# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Daniel Mindiola' _publ_contact_author_email MINDIOLA@INDIANA.EDU _publ_section_title ; Phosphinidene Group-Transfer with the Phospha-Wittig Reagent Me3P=PAr (Ar = 2,4,6-tBu3C6H2 and 2,6-Mes2C6H3). New Entry Way to Transition Metal Phosphorus Multiple Bonds. ; loop_ _publ_author_name 'Daniel Mindiola' 'Hongjun Fan' 'Uriah J Kilgore' 'Maren Pink' 'J Protasiewicz' 'Eugenijus Urnezius' # Attachment '08120.cif' data_08120 _database_code_depnum_ccdc_archive 'CCDC 730564' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H79 N P3 V' _chemical_formula_sum 'C49 H79 N P3 V' _chemical_formula_weight 825.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.6462(19) _cell_length_b 20.238(3) _cell_length_c 18.507(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.990(3) _cell_angle_gamma 90.00 _cell_volume 4690.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4204 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 26.2 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.346 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.9308 _exptl_absorpt_correction_T_max 0.9629 _exptl_absorpt_process_details 'SADABS, R. Blessing; 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details '0.30 degree frames measured for 30 seconds each' _diffrn_measurement_method 'omega and phi scans' _diffrn_measurement_device 'APEX Kappa Duo' _diffrn_measurement_device_type Kappa _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker APEXII' _diffrn_detector_area_resol_mean 83.33 _diffrn_reflns_number 44669 _diffrn_reflns_av_R_equivalents 0.1059 _diffrn_reflns_av_sigmaI/netI 0.0872 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 26.44 _reflns_number_total 9627 _reflns_number_gt 6262 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II v.2.2 (Bruker, 2007)' _computing_cell_refinement 'APEX II v.2.2 (Bruker, 2007)' _computing_data_reduction 'APEX II v.2.2 (Bruker, 2007)' _computing_structure_solution 'SIR-2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Bruker, 2008)' _computing_publication_material 'SHELXTL (Bruker, 2008)' _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^)+(0.0386P)^2^+1.1745P] 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 9627 _refine_ls_number_parameters 509 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0902 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1116 _refine_ls_wR_factor_gt 0.0947 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 V1 V 0.71992(3) 0.19252(2) 0.91345(2) 0.01566(11) Uani 1 1 d . . . P1 P 0.64725(5) 0.10405(3) 0.82600(4) 0.01756(16) Uani 1 1 d . . . P2 P 0.70103(5) 0.30300(3) 0.96897(3) 0.01719(15) Uani 1 1 d . . . P3 P 0.88420(5) 0.19932(4) 0.89754(4) 0.02062(16) Uani 1 1 d . . . N1 N 0.58524(16) 0.23385(10) 0.85424(11) 0.0179(5) Uani 1 1 d . . . C1 C 0.6781(2) 0.10573(13) 0.73076(13) 0.0211(6) Uani 1 1 d . . . H1 H 0.7573 0.1014 0.7333 0.025 Uiso 1 1 calc R . . C2 C 0.6468(2) 0.17230(14) 0.69547(14) 0.0261(6) Uani 1 1 d . . . H2A H 0.6723 0.1749 0.6479 0.039 Uiso 1 1 calc R . . H2B H 0.6791 0.2079 0.7270 0.039 Uiso 1 1 calc R . . H2C H 0.5689 0.1769 0.6888 0.039 Uiso 1 1 calc R . . C3 C 0.6278(2) 0.04992(15) 0.68210(15) 0.0318(7) Uani 1 1 d . . . H3A H 0.6430 0.0567 0.6321 0.048 Uiso 1 1 calc R . . H3B H 0.5504 0.0497 0.6825 0.048 Uiso 1 1 calc R . . H3C H 0.6579 0.0075 0.7005 0.048 Uiso 1 1 calc R . . C4 C 0.6516(2) 0.01526(13) 0.84729(14) 0.0215(6) Uani 1 1 d . . . H4 H 0.6055 -0.0082 0.8070 0.026 Uiso 1 1 calc R . . C5 C 0.6083(2) 0.00025(15) 0.91848(15) 0.0286(7) Uani 1 1 d . . . H5A H 0.6037 -0.0477 0.9247 0.043 Uiso 1 1 calc R . . H5B H 0.5371 0.0198 0.9169 0.043 Uiso 1 1 calc R . . H5C H 0.6563 0.0190 0.9595 0.043 Uiso 1 1 calc R . . C6 C 0.7654(2) -0.01037(15) 0.84924(16) 0.0314(7) Uani 1 1 d . . . H6A H 0.7676 -0.0575 0.8614 0.047 Uiso 1 1 calc R . . H6B H 0.8132 0.0139 0.8862 0.047 Uiso 1 1 calc R . . H6C H 0.7886 -0.0040 0.8013 0.047 Uiso 1 1 calc R . . C7 C 0.50804(19) 0.12822(13) 0.81635(13) 0.0179(6) Uani 1 1 d . . . C8 C 0.4198(2) 0.08780(14) 0.79602(13) 0.0211(6) Uani 1 1 d . . . H8 H 0.4305 0.0423 0.7869 0.025 Uiso 1 1 calc R . . C9 C 0.3164(2) 0.11257(14) 0.78873(14) 0.0228(6) Uani 1 1 d . . . C10 C 0.2211(2) 0.06880(15) 0.76705(16) 0.0299(7) Uani 1 1 d . . . H10A H 0.1572 0.0962 0.7549 0.045 Uiso 1 1 calc R . . H10B H 0.2115 0.0394 0.8077 0.045 Uiso 1 1 calc R . . H10C H 0.2326 0.0424 0.7244 0.045 Uiso 1 1 calc R . . C11 C 0.3039(2) 0.17884(14) 0.80334(14) 0.0245(6) Uani 1 1 d . . . H11 H 0.2339 0.1968 0.7994 0.029 Uiso 1 1 calc R . . C12 C 0.38984(19) 0.21950(14) 0.82345(14) 0.0219(6) Uani 1 1 d . . . H12A H 0.3780 0.2649 0.8328 0.026 Uiso 1 1 calc R . . C13 C 0.49486(19) 0.19543(13) 0.83045(13) 0.0182(6) Uani 1 1 d . . . C14 C 0.57893(18) 0.30197(13) 0.83887(13) 0.0170(5) Uani 1 1 d . . . C15 C 0.5290(2) 0.32861(13) 0.77332(14) 0.0213(6) Uani 1 1 d . . . H15 H 0.4960 0.3000 0.7361 0.026 Uiso 1 1 calc R . . C16 C 0.5269(2) 0.39590(14) 0.76188(14) 0.0236(6) Uani 1 1 d . . . H16 H 0.4923 0.4127 0.7167 0.028 Uiso 1 1 calc R . . C17 C 0.5739(2) 0.44016(13) 0.81452(14) 0.0202(6) Uani 1 1 d . . . C18 C 0.5625(2) 0.51378(14) 0.80438(15) 0.0269(7) Uani 1 1 d . . . H18A H 0.6254 0.5359 0.8305 0.040 Uiso 1 1 calc R . . H18B H 0.4983 0.5289 0.8237 0.040 Uiso 1 1 calc R . . H18C H 0.5563 0.5244 0.7523 0.040 Uiso 1 1 calc R . . C19 C 0.62739(19) 0.41330(13) 0.87823(14) 0.0201(6) Uani 1 1 d . . . H19 H 0.6622 0.4421 0.9145 0.024 Uiso 1 1 calc R . . C20 C 0.63162(19) 0.34595(13) 0.89067(13) 0.0164(5) Uani 1 1 d . . . C21 C 0.6037(2) 0.30663(14) 1.03620(13) 0.0220(6) Uani 1 1 d . . . H21 H 0.6361 0.2818 1.0806 0.026 Uiso 1 1 calc R . . C22 C 0.5802(2) 0.37624(15) 1.06073(16) 0.0323(7) Uani 1 1 d . . . H22A H 0.5267 0.3743 1.0942 0.048 Uiso 1 1 calc R . . H22B H 0.5529 0.4030 1.0181 0.048 Uiso 1 1 calc R . . H22C H 0.6460 0.3962 1.0857 0.048 Uiso 1 1 calc R . . C23 C 0.4989(2) 0.27269(14) 1.00781(15) 0.0258(6) Uani 1 1 d . . . H23A H 0.4510 0.2747 1.0451 0.039 Uiso 1 1 calc R . . H23B H 0.5126 0.2264 0.9966 0.039 Uiso 1 1 calc R . . H23C H 0.4655 0.2951 0.9635 0.039 Uiso 1 1 calc R . . C24 C 0.8042(2) 0.36237(13) 1.00803(14) 0.0219(6) Uani 1 1 d . . . H24 H 0.7667 0.4046 1.0166 0.026 Uiso 1 1 calc R . . C25 C 0.8601(2) 0.33904(15) 1.08230(15) 0.0306(7) Uani 1 1 d . . . H25A H 0.9104 0.3731 1.1034 0.046 Uiso 1 1 calc R . . H25B H 0.8990 0.2980 1.0761 0.046 Uiso 1 1 calc R . . H25C H 0.8068 0.3311 1.1150 0.046 Uiso 1 1 calc R . . C26 C 0.8850(2) 0.37831(15) 0.95750(16) 0.0303(7) Uani 1 1 d . . . H26A H 0.9307 0.4147 0.9780 0.045 Uiso 1 1 calc R . . H26B H 0.8475 0.3913 0.9097 0.045 Uiso 1 1 calc R . . H26C H 0.9289 0.3392 0.9520 0.045 Uiso 1 1 calc R . . C27 C 0.7094(2) 0.14684(13) 0.99719(13) 0.0199(6) Uani 1 1 d . . . H27 H 0.6345 0.1397 0.9930 0.024 Uiso 1 1 calc R . . C28 C 0.7478(2) 0.11317(13) 1.06986(14) 0.0205(6) Uani 1 1 d . . . C29 C 0.7878(2) 0.16611(14) 1.12646(14) 0.0263(6) Uani 1 1 d . . . H29A H 0.8166 0.1447 1.1725 0.039 Uiso 1 1 calc R . . H29B H 0.7283 0.1951 1.1344 0.039 Uiso 1 1 calc R . . H29C H 0.8439 0.1923 1.1086 0.039 Uiso 1 1 calc R . . C30 C 0.8393(2) 0.06601(14) 1.06075(16) 0.0279(7) Uani 1 1 d . . . H30A H 0.8690 0.0480 1.1085 0.042 Uiso 1 1 calc R . . H30B H 0.8952 0.0900 1.0398 0.042 Uiso 1 1 calc R . . H30C H 0.8126 0.0298 1.0281 0.042 Uiso 1 1 calc R . . C31 C 0.6580(2) 0.07516(15) 1.09944(15) 0.0289(7) Uani 1 1 d . . . H31A H 0.6828 0.0604 1.1493 0.043 Uiso 1 1 calc R . . H31B H 0.6379 0.0367 1.0684 0.043 Uiso 1 1 calc R . . H31C H 0.5959 0.1041 1.0995 0.043 Uiso 1 1 calc R . . C32 C 1.00586(19) 0.24254(13) 0.88298(13) 0.0179(6) Uani 1 1 d . . . C33 C 1.00714(19) 0.28850(13) 0.82472(13) 0.0185(6) Uani 1 1 d . . . C34 C 1.0796(2) 0.33980(13) 0.83379(14) 0.0198(6) Uani 1 1 d . . . H34 H 1.0792 0.3711 0.7955 0.024 Uiso 1 1 calc R . . C35 C 1.15331(19) 0.34779(13) 0.89649(14) 0.0193(6) Uani 1 1 d . . . C36 C 1.16355(19) 0.29574(13) 0.94496(14) 0.0188(6) Uani 1 1 d . . . H36 H 1.2200 0.2970 0.9846 0.023 Uiso 1 1 calc R . . C37 C 1.09537(19) 0.24139(13) 0.93890(13) 0.0187(6) Uani 1 1 d . . . C38 C 0.9320(2) 0.28423(13) 0.75146(13) 0.0210(6) Uani 1 1 d . . . C39 C 0.9216(2) 0.21284(14) 0.72535(15) 0.0282(7) Uani 1 1 d . . . H39A H 0.8762 0.2110 0.6780 0.042 Uiso 1 1 calc R . . H39B H 0.8894 0.1863 0.7609 0.042 Uiso 1 1 calc R . . H39C H 0.9925 0.1953 0.7204 0.042 Uiso 1 1 calc R . . C40 C 0.9785(2) 0.32227(15) 0.69129(14) 0.0290(7) Uani 1 1 d . . . H40A H 0.9352 0.3135 0.6441 0.044 Uiso 1 1 calc R . . H40B H 1.0521 0.3078 0.6897 0.044 Uiso 1 1 calc R . . H40C H 0.9777 0.3697 0.7017 0.044 Uiso 1 1 calc R . . C41 C 0.8233(2) 0.31530(14) 0.75757(15) 0.0266(6) Uani 1 1 d . . . H41A H 0.7780 0.3130 0.7101 0.040 Uiso 1 1 calc R . . H41B H 0.8331 0.3616 0.7725 0.040 Uiso 1 1 calc R . . H41C H 0.7891 0.2912 0.7940 0.040 Uiso 1 1 calc R . . C42 C 1.2205(2) 0.41095(13) 0.90757(14) 0.0205(6) Uani 1 1 d . . . C43 C 1.2740(2) 0.41825(15) 0.98640(16) 0.0342(7) Uani 1 1 d . . . H43A H 1.3234 0.3814 0.9988 0.051 Uiso 1 1 calc R . . H43B H 1.2194 0.4180 1.0191 0.051 Uiso 1 1 calc R . . H43C H 1.3135 0.4600 0.9918 0.051 Uiso 1 1 calc R . . C44 C 1.1490(2) 0.47133(14) 0.88920(17) 0.0304(7) Uani 1 1 d . . . H44A H 1.1164 0.4691 0.8380 0.046 Uiso 1 1 calc R . . H44B H 1.1919 0.5116 0.8971 0.046 Uiso 1 1 calc R . . H44C H 1.0927 0.4719 0.9207 0.046 Uiso 1 1 calc R . . C45 C 1.3068(2) 0.41015(15) 0.85761(16) 0.0303(7) Uani 1 1 d . . . H45A H 1.3565 0.3737 0.8717 0.046 Uiso 1 1 calc R . . H45B H 1.3457 0.4522 0.8621 0.046 Uiso 1 1 calc R . . H45C H 1.2735 0.4040 0.8070 0.046 Uiso 1 1 calc R . . C46 C 1.1215(2) 0.18389(13) 0.99314(14) 0.0216(6) Uani 1 1 d . . . C47 C 1.0596(2) 0.19025(15) 1.05796(14) 0.0279(6) Uani 1 1 d . . . H47A H 0.9828 0.1892 1.0406 0.042 Uiso 1 1 calc R . . H47B H 1.0781 0.2321 1.0832 0.042 Uiso 1 1 calc R . . H47C H 1.0783 0.1535 1.0918 0.042 Uiso 1 1 calc R . . C48 C 1.1002(2) 0.11684(14) 0.95542(16) 0.0318(7) Uani 1 1 d . . . H48A H 1.0243 0.1133 0.9360 0.048 Uiso 1 1 calc R . . H48B H 1.1197 0.0813 0.9908 0.048 Uiso 1 1 calc R . . H48C H 1.1430 0.1131 0.9154 0.048 Uiso 1 1 calc R . . C49 C 1.2415(2) 0.18388(15) 1.02332(17) 0.0342(8) Uani 1 1 d . . . H49A H 1.2576 0.2217 1.0561 0.051 Uiso 1 1 calc R . . H49B H 1.2835 0.1871 0.9828 0.051 Uiso 1 1 calc R . . H49C H 1.2596 0.1428 1.0503 0.051 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 V1 0.0134(2) 0.0156(2) 0.0175(2) -0.00056(19) 0.00040(16) -0.00124(18) P1 0.0160(3) 0.0159(4) 0.0200(3) -0.0002(3) -0.0001(3) -0.0008(3) P2 0.0152(3) 0.0172(4) 0.0187(3) -0.0016(3) 0.0008(2) -0.0005(3) P3 0.0167(3) 0.0215(4) 0.0240(3) -0.0028(3) 0.0042(3) -0.0034(3) N1 0.0164(11) 0.0149(12) 0.0215(11) 0.0000(9) -0.0003(9) -0.0019(9) C1 0.0197(13) 0.0218(16) 0.0219(13) -0.0033(12) 0.0039(11) -0.0014(11) C2 0.0294(15) 0.0262(17) 0.0223(14) 0.0033(12) 0.0021(12) -0.0020(12) C3 0.0394(18) 0.0317(19) 0.0241(15) -0.0055(13) 0.0034(13) -0.0058(14) C4 0.0262(14) 0.0133(15) 0.0245(14) -0.0010(11) 0.0016(11) 0.0003(11) C5 0.0309(15) 0.0220(17) 0.0328(16) 0.0034(13) 0.0039(13) -0.0031(12) C6 0.0352(17) 0.0234(17) 0.0360(16) 0.0057(14) 0.0068(13) 0.0091(13) C7 0.0140(12) 0.0208(16) 0.0190(13) 0.0009(11) 0.0032(10) 0.0008(11) C8 0.0235(14) 0.0183(15) 0.0209(13) -0.0016(11) 0.0002(11) -0.0037(11) C9 0.0201(13) 0.0247(17) 0.0228(14) 0.0006(12) -0.0003(11) -0.0058(12) C10 0.0233(15) 0.0306(18) 0.0340(16) -0.0034(13) -0.0024(12) -0.0048(13) C11 0.0158(13) 0.0283(18) 0.0283(15) -0.0010(12) -0.0003(11) 0.0007(11) C12 0.0185(13) 0.0187(15) 0.0279(14) -0.0036(12) 0.0012(11) 0.0009(11) C13 0.0176(12) 0.0202(15) 0.0160(12) -0.0012(11) 0.0000(10) -0.0028(11) C14 0.0134(12) 0.0172(15) 0.0206(13) -0.0028(11) 0.0028(10) 0.0012(10) C15 0.0193(13) 0.0221(16) 0.0211(13) -0.0033(12) -0.0023(11) -0.0029(11) C16 0.0196(13) 0.0272(17) 0.0237(14) 0.0032(12) 0.0016(11) 0.0020(12) C17 0.0161(13) 0.0183(15) 0.0273(14) 0.0019(12) 0.0069(11) 0.0013(11) C18 0.0266(15) 0.0203(16) 0.0339(16) 0.0056(13) 0.0045(12) 0.0014(12) C19 0.0169(13) 0.0214(16) 0.0222(13) -0.0043(12) 0.0027(11) -0.0025(11) C20 0.0154(12) 0.0165(15) 0.0175(13) 0.0012(11) 0.0033(10) -0.0007(10) C21 0.0212(13) 0.0264(16) 0.0187(13) -0.0003(12) 0.0035(10) 0.0043(12) C22 0.0277(15) 0.0350(19) 0.0358(17) -0.0087(14) 0.0105(13) -0.0015(13) C23 0.0172(13) 0.0295(17) 0.0318(15) 0.0008(13) 0.0074(11) -0.0011(12) C24 0.0184(13) 0.0175(15) 0.0287(15) -0.0071(12) -0.0007(11) -0.0022(11) C25 0.0275(15) 0.0258(17) 0.0349(17) -0.0054(13) -0.0086(13) -0.0025(13) C26 0.0215(14) 0.0270(18) 0.0426(17) -0.0102(14) 0.0047(13) -0.0061(12) C27 0.0206(13) 0.0173(15) 0.0226(14) -0.0031(11) 0.0055(11) -0.0033(11) C28 0.0200(13) 0.0213(16) 0.0201(13) 0.0039(11) 0.0028(10) -0.0015(11) C29 0.0279(15) 0.0252(17) 0.0249(14) 0.0009(12) 0.0003(12) -0.0030(12) C30 0.0290(15) 0.0239(17) 0.0303(15) 0.0022(13) 0.0017(13) 0.0042(12) C31 0.0300(15) 0.0319(18) 0.0256(15) 0.0054(13) 0.0067(12) -0.0039(13) C32 0.0151(12) 0.0155(15) 0.0240(13) -0.0008(11) 0.0053(10) -0.0015(10) C33 0.0145(12) 0.0199(15) 0.0216(13) -0.0010(11) 0.0048(10) 0.0019(11) C34 0.0205(13) 0.0186(15) 0.0210(13) 0.0043(11) 0.0052(11) 0.0015(11) C35 0.0155(12) 0.0203(15) 0.0223(13) -0.0016(11) 0.0035(10) -0.0001(11) C36 0.0146(12) 0.0190(15) 0.0224(13) 0.0001(11) 0.0008(10) 0.0008(11) C37 0.0144(12) 0.0213(15) 0.0214(13) -0.0003(11) 0.0060(10) 0.0013(11) C38 0.0225(14) 0.0219(16) 0.0183(13) -0.0005(11) 0.0021(11) -0.0032(11) C39 0.0269(15) 0.0332(19) 0.0234(14) -0.0070(13) 0.0000(12) -0.0017(13) C40 0.0288(15) 0.0376(19) 0.0202(14) 0.0003(13) 0.0014(12) -0.0069(13) C41 0.0220(14) 0.0302(18) 0.0261(14) 0.0005(13) -0.0016(11) 0.0009(12) C42 0.0183(13) 0.0185(15) 0.0244(14) 0.0004(12) 0.0019(11) -0.0017(11) C43 0.0385(17) 0.0279(18) 0.0338(17) -0.0027(14) -0.0034(14) -0.0122(14) C44 0.0242(15) 0.0190(16) 0.0475(18) -0.0035(14) 0.0031(13) 0.0011(12) C45 0.0268(15) 0.0240(17) 0.0426(17) 0.0016(14) 0.0128(13) -0.0052(13) C46 0.0198(13) 0.0206(16) 0.0242(14) 0.0033(12) 0.0018(11) 0.0008(11) C47 0.0325(15) 0.0266(17) 0.0249(14) 0.0026(13) 0.0048(12) -0.0025(13) C48 0.0361(17) 0.0220(17) 0.0375(17) 0.0020(14) 0.0060(14) 0.0079(13) C49 0.0215(14) 0.0352(19) 0.0438(18) 0.0182(15) -0.0032(13) 0.0024(13) _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 V1 C27 1.825(3) . ? V1 N1 2.069(2) . ? V1 P3 2.1428(8) . ? V1 P2 2.4860(9) . ? V1 P1 2.5011(8) . ? P1 C7 1.812(3) . ? P1 C4 1.839(3) . ? P1 C1 1.858(3) . ? P2 C20 1.809(2) . ? P2 C24 1.846(3) . ? P2 C21 1.869(3) . ? P3 C32 1.822(3) . ? N1 C13 1.402(3) . ? N1 C14 1.408(3) . ? C1 C2 1.525(4) . ? C1 C3 1.527(4) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C6 1.526(4) . ? C4 C5 1.526(4) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.393(3) . ? C7 C13 1.399(4) . ? C8 C9 1.389(4) . ? C8 H8 0.9500 . ? C9 C11 1.382(4) . ? C9 C10 1.505(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.373(4) . ? C11 H11 0.9500 . ? C12 C13 1.404(3) . ? C12 H12A 0.9500 . ? C14 C15 1.396(3) . ? C14 C20 1.406(3) . ? C15 C16 1.378(4) . ? C15 H15 0.9500 . ? C16 C17 1.395(4) . ? C16 H16 0.9500 . ? C17 C19 1.386(3) . ? C17 C18 1.506(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.382(4) . ? C19 H19 0.9500 . ? C21 C23 1.520(3) . ? C21 C22 1.522(4) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C26 1.512(4) . ? C24 C25 1.530(4) . ? 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(3) . ? C27 H27 0.9500 . ? C28 C30 1.527(4) . ? C28 C29 1.534(4) . ? C28 C31 1.534(4) . ? 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 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C37 1.424(3) . ? C32 C33 1.426(4) . ? C33 C34 1.379(4) . ? C33 C38 1.546(3) . ? C34 C35 1.393(3) . ? C34 H34 0.9500 . ? C35 C36 1.378(4) . ? C35 C42 1.532(4) . ? C36 C37 1.392(3) . ? C36 H36 0.9500 . ? C37 C46 1.542(4) . ? C38 C39 1.523(4) . ? C38 C41 1.531(4) . ? C38 C40 1.536(4) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C45 1.525(4) . ? C42 C43 1.528(4) . ? C42 C44 1.530(4) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.526(4) . ? C46 C48 1.532(4) . ? C46 C49 1.543(3) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C27 V1 N1 120.16(10) . . ? C27 V1 P3 109.62(9) . . ? N1 V1 P3 130.07(6) . . ? C27 V1 P2 94.70(8) . . ? N1 V1 P2 74.70(6) . . ? P3 V1 P2 98.61(3) . . ? C27 V1 P1 97.08(8) . . ? N1 V1 P1 75.25(6) . . ? P3 V1 P1 103.48(3) . . ? P2 V1 P1 149.71(3) . . ? C7 P1 C4 106.54(12) . . ? C7 P1 C1 103.34(11) . . ? C4 P1 C1 102.55(12) . . ? C7 P1 V1 97.76(9) . . ? C4 P1 V1 124.30(9) . . ? C1 P1 V1 119.61(9) . . ? C20 P2 C24 103.82(12) . . ? C20 P2 C21 102.91(12) . . ? C24 P2 C21 102.05(12) . . ? C20 P2 V1 99.49(9) . . ? C24 P2 V1 130.09(9) . . ? C21 P2 V1 114.87(9) . . ? C32 P3 V1 154.94(9) . . ? C13 N1 C14 117.3(2) . . ? C13 N1 V1 121.15(17) . . ? C14 N1 V1 121.48(15) . . ? C2 C1 C3 109.8(2) . . ? C2 C1 P1 110.27(18) . . ? C3 C1 P1 114.91(19) . . ? C2 C1 H1 107.2 . . ? C3 C1 H1 107.2 . . ? P1 C1 H1 107.2 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C6 C4 C5 111.3(2) . . ? C6 C4 P1 109.73(19) . . ? C5 C4 P1 112.08(19) . . ? C6 C4 H4 107.9 . . ? C5 C4 H4 107.9 . . ? P1 C4 H4 107.9 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C13 120.6(2) . . ? C8 C7 P1 126.8(2) . . ? C13 C7 P1 112.54(18) . . ? C9 C8 C7 121.5(3) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C11 C9 C8 117.6(2) . . ? C11 C9 C10 121.0(2) . . ? C8 C9 C10 121.4(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C9 121.8(2) . . ? C12 C11 H11 119.1 . . ? C9 C11 H11 119.1 . . ? C11 C12 C13 121.4(3) . . ? C11 C12 H12A 119.3 . . ? C13 C12 H12A 119.3 . . ? C7 C13 N1 119.0(2) . . ? C7 C13 C12 117.1(2) . . ? N1 C13 C12 123.8(2) . . ? C15 C14 C20 117.5(2) . . ? C15 C14 N1 124.1(2) . . ? C20 C14 N1 118.3(2) . . ? C16 C15 C14 120.8(2) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 122.0(2) . . ? C15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C19 C17 C16 116.9(2) . . ? C19 C17 C18 121.4(2) . . ? C16 C17 C18 121.6(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C17 122.1(2) . . ? C20 C19 H19 118.9 . . ? C17 C19 H19 118.9 . . ? C19 C20 C14 120.5(2) . . ? C19 C20 P2 127.63(19) . . ? C14 C20 P2 111.91(19) . . ? C23 C21 C22 108.9(2) . . ? C23 C21 P2 112.04(18) . . ? C22 C21 P2 114.1(2) . . ? C23 C21 H21 107.1 . . ? C22 C21 H21 107.1 . . ? P2 C21 H21 107.1 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C26 C24 C25 110.7(2) . . ? C26 C24 P2 113.46(18) . . ? C25 C24 P2 111.35(19) . . ? C26 C24 H24 107.0 . . ? C25 C24 H24 107.0 . . ? P2 C24 H24 107.0 . . ? 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 . . ? C28 C27 V1 157.3(2) . . ? C28 C27 H27 101.3 . . ? V1 C27 H27 101.3 . . ? C27 C28 C30 109.6(2) . . ? C27 C28 C29 108.9(2) . . ? C30 C28 C29 109.2(2) . . ? C27 C28 C31 112.2(2) . . ? C30 C28 C31 109.6(2) . . ? C29 C28 C31 107.2(2) . . ? 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 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C37 C32 C33 118.0(2) . . ? C37 C32 P3 119.14(19) . . ? C33 C32 P3 121.58(18) . . ? C34 C33 C32 118.4(2) . . ? C34 C33 C38 117.7(2) . . ? C32 C33 C38 123.8(2) . . ? C33 C34 C35 123.0(2) . . ? C33 C34 H34 118.5 . . ? C35 C34 H34 118.5 . . ? C36 C35 C34 116.4(2) . . ? C36 C35 C42 123.4(2) . . ? C34 C35 C42 120.2(2) . . ? C35 C36 C37 123.4(2) . . ? C35 C36 H36 118.3 . . ? C37 C36 H36 118.3 . . ? C36 C37 C32 117.8(2) . . ? C36 C37 C46 118.0(2) . . ? C32 C37 C46 124.2(2) . . ? C39 C38 C41 112.0(2) . . ? C39 C38 C40 105.7(2) . . ? C41 C38 C40 106.6(2) . . ? C39 C38 C33 110.3(2) . . ? C41 C38 C33 111.2(2) . . ? C40 C38 C33 111.0(2) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C45 C42 C43 108.7(2) . . ? C45 C42 C44 108.9(2) . . ? C43 C42 C44 107.7(2) . . ? C45 C42 C35 109.9(2) . . ? C43 C42 C35 111.9(2) . . ? C44 C42 C35 109.7(2) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 C48 110.9(2) . . ? C47 C46 C37 111.2(2) . . ? C48 C46 C37 111.3(2) . . ? C47 C46 C49 107.5(2) . . ? C48 C46 C49 105.5(2) . . ? C37 C46 C49 110.3(2) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? 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 C27 V1 P1 C7 91.12(12) . . . . ? N1 V1 P1 C7 -28.28(10) . . . . ? P3 V1 P1 C7 -156.70(9) . . . . ? P2 V1 P1 C7 -20.99(11) . . . . ? C27 V1 P1 C4 -25.04(14) . . . . ? N1 V1 P1 C4 -144.44(12) . . . . ? P3 V1 P1 C4 87.14(11) . . . . ? P2 V1 P1 C4 -137.15(11) . . . . ? C27 V1 P1 C1 -158.69(13) . . . . ? N1 V1 P1 C1 81.92(11) . . . . ? P3 V1 P1 C1 -46.50(10) . . . . ? P2 V1 P1 C1 89.21(11) . . . . ? C27 V1 P2 C20 -147.11(12) . . . . ? N1 V1 P2 C20 -27.10(10) . . . . ? P3 V1 P2 C20 102.21(8) . . . . ? P1 V1 P2 C20 -34.41(10) . . . . ? C27 V1 P2 C24 95.68(14) . . . . ? N1 V1 P2 C24 -144.31(13) . . . . ? P3 V1 P2 C24 -15.00(12) . . . . ? P1 V1 P2 C24 -151.62(12) . . . . ? C27 V1 P2 C21 -38.02(12) . . . . ? N1 V1 P2 C21 81.99(11) . . . . ? P3 V1 P2 C21 -148.70(9) . . . . ? P1 V1 P2 C21 74.68(11) . . . . ? C27 V1 P3 C32 -124.7(2) . . . . ? N1 V1 P3 C32 50.6(2) . . . . ? P2 V1 P3 C32 -26.6(2) . . . . ? P1 V1 P3 C32 132.6(2) . . . . ? C27 V1 N1 C13 -54.8(2) . . . . ? P3 V1 N1 C13 130.26(17) . . . . ? P2 V1 N1 C13 -141.30(19) . . . . ? P1 V1 N1 C13 34.89(17) . . . . ? C27 V1 N1 C14 122.52(19) . . . . ? P3 V1 N1 C14 -52.4(2) . . . . ? P2 V1 N1 C14 36.01(17) . . . . ? P1 V1 N1 C14 -147.80(19) . . . . ? C7 P1 C1 C2 52.9(2) . . . . ? C4 P1 C1 C2 163.51(18) . . . . ? V1 P1 C1 C2 -54.3(2) . . . . ? C7 P1 C1 C3 -71.9(2) . . . . ? C4 P1 C1 C3 38.8(2) . . . . ? V1 P1 C1 C3 -179.01(16) . . . . ? C7 P1 C4 C6 174.72(18) . . . . ? C1 P1 C4 C6 66.5(2) . . . . ? V1 P1 C4 C6 -73.4(2) . . . . ? C7 P1 C4 C5 -61.1(2) . . . . ? C1 P1 C4 C5 -169.36(19) . . . . ? V1 P1 C4 C5 50.8(2) . . . . ? C4 P1 C7 C8 -26.4(3) . . . . ? C1 P1 C7 C8 81.3(2) . . . . ? V1 P1 C7 C8 -155.7(2) . . . . ? C4 P1 C7 C13 154.88(18) . . . . ? C1 P1 C7 C13 -97.47(19) . . . . ? V1 P1 C7 C13 25.55(19) . . . . ? C13 C7 C8 C9 0.3(4) . . . . ? P1 C7 C8 C9 -178.4(2) . . . . ? C7 C8 C9 C11 -0.8(4) . . . . ? C7 C8 C9 C10 -179.8(2) . . . . ? C8 C9 C11 C12 0.8(4) . . . . ? C10 C9 C11 C12 179.8(3) . . . . ? C9 C11 C12 C13 -0.3(4) . . . . ? C8 C7 C13 N1 176.9(2) . . . . ? P1 C7 C13 N1 -4.3(3) . . . . ? C8 C7 C13 C12 0.3(4) . . . . ? P1 C7 C13 C12 179.11(19) . . . . ? C14 N1 C13 C7 153.7(2) . . . . ? V1 N1 C13 C7 -28.9(3) . . . . ? C14 N1 C13 C12 -29.9(3) . . . . ? V1 N1 C13 C12 147.5(2) . . . . ? C11 C12 C13 C7 -0.3(4) . . . . ? C11 C12 C13 N1 -176.7(2) . . . . ? C13 N1 C14 C15 -39.7(3) . . . . ? V1 N1 C14 C15 142.9(2) . . . . ? C13 N1 C14 C20 144.4(2) . . . . ? V1 N1 C14 C20 -33.0(3) . . . . ? C20 C14 C15 C16 -3.4(4) . . . . ? N1 C14 C15 C16 -179.4(2) . . . . ? C14 C15 C16 C17 0.0(4) . . . . ? C15 C16 C17 C19 2.7(4) . . . . ? C15 C16 C17 C18 -174.2(3) . . . . ? C16 C17 C19 C20 -2.0(4) . . . . ? C18 C17 C19 C20 175.0(2) . . . . ? C17 C19 C20 C14 -1.4(4) . . . . ? C17 C19 C20 P2 177.8(2) . . . . ? C15 C14 C20 C19 4.1(4) . . . . ? N1 C14 C20 C19 -179.7(2) . . . . ? C15 C14 C20 P2 -175.29(19) . . . . ? N1 C14 C20 P2 0.9(3) . . . . ? C24 P2 C20 C19 -21.9(3) . . . . ? C21 P2 C20 C19 84.2(3) . . . . ? V1 P2 C20 C19 -157.4(2) . . . . ? C24 P2 C20 C14 157.45(18) . . . . ? C21 P2 C20 C14 -96.47(19) . . . . ? V1 P2 C20 C14 21.93(18) . . . . ? C20 P2 C21 C23 60.4(2) . . . . ? C24 P2 C21 C23 167.82(19) . . . . ? V1 P2 C21 C23 -46.6(2) . . . . ? C20 P2 C21 C22 -64.0(2) . . . . ? C24 P2 C21 C22 43.5(2) . . . . ? V1 P2 C21 C22 -170.98(16) . . . . ? C20 P2 C24 C26 -63.4(2) . . . . ? C21 P2 C24 C26 -170.1(2) . . . . ? V1 P2 C24 C26 52.0(2) . . . . ? C20 P2 C24 C25 170.87(19) . . . . ? C21 P2 C24 C25 64.1(2) . . . . ? V1 P2 C24 C25 -73.7(2) . . . . ? N1 V1 C27 C28 -164.9(5) . . . . ? P3 V1 C27 C28 11.0(5) . . . . ? P2 V1 C27 C28 -89.8(5) . . . . ? P1 V1 C27 C28 118.1(5) . . . . ? V1 C27 C28 C30 -50.2(6) . . . . ? V1 C27 C28 C29 69.3(6) . . . . ? V1 C27 C28 C31 -172.2(4) . . . . ? V1 P3 C32 C37 113.2(2) . . . . ? V1 P3 C32 C33 -53.4(3) . . . . ? C37 C32 C33 C34 -15.9(4) . . . . ? P3 C32 C33 C34 150.8(2) . . . . ? C37 C32 C33 C38 163.9(2) . . . . ? P3 C32 C33 C38 -29.3(3) . . . . ? C32 C33 C34 C35 1.7(4) . . . . ? C38 C33 C34 C35 -178.2(2) . . . . ? C33 C34 C35 C36 10.7(4) . . . . ? C33 C34 C35 C42 -171.3(2) . . . . ? C34 C35 C36 C37 -8.9(4) . . . . ? C42 C35 C36 C37 173.2(2) . . . . ? C35 C36 C37 C32 -5.1(4) . . . . ? C35 C36 C37 C46 175.0(2) . . . . ? C33 C32 C37 C36 17.5(4) . . . . ? P3 C32 C37 C36 -149.6(2) . . . . ? C33 C32 C37 C46 -162.6(2) . . . . ? P3 C32 C37 C46 30.3(3) . . . . ? C34 C33 C38 C39 138.1(2) . . . . ? C32 C33 C38 C39 -41.7(3) . . . . ? C34 C33 C38 C41 -97.1(3) . . . . ? C32 C33 C38 C41 83.1(3) . . . . ? C34 C33 C38 C40 21.3(3) . . . . ? C32 C33 C38 C40 -158.5(2) . . . . ? C36 C35 C42 C45 103.9(3) . . . . ? C34 C35 C42 C45 -74.0(3) . . . . ? C36 C35 C42 C43 -16.9(4) . . . . ? C34 C35 C42 C43 165.2(2) . . . . ? C36 C35 C42 C44 -136.4(3) . . . . ? C34 C35 C42 C44 45.8(3) . . . . ? C36 C37 C46 C47 95.6(3) . . . . ? C32 C37 C46 C47 -84.4(3) . . . . ? C36 C37 C46 C48 -140.3(2) . . . . ? C32 C37 C46 C48 39.8(3) . . . . ? C36 C37 C46 C49 -23.6(3) . . . . ? C32 C37 C46 C49 156.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.372 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.064