# Electronic Supplementary Material (ESI) for Catalysis Science & Technology # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_2011src0390 _database_code_depnum_ccdc_archive 'CCDC 837291' #TrackingRef 'lucypap3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 2' _chemical_melting_point ? _chemical_formula_structural '[VCl(L)(THF)]2,1.5(THF)' _chemical_formula_moiety '2(C30 H26 Cl N2 O3 V), 1.5(C4 H8 O)' _chemical_formula_sum 'C66 H64 Cl2 N4 O7.50 V2' _chemical_formula_weight 1205.99 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' O O 0.0106 0.0060 '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 Monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 17.8598(14) _cell_length_b 10.7750(8) _cell_length_c 31.054(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.730(4) _cell_angle_gamma 90.00 _cell_volume 5851.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 38471 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description slab _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2512 _exptl_absorpt_coefficient_mu 0.470 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6039 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Roper CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_reflns_number 27495 _diffrn_reflns_av_R_equivalents 0.1106 _diffrn_reflns_av_sigmaI/netI 0.0878 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 20.00 _reflns_number_total 5438 _reflns_number_gt 3866 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' # Although determined using DirAx, the cell is refined in the HKL # package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Johnson, 1971 and Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 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^ > 2\s(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^)+(0.0046P)^2^+19.6498P] 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 5438 _refine_ls_number_parameters 737 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1007 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.1271 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.28695(6) 0.61584(11) 0.11575(4) 0.0282(4) Uani 1 1 d . . . Cl1 Cl 0.34602(10) 0.73438(16) 0.06841(5) 0.0351(5) Uani 1 1 d . . . O1 O 0.2218(3) 0.5374(4) 0.15012(13) 0.0298(12) Uani 1 1 d . . . C11 C 0.1455(4) 0.5403(7) 0.1407(2) 0.0303(19) Uani 1 1 d . . . C12 C 0.1056(4) 0.6513(6) 0.1244(2) 0.0245(18) Uani 1 1 d . . . C13 C 0.0259(4) 0.6529(7) 0.11597(19) 0.0278(18) Uani 1 1 d . . . H13 H 0.0001 0.7254 0.1057 0.033 Uiso 1 1 calc R . . C14 C -0.0154(4) 0.5495(7) 0.1225(2) 0.0327(19) Uani 1 1 d . . . H14 H -0.0686 0.5507 0.1158 0.039 Uiso 1 1 calc R . . C15 C 0.0241(5) 0.4423(7) 0.1395(2) 0.035(2) Uani 1 1 d . . . H15 H -0.0033 0.3721 0.1445 0.042 Uiso 1 1 calc R . . C16 C 0.1026(4) 0.4389(7) 0.1490(2) 0.0309(19) Uani 1 1 d . . . H16 H 0.1274 0.3674 0.1612 0.037 Uiso 1 1 calc R . . C17 C 0.1473(4) 0.7642(6) 0.12058(18) 0.0247(18) Uani 1 1 d . . . H17 H 0.1194 0.8377 0.1177 0.030 Uiso 1 1 calc R . . N2 N 0.2192(3) 0.7732(5) 0.12079(16) 0.0249(14) Uani 1 1 d . . . C21 C 0.2498(4) 0.8963(7) 0.1222(2) 0.0260(18) Uani 1 1 d . . . C22 C 0.2991(4) 0.9374(6) 0.1608(2) 0.0263(18) Uani 1 1 d . . . C23 C 0.3257(4) 1.0582(7) 0.1610(2) 0.0317(19) Uani 1 1 d . . . H23 H 0.3579 1.0885 0.1862 0.038 Uiso 1 1 calc R . . C24 C 0.3058(4) 1.1353(7) 0.1246(3) 0.036(2) Uani 1 1 d . . . H24 H 0.3253 1.2154 0.1255 0.043 Uiso 1 1 calc R . . C25 C 0.2569(4) 1.0929(7) 0.0872(2) 0.0334(19) Uani 1 1 d . . . H25 H 0.2426 1.1447 0.0630 0.040 Uiso 1 1 calc R . . C26 C 0.2293(4) 0.9724(7) 0.0861(2) 0.0305(19) Uani 1 1 d . . . H26 H 0.1968 0.9430 0.0609 0.037 Uiso 1 1 calc R . . N3 N 0.3630(3) 0.6702(5) 0.17309(17) 0.0281(15) Uani 1 1 d . . . C31 C 0.3407(4) 0.7425(7) 0.2083(2) 0.0273(18) Uani 1 1 d . . . C32 C 0.3140(4) 0.8633(6) 0.2019(2) 0.0259(18) Uani 1 1 d . . . C33 C 0.3010(4) 0.9243(7) 0.2397(3) 0.035(2) Uani 1 1 d . . . H33 H 0.2833 1.0056 0.2370 0.042 Uiso 1 1 calc R . . C34 C 0.3131(4) 0.8693(8) 0.2809(2) 0.039(2) Uani 1 1 d . . . H34 H 0.3049 0.9139 0.3052 0.047 Uiso 1 1 calc R . . C35 C 0.3374(4) 0.7474(8) 0.2856(2) 0.043(2) Uani 1 1 d . . . H35 H 0.3446 0.7083 0.3128 0.051 Uiso 1 1 calc R . . C36 C 0.3510(4) 0.6845(7) 0.2490(2) 0.036(2) Uani 1 1 d . . . H36 H 0.3672 0.6023 0.2518 0.044 Uiso 1 1 calc R . . O4 O 0.3489(3) 0.4731(4) 0.11117(14) 0.0331(12) Uani 1 1 d . . . C41 C 0.4236(4) 0.4627(6) 0.1238(2) 0.0296(19) Uani 1 1 d . . . C42 C 0.4668(4) 0.5348(6) 0.1585(2) 0.0291(18) Uani 1 1 d . . . C43 C 0.5461(4) 0.5142(6) 0.1720(2) 0.0317(19) Uani 1 1 d . . . H43 H 0.5737 0.5593 0.1955 0.038 Uiso 1 1 calc R . . C44 C 0.5829(4) 0.4294(7) 0.1513(3) 0.040(2) Uani 1 1 d . . . H44 H 0.6353 0.4169 0.1605 0.047 Uiso 1 1 calc R . . C45 C 0.5417(5) 0.3612(7) 0.1161(3) 0.041(2) Uani 1 1 d . . . H45 H 0.5669 0.3044 0.1015 0.049 Uiso 1 1 calc R . . C46 C 0.4641(4) 0.3775(6) 0.1029(2) 0.0348(19) Uani 1 1 d . . . H46 H 0.4376 0.3308 0.0795 0.042 Uiso 1 1 calc R . . C47 C 0.4325(4) 0.6262(6) 0.1831(2) 0.0302(19) Uani 1 1 d . . . H47 H 0.4635 0.6565 0.2087 0.036 Uiso 1 1 calc R . . O5 O 0.2079(2) 0.5497(4) 0.05977(14) 0.0317(12) Uani 1 1 d . . . C51 C 0.1919(4) 0.4201(6) 0.0517(2) 0.037(2) Uani 1 1 d . . . H51A H 0.1938 0.3755 0.0790 0.044 Uiso 1 1 calc R . . H51B H 0.2280 0.3830 0.0360 0.044 Uiso 1 1 calc R . . C52 C 0.1121(4) 0.4188(7) 0.0240(2) 0.048(2) Uani 1 1 d . . . H52A H 0.0739 0.4290 0.0418 0.058 Uiso 1 1 calc R . . H52B H 0.1021 0.3427 0.0071 0.058 Uiso 1 1 calc R . . C53 C 0.1146(4) 0.5305(8) -0.0057(2) 0.054(2) Uani 1 1 d . . . H53A H 0.1335 0.5071 -0.0317 0.064 Uiso 1 1 calc R . . H53B H 0.0641 0.5668 -0.0148 0.064 Uiso 1 1 calc R . . C54 C 0.1687(4) 0.6204(7) 0.0223(2) 0.042(2) Uani 1 1 d . . . H54A H 0.2049 0.6538 0.0059 0.050 Uiso 1 1 calc R . . H54B H 0.1405 0.6887 0.0319 0.050 Uiso 1 1 calc R . . V2 V 0.37224(7) 0.27267(12) 0.40426(4) 0.0399(4) Uani 1 1 d . A . Cl2 Cl 0.31563(11) 0.09084(18) 0.42420(6) 0.0460(6) Uani 1 1 d . . . O6 O 0.4052(3) 0.4320(5) 0.38668(14) 0.0432(14) Uani 1 1 d . . . C61 C 0.3709(5) 0.5390(8) 0.3918(2) 0.039(2) Uani 1 1 d . . . C62 C 0.2896(5) 0.5508(8) 0.3841(2) 0.042(2) Uani 1 1 d . . . C63 C 0.2573(6) 0.6682(9) 0.3873(3) 0.068(3) Uani 1 1 d . . . H63 H 0.2044 0.6766 0.3809 0.081 Uiso 1 1 calc R . . C64 C 0.3020(8) 0.7709(9) 0.3995(3) 0.078(3) Uani 1 1 d . . . H64 H 0.2793 0.8473 0.4025 0.094 Uiso 1 1 calc R . . C65 C 0.3808(7) 0.7607(9) 0.4073(3) 0.067(3) Uani 1 1 d . . . H65 H 0.4113 0.8301 0.4157 0.081 Uiso 1 1 calc R . . C66 C 0.4141(5) 0.6474(9) 0.4027(2) 0.051(2) Uani 1 1 d . . . H66 H 0.4670 0.6427 0.4069 0.061 Uiso 1 1 calc R . . C67 C 0.2422(5) 0.4467(8) 0.3710(2) 0.041(2) Uani 1 1 d . . . H67 H 0.1909 0.4629 0.3594 0.049 Uiso 1 1 calc R . . N7 N 0.2630(3) 0.3309(6) 0.37331(17) 0.0325(15) Uani 1 1 d . . . C71 C 0.2061(4) 0.2442(7) 0.3518(2) 0.036(2) Uani 1 1 d . . . C72 C 0.2167(4) 0.1889(7) 0.3125(2) 0.036(2) Uani 1 1 d . . . C73 C 0.1627(5) 0.0990(7) 0.2944(3) 0.048(2) Uani 1 1 d . . . H73 H 0.1677 0.0606 0.2684 0.058 Uiso 1 1 calc R . . C74 C 0.1021(5) 0.0645(8) 0.3137(3) 0.055(2) Uani 1 1 d . . . H74 H 0.0682 0.0029 0.3010 0.066 Uiso 1 1 calc R . . C75 C 0.0928(5) 0.1226(9) 0.3517(3) 0.058(2) Uani 1 1 d . . . H75 H 0.0520 0.1014 0.3647 0.069 Uiso 1 1 calc R . . C76 C 0.1444(5) 0.2125(8) 0.3706(2) 0.047(2) Uani 1 1 d . . . H76 H 0.1377 0.2522 0.3961 0.056 Uiso 1 1 calc R . . N8 N 0.3894(3) 0.1879(6) 0.34685(18) 0.0351(16) Uani 1 1 d . . . C81 C 0.3537(4) 0.2341(6) 0.3036(2) 0.0312(19) Uani 1 1 d . . . C82 C 0.2748(4) 0.2340(6) 0.2883(2) 0.0323(19) Uani 1 1 d . . . C83 C 0.2486(5) 0.2829(7) 0.2457(2) 0.045(2) Uani 1 1 d . . . H83 H 0.1962 0.2866 0.2347 0.054 Uiso 1 1 calc R . . C84 C 0.2974(5) 0.3255(7) 0.2197(3) 0.048(2) Uani 1 1 d . . . H84 H 0.2780 0.3560 0.1916 0.057 Uiso 1 1 calc R . . C85 C 0.3748(5) 0.3223(6) 0.2356(2) 0.037(2) Uani 1 1 d . . . H85 H 0.4081 0.3513 0.2184 0.044 Uiso 1 1 calc R . . C86 C 0.4034(4) 0.2761(6) 0.2771(2) 0.039(2) Uani 1 1 d . . . H86 H 0.4560 0.2728 0.2875 0.047 Uiso 1 1 calc R . . O9 O 0.4730(3) 0.2199(5) 0.43370(14) 0.0423(13) Uani 1 1 d . . . C91 C 0.5044(4) 0.1115(8) 0.4269(3) 0.042(2) Uani 1 1 d . . . C92 C 0.4904(4) 0.0500(8) 0.3868(3) 0.038(2) Uani 1 1 d . . . C93 C 0.5266(5) -0.0623(8) 0.3820(3) 0.055(2) Uani 1 1 d . . . H93 H 0.5182 -0.1015 0.3548 0.066 Uiso 1 1 calc R . . C94 C 0.5749(5) -0.1154(9) 0.4175(3) 0.064(3) Uani 1 1 d . . . H94 H 0.5978 -0.1917 0.4149 0.077 Uiso 1 1 calc R . . C95 C 0.5885(5) -0.0520(11) 0.4576(3) 0.070(3) Uani 1 1 d . . . H95 H 0.6208 -0.0876 0.4818 0.084 Uiso 1 1 calc R . . C96 C 0.5564(5) 0.0594(9) 0.4625(3) 0.059(3) Uani 1 1 d . . . H96 H 0.5686 0.1013 0.4892 0.071 Uiso 1 1 calc R . . C97 C 0.4403(4) 0.1002(8) 0.3481(2) 0.040(2) Uani 1 1 d . . . H97 H 0.4448 0.0663 0.3212 0.048 Uiso 1 1 calc R . . O10 O 0.3561(3) 0.3560(5) 0.46303(16) 0.0584(16) Uani 1 1 d . . . C101 C 0.2888(6) 0.3646(8) 0.4818(3) 0.081(3) Uani 0.90(2) 1 d P A 1 H10A H 0.2673 0.2829 0.4843 0.098 Uiso 0.90(2) 1 calc PR A 1 H10B H 0.2504 0.4160 0.4635 0.098 Uiso 0.90(2) 1 calc PR A 1 C102 C 0.3139(12) 0.422(2) 0.5264(5) 0.169(12) Uani 0.90(2) 1 d P A 1 H10C H 0.2744 0.4746 0.5338 0.203 Uiso 0.90(2) 1 calc PR A 1 H10D H 0.3278 0.3589 0.5490 0.203 Uiso 0.90(2) 1 calc PR A 1 C103 C 0.3800(10) 0.4937(14) 0.5207(5) 0.150(7) Uani 0.90(2) 1 d P A 1 H10E H 0.4136 0.5091 0.5489 0.180 Uiso 0.90(2) 1 calc PR A 1 H10F H 0.3642 0.5727 0.5069 0.180 Uiso 0.90(2) 1 calc PR A 1 C104 C 0.4194(6) 0.4176(9) 0.4922(3) 0.086(3) Uani 1 1 d . A . H10G H 0.4482 0.4693 0.4758 0.104 Uiso 1 1 calc R B 1 H10H H 0.4537 0.3577 0.5094 0.104 Uiso 1 1 calc R B 1 C107 C 0.2888(6) 0.3646(8) 0.4818(3) 0.081(3) Uani 0.10(2) 1 d P A 2 H10I H 0.2887 0.3043 0.5050 0.098 Uiso 0.10(2) 1 calc PR A 2 H10J H 0.2418 0.3585 0.4599 0.098 Uiso 0.10(2) 1 calc PR A 2 C108 C 0.307(3) 0.516(6) 0.502(2) 0.00(3) Uiso 0.10(2) 1 d P A 2 H10K H 0.3011 0.5773 0.4789 0.004 Uiso 0.10(2) 1 calc PR A 2 H10L H 0.2760 0.5379 0.5232 0.004 Uiso 0.10(2) 1 calc PR A 2 C109 C 0.3800(10) 0.4937(14) 0.5207(5) 0.150(7) Uani 0.10(2) 1 d P A 2 H10M H 0.3822 0.4509 0.5485 0.180 Uiso 0.10(2) 1 calc PR A 2 H10N H 0.4066 0.5722 0.5270 0.180 Uiso 0.10(2) 1 calc PR A 2 O11 O 0.5551(3) 0.7809(6) 0.26381(18) 0.0673(17) Uani 1 1 d . . . C111 C 0.5219(5) 0.8953(8) 0.2491(3) 0.055(2) Uani 1 1 d . . . H11A H 0.4771 0.9107 0.2614 0.066 Uiso 1 1 calc R . . H11B H 0.5068 0.8958 0.2172 0.066 Uiso 1 1 calc R . . C112 C 0.5825(5) 0.9932(8) 0.2645(3) 0.056(2) Uani 1 1 d . . . H11C H 0.5827 1.0189 0.2944 0.067 Uiso 1 1 calc R . . H11D H 0.5750 1.0654 0.2454 0.067 Uiso 1 1 calc R . . C113 C 0.6563(4) 0.9246(8) 0.2614(2) 0.052(2) Uani 1 1 d . . . H11E H 0.6734 0.9467 0.2346 0.062 Uiso 1 1 calc R . . H11F H 0.6967 0.9431 0.2865 0.062 Uiso 1 1 calc R . . C114 C 0.6334(5) 0.7877(9) 0.2609(3) 0.087(3) Uani 1 1 d . . . H11G H 0.6409 0.7486 0.2340 0.104 Uiso 1 1 calc R . . H11H H 0.6648 0.7447 0.2856 0.104 Uiso 1 1 calc R . . O12 O 0.4251(5) 0.3995(8) -0.0087(3) 0.037(2) Uiso 0.50 1 d P . . C121 C 0.4224(10) 0.5295(16) 0.0040(6) 0.032(5) Uiso 0.50 1 d P . . H12A H 0.3971 0.5386 0.0286 0.038 Uiso 0.50 1 calc PR . . H12B H 0.3956 0.5791 -0.0204 0.038 Uiso 0.50 1 calc PR . . C122 C 0.5114(11) 0.5700(18) 0.0176(6) 0.042(6) Uiso 0.50 1 d P . . H12C H 0.5212 0.6455 0.0026 0.050 Uiso 0.50 1 calc PR . . H12D H 0.5270 0.5819 0.0491 0.050 Uiso 0.50 1 calc PR . . C123 C 0.5509(11) 0.4610(16) 0.0024(6) 0.029(5) Uiso 0.50 1 d P . . H12E H 0.5892 0.4892 -0.0135 0.035 Uiso 0.50 1 calc PR . . H12F H 0.5763 0.4126 0.0275 0.035 Uiso 0.50 1 calc PR . . C124 C 0.4933(10) 0.3844(18) -0.0264(5) 0.044(6) Uiso 0.50 1 d P . . H12G H 0.4849 0.4135 -0.0566 0.052 Uiso 0.50 1 calc PR . . H12H H 0.5089 0.2981 -0.0255 0.052 Uiso 0.50 1 calc PR . . 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 0.0194(8) 0.0249(8) 0.0377(8) -0.0006(6) -0.0005(6) 0.0004(6) Cl1 0.0246(11) 0.0370(12) 0.0426(11) -0.0007(10) 0.0044(9) -0.0039(10) O1 0.016(3) 0.031(3) 0.039(3) -0.002(2) -0.001(2) 0.000(2) C11 0.023(5) 0.041(6) 0.026(4) 0.003(4) 0.002(4) -0.005(5) C12 0.017(5) 0.029(5) 0.028(4) -0.001(4) 0.005(3) -0.002(4) C13 0.031(6) 0.028(5) 0.022(4) 0.004(3) -0.001(4) 0.006(4) C14 0.023(5) 0.037(5) 0.037(5) -0.002(4) 0.004(4) -0.009(5) C15 0.042(6) 0.030(5) 0.034(5) 0.000(4) 0.010(4) -0.009(5) C16 0.019(5) 0.035(5) 0.035(5) 0.011(4) -0.002(4) -0.002(4) C17 0.031(6) 0.020(5) 0.020(4) 0.003(3) -0.003(3) 0.004(4) N2 0.013(4) 0.020(4) 0.039(4) 0.001(3) 0.000(3) 0.000(3) C21 0.023(5) 0.021(5) 0.035(5) -0.007(4) 0.008(4) -0.004(4) C22 0.023(5) 0.018(5) 0.036(5) -0.003(4) 0.002(4) 0.001(4) C23 0.029(5) 0.025(5) 0.042(5) -0.006(4) 0.007(4) -0.003(4) C24 0.032(5) 0.023(5) 0.058(6) -0.003(5) 0.023(5) -0.007(4) C25 0.039(5) 0.025(5) 0.038(5) 0.006(4) 0.011(4) 0.000(4) C26 0.023(5) 0.025(5) 0.043(5) -0.002(4) 0.006(4) -0.002(4) N3 0.012(4) 0.027(4) 0.041(4) 0.004(3) -0.003(3) -0.002(3) C31 0.012(4) 0.036(5) 0.030(5) -0.007(4) -0.004(3) 0.002(4) C32 0.011(4) 0.022(5) 0.041(5) -0.010(4) -0.003(3) -0.002(4) C33 0.024(5) 0.027(5) 0.049(6) -0.005(5) -0.004(4) -0.001(4) C34 0.029(5) 0.046(6) 0.037(6) -0.010(5) -0.005(4) -0.010(4) C35 0.046(6) 0.043(6) 0.037(5) 0.007(5) 0.001(4) -0.004(5) C36 0.030(5) 0.046(5) 0.033(5) 0.003(5) 0.004(4) 0.007(4) O4 0.024(3) 0.032(3) 0.041(3) 0.000(2) 0.001(2) 0.002(3) C41 0.018(5) 0.021(5) 0.048(5) 0.005(4) 0.002(4) -0.006(4) C42 0.020(5) 0.022(5) 0.046(5) 0.008(4) 0.006(4) -0.001(4) C43 0.023(5) 0.023(5) 0.048(5) 0.003(4) 0.003(4) -0.003(4) C44 0.022(5) 0.033(5) 0.060(6) 0.016(5) 0.000(5) 0.007(5) C45 0.042(7) 0.031(5) 0.054(6) 0.014(4) 0.020(5) 0.010(5) C46 0.031(6) 0.029(5) 0.044(5) -0.002(4) 0.006(4) 0.011(4) C47 0.028(5) 0.027(5) 0.031(4) 0.006(4) -0.004(4) -0.011(4) O5 0.021(3) 0.032(3) 0.037(3) -0.003(3) -0.007(2) 0.002(3) C51 0.037(5) 0.017(5) 0.056(5) -0.014(4) 0.013(4) -0.004(4) C52 0.037(6) 0.052(6) 0.057(5) -0.016(5) 0.011(4) -0.026(5) C53 0.033(5) 0.067(6) 0.055(5) -0.015(5) -0.006(4) -0.012(5) C54 0.043(5) 0.044(5) 0.034(5) 0.000(4) -0.002(4) -0.004(5) V2 0.0371(9) 0.0442(9) 0.0359(8) -0.0009(7) 0.0017(6) -0.0019(7) Cl2 0.0406(13) 0.0423(13) 0.0548(13) 0.0062(11) 0.0092(10) 0.0005(11) O6 0.046(4) 0.043(4) 0.039(3) -0.008(3) 0.005(3) -0.001(3) C61 0.060(7) 0.030(6) 0.027(5) -0.012(4) 0.006(4) -0.020(6) C62 0.049(7) 0.039(6) 0.041(5) -0.003(4) 0.017(4) 0.000(6) C63 0.075(7) 0.038(6) 0.102(8) -0.009(6) 0.046(6) -0.002(7) C64 0.120(11) 0.033(7) 0.102(8) -0.016(6) 0.071(8) 0.000(7) C65 0.100(10) 0.050(8) 0.058(6) -0.014(5) 0.032(6) -0.034(7) C66 0.061(6) 0.051(6) 0.040(5) -0.001(5) 0.008(4) -0.015(6) C67 0.038(6) 0.045(6) 0.037(5) 0.001(4) 0.003(4) 0.001(5) N7 0.031(4) 0.029(4) 0.039(4) -0.017(3) 0.011(3) -0.009(4) C71 0.028(5) 0.040(5) 0.038(5) 0.006(5) 0.003(4) 0.006(4) C72 0.030(5) 0.036(5) 0.038(5) 0.001(4) -0.002(4) 0.010(5) C73 0.031(6) 0.047(6) 0.059(5) -0.010(5) -0.010(5) 0.004(5) C74 0.026(6) 0.059(6) 0.075(7) 0.002(6) -0.002(5) 0.000(5) C75 0.035(6) 0.077(7) 0.058(6) 0.005(6) 0.001(5) 0.001(6) C76 0.037(6) 0.060(6) 0.042(5) 0.000(5) 0.008(5) 0.015(5) N8 0.026(4) 0.034(4) 0.043(4) 0.002(3) 0.003(3) 0.003(4) C81 0.044(6) 0.018(4) 0.032(5) -0.001(4) 0.007(5) -0.004(4) C82 0.028(6) 0.029(5) 0.036(5) -0.015(4) -0.003(4) -0.003(4) C83 0.056(6) 0.041(5) 0.032(5) -0.006(4) -0.005(5) 0.014(5) C84 0.058(7) 0.048(6) 0.032(5) -0.003(4) -0.003(5) 0.003(5) C85 0.059(7) 0.021(5) 0.029(5) 0.003(4) 0.005(4) -0.003(4) C86 0.039(5) 0.031(5) 0.043(5) -0.006(4) 0.001(5) -0.004(4) O9 0.031(3) 0.056(4) 0.036(3) 0.001(3) -0.005(2) -0.006(3) C91 0.026(5) 0.049(6) 0.053(6) 0.010(6) 0.013(5) 0.009(5) C92 0.027(5) 0.047(6) 0.039(6) 0.008(5) 0.006(4) 0.011(5) C93 0.039(6) 0.073(7) 0.055(6) 0.020(5) 0.016(5) 0.023(5) C94 0.043(6) 0.087(7) 0.065(7) 0.022(7) 0.017(5) 0.025(6) C95 0.046(6) 0.104(9) 0.058(7) 0.028(7) 0.007(5) 0.016(7) C96 0.046(6) 0.068(7) 0.058(6) 0.016(5) 0.001(5) 0.015(6) C97 0.032(5) 0.055(6) 0.034(5) 0.002(5) 0.007(4) -0.005(5) O10 0.070(4) 0.060(4) 0.046(3) -0.012(3) 0.013(3) -0.014(3) C101 0.101(9) 0.071(7) 0.097(8) 0.008(6) 0.077(7) 0.026(6) C102 0.23(2) 0.24(3) 0.064(10) 0.022(13) 0.090(14) 0.150(19) C103 0.23(2) 0.144(14) 0.059(9) -0.036(9) -0.010(11) 0.124(15) C104 0.138(10) 0.073(7) 0.042(6) -0.004(6) 0.004(7) -0.015(7) C107 0.101(9) 0.071(7) 0.097(8) 0.008(6) 0.077(7) 0.026(6) C109 0.23(2) 0.144(14) 0.059(9) -0.036(9) -0.010(11) 0.124(15) O11 0.047(4) 0.066(5) 0.082(4) 0.008(4) -0.005(3) -0.008(4) C111 0.042(6) 0.064(6) 0.053(5) -0.001(5) -0.006(4) 0.006(6) C112 0.042(6) 0.070(6) 0.054(5) -0.011(5) 0.003(4) -0.016(6) C113 0.026(5) 0.077(7) 0.049(5) -0.003(5) 0.000(4) -0.007(5) C114 0.045(7) 0.079(8) 0.134(9) -0.008(7) 0.011(6) -0.005(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O4 1.917(5) . ? V1 O1 1.926(4) . ? V1 N3 2.092(5) . ? V1 N2 2.107(5) . ? V1 O5 2.127(4) . ? V1 Cl1 2.353(2) . ? O1 C11 1.335(8) . ? C11 C16 1.389(9) . ? C11 C12 1.431(9) . ? C12 C13 1.394(9) . ? C12 C17 1.444(9) . ? C13 C14 1.374(9) . ? C13 H13 0.9300 . ? C14 C15 1.400(9) . ? C14 H14 0.9300 . ? C15 C16 1.372(9) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 N2 1.287(8) . ? C17 H17 0.9300 . ? N2 C21 1.432(8) . ? C21 C26 1.377(9) . ? C21 C22 1.408(9) . ? C22 C23 1.386(9) . ? C22 C32 1.481(9) . ? C23 C24 1.388(9) . ? C23 H23 0.9300 . ? C24 C25 1.382(9) . ? C24 H24 0.9300 . ? C25 C26 1.386(9) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? N3 C47 1.306(8) . ? N3 C31 1.462(8) . ? C31 C32 1.387(9) . ? C31 C36 1.390(9) . ? C32 C33 1.407(9) . ? C33 C34 1.386(9) . ? C33 H33 0.9300 . ? C34 C35 1.381(9) . ? C34 H34 0.9300 . ? C35 C36 1.384(9) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? O4 C41 1.317(8) . ? C41 C46 1.407(9) . ? C41 C42 1.420(9) . ? C42 C43 1.411(9) . ? C42 C47 1.456(9) . ? C43 C44 1.362(9) . ? C43 H43 0.9300 . ? C44 C45 1.396(9) . ? C44 H44 0.9300 . ? C45 C46 1.375(9) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? O5 C51 1.437(7) . ? O5 C54 1.446(7) . ? C51 C52 1.507(9) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.522(10) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.513(9) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? V2 O6 1.930(5) . ? V2 O9 1.931(5) . ? V2 N8 2.080(6) . ? V2 N7 2.089(6) . ? V2 O10 2.106(5) . ? V2 Cl2 2.345(2) . ? O6 C61 1.330(8) . ? C61 C66 1.402(10) . ? C61 C62 1.429(11) . ? C62 C63 1.402(10) . ? C62 C67 1.414(10) . ? C63 C64 1.372(12) . ? C63 H63 0.9300 . ? C64 C65 1.384(12) . ? C64 H64 0.9300 . ? C65 C66 1.378(11) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 N7 1.300(8) . ? C67 H67 0.9300 . ? N7 C71 1.441(9) . ? C71 C76 1.389(9) . ? C71 C72 1.407(9) . ? C72 C73 1.400(10) . ? C72 C82 1.482(10) . ? C73 C74 1.389(10) . ? C73 H73 0.9300 . ? C74 C75 1.377(10) . ? C74 H74 0.9300 . ? C75 C76 1.382(10) . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? N8 C97 1.307(8) . ? N8 C81 1.451(8) . ? C81 C82 1.392(9) . ? C81 C86 1.404(9) . ? C82 C83 1.411(9) . ? C83 C84 1.383(10) . ? C83 H83 0.9300 . ? C84 C85 1.371(10) . ? C84 H84 0.9300 . ? C85 C86 1.377(9) . ? C85 H85 0.9300 . ? C86 H86 0.9300 . ? O9 C91 1.330(8) . ? C91 C92 1.390(10) . ? C91 C96 1.408(10) . ? C92 C93 1.394(10) . ? C92 C97 1.449(10) . ? C93 C94 1.378(10) . ? C93 H93 0.9300 . ? C94 C95 1.398(11) . ? C94 H94 0.9300 . ? C95 C96 1.352(11) . ? C95 H95 0.9300 . ? C96 H96 0.9300 . ? C97 H97 0.9300 . ? O10 C101 1.441(9) . ? O10 C104 1.457(10) . ? C101 C102 1.499(19) . ? C101 H10A 0.9700 . ? C101 H10B 0.9700 . ? C102 C103 1.45(2) . ? C102 H10C 0.9700 . ? C102 H10D 0.9700 . ? C103 C104 1.485(14) . ? C103 H10E 0.9700 . ? C103 H10F 0.9700 . ? C104 H10G 0.9700 . ? C104 H10H 0.9700 . ? C108 H10K 0.9700 . ? C108 H10L 0.9700 . ? O11 C111 1.403(9) . ? O11 C114 1.422(9) . ? C111 C112 1.518(10) . ? C111 H11A 0.9700 . ? C111 H11B 0.9700 . ? C112 C113 1.531(10) . ? C112 H11C 0.9700 . ? C112 H11D 0.9700 . ? C113 C114 1.530(11) . ? C113 H11E 0.9700 . ? C113 H11F 0.9700 . ? C114 H11G 0.9700 . ? C114 H11H 0.9700 . ? O12 C124 1.44(2) . ? O12 C121 1.459(18) . ? C121 C122 1.62(3) . ? C121 H12A 0.9700 . ? C121 H12B 0.9700 . ? C122 C123 1.50(2) . ? C122 H12C 0.9700 . ? C122 H12D 0.9700 . ? C123 C124 1.47(3) . ? C123 H12E 0.9700 . ? C123 H12F 0.9700 . ? C124 H12G 0.9700 . ? C124 H12H 0.9700 . ? 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 O4 V1 O1 96.41(19) . . ? O4 V1 N3 90.2(2) . . ? O1 V1 N3 90.7(2) . . ? O4 V1 N2 179.8(2) . . ? O1 V1 N2 83.8(2) . . ? N3 V1 N2 89.7(2) . . ? O4 V1 O5 88.14(18) . . ? O1 V1 O5 86.03(18) . . ? N3 V1 O5 176.12(19) . . ? N2 V1 O5 91.99(19) . . ? O4 V1 Cl1 92.89(14) . . ? O1 V1 Cl1 169.19(15) . . ? N3 V1 Cl1 94.80(15) . . ? N2 V1 Cl1 86.95(16) . . ? O5 V1 Cl1 88.77(13) . . ? C11 O1 V1 124.9(4) . . ? O1 C11 C16 121.2(7) . . ? O1 C11 C12 120.7(7) . . ? C16 C11 C12 117.9(7) . . ? C13 C12 C11 119.5(6) . . ? C13 C12 C17 119.9(7) . . ? C11 C12 C17 120.3(6) . . ? C14 C13 C12 121.4(7) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 118.7(7) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C16 C15 C14 121.2(7) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C11 121.2(7) . . ? C15 C16 H16 119.4 . . ? C11 C16 H16 119.4 . . ? N2 C17 C12 126.4(6) . . ? N2 C17 H17 116.8 . . ? C12 C17 H17 116.8 . . ? C17 N2 C21 116.4(6) . . ? C17 N2 V1 121.8(5) . . ? C21 N2 V1 121.7(4) . . ? C26 C21 C22 121.6(7) . . ? C26 C21 N2 119.4(6) . . ? C22 C21 N2 119.0(6) . . ? C23 C22 C21 116.9(6) . . ? C23 C22 C32 120.1(6) . . ? C21 C22 C32 122.5(6) . . ? C22 C23 C24 121.8(7) . . ? C22 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C25 C24 C23 120.0(7) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 119.4(7) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C21 C26 C25 120.2(7) . . ? C21 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C47 N3 C31 113.9(5) . . ? C47 N3 V1 121.5(5) . . ? C31 N3 V1 123.8(4) . . ? C32 C31 C36 122.0(7) . . ? C32 C31 N3 122.1(6) . . ? C36 C31 N3 115.8(6) . . ? C31 C32 C33 115.4(7) . . ? C31 C32 C22 128.8(7) . . ? C33 C32 C22 115.9(6) . . ? C34 C33 C32 123.4(7) . . ? C34 C33 H33 118.3 . . ? C32 C33 H33 118.3 . . ? C35 C34 C33 119.3(7) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? C34 C35 C36 119.0(7) . . ? C34 C35 H35 120.5 . . ? C36 C35 H35 120.5 . . ? C35 C36 C31 120.9(7) . . ? C35 C36 H36 119.6 . . ? C31 C36 H36 119.6 . . ? C41 O4 V1 127.7(4) . . ? O4 C41 C46 120.1(7) . . ? O4 C41 C42 122.8(7) . . ? C46 C41 C42 117.1(7) . . ? C43 C42 C41 119.8(7) . . ? C43 C42 C47 117.0(7) . . ? C41 C42 C47 123.1(7) . . ? C44 C43 C42 121.1(7) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C43 C44 C45 119.7(7) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C46 C45 C44 120.3(7) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C41 121.9(7) . . ? C45 C46 H46 119.1 . . ? C41 C46 H46 119.1 . . ? N3 C47 C42 126.9(6) . . ? N3 C47 H47 116.5 . . ? C42 C47 H47 116.5 . . ? C51 O5 C54 109.0(5) . . ? C51 O5 V1 122.9(4) . . ? C54 O5 V1 127.8(4) . . ? O5 C51 C52 103.9(6) . . ? O5 C51 H51A 111.0 . . ? C52 C51 H51A 111.0 . . ? O5 C51 H51B 111.0 . . ? C52 C51 H51B 111.0 . . ? H51A C51 H51B 109.0 . . ? C51 C52 C53 101.5(6) . . ? C51 C52 H52A 111.5 . . ? C53 C52 H52A 111.5 . . ? C51 C52 H52B 111.5 . . ? C53 C52 H52B 111.5 . . ? H52A C52 H52B 109.3 . . ? C54 C53 C52 104.6(6) . . ? C54 C53 H53A 110.8 . . ? C52 C53 H53A 110.8 . . ? C54 C53 H53B 110.8 . . ? C52 C53 H53B 110.8 . . ? H53A C53 H53B 108.9 . . ? O5 C54 C53 105.9(6) . . ? O5 C54 H54A 110.6 . . ? C53 C54 H54A 110.6 . . ? O5 C54 H54B 110.6 . . ? C53 C54 H54B 110.6 . . ? H54A C54 H54B 108.7 . . ? O6 V2 O9 95.0(2) . . ? O6 V2 N8 92.4(2) . . ? O9 V2 N8 89.5(2) . . ? O6 V2 N7 85.0(2) . . ? O9 V2 N7 179.1(2) . . ? N8 V2 N7 91.4(2) . . ? O6 V2 O10 88.2(2) . . ? O9 V2 O10 89.7(2) . . ? N8 V2 O10 179.0(2) . . ? N7 V2 O10 89.5(2) . . ? O6 V2 Cl2 172.28(17) . . ? O9 V2 Cl2 92.24(16) . . ? N8 V2 Cl2 90.35(17) . . ? N7 V2 Cl2 87.70(18) . . ? O10 V2 Cl2 89.15(16) . . ? C61 O6 V2 124.2(5) . . ? O6 C61 C66 120.5(8) . . ? O6 C61 C62 122.3(7) . . ? C66 C61 C62 117.2(8) . . ? C63 C62 C67 120.3(9) . . ? C63 C62 C61 119.1(8) . . ? C67 C62 C61 120.4(8) . . ? C64 C63 C62 121.5(9) . . ? C64 C63 H63 119.2 . . ? C62 C63 H63 119.2 . . ? C63 C64 C65 119.9(9) . . ? C63 C64 H64 120.1 . . ? C65 C64 H64 120.1 . . ? C66 C65 C64 119.8(9) . . ? C66 C65 H65 120.1 . . ? C64 C65 H65 120.1 . . ? C65 C66 C61 122.4(9) . . ? C65 C66 H66 118.8 . . ? C61 C66 H66 118.8 . . ? N7 C67 C62 126.7(8) . . ? N7 C67 H67 116.7 . . ? C62 C67 H67 116.7 . . ? C67 N7 C71 115.5(6) . . ? C67 N7 V2 122.9(5) . . ? C71 N7 V2 121.6(5) . . ? C76 C71 C72 121.2(7) . . ? C76 C71 N7 120.7(7) . . ? C72 C71 N7 118.0(7) . . ? C73 C72 C71 115.9(7) . . ? C73 C72 C82 121.4(7) . . ? C71 C72 C82 122.2(7) . . ? C74 C73 C72 123.1(8) . . ? C74 C73 H73 118.4 . . ? C72 C73 H73 118.4 . . ? C75 C74 C73 119.2(8) . . ? C75 C74 H74 120.4 . . ? C73 C74 H74 120.4 . . ? C74 C75 C76 119.7(8) . . ? C74 C75 H75 120.2 . . ? C76 C75 H75 120.2 . . ? C75 C76 C71 120.8(7) . . ? C75 C76 H76 119.6 . . ? C71 C76 H76 119.6 . . ? C97 N8 C81 116.5(6) . . ? C97 N8 V2 121.0(5) . . ? C81 N8 V2 121.9(5) . . ? C82 C81 C86 121.0(7) . . ? C82 C81 N8 122.7(6) . . ? C86 C81 N8 116.3(7) . . ? C81 C82 C83 116.2(7) . . ? C81 C82 C72 126.3(7) . . ? C83 C82 C72 117.6(7) . . ? C84 C83 C82 122.9(7) . . ? C84 C83 H83 118.6 . . ? C82 C83 H83 118.6 . . ? C85 C84 C83 119.3(7) . . ? C85 C84 H84 120.3 . . ? C83 C84 H84 120.3 . . ? C84 C85 C86 120.1(7) . . ? C84 C85 H85 119.9 . . ? C86 C85 H85 119.9 . . ? C85 C86 C81 120.5(7) . . ? C85 C86 H86 119.8 . . ? C81 C86 H86 119.8 . . ? C91 O9 V2 124.5(5) . . ? O9 C91 C92 123.8(7) . . ? O9 C91 C96 117.3(8) . . ? C92 C91 C96 118.9(8) . . ? C91 C92 C93 120.4(7) . . ? C91 C92 C97 122.3(8) . . ? C93 C92 C97 117.3(8) . . ? C94 C93 C92 120.2(8) . . ? C94 C93 H93 119.9 . . ? C92 C93 H93 119.9 . . ? C93 C94 C95 118.5(9) . . ? C93 C94 H94 120.7 . . ? C95 C94 H94 120.7 . . ? C96 C95 C94 122.2(9) . . ? C96 C95 H95 118.9 . . ? C94 C95 H95 118.9 . . ? C95 C96 C91 119.6(9) . . ? C95 C96 H96 120.2 . . ? C91 C96 H96 120.2 . . ? N8 C97 C92 127.1(7) . . ? N8 C97 H97 116.5 . . ? C92 C97 H97 116.5 . . ? C101 O10 C104 108.9(6) . . ? C101 O10 V2 130.6(5) . . ? C104 O10 V2 120.5(5) . . ? O10 C101 C102 106.4(10) . . ? O10 C101 H10A 110.4 . . ? C102 C101 H10A 110.4 . . ? O10 C101 H10B 110.4 . . ? C102 C101 H10B 110.4 . . ? H10A C101 H10B 108.6 . . ? C103 C102 C101 101.8(11) . . ? C103 C102 H10C 111.4 . . ? C101 C102 H10C 111.4 . . ? C103 C102 H10D 111.4 . . ? C101 C102 H10D 111.4 . . ? H10C C102 H10D 109.3 . . ? C102 C103 C104 105.9(14) . . ? C102 C103 H10E 110.6 . . ? C104 C103 H10E 110.6 . . ? C102 C103 H10F 110.6 . . ? C104 C103 H10F 110.6 . . ? H10E C103 H10F 108.7 . . ? O10 C104 C103 102.7(10) . . ? O10 C104 H10G 111.2 . . ? C103 C104 H10G 111.2 . . ? O10 C104 H10H 111.2 . . ? C103 C104 H10H 111.2 . . ? H10G C104 H10H 109.1 . . ? H10K C108 H10L 110.2 . . ? C111 O11 C114 106.8(7) . . ? O11 C111 C112 106.3(6) . . ? O11 C111 H11A 110.5 . . ? C112 C111 H11A 110.5 . . ? O11 C111 H11B 110.5 . . ? C112 C111 H11B 110.5 . . ? H11A C111 H11B 108.7 . . ? C111 C112 C113 102.3(6) . . ? C111 C112 H11C 111.3 . . ? C113 C112 H11C 111.3 . . ? C111 C112 H11D 111.3 . . ? C113 C112 H11D 111.3 . . ? H11C C112 H11D 109.2 . . ? C114 C113 C112 103.5(7) . . ? C114 C113 H11E 111.1 . . ? C112 C113 H11E 111.1 . . ? C114 C113 H11F 111.1 . . ? C112 C113 H11F 111.1 . . ? H11E C113 H11F 109.0 . . ? O11 C114 C113 108.3(7) . . ? O11 C114 H11G 110.0 . . ? C113 C114 H11G 110.0 . . ? O11 C114 H11H 110.0 . . ? C113 C114 H11H 110.0 . . ? H11G C114 H11H 108.4 . . ? C124 O12 C121 106.7(12) . . ? O12 C121 C122 104.2(13) . . ? O12 C121 H12A 110.9 . . ? C122 C121 H12A 110.9 . . ? O12 C121 H12B 110.9 . . ? C122 C121 H12B 110.9 . . ? H12A C121 H12B 108.9 . . ? C123 C122 C121 102.0(18) . . ? C123 C122 H12C 111.4 . . ? C121 C122 H12C 111.4 . . ? C123 C122 H12D 111.4 . . ? C121 C122 H12D 111.4 . . ? H12C C122 H12D 109.2 . . ? C124 C123 C122 108(2) . . ? C124 C123 H12E 110.0 . . ? C122 C123 H12E 110.0 . . ? C124 C123 H12F 110.0 . . ? C122 C123 H12F 110.0 . . ? H12E C123 H12F 108.4 . . ? O12 C124 C123 104.1(14) . . ? O12 C124 H12G 110.9 . . ? C123 C124 H12G 110.9 . . ? O12 C124 H12H 110.9 . . ? C123 C124 H12H 110.9 . . ? H12G C124 H12H 108.9 . . ? 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 O4 V1 O1 C11 -129.5(5) . . . . ? N3 V1 O1 C11 140.3(5) . . . . ? N2 V1 O1 C11 50.7(5) . . . . ? O5 V1 O1 C11 -41.8(5) . . . . ? Cl1 V1 O1 C11 19.7(11) . . . . ? V1 O1 C11 C16 144.3(5) . . . . ? V1 O1 C11 C12 -39.8(8) . . . . ? O1 C11 C12 C13 -178.2(5) . . . . ? C16 C11 C12 C13 -2.2(9) . . . . ? O1 C11 C12 C17 -4.0(9) . . . . ? C16 C11 C12 C17 171.9(6) . . . . ? C11 C12 C13 C14 -0.7(9) . . . . ? C17 C12 C13 C14 -175.0(6) . . . . ? C12 C13 C14 C15 2.4(9) . . . . ? C13 C14 C15 C16 -0.9(10) . . . . ? C14 C15 C16 C11 -2.1(10) . . . . ? O1 C11 C16 C15 179.6(6) . . . . ? C12 C11 C16 C15 3.7(9) . . . . ? C13 C12 C17 N2 -168.8(6) . . . . ? C11 C12 C17 N2 17.1(10) . . . . ? C12 C17 N2 C21 -172.4(6) . . . . ? C12 C17 N2 V1 11.0(8) . . . . ? O4 V1 N2 C17 178(100) . . . . ? O1 V1 N2 C17 -35.6(5) . . . . ? N3 V1 N2 C17 -126.3(5) . . . . ? O5 V1 N2 C17 50.2(5) . . . . ? Cl1 V1 N2 C17 138.9(5) . . . . ? O4 V1 N2 C21 2(45) . . . . ? O1 V1 N2 C21 148.0(5) . . . . ? N3 V1 N2 C21 57.3(5) . . . . ? O5 V1 N2 C21 -126.2(5) . . . . ? Cl1 V1 N2 C21 -37.5(5) . . . . ? C17 N2 C21 C26 -69.1(8) . . . . ? V1 N2 C21 C26 107.5(6) . . . . ? C17 N2 C21 C22 109.6(7) . . . . ? V1 N2 C21 C22 -73.8(7) . . . . ? C26 C21 C22 C23 0.2(10) . . . . ? N2 C21 C22 C23 -178.4(6) . . . . ? C26 C21 C22 C32 171.9(6) . . . . ? N2 C21 C22 C32 -6.7(9) . . . . ? C21 C22 C23 C24 -0.7(10) . . . . ? C32 C22 C23 C24 -172.6(6) . . . . ? C22 C23 C24 C25 1.2(10) . . . . ? C23 C24 C25 C26 -1.2(10) . . . . ? C22 C21 C26 C25 -0.2(10) . . . . ? N2 C21 C26 C25 178.4(6) . . . . ? C24 C25 C26 C21 0.7(10) . . . . ? O4 V1 N3 C47 18.1(5) . . . . ? O1 V1 N3 C47 114.6(5) . . . . ? N2 V1 N3 C47 -161.7(5) . . . . ? O5 V1 N3 C47 82(3) . . . . ? Cl1 V1 N3 C47 -74.8(5) . . . . ? O4 V1 N3 C31 -151.6(5) . . . . ? O1 V1 N3 C31 -55.2(5) . . . . ? N2 V1 N3 C31 28.6(5) . . . . ? O5 V1 N3 C31 -88(3) . . . . ? Cl1 V1 N3 C31 115.5(5) . . . . ? C47 N3 C31 C32 124.8(7) . . . . ? V1 N3 C31 C32 -64.8(7) . . . . ? C47 N3 C31 C36 -52.6(8) . . . . ? V1 N3 C31 C36 117.9(5) . . . . ? C36 C31 C32 C33 2.3(9) . . . . ? N3 C31 C32 C33 -174.9(5) . . . . ? C36 C31 C32 C22 -179.1(6) . . . . ? N3 C31 C32 C22 3.7(10) . . . . ? C23 C22 C32 C31 -133.0(7) . . . . ? C21 C22 C32 C31 55.6(10) . . . . ? C23 C22 C32 C33 45.6(9) . . . . ? C21 C22 C32 C33 -125.8(7) . . . . ? C31 C32 C33 C34 -0.3(10) . . . . ? C22 C32 C33 C34 -179.1(6) . . . . ? C32 C33 C34 C35 -1.7(10) . . . . ? C33 C34 C35 C36 1.6(10) . . . . ? C34 C35 C36 C31 0.3(11) . . . . ? C32 C31 C36 C35 -2.4(10) . . . . ? N3 C31 C36 C35 175.0(6) . . . . ? O1 V1 O4 C41 -122.1(5) . . . . ? N3 V1 O4 C41 -31.4(5) . . . . ? N2 V1 O4 C41 24(45) . . . . ? O5 V1 O4 C41 152.1(5) . . . . ? Cl1 V1 O4 C41 63.4(5) . . . . ? V1 O4 C41 C46 -153.0(5) . . . . ? V1 O4 C41 C42 27.1(9) . . . . ? O4 C41 C42 C43 176.5(6) . . . . ? C46 C41 C42 C43 -3.4(9) . . . . ? O4 C41 C42 C47 0.1(10) . . . . ? C46 C41 C42 C47 -179.8(6) . . . . ? C41 C42 C43 C44 2.6(10) . . . . ? C47 C42 C43 C44 179.2(6) . . . . ? C42 C43 C44 C45 -0.2(10) . . . . ? C43 C44 C45 C46 -1.3(10) . . . . ? C44 C45 C46 C41 0.4(10) . . . . ? O4 C41 C46 C45 -177.9(6) . . . . ? C42 C41 C46 C45 2.0(10) . . . . ? C31 N3 C47 C42 169.0(6) . . . . ? V1 N3 C47 C42 -1.7(9) . . . . ? C43 C42 C47 N3 171.1(6) . . . . ? C41 C42 C47 N3 -12.5(10) . . . . ? O4 V1 O5 C51 36.2(5) . . . . ? O1 V1 O5 C51 -60.4(5) . . . . ? N3 V1 O5 C51 -28(3) . . . . ? N2 V1 O5 C51 -144.0(5) . . . . ? Cl1 V1 O5 C51 129.1(4) . . . . ? O4 V1 O5 C54 -136.8(5) . . . . ? O1 V1 O5 C54 126.6(5) . . . . ? N3 V1 O5 C54 159(3) . . . . ? N2 V1 O5 C54 43.0(5) . . . . ? Cl1 V1 O5 C54 -43.9(5) . . . . ? C54 O5 C51 C52 -31.8(7) . . . . ? V1 O5 C51 C52 154.0(4) . . . . ? O5 C51 C52 C53 38.9(7) . . . . ? C51 C52 C53 C54 -32.1(7) . . . . ? C51 O5 C54 C53 11.0(7) . . . . ? V1 O5 C54 C53 -175.2(4) . . . . ? C52 C53 C54 O5 14.0(8) . . . . ? O9 V2 O6 C61 -132.6(5) . . . . ? N8 V2 O6 C61 137.7(5) . . . . ? N7 V2 O6 C61 46.5(5) . . . . ? O10 V2 O6 C61 -43.1(5) . . . . ? Cl2 V2 O6 C61 27.2(15) . . . . ? V2 O6 C61 C66 143.4(5) . . . . ? V2 O6 C61 C62 -40.3(9) . . . . ? O6 C61 C62 C63 -175.7(7) . . . . ? C66 C61 C62 C63 0.7(10) . . . . ? O6 C61 C62 C67 0.5(11) . . . . ? C66 C61 C62 C67 176.9(6) . . . . ? C67 C62 C63 C64 -179.3(8) . . . . ? C61 C62 C63 C64 -3.1(12) . . . . ? C62 C63 C64 C65 2.6(14) . . . . ? C63 C64 C65 C66 0.3(13) . . . . ? C64 C65 C66 C61 -2.6(12) . . . . ? O6 C61 C66 C65 178.5(7) . . . . ? C62 C61 C66 C65 2.1(11) . . . . ? C63 C62 C67 N7 -168.2(7) . . . . ? C61 C62 C67 N7 15.6(11) . . . . ? C62 C67 N7 C71 -171.3(7) . . . . ? C62 C67 N7 V2 6.9(10) . . . . ? O6 V2 N7 C67 -30.2(5) . . . . ? O9 V2 N7 C67 62(16) . . . . ? N8 V2 N7 C67 -122.4(6) . . . . ? O10 V2 N7 C67 58.1(6) . . . . ? Cl2 V2 N7 C67 147.3(5) . . . . ? O6 V2 N7 C71 147.9(5) . . . . ? O9 V2 N7 C71 -120(16) . . . . ? N8 V2 N7 C71 55.6(5) . . . . ? O10 V2 N7 C71 -123.9(5) . . . . ? Cl2 V2 N7 C71 -34.7(5) . . . . ? C67 N7 C71 C76 -75.0(8) . . . . ? V2 N7 C71 C76 106.8(7) . . . . ? C67 N7 C71 C72 107.7(7) . . . . ? V2 N7 C71 C72 -70.4(7) . . . . ? C76 C71 C72 C73 -1.5(10) . . . . ? N7 C71 C72 C73 175.7(6) . . . . ? C76 C71 C72 C82 170.7(7) . . . . ? N7 C71 C72 C82 -12.1(10) . . . . ? C71 C72 C73 C74 -0.3(11) . . . . ? C82 C72 C73 C74 -172.5(7) . . . . ? C72 C73 C74 C75 1.5(12) . . . . ? C73 C74 C75 C76 -1.1(12) . . . . ? C74 C75 C76 C71 -0.7(12) . . . . ? C72 C71 C76 C75 2.0(11) . . . . ? N7 C71 C76 C75 -175.1(7) . . . . ? O6 V2 N8 C97 116.3(5) . . . . ? O9 V2 N8 C97 21.3(5) . . . . ? N7 V2 N8 C97 -158.6(5) . . . . ? O10 V2 N8 C97 -11(14) . . . . ? Cl2 V2 N8 C97 -70.9(5) . . . . ? O6 V2 N8 C81 -55.0(5) . . . . ? O9 V2 N8 C81 -150.0(5) . . . . ? N7 V2 N8 C81 30.0(5) . . . . ? O10 V2 N8 C81 178(100) . . . . ? Cl2 V2 N8 C81 117.8(5) . . . . ? C97 N8 C81 C82 123.7(7) . . . . ? V2 N8 C81 C82 -64.5(8) . . . . ? C97 N8 C81 C86 -54.5(8) . . . . ? V2 N8 C81 C86 117.2(6) . . . . ? C86 C81 C82 C83 -2.4(10) . . . . ? N8 C81 C82 C83 179.4(6) . . . . ? C86 C81 C82 C72 178.1(6) . . . . ? N8 C81 C82 C72 0.0(11) . . . . ? C73 C72 C82 C81 -125.0(8) . . . . ? C71 C72 C82 C81 63.2(10) . . . . ? C73 C72 C82 C83 55.6(9) . . . . ? C71 C72 C82 C83 -116.2(7) . . . . ? C81 C82 C83 C84 1.8(10) . . . . ? C72 C82 C83 C84 -178.7(7) . . . . ? C82 C83 C84 C85 -0.9(11) . . . . ? C83 C84 C85 C86 0.5(11) . . . . ? C84 C85 C86 C81 -1.1(10) . . . . ? C82 C81 C86 C85 2.2(10) . . . . ? N8 C81 C86 C85 -179.6(6) . . . . ? O6 V2 O9 C91 -129.6(5) . . . . ? N8 V2 O9 C91 -37.3(5) . . . . ? N7 V2 O9 C91 139(16) . . . . ? O10 V2 O9 C91 142.2(5) . . . . ? Cl2 V2 O9 C91 53.0(5) . . . . ? V2 O9 C91 C92 32.3(9) . . . . ? V2 O9 C91 C96 -149.7(5) . . . . ? O9 C91 C92 C93 178.8(7) . . . . ? C96 C91 C92 C93 0.8(11) . . . . ? O9 C91 C92 C97 0.7(11) . . . . ? C96 C91 C92 C97 -177.2(7) . . . . ? C91 C92 C93 C94 2.0(12) . . . . ? C97 C92 C93 C94 -179.8(7) . . . . ? C92 C93 C94 C95 -2.3(12) . . . . ? C93 C94 C95 C96 -0.4(13) . . . . ? C94 C95 C96 C91 3.2(13) . . . . ? O9 C91 C96 C95 178.5(7) . . . . ? C92 C91 C96 C95 -3.4(12) . . . . ? C81 N8 C97 C92 171.6(7) . . . . ? V2 N8 C97 C92 -0.1(10) . . . . ? C91 C92 C97 N8 -17.3(12) . . . . ? C93 C92 C97 N8 164.6(7) . . . . ? O6 V2 O10 C101 122.2(7) . . . . ? O9 V2 O10 C101 -142.7(7) . . . . ? N8 V2 O10 C101 -110(14) . . . . ? N7 V2 O10 C101 37.2(7) . . . . ? Cl2 V2 O10 C101 -50.5(6) . . . . ? O6 V2 O10 C104 -58.0(6) . . . . ? O9 V2 O10 C104 37.0(6) . . . . ? N8 V2 O10 C104 69(14) . . . . ? N7 V2 O10 C104 -143.0(6) . . . . ? Cl2 V2 O10 C104 129.3(6) . . . . ? C104 O10 C101 C102 -6.0(13) . . . . ? V2 O10 C101 C102 173.7(10) . . . . ? O10 C101 C102 C103 26.8(16) . . . . ? C101 C102 C103 C104 -37.7(17) . . . . ? C101 O10 C104 C103 -16.8(10) . . . . ? V2 O10 C104 C103 163.4(7) . . . . ? C102 C103 C104 O10 34.4(15) . . . . ? C114 O11 C111 C112 -35.8(8) . . . . ? O11 C111 C112 C113 34.3(8) . . . . ? C111 C112 C113 C114 -19.6(8) . . . . ? C111 O11 C114 C113 22.4(9) . . . . ? C112 C113 C114 O11 -0.4(9) . . . . ? C124 O12 C121 C122 -30.6(14) . . . . ? O12 C121 C122 C123 10.1(18) . . . . ? C121 C122 C123 C124 13(2) . . . . ? C121 O12 C124 C123 39.6(14) . . . . ? C122 C123 C124 O12 -32.7(19) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.393 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.061 data_lucyc2 _database_code_depnum_ccdc_archive 'CCDC 837292' #TrackingRef 'lucypap3.cif' _audit_creation_method 'SHELXL-97 and CrysAlis RED' _chemical_name_systematic ; ? ; _chemical_name_common 'Compound L5' _chemical_melting_point ? _chemical_formula_structural (4,6-tBu2-HOC6H2-CH=N-C6H4-CH2-)2 _chemical_formula_moiety 'C44 H56 N2 O2' _chemical_formula_sum 'C44 H56 N2 O2' _chemical_formula_weight 644.91 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 9.6297(3) _cell_length_b 12.1792(4) _cell_length_c 16.2276(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.851(4) _cell_angle_gamma 90.00 _cell_volume 1869.18(11) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.904 _exptl_absorpt_correction_T_max 1.118 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 19826 _diffrn_reflns_av_R_equivalents 0.1058 _diffrn_reflns_av_sigmaI/netI 0.0849 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3295 _reflns_number_gt 1981 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Johnson, 1976 and Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008) and WINGX (Farrugia, 1999)' _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^)+(0.0398P)^2^+0.0000P] 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 3295 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1056 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0835 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.926 _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 O1 O 0.74805(15) 0.48739(11) 0.29443(9) 0.0262(4) Uani 1 1 d . . . C1 C 0.6120(2) 0.51639(15) 0.26412(12) 0.0198(5) Uani 1 1 d . . . C2 C 0.5486(2) 0.59995(15) 0.30470(12) 0.0179(5) Uani 1 1 d . . . C3 C 0.4085(2) 0.62962(16) 0.27366(12) 0.0203(5) Uani 1 1 d . . . H3 H 0.3673 0.6846 0.3007 0.024 Uiso 1 1 calc R . . C4 C 0.3289(2) 0.57939(16) 0.20361(12) 0.0205(5) Uani 1 1 d . . . C5 C 0.3971(2) 0.49812(16) 0.16515(12) 0.0219(5) Uani 1 1 d . . . H5 H 0.3456 0.4642 0.1177 0.026 Uiso 1 1 calc R . . C6 C 0.5363(2) 0.46404(16) 0.19240(12) 0.0204(5) Uani 1 1 d . . . C20 C 0.6280(2) 0.65818(15) 0.37673(12) 0.0196(5) Uani 1 1 d . . . H20 H 0.5830 0.7130 0.4018 0.024 Uiso 1 1 calc R . . N20 N 0.75804(17) 0.63645(13) 0.40681(10) 0.0201(4) Uani 1 1 d . . . C21 C 0.8386(2) 0.69842(15) 0.47347(12) 0.0188(5) Uani 1 1 d . . . C22 C 0.9367(2) 0.64170(15) 0.53302(12) 0.0195(5) Uani 1 1 d . . . C23 C 1.0224(2) 0.70232(18) 0.59501(13) 0.0271(5) Uani 1 1 d . . . H23 H 1.0878 0.6658 0.6352 0.033 Uiso 1 1 calc R . . C24 C 1.0132(2) 0.81561(17) 0.59878(14) 0.0297(6) Uani 1 1 d . . . H24 H 1.0725 0.8544 0.6407 0.036 Uiso 1 1 calc R . . C25 C 0.9155(2) 0.87065(17) 0.53999(13) 0.0246(5) Uani 1 1 d . . . H25 H 0.9082 0.9467 0.5424 0.030 Uiso 1 1 calc R . . C26 C 0.8283(2) 0.81220(15) 0.47730(12) 0.0211(5) Uani 1 1 d . . . H26 H 0.7626 0.8493 0.4376 0.025 Uiso 1 1 calc R . . C27 C 0.9502(2) 0.51861(15) 0.52894(12) 0.0223(5) Uani 1 1 d . . . H27A H 0.8574 0.4872 0.5092 0.027 Uiso 1 1 calc R . . H27B H 0.9851 0.4906 0.5850 0.027 Uiso 1 1 calc R . . C41 C 0.1761(2) 0.61445(17) 0.17147(13) 0.0237(5) Uani 1 1 d . . . C42 C 0.1726(2) 0.73715(18) 0.14817(14) 0.0330(6) Uani 1 1 d . . . H42A H 0.0765 0.7595 0.1283 0.050 Uiso 1 1 calc R . . H42B H 0.2267 0.7488 0.1049 0.050 Uiso 1 1 calc R . . H42C H 0.2123 0.7796 0.1968 0.050 Uiso 1 1 calc R . . C43 C 0.0894(2) 0.59536(18) 0.24078(13) 0.0317(6) Uani 1 1 d . . . H43A H -0.0067 0.6178 0.2210 0.048 Uiso 1 1 calc R . . H43B H 0.1291 0.6376 0.2895 0.048 Uiso 1 1 calc R . . H43C H 0.0916 0.5188 0.2551 0.048 Uiso 1 1 calc R . . C44 C 0.1051(2) 0.54976(18) 0.09415(13) 0.0321(6) Uani 1 1 d . . . H44A H 0.0096 0.5750 0.0766 0.048 Uiso 1 1 calc R . . H44B H 0.1045 0.4731 0.1078 0.048 Uiso 1 1 calc R . . H44C H 0.1565 0.5606 0.0495 0.048 Uiso 1 1 calc R . . C61 C 0.6052(2) 0.37515(16) 0.14637(13) 0.0248(5) Uani 1 1 d . . . C62 C 0.5061(2) 0.33520(17) 0.06675(14) 0.0347(6) Uani 1 1 d . . . H62A H 0.5531 0.2800 0.0399 0.052 Uiso 1 1 calc R . . H62B H 0.4812 0.3959 0.0291 0.052 Uiso 1 1 calc R . . H62C H 0.4221 0.3047 0.0814 0.052 Uiso 1 1 calc R . . C63 C 0.6443(3) 0.27506(16) 0.20408(14) 0.0351(6) Uani 1 1 d . . . H63A H 0.7067 0.2977 0.2545 0.053 Uiso 1 1 calc R . . H63B H 0.6905 0.2210 0.1757 0.053 Uiso 1 1 calc R . . H63C H 0.5599 0.2441 0.2181 0.053 Uiso 1 1 calc R . . C64 C 0.7386(2) 0.42145(18) 0.11933(14) 0.0355(6) Uani 1 1 d . . . H64A H 0.8030 0.4476 0.1678 0.053 Uiso 1 1 calc R . . H64B H 0.7126 0.4810 0.0807 0.053 Uiso 1 1 calc R . . H64C H 0.7832 0.3647 0.0926 0.053 Uiso 1 1 calc R . . H1O H 0.781(3) 0.537(2) 0.3436(18) 0.078(9) Uiso 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 O1 0.0204(9) 0.0252(9) 0.0311(9) -0.0053(7) -0.0002(7) 0.0050(7) C1 0.0171(12) 0.0178(11) 0.0245(12) 0.0015(9) 0.0042(10) 0.0008(9) C2 0.0195(12) 0.0157(12) 0.0186(11) 0.0013(9) 0.0037(9) -0.0027(9) C3 0.0207(12) 0.0186(11) 0.0227(12) -0.0019(9) 0.0071(10) 0.0009(9) C4 0.0204(12) 0.0202(12) 0.0209(11) 0.0010(9) 0.0040(10) -0.0014(9) C5 0.0231(13) 0.0215(12) 0.0207(11) -0.0013(9) 0.0035(10) -0.0048(9) C6 0.0216(13) 0.0178(12) 0.0219(12) -0.0010(9) 0.0046(10) -0.0011(9) C20 0.0198(13) 0.0178(12) 0.0223(12) 0.0012(9) 0.0066(10) -0.0005(9) N20 0.0184(10) 0.0189(10) 0.0221(10) -0.0017(8) 0.0019(8) 0.0002(7) C21 0.0177(12) 0.0197(12) 0.0201(12) -0.0030(9) 0.0063(10) -0.0018(9) C22 0.0185(12) 0.0184(12) 0.0219(11) 0.0003(9) 0.0048(10) 0.0024(9) C23 0.0214(13) 0.0291(14) 0.0282(13) -0.0017(10) -0.0025(11) 0.0036(10) C24 0.0290(14) 0.0275(14) 0.0304(13) -0.0091(10) 0.0001(11) 0.0011(10) C25 0.0264(13) 0.0157(11) 0.0318(13) -0.0062(10) 0.0057(11) 0.0024(9) C26 0.0197(12) 0.0208(12) 0.0231(12) -0.0005(9) 0.0049(10) 0.0049(9) C27 0.0197(12) 0.0221(12) 0.0243(12) -0.0004(9) 0.0022(10) 0.0000(9) C41 0.0196(12) 0.0273(13) 0.0232(12) -0.0027(9) 0.0016(10) 0.0000(9) C42 0.0246(13) 0.0359(14) 0.0364(14) 0.0005(11) 0.0004(11) 0.0058(10) C43 0.0247(14) 0.0400(15) 0.0302(13) -0.0055(11) 0.0048(11) -0.0008(10) C44 0.0219(13) 0.0435(15) 0.0285(13) -0.0069(11) -0.0011(11) 0.0034(10) C61 0.0258(13) 0.0207(12) 0.0279(12) -0.0063(9) 0.0051(10) 0.0017(9) C62 0.0381(15) 0.0295(14) 0.0354(14) -0.0120(11) 0.0036(12) 0.0041(11) C63 0.0447(16) 0.0216(13) 0.0383(14) -0.0073(10) 0.0062(12) 0.0046(11) C64 0.0333(15) 0.0382(14) 0.0371(14) -0.0063(11) 0.0120(12) 0.0031(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 O1 C1 1.357(2) . ? O1 H1O 1.00(3) . ? C1 C6 1.404(3) . ? C1 C2 1.412(3) . ? C2 C3 1.396(3) . ? C2 C20 1.455(3) . ? C3 C4 1.388(3) . ? C3 H3 0.9300 . ? C4 C5 1.398(3) . ? C4 C41 1.526(3) . ? C5 C6 1.394(3) . ? C5 H5 0.9300 . ? C6 C61 1.535(3) . ? C20 N20 1.283(2) . ? C20 H20 0.9300 . ? N20 C21 1.423(2) . ? C21 C26 1.392(2) . ? C21 C22 1.400(3) . ? C22 C23 1.387(3) . ? C22 C27 1.507(3) . ? C23 C24 1.385(3) . ? C23 H23 0.9300 . ? C24 C25 1.381(3) . ? C24 H24 0.9300 . ? C25 C26 1.387(3) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C27 1.532(4) 3_766 ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C41 C44 1.530(3) . ? C41 C43 1.539(3) . ? C41 C42 1.540(3) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C61 C62 1.533(3) . ? C61 C63 1.540(3) . ? C61 C64 1.540(3) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 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 C1 O1 H1O 105.8(16) . . ? O1 C1 C6 119.80(18) . . ? O1 C1 C2 119.41(17) . . ? C6 C1 C2 120.78(18) . . ? C3 C2 C1 119.44(18) . . ? C3 C2 C20 119.30(18) . . ? C1 C2 C20 121.23(18) . . ? C4 C3 C2 121.91(19) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C3 C4 C5 116.37(19) . . ? C3 C4 C41 120.31(18) . . ? C5 C4 C41 123.31(18) . . ? C6 C5 C4 125.03(19) . . ? C6 C5 H5 117.5 . . ? C4 C5 H5 117.5 . . ? C5 C6 C1 116.46(18) . . ? C5 C6 C61 122.23(18) . . ? C1 C6 C61 121.30(18) . . ? N20 C20 C2 122.17(19) . . ? N20 C20 H20 118.9 . . ? C2 C20 H20 118.9 . . ? C20 N20 C21 122.22(17) . . ? C26 C21 C22 120.34(19) . . ? C26 C21 N20 121.91(18) . . ? C22 C21 N20 117.62(18) . . ? C23 C22 C21 118.02(19) . . ? C23 C22 C27 121.11(19) . . ? C21 C22 C27 120.86(18) . . ? C24 C23 C22 121.9(2) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C25 C24 C23 119.6(2) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 119.8(2) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C26 C21 120.3(2) . . ? C25 C26 H26 119.8 . . ? C21 C26 H26 119.8 . . ? C22 C27 C27 113.0(2) . 3_766 ? C22 C27 H27A 109.0 . . ? C27 C27 H27A 109.0 3_766 . ? C22 C27 H27B 109.0 . . ? C27 C27 H27B 109.0 3_766 . ? H27A C27 H27B 107.8 . . ? C4 C41 C44 112.93(17) . . ? C4 C41 C43 109.19(17) . . ? C44 C41 C43 107.52(17) . . ? C4 C41 C42 109.30(16) . . ? C44 C41 C42 108.21(18) . . ? C43 C41 C42 109.64(17) . . ? 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 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? 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 . . ? C62 C61 C6 112.14(17) . . ? C62 C61 C63 107.65(17) . . ? C6 C61 C63 109.93(17) . . ? C62 C61 C64 107.21(18) . . ? C6 C61 C64 109.87(17) . . ? C63 C61 C64 109.97(18) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -179.82(17) . . . . ? C6 C1 C2 C3 0.9(3) . . . . ? O1 C1 C2 C20 2.1(3) . . . . ? C6 C1 C2 C20 -177.16(18) . . . . ? C1 C2 C3 C4 -0.1(3) . . . . ? C20 C2 C3 C4 177.98(18) . . . . ? C2 C3 C4 C5 -0.6(3) . . . . ? C2 C3 C4 C41 -179.79(18) . . . . ? C3 C4 C5 C6 0.7(3) . . . . ? C41 C4 C5 C6 179.83(19) . . . . ? C4 C5 C6 C1 0.0(3) . . . . ? C4 C5 C6 C61 -179.22(19) . . . . ? O1 C1 C6 C5 179.89(17) . . . . ? C2 C1 C6 C5 -0.8(3) . . . . ? O1 C1 C6 C61 -0.9(3) . . . . ? C2 C1 C6 C61 178.41(18) . . . . ? C3 C2 C20 N20 -178.29(18) . . . . ? C1 C2 C20 N20 -0.2(3) . . . . ? C2 C20 N20 C21 175.49(17) . . . . ? C20 N20 C21 C26 -40.9(3) . . . . ? C20 N20 C21 C22 143.25(19) . . . . ? C26 C21 C22 C23 -0.2(3) . . . . ? N20 C21 C22 C23 175.78(18) . . . . ? C26 C21 C22 C27 -179.23(18) . . . . ? N20 C21 C22 C27 -3.3(3) . . . . ? C21 C22 C23 C24 -0.3(3) . . . . ? C27 C22 C23 C24 178.8(2) . . . . ? C22 C23 C24 C25 0.6(3) . . . . ? C23 C24 C25 C26 -0.5(3) . . . . ? C24 C25 C26 C21 0.1(3) . . . . ? C22 C21 C26 C25 0.2(3) . . . . ? N20 C21 C26 C25 -175.53(19) . . . . ? C23 C22 C27 C27 -93.3(3) . . . 3_766 ? C21 C22 C27 C27 85.7(3) . . . 3_766 ? C3 C4 C41 C44 -179.71(19) . . . . ? C5 C4 C41 C44 1.2(3) . . . . ? C3 C4 C41 C43 -60.1(2) . . . . ? C5 C4 C41 C43 120.8(2) . . . . ? C3 C4 C41 C42 59.8(2) . . . . ? C5 C4 C41 C42 -119.3(2) . . . . ? C5 C6 C61 C62 3.0(3) . . . . ? C1 C6 C61 C62 -176.19(18) . . . . ? C5 C6 C61 C63 -116.7(2) . . . . ? C1 C6 C61 C63 64.1(2) . . . . ? C5 C6 C61 C64 122.1(2) . . . . ? C1 C6 C61 C64 -57.1(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1O N20 1.00(3) 1.63(3) 2.562(2) 152(2) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.158 _refine_diff_density_min -0.154 _refine_diff_density_rms 0.037 data_lucy3a _database_code_depnum_ccdc_archive 'CCDC 837293' #TrackingRef 'lucypap3.cif' _audit_creation_method 'SHELXL-97 and CrysAlisPro RED' _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 5' _chemical_melting_point ? _chemical_formula_structural '[{V Cl2 (thf)2}2 (OC6H2-4,6-bis-tBu,-2-CHNC6H4CH2-)2]' _chemical_formula_moiety 'C60 H86 Cl4 N2 O6 V2' _chemical_formula_sum 'C60 H86 Cl4 N2 O6 V2' _chemical_formula_weight 1174.99 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' 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' Cl Cl 0.1484 0.1585 '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 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 15.4851(3) _cell_length_b 12.3449(2) _cell_length_c 33.0323(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6314.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2488 _exptl_absorpt_coefficient_mu 0.512 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.982 _exptl_absorpt_correction_T_max 1.020 _exptl_absorpt_process_details ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 104961 _diffrn_reflns_av_R_equivalents 0.0724 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5557 _reflns_number_gt 4572 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlisPro CCD, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_cell_refinement ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_data_reduction ; CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.32.24 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Johnson, 1976 and Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008) and WINGX (Farrugia, 1999)' _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^)+(0.0358P)^2^+7.2289P] 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 5557 _refine_ls_number_parameters 339 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0867 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1129 _refine_ls_wR_factor_gt 0.1045 _refine_ls_goodness_of_fit_ref 1.199 _refine_ls_restrained_S_all 1.199 _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 0.40865(3) 0.25662(4) 0.604988(14) 0.01758(13) Uani 1 1 d . A . Cl3 Cl 0.45466(5) 0.07494(6) 0.60741(2) 0.0284(2) Uani 1 1 d . . . Cl4 Cl 0.35347(5) 0.43437(6) 0.60121(2) 0.02729(19) Uani 1 1 d . . . O1 O 0.47932(13) 0.29612(16) 0.64845(6) 0.0201(5) Uani 1 1 d . . . C11 C 0.54088(19) 0.3711(2) 0.65061(9) 0.0187(7) Uani 1 1 d . . . C12 C 0.5862(2) 0.4036(2) 0.61584(8) 0.0179(6) Uani 1 1 d . . . C13 C 0.6536(2) 0.4792(2) 0.61839(9) 0.0253(7) Uani 1 1 d . . . H13 H 0.6836 0.4977 0.5950 0.030 Uiso 1 1 calc R . . C14 C 0.6765(2) 0.5264(3) 0.65422(10) 0.0310(8) Uani 1 1 d . . . C15 C 0.6301(2) 0.4927(3) 0.68856(10) 0.0301(8) Uani 1 1 d . . . H15 H 0.6450 0.5236 0.7133 0.036 Uiso 1 1 calc R . . C16 C 0.5642(2) 0.4172(2) 0.68851(9) 0.0227(7) Uani 1 1 d . . . C141 C 0.7515(3) 0.6075(3) 0.65775(11) 0.0474(11) Uani 1 1 d . . . C142 C 0.7205(3) 0.7091(3) 0.67929(16) 0.0699(15) Uani 1 1 d . . . H14A H 0.6751 0.7422 0.6638 0.105 Uiso 1 1 calc R . . H14B H 0.7677 0.7591 0.6820 0.105 Uiso 1 1 calc R . . H14C H 0.6992 0.6903 0.7057 0.105 Uiso 1 1 calc R . . C143 C 0.8244(3) 0.5547(4) 0.68189(14) 0.0564(12) Uani 1 1 d . . . H14D H 0.8442 0.4911 0.6679 0.085 Uiso 1 1 calc R . . H14E H 0.8036 0.5348 0.7082 0.085 Uiso 1 1 calc R . . H14F H 0.8714 0.6049 0.6847 0.085 Uiso 1 1 calc R . . C144 C 0.7890(4) 0.6365(4) 0.61607(14) 0.0808(19) Uani 1 1 d . . . H14G H 0.8086 0.5718 0.6028 0.121 Uiso 1 1 calc R . . H14H H 0.8367 0.6854 0.6194 0.121 Uiso 1 1 calc R . . H14I H 0.7452 0.6705 0.5999 0.121 Uiso 1 1 calc R . . C161 C 0.5162(2) 0.3848(3) 0.72742(9) 0.0260(7) Uani 1 1 d . . . C162 C 0.4202(2) 0.4145(3) 0.72335(11) 0.0404(9) Uani 1 1 d . . . H16A H 0.3902 0.3944 0.7476 0.061 Uiso 1 1 calc R . . H16B H 0.3958 0.3766 0.7007 0.061 Uiso 1 1 calc R . . H16C H 0.4148 0.4911 0.7191 0.061 Uiso 1 1 calc R . . C163 C 0.5255(2) 0.2631(3) 0.73517(9) 0.0280(8) Uani 1 1 d . . . H16D H 0.4950 0.2441 0.7595 0.042 Uiso 1 1 calc R . . H16E H 0.5855 0.2452 0.7382 0.042 Uiso 1 1 calc R . . H16F H 0.5017 0.2236 0.7127 0.042 Uiso 1 1 calc R . . C164 C 0.5518(3) 0.4438(3) 0.76488(10) 0.0416(10) Uani 1 1 d . . . H16G H 0.5200 0.4216 0.7884 0.062 Uiso 1 1 calc R . . H16H H 0.5458 0.5206 0.7613 0.062 Uiso 1 1 calc R . . H16I H 0.6117 0.4260 0.7683 0.062 Uiso 1 1 calc R . . C121 C 0.57059(19) 0.3589(2) 0.57627(9) 0.0170(6) Uani 1 1 d . . . H121 H 0.6111 0.3758 0.5565 0.020 Uiso 1 1 calc R . . N2 N 0.50749(15) 0.29849(19) 0.56498(7) 0.0159(5) Uani 1 1 d . . . C21 C 0.50909(19) 0.2677(2) 0.52250(9) 0.0182(7) Uani 1 1 d . . . C22 C 0.5306(2) 0.1619(2) 0.51259(10) 0.0262(8) Uani 1 1 d . . . H22 H 0.5421 0.1117 0.5329 0.031 Uiso 1 1 calc R . . C23 C 0.5347(2) 0.1315(3) 0.47220(11) 0.0360(9) Uani 1 1 d . . . H23 H 0.5491 0.0607 0.4653 0.043 Uiso 1 1 calc R . . C24 C 0.5173(2) 0.2066(3) 0.44220(10) 0.0364(9) Uani 1 1 d . . . H24 H 0.5204 0.1864 0.4151 0.044 Uiso 1 1 calc R . . C25 C 0.4956(2) 0.3112(3) 0.45244(10) 0.0318(8) Uani 1 1 d . . . H25 H 0.4842 0.3611 0.4320 0.038 Uiso 1 1 calc R . . C26 C 0.4902(2) 0.3442(2) 0.49303(9) 0.0216(7) Uani 1 1 d . . . C27 C 0.4636(2) 0.4588(2) 0.50261(9) 0.0226(7) Uani 1 1 d . . . H27A H 0.4431 0.4618 0.5303 0.027 Uiso 1 1 calc R . . H27B H 0.4160 0.4789 0.4851 0.027 Uiso 1 1 calc R . . O5 O 0.30551(15) 0.21673(19) 0.64384(7) 0.0306(6) Uani 1 1 d . . . C51 C 0.3112(3) 0.1424(3) 0.67742(12) 0.0509(11) Uani 0.785(17) 1 d P A 1 H51A H 0.3613 0.1579 0.6940 0.061 Uiso 0.785(17) 1 calc PR A 1 H51B H 0.3144 0.0681 0.6680 0.061 Uiso 0.785(17) 1 calc PR A 1 C52 C 0.2284(4) 0.1624(8) 0.70062(17) 0.054(3) Uani 0.785(17) 1 d P A 1 H52A H 0.2106 0.0977 0.7151 0.065 Uiso 0.785(17) 1 calc PR A 1 H52B H 0.2357 0.2210 0.7199 0.065 Uiso 0.785(17) 1 calc PR A 1 C53 C 0.1660(3) 0.1910(4) 0.66989(12) 0.0518(12) Uani 0.785(17) 1 d P A 1 H53A H 0.1190 0.2333 0.6812 0.062 Uiso 0.785(17) 1 calc PR A 1 H53B H 0.1425 0.1270 0.6569 0.062 Uiso 0.785(17) 1 calc PR A 1 C54 C 0.2174(2) 0.2559(4) 0.64119(14) 0.0618(13) Uani 1 1 d . A . H54A H 0.1955 0.2472 0.6139 0.074 Uiso 1 1 calc R B 1 H54B H 0.2148 0.3321 0.6483 0.074 Uiso 1 1 calc R B 1 O6 O 0.32359(13) 0.21482(17) 0.55730(6) 0.0252(5) Uani 1 1 d . . . C61 C 0.2880(3) 0.1087(3) 0.54971(15) 0.0686(16) Uani 1 1 d . A . H61A H 0.3331 0.0544 0.5519 0.082 Uiso 1 1 calc R . . H61B H 0.2439 0.0924 0.5697 0.082 Uiso 1 1 calc R . . C62 C 0.2517(4) 0.1062(4) 0.51049(14) 0.087(2) Uani 1 1 d . . . H62A H 0.1901 0.0922 0.5120 0.105 Uiso 1 1 calc R A . H62B H 0.2784 0.0495 0.4944 0.105 Uiso 1 1 calc R . . C63 C 0.2684(3) 0.2157(3) 0.49164(11) 0.0501(11) Uani 1 1 d . A . H63A H 0.3182 0.2136 0.4739 0.060 Uiso 1 1 calc R . . H63B H 0.2186 0.2406 0.4764 0.060 Uiso 1 1 calc R . . C64 C 0.2847(2) 0.2864(3) 0.52751(10) 0.0323(8) Uani 1 1 d . A . H64A H 0.3237 0.3450 0.5206 0.039 Uiso 1 1 calc R . . H64B H 0.2312 0.3168 0.5377 0.039 Uiso 1 1 calc R . . C51X C 0.3112(3) 0.1424(3) 0.67742(12) 0.0509(11) Uani 0.215(17) 1 d P A 2 H51X H 0.3515 0.0854 0.6703 0.061 Uiso 0.215(17) 1 calc PR A 2 H51Y H 0.3352 0.1809 0.7004 0.061 Uiso 0.215(17) 1 calc PR A 2 C52X C 0.2399(13) 0.098(2) 0.6885(8) 0.046(7) Uiso 0.215(17) 1 d P A 2 H52X H 0.2362 0.0918 0.7177 0.055 Uiso 0.215(17) 1 calc PR A 2 H52Y H 0.2323 0.0275 0.6763 0.055 Uiso 0.215(17) 1 calc PR A 2 C53X C 0.1660(3) 0.1910(4) 0.66989(12) 0.0518(12) Uani 0.215(17) 1 d P A 2 H53X H 0.1186 0.1548 0.6562 0.062 Uiso 0.215(17) 1 calc PR A 2 H53Y H 0.1429 0.2359 0.6914 0.062 Uiso 0.215(17) 1 calc PR A 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 0.0187(3) 0.0181(3) 0.0160(2) 0.0011(2) 0.0003(2) -0.0024(2) Cl3 0.0381(5) 0.0191(4) 0.0279(4) 0.0007(3) -0.0029(4) 0.0008(3) Cl4 0.0297(4) 0.0236(4) 0.0286(4) 0.0018(3) 0.0031(4) 0.0065(3) O1 0.0212(11) 0.0223(11) 0.0169(11) 0.0006(9) 0.0015(9) -0.0023(9) C11 0.0219(17) 0.0162(15) 0.0181(15) -0.0005(12) -0.0034(13) 0.0038(13) C12 0.0221(16) 0.0150(15) 0.0165(15) 0.0006(12) -0.0044(12) 0.0016(13) C13 0.0295(18) 0.0239(17) 0.0225(16) 0.0062(14) -0.0056(14) -0.0078(15) C14 0.040(2) 0.0273(18) 0.0255(18) 0.0054(15) -0.0158(16) -0.0097(16) C15 0.049(2) 0.0221(17) 0.0195(17) -0.0002(14) -0.0141(16) -0.0056(16) C16 0.0327(19) 0.0161(15) 0.0194(16) -0.0004(13) -0.0065(14) 0.0053(14) C141 0.065(3) 0.040(2) 0.036(2) 0.0058(18) -0.018(2) -0.033(2) C142 0.076(4) 0.034(2) 0.100(4) -0.002(3) -0.030(3) -0.019(2) C143 0.048(3) 0.062(3) 0.059(3) -0.008(2) -0.017(2) -0.020(2) C144 0.097(4) 0.092(4) 0.054(3) 0.015(3) -0.017(3) -0.074(3) C161 0.035(2) 0.0260(17) 0.0167(16) -0.0027(14) -0.0037(14) 0.0056(15) C162 0.049(2) 0.045(2) 0.0275(19) -0.0012(17) 0.0049(17) 0.018(2) C163 0.0362(19) 0.0297(18) 0.0181(16) 0.0020(14) -0.0008(14) 0.0032(16) C164 0.068(3) 0.037(2) 0.0197(18) -0.0081(16) -0.0023(18) 0.000(2) C121 0.0174(16) 0.0165(15) 0.0172(15) 0.0042(12) 0.0005(12) 0.0009(13) N2 0.0181(13) 0.0146(12) 0.0149(12) 0.0002(10) -0.0016(10) 0.0005(11) C21 0.0180(16) 0.0203(16) 0.0163(15) -0.0039(12) 0.0029(12) -0.0054(13) C22 0.0320(19) 0.0196(17) 0.0271(18) -0.0027(14) 0.0042(15) -0.0032(14) C23 0.043(2) 0.0277(19) 0.037(2) -0.0175(16) 0.0109(17) -0.0085(17) C24 0.047(2) 0.044(2) 0.0176(18) -0.0129(16) 0.0051(16) -0.0115(18) C25 0.042(2) 0.037(2) 0.0172(17) 0.0001(15) -0.0008(15) -0.0066(17) C26 0.0211(17) 0.0254(17) 0.0182(16) -0.0011(13) -0.0002(13) -0.0062(13) C27 0.0276(18) 0.0254(17) 0.0148(15) 0.0037(13) -0.0005(13) -0.0011(14) O5 0.0251(12) 0.0376(14) 0.0290(13) 0.0103(11) 0.0074(10) -0.0029(10) C51 0.059(3) 0.054(3) 0.040(2) 0.027(2) 0.016(2) -0.004(2) C52 0.049(4) 0.086(6) 0.027(3) 0.010(3) 0.015(3) -0.023(4) C53 0.043(3) 0.072(3) 0.040(2) -0.012(2) 0.020(2) -0.021(2) C54 0.030(2) 0.092(4) 0.063(3) 0.022(3) 0.019(2) 0.006(3) O6 0.0240(12) 0.0247(12) 0.0269(12) 0.0067(9) -0.0054(10) -0.0083(10) C61 0.090(4) 0.036(2) 0.080(3) 0.015(2) -0.053(3) -0.029(2) C62 0.148(5) 0.060(3) 0.055(3) 0.011(2) -0.048(3) -0.052(3) C63 0.057(3) 0.059(3) 0.034(2) 0.0070(19) -0.018(2) -0.025(2) C64 0.0269(19) 0.036(2) 0.034(2) 0.0138(16) -0.0072(16) -0.0062(16) C51X 0.059(3) 0.054(3) 0.040(2) 0.027(2) 0.016(2) -0.004(2) C53X 0.043(3) 0.072(3) 0.040(2) -0.012(2) 0.020(2) -0.021(2) _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 1.870(2) . ? V1 N2 2.087(2) . ? V1 O5 2.107(2) . ? V1 O6 2.117(2) . ? V1 Cl3 2.3546(9) . ? V1 Cl4 2.3581(9) . ? O1 C11 1.331(4) . ? C11 C12 1.405(4) . ? C11 C16 1.422(4) . ? C12 C13 1.402(4) . ? C12 C121 1.439(4) . ? C13 C14 1.366(4) . ? C13 H13 0.9300 . ? C14 C15 1.406(5) . ? C14 C141 1.538(5) . ? C15 C16 1.382(5) . ? C15 H15 0.9300 . ? C16 C161 1.537(4) . ? C141 C142 1.521(6) . ? C141 C143 1.528(6) . ? C141 C144 1.536(6) . ? C142 H14A 0.9600 . ? C142 H14B 0.9600 . ? C142 H14C 0.9600 . ? C143 H14D 0.9600 . ? C143 H14E 0.9600 . ? C143 H14F 0.9600 . ? C144 H14G 0.9600 . ? C144 H14H 0.9600 . ? C144 H14I 0.9600 . ? C161 C163 1.531(4) . ? C161 C162 1.537(5) . ? C161 C164 1.537(4) . ? C162 H16A 0.9600 . ? C162 H16B 0.9600 . ? C162 H16C 0.9600 . ? C163 H16D 0.9600 . ? C163 H16E 0.9600 . ? C163 H16F 0.9600 . ? C164 H16G 0.9600 . ? C164 H16H 0.9600 . ? C164 H16I 0.9600 . ? C121 N2 1.285(4) . ? C121 H121 0.9300 . ? N2 C21 1.454(4) . ? C21 C22 1.387(4) . ? C21 C26 1.387(4) . ? C22 C23 1.388(5) . ? C22 H22 0.9300 . ? C23 C24 1.384(5) . ? C23 H23 0.9300 . ? C24 C25 1.377(5) . ? C24 H24 0.9300 . ? C25 C26 1.404(4) . ? C25 H25 0.9300 . ? C26 C27 1.507(4) . ? C27 C27 1.528(6) 5_666 ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? O5 C51 1.442(4) . ? O5 C54 1.450(4) . ? C51 C52 1.514(8) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.446(7) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.475(5) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? O6 C61 1.444(4) . ? O6 C64 1.453(4) . ? C61 C62 1.412(6) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.511(6) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.493(5) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C52X H52X 0.9700 . ? C52X H52Y 0.9700 . ? 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 89.56(9) . . ? O1 V1 O5 92.12(9) . . ? N2 V1 O5 177.87(9) . . ? O1 V1 O6 177.31(9) . . ? N2 V1 O6 92.60(9) . . ? O5 V1 O6 85.68(9) . . ? O1 V1 Cl3 92.59(7) . . ? N2 V1 Cl3 92.04(7) . . ? O5 V1 Cl3 89.20(7) . . ? O6 V1 Cl3 88.94(6) . . ? O1 V1 Cl4 90.57(7) . . ? N2 V1 Cl4 90.10(7) . . ? O5 V1 Cl4 88.57(7) . . ? O6 V1 Cl4 87.82(6) . . ? Cl3 V1 Cl4 176.20(4) . . ? C11 O1 V1 129.93(18) . . ? O1 C11 C12 120.9(3) . . ? O1 C11 C16 120.5(3) . . ? C12 C11 C16 118.6(3) . . ? C13 C12 C11 120.9(3) . . ? C13 C12 C121 115.8(3) . . ? C11 C12 C121 123.3(3) . . ? C14 C13 C12 121.9(3) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C13 C14 C15 116.1(3) . . ? C13 C14 C141 122.6(3) . . ? C15 C14 C141 121.2(3) . . ? C16 C15 C14 125.2(3) . . ? C16 C15 H15 117.4 . . ? C14 C15 H15 117.4 . . ? C15 C16 C11 117.3(3) . . ? C15 C16 C161 122.1(3) . . ? C11 C16 C161 120.6(3) . . ? C142 C141 C143 110.0(3) . . ? C142 C141 C144 110.2(4) . . ? C143 C141 C144 106.8(4) . . ? C142 C141 C14 109.5(4) . . ? C143 C141 C14 108.7(3) . . ? C144 C141 C14 111.7(3) . . ? C141 C142 H14A 109.5 . . ? C141 C142 H14B 109.5 . . ? H14A C142 H14B 109.5 . . ? C141 C142 H14C 109.5 . . ? H14A C142 H14C 109.5 . . ? H14B C142 H14C 109.5 . . ? C141 C143 H14D 109.5 . . ? C141 C143 H14E 109.5 . . ? H14D C143 H14E 109.5 . . ? C141 C143 H14F 109.5 . . ? H14D C143 H14F 109.5 . . ? H14E C143 H14F 109.5 . . ? C141 C144 H14G 109.5 . . ? C141 C144 H14H 109.5 . . ? H14G C144 H14H 109.5 . . ? C141 C144 H14I 109.5 . . ? H14G C144 H14I 109.5 . . ? H14H C144 H14I 109.5 . . ? C163 C161 C162 109.8(3) . . ? C163 C161 C16 110.5(3) . . ? C162 C161 C16 109.4(3) . . ? C163 C161 C164 107.2(3) . . ? C162 C161 C164 107.7(3) . . ? C16 C161 C164 112.1(3) . . ? C161 C162 H16A 109.5 . . ? C161 C162 H16B 109.5 . . ? H16A C162 H16B 109.5 . . ? C161 C162 H16C 109.5 . . ? H16A C162 H16C 109.5 . . ? H16B C162 H16C 109.5 . . ? C161 C163 H16D 109.5 . . ? C161 C163 H16E 109.5 . . ? H16D C163 H16E 109.5 . . ? C161 C163 H16F 109.5 . . ? H16D C163 H16F 109.5 . . ? H16E C163 H16F 109.5 . . ? C161 C164 H16G 109.5 . . ? C161 C164 H16H 109.5 . . ? H16G C164 H16H 109.5 . . ? C161 C164 H16I 109.5 . . ? H16G C164 H16I 109.5 . . ? H16H C164 H16I 109.5 . . ? N2 C121 C12 127.9(3) . . ? N2 C121 H121 116.1 . . ? C12 C121 H121 116.1 . . ? C121 N2 C21 114.8(2) . . ? C121 N2 V1 121.2(2) . . ? C21 N2 V1 123.98(18) . . ? C22 C21 C26 121.7(3) . . ? C22 C21 N2 118.6(3) . . ? C26 C21 N2 119.7(3) . . ? C21 C22 C23 119.5(3) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C24 C23 C22 119.9(3) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C25 C24 C23 120.0(3) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 121.4(3) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C21 C26 C25 117.4(3) . . ? C21 C26 C27 123.3(3) . . ? C25 C26 C27 119.3(3) . . ? C26 C27 C27 113.6(3) . 5_666 ? C26 C27 H27A 108.9 . . ? C27 C27 H27A 108.9 5_666 . ? C26 C27 H27B 108.9 . . ? C27 C27 H27B 108.9 5_666 . ? H27A C27 H27B 107.7 . . ? C51 O5 C54 108.4(3) . . ? C51 O5 V1 124.8(2) . . ? C54 O5 V1 126.7(2) . . ? O5 C51 C52 103.5(4) . . ? O5 C51 H51A 111.1 . . ? C52 C51 H51A 111.1 . . ? O5 C51 H51B 111.1 . . ? C52 C51 H51B 111.1 . . ? H51A C51 H51B 109.0 . . ? C53 C52 C51 104.5(4) . . ? C53 C52 H52A 110.8 . . ? C51 C52 H52A 110.8 . . ? C53 C52 H52B 110.8 . . ? C51 C52 H52B 110.8 . . ? H52A C52 H52B 108.9 . . ? C52 C53 C54 102.9(4) . . ? C52 C53 H53A 111.2 . . ? C54 C53 H53A 111.2 . . ? C52 C53 H53B 111.2 . . ? C54 C53 H53B 111.2 . . ? H53A C53 H53B 109.1 . . ? O5 C54 C53 106.7(4) . . ? O5 C54 H54A 110.4 . . ? C53 C54 H54A 110.4 . . ? O5 C54 H54B 110.4 . . ? C53 C54 H54B 110.4 . . ? H54A C54 H54B 108.6 . . ? C61 O6 C64 106.0(3) . . ? C61 O6 V1 126.0(2) . . ? C64 O6 V1 127.84(19) . . ? C62 C61 O6 109.3(3) . . ? C62 C61 H61A 109.8 . . ? O6 C61 H61A 109.8 . . ? C62 C61 H61B 109.8 . . ? O6 C61 H61B 109.8 . . ? H61A C61 H61B 108.3 . . ? C61 C62 C63 106.9(4) . . ? C61 C62 H62A 110.3 . . ? C63 C62 H62A 110.3 . . ? C61 C62 H62B 110.3 . . ? C63 C62 H62B 110.3 . . ? H62A C62 H62B 108.6 . . ? C64 C63 C62 103.0(3) . . ? C64 C63 H63A 111.2 . . ? C62 C63 H63A 111.2 . . ? C64 C63 H63B 111.2 . . ? C62 C63 H63B 111.2 . . ? H63A C63 H63B 109.1 . . ? O6 C64 C63 104.7(3) . . ? O6 C64 H64A 110.8 . . ? C63 C64 H64A 110.8 . . ? O6 C64 H64B 110.8 . . ? C63 C64 H64B 110.8 . . ? H64A C64 H64B 108.9 . . ? H52X C52X H52Y 109.4 . . ? 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 N2 V1 O1 C11 30.8(2) . . . . ? O5 V1 O1 C11 -147.9(2) . . . . ? O6 V1 O1 C11 -112.8(18) . . . . ? Cl3 V1 O1 C11 122.8(2) . . . . ? Cl4 V1 O1 C11 -59.3(2) . . . . ? V1 O1 C11 C12 -26.3(4) . . . . ? V1 O1 C11 C16 155.9(2) . . . . ? O1 C11 C12 C13 -177.2(3) . . . . ? C16 C11 C12 C13 0.6(4) . . . . ? O1 C11 C12 C121 -0.5(4) . . . . ? C16 C11 C12 C121 177.3(3) . . . . ? C11 C12 C13 C14 -1.8(5) . . . . ? C121 C12 C13 C14 -178.7(3) . . . . ? C12 C13 C14 C15 1.6(5) . . . . ? C12 C13 C14 C141 178.6(3) . . . . ? C13 C14 C15 C16 -0.4(5) . . . . ? C141 C14 C15 C16 -177.3(3) . . . . ? C14 C15 C16 C11 -0.8(5) . . . . ? C14 C15 C16 C161 -179.8(3) . . . . ? O1 C11 C16 C15 178.4(3) . . . . ? C12 C11 C16 C15 0.6(4) . . . . ? O1 C11 C16 C161 -2.5(4) . . . . ? C12 C11 C16 C161 179.7(3) . . . . ? C13 C14 C141 C142 128.6(4) . . . . ? C15 C14 C141 C142 -54.6(5) . . . . ? C13 C14 C141 C143 -111.2(4) . . . . ? C15 C14 C141 C143 65.5(5) . . . . ? C13 C14 C141 C144 6.3(6) . . . . ? C15 C14 C141 C144 -177.0(4) . . . . ? C15 C16 C161 C163 -120.8(3) . . . . ? C11 C16 C161 C163 60.2(4) . . . . ? C15 C16 C161 C162 118.2(3) . . . . ? C11 C16 C161 C162 -60.8(4) . . . . ? C15 C16 C161 C164 -1.2(4) . . . . ? C11 C16 C161 C164 179.8(3) . . . . ? C13 C12 C121 N2 -171.4(3) . . . . ? C11 C12 C121 N2 11.7(5) . . . . ? C12 C121 N2 C21 179.0(3) . . . . ? C12 C121 N2 V1 2.0(4) . . . . ? O1 V1 N2 C121 -17.6(2) . . . . ? O5 V1 N2 C121 124(3) . . . . ? O6 V1 N2 C121 160.8(2) . . . . ? Cl3 V1 N2 C121 -110.2(2) . . . . ? Cl4 V1 N2 C121 73.0(2) . . . . ? O1 V1 N2 C21 165.6(2) . . . . ? O5 V1 N2 C21 -52(3) . . . . ? O6 V1 N2 C21 -16.0(2) . . . . ? Cl3 V1 N2 C21 73.1(2) . . . . ? Cl4 V1 N2 C21 -103.8(2) . . . . ? C121 N2 C21 C22 107.0(3) . . . . ? V1 N2 C21 C22 -76.1(3) . . . . ? C121 N2 C21 C26 -72.3(4) . . . . ? V1 N2 C21 C26 104.6(3) . . . . ? C26 C21 C22 C23 1.0(5) . . . . ? N2 C21 C22 C23 -178.3(3) . . . . ? C21 C22 C23 C24 0.0(5) . . . . ? C22 C23 C24 C25 -0.3(6) . . . . ? C23 C24 C25 C26 -0.1(6) . . . . ? C22 C21 C26 C25 -1.4(5) . . . . ? N2 C21 C26 C25 177.9(3) . . . . ? C22 C21 C26 C27 177.8(3) . . . . ? N2 C21 C26 C27 -2.9(4) . . . . ? C24 C25 C26 C21 1.0(5) . . . . ? C24 C25 C26 C27 -178.2(3) . . . . ? C21 C26 C27 C27 101.9(4) . . . 5_666 ? C25 C26 C27 C27 -78.9(4) . . . 5_666 ? O1 V1 O5 C51 -54.1(3) . . . . ? N2 V1 O5 C51 164(3) . . . . ? O6 V1 O5 C51 127.5(3) . . . . ? Cl3 V1 O5 C51 38.5(3) . . . . ? Cl4 V1 O5 C51 -144.6(3) . . . . ? O1 V1 O5 C54 127.5(3) . . . . ? N2 V1 O5 C54 -14(3) . . . . ? O6 V1 O5 C54 -50.9(3) . . . . ? Cl3 V1 O5 C54 -139.9(3) . . . . ? Cl4 V1 O5 C54 37.0(3) . . . . ? C54 O5 C51 C52 -14.1(5) . . . . ? V1 O5 C51 C52 167.2(4) . . . . ? O5 C51 C52 C53 32.4(7) . . . . ? C51 C52 C53 C54 -37.3(7) . . . . ? C51 O5 C54 C53 -8.7(5) . . . . ? V1 O5 C54 C53 169.9(2) . . . . ? C52 C53 C54 O5 28.9(6) . . . . ? O1 V1 O6 C61 -99.4(19) . . . . ? N2 V1 O6 C61 117.1(3) . . . . ? O5 V1 O6 C61 -64.1(3) . . . . ? Cl3 V1 O6 C61 25.1(3) . . . . ? Cl4 V1 O6 C61 -152.9(3) . . . . ? O1 V1 O6 C64 76.1(19) . . . . ? N2 V1 O6 C64 -67.4(3) . . . . ? O5 V1 O6 C64 111.4(3) . . . . ? Cl3 V1 O6 C64 -159.4(2) . . . . ? Cl4 V1 O6 C64 22.6(2) . . . . ? C64 O6 C61 C62 17.7(6) . . . . ? V1 O6 C61 C62 -166.0(4) . . . . ? O6 C61 C62 C63 2.2(7) . . . . ? C61 C62 C63 C64 -20.4(6) . . . . ? C61 O6 C64 C63 -30.3(4) . . . . ? V1 O6 C64 C63 153.4(2) . . . . ? C62 C63 C64 O6 30.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.393 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.053 data_s0481 _database_code_depnum_ccdc_archive 'CCDC 895725' #TrackingRef 'lucypap3.cif' _audit_creation_method SHELXL-97 # and Rigaku CrystalClear-SM Expert 2.0 r11' _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 13' _chemical_melting_point ? _chemical_formula_structural ? # '[V O Cl2 (OC6H4-2-CH=N-C6H3-2,6-iPr2)2].2MeCN' _chemical_formula_moiety 'C38 H46 Cl2 N2 O3 V, 2(C2 H3 N)' _chemical_formula_sum 'C42 H52 Cl2 N4 O3 V' _chemical_formula_weight 782.72 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' Cl Cl 0.1484 0.1585 '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 Orthorhombic _symmetry_space_group_name_H-M P21nb loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, -z' 'x+1/2, -y+1/2, z+1/2' 'x, y+1/2, -z+1/2' _cell_length_a 11.0873(5) _cell_length_b 17.9157(8) _cell_length_c 20.6832(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4108.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9248 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description needle _exptl_crystal_colour 'Dark Orange' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1652 _exptl_absorpt_coefficient_mu 0.414 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.480 _exptl_absorpt_process_details 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_source_power 2.5 _diffrn_source_voltage 45.0 _diffrn_source_current 55.0 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_specimen_support Mitegen _diffrn_detector CCD _diffrn_measurement_device 'AFC12 (Right): Kappa 3 circle' _diffrn_measurement_device_type 'Rigaku Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean 28.5714 _diffrn_measurement_method 'profile data from \w-scans' _diffrn_reflns_number 9744 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0833 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5871 _reflns_number_gt 4516 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Johnson, 1971 and Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 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^ > 2\s(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^)+(0.0206P)^2^+2.8166P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 5871 _refine_ls_number_parameters 471 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 V V 0.41544(8) 0.27652(4) 0.37639(3) 0.01677(18) Uani 1 1 d . . . O1 O 0.5141(3) 0.18621(17) 0.39419(14) 0.0189(8) Uani 1 1 d . . . C1 C 0.4948(4) 0.1139(2) 0.39658(19) 0.0156(11) Uani 1 1 d . . . C2 C 0.5846(5) 0.0690(2) 0.4275(2) 0.0193(11) Uani 1 1 d . . . C3 C 0.5666(5) -0.0083(3) 0.4327(2) 0.0294(12) Uani 1 1 d . . . H3 H 0.6250 -0.0374 0.4528 0.035 Uiso 1 1 calc R . . C4 C 0.4658(5) -0.0413(3) 0.4090(3) 0.0309(14) Uani 1 1 d . . . H4 H 0.4545 -0.0925 0.4131 0.037 Uiso 1 1 calc R . . C5 C 0.3795(5) 0.0027(3) 0.3783(2) 0.0273(13) Uani 1 1 d . . . H5 H 0.3116 -0.0200 0.3607 0.033 Uiso 1 1 calc R . . C6 C 0.3919(4) 0.0782(2) 0.3734(2) 0.0225(12) Uani 1 1 d . . . H6 H 0.3308 0.1062 0.3544 0.027 Uiso 1 1 calc R . . C7 C 0.6881(5) 0.1011(3) 0.4568(2) 0.0193(11) Uani 1 1 d . . . H7 H 0.7428 0.0683 0.4757 0.023 Uiso 1 1 calc R . . N8 N 0.7141(4) 0.1724(2) 0.45962(17) 0.0182(9) Uani 1 1 d . . . H8 H 0.6680 0.2034 0.4397 0.022 Uiso 1 1 calc R . . C11 C 0.8155(4) 0.2011(3) 0.4944(2) 0.0162(11) Uani 1 1 d . . . C12 C 0.9287(5) 0.2015(2) 0.4649(2) 0.0191(11) Uani 1 1 d . . . C13 C 1.0254(5) 0.2268(3) 0.5010(2) 0.0226(12) Uani 1 1 d . . . H13 H 1.1021 0.2278 0.4829 0.027 Uiso 1 1 calc R . . C14 C 1.0084(5) 0.2509(2) 0.5645(2) 0.0203(11) Uani 1 1 d . . . H14 H 1.0744 0.2660 0.5890 0.024 Uiso 1 1 calc R . . C15 C 0.8948(4) 0.2526(2) 0.5913(2) 0.0186(11) Uani 1 1 d . . . H15 H 0.8850 0.2703 0.6333 0.022 Uiso 1 1 calc R . . C16 C 0.7950(4) 0.2286(3) 0.5570(2) 0.0187(11) Uani 1 1 d . . . C121 C 0.9449(5) 0.1809(3) 0.3935(2) 0.0292(14) Uani 1 1 d . . . H121 H 0.8834 0.1436 0.3827 0.035 Uiso 1 1 calc R . . C122 C 0.9189(7) 0.2507(3) 0.3527(2) 0.0484(16) Uani 1 1 d . . . H12A H 0.9268 0.2388 0.3077 0.073 Uiso 1 1 calc R . . H12B H 0.9752 0.2893 0.3638 0.073 Uiso 1 1 calc R . . H12C H 0.8383 0.2677 0.3612 0.073 Uiso 1 1 calc R . . C123 C 1.0656(5) 0.1477(4) 0.3774(3) 0.0506(18) Uani 1 1 d . . . H12D H 1.0684 0.1357 0.3322 0.076 Uiso 1 1 calc R . . H12E H 1.0775 0.1032 0.4024 0.076 Uiso 1 1 calc R . . H12F H 1.1280 0.1830 0.3874 0.076 Uiso 1 1 calc R . . C161 C 0.6693(5) 0.2302(3) 0.5854(2) 0.0208(11) Uani 1 1 d . . . H161 H 0.6120 0.2327 0.5494 0.025 Uiso 1 1 calc R . . C162 C 0.6469(5) 0.2980(3) 0.6289(3) 0.0381(15) Uani 1 1 d . . . H16A H 0.5659 0.2963 0.6452 0.057 Uiso 1 1 calc R . . H16B H 0.6581 0.3429 0.6043 0.057 Uiso 1 1 calc R . . H16C H 0.7027 0.2972 0.6644 0.057 Uiso 1 1 calc R . . C163 C 0.6450(5) 0.1577(3) 0.6223(3) 0.0343(14) Uani 1 1 d . . . H16D H 0.5647 0.1587 0.6396 0.051 Uiso 1 1 calc R . . H16E H 0.7021 0.1528 0.6570 0.051 Uiso 1 1 calc R . . H16F H 0.6531 0.1160 0.5934 0.051 Uiso 1 1 calc R . . O2 O 0.3851(3) 0.37998(16) 0.34718(13) 0.0214(8) Uani 1 1 d . . . C21 C 0.2975(4) 0.4154(3) 0.3175(2) 0.0160(11) Uani 1 1 d . . . C22 C 0.3107(4) 0.4936(3) 0.3056(2) 0.0168(11) Uani 1 1 d . . . C23 C 0.2200(5) 0.5319(3) 0.2711(2) 0.0215(12) Uani 1 1 d . . . H23 H 0.2303 0.5822 0.2617 0.026 Uiso 1 1 calc R . . C24 C 0.1170(4) 0.4963(3) 0.2512(2) 0.0200(11) Uani 1 1 d . . . H24 H 0.0586 0.5219 0.2277 0.024 Uiso 1 1 calc R . . C25 C 0.1016(4) 0.4221(3) 0.2664(2) 0.0218(12) Uani 1 1 d . . . H25 H 0.0299 0.3988 0.2548 0.026 Uiso 1 1 calc R . . C26 C 0.1890(4) 0.3809(3) 0.2984(2) 0.0199(11) Uani 1 1 d . . . H26 H 0.1760 0.3307 0.3073 0.024 Uiso 1 1 calc R . . C27 C 0.4107(5) 0.5338(2) 0.33014(18) 0.0166(10) Uani 1 1 d . . . H27 H 0.4165 0.5840 0.3190 0.020 Uiso 1 1 calc R . . N28 N 0.4947(3) 0.5070(2) 0.36667(17) 0.0163(9) Uani 1 1 d . . . H28 H 0.4925 0.4600 0.3750 0.020 Uiso 1 1 calc R . . C31 C 0.5914(4) 0.5498(2) 0.3944(2) 0.0162(11) Uani 1 1 d . . . C32 C 0.5939(5) 0.5568(2) 0.4624(2) 0.0172(11) Uani 1 1 d . . . C33 C 0.6859(5) 0.5989(3) 0.4888(2) 0.0222(12) Uani 1 1 d . . . H33 H 0.6892 0.6051 0.5334 0.027 Uiso 1 1 calc R . . C34 C 0.7729(4) 0.6317(3) 0.4506(2) 0.0206(11) Uani 1 1 d . . . H34 H 0.8338 0.6599 0.4696 0.025 Uiso 1 1 calc R . . C35 C 0.7698(4) 0.6229(3) 0.3840(2) 0.0182(11) Uani 1 1 d . . . H35 H 0.8291 0.6452 0.3587 0.022 Uiso 1 1 calc R . . C36 C 0.6791(4) 0.5809(3) 0.3542(2) 0.0172(11) Uani 1 1 d . . . C321 C 0.4942(5) 0.5225(3) 0.5039(2) 0.0213(12) Uani 1 1 d . . . H321 H 0.4667 0.4770 0.4821 0.026 Uiso 1 1 calc R . . C322 C 0.3860(5) 0.5748(3) 0.5094(3) 0.0372(15) Uani 1 1 d . . . H32A H 0.3587 0.5882 0.4669 0.056 Uiso 1 1 calc R . . H32B H 0.4091 0.6190 0.5325 0.056 Uiso 1 1 calc R . . H32C H 0.3221 0.5501 0.5322 0.056 Uiso 1 1 calc R . . C323 C 0.5385(5) 0.5003(3) 0.5704(2) 0.0437(17) Uani 1 1 d . . . H32D H 0.4730 0.4791 0.5947 0.066 Uiso 1 1 calc R . . H32E H 0.5687 0.5435 0.5925 0.066 Uiso 1 1 calc R . . H32F H 0.6018 0.4641 0.5662 0.066 Uiso 1 1 calc R . . C361 C 0.6848(5) 0.5679(3) 0.2816(2) 0.0229(12) Uani 1 1 d . . . H361 H 0.6152 0.5376 0.2687 0.028 Uiso 1 1 calc R . . C362 C 0.6825(6) 0.6401(3) 0.2442(3) 0.0430(16) Uani 1 1 d . . . H36A H 0.6096 0.6668 0.2539 0.064 Uiso 1 1 calc R . . H36B H 0.6856 0.6296 0.1987 0.064 Uiso 1 1 calc R . . H36C H 0.7509 0.6700 0.2561 0.064 Uiso 1 1 calc R . . C363 C 0.7999(5) 0.5250(4) 0.2660(3) 0.0503(18) Uani 1 1 d . . . H36D H 0.8006 0.4788 0.2897 0.075 Uiso 1 1 calc R . . H36E H 0.8687 0.5544 0.2781 0.075 Uiso 1 1 calc R . . H36F H 0.8029 0.5146 0.2205 0.075 Uiso 1 1 calc R . . Cl3 Cl 0.57550(12) 0.33565(6) 0.43142(5) 0.0241(3) Uani 1 1 d . . . Cl4 Cl 0.37205(11) 0.23220(7) 0.27325(5) 0.0260(3) Uani 1 1 d . . . O5 O 0.3037(3) 0.26242(17) 0.42162(14) 0.0221(8) Uani 1 1 d . . . N71 N 0.8938(5) -0.0195(3) 0.4149(2) 0.0515(14) Uani 1 1 d . . . C72 C 0.8769(6) -0.0789(3) 0.4336(2) 0.0360(14) Uani 1 1 d . . . C73 C 0.8505(6) -0.1524(3) 0.4575(3) 0.0441(16) Uani 1 1 d . . . H73A H 0.7879 -0.1494 0.4895 0.066 Uiso 1 1 calc R . . H73B H 0.9217 -0.1735 0.4766 0.066 Uiso 1 1 calc R . . H73C H 0.8241 -0.1835 0.4225 0.066 Uiso 1 1 calc R . . N81 N 0.8271(5) 0.3169(3) 0.1969(3) 0.0573(16) Uani 1 1 d . . . C82 C 0.7345(7) 0.3373(3) 0.2125(3) 0.0413(16) Uani 1 1 d . . . C83 C 0.6177(6) 0.3625(4) 0.2351(3) 0.060(2) Uani 1 1 d . . . H83A H 0.6240 0.3780 0.2794 0.091 Uiso 1 1 calc R . . H83B H 0.5605 0.3225 0.2318 0.091 Uiso 1 1 calc R . . H83C H 0.5912 0.4038 0.2092 0.091 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 V 0.0207(5) 0.0120(4) 0.0176(3) -0.0001(3) -0.0016(4) -0.0029(4) O1 0.025(2) 0.0117(17) 0.0201(16) -0.0019(13) -0.0013(15) -0.0046(15) C1 0.022(3) 0.009(2) 0.016(2) -0.0025(19) 0.004(2) -0.007(2) C2 0.018(3) 0.015(2) 0.025(2) -0.001(2) 0.003(2) 0.001(3) C3 0.030(3) 0.011(2) 0.047(3) -0.002(2) -0.002(3) 0.004(3) C4 0.033(4) 0.014(3) 0.046(3) 0.003(2) -0.004(3) -0.006(3) C5 0.027(4) 0.024(3) 0.031(3) -0.001(2) -0.005(3) -0.008(2) C6 0.021(4) 0.017(2) 0.029(2) 0.003(2) -0.001(3) 0.001(2) C7 0.019(3) 0.014(3) 0.025(3) 0.004(2) 0.002(2) 0.007(2) N8 0.020(3) 0.012(2) 0.022(2) 0.0027(17) 0.0014(18) -0.0025(19) C11 0.012(3) 0.011(2) 0.026(3) 0.003(2) -0.006(2) 0.000(2) C12 0.017(3) 0.015(2) 0.025(2) -0.0014(19) -0.001(3) -0.006(2) C13 0.015(3) 0.017(3) 0.035(3) 0.001(2) 0.003(2) -0.004(2) C14 0.021(3) 0.013(2) 0.028(3) 0.001(2) -0.002(2) -0.005(2) C15 0.021(3) 0.015(2) 0.020(2) -0.0024(18) -0.005(2) -0.002(2) C16 0.021(3) 0.010(2) 0.026(3) 0.002(2) 0.000(2) -0.002(2) C121 0.033(4) 0.025(3) 0.030(3) -0.012(2) 0.005(2) -0.013(3) C122 0.066(4) 0.051(4) 0.028(2) 0.003(2) 0.012(3) -0.019(4) C123 0.033(4) 0.059(4) 0.059(4) -0.037(3) 0.013(4) -0.014(3) C161 0.020(3) 0.023(3) 0.019(2) -0.001(2) -0.002(2) 0.003(2) C162 0.033(4) 0.038(4) 0.043(3) -0.013(3) 0.005(3) 0.009(3) C163 0.029(4) 0.043(4) 0.032(3) 0.015(3) 0.004(3) 0.002(3) O2 0.022(2) 0.0147(16) 0.0274(16) 0.0007(14) -0.0078(16) -0.0050(16) C21 0.021(3) 0.014(2) 0.013(2) -0.005(2) -0.001(2) -0.002(2) C22 0.016(3) 0.018(3) 0.017(2) -0.002(2) 0.003(2) -0.005(2) C23 0.026(3) 0.018(3) 0.020(3) 0.005(2) 0.000(2) 0.005(2) C24 0.011(3) 0.028(3) 0.021(2) -0.001(2) -0.002(2) 0.003(2) C25 0.015(3) 0.026(3) 0.024(3) -0.005(2) -0.001(2) -0.004(2) C26 0.021(3) 0.017(3) 0.021(2) -0.001(2) 0.000(2) -0.004(2) C27 0.020(3) 0.014(2) 0.015(2) 0.0015(18) 0.000(2) 0.001(3) N28 0.019(2) 0.0068(19) 0.024(2) 0.0026(17) 0.0012(19) -0.0050(18) C31 0.010(3) 0.013(2) 0.025(3) -0.003(2) -0.002(2) -0.003(2) C32 0.019(3) 0.012(2) 0.020(2) 0.000(2) 0.003(2) 0.003(2) C33 0.028(3) 0.014(3) 0.024(3) -0.002(2) -0.005(2) -0.002(2) C34 0.014(3) 0.015(3) 0.033(3) -0.007(2) -0.003(2) -0.002(2) C35 0.012(3) 0.015(2) 0.028(3) 0.002(2) -0.005(2) -0.001(2) C36 0.014(3) 0.016(3) 0.021(2) -0.001(2) -0.001(2) 0.004(2) C321 0.028(3) 0.016(3) 0.020(2) 0.000(2) 0.001(2) -0.004(2) C322 0.041(4) 0.020(3) 0.051(3) -0.003(2) 0.022(3) -0.007(3) C323 0.044(4) 0.059(4) 0.028(3) 0.015(3) -0.008(3) -0.022(3) C361 0.020(3) 0.022(3) 0.027(3) 0.002(2) 0.001(2) 0.001(2) C362 0.051(4) 0.044(4) 0.033(3) 0.004(3) -0.009(3) -0.016(3) C363 0.039(4) 0.077(5) 0.036(3) -0.026(3) 0.002(3) 0.010(4) Cl3 0.0280(7) 0.0132(5) 0.0311(6) -0.0009(5) -0.0121(6) -0.0021(6) Cl4 0.0377(8) 0.0204(6) 0.0198(5) -0.0021(5) -0.0052(5) -0.0021(6) O5 0.026(2) 0.0190(19) 0.0219(16) 0.0023(14) -0.0009(15) -0.0014(16) N71 0.052(4) 0.033(3) 0.069(3) -0.004(3) 0.002(3) 0.005(3) C72 0.038(4) 0.032(3) 0.038(3) -0.005(3) 0.000(3) 0.007(3) C73 0.047(4) 0.046(4) 0.039(3) 0.012(3) 0.006(3) 0.003(3) N81 0.049(4) 0.064(4) 0.059(4) 0.003(3) 0.014(3) 0.003(3) C82 0.058(5) 0.030(3) 0.036(3) 0.006(3) 0.003(3) -0.013(3) C83 0.055(5) 0.051(4) 0.075(5) 0.001(4) 0.016(4) -0.018(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O5 1.573(3) . ? V O2 1.978(3) . ? V O1 1.987(3) . ? V Cl4 2.3265(12) . ? V Cl3 2.3594(14) . ? O1 C1 1.314(5) . ? C1 C6 1.394(6) . ? C1 C2 1.431(7) . ? C2 C3 1.403(6) . ? C2 C7 1.419(7) . ? C3 C4 1.356(7) . ? C3 H3 0.9300 . ? C4 C5 1.393(7) . ? C4 H4 0.9300 . ? C5 C6 1.362(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 N8 1.312(6) . ? C7 H7 0.9300 . ? N8 C11 1.430(6) . ? N8 H8 0.8600 . ? C11 C12 1.395(6) . ? C11 C16 1.404(6) . ? C12 C13 1.384(7) . ? C12 C121 1.533(6) . ? C13 C14 1.395(7) . ? C13 H13 0.9300 . ? C14 C15 1.376(7) . ? C14 H14 0.9300 . ? C15 C16 1.383(6) . ? C15 H15 0.9300 . ? C16 C161 1.513(7) . ? C121 C123 1.501(7) . ? C121 C122 1.536(7) . ? C121 H121 0.9800 . ? C122 H12A 0.9600 . ? C122 H12B 0.9600 . ? C122 H12C 0.9600 . ? C123 H12D 0.9600 . ? C123 H12E 0.9600 . ? C123 H12F 0.9600 . ? C161 C163 1.531(7) . ? C161 C162 1.531(7) . ? C161 H161 0.9800 . ? C162 H16A 0.9600 . ? C162 H16B 0.9600 . ? C162 H16C 0.9600 . ? C163 H16D 0.9600 . ? C163 H16E 0.9600 . ? C163 H16F 0.9600 . ? O2 C21 1.313(5) . ? C21 C26 1.409(6) . ? C21 C22 1.430(6) . ? C22 C23 1.410(6) . ? C22 C27 1.416(6) . ? C23 C24 1.371(6) . ? C23 H23 0.9300 . ? C24 C25 1.377(7) . ? C24 H24 0.9300 . ? C25 C26 1.386(6) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 N28 1.291(6) . ? C27 H27 0.9300 . ? N28 C31 1.439(6) . ? N28 H28 0.8600 . ? C31 C36 1.396(6) . ? C31 C32 1.412(6) . ? C32 C33 1.381(7) . ? C32 C321 1.529(6) . ? C33 C34 1.379(7) . ? C33 H33 0.9300 . ? C34 C35 1.388(6) . ? C34 H34 0.9300 . ? C35 C36 1.398(6) . ? C35 H35 0.9300 . ? C36 C361 1.522(6) . ? C321 C323 1.513(7) . ? C321 C322 1.526(7) . ? C321 H321 0.9800 . ? C322 H32A 0.9600 . ? C322 H32B 0.9600 . ? C322 H32C 0.9600 . ? C323 H32D 0.9600 . ? C323 H32E 0.9600 . ? C323 H32F 0.9600 . ? C361 C362 1.508(7) . ? C361 C363 1.524(7) . ? C361 H361 0.9800 . ? C362 H36A 0.9600 . ? C362 H36B 0.9600 . ? C362 H36C 0.9600 . ? C363 H36D 0.9600 . ? C363 H36E 0.9600 . ? C363 H36F 0.9600 . ? N71 C72 1.149(7) . ? C72 C73 1.437(7) . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? N81 C82 1.137(8) . ? C82 C83 1.449(9) . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 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 O5 V O2 101.43(15) . . ? O5 V O1 101.11(15) . . ? O2 V O1 155.91(14) . . ? O5 V Cl4 109.12(12) . . ? O2 V Cl4 90.26(9) . . ? O1 V Cl4 90.33(9) . . ? O5 V Cl3 112.20(12) . . ? O2 V Cl3 81.64(9) . . ? O1 V Cl3 82.08(10) . . ? Cl4 V Cl3 138.69(5) . . ? C1 O1 V 136.1(3) . . ? O1 C1 C6 125.0(4) . . ? O1 C1 C2 117.3(4) . . ? C6 C1 C2 117.7(4) . . ? C3 C2 C7 118.8(5) . . ? C3 C2 C1 119.3(5) . . ? C7 C2 C1 121.7(4) . . ? C4 C3 C2 121.3(5) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 119.0(5) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C6 C5 C4 121.7(5) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C1 120.9(4) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? N8 C7 C2 126.2(4) . . ? N8 C7 H7 116.9 . . ? C2 C7 H7 116.9 . . ? C7 N8 C11 123.0(4) . . ? C7 N8 H8 118.5 . . ? C11 N8 H8 118.5 . . ? C12 C11 C16 123.2(4) . . ? C12 C11 N8 119.3(4) . . ? C16 C11 N8 117.5(4) . . ? C13 C12 C11 117.5(4) . . ? C13 C12 C121 120.6(5) . . ? C11 C12 C121 121.7(4) . . ? C12 C13 C14 120.4(5) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 120.6(5) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 121.2(4) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C15 C16 C11 116.9(4) . . ? C15 C16 C161 122.1(4) . . ? C11 C16 C161 120.9(4) . . ? C123 C121 C12 114.4(5) . . ? C123 C121 C122 111.7(5) . . ? C12 C121 C122 108.1(4) . . ? C123 C121 H121 107.5 . . ? C12 C121 H121 107.5 . . ? C122 C121 H121 107.5 . . ? C121 C122 H12A 109.5 . . ? C121 C122 H12B 109.5 . . ? H12A C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12A C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C121 C123 H12D 109.5 . . ? C121 C123 H12E 109.5 . . ? H12D C123 H12E 109.5 . . ? C121 C123 H12F 109.5 . . ? H12D C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C16 C161 C163 109.8(4) . . ? C16 C161 C162 113.1(4) . . ? C163 C161 C162 110.6(4) . . ? C16 C161 H161 107.7 . . ? C163 C161 H161 107.7 . . ? C162 C161 H161 107.7 . . ? C161 C162 H16A 109.5 . . ? C161 C162 H16B 109.5 . . ? H16A C162 H16B 109.5 . . ? C161 C162 H16C 109.5 . . ? H16A C162 H16C 109.5 . . ? H16B C162 H16C 109.5 . . ? C161 C163 H16D 109.5 . . ? C161 C163 H16E 109.5 . . ? H16D C163 H16E 109.5 . . ? C161 C163 H16F 109.5 . . ? H16D C163 H16F 109.5 . . ? H16E C163 H16F 109.5 . . ? C21 O2 V 136.2(3) . . ? O2 C21 C26 123.4(4) . . ? O2 C21 C22 118.6(4) . . ? C26 C21 C22 118.0(4) . . ? C23 C22 C27 119.5(4) . . ? C23 C22 C21 119.3(4) . . ? C27 C22 C21 121.1(4) . . ? C24 C23 C22 121.4(5) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C25 118.9(5) . . ? C23 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? C24 C25 C26 122.5(5) . . ? C24 C25 H25 118.8 . . ? C26 C25 H25 118.8 . . ? C25 C26 C21 119.8(5) . . ? C25 C26 H26 120.1 . . ? C21 C26 H26 120.1 . . ? N28 C27 C22 125.8(4) . . ? N28 C27 H27 117.1 . . ? C22 C27 H27 117.1 . . ? C27 N28 C31 124.9(4) . . ? C27 N28 H28 117.6 . . ? C31 N28 H28 117.6 . . ? C36 C31 C32 123.0(4) . . ? C36 C31 N28 119.7(4) . . ? C32 C31 N28 117.3(4) . . ? C33 C32 C31 117.2(4) . . ? C33 C32 C321 122.0(4) . . ? C31 C32 C321 120.7(4) . . ? C34 C33 C32 121.5(4) . . ? C34 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? C33 C34 C35 120.2(5) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C34 C35 C36 121.1(5) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C31 C36 C35 117.0(4) . . ? C31 C36 C361 123.7(4) . . ? C35 C36 C361 119.2(4) . . ? C323 C321 C322 110.4(4) . . ? C323 C321 C32 112.5(4) . . ? C322 C321 C32 111.3(4) . . ? C323 C321 H321 107.5 . . ? C322 C321 H321 107.5 . . ? C32 C321 H321 107.5 . . ? C321 C322 H32A 109.5 . . ? C321 C322 H32B 109.5 . . ? H32A C322 H32B 109.5 . . ? C321 C322 H32C 109.5 . . ? H32A C322 H32C 109.5 . . ? H32B C322 H32C 109.5 . . ? C321 C323 H32D 109.5 . . ? C321 C323 H32E 109.5 . . ? H32D C323 H32E 109.5 . . ? C321 C323 H32F 109.5 . . ? H32D C323 H32F 109.5 . . ? H32E C323 H32F 109.5 . . ? C362 C361 C36 111.9(4) . . ? C362 C361 C363 109.8(5) . . ? C36 C361 C363 108.7(4) . . ? C362 C361 H361 108.8 . . ? C36 C361 H361 108.8 . . ? C363 C361 H361 108.8 . . ? C361 C362 H36A 109.5 . . ? C361 C362 H36B 109.5 . . ? H36A C362 H36B 109.5 . . ? C361 C362 H36C 109.5 . . ? H36A C362 H36C 109.5 . . ? H36B C362 H36C 109.5 . . ? C361 C363 H36D 109.5 . . ? C361 C363 H36E 109.5 . . ? H36D C363 H36E 109.5 . . ? C361 C363 H36F 109.5 . . ? H36D C363 H36F 109.5 . . ? H36E C363 H36F 109.5 . . ? N71 C72 C73 177.5(7) . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? N81 C82 C83 177.6(7) . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 V O1 C1 48.9(4) . . . . ? O2 V O1 C1 -152.1(4) . . . . ? Cl4 V O1 C1 -60.7(4) . . . . ? Cl3 V O1 C1 160.1(4) . . . . ? V O1 C1 C6 13.3(7) . . . . ? V O1 C1 C2 -164.2(3) . . . . ? O1 C1 C2 C3 178.4(4) . . . . ? C6 C1 C2 C3 0.7(6) . . . . ? O1 C1 C2 C7 2.4(6) . . . . ? C6 C1 C2 C7 -175.3(4) . . . . ? C7 C2 C3 C4 176.1(5) . . . . ? C1 C2 C3 C4 0.0(7) . . . . ? C2 C3 C4 C5 0.7(8) . . . . ? C3 C4 C5 C6 -2.2(8) . . . . ? C4 C5 C6 C1 2.9(7) . . . . ? O1 C1 C6 C5 -179.7(4) . . . . ? C2 C1 C6 C5 -2.1(6) . . . . ? C3 C2 C7 N8 -175.7(5) . . . . ? C1 C2 C7 N8 0.4(7) . . . . ? C2 C7 N8 C11 174.9(4) . . . . ? C7 N8 C11 C12 83.4(6) . . . . ? C7 N8 C11 C16 -97.4(5) . . . . ? C16 C11 C12 C13 3.4(7) . . . . ? N8 C11 C12 C13 -177.5(4) . . . . ? C16 C11 C12 C121 -171.6(4) . . . . ? N8 C11 C12 C121 7.5(7) . . . . ? C11 C12 C13 C14 -0.1(7) . . . . ? C121 C12 C13 C14 175.0(4) . . . . ? C12 C13 C14 C15 -2.5(7) . . . . ? C13 C14 C15 C16 1.9(7) . . . . ? C14 C15 C16 C11 1.3(6) . . . . ? C14 C15 C16 C161 -179.8(4) . . . . ? C12 C11 C16 C15 -4.0(7) . . . . ? N8 C11 C16 C15 176.8(4) . . . . ? C12 C11 C16 C161 177.0(4) . . . . ? N8 C11 C16 C161 -2.1(6) . . . . ? C13 C12 C121 C123 33.9(6) . . . . ? C11 C12 C121 C123 -151.2(5) . . . . ? C13 C12 C121 C122 -91.2(6) . . . . ? C11 C12 C121 C122 83.7(6) . . . . ? C15 C16 C161 C163 -87.7(5) . . . . ? C11 C16 C161 C163 91.2(5) . . . . ? C15 C16 C161 C162 36.3(6) . . . . ? C11 C16 C161 C162 -144.8(5) . . . . ? O5 V O2 C21 -56.9(4) . . . . ? O1 V O2 C21 144.0(4) . . . . ? Cl4 V O2 C21 52.7(4) . . . . ? Cl3 V O2 C21 -168.0(4) . . . . ? V O2 C21 C26 1.2(7) . . . . ? V O2 C21 C22 179.2(3) . . . . ? O2 C21 C22 C23 177.1(4) . . . . ? C26 C21 C22 C23 -4.9(6) . . . . ? O2 C21 C22 C27 -5.6(6) . . . . ? C26 C21 C22 C27 172.5(4) . . . . ? C27 C22 C23 C24 -174.6(4) . . . . ? C21 C22 C23 C24 2.8(7) . . . . ? C22 C23 C24 C25 1.3(7) . . . . ? C23 C24 C25 C26 -3.3(7) . . . . ? C24 C25 C26 C21 1.1(7) . . . . ? O2 C21 C26 C25 -179.0(4) . . . . ? C22 C21 C26 C25 3.0(6) . . . . ? C23 C22 C27 N28 174.2(4) . . . . ? C21 C22 C27 N28 -3.2(7) . . . . ? C22 C27 N28 C31 -175.9(4) . . . . ? C27 N28 C31 C36 -67.0(6) . . . . ? C27 N28 C31 C32 114.4(5) . . . . ? C36 C31 C32 C33 2.4(7) . . . . ? N28 C31 C32 C33 -179.1(4) . . . . ? C36 C31 C32 C321 179.0(4) . . . . ? N28 C31 C32 C321 -2.5(7) . . . . ? C31 C32 C33 C34 -1.0(7) . . . . ? C321 C32 C33 C34 -177.6(4) . . . . ? C32 C33 C34 C35 -0.2(7) . . . . ? C33 C34 C35 C36 0.2(7) . . . . ? C32 C31 C36 C35 -2.4(7) . . . . ? N28 C31 C36 C35 179.1(4) . . . . ? C32 C31 C36 C361 173.9(4) . . . . ? N28 C31 C36 C361 -4.6(7) . . . . ? C34 C35 C36 C31 1.1(7) . . . . ? C34 C35 C36 C361 -175.4(4) . . . . ? C33 C32 C321 C323 -32.8(7) . . . . ? C31 C32 C321 C323 150.7(5) . . . . ? C33 C32 C321 C322 91.7(5) . . . . ? C31 C32 C321 C322 -84.8(5) . . . . ? C31 C36 C361 C362 123.8(5) . . . . ? C35 C36 C361 C362 -59.9(6) . . . . ? C31 C36 C361 C363 -114.8(6) . . . . ? C35 C36 C361 C363 61.5(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N8 H8 O1 0.86 1.97 2.610(5) 130.0 . N8 H8 Cl3 0.86 2.59 3.355(4) 149.1 . N28 H28 O2 0.86 1.95 2.610(5) 132.6 . N28 H28 Cl3 0.86 2.68 3.467(4) 153.2 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.307 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.066 #===END