Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_referee _database_code_CSD 176858 _audit_creation_method SHELXL-97 _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Milione, Stefano' ; Dipartimento di Chimica Univ. di Salerno Via S. Allende I-84081 Baronissi (SA) ITALY ; 'Cavallo, Gabriella' ; Dipartimento di Chimica Univ. di Salerno Via S. Allende I-84081 Baronissi (SA) ITALY ; 'Tedesco, Consiglia' ; Dipartimento di Chimica Univ. di Salerno Via S. Allende I-84081 Baronissi (SA) ITALY ; 'Grassi, Alfonso' ; Dipartimento di Chimica Univ. di Salerno Via S. Allende I-84081 Baronissi (SA) ITALY ; _publ_requested_journal 'Dalton Transactions' _publ_contact_author_name 'Prof Alfonso Grassi' _publ_contact_author_address ; Universita di Salerno Dipartimento di Chimica Via S Allende Baronissi 84081 ITALY ; _publ_contact_author_email grassi@chem.unisa.it _publ_contact_author_fax '39(089)965296' _publ_section_title ; Synthesis of alpha-diimine V(III) complexes adn their role as ethylene polymerisation catalysts ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23.50 H28 Cl3 N2 O V' _chemical_formula_weight 511.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P21/n 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 11.024(9) _cell_length_b 16.299(4) _cell_length_c 13.722(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.47(5) _cell_angle_gamma 90.00 _cell_volume 2465(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 20 _cell_measurement_theta_max 28 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1060 _exptl_absorpt_coefficient_mu 0.745 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'four circle diffractometer' _diffrn_measurement_method '\w-2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 150 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4343 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1488 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4343 _reflns_number_gt 1647 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Molecular Structure Co., 1992' _computing_cell_refinement 'Molecular Structure Co., 1992' _computing_data_reduction 'TEXSAN, Molecular Structure Co., 1992' _computing_structure_solution 'SIR-92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0707P)^2^+12.2190P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4343 _refine_ls_number_parameters 257 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.2047 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.2192 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.006 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.34298(13) 0.16443(9) 0.12654(10) 0.0459(4) Uani 1 1 d . . . Cl1 Cl 0.3130(2) 0.21589(14) 0.28241(16) 0.0627(6) Uani 1 1 d . . . Cl2 Cl 0.3993(2) 0.10114(15) -0.01951(16) 0.0660(7) Uani 1 1 d . . . Cl3 Cl 0.1632(2) 0.21481(16) 0.0655(2) 0.0756(8) Uani 1 1 d . . . O1 O 0.4358(5) 0.2723(4) 0.0829(4) 0.0598(16) Uani 1 1 d . . . N1 N 0.5055(5) 0.1120(4) 0.1845(5) 0.0438(16) Uani 1 1 d . . . N2 N 0.2936(5) 0.0449(4) 0.1742(4) 0.0435(16) Uani 1 1 d . . . C1 C 0.6185(7) 0.1588(5) 0.1906(7) 0.057(2) Uani 1 1 d . . . C2 C 0.6931(8) 0.1567(6) 0.1103(7) 0.074(3) Uani 1 1 d . . . H2 H 0.6727 0.1254 0.0559 0.089 Uiso 1 1 calc R . . C3 C 0.7980(9) 0.2017(8) 0.1127(9) 0.100(4) Uani 1 1 d . . . H3 H 0.8488 0.2013 0.0589 0.119 Uiso 1 1 calc R . . C4 C 0.8287(10) 0.2463(7) 0.1909(11) 0.093(4) Uani 1 1 d . . . H4 H 0.9017 0.2748 0.1913 0.112 Uiso 1 1 calc R . . C5 C 0.7543(11) 0.2506(6) 0.2708(10) 0.089(4) Uani 1 1 d . . . H5 H 0.7752 0.2834 0.3238 0.107 Uiso 1 1 calc R . . C6 C 0.6470(9) 0.2053(6) 0.2711(6) 0.068(3) Uani 1 1 d . . . H6 H 0.5959 0.2065 0.3246 0.082 Uiso 1 1 calc R . . C7 C 0.5009(7) 0.0372(5) 0.2135(5) 0.0409(18) Uani 1 1 d . . . C8 C 0.3798(7) -0.0018(4) 0.2051(5) 0.0412(19) Uani 1 1 d . . . C9 C 0.6058(7) -0.0087(5) 0.2542(6) 0.050(2) Uani 1 1 d . . . H9A H 0.6762 0.0260 0.2545 0.075 Uiso 1 1 calc R . . H9B H 0.6208 -0.0562 0.2148 0.075 Uiso 1 1 calc R . . H9C H 0.5882 -0.0254 0.3196 0.075 Uiso 1 1 calc R . . C10 C 0.3670(7) -0.0899(5) 0.2306(7) 0.056(2) Uani 1 1 d . . . H10A H 0.2842 -0.1065 0.2213 0.084 Uiso 1 1 calc R . . H10B H 0.3902 -0.0981 0.2975 0.084 Uiso 1 1 calc R . . H10C H 0.4184 -0.1222 0.1894 0.084 Uiso 1 1 calc R . . C11 C 0.1716(7) 0.0154(5) 0.1633(6) 0.048(2) Uani 1 1 d . . . C12 C 0.0803(7) 0.0531(6) 0.2159(7) 0.062(3) Uani 1 1 d . . . H12 H 0.0990 0.0959 0.2582 0.075 Uiso 1 1 calc R . . C13 C -0.0382(9) 0.0271(7) 0.2053(8) 0.077(3) Uani 1 1 d . . . H13 H -0.0993 0.0522 0.2408 0.093 Uiso 1 1 calc R . . C14 C -0.0661(8) -0.0362(7) 0.1420(8) 0.074(3) Uani 1 1 d . . . H14 H -0.1460 -0.0536 0.1349 0.088 Uiso 1 1 calc R . . C15 C 0.0230(9) -0.0732(7) 0.0901(8) 0.083(3) Uani 1 1 d . . . H15 H 0.0042 -0.1159 0.0477 0.099 Uiso 1 1 calc R . . C16 C 0.1424(8) -0.0470(7) 0.1006(7) 0.073(3) Uani 1 1 d . . . H16 H 0.2031 -0.0722 0.0646 0.087 Uiso 1 1 calc R . . C17 C 0.4573(11) 0.3434(6) 0.1392(7) 0.085(3) Uani 1 1 d . . . H17A H 0.4909 0.3285 0.2023 0.102 Uiso 1 1 calc R . . H17B H 0.3820 0.3729 0.1493 0.102 Uiso 1 1 calc R . . C18 C 0.5449(16) 0.3957(8) 0.0847(9) 0.148(7) Uani 1 1 d . . . H18A H 0.6276 0.3857 0.1062 0.178 Uiso 1 1 calc R . . H18B H 0.5263 0.4535 0.0924 0.178 Uiso 1 1 calc R . . C19 C 0.5258(16) 0.3686(9) -0.0176(10) 0.157(7) Uani 1 1 d . . . H19A H 0.4818 0.4103 -0.0538 0.189 Uiso 1 1 calc R . . H19B H 0.6034 0.3600 -0.0488 0.189 Uiso 1 1 calc R . . C20 C 0.4593(14) 0.2950(8) -0.0171(8) 0.129(6) Uani 1 1 d . . . H20A H 0.5050 0.2520 -0.0490 0.155 Uiso 1 1 calc R . . H20B H 0.3833 0.3023 -0.0522 0.155 Uiso 1 1 calc R . . C31 C 0.4147(13) 0.0167(14) 0.4837(14) 0.072(3) Uiso 0.25 1 d PGD A -1 C32 C 0.4431(17) -0.0653(14) 0.5021(15) 0.072(3) Uiso 0.25 1 d PGD A -1 H32 H 0.3828 -0.1051 0.4990 0.087 Uiso 0.25 1 calc PR A -1 C33 C 0.5044(18) 0.0767(13) 0.4918(15) 0.072(3) Uiso 0.25 1 d PGD A -1 H33 H 0.4847 0.1316 0.4818 0.087 Uiso 0.25 1 calc PR A -1 C34 C 0.2877(15) 0.040(2) 0.4554(15) 0.072(3) Uiso 0.25 1 d PGD A -1 H34A H 0.2835 0.0986 0.4455 0.108 Uiso 0.13 1 calc PR A -1 H34B H 0.2330 0.0249 0.5063 0.108 Uiso 0.13 1 calc PR A -1 H34C H 0.2652 0.0126 0.3962 0.108 Uiso 0.13 1 calc PR A -1 H34D H 0.2376 -0.0079 0.4531 0.108 Uiso 0.13 1 calc PR A -1 H34E H 0.2881 0.0658 0.3923 0.108 Uiso 0.13 1 calc PR A -1 H34F H 0.2560 0.0781 0.5024 0.108 Uiso 0.13 1 calc PR A -1 C31E C 0.6511(15) -0.0270(18) 0.5329(15) 0.072(3) Uiso 0.25 1 d PG A -1 H31 H 0.7299 -0.0417 0.5505 0.087 Uiso 0.25 1 calc PR A -1 C32E C 0.6227(16) 0.0549(17) 0.5146(16) 0.072(3) Uiso 0.25 1 d PG A -1 H32E H 0.6830 0.0948 0.5177 0.087 Uiso 0.25 1 calc PR A -1 C33E C 0.561(2) -0.0871(15) 0.5249(16) 0.072(3) Uiso 0.25 1 d PG A -1 H33E H 0.5811 -0.1419 0.5349 0.087 Uiso 0.25 1 calc PR A -1 C21 C 0.3367(13) -0.0085(18) 0.4726(15) 0.072(3) Uiso 0.25 1 d PGD B -2 H21 H 0.2550 -0.0148 0.4569 0.087 Uiso 0.25 1 calc PR B -2 C22 C 0.4065(18) -0.0769(14) 0.4974(16) 0.072(3) Uiso 0.25 1 d PGD B -2 H22 H 0.3709 -0.1285 0.5005 0.087 Uiso 0.25 1 calc PR B -2 C23 C 0.3894(18) 0.0692(15) 0.4712(15) 0.072(3) Uiso 0.25 1 d PGD B -2 H23 H 0.3421 0.1150 0.4568 0.087 Uiso 0.25 1 calc PR B -2 C23E C 0.5291(17) -0.0675(13) 0.5174(15) 0.072(3) Uiso 0.25 1 d PG B -2 H23E H 0.5764 -0.1133 0.5317 0.087 Uiso 0.25 1 calc PR B -2 C22E C 0.5121(18) 0.0786(13) 0.4911(15) 0.072(3) Uiso 0.25 1 d PG B -2 H22E H 0.5477 0.1302 0.4880 0.087 Uiso 0.25 1 calc PR B -2 C21E C 0.5819(13) 0.0102(14) 0.5160(14) 0.072(3) Uiso 0.25 1 d PG B -2 C24 C 0.7137(14) 0.020(2) 0.5413(17) 0.072(3) Uiso 0.25 1 d PGD B -2 H24A H 0.7354 0.0773 0.5369 0.108 Uiso 0.13 1 calc PR B -2 H24B H 0.7618 -0.0109 0.4967 0.108 Uiso 0.13 1 calc PR B -2 H24C H 0.7282 0.0012 0.6065 0.108 Uiso 0.13 1 calc PR B -2 H24D H 0.7482 -0.0322 0.5565 0.108 Uiso 0.13 1 calc PR B -2 H24E H 0.7218 0.0560 0.5967 0.108 Uiso 0.13 1 calc PR B -2 H24F H 0.7555 0.0438 0.4869 0.108 Uiso 0.13 1 calc PR B -2 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 0.0465(8) 0.0446(8) 0.0467(8) 0.0008(7) 0.0039(6) 0.0021(7) Cl1 0.0789(16) 0.0545(14) 0.0550(14) -0.0070(11) 0.0151(11) 0.0041(12) Cl2 0.0859(18) 0.0671(16) 0.0451(13) -0.0076(11) 0.0052(12) 0.0022(13) Cl3 0.0585(15) 0.0708(17) 0.097(2) 0.0093(15) -0.0107(13) 0.0065(13) O1 0.070(4) 0.059(4) 0.051(4) 0.001(3) 0.007(3) -0.012(3) N1 0.039(4) 0.045(4) 0.048(4) -0.006(3) 0.007(3) -0.001(3) N2 0.037(4) 0.050(4) 0.044(4) -0.001(3) 0.005(3) 0.004(3) C1 0.037(5) 0.052(5) 0.082(7) 0.004(5) 0.006(4) 0.001(4) C2 0.064(6) 0.086(8) 0.071(7) -0.038(6) 0.004(5) -0.035(6) C3 0.059(7) 0.127(11) 0.113(10) -0.048(9) 0.019(6) -0.035(7) C4 0.048(6) 0.090(9) 0.142(12) 0.014(8) 0.006(7) -0.020(6) C5 0.088(8) 0.061(7) 0.118(11) -0.006(7) -0.040(8) -0.022(6) C6 0.075(7) 0.084(7) 0.045(5) -0.011(5) -0.012(5) -0.024(6) C7 0.041(5) 0.045(5) 0.036(4) -0.003(4) -0.004(3) -0.002(4) C8 0.054(5) 0.028(4) 0.042(5) -0.002(3) 0.010(4) 0.001(4) C9 0.056(5) 0.043(5) 0.050(5) 0.003(4) 0.004(4) 0.005(4) C10 0.048(5) 0.048(5) 0.073(6) -0.005(5) 0.004(4) 0.001(4) C11 0.038(5) 0.068(6) 0.039(5) 0.006(4) -0.007(4) 0.001(4) C12 0.044(5) 0.071(6) 0.071(6) -0.011(5) 0.012(5) -0.004(5) C13 0.061(7) 0.092(8) 0.080(7) -0.003(6) 0.018(6) 0.007(6) C14 0.037(5) 0.099(9) 0.085(8) 0.022(7) -0.005(5) 0.004(6) C15 0.067(7) 0.090(8) 0.091(8) -0.024(7) -0.012(6) -0.022(6) C16 0.047(6) 0.095(8) 0.076(7) -0.032(6) 0.000(5) -0.016(5) C17 0.144(10) 0.042(6) 0.070(7) -0.003(5) 0.010(7) -0.019(6) C18 0.260(19) 0.098(10) 0.088(10) -0.002(8) 0.063(11) -0.091(12) C19 0.26(2) 0.119(12) 0.091(11) 0.008(9) 0.051(12) -0.105(13) C20 0.234(17) 0.095(10) 0.059(7) 0.012(7) 0.033(9) -0.070(11) _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 O1 2.123(6) . ? V1 N2 2.128(7) . ? V1 N1 2.132(7) . ? V1 Cl3 2.297(3) . ? V1 Cl1 2.324(3) . ? V1 Cl2 2.342(3) . ? O1 C17 1.412(10) . ? O1 C20 1.446(11) . ? N1 C7 1.284(9) . ? N1 C1 1.463(10) . ? N2 C8 1.287(9) . ? N2 C11 1.435(9) . ? C1 C6 1.374(12) . ? C1 C2 1.381(12) . ? C2 C3 1.370(13) . ? C2 H2 0.9300 . ? C3 C4 1.337(15) . ? C3 H3 0.9300 . ? C4 C5 1.376(16) . ? C4 H4 0.9300 . ? C5 C6 1.394(13) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.482(10) . ? C7 C9 1.482(10) . ? C8 C10 1.485(10) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C16 1.369(12) . ? C11 C12 1.386(11) . ? C12 C13 1.380(12) . ? C12 H12 0.9300 . ? C13 C14 1.382(14) . ? C13 H13 0.9300 . ? C14 C15 1.359(13) . ? C14 H14 0.9300 . ? C15 C16 1.390(12) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.493(14) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.486(16) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.406(15) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C31 C32 1.3948 . ? C31 C33 1.3949 . ? C31 C34 1.5002 . ? C32 C33E 1.3857 . ? C32 H32 0.9300 . ? C33 C32E 1.3858 . ? C33 H33 0.9300 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C34 H34D 0.9600 . ? C34 H34E 0.9600 . ? C34 H34F 0.9600 . ? C31E C32E 1.3946 . ? C31E C33E 1.3950 . ? C31E H31 0.9300 . ? C32E H32E 0.9300 . ? C33E H33E 0.9300 . ? C21 C23 1.3948 . ? C21 C22 1.3948 . ? C21 H21 0.9300 . ? C22 C23E 1.3857 . ? C22 H22 0.9300 . ? C23 C22E 1.3857 . ? C23 H23 0.9300 . ? C23E C21E 1.3947 . ? C23E H23E 0.9300 . ? C22E C21E 1.3949 . ? C22E H22E 0.9300 . ? C21E C24 1.5003 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C24 H24D 0.9600 . ? C24 H24E 0.9600 . ? C24 H24F 0.9600 . ? 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 O1 V1 N2 166.0(2) . . ? O1 V1 N1 91.8(2) . . ? N2 V1 N1 74.6(2) . . ? O1 V1 Cl3 91.00(19) . . ? N2 V1 Cl3 102.55(19) . . ? N1 V1 Cl3 177.2(2) . . ? O1 V1 Cl1 91.92(17) . . ? N2 V1 Cl1 90.53(18) . . ? N1 V1 Cl1 85.79(18) . . ? Cl3 V1 Cl1 94.46(11) . . ? O1 V1 Cl2 89.50(17) . . ? N2 V1 Cl2 85.97(18) . . ? N1 V1 Cl2 85.12(18) . . ? Cl3 V1 Cl2 94.57(11) . . ? Cl1 V1 Cl2 170.84(11) . . ? C17 O1 C20 106.2(7) . . ? C17 O1 V1 127.2(5) . . ? C20 O1 V1 124.8(6) . . ? C7 N1 C1 120.8(7) . . ? C7 N1 V1 117.5(5) . . ? C1 N1 V1 121.7(5) . . ? C8 N2 C11 121.7(7) . . ? C8 N2 V1 116.9(5) . . ? C11 N2 V1 121.1(5) . . ? C6 C1 C2 121.4(8) . . ? C6 C1 N1 121.5(8) . . ? C2 C1 N1 117.0(8) . . ? C3 C2 C1 118.4(9) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C4 C3 C2 121.2(11) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 121.3(10) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C4 C5 C6 119.1(11) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C1 C6 C5 118.6(10) . . ? C1 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? N1 C7 C8 114.9(7) . . ? N1 C7 C9 124.3(7) . . ? C8 C7 C9 120.8(7) . . ? N2 C8 C7 115.7(7) . . ? N2 C8 C10 125.3(7) . . ? C7 C8 C10 118.9(7) . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 119.3(8) . . ? C16 C11 N2 121.9(8) . . ? C12 C11 N2 118.8(8) . . ? C11 C12 C13 119.9(9) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 120.1(9) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 120.1(9) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 119.9(10) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C11 C16 C15 120.7(9) . . ? C11 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? O1 C17 C18 107.5(9) . . ? O1 C17 H17A 110.2 . . ? C18 C17 H17A 110.2 . . ? O1 C17 H17B 110.2 . . ? C18 C17 H17B 110.2 . . ? H17A C17 H17B 108.5 . . ? C17 C18 C19 102.5(10) . . ? C17 C18 H18A 111.3 . . ? C19 C18 H18A 111.3 . . ? C17 C18 H18B 111.3 . . ? C19 C18 H18B 111.3 . . ? H18A C18 H18B 109.2 . . ? C20 C19 C18 108.6(10) . . ? C20 C19 H19A 110.0 . . ? C18 C19 H19A 110.0 . . ? C20 C19 H19B 110.0 . . ? C18 C19 H19B 110.0 . . ? H19A C19 H19B 108.4 . . ? C19 C20 O1 108.7(10) . . ? C19 C20 H20A 109.9 . . ? O1 C20 H20A 109.9 . . ? C19 C20 H20B 109.9 . . ? O1 C20 H20B 109.9 . . ? H20A C20 H20B 108.3 . . ? C32 C31 C33 120.0 . . ? C32 C31 C34 120.0 . . ? C33 C31 C34 120.0 . . ? C33E C32 C31 119.7 . . ? C33E C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32E C33 C31 120.2 . . ? C32E C33 H33 119.9 . . ? C31 C33 H33 119.9 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C34 H34D 109.5 . . ? H34A C34 H34D 141.1 . . ? H34B C34 H34D 56.3 . . ? H34C C34 H34D 56.3 . . ? C31 C34 H34E 109.5 . . ? H34A C34 H34E 56.3 . . ? H34B C34 H34E 141.1 . . ? H34C C34 H34E 56.3 . . ? H34D C34 H34E 109.5 . . ? C31 C34 H34F 109.5 . . ? H34A C34 H34F 56.3 . . ? H34B C34 H34F 56.3 . . ? H34C C34 H34F 141.1 . . ? H34D C34 H34F 109.5 . . ? H34E C34 H34F 109.5 . . ? C32E C31E C33E 120.0 . . ? C32E C31E H31 120.0 . . ? C33E C31E H31 120.0 . . ? C33 C32E C31E 119.7 . . ? C33 C32E H32E 120.1 . . ? C31E C32E H32E 120.1 . . ? C32 C33E C31E 120.2 . . ? C32 C33E H33E 119.9 . . ? C31E C33E H33E 119.9 . . ? C23 C21 C22 120.0 . . ? C23 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23E C22 C21 119.7 . . ? C23E C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22E C23 C21 120.2 . . ? C22E C23 H23 119.9 . . ? C21 C23 H23 119.9 . . ? C22 C23E C21E 120.3 . . ? C22 C23E H23E 119.9 . . ? C21E C23E H23E 119.9 . . ? C23 C22E C21E 119.7 . . ? C23 C22E H22E 120.1 . . ? C21E C22E H22E 120.1 . . ? C23E C21E C22E 120.0 . . ? C23E C21E C24 120.0 . . ? C22E C21E C24 120.0 . . ? C21E C24 H24A 109.5 . . ? C21E C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21E C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21E C24 H24D 109.5 . . ? H24A C24 H24D 141.1 . . ? H24B C24 H24D 56.3 . . ? H24C C24 H24D 56.3 . . ? C21E C24 H24E 109.5 . . ? H24A C24 H24E 56.3 . . ? H24B C24 H24E 141.1 . . ? H24C C24 H24E 56.3 . . ? H24D C24 H24E 109.5 . . ? C21E C24 H24F 109.5 . . ? H24A C24 H24F 56.3 . . ? H24B C24 H24F 56.3 . . ? H24C C24 H24F 141.1 . . ? H24D C24 H24F 109.5 . . ? H24E C24 H24F 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.445 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.092