Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_amt182 _database_code_CSD 167901 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Alonso, Pablo J.' 'Fornies, Juan' 'Garcia-Monforte, M. Angeles' 'Martin, Antonio' 'Menjon, Babil' _publ_contact_author_name 'Prof Juan Fornies' _publ_contact_author_address ; Instituto de Ciencia de Materiales de Aragon Universidad de Zaragoza - C.S.I.C Facultad de Ciencias Pza. S. Francisco S/n E-50009 Zaragoza SPAIN ; _publ_contact_author_email 'FORNIESJ@POSTA.UNIZAR.ES' _publ_section_title ; The first structurally characterised homoleptic organovanadium(III) compounds ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H36 Cl20 N V' _chemical_formula_weight 1290.64 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' 'Cl' 'Cl' 0.1484 0.1585 '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 ? _symmetry_space_group_name_H-M ? 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 19.3800(10) _cell_length_b 21.2586(13) _cell_length_c 25.9052(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10672.7(10) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5168 _exptl_absorpt_coefficient_mu 1.219 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6222 _exptl_absorpt_correction_T_max 0.7265 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9361 _diffrn_reflns_av_R_equivalents 0.0031 _diffrn_reflns_av_sigmaI/netI 0.0983 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 24.97 _reflns_number_total 9358 _reflns_number_gt 5228 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+10.8388P] 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 9358 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1468 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1398 _refine_ls_wR_factor_gt 0.1128 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V V 0.33778(5) 0.10762(4) 0.32656(4) 0.0321(2) Uani 1 d . . . Cl1 Cl 0.29224(9) -0.01266(8) 0.42089(6) 0.0552(4) Uani 1 d . . . Cl2 Cl 0.18933(10) -0.12073(8) 0.39825(7) 0.0732(6) Uani 1 d . . . Cl3 Cl 0.10725(10) -0.12367(9) 0.29578(8) 0.0800(6) Uani 1 d . . . Cl4 Cl 0.12353(10) -0.01370(9) 0.21657(8) 0.0795(6) Uani 1 d . . . Cl5 Cl 0.23316(9) 0.09020(7) 0.23636(5) 0.0518(4) Uani 1 d . . . Cl6 Cl 0.44589(8) 0.21201(7) 0.30253(7) 0.0576(5) Uani 1 d . . . Cl7 Cl 0.57004(10) 0.21242(10) 0.22658(8) 0.0854(7) Uani 1 d . . . Cl8 Cl 0.58621(9) 0.10394(11) 0.14673(7) 0.0825(6) Uani 1 d . . . Cl9 Cl 0.48576(9) -0.00959(9) 0.14963(7) 0.0676(5) Uani 1 d . . . Cl10 Cl 0.36833(9) -0.01435(7) 0.22932(6) 0.0541(4) Uani 1 d . . . Cl11 Cl 0.38346(9) 0.22703(7) 0.42263(7) 0.0633(5) Uani 1 d . . . Cl12 Cl 0.49676(9) 0.20989(9) 0.50427(7) 0.0716(6) Uani 1 d . . . Cl13 Cl 0.58597(9) 0.08908(9) 0.50684(7) 0.0709(6) Uani 1 d . . . Cl14 Cl 0.56111(9) -0.01587(8) 0.42490(8) 0.0706(5) Uani 1 d . . . Cl15 Cl 0.43930(8) -0.00431(7) 0.34787(6) 0.0484(4) Uani 1 d . . . Cl16 Cl 0.24265(8) 0.13567(8) 0.41744(6) 0.0525(4) Uani 1 d . . . Cl17 Cl 0.14688(10) 0.24973(10) 0.43965(8) 0.0895(7) Uani 1 d . . . Cl18 Cl 0.12582(10) 0.35241(8) 0.35547(9) 0.0857(7) Uani 1 d . . . Cl19 Cl 0.20331(11) 0.34169(8) 0.25084(8) 0.0793(6) Uani 1 d . . . Cl20 Cl 0.30326(9) 0.23238(7) 0.23133(6) 0.0553(4) Uani 1 d . . . C1 C 0.2632(3) 0.0331(2) 0.3256(2) 0.0330(13) Uani 1 d . . . C2 C 0.2495(3) -0.0138(3) 0.3616(2) 0.0366(13) Uani 1 d . . . C3 C 0.2018(3) -0.0617(3) 0.3534(2) 0.0440(15) Uani 1 d . . . C4 C 0.1642(3) -0.0631(3) 0.3077(3) 0.0480(16) Uani 1 d . . . C5 C 0.1737(3) -0.0154(3) 0.2720(2) 0.0448(15) Uani 1 d . . . C6 C 0.2216(3) 0.0309(3) 0.2821(2) 0.0395(14) Uani 1 d . . . C7 C 0.4096(3) 0.1008(2) 0.2631(2) 0.0356(14) Uani 1 d . . . C8 C 0.4568(3) 0.1497(3) 0.2601(2) 0.0430(15) Uani 1 d . . . C9 C 0.5123(3) 0.1504(3) 0.2258(3) 0.0496(17) Uani 1 d . . . C10 C 0.5199(3) 0.1020(3) 0.1912(2) 0.0477(16) Uani 1 d . . . C11 C 0.4744(3) 0.0517(3) 0.1919(2) 0.0454(16) Uani 1 d . . . C12 C 0.4211(3) 0.0521(3) 0.2281(2) 0.0378(14) Uani 1 d . . . C13 C 0.4116(3) 0.1086(3) 0.3886(2) 0.0370(14) Uani 1 d . . . C14 C 0.4278(3) 0.1554(3) 0.4242(2) 0.0428(15) Uani 1 d . . . C15 C 0.4799(3) 0.1503(3) 0.4609(2) 0.0443(15) Uani 1 d . . . C16 C 0.5203(3) 0.0966(3) 0.4622(2) 0.0433(15) Uani 1 d . . . C17 C 0.5084(3) 0.0496(3) 0.4265(2) 0.0427(15) Uani 1 d . . . C18 C 0.4545(3) 0.0563(2) 0.3917(2) 0.0382(14) Uani 1 d . . . C19 C 0.2721(3) 0.1887(2) 0.3269(2) 0.0313(13) Uani 1 d . . . C20 C 0.2339(3) 0.1952(2) 0.3715(2) 0.0368(14) Uani 1 d . . . C21 C 0.1903(3) 0.2455(3) 0.3815(3) 0.0473(16) Uani 1 d . . . C22 C 0.1812(3) 0.2905(3) 0.3444(3) 0.0510(18) Uani 1 d . . . C23 C 0.2162(3) 0.2858(3) 0.2979(3) 0.0480(16) Uani 1 d . . . C24 C 0.2608(3) 0.2357(3) 0.2907(2) 0.0394(14) Uani 1 d . . . N N 0.8289(3) 0.1305(2) 0.42522(18) 0.0500(13) Uani 1 d . . . C25 C 0.7607(3) 0.1619(3) 0.4390(2) 0.0599(19) Uani 1 d . . . H25A H 0.7398 0.1388 0.4672 0.072 Uiso 1 calc R . . H25B H 0.7703 0.2041 0.4513 0.072 Uiso 1 calc R . . C26 C 0.7090(4) 0.1663(4) 0.3955(3) 0.076(2) Uani 1 d . . . H26A H 0.6870 0.1258 0.3902 0.091 Uiso 1 calc R . . H26B H 0.7322 0.1781 0.3637 0.091 Uiso 1 calc R . . C27 C 0.6542(4) 0.2164(5) 0.4099(3) 0.119(4) Uani 1 d . . . H27A H 0.6291 0.2020 0.4400 0.143 Uiso 1 calc R . . H27B H 0.6777 0.2551 0.4192 0.143 Uiso 1 calc R . . C28 C 0.6083(6) 0.2291(7) 0.3718(4) 0.217(8) Uani 1 d . . . H28A H 0.5759 0.2602 0.3836 0.325 Uiso 1 calc R . . H28B H 0.5840 0.1913 0.3627 0.325 Uiso 1 calc R . . H28C H 0.6324 0.2449 0.3421 0.325 Uiso 1 calc R . . C29 C 0.8712(4) 0.1290(3) 0.4747(2) 0.0614(19) Uani 1 d . . . H29A H 0.8705 0.1707 0.4898 0.074 Uiso 1 calc R . . H29B H 0.8485 0.1009 0.4988 0.074 Uiso 1 calc R . . C30 C 0.9454(4) 0.1085(4) 0.4696(3) 0.075(2) Uani 1 d . . . H30A H 0.9701 0.1385 0.4483 0.091 Uiso 1 calc R . . H30B H 0.9472 0.0679 0.4526 0.091 Uiso 1 calc R . . C31 C 0.9803(4) 0.1040(4) 0.5219(3) 0.088(3) Uani 1 d . . . H31A H 0.9727 0.1428 0.5407 0.106 Uiso 1 calc R . . H31B H 0.9592 0.0701 0.5414 0.106 Uiso 1 calc R . . C32 C 1.0556(5) 0.0923(5) 0.5181(4) 0.128(4) Uani 1 d . . . H32A H 1.0750 0.0902 0.5522 0.192 Uiso 1 calc R . . H32B H 1.0770 0.1260 0.4993 0.192 Uiso 1 calc R . . H32C H 1.0636 0.0533 0.5005 0.192 Uiso 1 calc R . . C33 C 0.8176(3) 0.0645(3) 0.4039(2) 0.0522(17) Uani 1 d . . . H33A H 0.7909 0.0681 0.3723 0.063 Uiso 1 calc R . . H33B H 0.8623 0.0473 0.3946 0.063 Uiso 1 calc R . . C34 C 0.7818(4) 0.0179(3) 0.4386(3) 0.065(2) Uani 1 d . . . H34A H 0.7387 0.0356 0.4511 0.078 Uiso 1 calc R . . H34B H 0.8107 0.0087 0.4683 0.078 Uiso 1 calc R . . C35 C 0.7673(4) -0.0426(3) 0.4088(3) 0.081(2) Uani 1 d . . . H35A H 0.7353 -0.0337 0.3809 0.097 Uiso 1 calc R . . H35B H 0.8099 -0.0579 0.3937 0.097 Uiso 1 calc R . . C36 C 0.7373(5) -0.0928(4) 0.4430(4) 0.113(3) Uani 1 d . . . H36A H 0.7287 -0.1300 0.4230 0.169 Uiso 1 calc R . . H36B H 0.6948 -0.0781 0.4577 0.169 Uiso 1 calc R . . H36C H 0.7693 -0.1024 0.4702 0.169 Uiso 1 calc R . . C37 C 0.8666(3) 0.1672(3) 0.3839(2) 0.0519(17) Uani 1 d . . . H37A H 0.8424 0.1612 0.3514 0.062 Uiso 1 calc R . . H37B H 0.9123 0.1493 0.3799 0.062 Uiso 1 calc R . . C38 C 0.8742(3) 0.2372(3) 0.3931(2) 0.0574(18) Uani 1 d . . . H38A H 0.8850 0.2446 0.4291 0.069 Uiso 1 calc R . . H38B H 0.8308 0.2580 0.3855 0.069 Uiso 1 calc R . . C39 C 0.9306(3) 0.2651(3) 0.3596(2) 0.0593(19) Uani 1 d . . . H39A H 0.9750 0.2507 0.3722 0.071 Uiso 1 calc R . . H39B H 0.9252 0.2496 0.3246 0.071 Uiso 1 calc R . . C40 C 0.9304(4) 0.3359(3) 0.3586(3) 0.093(3) Uani 1 d . . . H40A H 0.9672 0.3507 0.3369 0.140 Uiso 1 calc R . . H40B H 0.9368 0.3517 0.3930 0.140 Uiso 1 calc R . . H40C H 0.8871 0.3506 0.3453 0.140 Uiso 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 V 0.0280(5) 0.0326(5) 0.0358(5) -0.0052(4) -0.0019(5) 0.0011(4) Cl1 0.0692(11) 0.0584(10) 0.0380(9) 0.0082(8) -0.0021(8) 0.0072(9) Cl2 0.0908(14) 0.0525(11) 0.0763(13) 0.0134(10) 0.0352(11) -0.0071(10) Cl3 0.0628(12) 0.0582(11) 0.1190(17) -0.0227(11) 0.0114(12) -0.0272(10) Cl4 0.0774(14) 0.0829(14) 0.0783(13) -0.0166(11) -0.0349(11) -0.0171(11) Cl5 0.0661(11) 0.0501(9) 0.0393(9) 0.0037(7) -0.0045(8) -0.0052(8) Cl6 0.0540(10) 0.0394(9) 0.0793(12) -0.0025(9) -0.0022(9) -0.0092(8) Cl7 0.0593(12) 0.0993(16) 0.0975(16) 0.0221(13) 0.0036(11) -0.0417(11) Cl8 0.0450(11) 0.1299(18) 0.0727(13) 0.0231(13) 0.0253(10) 0.0022(11) Cl9 0.0659(12) 0.0824(13) 0.0546(11) -0.0065(10) 0.0130(9) 0.0245(10) Cl10 0.0613(11) 0.0424(9) 0.0587(10) -0.0105(8) 0.0138(9) -0.0094(8) Cl11 0.0555(10) 0.0483(9) 0.0859(13) -0.0305(9) -0.0268(10) 0.0166(8) Cl12 0.0575(11) 0.0902(14) 0.0670(12) -0.0397(11) -0.0210(9) 0.0063(10) Cl13 0.0549(11) 0.0903(14) 0.0673(12) 0.0050(11) -0.0302(10) 0.0050(10) Cl14 0.0600(11) 0.0552(11) 0.0967(15) 0.0042(10) -0.0176(11) 0.0221(9) Cl15 0.0567(10) 0.0331(8) 0.0554(10) -0.0060(7) -0.0045(8) 0.0021(7) Cl16 0.0559(10) 0.0605(10) 0.0413(9) -0.0016(8) 0.0041(8) 0.0041(8) Cl17 0.0800(14) 0.0970(15) 0.0916(15) -0.0347(13) 0.0422(12) 0.0161(12) Cl18 0.0603(12) 0.0519(11) 0.145(2) -0.0324(12) -0.0064(13) 0.0252(10) Cl19 0.0878(15) 0.0430(10) 0.1070(16) 0.0131(11) -0.0297(12) 0.0103(10) Cl20 0.0680(11) 0.0492(10) 0.0486(10) 0.0056(8) 0.0049(9) 0.0003(8) C1 0.029(3) 0.034(3) 0.036(3) -0.008(3) 0.005(3) -0.001(3) C2 0.037(3) 0.035(3) 0.038(3) 0.000(3) 0.013(3) 0.005(3) C3 0.042(4) 0.035(3) 0.055(4) -0.002(3) 0.016(3) 0.002(3) C4 0.038(4) 0.040(4) 0.066(4) -0.017(3) 0.012(3) -0.004(3) C5 0.044(4) 0.046(4) 0.044(4) -0.010(3) 0.003(3) 0.000(3) C6 0.038(4) 0.037(3) 0.044(4) -0.010(3) 0.007(3) -0.001(3) C7 0.027(3) 0.035(3) 0.045(4) 0.010(3) 0.003(3) -0.002(3) C8 0.039(4) 0.040(3) 0.049(4) 0.009(3) -0.003(3) -0.003(3) C9 0.029(3) 0.053(4) 0.067(4) 0.023(4) 0.001(3) -0.009(3) C10 0.029(3) 0.070(5) 0.044(4) 0.012(4) 0.005(3) 0.009(3) C11 0.035(4) 0.057(4) 0.044(4) 0.006(3) 0.000(3) 0.015(3) C12 0.032(3) 0.041(3) 0.041(3) 0.005(3) 0.006(3) 0.005(3) C13 0.034(3) 0.039(3) 0.038(3) 0.000(3) -0.002(3) 0.000(3) C14 0.035(3) 0.043(4) 0.050(4) -0.011(3) -0.010(3) 0.007(3) C15 0.032(3) 0.062(4) 0.039(4) -0.008(3) -0.003(3) -0.005(3) C16 0.038(4) 0.052(4) 0.040(4) 0.004(3) -0.011(3) -0.004(3) C17 0.032(3) 0.038(3) 0.057(4) 0.010(3) -0.002(3) 0.007(3) C18 0.038(3) 0.030(3) 0.046(4) -0.005(3) 0.000(3) -0.002(3) C19 0.028(3) 0.034(3) 0.032(3) -0.010(3) -0.006(3) 0.003(2) C20 0.032(3) 0.036(3) 0.042(3) -0.012(3) -0.005(3) 0.001(3) C21 0.030(3) 0.050(4) 0.062(4) -0.025(4) 0.008(3) 0.004(3) C22 0.033(4) 0.035(4) 0.085(5) -0.018(4) -0.013(4) 0.007(3) C23 0.045(4) 0.031(3) 0.068(5) -0.006(3) -0.014(4) -0.003(3) C24 0.034(3) 0.038(3) 0.047(4) -0.008(3) -0.004(3) -0.006(3) N 0.052(3) 0.065(4) 0.033(3) -0.004(3) 0.003(3) 0.004(3) C25 0.057(4) 0.073(5) 0.050(4) -0.002(4) 0.012(4) 0.017(4) C26 0.056(5) 0.108(7) 0.065(5) 0.012(5) 0.004(4) 0.006(5) C27 0.066(6) 0.211(12) 0.080(7) 0.031(7) 0.010(5) 0.056(7) C28 0.130(10) 0.40(2) 0.121(10) 0.071(13) 0.022(9) 0.120(13) C29 0.077(5) 0.077(5) 0.030(4) -0.003(3) -0.002(4) 0.004(4) C30 0.082(6) 0.091(6) 0.053(5) 0.005(4) -0.007(4) 0.018(5) C31 0.083(6) 0.105(7) 0.076(6) 0.021(5) -0.021(5) 0.013(5) C32 0.099(8) 0.154(10) 0.132(9) 0.047(8) -0.026(7) -0.004(7) C33 0.061(4) 0.052(4) 0.044(4) -0.005(3) 0.000(3) 0.005(3) C34 0.065(5) 0.072(5) 0.057(4) 0.007(4) -0.003(4) 0.004(4) C35 0.089(6) 0.072(5) 0.082(6) 0.011(5) -0.012(5) -0.012(5) C36 0.103(7) 0.086(6) 0.149(9) 0.032(7) -0.013(7) -0.018(6) C37 0.054(4) 0.065(4) 0.037(4) -0.002(3) 0.008(3) 0.002(4) C38 0.055(4) 0.065(5) 0.053(4) -0.006(4) -0.007(4) 0.008(4) C39 0.054(4) 0.067(5) 0.057(4) -0.004(4) -0.004(4) -0.009(4) C40 0.107(7) 0.060(5) 0.113(7) 0.010(5) -0.005(6) -0.007(5) _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 V C19 2.142(5) . ? V C1 2.144(5) . ? V C13 2.152(5) . ? V C7 2.158(5) . ? Cl1 C2 1.746(6) . ? Cl2 C3 1.726(6) . ? Cl3 C4 1.724(6) . ? Cl4 C5 1.735(6) . ? Cl5 C6 1.743(6) . ? Cl6 C8 1.734(6) . ? Cl7 C9 1.729(6) . ? Cl8 C10 1.725(6) . ? Cl9 C11 1.717(6) . ? Cl10 C12 1.744(6) . ? Cl11 C14 1.748(6) . ? Cl12 C15 1.725(6) . ? Cl13 C16 1.728(6) . ? Cl14 C17 1.726(6) . ? Cl15 C18 1.742(6) . ? Cl16 C20 1.745(6) . ? Cl17 C21 1.727(6) . ? Cl18 C22 1.722(6) . ? Cl19 C23 1.720(6) . ? Cl20 C24 1.745(6) . ? C1 C6 1.387(7) . ? C1 C2 1.392(7) . ? C2 C3 1.391(8) . ? C3 C4 1.391(8) . ? C4 C5 1.384(8) . ? C5 C6 1.379(7) . ? C7 C8 1.387(7) . ? C7 C12 1.396(7) . ? C8 C9 1.395(8) . ? C9 C10 1.373(8) . ? C10 C11 1.386(8) . ? C11 C12 1.395(7) . ? C13 C14 1.393(7) . ? C13 C18 1.392(7) . ? C14 C15 1.392(7) . ? C15 C16 1.384(8) . ? C16 C17 1.381(8) . ? C17 C18 1.387(7) . ? C19 C20 1.380(7) . ? C19 C24 1.389(7) . ? C20 C21 1.388(7) . ? C21 C22 1.368(8) . ? C22 C23 1.386(9) . ? C23 C24 1.386(8) . ? N C37 1.513(7) . ? N C33 1.524(7) . ? N C29 1.522(7) . ? N C25 1.523(7) . ? C25 C26 1.511(9) . ? C26 C27 1.552(10) . ? C27 C28 1.355(11) . ? C29 C30 1.508(9) . ? C30 C31 1.517(9) . ? C31 C32 1.483(10) . ? C33 C34 1.510(8) . ? C34 C35 1.526(9) . ? C35 C36 1.504(9) . ? C37 C38 1.515(8) . ? C38 C39 1.518(8) . ? C39 C40 1.506(9) . ? 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 C19 V C1 101.15(19) . . ? C19 V C13 112.6(2) . . ? C1 V C13 117.6(2) . . ? C19 V C7 116.1(2) . . ? C1 V C7 112.1(2) . . ? C13 V C7 98.1(2) . . ? C6 C1 C2 114.2(5) . . ? C6 C1 V 115.2(4) . . ? C2 C1 V 130.6(4) . . ? C3 C2 C1 123.4(5) . . ? C3 C2 Cl1 117.4(4) . . ? C1 C2 Cl1 119.2(4) . . ? C2 C3 C4 119.5(5) . . ? C2 C3 Cl2 121.5(5) . . ? C4 C3 Cl2 119.0(5) . . ? C5 C4 C3 118.9(5) . . ? C5 C4 Cl3 120.9(5) . . ? C3 C4 Cl3 120.2(5) . . ? C6 C5 C4 119.2(6) . . ? C6 C5 Cl4 121.2(5) . . ? C4 C5 Cl4 119.6(5) . . ? C5 C6 C1 124.7(5) . . ? C5 C6 Cl5 118.4(5) . . ? C1 C6 Cl5 117.0(4) . . ? C8 C7 C12 114.4(5) . . ? C8 C7 V 114.8(4) . . ? C12 C7 V 130.4(4) . . ? C7 C8 C9 123.6(6) . . ? C7 C8 Cl6 117.1(5) . . ? C9 C8 Cl6 119.3(5) . . ? C10 C9 C8 119.4(6) . . ? C10 C9 Cl7 120.6(5) . . ? C8 C9 Cl7 120.0(5) . . ? C9 C10 C11 120.0(5) . . ? C9 C10 Cl8 119.9(5) . . ? C11 C10 Cl8 120.1(5) . . ? C10 C11 C12 118.4(6) . . ? C10 C11 Cl9 119.7(5) . . ? C12 C11 Cl9 121.9(5) . . ? C11 C12 C7 124.1(5) . . ? C11 C12 Cl10 116.2(5) . . ? C7 C12 Cl10 119.7(4) . . ? C14 C13 C18 113.5(5) . . ? C14 C13 V 130.7(4) . . ? C18 C13 V 115.6(4) . . ? C15 C14 C13 124.0(5) . . ? C15 C14 Cl11 116.2(5) . . ? C13 C14 Cl11 119.7(4) . . ? C16 C15 C14 119.5(5) . . ? C16 C15 Cl12 118.9(4) . . ? C14 C15 Cl12 121.6(5) . . ? C17 C16 C15 119.1(5) . . ? C17 C16 Cl13 120.3(5) . . ? C15 C16 Cl13 120.6(5) . . ? C16 C17 C18 119.1(5) . . ? C16 C17 Cl14 120.1(5) . . ? C18 C17 Cl14 120.8(5) . . ? C17 C18 C13 124.7(5) . . ? C17 C18 Cl15 118.4(4) . . ? C13 C18 Cl15 116.9(4) . . ? C20 C19 C24 114.2(5) . . ? C20 C19 V 113.8(4) . . ? C24 C19 V 132.0(4) . . ? C19 C20 C21 124.1(6) . . ? C19 C20 Cl16 116.5(4) . . ? C21 C20 Cl16 119.4(5) . . ? C22 C21 C20 119.1(6) . . ? C22 C21 Cl17 120.9(5) . . ? C20 C21 Cl17 120.0(5) . . ? C21 C22 C23 119.8(5) . . ? C21 C22 Cl18 119.8(5) . . ? C23 C22 Cl18 120.3(5) . . ? C24 C23 C22 118.6(6) . . ? C24 C23 Cl19 121.7(5) . . ? C22 C23 Cl19 119.7(5) . . ? C23 C24 C19 124.1(5) . . ? C23 C24 Cl20 116.4(5) . . ? C19 C24 Cl20 119.5(4) . . ? C37 N C33 106.7(4) . . ? C37 N C29 110.4(5) . . ? C33 N C29 111.3(5) . . ? C37 N C25 111.0(5) . . ? C33 N C25 111.3(5) . . ? C29 N C25 106.2(5) . . ? C26 C25 N 115.3(5) . . ? C25 C26 C27 108.5(6) . . ? C28 C27 C26 114.3(9) . . ? C30 C29 N 116.5(5) . . ? C29 C30 C31 111.5(6) . . ? C32 C31 C30 113.1(7) . . ? C34 C33 N 117.0(5) . . ? C33 C34 C35 109.6(6) . . ? C36 C35 C34 111.8(7) . . ? N C37 C38 116.2(5) . . ? C37 C38 C39 111.3(5) . . ? C40 C39 C38 113.4(6) . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 0.390 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.077