# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_publication_text data_p-1 #TrackingRef '18393_web_deposit_cif_file_0_CarstenStreb_1362733185.CS1161_Hugo.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H92 Ba2 N11 O57 V15' _chemical_melting_point ? _exptl_crystal_description plate _exptl_crystal_colour orange _diffrn_ambient_temperature 150(2) _chemical_formula_weight 2858.1 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' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 '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_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.240(2) _cell_length_b 13.285(3) _cell_length_c 33.139(7) _cell_angle_alpha 98.09(3) _cell_angle_beta 91.58(3) _cell_angle_gamma 106.32(3) _cell_volume 5107.2(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 241 _cell_measurement_theta_min 4.7 _cell_measurement_theta_max 22.8 _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.858 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2823 _exptl_absorpt_coefficient_mu 2.156 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.712 _exptl_absorpt_correction_T_max 0.891 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa Nonius CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 116359 _diffrn_reflns_av_R_equivalents 0.1241 _diffrn_reflns_av_sigmaI/netI 0.0907 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 5.82 _diffrn_reflns_theta_max 26.50 _reflns_number_total 20942 _reflns_number_gt 14582 _reflns_threshold_expression >2\s(I) _computing_data_collection SUPERGUI _computing_cell_refinement SUPERGUI _computing_data_reduction SUPERGUI _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0657P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20942 _refine_ls_number_parameters 1343 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1411 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V3 V 0.44277(8) 0.36353(7) 0.28332(3) 0.0186(2) Uani 1 1 d . . . V1 V 0.63911(8) 0.60022(7) 0.29231(3) 0.0188(2) Uani 1 1 d . . . V6 V 0.60265(8) 0.77664(7) 0.35882(3) 0.0192(2) Uani 1 1 d . . . V2 V 0.42057(7) 0.55065(7) 0.34867(3) 0.0152(2) Uani 1 1 d . . . V5 V 0.35867(8) 0.74083(7) 0.32157(3) 0.0217(2) Uani 1 1 d . . . V8 V 0.50140(8) 0.36770(7) 0.37522(3) 0.0213(2) Uani 1 1 d . . . V7 V 0.67132(8) 0.59312(7) 0.38588(3) 0.0189(2) Uani 1 1 d . . . V10 V 0.56130(9) 0.78404(8) 0.26730(3) 0.0253(2) Uani 1 1 d . . . V4 V 0.36890(8) 0.55188(7) 0.25644(3) 0.0186(2) Uani 1 1 d . . . V9 V 0.70453(8) 0.41454(7) 0.32108(3) 0.0235(2) Uani 1 1 d . . . O6 O 0.3216(3) 0.6175(3) 0.35344(11) 0.0204(8) Uani 1 1 d . . . O3 O 0.3529(3) 0.4603(3) 0.29711(11) 0.0171(8) Uani 1 1 d . . . O19 O 0.7511(3) 0.6752(3) 0.42257(12) 0.0234(9) Uani 1 1 d . . . O25 O 0.6833(3) 0.8547(3) 0.39659(12) 0.0214(9) Uani 1 1 d . . . O8 O 0.7011(3) 0.6835(3) 0.34116(11) 0.0181(8) Uani 1 1 d . . . O11 O 0.3862(3) 0.4534(3) 0.37771(11) 0.0183(8) Uani 1 1 d . . . O9 O 0.5382(3) 0.6486(3) 0.38438(11) 0.0159(8) Uani 1 1 d . . . O10 O 0.5939(3) 0.4844(3) 0.41004(11) 0.0208(8) Uani 1 1 d . . . O15 O 0.5884(3) 0.3336(3) 0.27597(12) 0.0259(9) Uani 1 1 d . . . O16 O 0.7674(3) 0.5206(3) 0.36256(12) 0.0226(9) Uani 1 1 d . . . O14 O 0.7313(3) 0.5272(3) 0.28403(12) 0.0253(9) Uani 1 1 d . . . O26 O 0.2567(3) 0.7920(3) 0.33214(13) 0.0309(10) Uani 1 1 d . . . O5 O 0.2824(3) 0.6251(3) 0.27650(11) 0.0216(9) Uani 1 1 d . . . O27 O 0.2970(3) 0.4709(3) 0.21768(12) 0.0250(9) Uani 1 1 d . . . O20 O 0.6428(3) 0.8463(3) 0.31557(12) 0.0235(9) Uani 1 1 d . . . O28 O 0.3672(3) 0.2878(3) 0.24416(12) 0.0252(9) Uani 1 1 d . . . O4 O 0.5141(3) 0.4937(3) 0.25170(12) 0.0219(9) Uani 1 1 d . . . O1 O 0.4961(3) 0.6504(3) 0.30664(11) 0.0181(8) Uani 1 1 d . . . O2 O 0.5576(3) 0.4911(3) 0.32927(11) 0.0161(8) Uani 1 1 d . . . O13 O 0.6216(3) 0.3294(3) 0.35498(12) 0.0252(9) Uani 1 1 d . . . O22 O 0.4610(3) 0.6623(3) 0.22764(12) 0.0259(9) Uani 1 1 d . . . O12 O 0.4082(3) 0.2968(3) 0.32394(12) 0.0225(9) Uani 1 1 d . . . O18 O 0.4519(4) 0.2854(3) 0.40530(13) 0.0325(10) Uani 1 1 d . . . O23 O 0.4328(3) 0.8152(3) 0.28359(12) 0.0261(9) Uani 1 1 d . . . O7 O 0.4682(3) 0.8087(3) 0.36235(12) 0.0220(9) Uani 1 1 d . . . O21 O 0.6681(3) 0.6913(3) 0.26041(12) 0.0257(9) Uani 1 1 d . . . O24 O 0.6102(4) 0.8659(3) 0.23679(14) 0.0398(12) Uani 1 1 d . . . O17 O 0.8059(3) 0.3641(3) 0.30942(14) 0.0359(11) Uani 1 1 d . . . V11 V 0.09823(8) 0.93761(8) -0.00416(3) 0.0214(2) Uani 1 1 d . . . V13 V 0.14954(9) 1.19339(8) 0.03453(3) 0.0272(2) Uani 1 1 d . . . V12 V 0.00827(8) 1.02122(8) 0.08413(3) 0.0217(2) Uani 1 1 d . . . V15 V -0.23588(9) 0.88392(8) 0.04928(3) 0.0278(2) Uani 1 1 d . . . V14 V -0.04361(10) 0.77590(8) 0.04601(3) 0.0290(3) Uani 1 1 d . . . O41 O 0.0738(4) 1.0954(3) 0.12538(12) 0.0302(10) Uani 1 1 d . . . O34 O 0.2133(4) 1.2609(3) 0.07713(13) 0.0387(11) Uani 1 1 d . . . O30 O 0.1518(3) 1.0445(3) 0.04771(11) 0.0233(9) Uani 1 1 d . . . O32 O 0.2730(3) 1.1873(3) 0.00341(13) 0.0324(10) Uani 1 1 d . . . O35 O 0.0367(3) 0.8888(3) 0.08896(12) 0.0279(9) Uani 1 1 d . . . O31 O -0.0031(3) 1.1301(3) 0.05181(11) 0.0210(8) Uani 1 1 d . . . O33 O 0.1065(4) 1.2820(3) 0.00812(12) 0.0310(10) Uani 1 1 d . . . O38 O -0.1324(3) 0.9828(3) 0.09330(12) 0.0267(9) Uani 1 1 d . . . O29 O -0.0548(3) 0.9272(3) 0.02125(11) 0.0205(8) Uani 1 1 d . . . O42 O 0.2230(3) 0.9820(3) -0.02637(12) 0.0257(9) Uani 1 1 d . . . O36 O 0.1061(4) 0.8321(3) 0.01583(12) 0.0272(9) Uani 1 1 d . . . O40 O -0.0169(4) 0.6777(3) 0.06210(14) 0.0434(12) Uani 1 1 d . . . O37 O -0.1779(4) 0.7769(3) 0.06400(12) 0.0312(10) Uani 1 1 d . . . O39 O -0.3559(4) 0.8647(4) 0.06905(14) 0.0402(12) Uani 1 1 d . . . O52 O 0.5798(4) 0.5574(4) 0.17365(16) 0.0512(14) Uani 1 1 d . . . N10 N 0.7747(11) 0.6060(12) 0.1708(3) 0.030(2) Uani 0.60 1 d P A 1 C50 C 0.8237(8) 0.7858(8) 0.1652(3) 0.033(2) Uani 0.60 1 d PU A 1 H50A H 0.8574 0.8327 0.1461 0.039 Uiso 0.60 1 calc PR A 1 H50B H 0.8403 0.8246 0.1928 0.039 Uiso 0.60 1 calc PR A 1 C46 C 0.6733(14) 0.6246(18) 0.1670(5) 0.030(3) Uani 0.60 1 d P A 1 C50A C 0.875(3) 0.563(3) 0.1625(11) 0.113(11) Uani 0.40 1 d PU A 2 N10A N 0.740(3) 0.6571(16) 0.1606(7) 0.063(6) Uani 0.40 1 d P A 2 C46A C 0.685(3) 0.573(2) 0.1717(7) 0.050(8) Uani 0.40 1 d P A 2 C49 C 0.7776(8) 0.5054(7) 0.1797(3) 0.061(2) Uani 1 1 d . . . H49A H 0.8553 0.5032 0.1816 0.092 Uiso 1 1 calc R A 1 H49B H 0.7349 0.4508 0.1583 0.092 Uiso 1 1 calc R A 1 H49C H 0.7446 0.4941 0.2052 0.092 Uiso 1 1 calc R A 1 C51 C 0.6917(7) 0.7364(6) 0.1550(3) 0.051(2) Uani 1 1 d . . . H51A H 0.6485 0.7763 0.1712 0.061 Uiso 1 1 calc R A 1 H51B H 0.6711 0.7324 0.1262 0.061 Uiso 1 1 calc R A 1 C47 C 0.8663(6) 0.6862(6) 0.1607(3) 0.052(2) Uani 1 1 d . . . H47A H 0.8856 0.6686 0.1330 0.063 Uiso 1 1 calc R A 1 H47B H 0.9329 0.6973 0.1792 0.063 Uiso 1 1 calc R A 1 O53 O 0.0881(3) 0.0140(3) 0.46608(12) 0.0221(9) Uani 1 1 d . . . O43 O 1.0956(6) 0.3741(5) 0.14164(17) 0.075(2) Uani 1 1 d . . . N1 N 1.0212(8) 0.4167(8) 0.0877(3) 0.085(3) Uani 1 1 d . . . C4 C 0.8936(9) 0.2836(8) 0.1185(4) 0.095(4) Uani 1 1 d . . . H4A H 0.8601 0.2987 0.1440 0.114 Uiso 1 1 calc R . . H4B H 0.8954 0.2103 0.1143 0.114 Uiso 1 1 calc R . . C1 C 1.0143(11) 0.3631(9) 0.1164(3) 0.080(4) Uani 1 1 d . . . C5 C 1.1175(9) 0.4885(7) 0.0773(3) 0.071(3) Uani 1 1 d . . . H5A H 1.0983 0.5185 0.0544 0.107 Uiso 1 1 calc R . . H5B H 1.1742 0.4529 0.0703 0.107 Uiso 1 1 calc R . . H5C H 1.1470 0.5439 0.1001 0.107 Uiso 1 1 calc R . . C3 C 0.8290(12) 0.3115(12) 0.0801(4) 0.107(4) Uani 1 1 d . . . H3A H 0.7956 0.2477 0.0606 0.129 Uiso 1 1 calc R . . H3B H 0.7684 0.3409 0.0895 0.129 Uiso 1 1 calc R . . C2 C 0.9134(10) 0.3898(9) 0.0605(3) 0.082(4) Uani 1 1 d . . . H2A H 0.8887 0.4525 0.0590 0.099 Uiso 1 1 calc R . . H2B H 0.9246 0.3592 0.0332 0.099 Uiso 1 1 calc R . . O44 O 0.3206(3) 0.1459(3) 0.50619(13) 0.0320(10) Uani 1 1 d . . . N2 N 0.4508(4) 0.3083(4) 0.51040(16) 0.0293(12) Uani 1 1 d . . . C9 C 0.5184(5) 0.1764(5) 0.5309(2) 0.0325(15) Uani 1 1 d . . . H9A H 0.5373 0.1235 0.5112 0.039 Uiso 1 1 calc R F . H9B H 0.5012 0.1477 0.5561 0.039 Uiso 1 1 calc R . . C6 C 0.4188(5) 0.2077(5) 0.51437(19) 0.0284(14) Uani 1 1 d . . . C10 C 0.3763(6) 0.3642(5) 0.4949(2) 0.0372(16) Uani 1 1 d . . . C8 C 0.6164(5) 0.2784(5) 0.5385(2) 0.0351(16) Uani 1 1 d . F . H8A H 0.6822 0.2691 0.5245 0.042 Uiso 1 1 calc R . . H8B H 0.6381 0.2994 0.5675 0.042 Uiso 1 1 calc R . . C7 C 0.5722(5) 0.3617(5) 0.5218(2) 0.0351(16) Uani 1 1 d . F . H7A H 0.5817 0.4236 0.5424 0.042 Uiso 1 1 calc R . . H7B H 0.6121 0.3837 0.4982 0.042 Uiso 1 1 calc R . . O45 O 0.0966(4) 0.2362(3) 0.21876(13) 0.0337(10) Uani 1 1 d . . . N3 N 0.0691(4) 0.3627(4) 0.26791(15) 0.0274(12) Uani 1 1 d . . . C11 C 0.0950(5) 0.2742(5) 0.2553(2) 0.0286(14) Uani 1 1 d . . . C14 C 0.1178(5) 0.2244(5) 0.29148(19) 0.0314(15) Uani 1 1 d . . . H14A H 0.1909 0.2093 0.2903 0.038 Uiso 1 1 calc R . . H14B H 0.0585 0.1587 0.2924 0.038 Uiso 1 1 calc R . . C15 C 0.0341(6) 0.4277(5) 0.2414(2) 0.0385(16) Uani 1 1 d . . . H15A H 0.0199 0.4879 0.2576 0.058 Uiso 1 1 calc R . . H15B H -0.0343 0.3865 0.2252 0.058 Uiso 1 1 calc R . . H15C H 0.0936 0.4518 0.2236 0.058 Uiso 1 1 calc R . . C12 C 0.0814(5) 0.3952(5) 0.31238(18) 0.0285(14) Uani 1 1 d . . . H12A H 0.0097 0.4005 0.3228 0.034 Uiso 1 1 calc R . . H12B H 0.1389 0.4631 0.3199 0.034 Uiso 1 1 calc R . . C13 C 0.1183(6) 0.3067(5) 0.3288(2) 0.0344(15) Uani 1 1 d . . . H13A H 0.1941 0.3343 0.3426 0.041 Uiso 1 1 calc R . . H13B H 0.0655 0.2752 0.3479 0.041 Uiso 1 1 calc R . . O46 O 0.9644(4) 0.8562(4) 0.38460(13) 0.0380(11) Uani 1 1 d . . . N4 N 0.9995(4) 0.7164(4) 0.34563(18) 0.0374(13) Uani 1 1 d . . . C17 C 0.9983(5) 0.6691(5) 0.3026(2) 0.0399(18) Uani 1 1 d . . . H17A H 0.9419 0.6002 0.2968 0.048 Uiso 1 1 calc R . . H17B H 1.0726 0.6610 0.2963 0.048 Uiso 1 1 calc R . . C18 C 0.9681(7) 0.7461(6) 0.2786(2) 0.050(2) Uani 1 1 d . . . H18A H 0.9023 0.7106 0.2596 0.060 Uiso 1 1 calc R . . H18B H 1.0316 0.7785 0.2633 0.060 Uiso 1 1 calc R . . C19 C 0.9411(6) 0.8302(5) 0.3104(2) 0.0408(17) Uani 1 1 d . . . H19A H 0.9865 0.9009 0.3073 0.049 Uiso 1 1 calc R . . H19B H 0.8609 0.8267 0.3077 0.049 Uiso 1 1 calc R . . C16 C 0.9707(5) 0.8034(5) 0.3509(2) 0.0314(15) Uani 1 1 d . . . C20 C 1.0293(6) 0.6660(6) 0.3781(3) 0.052(2) Uani 1 1 d . . . H20A H 1.0476 0.6026 0.3668 0.078 Uiso 1 1 calc R . . H20B H 0.9660 0.6480 0.3948 0.078 Uiso 1 1 calc R . . H20C H 1.0942 0.7136 0.3944 0.078 Uiso 1 1 calc R . . O47 O 0.1229(5) 0.8182(4) 0.14392(15) 0.0486(13) Uani 1 1 d . . . N5 N 0.2611(5) 0.7455(5) 0.15908(19) 0.0472(16) Uani 1 1 d . . . C25 C 0.2121(8) 0.6972(9) 0.1938(3) 0.078(3) Uani 1 1 d . . . H25A H 0.2624 0.6620 0.2045 0.116 Uiso 1 1 calc R . . H25B H 0.1395 0.6464 0.1850 0.116 Uiso 1 1 calc R . . H25C H 0.2020 0.7512 0.2146 0.116 Uiso 1 1 calc R . . C22 C 0.3704(7) 0.7357(10) 0.1463(3) 0.080(3) Uani 1 1 d . . . H22A H 0.3679 0.6618 0.1388 0.096 Uiso 1 1 calc R . . H22B H 0.4305 0.7692 0.1677 0.096 Uiso 1 1 calc R . . C23 C 0.3880(11) 0.7930(19) 0.1097(6) 0.221(11) Uani 1 1 d U . . H23A H 0.4568 0.8524 0.1145 0.265 Uiso 1 1 calc R . . H23B H 0.3958 0.7453 0.0857 0.265 Uiso 1 1 calc R . . C24 C 0.2867(8) 0.8314(10) 0.1034(3) 0.095(4) Uani 1 1 d . . . H24A H 0.3093 0.9080 0.1049 0.115 Uiso 1 1 calc R . . H24B H 0.2468 0.7994 0.0770 0.115 Uiso 1 1 calc R . . C21 C 0.2134(6) 0.7983(5) 0.1370(2) 0.0389(17) Uani 1 1 d . . . O48 O 1.0598(4) 0.6182(3) 0.47147(13) 0.0338(11) Uani 1 1 d . . . N6 N 1.0272(4) 0.4542(4) 0.43383(15) 0.0270(11) Uani 1 1 d . . . C26 C 0.9931(5) 0.5311(5) 0.45557(18) 0.0258(13) Uani 1 1 d . . . C28 C 0.8313(5) 0.3794(5) 0.4386(2) 0.0360(16) Uani 1 1 d . . . H28A H 0.8158 0.3355 0.4600 0.043 Uiso 1 1 calc R . . H28B H 0.7635 0.3623 0.4202 0.043 Uiso 1 1 calc R . . C29 C 0.8682(5) 0.4967(5) 0.4566(2) 0.0333(15) Uani 1 1 d . . . H29A H 0.8335 0.5366 0.4405 0.040 Uiso 1 1 calc R . . H29B H 0.8463 0.5069 0.4845 0.040 Uiso 1 1 calc R . . O51 O 0.8579(4) 0.0785(3) 0.43347(13) 0.0342(11) Uani 1 1 d . . . O49 O 0.6409(4) 0.2585(4) 0.20150(15) 0.0481(13) Uani 1 1 d . . . N7 N 0.6804(5) 0.1129(4) 0.16775(17) 0.0407(14) Uani 1 1 d . . . C35 C 0.6152(9) 0.1053(8) 0.1299(3) 0.082(3) Uani 1 1 d . . . H35A H 0.6228 0.0465 0.1109 0.123 Uiso 1 1 calc R . . H35B H 0.6431 0.1697 0.1186 0.123 Uiso 1 1 calc R . . H35C H 0.5362 0.0949 0.1350 0.123 Uiso 1 1 calc R . . C32 C 0.7328(8) 0.0318(6) 0.1749(2) 0.054(2) Uani 1 1 d . . . H32A H 0.7792 0.0178 0.1527 0.064 Uiso 1 1 calc R . . H32B H 0.6754 -0.0337 0.1777 0.064 Uiso 1 1 calc R . . C31 C 0.6880(5) 0.1860(5) 0.2001(2) 0.0349(16) Uani 1 1 d . . . C33 C 0.8063(6) 0.0782(6) 0.2147(3) 0.052(2) Uani 1 1 d . . . H33A H 0.8854 0.1092 0.2096 0.063 Uiso 1 1 calc R . . H33B H 0.8020 0.0246 0.2322 0.063 Uiso 1 1 calc R . . C34 C 0.7528(8) 0.1634(6) 0.2338(3) 0.059(2) Uani 1 1 d . . . H34A H 0.7028 0.1375 0.2546 0.071 Uiso 1 1 calc R . . H34B H 0.8115 0.2268 0.2461 0.071 Uiso 1 1 calc R . . O50 O 0.2931(4) 0.0874(3) 0.17707(15) 0.0436(12) Uani 1 1 d . . . N8 N 0.2150(5) 0.0095(4) 0.23066(16) 0.0333(13) Uani 1 1 d . . . C36 C 0.3013(6) 0.0542(5) 0.2100(2) 0.0376(17) Uani 1 1 d . . . C39 C 0.4088(6) 0.0558(5) 0.2328(3) 0.0456(19) Uani 1 1 d . . . H39A H 0.4660 0.1238 0.2337 0.055 Uiso 1 1 calc R . . H39B H 0.4392 0.0002 0.2200 0.055 Uiso 1 1 calc R . . C40 C 0.0965(6) -0.0172(6) 0.2159(2) 0.0429(18) Uani 1 1 d . . . H40A H 0.0489 -0.0492 0.2359 0.064 Uiso 1 1 calc R . . H40B H 0.0836 -0.0661 0.1908 0.064 Uiso 1 1 calc R . . H40C H 0.0784 0.0462 0.2112 0.064 Uiso 1 1 calc R . . C38 C 0.3747(7) 0.0376(5) 0.2753(3) 0.053(2) Uani 1 1 d . . . H38A H 0.3852 0.1043 0.2933 0.064 Uiso 1 1 calc R . . H38B H 0.4185 -0.0032 0.2870 0.064 Uiso 1 1 calc R . . C37 C 0.2490(7) -0.0245(6) 0.2682(2) 0.049(2) Uani 1 1 d . . . H37A H 0.2387 -0.1005 0.2643 0.059 Uiso 1 1 calc R . . H37B H 0.2061 -0.0058 0.2908 0.059 Uiso 1 1 calc R . . O54 O 0.0226(4) 0.2194(3) 0.49971(13) 0.0337(11) Uani 1 1 d . . . O55 O 0.3713(5) 0.4564(4) 0.12590(18) 0.0641(16) Uani 1 1 d . . . O56 O 0.3445(7) 0.0842(8) 0.0909(3) 0.151(4) Uani 1 1 d . . . O57 O 0.4798(6) 0.3124(9) 0.1562(4) 0.167(5) Uani 1 1 d . . . Ba1 Ba 0.13102(3) 0.11347(2) 0.545779(10) 0.01784(9) Uani 1 1 d . . . Ba2 Ba 0.24867(3) 0.27605(3) 0.163850(11) 0.03109(11) Uani 1 1 d . . . C61 C 0.7906(6) 0.0855(5) 0.4083(3) 0.048(2) Uani 1 1 d D . . C62 C 0.6530(10) 0.0933(6) 0.3604(4) 0.085(4) Uani 1 1 d D . . H62A H 0.6190 0.1502 0.3580 0.102 Uiso 1 1 calc R B 1 H62B H 0.5956 0.0257 0.3521 0.102 Uiso 1 1 calc R B 1 C68 C 0.2835(6) 0.0326(6) 0.3886(2) 0.0395(17) Uani 1 1 d D . . H68A H 0.2879 -0.0226 0.3667 0.047 Uiso 1 1 calc R C 1 H68B H 0.3600 0.0765 0.3981 0.047 Uiso 1 1 calc R C 1 C70 C 0.1484(6) 0.1310(6) 0.4094(3) 0.050(2) Uani 1 1 d D . . H70A H 0.0714 0.1321 0.4021 0.059 Uiso 1 1 calc R D 1 H70B H 0.1906 0.2000 0.4243 0.059 Uiso 1 1 calc R D 1 C66 C 0.2403(7) -0.0864(6) 0.4419(3) 0.057(2) Uani 1 1 d D . . H66A H 0.2953 -0.1170 0.4290 0.085 Uiso 1 1 calc R E 1 H66B H 0.1695 -0.1409 0.4420 0.085 Uiso 1 1 calc R E 1 H66C H 0.2680 -0.0549 0.4694 0.085 Uiso 1 1 calc R E 1 C27 C 0.9322(5) 0.3632(5) 0.4158(2) 0.0310(15) Uani 1 1 d . . . H27A H 0.9464 0.2970 0.4198 0.037 Uiso 1 1 calc R . . H27B H 0.9194 0.3631 0.3867 0.037 Uiso 1 1 calc R . . C30 C 1.1446(5) 0.4636(5) 0.4248(2) 0.0344(15) Uani 1 1 d . . . H30A H 1.1488 0.3987 0.4088 0.052 Uiso 1 1 calc R . . H30B H 1.1912 0.4771 0.4498 0.052 Uiso 1 1 calc R . . H30C H 1.1716 0.5212 0.4096 0.052 Uiso 1 1 calc R . . N12 N 0.2232(7) -0.0107(6) 0.4208(3) 0.030(2) Uani 0.60 1 d PD F 1 C67 C 0.2037(10) 0.1038(9) 0.3741(4) 0.039(3) Uani 0.60 1 d P F 1 H67A H 0.2504 0.1672 0.3648 0.047 Uiso 0.60 1 calc PR F 1 H67B H 0.1483 0.0630 0.3521 0.047 Uiso 0.60 1 calc PR F 1 C69 C 0.1467(10) 0.0387(9) 0.4360(4) 0.031(3) Uani 0.60 1 d PD F 1 C67A C 0.3256(16) -0.0413(14) 0.4200(6) 0.042(5) Uani 0.40 1 d P F 2 N12A N 0.2004(12) 0.0577(11) 0.4145(4) 0.027(3) Uani 0.40 1 d P F 2 C69A C 0.1649(14) 0.0053(13) 0.4433(5) 0.012(4) Uiso 0.40 1 d P F 2 N13 N 0.6991(11) 0.1015(7) 0.4012(4) 0.046(3) Uani 0.60 1 d P G 1 C65 C 0.6379(18) 0.1056(12) 0.4395(6) 0.090(7) Uani 0.60 1 d P G 1 H65A H 0.5659 0.1182 0.4339 0.136 Uiso 0.60 1 calc PR G 1 H65B H 0.6834 0.1620 0.4597 0.136 Uiso 0.60 1 calc PR G 1 H65C H 0.6252 0.0393 0.4496 0.136 Uiso 0.60 1 calc PR G 1 C63 C 0.7531(15) 0.1024(12) 0.3355(5) 0.076(5) Uani 0.60 1 d PD G 1 H63A H 0.7324 0.0555 0.3095 0.091 Uiso 0.60 1 calc PR G 1 H63B H 0.7845 0.1747 0.3304 0.091 Uiso 0.60 1 calc PR G 1 C64 C 0.8337(19) 0.0715(16) 0.3600(6) 0.048(6) Uani 0.60 1 d PD G 1 H64A H 0.9105 0.1170 0.3588 0.058 Uiso 0.60 1 calc PR G 1 H64B H 0.8321 -0.0015 0.3507 0.058 Uiso 0.60 1 calc PR G 1 N13A N 0.7603(14) 0.0900(11) 0.3735(6) 0.046(4) Uani 0.40 1 d PD G 2 C63A C 0.5878(18) 0.0841(19) 0.3970(7) 0.102(11) Uani 0.40 1 d PDU G 2 C65A C 0.857(4) 0.071(4) 0.3459(12) 0.092(17) Uani 0.40 1 d P G 2 C64A C 0.6799(17) 0.098(3) 0.4282(9) 0.071(9) Uiso 0.40 1 d PD G 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V3 0.0180(5) 0.0152(5) 0.0200(5) -0.0045(4) -0.0035(4) 0.0042(4) V1 0.0151(5) 0.0197(5) 0.0181(5) 0.0009(4) 0.0000(4) 0.0007(4) V6 0.0212(5) 0.0117(4) 0.0221(5) 0.0001(4) -0.0051(4) 0.0022(4) V2 0.0151(5) 0.0128(4) 0.0163(5) -0.0004(4) -0.0003(4) 0.0030(4) V5 0.0211(5) 0.0147(5) 0.0279(6) 0.0003(4) -0.0054(4) 0.0053(4) V8 0.0255(5) 0.0132(4) 0.0229(5) 0.0020(4) -0.0044(4) 0.0029(4) V7 0.0218(5) 0.0131(4) 0.0191(5) -0.0014(4) -0.0068(4) 0.0035(4) V10 0.0289(6) 0.0188(5) 0.0244(6) 0.0083(4) -0.0028(5) -0.0013(4) V4 0.0180(5) 0.0182(5) 0.0169(5) 0.0012(4) -0.0032(4) 0.0020(4) V9 0.0198(5) 0.0209(5) 0.0282(6) -0.0058(4) -0.0057(4) 0.0085(4) O6 0.021(2) 0.0145(18) 0.023(2) -0.0043(16) -0.0013(17) 0.0053(16) O3 0.0172(19) 0.0132(18) 0.018(2) -0.0015(15) -0.0004(16) 0.0024(15) O19 0.022(2) 0.019(2) 0.026(2) -0.0009(17) -0.0094(18) 0.0042(17) O25 0.022(2) 0.0166(19) 0.022(2) -0.0036(16) -0.0081(17) 0.0049(16) O8 0.0135(18) 0.0154(18) 0.022(2) 0.0006(16) -0.0030(16) 0.0007(15) O11 0.0185(19) 0.0165(18) 0.017(2) 0.0006(15) -0.0008(16) 0.0025(15) O9 0.0147(18) 0.0142(18) 0.0162(19) -0.0010(15) -0.0017(15) 0.0018(15) O10 0.026(2) 0.0134(18) 0.020(2) 0.0020(16) -0.0050(17) 0.0031(16) O15 0.0143(19) 0.026(2) 0.034(2) -0.0100(18) -0.0100(18) 0.0075(17) O16 0.024(2) 0.021(2) 0.020(2) -0.0040(16) -0.0053(17) 0.0059(17) O14 0.017(2) 0.032(2) 0.023(2) -0.0051(18) 0.0000(17) 0.0057(17) O26 0.022(2) 0.025(2) 0.044(3) -0.005(2) -0.006(2) 0.0105(18) O5 0.022(2) 0.0185(19) 0.022(2) 0.0002(16) -0.0085(17) 0.0046(16) O27 0.025(2) 0.022(2) 0.023(2) -0.0011(17) -0.0062(18) 0.0007(17) O20 0.023(2) 0.0177(19) 0.026(2) 0.0083(17) -0.0039(18) -0.0026(16) O28 0.022(2) 0.023(2) 0.027(2) -0.0059(17) -0.0053(18) 0.0059(17) O4 0.0151(19) 0.022(2) 0.024(2) -0.0016(17) -0.0073(17) 0.0010(16) O1 0.0175(19) 0.0186(19) 0.016(2) 0.0033(16) -0.0045(16) 0.0015(16) O2 0.0189(19) 0.0091(17) 0.018(2) -0.0011(15) 0.0001(16) 0.0014(15) O13 0.030(2) 0.0168(19) 0.027(2) -0.0010(17) -0.0089(18) 0.0075(17) O22 0.028(2) 0.025(2) 0.022(2) 0.0117(18) -0.0056(18) 0.0001(18) O12 0.026(2) 0.0122(18) 0.026(2) -0.0017(16) -0.0053(18) 0.0031(16) O18 0.042(3) 0.020(2) 0.033(3) 0.0087(18) -0.003(2) 0.0033(19) O23 0.028(2) 0.019(2) 0.030(2) 0.0073(18) -0.0056(19) 0.0020(17) O7 0.020(2) 0.0124(18) 0.030(2) -0.0025(16) -0.0021(17) 0.0023(15) O21 0.022(2) 0.030(2) 0.021(2) 0.0063(18) 0.0011(17) 0.0004(17) O24 0.044(3) 0.032(2) 0.037(3) 0.018(2) -0.005(2) -0.006(2) O17 0.026(2) 0.037(3) 0.041(3) -0.016(2) -0.005(2) 0.015(2) V11 0.0242(5) 0.0247(5) 0.0178(5) 0.0011(4) -0.0002(4) 0.0124(4) V13 0.0340(6) 0.0236(5) 0.0181(5) -0.0007(4) -0.0014(5) 0.0007(5) V12 0.0256(5) 0.0240(5) 0.0137(5) 0.0002(4) -0.0011(4) 0.0059(4) V15 0.0233(5) 0.0354(6) 0.0217(6) 0.0028(5) 0.0037(4) 0.0041(5) V14 0.0430(7) 0.0232(5) 0.0222(6) 0.0054(4) 0.0020(5) 0.0111(5) O41 0.036(2) 0.030(2) 0.020(2) -0.0006(18) -0.0044(19) 0.0046(19) O34 0.049(3) 0.031(2) 0.024(2) -0.002(2) -0.006(2) -0.004(2) O30 0.028(2) 0.026(2) 0.016(2) 0.0008(17) -0.0022(17) 0.0096(18) O32 0.029(2) 0.037(2) 0.026(2) 0.006(2) 0.0020(19) 0.0002(19) O35 0.033(2) 0.031(2) 0.020(2) 0.0038(18) -0.0021(18) 0.0101(19) O31 0.026(2) 0.021(2) 0.017(2) -0.0001(16) 0.0036(17) 0.0097(17) O33 0.044(3) 0.024(2) 0.022(2) -0.0012(18) 0.004(2) 0.008(2) O38 0.031(2) 0.031(2) 0.019(2) 0.0032(18) 0.0038(18) 0.0113(19) O29 0.022(2) 0.021(2) 0.019(2) 0.0010(16) -0.0002(17) 0.0071(16) O42 0.020(2) 0.036(2) 0.023(2) 0.0014(18) 0.0063(17) 0.0120(18) O36 0.040(2) 0.026(2) 0.021(2) 0.0045(18) 0.0023(19) 0.0181(19) O40 0.067(3) 0.036(3) 0.035(3) 0.013(2) 0.006(2) 0.025(2) O37 0.042(3) 0.027(2) 0.018(2) 0.0040(18) 0.0038(19) -0.0005(19) O39 0.025(2) 0.061(3) 0.030(3) 0.009(2) 0.007(2) 0.005(2) O52 0.032(3) 0.056(3) 0.052(3) -0.009(3) 0.000(3) -0.001(3) N10 0.032(7) 0.027(6) 0.032(6) 0.005(4) -0.003(5) 0.010(6) C50 0.026(6) 0.035(6) 0.034(6) 0.004(5) 0.007(5) 0.003(5) C46 0.030(8) 0.018(8) 0.032(8) 0.001(6) -0.007(6) -0.005(7) C50A 0.10(2) 0.11(2) 0.17(3) 0.07(2) 0.07(2) 0.070(18) N10A 0.09(2) 0.031(12) 0.060(14) 0.005(10) 0.014(14) 0.008(16) C46A 0.09(3) 0.025(13) 0.027(12) -0.012(10) 0.001(12) 0.011(17) C49 0.084(7) 0.056(5) 0.054(5) 0.015(4) 0.019(5) 0.031(5) C51 0.063(5) 0.040(4) 0.055(5) 0.016(4) 0.014(4) 0.020(4) C47 0.037(4) 0.069(5) 0.054(5) 0.022(4) 0.014(4) 0.013(4) O53 0.020(2) 0.021(2) 0.018(2) -0.0010(17) -0.0001(17) -0.0029(17) O43 0.112(5) 0.105(5) 0.033(3) 0.003(3) -0.013(3) 0.076(4) N1 0.094(7) 0.092(7) 0.073(6) -0.019(5) -0.011(5) 0.052(6) C4 0.074(7) 0.074(7) 0.123(10) -0.045(7) 0.028(7) 0.026(6) C1 0.154(11) 0.099(8) 0.032(5) 0.007(5) 0.017(6) 0.107(9) C5 0.084(7) 0.048(5) 0.083(7) 0.021(5) -0.007(6) 0.018(5) C3 0.099(9) 0.129(11) 0.094(10) -0.017(8) -0.005(8) 0.051(9) C2 0.096(8) 0.103(8) 0.060(6) -0.042(6) -0.042(6) 0.077(7) O44 0.026(2) 0.027(2) 0.034(3) -0.0065(19) -0.003(2) -0.0006(19) N2 0.028(3) 0.029(3) 0.028(3) 0.002(2) 0.001(2) 0.006(2) C9 0.022(3) 0.029(3) 0.046(4) -0.001(3) 0.008(3) 0.010(3) C6 0.026(3) 0.026(3) 0.027(3) -0.008(3) 0.006(3) 0.003(3) C10 0.051(4) 0.039(4) 0.027(4) 0.007(3) 0.001(3) 0.023(3) C8 0.025(3) 0.037(4) 0.038(4) 0.001(3) 0.009(3) 0.001(3) C7 0.030(4) 0.028(3) 0.040(4) 0.004(3) 0.009(3) -0.004(3) O45 0.035(3) 0.031(2) 0.028(3) -0.004(2) 0.000(2) 0.003(2) N3 0.025(3) 0.028(3) 0.027(3) 0.000(2) 0.000(2) 0.006(2) C11 0.018(3) 0.025(3) 0.036(4) -0.003(3) -0.002(3) -0.001(3) C14 0.026(3) 0.032(3) 0.034(4) 0.007(3) 0.001(3) 0.004(3) C15 0.041(4) 0.041(4) 0.031(4) -0.003(3) -0.003(3) 0.014(3) C12 0.024(3) 0.038(4) 0.021(3) -0.002(3) 0.004(3) 0.008(3) C13 0.031(4) 0.036(4) 0.031(4) 0.008(3) 0.005(3) -0.001(3) O46 0.031(2) 0.045(3) 0.027(3) -0.013(2) 0.006(2) 0.001(2) N4 0.025(3) 0.042(3) 0.042(4) 0.007(3) 0.005(3) 0.004(3) C17 0.020(3) 0.046(4) 0.040(4) -0.023(3) 0.004(3) 0.001(3) C18 0.056(5) 0.047(4) 0.037(4) -0.001(4) 0.016(4) 0.001(4) C19 0.036(4) 0.040(4) 0.033(4) -0.004(3) 0.013(3) -0.008(3) C16 0.016(3) 0.035(4) 0.033(4) -0.005(3) 0.003(3) -0.006(3) C20 0.037(4) 0.051(5) 0.064(6) 0.022(4) -0.005(4) 0.001(4) O47 0.061(3) 0.061(3) 0.036(3) 0.014(2) -0.004(3) 0.034(3) N5 0.038(3) 0.069(4) 0.047(4) 0.030(3) 0.004(3) 0.025(3) C25 0.074(6) 0.120(8) 0.068(6) 0.054(6) 0.023(5) 0.055(6) C22 0.037(5) 0.145(9) 0.086(7) 0.068(7) 0.015(5) 0.045(6) C23 0.094(9) 0.44(3) 0.240(18) 0.29(2) 0.095(10) 0.135(14) C24 0.048(5) 0.154(10) 0.102(8) 0.094(8) 0.007(5) 0.022(6) C21 0.029(4) 0.043(4) 0.042(4) 0.010(3) -0.009(3) 0.006(3) O48 0.045(3) 0.026(2) 0.030(3) -0.0041(19) -0.009(2) 0.016(2) N6 0.025(3) 0.024(3) 0.028(3) 0.000(2) -0.004(2) 0.004(2) C26 0.032(3) 0.028(3) 0.020(3) 0.004(3) -0.005(3) 0.011(3) C28 0.026(3) 0.052(4) 0.031(4) 0.013(3) -0.005(3) 0.010(3) C29 0.032(4) 0.048(4) 0.026(3) 0.008(3) -0.006(3) 0.022(3) O51 0.042(3) 0.021(2) 0.034(3) -0.0025(19) -0.018(2) 0.005(2) O49 0.056(3) 0.047(3) 0.048(3) 0.002(2) 0.013(3) 0.028(3) N7 0.050(4) 0.037(3) 0.032(3) 0.001(3) 0.012(3) 0.008(3) C35 0.112(8) 0.075(7) 0.048(6) 0.005(5) -0.018(6) 0.013(6) C32 0.089(6) 0.040(4) 0.040(5) 0.009(4) 0.032(4) 0.029(4) C31 0.030(4) 0.025(3) 0.043(4) -0.004(3) 0.010(3) 0.001(3) C33 0.035(4) 0.044(4) 0.084(7) 0.013(4) 0.011(4) 0.019(3) C34 0.073(6) 0.045(5) 0.059(6) -0.011(4) -0.002(5) 0.024(4) O50 0.058(3) 0.031(3) 0.036(3) 0.001(2) 0.006(2) 0.004(2) N8 0.040(3) 0.023(3) 0.032(3) 0.000(2) -0.003(3) 0.004(2) C36 0.050(4) 0.020(3) 0.039(4) -0.001(3) 0.000(4) 0.007(3) C39 0.042(4) 0.025(3) 0.070(6) 0.003(4) 0.000(4) 0.012(3) C40 0.048(4) 0.039(4) 0.038(4) 0.003(3) 0.000(3) 0.008(3) C38 0.064(5) 0.026(4) 0.065(6) -0.003(4) -0.032(5) 0.014(4) C37 0.065(5) 0.042(4) 0.041(5) 0.009(4) -0.007(4) 0.015(4) O54 0.039(3) 0.027(2) 0.035(3) -0.0006(19) -0.012(2) 0.013(2) O55 0.058(4) 0.058(4) 0.069(4) 0.015(3) -0.002(3) 0.003(3) O56 0.080(6) 0.170(9) 0.189(10) -0.002(7) -0.077(6) 0.038(6) O57 0.076(5) 0.264(12) 0.248(12) 0.206(10) 0.094(6) 0.102(7) Ba1 0.01837(17) 0.01469(16) 0.01690(18) -0.00203(13) -0.00293(13) 0.00156(13) Ba2 0.0332(2) 0.0310(2) 0.0196(2) -0.00030(16) -0.00682(16) -0.00331(17) C61 0.033(4) 0.012(3) 0.091(7) 0.006(4) -0.031(4) 0.001(3) C62 0.103(9) 0.030(4) 0.119(10) -0.004(5) -0.079(8) 0.028(5) C68 0.032(4) 0.046(4) 0.039(4) -0.003(3) 0.015(3) 0.012(3) C70 0.033(4) 0.041(4) 0.070(6) -0.006(4) -0.004(4) 0.010(3) C66 0.058(5) 0.036(4) 0.069(6) 0.015(4) -0.013(5) 0.002(4) C27 0.031(3) 0.026(3) 0.032(4) 0.003(3) 0.002(3) 0.003(3) C30 0.024(3) 0.035(4) 0.041(4) -0.001(3) 0.001(3) 0.009(3) N12 0.025(5) 0.019(5) 0.040(6) 0.000(4) -0.006(4) 0.001(4) C67 0.045(7) 0.036(6) 0.031(6) 0.007(5) 0.011(6) 0.001(5) C69 0.022(7) 0.016(6) 0.049(9) -0.012(6) -0.017(7) 0.004(5) C67A 0.048(11) 0.037(10) 0.053(12) -0.004(9) 0.014(9) 0.034(9) N12A 0.017(7) 0.032(8) 0.029(8) -0.008(6) -0.002(6) 0.009(6) N13 0.078(9) 0.017(5) 0.037(7) 0.008(5) -0.020(6) 0.005(5) C65 0.120(15) 0.036(8) 0.099(14) 0.000(8) 0.094(13) -0.009(9) C63 0.138(17) 0.040(8) 0.047(10) 0.016(7) 0.033(11) 0.014(10) C64 0.062(16) 0.029(8) 0.040(13) -0.013(8) -0.005(11) -0.001(9) N13A 0.056(12) 0.018(8) 0.055(13) 0.014(8) -0.012(11) -0.005(8) C63A 0.042(14) 0.055(15) 0.20(3) -0.018(19) -0.017(18) 0.029(12) C65A 0.061(19) 0.12(3) 0.06(3) -0.02(2) 0.029(19) -0.013(18) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V3 O28 1.611(4) . ? V3 O12 1.713(4) . ? V3 O3 1.931(4) . ? V3 O15 1.946(4) . ? V3 O4 2.136(4) . ? V3 O2 2.232(4) . ? V3 V8 3.0989(15) . ? V3 V4 3.1187(15) . ? V1 O14 1.687(4) . ? V1 O21 1.687(4) . ? V1 O8 1.838(4) . ? V1 O4 2.071(4) . ? V1 O1 2.085(4) . ? V1 O2 2.086(4) . ? V1 V9 3.0602(15) . ? V1 V10 3.0645(15) . ? V6 O25 1.614(4) . ? V6 O7 1.815(4) . ? V6 O20 1.819(4) . ? V6 O9 1.980(4) . ? V6 O8 2.000(4) . ? V6 O1 2.310(4) . ? V6 V7 3.0298(14) . ? V6 V10 3.0808(15) . ? V6 V5 3.0824(15) . ? V2 O11 1.685(4) . ? V2 O6 1.690(4) . ? V2 O9 1.894(3) . ? V2 O3 1.958(4) . ? V2 O1 2.110(4) . ? V2 O2 2.124(4) . ? V2 V5 3.0725(14) . ? V2 V8 3.0929(14) . ? V2 V4 3.1071(15) . ? V5 O26 1.605(4) . ? V5 O23 1.815(4) . ? V5 O7 1.821(4) . ? V5 O5 1.984(4) . ? V5 O6 2.025(4) . ? V5 O1 2.352(4) . ? V5 V10 3.0741(17) . ? V5 V4 3.1050(17) . ? V8 O18 1.589(4) . ? V8 O13 1.804(4) . ? V8 O10 1.859(4) . ? V8 O12 1.979(4) . ? V8 O11 2.043(4) . ? V8 O2 2.368(4) . ? V8 V9 3.0788(17) . ? V8 V7 3.0951(17) . ? V7 O19 1.607(4) . ? V7 O10 1.795(4) . ? V7 O16 1.840(4) . ? V7 O9 1.970(4) . ? V7 O8 2.014(4) . ? V7 O2 2.318(4) . ? V7 V9 3.0921(16) . ? V10 O24 1.594(4) . ? V10 O23 1.813(4) . ? V10 O20 1.821(4) . ? V10 O22 2.012(4) . ? V10 O21 2.031(4) . ? V10 O1 2.324(4) . ? V4 O27 1.612(4) . ? V4 O5 1.715(4) . ? V4 O3 1.918(4) . ? V4 O22 1.964(4) . ? V4 O4 2.129(4) . ? V4 O1 2.237(4) . ? V9 O17 1.599(4) . ? V9 O16 1.804(4) . ? V9 O13 1.830(4) . ? V9 O15 1.996(4) . ? V9 O14 2.030(4) . ? V9 O2 2.307(4) . ? O19 Ba1 2.806(4) 2_666 ? O25 Ba1 2.826(4) 2_666 ? O27 Ba2 2.831(4) . ? O28 Ba2 2.959(4) . ? V11 O36 1.657(4) . ? V11 O42 1.703(4) . ? V11 O31 1.889(4) 2_575 ? V11 O30 2.032(4) . ? V11 O29 2.052(4) . ? V11 O29 2.153(4) 2_575 ? V11 V14 3.0759(18) . ? V11 V15 3.0963(18) 2_575 ? V11 V13 3.1002(18) 2_575 ? V11 V12 3.1047(16) 2_575 ? V13 O34 1.611(4) . ? V13 O33 1.744(4) . ? V13 O32 1.867(4) . ? V13 O31 1.959(4) . ? V13 O30 2.092(4) . ? V13 O29 2.309(4) 2_575 ? V13 V14 3.0634(16) 2_575 ? V13 V11 3.1002(18) 2_575 ? V12 O41 1.612(4) . ? V12 O38 1.702(4) . ? V12 O35 1.913(4) . ? V12 O31 1.950(4) . ? V12 O30 2.134(4) . ? V12 O29 2.266(4) . ? V12 V11 3.1047(15) 2_575 ? V15 O39 1.594(4) . ? V15 O32 1.844(4) 2_575 ? V15 O37 1.872(4) . ? V15 O38 1.970(4) . ? V15 O42 2.001(4) 2_575 ? V15 O29 2.378(4) . ? V15 V14 3.0786(17) . ? V15 V11 3.0963(18) 2_575 ? V14 O40 1.587(4) . ? V14 O37 1.767(4) . ? V14 O33 1.898(4) 2_575 ? V14 O35 1.933(4) . ? V14 O36 2.112(4) . ? V14 O29 2.312(4) . ? V14 V13 3.0633(16) 2_575 ? O41 Ba2 2.840(4) 1_565 ? O34 Ba2 2.865(4) 1_565 ? O32 V15 1.844(4) 2_575 ? O31 V11 1.889(4) 2_575 ? O33 V14 1.898(4) 2_575 ? O29 V11 2.153(4) 2_575 ? O29 V13 2.309(4) 2_575 ? O42 V15 2.001(4) 2_575 ? O52 C46A 1.25(4) . ? O52 C46 1.28(2) . ? N10 C46 1.34(2) . ? N10 C47 1.397(17) . ? N10 C49 1.419(16) . ? C50 C47 1.543(13) . ? C50 C51 1.571(12) . ? C46 C51 1.55(2) . ? C50A C49 1.40(3) . ? C50A C47 1.68(3) . ? N10A C46A 1.24(3) . ? N10A C51 1.37(3) . ? N10A C47 1.49(4) . ? C46A C49 1.67(5) . ? O53 C69A 1.241(18) . ? O53 C69 1.272(16) . ? O53 Ba1 2.724(4) 2_556 ? O53 Ba1 2.748(4) . ? O43 C1 1.244(11) . ? O43 Ba2 2.704(6) 1_655 ? N1 C1 1.257(12) . ? N1 C5 1.378(12) . ? N1 C2 1.503(11) . ? C4 C1 1.565(15) . ? C4 C3 1.618(17) . ? C3 C2 1.481(16) . ? O44 C6 1.248(7) . ? O44 Ba1 2.656(4) . ? N2 C6 1.309(8) . ? N2 C10 1.454(8) . ? N2 C7 1.468(7) . ? C9 C6 1.507(8) . ? C9 C8 1.521(8) . ? C8 C7 1.522(9) . ? O45 C11 1.246(7) . ? O45 Ba2 2.638(5) . ? N3 C11 1.318(7) . ? N3 C15 1.451(8) . ? N3 C12 1.467(7) . ? C11 C14 1.506(9) . ? C14 C13 1.529(9) . ? C12 C13 1.532(9) . ? O46 C16 1.248(7) . ? O46 Ba1 2.646(4) 2_666 ? N4 C16 1.292(8) . ? N4 C20 1.434(9) . ? N4 C17 1.472(8) . ? C17 C18 1.498(10) . ? C18 C19 1.539(9) . ? C19 C16 1.497(10) . ? O47 C21 1.229(8) . ? N5 C21 1.312(8) . ? N5 C22 1.448(10) . ? N5 C25 1.457(10) . ? C22 C23 1.509(14) . ? C23 C24 1.487(14) . ? C24 C21 1.486(11) . ? O48 C26 1.247(7) . ? N6 C26 1.337(7) . ? N6 C30 1.451(8) . ? N6 C27 1.462(7) . ? C26 C29 1.470(9) . ? C28 C27 1.516(9) . ? C28 C29 1.522(9) . ? O51 C61 1.187(8) . ? O51 Ba1 2.772(4) 2_656 ? O49 C31 1.250(8) . ? N7 C31 1.323(8) . ? N7 C32 1.442(9) . ? N7 C35 1.444(10) . ? C32 C33 1.524(11) . ? C31 C34 1.464(10) . ? C33 C34 1.531(10) . ? O50 C36 1.246(8) . ? O50 Ba2 2.798(5) . ? N8 C36 1.318(9) . ? N8 C40 1.446(8) . ? N8 C37 1.471(9) . ? C36 C39 1.492(10) . ? C39 C38 1.513(11) . ? C38 C37 1.521(10) . ? O54 Ba1 2.760(4) . ? O55 Ba2 2.916(6) . ? O57 Ba2 2.758(7) . ? Ba1 O46 2.646(4) 2_666 ? Ba1 O53 2.724(4) 2_556 ? Ba1 O51 2.772(4) 2_656 ? Ba1 O19 2.806(4) 2_666 ? Ba1 O25 2.826(4) 2_666 ? Ba1 Ba1 4.476(2) 2_556 ? Ba2 O43 2.704(6) 1_455 ? Ba2 O41 2.840(4) 1_545 ? Ba2 O34 2.865(4) 1_545 ? C61 N13A 1.217(14) . ? C61 N13 1.220(13) . ? C61 C64A 1.562(18) . ? C61 C64 1.70(2) . ? C62 N13A 1.386(15) . ? C62 N13 1.426(14) . ? C62 C63A 1.470(18) . ? C62 C63 1.483(14) . ? C68 N12 1.410(10) . ? C68 N12A 1.429(16) . ? C68 C67 1.644(13) . ? C68 C67A 1.688(19) . ? C70 N12A 1.331(16) . ? C70 C67 1.422(13) . ? C70 C69 1.604(14) . ? C66 C67A 1.34(2) . ? C66 N12 1.360(10) . ? C66 C69A 1.719(19) . ? N12 C69 1.356(13) . ? N12A C69A 1.27(2) . ? N13 C65 1.49(2) . ? C63 C64 1.443(18) . ? N13A C65A 1.57(4) . ? C63A C64A 1.463(19) . ? 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 O28 V3 O12 106.1(2) . . ? O28 V3 O3 100.65(17) . . ? O12 V3 O3 95.54(17) . . ? O28 V3 O15 100.67(18) . . ? O12 V3 O15 96.16(19) . . ? O3 V3 O15 151.72(16) . . ? O28 V3 O4 95.35(18) . . ? O12 V3 O4 158.02(16) . . ? O3 V3 O4 75.42(15) . . ? O15 V3 O4 84.29(17) . . ? O28 V3 O2 168.93(18) . . ? O12 V3 O2 84.91(16) . . ? O3 V3 O2 76.73(14) . . ? O15 V3 O2 78.79(14) . . ? O4 V3 O2 73.58(14) . . ? O28 V3 V8 141.54(16) . . ? O12 V3 V8 35.69(12) . . ? O3 V3 V8 90.37(12) . . ? O15 V3 V8 84.34(13) . . ? O4 V3 V8 123.11(11) . . ? O2 V3 V8 49.53(10) . . ? O28 V3 V4 88.36(14) . . ? O12 V3 V4 131.27(13) . . ? O3 V3 V4 35.73(11) . . ? O15 V3 V4 127.20(13) . . ? O4 V3 V4 42.93(10) . . ? O2 V3 V4 83.35(9) . . ? V8 V3 V4 119.00(4) . . ? O14 V1 O21 107.0(2) . . ? O14 V1 O8 100.90(17) . . ? O21 V1 O8 100.71(18) . . ? O14 V1 O4 92.64(17) . . ? O21 V1 O4 93.01(17) . . ? O8 V1 O4 156.88(17) . . ? O14 V1 O1 163.80(18) . . ? O21 V1 O1 87.17(17) . . ? O8 V1 O1 83.68(15) . . ? O4 V1 O1 78.47(15) . . ? O14 V1 O2 86.80(17) . . ? O21 V1 O2 164.06(17) . . ? O8 V1 O2 84.03(15) . . ? O4 V1 O2 78.06(15) . . ? O1 V1 O2 78.18(14) . . ? O14 V1 V9 38.40(14) . . ? O21 V1 V9 145.38(15) . . ? O8 V1 V9 89.43(12) . . ? O4 V1 V9 89.71(11) . . ? O1 V1 V9 127.07(11) . . ? O2 V1 V9 48.90(10) . . ? O14 V1 V10 145.29(15) . . ? O21 V1 V10 38.31(14) . . ? O8 V1 V10 89.53(12) . . ? O4 V1 V10 89.86(11) . . ? O1 V1 V10 49.28(10) . . ? O2 V1 V10 127.45(10) . . ? V9 V1 V10 176.31(5) . . ? O25 V6 O7 104.09(18) . . ? O25 V6 O20 103.40(19) . . ? O7 V6 O20 93.65(18) . . ? O25 V6 O9 100.83(18) . . ? O7 V6 O9 90.02(16) . . ? O20 V6 O9 153.80(16) . . ? O25 V6 O8 99.92(17) . . ? O7 V6 O8 154.30(16) . . ? O20 V6 O8 89.58(17) . . ? O9 V6 O8 76.48(15) . . ? O25 V6 O1 173.55(16) . . ? O7 V6 O1 80.84(15) . . ? O20 V6 O1 80.21(15) . . ? O9 V6 O1 74.78(14) . . ? O8 V6 O1 74.60(14) . . ? O25 V6 V7 88.83(13) . . ? O7 V6 V7 129.80(13) . . ? O20 V6 V7 130.74(13) . . ? O9 V6 V7 39.79(10) . . ? O8 V6 V7 41.17(11) . . ? O1 V6 V7 84.79(9) . . ? O25 V6 V10 135.50(15) . . ? O7 V6 V10 83.12(13) . . ? O20 V6 V10 32.19(12) . . ? O9 V6 V10 123.29(11) . . ? O8 V6 V10 86.21(11) . . ? O1 V6 V10 48.53(9) . . ? V7 V6 V10 120.41(5) . . ? O25 V6 V5 136.05(14) . . ? O7 V6 V5 32.08(12) . . ? O20 V6 V5 83.18(12) . . ? O9 V6 V5 86.33(11) . . ? O8 V6 V5 123.77(11) . . ? O1 V6 V5 49.20(9) . . ? V7 V6 V5 119.87(5) . . ? V10 V6 V5 59.84(4) . . ? O11 V2 O6 107.96(19) . . ? O11 V2 O9 98.23(17) . . ? O6 V2 O9 98.28(16) . . ? O11 V2 O3 95.80(16) . . ? O6 V2 O3 96.04(16) . . ? O9 V2 O3 155.77(16) . . ? O11 V2 O1 164.29(17) . . ? O6 V2 O1 87.56(17) . . ? O9 V2 O1 81.49(15) . . ? O3 V2 O1 79.70(15) . . ? O11 V2 O2 87.59(16) . . ? O6 V2 O2 164.14(17) . . ? O9 V2 O2 82.12(14) . . ? O3 V2 O2 78.83(14) . . ? O1 V2 O2 76.79(14) . . ? O11 V2 V5 145.79(13) . . ? O6 V2 V5 37.89(13) . . ? O9 V2 V5 88.11(11) . . ? O3 V2 V5 91.32(11) . . ? O1 V2 V5 49.85(10) . . ? O2 V2 V5 126.62(10) . . ? O11 V2 V8 37.85(12) . . ? O6 V2 V8 145.80(14) . . ? O9 V2 V8 89.00(11) . . ? O3 V2 V8 90.06(11) . . ? O1 V2 V8 126.63(11) . . ? O2 V2 V8 49.86(10) . . ? V5 V2 V8 175.80(4) . . ? O11 V2 V4 131.96(13) . . ? O6 V2 V4 81.87(14) . . ? O9 V2 V4 127.51(12) . . ? O3 V2 V4 36.26(11) . . ? O1 V2 V4 46.03(10) . . ? O2 V2 V4 85.35(10) . . ? V5 V2 V4 60.32(4) . . ? V8 V2 V4 119.55(4) . . ? O26 V5 O23 104.1(2) . . ? O26 V5 O7 103.18(19) . . ? O23 V5 O7 93.67(18) . . ? O26 V5 O5 100.66(18) . . ? O23 V5 O5 88.34(17) . . ? O7 V5 O5 154.79(16) . . ? O26 V5 O6 101.4(2) . . ? O23 V5 O6 153.74(17) . . ? O7 V5 O6 86.41(16) . . ? O5 V5 O6 80.95(15) . . ? O26 V5 O1 174.64(18) . . ? O23 V5 O1 80.19(16) . . ? O7 V5 O1 79.56(14) . . ? O5 V5 O1 76.03(14) . . ? O6 V5 O1 73.99(14) . . ? O26 V5 V2 132.27(17) . . ? O23 V5 V2 123.47(13) . . ? O7 V5 V2 79.52(12) . . ? O5 V5 V2 78.46(11) . . ? O6 V5 V2 30.84(10) . . ? O1 V5 V2 43.29(9) . . ? O26 V5 V10 136.00(17) . . ? O23 V5 V10 32.05(13) . . ? O7 V5 V10 83.23(13) . . ? O5 V5 V10 85.31(12) . . ? O6 V5 V10 122.49(11) . . ? O1 V5 V10 48.50(9) . . ? V2 V5 V10 91.72(4) . . ? O26 V5 V6 135.06(15) . . ? O23 V5 V6 83.22(13) . . ? O7 V5 V6 31.96(12) . . ? O5 V5 V6 124.05(12) . . ? O6 V5 V6 83.11(11) . . ? O1 V5 V6 48.02(9) . . ? V2 V5 V6 61.86(4) . . ? V10 V5 V6 60.05(4) . . ? O26 V5 V4 130.98(15) . . ? O23 V5 V4 81.14(13) . . ? O7 V5 V4 125.36(12) . . ? O5 V5 V4 30.32(11) . . ? O6 V5 V4 77.53(11) . . ? O1 V5 V4 45.87(9) . . ? V2 V5 V4 60.39(3) . . ? V10 V5 V4 64.08(4) . . ? V6 V5 V4 93.84(5) . . ? O18 V8 O13 104.6(2) . . ? O18 V8 O10 103.14(19) . . ? O13 V8 O10 92.96(17) . . ? O18 V8 O12 101.20(19) . . ? O13 V8 O12 89.93(17) . . ? O10 V8 O12 153.90(16) . . ? O18 V8 O11 101.6(2) . . ? O13 V8 O11 153.52(17) . . ? O10 V8 O11 84.64(15) . . ? O12 V8 O11 81.35(15) . . ? O18 V8 O2 174.65(18) . . ? O13 V8 O2 80.04(16) . . ? O10 V8 O2 79.08(14) . . ? O12 V8 O2 75.89(14) . . ? O11 V8 O2 73.60(14) . . ? O18 V8 V9 136.82(17) . . ? O13 V8 V9 32.33(13) . . ? O10 V8 V9 83.01(13) . . ? O12 V8 V9 85.72(12) . . ? O11 V8 V9 121.54(11) . . ? O2 V8 V9 47.97(9) . . ? O18 V8 V2 132.03(17) . . ? O13 V8 V2 123.34(13) . . ? O10 V8 V2 78.50(11) . . ? O12 V8 V2 78.28(11) . . ? O11 V8 V2 30.40(11) . . ? O2 V8 V2 43.30(9) . . ? V9 V8 V2 91.16(4) . . ? O18 V8 V7 134.57(16) . . ? O13 V8 V7 82.91(12) . . ? O10 V8 V7 31.48(12) . . ? O12 V8 V7 123.84(12) . . ? O11 V8 V7 81.41(10) . . ? O2 V8 V7 47.98(9) . . ? V9 V8 V7 60.11(4) . . ? V2 V8 V7 61.06(3) . . ? O18 V8 V3 131.50(16) . . ? O13 V8 V3 81.54(13) . . ? O10 V8 V3 124.84(12) . . ? O12 V8 V3 30.33(11) . . ? O11 V8 V3 78.37(11) . . ? O2 V8 V3 45.82(9) . . ? V9 V8 V3 63.64(4) . . ? V2 V8 V3 60.88(4) . . ? V7 V8 V3 93.77(5) . . ? O19 V7 O10 104.14(19) . . ? O19 V7 O16 103.17(18) . . ? O10 V7 O16 93.73(18) . . ? O19 V7 O9 101.15(17) . . ? O10 V7 O9 91.36(16) . . ? O16 V7 O9 153.08(16) . . ? O19 V7 O8 99.38(18) . . ? O10 V7 O8 155.21(16) . . ? O16 V7 O8 88.39(17) . . ? O9 V7 O8 76.38(15) . . ? O19 V7 O2 173.54(17) . . ? O10 V7 O2 81.70(15) . . ? O16 V7 O2 78.94(14) . . ? O9 V7 O2 75.67(13) . . ? O8 V7 O2 74.47(13) . . ? O19 V7 V6 88.71(14) . . ? O10 V7 V6 131.40(13) . . ? O16 V7 V6 129.20(13) . . ? O9 V7 V6 40.04(11) . . ? O8 V7 V6 40.81(11) . . ? O2 V7 V6 85.29(9) . . ? O19 V7 V9 134.70(14) . . ? O10 V7 V9 83.58(13) . . ? O16 V7 V9 31.59(11) . . ? O9 V7 V9 123.52(11) . . ? O8 V7 V9 85.45(11) . . ? O2 V7 V9 47.89(9) . . ? V6 V7 V9 119.70(4) . . ? O19 V7 V8 136.70(15) . . ? O10 V7 V8 32.75(12) . . ? O16 V7 V8 82.61(12) . . ? O9 V7 V8 87.59(11) . . ? O8 V7 V8 123.82(11) . . ? O2 V7 V8 49.36(9) . . ? V6 V7 V8 121.04(4) . . ? V9 V7 V8 59.68(4) . . ? O24 V10 O23 104.1(2) . . ? O24 V10 O20 103.8(2) . . ? O23 V10 O20 93.75(18) . . ? O24 V10 O22 100.0(2) . . ? O23 V10 O22 87.79(17) . . ? O20 V10 O22 155.01(16) . . ? O24 V10 O21 101.0(2) . . ? O23 V10 O21 154.03(17) . . ? O20 V10 O21 86.68(17) . . ? O22 V10 O21 81.32(16) . . ? O24 V10 O1 173.5(2) . . ? O23 V10 O1 81.01(16) . . ? O20 V10 O1 79.79(15) . . ? O22 V10 O1 75.82(14) . . ? O21 V10 O1 73.50(15) . . ? O24 V10 V1 131.96(19) . . ? O23 V10 V1 123.84(13) . . ? O20 V10 V1 78.55(12) . . ? O22 V10 V1 79.92(11) . . ? O21 V10 V1 30.99(11) . . ? O1 V10 V1 42.84(9) . . ? O24 V10 V5 136.06(19) . . ? O23 V10 V5 32.08(12) . . ? O20 V10 V5 83.40(13) . . ? O22 V10 V5 84.82(12) . . ? O21 V10 V5 122.79(12) . . ? O1 V10 V5 49.29(9) . . ? V1 V10 V5 91.97(4) . . ? O24 V10 V6 135.84(16) . . ? O23 V10 V6 83.29(13) . . ? O20 V10 V6 32.17(12) . . ? O22 V10 V6 123.94(12) . . ? O21 V10 V6 83.41(12) . . ? O1 V10 V6 48.13(9) . . ? V1 V10 V6 61.04(4) . . ? V5 V10 V6 60.11(4) . . ? O27 V4 O5 106.69(19) . . ? O27 V4 O3 101.18(18) . . ? O5 V4 O3 97.26(17) . . ? O27 V4 O22 99.14(19) . . ? O5 V4 O22 95.57(18) . . ? O3 V4 O22 151.67(16) . . ? O27 V4 O4 94.81(18) . . ? O5 V4 O4 158.38(16) . . ? O3 V4 O4 75.86(15) . . ? O22 V4 O4 82.97(16) . . ? O27 V4 O1 168.75(18) . . ? O5 V4 O1 84.55(15) . . ? O3 V4 O1 77.39(14) . . ? O22 V4 O1 78.81(15) . . ? O4 V4 O1 73.99(14) . . ? O27 V4 V5 142.15(15) . . ? O5 V4 V5 35.73(12) . . ? O3 V4 V5 91.11(11) . . ? O22 V4 V5 84.73(13) . . ? O4 V4 V5 122.97(11) . . ? O1 V4 V5 49.00(10) . . ? O27 V4 V2 137.98(15) . . ? O5 V4 V2 81.04(13) . . ? O3 V4 V2 37.14(10) . . ? O22 V4 V2 121.57(12) . . ? O4 V4 V2 81.42(11) . . ? O1 V4 V2 42.76(10) . . ? V5 V4 V2 59.29(4) . . ? O27 V4 V3 88.35(14) . . ? O5 V4 V3 133.28(14) . . ? O3 V4 V3 36.02(11) . . ? O22 V4 V3 126.07(12) . . ? O4 V4 V3 43.11(11) . . ? O1 V4 V3 84.09(10) . . ? V5 V4 V3 119.74(4) . . ? V2 V4 V3 60.51(4) . . ? O17 V9 O16 104.05(19) . . ? O17 V9 O13 104.6(2) . . ? O16 V9 O13 93.01(18) . . ? O17 V9 O15 99.40(19) . . ? O16 V9 O15 155.58(16) . . ? O13 V9 O15 87.56(18) . . ? O17 V9 O14 100.1(2) . . ? O16 V9 O14 87.07(17) . . ? O13 V9 O14 154.46(17) . . ? O15 V9 O14 82.16(17) . . ? O17 V9 O2 172.6(2) . . ? O16 V9 O2 79.94(15) . . ? O13 V9 O2 81.23(15) . . ? O15 V9 O2 76.02(14) . . ? O14 V9 O2 73.63(14) . . ? O17 V9 V1 131.15(19) . . ? O16 V9 V1 78.55(12) . . ? O13 V9 V1 124.16(13) . . ? O15 V9 V1 80.96(12) . . ? O14 V9 V1 31.08(11) . . ? O2 V9 V1 42.94(9) . . ? O17 V9 V8 136.37(18) . . ? O16 V9 V8 83.62(14) . . ? O13 V9 V8 31.82(12) . . ? O15 V9 V8 84.11(13) . . ? O14 V9 V8 123.30(11) . . ? O2 V9 V8 49.67(9) . . ? V1 V9 V8 92.45(4) . . ? O17 V9 V7 136.28(15) . . ? O16 V9 V7 32.29(12) . . ? O13 V9 V7 82.61(12) . . ? O15 V9 V7 124.17(11) . . ? O14 V9 V7 83.97(11) . . ? O2 V9 V7 48.20(9) . . ? V1 V9 V7 61.22(3) . . ? V8 V9 V7 60.21(4) . . ? V2 O6 V5 111.3(2) . . ? V4 O3 V3 108.25(18) . . ? V4 O3 V2 106.59(16) . . ? V3 O3 V2 107.54(17) . . ? V7 O19 Ba1 147.8(2) . 2_666 ? V6 O25 Ba1 146.59(19) . 2_666 ? V1 O8 V6 108.75(17) . . ? V1 O8 V7 108.76(17) . . ? V6 O8 V7 98.02(17) . . ? V2 O11 V8 111.75(19) . . ? V2 O9 V7 108.88(17) . . ? V2 O9 V6 109.46(17) . . ? V7 O9 V6 100.16(16) . . ? V7 O10 V8 115.8(2) . . ? V3 O15 V9 111.43(19) . . ? V9 O16 V7 116.1(2) . . ? V1 O14 V9 110.5(2) . . ? V4 O5 V5 113.95(19) . . ? V4 O27 Ba2 150.6(2) . . ? V6 O20 V10 115.64(19) . . ? V3 O28 Ba2 146.5(2) . . ? V1 O4 V4 105.23(17) . . ? V1 O4 V3 105.41(17) . . ? V4 O4 V3 93.96(16) . . ? V1 O1 V2 102.54(15) . . ? V1 O1 V4 101.06(15) . . ? V2 O1 V4 91.21(13) . . ? V1 O1 V6 90.34(13) . . ? V2 O1 V6 91.29(14) . . ? V4 O1 V6 167.50(18) . . ? V1 O1 V10 87.89(14) . . ? V2 O1 V10 168.34(19) . . ? V4 O1 V10 91.89(13) . . ? V6 O1 V10 83.34(12) . . ? V1 O1 V5 168.52(18) . . ? V2 O1 V5 86.86(14) . . ? V4 O1 V5 85.13(12) . . ? V6 O1 V5 82.78(12) . . ? V10 O1 V5 82.21(12) . . ? V1 O2 V2 102.02(14) . . ? V1 O2 V3 101.57(15) . . ? V2 O2 V3 92.09(13) . . ? V1 O2 V9 88.16(14) . . ? V2 O2 V9 168.19(19) . . ? V3 O2 V9 91.69(13) . . ? V1 O2 V7 90.53(13) . . ? V2 O2 V7 89.97(13) . . ? V3 O2 V7 167.01(17) . . ? V9 O2 V7 83.90(12) . . ? V1 O2 V8 168.86(18) . . ? V2 O2 V8 86.85(13) . . ? V3 O2 V8 84.65(12) . . ? V9 O2 V8 82.37(12) . . ? V7 O2 V8 82.66(12) . . ? V8 O13 V9 115.9(2) . . ? V4 O22 V10 111.07(19) . . ? V3 O12 V8 113.98(19) . . ? V10 O23 V5 115.9(2) . . ? V6 O7 V5 116.0(2) . . ? V1 O21 V10 110.7(2) . . ? O36 V11 O42 106.6(2) . . ? O36 V11 O31 99.82(18) . 2_575 ? O42 V11 O31 98.69(18) . 2_575 ? O36 V11 O30 96.45(18) . . ? O42 V11 O30 93.31(18) . . ? O31 V11 O30 156.06(16) 2_575 . ? O36 V11 O29 89.20(18) . . ? O42 V11 O29 163.47(17) . . ? O31 V11 O29 82.93(16) 2_575 . ? O30 V11 O29 79.85(16) . . ? O36 V11 O29 166.51(18) . 2_575 ? O42 V11 O29 86.46(17) . 2_575 ? O31 V11 O29 81.00(15) 2_575 2_575 ? O30 V11 O29 79.14(14) . 2_575 ? O29 V11 O29 77.51(16) . 2_575 ? O36 V11 V14 40.53(15) . . ? O42 V11 V14 147.10(14) . . ? O31 V11 V14 91.00(12) 2_575 . ? O30 V11 V14 90.03(12) . . ? O29 V11 V14 48.72(11) . . ? O29 V11 V14 126.23(11) 2_575 . ? O36 V11 V15 142.93(15) . 2_575 ? O42 V11 V15 36.44(14) . 2_575 ? O31 V11 V15 91.66(12) 2_575 2_575 ? O30 V11 V15 85.76(12) . 2_575 ? O29 V11 V15 127.36(11) . 2_575 ? O29 V11 V15 50.02(10) 2_575 2_575 ? V14 V11 V15 174.87(4) . 2_575 ? O36 V11 V13 86.06(15) . 2_575 ? O42 V11 V13 135.77(14) . 2_575 ? O31 V11 V13 37.10(12) 2_575 2_575 ? O30 V11 V13 127.96(12) . 2_575 ? O29 V11 V13 48.15(10) . 2_575 ? O29 V11 V13 86.72(10) 2_575 2_575 ? V14 V11 V13 59.47(4) . 2_575 ? V15 V11 V13 121.35(5) 2_575 2_575 ? O36 V11 V12 136.30(15) . 2_575 ? O42 V11 V12 83.20(14) . 2_575 ? O31 V11 V12 36.69(11) 2_575 2_575 ? O30 V11 V12 125.98(11) . 2_575 ? O29 V11 V12 88.67(11) . 2_575 ? O29 V11 V12 46.87(10) 2_575 2_575 ? V14 V11 V12 120.41(5) . 2_575 ? V15 V11 V12 60.45(4) 2_575 2_575 ? V13 V11 V12 60.99(4) 2_575 2_575 ? O34 V13 O33 106.5(2) . . ? O34 V13 O32 101.6(2) . . ? O33 V13 O32 95.6(2) . . ? O34 V13 O31 100.8(2) . . ? O33 V13 O31 94.14(19) . . ? O32 V13 O31 151.85(17) . . ? O34 V13 O30 96.52(19) . . ? O33 V13 O30 156.08(17) . . ? O32 V13 O30 85.71(18) . . ? O31 V13 O30 74.99(16) . . ? O34 V13 O29 170.69(19) . 2_575 ? O33 V13 O29 82.23(16) . 2_575 ? O32 V13 O29 80.29(16) . 2_575 ? O31 V13 O29 74.96(15) . 2_575 ? O30 V13 O29 74.44(14) . 2_575 ? O34 V13 V14 140.56(17) . 2_575 ? O33 V13 V14 34.35(13) . 2_575 ? O32 V13 V14 83.36(13) . 2_575 ? O31 V13 V14 90.05(12) . 2_575 ? O30 V13 V14 122.91(11) . 2_575 ? O29 V13 V14 48.51(9) 2_575 2_575 ? O34 V13 V11 135.96(18) . 2_575 ? O33 V13 V11 78.89(14) . 2_575 ? O32 V13 V11 121.72(13) . 2_575 ? O31 V13 V11 35.57(11) . 2_575 ? O30 V13 V11 80.14(11) . 2_575 ? O29 V13 V11 41.43(10) 2_575 2_575 ? V14 V13 V11 59.87(4) 2_575 2_575 ? O41 V12 O38 106.1(2) . . ? O41 V12 O35 101.88(19) . . ? O38 V12 O35 96.40(19) . . ? O41 V12 O31 99.88(19) . . ? O38 V12 O31 95.75(18) . . ? O35 V12 O31 150.98(17) . . ? O41 V12 O30 97.07(19) . . ? O38 V12 O30 156.06(17) . . ? O35 V12 O30 84.22(17) . . ? O31 V12 O30 74.21(15) . . ? O41 V12 O29 170.07(19) . . ? O38 V12 O29 83.61(17) . . ? O35 V12 O29 78.40(15) . . ? O31 V12 O29 76.89(14) . . ? O30 V12 O29 73.04(14) . . ? O41 V12 V11 134.72(15) . 2_575 ? O38 V12 V11 80.09(14) . 2_575 ? O35 V12 V11 122.31(13) . 2_575 ? O31 V12 V11 35.37(11) . 2_575 ? O30 V12 V11 79.44(10) . 2_575 ? O29 V12 V11 43.91(9) . 2_575 ? O39 V15 O32 103.7(2) . 2_575 ? O39 V15 O37 104.4(2) . . ? O32 V15 O37 91.09(19) 2_575 . ? O39 V15 O38 101.7(2) . . ? O32 V15 O38 153.99(18) 2_575 . ? O37 V15 O38 87.77(17) . . ? O39 V15 O42 102.0(2) . 2_575 ? O32 V15 O42 87.33(18) 2_575 2_575 ? O37 V15 O42 153.21(18) . 2_575 ? O38 V15 O42 82.21(17) . 2_575 ? O39 V15 O29 175.5(2) . . ? O32 V15 O29 78.87(16) 2_575 . ? O37 V15 O29 79.16(16) . . ? O38 V15 O29 75.39(15) . . ? O42 V15 O29 74.29(14) 2_575 . ? O39 V15 V14 135.54(18) . . ? O32 V15 V14 83.26(14) 2_575 . ? O37 V15 V14 31.19(13) . . ? O38 V15 V14 82.39(12) . . ? O42 V15 V14 122.33(12) 2_575 . ? O29 V15 V14 48.04(9) . . ? O39 V15 V11 132.33(18) . 2_575 ? O32 V15 V11 81.96(14) 2_575 2_575 ? O37 V15 V11 123.02(14) . 2_575 ? O38 V15 V11 76.98(12) . 2_575 ? O42 V15 V11 30.37(11) 2_575 2_575 ? O29 V15 V11 43.93(9) . 2_575 ? V14 V15 V11 91.97(4) . 2_575 ? O40 V14 O37 104.8(2) . . ? O40 V14 O33 102.7(2) . 2_575 ? O37 V14 O33 92.88(19) . 2_575 ? O40 V14 O35 100.0(2) . . ? O37 V14 O35 92.32(18) . . ? O33 V14 O35 154.60(18) 2_575 . ? O40 V14 O36 99.6(2) . . ? O37 V14 O36 155.57(17) . . ? O33 V14 O36 82.59(18) 2_575 . ? O35 V14 O36 82.44(17) . . ? O40 V14 O29 171.7(2) . . ? O37 V14 O29 83.12(17) . . ? O33 V14 O29 79.08(16) 2_575 . ? O35 V14 O29 76.89(15) . . ? O36 V14 O29 72.45(14) . . ? O40 V14 V13 133.87(18) . 2_575 ? O37 V14 V13 83.53(14) . 2_575 ? O33 V14 V13 31.22(12) 2_575 2_575 ? O35 V14 V13 125.32(13) . 2_575 ? O36 V14 V13 80.24(11) . 2_575 ? O29 V14 V13 48.44(9) . 2_575 ? O40 V14 V11 130.31(19) . . ? O37 V14 V11 124.92(14) . . ? O33 V14 V11 77.66(13) 2_575 . ? O35 V14 V11 78.99(13) . . ? O36 V14 V11 30.66(10) . . ? O29 V14 V11 41.83(10) . . ? V13 V14 V11 60.66(4) 2_575 . ? O40 V14 V15 138.04(19) . . ? O37 V14 V15 33.28(13) . . ? O33 V14 V15 84.36(13) 2_575 . ? O35 V14 V15 86.46(13) . . ? O36 V14 V15 122.31(11) . . ? O29 V14 V15 49.91(10) . . ? V13 V14 V15 61.48(4) 2_575 . ? V11 V14 V15 91.65(4) . . ? V12 O41 Ba2 149.4(2) . 1_565 ? V13 O34 Ba2 148.6(2) . 1_565 ? V11 O30 V13 107.88(17) . . ? V11 O30 V12 105.19(17) . . ? V13 O30 V12 96.32(16) . . ? V15 O32 V13 115.6(2) 2_575 . ? V12 O35 V14 112.72(19) . . ? V11 O31 V12 107.95(18) 2_575 . ? V11 O31 V13 107.34(18) 2_575 . ? V12 O31 V13 107.33(18) . . ? V13 O33 V14 114.4(2) . 2_575 ? V12 O38 V15 116.3(2) . . ? V11 O29 V11 102.49(16) . 2_575 ? V11 O29 V12 100.00(15) . . ? V11 O29 V12 89.23(13) 2_575 . ? V11 O29 V13 90.42(15) . 2_575 ? V11 O29 V13 96.62(14) 2_575 2_575 ? V12 O29 V13 166.70(19) . 2_575 ? V11 O29 V14 89.45(14) . . ? V11 O29 V14 168.06(19) 2_575 . ? V12 O29 V14 88.77(13) . . ? V13 O29 V14 83.04(12) 2_575 . ? V11 O29 V15 170.35(19) . . ? V11 O29 V15 86.05(13) 2_575 . ? V12 O29 V15 84.43(13) . . ? V13 O29 V15 84.08(12) 2_575 . ? V14 O29 V15 82.04(13) . . ? V11 O42 V15 113.2(2) . 2_575 ? V11 O36 V14 108.8(2) . . ? V14 O37 V15 115.5(2) . . ? C46A O52 C46 35.4(11) . . ? C46 N10 C47 114.3(19) . . ? C46 N10 C49 118(2) . . ? C47 N10 C49 126.8(9) . . ? C47 C50 C51 102.1(7) . . ? O52 C46 N10 122(2) . . ? O52 C46 C51 128.8(13) . . ? N10 C46 C51 109(2) . . ? C49 C50A C47 109.1(17) . . ? C46A N10A C51 122(5) . . ? C46A N10A C47 121(4) . . ? C51 N10A C47 115.5(17) . . ? N10A C46A O52 117(5) . . ? N10A C46A C49 107(4) . . ? O52 C46A C49 136(2) . . ? C50A C49 N10 64.6(12) . . ? C50A C49 C46A 101.8(16) . . ? N10 C49 C46A 39.3(10) . . ? N10A C51 C46 33.3(13) . . ? N10A C51 C50 70.8(16) . . ? C46 C51 C50 101.1(8) . . ? N10 C47 N10A 39.9(8) . . ? N10 C47 C50 104.6(8) . . ? N10A C47 C50 68.8(10) . . ? N10 C47 C50A 57.8(11) . . ? N10A C47 C50A 95.2(14) . . ? C50 C47 C50A 162.2(12) . . ? C69A O53 C69 28.7(7) . . ? C69A O53 Ba1 124.2(8) . 2_556 ? C69 O53 Ba1 121.0(5) . 2_556 ? C69A O53 Ba1 123.0(7) . . ? C69 O53 Ba1 127.2(5) . . ? Ba1 O53 Ba1 109.80(14) 2_556 . ? C1 O43 Ba2 142.0(5) . 1_655 ? C1 N1 C5 127.0(10) . . ? C1 N1 C2 114.1(11) . . ? C5 N1 C2 118.7(10) . . ? C1 C4 C3 98.3(10) . . ? O43 C1 N1 122.9(13) . . ? O43 C1 C4 122.8(10) . . ? N1 C1 C4 114.3(11) . . ? C2 C3 C4 108.5(10) . . ? C3 C2 N1 104.6(10) . . ? C6 O44 Ba1 133.2(4) . . ? C6 N2 C10 124.5(5) . . ? C6 N2 C7 114.2(5) . . ? C10 N2 C7 121.3(5) . . ? C6 C9 C8 105.0(5) . . ? O44 C6 N2 125.8(6) . . ? O44 C6 C9 124.2(6) . . ? N2 C6 C9 110.0(5) . . ? C9 C8 C7 105.9(5) . . ? N2 C7 C8 104.4(5) . . ? C11 O45 Ba2 133.3(4) . . ? C11 N3 C15 124.8(5) . . ? C11 N3 C12 114.7(5) . . ? C15 N3 C12 120.4(5) . . ? O45 C11 N3 124.9(6) . . ? O45 C11 C14 125.4(6) . . ? N3 C11 C14 109.7(6) . . ? C11 C14 C13 105.0(5) . . ? N3 C12 C13 104.1(5) . . ? C14 C13 C12 105.9(5) . . ? C16 O46 Ba1 152.7(4) . 2_666 ? C16 N4 C20 124.4(6) . . ? C16 N4 C17 114.7(6) . . ? C20 N4 C17 120.8(6) . . ? N4 C17 C18 104.7(5) . . ? C17 C18 C19 105.4(6) . . ? C16 C19 C18 105.0(6) . . ? O46 C16 N4 125.8(7) . . ? O46 C16 C19 124.4(6) . . ? N4 C16 C19 109.8(6) . . ? C21 N5 C22 114.8(6) . . ? C21 N5 C25 125.2(6) . . ? C22 N5 C25 120.0(6) . . ? N5 C22 C23 103.1(7) . . ? C24 C23 C22 107.5(9) . . ? C21 C24 C23 105.0(8) . . ? O47 C21 N5 124.4(7) . . ? O47 C21 C24 126.1(7) . . ? N5 C21 C24 109.5(7) . . ? C26 N6 C30 124.1(5) . . ? C26 N6 C27 113.0(5) . . ? C30 N6 C27 122.5(5) . . ? O48 C26 N6 123.5(6) . . ? O48 C26 C29 127.1(6) . . ? N6 C26 C29 109.4(5) . . ? C27 C28 C29 104.3(5) . . ? C26 C29 C28 105.5(5) . . ? C61 O51 Ba1 123.3(4) . 2_656 ? C31 N7 C32 113.7(6) . . ? C31 N7 C35 124.5(7) . . ? C32 N7 C35 121.4(7) . . ? N7 C32 C33 104.2(6) . . ? O49 C31 N7 124.2(7) . . ? O49 C31 C34 126.5(6) . . ? N7 C31 C34 109.2(6) . . ? C32 C33 C34 102.7(6) . . ? C31 C34 C33 105.7(6) . . ? C36 O50 Ba2 128.5(4) . . ? C36 N8 C40 124.0(6) . . ? C36 N8 C37 114.1(6) . . ? C40 N8 C37 121.4(6) . . ? O50 C36 N8 125.4(7) . . ? O50 C36 C39 126.7(7) . . ? N8 C36 C39 107.9(6) . . ? C36 C39 C38 104.9(6) . . ? C39 C38 C37 103.2(6) . . ? N8 C37 C38 102.2(6) . . ? O46 Ba1 O44 147.68(13) 2_666 . ? O46 Ba1 O53 73.71(13) 2_666 2_556 ? O44 Ba1 O53 137.92(12) . 2_556 ? O46 Ba1 O53 143.72(12) 2_666 . ? O44 Ba1 O53 68.55(12) . . ? O53 Ba1 O53 70.20(14) 2_556 . ? O46 Ba1 O54 98.91(14) 2_666 . ? O44 Ba1 O54 96.45(14) . . ? O53 Ba1 O54 76.20(12) 2_556 . ? O53 Ba1 O54 69.12(12) . . ? O46 Ba1 O51 87.25(15) 2_666 2_656 ? O44 Ba1 O51 94.61(14) . 2_656 ? O53 Ba1 O51 75.42(12) 2_556 2_656 ? O53 Ba1 O51 87.30(12) . 2_656 ? O54 Ba1 O51 147.90(12) . 2_656 ? O46 Ba1 O19 77.60(13) 2_666 2_666 ? O44 Ba1 O19 77.47(12) . 2_666 ? O53 Ba1 O19 138.62(11) 2_556 2_666 ? O53 Ba1 O19 129.75(12) . 2_666 ? O54 Ba1 O19 79.54(11) . 2_666 ? O51 Ba1 O19 132.38(11) 2_656 2_666 ? O46 Ba1 O25 78.61(13) 2_666 2_666 ? O44 Ba1 O25 71.98(12) . 2_666 ? O53 Ba1 O25 135.81(12) 2_556 2_666 ? O53 Ba1 O25 131.88(11) . 2_666 ? O54 Ba1 O25 142.65(11) . 2_666 ? O51 Ba1 O25 69.44(11) 2_656 2_666 ? O19 Ba1 O25 63.43(11) 2_666 2_666 ? O46 Ba1 Ba1 108.92(9) 2_666 2_556 ? O44 Ba1 Ba1 103.13(9) . 2_556 ? O53 Ba1 Ba1 35.28(8) 2_556 2_556 ? O53 Ba1 Ba1 34.93(8) . 2_556 ? O54 Ba1 Ba1 68.66(9) . 2_556 ? O51 Ba1 Ba1 79.51(9) 2_656 2_556 ? O19 Ba1 Ba1 148.11(8) 2_666 2_556 ? O25 Ba1 Ba1 147.79(7) 2_666 2_556 ? O45 Ba2 O43 77.61(17) . 1_455 ? O45 Ba2 O57 140.4(2) . . ? O43 Ba2 O57 133.4(2) 1_455 . ? O45 Ba2 O50 85.73(14) . . ? O43 Ba2 O50 148.18(19) 1_455 . ? O57 Ba2 O50 75.1(2) . . ? O45 Ba2 O27 76.46(12) . . ? O43 Ba2 O27 73.77(15) 1_455 . ? O57 Ba2 O27 88.8(3) . . ? O50 Ba2 O27 128.45(12) . . ? O45 Ba2 O41 75.14(13) . 1_545 ? O43 Ba2 O41 80.88(17) 1_455 1_545 ? O57 Ba2 O41 126.0(3) . 1_545 ? O50 Ba2 O41 68.64(13) . 1_545 ? O27 Ba2 O41 145.23(12) . 1_545 ? O45 Ba2 O34 129.19(13) . 1_545 ? O43 Ba2 O34 66.69(15) 1_455 1_545 ? O57 Ba2 O34 89.7(3) . 1_545 ? O50 Ba2 O34 106.06(13) . 1_545 ? O27 Ba2 O34 122.77(12) . 1_545 ? O41 Ba2 O34 64.78(12) 1_545 1_545 ? O45 Ba2 O55 138.02(15) . . ? O43 Ba2 O55 72.4(2) 1_455 . ? O57 Ba2 O55 61.1(2) . . ? O50 Ba2 O55 133.71(16) . . ? O27 Ba2 O55 67.50(15) . . ? O41 Ba2 O55 126.46(14) 1_545 . ? O34 Ba2 O55 62.19(14) 1_545 . ? O45 Ba2 O28 70.71(12) . . ? O43 Ba2 O28 130.79(14) 1_455 . ? O57 Ba2 O28 69.9(2) . . ? O50 Ba2 O28 65.49(12) . . ? O27 Ba2 O28 62.98(11) . . ? O41 Ba2 O28 123.71(11) 1_545 . ? O34 Ba2 O28 159.15(12) 1_545 . ? O55 Ba2 O28 108.72(14) . . ? O51 C61 N13A 152.7(13) . . ? O51 C61 N13 147.0(11) . . ? N13A C61 N13 60.0(11) . . ? O51 C61 C64A 110.5(12) . . ? N13A C61 C64A 96.7(15) . . ? N13 C61 C64A 36.8(11) . . ? O51 C61 C64 113.3(9) . . ? N13A C61 C64 39.6(11) . . ? N13 C61 C64 99.6(11) . . ? C64A C61 C64 136.0(14) . . ? N13A C62 N13 51.4(10) . . ? N13A C62 C63A 104.2(14) . . ? N13 C62 C63A 54.0(12) . . ? N13A C62 C63 53.6(11) . . ? N13 C62 C63 104.0(10) . . ? C63A C62 C63 157.8(12) . . ? N12 C68 N12A 44.2(7) . . ? N12 C68 C67 101.5(6) . . ? N12A C68 C67 59.9(7) . . ? N12 C68 C67A 53.8(7) . . ? N12A C68 C67A 94.9(9) . . ? C67 C68 C67A 154.7(8) . . ? N12A C70 C67 68.3(9) . . ? N12A C70 C69 38.1(7) . . ? C67 C70 C69 103.8(8) . . ? C67A C66 N12 63.6(9) . . ? C67A C66 C69A 99.3(10) . . ? N12 C66 C69A 39.2(7) . . ? N6 C27 C28 103.7(5) . . ? C69 N12 C66 115.2(10) . . ? C69 N12 C68 115.2(10) . . ? C66 N12 C68 129.1(8) . . ? C70 C67 C68 105.2(8) . . ? O53 C69 N12 124.2(12) . . ? O53 C69 C70 128.8(9) . . ? N12 C69 C70 107.0(11) . . ? C66 C67A C68 111.0(11) . . ? C69A N12A C70 114.5(15) . . ? C69A N12A C68 121.3(14) . . ? C70 N12A C68 124.1(13) . . ? O53 C69A N12A 127.8(17) . . ? O53 C69A C66 127.0(12) . . ? N12A C69A C66 105.0(14) . . ? C61 N13 C62 121.9(13) . . ? C61 N13 C65 109.5(13) . . ? C62 N13 C65 127.3(14) . . ? C64 C63 C62 104.3(14) . . ? C63 C64 C61 104.9(15) . . ? C61 N13A C62 125.6(18) . . ? C61 N13A C65A 107(2) . . ? C62 N13A C65A 127(2) . . ? C64A C63A C62 100.2(18) . . ? C63A C64A C61 111.1(19) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.940 _refine_diff_density_min -1.586 _refine_diff_density_rms 0.137 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.500 0.633 0.000 429 50 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 928366' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_publication_text # Attachment '18394_web_deposit_cif_file_1_CarstenStreb_1362733185.CS1217_HugoDMF.cif' data_p-1a _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H54 Ba2 N8 O36 V10' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour yellow-orange _diffrn_ambient_temperature 150(2) _chemical_formula_weight 1814.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 '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_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.340(2) _cell_length_b 11.638(2) _cell_length_c 12.492(3) _cell_angle_alpha 104.74(3) _cell_angle_beta 103.04(3) _cell_angle_gamma 107.93(3) _cell_volume 1431.8(5) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 368 _cell_measurement_theta_min 6.7 _cell_measurement_theta_max 23.1 _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 2.999 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.931 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius-Kappa CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34583 _diffrn_reflns_av_R_equivalents 0.1061 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 5.82 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5789 _reflns_number_gt 4323 _reflns_threshold_expression >2\s(I) _computing_data_collection SUPERGUI _computing_cell_refinement SUPERGUI _computing_data_reduction SUPERGUI _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+5.4115P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5789 _refine_ls_number_parameters 436 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1261 _refine_ls_wR_factor_gt 0.1138 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9191(13) 0.5939(13) 0.2155(12) 0.048(4) Uani 0.587(14) 1 d P A 1 H1 H 1.0015 0.6108 0.2658 0.057 Uiso 0.587(14) 1 calc PR A 1 C2 C 0.9339(16) 0.4045(15) 0.0916(13) 0.053(4) Uani 0.587(14) 1 d P A 1 H2A H 0.8812 0.3375 0.0173 0.080 Uiso 0.587(14) 1 calc PR A 1 H2B H 0.9454 0.3670 0.1514 0.080 Uiso 0.587(14) 1 calc PR A 1 H2C H 1.0181 0.4509 0.0878 0.080 Uiso 0.587(14) 1 calc PR A 1 C3 C 0.736(2) 0.458(3) 0.038(2) 0.099(9) Uani 0.587(14) 1 d P A 1 H3A H 0.7153 0.3827 -0.0282 0.148 Uiso 0.587(14) 1 calc PR A 1 H3B H 0.7347 0.5282 0.0106 0.148 Uiso 0.587(14) 1 calc PR A 1 H3C H 0.6725 0.4412 0.0768 0.148 Uiso 0.587(14) 1 calc PR A 1 N1 N 0.8682(11) 0.4933(10) 0.1198(10) 0.045(3) Uani 0.587(14) 1 d P A 1 C4 C 0.854(4) 0.567(3) 0.026(3) 0.099(13) Uani 0.413(14) 1 d P A 2 H4A H 0.8288 0.5097 -0.0533 0.148 Uiso 0.413(14) 1 calc PR A 2 H4B H 0.9158 0.5482 0.0771 0.148 Uiso 0.413(14) 1 calc PR A 2 H4C H 0.8928 0.6545 0.0295 0.148 Uiso 0.413(14) 1 calc PR A 2 C5 C 0.610(4) 0.460(3) -0.025(2) 0.116(15) Uani 0.413(14) 1 d P A 2 H5A H 0.6256 0.4207 -0.0951 0.174 Uiso 0.413(14) 1 calc PR A 2 H5B H 0.5544 0.5054 -0.0423 0.174 Uiso 0.413(14) 1 calc PR A 2 H5C H 0.5681 0.3950 0.0034 0.174 Uiso 0.413(14) 1 calc PR A 2 C6 C 0.746(3) 0.619(2) 0.1696(19) 0.060(7) Uani 0.413(14) 1 d P A 2 H6 H 0.6711 0.6227 0.1870 0.072 Uiso 0.413(14) 1 calc PR A 2 N1A N 0.733(3) 0.5497(19) 0.0630(15) 0.072(7) Uani 0.413(14) 1 d P A 2 C8 C 0.6562(19) 0.977(2) 0.0468(16) 0.086(7) Uani 0.613(14) 1 d P B 1 H8A H 0.5704 0.9483 -0.0090 0.129 Uiso 0.613(14) 1 calc PR B 1 H8B H 0.6605 0.9111 0.0795 0.129 Uiso 0.613(14) 1 calc PR B 1 H8C H 0.7208 0.9925 0.0084 0.129 Uiso 0.613(14) 1 calc PR B 1 C9 C 0.579(2) 1.147(3) 0.140(3) 0.128(12) Uani 0.613(14) 1 d P B 1 H9A H 0.5054 1.0922 0.0699 0.192 Uiso 0.613(14) 1 calc PR B 1 H9B H 0.6092 1.2332 0.1395 0.192 Uiso 0.613(14) 1 calc PR B 1 H9C H 0.5516 1.1458 0.2073 0.192 Uiso 0.613(14) 1 calc PR B 1 N2 N 0.6832(13) 1.1000(17) 0.1444(15) 0.075(5) Uani 0.613(14) 1 d P B 1 C10 C 0.6747(19) 1.246(2) 0.126(2) 0.046(6) Uani 0.387(14) 1 d P B 2 H10A H 0.6825 1.3146 0.0954 0.069 Uiso 0.387(14) 1 calc PR B 2 H10B H 0.6262 1.2515 0.1795 0.069 Uiso 0.387(14) 1 calc PR B 2 H10C H 0.6295 1.1645 0.0625 0.069 Uiso 0.387(14) 1 calc PR B 2 C11 C 0.9175(18) 1.3594(18) 0.1876(19) 0.037(5) Uani 0.387(14) 1 d P B 2 H11A H 0.8875 1.4111 0.1482 0.056 Uiso 0.387(14) 1 calc PR B 2 H11B H 0.9679 1.3231 0.1479 0.056 Uiso 0.387(14) 1 calc PR B 2 H11C H 0.9714 1.4122 0.2671 0.056 Uiso 0.387(14) 1 calc PR B 2 N2A N 0.8047(14) 1.2559(13) 0.1869(12) 0.027(4) Uani 0.387(14) 1 d P B 2 C7 C 0.8023(12) 1.1573(10) 0.2347(9) 0.064(3) Uani 1 1 d . . . C12 C 0.8980(13) 0.8370(13) -0.0109(11) 0.044(4) Uani 0.62(2) 1 d P A 1 H12 H 0.9829 0.8567 -0.0138 0.053 Uiso 0.62(2) 1 calc PR A 1 C12A C 0.751(2) 0.815(2) 0.006(2) 0.053(7) Uani 0.38(2) 1 d P A 2 H12A H 0.6710 0.8078 0.0171 0.063 Uiso 0.38(2) 1 calc PR A 2 C13 C 1.1336(6) 1.2775(7) 0.5010(6) 0.0316(15) Uani 1 1 d . . . H13 H 1.0488 1.2690 0.4991 0.038 Uiso 1 1 calc R . . C14 C 1.1840(9) 1.5070(8) 0.5598(9) 0.052(2) Uani 1 1 d . . . H14A H 1.2582 1.5843 0.5762 0.078 Uiso 1 1 calc R . . H14B H 1.1580 1.5112 0.6282 0.078 Uiso 1 1 calc R . . H14C H 1.1124 1.4986 0.4961 0.078 Uiso 1 1 calc R . . C15 C 1.3562(8) 1.4195(8) 0.5355(8) 0.047(2) Uani 1 1 d . . . H15A H 1.4036 1.5102 0.5555 0.071 Uiso 1 1 calc R . . H15B H 1.3596 1.3734 0.4614 0.071 Uiso 1 1 calc R . . H15C H 1.3952 1.3912 0.5949 0.071 Uiso 1 1 calc R . . C16 C 0.651(2) 0.7020(18) -0.154(2) 0.165(10) Uani 1 1 d . A . H16A H 0.6213 0.6941 -0.0892 0.248 Uiso 1 1 calc R . . H16B H 0.6367 0.6182 -0.2048 0.248 Uiso 1 1 calc R . . H16C H 0.6027 0.7401 -0.1972 0.248 Uiso 1 1 calc R . . C17 C 0.8375(15) 0.7986(15) -0.1975(19) 0.127(7) Uani 1 1 d . A . H17A H 0.9292 0.8530 -0.1625 0.190 Uiso 1 1 calc R . . H17B H 0.7927 0.8386 -0.2411 0.190 Uiso 1 1 calc R . . H17C H 0.8271 0.7168 -0.2492 0.190 Uiso 1 1 calc R . . N4 N 1.2200(5) 1.3946(5) 0.5274(5) 0.0298(12) Uani 1 1 d . . . N5 N 0.7861(14) 0.7808(8) -0.1121(6) 0.092(4) Uani 1 1 d . . . O2 O 1.1197(4) 0.9196(4) 0.5099(4) 0.0237(9) Uani 1 1 d . . . O3 O 1.3543(4) 1.0969(4) 0.5156(3) 0.0196(8) Uani 1 1 d . . . O4 O 1.3745(4) 0.9367(4) 0.6093(3) 0.0214(9) Uani 1 1 d . A . O5 O 1.1986(4) 0.7321(4) 0.4149(4) 0.0260(9) Uani 1 1 d . A . O6 O 1.4112(4) 0.9064(4) 0.4060(3) 0.0190(8) Uani 1 1 d . . . O7 O 1.4313(4) 0.7329(4) 0.5046(4) 0.0258(9) Uani 1 1 d . . . O8 O 1.3876(4) 1.0724(4) 0.3007(4) 0.0250(9) Uani 1 1 d . . . O9 O 0.6728(4) 0.8635(5) 0.2596(4) 0.0315(11) Uani 1 1 d . . . O10 O 1.4361(4) 0.8773(4) 0.1913(4) 0.0271(10) Uani 1 1 d . . . O11 O 1.1754(4) 0.9088(4) 0.3148(4) 0.0213(9) Uani 1 1 d . A . O12 O 1.2502(5) 0.5258(4) 0.3002(4) 0.0361(11) Uani 1 1 d . . . O13 O 1.4617(4) 0.7058(4) 0.2946(4) 0.0283(10) Uani 1 1 d . . . O14 O 1.1554(4) 1.1773(4) 0.4786(5) 0.0392(12) Uani 1 1 d . . . O15 O 1.2270(4) 0.7099(4) 0.2068(4) 0.0278(10) Uani 1 1 d . . . O16 O 1.1905(5) 0.8749(5) 0.0958(4) 0.0332(11) Uani 1 1 d . . . O18 O 0.8562(7) 0.6798(6) 0.2482(6) 0.0636(18) Uani 1 1 d . . . O19 O 0.9014(8) 1.1366(8) 0.2641(6) 0.076(2) Uani 1 1 d . A . O26 O 0.8735(9) 0.8584(11) 0.0835(5) 0.127(4) Uani 1 1 d . . . V3 V 1.27362(10) 0.87686(11) 0.21958(9) 0.0240(2) Uani 1 1 d . . . V4 V 1.44687(10) 1.12604(10) 0.69290(9) 0.0234(2) Uani 1 1 d . . . V5 V 1.50804(10) 0.89475(9) 0.56613(9) 0.0199(2) Uani 1 1 d . . . V6 V 1.31484(10) 0.67950(10) 0.33349(10) 0.0261(3) Uani 1 1 d . . . V10 V 1.23513(10) 0.89569(10) 0.45971(9) 0.0201(2) Uani 1 1 d . . . Ba1 Ba 0.94465(4) 0.93776(4) 0.31392(3) 0.02947(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.030(7) 0.032(8) 0.054(8) -0.008(6) 0.007(6) 0.003(6) C2 0.059(10) 0.047(9) 0.046(8) 0.002(7) 0.007(7) 0.029(8) C3 0.063(13) 0.11(2) 0.084(15) -0.014(14) -0.005(11) 0.047(14) N1 0.048(7) 0.028(6) 0.047(7) 0.002(5) 0.014(5) 0.011(5) C4 0.19(4) 0.10(3) 0.10(2) 0.08(2) 0.11(3) 0.11(3) C5 0.18(4) 0.054(17) 0.055(16) 0.032(14) -0.019(19) 0.003(19) C6 0.12(2) 0.041(13) 0.048(12) 0.028(11) 0.042(15) 0.049(15) N1A 0.15(2) 0.034(11) 0.034(9) 0.011(8) 0.019(12) 0.043(13) C8 0.073(12) 0.15(2) 0.059(10) 0.050(13) 0.028(9) 0.058(14) C9 0.074(13) 0.18(3) 0.25(3) 0.18(3) 0.095(18) 0.090(16) N2 0.057(9) 0.115(13) 0.118(13) 0.097(12) 0.051(9) 0.057(9) C10 0.030(11) 0.047(13) 0.056(13) 0.016(11) 0.010(9) 0.013(10) C11 0.034(10) 0.032(11) 0.063(13) 0.027(10) 0.022(9) 0.020(9) N2A 0.035(8) 0.021(8) 0.028(8) 0.017(6) 0.010(6) 0.009(6) C7 0.091(8) 0.053(6) 0.069(6) 0.034(5) 0.031(6) 0.044(6) C12 0.036(7) 0.054(9) 0.043(8) 0.014(6) 0.007(6) 0.025(6) C12A 0.048(14) 0.050(15) 0.058(15) 0.009(12) 0.022(12) 0.021(11) C13 0.021(3) 0.026(4) 0.045(4) 0.009(3) 0.009(3) 0.010(3) C14 0.054(5) 0.027(4) 0.089(7) 0.022(4) 0.035(5) 0.024(4) C15 0.039(4) 0.029(4) 0.073(6) 0.019(4) 0.016(4) 0.012(3) C16 0.151(16) 0.106(13) 0.32(3) 0.085(17) 0.18(2) 0.071(13) C17 0.110(11) 0.098(11) 0.24(2) 0.120(13) 0.081(13) 0.067(10) N4 0.027(3) 0.022(3) 0.042(3) 0.011(3) 0.012(3) 0.010(2) N5 0.169(11) 0.040(5) 0.026(4) 0.006(4) -0.006(5) 0.019(6) O2 0.020(2) 0.022(2) 0.027(2) 0.0070(18) 0.0058(18) 0.0071(18) O3 0.018(2) 0.014(2) 0.022(2) 0.0013(17) 0.0025(17) 0.0068(17) O4 0.020(2) 0.020(2) 0.024(2) 0.0089(18) 0.0049(17) 0.0089(18) O5 0.021(2) 0.016(2) 0.035(2) 0.0068(19) 0.0024(19) 0.0059(18) O6 0.0154(19) 0.012(2) 0.024(2) 0.0029(17) 0.0007(16) 0.0044(16) O7 0.026(2) 0.018(2) 0.034(2) 0.0110(19) 0.0068(19) 0.0104(19) O8 0.023(2) 0.027(2) 0.026(2) 0.0106(19) 0.0051(18) 0.0123(19) O9 0.017(2) 0.036(3) 0.034(2) 0.005(2) 0.0035(19) 0.010(2) O10 0.024(2) 0.032(3) 0.024(2) 0.0081(19) 0.0051(18) 0.012(2) O11 0.016(2) 0.020(2) 0.027(2) 0.0088(18) 0.0043(17) 0.0085(17) O12 0.034(3) 0.013(2) 0.051(3) 0.003(2) 0.007(2) 0.008(2) O13 0.023(2) 0.019(2) 0.034(2) 0.0013(19) 0.0020(19) 0.0103(19) O14 0.023(2) 0.018(2) 0.065(3) 0.005(2) 0.002(2) 0.008(2) O15 0.023(2) 0.023(2) 0.031(2) 0.0016(19) 0.0048(19) 0.0091(19) O16 0.030(2) 0.042(3) 0.025(2) 0.010(2) 0.002(2) 0.017(2) O18 0.056(4) 0.044(4) 0.055(4) -0.001(3) 0.008(3) -0.004(3) O19 0.101(6) 0.112(6) 0.084(5) 0.071(5) 0.050(4) 0.087(5) O26 0.106(7) 0.185(11) 0.018(3) 0.011(5) -0.001(4) -0.002(7) V3 0.0193(5) 0.0259(6) 0.0238(5) 0.0065(4) 0.0028(4) 0.0097(5) V4 0.0195(5) 0.0226(6) 0.0239(5) 0.0030(4) 0.0036(4) 0.0093(4) V5 0.0193(5) 0.0146(5) 0.0253(5) 0.0081(4) 0.0039(4) 0.0074(4) V6 0.0231(5) 0.0138(5) 0.0337(6) 0.0014(5) 0.0030(5) 0.0074(4) V10 0.0176(5) 0.0153(5) 0.0256(5) 0.0058(4) 0.0044(4) 0.0070(4) Ba1 0.0230(2) 0.0384(3) 0.0256(2) 0.00581(17) 0.00345(15) 0.01776(18) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.301(16) . ? C1 O18 1.428(15) . ? C2 N1 1.468(17) . ? C3 N1 1.48(2) . ? C4 N1A 1.51(4) . ? C5 N1A 1.44(4) . ? C6 O18 1.26(3) . ? C6 N1A 1.32(3) . ? C6 Ba1 3.42(2) . ? C8 N2 1.52(3) . ? C9 N2 1.44(2) . ? N2 C7 1.384(19) . ? C10 N2A 1.45(2) . ? C11 N2A 1.46(2) . ? N2A C7 1.418(15) . ? C7 O19 1.217(11) . ? C12 O26 1.253(15) . ? C12 N5 1.408(15) . ? C12A O26 1.36(2) . ? C12A N5 1.59(3) . ? C13 O14 1.243(8) . ? C13 N4 1.315(9) . ? C14 N4 1.475(9) . ? C15 N4 1.456(9) . ? C16 N5 1.41(2) . ? C17 N5 1.356(18) . ? O2 V10 1.640(4) . ? O2 Ba1 2.783(4) 2_776 ? O2 Ba1 2.882(4) . ? O3 V5 2.041(4) 2_876 ? O3 V4 2.115(4) . ? O3 V10 2.142(4) . ? O4 V5 1.875(4) . ? O4 V4 1.987(4) . ? O4 V10 1.991(4) . ? O5 V10 1.725(4) . ? O5 V6 1.983(4) . ? O6 V5 2.111(4) 2_876 ? O6 V5 2.113(4) . ? O6 V10 2.224(4) . ? O6 V4 2.301(4) 2_876 ? O6 V6 2.355(4) . ? O6 V3 2.366(4) . ? O7 V5 1.688(4) . ? O7 V6 2.060(4) . ? O8 V5 1.680(4) 2_876 ? O8 V3 2.074(5) . ? O9 V4 1.625(4) 2_776 ? O9 Ba1 2.797(4) . ? O10 V4 1.747(4) 2_876 ? O10 V3 1.951(4) . ? O11 V10 1.847(4) . ? O11 V3 1.850(4) . ? O11 Ba1 2.737(4) . ? O12 V6 1.608(5) . ? O13 V6 1.798(5) . ? O13 V4 1.858(5) 2_876 ? O14 Ba1 2.911(5) . ? O15 V3 1.804(5) . ? O15 V6 1.847(5) . ? O16 V3 1.610(4) . ? O18 Ba1 2.686(7) . ? O19 Ba1 2.698(6) . ? O26 Ba1 2.632(6) . ? V3 V6 3.0892(17) . ? V3 V10 3.0906(16) . ? V3 V5 3.114(2) 2_876 ? V4 O9 1.625(4) 2_776 ? V4 O10 1.747(4) 2_876 ? V4 O13 1.858(5) 2_876 ? V4 O6 2.301(4) 2_876 ? V4 V6 3.090(2) 2_876 ? V4 V5 3.1161(17) . ? V5 O8 1.680(4) 2_876 ? V5 O3 2.041(4) 2_876 ? V5 O6 2.111(4) 2_876 ? V5 V10 3.0850(16) . ? V5 V6 3.093(2) . ? V5 V3 3.114(2) 2_876 ? V6 V4 3.0901(19) 2_876 ? V6 V10 3.1078(16) . ? V10 Ba1 3.6258(15) . ? Ba1 O2 2.783(4) 2_776 ? Ba1 Ba1 4.2553(16) 2_776 ? 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 N1 C1 O18 124.1(12) . . ? C1 N1 C2 122.4(12) . . ? C1 N1 C3 120.9(13) . . ? C2 N1 C3 116.6(13) . . ? O18 C6 N1A 121(2) . . ? O18 C6 Ba1 45.0(8) . . ? N1A C6 Ba1 125.5(17) . . ? C6 N1A C5 124(3) . . ? C6 N1A C4 119(3) . . ? C5 N1A C4 116(3) . . ? C7 N2 C9 124(2) . . ? C7 N2 C8 118.9(11) . . ? C9 N2 C8 117.2(19) . . ? C7 N2A C10 113.2(14) . . ? C7 N2A C11 129.1(13) . . ? C10 N2A C11 117.7(14) . . ? O19 C7 N2 137.9(11) . . ? O19 C7 N2A 119.7(11) . . ? N2 C7 N2A 78.0(9) . . ? O26 C12 N5 114.3(12) . . ? O26 C12A N5 98.1(15) . . ? O14 C13 N4 125.7(6) . . ? C13 N4 C15 121.8(6) . . ? C13 N4 C14 120.4(6) . . ? C15 N4 C14 117.5(6) . . ? C17 N5 C12 102.8(14) . . ? C17 N5 C16 114.1(14) . . ? C12 N5 C16 142.3(15) . . ? C17 N5 C12A 159.3(14) . . ? C12 N5 C12A 67.6(11) . . ? C16 N5 C12A 79.6(15) . . ? V10 O2 Ba1 147.8(2) . 2_776 ? V10 O2 Ba1 103.16(19) . . ? Ba1 O2 Ba1 97.36(12) 2_776 . ? V5 O3 V4 107.36(17) 2_876 . ? V5 O3 V10 104.78(17) 2_876 . ? V4 O3 V10 98.12(17) . . ? V5 O4 V4 107.6(2) . . ? V5 O4 V10 105.8(2) . . ? V4 O4 V10 107.89(19) . . ? V10 O5 V6 113.7(2) . . ? V5 O6 V5 103.24(17) 2_876 . ? V5 O6 V10 99.73(16) 2_876 . ? V5 O6 V10 90.66(16) . . ? V5 O6 V4 89.76(16) 2_876 2_876 ? V5 O6 V4 98.60(15) . 2_876 ? V10 O6 V4 164.92(19) . 2_876 ? V5 O6 V6 168.0(2) 2_876 . ? V5 O6 V6 87.41(15) . . ? V10 O6 V6 85.43(14) . . ? V4 O6 V6 83.14(13) 2_876 . ? V5 O6 V3 87.96(15) 2_876 . ? V5 O6 V3 168.5(2) . . ? V10 O6 V3 84.60(13) . . ? V4 O6 V3 84.05(13) 2_876 . ? V6 O6 V3 81.74(13) . . ? V5 O7 V6 110.8(2) . . ? V5 O8 V3 111.7(2) 2_876 . ? V4 O9 Ba1 146.4(2) 2_776 . ? V4 O10 V3 115.2(2) 2_876 . ? V10 O11 V3 113.5(2) . . ? V10 O11 Ba1 102.83(17) . . ? V3 O11 Ba1 142.9(2) . . ? V6 O13 V4 115.4(2) . 2_876 ? C13 O14 Ba1 118.8(4) . . ? V3 O15 V6 115.6(2) . . ? C6 O18 C1 99.5(12) . . ? C6 O18 Ba1 115.7(10) . . ? C1 O18 Ba1 130.5(7) . . ? C7 O19 Ba1 132.8(7) . . ? C12 O26 C12A 79.8(12) . . ? C12 O26 Ba1 152.4(9) . . ? C12A O26 Ba1 127.8(11) . . ? O16 V3 O15 105.2(2) . . ? O16 V3 O11 103.2(2) . . ? O15 V3 O11 93.9(2) . . ? O16 V3 O10 101.1(2) . . ? O15 V3 O10 89.6(2) . . ? O11 V3 O10 153.53(18) . . ? O16 V3 O8 100.4(2) . . ? O15 V3 O8 154.05(18) . . ? O11 V3 O8 84.50(18) . . ? O10 V3 O8 81.07(18) . . ? O16 V3 O6 173.0(2) . . ? O15 V3 O6 81.60(17) . . ? O11 V3 O6 77.57(16) . . ? O10 V3 O6 77.00(16) . . ? O8 V3 O6 72.74(15) . . ? O16 V3 V6 137.75(19) . . ? O15 V3 V6 32.64(14) . . ? O11 V3 V6 87.31(13) . . ? O10 V3 V6 81.56(14) . . ? O8 V3 V6 121.51(12) . . ? O6 V3 V6 48.99(10) . . ? O16 V3 V10 136.08(17) . . ? O15 V3 V10 80.36(15) . . ? O11 V3 V10 33.24(12) . . ? O10 V3 V10 122.64(13) . . ? O8 V3 V10 84.41(13) . . ? O6 V3 V10 45.75(10) . . ? V6 V3 V10 60.38(4) . . ? O16 V3 V5 130.44(19) . 2_876 ? O15 V3 V5 124.09(15) . 2_876 ? O11 V3 V5 80.08(13) . 2_876 ? O10 V3 V5 76.31(13) . 2_876 ? O8 V3 V5 30.10(11) . 2_876 ? O6 V3 V5 42.64(10) . 2_876 ? V6 V3 V5 91.46(5) . 2_876 ? V10 V3 V5 64.58(4) . 2_876 ? O9 V4 O10 106.1(2) 2_776 2_876 ? O9 V4 O13 103.2(2) 2_776 2_876 ? O10 V4 O13 96.5(2) 2_876 2_876 ? O9 V4 O4 99.0(2) 2_776 . ? O10 V4 O4 94.0(2) 2_876 . ? O13 V4 O4 151.64(19) 2_876 . ? O9 V4 O3 97.6(2) 2_776 . ? O10 V4 O3 155.08(18) 2_876 . ? O13 V4 O3 85.41(18) 2_876 . ? O4 V4 O3 74.33(16) . . ? O9 V4 O6 170.06(19) 2_776 2_876 ? O10 V4 O6 82.72(17) 2_876 2_876 ? O13 V4 O6 79.92(17) 2_876 2_876 ? O4 V4 O6 75.38(16) . 2_876 ? O3 V4 O6 73.12(14) . 2_876 ? O9 V4 V6 134.84(18) 2_776 2_876 ? O10 V4 V6 84.59(16) 2_876 2_876 ? O13 V4 V6 31.71(13) 2_876 2_876 ? O4 V4 V6 124.35(13) . 2_876 ? O3 V4 V6 84.22(13) . 2_876 ? O6 V4 V6 49.18(10) 2_876 2_876 ? O9 V4 V5 133.46(18) 2_776 . ? O10 V4 V5 78.70(15) 2_876 . ? O13 V4 V5 122.55(14) 2_876 . ? O4 V4 V5 35.00(12) . . ? O3 V4 V5 79.40(11) . . ? O6 V4 V5 42.64(10) 2_876 . ? V6 V4 V5 91.41(5) 2_876 . ? O8 V5 O7 107.1(2) 2_876 . ? O8 V5 O4 99.93(19) 2_876 . ? O7 V5 O4 100.3(2) . . ? O8 V5 O3 94.81(19) 2_876 2_876 ? O7 V5 O3 93.75(19) . 2_876 ? O4 V5 O3 155.55(17) . 2_876 ? O8 V5 O6 87.64(19) 2_876 2_876 ? O7 V5 O6 164.06(19) . 2_876 ? O4 V5 O6 82.48(17) . 2_876 ? O3 V5 O6 78.74(16) 2_876 2_876 ? O8 V5 O6 164.0(2) 2_876 . ? O7 V5 O6 88.03(18) . . ? O4 V5 O6 81.87(16) . . ? O3 V5 O6 78.72(16) 2_876 . ? O6 V5 O6 76.76(17) 2_876 . ? O8 V5 V10 138.27(15) 2_876 . ? O7 V5 V10 84.82(15) . . ? O4 V5 V10 38.39(12) . . ? O3 V5 V10 124.82(12) 2_876 . ? O6 V5 V10 87.99(11) 2_876 . ? O6 V5 V10 46.11(11) . . ? O8 V5 V6 145.30(16) 2_876 . ? O7 V5 V6 38.50(15) . . ? O4 V5 V6 93.29(13) . . ? O3 V5 V6 85.35(12) 2_876 . ? O6 V5 V6 126.06(11) 2_876 . ? O6 V5 V6 49.54(11) . . ? V10 V5 V6 60.41(4) . . ? O8 V5 V3 38.25(16) 2_876 2_876 ? O7 V5 V3 145.16(15) . 2_876 ? O4 V5 V3 92.21(13) . 2_876 ? O3 V5 V3 87.37(12) 2_876 2_876 ? O6 V5 V3 49.40(11) 2_876 2_876 ? O6 V5 V3 126.10(12) . 2_876 ? V10 V5 V3 122.52(5) . 2_876 ? V6 V5 V3 172.22(5) . 2_876 ? O8 V5 V4 84.67(15) 2_876 . ? O7 V5 V4 137.69(16) . . ? O4 V5 V4 37.43(13) . . ? O3 V5 V4 126.34(12) 2_876 . ? O6 V5 V4 47.60(11) 2_876 . ? O6 V5 V4 87.44(11) . . ? V10 V5 V4 62.48(5) . . ? V6 V5 V4 122.78(5) . . ? V3 V5 V4 60.21(4) 2_876 . ? O12 V6 O13 103.8(2) . . ? O12 V6 O15 104.6(2) . . ? O13 V6 O15 93.7(2) . . ? O12 V6 O5 100.3(2) . . ? O13 V6 O5 154.7(2) . . ? O15 V6 O5 87.45(18) . . ? O12 V6 O7 100.2(2) . . ? O13 V6 O7 87.51(19) . . ? O15 V6 O7 154.05(18) . . ? O5 V6 O7 80.76(17) . . ? O12 V6 O6 173.0(2) . . ? O13 V6 O6 79.60(17) . . ? O15 V6 O6 81.03(17) . . ? O5 V6 O6 75.63(16) . . ? O7 V6 O6 73.70(16) . . ? O12 V6 V3 136.38(18) . . ? O13 V6 V3 86.30(15) . . ? O15 V6 V3 31.78(14) . . ? O5 V6 V3 81.48(13) . . ? O7 V6 V3 122.83(13) . . ? O6 V6 V3 49.28(10) . . ? O12 V6 V4 136.47(19) . 2_876 ? O13 V6 V4 32.91(14) . 2_876 ? O15 V6 V4 81.30(15) . 2_876 ? O5 V6 V4 123.19(13) . 2_876 ? O7 V6 V4 85.94(14) . 2_876 ? O6 V6 V4 47.68(10) . 2_876 ? V3 V6 V4 60.75(4) . 2_876 ? O12 V6 V5 130.81(19) . . ? O13 V6 V5 82.31(14) . . ? O15 V6 V5 123.87(14) . . ? O5 V6 V5 76.16(13) . . ? O7 V6 V5 30.66(12) . . ? O6 V6 V5 43.05(10) . . ? V3 V6 V5 92.25(5) . . ? V4 V6 V5 65.59(5) 2_876 . ? O12 V6 V10 130.80(19) . . ? O13 V6 V10 125.09(15) . . ? O15 V6 V10 79.29(14) . . ? O5 V6 V10 30.55(13) . . ? O7 V6 V10 78.84(12) . . ? O6 V6 V10 45.50(10) . . ? V3 V6 V10 59.83(4) . . ? V4 V6 V10 92.73(5) 2_876 . ? V5 V6 V10 59.68(4) . . ? O2 V10 O5 107.1(2) . . ? O2 V10 O11 97.99(19) . . ? O5 V10 O11 98.8(2) . . ? O2 V10 O4 100.35(19) . . ? O5 V10 O4 94.59(19) . . ? O11 V10 O4 153.00(19) . . ? O2 V10 O3 94.24(19) . . ? O5 V10 O3 157.29(18) . . ? O11 V10 O3 85.44(17) . . ? O4 V10 O3 73.63(17) . . ? O2 V10 O6 168.42(19) . . ? O5 V10 O6 84.33(18) . . ? O11 V10 O6 81.46(16) . . ? O4 V10 O6 76.61(16) . . ? O3 V10 O6 74.18(15) . . ? O2 V10 V5 135.81(15) . . ? O5 V10 V5 79.55(15) . . ? O11 V10 V5 124.69(13) . . ? O4 V10 V5 35.78(12) . . ? O3 V10 V5 79.76(11) . . ? O6 V10 V5 43.23(10) . . ? O2 V10 V3 131.20(15) . . ? O5 V10 V3 85.34(16) . . ? O11 V10 V3 33.30(12) . . ? O4 V10 V3 126.08(13) . . ? O3 V10 V3 86.26(12) . . ? O6 V10 V3 49.65(10) . . ? V5 V10 V3 92.37(5) . . ? O2 V10 V6 142.51(16) . . ? O5 V10 V6 35.74(15) . . ? O11 V10 V6 86.80(13) . . ? O4 V10 V6 90.56(12) . . ? O3 V10 V6 123.25(11) . . ? O6 V10 V6 49.07(10) . . ? V5 V10 V6 59.92(5) . . ? V3 V10 V6 59.79(4) . . ? O2 V10 Ba1 50.72(14) . . ? O5 V10 Ba1 106.87(15) . . ? O11 V10 Ba1 47.39(12) . . ? O4 V10 Ba1 147.67(12) . . ? O3 V10 Ba1 92.45(11) . . ? O6 V10 Ba1 128.36(11) . . ? V5 V10 Ba1 169.82(4) . . ? V3 V10 Ba1 80.49(4) . . ? V6 V10 Ba1 120.95(5) . . ? O26 Ba1 O18 75.9(3) . . ? O26 Ba1 O19 77.0(3) . . ? O18 Ba1 O19 144.6(2) . . ? O26 Ba1 O11 87.7(3) . . ? O18 Ba1 O11 81.27(18) . . ? O19 Ba1 O11 119.85(19) . . ? O26 Ba1 O2 137.7(3) . 2_776 ? O18 Ba1 O2 120.82(17) . 2_776 ? O19 Ba1 O2 68.87(17) . 2_776 ? O11 Ba1 O2 130.74(12) . 2_776 ? O26 Ba1 O9 80.4(2) . . ? O18 Ba1 O9 76.89(18) . . ? O19 Ba1 O9 76.6(2) . . ? O11 Ba1 O9 157.09(13) . . ? O2 Ba1 O9 68.19(13) 2_776 . ? O26 Ba1 O2 139.7(3) . . ? O18 Ba1 O2 81.46(18) . . ? O19 Ba1 O2 133.6(2) . . ? O11 Ba1 O2 55.85(12) . . ? O2 Ba1 O2 82.64(12) 2_776 . ? O9 Ba1 O2 126.21(13) . . ? O26 Ba1 O14 126.9(3) . . ? O18 Ba1 O14 143.97(18) . . ? O19 Ba1 O14 71.4(2) . . ? O11 Ba1 O14 73.31(13) . . ? O2 Ba1 O14 64.12(14) 2_776 . ? O9 Ba1 O14 129.33(13) . . ? O2 Ba1 O14 63.25(13) . . ? O26 Ba1 C6 64.1(4) . . ? O18 Ba1 C6 19.3(4) . . ? O19 Ba1 C6 125.4(4) . . ? O11 Ba1 C6 96.1(5) . . ? O2 Ba1 C6 118.2(4) 2_776 . ? O9 Ba1 C6 61.1(5) . . ? O2 Ba1 C6 100.0(4) . . ? O14 Ba1 C6 163.2(4) . . ? O26 Ba1 V10 115.4(3) . . ? O18 Ba1 V10 78.91(16) . . ? O19 Ba1 V10 133.95(18) . . ? O11 Ba1 V10 29.78(9) . . ? O2 Ba1 V10 106.31(9) 2_776 . ? O9 Ba1 V10 146.61(10) . . ? O2 Ba1 V10 26.13(8) . . ? O14 Ba1 V10 66.30(9) . . ? C6 Ba1 V10 97.9(4) . . ? O26 Ba1 Ba1 179.3(2) . 2_776 ? O18 Ba1 Ba1 103.56(15) . 2_776 ? O19 Ba1 Ba1 103.35(16) . 2_776 ? O11 Ba1 Ba1 92.67(9) . 2_776 ? O2 Ba1 Ba1 42.20(8) 2_776 2_776 ? O9 Ba1 Ba1 99.04(10) . 2_776 ? O2 Ba1 Ba1 40.44(8) . 2_776 ? O14 Ba1 Ba1 53.82(12) . 2_776 ? C6 Ba1 Ba1 115.3(3) . 2_776 ? V10 Ba1 Ba1 64.88(3) . 2_776 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.118 _refine_diff_density_min -1.157 _refine_diff_density_rms 0.154 _database_code_depnum_ccdc_archive 'CCDC 928367'