# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Christine Joy McKenzie' _publ_contact_author_email CHK@IFK.SDU.DK _publ_section_title ; Selective recognition and binding of arsenate over phosphate ; loop_ _publ_author_name 'Christine Joy McKenzie' 'Andrew D Bond' 'Rune Kirk Egdal' 'Maria P. B. Espino' 'Kevin Francesconi' ; M.Hussain ; 'Georg Raber' # Attachment 'submit.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 722650' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C36 H40 N6 O7 P V2 +, C36 H41 N6 O7 P V2 2+, 3(Cl O4 -) ; _chemical_formula_sum 'C72 H81 Cl3 N12 O26 P2 V4' _chemical_formula_weight 1902.54 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' P P 0.1023 0.0942 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3735(4) _cell_length_b 21.3057(10) _cell_length_c 21.9212(10) _cell_angle_alpha 71.600(2) _cell_angle_beta 77.945(1) _cell_angle_gamma 87.094(2) _cell_volume 4495.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 4171 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 20.70 _exptl_crystal_description plate _exptl_crystal_colour violet _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1956 _exptl_absorpt_coefficient_mu 0.606 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.806 _exptl_absorpt_correction_T_max 0.964 _exptl_absorpt_process_details ; SADABS v.2.10 (Sheldrick, 2003) Ratio of minimum to maximum apparent transmission: 0.836511 ; _exptl_special_details ; This CIF refers to refinement against SQUEEZED data (v.d.Sluis & Spek, 1990), with all lattice solvent omitted. See the bottom of this CIF for details of the SQUEEZE process. The Cl---O and O...O distances of the perchlorate anions are restrained to a single refined value and 1.633 times that value, respectively. The displacement parameters of the O atoms in the disordered perchlorate are restrained to approximate isotropic behaviour. H atoms of the phosphate groups are placed so as to form the best available hydrogen bonds. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 57173 _diffrn_reflns_av_R_equivalents 0.0909 _diffrn_reflns_av_sigmaI/netI 0.1481 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 25.03 _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.973 _reflns_number_total 15467 _reflns_number_gt 7840 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _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^)+(0.1041P)^2^] 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 15467 _refine_ls_number_parameters 1109 _refine_ls_number_restraints 88 _refine_ls_R_factor_all 0.1368 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.1958 _refine_ls_wR_factor_gt 0.1764 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.970 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.687 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.094 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 0.23944(9) 0.45861(5) 0.19860(5) 0.0243(3) Uani 1 1 d . . . V2 V -0.08655(9) 0.39957(5) 0.26444(4) 0.0237(3) Uani 1 1 d . . . P1 P 0.03827(15) 0.44286(8) 0.10900(7) 0.0291(4) Uani 1 1 d . . . O1 O 0.2746(4) 0.38210(18) 0.22124(18) 0.0300(10) Uani 1 1 d . . . O2 O -0.0032(3) 0.33594(18) 0.29305(17) 0.0279(9) Uani 1 1 d . . . O3 O 0.0562(3) 0.46706(18) 0.25353(17) 0.0248(9) Uani 1 1 d . . . O4 O 0.1537(4) 0.4725(2) 0.12345(17) 0.0333(10) Uani 1 1 d . . . O5 O -0.0661(4) 0.41282(19) 0.17138(17) 0.0306(10) Uani 1 1 d . . . O6 O 0.0949(4) 0.3858(2) 0.08063(19) 0.0396(11) Uani 1 1 d . . . H6 H 0.0386 0.3692 0.0641 0.059 Uiso 1 1 d R . . O7 O -0.0248(4) 0.4948(2) 0.05918(18) 0.0404(11) Uani 1 1 d . . . H7 H -0.0082 0.4982 0.0190 0.061 Uiso 0.50 1 d PR . . N1 N 0.2580(4) 0.5705(2) 0.1725(2) 0.0269(11) Uani 1 1 d . . . N2 N 0.4185(4) 0.4870(2) 0.1286(2) 0.0276(12) Uani 1 1 d . . . N3 N 0.3146(4) 0.4739(2) 0.2760(2) 0.0252(11) Uani 1 1 d . . . N4 N -0.1730(4) 0.4040(2) 0.3608(2) 0.0245(11) Uani 1 1 d . . . N5 N -0.2618(4) 0.3433(2) 0.2881(2) 0.0263(11) Uani 1 1 d . . . N6 N -0.2155(4) 0.4913(2) 0.2469(2) 0.0295(12) Uani 1 1 d . . . C1 C 0.0331(5) 0.5114(3) 0.2892(3) 0.0240(13) Uani 1 1 d . . . C2 C 0.0613(5) 0.5780(3) 0.2552(3) 0.0266(14) Uani 1 1 d . . . C3 C 0.0385(6) 0.6233(3) 0.2894(3) 0.0343(15) Uani 1 1 d . . . H3A H 0.0599 0.6686 0.2664 0.041 Uiso 1 1 calc R . . C4 C -0.0157(5) 0.6043(3) 0.3574(3) 0.0275(14) Uani 1 1 d . . . C5 C -0.0442(5) 0.5390(3) 0.3883(3) 0.0302(15) Uani 1 1 d . . . H5A H -0.0809 0.5248 0.4340 0.036 Uiso 1 1 calc R . . C6 C -0.0211(5) 0.4912(3) 0.3549(3) 0.0241(14) Uani 1 1 d . . . C7 C -0.0384(6) 0.6583(3) 0.3914(3) 0.0398(17) Uani 1 1 d . . . C8 C -0.1121(7) 0.6283(4) 0.4646(3) 0.0500(19) Uani 1 1 d . . . H8A H -0.1242 0.6629 0.4859 0.075 Uiso 1 1 calc R . . H8B H -0.0598 0.5926 0.4878 0.075 Uiso 1 1 calc R . . H8C H -0.1984 0.6107 0.4658 0.075 Uiso 1 1 calc R . . C9 C 0.0953(7) 0.6871(4) 0.3903(4) 0.070(2) Uani 1 1 d . . . H9A H 0.0810 0.7213 0.4121 0.105 Uiso 1 1 calc R . . H9B H 0.1418 0.7065 0.3447 0.105 Uiso 1 1 calc R . . H9C H 0.1484 0.6517 0.4134 0.105 Uiso 1 1 calc R . . C10 C -0.1243(10) 0.7121(4) 0.3568(4) 0.088(3) Uani 1 1 d . . . H10A H -0.1374 0.7467 0.3781 0.132 Uiso 1 1 calc R . . H10B H -0.2099 0.6929 0.3593 0.132 Uiso 1 1 calc R . . H10C H -0.0809 0.7313 0.3106 0.132 Uiso 1 1 calc R . . C11 C 0.1232(5) 0.5997(3) 0.1832(3) 0.0316(15) Uani 1 1 d . . . H11A H 0.0669 0.5851 0.1587 0.038 Uiso 1 1 calc R . . H11B H 0.1304 0.6486 0.1663 0.038 Uiso 1 1 calc R . . C12 C 0.3198(6) 0.5933(3) 0.1016(3) 0.0377(16) Uani 1 1 d . . . H12A H 0.3514 0.6397 0.0884 0.045 Uiso 1 1 calc R . . H12B H 0.2548 0.5911 0.0751 0.045 Uiso 1 1 calc R . . C13 C 0.4329(6) 0.5492(3) 0.0907(3) 0.0324(15) Uani 1 1 d . . . C14 C 0.5477(7) 0.5717(4) 0.0423(3) 0.052(2) Uani 1 1 d . . . H14A H 0.5565 0.6164 0.0148 0.062 Uiso 1 1 calc R . . C15 C 0.6475(7) 0.5271(4) 0.0357(4) 0.057(2) Uani 1 1 d . . . H15A H 0.7269 0.5413 0.0042 0.068 Uiso 1 1 calc R . . C16 C 0.6317(6) 0.4629(4) 0.0746(3) 0.0450(18) Uani 1 1 d . . . H16A H 0.6986 0.4317 0.0699 0.054 Uiso 1 1 calc R . . C17 C 0.5187(6) 0.4443(3) 0.1202(3) 0.0367(16) Uani 1 1 d . . . H17A H 0.5087 0.3996 0.1476 0.044 Uiso 1 1 calc R . . C18 C 0.3407(6) 0.5882(3) 0.2113(3) 0.0293(14) Uani 1 1 d . . . H18A H 0.3103 0.6303 0.2192 0.035 Uiso 1 1 calc R . . H18B H 0.4330 0.5949 0.1865 0.035 Uiso 1 1 calc R . . C19 C 0.3353(5) 0.5350(3) 0.2761(3) 0.0320(15) Uani 1 1 d . . . C20 C 0.3565(6) 0.5475(3) 0.3313(3) 0.0366(16) Uani 1 1 d . . . H20A H 0.3684 0.5915 0.3309 0.044 Uiso 1 1 calc R . . C21 C 0.3604(6) 0.4949(4) 0.3871(3) 0.0434(18) Uani 1 1 d . . . H21A H 0.3752 0.5026 0.4255 0.052 Uiso 1 1 calc R . . C22 C 0.3429(6) 0.4316(3) 0.3873(3) 0.0384(16) Uani 1 1 d . . . H22A H 0.3465 0.3948 0.4251 0.046 Uiso 1 1 calc R . . C23 C 0.3199(6) 0.4232(3) 0.3309(3) 0.0338(15) Uani 1 1 d . . . H23A H 0.3071 0.3795 0.3305 0.041 Uiso 1 1 calc R . . C24 C -0.0683(5) 0.4202(3) 0.3910(3) 0.0296(14) Uani 1 1 d . . . H24A H 0.0063 0.3898 0.3879 0.036 Uiso 1 1 calc R . . H24B H -0.1037 0.4148 0.4379 0.036 Uiso 1 1 calc R . . C25 C -0.2286(6) 0.3343(3) 0.3967(3) 0.0269(14) Uani 1 1 d . . . H25A H -0.1562 0.3025 0.4040 0.032 Uiso 1 1 calc R . . H25B H -0.2845 0.3323 0.4398 0.032 Uiso 1 1 calc R . . C26 C -0.3096(5) 0.3176(3) 0.3537(3) 0.0262(14) Uani 1 1 d . . . C27 C -0.4234(6) 0.2803(3) 0.3786(3) 0.0340(15) Uani 1 1 d . . . H27A H -0.4549 0.2634 0.4247 0.041 Uiso 1 1 calc R . . C28 C -0.4921(6) 0.2673(3) 0.3360(3) 0.0390(16) Uani 1 1 d . . . H28A H -0.5715 0.2416 0.3522 0.047 Uiso 1 1 calc R . . C29 C -0.4417(6) 0.2928(3) 0.2685(3) 0.0393(17) Uani 1 1 d . . . H29A H -0.4865 0.2848 0.2380 0.047 Uiso 1 1 calc R . . C30 C -0.3259(6) 0.3301(3) 0.2465(3) 0.0343(15) Uani 1 1 d . . . H30A H -0.2910 0.3466 0.2007 0.041 Uiso 1 1 calc R . . C31 C -0.2825(6) 0.4516(3) 0.3632(3) 0.0313(15) Uani 1 1 d . . . H31A H -0.2832 0.4693 0.4000 0.038 Uiso 1 1 calc R . . H31B H -0.3675 0.4281 0.3718 0.038 Uiso 1 1 calc R . . C32 C -0.2693(5) 0.5076(3) 0.3008(3) 0.0278(14) Uani 1 1 d . . . C33 C -0.3144(6) 0.5704(3) 0.2982(3) 0.0399(17) Uani 1 1 d . . . H33A H -0.3484 0.5808 0.3375 0.048 Uiso 1 1 calc R . . C34 C -0.3093(6) 0.6172(3) 0.2383(4) 0.0442(18) Uani 1 1 d . . . H34A H -0.3399 0.6607 0.2354 0.053 Uiso 1 1 calc R . . C35 C -0.2593(7) 0.6005(3) 0.1820(3) 0.0467(18) Uani 1 1 d . . . H35A H -0.2584 0.6316 0.1399 0.056 Uiso 1 1 calc R . . C36 C -0.2107(6) 0.5380(3) 0.1884(3) 0.0370(16) Uani 1 1 d . . . H36A H -0.1720 0.5273 0.1497 0.044 Uiso 1 1 calc R . . V3 V 0.62409(10) 0.06575(5) 0.14973(5) 0.0296(3) Uani 1 1 d . . . V4 V 0.90530(10) 0.13040(5) 0.17574(5) 0.0296(3) Uani 1 1 d . . . P2 P 0.90601(17) 0.07899(10) 0.05256(9) 0.0416(5) Uani 1 1 d . . . O8 O 0.5923(4) 0.1423(2) 0.11938(19) 0.0394(11) Uani 1 1 d . . . O9 O 0.8165(4) 0.19522(19) 0.1600(2) 0.0377(11) Uani 1 1 d . . . O10 O 0.7540(4) 0.06351(18) 0.20903(18) 0.0281(9) Uani 1 1 d . . . O11 O 0.7720(4) 0.0470(2) 0.08663(18) 0.0361(10) Uani 1 1 d . . . O12 O 0.9636(4) 0.1118(2) 0.09378(19) 0.0401(11) Uani 1 1 d . . . O13 O 0.8908(6) 0.1303(3) -0.0125(2) 0.0849(19) Uani 1 1 d . . . H13 H 0.8375 0.1604 -0.0247 0.127 Uiso 1 1 d R . . O14 O 1.0073(5) 0.0311(3) 0.0354(3) 0.094(2) Uani 1 1 d . . . H14 H 1.0025 0.0103 0.0091 0.141 Uiso 0.50 1 d PR . . N7 N 0.6008(5) -0.0455(2) 0.1996(2) 0.0297(12) Uani 1 1 d . . . N8 N 0.4930(5) 0.0312(2) 0.1041(2) 0.0289(12) Uani 1 1 d . . . N9 N 0.4733(5) 0.0555(2) 0.2360(2) 0.0313(12) Uani 1 1 d . . . N10 N 0.9046(5) 0.1325(2) 0.2726(2) 0.0308(12) Uani 1 1 d . . . N11 N 1.0771(5) 0.1859(2) 0.1612(2) 0.0294(12) Uani 1 1 d . . . N12 N 1.0218(4) 0.0385(2) 0.2215(3) 0.0337(13) Uani 1 1 d . . . C37 C 0.7329(5) 0.0227(3) 0.2728(3) 0.0306(15) Uani 1 1 d . . . C38 C 0.7171(5) -0.0458(3) 0.2857(3) 0.0246(14) Uani 1 1 d . . . C39 C 0.7010(6) -0.0863(3) 0.3495(3) 0.0342(15) Uani 1 1 d . . . H39A H 0.6907 -0.1325 0.3578 0.041 Uiso 1 1 calc R . . C40 C 0.6988(5) -0.0639(3) 0.4026(3) 0.0291(14) Uani 1 1 d . . . C41 C 0.7138(6) 0.0046(3) 0.3884(3) 0.0284(14) Uani 1 1 d . . . H41A H 0.7110 0.0220 0.4236 0.034 Uiso 1 1 calc R . . C42 C 0.7326(6) 0.0481(3) 0.3247(3) 0.0293(15) Uani 1 1 d . . . C43 C 0.6855(6) -0.1093(3) 0.4732(3) 0.0337(15) Uani 1 1 d . . . C44 C 0.8093(6) -0.0988(3) 0.4982(3) 0.0444(18) Uani 1 1 d . . . H44A H 0.8162 -0.0523 0.4955 0.067 Uiso 1 1 calc R . . H44B H 0.8881 -0.1109 0.4711 0.067 Uiso 1 1 calc R . . H44C H 0.8018 -0.1267 0.5440 0.067 Uiso 1 1 calc R . . C45 C 0.5604(6) -0.0915(3) 0.5169(3) 0.0471(18) Uani 1 1 d . . . H45A H 0.5661 -0.0450 0.5146 0.071 Uiso 1 1 calc R . . H45B H 0.5540 -0.1197 0.5625 0.071 Uiso 1 1 calc R . . H45C H 0.4820 -0.0984 0.5013 0.071 Uiso 1 1 calc R . . C46 C 0.6761(7) -0.1818(3) 0.4789(3) 0.053(2) Uani 1 1 d . . . H46A H 0.7550 -0.1939 0.4519 0.080 Uiso 1 1 calc R . . H46B H 0.5977 -0.1895 0.4637 0.080 Uiso 1 1 calc R . . H46C H 0.6696 -0.2088 0.5249 0.080 Uiso 1 1 calc R . . C47 C 0.7161(6) -0.0722(3) 0.2301(3) 0.0330(15) Uani 1 1 d . . . H47A H 0.7988 -0.0589 0.1968 0.040 Uiso 1 1 calc R . . H47B H 0.7106 -0.1211 0.2465 0.040 Uiso 1 1 calc R . . C48 C 0.5919(6) -0.0729(3) 0.1470(3) 0.0378(16) Uani 1 1 d . . . H48A H 0.5633 -0.1200 0.1658 0.045 Uiso 1 1 calc R . . H48B H 0.6790 -0.0702 0.1173 0.045 Uiso 1 1 calc R . . C49 C 0.4930(6) -0.0331(3) 0.1096(3) 0.0309(15) Uani 1 1 d . . . C50 C 0.4076(6) -0.0593(3) 0.0836(3) 0.0388(17) Uani 1 1 d . . . H50A H 0.4094 -0.1051 0.0876 0.047 Uiso 1 1 calc R . . C51 C 0.3181(6) -0.0175(4) 0.0512(3) 0.0399(17) Uani 1 1 d . . . H51A H 0.2568 -0.0349 0.0338 0.048 Uiso 1 1 calc R . . C52 C 0.3189(6) 0.0486(4) 0.0446(3) 0.0376(16) Uani 1 1 d . . . H52A H 0.2596 0.0780 0.0223 0.045 Uiso 1 1 calc R . . C53 C 0.4078(6) 0.0704(3) 0.0712(3) 0.0395(17) Uani 1 1 d . . . H53A H 0.4099 0.1163 0.0662 0.047 Uiso 1 1 calc R . . C54 C 0.4745(6) -0.0615(3) 0.2511(3) 0.0336(15) Uani 1 1 d . . . H54A H 0.4027 -0.0706 0.2315 0.040 Uiso 1 1 calc R . . H54B H 0.4866 -0.1017 0.2873 0.040 Uiso 1 1 calc R . . C55 C 0.4373(6) -0.0053(3) 0.2777(3) 0.0317(15) Uani 1 1 d . . . C56 C 0.3607(6) -0.0143(3) 0.3396(3) 0.0404(17) Uani 1 1 d . . . H56A H 0.3382 -0.0575 0.3690 0.048 Uiso 1 1 calc R . . C57 C 0.3178(6) 0.0405(4) 0.3579(3) 0.0467(18) Uani 1 1 d . . . H57A H 0.2634 0.0352 0.3999 0.056 Uiso 1 1 calc R . . C58 C 0.3530(6) 0.1027(4) 0.3159(3) 0.0430(17) Uani 1 1 d . . . H58A H 0.3245 0.1408 0.3284 0.052 Uiso 1 1 calc R . . C59 C 0.4310(6) 0.1086(3) 0.2548(3) 0.0338(15) Uani 1 1 d . . . H59A H 0.4554 0.1516 0.2251 0.041 Uiso 1 1 calc R . . C60 C 0.7646(6) 0.1199(3) 0.3114(3) 0.0298(15) Uani 1 1 d . . . H60A H 0.7563 0.1298 0.3532 0.036 Uiso 1 1 calc R . . H60B H 0.7032 0.1484 0.2860 0.036 Uiso 1 1 calc R . . C61 C 0.9517(6) 0.2026(3) 0.2612(3) 0.0304(15) Uani 1 1 d . . . H61A H 0.8825 0.2347 0.2479 0.036 Uiso 1 1 calc R . . H61B H 0.9720 0.2067 0.3020 0.036 Uiso 1 1 calc R . . C62 C 1.0740(6) 0.2163(3) 0.2075(3) 0.0322(15) Uani 1 1 d . . . C63 C 1.1781(6) 0.2554(3) 0.2035(3) 0.0399(17) Uani 1 1 d . . . H63A H 1.1770 0.2753 0.2368 0.048 Uiso 1 1 calc R . . C64 C 1.2842(6) 0.2661(3) 0.1518(3) 0.0423(17) Uani 1 1 d . . . H64A H 1.3557 0.2937 0.1491 0.051 Uiso 1 1 calc R . . C65 C 1.2861(6) 0.2368(3) 0.1044(3) 0.0437(18) Uani 1 1 d . . . H65A H 1.3579 0.2437 0.0680 0.052 Uiso 1 1 calc R . . C66 C 1.1820(6) 0.1975(3) 0.1113(3) 0.0394(17) Uani 1 1 d . . . H66A H 1.1832 0.1769 0.0786 0.047 Uiso 1 1 calc R . . C67 C 0.9958(6) 0.0861(3) 0.3089(3) 0.0355(16) Uani 1 1 d . . . H67A H 0.9560 0.0714 0.3563 0.043 Uiso 1 1 calc R . . H67B H 1.0796 0.1098 0.3028 0.043 Uiso 1 1 calc R . . C68 C 1.0247(6) 0.0264(3) 0.2858(3) 0.0298(15) Uani 1 1 d . . . C69 C 1.0567(6) -0.0329(3) 0.3242(3) 0.0401(17) Uani 1 1 d . . . H69A H 1.0561 -0.0394 0.3692 0.048 Uiso 1 1 calc R . . C70 C 1.0905(6) -0.0843(3) 0.2982(4) 0.0452(18) Uani 1 1 d . . . H70A H 1.1107 -0.1268 0.3249 0.054 Uiso 1 1 calc R . . C71 C 1.0937(6) -0.0714(3) 0.2324(4) 0.0495(19) Uani 1 1 d . . . H71A H 1.1215 -0.1046 0.2122 0.059 Uiso 1 1 calc R . . C72 C 1.0571(6) -0.0112(4) 0.1961(3) 0.0417(17) Uani 1 1 d . . . H72A H 1.0565 -0.0040 0.1512 0.050 Uiso 1 1 calc R . . Cl1 Cl 0.5871(3) 0.75830(12) 0.08141(13) 0.0907(8) Uani 0.60 1 d PD A 1 O1A O 0.5663(12) 0.7550(5) 0.1522(4) 0.111(4) Uani 0.60 1 d PDU A 1 O1B O 0.5798(9) 0.6957(3) 0.0787(5) 0.071(3) Uani 0.60 1 d PDU A 1 O1C O 0.7070(12) 0.7930(7) 0.0507(7) 0.203(7) Uani 0.60 1 d PDU A 1 O1D O 0.4807(13) 0.7984(6) 0.0590(6) 0.186(7) Uani 0.60 1 d PDU A 1 Cl1A Cl 0.5871(3) 0.75830(12) 0.08141(13) 0.0907(8) Uani 0.40 1 d PD B 2 O1E O 0.5988(18) 0.8234(4) 0.0746(8) 0.122(6) Uani 0.40 1 d PDU B 2 O1F O 0.5256(15) 0.7147(8) 0.1389(6) 0.140(7) Uani 0.40 1 d PDU B 2 O1G O 0.5063(17) 0.7580(10) 0.0302(8) 0.173(9) Uani 0.40 1 d PDU B 2 O1H O 0.7115(12) 0.7334(8) 0.0525(7) 0.127(6) Uani 0.40 1 d PDU B 2 Cl2 Cl 0.83751(18) 0.14778(10) 0.48748(10) 0.0581(5) Uani 1 1 d D . . O2A O 0.8328(7) 0.0778(2) 0.5018(4) 0.134(3) Uani 1 1 d D . . O2B O 0.8758(6) 0.1612(4) 0.5400(3) 0.132(3) Uani 1 1 d D . . O2C O 0.9314(6) 0.1745(3) 0.4285(3) 0.122(3) Uani 1 1 d D . . O2D O 0.7138(5) 0.1761(3) 0.4795(4) 0.156(4) Uani 1 1 d D . . Cl3 Cl 0.51745(17) 0.36999(9) 0.54999(8) 0.0469(5) Uani 1 1 d D . . O3A O 0.6503(4) 0.3946(3) 0.5265(2) 0.0710(16) Uani 1 1 d D . . O3B O 0.4287(5) 0.4239(2) 0.5439(2) 0.0727(16) Uani 1 1 d D . . O3C O 0.4914(5) 0.3295(3) 0.5136(2) 0.0783(17) Uani 1 1 d D . . O3D O 0.5023(5) 0.3333(2) 0.6186(2) 0.0729(16) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0213(5) 0.0294(6) 0.0209(6) -0.0089(5) 0.0012(4) -0.0035(4) V2 0.0203(5) 0.0307(6) 0.0193(6) -0.0084(5) -0.0007(4) -0.0023(4) P1 0.0248(9) 0.0452(11) 0.0172(9) -0.0110(8) -0.0017(7) 0.0002(7) O1 0.027(2) 0.029(2) 0.031(2) -0.0079(19) -0.0016(18) -0.0008(18) O2 0.024(2) 0.033(2) 0.024(2) -0.0072(19) 0.0001(17) -0.0012(18) O3 0.019(2) 0.036(2) 0.019(2) -0.0104(19) 0.0005(16) -0.0035(17) O4 0.026(2) 0.052(3) 0.016(2) -0.007(2) 0.0030(17) -0.0109(19) O5 0.025(2) 0.045(3) 0.018(2) -0.0075(19) 0.0014(17) -0.0053(19) O6 0.042(3) 0.045(3) 0.035(3) -0.023(2) 0.003(2) 0.000(2) O7 0.029(2) 0.068(3) 0.020(2) -0.010(2) -0.0035(18) 0.011(2) N1 0.028(3) 0.032(3) 0.020(3) -0.012(2) 0.005(2) -0.004(2) N2 0.028(3) 0.034(3) 0.022(3) -0.011(3) -0.003(2) -0.005(2) N3 0.020(3) 0.030(3) 0.023(3) -0.007(3) 0.000(2) -0.008(2) N4 0.021(3) 0.028(3) 0.021(3) -0.004(2) -0.001(2) -0.003(2) N5 0.022(3) 0.029(3) 0.026(3) -0.006(2) -0.004(2) -0.002(2) N6 0.023(3) 0.038(3) 0.027(3) -0.010(3) -0.005(2) 0.003(2) C1 0.024(3) 0.024(4) 0.025(3) -0.012(3) -0.002(3) 0.004(3) C2 0.019(3) 0.036(4) 0.023(3) -0.007(3) -0.001(3) -0.003(3) C3 0.029(4) 0.038(4) 0.034(4) -0.016(3) 0.005(3) -0.002(3) C4 0.026(3) 0.029(4) 0.029(4) -0.011(3) -0.004(3) -0.002(3) C5 0.029(4) 0.045(4) 0.019(3) -0.014(3) -0.005(3) -0.002(3) C6 0.020(3) 0.033(4) 0.021(3) -0.011(3) 0.000(2) -0.005(3) C7 0.045(4) 0.043(4) 0.036(4) -0.024(3) 0.000(3) -0.001(3) C8 0.054(5) 0.070(5) 0.035(4) -0.035(4) 0.001(3) -0.003(4) C9 0.067(6) 0.068(6) 0.088(6) -0.051(5) 0.005(5) -0.027(4) C10 0.134(9) 0.064(6) 0.065(6) -0.035(5) 0.000(6) 0.027(6) C11 0.026(3) 0.036(4) 0.034(4) -0.015(3) -0.002(3) 0.005(3) C12 0.036(4) 0.046(4) 0.024(4) -0.009(3) 0.010(3) -0.013(3) C13 0.024(3) 0.039(4) 0.034(4) -0.013(3) -0.002(3) -0.003(3) C14 0.046(5) 0.048(5) 0.042(4) -0.006(4) 0.020(4) -0.012(4) C15 0.028(4) 0.079(6) 0.062(5) -0.035(5) 0.017(4) -0.005(4) C16 0.026(4) 0.057(5) 0.045(4) -0.015(4) 0.009(3) -0.005(3) C17 0.031(4) 0.047(4) 0.031(4) -0.010(3) -0.005(3) 0.003(3) C18 0.025(3) 0.032(4) 0.028(4) -0.010(3) 0.005(3) -0.009(3) C19 0.021(3) 0.041(4) 0.036(4) -0.019(3) 0.004(3) -0.009(3) C20 0.036(4) 0.043(4) 0.038(4) -0.018(4) -0.013(3) -0.002(3) C21 0.034(4) 0.070(6) 0.036(4) -0.034(4) -0.003(3) 0.000(4) C22 0.037(4) 0.042(4) 0.034(4) -0.007(3) -0.008(3) -0.004(3) C23 0.030(4) 0.041(4) 0.031(4) -0.014(3) -0.002(3) -0.002(3) C24 0.025(3) 0.043(4) 0.019(3) -0.012(3) 0.002(3) -0.004(3) C25 0.030(3) 0.027(4) 0.018(3) -0.002(3) 0.003(3) -0.003(3) C26 0.025(3) 0.026(4) 0.027(4) -0.009(3) -0.001(3) -0.005(3) C27 0.032(4) 0.034(4) 0.033(4) -0.008(3) -0.001(3) -0.005(3) C28 0.029(4) 0.037(4) 0.045(5) -0.009(3) 0.000(3) -0.005(3) C29 0.034(4) 0.046(4) 0.044(4) -0.018(4) -0.014(3) -0.004(3) C30 0.028(4) 0.044(4) 0.035(4) -0.019(3) -0.007(3) -0.001(3) C31 0.028(3) 0.043(4) 0.026(4) -0.016(3) -0.004(3) -0.005(3) C32 0.024(3) 0.034(4) 0.026(4) -0.010(3) -0.006(3) -0.002(3) C33 0.036(4) 0.038(4) 0.046(5) -0.017(4) -0.004(3) 0.007(3) C34 0.045(4) 0.031(4) 0.052(5) -0.008(4) -0.010(4) 0.009(3) C35 0.051(5) 0.042(5) 0.034(4) -0.004(4) 0.005(3) 0.006(4) C36 0.022(3) 0.053(5) 0.037(4) -0.014(4) -0.011(3) 0.007(3) V3 0.0298(6) 0.0304(7) 0.0301(6) -0.0090(5) -0.0092(5) -0.0039(5) V4 0.0295(6) 0.0323(7) 0.0292(6) -0.0101(5) -0.0089(5) -0.0044(5) P2 0.0331(10) 0.0640(13) 0.0361(11) -0.0276(10) -0.0054(8) -0.0048(9) O8 0.038(3) 0.039(3) 0.041(3) -0.007(2) -0.015(2) -0.005(2) O9 0.038(3) 0.031(3) 0.046(3) -0.008(2) -0.018(2) 0.001(2) O10 0.033(2) 0.026(2) 0.024(2) -0.0040(19) -0.0081(18) -0.0021(18) O11 0.035(3) 0.050(3) 0.029(2) -0.020(2) -0.0073(19) -0.002(2) O12 0.040(3) 0.054(3) 0.035(3) -0.025(2) -0.005(2) -0.014(2) O13 0.089(4) 0.115(5) 0.041(3) 0.001(3) -0.020(3) -0.047(4) O14 0.048(3) 0.157(6) 0.135(5) -0.123(5) -0.031(3) 0.026(3) N7 0.033(3) 0.030(3) 0.028(3) -0.008(2) -0.012(2) -0.005(2) N8 0.028(3) 0.034(3) 0.021(3) -0.002(2) -0.008(2) -0.002(2) N9 0.032(3) 0.030(3) 0.035(3) -0.011(3) -0.011(2) -0.003(2) N10 0.030(3) 0.034(3) 0.035(3) -0.015(3) -0.013(2) 0.000(2) N11 0.031(3) 0.028(3) 0.031(3) -0.013(3) -0.006(2) 0.001(2) N12 0.021(3) 0.042(3) 0.044(4) -0.020(3) -0.008(2) 0.001(2) C37 0.025(3) 0.037(4) 0.028(4) -0.007(3) -0.005(3) 0.004(3) C38 0.030(3) 0.022(4) 0.021(3) -0.006(3) -0.003(3) -0.003(3) C39 0.039(4) 0.024(4) 0.041(4) -0.009(3) -0.011(3) 0.003(3) C40 0.026(3) 0.032(4) 0.026(4) -0.005(3) -0.005(3) -0.003(3) C41 0.037(4) 0.031(4) 0.018(3) -0.009(3) -0.004(3) 0.000(3) C42 0.029(3) 0.033(4) 0.035(4) -0.019(3) -0.013(3) 0.005(3) C43 0.040(4) 0.034(4) 0.023(4) -0.002(3) -0.011(3) 0.004(3) C44 0.043(4) 0.057(5) 0.026(4) -0.004(3) -0.008(3) 0.013(3) C45 0.036(4) 0.059(5) 0.039(4) -0.010(4) 0.000(3) 0.002(3) C46 0.078(6) 0.035(4) 0.037(4) -0.004(3) 0.000(4) 0.001(4) C47 0.038(4) 0.025(4) 0.036(4) -0.004(3) -0.015(3) -0.001(3) C48 0.045(4) 0.037(4) 0.034(4) -0.014(3) -0.011(3) 0.003(3) C49 0.028(4) 0.039(4) 0.027(4) -0.016(3) 0.002(3) -0.011(3) C50 0.041(4) 0.046(4) 0.036(4) -0.023(3) -0.002(3) -0.016(3) C51 0.027(4) 0.067(5) 0.035(4) -0.025(4) -0.012(3) -0.005(3) C52 0.025(4) 0.058(5) 0.031(4) -0.015(4) -0.004(3) -0.008(3) C53 0.037(4) 0.056(5) 0.025(4) -0.013(3) -0.004(3) -0.002(3) C54 0.040(4) 0.029(4) 0.031(4) -0.006(3) -0.008(3) -0.007(3) C55 0.029(4) 0.035(4) 0.036(4) -0.015(3) -0.012(3) -0.004(3) C56 0.039(4) 0.052(5) 0.029(4) -0.013(3) 0.001(3) -0.018(3) C57 0.039(4) 0.063(5) 0.043(5) -0.028(4) 0.000(3) -0.003(4) C58 0.042(4) 0.046(5) 0.050(5) -0.026(4) -0.012(4) 0.003(3) C59 0.029(4) 0.033(4) 0.045(4) -0.017(3) -0.010(3) 0.002(3) C60 0.031(4) 0.026(4) 0.031(4) -0.009(3) -0.001(3) -0.003(3) C61 0.031(4) 0.025(4) 0.033(4) -0.009(3) -0.003(3) 0.001(3) C62 0.039(4) 0.025(4) 0.036(4) -0.011(3) -0.013(3) -0.003(3) C63 0.049(4) 0.029(4) 0.046(4) -0.019(3) -0.006(4) -0.005(3) C64 0.030(4) 0.046(4) 0.053(5) -0.018(4) -0.006(3) -0.008(3) C65 0.033(4) 0.042(4) 0.055(5) -0.023(4) 0.006(3) -0.013(3) C66 0.046(4) 0.039(4) 0.038(4) -0.024(3) 0.000(3) -0.004(3) C67 0.036(4) 0.042(4) 0.036(4) -0.017(3) -0.015(3) -0.002(3) C68 0.029(4) 0.023(4) 0.042(4) -0.013(3) -0.012(3) -0.005(3) C69 0.031(4) 0.036(4) 0.051(5) -0.008(4) -0.011(3) -0.002(3) C70 0.045(4) 0.030(4) 0.061(5) -0.015(4) -0.013(4) 0.010(3) C71 0.039(4) 0.036(5) 0.077(6) -0.023(4) -0.015(4) 0.008(3) C72 0.037(4) 0.051(5) 0.046(4) -0.028(4) -0.007(3) 0.001(3) Cl1 0.121(2) 0.0553(16) 0.0828(19) -0.0115(14) -0.0106(16) 0.0141(15) O1A 0.155(9) 0.096(7) 0.089(7) -0.043(6) -0.024(6) 0.021(6) O1B 0.100(6) 0.026(4) 0.105(6) -0.024(4) -0.057(5) 0.006(4) O1C 0.218(11) 0.173(10) 0.201(11) -0.058(9) 0.006(8) -0.046(9) O1D 0.223(11) 0.152(9) 0.182(10) -0.055(8) -0.056(8) 0.096(8) Cl1A 0.121(2) 0.0553(16) 0.0828(19) -0.0115(14) -0.0106(16) 0.0141(15) O1E 0.127(10) 0.064(8) 0.147(10) -0.002(7) -0.020(8) 0.014(8) O1F 0.112(10) 0.123(11) 0.140(11) 0.014(8) -0.011(8) -0.023(8) O1G 0.188(13) 0.181(13) 0.166(12) -0.061(9) -0.059(9) 0.011(9) O1H 0.125(10) 0.119(10) 0.115(10) -0.030(8) 0.001(8) 0.046(8) Cl2 0.0498(12) 0.0562(13) 0.0589(13) 0.0030(10) -0.0205(10) -0.0118(10) O2A 0.160(7) 0.052(4) 0.155(7) 0.005(4) -0.016(6) -0.002(4) O2B 0.110(6) 0.205(8) 0.152(7) -0.128(7) -0.079(5) 0.064(5) O2C 0.108(6) 0.158(7) 0.067(4) 0.007(4) -0.002(4) -0.045(5) O2D 0.075(5) 0.112(6) 0.255(10) 0.018(6) -0.095(6) 0.005(4) Cl3 0.0442(11) 0.0623(13) 0.0371(11) -0.0234(10) -0.0018(8) -0.0018(9) O3A 0.051(3) 0.111(5) 0.059(3) -0.046(3) 0.008(3) -0.025(3) O3B 0.074(4) 0.081(4) 0.062(4) -0.022(3) -0.013(3) 0.012(3) O3C 0.070(4) 0.105(5) 0.081(4) -0.066(4) -0.002(3) -0.012(3) O3D 0.082(4) 0.072(4) 0.046(3) -0.003(3) 0.001(3) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O1 1.594(4) . ? V1 O4 1.968(4) . ? V1 O3 2.060(3) . ? V1 N2 2.123(5) . ? V1 N3 2.126(4) . ? V1 N1 2.278(5) . ? V2 O2 1.597(4) . ? V2 O5 1.936(4) . ? V2 O3 2.041(4) . ? V2 N5 2.109(4) . ? V2 N4 2.146(4) . ? V2 N6 2.287(5) . ? P1 O4 1.514(4) . ? P1 O7 1.518(4) . ? P1 O5 1.534(4) . ? P1 O6 1.570(4) . ? O3 C1 1.388(6) . ? O6 H6 0.887 . ? O7 H7 0.840 . ? N1 C18 1.464(7) . ? N1 C12 1.483(7) . ? N1 C11 1.505(7) . ? N2 C13 1.319(7) . ? N2 C17 1.368(7) . ? N3 C19 1.332(7) . ? N3 C23 1.349(7) . ? N4 C31 1.488(7) . ? N4 C24 1.489(7) . ? N4 C25 1.521(7) . ? N5 C30 1.335(7) . ? N5 C26 1.360(7) . ? N6 C32 1.338(7) . ? N6 C36 1.346(7) . ? C1 C6 1.368(7) . ? C1 C2 1.391(7) . ? C2 C3 1.381(8) . ? C2 C11 1.506(8) . ? C3 C4 1.412(8) . ? C3 H3A 0.950 . ? C4 C5 1.358(8) . ? C4 C7 1.543(8) . ? C5 C6 1.413(7) . ? C5 H5A 0.950 . ? C6 C24 1.521(8) . ? C7 C10 1.520(10) . ? C7 C9 1.538(9) . ? C7 C8 1.567(9) . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? C10 H10A 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 C13 1.494(8) . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C13 C14 1.409(8) . ? C14 C15 1.386(9) . ? C14 H14A 0.950 . ? C15 C16 1.360(9) . ? C15 H15A 0.950 . ? C16 C17 1.355(8) . ? C16 H16A 0.950 . ? C17 H17A 0.950 . ? C18 C19 1.503(8) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 C20 1.380(8) . ? C20 C21 1.380(9) . ? C20 H20A 0.950 . ? C21 C22 1.367(8) . ? C21 H21A 0.950 . ? C22 C23 1.374(8) . ? C22 H22A 0.950 . ? C23 H23A 0.950 . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C25 C26 1.513(7) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 C27 1.370(8) . ? C27 C28 1.385(8) . ? C27 H27A 0.950 . ? C28 C29 1.398(8) . ? C28 H28A 0.950 . ? C29 C30 1.386(8) . ? C29 H29A 0.950 . ? C30 H30A 0.950 . ? C31 C32 1.492(8) . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C32 C33 1.383(8) . ? C33 C34 1.369(8) . ? C33 H33A 0.950 . ? C34 C35 1.381(9) . ? C34 H34A 0.950 . ? C35 C36 1.376(8) . ? C35 H35A 0.950 . ? C36 H36A 0.950 . ? V3 O8 1.600(4) . ? V3 O11 1.956(4) . ? V3 O10 2.048(4) . ? V3 N8 2.128(5) . ? V3 N9 2.146(5) . ? V3 N7 2.278(5) . ? V4 O9 1.605(4) . ? V4 O12 1.929(4) . ? V4 O10 2.030(4) . ? V4 N11 2.100(5) . ? V4 N10 2.136(5) . ? V4 N12 2.308(5) . ? P2 O14 1.503(5) . ? P2 O11 1.515(4) . ? P2 O12 1.526(4) . ? P2 O13 1.531(5) . ? O10 C37 1.372(6) . ? O13 H13 0.840 . ? O14 H14 0.840 . ? N7 C48 1.469(7) . ? N7 C47 1.491(7) . ? N7 C54 1.514(7) . ? N8 C49 1.335(7) . ? N8 C53 1.346(7) . ? N9 C59 1.346(7) . ? N9 C55 1.347(7) . ? N10 C67 1.492(7) . ? N10 C60 1.512(7) . ? N10 C61 1.524(7) . ? N11 C66 1.342(7) . ? N11 C62 1.362(7) . ? N12 C72 1.345(7) . ? N12 C68 1.358(7) . ? C37 C38 1.406(8) . ? C37 C42 1.406(8) . ? C38 C39 1.374(8) . ? C38 C47 1.496(7) . ? C39 C40 1.386(8) . ? C39 H39A 0.9500 . ? C40 C41 1.403(8) . ? C40 C43 1.525(8) . ? C41 C42 1.389(8) . ? C41 H41A 0.9500 . ? C42 C60 1.505(8) . ? C43 C46 1.515(8) . ? C43 C44 1.550(8) . ? C43 C45 1.553(8) . ? C44 H44A 0.980 . ? C44 H44B 0.980 . ? C44 H44C 0.980 . ? C45 H45A 0.980 . ? C45 H45B 0.980 . ? C45 H45C 0.980 . ? C46 H46A 0.980 . ? C46 H46B 0.980 . ? C46 H46C 0.980 . ? C47 H47A 0.990 . ? C47 H47B 0.990 . ? C48 C49 1.506(8) . ? C48 H48A 0.990 . ? C48 H48B 0.990 . ? C49 C50 1.372(8) . ? C50 C51 1.398(9) . ? C50 H50A 0.950 . ? C51 C52 1.371(8) . ? C51 H51A 0.950 . ? C52 C53 1.358(8) . ? C52 H52A 0.950 . ? C53 H53A 0.950 . ? C54 C55 1.491(8) . ? C54 H54A 0.990 . ? C54 H54B 0.990 . ? C55 C56 1.383(8) . ? C56 C57 1.374(9) . ? C56 H56A 0.950 . ? C57 C58 1.369(9) . ? C57 H57A 0.950 . ? C58 C59 1.384(8) . ? C58 H58A 0.950 . ? C59 H59A 0.950 . ? C60 H60A 0.990 . ? C60 H60B 0.990 . ? C61 C62 1.509(8) . ? C61 H61A 0.990 . ? C61 H61B 0.990 . ? C62 C63 1.368(8) . ? C63 C64 1.375(8) . ? C63 H63A 0.950 . ? C64 C65 1.368(8) . ? C64 H64A 0.950 . ? C65 C66 1.354(8) . ? C65 H65A 0.950 . ? C66 H66A 0.950 . ? C67 C68 1.507(8) . ? C67 H67A 0.990 . ? C67 H67B 0.990 . ? C68 C69 1.347(8) . ? C69 C70 1.386(8) . ? C69 H69A 0.950 . ? C70 C71 1.374(9) . ? C70 H70A 0.950 . ? C71 C72 1.362(9) . ? C71 H71A 0.950 . ? C72 H72A 0.950 . ? Cl1 O1B 1.360(6) . ? Cl1 O1C 1.405(8) . ? Cl1 O1D 1.434(7) . ? Cl1 O1A 1.501(7) . ? Cl2 O2B 1.405(5) . ? Cl2 O2D 1.411(5) . ? Cl2 O2C 1.419(5) . ? Cl2 O2A 1.424(5) . ? Cl3 O3C 1.416(4) . ? Cl3 O3B 1.425(4) . ? Cl3 O3A 1.431(4) . ? Cl3 O3D 1.438(4) . ? 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 O4 106.10(18) . . ? O1 V1 O3 106.37(17) . . ? O4 V1 O3 87.54(15) . . ? O1 V1 N2 94.28(19) . . ? O4 V1 N2 86.67(16) . . ? O3 V1 N2 159.34(18) . . ? O1 V1 N3 91.25(19) . . ? O4 V1 N3 162.54(18) . . ? O3 V1 N3 85.58(15) . . ? N2 V1 N3 94.17(17) . . ? O1 V1 N1 160.73(18) . . ? O4 V1 N1 88.48(17) . . ? O3 V1 N1 86.40(15) . . ? N2 V1 N1 73.65(17) . . ? N3 V1 N1 75.09(17) . . ? O2 V2 O5 106.80(17) . . ? O2 V2 O3 95.63(17) . . ? O5 V2 O3 95.00(15) . . ? O2 V2 N5 92.60(18) . . ? O5 V2 N5 92.86(17) . . ? O3 V2 N5 166.47(16) . . ? O2 V2 N4 92.22(18) . . ? O5 V2 N4 159.18(17) . . ? O3 V2 N4 91.40(15) . . ? N5 V2 N4 77.55(17) . . ? O2 V2 N6 167.26(18) . . ? O5 V2 N6 85.93(17) . . ? O3 V2 N6 82.65(16) . . ? N5 V2 N6 86.95(17) . . ? N4 V2 N6 75.25(17) . . ? O4 P1 O7 110.6(2) . . ? O4 P1 O5 111.8(2) . . ? O7 P1 O5 109.4(2) . . ? O4 P1 O6 106.6(2) . . ? O7 P1 O6 110.2(2) . . ? O5 P1 O6 108.2(2) . . ? C1 O3 V2 119.8(3) . . ? C1 O3 V1 121.8(3) . . ? V2 O3 V1 117.92(17) . . ? P1 O4 V1 137.0(2) . . ? P1 O5 V2 136.9(2) . . ? P1 O6 H6 114.5 . . ? P1 O7 H7 122.5 . . ? C18 N1 C12 110.9(4) . . ? C18 N1 C11 110.7(4) . . ? C12 N1 C11 109.8(4) . . ? C18 N1 V1 110.9(3) . . ? C12 N1 V1 104.7(3) . . ? C11 N1 V1 109.7(3) . . ? C13 N2 C17 118.3(5) . . ? C13 N2 V1 118.0(4) . . ? C17 N2 V1 123.7(4) . . ? C19 N3 C23 118.4(5) . . ? C19 N3 V1 120.1(4) . . ? C23 N3 V1 120.4(4) . . ? C31 N4 C24 109.5(4) . . ? C31 N4 C25 108.5(4) . . ? C24 N4 C25 111.7(4) . . ? C31 N4 V2 114.8(3) . . ? C24 N4 V2 109.2(3) . . ? C25 N4 V2 103.0(3) . . ? C30 N5 C26 119.0(5) . . ? C30 N5 V2 127.4(4) . . ? C26 N5 V2 113.6(3) . . ? C32 N6 C36 117.5(5) . . ? C32 N6 V2 115.0(4) . . ? C36 N6 V2 124.7(4) . . ? C6 C1 O3 121.6(5) . . ? C6 C1 C2 120.7(5) . . ? O3 C1 C2 117.7(5) . . ? C3 C2 C1 119.0(5) . . ? C3 C2 C11 120.5(5) . . ? C1 C2 C11 120.5(5) . . ? C2 C3 C4 121.9(6) . . ? C2 C3 H3A 119.0 . . ? C4 C3 H3A 119.0 . . ? C5 C4 C3 117.1(5) . . ? C5 C4 C7 124.5(5) . . ? C3 C4 C7 118.4(5) . . ? C4 C5 C6 122.4(5) . . ? C4 C5 H5A 118.8 . . ? C6 C5 H5A 118.8 . . ? C1 C6 C5 118.9(5) . . ? C1 C6 C24 121.3(5) . . ? C5 C6 C24 119.6(5) . . ? C10 C7 C9 110.9(7) . . ? C10 C7 C4 109.7(5) . . ? C9 C7 C4 109.4(5) . . ? C10 C7 C8 107.8(6) . . ? C9 C7 C8 108.8(5) . . ? C4 C7 C8 110.3(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C2 110.0(5) . . ? N1 C11 H11A 109.7 . . ? C2 C11 H11A 109.7 . . ? N1 C11 H11B 109.7 . . ? C2 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? N1 C12 C13 107.8(5) . . ? N1 C12 H12A 110.2 . . ? C13 C12 H12A 110.2 . . ? N1 C12 H12B 110.2 . . ? C13 C12 H12B 110.2 . . ? H12A C12 H12B 108.5 . . ? N2 C13 C14 121.5(6) . . ? N2 C13 C12 116.0(5) . . ? C14 C13 C12 122.5(6) . . ? C15 C14 C13 118.4(7) . . ? C15 C14 H14A 120.8 . . ? C13 C14 H14A 120.8 . . ? C16 C15 C14 119.9(6) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C17 C16 C15 118.9(6) . . ? C17 C16 H16A 120.6 . . ? C15 C16 H16A 120.6 . . ? C16 C17 N2 123.0(6) . . ? C16 C17 H17A 118.5 . . ? N2 C17 H17A 118.5 . . ? N1 C18 C19 111.1(4) . . ? N1 C18 H18A 109.4 . . ? C19 C18 H18A 109.4 . . ? N1 C18 H18B 109.4 . . ? C19 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? N3 C19 C20 121.6(6) . . ? N3 C19 C18 115.3(5) . . ? C20 C19 C18 123.0(6) . . ? C21 C20 C19 118.9(6) . . ? C21 C20 H20A 120.5 . . ? C19 C20 H20A 120.5 . . ? C22 C21 C20 120.2(6) . . ? C22 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? C21 C22 C23 117.6(6) . . ? C21 C22 H22A 121.2 . . ? C23 C22 H22A 121.2 . . ? N3 C23 C22 123.2(6) . . ? N3 C23 H23A 118.4 . . ? C22 C23 H23A 118.4 . . ? N4 C24 C6 109.2(4) . . ? N4 C24 H24A 109.8 . . ? C6 C24 H24A 109.8 . . ? N4 C24 H24B 109.8 . . ? C6 C24 H24B 109.8 . . ? H24A C24 H24B 108.3 . . ? C26 C25 N4 107.0(4) . . ? C26 C25 H25A 110.3 . . ? N4 C25 H25A 110.3 . . ? C26 C25 H25B 110.3 . . ? N4 C25 H25B 110.3 . . ? H25A C25 H25B 108.6 . . ? N5 C26 C27 122.1(5) . . ? N5 C26 C25 114.9(5) . . ? C27 C26 C25 123.0(5) . . ? C26 C27 C28 119.5(6) . . ? C26 C27 H27A 120.2 . . ? C28 C27 H27A 120.2 . . ? C27 C28 C29 118.3(6) . . ? C27 C28 H28A 120.9 . . ? C29 C28 H28A 120.9 . . ? C30 C29 C28 119.4(6) . . ? C30 C29 H29A 120.3 . . ? C28 C29 H29A 120.3 . . ? N5 C30 C29 121.7(6) . . ? N5 C30 H30A 119.1 . . ? C29 C30 H30A 119.1 . . ? N4 C31 C32 111.9(5) . . ? N4 C31 H31A 109.2 . . ? C32 C31 H31A 109.2 . . ? N4 C31 H31B 109.2 . . ? C32 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? N6 C32 C33 122.6(6) . . ? N6 C32 C31 114.3(5) . . ? C33 C32 C31 123.0(5) . . ? C34 C33 C32 119.1(6) . . ? C34 C33 H33A 120.5 . . ? C32 C33 H33A 120.5 . . ? C33 C34 C35 119.1(6) . . ? C33 C34 H34A 120.4 . . ? C35 C34 H34A 120.4 . . ? C36 C35 C34 118.6(6) . . ? C36 C35 H35A 120.7 . . ? C34 C35 H35A 120.7 . . ? N6 C36 C35 123.0(6) . . ? N6 C36 H36A 118.5 . . ? C35 C36 H36A 118.5 . . ? O8 V3 O11 105.7(2) . . ? O8 V3 O10 105.42(17) . . ? O11 V3 O10 87.98(16) . . ? O8 V3 N8 94.9(2) . . ? O11 V3 N8 88.85(17) . . ? O10 V3 N8 159.53(18) . . ? O8 V3 N9 92.0(2) . . ? O11 V3 N9 162.23(19) . . ? O10 V3 N9 85.58(16) . . ? N8 V3 N9 91.41(17) . . ? O8 V3 N7 162.43(19) . . ? O11 V3 N7 87.41(17) . . ? O10 V3 N7 86.30(15) . . ? N8 V3 N7 73.35(17) . . ? N9 V3 N7 75.67(18) . . ? O9 V4 O12 106.2(2) . . ? O9 V4 O10 96.55(18) . . ? O12 V4 O10 94.54(16) . . ? O9 V4 N11 92.79(19) . . ? O12 V4 N11 92.19(17) . . ? O10 V4 N11 166.49(17) . . ? O9 V4 N10 92.56(19) . . ? O12 V4 N10 159.29(18) . . ? O10 V4 N10 91.95(17) . . ? N11 V4 N10 77.87(18) . . ? O9 V4 N12 167.4(2) . . ? O12 V4 N12 86.41(18) . . ? O10 V4 N12 82.06(16) . . ? N11 V4 N12 86.70(17) . . ? N10 V4 N12 75.03(18) . . ? O14 P2 O11 113.2(3) . . ? O14 P2 O12 106.3(3) . . ? O11 P2 O12 112.9(2) . . ? O14 P2 O13 106.4(4) . . ? O11 P2 O13 107.8(3) . . ? O12 P2 O13 110.0(3) . . ? C37 O10 V4 119.4(3) . . ? C37 O10 V3 121.3(3) . . ? V4 O10 V3 118.90(18) . . ? P2 O11 V3 134.4(2) . . ? P2 O12 V4 136.9(3) . . ? P2 O13 H13 136.1 . . ? P2 O14 H14 124.3 . . ? C48 N7 C47 111.5(4) . . ? C48 N7 C54 109.3(4) . . ? C47 N7 C54 110.1(4) . . ? C48 N7 V3 104.9(3) . . ? C47 N7 V3 110.6(3) . . ? C54 N7 V3 110.4(3) . . ? C49 N8 C53 118.2(5) . . ? C49 N8 V3 118.4(4) . . ? C53 N8 V3 123.4(4) . . ? C59 N9 C55 118.9(5) . . ? C59 N9 V3 120.7(4) . . ? C55 N9 V3 119.5(4) . . ? C67 N10 C60 110.2(5) . . ? C67 N10 C61 107.4(4) . . ? C60 N10 C61 111.8(4) . . ? C67 N10 V4 116.2(3) . . ? C60 N10 V4 107.8(3) . . ? C61 N10 V4 103.3(3) . . ? C66 N11 C62 117.9(5) . . ? C66 N11 V4 128.6(4) . . ? C62 N11 V4 113.4(4) . . ? C72 N12 C68 116.9(5) . . ? C72 N12 V4 125.5(4) . . ? C68 N12 V4 115.4(4) . . ? O10 C37 C38 119.2(5) . . ? O10 C37 C42 120.8(5) . . ? C38 C37 C42 119.9(5) . . ? C39 C38 C37 118.6(5) . . ? C39 C38 C47 122.0(5) . . ? C37 C38 C47 119.5(5) . . ? C38 C39 C40 123.9(6) . . ? C38 C39 H39A 118.0 . . ? C40 C39 H39A 118.0 . . ? C39 C40 C41 116.3(5) . . ? C39 C40 C43 123.7(5) . . ? C41 C40 C43 120.0(5) . . ? C42 C41 C40 122.5(5) . . ? C42 C41 H41A 118.8 . . ? C40 C41 H41A 118.8 . . ? C41 C42 C37 118.8(5) . . ? C41 C42 C60 120.2(5) . . ? C37 C42 C60 120.8(5) . . ? C46 C43 C40 112.7(5) . . ? C46 C43 C44 108.3(5) . . ? C40 C43 C44 108.0(5) . . ? C46 C43 C45 108.5(5) . . ? C40 C43 C45 109.8(5) . . ? C44 C43 C45 109.5(5) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N7 C47 C38 109.6(5) . . ? N7 C47 H47A 109.8 . . ? C38 C47 H47A 109.8 . . ? N7 C47 H47B 109.8 . . ? C38 C47 H47B 109.8 . . ? H47A C47 H47B 108.2 . . ? N7 C48 C49 107.8(5) . . ? N7 C48 H48A 110.2 . . ? C49 C48 H48A 110.2 . . ? N7 C48 H48B 110.2 . . ? C49 C48 H48B 110.2 . . ? H48A C48 H48B 108.5 . . ? N8 C49 C50 121.6(6) . . ? N8 C49 C48 114.4(5) . . ? C50 C49 C48 124.0(6) . . ? C49 C50 C51 118.8(6) . . ? C49 C50 H50A 120.6 . . ? C51 C50 H50A 120.6 . . ? C52 C51 C50 119.9(6) . . ? C52 C51 H51A 120.1 . . ? C50 C51 H51A 120.1 . . ? C53 C52 C51 117.3(6) . . ? C53 C52 H52A 121.4 . . ? C51 C52 H52A 121.4 . . ? N8 C53 C52 124.3(6) . . ? N8 C53 H53A 117.9 . . ? C52 C53 H53A 117.9 . . ? C55 C54 N7 110.7(5) . . ? C55 C54 H54A 109.5 . . ? N7 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? N7 C54 H54B 109.5 . . ? H54A C54 H54B 108.1 . . ? N9 C55 C56 121.6(6) . . ? N9 C55 C54 116.1(5) . . ? C56 C55 C54 122.1(6) . . ? C57 C56 C55 118.8(6) . . ? C57 C56 H56A 120.6 . . ? C55 C56 H56A 120.6 . . ? C58 C57 C56 120.4(6) . . ? C58 C57 H57A 119.8 . . ? C56 C57 H57A 119.8 . . ? C57 C58 C59 118.3(6) . . ? C57 C58 H58A 120.9 . . ? C59 C58 H58A 120.9 . . ? N9 C59 C58 122.1(6) . . ? N9 C59 H59A 118.9 . . ? C58 C59 H59A 118.9 . . ? C42 C60 N10 107.2(4) . . ? C42 C60 H60A 110.3 . . ? N10 C60 H60A 110.3 . . ? C42 C60 H60B 110.3 . . ? N10 C60 H60B 110.3 . . ? H60A C60 H60B 108.5 . . ? C62 C61 N10 107.4(4) . . ? C62 C61 H61A 110.2 . . ? N10 C61 H61A 110.2 . . ? C62 C61 H61B 110.2 . . ? N10 C61 H61B 110.2 . . ? H61A C61 H61B 108.5 . . ? N11 C62 C63 119.9(6) . . ? N11 C62 C61 115.3(5) . . ? C63 C62 C61 124.8(5) . . ? C62 C63 C64 120.6(6) . . ? C62 C63 H63A 119.7 . . ? C64 C63 H63A 119.7 . . ? C65 C64 C63 119.6(6) . . ? C65 C64 H64A 120.2 . . ? C63 C64 H64A 120.2 . . ? C66 C65 C64 117.6(6) . . ? C66 C65 H65A 121.2 . . ? C64 C65 H65A 121.2 . . ? N11 C66 C65 124.3(6) . . ? N11 C66 H66A 117.8 . . ? C65 C66 H66A 117.8 . . ? N10 C67 C68 112.2(5) . . ? N10 C67 H67A 109.2 . . ? C68 C67 H67A 109.2 . . ? N10 C67 H67B 109.2 . . ? C68 C67 H67B 109.2 . . ? H67A C67 H67B 107.9 . . ? C69 C68 N12 122.8(6) . . ? C69 C68 C67 123.5(6) . . ? N12 C68 C67 113.7(5) . . ? C68 C69 C70 120.1(7) . . ? C68 C69 H69A 120.0 . . ? C70 C69 H69A 120.0 . . ? C71 C70 C69 117.4(6) . . ? C71 C70 H70A 121.3 . . ? C69 C70 H70A 121.3 . . ? C72 C71 C70 120.2(7) . . ? C72 C71 H71A 119.9 . . ? C70 C71 H71A 119.9 . . ? N12 C72 C71 122.6(6) . . ? N12 C72 H72A 118.7 . . ? C71 C72 H72A 118.7 . . ? O1B Cl1 O1C 116.7(7) . . ? O1B Cl1 O1D 112.4(6) . . ? O1C Cl1 O1D 109.3(6) . . ? O1B Cl1 O1A 108.3(5) . . ? O1C Cl1 O1A 105.7(6) . . ? O1D Cl1 O1A 103.3(6) . . ? O2B Cl2 O2D 109.6(4) . . ? O2B Cl2 O2C 110.4(4) . . ? O2D Cl2 O2C 109.1(4) . . ? O2B Cl2 O2A 107.9(4) . . ? O2D Cl2 O2A 111.5(4) . . ? O2C Cl2 O2A 108.3(4) . . ? O3C Cl3 O3B 110.4(3) . . ? O3C Cl3 O3A 109.5(3) . . ? O3B Cl3 O3A 109.8(3) . . ? O3C Cl3 O3D 111.2(3) . . ? O3B Cl3 O3D 108.0(3) . . ? O3A Cl3 O3D 108.0(3) . . ? 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 O2 V2 O3 C1 -117.0(4) . . . . ? O5 V2 O3 C1 135.6(4) . . . . ? N5 V2 O3 C1 10.2(9) . . . . ? N4 V2 O3 C1 -24.6(4) . . . . ? N6 V2 O3 C1 50.3(4) . . . . ? O2 V2 O3 V1 55.1(2) . . . . ? O5 V2 O3 V1 -52.4(2) . . . . ? N5 V2 O3 V1 -177.7(6) . . . . ? N4 V2 O3 V1 147.4(2) . . . . ? N6 V2 O3 V1 -137.6(2) . . . . ? O1 V1 O3 C1 127.3(4) . . . . ? O4 V1 O3 C1 -126.7(4) . . . . ? N2 V1 O3 C1 -52.9(6) . . . . ? N3 V1 O3 C1 37.3(4) . . . . ? N1 V1 O3 C1 -38.0(4) . . . . ? O1 V1 O3 V2 -44.6(2) . . . . ? O4 V1 O3 V2 61.5(2) . . . . ? N2 V1 O3 V2 135.3(4) . . . . ? N3 V1 O3 V2 -134.6(2) . . . . ? N1 V1 O3 V2 150.1(2) . . . . ? O7 P1 O4 V1 148.9(3) . . . . ? O5 P1 O4 V1 26.7(4) . . . . ? O6 P1 O4 V1 -91.3(4) . . . . ? O1 V1 O4 P1 54.0(4) . . . . ? O3 V1 O4 P1 -52.3(4) . . . . ? N2 V1 O4 P1 147.5(4) . . . . ? N3 V1 O4 P1 -119.1(5) . . . . ? N1 V1 O4 P1 -138.8(4) . . . . ? O4 P1 O5 V2 -3.1(4) . . . . ? O7 P1 O5 V2 -125.9(3) . . . . ? O6 P1 O5 V2 114.0(4) . . . . ? O2 V2 O5 P1 -79.7(4) . . . . ? O3 V2 O5 P1 17.8(4) . . . . ? N5 V2 O5 P1 -173.2(4) . . . . ? N4 V2 O5 P1 125.2(5) . . . . ? N6 V2 O5 P1 100.0(4) . . . . ? O1 V1 N1 C18 -30.9(7) . . . . ? O4 V1 N1 C18 -170.8(3) . . . . ? O3 V1 N1 C18 101.6(3) . . . . ? N2 V1 N1 C18 -83.8(3) . . . . ? N3 V1 N1 C18 15.2(3) . . . . ? O1 V1 N1 C12 88.7(6) . . . . ? O4 V1 N1 C12 -51.1(3) . . . . ? O3 V1 N1 C12 -138.7(3) . . . . ? N2 V1 N1 C12 35.9(3) . . . . ? N3 V1 N1 C12 134.9(4) . . . . ? O1 V1 N1 C11 -153.5(5) . . . . ? O4 V1 N1 C11 66.7(3) . . . . ? O3 V1 N1 C11 -21.0(3) . . . . ? N2 V1 N1 C11 153.6(4) . . . . ? N3 V1 N1 C11 -107.4(3) . . . . ? O1 V1 N2 C13 174.5(4) . . . . ? O4 V1 N2 C13 68.5(4) . . . . ? O3 V1 N2 C13 -5.4(7) . . . . ? N3 V1 N2 C13 -94.0(4) . . . . ? N1 V1 N2 C13 -20.8(4) . . . . ? O1 V1 N2 C17 -4.7(5) . . . . ? O4 V1 N2 C17 -110.7(4) . . . . ? O3 V1 N2 C17 175.4(4) . . . . ? N3 V1 N2 C17 86.8(4) . . . . ? N1 V1 N2 C17 160.0(5) . . . . ? O1 V1 N3 C19 167.3(4) . . . . ? O4 V1 N3 C19 -19.3(8) . . . . ? O3 V1 N3 C19 -86.4(4) . . . . ? N2 V1 N3 C19 72.9(4) . . . . ? N1 V1 N3 C19 1.0(4) . . . . ? O1 V1 N3 C23 -24.5(4) . . . . ? O4 V1 N3 C23 148.9(5) . . . . ? O3 V1 N3 C23 81.8(4) . . . . ? N2 V1 N3 C23 -118.9(4) . . . . ? N1 V1 N3 C23 169.3(4) . . . . ? O2 V2 N4 C31 -170.4(4) . . . . ? O5 V2 N4 C31 -14.1(7) . . . . ? O3 V2 N4 C31 93.9(4) . . . . ? N5 V2 N4 C31 -78.2(4) . . . . ? N6 V2 N4 C31 11.9(3) . . . . ? O2 V2 N4 C24 66.3(4) . . . . ? O5 V2 N4 C24 -137.4(5) . . . . ? O3 V2 N4 C24 -29.4(3) . . . . ? N5 V2 N4 C24 158.5(4) . . . . ? N6 V2 N4 C24 -111.4(4) . . . . ? O2 V2 N4 C25 -52.5(3) . . . . ? O5 V2 N4 C25 103.7(5) . . . . ? O3 V2 N4 C25 -148.2(3) . . . . ? N5 V2 N4 C25 39.6(3) . . . . ? N6 V2 N4 C25 129.7(3) . . . . ? O2 V2 N5 C30 -110.4(5) . . . . ? O5 V2 N5 C30 -3.4(5) . . . . ? O3 V2 N5 C30 122.1(7) . . . . ? N4 V2 N5 C30 157.9(5) . . . . ? N6 V2 N5 C30 82.3(5) . . . . ? O2 V2 N5 C26 68.3(4) . . . . ? O5 V2 N5 C26 175.3(4) . . . . ? O3 V2 N5 C26 -59.2(9) . . . . ? N4 V2 N5 C26 -23.4(4) . . . . ? N6 V2 N5 C26 -99.0(4) . . . . ? O2 V2 N6 C32 -4.0(10) . . . . ? O5 V2 N6 C32 177.5(4) . . . . ? O3 V2 N6 C32 -87.0(4) . . . . ? N5 V2 N6 C32 84.4(4) . . . . ? N4 V2 N6 C32 6.4(4) . . . . ? O2 V2 N6 C36 156.6(7) . . . . ? O5 V2 N6 C36 -22.0(5) . . . . ? O3 V2 N6 C36 73.6(5) . . . . ? N5 V2 N6 C36 -115.1(5) . . . . ? N4 V2 N6 C36 167.0(5) . . . . ? V2 O3 C1 C6 46.0(6) . . . . ? V1 O3 C1 C6 -125.7(5) . . . . ? V2 O3 C1 C2 -131.0(4) . . . . ? V1 O3 C1 C2 57.2(6) . . . . ? C6 C1 C2 C3 2.4(8) . . . . ? O3 C1 C2 C3 179.5(5) . . . . ? C6 C1 C2 C11 178.9(5) . . . . ? O3 C1 C2 C11 -4.0(7) . . . . ? C1 C2 C3 C4 -1.6(8) . . . . ? C11 C2 C3 C4 -178.1(5) . . . . ? C2 C3 C4 C5 0.4(8) . . . . ? C2 C3 C4 C7 -179.7(5) . . . . ? C3 C4 C5 C6 0.1(8) . . . . ? C7 C4 C5 C6 -179.8(5) . . . . ? O3 C1 C6 C5 -178.9(5) . . . . ? C2 C1 C6 C5 -2.0(8) . . . . ? O3 C1 C6 C24 -4.8(8) . . . . ? C2 C1 C6 C24 172.2(5) . . . . ? C4 C5 C6 C1 0.7(8) . . . . ? C4 C5 C6 C24 -173.6(5) . . . . ? C5 C4 C7 C10 -124.5(7) . . . . ? C3 C4 C7 C10 55.6(8) . . . . ? C5 C4 C7 C9 113.7(7) . . . . ? C3 C4 C7 C9 -66.2(7) . . . . ? C5 C4 C7 C8 -5.9(8) . . . . ? C3 C4 C7 C8 174.2(5) . . . . ? C18 N1 C11 C2 -56.0(6) . . . . ? C12 N1 C11 C2 -178.7(5) . . . . ? V1 N1 C11 C2 66.8(5) . . . . ? C3 C2 C11 N1 113.1(6) . . . . ? C1 C2 C11 N1 -63.4(7) . . . . ? C18 N1 C12 C13 73.5(6) . . . . ? C11 N1 C12 C13 -163.9(5) . . . . ? V1 N1 C12 C13 -46.1(5) . . . . ? C17 N2 C13 C14 0.4(8) . . . . ? V1 N2 C13 C14 -178.9(5) . . . . ? C17 N2 C13 C12 179.4(5) . . . . ? V1 N2 C13 C12 0.2(7) . . . . ? N1 C12 C13 N2 33.1(7) . . . . ? N1 C12 C13 C14 -147.9(6) . . . . ? N2 C13 C14 C15 -1.0(10) . . . . ? C12 C13 C14 C15 -180.0(6) . . . . ? C13 C14 C15 C16 1.5(11) . . . . ? C14 C15 C16 C17 -1.4(11) . . . . ? C15 C16 C17 N2 0.8(10) . . . . ? C13 N2 C17 C16 -0.3(9) . . . . ? V1 N2 C17 C16 178.9(5) . . . . ? C12 N1 C18 C19 -143.5(5) . . . . ? C11 N1 C18 C19 94.4(5) . . . . ? V1 N1 C18 C19 -27.6(5) . . . . ? C23 N3 C19 C20 -2.5(8) . . . . ? V1 N3 C19 C20 165.9(4) . . . . ? C23 N3 C19 C18 174.4(5) . . . . ? V1 N3 C19 C18 -17.2(6) . . . . ? N1 C18 C19 N3 29.9(7) . . . . ? N1 C18 C19 C20 -153.2(5) . . . . ? N3 C19 C20 C21 2.0(9) . . . . ? C18 C19 C20 C21 -174.7(5) . . . . ? C19 C20 C21 C22 -0.2(9) . . . . ? C20 C21 C22 C23 -0.9(9) . . . . ? C19 N3 C23 C22 1.4(8) . . . . ? V1 N3 C23 C22 -167.1(5) . . . . ? C21 C22 C23 N3 0.4(9) . . . . ? C31 N4 C24 C6 -57.3(5) . . . . ? C25 N4 C24 C6 -177.6(4) . . . . ? V2 N4 C24 C6 69.2(5) . . . . ? C1 C6 C24 N4 -59.9(7) . . . . ? C5 C6 C24 N4 114.2(5) . . . . ? C31 N4 C25 C26 71.8(5) . . . . ? C24 N4 C25 C26 -167.4(4) . . . . ? V2 N4 C25 C26 -50.4(4) . . . . ? C30 N5 C26 C27 -1.9(8) . . . . ? V2 N5 C26 C27 179.3(4) . . . . ? C30 N5 C26 C25 178.8(5) . . . . ? V2 N5 C26 C25 0.0(6) . . . . ? N4 C25 C26 N5 34.9(6) . . . . ? N4 C25 C26 C27 -144.4(5) . . . . ? N5 C26 C27 C28 0.7(9) . . . . ? C25 C26 C27 C28 179.9(5) . . . . ? C26 C27 C28 C29 0.3(9) . . . . ? C27 C28 C29 C30 0.0(9) . . . . ? C26 N5 C30 C29 2.2(8) . . . . ? V2 N5 C30 C29 -179.2(4) . . . . ? C28 C29 C30 N5 -1.2(9) . . . . ? C24 N4 C31 C32 95.6(5) . . . . ? C25 N4 C31 C32 -142.2(4) . . . . ? V2 N4 C31 C32 -27.5(6) . . . . ? C36 N6 C32 C33 -2.6(8) . . . . ? V2 N6 C32 C33 159.4(5) . . . . ? C36 N6 C32 C31 174.6(5) . . . . ? V2 N6 C32 C31 -23.4(6) . . . . ? N4 C31 C32 N6 33.4(6) . . . . ? N4 C31 C32 C33 -149.4(5) . . . . ? N6 C32 C33 C34 2.9(9) . . . . ? C31 C32 C33 C34 -174.0(6) . . . . ? C32 C33 C34 C35 -0.1(9) . . . . ? C33 C34 C35 C36 -2.9(10) . . . . ? C32 N6 C36 C35 -0.6(8) . . . . ? V2 N6 C36 C35 -160.7(5) . . . . ? C34 C35 C36 N6 3.3(9) . . . . ? O9 V4 O10 C37 -117.6(4) . . . . ? O12 V4 O10 C37 135.5(4) . . . . ? N11 V4 O10 C37 15.9(9) . . . . ? N10 V4 O10 C37 -24.8(4) . . . . ? N12 V4 O10 C37 49.8(4) . . . . ? O9 V4 O10 V3 55.6(2) . . . . ? O12 V4 O10 V3 -51.2(2) . . . . ? N11 V4 O10 V3 -170.9(6) . . . . ? N10 V4 O10 V3 148.4(2) . . . . ? N12 V4 O10 V3 -137.0(2) . . . . ? O8 V3 O10 C37 129.1(4) . . . . ? O11 V3 O10 C37 -125.1(4) . . . . ? N8 V3 O10 C37 -43.9(7) . . . . ? N9 V3 O10 C37 38.3(4) . . . . ? N7 V3 O10 C37 -37.6(4) . . . . ? O8 V3 O10 V4 -44.0(3) . . . . ? O11 V3 O10 V4 61.8(2) . . . . ? N8 V3 O10 V4 143.0(4) . . . . ? N9 V3 O10 V4 -134.8(2) . . . . ? N7 V3 O10 V4 149.3(2) . . . . ? O14 P2 O11 V3 151.7(4) . . . . ? O12 P2 O11 V3 30.8(4) . . . . ? O13 P2 O11 V3 -90.9(4) . . . . ? O8 V3 O11 P2 51.2(4) . . . . ? O10 V3 O11 P2 -54.2(4) . . . . ? N8 V3 O11 P2 146.0(4) . . . . ? N9 V3 O11 P2 -123.0(5) . . . . ? N7 V3 O11 P2 -140.6(4) . . . . ? O14 P2 O12 V4 -131.3(4) . . . . ? O11 P2 O12 V4 -6.5(5) . . . . ? O13 P2 O12 V4 113.9(4) . . . . ? O9 V4 O12 P2 -79.9(4) . . . . ? O10 V4 O12 P2 18.3(4) . . . . ? N11 V4 O12 P2 -173.4(4) . . . . ? N10 V4 O12 P2 126.2(5) . . . . ? N12 V4 O12 P2 100.0(4) . . . . ? O8 V3 N7 C48 86.1(7) . . . . ? O11 V3 N7 C48 -53.0(4) . . . . ? O10 V3 N7 C48 -141.2(4) . . . . ? N8 V3 N7 C48 36.6(3) . . . . ? N9 V3 N7 C48 132.5(4) . . . . ? O8 V3 N7 C47 -153.6(6) . . . . ? O11 V3 N7 C47 67.3(4) . . . . ? O10 V3 N7 C47 -20.9(4) . . . . ? N8 V3 N7 C47 156.8(4) . . . . ? N9 V3 N7 C47 -107.3(4) . . . . ? O8 V3 N7 C54 -31.5(8) . . . . ? O11 V3 N7 C54 -170.6(3) . . . . ? O10 V3 N7 C54 101.2(3) . . . . ? N8 V3 N7 C54 -81.1(4) . . . . ? N9 V3 N7 C54 14.8(3) . . . . ? O8 V3 N8 C49 173.5(4) . . . . ? O11 V3 N8 C49 67.8(4) . . . . ? O10 V3 N8 C49 -13.3(7) . . . . ? N9 V3 N8 C49 -94.4(4) . . . . ? N7 V3 N8 C49 -19.8(4) . . . . ? O8 V3 N8 C53 -8.2(5) . . . . ? O11 V3 N8 C53 -113.9(4) . . . . ? O10 V3 N8 C53 165.0(5) . . . . ? N9 V3 N8 C53 83.9(5) . . . . ? N7 V3 N8 C53 158.5(5) . . . . ? O8 V3 N9 C59 -23.0(4) . . . . ? O11 V3 N9 C59 151.4(5) . . . . ? O10 V3 N9 C59 82.3(4) . . . . ? N8 V3 N9 C59 -117.9(4) . . . . ? N7 V3 N9 C59 169.7(4) . . . . ? O8 V3 N9 C55 168.7(4) . . . . ? O11 V3 N9 C55 -16.9(8) . . . . ? O10 V3 N9 C55 -86.0(4) . . . . ? N8 V3 N9 C55 73.7(4) . . . . ? N7 V3 N9 C55 1.3(4) . . . . ? O9 V4 N10 C67 -170.3(4) . . . . ? O12 V4 N10 C67 -15.3(7) . . . . ? O10 V4 N10 C67 93.0(4) . . . . ? N11 V4 N10 C67 -78.0(4) . . . . ? N12 V4 N10 C67 11.8(4) . . . . ? O9 V4 N10 C60 65.4(4) . . . . ? O12 V4 N10 C60 -139.5(5) . . . . ? O10 V4 N10 C60 -31.2(3) . . . . ? N11 V4 N10 C60 157.7(4) . . . . ? N12 V4 N10 C60 -112.5(3) . . . . ? O9 V4 N10 C61 -53.0(3) . . . . ? O12 V4 N10 C61 102.1(5) . . . . ? O10 V4 N10 C61 -149.6(3) . . . . ? N11 V4 N10 C61 39.3(3) . . . . ? N12 V4 N10 C61 129.1(3) . . . . ? O9 V4 N11 C66 -108.1(5) . . . . ? O12 V4 N11 C66 -1.8(5) . . . . ? O10 V4 N11 C66 118.1(8) . . . . ? N10 V4 N11 C66 159.8(5) . . . . ? N12 V4 N11 C66 84.4(5) . . . . ? O9 V4 N11 C62 67.5(4) . . . . ? O12 V4 N11 C62 173.9(4) . . . . ? O10 V4 N11 C62 -66.2(9) . . . . ? N10 V4 N11 C62 -24.5(4) . . . . ? N12 V4 N11 C62 -99.9(4) . . . . ? O9 V4 N12 C72 158.4(8) . . . . ? O12 V4 N12 C72 -21.2(5) . . . . ? O10 V4 N12 C72 73.9(5) . . . . ? N11 V4 N12 C72 -113.6(5) . . . . ? N10 V4 N12 C72 168.1(5) . . . . ? O9 V4 N12 C68 -4.3(11) . . . . ? O12 V4 N12 C68 176.1(4) . . . . ? O10 V4 N12 C68 -88.8(4) . . . . ? N11 V4 N12 C68 83.7(4) . . . . ? N10 V4 N12 C68 5.4(4) . . . . ? V4 O10 C37 C38 -130.3(4) . . . . ? V3 O10 C37 C38 56.6(6) . . . . ? V4 O10 C37 C42 46.9(6) . . . . ? V3 O10 C37 C42 -126.1(5) . . . . ? O10 C37 C38 C39 177.6(5) . . . . ? C42 C37 C38 C39 0.3(8) . . . . ? O10 C37 C38 C47 -3.4(8) . . . . ? C42 C37 C38 C47 179.3(5) . . . . ? C37 C38 C39 C40 0.2(9) . . . . ? C47 C38 C39 C40 -178.7(6) . . . . ? C38 C39 C40 C41 0.2(9) . . . . ? C38 C39 C40 C43 -177.9(5) . . . . ? C39 C40 C41 C42 -1.3(8) . . . . ? C43 C40 C41 C42 176.9(5) . . . . ? C40 C41 C42 C37 1.9(8) . . . . ? C40 C41 C42 C60 -172.5(5) . . . . ? O10 C37 C42 C41 -178.5(5) . . . . ? C38 C37 C42 C41 -1.3(8) . . . . ? O10 C37 C42 C60 -4.2(8) . . . . ? C38 C37 C42 C60 173.0(5) . . . . ? C39 C40 C43 C46 0.5(8) . . . . ? C41 C40 C43 C46 -177.5(5) . . . . ? C39 C40 C43 C44 120.2(6) . . . . ? C41 C40 C43 C44 -57.9(7) . . . . ? C39 C40 C43 C45 -120.6(6) . . . . ? C41 C40 C43 C45 61.4(7) . . . . ? C48 N7 C47 C38 -177.0(5) . . . . ? C54 N7 C47 C38 -55.5(6) . . . . ? V3 N7 C47 C38 66.7(5) . . . . ? C39 C38 C47 N7 115.6(6) . . . . ? C37 C38 C47 N7 -63.4(7) . . . . ? C47 N7 C48 C49 -167.8(5) . . . . ? C54 N7 C48 C49 70.2(6) . . . . ? V3 N7 C48 C49 -48.2(5) . . . . ? C53 N8 C49 C50 -1.0(8) . . . . ? V3 N8 C49 C50 177.4(4) . . . . ? C53 N8 C49 C48 179.8(5) . . . . ? V3 N8 C49 C48 -1.8(6) . . . . ? N7 C48 C49 N8 35.4(7) . . . . ? N7 C48 C49 C50 -143.8(6) . . . . ? N8 C49 C50 C51 -0.6(9) . . . . ? C48 C49 C50 C51 178.5(6) . . . . ? C49 C50 C51 C52 1.5(9) . . . . ? C50 C51 C52 C53 -0.7(9) . . . . ? C49 N8 C53 C52 1.8(9) . . . . ? V3 N8 C53 C52 -176.5(4) . . . . ? C51 C52 C53 N8 -0.9(9) . . . . ? C48 N7 C54 C55 -142.6(5) . . . . ? C47 N7 C54 C55 94.6(5) . . . . ? V3 N7 C54 C55 -27.7(5) . . . . ? C59 N9 C55 C56 -1.5(8) . . . . ? V3 N9 C55 C56 167.1(4) . . . . ? C59 N9 C55 C54 173.3(5) . . . . ? V3 N9 C55 C54 -18.2(6) . . . . ? N7 C54 C55 N9 30.6(7) . . . . ? N7 C54 C55 C56 -154.7(5) . . . . ? N9 C55 C56 C57 1.8(9) . . . . ? C54 C55 C56 C57 -172.6(5) . . . . ? C55 C56 C57 C58 -1.4(9) . . . . ? C56 C57 C58 C59 0.8(9) . . . . ? C55 N9 C59 C58 0.8(8) . . . . ? V3 N9 C59 C58 -167.6(5) . . . . ? C57 C58 C59 N9 -0.4(9) . . . . ? C41 C42 C60 N10 112.1(6) . . . . ? C37 C42 C60 N10 -62.2(7) . . . . ? C67 N10 C60 C42 -55.8(6) . . . . ? C61 N10 C60 C42 -175.2(4) . . . . ? V4 N10 C60 C42 72.0(5) . . . . ? C67 N10 C61 C62 74.5(5) . . . . ? C60 N10 C61 C62 -164.5(5) . . . . ? V4 N10 C61 C62 -48.8(5) . . . . ? C66 N11 C62 C63 -2.4(8) . . . . ? V4 N11 C62 C63 -178.6(5) . . . . ? C66 N11 C62 C61 178.4(5) . . . . ? V4 N11 C62 C61 2.2(6) . . . . ? N10 C61 C62 N11 32.4(7) . . . . ? N10 C61 C62 C63 -146.8(6) . . . . ? N11 C62 C63 C64 2.2(9) . . . . ? C61 C62 C63 C64 -178.6(6) . . . . ? C62 C63 C64 C65 -0.7(10) . . . . ? C63 C64 C65 C66 -0.6(10) . . . . ? C62 N11 C66 C65 1.1(9) . . . . ? V4 N11 C66 C65 176.7(5) . . . . ? C64 C65 C66 N11 0.4(10) . . . . ? C60 N10 C67 C68 96.6(5) . . . . ? C61 N10 C67 C68 -141.4(5) . . . . ? V4 N10 C67 C68 -26.4(6) . . . . ? C72 N12 C68 C69 -2.2(8) . . . . ? V4 N12 C68 C69 162.0(5) . . . . ? C72 N12 C68 C67 174.8(5) . . . . ? V4 N12 C68 C67 -21.0(6) . . . . ? N10 C67 C68 C69 -152.4(6) . . . . ? N10 C67 C68 N12 30.6(7) . . . . ? N12 C68 C69 C70 1.0(9) . . . . ? C67 C68 C69 C70 -175.7(5) . . . . ? C68 C69 C70 C71 2.0(9) . . . . ? C69 C70 C71 C72 -3.8(9) . . . . ? C68 N12 C72 C71 0.4(8) . . . . ? V4 N12 C72 C71 -162.1(5) . . . . ? C70 C71 C72 N12 2.6(10) . . . . ? # SQUEEZE RESULTS loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.124 0.244 0.860 266.9 100.6 2 0.107 0.756 0.140 267.1 99.3 3 0.144 0.261 0.407 30.1 14.8 4 0.856 0.739 0.593 30.1 14.2 _platon_squeeze_details ; Total electron count corrected for: 228.9. The solvent could comprise either water or methanol. ; #---------------------------------------------------------------------- data_4 _database_code_depnum_ccdc_archive 'CCDC 722651' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H49 N6 O7 P V2 +, 2(Cl O4 -)' _chemical_formula_sum 'C48 H49 Cl2 N6 O15 P V2' _chemical_formula_weight 1153.68 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' P P 0.1023 0.0942 '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 trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 34.3754(12) _cell_length_b 34.3754(12) _cell_length_c 24.9569(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 25539.7(15) _cell_formula_units_Z 18 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9617 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.00 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10692 _exptl_absorpt_coefficient_mu 0.518 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.687 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _exptl_special_details ; This CIF refers to refinement against SQUEEZED data (v.d.Sluis & Spek, 1990), with all lattice solvent omitted. See the bottom of this CIF for details of the SQUEEZE process. The Cl---O and O...O distances of the perchlorate anions are restrained to a single refined value and 1.633 times that value, respectively. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 40700 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 28.00 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.987 _reflns_number_total 13547 _reflns_number_gt 10499 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _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^)+(0.0770P)^2^] 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 13547 _refine_ls_number_parameters 695 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1339 _refine_ls_wR_factor_gt 0.1264 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.461 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.074 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 0.487034(11) 0.406085(11) 0.555264(14) 0.01832(9) Uani 1 1 d . . . V2 V 0.499104(11) 0.486464(11) 0.652468(14) 0.01880(9) Uani 1 1 d . . . P1 P 0.415816(18) 0.388730(18) 0.64736(2) 0.02095(12) Uani 1 1 d . . . O1 O 0.47575(5) 0.44033(5) 0.52510(6) 0.0256(3) Uani 1 1 d . . . O2 O 0.47232(5) 0.49763(5) 0.60824(6) 0.0258(3) Uani 1 1 d . . . O3 O 0.52549(5) 0.45228(5) 0.61394(5) 0.0197(3) Uani 1 1 d . . . O4 O 0.43381(5) 0.37192(5) 0.60346(6) 0.0233(3) Uani 1 1 d . . . O5 O 0.45081(5) 0.42609(5) 0.68119(6) 0.0236(3) Uani 1 1 d . . . O6 O 0.38216(5) 0.34792(5) 0.68343(6) 0.0290(4) Uani 1 1 d . . . O7 O 0.38436(5) 0.40616(5) 0.62550(6) 0.0275(3) Uani 1 1 d . . . N1 N 0.54467(6) 0.42222(6) 0.50720(7) 0.0202(4) Uani 1 1 d . . . N2 N 0.51795(6) 0.36767(6) 0.59584(7) 0.0248(4) Uani 1 1 d . . . N3 N 0.45888(6) 0.35861(6) 0.49157(7) 0.0221(4) Uani 1 1 d . . . N4 N 0.54422(6) 0.49353(6) 0.72321(7) 0.0221(4) Uani 1 1 d . . . N5 N 0.56050(6) 0.54523(6) 0.63484(7) 0.0206(4) Uani 1 1 d . . . N6 N 0.48048(6) 0.51534(6) 0.71602(7) 0.0252(4) Uani 1 1 d . . . C1 C 0.57077(7) 0.46658(7) 0.61862(8) 0.0195(4) Uani 1 1 d . . . C2 C 0.59803(7) 0.47703(7) 0.57281(8) 0.0207(4) Uani 1 1 d . . . C3 C 0.64365(7) 0.49133(7) 0.57918(9) 0.0241(4) Uani 1 1 d . . . H3A H 0.6620 0.4985 0.5481 0.029 Uiso 1 1 calc R . . C4 C 0.66353(7) 0.49556(7) 0.62962(9) 0.0260(5) Uani 1 1 d . . . C5 C 0.63534(7) 0.48463(8) 0.67406(9) 0.0265(5) Uani 1 1 d . . . H5A H 0.6477 0.4870 0.7088 0.032 Uiso 1 1 calc R . . C6 C 0.58955(7) 0.47031(7) 0.66939(8) 0.0229(4) Uani 1 1 d . . . C7 C 0.71430(8) 0.51257(9) 0.63337(10) 0.0334(5) Uani 1 1 d . . . C8 C 0.72820(9) 0.50784(10) 0.69026(11) 0.0436(7) Uani 1 1 d . . . H8A H 0.7128 0.4760 0.7004 0.065 Uiso 1 1 calc R . . H8B H 0.7200 0.5245 0.7153 0.065 Uiso 1 1 calc R . . H8C H 0.7608 0.5200 0.6915 0.065 Uiso 1 1 calc R . . C9 C 0.74011(9) 0.56254(10) 0.61744(13) 0.0495(7) Uani 1 1 d . . . H9A H 0.7321 0.5659 0.5807 0.074 Uiso 1 1 calc R . . H9B H 0.7725 0.5738 0.6196 0.074 Uiso 1 1 calc R . . H9C H 0.7321 0.5798 0.6419 0.074 Uiso 1 1 calc R . . C10 C 0.72669(9) 0.48540(11) 0.59490(12) 0.0471(7) Uani 1 1 d . . . H10A H 0.7108 0.4537 0.6056 0.071 Uiso 1 1 calc R . . H10B H 0.7592 0.4971 0.5963 0.071 Uiso 1 1 calc R . . H10C H 0.7180 0.4881 0.5583 0.071 Uiso 1 1 calc R . . C11 C 0.57879(7) 0.47082(7) 0.51703(8) 0.0221(4) Uani 1 1 d . . . H11A H 0.5644 0.4894 0.5127 0.027 Uiso 1 1 calc R . . H11B H 0.6033 0.4810 0.4904 0.027 Uiso 1 1 calc R . . C12 C 0.56452(8) 0.39251(8) 0.51705(9) 0.0256(5) Uani 1 1 d . . . H12A H 0.5971 0.4094 0.5091 0.031 Uiso 1 1 calc R . . H12B H 0.5503 0.3663 0.4927 0.031 Uiso 1 1 calc R . . C13 C 0.55752(7) 0.37633(7) 0.57432(9) 0.0241(4) Uani 1 1 d . . . C14 C 0.58888(8) 0.36995(8) 0.60254(10) 0.0329(5) Uani 1 1 d . . . H14A H 0.6163 0.3760 0.5862 0.039 Uiso 1 1 calc R . . C15 C 0.57914(9) 0.35456(9) 0.65495(11) 0.0415(6) Uani 1 1 d . . . H15A H 0.6002 0.3506 0.6755 0.050 Uiso 1 1 calc R . . C16 C 0.53808(9) 0.34494(8) 0.67707(10) 0.0370(6) Uani 1 1 d . . . H16A H 0.5306 0.3340 0.7127 0.044 Uiso 1 1 calc R . . C17 C 0.50856(8) 0.35154(7) 0.64661(9) 0.0290(5) Uani 1 1 d . . . H17A H 0.4804 0.3445 0.6618 0.035 Uiso 1 1 calc R . . C18 C 0.52842(7) 0.41564(7) 0.45070(8) 0.0235(4) Uani 1 1 d . . . H18A H 0.5506 0.4141 0.4268 0.028 Uiso 1 1 calc R . . H18B H 0.5252 0.4415 0.4393 0.028 Uiso 1 1 calc R . . C19 C 0.48391(7) 0.37299(7) 0.44602(9) 0.0233(4) Uani 1 1 d . . . C20 C 0.46785(8) 0.35065(8) 0.39798(9) 0.0291(5) Uani 1 1 d . . . H20A H 0.4862 0.3603 0.3669 0.035 Uiso 1 1 calc R . . C21 C 0.42474(8) 0.31408(8) 0.39551(10) 0.0319(5) Uani 1 1 d . . . H21A H 0.4130 0.2990 0.3625 0.038 Uiso 1 1 calc R . . C22 C 0.39884(8) 0.29962(8) 0.44171(10) 0.0300(5) Uani 1 1 d . . . H22A H 0.3691 0.2747 0.4408 0.036 Uiso 1 1 calc R . . C23 C 0.41724(7) 0.32225(7) 0.48927(9) 0.0264(5) Uani 1 1 d . . . H23A H 0.4000 0.3119 0.5212 0.032 Uiso 1 1 calc R . . C24 C 0.56048(8) 0.46063(8) 0.71858(9) 0.0255(5) Uani 1 1 d . . . H24A H 0.5344 0.4298 0.7163 0.031 Uiso 1 1 calc R . . H24B H 0.5780 0.4625 0.7509 0.031 Uiso 1 1 calc R . . C25 C 0.58263(7) 0.54067(7) 0.72528(9) 0.0273(5) Uani 1 1 d . . . H25A H 0.6090 0.5409 0.7414 0.033 Uiso 1 1 calc R . . H25B H 0.5745 0.5589 0.7483 0.033 Uiso 1 1 calc R . . C26 C 0.59467(7) 0.56121(7) 0.67026(9) 0.0232(4) Uani 1 1 d . . . C27 C 0.63753(8) 0.59521(8) 0.65677(10) 0.0323(5) Uani 1 1 d . . . H27A H 0.6612 0.6060 0.6823 0.039 Uiso 1 1 calc R . . C28 C 0.64533(8) 0.61302(8) 0.60581(10) 0.0336(6) Uani 1 1 d . . . H28A H 0.6744 0.6364 0.5960 0.040 Uiso 1 1 calc R . . C29 C 0.61042(8) 0.59653(8) 0.56896(10) 0.0296(5) Uani 1 1 d . . . H29A H 0.6152 0.6084 0.5336 0.036 Uiso 1 1 calc R . . C30 C 0.56866(8) 0.56257(7) 0.58477(9) 0.0248(5) Uani 1 1 d . . . H30A H 0.5448 0.5509 0.5596 0.030 Uiso 1 1 calc R . . C31 C 0.51587(8) 0.48395(8) 0.77158(9) 0.0284(5) Uani 1 1 d . . . H31A H 0.5350 0.4941 0.8040 0.034 Uiso 1 1 calc R . . H31B H 0.4949 0.4512 0.7747 0.034 Uiso 1 1 calc R . . C32 C 0.48954(7) 0.50844(7) 0.76715(9) 0.0267(5) Uani 1 1 d . . . C33 C 0.47480(8) 0.52218(8) 0.81100(10) 0.0363(6) Uani 1 1 d . . . H33A H 0.4813 0.5170 0.8464 0.044 Uiso 1 1 calc R . . C34 C 0.45027(9) 0.54370(9) 0.80240(11) 0.0414(7) Uani 1 1 d . . . H34A H 0.4396 0.5531 0.8320 0.050 Uiso 1 1 calc R . . C35 C 0.44148(9) 0.55142(8) 0.75075(12) 0.0408(6) Uani 1 1 d . . . H35A H 0.4252 0.5666 0.7443 0.049 Uiso 1 1 calc R . . C36 C 0.45683(8) 0.53664(8) 0.70840(11) 0.0323(5) Uani 1 1 d . . . H36A H 0.4505 0.5417 0.6728 0.039 Uiso 1 1 calc R . . C37 C 0.39513(9) 0.31905(8) 0.70849(10) 0.0357(6) Uani 1 1 d . . . C38 C 0.42288(10) 0.33392(11) 0.75268(11) 0.0467(7) Uani 1 1 d . . . H38A H 0.4341 0.3635 0.7662 0.056 Uiso 1 1 calc R . . C39 C 0.43393(14) 0.30418(15) 0.77678(15) 0.0737(12) Uani 1 1 d . . . H39A H 0.4535 0.3138 0.8068 0.088 Uiso 1 1 calc R . . C40 C 0.41692(19) 0.26130(17) 0.7578(2) 0.0936(18) Uani 1 1 d . . . H40A H 0.4245 0.2413 0.7748 0.112 Uiso 1 1 calc R . . C41 C 0.38890(18) 0.24723(13) 0.7142(2) 0.0863(15) Uani 1 1 d . . . H41A H 0.3773 0.2175 0.7012 0.104 Uiso 1 1 calc R . . C42 C 0.37717(12) 0.27601(10) 0.68855(14) 0.0590(9) Uani 1 1 d . . . H42A H 0.3576 0.2663 0.6585 0.071 Uiso 1 1 calc R . . C43 C 0.35214(7) 0.38893(7) 0.58458(9) 0.0248(5) Uani 1 1 d . . . C44 C 0.33850(8) 0.41839(8) 0.56599(10) 0.0338(5) Uani 1 1 d . . . H44A H 0.3513 0.4479 0.5801 0.041 Uiso 1 1 calc R . . C45 C 0.30575(9) 0.40373(10) 0.52625(11) 0.0411(6) Uani 1 1 d . . . H45A H 0.2959 0.4233 0.5132 0.049 Uiso 1 1 calc R . . C46 C 0.28753(8) 0.36088(10) 0.50569(11) 0.0403(6) Uani 1 1 d . . . H46A H 0.2653 0.3512 0.4785 0.048 Uiso 1 1 calc R . . C47 C 0.30149(8) 0.33172(9) 0.52454(10) 0.0333(5) Uani 1 1 d . . . H47A H 0.2889 0.3023 0.5101 0.040 Uiso 1 1 calc R . . C48 C 0.33403(7) 0.34563(8) 0.56467(9) 0.0271(5) Uani 1 1 d . . . H48A H 0.3436 0.3259 0.5781 0.033 Uiso 1 1 calc R . . Cl1 Cl 0.45674(2) 0.40798(3) 0.88924(3) 0.04660(18) Uani 0.70 1 d PD A 1 O8 O 0.42796(7) 0.40923(8) 0.84891(9) 0.0643(6) Uani 0.70 1 d PD A 1 O9 O 0.49528(12) 0.41144(15) 0.86111(15) 0.0703(11) Uani 0.70 1 d PD A 1 O10 O 0.43689(14) 0.36920(17) 0.9190(2) 0.102(2) Uani 0.70 1 d PD A 1 O11 O 0.47457(16) 0.44704(17) 0.9220(2) 0.1064(17) Uani 0.70 1 d PD A 1 Cl1A Cl 0.45674(2) 0.40798(3) 0.88924(3) 0.04660(18) Uani 0.30 1 d PD B 2 O8A O 0.42796(7) 0.40923(8) 0.84891(9) 0.0643(6) Uani 0.30 1 d PD B 2 O9A O 0.4986(2) 0.4418(3) 0.8899(4) 0.107(5) Uani 0.30 1 d PD B 2 O10A O 0.4534(4) 0.3639(3) 0.8864(4) 0.093(4) Uani 0.30 1 d PD B 2 O11A O 0.4334(4) 0.4051(4) 0.9389(3) 0.106(4) Uani 0.30 1 d PD B 2 Cl2 Cl 0.47311(2) 0.67801(2) 0.72796(3) 0.04325(17) Uani 1 1 d D . . O12 O 0.45296(10) 0.70540(10) 0.73447(12) 0.0864(8) Uani 1 1 d D . . O13 O 0.51762(8) 0.70538(8) 0.70929(10) 0.0734(7) Uani 1 1 d D . . O14 O 0.47392(10) 0.65920(8) 0.77865(9) 0.0821(8) Uani 1 1 d D . . O15 O 0.44807(8) 0.64270(8) 0.69060(9) 0.0705(7) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.01947(17) 0.01902(17) 0.01616(19) -0.00075(13) 0.00061(13) 0.00939(14) V2 0.02081(17) 0.01859(17) 0.01586(19) -0.00010(13) 0.00018(13) 0.00900(14) P1 0.0218(3) 0.0188(2) 0.0208(3) 0.0017(2) 0.0045(2) 0.0090(2) O1 0.0326(8) 0.0263(8) 0.0195(8) -0.0027(6) -0.0039(6) 0.0159(7) O2 0.0273(8) 0.0261(8) 0.0239(8) 0.0006(6) -0.0006(6) 0.0134(7) O3 0.0195(7) 0.0221(7) 0.0175(8) -0.0020(6) -0.0012(6) 0.0104(6) O4 0.0220(7) 0.0221(7) 0.0243(8) -0.0002(6) 0.0047(6) 0.0100(6) O5 0.0257(8) 0.0223(7) 0.0204(8) 0.0015(6) 0.0036(6) 0.0101(6) O6 0.0279(8) 0.0238(8) 0.0313(9) 0.0069(7) 0.0106(7) 0.0098(7) O7 0.0280(8) 0.0270(8) 0.0303(9) -0.0046(7) -0.0012(7) 0.0159(7) N1 0.0203(8) 0.0228(9) 0.0152(9) -0.0009(7) -0.0011(7) 0.0090(7) N2 0.0299(10) 0.0213(9) 0.0248(10) -0.0009(7) 0.0015(8) 0.0140(8) N3 0.0249(9) 0.0220(9) 0.0207(9) -0.0030(7) 0.0003(7) 0.0126(7) N4 0.0267(9) 0.0236(9) 0.0148(9) 0.0008(7) 0.0024(7) 0.0117(8) N5 0.0234(9) 0.0203(8) 0.0181(9) -0.0006(7) 0.0000(7) 0.0110(7) N6 0.0275(9) 0.0199(9) 0.0258(10) 0.0005(7) 0.0042(8) 0.0101(8) C1 0.0204(10) 0.0190(9) 0.0204(11) -0.0015(8) -0.0027(8) 0.0107(8) C2 0.0215(10) 0.0196(10) 0.0191(11) -0.0016(8) -0.0017(8) 0.0089(8) C3 0.0239(10) 0.0257(10) 0.0219(12) -0.0018(9) -0.0002(9) 0.0119(9) C4 0.0259(11) 0.0289(11) 0.0255(12) -0.0041(9) -0.0043(9) 0.0155(9) C5 0.0286(11) 0.0310(12) 0.0241(12) -0.0026(9) -0.0072(9) 0.0180(10) C6 0.0281(11) 0.0234(10) 0.0198(11) -0.0010(8) -0.0017(9) 0.0149(9) C7 0.0246(11) 0.0451(14) 0.0333(14) -0.0067(11) -0.0065(10) 0.0195(11) C8 0.0340(14) 0.0644(19) 0.0387(16) -0.0100(13) -0.0126(12) 0.0294(14) C9 0.0289(13) 0.0504(17) 0.0582(19) -0.0002(14) -0.0061(13) 0.0115(12) C10 0.0355(14) 0.073(2) 0.0451(17) -0.0126(15) -0.0061(12) 0.0358(15) C11 0.0220(10) 0.0223(10) 0.0192(11) 0.0016(8) 0.0023(8) 0.0089(8) C12 0.0266(11) 0.0296(11) 0.0251(12) -0.0008(9) 0.0020(9) 0.0174(9) C13 0.0277(11) 0.0218(10) 0.0235(12) -0.0017(9) 0.0002(9) 0.0128(9) C14 0.0331(12) 0.0357(13) 0.0367(15) 0.0021(11) -0.0006(10) 0.0224(11) C15 0.0464(15) 0.0422(15) 0.0434(16) 0.0041(12) -0.0100(12) 0.0279(13) C16 0.0547(16) 0.0332(13) 0.0278(14) 0.0064(10) 0.0011(11) 0.0256(12) C17 0.0399(13) 0.0266(11) 0.0247(12) 0.0057(9) 0.0073(10) 0.0199(10) C18 0.0239(10) 0.0289(11) 0.0160(11) -0.0004(8) 0.0001(8) 0.0119(9) C19 0.0264(11) 0.0257(11) 0.0215(11) -0.0032(9) -0.0020(9) 0.0157(9) C20 0.0356(12) 0.0324(12) 0.0192(12) -0.0039(9) -0.0012(9) 0.0170(10) C21 0.0374(13) 0.0315(12) 0.0253(13) -0.0101(10) -0.0080(10) 0.0161(11) C22 0.0287(11) 0.0227(11) 0.0348(14) -0.0058(9) -0.0069(10) 0.0099(9) C23 0.0280(11) 0.0238(11) 0.0274(12) -0.0013(9) 0.0021(9) 0.0129(9) C24 0.0309(11) 0.0299(11) 0.0177(11) 0.0019(9) -0.0024(9) 0.0168(10) C25 0.0265(11) 0.0283(11) 0.0204(12) -0.0057(9) -0.0028(9) 0.0088(9) C26 0.0281(11) 0.0201(10) 0.0200(11) -0.0061(8) -0.0002(9) 0.0109(9) C27 0.0282(12) 0.0270(11) 0.0300(13) -0.0068(10) -0.0014(10) 0.0050(10) C28 0.0301(12) 0.0247(11) 0.0321(14) -0.0011(10) 0.0074(10) 0.0032(10) C29 0.0358(12) 0.0260(11) 0.0265(13) 0.0074(9) 0.0087(10) 0.0150(10) C30 0.0293(11) 0.0239(10) 0.0216(12) 0.0021(9) -0.0003(9) 0.0137(9) C31 0.0349(12) 0.0314(12) 0.0151(11) 0.0013(9) 0.0044(9) 0.0137(10) C32 0.0264(11) 0.0232(10) 0.0229(12) -0.0030(9) 0.0050(9) 0.0068(9) C33 0.0367(13) 0.0343(13) 0.0277(14) -0.0066(10) 0.0067(11) 0.0101(11) C34 0.0412(15) 0.0350(14) 0.0427(17) -0.0113(12) 0.0139(12) 0.0151(12) C35 0.0403(14) 0.0319(13) 0.0534(18) -0.0036(12) 0.0108(12) 0.0204(12) C36 0.0331(12) 0.0259(11) 0.0374(14) -0.0014(10) 0.0035(10) 0.0145(10) C37 0.0435(14) 0.0321(12) 0.0378(15) 0.0156(11) 0.0241(12) 0.0235(11) C38 0.0568(18) 0.0551(17) 0.0391(16) 0.0222(14) 0.0201(14) 0.0362(15) C39 0.082(3) 0.113(3) 0.057(2) 0.049(2) 0.0336(19) 0.072(3) C40 0.145(4) 0.102(3) 0.094(3) 0.070(3) 0.078(3) 0.106(4) C41 0.135(4) 0.050(2) 0.095(3) 0.036(2) 0.068(3) 0.063(3) C42 0.079(2) 0.0341(15) 0.066(2) 0.0133(14) 0.0320(18) 0.0297(16) C43 0.0207(10) 0.0290(11) 0.0229(12) 0.0044(9) 0.0045(8) 0.0111(9) C44 0.0358(13) 0.0320(12) 0.0382(15) 0.0066(11) 0.0057(11) 0.0204(11) C45 0.0372(14) 0.0500(16) 0.0436(16) 0.0122(13) 0.0020(12) 0.0275(13) C46 0.0269(12) 0.0594(17) 0.0304(14) 0.0083(12) 0.0028(10) 0.0184(12) C47 0.0229(11) 0.0354(13) 0.0306(14) -0.0012(10) 0.0052(10) 0.0064(10) C48 0.0248(11) 0.0277(11) 0.0287(13) 0.0036(9) 0.0052(9) 0.0129(9) Cl1 0.0354(3) 0.0579(4) 0.0348(4) 0.0111(3) -0.0018(3) 0.0145(3) O8 0.0494(13) 0.0698(15) 0.0671(15) 0.0125(12) -0.0169(11) 0.0248(12) O9 0.061(2) 0.095(3) 0.061(3) 0.030(2) 0.0134(19) 0.044(2) O10 0.054(2) 0.101(4) 0.091(4) 0.070(3) -0.010(2) -0.007(2) O11 0.074(3) 0.127(4) 0.104(4) -0.056(3) -0.033(3) 0.040(3) Cl1A 0.0354(3) 0.0579(4) 0.0348(4) 0.0111(3) -0.0018(3) 0.0145(3) O8A 0.0494(13) 0.0698(15) 0.0671(15) 0.0125(12) -0.0169(11) 0.0248(12) O9A 0.047(5) 0.109(9) 0.074(8) 0.057(7) -0.022(5) -0.030(6) O10A 0.126(11) 0.086(8) 0.104(9) -0.018(7) -0.044(7) 0.082(8) O11A 0.155(12) 0.099(8) 0.060(6) 0.023(6) 0.057(6) 0.060(9) Cl2 0.0455(4) 0.0397(3) 0.0442(4) -0.0087(3) -0.0079(3) 0.0210(3) O12 0.092(2) 0.0860(19) 0.110(2) -0.0072(17) 0.0001(17) 0.0665(18) O13 0.0513(14) 0.0652(16) 0.0874(18) -0.0057(13) 0.0036(13) 0.0169(12) O14 0.115(2) 0.0610(15) 0.0522(15) -0.0003(12) -0.0232(14) 0.0304(15) O15 0.0729(16) 0.0561(14) 0.0588(15) -0.0179(11) -0.0198(12) 0.0145(12) _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 1.5998(15) . ? V1 O4 2.0062(14) . ? V1 O3 2.0770(14) . ? V1 N3 2.1325(17) . ? V1 N1 2.1385(17) . ? V1 N2 2.3024(18) . ? V2 O2 1.6022(15) . ? V2 O5 2.0326(15) . ? V2 O3 2.0478(14) . ? V2 N5 2.1132(17) . ? V2 N6 2.1323(18) . ? V2 N4 2.2813(18) . ? P1 O5 1.5049(16) . ? P1 O4 1.5080(15) . ? P1 O7 1.5729(16) . ? P1 O6 1.5792(15) . ? O3 C1 1.383(2) . ? O6 C37 1.420(3) . ? O7 C43 1.401(3) . ? N1 C18 1.492(3) . ? N1 C12 1.505(3) . ? N1 C11 1.506(3) . ? N2 C13 1.350(3) . ? N2 C17 1.356(3) . ? N3 C23 1.351(3) . ? N3 C19 1.361(3) . ? N4 C31 1.481(3) . ? N4 C25 1.494(3) . ? N4 C24 1.496(3) . ? N5 C26 1.348(3) . ? N5 C30 1.352(3) . ? N6 C36 1.352(3) . ? N6 C32 1.362(3) . ? C1 C6 1.398(3) . ? C1 C2 1.406(3) . ? C2 C3 1.398(3) . ? C2 C11 1.510(3) . ? C3 C4 1.405(3) . ? C3 H3A 0.950 . ? C4 C5 1.395(3) . ? C4 C7 1.542(3) . ? C5 C6 1.400(3) . ? C5 H5A 0.950 . ? C6 C24 1.511(3) . ? C7 C8 1.532(4) . ? C7 C9 1.540(4) . ? C7 C10 1.541(4) . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? C10 H10A 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 C13 1.509(3) . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C13 C14 1.394(3) . ? C14 C15 1.388(4) . ? C14 H14A 0.950 . ? C15 C16 1.393(4) . ? C15 H15A 0.950 . ? C16 C17 1.375(3) . ? C16 H16A 0.950 . ? C17 H17A 0.950 . ? C18 C19 1.504(3) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 C20 1.381(3) . ? C20 C21 1.385(3) . ? C20 H20A 0.950 . ? C21 C22 1.388(3) . ? C21 H21A 0.950 . ? C22 C23 1.387(3) . ? C22 H22A 0.950 . ? C23 H23A 0.950 . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C25 C26 1.504(3) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 C27 1.389(3) . ? C27 C28 1.379(3) . ? C27 H27A 0.950 . ? C28 C29 1.388(4) . ? C28 H28A 0.950 . ? C29 C30 1.380(3) . ? C29 H29A 0.950 . ? C30 H30A 0.950 . ? C31 C32 1.517(3) . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C32 C33 1.384(3) . ? C33 C34 1.388(4) . ? C33 H33A 0.950 . ? C34 C35 1.380(4) . ? C34 H34A 0.950 . ? C35 C36 1.386(3) . ? C35 H35A 0.950 . ? C36 H36A 0.950 . ? C37 C38 1.378(4) . ? C37 C42 1.380(4) . ? C38 C39 1.393(4) . ? C38 H38A 0.950 . ? C39 C40 1.370(6) . ? C39 H39A 0.950 . ? C40 C41 1.371(7) . ? C40 H40A 0.950 . ? C41 C42 1.396(5) . ? C41 H41A 0.950 . ? C42 H42A 0.950 . ? C43 C48 1.387(3) . ? C43 C44 1.391(3) . ? C44 C45 1.392(4) . ? C44 H44A 0.950 . ? C45 C46 1.379(4) . ? C45 H45A 0.950 . ? C46 C47 1.392(4) . ? C46 H46A 0.950 . ? C47 C48 1.396(3) . ? C47 H47A 0.950 . ? C48 H48A 0.950 . ? Cl1 O10 1.373(3) . ? Cl1 O11 1.422(4) . ? Cl1 O8 1.427(2) . ? Cl1 O9 1.451(3) . ? Cl2 O13 1.416(2) . ? Cl2 O14 1.427(2) . ? Cl2 O15 1.428(2) . ? Cl2 O12 1.430(2) . ? 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 O4 103.13(7) . . ? O1 V1 O3 93.72(7) . . ? O4 V1 O3 94.03(6) . . ? O1 V1 N3 91.62(7) . . ? O4 V1 N3 93.83(6) . . ? O3 V1 N3 169.25(6) . . ? O1 V1 N1 94.55(7) . . ? O4 V1 N1 160.68(6) . . ? O3 V1 N1 92.53(6) . . ? N3 V1 N1 77.73(7) . . ? O1 V1 N2 168.56(7) . . ? O4 V1 N2 87.02(6) . . ? O3 V1 N2 80.13(6) . . ? N3 V1 N2 92.97(7) . . ? N1 V1 N2 76.23(7) . . ? O2 V2 O5 102.35(7) . . ? O2 V2 O3 106.65(7) . . ? O5 V2 O3 87.12(6) . . ? O2 V2 N5 92.66(7) . . ? O5 V2 N5 164.79(7) . . ? O3 V2 N5 86.19(6) . . ? O2 V2 N6 93.36(8) . . ? O5 V2 N6 86.03(6) . . ? O3 V2 N6 159.82(7) . . ? N5 V2 N6 95.67(7) . . ? O2 V2 N4 161.65(7) . . ? O5 V2 N4 90.03(6) . . ? O3 V2 N4 87.25(6) . . ? N5 V2 N4 76.02(7) . . ? N6 V2 N4 73.80(7) . . ? O5 P1 O4 115.38(9) . . ? O5 P1 O7 106.14(8) . . ? O4 P1 O7 112.69(9) . . ? O5 P1 O6 110.87(9) . . ? O4 P1 O6 109.42(9) . . ? O7 P1 O6 101.43(9) . . ? C1 O3 V2 119.93(12) . . ? C1 O3 V1 120.27(12) . . ? V2 O3 V1 118.34(7) . . ? P1 O4 V1 129.80(9) . . ? P1 O5 V2 124.73(9) . . ? C37 O6 P1 121.67(14) . . ? C43 O7 P1 129.81(14) . . ? C18 N1 C12 108.28(16) . . ? C18 N1 C11 110.31(16) . . ? C12 N1 C11 111.12(16) . . ? C18 N1 V1 105.24(12) . . ? C12 N1 V1 114.07(13) . . ? C11 N1 V1 107.65(12) . . ? C13 N2 C17 117.99(19) . . ? C13 N2 V1 113.69(14) . . ? C17 N2 V1 124.19(15) . . ? C23 N3 C19 119.05(18) . . ? C23 N3 V1 127.24(15) . . ? C19 N3 V1 112.46(13) . . ? C31 N4 C25 109.84(17) . . ? C31 N4 C24 110.36(17) . . ? C25 N4 C24 111.15(17) . . ? C31 N4 V2 105.69(13) . . ? C25 N4 V2 109.11(13) . . ? C24 N4 V2 110.54(13) . . ? C26 N5 C30 118.69(19) . . ? C26 N5 V2 120.21(14) . . ? C30 N5 V2 120.10(14) . . ? C36 N6 C32 118.5(2) . . ? C36 N6 V2 123.32(16) . . ? C32 N6 V2 117.89(15) . . ? O3 C1 C6 119.67(18) . . ? O3 C1 C2 120.65(18) . . ? C6 C1 C2 119.68(19) . . ? C3 C2 C1 118.97(19) . . ? C3 C2 C11 119.30(18) . . ? C1 C2 C11 121.65(18) . . ? C2 C3 C4 122.7(2) . . ? C2 C3 H3A 118.7 . . ? C4 C3 H3A 118.7 . . ? C5 C4 C3 116.6(2) . . ? C5 C4 C7 123.8(2) . . ? C3 C4 C7 119.6(2) . . ? C4 C5 C6 122.4(2) . . ? C4 C5 H5A 118.8 . . ? C6 C5 H5A 118.8 . . ? C1 C6 C5 119.6(2) . . ? C1 C6 C24 119.46(19) . . ? C5 C6 C24 120.89(19) . . ? C8 C7 C9 108.7(2) . . ? C8 C7 C10 108.5(2) . . ? C9 C7 C10 109.6(2) . . ? C8 C7 C4 111.7(2) . . ? C9 C7 C4 108.6(2) . . ? C10 C7 C4 109.6(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C2 110.49(16) . . ? N1 C11 H11A 109.6 . . ? C2 C11 H11A 109.6 . . ? N1 C11 H11B 109.6 . . ? C2 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? N1 C12 C13 111.23(17) . . ? N1 C12 H12A 109.4 . . ? C13 C12 H12A 109.4 . . ? N1 C12 H12B 109.4 . . ? C13 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? N2 C13 C14 122.5(2) . . ? N2 C13 C12 114.54(19) . . ? C14 C13 C12 122.9(2) . . ? C15 C14 C13 118.6(2) . . ? C15 C14 H14A 120.7 . . ? C13 C14 H14A 120.7 . . ? C14 C15 C16 119.1(2) . . ? C14 C15 H15A 120.4 . . ? C16 C15 H15A 120.4 . . ? C17 C16 C15 119.1(2) . . ? C17 C16 H16A 120.5 . . ? C15 C16 H16A 120.5 . . ? N2 C17 C16 122.7(2) . . ? N2 C17 H17A 118.7 . . ? C16 C17 H17A 118.7 . . ? N1 C18 C19 110.04(17) . . ? N1 C18 H18A 109.7 . . ? C19 C18 H18A 109.7 . . ? N1 C18 H18B 109.7 . . ? C19 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? N3 C19 C20 121.2(2) . . ? N3 C19 C18 116.09(18) . . ? C20 C19 C18 122.6(2) . . ? C19 C20 C21 119.5(2) . . ? C19 C20 H20A 120.3 . . ? C21 C20 H20A 120.3 . . ? C20 C21 C22 119.5(2) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? C23 C22 C21 118.6(2) . . ? C23 C22 H22A 120.7 . . ? C21 C22 H22A 120.7 . . ? N3 C23 C22 122.0(2) . . ? N3 C23 H23A 119.0 . . ? C22 C23 H23A 119.0 . . ? N4 C24 C6 110.63(17) . . ? N4 C24 H24A 109.5 . . ? C6 C24 H24A 109.5 . . ? N4 C24 H24B 109.5 . . ? C6 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? N4 C25 C26 111.35(17) . . ? N4 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? N4 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? N5 C26 C27 121.7(2) . . ? N5 C26 C25 115.35(19) . . ? C27 C26 C25 122.9(2) . . ? C28 C27 C26 119.1(2) . . ? C28 C27 H27A 120.4 . . ? C26 C27 H27A 120.4 . . ? C27 C28 C29 119.6(2) . . ? C27 C28 H28A 120.2 . . ? C29 C28 H28A 120.2 . . ? C30 C29 C28 118.5(2) . . ? C30 C29 H29A 120.7 . . ? C28 C29 H29A 120.7 . . ? N5 C30 C29 122.4(2) . . ? N5 C30 H30A 118.8 . . ? C29 C30 H30A 118.8 . . ? N4 C31 C32 109.02(18) . . ? N4 C31 H31A 109.9 . . ? C32 C31 H31A 109.9 . . ? N4 C31 H31B 109.9 . . ? C32 C31 H31B 109.9 . . ? H31A C31 H31B 108.3 . . ? N6 C32 C33 121.8(2) . . ? N6 C32 C31 114.61(19) . . ? C33 C32 C31 123.6(2) . . ? C32 C33 C34 118.9(2) . . ? C32 C33 H33A 120.6 . . ? C34 C33 H33A 120.6 . . ? C35 C34 C33 119.8(2) . . ? C35 C34 H34A 120.1 . . ? C33 C34 H34A 120.1 . . ? C34 C35 C36 118.8(2) . . ? C34 C35 H35A 120.6 . . ? C36 C35 H35A 120.6 . . ? N6 C36 C35 122.2(2) . . ? N6 C36 H36A 118.9 . . ? C35 C36 H36A 118.9 . . ? C38 C37 C42 122.8(3) . . ? C38 C37 O6 119.6(2) . . ? C42 C37 O6 117.5(3) . . ? C37 C38 C39 117.7(3) . . ? C37 C38 H38A 121.1 . . ? C39 C38 H38A 121.1 . . ? C40 C39 C38 120.9(4) . . ? C40 C39 H39A 119.5 . . ? C38 C39 H39A 119.5 . . ? C39 C40 C41 120.0(3) . . ? C39 C40 H40A 120.0 . . ? C41 C40 H40A 120.0 . . ? C40 C41 C42 121.0(4) . . ? C40 C41 H41A 119.5 . . ? C42 C41 H41A 119.5 . . ? C37 C42 C41 117.5(4) . . ? C37 C42 H42A 121.3 . . ? C41 C42 H42A 121.3 . . ? C48 C43 C44 121.9(2) . . ? C48 C43 O7 123.4(2) . . ? C44 C43 O7 114.7(2) . . ? C43 C44 C45 118.7(2) . . ? C43 C44 H44A 120.7 . . ? C45 C44 H44A 120.7 . . ? C46 C45 C44 120.3(2) . . ? C46 C45 H45A 119.8 . . ? C44 C45 H45A 119.8 . . ? C45 C46 C47 120.5(2) . . ? C45 C46 H46A 119.8 . . ? C47 C46 H46A 119.8 . . ? C46 C47 C48 120.1(2) . . ? C46 C47 H47A 119.9 . . ? C48 C47 H47A 119.9 . . ? C43 C48 C47 118.5(2) . . ? C43 C48 H48A 120.7 . . ? C47 C48 H48A 120.7 . . ? O10 Cl1 O11 112.1(3) . . ? O10 Cl1 O8 113.3(2) . . ? O11 Cl1 O8 110.8(2) . . ? O10 Cl1 O9 109.4(3) . . ? O11 Cl1 O9 104.8(3) . . ? O8 Cl1 O9 105.93(18) . . ? O13 Cl2 O14 109.48(17) . . ? O13 Cl2 O15 109.99(15) . . ? O14 Cl2 O15 109.50(15) . . ? O13 Cl2 O12 108.55(17) . . ? O14 Cl2 O12 108.84(17) . . ? O15 Cl2 O12 110.44(17) . . ? 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 O2 V2 O3 C1 127.86(14) . . . . ? O5 V2 O3 C1 -130.11(14) . . . . ? N5 V2 O3 C1 36.22(14) . . . . ? N6 V2 O3 C1 -59.9(2) . . . . ? N4 V2 O3 C1 -39.94(14) . . . . ? O2 V2 O3 V1 -38.42(9) . . . . ? O5 V2 O3 V1 63.61(8) . . . . ? N5 V2 O3 V1 -130.06(8) . . . . ? N6 V2 O3 V1 133.86(17) . . . . ? N4 V2 O3 V1 153.77(8) . . . . ? O1 V1 O3 C1 -116.87(14) . . . . ? O4 V1 O3 C1 139.67(14) . . . . ? N3 V1 O3 C1 2.7(4) . . . . ? N1 V1 O3 C1 -22.14(14) . . . . ? N2 V1 O3 C1 53.41(14) . . . . ? O1 V1 O3 V2 49.37(9) . . . . ? O4 V1 O3 V2 -54.09(8) . . . . ? N3 V1 O3 V2 169.0(3) . . . . ? N1 V1 O3 V2 144.10(8) . . . . ? N2 V1 O3 V2 -140.35(9) . . . . ? O5 P1 O4 V1 -38.48(15) . . . . ? O7 P1 O4 V1 83.65(13) . . . . ? O6 P1 O4 V1 -164.31(11) . . . . ? O1 V1 O4 P1 -59.28(13) . . . . ? O3 V1 O4 P1 35.50(12) . . . . ? N3 V1 O4 P1 -151.84(12) . . . . ? N1 V1 O4 P1 145.06(16) . . . . ? N2 V1 O4 P1 115.38(12) . . . . ? O4 P1 O5 V2 58.19(13) . . . . ? O7 P1 O5 V2 -67.38(12) . . . . ? O6 P1 O5 V2 -176.72(9) . . . . ? O2 V2 O5 P1 40.14(12) . . . . ? O3 V2 O5 P1 -66.28(11) . . . . ? N5 V2 O5 P1 -130.3(2) . . . . ? N6 V2 O5 P1 132.71(11) . . . . ? N4 V2 O5 P1 -153.53(11) . . . . ? O5 P1 O6 C37 -72.87(19) . . . . ? O4 P1 O6 C37 55.5(2) . . . . ? O7 P1 O6 C37 174.75(18) . . . . ? O5 P1 O7 C43 166.38(17) . . . . ? O4 P1 O7 C43 39.2(2) . . . . ? O6 P1 O7 C43 -77.72(19) . . . . ? O1 V1 N1 C18 -54.09(13) . . . . ? O4 V1 N1 C18 102.2(2) . . . . ? O3 V1 N1 C18 -148.03(13) . . . . ? N3 V1 N1 C18 36.58(12) . . . . ? N2 V1 N1 C18 132.77(13) . . . . ? O1 V1 N1 C12 -172.63(14) . . . . ? O4 V1 N1 C12 -16.4(3) . . . . ? O3 V1 N1 C12 93.44(14) . . . . ? N3 V1 N1 C12 -81.96(14) . . . . ? N2 V1 N1 C12 14.24(13) . . . . ? O1 V1 N1 C11 63.57(13) . . . . ? O4 V1 N1 C11 -140.18(18) . . . . ? O3 V1 N1 C11 -30.37(13) . . . . ? N3 V1 N1 C11 154.24(13) . . . . ? N2 V1 N1 C11 -109.57(13) . . . . ? O1 V1 N2 C13 -31.5(4) . . . . ? O4 V1 N2 C13 175.70(15) . . . . ? O3 V1 N2 C13 -89.68(15) . . . . ? N3 V1 N2 C13 82.01(15) . . . . ? N1 V1 N2 C13 5.41(14) . . . . ? O1 V1 N2 C17 125.1(4) . . . . ? O4 V1 N2 C17 -27.71(18) . . . . ? O3 V1 N2 C17 66.91(18) . . . . ? N3 V1 N2 C17 -121.40(18) . . . . ? N1 V1 N2 C17 162.01(19) . . . . ? O1 V1 N3 C23 -97.87(18) . . . . ? O4 V1 N3 C23 5.41(18) . . . . ? O3 V1 N3 C23 142.3(3) . . . . ? N1 V1 N3 C23 167.83(19) . . . . ? N2 V1 N3 C23 92.61(18) . . . . ? O1 V1 N3 C19 69.11(15) . . . . ? O4 V1 N3 C19 172.39(14) . . . . ? O3 V1 N3 C19 -50.7(4) . . . . ? N1 V1 N3 C19 -25.19(14) . . . . ? N2 V1 N3 C19 -100.41(14) . . . . ? O2 V2 N4 C31 83.4(3) . . . . ? O5 V2 N4 C31 -49.50(13) . . . . ? O3 V2 N4 C31 -136.61(13) . . . . ? N5 V2 N4 C31 136.63(14) . . . . ? N6 V2 N4 C31 36.36(13) . . . . ? O2 V2 N4 C25 -34.7(3) . . . . ? O5 V2 N4 C25 -167.57(13) . . . . ? O3 V2 N4 C25 105.32(13) . . . . ? N5 V2 N4 C25 18.56(13) . . . . ? N6 V2 N4 C25 -81.70(14) . . . . ? O2 V2 N4 C24 -157.2(2) . . . . ? O5 V2 N4 C24 69.91(13) . . . . ? O3 V2 N4 C24 -17.20(13) . . . . ? N5 V2 N4 C24 -103.96(14) . . . . ? N6 V2 N4 C24 155.77(14) . . . . ? O2 V2 N5 C26 161.51(16) . . . . ? O5 V2 N5 C26 -27.9(3) . . . . ? O3 V2 N5 C26 -91.98(16) . . . . ? N6 V2 N5 C26 67.86(16) . . . . ? N4 V2 N5 C26 -3.87(15) . . . . ? O2 V2 N5 C30 -30.01(16) . . . . ? O5 V2 N5 C30 140.6(2) . . . . ? O3 V2 N5 C30 76.51(16) . . . . ? N6 V2 N5 C30 -123.65(16) . . . . ? N4 V2 N5 C30 164.62(17) . . . . ? O2 V2 N6 C36 -4.23(18) . . . . ? O5 V2 N6 C36 -106.39(18) . . . . ? O3 V2 N6 C36 -176.83(17) . . . . ? N5 V2 N6 C36 88.78(18) . . . . ? N4 V2 N6 C36 162.43(19) . . . . ? O2 V2 N6 C32 169.86(16) . . . . ? O5 V2 N6 C32 67.70(15) . . . . ? O3 V2 N6 C32 -2.7(3) . . . . ? N5 V2 N6 C32 -97.13(16) . . . . ? N4 V2 N6 C32 -23.48(15) . . . . ? V2 O3 C1 C6 57.1(2) . . . . ? V1 O3 C1 C6 -136.84(16) . . . . ? V2 O3 C1 C2 -123.41(17) . . . . ? V1 O3 C1 C2 42.6(2) . . . . ? O3 C1 C2 C3 -179.94(18) . . . . ? C6 C1 C2 C3 -0.5(3) . . . . ? O3 C1 C2 C11 -3.3(3) . . . . ? C6 C1 C2 C11 176.19(19) . . . . ? C1 C2 C3 C4 0.3(3) . . . . ? C11 C2 C3 C4 -176.5(2) . . . . ? C2 C3 C4 C5 0.1(3) . . . . ? C2 C3 C4 C7 -178.6(2) . . . . ? C3 C4 C5 C6 -0.3(3) . . . . ? C7 C4 C5 C6 178.4(2) . . . . ? O3 C1 C6 C5 179.77(18) . . . . ? C2 C1 C6 C5 0.3(3) . . . . ? O3 C1 C6 C24 -2.7(3) . . . . ? C2 C1 C6 C24 177.83(19) . . . . ? C4 C5 C6 C1 0.1(3) . . . . ? C4 C5 C6 C24 -177.4(2) . . . . ? C5 C4 C7 C8 10.4(3) . . . . ? C3 C4 C7 C8 -171.0(2) . . . . ? C5 C4 C7 C9 -109.6(3) . . . . ? C3 C4 C7 C9 69.1(3) . . . . ? C5 C4 C7 C10 130.7(2) . . . . ? C3 C4 C7 C10 -50.6(3) . . . . ? C18 N1 C11 C2 -175.53(17) . . . . ? C12 N1 C11 C2 -55.4(2) . . . . ? V1 N1 C11 C2 70.15(17) . . . . ? C3 C2 C11 N1 115.5(2) . . . . ? C1 C2 C11 N1 -61.2(2) . . . . ? C18 N1 C12 C13 -147.61(18) . . . . ? C11 N1 C12 C13 91.1(2) . . . . ? V1 N1 C12 C13 -30.8(2) . . . . ? C17 N2 C13 C14 -1.0(3) . . . . ? V1 N2 C13 C14 157.14(18) . . . . ? C17 N2 C13 C12 177.82(19) . . . . ? V1 N2 C13 C12 -24.0(2) . . . . ? N1 C12 C13 N2 36.2(3) . . . . ? N1 C12 C13 C14 -145.0(2) . . . . ? N2 C13 C14 C15 -0.7(3) . . . . ? C12 C13 C14 C15 -179.4(2) . . . . ? C13 C14 C15 C16 1.6(4) . . . . ? C14 C15 C16 C17 -0.9(4) . . . . ? C13 N2 C17 C16 1.8(3) . . . . ? V1 N2 C17 C16 -153.85(19) . . . . ? C15 C16 C17 N2 -0.9(4) . . . . ? C12 N1 C18 C19 79.0(2) . . . . ? C11 N1 C18 C19 -159.25(17) . . . . ? V1 N1 C18 C19 -43.40(18) . . . . ? C23 N3 C19 C20 -1.2(3) . . . . ? V1 N3 C19 C20 -169.38(17) . . . . ? C23 N3 C19 C18 175.47(19) . . . . ? V1 N3 C19 C18 7.3(2) . . . . ? N1 C18 C19 N3 25.0(2) . . . . ? N1 C18 C19 C20 -158.3(2) . . . . ? N3 C19 C20 C21 2.8(3) . . . . ? C18 C19 C20 C21 -173.7(2) . . . . ? C19 C20 C21 C22 -1.9(4) . . . . ? C20 C21 C22 C23 -0.5(3) . . . . ? C19 N3 C23 C22 -1.3(3) . . . . ? V1 N3 C23 C22 164.94(17) . . . . ? C21 C22 C23 N3 2.1(3) . . . . ? C31 N4 C24 C6 -179.83(17) . . . . ? C25 N4 C24 C6 -57.7(2) . . . . ? V2 N4 C24 C6 63.62(19) . . . . ? C1 C6 C24 N4 -63.5(3) . . . . ? C5 C6 C24 N4 114.0(2) . . . . ? C31 N4 C25 C26 -145.33(19) . . . . ? C24 N4 C25 C26 92.2(2) . . . . ? V2 N4 C25 C26 -29.9(2) . . . . ? C30 N5 C26 C27 0.9(3) . . . . ? V2 N5 C26 C27 169.50(16) . . . . ? C30 N5 C26 C25 179.08(19) . . . . ? V2 N5 C26 C25 -12.3(2) . . . . ? N4 C25 C26 N5 28.7(3) . . . . ? N4 C25 C26 C27 -153.1(2) . . . . ? N5 C26 C27 C28 -0.1(3) . . . . ? C25 C26 C27 C28 -178.2(2) . . . . ? C26 C27 C28 C29 -0.4(4) . . . . ? C27 C28 C29 C30 0.1(4) . . . . ? C26 N5 C30 C29 -1.2(3) . . . . ? V2 N5 C30 C29 -169.86(17) . . . . ? C28 C29 C30 N5 0.7(3) . . . . ? C25 N4 C31 C32 72.9(2) . . . . ? C24 N4 C31 C32 -164.17(18) . . . . ? V2 N4 C31 C32 -44.64(19) . . . . ? C36 N6 C32 C33 0.7(3) . . . . ? V2 N6 C32 C33 -173.65(17) . . . . ? C36 N6 C32 C31 179.5(2) . . . . ? V2 N6 C32 C31 5.1(2) . . . . ? N4 C31 C32 N6 28.5(3) . . . . ? N4 C31 C32 C33 -152.8(2) . . . . ? N6 C32 C33 C34 -0.3(3) . . . . ? C31 C32 C33 C34 -178.9(2) . . . . ? C32 C33 C34 C35 -0.7(4) . . . . ? C33 C34 C35 C36 1.1(4) . . . . ? C32 N6 C36 C35 -0.3(3) . . . . ? V2 N6 C36 C35 173.79(18) . . . . ? C34 C35 C36 N6 -0.7(4) . . . . ? P1 O6 C37 C38 74.6(3) . . . . ? P1 O6 C37 C42 -108.6(2) . . . . ? C42 C37 C38 C39 1.9(4) . . . . ? O6 C37 C38 C39 178.5(2) . . . . ? C37 C38 C39 C40 -1.4(5) . . . . ? C38 C39 C40 C41 0.6(5) . . . . ? C39 C40 C41 C42 -0.1(6) . . . . ? C38 C37 C42 C41 -1.5(4) . . . . ? O6 C37 C42 C41 -178.2(3) . . . . ? C40 C41 C42 C37 0.6(5) . . . . ? P1 O7 C43 C48 17.4(3) . . . . ? P1 O7 C43 C44 -164.21(17) . . . . ? C48 C43 C44 C45 -0.1(3) . . . . ? O7 C43 C44 C45 -178.4(2) . . . . ? C43 C44 C45 C46 -0.4(4) . . . . ? C44 C45 C46 C47 0.3(4) . . . . ? C45 C46 C47 C48 0.2(4) . . . . ? C44 C43 C48 C47 0.6(3) . . . . ? O7 C43 C48 C47 178.79(19) . . . . ? C46 C47 C48 C43 -0.6(3) . . . . ? # SQUEEZE RESULTS loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 -0.010 1172.9 505.6 2 0.333 0.667 0.169 1166.8 505.3 3 0.667 0.333 0.836 1166.8 505.3 _platon_squeeze_details ; The SQUEEZE procedure accounts for poorly resolved solvent molecules lying in channels along the c axis. It is possible to model several MeOH molecules using conventional refinement, but the best wR2 is ca 25% and the su's on the bond distances and angles of the main complexes are ca 2 times as large. The total of ca 1500 electrons per unit cell amounts to ca 84 MeOH molecule per cell, which corresponds to ca 4.5 per V complex. ;