# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'John C. Gordon' _publ_contact_author_email jgordon@lanl.gov loop_ _publ_author_name T.K.Mukhopadhyay R.K.Feller F.N.Rein N.J.Henson N.C.Smythe ; R.J.Trovitch ; J.C.Gordon # Attachment '- apx1342_0m.cif' data_apx1342_0m _database_code_depnum_ccdc_archive 'CCDC 884463' #TrackingRef '- apx1342_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H41 Fe N2 P3' _chemical_formula_weight 746.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 14.8559(19) _cell_length_b 14.3443(18) _cell_length_c 18.850(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.0300(10) _cell_angle_gamma 90.00 _cell_volume 3797.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 5624 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.77 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8078 _exptl_absorpt_correction_T_max 0.9464 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41383 _diffrn_reflns_av_R_equivalents 0.0735 _diffrn_reflns_av_sigmaI/netI 0.0662 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.68 _reflns_number_total 8717 _reflns_number_gt 6196 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+1.8442P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8717 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.39756(3) 0.05794(2) 0.23096(2) 0.01241(10) Uani 1 1 d . . . P1 P 0.39689(5) 0.18991(5) 0.17529(4) 0.01417(15) Uani 1 1 d . . . P2 P 0.35532(5) 0.13902(5) 0.31145(4) 0.01355(15) Uani 1 1 d . . . P3 P 0.52598(5) 0.02612(5) 0.32670(4) 0.01464(15) Uani 1 1 d . . . N1 N 0.43394(15) -0.01657(15) 0.15775(12) 0.0160(5) Uani 1 1 d . . . N2 N 0.27535(15) 0.00223(14) 0.17802(11) 0.0138(4) Uani 1 1 d . . . C1 C 0.5217(2) -0.0228(2) 0.15001(16) 0.0233(6) Uani 1 1 d . . . H1 H 0.5729 0.0094 0.1852 0.028 Uiso 1 1 calc R . . C2 C 0.5404(2) -0.0723(2) 0.09493(18) 0.0310(7) Uani 1 1 d . . . H2 H 0.6032 -0.0740 0.0923 0.037 Uiso 1 1 calc R . . C3 C 0.4661(2) -0.1211(2) 0.04167(18) 0.0312(7) Uani 1 1 d . . . H3 H 0.4779 -0.1568 0.0032 0.037 Uiso 1 1 calc R . . C4 C 0.3775(2) -0.11550(19) 0.04706(16) 0.0232(6) Uani 1 1 d . . . H4 H 0.3262 -0.1472 0.0116 0.028 Uiso 1 1 calc R . . C5 C 0.36096(19) -0.06309(18) 0.10479(15) 0.0173(5) Uani 1 1 d . . . C6 C 0.27072(19) -0.04927(17) 0.11391(14) 0.0147(5) Uani 1 1 d . . . C7 C 0.1842(2) -0.07794(18) 0.06188(15) 0.0198(6) Uani 1 1 d . . . H7 H 0.1844 -0.1109 0.0182 0.024 Uiso 1 1 calc R . . C8 C 0.09940(19) -0.05938(19) 0.07270(15) 0.0216(6) Uani 1 1 d . . . H8 H 0.0406 -0.0784 0.0373 0.026 Uiso 1 1 calc R . . C9 C 0.10258(19) -0.01095(19) 0.13845(15) 0.0198(6) Uani 1 1 d . . . H9 H 0.0455 0.0014 0.1491 0.024 Uiso 1 1 calc R . . C10 C 0.18811(18) 0.01813(18) 0.18684(15) 0.0167(6) Uani 1 1 d . . . H10 H 0.1874 0.0520 0.2300 0.020 Uiso 1 1 calc R . . C11 C 0.49010(19) 0.24026(18) 0.14300(14) 0.0165(5) Uani 1 1 d . . . C12 C 0.5847(2) 0.2149(2) 0.17773(17) 0.0275(7) Uani 1 1 d . . . H12 H 0.6003 0.1716 0.2181 0.033 Uiso 1 1 calc R . . C13 C 0.6572(2) 0.2520(2) 0.15424(18) 0.0319(7) Uani 1 1 d . . . H13 H 0.7213 0.2335 0.1783 0.038 Uiso 1 1 calc R . . C14 C 0.6359(2) 0.3152(2) 0.09632(17) 0.0275(7) Uani 1 1 d . . . H14 H 0.6851 0.3404 0.0802 0.033 Uiso 1 1 calc R . . C15 C 0.5422(2) 0.3419(2) 0.06157(16) 0.0243(6) Uani 1 1 d . . . H15 H 0.5275 0.3864 0.0221 0.029 Uiso 1 1 calc R . . C16 C 0.4696(2) 0.30427(18) 0.08385(16) 0.0196(6) Uani 1 1 d . . . H16 H 0.4055 0.3221 0.0587 0.024 Uiso 1 1 calc R . . C17 C 0.29807(19) 0.18391(17) 0.08662(14) 0.0155(5) Uani 1 1 d . . . C18 C 0.31051(19) 0.13360(18) 0.02665(15) 0.0184(6) Uani 1 1 d . . . H18 H 0.3722 0.1121 0.0298 0.022 Uiso 1 1 calc R . . C19 C 0.2342(2) 0.1150(2) -0.03683(15) 0.0217(6) Uani 1 1 d . . . H19 H 0.2438 0.0811 -0.0770 0.026 Uiso 1 1 calc R . . C20 C 0.1440(2) 0.1453(2) -0.04238(16) 0.0237(6) Uani 1 1 d . . . H20 H 0.0916 0.1320 -0.0861 0.028 Uiso 1 1 calc R . . C21 C 0.1304(2) 0.1953(2) 0.01640(16) 0.0226(6) Uani 1 1 d . . . H21 H 0.0684 0.2162 0.0128 0.027 Uiso 1 1 calc R . . C22 C 0.20665(19) 0.21490(18) 0.08015(15) 0.0187(6) Uani 1 1 d . . . H22 H 0.1967 0.2497 0.1198 0.022 Uiso 1 1 calc R . . C23 C 0.36789(19) 0.28939(18) 0.22675(15) 0.0176(6) Uani 1 1 d . . . H23A H 0.4275 0.3189 0.2589 0.021 Uiso 1 1 calc R . . H23B H 0.3311 0.3366 0.1905 0.021 Uiso 1 1 calc R . . C24 C 0.30946(19) 0.25569(18) 0.27544(15) 0.0173(6) Uani 1 1 d . . . H24A H 0.2412 0.2519 0.2452 0.021 Uiso 1 1 calc R . . H24B H 0.3167 0.2994 0.3176 0.021 Uiso 1 1 calc R . . C25 C 0.27351(18) 0.09926(18) 0.36048(14) 0.0162(5) Uani 1 1 d . . . C26 C 0.20678(19) 0.1571(2) 0.37597(15) 0.0208(6) Uani 1 1 d . . . H26 H 0.2002 0.2200 0.3593 0.025 Uiso 1 1 calc R . . C27 C 0.1499(2) 0.1228(2) 0.41572(16) 0.0251(6) Uani 1 1 d . . . H27 H 0.1034 0.1620 0.4249 0.030 Uiso 1 1 calc R . . C28 C 0.1604(2) 0.0318(2) 0.44209(17) 0.0259(7) Uani 1 1 d . . . H28 H 0.1224 0.0094 0.4704 0.031 Uiso 1 1 calc R . . C29 C 0.2268(2) -0.0262(2) 0.42699(15) 0.0207(6) Uani 1 1 d . . . H29 H 0.2345 -0.0884 0.4452 0.025 Uiso 1 1 calc R . . C30 C 0.28162(19) 0.00658(18) 0.38536(15) 0.0183(6) Uani 1 1 d . . . H30 H 0.3252 -0.0341 0.3736 0.022 Uiso 1 1 calc R . . C31 C 0.45902(18) 0.16772(18) 0.39376(14) 0.0168(6) Uani 1 1 d . . . H31A H 0.4968 0.2183 0.3814 0.020 Uiso 1 1 calc R . . H31B H 0.4381 0.1885 0.4360 0.020 Uiso 1 1 calc R . . C32 C 0.51830(19) 0.07891(18) 0.41479(14) 0.0183(6) Uani 1 1 d . . . H32A H 0.4879 0.0347 0.4404 0.022 Uiso 1 1 calc R . . H32B H 0.5828 0.0938 0.4492 0.022 Uiso 1 1 calc R . . C33 C 0.54027(19) -0.09863(19) 0.35129(15) 0.0177(6) Uani 1 1 d . . . C34 C 0.4792(2) -0.16411(19) 0.30583(16) 0.0234(6) Uani 1 1 d . . . H34 H 0.4304 -0.1442 0.2618 0.028 Uiso 1 1 calc R . . C35 C 0.4886(2) -0.2583(2) 0.32400(17) 0.0285(7) Uani 1 1 d . . . H35 H 0.4469 -0.3024 0.2921 0.034 Uiso 1 1 calc R . . C36 C 0.5584(2) -0.2878(2) 0.38830(17) 0.0272(7) Uani 1 1 d . . . H36 H 0.5647 -0.3522 0.4009 0.033 Uiso 1 1 calc R . . C37 C 0.6195(2) -0.22312(19) 0.43462(16) 0.0232(6) Uani 1 1 d . . . H37 H 0.6675 -0.2434 0.4789 0.028 Uiso 1 1 calc R . . C38 C 0.61072(19) -0.12958(18) 0.41657(15) 0.0192(6) Uani 1 1 d . . . H38 H 0.6527 -0.0858 0.4486 0.023 Uiso 1 1 calc R . . C39 C 0.65173(19) 0.05373(18) 0.33669(15) 0.0179(6) Uani 1 1 d . . . C40 C 0.7085(2) -0.0062(2) 0.31143(17) 0.0247(6) Uani 1 1 d . . . H40 H 0.6845 -0.0657 0.2921 0.030 Uiso 1 1 calc R . . C41 C 0.8000(2) 0.0198(2) 0.31414(19) 0.0338(8) Uani 1 1 d . . . H41 H 0.8373 -0.0218 0.2960 0.041 Uiso 1 1 calc R . . C42 C 0.8367(2) 0.1050(2) 0.3427(2) 0.0374(8) Uani 1 1 d . . . H42 H 0.8986 0.1228 0.3436 0.045 Uiso 1 1 calc R . . C43 C 0.7827(2) 0.1646(2) 0.37023(18) 0.0318(7) Uani 1 1 d . . . H43 H 0.8084 0.2226 0.3918 0.038 Uiso 1 1 calc R . . C44 C 0.6906(2) 0.1397(2) 0.36637(15) 0.0224(6) Uani 1 1 d . . . H44 H 0.6535 0.1818 0.3842 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01376(19) 0.01241(19) 0.01098(19) -0.00070(14) 0.00392(14) 0.00003(14) P1 0.0163(3) 0.0137(3) 0.0129(3) 0.0003(3) 0.0053(3) -0.0005(3) P2 0.0154(3) 0.0134(3) 0.0120(3) -0.0008(3) 0.0047(3) -0.0002(3) P3 0.0160(3) 0.0135(3) 0.0135(3) 0.0011(3) 0.0036(3) 0.0002(3) N1 0.0157(11) 0.0168(11) 0.0146(11) -0.0001(9) 0.0038(9) 0.0006(9) N2 0.0170(11) 0.0138(11) 0.0117(11) 0.0001(8) 0.0061(9) 0.0000(9) C1 0.0202(15) 0.0307(16) 0.0200(15) -0.0054(12) 0.0078(12) -0.0009(12) C2 0.0221(16) 0.045(2) 0.0302(17) -0.0082(15) 0.0141(13) 0.0007(14) C3 0.0382(19) 0.0301(17) 0.0320(18) -0.0142(14) 0.0206(15) -0.0003(14) C4 0.0308(17) 0.0198(14) 0.0225(15) -0.0053(12) 0.0137(13) -0.0032(12) C5 0.0221(14) 0.0138(13) 0.0164(13) -0.0001(11) 0.0070(11) 0.0018(11) C6 0.0205(14) 0.0106(12) 0.0136(13) -0.0006(10) 0.0064(11) -0.0009(10) C7 0.0267(15) 0.0165(13) 0.0146(13) -0.0027(11) 0.0044(11) -0.0053(11) C8 0.0164(14) 0.0213(14) 0.0216(14) -0.0021(12) -0.0012(11) -0.0053(11) C9 0.0161(14) 0.0198(14) 0.0223(15) 0.0019(11) 0.0045(11) 0.0003(11) C10 0.0176(14) 0.0142(13) 0.0190(14) -0.0014(11) 0.0068(11) 0.0009(10) C11 0.0204(14) 0.0142(13) 0.0159(13) -0.0006(10) 0.0071(11) -0.0019(11) C12 0.0253(16) 0.0319(17) 0.0238(16) 0.0089(13) 0.0058(13) -0.0030(13) C13 0.0193(16) 0.0408(19) 0.0339(18) 0.0071(15) 0.0063(14) -0.0033(14) C14 0.0262(16) 0.0285(16) 0.0321(17) -0.0008(13) 0.0155(14) -0.0089(13) C15 0.0308(17) 0.0204(15) 0.0254(16) 0.0025(12) 0.0145(13) -0.0003(12) C16 0.0212(14) 0.0165(13) 0.0235(15) -0.0005(11) 0.0107(12) -0.0002(11) C17 0.0182(13) 0.0118(12) 0.0154(13) 0.0032(10) 0.0042(11) -0.0021(10) C18 0.0183(14) 0.0187(14) 0.0182(14) 0.0023(11) 0.0062(11) 0.0008(11) C19 0.0255(15) 0.0228(15) 0.0167(14) -0.0005(12) 0.0067(12) -0.0019(12) C20 0.0223(15) 0.0258(15) 0.0189(14) 0.0053(12) 0.0011(12) -0.0034(12) C21 0.0190(15) 0.0246(15) 0.0235(15) 0.0050(12) 0.0059(12) 0.0025(12) C22 0.0213(14) 0.0172(14) 0.0183(14) 0.0024(11) 0.0073(11) 0.0013(11) C23 0.0223(14) 0.0143(13) 0.0169(13) 0.0003(10) 0.0074(11) 0.0004(11) C24 0.0228(14) 0.0147(13) 0.0154(13) -0.0005(10) 0.0074(11) 0.0009(11) C25 0.0169(13) 0.0193(13) 0.0123(13) -0.0028(10) 0.0045(10) -0.0023(11) C26 0.0211(14) 0.0200(14) 0.0221(15) -0.0047(12) 0.0082(12) 0.0008(11) C27 0.0260(16) 0.0263(16) 0.0277(16) -0.0061(13) 0.0154(13) -0.0004(12) C28 0.0316(17) 0.0237(15) 0.0301(17) -0.0037(13) 0.0205(14) -0.0062(13) C29 0.0251(15) 0.0189(14) 0.0193(14) -0.0029(11) 0.0088(12) -0.0078(12) C30 0.0181(14) 0.0175(13) 0.0194(14) -0.0024(11) 0.0062(11) -0.0020(11) C31 0.0165(13) 0.0189(14) 0.0144(13) -0.0038(11) 0.0040(11) -0.0035(11) C32 0.0202(14) 0.0209(14) 0.0122(13) -0.0009(11) 0.0032(11) -0.0026(11) C33 0.0194(14) 0.0178(13) 0.0157(13) 0.0015(11) 0.0054(11) -0.0010(11) C34 0.0234(15) 0.0200(14) 0.0218(15) 0.0053(12) 0.0006(12) -0.0023(12) C35 0.0339(17) 0.0179(15) 0.0284(17) 0.0010(12) 0.0029(14) -0.0068(13) C36 0.0341(18) 0.0179(15) 0.0264(16) 0.0052(12) 0.0054(14) -0.0001(13) C37 0.0273(16) 0.0212(15) 0.0185(14) 0.0025(12) 0.0039(12) 0.0023(12) C38 0.0203(14) 0.0163(13) 0.0180(14) 0.0018(11) 0.0019(11) -0.0004(11) C39 0.0191(14) 0.0164(13) 0.0168(13) 0.0043(11) 0.0042(11) 0.0023(11) C40 0.0226(15) 0.0220(15) 0.0306(17) 0.0021(12) 0.0103(13) 0.0034(12) C41 0.0223(16) 0.0381(19) 0.043(2) 0.0013(16) 0.0136(15) 0.0059(14) C42 0.0181(16) 0.045(2) 0.050(2) 0.0028(17) 0.0122(15) -0.0046(14) C43 0.0241(16) 0.0312(17) 0.0369(19) -0.0045(14) 0.0057(14) -0.0092(13) C44 0.0201(15) 0.0221(15) 0.0229(15) -0.0008(12) 0.0042(12) -0.0013(12) _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 N2 1.936(2) . ? Fe1 N1 1.956(2) . ? Fe1 P2 2.1608(8) . ? Fe1 P1 2.1628(8) . ? Fe1 P3 2.2045(8) . ? P1 C17 1.832(3) . ? P1 C11 1.833(3) . ? P1 C23 1.853(3) . ? P2 C25 1.841(3) . ? P2 C31 1.842(3) . ? P2 C24 1.850(3) . ? P3 C33 1.843(3) . ? P3 C39 1.858(3) . ? P3 C32 1.862(3) . ? N1 C1 1.361(3) . ? N1 C5 1.383(3) . ? N2 C10 1.378(3) . ? N2 C6 1.399(3) . ? C1 C2 1.360(4) . ? C1 H1 0.9500 . ? C2 C3 1.412(4) . ? C2 H2 0.9500 . ? C3 C4 1.355(4) . ? C3 H3 0.9500 . ? C4 C5 1.409(4) . ? C4 H4 0.9500 . ? C5 C6 1.420(4) . ? C6 C7 1.401(4) . ? C7 C8 1.366(4) . ? C7 H7 0.9500 . ? C8 C9 1.408(4) . ? C8 H8 0.9500 . ? C9 C10 1.366(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.392(4) . ? C11 C16 1.399(4) . ? C12 C13 1.396(4) . ? C12 H12 0.9500 . ? C13 C14 1.374(4) . ? C13 H13 0.9500 . ? C14 C15 1.385(4) . ? C14 H14 0.9500 . ? C15 C16 1.388(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.396(4) . ? C17 C18 1.403(4) . ? C18 C19 1.379(4) . ? C18 H18 0.9500 . ? C19 C20 1.379(4) . ? C19 H19 0.9500 . ? C20 C21 1.389(4) . ? C20 H20 0.9500 . ? C21 C22 1.385(4) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.533(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.394(4) . ? C25 C30 1.402(4) . ? C26 C27 1.389(4) . ? C26 H26 0.9500 . ? C27 C28 1.386(4) . ? C27 H27 0.9500 . ? C28 C29 1.389(4) . ? C28 H28 0.9500 . ? C29 C30 1.385(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.526(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.390(4) . ? C33 C38 1.403(4) . ? C34 C35 1.390(4) . ? C34 H34 0.9500 . ? C35 C36 1.380(4) . ? C35 H35 0.9500 . ? C36 C37 1.389(4) . ? C36 H36 0.9500 . ? C37 C38 1.380(4) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.392(4) . ? C39 C44 1.398(4) . ? C40 C41 1.394(4) . ? C40 H40 0.9500 . ? C41 C42 1.375(5) . ? C41 H41 0.9500 . ? C42 C43 1.383(5) . ? C42 H42 0.9500 . ? C43 C44 1.393(4) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N1 80.75(9) . . ? N2 Fe1 P2 98.38(7) . . ? N1 Fe1 P2 179.09(7) . . ? N2 Fe1 P1 104.83(7) . . ? N1 Fe1 P1 95.43(7) . . ? P2 Fe1 P1 85.02(3) . . ? N2 Fe1 P3 138.77(7) . . ? N1 Fe1 P3 95.74(7) . . ? P2 Fe1 P3 84.75(3) . . ? P1 Fe1 P3 116.38(3) . . ? C17 P1 C11 100.54(12) . . ? C17 P1 C23 105.06(12) . . ? C11 P1 C23 101.54(12) . . ? C17 P1 Fe1 106.09(8) . . ? C11 P1 Fe1 128.43(9) . . ? C23 P1 Fe1 112.65(9) . . ? C25 P2 C31 98.86(12) . . ? C25 P2 C24 103.88(12) . . ? C31 P2 C24 102.33(12) . . ? C25 P2 Fe1 125.19(9) . . ? C31 P2 Fe1 110.93(9) . . ? C24 P2 Fe1 112.68(9) . . ? C33 P3 C39 98.74(12) . . ? C33 P3 C32 101.90(12) . . ? C39 P3 C32 100.07(12) . . ? C33 P3 Fe1 113.88(9) . . ? C39 P3 Fe1 127.72(9) . . ? C32 P3 Fe1 110.95(9) . . ? C1 N1 C5 116.4(2) . . ? C1 N1 Fe1 127.30(18) . . ? C5 N1 Fe1 116.18(17) . . ? C10 N2 C6 114.1(2) . . ? C10 N2 Fe1 129.06(17) . . ? C6 N2 Fe1 115.90(17) . . ? C2 C1 N1 123.9(3) . . ? C2 C1 H1 118.1 . . ? N1 C1 H1 118.1 . . ? C1 C2 C3 119.6(3) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C3 C2 118.1(3) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? C3 C4 C5 120.5(3) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? N1 C5 C4 121.5(2) . . ? N1 C5 C6 113.2(2) . . ? C4 C5 C6 125.3(3) . . ? N2 C6 C7 122.4(2) . . ? N2 C6 C5 113.3(2) . . ? C7 C6 C5 124.2(2) . . ? C8 C7 C6 121.2(2) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C7 C8 C9 117.4(2) . . ? C7 C8 H8 121.3 . . ? C9 C8 H8 121.3 . . ? C10 C9 C8 119.7(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 N2 125.1(2) . . ? C9 C10 H10 117.4 . . ? N2 C10 H10 117.4 . . ? C12 C11 C16 118.1(2) . . ? C12 C11 P1 119.8(2) . . ? C16 C11 P1 122.1(2) . . ? C11 C12 C13 121.1(3) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C14 C13 C12 120.1(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 119.6(3) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 C16 120.6(3) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C11 120.5(3) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? C22 C17 C18 118.2(2) . . ? C22 C17 P1 122.1(2) . . ? C18 C17 P1 118.8(2) . . ? C19 C18 C17 120.7(3) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C20 C19 C18 120.5(3) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 119.5(3) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 120.4(3) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C17 120.5(3) . . ? C21 C22 H22 119.7 . . ? C17 C22 H22 119.7 . . ? C24 C23 P1 110.13(17) . . ? C24 C23 H23A 109.6 . . ? P1 C23 H23A 109.6 . . ? C24 C23 H23B 109.6 . . ? P1 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? C23 C24 P2 107.00(18) . . ? C23 C24 H24A 110.3 . . ? P2 C24 H24A 110.3 . . ? C23 C24 H24B 110.3 . . ? P2 C24 H24B 110.3 . . ? H24A C24 H24B 108.6 . . ? C26 C25 C30 118.9(2) . . ? C26 C25 P2 123.5(2) . . ? C30 C25 P2 117.6(2) . . ? C27 C26 C25 120.1(3) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C26 120.6(3) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 119.7(3) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C30 C29 C28 120.0(3) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C25 120.6(3) . . ? C29 C30 H30 119.7 . . ? C25 C30 H30 119.7 . . ? C32 C31 P2 106.59(17) . . ? C32 C31 H31A 110.4 . . ? P2 C31 H31A 110.4 . . ? C32 C31 H31B 110.4 . . ? P2 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? C31 C32 P3 107.82(17) . . ? C31 C32 H32A 110.1 . . ? P3 C32 H32A 110.1 . . ? C31 C32 H32B 110.1 . . ? P3 C32 H32B 110.1 . . ? H32A C32 H32B 108.5 . . ? C34 C33 C38 118.5(2) . . ? C34 C33 P3 120.2(2) . . ? C38 C33 P3 121.3(2) . . ? C35 C34 C33 120.8(3) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C36 C35 C34 120.1(3) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 119.8(3) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C38 C37 C36 120.3(3) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C37 C38 C33 120.5(3) . . ? C37 C38 H38 119.8 . . ? C33 C38 H38 119.8 . . ? C40 C39 C44 117.7(3) . . ? C40 C39 P3 122.3(2) . . ? C44 C39 P3 119.9(2) . . ? C39 C40 C41 120.9(3) . . ? C39 C40 H40 119.5 . . ? C41 C40 H40 119.5 . . ? C42 C41 C40 120.6(3) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C41 C42 C43 119.5(3) . . ? C41 C42 H42 120.3 . . ? C43 C42 H42 120.3 . . ? C42 C43 C44 120.1(3) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C39 121.2(3) . . ? C43 C44 H44 119.4 . . ? C39 C44 H44 119.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe1 P1 C17 -14.74(11) . . . . ? N1 Fe1 P1 C17 67.11(11) . . . . ? P2 Fe1 P1 C17 -112.10(9) . . . . ? P3 Fe1 P1 C17 166.27(9) . . . . ? N2 Fe1 P1 C11 -132.90(13) . . . . ? N1 Fe1 P1 C11 -51.05(13) . . . . ? P2 Fe1 P1 C11 129.74(11) . . . . ? P3 Fe1 P1 C11 48.11(12) . . . . ? N2 Fe1 P1 C23 99.68(12) . . . . ? N1 Fe1 P1 C23 -178.48(11) . . . . ? P2 Fe1 P1 C23 2.31(10) . . . . ? P3 Fe1 P1 C23 -79.31(10) . . . . ? N2 Fe1 P2 C25 40.51(12) . . . . ? N1 Fe1 P2 C25 25(4) . . . . ? P1 Fe1 P2 C25 144.81(11) . . . . ? P3 Fe1 P2 C25 -98.07(11) . . . . ? N2 Fe1 P2 C31 158.64(11) . . . . ? N1 Fe1 P2 C31 143(4) . . . . ? P1 Fe1 P2 C31 -97.06(9) . . . . ? P3 Fe1 P2 C31 20.06(9) . . . . ? N2 Fe1 P2 C24 -87.29(11) . . . . ? N1 Fe1 P2 C24 -103(4) . . . . ? P1 Fe1 P2 C24 17.00(10) . . . . ? P3 Fe1 P2 C24 134.12(10) . . . . ? N2 Fe1 P3 C33 20.66(14) . . . . ? N1 Fe1 P3 C33 -61.84(12) . . . . ? P2 Fe1 P3 C33 117.39(10) . . . . ? P1 Fe1 P3 C33 -160.82(10) . . . . ? N2 Fe1 P3 C39 144.20(14) . . . . ? N1 Fe1 P3 C39 61.70(13) . . . . ? P2 Fe1 P3 C39 -119.06(11) . . . . ? P1 Fe1 P3 C39 -37.28(12) . . . . ? N2 Fe1 P3 C32 -93.60(14) . . . . ? N1 Fe1 P3 C32 -176.11(11) . . . . ? P2 Fe1 P3 C32 3.13(10) . . . . ? P1 Fe1 P3 C32 84.92(10) . . . . ? N2 Fe1 N1 C1 179.6(2) . . . . ? P2 Fe1 N1 C1 -165(4) . . . . ? P1 Fe1 N1 C1 75.4(2) . . . . ? P3 Fe1 N1 C1 -41.8(2) . . . . ? N2 Fe1 N1 C5 4.41(18) . . . . ? P2 Fe1 N1 C5 20(5) . . . . ? P1 Fe1 N1 C5 -99.78(18) . . . . ? P3 Fe1 N1 C5 142.95(18) . . . . ? N1 Fe1 N2 C10 -175.3(2) . . . . ? P2 Fe1 N2 C10 5.0(2) . . . . ? P1 Fe1 N2 C10 -82.1(2) . . . . ? P3 Fe1 N2 C10 96.5(2) . . . . ? N1 Fe1 N2 C6 -7.17(17) . . . . ? P2 Fe1 N2 C6 173.08(16) . . . . ? P1 Fe1 N2 C6 86.05(17) . . . . ? P3 Fe1 N2 C6 -95.32(18) . . . . ? C5 N1 C1 C2 -1.0(4) . . . . ? Fe1 N1 C1 C2 -176.2(2) . . . . ? N1 C1 C2 C3 0.0(5) . . . . ? C1 C2 C3 C4 0.9(5) . . . . ? C2 C3 C4 C5 -0.6(5) . . . . ? C1 N1 C5 C4 1.3(4) . . . . ? Fe1 N1 C5 C4 177.0(2) . . . . ? C1 N1 C5 C6 -176.7(2) . . . . ? Fe1 N1 C5 C6 -0.9(3) . . . . ? C3 C4 C5 N1 -0.5(4) . . . . ? C3 C4 C5 C6 177.2(3) . . . . ? C10 N2 C6 C7 2.8(3) . . . . ? Fe1 N2 C6 C7 -167.1(2) . . . . ? C10 N2 C6 C5 178.6(2) . . . . ? Fe1 N2 C6 C5 8.7(3) . . . . ? N1 C5 C6 N2 -4.9(3) . . . . ? C4 C5 C6 N2 177.2(2) . . . . ? N1 C5 C6 C7 170.8(2) . . . . ? C4 C5 C6 C7 -7.1(4) . . . . ? N2 C6 C7 C8 -2.2(4) . . . . ? C5 C6 C7 C8 -177.5(3) . . . . ? C6 C7 C8 C9 -0.5(4) . . . . ? C7 C8 C9 C10 2.3(4) . . . . ? C8 C9 C10 N2 -1.6(4) . . . . ? C6 N2 C10 C9 -1.0(4) . . . . ? Fe1 N2 C10 C9 167.3(2) . . . . ? C17 P1 C11 C12 -146.6(2) . . . . ? C23 P1 C11 C12 105.5(2) . . . . ? Fe1 P1 C11 C12 -26.1(3) . . . . ? C17 P1 C11 C16 33.4(2) . . . . ? C23 P1 C11 C16 -74.5(2) . . . . ? Fe1 P1 C11 C16 153.92(18) . . . . ? C16 C11 C12 C13 -0.1(4) . . . . ? P1 C11 C12 C13 179.9(2) . . . . ? C11 C12 C13 C14 0.5(5) . . . . ? C12 C13 C14 C15 0.1(5) . . . . ? C13 C14 C15 C16 -1.1(5) . . . . ? C14 C15 C16 C11 1.5(4) . . . . ? C12 C11 C16 C15 -0.9(4) . . . . ? P1 C11 C16 C15 179.1(2) . . . . ? C11 P1 C17 C22 -132.9(2) . . . . ? C23 P1 C17 C22 -27.8(2) . . . . ? Fe1 P1 C17 C22 91.7(2) . . . . ? C11 P1 C17 C18 57.3(2) . . . . ? C23 P1 C17 C18 162.4(2) . . . . ? Fe1 P1 C17 C18 -78.1(2) . . . . ? C22 C17 C18 C19 -0.3(4) . . . . ? P1 C17 C18 C19 169.9(2) . . . . ? C17 C18 C19 C20 -0.3(4) . . . . ? C18 C19 C20 C21 0.4(4) . . . . ? C19 C20 C21 C22 0.1(4) . . . . ? C20 C21 C22 C17 -0.7(4) . . . . ? C18 C17 C22 C21 0.7(4) . . . . ? P1 C17 C22 C21 -169.1(2) . . . . ? C17 P1 C23 C24 90.0(2) . . . . ? C11 P1 C23 C24 -165.60(18) . . . . ? Fe1 P1 C23 C24 -25.0(2) . . . . ? P1 C23 C24 P2 36.1(2) . . . . ? C25 P2 C24 C23 -174.25(17) . . . . ? C31 P2 C24 C23 83.24(19) . . . . ? Fe1 P2 C24 C23 -35.95(19) . . . . ? C31 P2 C25 C26 94.3(2) . . . . ? C24 P2 C25 C26 -10.8(3) . . . . ? Fe1 P2 C25 C26 -142.1(2) . . . . ? C31 P2 C25 C30 -83.6(2) . . . . ? C24 P2 C25 C30 171.3(2) . . . . ? Fe1 P2 C25 C30 40.0(2) . . . . ? C30 C25 C26 C27 0.3(4) . . . . ? P2 C25 C26 C27 -177.6(2) . . . . ? C25 C26 C27 C28 1.7(4) . . . . ? C26 C27 C28 C29 -1.7(4) . . . . ? C27 C28 C29 C30 -0.4(4) . . . . ? C28 C29 C30 C25 2.4(4) . . . . ? C26 C25 C30 C29 -2.3(4) . . . . ? P2 C25 C30 C29 175.7(2) . . . . ? C25 P2 C31 C32 89.19(19) . . . . ? C24 P2 C31 C32 -164.39(18) . . . . ? Fe1 P2 C31 C32 -43.97(19) . . . . ? P2 C31 C32 P3 44.4(2) . . . . ? C33 P3 C32 C31 -151.95(18) . . . . ? C39 P3 C32 C31 106.80(19) . . . . ? Fe1 P3 C32 C31 -30.4(2) . . . . ? C39 P3 C33 C34 -131.2(2) . . . . ? C32 P3 C33 C34 126.5(2) . . . . ? Fe1 P3 C33 C34 7.0(3) . . . . ? C39 P3 C33 C38 50.4(2) . . . . ? C32 P3 C33 C38 -51.9(2) . . . . ? Fe1 P3 C33 C38 -171.45(19) . . . . ? C38 C33 C34 C35 -1.0(4) . . . . ? P3 C33 C34 C35 -179.5(2) . . . . ? C33 C34 C35 C36 0.8(5) . . . . ? C34 C35 C36 C37 -0.3(5) . . . . ? C35 C36 C37 C38 -0.1(5) . . . . ? C36 C37 C38 C33 -0.1(4) . . . . ? C34 C33 C38 C37 0.6(4) . . . . ? P3 C33 C38 C37 179.1(2) . . . . ? C33 P3 C39 C40 41.3(2) . . . . ? C32 P3 C39 C40 145.1(2) . . . . ? Fe1 P3 C39 C40 -88.3(2) . . . . ? C33 P3 C39 C44 -142.6(2) . . . . ? C32 P3 C39 C44 -38.8(2) . . . . ? Fe1 P3 C39 C44 87.8(2) . . . . ? C44 C39 C40 C41 -1.5(4) . . . . ? P3 C39 C40 C41 174.7(2) . . . . ? C39 C40 C41 C42 0.8(5) . . . . ? C40 C41 C42 C43 1.1(5) . . . . ? C41 C42 C43 C44 -2.3(5) . . . . ? C42 C43 C44 C39 1.6(5) . . . . ? C40 C39 C44 C43 0.3(4) . . . . ? P3 C39 C44 C43 -176.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.68 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.699 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.086 data_apx1234_0m _database_code_depnum_ccdc_archive 'CCDC 884464' #TrackingRef '- Apx1234_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H74 Cl2 Fe P6' _chemical_formula_weight 1287.91 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' 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' Cl Cl 0.1484 0.1585 '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 10.3077(7) _cell_length_b 10.9001(8) _cell_length_c 15.4955(11) _cell_angle_alpha 71.4830(10) _cell_angle_beta 84.0830(10) _cell_angle_gamma 77.5960(10) _cell_volume 1611.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5432 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.86 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 674 _exptl_absorpt_coefficient_mu 0.510 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8831 _exptl_absorpt_correction_T_max 0.9274 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16475 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.89 _reflns_number_total 6231 _reflns_number_gt 5264 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. C41 C42 C43 C44 C45; ISOR restraints were placed on these carbon atoms residing in a disordered lattice toluene molecule to keep them from going non-positive-definite. ; _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^)+(0.0435P)^2^+0.8744P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6231 _refine_ls_number_parameters 394 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0927 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.063 _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 1.0000 0.5000 0.5000 0.01309(11) Uani 1 2 d S . . Cl1 Cl 0.83054(5) 0.43872(5) 0.43991(3) 0.01587(12) Uani 1 1 d . . . P1 P 1.09761(5) 0.63911(5) 0.33994(3) 0.01337(12) Uani 1 1 d . . . P2 P 0.86451(5) 0.73847(5) 0.48211(3) 0.01357(12) Uani 1 1 d . . . P3 P 0.84064(5) 0.82583(5) 0.74782(4) 0.01658(13) Uani 1 1 d . . . C1 C 1.0169(2) 0.69102(19) 0.23051(13) 0.0160(4) Uani 1 1 d . . . C2 C 0.8974(2) 0.6554(2) 0.22470(15) 0.0223(5) Uani 1 1 d . . . H2 H 0.8590 0.6004 0.2772 0.027 Uiso 1 1 calc R . . C3 C 0.8336(2) 0.6997(2) 0.14246(16) 0.0285(5) Uani 1 1 d . . . H3 H 0.7514 0.6755 0.1393 0.034 Uiso 1 1 calc R . . C4 C 0.8887(2) 0.7784(2) 0.06552(15) 0.0249(5) Uani 1 1 d . . . H4 H 0.8456 0.8071 0.0093 0.030 Uiso 1 1 calc R . . C5 C 1.0071(2) 0.8154(2) 0.07080(14) 0.0224(5) Uani 1 1 d . . . H5 H 1.0450 0.8704 0.0182 0.027 Uiso 1 1 calc R . . C6 C 1.0706(2) 0.7723(2) 0.15253(14) 0.0198(5) Uani 1 1 d . . . H6 H 1.1517 0.7985 0.1556 0.024 Uiso 1 1 calc R . . C7 C 1.2735(2) 0.60615(19) 0.30643(13) 0.0154(4) Uani 1 1 d . . . C8 C 1.3180(2) 0.5427(2) 0.24043(14) 0.0177(4) Uani 1 1 d . . . H8 H 1.2555 0.5222 0.2087 0.021 Uiso 1 1 calc R . . C9 C 1.4530(2) 0.5095(2) 0.22095(15) 0.0215(5) Uani 1 1 d . . . H9 H 1.4826 0.4662 0.1761 0.026 Uiso 1 1 calc R . . C10 C 1.5449(2) 0.5393(2) 0.26672(15) 0.0228(5) Uani 1 1 d . . . H10 H 1.6372 0.5161 0.2533 0.027 Uiso 1 1 calc R . . C11 C 1.5024(2) 0.6024(2) 0.33182(15) 0.0222(5) Uani 1 1 d . . . H11 H 1.5653 0.6237 0.3627 0.027 Uiso 1 1 calc R . . C12 C 1.3675(2) 0.6349(2) 0.35208(14) 0.0189(4) Uani 1 1 d . . . H12 H 1.3388 0.6771 0.3976 0.023 Uiso 1 1 calc R . . C13 C 1.0770(2) 0.80089(19) 0.35963(14) 0.0157(4) Uani 1 1 d . . . H13A H 1.1293 0.7922 0.4121 0.019 Uiso 1 1 calc R . . H13B H 1.1099 0.8648 0.3052 0.019 Uiso 1 1 calc R . . C14 C 0.9299(2) 0.85057(19) 0.37887(13) 0.0162(4) Uani 1 1 d . . . H14A H 0.8783 0.8589 0.3261 0.019 Uiso 1 1 calc R . . H14B H 0.9184 0.9391 0.3865 0.019 Uiso 1 1 calc R . . C15 C 0.6847(2) 0.7907(2) 0.47028(13) 0.0153(4) Uani 1 1 d . . . C16 C 0.6021(2) 0.7077(2) 0.52424(14) 0.0193(4) Uani 1 1 d . . . H16 H 0.6401 0.6247 0.5646 0.023 Uiso 1 1 calc R . . C17 C 0.4652(2) 0.7451(2) 0.51962(15) 0.0225(5) Uani 1 1 d . . . H17 H 0.4097 0.6886 0.5575 0.027 Uiso 1 1 calc R . . C18 C 0.4093(2) 0.8648(2) 0.45970(16) 0.0257(5) Uani 1 1 d . . . H18 H 0.3154 0.8904 0.4561 0.031 Uiso 1 1 calc R . . C19 C 0.4899(2) 0.9472(2) 0.40513(17) 0.0292(5) Uani 1 1 d . . . H19 H 0.4514 1.0289 0.3636 0.035 Uiso 1 1 calc R . . C20 C 0.6266(2) 0.9111(2) 0.41078(16) 0.0237(5) Uani 1 1 d . . . H20 H 0.6814 0.9690 0.3737 0.028 Uiso 1 1 calc R . . C21 C 0.8925(2) 0.8119(2) 0.56883(13) 0.0165(4) Uani 1 1 d . . . H21A H 0.9875 0.8173 0.5661 0.020 Uiso 1 1 calc R . . H21B H 0.8398 0.9028 0.5547 0.020 Uiso 1 1 calc R . . C22 C 0.8542(2) 0.7329(2) 0.66521(13) 0.0170(4) Uani 1 1 d . . . H22A H 0.9218 0.6511 0.6854 0.020 Uiso 1 1 calc R . . H22B H 0.7679 0.7073 0.6643 0.020 Uiso 1 1 calc R . . C23 C 1.0138(2) 0.82108(19) 0.76779(13) 0.0162(4) Uani 1 1 d . . . C24 C 1.1256(2) 0.7556(2) 0.73009(14) 0.0201(5) Uani 1 1 d . . . H24 H 1.1149 0.7029 0.6939 0.024 Uiso 1 1 calc R . . C25 C 1.2524(2) 0.7673(2) 0.74528(15) 0.0235(5) Uani 1 1 d . . . H25 H 1.3277 0.7236 0.7184 0.028 Uiso 1 1 calc R . . C26 C 1.2703(2) 0.8416(2) 0.79879(15) 0.0234(5) Uani 1 1 d . . . H26 H 1.3573 0.8482 0.8095 0.028 Uiso 1 1 calc R . . C27 C 1.1602(2) 0.9068(2) 0.83693(14) 0.0224(5) Uani 1 1 d . . . H27 H 1.1716 0.9583 0.8738 0.027 Uiso 1 1 calc R . . C28 C 1.0338(2) 0.8967(2) 0.82119(13) 0.0183(4) Uani 1 1 d . . . H28 H 0.9591 0.9422 0.8473 0.022 Uiso 1 1 calc R . . C29 C 0.7935(2) 0.7032(2) 0.85214(14) 0.0175(4) Uani 1 1 d . . . C30 C 0.8768(2) 0.5840(2) 0.89358(14) 0.0199(5) Uani 1 1 d . . . H30 H 0.9642 0.5641 0.8689 0.024 Uiso 1 1 calc R . . C31 C 0.8329(2) 0.4944(2) 0.97058(15) 0.0248(5) Uani 1 1 d . . . H31 H 0.8904 0.4134 0.9985 0.030 Uiso 1 1 calc R . . C32 C 0.7060(2) 0.5224(2) 1.00686(16) 0.0285(5) Uani 1 1 d . . . H32 H 0.6759 0.4602 1.0592 0.034 Uiso 1 1 calc R . . C33 C 0.6225(2) 0.6409(3) 0.96712(17) 0.0314(6) Uani 1 1 d . . . H33 H 0.5355 0.6606 0.9923 0.038 Uiso 1 1 calc R . . C34 C 0.6667(2) 0.7310(2) 0.89017(15) 0.0247(5) Uani 1 1 d . . . H34 H 0.6095 0.8126 0.8632 0.030 Uiso 1 1 calc R . . C41 C 0.5280(5) 0.0372(5) 0.9482(3) 0.0284(11) Uani 0.50 1 d PU . . C42 C 0.4613(6) 0.0632(6) 0.8871(4) 0.0410(13) Uani 0.50 1 d PU . . C43 C 0.6339(5) 0.0924(6) 0.9686(4) 0.0401(13) Uani 0.50 1 d PU . . C44 C 0.4145(3) -0.0139(3) 0.9595(2) 0.0409(7) Uani 1 1 d U . . C45 C 0.5783(3) 0.1171(3) 0.8729(2) 0.0548(8) Uani 1 1 d U . . 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 0.0122(2) 0.0144(2) 0.0131(2) -0.00400(16) -0.00109(16) -0.00345(16) Cl1 0.0143(2) 0.0183(3) 0.0156(2) -0.00440(19) -0.00199(19) -0.00482(19) P1 0.0132(3) 0.0148(3) 0.0120(3) -0.0031(2) -0.0005(2) -0.0039(2) P2 0.0138(3) 0.0145(3) 0.0122(3) -0.0035(2) -0.0007(2) -0.0030(2) P3 0.0166(3) 0.0183(3) 0.0159(3) -0.0067(2) -0.0024(2) -0.0025(2) C1 0.0190(11) 0.0150(10) 0.0134(10) -0.0044(8) -0.0010(8) -0.0017(8) C2 0.0223(12) 0.0264(12) 0.0173(11) -0.0029(9) -0.0032(9) -0.0076(9) C3 0.0247(12) 0.0376(14) 0.0239(12) -0.0046(10) -0.0065(10) -0.0122(11) C4 0.0299(13) 0.0285(12) 0.0160(11) -0.0072(9) -0.0071(9) -0.0015(10) C5 0.0281(12) 0.0220(12) 0.0150(11) -0.0039(9) 0.0009(9) -0.0041(9) C6 0.0208(11) 0.0210(11) 0.0178(11) -0.0056(9) -0.0007(9) -0.0054(9) C7 0.0148(10) 0.0134(10) 0.0154(10) -0.0005(8) 0.0004(8) -0.0036(8) C8 0.0171(11) 0.0186(11) 0.0177(10) -0.0045(9) -0.0016(8) -0.0052(8) C9 0.0204(11) 0.0221(11) 0.0224(11) -0.0091(9) 0.0051(9) -0.0040(9) C10 0.0140(11) 0.0243(12) 0.0296(12) -0.0080(10) 0.0040(9) -0.0052(9) C11 0.0178(11) 0.0244(12) 0.0262(12) -0.0083(10) -0.0030(9) -0.0058(9) C12 0.0185(11) 0.0209(11) 0.0190(11) -0.0067(9) -0.0004(9) -0.0067(9) C13 0.0188(11) 0.0141(10) 0.0145(10) -0.0035(8) 0.0022(8) -0.0062(8) C14 0.0195(11) 0.0142(10) 0.0132(10) -0.0023(8) 0.0000(8) -0.0024(8) C15 0.0151(10) 0.0182(10) 0.0149(10) -0.0083(8) -0.0017(8) -0.0026(8) C16 0.0208(11) 0.0207(11) 0.0173(10) -0.0060(9) -0.0039(9) -0.0044(9) C17 0.0191(11) 0.0292(12) 0.0243(12) -0.0133(10) 0.0011(9) -0.0081(9) C18 0.0154(11) 0.0288(13) 0.0372(14) -0.0178(11) -0.0061(10) 0.0005(9) C19 0.0252(12) 0.0203(12) 0.0394(14) -0.0074(10) -0.0115(11) 0.0038(10) C20 0.0218(12) 0.0193(11) 0.0274(12) -0.0042(9) -0.0030(9) -0.0020(9) C21 0.0173(11) 0.0161(10) 0.0171(10) -0.0061(8) -0.0001(8) -0.0042(8) C22 0.0191(11) 0.0193(11) 0.0139(10) -0.0053(8) -0.0017(8) -0.0052(9) C23 0.0195(11) 0.0149(10) 0.0130(10) -0.0006(8) -0.0042(8) -0.0045(8) C24 0.0232(11) 0.0182(11) 0.0205(11) -0.0083(9) -0.0017(9) -0.0028(9) C25 0.0194(11) 0.0235(12) 0.0242(12) -0.0052(9) -0.0014(9) 0.0000(9) C26 0.0201(11) 0.0263(12) 0.0226(11) -0.0025(9) -0.0054(9) -0.0071(9) C27 0.0273(12) 0.0272(12) 0.0164(11) -0.0079(9) -0.0034(9) -0.0096(10) C28 0.0225(11) 0.0191(11) 0.0129(10) -0.0040(8) 0.0015(8) -0.0055(9) C29 0.0214(11) 0.0210(11) 0.0137(10) -0.0082(8) -0.0012(8) -0.0067(9) C30 0.0213(11) 0.0236(11) 0.0175(11) -0.0094(9) -0.0004(9) -0.0054(9) C31 0.0320(13) 0.0244(12) 0.0204(11) -0.0077(9) -0.0048(10) -0.0077(10) C32 0.0355(14) 0.0328(13) 0.0198(12) -0.0057(10) 0.0040(10) -0.0180(11) C33 0.0224(12) 0.0453(15) 0.0290(13) -0.0135(12) 0.0062(10) -0.0120(11) C34 0.0214(12) 0.0300(13) 0.0239(12) -0.0107(10) -0.0002(9) -0.0039(10) C41 0.0267(19) 0.0248(19) 0.035(2) -0.0103(16) -0.0006(16) -0.0047(15) C42 0.042(2) 0.038(2) 0.041(2) -0.0127(18) -0.0083(18) -0.0008(18) C43 0.038(2) 0.042(2) 0.040(2) -0.0092(18) 0.0002(18) -0.0140(18) C44 0.0302(13) 0.0391(14) 0.0541(15) -0.0100(12) -0.0088(12) -0.0113(11) C45 0.0463(15) 0.0420(15) 0.0730(18) -0.0090(13) -0.0068(14) -0.0126(12) _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 Cl1 2.3656(5) . ? Fe1 Cl1 2.3656(5) 2_766 ? Fe1 P2 2.6166(5) . ? Fe1 P2 2.6166(5) 2_766 ? Fe1 P1 2.6861(5) 2_766 ? Fe1 P1 2.6861(5) . ? P1 C7 1.825(2) . ? P1 C1 1.835(2) . ? P1 C13 1.848(2) . ? P2 C15 1.828(2) . ? P2 C21 1.841(2) . ? P2 C14 1.843(2) . ? P3 C23 1.830(2) . ? P3 C29 1.839(2) . ? P3 C22 1.846(2) . ? C1 C2 1.389(3) . ? C1 C6 1.394(3) . ? C2 C3 1.391(3) . ? C3 C4 1.378(3) . ? C4 C5 1.383(3) . ? C5 C6 1.383(3) . ? C7 C12 1.396(3) . ? C7 C8 1.397(3) . ? C8 C9 1.388(3) . ? C9 C10 1.386(3) . ? C10 C11 1.380(3) . ? C11 C12 1.387(3) . ? C13 C14 1.529(3) . ? C15 C20 1.392(3) . ? C15 C16 1.395(3) . ? C16 C17 1.385(3) . ? C17 C18 1.384(3) . ? C18 C19 1.380(3) . ? C19 C20 1.384(3) . ? C21 C22 1.528(3) . ? C23 C28 1.396(3) . ? C23 C24 1.396(3) . ? C24 C25 1.392(3) . ? C25 C26 1.378(3) . ? C26 C27 1.387(3) . ? C27 C28 1.383(3) . ? C29 C34 1.391(3) . ? C29 C30 1.393(3) . ? C30 C31 1.386(3) . ? C31 C32 1.381(3) . ? C32 C33 1.384(4) . ? C33 C34 1.389(3) . ? C41 C42 1.152(7) . ? C41 C45 1.347(6) . ? C41 C44 1.372(5) . ? C41 C43 1.458(7) . ? C41 C44 1.529(6) 2_657 ? C41 C41 1.658(10) 2_657 ? C42 C44 1.289(6) . ? C42 C45 1.419(6) . ? C43 C44 1.298(6) 2_657 ? C43 C45 1.567(6) . ? C44 C43 1.298(6) 2_657 ? C44 C41 1.529(6) 2_657 ? 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 Cl1 Fe1 Cl1 180.00 . 2_766 ? Cl1 Fe1 P2 93.143(17) . . ? Cl1 Fe1 P2 86.857(17) 2_766 . ? Cl1 Fe1 P2 86.857(17) . 2_766 ? Cl1 Fe1 P2 93.143(17) 2_766 2_766 ? P2 Fe1 P2 180.00 . 2_766 ? Cl1 Fe1 P1 83.255(16) . 2_766 ? Cl1 Fe1 P1 96.745(16) 2_766 2_766 ? P2 Fe1 P1 102.142(16) . 2_766 ? P2 Fe1 P1 77.858(16) 2_766 2_766 ? Cl1 Fe1 P1 96.745(16) . . ? Cl1 Fe1 P1 83.255(16) 2_766 . ? P2 Fe1 P1 77.858(16) . . ? P2 Fe1 P1 102.142(16) 2_766 . ? P1 Fe1 P1 180.0 2_766 . ? C7 P1 C1 102.38(9) . . ? C7 P1 C13 102.52(9) . . ? C1 P1 C13 99.64(9) . . ? C7 P1 Fe1 121.97(6) . . ? C1 P1 Fe1 125.38(7) . . ? C13 P1 Fe1 99.97(6) . . ? C15 P2 C21 101.55(9) . . ? C15 P2 C14 102.54(9) . . ? C21 P2 C14 100.62(9) . . ? C15 P2 Fe1 125.69(7) . . ? C21 P2 Fe1 115.35(7) . . ? C14 P2 Fe1 107.77(7) . . ? C23 P3 C29 101.67(9) . . ? C23 P3 C22 103.58(9) . . ? C29 P3 C22 100.30(9) . . ? C2 C1 C6 118.55(19) . . ? C2 C1 P1 120.50(15) . . ? C6 C1 P1 120.87(16) . . ? C1 C2 C3 120.3(2) . . ? C4 C3 C2 120.6(2) . . ? C3 C4 C5 119.5(2) . . ? C4 C5 C6 120.2(2) . . ? C5 C6 C1 120.8(2) . . ? C12 C7 C8 118.63(19) . . ? C12 C7 P1 119.96(16) . . ? C8 C7 P1 121.22(15) . . ? C9 C8 C7 120.29(19) . . ? C10 C9 C8 120.3(2) . . ? C11 C10 C9 120.1(2) . . ? C10 C11 C12 119.9(2) . . ? C11 C12 C7 120.9(2) . . ? C14 C13 P1 109.30(13) . . ? C13 C14 P2 111.77(14) . . ? C20 C15 C16 118.58(19) . . ? C20 C15 P2 122.66(16) . . ? C16 C15 P2 118.75(16) . . ? C17 C16 C15 120.7(2) . . ? C18 C17 C16 119.9(2) . . ? C19 C18 C17 120.0(2) . . ? C18 C19 C20 120.2(2) . . ? C19 C20 C15 120.6(2) . . ? C22 C21 P2 112.70(14) . . ? C21 C22 P3 112.79(14) . . ? C28 C23 C24 118.05(19) . . ? C28 C23 P3 116.04(16) . . ? C24 C23 P3 125.79(16) . . ? C25 C24 C23 120.3(2) . . ? C26 C25 C24 120.8(2) . . ? C25 C26 C27 119.5(2) . . ? C28 C27 C26 119.9(2) . . ? C27 C28 C23 121.4(2) . . ? C34 C29 C30 118.8(2) . . ? C34 C29 P3 117.60(16) . . ? C30 C29 P3 123.61(16) . . ? C31 C30 C29 120.4(2) . . ? C32 C31 C30 120.2(2) . . ? C31 C32 C33 120.1(2) . . ? C32 C33 C34 119.7(2) . . ? C33 C34 C29 120.8(2) . . ? C42 C41 C45 68.7(4) . . ? C42 C41 C44 60.7(4) . . ? C45 C41 C44 129.3(4) . . ? C42 C41 C43 134.7(5) . . ? C45 C41 C43 67.8(3) . . ? C44 C41 C43 159.8(5) . . ? C42 C41 C44 166.4(5) . 2_657 ? C45 C41 C44 119.2(4) . 2_657 ? C44 C41 C44 110.6(3) . 2_657 ? C43 C41 C44 51.4(3) . 2_657 ? C42 C41 C41 119.4(6) . 2_657 ? C45 C41 C41 167.2(6) . 2_657 ? C44 C41 C41 59.7(3) . 2_657 ? C43 C41 C41 101.7(5) . 2_657 ? C44 C41 C41 50.8(3) 2_657 2_657 ? C41 C42 C44 68.1(4) . . ? C41 C42 C45 62.2(4) . . ? C44 C42 C45 130.3(5) . . ? C44 C43 C41 67.1(3) 2_657 . ? C44 C43 C45 119.8(4) 2_657 . ? C41 C43 C45 52.7(3) . . ? C42 C44 C43 178.9(4) . 2_657 ? C42 C44 C41 51.2(3) . . ? C43 C44 C41 129.8(4) 2_657 . ? C42 C44 C41 119.7(4) . 2_657 ? C43 C44 C41 61.4(3) 2_657 2_657 ? C41 C44 C41 69.4(3) . 2_657 ? C41 C45 C42 49.2(3) . . ? C41 C45 C43 59.5(3) . . ? C42 C45 C43 107.6(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.89 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.551 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.060