# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Paul, Frederic' _publ_contact_author_email frederic.paul@univ-rennes1.fr _publ_section_title ; Stille-Type Aryl-Aryl Cross-Coupling Catalysis using Triarylphosphine Ligands with Electron-Rich Fe(II)-alkynyl Substituents ; loop_ _publ_author_name G.Grelaud A.Tohme G.Argouarch T.Roisnel F.Paul data_paraPPh2 _database_code_depnum_ccdc_archive 'CCDC 755886' #TrackingRef 'paraPPh2.cif' _audit_creation_date 2009-02-25T11:12:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C56 H53 Fe1 P3' _chemical_formula_sum 'C56 H53 Fe P3' _chemical_formula_weight 874.74 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9096(6) _cell_length_b 11.1052(5) _cell_length_c 20.2561(10) _cell_angle_alpha 102.897(3) _cell_angle_beta 94.369(3) _cell_angle_gamma 107.657(2) _cell_volume 2251.97(19) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2521 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 24.66 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description stick _exptl_crystal_colour orange _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.29 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.479 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.916 _exptl_absorpt_correction_T_max 0.976 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0775 _diffrn_reflns_av_unetI/netI 0.1175 _diffrn_reflns_number 22820 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 27.38 _diffrn_reflns_theta_full 27.38 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 10073 _reflns_number_gt 6815 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SAINT' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0329P)^2^+0.7125P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10073 _refine_ls_number_parameters 546 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1037 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1103 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.457 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.086 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.31171(4) 0.08736(4) 0.85311(2) 0.01292(12) Uani 1 d . . . P1 P 0.36745(8) 0.16923(8) 0.76741(4) 0.01492(19) Uani 1 d . . . P2 P 0.11471(8) 0.07412(8) 0.81539(4) 0.01462(19) Uani 1 d . . . C1 C 0.4800(3) 0.2048(3) 0.92495(16) 0.0146(7) Uani 1 d . . . C2 C 0.4744(3) 0.0710(3) 0.90767(16) 0.0150(7) Uani 1 d . . . C3 C 0.3590(3) -0.0030(3) 0.92957(16) 0.0166(7) Uani 1 d . . . C4 C 0.2925(3) 0.0837(3) 0.95737(16) 0.0150(7) Uani 1 d . . . C5 C 0.3679(3) 0.2139(3) 0.95491(16) 0.0150(7) Uani 1 d . . . C6 C 0.5974(3) 0.3178(3) 0.92203(17) 0.0190(7) Uani 1 d . . . H6A H 0.5689 0.3884 0.9122 0.028 Uiso 1 calc R . . H6B H 0.6443 0.2881 0.8858 0.028 Uiso 1 calc R . . H6C H 0.6552 0.35 0.9662 0.028 Uiso 1 calc R . . C7 C 0.5743(3) 0.0160(3) 0.87867(17) 0.0210(8) Uani 1 d . . . H7A H 0.6286 0.0763 0.8556 0.032 Uiso 1 calc R . . H7B H 0.5304 -0.0689 0.8456 0.032 Uiso 1 calc R . . H7C H 0.6291 0.0045 0.9158 0.032 Uiso 1 calc R . . C8 C 0.3238(3) -0.1457(3) 0.92702(17) 0.0228(8) Uani 1 d . . . H8A H 0.2407 -0.1747 0.9438 0.034 Uiso 1 calc R . . H8B H 0.392 -0.1594 0.9559 0.034 Uiso 1 calc R . . H8C H 0.3158 -0.1962 0.8796 0.034 Uiso 1 calc R . . C9 C 0.1758(3) 0.0544(3) 0.99337(17) 0.0199(8) Uani 1 d . . . H9A H 0.1222 -0.0377 0.975 0.03 Uiso 1 calc R . . H9B H 0.1245 0.1103 0.986 0.03 Uiso 1 calc R . . H9C H 0.2047 0.0714 1.0426 0.03 Uiso 1 calc R . . C10 C 0.3397(3) 0.3348(3) 0.99009(16) 0.0186(7) Uani 1 d . . . H10A H 0.3453 0.342 1.0394 0.028 Uiso 1 calc R . . H10B H 0.2519 0.3291 0.9715 0.028 Uiso 1 calc R . . H10C H 0.4035 0.412 0.9823 0.028 Uiso 1 calc R . . C11 C 0.2304(3) 0.0891(3) 0.69543(16) 0.0172(7) Uani 1 d . . . H11A H 0.2385 0.1421 0.6617 0.021 Uiso 1 calc R . . H11B H 0.2327 0.0016 0.6721 0.021 Uiso 1 calc R . . C12 C 0.1010(3) 0.0753(3) 0.72295(16) 0.0189(7) Uani 1 d . . . H12A H 0.0344 -0.0069 0.6956 0.023 Uiso 1 calc R . . H12B H 0.0714 0.1489 0.7173 0.023 Uiso 1 calc R . . C13 C 0.3952(3) 0.3434(3) 0.77199(18) 0.0193(8) Uani 1 d . . . C14 C 0.3905(3) 0.4284(3) 0.83259(18) 0.0214(8) Uani 1 d . . . H14 H 0.3772 0.3966 0.8722 0.026 Uiso 1 calc R . . C15 C 0.4048(3) 0.5592(3) 0.8371(2) 0.0282(9) Uani 1 d . . . H15 H 0.4034 0.6163 0.8794 0.034 Uiso 1 calc R . . C16 C 0.4211(3) 0.6050(3) 0.7788(2) 0.0298(9) Uani 1 d . . . H16 H 0.4288 0.6934 0.7808 0.036 Uiso 1 calc R . . C17 C 0.4260(3) 0.5216(3) 0.7177(2) 0.0301(9) Uani 1 d . . . H17 H 0.4374 0.5532 0.6779 0.036 Uiso 1 calc R . . C18 C 0.4144(3) 0.3922(3) 0.71424(19) 0.0238(8) Uani 1 d . . . H18 H 0.4196 0.3364 0.6723 0.029 Uiso 1 calc R . . C19 C 0.5109(3) 0.1467(3) 0.73076(17) 0.0181(7) Uani 1 d . . . C20 C 0.6277(3) 0.2516(3) 0.74099(18) 0.0243(8) Uani 1 d . . . H20 H 0.6321 0.3368 0.7655 0.029 Uiso 1 calc R . . C21 C 0.7365(4) 0.2319(4) 0.7155(2) 0.0314(9) Uani 1 d . . . H21 H 0.8146 0.3039 0.7229 0.038 Uiso 1 calc R . . C22 C 0.7332(4) 0.1096(4) 0.67981(18) 0.0307(9) Uani 1 d . . . H22 H 0.808 0.097 0.6622 0.037 Uiso 1 calc R . . C23 C 0.6190(4) 0.0052(3) 0.66999(18) 0.0266(8) Uani 1 d . . . H23 H 0.6155 -0.0795 0.6452 0.032 Uiso 1 calc R . . C24 C 0.5101(3) 0.0227(3) 0.69572(17) 0.0225(8) Uani 1 d . . . H24 H 0.4335 -0.0507 0.6895 0.027 Uiso 1 calc R . . C25 C 0.0469(3) 0.2027(3) 0.85392(16) 0.0153(7) Uani 1 d . . . C26 C -0.0343(3) 0.1869(3) 0.90373(17) 0.0192(7) Uani 1 d . . . H26 H -0.0593 0.1062 0.9161 0.023 Uiso 1 calc R . . C27 C -0.0795(3) 0.2857(3) 0.93553(18) 0.0237(8) Uani 1 d . . . H27 H -0.1346 0.2723 0.9692 0.028 Uiso 1 calc R . . C28 C -0.0441(3) 0.4040(3) 0.91804(18) 0.0264(8) Uani 1 d . . . H28 H -0.0758 0.4717 0.939 0.032 Uiso 1 calc R . . C29 C 0.0381(3) 0.4223(3) 0.86961(19) 0.0255(8) Uani 1 d . . . H29 H 0.0644 0.5039 0.8582 0.031 Uiso 1 calc R . . C30 C 0.0822(3) 0.3230(3) 0.83764(18) 0.0201(8) Uani 1 d . . . H30 H 0.1375 0.337 0.8041 0.024 Uiso 1 calc R . . C31 C -0.0230(3) -0.0723(3) 0.81570(16) 0.0161(7) Uani 1 d . . . C32 C -0.0029(3) -0.1724(3) 0.84091(17) 0.0185(7) Uani 1 d . . . H32 H 0.0829 -0.1665 0.8578 0.022 Uiso 1 calc R . . C33 C -0.1075(3) -0.2814(3) 0.84167(18) 0.0227(8) Uani 1 d . . . H33 H -0.0926 -0.3491 0.8592 0.027 Uiso 1 calc R . . C34 C -0.2325(3) -0.2916(3) 0.81707(17) 0.0224(8) Uani 1 d . . . H34 H -0.3036 -0.3659 0.8178 0.027 Uiso 1 calc R . . C35 C -0.2545(3) -0.1925(3) 0.79105(17) 0.0225(8) Uani 1 d . . . H35 H -0.3404 -0.1992 0.7738 0.027 Uiso 1 calc R . . C36 C -0.1492(3) -0.0835(3) 0.79064(17) 0.0201(8) Uani 1 d . . . H36 H -0.1641 -0.016 0.773 0.024 Uiso 1 calc R . . C37 C 0.2677(3) -0.0769(3) 0.78746(16) 0.0155(7) Uani 1 d . . . C38 C 0.2343(3) -0.1833(3) 0.74651(17) 0.0172(7) Uani 1 d . . . C39 C 0.1908(3) -0.3128(3) 0.70003(16) 0.0164(7) Uani 1 d . . . C40 C 0.2188(3) -0.3364(3) 0.63308(17) 0.0191(8) Uani 1 d . . . H40 H 0.2643 -0.2649 0.6162 0.023 Uiso 1 calc R . . C41 C 0.1813(3) -0.4625(3) 0.59091(17) 0.0204(8) Uani 1 d . . . H41 H 0.2008 -0.4758 0.5455 0.024 Uiso 1 calc R . . C42 C 0.1203(3) -0.4213(3) 0.72283(17) 0.0191(7) Uani 1 d . . . H42 H 0.0965 -0.4079 0.7674 0.023 Uiso 1 calc R . . C43 C 0.0857(3) -0.5470(3) 0.68080(17) 0.0201(8) Uani 1 d . . . H43 H 0.0409 -0.619 0.6976 0.024 Uiso 1 calc R . . C44 C 0.1154(3) -0.5703(3) 0.61408(17) 0.0178(7) Uani 1 d . . . C45 C 0.1466(4) -0.7192(3) 0.48812(18) 0.0237(8) Uani 1 d . . . C46 C 0.0826(4) -0.7127(3) 0.42683(18) 0.0255(8) Uani 1 d . . . H46 H -0.0084 -0.7274 0.4214 0.031 Uiso 1 calc R . . C47 C 0.1518(4) -0.6849(3) 0.37394(19) 0.0326(9) Uani 1 d . . . H47 H 0.1077 -0.6811 0.3325 0.039 Uiso 1 calc R . . C48 C 0.2853(4) -0.6626(4) 0.3817(2) 0.0379(10) Uani 1 d . . . H48 H 0.3328 -0.6422 0.3459 0.045 Uiso 1 calc R . . C49 C 0.3489(4) -0.6702(4) 0.4420(2) 0.0409(11) Uani 1 d . . . H49 H 0.4401 -0.6546 0.4475 0.049 Uiso 1 calc R . . P5 P 0.06864(10) -0.74164(8) 0.56365(5) 0.0237(2) Uani 1 d . . . C50 C 0.2797(4) -0.7006(3) 0.4941(2) 0.0336(9) Uani 1 d . . . H50 H 0.3235 -0.7087 0.5344 0.04 Uiso 1 calc R . . C51 C -0.1051(4) -0.7796(3) 0.53321(17) 0.0233(8) Uani 1 d . . . C52 C -0.1766(4) -0.9062(3) 0.49443(18) 0.0294(9) Uani 1 d . . . H52 H -0.1332 -0.9683 0.482 0.035 Uiso 1 calc R . . C53 C -0.3087(4) -0.9426(4) 0.47390(19) 0.0334(10) Uani 1 d . . . H53 H -0.3554 -1.0291 0.4472 0.04 Uiso 1 calc R . . C54 C -0.3742(4) -0.8536(4) 0.49200(19) 0.0331(10) Uani 1 d . . . H54 H -0.4655 -0.8795 0.4779 0.04 Uiso 1 calc R . . C55 C -0.3069(4) -0.7272(3) 0.53046(18) 0.0296(9) Uani 1 d . . . H55 H -0.3516 -0.6663 0.5432 0.036 Uiso 1 calc R . . C56 C -0.1722(4) -0.6903(3) 0.55032(18) 0.0266(9) Uani 1 d . . . H56 H -0.1254 -0.6031 0.5759 0.032 Uiso 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 0.0115(2) 0.0138(2) 0.0143(3) 0.00323(18) 0.00352(19) 0.00543(18) P1 0.0129(4) 0.0159(4) 0.0183(5) 0.0064(3) 0.0050(4) 0.0059(3) P2 0.0119(4) 0.0170(4) 0.0167(5) 0.0048(3) 0.0050(4) 0.0061(3) C1 0.0145(17) 0.0168(15) 0.0139(17) 0.0036(13) 0.0009(13) 0.0080(13) C2 0.0155(17) 0.0209(16) 0.0116(17) 0.0042(13) -0.0011(13) 0.0110(14) C3 0.0193(18) 0.0186(15) 0.0131(17) 0.0031(13) 0.0003(14) 0.0090(14) C4 0.0131(17) 0.0172(15) 0.0151(17) 0.0032(13) 0.0022(14) 0.0066(13) C5 0.0157(17) 0.0164(15) 0.0140(17) 0.0029(13) 0.0036(14) 0.0074(13) C6 0.0127(17) 0.0197(16) 0.025(2) 0.0039(14) 0.0039(15) 0.0066(14) C7 0.0169(18) 0.0249(17) 0.0218(19) 0.0038(15) 0.0053(15) 0.0087(15) C8 0.029(2) 0.0209(17) 0.022(2) 0.0069(15) 0.0006(16) 0.0143(16) C9 0.0183(18) 0.0228(17) 0.0207(19) 0.0075(14) 0.0063(15) 0.0075(14) C10 0.0185(18) 0.0219(16) 0.0170(18) 0.0023(14) 0.0045(14) 0.0107(14) C11 0.0171(18) 0.0215(16) 0.0155(18) 0.0072(14) 0.0065(14) 0.0070(14) C12 0.0164(18) 0.0237(17) 0.0181(18) 0.0058(14) 0.0022(14) 0.0083(14) C13 0.0107(17) 0.0200(16) 0.032(2) 0.0123(15) 0.0061(15) 0.0070(14) C14 0.0148(18) 0.0233(17) 0.030(2) 0.0103(15) 0.0031(15) 0.0094(15) C15 0.021(2) 0.0200(17) 0.044(3) 0.0077(17) 0.0010(18) 0.0082(15) C16 0.0125(19) 0.0175(17) 0.059(3) 0.0145(18) -0.0017(18) 0.0037(14) C17 0.0146(19) 0.033(2) 0.046(3) 0.0237(19) 0.0011(18) 0.0038(16) C18 0.0170(19) 0.0255(18) 0.032(2) 0.0139(16) 0.0036(16) 0.0063(15) C19 0.0168(18) 0.0237(16) 0.0179(18) 0.0101(14) 0.0067(14) 0.0083(14) C20 0.021(2) 0.0290(18) 0.027(2) 0.0120(16) 0.0038(16) 0.0100(16) C21 0.016(2) 0.045(2) 0.038(2) 0.0200(19) 0.0093(18) 0.0077(17) C22 0.025(2) 0.057(3) 0.027(2) 0.0216(19) 0.0165(17) 0.026(2) C23 0.030(2) 0.038(2) 0.019(2) 0.0063(16) 0.0060(16) 0.0210(18) C24 0.0177(19) 0.0277(18) 0.023(2) 0.0062(15) 0.0066(15) 0.0088(15) C25 0.0109(16) 0.0194(15) 0.0161(17) 0.0042(13) 0.0020(13) 0.0062(13) C26 0.0180(18) 0.0204(16) 0.0220(19) 0.0093(14) 0.0062(15) 0.0072(14) C27 0.023(2) 0.0255(18) 0.027(2) 0.0075(16) 0.0106(16) 0.0118(16) C28 0.025(2) 0.0282(18) 0.031(2) 0.0045(16) 0.0082(17) 0.0171(16) C29 0.028(2) 0.0196(17) 0.038(2) 0.0165(16) 0.0086(18) 0.0126(16) C30 0.0158(18) 0.0233(17) 0.025(2) 0.0126(15) 0.0095(15) 0.0062(14) C31 0.0156(17) 0.0174(15) 0.0152(17) 0.0021(13) 0.0054(14) 0.0064(14) C32 0.0158(18) 0.0193(16) 0.0213(19) 0.0060(14) 0.0037(15) 0.0063(14) C33 0.0209(19) 0.0194(16) 0.034(2) 0.0103(15) 0.0120(17) 0.0108(15) C34 0.0195(19) 0.0211(17) 0.026(2) 0.0060(15) 0.0134(16) 0.0041(15) C35 0.0150(18) 0.0225(17) 0.026(2) 0.0002(15) 0.0033(15) 0.0049(14) C36 0.0174(18) 0.0219(16) 0.024(2) 0.0075(15) 0.0073(15) 0.0086(15) C37 0.0128(17) 0.0190(16) 0.0204(18) 0.0119(14) 0.0051(14) 0.0079(13) C38 0.0157(18) 0.0191(16) 0.0184(18) 0.0062(14) 0.0048(14) 0.0065(14) C39 0.0158(17) 0.0179(15) 0.0176(18) 0.0042(13) 0.0018(14) 0.0091(14) C40 0.0226(19) 0.0158(15) 0.0201(19) 0.0064(14) 0.0071(15) 0.0057(14) C41 0.0233(19) 0.0239(17) 0.0139(18) 0.0037(14) 0.0046(15) 0.0083(15) C42 0.0184(18) 0.0234(17) 0.0180(18) 0.0049(14) 0.0054(15) 0.0101(15) C43 0.0168(18) 0.0175(16) 0.025(2) 0.0082(14) 0.0036(15) 0.0029(14) C44 0.0161(18) 0.0161(15) 0.0215(19) 0.0057(14) 0.0015(14) 0.0053(14) C45 0.029(2) 0.0142(16) 0.025(2) -0.0029(14) 0.0041(17) 0.0093(15) C46 0.022(2) 0.0261(18) 0.024(2) 0.0007(16) 0.0028(16) 0.0057(16) C47 0.035(2) 0.040(2) 0.024(2) 0.0034(17) 0.0076(18) 0.0162(19) C48 0.036(3) 0.045(2) 0.026(2) -0.0027(18) 0.013(2) 0.010(2) C49 0.023(2) 0.050(2) 0.039(3) -0.005(2) 0.003(2) 0.0088(19) P5 0.0306(6) 0.0162(4) 0.0220(5) 0.0022(4) 0.0012(4) 0.0070(4) C50 0.033(2) 0.037(2) 0.027(2) -0.0011(17) -0.0016(18) 0.0147(19) C51 0.028(2) 0.0188(16) 0.021(2) 0.0074(14) 0.0049(16) 0.0019(15) C52 0.037(2) 0.0236(18) 0.021(2) 0.0031(15) 0.0100(18) 0.0011(17) C53 0.036(2) 0.0285(19) 0.024(2) 0.0060(17) 0.0101(19) -0.0065(18) C54 0.023(2) 0.040(2) 0.027(2) 0.0110(18) 0.0085(18) -0.0051(18) C55 0.033(2) 0.035(2) 0.022(2) 0.0085(17) 0.0067(18) 0.0116(18) C56 0.033(2) 0.0197(17) 0.023(2) 0.0049(15) 0.0041(17) 0.0033(16) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C37 1.901(3) . ? Fe1 C2 2.095(3) . ? Fe1 C1 2.117(3) . ? Fe1 C3 2.135(3) . ? Fe1 C5 2.143(3) . ? Fe1 C4 2.146(3) . ? Fe1 P2 2.1754(10) . ? Fe1 P1 2.1772(9) . ? P1 C19 1.843(3) . ? P1 C13 1.844(3) . ? P1 C11 1.854(3) . ? P2 C25 1.851(3) . ? P2 C31 1.851(3) . ? P2 C12 1.870(3) . ? C1 C5 1.426(4) . ? C1 C2 1.430(4) . ? C1 C6 1.513(4) . ? C2 C3 1.441(4) . ? C2 C7 1.499(4) . ? C3 C4 1.420(4) . ? C3 C8 1.501(4) . ? C4 C5 1.444(4) . ? C4 C9 1.501(4) . ? C5 C10 1.504(4) . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 C12 1.534(4) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.386(4) . ? C13 C18 1.400(5) . ? C14 C15 1.395(4) . ? C14 H14 0.95 . ? C15 C16 1.388(5) . ? C15 H15 0.95 . ? C16 C17 1.386(5) . ? C16 H16 0.95 . ? C17 C18 1.389(5) . ? C17 H17 0.95 . ? C18 H18 0.95 . ? C19 C24 1.398(4) . ? C19 C20 1.405(4) . ? C20 C21 1.387(5) . ? C20 H20 0.95 . ? C21 C22 1.378(5) . ? C21 H21 0.95 . ? C22 C23 1.385(5) . ? C22 H22 0.95 . ? C23 C24 1.382(4) . ? C23 H23 0.95 . ? C24 H24 0.95 . ? C25 C30 1.395(4) . ? C25 C26 1.398(4) . ? C26 C27 1.386(4) . ? C26 H26 0.95 . ? C27 C28 1.386(5) . ? C27 H27 0.95 . ? C28 C29 1.386(5) . ? C28 H28 0.95 . ? C29 C30 1.386(4) . ? C29 H29 0.95 . ? C30 H30 0.95 . ? C31 C32 1.389(4) . ? C31 C36 1.390(4) . ? C32 C33 1.393(4) . ? C32 H32 0.95 . ? C33 C34 1.378(5) . ? C33 H33 0.95 . ? C34 C35 1.395(5) . ? C34 H34 0.95 . ? C35 C36 1.395(4) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C37 C38 1.214(4) . ? C38 C39 1.446(4) . ? C39 C40 1.398(4) . ? C39 C42 1.413(4) . ? C40 C41 1.386(4) . ? C40 H40 0.95 . ? C41 C44 1.396(4) . ? C41 H41 0.95 . ? C42 C43 1.385(4) . ? C42 H42 0.95 . ? C43 C44 1.400(4) . ? C43 H43 0.95 . ? C44 P5 1.841(3) . ? C45 C50 1.395(5) . ? C45 C46 1.404(5) . ? C45 P5 1.834(4) . ? C46 C47 1.394(5) . ? C46 H46 0.95 . ? C47 C48 1.391(5) . ? C47 H47 0.95 . ? C48 C49 1.390(6) . ? C48 H48 0.95 . ? C49 C50 1.387(5) . ? C49 H49 0.95 . ? P5 C51 1.836(4) . ? C50 H50 0.95 . ? C51 C52 1.396(4) . ? C51 C56 1.402(5) . ? C52 C53 1.377(5) . ? C52 H52 0.95 . ? C53 C54 1.389(5) . ? C53 H53 0.95 . ? C54 C55 1.384(5) . ? C54 H54 0.95 . ? C55 C56 1.400(5) . ? C55 H55 0.95 . ? C56 H56 0.95 . ? 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 C37 Fe1 C2 96.01(13) . . ? C37 Fe1 C1 133.51(13) . . ? C2 Fe1 C1 39.70(11) . . ? C37 Fe1 C3 88.53(13) . . ? C2 Fe1 C3 39.82(12) . . ? C1 Fe1 C3 65.88(12) . . ? C37 Fe1 C5 153.98(13) . . ? C2 Fe1 C5 66.45(12) . . ? C1 Fe1 C5 39.12(11) . . ? C3 Fe1 C5 65.62(11) . . ? C37 Fe1 C4 117.01(12) . . ? C2 Fe1 C4 66.31(12) . . ? C1 Fe1 C4 65.74(12) . . ? C3 Fe1 C4 38.74(11) . . ? C5 Fe1 C4 39.34(11) . . ? C37 Fe1 P2 82.99(10) . . ? C2 Fe1 P2 164.00(9) . . ? C1 Fe1 P2 143.48(9) . . ? C3 Fe1 P2 124.23(9) . . ? C5 Fe1 P2 108.44(9) . . ? C4 Fe1 P2 99.82(9) . . ? C37 Fe1 P1 84.61(10) . . ? C2 Fe1 P1 110.15(9) . . ? C1 Fe1 P1 97.29(9) . . ? C3 Fe1 P1 148.21(9) . . ? C5 Fe1 P1 118.77(9) . . ? C4 Fe1 P1 158.08(8) . . ? P2 Fe1 P1 85.70(4) . . ? C19 P1 C13 100.91(14) . . ? C19 P1 C11 104.69(15) . . ? C13 P1 C11 101.10(15) . . ? C19 P1 Fe1 118.63(11) . . ? C13 P1 Fe1 121.66(11) . . ? C11 P1 Fe1 107.45(10) . . ? C25 P2 C31 99.21(14) . . ? C25 P2 C12 102.77(15) . . ? C31 P2 C12 102.85(15) . . ? C25 P2 Fe1 120.37(11) . . ? C31 P2 Fe1 119.34(11) . . ? C12 P2 Fe1 109.81(11) . . ? C5 C1 C2 108.8(3) . . ? C5 C1 C6 126.5(3) . . ? C2 C1 C6 124.0(3) . . ? C5 C1 Fe1 71.43(18) . . ? C2 C1 Fe1 69.34(17) . . ? C6 C1 Fe1 132.7(2) . . ? C1 C2 C3 107.3(3) . . ? C1 C2 C7 127.7(3) . . ? C3 C2 C7 124.8(3) . . ? C1 C2 Fe1 70.97(18) . . ? C3 C2 Fe1 71.57(19) . . ? C7 C2 Fe1 127.2(2) . . ? C4 C3 C2 108.4(3) . . ? C4 C3 C8 127.3(3) . . ? C2 C3 C8 124.2(3) . . ? C4 C3 Fe1 71.05(18) . . ? C2 C3 Fe1 68.61(18) . . ? C8 C3 Fe1 129.2(2) . . ? C3 C4 C5 108.1(3) . . ? C3 C4 C9 127.6(3) . . ? C5 C4 C9 123.7(3) . . ? C3 C4 Fe1 70.21(18) . . ? C5 C4 Fe1 70.22(17) . . ? C9 C4 Fe1 132.1(2) . . ? C1 C5 C4 107.4(3) . . ? C1 C5 C10 128.4(3) . . ? C4 C5 C10 123.3(3) . . ? C1 C5 Fe1 69.45(17) . . ? C4 C5 Fe1 70.44(17) . . ? C10 C5 Fe1 133.6(2) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 P1 109.5(2) . . ? C12 C11 H11A 109.8 . . ? P1 C11 H11A 109.8 . . ? C12 C11 H11B 109.8 . . ? P1 C11 H11B 109.8 . . ? H11A C11 H11B 108.2 . . ? C11 C12 P2 112.5(2) . . ? C11 C12 H12A 109.1 . . ? P2 C12 H12A 109.1 . . ? C11 C12 H12B 109.1 . . ? P2 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? C14 C13 C18 118.0(3) . . ? C14 C13 P1 120.3(3) . . ? C18 C13 P1 121.6(3) . . ? C13 C14 C15 121.9(3) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C16 C15 C14 119.1(3) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 C15 119.9(3) . . ? C17 C16 H16 120 . . ? C15 C16 H16 120 . . ? C16 C17 C18 120.4(4) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 120.6(3) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? C24 C19 C20 117.6(3) . . ? C24 C19 P1 121.0(2) . . ? C20 C19 P1 121.2(2) . . ? C21 C20 C19 120.5(3) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C22 C21 C20 121.1(3) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 118.8(3) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C24 C23 C22 120.9(3) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C19 121.0(3) . . ? C23 C24 H24 119.5 . . ? C19 C24 H24 119.5 . . ? C30 C25 C26 117.3(3) . . ? C30 C25 P2 120.9(2) . . ? C26 C25 P2 121.6(2) . . ? C27 C26 C25 121.8(3) . . ? C27 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? C28 C27 C26 119.8(3) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C29 C28 C27 119.2(3) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C30 C29 C28 120.7(3) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C25 121.1(3) . . ? C29 C30 H30 119.5 . . ? C25 C30 H30 119.5 . . ? C32 C31 C36 118.8(3) . . ? C32 C31 P2 121.1(3) . . ? C36 C31 P2 120.1(2) . . ? C31 C32 C33 120.6(3) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C34 C33 C32 120.3(3) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 119.9(3) . . ? C33 C34 H34 120 . . ? C35 C34 H34 120 . . ? C34 C35 C36 119.4(3) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C31 C36 C35 121.0(3) . . ? C31 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C38 C37 Fe1 177.1(3) . . ? C37 C38 C39 177.2(3) . . ? C40 C39 C42 117.8(3) . . ? C40 C39 C38 122.5(3) . . ? C42 C39 C38 119.6(3) . . ? C41 C40 C39 121.1(3) . . ? C41 C40 H40 119.4 . . ? C39 C40 H40 119.4 . . ? C40 C41 C44 121.1(3) . . ? C40 C41 H41 119.4 . . ? C44 C41 H41 119.4 . . ? C43 C42 C39 120.5(3) . . ? C43 C42 H42 119.7 . . ? C39 C42 H42 119.7 . . ? C42 C43 C44 121.3(3) . . ? C42 C43 H43 119.3 . . ? C44 C43 H43 119.3 . . ? C41 C44 C43 118.0(3) . . ? C41 C44 P5 124.4(2) . . ? C43 C44 P5 117.6(2) . . ? C50 C45 C46 118.6(3) . . ? C50 C45 P5 117.0(3) . . ? C46 C45 P5 124.3(3) . . ? C47 C46 C45 120.5(4) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C48 C47 C46 120.1(4) . . ? C48 C47 H47 119.9 . . ? C46 C47 H47 119.9 . . ? C49 C48 C47 119.7(4) . . ? C49 C48 H48 120.2 . . ? C47 C48 H48 120.2 . . ? C50 C49 C48 120.3(4) . . ? C50 C49 H49 119.9 . . ? C48 C49 H49 119.9 . . ? C45 P5 C51 103.94(17) . . ? C45 P5 C44 100.20(14) . . ? C51 P5 C44 102.12(15) . . ? C49 C50 C45 120.8(4) . . ? C49 C50 H50 119.6 . . ? C45 C50 H50 119.6 . . ? C52 C51 C56 117.8(4) . . ? C52 C51 P5 118.7(3) . . ? C56 C51 P5 123.4(3) . . ? C53 C52 C51 121.3(4) . . ? C53 C52 H52 119.4 . . ? C51 C52 H52 119.4 . . ? C52 C53 C54 120.3(3) . . ? C52 C53 H53 119.9 . . ? C54 C53 H53 119.9 . . ? C55 C54 C53 120.3(4) . . ? C55 C54 H54 119.9 . . ? C53 C54 H54 119.9 . . ? C54 C55 C56 119.2(4) . . ? C54 C55 H55 120.4 . . ? C56 C55 H55 120.4 . . ? C55 C56 C51 121.2(3) . . ? C55 C56 H56 119.4 . . ? C51 C56 H56 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 C37 Fe1 P1 C19 -68.54(16) . . . . ? C2 Fe1 P1 C19 25.91(15) . . . . ? C1 Fe1 P1 C19 64.71(15) . . . . ? C3 Fe1 P1 C19 9.9(2) . . . . ? C5 Fe1 P1 C19 99.41(16) . . . . ? C4 Fe1 P1 C19 102.4(3) . . . . ? P2 Fe1 P1 C19 -151.89(12) . . . . ? C37 Fe1 P1 C13 165.32(16) . . . . ? C2 Fe1 P1 C13 -100.24(15) . . . . ? C1 Fe1 P1 C13 -61.44(15) . . . . ? C3 Fe1 P1 C13 -116.3(2) . . . . ? C5 Fe1 P1 C13 -26.74(17) . . . . ? C4 Fe1 P1 C13 -23.8(3) . . . . ? P2 Fe1 P1 C13 81.97(13) . . . . ? C37 Fe1 P1 C11 49.79(14) . . . . ? C2 Fe1 P1 C11 144.23(14) . . . . ? C1 Fe1 P1 C11 -176.97(13) . . . . ? C3 Fe1 P1 C11 128.18(19) . . . . ? C5 Fe1 P1 C11 -142.27(14) . . . . ? C4 Fe1 P1 C11 -139.3(3) . . . . ? P2 Fe1 P1 C11 -33.56(11) . . . . ? C37 Fe1 P2 C25 177.32(15) . . . . ? C2 Fe1 P2 C25 89.9(3) . . . . ? C1 Fe1 P2 C25 -1.1(2) . . . . ? C3 Fe1 P2 C25 93.92(16) . . . . ? C5 Fe1 P2 C25 21.34(15) . . . . ? C4 Fe1 P2 C25 61.02(14) . . . . ? P1 Fe1 P2 C25 -97.59(12) . . . . ? C37 Fe1 P2 C31 54.50(15) . . . . ? C2 Fe1 P2 C31 -32.9(3) . . . . ? C1 Fe1 P2 C31 -123.97(18) . . . . ? C3 Fe1 P2 C31 -28.90(15) . . . . ? C5 Fe1 P2 C31 -101.49(14) . . . . ? C4 Fe1 P2 C31 -61.80(14) . . . . ? P1 Fe1 P2 C31 139.58(11) . . . . ? C37 Fe1 P2 C12 -63.77(14) . . . . ? C2 Fe1 P2 C12 -151.2(3) . . . . ? C1 Fe1 P2 C12 117.76(18) . . . . ? C3 Fe1 P2 C12 -147.17(15) . . . . ? C5 Fe1 P2 C12 140.25(14) . . . . ? C4 Fe1 P2 C12 179.93(13) . . . . ? P1 Fe1 P2 C12 21.31(11) . . . . ? C37 Fe1 C1 C5 -142.80(19) . . . . ? C2 Fe1 C1 C5 -119.3(3) . . . . ? C3 Fe1 C1 C5 -80.43(19) . . . . ? C4 Fe1 C1 C5 -37.79(17) . . . . ? P2 Fe1 C1 C5 35.1(2) . . . . ? P1 Fe1 C1 C5 127.73(17) . . . . ? C37 Fe1 C1 C2 -23.5(3) . . . . ? C3 Fe1 C1 C2 38.91(18) . . . . ? C5 Fe1 C1 C2 119.3(3) . . . . ? C4 Fe1 C1 C2 81.55(19) . . . . ? P2 Fe1 C1 C2 154.44(15) . . . . ? P1 Fe1 C1 C2 -112.94(17) . . . . ? C37 Fe1 C1 C6 94.2(3) . . . . ? C2 Fe1 C1 C6 117.7(4) . . . . ? C3 Fe1 C1 C6 156.6(3) . . . . ? C5 Fe1 C1 C6 -123.0(4) . . . . ? C4 Fe1 C1 C6 -160.8(3) . . . . ? P2 Fe1 C1 C6 -87.9(3) . . . . ? P1 Fe1 C1 C6 4.7(3) . . . . ? C5 C1 C2 C3 -2.0(4) . . . . ? C6 C1 C2 C3 168.9(3) . . . . ? Fe1 C1 C2 C3 -62.8(2) . . . . ? C5 C1 C2 C7 -176.4(3) . . . . ? C6 C1 C2 C7 -5.5(5) . . . . ? Fe1 C1 C2 C7 122.8(3) . . . . ? C5 C1 C2 Fe1 60.8(2) . . . . ? C6 C1 C2 Fe1 -128.3(3) . . . . ? C37 Fe1 C2 C1 163.12(18) . . . . ? C3 Fe1 C2 C1 -116.5(2) . . . . ? C5 Fe1 C2 C1 -36.87(17) . . . . ? C4 Fe1 C2 C1 -79.98(18) . . . . ? P2 Fe1 C2 C1 -111.3(3) . . . . ? P1 Fe1 C2 C1 76.67(17) . . . . ? C37 Fe1 C2 C3 -80.40(18) . . . . ? C1 Fe1 C2 C3 116.5(2) . . . . ? C5 Fe1 C2 C3 79.61(18) . . . . ? C4 Fe1 C2 C3 36.50(16) . . . . ? P2 Fe1 C2 C3 5.2(4) . . . . ? P1 Fe1 C2 C3 -166.85(15) . . . . ? C37 Fe1 C2 C7 39.7(3) . . . . ? C1 Fe1 C2 C7 -123.4(4) . . . . ? C3 Fe1 C2 C7 120.1(3) . . . . ? C5 Fe1 C2 C7 -160.2(3) . . . . ? C4 Fe1 C2 C7 156.6(3) . . . . ? P2 Fe1 C2 C7 125.3(3) . . . . ? P1 Fe1 C2 C7 -46.7(3) . . . . ? C1 C2 C3 C4 2.2(4) . . . . ? C7 C2 C3 C4 176.8(3) . . . . ? Fe1 C2 C3 C4 -60.2(2) . . . . ? C1 C2 C3 C8 -173.9(3) . . . . ? C7 C2 C3 C8 0.7(5) . . . . ? Fe1 C2 C3 C8 123.7(3) . . . . ? C1 C2 C3 Fe1 62.4(2) . . . . ? C7 C2 C3 Fe1 -123.0(3) . . . . ? C37 Fe1 C3 C4 -139.3(2) . . . . ? C2 Fe1 C3 C4 119.5(3) . . . . ? C1 Fe1 C3 C4 80.71(19) . . . . ? C5 Fe1 C3 C4 37.63(18) . . . . ? P2 Fe1 C3 C4 -58.8(2) . . . . ? P1 Fe1 C3 C4 143.42(17) . . . . ? C37 Fe1 C3 C2 101.22(18) . . . . ? C1 Fe1 C3 C2 -38.79(17) . . . . ? C5 Fe1 C3 C2 -81.87(18) . . . . ? C4 Fe1 C3 C2 -119.5(3) . . . . ? P2 Fe1 C3 C2 -178.28(14) . . . . ? P1 Fe1 C3 C2 23.9(3) . . . . ? C37 Fe1 C3 C8 -16.2(3) . . . . ? C2 Fe1 C3 C8 -117.4(4) . . . . ? C1 Fe1 C3 C8 -156.2(3) . . . . ? C5 Fe1 C3 C8 160.7(3) . . . . ? C4 Fe1 C3 C8 123.1(4) . . . . ? P2 Fe1 C3 C8 64.3(3) . . . . ? P1 Fe1 C3 C8 -93.5(3) . . . . ? C2 C3 C4 C5 -1.6(4) . . . . ? C8 C3 C4 C5 174.3(3) . . . . ? Fe1 C3 C4 C5 -60.3(2) . . . . ? C2 C3 C4 C9 -172.9(3) . . . . ? C8 C3 C4 C9 3.1(6) . . . . ? Fe1 C3 C4 C9 128.5(3) . . . . ? C2 C3 C4 Fe1 58.6(2) . . . . ? C8 C3 C4 Fe1 -125.4(3) . . . . ? C37 Fe1 C4 C3 47.0(2) . . . . ? C2 Fe1 C4 C3 -37.49(18) . . . . ? C1 Fe1 C4 C3 -81.1(2) . . . . ? C5 Fe1 C4 C3 -118.7(3) . . . . ? P2 Fe1 C4 C3 134.14(17) . . . . ? P1 Fe1 C4 C3 -122.8(2) . . . . ? C37 Fe1 C4 C5 165.74(18) . . . . ? C2 Fe1 C4 C5 81.20(19) . . . . ? C1 Fe1 C4 C5 37.57(18) . . . . ? C3 Fe1 C4 C5 118.7(3) . . . . ? P2 Fe1 C4 C5 -107.17(17) . . . . ? P1 Fe1 C4 C5 -4.1(3) . . . . ? C37 Fe1 C4 C9 -76.2(3) . . . . ? C2 Fe1 C4 C9 -160.7(3) . . . . ? C1 Fe1 C4 C9 155.7(3) . . . . ? C3 Fe1 C4 C9 -123.2(4) . . . . ? C5 Fe1 C4 C9 118.1(4) . . . . ? P2 Fe1 C4 C9 10.9(3) . . . . ? P1 Fe1 C4 C9 114.0(3) . . . . ? C2 C1 C5 C4 1.0(4) . . . . ? C6 C1 C5 C4 -169.6(3) . . . . ? Fe1 C1 C5 C4 60.5(2) . . . . ? C2 C1 C5 C10 170.5(3) . . . . ? C6 C1 C5 C10 -0.1(6) . . . . ? Fe1 C1 C5 C10 -130.0(4) . . . . ? C2 C1 C5 Fe1 -59.5(2) . . . . ? C6 C1 C5 Fe1 129.9(3) . . . . ? C3 C4 C5 C1 0.4(4) . . . . ? C9 C4 C5 C1 172.1(3) . . . . ? Fe1 C4 C5 C1 -59.9(2) . . . . ? C3 C4 C5 C10 -169.8(3) . . . . ? C9 C4 C5 C10 1.9(5) . . . . ? Fe1 C4 C5 C10 130.0(3) . . . . ? C3 C4 C5 Fe1 60.3(2) . . . . ? C9 C4 C5 Fe1 -128.1(3) . . . . ? C37 Fe1 C5 C1 88.2(3) . . . . ? C2 Fe1 C5 C1 37.40(18) . . . . ? C3 Fe1 C5 C1 81.2(2) . . . . ? C4 Fe1 C5 C1 118.2(3) . . . . ? P2 Fe1 C5 C1 -158.85(16) . . . . ? P1 Fe1 C5 C1 -63.52(19) . . . . ? C37 Fe1 C5 C4 -30.0(4) . . . . ? C2 Fe1 C5 C4 -80.82(19) . . . . ? C1 Fe1 C5 C4 -118.2(3) . . . . ? C3 Fe1 C5 C4 -37.07(18) . . . . ? P2 Fe1 C5 C4 82.93(18) . . . . ? P1 Fe1 C5 C4 178.26(15) . . . . ? C37 Fe1 C5 C10 -147.8(3) . . . . ? C2 Fe1 C5 C10 161.4(3) . . . . ? C1 Fe1 C5 C10 124.0(4) . . . . ? C3 Fe1 C5 C10 -154.8(3) . . . . ? C4 Fe1 C5 C10 -117.7(4) . . . . ? P2 Fe1 C5 C10 -34.8(3) . . . . ? P1 Fe1 C5 C10 60.5(3) . . . . ? C19 P1 C11 C12 167.9(2) . . . . ? C13 P1 C11 C12 -87.5(2) . . . . ? Fe1 P1 C11 C12 41.0(2) . . . . ? P1 C11 C12 P2 -24.2(3) . . . . ? C25 P2 C12 C11 127.6(2) . . . . ? C31 P2 C12 C11 -129.7(2) . . . . ? Fe1 P2 C12 C11 -1.6(2) . . . . ? C19 P1 C13 C14 -128.9(3) . . . . ? C11 P1 C13 C14 123.6(3) . . . . ? Fe1 P1 C13 C14 4.9(3) . . . . ? C19 P1 C13 C18 54.6(3) . . . . ? C11 P1 C13 C18 -52.9(3) . . . . ? Fe1 P1 C13 C18 -171.6(2) . . . . ? C18 C13 C14 C15 -0.3(5) . . . . ? P1 C13 C14 C15 -176.9(3) . . . . ? C13 C14 C15 C16 1.6(5) . . . . ? C14 C15 C16 C17 -1.5(5) . . . . ? C15 C16 C17 C18 0.2(5) . . . . ? C16 C17 C18 C13 1.2(5) . . . . ? C14 C13 C18 C17 -1.1(5) . . . . ? P1 C13 C18 C17 175.4(3) . . . . ? C13 P1 C19 C24 -157.0(3) . . . . ? C11 P1 C19 C24 -52.3(3) . . . . ? Fe1 P1 C19 C24 67.5(3) . . . . ? C13 P1 C19 C20 27.4(3) . . . . ? C11 P1 C19 C20 132.1(3) . . . . ? Fe1 P1 C19 C20 -108.2(3) . . . . ? C24 C19 C20 C21 1.4(5) . . . . ? P1 C19 C20 C21 177.2(3) . . . . ? C19 C20 C21 C22 -0.1(6) . . . . ? C20 C21 C22 C23 -0.5(6) . . . . ? C21 C22 C23 C24 -0.3(6) . . . . ? C22 C23 C24 C19 1.8(6) . . . . ? C20 C19 C24 C23 -2.3(5) . . . . ? P1 C19 C24 C23 -178.1(3) . . . . ? C31 P2 C25 C30 -150.5(3) . . . . ? C12 P2 C25 C30 -45.0(3) . . . . ? Fe1 P2 C25 C30 77.4(3) . . . . ? C31 P2 C25 C26 33.9(3) . . . . ? C12 P2 C25 C26 139.5(3) . . . . ? Fe1 P2 C25 C26 -98.1(3) . . . . ? C30 C25 C26 C27 0.6(5) . . . . ? P2 C25 C26 C27 176.3(3) . . . . ? C25 C26 C27 C28 0.0(6) . . . . ? C26 C27 C28 C29 -1.1(6) . . . . ? C27 C28 C29 C30 1.5(6) . . . . ? C28 C29 C30 C25 -0.9(6) . . . . ? C26 C25 C30 C29 -0.1(5) . . . . ? P2 C25 C30 C29 -175.9(3) . . . . ? C25 P2 C31 C32 -131.4(3) . . . . ? C12 P2 C31 C32 123.2(3) . . . . ? Fe1 P2 C31 C32 1.4(3) . . . . ? C25 P2 C31 C36 48.4(3) . . . . ? C12 P2 C31 C36 -57.0(3) . . . . ? Fe1 P2 C31 C36 -178.8(2) . . . . ? C36 C31 C32 C33 -0.6(5) . . . . ? P2 C31 C32 C33 179.2(2) . . . . ? C31 C32 C33 C34 0.3(5) . . . . ? C32 C33 C34 C35 0.2(5) . . . . ? C33 C34 C35 C36 -0.4(5) . . . . ? C32 C31 C36 C35 0.5(5) . . . . ? P2 C31 C36 C35 -179.3(2) . . . . ? C34 C35 C36 C31 0.0(5) . . . . ? C42 C39 C40 C41 -1.4(5) . . . . ? C38 C39 C40 C41 176.7(3) . . . . ? C39 C40 C41 C44 -0.6(5) . . . . ? C40 C39 C42 C43 2.8(5) . . . . ? C38 C39 C42 C43 -175.4(3) . . . . ? C39 C42 C43 C44 -2.1(5) . . . . ? C40 C41 C44 C43 1.3(5) . . . . ? C40 C41 C44 P5 -176.9(3) . . . . ? C42 C43 C44 C41 0.0(5) . . . . ? C42 C43 C44 P5 178.4(3) . . . . ? C50 C45 C46 C47 -1.6(5) . . . . ? P5 C45 C46 C47 174.8(3) . . . . ? C45 C46 C47 C48 -0.3(5) . . . . ? C46 C47 C48 C49 1.0(6) . . . . ? C47 C48 C49 C50 0.3(6) . . . . ? C50 C45 P5 C51 -174.3(3) . . . . ? C46 C45 P5 C51 9.2(3) . . . . ? C50 C45 P5 C44 80.3(3) . . . . ? C46 C45 P5 C44 -96.1(3) . . . . ? C41 C44 P5 C45 5.4(3) . . . . ? C43 C44 P5 C45 -172.8(3) . . . . ? C41 C44 P5 C51 -101.4(3) . . . . ? C43 C44 P5 C51 80.4(3) . . . . ? C48 C49 C50 C45 -2.3(6) . . . . ? C46 C45 C50 C49 3.0(5) . . . . ? P5 C45 C50 C49 -173.7(3) . . . . ? C45 P5 C51 C52 78.6(3) . . . . ? C44 P5 C51 C52 -177.5(3) . . . . ? C45 P5 C51 C56 -105.4(3) . . . . ? C44 P5 C51 C56 -1.5(3) . . . . ? C56 C51 C52 C53 -0.4(5) . . . . ? P5 C51 C52 C53 175.8(3) . . . . ? C51 C52 C53 C54 -0.5(6) . . . . ? C52 C53 C54 C55 0.4(6) . . . . ? C53 C54 C55 C56 0.5(6) . . . . ? C54 C55 C56 C51 -1.4(5) . . . . ? C52 C51 C56 C55 1.3(5) . . . . ? P5 C51 C56 C55 -174.7(3) . . . . ? # Attachment 'metaPPh2.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-03-04 at 09:47:20 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\progs\wingx\files\archive.dat # CIF files read : job struct data_metaPPh2 _database_code_depnum_ccdc_archive 'CCDC 755887' #TrackingRef 'metaPPh2.cif' _audit_creation_date 2009-03-04T09:47:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C56 H53 Fe1 P3' _chemical_formula_sum 'C56 H53 Fe P3' _chemical_formula_weight 874.74 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 12.2780(4) _cell_length_b 21.9742(10) _cell_length_c 16.8487(7) _cell_angle_alpha 90 _cell_angle_beta 103.994(2) _cell_angle_gamma 90 _cell_volume 4410.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5799 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.51 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.489 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.858 _exptl_absorpt_correction_T_max 0.966 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0875 _diffrn_reflns_av_unetI/netI 0.0758 _diffrn_reflns_number 46370 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 10013 _reflns_number_gt 7719 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SAINT' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0311P)^2^+2.7244P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10013 _refine_ls_number_parameters 546 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0943 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.392 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.077 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.02587(3) 0.178955(15) 0.62043(2) 0.00853(9) Uani 1 d . . . P1 P 0.15405(5) 0.10800(3) 0.65329(4) 0.00962(13) Uani 1 d . . . P2 P 0.01578(5) 0.15370(3) 0.49360(4) 0.00914(13) Uani 1 d . . . C1 C 0.00531(19) 0.21945(11) 0.72846(15) 0.0130(5) Uani 1 d . . . C2 C -0.08785(18) 0.23637(11) 0.66300(15) 0.0125(5) Uani 1 d . . . C3 C -0.04678(18) 0.26828(10) 0.60280(15) 0.0114(5) Uani 1 d . . . C4 C 0.07419(18) 0.27199(11) 0.63189(15) 0.0120(5) Uani 1 d . . . C5 C 0.10515(18) 0.24267(11) 0.70928(15) 0.0121(5) Uani 1 d . . . C6 C -0.0034(2) 0.18834(12) 0.80610(16) 0.0199(6) Uani 1 d . . . H6A H -0.0172 0.2188 0.8451 0.03 Uiso 1 calc R . . H6B H 0.0668 0.1668 0.8298 0.03 Uiso 1 calc R . . H6C H -0.0656 0.1592 0.794 0.03 Uiso 1 calc R . . C7 C -0.20954(18) 0.22619(11) 0.66153(16) 0.0161(5) Uani 1 d . . . H7A H -0.231 0.2527 0.702 0.024 Uiso 1 calc R . . H7B H -0.2209 0.1836 0.6746 0.024 Uiso 1 calc R . . H7C H -0.2559 0.2357 0.607 0.024 Uiso 1 calc R . . C8 C -0.11640(19) 0.30135(11) 0.53034(15) 0.0156(5) Uani 1 d . . . H8A H -0.1793 0.2755 0.5028 0.023 Uiso 1 calc R . . H8B H -0.07 0.3112 0.4922 0.023 Uiso 1 calc R . . H8C H -0.1455 0.339 0.5486 0.023 Uiso 1 calc R . . C9 C 0.14929(19) 0.30961(11) 0.59269(16) 0.0171(5) Uani 1 d . . . H9A H 0.1358 0.3529 0.6004 0.026 Uiso 1 calc R . . H9B H 0.1331 0.3005 0.5341 0.026 Uiso 1 calc R . . H9C H 0.2279 0.2999 0.618 0.026 Uiso 1 calc R . . C10 C 0.21970(18) 0.24212(12) 0.76578(15) 0.0164(5) Uani 1 d . . . H10A H 0.2758 0.2342 0.7344 0.025 Uiso 1 calc R . . H10B H 0.2236 0.2101 0.8069 0.025 Uiso 1 calc R . . H10C H 0.2348 0.2817 0.7931 0.025 Uiso 1 calc R . . C11 C 0.11648(18) 0.04901(11) 0.57285(14) 0.0118(5) Uani 1 d . . . H11A H 0.1783 0.0192 0.578 0.014 Uiso 1 calc R . . H11B H 0.048 0.027 0.5776 0.014 Uiso 1 calc R . . C12 C 0.09599(19) 0.08219(11) 0.49055(15) 0.0130(5) Uani 1 d . . . H12A H 0.0534 0.0554 0.4466 0.016 Uiso 1 calc R . . H12B H 0.1688 0.0919 0.4781 0.016 Uiso 1 calc R . . C13 C 0.16411(18) 0.06851(11) 0.75094(15) 0.0117(5) Uani 1 d . . . C14 C 0.24533(18) 0.08460(11) 0.82153(15) 0.0134(5) Uani 1 d . . . H14 H 0.302 0.1131 0.8177 0.016 Uiso 1 calc R . . C15 C 0.24448(19) 0.05951(12) 0.89728(15) 0.0162(5) Uani 1 d . . . H15 H 0.2995 0.0716 0.9447 0.019 Uiso 1 calc R . . C16 C 0.1634(2) 0.01693(12) 0.90377(16) 0.0182(6) Uani 1 d . . . H16 H 0.1629 -0.0003 0.9554 0.022 Uiso 1 calc R . . C17 C 0.0832(2) -0.00017(12) 0.83429(15) 0.0174(5) Uani 1 d . . . H17 H 0.0279 -0.0295 0.8382 0.021 Uiso 1 calc R . . C18 C 0.08339(19) 0.02552(11) 0.75886(15) 0.0132(5) Uani 1 d . . . H18 H 0.0276 0.0136 0.7118 0.016 Uiso 1 calc R . . C19 C 0.30453(18) 0.11720(11) 0.65399(14) 0.0112(5) Uani 1 d . . . C20 C 0.34199(18) 0.16889(11) 0.62103(14) 0.0126(5) Uani 1 d . . . H20 H 0.2919 0.2019 0.6037 0.015 Uiso 1 calc R . . C21 C 0.45270(19) 0.17284(12) 0.61314(16) 0.0174(5) Uani 1 d . . . H21 H 0.477 0.2081 0.5897 0.021 Uiso 1 calc R . . C22 C 0.52694(19) 0.12528(12) 0.63945(15) 0.0160(5) Uani 1 d . . . H22 H 0.602 0.1279 0.6341 0.019 Uiso 1 calc R . . C23 C 0.49119(19) 0.07370(12) 0.67371(15) 0.0158(5) Uani 1 d . . . H23 H 0.5422 0.0413 0.6925 0.019 Uiso 1 calc R . . C24 C 0.38070(18) 0.06941(11) 0.68058(15) 0.0131(5) Uani 1 d . . . H24 H 0.3566 0.0338 0.7035 0.016 Uiso 1 calc R . . C25 C 0.07180(18) 0.20463(11) 0.42567(14) 0.0108(5) Uani 1 d . . . C26 C 0.00027(19) 0.24660(11) 0.37609(14) 0.0132(5) Uani 1 d . . . H26 H -0.0779 0.2455 0.3734 0.016 Uiso 1 calc R . . C27 C 0.0421(2) 0.28993(12) 0.33069(15) 0.0175(5) Uani 1 d . . . H27 H -0.0073 0.3184 0.2979 0.021 Uiso 1 calc R . . C28 C 0.1556(2) 0.29148(12) 0.33343(16) 0.0182(6) Uani 1 d . . . H28 H 0.1843 0.3211 0.3029 0.022 Uiso 1 calc R . . C29 C 0.2272(2) 0.24965(12) 0.38089(16) 0.0182(6) Uani 1 d . . . H29 H 0.3049 0.2503 0.382 0.022 Uiso 1 calc R . . C30 C 0.18622(19) 0.20680(12) 0.42687(15) 0.0151(5) Uani 1 d . . . H30 H 0.2364 0.1786 0.4595 0.018 Uiso 1 calc R . . C31 C -0.12418(18) 0.13665(11) 0.42685(15) 0.0120(5) Uani 1 d . . . C32 C -0.22004(18) 0.15238(11) 0.45304(15) 0.0140(5) Uani 1 d . . . H32 H -0.2125 0.1729 0.5037 0.017 Uiso 1 calc R . . C33 C -0.32648(19) 0.13833(12) 0.40564(16) 0.0193(6) Uani 1 d . . . H33 H -0.3911 0.1495 0.4239 0.023 Uiso 1 calc R . . C34 C -0.3384(2) 0.10816(12) 0.33218(16) 0.0210(6) Uani 1 d . . . H34 H -0.4111 0.0976 0.3007 0.025 Uiso 1 calc R . . C35 C -0.2442(2) 0.09327(12) 0.30420(16) 0.0189(6) Uani 1 d . . . H35 H -0.2525 0.0732 0.2531 0.023 Uiso 1 calc R . . C36 C -0.13742(19) 0.10778(11) 0.35102(15) 0.0149(5) Uani 1 d . . . H36 H -0.0732 0.098 0.3314 0.018 Uiso 1 calc R . . C37 C -0.07582(18) 0.11374(11) 0.62235(14) 0.0112(5) Uani 1 d . . . C38 C -0.14370(18) 0.07325(11) 0.62317(15) 0.0124(5) Uani 1 d . . . C39 C -0.22011(18) 0.02332(11) 0.62159(15) 0.0112(5) Uani 1 d . . . P4 P -0.29801(5) -0.10670(3) 0.78030(4) 0.01414(14) Uani 1 d . . . C40 C -0.21429(18) -0.01326(11) 0.69093(15) 0.0118(5) Uani 1 d . . . H40 H -0.1593 -0.0044 0.7398 0.014 Uiso 1 calc R . . C41 C -0.30258(18) 0.00890(11) 0.54978(15) 0.0125(5) Uani 1 d . . . H41 H -0.3097 0.0333 0.5023 0.015 Uiso 1 calc R . . C42 C -0.37330(19) -0.04065(11) 0.54813(15) 0.0142(5) Uani 1 d . . . H42 H -0.4274 -0.0503 0.4991 0.017 Uiso 1 calc R . . C43 C -0.36573(18) -0.07617(11) 0.61733(15) 0.0148(5) Uani 1 d . . . H43 H -0.4142 -0.1101 0.6153 0.018 Uiso 1 calc R . . C44 C -0.28720(18) -0.06232(11) 0.69002(15) 0.0123(5) Uani 1 d . . . C45 C -0.15154(19) -0.11851(11) 0.83664(15) 0.0139(5) Uani 1 d . . . C46 C -0.07609(19) -0.14521(11) 0.79608(15) 0.0155(5) Uani 1 d . . . H46 H -0.0985 -0.1518 0.7387 0.019 Uiso 1 calc R . . C47 C 0.0302(2) -0.16193(12) 0.83894(17) 0.0206(6) Uani 1 d . . . H47 H 0.0806 -0.1798 0.8108 0.025 Uiso 1 calc R . . C48 C 0.0644(2) -0.15288(12) 0.92320(17) 0.0223(6) Uani 1 d . . . H48 H 0.1378 -0.1642 0.9524 0.027 Uiso 1 calc R . . C49 C -0.0097(2) -0.12726(13) 0.96396(16) 0.0215(6) Uani 1 d . . . H49 H 0.0127 -0.1212 1.0214 0.026 Uiso 1 calc R . . C50 C -0.1170(2) -0.11036(12) 0.92071(16) 0.0183(6) Uani 1 d . . . H50 H -0.1673 -0.093 0.9492 0.022 Uiso 1 calc R . . C51 C -0.34687(19) -0.04705(12) 0.83994(15) 0.0161(5) Uani 1 d . . . C52 C -0.2901(2) 0.00727(12) 0.86656(16) 0.0203(6) Uani 1 d . . . H52 H -0.217 0.0137 0.8585 0.024 Uiso 1 calc R . . C53 C -0.3396(2) 0.05192(13) 0.90466(17) 0.0265(6) Uani 1 d . . . H53 H -0.3003 0.0886 0.9225 0.032 Uiso 1 calc R . . C54 C -0.4466(2) 0.04307(15) 0.91681(17) 0.0306(7) Uani 1 d . . . H54 H -0.4812 0.074 0.9417 0.037 Uiso 1 calc R . . C55 C -0.5021(2) -0.01089(15) 0.89253(17) 0.0292(7) Uani 1 d . . . H55 H -0.5746 -0.0174 0.9018 0.035 Uiso 1 calc R . . C56 C -0.4534(2) -0.05542(13) 0.85501(16) 0.0219(6) Uani 1 d . . . H56 H -0.4925 -0.0924 0.8391 0.026 Uiso 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 0.00744(16) 0.00818(17) 0.01021(18) -0.00041(13) 0.00261(13) -0.00010(12) P1 0.0083(3) 0.0093(3) 0.0111(3) -0.0003(2) 0.0020(2) 0.0001(2) P2 0.0084(3) 0.0090(3) 0.0099(3) 0.0006(2) 0.0019(2) -0.0003(2) C1 0.0159(12) 0.0120(13) 0.0121(13) -0.0036(10) 0.0057(10) 0.0000(9) C2 0.0125(11) 0.0098(12) 0.0157(13) -0.0026(10) 0.0048(10) 0.0010(9) C3 0.0131(11) 0.0061(12) 0.0154(13) -0.0011(9) 0.0041(10) 0.0012(9) C4 0.0119(11) 0.0070(12) 0.0182(14) -0.0037(10) 0.0060(10) -0.0010(9) C5 0.0124(11) 0.0089(12) 0.0148(13) -0.0045(10) 0.0030(10) 0.0004(9) C6 0.0211(13) 0.0238(15) 0.0170(14) -0.0008(11) 0.0087(11) 0.0030(11) C7 0.0130(12) 0.0126(13) 0.0256(15) -0.0019(11) 0.0106(11) -0.0005(9) C8 0.0151(12) 0.0123(13) 0.0184(14) 0.0011(10) 0.0023(10) 0.0029(9) C9 0.0153(12) 0.0129(13) 0.0245(15) 0.0000(11) 0.0075(11) -0.0013(9) C10 0.0143(12) 0.0164(14) 0.0165(14) -0.0051(11) 0.0001(10) -0.0008(10) C11 0.0099(11) 0.0090(12) 0.0156(13) -0.0010(10) 0.0017(9) 0.0014(9) C12 0.0121(11) 0.0118(13) 0.0152(13) -0.0018(10) 0.0036(10) 0.0001(9) C13 0.0136(11) 0.0082(12) 0.0139(13) -0.0006(10) 0.0044(9) 0.0036(9) C14 0.0099(11) 0.0136(13) 0.0167(14) -0.0011(10) 0.0034(10) 0.0014(9) C15 0.0143(12) 0.0216(14) 0.0106(13) -0.0022(11) -0.0010(10) 0.0021(10) C16 0.0225(13) 0.0198(14) 0.0126(14) 0.0032(11) 0.0051(11) 0.0036(10) C17 0.0180(12) 0.0165(14) 0.0182(14) 0.0039(11) 0.0052(11) -0.0012(10) C18 0.0147(12) 0.0115(13) 0.0122(13) 0.0009(10) 0.0010(10) 0.0003(9) C19 0.0103(11) 0.0131(13) 0.0094(12) -0.0016(10) 0.0008(9) 0.0017(9) C20 0.0139(11) 0.0112(13) 0.0120(13) -0.0016(10) 0.0017(10) 0.0019(9) C21 0.0173(12) 0.0176(14) 0.0183(14) -0.0018(11) 0.0064(10) -0.0049(10) C22 0.0078(11) 0.0234(15) 0.0178(14) -0.0082(11) 0.0048(10) -0.0036(9) C23 0.0131(12) 0.0197(14) 0.0131(13) -0.0057(10) 0.0002(10) 0.0047(10) C24 0.0112(11) 0.0139(13) 0.0137(13) 0.0020(10) 0.0022(9) -0.0002(9) C25 0.0119(11) 0.0118(12) 0.0093(12) -0.0017(9) 0.0040(9) -0.0029(9) C26 0.0118(11) 0.0154(13) 0.0122(13) -0.0010(10) 0.0023(10) -0.0003(9) C27 0.0209(13) 0.0179(14) 0.0133(14) 0.0015(11) 0.0036(10) -0.0003(10) C28 0.0260(13) 0.0147(14) 0.0171(14) 0.0009(11) 0.0113(11) -0.0063(10) C29 0.0139(12) 0.0221(14) 0.0212(15) -0.0013(11) 0.0093(11) -0.0033(10) C30 0.0114(11) 0.0191(14) 0.0144(13) -0.0014(10) 0.0024(10) 0.0012(9) C31 0.0129(11) 0.0093(12) 0.0138(13) 0.0034(10) 0.0030(9) -0.0001(9) C32 0.0113(11) 0.0138(13) 0.0156(13) 0.0055(10) 0.0012(10) -0.0021(9) C33 0.0094(12) 0.0254(15) 0.0215(15) 0.0071(12) 0.0004(10) -0.0002(10) C34 0.0149(12) 0.0197(15) 0.0221(15) 0.0046(12) -0.0076(11) -0.0054(10) C35 0.0245(13) 0.0143(14) 0.0133(14) -0.0010(10) -0.0040(11) -0.0028(10) C36 0.0156(12) 0.0125(13) 0.0151(13) 0.0005(10) 0.0006(10) 0.0001(9) C37 0.0104(11) 0.0130(13) 0.0099(12) -0.0012(10) 0.0021(9) 0.0018(9) C38 0.0122(11) 0.0135(13) 0.0119(13) -0.0003(10) 0.0038(9) 0.0011(9) C39 0.0100(11) 0.0097(12) 0.0151(13) -0.0018(10) 0.0054(9) 0.0021(9) P4 0.0128(3) 0.0139(3) 0.0164(4) 0.0027(3) 0.0049(3) -0.0022(2) C40 0.0090(11) 0.0133(13) 0.0127(13) -0.0021(10) 0.0022(9) -0.0005(9) C41 0.0134(11) 0.0126(13) 0.0124(13) 0.0012(10) 0.0047(10) 0.0020(9) C42 0.0113(11) 0.0174(13) 0.0130(13) -0.0025(10) 0.0011(10) 0.0012(9) C43 0.0100(11) 0.0136(13) 0.0216(14) -0.0015(10) 0.0057(10) -0.0040(9) C44 0.0125(11) 0.0116(12) 0.0139(13) 0.0006(10) 0.0053(10) 0.0007(9) C45 0.0147(11) 0.0089(12) 0.0192(14) 0.0034(10) 0.0058(10) 0.0002(9) C46 0.0189(12) 0.0147(13) 0.0128(13) -0.0012(10) 0.0035(10) -0.0010(10) C47 0.0208(13) 0.0192(14) 0.0242(15) -0.0011(11) 0.0101(11) 0.0052(10) C48 0.0156(13) 0.0228(15) 0.0273(16) 0.0041(12) 0.0026(11) 0.0044(11) C49 0.0205(13) 0.0293(16) 0.0132(14) 0.0017(12) 0.0013(11) 0.0033(11) C50 0.0194(13) 0.0203(14) 0.0177(14) 0.0005(11) 0.0093(11) 0.0023(10) C51 0.0163(12) 0.0184(14) 0.0135(13) 0.0059(10) 0.0034(10) 0.0046(10) C52 0.0226(13) 0.0230(15) 0.0172(14) 0.0042(11) 0.0083(11) 0.0058(11) C53 0.0374(16) 0.0229(16) 0.0182(15) 0.0057(12) 0.0050(12) 0.0061(12) C54 0.0362(17) 0.0385(19) 0.0210(16) 0.0028(14) 0.0146(13) 0.0214(14) C55 0.0200(14) 0.046(2) 0.0231(16) 0.0057(14) 0.0079(12) 0.0100(13) C56 0.0162(13) 0.0339(17) 0.0149(14) 0.0067(12) 0.0022(11) 0.0047(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C37 1.906(2) . ? Fe1 C1 2.095(2) . ? Fe1 C5 2.108(2) . ? Fe1 C4 2.124(2) . ? Fe1 C2 2.131(2) . ? Fe1 C3 2.147(2) . ? Fe1 P2 2.1821(7) . ? Fe1 P1 2.1893(7) . ? P1 C13 1.838(2) . ? P1 C11 1.851(2) . ? P1 C19 1.856(2) . ? P2 C25 1.848(2) . ? P2 C31 1.850(2) . ? P2 C12 1.862(2) . ? C1 C2 1.433(3) . ? C1 C5 1.435(3) . ? C1 C6 1.503(3) . ? C2 C3 1.422(3) . ? C2 C7 1.505(3) . ? C3 C4 1.449(3) . ? C3 C8 1.498(3) . ? C4 C5 1.421(3) . ? C4 C9 1.505(3) . ? C5 C10 1.496(3) . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 C12 1.533(3) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C18 1.399(3) . ? C13 C14 1.400(3) . ? C14 C15 1.393(3) . ? C14 H14 0.95 . ? C15 C16 1.390(3) . ? C15 H15 0.95 . ? C16 C17 1.387(4) . ? C16 H16 0.95 . ? C17 C18 1.391(3) . ? C17 H17 0.95 . ? C18 H18 0.95 . ? C19 C20 1.391(3) . ? C19 C24 1.405(3) . ? C20 C21 1.400(3) . ? C20 H20 0.95 . ? C21 C22 1.387(3) . ? C21 H21 0.95 . ? C22 C23 1.390(4) . ? C22 H22 0.95 . ? C23 C24 1.392(3) . ? C23 H23 0.95 . ? C24 H24 0.95 . ? C25 C30 1.401(3) . ? C25 C26 1.402(3) . ? C26 C27 1.395(3) . ? C26 H26 0.95 . ? C27 C28 1.384(3) . ? C27 H27 0.95 . ? C28 C29 1.384(4) . ? C28 H28 0.95 . ? C29 C30 1.388(3) . ? C29 H29 0.95 . ? C30 H30 0.95 . ? C31 C32 1.397(3) . ? C31 C36 1.400(3) . ? C32 C33 1.391(3) . ? C32 H32 0.95 . ? C33 C34 1.380(4) . ? C33 H33 0.95 . ? C34 C35 1.390(4) . ? C34 H34 0.95 . ? C35 C36 1.394(3) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C37 C38 1.221(3) . ? C38 C39 1.440(3) . ? C39 C40 1.406(3) . ? C39 C41 1.413(3) . ? P4 C45 1.838(2) . ? P4 C51 1.838(3) . ? P4 C44 1.838(2) . ? C40 C44 1.399(3) . ? C40 H40 0.95 . ? C41 C42 1.389(3) . ? C41 H41 0.95 . ? C42 C43 1.387(3) . ? C42 H42 0.95 . ? C43 C44 1.397(3) . ? C43 H43 0.95 . ? C45 C50 1.388(4) . ? C45 C46 1.406(3) . ? C46 C47 1.380(3) . ? C46 H46 0.95 . ? C47 C48 1.394(4) . ? C47 H47 0.95 . ? C48 C49 1.385(4) . ? C48 H48 0.95 . ? C49 C50 1.392(3) . ? C49 H49 0.95 . ? C50 H50 0.95 . ? C51 C52 1.400(4) . ? C51 C56 1.403(3) . ? C52 C53 1.390(4) . ? C52 H52 0.95 . ? C53 C54 1.391(4) . ? C53 H53 0.95 . ? C54 C55 1.380(4) . ? C54 H54 0.95 . ? C55 C56 1.378(4) . ? C55 H55 0.95 . ? C56 H56 0.95 . ? 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 C37 Fe1 C1 95.02(9) . . ? C37 Fe1 C5 132.77(10) . . ? C1 Fe1 C5 39.92(8) . . ? C37 Fe1 C4 153.08(9) . . ? C1 Fe1 C4 66.55(9) . . ? C5 Fe1 C4 39.24(9) . . ? C37 Fe1 C2 87.38(9) . . ? C1 Fe1 C2 39.63(9) . . ? C5 Fe1 C2 66.13(9) . . ? C4 Fe1 C2 65.85(8) . . ? C37 Fe1 C3 115.97(9) . . ? C1 Fe1 C3 66.34(9) . . ? C5 Fe1 C3 66.18(9) . . ? C4 Fe1 C3 39.67(8) . . ? C2 Fe1 C3 38.83(9) . . ? C37 Fe1 P2 86.74(7) . . ? C1 Fe1 P2 165.56(7) . . ? C5 Fe1 P2 140.48(7) . . ? C4 Fe1 P2 106.39(7) . . ? C2 Fe1 P2 126.41(7) . . ? C3 Fe1 P2 100.01(7) . . ? C37 Fe1 P1 83.92(7) . . ? C1 Fe1 P1 108.23(7) . . ? C5 Fe1 P1 96.49(7) . . ? C4 Fe1 P1 119.63(6) . . ? C2 Fe1 P1 145.69(7) . . ? C3 Fe1 P1 159.29(6) . . ? P2 Fe1 P1 86.20(2) . . ? C13 P1 C11 106.00(11) . . ? C13 P1 C19 101.22(10) . . ? C11 P1 C19 98.76(10) . . ? C13 P1 Fe1 116.83(7) . . ? C11 P1 Fe1 106.07(7) . . ? C19 P1 Fe1 125.29(8) . . ? C25 P2 C31 100.15(10) . . ? C25 P2 C12 102.44(10) . . ? C31 P2 C12 103.42(11) . . ? C25 P2 Fe1 120.72(8) . . ? C31 P2 Fe1 118.11(8) . . ? C12 P2 Fe1 109.67(8) . . ? C2 C1 C5 107.5(2) . . ? C2 C1 C6 125.2(2) . . ? C5 C1 C6 127.1(2) . . ? C2 C1 Fe1 71.51(13) . . ? C5 C1 Fe1 70.52(13) . . ? C6 C1 Fe1 127.73(17) . . ? C3 C2 C1 108.80(19) . . ? C3 C2 C7 125.7(2) . . ? C1 C2 C7 125.3(2) . . ? C3 C2 Fe1 71.19(13) . . ? C1 C2 Fe1 68.86(12) . . ? C7 C2 Fe1 129.43(17) . . ? C2 C3 C4 107.3(2) . . ? C2 C3 C8 126.1(2) . . ? C4 C3 C8 125.8(2) . . ? C2 C3 Fe1 69.98(13) . . ? C4 C3 Fe1 69.34(13) . . ? C8 C3 Fe1 133.82(17) . . ? C5 C4 C3 108.0(2) . . ? C5 C4 C9 126.5(2) . . ? C3 C4 C9 124.7(2) . . ? C5 C4 Fe1 69.76(13) . . ? C3 C4 Fe1 70.99(13) . . ? C9 C4 Fe1 132.54(16) . . ? C4 C5 C1 108.3(2) . . ? C4 C5 C10 126.1(2) . . ? C1 C5 C10 125.2(2) . . ? C4 C5 Fe1 71.00(13) . . ? C1 C5 Fe1 69.57(13) . . ? C10 C5 Fe1 130.41(17) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 P1 106.65(16) . . ? C12 C11 H11A 110.4 . . ? P1 C11 H11A 110.4 . . ? C12 C11 H11B 110.4 . . ? P1 C11 H11B 110.4 . . ? H11A C11 H11B 108.6 . . ? C11 C12 P2 110.41(16) . . ? C11 C12 H12A 109.6 . . ? P2 C12 H12A 109.6 . . ? C11 C12 H12B 109.6 . . ? P2 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? C18 C13 C14 117.7(2) . . ? C18 C13 P1 120.57(18) . . ? C14 C13 P1 121.41(18) . . ? C15 C14 C13 121.1(2) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C16 C15 C14 120.2(2) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 119.5(2) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 120.2(2) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C13 121.3(2) . . ? C17 C18 H18 119.4 . . ? C13 C18 H18 119.4 . . ? C20 C19 C24 118.6(2) . . ? C20 C19 P1 120.76(17) . . ? C24 C19 P1 120.35(18) . . ? C19 C20 C21 120.7(2) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C22 C21 C20 120.1(2) . . ? C22 C21 H21 120 . . ? C20 C21 H21 120 . . ? C21 C22 C23 119.9(2) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C22 C23 C24 120.1(2) . . ? C22 C23 H23 120 . . ? C24 C23 H23 120 . . ? C23 C24 C19 120.6(2) . . ? C23 C24 H24 119.7 . . ? C19 C24 H24 119.7 . . ? C30 C25 C26 117.9(2) . . ? C30 C25 P2 122.26(18) . . ? C26 C25 P2 119.61(16) . . ? C27 C26 C25 121.0(2) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C28 C27 C26 120.0(2) . . ? C28 C27 H27 120 . . ? C26 C27 H27 120 . . ? C27 C28 C29 119.8(2) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C28 C29 C30 120.5(2) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C29 C30 C25 120.8(2) . . ? C29 C30 H30 119.6 . . ? C25 C30 H30 119.6 . . ? C32 C31 C36 118.7(2) . . ? C32 C31 P2 119.18(18) . . ? C36 C31 P2 122.15(17) . . ? C33 C32 C31 120.7(2) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C34 C33 C32 120.2(2) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 120.0(2) . . ? C33 C34 H34 120 . . ? C35 C34 H34 120 . . ? C34 C35 C36 120.0(2) . . ? C34 C35 H35 120 . . ? C36 C35 H35 120 . . ? C35 C36 C31 120.4(2) . . ? C35 C36 H36 119.8 . . ? C31 C36 H36 119.8 . . ? C38 C37 Fe1 178.0(2) . . ? C37 C38 C39 176.7(2) . . ? C40 C39 C41 117.7(2) . . ? C40 C39 C38 121.2(2) . . ? C41 C39 C38 121.0(2) . . ? C45 P4 C51 103.08(11) . . ? C45 P4 C44 104.18(10) . . ? C51 P4 C44 99.93(11) . . ? C44 C40 C39 121.9(2) . . ? C44 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? C42 C41 C39 120.5(2) . . ? C42 C41 H41 119.7 . . ? C39 C41 H41 119.7 . . ? C43 C42 C41 120.6(2) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C42 C43 C44 120.4(2) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C43 C44 C40 118.8(2) . . ? C43 C44 P4 115.93(17) . . ? C40 C44 P4 125.01(19) . . ? C50 C45 C46 118.4(2) . . ? C50 C45 P4 121.90(17) . . ? C46 C45 P4 119.04(19) . . ? C47 C46 C45 120.5(2) . . ? C47 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? C46 C47 C48 120.6(2) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C49 C48 C47 119.4(2) . . ? C49 C48 H48 120.3 . . ? C47 C48 H48 120.3 . . ? C48 C49 C50 120.0(3) . . ? C48 C49 H49 120 . . ? C50 C49 H49 120 . . ? C45 C50 C49 121.1(2) . . ? C45 C50 H50 119.4 . . ? C49 C50 H50 119.4 . . ? C52 C51 C56 117.8(2) . . ? C52 C51 P4 125.46(18) . . ? C56 C51 P4 116.6(2) . . ? C53 C52 C51 120.7(2) . . ? C53 C52 H52 119.7 . . ? C51 C52 H52 119.7 . . ? C52 C53 C54 120.2(3) . . ? C52 C53 H53 119.9 . . ? C54 C53 H53 119.9 . . ? C55 C54 C53 119.5(3) . . ? C55 C54 H54 120.2 . . ? C53 C54 H54 120.2 . . ? C56 C55 C54 120.5(3) . . ? C56 C55 H55 119.7 . . ? C54 C55 H55 119.7 . . ? C55 C56 C51 121.2(3) . . ? C55 C56 H56 119.4 . . ? C51 C56 H56 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 C37 Fe1 P1 C13 -61.75(11) . . . . ? C1 Fe1 P1 C13 31.55(11) . . . . ? C5 Fe1 P1 C13 70.72(11) . . . . ? C4 Fe1 P1 C13 104.41(11) . . . . ? C2 Fe1 P1 C13 14.49(15) . . . . ? C3 Fe1 P1 C13 102.7(2) . . . . ? P2 Fe1 P1 C13 -148.87(9) . . . . ? C37 Fe1 P1 C11 56.10(10) . . . . ? C1 Fe1 P1 C11 149.40(10) . . . . ? C5 Fe1 P1 C11 -171.43(10) . . . . ? C4 Fe1 P1 C11 -137.73(11) . . . . ? C2 Fe1 P1 C11 132.34(13) . . . . ? C3 Fe1 P1 C11 -139.5(2) . . . . ? P2 Fe1 P1 C11 -31.02(8) . . . . ? C37 Fe1 P1 C19 169.56(12) . . . . ? C1 Fe1 P1 C19 -97.14(12) . . . . ? C5 Fe1 P1 C19 -57.97(11) . . . . ? C4 Fe1 P1 C19 -24.28(12) . . . . ? C2 Fe1 P1 C19 -114.20(15) . . . . ? C3 Fe1 P1 C19 -26.0(2) . . . . ? P2 Fe1 P1 C19 82.44(10) . . . . ? C37 Fe1 P2 C25 167.59(11) . . . . ? C1 Fe1 P2 C25 70.1(3) . . . . ? C5 Fe1 P2 C25 -12.70(14) . . . . ? C4 Fe1 P2 C25 11.50(11) . . . . ? C2 Fe1 P2 C25 83.27(12) . . . . ? C3 Fe1 P2 C25 51.78(11) . . . . ? P1 Fe1 P2 C25 -108.30(9) . . . . ? C37 Fe1 P2 C31 44.23(11) . . . . ? C1 Fe1 P2 C31 -53.3(3) . . . . ? C5 Fe1 P2 C31 -136.06(13) . . . . ? C4 Fe1 P2 C31 -111.86(11) . . . . ? C2 Fe1 P2 C31 -40.10(12) . . . . ? C3 Fe1 P2 C31 -71.58(11) . . . . ? P1 Fe1 P2 C31 128.34(9) . . . . ? C37 Fe1 P2 C12 -73.82(10) . . . . ? C1 Fe1 P2 C12 -171.3(3) . . . . ? C5 Fe1 P2 C12 105.89(13) . . . . ? C4 Fe1 P2 C12 130.09(10) . . . . ? C2 Fe1 P2 C12 -158.14(11) . . . . ? C3 Fe1 P2 C12 170.37(10) . . . . ? P1 Fe1 P2 C12 10.29(8) . . . . ? C37 Fe1 C1 C2 -79.74(14) . . . . ? C5 Fe1 C1 C2 117.04(19) . . . . ? C4 Fe1 C1 C2 79.90(14) . . . . ? C3 Fe1 C1 C2 36.45(13) . . . . ? P2 Fe1 C1 C2 16.7(3) . . . . ? P1 Fe1 C1 C2 -164.98(12) . . . . ? C37 Fe1 C1 C5 163.22(14) . . . . ? C4 Fe1 C1 C5 -37.14(13) . . . . ? C2 Fe1 C1 C5 -117.04(19) . . . . ? C3 Fe1 C1 C5 -80.59(14) . . . . ? P2 Fe1 C1 C5 -100.3(3) . . . . ? P1 Fe1 C1 C5 77.99(13) . . . . ? C37 Fe1 C1 C6 40.9(2) . . . . ? C5 Fe1 C1 C6 -122.3(3) . . . . ? C4 Fe1 C1 C6 -159.5(2) . . . . ? C2 Fe1 C1 C6 120.6(3) . . . . ? C3 Fe1 C1 C6 157.1(2) . . . . ? P2 Fe1 C1 C6 137.4(2) . . . . ? P1 Fe1 C1 C6 -44.3(2) . . . . ? C5 C1 C2 C3 1.5(3) . . . . ? C6 C1 C2 C3 176.2(2) . . . . ? Fe1 C1 C2 C3 -60.21(16) . . . . ? C5 C1 C2 C7 -174.2(2) . . . . ? C6 C1 C2 C7 0.5(4) . . . . ? Fe1 C1 C2 C7 124.1(2) . . . . ? C5 C1 C2 Fe1 61.70(16) . . . . ? C6 C1 C2 Fe1 -123.6(2) . . . . ? C37 Fe1 C2 C3 -139.11(15) . . . . ? C1 Fe1 C2 C3 119.79(19) . . . . ? C5 Fe1 C2 C3 81.10(15) . . . . ? C4 Fe1 C2 C3 37.97(14) . . . . ? P2 Fe1 C2 C3 -55.10(15) . . . . ? P1 Fe1 C2 C3 145.69(12) . . . . ? C37 Fe1 C2 C1 101.11(14) . . . . ? C5 Fe1 C2 C1 -38.68(13) . . . . ? C4 Fe1 C2 C1 -81.82(15) . . . . ? C3 Fe1 C2 C1 -119.79(19) . . . . ? P2 Fe1 C2 C1 -174.89(11) . . . . ? P1 Fe1 C2 C1 25.90(19) . . . . ? C37 Fe1 C2 C7 -17.9(2) . . . . ? C1 Fe1 C2 C7 -119.0(3) . . . . ? C5 Fe1 C2 C7 -157.7(2) . . . . ? C4 Fe1 C2 C7 159.2(2) . . . . ? C3 Fe1 C2 C7 121.2(3) . . . . ? P2 Fe1 C2 C7 66.1(2) . . . . ? P1 Fe1 C2 C7 -93.1(2) . . . . ? C1 C2 C3 C4 -0.8(3) . . . . ? C7 C2 C3 C4 174.9(2) . . . . ? Fe1 C2 C3 C4 -59.53(16) . . . . ? C1 C2 C3 C8 -171.0(2) . . . . ? C7 C2 C3 C8 4.7(4) . . . . ? Fe1 C2 C3 C8 130.3(2) . . . . ? C1 C2 C3 Fe1 58.77(16) . . . . ? C7 C2 C3 Fe1 -125.6(2) . . . . ? C37 Fe1 C3 C2 46.67(17) . . . . ? C1 Fe1 C3 C2 -37.18(14) . . . . ? C5 Fe1 C3 C2 -80.97(15) . . . . ? C4 Fe1 C3 C2 -118.4(2) . . . . ? P2 Fe1 C3 C2 137.91(13) . . . . ? P1 Fe1 C3 C2 -116.05(18) . . . . ? C37 Fe1 C3 C4 165.09(14) . . . . ? C1 Fe1 C3 C4 81.24(15) . . . . ? C5 Fe1 C3 C4 37.45(14) . . . . ? C2 Fe1 C3 C4 118.4(2) . . . . ? P2 Fe1 C3 C4 -103.66(13) . . . . ? P1 Fe1 C3 C4 2.4(3) . . . . ? C37 Fe1 C3 C8 -74.7(2) . . . . ? C1 Fe1 C3 C8 -158.5(2) . . . . ? C5 Fe1 C3 C8 157.7(2) . . . . ? C4 Fe1 C3 C8 120.2(3) . . . . ? C2 Fe1 C3 C8 -121.3(3) . . . . ? P2 Fe1 C3 C8 16.6(2) . . . . ? P1 Fe1 C3 C8 122.6(2) . . . . ? C2 C3 C4 C5 -0.3(3) . . . . ? C8 C3 C4 C5 170.0(2) . . . . ? Fe1 C3 C4 C5 -60.20(16) . . . . ? C2 C3 C4 C9 -170.9(2) . . . . ? C8 C3 C4 C9 -0.7(4) . . . . ? Fe1 C3 C4 C9 129.1(2) . . . . ? C2 C3 C4 Fe1 59.94(16) . . . . ? C8 C3 C4 Fe1 -129.8(2) . . . . ? C37 Fe1 C4 C5 87.7(2) . . . . ? C1 Fe1 C4 C5 37.76(13) . . . . ? C2 Fe1 C4 C5 81.25(14) . . . . ? C3 Fe1 C4 C5 118.42(19) . . . . ? P2 Fe1 C4 C5 -155.65(11) . . . . ? P1 Fe1 C4 C5 -60.61(13) . . . . ? C37 Fe1 C4 C3 -30.7(3) . . . . ? C1 Fe1 C4 C3 -80.66(14) . . . . ? C5 Fe1 C4 C3 -118.42(19) . . . . ? C2 Fe1 C4 C3 -37.18(14) . . . . ? P2 Fe1 C4 C3 85.93(13) . . . . ? P1 Fe1 C4 C3 -179.03(11) . . . . ? C37 Fe1 C4 C9 -150.8(2) . . . . ? C1 Fe1 C4 C9 159.3(3) . . . . ? C5 Fe1 C4 C9 121.5(3) . . . . ? C2 Fe1 C4 C9 -157.2(3) . . . . ? C3 Fe1 C4 C9 -120.1(3) . . . . ? P2 Fe1 C4 C9 -34.1(2) . . . . ? P1 Fe1 C4 C9 60.9(2) . . . . ? C3 C4 C5 C1 1.2(3) . . . . ? C9 C4 C5 C1 171.6(2) . . . . ? Fe1 C4 C5 C1 -59.80(16) . . . . ? C3 C4 C5 C10 -172.3(2) . . . . ? C9 C4 C5 C10 -1.9(4) . . . . ? Fe1 C4 C5 C10 126.7(2) . . . . ? C3 C4 C5 Fe1 60.98(16) . . . . ? C9 C4 C5 Fe1 -128.6(2) . . . . ? C2 C1 C5 C4 -1.6(3) . . . . ? C6 C1 C5 C4 -176.2(2) . . . . ? Fe1 C1 C5 C4 60.70(16) . . . . ? C2 C1 C5 C10 171.9(2) . . . . ? C6 C1 C5 C10 -2.6(4) . . . . ? Fe1 C1 C5 C10 -125.7(2) . . . . ? C2 C1 C5 Fe1 -62.34(16) . . . . ? C6 C1 C5 Fe1 123.1(2) . . . . ? C37 Fe1 C5 C4 -141.95(14) . . . . ? C1 Fe1 C5 C4 -118.89(19) . . . . ? C2 Fe1 C5 C4 -80.48(14) . . . . ? C3 Fe1 C5 C4 -37.86(13) . . . . ? P2 Fe1 C5 C4 38.44(17) . . . . ? P1 Fe1 C5 C4 130.34(12) . . . . ? C37 Fe1 C5 C1 -23.07(19) . . . . ? C4 Fe1 C5 C1 118.89(19) . . . . ? C2 Fe1 C5 C1 38.41(13) . . . . ? C3 Fe1 C5 C1 81.03(14) . . . . ? P2 Fe1 C5 C1 157.33(11) . . . . ? P1 Fe1 C5 C1 -110.77(13) . . . . ? C37 Fe1 C5 C10 96.4(2) . . . . ? C1 Fe1 C5 C10 119.4(3) . . . . ? C4 Fe1 C5 C10 -121.7(3) . . . . ? C2 Fe1 C5 C10 157.8(3) . . . . ? C3 Fe1 C5 C10 -159.5(2) . . . . ? P2 Fe1 C5 C10 -83.2(2) . . . . ? P1 Fe1 C5 C10 8.6(2) . . . . ? C13 P1 C11 C12 174.36(14) . . . . ? C19 P1 C11 C12 -81.23(16) . . . . ? Fe1 P1 C11 C12 49.52(15) . . . . ? P1 C11 C12 P2 -41.62(18) . . . . ? C25 P2 C12 C11 147.16(16) . . . . ? C31 P2 C12 C11 -109.06(17) . . . . ? Fe1 P2 C12 C11 17.78(17) . . . . ? C11 P1 C13 C18 -43.5(2) . . . . ? C19 P1 C13 C18 -146.14(19) . . . . ? Fe1 P1 C13 C18 74.4(2) . . . . ? C11 P1 C13 C14 143.00(19) . . . . ? C19 P1 C13 C14 40.4(2) . . . . ? Fe1 P1 C13 C14 -99.11(18) . . . . ? C18 C13 C14 C15 -1.2(3) . . . . ? P1 C13 C14 C15 172.46(18) . . . . ? C13 C14 C15 C16 1.1(4) . . . . ? C14 C15 C16 C17 -0.3(4) . . . . ? C15 C16 C17 C18 -0.5(4) . . . . ? C16 C17 C18 C13 0.4(4) . . . . ? C14 C13 C18 C17 0.4(3) . . . . ? P1 C13 C18 C17 -173.31(18) . . . . ? C13 P1 C19 C20 -144.6(2) . . . . ? C11 P1 C19 C20 107.1(2) . . . . ? Fe1 P1 C19 C20 -9.8(2) . . . . ? C13 P1 C19 C24 41.7(2) . . . . ? C11 P1 C19 C24 -66.7(2) . . . . ? Fe1 P1 C19 C24 176.45(15) . . . . ? C24 C19 C20 C21 1.1(3) . . . . ? P1 C19 C20 C21 -172.74(18) . . . . ? C19 C20 C21 C22 -1.0(4) . . . . ? C20 C21 C22 C23 0.0(4) . . . . ? C21 C22 C23 C24 0.9(4) . . . . ? C22 C23 C24 C19 -0.7(4) . . . . ? C20 C19 C24 C23 -0.3(3) . . . . ? P1 C19 C24 C23 173.62(18) . . . . ? C31 P2 C25 C30 -147.5(2) . . . . ? C12 P2 C25 C30 -41.2(2) . . . . ? Fe1 P2 C25 C30 80.9(2) . . . . ? C31 P2 C25 C26 38.3(2) . . . . ? C12 P2 C25 C26 144.57(19) . . . . ? Fe1 P2 C25 C26 -93.29(19) . . . . ? C30 C25 C26 C27 -1.3(4) . . . . ? P2 C25 C26 C27 173.19(19) . . . . ? C25 C26 C27 C28 0.8(4) . . . . ? C26 C27 C28 C29 0.4(4) . . . . ? C27 C28 C29 C30 -1.1(4) . . . . ? C28 C29 C30 C25 0.6(4) . . . . ? C26 C25 C30 C29 0.6(4) . . . . ? P2 C25 C30 C29 -173.70(19) . . . . ? C25 P2 C31 C32 -119.9(2) . . . . ? C12 P2 C31 C32 134.60(19) . . . . ? Fe1 P2 C31 C32 13.3(2) . . . . ? C25 P2 C31 C36 60.8(2) . . . . ? C12 P2 C31 C36 -44.7(2) . . . . ? Fe1 P2 C31 C36 -165.99(17) . . . . ? C36 C31 C32 C33 1.5(4) . . . . ? P2 C31 C32 C33 -177.77(19) . . . . ? C31 C32 C33 C34 0.5(4) . . . . ? C32 C33 C34 C35 -1.9(4) . . . . ? C33 C34 C35 C36 1.2(4) . . . . ? C34 C35 C36 C31 0.8(4) . . . . ? C32 C31 C36 C35 -2.2(4) . . . . ? P2 C31 C36 C35 177.11(19) . . . . ? C41 C39 C40 C44 -0.2(3) . . . . ? C38 C39 C40 C44 -179.3(2) . . . . ? C40 C39 C41 C42 -1.4(3) . . . . ? C38 C39 C41 C42 177.8(2) . . . . ? C39 C41 C42 C43 1.2(3) . . . . ? C41 C42 C43 C44 0.5(3) . . . . ? C42 C43 C44 C40 -2.0(3) . . . . ? C42 C43 C44 P4 172.40(18) . . . . ? C39 C40 C44 C43 1.8(3) . . . . ? C39 C40 C44 P4 -171.98(17) . . . . ? C45 P4 C44 C43 143.06(18) . . . . ? C51 P4 C44 C43 -110.61(19) . . . . ? C45 P4 C44 C40 -43.0(2) . . . . ? C51 P4 C44 C40 63.3(2) . . . . ? C51 P4 C45 C50 30.9(2) . . . . ? C44 P4 C45 C50 134.9(2) . . . . ? C51 P4 C45 C46 -158.83(19) . . . . ? C44 P4 C45 C46 -54.9(2) . . . . ? C50 C45 C46 C47 -1.0(4) . . . . ? P4 C45 C46 C47 -171.6(2) . . . . ? C45 C46 C47 C48 0.3(4) . . . . ? C46 C47 C48 C49 0.4(4) . . . . ? C47 C48 C49 C50 -0.5(4) . . . . ? C46 C45 C50 C49 1.0(4) . . . . ? P4 C45 C50 C49 171.3(2) . . . . ? C48 C49 C50 C45 -0.2(4) . . . . ? C45 P4 C51 C52 48.5(2) . . . . ? C44 P4 C51 C52 -58.7(2) . . . . ? C45 P4 C51 C56 -135.86(19) . . . . ? C44 P4 C51 C56 116.93(19) . . . . ? C56 C51 C52 C53 -1.7(4) . . . . ? P4 C51 C52 C53 173.8(2) . . . . ? C51 C52 C53 C54 0.0(4) . . . . ? C52 C53 C54 C55 1.5(4) . . . . ? C53 C54 C55 C56 -1.3(4) . . . . ? C54 C55 C56 C51 -0.5(4) . . . . ? C52 C51 C56 C55 2.0(4) . . . . ? P4 C51 C56 C55 -174.0(2) . . . . ?