data_publication_text _publ_contact_author_name 'Jonas C. Peters' _publ_contact_author_address ;Caltech Division of Chemistry and Chemical Engineering 1200 E. California Blvd. Pasadena, CA 91125 ; _publ_contact_author_email jpeters@caltech.edu _publ_contact_author_phone 626-395-3113 loop_ _publ_author_name _publ_author_address 'Peters, Jonas C.' ;Caltech Division of Chemistry and Chemical Engineering 1200 E. California Blvd. Pasadena, CA 91125 ; 'Suess, Daniel L. M.' ;Caltech Division of Chemistry and Chemical Engineering 1200 E. California Blvd. Pasadena, CA 91125 ; ####################################################### # Compound 3a: (iPrDPBPh)FeBr # ####################################################### data_3a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H41 B Br Fe P2' _chemical_formula_weight 610.14 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' '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' 'Br' 'Br' -0.2901 2.4595 '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, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.921(3) _cell_length_b 9.9768(12) _cell_length_c 31.705(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.872(8) _cell_angle_gamma 90.00 _cell_volume 5784.4(13) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9456 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 41.66 _exptl_crystal_description chunk _exptl_crystal_colour red _exptl_crystal_size_max 0.388 _exptl_crystal_size_mid 0.312 _exptl_crystal_size_min 0.298 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2536 _exptl_absorpt_coefficient_mu 2.031 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; 'Bruker KAPPA APEX II' ; _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 130537 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -59 _diffrn_reflns_limit_l_max 62 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 44.08 _reflns_number_total 22550 _reflns_number_gt 16686 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0418P)^2^+5.3349P] 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 22550 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1012 _refine_ls_wR_factor_gt 0.0929 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.636322(8) 0.278912(14) 0.606435(4) 0.00984(2) Uani 1 1 d . . . Br1 Br 0.582959(7) 0.494059(11) 0.586543(4) 0.02057(3) Uani 1 1 d . . . P2 P 0.615029(14) 0.21735(3) 0.674603(8) 0.01054(4) Uani 1 1 d . . . P1 P 0.765032(14) 0.26489(3) 0.615148(8) 0.01072(4) Uani 1 1 d . . . C8 C 0.72644(6) 0.01626(10) 0.58419(3) 0.01250(14) Uani 1 1 d . . . C7 C 0.78034(5) 0.11533(10) 0.58609(3) 0.01268(14) Uani 1 1 d . . . C16 C 0.83273(5) 0.23891(11) 0.66912(3) 0.01349(15) Uani 1 1 d . . . H16 H 0.8188 0.2996 0.6908 0.016 Uiso 1 1 calc R . . C1 C 0.58721(5) 0.10337(9) 0.56383(3) 0.01136(13) Uani 1 1 d . . . C28 C 0.52781(6) 0.26559(11) 0.68780(3) 0.01461(15) Uani 1 1 d . . . H28 H 0.5266 0.2216 0.7159 0.018 Uiso 1 1 calc R . . C25 C 0.68791(6) 0.26866(10) 0.72391(3) 0.01300(14) Uani 1 1 d . . . H25 H 0.7317 0.2127 0.7237 0.016 Uiso 1 1 calc R . . C27 C 0.71102(6) 0.41520(11) 0.72001(4) 0.01628(17) Uani 1 1 d . . . H27A H 0.6732 0.4754 0.7252 0.024 Uiso 1 1 calc R . . H27B H 0.7173 0.4308 0.6907 0.024 Uiso 1 1 calc R . . H27C H 0.7573 0.4327 0.7417 0.024 Uiso 1 1 calc R . . C19 C 0.61467(5) 0.03407(10) 0.67502(3) 0.01190(14) Uani 1 1 d . . . C6 C 0.51351(6) 0.08189(12) 0.56504(4) 0.01648(17) Uani 1 1 d . . . C20 C 0.63724(5) -0.03014(9) 0.64071(3) 0.01175(14) Uani 1 1 d . . . C2 C 0.59770(6) 0.18466(11) 0.52920(3) 0.01524(16) Uani 1 1 d . . . C4 C 0.46768(6) 0.21405(13) 0.49996(4) 0.01961(19) Uani 1 1 d . . . C30 C 0.46196(6) 0.21578(14) 0.65236(4) 0.0221(2) Uani 1 1 d . . . H30A H 0.4168 0.2391 0.6603 0.033 Uiso 1 1 calc R . . H30B H 0.4649 0.1182 0.6496 0.033 Uiso 1 1 calc R . . H30C H 0.4620 0.2581 0.6245 0.033 Uiso 1 1 calc R . . C13 C 0.80261(6) 0.40906(11) 0.59109(3) 0.01604(17) Uani 1 1 d . . . H13 H 0.8554 0.3918 0.5929 0.019 Uiso 1 1 calc R . . C29 C 0.52161(6) 0.41765(12) 0.69336(4) 0.01928(19) Uani 1 1 d . . . H29A H 0.5264 0.4632 0.6669 0.029 Uiso 1 1 calc R . . H29B H 0.5605 0.4479 0.7183 0.029 Uiso 1 1 calc R . . H29C H 0.4739 0.4389 0.6984 0.029 Uiso 1 1 calc R . . B1 B 0.65435(6) 0.04995(11) 0.60052(3) 0.01148(15) Uani 1 1 d . . . C26 C 0.67145(7) 0.24331(12) 0.76819(3) 0.01872(18) Uani 1 1 d . . . H26A H 0.7141 0.2683 0.7917 0.028 Uiso 1 1 calc R . . H26B H 0.6605 0.1481 0.7708 0.028 Uiso 1 1 calc R . . H26C H 0.6293 0.2974 0.7704 0.028 Uiso 1 1 calc R . . C18 C 0.82785(6) 0.09372(11) 0.68456(3) 0.01606(16) Uani 1 1 d . . . H18A H 0.8465 0.0325 0.6658 0.024 Uiso 1 1 calc R . . H18B H 0.7768 0.0717 0.6830 0.024 Uiso 1 1 calc R . . H18C H 0.8572 0.0846 0.7148 0.024 Uiso 1 1 calc R . . C24 C 0.59404(6) -0.04125(11) 0.70746(3) 0.01556(16) Uani 1 1 d . . . H24 H 0.5776 0.0033 0.7297 0.019 Uiso 1 1 calc R . . C3 C 0.53893(7) 0.24070(13) 0.49821(4) 0.01966(19) Uani 1 1 d . . . C21 C 0.63998(6) -0.17138(10) 0.64170(4) 0.01667(17) Uani 1 1 d . . . H21 H 0.6557 -0.2174 0.6195 0.020 Uiso 1 1 calc R . . C23 C 0.59752(6) -0.18079(11) 0.70717(4) 0.01732(18) Uani 1 1 d . . . H23 H 0.5844 -0.2313 0.7294 0.021 Uiso 1 1 calc R . . C10 C 0.80039(7) -0.13237(12) 0.55106(4) 0.01914(19) Uani 1 1 d . . . H10 H 0.8069 -0.2175 0.5392 0.023 Uiso 1 1 calc R . . C12 C 0.84284(6) 0.09170(12) 0.57085(4) 0.01722(17) Uani 1 1 d . . . H12 H 0.8779 0.1608 0.5723 0.021 Uiso 1 1 calc R . . C17 C 0.91237(6) 0.26980(14) 0.66956(4) 0.0211(2) Uani 1 1 d . . . H17A H 0.9442 0.2492 0.6984 0.032 Uiso 1 1 calc R . . H17B H 0.9170 0.3649 0.6630 0.032 Uiso 1 1 calc R . . H17C H 0.9268 0.2150 0.6475 0.032 Uiso 1 1 calc R . . C9 C 0.73796(6) -0.10815(11) 0.56576(4) 0.01631(17) Uani 1 1 d . . . H9 H 0.7024 -0.1770 0.5633 0.020 Uiso 1 1 calc R . . C11 C 0.85319(7) -0.03299(13) 0.55359(4) 0.01973(19) Uani 1 1 d . . . H11 H 0.8956 -0.0501 0.5437 0.024 Uiso 1 1 calc R . . C22 C 0.62038(7) -0.24562(11) 0.67419(4) 0.01844(18) Uani 1 1 d . . . H22 H 0.6227 -0.3407 0.6738 0.022 Uiso 1 1 calc R . . C15 C 0.76138(7) 0.42653(13) 0.54317(4) 0.0214(2) Uani 1 1 d . . . H15A H 0.7093 0.4409 0.5410 0.032 Uiso 1 1 calc R . . H15B H 0.7673 0.3458 0.5268 0.032 Uiso 1 1 calc R . . H15C H 0.7811 0.5041 0.5310 0.032 Uiso 1 1 calc R . . C5 C 0.45525(6) 0.13304(13) 0.53313(4) 0.01992(19) Uani 1 1 d . . . C14 C 0.79632(7) 0.53616(12) 0.61724(4) 0.0215(2) Uani 1 1 d . . . H14A H 0.8164 0.6127 0.6048 0.032 Uiso 1 1 calc R . . H14B H 0.8238 0.5238 0.6477 0.032 Uiso 1 1 calc R . . H14C H 0.7448 0.5531 0.6159 0.032 Uiso 1 1 calc R . . H2 H 0.6448(10) 0.1951(19) 0.5267(6) 0.022(4) Uiso 1 1 d . . . H5 H 0.4034(11) 0.115(2) 0.5333(7) 0.033(5) Uiso 1 1 d . . . H3 H 0.5466(10) 0.2979(19) 0.4754(6) 0.025(5) Uiso 1 1 d . . . H4 H 0.4302(11) 0.2516(19) 0.4790(6) 0.024(5) Uiso 1 1 d . . . H6 H 0.5058(11) 0.028(2) 0.5868(7) 0.027(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.00967(5) 0.00819(5) 0.01115(5) -0.00001(4) 0.00173(4) 0.00039(4) Br1 0.02676(6) 0.01289(5) 0.02089(5) 0.00262(3) 0.00394(4) 0.00636(4) P2 0.00966(9) 0.00982(9) 0.01233(9) 0.00002(7) 0.00318(7) 0.00021(7) P1 0.00997(9) 0.01087(9) 0.01121(8) 0.00090(7) 0.00249(7) -0.00105(7) C8 0.0124(4) 0.0112(3) 0.0137(3) 0.0001(3) 0.0030(3) 0.0021(3) C7 0.0116(4) 0.0140(4) 0.0128(3) 0.0007(3) 0.0040(3) 0.0004(3) C16 0.0106(3) 0.0164(4) 0.0128(3) 0.0013(3) 0.0017(3) -0.0004(3) C1 0.0105(3) 0.0106(3) 0.0125(3) -0.0020(3) 0.0021(3) -0.0003(3) C28 0.0115(4) 0.0162(4) 0.0170(4) -0.0009(3) 0.0053(3) 0.0004(3) C25 0.0120(3) 0.0125(4) 0.0140(3) -0.0010(3) 0.0026(3) 0.0012(3) C27 0.0145(4) 0.0145(4) 0.0189(4) -0.0034(3) 0.0027(3) -0.0020(3) C19 0.0110(3) 0.0104(3) 0.0141(3) 0.0016(3) 0.0029(3) -0.0009(3) C6 0.0123(4) 0.0188(4) 0.0182(4) 0.0013(3) 0.0038(3) 0.0006(3) C20 0.0110(3) 0.0093(3) 0.0145(3) 0.0010(3) 0.0023(3) 0.0000(3) C2 0.0132(4) 0.0174(4) 0.0142(3) 0.0019(3) 0.0018(3) -0.0010(3) C4 0.0156(4) 0.0226(5) 0.0176(4) 0.0001(4) -0.0013(3) 0.0030(4) C30 0.0112(4) 0.0274(6) 0.0273(5) -0.0076(4) 0.0041(4) -0.0014(4) C13 0.0148(4) 0.0168(4) 0.0160(4) 0.0034(3) 0.0029(3) -0.0044(3) C29 0.0141(4) 0.0186(4) 0.0260(5) -0.0031(4) 0.0069(4) 0.0042(3) B1 0.0111(4) 0.0102(4) 0.0129(4) -0.0006(3) 0.0026(3) 0.0007(3) C26 0.0201(5) 0.0217(5) 0.0137(4) -0.0001(3) 0.0031(3) 0.0009(4) C18 0.0142(4) 0.0174(4) 0.0156(4) 0.0042(3) 0.0021(3) 0.0027(3) C24 0.0153(4) 0.0153(4) 0.0163(4) 0.0028(3) 0.0045(3) -0.0023(3) C3 0.0181(4) 0.0232(5) 0.0154(4) 0.0044(3) 0.0001(3) -0.0005(4) C21 0.0201(5) 0.0099(3) 0.0206(4) 0.0012(3) 0.0063(3) 0.0003(3) C23 0.0159(4) 0.0157(4) 0.0194(4) 0.0061(3) 0.0027(3) -0.0030(3) C10 0.0212(5) 0.0178(4) 0.0196(4) 0.0000(3) 0.0074(4) 0.0077(4) C12 0.0136(4) 0.0221(5) 0.0176(4) -0.0005(3) 0.0071(3) 0.0003(3) C17 0.0116(4) 0.0305(6) 0.0200(4) 0.0038(4) 0.0019(3) -0.0038(4) C9 0.0173(4) 0.0133(4) 0.0188(4) -0.0011(3) 0.0055(3) 0.0024(3) C11 0.0174(4) 0.0244(5) 0.0192(4) -0.0002(4) 0.0080(3) 0.0064(4) C22 0.0206(5) 0.0103(4) 0.0231(4) 0.0044(3) 0.0032(4) -0.0009(3) C15 0.0230(5) 0.0247(5) 0.0157(4) 0.0060(4) 0.0037(4) -0.0055(4) C5 0.0104(4) 0.0258(5) 0.0222(4) 0.0002(4) 0.0018(3) 0.0019(4) C14 0.0231(5) 0.0148(4) 0.0240(5) 0.0008(4) 0.0016(4) -0.0070(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 2.2608(9) . ? Fe1 B1 2.3243(11) . ? Fe1 P2 2.3785(4) . ? Fe1 P1 2.3835(5) . ? Fe1 Br1 2.3870(3) . ? Fe1 C2 2.5486(11) . ? Fe1 C6 3.0692(12) . ? P2 C19 1.8286(10) . ? P2 C28 1.8666(11) . ? P2 C25 1.8711(10) . ? P1 C7 1.8155(10) . ? P1 C13 1.8532(11) . ? P1 C16 1.8737(10) . ? C8 C7 1.4105(14) . ? C8 C9 1.4124(14) . ? C8 B1 1.6136(15) . ? C7 C12 1.4074(15) . ? C16 C17 1.5346(15) . ? C16 C18 1.5395(15) . ? C16 H16 1.0000 . ? C1 C2 1.4191(14) . ? C1 C6 1.4212(15) . ? C1 B1 1.5789(14) . ? C28 C30 1.5307(16) . ? C28 C29 1.5353(16) . ? C28 H28 1.0000 . ? C25 C26 1.5349(15) . ? C25 C27 1.5400(15) . ? C25 H25 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C19 C24 1.4073(14) . ? C19 C20 1.4195(14) . ? C6 C5 1.3880(16) . ? C6 H6 0.92(2) . ? C20 C21 1.4101(14) . ? C20 B1 1.6057(15) . ? C2 C3 1.3977(15) . ? C2 H2 0.921(19) . ? C4 C3 1.3891(18) . ? C4 C5 1.3935(18) . ? C4 H4 0.918(19) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C13 C15 1.5292(15) . ? C13 C14 1.5363(17) . ? C13 H13 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C24 C23 1.3939(16) . ? C24 H24 0.9500 . ? C3 H3 0.962(19) . ? C21 C22 1.3939(16) . ? C21 H21 0.9500 . ? C23 C22 1.3896(18) . ? C23 H23 0.9500 . ? C10 C11 1.3952(19) . ? C10 C9 1.3976(16) . ? C10 H10 0.9500 . ? C12 C11 1.3930(17) . ? C12 H12 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C9 H9 0.9500 . ? C11 H11 0.9500 . ? C22 H22 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C5 H5 1.00(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 B1 40.25(4) . . ? C1 Fe1 P2 101.74(3) . . ? B1 Fe1 P2 83.23(3) . . ? C1 Fe1 P1 105.95(3) . . ? B1 Fe1 P1 77.58(3) . . ? P2 Fe1 P1 106.609(12) . . ? C1 Fe1 Br1 117.23(3) . . ? B1 Fe1 Br1 157.42(3) . . ? P2 Fe1 Br1 108.270(9) . . ? P1 Fe1 Br1 115.703(10) . . ? C1 Fe1 C2 33.65(3) . . ? B1 Fe1 C2 64.64(4) . . ? P2 Fe1 C2 134.75(3) . . ? P1 Fe1 C2 97.02(3) . . ? Br1 Fe1 C2 94.61(3) . . ? C1 Fe1 C6 25.64(3) . . ? B1 Fe1 C6 56.41(4) . . ? P2 Fe1 C6 86.38(2) . . ? P1 Fe1 C6 130.61(2) . . ? Br1 Fe1 C6 103.91(2) . . ? C2 Fe1 C6 49.76(3) . . ? C19 P2 C28 104.54(5) . . ? C19 P2 C25 105.72(4) . . ? C28 P2 C25 104.27(5) . . ? C19 P2 Fe1 105.47(3) . . ? C28 P2 Fe1 120.18(4) . . ? C25 P2 Fe1 115.35(4) . . ? C7 P1 C13 107.52(5) . . ? C7 P1 C16 100.89(5) . . ? C13 P1 C16 103.81(5) . . ? C7 P1 Fe1 106.31(3) . . ? C13 P1 Fe1 113.28(4) . . ? C16 P1 Fe1 123.55(3) . . ? C7 C8 C9 116.53(9) . . ? C7 C8 B1 120.12(9) . . ? C9 C8 B1 123.28(9) . . ? C12 C7 C8 122.01(10) . . ? C12 C7 P1 124.72(8) . . ? C8 C7 P1 112.94(7) . . ? C17 C16 C18 108.96(9) . . ? C17 C16 P1 114.84(7) . . ? C18 C16 P1 109.75(7) . . ? C17 C16 H16 107.7 . . ? C18 C16 H16 107.7 . . ? P1 C16 H16 107.7 . . ? C2 C1 C6 116.12(9) . . ? C2 C1 B1 121.14(9) . . ? C6 C1 B1 122.59(9) . . ? C2 C1 Fe1 84.37(6) . . ? C6 C1 Fe1 110.87(7) . . ? B1 C1 Fe1 72.04(5) . . ? C30 C28 C29 109.47(9) . . ? C30 C28 P2 110.59(8) . . ? C29 C28 P2 112.25(7) . . ? C30 C28 H28 108.1 . . ? C29 C28 H28 108.1 . . ? P2 C28 H28 108.1 . . ? C26 C25 C27 111.00(9) . . ? C26 C25 P2 116.11(8) . . ? C27 C25 P2 110.87(7) . . ? C26 C25 H25 106.0 . . ? C27 C25 H25 106.0 . . ? P2 C25 H25 106.0 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C19 C20 120.90(9) . . ? C24 C19 P2 122.79(8) . . ? C20 C19 P2 116.31(7) . . ? C5 C6 C1 121.73(10) . . ? C5 C6 Fe1 116.66(8) . . ? C1 C6 Fe1 43.49(5) . . ? C5 C6 H6 120.9(13) . . ? C1 C6 H6 117.2(13) . . ? Fe1 C6 H6 107.6(13) . . ? C21 C20 C19 116.77(9) . . ? C21 C20 B1 120.09(9) . . ? C19 C20 B1 123.04(8) . . ? C3 C2 C1 121.90(10) . . ? C3 C2 Fe1 120.53(8) . . ? C1 C2 Fe1 61.98(5) . . ? C3 C2 H2 120.4(12) . . ? C1 C2 H2 117.5(12) . . ? Fe1 C2 H2 89.8(12) . . ? C3 C4 C5 119.64(10) . . ? C3 C4 H4 118.2(12) . . ? C5 C4 H4 122.2(12) . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C15 C13 C14 110.59(10) . . ? C15 C13 P1 110.22(8) . . ? C14 C13 P1 109.11(8) . . ? C15 C13 H13 109.0 . . ? C14 C13 H13 109.0 . . ? P1 C13 H13 109.0 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C1 B1 C20 117.69(9) . . ? C1 B1 C8 114.86(8) . . ? C20 B1 C8 120.67(8) . . ? C1 B1 Fe1 67.71(5) . . ? C20 B1 Fe1 111.19(6) . . ? C8 B1 Fe1 112.60(7) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C23 C24 C19 120.41(10) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? C4 C3 C2 120.04(11) . . ? C4 C3 H3 118.7(12) . . ? C2 C3 H3 121.3(12) . . ? C22 C21 C20 122.16(10) . . ? C22 C21 H21 118.9 . . ? C20 C21 H21 118.9 . . ? C22 C23 C24 119.61(10) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C11 C10 C9 120.80(10) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C11 C12 C7 119.99(11) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C10 C9 C8 121.56(11) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C12 C11 C10 119.09(10) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C23 C22 C21 120.13(10) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? 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 . . ? C6 C5 C4 120.47(11) . . ? C6 C5 H5 121.7(12) . . ? C4 C5 H5 117.8(12) . . ? 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 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 44.08 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.987 _refine_diff_density_min -1.739 _refine_diff_density_rms 0.101 ####################################################### # Compound 6a: (iPrDPBPh)FeNNSi2 # ####################################################### data_6a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H57 B Fe N2 P2 Si2' _chemical_formula_weight 702.62 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' 'Si' 'Si' 0.0817 0.0704 '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 10.5707(8) _cell_length_b 19.9433(14) _cell_length_c 20.5612(15) _cell_angle_alpha 118.196(3) _cell_angle_beta 97.760(4) _cell_angle_gamma 92.754(3) _cell_volume 3754.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9484 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 49.60 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 0.578 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8102 _exptl_absorpt_correction_T_max 0.8411 _exptl_absorpt_process_details 'SADABS v2008/1 (Bruker-AXS, 2008)' _exptl_special_details ; 'Bruker KAPPA APEX II' ; _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 501556 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 50.11 _reflns_number_total 77845 _reflns_number_gt 55692 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0377P)^2^+0.6849P] 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 77845 _refine_ls_number_parameters 857 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0690 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0937 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 Fe1 Fe 0.930326(7) 0.694711(4) 0.261510(4) 0.00714(1) Uani 1 1 d . . . Fe2 Fe 0.530606(8) 0.822848(4) 0.758980(4) 0.00883(1) Uani 1 1 d . . . P1 P 0.953568(13) 0.795428(8) 0.376239(8) 0.00803(2) Uani 1 1 d . . . P11 P 0.503247(14) 0.725587(8) 0.639670(8) 0.00969(2) Uani 1 1 d . . . P2 P 0.941127(14) 0.585912(8) 0.270138(8) 0.00892(2) Uani 1 1 d . . . P12 P 0.551430(15) 0.768157(9) 0.831920(9) 0.01110(2) Uani 1 1 d . . . Si11 Si 0.707334(18) 1.014276(10) 0.752372(11) 0.01409(3) Uani 1 1 d . . . Si12 Si 0.908735(18) 0.944301(11) 0.804254(12) 0.01660(3) Uani 1 1 d . . . Si1 Si 0.525221(17) 0.670121(11) 0.167166(10) 0.01307(3) Uani 1 1 d . . . Si2 Si 0.702867(17) 0.660446(11) 0.064501(10) 0.01263(3) Uani 1 1 d . . . N11 N 0.65012(5) 0.88535(3) 0.76700(3) 0.01072(6) Uani 1 1 d . . . N1 N 0.79426(4) 0.68301(3) 0.20433(3) 0.00934(6) Uani 1 1 d . . . N2 N 0.68972(5) 0.67243(3) 0.15510(3) 0.01185(7) Uani 1 1 d . . . C119 C 0.40629(6) 0.76590(4) 0.86942(3) 0.01372(8) Uani 1 1 d . . . C8 C 1.20375(5) 0.79820(3) 0.37463(3) 0.00926(7) Uani 1 1 d . . . C7 C 1.11278(5) 0.84886(3) 0.40311(3) 0.00987(7) Uani 1 1 d . . . C13 C 0.94368(5) 0.79117(3) 0.46502(3) 0.01156(8) Uani 1 1 d . . . H13 H 0.8666 0.7541 0.4545 0.014 Uiso 1 1 calc R . . C3 C 1.05717(6) 0.75309(3) 0.15142(3) 0.01459(9) Uani 1 1 d . . . C1 C 1.11863(5) 0.69652(3) 0.23344(3) 0.00897(7) Uani 1 1 d . . . N12 N 0.73958(5) 0.93656(3) 0.77090(3) 0.01295(7) Uani 1 1 d . . . C107 C 0.33879(6) 0.67557(3) 0.60678(3) 0.01253(8) Uani 1 1 d . . . C9 C 1.33303(5) 0.83007(3) 0.39268(3) 0.01201(8) Uani 1 1 d . . . H9 H 1.3970 0.7974 0.3745 0.014 Uiso 1 1 calc R . . C19 C 1.10654(5) 0.57346(3) 0.29628(3) 0.01054(7) Uani 1 1 d . . . C20 C 1.19373(5) 0.64087(3) 0.32615(3) 0.00948(7) Uani 1 1 d . . . C6 C 1.14004(5) 0.63021(3) 0.16763(3) 0.01128(7) Uani 1 1 d . . . C21 C 1.31946(5) 0.63977(3) 0.35781(3) 0.01146(7) Uani 1 1 d . . . H21 H 1.3784 0.6856 0.3818 0.014 Uiso 1 1 calc R . . C5 C 1.12568(6) 0.62716(4) 0.09907(3) 0.01388(8) Uani 1 1 d . . . C16 C 0.83831(5) 0.86460(3) 0.38134(3) 0.01186(8) Uani 1 1 d . . . H16 H 0.8631 0.9120 0.4311 0.014 Uiso 1 1 calc R . . C12 C 1.14831(6) 0.92803(3) 0.44637(4) 0.01419(9) Uani 1 1 d . . . H12 H 1.0847 0.9612 0.4642 0.017 Uiso 1 1 calc R . . C120 C 0.29660(6) 0.75378(3) 0.81637(3) 0.01330(8) Uani 1 1 d . . . C25 C 0.87458(6) 0.49067(3) 0.18782(3) 0.01331(8) Uani 1 1 d . . . H25 H 0.8799 0.4515 0.2051 0.016 Uiso 1 1 calc R . . B1 B 1.15054(6) 0.71052(3) 0.31541(3) 0.00943(8) Uani 1 1 d . . . C116 C 0.52389(6) 0.74856(3) 0.56338(3) 0.01350(8) Uani 1 1 d . . . H116 H 0.5108 0.6990 0.5153 0.016 Uiso 1 1 calc R . . C113 C 0.60968(6) 0.64775(3) 0.62116(4) 0.01369(8) Uani 1 1 d . . . H113 H 0.5753 0.6166 0.6428 0.016 Uiso 1 1 calc R . . C22 C 1.35952(6) 0.57316(4) 0.35476(3) 0.01403(8) Uani 1 1 d . . . H22 H 1.4455 0.5736 0.3758 0.017 Uiso 1 1 calc R . . C28 C 0.86767(6) 0.58521(3) 0.34802(3) 0.01234(8) Uani 1 1 d . . . H28 H 0.9251 0.6240 0.3954 0.015 Uiso 1 1 calc R . . C15 C 1.06223(6) 0.76139(4) 0.48903(3) 0.01512(9) Uani 1 1 d . . . H15A H 1.1356 0.8020 0.5112 0.023 Uiso 1 1 calc R . . H15B H 1.0825 0.7170 0.4451 0.023 Uiso 1 1 calc R . . H15C H 1.0443 0.7462 0.5261 0.023 Uiso 1 1 calc R . . C110 C 0.08270(7) 0.60919(4) 0.56421(4) 0.01984(11) Uani 1 1 d . . . H110 H -0.0046 0.5867 0.5501 0.024 Uiso 1 1 calc R . . C128 C 0.58075(6) 0.66544(4) 0.79782(4) 0.01418(9) Uani 1 1 d . . . H128 H 0.6489 0.6554 0.7662 0.017 Uiso 1 1 calc R . . C109 C 0.13195(6) 0.66216(4) 0.63851(4) 0.01708(10) Uani 1 1 d . . . H109 H 0.0772 0.6751 0.6747 0.020 Uiso 1 1 calc R . . C101 C 0.33467(6) 0.84612(3) 0.75860(3) 0.01266(8) Uani 1 1 d . . . C2 C 1.07173(5) 0.75716(3) 0.22311(3) 0.01103(7) Uani 1 1 d . . . C11 C 1.27712(6) 0.95807(3) 0.46324(4) 0.01728(10) Uani 1 1 d . . . H11 H 1.3022 1.0118 0.4926 0.021 Uiso 1 1 calc R . . C23 C 1.27392(6) 0.50581(4) 0.32091(4) 0.01575(9) Uani 1 1 d . . . H23 H 1.3019 0.4599 0.3176 0.019 Uiso 1 1 calc R . . C106 C 0.27738(6) 0.86978(4) 0.70653(4) 0.01618(10) Uani 1 1 d . . . C108 C 0.26055(5) 0.69723(3) 0.66188(3) 0.01216(8) Uani 1 1 d . . . C4 C 1.08571(7) 0.69020(4) 0.09103(3) 0.01616(9) Uani 1 1 d . . . C18 C 0.70254(6) 0.83027(4) 0.37621(4) 0.01600(9) Uani 1 1 d . . . H18A H 0.6418 0.8665 0.3782 0.024 Uiso 1 1 calc R . . H18B H 0.7006 0.8201 0.4183 0.024 Uiso 1 1 calc R . . H18C H 0.6781 0.7822 0.3288 0.024 Uiso 1 1 calc R . . C121 C 0.17659(7) 0.73994(4) 0.83302(4) 0.01901(11) Uani 1 1 d . . . H121 H 0.1005 0.7307 0.7981 0.023 Uiso 1 1 calc R . . C102 C 0.40595(7) 0.90454(4) 0.82878(4) 0.01563(9) Uani 1 1 d . . . C30 C 0.86215(7) 0.51040(4) 0.35191(4) 0.01788(10) Uani 1 1 d . . . H30A H 0.8334 0.5188 0.3982 0.027 Uiso 1 1 calc R . . H30B H 0.9479 0.4938 0.3514 0.027 Uiso 1 1 calc R . . H30C H 0.8016 0.4707 0.3086 0.027 Uiso 1 1 calc R . . C27 C 0.95151(8) 0.46755(4) 0.12437(4) 0.01977(11) Uani 1 1 d . . . H27A H 0.9144 0.4167 0.0832 0.030 Uiso 1 1 calc R . . H27B H 1.0412 0.4661 0.1429 0.030 Uiso 1 1 calc R . . H27C H 0.9483 0.5050 0.1062 0.030 Uiso 1 1 calc R . . C115 C 0.74768(6) 0.68094(4) 0.66369(4) 0.01728(10) Uani 1 1 d . . . H11A H 0.7935 0.6400 0.6653 0.026 Uiso 1 1 calc R . . H11B H 0.7458 0.7209 0.7149 0.026 Uiso 1 1 calc R . . H11C H 0.7921 0.7031 0.6380 0.026 Uiso 1 1 calc R . . C10 C 1.36921(6) 0.90886(3) 0.43679(4) 0.01537(9) Uani 1 1 d . . . H10 H 1.4575 0.9292 0.4489 0.018 Uiso 1 1 calc R . . C125 C 0.68057(7) 0.81930(4) 0.91567(4) 0.01822(10) Uani 1 1 d . . . H125 H 0.6722 0.7967 0.9494 0.022 Uiso 1 1 calc R . . C24 C 1.14740(6) 0.50592(3) 0.29201(4) 0.01429(9) Uani 1 1 d . . . H24 H 1.0885 0.4602 0.2693 0.017 Uiso 1 1 calc R . . C26 C 0.73299(7) 0.48815(4) 0.15805(4) 0.01878(11) Uani 1 1 d . . . H26A H 0.7241 0.5275 0.1426 0.028 Uiso 1 1 calc R . . H26B H 0.6825 0.4978 0.1976 0.028 Uiso 1 1 calc R . . H26C H 0.7015 0.4375 0.1149 0.028 Uiso 1 1 calc R . . C122 C 0.16701(8) 0.73951(5) 0.89984(5) 0.02345(13) Uani 1 1 d . . . H122 H 0.0849 0.7291 0.9094 0.028 Uiso 1 1 calc R . . C130 C 0.45966(6) 0.61023(4) 0.74800(4) 0.01643(10) Uani 1 1 d . . . H13A H 0.4820 0.5579 0.7220 0.025 Uiso 1 1 calc R . . H13B H 0.4236 0.6252 0.7110 0.025 Uiso 1 1 calc R . . H13C H 0.3959 0.6122 0.7791 0.025 Uiso 1 1 calc R . . C17 C 0.84131(7) 0.88718(4) 0.32002(4) 0.01872(11) Uani 1 1 d . . . H17A H 0.8201 0.8412 0.2707 0.028 Uiso 1 1 calc R . . H17B H 0.9275 0.9121 0.3260 0.028 Uiso 1 1 calc R . . H17C H 0.7782 0.9228 0.3240 0.028 Uiso 1 1 calc R . . C34 C 0.52776(6) 0.63204(4) 0.02035(4) 0.01770(10) Uani 1 1 d . . . H34A H 0.4905 0.6763 0.0196 0.021 Uiso 1 1 calc R . . H34B H 0.5182 0.5901 -0.0320 0.021 Uiso 1 1 calc R . . C14 C 0.92928(7) 0.86802(4) 0.53207(3) 0.01648(10) Uani 1 1 d . . . H14A H 0.9309 0.8618 0.5767 0.025 Uiso 1 1 calc R . . H14B H 0.8473 0.8848 0.5211 0.025 Uiso 1 1 calc R . . H14C H 1.0004 0.9066 0.5413 0.025 Uiso 1 1 calc R . . C112 C 0.28875(7) 0.62256(4) 0.53180(4) 0.01700(10) Uani 1 1 d . . . H112 H 0.3425 0.6093 0.4951 0.020 Uiso 1 1 calc R . . B11 B 0.31592(6) 0.76294(4) 0.74501(4) 0.01218(9) Uani 1 1 d . . . C118 C 0.42195(7) 0.79673(4) 0.55522(4) 0.01916(11) Uani 1 1 d . . . H11D H 0.4256 0.8432 0.6034 0.029 Uiso 1 1 calc R . . H11E H 0.3366 0.7669 0.5397 0.029 Uiso 1 1 calc R . . H11F H 0.4380 0.8111 0.5173 0.029 Uiso 1 1 calc R . . C29 C 0.73562(6) 0.61348(4) 0.35208(4) 0.01636(9) Uani 1 1 d . . . H29A H 0.6701 0.5720 0.3143 0.025 Uiso 1 1 calc R . . H29B H 0.7366 0.6572 0.3425 0.025 Uiso 1 1 calc R . . H29C H 0.7155 0.6294 0.4021 0.025 Uiso 1 1 calc R . . C103 C 0.41703(8) 0.98296(4) 0.84437(4) 0.02155(12) Uani 1 1 d . . . C117 C 0.65898(7) 0.78778(4) 0.57462(4) 0.01758(10) Uani 1 1 d . . . H11G H 0.6622 0.8039 0.5365 0.026 Uiso 1 1 calc R . . H11H H 0.7217 0.7518 0.5699 0.026 Uiso 1 1 calc R . . H11I H 0.6797 0.8328 0.6247 0.026 Uiso 1 1 calc R . . C124 C 0.39685(7) 0.76737(4) 0.93736(4) 0.01869(11) Uani 1 1 d . . . H124 H 0.4724 0.7774 0.9730 0.022 Uiso 1 1 calc R . . C31 C 0.49176(7) 0.63112(5) 0.22918(4) 0.02160(12) Uani 1 1 d . . . H31A H 0.5188 0.5799 0.2104 0.032 Uiso 1 1 calc R . . H31B H 0.3993 0.6278 0.2301 0.032 Uiso 1 1 calc R . . H31C H 0.5394 0.6649 0.2800 0.032 Uiso 1 1 calc R . . C33 C 0.45615(6) 0.60504(4) 0.06621(4) 0.01688(10) Uani 1 1 d . . . H33A H 0.4685 0.5513 0.0523 0.020 Uiso 1 1 calc R . . H33B H 0.3628 0.6079 0.0564 0.020 Uiso 1 1 calc R . . C111 C 0.16110(7) 0.58912(4) 0.51047(4) 0.01987(11) Uani 1 1 d . . . H111 H 0.1278 0.5529 0.4596 0.024 Uiso 1 1 calc R . . C114 C 0.61258(8) 0.59110(4) 0.53887(4) 0.02080(12) Uani 1 1 d . . . H11J H 0.6538 0.6179 0.5162 0.031 Uiso 1 1 calc R . . H11K H 0.5244 0.5696 0.5116 0.031 Uiso 1 1 calc R . . H11L H 0.6615 0.5496 0.5362 0.031 Uiso 1 1 calc R . . C35 C 0.79806(7) 0.58125(4) 0.01714(4) 0.02027(11) Uani 1 1 d . . . H35A H 0.8800 0.5898 0.0503 0.030 Uiso 1 1 calc R . . H35B H 0.8149 0.5795 -0.0293 0.030 Uiso 1 1 calc R . . H35C H 0.7498 0.5325 0.0053 0.030 Uiso 1 1 calc R . . C131 C 0.56848(8) 0.99312(4) 0.67773(5) 0.02172(12) Uani 1 1 d . . . H13D H 0.5890 0.9571 0.6290 0.033 Uiso 1 1 calc R . . H13E H 0.5495 1.0408 0.6778 0.033 Uiso 1 1 calc R . . H13F H 0.4933 0.9702 0.6868 0.033 Uiso 1 1 calc R . . C32 C 0.46989(8) 0.76587(5) 0.19836(5) 0.02478(14) Uani 1 1 d . . . H32A H 0.5167 0.8019 0.2488 0.037 Uiso 1 1 calc R . . H32B H 0.3774 0.7617 0.1991 0.037 Uiso 1 1 calc R . . H32C H 0.4864 0.7846 0.1636 0.037 Uiso 1 1 calc R . . C104 C 0.35549(9) 1.00279(4) 0.79443(5) 0.02458(14) Uani 1 1 d . . . C135 C 0.97118(7) 0.85151(4) 0.75333(5) 0.02336(13) Uani 1 1 d . . . H13G H 0.9297 0.8135 0.7638 0.035 Uiso 1 1 calc R . . H13H H 1.0645 0.8582 0.7699 0.035 Uiso 1 1 calc R . . H13I H 0.9524 0.8338 0.6993 0.035 Uiso 1 1 calc R . . C129 C 0.62674(8) 0.64466(5) 0.85921(5) 0.02267(13) Uani 1 1 d . . . H12A H 0.5644 0.6568 0.8932 0.034 Uiso 1 1 calc R . . H12B H 0.7107 0.6742 0.8876 0.034 Uiso 1 1 calc R . . H12C H 0.6345 0.5897 0.8362 0.034 Uiso 1 1 calc R . . C132 C 0.69638(8) 1.09907(4) 0.84358(5) 0.02208(12) Uani 1 1 d . . . H13J H 0.6123 1.0935 0.8569 0.033 Uiso 1 1 calc R . . H13K H 0.7063 1.1458 0.8392 0.033 Uiso 1 1 calc R . . H13L H 0.7647 1.1025 0.8827 0.033 Uiso 1 1 calc R . . C123 C 0.27661(8) 0.75411(5) 0.95249(4) 0.02265(13) Uani 1 1 d . . . H123 H 0.2695 0.7550 0.9985 0.027 Uiso 1 1 calc R . . C105 C 0.28337(7) 0.94524(4) 0.72460(5) 0.02165(13) Uani 1 1 d . . . C133 C 0.86408(7) 1.02573(4) 0.72461(4) 0.01950(11) Uani 1 1 d . . . H13M H 0.8648 0.9854 0.6726 0.023 Uiso 1 1 calc R . . H13N H 0.8789 1.0765 0.7274 0.023 Uiso 1 1 calc R . . C134 C 0.96930(7) 1.01850(4) 0.78011(5) 0.02376(14) Uani 1 1 d . . . H13O H 0.9932 1.0686 0.8263 0.029 Uiso 1 1 calc R . . H13P H 1.0470 1.0036 0.7573 0.029 Uiso 1 1 calc R . . C36 C 0.76290(7) 0.75452(5) 0.07344(5) 0.02191(12) Uani 1 1 d . . . H36A H 0.6896 0.7798 0.0656 0.033 Uiso 1 1 calc R . . H36B H 0.8169 0.7460 0.0357 0.033 Uiso 1 1 calc R . . H36C H 0.8137 0.7872 0.1237 0.033 Uiso 1 1 calc R . . C127 C 0.81281(7) 0.80768(5) 0.89304(5) 0.02387(13) Uani 1 1 d . . . H12D H 0.8226 0.8286 0.8591 0.036 Uiso 1 1 calc R . . H12E H 0.8209 0.7528 0.8675 0.036 Uiso 1 1 calc R . . H12F H 0.8799 0.8342 0.9379 0.036 Uiso 1 1 calc R . . C126 C 0.66569(9) 0.90457(5) 0.95900(4) 0.02552(14) Uani 1 1 d . . . H12G H 0.7335 0.9302 1.0036 0.038 Uiso 1 1 calc R . . H12H H 0.5812 0.9102 0.9743 0.038 Uiso 1 1 calc R . . H12I H 0.6729 0.9279 0.9268 0.038 Uiso 1 1 calc R . . C136 C 0.94913(10) 0.98443(6) 0.90766(5) 0.03200(18) Uani 1 1 d . . . H13Q H 0.9153 1.0336 0.9325 0.048 Uiso 1 1 calc R . . H13R H 1.0428 0.9922 0.9232 0.048 Uiso 1 1 calc R . . H13S H 0.9105 0.9486 0.9217 0.048 Uiso 1 1 calc R . . H102 H 0.4197(11) 0.8962(7) 0.8699(7) 0.020(3) Uiso 1 1 d . . . H2 H 1.0750(10) 0.8047(6) 0.2641(6) 0.013(2) Uiso 1 1 d . . . H106 H 0.2271(11) 0.8311(7) 0.6595(7) 0.019(3) Uiso 1 1 d . . . H5 H 1.1434(11) 0.5826(7) 0.0568(6) 0.017(3) Uiso 1 1 d . . . H6 H 1.1699(11) 0.5875(6) 0.1729(6) 0.015(2) Uiso 1 1 d . . . H105 H 0.2385(13) 0.9591(8) 0.6898(7) 0.031(3) Uiso 1 1 d . . . H4 H 1.0766(12) 0.6892(7) 0.0433(7) 0.022(3) Uiso 1 1 d . . . H3 H 1.0307(11) 0.7974(7) 0.1462(7) 0.021(3) Uiso 1 1 d . . . H103 H 0.4635(12) 1.0210(7) 0.8911(7) 0.025(3) Uiso 1 1 d . . . H104 H 0.3607(13) 1.0553(8) 0.8060(8) 0.034(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.00682(2) 0.00681(2) 0.00726(2) 0.00313(2) 0.00066(2) 0.00089(2) Fe2 0.00898(3) 0.00934(3) 0.00946(3) 0.00548(2) 0.00237(2) 0.00040(2) P1 0.00747(5) 0.00719(4) 0.00831(5) 0.00274(4) 0.00186(4) 0.00084(3) P11 0.00985(5) 0.01068(5) 0.00945(5) 0.00567(4) 0.00175(4) 0.00039(4) P2 0.00925(5) 0.00757(4) 0.00963(5) 0.00434(4) 0.00041(4) 0.00012(4) P12 0.01127(5) 0.01393(5) 0.01002(5) 0.00747(4) 0.00185(4) 0.00037(4) Si11 0.01538(7) 0.01054(6) 0.01872(7) 0.00819(6) 0.00615(6) 0.00177(5) Si12 0.01170(7) 0.01505(7) 0.02347(8) 0.01043(6) 0.00128(6) -0.00160(5) Si1 0.00907(6) 0.01862(7) 0.01296(6) 0.00871(6) 0.00182(5) 0.00324(5) Si2 0.01010(6) 0.01789(7) 0.01183(6) 0.00944(6) 0.00005(5) -0.00054(5) N11 0.01117(16) 0.00974(15) 0.01181(16) 0.00547(13) 0.00320(13) 0.00033(12) N1 0.00850(15) 0.01036(14) 0.00963(15) 0.00550(12) 0.00057(12) 0.00099(11) N2 0.00840(16) 0.01720(18) 0.01163(16) 0.00876(15) 0.00009(13) 0.00133(13) C119 0.0152(2) 0.0165(2) 0.0126(2) 0.00893(17) 0.00516(17) 0.00188(16) C8 0.00909(17) 0.00838(15) 0.00940(16) 0.00356(13) 0.00194(13) 0.00065(12) C7 0.00905(17) 0.00795(15) 0.01032(17) 0.00256(13) 0.00217(13) 0.00012(12) C13 0.01171(19) 0.01250(18) 0.00926(17) 0.00424(14) 0.00246(14) 0.00062(14) C3 0.0176(2) 0.0139(2) 0.0133(2) 0.00832(17) -0.00006(17) -0.00012(16) C1 0.00876(16) 0.00867(15) 0.00933(16) 0.00408(13) 0.00226(13) 0.00112(12) N12 0.01155(17) 0.01096(16) 0.01776(19) 0.00795(15) 0.00370(15) -0.00006(13) C107 0.01147(19) 0.01376(19) 0.01260(19) 0.00730(16) 0.00023(15) -0.00107(15) C9 0.00916(18) 0.01094(17) 0.01384(19) 0.00443(15) 0.00205(15) 0.00024(13) C19 0.01123(18) 0.00875(16) 0.01204(18) 0.00542(14) 0.00160(14) 0.00199(13) C20 0.01001(17) 0.00914(16) 0.00919(16) 0.00424(13) 0.00190(13) 0.00191(13) C6 0.01023(18) 0.01088(17) 0.01090(18) 0.00355(14) 0.00262(14) 0.00223(14) C21 0.01018(18) 0.01310(18) 0.01127(18) 0.00605(15) 0.00147(14) 0.00259(14) C5 0.0126(2) 0.0160(2) 0.01001(18) 0.00358(16) 0.00323(15) 0.00112(16) C16 0.01075(18) 0.00984(17) 0.01378(19) 0.00430(15) 0.00330(15) 0.00314(14) C12 0.0120(2) 0.00852(17) 0.0167(2) 0.00156(15) 0.00378(17) 0.00012(14) C120 0.0127(2) 0.0154(2) 0.0160(2) 0.01010(18) 0.00569(17) 0.00245(16) C25 0.0159(2) 0.00935(17) 0.01236(19) 0.00436(15) -0.00008(16) -0.00125(15) B1 0.0101(2) 0.00811(17) 0.00957(19) 0.00385(15) 0.00193(16) 0.00145(14) C116 0.0164(2) 0.0145(2) 0.01100(18) 0.00746(16) 0.00246(16) 0.00071(16) C113 0.0144(2) 0.01279(19) 0.0157(2) 0.00776(17) 0.00465(17) 0.00261(15) C22 0.0126(2) 0.0167(2) 0.0151(2) 0.00907(18) 0.00304(17) 0.00596(16) C28 0.0125(2) 0.01311(18) 0.01245(19) 0.00767(16) 0.00076(15) -0.00098(15) C15 0.0159(2) 0.0173(2) 0.0124(2) 0.00768(17) 0.00126(17) 0.00282(17) C110 0.0137(2) 0.0202(3) 0.0249(3) 0.0127(2) -0.0039(2) -0.00484(19) C128 0.0147(2) 0.0166(2) 0.0161(2) 0.01151(18) 0.00349(17) 0.00275(17) C109 0.0119(2) 0.0190(2) 0.0217(3) 0.0118(2) 0.00127(19) -0.00171(17) C101 0.01169(19) 0.01352(19) 0.0163(2) 0.00907(17) 0.00561(16) 0.00326(15) C2 0.01155(19) 0.00945(16) 0.01175(18) 0.00510(14) 0.00130(15) 0.00093(13) C11 0.0138(2) 0.00942(18) 0.0210(3) 0.00160(17) 0.00315(19) -0.00176(15) C23 0.0163(2) 0.0146(2) 0.0200(2) 0.01058(19) 0.00439(19) 0.00710(17) C106 0.0131(2) 0.0196(2) 0.0234(3) 0.0154(2) 0.00620(19) 0.00537(18) C108 0.01074(19) 0.01319(18) 0.0148(2) 0.00895(16) 0.00124(15) -0.00005(14) C4 0.0184(2) 0.0189(2) 0.01089(19) 0.00767(18) 0.00124(17) -0.00178(18) C18 0.0103(2) 0.0165(2) 0.0188(2) 0.00631(19) 0.00307(17) 0.00273(16) C121 0.0147(2) 0.0263(3) 0.0246(3) 0.0178(3) 0.0084(2) 0.0040(2) C102 0.0180(2) 0.0134(2) 0.0163(2) 0.00654(18) 0.00803(19) 0.00260(17) C30 0.0191(3) 0.0183(2) 0.0211(3) 0.0143(2) 0.0013(2) -0.00139(19) C27 0.0244(3) 0.0150(2) 0.0137(2) 0.00220(18) 0.0038(2) -0.0005(2) C115 0.0129(2) 0.0202(2) 0.0223(3) 0.0127(2) 0.00493(19) 0.00358(18) C10 0.01026(19) 0.01185(19) 0.0189(2) 0.00376(17) 0.00211(17) -0.00210(15) C125 0.0175(2) 0.0242(3) 0.0126(2) 0.0101(2) -0.00131(18) -0.0026(2) C24 0.0155(2) 0.01023(18) 0.0183(2) 0.00773(17) 0.00252(18) 0.00340(15) C26 0.0166(2) 0.0159(2) 0.0189(2) 0.0067(2) -0.0037(2) -0.00323(18) C122 0.0209(3) 0.0322(4) 0.0289(3) 0.0214(3) 0.0143(3) 0.0056(3) C130 0.0163(2) 0.0143(2) 0.0214(3) 0.0106(2) 0.0043(2) 0.00101(17) C17 0.0217(3) 0.0177(2) 0.0233(3) 0.0138(2) 0.0074(2) 0.0084(2) C34 0.0122(2) 0.0274(3) 0.0153(2) 0.0132(2) -0.00184(17) -0.00096(19) C14 0.0190(2) 0.0161(2) 0.0110(2) 0.00326(17) 0.00482(18) 0.00288(18) C112 0.0174(2) 0.0179(2) 0.0129(2) 0.00659(18) -0.00115(18) -0.00284(18) B11 0.0110(2) 0.0141(2) 0.0145(2) 0.00912(19) 0.00342(18) 0.00150(17) C118 0.0206(3) 0.0221(3) 0.0201(3) 0.0150(2) 0.0015(2) 0.0033(2) C29 0.0134(2) 0.0196(2) 0.0184(2) 0.0106(2) 0.00449(18) 0.00131(18) C103 0.0277(3) 0.0129(2) 0.0235(3) 0.0060(2) 0.0135(3) 0.0034(2) C117 0.0187(3) 0.0202(2) 0.0177(2) 0.0117(2) 0.0063(2) 0.00009(19) C124 0.0219(3) 0.0240(3) 0.0150(2) 0.0124(2) 0.0069(2) 0.0027(2) C31 0.0140(2) 0.0367(4) 0.0220(3) 0.0201(3) 0.0048(2) 0.0031(2) C33 0.0104(2) 0.0239(3) 0.0154(2) 0.0096(2) 0.00016(17) -0.00170(18) C111 0.0193(3) 0.0187(2) 0.0178(2) 0.0086(2) -0.0051(2) -0.0051(2) C114 0.0267(3) 0.0146(2) 0.0189(3) 0.0052(2) 0.0077(2) 0.0051(2) C35 0.0158(2) 0.0221(3) 0.0195(3) 0.0071(2) 0.0044(2) 0.0011(2) C131 0.0215(3) 0.0224(3) 0.0252(3) 0.0148(3) 0.0034(2) 0.0031(2) C32 0.0219(3) 0.0251(3) 0.0259(3) 0.0108(3) 0.0025(3) 0.0117(3) C104 0.0303(4) 0.0151(2) 0.0355(4) 0.0143(3) 0.0183(3) 0.0091(2) C135 0.0155(3) 0.0213(3) 0.0395(4) 0.0185(3) 0.0091(3) 0.0047(2) C129 0.0277(3) 0.0261(3) 0.0230(3) 0.0191(3) 0.0033(3) 0.0063(3) C132 0.0260(3) 0.0133(2) 0.0251(3) 0.0066(2) 0.0091(3) 0.0038(2) C123 0.0268(3) 0.0289(3) 0.0207(3) 0.0165(3) 0.0129(3) 0.0052(3) C105 0.0202(3) 0.0222(3) 0.0349(4) 0.0212(3) 0.0124(3) 0.0103(2) C133 0.0207(3) 0.0143(2) 0.0274(3) 0.0117(2) 0.0106(2) 0.00126(19) C134 0.0154(3) 0.0189(3) 0.0405(4) 0.0170(3) 0.0065(3) -0.0013(2) C36 0.0198(3) 0.0251(3) 0.0272(3) 0.0195(3) -0.0012(2) -0.0021(2) C127 0.0151(3) 0.0332(4) 0.0231(3) 0.0153(3) -0.0019(2) -0.0020(2) C126 0.0275(4) 0.0246(3) 0.0152(3) 0.0039(2) -0.0007(2) -0.0038(3) C136 0.0296(4) 0.0334(4) 0.0260(4) 0.0133(3) -0.0076(3) -0.0105(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.6605(5) . ? Fe1 C1 2.1493(5) . ? Fe1 P1 2.2312(2) . ? Fe1 P2 2.2660(2) . ? Fe1 C2 2.3405(6) . ? Fe1 B1 2.3768(6) . ? Fe2 N11 1.6658(5) . ? Fe2 C101 2.1440(6) . ? Fe2 C102 2.2266(6) . ? Fe2 P12 2.2287(2) . ? Fe2 P11 2.2632(2) . ? Fe2 B11 2.4288(7) . ? P1 C7 1.8148(5) . ? P1 C16 1.8596(6) . ? P1 C13 1.8835(6) . ? P11 C107 1.8311(6) . ? P11 C116 1.8656(6) . ? P11 C113 1.8830(6) . ? P2 C19 1.8226(6) . ? P2 C25 1.8653(6) . ? P2 C28 1.8771(6) . ? P12 C119 1.8155(6) . ? P12 C125 1.8549(7) . ? P12 C128 1.8833(6) . ? Si11 N12 1.7991(5) . ? Si11 C131 1.8460(8) . ? Si11 C133 1.8616(7) . ? Si11 C132 1.8630(8) . ? Si12 N12 1.7983(6) . ? Si12 C135 1.8519(8) . ? Si12 C136 1.8594(10) . ? Si12 C134 1.8802(8) . ? Si1 N2 1.7908(5) . ? Si1 C31 1.8409(7) . ? Si1 C32 1.8578(8) . ? Si1 C33 1.8656(7) . ? Si2 N2 1.7885(5) . ? Si2 C35 1.8491(8) . ? Si2 C36 1.8667(7) . ? Si2 C34 1.8790(7) . ? N11 N12 1.3242(7) . ? N1 N2 1.3282(6) . ? C119 C124 1.4004(9) . ? C119 C120 1.4055(9) . ? C8 C9 1.4021(8) . ? C8 C7 1.4053(7) . ? C8 B1 1.6016(8) . ? C7 C12 1.3967(7) . ? C13 C15 1.5325(9) . ? C13 C14 1.5348(8) . ? C13 H13 1.0000 . ? C3 C4 1.3681(9) . ? C3 C2 1.4238(8) . ? C3 H3 0.988(12) . ? C1 C2 1.4231(7) . ? C1 C6 1.4324(7) . ? C1 B1 1.5574(8) . ? C107 C112 1.4000(9) . ? C107 C108 1.4069(9) . ? C9 C10 1.3928(8) . ? C9 H9 0.9500 . ? C19 C24 1.4011(7) . ? C19 C20 1.4077(7) . ? C20 C21 1.4047(8) . ? C20 B1 1.5843(8) . ? C6 C5 1.3690(8) . ? C6 H6 0.971(11) . ? C21 C22 1.3894(8) . ? C21 H21 0.9500 . ? C5 C4 1.4196(10) . ? C5 H5 0.955(11) . ? C16 C18 1.5284(9) . ? C16 C17 1.5295(9) . ? C16 H16 1.0000 . ? C12 C11 1.3896(9) . ? C12 H12 0.9500 . ? C120 C121 1.4055(9) . ? C120 B11 1.5994(9) . ? C25 C27 1.5263(10) . ? C25 C26 1.5276(9) . ? C25 H25 1.0000 . ? C116 C118 1.5215(9) . ? C116 C117 1.5288(9) . ? C116 H116 1.0000 . ? C113 C115 1.5318(9) . ? C113 C114 1.5333(9) . ? C113 H113 1.0000 . ? C22 C23 1.3919(9) . ? C22 H22 0.9500 . ? C28 C29 1.5284(9) . ? C28 C30 1.5302(8) . ? C28 H28 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C110 C109 1.3886(10) . ? C110 C111 1.3890(12) . ? C110 H110 0.9500 . ? C128 C130 1.5312(9) . ? C128 C129 1.5326(9) . ? C128 H128 1.0000 . ? C109 C108 1.4080(8) . ? C109 H109 0.9500 . ? C101 C102 1.4285(9) . ? C101 C106 1.4372(9) . ? C101 B11 1.5443(9) . ? C2 H2 0.919(11) . ? C11 C10 1.3917(9) . ? C11 H11 0.9500 . ? C23 C24 1.3887(9) . ? C23 H23 0.9500 . ? C106 C105 1.3648(9) . ? C106 H106 0.965(12) . ? C108 B11 1.5878(9) . ? C4 H4 0.964(12) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C121 C122 1.3953(10) . ? C121 H121 0.9500 . ? C102 C103 1.4357(9) . ? C102 H102 0.931(12) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C115 H11A 0.9800 . ? C115 H11B 0.9800 . ? C115 H11C 0.9800 . ? C10 H10 0.9500 . ? C125 C127 1.5262(11) . ? C125 C126 1.5305(12) . ? C125 H125 1.0000 . ? C24 H24 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C122 C123 1.3892(12) . ? C122 H122 0.9500 . ? C130 H13A 0.9800 . ? C130 H13B 0.9800 . ? C130 H13C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C34 C33 1.5445(10) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C112 C111 1.3911(10) . ? C112 H112 0.9500 . ? C118 H11D 0.9800 . ? C118 H11E 0.9800 . ? C118 H11F 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C103 C104 1.3645(13) . ? C103 H103 0.942(13) . ? C117 H11G 0.9800 . ? C117 H11H 0.9800 . ? C117 H11I 0.9800 . ? C124 C123 1.3908(11) . ? C124 H124 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C111 H111 0.9500 . ? C114 H11J 0.9800 . ? C114 H11K 0.9800 . ? C114 H11L 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C131 H13D 0.9800 . ? C131 H13E 0.9800 . ? C131 H13F 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C104 C105 1.4223(13) . ? C104 H104 0.955(14) . ? C135 H13G 0.9800 . ? C135 H13H 0.9800 . ? C135 H13I 0.9800 . ? C129 H12A 0.9800 . ? C129 H12B 0.9800 . ? C129 H12C 0.9800 . ? C132 H13J 0.9800 . ? C132 H13K 0.9800 . ? C132 H13L 0.9800 . ? C123 H123 0.9500 . ? C105 H105 0.960(13) . ? C133 C134 1.5454(12) . ? C133 H13M 0.9900 . ? C133 H13N 0.9900 . ? C134 H13O 0.9900 . ? C134 H13P 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C127 H12D 0.9800 . ? C127 H12E 0.9800 . ? C127 H12F 0.9800 . ? C126 H12G 0.9800 . ? C126 H12H 0.9800 . ? C126 H12I 0.9800 . ? C136 H13Q 0.9800 . ? C136 H13R 0.9800 . ? C136 H13S 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 C1 124.23(2) . . ? N1 Fe1 P1 115.257(18) . . ? C1 Fe1 P1 103.259(15) . . ? N1 Fe1 P2 107.771(17) . . ? C1 Fe1 P2 94.473(14) . . ? P1 Fe1 P2 109.521(8) . . ? N1 Fe1 C2 100.68(2) . . ? C1 Fe1 C2 36.646(19) . . ? P1 Fe1 C2 92.649(15) . . ? P2 Fe1 C2 130.728(15) . . ? N1 Fe1 B1 164.05(2) . . ? C1 Fe1 B1 39.85(2) . . ? P1 Fe1 B1 74.585(15) . . ? P2 Fe1 B1 78.689(15) . . ? C2 Fe1 B1 65.30(2) . . ? N11 Fe2 C101 122.67(2) . . ? N11 Fe2 C102 99.39(2) . . ? C101 Fe2 C102 38.09(2) . . ? N11 Fe2 P12 119.708(19) . . ? C101 Fe2 P12 102.087(17) . . ? C102 Fe2 P12 92.211(19) . . ? N11 Fe2 P11 105.884(18) . . ? C101 Fe2 P11 97.394(18) . . ? C102 Fe2 P11 135.216(19) . . ? P12 Fe2 P11 105.878(10) . . ? N11 Fe2 B11 161.34(2) . . ? C101 Fe2 B11 38.85(2) . . ? C102 Fe2 B11 66.53(2) . . ? P12 Fe2 B11 74.645(17) . . ? P11 Fe2 B11 79.103(18) . . ? C7 P1 C16 105.78(3) . . ? C7 P1 C13 99.26(3) . . ? C16 P1 C13 101.20(3) . . ? C7 P1 Fe1 110.465(18) . . ? C16 P1 Fe1 112.20(2) . . ? C13 P1 Fe1 125.759(19) . . ? C107 P11 C116 101.28(3) . . ? C107 P11 C113 104.92(3) . . ? C116 P11 C113 101.43(3) . . ? C107 P11 Fe2 111.85(2) . . ? C116 P11 Fe2 118.70(2) . . ? C113 P11 Fe2 116.66(2) . . ? C19 P2 C25 103.31(3) . . ? C19 P2 C28 100.65(3) . . ? C25 P2 C28 103.35(3) . . ? C19 P2 Fe1 111.878(18) . . ? C25 P2 Fe1 120.49(2) . . ? C28 P2 Fe1 114.763(19) . . ? C119 P12 C125 104.70(3) . . ? C119 P12 C128 98.75(3) . . ? C125 P12 C128 101.43(3) . . ? C119 P12 Fe2 111.84(2) . . ? C125 P12 Fe2 113.80(2) . . ? C128 P12 Fe2 123.84(2) . . ? N12 Si11 C131 115.60(3) . . ? N12 Si11 C133 96.95(3) . . ? C131 Si11 C133 112.60(4) . . ? N12 Si11 C132 107.24(3) . . ? C131 Si11 C132 113.24(4) . . ? C133 Si11 C132 109.97(4) . . ? N12 Si12 C135 111.09(3) . . ? N12 Si12 C136 112.99(4) . . ? C135 Si12 C136 111.95(5) . . ? N12 Si12 C134 98.81(3) . . ? C135 Si12 C134 112.87(4) . . ? C136 Si12 C134 108.46(4) . . ? N2 Si1 C31 113.82(3) . . ? N2 Si1 C32 111.27(3) . . ? C31 Si1 C32 111.14(4) . . ? N2 Si1 C33 95.98(3) . . ? C31 Si1 C33 113.74(4) . . ? C32 Si1 C33 110.02(4) . . ? N2 Si2 C35 109.88(3) . . ? N2 Si2 C36 109.61(3) . . ? C35 Si2 C36 115.53(4) . . ? N2 Si2 C34 98.59(3) . . ? C35 Si2 C34 111.17(3) . . ? C36 Si2 C34 110.75(3) . . ? N12 N11 Fe2 176.17(5) . . ? N2 N1 Fe1 176.35(4) . . ? N1 N2 Si2 120.68(4) . . ? N1 N2 Si1 127.93(4) . . ? Si2 N2 Si1 111.37(3) . . ? C124 C119 C120 121.76(6) . . ? C124 C119 P12 127.56(5) . . ? C120 C119 P12 110.36(4) . . ? C9 C8 C7 117.32(5) . . ? C9 C8 B1 124.59(5) . . ? C7 C8 B1 117.55(5) . . ? C12 C7 C8 121.80(5) . . ? C12 C7 P1 128.24(4) . . ? C8 C7 P1 109.96(4) . . ? C15 C13 C14 107.59(5) . . ? C15 C13 P1 111.40(4) . . ? C14 C13 P1 114.52(4) . . ? C15 C13 H13 107.7 . . ? C14 C13 H13 107.7 . . ? P1 C13 H13 107.7 . . ? C4 C3 C2 120.57(6) . . ? C4 C3 H3 120.0(7) . . ? C2 C3 H3 119.3(7) . . ? C2 C1 C6 116.60(5) . . ? C2 C1 B1 117.21(5) . . ? C6 C1 B1 126.06(5) . . ? C2 C1 Fe1 79.00(3) . . ? C6 C1 Fe1 116.08(4) . . ? B1 C1 Fe1 77.97(3) . . ? N11 N12 Si12 124.97(4) . . ? N11 N12 Si11 124.64(4) . . ? Si12 N12 Si11 110.12(3) . . ? C112 C107 C108 120.77(6) . . ? C112 C107 P11 123.86(5) . . ? C108 C107 P11 115.27(4) . . ? C10 C9 C8 121.10(5) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C24 C19 C20 120.91(5) . . ? C24 C19 P2 125.47(4) . . ? C20 C19 P2 113.54(4) . . ? C21 C20 C19 117.47(5) . . ? C21 C20 B1 123.23(5) . . ? C19 C20 B1 119.00(5) . . ? C5 C6 C1 122.03(5) . . ? C5 C6 H6 119.6(7) . . ? C1 C6 H6 118.3(7) . . ? C22 C21 C20 121.45(5) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C6 C5 C4 120.20(5) . . ? C6 C5 H5 119.6(7) . . ? C4 C5 H5 120.2(7) . . ? C18 C16 C17 110.49(5) . . ? C18 C16 P1 109.60(4) . . ? C17 C16 P1 112.01(4) . . ? C18 C16 H16 108.2 . . ? C17 C16 H16 108.2 . . ? P1 C16 H16 108.2 . . ? C11 C12 C7 119.64(5) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? C119 C120 C121 117.03(6) . . ? C119 C120 B11 118.11(5) . . ? C121 C120 B11 124.69(6) . . ? C27 C25 C26 109.74(6) . . ? C27 C25 P2 112.57(4) . . ? C26 C25 P2 111.76(4) . . ? C27 C25 H25 107.5 . . ? C26 C25 H25 107.5 . . ? P2 C25 H25 107.5 . . ? C1 B1 C20 116.95(4) . . ? C1 B1 C8 112.57(4) . . ? C20 B1 C8 122.93(5) . . ? C1 B1 Fe1 62.18(3) . . ? C20 B1 Fe1 114.72(4) . . ? C8 B1 Fe1 112.26(4) . . ? C118 C116 C117 110.87(5) . . ? C118 C116 P11 110.77(5) . . ? C117 C116 P11 112.54(4) . . ? C118 C116 H116 107.5 . . ? C117 C116 H116 107.5 . . ? P11 C116 H116 107.5 . . ? C115 C113 C114 109.36(6) . . ? C115 C113 P11 111.48(4) . . ? C114 C113 P11 116.98(5) . . ? C115 C113 H113 106.1 . . ? C114 C113 H113 106.1 . . ? P11 C113 H113 106.1 . . ? C21 C22 C23 120.10(5) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C29 C28 C30 109.96(5) . . ? C29 C28 P2 112.85(4) . . ? C30 C28 P2 116.66(5) . . ? C29 C28 H28 105.5 . . ? C30 C28 H28 105.5 . . ? P2 C28 H28 105.5 . . ? 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 . . ? C109 C110 C111 120.00(6) . . ? C109 C110 H110 120.0 . . ? C111 C110 H110 120.0 . . ? C130 C128 C129 107.80(5) . . ? C130 C128 P12 110.98(4) . . ? C129 C128 P12 115.58(5) . . ? C130 C128 H128 107.4 . . ? C129 C128 H128 107.4 . . ? P12 C128 H128 107.4 . . ? C110 C109 C108 121.97(7) . . ? C110 C109 H109 119.0 . . ? C108 C109 H109 119.0 . . ? C102 C101 C106 117.26(6) . . ? C102 C101 B11 118.78(5) . . ? C106 C101 B11 123.83(6) . . ? C102 C101 Fe2 74.09(4) . . ? C106 C101 Fe2 118.68(4) . . ? B11 C101 Fe2 80.59(3) . . ? C1 C2 C3 120.52(5) . . ? C1 C2 Fe1 64.35(3) . . ? C3 C2 Fe1 126.15(4) . . ? C1 C2 H2 119.3(7) . . ? C3 C2 H2 117.4(7) . . ? Fe1 C2 H2 94.9(7) . . ? C12 C11 C10 119.57(5) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C24 C23 C22 119.77(5) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C105 C106 C101 121.82(7) . . ? C105 C106 H106 119.8(7) . . ? C101 C106 H106 118.1(7) . . ? C107 C108 C109 117.19(6) . . ? C107 C108 B11 119.78(5) . . ? C109 C108 B11 122.90(6) . . ? C3 C4 C5 119.87(6) . . ? C3 C4 H4 119.0(7) . . ? C5 C4 H4 121.1(7) . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C122 C121 C120 121.34(7) . . ? C122 C121 H121 119.3 . . ? C120 C121 H121 119.3 . . ? C101 C102 C103 119.55(6) . . ? C101 C102 Fe2 67.82(3) . . ? C103 C102 Fe2 121.51(5) . . ? C101 C102 H102 120.2(7) . . ? C103 C102 H102 116.7(7) . . ? Fe2 C102 H102 98.7(7) . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C113 C115 H11A 109.5 . . ? C113 C115 H11B 109.5 . . ? H11A C115 H11B 109.5 . . ? C113 C115 H11C 109.5 . . ? H11A C115 H11C 109.5 . . ? H11B C115 H11C 109.5 . . ? C11 C10 C9 120.55(5) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C127 C125 C126 111.37(6) . . ? C127 C125 P12 110.48(5) . . ? C126 C125 P12 110.83(5) . . ? C127 C125 H125 108.0 . . ? C126 C125 H125 108.0 . . ? P12 C125 H125 108.0 . . ? C23 C24 C19 120.05(5) . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C123 C122 C121 120.53(7) . . ? C123 C122 H122 119.7 . . ? C121 C122 H122 119.7 . . ? C128 C130 H13A 109.5 . . ? C128 C130 H13B 109.5 . . ? H13A C130 H13B 109.5 . . ? C128 C130 H13C 109.5 . . ? H13A C130 H13C 109.5 . . ? H13B C130 H13C 109.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C33 C34 Si2 109.03(4) . . ? C33 C34 H34A 109.9 . . ? Si2 C34 H34A 109.9 . . ? C33 C34 H34B 109.9 . . ? Si2 C34 H34B 109.9 . . ? H34A C34 H34B 108.3 . . ? 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 . . ? C111 C112 C107 120.63(7) . . ? C111 C112 H112 119.7 . . ? C107 C112 H112 119.7 . . ? C101 B11 C108 117.39(5) . . ? C101 B11 C120 115.75(5) . . ? C108 B11 C120 121.77(5) . . ? C101 B11 Fe2 60.56(3) . . ? C108 B11 Fe2 113.20(4) . . ? C120 B11 Fe2 112.30(4) . . ? C116 C118 H11D 109.5 . . ? C116 C118 H11E 109.5 . . ? H11D C118 H11E 109.5 . . ? C116 C118 H11F 109.5 . . ? H11D C118 H11F 109.5 . . ? H11E C118 H11F 109.5 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C104 C103 C102 120.80(7) . . ? C104 C103 H103 120.4(8) . . ? C102 C103 H103 118.7(8) . . ? C116 C117 H11G 109.5 . . ? C116 C117 H11H 109.5 . . ? H11G C117 H11H 109.5 . . ? C116 C117 H11I 109.5 . . ? H11G C117 H11I 109.5 . . ? H11H C117 H11I 109.5 . . ? C123 C124 C119 119.81(7) . . ? C123 C124 H124 120.1 . . ? C119 C124 H124 120.1 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C34 C33 Si1 106.97(4) . . ? C34 C33 H33A 110.3 . . ? Si1 C33 H33A 110.3 . . ? C34 C33 H33B 110.3 . . ? Si1 C33 H33B 110.3 . . ? H33A C33 H33B 108.6 . . ? C110 C111 C112 119.44(6) . . ? C110 C111 H111 120.3 . . ? C112 C111 H111 120.3 . . ? C113 C114 H11J 109.5 . . ? C113 C114 H11K 109.5 . . ? H11J C114 H11K 109.5 . . ? C113 C114 H11L 109.5 . . ? H11J C114 H11L 109.5 . . ? H11K C114 H11L 109.5 . . ? Si2 C35 H35A 109.5 . . ? Si2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si11 C131 H13D 109.5 . . ? Si11 C131 H13E 109.5 . . ? H13D C131 H13E 109.5 . . ? Si11 C131 H13F 109.5 . . ? H13D C131 H13F 109.5 . . ? H13E C131 H13F 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C103 C104 C105 120.15(6) . . ? C103 C104 H104 120.3(8) . . ? C105 C104 H104 119.6(8) . . ? Si12 C135 H13G 109.5 . . ? Si12 C135 H13H 109.5 . . ? H13G C135 H13H 109.5 . . ? Si12 C135 H13I 109.5 . . ? H13G C135 H13I 109.5 . . ? H13H C135 H13I 109.5 . . ? C128 C129 H12A 109.5 . . ? C128 C129 H12B 109.5 . . ? H12A C129 H12B 109.5 . . ? C128 C129 H12C 109.5 . . ? H12A C129 H12C 109.5 . . ? H12B C129 H12C 109.5 . . ? Si11 C132 H13J 109.5 . . ? Si11 C132 H13K 109.5 . . ? H13J C132 H13K 109.5 . . ? Si11 C132 H13L 109.5 . . ? H13J C132 H13L 109.5 . . ? H13K C132 H13L 109.5 . . ? C122 C123 C124 119.47(7) . . ? C122 C123 H123 120.3 . . ? C124 C123 H123 120.3 . . ? C106 C105 C104 120.23(7) . . ? C106 C105 H105 119.5(8) . . ? C104 C105 H105 120.3(8) . . ? C134 C133 Si11 106.69(5) . . ? C134 C133 H13M 110.4 . . ? Si11 C133 H13M 110.4 . . ? C134 C133 H13N 110.4 . . ? Si11 C133 H13N 110.4 . . ? H13M C133 H13N 108.6 . . ? C133 C134 Si12 110.09(5) . . ? C133 C134 H13O 109.6 . . ? Si12 C134 H13O 109.6 . . ? C133 C134 H13P 109.6 . . ? Si12 C134 H13P 109.6 . . ? H13O C134 H13P 108.2 . . ? Si2 C36 H36A 109.5 . . ? Si2 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si2 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C125 C127 H12D 109.5 . . ? C125 C127 H12E 109.5 . . ? H12D C127 H12E 109.5 . . ? C125 C127 H12F 109.5 . . ? H12D C127 H12F 109.5 . . ? H12E C127 H12F 109.5 . . ? C125 C126 H12G 109.5 . . ? C125 C126 H12H 109.5 . . ? H12G C126 H12H 109.5 . . ? C125 C126 H12I 109.5 . . ? H12G C126 H12I 109.5 . . ? H12H C126 H12I 109.5 . . ? Si12 C136 H13Q 109.5 . . ? Si12 C136 H13R 109.5 . . ? H13Q C136 H13R 109.5 . . ? Si12 C136 H13S 109.5 . . ? H13Q C136 H13S 109.5 . . ? H13R C136 H13S 109.5 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.858 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.083 ####################################################### # Compound 4: [(iPrDPBPh)Fe]2N2 # ####################################################### data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H82 B2 Fe2 N2 P4' _chemical_formula_weight 1088.54 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' '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' 'N' 'N' 0.0061 0.0033 '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 13.6080(5) _cell_length_b 22.6752(7) _cell_length_c 18.8057(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.3660(10) _cell_angle_gamma 90.00 _cell_volume 5645.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5086 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 35.83 _exptl_crystal_description chunk _exptl_crystal_colour brown _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; 'Bruker KAPPA APEX II' ; _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 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 485205 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 46.11 _reflns_number_total 48837 _reflns_number_gt 35070 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7-0 (Bruker-AXS, 2007)' _computing_cell_refinement 'SAINT V7.68A (Bruker-AXS, 2007)' _computing_data_reduction 'SAINT V7.68A (Bruker-AXS, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0375P)^2^+1.2348P] 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 48837 _refine_ls_number_parameters 687 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0916 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.426480(7) 0.283792(4) 0.396562(5) 0.00960(2) Uani 1 1 d . . . Fe2 Fe 0.132839(7) 0.392469(4) 0.269872(5) 0.00985(2) Uani 1 1 d . . . P3 P 0.129582(13) 0.491853(8) 0.303516(9) 0.01141(3) Uani 1 1 d . . . P1 P 0.573136(13) 0.320578(7) 0.370411(9) 0.01084(3) Uani 1 1 d . . . P2 P 0.420051(13) 0.182123(7) 0.365490(10) 0.01199(3) Uani 1 1 d . . . P4 P 0.121034(13) 0.389497(8) 0.143898(9) 0.01140(3) Uani 1 1 d . . . N2 N 0.24841(4) 0.35314(2) 0.31539(3) 0.01154(8) Uani 1 1 d . . . N1 N 0.31843(4) 0.32503(2) 0.34427(3) 0.01130(8) Uani 1 1 d . . . C1 C 0.48182(5) 0.28855(3) 0.51889(3) 0.01263(9) Uani 1 1 d . . . C101 C -0.01697(5) 0.35927(3) 0.27836(4) 0.01327(9) Uani 1 1 d . . . C120 C -0.07723(5) 0.41069(3) 0.14479(4) 0.01254(9) Uani 1 1 d . . . C6 C 0.51882(6) 0.34251(3) 0.55464(4) 0.01630(11) Uani 1 1 d . . . C16 C 0.61087(5) 0.28533(3) 0.29076(4) 0.01402(10) Uani 1 1 d . . . H16 H 0.6310 0.2441 0.3066 0.017 Uiso 1 1 calc R . . C2 C 0.37544(5) 0.28040(3) 0.50326(4) 0.01450(10) Uani 1 1 d . . . C119 C -0.01281(5) 0.39379(3) 0.09914(4) 0.01376(9) Uani 1 1 d . . . C20 C 0.52422(5) 0.17476(3) 0.50579(4) 0.01330(9) Uani 1 1 d . . . C7 C 0.68139(5) 0.30638(3) 0.44639(4) 0.01321(9) Uani 1 1 d . . . C11 C 0.85239(6) 0.32226(4) 0.51622(5) 0.02027(13) Uani 1 1 d . . . H11 H 0.9155 0.3419 0.5230 0.024 Uiso 1 1 calc R . . C28 C 0.50449(5) 0.14435(3) 0.31324(4) 0.01516(10) Uani 1 1 d . . . H28 H 0.5074 0.1699 0.2704 0.018 Uiso 1 1 calc R . . C19 C 0.45413(5) 0.14356(3) 0.45229(4) 0.01407(10) Uani 1 1 d . . . C107 C 0.00490(5) 0.50734(3) 0.31852(4) 0.01325(9) Uani 1 1 d . . . C125 C 0.17907(6) 0.45271(3) 0.10478(4) 0.01571(10) Uani 1 1 d . . . H125 H 0.1380 0.4882 0.1106 0.019 Uiso 1 1 calc R . . C30 C 0.61242(6) 0.13905(3) 0.36029(4) 0.01792(11) Uani 1 1 d . . . H30A H 0.6158 0.1063 0.3948 0.027 Uiso 1 1 calc R . . H30B H 0.6312 0.1758 0.3874 0.027 Uiso 1 1 calc R . . H30C H 0.6592 0.1316 0.3287 0.027 Uiso 1 1 calc R . . C121 C -0.18060(5) 0.41675(3) 0.11094(4) 0.01606(11) Uani 1 1 d . . . H121 H -0.2258 0.4296 0.1394 0.019 Uiso 1 1 calc R . . C18 C 0.52086(6) 0.27923(3) 0.22487(4) 0.01719(11) Uani 1 1 d . . . H18A H 0.5057 0.3177 0.2011 0.026 Uiso 1 1 calc R . . H18B H 0.4618 0.2651 0.2414 0.026 Uiso 1 1 calc R . . H18C H 0.5376 0.2510 0.1900 0.026 Uiso 1 1 calc R . . C5 C 0.45614(7) 0.38171(3) 0.57868(4) 0.01997(13) Uani 1 1 d . . . C17 C 0.70268(6) 0.31220(4) 0.26843(4) 0.02154(13) Uani 1 1 d . . . H17A H 0.7210 0.2877 0.2306 0.032 Uiso 1 1 calc R . . H17B H 0.7597 0.3140 0.3111 0.032 Uiso 1 1 calc R . . H17C H 0.6861 0.3521 0.2493 0.032 Uiso 1 1 calc R . . C23 C 0.45936(7) 0.05965(3) 0.53243(5) 0.02054(13) Uani 1 1 d . . . H23 H 0.4364 0.0215 0.5420 0.025 Uiso 1 1 calc R . . C109 C -0.17018(5) 0.48100(4) 0.28195(4) 0.01810(11) Uani 1 1 d . . . H109 H -0.2231 0.4577 0.2537 0.022 Uiso 1 1 calc R . . C3 C 0.31098(6) 0.32242(3) 0.52509(4) 0.01850(12) Uani 1 1 d . . . C108 C -0.07023(5) 0.47136(3) 0.27577(4) 0.01317(9) Uani 1 1 d . . . C122 C -0.21846(5) 0.40455(4) 0.03725(4) 0.01842(12) Uani 1 1 d . . . H122 H -0.2886 0.4090 0.0163 0.022 Uiso 1 1 calc R . . C10 C 0.83699(6) 0.28066(4) 0.56672(4) 0.02030(13) Uani 1 1 d . . . H10 H 0.8898 0.2719 0.6081 0.024 Uiso 1 1 calc R . . C8 C 0.66359(5) 0.26472(3) 0.49769(4) 0.01312(9) Uani 1 1 d . . . B2 B -0.03588(5) 0.41760(3) 0.23134(4) 0.01260(10) Uani 1 1 d . . . C116 C 0.21804(5) 0.51147(3) 0.39105(4) 0.01635(11) Uani 1 1 d . . . H116 H 0.2090 0.5541 0.4017 0.020 Uiso 1 1 calc R . . C130 C 0.10681(6) 0.26873(3) 0.11012(5) 0.01950(12) Uani 1 1 d . . . H13A H 0.1353 0.2346 0.0900 0.029 Uiso 1 1 calc R . . H13B H 0.0361 0.2739 0.0842 0.029 Uiso 1 1 calc R . . H13C H 0.1106 0.2622 0.1622 0.029 Uiso 1 1 calc R . . C15 C 0.50148(7) 0.42172(3) 0.28918(4) 0.02042(13) Uani 1 1 d . . . H15A H 0.4353 0.4088 0.2955 0.031 Uiso 1 1 calc R . . H15B H 0.5139 0.4047 0.2441 0.031 Uiso 1 1 calc R . . H15C H 0.5026 0.4648 0.2861 0.031 Uiso 1 1 calc R . . C129 C 0.28029(5) 0.31519(3) 0.13214(4) 0.01805(12) Uani 1 1 d . . . H12A H 0.2952 0.3196 0.1854 0.027 Uiso 1 1 calc R . . H12B H 0.3184 0.3446 0.1114 0.027 Uiso 1 1 calc R . . H12C H 0.2998 0.2756 0.1198 0.027 Uiso 1 1 calc R . . C128 C 0.16687(5) 0.32417(3) 0.10068(4) 0.01434(10) Uani 1 1 d . . . H128 H 0.1563 0.3322 0.0472 0.017 Uiso 1 1 calc R . . C9 C 0.74478(6) 0.25167(3) 0.55708(4) 0.01780(11) Uani 1 1 d . . . H9 H 0.7363 0.2224 0.5913 0.021 Uiso 1 1 calc R . . C14 C 0.57753(7) 0.43534(3) 0.42332(5) 0.02188(13) Uani 1 1 d . . . H14A H 0.5799 0.4777 0.4138 0.033 Uiso 1 1 calc R . . H14B H 0.6346 0.4245 0.4634 0.033 Uiso 1 1 calc R . . H14C H 0.5141 0.4258 0.4369 0.033 Uiso 1 1 calc R . . C24 C 0.42090(6) 0.08684(3) 0.46539(4) 0.01823(12) Uani 1 1 d . . . H24 H 0.3724 0.0671 0.4287 0.022 Uiso 1 1 calc R . . C102 C 0.01133(6) 0.36074(3) 0.35581(4) 0.01771(11) Uani 1 1 d . . . C124 C -0.05136(6) 0.38067(4) 0.02497(4) 0.01823(12) Uani 1 1 d . . . H124 H -0.0069 0.3682 -0.0042 0.022 Uiso 1 1 calc R . . C106 C -0.02296(6) 0.30255(3) 0.24601(4) 0.01845(12) Uani 1 1 d . . . C113 C 0.14384(6) 0.55476(3) 0.24108(4) 0.01681(11) Uani 1 1 d . . . H113 H 0.1971 0.5432 0.2150 0.020 Uiso 1 1 calc R . . C4 C 0.35093(6) 0.37159(4) 0.56354(4) 0.02034(13) Uani 1 1 d . . . B1 B 0.55116(6) 0.24223(3) 0.49304(4) 0.01267(10) Uani 1 1 d . . . C12 C 0.77500(5) 0.33504(3) 0.45573(4) 0.01765(11) Uani 1 1 d . . . H12 H 0.7854 0.3631 0.4207 0.021 Uiso 1 1 calc R . . C13 C 0.58376(5) 0.40108(3) 0.35453(4) 0.01602(10) Uani 1 1 d . . . H13 H 0.6511 0.4089 0.3436 0.019 Uiso 1 1 calc R . . C112 C -0.01782(6) 0.55069(3) 0.36540(4) 0.01765(11) Uani 1 1 d . . . H112 H 0.0345 0.5744 0.3936 0.021 Uiso 1 1 calc R . . C25 C 0.29300(6) 0.15393(3) 0.32131(5) 0.01979(12) Uani 1 1 d . . . H25 H 0.2961 0.1100 0.3171 0.024 Uiso 1 1 calc R . . C123 C -0.15395(6) 0.38580(4) -0.00604(4) 0.01923(12) Uani 1 1 d . . . H123 H -0.1799 0.3766 -0.0562 0.023 Uiso 1 1 calc R . . C127 C 0.28681(6) 0.46539(3) 0.14909(5) 0.01953(12) Uani 1 1 d . . . H12D H 0.3333 0.4361 0.1369 0.029 Uiso 1 1 calc R . . H12E H 0.2885 0.4632 0.2014 0.029 Uiso 1 1 calc R . . H12F H 0.3073 0.5049 0.1372 0.029 Uiso 1 1 calc R . . C110 C -0.19326(6) 0.52385(4) 0.32859(5) 0.02144(13) Uani 1 1 d . . . H110 H -0.2613 0.5293 0.3319 0.026 Uiso 1 1 calc R . . C104 C 0.01280(7) 0.25444(4) 0.36360(6) 0.02656(17) Uani 1 1 d . . . C126 C 0.17657(8) 0.44841(4) 0.02319(5) 0.02468(15) Uani 1 1 d . . . H12G H 0.2034 0.4849 0.0070 0.037 Uiso 1 1 calc R . . H12H H 0.1068 0.4426 -0.0044 0.037 Uiso 1 1 calc R . . H12I H 0.2180 0.4150 0.0146 0.037 Uiso 1 1 calc R . . C118 C 0.32651(6) 0.50157(4) 0.38361(5) 0.02604(17) Uani 1 1 d . . . H11A H 0.3738 0.5139 0.4288 0.039 Uiso 1 1 calc R . . H11B H 0.3386 0.5249 0.3426 0.039 Uiso 1 1 calc R . . H11C H 0.3366 0.4597 0.3748 0.039 Uiso 1 1 calc R . . C111 C -0.11735(6) 0.55885(4) 0.37047(5) 0.02100(13) Uani 1 1 d . . . H111 H -0.1334 0.5880 0.4022 0.025 Uiso 1 1 calc R . . C117 C 0.19632(7) 0.47418(4) 0.45344(4) 0.02397(15) Uani 1 1 d . . . H11D H 0.2033 0.4323 0.4428 0.036 Uiso 1 1 calc R . . H11E H 0.1274 0.4819 0.4584 0.036 Uiso 1 1 calc R . . H11F H 0.2444 0.4845 0.4991 0.036 Uiso 1 1 calc R . . C27 C 0.25964(7) 0.18050(4) 0.24472(5) 0.02759(17) Uani 1 1 d . . . H27A H 0.1931 0.1648 0.2207 0.041 Uiso 1 1 calc R . . H27B H 0.3087 0.1702 0.2160 0.041 Uiso 1 1 calc R . . H27C H 0.2557 0.2235 0.2485 0.041 Uiso 1 1 calc R . . C21 C 0.56294(6) 0.14535(3) 0.57231(4) 0.01714(11) Uani 1 1 d . . . H21 H 0.6117 0.1646 0.6093 0.021 Uiso 1 1 calc R . . C115 C 0.04535(7) 0.56393(4) 0.18283(5) 0.02198(14) Uani 1 1 d . . . H11G H -0.0049 0.5828 0.2052 0.033 Uiso 1 1 calc R . . H11H H 0.0197 0.5257 0.1624 0.033 Uiso 1 1 calc R . . H11I H 0.0585 0.5892 0.1438 0.033 Uiso 1 1 calc R . . C105 C -0.01009(8) 0.25127(4) 0.28751(6) 0.02635(16) Uani 1 1 d . . . C103 C 0.02536(7) 0.30902(4) 0.39745(5) 0.02345(15) Uani 1 1 d . . . C29 C 0.46918(7) 0.08309(4) 0.28360(5) 0.02348(14) Uani 1 1 d . . . H29A H 0.5189 0.0661 0.2592 0.035 Uiso 1 1 calc R . . H29B H 0.4038 0.0865 0.2485 0.035 Uiso 1 1 calc R . . H29C H 0.4622 0.0575 0.3241 0.035 Uiso 1 1 calc R . . C114 C 0.17651(8) 0.61357(4) 0.27985(5) 0.02689(17) Uani 1 1 d . . . H11J H 0.1776 0.6442 0.2433 0.040 Uiso 1 1 calc R . . H11K H 0.2442 0.6093 0.3117 0.040 Uiso 1 1 calc R . . H11L H 0.1286 0.6246 0.3093 0.040 Uiso 1 1 calc R . . C22 C 0.53152(7) 0.08868(3) 0.58517(4) 0.02052(13) Uani 1 1 d . . . H22 H 0.5597 0.0697 0.6303 0.025 Uiso 1 1 calc R . . C26 C 0.21783(6) 0.16992(4) 0.36748(6) 0.02811(18) Uani 1 1 d . . . H26A H 0.2130 0.2129 0.3707 0.042 Uiso 1 1 calc R . . H26B H 0.2411 0.1534 0.4167 0.042 Uiso 1 1 calc R . . H26C H 0.1513 0.1536 0.3447 0.042 Uiso 1 1 calc R . . H106 H -0.0413(9) 0.3005(6) 0.1941(7) 0.020(3) Uiso 1 1 d . . . H102 H 0.0177(9) 0.3979(6) 0.3810(7) 0.021(3) Uiso 1 1 d . . . H2 H 0.3482(9) 0.2437(6) 0.4864(7) 0.021(3) Uiso 1 1 d . . . H6 H 0.5892(10) 0.3505(6) 0.5634(7) 0.027(3) Uiso 1 1 d . . . H3 H 0.2381(10) 0.3146(6) 0.5142(7) 0.027(3) Uiso 1 1 d . . . H5 H 0.4834(10) 0.4159(6) 0.6058(7) 0.026(3) Uiso 1 1 d . . . H4 H 0.3081(10) 0.4003(6) 0.5789(8) 0.027(3) Uiso 1 1 d . . . H103 H 0.0385(10) 0.3107(6) 0.4490(8) 0.030(3) Uiso 1 1 d . . . H104 H 0.0212(11) 0.2198(7) 0.3928(8) 0.036(4) Uiso 1 1 d . . . H105 H -0.0208(11) 0.2136(7) 0.2631(9) 0.037(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.00990(3) 0.00894(3) 0.01010(3) 0.00099(2) 0.00259(2) 0.00136(2) Fe2 0.00851(3) 0.01094(3) 0.00998(3) -0.00063(2) 0.00190(2) 0.00125(2) P3 0.01070(6) 0.01194(6) 0.01164(6) -0.00132(5) 0.00269(5) 0.00156(5) P1 0.01026(6) 0.01128(6) 0.01109(6) 0.00062(5) 0.00269(5) 0.00039(5) P2 0.01317(6) 0.00954(6) 0.01260(6) 0.00025(5) 0.00166(5) 0.00041(5) P4 0.00975(6) 0.01381(6) 0.01059(6) -0.00136(5) 0.00227(5) 0.00050(5) N2 0.01116(19) 0.01186(19) 0.01167(19) -0.00013(15) 0.00278(15) 0.00098(15) N1 0.01121(19) 0.01064(18) 0.0123(2) 0.00062(15) 0.00320(15) 0.00096(15) C1 0.0151(2) 0.0124(2) 0.0110(2) 0.00075(17) 0.00414(18) 0.00331(18) C101 0.0105(2) 0.0145(2) 0.0155(2) 0.00045(18) 0.00428(18) -0.00060(18) C120 0.0105(2) 0.0141(2) 0.0127(2) -0.00001(18) 0.00191(17) -0.00014(17) C6 0.0186(3) 0.0146(2) 0.0161(3) -0.0027(2) 0.0049(2) 0.0026(2) C16 0.0138(2) 0.0168(2) 0.0120(2) 0.00033(18) 0.00404(18) 0.00103(19) C2 0.0156(2) 0.0149(2) 0.0146(2) 0.00172(19) 0.0066(2) 0.00228(19) C119 0.0114(2) 0.0177(3) 0.0116(2) -0.00095(19) 0.00138(17) 0.00064(19) C20 0.0169(2) 0.0123(2) 0.0118(2) 0.00120(17) 0.00549(19) 0.00457(18) C7 0.0111(2) 0.0152(2) 0.0128(2) -0.00119(18) 0.00189(17) 0.00131(18) C11 0.0120(2) 0.0261(3) 0.0213(3) -0.0065(3) 0.0008(2) 0.0011(2) C28 0.0193(3) 0.0127(2) 0.0129(2) -0.00136(18) 0.0027(2) 0.0024(2) C19 0.0178(3) 0.0105(2) 0.0148(2) 0.00190(18) 0.0057(2) 0.00243(19) C107 0.0126(2) 0.0145(2) 0.0131(2) -0.00085(18) 0.00383(18) 0.00287(18) C125 0.0182(3) 0.0155(2) 0.0149(3) -0.00024(19) 0.0068(2) -0.0001(2) C30 0.0188(3) 0.0181(3) 0.0166(3) -0.0007(2) 0.0036(2) 0.0059(2) C121 0.0110(2) 0.0217(3) 0.0151(3) 0.0014(2) 0.00219(19) 0.0000(2) C18 0.0171(3) 0.0213(3) 0.0127(2) 0.0009(2) 0.0026(2) -0.0020(2) C5 0.0261(3) 0.0156(3) 0.0199(3) -0.0034(2) 0.0087(3) 0.0045(2) C17 0.0152(3) 0.0338(4) 0.0172(3) -0.0014(3) 0.0070(2) -0.0031(3) C23 0.0304(4) 0.0125(2) 0.0238(3) 0.0056(2) 0.0166(3) 0.0059(2) C109 0.0119(2) 0.0227(3) 0.0203(3) -0.0024(2) 0.0049(2) 0.0023(2) C3 0.0178(3) 0.0206(3) 0.0200(3) 0.0027(2) 0.0102(2) 0.0054(2) C108 0.0115(2) 0.0150(2) 0.0133(2) 0.00026(18) 0.00352(18) 0.00197(18) C122 0.0121(2) 0.0257(3) 0.0158(3) 0.0021(2) -0.0001(2) -0.0021(2) C10 0.0149(3) 0.0252(3) 0.0180(3) -0.0035(2) -0.0021(2) 0.0067(2) C8 0.0132(2) 0.0137(2) 0.0120(2) -0.00130(17) 0.00184(18) 0.00416(18) B2 0.0116(2) 0.0138(3) 0.0124(3) -0.0002(2) 0.0028(2) 0.0007(2) C116 0.0145(2) 0.0173(3) 0.0160(3) -0.0046(2) 0.0010(2) 0.0012(2) C130 0.0176(3) 0.0168(3) 0.0245(3) -0.0042(2) 0.0058(2) -0.0019(2) C15 0.0262(3) 0.0167(3) 0.0192(3) 0.0057(2) 0.0069(3) 0.0042(2) C129 0.0135(2) 0.0188(3) 0.0222(3) -0.0048(2) 0.0048(2) 0.0015(2) C128 0.0133(2) 0.0155(2) 0.0143(2) -0.00337(19) 0.00349(19) 0.00012(19) C9 0.0170(3) 0.0197(3) 0.0148(3) 0.0004(2) -0.0002(2) 0.0061(2) C14 0.0245(3) 0.0144(3) 0.0247(3) -0.0039(2) 0.0014(3) 0.0015(2) C24 0.0242(3) 0.0113(2) 0.0215(3) 0.0022(2) 0.0099(3) 0.0014(2) C102 0.0181(3) 0.0202(3) 0.0153(3) 0.0031(2) 0.0048(2) 0.0022(2) C124 0.0154(3) 0.0264(3) 0.0120(2) -0.0025(2) 0.0013(2) 0.0012(2) C106 0.0199(3) 0.0147(3) 0.0219(3) -0.0007(2) 0.0070(2) -0.0013(2) C113 0.0207(3) 0.0133(2) 0.0184(3) 0.0003(2) 0.0084(2) 0.0015(2) C4 0.0250(3) 0.0187(3) 0.0205(3) 0.0011(2) 0.0119(3) 0.0087(2) B1 0.0146(3) 0.0123(2) 0.0113(2) -0.00004(19) 0.0032(2) 0.0031(2) C12 0.0127(2) 0.0215(3) 0.0184(3) -0.0024(2) 0.0028(2) -0.0013(2) C13 0.0161(3) 0.0125(2) 0.0201(3) 0.0018(2) 0.0055(2) -0.00060(19) C112 0.0175(3) 0.0178(3) 0.0184(3) -0.0040(2) 0.0056(2) 0.0037(2) C25 0.0165(3) 0.0135(2) 0.0264(3) 0.0004(2) -0.0012(2) -0.0024(2) C123 0.0154(3) 0.0270(3) 0.0133(3) -0.0008(2) -0.0008(2) -0.0015(2) C127 0.0166(3) 0.0187(3) 0.0254(3) -0.0036(2) 0.0093(2) -0.0032(2) C110 0.0148(3) 0.0268(3) 0.0241(3) -0.0030(3) 0.0074(2) 0.0063(2) C104 0.0281(4) 0.0215(3) 0.0345(4) 0.0130(3) 0.0163(3) 0.0061(3) C126 0.0351(4) 0.0246(3) 0.0168(3) 0.0011(3) 0.0111(3) -0.0035(3) C118 0.0137(3) 0.0319(4) 0.0302(4) -0.0150(3) 0.0001(3) 0.0016(3) C111 0.0200(3) 0.0229(3) 0.0219(3) -0.0043(2) 0.0085(2) 0.0067(2) C117 0.0288(4) 0.0240(3) 0.0153(3) 0.0003(2) -0.0028(3) -0.0004(3) C27 0.0273(4) 0.0203(3) 0.0271(4) 0.0007(3) -0.0102(3) -0.0028(3) C21 0.0230(3) 0.0175(3) 0.0121(2) 0.0031(2) 0.0067(2) 0.0067(2) C115 0.0256(3) 0.0218(3) 0.0195(3) 0.0065(2) 0.0072(3) 0.0074(3) C105 0.0321(4) 0.0147(3) 0.0351(4) 0.0033(3) 0.0134(3) 0.0002(3) C103 0.0237(3) 0.0282(4) 0.0207(3) 0.0106(3) 0.0095(3) 0.0068(3) C29 0.0318(4) 0.0152(3) 0.0225(3) -0.0067(2) 0.0042(3) 0.0009(3) C114 0.0406(5) 0.0139(3) 0.0288(4) -0.0019(3) 0.0135(4) -0.0030(3) C22 0.0296(4) 0.0182(3) 0.0173(3) 0.0074(2) 0.0129(3) 0.0098(3) C26 0.0159(3) 0.0227(3) 0.0459(5) 0.0015(3) 0.0075(3) -0.0026(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.8262(6) . ? Fe1 C1 2.2516(7) . ? Fe1 C2 2.2714(7) . ? Fe1 P1 2.3182(2) . ? Fe1 B1 2.3739(7) . ? Fe1 P2 2.3749(2) . ? Fe2 N2 1.8382(6) . ? Fe2 C101 2.2133(6) . ? Fe2 B2 2.3134(7) . ? Fe2 P4 2.3381(2) . ? Fe2 P3 2.3439(2) . ? Fe2 C102 2.6645(7) . ? P3 C107 1.8174(7) . ? P3 C116 1.8548(7) . ? P3 C113 1.8858(7) . ? P1 C7 1.8282(7) . ? P1 C13 1.8607(7) . ? P1 C16 1.8713(7) . ? P2 C19 1.8151(7) . ? P2 C25 1.8504(8) . ? P2 C28 1.8819(7) . ? P4 C119 1.8238(7) . ? P4 C128 1.8650(7) . ? P4 C125 1.8676(7) . ? N2 N1 1.1704(8) . ? C1 C2 1.4211(10) . ? C1 C6 1.4304(10) . ? C1 B1 1.5626(9) . ? C101 C106 1.4169(10) . ? C101 C102 1.4184(10) . ? C101 B2 1.5788(10) . ? C120 C121 1.4103(9) . ? C120 C119 1.4141(9) . ? C120 B2 1.6022(10) . ? C6 C5 1.3784(10) . ? C6 H6 0.952(13) . ? C16 C17 1.5332(10) . ? C16 C18 1.5340(10) . ? C16 H16 1.0000 . ? C2 C3 1.4186(10) . ? C2 H2 0.936(13) . ? C119 C124 1.4039(10) . ? C20 C19 1.4067(10) . ? C20 C21 1.4080(9) . ? C20 B1 1.6041(10) . ? C7 C12 1.4044(10) . ? C7 C8 1.4105(10) . ? C11 C10 1.3884(13) . ? C11 C12 1.3904(11) . ? C11 H11 0.9500 . ? C28 C29 1.5323(10) . ? C28 C30 1.5342(10) . ? C28 H28 1.0000 . ? C19 C24 1.4037(10) . ? C107 C112 1.4019(9) . ? C107 C108 1.4061(10) . ? C125 C126 1.5301(11) . ? C125 C127 1.5368(11) . ? C125 H125 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C121 C122 1.3900(10) . ? C121 H121 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C5 C4 1.4125(12) . ? C5 H5 0.956(14) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C23 C22 1.3896(13) . ? C23 C24 1.3922(11) . ? C23 H23 0.9500 . ? C109 C110 1.3924(11) . ? C109 C108 1.4087(9) . ? C109 H109 0.9500 . ? C3 C4 1.3709(12) . ? C3 H3 0.981(13) . ? C108 B2 1.6072(10) . ? C122 C123 1.3944(11) . ? C122 H122 0.9500 . ? C10 C9 1.3908(11) . ? C10 H10 0.9500 . ? C8 C9 1.4090(10) . ? C8 B1 1.5958(10) . ? C116 C117 1.5295(12) . ? C116 C118 1.5311(11) . ? C116 H116 1.0000 . ? C130 C128 1.5319(10) . ? C130 H13A 0.9800 . ? C130 H13B 0.9800 . ? C130 H13C 0.9800 . ? C15 C13 1.5320(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C129 C128 1.5335(10) . ? C129 H12A 0.9800 . ? C129 H12B 0.9800 . ? C129 H12C 0.9800 . ? C128 H128 1.0000 . ? C9 H9 0.9500 . ? C14 C13 1.5280(11) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C24 H24 0.9500 . ? C102 C103 1.3984(11) . ? C102 H102 0.960(13) . ? C124 C123 1.3878(10) . ? C124 H124 0.9500 . ? C106 C105 1.3888(12) . ? C106 H106 0.952(13) . ? C113 C114 1.5355(11) . ? C113 C115 1.5364(12) . ? C113 H113 1.0000 . ? C4 H4 0.961(13) . ? C12 H12 0.9500 . ? C13 H13 1.0000 . ? C112 C111 1.3919(11) . ? C112 H112 0.9500 . ? C25 C27 1.5301(12) . ? C25 C26 1.5305(13) . ? C25 H25 1.0000 . ? C123 H123 0.9500 . ? C127 H12D 0.9800 . ? C127 H12E 0.9800 . ? C127 H12F 0.9800 . ? C110 C111 1.3932(12) . ? C110 H110 0.9500 . ? C104 C103 1.3842(14) . ? C104 C105 1.3943(15) . ? C104 H104 0.949(15) . ? C126 H12G 0.9800 . ? C126 H12H 0.9800 . ? C126 H12I 0.9800 . ? C118 H11A 0.9800 . ? C118 H11B 0.9800 . ? C118 H11C 0.9800 . ? C111 H111 0.9500 . ? C117 H11D 0.9800 . ? C117 H11E 0.9800 . ? C117 H11F 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C21 C22 1.3930(11) . ? C21 H21 0.9500 . ? C115 H11G 0.9800 . ? C115 H11H 0.9800 . ? C115 H11I 0.9800 . ? C105 H105 0.964(15) . ? C103 H103 0.945(14) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C114 H11J 0.9800 . ? C114 H11K 0.9800 . ? C114 H11L 0.9800 . ? C22 H22 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 C1 124.27(2) . . ? N1 Fe1 C2 96.92(2) . . ? C1 Fe1 C2 36.62(2) . . ? N1 Fe1 P1 109.088(18) . . ? C1 Fe1 P1 95.653(18) . . ? C2 Fe1 P1 130.817(19) . . ? N1 Fe1 B1 163.55(2) . . ? C1 Fe1 B1 39.38(2) . . ? C2 Fe1 B1 67.78(2) . . ? P1 Fe1 B1 78.859(19) . . ? N1 Fe1 P2 112.662(18) . . ? C1 Fe1 P2 106.407(17) . . ? C2 Fe1 P2 100.549(18) . . ? P1 Fe1 P2 106.358(7) . . ? B1 Fe1 P2 77.398(18) . . ? N2 Fe2 C101 120.30(2) . . ? N2 Fe2 B2 161.02(3) . . ? C101 Fe2 B2 40.75(3) . . ? N2 Fe2 P4 107.992(18) . . ? C101 Fe2 P4 102.389(18) . . ? B2 Fe2 P4 81.893(19) . . ? N2 Fe2 P3 114.099(18) . . ? C101 Fe2 P3 103.437(18) . . ? B2 Fe2 P3 76.606(19) . . ? P4 Fe2 P3 107.462(7) . . ? N2 Fe2 C102 99.82(2) . . ? C101 Fe2 C102 32.15(2) . . ? B2 Fe2 C102 63.03(2) . . ? P4 Fe2 C102 134.419(18) . . ? P3 Fe2 C102 92.452(18) . . ? C107 P3 C116 104.68(3) . . ? C107 P3 C113 100.64(3) . . ? C116 P3 C113 103.42(3) . . ? C107 P3 Fe2 107.71(2) . . ? C116 P3 Fe2 114.91(2) . . ? C113 P3 Fe2 123.23(2) . . ? C7 P1 C13 102.69(3) . . ? C7 P1 C16 103.28(3) . . ? C13 P1 C16 104.16(3) . . ? C7 P1 Fe1 110.39(2) . . ? C13 P1 Fe1 119.32(2) . . ? C16 P1 Fe1 115.16(2) . . ? C19 P2 C25 104.79(4) . . ? C19 P2 C28 100.98(3) . . ? C25 P2 C28 103.19(4) . . ? C19 P2 Fe1 105.02(2) . . ? C25 P2 Fe1 115.04(3) . . ? C28 P2 Fe1 125.31(2) . . ? C119 P4 C128 103.90(3) . . ? C119 P4 C125 104.20(3) . . ? C128 P4 C125 102.92(3) . . ? C119 P4 Fe2 107.06(2) . . ? C128 P4 Fe2 120.85(2) . . ? C125 P4 Fe2 116.15(2) . . ? N1 N2 Fe2 175.87(5) . . ? N2 N1 Fe1 175.21(5) . . ? C2 C1 C6 116.07(6) . . ? C2 C1 B1 120.52(6) . . ? C6 C1 B1 123.29(6) . . ? C2 C1 Fe1 72.45(4) . . ? C6 C1 Fe1 121.29(5) . . ? B1 C1 Fe1 74.54(4) . . ? C106 C101 C102 115.93(6) . . ? C106 C101 B2 122.29(6) . . ? C102 C101 B2 121.72(6) . . ? C106 C101 Fe2 103.90(5) . . ? C102 C101 Fe2 91.72(4) . . ? B2 C101 Fe2 73.03(4) . . ? C121 C120 C119 116.49(6) . . ? C121 C120 B2 121.90(6) . . ? C119 C120 B2 121.45(6) . . ? C5 C6 C1 121.91(7) . . ? C5 C6 H6 119.7(8) . . ? C1 C6 H6 118.4(8) . . ? C17 C16 C18 111.32(6) . . ? C17 C16 P1 116.19(5) . . ? C18 C16 P1 111.68(5) . . ? C17 C16 H16 105.6 . . ? C18 C16 H16 105.6 . . ? P1 C16 H16 105.6 . . ? C3 C2 C1 121.42(7) . . ? C3 C2 Fe1 124.66(5) . . ? C1 C2 Fe1 70.93(4) . . ? C3 C2 H2 118.2(8) . . ? C1 C2 H2 119.4(8) . . ? Fe1 C2 H2 84.8(8) . . ? C124 C119 C120 121.25(6) . . ? C124 C119 P4 123.44(5) . . ? C120 C119 P4 115.30(5) . . ? C19 C20 C21 116.73(6) . . ? C19 C20 B1 120.89(6) . . ? C21 C20 B1 122.21(6) . . ? C12 C7 C8 121.23(6) . . ? C12 C7 P1 124.05(5) . . ? C8 C7 P1 114.69(5) . . ? C10 C11 C12 119.71(7) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C29 C28 C30 108.46(6) . . ? C29 C28 P2 115.12(6) . . ? C30 C28 P2 110.68(5) . . ? C29 C28 H28 107.4 . . ? C30 C28 H28 107.4 . . ? P2 C28 H28 107.4 . . ? C24 C19 C20 121.87(6) . . ? C24 C19 P2 124.99(6) . . ? C20 C19 P2 113.01(5) . . ? C112 C107 C108 121.97(6) . . ? C112 C107 P3 125.64(5) . . ? C108 C107 P3 112.37(5) . . ? C126 C125 C127 110.67(6) . . ? C126 C125 P4 115.64(5) . . ? C127 C125 P4 111.55(5) . . ? C126 C125 H125 106.1 . . ? C127 C125 H125 106.1 . . ? P4 C125 H125 106.1 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C122 C121 C120 122.12(6) . . ? C122 C121 H121 118.9 . . ? C120 C121 H121 118.9 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C6 C5 C4 120.28(7) . . ? C6 C5 H5 120.4(8) . . ? C4 C5 H5 119.4(8) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C22 C23 C24 119.49(7) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C110 C109 C108 121.53(7) . . ? C110 C109 H109 119.2 . . ? C108 C109 H109 119.2 . . ? C4 C3 C2 120.16(7) . . ? C4 C3 H3 121.0(8) . . ? C2 C3 H3 118.8(8) . . ? C107 C108 C109 116.81(6) . . ? C107 C108 B2 118.48(5) . . ? C109 C108 B2 124.27(6) . . ? C121 C122 C123 120.29(7) . . ? C121 C122 H122 119.9 . . ? C123 C122 H122 119.9 . . ? C11 C10 C9 120.41(7) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C9 C8 C7 117.11(6) . . ? C9 C8 B1 122.85(6) . . ? C7 C8 B1 119.38(6) . . ? C101 B2 C120 117.42(6) . . ? C101 B2 C108 111.94(6) . . ? C120 B2 C108 121.75(6) . . ? C101 B2 Fe2 66.22(3) . . ? C120 B2 Fe2 112.59(4) . . ? C108 B2 Fe2 114.26(4) . . ? C117 C116 C118 110.51(7) . . ? C117 C116 P3 110.33(5) . . ? C118 C116 P3 108.99(5) . . ? C117 C116 H116 109.0 . . ? C118 C116 H116 109.0 . . ? P3 C116 H116 109.0 . . ? C128 C130 H13A 109.5 . . ? C128 C130 H13B 109.5 . . ? H13A C130 H13B 109.5 . . ? C128 C130 H13C 109.5 . . ? H13A C130 H13C 109.5 . . ? H13B C130 H13C 109.5 . . ? 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 . . ? C128 C129 H12A 109.5 . . ? C128 C129 H12B 109.5 . . ? H12A C129 H12B 109.5 . . ? C128 C129 H12C 109.5 . . ? H12A C129 H12C 109.5 . . ? H12B C129 H12C 109.5 . . ? C130 C128 C129 111.27(6) . . ? C130 C128 P4 111.11(5) . . ? C129 C128 P4 110.21(5) . . ? C130 C128 H128 108.0 . . ? C129 C128 H128 108.0 . . ? P4 C128 H128 108.0 . . ? C10 C9 C8 121.51(7) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? 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 . . ? C23 C24 C19 119.71(8) . . ? C23 C24 H24 120.1 . . ? C19 C24 H24 120.1 . . ? C103 C102 C101 121.66(8) . . ? C103 C102 Fe2 122.86(5) . . ? C101 C102 Fe2 56.13(4) . . ? C103 C102 H102 118.3(8) . . ? C101 C102 H102 119.9(8) . . ? Fe2 C102 H102 93.7(8) . . ? C123 C124 C119 120.55(7) . . ? C123 C124 H124 119.7 . . ? C119 C124 H124 119.7 . . ? C105 C106 C101 122.10(8) . . ? C105 C106 H106 120.3(8) . . ? C101 C106 H106 117.4(8) . . ? C114 C113 C115 109.28(7) . . ? C114 C113 P3 114.92(6) . . ? C115 C113 P3 110.36(5) . . ? C114 C113 H113 107.3 . . ? C115 C113 H113 107.3 . . ? P3 C113 H113 107.3 . . ? C3 C4 C5 119.89(7) . . ? C3 C4 H4 121.0(8) . . ? C5 C4 H4 119.1(8) . . ? C1 B1 C8 114.10(6) . . ? C1 B1 C20 114.79(6) . . ? C8 B1 C20 123.09(6) . . ? C1 B1 Fe1 66.09(3) . . ? C8 B1 Fe1 114.94(4) . . ? C20 B1 Fe1 110.20(5) . . ? C11 C12 C7 119.97(7) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C14 C13 C15 110.53(6) . . ? C14 C13 P1 109.96(5) . . ? C15 C13 P1 111.03(5) . . ? C14 C13 H13 108.4 . . ? C15 C13 H13 108.4 . . ? P1 C13 H13 108.4 . . ? C111 C112 C107 119.73(7) . . ? C111 C112 H112 120.1 . . ? C107 C112 H112 120.1 . . ? C27 C25 C26 110.42(8) . . ? C27 C25 P2 109.25(6) . . ? C26 C25 P2 109.94(6) . . ? C27 C25 H25 109.1 . . ? C26 C25 H25 109.1 . . ? P2 C25 H25 109.1 . . ? C124 C123 C122 119.21(7) . . ? C124 C123 H123 120.4 . . ? C122 C123 H123 120.4 . . ? C125 C127 H12D 109.5 . . ? C125 C127 H12E 109.5 . . ? H12D C127 H12E 109.5 . . ? C125 C127 H12F 109.5 . . ? H12D C127 H12F 109.5 . . ? H12E C127 H12F 109.5 . . ? C109 C110 C111 120.52(7) . . ? C109 C110 H110 119.7 . . ? C111 C110 H110 119.7 . . ? C103 C104 C105 119.51(8) . . ? C103 C104 H104 119.2(9) . . ? C105 C104 H104 121.3(9) . . ? C125 C126 H12G 109.5 . . ? C125 C126 H12H 109.5 . . ? H12G C126 H12H 109.5 . . ? C125 C126 H12I 109.5 . . ? H12G C126 H12I 109.5 . . ? H12H C126 H12I 109.5 . . ? C116 C118 H11A 109.5 . . ? C116 C118 H11B 109.5 . . ? H11A C118 H11B 109.5 . . ? C116 C118 H11C 109.5 . . ? H11A C118 H11C 109.5 . . ? H11B C118 H11C 109.5 . . ? C112 C111 C110 119.44(7) . . ? C112 C111 H111 120.3 . . ? C110 C111 H111 120.3 . . ? C116 C117 H11D 109.5 . . ? C116 C117 H11E 109.5 . . ? H11D C117 H11E 109.5 . . ? C116 C117 H11F 109.5 . . ? H11D C117 H11F 109.5 . . ? H11E C117 H11F 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C22 C21 C20 121.62(7) . . ? C22 C21 H21 119.2 . . ? C20 C21 H21 119.2 . . ? C113 C115 H11G 109.5 . . ? C113 C115 H11H 109.5 . . ? H11G C115 H11H 109.5 . . ? C113 C115 H11I 109.5 . . ? H11G C115 H11I 109.5 . . ? H11H C115 H11I 109.5 . . ? C106 C105 C104 120.19(8) . . ? C106 C105 H105 119.2(9) . . ? C104 C105 H105 120.5(9) . . ? C104 C103 C102 120.40(8) . . ? C104 C103 H103 118.9(9) . . ? C102 C103 H103 120.6(9) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C113 C114 H11J 109.5 . . ? C113 C114 H11K 109.5 . . ? H11J C114 H11K 109.5 . . ? C113 C114 H11L 109.5 . . ? H11J C114 H11L 109.5 . . ? H11K C114 H11L 109.5 . . ? C23 C22 C21 120.50(7) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.972 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.082 ####################################################### # Compound 8: (iPrDPBH)FeNSiNSi2 # ####################################################### data_8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H65 B Fe N2 P2 Si3' _chemical_formula_weight 810.83 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' 'Si' 'Si' 0.0817 0.0704 '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 10.167(15) _cell_length_b 12.843(12) _cell_length_c 18.21(3) _cell_angle_alpha 99.79(5) _cell_angle_beta 95.23(5) _cell_angle_gamma 101.42(5) _cell_volume 2277(5) _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 plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 0.510 _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 0.073 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11316 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 24.55 _reflns_number_total 5912 _reflns_number_gt 4737 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1124P)^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 5912 _refine_ls_number_parameters 485 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1615 _refine_ls_wR_factor_gt 0.1547 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.28672(5) 0.16791(4) 0.22982(3) 0.03731(19) Uani 1 1 d . . . P2 P 0.28325(9) -0.03080(7) 0.19585(5) 0.0378(2) Uani 1 1 d . . . P1 P 0.13894(9) 0.20418(8) 0.32376(6) 0.0421(3) Uani 1 1 d . . . Si3 Si 0.29402(11) 0.46518(8) 0.15221(7) 0.0464(3) Uani 1 1 d . . . Si2 Si 0.20685(11) 0.26506(9) 0.03932(6) 0.0458(3) Uani 1 1 d . . . Si1 Si 0.54158(10) 0.28111(9) 0.16385(7) 0.0467(3) Uani 1 1 d . . . N2 N 0.2976(3) 0.3288(2) 0.12618(19) 0.0427(7) Uani 1 1 d . . . C20 C 0.4923(3) 0.0169(3) 0.3166(2) 0.0371(8) Uani 1 1 d . . . C10 C 0.1645(4) -0.0890(3) 0.4381(2) 0.0468(9) Uani 1 1 d . . . H10 H 0.1697 -0.1496 0.4609 0.056 Uiso 1 1 calc R . . C13 C 0.1795(4) 0.3300(3) 0.3979(3) 0.0522(10) Uani 1 1 d . . . H13 H 0.1457 0.3870 0.3753 0.063 Uiso 1 1 calc R . . N1 N 0.3713(3) 0.2662(2) 0.17101(18) 0.0411(7) Uani 1 1 d . . . C7 C 0.1527(3) 0.0917(3) 0.3727(2) 0.0403(8) Uani 1 1 d . . . C30 C 0.3900(5) -0.0136(4) 0.0640(3) 0.0612(11) Uani 1 1 d . . . H30A H 0.4751 -0.0287 0.0847 0.092 Uiso 1 1 calc R . . H30B H 0.3912 0.0635 0.0799 0.092 Uiso 1 1 calc R . . H30C H 0.3797 -0.0321 0.0090 0.092 Uiso 1 1 calc R . . C9 C 0.2793(4) -0.0293(3) 0.4176(2) 0.0436(9) Uani 1 1 d . . . H9 H 0.3627 -0.0503 0.4276 0.052 Uiso 1 1 calc R . . C27 C 0.0130(4) -0.1521(3) 0.1710(2) 0.0484(9) Uani 1 1 d . . . H27A H 0.0169 -0.2091 0.1285 0.073 Uiso 1 1 calc R . . H27B H 0.0026 -0.0864 0.1524 0.073 Uiso 1 1 calc R . . H27C H -0.0644 -0.1763 0.1970 0.073 Uiso 1 1 calc R . . C28 C 0.2733(4) -0.0803(3) 0.0924(2) 0.0449(9) Uani 1 1 d . . . H28 H 0.1906 -0.0603 0.0698 0.054 Uiso 1 1 calc R . . C21 C 0.6061(4) -0.0081(3) 0.3556(2) 0.0462(9) Uani 1 1 d . . . H21 H 0.6440 0.0344 0.4036 0.055 Uiso 1 1 calc R . . C29 C 0.2571(4) -0.2011(3) 0.0601(2) 0.0517(10) Uani 1 1 d . . . H29A H 0.2200 -0.2161 0.0069 0.078 Uiso 1 1 calc R . . H29B H 0.1955 -0.2438 0.0876 0.078 Uiso 1 1 calc R . . H29C H 0.3456 -0.2204 0.0652 0.078 Uiso 1 1 calc R . . C22 C 0.6640(4) -0.0934(3) 0.3255(3) 0.0503(10) Uani 1 1 d . . . H22 H 0.7386 -0.1092 0.3535 0.060 Uiso 1 1 calc R . . C19 C 0.4413(3) -0.0494(3) 0.2453(2) 0.0380(8) Uani 1 1 d . . . C8 C 0.2803(3) 0.0606(3) 0.3827(2) 0.0376(8) Uani 1 1 d . . . C6 C 0.5129(4) 0.2005(3) 0.5014(3) 0.0551(11) Uani 1 1 d . . . H6 H 0.4383 0.1530 0.5145 0.066 Uiso 1 1 calc R . . C25 C 0.1453(3) -0.1273(3) 0.2263(2) 0.0427(9) Uani 1 1 d . . . H25 H 0.1245 -0.0877 0.2745 0.051 Uiso 1 1 calc R . . C38 C 0.2827(5) 0.5052(4) 0.2536(3) 0.0618(12) Uani 1 1 d . . . H38A H 0.1943 0.4695 0.2648 0.093 Uiso 1 1 calc R . . H38B H 0.2932 0.5839 0.2666 0.093 Uiso 1 1 calc R . . H38C H 0.3545 0.4834 0.2831 0.093 Uiso 1 1 calc R . . C24 C 0.5025(4) -0.1322(3) 0.2152(3) 0.0474(9) Uani 1 1 d . . . H24 H 0.4680 -0.1741 0.1666 0.057 Uiso 1 1 calc R . . C12 C 0.0369(4) 0.0330(3) 0.3942(2) 0.0460(9) Uani 1 1 d . . . H12 H -0.0461 0.0558 0.3879 0.055 Uiso 1 1 calc R . . C23 C 0.6131(4) -0.1543(3) 0.2553(3) 0.0494(10) Uani 1 1 d . . . H23 H 0.6536 -0.2112 0.2343 0.059 Uiso 1 1 calc R . . C5 C 0.6032(6) 0.2739(4) 0.5596(3) 0.0678(15) Uani 1 1 d . . . H5 H 0.5890 0.2766 0.6107 0.081 Uiso 1 1 calc R . . C16 C -0.0448(4) 0.1924(3) 0.2928(3) 0.0534(11) Uani 1 1 d . . . H16 H -0.0950 0.1917 0.3375 0.064 Uiso 1 1 calc R . . C37 C 0.4376(4) 0.5602(4) 0.1257(3) 0.0641(13) Uani 1 1 d . . . H37A H 0.5202 0.5642 0.1592 0.096 Uiso 1 1 calc R . . H37B H 0.4171 0.6323 0.1302 0.096 Uiso 1 1 calc R . . H37C H 0.4508 0.5341 0.0737 0.096 Uiso 1 1 calc R . . C36 C 0.7521(4) 0.4684(4) 0.1737(3) 0.0558(11) Uani 1 1 d . . . H36 H 0.7634 0.4363 0.1243 0.067 Uiso 1 1 calc R . . C11 C 0.0414(4) -0.0595(3) 0.4250(2) 0.0488(9) Uani 1 1 d . . . H11 H -0.0390 -0.1015 0.4369 0.059 Uiso 1 1 calc R . . C4 C 0.7128(5) 0.3418(4) 0.5405(3) 0.0713(16) Uani 1 1 d . . . H4 H 0.7755 0.3908 0.5790 0.086 Uiso 1 1 calc R . . C35 C 0.8359(5) 0.5677(4) 0.2085(3) 0.0668(13) Uani 1 1 d . . . H35 H 0.9038 0.6029 0.1829 0.080 Uiso 1 1 calc R . . C15 C 0.1063(5) 0.3169(4) 0.4663(3) 0.0757(14) Uani 1 1 d . . . H15A H 0.1439 0.2677 0.4935 0.114 Uiso 1 1 calc R . . H15B H 0.0097 0.2870 0.4498 0.114 Uiso 1 1 calc R . . H15C H 0.1182 0.3877 0.4994 0.114 Uiso 1 1 calc R . . C33 C 0.7211(5) 0.5643(4) 0.3171(3) 0.0674(13) Uani 1 1 d . . . H33 H 0.7096 0.5975 0.3661 0.081 Uiso 1 1 calc R . . C34 C 0.8196(5) 0.6140(4) 0.2794(3) 0.0723(15) Uani 1 1 d . . . H34 H 0.8770 0.6814 0.3031 0.087 Uiso 1 1 calc R . . C26 C 0.1836(4) -0.2303(3) 0.2447(2) 0.0498(10) Uani 1 1 d . . . H26A H 0.1098 -0.2708 0.2664 0.075 Uiso 1 1 calc R . . H26B H 0.2661 -0.2107 0.2809 0.075 Uiso 1 1 calc R . . H26C H 0.1995 -0.2752 0.1986 0.075 Uiso 1 1 calc R . . C2 C 0.6418(4) 0.2647(3) 0.4097(3) 0.0517(11) Uani 1 1 d . . . H2 H 0.6582 0.2618 0.3589 0.062 Uiso 1 1 calc R . . C18 C -0.1040(4) 0.0887(4) 0.2349(3) 0.0561(11) Uani 1 1 d . . . H18A H -0.2017 0.0815 0.2232 0.084 Uiso 1 1 calc R . . H18B H -0.0867 0.0262 0.2554 0.084 Uiso 1 1 calc R . . H18C H -0.0613 0.0919 0.1889 0.084 Uiso 1 1 calc R . . C17 C -0.0634(5) 0.2905(4) 0.2576(3) 0.0664(13) Uani 1 1 d . . . H17A H -0.0103 0.2942 0.2155 0.100 Uiso 1 1 calc R . . H17B H -0.0324 0.3571 0.2956 0.100 Uiso 1 1 calc R . . H17C H -0.1593 0.2826 0.2395 0.100 Uiso 1 1 calc R . . C42 C 0.3116(4) 0.2169(4) -0.0326(3) 0.0583(11) Uani 1 1 d . . . H42A H 0.3809 0.2781 -0.0396 0.087 Uiso 1 1 calc R . . H42B H 0.2537 0.1851 -0.0804 0.087 Uiso 1 1 calc R . . H42C H 0.3554 0.1621 -0.0157 0.087 Uiso 1 1 calc R . . C14 C 0.3293(4) 0.3725(3) 0.4221(3) 0.0572(11) Uani 1 1 d . . . H14A H 0.3450 0.4454 0.4527 0.086 Uiso 1 1 calc R . . H14B H 0.3763 0.3752 0.3775 0.086 Uiso 1 1 calc R . . H14C H 0.3640 0.3245 0.4517 0.086 Uiso 1 1 calc R . . C41 C 0.0722(4) 0.1492(3) 0.0510(3) 0.0564(11) Uani 1 1 d . . . H41A H 0.1112 0.1055 0.0826 0.085 Uiso 1 1 calc R . . H41B H 0.0344 0.1044 0.0017 0.085 Uiso 1 1 calc R . . H41C H 0.0003 0.1770 0.0750 0.085 Uiso 1 1 calc R . . C1 C 0.5281(4) 0.1946(3) 0.4260(2) 0.0444(9) Uani 1 1 d . . . C40 C 0.1371(4) 0.3833(3) 0.0141(3) 0.0540(11) Uani 1 1 d . . . H40A H 0.1953 0.4208 -0.0184 0.065 Uiso 1 1 calc R . . H40B H 0.0446 0.3570 -0.0133 0.065 Uiso 1 1 calc R . . C39 C 0.1348(4) 0.4618(3) 0.0886(2) 0.0525(10) Uani 1 1 d . . . H39A H 0.0537 0.4359 0.1122 0.063 Uiso 1 1 calc R . . H39B H 0.1329 0.5351 0.0789 0.063 Uiso 1 1 calc R . . C31 C 0.6511(4) 0.4155(3) 0.2106(3) 0.0506(10) Uani 1 1 d . . . B1 B 0.4241(4) 0.1134(3) 0.3573(2) 0.0374(9) Uani 1 1 d . . . C3 C 0.7323(5) 0.3395(3) 0.4672(3) 0.0649(14) Uani 1 1 d . . . H3 H 0.8065 0.3880 0.4548 0.078 Uiso 1 1 calc R . . C32 C 0.6380(4) 0.4641(4) 0.2821(3) 0.0541(11) Uani 1 1 d . . . H32 H 0.5712 0.4291 0.3083 0.065 Uiso 1 1 calc R . . H101 H 0.581(3) 0.211(3) 0.202(2) 0.036(9) Uiso 1 1 d . . . H103 H 0.398(4) 0.162(3) 0.309(2) 0.045(10) Uiso 1 1 d . . . H102 H 0.588(5) 0.281(5) 0.090(3) 0.092(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0336(3) 0.0284(3) 0.0497(3) 0.0096(2) -0.0025(2) 0.0082(2) P2 0.0380(5) 0.0293(5) 0.0458(6) 0.0072(4) -0.0011(4) 0.0095(4) P1 0.0379(5) 0.0376(6) 0.0541(6) 0.0107(4) -0.0004(4) 0.0170(4) Si3 0.0481(6) 0.0287(6) 0.0596(7) 0.0070(5) -0.0112(5) 0.0110(4) Si2 0.0463(6) 0.0332(6) 0.0548(7) 0.0082(5) -0.0106(5) 0.0094(4) Si1 0.0352(5) 0.0360(6) 0.0676(8) 0.0124(5) -0.0026(5) 0.0068(4) N2 0.0419(16) 0.0293(17) 0.056(2) 0.0121(14) -0.0081(14) 0.0102(13) C20 0.0298(16) 0.029(2) 0.053(2) 0.0111(16) 0.0017(14) 0.0077(14) C10 0.059(2) 0.041(2) 0.045(2) 0.0142(17) 0.0026(17) 0.0200(18) C13 0.054(2) 0.037(2) 0.068(3) 0.0076(19) 0.0000(19) 0.0202(18) N1 0.0383(15) 0.0286(17) 0.056(2) 0.0125(14) -0.0080(13) 0.0101(12) C7 0.0394(18) 0.041(2) 0.043(2) 0.0082(16) 0.0007(15) 0.0168(16) C30 0.065(3) 0.051(3) 0.067(3) 0.008(2) 0.011(2) 0.012(2) C9 0.0434(19) 0.041(2) 0.048(2) 0.0067(17) -0.0022(16) 0.0183(17) C27 0.0417(19) 0.046(2) 0.054(2) 0.0076(18) -0.0046(17) 0.0069(17) C28 0.047(2) 0.040(2) 0.047(2) 0.0069(17) 0.0005(16) 0.0106(16) C21 0.0366(18) 0.035(2) 0.066(3) 0.0119(18) -0.0035(17) 0.0104(16) C29 0.053(2) 0.049(3) 0.053(2) 0.0065(19) 0.0014(18) 0.0163(19) C22 0.0324(18) 0.041(2) 0.080(3) 0.016(2) -0.0047(18) 0.0144(16) C19 0.0333(16) 0.031(2) 0.050(2) 0.0089(15) 0.0000(15) 0.0089(14) C8 0.0411(18) 0.032(2) 0.0383(19) -0.0007(14) -0.0028(14) 0.0162(15) C6 0.063(2) 0.038(2) 0.063(3) 0.0046(19) -0.019(2) 0.024(2) C25 0.0382(18) 0.039(2) 0.048(2) 0.0070(16) -0.0037(15) 0.0080(16) C38 0.074(3) 0.041(2) 0.067(3) 0.006(2) -0.015(2) 0.022(2) C24 0.0417(19) 0.033(2) 0.067(3) 0.0076(18) 0.0033(17) 0.0102(16) C12 0.0404(19) 0.053(3) 0.050(2) 0.0113(18) 0.0055(16) 0.0204(18) C23 0.0418(19) 0.036(2) 0.070(3) 0.0036(19) 0.0014(18) 0.0168(17) C5 0.095(4) 0.039(3) 0.062(3) -0.004(2) -0.031(3) 0.030(3) C16 0.043(2) 0.050(3) 0.073(3) 0.019(2) 0.0012(19) 0.0211(18) C37 0.061(2) 0.036(2) 0.094(4) 0.021(2) -0.008(2) 0.008(2) C36 0.044(2) 0.045(3) 0.078(3) 0.020(2) -0.0048(19) 0.0058(18) C11 0.047(2) 0.051(3) 0.053(2) 0.0156(19) 0.0107(17) 0.0123(18) C4 0.080(3) 0.035(3) 0.085(4) -0.007(2) -0.043(3) 0.021(2) C35 0.052(2) 0.045(3) 0.097(4) 0.014(3) -0.006(2) 0.002(2) C15 0.081(3) 0.063(3) 0.075(4) -0.009(3) 0.011(3) 0.015(3) C33 0.060(3) 0.058(3) 0.075(3) 0.009(2) -0.012(2) 0.005(2) C34 0.056(3) 0.049(3) 0.099(4) 0.010(3) -0.017(3) -0.004(2) C26 0.047(2) 0.036(2) 0.063(3) 0.0122(18) -0.0056(18) 0.0044(17) C2 0.047(2) 0.033(2) 0.072(3) 0.0011(19) -0.0113(19) 0.0161(17) C18 0.0402(19) 0.059(3) 0.071(3) 0.020(2) -0.0032(18) 0.0127(19) C17 0.050(2) 0.057(3) 0.095(4) 0.025(3) -0.015(2) 0.021(2) C42 0.061(2) 0.053(3) 0.057(3) 0.007(2) -0.008(2) 0.016(2) C14 0.058(2) 0.039(2) 0.072(3) 0.002(2) -0.009(2) 0.0204(19) C41 0.054(2) 0.040(2) 0.069(3) 0.0116(19) -0.017(2) 0.0043(18) C1 0.047(2) 0.029(2) 0.056(2) 0.0027(16) -0.0137(17) 0.0202(17) C40 0.056(2) 0.043(2) 0.062(3) 0.0128(19) -0.0135(19) 0.0137(19) C39 0.058(2) 0.038(2) 0.064(3) 0.0129(19) -0.0090(19) 0.0210(18) C31 0.0350(18) 0.040(2) 0.077(3) 0.021(2) -0.0091(18) 0.0066(16) B1 0.041(2) 0.028(2) 0.044(2) 0.0072(17) -0.0055(17) 0.0130(17) C3 0.057(2) 0.031(2) 0.096(4) -0.001(2) -0.026(2) 0.0138(19) C32 0.046(2) 0.047(3) 0.069(3) 0.016(2) -0.0033(19) 0.0083(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.918(4) . ? Fe1 P1 2.424(3) . ? Fe1 P2 2.514(3) . ? Fe1 B1 2.859(5) . ? Fe1 H103 1.77(4) . ? P2 C19 1.846(4) . ? P2 C28 1.869(5) . ? P2 C25 1.870(4) . ? P1 C7 1.842(4) . ? P1 C13 1.870(5) . ? P1 C16 1.871(5) . ? Si3 N2 1.743(4) . ? Si3 C38 1.851(6) . ? Si3 C37 1.865(5) . ? Si3 C39 1.892(4) . ? Si2 N2 1.737(4) . ? Si2 C42 1.864(5) . ? Si2 C41 1.868(5) . ? Si2 C40 1.903(4) . ? Si1 N1 1.723(4) . ? Si1 C31 1.874(5) . ? Si1 H101 1.33(3) . ? Si1 H102 1.47(6) . ? N2 N1 1.492(4) . ? C20 C19 1.416(6) . ? C20 C21 1.422(5) . ? C20 B1 1.640(5) . ? C10 C9 1.383(6) . ? C10 C11 1.390(6) . ? C10 H10 0.9500 . ? C13 C14 1.510(6) . ? C13 C15 1.523(7) . ? C13 H13 1.0000 . ? C7 C12 1.394(6) . ? C7 C8 1.437(5) . ? C30 C28 1.507(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C9 C8 1.407(5) . ? C9 H9 0.9500 . ? C27 C25 1.549(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.533(6) . ? C28 H28 1.0000 . ? C21 C22 1.399(6) . ? C21 H21 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C22 C23 1.375(6) . ? C22 H22 0.9500 . ? C19 C24 1.395(5) . ? C8 B1 1.627(6) . ? C6 C1 1.387(7) . ? C6 C5 1.413(6) . ? C6 H6 0.9500 . ? C25 C26 1.531(5) . ? C25 H25 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C24 C23 1.388(5) . ? C24 H24 0.9500 . ? C12 C11 1.404(6) . ? C12 H12 0.9500 . ? C23 H23 0.9500 . ? C5 C4 1.384(8) . ? C5 H5 0.9500 . ? C16 C18 1.528(6) . ? C16 C17 1.543(6) . ? C16 H16 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C36 C35 1.397(7) . ? C36 C31 1.405(6) . ? C36 H36 0.9500 . ? C11 H11 0.9500 . ? C4 C3 1.363(8) . ? C4 H4 0.9500 . ? C35 C34 1.365(8) . ? C35 H35 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C33 C34 1.380(8) . ? C33 C32 1.403(7) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C2 C1 1.407(6) . ? C2 C3 1.413(6) . ? C2 H2 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C1 B1 1.628(6) . ? C40 C39 1.551(7) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C31 C32 1.374(7) . ? B1 H103 1.20(4) . ? C3 H3 0.9500 . ? C32 H32 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 Fe1 P1 127.08(11) . . ? N1 Fe1 P2 120.31(12) . . ? P1 Fe1 P2 111.54(6) . . ? N1 Fe1 B1 124.03(14) . . ? P1 Fe1 B1 78.95(14) . . ? P2 Fe1 B1 73.66(11) . . ? N1 Fe1 H103 111.7(13) . . ? P1 Fe1 H103 83.0(12) . . ? P2 Fe1 H103 83.3(13) . . ? B1 Fe1 H103 13.1(13) . . ? C19 P2 C28 110.42(18) . . ? C19 P2 C25 104.86(18) . . ? C28 P2 C25 104.70(19) . . ? C19 P2 Fe1 105.81(13) . . ? C28 P2 Fe1 113.04(13) . . ? C25 P2 Fe1 117.70(14) . . ? C7 P1 C13 106.3(2) . . ? C7 P1 C16 107.42(19) . . ? C13 P1 C16 101.97(19) . . ? C7 P1 Fe1 98.34(14) . . ? C13 P1 Fe1 122.41(16) . . ? C16 P1 Fe1 119.05(18) . . ? N2 Si3 C38 112.67(19) . . ? N2 Si3 C37 114.3(2) . . ? C38 Si3 C37 109.4(2) . . ? N2 Si3 C39 97.15(17) . . ? C38 Si3 C39 114.2(2) . . ? C37 Si3 C39 108.7(2) . . ? N2 Si2 C42 114.6(2) . . ? N2 Si2 C41 109.8(2) . . ? C42 Si2 C41 109.6(2) . . ? N2 Si2 C40 98.72(18) . . ? C42 Si2 C40 110.7(2) . . ? C41 Si2 C40 113.2(2) . . ? N1 Si1 C31 115.76(18) . . ? N1 Si1 H101 104.6(15) . . ? C31 Si1 H101 104.8(16) . . ? N1 Si1 H102 119(2) . . ? C31 Si1 H102 96(2) . . ? H101 Si1 H102 116(3) . . ? N1 N2 Si2 119.5(2) . . ? N1 N2 Si3 125.8(2) . . ? Si2 N2 Si3 114.69(17) . . ? C19 C20 C21 116.1(3) . . ? C19 C20 B1 124.4(3) . . ? C21 C20 B1 119.4(3) . . ? C9 C10 C11 119.3(4) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C14 C13 C15 110.2(4) . . ? C14 C13 P1 113.4(3) . . ? C15 C13 P1 112.6(3) . . ? C14 C13 H13 106.7 . . ? C15 C13 H13 106.7 . . ? P1 C13 H13 106.7 . . ? N2 N1 Si1 115.8(2) . . ? N2 N1 Fe1 124.2(2) . . ? Si1 N1 Fe1 119.91(16) . . ? C12 C7 C8 121.0(3) . . ? C12 C7 P1 119.4(3) . . ? C8 C7 P1 119.5(3) . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C10 C9 C8 124.0(3) . . ? C10 C9 H9 118.0 . . ? C8 C9 H9 118.0 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C29 110.8(3) . . ? C30 C28 P2 108.5(3) . . ? C29 C28 P2 120.8(3) . . ? C30 C28 H28 105.2 . . ? C29 C28 H28 105.2 . . ? P2 C28 H28 105.2 . . ? C22 C21 C20 122.0(4) . . ? C22 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C23 C22 C21 120.1(3) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C19 C20 121.2(3) . . ? C24 C19 P2 120.3(3) . . ? C20 C19 P2 118.4(3) . . ? C9 C8 C7 115.3(3) . . ? C9 C8 B1 116.0(3) . . ? C7 C8 B1 128.6(3) . . ? C1 C6 C5 123.0(5) . . ? C1 C6 H6 118.5 . . ? C5 C6 H6 118.5 . . ? C26 C25 C27 112.3(3) . . ? C26 C25 P2 115.3(3) . . ? C27 C25 P2 111.5(3) . . ? C26 C25 H25 105.6 . . ? C27 C25 H25 105.6 . . ? P2 C25 H25 105.6 . . ? Si3 C38 H38A 109.5 . . ? Si3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C23 C24 C19 120.9(4) . . ? C23 C24 H24 119.5 . . ? C19 C24 H24 119.5 . . ? C7 C12 C11 120.8(3) . . ? C7 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C22 C23 C24 119.8(4) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C4 C5 C6 118.4(5) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? C18 C16 C17 108.9(4) . . ? C18 C16 P1 111.4(3) . . ? C17 C16 P1 109.6(3) . . ? C18 C16 H16 109.0 . . ? C17 C16 H16 109.0 . . ? P1 C16 H16 109.0 . . ? Si3 C37 H37A 109.5 . . ? Si3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C36 C31 120.9(5) . . ? C35 C36 H36 119.5 . . ? C31 C36 H36 119.5 . . ? C10 C11 C12 119.4(4) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C3 C4 C5 120.9(4) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C34 C35 C36 119.6(5) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? 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 . . ? C34 C33 C32 119.2(5) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C35 C34 C33 120.9(5) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C1 C2 C3 121.4(5) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C42 H42A 109.5 . . ? Si2 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si2 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 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 . . ? Si2 C41 H41A 109.5 . . ? Si2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C6 C1 C2 116.3(4) . . ? C6 C1 B1 124.4(4) . . ? C2 C1 B1 119.3(4) . . ? C39 C40 Si2 107.6(3) . . ? C39 C40 H40A 110.2 . . ? Si2 C40 H40A 110.2 . . ? C39 C40 H40B 110.2 . . ? Si2 C40 H40B 110.2 . . ? H40A C40 H40B 108.5 . . ? C40 C39 Si3 106.7(3) . . ? C40 C39 H39A 110.4 . . ? Si3 C39 H39A 110.4 . . ? C40 C39 H39B 110.4 . . ? Si3 C39 H39B 110.4 . . ? H39A C39 H39B 108.6 . . ? C32 C31 C36 118.0(4) . . ? C32 C31 Si1 121.7(3) . . ? C36 C31 Si1 120.4(4) . . ? C8 B1 C1 113.2(3) . . ? C8 B1 C20 109.7(3) . . ? C1 B1 C20 111.6(3) . . ? C8 B1 Fe1 90.8(2) . . ? C1 B1 Fe1 128.0(3) . . ? C20 B1 Fe1 101.1(2) . . ? C8 B1 H103 106.7(18) . . ? C1 B1 H103 110(2) . . ? C20 B1 H103 105.4(19) . . ? Fe1 B1 H103 19.5(19) . . ? C4 C3 C2 119.9(5) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C31 C32 C33 121.4(5) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? _diffrn_measured_fraction_theta_max 0.778 _diffrn_reflns_theta_full 24.55 _diffrn_measured_fraction_theta_full 0.778 _refine_diff_density_max 0.778 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.087 ####################################################### # Compound 9: (PhDPBPh*)FeNSiNSi # ####################################################### data_9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H67 B Fe N2 O2 P2 Si2' _chemical_formula_weight 984.90 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' 'Si' 'Si' 0.0817 0.0704 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2122(7) _cell_length_b 13.2685(8) _cell_length_c 16.1433(12) _cell_angle_alpha 88.967(3) _cell_angle_beta 80.813(3) _cell_angle_gamma 84.376(2) _cell_volume 2569.8(3) _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 block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 0.446 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; 'Bruker KAPPA APEX II' ; _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 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 310067 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 44.14 _reflns_number_total 40098 _reflns_number_gt 29046 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7-0 (Bruker-AXS, 2007)' _computing_cell_refinement 'SAINT V7.68A (Bruker-AXS, 2007)' _computing_data_reduction 'SAINT V7.68A (Bruker-AXS, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0627P)^2^+0.2368P] 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 40098 _refine_ls_number_parameters 627 _refine_ls_number_restraints 585 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1070 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.021 _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 Fe1 Fe 0.320362(8) 0.177539(7) 0.198216(6) 0.01012(2) Uani 1 1 d U . . P2 P 0.173410(14) 0.005178(13) 0.254121(11) 0.00967(3) Uani 1 1 d U . . P1 P 0.503053(14) 0.149701(13) 0.240020(11) 0.01068(3) Uani 1 1 d U . . Si2 Si 0.260895(16) 0.026863(15) 0.067303(12) 0.01066(3) Uani 1 1 d U . . Si1 Si 0.25858(2) 0.347150(17) 0.059899(15) 0.01721(4) Uani 1 1 d U . . C7 C 0.48777(5) 0.22225(5) 0.33677(4) 0.01106(9) Uani 1 1 d U . . C8 C 0.38566(5) 0.22182(5) 0.39299(4) 0.01041(9) Uani 1 1 d U . . C6 C 0.12291(6) 0.17239(6) 0.51303(5) 0.01649(11) Uani 1 1 d U . . H6 H 0.1529 0.1076 0.5292 0.020 Uiso 1 1 calc R . . C37 C 0.05453(5) 0.08772(5) 0.29984(4) 0.01363(10) Uani 1 1 d U . . N2 N 0.24724(5) 0.05332(4) 0.17466(3) 0.01082(8) Uani 1 1 d U . . N1 N 0.29119(6) 0.30976(5) 0.15481(4) 0.01723(11) Uani 1 1 d U . . C1 C 0.16737(5) 0.21340(5) 0.43594(4) 0.01181(9) Uani 1 1 d U . . C9 C 0.37853(6) 0.27865(5) 0.46692(4) 0.01298(10) Uani 1 1 d U . . H9 H 0.3132 0.2779 0.5077 0.016 Uiso 1 1 calc R . . C28 C 0.37910(6) -0.10140(5) 0.46086(5) 0.01454(10) Uani 1 1 d U . . H28 H 0.4251 -0.1243 0.5010 0.017 Uiso 1 1 calc R . . C30 C 0.26390(6) -0.13539(5) 0.35935(4) 0.01341(10) Uani 1 1 d U . . H30 H 0.2285 -0.1823 0.3315 0.016 Uiso 1 1 calc R . . C42 C -0.00471(6) 0.05989(7) 0.37712(5) 0.01839(12) Uani 1 1 d U . . H42 H 0.0206 0.0007 0.4052 0.022 Uiso 1 1 calc R . . C25 C 0.25024(5) -0.03199(5) 0.33915(4) 0.01057(9) Uani 1 1 d U . . C3 C 0.02951(7) 0.36011(7) 0.46740(6) 0.02436(16) Uani 1 1 d U . . H3 H -0.0025 0.4240 0.4509 0.029 Uiso 1 1 calc R . . C27 C 0.36194(6) 0.00147(5) 0.44311(4) 0.01317(10) Uani 1 1 d U . . H27 H 0.3956 0.0476 0.4732 0.016 Uiso 1 1 calc R . . C40 C -0.13599(7) 0.20570(8) 0.37162(6) 0.02794(19) Uani 1 1 d U . . H40 H -0.2009 0.2465 0.3962 0.034 Uiso 1 1 calc R . . C19 C 0.55860(5) 0.02193(5) 0.26406(4) 0.01258(10) Uani 1 1 d U . . C48 C 0.12708(6) 0.00049(6) 0.03367(5) 0.01774(12) Uani 1 1 d U . . H48A H 0.1124 -0.0695 0.0479 0.027 Uiso 1 1 calc R . . H48B H 0.1325 0.0103 -0.0271 0.027 Uiso 1 1 calc R . . H48C H 0.0661 0.0469 0.0625 0.027 Uiso 1 1 calc R . . C13 C 0.61856(6) 0.20140(5) 0.17176(4) 0.01331(10) Uani 1 1 d U . . C26 C 0.29739(5) 0.04087(5) 0.38287(4) 0.01051(9) Uani 1 1 d U . . C41 C -0.10026(7) 0.11871(8) 0.41264(6) 0.02444(16) Uani 1 1 d U . . H41 H -0.1410 0.0996 0.4647 0.029 Uiso 1 1 calc R . . C38 C 0.01824(6) 0.17450(6) 0.25837(5) 0.01836(12) Uani 1 1 d U . . H38 H 0.0581 0.1933 0.2059 0.022 Uiso 1 1 calc R . . C31 C 0.11423(6) -0.10419(5) 0.22013(4) 0.01389(10) Uani 1 1 d U . . C5 C 0.03523(7) 0.22444(8) 0.56708(5) 0.02409(16) Uani 1 1 d U . . H5 H 0.0074 0.1952 0.6194 0.029 Uiso 1 1 calc R . . C2 C 0.11725(6) 0.30807(6) 0.41442(5) 0.01675(12) Uani 1 1 d U . . H2 H 0.1441 0.3376 0.3620 0.020 Uiso 1 1 calc R . . C12 C 0.57223(6) 0.28002(6) 0.35250(4) 0.01430(10) Uani 1 1 d U . . H12 H 0.6391 0.2795 0.3132 0.017 Uiso 1 1 calc R . . C29 C 0.32846(6) -0.17022(5) 0.41951(5) 0.01489(11) Uani 1 1 d U . . H29 H 0.3378 -0.2404 0.4322 0.018 Uiso 1 1 calc R . . C11 C 0.55952(6) 0.33819(6) 0.42499(5) 0.01514(11) Uani 1 1 d U . . H11 H 0.6161 0.3788 0.4346 0.018 Uiso 1 1 calc R . . C23 C 0.56507(8) -0.15815(6) 0.23869(6) 0.02371(15) Uani 1 1 d U . . H23 H 0.5414 -0.2126 0.2109 0.028 Uiso 1 1 calc R . . C20 C 0.63487(7) 0.00191(6) 0.31994(5) 0.01877(13) Uani 1 1 d U . . H20 H 0.6588 0.0561 0.3479 0.023 Uiso 1 1 calc R . . C18 C 0.72961(6) 0.16055(7) 0.16502(5) 0.01856(12) Uani 1 1 d U . . H18 H 0.7482 0.1012 0.1956 0.022 Uiso 1 1 calc R . . C39 C -0.07766(8) 0.23349(7) 0.29512(6) 0.02625(17) Uani 1 1 d U . . H39 H -0.1031 0.2930 0.2675 0.031 Uiso 1 1 calc R . . C36 C 0.18517(7) -0.18757(6) 0.18575(5) 0.01729(12) Uani 1 1 d U . . H36 H 0.2629 -0.1899 0.1871 0.021 Uiso 1 1 calc R . . C10 C 0.46251(6) 0.33586(5) 0.48320(4) 0.01466(11) Uani 1 1 d U . . H10 H 0.4536 0.3732 0.5339 0.018 Uiso 1 1 calc R . . C24 C 0.52376(7) -0.05891(6) 0.22403(5) 0.01701(12) Uani 1 1 d U . . H24 H 0.4715 -0.0461 0.1865 0.020 Uiso 1 1 calc R . . C4 C -0.01102(7) 0.31850(8) 0.54432(6) 0.02773(19) Uani 1 1 d U . . H4 H -0.0700 0.3542 0.5811 0.033 Uiso 1 1 calc R . . C33 C -0.04148(8) -0.18170(8) 0.18094(6) 0.02594(17) Uani 1 1 d U . . H33 H -0.1191 -0.1800 0.1795 0.031 Uiso 1 1 calc R . . C35 C 0.14332(9) -0.26693(6) 0.14976(5) 0.02333(15) Uani 1 1 d U . . H35 H 0.1920 -0.3236 0.1274 0.028 Uiso 1 1 calc R . . C45 C 0.21977(7) 0.23383(6) 0.00795(5) 0.01981(13) Uani 1 1 d U . . H45A H 0.1472 0.2152 0.0377 0.024 Uiso 1 1 calc R . . H45B H 0.2107 0.2515 -0.0506 0.024 Uiso 1 1 calc R . . C32 C -0.00011(6) -0.10204(7) 0.21778(5) 0.01908(13) Uani 1 1 d U . . H32 H -0.0495 -0.0464 0.2412 0.023 Uiso 1 1 calc R . . C14 C 0.59262(7) 0.28727(6) 0.12462(5) 0.01980(13) Uani 1 1 d U . . H14 H 0.5172 0.3146 0.1275 0.024 Uiso 1 1 calc R . . C16 C 0.78703(8) 0.29339(8) 0.06841(6) 0.02463(16) Uani 1 1 d U . . H16 H 0.8444 0.3254 0.0342 0.030 Uiso 1 1 calc R . . C34 C 0.02985(9) -0.26313(7) 0.14653(6) 0.02757(18) Uani 1 1 d U . . H34 H 0.0013 -0.3165 0.1207 0.033 Uiso 1 1 calc R . . C47 C 0.37089(6) -0.07923(6) 0.03387(5) 0.01753(12) Uani 1 1 d U . . H47A H 0.4397 -0.0668 0.0544 0.026 Uiso 1 1 calc R . . H47B H 0.3851 -0.0833 -0.0275 0.026 Uiso 1 1 calc R . . H47C H 0.3455 -0.1432 0.0572 0.026 Uiso 1 1 calc R . . C17 C 0.81323(7) 0.20700(8) 0.11340(5) 0.02225(15) Uani 1 1 d U . . H17 H 0.8886 0.1791 0.1091 0.027 Uiso 1 1 calc R . . C46 C 0.30821(6) 0.14115(6) 0.00738(5) 0.01630(11) Uani 1 1 d U . . H46A H 0.3725 0.1628 0.0305 0.020 Uiso 1 1 calc R . . H46B H 0.3351 0.1210 -0.0517 0.020 Uiso 1 1 calc R . . C44 C 0.38084(9) 0.39350(8) -0.01106(7) 0.03049(19) Uani 1 1 d U . . H44A H 0.4076 0.4499 0.0158 0.046 Uiso 1 1 calc R . . H44B H 0.3580 0.4165 -0.0643 0.046 Uiso 1 1 calc R . . H44C H 0.4407 0.3383 -0.0217 0.046 Uiso 1 1 calc R . . C22 C 0.64096(8) -0.17746(7) 0.29399(6) 0.02500(16) Uani 1 1 d U . . H22 H 0.6691 -0.2451 0.3041 0.030 Uiso 1 1 calc R . . C21 C 0.67557(8) -0.09752(7) 0.33440(6) 0.02447(16) Uani 1 1 d U . . H21 H 0.7274 -0.1108 0.3722 0.029 Uiso 1 1 calc R . . C15 C 0.67672(8) 0.33309(7) 0.07336(6) 0.02667(17) Uani 1 1 d U . . H15 H 0.6585 0.3917 0.0417 0.032 Uiso 1 1 calc R . . O1 O 0.31080(7) 0.54195(8) 0.20959(6) 0.0431(2) Uani 1 1 d U A 1 C49 C 0.23830(10) 0.54969(10) 0.28809(8) 0.0375(2) Uani 1 1 d U A 1 H49A H 0.1840 0.4984 0.2919 0.045 Uiso 1 1 calc R A 1 H49B H 0.1967 0.6177 0.2942 0.045 Uiso 1 1 calc R A 1 C52 C 0.42376(11) 0.54397(15) 0.22328(10) 0.0519(4) Uani 1 1 d DU A 1 H52A H 0.4603 0.5960 0.1871 0.062 Uiso 1 1 calc R A 1 H52B H 0.4662 0.4774 0.2094 0.062 Uiso 1 1 calc R A 1 C50 C 0.31004(11) 0.53197(12) 0.35581(9) 0.0433(3) Uani 1 1 d DU A 1 H50A H 0.3189 0.4594 0.3711 0.052 Uiso 1 1 calc R A 1 H50B H 0.2781 0.5719 0.4067 0.052 Uiso 1 1 calc R A 1 C51 C 0.42157(11) 0.56843(17) 0.31457(9) 0.0320(4) Uani 0.853(8) 1 d PDU A 1 H51A H 0.4230 0.6420 0.3230 0.038 Uiso 0.853(8) 1 calc PR A 1 H51B H 0.4850 0.5313 0.3368 0.038 Uiso 0.853(8) 1 calc PR A 1 C51A C 0.4145(8) 0.5178(15) 0.3068(5) 0.051(4) Uani 0.147(8) 1 d PDU A 2 O2 O 0.29415(7) 0.44287(7) 0.66522(5) 0.03539(17) Uani 1 1 d DU B 1 C54 C 0.16289(10) 0.46673(13) 0.78770(8) 0.0428(3) Uani 1 1 d U B 1 H54A H 0.1305 0.5246 0.8245 0.051 Uiso 1 1 calc R B 1 H54B H 0.1601 0.4035 0.8212 0.051 Uiso 1 1 calc R B 1 C55 C 0.10046(9) 0.46106(11) 0.71274(8) 0.0365(2) Uani 1 1 d DU B 1 H55A H 0.0687 0.3954 0.7116 0.044 Uiso 1 1 calc R B 1 H55B H 0.0398 0.5166 0.7145 0.044 Uiso 1 1 calc R B 1 C53 C 0.28016(10) 0.48086(12) 0.74829(8) 0.0393(3) Uani 1 1 d U B 1 H53A H 0.2927 0.5535 0.7475 0.047 Uiso 1 1 calc R B 1 H53B H 0.3338 0.4433 0.7803 0.047 Uiso 1 1 calc R B 1 C56 C 0.19138(14) 0.4722(2) 0.63728(12) 0.0281(4) Uani 0.829(12) 1 d PDU B 1 H56A H 0.1814 0.4282 0.5907 0.034 Uiso 0.829(12) 1 calc PR B 1 H56B H 0.1889 0.5432 0.6173 0.034 Uiso 0.829(12) 1 calc PR B 1 C56A C 0.1850(8) 0.430(2) 0.6420(10) 0.056(5) Uani 0.171(12) 1 d PDU B 2 B1 B 0.27836(6) 0.16386(6) 0.37562(4) 0.01069(10) Uani 1 1 d U . . C43 C 0.13928(10) 0.44889(8) 0.06765(8) 0.0324(2) Uani 1 1 d U . . H43A H 0.0723 0.4232 0.0992 0.049 Uiso 1 1 calc R . . H43B H 0.1256 0.4688 0.0112 0.049 Uiso 1 1 calc R . . H43C H 0.1577 0.5078 0.0966 0.049 Uiso 1 1 calc R . . H101 H 0.2589(10) 0.1873(9) 0.3080(7) 0.016(3) Uiso 1 1 d . . . H102 H 0.2945(17) 0.3498(16) 0.1802(13) 0.067(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01104(4) 0.00978(4) 0.01017(4) -0.00073(3) -0.00320(3) -0.00152(3) P2 0.00883(6) 0.01053(6) 0.00987(6) -0.00179(5) -0.00187(5) -0.00113(5) P1 0.00952(6) 0.01241(7) 0.01018(6) -0.00200(5) -0.00208(5) -0.00027(5) Si2 0.01037(7) 0.01164(7) 0.01019(7) -0.00243(5) -0.00238(5) -0.00045(5) Si1 0.02161(10) 0.01267(8) 0.01845(9) 0.00233(7) -0.00711(7) -0.00103(7) C7 0.0104(2) 0.0122(2) 0.0108(2) -0.00182(18) -0.00230(17) -0.00084(17) C8 0.0107(2) 0.0102(2) 0.0105(2) -0.00116(17) -0.00246(17) -0.00056(16) C6 0.0140(3) 0.0226(3) 0.0127(3) -0.0011(2) -0.0005(2) -0.0037(2) C37 0.0092(2) 0.0173(3) 0.0143(3) -0.0048(2) -0.00244(18) 0.00048(18) N2 0.0113(2) 0.0115(2) 0.0100(2) -0.00174(15) -0.00215(15) -0.00174(15) N1 0.0239(3) 0.0124(2) 0.0169(3) 0.00103(19) -0.0077(2) -0.0022(2) C1 0.0099(2) 0.0136(2) 0.0119(2) -0.00276(18) -0.00196(17) -0.00066(17) C9 0.0125(2) 0.0147(3) 0.0119(2) -0.00342(19) -0.00222(18) -0.00101(18) C28 0.0141(3) 0.0148(3) 0.0151(3) 0.0011(2) -0.0049(2) 0.00074(19) C30 0.0154(3) 0.0112(2) 0.0139(2) -0.00062(19) -0.00302(19) -0.00122(18) C42 0.0116(3) 0.0260(3) 0.0168(3) -0.0045(2) 0.0004(2) -0.0015(2) C25 0.0103(2) 0.0109(2) 0.0106(2) -0.00096(17) -0.00174(17) -0.00069(16) C3 0.0194(3) 0.0241(4) 0.0286(4) -0.0111(3) -0.0065(3) 0.0088(3) C27 0.0127(2) 0.0135(2) 0.0140(2) -0.00071(19) -0.00467(19) -0.00090(18) C40 0.0128(3) 0.0396(5) 0.0308(4) -0.0179(4) -0.0060(3) 0.0082(3) C19 0.0117(2) 0.0142(2) 0.0114(2) -0.00151(19) -0.00185(18) 0.00120(18) C48 0.0160(3) 0.0221(3) 0.0170(3) -0.0022(2) -0.0074(2) -0.0035(2) C13 0.0128(2) 0.0158(3) 0.0112(2) -0.00245(19) -0.00088(18) -0.00221(19) C26 0.0093(2) 0.0111(2) 0.0112(2) -0.00142(17) -0.00187(17) -0.00035(16) C41 0.0113(3) 0.0388(5) 0.0221(3) -0.0122(3) 0.0013(2) -0.0007(3) C38 0.0162(3) 0.0197(3) 0.0193(3) -0.0042(2) -0.0067(2) 0.0049(2) C31 0.0160(3) 0.0143(3) 0.0125(2) -0.00123(19) -0.00314(19) -0.0054(2) C5 0.0165(3) 0.0392(5) 0.0154(3) -0.0070(3) 0.0029(2) -0.0046(3) C2 0.0157(3) 0.0158(3) 0.0182(3) -0.0035(2) -0.0035(2) 0.0034(2) C12 0.0117(2) 0.0168(3) 0.0149(3) -0.0025(2) -0.00208(19) -0.00350(19) C29 0.0170(3) 0.0119(2) 0.0157(3) 0.0007(2) -0.0037(2) 0.00072(19) C11 0.0142(3) 0.0160(3) 0.0164(3) -0.0036(2) -0.0042(2) -0.0038(2) C23 0.0269(4) 0.0143(3) 0.0297(4) -0.0027(3) -0.0056(3) 0.0014(3) C20 0.0188(3) 0.0219(3) 0.0162(3) -0.0018(2) -0.0075(2) 0.0032(2) C18 0.0129(3) 0.0268(4) 0.0155(3) -0.0001(2) -0.0009(2) -0.0018(2) C39 0.0210(3) 0.0274(4) 0.0302(4) -0.0094(3) -0.0112(3) 0.0117(3) C36 0.0236(3) 0.0134(3) 0.0157(3) -0.0023(2) -0.0042(2) -0.0036(2) C10 0.0153(3) 0.0151(3) 0.0144(3) -0.0049(2) -0.0043(2) -0.0013(2) C24 0.0186(3) 0.0145(3) 0.0184(3) -0.0028(2) -0.0050(2) 0.0002(2) C4 0.0155(3) 0.0401(5) 0.0254(4) -0.0165(4) 0.0005(3) 0.0047(3) C33 0.0242(4) 0.0348(5) 0.0216(4) -0.0051(3) -0.0019(3) -0.0186(3) C35 0.0376(5) 0.0150(3) 0.0187(3) -0.0028(2) -0.0044(3) -0.0087(3) C45 0.0241(3) 0.0160(3) 0.0215(3) 0.0009(2) -0.0112(3) -0.0003(2) C32 0.0158(3) 0.0262(4) 0.0166(3) -0.0036(2) -0.0018(2) -0.0095(2) C14 0.0202(3) 0.0162(3) 0.0214(3) 0.0019(2) 0.0005(2) -0.0008(2) C16 0.0237(4) 0.0302(4) 0.0195(3) -0.0027(3) 0.0039(3) -0.0116(3) C34 0.0390(5) 0.0263(4) 0.0206(4) -0.0041(3) -0.0031(3) -0.0208(4) C47 0.0172(3) 0.0164(3) 0.0175(3) -0.0045(2) -0.0003(2) 0.0022(2) C17 0.0145(3) 0.0345(4) 0.0174(3) -0.0031(3) 0.0013(2) -0.0059(3) C46 0.0187(3) 0.0156(3) 0.0141(3) -0.0001(2) -0.0013(2) -0.0014(2) C44 0.0342(5) 0.0295(4) 0.0289(4) 0.0116(4) -0.0051(4) -0.0108(4) C22 0.0267(4) 0.0189(3) 0.0268(4) 0.0028(3) -0.0023(3) 0.0074(3) C21 0.0245(4) 0.0266(4) 0.0216(3) 0.0019(3) -0.0084(3) 0.0079(3) C15 0.0290(4) 0.0214(4) 0.0274(4) 0.0046(3) 0.0037(3) -0.0056(3) O1 0.0277(4) 0.0575(6) 0.0441(5) -0.0213(4) -0.0070(3) 0.0020(4) C49 0.0273(5) 0.0371(6) 0.0463(6) 0.0130(5) -0.0025(4) -0.0009(4) C52 0.0285(5) 0.0800(11) 0.0469(7) -0.0294(7) -0.0004(5) -0.0081(6) C50 0.0363(6) 0.0495(7) 0.0437(7) 0.0180(6) -0.0064(5) -0.0057(5) C51 0.0249(5) 0.0380(9) 0.0333(6) -0.0099(5) -0.0046(4) -0.0020(5) C51A 0.037(4) 0.066(9) 0.052(5) -0.018(5) -0.027(4) 0.024(5) O2 0.0252(3) 0.0461(5) 0.0335(4) -0.0049(3) -0.0048(3) 0.0044(3) C54 0.0296(5) 0.0726(9) 0.0281(5) 0.0034(5) -0.0019(4) -0.0197(5) C55 0.0250(4) 0.0515(7) 0.0355(5) 0.0023(5) -0.0058(4) -0.0144(4) C53 0.0289(5) 0.0591(8) 0.0328(5) -0.0041(5) -0.0052(4) -0.0178(5) C56 0.0232(5) 0.0334(8) 0.0278(6) 0.0003(5) -0.0047(4) -0.0022(5) C56A 0.028(4) 0.082(11) 0.062(6) -0.041(7) -0.024(4) 0.011(5) B1 0.0102(2) 0.0117(3) 0.0102(2) -0.0017(2) -0.00208(19) -0.00036(19) C43 0.0360(5) 0.0203(4) 0.0414(6) -0.0022(4) -0.0149(4) 0.0085(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.8996(7) . ? Fe1 N2 2.0194(6) . ? Fe1 P1 2.4248(2) . ? Fe1 B1 2.8335(8) . ? Fe1 H101 1.813(12) . ? P2 N2 1.6064(6) . ? P2 C37 1.7964(7) . ? P2 C31 1.8139(7) . ? P2 C25 1.8177(7) . ? P1 C19 1.8221(7) . ? P1 C7 1.8240(7) . ? P1 C13 1.8277(7) . ? Si2 N2 1.7529(6) . ? Si2 C48 1.8682(7) . ? Si2 C47 1.8715(8) . ? Si2 C46 1.8734(8) . ? Si1 N1 1.6974(7) . ? Si1 C45 1.8710(8) . ? Si1 C43 1.8769(10) . ? Si1 C44 1.8783(10) . ? C7 C12 1.4005(9) . ? C7 C8 1.4208(9) . ? C8 C9 1.4095(9) . ? C8 B1 1.6461(9) . ? C6 C1 1.3991(10) . ? C6 C5 1.4011(11) . ? C6 H6 0.9500 . ? C37 C38 1.3918(11) . ? C37 C42 1.4014(11) . ? N2 N1 3.4974(9) . ? N1 H102 0.68(2) . ? C1 C2 1.4052(10) . ? C1 B1 1.6262(10) . ? C9 C10 1.3940(10) . ? C9 H9 0.9500 . ? C28 C29 1.3879(10) . ? C28 C27 1.3922(10) . ? C28 H28 0.9500 . ? C30 C29 1.3911(10) . ? C30 C25 1.4045(9) . ? C30 H30 0.9500 . ? C42 C41 1.3869(11) . ? C42 H42 0.9500 . ? C25 C26 1.4240(9) . ? C3 C4 1.3871(15) . ? C3 C2 1.3929(11) . ? C3 H3 0.9500 . ? C27 C26 1.4093(9) . ? C27 H27 0.9500 . ? C40 C39 1.3866(15) . ? C40 C41 1.3883(15) . ? C40 H40 0.9500 . ? C19 C24 1.3969(10) . ? C19 C20 1.4011(10) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C13 C14 1.3973(11) . ? C13 C18 1.3985(10) . ? C26 B1 1.6304(10) . ? C41 H41 0.9500 . ? C38 C39 1.3969(11) . ? C38 H38 0.9500 . ? C31 C32 1.4004(10) . ? C31 C36 1.4012(11) . ? C5 C4 1.3867(15) . ? C5 H5 0.9500 . ? C2 H2 0.9500 . ? C12 C11 1.3930(10) . ? C12 H12 0.9500 . ? C29 H29 0.9500 . ? C11 C10 1.3922(10) . ? C11 H11 0.9500 . ? C23 C22 1.3895(14) . ? C23 C24 1.3932(11) . ? C23 H23 0.9500 . ? C20 C21 1.3926(12) . ? C20 H20 0.9500 . ? C18 C17 1.3965(11) . ? C18 H18 0.9500 . ? C39 H39 0.9500 . ? C36 C35 1.3892(11) . ? C36 H36 0.9500 . ? C10 H10 0.9500 . ? C24 H24 0.9500 . ? C4 H4 0.9500 . ? C33 C34 1.3848(15) . ? C33 C32 1.3962(11) . ? C33 H33 0.9500 . ? C35 C34 1.3910(15) . ? C35 H35 0.9500 . ? C45 C46 1.5542(11) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C32 H32 0.9500 . ? C14 C15 1.3936(12) . ? C14 H14 0.9500 . ? C16 C17 1.3842(14) . ? C16 C15 1.3880(14) . ? C16 H16 0.9500 . ? C34 H34 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C17 H17 0.9500 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C22 C21 1.3893(14) . ? C22 H22 0.9500 . ? C21 H21 0.9500 . ? C15 H15 0.9500 . ? O1 C49 1.4245(16) . ? O1 C52 1.4343(16) . ? C49 C50 1.5079(19) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C52 C51 1.510(2) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C50 C51 1.5364(19) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? O2 C56 1.4174(19) . ? O2 C53 1.4198(15) . ? C54 C53 1.4995(16) . ? C54 C55 1.5363(17) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.527(2) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? B1 H101 1.183(12) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N2 126.33(3) . . ? N1 Fe1 P1 112.75(2) . . ? N2 Fe1 P1 116.926(17) . . ? N1 Fe1 B1 114.56(3) . . ? N2 Fe1 B1 96.97(2) . . ? P1 Fe1 B1 75.004(15) . . ? N1 Fe1 H101 104.2(4) . . ? N2 Fe1 H101 95.8(4) . . ? P1 Fe1 H101 89.1(4) . . ? B1 Fe1 H101 15.2(4) . . ? N2 P2 C37 113.77(3) . . ? N2 P2 C31 109.07(3) . . ? C37 P2 C31 104.29(3) . . ? N2 P2 C25 113.88(3) . . ? C37 P2 C25 106.10(3) . . ? C31 P2 C25 109.23(3) . . ? C19 P1 C7 106.44(3) . . ? C19 P1 C13 104.18(3) . . ? C7 P1 C13 104.21(3) . . ? C19 P1 Fe1 119.78(2) . . ? C7 P1 Fe1 103.56(2) . . ? C13 P1 Fe1 117.18(2) . . ? N2 Si2 C48 113.27(3) . . ? N2 Si2 C47 112.32(3) . . ? C48 Si2 C47 109.88(4) . . ? N2 Si2 C46 108.07(3) . . ? C48 Si2 C46 106.92(4) . . ? C47 Si2 C46 105.96(4) . . ? N1 Si1 C45 107.72(4) . . ? N1 Si1 C43 113.04(5) . . ? C45 Si1 C43 108.78(4) . . ? N1 Si1 C44 112.01(4) . . ? C45 Si1 C44 106.73(5) . . ? C43 Si1 C44 108.33(5) . . ? C12 C7 C8 121.61(6) . . ? C12 C7 P1 120.61(5) . . ? C8 C7 P1 117.70(5) . . ? C9 C8 C7 115.35(6) . . ? C9 C8 B1 119.91(6) . . ? C7 C8 B1 124.72(5) . . ? C1 C6 C5 121.70(8) . . ? C1 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C38 C37 C42 120.36(7) . . ? C38 C37 P2 121.44(6) . . ? C42 C37 P2 118.13(6) . . ? P2 N2 Si2 130.62(4) . . ? P2 N2 Fe1 115.76(3) . . ? Si2 N2 Fe1 113.00(3) . . ? P2 N2 N1 124.28(3) . . ? Si2 N2 N1 97.25(3) . . ? Fe1 N2 N1 25.950(15) . . ? Si1 N1 Fe1 130.10(4) . . ? Si1 N1 N2 106.15(3) . . ? Fe1 N1 N2 27.722(15) . . ? Si1 N1 H102 112.5(18) . . ? Fe1 N1 H102 117.4(18) . . ? N2 N1 H102 138.6(18) . . ? C6 C1 C2 116.52(6) . . ? C6 C1 B1 124.20(6) . . ? C2 C1 B1 119.02(6) . . ? C10 C9 C8 123.27(6) . . ? C10 C9 H9 118.4 . . ? C8 C9 H9 118.4 . . ? C29 C28 C27 119.47(6) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C29 C30 C25 121.08(6) . . ? C29 C30 H30 119.5 . . ? C25 C30 H30 119.5 . . ? C41 C42 C37 120.05(8) . . ? C41 C42 H42 120.0 . . ? C37 C42 H42 120.0 . . ? C30 C25 C26 120.82(6) . . ? C30 C25 P2 117.91(5) . . ? C26 C25 P2 121.25(5) . . ? C4 C3 C2 119.88(8) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C28 C27 C26 123.51(6) . . ? C28 C27 H27 118.2 . . ? C26 C27 H27 118.2 . . ? C39 C40 C41 120.54(8) . . ? C39 C40 H40 119.7 . . ? C41 C40 H40 119.7 . . ? C24 C19 C20 119.14(7) . . ? C24 C19 P1 117.98(5) . . ? C20 C19 P1 122.88(6) . . ? Si2 C48 H48A 109.5 . . ? Si2 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si2 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C14 C13 C18 119.09(7) . . ? C14 C13 P1 117.06(5) . . ? C18 C13 P1 123.85(6) . . ? C27 C26 C25 115.65(6) . . ? C27 C26 B1 116.72(5) . . ? C25 C26 B1 127.49(6) . . ? C42 C41 C40 119.60(8) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C37 C38 C39 119.02(8) . . ? C37 C38 H38 120.5 . . ? C39 C38 H38 120.5 . . ? C32 C31 C36 118.87(7) . . ? C32 C31 P2 121.11(6) . . ? C36 C31 P2 119.53(5) . . ? C4 C5 C6 120.16(8) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C3 C2 C1 122.22(8) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? C11 C12 C7 120.88(6) . . ? C11 C12 H12 119.6 . . ? C7 C12 H12 119.6 . . ? C28 C29 C30 119.37(6) . . ? C28 C29 H29 120.3 . . ? C30 C29 H29 120.3 . . ? C10 C11 C12 118.94(6) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C22 C23 C24 120.02(8) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C21 C20 C19 119.96(8) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C17 C18 C13 120.05(8) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C40 C39 C38 120.43(9) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C35 C36 C31 120.83(8) . . ? C35 C36 H36 119.6 . . ? C31 C36 H36 119.6 . . ? C11 C10 C9 119.85(6) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C23 C24 C19 120.55(7) . . ? C23 C24 H24 119.7 . . ? C19 C24 H24 119.7 . . ? C5 C4 C3 119.50(7) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C34 C33 C32 120.45(8) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C36 C35 C34 119.77(8) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C46 C45 Si1 112.61(5) . . ? C46 C45 H45A 109.1 . . ? Si1 C45 H45A 109.1 . . ? C46 C45 H45B 109.1 . . ? Si1 C45 H45B 109.1 . . ? H45A C45 H45B 107.8 . . ? C33 C32 C31 119.98(8) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C15 C14 C13 120.37(8) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C17 C16 C15 119.83(8) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C33 C34 C35 120.07(8) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? Si2 C47 H47A 109.5 . . ? Si2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? Si2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C16 C17 C18 120.44(8) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C45 C46 Si2 116.24(6) . . ? C45 C46 H46A 108.2 . . ? Si2 C46 H46A 108.2 . . ? C45 C46 H46B 108.2 . . ? Si2 C46 H46B 108.2 . . ? H46A C46 H46B 107.4 . . ? Si1 C44 H44A 109.5 . . ? Si1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C21 C22 C23 119.78(8) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C22 C21 C20 120.55(8) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C16 C15 C14 120.19(9) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C49 O1 C52 109.39(10) . . ? O1 C49 C50 107.17(10) . . ? O1 C49 H49A 110.3 . . ? C50 C49 H49A 110.3 . . ? O1 C49 H49B 110.3 . . ? C50 C49 H49B 110.3 . . ? H49A C49 H49B 108.5 . . ? O1 C52 C51 107.93(10) . . ? O1 C52 H52A 110.1 . . ? C51 C52 H52A 110.1 . . ? O1 C52 H52B 110.1 . . ? C51 C52 H52B 110.1 . . ? H52A C52 H52B 108.4 . . ? C49 C50 C51 102.94(10) . . ? C49 C50 H50A 111.2 . . ? C51 C50 H50A 111.2 . . ? C49 C50 H50B 111.2 . . ? C51 C50 H50B 111.2 . . ? H50A C50 H50B 109.1 . . ? C52 C51 C50 102.10(12) . . ? C52 C51 H51A 111.4 . . ? C50 C51 H51A 111.4 . . ? C52 C51 H51B 111.3 . . ? C50 C51 H51B 111.3 . . ? H51A C51 H51B 109.2 . . ? C56 O2 C53 104.79(12) . . ? C53 C54 C55 104.15(10) . . ? C53 C54 H54A 110.9 . . ? C55 C54 H54A 110.9 . . ? C53 C54 H54B 110.9 . . ? C55 C54 H54B 110.9 . . ? H54A C54 H54B 108.9 . . ? C56 C55 C54 103.04(11) . . ? C56 C55 H55A 111.2 . . ? C54 C55 H55A 111.2 . . ? C56 C55 H55B 111.2 . . ? C54 C55 H55B 111.2 . . ? H55A C55 H55B 109.1 . . ? O2 C53 C54 106.73(9) . . ? O2 C53 H53A 110.4 . . ? C54 C53 H53A 110.4 . . ? O2 C53 H53B 110.4 . . ? C54 C53 H53B 110.4 . . ? H53A C53 H53B 108.6 . . ? O2 C56 C55 106.30(12) . . ? O2 C56 H56A 110.5 . . ? C55 C56 H56A 110.5 . . ? O2 C56 H56B 110.5 . . ? C55 C56 H56B 110.5 . . ? H56A C56 H56B 108.7 . . ? C1 B1 C26 113.53(5) . . ? C1 B1 C8 108.64(5) . . ? C26 B1 C8 113.76(5) . . ? C1 B1 Fe1 125.67(4) . . ? C26 B1 Fe1 97.49(4) . . ? C8 B1 Fe1 96.70(4) . . ? C1 B1 H101 102.0(6) . . ? C26 B1 H101 109.9(6) . . ? C8 B1 H101 108.2(6) . . ? Fe1 B1 H101 23.7(6) . . ? Si1 C43 H43A 109.5 . . ? Si1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 44.14 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.304 _refine_diff_density_min -0.835 _refine_diff_density_rms 0.081 ####################################################### # Compound 6b: (PhDPBPh)FeNNSi2 # ####################################################### data_6b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H49 B Fe N2 P2 Si2' _chemical_formula_weight 838.67 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' 'Si' 'Si' 0.0817 0.0704 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.7196(6) _cell_length_b 18.1906(11) _cell_length_c 21.7101(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.637(2) _cell_angle_gamma 90.00 _cell_volume 4228.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9395 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 39.07 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 0.526 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9285 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS v2008/1 (Bruker-AXS, 2008)' _exptl_special_details ; 'Bruker KAPPA APEX II' ; _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 196104 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 41.63 _reflns_number_total 28150 _reflns_number_gt 19764 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0438P)^2^+1.0194P] 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 28150 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0750 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1024 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.538048(11) 0.222425(7) 0.826543(5) 0.00753(2) Uani 1 1 d . . . P1 P 0.61908(2) 0.206703(13) 0.920698(10) 0.00834(4) Uani 1 1 d . . . P2 P 0.45373(2) 0.334162(13) 0.829382(10) 0.00918(4) Uani 1 1 d . . . Si1 Si 0.67471(3) 0.269719(16) 0.650303(12) 0.01289(5) Uani 1 1 d . . . Si2 Si 0.88315(2) 0.224512(16) 0.738467(12) 0.01237(5) Uani 1 1 d . . . N1 N 0.63655(7) 0.22847(4) 0.76990(3) 0.00962(11) Uani 1 1 d . . . N2 N 0.71747(7) 0.23819(5) 0.72664(3) 0.01185(13) Uani 1 1 d . . . C19 C 0.65747(8) 0.28450(5) 0.97198(4) 0.00975(13) Uani 1 1 d . . . C11 C 0.47778(10) 0.06702(6) 1.05201(4) 0.01610(16) Uani 1 1 d . . . H11 H 0.5041 0.0401 1.0878 0.019 Uiso 1 1 calc R . . C9 C 0.31399(9) 0.10634(5) 0.97931(4) 0.01357(15) Uani 1 1 d . . . H9 H 0.2288 0.1048 0.9653 0.016 Uiso 1 1 calc R . . C7 C 0.52319(8) 0.14980(5) 0.96920(4) 0.01042(13) Uani 1 1 d . . . C40 C 0.73547(11) 0.51432(6) 0.89492(5) 0.0226(2) Uani 1 1 d . . . H40 H 0.7945 0.5511 0.9071 0.027 Uiso 1 1 calc R . . C38 C 0.67204(9) 0.41383(6) 0.82832(4) 0.01619(16) Uani 1 1 d . . . H38 H 0.6891 0.3816 0.7953 0.019 Uiso 1 1 calc R . . C23 C 0.61184(10) 0.36007(6) 1.05980(4) 0.01714(17) Uani 1 1 d . . . H23 H 0.5596 0.3713 1.0927 0.021 Uiso 1 1 calc R . . C26 C 0.28206(8) 0.27199(5) 0.90143(4) 0.01091(13) Uani 1 1 d . . . C2 C 0.46267(8) 0.10998(5) 0.81791(4) 0.01217(14) Uani 1 1 d . . . C5 C 0.28929(10) 0.13635(6) 0.71940(4) 0.01807(18) Uani 1 1 d . . . C3 C 0.47332(10) 0.07318(6) 0.75996(5) 0.01701(17) Uani 1 1 d . . . C8 C 0.39806(8) 0.15039(5) 0.94798(4) 0.01029(13) Uani 1 1 d . . . C37 C 0.56015(8) 0.40659(5) 0.85857(4) 0.01172(14) Uani 1 1 d . . . C24 C 0.58105(9) 0.30191(5) 1.02018(4) 0.01396(15) Uani 1 1 d . . . H24 H 0.5077 0.2740 1.0260 0.017 Uiso 1 1 calc R . . C41 C 0.62574(11) 0.50694(6) 0.92571(5) 0.02032(19) Uani 1 1 d . . . H41 H 0.6101 0.5385 0.9594 0.024 Uiso 1 1 calc R . . C32 C 0.34637(10) 0.33303(5) 0.70937(4) 0.01527(16) Uani 1 1 d . . . H32 H 0.3503 0.2811 0.7136 0.018 Uiso 1 1 calc R . . C29 C 0.13929(9) 0.40125(6) 0.91693(5) 0.01802(18) Uani 1 1 d . . . H29 H 0.0898 0.4441 0.9213 0.022 Uiso 1 1 calc R . . C36 C 0.39081(9) 0.45400(5) 0.74913(4) 0.01360(15) Uani 1 1 d . . . H36 H 0.4250 0.4852 0.7807 0.016 Uiso 1 1 calc R . . C10 C 0.35317(10) 0.06481(5) 1.03052(4) 0.01563(16) Uani 1 1 d . . . H10 H 0.2950 0.0350 1.0508 0.019 Uiso 1 1 calc R . . C31 C 0.39602(8) 0.37772(5) 0.75684(4) 0.01110(13) Uani 1 1 d . . . C1 C 0.36465(8) 0.16250(5) 0.82561(4) 0.01095(13) Uani 1 1 d . . . C25 C 0.31368(8) 0.33883(5) 0.87361(4) 0.01142(14) Uani 1 1 d . . . C42 C 0.53795(10) 0.45348(6) 0.90767(4) 0.01543(16) Uani 1 1 d . . . H42 H 0.4628 0.4491 0.9289 0.019 Uiso 1 1 calc R . . C35 C 0.33609(10) 0.48471(6) 0.69576(4) 0.01577(16) Uani 1 1 d . . . H35 H 0.3329 0.5366 0.6911 0.019 Uiso 1 1 calc R . . C34 C 0.28604(10) 0.43963(6) 0.64917(5) 0.01760(17) Uani 1 1 d . . . H34 H 0.2484 0.4606 0.6128 0.021 Uiso 1 1 calc R . . C48 C 0.92110(10) 0.12504(6) 0.73321(5) 0.01822(17) Uani 1 1 d . . . H48A H 0.8601 0.0964 0.7554 0.027 Uiso 1 1 calc R . . H48B H 1.0050 0.1162 0.7516 0.027 Uiso 1 1 calc R . . H48C H 0.9182 0.1100 0.6898 0.027 Uiso 1 1 calc R . . C39 C 0.75864(10) 0.46771(7) 0.84612(5) 0.0215(2) Uani 1 1 d . . . H39 H 0.8337 0.4726 0.8248 0.026 Uiso 1 1 calc R . . C22 C 0.71799(10) 0.40154(6) 1.05158(4) 0.01675(17) Uani 1 1 d . . . H22 H 0.7390 0.4408 1.0789 0.020 Uiso 1 1 calc R . . C47 C 0.93980(10) 0.26760(7) 0.81177(5) 0.01983(19) Uani 1 1 d . . . H47A H 0.9029 0.3166 0.8152 0.030 Uiso 1 1 calc R . . H47B H 1.0310 0.2718 0.8124 0.030 Uiso 1 1 calc R . . H47C H 0.9155 0.2371 0.8465 0.030 Uiso 1 1 calc R . . C12 C 0.56316(9) 0.10868(5) 1.02097(4) 0.01376(15) Uani 1 1 d . . . H12 H 0.6485 0.1093 1.0348 0.017 Uiso 1 1 calc R . . C21 C 0.79368(9) 0.38536(6) 1.00302(5) 0.01576(16) Uani 1 1 d . . . H21 H 0.8663 0.4140 0.9970 0.019 Uiso 1 1 calc R . . C27 C 0.17988(9) 0.27337(6) 0.93996(4) 0.01493(15) Uani 1 1 d . . . H27 H 0.1577 0.2297 0.9609 0.018 Uiso 1 1 calc R . . C30 C 0.24075(9) 0.40219(6) 0.87934(5) 0.01582(16) Uani 1 1 d . . . H30 H 0.2606 0.4456 0.8576 0.019 Uiso 1 1 calc R . . C6 C 0.27948(9) 0.17406(6) 0.77348(4) 0.01370(15) Uani 1 1 d . . . C44 C 0.64428(10) 0.37041(6) 0.65156(5) 0.01804(17) Uani 1 1 d . . . H44A H 0.5712 0.3803 0.6758 0.027 Uiso 1 1 calc R . . H44B H 0.6284 0.3881 0.6093 0.027 Uiso 1 1 calc R . . H44C H 0.7172 0.3958 0.6703 0.027 Uiso 1 1 calc R . . C15 C 0.89330(9) 0.05841(5) 0.88291(5) 0.01480(15) Uani 1 1 d . . . H15 H 0.9084 0.0249 0.8505 0.018 Uiso 1 1 calc R . . C13 C 0.76634(8) 0.15451(5) 0.92548(4) 0.01050(13) Uani 1 1 d . . . C17 C 0.95283(9) 0.11078(6) 0.98145(5) 0.01764(17) Uani 1 1 d . . . H17 H 1.0085 0.1129 1.0167 0.021 Uiso 1 1 calc R . . C20 C 0.76351(8) 0.32753(5) 0.96332(4) 0.01290(14) Uani 1 1 d . . . H20 H 0.8152 0.3171 0.9300 0.015 Uiso 1 1 calc R . . C4 C 0.38906(11) 0.08604(6) 0.71217(5) 0.02014(19) Uani 1 1 d . . . C33 C 0.29141(11) 0.36364(6) 0.65618(5) 0.01898(18) Uani 1 1 d . . . H33 H 0.2574 0.3326 0.6245 0.023 Uiso 1 1 calc R . . C18 C 0.84994(9) 0.15731(6) 0.97702(4) 0.01432(15) Uani 1 1 d . . . H18 H 0.8361 0.1913 1.0092 0.017 Uiso 1 1 calc R . . C16 C 0.97453(9) 0.06109(6) 0.93437(5) 0.01710(17) Uani 1 1 d . . . H16 H 1.0447 0.0292 0.9375 0.021 Uiso 1 1 calc R . . C28 C 0.11088(9) 0.33685(6) 0.94813(5) 0.01755(17) Uani 1 1 d . . . H28 H 0.0437 0.3364 0.9752 0.021 Uiso 1 1 calc R . . C43 C 0.54143(11) 0.21640(6) 0.61584(5) 0.02026(19) Uani 1 1 d . . . H43A H 0.5671 0.1653 0.6099 0.030 Uiso 1 1 calc R . . H43B H 0.5151 0.2379 0.5759 0.030 Uiso 1 1 calc R . . H43C H 0.4717 0.2179 0.6435 0.030 Uiso 1 1 calc R . . C14 C 0.78949(8) 0.10469(5) 0.87847(4) 0.01237(14) Uani 1 1 d . . . H14 H 0.7340 0.1023 0.8431 0.015 Uiso 1 1 calc R . . C46 C 0.93077(10) 0.27143(6) 0.66650(5) 0.01791(17) Uani 1 1 d . . . H46A H 0.9358 0.3253 0.6729 0.021 Uiso 1 1 calc R . . H46B H 1.0134 0.2534 0.6545 0.021 Uiso 1 1 calc R . . C45 C 0.82870(9) 0.25255(6) 0.61579(4) 0.01691(17) Uani 1 1 d . . . H45A H 0.8356 0.2005 0.6032 0.020 Uiso 1 1 calc R . . H45B H 0.8380 0.2840 0.5791 0.020 Uiso 1 1 calc R . . B1 B 0.36091(9) 0.19982(6) 0.88942(4) 0.01044(15) Uani 1 1 d . . . H6 H 0.2142(13) 0.2082(8) 0.7781(6) 0.015(3) Uiso 1 1 d . . . H3 H 0.5359(15) 0.0371(9) 0.7572(7) 0.028(4) Uiso 1 1 d . . . H2 H 0.4997(13) 0.0881(8) 0.8541(6) 0.015(3) Uiso 1 1 d . . . H5 H 0.2290(16) 0.1444(9) 0.6851(8) 0.032(4) Uiso 1 1 d . . . H4 H 0.3999(15) 0.0611(9) 0.6746(7) 0.026(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.00726(5) 0.00912(5) 0.00633(4) -0.00025(3) 0.00164(3) 0.00012(4) P1 0.00783(8) 0.01003(9) 0.00723(8) -0.00019(6) 0.00108(6) -0.00027(7) P2 0.00929(9) 0.00963(9) 0.00878(8) -0.00037(6) 0.00211(6) 0.00033(7) Si1 0.01440(11) 0.01559(12) 0.00895(10) 0.00163(8) 0.00360(8) 0.00293(9) Si2 0.01008(10) 0.01564(12) 0.01162(10) -0.00020(8) 0.00308(8) 0.00083(9) N1 0.0098(3) 0.0109(3) 0.0083(3) 0.0000(2) 0.0023(2) 0.0007(2) N2 0.0102(3) 0.0161(3) 0.0097(3) 0.0023(2) 0.0039(2) 0.0012(2) C19 0.0099(3) 0.0115(3) 0.0079(3) -0.0008(2) 0.0006(2) 0.0003(3) C11 0.0205(4) 0.0155(4) 0.0126(4) 0.0045(3) 0.0036(3) 0.0005(3) C9 0.0116(3) 0.0144(4) 0.0151(4) 0.0009(3) 0.0044(3) -0.0016(3) C7 0.0114(3) 0.0114(3) 0.0085(3) 0.0007(2) 0.0018(2) -0.0007(3) C40 0.0254(5) 0.0160(5) 0.0256(5) 0.0020(4) -0.0072(4) -0.0075(4) C38 0.0156(4) 0.0185(4) 0.0146(4) 0.0002(3) 0.0024(3) -0.0038(3) C23 0.0232(4) 0.0169(4) 0.0116(4) -0.0034(3) 0.0039(3) 0.0022(3) C26 0.0089(3) 0.0142(4) 0.0098(3) -0.0005(2) 0.0015(2) 0.0003(3) C2 0.0129(3) 0.0115(4) 0.0122(3) -0.0014(3) 0.0022(3) -0.0012(3) C5 0.0201(4) 0.0214(5) 0.0124(4) -0.0009(3) -0.0027(3) -0.0067(4) C3 0.0196(4) 0.0146(4) 0.0172(4) -0.0061(3) 0.0049(3) -0.0016(3) C8 0.0103(3) 0.0113(3) 0.0095(3) -0.0010(2) 0.0026(2) -0.0006(3) C37 0.0127(3) 0.0108(4) 0.0117(3) 0.0003(3) 0.0006(3) -0.0002(3) C24 0.0151(4) 0.0152(4) 0.0120(3) -0.0018(3) 0.0051(3) -0.0005(3) C41 0.0265(5) 0.0145(4) 0.0193(4) -0.0045(3) -0.0060(4) 0.0007(4) C32 0.0203(4) 0.0127(4) 0.0127(3) -0.0005(3) 0.0001(3) -0.0018(3) C29 0.0148(4) 0.0180(5) 0.0218(4) -0.0025(3) 0.0067(3) 0.0053(3) C36 0.0162(4) 0.0114(4) 0.0131(3) -0.0002(3) 0.0000(3) 0.0008(3) C10 0.0185(4) 0.0135(4) 0.0156(4) 0.0023(3) 0.0079(3) -0.0008(3) C31 0.0114(3) 0.0119(4) 0.0101(3) 0.0002(2) 0.0014(2) 0.0005(3) C1 0.0102(3) 0.0116(4) 0.0110(3) -0.0005(2) 0.0009(2) -0.0025(3) C25 0.0100(3) 0.0133(4) 0.0112(3) -0.0006(3) 0.0027(2) 0.0012(3) C42 0.0174(4) 0.0150(4) 0.0138(4) -0.0030(3) -0.0008(3) 0.0021(3) C35 0.0188(4) 0.0130(4) 0.0154(4) 0.0021(3) -0.0003(3) 0.0021(3) C34 0.0191(4) 0.0187(4) 0.0146(4) 0.0031(3) -0.0037(3) -0.0001(3) C48 0.0189(4) 0.0186(5) 0.0172(4) -0.0002(3) 0.0023(3) 0.0045(4) C39 0.0185(4) 0.0235(5) 0.0224(5) 0.0036(4) 0.0005(4) -0.0088(4) C22 0.0207(4) 0.0146(4) 0.0147(4) -0.0049(3) -0.0024(3) 0.0009(3) C47 0.0154(4) 0.0256(5) 0.0185(4) -0.0057(4) 0.0014(3) -0.0009(4) C12 0.0150(4) 0.0157(4) 0.0106(3) 0.0025(3) 0.0001(3) -0.0004(3) C21 0.0132(4) 0.0146(4) 0.0192(4) -0.0032(3) -0.0018(3) -0.0015(3) C27 0.0120(3) 0.0180(4) 0.0151(4) 0.0012(3) 0.0051(3) 0.0011(3) C30 0.0150(4) 0.0137(4) 0.0192(4) -0.0005(3) 0.0052(3) 0.0030(3) C6 0.0119(3) 0.0161(4) 0.0129(3) 0.0002(3) -0.0013(3) -0.0033(3) C44 0.0211(4) 0.0165(4) 0.0169(4) 0.0036(3) 0.0053(3) 0.0039(3) C15 0.0144(4) 0.0122(4) 0.0180(4) -0.0001(3) 0.0036(3) 0.0022(3) C13 0.0095(3) 0.0110(3) 0.0111(3) 0.0007(2) 0.0014(2) 0.0007(3) C17 0.0131(4) 0.0204(5) 0.0191(4) 0.0017(3) -0.0037(3) 0.0029(3) C20 0.0108(3) 0.0135(4) 0.0145(3) -0.0021(3) 0.0016(3) -0.0003(3) C4 0.0266(5) 0.0202(5) 0.0138(4) -0.0066(3) 0.0030(3) -0.0067(4) C33 0.0252(5) 0.0174(4) 0.0138(4) 0.0005(3) -0.0044(3) -0.0035(4) C18 0.0129(4) 0.0171(4) 0.0128(3) -0.0003(3) -0.0011(3) 0.0019(3) C16 0.0129(4) 0.0154(4) 0.0230(4) 0.0029(3) 0.0007(3) 0.0038(3) C28 0.0124(4) 0.0225(5) 0.0183(4) -0.0015(3) 0.0069(3) 0.0031(3) C43 0.0211(5) 0.0237(5) 0.0158(4) -0.0033(3) -0.0007(3) 0.0016(4) C14 0.0121(3) 0.0131(4) 0.0120(3) -0.0003(3) 0.0014(3) 0.0009(3) C46 0.0159(4) 0.0203(5) 0.0183(4) 0.0022(3) 0.0083(3) 0.0001(3) C45 0.0185(4) 0.0200(5) 0.0129(4) 0.0031(3) 0.0075(3) 0.0033(3) B1 0.0084(3) 0.0123(4) 0.0108(4) -0.0002(3) 0.0019(3) -0.0010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.6610(7) . ? Fe1 C1 2.1542(9) . ? Fe1 P1 2.2026(3) . ? Fe1 C2 2.2041(9) . ? Fe1 P2 2.2264(3) . ? Fe1 B1 2.4242(10) . ? P1 C7 1.8265(9) . ? P1 C19 1.8356(9) . ? P1 C13 1.8409(9) . ? P2 C25 1.8208(9) . ? P2 C37 1.8363(10) . ? P2 C31 1.8442(9) . ? Si1 N2 1.7933(8) . ? Si1 C43 1.8556(12) . ? Si1 C44 1.8608(11) . ? Si1 C45 1.8702(10) . ? Si2 N2 1.8001(8) . ? Si2 C47 1.8512(11) . ? Si2 C48 1.8593(11) . ? Si2 C46 1.8718(10) . ? N1 N2 1.3193(10) . ? C19 C24 1.3947(12) . ? C19 C20 1.3999(13) . ? C11 C12 1.3866(14) . ? C11 C10 1.3950(15) . ? C11 H11 0.9500 . ? C9 C10 1.3930(14) . ? C9 C8 1.4047(12) . ? C9 H9 0.9500 . ? C7 C8 1.3980(12) . ? C7 C12 1.4009(12) . ? C40 C41 1.3860(17) . ? C40 C39 1.3883(17) . ? C40 H40 0.9500 . ? C38 C39 1.3923(15) . ? C38 C37 1.4000(13) . ? C38 H38 0.9500 . ? C23 C22 1.3836(15) . ? C23 C24 1.3936(14) . ? C23 H23 0.9500 . ? C26 C25 1.4059(13) . ? C26 C27 1.4086(12) . ? C26 B1 1.5895(14) . ? C2 C3 1.4342(13) . ? C2 C1 1.4356(13) . ? C2 H2 0.951(14) . ? C5 C6 1.3680(14) . ? C5 C4 1.4218(17) . ? C5 H5 0.974(17) . ? C3 C4 1.3641(16) . ? C3 H3 0.942(17) . ? C8 B1 1.5927(13) . ? C37 C42 1.3942(13) . ? C24 H24 0.9500 . ? C41 C42 1.3967(15) . ? C41 H41 0.9500 . ? C32 C33 1.3886(14) . ? C32 C31 1.3986(13) . ? C32 H32 0.9500 . ? C29 C30 1.3895(13) . ? C29 C28 1.3940(16) . ? C29 H29 0.9500 . ? C36 C35 1.3914(13) . ? C36 C31 1.3985(13) . ? C36 H36 0.9500 . ? C10 H10 0.9500 . ? C1 C6 1.4365(13) . ? C1 B1 1.5450(13) . ? C25 C30 1.4015(13) . ? C42 H42 0.9500 . ? C35 C34 1.3906(14) . ? C35 H35 0.9500 . ? C34 C33 1.3916(15) . ? C34 H34 0.9500 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C39 H39 0.9500 . ? C22 C21 1.3911(14) . ? C22 H22 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C12 H12 0.9500 . ? C21 C20 1.3888(13) . ? C21 H21 0.9500 . ? C27 C28 1.3870(14) . ? C27 H27 0.9500 . ? C30 H30 0.9500 . ? C6 H6 0.944(14) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C15 C16 1.3853(14) . ? C15 C14 1.3952(13) . ? C15 H15 0.9500 . ? C13 C14 1.3956(13) . ? C13 C18 1.4021(13) . ? C17 C18 1.3901(14) . ? C17 C16 1.3920(15) . ? C17 H17 0.9500 . ? C20 H20 0.9500 . ? C4 H4 0.945(16) . ? C33 H33 0.9500 . ? C18 H18 0.9500 . ? C16 H16 0.9500 . ? C28 H28 0.9500 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C14 H14 0.9500 . ? C46 C45 1.5545(15) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C45 H45A 0.9900 . ? C45 H45B 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 Fe1 C1 127.17(4) . . ? N1 Fe1 P1 117.30(3) . . ? C1 Fe1 P1 104.26(2) . . ? N1 Fe1 C2 103.97(4) . . ? C1 Fe1 C2 38.44(3) . . ? P1 Fe1 C2 94.92(3) . . ? N1 Fe1 P2 103.46(3) . . ? C1 Fe1 P2 96.38(3) . . ? P1 Fe1 P2 103.657(10) . . ? C2 Fe1 P2 134.58(3) . . ? N1 Fe1 B1 165.75(4) . . ? C1 Fe1 B1 38.88(3) . . ? P1 Fe1 B1 74.99(2) . . ? C2 Fe1 B1 66.23(3) . . ? P2 Fe1 B1 79.03(3) . . ? C7 P1 C19 101.75(4) . . ? C7 P1 C13 100.32(4) . . ? C19 P1 C13 101.29(4) . . ? C7 P1 Fe1 113.59(3) . . ? C19 P1 Fe1 122.04(3) . . ? C13 P1 Fe1 114.82(3) . . ? C25 P2 C37 107.38(4) . . ? C25 P2 C31 100.25(4) . . ? C37 P2 C31 99.51(4) . . ? C25 P2 Fe1 113.75(3) . . ? C37 P2 Fe1 114.71(3) . . ? C31 P2 Fe1 119.29(3) . . ? N2 Si1 C43 111.39(5) . . ? N2 Si1 C44 109.80(4) . . ? C43 Si1 C44 112.84(5) . . ? N2 Si1 C45 97.13(4) . . ? C43 Si1 C45 115.37(5) . . ? C44 Si1 C45 109.20(5) . . ? N2 Si2 C47 110.28(4) . . ? N2 Si2 C48 110.06(5) . . ? C47 Si2 C48 113.63(5) . . ? N2 Si2 C46 97.07(4) . . ? C47 Si2 C46 115.68(5) . . ? C48 Si2 C46 108.88(5) . . ? N2 N1 Fe1 175.62(7) . . ? N1 N2 Si1 123.53(6) . . ? N1 N2 Si2 123.82(6) . . ? Si1 N2 Si2 112.62(4) . . ? C24 C19 C20 118.85(8) . . ? C24 C19 P1 120.46(7) . . ? C20 C19 P1 120.69(6) . . ? C12 C11 C10 119.77(9) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C10 C9 C8 121.28(9) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C8 C7 C12 121.46(8) . . ? C8 C7 P1 111.26(6) . . ? C12 C7 P1 127.28(7) . . ? C41 C40 C39 119.64(10) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C39 C38 C37 120.71(10) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C22 C23 C24 120.47(9) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C26 C27 116.69(8) . . ? C25 C26 B1 120.22(7) . . ? C27 C26 B1 123.09(8) . . ? C3 C2 C1 120.06(9) . . ? C3 C2 Fe1 117.65(7) . . ? C1 C2 Fe1 68.89(5) . . ? C3 C2 H2 118.8(8) . . ? C1 C2 H2 117.6(8) . . ? Fe1 C2 H2 100.5(9) . . ? C6 C5 C4 120.36(9) . . ? C6 C5 H5 120.4(10) . . ? C4 C5 H5 119.3(10) . . ? C4 C3 C2 120.70(10) . . ? C4 C3 H3 121.3(10) . . ? C2 C3 H3 117.8(10) . . ? C7 C8 C9 117.60(8) . . ? C7 C8 B1 117.92(7) . . ? C9 C8 B1 124.48(8) . . ? C42 C37 C38 118.76(9) . . ? C42 C37 P2 125.29(7) . . ? C38 C37 P2 115.95(7) . . ? C23 C24 C19 120.32(9) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? C40 C41 C42 120.53(10) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C33 C32 C31 120.82(9) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C30 C29 C28 119.34(9) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C35 C36 C31 120.73(9) . . ? C35 C36 H36 119.6 . . ? C31 C36 H36 119.6 . . ? C9 C10 C11 120.01(9) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C36 C31 C32 118.48(8) . . ? C36 C31 P2 122.58(7) . . ? C32 C31 P2 118.74(7) . . ? C2 C1 C6 116.60(8) . . ? C2 C1 B1 116.49(8) . . ? C6 C1 B1 126.90(8) . . ? C2 C1 Fe1 72.66(5) . . ? C6 C1 Fe1 116.76(6) . . ? B1 C1 Fe1 80.05(5) . . ? C30 C25 C26 121.76(8) . . ? C30 C25 P2 124.20(7) . . ? C26 C25 P2 114.03(7) . . ? C37 C42 C41 120.26(10) . . ? C37 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C34 C35 C36 120.18(9) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C34 C33 119.58(9) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? Si2 C48 H48A 109.5 . . ? Si2 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si2 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C40 C39 C38 120.09(10) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C23 C22 C21 119.62(9) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? Si2 C47 H47A 109.5 . . ? Si2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? Si2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C11 C12 C7 119.83(9) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C20 C21 C22 120.22(9) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C28 C27 C26 121.64(9) . . ? C28 C27 H27 119.2 . . ? C26 C27 H27 119.2 . . ? C29 C30 C25 119.81(9) . . ? C29 C30 H30 120.1 . . ? C25 C30 H30 120.1 . . ? C5 C6 C1 122.11(9) . . ? C5 C6 H6 120.4(9) . . ? C1 C6 H6 117.4(9) . . ? Si1 C44 H44A 109.5 . . ? Si1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C16 C15 C14 120.27(9) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C14 C13 C18 118.60(8) . . ? C14 C13 P1 118.33(7) . . ? C18 C13 P1 122.76(7) . . ? C18 C17 C16 120.23(9) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C21 C20 C19 120.50(8) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C3 C4 C5 120.10(9) . . ? C3 C4 H4 118.1(10) . . ? C5 C4 H4 121.8(10) . . ? C32 C33 C34 120.21(9) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C17 C18 C13 120.60(9) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? C15 C16 C17 119.67(9) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C27 C28 C29 120.51(9) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? Si1 C43 H43A 109.5 . . ? Si1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C15 C14 C13 120.63(8) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C45 C46 Si2 106.28(7) . . ? C45 C46 H46A 110.5 . . ? Si2 C46 H46A 110.5 . . ? C45 C46 H46B 110.5 . . ? Si2 C46 H46B 110.5 . . ? H46A C46 H46B 108.7 . . ? C46 C45 Si1 106.54(6) . . ? C46 C45 H45A 110.4 . . ? Si1 C45 H45A 110.4 . . ? C46 C45 H45B 110.4 . . ? Si1 C45 H45B 110.4 . . ? H45A C45 H45B 108.6 . . ? C1 B1 C26 123.09(8) . . ? C1 B1 C8 116.86(8) . . ? C26 B1 C8 116.79(7) . . ? C1 B1 Fe1 61.07(4) . . ? C26 B1 Fe1 112.86(6) . . ? C8 B1 Fe1 111.82(6) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.789 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.087 ####################################################### # Compound 3b: (PhDPBPh)FeBr # ####################################################### data_3b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H16.50 B0.50 Br0.50 Fe0.50 P' _chemical_formula_weight 373.10 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' '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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6143(6) _cell_length_b 9.7710(5) _cell_length_c 19.9222(14) _cell_angle_alpha 87.525(3) _cell_angle_beta 88.376(4) _cell_angle_gamma 68.912(2) _cell_volume 1744.39(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9908 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 25.02 _exptl_crystal_description chunk _exptl_crystal_colour brown _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 762 _exptl_absorpt_coefficient_mu 1.699 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; 'Bruker KAPPA APEX II' ; _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 66744 _diffrn_reflns_av_R_equivalents 0.0822 _diffrn_reflns_av_sigmaI/netI 0.0710 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.11 _reflns_number_total 7693 _reflns_number_gt 5280 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0624P)^2^+0.1178P] 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 7693 _refine_ls_number_parameters 444 _refine_ls_number_restraints 434 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1196 _refine_ls_wR_factor_gt 0.1122 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br -0.28361(4) 0.07588(4) 0.248641(19) 0.02982(12) Uani 1 1 d U . . Fe1 Fe -0.07894(5) 0.15146(5) 0.25024(2) 0.01773(13) Uani 1 1 d U . . P1 P -0.08730(9) 0.29279(9) 0.15115(4) 0.0184(2) Uani 1 1 d U . . P2 P -0.10991(10) 0.29643(9) 0.34457(4) 0.0205(2) Uani 1 1 d U . . C13 C -0.1914(4) 0.4892(4) 0.15056(15) 0.0209(7) Uani 1 1 d U . . C31 C -0.2217(4) 0.4913(4) 0.33803(16) 0.0256(8) Uani 1 1 d U . . C1 C 0.1554(3) 0.0062(4) 0.25710(16) 0.0220(7) Uani 1 1 d U . . C7 C 0.1027(4) 0.2724(4) 0.12816(16) 0.0211(7) Uani 1 1 d U . . C25 C 0.0736(4) 0.2851(4) 0.36999(16) 0.0231(7) Uani 1 1 d U . . C8 C 0.2050(4) 0.2208(4) 0.18083(17) 0.0227(7) Uani 1 1 d U . . C27 C 0.3283(4) 0.2301(4) 0.33776(18) 0.0283(8) Uani 1 1 d U . . H27 H 0.4069 0.1991 0.3054 0.034 Uiso 1 1 calc R . . C18 C -0.1205(4) 0.5898(4) 0.1468(2) 0.0346(9) Uani 1 1 d U . . H18 H -0.0149 0.5573 0.1434 0.041 Uiso 1 1 calc R . . C30 C 0.1035(4) 0.3263(4) 0.43271(18) 0.0288(8) Uani 1 1 d U . . H30 H 0.0258 0.3592 0.4653 0.035 Uiso 1 1 calc R . . C14 C -0.3456(4) 0.5381(4) 0.15571(18) 0.0297(8) Uani 1 1 d U . . H14 H -0.3950 0.4696 0.1597 0.036 Uiso 1 1 calc R . . C32 C -0.1625(4) 0.5988(4) 0.34770(19) 0.0342(9) Uani 1 1 d U . . H32 H -0.0598 0.5724 0.3574 0.041 Uiso 1 1 calc R . . C26 C 0.1867(4) 0.2327(4) 0.32081(16) 0.0210(7) Uani 1 1 d U . . C38 C -0.1868(4) 0.0939(4) 0.42483(18) 0.0326(9) Uani 1 1 d U . . H38 H -0.1336 0.0258 0.3921 0.039 Uiso 1 1 calc R . . C15 C -0.4279(4) 0.6889(4) 0.15505(18) 0.0331(9) Uani 1 1 d U . . H15 H -0.5337 0.7224 0.1571 0.040 Uiso 1 1 calc R . . C20 C -0.1507(4) 0.0900(4) 0.07571(18) 0.0285(8) Uani 1 1 d U . . H20 H -0.0988 0.0216 0.1100 0.034 Uiso 1 1 calc R . . C12 C 0.1460(4) 0.3048(4) 0.06330(17) 0.0271(8) Uani 1 1 d U . . H12 H 0.0743 0.3391 0.0288 0.033 Uiso 1 1 calc R . . C5 C 0.1407(4) -0.2077(4) 0.2026(2) 0.0304(8) Uani 1 1 d U . . C9 C 0.3522(4) 0.2066(4) 0.16520(18) 0.0316(9) Uani 1 1 d U . . H9 H 0.4247 0.1734 0.1995 0.038 Uiso 1 1 calc R . . C6 C 0.1535(4) -0.0715(4) 0.19863(19) 0.0255(8) Uani 1 1 d U . . C28 C 0.3577(4) 0.2709(4) 0.39982(19) 0.0352(9) Uani 1 1 d U . . H28 H 0.4556 0.2658 0.4097 0.042 Uiso 1 1 calc R . . C10 C 0.3964(4) 0.2392(4) 0.10140(19) 0.0343(9) Uani 1 1 d U . . H10 H 0.4973 0.2290 0.0929 0.041 Uiso 1 1 calc R . . C19 C -0.1635(4) 0.2359(4) 0.07849(16) 0.0217(7) Uani 1 1 d U . . C2 C 0.1354(4) -0.0623(4) 0.31797(19) 0.0259(8) Uani 1 1 d U . . C17 C -0.2054(5) 0.7398(4) 0.1481(2) 0.0452(11) Uani 1 1 d U . . H17 H -0.1564 0.8088 0.1467 0.054 Uiso 1 1 calc R . . C42 C -0.2776(4) 0.3368(4) 0.46711(17) 0.0288(8) Uani 1 1 d U . . H42 H -0.2876 0.4371 0.4631 0.035 Uiso 1 1 calc R . . C36 C -0.3726(4) 0.5312(4) 0.32349(18) 0.0337(9) Uani 1 1 d U . . H36 H -0.4141 0.4583 0.3164 0.040 Uiso 1 1 calc R . . C3 C 0.1223(4) -0.1990(4) 0.3210(2) 0.0291(9) Uani 1 1 d U . . C24 C -0.2396(4) 0.3329(4) 0.02735(17) 0.0324(9) Uani 1 1 d U . . H24 H -0.2484 0.4328 0.0278 0.039 Uiso 1 1 calc R . . C16 C -0.3578(5) 0.7887(4) 0.15148(19) 0.0360(9) Uani 1 1 d U . . H16 H -0.4144 0.8909 0.1513 0.043 Uiso 1 1 calc R . . C41 C -0.3424(4) 0.2886(4) 0.52054(17) 0.0330(9) Uani 1 1 d U . . H41 H -0.3949 0.3556 0.5538 0.040 Uiso 1 1 calc R . . C37 C -0.1963(4) 0.2387(4) 0.41809(16) 0.0221(7) Uani 1 1 d U . . C4 C 0.1252(4) -0.2724(4) 0.2637(2) 0.0306(9) Uani 1 1 d U . . C29 C 0.2449(4) 0.3193(4) 0.44751(18) 0.0330(9) Uani 1 1 d U . . H29 H 0.2649 0.3475 0.4902 0.040 Uiso 1 1 calc R . . C22 C -0.2906(4) 0.1420(5) -0.02545(18) 0.0371(10) Uani 1 1 d U . . H22 H -0.3363 0.1109 -0.0604 0.044 Uiso 1 1 calc R . . C23 C -0.3024(5) 0.2859(5) -0.02379(18) 0.0410(10) Uani 1 1 d U . . H23 H -0.3544 0.3537 -0.0583 0.049 Uiso 1 1 calc R . . C34 C -0.4039(5) 0.7857(4) 0.32905(19) 0.0429(11) Uani 1 1 d U . . H34 H -0.4665 0.8862 0.3260 0.052 Uiso 1 1 calc R . . C11 C 0.2929(4) 0.2869(4) 0.04986(18) 0.0316(9) Uani 1 1 d U . . H11 H 0.3233 0.3068 0.0059 0.038 Uiso 1 1 calc R . . C40 C -0.3330(4) 0.1452(4) 0.52695(18) 0.0348(9) Uani 1 1 d U . . H40 H -0.3800 0.1136 0.5639 0.042 Uiso 1 1 calc R . . C21 C -0.2128(4) 0.0429(4) 0.02341(18) 0.0340(9) Uani 1 1 d U . . H21 H -0.2014 -0.0575 0.0215 0.041 Uiso 1 1 calc R . . C39 C -0.2551(5) 0.0477(4) 0.47956(19) 0.0396(10) Uani 1 1 d U . . H39 H -0.2475 -0.0519 0.4840 0.048 Uiso 1 1 calc R . . C35 C -0.4611(4) 0.6789(4) 0.3195(2) 0.0404(10) Uani 1 1 d U . . H35 H -0.5640 0.7064 0.3099 0.049 Uiso 1 1 calc R . . B1 B 0.1571(4) 0.1670(4) 0.25234(19) 0.0211(8) Uani 1 1 d U . . C33 C -0.2553(5) 0.7467(4) 0.3430(2) 0.0448(11) Uani 1 1 d U . . H33 H -0.2151 0.8208 0.3496 0.054 Uiso 1 1 calc R . . H5 H 0.146(3) -0.253(3) 0.1578(15) 0.010(8) Uiso 1 1 d . . . H2 H 0.144(4) -0.025(4) 0.3560(17) 0.023(10) Uiso 1 1 d . . . H3 H 0.121(4) -0.236(4) 0.3556(18) 0.023(11) Uiso 1 1 d . . . H6 H 0.156(3) -0.029(3) 0.1529(16) 0.017(8) Uiso 1 1 d . . . H4 H 0.114(4) -0.365(4) 0.2689(17) 0.028(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.01844(19) 0.0344(2) 0.0382(2) 0.00002(17) 0.00248(15) -0.01174(16) Fe1 0.0135(2) 0.0192(3) 0.0186(2) -0.00236(19) 0.00228(18) -0.00356(19) P1 0.0167(4) 0.0209(5) 0.0174(4) -0.0023(3) 0.0002(3) -0.0062(4) P2 0.0207(5) 0.0200(5) 0.0184(4) -0.0025(4) 0.0044(4) -0.0045(4) C13 0.0227(18) 0.0250(18) 0.0130(16) -0.0018(13) -0.0048(13) -0.0055(14) C31 0.0278(19) 0.0290(19) 0.0154(17) -0.0028(14) 0.0087(14) -0.0053(15) C1 0.0132(16) 0.0229(18) 0.0228(17) -0.0041(13) 0.0004(13) 0.0022(13) C7 0.0199(17) 0.0238(19) 0.0194(17) -0.0056(14) 0.0032(13) -0.0071(14) C25 0.0280(18) 0.0202(18) 0.0199(17) 0.0008(14) 0.0015(14) -0.0076(15) C8 0.0171(17) 0.0257(19) 0.0236(17) -0.0069(14) 0.0022(14) -0.0049(15) C27 0.029(2) 0.031(2) 0.0254(19) -0.0034(16) 0.0024(15) -0.0114(17) C18 0.029(2) 0.027(2) 0.049(2) 0.0017(18) -0.0083(18) -0.0126(17) C30 0.038(2) 0.026(2) 0.0249(19) -0.0071(15) 0.0066(16) -0.0144(17) C14 0.0242(19) 0.031(2) 0.031(2) -0.0033(16) 0.0029(16) -0.0058(16) C32 0.035(2) 0.024(2) 0.041(2) 0.0010(17) 0.0114(18) -0.0097(17) C26 0.0203(17) 0.0192(18) 0.0219(17) 0.0031(14) 0.0004(13) -0.0055(14) C38 0.036(2) 0.027(2) 0.027(2) 0.0015(16) 0.0116(17) -0.0030(17) C15 0.028(2) 0.033(2) 0.031(2) -0.0024(17) -0.0048(16) -0.0021(17) C20 0.025(2) 0.032(2) 0.029(2) -0.0075(16) 0.0007(15) -0.0101(16) C12 0.0280(19) 0.030(2) 0.0228(18) 0.0003(15) 0.0001(15) -0.0097(16) C5 0.023(2) 0.034(2) 0.033(2) -0.0112(17) 0.0040(16) -0.0078(16) C9 0.0195(18) 0.044(2) 0.028(2) -0.0052(17) 0.0008(15) -0.0074(17) C6 0.0152(17) 0.029(2) 0.029(2) -0.0049(16) 0.0022(15) -0.0033(15) C28 0.034(2) 0.039(2) 0.039(2) 0.0015(18) -0.0062(17) -0.0211(19) C10 0.0212(19) 0.045(2) 0.037(2) -0.0033(18) 0.0084(16) -0.0128(18) C19 0.0200(18) 0.031(2) 0.0145(16) -0.0056(14) 0.0037(13) -0.0098(15) C2 0.0215(19) 0.026(2) 0.0251(19) -0.0035(15) -0.0003(15) -0.0019(15) C17 0.051(3) 0.026(2) 0.064(3) 0.005(2) -0.020(2) -0.020(2) C42 0.030(2) 0.032(2) 0.0216(18) -0.0064(15) 0.0040(15) -0.0085(17) C36 0.033(2) 0.031(2) 0.030(2) -0.0008(17) 0.0012(17) -0.0032(17) C3 0.024(2) 0.027(2) 0.032(2) 0.0011(18) 0.0028(17) -0.0049(16) C24 0.047(2) 0.033(2) 0.0195(18) 0.0011(15) -0.0021(16) -0.0180(19) C16 0.043(2) 0.021(2) 0.032(2) -0.0036(16) -0.0119(18) 0.0033(17) C41 0.032(2) 0.045(2) 0.0172(18) -0.0032(17) 0.0029(15) -0.0082(18) C37 0.0201(18) 0.0260(19) 0.0192(17) -0.0017(14) 0.0016(13) -0.0071(15) C4 0.022(2) 0.025(2) 0.043(2) -0.0044(17) 0.0038(17) -0.0070(16) C29 0.050(2) 0.032(2) 0.026(2) -0.0066(17) -0.0008(17) -0.0243(19) C22 0.042(2) 0.060(3) 0.0163(18) -0.0135(18) 0.0036(16) -0.027(2) C23 0.049(3) 0.057(3) 0.0178(19) 0.0020(18) -0.0087(17) -0.020(2) C34 0.053(3) 0.028(2) 0.033(2) 0.0063(17) 0.022(2) 0.0014(19) C11 0.036(2) 0.036(2) 0.0235(19) -0.0004(16) 0.0101(16) -0.0151(18) C40 0.030(2) 0.051(3) 0.0189(19) 0.0104(17) 0.0016(15) -0.0104(19) C21 0.033(2) 0.040(2) 0.030(2) -0.0119(17) 0.0045(17) -0.0137(18) C39 0.050(3) 0.028(2) 0.034(2) 0.0100(17) 0.0067(19) -0.0075(19) C35 0.031(2) 0.037(2) 0.039(2) 0.0046(19) 0.0146(18) 0.0039(18) B1 0.0115(17) 0.026(2) 0.0218(19) -0.0023(16) 0.0017(14) -0.0012(16) C33 0.059(3) 0.023(2) 0.051(3) 0.0041(19) 0.014(2) -0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Fe1 2.3388(6) . ? Fe1 C1 2.193(3) . ? Fe1 B1 2.330(4) . ? Fe1 P1 2.3460(10) . ? Fe1 P2 2.3499(10) . ? Fe1 C2 2.692(4) . ? Fe1 C6 2.712(3) . ? P1 C7 1.812(3) . ? P1 C13 1.817(3) . ? P1 C19 1.834(3) . ? P2 C25 1.813(4) . ? P2 C31 1.820(4) . ? P2 C37 1.830(3) . ? C13 C18 1.382(5) . ? C13 C14 1.387(5) . ? C31 C32 1.385(5) . ? C31 C36 1.396(5) . ? C1 C2 1.402(5) . ? C1 C6 1.421(5) . ? C1 B1 1.576(5) . ? C7 C12 1.405(5) . ? C7 C8 1.407(5) . ? C25 C30 1.398(5) . ? C25 C26 1.410(4) . ? C8 C9 1.399(5) . ? C8 B1 1.610(5) . ? C27 C28 1.383(5) . ? C27 C26 1.403(5) . ? C27 H27 0.9500 . ? C18 C17 1.399(5) . ? C18 H18 0.9500 . ? C30 C29 1.376(5) . ? C30 H30 0.9500 . ? C14 C15 1.399(5) . ? C14 H14 0.9500 . ? C32 C33 1.399(5) . ? C32 H32 0.9500 . ? C26 B1 1.607(5) . ? C38 C37 1.386(5) . ? C38 C39 1.398(5) . ? C38 H38 0.9500 . ? C15 C16 1.370(5) . ? C15 H15 0.9500 . ? C20 C21 1.389(5) . ? C20 C19 1.389(5) . ? C20 H20 0.9500 . ? C12 C11 1.379(5) . ? C12 H12 0.9500 . ? C5 C4 1.377(5) . ? C5 C6 1.379(5) . ? C5 H5 1.00(3) . ? C9 C10 1.389(5) . ? C9 H9 0.9500 . ? C6 H6 0.99(3) . ? C28 C29 1.383(5) . ? C28 H28 0.9500 . ? C10 C11 1.394(5) . ? C10 H10 0.9500 . ? C19 C24 1.390(5) . ? C2 C3 1.384(5) . ? C2 H2 0.87(3) . ? C17 C16 1.369(6) . ? C17 H17 0.9500 . ? C42 C41 1.369(5) . ? C42 C37 1.408(4) . ? C42 H42 0.9500 . ? C36 C35 1.387(5) . ? C36 H36 0.9500 . ? C3 C4 1.369(5) . ? C3 H3 0.76(4) . ? C24 C23 1.374(5) . ? C24 H24 0.9500 . ? C16 H16 0.9500 . ? C41 C40 1.371(5) . ? C41 H41 0.9500 . ? C4 H4 0.95(4) . ? C29 H29 0.9500 . ? C22 C23 1.371(6) . ? C22 C21 1.372(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C34 C35 1.365(6) . ? C34 C33 1.374(6) . ? C34 H34 0.9500 . ? C11 H11 0.9500 . ? C40 C39 1.373(5) . ? C40 H40 0.9500 . ? C21 H21 0.9500 . ? C39 H39 0.9500 . ? C35 H35 0.9500 . ? C33 H33 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 C1 Fe1 B1 40.64(13) . . ? C1 Fe1 Br1 125.74(9) . . ? B1 Fe1 Br1 166.36(10) . . ? C1 Fe1 P1 104.04(9) . . ? B1 Fe1 P1 80.20(10) . . ? Br1 Fe1 P1 106.78(3) . . ? C1 Fe1 P2 102.46(9) . . ? B1 Fe1 P2 80.60(9) . . ? Br1 Fe1 P2 107.03(3) . . ? P1 Fe1 P2 110.33(4) . . ? C1 Fe1 C2 31.28(11) . . ? B1 Fe1 C2 62.28(13) . . ? Br1 Fe1 C2 106.06(8) . . ? P1 Fe1 C2 135.30(8) . . ? P2 Fe1 C2 87.74(9) . . ? C1 Fe1 C6 31.48(11) . . ? B1 Fe1 C6 62.00(12) . . ? Br1 Fe1 C6 105.70(8) . . ? P1 Fe1 C6 89.85(8) . . ? P2 Fe1 C6 133.94(8) . . ? C2 Fe1 C6 52.31(11) . . ? C7 P1 C13 105.81(16) . . ? C7 P1 C19 106.05(14) . . ? C13 P1 C19 102.14(15) . . ? C7 P1 Fe1 107.58(11) . . ? C13 P1 Fe1 119.41(11) . . ? C19 P1 Fe1 114.82(11) . . ? C25 P2 C31 105.85(16) . . ? C25 P2 C37 106.53(15) . . ? C31 P2 C37 101.08(15) . . ? C25 P2 Fe1 107.66(11) . . ? C31 P2 Fe1 119.58(11) . . ? C37 P2 Fe1 115.12(11) . . ? C18 C13 C14 119.6(3) . . ? C18 C13 P1 121.7(3) . . ? C14 C13 P1 118.7(3) . . ? C32 C31 C36 119.8(3) . . ? C32 C31 P2 122.4(3) . . ? C36 C31 P2 117.8(3) . . ? C2 C1 C6 115.1(3) . . ? C2 C1 B1 122.8(3) . . ? C6 C1 B1 121.6(3) . . ? C2 C1 Fe1 94.4(2) . . ? C6 C1 Fe1 94.9(2) . . ? B1 C1 Fe1 74.36(18) . . ? C12 C7 C8 122.1(3) . . ? C12 C7 P1 123.4(3) . . ? C8 C7 P1 114.5(2) . . ? C30 C25 C26 121.4(3) . . ? C30 C25 P2 123.8(3) . . ? C26 C25 P2 114.8(2) . . ? C9 C8 C7 116.0(3) . . ? C9 C8 B1 122.4(3) . . ? C7 C8 B1 121.3(3) . . ? C28 C27 C26 122.4(3) . . ? C28 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? C13 C18 C17 119.5(4) . . ? C13 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C29 C30 C25 120.4(3) . . ? C29 C30 H30 119.8 . . ? C25 C30 H30 119.8 . . ? C13 C14 C15 119.6(3) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C31 C32 C33 119.5(4) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C27 C26 C25 116.0(3) . . ? C27 C26 B1 122.4(3) . . ? C25 C26 B1 121.4(3) . . ? C37 C38 C39 120.3(3) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C16 C15 C14 120.8(4) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C21 C20 C19 120.8(4) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C11 C12 C7 119.9(3) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C4 C5 C6 121.0(4) . . ? C4 C5 H5 125.2(17) . . ? C6 C5 H5 113.8(17) . . ? C10 C9 C8 122.5(3) . . ? C10 C9 H9 118.8 . . ? C8 C9 H9 118.8 . . ? C5 C6 C1 121.7(3) . . ? C5 C6 Fe1 115.8(2) . . ? C1 C6 Fe1 53.66(16) . . ? C5 C6 H6 116.2(18) . . ? C1 C6 H6 122.0(18) . . ? Fe1 C6 H6 98.7(18) . . ? C27 C28 C29 120.2(4) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C9 C10 C11 120.1(3) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C20 C19 C24 118.1(3) . . ? C20 C19 P1 118.6(3) . . ? C24 C19 P1 123.2(3) . . ? C3 C2 C1 122.4(4) . . ? C3 C2 Fe1 116.0(3) . . ? C1 C2 Fe1 54.31(17) . . ? C3 C2 H2 117(2) . . ? C1 C2 H2 120(2) . . ? Fe1 C2 H2 106(2) . . ? C16 C17 C18 121.0(4) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C41 C42 C37 120.5(4) . . ? C41 C42 H42 119.8 . . ? C37 C42 H42 119.8 . . ? C35 C36 C31 119.0(4) . . ? C35 C36 H36 120.5 . . ? C31 C36 H36 120.5 . . ? C4 C3 C2 120.8(4) . . ? C4 C3 H3 120(3) . . ? C2 C3 H3 118(3) . . ? C23 C24 C19 120.8(4) . . ? C23 C24 H24 119.6 . . ? C19 C24 H24 119.6 . . ? C17 C16 C15 119.4(4) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C42 C41 C40 121.2(3) . . ? C42 C41 H41 119.4 . . ? C40 C41 H41 119.4 . . ? C38 C37 C42 118.2(3) . . ? C38 C37 P2 119.0(2) . . ? C42 C37 P2 122.8(3) . . ? C3 C4 C5 118.9(4) . . ? C3 C4 H4 117(2) . . ? C5 C4 H4 124(2) . . ? C30 C29 C28 119.5(3) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C23 C22 C21 120.0(4) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.5(4) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C35 C34 C33 119.5(4) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C12 C11 C10 119.4(3) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C41 C40 C39 119.5(3) . . ? C41 C40 H40 120.3 . . ? C39 C40 H40 120.3 . . ? C22 C21 C20 119.8(4) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C40 C39 C38 120.5(4) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C34 C35 C36 121.6(4) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C1 B1 C26 116.7(3) . . ? C1 B1 C8 116.5(3) . . ? C26 B1 C8 120.6(3) . . ? C1 B1 Fe1 65.00(17) . . ? C26 B1 Fe1 112.6(2) . . ? C8 B1 Fe1 112.3(2) . . ? C34 C33 C32 120.5(4) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.545 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.088 ####################################################### # Compound 5: (PhDPBPh)Fe # ####################################################### data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H45 B1 Fe1 P2' _chemical_formula_weight 822.5 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' '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 9.8333(19) _cell_length_b 11.167(3) _cell_length_c 19.774(3) _cell_angle_alpha 78.661(7) _cell_angle_beta 76.780(5) _cell_angle_gamma 88.148(8) _cell_volume 2072.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9879 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 39.42 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 0.479 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; 'Bruker KAPPA APEX II' ; _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.19 _diffrn_reflns_number 88753 _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_sigmaI/netI 0.0894 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 41.29 _reflns_number_total 25823 _reflns_number_gt 16012 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0606P)^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 25823 _refine_ls_number_parameters 543 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0929 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1311 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.622033(16) -0.004282(14) 0.798619(8) 0.00786(4) Uani 1 1 d . . . P1 P 0.67347(3) 0.01415(3) 0.683637(15) 0.00842(5) Uani 1 1 d . . . P2 P 0.58502(3) -0.20086(3) 0.833668(15) 0.00850(5) Uani 1 1 d . . . C27 C 0.99749(12) -0.23219(10) 0.83691(6) 0.0124(2) Uani 1 1 d . . . H27 H 1.0772 -0.1796 0.8214 0.015 Uiso 1 1 calc R . . C26 C 0.86819(11) -0.18655(10) 0.82498(6) 0.00972(18) Uani 1 1 d . . . C44 C 0.10707(15) 0.19588(15) 0.83790(8) 0.0254(3) Uani 1 1 d . . . H44 H 0.0864 0.1877 0.7944 0.031 Uiso 1 1 calc R . . C25 C 0.75259(11) -0.26890(10) 0.84699(6) 0.01003(18) Uani 1 1 d . . . C24 C 0.45413(12) 0.16532(11) 0.65683(6) 0.0138(2) Uani 1 1 d . . . H24 H 0.3983 0.0962 0.6827 0.017 Uiso 1 1 calc R . . C5 C 0.53335(12) 0.03681(11) 0.90227(6) 0.0123(2) Uani 1 1 d . . . C35 C 0.44835(16) -0.48038(12) 0.75373(8) 0.0223(3) Uani 1 1 d . . . H35 H 0.4652 -0.5646 0.7538 0.027 Uiso 1 1 calc R . . C51 C 1.04302(15) -0.35805(14) 0.63340(9) 0.0277(3) Uani 1 1 d . . . H51 H 1.0549 -0.2724 0.6285 0.033 Uiso 1 1 calc R . . C48 C 0.16806(15) 0.32243(12) 0.91231(8) 0.0233(3) Uani 1 1 d . . . H48 H 0.1904 0.4005 0.9195 0.028 Uiso 1 1 calc R . . C52 C 0.97586(16) -0.42775(14) 0.69765(8) 0.0243(3) Uani 1 1 d . . . H52 H 0.9412 -0.3897 0.7371 0.029 Uiso 1 1 calc R . . C46 C 0.13339(13) 0.10643(12) 0.95505(8) 0.0195(2) Uani 1 1 d . . . H46 H 0.1330 0.0365 0.9913 0.023 Uiso 1 1 calc R . . C19 C 0.60022(12) 0.15584(10) 0.64188(6) 0.01051(18) Uani 1 1 d . . . C8 C 0.93789(11) -0.00235(10) 0.70789(6) 0.01007(18) Uani 1 1 d . . . C7 C 0.86423(11) 0.03064(10) 0.65385(6) 0.01033(18) Uani 1 1 d . . . B1 B 0.85187(13) -0.04757(11) 0.78806(7) 0.0101(2) Uani 1 1 d . . . C37 C 0.46503(12) -0.24435(10) 0.92191(6) 0.01102(19) Uani 1 1 d . . . C14 C 0.55451(13) -0.08134(11) 0.58514(6) 0.0134(2) Uani 1 1 d . . . H14 H 0.5047 -0.0073 0.5784 0.016 Uiso 1 1 calc R . . C28 C 1.01231(13) -0.35193(11) 0.87072(7) 0.0150(2) Uani 1 1 d . . . H28 H 1.1011 -0.3799 0.8780 0.018 Uiso 1 1 calc R . . C11 C 1.07916(13) 0.07237(12) 0.56393(7) 0.0160(2) Uani 1 1 d . . . H11 H 1.1266 0.0981 0.5158 0.019 Uiso 1 1 calc R . . C13 C 0.64448(12) -0.09807(10) 0.63128(6) 0.01003(18) Uani 1 1 d . . . C42 C 0.50956(13) -0.28878(11) 0.98392(6) 0.0144(2) Uani 1 1 d . . . H42 H 0.6056 -0.3061 0.9816 0.017 Uiso 1 1 calc R . . C47 C 0.16304(13) 0.22074(12) 0.96571(7) 0.0189(2) Uani 1 1 d . . . H47 H 0.1800 0.2294 1.0099 0.023 Uiso 1 1 calc R . . C1 C 0.77981(11) 0.04850(10) 0.83193(6) 0.00994(18) Uani 1 1 d . . . C54 C 1.00967(15) -0.60908(15) 0.64726(9) 0.0262(3) Uani 1 1 d . . . H54 H 0.9988 -0.6948 0.6521 0.031 Uiso 1 1 calc R . . C53 C 0.95890(16) -0.55249(14) 0.70477(8) 0.0243(3) Uani 1 1 d . . . H53 H 0.9125 -0.5997 0.7490 0.029 Uiso 1 1 calc R . . C4 C 0.49032(13) 0.12792(11) 0.85142(6) 0.0130(2) Uani 1 1 d . . . C6 C 0.67459(12) 0.00037(10) 0.89437(6) 0.01120(19) Uani 1 1 d . . . C17 C 0.70104(14) -0.29858(11) 0.60328(7) 0.0167(2) Uani 1 1 d . . . H17 H 0.7510 -0.3727 0.6096 0.020 Uiso 1 1 calc R . . C3 C 0.59551(12) 0.19015(10) 0.79605(6) 0.0122(2) Uani 1 1 d . . . C12 C 0.93414(12) 0.06615(11) 0.58259(6) 0.0127(2) Uani 1 1 d . . . H12 H 0.8821 0.0860 0.5470 0.015 Uiso 1 1 calc R . . C50 C 1.09261(19) -0.41438(17) 0.57644(9) 0.0380(4) Uani 1 1 d . . . H50 H 1.1387 -0.3672 0.5322 0.046 Uiso 1 1 calc R . . C34 C 0.34599(14) -0.42246(11) 0.72176(7) 0.0179(2) Uani 1 1 d . . . H34 H 0.2925 -0.4669 0.7004 0.022 Uiso 1 1 calc R . . C38 C 0.32248(12) -0.22082(12) 0.92695(7) 0.0163(2) Uani 1 1 d . . . H38 H 0.2900 -0.1911 0.8851 0.020 Uiso 1 1 calc R . . C18 C 0.71867(13) -0.20721(10) 0.63966(6) 0.0134(2) Uani 1 1 d . . . H18 H 0.7815 -0.2191 0.6704 0.016 Uiso 1 1 calc R . . C49 C 1.07555(19) -0.53945(18) 0.58344(9) 0.0362(4) Uani 1 1 d . . . H49 H 1.1096 -0.5772 0.5439 0.043 Uiso 1 1 calc R . . C2 C 0.73680(12) 0.15604(10) 0.78780(6) 0.01149(19) Uani 1 1 d . . . C30 C 0.76783(12) -0.38972(10) 0.88188(6) 0.0127(2) Uani 1 1 d . . . H30 H 0.6893 -0.4436 0.8974 0.015 Uiso 1 1 calc R . . C22 C 0.47004(15) 0.37627(11) 0.59816(7) 0.0185(2) Uani 1 1 d . . . H22 H 0.4264 0.4506 0.5829 0.022 Uiso 1 1 calc R . . C36 C 0.52676(14) -0.41691(11) 0.78572(7) 0.0170(2) Uani 1 1 d . . . H36 H 0.5967 -0.4578 0.8074 0.020 Uiso 1 1 calc R . . C41 C 0.41493(15) -0.30825(11) 1.04953(7) 0.0183(2) Uani 1 1 d . . . H41 H 0.4468 -0.3389 1.0915 0.022 Uiso 1 1 calc R . . C21 C 0.61445(15) 0.36955(11) 0.58427(7) 0.0185(2) Uani 1 1 d . . . H21 H 0.6695 0.4401 0.5602 0.022 Uiso 1 1 calc R . . C29 C 0.89705(13) -0.43059(11) 0.89378(7) 0.0158(2) Uani 1 1 d . . . H29 H 0.9065 -0.5120 0.9176 0.019 Uiso 1 1 calc R . . C23 C 0.38936(14) 0.27354(11) 0.63462(7) 0.0171(2) Uani 1 1 d . . . H23 H 0.2903 0.2774 0.6443 0.021 Uiso 1 1 calc R . . C9 C 1.08503(12) 0.00342(11) 0.68703(7) 0.0142(2) Uani 1 1 d . . . H9 H 1.1384 -0.0186 0.7219 0.017 Uiso 1 1 calc R . . C15 C 0.53733(14) -0.17294(11) 0.54886(7) 0.0173(2) Uani 1 1 d . . . H15 H 0.4752 -0.1613 0.5178 0.021 Uiso 1 1 calc R . . C39 C 0.22813(14) -0.24036(12) 0.99214(7) 0.0206(3) Uani 1 1 d . . . H39 H 0.1318 -0.2245 0.9946 0.025 Uiso 1 1 calc R . . C45 C 0.10415(15) 0.09413(13) 0.89113(8) 0.0231(3) Uani 1 1 d . . . H45 H 0.0822 0.0160 0.8840 0.028 Uiso 1 1 calc R . . C31 C 0.50284(12) -0.29263(10) 0.78609(6) 0.01076(19) Uani 1 1 d . . . C16 C 0.61073(15) -0.28119(11) 0.55794(7) 0.0180(2) Uani 1 1 d . . . H16 H 0.5989 -0.3432 0.5330 0.022 Uiso 1 1 calc R . . C43 C 0.14036(15) 0.31002(14) 0.84830(8) 0.0257(3) Uani 1 1 d . . . H43 H 0.1441 0.3796 0.8115 0.031 Uiso 1 1 calc R . . C33 C 0.32194(12) -0.29882(11) 0.72117(7) 0.0145(2) Uani 1 1 d . . . H33 H 0.2524 -0.2582 0.6991 0.017 Uiso 1 1 calc R . . C40 C 0.27442(15) -0.28305(12) 1.05376(7) 0.0207(3) Uani 1 1 d . . . H40 H 0.2103 -0.2949 1.0985 0.025 Uiso 1 1 calc R . . C32 C 0.40009(12) -0.23522(10) 0.75306(6) 0.0124(2) Uani 1 1 d . . . H32 H 0.3834 -0.1508 0.7524 0.015 Uiso 1 1 calc R . . C10 C 1.15391(12) 0.04066(12) 0.61630(7) 0.0170(2) Uani 1 1 d . . . H10 H 1.2531 0.0444 0.6038 0.020 Uiso 1 1 calc R . . C20 C 0.67990(13) 0.26002(11) 0.60534(6) 0.0142(2) Uani 1 1 d . . . H20 H 0.7790 0.2563 0.5948 0.017 Uiso 1 1 calc R . . H3 H 0.5717(16) 0.2528(14) 0.7603(8) 0.018(4) Uiso 1 1 d . . . H5 H 0.4692(16) -0.0048(13) 0.9392(8) 0.014(4) Uiso 1 1 d . . . H6 H 0.6977(16) -0.0739(14) 0.9275(8) 0.015(4) Uiso 1 1 d . . . H2 H 0.7986(17) 0.1905(14) 0.7483(9) 0.021(4) Uiso 1 1 d . . . H4 H 0.3975(17) 0.1451(14) 0.8517(8) 0.021(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.00742(7) 0.00727(6) 0.00868(7) -0.00154(5) -0.00149(5) 0.00087(5) P1 0.00783(11) 0.00854(11) 0.00881(12) -0.00122(9) -0.00216(9) 0.00034(9) P2 0.00671(11) 0.00797(11) 0.01029(12) -0.00075(9) -0.00173(9) 0.00017(9) C27 0.0090(4) 0.0129(5) 0.0158(5) -0.0026(4) -0.0040(4) 0.0016(4) C26 0.0084(4) 0.0107(4) 0.0100(4) -0.0026(4) -0.0017(3) 0.0008(3) C44 0.0208(6) 0.0351(8) 0.0223(7) -0.0066(6) -0.0080(5) 0.0009(6) C25 0.0090(4) 0.0094(4) 0.0115(5) -0.0016(4) -0.0025(4) 0.0014(3) C24 0.0124(5) 0.0133(5) 0.0155(5) -0.0014(4) -0.0039(4) 0.0006(4) C5 0.0127(5) 0.0131(5) 0.0111(5) -0.0051(4) -0.0005(4) 0.0004(4) C35 0.0286(7) 0.0123(5) 0.0304(7) -0.0085(5) -0.0125(6) 0.0029(5) C51 0.0179(6) 0.0258(7) 0.0377(9) -0.0001(6) -0.0084(6) 0.0008(5) C48 0.0189(6) 0.0154(5) 0.0373(8) -0.0053(6) -0.0098(6) 0.0037(5) C52 0.0242(7) 0.0292(7) 0.0228(7) -0.0071(6) -0.0108(6) 0.0024(6) C46 0.0139(5) 0.0183(6) 0.0230(6) 0.0017(5) -0.0023(5) -0.0031(4) C19 0.0118(5) 0.0103(4) 0.0098(4) -0.0015(4) -0.0038(4) 0.0012(4) C8 0.0086(4) 0.0092(4) 0.0124(5) -0.0025(4) -0.0018(4) -0.0005(3) C7 0.0088(4) 0.0100(4) 0.0113(5) -0.0020(4) -0.0004(4) -0.0008(3) B1 0.0089(5) 0.0101(5) 0.0117(5) -0.0024(4) -0.0029(4) 0.0006(4) C37 0.0096(4) 0.0094(4) 0.0126(5) -0.0009(4) -0.0004(4) -0.0015(3) C14 0.0158(5) 0.0122(5) 0.0130(5) -0.0003(4) -0.0069(4) -0.0002(4) C28 0.0117(5) 0.0138(5) 0.0196(6) -0.0023(4) -0.0056(4) 0.0044(4) C11 0.0130(5) 0.0199(5) 0.0133(5) -0.0047(4) 0.0024(4) -0.0032(4) C13 0.0108(4) 0.0098(4) 0.0093(4) -0.0015(4) -0.0022(4) -0.0004(3) C42 0.0153(5) 0.0134(5) 0.0141(5) -0.0016(4) -0.0030(4) -0.0020(4) C47 0.0114(5) 0.0244(6) 0.0217(6) -0.0060(5) -0.0041(4) 0.0024(5) C1 0.0100(4) 0.0105(4) 0.0105(4) -0.0037(4) -0.0031(4) -0.0013(3) C54 0.0199(6) 0.0290(7) 0.0316(8) -0.0092(6) -0.0068(6) 0.0017(6) C53 0.0229(7) 0.0293(7) 0.0195(6) -0.0006(6) -0.0057(5) -0.0019(6) C4 0.0123(5) 0.0127(5) 0.0144(5) -0.0053(4) -0.0018(4) 0.0033(4) C6 0.0128(5) 0.0108(4) 0.0108(5) -0.0037(4) -0.0033(4) 0.0011(4) C17 0.0213(6) 0.0122(5) 0.0183(6) -0.0058(4) -0.0059(5) 0.0023(4) C3 0.0151(5) 0.0088(4) 0.0137(5) -0.0033(4) -0.0047(4) 0.0031(4) C12 0.0117(5) 0.0155(5) 0.0104(5) -0.0032(4) -0.0008(4) -0.0011(4) C50 0.0323(9) 0.0398(10) 0.0282(8) 0.0089(7) 0.0073(7) 0.0060(7) C34 0.0185(6) 0.0162(5) 0.0217(6) -0.0073(5) -0.0064(5) -0.0029(4) C38 0.0102(5) 0.0198(6) 0.0172(6) -0.0030(5) -0.0003(4) -0.0001(4) C18 0.0151(5) 0.0124(5) 0.0140(5) -0.0040(4) -0.0052(4) 0.0020(4) C49 0.0345(9) 0.0473(10) 0.0247(8) -0.0113(7) -0.0002(7) 0.0122(8) C2 0.0133(5) 0.0084(4) 0.0132(5) -0.0035(4) -0.0028(4) -0.0002(4) C30 0.0120(5) 0.0098(4) 0.0157(5) 0.0000(4) -0.0038(4) 0.0004(4) C22 0.0271(7) 0.0136(5) 0.0158(6) -0.0035(4) -0.0071(5) 0.0083(5) C36 0.0211(6) 0.0107(5) 0.0218(6) -0.0037(4) -0.0101(5) 0.0030(4) C41 0.0260(6) 0.0151(5) 0.0123(5) -0.0024(4) -0.0007(5) -0.0059(5) C21 0.0246(6) 0.0112(5) 0.0173(6) -0.0004(4) -0.0023(5) 0.0018(4) C29 0.0164(5) 0.0116(5) 0.0189(6) 0.0005(4) -0.0065(4) 0.0034(4) C23 0.0166(5) 0.0166(5) 0.0199(6) -0.0044(5) -0.0078(5) 0.0065(4) C9 0.0089(5) 0.0171(5) 0.0164(5) -0.0027(4) -0.0023(4) -0.0018(4) C15 0.0231(6) 0.0164(5) 0.0148(5) -0.0009(4) -0.0105(5) -0.0036(5) C39 0.0128(5) 0.0220(6) 0.0237(7) -0.0075(5) 0.0054(5) -0.0030(5) C45 0.0189(6) 0.0220(6) 0.0297(7) -0.0084(6) -0.0052(5) -0.0029(5) C31 0.0101(4) 0.0098(4) 0.0121(5) -0.0017(4) -0.0019(4) -0.0007(3) C16 0.0268(7) 0.0142(5) 0.0145(5) -0.0041(4) -0.0059(5) -0.0039(5) C43 0.0218(7) 0.0245(7) 0.0278(7) 0.0069(6) -0.0101(6) 0.0003(5) C33 0.0118(5) 0.0165(5) 0.0159(5) -0.0033(4) -0.0043(4) -0.0004(4) C40 0.0235(6) 0.0179(6) 0.0169(6) -0.0073(5) 0.0078(5) -0.0090(5) C32 0.0106(5) 0.0115(4) 0.0151(5) -0.0031(4) -0.0029(4) 0.0009(4) C10 0.0080(5) 0.0228(6) 0.0184(6) -0.0057(5) 0.0020(4) -0.0018(4) C20 0.0151(5) 0.0119(5) 0.0141(5) -0.0006(4) -0.0023(4) 0.0009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 1.9667(11) . ? Fe1 C6 2.0838(12) . ? Fe1 C2 2.0962(12) . ? Fe1 C5 2.1676(11) . ? Fe1 C3 2.1705(12) . ? Fe1 P1 2.1827(5) . ? Fe1 P2 2.1840(6) . ? Fe1 C4 2.1934(11) . ? Fe1 B1 2.2668(13) . ? P1 C7 1.8368(12) . ? P1 C19 1.8408(12) . ? P1 C13 1.8417(11) . ? P2 C31 1.8354(12) . ? P2 C25 1.8441(11) . ? P2 C37 1.8533(12) . ? C27 C28 1.3916(16) . ? C27 C26 1.4071(15) . ? C27 H27 0.9500 . ? C26 C25 1.4181(16) . ? C26 B1 1.5999(17) . ? C44 C45 1.385(2) . ? C44 C43 1.391(2) . ? C44 H44 0.9500 . ? C25 C30 1.4096(16) . ? C24 C23 1.3888(16) . ? C24 C19 1.4037(16) . ? C24 H24 0.9500 . ? C5 C4 1.4106(17) . ? C5 C6 1.4171(16) . ? C5 H5 0.907(15) . ? C35 C34 1.3854(19) . ? C35 C36 1.3898(19) . ? C35 H35 0.9500 . ? C51 C50 1.382(2) . ? C51 C52 1.384(2) . ? C51 H51 0.9500 . ? C48 C47 1.384(2) . ? C48 C43 1.387(2) . ? C48 H48 0.9500 . ? C52 C53 1.384(2) . ? C52 H52 0.9500 . ? C46 C47 1.3844(19) . ? C46 C45 1.391(2) . ? C46 H46 0.9500 . ? C19 C20 1.3996(17) . ? C8 C7 1.4087(16) . ? C8 C9 1.4108(16) . ? C8 B1 1.6070(17) . ? C7 C12 1.4037(16) . ? B1 C1 1.5625(16) . ? C37 C42 1.3904(17) . ? C37 C38 1.4024(16) . ? C14 C13 1.3933(16) . ? C14 C15 1.3944(17) . ? C14 H14 0.9500 . ? C28 C29 1.3909(18) . ? C28 H28 0.9500 . ? C11 C10 1.3874(19) . ? C11 C12 1.3893(17) . ? C11 H11 0.9500 . ? C13 C18 1.4013(16) . ? C42 C41 1.3951(17) . ? C42 H42 0.9500 . ? C47 H47 0.9500 . ? C1 C6 1.4403(16) . ? C1 C2 1.4513(16) . ? C1 C4 2.9169(17) . ? C54 C49 1.375(2) . ? C54 C53 1.394(2) . ? C54 H54 0.9500 . ? C53 H53 0.9500 . ? C4 C3 1.4074(17) . ? C4 H4 0.925(17) . ? C6 H6 1.005(15) . ? C17 C16 1.3838(19) . ? C17 C18 1.3948(16) . ? C17 H17 0.9500 . ? C3 C2 1.4102(17) . ? C3 H3 0.956(16) . ? C12 H12 0.9500 . ? C50 C49 1.388(3) . ? C50 H50 0.9500 . ? C34 C33 1.3915(17) . ? C34 H34 0.9500 . ? C38 C39 1.3876(17) . ? C38 H38 0.9500 . ? C18 H18 0.9500 . ? C49 H49 0.9500 . ? C2 H2 0.899(17) . ? C30 C29 1.3911(17) . ? C30 H30 0.9500 . ? C22 C21 1.3857(19) . ? C22 C23 1.3919(19) . ? C22 H22 0.9500 . ? C36 C31 1.4012(16) . ? C36 H36 0.9500 . ? C41 C40 1.388(2) . ? C41 H41 0.9500 . ? C21 C20 1.3982(17) . ? C21 H21 0.9500 . ? C29 H29 0.9500 . ? C23 H23 0.9500 . ? C9 C10 1.3943(17) . ? C9 H9 0.9500 . ? C15 C16 1.3900(18) . ? C15 H15 0.9500 . ? C39 C40 1.389(2) . ? C39 H39 0.9500 . ? C45 H45 0.9500 . ? C31 C32 1.3978(16) . ? C16 H16 0.9500 . ? C43 H43 0.9500 . ? C33 C32 1.3875(17) . ? C33 H33 0.9500 . ? C40 H40 0.9500 . ? C32 H32 0.9500 . ? C10 H10 0.9500 . ? C20 H20 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 C1 Fe1 C6 41.53(5) . . ? C1 Fe1 C2 41.71(5) . . ? C6 Fe1 C2 70.88(5) . . ? C1 Fe1 C5 74.12(5) . . ? C6 Fe1 C5 38.88(4) . . ? C2 Fe1 C5 81.92(5) . . ? C1 Fe1 C3 74.18(5) . . ? C6 Fe1 C3 82.29(4) . . ? C2 Fe1 C3 38.55(5) . . ? C5 Fe1 C3 67.34(5) . . ? C1 Fe1 P1 111.01(4) . . ? C6 Fe1 P1 152.23(3) . . ? C2 Fe1 P1 89.47(3) . . ? C5 Fe1 P1 159.67(3) . . ? C3 Fe1 P1 94.58(3) . . ? C1 Fe1 P2 110.90(4) . . ? C6 Fe1 P2 88.91(3) . . ? C2 Fe1 P2 152.40(4) . . ? C5 Fe1 P2 94.16(4) . . ? C3 Fe1 P2 159.26(3) . . ? P1 Fe1 P2 101.757(15) . . ? C1 Fe1 C4 88.87(5) . . ? C6 Fe1 C4 70.45(5) . . ? C2 Fe1 C4 69.97(5) . . ? C5 Fe1 C4 37.74(5) . . ? C3 Fe1 C4 37.63(5) . . ? P1 Fe1 C4 121.94(4) . . ? P2 Fe1 C4 121.64(4) . . ? C1 Fe1 B1 42.58(4) . . ? C6 Fe1 B1 71.29(5) . . ? C2 Fe1 B1 70.00(5) . . ? C5 Fe1 B1 110.07(5) . . ? C3 Fe1 B1 108.53(5) . . ? P1 Fe1 B1 83.80(3) . . ? P2 Fe1 B1 86.07(3) . . ? C4 Fe1 B1 131.42(5) . . ? C7 P1 C19 106.36(5) . . ? C7 P1 C13 99.04(5) . . ? C19 P1 C13 103.69(5) . . ? C7 P1 Fe1 107.29(4) . . ? C19 P1 Fe1 110.36(4) . . ? C13 P1 Fe1 128.02(4) . . ? C31 P2 C25 109.88(5) . . ? C31 P2 C37 97.93(5) . . ? C25 P2 C37 103.74(5) . . ? C31 P2 Fe1 122.91(4) . . ? C25 P2 Fe1 106.81(4) . . ? C37 P2 Fe1 113.95(4) . . ? C28 C27 C26 122.09(11) . . ? C28 C27 H27 119.0 . . ? C26 C27 H27 119.0 . . ? C27 C26 C25 117.27(10) . . ? C27 C26 B1 121.51(10) . . ? C25 C26 B1 121.22(10) . . ? C45 C44 C43 119.85(14) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C30 C25 C26 120.38(10) . . ? C30 C25 P2 124.55(9) . . ? C26 C25 P2 114.82(8) . . ? C23 C24 C19 121.45(11) . . ? C23 C24 H24 119.3 . . ? C19 C24 H24 119.3 . . ? C4 C5 C6 121.63(11) . . ? C4 C5 Fe1 72.12(7) . . ? C6 C5 Fe1 67.37(6) . . ? C4 C5 H5 120.1(10) . . ? C6 C5 H5 118.0(10) . . ? Fe1 C5 H5 130.5(9) . . ? C34 C35 C36 120.91(12) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C50 C51 C52 119.26(15) . . ? C50 C51 H51 120.4 . . ? C52 C51 H51 120.4 . . ? C47 C48 C43 119.77(13) . . ? C47 C48 H48 120.1 . . ? C43 C48 H48 120.1 . . ? C53 C52 C51 120.35(14) . . ? C53 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C47 C46 C45 119.88(13) . . ? C47 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C20 C19 C24 118.07(10) . . ? C20 C19 P1 124.07(9) . . ? C24 C19 P1 117.16(9) . . ? C7 C8 C9 116.81(10) . . ? C7 C8 B1 119.09(10) . . ? C9 C8 B1 124.08(10) . . ? C12 C7 C8 121.49(10) . . ? C12 C7 P1 123.60(9) . . ? C8 C7 P1 114.81(8) . . ? C1 B1 C26 121.37(10) . . ? C1 B1 C8 119.56(10) . . ? C26 B1 C8 117.97(9) . . ? C1 B1 Fe1 58.40(6) . . ? C26 B1 Fe1 109.47(8) . . ? C8 B1 Fe1 110.78(8) . . ? C42 C37 C38 118.33(11) . . ? C42 C37 P2 123.77(9) . . ? C38 C37 P2 117.66(9) . . ? C13 C14 C15 120.25(11) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C29 C28 C27 119.93(11) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C10 C11 C12 119.27(11) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C14 C13 C18 118.98(10) . . ? C14 C13 P1 124.48(8) . . ? C18 C13 P1 116.54(9) . . ? C37 C42 C41 120.79(12) . . ? C37 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C48 C47 C46 120.35(13) . . ? C48 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C6 C1 C2 113.91(10) . . ? C6 C1 B1 115.46(10) . . ? C2 C1 B1 112.48(10) . . ? C6 C1 Fe1 73.60(7) . . ? C2 C1 Fe1 73.93(7) . . ? B1 C1 Fe1 79.02(7) . . ? C6 C1 C4 57.71(6) . . ? C2 C1 C4 57.42(6) . . ? B1 C1 C4 127.73(8) . . ? Fe1 C1 C4 48.75(3) . . ? C49 C54 C53 119.25(15) . . ? C49 C54 H54 120.4 . . ? C53 C54 H54 120.4 . . ? C52 C53 C54 120.22(14) . . ? C52 C53 H53 119.9 . . ? C54 C53 H53 119.9 . . ? C3 C4 C5 117.17(11) . . ? C3 C4 Fe1 70.30(6) . . ? C5 C4 Fe1 70.14(6) . . ? C3 C4 C1 58.93(7) . . ? C5 C4 C1 58.78(7) . . ? Fe1 C4 C1 42.38(3) . . ? C3 C4 H4 119.5(10) . . ? C5 C4 H4 123.2(10) . . ? Fe1 C4 H4 127.7(10) . . ? C1 C4 H4 170.0(10) . . ? C5 C6 C1 121.79(11) . . ? C5 C6 Fe1 73.76(7) . . ? C1 C6 Fe1 64.87(6) . . ? C5 C6 H6 118.7(9) . . ? C1 C6 H6 118.1(9) . . ? Fe1 C6 H6 124.1(9) . . ? C16 C17 C18 119.93(11) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C4 C3 C2 121.69(11) . . ? C4 C3 Fe1 72.07(7) . . ? C2 C3 Fe1 67.88(6) . . ? C4 C3 H3 120.4(10) . . ? C2 C3 H3 117.7(10) . . ? Fe1 C3 H3 129.9(9) . . ? C11 C12 C7 120.24(11) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? C51 C50 C49 120.48(16) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C35 C34 C33 119.60(12) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C39 C38 C37 120.98(12) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C17 C18 C13 120.54(11) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? C54 C49 C50 120.44(15) . . ? C54 C49 H49 119.8 . . ? C50 C49 H49 119.8 . . ? C3 C2 C1 121.79(11) . . ? C3 C2 Fe1 73.57(7) . . ? C1 C2 Fe1 64.36(6) . . ? C3 C2 H2 118.8(10) . . ? C1 C2 H2 117.9(10) . . ? Fe1 C2 H2 124.5(10) . . ? C29 C30 C25 120.50(11) . . ? C29 C30 H30 119.8 . . ? C25 C30 H30 119.8 . . ? C21 C22 C23 119.64(11) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C35 C36 C31 120.11(12) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? C40 C41 C42 120.22(13) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C22 C21 C20 120.67(12) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C28 C29 C30 119.79(11) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C24 C23 C22 119.78(12) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C10 C9 C8 121.46(11) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C16 C15 C14 120.29(12) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C38 C39 C40 120.07(13) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C44 C45 C46 119.96(13) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C32 C31 C36 118.30(11) . . ? C32 C31 P2 116.43(8) . . ? C36 C31 P2 125.03(9) . . ? C17 C16 C15 120.01(11) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C48 C43 C44 120.15(14) . . ? C48 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C32 C33 C34 119.61(12) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C41 C40 C39 119.60(12) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C33 C32 C31 121.47(11) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C11 C10 C9 120.72(11) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C21 C20 C19 120.36(12) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.331 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.112