Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 # 1. SUBMISSION DETAILS _publ_contact_author ; Myoung Soo Lah ; _publ_contact_author_phone '82 31 400 5496' _publ_contact_author_fax '82 31 407 3863' _publ_contact_author_email mslah@hanyang.ac.kr _publ_requested_journal 'Dalton Transactions' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication in "Dalton Transactions". Myoung Soo Lah ; #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Linear Trinuclear Mixed Valence Vanadium(V/IV/V) Complex: Synthesis, Characterization and Solution Behavior ; loop_ _publ_author_name _publ_author_address 'Lah, Myoung Soo' ; Department of Chemistry College of Science Hanyang University Ansan, Kyunggi-do 425-791 Korea ; 'Jin, Yinshi' ; Department of Chemistry College of Science Hanyang University Ansan, Kyunggi-do 425-791 Korea ; 'Lee, Hongin' ; Department of Chemistry Education Kyungpook National University Daegu 702-701 Korea ; 'Pyo, Myungho' ; Department of Chemistry College of Science Sunchon National University Sunchon 540-742 Korea ; data_l03_25tr _database_code_depnum_ccdc_archive 'CCDC 249323' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H40 N4 O11 V3' _chemical_formula_weight 785.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.407(2) _cell_length_b 14.364(4) _cell_length_c 14.709(4) _cell_angle_alpha 65.655(4) _cell_angle_beta 89.823(4) _cell_angle_gamma 75.980(4) _cell_volume 1746.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6121 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.52 _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 810 _exptl_absorpt_coefficient_mu 0.848 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7849 _exptl_absorpt_correction_T_max 0.9750 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2.0 _diffrn_reflns_number 34223 _diffrn_reflns_av_R_equivalents 0.1038 _diffrn_reflns_av_sigmaI/netI 0.1227 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.41 _reflns_number_total 8352 _reflns_number_gt 3812 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics ORTEP3 _computing_publication_material WinGX _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^)+(0.0612P)^2^+7.5753P] 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 8352 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1797 _refine_ls_R_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.2243 _refine_ls_wR_factor_gt 0.1777 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.72749(13) -0.06598(10) 0.72778(8) 0.0382(3) Uani 1 1 d . . . V2 V 0.56589(12) 0.17653(9) 0.37674(8) 0.0340(3) Uani 1 1 d . . . V3 V 0.61842(14) 0.49310(9) 0.09698(8) 0.0416(3) Uani 1 1 d . . . O1 O 0.8228(5) -0.0008(4) 0.7519(3) 0.0468(12) Uani 1 1 d . . . O2 O 0.8633(5) -0.1671(4) 0.7068(3) 0.0428(12) Uani 1 1 d . . . O3 O 0.7454(5) 0.0615(3) 0.4105(3) 0.0340(10) Uani 1 1 d . . . O4 O 0.5362(5) 0.0414(4) 0.6926(3) 0.0421(12) Uani 1 1 d . . . O5 O 0.6751(5) -0.1372(4) 0.8455(3) 0.0485(13) Uani 1 1 d . . . O6 O 0.7583(6) 0.5163(4) 0.1305(4) 0.0519(13) Uani 1 1 d . . . O7 O 0.4715(6) 0.5853(4) 0.1244(3) 0.0480(13) Uani 1 1 d . . . O8 O 0.4976(5) 0.3131(4) 0.3838(3) 0.0385(11) Uani 1 1 d . . . O9 O 0.7163(5) 0.3535(4) 0.1013(3) 0.0450(12) Uani 1 1 d . . . O10 O 0.6004(5) 0.5525(4) -0.0355(3) 0.0434(12) Uani 1 1 d . . . O11 O 0.4362(5) 0.1503(4) 0.3313(3) 0.0382(11) Uani 1 1 d . . . N1 N 0.7009(6) 0.0115(4) 0.5742(4) 0.0337(12) Uani 1 1 d . . . N2 N 0.5773(6) 0.0999(4) 0.5301(4) 0.0360(13) Uani 1 1 d . . . N3 N 0.5793(6) 0.3836(4) 0.2314(4) 0.0362(13) Uani 1 1 d . . . N4 N 0.6373(6) 0.2764(4) 0.2516(4) 0.0345(12) Uani 1 1 d . . . C1 C 0.9373(7) -0.1771(5) 0.6310(5) 0.0349(15) Uani 1 1 d . . . C2 C 1.0479(8) -0.2696(5) 0.6517(5) 0.0409(16) Uani 1 1 d . . . H2 H 1.0682 -0.3251 0.7176 0.049 Uiso 1 1 calc R . . C3 C 1.1277(7) -0.2807(5) 0.5764(5) 0.0400(16) Uani 1 1 d . . . H3 H 1.2032 -0.3439 0.5910 0.048 Uiso 1 1 calc R . . C4 C 1.0996(7) -0.2013(5) 0.4804(5) 0.0397(16) Uani 1 1 d . . . H4 H 1.1564 -0.2093 0.4293 0.048 Uiso 1 1 calc R . . C5 C 0.9897(7) -0.1106(5) 0.4586(5) 0.0348(15) Uani 1 1 d . . . H5 H 0.9711 -0.0558 0.3924 0.042 Uiso 1 1 calc R . . C6 C 0.9040(7) -0.0978(5) 0.5331(5) 0.0315(14) Uani 1 1 d . . . C7 C 0.7792(7) -0.0042(5) 0.5047(5) 0.0321(14) Uani 1 1 d . . . C8 C 0.4953(7) 0.1056(6) 0.6017(5) 0.0382(16) Uani 1 1 d . . . C9 C 0.3508(7) 0.1883(6) 0.5764(5) 0.0433(17) Uani 1 1 d . . . H9A H 0.2697 0.1532 0.5924 0.052 Uiso 1 1 calc R . . H9B H 0.3366 0.2346 0.5035 0.052 Uiso 1 1 calc R . . C10 C 0.3441(8) 0.2552(6) 0.6337(6) 0.0471(18) Uani 1 1 d . . . H10A H 0.4202 0.2947 0.6131 0.056 Uiso 1 1 calc R . . H10B H 0.3680 0.2079 0.7062 0.056 Uiso 1 1 calc R . . C11 C 0.1954(8) 0.3336(6) 0.6176(6) 0.053(2) Uani 1 1 d . . . H11A H 0.1744 0.3834 0.5457 0.063 Uiso 1 1 calc R . . H11B H 0.1186 0.2945 0.6342 0.063 Uiso 1 1 calc R . . C12 C 0.1846(9) 0.3963(7) 0.6788(7) 0.059(2) Uani 1 1 d . . . H12A H 0.2527 0.4422 0.6561 0.070 Uiso 1 1 calc R . . H12B H 0.2179 0.3465 0.7499 0.070 Uiso 1 1 calc R . . C13 C 0.0324(10) 0.4644(8) 0.6728(8) 0.079(3) Uani 1 1 d . . . H13A H -0.0006 0.5157 0.6030 0.119 Uiso 1 1 calc R . . H13B H 0.0346 0.5023 0.7148 0.119 Uiso 1 1 calc R . . H13C H -0.0358 0.4196 0.6966 0.119 Uiso 1 1 calc R . . C14 C 0.6665(15) -0.1115(11) 0.9315(7) 0.123(6) Uani 1 1 d . . . H14A H 0.7546 -0.0880 0.9391 0.148 Uiso 1 1 calc R . . H14B H 0.5789 -0.0513 0.9179 0.148 Uiso 1 1 calc R . . C15 C 0.6575(14) -0.1941(10) 1.0209(8) 0.112(4) Uani 1 1 d . . . H15A H 0.5864 -0.2293 1.0101 0.168 Uiso 1 1 calc R . . H15B H 0.6253 -0.1665 1.0705 0.168 Uiso 1 1 calc R . . H15C H 0.7546 -0.2451 1.0455 0.168 Uiso 1 1 calc R . . C16 C 0.4305(8) 0.5918(6) 0.2102(5) 0.0408(16) Uani 1 1 d . . . C17 C 0.3666(8) 0.6917(6) 0.2069(5) 0.0460(18) Uani 1 1 d . . . H17 H 0.3570 0.7535 0.1461 0.055 Uiso 1 1 calc R . . C18 C 0.3180(8) 0.7003(6) 0.2915(6) 0.052(2) Uani 1 1 d . . . H18 H 0.2732 0.7683 0.2889 0.062 Uiso 1 1 calc R . . C19 C 0.3332(9) 0.6109(6) 0.3810(6) 0.054(2) Uani 1 1 d . . . H19 H 0.3018 0.6176 0.4400 0.064 Uiso 1 1 calc R . . C20 C 0.3941(8) 0.5128(6) 0.3836(5) 0.0447(17) Uani 1 1 d . . . H20 H 0.4020 0.4515 0.4445 0.054 Uiso 1 1 calc R . . C21 C 0.4442(7) 0.5010(5) 0.2994(5) 0.0382(16) Uani 1 1 d . . . C22 C 0.5091(7) 0.3948(5) 0.3053(5) 0.0334(14) Uani 1 1 d . . . C23 C 0.7094(7) 0.2693(5) 0.1772(5) 0.0393(16) Uani 1 1 d . . . C24 C 0.7891(9) 0.1658(6) 0.1778(5) 0.0473(18) Uani 1 1 d . . . H24A H 0.8955 0.1620 0.1759 0.057 Uiso 1 1 calc R . . H24B H 0.7775 0.1079 0.2413 0.057 Uiso 1 1 calc R . . C25 C 0.7366(12) 0.1498(7) 0.0936(7) 0.085(3) Uani 1 1 d . . . H25A H 0.7287 0.2147 0.0312 0.102 Uiso 1 1 calc R . . H25B H 0.6365 0.1392 0.1032 0.102 Uiso 1 1 calc R . . C26 C 0.8352(13) 0.0556(7) 0.0807(6) 0.085(3) Uani 1 1 d . . . H26A H 0.7959 0.0539 0.0192 0.102 Uiso 1 1 calc R . . H26B H 0.9349 0.0667 0.0706 0.102 Uiso 1 1 calc R . . C27 C 0.8483(11) -0.0478(7) 0.1653(8) 0.074(3) Uani 1 1 d . . . H27A H 0.7493 -0.0605 0.1741 0.089 Uiso 1 1 calc R . . H27B H 0.8849 -0.0459 0.2274 0.089 Uiso 1 1 calc R . . C28 C 0.9518(10) -0.1402(7) 0.1516(7) 0.075(3) Uani 1 1 d . . . H28A H 0.9112 -0.1472 0.0941 0.113 Uiso 1 1 calc R . . H28B H 0.9614 -0.2058 0.2124 0.113 Uiso 1 1 calc R . . H28C H 1.0489 -0.1267 0.1395 0.113 Uiso 1 1 calc R . . C29 C 0.7109(10) 0.6022(7) -0.0954(6) 0.063(2) Uani 1 1 d . . . H29A H 0.7570 0.6340 -0.0591 0.075 Uiso 1 1 calc R . . H29B H 0.6612 0.6595 -0.1605 0.075 Uiso 1 1 calc R . . C30 C 0.8266(10) 0.5228(9) -0.1135(8) 0.085(3) Uani 1 1 d . . . H30A H 0.8952 0.4790 -0.0524 0.128 Uiso 1 1 calc R . . H30B H 0.8805 0.5593 -0.1684 0.128 Uiso 1 1 calc R . . H30C H 0.7806 0.4776 -0.1317 0.128 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 0.0396(7) 0.0429(7) 0.0279(6) -0.0123(5) 0.0044(5) -0.0085(5) V2 0.0345(6) 0.0332(6) 0.0301(6) -0.0122(5) 0.0028(5) -0.0038(5) V3 0.0517(7) 0.0356(7) 0.0281(6) -0.0089(5) 0.0032(5) -0.0032(6) O1 0.050(3) 0.057(3) 0.037(3) -0.018(2) 0.003(2) -0.023(3) O2 0.041(3) 0.049(3) 0.027(2) -0.010(2) 0.002(2) -0.003(2) O3 0.040(3) 0.032(2) 0.025(2) -0.0095(19) 0.0044(19) -0.008(2) O4 0.049(3) 0.045(3) 0.027(2) -0.013(2) 0.007(2) -0.005(2) O5 0.050(3) 0.063(3) 0.033(3) -0.021(2) 0.004(2) -0.015(3) O6 0.057(3) 0.051(3) 0.044(3) -0.014(3) 0.013(2) -0.019(3) O7 0.067(3) 0.038(3) 0.028(2) -0.008(2) 0.006(2) -0.006(2) O8 0.039(3) 0.037(3) 0.033(2) -0.011(2) 0.009(2) -0.005(2) O9 0.056(3) 0.041(3) 0.028(2) -0.011(2) 0.008(2) -0.002(2) O10 0.052(3) 0.040(3) 0.029(2) -0.010(2) 0.008(2) -0.004(2) O11 0.038(3) 0.043(3) 0.036(3) -0.016(2) -0.001(2) -0.016(2) N1 0.032(3) 0.033(3) 0.034(3) -0.014(2) 0.005(2) -0.004(2) N2 0.034(3) 0.037(3) 0.035(3) -0.017(3) 0.004(2) -0.003(2) N3 0.045(3) 0.032(3) 0.024(3) -0.011(2) -0.003(2) 0.002(2) N4 0.032(3) 0.032(3) 0.032(3) -0.012(2) -0.001(2) 0.003(2) C1 0.029(3) 0.037(4) 0.030(3) -0.006(3) -0.001(3) -0.007(3) C2 0.048(4) 0.030(4) 0.033(4) -0.006(3) -0.003(3) -0.003(3) C3 0.041(4) 0.030(4) 0.044(4) -0.016(3) -0.006(3) 0.000(3) C4 0.040(4) 0.032(4) 0.045(4) -0.019(3) 0.007(3) -0.001(3) C5 0.033(3) 0.030(4) 0.037(4) -0.010(3) 0.005(3) -0.007(3) C6 0.029(3) 0.030(3) 0.034(3) -0.014(3) 0.004(3) -0.005(3) C7 0.031(3) 0.034(4) 0.030(3) -0.014(3) 0.004(3) -0.007(3) C8 0.041(4) 0.045(4) 0.036(4) -0.024(3) 0.009(3) -0.012(3) C9 0.037(4) 0.050(5) 0.049(4) -0.027(4) 0.012(3) -0.010(3) C10 0.043(4) 0.040(4) 0.058(5) -0.024(4) 0.008(4) -0.007(3) C11 0.052(5) 0.052(5) 0.062(5) -0.035(4) 0.006(4) -0.009(4) C12 0.058(5) 0.056(5) 0.068(6) -0.034(5) 0.008(4) -0.011(4) C13 0.074(7) 0.071(7) 0.101(8) -0.053(6) 0.009(6) -0.004(5) C14 0.182(13) 0.199(14) 0.039(5) -0.044(7) 0.028(7) -0.151(12) C15 0.122(10) 0.134(11) 0.070(7) -0.023(7) 0.022(7) -0.051(9) C16 0.048(4) 0.042(4) 0.029(3) -0.017(3) -0.002(3) 0.000(3) C17 0.053(4) 0.034(4) 0.038(4) -0.010(3) 0.000(3) 0.001(3) C18 0.055(5) 0.046(5) 0.053(5) -0.028(4) 0.003(4) 0.001(4) C19 0.056(5) 0.047(5) 0.055(5) -0.025(4) 0.012(4) -0.004(4) C20 0.051(4) 0.043(4) 0.042(4) -0.022(3) 0.010(3) -0.007(3) C21 0.035(4) 0.041(4) 0.035(4) -0.016(3) 0.000(3) -0.004(3) C22 0.034(3) 0.040(4) 0.026(3) -0.017(3) 0.000(3) -0.004(3) C23 0.043(4) 0.037(4) 0.026(3) -0.008(3) 0.003(3) 0.000(3) C24 0.060(5) 0.038(4) 0.034(4) -0.014(3) 0.003(3) 0.000(4) C25 0.112(8) 0.051(6) 0.078(7) -0.033(5) -0.041(6) 0.012(5) C26 0.144(10) 0.061(6) 0.040(5) -0.022(5) 0.003(5) -0.008(6) C27 0.087(7) 0.054(6) 0.088(7) -0.040(5) 0.016(6) -0.011(5) C28 0.073(6) 0.067(6) 0.085(7) -0.037(6) 0.010(5) -0.006(5) C29 0.073(6) 0.070(6) 0.041(5) -0.013(4) 0.015(4) -0.031(5) C30 0.063(6) 0.132(10) 0.093(8) -0.071(7) 0.038(5) -0.041(6) _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 1.577(5) . ? V1 O5 1.750(5) . ? V1 O2 1.818(5) . ? V1 O4 1.972(5) . ? V1 N1 2.049(5) . ? V2 O11 1.585(4) . ? V2 O3 1.950(4) . ? V2 O8 1.957(5) . ? V2 N4 2.045(5) . ? V2 N2 2.051(5) . ? V3 O6 1.561(5) . ? V3 O10 1.765(4) . ? V3 O7 1.837(5) . ? V3 O9 1.967(5) . ? V3 N3 2.057(5) . ? O2 C1 1.351(7) . ? O3 C7 1.300(7) . ? O4 C8 1.265(8) . ? O5 C14 1.454(11) . ? O7 C16 1.351(7) . ? O8 C22 1.291(7) . ? O9 C23 1.279(7) . ? O10 C29 1.483(9) . ? N1 C7 1.321(7) . ? N1 N2 1.412(7) . ? N2 C8 1.322(8) . ? N3 C22 1.316(7) . ? N3 N4 1.405(7) . ? N4 C23 1.312(8) . ? C1 C2 1.393(9) . ? C1 C6 1.396(8) . ? C2 C3 1.377(9) . ? C3 C4 1.376(9) . ? C4 C5 1.368(9) . ? C5 C6 1.404(8) . ? C6 C7 1.462(8) . ? C8 C9 1.501(9) . ? C9 C10 1.509(10) . ? C10 C11 1.516(10) . ? C11 C12 1.501(10) . ? C12 C13 1.505(11) . ? C14 C15 1.380(13) . ? C16 C21 1.396(9) . ? C16 C17 1.396(10) . ? C17 C18 1.367(10) . ? C18 C19 1.386(10) . ? C19 C20 1.372(10) . ? C20 C21 1.383(9) . ? C21 C22 1.465(9) . ? C23 C24 1.490(9) . ? C24 C25 1.458(11) . ? C25 C26 1.526(12) . ? C26 C27 1.469(12) . ? C27 C28 1.530(11) . ? C29 C30 1.485(12) . ? 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 O5 102.4(2) . . ? O1 V1 O2 103.8(2) . . ? O5 V1 O2 103.1(2) . . ? O1 V1 O4 97.5(2) . . ? O5 V1 O4 90.3(2) . . ? O2 V1 O4 151.7(2) . . ? O1 V1 N1 99.2(2) . . ? O5 V1 N1 154.8(2) . . ? O2 V1 N1 83.9(2) . . ? O4 V1 N1 74.24(19) . . ? O11 V2 O3 110.1(2) . . ? O11 V2 O8 110.8(2) . . ? O3 V2 O8 139.09(19) . . ? O11 V2 N4 102.8(2) . . ? O3 V2 N4 94.23(19) . . ? O8 V2 N4 77.53(19) . . ? O11 V2 N2 107.3(2) . . ? O3 V2 N2 77.33(19) . . ? O8 V2 N2 90.0(2) . . ? N4 V2 N2 149.9(2) . . ? O6 V3 O10 105.6(2) . . ? O6 V3 O7 101.0(3) . . ? O10 V3 O7 102.0(2) . . ? O6 V3 O9 97.2(3) . . ? O10 V3 O9 91.5(2) . . ? O7 V3 O9 153.4(2) . . ? O6 V3 N3 100.9(2) . . ? O10 V3 N3 151.3(2) . . ? O7 V3 N3 83.3(2) . . ? O9 V3 N3 74.3(2) . . ? C1 O2 V1 138.2(4) . . ? C7 O3 V2 116.8(4) . . ? C8 O4 V1 119.3(4) . . ? C14 O5 V1 127.7(5) . . ? C16 O7 V3 133.4(4) . . ? C22 O8 V2 115.8(4) . . ? C23 O9 V3 119.7(4) . . ? C29 O10 V3 123.5(5) . . ? C7 N1 N2 110.7(5) . . ? C7 N1 V1 132.4(4) . . ? N2 N1 V1 116.9(4) . . ? C8 N2 N1 108.2(5) . . ? C8 N2 V2 137.7(5) . . ? N1 N2 V2 114.0(4) . . ? C22 N3 N4 111.8(5) . . ? C22 N3 V3 131.6(5) . . ? N4 N3 V3 116.5(4) . . ? C23 N4 N3 109.6(5) . . ? C23 N4 V2 137.2(5) . . ? N3 N4 V2 112.7(4) . . ? O2 C1 C2 118.8(6) . . ? O2 C1 C6 121.6(6) . . ? C2 C1 C6 119.6(6) . . ? C3 C2 C1 120.0(6) . . ? C4 C3 C2 120.8(6) . . ? C5 C4 C3 119.9(6) . . ? C4 C5 C6 120.7(6) . . ? C1 C6 C5 118.8(6) . . ? C1 C6 C7 122.2(6) . . ? C5 C6 C7 118.9(6) . . ? O3 C7 N1 121.0(6) . . ? O3 C7 C6 119.1(5) . . ? N1 C7 C6 119.9(6) . . ? O4 C8 N2 120.9(6) . . ? O4 C8 C9 118.7(6) . . ? N2 C8 C9 120.4(6) . . ? C8 C9 C10 111.8(6) . . ? C9 C10 C11 113.8(6) . . ? C12 C11 C10 114.3(7) . . ? C11 C12 C13 114.5(7) . . ? C15 C14 O5 114.4(11) . . ? O7 C16 C21 121.4(6) . . ? O7 C16 C17 118.5(6) . . ? C21 C16 C17 120.1(6) . . ? C18 C17 C16 119.8(7) . . ? C17 C18 C19 120.7(7) . . ? C20 C19 C18 119.4(7) . . ? C19 C20 C21 121.5(7) . . ? C20 C21 C16 118.5(6) . . ? C20 C21 C22 119.8(6) . . ? C16 C21 C22 121.6(6) . . ? O8 C22 N3 120.8(6) . . ? O8 C22 C21 119.3(5) . . ? N3 C22 C21 119.9(6) . . ? O9 C23 N4 119.9(6) . . ? O9 C23 C24 117.4(6) . . ? N4 C23 C24 122.6(6) . . ? C25 C24 C23 113.1(7) . . ? C24 C25 C26 114.0(8) . . ? C27 C26 C25 114.8(8) . . ? C26 C27 C28 113.5(8) . . ? O10 C29 C30 110.9(7) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 28.41 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.716 _refine_diff_density_min -0.922 _refine_diff_density_rms 0.117