# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. # 1. SUBMISSION DETAILS _journal_coden_Cambridge 0182 _publ_contact_author_name 'Alan H. Cowley' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of Texas-Austin 1 University Station, A5300 Austin, TX 78701 USA ; _publ_contact_author_phone 512-471-7710 _publ_contact_author_fax 512-471-6822 _publ_contact_author_email cowley@mail.utexas.edu _publ_contact_letter ; Please consider this CIF submission for publication in Chemical Communications ; # 2. TITLE AND AUTHOR LIST _publ_section_title ; N,C-chelated beta-diketiminato phosphenium cations ; loop_ _publ_author_name _publ_author_address L.Zheng ; Department of Chemistry and Biochemistry University of Texas-Austin 1 University Station, A5300 Austin, TX 78701 USA ; 'Gregor Reeske' ; Department of Chemistry and Biochemistry University of Texas-Austin 1 University Station, A5300 Austin, TX 78701 USA ; 'Jennifer A. Moore' ; Department of Chemistry and Biochemistry University of Texas-Austin 1 University Station, A5300 Austin, TX 78701 USA ; 'Alan H. Cowley' ; Department of Chemistry and Biochemistry University of Texas-Austin 1 University Station, A5300 Austin, TX 78701 USA ; _publ_section_references ; Allen, F.H. (2002). Acta Cryst. B58, 380-388. Cremer D. & Pople J.A. (1975). J. Am. Chem. Soc. 97, 1358-1367. Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; data_squeeze _database_code_depnum_ccdc_archive 'CCDC 617244' _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H41 Cl N2 P, C F3 O3 S' _chemical_formula_sum 'C30 H41 Cl F3 N2 O3 P S' _chemical_formula_weight 633.13 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 _symmetry_space_group_name_Hall -p1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.356(2) _cell_length_b 12.553(3) _cell_length_c 14.756(3) _cell_angle_alpha 100.40(3) _cell_angle_beta 90.53(3) _cell_angle_gamma 110.49(3) _cell_volume 1761.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 0.259 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.962 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11412 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.1306 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7893 _reflns_number_gt 3999 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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. One molecule of what appeared to be dichloromethane was found to be badly disordered. Attempts to model the disorder were unsatisfactory. The contributions to the scattering factors due to these solvent molecules were removed by use of the utility SQUEEZE (Sluis and Spek, 1990) in PLATON98 (Spek, 1998). PLATON98 was used as incorporated in WinGX (Farrugia, 1999). ; _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^)+(0.1091P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7893 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1463 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.2103 _refine_ls_wR_factor_gt 0.1841 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0792(4) 0.5686(3) 0.3096(2) 0.0386(8) Uani 1 1 d . . . H1A H 0.0172 0.4873 0.3000 0.058 Uiso 1 1 calc R . . H1B H 0.0375 0.6121 0.2777 0.058 Uiso 1 1 calc R . . H1C H 0.0941 0.6020 0.3759 0.058 Uiso 1 1 calc R . . C2 C 0.2116(3) 0.5750(2) 0.2727(2) 0.0291(8) Uani 1 1 d . . . C3 C 0.2570(3) 0.6326(2) 0.2008(2) 0.0293(7) Uani 1 1 d . . . H3 H 0.2046 0.6740 0.1807 0.035 Uiso 1 1 calc R . . C4 C 0.3755(3) 0.6333(2) 0.1562(2) 0.0258(7) Uani 1 1 d . . . C5 C 0.4367(4) 0.5440(3) 0.1660(2) 0.0358(8) Uani 1 1 d . . . H5A H 0.5296 0.5663 0.1422 0.043 Uiso 1 1 calc R . . H5B H 0.3782 0.4686 0.1278 0.043 Uiso 1 1 calc R . . C6 C 0.2387(3) 0.4627(3) 0.3889(2) 0.0288(7) Uani 1 1 d . . . C7 C 0.1707(3) 0.3423(3) 0.3663(2) 0.0299(8) Uani 1 1 d . . . C8 C 0.1308(4) 0.2835(3) 0.4383(3) 0.0372(8) Uani 1 1 d . . . H8 H 0.0853 0.2016 0.4251 0.045 Uiso 1 1 calc R . . C9 C 0.1564(4) 0.3423(3) 0.5291(3) 0.0428(9) Uani 1 1 d . . . H9 H 0.1296 0.3005 0.5776 0.051 Uiso 1 1 calc R . . C10 C 0.2207(4) 0.4614(3) 0.5499(2) 0.0400(9) Uani 1 1 d . . . H10 H 0.2363 0.5006 0.6127 0.048 Uiso 1 1 calc R . . C11 C 0.2630(3) 0.5251(3) 0.4807(2) 0.0316(8) Uani 1 1 d . . . C12 C 0.1426(4) 0.2765(3) 0.2662(2) 0.0351(8) Uani 1 1 d . . . H12 H 0.1599 0.3341 0.2247 0.042 Uiso 1 1 calc R . . C13 C -0.0073(4) 0.1927(3) 0.2459(3) 0.0499(10) Uani 1 1 d . . . H13A H -0.0250 0.1338 0.2844 0.075 Uiso 1 1 calc R . . H13B H -0.0231 0.1548 0.1806 0.075 Uiso 1 1 calc R . . H13C H -0.0698 0.2357 0.2599 0.075 Uiso 1 1 calc R . . C14 C 0.2381(4) 0.2090(4) 0.2440(3) 0.0582(12) Uani 1 1 d . . . H14A H 0.3345 0.2624 0.2548 0.087 Uiso 1 1 calc R . . H14B H 0.2197 0.1693 0.1791 0.087 Uiso 1 1 calc R . . H14C H 0.2221 0.1516 0.2837 0.087 Uiso 1 1 calc R . . C15 C 0.3336(4) 0.6554(3) 0.5066(2) 0.0394(9) Uani 1 1 d . . . H15 H 0.3524 0.6859 0.4481 0.047 Uiso 1 1 calc R . . C16 C 0.2413(5) 0.7127(4) 0.5604(3) 0.0604(12) Uani 1 1 d . . . H16A H 0.1532 0.6911 0.5240 0.091 Uiso 1 1 calc R . . H16B H 0.2876 0.7972 0.5723 0.091 Uiso 1 1 calc R . . H16C H 0.2240 0.6864 0.6193 0.091 Uiso 1 1 calc R . . C17 C 0.4728(4) 0.6875(3) 0.5615(3) 0.0528(11) Uani 1 1 d . . . H17A H 0.4567 0.6683 0.6229 0.079 Uiso 1 1 calc R . . H17B H 0.5244 0.7708 0.5680 0.079 Uiso 1 1 calc R . . H17C H 0.5262 0.6439 0.5287 0.079 Uiso 1 1 calc R . . C18 C 0.3864(3) 0.7961(2) 0.0817(2) 0.0280(7) Uani 1 1 d . . . C19 C 0.3176(3) 0.7760(3) -0.0048(2) 0.0327(8) Uani 1 1 d . . . C20 C 0.2824(4) 0.8659(3) -0.0273(3) 0.0425(9) Uani 1 1 d . . . H20 H 0.2372 0.8560 -0.0862 0.051 Uiso 1 1 calc R . . C21 C 0.3126(4) 0.9697(3) 0.0353(3) 0.0414(9) Uani 1 1 d . . . H21 H 0.2873 1.0300 0.0191 0.050 Uiso 1 1 calc R . . C22 C 0.3790(4) 0.9858(3) 0.1206(3) 0.0410(9) Uani 1 1 d . . . H22 H 0.3996 1.0578 0.1624 0.049 Uiso 1 1 calc R . . C23 C 0.4164(3) 0.8998(3) 0.1468(2) 0.0322(8) Uani 1 1 d . . . C24 C 0.2811(4) 0.6598(3) -0.0717(2) 0.0376(9) Uani 1 1 d . . . H24 H 0.3208 0.6105 -0.0431 0.045 Uiso 1 1 calc R . . C25 C 0.1268(5) 0.5985(4) -0.0855(4) 0.0838(17) Uani 1 1 d . . . H25A H 0.0903 0.5831 -0.0262 0.126 Uiso 1 1 calc R . . H25B H 0.1051 0.5249 -0.1295 0.126 Uiso 1 1 calc R . . H25C H 0.0846 0.6474 -0.1097 0.126 Uiso 1 1 calc R . . C26 C 0.3432(7) 0.6738(4) -0.1624(3) 0.0852(18) Uani 1 1 d . . . H26A H 0.3209 0.5974 -0.2024 0.128 Uiso 1 1 calc R . . H26B H 0.4438 0.7119 -0.1516 0.128 Uiso 1 1 calc R . . H26C H 0.3053 0.7213 -0.1923 0.128 Uiso 1 1 calc R . . C27 C 0.4902(4) 0.9193(3) 0.2406(2) 0.0404(9) Uani 1 1 d . . . H27 H 0.4994 0.8443 0.2473 0.048 Uiso 1 1 calc R . . C28 C 0.4084(5) 0.9521(4) 0.3194(3) 0.0700(14) Uani 1 1 d . . . H28A H 0.4014 1.0273 0.3166 0.105 Uiso 1 1 calc R . . H28B H 0.4559 0.9571 0.3787 0.105 Uiso 1 1 calc R . . H28C H 0.3155 0.8929 0.3135 0.105 Uiso 1 1 calc R . . C29 C 0.6362(4) 1.0091(4) 0.2467(3) 0.0603(12) Uani 1 1 d . . . H29A H 0.6878 0.9832 0.1976 0.090 Uiso 1 1 calc R . . H29B H 0.6834 1.0183 0.3070 0.090 Uiso 1 1 calc R . . H29C H 0.6310 1.0836 0.2393 0.090 Uiso 1 1 calc R . . C30 C 0.9173(6) 0.8157(5) 0.0999(4) 0.0840(16) Uani 1 1 d . . . N1 N 0.2907(3) 0.5255(2) 0.31433(18) 0.0281(6) Uani 1 1 d . . . N2 N 0.4335(3) 0.7067(2) 0.10270(19) 0.0293(6) Uani 1 1 d . . . O1 O 0.7456(4) 0.6201(3) 0.1013(4) 0.1226(18) Uani 1 1 d . . . O2 O 0.8420(4) 0.6603(5) -0.0415(3) 0.148(2) Uani 1 1 d . . . O3 O 0.6760(3) 0.7409(3) 0.0193(2) 0.0861(11) Uani 1 1 d . . . F1 F 0.8753(6) 0.8649(4) 0.1716(4) 0.201(3) Uani 1 1 d . . . F2 F 0.9649(4) 0.8941(3) 0.0456(5) 0.183(3) Uani 1 1 d . . . F3 F 1.0245(3) 0.7895(3) 0.1241(2) 0.1054(11) Uani 1 1 d . . . P1 P 0.45154(9) 0.52717(7) 0.28526(6) 0.0349(3) Uani 1 1 d . . . S1 S 0.78101(11) 0.69554(9) 0.03702(8) 0.0575(3) Uani 1 1 d . . . Cl1 Cl 0.57929(9) 0.69886(8) 0.33898(6) 0.0464(3) Uani 1 1 d . . . H2N H 0.506(5) 0.707(3) 0.076(3) 0.056(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.034(2) 0.044(2) 0.041(2) 0.0149(16) 0.0026(16) 0.0145(15) C2 0.0305(19) 0.0236(15) 0.0287(18) -0.0006(13) -0.0015(15) 0.0070(13) C3 0.0288(18) 0.0256(16) 0.0338(18) 0.0046(14) 0.0009(15) 0.0109(13) C4 0.0274(18) 0.0238(15) 0.0235(16) 0.0022(13) -0.0012(14) 0.0069(13) C5 0.039(2) 0.0318(17) 0.039(2) 0.0090(15) 0.0053(16) 0.0145(15) C6 0.0269(18) 0.0304(17) 0.0295(18) 0.0064(14) 0.0022(14) 0.0105(13) C7 0.0255(18) 0.0303(17) 0.0367(19) 0.0084(15) 0.0032(15) 0.0124(13) C8 0.032(2) 0.0333(18) 0.048(2) 0.0119(16) 0.0035(17) 0.0115(14) C9 0.039(2) 0.052(2) 0.041(2) 0.0228(18) 0.0079(17) 0.0149(17) C10 0.040(2) 0.049(2) 0.032(2) 0.0075(16) 0.0020(16) 0.0181(17) C11 0.0313(19) 0.0333(17) 0.0300(18) 0.0039(15) 0.0026(15) 0.0126(14) C12 0.035(2) 0.0312(17) 0.037(2) 0.0032(15) 0.0008(16) 0.0106(14) C13 0.041(2) 0.046(2) 0.053(2) 0.0020(18) -0.0098(19) 0.0080(17) C14 0.052(3) 0.066(3) 0.056(3) -0.013(2) -0.006(2) 0.032(2) C15 0.049(2) 0.0339(18) 0.0310(19) -0.0028(15) -0.0035(17) 0.0139(16) C16 0.075(3) 0.058(2) 0.052(3) -0.010(2) -0.001(2) 0.038(2) C17 0.056(3) 0.047(2) 0.046(2) 0.0065(18) -0.014(2) 0.0087(18) C18 0.0270(18) 0.0263(16) 0.0314(18) 0.0053(13) 0.0034(14) 0.0107(13) C19 0.033(2) 0.0334(17) 0.0325(19) 0.0043(14) 0.0004(15) 0.0147(14) C20 0.046(2) 0.049(2) 0.038(2) 0.0112(17) -0.0019(17) 0.0222(18) C21 0.041(2) 0.0351(19) 0.056(2) 0.0143(17) 0.0065(19) 0.0207(16) C22 0.043(2) 0.0299(18) 0.048(2) 0.0005(16) 0.0061(18) 0.0130(16) C23 0.0314(19) 0.0297(17) 0.0343(19) 0.0064(14) 0.0057(15) 0.0094(14) C24 0.043(2) 0.0376(19) 0.0308(19) -0.0011(15) -0.0079(16) 0.0170(16) C25 0.059(3) 0.055(3) 0.113(4) -0.026(3) -0.006(3) 0.012(2) C26 0.127(5) 0.060(3) 0.060(3) -0.004(2) 0.036(3) 0.030(3) C27 0.049(2) 0.0287(17) 0.037(2) -0.0030(15) -0.0065(17) 0.0115(16) C28 0.076(4) 0.088(3) 0.042(2) -0.006(2) 0.008(2) 0.033(3) C29 0.049(3) 0.066(3) 0.058(3) 0.008(2) -0.012(2) 0.013(2) C30 0.066(4) 0.078(4) 0.101(4) -0.001(3) 0.013(3) 0.026(3) N1 0.0277(15) 0.0260(13) 0.0294(15) 0.0053(11) -0.0014(12) 0.0083(11) N2 0.0298(17) 0.0311(15) 0.0276(15) 0.0046(12) 0.0014(13) 0.0124(12) O1 0.065(3) 0.077(2) 0.257(6) 0.090(3) 0.069(3) 0.0351(19) O2 0.067(3) 0.256(6) 0.090(3) -0.079(3) -0.007(2) 0.073(3) O3 0.047(2) 0.148(3) 0.090(3) 0.052(2) 0.0282(18) 0.053(2) F1 0.169(5) 0.181(4) 0.191(5) -0.134(4) -0.035(4) 0.071(4) F2 0.097(3) 0.098(3) 0.369(8) 0.119(4) 0.048(4) 0.016(2) F3 0.056(2) 0.145(3) 0.097(2) 0.005(2) -0.0193(17) 0.0234(19) P1 0.0311(5) 0.0384(5) 0.0398(5) 0.0125(4) 0.0047(4) 0.0157(4) S1 0.0368(6) 0.0631(7) 0.0623(7) -0.0114(5) 0.0098(5) 0.0169(5) Cl1 0.0339(5) 0.0474(5) 0.0485(6) 0.0114(4) -0.0070(4) 0.0022(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.461(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.385(4) . ? C2 C3 1.385(5) . ? C3 C4 1.396(4) . ? C3 H3 0.9500 . ? C4 N2 1.310(4) . ? C4 C5 1.495(5) . ? C5 P1 1.821(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.400(4) . ? C6 C11 1.408(4) . ? C6 N1 1.466(4) . ? C7 C8 1.387(5) . ? C7 C12 1.528(5) . ? C8 C9 1.382(5) . ? C8 H8 0.9500 . ? C9 C10 1.381(5) . ? C9 H9 0.9500 . ? C10 C11 1.390(5) . ? C10 H10 0.9500 . ? C11 C15 1.512(5) . ? C12 C14 1.515(5) . ? C12 C13 1.530(5) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.533(5) . ? C15 C16 1.533(5) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.393(5) . ? C18 C23 1.405(4) . ? C18 N2 1.449(4) . ? C19 C20 1.391(5) . ? C19 C24 1.528(4) . ? C20 C21 1.387(5) . ? C20 H20 0.9500 . ? C21 C22 1.376(5) . ? C21 H21 0.9500 . ? C22 C23 1.381(5) . ? C22 H22 0.9500 . ? C23 C27 1.512(5) . ? C24 C26 1.502(6) . ? C24 C25 1.505(6) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.526(6) . ? C27 C29 1.527(5) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 F1 1.285(7) . ? C30 F3 1.327(7) . ? C30 F2 1.344(8) . ? C30 S1 1.763(6) . ? N1 P1 1.718(3) . ? N2 O3 2.738(4) . ? N2 H2N 0.85(4) . ? O1 S1 1.421(4) . ? O2 S1 1.401(4) . ? O3 S1 1.434(3) . ? P1 Cl1 2.0955(15) . ? 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 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 121.9(3) . . ? N1 C2 C1 117.7(3) . . ? C3 C2 C1 120.3(3) . . ? C2 C3 C4 123.7(3) . . ? C2 C3 H3 118.2 . . ? C4 C3 H3 118.2 . . ? N2 C4 C3 122.8(3) . . ? N2 C4 C5 117.9(3) . . ? C3 C4 C5 119.3(3) . . ? C4 C5 P1 112.7(2) . . ? C4 C5 H5A 109.1 . . ? P1 C5 H5A 109.1 . . ? C4 C5 H5B 109.1 . . ? P1 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? C7 C6 C11 122.6(3) . . ? C7 C6 N1 118.6(3) . . ? C11 C6 N1 118.8(3) . . ? C8 C7 C6 117.7(3) . . ? C8 C7 C12 120.5(3) . . ? C6 C7 C12 121.8(3) . . ? C9 C8 C7 120.9(3) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C10 C9 C8 120.6(3) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 121.2(3) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C6 117.1(3) . . ? C10 C11 C15 119.4(3) . . ? C6 C11 C15 123.5(3) . . ? C14 C12 C7 111.1(3) . . ? C14 C12 C13 108.9(3) . . ? C7 C12 C13 111.5(3) . . ? C14 C12 H12 108.4 . . ? C7 C12 H12 108.4 . . ? C13 C12 H12 108.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 110.6(3) . . ? C11 C15 C16 111.7(3) . . ? C17 C15 C16 110.9(3) . . ? C11 C15 H15 107.8 . . ? C17 C15 H15 107.8 . . ? C16 C15 H15 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 123.1(3) . . ? C19 C18 N2 117.6(3) . . ? C23 C18 N2 119.3(3) . . ? C20 C19 C18 117.2(3) . . ? C20 C19 C24 121.4(3) . . ? C18 C19 C24 121.4(3) . . ? C21 C20 C19 120.7(3) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C22 C21 C20 120.4(3) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 121.5(3) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C22 C23 C18 117.0(3) . . ? C22 C23 C27 120.8(3) . . ? C18 C23 C27 122.2(3) . . ? C26 C24 C25 111.2(4) . . ? C26 C24 C19 111.8(3) . . ? C25 C24 C19 110.5(3) . . ? C26 C24 H24 107.7 . . ? C25 C24 H24 107.7 . . ? C19 C24 H24 107.7 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C28 112.2(3) . . ? C23 C27 C29 110.8(3) . . ? C28 C27 C29 111.5(3) . . ? C23 C27 H27 107.4 . . ? C28 C27 H27 107.4 . . ? C29 C27 H27 107.4 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? F1 C30 F3 110.0(6) . . ? F1 C30 F2 107.5(6) . . ? F3 C30 F2 106.0(5) . . ? F1 C30 S1 111.3(5) . . ? F3 C30 S1 113.2(4) . . ? F2 C30 S1 108.5(5) . . ? C2 N1 C6 120.8(3) . . ? C2 N1 P1 125.7(2) . . ? C6 N1 P1 113.5(2) . . ? C4 N2 C18 126.0(3) . . ? C4 N2 O3 129.2(2) . . ? C18 N2 O3 104.6(2) . . ? C4 N2 H2N 122(3) . . ? C18 N2 H2N 112(3) . . ? O3 N2 H2N 8(3) . . ? S1 O3 N2 127.0(2) . . ? N1 P1 C5 97.90(15) . . ? N1 P1 Cl1 102.82(10) . . ? C5 P1 Cl1 96.74(12) . . ? O2 S1 O1 116.6(3) . . ? O2 S1 O3 114.8(3) . . ? O1 S1 O3 113.4(2) . . ? O2 S1 C30 103.3(3) . . ? O1 S1 C30 101.8(3) . . ? O3 S1 C30 104.6(3) . . ? 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 N1 C2 C3 C4 8.6(4) . . . . ? C1 C2 C3 C4 -173.8(3) . . . . ? C2 C3 C4 N2 -165.0(3) . . . . ? C2 C3 C4 C5 17.6(4) . . . . ? N2 C4 C5 P1 135.9(2) . . . . ? C3 C4 C5 P1 -46.6(4) . . . . ? C11 C6 C7 C8 -2.3(5) . . . . ? N1 C6 C7 C8 175.6(3) . . . . ? C11 C6 C7 C12 178.7(3) . . . . ? N1 C6 C7 C12 -3.4(5) . . . . ? C6 C7 C8 C9 0.6(5) . . . . ? C12 C7 C8 C9 179.7(3) . . . . ? C7 C8 C9 C10 0.9(6) . . . . ? C8 C9 C10 C11 -0.9(6) . . . . ? C9 C10 C11 C6 -0.6(5) . . . . ? C9 C10 C11 C15 -179.7(3) . . . . ? C7 C6 C11 C10 2.3(5) . . . . ? N1 C6 C11 C10 -175.6(3) . . . . ? C7 C6 C11 C15 -178.7(3) . . . . ? N1 C6 C11 C15 3.4(5) . . . . ? C8 C7 C12 C14 -72.9(4) . . . . ? C6 C7 C12 C14 106.1(4) . . . . ? C8 C7 C12 C13 48.8(4) . . . . ? C6 C7 C12 C13 -132.2(3) . . . . ? C10 C11 C15 C17 64.8(4) . . . . ? C6 C11 C15 C17 -114.2(4) . . . . ? C10 C11 C15 C16 -59.3(5) . . . . ? C6 C11 C15 C16 121.6(4) . . . . ? C23 C18 C19 C20 2.3(5) . . . . ? N2 C18 C19 C20 -175.0(3) . . . . ? C23 C18 C19 C24 -177.1(3) . . . . ? N2 C18 C19 C24 5.5(5) . . . . ? C18 C19 C20 C21 -1.4(5) . . . . ? C24 C19 C20 C21 178.1(3) . . . . ? C19 C20 C21 C22 0.5(6) . . . . ? C20 C21 C22 C23 -0.5(6) . . . . ? C21 C22 C23 C18 1.4(5) . . . . ? C21 C22 C23 C27 179.6(3) . . . . ? C19 C18 C23 C22 -2.4(5) . . . . ? N2 C18 C23 C22 175.0(3) . . . . ? C19 C18 C23 C27 179.5(3) . . . . ? N2 C18 C23 C27 -3.2(5) . . . . ? C20 C19 C24 C26 58.6(5) . . . . ? C18 C19 C24 C26 -122.0(4) . . . . ? C20 C19 C24 C25 -65.8(5) . . . . ? C18 C19 C24 C25 113.6(4) . . . . ? C22 C23 C27 C28 57.1(5) . . . . ? C18 C23 C27 C28 -124.8(4) . . . . ? C22 C23 C27 C29 -68.2(5) . . . . ? C18 C23 C27 C29 109.9(4) . . . . ? C3 C2 N1 C6 -178.6(3) . . . . ? C1 C2 N1 C6 3.7(4) . . . . ? C3 C2 N1 P1 0.1(4) . . . . ? C1 C2 N1 P1 -177.6(2) . . . . ? C7 C6 N1 C2 93.9(4) . . . . ? C11 C6 N1 C2 -88.2(4) . . . . ? C7 C6 N1 P1 -84.9(3) . . . . ? C11 C6 N1 P1 93.0(3) . . . . ? C3 C4 N2 C18 0.0(5) . . . . ? C5 C4 N2 C18 177.5(3) . . . . ? C3 C4 N2 O3 174.1(2) . . . . ? C5 C4 N2 O3 -8.5(4) . . . . ? C19 C18 N2 C4 -103.7(4) . . . . ? C23 C18 N2 C4 78.8(4) . . . . ? C19 C18 N2 O3 81.0(3) . . . . ? C23 C18 N2 O3 -96.4(3) . . . . ? C4 N2 O3 S1 -11.6(4) . . . . ? C18 N2 O3 S1 163.4(3) . . . . ? C2 N1 P1 C5 -24.9(3) . . . . ? C6 N1 P1 C5 153.8(2) . . . . ? C2 N1 P1 Cl1 73.9(2) . . . . ? C6 N1 P1 Cl1 -107.39(19) . . . . ? C4 C5 P1 N1 44.7(3) . . . . ? C4 C5 P1 Cl1 -59.3(2) . . . . ? N2 O3 S1 O2 141.4(3) . . . . ? N2 O3 S1 O1 3.9(4) . . . . ? N2 O3 S1 C30 -106.1(3) . . . . ? F1 C30 S1 O2 174.8(6) . . . . ? F3 C30 S1 O2 -60.6(5) . . . . ? F2 C30 S1 O2 56.8(5) . . . . ? F1 C30 S1 O1 -63.9(6) . . . . ? F3 C30 S1 O1 60.7(5) . . . . ? F2 C30 S1 O1 178.1(4) . . . . ? F1 C30 S1 O3 54.4(6) . . . . ? F3 C30 S1 O3 178.9(4) . . . . ? F2 C30 S1 O3 -63.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.632 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.078 # Attachment 'CCDC619044_revised.cif' data_shelx _database_code_depnum_ccdc_archive 'CCDC 619044' _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H47 N2 P, Al Cl4, C H2 Cl2 ' _chemical_formula_sum 'C37 H49 Al Cl6 N2 P' _chemical_formula_weight 792.43 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p21/c _symmetry_space_group_name_Hall -p2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.640(5) _cell_length_b 13.086(5) _cell_length_c 23.778(5) _cell_angle_alpha 90.000 _cell_angle_beta 97.133(5) _cell_angle_gamma 90.000 _cell_volume 4211(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 0.494 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8659 _exptl_absorpt_correction_T_max 0.9522 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30020 _diffrn_reflns_av_R_equivalents 0.1703 _diffrn_reflns_av_sigmaI/netI 0.2240 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9608 _reflns_number_gt 3808 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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^)+(0.0931P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9608 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2305 _refine_ls_R_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.2135 _refine_ls_wR_factor_gt 0.1636 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5464(3) -0.0682(4) 0.38859(19) 0.0362(12) Uani 1 1 d . . . H1A H 0.5346 -0.1327 0.4076 0.054 Uiso 1 1 calc R . . H1B H 0.4969 -0.0599 0.3553 0.054 Uiso 1 1 calc R . . H1C H 0.5414 -0.0112 0.4148 0.054 Uiso 1 1 calc R . . C2 C 0.6485(3) -0.0696(4) 0.37008(19) 0.0302(11) Uani 1 1 d . . . C3 C 0.6655(3) -0.1264(3) 0.32311(18) 0.0265(11) Uani 1 1 d . . . C4 C 0.7482(3) -0.1087(3) 0.29532(19) 0.0294(11) Uani 1 1 d . . . C5 C 0.8163(3) -0.0213(4) 0.31178(19) 0.0346(12) Uani 1 1 d . . . H5A H 0.7874 0.0415 0.2934 0.042 Uiso 1 1 calc R . . H5B H 0.8798 -0.0342 0.2969 0.042 Uiso 1 1 calc R . . C6 C 0.5914(3) -0.2055(4) 0.29779(19) 0.0356(12) Uani 1 1 d . . . H6A H 0.6198 -0.2740 0.3039 0.053 Uiso 1 1 calc R . . H6B H 0.5756 -0.1930 0.2570 0.053 Uiso 1 1 calc R . . H6C H 0.5311 -0.2004 0.3161 0.053 Uiso 1 1 calc R . . C7 C 0.6987(3) 0.0423(4) 0.45205(19) 0.0298(11) Uani 1 1 d . . . C8 C 0.6990(3) -0.0068(4) 0.50481(19) 0.0316(11) Uani 1 1 d . . . C9 C 0.6887(3) 0.0548(4) 0.5516(2) 0.0383(13) Uani 1 1 d . . . H9 H 0.6920 0.0246 0.5881 0.046 Uiso 1 1 calc R . . C10 C 0.6738(4) 0.1581(4) 0.5460(2) 0.0408(13) Uani 1 1 d . . . H10 H 0.6656 0.1983 0.5784 0.049 Uiso 1 1 calc R . . C11 C 0.6706(3) 0.2038(4) 0.4940(2) 0.0384(13) Uani 1 1 d . . . H11 H 0.6588 0.2753 0.4909 0.046 Uiso 1 1 calc R . . C12 C 0.6842(3) 0.1488(4) 0.44575(19) 0.0327(12) Uani 1 1 d . . . C13 C 0.7094(4) -0.1217(4) 0.5126(2) 0.0385(13) Uani 1 1 d . . . H13 H 0.7124 -0.1531 0.4745 0.046 Uiso 1 1 calc R . . C14 C 0.8037(4) -0.1505(4) 0.5507(2) 0.0482(14) Uani 1 1 d . . . H14A H 0.8612 -0.1272 0.5333 0.072 Uiso 1 1 calc R . . H14B H 0.8067 -0.2248 0.5554 0.072 Uiso 1 1 calc R . . H14C H 0.8038 -0.1179 0.5878 0.072 Uiso 1 1 calc R . . C15 C 0.6186(4) -0.1646(4) 0.5363(2) 0.0448(14) Uani 1 1 d . . . H15A H 0.6154 -0.1365 0.5742 0.067 Uiso 1 1 calc R . . H15B H 0.6235 -0.2392 0.5386 0.067 Uiso 1 1 calc R . . H15C H 0.5589 -0.1454 0.5113 0.067 Uiso 1 1 calc R . . C16 C 0.6828(4) 0.2031(4) 0.3892(2) 0.0400(13) Uani 1 1 d . . . H16 H 0.6940 0.1504 0.3602 0.048 Uiso 1 1 calc R . . C17 C 0.7660(4) 0.2815(4) 0.3905(2) 0.0524(15) Uani 1 1 d . . . H17A H 0.7566 0.3348 0.4182 0.079 Uiso 1 1 calc R . . H17B H 0.7652 0.3123 0.3529 0.079 Uiso 1 1 calc R . . H17C H 0.8296 0.2475 0.4012 0.079 Uiso 1 1 calc R . . C18 C 0.5817(4) 0.2516(4) 0.3708(2) 0.0537(15) Uani 1 1 d . . . H18A H 0.5305 0.1987 0.3685 0.081 Uiso 1 1 calc R . . H18B H 0.5818 0.2839 0.3337 0.081 Uiso 1 1 calc R . . H18C H 0.5681 0.3033 0.3987 0.081 Uiso 1 1 calc R . . C19 C 0.8389(3) -0.1396(4) 0.21302(18) 0.0322(12) Uani 1 1 d . . . C20 C 0.9288(4) -0.1912(4) 0.2170(2) 0.0399(13) Uani 1 1 d . . . C21 C 0.9936(4) -0.1616(5) 0.1785(2) 0.0528(15) Uani 1 1 d . . . H21 H 1.0561 -0.1943 0.1801 0.063 Uiso 1 1 calc R . . C22 C 0.9694(4) -0.0867(5) 0.1388(2) 0.0518(15) Uani 1 1 d . . . H22 H 1.0149 -0.0685 0.1133 0.062 Uiso 1 1 calc R . . C23 C 0.8794(4) -0.0378(4) 0.1356(2) 0.0443(14) Uani 1 1 d . . . H23 H 0.8634 0.0139 0.1079 0.053 Uiso 1 1 calc R . . C24 C 0.8116(4) -0.0634(4) 0.1726(2) 0.0354(12) Uani 1 1 d . . . C25 C 0.9570(4) -0.2748(4) 0.2599(2) 0.0506(15) Uani 1 1 d . . . H25 H 0.8999 -0.2863 0.2817 0.061 Uiso 1 1 calc R . . C26 C 0.9776(5) -0.3744(5) 0.2303(3) 0.072(2) Uani 1 1 d . . . H26A H 0.9176 -0.3970 0.2066 0.108 Uiso 1 1 calc R . . H26B H 0.9983 -0.4268 0.2588 0.108 Uiso 1 1 calc R . . H26C H 1.0304 -0.3635 0.2064 0.108 Uiso 1 1 calc R . . C27 C 1.0451(4) -0.2417(5) 0.3013(3) 0.0711(19) Uani 1 1 d . . . H27A H 1.1016 -0.2284 0.2806 0.107 Uiso 1 1 calc R . . H27B H 1.0621 -0.2961 0.3291 0.107 Uiso 1 1 calc R . . H27C H 1.0284 -0.1793 0.3208 0.107 Uiso 1 1 calc R . . C28 C 0.7084(4) -0.0148(4) 0.1669(2) 0.0372(12) Uani 1 1 d . . . H28 H 0.6861 -0.0139 0.2054 0.045 Uiso 1 1 calc R . . C29 C 0.6364(4) -0.0811(4) 0.1288(2) 0.0461(14) Uani 1 1 d . . . H29A H 0.5696 -0.0532 0.1276 0.069 Uiso 1 1 calc R . . H29B H 0.6378 -0.1509 0.1439 0.069 Uiso 1 1 calc R . . H29C H 0.6557 -0.0820 0.0905 0.069 Uiso 1 1 calc R . . C30 C 0.7070(4) 0.0945(4) 0.1455(3) 0.0579(16) Uani 1 1 d . . . H30A H 0.7254 0.0956 0.1069 0.087 Uiso 1 1 calc R . . H30B H 0.7541 0.1356 0.1704 0.087 Uiso 1 1 calc R . . H30C H 0.6404 0.1230 0.1452 0.087 Uiso 1 1 calc R . . C31 C 0.9051(4) -0.1138(4) 0.4151(2) 0.0380(13) Uani 1 1 d . . . C32 C 1.0002(4) -0.0954(5) 0.4432(2) 0.0480(14) Uani 1 1 d . . . H32 H 1.0244 -0.0273 0.4466 0.058 Uiso 1 1 calc R . . C33 C 1.0591(4) -0.1747(6) 0.4660(2) 0.0645(18) Uani 1 1 d . . . H33 H 1.1240 -0.1613 0.4841 0.077 Uiso 1 1 calc R . . C34 C 1.0228(5) -0.2743(5) 0.4624(2) 0.0585(16) Uani 1 1 d . . . H34 H 1.0625 -0.3286 0.4790 0.070 Uiso 1 1 calc R . . C35 C 0.9306(4) -0.2946(5) 0.4350(2) 0.0512(15) Uani 1 1 d . . . H35 H 0.9071 -0.3629 0.4315 0.061 Uiso 1 1 calc R . . C36 C 0.8714(4) -0.2137(4) 0.4122(2) 0.0428(13) Uani 1 1 d . . . H36 H 0.8065 -0.2276 0.3944 0.051 Uiso 1 1 calc R . . C37 C 0.6185(6) 0.5340(7) 0.4387(3) 0.109(3) Uani 1 1 d . . . H37A H 0.5855 0.4685 0.4452 0.130 Uiso 1 1 calc R . . H37B H 0.6331 0.5341 0.3989 0.130 Uiso 1 1 calc R . . N1 N 0.7192(3) -0.0167(3) 0.40328(14) 0.0283(9) Uani 1 1 d . . . N2 N 0.7682(3) -0.1672(3) 0.25152(15) 0.0317(10) Uani 1 1 d . . . Al1 Al 0.67030(11) -0.49149(11) 0.25319(6) 0.0362(4) Uani 1 1 d . . . P1 P 0.84124(9) 0.00113(10) 0.38794(5) 0.0345(3) Uani 1 1 d . . . Cl1 Cl 0.69455(11) -0.64022(10) 0.22168(6) 0.0551(4) Uani 1 1 d . . . Cl2 Cl 0.52375(11) -0.47981(12) 0.27370(6) 0.0602(4) Uani 1 1 d . . . Cl3 Cl 0.77247(11) -0.45421(11) 0.32548(6) 0.0561(4) Uani 1 1 d . . . Cl4 Cl 0.68821(11) -0.38110(10) 0.18880(5) 0.0490(4) Uani 1 1 d . . . Cl5 Cl 0.72811(16) 0.5386(2) 0.48229(8) 0.1141(8) Uani 1 1 d . . . Cl6 Cl 0.5371(2) 0.6319(2) 0.44671(12) 0.1608(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.028(3) 0.048(3) 0.034(3) -0.007(2) 0.010(2) -0.003(2) C2 0.027(3) 0.033(3) 0.031(3) 0.008(2) 0.006(2) 0.005(2) C3 0.019(3) 0.028(3) 0.032(3) 0.001(2) 0.002(2) -0.002(2) C4 0.026(3) 0.028(3) 0.032(3) 0.000(2) -0.003(2) 0.003(2) C5 0.026(3) 0.043(3) 0.036(3) -0.004(2) 0.009(2) -0.004(2) C6 0.028(3) 0.040(3) 0.039(3) -0.006(2) 0.007(2) 0.001(2) C7 0.020(3) 0.040(3) 0.029(3) -0.004(2) 0.004(2) -0.005(2) C8 0.030(3) 0.034(3) 0.030(3) 0.001(2) 0.003(2) -0.005(2) C9 0.034(3) 0.050(4) 0.032(3) 0.001(3) 0.007(2) -0.008(3) C10 0.039(3) 0.044(4) 0.040(3) -0.006(3) 0.008(2) 0.001(3) C11 0.031(3) 0.035(3) 0.051(3) 0.000(3) 0.008(2) 0.005(2) C12 0.024(3) 0.038(3) 0.036(3) -0.001(2) 0.004(2) -0.001(2) C13 0.052(4) 0.031(3) 0.033(3) 0.001(2) 0.010(2) -0.001(3) C14 0.051(4) 0.048(4) 0.045(3) 0.012(3) 0.002(3) 0.012(3) C15 0.047(4) 0.044(3) 0.043(3) 0.003(3) 0.005(3) -0.009(3) C16 0.043(3) 0.038(3) 0.038(3) 0.004(2) 0.004(2) 0.012(3) C17 0.035(3) 0.055(4) 0.068(4) 0.019(3) 0.010(3) -0.009(3) C18 0.045(4) 0.056(4) 0.058(4) 0.014(3) -0.001(3) 0.006(3) C19 0.033(3) 0.033(3) 0.031(3) 0.000(2) 0.008(2) -0.005(2) C20 0.031(3) 0.043(3) 0.048(3) -0.005(3) 0.014(2) 0.003(3) C21 0.030(3) 0.070(4) 0.061(4) 0.005(3) 0.020(3) 0.009(3) C22 0.050(4) 0.063(4) 0.048(4) 0.000(3) 0.023(3) 0.001(3) C23 0.048(4) 0.047(4) 0.040(3) 0.002(3) 0.011(3) -0.003(3) C24 0.036(3) 0.035(3) 0.036(3) -0.008(2) 0.007(2) -0.005(2) C25 0.037(3) 0.059(4) 0.058(4) 0.012(3) 0.017(3) 0.016(3) C26 0.080(5) 0.058(4) 0.082(5) 0.011(4) 0.025(4) 0.030(4) C27 0.044(4) 0.100(5) 0.069(4) 0.016(4) 0.004(3) 0.008(4) C28 0.036(3) 0.037(3) 0.038(3) 0.000(2) 0.004(2) -0.001(2) C29 0.048(3) 0.036(3) 0.053(3) -0.006(3) 0.001(3) -0.001(3) C30 0.046(4) 0.051(4) 0.076(4) 0.003(3) 0.003(3) 0.003(3) C31 0.036(3) 0.040(3) 0.039(3) -0.007(2) 0.006(2) -0.004(3) C32 0.030(3) 0.062(4) 0.052(3) -0.010(3) 0.001(3) -0.007(3) C33 0.029(3) 0.100(6) 0.060(4) -0.007(4) -0.013(3) 0.015(4) C34 0.049(4) 0.067(5) 0.056(4) 0.001(3) -0.004(3) 0.020(4) C35 0.048(4) 0.053(4) 0.051(4) -0.002(3) -0.005(3) 0.004(3) C36 0.031(3) 0.053(4) 0.043(3) -0.005(3) -0.001(2) 0.000(3) C37 0.096(6) 0.127(7) 0.097(6) -0.045(5) -0.009(5) 0.013(5) N1 0.026(2) 0.032(2) 0.026(2) -0.0020(18) 0.0008(17) -0.0041(19) N2 0.027(2) 0.037(2) 0.032(2) 0.0004(19) 0.0088(18) 0.0052(18) Al1 0.0370(9) 0.0345(9) 0.0369(9) -0.0029(7) 0.0040(7) -0.0012(7) P1 0.0261(7) 0.0402(8) 0.0376(7) -0.0059(6) 0.0056(6) -0.0055(6) Cl1 0.0548(9) 0.0400(9) 0.0700(10) -0.0103(7) 0.0057(7) 0.0054(7) Cl2 0.0469(9) 0.0577(10) 0.0797(11) -0.0194(8) 0.0220(8) -0.0101(7) Cl3 0.0629(10) 0.0573(10) 0.0442(8) 0.0038(7) -0.0093(7) -0.0124(8) Cl4 0.0699(10) 0.0432(8) 0.0342(7) -0.0017(6) 0.0073(6) -0.0026(7) Cl5 0.0940(16) 0.181(2) 0.0674(12) -0.0230(14) 0.0115(11) -0.0001(15) Cl6 0.181(3) 0.124(2) 0.156(2) -0.0682(19) -0.063(2) 0.035(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 C1 C2 1.513(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.358(6) . ? C2 C3 1.385(6) . ? C3 C4 1.395(6) . ? C3 C6 1.517(6) . ? C4 N2 1.348(5) . ? C4 C5 1.495(6) . ? C5 P1 1.825(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.409(6) . ? C7 C12 1.413(7) . ? C7 N1 1.449(6) . ? C8 C9 1.395(6) . ? C8 C13 1.520(7) . ? C9 C10 1.371(7) . ? C9 H9 0.9500 . ? C10 C11 1.369(7) . ? C10 H10 0.9500 . ? C11 C12 1.386(6) . ? C11 H11 0.9500 . ? C12 C16 1.520(6) . ? C13 C14 1.525(7) . ? C13 C15 1.529(7) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.527(7) . ? C16 C18 1.531(7) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.393(7) . ? C19 C24 1.404(6) . ? C19 N2 1.455(5) . ? C20 C21 1.402(7) . ? C20 C25 1.513(7) . ? C21 C22 1.374(7) . ? C21 H21 0.9500 . ? C22 C23 1.378(7) . ? C22 H22 0.9500 . ? C23 C24 1.394(7) . ? C23 H23 0.9500 . ? C24 C28 1.535(7) . ? C25 C27 1.518(8) . ? C25 C26 1.524(8) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.517(7) . ? C28 C29 1.522(7) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C36 1.384(7) . ? C31 C32 1.404(7) . ? C31 P1 1.817(5) . ? C32 C33 1.382(8) . ? C32 H32 0.9500 . ? C33 C34 1.393(8) . ? C33 H33 0.9500 . ? C34 C35 1.369(7) . ? C34 H34 0.9500 . ? C35 C36 1.399(7) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 Cl5 1.712(8) . ? C37 Cl6 1.721(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? N1 P1 1.763(4) . ? Al1 Cl2 2.121(2) . ? Al1 Cl1 2.126(2) . ? Al1 Cl3 2.131(2) . ? Al1 Cl4 2.141(2) . ? 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 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 124.4(4) . . ? N1 C2 C1 116.0(4) . . ? C3 C2 C1 119.6(4) . . ? C2 C3 C4 121.2(4) . . ? C2 C3 C6 121.0(4) . . ? C4 C3 C6 117.6(4) . . ? N2 C4 C3 121.7(4) . . ? N2 C4 C5 117.2(4) . . ? C3 C4 C5 121.1(4) . . ? C4 C5 P1 114.6(3) . . ? C4 C5 H5A 108.6 . . ? P1 C5 H5A 108.6 . . ? C4 C5 H5B 108.6 . . ? P1 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C12 121.9(4) . . ? C8 C7 N1 119.3(4) . . ? C12 C7 N1 118.6(4) . . ? C9 C8 C7 117.2(4) . . ? C9 C8 C13 119.5(4) . . ? C7 C8 C13 123.4(4) . . ? C10 C9 C8 121.4(5) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C11 C10 C9 120.4(5) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 121.8(5) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C11 C12 C7 117.2(4) . . ? C11 C12 C16 120.1(4) . . ? C7 C12 C16 122.8(4) . . ? C8 C13 C14 112.0(4) . . ? C8 C13 C15 109.9(4) . . ? C14 C13 C15 110.6(4) . . ? C8 C13 H13 108.1 . . ? C14 C13 H13 108.1 . . ? C15 C13 H13 108.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 C17 111.6(4) . . ? C12 C16 C18 111.0(4) . . ? C17 C16 C18 111.6(4) . . ? C12 C16 H16 107.5 . . ? C17 C16 H16 107.5 . . ? C18 C16 H16 107.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 123.2(4) . . ? C20 C19 N2 119.0(4) . . ? C24 C19 N2 117.8(4) . . ? C19 C20 C21 116.3(5) . . ? C19 C20 C25 122.9(4) . . ? C21 C20 C25 120.7(5) . . ? C22 C21 C20 121.9(5) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C21 C22 C23 120.4(5) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C24 120.7(5) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C23 C24 C19 117.5(5) . . ? C23 C24 C28 121.2(5) . . ? C19 C24 C28 121.2(4) . . ? C20 C25 C27 110.2(5) . . ? C20 C25 C26 110.7(4) . . ? C27 C25 C26 111.5(5) . . ? C20 C25 H25 108.1 . . ? C27 C25 H25 108.1 . . ? C26 C25 H25 108.1 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C29 111.0(4) . . ? C30 C28 C24 113.2(4) . . ? C29 C28 C24 109.4(4) . . ? C30 C28 H28 107.7 . . ? C29 C28 H28 107.7 . . ? C24 C28 H28 107.7 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 117.9(5) . . ? C36 C31 P1 128.5(4) . . ? C32 C31 P1 113.6(4) . . ? C33 C32 C31 121.0(6) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 C34 119.5(5) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C35 C34 C33 120.7(6) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C36 119.3(6) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C31 C36 C35 121.5(5) . . ? C31 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? Cl5 C37 Cl6 115.7(4) . . ? Cl5 C37 H37A 108.4 . . ? Cl6 C37 H37A 108.4 . . ? Cl5 C37 H37B 108.4 . . ? Cl6 C37 H37B 108.4 . . ? H37A C37 H37B 107.4 . . ? C2 N1 C7 122.9(4) . . ? C2 N1 P1 124.6(3) . . ? C7 N1 P1 112.1(3) . . ? C4 N2 C19 124.0(4) . . ? Cl2 Al1 Cl1 109.83(9) . . ? Cl2 Al1 Cl3 109.79(9) . . ? Cl1 Al1 Cl3 112.27(9) . . ? Cl2 Al1 Cl4 108.08(9) . . ? Cl1 Al1 Cl4 109.22(8) . . ? Cl3 Al1 Cl4 107.53(9) . . ? N1 P1 C31 103.9(2) . . ? N1 P1 C5 96.89(19) . . ? C31 P1 C5 104.0(2) . . ? 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 N1 C2 C3 C4 -20.8(7) . . . . ? C1 C2 C3 C4 162.1(4) . . . . ? N1 C2 C3 C6 163.3(4) . . . . ? C1 C2 C3 C6 -13.9(6) . . . . ? C2 C3 C4 N2 176.3(4) . . . . ? C6 C3 C4 N2 -7.6(6) . . . . ? C2 C3 C4 C5 -5.8(7) . . . . ? C6 C3 C4 C5 170.2(4) . . . . ? N2 C4 C5 P1 -142.0(4) . . . . ? C3 C4 C5 P1 40.0(6) . . . . ? C12 C7 C8 C9 -2.8(6) . . . . ? N1 C7 C8 C9 173.8(4) . . . . ? C12 C7 C8 C13 176.9(4) . . . . ? N1 C7 C8 C13 -6.6(7) . . . . ? C7 C8 C9 C10 3.2(7) . . . . ? C13 C8 C9 C10 -176.4(5) . . . . ? C8 C9 C10 C11 -1.3(7) . . . . ? C9 C10 C11 C12 -1.4(7) . . . . ? C10 C11 C12 C7 1.8(7) . . . . ? C10 C11 C12 C16 -178.4(4) . . . . ? C8 C7 C12 C11 0.3(7) . . . . ? N1 C7 C12 C11 -176.2(4) . . . . ? C8 C7 C12 C16 -179.5(4) . . . . ? N1 C7 C12 C16 3.9(6) . . . . ? C9 C8 C13 C14 -64.0(6) . . . . ? C7 C8 C13 C14 116.3(5) . . . . ? C9 C8 C13 C15 59.4(6) . . . . ? C7 C8 C13 C15 -120.2(5) . . . . ? C11 C12 C16 C17 62.2(6) . . . . ? C7 C12 C16 C17 -118.0(5) . . . . ? C11 C12 C16 C18 -63.0(6) . . . . ? C7 C12 C16 C18 116.9(5) . . . . ? C24 C19 C20 C21 1.2(7) . . . . ? N2 C19 C20 C21 179.6(4) . . . . ? C24 C19 C20 C25 -178.7(5) . . . . ? N2 C19 C20 C25 -0.3(7) . . . . ? C19 C20 C21 C22 -0.7(8) . . . . ? C25 C20 C21 C22 179.3(5) . . . . ? C20 C21 C22 C23 0.1(9) . . . . ? C21 C22 C23 C24 0.0(8) . . . . ? C22 C23 C24 C19 0.5(7) . . . . ? C22 C23 C24 C28 -175.8(5) . . . . ? C20 C19 C24 C23 -1.2(7) . . . . ? N2 C19 C24 C23 -179.6(4) . . . . ? C20 C19 C24 C28 175.1(4) . . . . ? N2 C19 C24 C28 -3.3(6) . . . . ? C19 C20 C25 C27 -115.3(6) . . . . ? C21 C20 C25 C27 64.7(6) . . . . ? C19 C20 C25 C26 120.8(5) . . . . ? C21 C20 C25 C26 -59.1(7) . . . . ? C23 C24 C28 C30 -32.9(6) . . . . ? C19 C24 C28 C30 150.9(5) . . . . ? C23 C24 C28 C29 91.3(5) . . . . ? C19 C24 C28 C29 -84.8(5) . . . . ? C36 C31 C32 C33 1.5(7) . . . . ? P1 C31 C32 C33 -179.5(4) . . . . ? C31 C32 C33 C34 -1.6(8) . . . . ? C32 C33 C34 C35 1.9(9) . . . . ? C33 C34 C35 C36 -2.1(8) . . . . ? C32 C31 C36 C35 -1.8(7) . . . . ? P1 C31 C36 C35 179.4(4) . . . . ? C34 C35 C36 C31 2.1(8) . . . . ? C3 C2 N1 C7 179.8(4) . . . . ? C1 C2 N1 C7 -3.0(6) . . . . ? C3 C2 N1 P1 7.7(6) . . . . ? C1 C2 N1 P1 -175.1(3) . . . . ? C8 C7 N1 C2 85.5(5) . . . . ? C12 C7 N1 C2 -97.9(5) . . . . ? C8 C7 N1 P1 -101.5(4) . . . . ? C12 C7 N1 P1 75.1(4) . . . . ? C3 C4 N2 C19 165.5(4) . . . . ? C5 C4 N2 C19 -12.4(6) . . . . ? C20 C19 N2 C4 107.2(5) . . . . ? C24 C19 N2 C4 -74.4(6) . . . . ? C2 N1 P1 C31 -84.4(4) . . . . ? C7 N1 P1 C31 102.7(3) . . . . ? C2 N1 P1 C5 21.9(4) . . . . ? C7 N1 P1 C5 -151.0(3) . . . . ? C36 C31 P1 N1 40.2(5) . . . . ? C32 C31 P1 N1 -138.7(4) . . . . ? C36 C31 P1 C5 -60.7(5) . . . . ? C32 C31 P1 C5 120.4(4) . . . . ? C4 C5 P1 N1 -42.2(4) . . . . ? C4 C5 P1 C31 64.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.629 _refine_diff_density_min -0.864 _refine_diff_density_rms 0.076