . ? P3 Fe2 P4 100.96(16) . . ? C72 N4 N5 107.6(7) . . ? C72 N4 B2 131.2(8) . . ? N5 N4 B2 121.1(6) . . ? C74 N5 N4 108.9(7) . . ? C74 N5 Fe2 124.6(7) . . ? N4 N5 Fe2 126.5(6) . . ? C38 N6 Fe2 162.5(18) . . ? C54 P3 C59 108.6(6) . . ? C54 P3 C55 106.6(5) . . ? C59 P3 C55 104.2(9) . . ? C54 P3 Fe2 106.4(3) . . ? C59 P3 Fe2 115.2(8) . . ? C55 P3 Fe2 115.4(4) . . ? C63 P4 C68 105.8(4) . . ? C63 P4 C64 105.9(5) . . ? C68 P4 C64 106.5(5) . . ? C63 P4 Fe2 108.4(3) . . ? C68 P4 Fe2 122.6(4) . . ? C64 P4 Fe2 106.7(4) . . ? C39 C38 C43 128(4) . . ? C39 C38 N6 112(4) . . ? C43 C38 N6 113(4) . . ? C39 C38 C44 100(3) . . ? C43 C38 C44 103(4) . . ? N6 C38 C44 92.5(19) . . ? C38 C39 C40 108(4) . . ? C38 C39 H39A 111.7 . . ? C40 C39 H39A 110.1 . . ? C38 C39 H39B 108.4 . . ? C40 C39 H39B 109.9 . . ? H39A C39 H39B 108.5 . . ? C41 C40 C39 104.6(19) . . ? C41 C40 C46 109(2) . . ? C39 C40 C46 110.8(15) . . ? C41 C40 H40 110.8 . . ? C39 C40 H40 110.9 . . ? C46 C40 H40 110.6 . . ? C40 C41 C42 118(3) . . ? C40 C41 H41A 108.1 . . ? C42 C41 H41A 108.1 . . ? C40 C41 H41B 107.6 . . ? C42 C41 H41B 107.4 . . ? H41A C41 H41B 107.3 . . ? C43 C42 C41 107(3) . . ? C43 C42 C47 105(3) . . ? C41 C42 C47 105(4) . . ? C43 C42 H42 112.7 . . ? C41 C42 H42 113.0 . . ? C47 C42 H42 112.7 . . ? C38 C43 C42 113(4) . . ? C38 C43 H43A 107.8 . . ? C42 C43 H43A 109.0 . . ? C38 C43 H43B 109.8 . . ? C42 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? C45 C44 C38 103(2) . . ? C45 C44 H44A 111.2 . . ? C38 C44 H44A 112.0 . . ? C45 C44 H44B 111.3 . . ? C38 C44 H44B 110.5 . . ? H44A C44 H44B 109.2 . . ? C46 C45 C44 113.0(9) . . ? C46 C45 C47 110.3(8) . . ? C44 C45 C47 109.7(9) . . ? C46 C45 H45 107.9 . . ? C44 C45 H45 108.0 . . ? C47 C45 H45 107.8 . . ? C45 C46 C40 109.8(9) . . ? C45 C46 H46A 109.7 . . ? C40 C46 H46A 109.6 . . ? C45 C46 H46B 109.7 . . ? C40 C46 H46B 109.8 . . ? H46A C46 H46B 108.2 . . ? C45 C47 C42 109(2) . . ? C45 C47 H47A 110.0 . . ? C42 C47 H47A 110.0 . . ? C45 C47 H47B 109.9 . . ? C42 C47 H47B 109.6 . . ? H47A C47 H47B 108.3 . . ? C49 C48 C53 116.5(15) . . ? C49 C48 B2 121.0(15) . . ? C53 C48 B2 122.5(13) . . ? C48 C49 C50 122.3(17) . . ? C48 C49 H49 118.8 . . ? C50 C49 H49 118.9 . . ? C51 C50 C49 118.2(13) . . ? C51 C50 H50 120.9 . . ? C49 C50 H50 120.9 . . ? C52 C51 C50 118.6(15) . . ? C52 C51 H51 120.7 . . ? C50 C51 H51 120.7 . . ? C53 C52 C51 123(2) . . ? C53 C52 H52 118.5 . . ? C51 C52 H52 118.6 . . ? C52 C53 C48 121.2(16) . . ? C52 C53 H53 119.5 . . ? C48 C53 H53 119.4 . . ? B2 C54 P3 114.6(6) . . ? B2 C54 H54A 108.6 . . ? P3 C54 H54A 108.6 . . ? B2 C54 H54B 108.7 . . ? P3 C54 H54B 108.6 . . ? H54A C54 H54B 107.6 . . ? C56 C55 C57 106.5(9) . . ? C56 C55 C58 107.2(11) . . ? C57 C55 C58 106.1(12) . . ? C56 C55 P3 111.3(8) . . ? C57 C55 P3 112.1(7) . . ? C58 C55 P3 113.2(11) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.4 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.4 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C55 C58 H58A 109.4 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C61 C59 C62 119(2) . . ? C61 C59 C60 103.9(15) . . ? C62 C59 C60 105.2(15) . . ? C61 C59 P3 109.4(12) . . ? C62 C59 P3 110.4(19) . . ? C60 C59 P3 107.9(14) . . ? C59 C60 H60A 109.3 . . ? C59 C60 H60B 109.6 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 H61A 109.6 . . ? C59 C61 H61B 109.8 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.0 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C59 C62 H62A 109.0 . . ? C59 C62 H62B 110.3 . . ? H62A C62 H62B 109.5 . . ? C59 C62 H62C 109.2 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? B2 C63 P4 115.5(6) . . ? B2 C63 H63A 108.5 . . ? P4 C63 H63A 108.4 . . ? B2 C63 H63B 108.3 . . ? P4 C63 H63B 108.4 . . ? H63A C63 H63B 107.5 . . ? C66 C64 C67 107.2(12) . . ? C66 C64 C65 103.6(11) . . ? C67 C64 C65 105.5(9) . . ? C66 C64 P4 113.4(9) . . ? C67 C64 P4 116.9(8) . . ? C65 C64 P4 109.1(8) . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C64 C66 H66A 109.5 . . ? C64 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C64 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C64 C67 H67A 109.5 . . ? C64 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C64 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C69 C68 C71 110.5(9) . . ? C69 C68 C70 102.7(17) . . ? C71 C68 C70 107.8(15) . . ? C69 C68 P4 108.5(6) . . ? C71 C68 P4 109.8(9) . . ? C70 C68 P4 117.1(13) . . ? C68 C69 H69A 109.4 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.4 . . ? C68 C70 H70B 109.4 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.6 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C68 C71 H71A 109.5 . . ? C68 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C68 C71 H71C 109.4 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N4 C72 C73 110.4(8) . . ? N4 C72 H72 124.8 . . ? C73 C72 H72 124.8 . . ? C72 C73 C74 104.0(9) . . ? C72 C73 H73 128.0 . . ? C74 C73 H73 128.0 . . ? N5 C74 C73 109.1(10) . . ? N5 C74 H74 125.4 . . ? C73 C74 H74 125.5 . . ? _diffrn_measured_fraction_theta_max 0.318 _diffrn_reflns_theta_full 27.68 _diffrn_measured_fraction_theta_full 0.318 _refine_diff_density_max 0.560 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.081 #===END data_cmt46 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42.75 H36.75 B0.75 Fe0.75 N2.25 P1.50' _chemical_formula_weight 678.44 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' 'P' 'P' 0.1023 0.0942 '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 Monoclinic _symmetry_space_group_name_H-M C2/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 10.8828(9) _cell_length_b 20.2565(17) _cell_length_c 33.573(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.412(2) _cell_angle_gamma 90.00 _cell_volume 7379.1(11) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3176 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.88 _exptl_crystal_description block _exptl_crystal_colour purple-blac _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2838 _exptl_absorpt_coefficient_mu 0.412 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17743 _diffrn_reflns_av_R_equivalents 0.0940 _diffrn_reflns_av_sigmaI/netI 0.1163 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 27.68 _reflns_number_total 5487 _reflns_number_gt 3057 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5487 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1539 _refine_ls_R_factor_gt 0.0893 _refine_ls_wR_factor_ref 0.1301 _refine_ls_wR_factor_gt 0.1237 _refine_ls_goodness_of_fit_ref 1.897 _refine_ls_restrained_S_all 1.897 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.1515(11) 0.8728(6) 0.4180(3) 0.016(3) Uiso 1 1 d . . . Fe1 Fe 0.32580(12) 0.99931(8) 0.38440(3) 0.0140(4) Uiso 1 1 d . . . P1 P 0.3665(3) 0.88670(15) 0.36962(8) 0.0141(8) Uiso 1 1 d . . . P2 P 0.1141(2) 1.00108(15) 0.37509(6) 0.0107(6) Uiso 1 1 d . . . N1 N 0.2239(7) 0.9190(4) 0.4503(2) 0.0102(19) Uiso 1 1 d . . . N2 N 0.2951(8) 0.9696(4) 0.4401(2) 0.020(2) Uiso 1 1 d . . . N3 N 0.4061(8) 1.0588(4) 0.3668(2) 0.018(2) Uiso 1 1 d . . . C1 C 0.464(3) 1.1095(15) 0.3511(8) 0.019(10) Uiso 1 1 d . . . C2 C 0.3968(10) 1.1772(5) 0.3568(3) 0.017(3) Uiso 1 1 d . . . H2A H 0.3088 1.1721 0.3474 0.020 Uiso 1 1 calc R . . H2B H 0.4006 1.1875 0.3857 0.020 Uiso 1 1 calc R . . C3 C 0.4476(18) 1.2339(11) 0.3357(6) 0.011(7) Uiso 1 1 d . . . H3 H 0.4016 1.2746 0.3424 0.013 Uiso 1 1 calc R . . C4 C 0.4493(11) 1.2297(6) 0.2940(3) 0.005(3) Uiso 1 1 d . . . H4A H 0.4938 1.2681 0.2839 0.006 Uiso 1 1 calc R . . H4B H 0.3639 1.2303 0.2815 0.006 Uiso 1 1 calc R . . C5 C 0.5135(10) 1.1657(5) 0.2832(3) 0.029(3) Uiso 1 1 d . . . H5 H 0.5062 1.1605 0.2535 0.035 Uiso 1 1 calc R . . C6 C 0.4592(12) 1.1056(7) 0.3018(3) 0.017(4) Uiso 1 1 d . . . H6A H 0.5048 1.0659 0.2941 0.020 Uiso 1 1 calc R . . H6B H 0.3724 1.1006 0.2911 0.020 Uiso 1 1 calc R . . C7 C 0.5990(9) 1.1182(5) 0.3625(3) 0.013(3) Uiso 1 1 d . . . H7A H 0.6426 1.0778 0.3548 0.016 Uiso 1 1 calc R . . H7B H 0.6109 1.1222 0.3920 0.016 Uiso 1 1 calc R . . C8 C 0.6606(10) 1.1786(5) 0.3437(3) 0.022(3) Uiso 1 1 d . . . H8 H 0.7492 1.1814 0.3539 0.026 Uiso 1 1 calc R . . C9 C 0.5941(9) 1.2416(5) 0.3540(3) 0.018(3) Uiso 1 1 d . . . H9A H 0.6327 1.2803 0.3420 0.021 Uiso 1 1 calc R . . H9B H 0.5982 1.2477 0.3834 0.021 Uiso 1 1 calc R . . C10 C 0.6505(10) 1.1700(6) 0.2978(3) 0.035(3) Uiso 1 1 d . . . H10A H 0.6893 1.2080 0.2851 0.043 Uiso 1 1 calc R . . H10B H 0.6937 1.1293 0.2905 0.043 Uiso 1 1 calc R . . C11 C 0.0700(10) 0.8221(5) 0.4411(3) 0.014(3) Uiso 1 1 d . . . C12 C -0.0449(13) 0.8385(6) 0.4562(3) 0.018(3) Uiso 1 1 d . . . H12 H -0.0735 0.8823 0.4516 0.021 Uiso 1 1 calc R . . C13 C -0.1172(10) 0.7986(5) 0.4762(3) 0.022(3) Uiso 1 1 d . . . H13 H -0.1938 0.8144 0.4842 0.027 Uiso 1 1 calc R . . C14 C -0.0796(12) 0.7338(7) 0.4854(4) 0.031(4) Uiso 1 1 d . . . H14 H -0.1275 0.7052 0.5004 0.038 Uiso 1 1 calc R . . C15 C 0.0304(13) 0.7136(6) 0.4715(3) 0.017(3) Uiso 1 1 d . . . H15 H 0.0565 0.6693 0.4759 0.020 Uiso 1 1 calc R . . C16 C 0.1065(9) 0.7571(5) 0.4506(3) 0.016(3) Uiso 1 1 d . . . H16 H 0.1838 0.7417 0.4430 0.019 Uiso 1 1 calc R . . C17 C 0.2610(9) 0.8353(5) 0.3974(2) 0.015(3) Uiso 1 1 d . . . H17A H 0.2233 0.8019 0.3787 0.018 Uiso 1 1 calc R . . H17B H 0.3112 0.8113 0.4185 0.018 Uiso 1 1 calc R . . C18 C 0.5294(12) 0.8689(6) 0.3931(3) 0.025(3) Uiso 1 1 d . . . C19 C 0.5458(10) 0.9044(5) 0.4336(3) 0.024(3) Uiso 1 1 d . . . H19A H 0.4830 0.8889 0.4508 0.036 Uiso 1 1 calc R . . H19B H 0.5369 0.9521 0.4295 0.036 Uiso 1 1 calc R . . H19C H 0.6279 0.8949 0.4463 0.036 Uiso 1 1 calc R . . C20 C 0.5574(10) 0.7976(5) 0.4022(3) 0.028(3) Uiso 1 1 d . . . H20A H 0.6320 0.7945 0.4204 0.041 Uiso 1 1 calc R . . H20B H 0.5705 0.7742 0.3773 0.041 Uiso 1 1 calc R . . H20C H 0.4881 0.7776 0.4147 0.041 Uiso 1 1 calc R . . C21 C 0.6293(13) 0.9008(6) 0.3681(3) 0.040(4) Uiso 1 1 d . . . H21A H 0.7100 0.8980 0.3831 0.060 Uiso 1 1 calc R . . H21B H 0.6086 0.9472 0.3628 0.060 Uiso 1 1 calc R . . H21C H 0.6319 0.8771 0.3427 0.060 Uiso 1 1 calc R . . C22 C 0.3587(9) 0.8509(5) 0.3161(3) 0.015(3) Uiso 1 1 d . . . C23 C 0.2263(9) 0.8315(5) 0.3042(3) 0.018(3) Uiso 1 1 d . . . H23A H 0.1705 0.8636 0.3151 0.028 Uiso 1 1 calc R . . H23B H 0.2101 0.7875 0.3147 0.028 Uiso 1 1 calc R . . H23C H 0.2128 0.8309 0.2750 0.028 Uiso 1 1 calc R . . C24 C 0.4076(11) 0.9028(6) 0.2878(3) 0.028(3) Uiso 1 1 d . . . H24A H 0.3957 0.8870 0.2602 0.042 Uiso 1 1 calc R . . H24B H 0.4956 0.9101 0.2949 0.042 Uiso 1 1 calc R . . H24C H 0.3627 0.9443 0.2904 0.042 Uiso 1 1 calc R . . C25 C 0.4361(13) 0.7890(7) 0.3131(4) 0.009(4) Uiso 1 1 d . . . H25A H 0.4153 0.7575 0.3337 0.013 Uiso 1 1 calc R . . H25B H 0.5236 0.8005 0.3171 0.013 Uiso 1 1 calc R . . H25C H 0.4193 0.7691 0.2867 0.013 Uiso 1 1 calc R . . C26 C 0.0644(9) 0.9168(4) 0.3847(3) 0.016(3) Uiso 1 1 d . . . H26A H -0.0199 0.9189 0.3938 0.019 Uiso 1 1 calc R . . H26B H 0.0591 0.8925 0.3591 0.019 Uiso 1 1 calc R . . C27 C 0.0366(13) 1.0609(6) 0.4097(4) 0.008(4) Uiso 1 1 d . . . C28 C 0.0986(9) 1.1260(5) 0.4126(3) 0.019(3) Uiso 1 1 d . . . H28A H 0.0837 1.1496 0.3872 0.028 Uiso 1 1 calc R . . H28B H 0.1874 1.1196 0.4184 0.028 Uiso 1 1 calc R . . H28C H 0.0656 1.1518 0.4340 0.028 Uiso 1 1 calc R . . C29 C -0.1076(12) 1.0625(7) 0.3991(4) 0.029(5) Uiso 1 1 d . . . H29A H -0.1482 1.0812 0.4216 0.044 Uiso 1 1 calc R . . H29B H -0.1377 1.0175 0.3939 0.044 Uiso 1 1 calc R . . H29C H -0.1261 1.0899 0.3753 0.044 Uiso 1 1 calc R . . C30 C 0.0435(9) 1.0308(5) 0.4540(2) 0.017(3) Uiso 1 1 d . . . H30A H 0.1296 1.0292 0.4649 0.026 Uiso 1 1 calc R . . H30B H 0.0091 0.9860 0.4531 0.026 Uiso 1 1 calc R . . H30C H -0.0041 1.0586 0.4710 0.026 Uiso 1 1 calc R . . C31 C 0.0499(10) 1.0261(5) 0.3219(3) 0.016(3) Uiso 1 1 d . . . C32 C 0.1358(9) 1.0021(5) 0.2925(2) 0.025(3) Uiso 1 1 d . . . H32A H 0.1050 1.0155 0.2655 0.037 Uiso 1 1 calc R . . H32B H 0.1412 0.9539 0.2938 0.037 Uiso 1 1 calc R . . H32C H 0.2177 1.0212 0.2989 0.037 Uiso 1 1 calc R . . C33 C 0.0349(9) 1.1014(5) 0.3154(3) 0.020(3) Uiso 1 1 d . . . H33A H 0.1140 1.1234 0.3221 0.030 Uiso 1 1 calc R . . H33B H -0.0266 1.1184 0.3327 0.030 Uiso 1 1 calc R . . H33C H 0.0077 1.1102 0.2874 0.030 Uiso 1 1 calc R . . C34 C -0.0787(12) 0.9912(6) 0.3113(3) 0.024(3) Uiso 1 1 d . . . H34A H -0.1065 1.0000 0.2834 0.037 Uiso 1 1 calc R . . H34B H -0.1395 1.0084 0.3287 0.037 Uiso 1 1 calc R . . H34C H -0.0698 0.9434 0.3154 0.037 Uiso 1 1 calc R . . C35 C 0.2349(9) 0.9138(5) 0.4900(3) 0.012(2) Uiso 1 1 d . . . H35 H 0.1940 0.8816 0.5048 0.014 Uiso 1 1 calc R . . C36 C 0.3128(9) 0.9608(5) 0.5065(3) 0.020(3) Uiso 1 1 d . . . H36 H 0.3358 0.9684 0.5340 0.023 Uiso 1 1 calc R . . C37 C 0.3508(8) 0.9953(5) 0.4737(2) 0.018(2) Uiso 1 1 d . . . H37 H 0.4071 1.0312 0.4749 0.021 Uiso 1 1 calc R . . B2 B 0.3096(11) 0.3706(6) 0.4192(3) 0.013(3) Uiso 1 1 d . . . Fe2 Fe 0.11777(12) 0.49665(8) 0.38786(3) 0.0144(4) Uiso 1 1 d . . . N4 N 0.2547(7) 0.4159(3) 0.45317(19) 0.0071(19) Uiso 1 1 d . . . N5 N 0.1765(7) 0.4672(4) 0.4432(2) 0.018(2) Uiso 1 1 d . . . N6 N 0.0294(8) 0.5573(4) 0.3710(2) 0.014(2) Uiso 1 1 d . . . P3 P 0.3242(2) 0.49789(15) 0.37685(6) 0.0107(6) Uiso 1 1 d . . . P4 P 0.0676(3) 0.38476(17) 0.37408(10) 0.0152(8) Uiso 1 1 d . . . C38 C -0.044(3) 0.6154(13) 0.3481(7) 0.008(9) Uiso 1 1 d . . . C39 C -0.0811(12) 0.5958(7) 0.3076(3) 0.023(4) Uiso 1 1 d . . . H39A H -0.1306 0.5548 0.3077 0.027 Uiso 1 1 calc R . . H39B H -0.0076 0.5873 0.2928 0.027 Uiso 1 1 calc R . . C40 C -0.1566(10) 0.6507(5) 0.2880(3) 0.025(3) Uiso 1 1 d . . . H40 H -0.1806 0.6393 0.2595 0.030 Uiso 1 1 calc R . . C41 C -0.0827(14) 0.7111(7) 0.2902(4) 0.039(5) Uiso 1 1 d . . . H41A H -0.1324 0.7474 0.2775 0.046 Uiso 1 1 calc R . . H41B H -0.0101 0.7046 0.2746 0.046 Uiso 1 1 calc R . . C42 C -0.0323(19) 0.7346(13) 0.3383(6) 0.024(8) Uiso 1 1 d . . . H42 H 0.0186 0.7758 0.3399 0.029 Uiso 1 1 calc R . . C43 C 0.0336(10) 0.6746(5) 0.3542(3) 0.021(3) Uiso 1 1 d . . . H43A H 0.1103 0.6688 0.3405 0.025 Uiso 1 1 calc R . . H43B H 0.0567 0.6804 0.3831 0.025 Uiso 1 1 calc R . . C44 C -0.1619(9) 0.6209(5) 0.3741(3) 0.022(3) Uiso 1 1 d . . . H44A H -0.2096 0.5793 0.3733 0.026 Uiso 1 1 calc R . . H44B H -0.1372 0.6324 0.4023 0.026 Uiso 1 1 calc R . . C45 C -0.2343(10) 0.6759(5) 0.3533(3) 0.022(3) Uiso 1 1 d . . . H45 H -0.3114 0.6819 0.3672 0.027 Uiso 1 1 calc R . . C46 C -0.2714(10) 0.6612(5) 0.3105(3) 0.031(3) Uiso 1 1 d . . . H46A H -0.3202 0.6984 0.2985 0.037 Uiso 1 1 calc R . . H46B H -0.3233 0.6210 0.3086 0.037 Uiso 1 1 calc R . . C47 C -0.1604(9) 0.7407(5) 0.3579(3) 0.026(3) Uiso 1 1 d . . . H47A H -0.1451 0.7514 0.3866 0.031 Uiso 1 1 calc R . . H47B H -0.2092 0.7771 0.3449 0.031 Uiso 1 1 calc R . . C48 C 0.4037(10) 0.3187(5) 0.4435(3) 0.015(3) Uiso 1 1 d . . . C49 C 0.5243(13) 0.3365(6) 0.4567(3) 0.014(3) Uiso 1 1 d . . . H49 H 0.5525 0.3793 0.4503 0.017 Uiso 1 1 calc R . . C50 C 0.6055(10) 0.2944(5) 0.4789(3) 0.024(3) Uiso 1 1 d . . . H50 H 0.6856 0.3092 0.4880 0.028 Uiso 1 1 calc R . . C51 C 0.5675(11) 0.2310(6) 0.4874(3) 0.025(3) Uiso 1 1 d . . . H51 H 0.6224 0.2009 0.5013 0.030 Uiso 1 1 calc R . . C52 C 0.4486(13) 0.2125(6) 0.4754(3) 0.016(3) Uiso 1 1 d . . . H52 H 0.4209 0.1697 0.4820 0.019 Uiso 1 1 calc R . . C53 C 0.3697(9) 0.2541(5) 0.4540(3) 0.013(2) Uiso 1 1 d . . . H53 H 0.2890 0.2390 0.4459 0.016 Uiso 1 1 calc R . . C54 C 0.3825(9) 0.4128(5) 0.3867(3) 0.018(3) Uiso 1 1 d . . . H54A H 0.3773 0.3882 0.3611 0.022 Uiso 1 1 calc R . . H54B H 0.4706 0.4154 0.3964 0.022 Uiso 1 1 calc R . . C55 C 0.3626(10) 0.5209(5) 0.3234(3) 0.015(3) Uiso 1 1 d . . . C56 C 0.2641(9) 0.4947(6) 0.2933(3) 0.037(3) Uiso 1 1 d . . . H56A H 0.2871 0.5040 0.2662 0.055 Uiso 1 1 calc R . . H56B H 0.1853 0.5161 0.2974 0.055 Uiso 1 1 calc R . . H56C H 0.2559 0.4469 0.2967 0.055 Uiso 1 1 calc R . . C57 C 0.3702(10) 0.5969(5) 0.3168(3) 0.026(3) Uiso 1 1 d . . . H57A H 0.3877 0.6059 0.2891 0.039 Uiso 1 1 calc R . . H57B H 0.4361 0.6154 0.3350 0.039 Uiso 1 1 calc R . . H57C H 0.2915 0.6173 0.3222 0.039 Uiso 1 1 calc R . . C58 C 0.4892(12) 0.4915(6) 0.3124(3) 0.028(3) Uiso 1 1 d . . . H58A H 0.4814 0.4436 0.3090 0.042 Uiso 1 1 calc R . . H58B H 0.5526 0.5010 0.3340 0.042 Uiso 1 1 calc R . . H58C H 0.5126 0.5114 0.2875 0.042 Uiso 1 1 calc R . . C59 C 0.4200(13) 0.5577(6) 0.4109(4) 0.014(3) Uiso 1 1 d . . . C60 C 0.4335(10) 0.5294(5) 0.4548(2) 0.020(3) Uiso 1 1 d . . . H60A H 0.4937 0.5558 0.4712 0.030 Uiso 1 1 calc R . . H60B H 0.4617 0.4835 0.4543 0.030 Uiso 1 1 calc R . . H60C H 0.3536 0.5312 0.4664 0.030 Uiso 1 1 calc R . . C61 C 0.3570(9) 0.6222(5) 0.4134(3) 0.020(3) Uiso 1 1 d . . . H61A H 0.4040 0.6505 0.4327 0.030 Uiso 1 1 calc R . . H61B H 0.2740 0.6153 0.4221 0.030 Uiso 1 1 calc R . . H61C H 0.3512 0.6434 0.3871 0.030 Uiso 1 1 calc R . . C62 C 0.5527(13) 0.5617(8) 0.3983(4) 0.035(6) Uiso 1 1 d . . . H62A H 0.5522 0.5813 0.3716 0.052 Uiso 1 1 calc R . . H62B H 0.5881 0.5172 0.3978 0.052 Uiso 1 1 calc R . . H62C H 0.6025 0.5891 0.4174 0.052 Uiso 1 1 calc R . . C63 C 0.1866(9) 0.3326(5) 0.4001(3) 0.012(2) Uiso 1 1 d . . . H63A H 0.1488 0.3089 0.4219 0.015 Uiso 1 1 calc R . . H63B H 0.2124 0.2990 0.3810 0.015 Uiso 1 1 calc R . . C64 C -0.0804(11) 0.3675(5) 0.3976(3) 0.022(3) Uiso 1 1 d . . . C65 C -0.0761(10) 0.4017(5) 0.4393(3) 0.031(3) Uiso 1 1 d . . . H65A H -0.0651 0.4494 0.4360 0.047 Uiso 1 1 calc R . . H65B H -0.0071 0.3839 0.4565 0.047 Uiso 1 1 calc R . . H65C H -0.1535 0.3934 0.4516 0.047 Uiso 1 1 calc R . . C66 C -0.1945(11) 0.3976(6) 0.3735(3) 0.028(4) Uiso 1 1 d . . . H66A H -0.2133 0.3718 0.3491 0.042 Uiso 1 1 calc R . . H66B H -0.1767 0.4433 0.3664 0.042 Uiso 1 1 calc R . . H66C H -0.2654 0.3967 0.3898 0.042 Uiso 1 1 calc R . . C67 C -0.1084(10) 0.2938(5) 0.4068(3) 0.024(3) Uiso 1 1 d . . . H67A H -0.1773 0.2914 0.4239 0.036 Uiso 1 1 calc R . . H67B H -0.0353 0.2734 0.4206 0.036 Uiso 1 1 calc R . . H67C H -0.1301 0.2703 0.3817 0.036 Uiso 1 1 calc R . . C68 C 0.0460(9) 0.3507(5) 0.3212(3) 0.015(3) Uiso 1 1 d . . . C69 C 0.1747(9) 0.3305(5) 0.3081(3) 0.015(3) Uiso 1 1 d . . . H69A H 0.1697 0.3244 0.2790 0.023 Uiso 1 1 calc R . . H69B H 0.2008 0.2891 0.3212 0.023 Uiso 1 1 calc R . . H69C H 0.2346 0.3653 0.3156 0.023 Uiso 1 1 calc R . . C70 C -0.0268(14) 0.2841(9) 0.3152(6) 0.040(6) Uiso 1 1 d . . . H70A H -0.0232 0.2690 0.2876 0.059 Uiso 1 1 calc R . . H70B H -0.1129 0.2910 0.3208 0.059 Uiso 1 1 calc R . . H70C H 0.0103 0.2507 0.3336 0.059 Uiso 1 1 calc R . . C71 C -0.0139(11) 0.4055(6) 0.2932(3) 0.025(3) Uiso 1 1 d . . . H71A H 0.0260 0.4480 0.2996 0.038 Uiso 1 1 calc R . . H71B H -0.1020 0.4088 0.2971 0.038 Uiso 1 1 calc R . . H71C H -0.0032 0.3942 0.2653 0.038 Uiso 1 1 calc R . . C72 C 0.2654(9) 0.4112(5) 0.4927(3) 0.014(3) Uiso 1 1 d . . . H72 H 0.3149 0.3797 0.5075 0.017 Uiso 1 1 calc R . . C73 C 0.1936(9) 0.4590(5) 0.5093(3) 0.023(3) Uiso 1 1 d . . . H73 H 0.1830 0.4656 0.5369 0.028 Uiso 1 1 calc R . . C74 C 0.1401(8) 0.4955(5) 0.4772(2) 0.013(2) Uiso 1 1 d . . . H74 H 0.0881 0.5329 0.4787 0.016 Uiso 1 1 calc R . . _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 1.595(12) . ? B1 C11 1.597(15) . ? B1 C17 1.613(15) . ? B1 C26 1.666(13) . ? Fe1 N3 1.626(9) . ? Fe1 N2 2.017(8) . ? Fe1 P2 2.301(3) . ? Fe1 P1 2.383(4) . ? P1 C17 1.853(10) . ? P1 C18 1.919(12) . ? P1 C22 1.934(9) . ? P2 C26 1.828(9) . ? P2 C27 1.919(14) . ? P2 C31 1.936(9) . ? N1 C35 1.333(10) . ? N1 N2 1.345(10) . ? N2 C37 1.344(10) . ? N3 C1 1.34(3) . ? C1 C7 1.50(3) . ? C1 C2 1.57(3) . ? C1 C6 1.65(3) . ? C2 C3 1.48(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.40(2) . ? C3 C9 1.67(2) . ? C3 H3 1.0000 . ? C4 C5 1.531(15) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.511(15) . ? C5 C10 1.536(14) . ? C5 H5 1.0000 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.552(13) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.519(13) . ? C8 C10 1.547(13) . ? C8 H8 1.0000 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.406(13) . ? C11 C12 1.423(17) . ? C12 C13 1.343(14) . ? C12 H12 0.9500 . ? C13 C14 1.403(15) . ? C13 H13 0.9500 . ? C14 C15 1.381(18) . ? C14 H14 0.9500 . ? C15 C16 1.428(14) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C20 1.503(13) . ? C18 C19 1.535(13) . ? C18 C21 1.563(16) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C25 1.517(16) . ? C22 C23 1.517(13) . ? C22 C24 1.538(14) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.480(15) . ? C27 C29 1.582(19) . ? C27 C30 1.604(15) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.491(13) . ? C31 C33 1.547(13) . ? C31 C34 1.585(16) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.365(12) . ? C35 H35 0.9500 . ? C36 C37 1.392(12) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? B2 N4 1.614(13) . ? B2 C63 1.633(14) . ? B2 C54 1.638(14) . ? B2 C48 1.642(14) . ? Fe2 N6 1.635(8) . ? Fe2 N5 2.007(7) . ? Fe2 P3 2.305(3) . ? Fe2 P4 2.369(4) . ? N4 C72 1.328(10) . ? N4 N5 1.369(9) . ? N5 C74 1.363(10) . ? N6 C38 1.59(3) . ? P3 C54 1.858(10) . ? P3 C59 1.918(13) . ? P3 C55 1.932(10) . ? P4 C63 1.839(9) . ? P4 C64 1.881(12) . ? P4 C68 1.902(9) . ? C38 C39 1.44(3) . ? C38 C43 1.47(3) . ? C38 C44 1.61(3) . ? C39 C40 1.504(16) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.462(15) . ? C40 C46 1.525(14) . ? C40 H40 1.0000 . ? C41 C42 1.73(2) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.49(2) . ? C42 C47 1.59(2) . ? C42 H42 1.0000 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.504(13) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.491(12) . ? C45 C47 1.541(13) . ? C45 H45 1.0000 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.400(16) . ? C48 C53 1.411(13) . ? C49 C50 1.399(14) . ? C49 H49 0.9500 . ? C50 C51 1.385(13) . ? C50 H50 0.9500 . ? C51 C52 1.378(17) . ? C51 H51 0.9500 . ? C52 C53 1.367(14) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.511(12) . ? C55 C57 1.560(13) . ? C55 C58 1.571(15) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C61 1.482(15) . ? C59 C62 1.54(2) . ? C59 C60 1.580(14) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C66 1.553(14) . ? C64 C67 1.559(13) . ? C64 C65 1.559(13) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C69 1.555(13) . ? C68 C71 1.565(13) . ? C68 C70 1.569(18) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.387(13) . ? C72 H72 0.9500 . ? C73 C74 1.398(12) . ? C73 H73 0.9500 . ? C74 H74 0.9500 . ? 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 C11 108.1(8) . . ? N1 B1 C17 103.0(8) . . ? C11 B1 C17 111.3(9) . . ? N1 B1 C26 111.5(8) . . ? C11 B1 C26 111.2(9) . . ? C17 B1 C26 111.4(8) . . ? N3 Fe1 N2 133.6(4) . . ? N3 Fe1 P2 120.0(3) . . ? N2 Fe1 P2 84.0(2) . . ? N3 Fe1 P1 121.3(3) . . ? N2 Fe1 P1 87.4(2) . . ? P2 Fe1 P1 100.76(13) . . ? C17 P1 C18 106.0(5) . . ? C17 P1 C22 105.8(4) . . ? C18 P1 C22 106.6(5) . . ? C17 P1 Fe1 107.5(3) . . ? C18 P1 Fe1 105.9(4) . . ? C22 P1 Fe1 123.8(3) . . ? C26 P2 C27 109.5(5) . . ? C26 P2 C31 108.5(4) . . ? C27 P2 C31 104.4(5) . . ? C26 P2 Fe1 105.6(3) . . ? C27 P2 Fe1 114.2(4) . . ? C31 P2 Fe1 114.6(3) . . ? C35 N1 N2 107.8(7) . . ? C35 N1 B1 129.4(8) . . ? N2 N1 B1 122.6(7) . . ? C37 N2 N1 108.2(7) . . ? C37 N2 Fe1 124.5(7) . . ? N1 N2 Fe1 127.1(5) . . ? C1 N3 Fe1 175.6(15) . . ? N3 C1 C7 118.1(19) . . ? N3 C1 C2 113(2) . . ? C7 C1 C2 109(2) . . ? N3 C1 C6 112(2) . . ? C7 C1 C6 103(2) . . ? C2 C1 C6 100.6(15) . . ? C3 C2 C1 115.1(17) . . ? C3 C2 H2A 108.5 . . ? C1 C2 H2A 108.5 . . ? C3 C2 H2B 108.5 . . ? C1 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? C4 C3 C2 117.7(16) . . ? C4 C3 C9 106.7(13) . . ? C2 C3 C9 106.1(12) . . ? C4 C3 H3 108.7 . . ? C2 C3 H3 108.7 . . ? C9 C3 H3 108.7 . . ? C3 C4 C5 109.2(12) . . ? C3 C4 H4A 109.8 . . ? C5 C4 H4A 109.8 . . ? C3 C4 H4B 109.8 . . ? C5 C4 H4B 109.8 . . ? H4A C4 H4B 108.3 . . ? C6 C5 C4 112.6(10) . . ? C6 C5 C10 108.3(9) . . ? C4 C5 C10 109.0(9) . . ? C6 C5 H5 109.0 . . ? C4 C5 H5 109.0 . . ? C10 C5 H5 109.0 . . ? C5 C6 C1 113.2(14) . . ? C5 C6 H6A 108.9 . . ? C1 C6 H6A 108.9 . . ? C5 C6 H6B 108.9 . . ? C1 C6 H6B 108.9 . . ? H6A C6 H6B 107.8 . . ? C1 C7 C8 115.7(13) . . ? C1 C7 H7A 108.4 . . ? C8 C7 H7A 108.4 . . ? C1 C7 H7B 108.4 . . ? C8 C7 H7B 108.4 . . ? H7A C7 H7B 107.4 . . ? C9 C8 C10 108.9(8) . . ? C9 C8 C7 109.9(9) . . ? C10 C8 C7 108.5(8) . . ? C9 C8 H8 109.8 . . ? C10 C8 H8 109.8 . . ? C7 C8 H8 109.8 . . ? C8 C9 C3 107.2(10) . . ? C8 C9 H9A 110.3 . . ? C3 C9 H9A 110.3 . . ? C8 C9 H9B 110.3 . . ? C3 C9 H9B 110.3 . . ? H9A C9 H9B 108.5 . . ? C5 C10 C8 108.5(9) . . ? C5 C10 H10A 110.0 . . ? C8 C10 H10A 110.0 . . ? C5 C10 H10B 110.0 . . ? C8 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? C16 C11 C12 112.3(9) . . ? C16 C11 B1 123.7(10) . . ? C12 C11 B1 124.0(10) . . ? C13 C12 C11 127.0(11) . . ? C13 C12 H12 116.5 . . ? C11 C12 H12 116.5 . . ? C12 C13 C14 120.0(12) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 116.6(12) . . ? C15 C14 H14 121.7 . . ? C13 C14 H14 121.7 . . ? C14 C15 C16 122.3(11) . . ? C14 C15 H15 118.8 . . ? C16 C15 H15 118.8 . . ? C11 C16 C15 121.6(10) . . ? C11 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? B1 C17 P1 117.3(7) . . ? B1 C17 H17A 108.0 . . ? P1 C17 H17A 108.0 . . ? B1 C17 H17B 108.0 . . ? P1 C17 H17B 108.0 . . ? H17A C17 H17B 107.2 . . ? C20 C18 C19 105.3(9) . . ? C20 C18 C21 111.5(10) . . ? C19 C18 C21 104.1(9) . . ? C20 C18 P1 115.5(8) . . ? C19 C18 P1 108.5(8) . . ? C21 C18 P1 111.1(8) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C25 C22 C23 106.8(9) . . ? C25 C22 C24 107.7(10) . . ? C23 C22 C24 112.4(8) . . ? C25 C22 P1 112.7(8) . . ? C23 C22 P1 108.4(7) . . ? C24 C22 P1 108.9(7) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? B1 C26 P2 117.3(7) . . ? B1 C26 H26A 108.0 . . ? P2 C26 H26A 108.0 . . ? B1 C26 H26B 108.0 . . ? P2 C26 H26B 108.0 . . ? H26A C26 H26B 107.2 . . ? C28 C27 C29 115.8(10) . . ? C28 C27 C30 106.9(9) . . ? C29 C27 C30 101.0(11) . . ? C28 C27 P2 112.5(9) . . ? C29 C27 P2 110.6(8) . . ? C30 C27 P2 109.2(8) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C33 107.1(9) . . ? C32 C31 C34 107.2(9) . . ? C33 C31 C34 109.1(9) . . ? C32 C31 P2 108.9(7) . . ? C33 C31 P2 114.5(7) . . ? C34 C31 P2 109.8(6) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N1 C35 C36 110.8(9) . . ? N1 C35 H35 124.6 . . ? C36 C35 H35 124.6 . . ? C35 C36 C37 104.0(9) . . ? C35 C36 H36 128.0 . . ? C37 C36 H36 128.0 . . ? N2 C37 C36 109.1(9) . . ? N2 C37 H37 125.4 . . ? C36 C37 H37 125.4 . . ? N4 B2 C63 102.0(8) . . ? N4 B2 C54 113.5(8) . . ? C63 B2 C54 114.1(8) . . ? N4 B2 C48 105.3(7) . . ? C63 B2 C48 110.8(9) . . ? C54 B2 C48 110.5(9) . . ? N6 Fe2 N5 132.9(3) . . ? N6 Fe2 P3 119.4(3) . . ? N5 Fe2 P3 84.6(2) . . ? N6 Fe2 P4 122.1(3) . . ? N5 Fe2 P4 87.1(2) . . ? P3 Fe2 P4 101.07(14) . . ? C72 N4 N5 107.8(7) . . ? C72 N4 B2 131.1(8) . . ? N5 N4 B2 121.0(7) . . ? C74 N5 N4 109.2(7) . . ? C74 N5 Fe2 123.9(6) . . ? N4 N5 Fe2 126.9(6) . . ? C38 N6 Fe2 170.2(11) . . ? C54 P3 C59 108.5(5) . . ? C54 P3 C55 107.1(4) . . ? C59 P3 C55 104.8(5) . . ? C54 P3 Fe2 106.6(3) . . ? C59 P3 Fe2 113.8(4) . . ? C55 P3 Fe2 115.8(3) . . ? C63 P4 C64 106.7(5) . . ? C63 P4 C68 105.5(4) . . ? C64 P4 C68 106.1(5) . . ? C63 P4 Fe2 108.3(3) . . ? C64 P4 Fe2 106.7(3) . . ? C68 P4 Fe2 122.6(4) . . ? C39 C38 C43 118(2) . . ? C39 C38 N6 110.4(17) . . ? C43 C38 N6 106.0(17) . . ? C39 C38 C44 110.5(19) . . ? C43 C38 C44 109.9(17) . . ? N6 C38 C44 100.4(15) . . ? C38 C39 C40 108.3(14) . . ? C38 C39 H39A 110.0 . . ? C40 C39 H39A 110.0 . . ? C38 C39 H39B 110.0 . . ? C40 C39 H39B 110.0 . . ? H39A C39 H39B 108.4 . . ? C41 C40 C39 108.5(11) . . ? C41 C40 C46 109.1(10) . . ? C39 C40 C46 109.0(9) . . ? C41 C40 H40 110.1 . . ? C39 C40 H40 110.1 . . ? C46 C40 H40 110.1 . . ? C40 C41 C42 114.3(13) . . ? C40 C41 H41A 108.7 . . ? C42 C41 H41A 108.7 . . ? C40 C41 H41B 108.7 . . ? C42 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? C43 C42 C47 109.2(15) . . ? C43 C42 C41 102.6(15) . . ? C47 C42 C41 100.4(12) . . ? C43 C42 H42 114.4 . . ? C47 C42 H42 114.4 . . ? C41 C42 H42 114.4 . . ? C38 C43 C42 111.2(15) . . ? C38 C43 H43A 109.4 . . ? C42 C43 H43A 109.4 . . ? C38 C43 H43B 109.4 . . ? C42 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? C45 C44 C38 102.1(11) . . ? C45 C44 H44A 111.3 . . ? C38 C44 H44A 111.3 . . ? C45 C44 H44B 111.3 . . ? C38 C44 H44B 111.3 . . ? H44A C44 H44B 109.2 . . ? C46 C45 C44 113.2(9) . . ? C46 C45 C47 111.6(9) . . ? C44 C45 C47 109.5(8) . . ? C46 C45 H45 107.5 . . ? C44 C45 H45 107.5 . . ? C47 C45 H45 107.5 . . ? C45 C46 C40 109.5(9) . . ? C45 C46 H46A 109.8 . . ? C40 C46 H46A 109.8 . . ? C45 C46 H46B 109.8 . . ? C40 C46 H46B 109.8 . . ? H46A C46 H46B 108.2 . . ? C45 C47 C42 111.1(12) . . ? C45 C47 H47A 109.4 . . ? C42 C47 H47A 109.4 . . ? C45 C47 H47B 109.4 . . ? C42 C47 H47B 109.4 . . ? H47A C47 H47B 108.0 . . ? C49 C48 C53 114.6(9) . . ? C49 C48 B2 121.8(10) . . ? C53 C48 B2 123.5(9) . . ? C50 C49 C48 123.4(10) . . ? C50 C49 H49 118.3 . . ? C48 C49 H49 118.3 . . ? C51 C50 C49 119.2(11) . . ? C51 C50 H50 120.4 . . ? C49 C50 H50 120.4 . . ? C52 C51 C50 118.7(10) . . ? C52 C51 H51 120.6 . . ? C50 C51 H51 120.6 . . ? C53 C52 C51 121.6(11) . . ? C53 C52 H52 119.2 . . ? C51 C52 H52 119.2 . . ? C52 C53 C48 122.4(10) . . ? C52 C53 H53 118.8 . . ? C48 C53 H53 118.8 . . ? B2 C54 P3 115.2(7) . . ? B2 C54 H54A 108.5 . . ? P3 C54 H54A 108.5 . . ? B2 C54 H54B 108.5 . . ? P3 C54 H54B 108.5 . . ? H54A C54 H54B 107.5 . . ? C56 C55 C57 107.2(9) . . ? C56 C55 C58 107.5(9) . . ? C57 C55 C58 106.5(9) . . ? C56 C55 P3 110.1(7) . . ? C57 C55 P3 112.8(7) . . ? C58 C55 P3 112.5(6) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C61 C59 C62 114.7(11) . . ? C61 C59 C60 106.1(9) . . ? C62 C59 C60 104.8(11) . . ? C61 C59 P3 111.0(9) . . ? C62 C59 P3 110.4(8) . . ? C60 C59 P3 109.5(8) . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C59 C62 H62A 109.5 . . ? C59 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C59 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? B2 C63 P4 116.2(7) . . ? B2 C63 H63A 108.2 . . ? P4 C63 H63A 108.2 . . ? B2 C63 H63B 108.2 . . ? P4 C63 H63B 108.2 . . ? H63A C63 H63B 107.4 . . ? C66 C64 C67 108.6(9) . . ? C66 C64 C65 105.1(9) . . ? C67 C64 C65 104.0(8) . . ? C66 C64 P4 112.6(8) . . ? C67 C64 P4 116.6(8) . . ? C65 C64 P4 109.1(8) . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C64 C66 H66A 109.5 . . ? C64 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C64 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C64 C67 H67A 109.5 . . ? C64 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C64 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C69 C68 C71 111.0(8) . . ? C69 C68 C70 101.2(9) . . ? C71 C68 C70 110.5(10) . . ? C69 C68 P4 108.1(6) . . ? C71 C68 P4 108.6(7) . . ? C70 C68 P4 117.1(9) . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C68 C71 H71A 109.5 . . ? C68 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C68 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N4 C72 C73 110.1(9) . . ? N4 C72 H72 125.0 . . ? C73 C72 H72 125.0 . . ? C72 C73 C74 105.8(9) . . ? C72 C73 H73 127.1 . . ? C74 C73 H73 127.1 . . ? N5 C74 C73 107.2(9) . . ? N5 C74 H74 126.4 . . ? C73 C74 H74 126.4 . . ? _diffrn_measured_fraction_theta_max 0.318 _diffrn_reflns_theta_full 27.68 _diffrn_measured_fraction_theta_full 0.318 _refine_diff_density_max 0.814 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.089 #===END data_cmt64 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H65 B Fe N3 P2' _chemical_formula_weight 704.54 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' 'P' 'P' 0.1023 0.0942 '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 10.886(4) _cell_length_b 17.390(5) _cell_length_c 21.104(6) _cell_angle_alpha 83.777(11) _cell_angle_beta 75.874(7) _cell_angle_gamma 85.190(8) _cell_volume 3845(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1936 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 21.52 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.074 _exptl_crystal_size_min 0.028 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1524 _exptl_absorpt_coefficient_mu 0.506 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22556 _diffrn_reflns_av_R_equivalents 0.1215 _diffrn_reflns_av_sigmaI/netI 0.2118 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 23.96 _reflns_number_total 10268 _reflns_number_gt 4935 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10268 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1739 _refine_ls_R_factor_gt 0.0885 _refine_ls_wR_factor_ref 0.1655 _refine_ls_wR_factor_gt 0.1504 _refine_ls_goodness_of_fit_ref 1.252 _refine_ls_restrained_S_all 1.252 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.5912(10) 0.6736(6) 0.3630(5) 0.012(3) Uiso 1 1 d . . . Fe1 Fe 0.68252(12) 0.78643(7) 0.46353(6) 0.0115(4) Uiso 1 1 d . . . N1 N 0.6080(6) 0.8140(4) 0.3874(3) 0.0089(18) Uiso 1 1 d . . . N2 N 0.5670(7) 0.7660(4) 0.3487(3) 0.0143(19) Uiso 1 1 d . . . N3 N 0.7322(7) 0.8363(4) 0.5135(3) 0.015(2) Uiso 1 1 d . . . P1 P 0.8280(2) 0.70382(14) 0.39793(12) 0.0124(6) Uiso 1 1 d . . . P2 P 0.5159(2) 0.70988(14) 0.50391(12) 0.0115(6) Uiso 1 1 d . . . C1 C 0.7752(8) 0.8705(5) 0.5634(4) 0.014(2) Uiso 1 1 d . . . C2 C 0.6638(8) 0.8810(5) 0.6233(4) 0.015(2) Uiso 1 1 d . . . H2A H 0.6338 0.8297 0.6432 0.018 Uiso 1 1 calc R . . H2B H 0.5926 0.9116 0.6093 0.018 Uiso 1 1 calc R . . C3 C 0.8226(8) 0.9504(5) 0.5350(4) 0.013(2) Uiso 1 1 d . . . H3A H 0.8938 0.9445 0.4961 0.016 Uiso 1 1 calc R . . H3B H 0.7534 0.9828 0.5206 0.016 Uiso 1 1 calc R . . C4 C 0.8832(8) 0.8218(5) 0.5861(4) 0.014(2) Uiso 1 1 d . . . H4A H 0.9556 0.8144 0.5479 0.017 Uiso 1 1 calc R . . H4B H 0.8539 0.7701 0.6053 0.017 Uiso 1 1 calc R . . C5 C 0.8663(8) 0.9902(5) 0.5846(4) 0.017(2) Uiso 1 1 d . . . H5 H 0.8972 1.0418 0.5642 0.020 Uiso 1 1 calc R . . C6 C 0.7064(8) 0.9230(5) 0.6744(4) 0.019(3) Uiso 1 1 d . . . H6 H 0.6332 0.9299 0.7130 0.023 Uiso 1 1 calc R . . C7 C 0.9270(8) 0.8633(5) 0.6383(4) 0.018(2) Uiso 1 1 d . . . H7 H 0.9971 0.8313 0.6533 0.022 Uiso 1 1 calc R . . C8 C 0.9734(8) 0.9421(5) 0.6069(4) 0.017(2) Uiso 1 1 d . . . H8A H 1.0024 0.9692 0.6390 0.020 Uiso 1 1 calc R . . H8B H 1.0460 0.9349 0.5689 0.020 Uiso 1 1 calc R . . C9 C 0.8131(8) 0.8739(5) 0.6968(4) 0.021(3) Uiso 1 1 d . . . H9A H 0.7826 0.8225 0.7165 0.025 Uiso 1 1 calc R . . H9B H 0.8393 0.8994 0.7307 0.025 Uiso 1 1 calc R . . C10 C 0.7521(8) 1.0024(5) 0.6436(4) 0.020(3) Uiso 1 1 d . . . H10A H 0.7780 1.0301 0.6764 0.024 Uiso 1 1 calc R . . H10B H 0.6826 1.0339 0.6287 0.024 Uiso 1 1 calc R . . C11 C 0.6166(9) 0.9567(5) 0.3935(5) 0.022(3) Uiso 1 1 d . . . H11A H 0.6257 1.0022 0.3613 0.033 Uiso 1 1 calc R . . H11B H 0.6956 0.9450 0.4079 0.033 Uiso 1 1 calc R . . H11C H 0.5469 0.9672 0.4313 0.033 Uiso 1 1 calc R . . C12 C 0.5878(8) 0.8873(5) 0.3620(4) 0.009(2) Uiso 1 1 d . . . C13 C 0.5387(8) 0.8867(5) 0.3096(4) 0.015(2) Uiso 1 1 d . . . H13 H 0.5180 0.9310 0.2828 0.018 Uiso 1 1 calc R . . C14 C 0.5229(8) 0.8086(5) 0.3010(4) 0.009(2) Uiso 1 1 d . . . C15 C 0.4684(8) 0.7826(5) 0.2505(4) 0.014(2) Uiso 1 1 d . . . H15A H 0.5257 0.7424 0.2278 0.021 Uiso 1 1 calc R . . H15B H 0.4572 0.8266 0.2188 0.021 Uiso 1 1 calc R . . H15C H 0.3860 0.7615 0.2711 0.021 Uiso 1 1 calc R . . C16 C 0.7455(8) 0.6595(5) 0.3470(4) 0.012(2) Uiso 1 1 d . . . H16A H 0.7800 0.6790 0.3007 0.014 Uiso 1 1 calc R . . H16B H 0.7664 0.6029 0.3508 0.014 Uiso 1 1 calc R . . C17 C 0.9166(8) 0.6194(5) 0.4362(4) 0.013(2) Uiso 1 1 d . . . C18 C 1.0385(8) 0.5893(5) 0.3901(4) 0.020(3) Uiso 1 1 d . . . H18A H 1.1007 0.6292 0.3800 0.030 Uiso 1 1 calc R . . H18B H 1.0194 0.5770 0.3494 0.030 Uiso 1 1 calc R . . H18C H 1.0734 0.5425 0.4114 0.030 Uiso 1 1 calc R . . C19 C 0.8273(9) 0.5509(5) 0.4556(5) 0.024(3) Uiso 1 1 d . . . H19A H 0.8410 0.5187 0.4189 0.036 Uiso 1 1 calc R . . H19B H 0.7388 0.5714 0.4662 0.036 Uiso 1 1 calc R . . H19C H 0.8459 0.5195 0.4940 0.036 Uiso 1 1 calc R . . C20 C 0.9514(8) 0.6453(5) 0.4973(4) 0.019(3) Uiso 1 1 d . . . H20A H 0.9854 0.6003 0.5212 0.029 Uiso 1 1 calc R . . H20B H 0.8754 0.6680 0.5259 0.029 Uiso 1 1 calc R . . H20C H 1.0155 0.6839 0.4833 0.029 Uiso 1 1 calc R . . C21 C 0.9523(8) 0.7651(5) 0.3381(4) 0.016(2) Uiso 1 1 d . . . C22 C 1.0435(8) 0.7930(5) 0.3752(4) 0.022(3) Uiso 1 1 d . . . H22A H 1.1034 0.8271 0.3452 0.033 Uiso 1 1 calc R . . H22B H 1.0902 0.7481 0.3923 0.033 Uiso 1 1 calc R . . H22C H 0.9947 0.8215 0.4117 0.033 Uiso 1 1 calc R . . C23 C 1.0289(8) 0.7231(5) 0.2787(4) 0.023(3) Uiso 1 1 d . . . H23A H 0.9706 0.6989 0.2592 0.035 Uiso 1 1 calc R . . H23B H 1.0876 0.6832 0.2933 0.035 Uiso 1 1 calc R . . H23C H 1.0772 0.7606 0.2460 0.035 Uiso 1 1 calc R . . C24 C 0.8843(8) 0.8356(5) 0.3113(4) 0.018(2) Uiso 1 1 d . . . H24A H 0.8392 0.8658 0.3475 0.027 Uiso 1 1 calc R . . H24B H 0.8232 0.8192 0.2889 0.027 Uiso 1 1 calc R . . H24C H 0.9461 0.8675 0.2802 0.027 Uiso 1 1 calc R . . C25 C 0.5187(8) 0.6450(5) 0.4408(4) 0.013(2) Uiso 1 1 d . . . H25A H 0.5601 0.5947 0.4532 0.016 Uiso 1 1 calc R . . H25B H 0.4298 0.6356 0.4418 0.016 Uiso 1 1 calc R . . C26 C 0.3535(8) 0.7655(5) 0.5144(4) 0.016(2) Uiso 1 1 d . . . C27 C 0.3475(8) 0.8349(5) 0.5531(4) 0.018(2) Uiso 1 1 d . . . H27A H 0.4197 0.8665 0.5329 0.027 Uiso 1 1 calc R . . H27B H 0.3506 0.8169 0.5984 0.027 Uiso 1 1 calc R . . H27C H 0.2682 0.8661 0.5531 0.027 Uiso 1 1 calc R . . C28 C 0.3233(8) 0.7960(5) 0.4493(4) 0.019(2) Uiso 1 1 d . . . H28A H 0.2343 0.8157 0.4570 0.028 Uiso 1 1 calc R . . H28B H 0.3377 0.7541 0.4204 0.028 Uiso 1 1 calc R . . H28C H 0.3783 0.8381 0.4287 0.028 Uiso 1 1 calc R . . C29 C 0.2424(8) 0.7111(5) 0.5477(4) 0.020(3) Uiso 1 1 d . . . H29A H 0.2501 0.6920 0.5920 0.030 Uiso 1 1 calc R . . H29B H 0.2474 0.6672 0.5216 0.030 Uiso 1 1 calc R . . H29C H 0.1607 0.7404 0.5501 0.030 Uiso 1 1 calc R . . C30 C 0.5069(8) 0.6483(5) 0.5864(4) 0.017(2) Uiso 1 1 d . . . C31 C 0.6458(8) 0.6303(5) 0.5966(4) 0.019(3) Uiso 1 1 d . . . H31A H 0.6424 0.5984 0.6381 0.028 Uiso 1 1 calc R . . H31B H 0.6842 0.6790 0.5976 0.028 Uiso 1 1 calc R . . H31C H 0.6970 0.6023 0.5603 0.028 Uiso 1 1 calc R . . C32 C 0.4412(8) 0.6901(5) 0.6465(4) 0.021(3) Uiso 1 1 d . . . H32A H 0.3505 0.6988 0.6478 0.032 Uiso 1 1 calc R . . H32B H 0.4784 0.7400 0.6440 0.032 Uiso 1 1 calc R . . H32C H 0.4523 0.6584 0.6862 0.032 Uiso 1 1 calc R . . C33 C 0.4514(9) 0.5706(5) 0.5882(5) 0.023(3) Uiso 1 1 d . . . H33A H 0.4524 0.5405 0.6301 0.034 Uiso 1 1 calc R . . H33B H 0.5022 0.5421 0.5521 0.034 Uiso 1 1 calc R . . H33C H 0.3639 0.5790 0.5834 0.034 Uiso 1 1 calc R . . C34 C 0.5348(8) 0.6253(5) 0.3151(4) 0.008(2) Uiso 1 1 d . . . C35 C 0.6096(9) 0.5855(5) 0.2642(4) 0.017(2) Uiso 1 1 d . . . H35 H 0.6987 0.5903 0.2550 0.021 Uiso 1 1 calc R . . C36 C 0.5673(9) 0.5409(5) 0.2267(4) 0.016(2) Uiso 1 1 d . . . H36 H 0.6256 0.5180 0.1916 0.019 Uiso 1 1 calc R . . C37 C 0.4418(8) 0.5284(5) 0.2388(4) 0.019(3) Uiso 1 1 d . . . H37 H 0.4110 0.4965 0.2130 0.022 Uiso 1 1 calc R . . C38 C 0.3594(9) 0.5641(5) 0.2906(5) 0.023(3) Uiso 1 1 d . . . H38 H 0.2711 0.5566 0.3001 0.028 Uiso 1 1 calc R . . C39 C 0.4044(8) 0.6095(5) 0.3275(4) 0.014(2) Uiso 1 1 d . . . H39 H 0.3462 0.6316 0.3631 0.017 Uiso 1 1 calc R . . B2 B 0.8041(10) 0.1715(6) -0.0354(5) 0.014(3) Uiso 1 1 d . . . Fe2 Fe 0.89081(12) 0.28232(8) 0.06937(6) 0.0126(4) Uiso 1 1 d . . . N4 N 0.7983(6) 0.3112(4) -0.0008(3) 0.0109(19) Uiso 1 1 d . . . N5 N 0.7627(7) 0.2644(4) -0.0411(3) 0.0125(19) Uiso 1 1 d . . . N6 N 0.9411(7) 0.3302(4) 0.1207(3) 0.017(2) Uiso 1 1 d . . . P3 P 1.0440(2) 0.21662(14) -0.00820(12) 0.0128(6) Uiso 1 1 d . . . P4 P 0.7441(2) 0.19096(15) 0.10817(12) 0.0140(7) Uiso 1 1 d . . . C40 C 0.9902(8) 0.3621(5) 0.1693(4) 0.009(2) Uiso 1 1 d . . . C41 C 0.9065(8) 0.4361(5) 0.1909(4) 0.018(2) Uiso 1 1 d . . . H41A H 0.9065 0.4738 0.1522 0.022 Uiso 1 1 calc R . . H41B H 0.8180 0.4224 0.2107 0.022 Uiso 1 1 calc R . . C42 C 1.1274(8) 0.3846(5) 0.1381(4) 0.014(2) Uiso 1 1 d . . . H42A H 1.1821 0.3380 0.1245 0.017 Uiso 1 1 calc R . . H42B H 1.1293 0.4217 0.0989 0.017 Uiso 1 1 calc R . . C43 C 0.9901(9) 0.3039(5) 0.2303(4) 0.027(3) Uiso 1 1 d . . . H43A H 1.0460 0.2574 0.2176 0.032 Uiso 1 1 calc R . . H43B H 0.9031 0.2873 0.2501 0.032 Uiso 1 1 calc R . . C44 C 0.9580(9) 0.4718(6) 0.2401(5) 0.024(3) Uiso 1 1 d . . . H44 H 0.9043 0.5196 0.2533 0.028 Uiso 1 1 calc R . . C45 C 1.1759(9) 0.4219(5) 0.1892(5) 0.022(3) Uiso 1 1 d . . . H45 H 1.2649 0.4365 0.1692 0.027 Uiso 1 1 calc R . . C46 C 1.0395(9) 0.3455(6) 0.2808(5) 0.025(3) Uiso 1 1 d . . . H46 H 1.0385 0.3089 0.3209 0.030 Uiso 1 1 calc R . . C47 C 0.9579(9) 0.4167(5) 0.3002(5) 0.025(3) Uiso 1 1 d . . . H47A H 0.9910 0.4418 0.3321 0.030 Uiso 1 1 calc R . . H47B H 0.8702 0.4025 0.3214 0.030 Uiso 1 1 calc R . . C48 C 1.1759(9) 0.3661(6) 0.2496(5) 0.028(3) Uiso 1 1 d . . . H48A H 1.2108 0.3904 0.2812 0.033 Uiso 1 1 calc R . . H48B H 1.2294 0.3186 0.2372 0.033 Uiso 1 1 calc R . . C49 C 1.0950(8) 0.4943(5) 0.2077(5) 0.023(3) Uiso 1 1 d . . . H49A H 1.0957 0.5306 0.1681 0.028 Uiso 1 1 calc R . . H49B H 1.1290 0.5204 0.2386 0.028 Uiso 1 1 calc R . . C50 C 0.7720(9) 0.4514(5) 0.0210(4) 0.023(3) Uiso 1 1 d . . . H50A H 0.7392 0.4388 0.0682 0.035 Uiso 1 1 calc R . . H50B H 0.7250 0.4977 0.0063 0.035 Uiso 1 1 calc R . . H50C H 0.8622 0.4613 0.0121 0.035 Uiso 1 1 calc R . . C51 C 0.7560(8) 0.3840(5) -0.0156(4) 0.009(2) Uiso 1 1 d . . . C52 C 0.7000(8) 0.3849(5) -0.0677(4) 0.013(2) Uiso 1 1 d . . . H52 H 0.6662 0.4294 -0.0896 0.016 Uiso 1 1 calc R . . C53 C 0.7022(8) 0.3075(5) -0.0825(4) 0.009(2) Uiso 1 1 d . . . C54 C 0.6455(8) 0.2826(5) -0.1340(4) 0.019(3) Uiso 1 1 d . . . H54A H 0.7058 0.2466 -0.1604 0.028 Uiso 1 1 calc R . . H54B H 0.6262 0.3281 -0.1625 0.028 Uiso 1 1 calc R . . H54C H 0.5672 0.2568 -0.1132 0.028 Uiso 1 1 calc R . . C55 C 0.7511(8) 0.1305(5) 0.0409(4) 0.014(2) Uiso 1 1 d . . . H55A H 0.8063 0.0835 0.0471 0.017 Uiso 1 1 calc R . . H55B H 0.6648 0.1136 0.0448 0.017 Uiso 1 1 calc R . . C56 C 0.5714(8) 0.2341(5) 0.1281(4) 0.015(2) Uiso 1 1 d . . . C57 C 0.5249(8) 0.2664(5) 0.0663(4) 0.021(3) Uiso 1 1 d . . . H57A H 0.4337 0.2806 0.0788 0.032 Uiso 1 1 calc R . . H57B H 0.5406 0.2268 0.0351 0.032 Uiso 1 1 calc R . . H57C H 0.5707 0.3123 0.0459 0.032 Uiso 1 1 calc R . . C58 C 0.5611(9) 0.3022(5) 0.1688(5) 0.025(3) Uiso 1 1 d . . . H58A H 0.4751 0.3267 0.1756 0.038 Uiso 1 1 calc R . . H58B H 0.6225 0.3399 0.1457 0.038 Uiso 1 1 calc R . . H58C H 0.5791 0.2838 0.2114 0.038 Uiso 1 1 calc R . . C59 C 0.4774(9) 0.1726(6) 0.1625(5) 0.033(3) Uiso 1 1 d . . . H59A H 0.5016 0.1487 0.2023 0.049 Uiso 1 1 calc R . . H59B H 0.4791 0.1327 0.1328 0.049 Uiso 1 1 calc R . . H59C H 0.3916 0.1972 0.1743 0.049 Uiso 1 1 calc R . . C60 C 0.7587(8) 0.1219(5) 0.1844(4) 0.012(2) Uiso 1 1 d . . . C61 C 0.9021(8) 0.1080(5) 0.1863(4) 0.021(3) Uiso 1 1 d . . . H61A H 0.9090 0.0764 0.2268 0.031 Uiso 1 1 calc R . . H61B H 0.9386 0.1579 0.1848 0.031 Uiso 1 1 calc R . . H61C H 0.9482 0.0809 0.1483 0.031 Uiso 1 1 calc R . . C62 C 0.6980(9) 0.1601(5) 0.2480(4) 0.025(3) Uiso 1 1 d . . . H62A H 0.6088 0.1754 0.2492 0.037 Uiso 1 1 calc R . . H62B H 0.7433 0.2061 0.2493 0.037 Uiso 1 1 calc R . . H62C H 0.7033 0.1232 0.2859 0.037 Uiso 1 1 calc R . . C63 C 0.7099(9) 0.0433(5) 0.1853(5) 0.031(3) Uiso 1 1 d . . . H63A H 0.7094 0.0139 0.2277 0.047 Uiso 1 1 calc R . . H63B H 0.7652 0.0153 0.1501 0.047 Uiso 1 1 calc R . . H63C H 0.6235 0.0493 0.1786 0.047 Uiso 1 1 calc R . . C64 C 0.9597(8) 0.1700(5) -0.0588(4) 0.014(2) Uiso 1 1 d . . . H64A H 0.9828 0.1953 -0.1041 0.016 Uiso 1 1 calc R . . H64B H 0.9923 0.1152 -0.0606 0.016 Uiso 1 1 calc R . . C65 C 1.1462(8) 0.2894(5) -0.0704(4) 0.014(2) Uiso 1 1 d . . . C66 C 1.0542(9) 0.3561(5) -0.0888(5) 0.026(3) Uiso 1 1 d . . . H66A H 1.1020 0.3936 -0.1216 0.040 Uiso 1 1 calc R . . H66B H 1.0117 0.3818 -0.0495 0.040 Uiso 1 1 calc R . . H66C H 0.9906 0.3350 -0.1068 0.040 Uiso 1 1 calc R . . C67 C 1.2169(8) 0.2574(5) -0.1344(4) 0.022(3) Uiso 1 1 d . . . H67A H 1.2848 0.2912 -0.1570 0.033 Uiso 1 1 calc R . . H67B H 1.1578 0.2550 -0.1624 0.033 Uiso 1 1 calc R . . H67C H 1.2537 0.2052 -0.1251 0.033 Uiso 1 1 calc R . . C68 C 1.2371(8) 0.3237(5) -0.0380(5) 0.025(3) Uiso 1 1 d . . . H68A H 1.3040 0.2844 -0.0316 0.037 Uiso 1 1 calc R . . H68B H 1.1905 0.3405 0.0045 0.037 Uiso 1 1 calc R . . H68C H 1.2754 0.3682 -0.0662 0.037 Uiso 1 1 calc R . . C69 C 1.1586(9) 0.1416(5) 0.0197(4) 0.020(3) Uiso 1 1 d . . . C70 C 1.0908(8) 0.0628(5) 0.0372(4) 0.022(3) Uiso 1 1 d . . . H70A H 1.1337 0.0279 0.0658 0.034 Uiso 1 1 calc R . . H70B H 1.0948 0.0387 -0.0032 0.034 Uiso 1 1 calc R . . H70C H 1.0019 0.0728 0.0599 0.034 Uiso 1 1 calc R . . C71 C 1.1962(9) 0.1641(5) 0.0786(4) 0.023(3) Uiso 1 1 d . . . H71A H 1.2464 0.1210 0.0958 0.034 Uiso 1 1 calc R . . H71B H 1.1199 0.1763 0.1125 0.034 Uiso 1 1 calc R . . H71C H 1.2470 0.2097 0.0660 0.034 Uiso 1 1 calc R . . C72 C 1.2835(8) 0.1194(5) -0.0310(4) 0.025(3) Uiso 1 1 d . . . H72A H 1.3371 0.1638 -0.0423 0.037 Uiso 1 1 calc R . . H72B H 1.2627 0.1051 -0.0707 0.037 Uiso 1 1 calc R . . H72C H 1.3290 0.0754 -0.0119 0.037 Uiso 1 1 calc R . . C73 C 0.7525(8) 0.1248(5) -0.0851(4) 0.009(2) Uiso 1 1 d . . . C74 C 0.6344(9) 0.0945(5) -0.0709(5) 0.020(3) Uiso 1 1 d . . . H74 H 0.5766 0.1068 -0.0313 0.024 Uiso 1 1 calc R . . C75 C 0.5933(9) 0.0475(5) -0.1101(4) 0.018(2) Uiso 1 1 d . . . H75 H 0.5113 0.0277 -0.0966 0.021 Uiso 1 1 calc R . . C76 C 0.6739(9) 0.0301(5) -0.1688(5) 0.021(3) Uiso 1 1 d . . . H76 H 0.6477 -0.0017 -0.1964 0.026 Uiso 1 1 calc R . . C77 C 0.7927(9) 0.0592(5) -0.1871(5) 0.018(2) Uiso 1 1 d . . . H77 H 0.8483 0.0480 -0.2278 0.021 Uiso 1 1 calc R . . C78 C 0.8316(9) 0.1053(5) -0.1458(4) 0.018(2) Uiso 1 1 d . . . H78 H 0.9143 0.1242 -0.1592 0.022 Uiso 1 1 calc R . . _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 N2 1.614(12) . ? B1 C16 1.633(12) . ? B1 C34 1.637(14) . ? B1 C25 1.679(13) . ? Fe1 N3 1.646(7) . ? Fe1 N1 1.968(7) . ? Fe1 P2 2.279(3) . ? Fe1 P1 2.338(3) . ? N1 C12 1.351(10) . ? N1 N2 1.398(9) . ? N2 C14 1.345(10) . ? N3 C1 1.452(11) . ? P1 C16 1.823(9) . ? P1 C17 1.904(9) . ? P1 C21 1.918(9) . ? P2 C25 1.830(9) . ? P2 C26 1.918(9) . ? P2 C30 1.928(9) . ? C1 C3 1.531(11) . ? C1 C4 1.532(11) . ? C1 C2 1.538(12) . ? C2 C6 1.544(12) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C5 1.502(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C7 1.566(12) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C8 1.517(11) . ? C5 C10 1.550(11) . ? C5 H5 1.0000 . ? C6 C9 1.521(11) . ? C6 C10 1.529(12) . ? C6 H6 1.0000 . ? C7 C8 1.525(11) . ? C7 C9 1.536(12) . ? C7 H7 1.0000 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.527(12) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.342(11) . ? C13 C14 1.419(11) . ? C13 H13 0.9500 . ? C14 C15 1.466(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.531(11) . ? C17 C20 1.549(12) . ? C17 C19 1.557(12) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C24 1.506(11) . ? C21 C22 1.541(12) . ? C21 C23 1.545(12) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.517(12) . ? C26 C28 1.519(12) . ? C26 C29 1.576(11) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C33 1.519(12) . ? C30 C32 1.522(12) . ? C30 C31 1.579(11) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.392(11) . ? C34 C39 1.423(11) . ? C35 C36 1.345(12) . ? C35 H35 0.9500 . ? C36 C37 1.359(11) . ? C36 H36 0.9500 . ? C37 C38 1.400(12) . ? C37 H37 0.9500 . ? C38 C39 1.362(12) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? B2 C73 1.619(14) . ? B2 N5 1.641(12) . ? B2 C64 1.644(13) . ? B2 C55 1.674(13) . ? Fe2 N6 1.652(7) . ? Fe2 N4 1.985(7) . ? Fe2 P4 2.292(3) . ? Fe2 P3 2.349(3) . ? N4 C51 1.342(10) . ? N4 N5 1.379(9) . ? N5 C53 1.346(10) . ? N6 C40 1.443(11) . ? P3 C64 1.853(9) . ? P3 C69 1.877(9) . ? P3 C65 1.930(9) . ? P4 C55 1.839(9) . ? P4 C56 1.928(9) . ? P4 C60 1.931(9) . ? C40 C42 1.543(11) . ? C40 C43 1.549(11) . ? C40 C41 1.557(11) . ? C41 C44 1.502(12) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C45 1.531(12) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C46 1.568(13) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C47 1.506(12) . ? C44 C49 1.545(12) . ? C44 H44 1.0000 . ? C45 C49 1.506(12) . ? C45 C48 1.517(12) . ? C45 H45 1.0000 . ? C46 C47 1.496(12) . ? C46 C48 1.526(12) . ? C46 H46 1.0000 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.515(12) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.381(11) . ? C52 C53 1.411(11) . ? C52 H52 0.9500 . ? C53 C54 1.493(12) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C58 1.518(12) . ? C56 C59 1.540(12) . ? C56 C57 1.544(12) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 C63 1.504(12) . ? C60 C62 1.539(12) . ? C60 C61 1.569(11) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C67 1.520(11) . ? C65 C68 1.523(12) . ? C65 C66 1.548(11) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C71 1.498(12) . ? C69 C72 1.560(12) . ? C69 C70 1.577(12) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C74 1.382(11) . ? C73 C78 1.416(11) . ? C74 C75 1.393(12) . ? C74 H74 0.9500 . ? C75 C76 1.379(12) . ? C75 H75 0.9500 . ? C76 C77 1.380(11) . ? C76 H76 0.9500 . ? C77 C78 1.403(12) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? 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 N2 B1 C16 104.4(7) . . ? N2 B1 C34 111.9(7) . . ? C16 B1 C34 109.6(7) . . ? N2 B1 C25 110.0(7) . . ? C16 B1 C25 113.7(7) . . ? C34 B1 C25 107.4(7) . . ? N3 Fe1 N1 134.5(3) . . ? N3 Fe1 P2 119.6(3) . . ? N1 Fe1 P2 86.2(2) . . ? N3 Fe1 P1 119.0(3) . . ? N1 Fe1 P1 87.0(2) . . ? P2 Fe1 P1 101.80(10) . . ? C12 N1 N2 106.1(7) . . ? C12 N1 Fe1 124.3(6) . . ? N2 N1 Fe1 129.6(5) . . ? C14 N2 N1 110.4(7) . . ? C14 N2 B1 131.6(7) . . ? N1 N2 B1 117.7(7) . . ? C1 N3 Fe1 172.1(6) . . ? C16 P1 C17 104.7(4) . . ? C16 P1 C21 105.7(4) . . ? C17 P1 C21 107.5(4) . . ? C16 P1 Fe1 108.5(3) . . ? C17 P1 Fe1 120.9(3) . . ? C21 P1 Fe1 108.6(3) . . ? C25 P2 C26 104.2(4) . . ? C25 P2 C30 108.6(4) . . ? C26 P2 C30 104.5(4) . . ? C25 P2 Fe1 106.2(3) . . ? C26 P2 Fe1 113.6(3) . . ? C30 P2 Fe1 118.8(3) . . ? N3 C1 C3 108.3(7) . . ? N3 C1 C4 112.9(7) . . ? C3 C1 C4 108.4(7) . . ? N3 C1 C2 109.7(7) . . ? C3 C1 C2 108.6(7) . . ? C4 C1 C2 108.7(7) . . ? C1 C2 C6 110.0(7) . . ? C1 C2 H2A 109.7 . . ? C6 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? C6 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C5 C3 C1 111.4(7) . . ? C5 C3 H3A 109.3 . . ? C1 C3 H3A 109.3 . . ? C5 C3 H3B 109.3 . . ? C1 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C1 C4 C7 110.0(7) . . ? C1 C4 H4A 109.7 . . ? C7 C4 H4A 109.7 . . ? C1 C4 H4B 109.7 . . ? C7 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C3 C5 C8 110.4(7) . . ? C3 C5 C10 108.5(7) . . ? C8 C5 C10 110.5(7) . . ? C3 C5 H5 109.1 . . ? C8 C5 H5 109.1 . . ? C10 C5 H5 109.1 . . ? C9 C6 C10 110.3(8) . . ? C9 C6 C2 108.9(7) . . ? C10 C6 C2 109.6(7) . . ? C9 C6 H6 109.4 . . ? C10 C6 H6 109.4 . . ? C2 C6 H6 109.4 . . ? C8 C7 C9 110.2(7) . . ? C8 C7 C4 108.4(7) . . ? C9 C7 C4 108.5(7) . . ? C8 C7 H7 109.9 . . ? C9 C7 H7 109.9 . . ? C4 C7 H7 109.9 . . ? C5 C8 C7 109.5(7) . . ? C5 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? C5 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? C6 C9 C7 110.1(8) . . ? C6 C9 H9A 109.6 . . ? C7 C9 H9A 109.6 . . ? C6 C9 H9B 109.6 . . ? C7 C9 H9B 109.6 . . ? H9A C9 H9B 108.2 . . ? C6 C10 C5 108.5(7) . . ? C6 C10 H10A 110.0 . . ? C5 C10 H10A 110.0 . . ? C6 C10 H10B 110.0 . . ? C5 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 N1 109.9(8) . . ? C13 C12 C11 128.9(8) . . ? N1 C12 C11 121.2(8) . . ? C12 C13 C14 108.4(8) . . ? C12 C13 H13 125.8 . . ? C14 C13 H13 125.8 . . ? N2 C14 C13 105.2(8) . . ? N2 C14 C15 128.9(8) . . ? C13 C14 C15 125.9(8) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? B1 C16 P1 117.1(6) . . ? B1 C16 H16A 108.0 . . ? P1 C16 H16A 108.0 . . ? B1 C16 H16B 108.0 . . ? P1 C16 H16B 108.0 . . ? H16A C16 H16B 107.3 . . ? C18 C17 C20 108.3(7) . . ? C18 C17 C19 106.8(7) . . ? C20 C17 C19 111.1(7) . . ? C18 C17 P1 114.2(6) . . ? C20 C17 P1 108.7(6) . . ? C19 C17 P1 107.7(6) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C24 C21 C22 108.0(7) . . ? C24 C21 C23 107.1(7) . . ? C22 C21 C23 109.8(7) . . ? C24 C21 P1 108.1(6) . . ? C22 C21 P1 109.6(6) . . ? C23 C21 P1 114.0(6) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? B1 C25 P2 117.9(6) . . ? B1 C25 H25A 107.8 . . ? P2 C25 H25A 107.8 . . ? B1 C25 H25B 107.8 . . ? P2 C25 H25B 107.8 . . ? H25A C25 H25B 107.2 . . ? C27 C26 C28 107.0(7) . . ? C27 C26 C29 110.8(7) . . ? C28 C26 C29 103.7(7) . . ? C27 C26 P2 110.9(6) . . ? C28 C26 P2 112.8(6) . . ? C29 C26 P2 111.4(6) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C33 C30 C32 111.2(8) . . ? C33 C30 C31 106.7(7) . . ? C32 C30 C31 102.6(7) . . ? C33 C30 P2 112.4(6) . . ? C32 C30 P2 114.4(6) . . ? C31 C30 P2 108.8(6) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C39 112.2(8) . . ? C35 C34 B1 124.2(8) . . ? C39 C34 B1 123.0(8) . . ? C36 C35 C34 125.9(9) . . ? C36 C35 H35 117.0 . . ? C34 C35 H35 117.0 . . ? C35 C36 C37 120.4(9) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C36 C37 C38 117.7(9) . . ? C36 C37 H37 121.1 . . ? C38 C37 H37 121.1 . . ? C39 C38 C37 120.8(10) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C38 C39 C34 122.8(9) . . ? C38 C39 H39 118.6 . . ? C34 C39 H39 118.6 . . ? C73 B2 N5 112.6(7) . . ? C73 B2 C64 108.5(8) . . ? N5 B2 C64 102.8(7) . . ? C73 B2 C55 108.3(7) . . ? N5 B2 C55 111.4(7) . . ? C64 B2 C55 113.2(8) . . ? N6 Fe2 N4 135.1(3) . . ? N6 Fe2 P4 120.5(3) . . ? N4 Fe2 P4 85.7(2) . . ? N6 Fe2 P3 117.8(3) . . ? N4 Fe2 P3 87.2(2) . . ? P4 Fe2 P3 101.85(10) . . ? C51 N4 N5 107.6(7) . . ? C51 N4 Fe2 123.2(6) . . ? N5 N4 Fe2 129.1(5) . . ? C53 N5 N4 110.0(7) . . ? C53 N5 B2 131.0(7) . . ? N4 N5 B2 118.9(7) . . ? C40 N6 Fe2 172.4(6) . . ? C64 P3 C69 107.7(4) . . ? C64 P3 C65 103.7(4) . . ? C69 P3 C65 106.0(4) . . ? C64 P3 Fe2 107.8(3) . . ? C69 P3 Fe2 120.0(3) . . ? C65 P3 Fe2 110.5(3) . . ? C55 P4 C56 104.0(4) . . ? C55 P4 C60 107.3(4) . . ? C56 P4 C60 105.1(4) . . ? C55 P4 Fe2 107.1(3) . . ? C56 P4 Fe2 113.5(3) . . ? C60 P4 Fe2 118.8(3) . . ? N6 C40 C42 108.9(7) . . ? N6 C40 C43 112.3(7) . . ? C42 C40 C43 109.0(7) . . ? N6 C40 C41 108.5(7) . . ? C42 C40 C41 109.0(7) . . ? C43 C40 C41 109.2(7) . . ? C44 C41 C40 109.6(7) . . ? C44 C41 H41A 109.8 . . ? C40 C41 H41A 109.8 . . ? C44 C41 H41B 109.8 . . ? C40 C41 H41B 109.8 . . ? H41A C41 H41B 108.2 . . ? C45 C42 C40 108.3(7) . . ? C45 C42 H42A 110.0 . . ? C40 C42 H42A 110.0 . . ? C45 C42 H42B 110.0 . . ? C40 C42 H42B 110.0 . . ? H42A C42 H42B 108.4 . . ? C40 C43 C46 107.9(7) . . ? C40 C43 H43A 110.1 . . ? C46 C43 H43A 110.1 . . ? C40 C43 H43B 110.1 . . ? C46 C43 H43B 110.1 . . ? H43A C43 H43B 108.4 . . ? C41 C44 C47 111.4(8) . . ? C41 C44 C49 108.8(8) . . ? C47 C44 C49 109.5(8) . . ? C41 C44 H44 109.0 . . ? C47 C44 H44 109.0 . . ? C49 C44 H44 109.0 . . ? C49 C45 C48 110.4(8) . . ? C49 C45 C42 109.6(8) . . ? C48 C45 C42 111.3(8) . . ? C49 C45 H45 108.5 . . ? C48 C45 H45 108.5 . . ? C42 C45 H45 108.5 . . ? C47 C46 C48 110.5(8) . . ? C47 C46 C43 111.3(8) . . ? C48 C46 C43 108.3(8) . . ? C47 C46 H46 108.9 . . ? C48 C46 H46 108.9 . . ? C43 C46 H46 108.9 . . ? C46 C47 C44 109.3(8) . . ? C46 C47 H47A 109.8 . . ? C44 C47 H47A 109.8 . . ? C46 C47 H47B 109.8 . . ? C44 C47 H47B 109.8 . . ? H47A C47 H47B 108.3 . . ? C45 C48 C46 108.3(8) . . ? C45 C48 H48A 110.0 . . ? C46 C48 H48A 110.0 . . ? C45 C48 H48B 110.0 . . ? C46 C48 H48B 110.0 . . ? H48A C48 H48B 108.4 . . ? C45 C49 C44 108.7(8) . . ? C45 C49 H49A 109.9 . . ? C44 C49 H49A 109.9 . . ? C45 C49 H49B 109.9 . . ? C44 C49 H49B 109.9 . . ? H49A C49 H49B 108.3 . . ? C51 C50 H50A 109.5 . . ? C51 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C51 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N4 C51 C52 108.8(8) . . ? N4 C51 C50 122.9(8) . . ? C52 C51 C50 128.3(8) . . ? C51 C52 C53 107.2(8) . . ? C51 C52 H52 126.4 . . ? C53 C52 H52 126.4 . . ? N5 C53 C52 106.2(7) . . ? N5 C53 C54 129.4(8) . . ? C52 C53 C54 124.4(8) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? B2 C55 P4 116.7(6) . . ? B2 C55 H55A 108.1 . . ? P4 C55 H55A 108.1 . . ? B2 C55 H55B 108.1 . . ? P4 C55 H55B 108.1 . . ? H55A C55 H55B 107.3 . . ? C58 C56 C59 111.5(7) . . ? C58 C56 C57 105.8(7) . . ? C59 C56 C57 104.7(7) . . ? C58 C56 P4 109.6(6) . . ? C59 C56 P4 111.8(6) . . ? C57 C56 P4 113.2(6) . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C56 C59 H59A 109.5 . . ? C56 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C56 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C63 C60 C62 111.9(8) . . ? C63 C60 C61 106.5(7) . . ? C62 C60 C61 103.6(7) . . ? C63 C60 P4 113.9(6) . . ? C62 C60 P4 111.0(6) . . ? C61 C60 P4 109.5(6) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C60 C63 H63A 109.5 . . ? C60 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C60 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? B2 C64 P3 117.4(6) . . ? B2 C64 H64A 107.9 . . ? P3 C64 H64A 107.9 . . ? B2 C64 H64B 107.9 . . ? P3 C64 H64B 107.9 . . ? H64A C64 H64B 107.2 . . ? C67 C65 C68 111.0(7) . . ? C67 C65 C66 106.3(7) . . ? C68 C65 C66 107.7(8) . . ? C67 C65 P3 114.9(6) . . ? C68 C65 P3 109.8(6) . . ? C66 C65 P3 106.7(6) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C71 C69 C72 107.0(8) . . ? C71 C69 C70 109.9(7) . . ? C72 C69 C70 102.7(7) . . ? C71 C69 P3 111.2(6) . . ? C72 C69 P3 118.0(6) . . ? C70 C69 P3 107.5(6) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 C71 H71A 109.5 . . ? C69 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C69 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C69 C72 H72A 109.5 . . ? C69 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C69 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C74 C73 C78 113.7(8) . . ? C74 C73 B2 124.5(8) . . ? C78 C73 B2 121.5(8) . . ? C73 C74 C75 125.3(9) . . ? C73 C74 H74 117.3 . . ? C75 C74 H74 117.3 . . ? C76 C75 C74 118.8(9) . . ? C76 C75 H75 120.6 . . ? C74 C75 H75 120.6 . . ? C75 C76 C77 119.5(9) . . ? C75 C76 H76 120.3 . . ? C77 C76 H76 120.3 . . ? C76 C77 C78 120.1(9) . . ? C76 C77 H77 120.0 . . ? C78 C77 H77 120.0 . . ? C77 C78 C73 122.6(9) . . ? C77 C78 H78 118.7 . . ? C73 C78 H78 118.7 . . ? _diffrn_measured_fraction_theta_max 0.852 _diffrn_reflns_theta_full 23.96 _diffrn_measured_fraction_theta_full 0.852 _refine_diff_density_max 0.829 _refine_diff_density_min -0.801 _refine_diff_density_rms 0.115 #===END data_cmt55 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H121 B F24 Fe N3 O3 P2' _chemical_formula_weight 1769.41 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' 'O' 'O' 0.0106 0.0060 '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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.2246(19) _cell_length_b 27.556(4) _cell_length_c 12.862(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.822(4) _cell_angle_gamma 90.00 _cell_volume 4224.7(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1858 _exptl_absorpt_coefficient_mu 0.318 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16238 _diffrn_reflns_av_R_equivalents 0.1479 _diffrn_reflns_av_sigmaI/netI 0.3650 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 26.20 _reflns_number_total 9760 _reflns_number_gt 3723 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(5) _refine_ls_number_reflns 9760 _refine_ls_number_parameters 477 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.2941 _refine_ls_R_factor_gt 0.1237 _refine_ls_wR_factor_ref 0.1972 _refine_ls_wR_factor_gt 0.1716 _refine_ls_goodness_of_fit_ref 1.380 _refine_ls_restrained_S_all 1.382 _refine_ls_shift/su_max 0.007 _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 Fe Fe 0.0795(2) 0.93882(9) 0.0357(2) 0.0240(8) Uiso 1 1 d . B . N1 N -0.0060(12) 0.9947(5) 0.0542(11) 0.022(4) Uiso 1 1 d . . . N2 N -0.1198(12) 1.0038(5) 0.0095(11) 0.026(4) Uiso 1 1 d . B . N3 N 0.2016(11) 0.9143(5) 0.0707(10) 0.020(4) Uiso 1 1 d . . . P1 P -0.0623(4) 0.89281(18) 0.0903(4) 0.0204(13) Uiso 1 1 d . . . P2 P 0.0364(4) 0.95831(18) -0.1488(4) 0.0219(14) Uiso 1 1 d . . . B1 B -0.1813(17) 0.9664(8) -0.0792(16) 0.021(6) Uiso 1 1 d . . . C1 C 0.3049(14) 0.8880(6) 0.1065(12) 0.012(4) Uiso 1 1 d . . . C2 C 0.3270(14) 0.8816(7) 0.2350(13) 0.031(6) Uiso 1 1 d . . . H2A H 0.3271 0.9137 0.2697 0.037 Uiso 1 1 calc R . . H2B H 0.2671 0.8615 0.2538 0.037 Uiso 1 1 calc R . . C3 C 0.4045(13) 0.9154(6) 0.0829(13) 0.022(5) Uiso 1 1 d . . . H3A H 0.3905 0.9201 0.0047 0.027 Uiso 1 1 calc R . . H3B H 0.4053 0.9480 0.1153 0.027 Uiso 1 1 calc R . . C4 C 0.3004(15) 0.8388(6) 0.0525(14) 0.031(6) Uiso 1 1 d . . . H4A H 0.2852 0.8429 -0.0259 0.037 Uiso 1 1 calc R . . H4B H 0.2398 0.8188 0.0702 0.037 Uiso 1 1 calc R . . C5 C 0.4341(15) 0.8584(6) 0.2705(15) 0.024(5) Uiso 1 1 d . . . H5 H 0.4489 0.8543 0.3497 0.029 Uiso 1 1 calc R . . C6 C 0.4403(19) 0.8066(8) 0.2177(16) 0.060(7) Uiso 1 1 d . . . H6A H 0.5154 0.7920 0.2443 0.072 Uiso 1 1 calc R . . H6B H 0.3835 0.7846 0.2363 0.072 Uiso 1 1 calc R . . C7 C 0.4173(16) 0.8136(7) 0.0939(15) 0.035(6) Uiso 1 1 d . . . H7 H 0.4155 0.7810 0.0596 0.043 Uiso 1 1 calc R . . C8 C 0.5161(17) 0.8404(7) 0.0759(15) 0.042(6) Uiso 1 1 d . . . H8A H 0.5159 0.8403 -0.0011 0.050 Uiso 1 1 calc R . . H8B H 0.5855 0.8241 0.1144 0.050 Uiso 1 1 calc R . . C9 C 0.5141(15) 0.8953(7) 0.1171(13) 0.028(5) Uiso 1 1 d . . . H9 H 0.5742 0.9161 0.0987 0.034 Uiso 1 1 calc R . . C10 C 0.5308(16) 0.8859(7) 0.2432(14) 0.044(6) Uiso 1 1 d . . . H10A H 0.6009 0.8674 0.2689 0.053 Uiso 1 1 calc R . . H10B H 0.5388 0.9175 0.2807 0.053 Uiso 1 1 calc R . . C11 C 0.0347(18) 1.0348(7) 0.1247(16) 0.049(7) Uiso 1 1 d . . . H11 H 0.1077 1.0387 0.1685 0.059 Uiso 1 1 calc R . . C12 C -0.0604(15) 1.0679(7) 0.1143(14) 0.034(6) Uiso 1 1 d . B . H12 H -0.0596 1.0980 0.1505 0.040 Uiso 1 1 calc R . . C13 C -0.1532(16) 1.0483(7) 0.0423(14) 0.033(6) Uiso 1 1 d . . . H13 H -0.2252 1.0627 0.0202 0.039 Uiso 1 1 calc R B . C14 C 0.0924(14) 1.0202(6) -0.1734(13) 0.012(5) Uiso 1 1 d . A . C15 C 0.2059(15) 1.0251(7) -0.0918(14) 0.039(6) Uiso 1 1 d . . . H15A H 0.2418 0.9932 -0.0795 0.059 Uiso 1 1 calc R B . H15B H 0.1928 1.0378 -0.0244 0.059 Uiso 1 1 calc R . . H15C H 0.2548 1.0474 -0.1198 0.059 Uiso 1 1 calc R . . C16 C 0.1055(17) 1.0313(7) -0.2776(15) 0.051(7) Uiso 1 1 d . . . H16A H 0.0341 1.0262 -0.3288 0.077 Uiso 1 1 calc R B . H16B H 0.1629 1.0100 -0.2957 0.077 Uiso 1 1 calc R . . H16C H 0.1287 1.0652 -0.2804 0.077 Uiso 1 1 calc R . . C17 C 0.0152(17) 1.0594(7) -0.1434(16) 0.060(7) Uiso 1 1 d . A 1 H17A H 0.0411 1.0915 -0.1599 0.089 Uiso 1 1 calc R A 1 H17B H 0.0170 1.0574 -0.0669 0.089 Uiso 1 1 calc R A 1 H17C H -0.0618 1.0542 -0.1841 0.089 Uiso 1 1 calc R A 1 C18 C 0.0801(13) 0.9138(6) -0.2487(13) 0.016(5) Uiso 1 1 d . B 1 C19 C 0.2078(13) 0.9157(6) -0.2362(14) 0.033(6) Uiso 1 1 d . B 1 H19A H 0.2312 0.8902 -0.2795 0.050 Uiso 1 1 calc R B 1 H19B H 0.2447 0.9109 -0.1611 0.050 Uiso 1 1 calc R B 1 H19C H 0.2291 0.9475 -0.2599 0.050 Uiso 1 1 calc R B 1 C20 C 0.0475(16) 0.8606(6) -0.2190(14) 0.038(6) Uiso 1 1 d . B 1 H20A H -0.0342 0.8580 -0.2306 0.057 Uiso 1 1 calc R B 1 H20B H 0.0817 0.8540 -0.1440 0.057 Uiso 1 1 calc R B 1 H20C H 0.0750 0.8370 -0.2642 0.057 Uiso 1 1 calc R B 1 C21 C 0.0147(16) 0.9232(7) -0.3669(14) 0.054(7) Uiso 1 1 d . B 1 H21A H 0.0211 0.9575 -0.3845 0.081 Uiso 1 1 calc R B 1 H21B H -0.0646 0.9148 -0.3741 0.081 Uiso 1 1 calc R B 1 H21C H 0.0467 0.9031 -0.4155 0.081 Uiso 1 1 calc R B 1 C22 C -0.1147(13) 0.9583(6) -0.1716(12) 0.021(5) Uiso 1 1 d . B 1 H22A H -0.1417 0.9835 -0.2260 0.025 Uiso 1 1 calc R B 1 H22B H -0.1402 0.9268 -0.2053 0.025 Uiso 1 1 calc R B 1 C23 C -0.0599(14) 0.8224(6) 0.0772(13) 0.013(5) Uiso 1 1 d . C 1 C24 C -0.1780(14) 0.8050(6) 0.0813(14) 0.027(5) Uiso 1 1 d . C 1 H24A H -0.2338 0.8272 0.0402 0.041 Uiso 1 1 calc R C 1 H24B H -0.1856 0.8043 0.1555 0.041 Uiso 1 1 calc R C 1 H24C H -0.1900 0.7723 0.0508 0.041 Uiso 1 1 calc R C 1 C25 C -0.0333(15) 0.8139(7) -0.0241(13) 0.038(6) Uiso 1 1 d . C 1 H25A H -0.0368 0.7791 -0.0393 0.057 Uiso 1 1 calc R C 1 H25B H 0.0425 0.8259 -0.0227 0.057 Uiso 1 1 calc R C 1 H25C H -0.0874 0.8310 -0.0797 0.057 Uiso 1 1 calc R C 1 C26 C 0.0262(16) 0.8042(7) 0.1737(14) 0.047(6) Uiso 1 1 d . C 1 H26A H 0.0134 0.7696 0.1844 0.070 Uiso 1 1 calc R C 1 H26B H 0.0186 0.8224 0.2371 0.070 Uiso 1 1 calc R C 1 H26C H 0.1018 0.8088 0.1615 0.070 Uiso 1 1 calc R C 1 C27 C -0.0708(15) 0.9101(6) 0.2311(13) 0.023(5) Uiso 1 1 d . C 1 C28 C -0.1367(14) 0.9605(6) 0.2247(13) 0.035(6) Uiso 1 1 d . C 1 H28A H -0.1373 0.9717 0.2969 0.052 Uiso 1 1 calc R C 1 H28B H -0.2140 0.9560 0.1842 0.052 Uiso 1 1 calc R C 1 H28C H -0.0993 0.9847 0.1889 0.052 Uiso 1 1 calc R C 1 C29 C -0.1386(15) 0.8758(6) 0.2815(13) 0.032(6) Uiso 1 1 d . C 1 H29A H -0.1057 0.8432 0.2843 0.048 Uiso 1 1 calc R C 1 H29B H -0.2158 0.8748 0.2391 0.048 Uiso 1 1 calc R C 1 H29C H -0.1386 0.8867 0.3539 0.048 Uiso 1 1 calc R C 1 C30 C 0.0410(14) 0.9138(7) 0.2919(13) 0.038(6) Uiso 1 1 d . C 1 H30A H 0.0401 0.9226 0.3655 0.057 Uiso 1 1 calc R C 1 H30B H 0.0812 0.9387 0.2609 0.057 Uiso 1 1 calc R C 1 H30C H 0.0790 0.8825 0.2913 0.057 Uiso 1 1 calc R C 1 C31 C -0.1892(16) 0.9119(7) 0.0003(15) 0.044(6) Uiso 1 1 d . B 1 H31A H -0.2467 0.9174 0.0424 0.052 Uiso 1 1 calc R B 1 H31B H -0.2159 0.8847 -0.0493 0.052 Uiso 1 1 calc R B 1 C32 C -0.3053(16) 0.9828(7) -0.1236(14) 0.030(5) Uiso 1 1 d . B 1 C33 C -0.4097(13) 0.9590(6) -0.1256(11) 0.014(5) Uiso 1 1 d . B 1 H33 H -0.4016 0.9288 -0.0887 0.016 Uiso 1 1 calc R B 1 C34 C -0.5120(14) 0.9700(6) -0.1668(12) 0.017(5) Uiso 1 1 d . B 1 H34 H -0.5741 0.9504 -0.1603 0.021 Uiso 1 1 calc R B 1 C35 C -0.5232(17) 1.0192(7) -0.2291(14) 0.039(6) Uiso 1 1 d . B 1 H35 H -0.5943 1.0321 -0.2628 0.047 Uiso 1 1 calc R B 1 C36 C -0.4299(15) 1.0416(7) -0.2324(14) 0.029(5) Uiso 1 1 d . B 1 H36 H -0.4368 1.0706 -0.2733 0.035 Uiso 1 1 calc R B 1 C37 C -0.3232(15) 1.0279(7) -0.1835(13) 0.026(5) Uiso 1 1 d . B 1 H37 H -0.2611 1.0478 -0.1887 0.032 Uiso 1 1 calc R B 1 B2 B 0.5064(17) 0.1695(7) 0.5048(16) 0.016(6) Uiso 1 1 d . D 1 C38 C 0.3959(14) 0.1923(6) 0.4474(13) 0.018(5) Uiso 1 1 d . D 1 C39 C 0.3495(14) 0.2318(6) 0.4853(14) 0.022(5) Uiso 1 1 d . D 1 H39 H 0.3888 0.2459 0.5504 0.027 Uiso 1 1 calc R D 1 C40 C 0.2454(18) 0.2532(7) 0.4327(17) 0.043(6) Uiso 1 1 d . D 1 C41 C 0.1894(14) 0.2352(6) 0.3352(13) 0.014(5) Uiso 1 1 d . D 1 H41 H 0.1206 0.2497 0.2999 0.017 Uiso 1 1 calc R D 1 C42 C 0.2316(16) 0.1961(7) 0.2873(15) 0.031(6) Uiso 1 1 d . D 1 C43 C 0.3322(14) 0.1767(7) 0.3474(13) 0.025(5) Uiso 1 1 d . D 1 H43 H 0.3612 0.1495 0.3168 0.031 Uiso 1 1 calc R D 1 C44 C 0.197(2) 0.2962(9) 0.4869(18) 0.049(7) Uiso 1 1 d . D 1 C45 C 0.1738(15) 0.1809(7) 0.1844(15) 0.026(5) Uiso 1 1 d . D 1 C46 C 0.5995(14) 0.1965(6) 0.4563(14) 0.021(5) Uiso 1 1 d . D 1 C47 C 0.6498(16) 0.2378(7) 0.4969(16) 0.045(6) Uiso 1 1 d . D 1 H47 H 0.6284 0.2511 0.5576 0.054 Uiso 1 1 calc R D 1 C48 C 0.7315(14) 0.2631(6) 0.4570(14) 0.017(5) Uiso 1 1 d . D 1 C49 C 0.7623(17) 0.2468(7) 0.3589(15) 0.042(6) Uiso 1 1 d . D 1 H49 H 0.8163 0.2639 0.3303 0.050 Uiso 1 1 calc R D 1 C50 C 0.7121(16) 0.2071(7) 0.3108(15) 0.032(6) Uiso 1 1 d . D 1 C51 C 0.6329(14) 0.1845(7) 0.3601(14) 0.027(5) Uiso 1 1 d . D 1 H51 H 0.5962 0.1570 0.3234 0.032 Uiso 1 1 calc R D 1 C52 C 0.783(2) 0.3087(11) 0.507(2) 0.075(9) Uiso 1 1 d . D 1 C53 C 0.729(2) 0.1932(9) 0.2068(19) 0.056(7) Uiso 1 1 d . D 1 C54 C 0.5163(15) 0.1114(6) 0.4879(13) 0.026(5) Uiso 1 1 d . D 1 C55 C 0.6151(14) 0.0838(6) 0.4913(12) 0.015(5) Uiso 1 1 d . D 1 H55 H 0.6839 0.1010 0.4992 0.018 Uiso 1 1 calc R D 1 C56 C 0.6185(15) 0.0312(7) 0.4835(13) 0.021(5) Uiso 1 1 d . D 1 C57 C 0.5230(14) 0.0063(7) 0.4779(13) 0.023(5) Uiso 1 1 d . D 1 H57 H 0.5250 -0.0282 0.4748 0.027 Uiso 1 1 calc R D 1 C58 C 0.4189(17) 0.0295(7) 0.4765(15) 0.035(6) Uiso 1 1 d . D 1 C59 C 0.4139(15) 0.0784(6) 0.4796(13) 0.024(5) Uiso 1 1 d . D 1 H59 H 0.3430 0.0931 0.4765 0.028 Uiso 1 1 calc R D 1 C60 C 0.3058(16) 0.0032(7) 0.4619(16) 0.029(6) Uiso 1 1 d . D 1 C61 C 0.7251(17) 0.0127(8) 0.4936(16) 0.035(6) Uiso 1 1 d . D 1 C62 C 0.5328(12) 0.1736(6) 0.6334(12) 0.006(4) Uiso 1 1 d . D 1 C63 C 0.4420(15) 0.1739(7) 0.6844(14) 0.033(6) Uiso 1 1 d . D 1 H63 H 0.3670 0.1725 0.6438 0.040 Uiso 1 1 calc R D 1 C64 C 0.4649(13) 0.1764(6) 0.8012(13) 0.012(4) Uiso 1 1 d . D 1 C65 C 0.5674(14) 0.1780(6) 0.8610(14) 0.024(5) Uiso 1 1 d . D 1 H65 H 0.5786 0.1808 0.9363 0.028 Uiso 1 1 calc R D 1 C66 C 0.6611(15) 0.1757(7) 0.8127(14) 0.025(5) Uiso 1 1 d . D 1 C67 C 0.6360(14) 0.1721(6) 0.6976(13) 0.018(5) Uiso 1 1 d . D 1 H67 H 0.6977 0.1685 0.6645 0.022 Uiso 1 1 calc R D 1 C68 C 0.7710(19) 0.1719(9) 0.8699(18) 0.051(7) Uiso 1 1 d . D 1 C69 C 0.3729(15) 0.1780(7) 0.8504(14) 0.022(5) Uiso 1 1 d . D 1 F1 F 0.0616(9) 0.1905(4) 0.1567(8) 0.049(3) Uiso 1 1 d . D 1 F2 F 0.1820(9) 0.1330(4) 0.1749(8) 0.049(3) Uiso 1 1 d . D 1 F3 F 0.2149(8) 0.1971(4) 0.1067(8) 0.040(3) Uiso 1 1 d . D 1 F4 F 0.1210(13) 0.3209(5) 0.4297(11) 0.089(5) Uiso 1 1 d . D 1 F5 F 0.1648(13) 0.2801(6) 0.5711(13) 0.115(6) Uiso 1 1 d . D 1 F6 F 0.2727(11) 0.3240(5) 0.5362(10) 0.079(4) Uiso 1 1 d . D 1 F8 F 0.8916(14) 0.3127(6) 0.5179(12) 0.117(6) Uiso 1 1 d . D 1 F7 F 0.7849(11) 0.3161(5) 0.6076(11) 0.084(5) Uiso 1 1 d . D 1 F9 F 0.7374(17) 0.3454(7) 0.4639(15) 0.155(8) Uiso 1 1 d . D 1 F10 F 0.8251(12) 0.2073(5) 0.1902(11) 0.095(5) Uiso 1 1 d . D 1 F11 F 0.7359(11) 0.1454(5) 0.1992(9) 0.072(4) Uiso 1 1 d . D 1 F12 F 0.6467(13) 0.2030(5) 0.1275(12) 0.104(5) Uiso 1 1 d . D 1 F13 F 0.8043(10) 0.0202(4) 0.5774(9) 0.060(4) Uiso 1 1 d . D 1 F14 F 0.7811(11) 0.0276(5) 0.4160(10) 0.080(5) Uiso 1 1 d . D 1 F15 F 0.7207(12) -0.0344(6) 0.4719(11) 0.112(6) Uiso 1 1 d . D 1 F16 F 0.3288(11) -0.0445(5) 0.4795(10) 0.096(5) Uiso 1 1 d . D 1 F17 F 0.2485(10) 0.0060(4) 0.3649(9) 0.057(4) Uiso 1 1 d . D 1 F18 F 0.2457(10) 0.0139(4) 0.5287(9) 0.059(4) Uiso 1 1 d . D 1 F19 F 0.7896(9) 0.1515(4) 0.9674(9) 0.055(4) Uiso 1 1 d . D 1 F20 F 0.8594(10) 0.1662(5) 0.8323(10) 0.071(4) Uiso 1 1 d . D 1 F21 F 0.8065(11) 0.2195(5) 0.9122(11) 0.083(5) Uiso 1 1 d . D 1 F22 F 0.3924(10) 0.1901(4) 0.9548(10) 0.069(4) Uiso 1 1 d . D 1 F23 F 0.2966(10) 0.2113(4) 0.8075(9) 0.064(4) Uiso 1 1 d . D 1 F24 F 0.3010(10) 0.1405(4) 0.8405(9) 0.062(4) Uiso 1 1 d . D 1 O1 O 0.416(2) 0.0505(9) 0.189(2) 0.226(13) Uiso 1 1 d D E 1 C70 C 0.5105(15) 0.0227(6) 0.2087(13) 0.033(6) Uiso 1 1 d D E 1 H70A H 0.4892 -0.0120 0.2029 0.040 Uiso 1 1 calc R E 1 H70B H 0.5531 0.0288 0.2824 0.040 Uiso 1 1 calc R E 1 C71 C 0.5814(18) 0.0332(8) 0.1351(17) 0.079(9) Uiso 1 1 d D E 1 H71A H 0.5956 0.0032 0.0977 0.095 Uiso 1 1 calc R E 1 H71B H 0.6543 0.0465 0.1740 0.095 Uiso 1 1 calc R E 1 C72 C 0.521(2) 0.0697(9) 0.0567(17) 0.097(10) Uiso 1 1 d D E 1 H72A H 0.4815 0.0537 -0.0100 0.116 Uiso 1 1 calc R E 1 H72B H 0.5740 0.0940 0.0394 0.116 Uiso 1 1 calc R E 1 C73 C 0.439(2) 0.0929(8) 0.1136(19) 0.089(9) Uiso 1 1 d D E 1 H73A H 0.3693 0.1028 0.0627 0.107 Uiso 1 1 calc R E 1 H73B H 0.4723 0.1215 0.1554 0.107 Uiso 1 1 calc R E 1 O2 O 0.7004(13) 0.8531(6) 0.7475(13) 0.083(6) Uiso 1 1 d D F 1 C74 C 0.6467(17) 0.8811(7) 0.6645(16) 0.063(8) Uiso 1 1 d D F 1 H74A H 0.6903 0.8830 0.6083 0.076 Uiso 1 1 calc R F 1 H74B H 0.6342 0.9143 0.6886 0.076 Uiso 1 1 calc R F 1 C75 C 0.538(2) 0.8554(10) 0.6248(19) 0.142(13) Uiso 1 1 d D F 1 H75A H 0.5475 0.8284 0.5769 0.171 Uiso 1 1 calc R F 1 H75B H 0.4806 0.8780 0.5855 0.171 Uiso 1 1 calc R F 1 C76 C 0.5048(18) 0.8365(9) 0.723(2) 0.116(11) Uiso 1 1 d D F 1 H76A H 0.4507 0.8094 0.7060 0.139 Uiso 1 1 calc R F 1 H76B H 0.4718 0.8624 0.7598 0.139 Uiso 1 1 calc R F 1 C77 C 0.6159(18) 0.8194(9) 0.7904(17) 0.098(10) Uiso 1 1 d D F 1 H77A H 0.6292 0.7847 0.7779 0.118 Uiso 1 1 calc R F 1 H77B H 0.6203 0.8247 0.8674 0.118 Uiso 1 1 calc R F 1 O3 O 0.077(2) 0.1238(10) 0.480(2) 0.268(15) Uiso 1 1 d D G 1 C78 C -0.027(3) 0.1460(14) 0.445(2) 0.23(2) Uiso 1 1 d D G 1 H78A H -0.0801 0.1245 0.3965 0.277 Uiso 1 1 calc R G 1 H78B H -0.0197 0.1769 0.4073 0.277 Uiso 1 1 calc R G 1 C79 C -0.0613(19) 0.1543(11) 0.545(2) 0.139(13) Uiso 1 1 d D G 1 H79A H -0.0904 0.1237 0.5687 0.166 Uiso 1 1 calc R G 1 H79B H -0.1225 0.1786 0.5338 0.166 Uiso 1 1 calc R G 1 C80 C 0.035(2) 0.1719(10) 0.6290(19) 0.117(11) Uiso 1 1 d D G 1 H80A H 0.0330 0.1580 0.6997 0.140 Uiso 1 1 calc R G 1 H80B H 0.0358 0.2078 0.6338 0.140 Uiso 1 1 calc R G 1 C81 C 0.1326(17) 0.1527(9) 0.5872(19) 0.088(9) Uiso 1 1 d D G 1 H81A H 0.1795 0.1308 0.6399 0.106 Uiso 1 1 calc R G 1 H81B H 0.1800 0.1797 0.5716 0.106 Uiso 1 1 calc R G 1 _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 Fe N3 1.609(13) . ? Fe N1 1.906(14) . ? Fe P2 2.376(5) . ? Fe P1 2.376(5) . ? N1 N2 1.405(17) . ? N1 C11 1.44(2) . ? N2 C13 1.39(2) . ? N2 B1 1.60(2) . ? N3 C1 1.441(19) . ? P1 C31 1.795(18) . ? P1 C27 1.898(17) . ? P1 C23 1.948(17) . ? P2 C22 1.804(15) . ? P2 C14 1.891(16) . ? P2 C18 1.936(17) . ? B1 C32 1.56(3) . ? B1 C22 1.60(2) . ? B1 C31 1.83(3) . ? C1 C4 1.52(2) . ? C1 C3 1.52(2) . ? C1 C2 1.62(2) . ? C2 C5 1.44(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C9 1.43(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C7 1.57(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C10 1.51(2) . ? C5 C6 1.59(2) . ? C5 H5 1.0000 . ? C6 C7 1.57(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.48(2) . ? C7 H7 1.0000 . ? C8 C9 1.61(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.61(2) . ? C9 H9 1.0000 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.46(2) . ? C11 H11 0.9500 . ? C12 C13 1.40(2) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C16 1.42(2) . ? C14 C17 1.54(2) . ? C14 C15 1.55(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.53(2) . ? C18 C21 1.57(2) . ? C18 C20 1.59(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C25 1.43(2) . ? C23 C26 1.52(2) . ? C23 C24 1.53(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C30 1.42(2) . ? C27 C29 1.50(2) . ? C27 C28 1.60(2) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.43(2) . ? C32 C37 1.45(2) . ? C33 C34 1.281(19) . ? C33 H33 0.9500 . ? C34 C35 1.57(2) . ? C34 H34 0.9500 . ? C35 C36 1.31(2) . ? C35 H35 0.9500 . ? C36 C37 1.37(2) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? B2 C38 1.52(2) . ? B2 C46 1.60(2) . ? B2 C62 1.62(2) . ? B2 C54 1.62(2) . ? C38 C39 1.37(2) . ? C38 C43 1.41(2) . ? C39 C40 1.43(2) . ? C39 H39 0.9500 . ? C40 C41 1.38(2) . ? C40 C44 1.56(3) . ? C41 C42 1.40(2) . ? C41 H41 0.9500 . ? C42 C43 1.40(2) . ? C42 C45 1.42(2) . ? C43 H43 0.9500 . ? C44 F4 1.25(2) . ? C44 F6 1.26(2) . ? C44 F5 1.31(2) . ? C45 F3 1.294(18) . ? C45 F2 1.333(19) . ? C45 F1 1.364(18) . ? C46 C47 1.34(2) . ? C46 C51 1.43(2) . ? C47 C48 1.40(2) . ? C47 H47 0.9500 . ? C48 C49 1.47(2) . ? C48 C52 1.49(3) . ? C49 C50 1.34(2) . ? C49 H49 0.9500 . ? C50 C51 1.41(2) . ? C50 C53 1.45(3) . ? C51 H51 0.9500 . ? C52 F9 1.22(3) . ? C52 F8 1.30(3) . ? C52 F7 1.31(3) . ? C53 F12 1.29(2) . ? C53 F10 1.30(2) . ? C53 F11 1.32(2) . ? C54 C55 1.42(2) . ? C54 C59 1.53(2) . ? C55 C56 1.46(2) . ? C55 H55 0.9500 . ? C56 C57 1.34(2) . ? C56 C61 1.38(2) . ? C57 C58 1.42(2) . ? C57 H57 0.9500 . ? C58 C59 1.35(2) . ? C58 C60 1.54(2) . ? C59 H59 0.9500 . ? C60 F18 1.283(19) . ? C60 F17 1.290(19) . ? C60 F16 1.35(2) . ? C61 F13 1.295(19) . ? C61 F15 1.33(2) . ? C61 F14 1.39(2) . ? C62 C67 1.347(19) . ? C62 C63 1.41(2) . ? C63 C64 1.47(2) . ? C63 H63 0.9500 . ? C64 C65 1.32(2) . ? C64 C69 1.41(2) . ? C65 C66 1.42(2) . ? C65 H65 0.9500 . ? C66 C68 1.38(2) . ? C66 C67 1.45(2) . ? C67 H67 0.9500 . ? C68 F20 1.29(2) . ? C68 F19 1.35(2) . ? C68 F21 1.45(2) . ? C69 F23 1.337(18) . ? C69 F24 1.345(18) . ? C69 F22 1.353(18) . ? O1 C70 1.362(19) . ? O1 C73 1.582(19) . ? C70 C71 1.447(18) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.50(2) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.51(2) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? O2 C74 1.362(17) . ? O2 C77 1.579(18) . ? C74 C75 1.49(2) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.51(2) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 C77 1.51(2) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? O3 C78 1.39(2) . ? O3 C81 1.60(2) . ? C78 C79 1.46(2) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 C80 1.49(2) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 C81 1.51(2) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Fe N1 143.6(7) . . ? N3 Fe P2 111.1(5) . . ? N1 Fe P2 86.3(4) . . ? N3 Fe P1 112.7(5) . . ? N1 Fe P1 86.5(5) . . ? P2 Fe P1 113.7(2) . . ? N2 N1 C11 107.0(14) . . ? N2 N1 Fe 127.9(11) . . ? C11 N1 Fe 125.0(12) . . ? C13 N2 N1 111.4(15) . . ? C13 N2 B1 131.7(15) . . ? N1 N2 B1 116.3(14) . . ? C1 N3 Fe 173.7(12) . . ? C31 P1 C27 108.6(9) . . ? C31 P1 C23 105.2(8) . . ? C27 P1 C23 109.8(8) . . ? C31 P1 Fe 103.6(6) . . ? C27 P1 Fe 110.2(6) . . ? C23 P1 Fe 118.7(5) . . ? C22 P2 C14 111.6(8) . . ? C22 P2 C18 108.4(7) . . ? C14 P2 C18 107.3(7) . . ? C22 P2 Fe 98.9(5) . . ? C14 P2 Fe 111.2(5) . . ? C18 P2 Fe 119.1(5) . . ? C32 B1 N2 109.7(15) . . ? C32 B1 C22 112.4(15) . . ? N2 B1 C22 112.6(15) . . ? C32 B1 C31 106.0(15) . . ? N2 B1 C31 101.9(13) . . ? C22 B1 C31 113.6(15) . . ? N3 C1 C4 111.3(14) . . ? N3 C1 C3 111.7(13) . . ? C4 C1 C3 107.6(14) . . ? N3 C1 C2 108.4(13) . . ? C4 C1 C2 110.5(14) . . ? C3 C1 C2 107.3(13) . . ? C5 C2 C1 107.8(14) . . ? C5 C2 H2A 110.2 . . ? C1 C2 H2A 110.2 . . ? C5 C2 H2B 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? C9 C3 C1 119.0(15) . . ? C9 C3 H3A 107.6 . . ? C1 C3 H3A 107.6 . . ? C9 C3 H3B 107.6 . . ? C1 C3 H3B 107.6 . . ? H3A C3 H3B 107.0 . . ? C1 C4 C7 107.5(15) . . ? C1 C4 H4A 110.2 . . ? C7 C4 H4A 110.2 . . ? C1 C4 H4B 110.2 . . ? C7 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? C2 C5 C10 114.0(16) . . ? C2 C5 C6 113.0(16) . . ? C10 C5 C6 103.8(15) . . ? C2 C5 H5 108.6 . . ? C10 C5 H5 108.6 . . ? C6 C5 H5 108.6 . . ? C7 C6 C5 107.9(17) . . ? C7 C6 H6A 110.1 . . ? C5 C6 H6A 110.1 . . ? C7 C6 H6B 110.1 . . ? C5 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? C8 C7 C6 104.7(17) . . ? C8 C7 C4 116.1(16) . . ? C6 C7 C4 110.2(16) . . ? C8 C7 H7 108.6 . . ? C6 C7 H7 108.6 . . ? C4 C7 H7 108.6 . . ? C7 C8 C9 110.2(16) . . ? C7 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? C7 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C3 C9 C8 110.3(15) . . ? C3 C9 C10 105.9(15) . . ? C8 C9 C10 99.9(15) . . ? C3 C9 H9 113.3 . . ? C8 C9 H9 113.3 . . ? C10 C9 H9 113.3 . . ? C5 C10 C9 112.6(15) . . ? C5 C10 H10A 109.1 . . ? C9 C10 H10A 109.1 . . ? C5 C10 H10B 109.1 . . ? C9 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? N1 C11 C12 105.3(17) . . ? N1 C11 H11 127.3 . . ? C12 C11 H11 127.3 . . ? C13 C12 C11 109.2(17) . . ? C13 C12 H12 125.4 . . ? C11 C12 H12 125.4 . . ? N2 C13 C12 107.0(17) . . ? N2 C13 H13 126.5 . . ? C12 C13 H13 126.5 . . ? C16 C14 C17 107.0(16) . . ? C16 C14 C15 110.5(15) . . ? C17 C14 C15 106.1(14) . . ? C16 C14 P2 118.1(13) . . ? C17 C14 P2 109.0(12) . . ? C15 C14 P2 105.5(12) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? C19 C18 C21 112.5(14) . . ? C19 C18 C20 108.2(14) . . ? C21 C18 C20 106.5(15) . . ? C19 C18 P2 109.4(11) . . ? C21 C18 P2 112.3(12) . . ? C20 C18 P2 107.7(11) . . ? B1 C22 P2 123.4(12) . . ? B1 C22 H22A 106.5 . . ? P2 C22 H22A 106.5 . . ? B1 C22 H22B 106.5 . . ? P2 C22 H22B 106.5 . . ? H22A C22 H22B 106.5 . . ? C25 C23 C26 115.6(16) . . ? C25 C23 C24 112.7(15) . . ? C26 C23 C24 110.7(14) . . ? C25 C23 P1 104.6(12) . . ? C26 C23 P1 106.2(12) . . ? C24 C23 P1 106.1(12) . . ? C30 C27 C29 111.4(16) . . ? C30 C27 C28 112.4(16) . . ? C29 C27 C28 104.6(14) . . ? C30 C27 P1 107.0(13) . . ? C29 C27 P1 114.0(12) . . ? C28 C27 P1 107.6(11) . . ? P1 C31 B1 117.1(13) . . ? P1 C31 H31A 108.0 . . ? B1 C31 H31A 108.0 . . ? P1 C31 H31B 108.0 . . ? B1 C31 H31B 108.0 . . ? H31A C31 H31B 107.3 . . ? C33 C32 C37 110.7(16) . . ? C33 C32 B1 131.5(17) . . ? C37 C32 B1 117.5(17) . . ? C34 C33 C32 133.1(18) . . ? C34 C33 H33 113.4 . . ? C32 C33 H33 113.4 . . ? C33 C34 C35 112.6(17) . . ? C33 C34 H34 123.7 . . ? C35 C34 H34 123.7 . . ? C36 C35 C34 116.6(18) . . ? C36 C35 H35 121.7 . . ? C34 C35 H35 121.7 . . ? C35 C36 C37 127(2) . . ? C35 C36 H36 116.4 . . ? C37 C36 H36 116.4 . . ? C36 C37 C32 119.7(18) . . ? C36 C37 H37 120.2 . . ? C32 C37 H37 120.1 . . ? C38 B2 C46 104.4(14) . . ? C38 B2 C62 114.9(15) . . ? C46 B2 C62 111.6(15) . . ? C38 B2 C54 115.2(16) . . ? C46 B2 C54 109.1(15) . . ? C62 B2 C54 101.7(14) . . ? C39 C38 C43 112.2(16) . . ? C39 C38 B2 123.3(17) . . ? C43 C38 B2 124.4(16) . . ? C38 C39 C40 123.8(18) . . ? C38 C39 H39 118.1 . . ? C40 C39 H39 118.1 . . ? C41 C40 C39 119.4(19) . . ? C41 C40 C44 121.1(19) . . ? C39 C40 C44 119.5(19) . . ? C40 C41 C42 121.4(18) . . ? C40 C41 H41 119.3 . . ? C42 C41 H41 119.3 . . ? C41 C42 C43 114.6(18) . . ? C41 C42 C45 118.9(18) . . ? C43 C42 C45 126.5(18) . . ? C42 C43 C38 128.5(17) . . ? C42 C43 H43 115.7 . . ? C38 C43 H43 115.7 . . ? F4 C44 F6 109(2) . . ? F4 C44 F5 111(2) . . ? F6 C44 F5 96.3(18) . . ? F4 C44 C40 117(2) . . ? F6 C44 C40 112(2) . . ? F5 C44 C40 109(2) . . ? F3 C45 F2 102.7(15) . . ? F3 C45 F1 105.7(15) . . ? F2 C45 F1 105.1(15) . . ? F3 C45 C42 114.8(16) . . ? F2 C45 C42 110.3(17) . . ? F1 C45 C42 116.8(16) . . ? C47 C46 C51 109.9(18) . . ? C47 C46 B2 123.2(17) . . ? C51 C46 B2 126.6(17) . . ? C46 C47 C48 125(2) . . ? C46 C47 H47 117.3 . . ? C48 C47 H47 117.3 . . ? C47 C48 C49 120.2(18) . . ? C47 C48 C52 122.1(19) . . ? C49 C48 C52 117.6(19) . . ? C50 C49 C48 118.0(19) . . ? C50 C49 H49 121.0 . . ? C48 C49 H49 121.0 . . ? C49 C50 C51 116.3(19) . . ? C49 C50 C53 120(2) . . ? C51 C50 C53 123(2) . . ? C50 C51 C46 130.0(18) . . ? C50 C51 H51 115.0 . . ? C46 C51 H51 115.0 . . ? F9 C52 F8 109(3) . . ? F9 C52 F7 103(2) . . ? F8 C52 F7 95(2) . . ? F9 C52 C48 113(2) . . ? F8 C52 C48 116(2) . . ? F7 C52 C48 118(2) . . ? F12 C53 F10 113(2) . . ? F12 C53 F11 102(2) . . ? F10 C53 F11 102(2) . . ? F12 C53 C50 115(2) . . ? F10 C53 C50 113(2) . . ? F11 C53 C50 111(2) . . ? C55 C54 C59 111.2(14) . . ? C55 C54 B2 127.7(16) . . ? C59 C54 B2 120.7(15) . . ? C54 C55 C56 124.6(16) . . ? C54 C55 H55 117.7 . . ? C56 C55 H55 117.7 . . ? C57 C56 C61 127.5(18) . . ? C57 C56 C55 118.4(17) . . ? C61 C56 C55 113.7(18) . . ? C56 C57 C58 122.4(17) . . ? C56 C57 H57 118.8 . . ? C58 C57 H57 118.8 . . ? C59 C58 C57 119.8(19) . . ? C59 C58 C60 115.4(19) . . ? C57 C58 C60 124.6(17) . . ? C58 C59 C54 123.6(18) . . ? C58 C59 H59 118.2 . . ? C54 C59 H59 118.2 . . ? F18 C60 F17 111.4(16) . . ? F18 C60 F16 103.9(16) . . ? F17 C60 F16 105.4(17) . . ? F18 C60 C58 116.3(17) . . ? F17 C60 C58 111.9(16) . . ? F16 C60 C58 106.9(16) . . ? F13 C61 F15 108.6(18) . . ? F13 C61 C56 122.4(18) . . ? F15 C61 C56 110.4(19) . . ? F13 C61 F14 98.9(16) . . ? F15 C61 F14 98.2(16) . . ? C56 C61 F14 115.4(18) . . ? C67 C62 C63 116.2(16) . . ? C67 C62 B2 124.9(15) . . ? C63 C62 B2 118.5(15) . . ? C62 C63 C64 119.0(16) . . ? C62 C63 H63 120.5 . . ? C64 C63 H63 120.5 . . ? C65 C64 C69 119.2(17) . . ? C65 C64 C63 122.7(17) . . ? C69 C64 C63 118.1(16) . . ? C64 C65 C66 119.8(17) . . ? C64 C65 H65 120.1 . . ? C66 C65 H65 120.1 . . ? C68 C66 C65 123.6(18) . . ? C68 C66 C67 119.9(18) . . ? C65 C66 C67 116.3(17) . . ? C62 C67 C66 125.6(17) . . ? C62 C67 H67 117.2 . . ? C66 C67 H67 117.2 . . ? F20 C68 F19 108.4(19) . . ? F20 C68 C66 127(2) . . ? F19 C68 C66 118(2) . . ? F20 C68 F21 92.6(16) . . ? F19 C68 F21 93.0(16) . . ? C66 C68 F21 107.9(19) . . ? F23 C69 F24 96.1(13) . . ? F23 C69 F22 101.2(15) . . ? F24 C69 F22 104.4(15) . . ? F23 C69 C64 113.0(16) . . ? F24 C69 C64 120.3(16) . . ? F22 C69 C64 118.1(16) . . ? C70 O1 C73 105.7(16) . . ? O1 C70 C71 111.9(16) . . ? O1 C70 H70A 109.2 . . ? C71 C70 H70A 109.2 . . ? O1 C70 H70B 109.2 . . ? C71 C70 H70B 109.2 . . ? H70A C70 H70B 107.9 . . ? C70 C71 C72 107.4(16) . . ? C70 C71 H71A 110.2 . . ? C72 C71 H71A 110.2 . . ? C70 C71 H71B 110.2 . . ? C72 C71 H71B 110.2 . . ? H71A C71 H71B 108.5 . . ? C71 C72 C73 103.8(16) . . ? C71 C72 H72A 111.0 . . ? C73 C72 H72A 111.0 . . ? C71 C72 H72B 111.0 . . ? C73 C72 H72B 111.0 . . ? H72A C72 H72B 109.0 . . ? C72 C73 O1 102.2(15) . . ? C72 C73 H73A 111.3 . . ? O1 C73 H73A 111.3 . . ? C72 C73 H73B 111.3 . . ? O1 C73 H73B 111.3 . . ? H73A C73 H73B 109.2 . . ? C74 O2 C77 111.6(14) . . ? O2 C74 C75 103.7(16) . . ? O2 C74 H74A 111.0 . . ? C75 C74 H74A 111.0 . . ? O2 C74 H74B 111.0 . . ? C75 C74 H74B 111.0 . . ? H74A C74 H74B 109.0 . . ? C74 C75 C76 105.3(18) . . ? C74 C75 H75A 110.7 . . ? C76 C75 H75A 110.7 . . ? C74 C75 H75B 110.7 . . ? C76 C75 H75B 110.7 . . ? H75A C75 H75B 108.8 . . ? C75 C76 C77 102.2(17) . . ? C75 C76 H76A 111.3 . . ? C77 C76 H76A 111.3 . . ? C75 C76 H76B 111.3 . . ? C77 C76 H76B 111.3 . . ? H76A C76 H76B 109.2 . . ? C76 C77 O2 101.0(14) . . ? C76 C77 H77A 111.6 . . ? O2 C77 H77A 111.6 . . ? C76 C77 H77B 111.6 . . ? O2 C77 H77B 111.6 . . ? H77A C77 H77B 109.4 . . ? C78 O3 C81 104.2(18) . . ? O3 C78 C79 101(2) . . ? O3 C78 H78A 111.5 . . ? C79 C78 H78A 111.5 . . ? O3 C78 H78B 111.5 . . ? C79 C78 H78B 111.5 . . ? H78A C78 H78B 109.3 . . ? C78 C79 C80 111(2) . . ? C78 C79 H79A 109.4 . . ? C80 C79 H79A 109.4 . . ? C78 C79 H79B 109.4 . . ? C80 C79 H79B 109.4 . . ? H79A C79 H79B 108.0 . . ? C79 C80 C81 100.7(17) . . ? C79 C80 H80A 111.6 . . ? C81 C80 H80A 111.6 . . ? C79 C80 H80B 111.6 . . ? C81 C80 H80B 111.6 . . ? H80A C80 H80B 109.4 . . ? C80 C81 O3 105.1(15) . . ? C80 C81 H81A 110.7 . . ? O3 C81 H81A 110.7 . . ? C80 C81 H81B 110.7 . . ? O3 C81 H81B 110.7 . . ? H81A C81 H81B 108.8 . . ? _diffrn_measured_fraction_theta_max 0.832 _diffrn_reflns_theta_full 26.20 _diffrn_measured_fraction_theta_full 0.832 _refine_diff_density_max 0.825 _refine_diff_density_min -0.895 _refine_diff_density_rms 0.136 #===END data_cmt63 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H93 B2 F24 Fe N3 O2 P2' _chemical_formula_weight 1711.97 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' 'P' 'P' 0.1023 0.0942 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.438(17) _cell_length_b 18.86(2) _cell_length_c 22.418(17) _cell_angle_alpha 90.00 _cell_angle_beta 99.66(5) _cell_angle_gamma 90.00 _cell_volume 8104(14) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5317 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 21.01 _exptl_crystal_description blades _exptl_crystal_colour dark _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.074 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5316 _exptl_absorpt_coefficient_mu 0.492 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50257 _diffrn_reflns_av_R_equivalents 0.1154 _diffrn_reflns_av_sigmaI/netI 0.1548 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.74 _reflns_number_total 13730 _reflns_number_gt 6519 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13730 _refine_ls_number_parameters 1051 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1563 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.216 _refine_ls_restrained_S_all 1.218 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.7879(3) 0.2837(3) 0.9082(2) 0.0214(14) Uani 1 1 d . . . Fe1 Fe 0.74742(3) 0.39246(3) 0.79443(3) 0.02088(18) Uani 1 1 d . . . N1 N 0.77588(18) 0.24673(19) 0.84316(15) 0.0172(9) Uani 1 1 d . . . N2 N 0.75930(18) 0.29027(18) 0.79265(17) 0.0203(9) Uani 1 1 d . . . N3 N 0.73055(18) 0.45832(19) 0.74689(16) 0.0248(10) Uani 1 1 d . . . P1 P 0.66818(7) 0.38249(7) 0.86464(5) 0.0231(3) Uani 1 1 d . . . P2 P 0.86031(6) 0.39904(7) 0.84549(5) 0.0213(3) Uani 1 1 d . . . C1 C 0.7204(2) 0.5176(3) 0.7047(2) 0.0290(13) Uani 1 1 d . . . C2 C 0.6459(3) 0.5121(3) 0.6710(3) 0.085(3) Uani 1 1 d . . . H2A H 0.6125 0.5185 0.6995 0.102 Uiso 1 1 calc R . . H2B H 0.6378 0.4648 0.6519 0.102 Uiso 1 1 calc R . . C3 C 0.7702(3) 0.5076(2) 0.6591(2) 0.0395(15) Uani 1 1 d . . . H3A H 0.7626 0.4605 0.6396 0.047 Uiso 1 1 calc R . . H3B H 0.8192 0.5101 0.6802 0.047 Uiso 1 1 calc R . . C4 C 0.7327(3) 0.5898(2) 0.7340(2) 0.0526(18) Uani 1 1 d . . . H4A H 0.7812 0.5929 0.7560 0.063 Uiso 1 1 calc R . . H4B H 0.7007 0.5967 0.7635 0.063 Uiso 1 1 calc R . . C5 C 0.7566(3) 0.5665(3) 0.6106(2) 0.0495(17) Uani 1 1 d . . . H5 H 0.7893 0.5596 0.5810 0.059 Uiso 1 1 calc R . . C6 C 0.6832(4) 0.5614(4) 0.5774(3) 0.102(3) Uani 1 1 d . . . H6A H 0.6746 0.5985 0.5459 0.123 Uiso 1 1 calc R . . H6B H 0.6754 0.5145 0.5576 0.123 Uiso 1 1 calc R . . C7 C 0.6350(4) 0.5710(5) 0.6218(4) 0.118(4) Uani 1 1 d . . . H7 H 0.5861 0.5674 0.5995 0.142 Uiso 1 1 calc R . . C8 C 0.6439(4) 0.6422(4) 0.6515(4) 0.111(4) Uani 1 1 d U . . H8A H 0.6112 0.6474 0.6806 0.134 Uiso 1 1 calc R . . H8B H 0.6340 0.6801 0.6207 0.134 Uiso 1 1 calc R . . C9 C 0.7200(4) 0.6483(3) 0.6849(2) 0.063(2) Uani 1 1 d . . . H9 H 0.7275 0.6960 0.7044 0.076 Uiso 1 1 calc R . . C10 C 0.7708(3) 0.6381(3) 0.6407(2) 0.0452(16) Uani 1 1 d . . . H10A H 0.7644 0.6761 0.6098 0.054 Uiso 1 1 calc R . . H10B H 0.8195 0.6401 0.6625 0.054 Uiso 1 1 calc R . . C11 C 0.7313(2) 0.2768(2) 0.68008(19) 0.0292(13) Uani 1 1 d . . . H11A H 0.7233 0.3280 0.6820 0.044 Uiso 1 1 calc R . . H11B H 0.6891 0.2538 0.6586 0.044 Uiso 1 1 calc R . . H11C H 0.7703 0.2678 0.6585 0.044 Uiso 1 1 calc R . . C12 C 0.7482(2) 0.2478(3) 0.7423(2) 0.0199(12) Uani 1 1 d . . . C13 C 0.7560(2) 0.1782(2) 0.7608(2) 0.0228(12) Uani 1 1 d . . . H13 H 0.7509 0.1376 0.7353 0.027 Uiso 1 1 calc R . . C14 C 0.7728(2) 0.1779(2) 0.8238(2) 0.0217(12) Uani 1 1 d . . . C15 C 0.7863(2) 0.1146(2) 0.86426(19) 0.0289(13) Uani 1 1 d . . . H15A H 0.8336 0.1173 0.8875 0.043 Uiso 1 1 calc R . . H15B H 0.7816 0.0714 0.8397 0.043 Uiso 1 1 calc R . . H15C H 0.7524 0.1136 0.8921 0.043 Uiso 1 1 calc R . . C16 C 0.7080(2) 0.3123(2) 0.91421(19) 0.0226(12) Uani 1 1 d . . . H16A H 0.7093 0.3286 0.9564 0.027 Uiso 1 1 calc R . . H16B H 0.6763 0.2709 0.9082 0.027 Uiso 1 1 calc R . . C17 C 0.6507(3) 0.4587(2) 0.9162(2) 0.0271(13) Uani 1 1 d . . . C18 C 0.6430(2) 0.5285(2) 0.8801(2) 0.0314(14) Uani 1 1 d . . . H18A H 0.6029 0.5250 0.8472 0.047 Uiso 1 1 calc R . . H18B H 0.6854 0.5371 0.8630 0.047 Uiso 1 1 calc R . . H18C H 0.6357 0.5678 0.9069 0.047 Uiso 1 1 calc R . . C19 C 0.5846(2) 0.4476(2) 0.9446(2) 0.0332(14) Uani 1 1 d . . . H19A H 0.5809 0.4856 0.9736 0.050 Uiso 1 1 calc R . . H19B H 0.5875 0.4017 0.9654 0.050 Uiso 1 1 calc R . . H19C H 0.5434 0.4482 0.9127 0.050 Uiso 1 1 calc R . . C20 C 0.7113(2) 0.4637(2) 0.97011(19) 0.0299(13) Uani 1 1 d . . . H20A H 0.7558 0.4587 0.9555 0.045 Uiso 1 1 calc R . . H20B H 0.7068 0.4258 0.9991 0.045 Uiso 1 1 calc R . . H20C H 0.7098 0.5098 0.9900 0.045 Uiso 1 1 calc R . . C21 C 0.5823(2) 0.3483(3) 0.8215(2) 0.0279(13) Uani 1 1 d . . . C22 C 0.5975(2) 0.2965(2) 0.7728(2) 0.0342(14) Uani 1 1 d . . . H22A H 0.6274 0.2581 0.7918 0.051 Uiso 1 1 calc R . . H22B H 0.6213 0.3216 0.7438 0.051 Uiso 1 1 calc R . . H22C H 0.5536 0.2766 0.7516 0.051 Uiso 1 1 calc R . . C23 C 0.5384(2) 0.4100(2) 0.7877(2) 0.0371(14) Uani 1 1 d . . . H23A H 0.5684 0.4394 0.7668 0.056 Uiso 1 1 calc R . . H23B H 0.5188 0.4390 0.8170 0.056 Uiso 1 1 calc R . . H23C H 0.5004 0.3902 0.7581 0.056 Uiso 1 1 calc R . . C24 C 0.5380(2) 0.3075(2) 0.8606(2) 0.0344(14) Uani 1 1 d . . . H24A H 0.4965 0.2883 0.8348 0.052 Uiso 1 1 calc R . . H24B H 0.5236 0.3397 0.8906 0.052 Uiso 1 1 calc R . . H24C H 0.5655 0.2686 0.8814 0.052 Uiso 1 1 calc R . . C25 C 0.8484(2) 0.3480(2) 0.91145(18) 0.0234(12) Uani 1 1 d . . . H25A H 0.8940 0.3259 0.9274 0.028 Uiso 1 1 calc R . . H25B H 0.8388 0.3824 0.9424 0.028 Uiso 1 1 calc R . . C26 C 0.8956(2) 0.4894(2) 0.8694(2) 0.0245(12) Uani 1 1 d . . . C27 C 0.8371(2) 0.5344(2) 0.8878(2) 0.0311(13) Uani 1 1 d . . . H27A H 0.8239 0.5151 0.9249 0.047 Uiso 1 1 calc R . . H27B H 0.7966 0.5338 0.8553 0.047 Uiso 1 1 calc R . . H27C H 0.8535 0.5833 0.8951 0.047 Uiso 1 1 calc R . . C28 C 0.9203(2) 0.5287(2) 0.8160(2) 0.0320(14) Uani 1 1 d . . . H28A H 0.8828 0.5284 0.7809 0.048 Uiso 1 1 calc R . . H28B H 0.9614 0.5047 0.8056 0.048 Uiso 1 1 calc R . . H28C H 0.9323 0.5777 0.8278 0.048 Uiso 1 1 calc R . . C29 C 0.9546(3) 0.4865(2) 0.9242(2) 0.0401(15) Uani 1 1 d . . . H29A H 0.9659 0.5347 0.9391 0.060 Uiso 1 1 calc R . . H29B H 0.9961 0.4649 0.9122 0.060 Uiso 1 1 calc R . . H29C H 0.9397 0.4581 0.9563 0.060 Uiso 1 1 calc R . . C30 C 0.9254(2) 0.3512(2) 0.8044(2) 0.0241(12) Uani 1 1 d . . . C31 C 0.9114(2) 0.3724(2) 0.73705(18) 0.0309(13) Uani 1 1 d . . . H31A H 0.9431 0.3464 0.7153 0.046 Uiso 1 1 calc R . . H31B H 0.9191 0.4235 0.7334 0.046 Uiso 1 1 calc R . . H31C H 0.8630 0.3610 0.7196 0.046 Uiso 1 1 calc R . . C32 C 1.0019(2) 0.3681(2) 0.8328(2) 0.0344(14) Uani 1 1 d . . . H32A H 1.0093 0.3569 0.8761 0.052 Uiso 1 1 calc R . . H32B H 1.0113 0.4185 0.8273 0.052 Uiso 1 1 calc R . . H32C H 1.0336 0.3394 0.8129 0.052 Uiso 1 1 calc R . . C33 C 0.9195(2) 0.2704(2) 0.8087(2) 0.0275(13) Uani 1 1 d . . . H33A H 0.8745 0.2549 0.7858 0.041 Uiso 1 1 calc R . . H33B H 0.9225 0.2565 0.8512 0.041 Uiso 1 1 calc R . . H33C H 0.9575 0.2481 0.7918 0.041 Uiso 1 1 calc R . . C34 C 0.8138(3) 0.2268(2) 0.96218(19) 0.0197(12) Uani 1 1 d . . . C35 C 0.8835(3) 0.2054(2) 0.9776(2) 0.0301(13) Uani 1 1 d . . . H35 H 0.9172 0.2248 0.9561 0.036 Uiso 1 1 calc R . . C36 C 0.9052(3) 0.1562(3) 1.0238(2) 0.0378(14) Uani 1 1 d . . . H36 H 0.9529 0.1426 1.0329 0.045 Uiso 1 1 calc R . . C37 C 0.8580(3) 0.1277(3) 1.0558(2) 0.0388(15) Uani 1 1 d . . . H37 H 0.8728 0.0945 1.0872 0.047 Uiso 1 1 calc R . . C38 C 0.7897(3) 0.1470(3) 1.0427(2) 0.0406(15) Uani 1 1 d . . . H38 H 0.7567 0.1269 1.0647 0.049 Uiso 1 1 calc R . . C39 C 0.7683(3) 0.1959(2) 0.9973(2) 0.0310(13) Uani 1 1 d . . . H39 H 0.7205 0.2092 0.9895 0.037 Uiso 1 1 calc R . . B2 B 0.7534(3) 0.9413(3) 0.7030(2) 0.0196(14) Uani 1 1 d . . . C40 C 0.7654(2) 0.8739(2) 0.75084(18) 0.0179(12) Uani 1 1 d . . . C41 C 0.7086(2) 0.8398(2) 0.77025(18) 0.0199(12) Uani 1 1 d . . . H41 H 0.6627 0.8569 0.7563 0.024 Uiso 1 1 calc R . . C42 C 0.7175(2) 0.7813(2) 0.8095(2) 0.0229(12) Uani 1 1 d . A . C43 C 0.7827(3) 0.7539(2) 0.8283(2) 0.0274(13) Uani 1 1 d . . . H43 H 0.7886 0.7141 0.8547 0.033 Uiso 1 1 calc R . . C44 C 0.8400(3) 0.7839(2) 0.8090(2) 0.0223(12) Uani 1 1 d . . . C45 C 0.8298(2) 0.8432(2) 0.77024(18) 0.0202(12) Uani 1 1 d . . . H45 H 0.8694 0.8632 0.7567 0.024 Uiso 1 1 calc R . . C46 C 0.6551(4) 0.7525(3) 0.8304(4) 0.0490(19) Uani 1 1 d . . . C47 C 0.9118(3) 0.7563(3) 0.8274(2) 0.0312(14) Uani 1 1 d . . . C48 C 0.8191(2) 0.9959(2) 0.70884(19) 0.0161(11) Uani 1 1 d . . . C49 C 0.8246(2) 1.0412(2) 0.66010(19) 0.0201(12) Uani 1 1 d . . . H49 H 0.7919 1.0359 0.6238 0.024 Uiso 1 1 calc R . . C50 C 0.8756(2) 1.0934(2) 0.6626(2) 0.0216(12) Uani 1 1 d . . . C51 C 0.9249(2) 1.1030(2) 0.7144(2) 0.0238(12) Uani 1 1 d . . . H51 H 0.9595 1.1389 0.7166 0.029 Uiso 1 1 calc R . . C52 C 0.9219(2) 1.0586(2) 0.7625(2) 0.0212(12) Uani 1 1 d . . . C53 C 0.8698(2) 1.0072(2) 0.7603(2) 0.0203(12) Uani 1 1 d . . . H53 H 0.8686 0.9788 0.7952 0.024 Uiso 1 1 calc R . . C54 C 0.8771(3) 1.1406(3) 0.6086(2) 0.0349(14) Uani 1 1 d . . . C55 C 0.9760(3) 1.0646(3) 0.8183(2) 0.0336(14) Uani 1 1 d . . . C56 C 0.7410(2) 0.9025(2) 0.63683(18) 0.0165(11) Uani 1 1 d . . . C57 C 0.6757(2) 0.8793(2) 0.60634(18) 0.0177(11) Uani 1 1 d . . . H57 H 0.6355 0.8899 0.6236 0.021 Uiso 1 1 calc R . . C58 C 0.6670(2) 0.8420(2) 0.55269(19) 0.0179(11) Uani 1 1 d . . . C59 C 0.7237(2) 0.8238(2) 0.52594(19) 0.0204(12) Uani 1 1 d . . . H59 H 0.7179 0.7976 0.4892 0.024 Uiso 1 1 calc R . . C60 C 0.7891(2) 0.8450(2) 0.55454(19) 0.0178(11) Uani 1 1 d . . . C61 C 0.7975(2) 0.8833(2) 0.60787(19) 0.0207(12) Uani 1 1 d . . . H61 H 0.8432 0.8974 0.6258 0.025 Uiso 1 1 calc R . . C62 C 0.5949(3) 0.8203(3) 0.5229(2) 0.0290(13) Uani 1 1 d . . . C63 C 0.8521(3) 0.8267(3) 0.5269(2) 0.0293(13) Uani 1 1 d . . . C64 C 0.6871(2) 0.9903(2) 0.7133(2) 0.0195(12) Uani 1 1 d . . . C65 C 0.6676(2) 1.0004(2) 0.7705(2) 0.0211(12) Uani 1 1 d . . . H65 H 0.6907 0.9735 0.8038 0.025 Uiso 1 1 calc R . . C66 C 0.6160(2) 1.0480(2) 0.7806(2) 0.0205(12) Uani 1 1 d . . . C67 C 0.5810(2) 1.0869(2) 0.7334(2) 0.0243(12) Uani 1 1 d . . . H67 H 0.5450 1.1186 0.7400 0.029 Uiso 1 1 calc R . . C68 C 0.5979(2) 1.0802(2) 0.6768(2) 0.0232(12) Uani 1 1 d . . . C69 C 0.6500(2) 1.0316(2) 0.66760(19) 0.0193(12) Uani 1 1 d . . . H69 H 0.6604 1.0267 0.6279 0.023 Uiso 1 1 calc R . . C70 C 0.5615(3) 1.1215(3) 0.6242(2) 0.0341(14) Uani 1 1 d . . . C71 C 0.5956(3) 1.0558(3) 0.8420(2) 0.0337(14) Uani 1 1 d . . . F1A F 0.6001(7) 0.759(2) 0.7983(17) 0.065(10) Uani 0.51(6) 1 d P A 1 F3A F 0.6478(19) 0.7914(8) 0.8856(15) 0.060(7) Uani 0.51(6) 1 d P A 1 F1B F 0.6060(10) 0.721(2) 0.7764(10) 0.069(6) Uani 0.49(6) 1 d P A 2 F3B F 0.6143(18) 0.7946(7) 0.851(2) 0.073(10) Uani 0.49(6) 1 d P A 2 F2 F 0.66579(15) 0.69103(15) 0.85836(13) 0.0537(9) Uani 1 1 d . A . F4 F 0.91725(14) 0.70847(14) 0.87130(13) 0.0464(8) Uani 1 1 d . . . F5 F 0.95821(15) 0.80762(16) 0.84788(14) 0.0570(9) Uani 1 1 d . . . F6 F 0.93704(15) 0.72590(16) 0.78141(13) 0.0601(10) Uani 1 1 d . . . F7 F 0.81480(18) 1.15367(17) 0.57710(14) 0.0692(11) Uani 1 1 d . . . F8 F 0.9126(2) 1.1127(2) 0.56976(16) 0.1113(17) Uani 1 1 d . . . F9 F 0.9039(2) 1.20341(18) 0.62280(14) 0.0915(13) Uani 1 1 d . . . F10 F 1.03199(15) 1.10318(18) 0.80852(13) 0.0633(10) Uani 1 1 d . . . F11 F 1.00183(16) 1.00340(16) 0.83860(13) 0.0634(10) Uani 1 1 d . . . F12 F 0.95396(14) 1.09836(16) 0.86364(12) 0.0538(9) Uani 1 1 d . . . F13 F 0.57014(14) 0.76549(14) 0.55132(12) 0.0436(8) Uani 1 1 d . . . F14 F 0.54823(14) 0.87298(15) 0.52508(11) 0.0410(8) Uani 1 1 d . . . F15 F 0.59029(13) 0.80292(16) 0.46551(12) 0.0479(9) Uani 1 1 d . . . F16 F 0.83648(13) 0.80458(14) 0.46975(12) 0.0416(8) Uani 1 1 d . . . F17 F 0.89655(14) 0.88214(15) 0.52710(11) 0.0372(7) Uani 1 1 d . . . F18 F 0.89054(14) 0.77443(14) 0.55783(12) 0.0404(8) Uani 1 1 d . . . F19 F 0.60411(16) 1.15450(16) 0.59331(14) 0.0612(10) Uani 1 1 d . . . F20 F 0.52334(16) 1.08021(16) 0.58341(13) 0.0618(10) Uani 1 1 d . . . F21 F 0.51859(19) 1.17008(18) 0.63959(13) 0.0827(13) Uani 1 1 d . . . F22 F 0.52936(17) 1.04054(19) 0.84240(14) 0.0739(11) Uani 1 1 d . . . F23 F 0.60462(17) 1.12340(15) 0.86219(13) 0.0630(10) Uani 1 1 d . . . F24 F 0.63280(16) 1.01621(15) 0.88488(12) 0.0493(9) Uani 1 1 d . . . O1 O 0.8580(4) 0.9563(3) 0.9053(2) 0.128(2) Uani 1 1 d D . . C72 C 0.7989(4) 0.9283(4) 0.9316(3) 0.102(3) Uani 1 1 d D . . H72A H 0.7623 0.9095 0.8993 0.122 Uiso 1 1 calc R . . H72B H 0.7782 0.9661 0.9535 0.122 Uiso 1 1 calc R . . C73 C 0.8273(6) 0.8708(4) 0.9737(3) 0.139(5) Uani 1 1 d D . . H73A H 0.8343 0.8265 0.9518 0.167 Uiso 1 1 calc R . . H73B H 0.7967 0.8611 1.0039 0.167 Uiso 1 1 calc R . . C74 C 0.9026(5) 0.9063(7) 1.0055(5) 0.199(7) Uani 1 1 d D . . H74A H 0.8988 0.9312 1.0437 0.239 Uiso 1 1 calc R . . H74B H 0.9404 0.8706 1.0130 0.239 Uiso 1 1 calc R . . C75 C 0.9122(4) 0.9558(5) 0.9572(4) 0.145(4) Uani 1 1 d D . . H75A H 0.9166 1.0043 0.9744 0.173 Uiso 1 1 calc R . . H75B H 0.9568 0.9443 0.9436 0.173 Uiso 1 1 calc R . . O2 O 0.5953(4) 0.3618(4) 0.5881(4) 0.191(4) Uani 1 1 d D . . C76 C 0.5878(5) 0.3525(6) 0.5251(4) 0.187(6) Uani 1 1 d D . . H76A H 0.6295 0.3706 0.5099 0.225 Uiso 1 1 calc R . . H76B H 0.5820 0.3016 0.5145 0.225 Uiso 1 1 calc R . . C77 C 0.5289(4) 0.3905(5) 0.4999(3) 0.107(3) Uani 1 1 d D . . H77A H 0.5056 0.3681 0.4619 0.128 Uiso 1 1 calc R . . H77B H 0.5413 0.4399 0.4911 0.128 Uiso 1 1 calc R . . C78 C 0.4825(3) 0.3890(4) 0.5468(3) 0.079(2) Uani 1 1 d . . . H78A H 0.4676 0.4374 0.5561 0.095 Uiso 1 1 calc R . . H78B H 0.4407 0.3594 0.5336 0.095 Uiso 1 1 calc R . . C79 C 0.5273(5) 0.3580(5) 0.5981(3) 0.119(4) Uani 1 1 d . . . H79A H 0.5223 0.3840 0.6355 0.143 Uiso 1 1 calc R . . H79B H 0.5140 0.3079 0.6030 0.143 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 B1 0.021(4) 0.021(3) 0.023(4) -0.007(3) 0.005(3) 0.002(3) Fe1 0.0212(4) 0.0212(4) 0.0207(4) 0.0008(4) 0.0049(3) 0.0004(4) N1 0.014(2) 0.017(2) 0.021(2) 0.000(2) 0.0041(19) 0.0011(19) N2 0.022(2) 0.020(2) 0.018(2) 0.001(2) 0.0021(19) -0.002(2) N3 0.023(3) 0.030(3) 0.021(2) 0.005(2) 0.003(2) 0.004(2) P1 0.0236(8) 0.0214(8) 0.0260(8) 0.0005(6) 0.0088(6) 0.0024(7) P2 0.0218(8) 0.0210(8) 0.0211(7) 0.0001(6) 0.0037(6) -0.0008(7) C1 0.025(3) 0.038(4) 0.022(3) 0.009(3) -0.002(3) -0.002(3) C2 0.029(4) 0.128(6) 0.091(5) 0.093(5) -0.014(4) -0.013(4) C3 0.062(4) 0.028(3) 0.032(3) 0.004(3) 0.016(3) -0.004(3) C4 0.099(5) 0.026(4) 0.040(4) 0.006(3) 0.032(3) 0.025(3) C5 0.076(5) 0.049(4) 0.026(4) 0.014(3) 0.017(3) -0.013(4) C6 0.120(7) 0.120(7) 0.050(5) 0.048(5) -0.034(5) -0.066(6) C7 0.041(5) 0.159(9) 0.143(9) 0.135(8) -0.018(5) 0.006(6) C8 0.097(7) 0.124(8) 0.126(8) 0.111(7) 0.057(6) 0.094(7) C9 0.116(7) 0.036(4) 0.043(4) 0.027(3) 0.028(4) 0.024(4) C10 0.055(4) 0.036(4) 0.044(4) 0.025(3) 0.007(3) 0.001(3) C11 0.031(3) 0.032(3) 0.025(3) -0.002(2) 0.003(3) -0.003(3) C12 0.019(3) 0.028(3) 0.012(3) -0.005(2) 0.003(2) -0.003(3) C13 0.027(3) 0.020(3) 0.022(3) -0.013(2) 0.006(2) -0.001(2) C14 0.019(3) 0.020(3) 0.027(3) -0.004(2) 0.006(2) 0.000(2) C15 0.043(3) 0.017(3) 0.027(3) -0.002(2) 0.006(3) 0.001(3) C16 0.028(3) 0.021(3) 0.019(3) -0.002(2) 0.006(2) 0.000(2) C17 0.033(3) 0.018(3) 0.035(3) 0.004(2) 0.021(3) 0.006(3) C18 0.038(4) 0.026(3) 0.034(3) 0.003(3) 0.020(3) 0.002(3) C19 0.046(4) 0.024(3) 0.035(3) 0.004(3) 0.025(3) 0.007(3) C20 0.035(4) 0.028(3) 0.030(3) -0.005(3) 0.017(3) 0.000(3) C21 0.026(3) 0.032(3) 0.028(3) 0.005(3) 0.009(3) 0.003(3) C22 0.026(3) 0.036(3) 0.039(4) -0.009(3) 0.003(3) -0.006(3) C23 0.020(3) 0.046(4) 0.044(4) 0.005(3) 0.005(3) 0.000(3) C24 0.026(3) 0.033(3) 0.046(4) -0.003(3) 0.013(3) -0.001(3) C25 0.031(3) 0.019(3) 0.019(3) 0.003(2) 0.004(2) 0.005(3) C26 0.026(3) 0.020(3) 0.029(3) 0.000(2) 0.007(3) -0.002(2) C27 0.032(3) 0.026(3) 0.036(3) -0.002(3) 0.007(3) 0.002(3) C28 0.034(3) 0.027(3) 0.037(3) -0.002(3) 0.013(3) -0.007(3) C29 0.044(4) 0.034(4) 0.037(4) -0.006(3) -0.008(3) -0.010(3) C30 0.016(3) 0.031(3) 0.026(3) 0.003(2) 0.007(2) 0.003(2) C31 0.037(3) 0.032(3) 0.027(3) 0.002(2) 0.014(3) 0.004(3) C32 0.024(3) 0.033(3) 0.047(4) 0.001(3) 0.008(3) 0.005(3) C33 0.027(3) 0.025(3) 0.032(3) -0.004(2) 0.011(3) 0.003(3) C34 0.032(3) 0.009(3) 0.018(3) -0.005(2) 0.004(3) 0.000(2) C35 0.038(4) 0.026(3) 0.028(3) 0.001(3) 0.009(3) 0.005(3) C36 0.039(4) 0.029(3) 0.044(4) 0.006(3) 0.003(3) 0.018(3) C37 0.061(4) 0.032(4) 0.024(3) 0.010(3) 0.010(3) 0.011(3) C38 0.056(4) 0.034(4) 0.036(4) 0.010(3) 0.018(3) 0.011(3) C39 0.042(4) 0.026(3) 0.026(3) 0.002(3) 0.006(3) 0.012(3) B2 0.022(3) 0.015(3) 0.024(3) 0.000(3) 0.009(3) 0.001(3) C40 0.022(3) 0.022(3) 0.012(3) -0.008(2) 0.008(2) -0.003(2) C41 0.023(3) 0.024(3) 0.012(3) 0.001(2) 0.000(2) 0.004(2) C42 0.023(3) 0.027(3) 0.024(3) 0.007(2) 0.018(3) 0.000(3) C43 0.038(4) 0.022(3) 0.028(3) 0.012(2) 0.020(3) 0.007(3) C44 0.028(3) 0.020(3) 0.020(3) 0.004(2) 0.007(3) 0.007(3) C45 0.022(3) 0.021(3) 0.019(3) -0.001(2) 0.009(2) 0.000(2) C46 0.041(5) 0.035(4) 0.078(6) 0.038(4) 0.032(5) 0.021(4) C47 0.038(4) 0.026(3) 0.031(4) 0.013(3) 0.007(3) 0.002(3) C48 0.020(3) 0.012(3) 0.018(3) -0.003(2) 0.007(2) 0.002(2) C49 0.022(3) 0.023(3) 0.014(3) -0.002(2) -0.002(2) 0.004(2) C50 0.025(3) 0.018(3) 0.025(3) 0.000(2) 0.013(3) 0.000(3) C51 0.022(3) 0.019(3) 0.033(3) -0.007(3) 0.009(3) -0.002(3) C52 0.018(3) 0.020(3) 0.025(3) -0.010(2) 0.002(3) 0.004(2) C53 0.026(3) 0.018(3) 0.018(3) 0.003(2) 0.007(3) 0.008(3) C54 0.041(4) 0.027(4) 0.037(4) 0.011(3) 0.010(3) -0.005(3) C55 0.028(4) 0.037(4) 0.035(4) -0.004(3) 0.004(3) 0.005(3) C56 0.017(3) 0.015(3) 0.018(3) 0.004(2) 0.002(2) 0.000(2) C57 0.022(3) 0.018(3) 0.014(3) 0.004(2) 0.004(2) 0.003(2) C58 0.016(3) 0.021(3) 0.015(3) 0.004(2) -0.002(2) -0.003(2) C59 0.030(3) 0.017(3) 0.014(3) 0.002(2) 0.003(3) 0.003(3) C60 0.016(3) 0.017(3) 0.020(3) 0.005(2) 0.004(2) 0.005(2) C61 0.023(3) 0.019(3) 0.019(3) -0.002(2) 0.001(2) -0.002(2) C62 0.032(4) 0.037(4) 0.019(3) 0.004(3) 0.005(3) 0.000(3) C63 0.033(4) 0.033(4) 0.021(3) -0.010(3) 0.002(3) -0.001(3) C64 0.019(3) 0.016(3) 0.024(3) 0.002(2) 0.006(2) -0.008(2) C65 0.026(3) 0.017(3) 0.020(3) 0.003(2) 0.005(2) 0.005(2) C66 0.027(3) 0.014(3) 0.022(3) -0.002(2) 0.010(3) -0.004(2) C67 0.018(3) 0.018(3) 0.038(3) -0.006(3) 0.006(3) 0.001(2) C68 0.018(3) 0.018(3) 0.031(3) -0.001(2) -0.002(3) -0.003(2) C69 0.018(3) 0.025(3) 0.014(3) -0.006(2) 0.001(2) -0.003(3) C70 0.029(4) 0.033(4) 0.038(4) -0.003(3) -0.002(3) 0.010(3) C71 0.042(4) 0.020(3) 0.044(4) -0.005(3) 0.020(3) 0.004(3) F1A 0.021(6) 0.10(2) 0.077(15) 0.052(13) 0.002(8) -0.014(9) F3A 0.071(13) 0.044(5) 0.083(13) 0.012(6) 0.064(11) 0.006(6) F1B 0.041(7) 0.113(16) 0.051(8) 0.007(9) 0.005(5) -0.033(8) F3B 0.065(15) 0.039(6) 0.14(3) 0.021(10) 0.076(19) 0.011(8) F2 0.054(2) 0.036(2) 0.078(2) 0.0278(18) 0.0328(19) 0.0003(17) F4 0.043(2) 0.044(2) 0.056(2) 0.0303(17) 0.0204(17) 0.0179(17) F5 0.035(2) 0.041(2) 0.091(3) 0.0161(18) -0.0017(19) 0.0054(18) F6 0.061(2) 0.086(3) 0.040(2) 0.0159(18) 0.0271(18) 0.048(2) F7 0.055(2) 0.072(3) 0.076(3) 0.051(2) -0.003(2) -0.006(2) F8 0.169(4) 0.108(3) 0.085(3) 0.064(3) 0.102(3) 0.094(3) F9 0.140(4) 0.056(3) 0.068(3) 0.027(2) -0.014(2) -0.057(3) F10 0.038(2) 0.096(3) 0.052(2) -0.006(2) -0.0038(17) -0.027(2) F11 0.072(3) 0.046(2) 0.055(2) -0.0086(17) -0.0394(19) 0.020(2) F12 0.047(2) 0.076(2) 0.0355(19) -0.0238(18) -0.0023(16) 0.0188(19) F13 0.033(2) 0.044(2) 0.050(2) 0.0048(16) -0.0049(16) -0.0097(16) F14 0.0279(18) 0.052(2) 0.0414(19) 0.0021(15) 0.0018(14) 0.0108(16) F15 0.0259(18) 0.092(3) 0.0245(18) -0.0249(17) 0.0019(14) -0.0045(17) F16 0.0354(19) 0.063(2) 0.0282(18) -0.0197(16) 0.0115(15) -0.0012(17) F17 0.0327(18) 0.049(2) 0.0330(17) -0.0071(15) 0.0132(14) -0.0105(16) F18 0.0357(19) 0.0374(19) 0.049(2) -0.0018(15) 0.0086(16) 0.0138(16) F19 0.053(2) 0.060(2) 0.064(2) 0.0393(19) -0.0081(19) -0.0097(19) F20 0.064(2) 0.051(2) 0.053(2) 0.0070(17) -0.0393(19) -0.0055(19) F21 0.106(3) 0.090(3) 0.047(2) 0.0043(19) -0.003(2) 0.074(3) F22 0.041(2) 0.136(3) 0.052(2) -0.014(2) 0.0290(19) -0.012(2) F23 0.108(3) 0.040(2) 0.049(2) -0.0135(16) 0.034(2) 0.009(2) F24 0.063(2) 0.057(2) 0.033(2) 0.0091(16) 0.0207(17) 0.0197(19) O1 0.205(7) 0.093(4) 0.088(5) 0.008(3) 0.033(5) 0.032(5) C72 0.131(8) 0.102(7) 0.073(6) 0.008(5) 0.020(6) 0.017(6) C73 0.315(15) 0.049(5) 0.051(6) 0.000(4) 0.024(7) 0.074(8) C74 0.162(11) 0.329(17) 0.121(10) 0.144(11) 0.064(8) 0.105(11) C75 0.145(10) 0.158(10) 0.103(8) -0.030(7) -0.058(7) 0.077(8) O2 0.119(6) 0.242(9) 0.174(8) -0.023(6) -0.087(6) 0.049(6) C76 0.064(7) 0.353(17) 0.136(10) -0.134(11) -0.006(7) 0.062(8) C77 0.058(5) 0.203(9) 0.056(5) 0.052(6) -0.003(4) -0.032(6) C78 0.083(6) 0.098(6) 0.060(5) 0.005(5) 0.020(5) 0.010(5) C79 0.142(9) 0.131(8) 0.074(7) 0.045(5) -0.013(7) -0.058(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N1 1.599(6) . ? B1 C34 1.633(7) . ? B1 C16 1.671(6) . ? B1 C25 1.683(7) . ? Fe1 N3 1.634(4) . ? Fe1 N2 1.943(4) . ? Fe1 P2 2.302(2) . ? Fe1 P1 2.387(2) . ? N1 C14 1.367(5) . ? N1 N2 1.392(4) . ? N2 C12 1.372(5) . ? N3 C1 1.456(6) . ? P1 C16 1.815(4) . ? P1 C21 1.897(5) . ? P1 C17 1.911(5) . ? P2 C25 1.811(4) . ? P2 C26 1.881(5) . ? P2 C30 1.912(5) . ? C1 C4 1.513(6) . ? C1 C2 1.521(7) . ? C1 C3 1.533(6) . ? C2 C7 1.555(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C5 1.545(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C9 1.550(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.497(8) . ? C5 C10 1.515(7) . ? C5 H5 1.0000 . ? C6 C7 1.488(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.497(10) . ? C7 H7 1.0000 . ? C8 C9 1.545(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.524(7) . ? C9 H9 1.0000 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.482(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.379(6) . ? C13 C14 1.396(6) . ? C13 H13 0.9500 . ? C14 C15 1.495(6) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.540(6) . ? C17 C19 1.540(6) . ? C17 C20 1.542(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.530(6) . ? C21 C24 1.535(6) . ? C21 C23 1.562(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.529(6) . ? C26 C29 1.535(6) . ? C26 C28 1.551(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C33 1.533(6) . ? C30 C31 1.541(6) . ? C30 C32 1.549(6) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.400(6) . ? C34 C39 1.405(6) . ? C35 C36 1.401(6) . ? C35 H35 0.9500 . ? C36 C37 1.366(6) . ? C36 H36 0.9500 . ? C37 C38 1.360(6) . ? C37 H37 0.9500 . ? C38 C39 1.385(6) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? B2 C48 1.629(6) . ? B2 C64 1.634(7) . ? B2 C56 1.635(6) . ? B2 C40 1.655(7) . ? C40 C45 1.380(6) . ? C40 C41 1.410(6) . ? C41 C42 1.403(6) . ? C41 H41 0.9500 . ? C42 C43 1.370(6) . ? C42 C46 1.474(7) . ? C43 C44 1.381(6) . ? C43 H43 0.9500 . ? C44 C45 1.412(6) . ? C44 C47 1.482(6) . ? C45 H45 0.9500 . ? C46 F1A 1.191(18) . ? C46 F3B 1.261(14) . ? C46 F2 1.319(6) . ? C46 F3A 1.47(2) . ? C46 F1B 1.53(3) . ? C47 F4 1.325(5) . ? C47 F6 1.343(5) . ? C47 F5 1.350(5) . ? C48 C53 1.402(6) . ? C48 C49 1.405(5) . ? C49 C50 1.393(6) . ? C49 H49 0.9500 . ? C50 C51 1.389(6) . ? C50 C54 1.507(6) . ? C51 C52 1.374(6) . ? C51 H51 0.9500 . ? C52 C53 1.398(6) . ? C52 C55 1.498(6) . ? C53 H53 0.9500 . ? C54 F8 1.309(5) . ? C54 F9 1.311(5) . ? C54 F7 1.319(6) . ? C55 F11 1.310(5) . ? C55 F12 1.329(5) . ? C55 F10 1.357(5) . ? C56 C57 1.406(5) . ? C56 C61 1.413(5) . ? C57 C58 1.379(5) . ? C57 H57 0.9500 . ? C58 C59 1.384(6) . ? C58 C62 1.504(6) . ? C59 C60 1.384(6) . ? C59 H59 0.9500 . ? C60 C61 1.383(5) . ? C60 C63 1.501(6) . ? C61 H61 0.9500 . ? C62 F15 1.316(5) . ? C62 F13 1.345(5) . ? C62 F14 1.352(5) . ? C63 F16 1.334(5) . ? C63 F17 1.356(5) . ? C63 F18 1.356(5) . ? C64 C69 1.389(6) . ? C64 C65 1.410(5) . ? C65 C66 1.392(6) . ? C65 H65 0.9500 . ? C66 C67 1.370(6) . ? C66 C71 1.502(6) . ? C67 C68 1.371(6) . ? C67 H67 0.9500 . ? C68 C69 1.406(6) . ? C68 C70 1.489(6) . ? C69 H69 0.9500 . ? C70 F19 1.322(5) . ? C70 F21 1.324(5) . ? C70 F20 1.328(5) . ? C71 F22 1.321(6) . ? C71 F24 1.331(6) . ? C71 F23 1.354(5) . ? O1 C75 1.432(7) . ? O1 C72 1.475(7) . ? C72 C73 1.483(8) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.659(12) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.466(9) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? O2 C79 1.380(9) . ? O2 C76 1.408(8) . ? C76 C77 1.389(9) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 C78 1.495(7) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C79 1.445(9) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 B1 C34 111.6(4) . . ? N1 B1 C16 102.6(4) . . ? C34 B1 C16 109.2(4) . . ? N1 B1 C25 110.3(4) . . ? C34 B1 C25 108.4(4) . . ? C16 B1 C25 114.6(4) . . ? N3 Fe1 N2 138.82(18) . . ? N3 Fe1 P2 110.70(14) . . ? N2 Fe1 P2 87.54(12) . . ? N3 Fe1 P1 114.13(14) . . ? N2 Fe1 P1 91.57(11) . . ? P2 Fe1 P1 110.07(8) . . ? C14 N1 N2 108.1(3) . . ? C14 N1 B1 134.1(4) . . ? N2 N1 B1 117.6(4) . . ? C12 N2 N1 108.0(4) . . ? C12 N2 Fe1 126.4(3) . . ? N1 N2 Fe1 125.5(3) . . ? C1 N3 Fe1 176.2(3) . . ? C16 P1 C21 108.2(2) . . ? C16 P1 C17 106.2(2) . . ? C21 P1 C17 109.5(2) . . ? C16 P1 Fe1 101.85(14) . . ? C21 P1 Fe1 107.50(16) . . ? C17 P1 Fe1 122.64(15) . . ? C25 P2 C26 109.8(2) . . ? C25 P2 C30 109.2(2) . . ? C26 P2 C30 109.0(2) . . ? C25 P2 Fe1 97.81(16) . . ? C26 P2 Fe1 117.52(16) . . ? C30 P2 Fe1 112.81(16) . . ? N3 C1 C4 114.5(4) . . ? N3 C1 C2 106.5(4) . . ? C4 C1 C2 110.1(5) . . ? N3 C1 C3 107.9(4) . . ? C4 C1 C3 109.1(4) . . ? C2 C1 C3 108.5(4) . . ? C1 C2 C7 107.9(5) . . ? C1 C2 H2A 110.1 . . ? C7 C2 H2A 110.1 . . ? C1 C2 H2B 110.1 . . ? C7 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? C1 C3 C5 109.2(4) . . ? C1 C3 H3A 109.8 . . ? C5 C3 H3A 109.8 . . ? C1 C3 H3B 109.8 . . ? C5 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? C1 C4 C9 109.8(4) . . ? C1 C4 H4A 109.7 . . ? C9 C4 H4A 109.7 . . ? C1 C4 H4B 109.7 . . ? C9 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C6 C5 C10 111.4(6) . . ? C6 C5 C3 109.8(5) . . ? C10 C5 C3 109.2(4) . . ? C6 C5 H5 108.8 . . ? C10 C5 H5 108.8 . . ? C3 C5 H5 108.8 . . ? C7 C6 C5 108.4(6) . . ? C7 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? C7 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? C6 C7 C8 111.6(7) . . ? C6 C7 C2 111.2(7) . . ? C8 C7 C2 109.5(8) . . ? C6 C7 H7 108.1 . . ? C8 C7 H7 108.1 . . ? C2 C7 H7 108.1 . . ? C7 C8 C9 108.2(6) . . ? C7 C8 H8A 110.1 . . ? C9 C8 H8A 110.1 . . ? C7 C8 H8B 110.1 . . ? C9 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? C10 C9 C8 110.4(5) . . ? C10 C9 C4 109.1(5) . . ? C8 C9 C4 108.4(5) . . ? C10 C9 H9 109.6 . . ? C8 C9 H9 109.6 . . ? C4 C9 H9 109.6 . . ? C5 C10 C9 108.3(5) . . ? C5 C10 H10A 110.0 . . ? C9 C10 H10A 110.0 . . ? C5 C10 H10B 110.0 . . ? C9 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C13 108.3(4) . . ? N2 C12 C11 122.6(4) . . ? C13 C12 C11 129.1(4) . . ? C12 C13 C14 107.7(4) . . ? C12 C13 H13 126.2 . . ? C14 C13 H13 126.2 . . ? N1 C14 C13 107.9(4) . . ? N1 C14 C15 124.9(4) . . ? C13 C14 C15 127.1(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? B1 C16 P1 119.5(3) . . ? B1 C16 H16A 107.4 . . ? P1 C16 H16A 107.4 . . ? B1 C16 H16B 107.4 . . ? P1 C16 H16B 107.4 . . ? H16A C16 H16B 107.0 . . ? C18 C17 C19 108.6(4) . . ? C18 C17 C20 110.8(4) . . ? C19 C17 C20 105.4(4) . . ? C18 C17 P1 109.6(3) . . ? C19 C17 P1 113.1(3) . . ? C20 C17 P1 109.3(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C24 106.4(4) . . ? C22 C21 C23 106.5(4) . . ? C24 C21 C23 109.7(4) . . ? C22 C21 P1 108.8(3) . . ? C24 C21 P1 114.2(3) . . ? C23 C21 P1 110.9(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? B1 C25 P2 122.1(3) . . ? B1 C25 H25A 106.8 . . ? P2 C25 H25A 106.8 . . ? B1 C25 H25B 106.8 . . ? P2 C25 H25B 106.8 . . ? H25A C25 H25B 106.6 . . ? C27 C26 C29 107.1(4) . . ? C27 C26 C28 106.4(4) . . ? C29 C26 C28 110.3(4) . . ? C27 C26 P2 109.2(3) . . ? C29 C26 P2 112.6(3) . . ? C28 C26 P2 111.0(3) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C33 C30 C31 108.5(4) . . ? C33 C30 C32 104.8(4) . . ? C31 C30 C32 110.4(4) . . ? C33 C30 P2 112.1(3) . . ? C31 C30 P2 109.1(3) . . ? C32 C30 P2 111.9(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C39 114.6(4) . . ? C35 C34 B1 122.6(4) . . ? C39 C34 B1 122.8(4) . . ? C34 C35 C36 122.1(5) . . ? C34 C35 H35 118.9 . . ? C36 C35 H35 118.9 . . ? C37 C36 C35 120.2(5) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C38 C37 C36 120.0(5) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 119.8(5) . . ? C37 C38 H38 120.1 . . ? C39 C38 H38 120.1 . . ? C38 C39 C34 123.3(5) . . ? C38 C39 H39 118.3 . . ? C34 C39 H39 118.3 . . ? C48 B2 C64 105.0(3) . . ? C48 B2 C56 110.5(4) . . ? C64 B2 C56 112.5(4) . . ? C48 B2 C40 114.1(4) . . ? C64 B2 C40 111.8(4) . . ? C56 B2 C40 103.1(3) . . ? C45 C40 C41 115.3(4) . . ? C45 C40 B2 123.3(4) . . ? C41 C40 B2 121.2(4) . . ? C42 C41 C40 122.2(4) . . ? C42 C41 H41 118.9 . . ? C40 C41 H41 118.9 . . ? C43 C42 C41 120.0(4) . . ? C43 C42 C46 122.1(5) . . ? C41 C42 C46 117.9(5) . . ? C42 C43 C44 120.1(4) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C45 118.7(4) . . ? C43 C44 C47 122.6(4) . . ? C45 C44 C47 118.6(4) . . ? C40 C45 C44 123.6(4) . . ? C40 C45 H45 118.2 . . ? C44 C45 H45 118.2 . . ? F1A C46 F3B 66.6(8) . . ? F1A C46 F2 115.1(14) . . ? F3B C46 F2 116.0(15) . . ? F1A C46 F3A 104.9(12) . . ? F3B C46 F3A 39.0(12) . . ? F2 C46 F3A 93.9(11) . . ? F1A C46 C42 118.5(10) . . ? F3B C46 C42 119.0(8) . . ? F2 C46 C42 113.8(5) . . ? F3A C46 C42 106.6(11) . . ? F1A C46 F1B 35.0(13) . . ? F3B C46 F1B 100.6(15) . . ? F2 C46 F1B 93.4(13) . . ? F3A C46 F1B 136.5(9) . . ? C42 C46 F1B 109.3(8) . . ? F4 C47 F6 106.6(4) . . ? F4 C47 F5 105.7(4) . . ? F6 C47 F5 104.9(4) . . ? F4 C47 C44 113.6(4) . . ? F6 C47 C44 112.6(4) . . ? F5 C47 C44 112.8(4) . . ? C53 C48 C49 114.4(4) . . ? C53 C48 B2 126.6(4) . . ? C49 C48 B2 118.8(4) . . ? C50 C49 C48 123.1(4) . . ? C50 C49 H49 118.5 . . ? C48 C49 H49 118.5 . . ? C51 C50 C49 120.9(4) . . ? C51 C50 C54 119.4(5) . . ? C49 C50 C54 119.7(4) . . ? C52 C51 C50 117.5(4) . . ? C52 C51 H51 121.2 . . ? C50 C51 H51 121.2 . . ? C51 C52 C53 121.5(5) . . ? C51 C52 C55 119.5(5) . . ? C53 C52 C55 119.0(5) . . ? C52 C53 C48 122.6(4) . . ? C52 C53 H53 118.7 . . ? C48 C53 H53 118.7 . . ? F8 C54 F9 107.0(5) . . ? F8 C54 F7 105.0(5) . . ? F9 C54 F7 104.6(5) . . ? F8 C54 C50 112.4(4) . . ? F9 C54 C50 113.6(5) . . ? F7 C54 C50 113.6(4) . . ? F11 C55 F12 108.1(4) . . ? F11 C55 F10 104.9(4) . . ? F12 C55 F10 103.7(4) . . ? F11 C55 C52 113.4(4) . . ? F12 C55 C52 113.9(4) . . ? F10 C55 C52 112.0(4) . . ? C57 C56 C61 113.9(4) . . ? C57 C56 B2 124.3(4) . . ? C61 C56 B2 121.6(4) . . ? C58 C57 C56 123.5(4) . . ? C58 C57 H57 118.3 . . ? C56 C57 H57 118.3 . . ? C57 C58 C59 121.0(4) . . ? C57 C58 C62 119.7(4) . . ? C59 C58 C62 119.3(4) . . ? C58 C59 C60 117.7(4) . . ? C58 C59 H59 121.2 . . ? C60 C59 H59 121.2 . . ? C61 C60 C59 121.2(4) . . ? C61 C60 C63 119.3(4) . . ? C59 C60 C63 119.5(4) . . ? C60 C61 C56 122.8(4) . . ? C60 C61 H61 118.6 . . ? C56 C61 H61 118.6 . . ? F15 C62 F13 107.5(4) . . ? F15 C62 F14 106.4(4) . . ? F13 C62 F14 104.6(4) . . ? F15 C62 C58 114.1(4) . . ? F13 C62 C58 112.4(4) . . ? F14 C62 C58 111.4(4) . . ? F16 C63 F17 106.6(4) . . ? F16 C63 F18 106.2(4) . . ? F17 C63 F18 105.3(4) . . ? F16 C63 C60 113.5(4) . . ? F17 C63 C60 112.7(4) . . ? F18 C63 C60 112.0(4) . . ? C69 C64 C65 114.2(4) . . ? C69 C64 B2 122.4(4) . . ? C65 C64 B2 123.0(4) . . ? C66 C65 C64 123.0(4) . . ? C66 C65 H65 118.5 . . ? C64 C65 H65 118.5 . . ? C67 C66 C65 119.9(4) . . ? C67 C66 C71 118.8(5) . . ? C65 C66 C71 121.3(4) . . ? C66 C67 C68 120.0(4) . . ? C66 C67 H67 120.0 . . ? C68 C67 H67 120.0 . . ? C67 C68 C69 119.1(4) . . ? C67 C68 C70 121.9(5) . . ? C69 C68 C70 118.9(4) . . ? C64 C69 C68 123.7(4) . . ? C64 C69 H69 118.2 . . ? C68 C69 H69 118.2 . . ? F19 C70 F21 106.7(5) . . ? F19 C70 F20 104.0(4) . . ? F21 C70 F20 106.4(4) . . ? F19 C70 C68 113.9(4) . . ? F21 C70 C68 113.1(4) . . ? F20 C70 C68 112.0(4) . . ? F22 C71 F24 106.5(4) . . ? F22 C71 F23 105.9(4) . . ? F24 C71 F23 105.2(4) . . ? F22 C71 C66 113.1(5) . . ? F24 C71 C66 114.3(4) . . ? F23 C71 C66 111.0(4) . . ? C75 O1 C72 101.0(7) . . ? O1 C72 C73 106.5(7) . . ? O1 C72 H72A 110.4 . . ? C73 C72 H72A 110.4 . . ? O1 C72 H72B 110.4 . . ? C73 C72 H72B 110.4 . . ? H72A C72 H72B 108.6 . . ? C72 C73 C74 100.7(7) . . ? C72 C73 H73A 111.6 . . ? C74 C73 H73A 111.6 . . ? C72 C73 H73B 111.6 . . ? C74 C73 H73B 111.6 . . ? H73A C73 H73B 109.4 . . ? C75 C74 C73 98.8(8) . . ? C75 C74 H74A 112.0 . . ? C73 C74 H74A 112.0 . . ? C75 C74 H74B 112.0 . . ? C73 C74 H74B 112.0 . . ? H74A C74 H74B 109.7 . . ? O1 C75 C74 115.9(9) . . ? O1 C75 H75A 108.3 . . ? C74 C75 H75A 108.3 . . ? O1 C75 H75B 108.3 . . ? C74 C75 H75B 108.3 . . ? H75A C75 H75B 107.4 . . ? C79 O2 C76 102.5(7) . . ? C77 C76 O2 106.4(7) . . ? C77 C76 H76A 110.5 . . ? O2 C76 H76A 110.5 . . ? C77 C76 H76B 110.5 . . ? O2 C76 H76B 110.5 . . ? H76A C76 H76B 108.6 . . ? C76 C77 C78 105.0(6) . . ? C76 C77 H77A 110.7 . . ? C78 C77 H77A 110.7 . . ? C76 C77 H77B 110.7 . . ? C78 C77 H77B 110.7 . . ? H77A C77 H77B 108.8 . . ? C79 C78 C77 102.3(6) . . ? C79 C78 H78A 111.3 . . ? C77 C78 H78A 111.3 . . ? C79 C78 H78B 111.3 . . ? C77 C78 H78B 111.3 . . ? H78A C78 H78B 109.2 . . ? O2 C79 C78 108.4(7) . . ? O2 C79 H79A 110.0 . . ? C78 C79 H79A 110.0 . . ? O2 C79 H79B 110.0 . . ? C78 C79 H79B 110.0 . . ? H79A C79 H79B 108.4 . . ? _diffrn_measured_fraction_theta_max 0.886 _diffrn_reflns_theta_full 25.74 _diffrn_measured_fraction_theta_full 0.886 _refine_diff_density_max 0.710 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.082 #===END