# Supplementary Material (ESI) for Chemical Science # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Chemical Science' _journal_coden_Cambridge 1475 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Daniel Mindiola' _publ_contact_author_email mindiola@indiana.edu _publ_section_title ; Intermolecular C\^aH bond activation of benzene and pyridines by a vanadium(III) alkylidene including a stepwise conversion of benzene to a vanadium-benzyne complex ; loop_ _publ_author_name 'Daniel Mindiola' 'Jose Andino' 'Uriah Kilgore' 'Joshua Telser' 'Maren Pink' 'Jerzy Krzystek' ; A.Ozarowski ; 'Mu-Hyun Baik.' # Attachment '- 6.cif' data_08051 _database_code_depnum_ccdc_archive 'CCDC 730602' #TrackingRef '- 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H59 N2 P2 V, 0.5 (C5 H12)' _chemical_formula_sum 'C44.50 H65 N2 P2 V' _chemical_formula_weight 740.87 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)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 14.3987(7) _cell_length_b 10.4231(5) _cell_length_c 28.2627(15) _cell_angle_alpha 90.00 _cell_angle_beta 98.2770(10) _cell_angle_gamma 90.00 _cell_volume 4197.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9848 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 0.344 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9038 _exptl_absorpt_correction_T_max 0.9220 _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 2 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 35505 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 27.52 _reflns_number_total 9637 _reflns_number_gt 8327 _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^)+(0.0449P)^2^+1.7493P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9637 _refine_ls_number_parameters 472 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0906 _refine_ls_wR_factor_gt 0.0861 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.234989(15) 0.83554(2) 0.117362(8) 0.01526(6) Uani 1 1 d . . . P1 P 0.38425(2) 0.95479(3) 0.149035(13) 0.01819(8) Uani 1 1 d . . . P2 P 0.13156(2) 0.63307(3) 0.106050(12) 0.01615(8) Uani 1 1 d . . . N1 N 0.32158(8) 0.69268(11) 0.14649(4) 0.0167(2) Uani 1 1 d . . . N2 N 0.15853(8) 0.90813(11) 0.17243(4) 0.0197(2) Uani 1 1 d . . . C1 C 0.42573(11) 1.09438(14) 0.11672(6) 0.0268(3) Uani 1 1 d . . . H1 H 0.4416 1.0609 0.0857 0.032 Uiso 1 1 calc R . . C2 C 0.34469(13) 1.19040(16) 0.10430(7) 0.0378(4) Uani 1 1 d . . . H2A H 0.3626 1.2552 0.0821 0.057 Uiso 1 1 calc R . . H2B H 0.3313 1.2325 0.1336 0.057 Uiso 1 1 calc R . . H2C H 0.2886 1.1447 0.0893 0.057 Uiso 1 1 calc R . . C3 C 0.51318(13) 1.16478(16) 0.14127(7) 0.0378(4) Uani 1 1 d . . . H3A H 0.5330 1.2286 0.1193 0.057 Uiso 1 1 calc R . . H3B H 0.5639 1.1028 0.1501 0.057 Uiso 1 1 calc R . . H3C H 0.4984 1.2078 0.1701 0.057 Uiso 1 1 calc R . . C4 C 0.41889(10) 0.99270(14) 0.21328(5) 0.0242(3) Uani 1 1 d . . . H4 H 0.4852 1.0241 0.2174 0.029 Uiso 1 1 calc R . . C5 C 0.35819(13) 1.10013(16) 0.22928(6) 0.0344(4) Uani 1 1 d . . . H5A H 0.3784 1.1188 0.2632 0.052 Uiso 1 1 calc R . . H5B H 0.2923 1.0731 0.2246 0.052 Uiso 1 1 calc R . . H5C H 0.3650 1.1774 0.2103 0.052 Uiso 1 1 calc R . . C6 C 0.41593(12) 0.87378(16) 0.24478(5) 0.0308(3) Uani 1 1 d . . . H6A H 0.4339 0.8976 0.2784 0.046 Uiso 1 1 calc R . . H6B H 0.4598 0.8092 0.2359 0.046 Uiso 1 1 calc R . . H6C H 0.3522 0.8384 0.2403 0.046 Uiso 1 1 calc R . . C7 C 0.46011(9) 0.81989(13) 0.13967(5) 0.0195(3) Uani 1 1 d . . . C8 C 0.55281(10) 0.82772(15) 0.13061(5) 0.0249(3) Uani 1 1 d . . . H8 H 0.5804 0.9099 0.1284 0.030 Uiso 1 1 calc R . . C9 C 0.60589(10) 0.71905(16) 0.12474(6) 0.0281(3) Uani 1 1 d . . . C10 C 0.70465(12) 0.7299(2) 0.11291(7) 0.0415(4) Uani 1 1 d . . . H10A H 0.7276 0.8176 0.1191 0.062 Uiso 1 1 calc R . . H10B H 0.7048 0.7091 0.0791 0.062 Uiso 1 1 calc R . . H10C H 0.7456 0.6699 0.1328 0.062 Uiso 1 1 calc R . . C11 C 0.56427(11) 0.59993(15) 0.12888(6) 0.0271(3) Uani 1 1 d . . . H11 H 0.5998 0.5244 0.1259 0.032 Uiso 1 1 calc R . . C12 C 0.47233(10) 0.58894(14) 0.13726(5) 0.0230(3) Uani 1 1 d . . . H12 H 0.4457 0.5062 0.1395 0.028 Uiso 1 1 calc R . . C13 C 0.41756(9) 0.69856(13) 0.14252(5) 0.0183(3) Uani 1 1 d . . . C14 C 0.28719(9) 0.59117(12) 0.17142(5) 0.0176(3) Uani 1 1 d . . . C15 C 0.34019(10) 0.53076(13) 0.21099(5) 0.0219(3) Uani 1 1 d . . . H15 H 0.4049 0.5507 0.2191 0.026 Uiso 1 1 calc R . . C16 C 0.29897(11) 0.44267(14) 0.23819(5) 0.0241(3) Uani 1 1 d . . . H16 H 0.3362 0.4033 0.2647 0.029 Uiso 1 1 calc R . . C17 C 0.20438(11) 0.41027(13) 0.22761(5) 0.0236(3) Uani 1 1 d . . . C18 C 0.15928(13) 0.32087(16) 0.25957(6) 0.0341(4) Uani 1 1 d . . . H18A H 0.0969 0.2961 0.2436 0.051 Uiso 1 1 calc R . . H18B H 0.1534 0.3644 0.2897 0.051 Uiso 1 1 calc R . . H18C H 0.1983 0.2440 0.2661 0.051 Uiso 1 1 calc R . . C19 C 0.15274(10) 0.46574(13) 0.18750(5) 0.0213(3) Uani 1 1 d . . . H19 H 0.0887 0.4427 0.1790 0.026 Uiso 1 1 calc R . . C20 C 0.19249(9) 0.55463(12) 0.15924(5) 0.0173(3) Uani 1 1 d . . . C21 C 0.14369(10) 0.51183(13) 0.05880(5) 0.0214(3) Uani 1 1 d . . . H21 H 0.1074 0.5440 0.0283 0.026 Uiso 1 1 calc R . . C22 C 0.24607(11) 0.49980(15) 0.05100(6) 0.0283(3) Uani 1 1 d . . . H22A H 0.2507 0.4393 0.0249 0.042 Uiso 1 1 calc R . . H22B H 0.2837 0.4684 0.0804 0.042 Uiso 1 1 calc R . . H22C H 0.2695 0.5839 0.0427 0.042 Uiso 1 1 calc R . . C23 C 0.10407(12) 0.37977(14) 0.06885(6) 0.0287(3) Uani 1 1 d . . . H23A H 0.1128 0.3208 0.0429 0.043 Uiso 1 1 calc R . . H23B H 0.0370 0.3876 0.0710 0.043 Uiso 1 1 calc R . . H23C H 0.1370 0.3465 0.0991 0.043 Uiso 1 1 calc R . . C24 C 0.00510(9) 0.62354(14) 0.11153(5) 0.0211(3) Uani 1 1 d . . . H24 H -0.0094 0.5336 0.1203 0.025 Uiso 1 1 calc R . . C25 C -0.05426(11) 0.65545(18) 0.06361(6) 0.0333(4) Uani 1 1 d . . . H25A H -0.1209 0.6532 0.0672 0.050 Uiso 1 1 calc R . . H25B H -0.0420 0.5923 0.0396 0.050 Uiso 1 1 calc R . . H25C H -0.0379 0.7413 0.0533 0.050 Uiso 1 1 calc R . . C26 C -0.02014(10) 0.71308(15) 0.15039(6) 0.0259(3) Uani 1 1 d . . . H26A H -0.0860 0.7003 0.1543 0.039 Uiso 1 1 calc R . . H26B H -0.0106 0.8023 0.1412 0.039 Uiso 1 1 calc R . . H26C H 0.0200 0.6942 0.1806 0.039 Uiso 1 1 calc R . . C27 C 0.26400(10) 0.87839(14) 0.04767(5) 0.0223(3) Uani 1 1 d . . . H27A H 0.3061 0.9538 0.0524 0.027 Uiso 1 1 calc R . . H27B H 0.3042 0.8064 0.0401 0.027 Uiso 1 1 calc R . . C28 C 0.20066(11) 0.90616(14) -0.00022(5) 0.0266(3) Uani 1 1 d . . . C29 C 0.1362(2) 1.0179(2) 0.00499(7) 0.0698(8) Uani 1 1 d . . . H29A H 0.0989 1.0368 -0.0260 0.105 Uiso 1 1 calc R . . H29B H 0.1737 1.0933 0.0162 0.105 Uiso 1 1 calc R . . H29C H 0.0943 0.9961 0.0282 0.105 Uiso 1 1 calc R . . C30 C 0.14260(15) 0.7893(2) -0.01826(7) 0.0477(5) Uani 1 1 d . . . H30A H 0.1061 0.8087 -0.0494 0.072 Uiso 1 1 calc R . . H30B H 0.0999 0.7673 0.0045 0.072 Uiso 1 1 calc R . . H30C H 0.1845 0.7167 -0.0215 0.072 Uiso 1 1 calc R . . C31 C 0.13545(10) 0.96610(13) 0.12955(5) 0.0209(3) Uani 1 1 d . . . C33 C 0.06705(11) 1.06237(14) 0.12392(6) 0.0280(3) Uani 1 1 d . . . H33 H 0.0518 1.1054 0.0942 0.034 Uiso 1 1 calc R . . C32 C 0.26181(15) 0.9404(2) -0.03868(6) 0.0475(5) Uani 1 1 d . . . H32A H 0.2215 0.9584 -0.0689 0.071 Uiso 1 1 calc R . . H32B H 0.3034 0.8683 -0.0430 0.071 Uiso 1 1 calc R . . H32C H 0.2996 1.0165 -0.0286 0.071 Uiso 1 1 calc R . . C34 C 0.02197(11) 1.09392(15) 0.16233(6) 0.0328(4) Uani 1 1 d . . . H34 H -0.0260 1.1572 0.1589 0.039 Uiso 1 1 calc R . . C35 C 0.04693(11) 1.03296(15) 0.20595(6) 0.0298(3) Uani 1 1 d . . . H35 H 0.0157 1.0540 0.2323 0.036 Uiso 1 1 calc R . . C36 C 0.11791(10) 0.94071(14) 0.21101(5) 0.0230(3) Uani 1 1 d . . . C37 C 0.15006(10) 0.87915(15) 0.25780(5) 0.0240(3) Uani 1 1 d . . . C38 C 0.14815(13) 0.94839(16) 0.29995(6) 0.0343(4) Uani 1 1 d . . . H38 H 0.1247 1.0337 0.2984 0.041 Uiso 1 1 calc R . . C39 C 0.17995(14) 0.89416(17) 0.34402(6) 0.0380(4) Uani 1 1 d . . . H39 H 0.1783 0.9425 0.3724 0.046 Uiso 1 1 calc R . . C40 C 0.21405(12) 0.77004(17) 0.34701(6) 0.0347(4) Uani 1 1 d . . . H40 H 0.2364 0.7332 0.3773 0.042 Uiso 1 1 calc R . . C41 C 0.21541(12) 0.69995(17) 0.30562(6) 0.0327(4) Uani 1 1 d . . . H41 H 0.2381 0.6143 0.3075 0.039 Uiso 1 1 calc R . . C42 C 0.18375(11) 0.75406(15) 0.26131(6) 0.0281(3) Uani 1 1 d . . . H42 H 0.1852 0.7050 0.2331 0.034 Uiso 1 1 calc R . . C1S C 0.4864(3) 0.2048(5) -0.00052(16) 0.0531(11) Uani 0.50 1 d PD A -1 H1S1 H 0.4696 0.1993 0.0318 0.080 Uiso 0.50 1 calc PR A -1 H1S2 H 0.5258 0.1313 -0.0062 0.080 Uiso 0.50 1 calc PR A -1 H1S3 H 0.4292 0.2041 -0.0240 0.080 Uiso 0.50 1 calc PR A -1 C2S C 0.5397(16) 0.327(2) -0.0055(9) 0.052(2) Uani 0.50 1 d PD A -1 H2S1 H 0.5565 0.3326 -0.0382 0.062 Uiso 0.50 1 calc PR A -1 H2S2 H 0.5987 0.3262 0.0174 0.062 Uiso 0.50 1 calc PR A -1 C3S C 0.4829(16) 0.444(2) 0.0039(14) 0.046(2) Uani 0.50 1 d PD A -1 H3S1 H 0.4227 0.4427 -0.0180 0.056 Uiso 0.50 1 calc PR A -1 H3S2 H 0.4686 0.4404 0.0371 0.056 Uiso 0.50 1 calc PR A -1 C4S C 0.5339(16) 0.566(2) -0.0032(14) 0.046(2) Uani 0.50 1 d PD A -1 H4S1 H 0.5571 0.5625 -0.0345 0.056 Uiso 0.50 1 calc PR A -1 H4S2 H 0.5892 0.5726 0.0219 0.056 Uiso 0.50 1 calc PR A -1 C5S C 0.4746(16) 0.686(2) -0.0016(9) 0.052(2) Uani 0.50 1 d PD A -1 H5S1 H 0.4192 0.6808 -0.0261 0.078 Uiso 0.50 1 calc PR A -1 H5S2 H 0.5117 0.7619 -0.0077 0.078 Uiso 0.50 1 calc PR A -1 H5S3 H 0.4547 0.6942 0.0300 0.078 Uiso 0.50 1 calc PR A -1 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 0.01450(11) 0.01392(11) 0.01673(11) 0.00062(8) 0.00003(8) 0.00202(8) P1 0.01662(16) 0.01567(16) 0.02118(17) -0.00009(13) -0.00103(13) -0.00013(13) P2 0.01559(16) 0.01511(16) 0.01718(16) -0.00018(12) 0.00045(12) 0.00009(12) N1 0.0153(5) 0.0153(5) 0.0189(5) 0.0008(4) 0.0005(4) 0.0009(4) N2 0.0182(5) 0.0171(5) 0.0239(6) -0.0033(5) 0.0032(4) -0.0006(4) C1 0.0274(8) 0.0203(7) 0.0314(8) 0.0041(6) -0.0001(6) -0.0043(6) C2 0.0412(10) 0.0202(8) 0.0496(11) 0.0075(7) -0.0016(8) 0.0016(7) C3 0.0344(9) 0.0277(8) 0.0496(11) 0.0020(7) 0.0006(8) -0.0132(7) C4 0.0232(7) 0.0245(7) 0.0231(7) -0.0039(6) -0.0031(6) -0.0013(6) C5 0.0391(9) 0.0299(8) 0.0331(8) -0.0108(7) 0.0015(7) 0.0030(7) C6 0.0386(9) 0.0306(8) 0.0218(7) 0.0003(6) -0.0006(6) 0.0002(7) C7 0.0172(6) 0.0209(7) 0.0195(6) 0.0005(5) -0.0008(5) 0.0014(5) C8 0.0195(7) 0.0266(7) 0.0279(7) 0.0016(6) 0.0013(6) -0.0022(6) C9 0.0165(7) 0.0368(8) 0.0307(8) 0.0010(7) 0.0026(6) 0.0044(6) C10 0.0202(8) 0.0487(11) 0.0572(12) 0.0013(9) 0.0113(8) 0.0044(7) C11 0.0224(7) 0.0283(8) 0.0303(8) 0.0006(6) 0.0032(6) 0.0090(6) C12 0.0228(7) 0.0203(7) 0.0254(7) 0.0016(5) 0.0021(6) 0.0042(6) C13 0.0165(6) 0.0206(6) 0.0167(6) 0.0017(5) -0.0009(5) 0.0020(5) C14 0.0204(6) 0.0144(6) 0.0177(6) -0.0006(5) 0.0023(5) 0.0026(5) C15 0.0218(7) 0.0207(7) 0.0222(7) 0.0018(5) -0.0007(5) 0.0032(5) C16 0.0313(8) 0.0200(7) 0.0200(7) 0.0035(5) 0.0002(6) 0.0053(6) C17 0.0327(8) 0.0176(6) 0.0211(7) 0.0020(5) 0.0064(6) -0.0001(6) C18 0.0443(10) 0.0292(8) 0.0295(8) 0.0094(7) 0.0076(7) -0.0056(7) C19 0.0236(7) 0.0189(6) 0.0216(7) -0.0011(5) 0.0042(5) -0.0018(5) C20 0.0198(6) 0.0150(6) 0.0169(6) -0.0008(5) 0.0019(5) 0.0015(5) C21 0.0272(7) 0.0172(6) 0.0192(6) -0.0024(5) 0.0011(5) 0.0005(5) C22 0.0318(8) 0.0241(7) 0.0301(8) -0.0053(6) 0.0083(6) 0.0042(6) C23 0.0378(9) 0.0192(7) 0.0285(8) -0.0042(6) 0.0031(6) -0.0043(6) C24 0.0163(6) 0.0216(7) 0.0249(7) 0.0003(5) 0.0011(5) -0.0021(5) C25 0.0213(7) 0.0471(10) 0.0295(8) 0.0000(7) -0.0027(6) 0.0038(7) C26 0.0189(7) 0.0287(8) 0.0310(8) -0.0027(6) 0.0064(6) -0.0011(6) C27 0.0238(7) 0.0218(7) 0.0205(7) 0.0013(5) 0.0007(5) -0.0012(6) C28 0.0335(8) 0.0231(7) 0.0216(7) 0.0042(6) -0.0014(6) 0.0023(6) C29 0.0996(19) 0.0720(15) 0.0319(10) 0.0008(10) -0.0114(11) 0.0596(15) C30 0.0494(11) 0.0500(11) 0.0368(10) 0.0146(8) -0.0173(8) -0.0171(9) C31 0.0189(6) 0.0173(6) 0.0262(7) -0.0008(5) 0.0021(5) -0.0006(5) C33 0.0255(7) 0.0229(7) 0.0351(8) 0.0025(6) 0.0028(6) 0.0049(6) C32 0.0580(12) 0.0610(13) 0.0220(8) 0.0072(8) 0.0004(8) -0.0151(10) C34 0.0266(8) 0.0257(8) 0.0464(10) -0.0021(7) 0.0062(7) 0.0099(6) C35 0.0272(8) 0.0278(8) 0.0364(9) -0.0083(6) 0.0112(7) 0.0026(6) C36 0.0213(7) 0.0205(7) 0.0279(7) -0.0059(6) 0.0057(6) -0.0025(5) C37 0.0218(7) 0.0264(7) 0.0250(7) -0.0049(6) 0.0071(6) -0.0036(6) C38 0.0468(10) 0.0267(8) 0.0308(8) -0.0075(7) 0.0108(7) -0.0006(7) C39 0.0514(11) 0.0375(9) 0.0266(8) -0.0097(7) 0.0102(7) -0.0058(8) C40 0.0373(9) 0.0415(9) 0.0256(8) 0.0011(7) 0.0060(7) -0.0050(8) C41 0.0363(9) 0.0314(8) 0.0309(8) -0.0010(7) 0.0064(7) 0.0040(7) C42 0.0303(8) 0.0289(8) 0.0256(7) -0.0058(6) 0.0055(6) 0.0012(6) C1S 0.058(3) 0.066(3) 0.039(2) 0.010(2) 0.0172(19) -0.007(2) C2S 0.048(6) 0.058(5) 0.052(6) 0.001(4) 0.017(3) 0.012(3) C3S 0.030(7) 0.063(3) 0.0461(13) -0.010(3) 0.005(5) 0.010(3) C4S 0.030(7) 0.063(3) 0.0461(13) -0.010(3) 0.005(5) 0.010(3) C5S 0.048(6) 0.058(5) 0.052(6) 0.001(4) 0.017(3) 0.012(3) _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 N1 2.0381(11) . ? V1 C31 2.0414(14) . ? V1 C27 2.1191(14) . ? V1 N2 2.1680(12) . ? V1 P1 2.5320(4) . ? V1 P2 2.5762(4) . ? P1 C7 1.8230(14) . ? P1 C4 1.8549(15) . ? P1 C1 1.8615(15) . ? P2 C20 1.8216(13) . ? P2 C24 1.8521(14) . ? P2 C21 1.8648(14) . ? N1 C14 1.4005(17) . ? N1 C13 1.4038(17) . ? N2 C31 1.3521(18) . ? N2 C36 1.3526(18) . ? C1 C3 1.534(2) . ? C1 C2 1.539(2) . ? 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 C5 1.528(2) . ? C4 C6 1.530(2) . ? 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 1.397(2) . ? C7 C13 1.4126(19) . ? C8 C9 1.390(2) . ? C8 H8 0.9500 . ? C9 C11 1.391(2) . ? C9 C10 1.511(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.383(2) . ? C11 H11 0.9500 . ? C12 C13 1.4084(19) . ? C12 H12 0.9500 . ? C14 C15 1.4086(18) . ? C14 C20 1.4099(19) . ? C15 C16 1.385(2) . ? C15 H15 0.9500 . ? C16 C17 1.393(2) . ? C16 H16 0.9500 . ? C17 C19 1.389(2) . ? C17 C18 1.508(2) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.3984(19) . ? C19 H19 0.9500 . ? C21 C22 1.527(2) . ? C21 C23 1.532(2) . ? 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 1.525(2) . ? C24 C25 1.530(2) . ? 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 1.5466(19) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.509(2) . ? C28 C30 1.523(2) . ? C28 C32 1.536(2) . ? 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 C33 1.399(2) . ? C33 C34 1.382(2) . ? C33 H33 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C34 C35 1.387(2) . ? C34 H34 0.9500 . ? C35 C36 1.396(2) . ? C35 H35 0.9500 . ? C36 C37 1.483(2) . ? C37 C42 1.390(2) . ? C37 C38 1.396(2) . ? C38 C39 1.384(2) . ? C38 H38 0.9500 . ? C39 C40 1.382(3) . ? C39 H39 0.9500 . ? C40 C41 1.382(2) . ? C40 H40 0.9500 . ? C41 C42 1.389(2) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C1S C2S 1.506(19) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S C3S 1.508(17) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S C4S 1.499(5) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S C5S 1.521(17) . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? C5S H5S1 0.9800 . ? C5S H5S2 0.9800 . ? C5S H5S3 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 N1 V1 C31 145.33(5) . . ? N1 V1 C27 109.79(5) . . ? C31 V1 C27 104.68(6) . . ? N1 V1 N2 108.02(5) . . ? C31 V1 N2 37.32(5) . . ? C27 V1 N2 141.45(5) . . ? N1 V1 P1 77.12(3) . . ? C31 V1 P1 101.18(4) . . ? C27 V1 P1 87.38(4) . . ? N2 V1 P1 93.89(3) . . ? N1 V1 P2 76.16(3) . . ? C31 V1 P2 99.19(4) . . ? C27 V1 P2 104.19(4) . . ? N2 V1 P2 91.76(3) . . ? P1 V1 P2 153.139(14) . . ? C7 P1 C4 102.95(6) . . ? C7 P1 C1 106.88(7) . . ? C4 P1 C1 104.70(7) . . ? C7 P1 V1 93.78(5) . . ? C4 P1 V1 123.06(5) . . ? C1 P1 V1 121.75(5) . . ? C20 P2 C24 105.63(6) . . ? C20 P2 C21 101.72(6) . . ? C24 P2 C21 102.59(6) . . ? C20 P2 V1 93.67(4) . . ? C24 P2 V1 126.25(5) . . ? C21 P2 V1 122.13(5) . . ? C14 N1 C13 119.78(11) . . ? C14 N1 V1 121.00(9) . . ? C13 N1 V1 119.20(9) . . ? C31 N2 C36 122.09(12) . . ? C31 N2 V1 66.25(8) . . ? C36 N2 V1 171.66(10) . . ? C3 C1 C2 109.76(13) . . ? C3 C1 P1 116.89(11) . . ? C2 C1 P1 109.51(11) . . ? C3 C1 H1 106.7 . . ? C2 C1 H1 106.7 . . ? P1 C1 H1 106.7 . . ? 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 . . ? C5 C4 C6 110.87(13) . . ? C5 C4 P1 111.17(10) . . ? C6 C4 P1 111.77(10) . . ? C5 C4 H4 107.6 . . ? C6 C4 H4 107.6 . . ? P1 C4 H4 107.6 . . ? 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 119.76(13) . . ? C8 C7 P1 126.14(11) . . ? C13 C7 P1 114.10(10) . . ? C9 C8 C7 122.05(14) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? C8 C9 C11 117.80(14) . . ? C8 C9 C10 121.13(15) . . ? C11 C9 C10 121.05(15) . . ? 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 121.54(14) . . ? C12 C11 H11 119.2 . . ? C9 C11 H11 119.2 . . ? C11 C12 C13 121.02(14) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? N1 C13 C12 123.07(12) . . ? N1 C13 C7 118.93(12) . . ? C12 C13 C7 117.79(12) . . ? N1 C14 C15 123.14(12) . . ? N1 C14 C20 118.74(12) . . ? C15 C14 C20 117.87(12) . . ? C16 C15 C14 120.71(13) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 121.70(13) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C19 C17 C16 117.78(13) . . ? C19 C17 C18 121.32(14) . . ? C16 C17 C18 120.88(14) . . ? 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 . . ? C17 C19 C20 121.80(13) . . ? C17 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C19 C20 C14 120.03(12) . . ? C19 C20 P2 125.50(11) . . ? C14 C20 P2 114.47(10) . . ? C22 C21 C23 110.24(12) . . ? C22 C21 P2 110.55(10) . . ? C23 C21 P2 113.60(10) . . ? C22 C21 H21 107.4 . . ? C23 C21 H21 107.4 . . ? P2 C21 H21 107.4 . . ? 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 110.11(12) . . ? C26 C24 P2 111.50(10) . . ? C25 C24 P2 110.18(10) . . ? C26 C24 H24 108.3 . . ? C25 C24 H24 108.3 . . ? P2 C24 H24 108.3 . . ? 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 133.05(11) . . ? C28 C27 H27A 104.0 . . ? V1 C27 H27A 104.0 . . ? C28 C27 H27B 104.0 . . ? V1 C27 H27B 104.0 . . ? H27A C27 H27B 105.4 . . ? C29 C28 C30 109.53(18) . . ? C29 C28 C32 108.22(17) . . ? C30 C28 C32 106.98(15) . . ? C29 C28 C27 110.62(13) . . ? C30 C28 C27 111.67(12) . . ? C32 C28 C27 109.69(14) . . ? 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 . . ? N2 C31 C33 120.05(13) . . ? N2 C31 V1 76.43(8) . . ? C33 C31 V1 163.51(12) . . ? C34 C33 C31 118.93(15) . . ? C34 C33 H33 120.5 . . ? C31 C33 H33 120.5 . . ? C28 C32 H32A 109.5 . . ? C28 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C28 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C33 C34 C35 119.87(14) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C34 C35 C36 119.92(14) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? N2 C36 C35 119.05(14) . . ? N2 C36 C37 119.65(13) . . ? C35 C36 C37 121.30(13) . . ? C42 C37 C38 118.27(15) . . ? C42 C37 C36 122.04(13) . . ? C38 C37 C36 119.69(14) . . ? C39 C38 C37 120.79(16) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C40 C39 C38 120.38(15) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C41 C40 C39 119.44(16) . . ? C41 C40 H40 120.3 . . ? C39 C40 H40 120.3 . . ? C40 C41 C42 120.38(16) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C41 C42 C37 120.73(14) . . ? C41 C42 H42 119.6 . . ? C37 C42 H42 119.6 . . ? C1S C2S C3S 111.7(14) . . ? C1S C2S H2S1 109.3 . . ? C3S C2S H2S1 109.3 . . ? C1S C2S H2S2 109.3 . . ? C3S C2S H2S2 109.3 . . ? H2S1 C2S H2S2 107.9 . . ? C4S C3S C2S 111.9(11) . . ? C4S C3S H3S1 109.2 . . ? C2S C3S H3S1 109.2 . . ? C4S C3S H3S2 109.2 . . ? C2S C3S H3S2 109.2 . . ? H3S1 C3S H3S2 107.9 . . ? C3S C4S C5S 114.2(11) . . ? C3S C4S H4S1 108.7 . . ? C5S C4S H4S1 108.7 . . ? C3S C4S H4S2 108.7 . . ? C5S C4S H4S2 108.7 . . ? H4S1 C4S H4S2 107.6 . . ? 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 V1 P1 C7 30.90(6) . . . . ? C31 V1 P1 C7 175.47(6) . . . . ? C27 V1 P1 C7 -80.08(6) . . . . ? N2 V1 P1 C7 138.51(5) . . . . ? P2 V1 P1 C7 36.84(6) . . . . ? N1 V1 P1 C4 -77.22(7) . . . . ? C31 V1 P1 C4 67.35(7) . . . . ? C27 V1 P1 C4 171.80(7) . . . . ? N2 V1 P1 C4 30.39(7) . . . . ? P2 V1 P1 C4 -71.28(7) . . . . ? N1 V1 P1 C1 143.42(7) . . . . ? C31 V1 P1 C1 -72.01(8) . . . . ? C27 V1 P1 C1 32.44(7) . . . . ? N2 V1 P1 C1 -108.97(7) . . . . ? P2 V1 P1 C1 149.36(7) . . . . ? N1 V1 P2 C20 29.92(5) . . . . ? C31 V1 P2 C20 -114.99(6) . . . . ? C27 V1 P2 C20 137.21(6) . . . . ? N2 V1 P2 C20 -78.21(5) . . . . ? P1 V1 P2 C20 23.96(6) . . . . ? N1 V1 P2 C24 142.37(7) . . . . ? C31 V1 P2 C24 -2.53(7) . . . . ? C27 V1 P2 C24 -110.34(7) . . . . ? N2 V1 P2 C24 34.24(7) . . . . ? P1 V1 P2 C24 136.41(6) . . . . ? N1 V1 P2 C21 -76.39(6) . . . . ? C31 V1 P2 C21 138.71(7) . . . . ? C27 V1 P2 C21 30.91(7) . . . . ? N2 V1 P2 C21 175.48(6) . . . . ? P1 V1 P2 C21 -82.35(6) . . . . ? C31 V1 N1 C14 50.13(14) . . . . ? C27 V1 N1 C14 -136.37(10) . . . . ? N2 V1 N1 C14 51.30(11) . . . . ? P1 V1 N1 C14 141.23(10) . . . . ? P2 V1 N1 C14 -36.02(9) . . . . ? C31 V1 N1 C13 -128.09(11) . . . . ? C27 V1 N1 C13 45.40(11) . . . . ? N2 V1 N1 C13 -126.93(10) . . . . ? P1 V1 N1 C13 -37.00(9) . . . . ? P2 V1 N1 C13 145.75(10) . . . . ? N1 V1 N2 C31 -178.91(8) . . . . ? C27 V1 N2 C31 12.71(12) . . . . ? P1 V1 N2 C31 103.38(8) . . . . ? P2 V1 N2 C31 -102.89(8) . . . . ? N1 V1 N2 C36 0.4(7) . . . . ? C31 V1 N2 C36 179(100) . . . . ? C27 V1 N2 C36 -168.0(7) . . . . ? P1 V1 N2 C36 -77.3(7) . . . . ? P2 V1 N2 C36 76.4(7) . . . . ? C7 P1 C1 C3 -78.74(14) . . . . ? C4 P1 C1 C3 30.03(14) . . . . ? V1 P1 C1 C3 175.67(11) . . . . ? C7 P1 C1 C2 155.69(11) . . . . ? C4 P1 C1 C2 -95.55(12) . . . . ? V1 P1 C1 C2 50.10(13) . . . . ? C7 P1 C4 C5 -176.58(11) . . . . ? C1 P1 C4 C5 71.81(12) . . . . ? V1 P1 C4 C5 -73.26(12) . . . . ? C7 P1 C4 C6 -52.10(12) . . . . ? C1 P1 C4 C6 -163.71(11) . . . . ? V1 P1 C4 C6 51.21(13) . . . . ? C4 P1 C7 C8 -83.10(14) . . . . ? C1 P1 C7 C8 26.89(15) . . . . ? V1 P1 C7 C8 151.72(12) . . . . ? C4 P1 C7 C13 96.53(11) . . . . ? C1 P1 C7 C13 -153.48(10) . . . . ? V1 P1 C7 C13 -28.65(10) . . . . ? C13 C7 C8 C9 -0.7(2) . . . . ? P1 C7 C8 C9 178.86(12) . . . . ? C7 C8 C9 C11 -1.0(2) . . . . ? C7 C8 C9 C10 177.39(15) . . . . ? C8 C9 C11 C12 1.7(2) . . . . ? C10 C9 C11 C12 -176.63(15) . . . . ? C9 C11 C12 C13 -0.8(2) . . . . ? C14 N1 C13 C12 36.20(19) . . . . ? V1 N1 C13 C12 -145.55(11) . . . . ? C14 N1 C13 C7 -149.19(13) . . . . ? V1 N1 C13 C7 29.06(16) . . . . ? C11 C12 C13 N1 173.72(13) . . . . ? C11 C12 C13 C7 -1.0(2) . . . . ? C8 C7 C13 N1 -173.22(13) . . . . ? P1 C7 C13 N1 7.13(16) . . . . ? C8 C7 C13 C12 1.7(2) . . . . ? P1 C7 C13 C12 -177.97(10) . . . . ? C13 N1 C14 C15 32.12(19) . . . . ? V1 N1 C14 C15 -146.10(11) . . . . ? C13 N1 C14 C20 -153.67(12) . . . . ? V1 N1 C14 C20 28.11(16) . . . . ? N1 C14 C15 C16 171.40(13) . . . . ? C20 C14 C15 C16 -2.9(2) . . . . ? C14 C15 C16 C17 0.1(2) . . . . ? C15 C16 C17 C19 2.4(2) . . . . ? C15 C16 C17 C18 -175.87(14) . . . . ? C16 C17 C19 C20 -2.1(2) . . . . ? C18 C17 C19 C20 176.12(14) . . . . ? C17 C19 C20 C14 -0.6(2) . . . . ? C17 C19 C20 P2 179.98(11) . . . . ? N1 C14 C20 C19 -171.43(12) . . . . ? C15 C14 C20 C19 3.10(19) . . . . ? N1 C14 C20 P2 8.04(16) . . . . ? C15 C14 C20 P2 -177.44(10) . . . . ? C24 P2 C20 C19 21.83(14) . . . . ? C21 P2 C20 C19 -84.98(13) . . . . ? V1 P2 C20 C19 151.12(12) . . . . ? C24 P2 C20 C14 -157.60(10) . . . . ? C21 P2 C20 C14 95.58(11) . . . . ? V1 P2 C20 C14 -28.31(10) . . . . ? C20 P2 C21 C22 -67.61(11) . . . . ? C24 P2 C21 C22 -176.78(10) . . . . ? V1 P2 C21 C22 34.38(12) . . . . ? C20 P2 C21 C23 56.93(12) . . . . ? C24 P2 C21 C23 -52.24(12) . . . . ? V1 P2 C21 C23 158.92(9) . . . . ? C20 P2 C24 C26 71.64(11) . . . . ? C21 P2 C24 C26 177.82(10) . . . . ? V1 P2 C24 C26 -35.08(12) . . . . ? C20 P2 C24 C25 -165.78(10) . . . . ? C21 P2 C24 C25 -59.59(12) . . . . ? V1 P2 C24 C25 87.51(11) . . . . ? N1 V1 C27 C28 137.69(13) . . . . ? C31 V1 C27 C28 -46.13(15) . . . . ? N2 V1 C27 C28 -54.05(17) . . . . ? P1 V1 C27 C28 -147.00(14) . . . . ? P2 V1 C27 C28 57.55(14) . . . . ? V1 C27 C28 C29 56.8(2) . . . . ? V1 C27 C28 C30 -65.5(2) . . . . ? V1 C27 C28 C32 176.08(13) . . . . ? C36 N2 C31 C33 -0.5(2) . . . . ? V1 N2 C31 C33 179.35(14) . . . . ? C36 N2 C31 V1 -179.89(12) . . . . ? N1 V1 C31 N2 1.82(13) . . . . ? C27 V1 C31 N2 -171.85(8) . . . . ? P1 V1 C31 N2 -81.65(7) . . . . ? P2 V1 C31 N2 80.75(7) . . . . ? N1 V1 C31 C33 -176.2(4) . . . . ? C27 V1 C31 C33 10.1(4) . . . . ? N2 V1 C31 C33 -178.0(4) . . . . ? P1 V1 C31 C33 100.3(4) . . . . ? P2 V1 C31 C33 -97.3(4) . . . . ? N2 C31 C33 C34 -1.9(2) . . . . ? V1 C31 C33 C34 175.8(3) . . . . ? C31 C33 C34 C35 1.9(2) . . . . ? C33 C34 C35 C36 0.5(2) . . . . ? C31 N2 C36 C35 3.0(2) . . . . ? V1 N2 C36 C35 -176.3(6) . . . . ? C31 N2 C36 C37 -176.41(13) . . . . ? V1 N2 C36 C37 4.3(8) . . . . ? C34 C35 C36 N2 -2.9(2) . . . . ? C34 C35 C36 C37 176.45(14) . . . . ? N2 C36 C37 C42 -31.6(2) . . . . ? C35 C36 C37 C42 149.04(15) . . . . ? N2 C36 C37 C38 147.43(15) . . . . ? C35 C36 C37 C38 -31.9(2) . . . . ? C42 C37 C38 C39 0.7(2) . . . . ? C36 C37 C38 C39 -178.39(15) . . . . ? C37 C38 C39 C40 -0.1(3) . . . . ? C38 C39 C40 C41 -0.6(3) . . . . ? C39 C40 C41 C42 0.7(3) . . . . ? C40 C41 C42 C37 -0.1(3) . . . . ? C38 C37 C42 C41 -0.5(2) . . . . ? C36 C37 C42 C41 178.50(15) . . . . ? C1S C2S C3S C4S -177.4(11) . . . . ? C2S C3S C4S C5S 171(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.459 _refine_diff_density_min -0.301 _refine_diff_density_rms 0.048 # Attachment '- 5.cif' data_08073 _database_code_depnum_ccdc_archive 'CCDC 730603' #TrackingRef '- 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C37 H57 N2 P2 V), C26 H41 N P2' _chemical_formula_sum 'C100 H155 N5 P6 V2' _chemical_formula_weight 1714.99 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 C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.471(6) _cell_length_b 10.7761(18) _cell_length_c 28.001(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.454(7) _cell_angle_gamma 90.00 _cell_volume 9753(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9931 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 26.3 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3704 _exptl_absorpt_coefficient_mu 0.336 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.9206 _exptl_absorpt_correction_T_max 0.9671 _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 20 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 65782 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.53 _reflns_number_total 11205 _reflns_number_gt 8444 _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^)+(0.0438P)^2^+7.0147P] 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 11205 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.343464(9) 0.24447(3) 0.109690(10) 0.01896(8) Uani 1 1 d . . . P1 P 0.372964(13) 0.29083(4) 0.030535(15) 0.01987(10) Uani 1 1 d . . . P2 P 0.308261(14) 0.10618(4) 0.167225(15) 0.02215(10) Uani 1 1 d . . . N1 N 0.33113(4) 0.08692(13) 0.07075(5) 0.0202(3) Uani 1 1 d . . . N2 N 0.40460(4) 0.21626(14) 0.14160(5) 0.0241(3) Uani 1 1 d . . . C1 C 0.33561(5) 0.33683(18) -0.02099(6) 0.0252(4) Uani 1 1 d . . . H1 H 0.3249 0.4210 -0.0136 0.030 Uiso 1 1 calc R . . C2 C 0.29871(6) 0.2494(2) -0.02641(7) 0.0318(4) Uani 1 1 d . . . H2A H 0.2775 0.2834 -0.0500 0.048 Uiso 1 1 calc R . . H2B H 0.2873 0.2404 0.0046 0.048 Uiso 1 1 calc R . . H2C H 0.3076 0.1681 -0.0373 0.048 Uiso 1 1 calc R . . C3 C 0.35424(6) 0.3463(2) -0.06877(7) 0.0356(5) Uani 1 1 d . . . H3A H 0.3326 0.3692 -0.0940 0.053 Uiso 1 1 calc R . . H3B H 0.3662 0.2660 -0.0765 0.053 Uiso 1 1 calc R . . H3C H 0.3760 0.4097 -0.0665 0.053 Uiso 1 1 calc R . . C4 C 0.42029(5) 0.37732(17) 0.01884(7) 0.0261(4) Uani 1 1 d . . . H4 H 0.4274 0.3538 -0.0139 0.031 Uiso 1 1 calc R . . C5 C 0.41257(7) 0.51751(18) 0.01895(8) 0.0379(5) Uani 1 1 d . . . H5A H 0.4368 0.5608 0.0087 0.057 Uiso 1 1 calc R . . H5B H 0.4078 0.5444 0.0514 0.057 Uiso 1 1 calc R . . H5C H 0.3882 0.5371 -0.0032 0.057 Uiso 1 1 calc R . . C6 C 0.45717(6) 0.34450(19) 0.05436(7) 0.0332(4) Uani 1 1 d . . . H6A H 0.4819 0.3868 0.0451 0.050 Uiso 1 1 calc R . . H6B H 0.4616 0.2546 0.0542 0.050 Uiso 1 1 calc R . . H6C H 0.4517 0.3710 0.0866 0.050 Uiso 1 1 calc R . . C7 C 0.38456(5) 0.12917(16) 0.01809(6) 0.0206(3) Uani 1 1 d . . . C8 C 0.41554(5) 0.08769(17) -0.00934(6) 0.0252(4) Uani 1 1 d . . . H8 H 0.4318 0.1471 -0.0241 0.030 Uiso 1 1 calc R . . C9 C 0.42329(6) -0.03793(18) -0.01573(7) 0.0280(4) Uani 1 1 d . . . C10 C 0.45748(6) -0.0807(2) -0.04484(8) 0.0400(5) Uani 1 1 d . . . H10A H 0.4489 -0.1566 -0.0623 0.060 Uiso 1 1 calc R . . H10B H 0.4825 -0.0973 -0.0234 0.060 Uiso 1 1 calc R . . H10C H 0.4633 -0.0158 -0.0678 0.060 Uiso 1 1 calc R . . C11 C 0.39837(6) -0.12194(18) 0.00587(7) 0.0301(4) Uani 1 1 d . . . H11 H 0.4028 -0.2083 0.0018 0.036 Uiso 1 1 calc R . . C12 C 0.36739(6) -0.08359(17) 0.03312(7) 0.0273(4) Uani 1 1 d . . . H12 H 0.3510 -0.1438 0.0473 0.033 Uiso 1 1 calc R . . C13 C 0.35986(5) 0.04283(16) 0.04017(6) 0.0204(3) Uani 1 1 d . . . C14 C 0.29561(5) 0.01571(16) 0.07624(6) 0.0207(3) Uani 1 1 d . . . C15 C 0.27408(5) -0.04913(17) 0.03830(6) 0.0256(4) Uani 1 1 d . . . H15 H 0.2847 -0.0507 0.0078 0.031 Uiso 1 1 calc R . . C16 C 0.23756(6) -0.11092(17) 0.04447(7) 0.0273(4) Uani 1 1 d . . . H16 H 0.2235 -0.1533 0.0180 0.033 Uiso 1 1 calc R . . C17 C 0.22093(5) -0.11253(17) 0.08836(7) 0.0264(4) Uani 1 1 d . . . C18 C 0.18090(6) -0.17921(19) 0.09443(8) 0.0353(5) Uani 1 1 d . . . H18A H 0.1777 -0.1888 0.1287 0.053 Uiso 1 1 calc R . . H18B H 0.1813 -0.2612 0.0794 0.053 Uiso 1 1 calc R . . H18C H 0.1577 -0.1309 0.0792 0.053 Uiso 1 1 calc R . . C19 C 0.24227(5) -0.04959(17) 0.12630(6) 0.0246(4) Uani 1 1 d . . . H19A H 0.2316 -0.0502 0.1567 0.030 Uiso 1 1 calc R . . C20 C 0.27904(5) 0.01478(16) 0.12105(6) 0.0217(4) Uani 1 1 d . . . C21 C 0.34301(6) -0.00759(18) 0.20082(7) 0.0298(4) Uani 1 1 d . . . H21 H 0.3633 0.0411 0.2225 0.036 Uiso 1 1 calc R . . C22 C 0.32177(7) -0.0985(2) 0.23222(8) 0.0433(5) Uani 1 1 d . . . H22A H 0.3422 -0.1572 0.2470 0.065 Uiso 1 1 calc R . . H22B H 0.3003 -0.1439 0.2125 0.065 Uiso 1 1 calc R . . H22C H 0.3092 -0.0527 0.2574 0.065 Uiso 1 1 calc R . . C23 C 0.36773(6) -0.0799(2) 0.16684(8) 0.0378(5) Uani 1 1 d . . . H23A H 0.3899 -0.1256 0.1853 0.057 Uiso 1 1 calc R . . H23B H 0.3797 -0.0223 0.1449 0.057 Uiso 1 1 calc R . . H23C H 0.3495 -0.1385 0.1483 0.057 Uiso 1 1 calc R . . C24 C 0.27059(6) 0.1447(2) 0.21073(6) 0.0315(4) Uani 1 1 d . . . H24 H 0.2600 0.0646 0.2228 0.038 Uiso 1 1 calc R . . C25 C 0.23337(6) 0.2177(2) 0.18851(8) 0.0403(5) Uani 1 1 d . . . H25A H 0.2122 0.2212 0.2112 0.061 Uiso 1 1 calc R . . H25B H 0.2220 0.1768 0.1589 0.061 Uiso 1 1 calc R . . H25C H 0.2420 0.3022 0.1812 0.061 Uiso 1 1 calc R . . C26 C 0.29239(7) 0.2134(2) 0.25384(7) 0.0436(5) Uani 1 1 d . . . H26A H 0.2727 0.2288 0.2776 0.065 Uiso 1 1 calc R . . H26B H 0.3031 0.2927 0.2432 0.065 Uiso 1 1 calc R . . H26C H 0.3153 0.1628 0.2683 0.065 Uiso 1 1 calc R . . C27 C 0.29530(6) 0.37860(17) 0.10115(7) 0.0270(4) Uani 1 1 d . . . H27A H 0.2886 0.3876 0.0661 0.032 Uiso 1 1 calc R . . H27B H 0.2709 0.3384 0.1133 0.032 Uiso 1 1 calc R . . C28 C 0.29603(6) 0.51169(18) 0.12131(7) 0.0322(4) Uani 1 1 d . . . C29 C 0.25458(8) 0.5759(2) 0.10729(9) 0.0519(6) Uani 1 1 d . . . H29A H 0.2500 0.5819 0.0723 0.078 Uiso 1 1 calc R . . H29B H 0.2550 0.6594 0.1212 0.078 Uiso 1 1 calc R . . H29C H 0.2322 0.5277 0.1194 0.078 Uiso 1 1 calc R . . C30 C 0.30349(7) 0.5134(2) 0.17606(7) 0.0395(5) Uani 1 1 d . . . H30A H 0.3283 0.4646 0.1863 0.059 Uiso 1 1 calc R . . H30B H 0.2795 0.4774 0.1898 0.059 Uiso 1 1 calc R . . H30C H 0.3074 0.5991 0.1872 0.059 Uiso 1 1 calc R . . C31 C 0.33027(8) 0.5854(2) 0.10056(9) 0.0482(6) Uani 1 1 d . . . H31A H 0.3257 0.5849 0.0655 0.072 Uiso 1 1 calc R . . H31B H 0.3571 0.5474 0.1107 0.072 Uiso 1 1 calc R . . H31C H 0.3300 0.6711 0.1122 0.072 Uiso 1 1 calc R . . C32 C 0.38830(6) 0.32269(17) 0.15685(6) 0.0258(4) Uani 1 1 d . . . C33 C 0.41269(6) 0.3998(2) 0.18779(7) 0.0350(5) Uani 1 1 d . . . H33 H 0.4018 0.4752 0.1989 0.042 Uiso 1 1 calc R . . C34 C 0.45291(7) 0.3656(2) 0.20212(7) 0.0394(5) Uani 1 1 d . . . H34 H 0.4698 0.4170 0.2235 0.047 Uiso 1 1 calc R . . C35 C 0.46861(6) 0.2570(2) 0.18548(7) 0.0349(5) Uani 1 1 d . . . H35 H 0.4963 0.2333 0.1953 0.042 Uiso 1 1 calc R . . C36 C 0.44381(6) 0.18177(18) 0.15410(6) 0.0280(4) Uani 1 1 d . . . C37 C 0.45975(6) 0.0656(2) 0.13290(8) 0.0367(5) Uani 1 1 d . . . H37A H 0.4449 0.0510 0.1013 0.055 Uiso 1 1 calc R . . H37B H 0.4554 -0.0048 0.1540 0.055 Uiso 1 1 calc R . . H37C H 0.4894 0.0747 0.1296 0.055 Uiso 1 1 calc R . . P3 P 0.532549(18) 0.63360(5) 0.18285(2) 0.03866(14) Uani 1 1 d . . . N3 N 0.5000 0.8154(2) 0.2500 0.0416(6) Uani 1 2 d S . . H3N H 0.5000 0.7338 0.2500 0.050 Uiso 1 2 calc SR . . C38 C 0.57674(7) 0.5599(2) 0.15672(9) 0.0446(6) Uani 1 1 d . . . H38 H 0.5828 0.6076 0.1276 0.054 Uiso 1 1 calc R . . C39 C 0.56506(8) 0.4270(2) 0.14187(12) 0.0699(9) Uani 1 1 d . . . H39A H 0.5880 0.3885 0.1269 0.105 Uiso 1 1 calc R . . H39B H 0.5403 0.4281 0.1189 0.105 Uiso 1 1 calc R . . H39C H 0.5594 0.3792 0.1703 0.105 Uiso 1 1 calc R . . C40 C 0.61503(8) 0.5609(3) 0.19248(10) 0.0592(7) Uani 1 1 d . . . H40A H 0.6383 0.5244 0.1776 0.089 Uiso 1 1 calc R . . H40B H 0.6097 0.5124 0.2208 0.089 Uiso 1 1 calc R . . H40C H 0.6217 0.6466 0.2020 0.089 Uiso 1 1 calc R . . C41 C 0.49231(7) 0.6418(2) 0.13129(9) 0.0456(6) Uani 1 1 d . . . H41 H 0.4847 0.5544 0.1224 0.055 Uiso 1 1 calc R . . C42 C 0.45338(7) 0.7034(2) 0.14655(10) 0.0545(7) Uani 1 1 d . . . H42A H 0.4311 0.6966 0.1206 0.082 Uiso 1 1 calc R . . H42B H 0.4590 0.7912 0.1536 0.082 Uiso 1 1 calc R . . H42C H 0.4450 0.6621 0.1753 0.082 Uiso 1 1 calc R . . C43 C 0.57845(6) 0.8524(2) 0.16462(7) 0.0369(5) Uani 1 1 d . . . H43 H 0.5906 0.8042 0.1413 0.044 Uiso 1 1 calc R . . C44 C 0.50509(8) 0.7044(3) 0.08606(9) 0.0646(8) Uani 1 1 d . . . H44A H 0.4818 0.7032 0.0611 0.097 Uiso 1 1 calc R . . H44B H 0.5286 0.6597 0.0747 0.097 Uiso 1 1 calc R . . H44C H 0.5131 0.7905 0.0934 0.097 Uiso 1 1 calc R . . C45 C 0.54821(6) 0.79716(19) 0.18979(7) 0.0332(4) Uani 1 1 d . . . C46 C 0.59169(6) 0.9738(2) 0.17176(7) 0.0374(5) Uani 1 1 d . . . C47 C 0.62524(7) 1.0271(2) 0.14369(9) 0.0521(6) Uani 1 1 d . . . H47A H 0.6205 1.0008 0.1101 0.078 Uiso 1 1 calc R . . H47B H 0.6523 0.9970 0.1574 0.078 Uiso 1 1 calc R . . H47C H 0.6246 1.1179 0.1454 0.078 Uiso 1 1 calc R . . C48 C 0.57378(6) 1.0414(2) 0.20615(7) 0.0371(5) Uani 1 1 d . . . H48 H 0.5823 1.1248 0.2120 0.044 Uiso 1 1 calc R . . C49 C 0.54380(6) 0.99122(19) 0.23229(7) 0.0343(5) Uani 1 1 d . . . H49 H 0.5325 1.0401 0.2561 0.041 Uiso 1 1 calc R . . C50 C 0.52998(6) 0.87018(18) 0.22421(6) 0.0315(4) 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 V1 0.02058(14) 0.01704(15) 0.01943(14) -0.00146(12) 0.00291(11) 0.00027(11) P1 0.0209(2) 0.0179(2) 0.0213(2) 0.00107(17) 0.00478(17) 0.00086(17) P2 0.0240(2) 0.0235(2) 0.0195(2) -0.00038(18) 0.00493(17) -0.00156(18) N1 0.0227(7) 0.0177(7) 0.0207(7) -0.0010(6) 0.0056(6) -0.0016(6) N2 0.0237(8) 0.0255(8) 0.0231(7) 0.0036(6) 0.0027(6) -0.0016(6) C1 0.0264(9) 0.0279(10) 0.0216(8) 0.0035(7) 0.0036(7) 0.0060(8) C2 0.0257(9) 0.0429(12) 0.0261(9) 0.0019(9) -0.0008(7) 0.0012(9) C3 0.0375(11) 0.0454(13) 0.0245(9) 0.0072(9) 0.0070(8) 0.0044(10) C4 0.0262(9) 0.0232(10) 0.0297(9) 0.0017(8) 0.0070(7) -0.0030(7) C5 0.0385(11) 0.0238(10) 0.0521(13) 0.0041(9) 0.0081(10) -0.0063(9) C6 0.0256(10) 0.0336(11) 0.0405(11) 0.0014(9) 0.0037(8) -0.0073(8) C7 0.0221(8) 0.0200(9) 0.0200(8) 0.0002(7) 0.0029(6) 0.0024(7) C8 0.0242(9) 0.0272(10) 0.0251(9) 0.0011(8) 0.0065(7) 0.0031(7) C9 0.0273(9) 0.0292(10) 0.0281(9) -0.0042(8) 0.0061(7) 0.0060(8) C10 0.0373(11) 0.0387(12) 0.0466(12) -0.0079(10) 0.0172(10) 0.0096(9) C11 0.0374(11) 0.0193(9) 0.0344(10) -0.0041(8) 0.0068(8) 0.0054(8) C12 0.0317(10) 0.0205(9) 0.0309(10) -0.0008(8) 0.0083(8) -0.0011(8) C13 0.0232(8) 0.0195(9) 0.0189(8) -0.0018(7) 0.0030(6) 0.0003(7) C14 0.0219(8) 0.0168(8) 0.0235(8) 0.0008(7) 0.0029(7) 0.0019(7) C15 0.0285(9) 0.0243(9) 0.0241(9) -0.0024(7) 0.0034(7) -0.0005(8) C16 0.0278(9) 0.0224(10) 0.0307(9) -0.0035(8) -0.0031(8) -0.0009(8) C17 0.0214(9) 0.0191(9) 0.0384(10) 0.0013(8) 0.0016(7) 0.0000(7) C18 0.0231(10) 0.0322(11) 0.0506(12) 0.0006(10) 0.0036(9) -0.0039(8) C19 0.0230(9) 0.0231(9) 0.0285(9) 0.0014(8) 0.0060(7) -0.0004(7) C20 0.0219(8) 0.0207(9) 0.0226(8) 0.0008(7) 0.0017(7) 0.0017(7) C21 0.0311(10) 0.0295(10) 0.0278(9) 0.0060(8) -0.0024(8) -0.0034(8) C22 0.0530(14) 0.0387(13) 0.0387(12) 0.0158(10) 0.0064(10) -0.0020(11) C23 0.0341(11) 0.0328(12) 0.0466(12) 0.0108(10) 0.0041(9) 0.0063(9) C24 0.0338(10) 0.0366(11) 0.0257(9) -0.0050(8) 0.0116(8) -0.0040(9) C25 0.0325(11) 0.0473(13) 0.0435(12) -0.0138(10) 0.0154(9) 0.0019(10) C26 0.0552(14) 0.0494(14) 0.0270(10) -0.0085(10) 0.0081(9) -0.0011(11) C27 0.0286(9) 0.0250(10) 0.0274(9) -0.0031(8) 0.0033(7) 0.0041(8) C28 0.0409(11) 0.0227(10) 0.0327(10) -0.0044(8) 0.0030(8) 0.0060(8) C29 0.0617(16) 0.0422(14) 0.0502(14) -0.0089(11) -0.0038(12) 0.0268(12) C30 0.0481(13) 0.0353(12) 0.0349(11) -0.0110(9) 0.0030(9) 0.0058(10) C31 0.0698(16) 0.0250(11) 0.0508(14) -0.0004(10) 0.0109(12) -0.0053(11) C32 0.0290(10) 0.0264(10) 0.0222(9) 0.0022(7) 0.0033(7) -0.0024(8) C33 0.0405(11) 0.0310(11) 0.0323(10) -0.0028(9) -0.0020(9) -0.0057(9) C34 0.0402(12) 0.0385(12) 0.0370(11) 0.0018(10) -0.0095(9) -0.0125(10) C35 0.0271(10) 0.0374(12) 0.0387(11) 0.0127(9) -0.0044(8) -0.0046(9) C36 0.0246(9) 0.0316(11) 0.0278(9) 0.0109(8) 0.0030(7) -0.0006(8) C37 0.0311(11) 0.0393(12) 0.0400(11) 0.0058(10) 0.0054(9) 0.0072(9) P3 0.0445(3) 0.0290(3) 0.0470(3) -0.0082(2) 0.0282(3) -0.0086(2) N3 0.0634(17) 0.0262(13) 0.0402(14) 0.000 0.0306(13) 0.000 C38 0.0440(13) 0.0398(13) 0.0547(14) -0.0124(11) 0.0286(11) -0.0068(10) C39 0.0548(16) 0.0481(16) 0.113(2) -0.0299(16) 0.0428(17) -0.0034(13) C40 0.0535(15) 0.0612(17) 0.0663(17) 0.0013(14) 0.0231(13) 0.0039(13) C41 0.0419(12) 0.0383(13) 0.0598(14) -0.0172(11) 0.0210(11) -0.0140(10) C42 0.0469(14) 0.0381(14) 0.0808(19) -0.0096(13) 0.0188(13) -0.0045(11) C43 0.0413(12) 0.0419(12) 0.0285(10) -0.0018(9) 0.0090(9) -0.0118(10) C44 0.0566(16) 0.092(2) 0.0461(14) -0.0123(15) 0.0092(12) -0.0249(16) C45 0.0443(12) 0.0311(11) 0.0258(9) -0.0022(8) 0.0111(8) -0.0098(9) C46 0.0395(12) 0.0409(12) 0.0305(10) 0.0070(9) -0.0032(9) -0.0149(10) C47 0.0523(14) 0.0575(16) 0.0466(13) 0.0086(12) 0.0047(11) -0.0285(12) C48 0.0429(12) 0.0297(11) 0.0358(11) 0.0020(9) -0.0107(9) -0.0078(9) C49 0.0452(12) 0.0309(11) 0.0254(9) -0.0021(8) -0.0033(8) 0.0015(9) C50 0.0440(11) 0.0290(11) 0.0224(9) 0.0024(8) 0.0082(8) -0.0019(9) _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 N1 2.0369(14) . ? V1 C32 2.0514(18) . ? V1 N2 2.1200(15) . ? V1 C27 2.1262(18) . ? V1 P2 2.5442(6) . ? V1 P1 2.5462(6) . ? P1 C7 1.8229(18) . ? P1 C4 1.8529(18) . ? P1 C1 1.8617(18) . ? P2 C20 1.8191(18) . ? P2 C24 1.8537(18) . ? P2 C21 1.8598(19) . ? N1 C14 1.406(2) . ? N1 C13 1.407(2) . ? N2 C36 1.340(2) . ? N2 C32 1.349(2) . ? C1 C2 1.520(3) . ? C1 C3 1.523(2) . ? 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 1.524(3) . ? C4 C5 1.531(3) . ? 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 1.396(2) . ? C7 C13 1.409(2) . ? C8 C9 1.391(3) . ? C8 H8 0.9500 . ? C9 C11 1.390(3) . ? C9 C10 1.510(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.382(2) . ? C11 H11 0.9500 . ? C12 C13 1.401(2) . ? C12 H12 0.9500 . ? C14 C15 1.402(2) . ? C14 C20 1.411(2) . ? C15 C16 1.385(2) . ? C15 H15 0.9500 . ? C16 C17 1.389(3) . ? C16 H16 0.9500 . ? C17 C19 1.389(3) . ? C17 C18 1.509(2) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.400(2) . ? C19 H19A 0.9500 . ? C21 C23 1.517(3) . ? C21 C22 1.524(3) . ? 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 C25 1.525(3) . ? C24 C26 1.531(3) . ? 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 1.541(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C31 1.525(3) . ? C28 C30 1.529(3) . ? C28 C29 1.531(3) . ? 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 C33 1.392(3) . ? C33 C34 1.379(3) . ? C33 H33 0.9500 . ? C34 C35 1.375(3) . ? C34 H34 0.9500 . ? C35 C36 1.394(3) . ? C35 H35 0.9500 . ? C36 C37 1.498(3) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? P3 C45 1.840(2) . ? P3 C38 1.850(2) . ? P3 C41 1.855(3) . ? N3 C50 1.397(2) . ? N3 C50 1.397(2) 2_655 ? N3 H3N 0.8800 . ? C38 C40 1.520(4) . ? C38 C39 1.529(3) . ? C38 H38 1.0000 . ? 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 C42 1.524(3) . ? C41 C44 1.527(3) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C46 1.386(3) . ? C43 C45 1.395(3) . ? C43 H43 0.9500 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C50 1.417(3) . ? C46 C48 1.379(3) . ? C46 C47 1.516(3) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.382(3) . ? C48 H48 0.9500 . ? C49 C50 1.391(3) . ? C49 H49 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 V1 C32 141.12(7) . . ? N1 V1 N2 103.57(6) . . ? C32 V1 N2 37.70(6) . . ? N1 V1 C27 113.67(7) . . ? C32 V1 C27 105.21(7) . . ? N2 V1 C27 142.57(7) . . ? N1 V1 P2 76.91(4) . . ? C32 V1 P2 99.62(5) . . ? N2 V1 P2 96.21(4) . . ? C27 V1 P2 95.71(5) . . ? N1 V1 P1 76.62(4) . . ? C32 V1 P1 100.20(5) . . ? N2 V1 P1 88.87(4) . . ? C27 V1 P1 95.87(5) . . ? P2 V1 P1 153.503(19) . . ? C7 P1 C4 104.89(8) . . ? C7 P1 C1 103.74(8) . . ? C4 P1 C1 102.68(8) . . ? C7 P1 V1 94.62(5) . . ? C4 P1 V1 129.75(6) . . ? C1 P1 V1 117.10(6) . . ? C20 P2 C24 104.84(8) . . ? C20 P2 C21 104.65(8) . . ? C24 P2 C21 102.81(9) . . ? C20 P2 V1 95.88(6) . . ? C24 P2 V1 130.49(7) . . ? C21 P2 V1 114.77(6) . . ? C14 N1 C13 118.72(14) . . ? C14 N1 V1 121.19(10) . . ? C13 N1 V1 119.94(11) . . ? C36 N2 C32 122.99(16) . . ? C36 N2 V1 167.93(14) . . ? C32 N2 V1 68.39(10) . . ? C2 C1 C3 109.20(16) . . ? C2 C1 P1 111.20(12) . . ? C3 C1 P1 114.48(12) . . ? 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 110.27(16) . . ? C6 C4 P1 112.43(13) . . ? C5 C4 P1 110.92(13) . . ? C6 C4 H4 107.7 . . ? C5 C4 H4 107.7 . . ? P1 C4 H4 107.7 . . ? 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 119.99(16) . . ? C8 C7 P1 125.73(14) . . ? C13 C7 P1 114.24(12) . . ? C9 C8 C7 122.07(17) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? C11 C9 C8 117.23(16) . . ? C11 C9 C10 121.62(18) . . ? C8 C9 C10 121.15(18) . . ? 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 121.98(17) . . ? C12 C11 H11 119.0 . . ? C9 C11 H11 119.0 . . ? C11 C12 C13 120.94(17) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 N1 123.26(15) . . ? C12 C13 C7 117.77(15) . . ? N1 C13 C7 118.80(15) . . ? C15 C14 N1 122.98(15) . . ? C15 C14 C20 117.74(15) . . ? N1 C14 C20 119.16(15) . . ? C16 C15 C14 121.09(16) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 121.73(17) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C19 C17 C16 117.58(16) . . ? C19 C17 C18 121.27(17) . . ? C16 C17 C18 121.15(17) . . ? 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 . . ? C17 C19 C20 122.00(16) . . ? C17 C19 H19A 119.0 . . ? C20 C19 H19A 119.0 . . ? C19 C20 C14 119.85(16) . . ? C19 C20 P2 125.86(13) . . ? C14 C20 P2 114.25(12) . . ? C23 C21 C22 109.10(17) . . ? C23 C21 P2 110.67(13) . . ? C22 C21 P2 115.42(14) . . ? 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 . . ? C25 C24 C26 111.17(17) . . ? C25 C24 P2 113.23(13) . . ? C26 C24 P2 109.99(14) . . ? C25 C24 H24 107.4 . . ? C26 C24 H24 107.4 . . ? P2 C24 H24 107.4 . . ? 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 127.31(13) . . ? C28 C27 H27A 105.5 . . ? V1 C27 H27A 105.5 . . ? C28 C27 H27B 105.5 . . ? V1 C27 H27B 105.5 . . ? H27A C27 H27B 106.1 . . ? C31 C28 C30 108.91(18) . . ? C31 C28 C29 108.77(19) . . ? C30 C28 C29 107.66(17) . . ? C31 C28 C27 109.35(16) . . ? C30 C28 C27 111.94(16) . . ? C29 C28 C27 110.15(17) . . ? 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 . . ? N2 C32 C33 119.17(17) . . ? N2 C32 V1 73.91(10) . . ? C33 C32 V1 166.61(16) . . ? C34 C33 C32 119.2(2) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C35 C34 C33 120.03(19) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 119.86(18) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? N2 C36 C35 118.73(18) . . ? N2 C36 C37 118.91(17) . . ? C35 C36 C37 122.33(17) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C45 P3 C38 103.64(10) . . ? C45 P3 C41 101.75(10) . . ? C38 P3 C41 103.19(11) . . ? C50 N3 C50 130.0(2) . 2_655 ? C50 N3 H3N 115.0 . . ? C50 N3 H3N 115.0 2_655 . ? C40 C38 C39 110.6(2) . . ? C40 C38 P3 110.68(16) . . ? C39 C38 P3 109.14(15) . . ? C40 C38 H38 108.8 . . ? C39 C38 H38 108.8 . . ? P3 C38 H38 108.8 . . ? 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 . . ? C42 C41 C44 109.8(2) . . ? C42 C41 P3 110.13(17) . . ? C44 C41 P3 116.09(16) . . ? C42 C41 H41 106.8 . . ? C44 C41 H41 106.8 . . ? P3 C41 H41 106.8 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C46 C43 C45 123.6(2) . . ? C46 C43 H43 118.2 . . ? C45 C43 H43 118.2 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 C50 117.79(19) . . ? C43 C45 P3 123.80(16) . . ? C50 C45 P3 118.35(14) . . ? C48 C46 C43 116.98(19) . . ? C48 C46 C47 122.3(2) . . ? C43 C46 C47 120.7(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 C49 121.9(2) . . ? C46 C48 H48 119.1 . . ? C49 C48 H48 119.1 . . ? C48 C49 C50 120.87(19) . . ? C48 C49 H49 119.6 . . ? C50 C49 H49 119.6 . . ? C49 C50 N3 122.81(19) . . ? C49 C50 C45 118.84(18) . . ? N3 C50 C45 118.30(18) . . ? 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 V1 P1 C7 -29.18(7) . . . . ? C32 V1 P1 C7 111.19(8) . . . . ? N2 V1 P1 C7 75.05(7) . . . . ? C27 V1 P1 C7 -142.16(7) . . . . ? P2 V1 P1 C7 -26.66(7) . . . . ? N1 V1 P1 C4 -142.92(9) . . . . ? C32 V1 P1 C4 -2.55(10) . . . . ? N2 V1 P1 C4 -38.69(9) . . . . ? C27 V1 P1 C4 104.10(9) . . . . ? P2 V1 P1 C4 -140.41(8) . . . . ? N1 V1 P1 C1 78.82(8) . . . . ? C32 V1 P1 C1 -140.81(9) . . . . ? N2 V1 P1 C1 -176.95(8) . . . . ? C27 V1 P1 C1 -34.16(9) . . . . ? P2 V1 P1 C1 81.33(8) . . . . ? N1 V1 P2 C20 -25.93(7) . . . . ? C32 V1 P2 C20 -166.40(8) . . . . ? N2 V1 P2 C20 -128.47(7) . . . . ? C27 V1 P2 C20 87.08(7) . . . . ? P1 V1 P2 C20 -28.45(7) . . . . ? N1 V1 P2 C24 -141.18(9) . . . . ? C32 V1 P2 C24 78.36(10) . . . . ? N2 V1 P2 C24 116.29(9) . . . . ? C27 V1 P2 C24 -28.17(10) . . . . ? P1 V1 P2 C24 -143.70(9) . . . . ? N1 V1 P2 C21 83.19(8) . . . . ? C32 V1 P2 C21 -57.27(9) . . . . ? N2 V1 P2 C21 -19.34(8) . . . . ? C27 V1 P2 C21 -163.80(9) . . . . ? P1 V1 P2 C21 80.68(8) . . . . ? C32 V1 N1 C14 122.70(14) . . . . ? N2 V1 N1 C14 126.90(12) . . . . ? C27 V1 N1 C14 -56.99(14) . . . . ? P2 V1 N1 C14 33.56(11) . . . . ? P1 V1 N1 C14 -147.59(13) . . . . ? C32 V1 N1 C13 -52.77(17) . . . . ? N2 V1 N1 C13 -48.56(13) . . . . ? C27 V1 N1 C13 127.55(13) . . . . ? P2 V1 N1 C13 -141.90(13) . . . . ? P1 V1 N1 C13 36.95(11) . . . . ? N1 V1 N2 C36 22.9(6) . . . . ? C32 V1 N2 C36 -161.5(7) . . . . ? C27 V1 N2 C36 -151.3(6) . . . . ? P2 V1 N2 C36 100.8(6) . . . . ? P1 V1 N2 C36 -53.1(6) . . . . ? N1 V1 N2 C32 -175.69(10) . . . . ? C27 V1 N2 C32 10.17(15) . . . . ? P2 V1 N2 C32 -97.70(9) . . . . ? P1 V1 N2 C32 108.37(9) . . . . ? C7 P1 C1 C2 54.80(14) . . . . ? C4 P1 C1 C2 163.84(13) . . . . ? V1 P1 C1 C2 -47.80(14) . . . . ? C7 P1 C1 C3 -69.54(16) . . . . ? C4 P1 C1 C3 39.50(16) . . . . ? V1 P1 C1 C3 -172.15(12) . . . . ? C7 P1 C4 C6 -66.31(15) . . . . ? C1 P1 C4 C6 -174.47(14) . . . . ? V1 P1 C4 C6 42.94(17) . . . . ? C7 P1 C4 C5 169.70(14) . . . . ? C1 P1 C4 C5 61.54(15) . . . . ? V1 P1 C4 C5 -81.05(15) . . . . ? C4 P1 C7 C8 -19.51(18) . . . . ? C1 P1 C7 C8 87.88(16) . . . . ? V1 P1 C7 C8 -152.77(15) . . . . ? C4 P1 C7 C13 158.58(13) . . . . ? C1 P1 C7 C13 -94.03(14) . . . . ? V1 P1 C7 C13 25.32(13) . . . . ? C13 C7 C8 C9 -0.3(3) . . . . ? P1 C7 C8 C9 177.72(14) . . . . ? C7 C8 C9 C11 0.9(3) . . . . ? C7 C8 C9 C10 -178.91(17) . . . . ? C8 C9 C11 C12 -0.7(3) . . . . ? C10 C9 C11 C12 179.10(19) . . . . ? C9 C11 C12 C13 -0.1(3) . . . . ? C11 C12 C13 N1 -174.52(17) . . . . ? C11 C12 C13 C7 0.8(3) . . . . ? C14 N1 C13 C12 -31.9(2) . . . . ? V1 N1 C13 C12 143.70(15) . . . . ? C14 N1 C13 C7 152.87(15) . . . . ? V1 N1 C13 C7 -31.6(2) . . . . ? C8 C7 C13 C12 -0.6(2) . . . . ? P1 C7 C13 C12 -178.80(13) . . . . ? C8 C7 C13 N1 174.92(15) . . . . ? P1 C7 C13 N1 -3.3(2) . . . . ? C13 N1 C14 C15 -38.1(2) . . . . ? V1 N1 C14 C15 146.43(14) . . . . ? C13 N1 C14 C20 146.01(16) . . . . ? V1 N1 C14 C20 -29.5(2) . . . . ? N1 C14 C15 C16 -175.34(16) . . . . ? C20 C14 C15 C16 0.6(3) . . . . ? C14 C15 C16 C17 -0.7(3) . . . . ? C15 C16 C17 C19 0.0(3) . . . . ? C15 C16 C17 C18 179.41(17) . . . . ? C16 C17 C19 C20 0.7(3) . . . . ? C18 C17 C19 C20 -178.74(17) . . . . ? C17 C19 C20 C14 -0.7(3) . . . . ? C17 C19 C20 P2 176.95(14) . . . . ? C15 C14 C20 C19 0.0(2) . . . . ? N1 C14 C20 C19 176.15(15) . . . . ? C15 C14 C20 P2 -177.88(13) . . . . ? N1 C14 C20 P2 -1.7(2) . . . . ? C24 P2 C20 C19 -21.18(18) . . . . ? C21 P2 C20 C19 86.66(17) . . . . ? V1 P2 C20 C19 -155.81(15) . . . . ? C24 P2 C20 C14 156.56(13) . . . . ? C21 P2 C20 C14 -95.61(14) . . . . ? V1 P2 C20 C14 21.93(13) . . . . ? C20 P2 C21 C23 53.24(15) . . . . ? C24 P2 C21 C23 162.56(14) . . . . ? V1 P2 C21 C23 -50.49(15) . . . . ? C20 P2 C21 C22 -71.28(17) . . . . ? C24 P2 C21 C22 38.05(17) . . . . ? V1 P2 C21 C22 -175.01(13) . . . . ? C20 P2 C24 C25 -59.46(16) . . . . ? C21 P2 C24 C25 -168.65(15) . . . . ? V1 P2 C24 C25 51.98(18) . . . . ? C20 P2 C24 C26 175.48(15) . . . . ? C21 P2 C24 C26 66.30(16) . . . . ? V1 P2 C24 C26 -73.08(17) . . . . ? N1 V1 C27 C28 -173.77(15) . . . . ? C32 V1 C27 C28 6.44(18) . . . . ? N2 V1 C27 C28 0.0(2) . . . . ? P2 V1 C27 C28 108.04(16) . . . . ? P1 V1 C27 C28 -95.83(16) . . . . ? V1 C27 C28 C31 61.4(2) . . . . ? V1 C27 C28 C30 -59.4(2) . . . . ? V1 C27 C28 C29 -179.12(15) . . . . ? C36 N2 C32 C33 -1.4(3) . . . . ? V1 N2 C32 C33 -176.83(18) . . . . ? C36 N2 C32 V1 175.45(16) . . . . ? N1 V1 C32 N2 6.69(15) . . . . ? C27 V1 C32 N2 -173.62(10) . . . . ? P2 V1 C32 N2 87.72(9) . . . . ? P1 V1 C32 N2 -74.60(9) . . . . ? N1 V1 C32 C33 174.7(6) . . . . ? N2 V1 C32 C33 168.0(7) . . . . ? C27 V1 C32 C33 -5.6(6) . . . . ? P2 V1 C32 C33 -104.3(6) . . . . ? P1 V1 C32 C33 93.4(6) . . . . ? N2 C32 C33 C34 0.0(3) . . . . ? V1 C32 C33 C34 -166.8(5) . . . . ? C32 C33 C34 C35 0.7(3) . . . . ? C33 C34 C35 C36 0.0(3) . . . . ? C32 N2 C36 C35 2.1(3) . . . . ? V1 N2 C36 C35 161.4(5) . . . . ? C32 N2 C36 C37 -176.35(16) . . . . ? V1 N2 C36 C37 -17.0(7) . . . . ? C34 C35 C36 N2 -1.4(3) . . . . ? C34 C35 C36 C37 177.00(18) . . . . ? C45 P3 C38 C40 66.67(19) . . . . ? C41 P3 C38 C40 172.46(17) . . . . ? C45 P3 C38 C39 -171.4(2) . . . . ? C41 P3 C38 C39 -65.6(2) . . . . ? C45 P3 C41 C42 -71.69(17) . . . . ? C38 P3 C41 C42 -178.92(16) . . . . ? C45 P3 C41 C44 53.8(2) . . . . ? C38 P3 C41 C44 -53.4(2) . . . . ? C46 C43 C45 C50 0.5(3) . . . . ? C46 C43 C45 P3 -176.50(17) . . . . ? C38 P3 C45 C43 20.4(2) . . . . ? C41 P3 C45 C43 -86.5(2) . . . . ? C38 P3 C45 C50 -156.65(18) . . . . ? C41 P3 C45 C50 96.47(18) . . . . ? C45 C43 C46 C48 0.6(3) . . . . ? C45 C43 C46 C47 178.9(2) . . . . ? C43 C46 C48 C49 -0.3(3) . . . . ? C47 C46 C48 C49 -178.64(19) . . . . ? C46 C48 C49 C50 -1.1(3) . . . . ? C48 C49 C50 N3 179.49(17) . . . . ? C48 C49 C50 C45 2.2(3) . . . . ? C50 N3 C50 C49 21.49(15) 2_655 . . . ? C50 N3 C50 C45 -161.2(2) 2_655 . . . ? C43 C45 C50 C49 -1.9(3) . . . . ? P3 C45 C50 C49 175.27(15) . . . . ? C43 C45 C50 N3 -179.30(17) . . . . ? P3 C45 C50 N3 -2.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.328 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.050 # Attachment '- 4.cif' data_09510 _database_code_depnum_ccdc_archive 'CCDC 730604' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H50 N P2 V' _chemical_formula_sum 'C38 H50 N P2 V' _chemical_formula_weight 633.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0667 0.0580 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.2276 0.3376 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.1601(5) _cell_length_b 19.1808(5) _cell_length_c 20.2261(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7045.3(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9600 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 17.2 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.011 _exptl_crystal_size_mid 0.010 _exptl_crystal_size_min 0.003 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 0.211 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.9979 _exptl_absorpt_correction_T_max 0.9994 _exptl_absorpt_process_details 'SADABS, R. Blessing; 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.41328 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator 'diamond 1 1 1' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_measurement_method 'omega and phi scans' _diffrn_measurement_details '0.30 degree frames measured for 0.3 seconds each' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker APEXII' _diffrn_detector_area_resol_mean 83.33 _diffrn_reflns_number 137251 _diffrn_reflns_av_R_equivalents 0.0642 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 17.19 _reflns_number_total 10771 _reflns_number_gt 8869 _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^)+(0.0380P)^2^+2.9754P] 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 10771 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0876 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 V1 V 0.290205(10) 0.096114(10) 0.399030(9) 0.01419(5) Uani 1 1 d . . . P1 P 0.373320(15) 0.162988(15) 0.324637(14) 0.01482(6) Uani 1 1 d . . . P2 P 0.174911(16) 0.042630(16) 0.442858(15) 0.01611(6) Uani 1 1 d . . . N1 N 0.22178(5) 0.11727(5) 0.32583(5) 0.01609(18) Uani 1 1 d . . . C1 C 0.41354(7) 0.11176(7) 0.25508(6) 0.0204(2) Uani 1 1 d . . . H1A H 0.4524 0.0810 0.2745 0.025 Uiso 1 1 calc R . . C2 C 0.45069(8) 0.15546(8) 0.20153(7) 0.0307(3) Uani 1 1 d . . . H2A H 0.4702 0.1247 0.1671 0.046 Uiso 1 1 calc R . . H2B H 0.4911 0.1824 0.2211 0.046 Uiso 1 1 calc R . . H2C H 0.4146 0.1874 0.1820 0.046 Uiso 1 1 calc R . . C3 C 0.35531(8) 0.06379(7) 0.22416(6) 0.0248(3) Uani 1 1 d . . . H3A H 0.3782 0.0353 0.1896 0.037 Uiso 1 1 calc R . . H3B H 0.3159 0.0921 0.2048 0.037 Uiso 1 1 calc R . . H3C H 0.3347 0.0333 0.2584 0.037 Uiso 1 1 calc R . . C4 C 0.44683(6) 0.22613(6) 0.34673(6) 0.0201(2) Uani 1 1 d . . . H4A H 0.4617 0.2514 0.3056 0.024 Uiso 1 1 calc R . . C5 C 0.42129(7) 0.28053(7) 0.39757(7) 0.0254(3) Uani 1 1 d . . . H5A H 0.4605 0.3148 0.4046 0.038 Uiso 1 1 calc R . . H5B H 0.4100 0.2573 0.4395 0.038 Uiso 1 1 calc R . . H5C H 0.3771 0.3042 0.3811 0.038 Uiso 1 1 calc R . . C6 C 0.51469(7) 0.18652(7) 0.37291(8) 0.0289(3) Uani 1 1 d . . . H6A H 0.5553 0.2194 0.3798 0.043 Uiso 1 1 calc R . . H6B H 0.5296 0.1511 0.3407 0.043 Uiso 1 1 calc R . . H6C H 0.5024 0.1639 0.4149 0.043 Uiso 1 1 calc R . . C7 C 0.29869(6) 0.21330(6) 0.28726(6) 0.0159(2) Uani 1 1 d . . . C8 C 0.30536(7) 0.28019(6) 0.26011(6) 0.0189(2) Uani 1 1 d . . . H8A H 0.3525 0.3016 0.2589 0.023 Uiso 1 1 calc R . . C9 C 0.24489(7) 0.31638(6) 0.23472(6) 0.0207(2) Uani 1 1 d . . . C10 C 0.25246(8) 0.38955(7) 0.20766(7) 0.0287(3) Uani 1 1 d . . . H10A H 0.2062 0.4149 0.2143 0.043 Uiso 1 1 calc R . . H10B H 0.2637 0.3874 0.1603 0.043 Uiso 1 1 calc R . . H10C H 0.2924 0.4137 0.2309 0.043 Uiso 1 1 calc R . . C11 C 0.17670(7) 0.28252(6) 0.23585(6) 0.0225(2) Uani 1 1 d . . . H11A H 0.1350 0.3053 0.2174 0.027 Uiso 1 1 calc R . . C12 C 0.16821(6) 0.21648(6) 0.26318(6) 0.0200(2) Uani 1 1 d . . . H12A H 0.1209 0.1953 0.2635 0.024 Uiso 1 1 calc R . . C13 C 0.22868(6) 0.18062(6) 0.29046(5) 0.0161(2) Uani 1 1 d . . . C14 C 0.16507(6) 0.06943(6) 0.31005(6) 0.0162(2) Uani 1 1 d . . . C15 C 0.13938(6) 0.05920(6) 0.24484(6) 0.0184(2) Uani 1 1 d . . . H15A H 0.1591 0.0866 0.2099 0.022 Uiso 1 1 calc R . . C16 C 0.08565(7) 0.00960(6) 0.23110(6) 0.0204(2) Uani 1 1 d . . . H16A H 0.0692 0.0039 0.1868 0.024 Uiso 1 1 calc R . . C17 C 0.05524(7) -0.03217(6) 0.28082(6) 0.0210(2) Uani 1 1 d . . . C18 C -0.00329(8) -0.08604(7) 0.26470(7) 0.0295(3) Uani 1 1 d . . . H18A H -0.0255 -0.1031 0.3058 0.044 Uiso 1 1 calc R . . H18B H 0.0192 -0.1251 0.2409 0.044 Uiso 1 1 calc R . . H18C H -0.0414 -0.0647 0.2370 0.044 Uiso 1 1 calc R . . C19 C 0.08121(6) -0.02301(6) 0.34522(6) 0.0202(2) Uani 1 1 d . . . H19A H 0.0614 -0.0511 0.3796 0.024 Uiso 1 1 calc R . . C20 C 0.13570(6) 0.02641(6) 0.36075(6) 0.0174(2) Uani 1 1 d . . . C21 C 0.10170(7) 0.09502(7) 0.48448(6) 0.0222(2) Uani 1 1 d . . . H21A H 0.0568 0.0650 0.4875 0.027 Uiso 1 1 calc R . . C22 C 0.08069(7) 0.15998(7) 0.44433(7) 0.0272(3) Uani 1 1 d . . . H22A H 0.0349 0.1798 0.4619 0.041 Uiso 1 1 calc R . . H22B H 0.0736 0.1470 0.3979 0.041 Uiso 1 1 calc R . . H22C H 0.1202 0.1946 0.4476 0.041 Uiso 1 1 calc R . . C23 C 0.12338(8) 0.11547(8) 0.55539(6) 0.0274(3) Uani 1 1 d . . . H23A H 0.0851 0.1455 0.5744 0.041 Uiso 1 1 calc R . . H23B H 0.1703 0.1407 0.5546 0.041 Uiso 1 1 calc R . . H23C H 0.1285 0.0733 0.5824 0.041 Uiso 1 1 calc R . . C24 C 0.17882(6) -0.04094(6) 0.48988(6) 0.0191(2) Uani 1 1 d . . . H24A H 0.1959 -0.0776 0.4582 0.023 Uiso 1 1 calc R . . C25 C 0.23910(7) -0.03420(7) 0.54355(6) 0.0230(2) Uani 1 1 d . . . H25A H 0.2410 -0.0772 0.5697 0.034 Uiso 1 1 calc R . . H25B H 0.2275 0.0052 0.5726 0.034 Uiso 1 1 calc R . . H25C H 0.2869 -0.0263 0.5224 0.034 Uiso 1 1 calc R . . C26 C 0.10609(7) -0.06720(7) 0.51988(7) 0.0261(3) Uani 1 1 d . . . H26A H 0.1136 -0.1136 0.5389 0.039 Uiso 1 1 calc R . . H26B H 0.0684 -0.0697 0.4853 0.039 Uiso 1 1 calc R . . H26C H 0.0899 -0.0350 0.5546 0.039 Uiso 1 1 calc R . . C27 C 0.34840(7) 0.00235(6) 0.39622(6) 0.0193(2) Uani 1 1 d . . . C28 C 0.32225(7) -0.06354(7) 0.37595(6) 0.0240(2) Uani 1 1 d . . . H28A H 0.2749 -0.0666 0.3562 0.029 Uiso 1 1 calc R . . C29 C 0.36327(9) -0.12430(7) 0.38386(7) 0.0314(3) Uani 1 1 d . . . H29A H 0.3438 -0.1677 0.3697 0.038 Uiso 1 1 calc R . . C30 C 0.43301(10) -0.12135(8) 0.41264(8) 0.0386(4) Uani 1 1 d . . . H30A H 0.4608 -0.1628 0.4190 0.046 Uiso 1 1 calc R . . C31 C 0.46128(9) -0.05741(9) 0.43185(8) 0.0371(3) Uani 1 1 d . . . H31A H 0.5090 -0.0548 0.4509 0.045 Uiso 1 1 calc R . . C32 C 0.41980(8) 0.00333(7) 0.42333(7) 0.0267(3) Uani 1 1 d . . . H32A H 0.4405 0.0467 0.4363 0.032 Uiso 1 1 calc R . . C33 C 0.30081(7) 0.16654(6) 0.47552(6) 0.0197(2) Uani 1 1 d . . . C34 C 0.34136(7) 0.15684(7) 0.53401(6) 0.0241(2) Uani 1 1 d . . . H34A H 0.3701 0.1158 0.5390 0.029 Uiso 1 1 calc R . . C35\ C 0.34050(9) 0.20603(8) 0.58504(7) 0.0304(3) Uani 1 1 d . . . H35A H 0.3697 0.1987 0.6234 0.036 Uiso 1 1 calc R . . C36 C 0.29714(9) 0.26559(8) 0.57989(7) 0.0319(3) Uani 1 1 d . . . H36A H 0.2947 0.2979 0.6155 0.038 Uiso 1 1 calc R . . C37 C 0.25721(8) 0.27748(7) 0.52204(7) 0.0281(3) Uani 1 1 d . . . H37A H 0.2279 0.3183 0.5177 0.034 Uiso 1 1 calc R . . C38 C 0.26063(7) 0.22910(7) 0.47075(6) 0.0227(2) Uani 1 1 d . . . H38A H 0.2348 0.2387 0.4309 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.01319(9) 0.01458(9) 0.01480(9) -0.00006(7) -0.00167(6) -0.00005(6) P1 0.01299(12) 0.01496(13) 0.01653(13) 0.00037(10) -0.00089(10) -0.00057(10) P2 0.01410(13) 0.01722(14) 0.01702(13) 0.00031(10) -0.00028(10) -0.00128(10) N1 0.0141(4) 0.0164(4) 0.0178(4) 0.0022(3) -0.0029(3) -0.0018(3) C1 0.0173(5) 0.0246(6) 0.0194(5) -0.0014(4) 0.0013(4) 0.0031(4) C2 0.0248(6) 0.0431(8) 0.0241(6) -0.0024(6) 0.0073(5) -0.0074(6) C3 0.0308(6) 0.0230(6) 0.0205(6) -0.0053(5) 0.0031(5) -0.0015(5) C4 0.0162(5) 0.0201(5) 0.0240(6) 0.0011(4) -0.0014(4) -0.0039(4) C5 0.0232(6) 0.0221(6) 0.0308(6) -0.0044(5) -0.0015(5) -0.0062(5) C6 0.0178(6) 0.0299(7) 0.0388(7) -0.0011(6) -0.0077(5) -0.0018(5) C7 0.0159(5) 0.0152(5) 0.0168(5) 0.0000(4) -0.0013(4) 0.0010(4) C8 0.0198(5) 0.0169(5) 0.0199(5) 0.0014(4) -0.0007(4) -0.0017(4) C9 0.0248(6) 0.0156(5) 0.0218(6) 0.0009(4) -0.0021(4) 0.0016(4) C10 0.0348(7) 0.0174(6) 0.0338(7) 0.0055(5) -0.0044(6) 0.0018(5) C11 0.0218(6) 0.0191(5) 0.0265(6) 0.0010(5) -0.0048(5) 0.0048(4) C12 0.0149(5) 0.0193(5) 0.0258(6) 0.0009(4) -0.0036(4) 0.0008(4) C13 0.0161(5) 0.0157(5) 0.0164(5) -0.0003(4) -0.0010(4) 0.0001(4) C14 0.0134(5) 0.0153(5) 0.0197(5) 0.0002(4) -0.0020(4) 0.0006(4) C15 0.0187(5) 0.0183(5) 0.0183(5) 0.0008(4) -0.0028(4) 0.0004(4) C16 0.0201(5) 0.0191(5) 0.0220(5) -0.0023(4) -0.0062(4) 0.0015(4) C17 0.0190(5) 0.0161(5) 0.0277(6) -0.0023(4) -0.0058(4) -0.0016(4) C18 0.0298(7) 0.0242(6) 0.0344(7) -0.0007(5) -0.0100(6) -0.0092(5) C19 0.0182(5) 0.0186(5) 0.0237(6) 0.0017(4) -0.0018(4) -0.0030(4) C20 0.0147(5) 0.0181(5) 0.0192(5) 0.0001(4) -0.0017(4) -0.0006(4) C21 0.0156(5) 0.0250(6) 0.0259(6) -0.0018(5) 0.0020(4) 0.0018(4) C22 0.0212(6) 0.0281(6) 0.0322(7) -0.0031(5) -0.0036(5) 0.0058(5) C23 0.0278(6) 0.0313(7) 0.0231(6) -0.0036(5) 0.0051(5) 0.0057(5) C24 0.0191(5) 0.0187(5) 0.0194(5) 0.0021(4) 0.0012(4) -0.0020(4) C25 0.0246(6) 0.0236(6) 0.0207(5) 0.0032(5) -0.0020(5) -0.0007(5) C26 0.0245(6) 0.0278(6) 0.0259(6) 0.0049(5) 0.0031(5) -0.0064(5) C27 0.0216(5) 0.0196(5) 0.0166(5) 0.0014(4) 0.0020(4) 0.0025(4) C28 0.0285(6) 0.0227(6) 0.0208(6) -0.0012(5) 0.0048(5) -0.0011(5) C29 0.0491(9) 0.0185(6) 0.0267(6) -0.0013(5) 0.0099(6) 0.0024(6) C30 0.0537(10) 0.0289(7) 0.0333(7) 0.0046(6) 0.0033(7) 0.0213(7) C31 0.0350(8) 0.0407(8) 0.0355(8) -0.0002(6) -0.0108(6) 0.0163(7) C32 0.0280(6) 0.0258(6) 0.0265(6) -0.0019(5) -0.0060(5) 0.0039(5) C33 0.0198(5) 0.0200(5) 0.0192(5) -0.0026(4) 0.0021(4) -0.0040(4) C34 0.0252(6) 0.0238(6) 0.0234(6) -0.0005(5) -0.0022(5) 0.0002(5) C35\ 0.0388(8) 0.0316(7) 0.0207(6) -0.0026(5) -0.0063(5) -0.0023(6) C36 0.0452(8) 0.0254(7) 0.0251(6) -0.0094(5) 0.0007(6) -0.0031(6) C37 0.0326(7) 0.0197(6) 0.0318(7) -0.0039(5) 0.0027(5) -0.0003(5) C38 0.0232(6) 0.0220(6) 0.0228(6) -0.0009(5) -0.0015(5) -0.0023(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 V1 N1 1.9750(10) . ? V1 C33 2.0628(12) . ? V1 C27 2.0869(12) . ? V1 P1 2.4875(3) . ? V1 P2 2.4944(3) . ? P1 C7 1.8275(11) . ? P1 C4 1.8570(12) . ? P1 C1 1.8649(12) . ? P2 C20 1.8335(12) . ? P2 C24 1.8652(12) . ? P2 C21 1.8672(12) . ? N1 C13 1.4157(14) . ? N1 C14 1.4158(14) . ? C1 C2 1.5268(18) . ? C1 C3 1.5350(18) . ? C1 H1A 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 C5 1.5367(18) . ? C4 C6 1.5415(17) . ? C4 H4A 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 1.4009(16) . ? C7 C13 1.4190(15) . ? C8 C9 1.3969(16) . ? C8 H8A 0.9500 . ? C9 C11 1.3984(18) . ? C9 C10 1.5128(17) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.3905(17) . ? C11 H11A 0.9500 . ? C12 C13 1.4083(16) . ? C12 H12A 0.9500 . ? C14 C15 1.4126(16) . ? C14 C20 1.4202(16) . ? C15 C16 1.3909(16) . ? C15 H15A 0.9500 . ? C16 C17 1.3994(18) . ? C16 H16A 0.9500 . ? C17 C19 1.3964(17) . ? C17 C18 1.5177(17) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.4059(16) . ? C19 H19A 0.9500 . ? C21 C22 1.5354(18) . ? C21 C23 1.5382(18) . ? C21 H21A 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 1.5384(17) . ? C24 C25 1.5470(17) . ? C24 H24A 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 C32 1.4079(18) . ? C27 C28 1.4110(17) . ? C28 C29 1.3922(19) . ? C28 H28A 0.9500 . ? C29 C30 1.395(2) . ? C29 H29A 0.9500 . ? C30 C31 1.385(2) . ? C30 H30A 0.9500 . ? C31 C32 1.3980(19) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C34 1.4060(17) . ? C33 C38 1.4077(18) . ? C34 C35\ 1.3983(19) . ? C34 H34A 0.9500 . ? C35\ C36 1.392(2) . ? C35\ H35A 0.9500 . ? C36 C37 1.395(2) . ? C36 H36A 0.9500 . ? C37 C38 1.3931(18) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 V1 C33 119.10(5) . . ? N1 V1 C27 118.38(4) . . ? C33 V1 C27 122.51(5) . . ? N1 V1 P1 79.77(3) . . ? C33 V1 P1 93.40(3) . . ? C27 V1 P1 96.93(3) . . ? N1 V1 P2 79.79(3) . . ? C33 V1 P2 94.65(3) . . ? C27 V1 P2 94.61(3) . . ? P1 V1 P2 159.451(13) . . ? C7 P1 C4 106.75(5) . . ? C7 P1 C1 104.87(5) . . ? C4 P1 C1 104.10(6) . . ? C7 P1 V1 94.16(4) . . ? C4 P1 V1 128.82(4) . . ? C1 P1 V1 114.98(4) . . ? C20 P2 C24 109.32(5) . . ? C20 P2 C21 102.90(5) . . ? C24 P2 C21 105.06(6) . . ? C20 P2 V1 94.24(4) . . ? C24 P2 V1 120.18(4) . . ? C21 P2 V1 122.45(4) . . ? C13 N1 C14 120.44(9) . . ? C13 N1 V1 119.97(7) . . ? C14 N1 V1 119.57(7) . . ? C2 C1 C3 110.14(10) . . ? C2 C1 P1 114.77(9) . . ? C3 C1 P1 110.70(8) . . ? C2 C1 H1A 106.9 . . ? C3 C1 H1A 106.9 . . ? P1 C1 H1A 106.9 . . ? 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 . . ? C5 C4 C6 110.24(11) . . ? C5 C4 P1 112.77(8) . . ? C6 C4 P1 109.63(9) . . ? C5 C4 H4A 108.0 . . ? C6 C4 H4A 108.0 . . ? P1 C4 H4A 108.0 . . ? 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 120.00(10) . . ? C8 C7 P1 125.57(9) . . ? C13 C7 P1 114.35(8) . . ? C9 C8 C7 122.08(11) . . ? C9 C8 H8A 119.0 . . ? C7 C8 H8A 119.0 . . ? C8 C9 C11 117.35(11) . . ? C8 C9 C10 121.50(11) . . ? C11 C9 C10 121.15(11) . . ? 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 121.85(11) . . ? C12 C11 H11A 119.1 . . ? C9 C11 H11A 119.1 . . ? C11 C12 C13 120.94(11) . . ? C11 C12 H12A 119.5 . . ? C13 C12 H12A 119.5 . . ? C12 C13 N1 123.25(10) . . ? C12 C13 C7 117.71(10) . . ? N1 C13 C7 118.78(10) . . ? C15 C14 N1 122.73(10) . . ? C15 C14 C20 118.00(10) . . ? N1 C14 C20 119.14(10) . . ? C16 C15 C14 120.88(11) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C15 C16 C17 121.67(11) . . ? C15 C16 H16A 119.2 . . ? C17 C16 H16A 119.2 . . ? C19 C17 C16 117.70(11) . . ? C19 C17 C18 121.51(12) . . ? C16 C17 C18 120.78(11) . . ? 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 . . ? C17 C19 C20 122.07(11) . . ? C17 C19 H19A 119.0 . . ? C20 C19 H19A 119.0 . . ? C19 C20 C14 119.66(11) . . ? C19 C20 P2 126.17(9) . . ? C14 C20 P2 114.18(8) . . ? C22 C21 C23 110.48(11) . . ? C22 C21 P2 112.04(9) . . ? C23 C21 P2 112.05(9) . . ? C22 C21 H21A 107.3 . . ? C23 C21 H21A 107.3 . . ? P2 C21 H21A 107.3 . . ? 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 110.98(10) . . ? C26 C24 P2 116.73(9) . . ? C25 C24 P2 108.24(8) . . ? C26 C24 H24A 106.8 . . ? C25 C24 H24A 106.8 . . ? P2 C24 H24A 106.8 . . ? 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 . . ? C32 C27 C28 115.80(11) . . ? C32 C27 V1 116.37(9) . . ? C28 C27 V1 127.55(9) . . ? C29 C28 C27 122.43(13) . . ? C29 C28 H28A 118.8 . . ? C27 C28 H28A 118.8 . . ? C28 C29 C30 119.98(14) . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C31 C30 C29 119.30(13) . . ? C31 C30 H30A 120.4 . . ? C29 C30 H30A 120.4 . . ? C30 C31 C32 120.24(14) . . ? C30 C31 H31A 119.9 . . ? C32 C31 H31A 119.9 . . ? C31 C32 C27 122.20(13) . . ? C31 C32 H32A 118.9 . . ? C27 C32 H32A 118.9 . . ? C34 C33 C38 116.22(11) . . ? C34 C33 V1 126.39(9) . . ? C38 C33 V1 117.29(9) . . ? C35\ C34 C33 121.73(12) . . ? C35\ C34 H34A 119.1 . . ? C33 C34 H34A 119.1 . . ? C36 C35\ C34 120.34(13) . . ? C36 C35\ H35A 119.8 . . ? C34 C35\ H35A 119.8 . . ? C35\ C36 C37 119.40(13) . . ? C35\ C36 H36A 120.3 . . ? C37 C36 H36A 120.3 . . ? C38 C37 C36 119.50(13) . . ? C38 C37 H37A 120.3 . . ? C36 C37 H37A 120.3 . . ? C37 C38 C33 122.68(12) . . ? C37 C38 H38A 118.7 . . ? C33 C38 H38A 118.7 . . ? 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 V1 P1 C7 27.28(5) . . . . ? C33 V1 P1 C7 -91.69(5) . . . . ? C27 V1 P1 C7 144.97(5) . . . . ? P2 V1 P1 C7 21.27(5) . . . . ? N1 V1 P1 C4 142.72(6) . . . . ? C33 V1 P1 C4 23.75(6) . . . . ? C27 V1 P1 C4 -99.60(6) . . . . ? P2 V1 P1 C4 136.71(6) . . . . ? N1 V1 P1 C1 -81.24(5) . . . . ? C33 V1 P1 C1 159.79(6) . . . . ? C27 V1 P1 C1 36.44(5) . . . . ? P2 V1 P1 C1 -87.25(6) . . . . ? N1 V1 P2 C20 26.89(5) . . . . ? C33 V1 P2 C20 145.66(5) . . . . ? C27 V1 P2 C20 -91.14(5) . . . . ? P1 V1 P2 C20 32.90(5) . . . . ? N1 V1 P2 C24 142.15(5) . . . . ? C33 V1 P2 C24 -99.08(6) . . . . ? C27 V1 P2 C24 24.12(6) . . . . ? P1 V1 P2 C24 148.16(5) . . . . ? N1 V1 P2 C21 -81.31(6) . . . . ? C33 V1 P2 C21 37.45(6) . . . . ? C27 V1 P2 C21 160.66(6) . . . . ? P1 V1 P2 C21 -75.30(6) . . . . ? C33 V1 N1 C13 54.99(10) . . . . ? C27 V1 N1 C13 -125.61(9) . . . . ? P1 V1 N1 C13 -33.21(8) . . . . ? P2 V1 N1 C13 144.66(9) . . . . ? C33 V1 N1 C14 -123.68(9) . . . . ? C27 V1 N1 C14 55.72(10) . . . . ? P1 V1 N1 C14 148.12(9) . . . . ? P2 V1 N1 C14 -34.02(8) . . . . ? C7 P1 C1 C2 65.55(10) . . . . ? C4 P1 C1 C2 -46.42(10) . . . . ? V1 P1 C1 C2 167.47(8) . . . . ? C7 P1 C1 C3 -59.89(10) . . . . ? C4 P1 C1 C3 -171.86(9) . . . . ? V1 P1 C1 C3 42.02(10) . . . . ? C7 P1 C4 C5 61.81(10) . . . . ? C1 P1 C4 C5 172.42(9) . . . . ? V1 P1 C4 C5 -48.03(11) . . . . ? C7 P1 C4 C6 -174.95(9) . . . . ? C1 P1 C4 C6 -64.35(10) . . . . ? V1 P1 C4 C6 75.20(10) . . . . ? C4 P1 C7 C8 19.79(12) . . . . ? C1 P1 C7 C8 -90.27(11) . . . . ? V1 P1 C7 C8 152.51(10) . . . . ? C4 P1 C7 C13 -156.89(9) . . . . ? C1 P1 C7 C13 93.05(9) . . . . ? V1 P1 C7 C13 -24.17(9) . . . . ? C13 C7 C8 C9 -0.92(18) . . . . ? P1 C7 C8 C9 -177.43(9) . . . . ? C7 C8 C9 C11 -1.51(18) . . . . ? C7 C8 C9 C10 177.91(12) . . . . ? C8 C9 C11 C12 2.28(19) . . . . ? C10 C9 C11 C12 -177.14(12) . . . . ? C9 C11 C12 C13 -0.61(19) . . . . ? C11 C12 C13 N1 172.20(11) . . . . ? C11 C12 C13 C7 -1.84(17) . . . . ? C14 N1 C13 C12 31.21(16) . . . . ? V1 N1 C13 C12 -147.45(9) . . . . ? C14 N1 C13 C7 -154.81(11) . . . . ? V1 N1 C13 C7 26.53(14) . . . . ? C8 C7 C13 C12 2.57(17) . . . . ? P1 C7 C13 C12 179.46(9) . . . . ? C8 C7 C13 N1 -171.74(10) . . . . ? P1 C7 C13 N1 5.14(14) . . . . ? C13 N1 C14 C15 34.53(16) . . . . ? V1 N1 C14 C15 -146.81(9) . . . . ? C13 N1 C14 C20 -149.70(11) . . . . ? V1 N1 C14 C20 28.96(14) . . . . ? N1 C14 C15 C16 177.33(11) . . . . ? C20 C14 C15 C16 1.52(17) . . . . ? C14 C15 C16 C17 -0.30(18) . . . . ? C15 C16 C17 C19 -0.64(18) . . . . ? C15 C16 C17 C18 -179.93(12) . . . . ? C16 C17 C19 C20 0.34(18) . . . . ? C18 C17 C19 C20 179.62(12) . . . . ? C17 C19 C20 C14 0.90(18) . . . . ? C17 C19 C20 P2 -179.28(9) . . . . ? C15 C14 C20 C19 -1.80(16) . . . . ? N1 C14 C20 C19 -177.76(10) . . . . ? C15 C14 C20 P2 178.36(9) . . . . ? N1 C14 C20 P2 2.39(14) . . . . ? C24 P2 C20 C19 33.69(12) . . . . ? C21 P2 C20 C19 -77.57(11) . . . . ? V1 P2 C20 C19 157.75(10) . . . . ? C24 P2 C20 C14 -146.48(8) . . . . ? C21 P2 C20 C14 102.26(9) . . . . ? V1 P2 C20 C14 -22.42(9) . . . . ? C20 P2 C21 C22 -54.74(10) . . . . ? C24 P2 C21 C22 -169.13(9) . . . . ? V1 P2 C21 C22 48.88(10) . . . . ? C20 P2 C21 C23 -179.57(9) . . . . ? C24 P2 C21 C23 66.04(10) . . . . ? V1 P2 C21 C23 -75.96(10) . . . . ? C20 P2 C24 C26 -77.64(10) . . . . ? C21 P2 C24 C26 32.19(11) . . . . ? V1 P2 C24 C26 175.25(8) . . . . ? C20 P2 C24 C25 156.34(8) . . . . ? C21 P2 C24 C25 -93.83(9) . . . . ? V1 P2 C24 C25 49.23(9) . . . . ? N1 V1 C27 C32 146.52(9) . . . . ? C33 V1 C27 C32 -34.10(11) . . . . ? P1 V1 C27 C32 64.43(9) . . . . ? P2 V1 C27 C32 -132.60(9) . . . . ? N1 V1 C27 C28 -39.88(12) . . . . ? C33 V1 C27 C28 139.50(10) . . . . ? P1 V1 C27 C28 -121.97(10) . . . . ? P2 V1 C27 C28 40.99(11) . . . . ? C32 C27 C28 C29 1.82(18) . . . . ? V1 C27 C28 C29 -171.81(10) . . . . ? C27 C28 C29 C30 -0.1(2) . . . . ? C28 C29 C30 C31 -1.3(2) . . . . ? C29 C30 C31 C32 0.9(2) . . . . ? C30 C31 C32 C27 0.9(2) . . . . ? C28 C27 C32 C31 -2.2(2) . . . . ? V1 C27 C32 C31 172.17(12) . . . . ? N1 V1 C33 C34 173.62(10) . . . . ? C27 V1 C33 C34 -5.76(13) . . . . ? P1 V1 C33 C34 -106.20(11) . . . . ? P2 V1 C33 C34 92.72(11) . . . . ? N1 V1 C33 C38 -2.79(11) . . . . ? C27 V1 C33 C38 177.83(9) . . . . ? P1 V1 C33 C38 77.39(9) . . . . ? P2 V1 C33 C38 -83.69(9) . . . . ? C38 C33 C34 C35\ 1.26(19) . . . . ? V1 C33 C34 C35\ -175.18(11) . . . . ? C33 C34 C35\ C36 2.0(2) . . . . ? C34 C35\ C36 C37 -3.0(2) . . . . ? C35\ C36 C37 C38 0.9(2) . . . . ? C36 C37 C38 C33 2.5(2) . . . . ? C34 C33 C38 C37 -3.52(19) . . . . ? V1 C33 C38 C37 173.25(10) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 17.19 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.399 _refine_diff_density_min -0.306 _refine_diff_density_rms 0.053