# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Arthur Carty' _publ_contact_author_address ; National Science Advisor to the Prime Minister Privy Council Office 85 Sparks Street, Room 728 Ottawa ON K1A 0A3 CANADA ; _publ_contact_author_email ACARTY@PCO-BCP.GC.CA _publ_section_title ; Reactivity Patterns of Thermally Stable, Terminal, Electrophilic Phosphinidene Complexes Towards Diazoalkanes: Oxidation at the Phosphorus Centre and Formation of P-bound h1-Phosphaimine, h1-Phosphaalkene and h3-Diazaphosphaallene Complexes. ; loop_ _publ_author_name 'A. Carty' 'Todd Graham' 'Konstantin A. Udachin' # Attachment 'tg20 Compound 15.cif' data_tg20 _database_code_depnum_ccdc_archive 'CCDC 283075' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H41 Al Cl6 N3 O2 P W' _chemical_formula_weight 954.18 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 '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 monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.615(3) _cell_length_b 14.159(4) _cell_length_c 24.833(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.265(11) _cell_angle_gamma 90.00 _cell_volume 3939.9(18) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 3.434 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.2786 _exptl_absorpt_correction_T_max 0.4806 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44194 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 28.28 _reflns_number_total 9769 _reflns_number_gt 9245 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\\s^2^(Fo^2^)+(0.0324P)^2^+4.3889P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9769 _refine_ls_number_parameters 454 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0674 _refine_ls_wR_factor_gt 0.0665 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _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 W1 W 0.325881(8) -0.322500(6) -0.331490(4) 0.02050(4) Uani 1 1 d . . . Cl1 Cl 0.80737(7) -0.20526(5) -0.08148(3) 0.04270(17) Uani 1 1 d . . . Cl2 Cl 0.75055(10) -0.10469(6) 0.03562(3) 0.0553(2) Uani 1 1 d . . . Cl3 Cl 0.51666(8) -0.16055(7) -0.07936(5) 0.0589(2) Uani 1 1 d . . . Cl4 Cl 0.67602(9) -0.33959(5) 0.00425(4) 0.04825(19) Uani 1 1 d . . . P1 P 0.22278(5) -0.14888(4) -0.33362(2) 0.02068(11) Uani 1 1 d . . . Al1 Al 0.68737(7) -0.20356(6) -0.03023(3) 0.02746(15) Uani 1 1 d . . . O1 O 0.52880(16) -0.28596(15) -0.22264(8) 0.0329(4) Uani 1 1 d . . . O2 O 0.48022(18) -0.17422(14) -0.37493(10) 0.0359(5) Uani 1 1 d . . . N1 N 0.18638(17) -0.30101(14) -0.29507(8) 0.0204(4) Uani 1 1 d . . . N2 N 0.14988(16) -0.25416(14) -0.34756(8) 0.0205(4) Uani 1 1 d . . . N3 N 0.19802(17) -0.09933(14) -0.39540(8) 0.0218(4) Uani 1 1 d . . . C1 C 0.4520(2) -0.29708(17) -0.26199(10) 0.0243(4) Uani 1 1 d . . . C2 C 0.4218(2) -0.22717(18) -0.35893(11) 0.0260(5) Uani 1 1 d . . . C3 C 0.2424(2) -0.47478(17) -0.35159(11) 0.0262(5) Uani 1 1 d . . . C4 C 0.2373(2) -0.43271(17) -0.40378(10) 0.0259(5) Uani 1 1 d . . . C5 C 0.3564(2) -0.41142(19) -0.40563(11) 0.0302(5) Uani 1 1 d . . . C6 C 0.4357(2) -0.44249(19) -0.35409(12) 0.0316(5) Uani 1 1 d . . . C7 C 0.3649(2) -0.48144(18) -0.32032(11) 0.0306(5) Uani 1 1 d . . . C8 C 0.1364(3) -0.5125(2) -0.33484(13) 0.0371(6) Uani 1 1 d . . . H8C H 0.1090 -0.5708 -0.3555 0.055(11) Uiso 1 1 d R . . H8B H 0.1585 -0.5257 -0.2947 0.042(9) Uiso 1 1 d R . . H8A H 0.0721 -0.4656 -0.3435 0.053(11) Uiso 1 1 d R . . C9 C 0.1255(3) -0.4199(2) -0.44935(12) 0.0382(6) Uani 1 1 d . . . H9C H 0.0639 -0.3917 -0.4340 0.068(13) Uiso 1 1 d R . . H9B H 0.1411 -0.3782 -0.4781 0.088(16) Uiso 1 1 d R . . H9A H 0.0979 -0.4814 -0.4658 0.058(11) Uiso 1 1 d R . . C10 C 0.3927(3) -0.3772(3) -0.45576(14) 0.0473(8) Uani 1 1 d . . . H10C H 0.3349 -0.3303 -0.4756 0.11(2) Uiso 1 1 d R . . H10B H 0.4720 -0.3482 -0.4439 0.050(10) Uiso 1 1 d R . . H10A H 0.3949 -0.4305 -0.4806 0.054(11) Uiso 1 1 d R . . C11 C 0.5690(3) -0.4466(3) -0.34052(18) 0.0513(9) Uani 1 1 d . . . H11C H 0.5943 -0.5118 -0.3441 0.062(12) Uiso 1 1 d R . . H11B H 0.5972 -0.4061 -0.3664 0.037(9) Uiso 1 1 d R . . H11A H 0.6030 -0.4246 -0.3022 0.056(11) Uiso 1 1 d R . . C12 C 0.4097(3) -0.5337(2) -0.26613(14) 0.0461(8) Uani 1 1 d . . . H12C H 0.4904 -0.5120 -0.2474 0.075(14) Uiso 1 1 d R . . H12B H 0.3566 -0.5216 -0.2421 0.103(19) Uiso 1 1 d R . . H12A H 0.4114 -0.6016 -0.2736 0.053(11) Uiso 1 1 d R . . C13 C 0.1200(2) -0.31909(15) -0.26186(10) 0.0206(4) Uani 1 1 d . . . C14 C 0.1803(2) -0.37086(17) -0.21001(10) 0.0234(4) Uani 1 1 d . . . C15 C 0.1311(2) -0.45310(18) -0.19491(11) 0.0292(5) Uani 1 1 d . . . H15 H 0.0559 -0.4750 -0.2166 0.032(8) Uiso 1 1 d R . . C16 C 0.1924(3) -0.5031(2) -0.14810(13) 0.0393(7) Uani 1 1 d . . . H16 H 0.1595 -0.5599 -0.1382 0.041(9) Uiso 1 1 d R . . C17 C 0.3012(3) -0.4708(2) -0.11561(12) 0.0414(7) Uani 1 1 d . . . H17 H 0.3432 -0.5061 -0.0840 0.046(10) Uiso 1 1 d R . . C18 C 0.3487(3) -0.3875(2) -0.12919(11) 0.0356(6) Uani 1 1 d . . . H18 H 0.4220 -0.3644 -0.1062 0.046(10) Uiso 1 1 d R . . C19 C 0.2892(2) -0.33747(18) -0.17648(10) 0.0264(5) Uani 1 1 d . . . H19 H 0.3223 -0.2805 -0.1860 0.034(8) Uiso 1 1 d R . . C20 C -0.0068(2) -0.29259(16) -0.27283(10) 0.0218(4) Uani 1 1 d . . . C21 C -0.0541(2) -0.27895(17) -0.22722(10) 0.0248(5) Uani 1 1 d . . . H21 H -0.0047 -0.2881 -0.1905 0.032(8) Uiso 1 1 d R . . C22 C -0.1726(2) -0.25189(19) -0.23496(11) 0.0298(5) Uani 1 1 d . . . H22 H -0.2038 -0.2419 -0.2037 0.026(7) Uiso 1 1 d R . . C23 C -0.2445(2) -0.2397(2) -0.28850(12) 0.0309(5) Uani 1 1 d . . . H23 H -0.3251 -0.2204 -0.2940 0.031(8) Uiso 1 1 d R . . C24 C -0.1996(2) -0.2557(2) -0.33440(11) 0.0303(5) Uani 1 1 d . . . H24 H -0.2500 -0.2484 -0.3711 0.027(7) Uiso 1 1 d R . . C25 C -0.0815(2) -0.28200(18) -0.32683(10) 0.0254(5) Uani 1 1 d . . . H25 H -0.0513 -0.2930 -0.3583 0.017(6) Uiso 1 1 d R . . C26 C 0.2036(2) 0.00621(17) -0.39665(10) 0.0247(5) Uani 1 1 d . . . H26 H 0.1896 0.0254 -0.4366 0.022(7) Uiso 1 1 d R . . C27 C 0.3260(3) 0.0423(2) -0.36590(15) 0.0471(8) Uani 1 1 d . . . H27C H 0.3863 0.0142 -0.3821 0.039(9) Uiso 1 1 d R . . H27B H 0.3280 0.1112 -0.3693 0.035(8) Uiso 1 1 d R . . H27A H 0.3428 0.0248 -0.3264 0.073(15) Uiso 1 1 d R . . C28 C 0.1046(3) 0.0502(2) -0.37554(15) 0.0464(8) Uani 1 1 d . . . H28C H 0.1165 0.0340 -0.3361 0.050(10) Uiso 1 1 d R . . H28B H 0.1065 0.1190 -0.3796 0.052(11) Uiso 1 1 d R . . H28A H 0.0272 0.0260 -0.3972 0.11(2) Uiso 1 1 d R . . C29 C 0.1596(2) -0.15096(19) -0.44907(10) 0.0288(5) Uani 1 1 d . . . H29 H 0.1788 -0.2191 -0.4408 0.030(8) Uiso 1 1 d R . . C30 C 0.0259(3) -0.1442(2) -0.47346(14) 0.0458(8) Uani 1 1 d . . . H30C H 0.0022 -0.0776 -0.4774 0.051(10) Uiso 1 1 d R . . H30B H 0.0038 -0.1746 -0.5102 0.042(10) Uiso 1 1 d R . . H30A H -0.0147 -0.1759 -0.4486 0.063(13) Uiso 1 1 d R . . C31 C 0.2285(3) -0.1193(2) -0.49023(12) 0.0421(7) Uani 1 1 d . . . H31C H 0.3143 -0.1241 -0.4726 0.053(11) Uiso 1 1 d R . . H31B H 0.2076 -0.1598 -0.5234 0.069(14) Uiso 1 1 d R . . H31A H 0.2081 -0.0536 -0.5012 0.051(10) Uiso 1 1 d R . . Cl1A Cl 0.11112(9) -0.17293(7) -0.09503(3) 0.0516(2) Uani 1 1 d . . . Cl2A Cl 0.15774(8) -0.08754(6) -0.19413(4) 0.04848(18) Uani 1 1 d . . . C1A C 0.2028(3) -0.0997(4) -0.12141(15) 0.0629(12) Uani 1 1 d . . . H1A1 H 0.2850 -0.1252 -0.1105 0.076 Uiso 1 1 calc R . . H1A2 H 0.2045 -0.0364 -0.1042 0.076 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 W1 0.01993(6) 0.02037(6) 0.02105(6) -0.00024(3) 0.00513(4) -0.00018(3) Cl1 0.0539(4) 0.0343(3) 0.0503(4) 0.0045(3) 0.0321(3) 0.0034(3) Cl2 0.0913(7) 0.0385(4) 0.0364(4) -0.0102(3) 0.0175(4) -0.0099(4) Cl3 0.0372(4) 0.0580(5) 0.0748(6) 0.0142(5) 0.0030(4) 0.0092(4) Cl4 0.0734(6) 0.0305(3) 0.0457(4) 0.0101(3) 0.0242(4) -0.0037(3) P1 0.0233(3) 0.0199(3) 0.0184(3) 0.0013(2) 0.0046(2) 0.0006(2) Al1 0.0344(4) 0.0240(3) 0.0254(4) 0.0017(3) 0.0103(3) 0.0012(3) O1 0.0273(9) 0.0393(11) 0.0284(9) 0.0004(8) 0.0006(7) -0.0031(8) O2 0.0275(9) 0.0363(11) 0.0464(12) 0.0096(8) 0.0139(9) -0.0024(7) N1 0.0214(9) 0.0195(8) 0.0198(9) 0.0022(7) 0.0043(7) 0.0001(7) N2 0.0198(8) 0.0222(9) 0.0191(9) 0.0037(7) 0.0044(7) -0.0006(7) N3 0.0259(9) 0.0197(9) 0.0183(9) 0.0022(7) 0.0033(7) -0.0010(7) C1 0.0241(11) 0.0226(11) 0.0263(11) 0.0011(9) 0.0070(9) 0.0002(9) C2 0.0212(10) 0.0271(12) 0.0294(12) 0.0032(9) 0.0059(9) 0.0021(9) C3 0.0303(12) 0.0200(11) 0.0292(12) -0.0061(9) 0.0095(9) -0.0034(9) C4 0.0277(11) 0.0246(11) 0.0253(11) -0.0073(9) 0.0069(9) -0.0026(9) C5 0.0333(13) 0.0287(12) 0.0324(13) -0.0106(10) 0.0154(10) -0.0060(10) C6 0.0236(11) 0.0268(12) 0.0437(15) -0.0116(11) 0.0075(10) 0.0017(9) C7 0.0334(13) 0.0209(11) 0.0343(13) -0.0029(10) 0.0034(10) 0.0025(9) C8 0.0440(15) 0.0284(13) 0.0452(16) -0.0107(11) 0.0233(13) -0.0132(11) C9 0.0373(14) 0.0386(15) 0.0317(14) -0.0082(12) -0.0031(11) -0.0020(12) C10 0.061(2) 0.0496(19) 0.0426(17) -0.0150(14) 0.0340(16) -0.0185(16) C11 0.0246(13) 0.0452(18) 0.082(3) -0.0281(17) 0.0107(14) 0.0018(12) C12 0.0585(19) 0.0250(14) 0.0450(17) 0.0037(12) -0.0036(15) 0.0045(13) C13 0.0232(11) 0.0180(10) 0.0211(11) -0.0005(8) 0.0065(8) -0.0010(7) C14 0.0274(11) 0.0222(11) 0.0222(11) 0.0022(8) 0.0095(9) 0.0037(9) C15 0.0349(13) 0.0249(12) 0.0313(13) 0.0030(10) 0.0146(10) 0.0004(10) C16 0.0581(18) 0.0277(13) 0.0400(15) 0.0124(12) 0.0268(14) 0.0096(12) C17 0.0502(17) 0.0475(17) 0.0291(13) 0.0149(12) 0.0151(12) 0.0217(14) C18 0.0348(13) 0.0469(16) 0.0240(12) 0.0040(11) 0.0059(10) 0.0118(12) C19 0.0291(12) 0.0294(12) 0.0212(11) 0.0020(9) 0.0077(9) 0.0041(9) C20 0.0219(10) 0.0197(10) 0.0242(11) -0.0014(8) 0.0070(8) -0.0024(8) C21 0.0245(11) 0.0271(12) 0.0233(11) -0.0024(9) 0.0072(9) -0.0026(9) C22 0.0273(12) 0.0340(13) 0.0305(13) -0.0057(10) 0.0119(10) -0.0013(10) C23 0.0216(11) 0.0344(13) 0.0371(14) -0.0021(11) 0.0082(10) 0.0001(9) C24 0.0230(11) 0.0372(14) 0.0290(13) 0.0011(10) 0.0039(9) -0.0026(10) C25 0.0239(11) 0.0290(12) 0.0238(11) -0.0001(9) 0.0073(9) -0.0016(9) C26 0.0298(12) 0.0190(10) 0.0248(11) 0.0029(8) 0.0063(9) -0.0008(8) C27 0.0444(17) 0.0280(14) 0.0550(19) 0.0087(13) -0.0115(14) -0.0106(12) C28 0.064(2) 0.0302(14) 0.0550(19) 0.0076(13) 0.0337(17) 0.0121(14) C29 0.0392(14) 0.0250(12) 0.0192(11) 0.0008(9) 0.0021(10) -0.0050(10) C30 0.0405(16) 0.0447(18) 0.0397(16) 0.0051(14) -0.0114(13) -0.0110(13) C31 0.068(2) 0.0372(15) 0.0239(13) -0.0021(11) 0.0176(13) -0.0072(14) Cl1A 0.0552(5) 0.0624(5) 0.0310(4) 0.0005(3) 0.0004(3) -0.0090(4) Cl2A 0.0480(4) 0.0500(4) 0.0461(4) -0.0018(3) 0.0100(3) -0.0154(3) C1A 0.0447(18) 0.105(3) 0.0394(18) -0.028(2) 0.0120(14) -0.032(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C1 1.981(2) . ? W1 C2 1.981(3) . ? W1 N1 2.076(2) . ? W1 N2 2.2011(19) . ? W1 C6 2.281(3) . ? W1 C7 2.298(3) . ? W1 C5 2.333(2) . ? W1 C3 2.363(2) . ? W1 C4 2.397(2) . ? W1 P1 2.7289(9) . ? Cl1 Al1 2.1206(11) . ? Cl2 Al1 2.1309(12) . ? Cl3 Al1 2.1253(13) . ? Cl4 Al1 2.1259(12) . ? P1 N3 1.642(2) . ? P1 N2 1.704(2) . ? O1 C1 1.147(3) . ? O2 C2 1.150(3) . ? N1 C13 1.294(3) . ? N1 N2 1.424(3) . ? N3 C29 1.482(3) . ? N3 C26 1.497(3) . ? C3 C4 1.414(4) . ? C3 C7 1.434(4) . ? C3 C8 1.498(4) . ? C4 C5 1.429(3) . ? C4 C9 1.492(4) . ? C5 C6 1.435(4) . ? C5 C10 1.496(4) . ? C6 C7 1.430(4) . ? C6 C11 1.498(4) . ? C7 C12 1.503(4) . ? C13 C20 1.474(3) . ? C13 C14 1.487(3) . ? C14 C15 1.391(3) . ? C14 C19 1.400(4) . ? C15 C16 1.387(4) . ? C16 C17 1.386(5) . ? C17 C18 1.381(5) . ? C18 C19 1.390(4) . ? C20 C21 1.396(3) . ? C20 C25 1.400(3) . ? C21 C22 1.393(3) . ? C22 C23 1.382(4) . ? C23 C24 1.392(4) . ? C24 C25 1.385(3) . ? C26 C27 1.514(4) . ? C26 C28 1.517(4) . ? C29 C30 1.513(4) . ? C29 C31 1.523(4) . ? Cl1A C1A 1.734(4) . ? Cl2A C1A 1.751(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 W1 C2 79.75(10) . . ? C1 W1 N1 94.41(9) . . ? C2 W1 N1 128.61(9) . . ? C1 W1 N2 121.11(9) . . ? C2 W1 N2 102.56(9) . . ? N1 W1 N2 38.76(7) . . ? C1 W1 C6 90.95(10) . . ? C2 W1 C6 91.23(11) . . ? N1 W1 C6 140.12(9) . . ? N2 W1 C6 146.65(8) . . ? C1 W1 C7 89.75(10) . . ? C2 W1 C7 126.71(10) . . ? N1 W1 C7 104.05(9) . . ? N2 W1 C7 126.63(9) . . ? C6 W1 C7 36.40(10) . . ? C1 W1 C5 123.67(10) . . ? C2 W1 C5 83.12(10) . . ? N1 W1 C5 136.16(8) . . ? N2 W1 C5 114.89(9) . . ? C6 W1 C5 36.21(10) . . ? C7 W1 C5 60.05(10) . . ? C1 W1 C3 121.21(9) . . ? C2 W1 C3 141.77(10) . . ? N1 W1 C3 84.36(8) . . ? N2 W1 C3 93.03(8) . . ? C6 W1 C3 59.56(9) . . ? C7 W1 C3 35.79(9) . . ? C5 W1 C3 58.69(9) . . ? C1 W1 C4 147.59(9) . . ? C2 W1 C4 110.81(10) . . ? N1 W1 C4 101.04(8) . . ? N2 W1 C4 87.44(8) . . ? C6 W1 C4 59.23(9) . . ? C7 W1 C4 58.99(9) . . ? C5 W1 C4 35.13(8) . . ? C3 W1 C4 34.54(9) . . ? C1 W1 P1 94.20(7) . . ? C2 W1 P1 70.32(7) . . ? N1 W1 P1 59.17(6) . . ? N2 W1 P1 38.61(5) . . ? C6 W1 P1 159.55(8) . . ? C7 W1 P1 162.97(7) . . ? C5 W1 P1 128.89(7) . . ? C3 W1 P1 131.63(6) . . ? C4 W1 P1 118.19(6) . . ? N3 P1 N2 103.20(10) . . ? N3 P1 W1 111.78(8) . . ? N2 P1 W1 53.70(7) . . ? Cl1 Al1 Cl3 108.66(5) . . ? Cl1 Al1 Cl4 110.58(5) . . ? Cl3 Al1 Cl4 110.08(5) . . ? Cl1 Al1 Cl2 108.67(5) . . ? Cl3 Al1 Cl2 109.46(6) . . ? Cl4 Al1 Cl2 109.36(5) . . ? C13 N1 N2 126.28(19) . . ? C13 N1 W1 155.94(17) . . ? N2 N1 W1 75.39(11) . . ? N1 N2 P1 102.07(14) . . ? N1 N2 W1 65.85(11) . . ? P1 N2 W1 87.69(8) . . ? C29 N3 C26 118.56(19) . . ? C29 N3 P1 124.52(16) . . ? C26 N3 P1 116.63(15) . . ? O1 C1 W1 176.3(2) . . ? O2 C2 W1 177.7(2) . . ? C4 C3 C7 108.7(2) . . ? C4 C3 C8 124.5(2) . . ? C7 C3 C8 126.7(3) . . ? C4 C3 W1 74.03(14) . . ? C7 C3 W1 69.62(13) . . ? C8 C3 W1 126.03(17) . . ? C3 C4 C5 108.2(2) . . ? C3 C4 C9 124.4(2) . . ? C5 C4 C9 127.4(3) . . ? C3 C4 W1 71.43(13) . . ? C5 C4 W1 70.02(14) . . ? C9 C4 W1 127.24(18) . . ? C4 C5 C6 107.8(2) . . ? C4 C5 C10 125.6(3) . . ? C6 C5 C10 125.9(3) . . ? C4 C5 W1 74.85(14) . . ? C6 C5 W1 69.91(14) . . ? C10 C5 W1 128.0(2) . . ? C7 C6 C5 108.0(2) . . ? C7 C6 C11 125.0(3) . . ? C5 C6 C11 126.5(3) . . ? C7 C6 W1 72.44(14) . . ? C5 C6 W1 73.88(14) . . ? C11 C6 W1 125.85(19) . . ? C6 C7 C3 107.4(2) . . ? C6 C7 C12 126.7(3) . . ? C3 C7 C12 125.3(3) . . ? C6 C7 W1 71.16(15) . . ? C3 C7 W1 74.58(14) . . ? C12 C7 W1 126.92(19) . . ? N1 C13 C20 124.5(2) . . ? N1 C13 C14 115.2(2) . . ? C20 C13 C14 120.4(2) . . ? C15 C14 C19 119.5(2) . . ? C15 C14 C13 120.8(2) . . ? C19 C14 C13 119.6(2) . . ? C16 C15 C14 119.8(3) . . ? C17 C16 C15 120.5(3) . . ? C18 C17 C16 120.1(3) . . ? C17 C18 C19 120.0(3) . . ? C18 C19 C14 120.0(3) . . ? C21 C20 C25 119.0(2) . . ? C21 C20 C13 118.2(2) . . ? C25 C20 C13 122.8(2) . . ? C22 C21 C20 120.8(2) . . ? C23 C22 C21 119.5(2) . . ? C22 C23 C24 120.4(2) . . ? C25 C24 C23 120.3(2) . . ? C24 C25 C20 120.0(2) . . ? N3 C26 C27 111.5(2) . . ? N3 C26 C28 111.2(2) . . ? C27 C26 C28 112.5(3) . . ? N3 C29 C30 111.3(2) . . ? N3 C29 C31 111.8(2) . . ? C30 C29 C31 112.2(2) . . ? Cl1A C1A Cl2A 113.68(18) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.415 _refine_diff_density_min -1.106 _refine_diff_density_rms 0.096 data_tg39 _database_code_depnum_ccdc_archive 'CCDC 283076' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H31 Al Cl6 Fe N3 O2 P' _chemical_formula_weight 756.05 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3584(8) _cell_length_b 17.4493(14) _cell_length_c 18.9477(15) _cell_angle_alpha 90.00 _cell_angle_beta 99.5310(10) _cell_angle_gamma 90.00 _cell_volume 3377.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 1.025 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.6284 _exptl_absorpt_correction_T_max 0.9045 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41757 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0162 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 29.59 _reflns_number_total 9406 _reflns_number_gt 8221 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+2.0691P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9406 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 0.102450(18) 0.484505(11) 0.334098(10) 0.01737(5) Uani 1 1 d . . . Cl1 Cl -0.05781(4) 0.29880(3) 0.50285(2) 0.04238(10) Uani 1 1 d . . . Cl2 Cl 0.27589(4) 0.25739(3) 0.54340(2) 0.03830(10) Uani 1 1 d . . . Cl3 Cl 0.04676(5) 0.13313(2) 0.59663(2) 0.04161(11) Uani 1 1 d . . . Cl4 Cl 0.10496(4) 0.30992(2) 0.678745(19) 0.02835(8) Uani 1 1 d . . . P1 P -0.02848(3) 0.521413(18) 0.238779(17) 0.01537(7) Uani 1 1 d . A . Al1 Al 0.09302(4) 0.24941(2) 0.57963(2) 0.02257(9) Uani 1 1 d . . . O1 O -0.09100(11) 0.51474(7) 0.42736(6) 0.0317(2) Uani 1 1 d . . . O2 O 0.23301(11) 0.63140(6) 0.37083(7) 0.0322(2) Uani 1 1 d . . . N1 N 0.00971(10) 0.57578(6) 0.17581(6) 0.01608(19) Uani 1 1 d . . . N2 N -0.17338(11) 0.49240(7) 0.21614(6) 0.0198(2) Uani 1 1 d . . . N3 N -0.22119(11) 0.44879(7) 0.26845(6) 0.0205(2) Uani 1 1 d . A . C1 C -0.01907(14) 0.50375(8) 0.38959(7) 0.0232(3) Uani 1 1 d . A . C2 C 0.18133(13) 0.57521(8) 0.35566(7) 0.0222(3) Uani 1 1 d . A . C8 C 0.14764(12) 0.60218(8) 0.17982(7) 0.0195(2) Uani 1 1 d . A . H8 H 0.1997 0.5784 0.2235 0.023 Uiso 1 1 calc R . . C9 C 0.20595(15) 0.57392(9) 0.11568(8) 0.0286(3) Uani 1 1 d . . . H9C H 0.1602 0.5983 0.0720 0.034 Uiso 1 1 calc R A . H9B H 0.1960 0.5182 0.1116 0.034 Uiso 1 1 calc R . . H9A H 0.2991 0.5872 0.1223 0.034 Uiso 1 1 calc R . . C10 C 0.15897(15) 0.68871(8) 0.18919(9) 0.0284(3) Uani 1 1 d . . . H10C H 0.1227 0.7040 0.2317 0.034 Uiso 1 1 calc R A . H10B H 0.1102 0.7141 0.1468 0.034 Uiso 1 1 calc R . . H10A H 0.2513 0.7037 0.1951 0.034 Uiso 1 1 calc R . . C11 C -0.08594(13) 0.60325(8) 0.11227(7) 0.0189(2) Uani 1 1 d . A . H11 H -0.0361 0.6382 0.0847 0.023 Uiso 1 1 calc R . . C12 C -0.19499(15) 0.65119(9) 0.13481(8) 0.0262(3) Uani 1 1 d . . . H12C H -0.2485 0.6189 0.1609 0.031 Uiso 1 1 calc R A . H12B H -0.2499 0.6725 0.0922 0.031 Uiso 1 1 calc R . . H12A H -0.1567 0.6931 0.1658 0.031 Uiso 1 1 calc R . . C13 C -0.13801(14) 0.53880(9) 0.06175(7) 0.0245(3) Uani 1 1 d . . . H13C H -0.1917 0.5043 0.0857 0.029 Uiso 1 1 calc R A . H13B H -0.0645 0.5101 0.0482 0.029 Uiso 1 1 calc R . . H13A H -0.1914 0.5603 0.0188 0.029 Uiso 1 1 calc R . . C14 C -0.31689(12) 0.40388(7) 0.24242(7) 0.0188(2) Uani 1 1 d . . . C15 C -0.38118(13) 0.35964(8) 0.29362(8) 0.0213(3) Uani 1 1 d . A . C16 C -0.48305(14) 0.30911(8) 0.26820(9) 0.0253(3) Uani 1 1 d . . . H16 H -0.5095 0.3022 0.2182 0.030 Uiso 1 1 calc R A . C17 C -0.54598(15) 0.26873(9) 0.31639(10) 0.0312(3) Uani 1 1 d . A . H17 H -0.6151 0.2344 0.2990 0.037 Uiso 1 1 calc R . . C18 C -0.50831(16) 0.27839(9) 0.38903(10) 0.0325(3) Uani 1 1 d . . . H18 H -0.5522 0.2513 0.4215 0.039 Uiso 1 1 calc R A . C19 C -0.40625(16) 0.32769(10) 0.41483(9) 0.0315(3) Uani 1 1 d . A . H19 H -0.3799 0.3340 0.4650 0.038 Uiso 1 1 calc R . . C20 C -0.34274(14) 0.36782(9) 0.36745(8) 0.0267(3) Uani 1 1 d . . . H20 H -0.2724 0.4012 0.3854 0.032 Uiso 1 1 calc R A . C21 C -0.36424(13) 0.39554(8) 0.16431(7) 0.0208(2) Uani 1 1 d . A . C22 C -0.29986(16) 0.34774(9) 0.12305(9) 0.0307(3) Uani 1 1 d . . . H22 H -0.2254 0.3195 0.1448 0.037 Uiso 1 1 calc R A . C23 C -0.34434(19) 0.34122(11) 0.04985(10) 0.0394(4) Uani 1 1 d . A . H23 H -0.3000 0.3085 0.0217 0.047 Uiso 1 1 calc R . . C24 C -0.45177(19) 0.38174(11) 0.01831(9) 0.0385(4) Uani 1 1 d . . . H24 H -0.4813 0.3773 -0.0317 0.046 Uiso 1 1 calc R A . C25 C -0.51713(18) 0.42883(11) 0.05885(9) 0.0375(4) Uani 1 1 d . A . H25 H -0.5918 0.4567 0.0367 0.045 Uiso 1 1 calc R . . C26 C -0.47403(8) 0.43576(4) 0.13210(4) 0.0289(3) Uani 1 1 d . . . H26 H -0.5196 0.4680 0.1601 0.035 Uiso 1 1 calc R A . C3 C 0.10051(8) 0.37469(4) 0.28636(4) 0.0346(4) Uani 0.90 1 d PR A 1 H3 H 0.0379 0.3570 0.2474 0.042 Uiso 0.90 1 calc PR B 1 C4 C 0.09147(8) 0.36769(4) 0.36004(4) 0.0383(4) Uani 0.90 1 d PR A 1 H4 H 0.0217 0.3445 0.3791 0.046 Uiso 0.90 1 calc PR C 1 C5 C 0.20500(8) 0.40152(4) 0.40031(4) 0.0470(6) Uani 0.90 1 d PR A 1 H5 H 0.2245 0.4049 0.4510 0.056 Uiso 0.90 1 calc PR D 1 C6 C 0.28420(8) 0.42943(4) 0.35151(4) 0.0525(7) Uani 0.90 1 d PR A 1 H6 H 0.3660 0.4547 0.3638 0.063 Uiso 0.90 1 calc PR E 1 C7 C 0.21963(8) 0.41285(4) 0.28108(4) 0.0408(5) Uani 0.90 1 d PR A 1 H7 H 0.2507 0.4251 0.2380 0.049 Uiso 0.90 1 calc PR F 1 C3A C 0.09711(8) 0.36947(4) 0.29529(4) 0.0346(4) Uani 0.10 1 d PR A 2 H3A H 0.0200 0.3453 0.2713 0.042 Uiso 0.10 1 calc PR G 2 C4A C 0.13547(8) 0.37555(4) 0.37058(4) 0.0383(4) Uani 0.10 1 d PR A 2 H4A H 0.0886 0.3561 0.4058 0.046 Uiso 0.10 1 calc PR H 2 C5A C 0.25622(8) 0.41577(4) 0.38404(4) 0.0470(6) Uani 0.10 1 d PR A 2 H5A H 0.3043 0.4280 0.4298 0.056 Uiso 0.10 1 calc PR I 2 C6A C 0.29248(8) 0.43455(4) 0.31708(4) 0.0525(7) Uani 0.10 1 d PR A 2 H6A H 0.3691 0.4615 0.3102 0.063 Uiso 0.10 1 calc PR J 2 C7A C 0.19415(8) 0.40593(4) 0.26223(4) 0.0408(5) Uani 0.10 1 d PR A 2 H7A H 0.1934 0.4104 0.2122 0.049 Uiso 0.10 1 calc PR K 2 Cl1S Cl -0.45033(5) 0.55634(3) 0.43190(2) 0.04223(10) Uani 1 1 d . L 12 Cl2S Cl -0.51485(5) 0.58295(3) 0.27772(3) 0.04743(12) Uani 1 1 d . L 12 C1S C -0.38954(16) 0.57823(11) 0.35282(9) 0.0370(4) Uani 1 1 d . L 12 H1S2 H -0.3254 0.5386 0.3445 0.044 Uiso 1 1 calc R L 12 H1S1 H -0.3433 0.6281 0.3587 0.044 Uiso 1 1 calc R L 12 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 0.01609(9) 0.01882(9) 0.01637(9) 0.00266(6) 0.00027(7) -0.00067(6) Cl1 0.0399(2) 0.0599(3) 0.02547(19) 0.00656(18) -0.00027(16) 0.00494(19) Cl2 0.0355(2) 0.0432(2) 0.0410(2) -0.01264(17) 0.02038(17) -0.00564(16) Cl3 0.0634(3) 0.02424(18) 0.0406(2) -0.00499(15) 0.0188(2) -0.01099(17) Cl4 0.03548(18) 0.02923(17) 0.02130(16) -0.00695(12) 0.00752(13) 0.00060(14) P1 0.01402(14) 0.01699(14) 0.01486(14) 0.00211(11) 0.00171(11) -0.00165(11) Al1 0.0284(2) 0.0226(2) 0.01772(19) -0.00252(15) 0.00672(16) -0.00262(16) O1 0.0273(5) 0.0469(7) 0.0219(5) -0.0004(5) 0.0065(4) -0.0033(5) O2 0.0272(5) 0.0296(6) 0.0399(6) -0.0103(5) 0.0054(5) -0.0060(4) N1 0.0143(5) 0.0182(5) 0.0156(5) 0.0027(4) 0.0021(4) -0.0006(4) N2 0.0171(5) 0.0242(5) 0.0179(5) 0.0043(4) 0.0022(4) -0.0047(4) N3 0.0182(5) 0.0242(5) 0.0190(5) 0.0051(4) 0.0029(4) -0.0034(4) C1 0.0214(6) 0.0289(7) 0.0181(6) 0.0039(5) -0.0008(5) -0.0032(5) C2 0.0175(6) 0.0275(7) 0.0213(6) -0.0012(5) 0.0022(5) 0.0014(5) C8 0.0161(5) 0.0220(6) 0.0209(6) 0.0032(5) 0.0043(5) -0.0025(5) C9 0.0228(7) 0.0365(8) 0.0290(7) 0.0020(6) 0.0113(6) 0.0008(6) C10 0.0283(7) 0.0232(7) 0.0334(8) 0.0019(6) 0.0040(6) -0.0085(5) C11 0.0191(6) 0.0218(6) 0.0156(6) 0.0044(4) 0.0021(4) 0.0019(5) C12 0.0267(7) 0.0274(7) 0.0240(7) 0.0040(5) 0.0030(5) 0.0100(5) C13 0.0267(7) 0.0294(7) 0.0165(6) -0.0005(5) 0.0005(5) -0.0002(5) C14 0.0149(5) 0.0196(6) 0.0221(6) 0.0027(5) 0.0035(5) 0.0000(4) C15 0.0172(6) 0.0195(6) 0.0282(7) 0.0051(5) 0.0067(5) 0.0014(5) C16 0.0201(6) 0.0227(6) 0.0342(8) 0.0026(5) 0.0077(5) -0.0017(5) C17 0.0238(7) 0.0235(7) 0.0488(10) 0.0059(6) 0.0135(6) -0.0038(5) C18 0.0282(7) 0.0283(7) 0.0446(9) 0.0150(7) 0.0162(7) 0.0016(6) C19 0.0312(8) 0.0350(8) 0.0297(8) 0.0120(6) 0.0095(6) 0.0013(6) C20 0.0233(7) 0.0292(7) 0.0281(7) 0.0070(6) 0.0059(5) -0.0021(5) C21 0.0183(6) 0.0213(6) 0.0226(6) -0.0001(5) 0.0029(5) -0.0052(5) C22 0.0293(7) 0.0304(7) 0.0334(8) -0.0041(6) 0.0078(6) 0.0006(6) C23 0.0483(10) 0.0392(9) 0.0335(9) -0.0129(7) 0.0148(8) -0.0091(8) C24 0.0459(10) 0.0442(9) 0.0236(7) -0.0057(7) 0.0007(7) -0.0188(8) C25 0.0326(8) 0.0459(10) 0.0296(8) 0.0029(7) -0.0072(6) -0.0038(7) C26 0.0245(7) 0.0336(8) 0.0269(7) -0.0005(6) -0.0007(6) 0.0020(6) C3 0.0411(9) 0.0240(7) 0.0356(9) -0.0061(6) -0.0031(7) 0.0082(6) C4 0.0490(12) 0.0188(7) 0.0518(11) 0.0073(7) 0.0219(9) -0.0015(7) C5 0.0767(16) 0.0282(9) 0.0281(9) 0.0045(7) -0.0148(10) 0.0193(10) C6 0.0222(8) 0.0249(8) 0.103(2) 0.0012(11) -0.0107(11) 0.0069(7) C7 0.0479(11) 0.0301(8) 0.0511(12) 0.0149(8) 0.0274(10) 0.0205(8) C3A 0.0411(9) 0.0240(7) 0.0356(9) -0.0061(6) -0.0031(7) 0.0082(6) C4A 0.0490(12) 0.0188(7) 0.0518(11) 0.0073(7) 0.0219(9) -0.0015(7) C5A 0.0767(16) 0.0282(9) 0.0281(9) 0.0045(7) -0.0148(10) 0.0193(10) C6A 0.0222(8) 0.0249(8) 0.103(2) 0.0012(11) -0.0107(11) 0.0069(7) C7A 0.0479(11) 0.0301(8) 0.0511(12) 0.0149(8) 0.0274(10) 0.0205(8) Cl1S 0.0413(2) 0.0535(3) 0.0320(2) -0.00179(18) 0.00644(17) -0.01084(19) Cl2S 0.0349(2) 0.0710(3) 0.0352(2) 0.0051(2) 0.00237(17) 0.0094(2) C1S 0.0276(8) 0.0499(10) 0.0337(8) -0.0084(7) 0.0060(6) -0.0097(7) _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 C2 1.7970(14) . ? Fe1 C1 1.8002(15) . ? Fe1 C4A 2.0325 . ? Fe1 C5 2.0876 . ? Fe1 C6 2.0908 . ? Fe1 C5A 2.0909 . ? Fe1 C4 2.1043 . ? Fe1 C7 2.1094 . ? Fe1 C3 2.1177 . ? Fe1 C3A 2.1353 . ? Fe1 P1 2.1691(4) . ? Fe1 C6A 2.2246 . ? Cl1 Al1 2.1324(6) . ? Cl2 Al1 2.1236(6) . ? Cl3 Al1 2.1217(6) . ? Cl4 Al1 2.1400(5) . ? P1 N2 1.5748(11) . ? P1 N1 1.6237(11) . ? O1 C1 1.1316(18) . ? O2 C2 1.1312(18) . ? N1 C8 1.4911(16) . ? N1 C11 1.5053(16) . ? N2 N3 1.4033(15) . ? N3 C14 1.2955(17) . ? C8 C10 1.5225(19) . ? C8 C9 1.526(2) . ? C11 C13 1.5170(19) . ? C11 C12 1.5225(19) . ? C14 C15 1.4814(18) . ? C14 C21 1.4871(19) . ? C15 C20 1.397(2) . ? C15 C16 1.3980(19) . ? C16 C17 1.397(2) . ? C17 C18 1.377(3) . ? C18 C19 1.388(2) . ? C19 C20 1.387(2) . ? C21 C22 1.387(2) . ? C21 C26 1.3888(15) . ? C22 C23 1.392(2) . ? C23 C24 1.369(3) . ? C24 C25 1.377(3) . ? C25 C26 1.3912(19) . ? C3 C7 1.4200 . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C5 C6 1.4200 . ? C6 C7 1.4200 . ? C3A C4A 1.4200 . ? C3A C7A 1.4200 . ? C4A C5A 1.4200 . ? C5A C6A 1.4200 . ? C6A C7A 1.4200 . ? Cl1S C1S 1.7607(18) . ? Cl2S C1S 1.7620(18) . ? 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 C2 Fe1 C1 92.21(6) . . ? C2 Fe1 C4A 134.59(5) . . ? C1 Fe1 C4A 94.04(5) . . ? C2 Fe1 C5 107.90(5) . . ? C1 Fe1 C5 96.54(5) . . ? C4A Fe1 C5 26.7 . . ? C2 Fe1 C6 90.31(5) . . ? C1 Fe1 C6 133.79(5) . . ? C4A Fe1 C6 54.5 . . ? C5 Fe1 C6 39.7 . . ? C2 Fe1 C5A 96.82(5) . . ? C1 Fe1 C5A 113.37(5) . . ? C4A Fe1 C5A 40.3 . . ? C5 Fe1 C5A 19.3 . . ? C6 Fe1 C5A 21.0 . . ? C2 Fe1 C4 147.16(5) . . ? C1 Fe1 C4 88.52(5) . . ? C4A Fe1 C4 13.3 . . ? C5 Fe1 C4 39.6 . . ? C6 Fe1 C4 66.4 . . ? C5A Fe1 C4 53.5 . . ? C2 Fe1 C7 110.76(5) . . ? C1 Fe1 C7 154.40(5) . . ? C4A Fe1 C7 62.0 . . ? C5 Fe1 C7 66.4 . . ? C6 Fe1 C7 39.5 . . ? C5A Fe1 C7 54.6 . . ? C4 Fe1 C7 66.1 . . ? C2 Fe1 C3 149.98(5) . . ? C1 Fe1 C3 117.40(5) . . ? C4A Fe1 C3 44.6 . . ? C5 Fe1 C3 66.2 . . ? C6 Fe1 C3 66.2 . . ? C5A Fe1 C3 68.1 . . ? C4 Fe1 C3 39.3 . . ? C7 Fe1 C3 39.3 . . ? C2 Fe1 C3A 153.02(5) . . ? C1 Fe1 C3A 113.31(5) . . ? C4A Fe1 C3A 39.7 . . ? C5 Fe1 C3A 62.4 . . ? C6 Fe1 C3A 66.0 . . ? C5A Fe1 C3A 65.9 . . ? C4 Fe1 C3A 34.0 . . ? C7 Fe1 C3A 42.5 . . ? C3 Fe1 C3A 5.4 . . ? C2 Fe1 P1 97.23(5) . . ? C1 Fe1 P1 91.70(4) . . ? C4A Fe1 P1 127.42(3) . . ? C5 Fe1 P1 153.14(3) . . ? C6 Fe1 P1 133.66(3) . . ? C5A Fe1 P1 150.64(3) . . ? C4 Fe1 P1 115.57(2) . . ? C7 Fe1 P1 96.27(2) . . ? C3 Fe1 P1 87.28(2) . . ? C3A Fe1 P1 90.88(2) . . ? C2 Fe1 C6A 89.89(5) . . ? C1 Fe1 C6A 151.50(5) . . ? C4A Fe1 C6A 65.1 . . ? C5 Fe1 C6A 56.0 . . ? C6 Fe1 C6A 17.7 . . ? C5A Fe1 C6A 38.3 . . ? C4 Fe1 C6A 74.8 . . ? C7 Fe1 C6A 26.6 . . ? C3 Fe1 C6A 61.9 . . ? C3A Fe1 C6A 63.6 . . ? P1 Fe1 C6A 116.22(2) . . ? N2 P1 N1 108.96(6) . . ? N2 P1 Fe1 124.59(4) . . ? N1 P1 Fe1 126.19(4) . . ? Cl3 Al1 Cl2 110.34(3) . . ? Cl3 Al1 Cl1 109.37(3) . . ? Cl2 Al1 Cl1 110.18(3) . . ? Cl3 Al1 Cl4 108.68(2) . . ? Cl2 Al1 Cl4 109.04(2) . . ? Cl1 Al1 Cl4 109.19(3) . . ? C8 N1 C11 116.14(10) . . ? C8 N1 P1 119.41(8) . . ? C11 N1 P1 124.45(8) . . ? N3 N2 P1 114.45(9) . . ? C14 N3 N2 113.36(11) . . ? O1 C1 Fe1 176.54(13) . . ? O2 C2 Fe1 178.10(14) . . ? N1 C8 C10 111.53(11) . . ? N1 C8 C9 111.22(11) . . ? C10 C8 C9 112.36(12) . . ? N1 C11 C13 112.75(11) . . ? N1 C11 C12 111.79(11) . . ? C13 C11 C12 112.43(12) . . ? N3 C14 C15 117.68(12) . . ? N3 C14 C21 122.93(12) . . ? C15 C14 C21 119.39(11) . . ? C20 C15 C16 118.90(13) . . ? C20 C15 C14 121.20(12) . . ? C16 C15 C14 119.90(13) . . ? C17 C16 C15 120.00(15) . . ? C18 C17 C16 120.38(15) . . ? C17 C18 C19 120.08(14) . . ? C20 C19 C18 120.00(16) . . ? C19 C20 C15 120.62(14) . . ? C22 C21 C26 119.42(13) . . ? C22 C21 C14 120.64(13) . . ? C26 C21 C14 119.93(11) . . ? C21 C22 C23 120.01(16) . . ? C24 C23 C22 120.24(16) . . ? C23 C24 C25 120.25(16) . . ? C24 C25 C26 120.15(15) . . ? C21 C26 C25 119.92(11) . . ? C7 C3 C4 108.0 . . ? C7 C3 Fe1 70.1 . . ? C4 C3 Fe1 69.8 . . ? C5 C4 C3 108.0 . . ? C5 C4 Fe1 69.6 . . ? C3 C4 Fe1 70.9 . . ? C4 C5 C6 108.0 . . ? C4 C5 Fe1 70.8 . . ? C6 C5 Fe1 70.3 . . ? C5 C6 C7 108.0 . . ? C5 C6 Fe1 70.0 . . ? C7 C6 Fe1 70.9 . . ? C6 C7 C3 108.0 . . ? C6 C7 Fe1 69.5 . . ? C3 C7 Fe1 70.7 . . ? C4A C3A C7A 108.0 . . ? C4A C3A Fe1 66.2 . . ? C7A C3A Fe1 75.6 . . ? C3A C4A C5A 108.0 . . ? C3A C4A Fe1 74.0 . . ? C5A C4A Fe1 72.1 . . ? C6A C5A C4A 108.0 . . ? C6A C5A Fe1 76.0 . . ? C4A C5A Fe1 67.7 . . ? C5A C6A C7A 108.0 . . ? C5A C6A Fe1 65.8 . . ? C7A C6A Fe1 72.5 . . ? C6A C7A C3A 108.0 . . ? C6A C7A Fe1 70.5 . . ? C3A C7A Fe1 66.8 . . ? Cl1S C1S Cl2S 112.21(9) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 29.59 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.905 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.057 # Attachment 'tg46 Compound 9.cif' data_tg46 _database_code_depnum_ccdc_archive 'CCDC 283077' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H29 Al Cl4 Fe N O2 P Si' _chemical_formula_weight 563.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.7258(7) _cell_length_b 11.0115(7) _cell_length_c 11.2248(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.9410(10) _cell_angle_gamma 90.00 _cell_volume 1325.55(15) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 1.124 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.6034 _exptl_absorpt_correction_T_max 0.8064 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16380 _diffrn_reflns_av_R_equivalents 0.0152 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 29.56 _reflns_number_total 6824 _reflns_number_gt 6628 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\\s^2^(Fo^2^)+(0.0545P)^2^+0.8488P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.043(15) _refine_ls_number_reflns 6824 _refine_ls_number_parameters 373 _refine_ls_number_restraints 134 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.1068 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.7690(2) 0.5524(3) 1.2542(2) 0.0272(3) Uani 0.69 1 d PD A 1 Cl1 Cl 0.7842(2) 0.72883(14) 1.17913(15) 0.0495(4) Uani 0.69 1 d PD A 1 Cl2 Cl 0.6264(2) 0.5445(3) 1.3799(2) 0.0843(8) Uani 0.69 1 d PD A 1 Cl3 Cl 0.93967(19) 0.5091(3) 1.3490(3) 0.0474(4) Uani 0.69 1 d PD A 1 Cl4 Cl 0.7410(2) 0.42536(18) 1.1132(2) 0.0648(5) Uani 0.69 1 d PD A 1 Al1A Al 0.7790(14) 0.5547(15) 1.2675(15) 0.0272(3) Uani 0.12 1 d PD B 2 Cl1A Cl 0.7790(15) 0.7086(11) 1.1552(12) 0.0495(4) Uani 0.12 1 d PD B 2 Cl2A Cl 0.6418(16) 0.583(2) 1.3931(17) 0.0843(8) Uani 0.12 1 d PD B 2 Cl3A Cl 0.9680(7) 0.5330(8) 1.3092(7) 0.0474(4) Uani 0.12 1 d PD B 2 Cl4A Cl 0.7162(11) 0.4088(10) 1.1611(10) 0.0648(5) Uani 0.12 1 d PD B 2 Al1B Al 0.7988(13) 0.5590(16) 1.2532(14) 0.0272(3) Uani 0.07 1 d PD C 3 Cl1B Cl 0.7457(15) 0.4862(12) 1.0933(11) 0.0495(4) Uani 0.07 1 d PD C 3 Cl2B Cl 0.7534(14) 0.4437(19) 1.3986(13) 0.0843(8) Uani 0.07 1 d PD C 3 Cl3B Cl 0.9898(8) 0.5632(11) 1.2300(10) 0.0474(4) Uani 0.07 1 d PD C 3 Cl4B Cl 0.7054(14) 0.7253(13) 1.2896(15) 0.0648(5) Uani 0.07 1 d PD C 3 Al1C Al 0.7865(15) 0.5436(14) 1.2618(14) 0.0272(3) Uani 0.12 1 d PD D 4 Cl1C Cl 0.7332(8) 0.7321(6) 1.2414(8) 0.0495(4) Uani 0.12 1 d PD D 4 Cl2C Cl 0.6763(9) 0.4539(13) 1.3928(9) 0.0843(8) Uani 0.12 1 d PD D 4 Cl3C Cl 0.9590(14) 0.505(2) 1.3477(19) 0.0474(4) Uani 0.12 1 d PD D 4 Cl4C Cl 0.7216(15) 0.4541(14) 1.1028(15) 0.0648(5) Uani 0.12 1 d PD D 4 Fe1 Fe 0.02098(4) 0.53630(5) 0.76759(3) 0.02925(10) Uani 0.87 1 d PD E 11 P1 P 0.22649(7) 0.55538(7) 0.76806(5) 0.02492(13) Uani 0.87 1 d PD E 11 Si1 Si 0.30266(9) 0.58377(10) 1.04983(7) 0.0396(2) Uani 0.87 1 d PD E 11 O1 O 0.0325(3) 0.3961(4) 0.9869(3) 0.0694(10) Uani 0.87 1 d PD E 11 O2 O 0.0028(3) 0.3248(2) 0.6123(3) 0.0497(7) Uani 0.87 1 d PD E 11 N1 N 0.30147(19) 0.5527(3) 0.64138(19) 0.0292(4) Uani 0.87 1 d PD E 11 C1 C 0.3162(3) 0.5689(3) 0.8856(2) 0.0368(6) Uani 0.87 1 d PD E 11 H1 H 0.4013 0.5694 0.8636 0.044 Uiso 0.87 1 calc PR E 11 C2 C 0.1532(5) 0.6575(6) 1.0947(4) 0.0714(15) Uani 0.87 1 d PD E 11 H2A H 0.0863 0.5969 1.0942 0.086 Uiso 0.87 1 calc PR E 11 H2B H 0.1321 0.7226 1.0383 0.086 Uiso 0.87 1 calc PR E 11 H2C H 0.1630 0.6915 1.1749 0.086 Uiso 0.87 1 calc PR E 11 C3 C 0.3279(5) 0.4331(4) 1.1193(4) 0.0631(12) Uani 0.87 1 d PD E 11 H3A H 0.3940 0.3901 1.0773 0.076 Uiso 0.87 1 calc PR E 11 H3B H 0.2505 0.3859 1.1141 0.076 Uiso 0.87 1 calc PR E 11 H3C H 0.3525 0.4437 1.2031 0.076 Uiso 0.87 1 calc PR E 11 C4 C 0.4317(5) 0.6856(5) 1.0966(4) 0.0699(14) Uani 0.87 1 d PD E 11 H4A H 0.4426 0.6819 1.1834 0.084 Uiso 0.87 1 calc PR E 11 H4B H 0.4119 0.7691 1.0727 0.084 Uiso 0.87 1 calc PR E 11 H4C H 0.5089 0.6598 1.0586 0.084 Uiso 0.87 1 calc PR E 11 C5 C 0.4399(2) 0.5558(4) 0.6313(3) 0.0413(7) Uani 0.87 1 d PD E 11 H5 H 0.4554 0.5507 0.5438 0.050 Uiso 0.87 1 calc PR E 11 C6 C 0.5036(4) 0.4424(4) 0.6844(4) 0.0517(10) Uani 0.87 1 d PD E 11 H6A H 0.4963 0.4435 0.7713 0.062 Uiso 0.87 1 calc PR E 11 H6B H 0.5919 0.4423 0.6633 0.062 Uiso 0.87 1 calc PR E 11 H6C H 0.4632 0.3693 0.6523 0.062 Uiso 0.87 1 calc PR E 11 C7 C 0.4980(4) 0.6744(4) 0.6698(7) 0.0528(10) Uani 0.87 1 d PD E 11 H7A H 0.4529 0.7419 0.6318 0.063 Uiso 0.87 1 calc PR E 11 H7B H 0.5855 0.6763 0.6460 0.063 Uiso 0.87 1 calc PR E 11 H7C H 0.4934 0.6822 0.7566 0.063 Uiso 0.87 1 calc PR E 11 C8 C 0.2323(3) 0.5420(4) 0.5266(2) 0.0398(7) Uani 0.87 1 d PD E 11 H8 H 0.1414 0.5424 0.5450 0.048 Uiso 0.87 1 calc PR E 11 C9 C 0.2573(4) 0.6529(5) 0.4480(4) 0.0652(15) Uani 0.87 1 d PD E 11 H9A H 0.2399 0.7272 0.4929 0.078 Uiso 0.87 1 calc PR E 11 H9B H 0.2031 0.6497 0.3769 0.078 Uiso 0.87 1 calc PR E 11 H9C H 0.3447 0.6527 0.4241 0.078 Uiso 0.87 1 calc PR E 11 C10 C 0.2599(4) 0.4219(5) 0.4648(4) 0.0591(13) Uani 0.87 1 d PD E 11 H10A H 0.3457 0.4226 0.4361 0.071 Uiso 0.87 1 calc PR E 11 H10B H 0.2020 0.4109 0.3972 0.071 Uiso 0.87 1 calc PR E 11 H10C H 0.2498 0.3549 0.5214 0.071 Uiso 0.87 1 calc PR E 11 C11 C 0.0308(3) 0.4483(4) 0.9003(3) 0.0453(8) Uani 0.87 1 d PD E 11 C12 C 0.0169(3) 0.4074(3) 0.6730(3) 0.0360(6) Uani 0.87 1 d PD E 11 C13 C -0.0039(3) 0.7232(3) 0.7949(3) 0.0427(7) Uani 0.87 1 d PD E 11 H13 H 0.0573 0.7759 0.8287 0.051 Uiso 0.87 1 calc PR E 11 C14 C -0.0205(5) 0.6940(4) 0.6727(3) 0.0628(14) Uani 0.87 1 d PD E 11 H14 H 0.0281 0.7241 0.6092 0.075 Uiso 0.87 1 calc PR E 11 C15 C -0.1214(5) 0.6130(5) 0.6616(4) 0.0736(16) Uani 0.87 1 d PD E 11 H15 H -0.1530 0.5804 0.5888 0.088 Uiso 0.87 1 calc PR E 11 C16 C -0.1680(4) 0.5877(5) 0.7754(4) 0.0622(12) Uani 0.87 1 d PD E 11 H16 H -0.2343 0.5342 0.7942 0.075 Uiso 0.87 1 calc PR E 11 C17 C -0.0960(3) 0.6584(4) 0.8563(3) 0.0455(8) Uani 0.87 1 d PD E 11 H17 H -0.1080 0.6616 0.9399 0.055 Uiso 0.87 1 calc PR E 11 Fe1A Fe -0.0206(3) 0.5315(4) 0.7525(3) 0.02925(10) Uani 0.13 1 d PD F 12 P1A P 0.1799(3) 0.5649(5) 0.7901(3) 0.02492(13) Uani 0.13 1 d PD F 12 Si1A Si 0.3665(6) 0.5950(6) 1.0298(5) 0.0396(2) Uani 0.13 1 d PD F 12 O1A O -0.027(3) 0.3691(18) 0.9564(16) 0.0694(10) Uani 0.13 1 d PD F 12 O2A O 0.033(2) 0.3438(15) 0.5797(16) 0.0497(7) Uani 0.13 1 d PD F 12 N1A N 0.2806(6) 0.5722(14) 0.6818(6) 0.0292(4) Uani 0.13 1 d PD F 12 C1A C 0.2361(8) 0.5873(16) 0.9219(6) 0.0368(6) Uani 0.13 1 d PD F 12 H1A H 0.1651 0.6065 0.9677 0.044 Uiso 0.13 1 calc PR F 12 C2A C 0.3414(19) 0.7190(15) 1.1422(14) 0.0714(15) Uani 0.13 1 d PD F 12 H2A1 H 0.4151 0.7257 1.1945 0.086 Uiso 0.13 1 calc PR F 12 H2A2 H 0.2684 0.6996 1.1900 0.086 Uiso 0.13 1 calc PR F 12 H2A3 H 0.3276 0.7963 1.1008 0.086 Uiso 0.13 1 calc PR F 12 C3A C 0.387(2) 0.4439(11) 1.1003(19) 0.0631(12) Uani 0.13 1 d PD F 12 H3A1 H 0.4607 0.4040 1.0675 0.076 Uiso 0.13 1 calc PR F 12 H3A2 H 0.3132 0.3940 1.0842 0.076 Uiso 0.13 1 calc PR F 12 H3A3 H 0.3986 0.4539 1.1866 0.076 Uiso 0.13 1 calc PR F 12 C4A C 0.5091(11) 0.633(2) 0.9480(14) 0.0699(14) Uani 0.13 1 d PD F 12 H4A1 H 0.5387 0.5606 0.9061 0.084 Uiso 0.13 1 calc PR F 12 H4A2 H 0.5737 0.6608 1.0044 0.084 Uiso 0.13 1 calc PR F 12 H4A3 H 0.4907 0.6973 0.8901 0.084 Uiso 0.13 1 calc PR F 12 C5A C 0.4180(7) 0.5756(14) 0.7028(12) 0.0413(7) Uani 0.13 1 d PD F 12 H5A H 0.4277 0.5740 0.7916 0.050 Uiso 0.13 1 calc PR F 12 C6A C 0.4848(18) 0.460(2) 0.662(3) 0.0517(10) Uani 0.13 1 d PD F 12 H6A1 H 0.5014 0.4072 0.7304 0.062 Uiso 0.13 1 calc PR F 12 H6A2 H 0.5637 0.4818 0.6245 0.062 Uiso 0.13 1 calc PR F 12 H6A3 H 0.4317 0.4167 0.6036 0.062 Uiso 0.13 1 calc PR F 12 C7A C 0.4799(18) 0.692(2) 0.667(5) 0.0528(10) Uani 0.13 1 d PD F 12 H7A1 H 0.5382 0.6763 0.6023 0.063 Uiso 0.13 1 calc PR F 12 H7A2 H 0.5254 0.7266 0.7353 0.063 Uiso 0.13 1 calc PR F 12 H7A3 H 0.4164 0.7503 0.6391 0.063 Uiso 0.13 1 calc PR F 12 C8A C 0.2371(12) 0.5768(14) 0.5564(7) 0.0398(7) Uani 0.13 1 d PD F 12 H8A H 0.1449 0.5642 0.5587 0.048 Uiso 0.13 1 calc PR F 12 C9A C 0.255(3) 0.7023(17) 0.5013(17) 0.0652(15) Uani 0.13 1 d PD F 12 H9A1 H 0.2410 0.7649 0.5616 0.078 Uiso 0.13 1 calc PR F 12 H9A2 H 0.1961 0.7132 0.4348 0.078 Uiso 0.13 1 calc PR F 12 H9A3 H 0.3406 0.7094 0.4721 0.078 Uiso 0.13 1 calc PR F 12 C10A C 0.287(3) 0.473(2) 0.4814(15) 0.0591(13) Uani 0.13 1 d PD F 12 H10D H 0.3669 0.4974 0.4471 0.071 Uiso 0.13 1 calc PR F 12 H10E H 0.2273 0.4546 0.4171 0.071 Uiso 0.13 1 calc PR F 12 H10F H 0.2995 0.4014 0.5316 0.071 Uiso 0.13 1 calc PR F 12 C11A C -0.0279(10) 0.4394(10) 0.8826(9) 0.0453(8) Uani 0.13 1 d PD F 12 C12A C 0.0016(10) 0.4066(8) 0.6557(10) 0.0360(6) Uani 0.13 1 d PD F 12 C13A C -0.0609(10) 0.7162(6) 0.7780(11) 0.0427(7) Uani 0.13 1 d PD F 12 H13A H -0.0091 0.7716 0.8209 0.051 Uiso 0.13 1 calc PR F 12 C14A C -0.0560(10) 0.6890(8) 0.6549(10) 0.0628(14) Uani 0.13 1 d PD F 12 H14A H 0.0003 0.7230 0.5997 0.075 Uiso 0.13 1 calc PR F 12 C15A C -0.1492(9) 0.6029(12) 0.6287(9) 0.0736(16) Uani 0.13 1 d PD F 12 H15A H -0.1672 0.5703 0.5519 0.088 Uiso 0.13 1 calc PR F 12 C16A C -0.2117(6) 0.5723(11) 0.7336(11) 0.0622(12) Uani 0.13 1 d PD F 12 H16A H -0.2770 0.5148 0.7417 0.075 Uiso 0.13 1 calc PR F 12 C17A C -0.1576(8) 0.6449(10) 0.8244(10) 0.0455(8) Uani 0.13 1 d PD F 12 H17A H -0.1828 0.6454 0.9052 0.055 Uiso 0.13 1 calc PR F 12 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 Al1 0.0242(7) 0.0266(5) 0.0310(6) -0.0024(5) 0.0008(5) -0.0001(5) Cl1 0.0596(6) 0.0330(7) 0.0554(10) 0.0099(6) -0.0170(6) -0.0107(6) Cl2 0.0572(8) 0.134(2) 0.0627(8) 0.0184(13) 0.0366(7) 0.0075(12) Cl3 0.0395(9) 0.0458(6) 0.0564(6) 0.0025(4) -0.0125(7) 0.0090(7) Cl4 0.0716(11) 0.0535(11) 0.0689(9) -0.0368(10) -0.0135(8) 0.0130(7) Al1A 0.0242(7) 0.0266(5) 0.0310(6) -0.0024(5) 0.0008(5) -0.0001(5) Cl1A 0.0596(6) 0.0330(7) 0.0554(10) 0.0099(6) -0.0170(6) -0.0107(6) Cl2A 0.0572(8) 0.134(2) 0.0627(8) 0.0184(13) 0.0366(7) 0.0075(12) Cl3A 0.0395(9) 0.0458(6) 0.0564(6) 0.0025(4) -0.0125(7) 0.0090(7) Cl4A 0.0716(11) 0.0535(11) 0.0689(9) -0.0368(10) -0.0135(8) 0.0130(7) Al1B 0.0242(7) 0.0266(5) 0.0310(6) -0.0024(5) 0.0008(5) -0.0001(5) Cl1B 0.0596(6) 0.0330(7) 0.0554(10) 0.0099(6) -0.0170(6) -0.0107(6) Cl2B 0.0572(8) 0.134(2) 0.0627(8) 0.0184(13) 0.0366(7) 0.0075(12) Cl3B 0.0395(9) 0.0458(6) 0.0564(6) 0.0025(4) -0.0125(7) 0.0090(7) Cl4B 0.0716(11) 0.0535(11) 0.0689(9) -0.0368(10) -0.0135(8) 0.0130(7) Al1C 0.0242(7) 0.0266(5) 0.0310(6) -0.0024(5) 0.0008(5) -0.0001(5) Cl1C 0.0596(6) 0.0330(7) 0.0554(10) 0.0099(6) -0.0170(6) -0.0107(6) Cl2C 0.0572(8) 0.134(2) 0.0627(8) 0.0184(13) 0.0366(7) 0.0075(12) Cl3C 0.0395(9) 0.0458(6) 0.0564(6) 0.0025(4) -0.0125(7) 0.0090(7) Cl4C 0.0716(11) 0.0535(11) 0.0689(9) -0.0368(10) -0.0135(8) 0.0130(7) Fe1 0.0300(2) 0.0340(2) 0.02366(16) 0.00103(15) -0.00327(14) 0.0001(2) P1 0.0298(3) 0.0240(3) 0.0208(3) -0.0017(2) -0.0042(2) 0.0002(3) Si1 0.0432(5) 0.0525(5) 0.0231(3) -0.0005(3) -0.0050(3) 0.0063(4) O1 0.069(2) 0.089(2) 0.0504(16) 0.0319(17) -0.0024(15) -0.0161(19) O2 0.0642(19) 0.0277(12) 0.0564(17) -0.0042(11) -0.0183(13) -0.0084(11) N1 0.0269(9) 0.0381(13) 0.0226(9) -0.0017(10) -0.0024(7) 0.0033(10) C1 0.0361(12) 0.0482(18) 0.0259(11) -0.0035(11) -0.0067(9) -0.0036(12) C2 0.070(3) 0.111(4) 0.0326(17) -0.015(2) -0.0024(17) 0.032(3) C3 0.078(3) 0.065(3) 0.046(2) 0.0185(18) -0.010(2) 0.002(2) C4 0.085(3) 0.070(3) 0.053(2) -0.009(2) -0.034(2) -0.017(3) C5 0.0280(11) 0.061(2) 0.0344(12) 0.0039(15) 0.0006(10) 0.0016(15) C6 0.0396(18) 0.059(2) 0.056(3) 0.0058(19) -0.0065(16) 0.0175(16) C7 0.0393(18) 0.057(2) 0.062(2) 0.013(2) -0.001(2) -0.0044(17) C8 0.0339(11) 0.064(2) 0.0216(11) -0.0051(14) -0.0044(9) 0.0030(16) C9 0.046(2) 0.117(4) 0.0327(19) 0.033(2) -0.0037(17) -0.005(2) C10 0.0395(19) 0.095(4) 0.0429(19) -0.034(2) -0.0001(15) 0.007(2) C11 0.0388(17) 0.060(2) 0.0373(16) 0.0131(15) -0.0017(13) -0.0070(16) C12 0.0350(14) 0.0314(13) 0.0413(15) 0.0041(11) -0.0129(12) -0.0037(11) C13 0.0397(17) 0.0371(15) 0.0515(18) -0.0012(13) 0.0080(15) 0.0127(14) C14 0.085(3) 0.064(2) 0.0399(17) 0.0178(16) 0.0173(19) 0.051(2) C15 0.088(3) 0.082(3) 0.049(2) -0.031(2) -0.042(2) 0.054(3) C16 0.0411(19) 0.070(3) 0.075(3) -0.031(2) -0.0142(17) 0.0093(19) C17 0.0407(17) 0.059(2) 0.0374(16) -0.0114(15) 0.0097(13) 0.0028(16) Fe1A 0.0300(2) 0.0340(2) 0.02366(16) 0.00103(15) -0.00327(14) 0.0001(2) P1A 0.0298(3) 0.0240(3) 0.0208(3) -0.0017(2) -0.0042(2) 0.0002(3) Si1A 0.0432(5) 0.0525(5) 0.0231(3) -0.0005(3) -0.0050(3) 0.0063(4) O1A 0.069(2) 0.089(2) 0.0504(16) 0.0319(17) -0.0024(15) -0.0161(19) O2A 0.0642(19) 0.0277(12) 0.0564(17) -0.0042(11) -0.0183(13) -0.0084(11) N1A 0.0269(9) 0.0381(13) 0.0226(9) -0.0017(10) -0.0024(7) 0.0033(10) C1A 0.0361(12) 0.0482(18) 0.0259(11) -0.0035(11) -0.0067(9) -0.0036(12) C2A 0.070(3) 0.111(4) 0.0326(17) -0.015(2) -0.0024(17) 0.032(3) C3A 0.078(3) 0.065(3) 0.046(2) 0.0185(18) -0.010(2) 0.002(2) C4A 0.085(3) 0.070(3) 0.053(2) -0.009(2) -0.034(2) -0.017(3) C5A 0.0280(11) 0.061(2) 0.0344(12) 0.0039(15) 0.0006(10) 0.0016(15) C6A 0.0396(18) 0.059(2) 0.056(3) 0.0058(19) -0.0065(16) 0.0175(16) C7A 0.0393(18) 0.057(2) 0.062(2) 0.013(2) -0.001(2) -0.0044(17) C8A 0.0339(11) 0.064(2) 0.0216(11) -0.0051(14) -0.0044(9) 0.0030(16) C9A 0.046(2) 0.117(4) 0.0327(19) 0.033(2) -0.0037(17) -0.005(2) C10A 0.0395(19) 0.095(4) 0.0429(19) -0.034(2) -0.0001(15) 0.007(2) C11A 0.0388(17) 0.060(2) 0.0373(16) 0.0131(15) -0.0017(13) -0.0070(16) C12A 0.0350(14) 0.0314(13) 0.0413(15) 0.0041(11) -0.0129(12) -0.0037(11) C13A 0.0397(17) 0.0371(15) 0.0515(18) -0.0012(13) 0.0080(15) 0.0127(14) C14A 0.085(3) 0.064(2) 0.0399(17) 0.0178(16) 0.0173(19) 0.051(2) C15A 0.088(3) 0.082(3) 0.049(2) -0.031(2) -0.042(2) 0.054(3) C16A 0.0411(19) 0.070(3) 0.075(3) -0.031(2) -0.0142(17) 0.0093(19) C17A 0.0407(17) 0.059(2) 0.0374(16) -0.0114(15) 0.0097(13) 0.0028(16) _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 Al1 Cl2 2.100(3) . ? Al1 Cl1 2.125(3) . ? Al1 Cl4 2.130(3) . ? Al1 Cl3 2.155(3) . ? Al1A Cl2A 2.078(16) . ? Al1A Cl3A 2.086(15) . ? Al1A Cl4A 2.106(16) . ? Al1A Cl1A 2.113(16) . ? Al1B Cl1B 2.038(16) . ? Al1B Cl3B 2.070(14) . ? Al1B Cl4B 2.130(16) . ? Al1B Cl2B 2.131(16) . ? Al1C Cl3C 2.116(16) . ? Al1C Cl2C 2.143(16) . ? Al1C Cl4C 2.145(16) . ? Al1C Cl1C 2.164(15) . ? Fe1 C12 1.773(3) . ? Fe1 C11 1.779(3) . ? Fe1 C14 2.082(4) . ? Fe1 C15 2.098(4) . ? Fe1 C13 2.098(3) . ? Fe1 C17 2.101(3) . ? Fe1 C16 2.108(4) . ? Fe1 P1 2.2141(8) . ? P1 C1 1.627(3) . ? P1 N1 1.645(2) . ? Si1 C3 1.851(4) . ? Si1 C4 1.851(4) . ? Si1 C1 1.859(3) . ? Si1 C2 1.873(4) . ? O1 C11 1.130(4) . ? O2 C12 1.145(4) . ? N1 C8 1.481(3) . ? N1 C5 1.491(3) . ? C5 C7 1.508(6) . ? C5 C6 1.538(5) . ? C8 C10 1.525(6) . ? C8 C9 1.532(5) . ? C13 C17 1.408(5) . ? C13 C14 1.417(5) . ? C14 C15 1.406(8) . ? C15 C16 1.407(7) . ? C16 C17 1.415(5) . ? Fe1A C12A 1.771(5) . ? Fe1A C11A 1.781(5) . ? Fe1A C14A 2.083(5) . ? Fe1A C15A 2.095(6) . ? Fe1A C17A 2.100(5) . ? Fe1A C13A 2.100(5) . ? Fe1A C16A 2.106(6) . ? Fe1A P1A 2.216(3) . ? P1A C1A 1.607(5) . ? P1A N1A 1.641(5) . ? Si1A C1A 1.837(5) . ? Si1A C4A 1.844(7) . ? Si1A C3A 1.855(6) . ? Si1A C2A 1.882(6) . ? O1A C11A 1.134(6) . ? O2A C12A 1.153(6) . ? N1A C8A 1.476(6) . ? N1A C5A 1.489(6) . ? C5A C7A 1.506(8) . ? C5A C6A 1.537(7) . ? C8A C10A 1.519(7) . ? C8A C9A 1.528(7) . ? C13A C17A 1.408(7) . ? C13A C14A 1.416(7) . ? C14A C15A 1.405(9) . ? C15A C16A 1.405(9) . ? C16A C17A 1.413(7) . ? 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 Cl2 Al1 Cl1 111.42(17) . . ? Cl2 Al1 Cl4 112.14(16) . . ? Cl1 Al1 Cl4 108.46(14) . . ? Cl2 Al1 Cl3 106.34(17) . . ? Cl1 Al1 Cl3 109.13(16) . . ? Cl4 Al1 Cl3 109.29(17) . . ? Cl2A Al1A Cl3A 124.1(10) . . ? Cl2A Al1A Cl4A 105.9(9) . . ? Cl3A Al1A Cl4A 109.9(8) . . ? Cl2A Al1A Cl1A 107.1(10) . . ? Cl3A Al1A Cl1A 102.5(8) . . ? Cl4A Al1A Cl1A 106.0(8) . . ? Cl1B Al1B Cl3B 99.3(8) . . ? Cl1B Al1B Cl4B 112.5(9) . . ? Cl3B Al1B Cl4B 118.3(10) . . ? Cl1B Al1B Cl2B 112.1(10) . . ? Cl3B Al1B Cl2B 110.4(9) . . ? Cl4B Al1B Cl2B 104.6(10) . . ? Cl3C Al1C Cl2C 94.8(9) . . ? Cl3C Al1C Cl4C 123.8(10) . . ? Cl2C Al1C Cl4C 100.6(9) . . ? Cl3C Al1C Cl1C 117.9(10) . . ? Cl2C Al1C Cl1C 111.5(8) . . ? Cl4C Al1C Cl1C 105.7(8) . . ? C12 Fe1 C11 93.81(17) . . ? C12 Fe1 C14 111.00(15) . . ? C11 Fe1 C14 153.14(17) . . ? C12 Fe1 C15 88.39(15) . . ? C11 Fe1 C15 136.6(2) . . ? C14 Fe1 C15 39.3(2) . . ? C12 Fe1 C13 150.55(14) . . ? C11 Fe1 C13 114.68(17) . . ? C14 Fe1 C13 39.64(15) . . ? C15 Fe1 C13 66.12(17) . . ? C12 Fe1 C17 141.93(15) . . ? C11 Fe1 C17 88.81(17) . . ? C14 Fe1 C17 65.43(15) . . ? C15 Fe1 C17 64.94(15) . . ? C13 Fe1 C17 39.18(14) . . ? C12 Fe1 C16 103.06(16) . . ? C11 Fe1 C16 98.93(19) . . ? C14 Fe1 C16 66.4(2) . . ? C15 Fe1 C16 39.1(2) . . ? C13 Fe1 C16 66.79(17) . . ? C17 Fe1 C16 39.30(15) . . ? C12 Fe1 P1 95.29(10) . . ? C11 Fe1 P1 90.25(12) . . ? C14 Fe1 P1 97.28(15) . . ? C15 Fe1 P1 132.73(18) . . ? C13 Fe1 P1 92.03(11) . . ? C17 Fe1 P1 122.70(11) . . ? C16 Fe1 P1 158.81(14) . . ? C1 P1 N1 114.30(13) . . ? C1 P1 Fe1 125.89(11) . . ? N1 P1 Fe1 119.80(8) . . ? C3 Si1 C4 108.7(2) . . ? C3 Si1 C1 109.01(19) . . ? C4 Si1 C1 105.34(19) . . ? C3 Si1 C2 113.3(3) . . ? C4 Si1 C2 107.5(3) . . ? C1 Si1 C2 112.69(17) . . ? C8 N1 C5 114.9(2) . . ? C8 N1 P1 120.54(17) . . ? C5 N1 P1 124.51(18) . . ? P1 C1 Si1 139.24(18) . . ? N1 C5 C7 113.9(3) . . ? N1 C5 C6 112.9(3) . . ? C7 C5 C6 114.4(3) . . ? N1 C8 C10 111.5(3) . . ? N1 C8 C9 110.3(3) . . ? C10 C8 C9 113.1(3) . . ? O1 C11 Fe1 176.5(4) . . ? O2 C12 Fe1 173.8(3) . . ? C17 C13 C14 106.3(4) . . ? C17 C13 Fe1 70.5(2) . . ? C14 C13 Fe1 69.5(2) . . ? C15 C14 C13 108.3(4) . . ? C15 C14 Fe1 71.0(2) . . ? C13 C14 Fe1 70.8(2) . . ? C14 C15 C16 109.2(3) . . ? C14 C15 Fe1 69.7(2) . . ? C16 C15 Fe1 70.8(2) . . ? C15 C16 C17 106.0(4) . . ? C15 C16 Fe1 70.1(2) . . ? C17 C16 Fe1 70.1(2) . . ? C13 C17 C16 110.2(3) . . ? C13 C17 Fe1 70.31(18) . . ? C16 C17 Fe1 70.6(2) . . ? C12A Fe1A C11A 94.0(4) . . ? C12A Fe1A C14A 110.4(4) . . ? C11A Fe1A C14A 153.5(4) . . ? C12A Fe1A C15A 88.8(3) . . ? C11A Fe1A C15A 136.1(4) . . ? C14A Fe1A C15A 39.3(3) . . ? C12A Fe1A C17A 143.1(4) . . ? C11A Fe1A C17A 89.0(3) . . ? C14A Fe1A C17A 65.4(3) . . ? C15A Fe1A C17A 64.8(3) . . ? C12A Fe1A C13A 150.0(4) . . ? C11A Fe1A C13A 115.3(4) . . ? C14A Fe1A C13A 39.6(2) . . ? C15A Fe1A C13A 66.0(3) . . ? C17A Fe1A C13A 39.2(2) . . ? C12A Fe1A C16A 104.2(4) . . ? C11A Fe1A C16A 98.5(4) . . ? C14A Fe1A C16A 66.4(3) . . ? C15A Fe1A C16A 39.1(2) . . ? C17A Fe1A C16A 39.3(2) . . ? C13A Fe1A C16A 66.7(3) . . ? C12A Fe1A P1A 96.1(3) . . ? C11A Fe1A P1A 89.7(4) . . ? C14A Fe1A P1A 97.5(3) . . ? C15A Fe1A P1A 133.7(3) . . ? C17A Fe1A P1A 120.7(3) . . ? C13A Fe1A P1A 90.8(3) . . ? C16A Fe1A P1A 157.5(3) . . ? C1A P1A N1A 115.6(4) . . ? C1A P1A Fe1A 123.3(4) . . ? N1A P1A Fe1A 121.0(3) . . ? C1A Si1A C4A 108.1(5) . . ? C1A Si1A C3A 108.9(5) . . ? C4A Si1A C3A 108.7(6) . . ? C1A Si1A C2A 111.1(5) . . ? C4A Si1A C2A 107.4(6) . . ? C3A Si1A C2A 112.4(6) . . ? C8A N1A C5A 116.5(6) . . ? C8A N1A P1A 120.4(5) . . ? C5A N1A P1A 123.0(6) . . ? P1A C1A Si1A 152.1(6) . . ? N1A C5A C7A 114.7(8) . . ? N1A C5A C6A 113.3(8) . . ? C7A C5A C6A 114.7(9) . . ? N1A C8A C10A 113.2(8) . . ? N1A C8A C9A 112.1(8) . . ? C10A C8A C9A 113.9(8) . . ? O1A C11A Fe1A 171.2(17) . . ? O2A C12A Fe1A 164.4(14) . . ? C17A C13A C14A 106.4(6) . . ? C17A C13A Fe1A 70.4(3) . . ? C14A C13A Fe1A 69.5(3) . . ? C15A C14A C13A 108.1(6) . . ? C15A C14A Fe1A 70.8(3) . . ? C13A C14A Fe1A 70.9(3) . . ? C14A C15A C16A 109.5(6) . . ? C14A C15A Fe1A 69.9(3) . . ? C16A C15A Fe1A 70.9(3) . . ? C15A C16A C17A 105.9(6) . . ? C15A C16A Fe1A 70.0(3) . . ? C17A C16A Fe1A 70.1(3) . . ? C13A C17A C16A 110.2(6) . . ? C13A C17A Fe1A 70.4(3) . . ? C16A C17A Fe1A 70.6(3) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 29.56 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.727 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.064