# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Evamarie Hey-Hawkins' _publ_contact_author_email HEY@RZ.UNI-LEIPZIG.DE _publ_section_title ; Soluble Monometallic Salen Complexes Derived from O-functionalised Diamines as Metalloligands for the Synthesis of Heterobimetallic Complexes ; loop_ _publ_author_name 'Evamarie Hey-Hawkins' 'Sebastian Fritzsche' 'Peter Lonnecke' 'Michael Schley' data_s022_fin _database_code_depnum_ccdc_archive 'CCDC 736166' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H62 N2 Ni O8' _chemical_formula_weight 817.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.4763(10) _cell_length_b 14.9087(13) _cell_length_c 19.1295(11) _cell_angle_alpha 90.00 _cell_angle_beta 115.318(6) _cell_angle_gamma 90.00 _cell_volume 4505.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 6987 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 24.45 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 0.482 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8909 _exptl_absorpt_correction_T_max 0.9426 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(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 'Stoe IPDS area detector' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30196 _diffrn_reflns_av_R_equivalents 0.0895 _diffrn_reflns_av_sigmaI/netI 0.2335 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.96 _reflns_number_total 8271 _reflns_number_gt 2690 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software, STOE X-RED' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0176P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8271 _refine_ls_number_parameters 519 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1233 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_ref 0.563 _refine_ls_restrained_S_all 0.563 _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 Ni1 Ni 0.07426(3) 0.46993(3) 0.64101(3) 0.03698(12) Uani 1 1 d . . . O1 O 0.18111(12) 0.42961(13) 0.70523(13) 0.0430(7) Uani 1 1 d . . . O2 O 0.03828(12) 0.35829(12) 0.65367(13) 0.0407(6) Uani 1 1 d . . . O3 O 0.05684(18) 0.91361(17) 0.54332(17) 0.0769(10) Uani 1 1 d . . . O4 O -0.08456(16) 0.92155(17) 0.48210(17) 0.0735(9) Uani 1 1 d . . . H1O4 H -0.0708(6) 0.985(3) 0.471(2) 0.110 Uiso 1 1 calc R . . N1 N 0.10964(16) 0.58396(17) 0.63436(15) 0.0364(7) Uani 1 1 d . . . N2 N -0.03181(15) 0.50819(15) 0.57269(15) 0.0359(7) Uani 1 1 d . . . C1 C 0.2582(2) 0.5656(2) 0.7215(2) 0.0414(10) Uani 1 1 d . . . C2 C 0.25331(19) 0.4729(2) 0.73544(19) 0.0399(9) Uani 1 1 d . . . C3 C 0.3297(2) 0.4262(2) 0.7826(2) 0.0463(11) Uani 1 1 d . . . C4 C 0.40275(19) 0.4756(3) 0.8152(2) 0.0509(10) Uani 1 1 d . . . H4 H 0.4526 0.4447 0.8466 0.061 Uiso 1 1 calc R . . C5 C 0.4098(2) 0.5686(2) 0.8057(2) 0.0492(11) Uani 1 1 d . . . C6 C 0.3376(2) 0.6121(2) 0.7590(2) 0.0526(11) Uani 1 1 d . . . H6 H 0.3395 0.6741 0.7511 0.063 Uiso 1 1 calc R . . C7 C 0.3284(2) 0.3254(2) 0.7961(2) 0.0561(12) Uani 1 1 d . . . C8 C 0.2947(2) 0.2759(2) 0.7185(2) 0.0681(13) Uani 1 1 d . . . H8A H 0.2938 0.2119 0.7273 0.102 Uiso 1 1 calc R . . H8B H 0.3312 0.2881 0.6931 0.102 Uiso 1 1 calc R . . H8C H 0.2378 0.2965 0.6860 0.102 Uiso 1 1 calc R . . C9 C 0.2736(2) 0.3056(2) 0.8394(2) 0.0730(13) Uani 1 1 d . . . H9A H 0.2983 0.3345 0.8896 0.109 Uiso 1 1 calc R . . H9B H 0.2711 0.2414 0.8460 0.109 Uiso 1 1 calc R . . H9C H 0.2169 0.3286 0.8097 0.109 Uiso 1 1 calc R . . C10 C 0.4174(2) 0.2877(2) 0.8448(3) 0.0857(15) Uani 1 1 d . . . H10A H 0.4396 0.3135 0.8963 0.128 Uiso 1 1 calc R . . H10B H 0.4543 0.3028 0.8206 0.128 Uiso 1 1 calc R . . H10C H 0.4142 0.2230 0.8484 0.128 Uiso 1 1 calc R . . C11 C 0.4953(2) 0.6159(2) 0.8456(2) 0.0571(12) Uani 1 1 d . . . C12 C 0.4887(2) 0.7162(2) 0.8317(3) 0.1026(19) Uani 1 1 d . . . H12A H 0.4653 0.7280 0.7766 0.154 Uiso 1 1 calc R . . H12B H 0.5445 0.7430 0.8570 0.154 Uiso 1 1 calc R . . H12C H 0.4520 0.7420 0.8527 0.154 Uiso 1 1 calc R . . C13 C 0.5553(2) 0.5783(3) 0.8133(3) 0.0812(14) Uani 1 1 d . . . H13A H 0.5567 0.5133 0.8172 0.122 Uiso 1 1 calc R . . H13B H 0.6118 0.6019 0.8428 0.122 Uiso 1 1 calc R . . H13C H 0.5355 0.5956 0.7595 0.122 Uiso 1 1 calc R . . C14 C 0.5342(2) 0.5981(3) 0.9317(3) 0.0977(17) Uani 1 1 d . . . H14A H 0.4985 0.6238 0.9538 0.147 Uiso 1 1 calc R . . H14B H 0.5899 0.6251 0.9557 0.147 Uiso 1 1 calc R . . H14C H 0.5389 0.5339 0.9408 0.147 Uiso 1 1 calc R . . C15 C 0.1871(2) 0.6163(2) 0.6725(2) 0.0448(10) Uani 1 1 d . . . H15 H 0.1955 0.6776 0.6666 0.054 Uiso 1 1 calc R . . C16 C -0.10564(19) 0.3666(2) 0.5601(2) 0.0385(9) Uani 1 1 d . . . C17 C -0.0364(2) 0.3214(2) 0.6184(2) 0.0400(9) Uani 1 1 d . . . C18 C -0.0503(2) 0.2329(2) 0.6411(2) 0.0437(9) Uani 1 1 d . . . C19 C -0.1283(2) 0.1947(2) 0.5982(2) 0.0516(11) Uani 1 1 d . . . H19 H -0.1368 0.1361 0.6114 0.062 Uiso 1 1 calc R . . C20 C -0.1966(2) 0.2358(2) 0.5359(2) 0.0535(11) Uani 1 1 d . . . C21 C -0.1843(2) 0.3213(3) 0.5192(2) 0.0505(11) Uani 1 1 d . . . H21 H -0.2288 0.3518 0.4795 0.061 Uiso 1 1 calc R . . C22 C 0.0176(2) 0.1844(2) 0.7098(2) 0.0501(10) Uani 1 1 d . . . C23 C -0.0129(2) 0.0933(2) 0.7256(2) 0.0760(14) Uani 1 1 d . . . H23A H -0.0635 0.1018 0.7338 0.114 Uiso 1 1 calc R . . H23B H 0.0311 0.0665 0.7714 0.114 Uiso 1 1 calc R . . H23C H -0.0256 0.0539 0.6817 0.114 Uiso 1 1 calc R . . C24 C 0.0433(2) 0.2420(3) 0.7831(2) 0.0698(12) Uani 1 1 d . . . H24A H 0.0625 0.3003 0.7745 0.105 Uiso 1 1 calc R . . H24B H 0.0887 0.2125 0.8261 0.105 Uiso 1 1 calc R . . H24C H -0.0050 0.2496 0.7949 0.105 Uiso 1 1 calc R . . C25 C 0.0961(2) 0.1678(2) 0.6949(2) 0.0623(12) Uani 1 1 d . . . H25A H 0.0813 0.1284 0.6507 0.093 Uiso 1 1 calc R . . H25B H 0.1401 0.1402 0.7401 0.093 Uiso 1 1 calc R . . H25C H 0.1164 0.2245 0.6844 0.093 Uiso 1 1 calc R . . C26 C -0.2793(2) 0.1834(3) 0.4905(3) 0.0693(13) Uani 1 1 d . . . C27 C -0.2567(3) 0.0923(3) 0.4642(3) 0.129(2) Uani 1 1 d . . . H27A H -0.3077 0.0570 0.4382 0.194 Uiso 1 1 calc R . . H27B H -0.2172 0.0598 0.5091 0.194 Uiso 1 1 calc R . . H27C H -0.2310 0.1033 0.4290 0.194 Uiso 1 1 calc R . . C28 C -0.3190(3) 0.1620(4) 0.5439(3) 0.167(3) Uani 1 1 d . . . H28A H -0.3396 0.2168 0.5573 0.250 Uiso 1 1 calc R . . H28B H -0.2774 0.1342 0.5905 0.250 Uiso 1 1 calc R . . H28C H -0.3660 0.1211 0.5185 0.250 Uiso 1 1 calc R . . C29 C -0.3372(3) 0.2303(3) 0.4193(3) 0.136(2) Uani 1 1 d . . . H29A H -0.3866 0.1932 0.3915 0.204 Uiso 1 1 calc R . . H29B H -0.3082 0.2417 0.3868 0.204 Uiso 1 1 calc R . . H29C H -0.3548 0.2868 0.4329 0.204 Uiso 1 1 calc R . . C30 C -0.10023(19) 0.4571(2) 0.54182(19) 0.0399(9) Uani 1 1 d . . . H30 H -0.1495 0.4837 0.5044 0.048 Uiso 1 1 calc R . . C31 C 0.04276(19) 0.6433(2) 0.58637(19) 0.0368(9) Uani 1 1 d . . . C32 C -0.0351(2) 0.6000(2) 0.5525(2) 0.0404(9) Uani 1 1 d . . . C33 C -0.1073(2) 0.6484(2) 0.5055(2) 0.0489(10) Uani 1 1 d . . . H33 H -0.1602 0.6197 0.4820 0.059 Uiso 1 1 calc R . . C34 C -0.1002(2) 0.7395(2) 0.4940(2) 0.0530(11) Uani 1 1 d . . . H34 H -0.1485 0.7726 0.4626 0.064 Uiso 1 1 calc R . . C35 C -0.0219(2) 0.7819(2) 0.5286(2) 0.0429(9) Uani 1 1 d . . . C36 C 0.0501(2) 0.7338(2) 0.5739(2) 0.0445(10) Uani 1 1 d . . . H36 H 0.1033 0.7622 0.5958 0.053 Uiso 1 1 calc R . . C37 C -0.0144(3) 0.8764(3) 0.5178(2) 0.0570(11) Uani 1 1 d . . . O5 O 0.30088(16) 0.4737(2) 0.53404(19) 0.0891(9) Uani 1 1 d . . . O6 O 0.4610(2) 0.4233(3) 0.5501(3) 0.1261(15) Uani 1 1 d . . . C38 C 0.3710(3) 0.4695(4) 0.6052(3) 0.1194(19) Uani 1 1 d . . . H38A H 0.3709 0.4117 0.6296 0.143 Uiso 1 1 calc R . . H38B H 0.3664 0.5169 0.6388 0.143 Uiso 1 1 calc R . . C39 C 0.4493(3) 0.4796(5) 0.5994(4) 0.153(3) Uani 1 1 d . . . H39A H 0.4529 0.5412 0.5833 0.183 Uiso 1 1 calc R . . H39B H 0.4956 0.4711 0.6509 0.183 Uiso 1 1 calc R . . C40 C 0.3920(5) 0.4306(5) 0.4772(4) 0.164(3) Uani 1 1 d . . . H40A H 0.3979 0.3865 0.4418 0.196 Uiso 1 1 calc R . . H40B H 0.3916 0.4906 0.4559 0.196 Uiso 1 1 calc R . . C41 C 0.3126(4) 0.4155(4) 0.4833(4) 0.148(2) Uani 1 1 d . . . H41A H 0.2654 0.4222 0.4321 0.177 Uiso 1 1 calc R . . H41B H 0.3117 0.3538 0.5006 0.177 Uiso 1 1 calc R . . O7 O 0.2283(3) 0.5110(2) 0.2994(2) 0.1261(14) Uani 1 1 d . . . O8 O 0.2522(2) 0.67110(18) 0.2367(2) 0.0971(11) Uani 1 1 d . . . C42 C 0.2711(4) 0.5147(3) 0.2515(3) 0.1055(18) Uani 1 1 d . . . H42A H 0.2307 0.5051 0.1975 0.127 Uiso 1 1 calc R . . H42B H 0.3137 0.4670 0.2661 0.127 Uiso 1 1 calc R . . C43 C 0.3114(3) 0.5998(4) 0.2587(4) 0.126(2) Uani 1 1 d . . . H43A H 0.3527 0.6085 0.3125 0.152 Uiso 1 1 calc R . . H43B H 0.3421 0.6007 0.2262 0.152 Uiso 1 1 calc R . . C44 C 0.2068(4) 0.6691(4) 0.2821(4) 0.112(2) Uani 1 1 d . . . H44A H 0.1647 0.7173 0.2662 0.134 Uiso 1 1 calc R . . H44B H 0.2456 0.6783 0.3366 0.134 Uiso 1 1 calc R . . C45 C 0.1662(4) 0.5855(5) 0.2730(4) 0.142(2) Uani 1 1 d . . . H45A H 0.1277 0.5767 0.2184 0.171 Uiso 1 1 calc R . . H45B H 0.1324 0.5851 0.3027 0.171 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0296(2) 0.0402(2) 0.0395(3) 0.0020(3) 0.01319(19) 0.0024(2) O1 0.0270(12) 0.0379(14) 0.0527(17) 0.0072(11) 0.0062(12) 0.0043(10) O2 0.0314(12) 0.0377(13) 0.0518(16) 0.0035(11) 0.0165(12) -0.0042(10) O3 0.0656(19) 0.0491(17) 0.106(3) 0.0191(17) 0.0276(18) 0.0053(14) O4 0.075(2) 0.0500(16) 0.088(2) 0.0184(16) 0.0272(17) 0.0180(14) N1 0.0354(16) 0.0346(16) 0.0403(19) 0.0003(14) 0.0172(15) 0.0051(13) N2 0.0317(14) 0.0380(18) 0.0378(18) 0.0020(12) 0.0147(13) 0.0048(12) C1 0.0309(19) 0.044(2) 0.046(3) 0.0022(17) 0.0124(18) 0.0044(16) C2 0.0337(19) 0.038(2) 0.045(2) -0.003(2) 0.0135(18) -0.0024(19) C3 0.0273(19) 0.048(2) 0.057(3) 0.0041(18) 0.0115(19) 0.0027(16) C4 0.035(2) 0.062(2) 0.051(2) 0.009(2) 0.0137(18) 0.010(2) C5 0.032(2) 0.051(2) 0.055(3) -0.0045(19) 0.010(2) -0.0021(17) C6 0.039(2) 0.046(2) 0.066(3) 0.002(2) 0.016(2) -0.0028(18) C7 0.035(2) 0.048(2) 0.069(3) 0.015(2) 0.007(2) 0.0036(18) C8 0.052(2) 0.053(3) 0.094(4) 0.002(2) 0.026(2) 0.0049(19) C9 0.064(3) 0.077(3) 0.063(3) 0.028(2) 0.013(2) 0.000(2) C10 0.044(2) 0.064(3) 0.118(4) 0.031(3) 0.005(2) 0.015(2) C11 0.029(2) 0.064(3) 0.068(3) -0.009(2) 0.011(2) -0.0075(18) C12 0.045(2) 0.056(3) 0.174(5) -0.012(3) 0.016(3) -0.020(2) C13 0.044(2) 0.091(3) 0.106(4) -0.004(3) 0.030(3) -0.014(2) C14 0.048(3) 0.140(4) 0.086(4) -0.026(3) 0.011(3) -0.025(3) C15 0.042(2) 0.037(2) 0.055(3) -0.0009(18) 0.020(2) 0.0001(17) C16 0.0315(19) 0.041(2) 0.042(2) -0.0044(18) 0.0150(18) -0.0051(16) C17 0.034(2) 0.047(2) 0.041(2) -0.0081(18) 0.0186(19) -0.0039(18) C18 0.043(2) 0.046(2) 0.047(3) -0.0005(18) 0.0239(19) -0.0069(17) C19 0.053(2) 0.051(2) 0.057(3) 0.000(2) 0.028(2) -0.011(2) C20 0.043(2) 0.061(3) 0.059(3) 0.001(2) 0.024(2) -0.0087(19) C21 0.033(2) 0.063(3) 0.050(3) -0.003(2) 0.013(2) -0.0001(19) C22 0.052(2) 0.052(2) 0.053(3) 0.013(2) 0.028(2) -0.0023(19) C23 0.077(3) 0.068(3) 0.082(3) 0.029(2) 0.033(3) -0.009(2) C24 0.075(3) 0.091(3) 0.044(3) 0.003(2) 0.027(2) -0.008(2) C25 0.060(3) 0.064(3) 0.063(3) 0.021(2) 0.027(2) 0.010(2) C26 0.043(2) 0.071(3) 0.088(4) -0.012(3) 0.022(3) -0.022(2) C27 0.084(4) 0.113(4) 0.160(6) -0.065(4) 0.023(4) -0.040(3) C28 0.106(4) 0.294(8) 0.125(5) -0.078(5) 0.073(4) -0.129(5) C29 0.050(3) 0.141(5) 0.151(5) 0.023(4) -0.020(3) -0.036(3) C30 0.0291(18) 0.053(2) 0.036(2) -0.0032(19) 0.0125(17) 0.0047(17) C31 0.037(2) 0.039(2) 0.036(2) 0.0040(17) 0.0172(17) 0.0084(16) C32 0.042(2) 0.043(2) 0.040(2) -0.0027(18) 0.0201(19) 0.0048(18) C33 0.043(2) 0.049(2) 0.048(3) 0.0062(19) 0.0127(19) 0.0074(17) C34 0.046(2) 0.056(3) 0.046(3) 0.013(2) 0.010(2) 0.0150(19) C35 0.056(2) 0.035(2) 0.040(2) 0.0055(17) 0.022(2) 0.0065(18) C36 0.038(2) 0.049(2) 0.047(2) -0.0019(18) 0.0186(18) 0.0067(17) C37 0.053(3) 0.061(3) 0.052(3) 0.011(2) 0.018(2) 0.017(2) O5 0.0589(17) 0.116(2) 0.084(2) -0.007(2) 0.0234(17) 0.0259(19) O6 0.092(3) 0.140(3) 0.169(5) -0.004(3) 0.076(3) 0.024(2) C38 0.074(3) 0.206(5) 0.078(4) 0.000(4) 0.032(3) 0.034(4) C39 0.058(3) 0.239(8) 0.136(6) -0.078(6) 0.017(4) 0.009(4) C40 0.136(6) 0.265(9) 0.123(6) -0.086(6) 0.088(5) -0.069(6) C41 0.126(5) 0.209(7) 0.121(6) -0.064(5) 0.065(5) -0.044(5) O7 0.198(4) 0.078(3) 0.138(4) 0.001(2) 0.106(3) -0.026(2) O8 0.107(2) 0.063(2) 0.134(3) 0.0158(19) 0.065(2) 0.0242(18) C42 0.146(5) 0.061(4) 0.139(5) -0.008(3) 0.089(4) -0.004(3) C43 0.112(4) 0.099(4) 0.189(7) 0.019(4) 0.083(4) 0.014(4) C44 0.115(5) 0.090(4) 0.163(6) -0.019(4) 0.090(5) -0.002(3) C45 0.139(6) 0.145(6) 0.188(8) -0.018(6) 0.113(5) -0.019(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O2 1.8316(19) . ? Ni1 N1 1.832(3) . ? Ni1 O1 1.8428(19) . ? Ni1 N2 1.843(2) . ? O1 C2 1.311(3) . ? O2 C17 1.307(3) . ? O3 C37 1.256(4) . ? O4 C37 1.307(4) . ? N1 C15 1.324(4) . ? N1 C31 1.440(4) . ? N2 C30 1.324(4) . ? N2 C32 1.417(4) . ? C1 C15 1.414(4) . ? C1 C2 1.418(4) . ? C1 C6 1.437(4) . ? C2 C3 1.432(4) . ? C3 C4 1.371(4) . ? C3 C7 1.527(4) . ? C4 C5 1.411(4) . ? C5 C6 1.359(4) . ? C5 C11 1.529(4) . ? C7 C8 1.532(5) . ? C7 C10 1.537(4) . ? C7 C9 1.538(5) . ? C11 C14 1.514(5) . ? C11 C12 1.514(5) . ? C11 C13 1.532(5) . ? C16 C30 1.408(4) . ? C16 C17 1.416(4) . ? C16 C21 1.427(4) . ? C17 C18 1.442(4) . ? C18 C19 1.377(4) . ? C18 C22 1.524(4) . ? C19 C20 1.415(4) . ? C20 C21 1.355(4) . ? C20 C26 1.541(5) . ? C22 C25 1.536(5) . ? C22 C23 1.537(4) . ? C22 C24 1.539(5) . ? C26 C29 1.480(5) . ? C26 C28 1.495(6) . ? C26 C27 1.557(5) . ? C31 C36 1.387(4) . ? C31 C32 1.390(4) . ? C32 C33 1.397(4) . ? C33 C34 1.390(4) . ? C34 C35 1.391(4) . ? C35 C36 1.384(4) . ? C35 C37 1.437(4) . ? O5 C41 1.381(6) . ? O5 C38 1.390(5) . ? O6 C39 1.341(6) . ? O6 C40 1.404(7) . ? C38 C39 1.428(7) . ? C40 C41 1.460(7) . ? O7 C42 1.411(6) . ? O7 C45 1.482(6) . ? O8 C44 1.405(6) . ? O8 C43 1.416(5) . ? C42 C43 1.429(6) . ? C44 C45 1.407(6) . ? 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 O2 Ni1 N1 176.09(12) . . ? O2 Ni1 O1 85.56(9) . . ? N1 Ni1 O1 94.19(10) . . ? O2 Ni1 N2 94.42(10) . . ? N1 Ni1 N2 86.02(11) . . ? O1 Ni1 N2 177.19(12) . . ? C2 O1 Ni1 130.0(2) . . ? C17 O2 Ni1 129.6(2) . . ? C15 N1 C31 119.2(3) . . ? C15 N1 Ni1 126.6(2) . . ? C31 N1 Ni1 114.1(2) . . ? C30 N2 C32 120.7(3) . . ? C30 N2 Ni1 125.5(2) . . ? C32 N2 Ni1 113.77(19) . . ? C15 C1 C2 122.6(3) . . ? C15 C1 C6 117.4(3) . . ? C2 C1 C6 120.0(3) . . ? O1 C2 C1 121.4(3) . . ? O1 C2 C3 120.1(3) . . ? C1 C2 C3 118.5(3) . . ? C4 C3 C2 117.5(3) . . ? C4 C3 C7 122.0(3) . . ? C2 C3 C7 120.5(3) . . ? C3 C4 C5 125.8(3) . . ? C6 C5 C4 116.4(3) . . ? C6 C5 C11 122.9(3) . . ? C4 C5 C11 120.7(3) . . ? C5 C6 C1 121.7(3) . . ? C3 C7 C8 109.7(3) . . ? C3 C7 C10 112.2(3) . . ? C8 C7 C10 106.4(3) . . ? C3 C7 C9 109.7(3) . . ? C8 C7 C9 111.1(3) . . ? C10 C7 C9 107.8(3) . . ? C14 C11 C12 109.2(4) . . ? C14 C11 C5 110.5(3) . . ? C12 C11 C5 112.5(3) . . ? C14 C11 C13 108.0(3) . . ? C12 C11 C13 107.8(3) . . ? C5 C11 C13 108.7(3) . . ? N1 C15 C1 124.9(3) . . ? C30 C16 C17 121.7(3) . . ? C30 C16 C21 117.9(3) . . ? C17 C16 C21 120.4(3) . . ? O2 C17 C16 122.3(3) . . ? O2 C17 C18 119.2(3) . . ? C16 C17 C18 118.4(3) . . ? C19 C18 C17 116.7(3) . . ? C19 C18 C22 121.7(3) . . ? C17 C18 C22 121.6(3) . . ? C18 C19 C20 126.0(3) . . ? C21 C20 C19 116.3(3) . . ? C21 C20 C26 123.3(3) . . ? C19 C20 C26 120.4(3) . . ? C20 C21 C16 121.9(3) . . ? C18 C22 C25 110.1(3) . . ? C18 C22 C23 112.4(3) . . ? C25 C22 C23 107.9(3) . . ? C18 C22 C24 109.7(3) . . ? C25 C22 C24 108.9(3) . . ? C23 C22 C24 107.7(3) . . ? C29 C26 C28 113.3(4) . . ? C29 C26 C20 112.7(3) . . ? C28 C26 C20 108.7(4) . . ? C29 C26 C27 106.4(4) . . ? C28 C26 C27 106.9(4) . . ? C20 C26 C27 108.5(3) . . ? N2 C30 C16 125.7(3) . . ? C36 C31 C32 121.0(3) . . ? C36 C31 N1 126.7(3) . . ? C32 C31 N1 112.2(3) . . ? C31 C32 C33 119.7(3) . . ? C31 C32 N2 113.8(3) . . ? C33 C32 N2 126.4(3) . . ? C34 C33 C32 119.3(3) . . ? C33 C34 C35 120.4(3) . . ? C36 C35 C34 120.6(3) . . ? C36 C35 C37 118.9(3) . . ? C34 C35 C37 120.6(3) . . ? C35 C36 C31 119.0(3) . . ? O3 C37 O4 121.9(4) . . ? O3 C37 C35 120.9(4) . . ? O4 C37 C35 117.2(4) . . ? C41 O5 C38 109.1(4) . . ? C39 O6 C40 109.0(5) . . ? O5 C38 C39 113.0(5) . . ? O6 C39 C38 115.4(5) . . ? O6 C40 C41 110.4(6) . . ? O5 C41 C40 113.1(5) . . ? C42 O7 C45 105.3(4) . . ? C44 O8 C43 109.5(4) . . ? O7 C42 C43 110.4(5) . . ? O8 C43 C42 111.8(4) . . ? O8 C44 C45 109.3(5) . . ? C44 C45 O7 111.4(5) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.276 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.039 data_c2271fin _database_code_depnum_ccdc_archive 'CCDC 736167' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H67 Cl Cr N9 O4' _chemical_formula_weight 957.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cr Cr 0.3209 0.6236 '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' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.5121(11) _cell_length_b 16.7505(12) _cell_length_c 21.4550(15) _cell_angle_alpha 90.00 _cell_angle_beta 101.4050(10) _cell_angle_gamma 90.00 _cell_volume 5464.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 6761 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 26.71 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2036 _exptl_absorpt_coefficient_mu 0.307 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 CCD area detector' _diffrn_measurement_method '\F scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35900 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.81 _reflns_number_total 11401 _reflns_number_gt 7844 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR92 (Giacovazzo 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Two poorly defined acetonitrile molecules had been removed with SQUEEZE SQUEEZE - P. v.d. Sluis and A. L. Spek, Acta Crystallogr., Sect A 1990, 46, 194-201 ; _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^)+(0.1021P)^2^+0.2647P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11401 _refine_ls_number_parameters 632 _refine_ls_number_restraints 87 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1716 _refine_ls_wR_factor_gt 0.1593 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.004 _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 Cr1 Cr 0.53305(2) 0.15271(2) 0.117078(18) 0.03682(13) Uani 1 1 d . . . Cl1 Cl 0.52747(4) 0.02462(4) 0.15739(3) 0.04622(17) Uani 1 1 d . . . O1 O 0.40727(11) 0.16605(10) 0.09517(8) 0.0457(4) Uani 1 1 d . . . O2 O 0.54552(11) 0.19897(10) 0.20004(8) 0.0443(4) Uani 1 1 d . . . O3 O 0.94697(13) 0.05496(14) 0.05243(10) 0.0622(6) Uani 1 1 d . . . O4 O 0.89754(12) -0.00509(13) -0.04050(10) 0.0642(6) Uani 1 1 d . . . N1 N 0.53583(12) 0.11144(11) 0.02913(9) 0.0360(4) Uani 1 1 d . . . N2 N 0.66432(12) 0.14002(11) 0.12701(9) 0.0373(4) Uani 1 1 d . . . C1 C 0.38024(15) 0.13141(14) -0.01540(12) 0.0392(5) Uani 1 1 d . . . C2 C 0.35289(16) 0.16058(13) 0.04016(12) 0.0400(5) Uani 1 1 d . . . C3 C 0.26317(17) 0.18395(15) 0.03513(14) 0.0464(6) Uani 1 1 d . . . C4 C 0.20844(17) 0.17941(16) -0.02460(14) 0.0525(7) Uani 1 1 d . . . H4 H 0.1500 0.1966 -0.0281 0.063 Uiso 1 1 calc R . . C5 C 0.23374(17) 0.15086(17) -0.08081(14) 0.0516(6) Uani 1 1 d . . . C6 C 0.31968(16) 0.12678(16) -0.07339(13) 0.0465(6) Uani 1 1 d . . . H6 H 0.3391 0.1061 -0.1090 0.056 Uiso 1 1 calc R . . C7 C 0.22937(18) 0.21329(17) 0.09348(15) 0.0555(7) Uani 1 1 d . . . C8 C 0.2787(2) 0.28954(19) 0.11976(18) 0.0744(10) Uani 1 1 d . . . H8A H 0.3413 0.2787 0.1303 0.112 Uiso 1 1 calc R . . H8B H 0.2585 0.3067 0.1576 0.112 Uiso 1 1 calc R . . H8C H 0.2673 0.3313 0.0879 0.112 Uiso 1 1 calc R . . C9 C 0.2434(2) 0.14875(19) 0.14556(15) 0.0647(8) Uani 1 1 d . . . H9A H 0.2085 0.1021 0.1304 0.097 Uiso 1 1 calc R . . H9B H 0.2254 0.1693 0.1833 0.097 Uiso 1 1 calc R . . H9C H 0.3051 0.1342 0.1558 0.097 Uiso 1 1 calc R . . C10 C 0.1304(2) 0.2333(2) 0.07785(18) 0.0797(10) Uani 1 1 d . . . H10A H 0.1201 0.2767 0.0474 0.120 Uiso 1 1 calc R . . H10B H 0.1112 0.2490 0.1164 0.120 Uiso 1 1 calc R . . H10C H 0.0976 0.1866 0.0599 0.120 Uiso 1 1 calc R . . C11 C 0.16930(19) 0.1516(2) -0.14528(15) 0.0655(8) Uani 1 1 d D . . C12 C 0.0825(2) 0.1159(3) -0.1384(2) 0.1132(17) Uani 1 1 d D . . H12A H 0.0607 0.1434 -0.1049 0.170 Uiso 1 1 calc R . . H12B H 0.0905 0.0598 -0.1279 0.170 Uiso 1 1 calc R . . H12C H 0.0405 0.1217 -0.1782 0.170 Uiso 1 1 calc R . . C13 C 0.1586(4) 0.2371(3) -0.1684(3) 0.151(3) Uani 1 1 d D . . H13A H 0.1460 0.2709 -0.1346 0.226 Uiso 1 1 calc R . . H13B H 0.1105 0.2403 -0.2048 0.226 Uiso 1 1 calc R . . H13C H 0.2125 0.2548 -0.1805 0.226 Uiso 1 1 calc R . . C14 C 0.2043(3) 0.1019(4) -0.1948(2) 0.134(2) Uani 1 1 d D . . H14A H 0.1606 0.1002 -0.2339 0.200 Uiso 1 1 calc R . . H14B H 0.2165 0.0481 -0.1788 0.200 Uiso 1 1 calc R . . H14C H 0.2579 0.1259 -0.2029 0.200 Uiso 1 1 calc R . . C15 C 0.46774(15) 0.10694(13) -0.01711(11) 0.0380(5) Uani 1 1 d . . . H15 H 0.4772 0.0853 -0.0556 0.046 Uiso 1 1 calc R . . C16 C 0.70053(18) 0.18018(17) 0.23812(13) 0.0502(6) Uani 1 1 d . . . C17 C 0.61215(17) 0.19722(14) 0.24670(13) 0.0444(6) Uani 1 1 d . . . C18 C 0.60146(19) 0.21247(16) 0.30996(13) 0.0517(7) Uani 1 1 d . . . C19 C 0.6748(2) 0.2156(2) 0.35774(15) 0.0696(9) Uani 1 1 d . A . H19 H 0.6663 0.2273 0.3989 0.083 Uiso 1 1 calc R . . C20 C 0.7622(2) 0.2028(2) 0.34989(15) 0.0755(10) Uani 1 1 d . . . C21 C 0.7722(2) 0.1846(2) 0.28967(15) 0.0680(9) Uani 1 1 d . A . H21 H 0.8290 0.1746 0.2824 0.082 Uiso 1 1 calc R . . C22 C 0.5084(2) 0.22472(18) 0.32308(14) 0.0599(8) Uani 1 1 d . . . C23 C 0.4664(2) 0.2997(2) 0.28928(19) 0.0821(11) Uani 1 1 d . . . H23A H 0.4983 0.3465 0.3079 0.123 Uiso 1 1 calc R . . H23B H 0.4057 0.3034 0.2941 0.123 Uiso 1 1 calc R . . H23C H 0.4686 0.2968 0.2445 0.123 Uiso 1 1 calc R . . C24 C 0.4508(2) 0.1515(2) 0.30033(16) 0.0707(9) Uani 1 1 d . . . H24A H 0.3918 0.1604 0.3076 0.106 Uiso 1 1 calc R . . H24B H 0.4757 0.1046 0.3238 0.106 Uiso 1 1 calc R . . H24C H 0.4486 0.1432 0.2553 0.106 Uiso 1 1 calc R . . C25 C 0.5103(3) 0.2330(3) 0.39512(17) 0.0914(12) Uani 1 1 d . . . H25A H 0.5395 0.2824 0.4106 0.137 Uiso 1 1 calc R . . H25B H 0.5421 0.1883 0.4175 0.137 Uiso 1 1 calc R . . H25C H 0.4506 0.2335 0.4025 0.137 Uiso 1 1 calc R . . C26 C 0.8409(19) 0.2298(11) 0.4026(9) 0.091(4) Uani 0.404(12) 1 d PD A 1 C27 C 0.8151(10) 0.2180(12) 0.4662(6) 0.124(7) Uani 0.404(12) 1 d PD A 1 H27A H 0.8673 0.2198 0.4996 0.186 Uiso 0.404(12) 1 calc PR A 1 H27B H 0.7865 0.1666 0.4669 0.186 Uiso 0.404(12) 1 calc PR A 1 H27C H 0.7750 0.2601 0.4730 0.186 Uiso 0.404(12) 1 calc PR A 1 C28 C 0.8681(7) 0.3163(8) 0.3941(7) 0.121(6) Uani 0.404(12) 1 d PD A 1 H28A H 0.8409 0.3509 0.4209 0.182 Uiso 0.404(12) 1 calc PR A 1 H28B H 0.8491 0.3320 0.3500 0.182 Uiso 0.404(12) 1 calc PR A 1 H28C H 0.9316 0.3209 0.4061 0.182 Uiso 0.404(12) 1 calc PR A 1 C29 C 0.919(4) 0.1750(15) 0.396(3) 0.153(3) Uani 0.404(12) 1 d PD A 1 H29A H 0.9312 0.1796 0.3538 0.230 Uiso 0.404(12) 1 calc PR A 1 H29B H 0.9045 0.1200 0.4041 0.230 Uiso 0.404(12) 1 calc PR A 1 H29C H 0.9708 0.1909 0.4272 0.230 Uiso 0.404(12) 1 calc PR A 1 C26F C 0.8390(12) 0.1943(8) 0.4092(6) 0.091(4) Uani 0.596(12) 1 d PD A 2 C27F C 0.8450(9) 0.2727(8) 0.4440(7) 0.196(12) Uani 0.596(12) 1 d PD A 2 H27D H 0.7942 0.2790 0.4636 0.294 Uiso 0.596(12) 1 calc PR A 2 H27E H 0.8466 0.3160 0.4142 0.294 Uiso 0.596(12) 1 calc PR A 2 H27F H 0.8982 0.2737 0.4766 0.294 Uiso 0.596(12) 1 calc PR A 2 C28F C 0.8245(6) 0.1261(10) 0.4548(5) 0.152(6) Uani 0.596(12) 1 d PD A 2 H28D H 0.8711 0.1271 0.4923 0.228 Uiso 0.596(12) 1 calc PR A 2 H28E H 0.8251 0.0752 0.4334 0.228 Uiso 0.596(12) 1 calc PR A 2 H28F H 0.7682 0.1333 0.4673 0.228 Uiso 0.596(12) 1 calc PR A 2 C29F C 0.928(2) 0.1790(10) 0.387(2) 0.153(3) Uani 0.596(12) 1 d PD A 2 H29D H 0.9345 0.2177 0.3548 0.230 Uiso 0.596(12) 1 calc PR A 2 H29E H 0.9276 0.1256 0.3697 0.230 Uiso 0.596(12) 1 calc PR A 2 H29F H 0.9762 0.1843 0.4232 0.230 Uiso 0.596(12) 1 calc PR A 2 C30 C 0.72039(17) 0.15454(16) 0.17862(13) 0.0475(6) Uani 1 1 d . . . H30 H 0.7801 0.1477 0.1772 0.057 Uiso 1 1 calc R . . C31 C 0.62189(15) 0.09050(13) 0.02084(11) 0.0361(5) Uani 1 1 d . . . C32 C 0.69035(15) 0.10715(13) 0.07176(11) 0.0379(5) Uani 1 1 d . . . C33 C 0.77723(16) 0.08969(14) 0.06731(12) 0.0412(5) Uani 1 1 d . . . H33 H 0.8239 0.1022 0.1010 0.049 Uiso 1 1 calc R . . C34 C 0.79371(15) 0.05365(15) 0.01258(12) 0.0431(6) Uani 1 1 d . . . C35 C 0.72433(16) 0.03583(15) -0.03779(13) 0.0456(6) Uani 1 1 d . . . H35 H 0.7361 0.0109 -0.0745 0.055 Uiso 1 1 calc R . . C36 C 0.63989(16) 0.05419(15) -0.03422(12) 0.0433(6) Uani 1 1 d . . . H36 H 0.5938 0.0426 -0.0685 0.052 Uiso 1 1 calc R . . C37 C 0.88496(17) 0.03257(16) 0.00702(13) 0.0471(6) Uani 1 1 d . . . N3 N 0.54798(15) 0.26694(12) 0.08154(10) 0.0472(5) Uani 1 1 d . . . C38 C 0.5677(3) 0.3277(2) 0.06722(19) 0.0877(11) Uani 1 1 d . . . C39 C 0.5923(5) 0.4067(3) 0.0462(3) 0.157(2) Uani 1 1 d . . . H39A H 0.5995 0.4034 0.0024 0.235 Uiso 1 1 calc . . . H39B H 0.6472 0.4237 0.0729 0.235 Uiso 1 1 calc . . . H39C H 0.5465 0.4449 0.0494 0.235 Uiso 1 1 calc . . . H1O H 0.995(3) 0.040(3) 0.042(2) 0.137(18) Uiso 1 1 d . . . N4 N 1.5923(6) -0.0118(4) 0.4117(4) 0.176(4) Uani 0.821(10) 1 d PU B 1 C40 C 1.6250(7) -0.0104(5) 0.3697(4) 0.125(3) Uani 0.821(10) 1 d PU B 1 C41 C 1.6669(8) -0.0085(6) 0.3178(5) 0.105(3) Uani 0.821(10) 1 d PU B 1 H41A H 1.7301 -0.0107 0.3329 0.158 Uiso 0.82 1 calc P B 1 H41B H 1.6516 0.0405 0.2941 0.158 Uiso 0.82 1 calc P B 1 H41C H 1.6482 -0.0540 0.2905 0.158 Uiso 0.82 1 calc P B 1 N4F N 1.5390(12) -0.0883(14) 0.3789(13) 0.116(10) Uani 0.179(10) 1 d PDU B 2 C40F C 1.5872(14) -0.0562(18) 0.3521(12) 0.088(8) Uani 0.179(10) 1 d PDU B 2 C41F C 1.642(3) -0.0120(16) 0.316(2) 0.081(13) Uani 0.179(10) 1 d PDU B 2 H41D H 1.6741 -0.0491 0.2950 0.121 Uiso 0.18 1 calc P B 2 H41E H 1.6826 0.0213 0.3452 0.121 Uiso 0.18 1 calc P B 2 H41F H 1.6046 0.0214 0.2851 0.121 Uiso 0.18 1 calc P B 2 N5 N 0.9490(5) 0.1566(8) 0.2027(4) 0.218(6) Uani 0.853(11) 1 d PU C 1 C42 C 1.0013(6) 0.1148(9) 0.2195(4) 0.151(4) Uani 0.853(11) 1 d PU C 1 C43 C 1.0646(12) 0.0613(13) 0.2412(11) 0.254(8) Uani 0.853(11) 1 d PU C 1 H43A H 1.1216 0.0872 0.2476 0.382 Uiso 0.85 1 calc P C 1 H43B H 1.0626 0.0185 0.2105 0.382 Uiso 0.85 1 calc P C 1 H43C H 1.0555 0.0394 0.2813 0.382 Uiso 0.85 1 calc P C 1 N5F N 0.9246(12) 0.055(3) 0.252(2) 0.23(3) Uani 0.147(11) 1 d PDU C 2 C42F C 0.9937 0.0537 0.2391 0.17(2) Uani 0.147(11) 1 d PDU C 2 C43F C 1.0777(13) 0.046(3) 0.220(2) 0.124(18) Uani 0.147(11) 1 d PDU C 2 H43D H 1.0975 -0.0089 0.2248 0.186 Uiso 0.15 1 calc P C 2 H43E H 1.1205 0.0806 0.2456 0.186 Uiso 0.15 1 calc P C 2 H43F H 1.0711 0.0613 0.1753 0.186 Uiso 0.15 1 calc P C 2 N6 N 1.1654(9) 0.0665(8) 0.4526(8) 0.372(8) Uani 1 1 d . . . C44 C 1.2343(9) 0.0920(6) 0.4501(5) 0.227(5) Uani 1 1 d . . . C45 C 1.3187(5) 0.1229(4) 0.4512(3) 0.156(3) Uani 1 1 d . . . H45A H 1.3168 0.1807 0.4531 0.235 Uiso 1 1 calc . . . H45B H 1.3385 0.1067 0.4130 0.235 Uiso 1 1 calc . . . H45C H 1.3590 0.1027 0.4882 0.235 Uiso 1 1 calc . . . N7 N 1.2723(7) -0.0035(7) 0.3093(5) 0.285(5) Uani 1 1 d . . . C46 C 1.3079(6) -0.0373(6) 0.2726(5) 0.197(4) Uani 1 1 d . . . C47 C 1.3455(6) -0.0693(5) 0.2317(5) 0.205(4) Uani 1 1 d . . . H47A H 1.3015 -0.0872 0.1958 0.308 Uiso 1 1 calc . . . H47B H 1.3800 -0.1146 0.2507 0.308 Uiso 1 1 calc . . . H47C H 1.3839 -0.0307 0.2174 0.308 Uiso 1 1 calc . . . 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 Cr1 0.0307(2) 0.0425(2) 0.0397(2) -0.00442(16) 0.01284(16) 0.00284(15) Cl1 0.0484(4) 0.0464(3) 0.0449(3) -0.0014(3) 0.0119(3) -0.0035(3) O1 0.0339(9) 0.0611(10) 0.0446(10) -0.0056(8) 0.0140(8) 0.0081(8) O2 0.0398(10) 0.0497(9) 0.0460(10) -0.0068(8) 0.0145(9) 0.0041(7) O3 0.0289(11) 0.0947(15) 0.0642(13) -0.0233(11) 0.0121(10) 0.0051(10) O4 0.0356(11) 0.0964(15) 0.0640(13) -0.0281(11) 0.0181(10) 0.0066(10) N1 0.0259(10) 0.0426(10) 0.0417(11) -0.0032(8) 0.0123(9) 0.0023(8) N2 0.0325(11) 0.0427(10) 0.0388(11) -0.0064(8) 0.0119(9) 0.0001(8) C1 0.0310(13) 0.0447(12) 0.0427(13) 0.0009(10) 0.0094(11) -0.0003(9) C2 0.0329(13) 0.0406(12) 0.0484(14) 0.0008(11) 0.0127(11) 0.0024(10) C3 0.0334(14) 0.0453(13) 0.0630(17) -0.0008(12) 0.0155(13) 0.0049(10) C4 0.0335(15) 0.0582(15) 0.0671(19) 0.0042(13) 0.0132(14) 0.0068(11) C5 0.0339(14) 0.0656(16) 0.0548(16) 0.0049(13) 0.0073(12) 0.0020(12) C6 0.0343(14) 0.0597(15) 0.0474(15) 0.0015(12) 0.0128(12) -0.0018(11) C7 0.0396(15) 0.0614(16) 0.0693(19) -0.0111(14) 0.0199(14) 0.0069(12) C8 0.069(2) 0.0654(19) 0.095(3) -0.0244(18) 0.029(2) 0.0078(16) C9 0.0595(19) 0.079(2) 0.0643(19) -0.0102(16) 0.0332(16) 0.0023(15) C10 0.0465(19) 0.103(3) 0.094(3) -0.021(2) 0.0247(18) 0.0202(17) C11 0.0367(16) 0.097(2) 0.0589(18) 0.0087(17) -0.0010(14) -0.0013(15) C12 0.047(2) 0.196(5) 0.088(3) 0.009(3) -0.008(2) -0.028(3) C13 0.158(5) 0.120(4) 0.131(4) 0.054(3) -0.077(4) -0.032(3) C14 0.082(3) 0.236(7) 0.071(3) -0.037(3) -0.016(2) 0.042(4) C15 0.0317(13) 0.0450(12) 0.0397(12) -0.0024(10) 0.0131(11) 0.0004(10) C16 0.0413(15) 0.0641(16) 0.0466(15) -0.0132(12) 0.0120(12) -0.0054(12) C17 0.0463(16) 0.0402(12) 0.0497(15) -0.0084(11) 0.0167(13) -0.0042(10) C18 0.0542(17) 0.0524(14) 0.0522(16) -0.0154(12) 0.0192(14) -0.0023(12) C19 0.071(2) 0.090(2) 0.0491(17) -0.0235(16) 0.0166(16) -0.0006(17) C20 0.058(2) 0.112(3) 0.0548(19) -0.0289(19) 0.0052(16) -0.0073(19) C21 0.0446(18) 0.101(2) 0.0582(18) -0.0239(17) 0.0103(15) -0.0058(16) C22 0.0616(19) 0.0687(18) 0.0551(17) -0.0165(14) 0.0253(15) 0.0032(14) C23 0.074(2) 0.078(2) 0.101(3) -0.020(2) 0.036(2) 0.0183(18) C24 0.063(2) 0.088(2) 0.070(2) -0.0111(17) 0.0338(18) -0.0104(17) C25 0.084(3) 0.131(3) 0.067(2) -0.035(2) 0.035(2) 0.002(2) C26 0.064(3) 0.143(11) 0.060(4) -0.028(6) -0.001(3) 0.006(9) C27 0.108(11) 0.19(2) 0.063(7) -0.024(10) -0.023(6) -0.038(12) C28 0.061(7) 0.203(15) 0.099(9) -0.072(10) 0.016(7) -0.062(8) C29 0.095(7) 0.262(8) 0.085(11) -0.053(5) -0.025(3) 0.058(5) C26F 0.064(3) 0.143(11) 0.060(4) -0.028(6) -0.001(3) 0.006(9) C27F 0.138(13) 0.219(17) 0.186(19) -0.163(17) -0.077(12) 0.049(11) C28F 0.106(7) 0.244(17) 0.094(6) 0.048(8) -0.012(5) 0.002(8) C29F 0.095(7) 0.262(8) 0.085(11) -0.053(5) -0.025(3) 0.058(5) C30 0.0345(14) 0.0618(15) 0.0480(15) -0.0108(12) 0.0130(12) -0.0007(11) C31 0.0299(12) 0.0414(11) 0.0397(12) -0.0024(10) 0.0139(10) 0.0031(9) C32 0.0336(13) 0.0400(11) 0.0427(13) -0.0050(10) 0.0138(11) 0.0018(9) C33 0.0315(13) 0.0501(13) 0.0437(13) -0.0054(11) 0.0113(11) 0.0005(10) C34 0.0315(13) 0.0515(13) 0.0501(15) -0.0048(11) 0.0174(12) 0.0023(10) C35 0.0344(14) 0.0586(14) 0.0476(14) -0.0114(12) 0.0170(12) 0.0030(11) C36 0.0303(13) 0.0560(14) 0.0436(14) -0.0109(11) 0.0074(11) 0.0038(11) C37 0.0330(14) 0.0579(15) 0.0529(16) -0.0083(12) 0.0148(13) 0.0020(11) N3 0.0556(14) 0.0395(11) 0.0491(13) -0.0011(9) 0.0164(11) 0.0024(10) C38 0.104(3) 0.081(3) 0.078(3) -0.005(2) 0.017(2) 0.009(2) C39 0.236(7) 0.082(3) 0.158(5) 0.022(3) 0.051(5) -0.038(4) N4 0.278(10) 0.131(6) 0.137(6) 0.021(4) 0.082(6) 0.067(6) C40 0.212(9) 0.084(5) 0.077(4) 0.010(4) 0.029(5) 0.058(6) C41 0.134(9) 0.099(6) 0.081(5) 0.019(4) 0.015(5) 0.016(5) N4F 0.101(17) 0.097(17) 0.16(2) 0.043(16) 0.047(16) 0.013(12) C40F 0.12(2) 0.060(14) 0.079(16) 0.006(13) 0.007(15) 0.037(14) C41F 0.069(17) 0.027(10) 0.14(3) -0.022(13) 0.005(16) -0.004(9) N5 0.073(5) 0.403(17) 0.171(7) -0.098(8) 0.007(5) 0.012(7) C42 0.078(6) 0.250(13) 0.128(6) -0.073(8) 0.026(5) -0.054(7) C43 0.209(15) 0.201(14) 0.38(2) -0.049(14) 0.113(15) -0.063(12) N5F 0.10(2) 0.25(4) 0.34(5) -0.24(4) 0.05(3) -0.01(3) C42F 0.11(3) 0.17(4) 0.22(5) -0.09(3) 0.01(3) -0.07(3) C43F 0.08(2) 0.16(4) 0.14(3) 0.06(3) 0.05(2) -0.01(2) N6 0.365(17) 0.312(14) 0.46(2) -0.012(13) 0.124(14) -0.167(12) C44 0.310(15) 0.166(8) 0.241(10) -0.028(7) 0.143(11) -0.074(8) C45 0.205(7) 0.127(5) 0.166(6) 0.036(4) 0.107(5) 0.033(5) N7 0.257(11) 0.374(15) 0.246(11) -0.049(9) 0.104(8) -0.050(9) C46 0.189(8) 0.228(9) 0.206(9) 0.054(7) 0.114(7) 0.016(7) C47 0.229(8) 0.178(7) 0.260(9) -0.046(6) 0.172(8) -0.007(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O2 1.9157(17) . ? Cr1 O1 1.9273(17) . ? Cr1 N2 2.0164(19) . ? Cr1 N1 2.0180(19) . ? Cr1 N3 2.089(2) . ? Cr1 Cl1 2.3213(7) . ? O1 C2 1.311(3) . ? O2 C17 1.289(3) . ? O3 C37 1.282(3) . ? O4 C37 1.247(3) . ? N1 C15 1.300(3) . ? N1 C31 1.425(3) . ? N2 C30 1.289(3) . ? N2 C32 1.435(3) . ? C1 C6 1.405(3) . ? C1 C15 1.425(3) . ? C1 C2 1.428(3) . ? C2 C3 1.429(3) . ? C3 C4 1.392(4) . ? C3 C7 1.531(4) . ? C4 C5 1.423(4) . ? C5 C6 1.372(4) . ? C5 C11 1.538(4) . ? C7 C8 1.537(4) . ? C7 C9 1.539(4) . ? C7 C10 1.542(4) . ? C11 C12 1.506(5) . ? C11 C13 1.513(6) . ? C11 C14 1.531(5) . ? C16 C21 1.407(4) . ? C16 C30 1.437(3) . ? C16 C17 1.447(4) . ? C17 C18 1.422(4) . ? C18 C19 1.374(4) . ? C18 C22 1.538(4) . ? C19 C20 1.415(4) . ? C20 C21 1.366(4) . ? C20 C26 1.56(3) . ? C20 C26F 1.569(17) . ? C22 C23 1.530(5) . ? C22 C24 1.540(4) . ? C22 C25 1.546(4) . ? C26 C27 1.510(15) . ? C26 C28 1.530(16) . ? C26 C29 1.550(14) . ? C26F C27F 1.503(11) . ? C26F C28F 1.549(13) . ? C26F C29F 1.563(11) . ? C31 C32 1.393(3) . ? C31 C36 1.405(3) . ? C32 C33 1.401(3) . ? C33 C34 1.388(3) . ? C34 C35 1.398(4) . ? C34 C37 1.486(3) . ? C35 C36 1.362(3) . ? N3 C38 1.122(4) . ? C38 C39 1.473(6) . ? N4 C40 1.116(9) . ? C40 C41 1.397(12) . ? N4F C40F 1.1607(10) . ? C40F C41F 1.4507(10) . ? N5 C42 1.079(14) . ? C42 C43 1.34(2) . ? N5F C42F 1.1607(10) . ? C42F C43F 1.4508(10) . ? N6 C44 1.162(13) . ? C44 C45 1.403(12) . ? N7 C46 1.191(11) . ? C46 C47 1.263(10) . ? 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 O2 Cr1 O1 95.23(7) . . ? O2 Cr1 N2 91.73(7) . . ? O1 Cr1 N2 172.07(7) . . ? O2 Cr1 N1 172.07(7) . . ? O1 Cr1 N1 91.11(7) . . ? N2 Cr1 N1 81.65(8) . . ? O2 Cr1 N3 88.32(8) . . ? O1 Cr1 N3 89.13(8) . . ? N2 Cr1 N3 87.28(8) . . ? N1 Cr1 N3 87.03(8) . . ? O2 Cr1 Cl1 91.83(5) . . ? O1 Cr1 Cl1 95.02(6) . . ? N2 Cr1 Cl1 88.54(6) . . ? N1 Cr1 Cl1 92.35(6) . . ? N3 Cr1 Cl1 175.82(6) . . ? C2 O1 Cr1 130.66(14) . . ? C17 O2 Cr1 129.08(15) . . ? C15 N1 C31 122.01(19) . . ? C15 N1 Cr1 124.67(14) . . ? C31 N1 Cr1 113.25(15) . . ? C30 N2 C32 122.0(2) . . ? C30 N2 Cr1 124.52(16) . . ? C32 N2 Cr1 113.34(15) . . ? C6 C1 C15 115.8(2) . . ? C6 C1 C2 120.1(2) . . ? C15 C1 C2 124.2(2) . . ? O1 C2 C1 122.1(2) . . ? O1 C2 C3 119.5(2) . . ? C1 C2 C3 118.4(2) . . ? C4 C3 C2 117.5(2) . . ? C4 C3 C7 121.7(2) . . ? C2 C3 C7 120.8(2) . . ? C3 C4 C5 125.3(2) . . ? C6 C5 C4 115.2(3) . . ? C6 C5 C11 123.4(3) . . ? C4 C5 C11 121.3(2) . . ? C5 C6 C1 123.4(2) . . ? C3 C7 C8 109.9(2) . . ? C3 C7 C9 110.3(2) . . ? C8 C7 C9 109.2(3) . . ? C3 C7 C10 112.3(3) . . ? C8 C7 C10 107.5(2) . . ? C9 C7 C10 107.6(3) . . ? C12 C11 C13 111.4(4) . . ? C12 C11 C14 107.3(4) . . ? C13 C11 C14 108.6(4) . . ? C12 C11 C5 110.1(3) . . ? C13 C11 C5 108.2(3) . . ? C14 C11 C5 111.3(3) . . ? N1 C15 C1 126.7(2) . . ? C21 C16 C30 116.0(2) . . ? C21 C16 C17 120.7(2) . . ? C30 C16 C17 123.1(2) . . ? O2 C17 C18 120.7(2) . . ? O2 C17 C16 122.7(2) . . ? C18 C17 C16 116.7(2) . . ? C19 C18 C17 118.9(2) . . ? C19 C18 C22 121.8(2) . . ? C17 C18 C22 119.3(3) . . ? C18 C19 C20 125.2(3) . . ? C21 C20 C19 115.9(3) . . ? C21 C20 C26 122.1(8) . . ? C19 C20 C26 120.1(8) . . ? C21 C20 C26F 122.5(5) . . ? C19 C20 C26F 120.6(5) . . ? C26 C20 C26F 22.6(8) . . ? C20 C21 C16 122.4(3) . . ? C23 C22 C18 110.5(3) . . ? C23 C22 C24 109.7(3) . . ? C18 C22 C24 110.0(2) . . ? C23 C22 C25 108.8(3) . . ? C18 C22 C25 111.2(3) . . ? C24 C22 C25 106.5(3) . . ? C27 C26 C28 111.1(11) . . ? C27 C26 C29 110.7(13) . . ? C28 C26 C29 108.2(12) . . ? C27 C26 C20 108.0(15) . . ? C28 C26 C20 112.6(15) . . ? C29 C26 C20 106(3) . . ? C27F C26F C28F 109.5(9) . . ? C27F C26F C29F 108.8(10) . . ? C28F C26F C29F 108.5(9) . . ? C27F C26F C20 106.6(10) . . ? C28F C26F C20 113.4(10) . . ? C29F C26F C20 110.0(19) . . ? N2 C30 C16 126.4(2) . . ? C32 C31 C36 119.9(2) . . ? C32 C31 N1 116.14(19) . . ? C36 C31 N1 123.9(2) . . ? C31 C32 C33 120.0(2) . . ? C31 C32 N2 115.42(19) . . ? C33 C32 N2 124.6(2) . . ? C34 C33 C32 119.3(2) . . ? C33 C34 C35 120.3(2) . . ? C33 C34 C37 120.6(2) . . ? C35 C34 C37 119.1(2) . . ? C36 C35 C34 120.7(2) . . ? C35 C36 C31 119.9(2) . . ? O4 C37 O3 123.7(2) . . ? O4 C37 C34 119.4(2) . . ? O3 C37 C34 116.9(2) . . ? C38 N3 Cr1 170.3(3) . . ? N3 C38 C39 178.1(5) . . ? N4 C40 C41 179.2(13) . . ? N4F C40F C41F 175.4(17) . . ? N5 C42 C43 178.1(16) . . ? N5F C42F C43F 175.2(16) . . ? N6 C44 C45 176.5(15) . . ? N7 C46 C47 176.6(12) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.81 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.399 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.052 data_c1547fin _database_code_depnum_ccdc_archive 'CCDC 736168' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H58 Cl2 Mo N6 O4' _chemical_formula_weight 913.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo Mo -1.6832 0.6857 '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' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.129(2) _cell_length_b 16.508(3) _cell_length_c 20.585(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.592(3) _cell_angle_gamma 90.00 _cell_volume 4927.2(13) _cell_formula_units_Z 4 _cell_measurement_temperature 218(2) _cell_measurement_reflns_used 930 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.36 _exptl_crystal_description prism _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 0.419 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 218(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26767 _diffrn_reflns_av_R_equivalents 0.0755 _diffrn_reflns_av_sigmaI/netI 0.0889 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.37 _reflns_number_total 10009 _reflns_number_gt 6635 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+13.4642P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 10009 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1384 _refine_ls_R_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.1895 _refine_ls_wR_factor_gt 0.1608 _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_restrained_S_all 1.164 _refine_ls_shift/su_max 0.003 _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 Mo1 Mo 0.28421(4) 0.02470(3) 0.87999(2) 0.02877(15) Uani 1 1 d . . . Cl1 Cl 0.16547(12) 0.05605(10) 0.93134(8) 0.0453(4) Uani 1 1 d . . . Cl2 Cl 0.39840(11) -0.01252(9) 0.82449(7) 0.0396(4) Uani 1 1 d . . . O1 O 0.1925(3) 0.0408(2) 0.79459(18) 0.0339(9) Uani 1 1 d . . . O2 O 0.2932(3) -0.0850(2) 0.91277(18) 0.0333(9) Uani 1 1 d . . . O3 O 0.4480(4) 0.4286(2) 0.9439(2) 0.0576(14) Uani 1 1 d . . . H3O H 0.4605 0.4769 0.9532 0.086 Uiso 1 1 d R . . O4 O 0.5311(4) 0.4133(2) 1.0524(2) 0.0535(13) Uani 1 1 d . . . N1 N 0.3231(3) 0.1469(3) 0.8690(2) 0.0323(11) Uani 1 1 d . . . N2 N 0.3796(3) 0.0535(3) 0.9759(2) 0.0286(11) Uani 1 1 d . . . C1 C 0.1921(4) 0.0840(3) 0.7400(3) 0.0347(14) Uani 1 1 d . . . C2 C 0.2477(4) 0.1547(4) 0.7465(3) 0.0379(15) Uani 1 1 d . . . C3 C 0.2428(5) 0.2034(4) 0.6899(3) 0.0467(17) Uani 1 1 d . . . H3 H 0.2791 0.2505 0.6954 0.056 Uiso 1 1 calc R . . C4 C 0.1869(5) 0.1847(4) 0.6268(3) 0.0491(18) Uani 1 1 d . . . C5 C 0.1336(5) 0.1142(4) 0.6214(3) 0.0482(17) Uani 1 1 d . . . H5 H 0.0960 0.1000 0.5781 0.058 Uiso 1 1 calc R . . C6 C 0.1322(4) 0.0635(4) 0.6752(3) 0.0384(15) Uani 1 1 d . . . C7 C 0.1812(6) 0.2389(6) 0.5655(4) 0.070(3) Uani 1 1 d . . . C8 C 0.2526(10) 0.2999(10) 0.5777(6) 0.176(8) Uani 1 1 d . . . H8A H 0.2560 0.3218 0.5348 0.263 Uiso 1 1 calc R . . H8B H 0.3113 0.2757 0.6015 0.263 Uiso 1 1 calc R . . H8C H 0.2382 0.3431 0.6051 0.263 Uiso 1 1 calc R . . C9 C 0.2216(12) 0.1863(12) 0.5139(7) 0.196(9) Uani 1 1 d . . . H9A H 0.1877 0.1358 0.5034 0.295 Uiso 1 1 calc R . . H9B H 0.2863 0.1748 0.5350 0.295 Uiso 1 1 calc R . . H9C H 0.2149 0.2168 0.4725 0.295 Uiso 1 1 calc R . . C10 C 0.0906(8) 0.2557(10) 0.5272(7) 0.200(9) Uani 1 1 d . . . H10A H 0.0636 0.2949 0.5510 0.300 Uiso 1 1 calc R . . H10B H 0.0546 0.2061 0.5206 0.300 Uiso 1 1 calc R . . H10C H 0.0909 0.2775 0.4835 0.300 Uiso 1 1 calc R . . C11 C 0.0708(5) -0.0118(4) 0.6669(3) 0.0479(17) Uani 1 1 d . . . C12 C 0.1315(6) -0.0868(4) 0.6869(4) 0.072(3) Uani 1 1 d . . . H12A H 0.1710 -0.0920 0.6574 0.108 Uiso 1 1 calc R . . H12B H 0.0928 -0.1345 0.6825 0.108 Uiso 1 1 calc R . . H12C H 0.1691 -0.0816 0.7335 0.108 Uiso 1 1 calc R . . C13 C 0.0112(6) -0.0233(5) 0.5927(4) 0.079(3) Uani 1 1 d . . . H13A H -0.0235 0.0258 0.5770 0.119 Uiso 1 1 calc R . . H13B H -0.0311 -0.0681 0.5903 0.119 Uiso 1 1 calc R . . H13C H 0.0509 -0.0349 0.5643 0.119 Uiso 1 1 calc R . . C14 C 0.0047(6) -0.0044(5) 0.7101(4) 0.068(2) Uani 1 1 d . . . H14A H 0.0396 -0.0018 0.7576 0.102 Uiso 1 1 calc R . . H14B H -0.0357 -0.0513 0.7026 0.102 Uiso 1 1 calc R . . H14C H -0.0320 0.0444 0.6977 0.102 Uiso 1 1 calc R . . C15 C 0.3050(4) 0.1828(3) 0.8104(3) 0.0377(15) Uani 1 1 d . . . H15 H 0.3332 0.2334 0.8100 0.045 Uiso 1 1 calc R . . C16 C 0.3054(4) -0.1159(3) 0.9748(3) 0.0325(13) Uani 1 1 d . . . C17 C 0.3599(4) -0.0736(3) 1.0316(3) 0.0345(14) Uani 1 1 d . . . C18 C 0.3828(5) -0.1108(4) 1.0963(3) 0.0404(15) Uani 1 1 d . . . H18 H 0.4211 -0.0830 1.1336 0.048 Uiso 1 1 calc R . . C19 C 0.3508(5) -0.1860(4) 1.1060(3) 0.0428(16) Uani 1 1 d . . . C20 C 0.2926(5) -0.2238(4) 1.0489(3) 0.0447(16) Uani 1 1 d . . . H20 H 0.2685 -0.2747 1.0552 0.054 Uiso 1 1 calc R . . C21 C 0.2674(4) -0.1921(3) 0.9832(3) 0.0368(14) Uani 1 1 d . . . C22 C 0.3778(6) -0.2275(5) 1.1759(4) 0.061(2) Uani 1 1 d . . . C23 C 0.4355(13) -0.1770(8) 1.2293(5) 0.206(10) Uani 1 1 d . . . H23A H 0.3975 -0.1371 1.2433 0.309 Uiso 1 1 calc R . . H23B H 0.4812 -0.1495 1.2124 0.309 Uiso 1 1 calc R . . H23C H 0.4664 -0.2106 1.2677 0.309 Uiso 1 1 calc R . . C24 C 0.4310(13) -0.3044(9) 1.1714(6) 0.193(8) Uani 1 1 d . . . H24A H 0.4062 -0.3287 1.1270 0.290 Uiso 1 1 calc R . . H24B H 0.4252 -0.3423 1.2060 0.290 Uiso 1 1 calc R . . H24C H 0.4956 -0.2913 1.1784 0.290 Uiso 1 1 calc R . . C25 C 0.2949(9) -0.2570(11) 1.1926(6) 0.196(9) Uani 1 1 d . . . H25A H 0.3126 -0.2971 1.2284 0.294 Uiso 1 1 calc R . . H25B H 0.2530 -0.2814 1.1527 0.294 Uiso 1 1 calc R . . H25C H 0.2645 -0.2120 1.2077 0.294 Uiso 1 1 calc R . . C26 C 0.1989(5) -0.2359(4) 0.9228(3) 0.0450(16) Uani 1 1 d . . . C27 C 0.1600(6) -0.3130(4) 0.9466(4) 0.072(3) Uani 1 1 d . . . H27A H 0.1130 -0.3363 0.9089 0.108 Uiso 1 1 calc R . . H27B H 0.1332 -0.2993 0.9827 0.108 Uiso 1 1 calc R . . H27C H 0.2094 -0.3519 0.9632 0.108 Uiso 1 1 calc R . . C28 C 0.2465(5) -0.2604(4) 0.8700(4) 0.059(2) Uani 1 1 d . . . H28A H 0.2696 -0.2125 0.8530 0.089 Uiso 1 1 calc R . . H28B H 0.2028 -0.2880 0.8328 0.089 Uiso 1 1 calc R . . H28C H 0.2975 -0.2965 0.8905 0.089 Uiso 1 1 calc R . . C29 C 0.1171(5) -0.1793(4) 0.8920(4) 0.058(2) Uani 1 1 d . . . H29A H 0.1373 -0.1348 0.8689 0.088 Uiso 1 1 calc R . . H29B H 0.0935 -0.1581 0.9277 0.088 Uiso 1 1 calc R . . H29C H 0.0688 -0.2093 0.8598 0.088 Uiso 1 1 calc R . . C30 C 0.3949(4) 0.0057(3) 1.0292(3) 0.0338(14) Uani 1 1 d . . . H30 H 0.4331 0.0264 1.0701 0.041 Uiso 1 1 calc R . . C31 C 0.3800(4) 0.1845(3) 0.9279(3) 0.0292(13) Uani 1 1 d . . . C32 C 0.4155(4) 0.1342(3) 0.9838(3) 0.0306(13) Uani 1 1 d . . . C33 C 0.4783(4) 0.1648(3) 1.0418(3) 0.0329(13) Uani 1 1 d . . . H33 H 0.5056 0.1302 1.0783 0.039 Uiso 1 1 calc R . . C34 C 0.5003(4) 0.2460(3) 1.0454(3) 0.0378(15) Uani 1 1 d . . . H34 H 0.5419 0.2669 1.0849 0.045 Uiso 1 1 calc R . . C35 C 0.4614(4) 0.2973(3) 0.9911(3) 0.0343(14) Uani 1 1 d . . . C36 C 0.4013(4) 0.2670(3) 0.9326(3) 0.0354(14) Uani 1 1 d . . . H36 H 0.3747 0.3017 0.8961 0.042 Uiso 1 1 calc R . . C37 C 0.4815(5) 0.3863(3) 0.9950(3) 0.0438(16) Uani 1 1 d . . . N3 N 0.3071(10) 0.5226(8) 1.0341(7) 0.171(6) Uani 1 1 d . . . C38 C 0.3926(9) 0.4666(7) 1.1509(5) 0.108(4) Uani 1 1 d . . . H38A H 0.3971 0.4082 1.1478 0.161 Uiso 1 1 calc R . . H38B H 0.3604 0.4801 1.1840 0.161 Uiso 1 1 calc R . . H38C H 0.4540 0.4899 1.1647 0.161 Uiso 1 1 calc R . . C39 C 0.3428(9) 0.4984(7) 1.0863(6) 0.107(4) Uani 1 1 d . . . N4 N 0.3431(11) 0.4011(9) 0.7611(8) 0.177(6) Uani 1 1 d . . . C40 C 0.2682(8) 0.4998(7) 0.8281(7) 0.124(5) Uani 1 1 d . . . H40A H 0.3111 0.5430 0.8474 0.186 Uiso 1 1 calc R . . H40B H 0.2523 0.4708 0.8642 0.186 Uiso 1 1 calc R . . H40C H 0.2128 0.5226 0.7974 0.186 Uiso 1 1 calc R . . C41 C 0.3103(11) 0.4447(9) 0.7915(8) 0.133(5) Uani 1 1 d . . . N5 N 0.1646(11) 0.3172(8) 0.8341(8) 0.160(5) Uani 1 1 d . . . C42 C 0.0369(10) 0.2108(8) 0.7988(7) 0.138(5) Uani 1 1 d . . . H42A H 0.0628 0.1578 0.8131 0.208 Uiso 1 1 calc R . . H42B H 0.0103 0.2112 0.7500 0.208 Uiso 1 1 calc R . . H42C H -0.0107 0.2228 0.8205 0.208 Uiso 1 1 calc R . . C43 C 0.1066(11) 0.2695(9) 0.8172(7) 0.104(4) Uani 1 1 d . . . N6 N 0.1089 -0.0241 1.0726 0.414(16) Uiso 1 1 d . . . C44 C 0.1240 -0.1116 1.1776 0.334(15) Uiso 1 1 d . . . C45 C 0.1173 -0.0596 1.1222 0.278(12) Uiso 1 1 d . . . H44A H 0.0839 -0.1572 1.1631 0.418 Uiso 1 1 d . . . H44B H 0.1064 -0.0829 1.2125 0.418 Uiso 1 1 d . . . H44C H 0.1865 -0.1302 1.1950 0.418 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0419(3) 0.0177(2) 0.0237(2) -0.0008(2) 0.00463(19) -0.0052(2) Cl1 0.0513(11) 0.0427(9) 0.0435(9) -0.0061(7) 0.0161(7) 0.0002(8) Cl2 0.0509(10) 0.0350(8) 0.0336(7) -0.0005(6) 0.0130(7) -0.0009(7) O1 0.043(2) 0.024(2) 0.028(2) 0.0013(16) -0.0009(17) -0.0065(17) O2 0.053(3) 0.0227(19) 0.0215(18) -0.0011(15) 0.0066(17) -0.0094(18) O3 0.091(4) 0.019(2) 0.048(3) -0.0004(19) -0.002(3) -0.015(2) O4 0.081(4) 0.026(2) 0.044(3) -0.0024(19) 0.001(2) -0.017(2) N1 0.041(3) 0.020(2) 0.031(2) -0.0010(19) 0.002(2) -0.005(2) N2 0.039(3) 0.016(2) 0.031(2) -0.0029(18) 0.009(2) -0.007(2) C1 0.046(4) 0.024(3) 0.031(3) -0.006(2) 0.007(3) -0.001(3) C2 0.050(4) 0.030(3) 0.031(3) 0.003(2) 0.007(3) -0.005(3) C3 0.057(5) 0.038(4) 0.041(4) 0.009(3) 0.009(3) -0.010(3) C4 0.059(5) 0.053(4) 0.034(3) 0.008(3) 0.010(3) -0.009(4) C5 0.058(5) 0.051(4) 0.029(3) 0.000(3) 0.002(3) -0.004(3) C6 0.044(4) 0.035(3) 0.031(3) -0.004(3) 0.003(3) 0.002(3) C7 0.071(6) 0.092(6) 0.039(4) 0.027(4) 0.003(4) -0.027(5) C8 0.164(13) 0.229(17) 0.098(9) 0.111(11) -0.020(8) -0.087(12) C9 0.186(16) 0.31(2) 0.131(12) 0.107(15) 0.099(12) 0.044(16) C10 0.071(8) 0.30(2) 0.213(15) 0.229(15) 0.023(9) 0.022(10) C11 0.063(5) 0.036(4) 0.035(3) -0.005(3) -0.002(3) -0.012(3) C12 0.098(7) 0.033(4) 0.071(5) -0.011(4) 0.003(5) -0.005(4) C13 0.101(7) 0.063(5) 0.050(4) 0.002(4) -0.017(4) -0.021(5) C14 0.061(5) 0.069(5) 0.066(5) 0.000(4) 0.005(4) -0.025(4) C15 0.051(4) 0.021(3) 0.039(3) 0.002(2) 0.010(3) -0.009(3) C16 0.038(4) 0.024(3) 0.036(3) -0.002(2) 0.011(3) -0.004(3) C17 0.047(4) 0.023(3) 0.034(3) 0.005(2) 0.014(3) -0.006(3) C18 0.055(4) 0.032(3) 0.033(3) 0.002(3) 0.011(3) -0.011(3) C19 0.057(5) 0.033(3) 0.038(3) 0.007(3) 0.012(3) -0.009(3) C20 0.054(4) 0.029(3) 0.051(4) 0.010(3) 0.016(3) -0.015(3) C21 0.041(4) 0.025(3) 0.041(3) 0.000(2) 0.005(3) -0.010(3) C22 0.087(6) 0.051(4) 0.043(4) 0.017(3) 0.014(4) -0.013(4) C23 0.38(2) 0.131(10) 0.039(5) 0.040(6) -0.044(9) -0.145(14) C24 0.34(2) 0.157(13) 0.086(9) 0.072(9) 0.063(12) 0.117(15) C25 0.133(12) 0.37(2) 0.087(8) 0.105(12) 0.039(8) -0.092(14) C26 0.051(4) 0.028(3) 0.051(4) -0.001(3) 0.007(3) -0.014(3) C27 0.078(6) 0.047(4) 0.076(5) 0.007(4) 0.000(4) -0.035(4) C28 0.068(5) 0.045(4) 0.061(5) -0.022(4) 0.012(4) -0.014(4) C29 0.046(5) 0.046(4) 0.073(5) 0.001(4) 0.000(4) -0.008(3) C30 0.046(4) 0.025(3) 0.028(3) 0.000(2) 0.006(3) -0.007(3) C31 0.035(3) 0.023(3) 0.029(3) -0.003(2) 0.007(2) -0.008(2) C32 0.039(4) 0.018(3) 0.033(3) -0.004(2) 0.008(3) -0.005(2) C33 0.044(4) 0.020(3) 0.032(3) 0.002(2) 0.006(3) -0.004(3) C34 0.045(4) 0.025(3) 0.038(3) -0.006(2) 0.003(3) -0.009(3) C35 0.042(4) 0.022(3) 0.037(3) -0.002(2) 0.009(3) -0.007(3) C36 0.047(4) 0.022(3) 0.036(3) 0.005(2) 0.009(3) -0.003(3) C37 0.061(5) 0.021(3) 0.046(4) -0.002(3) 0.009(3) -0.007(3) N3 0.206(14) 0.156(12) 0.131(10) 0.043(9) 0.018(10) 0.042(10) C38 0.156(11) 0.107(8) 0.065(6) 0.013(6) 0.041(7) 0.011(8) C39 0.137(11) 0.102(9) 0.088(8) 0.018(7) 0.044(7) 0.022(8) N4 0.167(13) 0.148(12) 0.192(14) -0.060(10) 0.012(10) 0.009(10) C40 0.100(9) 0.084(8) 0.154(12) -0.020(8) -0.017(8) 0.015(7) C41 0.134(13) 0.098(10) 0.136(12) -0.015(9) -0.014(10) -0.003(9) N5 0.175(14) 0.105(10) 0.202(14) -0.014(10) 0.058(11) 0.034(9) C42 0.127(12) 0.102(10) 0.162(13) -0.002(9) 0.003(10) 0.044(9) C43 0.121(12) 0.083(9) 0.103(9) 0.002(7) 0.024(8) 0.054(8) _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 Mo1 O1 1.922(4) . ? Mo1 O2 1.923(4) . ? Mo1 N1 2.131(4) . ? Mo1 N2 2.140(4) . ? Mo1 Cl1 2.3868(18) . ? Mo1 Cl2 2.4071(17) . ? O1 C1 1.329(7) . ? O2 C16 1.338(6) . ? O3 C37 1.244(7) . ? O4 C37 1.285(7) . ? N1 C15 1.300(7) . ? N1 C31 1.415(7) . ? N2 C30 1.317(7) . ? N2 C32 1.431(7) . ? C1 C2 1.423(8) . ? C1 C6 1.423(8) . ? C2 C3 1.400(8) . ? C2 C15 1.430(8) . ? C3 C4 1.366(9) . ? C4 C5 1.401(9) . ? C4 C7 1.530(9) . ? C5 C6 1.394(9) . ? C6 C11 1.531(9) . ? C7 C10 1.399(13) . ? C7 C8 1.445(14) . ? C7 C9 1.621(18) . ? C11 C14 1.521(11) . ? C11 C12 1.526(10) . ? C11 C13 1.547(9) . ? C16 C17 1.409(8) . ? C16 C21 1.414(8) . ? C17 C18 1.416(8) . ? C17 C30 1.418(8) . ? C18 C19 1.367(8) . ? C19 C20 1.398(9) . ? C19 C22 1.541(9) . ? C20 C21 1.397(8) . ? C21 C26 1.553(8) . ? C22 C23 1.455(12) . ? C22 C25 1.475(13) . ? C22 C24 1.521(15) . ? C26 C28 1.519(10) . ? C26 C29 1.536(9) . ? C26 C27 1.539(9) . ? C31 C36 1.395(7) . ? C31 C32 1.397(7) . ? C32 C33 1.391(8) . ? C33 C34 1.378(7) . ? C34 C35 1.393(8) . ? C35 C36 1.379(8) . ? C35 C37 1.498(8) . ? N3 C39 1.129(14) . ? C38 C39 1.428(15) . ? N4 C41 1.155(18) . ? C40 C41 1.44(2) . ? N5 C43 1.156(17) . ? C42 C43 1.402(18) . ? N6 C45 1.15274(14) . ? C44 C45 1.40785(17) . ? 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 Mo1 O2 114.33(15) . . ? O1 Mo1 N1 85.43(16) . . ? O2 Mo1 N1 159.09(17) . . ? O1 Mo1 N2 159.01(16) . . ? O2 Mo1 N2 85.63(15) . . ? N1 Mo1 N2 75.77(16) . . ? O1 Mo1 Cl1 86.39(13) . . ? O2 Mo1 Cl1 92.05(13) . . ? N1 Mo1 Cl1 96.17(14) . . ? N2 Mo1 Cl1 86.43(13) . . ? O1 Mo1 Cl2 91.70(13) . . ? O2 Mo1 Cl2 86.42(13) . . ? N1 Mo1 Cl2 86.19(14) . . ? N2 Mo1 Cl2 96.22(13) . . ? Cl1 Mo1 Cl2 176.83(6) . . ? C1 O1 Mo1 132.5(4) . . ? C16 O2 Mo1 132.1(3) . . ? C15 N1 C31 120.6(5) . . ? C15 N1 Mo1 122.6(4) . . ? C31 N1 Mo1 116.3(3) . . ? C30 N2 C32 119.5(5) . . ? C30 N2 Mo1 123.2(4) . . ? C32 N2 Mo1 116.5(3) . . ? O1 C1 C2 120.0(5) . . ? O1 C1 C6 120.9(5) . . ? C2 C1 C6 119.0(5) . . ? C3 C2 C1 120.2(5) . . ? C3 C2 C15 117.0(5) . . ? C1 C2 C15 122.6(5) . . ? C4 C3 C2 122.2(6) . . ? C3 C4 C5 116.7(6) . . ? C3 C4 C7 121.7(6) . . ? C5 C4 C7 121.6(6) . . ? C6 C5 C4 125.0(6) . . ? C5 C6 C1 116.8(6) . . ? C5 C6 C11 123.0(5) . . ? C1 C6 C11 120.1(5) . . ? C10 C7 C8 121.6(10) . . ? C10 C7 C4 113.3(7) . . ? C8 C7 C4 113.7(7) . . ? C10 C7 C9 103.2(11) . . ? C8 C7 C9 94.8(11) . . ? C4 C7 C9 106.5(8) . . ? C14 C11 C12 110.6(6) . . ? C14 C11 C6 110.4(6) . . ? C12 C11 C6 109.2(6) . . ? C14 C11 C13 107.0(7) . . ? C12 C11 C13 107.6(6) . . ? C6 C11 C13 112.0(6) . . ? N1 C15 C2 128.1(5) . . ? O2 C16 C17 119.5(5) . . ? O2 C16 C21 120.5(5) . . ? C17 C16 C21 120.0(5) . . ? C16 C17 C18 119.6(5) . . ? C16 C17 C30 124.3(5) . . ? C18 C17 C30 116.1(5) . . ? C19 C18 C17 122.0(6) . . ? C18 C19 C20 116.5(6) . . ? C18 C19 C22 122.0(6) . . ? C20 C19 C22 121.5(6) . . ? C21 C20 C19 125.3(5) . . ? C20 C21 C16 116.4(5) . . ? C20 C21 C26 122.4(5) . . ? C16 C21 C26 121.2(5) . . ? C23 C22 C25 112.4(11) . . ? C23 C22 C24 108.1(11) . . ? C25 C22 C24 103.8(11) . . ? C23 C22 C19 113.1(6) . . ? C25 C22 C19 110.4(7) . . ? C24 C22 C19 108.5(7) . . ? C28 C26 C29 110.9(6) . . ? C28 C26 C27 108.0(6) . . ? C29 C26 C27 107.4(6) . . ? C28 C26 C21 110.7(6) . . ? C29 C26 C21 108.8(5) . . ? C27 C26 C21 111.0(5) . . ? N2 C30 C17 127.2(5) . . ? C36 C31 C32 119.7(5) . . ? C36 C31 N1 124.1(5) . . ? C32 C31 N1 116.2(5) . . ? C33 C32 C31 120.0(5) . . ? C33 C32 N2 125.4(5) . . ? C31 C32 N2 114.6(5) . . ? C34 C33 C32 119.6(5) . . ? C33 C34 C35 120.6(5) . . ? C36 C35 C34 120.1(5) . . ? C36 C35 C37 118.5(5) . . ? C34 C35 C37 121.4(5) . . ? C35 C36 C31 119.8(5) . . ? O3 C37 O4 125.0(5) . . ? O3 C37 C35 118.5(5) . . ? O4 C37 C35 116.5(5) . . ? N3 C39 C38 176.6(15) . . ? N4 C41 C40 178.8(18) . . ? N5 C43 C42 178.3(17) . . ? N6 C45 C44 172.784(1) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.133 _refine_diff_density_min -0.990 _refine_diff_density_rms 0.098 data_c1486fin _database_code_depnum_ccdc_archive 'CCDC 736169' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H102 Cl3 Mo2 N5 O10' _chemical_formula_weight 1591.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo Mo -1.6832 0.6857 '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' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.200(6) _cell_length_b 21.509(7) _cell_length_c 20.778(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.341(7) _cell_angle_gamma 90.00 _cell_volume 8127(5) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 858 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 27.61 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3328 _exptl_absorpt_coefficient_mu 0.465 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ccd area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34850 _diffrn_reflns_av_R_equivalents 0.1551 _diffrn_reflns_av_sigmaI/netI 0.1619 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 23.25 _reflns_number_total 11649 _reflns_number_gt 5574 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1511P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11649 _refine_ls_number_parameters 806 _refine_ls_number_restraints 147 _refine_ls_R_factor_all 0.2075 _refine_ls_R_factor_gt 0.1010 _refine_ls_wR_factor_ref 0.2854 _refine_ls_wR_factor_gt 0.2306 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.002 _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 Mo1 Mo 1.01472(5) 0.82985(5) 0.52854(4) 0.0408(3) Uani 1 1 d . . . Mo2 Mo 1.03290(5) 0.67798(5) 0.58507(4) 0.0383(3) Uani 1 1 d . . . Cl1 Cl 1.13105(16) 0.83048(16) 0.48402(13) 0.0524(9) Uani 1 1 d . . . Cl2 Cl 0.91472(15) 0.68065(16) 0.62732(13) 0.0512(8) Uani 1 1 d . . . Cl3 Cl 0.77004(16) 0.83531(15) 0.80617(13) 0.0547(9) Uani 1 1 d . . . O1 O 1.0546(4) 0.8806(4) 0.5989(3) 0.043(2) Uani 1 1 d . . . O2 O 0.5912(4) 0.7874(5) 0.5029(4) 0.068(3) Uani 1 1 d . . . H1O2 H 0.5461 0.7827 0.5052 0.102 Uiso 1 1 calc R . . O3 O 0.5846(4) 0.7937(5) 0.6096(4) 0.070(3) Uani 1 1 d . . . O4 O 0.9940(3) 0.6264(4) 0.5152(3) 0.041(2) Uani 1 1 d . . . O5 O 1.4410(4) 0.7787(4) 0.6088(4) 0.068(3) Uani 1 1 d . . . H1O5 H 1.4841 0.7907 0.6062 0.103 Uiso 1 1 calc R . . O6 O 1.4514(4) 0.7659(4) 0.5027(4) 0.063(3) Uani 1 1 d . . . O7 O 0.9740(4) 0.8786(4) 0.4774(4) 0.062(2) Uani 1 1 d . . . O8 O 0.9860(4) 0.7583(4) 0.5028(3) 0.048(2) Uani 1 1 d . . . O9 O 1.0626(4) 0.7494(4) 0.6093(3) 0.042(2) Uani 1 1 d . . . O10 O 1.0709(4) 0.6283(4) 0.6380(3) 0.058(2) Uani 1 1 d . . . N1 N 0.9246(4) 0.8300(4) 0.5907(4) 0.034(2) Uani 1 1 d . . . N2 N 0.8574(5) 0.8372(4) 0.6776(4) 0.040(2) Uani 1 1 d . . . H1N2 H 0.8459 0.8415 0.7176 0.048 Uiso 1 1 calc R . . N3 N 1.1262(5) 0.6756(4) 0.5246(4) 0.041(2) Uani 1 1 d . . . N4 N 1.1954(4) 0.6703(4) 0.4401(4) 0.040(2) Uani 1 1 d . . . H1N4 H 1.2093 0.6634 0.4012 0.048 Uiso 1 1 calc R . . N5 N 0.7218(6) 0.6961(5) 0.7841(5) 0.059(3) Uani 1 1 d . . . H5N H 0.7325 0.7376 0.7897 0.071 Uiso 1 1 calc R . . C1 C 1.0514(6) 0.8820(5) 0.6654(5) 0.043(3) Uani 1 1 d . . . C2 C 1.1105(6) 0.9083(6) 0.7021(5) 0.043(3) Uani 1 1 d . . . C3 C 1.1030(6) 0.9083(6) 0.7688(5) 0.049(3) Uani 1 1 d . . . H3 H 1.1409 0.9261 0.7948 0.059 Uiso 1 1 calc R . . C4 C 1.0423(6) 0.8835(6) 0.7991(5) 0.050(3) Uani 1 1 d . . . C5 C 0.9866(6) 0.8589(5) 0.7607(5) 0.041(3) Uani 1 1 d . . . H5 H 0.9455 0.8416 0.7800 0.049 Uiso 1 1 calc R . . C6 C 0.9894(5) 0.8589(5) 0.6943(5) 0.033(3) Uani 1 1 d . . . C7 C 1.1783(6) 0.9353(6) 0.6712(6) 0.053(3) Uani 1 1 d . . . C8 C 1.2197(7) 0.8833(7) 0.6383(6) 0.072(4) Uani 1 1 d . . . H8A H 1.2332 0.8515 0.6696 0.107 Uiso 1 1 calc R . . H8B H 1.2637 0.9001 0.6201 0.107 Uiso 1 1 calc R . . H8C H 1.1884 0.8653 0.6043 0.107 Uiso 1 1 calc R . . C9 C 1.2322(7) 0.9640(7) 0.7196(6) 0.070(4) Uani 1 1 d . . . H9A H 1.2475 0.9330 0.7513 0.105 Uiso 1 1 calc R . . H9B H 1.2088 0.9985 0.7409 0.105 Uiso 1 1 calc R . . H9C H 1.2747 0.9790 0.6977 0.105 Uiso 1 1 calc R . . C10 C 1.1567(7) 0.9858(7) 0.6238(7) 0.077(4) Uani 1 1 d . . . H10A H 1.2004 1.0020 0.6045 0.115 Uiso 1 1 calc R . . H10B H 1.1321 1.0190 0.6459 0.115 Uiso 1 1 calc R . . H10C H 1.1238 0.9688 0.5903 0.115 Uiso 1 1 calc R . . C11 C 1.0400(7) 0.8833(7) 0.8733(5) 0.055(4) Uani 1 1 d . . . C12 C 0.9841(12) 0.8414(9) 0.8964(6) 0.140(9) Uani 1 1 d . . . H12A H 0.9942 0.7994 0.8822 0.210 Uiso 1 1 calc R . . H12B H 0.9361 0.8543 0.8794 0.210 Uiso 1 1 calc R . . H12C H 0.9849 0.8425 0.9431 0.210 Uiso 1 1 calc R . . C13 C 1.1123(11) 0.8589(16) 0.9040(8) 0.231(17) Uani 1 1 d . . . H13A H 1.1526 0.8847 0.8908 0.347 Uiso 1 1 calc R . . H13B H 1.1201 0.8164 0.8902 0.347 Uiso 1 1 calc R . . H13C H 1.1098 0.8601 0.9506 0.347 Uiso 1 1 calc R . . C14 C 1.0306(15) 0.9455(9) 0.8945(7) 0.178(12) Uani 1 1 d . . . H14A H 1.0698 0.9712 0.8789 0.267 Uiso 1 1 calc R . . H14B H 1.0318 0.9465 0.9412 0.267 Uiso 1 1 calc R . . H14C H 0.9836 0.9611 0.8778 0.267 Uiso 1 1 calc R . . C15 C 0.9259(6) 0.8417(5) 0.6554(5) 0.036(3) Uani 1 1 d . . . C16 C 0.8497(6) 0.8189(5) 0.5724(5) 0.037(3) Uani 1 1 d . . . C17 C 0.8182(6) 0.8046(5) 0.5134(5) 0.043(3) Uani 1 1 d . . . H17 H 0.8468 0.8006 0.4769 0.051 Uiso 1 1 calc R . . C18 C 0.7426(6) 0.7961(6) 0.5091(5) 0.053(4) Uani 1 1 d . . . H18 H 0.7191 0.7854 0.4695 0.064 Uiso 1 1 calc R . . C19 C 0.7005(6) 0.8038(5) 0.5654(5) 0.041(3) Uani 1 1 d . . . C20 C 0.7339(6) 0.8183(5) 0.6239(5) 0.045(3) Uani 1 1 d . . . H20 H 0.7061 0.8237 0.6606 0.054 Uiso 1 1 calc R . . C21 C 0.8089(5) 0.8248(5) 0.6273(4) 0.034(3) Uani 1 1 d . . . C22 C 0.6207(6) 0.7946(6) 0.5605(6) 0.051(3) Uani 1 1 d . . . C23 C 1.0043(6) 0.6117(5) 0.4534(5) 0.036(3) Uani 1 1 d . . . C24 C 0.9490(6) 0.5790(6) 0.4183(5) 0.043(3) Uani 1 1 d . . . C25 C 0.9672(6) 0.5580(6) 0.3574(5) 0.049(3) Uani 1 1 d . . . H25 H 0.9318 0.5351 0.3332 0.059 Uiso 1 1 calc R . . C26 C 1.0346(7) 0.5689(6) 0.3302(5) 0.047(3) Uani 1 1 d . . . C27 C 1.0849(6) 0.6019(5) 0.3641(5) 0.040(3) Uani 1 1 d . . . H27 H 1.1303 0.6105 0.3460 0.048 Uiso 1 1 calc R . . C28 C 1.0715(6) 0.6244(5) 0.4269(4) 0.036(3) Uani 1 1 d . . . C29 C 0.8734(6) 0.5664(6) 0.4470(5) 0.043(3) Uani 1 1 d . . . C30 C 0.8379(6) 0.6282(7) 0.4627(6) 0.066(4) Uani 1 1 d . . . H30A H 0.8696 0.6508 0.4933 0.099 Uiso 1 1 calc R . . H30B H 0.7907 0.6208 0.4813 0.099 Uiso 1 1 calc R . . H30C H 0.8309 0.6524 0.4236 0.099 Uiso 1 1 calc R . . C31 C 0.8834(6) 0.5272(7) 0.5080(6) 0.070(4) Uani 1 1 d . . . H31A H 0.9156 0.5488 0.5389 0.104 Uiso 1 1 calc R . . H31B H 0.9049 0.4875 0.4974 0.104 Uiso 1 1 calc R . . H31C H 0.8359 0.5205 0.5265 0.104 Uiso 1 1 calc R . . C32 C 0.8231(7) 0.5326(7) 0.3992(6) 0.078(5) Uani 1 1 d . . . H32A H 0.8447 0.4929 0.3885 0.117 Uiso 1 1 calc R . . H32B H 0.8164 0.5575 0.3605 0.117 Uiso 1 1 calc R . . H32C H 0.7758 0.5258 0.4180 0.117 Uiso 1 1 calc R . . C33 C 1.0530(8) 0.5374(7) 0.2648(6) 0.062(4) Uani 1 1 d . . . C34 C 0.9916(9) 0.5022(10) 0.2346(7) 0.135(9) Uani 1 1 d . . . H34A H 0.9513 0.5303 0.2237 0.202 Uiso 1 1 calc R . . H34B H 0.9753 0.4709 0.2644 0.202 Uiso 1 1 calc R . . H34C H 1.0077 0.4822 0.1958 0.202 Uiso 1 1 calc R . . C35 C 1.1129(14) 0.4899(10) 0.2780(9) 0.170(11) Uani 1 1 d . . . H35A H 1.1556 0.5101 0.2981 0.255 Uiso 1 1 calc R . . H35B H 1.1264 0.4709 0.2378 0.255 Uiso 1 1 calc R . . H35C H 1.0952 0.4580 0.3066 0.255 Uiso 1 1 calc R . . C36 C 1.0800(11) 0.5861(8) 0.2205(6) 0.128(8) Uani 1 1 d . . . H36A H 1.1203 0.6087 0.2417 0.192 Uiso 1 1 calc R . . H36B H 1.0403 0.6147 0.2093 0.192 Uiso 1 1 calc R . . H36C H 1.0969 0.5667 0.1817 0.192 Uiso 1 1 calc R . . C37 C 1.1284(6) 0.6569(5) 0.4617(5) 0.036(3) Uani 1 1 d . . . C38 C 1.1959(6) 0.6998(5) 0.5415(5) 0.034(3) Uani 1 1 d . . . C39 C 1.2252(6) 0.7224(6) 0.6005(5) 0.046(3) Uani 1 1 d . . . H39 H 1.1964 0.7239 0.6370 0.056 Uiso 1 1 calc R . . C40 C 1.2955(6) 0.7417(6) 0.6035(5) 0.050(3) Uani 1 1 d . . . H40 H 1.3163 0.7560 0.6429 0.059 Uiso 1 1 calc R . . C41 C 1.3388(6) 0.7410(6) 0.5483(5) 0.045(3) Uani 1 1 d . . . C42 C 1.3106(6) 0.7189(6) 0.4901(5) 0.047(3) Uani 1 1 d . . . H42 H 1.3387 0.7189 0.4531 0.056 Uiso 1 1 calc R . . C43 C 1.2382(5) 0.6965(5) 0.4885(5) 0.033(3) Uani 1 1 d . . . C44 C 1.4146(7) 0.7634(6) 0.5519(6) 0.047(3) Uani 1 1 d . . . C45 C 0.7250(7) 0.6847(6) 0.7121(6) 0.061(4) Uani 1 1 d . . . H45A H 0.6906 0.7132 0.6897 0.073 Uiso 1 1 calc R . . H45B H 0.7745 0.6949 0.6986 0.073 Uiso 1 1 calc R . . C46 C 0.7075(7) 0.6211(7) 0.6915(6) 0.069(4) Uani 1 1 d . . . H46A H 0.6595 0.6092 0.7074 0.082 Uiso 1 1 calc R . . H46B H 0.7445 0.5925 0.7102 0.082 Uiso 1 1 calc R . . C47 C 0.7057(8) 0.6158(8) 0.6189(6) 0.086(5) Uani 1 1 d . . . H47A H 0.7539 0.6276 0.6034 0.104 Uiso 1 1 calc R . . H47B H 0.6693 0.6451 0.6005 0.104 Uiso 1 1 calc R . . C48 C 0.6866(9) 0.5496(9) 0.5945(7) 0.107(6) Uani 1 1 d . . . H48A H 0.6863 0.5489 0.5478 0.160 Uiso 1 1 calc R . . H48B H 0.6384 0.5379 0.6087 0.160 Uiso 1 1 calc R . . H48C H 0.7230 0.5204 0.6117 0.160 Uiso 1 1 calc R . . C49 C 0.6480(8) 0.6876(7) 0.8098(6) 0.076(5) Uani 1 1 d . . . H49A H 0.6514 0.6939 0.8565 0.091 Uiso 1 1 calc R . . H49B H 0.6324 0.6445 0.8019 0.091 Uiso 1 1 calc R . . C50 C 0.5900(8) 0.7304(8) 0.7814(7) 0.086(5) Uani 1 1 d . . . H50A H 0.5791 0.7189 0.7364 0.103 Uiso 1 1 calc R . . H50B H 0.6085 0.7731 0.7823 0.103 Uiso 1 1 calc R . . C51 C 0.5191(10) 0.7269(9) 0.8189(8) 0.104(6) Uani 1 1 d . . . H51A H 0.4987 0.6848 0.8159 0.124 Uiso 1 1 calc R . . H51B H 0.5302 0.7361 0.8645 0.124 Uiso 1 1 calc R . . C52 C 0.4638(12) 0.7725(13) 0.7922(12) 0.186(11) Uani 1 1 d . . . H52A H 0.4191 0.7695 0.8159 0.279 Uiso 1 1 calc R . . H52B H 0.4529 0.7633 0.7471 0.279 Uiso 1 1 calc R . . H52C H 0.4836 0.8143 0.7963 0.279 Uiso 1 1 calc R . . C53 C 0.7788(9) 0.6624(7) 0.8237(7) 0.088(5) Uani 1 1 d . . . H53A H 0.7696 0.6177 0.8192 0.106 Uiso 1 1 calc R . . H53B H 0.7728 0.6732 0.8690 0.106 Uiso 1 1 calc R . . C54 C 0.8575(9) 0.6749(8) 0.8077(9) 0.100(6) Uani 1 1 d . . . H54A H 0.8667 0.6563 0.7657 0.120 Uiso 1 1 calc R . . H54B H 0.8645 0.7199 0.8039 0.120 Uiso 1 1 calc R . . C55 C 0.9124(12) 0.6501(9) 0.8562(8) 0.118(7) Uani 1 1 d . . . H55A H 0.9046 0.6053 0.8619 0.141 Uiso 1 1 calc R . . H55B H 0.9061 0.6705 0.8978 0.141 Uiso 1 1 calc R . . C56 C 0.9910(10) 0.6618(10) 0.8336(11) 0.145(9) Uani 1 1 d . . . H56A H 1.0265 0.6448 0.8650 0.217 Uiso 1 1 calc R . . H56B H 0.9990 0.7062 0.8293 0.217 Uiso 1 1 calc R . . H56C H 0.9969 0.6418 0.7923 0.217 Uiso 1 1 calc R . . C57 C 0.4009(9) 0.5903(8) 0.5552(8) 0.112(6) Uiso 1 1 d D . . H57 H 0.4038 0.5829 0.5108 0.134 Uiso 1 1 calc R . . C58 C 0.3356(9) 0.5817(9) 0.5862(8) 0.123(7) Uiso 1 1 d D . . H58 H 0.2930 0.5688 0.5628 0.148 Uiso 1 1 calc R . . C59 C 0.3336(9) 0.5919(8) 0.6496(8) 0.111(6) Uiso 1 1 d D . . H59 H 0.2889 0.5856 0.6697 0.133 Uiso 1 1 calc R . . C60 C 0.3921(10) 0.6107(9) 0.6860(8) 0.127(7) Uiso 1 1 d D . . H60 H 0.3880 0.6181 0.7303 0.152 Uiso 1 1 calc R . . C61 C 0.4591(10) 0.6191(9) 0.6567(8) 0.126(7) Uiso 1 1 d D . . H61 H 0.5016 0.6307 0.6809 0.151 Uiso 1 1 calc R . . C62 C 0.4610(9) 0.6098(8) 0.5912(8) 0.109(6) Uiso 1 1 d D . . H62 H 0.5052 0.6171 0.5706 0.131 Uiso 1 1 calc R . . C63 C 0.8633(10) 1.0057(9) 0.6025(8) 0.125(7) Uiso 1 1 d D . . H63 H 0.8495 1.0056 0.5584 0.150 Uiso 1 1 calc R . . C64 C 0.8133(10) 0.9883(9) 0.6489(9) 0.133(7) Uiso 1 1 d D . . H64 H 0.7640 0.9789 0.6375 0.159 Uiso 1 1 calc R . . C65 C 0.8391(9) 0.9855(8) 0.7103(8) 0.113(6) Uiso 1 1 d D . . H65 H 0.8071 0.9708 0.7412 0.135 Uiso 1 1 calc R . . C66 C 0.9070(10) 1.0022(9) 0.7309(8) 0.124(7) Uiso 1 1 d D . . H66 H 0.9214 0.9987 0.7748 0.148 Uiso 1 1 calc R . . C67 C 0.9549(10) 1.0243(9) 0.6877(9) 0.133(7) Uiso 1 1 d D . . H67 H 1.0012 1.0398 0.7012 0.160 Uiso 1 1 calc R . . C68 C 0.9328(10) 1.0230(9) 0.6234(9) 0.134(7) Uiso 1 1 d D . . H68 H 0.9668 1.0344 0.5927 0.161 Uiso 1 1 calc R . . C69 C 0.764(2) 0.750(2) 0.307(2) 0.126(16) Uiso 0.51(3) 1 d PD A 1 H69 H 0.7937 0.7143 0.3120 0.151 Uiso 0.51(3) 1 calc PR A 1 C70 C 0.7870(15) 0.807(3) 0.3312(14) 0.093(12) Uiso 0.51(3) 1 d PD A 1 H70 H 0.8325 0.8112 0.3538 0.112 Uiso 0.51(3) 1 calc PR A 1 C71 C 0.742(3) 0.8570(19) 0.321(2) 0.114(15) Uiso 0.51(3) 1 d PD A 1 H71 H 0.7587 0.8955 0.3378 0.137 Uiso 0.51(3) 1 calc PR A 1 C72 C 0.676(2) 0.8550(16) 0.290(2) 0.126(15) Uiso 0.51(3) 1 d PD A 1 H72 H 0.6467 0.8910 0.2843 0.151 Uiso 0.51(3) 1 calc PR A 1 C73 C 0.6517(14) 0.798(2) 0.2664(13) 0.068(10) Uiso 0.51(3) 1 d PD A 1 H73 H 0.6057 0.7946 0.2443 0.081 Uiso 0.51(3) 1 calc PR A 1 C74 C 0.696(3) 0.7471(14) 0.276(2) 0.098(15) Uiso 0.51(3) 1 d PD A 1 H74 H 0.6793 0.7084 0.2600 0.117 Uiso 0.51(3) 1 calc PR A 1 C69F C 0.731(3) 0.7358(11) 0.3009(15) 0.093(12) Uiso 0.49(3) 1 d PD A 2 H69F H 0.7380 0.6925 0.2985 0.112 Uiso 0.49(3) 1 calc PR A 2 C70F C 0.672(2) 0.764(2) 0.2688(13) 0.064(10) Uiso 0.49(3) 1 d PD A 2 H70F H 0.6372 0.7404 0.2456 0.076 Uiso 0.49(3) 1 calc PR A 2 C71F C 0.6660(18) 0.827(2) 0.2711(16) 0.082(11) Uiso 0.49(3) 1 d PD A 2 H71F H 0.6266 0.8460 0.2480 0.099 Uiso 0.49(3) 1 calc PR A 2 C72F C 0.714(3) 0.8633(13) 0.3055(17) 0.108(15) Uiso 0.49(3) 1 d PD A 2 H72F H 0.7080 0.9067 0.3063 0.129 Uiso 0.49(3) 1 calc PR A 2 C73F C 0.772(2) 0.8360(17) 0.3391(13) 0.074(11) Uiso 0.49(3) 1 d PD A 2 H73F H 0.8060 0.8603 0.3636 0.089 Uiso 0.49(3) 1 calc PR A 2 C74F C 0.7803(15) 0.7721(19) 0.3365(14) 0.074(11) Uiso 0.49(3) 1 d PD A 2 H74F H 0.8198 0.7532 0.3595 0.089 Uiso 0.49(3) 1 calc PR A 2 C75 C 0.3715(15) 1.0525(10) 0.5362(11) 0.199(11) Uiso 1 1 d D . . H75 H 0.3723 1.0950 0.5469 0.238 Uiso 1 1 calc R . . C76 C 0.4258(15) 1.0126(15) 0.5599(13) 0.43(3) Uiso 1 1 d D . . H76 H 0.4657 1.0284 0.5850 0.516 Uiso 1 1 calc R . . C77 C 0.4216(14) 0.9509(14) 0.5471(12) 0.295(19) Uiso 1 1 d D . . H77 H 0.4591 0.9248 0.5639 0.354 Uiso 1 1 calc R . . C78 C 0.3658(14) 0.9253(10) 0.5112(10) 0.171(10) Uiso 1 1 d D . . H78 H 0.3632 0.8822 0.5040 0.206 Uiso 1 1 calc R . . C79 C 0.3130(13) 0.9650(13) 0.4855(10) 0.225(14) Uiso 1 1 d D . . H79 H 0.2737 0.9487 0.4600 0.270 Uiso 1 1 calc R . . C80 C 0.3165(13) 1.0284(12) 0.4966(11) 0.206(12) Uiso 1 1 d D . . H80 H 0.2812 1.0550 0.4770 0.247 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0286(6) 0.0640(8) 0.0309(6) 0.0002(5) 0.0149(4) -0.0025(6) Mo2 0.0271(6) 0.0599(8) 0.0290(5) -0.0021(5) 0.0137(4) -0.0023(5) Cl1 0.0411(18) 0.077(2) 0.0408(16) 0.0016(15) 0.0229(13) -0.0024(17) Cl2 0.0362(17) 0.072(2) 0.0472(17) -0.0043(15) 0.0231(13) -0.0068(16) Cl3 0.0485(19) 0.075(2) 0.0426(16) -0.0044(16) 0.0267(14) -0.0046(17) O1 0.032(4) 0.057(6) 0.042(4) 0.004(4) 0.013(3) -0.002(4) O2 0.027(5) 0.126(9) 0.052(6) -0.003(5) -0.001(4) -0.011(5) O3 0.028(5) 0.129(9) 0.056(6) -0.011(5) 0.016(4) -0.007(5) O4 0.021(4) 0.067(6) 0.037(4) 0.002(4) 0.016(3) -0.003(4) O5 0.026(5) 0.120(9) 0.059(6) -0.011(5) 0.006(4) -0.012(5) O6 0.025(5) 0.110(8) 0.055(5) 0.000(5) 0.017(4) -0.007(5) O7 0.052(5) 0.074(7) 0.062(5) 0.002(5) 0.029(4) -0.004(5) O8 0.028(4) 0.092(7) 0.026(4) 0.000(4) 0.016(3) 0.019(4) O9 0.028(4) 0.073(6) 0.027(4) -0.004(4) 0.017(3) 0.009(4) O10 0.041(5) 0.081(7) 0.052(5) 0.003(5) 0.020(4) 0.002(5) N1 0.027(5) 0.032(6) 0.043(5) -0.003(4) 0.003(4) -0.005(4) N2 0.031(5) 0.061(7) 0.029(5) -0.012(4) 0.011(4) -0.006(5) N3 0.032(6) 0.052(7) 0.040(5) -0.008(5) 0.002(4) 0.000(5) N4 0.024(5) 0.073(7) 0.025(5) -0.007(5) 0.021(4) 0.001(5) N5 0.059(7) 0.069(8) 0.051(7) 0.008(5) 0.021(6) -0.015(6) C1 0.039(7) 0.050(9) 0.040(7) -0.014(6) 0.017(6) -0.003(6) C2 0.027(7) 0.051(8) 0.050(7) -0.003(6) -0.003(5) 0.001(6) C3 0.035(7) 0.072(10) 0.043(7) -0.009(6) 0.011(6) -0.011(6) C4 0.034(7) 0.074(10) 0.043(7) -0.011(6) 0.001(6) 0.000(7) C5 0.039(7) 0.047(8) 0.037(7) -0.003(6) 0.010(5) -0.005(6) C6 0.018(6) 0.049(8) 0.033(6) -0.001(5) 0.008(5) -0.008(5) C7 0.033(7) 0.063(10) 0.066(8) -0.020(7) 0.019(6) -0.019(7) C8 0.047(8) 0.092(12) 0.078(9) -0.037(8) 0.022(7) -0.008(8) C9 0.050(9) 0.093(12) 0.068(9) -0.018(8) 0.030(7) -0.021(8) C10 0.053(9) 0.079(12) 0.099(11) -0.006(9) 0.026(8) -0.026(8) C11 0.055(9) 0.077(11) 0.033(7) -0.008(7) 0.020(6) -0.021(7) C12 0.22(2) 0.17(2) 0.026(8) -0.008(9) 0.010(10) -0.120(18) C13 0.093(16) 0.55(6) 0.051(11) 0.05(2) -0.001(10) 0.04(2) C14 0.39(4) 0.094(17) 0.058(11) -0.026(11) 0.083(17) -0.03(2) C15 0.031(7) 0.044(8) 0.035(6) -0.008(5) 0.012(5) -0.001(5) C16 0.027(7) 0.048(8) 0.038(6) 0.000(6) 0.008(5) 0.001(6) C17 0.028(7) 0.061(9) 0.040(7) -0.001(6) 0.011(5) -0.003(6) C18 0.033(8) 0.093(11) 0.036(7) 0.001(6) 0.017(5) -0.006(7) C19 0.021(6) 0.059(9) 0.044(7) -0.002(6) 0.003(5) -0.011(6) C20 0.028(7) 0.061(9) 0.048(7) -0.001(6) 0.018(5) -0.001(6) C21 0.029(7) 0.047(8) 0.026(6) 0.004(5) 0.007(5) 0.000(6) C22 0.025(7) 0.083(10) 0.045(8) -0.003(7) 0.003(6) -0.007(6) C23 0.036(7) 0.047(8) 0.026(6) 0.003(5) 0.006(5) 0.015(6) C24 0.036(7) 0.058(9) 0.035(7) 0.001(6) 0.008(5) -0.002(6) C25 0.038(8) 0.061(9) 0.048(8) 0.001(6) 0.000(6) -0.004(6) C26 0.059(9) 0.055(9) 0.029(6) -0.010(6) 0.021(6) -0.002(7) C27 0.040(7) 0.054(9) 0.027(6) -0.007(5) 0.014(5) -0.011(6) C28 0.033(7) 0.046(8) 0.029(6) -0.010(5) 0.016(5) 0.000(6) C29 0.028(7) 0.052(9) 0.051(7) -0.009(6) 0.015(5) -0.017(6) C30 0.032(7) 0.103(13) 0.064(9) 0.016(8) 0.020(6) 0.003(8) C31 0.031(7) 0.087(12) 0.092(10) 0.034(8) 0.027(7) -0.017(7) C32 0.041(8) 0.110(14) 0.085(10) -0.031(9) 0.018(7) -0.022(8) C33 0.079(10) 0.066(11) 0.042(8) -0.021(7) 0.019(7) -0.012(8) C34 0.098(14) 0.24(2) 0.070(11) -0.082(14) 0.030(10) -0.062(15) C35 0.25(3) 0.16(2) 0.106(16) -0.066(15) 0.015(17) 0.09(2) C36 0.21(2) 0.133(17) 0.041(9) -0.010(9) 0.059(11) -0.047(15) C37 0.027(7) 0.045(8) 0.035(6) -0.012(5) 0.006(5) -0.009(5) C38 0.021(6) 0.047(8) 0.036(6) 0.004(5) 0.006(5) 0.011(5) C39 0.022(7) 0.077(10) 0.042(7) -0.017(6) 0.012(5) -0.008(6) C40 0.036(8) 0.064(10) 0.048(7) -0.001(6) 0.000(6) 0.006(6) C41 0.030(7) 0.060(9) 0.044(7) -0.004(6) 0.003(5) -0.006(6) C42 0.024(7) 0.066(9) 0.051(8) -0.001(6) 0.008(5) -0.002(6) C43 0.019(6) 0.047(8) 0.032(6) -0.001(5) 0.000(5) 0.004(5) C44 0.042(8) 0.050(9) 0.049(8) 0.003(6) -0.002(6) 0.004(6) C45 0.053(8) 0.081(12) 0.050(8) -0.004(7) 0.019(6) -0.018(8) C46 0.069(10) 0.087(12) 0.051(8) -0.009(8) 0.020(7) -0.018(8) C47 0.076(11) 0.120(15) 0.065(10) -0.022(9) 0.022(8) -0.033(10) C48 0.081(12) 0.18(2) 0.065(10) -0.034(11) 0.029(8) -0.038(12) C49 0.080(11) 0.110(14) 0.040(8) -0.007(8) 0.038(7) -0.030(10) C50 0.051(10) 0.129(16) 0.080(11) 0.004(10) 0.024(8) -0.017(10) C51 0.085(14) 0.137(19) 0.090(12) 0.003(11) 0.030(10) -0.021(12) C52 0.096(18) 0.26(4) 0.20(3) 0.04(2) 0.072(17) 0.00(2) C53 0.127(16) 0.087(13) 0.053(9) 0.006(8) 0.024(10) -0.014(11) C54 0.096(14) 0.084(14) 0.125(15) -0.009(11) 0.049(12) 0.009(11) C55 0.139(19) 0.125(18) 0.086(13) -0.036(11) -0.028(13) 0.036(14) C56 0.075(14) 0.18(2) 0.18(2) -0.078(17) -0.008(14) 0.016(14) _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 Mo1 O7 1.647(8) . ? Mo1 O8 1.703(8) . ? Mo1 O1 1.941(7) . ? Mo1 N1 2.129(8) . ? Mo1 Cl1 2.345(3) . ? Mo2 O10 1.664(8) . ? Mo2 O9 1.699(8) . ? Mo2 O4 1.938(7) . ? Mo2 N3 2.153(9) . ? Mo2 Cl2 2.357(3) . ? O1 C1 1.384(11) . ? O2 C22 1.300(13) . ? O3 C22 1.236(13) . ? O4 C23 1.343(11) . ? O5 C44 1.301(12) . ? O6 C44 1.244(13) . ? N1 C15 1.366(12) . ? N1 C16 1.421(13) . ? N2 C15 1.351(12) . ? N2 C21 1.365(12) . ? N3 C37 1.370(12) . ? N3 C38 1.403(13) . ? N4 C37 1.348(12) . ? N4 C43 1.368(12) . ? N5 C49 1.477(15) . ? N5 C53 1.486(17) . ? N5 C45 1.519(14) . ? C1 C6 1.391(14) . ? C1 C2 1.412(14) . ? C2 C3 1.399(14) . ? C2 C7 1.528(15) . ? C3 C4 1.399(15) . ? C4 C5 1.369(14) . ? C4 C11 1.544(15) . ? C5 C6 1.384(13) . ? C6 C15 1.431(13) . ? C7 C9 1.508(16) . ? C7 C10 1.508(18) . ? C7 C8 1.525(16) . ? C11 C14 1.42(2) . ? C11 C12 1.455(18) . ? C11 C13 1.53(2) . ? C16 C17 1.367(14) . ? C16 C21 1.393(13) . ? C17 C18 1.387(14) . ? C18 C19 1.434(14) . ? C19 C20 1.372(14) . ? C19 C22 1.465(15) . ? C20 C21 1.372(14) . ? C23 C28 1.388(14) . ? C23 C24 1.407(14) . ? C24 C25 1.396(15) . ? C24 C29 1.548(14) . ? C25 C26 1.390(15) . ? C26 C27 1.336(15) . ? C26 C33 1.568(15) . ? C27 C28 1.421(13) . ? C28 C37 1.422(14) . ? C29 C32 1.509(15) . ? C29 C30 1.518(17) . ? C29 C31 1.525(16) . ? C33 C34 1.469(18) . ? C33 C36 1.492(19) . ? C33 C35 1.51(2) . ? C38 C43 1.371(13) . ? C38 C39 1.403(14) . ? C39 C40 1.344(14) . ? C40 C41 1.419(15) . ? C41 C42 1.377(14) . ? C41 C44 1.460(15) . ? C42 C43 1.404(14) . ? C45 C46 1.464(16) . ? C46 C47 1.513(16) . ? C47 C48 1.55(2) . ? C49 C50 1.503(19) . ? C50 C51 1.536(19) . ? C51 C52 1.50(3) . ? C53 C54 1.507(19) . ? C54 C55 1.49(2) . ? C55 C56 1.55(2) . ? C57 C62 1.364(14) . ? C57 C58 1.388(14) . ? C58 C59 1.337(14) . ? C59 C60 1.342(14) . ? C60 C61 1.398(14) . ? C61 C62 1.377(14) . ? C63 C68 1.373(14) . ? C63 C64 1.402(15) . ? C64 C65 1.343(14) . ? C65 C66 1.340(14) . ? C66 C67 1.362(15) . ? C67 C68 1.379(14) . ? C69 C74 1.373(13) . ? C69 C70 1.388(13) . ? C70 C71 1.356(13) . ? C71 C72 1.358(13) . ? C72 C73 1.378(13) . ? C73 C74 1.376(13) . ? C69F C74F 1.376(13) . ? C69F C70F 1.384(13) . ? C70F C71F 1.355(13) . ? C71F C72F 1.356(13) . ? C72F C73F 1.376(13) . ? C73F C74F 1.382(13) . ? C75 C80 1.371(13) . ? C75 C76 1.384(13) . ? C76 C77 1.355(13) . ? C77 C78 1.352(13) . ? C78 C79 1.377(13) . ? C79 C80 1.384(13) . ? 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 O7 Mo1 O8 104.4(4) . . ? O7 Mo1 O1 105.8(4) . . ? O8 Mo1 O1 147.6(3) . . ? O7 Mo1 N1 93.1(3) . . ? O8 Mo1 N1 87.6(3) . . ? O1 Mo1 N1 79.4(3) . . ? O7 Mo1 Cl1 97.6(3) . . ? O8 Mo1 Cl1 98.7(2) . . ? O1 Mo1 Cl1 88.8(2) . . ? N1 Mo1 Cl1 165.9(2) . . ? O10 Mo2 O9 105.5(4) . . ? O10 Mo2 O4 104.9(4) . . ? O9 Mo2 O4 147.3(3) . . ? O10 Mo2 N3 93.1(3) . . ? O9 Mo2 N3 86.8(3) . . ? O4 Mo2 N3 79.8(3) . . ? O10 Mo2 Cl2 97.5(3) . . ? O9 Mo2 Cl2 98.7(2) . . ? O4 Mo2 Cl2 89.0(2) . . ? N3 Mo2 Cl2 166.2(2) . . ? C1 O1 Mo1 137.2(7) . . ? C23 O4 Mo2 142.2(7) . . ? C15 N1 C16 105.8(8) . . ? C15 N1 Mo1 127.9(7) . . ? C16 N1 Mo1 126.2(7) . . ? C15 N2 C21 109.3(8) . . ? C37 N3 C38 106.7(8) . . ? C37 N3 Mo2 128.1(7) . . ? C38 N3 Mo2 124.9(7) . . ? C37 N4 C43 109.8(8) . . ? C49 N5 C53 111.3(11) . . ? C49 N5 C45 114.0(10) . . ? C53 N5 C45 114.4(11) . . ? O1 C1 C6 119.4(9) . . ? O1 C1 C2 119.0(10) . . ? C6 C1 C2 121.6(10) . . ? C3 C2 C1 115.6(10) . . ? C3 C2 C7 122.0(10) . . ? C1 C2 C7 122.4(10) . . ? C2 C3 C4 123.8(10) . . ? C5 C4 C3 117.7(10) . . ? C5 C4 C11 122.1(11) . . ? C3 C4 C11 120.2(10) . . ? C4 C5 C6 121.7(10) . . ? C5 C6 C1 119.6(10) . . ? C5 C6 C15 120.2(9) . . ? C1 C6 C15 119.9(9) . . ? C9 C7 C10 106.6(11) . . ? C9 C7 C8 106.2(10) . . ? C10 C7 C8 110.8(11) . . ? C9 C7 C2 112.9(10) . . ? C10 C7 C2 110.8(10) . . ? C8 C7 C2 109.4(11) . . ? C14 C11 C12 112.7(15) . . ? C14 C11 C13 107.8(17) . . ? C12 C11 C13 104.4(16) . . ? C14 C11 C4 108.4(12) . . ? C12 C11 C4 112.3(10) . . ? C13 C11 C4 111.1(11) . . ? N2 C15 N1 110.1(9) . . ? N2 C15 C6 124.1(9) . . ? N1 C15 C6 125.7(9) . . ? C17 C16 C21 122.5(10) . . ? C17 C16 N1 129.9(9) . . ? C21 C16 N1 107.6(9) . . ? C16 C17 C18 117.8(10) . . ? C17 C18 C19 119.6(10) . . ? C20 C19 C18 121.1(10) . . ? C20 C19 C22 119.6(10) . . ? C18 C19 C22 119.2(10) . . ? C21 C20 C19 118.2(10) . . ? N2 C21 C20 132.1(9) . . ? N2 C21 C16 107.2(9) . . ? C20 C21 C16 120.7(10) . . ? O3 C22 O2 122.9(10) . . ? O3 C22 C19 120.2(11) . . ? O2 C22 C19 116.9(10) . . ? O4 C23 C28 119.5(9) . . ? O4 C23 C24 119.2(9) . . ? C28 C23 C24 121.1(9) . . ? C25 C24 C23 116.1(10) . . ? C25 C24 C29 122.7(10) . . ? C23 C24 C29 121.1(9) . . ? C26 C25 C24 123.9(11) . . ? C27 C26 C25 118.2(10) . . ? C27 C26 C33 121.3(11) . . ? C25 C26 C33 120.1(11) . . ? C26 C27 C28 121.7(10) . . ? C23 C28 C27 118.9(10) . . ? C23 C28 C37 122.0(9) . . ? C27 C28 C37 119.1(9) . . ? C32 C29 C30 108.1(10) . . ? C32 C29 C31 109.2(11) . . ? C30 C29 C31 110.0(10) . . ? C32 C29 C24 110.8(9) . . ? C30 C29 C24 108.7(9) . . ? C31 C29 C24 109.9(9) . . ? C34 C33 C36 111.2(13) . . ? C34 C33 C35 105.1(15) . . ? C36 C33 C35 109.6(16) . . ? C34 C33 C26 114.0(12) . . ? C36 C33 C26 108.6(12) . . ? C35 C33 C26 108.3(11) . . ? N4 C37 N3 108.4(8) . . ? N4 C37 C28 125.8(9) . . ? N3 C37 C28 125.5(9) . . ? C43 C38 C39 120.9(10) . . ? C43 C38 N3 108.1(9) . . ? C39 C38 N3 130.9(9) . . ? C40 C39 C38 118.4(10) . . ? C39 C40 C41 121.2(11) . . ? C42 C41 C40 121.0(10) . . ? C42 C41 C44 118.4(10) . . ? C40 C41 C44 120.6(10) . . ? C41 C42 C43 117.0(10) . . ? N4 C43 C38 106.9(9) . . ? N4 C43 C42 131.7(10) . . ? C38 C43 C42 121.4(10) . . ? O6 C44 O5 123.0(11) . . ? O6 C44 C41 120.7(11) . . ? O5 C44 C41 116.3(10) . . ? C46 C45 N5 115.0(10) . . ? C45 C46 C47 111.0(11) . . ? C46 C47 C48 113.1(13) . . ? N5 C49 C50 114.6(11) . . ? C49 C50 C51 111.3(13) . . ? C52 C51 C50 110.3(15) . . ? N5 C53 C54 116.1(12) . . ? C55 C54 C53 113.9(16) . . ? C54 C55 C56 109.9(17) . . ? C62 C57 C58 117.9(15) . . ? C59 C58 C57 119.6(15) . . ? C58 C59 C60 123.5(16) . . ? C59 C60 C61 118.6(16) . . ? C62 C61 C60 118.0(15) . . ? C57 C62 C61 122.3(15) . . ? C68 C63 C64 118.0(15) . . ? C65 C64 C63 117.0(16) . . ? C66 C65 C64 125.1(16) . . ? C65 C66 C67 119.2(16) . . ? C66 C67 C68 117.6(16) . . ? C63 C68 C67 122.7(16) . . ? C74 C69 C70 117.5(19) . . ? C71 C70 C69 119(2) . . ? C70 C71 C72 125(2) . . ? C71 C72 C73 117(2) . . ? C74 C73 C72 119.0(18) . . ? C69 C74 C73 123(2) . . ? C74F C69F C70F 118.7(18) . . ? C71F C70F C69F 119.3(18) . . ? C70F C71F C72F 123(2) . . ? C71F C72F C73F 119(2) . . ? C72F C73F C74F 119.1(18) . . ? C69F C74F C73F 121.2(19) . . ? C80 C75 C76 118.2(19) . . ? C77 C76 C75 120(2) . . ? C78 C77 C76 123(2) . . ? C77 C78 C79 117.3(19) . . ? C78 C79 C80 121.3(19) . . ? C75 C80 C79 120.0(19) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.677 _refine_diff_density_min -1.126 _refine_diff_density_rms 0.145 data_c2176fin _database_code_depnum_ccdc_archive 'CCDC 736170' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C158.50 H206 B4 Fe2 La2 N28 O9' _chemical_formula_weight 3080.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.2894(11) _cell_length_b 24.0058(13) _cell_length_c 36.938(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.8210(10) _cell_angle_gamma 90.00 _cell_volume 16741.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 7826 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 26.36 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6444 _exptl_absorpt_coefficient_mu 0.731 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 CCD area detector' _diffrn_measurement_method '\F scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83559 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_sigmaI/netI 0.1051 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 26.46 _reflns_number_total 29634 _reflns_number_gt 17033 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXH-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0896P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 29634 _refine_ls_number_parameters 1794 _refine_ls_number_restraints 228 _refine_ls_R_factor_all 0.1303 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.1729 _refine_ls_wR_factor_gt 0.1504 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.005 _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 La1 La 0.128449(17) 0.277717(18) 1.031146(11) 0.04308(12) Uani 1 1 d . . . La2 La 0.074472(15) 0.508208(15) 0.742918(10) 0.03323(11) Uani 1 1 d . . . Fe1 Fe -0.30757(4) 0.38600(4) 0.87189(2) 0.0350(2) Uani 1 1 d . . . Fe2 Fe -0.28389(4) 0.27885(4) 0.81314(3) 0.0364(2) Uani 1 1 d . . . O1 O -0.34539(17) 0.44972(17) 0.84351(12) 0.0387(10) Uani 1 1 d . . . O2 O -0.38198(19) 0.38283(18) 0.89895(12) 0.0460(11) Uani 1 1 d . . . O3 O 0.07666(19) 0.3453(2) 0.98199(12) 0.0523(13) Uani 1 1 d . . . O4 O -0.00103(19) 0.2882(2) 0.99881(12) 0.0481(12) Uani 1 1 d . . . O5 O -0.29177(19) 0.20929(17) 0.83779(12) 0.0403(11) Uani 1 1 d . . . O6 O -0.35297(18) 0.26309(17) 0.76943(13) 0.0437(11) Uani 1 1 d . . . O7 O -0.04153(18) 0.46477(18) 0.75204(12) 0.0439(11) Uani 1 1 d . . . O8 O 0.05760(17) 0.42336(17) 0.77978(11) 0.0386(10) Uani 1 1 d . . . O9 O -0.31484(18) 0.32928(17) 0.84075(12) 0.0439(11) Uani 1 1 d . . . N1 N -0.2076(2) 0.4202(2) 0.86945(14) 0.0338(12) Uani 1 1 d . . . N2 N -0.2417(2) 0.3551(2) 0.92022(13) 0.0345(12) Uani 1 1 d . . . N3 N 0.1317(3) 0.3994(2) 1.06457(15) 0.0487(14) Uani 1 1 d . . . N4 N 0.0779(3) 0.3631(2) 1.06829(16) 0.0534(16) Uani 1 1 d . . . N5 N 0.2548(3) 0.3824(3) 1.05331(17) 0.0532(16) Uani 1 1 d . . . N6 N 0.2339(3) 0.3427(3) 1.02661(15) 0.0498(15) Uani 1 1 d . . . N7 N 0.2203(2) 0.3417(2) 1.11039(14) 0.0405(13) Uani 1 1 d . . . N8 N 0.1984(3) 0.2889(2) 1.09917(15) 0.0468(14) Uani 1 1 d . . . N9 N 0.2165(3) 0.1467(3) 1.0298(2) 0.076(2) Uani 1 1 d . . . N10 N 0.2338(3) 0.2007(3) 1.04099(17) 0.0575(17) Uani 1 1 d . . . N11 N 0.0944(3) 0.1359(3) 1.0452(2) 0.0633(18) Uani 1 1 d . . . N12 N 0.0766(3) 0.1883(3) 1.05470(17) 0.0551(16) Uani 1 1 d . . . N13 N 0.1071(4) 0.1543(5) 0.9794(3) 0.110(4) Uani 1 1 d . . . N14 N 0.1143(4) 0.2092(5) 0.9720(2) 0.095(3) Uani 1 1 d . . . N15 N -0.1752(2) 0.2740(2) 0.83687(14) 0.0342(12) Uani 1 1 d . . . N16 N -0.2366(2) 0.3306(2) 0.77836(13) 0.0328(12) Uani 1 1 d . . . N17 N 0.0142(2) 0.6060(2) 0.79691(13) 0.0363(12) Uani 1 1 d . . . N18 N 0.0514(2) 0.5568(2) 0.80435(14) 0.0402(13) Uani 1 1 d . . . N19 N 0.1063(2) 0.6507(2) 0.76545(14) 0.0345(12) Uani 1 1 d . . . N20 N 0.1429(2) 0.6057(2) 0.75537(14) 0.0399(13) Uani 1 1 d . . . N21 N -0.0183(2) 0.6347(2) 0.72915(14) 0.0380(13) Uani 1 1 d . . . N22 N -0.0155(2) 0.5837(2) 0.71296(14) 0.0385(13) Uani 1 1 d . . . N23 N 0.2302(2) 0.4390(2) 0.73726(15) 0.0416(14) Uani 1 1 d . . . N24 N 0.2038(2) 0.4685(2) 0.76273(15) 0.0451(14) Uani 1 1 d . . . N25 N 0.1715(2) 0.4820(2) 0.67567(14) 0.0386(13) Uani 1 1 d . . . N26 N 0.1327(2) 0.5250(2) 0.68533(15) 0.0392(13) Uani 1 1 d . . . N27 N 0.1140(2) 0.3995(2) 0.70136(14) 0.0385(13) Uani 1 1 d . . . N28 N 0.0486(2) 0.4246(2) 0.69165(15) 0.0431(14) Uani 1 1 d . . . C1 C -0.2513(3) 0.4716(2) 0.81312(16) 0.0319(14) Uani 1 1 d . . . C2 C -0.3250(3) 0.4699(2) 0.81424(18) 0.0347(15) Uani 1 1 d . . . C3 C -0.3743(3) 0.4927(2) 0.78415(17) 0.0346(14) Uani 1 1 d . . . C4 C -0.3489(3) 0.5178(3) 0.75593(17) 0.0406(16) Uani 1 1 d . . . H4 H -0.3821 0.5327 0.7361 0.049 Uiso 1 1 calc R . . C5 C -0.2765(3) 0.5228(3) 0.75476(18) 0.0422(17) Uani 1 1 d . . . C6 C -0.2289(3) 0.4989(3) 0.78342(17) 0.0386(16) Uani 1 1 d . . . H6 H -0.1803 0.5008 0.7833 0.046 Uiso 1 1 calc R . . C7 C -0.4541(3) 0.4879(3) 0.78347(18) 0.0426(16) Uani 1 1 d . . . C8 C -0.4733(3) 0.4258(3) 0.7843(2) 0.057(2) Uani 1 1 d . . . H8A H -0.4615 0.4072 0.7631 0.086 Uiso 1 1 calc R . . H8B H -0.5236 0.4221 0.7836 0.086 Uiso 1 1 calc R . . H8C H -0.4468 0.4091 0.8068 0.086 Uiso 1 1 calc R . . C9 C -0.4730(3) 0.5188(3) 0.8167(2) 0.057(2) Uani 1 1 d . . . H9A H -0.4465 0.5029 0.8395 0.086 Uiso 1 1 calc R . . H9B H -0.5233 0.5151 0.8160 0.086 Uiso 1 1 calc R . . H9C H -0.4610 0.5579 0.8155 0.086 Uiso 1 1 calc R . . C10 C -0.4990(3) 0.5138(3) 0.74810(19) 0.062(2) Uani 1 1 d . . . H10A H -0.4910 0.5537 0.7483 0.093 Uiso 1 1 calc R . . H10B H -0.5487 0.5065 0.7473 0.093 Uiso 1 1 calc R . . H10C H -0.4854 0.4975 0.7265 0.093 Uiso 1 1 calc R . . C11 C -0.2511(3) 0.5544(3) 0.7242(2) 0.0516(19) Uani 1 1 d . . . C12 C -0.2173(5) 0.5127(4) 0.7011(2) 0.092(3) Uani 1 1 d . . . H12A H -0.2097 0.5308 0.6788 0.138 Uiso 1 1 calc R . . H12B H -0.2488 0.4811 0.6945 0.138 Uiso 1 1 calc R . . H12C H -0.1724 0.4999 0.7155 0.138 Uiso 1 1 calc R . . C13 C -0.1967(5) 0.5976(4) 0.7403(2) 0.097(3) Uani 1 1 d . . . H13A H -0.2153 0.6208 0.7576 0.145 Uiso 1 1 calc R . . H13B H -0.1859 0.6205 0.7206 0.145 Uiso 1 1 calc R . . H13C H -0.1539 0.5791 0.7532 0.145 Uiso 1 1 calc R . . C14 C -0.3122(4) 0.5819(4) 0.6970(3) 0.104(4) Uani 1 1 d . . . H14A H -0.3360 0.6084 0.7100 0.156 Uiso 1 1 calc R . . H14B H -0.3456 0.5535 0.6857 0.156 Uiso 1 1 calc R . . H14C H -0.2936 0.6010 0.6779 0.156 Uiso 1 1 calc R . . C15 C -0.1976(3) 0.4490(3) 0.84151(17) 0.0348(15) Uani 1 1 d . . . H15 H -0.1504 0.4556 0.8397 0.042 Uiso 1 1 calc R . . C16 C -0.3386(3) 0.3161(3) 0.94566(18) 0.0453(17) Uani 1 1 d . . . C17 C -0.3939(3) 0.3468(3) 0.92342(18) 0.0421(16) Uani 1 1 d . . . C18 C -0.4643(3) 0.3388(3) 0.9290(2) 0.0504(19) Uani 1 1 d . . . C19 C -0.4747(3) 0.3027(3) 0.9557(2) 0.064(2) Uani 1 1 d . . . H19 H -0.5213 0.2978 0.9591 0.076 Uiso 1 1 calc R . . C20 C -0.4201(4) 0.2714(3) 0.9789(2) 0.061(2) Uani 1 1 d . . . C21 C -0.3523(3) 0.2788(3) 0.9731(2) 0.061(2) Uani 1 1 d . . . H21 H -0.3146 0.2589 0.9876 0.073 Uiso 1 1 calc R . . C22 C -0.5263(3) 0.3681(4) 0.9029(3) 0.073(3) Uani 1 1 d . . . C23 C -0.5984(4) 0.3546(4) 0.9143(3) 0.116(4) Uani 1 1 d . . . H23A H -0.5962 0.3662 0.9396 0.174 Uiso 1 1 calc R . . H23B H -0.6073 0.3148 0.9121 0.174 Uiso 1 1 calc R . . H23C H -0.6364 0.3744 0.8981 0.174 Uiso 1 1 calc R . . C24 C -0.5166(4) 0.4316(4) 0.9062(3) 0.113(4) Uani 1 1 d . . . H24A H -0.4741 0.4423 0.8977 0.169 Uiso 1 1 calc R . . H24B H -0.5122 0.4427 0.9318 0.169 Uiso 1 1 calc R . . H24C H -0.5573 0.4499 0.8911 0.169 Uiso 1 1 calc R . . C25 C -0.5318(4) 0.3468(5) 0.8634(3) 0.100(3) Uani 1 1 d . . . H25A H -0.5688 0.3671 0.8468 0.150 Uiso 1 1 calc R . . H25B H -0.5432 0.3074 0.8623 0.150 Uiso 1 1 calc R . . H25C H -0.4870 0.3525 0.8559 0.150 Uiso 1 1 calc R . . C26 C -0.4377(4) 0.2316(4) 1.0087(3) 0.091(3) Uani 1 1 d . . . C27 C -0.4978(6) 0.1910(6) 0.9904(4) 0.171(6) Uani 1 1 d . . . H27A H -0.4822 0.1695 0.9714 0.257 Uiso 1 1 calc R . . H27B H -0.5397 0.2121 0.9795 0.257 Uiso 1 1 calc R . . H27C H -0.5088 0.1659 1.0091 0.257 Uiso 1 1 calc R . . C28 C -0.3763(6) 0.1972(6) 1.0257(4) 0.195(8) Uani 1 1 d . . . H28A H -0.3557 0.2119 1.0500 0.292 Uiso 1 1 calc R . . H28B H -0.3412 0.1981 1.0103 0.292 Uiso 1 1 calc R . . H28C H -0.3916 0.1591 1.0281 0.292 Uiso 1 1 calc R . . C29 C -0.4656(9) 0.2671(6) 1.0371(4) 0.189(7) Uani 1 1 d . . . H29A H -0.4877 0.2432 1.0526 0.283 Uiso 1 1 calc R . . H29B H -0.5001 0.2936 1.0244 0.283 Uiso 1 1 calc R . . H29C H -0.4265 0.2871 1.0524 0.283 Uiso 1 1 calc R . . C30 C -0.2654(3) 0.3245(3) 0.94389(19) 0.0460(17) Uani 1 1 d . . . H30 H -0.2315 0.3059 0.9617 0.055 Uiso 1 1 calc R . . C31 C -0.1498(3) 0.4003(2) 0.89676(17) 0.0334(14) Uani 1 1 d . . . C32 C -0.1674(3) 0.3641(3) 0.92318(17) 0.0365(15) Uani 1 1 d . . . C33 C -0.1137(3) 0.3404(3) 0.94988(16) 0.0358(15) Uani 1 1 d . . . H33 H -0.1251 0.3145 0.9668 0.043 Uiso 1 1 calc R . . C34 C -0.0440(3) 0.3549(3) 0.95150(17) 0.0375(15) Uani 1 1 d . . . C35 C -0.0273(3) 0.3925(3) 0.92602(18) 0.0468(18) Uani 1 1 d . . . H35 H 0.0201 0.4029 0.9274 0.056 Uiso 1 1 calc R . . C36 C -0.0795(3) 0.4148(3) 0.89881(18) 0.0473(18) Uani 1 1 d . . . H36 H -0.0675 0.4399 0.8816 0.057 Uiso 1 1 calc R . . C37 C 0.0134(3) 0.3276(3) 0.97916(17) 0.0406(16) Uani 1 1 d . . . C38 C 0.0173(4) 0.3911(4) 1.0560(2) 0.060(2) Uani 1 1 d . . . C39 C 0.0321(4) 0.4436(4) 1.0443(2) 0.066(2) Uani 1 1 d . . . H39 H -0.0014 0.4709 1.0344 0.079 Uiso 1 1 calc R . . C40 C 0.1039(4) 0.4489(3) 1.0495(2) 0.060(2) Uani 1 1 d . . . C41 C -0.0538(4) 0.3658(4) 1.0567(2) 0.083(3) Uani 1 1 d . . . H41A H -0.0531 0.3265 1.0509 0.124 Uiso 1 1 calc R . . H41B H -0.0900 0.3843 1.0386 0.124 Uiso 1 1 calc R . . H41C H -0.0642 0.3705 1.0812 0.124 Uiso 1 1 calc R . . C42 C 0.1498(5) 0.4941(3) 1.0396(3) 0.082(3) Uani 1 1 d . . . H42A H 0.1743 0.4807 1.0208 0.123 Uiso 1 1 calc R . . H42B H 0.1843 0.5050 1.0615 0.123 Uiso 1 1 calc R . . H42C H 0.1208 0.5260 1.0302 0.123 Uiso 1 1 calc R . . C43 C 0.2829(4) 0.3448(4) 1.0062(2) 0.071(2) Uani 1 1 d . . . C44 C 0.3327(4) 0.3844(4) 1.0184(3) 0.089(3) Uani 1 1 d . . . H44 H 0.3718 0.3938 1.0080 0.107 Uiso 1 1 calc R . . C45 C 0.3145(4) 0.4073(4) 1.0481(3) 0.077(3) Uani 1 1 d . . . C46 C 0.2772(5) 0.3050(5) 0.9736(3) 0.106(3) Uani 1 1 d . . . H46A H 0.2432 0.2759 0.9756 0.159 Uiso 1 1 calc R . . H46B H 0.3232 0.2883 0.9739 0.159 Uiso 1 1 calc R . . H46C H 0.2617 0.3253 0.9507 0.159 Uiso 1 1 calc R . . C47 C 0.3510(5) 0.4530(4) 1.0730(3) 0.117(4) Uani 1 1 d . . . H47A H 0.3963 0.4614 1.0666 0.175 Uiso 1 1 calc R . . H47B H 0.3586 0.4409 1.0985 0.175 Uiso 1 1 calc R . . H47C H 0.3216 0.4862 1.0698 0.175 Uiso 1 1 calc R . . C48 C 0.2219(3) 0.2558(3) 1.12851(19) 0.0477(18) Uani 1 1 d . . . C49 C 0.2570(3) 0.2858(3) 1.15797(18) 0.0429(17) Uani 1 1 d . . . H49 H 0.2773 0.2723 1.1817 0.051 Uiso 1 1 calc R . . C50 C 0.2566(3) 0.3392(3) 1.14593(18) 0.0454(18) Uani 1 1 d . . . C51 C 0.2111(5) 0.1950(4) 1.1268(2) 0.088(3) Uani 1 1 d . . . H51A H 0.1699 0.1856 1.1368 0.133 Uiso 1 1 calc R . . H51B H 0.2526 0.1767 1.1412 0.133 Uiso 1 1 calc R . . H51C H 0.2039 0.1827 1.1013 0.133 Uiso 1 1 calc R . . C52 C 0.2900(4) 0.3900(3) 1.1661(2) 0.081(3) Uani 1 1 d . . . H52A H 0.3188 0.4088 1.1511 0.121 Uiso 1 1 calc R . . H52B H 0.3196 0.3790 1.1895 0.121 Uiso 1 1 calc R . . H52C H 0.2532 0.4151 1.1706 0.121 Uiso 1 1 calc R . . C53 C 0.3039(3) 0.2004(3) 1.0535(2) 0.060(2) Uani 1 1 d . . . C54 C 0.3314(4) 0.1487(4) 1.0501(3) 0.087(3) Uani 1 1 d . . . H54 H 0.3794 0.1385 1.0565 0.105 Uiso 1 1 calc R . . C55 C 0.2767(5) 0.1152(4) 1.0359(3) 0.093(3) Uani 1 1 d . . . C56 C 0.3448(4) 0.2501(4) 1.0703(3) 0.081(3) Uani 1 1 d . . . H56A H 0.3734 0.2641 1.0536 0.122 Uiso 1 1 calc R . . H56B H 0.3754 0.2395 1.0936 0.122 Uiso 1 1 calc R . . H56C H 0.3122 0.2788 1.0748 0.122 Uiso 1 1 calc R . . C57 C 0.2754(6) 0.0524(4) 1.0268(4) 0.153(6) Uani 1 1 d . . . H57A H 0.2562 0.0470 1.0006 0.229 Uiso 1 1 calc R . . H57B H 0.2461 0.0330 1.0411 0.229 Uiso 1 1 calc R . . H57C H 0.3233 0.0376 1.0328 0.229 Uiso 1 1 calc R . . C58 C 0.0414(4) 0.1809(4) 1.0811(2) 0.064(2) Uani 1 1 d . . . C59 C 0.0365(4) 0.1246(4) 1.0882(2) 0.073(3) Uani 1 1 d . . . H59 H 0.0141 0.1083 1.1060 0.087 Uiso 1 1 calc R . . C60 C 0.0695(5) 0.0980(4) 1.0651(3) 0.082(3) Uani 1 1 d . . . C61 C 0.0123(5) 0.2307(4) 1.0988(2) 0.094(3) Uani 1 1 d . . . H61A H 0.0458 0.2612 1.1012 0.140 Uiso 1 1 calc R . . H61B H 0.0049 0.2203 1.1231 0.140 Uiso 1 1 calc R . . H61C H -0.0324 0.2422 1.0834 0.140 Uiso 1 1 calc R . . C62 C 0.0779(5) 0.0369(4) 1.0617(4) 0.134(5) Uani 1 1 d . . . H62A H 0.1278 0.0278 1.0654 0.202 Uiso 1 1 calc R . . H62B H 0.0539 0.0249 1.0373 0.202 Uiso 1 1 calc R . . H62C H 0.0574 0.0182 1.0803 0.202 Uiso 1 1 calc R . . C63 C 0.0858(5) 0.2164(9) 0.9361(3) 0.144(7) Uani 1 1 d . . . C64 C 0.0610(7) 0.1649(10) 0.9214(4) 0.159(9) Uani 1 1 d . . . H64 H 0.0406 0.1574 0.8965 0.191 Uiso 1 1 calc R . . C65 C 0.0712(7) 0.1297(9) 0.9478(4) 0.160(8) Uani 1 1 d . . . C66 C 0.0884(7) 0.2701(8) 0.9165(3) 0.223(12) Uani 1 1 d . . . H66A H 0.0429 0.2887 0.9135 0.335 Uiso 1 1 calc R . . H66B H 0.0991 0.2632 0.8924 0.335 Uiso 1 1 calc R . . H66C H 0.1249 0.2937 0.9308 0.335 Uiso 1 1 calc R . . C67 C 0.0561(8) 0.0680(8) 0.9474(4) 0.267(13) Uani 1 1 d . . . H67A H 0.0117 0.0604 0.9304 0.400 Uiso 1 1 calc R . . H67B H 0.0529 0.0558 0.9721 0.400 Uiso 1 1 calc R . . H67C H 0.0941 0.0480 0.9394 0.400 Uiso 1 1 calc R . . C68 C -0.1936(3) 0.2160(2) 0.88842(18) 0.0362(15) Uani 1 1 d . . . C69 C -0.2624(3) 0.1960(2) 0.87216(19) 0.0361(15) Uani 1 1 d . . . C70 C -0.2984(3) 0.1612(3) 0.89336(19) 0.0409(16) Uani 1 1 d . . . C71 C -0.2632(3) 0.1468(3) 0.92808(19) 0.0444(17) Uani 1 1 d . . . H71 H -0.2870 0.1235 0.9420 0.053 Uiso 1 1 calc R . . C72 C -0.1936(3) 0.1642(3) 0.94487(19) 0.0436(17) Uani 1 1 d . . . C73 C -0.1607(3) 0.1992(3) 0.92385(19) 0.0415(16) Uani 1 1 d . . . H73 H -0.1146 0.2120 0.9338 0.050 Uiso 1 1 calc R . . C74 C -0.3746(3) 0.1417(3) 0.8778(2) 0.057(2) Uani 1 1 d . . . C75 C -0.4228(3) 0.1936(4) 0.8723(2) 0.077(3) Uani 1 1 d . . . H75A H -0.4207 0.2118 0.8959 0.116 Uiso 1 1 calc R . . H75B H -0.4712 0.1824 0.8621 0.116 Uiso 1 1 calc R . . H75C H -0.4068 0.2192 0.8554 0.116 Uiso 1 1 calc R . . C76 C -0.3794(4) 0.1095(3) 0.8411(2) 0.068(2) Uani 1 1 d . . . H76A H -0.3721 0.1351 0.8219 0.102 Uiso 1 1 calc R . . H76B H -0.4258 0.0925 0.8340 0.102 Uiso 1 1 calc R . . H76C H -0.3433 0.0807 0.8444 0.102 Uiso 1 1 calc R . . C77 C -0.4015(4) 0.1025(4) 0.9054(2) 0.089(3) Uani 1 1 d . . . H77A H -0.3679 0.0724 0.9124 0.134 Uiso 1 1 calc R . . H77B H -0.4472 0.0872 0.8937 0.134 Uiso 1 1 calc R . . H77C H -0.4062 0.1234 0.9272 0.134 Uiso 1 1 calc R . . C78 C -0.1575(3) 0.1448(3) 0.9836(2) 0.0502(18) Uani 1 1 d . . . C79 C -0.1591(11) 0.1890(7) 1.0109(3) 0.268(13) Uani 1 1 d . . . H79A H -0.2013 0.1850 1.0211 0.402 Uiso 1 1 calc R . . H79B H -0.1597 0.2251 0.9989 0.402 Uiso 1 1 calc R . . H79C H -0.1174 0.1862 1.0306 0.402 Uiso 1 1 calc R . . C80 C -0.0790(5) 0.1344(7) 0.9858(3) 0.195(8) Uani 1 1 d . . . H80A H -0.0529 0.1688 0.9923 0.292 Uiso 1 1 calc R . . H80B H -0.0717 0.1214 0.9620 0.292 Uiso 1 1 calc R . . H80C H -0.0623 0.1064 1.0045 0.292 Uiso 1 1 calc R . . C81 C -0.1844(8) 0.0927(6) 0.9944(4) 0.245(11) Uani 1 1 d . . . H81A H -0.1800 0.0920 1.0210 0.367 Uiso 1 1 calc R . . H81B H -0.1574 0.0622 0.9870 0.367 Uiso 1 1 calc R . . H81C H -0.2338 0.0888 0.9824 0.367 Uiso 1 1 calc R . . C82 C -0.1536(3) 0.2515(3) 0.86932(18) 0.0365(15) Uani 1 1 d . . . H82 H -0.1069 0.2595 0.8814 0.044 Uiso 1 1 calc R . . C83 C -0.3449(3) 0.3425(3) 0.73249(17) 0.0372(15) Uani 1 1 d . . . C84 C -0.3814(3) 0.2962(3) 0.74192(19) 0.0417(17) Uani 1 1 d . . . C85 C -0.4501(3) 0.2844(3) 0.7198(2) 0.060(2) Uani 1 1 d . . . C86 C -0.4766(3) 0.3184(3) 0.6910(2) 0.063(2) Uani 1 1 d . . . H86 H -0.5212 0.3095 0.6765 0.076 Uiso 1 1 calc R . . C87 C -0.4422(3) 0.3660(3) 0.68128(18) 0.0461(18) Uani 1 1 d . . . C88 C -0.3764(3) 0.3774(3) 0.70240(17) 0.0452(17) Uani 1 1 d . . . H88 H -0.3517 0.4090 0.6969 0.054 Uiso 1 1 calc R . . C89 C -0.4914(4) 0.2331(4) 0.7308(4) 0.109(4) Uani 1 1 d . . . C90 C -0.5048(5) 0.2414(5) 0.7699(4) 0.154(6) Uani 1 1 d . . . H90A H -0.5279 0.2086 0.7772 0.231 Uiso 1 1 calc R . . H90B H -0.5350 0.2737 0.7703 0.231 Uiso 1 1 calc R . . H90C H -0.4601 0.2472 0.7870 0.231 Uiso 1 1 calc R . . C91 C -0.4502(6) 0.1797(4) 0.7282(4) 0.164(7) Uani 1 1 d . . . H91A H -0.4033 0.1828 0.7436 0.245 Uiso 1 1 calc R . . H91B H -0.4462 0.1736 0.7027 0.245 Uiso 1 1 calc R . . H91C H -0.4749 0.1485 0.7365 0.245 Uiso 1 1 calc R . . C92 C -0.5633(5) 0.2282(5) 0.7029(4) 0.202(9) Uani 1 1 d . . . H92A H -0.5968 0.2081 0.7144 0.303 Uiso 1 1 calc R . . H92B H -0.5565 0.2082 0.6811 0.303 Uiso 1 1 calc R . . H92C H -0.5816 0.2651 0.6959 0.303 Uiso 1 1 calc R . . C93 C -0.4768(3) 0.3994(3) 0.64731(19) 0.054(2) Uani 1 1 d . . . C94 C -0.4382(4) 0.4549(4) 0.6453(2) 0.076(3) Uani 1 1 d . . . H94A H -0.4396 0.4768 0.6672 0.114 Uiso 1 1 calc R . . H94B H -0.4612 0.4752 0.6234 0.114 Uiso 1 1 calc R . . H94C H -0.3893 0.4476 0.6440 0.114 Uiso 1 1 calc R . . C95 C -0.5538(3) 0.4145(3) 0.6481(2) 0.070(2) Uani 1 1 d . . . H95A H -0.5824 0.3808 0.6455 0.106 Uiso 1 1 calc R . . H95B H -0.5721 0.4397 0.6279 0.106 Uiso 1 1 calc R . . H95C H -0.5557 0.4324 0.6714 0.106 Uiso 1 1 calc R . . C96 C -0.4758(4) 0.3653(4) 0.6123(2) 0.086(3) Uani 1 1 d . . . H96A H -0.4273 0.3567 0.6110 0.129 Uiso 1 1 calc R . . H96B H -0.4977 0.3866 0.5906 0.129 Uiso 1 1 calc R . . H96C H -0.5019 0.3309 0.6130 0.129 Uiso 1 1 calc R . . C97 C -0.2739(3) 0.3562(3) 0.75032(17) 0.0377(15) Uani 1 1 d . . . H97 H -0.2525 0.3866 0.7408 0.045 Uiso 1 1 calc R . . C98 C -0.1302(3) 0.3090(2) 0.82096(17) 0.0336(15) Uani 1 1 d . . . C99 C -0.1635(3) 0.3417(2) 0.79105(16) 0.0303(14) Uani 1 1 d . . . C100 C -0.1241(2) 0.3799(2) 0.77547(16) 0.0327(14) Uani 1 1 d . . . H100 H -0.1466 0.4033 0.7562 0.039 Uiso 1 1 calc R . . C101 C -0.0515(3) 0.3836(3) 0.78834(16) 0.0337(14) Uani 1 1 d . . . C102 C -0.0179(3) 0.3481(3) 0.81590(18) 0.0429(17) Uani 1 1 d . . . H102 H 0.0317 0.3491 0.8234 0.052 Uiso 1 1 calc R . . C103 C -0.0567(3) 0.3114(3) 0.83238(18) 0.0415(17) Uani 1 1 d . . . H103 H -0.0336 0.2879 0.8514 0.050 Uiso 1 1 calc R . . C104 C -0.0095(3) 0.4264(3) 0.77239(17) 0.0348(15) Uani 1 1 d . . . C105 C 0.0345(3) 0.5361(3) 0.83540(18) 0.0437(17) Uani 1 1 d . . . C106 C -0.0142(3) 0.5703(3) 0.8470(2) 0.0533(19) Uani 1 1 d . . . H106 H -0.0352 0.5649 0.8676 0.064 Uiso 1 1 calc R . . C107 C -0.0258(3) 0.6134(3) 0.8227(2) 0.0483(18) Uani 1 1 d . . . C108 C 0.0683(4) 0.4854(3) 0.8549(2) 0.065(2) Uani 1 1 d . . . H10D H 0.0317 0.4597 0.8589 0.098 Uiso 1 1 calc R . . H10E H 0.0973 0.4960 0.8785 0.098 Uiso 1 1 calc R . . H10F H 0.0976 0.4675 0.8399 0.098 Uiso 1 1 calc R . . C109 C -0.0723(4) 0.6639(3) 0.8229(2) 0.068(2) Uani 1 1 d . . . H10G H -0.0435 0.6973 0.8252 0.102 Uiso 1 1 calc R . . H10H H -0.0960 0.6616 0.8436 0.102 Uiso 1 1 calc R . . H10I H -0.1074 0.6653 0.8000 0.102 Uiso 1 1 calc R . . C110 C 0.2067(3) 0.6262(3) 0.75257(18) 0.0424(17) Uani 1 1 d . . . C111 C 0.2107(3) 0.6826(3) 0.76112(19) 0.0499(19) Uani 1 1 d . . . H111 H 0.2496 0.7061 0.7612 0.060 Uiso 1 1 calc R . . C112 C 0.1478(3) 0.6972(3) 0.76930(18) 0.0415(16) Uani 1 1 d . . . C113 C 0.2640(3) 0.5915(3) 0.7411(2) 0.059(2) Uani 1 1 d . . . H11A H 0.2996 0.5820 0.7628 0.089 Uiso 1 1 calc R . . H11B H 0.2858 0.6126 0.7240 0.089 Uiso 1 1 calc R . . H11C H 0.2433 0.5577 0.7292 0.089 Uiso 1 1 calc R . . C114 C 0.1248(3) 0.7527(3) 0.7809(2) 0.059(2) Uani 1 1 d . . . H11D H 0.1641 0.7787 0.7837 0.088 Uiso 1 1 calc R . . H11E H 0.1098 0.7490 0.8043 0.088 Uiso 1 1 calc R . . H11F H 0.0857 0.7665 0.7622 0.088 Uiso 1 1 calc R . . C115 C -0.0563(3) 0.5861(3) 0.67891(19) 0.0463(18) Uani 1 1 d . . . C116 C -0.0860(3) 0.6391(3) 0.6730(2) 0.0515(19) Uani 1 1 d . . . H116 H -0.1168 0.6521 0.6516 0.062 Uiso 1 1 calc R . . C117 C -0.0609(3) 0.6687(3) 0.7052(2) 0.0440(17) Uani 1 1 d . . . C118 C -0.0631(4) 0.5377(3) 0.65305(19) 0.066(2) Uani 1 1 d . . . H11G H -0.0163 0.5255 0.6506 0.098 Uiso 1 1 calc R . . H11H H -0.0902 0.5487 0.6290 0.098 Uiso 1 1 calc R . . H11I H -0.0872 0.5074 0.6627 0.098 Uiso 1 1 calc R . . C119 C -0.0773(4) 0.7272(3) 0.7141(2) 0.068(2) Uani 1 1 d . . . H11J H -0.1037 0.7271 0.7338 0.102 Uiso 1 1 calc R . . H11K H -0.1054 0.7447 0.6923 0.102 Uiso 1 1 calc R . . H11L H -0.0335 0.7477 0.7220 0.102 Uiso 1 1 calc R . . C120 C 0.2551(3) 0.4737(3) 0.7926(2) 0.055(2) Uani 1 1 d . . . C121 C 0.3150(3) 0.4461(3) 0.7855(2) 0.071(2) Uani 1 1 d . . . H121 H 0.3590 0.4429 0.8019 0.085 Uiso 1 1 calc R . . C122 C 0.2981(3) 0.4252(3) 0.7511(2) 0.060(2) Uani 1 1 d . . . C123 C 0.2455(4) 0.5052(4) 0.8258(2) 0.084(3) Uani 1 1 d . . . H12D H 0.2003 0.5243 0.8205 0.126 Uiso 1 1 calc R . . H12E H 0.2834 0.5322 0.8323 0.126 Uiso 1 1 calc R . . H12F H 0.2467 0.4796 0.8462 0.126 Uiso 1 1 calc R . . C124 C 0.3429(4) 0.3916(4) 0.7308(3) 0.095(3) Uani 1 1 d . . . H12G H 0.3163 0.3597 0.7194 0.142 Uiso 1 1 calc R . . H12H H 0.3849 0.3790 0.7480 0.142 Uiso 1 1 calc R . . H12I H 0.3567 0.4144 0.7117 0.142 Uiso 1 1 calc R . . C125 C 0.1387(3) 0.5675(3) 0.66237(18) 0.0428(17) Uani 1 1 d . . . C126 C 0.1813(4) 0.5524(3) 0.6379(2) 0.057(2) Uani 1 1 d . . . H126 H 0.1938 0.5743 0.6192 0.068 Uiso 1 1 calc R . . C127 C 0.2012(4) 0.4984(3) 0.6471(2) 0.056(2) Uani 1 1 d . . . C128 C 0.1065(4) 0.6239(3) 0.6648(2) 0.058(2) Uani 1 1 d . . . H12J H 0.0726 0.6221 0.6809 0.087 Uiso 1 1 calc R . . H12K H 0.0826 0.6358 0.6403 0.087 Uiso 1 1 calc R . . H12L H 0.1435 0.6504 0.6748 0.087 Uiso 1 1 calc R . . C129 C 0.2498(5) 0.4608(3) 0.6299(3) 0.086(3) Uani 1 1 d . . . H12M H 0.2873 0.4464 0.6492 0.129 Uiso 1 1 calc R . . H12N H 0.2704 0.4822 0.6124 0.129 Uiso 1 1 calc R . . H12O H 0.2226 0.4301 0.6171 0.129 Uiso 1 1 calc R . . C130 C 0.0013(3) 0.3827(3) 0.69021(17) 0.0419(17) Uani 1 1 d . . . C131 C 0.0365(3) 0.3320(3) 0.69944(19) 0.0486(18) Uani 1 1 d . . . H131 H 0.0158 0.2968 0.7007 0.058 Uiso 1 1 calc R . . C132 C 0.1070(3) 0.3443(3) 0.70627(19) 0.0456(17) Uani 1 1 d . . . C133 C -0.0764(3) 0.3918(3) 0.6784(2) 0.063(2) Uani 1 1 d . . . H13D H -0.0903 0.4236 0.6915 0.094 Uiso 1 1 calc R . . H13E H -0.1015 0.3589 0.6841 0.094 Uiso 1 1 calc R . . H13F H -0.0882 0.3988 0.6520 0.094 Uiso 1 1 calc R . . C134 C 0.1680(4) 0.3056(3) 0.7190(3) 0.077(3) Uani 1 1 d . . . H13G H 0.2011 0.3086 0.7025 0.115 Uiso 1 1 calc R . . H13H H 0.1507 0.2677 0.7188 0.115 Uiso 1 1 calc R . . H13I H 0.1918 0.3156 0.7439 0.115 Uiso 1 1 calc R . . B1 B 0.2114(4) 0.3910(4) 1.0838(2) 0.051(2) Uani 1 1 d . . . H1 H 0.2285 0.4251 1.0978 0.061 Uiso 1 1 calc R . . B2 B 0.1390(5) 0.1270(5) 1.0165(4) 0.094(4) Uani 1 1 d . . . H2 H 0.1405 0.0864 1.0121 0.113 Uiso 1 1 calc R . . B3 B 0.0271(3) 0.6476(3) 0.7675(2) 0.0382(18) Uani 1 1 d . . . H3 H 0.0129 0.6849 0.7750 0.046 Uiso 1 1 calc R . . B4 B 0.1850(3) 0.4284(3) 0.6977(2) 0.0424(19) Uani 1 1 d . . . H4A H 0.2115 0.4027 0.6845 0.051 Uiso 1 1 calc R . . C135 C 0.2211(8) 0.7038(7) 0.8718(4) 0.210(7) Uiso 1 1 d D . . C136 C 0.2792(7) 0.7151(6) 0.8577(3) 0.167(6) Uiso 1 1 d D . . H136 H 0.3049 0.6858 0.8499 0.200 Uiso 1 1 calc R . . C137 C 0.3007(7) 0.7698(7) 0.8548(4) 0.181(6) Uiso 1 1 d D . . H137 H 0.3388 0.7778 0.8433 0.218 Uiso 1 1 calc R . . C138 C 0.2682(8) 0.8098(7) 0.8680(4) 0.210(7) Uiso 1 1 d D . . H138 H 0.2816 0.8469 0.8650 0.253 Uiso 1 1 calc R . . C139 C 0.2126(8) 0.7986(7) 0.8870(4) 0.188(6) Uiso 1 1 d D . . H139 H 0.1924 0.8274 0.8986 0.225 Uiso 1 1 calc R . . C140 C 0.1892(7) 0.7450(7) 0.8880(4) 0.188(6) Uiso 1 1 d D . . H140 H 0.1516 0.7366 0.8996 0.225 Uiso 1 1 calc R . . C141 C 0.1902(9) 0.6495(7) 0.8717(5) 0.254(9) Uiso 1 1 d D . . H14D H 0.2163 0.6234 0.8595 0.381 Uiso 1 1 calc R . . H14E H 0.1412 0.6508 0.8585 0.381 Uiso 1 1 calc R . . H14F H 0.1921 0.6375 0.8969 0.381 Uiso 1 1 calc R . . C142 C 0.2798(7) 0.2754(6) 0.8208(4) 0.078(5) Uiso 0.50 1 d PD A -1 C143 C 0.2480(7) 0.3244(6) 0.8148(5) 0.094(6) Uiso 0.50 1 d PD A -1 H143 H 0.2567 0.3449 0.7945 0.113 Uiso 0.50 1 calc PR A -1 C144 C 0.2039(8) 0.3486(7) 0.8350(5) 0.093(6) Uiso 0.50 1 d PD A -1 H144 H 0.1826 0.3834 0.8285 0.112 Uiso 0.50 1 calc PR A -1 C145 C 0.1939(9) 0.3223(8) 0.8619(5) 0.120(8) Uiso 0.50 1 d PD A -1 H145 H 0.1649 0.3375 0.8770 0.144 Uiso 0.50 1 calc PR A -1 C146 C 0.2251(9) 0.2694(8) 0.8708(5) 0.099(6) Uiso 0.50 1 d PD A -1 H146 H 0.2153 0.2496 0.8911 0.119 Uiso 0.50 1 calc PR A -1 C147 C 0.2686(11) 0.2469(10) 0.8506(5) 0.165(16) Uiso 0.50 1 d PD A -1 H147 H 0.2906 0.2124 0.8570 0.198 Uiso 0.50 1 calc PR A -1 C148 C 0.3233(9) 0.2532(8) 0.7986(5) 0.135(8) Uiso 0.50 1 d PD A -1 H14G H 0.3256 0.2788 0.7785 0.202 Uiso 0.50 1 calc PR A -1 H14H H 0.3041 0.2179 0.7884 0.202 Uiso 0.50 1 calc PR A -1 H14I H 0.3705 0.2475 0.8133 0.202 Uiso 0.50 1 calc PR A -1 C242 C 0.3058(13) 0.1740(9) 0.9128(7) 0.30(2) Uiso 0.50 1 d PD B -2 C243 C 0.2605(14) 0.2095(11) 0.8923(7) 0.260(19) Uiso 0.50 1 d PD B -2 H243 H 0.2185 0.2166 0.9007 0.312 Uiso 0.50 1 calc PR B -2 C244 C 0.2677(17) 0.2371(12) 0.8604(8) 0.28(3) Uiso 0.50 1 d PD B -2 H244 H 0.2319 0.2606 0.8477 0.331 Uiso 0.50 1 calc PR B -2 C245 C 0.3232(17) 0.2296(11) 0.8494(7) 0.194(14) Uiso 0.50 1 d PD B -2 H245 H 0.3310 0.2452 0.8272 0.233 Uiso 0.50 1 calc PR B -2 C246 C 0.3739(15) 0.1961(12) 0.8721(8) 0.244(17) Uiso 0.50 1 d PD B -2 H246 H 0.4175 0.1929 0.8647 0.293 Uiso 0.50 1 calc PR B -2 C247 C 0.3691(13) 0.1679(12) 0.9030(8) 0.34(3) Uiso 0.50 1 d PD B -2 H247 H 0.4060 0.1461 0.9165 0.407 Uiso 0.50 1 calc PR B -2 C248 C 0.2886(14) 0.1450(11) 0.9422(7) 0.182(12) Uiso 0.50 1 d PD B -2 H24D H 0.2417 0.1560 0.9452 0.273 Uiso 0.50 1 calc PR B -2 H24E H 0.3229 0.1535 0.9646 0.273 Uiso 0.50 1 calc PR B -2 H24F H 0.2891 0.1054 0.9372 0.273 Uiso 0.50 1 calc PR B -2 C149 C 0.3831(12) 0.0004(11) 0.9544(6) 0.36(3) Uiso 0.50 1 d PD C -1 C150 C 0.3727(17) 0.0547(10) 0.9456(10) 0.72(8) Uiso 0.50 1 d PD C -1 H150 H 0.4075 0.0817 0.9540 0.861 Uiso 0.50 1 calc PR C -1 C151 C 0.3074(18) 0.0686(11) 0.9234(9) 0.43(4) Uiso 0.50 1 d PD C -1 H151 H 0.2984 0.1061 0.9166 0.515 Uiso 0.50 1 calc PR C -1 C152 C 0.2611(13) 0.0335(13) 0.9123(7) 0.215(15) Uiso 0.50 1 d PD C -1 H152 H 0.2169 0.0457 0.8990 0.258 Uiso 0.50 1 calc PR C -1 C153 C 0.2714(11) -0.0235(11) 0.9186(6) 0.146(9) Uiso 0.50 1 d PD C -1 H153 H 0.2377 -0.0504 0.9081 0.175 Uiso 0.50 1 calc PR C -1 C154 C 0.3340(13) -0.0369(9) 0.9411(7) 0.29(2) Uiso 0.50 1 d PD C -1 H154 H 0.3429 -0.0745 0.9476 0.350 Uiso 0.50 1 calc PR C -1 C155 C 0.4493(14) -0.0151(15) 0.9788(9) 0.27(2) Uiso 0.50 1 d PD C -1 H15A H 0.4781 0.0179 0.9854 0.411 Uiso 0.50 1 calc PR C -1 H15B H 0.4745 -0.0414 0.9663 0.411 Uiso 0.50 1 calc PR C -1 H15C H 0.4393 -0.0322 1.0010 0.411 Uiso 0.50 1 calc PR C -1 C156 C 0.2591(11) 0.5067(9) 0.9496(5) 0.498(9) Uiso 1 1 d D D -1 C157 C 0.3221(12) 0.5053(10) 0.9411(7) 0.498(9) Uiso 1 1 d D D -1 H157 H 0.3324 0.4775 0.9251 0.597 Uiso 1 1 calc R D -1 C158 C 0.3749(11) 0.5452(12) 0.9556(8) 0.498(9) Uiso 1 1 d D D -1 H158 H 0.4194 0.5443 0.9490 0.597 Uiso 1 1 calc R D -1 C159 C 0.3618(15) 0.5800(11) 0.9764(7) 0.498(9) Uiso 1 1 d D D -1 H159 H 0.3980 0.6035 0.9887 0.597 Uiso 1 1 calc R D -1 C160 C 0.2917(17) 0.5858(9) 0.9826(6) 0.498(9) Uiso 1 1 d D D -1 H160 H 0.2806 0.6162 0.9964 0.597 Uiso 1 1 calc R D -1 C161 C 0.2427(12) 0.5495(10) 0.9692(6) 0.498(9) Uiso 1 1 d D D -1 H161 H 0.1965 0.5535 0.9733 0.597 Uiso 1 1 calc R D -1 C162 C 0.2077(15) 0.4637(11) 0.9377(8) 0.498(9) Uiso 1 1 d D D -1 H16A H 0.2266 0.4370 0.9225 0.746 Uiso 1 1 calc R D -1 H16B H 0.1648 0.4802 0.9233 0.746 Uiso 1 1 calc R D -1 H16C H 0.1968 0.4450 0.9591 0.746 Uiso 1 1 calc R D -1 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 La1 0.03600(17) 0.0541(3) 0.0361(2) 0.0022(2) 0.00034(15) -0.00014(16) La2 0.02893(15) 0.0311(2) 0.0423(2) 0.00018(18) 0.01337(14) -0.00432(14) Fe1 0.0271(4) 0.0339(6) 0.0464(6) 0.0047(4) 0.0130(4) 0.0011(3) Fe2 0.0266(4) 0.0326(6) 0.0508(6) -0.0007(5) 0.0098(4) -0.0045(3) O1 0.0308(18) 0.037(3) 0.050(3) 0.005(2) 0.0131(19) 0.0044(17) O2 0.037(2) 0.044(3) 0.063(3) 0.014(2) 0.023(2) 0.0085(18) O3 0.034(2) 0.072(4) 0.047(3) 0.020(3) 0.000(2) -0.009(2) O4 0.039(2) 0.055(4) 0.048(3) 0.018(3) 0.003(2) -0.005(2) O5 0.039(2) 0.032(3) 0.051(3) -0.001(2) 0.012(2) -0.0112(17) O6 0.0304(19) 0.037(3) 0.061(3) -0.002(2) 0.003(2) -0.0065(17) O7 0.0304(19) 0.048(3) 0.054(3) 0.015(2) 0.0096(19) -0.0005(18) O8 0.0242(18) 0.044(3) 0.048(3) 0.007(2) 0.0092(17) -0.0012(16) O9 0.0336(19) 0.041(3) 0.059(3) -0.006(2) 0.015(2) -0.0007(17) N1 0.028(2) 0.033(3) 0.041(3) 0.003(3) 0.009(2) -0.0005(19) N2 0.030(2) 0.037(4) 0.040(3) 0.002(3) 0.014(2) -0.001(2) N3 0.061(3) 0.038(4) 0.048(4) -0.001(3) 0.013(3) 0.006(3) N4 0.048(3) 0.055(4) 0.056(4) 0.003(3) 0.006(3) 0.001(3) N5 0.046(3) 0.054(4) 0.060(4) 0.013(3) 0.010(3) -0.011(3) N6 0.048(3) 0.059(5) 0.042(3) 0.002(3) 0.008(3) -0.001(3) N7 0.046(3) 0.030(4) 0.043(3) -0.001(3) 0.003(3) -0.004(2) N8 0.060(3) 0.033(4) 0.043(3) 0.001(3) -0.001(3) -0.006(3) N9 0.050(3) 0.061(5) 0.112(6) -0.032(4) 0.001(3) 0.006(3) N10 0.042(3) 0.051(5) 0.074(5) -0.009(3) -0.003(3) -0.001(3) N11 0.057(3) 0.046(5) 0.084(5) -0.013(4) 0.006(3) -0.018(3) N12 0.060(3) 0.054(5) 0.051(4) -0.007(3) 0.011(3) -0.009(3) N13 0.053(4) 0.195(11) 0.086(7) -0.102(8) 0.022(4) -0.029(6) N14 0.058(4) 0.162(9) 0.055(5) -0.044(6) -0.011(4) 0.036(5) N15 0.030(2) 0.028(3) 0.047(3) 0.005(3) 0.012(2) -0.004(2) N16 0.025(2) 0.033(3) 0.041(3) -0.002(3) 0.008(2) -0.0025(19) N17 0.039(2) 0.035(4) 0.037(3) -0.004(3) 0.013(2) 0.000(2) N18 0.045(3) 0.039(4) 0.040(3) 0.004(3) 0.015(2) -0.003(2) N19 0.041(2) 0.024(3) 0.042(3) 0.000(2) 0.016(2) -0.002(2) N20 0.040(3) 0.033(4) 0.051(3) -0.009(3) 0.020(2) -0.004(2) N21 0.036(2) 0.031(4) 0.047(3) 0.003(3) 0.011(2) 0.001(2) N22 0.038(2) 0.038(4) 0.040(3) -0.001(3) 0.009(2) -0.006(2) N23 0.030(2) 0.042(4) 0.056(4) -0.009(3) 0.016(2) -0.002(2) N24 0.034(2) 0.051(4) 0.052(4) -0.007(3) 0.012(3) -0.005(2) N25 0.044(3) 0.029(4) 0.050(3) -0.006(3) 0.026(2) -0.008(2) N26 0.045(3) 0.029(4) 0.049(4) -0.002(3) 0.022(2) -0.006(2) N27 0.039(2) 0.034(4) 0.046(3) 0.000(3) 0.017(2) -0.005(2) N28 0.036(2) 0.036(4) 0.058(4) -0.002(3) 0.011(2) -0.007(2) C1 0.031(3) 0.029(4) 0.036(4) 0.002(3) 0.008(3) 0.000(2) C2 0.034(3) 0.026(4) 0.044(4) -0.002(3) 0.008(3) 0.002(2) C3 0.033(3) 0.028(4) 0.043(4) -0.006(3) 0.008(3) 0.003(2) C4 0.038(3) 0.044(5) 0.037(4) -0.001(3) 0.003(3) 0.001(3) C5 0.041(3) 0.046(5) 0.040(4) 0.005(3) 0.008(3) -0.008(3) C6 0.033(3) 0.036(4) 0.048(4) 0.000(3) 0.011(3) 0.001(2) C7 0.030(3) 0.043(5) 0.054(4) 0.000(3) 0.007(3) 0.004(3) C8 0.030(3) 0.062(6) 0.081(6) 0.005(4) 0.013(3) -0.008(3) C9 0.040(3) 0.063(6) 0.068(5) -0.005(4) 0.010(3) 0.011(3) C10 0.036(3) 0.084(6) 0.063(5) 0.004(4) 0.007(3) 0.007(3) C11 0.044(3) 0.050(5) 0.060(5) 0.022(4) 0.008(3) -0.001(3) C12 0.117(7) 0.112(9) 0.059(6) 0.009(6) 0.044(5) -0.014(6) C13 0.111(7) 0.107(8) 0.073(6) 0.017(6) 0.022(5) -0.057(6) C14 0.085(6) 0.128(9) 0.099(7) 0.083(7) 0.019(5) 0.008(6) C15 0.031(3) 0.032(4) 0.043(4) 0.003(3) 0.012(3) 0.003(2) C16 0.040(3) 0.054(5) 0.045(4) 0.009(4) 0.018(3) -0.003(3) C17 0.040(3) 0.043(5) 0.048(4) -0.001(4) 0.020(3) 0.001(3) C18 0.039(3) 0.051(5) 0.067(5) 0.011(4) 0.024(3) 0.003(3) C19 0.043(4) 0.075(6) 0.080(6) 0.020(5) 0.030(4) -0.006(4) C20 0.058(4) 0.065(6) 0.067(5) 0.009(4) 0.030(4) -0.009(4) C21 0.048(4) 0.065(6) 0.073(5) 0.030(4) 0.022(4) 0.001(3) C22 0.035(3) 0.089(8) 0.103(8) 0.031(6) 0.032(4) 0.008(4) C23 0.044(4) 0.166(11) 0.151(10) 0.076(8) 0.049(5) 0.024(5) C24 0.076(6) 0.096(9) 0.184(12) 0.053(8) 0.067(7) 0.037(5) C25 0.047(4) 0.165(10) 0.087(7) 0.042(7) 0.012(5) 0.000(5) C26 0.067(5) 0.118(9) 0.096(7) 0.063(7) 0.039(5) -0.005(5) C27 0.123(9) 0.174(14) 0.218(15) 0.087(12) 0.039(10) -0.058(9) C28 0.113(9) 0.251(17) 0.239(16) 0.202(14) 0.080(10) 0.027(10) C29 0.287(19) 0.183(15) 0.154(13) 0.055(11) 0.180(14) 0.048(13) C30 0.035(3) 0.051(5) 0.052(4) 0.011(4) 0.009(3) -0.002(3) C31 0.030(3) 0.031(4) 0.041(4) 0.004(3) 0.010(3) -0.002(2) C32 0.033(3) 0.035(4) 0.043(4) -0.005(3) 0.011(3) -0.001(2) C33 0.034(3) 0.036(4) 0.036(4) 0.005(3) 0.006(3) 0.000(2) C34 0.034(3) 0.041(5) 0.036(4) 0.001(3) 0.005(3) -0.002(3) C35 0.027(3) 0.061(5) 0.052(4) 0.014(4) 0.006(3) -0.004(3) C36 0.036(3) 0.054(5) 0.052(4) 0.020(4) 0.007(3) -0.004(3) C37 0.043(3) 0.041(5) 0.035(4) -0.001(3) 0.000(3) 0.001(3) C38 0.059(4) 0.070(7) 0.052(5) -0.005(4) 0.014(4) 0.021(4) C39 0.068(5) 0.075(7) 0.056(5) 0.005(5) 0.014(4) 0.038(4) C40 0.088(5) 0.039(6) 0.055(5) 0.002(4) 0.022(4) 0.021(4) C41 0.049(4) 0.107(8) 0.093(7) -0.007(6) 0.014(4) 0.014(4) C42 0.107(6) 0.038(6) 0.104(7) 0.015(5) 0.032(6) 0.016(5) C43 0.055(4) 0.116(8) 0.048(5) 0.001(5) 0.022(4) -0.003(4) C44 0.064(5) 0.124(9) 0.087(7) 0.009(6) 0.034(5) -0.032(5) C45 0.075(5) 0.086(8) 0.072(6) 0.013(5) 0.017(5) -0.027(5) C46 0.095(6) 0.155(11) 0.082(7) -0.002(7) 0.051(6) -0.007(6) C47 0.108(7) 0.120(10) 0.126(9) -0.011(7) 0.033(7) -0.072(7) C48 0.066(4) 0.028(5) 0.044(4) 0.007(4) -0.001(3) -0.004(3) C49 0.049(3) 0.040(5) 0.034(4) 0.009(4) -0.005(3) -0.003(3) C50 0.037(3) 0.057(6) 0.040(4) -0.011(4) 0.004(3) -0.002(3) C51 0.120(7) 0.058(7) 0.067(6) 0.010(5) -0.029(5) -0.014(5) C52 0.100(6) 0.052(6) 0.075(6) -0.011(5) -0.020(5) -0.013(4) C53 0.047(4) 0.056(6) 0.071(6) -0.005(4) -0.004(4) 0.006(3) C54 0.046(4) 0.070(7) 0.140(9) -0.016(6) 0.009(5) 0.013(4) C55 0.077(6) 0.067(7) 0.132(9) -0.033(6) 0.011(6) 0.014(5) C56 0.044(4) 0.084(7) 0.106(7) -0.012(6) -0.010(4) 0.001(4) C57 0.124(9) 0.083(10) 0.256(16) -0.081(10) 0.050(10) 0.022(7) C58 0.078(5) 0.067(7) 0.042(5) -0.002(4) 0.003(4) -0.019(4) C59 0.080(5) 0.063(7) 0.067(6) 0.020(5) -0.004(5) -0.029(5) C60 0.071(5) 0.047(8) 0.115(9) -0.015(6) -0.011(6) -0.007(4) C61 0.136(8) 0.085(8) 0.077(7) -0.011(6) 0.062(6) -0.023(6) C62 0.119(8) 0.062(9) 0.211(14) -0.008(8) 0.007(8) -0.024(6) C63 0.054(5) 0.33(2) 0.042(6) -0.054(11) -0.007(5) 0.066(9) C64 0.073(7) 0.34(3) 0.072(9) -0.092(14) 0.035(8) -0.045(11) C65 0.094(8) 0.28(2) 0.120(12) -0.131(14) 0.061(10) -0.098(11) C66 0.188(14) 0.44(3) 0.039(6) -0.007(11) 0.005(8) 0.227(18) C67 0.265(18) 0.37(3) 0.200(16) -0.222(18) 0.135(14) -0.253(19) C68 0.037(3) 0.023(4) 0.052(4) -0.004(3) 0.016(3) -0.003(2) C69 0.038(3) 0.020(4) 0.053(4) -0.001(3) 0.014(3) 0.003(2) C70 0.044(3) 0.030(4) 0.051(4) -0.001(3) 0.015(3) -0.006(3) C71 0.048(3) 0.032(5) 0.061(5) 0.000(4) 0.030(3) -0.009(3) C72 0.051(3) 0.031(5) 0.051(4) 0.002(3) 0.017(3) 0.000(3) C73 0.040(3) 0.033(4) 0.054(5) -0.002(3) 0.015(3) -0.005(3) C74 0.043(3) 0.063(6) 0.067(5) 0.007(4) 0.018(3) -0.016(3) C75 0.042(4) 0.092(7) 0.100(7) -0.004(5) 0.022(4) 0.001(4) C76 0.053(4) 0.073(6) 0.077(6) -0.006(5) 0.013(4) -0.024(4) C77 0.070(5) 0.102(8) 0.100(7) 0.019(6) 0.027(5) -0.045(5) C78 0.061(4) 0.042(5) 0.051(5) 0.007(4) 0.019(4) -0.002(3) C79 0.50(3) 0.224(18) 0.045(7) -0.015(9) -0.021(12) 0.23(2) C80 0.087(8) 0.38(2) 0.119(10) 0.129(13) 0.020(7) 0.045(11) C81 0.277(18) 0.175(15) 0.196(14) 0.152(13) -0.150(14) -0.151(14) C82 0.032(3) 0.029(4) 0.050(4) -0.004(3) 0.013(3) -0.001(2) C83 0.032(3) 0.039(5) 0.040(4) -0.006(3) 0.006(3) -0.003(3) C84 0.028(3) 0.035(5) 0.060(5) -0.010(4) 0.004(3) 0.000(3) C85 0.035(3) 0.046(5) 0.091(6) -0.006(5) -0.005(4) -0.007(3) C86 0.031(3) 0.054(6) 0.094(6) -0.012(5) -0.012(4) -0.003(3) C87 0.031(3) 0.060(5) 0.046(4) -0.009(4) 0.005(3) 0.001(3) C88 0.036(3) 0.058(5) 0.040(4) -0.007(4) 0.004(3) -0.005(3) C89 0.054(5) 0.053(7) 0.187(12) 0.044(7) -0.052(6) -0.028(4) C90 0.053(5) 0.178(13) 0.228(16) 0.130(12) 0.022(8) -0.018(6) C91 0.132(9) 0.051(8) 0.246(15) 0.025(8) -0.105(10) -0.034(6) C92 0.088(7) 0.113(10) 0.34(2) 0.084(11) -0.108(10) -0.071(7) C93 0.036(3) 0.075(6) 0.047(5) -0.005(4) 0.000(3) 0.001(3) C94 0.065(5) 0.095(8) 0.061(6) 0.012(5) -0.005(4) 0.000(4) C95 0.041(4) 0.095(7) 0.071(6) 0.022(5) 0.001(4) 0.009(4) C96 0.063(5) 0.131(9) 0.060(6) -0.022(6) 0.003(4) 0.015(5) C97 0.034(3) 0.036(4) 0.044(4) 0.000(3) 0.009(3) -0.006(3) C98 0.028(3) 0.023(4) 0.051(4) -0.002(3) 0.012(3) -0.006(2) C99 0.029(3) 0.024(4) 0.036(4) -0.004(3) 0.005(2) -0.003(2) C100 0.027(2) 0.033(4) 0.037(4) -0.001(3) 0.004(2) -0.003(2) C101 0.033(3) 0.033(4) 0.037(4) 0.000(3) 0.011(3) 0.000(2) C102 0.022(3) 0.042(5) 0.063(5) 0.013(4) 0.005(3) -0.002(2) C103 0.030(3) 0.042(5) 0.051(4) 0.018(3) 0.004(3) -0.002(3) C104 0.035(3) 0.027(4) 0.042(4) -0.002(3) 0.008(3) -0.005(2) C105 0.049(3) 0.046(5) 0.037(4) -0.001(4) 0.010(3) -0.012(3) C106 0.061(4) 0.060(6) 0.041(4) -0.002(4) 0.016(3) -0.010(4) C107 0.044(3) 0.054(5) 0.050(5) -0.016(4) 0.018(3) -0.004(3) C108 0.085(5) 0.060(6) 0.052(5) 0.013(4) 0.018(4) -0.007(4) C109 0.065(4) 0.080(7) 0.068(5) -0.021(5) 0.032(4) -0.001(4) C110 0.040(3) 0.042(5) 0.048(4) -0.010(3) 0.014(3) -0.007(3) C111 0.043(3) 0.045(5) 0.063(5) -0.006(4) 0.013(3) -0.018(3) C112 0.042(3) 0.039(5) 0.043(4) -0.001(3) 0.008(3) -0.007(3) C113 0.039(3) 0.062(6) 0.084(6) -0.017(4) 0.030(4) -0.011(3) C114 0.058(4) 0.031(5) 0.088(6) -0.014(4) 0.017(4) -0.008(3) C115 0.046(3) 0.054(6) 0.040(4) 0.013(4) 0.012(3) 0.002(3) C116 0.045(3) 0.062(6) 0.049(5) 0.023(4) 0.014(3) 0.006(3) C117 0.039(3) 0.042(5) 0.054(5) 0.012(4) 0.014(3) 0.004(3) C118 0.083(5) 0.069(6) 0.041(5) -0.006(4) 0.004(4) 0.000(4) C119 0.069(5) 0.052(6) 0.081(6) 0.007(5) 0.012(4) 0.018(4) C120 0.038(3) 0.065(6) 0.059(5) -0.010(4) 0.001(3) -0.002(3) C121 0.033(3) 0.091(7) 0.082(6) -0.011(5) -0.002(4) 0.008(3) C122 0.034(3) 0.066(6) 0.078(6) -0.017(5) 0.004(4) -0.001(3) C123 0.056(4) 0.128(9) 0.064(6) -0.030(6) 0.002(4) -0.004(5) C124 0.039(4) 0.110(8) 0.134(9) -0.046(7) 0.016(5) 0.015(4) C125 0.042(3) 0.041(5) 0.047(4) 0.001(4) 0.015(3) -0.005(3) C126 0.074(4) 0.049(6) 0.059(5) -0.001(4) 0.037(4) -0.016(4) C127 0.064(4) 0.050(6) 0.064(5) -0.008(4) 0.038(4) -0.017(4) C128 0.067(4) 0.052(6) 0.061(5) 0.018(4) 0.028(4) -0.004(4) C129 0.115(7) 0.064(7) 0.106(7) 0.006(5) 0.084(6) 0.007(5) C130 0.040(3) 0.049(5) 0.038(4) -0.004(3) 0.010(3) -0.013(3) C131 0.050(4) 0.036(5) 0.062(5) -0.007(4) 0.016(3) -0.016(3) C132 0.047(3) 0.031(5) 0.062(5) 0.000(4) 0.021(3) -0.011(3) C133 0.040(3) 0.066(6) 0.079(6) 0.009(4) 0.006(4) -0.019(3) C134 0.061(4) 0.054(6) 0.122(8) 0.022(5) 0.037(5) 0.005(4) B1 0.053(4) 0.037(6) 0.056(6) -0.006(4) -0.005(4) -0.006(3) B2 0.065(6) 0.091(10) 0.121(11) -0.075(8) 0.009(7) -0.024(5) B3 0.040(3) 0.028(5) 0.048(5) -0.004(4) 0.012(3) 0.005(3) B4 0.046(4) 0.031(5) 0.055(5) -0.012(4) 0.020(4) -0.006(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 La1 O3 2.486(4) . ? La1 O4 2.551(4) . ? La1 N12 2.593(6) . ? La1 N6 2.596(5) . ? La1 N8 2.611(5) . ? La1 N14 2.703(8) . ? La1 N10 2.716(6) . ? La1 N4 2.754(6) . ? La1 C37 2.881(6) . ? La2 O8 2.508(4) . ? La2 O7 2.553(4) . ? La2 N22 2.595(5) . ? La2 N24 2.631(5) . ? La2 N26 2.632(5) . ? La2 N18 2.668(5) . ? La2 N20 2.680(5) . ? La2 N28 2.734(5) . ? La2 C104 2.897(6) . ? Fe1 O9 1.769(4) . ? Fe1 O2 1.911(4) . ? Fe1 O1 1.913(4) . ? Fe1 N2 2.103(5) . ? Fe1 N1 2.115(4) . ? Fe2 O9 1.764(4) . ? Fe2 O6 1.909(4) . ? Fe2 O5 1.923(4) . ? Fe2 N15 2.103(4) . ? Fe2 N16 2.123(5) . ? O1 C2 1.316(7) . ? O2 C17 1.306(7) . ? O3 C37 1.276(7) . ? O4 C37 1.257(7) . ? O5 C69 1.319(7) . ? O6 C84 1.318(7) . ? O7 C104 1.267(7) . ? O8 C104 1.270(6) . ? N1 C15 1.289(7) . ? N1 C31 1.424(7) . ? N2 C30 1.296(7) . ? N2 C32 1.431(6) . ? N3 C40 1.375(8) . ? N3 N4 1.381(7) . ? N3 B1 1.569(9) . ? N4 C38 1.343(8) . ? N5 C45 1.348(9) . ? N5 N6 1.370(7) . ? N5 B1 1.547(10) . ? N6 C43 1.325(8) . ? N7 C50 1.357(8) . ? N7 N8 1.372(7) . ? N7 B1 1.526(10) . ? N8 C48 1.346(8) . ? N9 C55 1.366(9) . ? N9 N10 1.380(8) . ? N9 B2 1.549(10) . ? N10 C53 1.338(8) . ? N11 C60 1.319(11) . ? N11 N12 1.368(8) . ? N11 B2 1.512(13) . ? N12 C58 1.308(9) . ? N13 N14 1.360(12) . ? N13 C65 1.364(14) . ? N13 B2 1.528(16) . ? N14 C63 1.341(13) . ? N15 C82 1.303(7) . ? N15 C98 1.420(7) . ? N16 C97 1.290(7) . ? N16 C99 1.416(6) . ? N17 C107 1.356(7) . ? N17 N18 1.380(7) . ? N17 B3 1.531(9) . ? N18 C105 1.349(7) . ? N19 C112 1.362(7) . ? N19 N20 1.382(6) . ? N19 B3 1.549(7) . ? N20 C110 1.349(7) . ? N21 C117 1.351(7) . ? N21 N22 1.369(7) . ? N21 B3 1.537(9) . ? N22 C115 1.342(8) . ? N23 C122 1.346(7) . ? N23 N24 1.357(7) . ? N23 B4 1.562(9) . ? N24 C120 1.329(8) . ? N25 C127 1.357(8) . ? N25 N26 1.366(6) . ? N25 B4 1.515(9) . ? N26 C125 1.345(8) . ? N27 C132 1.349(8) . ? N27 N28 1.377(6) . ? N27 B4 1.565(8) . ? N28 C130 1.352(7) . ? C1 C6 1.419(8) . ? C1 C15 1.423(8) . ? C1 C2 1.430(7) . ? C2 C3 1.417(8) . ? C3 C4 1.378(8) . ? C3 C7 1.539(7) . ? C4 C5 1.410(7) . ? C5 C6 1.376(8) . ? C5 C11 1.522(9) . ? C7 C8 1.536(9) . ? C7 C9 1.541(9) . ? C7 C10 1.543(9) . ? C11 C13 1.508(10) . ? C11 C14 1.532(9) . ? C11 C12 1.545(11) . ? C16 C17 1.414(8) . ? C16 C21 1.416(9) . ? C16 C30 1.440(7) . ? C17 C18 1.428(7) . ? C18 C19 1.358(9) . ? C18 C22 1.543(10) . ? C19 C20 1.426(10) . ? C20 C21 1.380(8) . ? C20 C26 1.547(10) . ? C22 C25 1.529(12) . ? C22 C24 1.538(12) . ? C22 C23 1.569(9) . ? C26 C28 1.475(13) . ? C26 C29 1.533(15) . ? C26 C27 1.558(14) . ? C31 C36 1.385(7) . ? C31 C32 1.400(8) . ? C32 C33 1.397(8) . ? C33 C34 1.378(7) . ? C34 C35 1.388(8) . ? C34 C37 1.496(8) . ? C35 C36 1.377(8) . ? C38 C39 1.382(11) . ? C38 C41 1.506(10) . ? C39 C40 1.365(10) . ? C40 C42 1.492(11) . ? C43 C44 1.361(11) . ? C43 C46 1.523(12) . ? C44 C45 1.336(12) . ? C45 C47 1.510(12) . ? C48 C49 1.364(9) . ? C48 C51 1.473(10) . ? C49 C50 1.355(9) . ? C50 C52 1.504(9) . ? C53 C54 1.365(10) . ? C53 C56 1.493(10) . ? C54 C55 1.346(11) . ? C55 C57 1.545(13) . ? C58 C59 1.386(11) . ? C58 C61 1.524(11) . ? C59 C60 1.330(12) . ? C60 C62 1.482(13) . ? C63 C64 1.40(2) . ? C63 C66 1.48(2) . ? C64 C65 1.28(2) . ? C65 C67 1.51(2) . ? C68 C73 1.392(9) . ? C68 C69 1.423(8) . ? C68 C82 1.429(8) . ? C69 C70 1.421(8) . ? C70 C71 1.367(9) . ? C70 C74 1.537(8) . ? C71 C72 1.422(8) . ? C72 C73 1.383(8) . ? C72 C78 1.531(9) . ? C74 C75 1.543(10) . ? C74 C76 1.545(10) . ? C74 C77 1.552(10) . ? C78 C81 1.441(12) . ? C78 C79 1.467(13) . ? C78 C80 1.521(12) . ? C83 C84 1.398(8) . ? C83 C88 1.425(9) . ? C83 C97 1.432(7) . ? C84 C85 1.434(8) . ? C85 C86 1.355(10) . ? C85 C89 1.565(11) . ? C86 C87 1.405(9) . ? C87 C88 1.374(8) . ? C87 C93 1.524(9) . ? C89 C91 1.523(15) . ? C89 C90 1.533(17) . ? C89 C92 1.553(11) . ? C93 C95 1.535(8) . ? C93 C94 1.536(10) . ? C93 C96 1.536(10) . ? C98 C103 1.395(7) . ? C98 C99 1.400(8) . ? C99 C100 1.390(7) . ? C100 C101 1.386(7) . ? C101 C102 1.383(8) . ? C101 C104 1.500(8) . ? C102 C103 1.376(8) . ? C105 C106 1.381(9) . ? C105 C108 1.495(9) . ? C106 C107 1.357(9) . ? C107 C109 1.509(9) . ? C110 C111 1.387(9) . ? C110 C113 1.513(8) . ? C111 C112 1.355(8) . ? C112 C114 1.494(9) . ? C115 C116 1.393(9) . ? C115 C118 1.494(9) . ? C116 C117 1.383(9) . ? C117 C119 1.492(9) . ? C120 C121 1.400(9) . ? C120 C123 1.483(10) . ? C121 C122 1.344(10) . ? C122 C124 1.491(10) . ? C125 C126 1.388(9) . ? C125 C128 1.501(9) . ? C126 C127 1.374(10) . ? C127 C129 1.531(10) . ? C130 C131 1.400(9) . ? C130 C133 1.489(8) . ? C131 C132 1.364(8) . ? C132 C134 1.497(9) . ? C135 C136 1.355(15) . ? C135 C140 1.366(16) . ? C135 C141 1.433(16) . ? C136 C137 1.388(14) . ? C137 C138 1.295(15) . ? C138 C139 1.422(15) . ? C139 C140 1.366(15) . ? C142 C143 1.324(15) . ? C142 C147 1.351(18) . ? C142 C148 1.393(16) . ? C143 C144 1.369(16) . ? C144 C145 1.228(16) . ? C145 C146 1.415(17) . ? C146 C147 1.342(17) . ? C242 C243 1.338(19) . ? C242 C247 1.35(2) . ? C242 C248 1.386(18) . ? C243 C244 1.383(19) . ? C244 C245 1.234(19) . ? C245 C246 1.404(18) . ? C246 C247 1.348(19) . ? C149 C154 1.322(18) . ? C149 C150 1.347(18) . ? C149 C155 1.452(17) . ? C150 C151 1.395(18) . ? C151 C152 1.236(18) . ? C152 C153 1.395(17) . ? C153 C154 1.358(17) . ? C156 C157 1.317(17) . ? C156 C161 1.332(18) . ? C156 C162 1.436(17) . ? C157 C158 1.420(18) . ? C158 C159 1.195(18) . ? C159 C160 1.423(17) . ? C160 C161 1.307(18) . ? 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 O3 La1 O4 52.08(13) . . ? O3 La1 N12 131.31(15) . . ? O4 La1 N12 80.24(16) . . ? O3 La1 N6 76.33(15) . . ? O4 La1 N6 127.99(16) . . ? N12 La1 N6 151.72(17) . . ? O3 La1 N8 133.38(17) . . ? O4 La1 N8 134.75(16) . . ? N12 La1 N8 85.48(18) . . ? N6 La1 N8 75.10(17) . . ? O3 La1 N14 81.2(2) . . ? O4 La1 N14 75.79(17) . . ? N12 La1 N14 77.6(3) . . ? N6 La1 N14 105.3(3) . . ? N8 La1 N14 141.9(2) . . ? O3 La1 N10 136.02(17) . . ? O4 La1 N10 139.78(17) . . ? N12 La1 N10 73.79(18) . . ? N6 La1 N10 81.01(18) . . ? N8 La1 N10 73.52(18) . . ? N14 La1 N10 69.1(2) . . ? O3 La1 N4 75.40(16) . . ? O4 La1 N4 75.37(15) . . ? N12 La1 N4 104.42(19) . . ? N6 La1 N4 86.91(17) . . ? N8 La1 N4 67.04(17) . . ? N14 La1 N4 150.25(18) . . ? N10 La1 N4 140.49(17) . . ? O3 La1 C37 26.21(15) . . ? O4 La1 C37 25.86(14) . . ? N12 La1 C37 105.67(18) . . ? N6 La1 C37 102.36(18) . . ? N8 La1 C37 140.75(18) . . ? N14 La1 C37 77.2(2) . . ? N10 La1 C37 145.60(18) . . ? N4 La1 C37 73.73(17) . . ? O8 La2 O7 51.82(12) . . ? O8 La2 N22 130.48(13) . . ? O7 La2 N22 79.29(14) . . ? O8 La2 N24 77.04(14) . . ? O7 La2 N24 128.47(15) . . ? N22 La2 N24 152.24(16) . . ? O8 La2 N26 133.45(14) . . ? O7 La2 N26 134.43(14) . . ? N22 La2 N26 84.64(15) . . ? N24 La2 N26 75.13(16) . . ? O8 La2 N18 80.24(15) . . ? O7 La2 N18 76.28(14) . . ? N22 La2 N18 81.03(16) . . ? N24 La2 N18 103.63(16) . . ? N26 La2 N18 142.49(16) . . ? O8 La2 N20 136.91(15) . . ? O7 La2 N20 138.43(14) . . ? N22 La2 N20 74.07(15) . . ? N24 La2 N20 82.15(15) . . ? N26 La2 N20 74.22(15) . . ? N18 La2 N20 68.56(15) . . ? O8 La2 N28 75.77(15) . . ? O7 La2 N28 75.58(14) . . ? N22 La2 N28 101.91(16) . . ? N24 La2 N28 87.40(15) . . ? N26 La2 N28 66.46(15) . . ? N18 La2 N28 150.59(15) . . ? N20 La2 N28 140.67(15) . . ? O8 La2 C104 25.91(14) . . ? O7 La2 C104 25.91(13) . . ? N22 La2 C104 104.92(15) . . ? N24 La2 C104 102.78(16) . . ? N26 La2 C104 140.52(16) . . ? N18 La2 C104 76.90(16) . . ? N20 La2 C104 145.22(16) . . ? N28 La2 C104 74.08(16) . . ? O9 Fe1 O2 109.96(18) . . ? O9 Fe1 O1 106.78(19) . . ? O2 Fe1 O1 94.34(17) . . ? O9 Fe1 N2 103.56(19) . . ? O2 Fe1 N2 85.98(18) . . ? O1 Fe1 N2 147.50(19) . . ? O9 Fe1 N1 102.86(17) . . ? O2 Fe1 N1 145.8(2) . . ? O1 Fe1 N1 85.12(17) . . ? N2 Fe1 N1 77.00(18) . . ? O9 Fe2 O6 111.40(18) . . ? O9 Fe2 O5 104.67(19) . . ? O6 Fe2 O5 96.84(18) . . ? O9 Fe2 N15 102.94(19) . . ? O6 Fe2 N15 143.59(19) . . ? O5 Fe2 N15 85.57(17) . . ? O9 Fe2 N16 100.75(19) . . ? O6 Fe2 N16 85.19(18) . . ? O5 Fe2 N16 151.68(17) . . ? N15 Fe2 N16 76.70(18) . . ? C2 O1 Fe1 126.8(3) . . ? C17 O2 Fe1 130.3(4) . . ? C37 O3 La1 94.4(4) . . ? C37 O4 La1 91.9(3) . . ? C69 O5 Fe2 127.2(4) . . ? C84 O6 Fe2 129.9(4) . . ? C104 O7 La2 92.4(3) . . ? C104 O8 La2 94.4(4) . . ? Fe2 O9 Fe1 155.9(2) . . ? C15 N1 C31 121.5(4) . . ? C15 N1 Fe1 122.0(4) . . ? C31 N1 Fe1 115.4(4) . . ? C30 N2 C32 121.4(5) . . ? C30 N2 Fe1 122.5(4) . . ? C32 N2 Fe1 115.7(4) . . ? C40 N3 N4 110.3(6) . . ? C40 N3 B1 124.0(6) . . ? N4 N3 B1 124.1(6) . . ? C38 N4 N3 105.7(6) . . ? C38 N4 La1 125.1(5) . . ? N3 N4 La1 94.0(4) . . ? C45 N5 N6 109.8(7) . . ? C45 N5 B1 130.6(7) . . ? N6 N5 B1 119.5(5) . . ? C43 N6 N5 104.1(6) . . ? C43 N6 La1 136.0(6) . . ? N5 N6 La1 119.3(4) . . ? C50 N7 N8 108.5(5) . . ? C50 N7 B1 128.8(6) . . ? N8 N7 B1 122.3(5) . . ? C48 N8 N7 105.7(5) . . ? C48 N8 La1 137.5(5) . . ? N7 N8 La1 116.9(4) . . ? C55 N9 N10 109.0(6) . . ? C55 N9 B2 128.1(8) . . ? N10 N9 B2 122.6(6) . . ? C53 N10 N9 105.3(6) . . ? C53 N10 La1 136.5(5) . . ? N9 N10 La1 118.1(4) . . ? C60 N11 N12 110.7(8) . . ? C60 N11 B2 128.1(9) . . ? N12 N11 B2 121.2(8) . . ? C58 N12 N11 105.2(7) . . ? C58 N12 La1 131.0(6) . . ? N11 N12 La1 122.7(5) . . ? N14 N13 C65 107.6(14) . . ? N14 N13 B2 123.8(7) . . ? C65 N13 B2 128.5(15) . . ? C63 N14 N13 106.7(13) . . ? C63 N14 La1 132.5(10) . . ? N13 N14 La1 115.1(6) . . ? C82 N15 C98 121.2(5) . . ? C82 N15 Fe2 120.7(4) . . ? C98 N15 Fe2 115.9(4) . . ? C97 N16 C99 121.9(5) . . ? C97 N16 Fe2 121.9(4) . . ? C99 N16 Fe2 115.6(4) . . ? C107 N17 N18 108.7(5) . . ? C107 N17 B3 127.6(6) . . ? N18 N17 B3 123.1(5) . . ? C105 N18 N17 106.1(5) . . ? C105 N18 La2 132.4(4) . . ? N17 N18 La2 112.0(3) . . ? C112 N19 N20 110.4(5) . . ? C112 N19 B3 126.8(5) . . ? N20 N19 B3 122.6(5) . . ? C110 N20 N19 105.0(5) . . ? C110 N20 La2 136.9(4) . . ? N19 N20 La2 118.0(3) . . ? C117 N21 N22 109.0(5) . . ? C117 N21 B3 129.7(6) . . ? N22 N21 B3 121.1(5) . . ? C115 N22 N21 107.7(5) . . ? C115 N22 La2 130.0(5) . . ? N21 N22 La2 121.5(3) . . ? C122 N23 N24 109.9(5) . . ? C122 N23 B4 128.9(6) . . ? N24 N23 B4 121.1(5) . . ? C120 N24 N23 107.7(5) . . ? C120 N24 La2 134.4(4) . . ? N23 N24 La2 117.7(3) . . ? C127 N25 N26 108.9(6) . . ? C127 N25 B4 127.6(6) . . ? N26 N25 B4 123.0(5) . . ? C125 N26 N25 106.6(5) . . ? C125 N26 La2 137.0(4) . . ? N25 N26 La2 116.2(4) . . ? C132 N27 N28 110.7(5) . . ? C132 N27 B4 124.1(5) . . ? N28 N27 B4 123.7(5) . . ? C130 N28 N27 105.1(5) . . ? C130 N28 La2 126.9(4) . . ? N27 N28 La2 96.5(3) . . ? C6 C1 C15 117.1(5) . . ? C6 C1 C2 119.8(5) . . ? C15 C1 C2 123.0(5) . . ? O1 C2 C3 121.4(5) . . ? O1 C2 C1 120.1(5) . . ? C3 C2 C1 118.5(5) . . ? C4 C3 C2 118.5(5) . . ? C4 C3 C7 122.0(5) . . ? C2 C3 C7 119.5(5) . . ? C3 C4 C5 124.5(6) . . ? C6 C5 C4 116.8(6) . . ? C6 C5 C11 120.8(5) . . ? C4 C5 C11 122.4(6) . . ? C5 C6 C1 121.8(5) . . ? C8 C7 C3 108.5(5) . . ? C8 C7 C9 110.7(6) . . ? C3 C7 C9 110.4(5) . . ? C8 C7 C10 108.3(6) . . ? C3 C7 C10 111.6(5) . . ? C9 C7 C10 107.3(5) . . ? C13 C11 C5 110.7(6) . . ? C13 C11 C14 110.1(7) . . ? C5 C11 C14 112.4(5) . . ? C13 C11 C12 109.0(7) . . ? C5 C11 C12 108.8(6) . . ? C14 C11 C12 105.7(7) . . ? N1 C15 C1 126.1(5) . . ? C17 C16 C21 121.0(5) . . ? C17 C16 C30 122.1(6) . . ? C21 C16 C30 116.7(6) . . ? O2 C17 C16 121.9(5) . . ? O2 C17 C18 119.8(6) . . ? C16 C17 C18 118.3(6) . . ? C19 C18 C17 118.4(6) . . ? C19 C18 C22 122.4(5) . . ? C17 C18 C22 119.1(6) . . ? C18 C19 C20 124.9(6) . . ? C21 C20 C19 116.5(6) . . ? C21 C20 C26 122.9(7) . . ? C19 C20 C26 120.6(6) . . ? C20 C21 C16 120.9(6) . . ? C25 C22 C24 113.0(8) . . ? C25 C22 C18 109.8(7) . . ? C24 C22 C18 109.6(7) . . ? C25 C22 C23 107.1(8) . . ? C24 C22 C23 106.5(7) . . ? C18 C22 C23 110.7(6) . . ? C28 C26 C29 112.5(11) . . ? C28 C26 C20 112.0(7) . . ? C29 C26 C20 107.6(8) . . ? C28 C26 C27 107.1(11) . . ? C29 C26 C27 108.1(10) . . ? C20 C26 C27 109.4(8) . . ? N2 C30 C16 126.5(6) . . ? C36 C31 C32 119.5(5) . . ? C36 C31 N1 124.8(5) . . ? C32 C31 N1 115.8(4) . . ? C33 C32 C31 119.6(5) . . ? C33 C32 N2 125.4(5) . . ? C31 C32 N2 115.0(5) . . ? C34 C33 C32 120.3(6) . . ? C33 C34 C35 119.6(5) . . ? C33 C34 C37 119.9(6) . . ? C35 C34 C37 120.5(5) . . ? C36 C35 C34 120.8(5) . . ? C35 C36 C31 120.2(6) . . ? O4 C37 O3 121.6(5) . . ? O4 C37 C34 120.3(5) . . ? O3 C37 C34 118.1(6) . . ? O4 C37 La1 62.2(3) . . ? O3 C37 La1 59.4(3) . . ? C34 C37 La1 177.5(5) . . ? N4 C38 C39 109.9(7) . . ? N4 C38 C41 121.8(8) . . ? C39 C38 C41 128.3(7) . . ? C40 C39 C38 108.0(7) . . ? C39 C40 N3 106.1(7) . . ? C39 C40 C42 132.0(8) . . ? N3 C40 C42 121.7(7) . . ? N6 C43 C44 112.1(8) . . ? N6 C43 C46 118.8(7) . . ? C44 C43 C46 129.1(8) . . ? C45 C44 C43 105.8(7) . . ? C44 C45 N5 108.1(8) . . ? C44 C45 C47 129.1(8) . . ? N5 C45 C47 122.8(9) . . ? N8 C48 C49 111.1(6) . . ? N8 C48 C51 122.0(6) . . ? C49 C48 C51 126.9(7) . . ? C50 C49 C48 105.6(6) . . ? C49 C50 N7 109.1(6) . . ? C49 C50 C52 129.2(6) . . ? N7 C50 C52 121.7(7) . . ? N10 C53 C54 110.9(7) . . ? N10 C53 C56 123.4(7) . . ? C54 C53 C56 125.6(7) . . ? C55 C54 C53 106.9(7) . . ? C54 C55 N9 107.8(8) . . ? C54 C55 C57 130.2(8) . . ? N9 C55 C57 122.0(8) . . ? N12 C58 C59 109.9(8) . . ? N12 C58 C61 120.5(8) . . ? C59 C58 C61 129.6(9) . . ? C60 C59 C58 106.6(9) . . ? N11 C60 C59 107.6(9) . . ? N11 C60 C62 125.3(11) . . ? C59 C60 C62 127.0(11) . . ? N14 C63 C64 108.0(17) . . ? N14 C63 C66 123.1(16) . . ? C64 C63 C66 128.6(12) . . ? C65 C64 C63 107.6(14) . . ? C64 C65 N13 109.9(17) . . ? C64 C65 C67 130.0(16) . . ? N13 C65 C67 119.8(18) . . ? C73 C68 C69 120.3(6) . . ? C73 C68 C82 116.7(5) . . ? C69 C68 C82 122.9(6) . . ? O5 C69 C70 120.7(5) . . ? O5 C69 C68 120.3(5) . . ? C70 C69 C68 119.0(6) . . ? C71 C70 C69 117.4(5) . . ? C71 C70 C74 121.8(6) . . ? C69 C70 C74 120.7(6) . . ? C70 C71 C72 125.3(6) . . ? C73 C72 C71 115.8(6) . . ? C73 C72 C78 122.4(6) . . ? C71 C72 C78 121.8(6) . . ? C72 C73 C68 122.0(6) . . ? C70 C74 C75 107.9(6) . . ? C70 C74 C76 111.2(5) . . ? C75 C74 C76 111.2(6) . . ? C70 C74 C77 111.2(6) . . ? C75 C74 C77 107.6(6) . . ? C76 C74 C77 107.7(6) . . ? C81 C78 C79 112.3(12) . . ? C81 C78 C80 104.7(10) . . ? C79 C78 C80 104.1(11) . . ? C81 C78 C72 113.7(7) . . ? C79 C78 C72 110.6(7) . . ? C80 C78 C72 110.9(6) . . ? N15 C82 C68 126.7(5) . . ? C84 C83 C88 120.4(5) . . ? C84 C83 C97 123.5(6) . . ? C88 C83 C97 116.0(6) . . ? O6 C84 C83 121.3(5) . . ? O6 C84 C85 120.7(6) . . ? C83 C84 C85 117.9(6) . . ? C86 C85 C84 119.1(7) . . ? C86 C85 C89 123.1(6) . . ? C84 C85 C89 117.8(7) . . ? C85 C86 C87 124.6(6) . . ? C88 C87 C86 116.6(6) . . ? C88 C87 C93 124.1(6) . . ? C86 C87 C93 119.2(6) . . ? C87 C88 C83 121.5(6) . . ? C91 C89 C90 111.1(10) . . ? C91 C89 C92 107.5(9) . . ? C90 C89 C92 109.5(11) . . ? C91 C89 C85 110.3(10) . . ? C90 C89 C85 109.6(9) . . ? C92 C89 C85 108.8(8) . . ? C87 C93 C95 111.8(6) . . ? C87 C93 C94 111.2(5) . . ? C95 C93 C94 106.2(6) . . ? C87 C93 C96 109.5(6) . . ? C95 C93 C96 108.7(6) . . ? C94 C93 C96 109.3(7) . . ? N16 C97 C83 125.6(6) . . ? C103 C98 C99 119.3(5) . . ? C103 C98 N15 124.8(5) . . ? C99 C98 N15 115.9(5) . . ? C100 C99 C98 119.7(5) . . ? C100 C99 N16 125.4(5) . . ? C98 C99 N16 114.9(5) . . ? C101 C100 C99 120.0(5) . . ? C102 C101 C100 120.1(5) . . ? C102 C101 C104 120.1(5) . . ? C100 C101 C104 119.8(5) . . ? C103 C102 C101 120.3(5) . . ? C102 C103 C98 120.3(6) . . ? O7 C104 O8 121.4(5) . . ? O7 C104 C101 119.6(5) . . ? O8 C104 C101 119.0(5) . . ? O7 C104 La2 61.7(3) . . ? O8 C104 La2 59.7(3) . . ? C101 C104 La2 178.6(4) . . ? N18 C105 C106 110.1(6) . . ? N18 C105 C108 123.5(6) . . ? C106 C105 C108 126.3(6) . . ? C107 C106 C105 106.1(6) . . ? N17 C107 C106 108.9(6) . . ? N17 C107 C109 122.2(7) . . ? C106 C107 C109 128.8(7) . . ? N20 C110 C111 110.3(5) . . ? N20 C110 C113 123.4(6) . . ? C111 C110 C113 126.3(5) . . ? C112 C111 C110 107.1(5) . . ? C111 C112 N19 107.3(6) . . ? C111 C112 C114 128.8(6) . . ? N19 C112 C114 123.9(5) . . ? N22 C115 C116 109.2(6) . . ? N22 C115 C118 121.6(6) . . ? C116 C115 C118 129.2(7) . . ? C117 C116 C115 105.9(6) . . ? N21 C117 C116 108.2(6) . . ? N21 C117 C119 123.4(7) . . ? C116 C117 C119 128.4(6) . . ? N24 C120 C121 107.6(7) . . ? N24 C120 C123 122.4(6) . . ? C121 C120 C123 130.0(7) . . ? C122 C121 C120 107.7(6) . . ? C121 C122 N23 107.1(6) . . ? C121 C122 C124 128.6(6) . . ? N23 C122 C124 124.2(7) . . ? N26 C125 C126 110.6(6) . . ? N26 C125 C128 123.8(6) . . ? C126 C125 C128 125.6(6) . . ? C127 C126 C125 104.9(6) . . ? N25 C127 C126 109.0(6) . . ? N25 C127 C129 123.0(7) . . ? C126 C127 C129 128.1(6) . . ? N28 C130 C131 110.3(5) . . ? N28 C130 C133 122.2(6) . . ? C131 C130 C133 127.4(6) . . ? C132 C131 C130 105.8(6) . . ? N27 C132 C131 108.1(6) . . ? N27 C132 C134 124.0(5) . . ? C131 C132 C134 127.9(7) . . ? N7 B1 N5 111.1(6) . . ? N7 B1 N3 111.2(6) . . ? N5 B1 N3 108.3(6) . . ? N11 B2 N13 112.7(8) . . ? N11 B2 N9 112.7(8) . . ? N13 B2 N9 109.8(9) . . ? N17 B3 N21 112.2(5) . . ? N17 B3 N19 111.8(5) . . ? N21 B3 N19 110.2(5) . . ? N25 B4 N23 111.5(5) . . ? N25 B4 N27 111.4(5) . . ? N23 B4 N27 108.7(5) . . ? C136 C135 C140 120.2(15) . . ? C136 C135 C141 123.9(16) . . ? C140 C135 C141 115.9(16) . . ? C135 C136 C137 120.2(14) . . ? C138 C137 C136 119.8(15) . . ? C137 C138 C139 121.1(15) . . ? C140 C139 C138 118.5(14) . . ? C135 C140 C139 119.4(15) . . ? C143 C142 C147 116.0(15) . . ? C143 C142 C148 123.8(13) . . ? C147 C142 C148 120.2(14) . . ? C142 C143 C144 127.2(15) . . ? C145 C144 C143 116.2(17) . . ? C144 C145 C146 121.3(17) . . ? C147 C146 C145 121.1(17) . . ? C146 C147 C142 118.2(18) . . ? C243 C242 C247 116.2(18) . . ? C243 C242 C248 121.9(17) . . ? C247 C242 C248 121.9(17) . . ? C242 C243 C244 128(2) . . ? C245 C244 C243 117(2) . . ? C244 C245 C246 116(2) . . ? C247 C246 C245 129(2) . . ? C246 C247 C242 113(2) . . ? C154 C149 C150 120.3(12) . . ? C154 C149 C155 121.8(15) . . ? C150 C149 C155 117.8(14) . . ? C149 C150 C151 116.5(12) . . ? C152 C151 C150 122.3(13) . . ? C151 C152 C153 123.1(13) . . ? C154 C153 C152 114.3(12) . . ? C149 C154 C153 123.2(13) . . ? C157 C156 C161 118.8(12) . . ? C157 C156 C162 121.5(15) . . ? C161 C156 C162 119.7(15) . . ? C156 C157 C158 121.3(13) . . ? C159 C158 C157 118.9(13) . . ? C158 C159 C160 120.3(13) . . ? C161 C160 C159 120.7(13) . . ? C160 C161 C156 119.2(13) . . ? _diffrn_measured_fraction_theta_max 0.858 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.858 _refine_diff_density_max 0.789 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.087 data_i006_fin _database_code_depnum_ccdc_archive 'CCDC 736171' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H104 B2 La N14 Ni O6' _chemical_formula_weight 1504.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.4277(12) _cell_length_b 36.3382(14) _cell_length_c 21.0331(9) _cell_angle_alpha 90.00 _cell_angle_beta 112.113(3) _cell_angle_gamma 90.00 _cell_volume 16588.8(13) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 23800 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 25.49 _exptl_crystal_description 'thin needles' _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6312 _exptl_absorpt_coefficient_mu 0.789 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7535 _exptl_absorpt_correction_T_max 0.9691 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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 'Stoe IPDS area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37286 _diffrn_reflns_av_R_equivalents 0.1052 _diffrn_reflns_av_sigmaI/netI 0.1323 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 23.25 _reflns_number_total 11844 _reflns_number_gt 7410 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software, STOE X-RED' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1258P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11844 _refine_ls_number_parameters 870 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.1495 _refine_ls_R_factor_gt 0.0955 _refine_ls_wR_factor_ref 0.2386 _refine_ls_wR_factor_gt 0.2144 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.003 _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 La1 La 0.25730(3) 0.467719(16) 0.30552(3) 0.0356(2) Uani 1 1 d . . . Ni1 Ni 0.52313(6) 0.66581(3) 0.35199(7) 0.0354(4) Uani 1 1 d . . . O1 O 0.5055(4) 0.71117(17) 0.3780(4) 0.0423(19) Uani 1 1 d . . . O2 O 0.5923(3) 0.68807(17) 0.3476(3) 0.0388(18) Uani 1 1 d . . . O3 O 0.3045(3) 0.5321(2) 0.3219(4) 0.0441(18) Uani 1 1 d . . . O4 O 0.3655(3) 0.48441(18) 0.3253(4) 0.0386(18) Uani 1 1 d . . . N1 N 0.4502(4) 0.6444(2) 0.3481(4) 0.034(2) Uani 1 1 d . . . N2 N 0.5459(4) 0.6190(2) 0.3361(4) 0.033(2) Uani 1 1 d . . . N3 N 0.1807(4) 0.4927(2) 0.1294(4) 0.037(2) Uani 1 1 d . . . N4 N 0.2405(4) 0.4860(3) 0.1746(4) 0.042(2) Uani 1 1 d . . . N5 N 0.1211(4) 0.4428(2) 0.1621(4) 0.045(2) Uani 1 1 d . . . N6 N 0.1679(4) 0.4255(2) 0.2159(4) 0.042(2) Uani 1 1 d . . . N7 N 0.1153(4) 0.5081(2) 0.1984(4) 0.041(2) Uani 1 1 d . . . N8 N 0.1594(4) 0.5082(2) 0.2654(4) 0.040(2) Uani 1 1 d . . . N9 N 0.2446(4) 0.4074(2) 0.4265(4) 0.046(3) Uani 1 1 d . . . N10 N 0.2050(4) 0.4303(2) 0.3764(4) 0.041(2) Uani 1 1 d . . . N11 N 0.3276(5) 0.3865(2) 0.3832(5) 0.049(3) Uani 1 1 d . . . N12 N 0.3143(4) 0.4047(3) 0.3217(5) 0.045(2) Uani 1 1 d . . . N13 N 0.3436(4) 0.4449(2) 0.4514(5) 0.048(3) Uani 1 1 d . . . N14 N 0.3113(5) 0.4771(2) 0.4467(4) 0.046(3) Uani 1 1 d . . . C1 C 0.4008(5) 0.7006(3) 0.3656(5) 0.037(3) Uani 1 1 d . . . C2 C 0.4570(6) 0.7226(3) 0.3850(6) 0.046(3) Uani 1 1 d . . . C3 C 0.4528(6) 0.7590(3) 0.4124(5) 0.044(3) Uani 1 1 d . . . C4 C 0.3973(6) 0.7707(3) 0.4118(6) 0.050(3) Uani 1 1 d . . . H4 H 0.3956 0.7947 0.4285 0.060 Uiso 1 1 calc R . . C5 C 0.3415(6) 0.7497(3) 0.3880(6) 0.049(3) Uani 1 1 d . . . C6 C 0.3460(6) 0.7151(3) 0.3658(6) 0.053(3) Uani 1 1 d . . . H6 H 0.3100 0.7002 0.3498 0.064 Uiso 1 1 calc R . . C7 C 0.5109(6) 0.7828(3) 0.4393(6) 0.050(3) Uani 1 1 d . . . C8 C 0.5639(6) 0.7620(3) 0.4947(6) 0.061(4) Uani 1 1 d . . . H8A H 0.5517 0.7556 0.5330 0.092 Uiso 1 1 calc R . . H8B H 0.6006 0.7777 0.5114 0.092 Uiso 1 1 calc R . . H8C H 0.5732 0.7394 0.4748 0.092 Uiso 1 1 calc R . . C9 C 0.5289(6) 0.7942(3) 0.3790(7) 0.054(3) Uani 1 1 d . . . H9A H 0.5381 0.7722 0.3578 0.081 Uiso 1 1 calc R . . H9B H 0.5653 0.8101 0.3958 0.081 Uiso 1 1 calc R . . H9C H 0.4946 0.8076 0.3449 0.081 Uiso 1 1 calc R . . C10 C 0.5000(7) 0.8183(3) 0.4745(6) 0.062(4) Uani 1 1 d . . . H10A H 0.4635 0.8312 0.4431 0.094 Uiso 1 1 calc R . . H10B H 0.5361 0.8344 0.4860 0.094 Uiso 1 1 calc R . . H10C H 0.4937 0.8117 0.5165 0.094 Uiso 1 1 calc R . . C11 C 0.2839(6) 0.7669(4) 0.3915(7) 0.060(3) Uani 1 1 d . . . C12 C 0.2671(7) 0.8013(4) 0.3478(9) 0.075(4) Uani 1 1 d . . . H12A H 0.2568 0.7947 0.2996 0.113 Uiso 1 1 calc R . . H12B H 0.3021 0.8184 0.3626 0.113 Uiso 1 1 calc R . . H12C H 0.2314 0.8131 0.3529 0.113 Uiso 1 1 calc R . . C13 C 0.2958(9) 0.7769(5) 0.4670(9) 0.089(5) Uani 1 1 d . . . H13A H 0.3286 0.7954 0.4833 0.133 Uiso 1 1 calc R . . H13B H 0.3083 0.7548 0.4956 0.133 Uiso 1 1 calc R . . H13C H 0.2580 0.7869 0.4699 0.133 Uiso 1 1 calc R . . C14 C 0.2305(7) 0.7401(4) 0.3665(9) 0.076(4) Uani 1 1 d . . . H14A H 0.2209 0.7344 0.3181 0.115 Uiso 1 1 calc R . . H14B H 0.1943 0.7512 0.3716 0.115 Uiso 1 1 calc R . . H14C H 0.2416 0.7175 0.3937 0.115 Uiso 1 1 calc R . . C15 C 0.4029(6) 0.6626(3) 0.3482(5) 0.044(3) Uani 1 1 d . . . H15 H 0.3653 0.6494 0.3353 0.053 Uiso 1 1 calc R . . C16 C 0.6417(5) 0.6352(3) 0.3244(5) 0.039(3) Uani 1 1 d . . . C17 C 0.6375(5) 0.6739(3) 0.3354(5) 0.036(3) Uani 1 1 d . . . C18 C 0.6863(5) 0.6965(3) 0.3321(5) 0.037(3) Uani 1 1 d . . . C19 C 0.7347(5) 0.6801(3) 0.3213(5) 0.039(3) Uani 1 1 d . . . H19 H 0.7667 0.6955 0.3192 0.046 Uiso 1 1 calc R . . C20 C 0.7403(5) 0.6412(3) 0.3130(5) 0.038(3) Uani 1 1 d . . . C21 C 0.6931(5) 0.6202(3) 0.3142(5) 0.039(3) Uani 1 1 d . . . H21 H 0.6947 0.5944 0.3081 0.047 Uiso 1 1 calc R . . C22 C 0.6840(6) 0.7384(3) 0.3436(6) 0.047(3) Uani 1 1 d . . . C23 C 0.6823(6) 0.7455(3) 0.4152(6) 0.051(3) Uani 1 1 d . . . H23A H 0.6469 0.7326 0.4189 0.076 Uiso 1 1 calc R . . H23B H 0.6785 0.7719 0.4216 0.076 Uiso 1 1 calc R . . H23C H 0.7204 0.7363 0.4506 0.076 Uiso 1 1 calc R . . C24 C 0.6267(6) 0.7559(3) 0.2887(6) 0.047(3) Uani 1 1 d . . . H24A H 0.5899 0.7421 0.2858 0.071 Uiso 1 1 calc R . . H24B H 0.6310 0.7553 0.2441 0.071 Uiso 1 1 calc R . . H24C H 0.6228 0.7815 0.3012 0.071 Uiso 1 1 calc R . . C25 C 0.7410(6) 0.7579(3) 0.3397(8) 0.065(4) Uani 1 1 d . . . H25A H 0.7783 0.7483 0.3758 0.097 Uiso 1 1 calc R . . H25B H 0.7380 0.7844 0.3462 0.097 Uiso 1 1 calc R . . H25C H 0.7431 0.7533 0.2948 0.097 Uiso 1 1 calc R . . C26 C 0.7984(5) 0.6263(3) 0.3040(6) 0.048(3) Uani 1 1 d . . . C27 C 0.8548(7) 0.6428(5) 0.3595(12) 0.124(9) Uani 1 1 d . . . H27A H 0.8916 0.6367 0.3500 0.186 Uiso 1 1 calc R . . H27B H 0.8590 0.6327 0.4042 0.186 Uiso 1 1 calc R . . H27C H 0.8503 0.6696 0.3599 0.186 Uiso 1 1 calc R . . C28 C 0.7969(10) 0.6347(7) 0.2346(11) 0.131(9) Uani 1 1 d . . . H28A H 0.7624 0.6217 0.2003 0.197 Uiso 1 1 calc R . . H28B H 0.8357 0.6267 0.2312 0.197 Uiso 1 1 calc R . . H28C H 0.7918 0.6613 0.2263 0.197 Uiso 1 1 calc R . . C29 C 0.8016(7) 0.5850(4) 0.3124(10) 0.086(5) Uani 1 1 d . . . H29A H 0.7624 0.5741 0.2826 0.129 Uiso 1 1 calc R . . H29B H 0.8097 0.5787 0.3603 0.129 Uiso 1 1 calc R . . H29C H 0.8349 0.5753 0.2996 0.129 Uiso 1 1 calc R . . C30 C 0.5955(5) 0.6104(2) 0.3266(5) 0.032(2) Uani 1 1 d . . . H30 H 0.6018 0.5850 0.3207 0.039 Uiso 1 1 calc R . . C31 C 0.4495(5) 0.6058(3) 0.3405(5) 0.033(2) Uani 1 1 d . . . C32 C 0.5016(5) 0.5918(2) 0.3344(5) 0.032(2) Uani 1 1 d . . . C33 C 0.5089(5) 0.5534(3) 0.3319(6) 0.042(3) Uani 1 1 d . . . H33 H 0.5465 0.5437 0.3316 0.050 Uiso 1 1 calc R . . C34 C 0.4625(5) 0.5301(3) 0.3298(5) 0.038(2) Uani 1 1 d . . . H34 H 0.4670 0.5043 0.3260 0.045 Uiso 1 1 calc R . . C35 C 0.4084(5) 0.5445(3) 0.3331(5) 0.035(3) Uani 1 1 d . . . C36 C 0.4013(5) 0.5828(3) 0.3382(5) 0.037(3) Uani 1 1 d . . . H36 H 0.3644 0.5927 0.3400 0.045 Uiso 1 1 calc R . . C37 C 0.3556(5) 0.5190(3) 0.3269(5) 0.038(3) Uani 1 1 d . . . C38 C 0.2767(5) 0.4962(3) 0.1419(6) 0.041(3) Uani 1 1 d . . . C39 C 0.2413(6) 0.5099(3) 0.0768(6) 0.046(3) Uani 1 1 d . . . H39 H 0.2558 0.5185 0.0430 0.055 Uiso 1 1 calc R . . C40 C 0.1826(5) 0.5083(3) 0.0718(5) 0.040(3) Uani 1 1 d . . . C41 C 0.3454(6) 0.4926(4) 0.1712(6) 0.063(4) Uani 1 1 d . . . H41A H 0.3639 0.5163 0.1900 0.095 Uiso 1 1 calc R . . H41B H 0.3596 0.4849 0.1350 0.095 Uiso 1 1 calc R . . H41C H 0.3576 0.4741 0.2078 0.095 Uiso 1 1 calc R . . C42 C 0.1261(6) 0.5200(4) 0.0124(6) 0.065(4) Uani 1 1 d . . . H42A H 0.1382 0.5311 -0.0231 0.098 Uiso 1 1 calc R . . H42B H 0.1032 0.5380 0.0282 0.098 Uiso 1 1 calc R . . H42C H 0.1000 0.4985 -0.0066 0.098 Uiso 1 1 calc R . . C43 C 0.1490(6) 0.3905(3) 0.2171(6) 0.051(3) Uani 1 1 d . . . C44 C 0.0901(6) 0.3860(3) 0.1677(6) 0.060(4) Uani 1 1 d . . . H44 H 0.0653 0.3644 0.1596 0.072 Uiso 1 1 calc R . . C45 C 0.0746(6) 0.4188(3) 0.1330(6) 0.054(3) Uani 1 1 d . . . C46 C 0.1844(6) 0.3621(3) 0.2671(6) 0.053(3) Uani 1 1 d . . . H46A H 0.2218 0.3559 0.2590 0.079 Uiso 1 1 calc R . . H46B H 0.1590 0.3399 0.2615 0.079 Uiso 1 1 calc R . . H46C H 0.1957 0.3716 0.3138 0.079 Uiso 1 1 calc R . . C47 C 0.0156(6) 0.4291(4) 0.0734(7) 0.073(5) Uani 1 1 d . . . H47A H -0.0023 0.4511 0.0854 0.110 Uiso 1 1 calc R . . H47B H -0.0138 0.4087 0.0640 0.110 Uiso 1 1 calc R . . H47C H 0.0250 0.4340 0.0326 0.110 Uiso 1 1 calc R . . C48 C 0.1385(5) 0.5308(3) 0.3012(6) 0.045(3) Uani 1 1 d . . . C49 C 0.0841(6) 0.5470(4) 0.2597(6) 0.054(3) Uani 1 1 d . . . H49 H 0.0611 0.5650 0.2726 0.064 Uiso 1 1 calc R . . C50 C 0.0704(5) 0.5320(3) 0.1967(6) 0.047(3) Uani 1 1 d . . . C51 C 0.1759(6) 0.5381(3) 0.3763(6) 0.058(3) Uani 1 1 d . . . H51A H 0.1964 0.5153 0.3983 0.087 Uiso 1 1 calc R . . H51B H 0.1487 0.5467 0.3988 0.087 Uiso 1 1 calc R . . H51C H 0.2071 0.5569 0.3804 0.087 Uiso 1 1 calc R . . C52 C 0.0151(6) 0.5389(4) 0.1307(7) 0.074(4) Uani 1 1 d . . . H52A H 0.0276 0.5542 0.0999 0.111 Uiso 1 1 calc R . . H52B H -0.0172 0.5516 0.1414 0.111 Uiso 1 1 calc R . . H52C H -0.0008 0.5153 0.1084 0.111 Uiso 1 1 calc R . . C53 C 0.1483(6) 0.4219(3) 0.3718(6) 0.045(3) Uani 1 1 d . . . C54 C 0.1495(6) 0.3945(3) 0.4184(6) 0.051(3) Uani 1 1 d . . . H54 H 0.1155 0.3842 0.4265 0.061 Uiso 1 1 calc R . . C55 C 0.2115(6) 0.3853(3) 0.4508(5) 0.046(3) Uani 1 1 d . . . C56 C 0.0923(5) 0.4414(3) 0.3233(6) 0.050(3) Uani 1 1 d . . . H56A H 0.0843 0.4633 0.3459 0.075 Uiso 1 1 calc R . . H56B H 0.0567 0.4249 0.3104 0.075 Uiso 1 1 calc R . . H56C H 0.0995 0.4488 0.2821 0.075 Uiso 1 1 calc R . . C57 C 0.2382(7) 0.3554(4) 0.5031(6) 0.067(4) Uani 1 1 d . . . H57A H 0.2563 0.3363 0.4838 0.100 Uiso 1 1 calc R . . H57B H 0.2055 0.3446 0.5156 0.100 Uiso 1 1 calc R . . H57C H 0.2701 0.3658 0.5441 0.100 Uiso 1 1 calc R . . C58 C 0.3314(6) 0.3828(3) 0.2814(7) 0.052(3) Uani 1 1 d . . . C59 C 0.3548(7) 0.3507(4) 0.3163(8) 0.076(5) Uani 1 1 d . . . H59 H 0.3699 0.3302 0.2995 0.091 Uiso 1 1 calc R . . C60 C 0.3520(7) 0.3540(3) 0.3799(8) 0.067(4) Uani 1 1 d . . . C61 C 0.3206(8) 0.3935(4) 0.2095(7) 0.073(4) Uani 1 1 d . . . H61A H 0.3125 0.3714 0.1807 0.110 Uiso 1 1 calc R . . H61B H 0.3571 0.4061 0.2082 0.110 Uiso 1 1 calc R . . H61C H 0.2850 0.4100 0.1922 0.110 Uiso 1 1 calc R . . C62 C 0.3721(7) 0.3270(3) 0.4390(8) 0.081(5) Uani 1 1 d . . . H62A H 0.4084 0.3366 0.4763 0.121 Uiso 1 1 calc R . . H62B H 0.3823 0.3034 0.4234 0.121 Uiso 1 1 calc R . . H62C H 0.3385 0.3235 0.4555 0.121 Uiso 1 1 calc R . . C63 C 0.3544(6) 0.5024(3) 0.4777(6) 0.053(3) Uani 1 1 d . . . C64 C 0.4142(6) 0.4878(3) 0.5000(6) 0.054(3) Uani 1 1 d . . . H64 H 0.4523 0.5003 0.5221 0.064 Uiso 1 1 calc R . . C65 C 0.4049(5) 0.4515(3) 0.4825(6) 0.046(3) Uani 1 1 d . . . C66 C 0.3378(6) 0.5420(3) 0.4846(7) 0.059(4) Uani 1 1 d . . . H66A H 0.3210 0.5535 0.4391 0.089 Uiso 1 1 calc R . . H66B H 0.3747 0.5554 0.5136 0.089 Uiso 1 1 calc R . . H66C H 0.3068 0.5429 0.5055 0.089 Uiso 1 1 calc R . . C67 C 0.4511(6) 0.4219(4) 0.4907(7) 0.067(4) Uani 1 1 d . . . H67A H 0.4407 0.4004 0.5122 0.101 Uiso 1 1 calc R . . H67B H 0.4921 0.4309 0.5198 0.101 Uiso 1 1 calc R . . H67C H 0.4510 0.4151 0.4456 0.101 Uiso 1 1 calc R . . B1 B 0.1234(6) 0.4833(3) 0.1435(6) 0.038(3) Uani 1 1 d . . . H1 H 0.0872 0.4877 0.1000 0.046 Uiso 1 1 calc R . . B2 B 0.3140(7) 0.4055(3) 0.4414(7) 0.051(4) Uani 1 1 d . . . H2 H 0.3345 0.3912 0.4846 0.062 Uiso 1 1 calc R . . O5 O 0.1842(14) 0.4057(8) 0.0460(14) 0.224(10) Uiso 1 1 d D . . C68 C 0.2202(19) 0.3788(12) 0.028(2) 0.245(18) Uiso 1 1 d D . . H68A H 0.2622 0.3892 0.0427 0.293 Uiso 1 1 calc R . . H68B H 0.2233 0.3574 0.0587 0.293 Uiso 1 1 calc R . . C69 C 0.207(3) 0.3645(17) -0.036(3) 0.35(3) Uiso 1 1 d D . . H69A H 0.2283 0.3405 -0.0305 0.414 Uiso 1 1 calc R . . H69B H 0.2252 0.3810 -0.0605 0.414 Uiso 1 1 calc R . . C70 C 0.107(2) 0.3892(14) -0.069(2) 0.26(2) Uiso 1 1 d D . . H70A H 0.1118 0.4104 -0.0960 0.314 Uiso 1 1 calc R . . H70B H 0.0634 0.3819 -0.0868 0.314 Uiso 1 1 calc R . . C71 C 0.1237(16) 0.4000(11) -0.002(2) 0.214(15) Uiso 1 1 d D . . H71A H 0.1050 0.3817 0.0191 0.256 Uiso 1 1 calc R . . H71B H 0.1016 0.4234 -0.0039 0.256 Uiso 1 1 calc R . . O6 O 0.143(3) 0.3592(16) -0.078(3) 0.44(3) Uiso 1 1 d D . . C72 C 0.507(4) 0.4199(17) 0.293(3) 0.240(15) Uiso 0.50 1 d PD A -1 H72A H 0.5125 0.4219 0.2491 0.360 Uiso 0.50 1 calc PR A -1 H72B H 0.5287 0.4402 0.3231 0.360 Uiso 0.50 1 calc PR A -1 H72C H 0.4628 0.4214 0.2845 0.360 Uiso 0.50 1 calc PR A -1 C73 C 0.533(3) 0.3827(18) 0.327(3) 0.240(15) Uiso 0.50 1 d PD A -1 H73A H 0.5124 0.3622 0.2961 0.288 Uiso 0.50 1 calc PR A -1 H73B H 0.5776 0.3814 0.3372 0.288 Uiso 0.50 1 calc PR A -1 C74 C 0.522(3) 0.3792(16) 0.393(3) 0.240(15) Uiso 0.50 1 d PD A -1 H74A H 0.4837 0.3648 0.3845 0.288 Uiso 0.50 1 calc PR A -1 H74B H 0.5153 0.4041 0.4088 0.288 Uiso 0.50 1 calc PR A -1 C75 C 0.575(3) 0.3606(16) 0.451(3) 0.240(15) Uiso 0.50 1 d PD A -1 H75A H 0.5748 0.3678 0.4961 0.288 Uiso 0.50 1 calc PR A -1 H75B H 0.6149 0.3683 0.4487 0.288 Uiso 0.50 1 calc PR A -1 C76 C 0.567(3) 0.3189(15) 0.441(3) 0.240(15) Uiso 0.50 1 d PD A -1 H76A H 0.6004 0.3060 0.4778 0.288 Uiso 0.50 1 calc PR A -1 H76B H 0.5271 0.3113 0.4432 0.288 Uiso 0.50 1 calc PR A -1 C77 C 0.568(4) 0.3094(18) 0.372(4) 0.240(15) Uiso 0.50 1 d PD A -1 H77A H 0.5593 0.2832 0.3622 0.360 Uiso 0.50 1 calc PR A -1 H77B H 0.6093 0.3149 0.3715 0.360 Uiso 0.50 1 calc PR A -1 H77C H 0.5374 0.3241 0.3360 0.360 Uiso 0.50 1 calc PR A -1 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 La1 0.0395(3) 0.0311(3) 0.0281(3) 0.0096(3) 0.0034(2) -0.0094(3) Ni1 0.0456(8) 0.0172(6) 0.0339(7) -0.0002(5) 0.0042(6) -0.0026(6) O1 0.057(5) 0.016(3) 0.047(5) -0.007(3) 0.012(4) -0.003(3) O2 0.057(5) 0.017(3) 0.035(4) -0.002(3) 0.009(4) -0.005(3) O3 0.040(4) 0.032(4) 0.055(5) 0.011(4) 0.012(4) -0.003(4) O4 0.040(4) 0.029(4) 0.041(4) 0.010(3) 0.008(3) -0.003(3) N1 0.049(5) 0.015(4) 0.034(5) 0.003(3) 0.009(4) -0.002(4) N2 0.040(5) 0.020(4) 0.032(5) 0.002(3) 0.007(4) 0.000(4) N3 0.051(6) 0.034(5) 0.024(4) 0.005(4) 0.011(4) -0.006(4) N4 0.039(5) 0.049(5) 0.028(5) 0.009(4) 0.000(4) -0.008(4) N5 0.048(6) 0.042(5) 0.032(5) 0.018(4) 0.001(4) -0.014(4) N6 0.049(6) 0.041(5) 0.027(5) 0.012(4) 0.002(4) -0.009(4) N7 0.039(5) 0.045(5) 0.031(5) 0.011(4) 0.005(4) 0.000(4) N8 0.036(5) 0.043(5) 0.033(5) 0.010(4) 0.005(4) -0.009(4) N9 0.058(6) 0.034(5) 0.031(5) 0.008(4) -0.001(5) -0.008(4) N10 0.048(6) 0.038(5) 0.026(5) 0.005(4) 0.002(4) -0.004(4) N11 0.062(6) 0.025(5) 0.044(6) 0.013(4) 0.003(5) -0.008(4) N12 0.041(5) 0.045(5) 0.046(6) 0.012(5) 0.013(5) 0.008(4) N13 0.052(6) 0.033(5) 0.041(5) 0.014(4) -0.005(5) -0.010(4) N14 0.061(6) 0.033(5) 0.027(5) 0.003(4) -0.004(4) -0.013(4) C1 0.045(7) 0.026(5) 0.038(6) 0.004(5) 0.012(5) 0.004(5) C2 0.071(9) 0.023(6) 0.038(6) 0.006(5) 0.013(6) 0.006(6) C3 0.067(8) 0.030(6) 0.032(6) 0.004(5) 0.016(6) 0.009(6) C4 0.078(9) 0.029(6) 0.042(7) 0.006(5) 0.022(6) 0.001(6) C5 0.077(9) 0.025(6) 0.048(7) 0.005(5) 0.027(7) 0.004(6) C6 0.072(9) 0.039(7) 0.043(7) 0.016(5) 0.014(6) 0.000(6) C7 0.079(9) 0.024(6) 0.032(6) -0.004(5) 0.002(6) 0.000(6) C8 0.084(9) 0.033(6) 0.039(7) -0.004(5) -0.008(7) 0.006(6) C9 0.073(8) 0.020(5) 0.062(8) 0.007(5) 0.018(7) 0.001(5) C10 0.093(10) 0.037(7) 0.046(7) -0.007(6) 0.013(7) 0.001(7) C11 0.074(9) 0.050(8) 0.064(9) 0.003(6) 0.033(7) 0.000(7) C12 0.083(10) 0.058(9) 0.095(12) 0.004(8) 0.045(9) 0.020(8) C13 0.117(14) 0.077(11) 0.093(12) -0.013(9) 0.063(11) 0.003(10) C14 0.071(10) 0.066(9) 0.103(12) 0.001(8) 0.046(9) 0.012(8) C15 0.056(7) 0.037(6) 0.035(6) 0.000(5) 0.013(6) -0.002(6) C16 0.047(7) 0.024(5) 0.032(6) 0.000(4) -0.002(5) -0.001(5) C17 0.051(7) 0.022(5) 0.030(6) 0.001(4) 0.008(5) -0.006(5) C18 0.041(6) 0.022(5) 0.033(6) 0.003(4) -0.002(5) -0.009(5) C19 0.039(6) 0.027(5) 0.037(6) -0.006(5) 0.000(5) -0.006(5) C20 0.040(6) 0.031(6) 0.037(6) -0.003(5) 0.007(5) 0.003(5) C21 0.049(7) 0.024(5) 0.035(6) -0.007(4) 0.005(5) -0.005(5) C22 0.063(8) 0.017(5) 0.050(7) -0.005(5) 0.009(6) -0.010(5) C23 0.072(8) 0.025(6) 0.036(6) -0.005(5) -0.001(6) -0.002(5) C24 0.073(8) 0.016(5) 0.040(6) 0.003(5) 0.007(6) -0.002(5) C25 0.080(9) 0.025(6) 0.087(10) 0.000(6) 0.029(8) -0.010(6) C26 0.042(7) 0.042(7) 0.058(8) -0.002(6) 0.015(6) -0.001(5) C27 0.046(9) 0.102(14) 0.19(2) -0.085(14) 0.012(11) 0.006(9) C28 0.130(17) 0.18(2) 0.132(17) 0.061(16) 0.103(15) 0.073(16) C29 0.081(11) 0.046(8) 0.126(15) -0.003(9) 0.034(10) 0.016(7) C30 0.042(6) 0.016(5) 0.033(6) 0.004(4) 0.008(5) -0.005(4) C31 0.041(6) 0.027(5) 0.025(5) 0.000(4) 0.005(5) -0.005(5) C32 0.037(6) 0.018(5) 0.033(6) 0.004(4) 0.005(5) -0.011(4) C33 0.039(6) 0.033(6) 0.043(6) 0.006(5) 0.005(5) 0.001(5) C34 0.047(6) 0.027(5) 0.039(6) -0.002(5) 0.015(5) -0.004(5) C35 0.046(6) 0.027(5) 0.027(5) 0.001(4) 0.008(5) -0.008(5) C36 0.038(6) 0.029(5) 0.031(6) -0.003(4) -0.002(5) -0.007(5) C37 0.046(7) 0.034(6) 0.023(5) 0.012(4) 0.001(5) -0.006(5) C38 0.039(6) 0.045(6) 0.036(6) 0.001(5) 0.012(5) -0.009(5) C39 0.060(8) 0.051(7) 0.032(6) 0.009(5) 0.024(6) 0.004(6) C40 0.052(7) 0.034(6) 0.035(6) 0.006(5) 0.016(5) 0.003(5) C41 0.065(9) 0.083(10) 0.039(7) -0.003(7) 0.017(6) -0.023(7) C42 0.073(9) 0.073(9) 0.039(7) 0.019(6) 0.008(7) 0.002(7) C43 0.064(8) 0.036(6) 0.039(7) 0.001(5) 0.004(6) -0.018(6) C44 0.080(9) 0.036(7) 0.039(7) 0.003(5) -0.006(7) -0.028(6) C45 0.055(8) 0.056(8) 0.035(6) -0.004(6) -0.002(6) -0.018(6) C46 0.076(9) 0.029(6) 0.035(6) -0.001(5) 0.001(6) -0.019(6) C47 0.058(8) 0.074(9) 0.057(8) 0.014(7) -0.015(7) -0.033(7) C48 0.041(6) 0.053(7) 0.036(6) 0.011(6) 0.009(5) 0.002(6) C49 0.057(8) 0.063(8) 0.043(7) 0.005(6) 0.022(6) 0.003(6) C50 0.042(6) 0.056(7) 0.047(7) 0.012(6) 0.021(5) 0.002(6) C51 0.068(8) 0.054(8) 0.042(7) -0.007(6) 0.009(6) 0.003(6) C52 0.054(8) 0.101(12) 0.050(8) 0.008(8) -0.001(7) 0.024(8) C53 0.052(8) 0.039(6) 0.034(6) -0.007(5) 0.005(6) -0.008(5) C54 0.073(9) 0.050(7) 0.032(6) -0.011(5) 0.023(6) -0.027(6) C55 0.066(8) 0.038(6) 0.025(6) 0.001(5) 0.008(6) -0.023(6) C56 0.043(7) 0.066(8) 0.046(7) -0.003(6) 0.024(6) -0.014(6) C57 0.089(10) 0.052(8) 0.044(7) 0.015(6) 0.007(7) -0.017(7) C58 0.055(8) 0.045(7) 0.061(8) -0.005(6) 0.026(7) -0.009(6) C59 0.079(10) 0.045(8) 0.076(11) -0.002(7) -0.003(9) 0.007(7) C60 0.078(10) 0.027(7) 0.063(10) 0.009(6) -0.012(8) -0.007(6) C61 0.117(12) 0.050(8) 0.064(9) 0.001(7) 0.046(9) -0.008(8) C62 0.094(11) 0.036(7) 0.084(11) 0.019(7) 0.001(9) -0.001(7) C63 0.062(8) 0.046(7) 0.033(6) 0.012(5) -0.004(6) -0.007(6) C64 0.058(8) 0.054(8) 0.033(6) 0.002(6) 0.000(6) -0.022(6) C65 0.044(7) 0.049(7) 0.036(6) 0.011(5) 0.005(6) -0.009(6) C66 0.071(9) 0.039(7) 0.050(7) -0.005(6) 0.003(7) -0.013(6) C67 0.056(8) 0.078(10) 0.053(8) -0.001(7) 0.004(7) 0.002(7) B1 0.042(7) 0.046(7) 0.024(6) 0.005(5) 0.008(6) 0.000(6) B2 0.071(10) 0.032(7) 0.036(7) 0.021(6) 0.004(7) 0.003(7) _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 La1 O4 2.484(7) . ? La1 O3 2.557(7) . ? La1 N8 2.585(9) . ? La1 N12 2.607(9) . ? La1 N10 2.635(9) . ? La1 N6 2.706(8) . ? La1 N4 2.712(9) . ? La1 N14 2.775(8) . ? La1 C37 2.864(11) . ? Ni1 O1 1.832(7) . ? Ni1 O2 1.844(8) . ? Ni1 N2 1.849(8) . ? Ni1 N1 1.851(9) . ? O1 C2 1.269(15) . ? O2 C17 1.287(13) . ? O3 C37 1.254(13) . ? O4 C37 1.282(12) . ? N1 C15 1.292(14) . ? N1 C31 1.411(12) . ? N2 C30 1.288(13) . ? N2 C32 1.427(12) . ? N3 C40 1.352(14) . ? N3 N4 1.387(12) . ? N3 B1 1.520(16) . ? N4 C38 1.330(14) . ? N5 C45 1.349(14) . ? N5 N6 1.395(11) . ? N5 B1 1.529(15) . ? N6 C43 1.350(14) . ? N7 C50 1.356(14) . ? N7 N8 1.398(12) . ? N7 B1 1.532(16) . ? N8 C48 1.325(15) . ? N9 C55 1.342(14) . ? N9 N10 1.390(12) . ? N9 B2 1.538(19) . ? N10 C53 1.331(15) . ? N11 C60 1.326(16) . ? N11 N12 1.380(13) . ? N11 B2 1.538(19) . ? N12 C58 1.331(16) . ? N13 C65 1.356(14) . ? N13 N14 1.378(13) . ? N13 B2 1.570(15) . ? N14 C63 1.338(14) . ? C1 C6 1.390(17) . ? C1 C15 1.433(15) . ? C1 C2 1.461(16) . ? C2 C3 1.460(15) . ? C3 C4 1.363(17) . ? C3 C7 1.529(17) . ? C4 C5 1.431(17) . ? C5 C6 1.358(16) . ? C5 C11 1.514(19) . ? C7 C9 1.537(18) . ? C7 C8 1.545(15) . ? C7 C10 1.553(16) . ? C11 C12 1.513(19) . ? C11 C14 1.516(19) . ? C11 C13 1.55(2) . ? C16 C21 1.410(16) . ? C16 C30 1.423(15) . ? C16 C17 1.435(14) . ? C17 C18 1.431(15) . ? C18 C19 1.372(16) . ? C18 C22 1.549(14) . ? C19 C20 1.437(14) . ? C20 C21 1.351(15) . ? C20 C26 1.540(16) . ? C22 C25 1.540(18) . ? C22 C24 1.540(15) . ? C22 C23 1.543(17) . ? C26 C28 1.48(2) . ? C26 C29 1.511(17) . ? C26 C27 1.518(18) . ? C31 C32 1.371(15) . ? C31 C36 1.392(15) . ? C32 C33 1.407(14) . ? C33 C34 1.367(15) . ? C34 C35 1.398(15) . ? C35 C36 1.409(14) . ? C35 C37 1.512(15) . ? C38 C39 1.398(15) . ? C38 C41 1.497(17) . ? C39 C40 1.338(16) . ? C40 C42 1.500(16) . ? C43 C44 1.391(16) . ? C43 C46 1.483(16) . ? C44 C45 1.375(16) . ? C45 C47 1.521(16) . ? C48 C49 1.376(16) . ? C48 C51 1.514(16) . ? C49 C50 1.355(17) . ? C50 C52 1.521(16) . ? C53 C54 1.392(16) . ? C53 C56 1.501(16) . ? C54 C55 1.392(17) . ? C55 C57 1.505(16) . ? C58 C59 1.376(18) . ? C58 C61 1.488(18) . ? C59 C60 1.37(2) . ? C60 C62 1.514(18) . ? C63 C64 1.403(18) . ? C63 C66 1.515(17) . ? C64 C65 1.367(16) . ? C65 C67 1.488(18) . ? O5 C71 1.41(2) . ? O5 C68 1.43(2) . ? C68 C69 1.36(4) . ? C69 O6 1.44(3) . ? C70 C71 1.36(4) . ? C70 O6 1.43(3) . ? C72 C73 1.55(2) . ? C73 C74 1.51(2) . ? C74 C75 1.53(2) . ? C75 C76 1.53(2) . ? C76 C77 1.51(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 O4 La1 O3 52.5(2) . . ? O4 La1 N8 129.8(2) . . ? O3 La1 N8 79.0(2) . . ? O4 La1 N12 75.7(3) . . ? O3 La1 N12 127.7(3) . . ? N8 La1 N12 152.9(3) . . ? O4 La1 N10 133.9(2) . . ? O3 La1 N10 131.7(3) . . ? N8 La1 N10 86.2(3) . . ? N12 La1 N10 78.3(3) . . ? O4 La1 N6 136.8(3) . . ? O3 La1 N6 142.7(2) . . ? N8 La1 N6 74.7(3) . . ? N12 La1 N6 79.4(3) . . ? N10 La1 N6 72.5(3) . . ? O4 La1 N4 81.9(2) . . ? O3 La1 N4 78.6(3) . . ? N8 La1 N4 76.0(3) . . ? N12 La1 N4 102.6(3) . . ? N10 La1 N4 141.2(3) . . ? N6 La1 N4 69.7(3) . . ? O4 La1 N14 76.4(3) . . ? O3 La1 N14 75.1(2) . . ? N8 La1 N14 105.7(3) . . ? N12 La1 N14 87.9(3) . . ? N10 La1 N14 65.2(3) . . ? N6 La1 N14 137.4(3) . . ? N4 La1 N14 152.8(3) . . ? O4 La1 C37 26.6(3) . . ? O3 La1 C37 26.0(3) . . ? N8 La1 C37 104.1(3) . . ? N12 La1 C37 102.1(3) . . ? N10 La1 C37 139.9(3) . . ? N6 La1 C37 147.6(3) . . ? N4 La1 C37 78.5(3) . . ? N14 La1 C37 74.7(3) . . ? O1 Ni1 O2 85.5(3) . . ? O1 Ni1 N2 173.6(3) . . ? O2 Ni1 N2 94.3(4) . . ? O1 Ni1 N1 94.7(4) . . ? O2 Ni1 N1 174.9(3) . . ? N2 Ni1 N1 86.0(4) . . ? C2 O1 Ni1 129.9(7) . . ? C17 O2 Ni1 129.6(6) . . ? C37 O3 La1 90.8(6) . . ? C37 O4 La1 93.5(6) . . ? C15 N1 C31 122.4(9) . . ? C15 N1 Ni1 124.3(7) . . ? C31 N1 Ni1 113.1(7) . . ? C30 N2 C32 121.1(8) . . ? C30 N2 Ni1 126.2(7) . . ? C32 N2 Ni1 112.6(7) . . ? C40 N3 N4 108.9(9) . . ? C40 N3 B1 126.8(9) . . ? N4 N3 B1 124.3(8) . . ? C38 N4 N3 105.7(8) . . ? C38 N4 La1 135.7(7) . . ? N3 N4 La1 117.6(6) . . ? C45 N5 N6 109.3(8) . . ? C45 N5 B1 127.3(9) . . ? N6 N5 B1 123.3(8) . . ? C43 N6 N5 106.1(8) . . ? C43 N6 La1 134.0(7) . . ? N5 N6 La1 118.4(6) . . ? C50 N7 N8 107.2(9) . . ? C50 N7 B1 132.3(9) . . ? N8 N7 B1 120.5(9) . . ? C48 N8 N7 106.5(8) . . ? C48 N8 La1 129.7(7) . . ? N7 N8 La1 123.7(7) . . ? C55 N9 N10 109.3(9) . . ? C55 N9 B2 127.9(9) . . ? N10 N9 B2 122.2(9) . . ? C53 N10 N9 106.3(9) . . ? C53 N10 La1 137.8(7) . . ? N9 N10 La1 114.8(7) . . ? C60 N11 N12 109.1(11) . . ? C60 N11 B2 131.6(10) . . ? N12 N11 B2 119.3(9) . . ? C58 N12 N11 107.1(9) . . ? C58 N12 La1 134.9(8) . . ? N11 N12 La1 117.8(7) . . ? C65 N13 N14 109.8(9) . . ? C65 N13 B2 124.0(10) . . ? N14 N13 B2 124.2(10) . . ? C63 N14 N13 104.7(9) . . ? C63 N14 La1 124.2(7) . . ? N13 N14 La1 89.4(6) . . ? C6 C1 C15 119.1(11) . . ? C6 C1 C2 121.9(10) . . ? C15 C1 C2 119.0(10) . . ? O1 C2 C3 122.5(11) . . ? O1 C2 C1 122.7(10) . . ? C3 C2 C1 114.8(12) . . ? C4 C3 C2 118.8(11) . . ? C4 C3 C7 122.7(10) . . ? C2 C3 C7 118.5(11) . . ? C3 C4 C5 125.6(11) . . ? C6 C5 C4 115.7(12) . . ? C6 C5 C11 125.8(12) . . ? C4 C5 C11 118.5(10) . . ? C5 C6 C1 122.9(12) . . ? C3 C7 C9 109.1(9) . . ? C3 C7 C8 110.7(9) . . ? C9 C7 C8 111.2(11) . . ? C3 C7 C10 111.4(11) . . ? C9 C7 C10 108.3(9) . . ? C8 C7 C10 106.1(9) . . ? C12 C11 C5 110.2(11) . . ? C12 C11 C14 109.1(12) . . ? C5 C11 C14 110.6(11) . . ? C12 C11 C13 109.5(12) . . ? C5 C11 C13 109.2(12) . . ? C14 C11 C13 108.2(13) . . ? N1 C15 C1 127.3(11) . . ? C21 C16 C30 117.7(9) . . ? C21 C16 C17 121.2(10) . . ? C30 C16 C17 121.1(11) . . ? O2 C17 C18 120.8(9) . . ? O2 C17 C16 122.5(10) . . ? C18 C17 C16 116.7(11) . . ? C19 C18 C17 119.0(9) . . ? C19 C18 C22 122.2(10) . . ? C17 C18 C22 118.8(10) . . ? C18 C19 C20 124.5(10) . . ? C21 C20 C19 116.1(10) . . ? C21 C20 C26 124.9(10) . . ? C19 C20 C26 119.0(10) . . ? C20 C21 C16 122.5(10) . . ? C25 C22 C24 107.4(10) . . ? C25 C22 C23 108.5(10) . . ? C24 C22 C23 109.2(10) . . ? C25 C22 C18 111.2(10) . . ? C24 C22 C18 111.1(8) . . ? C23 C22 C18 109.3(9) . . ? C28 C26 C29 107.5(14) . . ? C28 C26 C27 111.5(16) . . ? C29 C26 C27 108.2(12) . . ? C28 C26 C20 110.8(11) . . ? C29 C26 C20 110.0(11) . . ? C27 C26 C20 108.8(11) . . ? N2 C30 C16 126.2(9) . . ? C32 C31 C36 120.7(9) . . ? C32 C31 N1 114.1(9) . . ? C36 C31 N1 125.2(10) . . ? C31 C32 C33 119.9(9) . . ? C31 C32 N2 113.9(8) . . ? C33 C32 N2 126.1(10) . . ? C34 C33 C32 120.6(11) . . ? C33 C34 C35 119.4(10) . . ? C34 C35 C36 120.6(10) . . ? C34 C35 C37 119.6(9) . . ? C36 C35 C37 119.7(10) . . ? C31 C36 C35 118.7(11) . . ? O3 C37 O4 123.2(10) . . ? O3 C37 C35 119.9(9) . . ? O4 C37 C35 116.9(10) . . ? O3 C37 La1 63.2(5) . . ? O4 C37 La1 60.0(5) . . ? C35 C37 La1 175.1(8) . . ? N4 C38 C39 110.4(10) . . ? N4 C38 C41 123.9(10) . . ? C39 C38 C41 125.7(11) . . ? C40 C39 C38 105.9(10) . . ? C39 C40 N3 109.0(10) . . ? C39 C40 C42 127.8(11) . . ? N3 C40 C42 123.2(11) . . ? N6 C43 C44 109.7(10) . . ? N6 C43 C46 124.7(10) . . ? C44 C43 C46 125.5(10) . . ? C45 C44 C43 106.5(10) . . ? N5 C45 C44 108.3(10) . . ? N5 C45 C47 122.9(11) . . ? C44 C45 C47 128.8(11) . . ? N8 C48 C49 110.9(10) . . ? N8 C48 C51 120.5(10) . . ? C49 C48 C51 128.4(12) . . ? C50 C49 C48 105.6(12) . . ? C49 C50 N7 109.6(10) . . ? C49 C50 C52 129.3(12) . . ? N7 C50 C52 121.0(11) . . ? N10 C53 C54 110.9(10) . . ? N10 C53 C56 122.3(10) . . ? C54 C53 C56 126.8(11) . . ? C55 C54 C53 104.9(11) . . ? N9 C55 C54 108.5(10) . . ? N9 C55 C57 124.7(12) . . ? C54 C55 C57 126.8(11) . . ? N12 C58 C59 108.8(13) . . ? N12 C58 C61 120.9(11) . . ? C59 C58 C61 130.2(14) . . ? C60 C59 C58 106.9(13) . . ? N11 C60 C59 108.1(11) . . ? N11 C60 C62 122.8(15) . . ? C59 C60 C62 129.1(14) . . ? N14 C63 C64 112.4(11) . . ? N14 C63 C66 121.6(11) . . ? C64 C63 C66 125.9(11) . . ? C65 C64 C63 103.6(10) . . ? N13 C65 C64 109.5(11) . . ? N13 C65 C67 121.4(11) . . ? C64 C65 C67 129.0(12) . . ? N3 B1 N5 112.8(10) . . ? N3 B1 N7 112.6(9) . . ? N5 B1 N7 110.3(9) . . ? N9 B2 N11 112.2(10) . . ? N9 B2 N13 111.6(10) . . ? N11 B2 N13 107.6(10) . . ? C71 O5 C68 104(3) . . ? C69 C68 O5 126(4) . . ? C68 C69 O6 117(6) . . ? C71 C70 O6 114(5) . . ? C70 C71 O5 127(4) . . ? C70 O6 C69 110(6) . . ? C74 C73 C72 109(2) . . ? C73 C74 C75 113(2) . . ? C74 C75 C76 107.9(19) . . ? C77 C76 C75 107.9(19) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.991 _refine_diff_density_min -0.914 _refine_diff_density_rms 0.125 data_s045_fin _database_code_depnum_ccdc_archive 'CCDC 736172' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H103 B2 Cu La N14 O4' _chemical_formula_weight 1464.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.5597(15) _cell_length_b 22.6673(16) _cell_length_c 21.8126(16) _cell_angle_alpha 90.00 _cell_angle_beta 107.794(9) _cell_angle_gamma 90.00 _cell_volume 7796.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 7998 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 25.70 _exptl_crystal_description platelet _exptl_crystal_colour 'orange brown' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3068 _exptl_absorpt_coefficient_mu 0.867 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8307 _exptl_absorpt_correction_T_max 0.9608 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Stoe IPDS area detector' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57213 _diffrn_reflns_av_R_equivalents 0.0829 _diffrn_reflns_av_sigmaI/netI 0.1393 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 26.03 _reflns_number_total 14483 _reflns_number_gt 6778 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software, STOE X-RED' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14483 _refine_ls_number_parameters 888 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0747 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 0.663 _refine_ls_restrained_S_all 0.670 _refine_ls_shift/su_max 0.008 _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 La1 La 0.448703(16) 0.214223(10) 0.369721(13) 0.04719(7) Uani 1 1 d . . . Cu1 Cu 0.17221(3) 0.54314(2) 0.13892(3) 0.05596(15) Uani 1 1 d . . . O1 O 0.13478(18) 0.60374(12) 0.18310(18) 0.0635(9) Uani 1 1 d . . . O2 O 0.11825(19) 0.57991(12) 0.05971(17) 0.0655(9) Uani 1 1 d . . . O3 O 0.3594(2) 0.30525(12) 0.33442(16) 0.0672(9) Uani 1 1 d . . . O4 O 0.43687(18) 0.27599(11) 0.27316(13) 0.0607(8) Uani 1 1 d . . . N1 N 0.2196(2) 0.49724(13) 0.21622(19) 0.0530(9) Uani 1 1 d . . . N2 N 0.2229(2) 0.48371(13) 0.0995(2) 0.0571(10) Uani 1 1 d . . . N3 N 0.5421(2) 0.32443(15) 0.4824(2) 0.0587(10) Uani 1 1 d . . . N4 N 0.5445(2) 0.31184(15) 0.4215(2) 0.0606(10) Uani 1 1 d . . . N5 N 0.4404(2) 0.26135(13) 0.52224(18) 0.0500(9) Uani 1 1 d . . . N6 N 0.3911(2) 0.23586(13) 0.46632(17) 0.0504(9) Uani 1 1 d . . . N7 N 0.5878(2) 0.22248(15) 0.52871(17) 0.0550(9) Uani 1 1 d . . . N8 N 0.5745(2) 0.18830(15) 0.47394(18) 0.0548(10) Uani 1 1 d . . . N9 N 0.3403(2) 0.11519(17) 0.24150(19) 0.0628(10) Uani 1 1 d . . . N10 N 0.3215(2) 0.16570(17) 0.27051(19) 0.0607(11) Uani 1 1 d . . . N11 N 0.5015(2) 0.10378(14) 0.27302(17) 0.0527(9) Uani 1 1 d . . . N12 N 0.5299(2) 0.15548(14) 0.30539(17) 0.0519(9) Uani 1 1 d . . . N13 N 0.4184(2) 0.05828(14) 0.34209(17) 0.0527(9) Uani 1 1 d . . . N14 N 0.4236(2) 0.09950(14) 0.38972(18) 0.0537(9) Uani 1 1 d . . . C1 C 0.1814(3) 0.56408(17) 0.2902(3) 0.0559(12) Uani 1 1 d . . . C2 C 0.1426(3) 0.60829(18) 0.2441(3) 0.0566(12) Uani 1 1 d . . . C3 C 0.1101(3) 0.66011(18) 0.2676(3) 0.0557(12) Uani 1 1 d . . . C4 C 0.1182(3) 0.66321(19) 0.3312(3) 0.0675(14) Uani 1 1 d . . . H4 H 0.0970 0.6973 0.3455 0.081 Uiso 1 1 calc R . . C5 C 0.1561(3) 0.61932(19) 0.3788(3) 0.0651(13) Uani 1 1 d . . . C6 C 0.1863(3) 0.57113(19) 0.3553(3) 0.0677(14) Uani 1 1 d . . . H6 H 0.2119 0.5409 0.3842 0.081 Uiso 1 1 calc R . . C7 C 0.0673(2) 0.70937(19) 0.2208(2) 0.0637(12) Uani 1 1 d . . . C8 C -0.0116(3) 0.6854(2) 0.1710(3) 0.0842(17) Uani 1 1 d . . . H8A H 0.0043 0.6534 0.1475 0.126 Uiso 1 1 calc R . . H8B H -0.0384 0.7166 0.1414 0.126 Uiso 1 1 calc R . . H8C H -0.0509 0.6708 0.1926 0.126 Uiso 1 1 calc R . . C9 C 0.1286(3) 0.73477(19) 0.1871(3) 0.0783(16) Uani 1 1 d . . . H9A H 0.1783 0.7506 0.2191 0.118 Uiso 1 1 calc R . . H9B H 0.1006 0.7660 0.1579 0.118 Uiso 1 1 calc R . . H9C H 0.1458 0.7038 0.1630 0.118 Uiso 1 1 calc R . . C10 C 0.0398(3) 0.76054(19) 0.2555(3) 0.0861(17) Uani 1 1 d . . . H10A H 0.0000 0.7463 0.2768 0.129 Uiso 1 1 calc R . . H10B H 0.0129 0.7907 0.2245 0.129 Uiso 1 1 calc R . . H10C H 0.0891 0.7770 0.2873 0.129 Uiso 1 1 calc R . . C11 C 0.1593(4) 0.6292(2) 0.4490(3) 0.0853(17) Uani 1 1 d . . . C12 C 0.2164(4) 0.6824(2) 0.4768(3) 0.0986(19) Uani 1 1 d . . . H12A H 0.2134 0.6911 0.5196 0.148 Uiso 1 1 calc R . . H12B H 0.1972 0.7164 0.4492 0.148 Uiso 1 1 calc R . . H12C H 0.2745 0.6732 0.4792 0.148 Uiso 1 1 calc R . . C13 C 0.0701(4) 0.6404(3) 0.4523(3) 0.113(2) Uani 1 1 d . . . H13A H 0.0344 0.6066 0.4347 0.169 Uiso 1 1 calc R . . H13B H 0.0469 0.6753 0.4274 0.169 Uiso 1 1 calc R . . H13C H 0.0720 0.6462 0.4968 0.169 Uiso 1 1 calc R . . C14 C 0.1940(4) 0.5748(2) 0.4901(3) 0.108(2) Uani 1 1 d . . . H14A H 0.2503 0.5658 0.4877 0.162 Uiso 1 1 calc R . . H14B H 0.1568 0.5415 0.4742 0.162 Uiso 1 1 calc R . . H14C H 0.1971 0.5827 0.5345 0.162 Uiso 1 1 calc R . . C15 C 0.2176(3) 0.51242(17) 0.2730(2) 0.0566(12) Uani 1 1 d . . . H15 H 0.2431 0.4861 0.3067 0.068 Uiso 1 1 calc R . . C16 C 0.1655(3) 0.51720(17) -0.0108(2) 0.0561(12) Uani 1 1 d . . . C17 C 0.1170(3) 0.56492(18) 0.0023(3) 0.0555(12) Uani 1 1 d . . . C18 C 0.0648(3) 0.59714(18) -0.0526(3) 0.0602(13) Uani 1 1 d . . . C19 C 0.0666(3) 0.5808(2) -0.1125(3) 0.0695(14) Uani 1 1 d . . . H19 H 0.0326 0.6026 -0.1476 0.083 Uiso 1 1 calc R . . C20 C 0.1152(3) 0.5339(2) -0.1269(2) 0.0646(14) Uani 1 1 d . . . C21 C 0.1635(3) 0.50306(19) -0.0741(3) 0.0654(13) Uani 1 1 d . . . H21 H 0.1965 0.4713 -0.0805 0.078 Uiso 1 1 calc R . . C22 C 0.0089(3) 0.6479(2) -0.0427(3) 0.0744(15) Uani 1 1 d . . . C23 C -0.0423(4) 0.6764(3) -0.1059(3) 0.140(3) Uani 1 1 d . . . H23A H -0.0783 0.7070 -0.0973 0.209 Uiso 1 1 calc R . . H23B H -0.0771 0.6468 -0.1338 0.209 Uiso 1 1 calc R . . H23C H -0.0039 0.6936 -0.1268 0.209 Uiso 1 1 calc R . . C24 C 0.0650(4) 0.6954(2) -0.0002(3) 0.106(2) Uani 1 1 d . . . H24A H 0.1003 0.6775 0.0394 0.159 Uiso 1 1 calc R . . H24B H 0.0294 0.7254 0.0100 0.159 Uiso 1 1 calc R . . H24C H 0.1008 0.7132 -0.0230 0.159 Uiso 1 1 calc R . . C25 C -0.0540(3) 0.6252(3) -0.0092(3) 0.102(2) Uani 1 1 d . . . H25A H -0.0230 0.6075 0.0317 0.153 Uiso 1 1 calc R . . H25B H -0.0907 0.5958 -0.0362 0.153 Uiso 1 1 calc R . . H25C H -0.0879 0.6577 -0.0020 0.153 Uiso 1 1 calc R . . C26 C 0.1102(3) 0.5194(2) -0.1955(3) 0.0773(16) Uani 1 1 d . . . C27 C 0.1425(4) 0.5720(2) -0.2265(3) 0.0997(19) Uani 1 1 d . . . H27A H 0.1089 0.6067 -0.2250 0.150 Uiso 1 1 calc R . . H27B H 0.1373 0.5627 -0.2709 0.150 Uiso 1 1 calc R . . H27C H 0.2015 0.5795 -0.2030 0.150 Uiso 1 1 calc R . . C28 C 0.0181(4) 0.5053(3) -0.2358(3) 0.117(2) Uani 1 1 d . . . H28A H -0.0038 0.4738 -0.2152 0.175 Uiso 1 1 calc R . . H28B H 0.0169 0.4930 -0.2786 0.175 Uiso 1 1 calc R . . H28C H -0.0167 0.5402 -0.2388 0.175 Uiso 1 1 calc R . . C29 C 0.1640(4) 0.4655(2) -0.2007(3) 0.0974(18) Uani 1 1 d . . . H29A H 0.2227 0.4726 -0.1761 0.146 Uiso 1 1 calc R . . H29B H 0.1598 0.4589 -0.2455 0.146 Uiso 1 1 calc R . . H29C H 0.1433 0.4311 -0.1838 0.146 Uiso 1 1 calc R . . C30 C 0.2142(3) 0.47987(17) 0.0388(3) 0.0571(12) Uani 1 1 d . . . H30 H 0.2433 0.4489 0.0261 0.069 Uiso 1 1 calc R . . C31 C 0.2634(2) 0.44613(16) 0.2060(2) 0.0479(11) Uani 1 1 d . . . C32 C 0.2676(3) 0.44039(17) 0.1435(2) 0.0545(12) Uani 1 1 d . . . C33 C 0.3139(3) 0.39407(19) 0.1286(2) 0.0704(14) Uani 1 1 d . . . H33 H 0.3183 0.3904 0.0868 0.084 Uiso 1 1 calc R . . C34 C 0.3531(3) 0.35376(18) 0.1755(2) 0.0708(14) Uani 1 1 d . . . H34 H 0.3859 0.3234 0.1659 0.085 Uiso 1 1 calc R . . C35 C 0.3448(3) 0.35743(18) 0.2364(2) 0.0545(12) Uani 1 1 d . . . C36 C 0.3003(3) 0.40347(17) 0.2521(2) 0.0526(12) Uani 1 1 d . . . H36 H 0.2948 0.4061 0.2936 0.063 Uiso 1 1 calc R . . C37 C 0.3833(3) 0.31007(18) 0.2853(2) 0.0565(12) Uani 1 1 d . . . C38 C 0.5615(3) 0.3629(2) 0.3975(3) 0.0726(14) Uani 1 1 d . . . C39 C 0.5683(3) 0.4079(2) 0.4408(3) 0.0846(17) Uani 1 1 d . . . H39 H 0.5790 0.4479 0.4348 0.102 Uiso 1 1 calc R . . C40 C 0.5563(4) 0.3828(2) 0.4943(3) 0.0803(16) Uani 1 1 d . . . C41 C 0.5762(4) 0.3690(2) 0.3330(3) 0.1003(19) Uani 1 1 d . . . H41A H 0.6359 0.3765 0.3393 0.150 Uiso 1 1 calc R . . H41B H 0.5428 0.4016 0.3095 0.150 Uiso 1 1 calc R . . H41C H 0.5595 0.3328 0.3087 0.150 Uiso 1 1 calc R . . C42 C 0.5602(5) 0.4113(2) 0.5574(3) 0.131(3) Uani 1 1 d . . . H42A H 0.5066 0.4056 0.5660 0.197 Uiso 1 1 calc R . . H42B H 0.5712 0.4532 0.5554 0.197 Uiso 1 1 calc R . . H42C H 0.6054 0.3934 0.5917 0.197 Uiso 1 1 calc R . . C43 C 0.3152(3) 0.22642(18) 0.4739(2) 0.0554(12) Uani 1 1 d . . . C44 C 0.3158(3) 0.24548(19) 0.5345(3) 0.0651(13) Uani 1 1 d . . . H44 H 0.2704 0.2436 0.5519 0.078 Uiso 1 1 calc R . . C45 C 0.3951(3) 0.26751(17) 0.5640(2) 0.0589(12) Uani 1 1 d . . . C46 C 0.2458(3) 0.1979(2) 0.4220(2) 0.0774(15) Uani 1 1 d . . . H46A H 0.2075 0.2279 0.3978 0.116 Uiso 1 1 calc R . . H46B H 0.2149 0.1709 0.4412 0.116 Uiso 1 1 calc R . . H46C H 0.2699 0.1763 0.3935 0.116 Uiso 1 1 calc R . . C47 C 0.4280(4) 0.2947(2) 0.6288(3) 0.0896(17) Uani 1 1 d . . . H47A H 0.4773 0.2729 0.6543 0.134 Uiso 1 1 calc R . . H47B H 0.3844 0.2936 0.6500 0.134 Uiso 1 1 calc R . . H47C H 0.4439 0.3353 0.6245 0.134 Uiso 1 1 calc R . . C48 C 0.6333(3) 0.14529(19) 0.4896(2) 0.0608(13) Uani 1 1 d . . . C49 C 0.6837(3) 0.1517(2) 0.5529(3) 0.0745(15) Uani 1 1 d . . . H49 H 0.7295 0.1277 0.5752 0.089 Uiso 1 1 calc R . . C50 C 0.6533(3) 0.2001(2) 0.5765(2) 0.0653(13) Uani 1 1 d . . . C51 C 0.6402(3) 0.0986(2) 0.4434(3) 0.0803(16) Uani 1 1 d . . . H51A H 0.5873 0.0961 0.4086 0.120 Uiso 1 1 calc R . . H51B H 0.6522 0.0610 0.4655 0.120 Uiso 1 1 calc R . . H51C H 0.6858 0.1085 0.4259 0.120 Uiso 1 1 calc R . . C52 C 0.6834(4) 0.2260(2) 0.6428(3) 0.0994(19) Uani 1 1 d . . . H52A H 0.7015 0.2663 0.6403 0.149 Uiso 1 1 calc R . . H52B H 0.7306 0.2029 0.6692 0.149 Uiso 1 1 calc R . . H52C H 0.6374 0.2253 0.6617 0.149 Uiso 1 1 calc R . . C53 C 0.2472(3) 0.1843(2) 0.2308(3) 0.0719(15) Uani 1 1 d . . . C54 C 0.2193(4) 0.1471(3) 0.1787(3) 0.095(2) Uani 1 1 d . . . H54 H 0.1688 0.1508 0.1444 0.114 Uiso 1 1 calc R . . C55 C 0.2786(4) 0.1043(3) 0.1864(3) 0.0897(18) Uani 1 1 d . . . C56 C 0.2015(3) 0.2373(2) 0.2451(3) 0.104(2) Uani 1 1 d . . . H56A H 0.2299 0.2509 0.2885 0.156 Uiso 1 1 calc R . . H56B H 0.1435 0.2266 0.2413 0.156 Uiso 1 1 calc R . . H56C H 0.2017 0.2684 0.2146 0.156 Uiso 1 1 calc R . . C57 C 0.2782(5) 0.0523(3) 0.1432(3) 0.144(3) Uani 1 1 d . . . H57A H 0.3267 0.0548 0.1272 0.216 Uiso 1 1 calc R . . H57B H 0.2263 0.0527 0.1072 0.216 Uiso 1 1 calc R . . H57C H 0.2812 0.0160 0.1674 0.216 Uiso 1 1 calc R . . C58 C 0.6049(3) 0.1670(2) 0.2970(2) 0.0624(13) Uani 1 1 d . . . C59 C 0.6246(3) 0.1230(2) 0.2593(2) 0.0699(14) Uani 1 1 d . . . H59 H 0.6736 0.1207 0.2462 0.084 Uiso 1 1 calc R . . C60 C 0.5594(3) 0.0844(2) 0.2451(2) 0.0619(13) Uani 1 1 d . . . C61 C 0.6556(3) 0.2191(2) 0.3287(3) 0.0960(18) Uani 1 1 d . . . H61A H 0.6498 0.2504 0.2974 0.144 Uiso 1 1 calc R . . H61B H 0.7148 0.2079 0.3459 0.144 Uiso 1 1 calc R . . H61C H 0.6351 0.2327 0.3634 0.144 Uiso 1 1 calc R . . C62 C 0.5474(4) 0.0286(2) 0.2065(3) 0.0910(17) Uani 1 1 d . . . H62A H 0.5487 -0.0049 0.2345 0.137 Uiso 1 1 calc R . . H62B H 0.5926 0.0248 0.1871 0.137 Uiso 1 1 calc R . . H62C H 0.4932 0.0298 0.1730 0.137 Uiso 1 1 calc R . . C63 C 0.4207(3) 0.06879(19) 0.4419(2) 0.0565(12) Uani 1 1 d . . . C64 C 0.4130(3) 0.00896(19) 0.4268(3) 0.0659(13) Uani 1 1 d . . . H64 H 0.4091 -0.0219 0.4546 0.079 Uiso 1 1 calc R . . C65 C 0.4120(3) 0.00354(18) 0.3645(2) 0.0598(12) Uani 1 1 d . . . C66 C 0.4264(3) 0.0967(2) 0.5042(2) 0.0797(16) Uani 1 1 d . . . H66A H 0.4755 0.1224 0.5169 0.119 Uiso 1 1 calc R . . H66B H 0.4319 0.0664 0.5366 0.119 Uiso 1 1 calc R . . H66C H 0.3755 0.1196 0.5000 0.119 Uiso 1 1 calc R . . C67 C 0.4078(4) -0.05158(19) 0.3257(3) 0.0896(17) Uani 1 1 d . . . H67A H 0.4592 -0.0554 0.3136 0.134 Uiso 1 1 calc R . . H67B H 0.3592 -0.0496 0.2872 0.134 Uiso 1 1 calc R . . H67C H 0.4020 -0.0855 0.3512 0.134 Uiso 1 1 calc R . . B1 B 0.5342(3) 0.2772(2) 0.5312(3) 0.0543(13) Uani 1 1 d . . . B2 B 0.4173(3) 0.0761(2) 0.2734(3) 0.0545(14) Uani 1 1 d . . . H1X H 0.5586(17) 0.2936(13) 0.5786(16) 0.030(8) Uiso 1 1 d . . . H2X H 0.4094(17) 0.0354(13) 0.2444(15) 0.030(8) Uiso 1 1 d . . . C68 C 0.3210(9) 0.4100(6) 0.4513(6) 0.254(8) Uani 1 1 d D . . H68A H 0.3623 0.4037 0.4287 0.381 Uiso 1 1 calc R . . H68B H 0.3420 0.3933 0.4942 0.381 Uiso 1 1 calc R . . H68C H 0.3117 0.4520 0.4545 0.381 Uiso 1 1 calc R . . C69 C 0.2356(11) 0.3795(6) 0.4137(8) 0.320(15) Uani 1 1 d D . . H69A H 0.2122 0.3957 0.3702 0.384 Uiso 1 1 calc R . . H69B H 0.2422 0.3367 0.4111 0.384 Uiso 1 1 calc R . . C70 C 0.1846(9) 0.3945(6) 0.4538(8) 0.287(8) Uani 1 1 d D . . H70A H 0.1626 0.4347 0.4443 0.345 Uiso 1 1 calc R . . H70B H 0.2185 0.3925 0.4992 0.345 Uiso 1 1 calc R . . C71 C 0.1131(10) 0.3514(7) 0.4401(12) 0.58(3) Uani 1 1 d D . . H71A H 0.1259 0.3156 0.4195 0.694 Uiso 1 1 calc R . . H71B H 0.1002 0.3404 0.4796 0.694 Uiso 1 1 calc R . . C72 C 0.0439(12) 0.3843(7) 0.3966(7) 0.358(14) Uani 1 1 d D . . H72A H 0.0589 0.3933 0.3576 0.430 Uiso 1 1 calc R . . H72B H -0.0065 0.3589 0.3841 0.430 Uiso 1 1 calc R . . C73 C 0.0221(10) 0.4381(8) 0.4217(8) 0.428(16) Uani 1 1 d D . . H73A H -0.0336 0.4343 0.4273 0.642 Uiso 1 1 calc R . . H73B H 0.0213 0.4700 0.3918 0.642 Uiso 1 1 calc R . . H73C H 0.0637 0.4466 0.4629 0.642 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.05474(14) 0.04724(12) 0.04122(15) 0.01115(13) 0.01710(10) 0.01827(14) Cu1 0.0600(3) 0.0406(3) 0.0597(4) 0.0093(2) 0.0071(3) 0.0077(2) O1 0.061(2) 0.0498(17) 0.070(3) 0.0097(16) 0.0053(17) 0.0110(14) O2 0.071(2) 0.0484(17) 0.067(3) 0.0093(16) 0.0074(18) 0.0053(14) O3 0.097(2) 0.063(2) 0.052(2) 0.0241(15) 0.0377(18) 0.0459(16) O4 0.085(2) 0.0554(18) 0.049(2) 0.0158(14) 0.0306(16) 0.0344(16) N1 0.056(2) 0.0425(19) 0.059(3) -0.0015(17) 0.0153(19) 0.0101(16) N2 0.070(3) 0.044(2) 0.049(3) 0.0136(17) 0.006(2) -0.0011(17) N3 0.071(3) 0.049(2) 0.059(3) 0.0035(19) 0.024(2) -0.0006(18) N4 0.075(3) 0.052(2) 0.057(3) 0.0074(19) 0.024(2) 0.0025(18) N5 0.065(2) 0.0468(19) 0.042(3) 0.0024(16) 0.021(2) 0.0034(16) N6 0.058(2) 0.051(2) 0.045(3) 0.0057(16) 0.0204(19) 0.0104(16) N7 0.055(2) 0.055(2) 0.047(3) 0.0114(18) 0.0058(18) 0.0042(18) N8 0.056(2) 0.059(2) 0.044(3) 0.0106(18) 0.0065(19) 0.0172(17) N9 0.065(3) 0.077(3) 0.042(3) 0.009(2) 0.009(2) -0.003(2) N10 0.050(2) 0.072(3) 0.055(3) 0.016(2) 0.009(2) 0.0047(19) N11 0.064(3) 0.049(2) 0.045(3) 0.0022(17) 0.0170(19) 0.0138(18) N12 0.059(2) 0.057(2) 0.045(3) 0.0015(17) 0.0224(19) 0.0121(18) N13 0.060(2) 0.044(2) 0.052(3) 0.0052(17) 0.0133(18) 0.0046(16) N14 0.066(2) 0.047(2) 0.051(3) 0.0177(18) 0.0213(18) 0.0131(17) C1 0.055(3) 0.048(3) 0.066(4) 0.000(2) 0.021(2) 0.008(2) C2 0.043(3) 0.045(3) 0.076(4) 0.007(2) 0.010(3) 0.0074(19) C3 0.039(3) 0.048(3) 0.078(4) -0.001(2) 0.014(2) 0.0071(19) C4 0.062(3) 0.046(3) 0.099(5) -0.007(3) 0.031(3) 0.009(2) C5 0.069(3) 0.058(3) 0.077(4) 0.002(3) 0.035(3) 0.013(2) C6 0.076(3) 0.055(3) 0.075(4) 0.002(2) 0.028(3) 0.014(2) C7 0.048(3) 0.046(2) 0.092(4) 0.000(3) 0.014(2) 0.008(2) C8 0.064(3) 0.060(3) 0.117(5) 0.000(3) 0.011(3) 0.013(2) C9 0.069(3) 0.057(3) 0.107(5) 0.012(3) 0.023(3) 0.006(2) C10 0.075(4) 0.055(3) 0.126(5) 0.000(3) 0.028(3) 0.020(2) C11 0.108(5) 0.064(3) 0.100(5) 0.001(3) 0.056(4) 0.019(3) C12 0.124(5) 0.078(4) 0.099(5) -0.021(3) 0.043(4) 0.005(3) C13 0.142(6) 0.096(4) 0.132(7) -0.004(4) 0.090(5) 0.010(4) C14 0.167(6) 0.090(4) 0.084(5) 0.003(3) 0.063(4) 0.022(4) C15 0.061(3) 0.043(2) 0.063(4) 0.008(2) 0.014(2) 0.012(2) C16 0.065(3) 0.043(2) 0.050(3) 0.012(2) 0.002(2) -0.009(2) C17 0.058(3) 0.044(2) 0.056(4) 0.014(2) 0.004(2) -0.007(2) C18 0.050(3) 0.053(3) 0.069(4) 0.025(2) 0.005(2) -0.008(2) C19 0.055(3) 0.072(3) 0.068(4) 0.027(3) -0.002(3) -0.005(2) C20 0.067(3) 0.064(3) 0.050(4) 0.013(2) -0.001(3) -0.021(3) C21 0.073(3) 0.052(3) 0.059(4) 0.011(2) 0.003(3) -0.009(2) C22 0.058(3) 0.086(4) 0.076(4) 0.043(3) 0.015(3) 0.019(3) C23 0.143(6) 0.186(7) 0.097(6) 0.086(5) 0.047(5) 0.100(5) C24 0.120(5) 0.060(4) 0.150(6) 0.030(4) 0.060(5) 0.016(3) C25 0.071(4) 0.146(5) 0.088(5) 0.025(4) 0.023(3) -0.005(4) C26 0.085(4) 0.073(3) 0.061(4) 0.017(3) 0.004(3) -0.016(3) C27 0.127(5) 0.097(4) 0.076(5) 0.016(3) 0.033(4) -0.015(4) C28 0.101(5) 0.151(6) 0.073(5) -0.010(4) -0.009(4) -0.048(4) C29 0.127(5) 0.094(4) 0.061(4) -0.002(3) 0.015(3) -0.012(4) C30 0.070(3) 0.040(2) 0.057(4) 0.008(2) 0.012(3) -0.001(2) C31 0.054(3) 0.040(2) 0.046(3) 0.0049(19) 0.010(2) 0.0105(19) C32 0.067(3) 0.042(2) 0.049(3) 0.013(2) 0.011(2) 0.012(2) C33 0.107(4) 0.058(3) 0.049(3) 0.018(2) 0.028(3) 0.032(3) C34 0.103(4) 0.053(3) 0.061(4) 0.018(2) 0.031(3) 0.037(3) C35 0.073(3) 0.050(3) 0.042(3) 0.008(2) 0.020(2) 0.022(2) C36 0.067(3) 0.049(2) 0.042(3) 0.008(2) 0.015(2) 0.014(2) C37 0.072(3) 0.050(3) 0.050(4) 0.010(2) 0.023(3) 0.021(2) C38 0.089(4) 0.054(3) 0.078(4) 0.017(3) 0.030(3) 0.000(3) C39 0.106(4) 0.051(3) 0.104(5) 0.014(3) 0.042(4) -0.003(3) C40 0.115(5) 0.054(3) 0.082(5) 0.000(3) 0.046(4) -0.004(3) C41 0.136(5) 0.083(4) 0.095(5) 0.032(3) 0.054(4) 0.001(3) C42 0.223(8) 0.065(4) 0.129(7) -0.024(4) 0.089(6) -0.025(4) C43 0.058(3) 0.064(3) 0.051(3) 0.009(2) 0.026(2) 0.014(2) C44 0.076(4) 0.064(3) 0.069(4) 0.010(2) 0.041(3) 0.010(3) C45 0.084(4) 0.057(3) 0.045(3) 0.001(2) 0.032(3) 0.005(2) C46 0.059(3) 0.111(4) 0.062(4) 0.007(3) 0.018(3) -0.005(3) C47 0.132(5) 0.079(4) 0.074(4) -0.018(3) 0.056(3) -0.024(3) C48 0.057(3) 0.067(3) 0.055(4) 0.022(2) 0.012(2) 0.020(2) C49 0.062(3) 0.076(3) 0.070(4) 0.025(3) -0.003(3) 0.020(3) C50 0.066(3) 0.069(3) 0.049(3) 0.014(2) 0.001(2) -0.002(2) C51 0.084(4) 0.081(3) 0.074(4) 0.012(3) 0.021(3) 0.039(3) C52 0.108(4) 0.098(4) 0.066(4) 0.009(3) -0.013(3) 0.007(3) C53 0.041(3) 0.097(4) 0.069(4) 0.040(3) 0.003(3) 0.007(3) C54 0.061(4) 0.137(5) 0.064(5) 0.034(4) -0.015(3) -0.006(4) C55 0.078(4) 0.114(5) 0.057(4) 0.015(3) -0.010(3) -0.001(4) C56 0.062(3) 0.121(5) 0.124(6) 0.052(4) 0.021(3) 0.031(3) C57 0.162(7) 0.149(6) 0.078(5) -0.038(5) -0.028(5) 0.004(5) C58 0.064(3) 0.063(3) 0.070(4) 0.004(2) 0.035(3) 0.011(2) C59 0.070(3) 0.076(3) 0.075(4) 0.003(3) 0.041(3) 0.018(3) C60 0.076(3) 0.062(3) 0.054(4) 0.003(2) 0.029(3) 0.024(3) C61 0.071(3) 0.093(4) 0.141(6) -0.016(4) 0.057(3) -0.010(3) C62 0.125(5) 0.072(3) 0.090(5) -0.015(3) 0.053(4) 0.019(3) C63 0.067(3) 0.052(3) 0.052(4) 0.018(2) 0.021(2) 0.013(2) C64 0.081(4) 0.054(3) 0.062(4) 0.021(2) 0.021(3) 0.003(2) C65 0.070(3) 0.052(3) 0.053(4) 0.014(2) 0.014(3) 0.001(2) C66 0.121(5) 0.065(3) 0.065(4) 0.026(3) 0.046(3) 0.030(3) C67 0.133(5) 0.056(3) 0.072(4) 0.004(3) 0.020(3) -0.007(3) B1 0.072(4) 0.054(3) 0.036(3) -0.002(2) 0.015(2) 0.000(3) B2 0.071(4) 0.051(3) 0.038(4) 0.001(2) 0.010(3) 0.000(3) C68 0.43(2) 0.177(12) 0.193(13) 0.043(9) 0.154(16) 0.119(14) C69 0.40(3) 0.207(16) 0.49(4) 0.22(2) 0.34(3) 0.139(17) C70 0.308(19) 0.175(12) 0.41(3) -0.071(13) 0.150(19) -0.018(12) C71 0.30(2) 0.24(2) 0.93(7) -0.12(3) -0.21(3) 0.074(18) C72 0.62(4) 0.180(13) 0.194(15) -0.050(11) 0.002(18) -0.074(18) C73 0.55(4) 0.50(3) 0.222(19) -0.03(2) 0.11(2) -0.34(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 La1 O4 2.487(3) . ? La1 O3 2.518(2) . ? La1 N12 2.589(3) . ? La1 N6 2.611(3) . ? La1 N8 2.638(3) . ? La1 N14 2.690(3) . ? La1 N10 2.747(4) . ? La1 N4 2.756(4) . ? La1 C37 2.840(4) . ? Cu1 O2 1.880(3) . ? Cu1 O1 1.888(3) . ? Cu1 N2 1.924(4) . ? Cu1 N1 1.932(4) . ? O1 C2 1.301(5) . ? O2 C17 1.292(5) . ? O3 C37 1.255(5) . ? O4 C37 1.264(5) . ? N1 C15 1.296(5) . ? N1 C31 1.420(5) . ? N2 C30 1.291(5) . ? N2 C32 1.413(5) . ? N3 C40 1.355(6) . ? N3 N4 1.373(5) . ? N3 B1 1.543(6) . ? N4 C38 1.335(5) . ? N5 C45 1.351(5) . ? N5 N6 1.371(4) . ? N5 B1 1.548(6) . ? N6 C43 1.334(5) . ? N7 C50 1.353(5) . ? N7 N8 1.384(5) . ? N7 B1 1.535(6) . ? N8 C48 1.346(5) . ? N9 C55 1.341(6) . ? N9 N10 1.389(5) . ? N9 B2 1.534(6) . ? N10 C53 1.338(5) . ? N11 C60 1.356(5) . ? N11 N12 1.375(4) . ? N11 B2 1.531(6) . ? N12 C58 1.336(5) . ? N13 C65 1.350(5) . ? N13 N14 1.380(5) . ? N13 B2 1.546(6) . ? N14 C63 1.347(5) . ? C1 C6 1.405(6) . ? C1 C15 1.417(6) . ? C1 C2 1.426(6) . ? C2 C3 1.449(6) . ? C3 C4 1.353(6) . ? C3 C7 1.532(6) . ? C4 C5 1.437(7) . ? C5 C6 1.366(6) . ? C5 C11 1.531(7) . ? C7 C8 1.522(6) . ? C7 C10 1.529(6) . ? C7 C9 1.536(6) . ? C11 C13 1.522(7) . ? C11 C14 1.529(7) . ? C11 C12 1.538(7) . ? C16 C21 1.408(6) . ? C16 C30 1.415(6) . ? C16 C17 1.427(6) . ? C17 C18 1.442(6) . ? C18 C19 1.369(7) . ? C18 C22 1.532(7) . ? C19 C20 1.424(7) . ? C20 C21 1.374(6) . ? C20 C26 1.509(7) . ? C22 C23 1.525(7) . ? C22 C25 1.532(7) . ? C22 C24 1.535(7) . ? C26 C29 1.536(7) . ? C26 C28 1.543(7) . ? C26 C27 1.543(7) . ? C31 C32 1.393(6) . ? C31 C36 1.394(5) . ? C32 C33 1.396(6) . ? C33 C34 1.377(6) . ? C34 C35 1.380(6) . ? C35 C36 1.380(5) . ? C35 C37 1.510(6) . ? C38 C39 1.370(7) . ? C38 C41 1.507(7) . ? C39 C40 1.366(7) . ? C40 C42 1.505(8) . ? C43 C44 1.389(6) . ? C43 C46 1.491(6) . ? C44 C45 1.369(6) . ? C45 C47 1.485(6) . ? C48 C49 1.385(6) . ? C48 C51 1.490(6) . ? C49 C50 1.371(6) . ? C50 C52 1.497(7) . ? C53 C54 1.377(8) . ? C53 C56 1.501(7) . ? C54 C55 1.355(7) . ? C55 C57 1.507(8) . ? C58 C59 1.395(6) . ? C58 C61 1.489(7) . ? C59 C60 1.351(6) . ? C60 C62 1.499(6) . ? C63 C64 1.392(6) . ? C63 C66 1.475(6) . ? C64 C65 1.361(6) . ? C65 C67 1.498(6) . ? C68 C69 1.563(15) . ? C69 C70 1.430(14) . ? C70 C71 1.494(14) . ? C71 C72 1.452(15) . ? C72 C73 1.427(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 La1 O3 52.60(9) . . ? O4 La1 N12 75.52(10) . . ? O3 La1 N12 127.54(11) . . ? O4 La1 N6 128.62(9) . . ? O3 La1 N6 76.57(10) . . ? N12 La1 N6 155.82(10) . . ? O4 La1 N8 133.82(10) . . ? O3 La1 N8 132.95(11) . . ? N12 La1 N8 87.03(11) . . ? N6 La1 N8 74.55(11) . . ? O4 La1 N14 134.88(10) . . ? O3 La1 N14 137.41(10) . . ? N12 La1 N14 73.89(11) . . ? N6 La1 N14 86.44(10) . . ? N8 La1 N14 76.44(11) . . ? O4 La1 N10 73.45(10) . . ? O3 La1 N10 81.37(11) . . ? N12 La1 N10 76.54(12) . . ? N6 La1 N10 109.25(12) . . ? N8 La1 N10 143.45(11) . . ? N14 La1 N10 67.74(11) . . ? O4 La1 N4 77.36(11) . . ? O3 La1 N4 71.22(10) . . ? N12 La1 N4 107.78(12) . . ? N6 La1 N4 79.95(12) . . ? N8 La1 N4 67.76(11) . . ? N14 La1 N4 143.91(11) . . ? N10 La1 N4 148.34(11) . . ? O4 La1 C37 26.39(11) . . ? O3 La1 C37 26.23(10) . . ? N12 La1 C37 101.55(13) . . ? N6 La1 C37 102.63(12) . . ? N8 La1 C37 140.66(12) . . ? N14 La1 C37 142.89(12) . . ? N10 La1 C37 75.33(12) . . ? N4 La1 C37 73.08(12) . . ? O2 Cu1 O1 90.49(14) . . ? O2 Cu1 N2 92.85(15) . . ? O1 Cu1 N2 173.63(14) . . ? O2 Cu1 N1 173.21(13) . . ? O1 Cu1 N1 93.19(15) . . ? N2 Cu1 N1 84.04(16) . . ? C2 O1 Cu1 129.3(3) . . ? C17 O2 Cu1 129.6(3) . . ? C37 O3 La1 91.4(2) . . ? C37 O4 La1 92.6(3) . . ? C15 N1 C31 122.0(4) . . ? C15 N1 Cu1 124.7(3) . . ? C31 N1 Cu1 113.1(3) . . ? C30 N2 C32 121.4(4) . . ? C30 N2 Cu1 125.3(3) . . ? C32 N2 Cu1 113.2(3) . . ? C40 N3 N4 109.5(4) . . ? C40 N3 B1 126.3(4) . . ? N4 N3 B1 123.9(4) . . ? C38 N4 N3 105.7(4) . . ? C38 N4 La1 134.4(4) . . ? N3 N4 La1 112.3(3) . . ? C45 N5 N6 109.9(4) . . ? C45 N5 B1 129.3(4) . . ? N6 N5 B1 120.8(4) . . ? C43 N6 N5 106.6(4) . . ? C43 N6 La1 131.3(3) . . ? N5 N6 La1 122.1(3) . . ? C50 N7 N8 109.5(4) . . ? C50 N7 B1 127.7(4) . . ? N8 N7 B1 122.8(3) . . ? C48 N8 N7 106.0(3) . . ? C48 N8 La1 134.4(3) . . ? N7 N8 La1 119.6(2) . . ? C55 N9 N10 110.2(4) . . ? C55 N9 B2 126.9(5) . . ? N10 N9 B2 122.7(4) . . ? C53 N10 N9 104.7(4) . . ? C53 N10 La1 135.7(4) . . ? N9 N10 La1 117.7(2) . . ? C60 N11 N12 109.2(4) . . ? C60 N11 B2 129.8(4) . . ? N12 N11 B2 121.0(4) . . ? C58 N12 N11 106.5(3) . . ? C58 N12 La1 129.2(3) . . ? N11 N12 La1 124.3(3) . . ? C65 N13 N14 110.1(4) . . ? C65 N13 B2 127.8(4) . . ? N14 N13 B2 122.1(3) . . ? C63 N14 N13 106.0(3) . . ? C63 N14 La1 133.1(3) . . ? N13 N14 La1 120.6(2) . . ? C6 C1 C15 117.5(4) . . ? C6 C1 C2 120.5(4) . . ? C15 C1 C2 122.0(5) . . ? O1 C2 C1 123.3(4) . . ? O1 C2 C3 119.6(4) . . ? C1 C2 C3 117.1(5) . . ? C4 C3 C2 118.2(4) . . ? C4 C3 C7 121.6(4) . . ? C2 C3 C7 120.1(5) . . ? C3 C4 C5 126.1(4) . . ? C6 C5 C4 114.2(5) . . ? C6 C5 C11 126.0(5) . . ? C4 C5 C11 119.7(4) . . ? C5 C6 C1 123.8(5) . . ? C8 C7 C10 107.7(4) . . ? C8 C7 C3 109.6(4) . . ? C10 C7 C3 111.8(4) . . ? C8 C7 C9 109.9(4) . . ? C10 C7 C9 107.1(4) . . ? C3 C7 C9 110.7(3) . . ? C13 C11 C14 107.7(5) . . ? C13 C11 C5 109.5(5) . . ? C14 C11 C5 111.1(4) . . ? C13 C11 C12 109.8(4) . . ? C14 C11 C12 108.9(5) . . ? C5 C11 C12 109.8(4) . . ? N1 C15 C1 127.5(4) . . ? C21 C16 C30 116.8(4) . . ? C21 C16 C17 121.5(4) . . ? C30 C16 C17 121.6(5) . . ? O2 C17 C16 123.4(4) . . ? O2 C17 C18 120.0(4) . . ? C16 C17 C18 116.7(5) . . ? C19 C18 C17 118.2(5) . . ? C19 C18 C22 121.9(4) . . ? C17 C18 C22 119.8(5) . . ? C18 C19 C20 126.2(5) . . ? C21 C20 C19 114.7(5) . . ? C21 C20 C26 124.2(5) . . ? C19 C20 C26 121.1(5) . . ? C20 C21 C16 122.6(5) . . ? C23 C22 C25 107.6(4) . . ? C23 C22 C18 112.5(5) . . ? C25 C22 C18 110.0(4) . . ? C23 C22 C24 108.4(5) . . ? C25 C22 C24 108.8(5) . . ? C18 C22 C24 109.4(4) . . ? C20 C26 C29 112.8(4) . . ? C20 C26 C28 110.8(5) . . ? C29 C26 C28 106.7(5) . . ? C20 C26 C27 110.2(4) . . ? C29 C26 C27 107.2(5) . . ? C28 C26 C27 109.0(5) . . ? N2 C30 C16 127.1(5) . . ? C32 C31 C36 120.0(4) . . ? C32 C31 N1 114.2(4) . . ? C36 C31 N1 125.8(4) . . ? C31 C32 C33 119.5(4) . . ? C31 C32 N2 115.3(4) . . ? C33 C32 N2 125.2(5) . . ? C34 C33 C32 119.6(5) . . ? C33 C34 C35 120.8(4) . . ? C34 C35 C36 120.1(4) . . ? C34 C35 C37 119.5(4) . . ? C36 C35 C37 120.4(4) . . ? C35 C36 C31 119.7(4) . . ? O3 C37 O4 123.4(4) . . ? O3 C37 C35 119.3(4) . . ? O4 C37 C35 117.3(4) . . ? O3 C37 La1 62.4(2) . . ? O4 C37 La1 61.0(2) . . ? C35 C37 La1 175.4(3) . . ? N4 C38 C39 111.1(5) . . ? N4 C38 C41 123.9(5) . . ? C39 C38 C41 124.9(5) . . ? C40 C39 C38 105.9(5) . . ? N3 C40 C39 107.8(5) . . ? N3 C40 C42 123.4(5) . . ? C39 C40 C42 128.8(5) . . ? N6 C43 C44 109.6(4) . . ? N6 C43 C46 120.9(4) . . ? C44 C43 C46 129.5(4) . . ? C45 C44 C43 106.6(4) . . ? N5 C45 C44 107.3(4) . . ? N5 C45 C47 124.5(5) . . ? C44 C45 C47 128.2(5) . . ? N8 C48 C49 110.2(4) . . ? N8 C48 C51 122.8(4) . . ? C49 C48 C51 127.0(4) . . ? C50 C49 C48 106.3(4) . . ? N7 C50 C49 108.1(4) . . ? N7 C50 C52 123.3(5) . . ? C49 C50 C52 128.6(4) . . ? N10 C53 C54 110.6(5) . . ? N10 C53 C56 122.7(6) . . ? C54 C53 C56 126.7(5) . . ? C55 C54 C53 106.7(5) . . ? N9 C55 C54 107.7(6) . . ? N9 C55 C57 124.2(6) . . ? C54 C55 C57 128.1(6) . . ? N12 C58 C59 109.6(4) . . ? N12 C58 C61 120.5(4) . . ? C59 C58 C61 129.9(5) . . ? C60 C59 C58 106.5(4) . . ? C59 C60 N11 108.3(4) . . ? C59 C60 C62 129.3(5) . . ? N11 C60 C62 122.4(5) . . ? N14 C63 C64 109.2(4) . . ? N14 C63 C66 123.2(4) . . ? C64 C63 C66 127.6(4) . . ? C65 C64 C63 107.2(4) . . ? N13 C65 C64 107.5(4) . . ? N13 C65 C67 123.9(5) . . ? C64 C65 C67 128.6(4) . . ? N7 B1 N3 111.4(4) . . ? N7 B1 N5 112.1(4) . . ? N3 B1 N5 111.5(4) . . ? N11 B2 N9 113.2(4) . . ? N11 B2 N13 111.8(4) . . ? N9 B2 N13 110.7(4) . . ? C70 C69 C68 100.5(13) . . ? C69 C70 C71 107.6(12) . . ? C72 C71 C70 102.3(12) . . ? C73 C72 C71 115.5(13) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.515 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.059 data_c2002fin _database_code_depnum_ccdc_archive 'CCDC 736173' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H103 B2 La N14 Ni O4' _chemical_formula_weight 1411.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.654(4) _cell_length_b 17.236(4) _cell_length_c 23.787(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.492(4) _cell_angle_gamma 90.00 _cell_volume 7192(3) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 1016 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 25.22 _exptl_crystal_description prism _exptl_crystal_colour 'bright red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2968 _exptl_absorpt_coefficient_mu 0.904 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75513 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.30 _reflns_number_total 17722 _reflns_number_gt 12600 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+7.4911P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17722 _refine_ls_number_parameters 875 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1093 _refine_ls_R_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.1362 _refine_ls_wR_factor_gt 0.1235 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.025 _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 La1 La 0.234648(13) 0.196328(13) 0.947838(10) 0.02672(7) Uani 1 1 d . . . Ni1 Ni 0.06124(3) 0.42712(3) 1.06688(2) 0.02540(12) Uani 1 1 d . . . O1 O 0.09746(16) 0.47595(17) 1.13424(12) 0.0327(7) Uani 1 1 d . . . O2 O -0.01304(15) 0.38316(16) 1.10601(11) 0.0292(6) Uani 1 1 d . . . O3 O 0.09704(16) 0.25405(17) 0.95202(13) 0.0342(7) Uani 1 1 d . . . O4 O 0.18932(18) 0.33384(17) 0.93540(16) 0.0468(9) Uani 1 1 d . . . N1 N 0.13361(18) 0.47196(19) 1.02723(14) 0.0267(7) Uani 1 1 d . . . N2 N 0.02271(18) 0.38262(18) 0.99875(14) 0.0258(7) Uani 1 1 d . . . N3 N 0.2813(2) 0.2859(2) 1.07875(16) 0.0386(9) Uani 1 1 d . . . N4 N 0.2215(2) 0.2425(2) 1.05291(16) 0.0356(9) Uani 1 1 d . . . N5 N 0.3660(2) 0.3290(2) 1.00240(18) 0.0405(9) Uani 1 1 d . . . N6 N 0.3420(2) 0.2972(2) 0.95101(17) 0.0404(9) Uani 1 1 d . . . N7 N 0.3901(2) 0.2023(2) 1.05489(15) 0.0361(8) Uani 1 1 d . . . N8 N 0.3528(2) 0.1472(2) 1.02008(16) 0.0361(9) Uani 1 1 d . . . N9 N 0.1632(2) 0.1039(2) 0.81790(16) 0.0400(9) Uani 1 1 d . . . N10 N 0.1623(2) 0.1759(2) 0.84233(15) 0.0364(9) Uani 1 1 d . . . N11 N 0.1741(2) 0.0110(2) 0.90273(17) 0.0397(9) Uani 1 1 d . . . N12 N 0.1914(2) 0.0525(2) 0.95219(16) 0.0376(9) Uani 1 1 d . . . N13 N 0.2909(2) 0.0500(2) 0.85625(15) 0.0366(9) Uani 1 1 d . . . N14 N 0.3231(2) 0.1144(2) 0.88432(16) 0.0375(9) Uani 1 1 d . . . C1 C 0.2124(2) 0.5300(2) 1.10586(19) 0.0348(10) Uani 1 1 d . . . C2 C 0.1625(2) 0.5121(2) 1.14677(19) 0.0348(10) Uani 1 1 d . . . C3 C 0.1850(3) 0.5375(3) 1.20409(19) 0.0383(11) Uani 1 1 d . . . C4 C 0.2546(3) 0.5737(3) 1.2151(2) 0.0455(12) Uani 1 1 d . . . C5 C 0.3052(3) 0.5903(3) 1.1753(2) 0.0462(12) Uani 1 1 d . . . C6 C 0.2823(3) 0.5687(3) 1.1210(2) 0.0417(11) Uani 1 1 d . . . C7 C 0.1334(3) 0.5250(3) 1.2505(2) 0.0452(12) Uani 1 1 d . . . C8 C 0.1162(3) 0.4387(3) 1.2566(2) 0.0580(15) Uani 1 1 d . . . H8A H 0.0921 0.4188 1.2208 0.087 Uiso 1 1 calc R . . H8B H 0.0822 0.4318 1.2855 0.087 Uiso 1 1 calc R . . H8C H 0.1633 0.4108 1.2673 0.087 Uiso 1 1 calc R . . C9 C 0.0592(3) 0.5698(3) 1.2352(2) 0.0569(15) Uani 1 1 d . . . H9A H 0.0704 0.6247 1.2324 0.085 Uiso 1 1 calc R . . H9B H 0.0257 0.5618 1.2644 0.085 Uiso 1 1 calc R . . H9C H 0.0344 0.5515 1.1992 0.085 Uiso 1 1 calc R . . C10 C 0.1693(3) 0.5548(4) 1.3082(2) 0.0714(19) Uani 1 1 d . . . H10A H 0.2163 0.5269 1.3194 0.107 Uiso 1 1 calc R . . H10B H 0.1341 0.5464 1.3362 0.107 Uiso 1 1 calc R . . H10C H 0.1800 0.6098 1.3056 0.107 Uiso 1 1 calc R . . C11 C 0.3816(3) 0.6302(4) 1.1941(3) 0.0614(16) Uani 1 1 d . . . C12 C 0.4324(4) 0.6346(5) 1.1475(3) 0.093(3) Uani 1 1 d . . . H12A H 0.4773 0.6651 1.1601 0.140 Uiso 1 1 calc R . . H12B H 0.4049 0.6588 1.1145 0.140 Uiso 1 1 calc R . . H12C H 0.4478 0.5827 1.1379 0.140 Uiso 1 1 calc R . . C13 C 0.4212(4) 0.5921(6) 1.2445(4) 0.139(4) Uani 1 1 d . . . H13A H 0.4279 0.5375 1.2367 0.208 Uiso 1 1 calc R . . H13B H 0.3912 0.5977 1.2760 0.208 Uiso 1 1 calc R . . H13C H 0.4707 0.6161 1.2541 0.208 Uiso 1 1 calc R . . C14 C 0.3648(5) 0.7166(5) 1.2092(4) 0.111(3) Uani 1 1 d . . . H14A H 0.3363 0.7179 1.2418 0.166 Uiso 1 1 calc R . . H14B H 0.3352 0.7412 1.1773 0.166 Uiso 1 1 calc R . . H14C H 0.4126 0.7442 1.2180 0.166 Uiso 1 1 calc R . . C15 C 0.1921(3) 0.5106(3) 1.0476(2) 0.0349(10) Uani 1 1 d . . . C16 C -0.0944(2) 0.3305(2) 1.02778(18) 0.0275(9) Uani 1 1 d . . . C17 C -0.0777(2) 0.3510(2) 1.08557(17) 0.0273(9) Uani 1 1 d . . . C18 C -0.1356(2) 0.3360(2) 1.12219(18) 0.0313(9) Uani 1 1 d . . . C19 C -0.2035(3) 0.3047(3) 1.0983(2) 0.0351(10) Uani 1 1 d . . . C20 C -0.2208(2) 0.2834(2) 1.04111(19) 0.0335(10) Uani 1 1 d . . . C21 C -0.1651(2) 0.2970(3) 1.0071(2) 0.0339(10) Uani 1 1 d . . . C22 C -0.1217(3) 0.3574(3) 1.18518(19) 0.0388(11) Uani 1 1 d . . . C23 C -0.0536(3) 0.3126(3) 1.2138(2) 0.0541(14) Uani 1 1 d . . . H23A H -0.0640 0.2574 1.2111 0.081 Uiso 1 1 calc R . . H23B H -0.0445 0.3275 1.2533 0.081 Uiso 1 1 calc R . . H23C H -0.0088 0.3243 1.1952 0.081 Uiso 1 1 calc R . . C24 C -0.1078(3) 0.4451(3) 1.1904(2) 0.0507(13) Uani 1 1 d . . . H24A H -0.0640 0.4590 1.1713 0.076 Uiso 1 1 calc R . . H24B H -0.0983 0.4592 1.2301 0.076 Uiso 1 1 calc R . . H24C H -0.1524 0.4727 1.1731 0.076 Uiso 1 1 calc R . . C25 C -0.1908(3) 0.3377(4) 1.2169(2) 0.0613(16) Uani 1 1 d . . . H25A H -0.2354 0.3653 1.1996 0.092 Uiso 1 1 calc R . . H25B H -0.1801 0.3532 1.2562 0.092 Uiso 1 1 calc R . . H25C H -0.2003 0.2823 1.2148 0.092 Uiso 1 1 calc R . . C26 C -0.2997(3) 0.2505(3) 1.0204(2) 0.0419(11) Uani 1 1 d . . . C27 C -0.3021(3) 0.2194(4) 0.9602(2) 0.0593(15) Uani 1 1 d . . . H27A H -0.2912 0.2612 0.9350 0.089 Uiso 1 1 calc R . . H27B H -0.3524 0.1986 0.9483 0.089 Uiso 1 1 calc R . . H27C H -0.2643 0.1788 0.9591 0.089 Uiso 1 1 calc R . . C28 C -0.3193(3) 0.1833(3) 1.0586(2) 0.0542(14) Uani 1 1 d . . . H28A H -0.2820 0.1421 1.0573 0.081 Uiso 1 1 calc R . . H28B H -0.3696 0.1635 1.0455 0.081 Uiso 1 1 calc R . . H28C H -0.3185 0.2017 1.0972 0.081 Uiso 1 1 calc R . . C29 C -0.3590(3) 0.3144(3) 1.0229(3) 0.0559(14) Uani 1 1 d . . . H29A H -0.3592 0.3316 1.0617 0.084 Uiso 1 1 calc R . . H29B H -0.4090 0.2945 1.0089 0.084 Uiso 1 1 calc R . . H29C H -0.3466 0.3578 0.9996 0.084 Uiso 1 1 calc R . . C30 C -0.0415(2) 0.3465(2) 0.9882(2) 0.0311(9) Uani 1 1 d . . . C31 C 0.1163(3) 0.4653(3) 0.96538(19) 0.0318(10) Uani 1 1 d . . . C32 C 0.0714(2) 0.3919(2) 0.95308(18) 0.0277(9) Uani 1 1 d . . . C33 C 0.1230(2) 0.3209(2) 0.94768(18) 0.0313(10) Uani 1 1 d . . . C34 C 0.2603(3) 0.3170(3) 1.1275(2) 0.0465(12) Uani 1 1 d . . . C35 C 0.1878(3) 0.2938(3) 1.1320(2) 0.0536(15) Uani 1 1 d . . . C36 C 0.1654(3) 0.2477(3) 1.0857(2) 0.0429(12) Uani 1 1 d . . . C37 C 0.3129(4) 0.3653(4) 1.1677(2) 0.0684(17) Uani 1 1 d . . . H37A H 0.3316 0.4089 1.1474 0.103 Uiso 1 1 calc R . . H37B H 0.3556 0.3339 1.1835 0.103 Uiso 1 1 calc R . . H37C H 0.2854 0.3844 1.1979 0.103 Uiso 1 1 calc R . . C38 C 0.0898(3) 0.2067(3) 1.0737(2) 0.0553(14) Uani 1 1 d . . . H38A H 0.0881 0.1792 1.0380 0.083 Uiso 1 1 calc R . . H38B H 0.0489 0.2445 1.0716 0.083 Uiso 1 1 calc R . . H38C H 0.0839 0.1700 1.1038 0.083 Uiso 1 1 calc R . . C39 C 0.3934(3) 0.4008(3) 0.9942(3) 0.0556(14) Uani 1 1 d . . . C40 C 0.3869(3) 0.4150(3) 0.9372(3) 0.0663(17) Uani 1 1 d . . . H40 H 0.4013 0.4604 0.9193 0.080 Uiso 1 1 calc R . . C41 C 0.3547(3) 0.3488(3) 0.9113(2) 0.0506(13) Uani 1 1 d . . . C42 C 0.4252(4) 0.4522(4) 1.0419(3) 0.090(2) Uani 1 1 d . . . H42A H 0.3897 0.4546 1.0702 0.135 Uiso 1 1 calc R . . H42B H 0.4329 0.5040 1.0275 0.135 Uiso 1 1 calc R . . H42C H 0.4735 0.4315 1.0589 0.135 Uiso 1 1 calc R . . C43 C 0.3329(4) 0.3321(4) 0.8499(3) 0.0711(18) Uani 1 1 d . . . H43A H 0.3144 0.2792 0.8455 0.107 Uiso 1 1 calc R . . H43B H 0.3770 0.3387 0.8295 0.107 Uiso 1 1 calc R . . H43C H 0.2930 0.3677 0.8349 0.107 Uiso 1 1 calc R . . C44 C 0.4517(3) 0.1705(3) 1.0845(2) 0.0422(12) Uani 1 1 d . . . C45 C 0.4559(3) 0.0945(3) 1.0686(2) 0.0453(12) Uani 1 1 d . . . C46 C 0.3932(3) 0.0814(3) 1.02894(19) 0.0382(11) Uani 1 1 d . . . C47 C 0.5027(3) 0.2140(4) 1.1286(2) 0.0599(16) Uani 1 1 d . . . H47A H 0.5245 0.2585 1.1113 0.090 Uiso 1 1 calc R . . H47B H 0.5432 0.1801 1.1448 0.090 Uiso 1 1 calc R . . H47C H 0.4731 0.2316 1.1582 0.090 Uiso 1 1 calc R . . C48 C 0.3711(3) 0.0068(3) 1.0004(2) 0.0484(13) Uani 1 1 d . . . H48A H 0.3377 0.0170 0.9659 0.073 Uiso 1 1 calc R . . H48B H 0.3446 -0.0252 1.0254 0.073 Uiso 1 1 calc R . . H48C H 0.4164 -0.0200 0.9913 0.073 Uiso 1 1 calc R . . C49 C 0.1263(3) 0.1063(4) 0.7649(2) 0.0564(15) Uani 1 1 d . . . C50 C 0.1009(3) 0.1793(4) 0.7550(2) 0.0642(17) Uani 1 1 d . . . H50 H 0.0730 0.1977 0.7217 0.077 Uiso 1 1 calc R . . C51 C 0.1237(3) 0.2222(3) 0.8033(2) 0.0478(13) Uani 1 1 d . . . C52 C 0.1176(4) 0.0367(4) 0.7254(3) 0.093(2) Uani 1 1 d . . . H52A H 0.1674 0.0207 0.7162 0.139 Uiso 1 1 calc R . . H52B H 0.0858 0.0508 0.6910 0.139 Uiso 1 1 calc R . . H52C H 0.0940 -0.0057 0.7438 0.139 Uiso 1 1 calc R . . C53 C 0.1075(4) 0.3054(4) 0.8130(2) 0.074(2) Uani 1 1 d . . . H53A H 0.0662 0.3098 0.8365 0.111 Uiso 1 1 calc R . . H53B H 0.0929 0.3307 0.7769 0.111 Uiso 1 1 calc R . . H53C H 0.1528 0.3302 0.8318 0.111 Uiso 1 1 calc R . . C54 C 0.1399(3) -0.0566(3) 0.9146(2) 0.0505(13) Uani 1 1 d . . . C55 C 0.1361(4) -0.0586(3) 0.9715(3) 0.0576(16) Uani 1 1 d . . . C56 C 0.1688(3) 0.0095(3) 0.9940(2) 0.0462(12) Uani 1 1 d . . . C57 C 0.1123(4) -0.1158(3) 0.8710(3) 0.0737(19) Uani 1 1 d . . . H57A H 0.1551 -0.1356 0.8532 0.111 Uiso 1 1 calc R . . H57B H 0.0758 -0.0920 0.8426 0.111 Uiso 1 1 calc R . . H57C H 0.0879 -0.1581 0.8890 0.111 Uiso 1 1 calc R . . C58 C 0.1850(4) 0.0335(3) 1.0543(2) 0.0645(17) Uani 1 1 d . . . H58A H 0.2131 0.0819 1.0565 0.097 Uiso 1 1 calc R . . H58B H 0.2150 -0.0063 1.0753 0.097 Uiso 1 1 calc R . . H58C H 0.1373 0.0405 1.0703 0.097 Uiso 1 1 calc R . . C59 C 0.3454(3) 0.0068(3) 0.8359(2) 0.0462(13) Uani 1 1 d . . . C60 C 0.4141(3) 0.0429(3) 0.8505(2) 0.0505(14) Uani 1 1 d . . . C61 C 0.3984(3) 0.1094(3) 0.8810(2) 0.0422(12) Uani 1 1 d . . . C62 C 0.3303(4) -0.0667(3) 0.8034(3) 0.0683(18) Uani 1 1 d . . . H62A H 0.3073 -0.1043 0.8267 0.102 Uiso 1 1 calc R . . H62B H 0.3779 -0.0872 0.7930 0.102 Uiso 1 1 calc R . . H62C H 0.2959 -0.0564 0.7695 0.102 Uiso 1 1 calc R . . C63 C 0.4553(3) 0.1654(4) 0.9065(3) 0.0625(16) Uani 1 1 d . . . H63A H 0.4449 0.1775 0.9447 0.094 Uiso 1 1 calc R . . H63B H 0.4526 0.2126 0.8841 0.094 Uiso 1 1 calc R . . H63C H 0.5059 0.1431 0.9075 0.094 Uiso 1 1 calc R . . B1 B 0.3615(3) 0.2860(3) 1.0590(3) 0.0419(13) Uani 1 1 d . . . B2 B 0.2045(3) 0.0341(3) 0.8467(2) 0.0423(13) Uani 1 1 d . . . H1X H 0.400(3) 0.314(2) 1.0919(19) 0.038(12) Uiso 1 1 d . . . H2X H 0.194(3) -0.015(3) 0.8172(19) 0.044(13) Uiso 1 1 d . . . H4 H 0.269(3) 0.588(3) 1.249(2) 0.041(14) Uiso 1 1 d . . . H6 H 0.311(2) 0.580(2) 1.0898(17) 0.025(11) Uiso 1 1 d . . . H15 H 0.222(2) 0.525(2) 1.0227(17) 0.024(11) Uiso 1 1 d . . . H19 H -0.237(2) 0.295(2) 1.1203(18) 0.027(11) Uiso 1 1 d . . . H21 H -0.171(2) 0.286(2) 0.9717(19) 0.028(12) Uiso 1 1 d . . . H30 H -0.056(2) 0.332(2) 0.9525(16) 0.012(9) Uiso 1 1 d . . . H31A H 0.084(3) 0.510(3) 0.952(2) 0.050(14) Uiso 1 1 d . . . H31B H 0.156(2) 0.468(2) 0.9484(17) 0.022(11) Uiso 1 1 d . . . H32 H 0.039(2) 0.400(2) 0.9177(16) 0.014(9) Uiso 1 1 d . . . H35 H 0.159(3) 0.308(3) 1.160(2) 0.039(13) Uiso 1 1 d . . . H45 H 0.489(3) 0.058(3) 1.083(2) 0.059(16) Uiso 1 1 d . . . H55 H 0.110(3) -0.093(3) 0.988(2) 0.063(17) Uiso 1 1 d . . . H60 H 0.463(3) 0.026(3) 0.8401(19) 0.042(13) Uiso 1 1 d . . . C64 C 0.1007(7) 0.8968(7) 0.1831(5) 0.191(2) Uani 1 1 d D . . H64A H 0.1165 0.9200 0.2196 0.286 Uiso 1 1 calc R . . H64B H 0.1437 0.8949 0.1611 0.286 Uiso 1 1 calc R . . H64C H 0.0823 0.8446 0.1884 0.286 Uiso 1 1 calc R . . C65 C 0.0348(7) 0.9470(7) 0.1506(6) 0.191(2) Uani 1 1 d D . . H65A H -0.0094 0.9492 0.1721 0.229 Uiso 1 1 calc R . . H65B H 0.0524 1.0000 0.1449 0.229 Uiso 1 1 calc R . . C66 C 0.0155(8) 0.9094(8) 0.0980(5) 0.191(2) Uani 1 1 d D . . H66A H 0.0281 0.9422 0.0667 0.229 Uiso 1 1 calc R . . H66B H -0.0391 0.8973 0.0923 0.229 Uiso 1 1 calc R . . C67 C 0.0622(7) 0.8359(8) 0.1011(5) 0.191(2) Uani 1 1 d D . . H67A H 0.0349 0.8040 0.0712 0.229 Uiso 1 1 calc R . . H67B H 0.1087 0.8525 0.0856 0.229 Uiso 1 1 calc R . . C68 C 0.0889(8) 0.7818(7) 0.1398(6) 0.191(2) Uani 1 1 d D . . H68A H 0.0865 0.7328 0.1188 0.229 Uiso 1 1 calc R . . H68B H 0.0497 0.7782 0.1657 0.229 Uiso 1 1 calc R . . C69 C 0.1574(7) 0.7787(8) 0.1744(6) 0.191(2) Uani 1 1 d D . . H69A H 0.1577 0.7336 0.1988 0.286 Uiso 1 1 calc R . . H69B H 0.1633 0.8253 0.1973 0.286 Uiso 1 1 calc R . . H69C H 0.1991 0.7750 0.1512 0.286 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.02695(12) 0.02381(11) 0.02996(13) -0.00105(11) 0.00569(9) 0.00273(11) Ni1 0.0239(3) 0.0259(3) 0.0269(3) -0.0003(2) 0.0049(2) 0.0005(2) O1 0.0299(16) 0.0394(17) 0.0297(16) -0.0052(13) 0.0064(13) -0.0061(13) O2 0.0288(15) 0.0314(15) 0.0281(15) 0.0005(12) 0.0063(12) -0.0035(12) O3 0.0312(16) 0.0319(16) 0.0402(18) -0.0021(13) 0.0074(13) 0.0007(13) O4 0.0364(18) 0.0267(16) 0.081(3) 0.0064(16) 0.0238(17) 0.0043(14) N1 0.0261(17) 0.0274(17) 0.0271(19) 0.0014(14) 0.0052(14) 0.0018(14) N2 0.0244(17) 0.0258(17) 0.0281(18) -0.0010(14) 0.0069(14) 0.0008(14) N3 0.047(2) 0.036(2) 0.033(2) -0.0050(16) 0.0060(18) 0.0051(17) N4 0.035(2) 0.037(2) 0.036(2) -0.0009(17) 0.0094(17) 0.0019(17) N5 0.033(2) 0.036(2) 0.053(3) -0.0062(18) 0.0099(19) -0.0065(17) N6 0.032(2) 0.039(2) 0.050(2) 0.0052(19) 0.0063(18) -0.0097(18) N7 0.0308(19) 0.043(2) 0.034(2) -0.0049(18) 0.0000(16) 0.0009(17) N8 0.036(2) 0.033(2) 0.039(2) -0.0034(17) -0.0004(17) 0.0060(17) N9 0.040(2) 0.049(2) 0.030(2) -0.0043(18) -0.0015(17) 0.0063(18) N10 0.036(2) 0.043(2) 0.031(2) 0.0038(16) 0.0045(16) 0.0117(17) N11 0.043(2) 0.030(2) 0.045(2) -0.0070(17) 0.0042(19) -0.0041(17) N12 0.044(2) 0.032(2) 0.038(2) -0.0005(17) 0.0082(18) -0.0012(17) N13 0.044(2) 0.036(2) 0.030(2) -0.0002(16) 0.0077(17) 0.0131(18) N14 0.033(2) 0.046(2) 0.034(2) -0.0010(18) 0.0066(17) 0.0102(17) C1 0.032(2) 0.032(2) 0.040(3) -0.002(2) 0.004(2) -0.0055(19) C2 0.034(2) 0.032(2) 0.038(3) -0.0026(19) 0.003(2) 0.0000(19) C3 0.032(2) 0.047(3) 0.035(3) -0.005(2) 0.003(2) -0.001(2) C4 0.043(3) 0.055(3) 0.038(3) -0.011(3) 0.000(2) -0.005(2) C5 0.039(3) 0.049(3) 0.050(3) -0.010(2) 0.002(2) -0.009(2) C6 0.040(3) 0.044(3) 0.042(3) -0.003(2) 0.007(2) -0.013(2) C7 0.043(3) 0.060(3) 0.033(3) -0.010(2) 0.004(2) -0.002(2) C8 0.060(4) 0.066(4) 0.050(3) 0.005(3) 0.018(3) -0.001(3) C9 0.046(3) 0.067(4) 0.061(4) -0.017(3) 0.018(3) -0.001(3) C10 0.064(4) 0.112(5) 0.039(3) -0.022(3) 0.013(3) -0.012(4) C11 0.044(3) 0.081(4) 0.058(4) -0.018(3) 0.003(3) -0.025(3) C12 0.050(4) 0.134(7) 0.094(6) -0.015(5) 0.004(4) -0.047(4) C13 0.068(5) 0.219(11) 0.116(7) 0.064(7) -0.047(5) -0.065(6) C14 0.087(6) 0.106(6) 0.136(8) -0.054(6) 0.002(5) -0.043(5) C15 0.032(2) 0.038(3) 0.035(3) 0.003(2) 0.009(2) -0.002(2) C16 0.027(2) 0.026(2) 0.030(2) -0.0002(17) 0.0056(17) 0.0028(17) C17 0.029(2) 0.0216(19) 0.032(2) 0.0020(17) 0.0061(18) 0.0038(17) C18 0.033(2) 0.028(2) 0.034(2) -0.0008(18) 0.0079(19) -0.0008(18) C19 0.034(2) 0.034(2) 0.039(3) 0.003(2) 0.014(2) -0.003(2) C20 0.032(2) 0.030(2) 0.039(3) -0.0005(18) 0.0081(19) -0.0008(17) C21 0.033(2) 0.035(2) 0.033(3) -0.007(2) 0.0007(19) -0.003(2) C22 0.041(3) 0.047(3) 0.029(2) -0.003(2) 0.011(2) -0.008(2) C23 0.059(3) 0.065(4) 0.036(3) 0.009(3) -0.001(2) -0.010(3) C24 0.062(3) 0.052(3) 0.041(3) -0.015(2) 0.016(3) -0.006(3) C25 0.061(4) 0.088(4) 0.039(3) -0.009(3) 0.023(3) -0.021(3) C26 0.032(2) 0.048(3) 0.045(3) -0.001(2) 0.004(2) -0.009(2) C27 0.042(3) 0.083(4) 0.053(3) -0.008(3) 0.006(3) -0.025(3) C28 0.042(3) 0.049(3) 0.071(4) 0.003(3) 0.006(3) -0.017(2) C29 0.033(3) 0.063(4) 0.071(4) 0.006(3) 0.004(3) -0.003(3) C30 0.033(2) 0.030(2) 0.030(2) -0.0057(19) 0.0034(19) 0.0024(19) C31 0.029(2) 0.035(2) 0.032(2) 0.0039(19) 0.010(2) 0.005(2) C32 0.027(2) 0.031(2) 0.025(2) 0.0015(17) 0.0049(18) 0.0008(17) C33 0.030(2) 0.035(2) 0.029(2) -0.0021(18) 0.0053(18) 0.0019(18) C34 0.060(3) 0.044(3) 0.035(3) -0.003(2) 0.004(2) 0.017(2) C35 0.067(4) 0.061(4) 0.037(3) 0.004(3) 0.021(3) 0.025(3) C36 0.050(3) 0.041(3) 0.040(3) 0.012(2) 0.016(2) 0.017(2) C37 0.087(5) 0.070(4) 0.048(3) -0.020(3) 0.003(3) 0.015(3) C38 0.044(3) 0.057(3) 0.068(4) 0.024(3) 0.024(3) 0.005(3) C39 0.053(3) 0.044(3) 0.074(4) -0.008(3) 0.024(3) -0.014(3) C40 0.071(4) 0.043(3) 0.089(5) 0.009(3) 0.029(4) -0.016(3) C41 0.037(3) 0.053(3) 0.063(4) 0.013(3) 0.012(3) -0.005(2) C42 0.118(6) 0.051(4) 0.107(6) -0.027(4) 0.040(5) -0.040(4) C43 0.070(4) 0.084(4) 0.059(4) 0.029(3) 0.005(3) -0.026(3) C44 0.030(2) 0.064(3) 0.033(3) 0.000(2) 0.005(2) 0.002(2) C45 0.036(3) 0.060(3) 0.040(3) 0.007(2) 0.003(2) 0.017(2) C46 0.038(3) 0.044(3) 0.033(3) 0.004(2) 0.007(2) 0.009(2) C47 0.041(3) 0.087(4) 0.049(3) -0.006(3) -0.008(2) 0.003(3) C48 0.054(3) 0.039(3) 0.052(3) 0.004(2) 0.004(3) 0.015(2) C49 0.050(3) 0.081(4) 0.035(3) -0.008(3) -0.008(2) 0.009(3) C50 0.055(3) 0.100(5) 0.036(3) 0.002(3) -0.006(3) 0.028(3) C51 0.047(3) 0.061(3) 0.037(3) 0.013(2) 0.013(2) 0.020(2) C52 0.111(6) 0.107(6) 0.051(4) -0.028(4) -0.031(4) 0.007(5) C53 0.105(5) 0.074(4) 0.046(3) 0.026(3) 0.018(3) 0.049(4) C54 0.052(3) 0.035(3) 0.064(4) -0.004(2) 0.003(3) -0.005(2) C55 0.066(4) 0.035(3) 0.074(4) 0.006(3) 0.022(3) -0.012(3) C56 0.055(3) 0.035(3) 0.052(3) 0.005(2) 0.020(3) 0.001(2) C57 0.087(5) 0.045(3) 0.088(5) -0.015(3) 0.004(4) -0.017(3) C58 0.102(5) 0.045(3) 0.050(4) 0.003(3) 0.026(3) -0.007(3) C59 0.063(3) 0.045(3) 0.033(3) 0.010(2) 0.017(2) 0.028(3) C60 0.049(3) 0.067(4) 0.040(3) 0.017(3) 0.022(3) 0.033(3) C61 0.034(2) 0.060(3) 0.034(3) 0.010(2) 0.012(2) 0.014(2) C62 0.108(5) 0.045(3) 0.058(4) -0.001(3) 0.036(4) 0.026(3) C63 0.033(3) 0.095(5) 0.062(4) 0.003(3) 0.012(3) 0.003(3) B1 0.038(3) 0.039(3) 0.048(3) -0.012(2) -0.001(3) 0.000(2) B2 0.046(3) 0.042(3) 0.038(3) -0.008(3) 0.002(3) 0.003(3) C64 0.176(6) 0.212(7) 0.181(6) 0.031(5) 0.003(5) -0.016(5) C65 0.176(6) 0.212(7) 0.181(6) 0.031(5) 0.003(5) -0.016(5) C66 0.176(6) 0.212(7) 0.181(6) 0.031(5) 0.003(5) -0.016(5) C67 0.176(6) 0.212(7) 0.181(6) 0.031(5) 0.003(5) -0.016(5) C68 0.176(6) 0.212(7) 0.181(6) 0.031(5) 0.003(5) -0.016(5) C69 0.176(6) 0.212(7) 0.181(6) 0.031(5) 0.003(5) -0.016(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O4 2.508(3) . ? La1 N6 2.567(4) . ? La1 N12 2.599(4) . ? La1 O3 2.637(3) . ? La1 N4 2.658(4) . ? La1 N8 2.685(4) . ? La1 N14 2.692(4) . ? La1 N10 2.707(4) . ? La1 C33 2.914(4) . ? Ni1 N1 1.842(3) . ? Ni1 N2 1.852(3) . ? Ni1 O2 1.854(3) . ? Ni1 O1 1.858(3) . ? O1 C2 1.311(5) . ? O2 C17 1.312(5) . ? O3 C33 1.248(5) . ? O4 C33 1.258(5) . ? N1 C15 1.277(5) . ? N1 C31 1.473(5) . ? N2 C30 1.293(5) . ? N2 C32 1.469(5) . ? N3 C34 1.365(6) . ? N3 N4 1.382(5) . ? N3 B1 1.540(7) . ? N4 C36 1.330(6) . ? N5 C39 1.350(6) . ? N5 N6 1.363(5) . ? N5 B1 1.548(7) . ? N6 C41 1.335(6) . ? N7 C44 1.343(6) . ? N7 N8 1.378(5) . ? N7 B1 1.535(6) . ? N8 C46 1.343(6) . ? N9 C49 1.352(6) . ? N9 N10 1.371(5) . ? N9 B2 1.528(7) . ? N10 C51 1.349(6) . ? N11 C54 1.356(6) . ? N11 N12 1.381(5) . ? N11 B2 1.545(7) . ? N12 C56 1.337(6) . ? N13 C59 1.348(6) . ? N13 N14 1.384(5) . ? N13 B2 1.541(7) . ? N14 C61 1.344(6) . ? C1 C6 1.413(6) . ? C1 C2 1.419(6) . ? C1 C15 1.432(6) . ? C2 C3 1.445(6) . ? C3 C4 1.375(7) . ? C3 C7 1.523(7) . ? C4 C5 1.404(7) . ? C5 C6 1.360(7) . ? C5 C11 1.535(7) . ? C7 C8 1.528(7) . ? C7 C9 1.529(7) . ? C7 C10 1.535(7) . ? C11 C13 1.472(9) . ? C11 C12 1.504(9) . ? C11 C14 1.569(10) . ? C16 C21 1.413(6) . ? C16 C17 1.418(6) . ? C16 C30 1.425(6) . ? C17 C18 1.439(6) . ? C18 C19 1.377(6) . ? C18 C22 1.535(6) . ? C19 C20 1.409(6) . ? C20 C21 1.363(6) . ? C20 C26 1.532(6) . ? C22 C23 1.524(7) . ? C22 C24 1.535(7) . ? C22 C25 1.542(6) . ? C26 C27 1.526(7) . ? C26 C29 1.526(7) . ? C26 C28 1.536(7) . ? C31 C32 1.505(6) . ? C32 C33 1.539(6) . ? C34 C35 1.359(8) . ? C34 C37 1.507(8) . ? C35 C36 1.379(7) . ? C36 C38 1.509(7) . ? C39 C40 1.370(8) . ? C39 C42 1.498(8) . ? C40 C41 1.387(8) . ? C41 C43 1.494(8) . ? C44 C45 1.367(7) . ? C44 C47 1.504(7) . ? C45 C46 1.390(7) . ? C46 C48 1.485(7) . ? C49 C50 1.348(8) . ? C49 C52 1.520(8) . ? C50 C51 1.388(8) . ? C51 C53 1.486(8) . ? C54 C55 1.363(8) . ? C54 C57 1.496(7) . ? C55 C56 1.388(7) . ? C56 C58 1.488(7) . ? C59 C60 1.373(8) . ? C59 C62 1.492(7) . ? C60 C61 1.400(7) . ? C61 C63 1.475(8) . ? C64 C65 1.580(12) . ? C65 C66 1.417(12) . ? C66 C67 1.509(12) . ? C67 C68 1.356(11) . ? C68 C69 1.384(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 La1 N6 65.66(11) . . ? O4 La1 N12 144.53(11) . . ? N6 La1 N12 149.80(12) . . ? O4 La1 O3 50.59(9) . . ? N6 La1 O3 115.05(11) . . ? N12 La1 O3 94.71(11) . . ? O4 La1 N4 76.54(12) . . ? N6 La1 N4 84.97(12) . . ? N12 La1 N4 101.00(12) . . ? O3 La1 N4 70.89(10) . . ? O4 La1 N8 126.01(11) . . ? N6 La1 N8 71.19(12) . . ? N12 La1 N8 83.35(12) . . ? O3 La1 N8 138.32(10) . . ? N4 La1 N8 68.71(11) . . ? O4 La1 N14 128.82(11) . . ? N6 La1 N14 84.19(12) . . ? N12 La1 N14 73.38(12) . . ? O3 La1 N14 144.50(10) . . ? N4 La1 N14 143.40(11) . . ? N8 La1 N14 74.70(11) . . ? O4 La1 N10 84.42(12) . . ? N6 La1 N10 112.62(12) . . ? N12 La1 N10 78.63(12) . . ? O3 La1 N10 75.17(10) . . ? N4 La1 N10 145.93(11) . . ? N8 La1 N10 143.43(11) . . ? N14 La1 N10 69.76(11) . . ? O4 La1 C33 25.45(11) . . ? N6 La1 C33 89.88(12) . . ? N12 La1 C33 120.05(12) . . ? O3 La1 C33 25.37(10) . . ? N4 La1 C33 69.48(11) . . ? N8 La1 C33 135.19(11) . . ? N14 La1 C33 145.16(12) . . ? N10 La1 C33 81.18(11) . . ? N1 Ni1 N2 86.16(15) . . ? N1 Ni1 O2 178.89(14) . . ? N2 Ni1 O2 93.40(13) . . ? N1 Ni1 O1 93.47(14) . . ? N2 Ni1 O1 177.35(14) . . ? O2 Ni1 O1 86.91(12) . . ? C2 O1 Ni1 128.2(3) . . ? C17 O2 Ni1 128.5(3) . . ? C33 O3 La1 89.8(2) . . ? C33 O4 La1 95.6(3) . . ? C15 N1 C31 119.1(4) . . ? C15 N1 Ni1 127.1(3) . . ? C31 N1 Ni1 113.7(3) . . ? C30 N2 C32 118.9(4) . . ? C30 N2 Ni1 126.6(3) . . ? C32 N2 Ni1 114.5(3) . . ? C34 N3 N4 108.8(4) . . ? C34 N3 B1 127.3(4) . . ? N4 N3 B1 123.2(4) . . ? C36 N4 N3 106.6(4) . . ? C36 N4 La1 136.2(3) . . ? N3 N4 La1 115.9(2) . . ? C39 N5 N6 108.6(4) . . ? C39 N5 B1 128.3(5) . . ? N6 N5 B1 123.1(4) . . ? C41 N6 N5 107.9(4) . . ? C41 N6 La1 127.8(3) . . ? N5 N6 La1 116.9(3) . . ? C44 N7 N8 109.8(4) . . ? C44 N7 B1 127.0(4) . . ? N8 N7 B1 123.2(4) . . ? C46 N8 N7 106.1(4) . . ? C46 N8 La1 136.6(3) . . ? N7 N8 La1 116.8(2) . . ? C49 N9 N10 109.9(4) . . ? C49 N9 B2 126.6(4) . . ? N10 N9 B2 123.4(4) . . ? C51 N10 N9 105.8(4) . . ? C51 N10 La1 135.2(3) . . ? N9 N10 La1 119.0(3) . . ? C54 N11 N12 109.2(4) . . ? C54 N11 B2 127.4(4) . . ? N12 N11 B2 122.5(4) . . ? C56 N12 N11 106.9(4) . . ? C56 N12 La1 132.2(3) . . ? N11 N12 La1 119.8(3) . . ? C59 N13 N14 110.2(4) . . ? C59 N13 B2 125.7(4) . . ? N14 N13 B2 124.0(4) . . ? C61 N14 N13 105.9(4) . . ? C61 N14 La1 135.0(3) . . ? N13 N14 La1 117.4(3) . . ? C6 C1 C2 121.3(4) . . ? C6 C1 C15 118.2(4) . . ? C2 C1 C15 120.4(4) . . ? O1 C2 C1 122.9(4) . . ? O1 C2 C3 119.9(4) . . ? C1 C2 C3 117.1(4) . . ? C4 C3 C2 117.5(4) . . ? C4 C3 C7 121.3(4) . . ? C2 C3 C7 121.2(4) . . ? C3 C4 C5 125.9(5) . . ? C6 C5 C4 116.2(5) . . ? C6 C5 C11 123.8(5) . . ? C4 C5 C11 120.0(5) . . ? C5 C6 C1 121.8(5) . . ? C3 C7 C8 110.4(4) . . ? C3 C7 C9 108.9(4) . . ? C8 C7 C9 109.9(4) . . ? C3 C7 C10 112.4(4) . . ? C8 C7 C10 107.8(5) . . ? C9 C7 C10 107.4(4) . . ? C13 C11 C12 110.8(6) . . ? C13 C11 C5 111.0(5) . . ? C12 C11 C5 112.6(5) . . ? C13 C11 C14 108.7(7) . . ? C12 C11 C14 105.4(6) . . ? C5 C11 C14 108.1(5) . . ? N1 C15 C1 126.3(4) . . ? C21 C16 C17 121.2(4) . . ? C21 C16 C30 117.9(4) . . ? C17 C16 C30 120.9(4) . . ? O2 C17 C16 122.7(4) . . ? O2 C17 C18 119.9(4) . . ? C16 C17 C18 117.3(4) . . ? C19 C18 C17 117.7(4) . . ? C19 C18 C22 122.1(4) . . ? C17 C18 C22 120.1(4) . . ? C18 C19 C20 125.8(4) . . ? C21 C20 C19 115.9(4) . . ? C21 C20 C26 124.3(4) . . ? C19 C20 C26 119.8(4) . . ? C20 C21 C16 122.1(4) . . ? C23 C22 C24 110.6(4) . . ? C23 C22 C18 110.2(4) . . ? C24 C22 C18 108.8(4) . . ? C23 C22 C25 107.3(4) . . ? C24 C22 C25 107.7(4) . . ? C18 C22 C25 112.2(4) . . ? C27 C26 C29 110.0(4) . . ? C27 C26 C20 111.1(4) . . ? C29 C26 C20 108.9(4) . . ? C27 C26 C28 107.8(4) . . ? C29 C26 C28 108.7(4) . . ? C20 C26 C28 110.3(4) . . ? N2 C30 C16 126.2(4) . . ? N1 C31 C32 107.8(3) . . ? N2 C32 C31 106.7(3) . . ? N2 C32 C33 112.2(3) . . ? C31 C32 C33 112.4(4) . . ? O3 C33 O4 122.9(4) . . ? O3 C33 C32 120.0(4) . . ? O4 C33 C32 116.9(4) . . ? O3 C33 La1 64.8(2) . . ? O4 C33 La1 59.0(2) . . ? C32 C33 La1 172.7(3) . . ? C35 C34 N3 107.6(5) . . ? C35 C34 C37 129.1(5) . . ? N3 C34 C37 123.3(5) . . ? C34 C35 C36 107.0(5) . . ? N4 C36 C35 110.1(5) . . ? N4 C36 C38 123.9(5) . . ? C35 C36 C38 126.0(5) . . ? N5 C39 C40 108.4(5) . . ? N5 C39 C42 122.9(6) . . ? C40 C39 C42 128.7(5) . . ? C39 C40 C41 106.1(5) . . ? N6 C41 C40 109.0(5) . . ? N6 C41 C43 121.2(5) . . ? C40 C41 C43 129.8(5) . . ? N7 C44 C45 108.1(4) . . ? N7 C44 C47 123.2(5) . . ? C45 C44 C47 128.6(5) . . ? C44 C45 C46 106.3(4) . . ? N8 C46 C45 109.7(4) . . ? N8 C46 C48 123.5(4) . . ? C45 C46 C48 126.8(4) . . ? C50 C49 N9 107.9(5) . . ? C50 C49 C52 128.3(5) . . ? N9 C49 C52 123.8(5) . . ? C49 C50 C51 107.0(5) . . ? N10 C51 C50 109.4(5) . . ? N10 C51 C53 123.8(5) . . ? C50 C51 C53 126.8(5) . . ? N11 C54 C55 107.5(5) . . ? N11 C54 C57 124.0(5) . . ? C55 C54 C57 128.5(5) . . ? C54 C55 C56 107.3(5) . . ? N12 C56 C55 109.1(5) . . ? N12 C56 C58 121.4(5) . . ? C55 C56 C58 129.3(5) . . ? N13 C59 C60 107.7(5) . . ? N13 C59 C62 124.2(5) . . ? C60 C59 C62 128.1(5) . . ? C59 C60 C61 106.3(4) . . ? N14 C61 C60 109.8(5) . . ? N14 C61 C63 124.5(5) . . ? C60 C61 C63 125.7(5) . . ? N7 B1 N3 109.8(4) . . ? N7 B1 N5 110.2(4) . . ? N3 B1 N5 113.9(4) . . ? N9 B2 N13 110.0(4) . . ? N9 B2 N11 113.2(4) . . ? N13 B2 N11 110.7(4) . . ? C66 C65 C64 105.7(10) . . ? C65 C66 C67 105.4(9) . . ? C68 C67 C66 139.1(13) . . ? C67 C68 C69 130.1(13) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.185 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.092 data_x0037fin _database_code_depnum_ccdc_archive 'CCDC 736174' _audit_creation_date 2009-06-01T00:26:16-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C69 H103 B2 Cu La N14 O4' _chemical_formula_weight 1416.72 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.4518(8) _cell_length_b 16.6530(19) _cell_length_c 17.2355(16) _cell_angle_alpha 108.151(9) _cell_angle_beta 109.351(7) _cell_angle_gamma 95.541(7) _cell_volume 3625.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 63752 _cell_measurement_theta_min 2.523 _cell_measurement_theta_max 31.9196 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'pale brown' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1486 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.93 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.89796 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_orient_matrix_ub_11 0.0333470459 _diffrn_orient_matrix_ub_12 -0.0109426078 _diffrn_orient_matrix_ub_13 -0.0220430194 _diffrn_orient_matrix_ub_21 -0.0350964317 _diffrn_orient_matrix_ub_22 -0.0395315553 _diffrn_orient_matrix_ub_23 -0.0293878827 _diffrn_orient_matrix_ub_31 -0.0226631681 _diffrn_orient_matrix_ub_32 0.0209044082 _diffrn_orient_matrix_ub_33 -0.0292767919 _diffrn_measurement_device_type 'ccd Xcalibur S' _diffrn_measurement_method \w-scans _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_unetI/netI 0.026 _diffrn_reflns_number 105164 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 30.51 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 21995 _reflns_number_gt 18549 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_solution ; SHELXS-97 Program for Crystal Structure Analysis (Release 97-2) G. M. Sheldrick, Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998. ; _computing_structure_refinement ; SHELXL-97 G. M. Sheldrick, 2008, Acta Cryst., A64, 112-122 ; _computing_molecular_graphics ; ORTEP3 for Windows L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565. ; _computing_publication_material ; WINGX L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838. ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0388P)^2^+3.4098P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 21995 _refine_ls_number_parameters 873 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.033 _refine_ls_wR_factor_ref 0.0847 _refine_ls_wR_factor_gt 0.0779 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.031 _refine_diff_density_min -1.257 _refine_diff_density_rms 0.078 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 La1 La 0.481654(8) 0.444482(7) 0.234168(7) 0.01740(3) Uani 1 1 d . . . Cu1 Cu 0.601319(16) 0.121943(15) 0.047641(15) 0.01815(5) Uani 1 1 d . A . O1 O 0.61051(10) 0.09505(9) -0.06537(9) 0.0225(3) Uani 1 1 d . . . O2 O 0.73997(10) 0.12315(10) 0.09825(9) 0.0241(3) Uani 1 1 d . . . O3 O 0.40020(11) 0.27990(10) 0.13796(11) 0.0212(4) Uani 0.945(4) 1 d P A 1 O4 O 0.54557(13) 0.31185(10) 0.25049(13) 0.0241(4) Uani 0.945(4) 1 d P A 1 O3F O 0.511(2) 0.298(2) 0.210(2) 0.018(6) Uiso 0.055(4) 1 d P A 2 O4F O 0.3723(17) 0.2909(14) 0.0936(16) 0.014(6) Uiso 0.055(4) 1 d P A 2 N1 N 0.45571(12) 0.09910(11) -0.00217(11) 0.0225(3) Uani 1 1 d D . . N2 N 0.58679(11) 0.15537(11) 0.15985(11) 0.0203(3) Uani 1 1 d D . . N3 N 0.67304(12) 0.40718(11) 0.16031(11) 0.0207(3) Uani 1 1 d . . . N4 N 0.56980(12) 0.39332(11) 0.12124(11) 0.0207(3) Uani 1 1 d . A . N5 N 0.73463(12) 0.47152(11) 0.33100(11) 0.0213(3) Uani 1 1 d . . . N6 N 0.65515(12) 0.47936(11) 0.35727(11) 0.0211(3) Uani 1 1 d . A . N7 N 0.69727(12) 0.56749(11) 0.23983(11) 0.0209(3) Uani 1 1 d . . . N8 N 0.60187(12) 0.57747(10) 0.23420(11) 0.0216(3) Uani 1 1 d . A . N9 N 0.26005(12) 0.44037(12) 0.27746(12) 0.0260(4) Uani 1 1 d . . . N10 N 0.33874(13) 0.39849(11) 0.28691(12) 0.0251(3) Uani 1 1 d . A . N11 N 0.25673(13) 0.51904(13) 0.17022(12) 0.0284(4) Uani 1 1 d . . . N12 N 0.33163(13) 0.49671(11) 0.14071(11) 0.0225(3) Uani 1 1 d . A . N13 N 0.35862(13) 0.59569(11) 0.33457(12) 0.0240(3) Uani 1 1 d . . . N14 N 0.45551(12) 0.58450(11) 0.34892(11) 0.0221(3) Uani 1 1 d . A . C1 C 0.43481(15) 0.06818(13) -0.15491(13) 0.0235(4) Uani 1 1 d . . . C2 C 0.53836(15) 0.08016(12) -0.14176(13) 0.0221(4) Uani 1 1 d . A . C3 C 0.56371(16) 0.07448(14) -0.21708(14) 0.0265(4) Uani 1 1 d . . . C4 C 0.48558(18) 0.05733(14) -0.29733(14) 0.0299(4) Uani 1 1 d . A . H4 H 0.5027 0.0538 -0.3468 0.036 Uiso 1 1 calc R . . C5 C 0.38279(17) 0.04478(13) -0.31103(14) 0.0287(4) Uani 1 1 d . . . C6 C 0.35937(16) 0.05026(14) -0.23915(14) 0.0278(4) Uani 1 1 d . A . H6 H 0.2908 0.0418 -0.2459 0.033 Uiso 1 1 calc R . . C7 C 0.67381(18) 0.08804(17) -0.20831(15) 0.0335(5) Uani 1 1 d . A . C8 C 0.73288(19) 0.17839(18) -0.14089(18) 0.0408(6) Uani 1 1 d . . . H8A H 0.7004 0.2224 -0.1586 0.061 Uiso 1 1 calc R A . H8B H 0.8019 0.1875 -0.1385 0.061 Uiso 1 1 calc R . . H8C H 0.734 0.183 -0.0825 0.061 Uiso 1 1 calc R . . C9 C 0.7226(2) 0.01873(19) -0.17877(19) 0.0446(6) Uani 1 1 d . . . H9A H 0.7211 0.0237 -0.121 0.067 Uiso 1 1 calc R A . H9B H 0.7925 0.0274 -0.1743 0.067 Uiso 1 1 calc R . . H9C H 0.6852 -0.039 -0.2222 0.067 Uiso 1 1 calc R . . C10 C 0.6834(2) 0.0808(3) -0.2965(2) 0.0566(8) Uani 1 1 d . . . H10A H 0.6488 0.0226 -0.3405 0.085 Uiso 1 1 calc R A . H10B H 0.7546 0.0911 -0.2878 0.085 Uiso 1 1 calc R . . H10C H 0.6527 0.124 -0.3173 0.085 Uiso 1 1 calc R . . C11 C 0.30397(19) 0.02495(15) -0.40417(15) 0.0346(5) Uani 1 1 d . A . C12 C 0.3101(3) -0.06131(18) -0.46650(17) 0.0497(7) Uani 1 1 d . . . H12A H 0.2986 -0.1072 -0.4442 0.075 Uiso 1 1 calc R A . H12B H 0.3768 -0.0562 -0.4695 0.075 Uiso 1 1 calc R . . H12C H 0.2586 -0.0757 -0.5256 0.075 Uiso 1 1 calc R . . C13 C 0.1976(2) 0.01759(19) -0.40485(17) 0.0437(6) Uani 1 1 d . . . H13A H 0.1932 0.072 -0.3643 0.066 Uiso 1 1 calc R A . H13B H 0.1818 -0.03 -0.386 0.066 Uiso 1 1 calc R . . H13C H 0.1495 0.006 -0.4647 0.066 Uiso 1 1 calc R . . C14 C 0.3248(2) 0.09715(18) -0.43774(17) 0.0428(6) Uani 1 1 d . . . H14A H 0.2753 0.0831 -0.4976 0.064 Uiso 1 1 calc R A . H14B H 0.3926 0.1024 -0.4385 0.064 Uiso 1 1 calc R . . H14C H 0.3198 0.1522 -0.3985 0.064 Uiso 1 1 calc R . . C15 C 0.39993(15) 0.07540(13) -0.08456(14) 0.0246(4) Uani 1 1 d . A . H15 H 0.3292 0.0614 -0.1004 0.03 Uiso 1 1 calc R . . C16 C 0.76217(14) 0.17252(13) 0.25106(13) 0.0221(4) Uani 1 1 d . . . C17 C 0.79680(14) 0.14339(12) 0.18136(13) 0.0209(3) Uani 1 1 d . A . C18 C 0.90042(14) 0.13542(13) 0.20466(14) 0.0226(4) Uani 1 1 d . . . C19 C 0.96093(15) 0.16249(14) 0.29354(14) 0.0263(4) Uani 1 1 d . A . H19 H 1.0293 0.1585 0.3083 0.032 Uiso 1 1 calc R . . C20 C 0.92884(15) 0.19544(15) 0.36378(14) 0.0277(4) Uani 1 1 d . . . C21 C 0.82861(15) 0.19850(14) 0.34041(14) 0.0260(4) Uani 1 1 d . A . H21 H 0.8034 0.2187 0.3857 0.031 Uiso 1 1 calc R . . C22 C 0.94039(15) 0.09807(14) 0.13194(14) 0.0248(4) Uani 1 1 d . A . C23 C 0.93967(18) 0.15810(16) 0.07979(17) 0.0342(5) Uani 1 1 d . . . H23A H 0.8708 0.1644 0.053 0.051 Uiso 1 1 calc R A . H23B H 0.9647 0.133 0.0333 0.051 Uiso 1 1 calc R . . H23C H 0.9831 0.2151 0.1198 0.051 Uiso 1 1 calc R . . C24 C 0.87536(17) 0.00779(15) 0.06809(16) 0.0318(5) Uani 1 1 d . . . H24A H 0.8736 -0.0301 0.1014 0.048 Uiso 1 1 calc R A . H24B H 0.9042 -0.0169 0.0243 0.048 Uiso 1 1 calc R . . H24C H 0.8068 0.0129 0.0379 0.048 Uiso 1 1 calc R . . C25 C 1.04883(17) 0.08708(18) 0.17010(17) 0.0380(5) Uani 1 1 d . . . H25A H 1.0934 0.1438 0.2093 0.057 Uiso 1 1 calc R A . H25B H 1.071 0.0616 0.1217 0.057 Uiso 1 1 calc R . . H25C H 1.0512 0.0488 0.2035 0.057 Uiso 1 1 calc R . . C26 C 1.00366(17) 0.22426(18) 0.45999(15) 0.0363(5) Uani 1 1 d . A . C27 C 1.0509(2) 0.1494(2) 0.4758(2) 0.0515(7) Uani 1 1 d . . . H27A H 0.9982 0.1013 0.4657 0.077 Uiso 1 1 calc R A . H27B H 1.0999 0.1692 0.5367 0.077 Uiso 1 1 calc R . . H27C H 1.0849 0.1298 0.4349 0.077 Uiso 1 1 calc R . . C28 C 1.08813(19) 0.2997(2) 0.47969(18) 0.0466(7) Uani 1 1 d . . . H28A H 1.1252 0.2806 0.4414 0.07 Uiso 1 1 calc R A . H28B H 1.1341 0.319 0.5417 0.07 Uiso 1 1 calc R . . H28C H 1.0591 0.3478 0.4686 0.07 Uiso 1 1 calc R . . C29 C 0.9513(2) 0.2523(3) 0.52455(17) 0.0595(9) Uani 1 1 d . . . H29A H 0.9242 0.3028 0.5188 0.089 Uiso 1 1 calc R A . H29B H 0.9998 0.2674 0.5851 0.089 Uiso 1 1 calc R . . H29C H 0.8962 0.2046 0.5112 0.089 Uiso 1 1 calc R . . C30 C 0.65829(14) 0.17556(13) 0.23588(13) 0.0218(4) Uani 1 1 d . A . H30 H 0.6412 0.194 0.2864 0.026 Uiso 1 1 calc R . . C31 C 0.40889(15) 0.10390(15) 0.06263(14) 0.0208(4) Uani 0.945(4) 1 d PD A 1 H31A H 0.389 0.0452 0.0623 0.025 Uiso 0.945(4) 1 calc PR A 1 H31B H 0.3477 0.1273 0.0468 0.025 Uiso 0.945(4) 1 calc PR A 1 C32 C 0.48406(13) 0.16283(13) 0.15459(13) 0.0179(4) Uani 0.945(4) 1 d PD A 1 H32 H 0.4708 0.1404 0.1982 0.022 Uiso 0.945(4) 1 calc PR A 1 C33 C 0.47607(16) 0.25879(15) 0.18147(15) 0.0181(4) Uani 0.945(4) 1 d P A 1 C31F C 0.4872(11) 0.123(3) 0.158(2) 0.020(7) Uiso 0.055(4) 1 d PD A 2 H31C H 0.4751 0.1573 0.2108 0.023 Uiso 0.055(4) 1 calc PR A 2 H31D H 0.474 0.0605 0.1491 0.023 Uiso 0.055(4) 1 calc PR A 2 C32F C 0.432(4) 0.141(4) 0.0756(19) 0.052(16) Uiso 0.055(4) 1 d PD A 2 H32F H 0.3601 0.1117 0.0574 0.062 Uiso 0.055(4) 1 calc PR A 2 C33F C 0.435(3) 0.254(2) 0.134(2) 0.010(6) Uiso 0.055(4) 1 d P A 2 C34 C 0.54141(16) 0.32883(13) 0.04247(13) 0.0242(4) Uani 1 1 d . . . C35 C 0.62505(18) 0.30078(14) 0.03023(14) 0.0286(4) Uani 1 1 d . A . H35 H 0.6256 0.2561 -0.0198 0.034 Uiso 1 1 calc R . . C36 C 0.70704(16) 0.35139(13) 0.10582(14) 0.0255(4) Uani 1 1 d . A . C37 C 0.43473(19) 0.29938(15) -0.02191(15) 0.0351(5) Uani 1 1 d . A . H37A H 0.3899 0.3147 0.0097 0.053 Uiso 1 1 calc R . . H37B H 0.419 0.2364 -0.0525 0.053 Uiso 1 1 calc R . . H37C H 0.4253 0.3277 -0.0651 0.053 Uiso 1 1 calc R . . C38 C 0.81495(18) 0.34726(17) 0.12742(18) 0.0371(5) Uani 1 1 d . . . H38A H 0.8565 0.406 0.151 0.056 Uiso 1 1 calc R A . H38B H 0.8236 0.3128 0.0738 0.056 Uiso 1 1 calc R . . H38C H 0.8356 0.3203 0.1716 0.056 Uiso 1 1 calc R . . C39 C 0.67890(16) 0.46328(13) 0.43175(13) 0.0247(4) Uani 1 1 d . . . C40 C 0.77410(18) 0.44541(18) 0.45481(16) 0.0370(5) Uani 1 1 d . A . H40 H 0.8092 0.4322 0.505 0.044 Uiso 1 1 calc R . . C41 C 0.80698(17) 0.45078(18) 0.38995(16) 0.0350(5) Uani 1 1 d . A . C42 C 0.60721(18) 0.46561(16) 0.47779(15) 0.0318(5) Uani 1 1 d . A . H42A H 0.5449 0.4779 0.4436 0.048 Uiso 1 1 calc R . . H42B H 0.6377 0.5111 0.5368 0.048 Uiso 1 1 calc R . . H42C H 0.5922 0.4094 0.4831 0.048 Uiso 1 1 calc R . . C43 C 0.9043(2) 0.4370(3) 0.3806(2) 0.0633(10) Uani 1 1 d . . . H43A H 0.8911 0.3851 0.3285 0.095 Uiso 1 1 calc R A . H43B H 0.9489 0.4293 0.4334 0.095 Uiso 1 1 calc R . . H43C H 0.9365 0.4875 0.3737 0.095 Uiso 1 1 calc R . . C44 C 0.59666(16) 0.65610(13) 0.23031(13) 0.0254(4) Uani 1 1 d . . . C45 C 0.68815(17) 0.69683(14) 0.23353(14) 0.0289(4) Uani 1 1 d . A . H45 H 0.7045 0.7531 0.2326 0.035 Uiso 1 1 calc R . . C46 C 0.74937(16) 0.63873(14) 0.23830(13) 0.0266(4) Uani 1 1 d . A . C47 C 0.50420(18) 0.69162(14) 0.22233(16) 0.0322(5) Uani 1 1 d . A . H47A H 0.4668 0.683 0.1603 0.048 Uiso 1 1 calc R . . H47B H 0.5235 0.7537 0.2581 0.048 Uiso 1 1 calc R . . H47C H 0.4617 0.6615 0.2433 0.048 Uiso 1 1 calc R . . C48 C 0.85203(18) 0.64499(18) 0.23518(18) 0.0394(6) Uani 1 1 d . . . H48A H 0.8958 0.6277 0.2814 0.059 Uiso 1 1 calc R A . H48B H 0.8802 0.7048 0.2449 0.059 Uiso 1 1 calc R . . H48C H 0.8473 0.6065 0.1772 0.059 Uiso 1 1 calc R . . C49 C 0.31073(18) 0.32931(14) 0.30514(15) 0.0318(5) Uani 1 1 d . . . C50 C 0.21500(19) 0.32729(16) 0.30787(17) 0.0397(6) Uani 1 1 d . A . H50 H 0.178 0.2856 0.3199 0.048 Uiso 1 1 calc R . . C51 C 0.18518(17) 0.39695(17) 0.28996(16) 0.0358(5) Uani 1 1 d . A . C52 C 0.3745(2) 0.26625(16) 0.3201(2) 0.0447(7) Uani 1 1 d . A . H52A H 0.3546 0.216 0.2651 0.067 Uiso 1 1 calc R . . H52B H 0.3657 0.2473 0.3661 0.067 Uiso 1 1 calc R . . H52C H 0.4453 0.294 0.3389 0.067 Uiso 1 1 calc R . . C53 C 0.08725(19) 0.4235(2) 0.2826(2) 0.0572(8) Uani 1 1 d . . . H53A H 0.1 0.481 0.3277 0.086 Uiso 1 1 calc R A . H53B H 0.0436 0.3814 0.2915 0.086 Uiso 1 1 calc R . . H53C H 0.0542 0.4256 0.2238 0.086 Uiso 1 1 calc R . . C54 C 0.30946(17) 0.50806(14) 0.06327(14) 0.0274(4) Uani 1 1 d . . . C55 C 0.2206(2) 0.53757(19) 0.04261(17) 0.0415(6) Uani 1 1 d . A . H55 H 0.188 0.5503 -0.0085 0.05 Uiso 1 1 calc R . . C56 C 0.18985(19) 0.5445(2) 0.11125(18) 0.0427(6) Uani 1 1 d . A . C57 C 0.3764(2) 0.49492(16) 0.01340(16) 0.0355(5) Uani 1 1 d . A . H57A H 0.4378 0.4815 0.0476 0.053 Uiso 1 1 calc R . . H57B H 0.394 0.5479 0.003 0.053 Uiso 1 1 calc R . . H57C H 0.3417 0.4467 -0.0434 0.053 Uiso 1 1 calc R . . C58 C 0.0987(3) 0.5735(3) 0.1233(3) 0.0787(13) Uani 1 1 d . . . H58A H 0.057 0.5273 0.1289 0.118 Uiso 1 1 calc R A . H58B H 0.0597 0.5866 0.0719 0.118 Uiso 1 1 calc R . . H58C H 0.1199 0.6256 0.1768 0.118 Uiso 1 1 calc R . . C59 C 0.51685(16) 0.65802(13) 0.41313(13) 0.0244(4) Uani 1 1 d . . . C60 C 0.45997(19) 0.71611(14) 0.43970(16) 0.0334(5) Uani 1 1 d . A . H60 H 0.4848 0.7726 0.4839 0.04 Uiso 1 1 calc R . . C61 C 0.36083(18) 0.67520(15) 0.38908(16) 0.0324(5) Uani 1 1 d . A . C62 C 0.62901(16) 0.67315(14) 0.44869(14) 0.0290(4) Uani 1 1 d . A . H62A H 0.6511 0.645 0.4917 0.044 Uiso 1 1 calc R . . H62B H 0.6582 0.7356 0.4776 0.044 Uiso 1 1 calc R . . H62C H 0.6512 0.6488 0.4001 0.044 Uiso 1 1 calc R . . C63 C 0.2684(2) 0.7079(2) 0.3906(2) 0.0560(8) Uani 1 1 d . . . H63A H 0.2305 0.71 0.3327 0.084 Uiso 1 1 calc R A . H63B H 0.2878 0.7662 0.4359 0.084 Uiso 1 1 calc R . . H63C H 0.2263 0.669 0.4043 0.084 Uiso 1 1 calc R . . B1 B 0.73560(16) 0.48559(15) 0.24644(15) 0.0215(4) Uani 1 1 d . A . B2 B 0.26350(17) 0.52750(17) 0.26386(16) 0.0267(5) Uani 1 1 d . A . H1B H 0.8124(18) 0.4918(16) 0.2500(16) 0.025(6) Uiso 1 1 d . . . H2B H 0.1954(19) 0.5491(17) 0.2737(17) 0.029(7) Uiso 1 1 d . . . C64 C 1.0280(5) 0.9057(5) 0.3165(5) 0.147(3) Uani 1 1 d D . . H64A H 1.0182 0.9404 0.3695 0.22 Uiso 1 1 calc R . . H64B H 1.0779 0.9408 0.3061 0.22 Uiso 1 1 calc R . . H64C H 1.0521 0.8548 0.3251 0.22 Uiso 1 1 calc R . . C65 C 0.9321(4) 0.8774(3) 0.2400(4) 0.0889(15) Uani 1 1 d D . . H65A H 0.9074 0.9284 0.2307 0.107 Uiso 1 1 calc R . . H65B H 0.881 0.8426 0.2502 0.107 Uiso 1 1 calc R . . C66 C 0.9503(5) 0.8204(4) 0.1551(4) 0.142(3) Uani 1 1 d D . . H66A H 0.993 0.8562 0.1381 0.17 Uiso 1 1 calc R . . H66B H 0.9819 0.7725 0.1654 0.17 Uiso 1 1 calc R . . C67 C 0.8402(4) 0.7847(3) 0.0828(4) 0.117(2) Uani 1 1 d D . . H67A H 0.8014 0.7396 0.0931 0.141 Uiso 1 1 calc R . . H67B H 0.8037 0.8318 0.0804 0.141 Uiso 1 1 calc R . . C68 C 0.8611(5) 0.7479(4) 0.0013(7) 0.216(6) Uani 1 1 d D . . H68A H 0.7938 0.7268 -0.0472 0.259 Uiso 1 1 calc R . . H68B H 0.8937 0.7991 -0.0053 0.259 Uiso 1 1 calc R . . C69 C 0.9111(5) 0.6878(3) -0.0216(4) 0.114(2) Uani 1 1 d D . . H69A H 0.9052 0.6766 -0.0825 0.172 Uiso 1 1 calc R . . H69B H 0.8829 0.6342 -0.0172 0.172 Uiso 1 1 calc R . . H69C H 0.9822 0.7083 0.0181 0.172 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.01554(5) 0.01557(5) 0.02293(5) 0.00606(4) 0.01010(4) 0.00490(3) Cu1 0.01718(10) 0.01959(11) 0.01967(11) 0.00719(9) 0.00860(8) 0.00720(8) O1 0.0235(6) 0.0250(7) 0.0202(6) 0.0076(5) 0.0094(5) 0.0092(5) O2 0.0195(6) 0.0351(8) 0.0207(6) 0.0105(6) 0.0096(5) 0.0116(6) O3 0.0171(7) 0.0194(7) 0.0271(8) 0.0081(6) 0.0083(6) 0.0060(6) O4 0.0247(8) 0.0186(7) 0.0239(9) 0.0058(6) 0.0048(7) 0.0055(6) N1 0.0210(7) 0.0233(8) 0.0249(8) 0.0093(7) 0.0100(6) 0.0066(6) N2 0.0183(7) 0.0214(7) 0.0232(8) 0.0075(6) 0.0103(6) 0.0073(6) N3 0.0210(7) 0.0224(8) 0.0225(8) 0.0084(6) 0.0126(6) 0.0057(6) N4 0.0211(7) 0.0207(7) 0.0192(7) 0.0060(6) 0.0077(6) 0.0033(6) N5 0.0174(7) 0.0276(8) 0.0209(7) 0.0099(6) 0.0084(6) 0.0065(6) N6 0.0223(7) 0.0243(8) 0.0209(7) 0.0091(6) 0.0118(6) 0.0079(6) N7 0.0215(7) 0.0205(7) 0.0195(7) 0.0064(6) 0.0085(6) -0.0001(6) N8 0.0235(8) 0.0192(7) 0.0232(8) 0.0077(6) 0.0105(6) 0.0041(6) N9 0.0187(7) 0.0307(9) 0.0271(8) 0.0045(7) 0.0133(7) 0.0025(7) N10 0.0254(8) 0.0218(8) 0.0322(9) 0.0073(7) 0.0186(7) 0.0048(6) N11 0.0220(8) 0.0372(10) 0.0275(9) 0.0116(8) 0.0094(7) 0.0141(7) N12 0.0244(8) 0.0216(8) 0.0234(8) 0.0078(6) 0.0111(7) 0.0083(6) N13 0.0235(8) 0.0235(8) 0.0279(8) 0.0075(7) 0.0135(7) 0.0110(6) N14 0.0209(7) 0.0212(8) 0.0250(8) 0.0068(6) 0.0108(6) 0.0064(6) C1 0.0249(9) 0.0209(9) 0.0227(9) 0.0077(7) 0.0069(7) 0.0053(7) C2 0.0262(9) 0.0181(8) 0.0222(9) 0.0067(7) 0.0095(7) 0.0085(7) C3 0.0316(10) 0.0250(10) 0.0244(9) 0.0077(8) 0.0122(8) 0.0114(8) C4 0.0411(12) 0.0272(10) 0.0209(9) 0.0075(8) 0.0115(9) 0.0108(9) C5 0.0359(11) 0.0207(9) 0.0227(9) 0.0056(8) 0.0051(8) 0.0063(8) C6 0.0272(10) 0.0243(10) 0.0269(10) 0.0092(8) 0.0048(8) 0.0048(8) C7 0.0346(11) 0.0457(13) 0.0290(11) 0.0156(10) 0.0188(9) 0.0172(10) C8 0.0340(12) 0.0467(15) 0.0466(14) 0.0166(12) 0.0222(11) 0.0073(11) C9 0.0453(14) 0.0525(16) 0.0475(15) 0.0184(13) 0.0264(12) 0.0301(13) C10 0.0506(16) 0.096(3) 0.0392(15) 0.0292(16) 0.0297(13) 0.0260(17) C11 0.0423(13) 0.0262(11) 0.0240(10) 0.0070(8) 0.0017(9) 0.0046(9) C12 0.0654(19) 0.0371(14) 0.0261(12) 0.0008(10) 0.0029(12) 0.0108(13) C13 0.0389(13) 0.0469(15) 0.0312(12) 0.0155(11) -0.0031(10) 0.0026(11) C14 0.0495(15) 0.0409(14) 0.0323(12) 0.0191(11) 0.0044(11) 0.0065(11) C15 0.0208(8) 0.0230(9) 0.0280(10) 0.0096(8) 0.0065(8) 0.0048(7) C16 0.0192(8) 0.0260(9) 0.0231(9) 0.0099(8) 0.0088(7) 0.0079(7) C17 0.0197(8) 0.0218(9) 0.0233(9) 0.0092(7) 0.0091(7) 0.0076(7) C18 0.0200(8) 0.0234(9) 0.0277(9) 0.0110(8) 0.0107(7) 0.0086(7) C19 0.0184(8) 0.0312(10) 0.0304(10) 0.0132(9) 0.0081(8) 0.0082(8) C20 0.0221(9) 0.0350(11) 0.0248(10) 0.0113(9) 0.0070(8) 0.0071(8) C21 0.0229(9) 0.0336(11) 0.0224(9) 0.0096(8) 0.0097(8) 0.0084(8) C22 0.0203(8) 0.0286(10) 0.0287(10) 0.0099(8) 0.0123(8) 0.0110(7) C23 0.0361(12) 0.0366(12) 0.0424(13) 0.0186(11) 0.0251(11) 0.0123(10) C24 0.0304(10) 0.0287(11) 0.0362(12) 0.0070(9) 0.0163(9) 0.0097(9) C25 0.0242(10) 0.0515(15) 0.0388(13) 0.0121(11) 0.0143(9) 0.0177(10) C26 0.0232(10) 0.0550(15) 0.0245(10) 0.0125(10) 0.0037(8) 0.0082(10) C27 0.0378(14) 0.071(2) 0.0436(15) 0.0318(15) 0.0029(12) 0.0144(14) C28 0.0281(11) 0.0588(17) 0.0364(13) 0.0121(12) 0.0000(10) -0.0007(11) C29 0.0327(13) 0.109(3) 0.0232(12) 0.0125(15) 0.0063(10) 0.0115(15) C30 0.0214(8) 0.0255(9) 0.0216(9) 0.0087(7) 0.0111(7) 0.0084(7) C31 0.0179(9) 0.0179(10) 0.0259(10) 0.0062(8) 0.0098(8) 0.0027(7) C32 0.0172(8) 0.0162(9) 0.0235(9) 0.0084(7) 0.0099(7) 0.0060(7) C33 0.0183(9) 0.0174(10) 0.0219(11) 0.0071(8) 0.0114(9) 0.0056(8) C34 0.0339(10) 0.0180(8) 0.0203(9) 0.0071(7) 0.0099(8) 0.0052(7) C35 0.0436(12) 0.0208(9) 0.0263(10) 0.0084(8) 0.0183(9) 0.0116(9) C36 0.0325(10) 0.0229(9) 0.0317(10) 0.0125(8) 0.0212(9) 0.0120(8) C37 0.0412(12) 0.0253(10) 0.0244(10) 0.0058(8) -0.0009(9) 0.0037(9) C38 0.0351(12) 0.0383(13) 0.0494(14) 0.0182(11) 0.0250(11) 0.0194(10) C39 0.0288(10) 0.0261(10) 0.0208(9) 0.0091(8) 0.0109(8) 0.0065(8) C40 0.0324(11) 0.0578(16) 0.0298(11) 0.0264(11) 0.0114(9) 0.0169(11) C41 0.0240(10) 0.0576(15) 0.0317(11) 0.0250(11) 0.0104(9) 0.0169(10) C42 0.0383(12) 0.0377(12) 0.0284(10) 0.0154(9) 0.0198(9) 0.0116(10) C43 0.0341(14) 0.128(3) 0.0623(19) 0.064(2) 0.0264(14) 0.0444(18) C44 0.0333(10) 0.0184(9) 0.0203(9) 0.0064(7) 0.0069(8) 0.0022(8) C45 0.0344(11) 0.0222(9) 0.0230(9) 0.0092(8) 0.0044(8) -0.0043(8) C46 0.0284(10) 0.0262(10) 0.0179(8) 0.0075(7) 0.0042(8) -0.0071(8) C47 0.0397(12) 0.0213(10) 0.0365(12) 0.0118(9) 0.0140(10) 0.0092(9) C48 0.0286(11) 0.0425(14) 0.0437(14) 0.0193(11) 0.0107(10) -0.0077(10) C49 0.0432(12) 0.0227(10) 0.0330(11) 0.0047(8) 0.0258(10) 0.0003(9) C50 0.0405(13) 0.0346(12) 0.0424(13) 0.0046(10) 0.0277(11) -0.0091(10) C51 0.0230(10) 0.0440(13) 0.0340(12) 0.0034(10) 0.0165(9) -0.0051(9) C52 0.0743(19) 0.0293(12) 0.0580(16) 0.0227(12) 0.0507(16) 0.0190(12) C53 0.0241(12) 0.081(2) 0.066(2) 0.0198(17) 0.0253(13) 0.0033(13) C54 0.0331(10) 0.0227(9) 0.0254(10) 0.0095(8) 0.0091(8) 0.0073(8) C55 0.0401(13) 0.0530(16) 0.0357(13) 0.0236(12) 0.0096(11) 0.0222(12) C56 0.0318(12) 0.0621(17) 0.0384(13) 0.0227(13) 0.0101(10) 0.0261(12) C57 0.0526(14) 0.0352(12) 0.0326(11) 0.0206(10) 0.0229(11) 0.0195(11) C58 0.0520(19) 0.145(4) 0.065(2) 0.055(3) 0.0251(17) 0.069(2) C59 0.0287(10) 0.0213(9) 0.0230(9) 0.0070(7) 0.0106(8) 0.0049(7) C60 0.0407(12) 0.0206(10) 0.0361(12) 0.0034(9) 0.0173(10) 0.0087(9) C61 0.0382(12) 0.0256(10) 0.0374(12) 0.0080(9) 0.0206(10) 0.0149(9) C62 0.0287(10) 0.0250(10) 0.0265(10) 0.0049(8) 0.0076(8) 0.0013(8) C63 0.0489(16) 0.0401(15) 0.076(2) 0.0040(14) 0.0314(16) 0.0249(13) B1 0.0180(9) 0.0250(10) 0.0221(10) 0.0076(8) 0.0100(8) 0.0030(8) B2 0.0203(10) 0.0322(12) 0.0293(11) 0.0091(9) 0.0121(9) 0.0117(9) C64 0.115(5) 0.186(8) 0.183(7) 0.118(7) 0.062(5) 0.036(5) C65 0.120(4) 0.071(3) 0.124(4) 0.059(3) 0.080(4) 0.029(3) C66 0.136(5) 0.132(5) 0.136(5) 0.086(5) 0.017(4) -0.061(4) C67 0.103(4) 0.097(4) 0.183(6) 0.103(4) 0.050(4) 0.000(3) C68 0.187(7) 0.098(5) 0.502(18) 0.136(8) 0.268(11) 0.062(5) C69 0.149(5) 0.076(3) 0.110(4) 0.019(3) 0.063(4) -0.010(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 La1 O3F 2.44(3) . ? La1 O4 2.5337(16) . ? La1 N6 2.5595(17) . ? La1 O3 2.6266(15) . ? La1 N4 2.6376(16) . ? La1 N12 2.6409(17) . ? La1 N10 2.6554(16) . ? La1 N8 2.6793(16) . ? La1 N14 2.6988(17) . ? La1 O4F 2.78(2) . ? La1 C33 2.924(2) . ? La1 C33F 2.98(3) . ? Cu1 O2 1.8972(14) . ? Cu1 O1 1.9109(14) . ? Cu1 N2 1.9275(16) . ? Cu1 N1 1.9377(16) . ? O1 C2 1.311(2) . ? O2 C17 1.306(2) . ? O3 C33 1.258(3) . ? O4 C33 1.260(3) . ? O3F C33F 1.32(4) . ? O4F C33F 1.28(4) . ? N1 C15 1.286(3) . ? N1 C31 1.472(2) . ? N1 C32F 1.477(5) . ? N2 C30 1.288(2) . ? N2 C31F 1.476(5) . ? N2 C32 1.477(2) . ? N3 C36 1.355(2) . ? N3 N4 1.380(2) . ? N3 B1 1.550(3) . ? N4 C34 1.342(2) . ? N5 C41 1.352(3) . ? N5 N6 1.371(2) . ? N5 B1 1.551(3) . ? N6 C39 1.333(3) . ? N7 C46 1.355(2) . ? N7 N8 1.380(2) . ? N7 B1 1.543(3) . ? N8 C44 1.340(3) . ? N9 C51 1.357(3) . ? N9 N10 1.381(2) . ? N9 B2 1.539(3) . ? N10 C49 1.345(3) . ? N11 C56 1.357(3) . ? N11 N12 1.376(2) . ? N11 B2 1.545(3) . ? N12 C54 1.344(3) . ? N13 C61 1.354(3) . ? N13 N14 1.381(2) . ? N13 B2 1.546(3) . ? N14 C59 1.344(3) . ? C1 C6 1.416(3) . ? C1 C2 1.421(3) . ? C1 C15 1.437(3) . ? C2 C3 1.440(3) . ? C3 C4 1.388(3) . ? C3 C7 1.535(3) . ? C4 C5 1.408(3) . ? C5 C6 1.368(3) . ? C5 C11 1.539(3) . ? C7 C8 1.532(4) . ? C7 C10 1.540(3) . ? C7 C9 1.541(4) . ? C11 C13 1.526(4) . ? C11 C14 1.533(3) . ? C11 C12 1.533(4) . ? C16 C21 1.416(3) . ? C16 C17 1.418(3) . ? C16 C30 1.445(3) . ? C17 C18 1.447(3) . ? C18 C19 1.386(3) . ? C18 C22 1.535(3) . ? C19 C20 1.410(3) . ? C20 C21 1.380(3) . ? C20 C26 1.538(3) . ? C22 C23 1.537(3) . ? C22 C24 1.538(3) . ? C22 C25 1.539(3) . ? C26 C29 1.527(4) . ? C26 C28 1.532(4) . ? C26 C27 1.532(4) . ? C31 C32 1.529(3) . ? C32 C33 1.547(3) . ? C31F C32F 1.529(6) . ? C32F C33F 1.82(6) . ? C34 C35 1.393(3) . ? C34 C37 1.493(3) . ? C35 C36 1.383(3) . ? C36 C38 1.492(3) . ? C39 C40 1.389(3) . ? C39 C42 1.496(3) . ? C40 C41 1.375(3) . ? C41 C43 1.499(3) . ? C44 C45 1.402(3) . ? C44 C47 1.495(3) . ? C45 C46 1.376(3) . ? C46 C48 1.497(3) . ? C49 C50 1.397(3) . ? C49 C52 1.489(4) . ? C50 C51 1.363(4) . ? C51 C53 1.501(4) . ? C54 C55 1.395(3) . ? C54 C57 1.483(3) . ? C55 C56 1.372(4) . ? C56 C58 1.501(4) . ? C59 C60 1.396(3) . ? C59 C62 1.494(3) . ? C60 C61 1.375(3) . ? C61 C63 1.496(3) . ? C64 C65 1.469(7) . ? C65 C66 1.596(7) . ? C66 C67 1.574(7) . ? C67 C68 1.491(8) . ? C68 C69 1.327(7) . ? 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 O3F La1 O4 15.2(8) . . ? O3F La1 N6 80.2(9) . . ? O4 La1 N6 65.99(6) . . ? O3F La1 O3 36.5(9) . . ? O4 La1 O3 50.76(5) . . ? N6 La1 O3 116.65(5) . . ? O3F La1 N4 65.8(6) . . ? O4 La1 N4 71.95(5) . . ? N6 La1 N4 87.10(5) . . ? O3 La1 N4 71.99(5) . . ? O3F La1 N12 129.3(9) . . ? O4 La1 N12 143.90(6) . . ? N6 La1 N12 150.08(5) . . ? O3 La1 N12 93.15(5) . . ? N4 La1 N12 100.52(5) . . ? O3F La1 N10 87.2(6) . . ? O4 La1 N10 87.66(5) . . ? N6 La1 N10 110.27(5) . . ? O3 La1 N10 73.42(5) . . ? N4 La1 N10 145.36(5) . . ? N12 La1 N10 79.48(5) . . ? O3F La1 N8 125.5(7) . . ? O4 La1 N8 120.74(5) . . ? N6 La1 N8 70.19(5) . . ? O3 La1 N8 138.93(5) . . ? N4 La1 N8 67.90(5) . . ? N12 La1 N8 85.82(5) . . ? N10 La1 N8 145.51(5) . . ? O3F La1 N14 144.7(7) . . ? O4 La1 N14 132.79(6) . . ? N6 La1 N14 83.49(5) . . ? O3 La1 N14 142.23(5) . . ? N4 La1 N14 144.23(5) . . ? N12 La1 N14 73.41(5) . . ? N10 La1 N14 69.51(5) . . ? N8 La1 N14 76.44(5) . . ? O3F La1 O4F 51.2(10) . . ? O4 La1 O4F 66.2(5) . . ? N6 La1 O4F 130.6(5) . . ? O3 La1 O4F 17.2(5) . . ? N4 La1 O4F 66.9(4) . . ? N12 La1 O4F 78.3(5) . . ? N10 La1 O4F 79.4(5) . . ? N8 La1 O4F 127.9(5) . . ? N14 La1 O4F 141.0(5) . . ? O3F La1 C33 11.1(8) . . ? O4 La1 C33 25.42(6) . . ? N6 La1 C33 91.17(6) . . ? O3 La1 C33 25.48(5) . . ? N4 La1 C33 68.00(5) . . ? N12 La1 C33 118.58(6) . . ? N10 La1 C33 81.49(5) . . ? N8 La1 C33 132.61(5) . . ? N14 La1 C33 146.33(5) . . ? O4F La1 C33 40.9(5) . . ? O3F La1 C33F 25.8(10) . . ? O4 La1 C33F 40.8(7) . . ? N6 La1 C33F 105.7(7) . . ? O3 La1 C33F 12.5(7) . . ? N4 La1 C33F 63.8(6) . . ? N12 La1 C33F 103.6(7) . . ? N10 La1 C33F 82.4(6) . . ? N8 La1 C33F 131.7(6) . . ? N14 La1 C33F 151.8(6) . . ? O4F La1 C33F 25.4(8) . . ? C33 La1 C33F 15.8(7) . . ? O2 Cu1 O1 89.48(6) . . ? O2 Cu1 N2 93.40(6) . . ? O1 Cu1 N2 175.82(6) . . ? O2 Cu1 N1 168.98(7) . . ? O1 Cu1 N1 93.01(7) . . ? N2 Cu1 N1 84.74(7) . . ? C2 O1 Cu1 128.10(13) . . ? C17 O2 Cu1 128.61(12) . . ? C33 O3 La1 90.58(13) . . ? C33 O4 La1 94.86(13) . . ? C33F O3F La1 101(2) . . ? C33F O4F La1 86.2(18) . . ? C15 N1 C31 119.74(17) . . ? C15 N1 C32F 128.7(18) . . ? C31 N1 C32F 24(3) . . ? C15 N1 Cu1 125.95(14) . . ? C31 N1 Cu1 114.13(13) . . ? C32F N1 Cu1 103(2) . . ? C30 N2 C31F 113.1(12) . . ? C30 N2 C32 119.64(16) . . ? C31F N2 C32 27.1(15) . . ? C30 N2 Cu1 125.88(13) . . ? C31F N2 Cu1 116.4(13) . . ? C32 N2 Cu1 114.35(12) . . ? C36 N3 N4 109.57(16) . . ? C36 N3 B1 127.99(17) . . ? N4 N3 B1 121.76(15) . . ? C34 N4 N3 106.46(16) . . ? C34 N4 La1 133.33(13) . . ? N3 N4 La1 114.07(11) . . ? C41 N5 N6 108.90(16) . . ? C41 N5 B1 128.34(17) . . ? N6 N5 B1 122.76(15) . . ? C39 N6 N5 107.21(16) . . ? C39 N6 La1 128.22(13) . . ? N5 N6 La1 116.18(11) . . ? C46 N7 N8 110.12(17) . . ? C46 N7 B1 126.56(17) . . ? N8 N7 B1 123.32(15) . . ? C44 N8 N7 106.13(16) . . ? C44 N8 La1 137.59(14) . . ? N7 N8 La1 116.29(11) . . ? C51 N9 N10 109.45(19) . . ? C51 N9 B2 126.31(19) . . ? N10 N9 B2 124.00(16) . . ? C49 N10 N9 106.37(17) . . ? C49 N10 La1 134.03(14) . . ? N9 N10 La1 117.90(12) . . ? C56 N11 N12 109.22(19) . . ? C56 N11 B2 127.78(19) . . ? N12 N11 B2 122.17(16) . . ? C54 N12 N11 106.68(17) . . ? C54 N12 La1 132.60(14) . . ? N11 N12 La1 120.72(12) . . ? C61 N13 N14 109.82(17) . . ? C61 N13 B2 126.23(18) . . ? N14 N13 B2 123.91(16) . . ? C59 N14 N13 106.31(16) . . ? C59 N14 La1 134.75(13) . . ? N13 N14 La1 117.98(12) . . ? C6 C1 C2 121.22(19) . . ? C6 C1 C15 115.82(19) . . ? C2 C1 C15 122.94(18) . . ? O1 C2 C1 123.25(18) . . ? O1 C2 C3 119.24(18) . . ? C1 C2 C3 117.51(18) . . ? C4 C3 C2 117.9(2) . . ? C4 C3 C7 121.3(2) . . ? C2 C3 C7 120.86(18) . . ? C3 C4 C5 125.0(2) . . ? C6 C5 C4 116.79(19) . . ? C6 C5 C11 123.9(2) . . ? C4 C5 C11 119.3(2) . . ? C5 C6 C1 121.6(2) . . ? C8 C7 C3 110.29(19) . . ? C8 C7 C10 107.5(2) . . ? C3 C7 C10 112.0(2) . . ? C8 C7 C9 109.5(2) . . ? C3 C7 C9 110.2(2) . . ? C10 C7 C9 107.4(2) . . ? C13 C11 C14 108.2(2) . . ? C13 C11 C12 108.8(2) . . ? C14 C11 C12 109.4(2) . . ? C13 C11 C5 111.6(2) . . ? C14 C11 C5 110.19(19) . . ? C12 C11 C5 108.7(2) . . ? N1 C15 C1 125.92(18) . . ? C21 C16 C17 120.99(17) . . ? C21 C16 C30 116.22(18) . . ? C17 C16 C30 122.77(18) . . ? O2 C17 C16 123.38(17) . . ? O2 C17 C18 119.10(17) . . ? C16 C17 C18 117.52(17) . . ? C19 C18 C17 118.00(18) . . ? C19 C18 C22 121.94(17) . . ? C17 C18 C22 120.07(17) . . ? C18 C19 C20 125.07(18) . . ? C21 C20 C19 116.23(19) . . ? C21 C20 C26 123.6(2) . . ? C19 C20 C26 120.17(19) . . ? C20 C21 C16 122.02(19) . . ? C18 C22 C23 110.50(17) . . ? C18 C22 C24 110.31(17) . . ? C23 C22 C24 109.17(19) . . ? C18 C22 C25 111.88(18) . . ? C23 C22 C25 107.94(18) . . ? C24 C22 C25 106.93(18) . . ? C29 C26 C28 109.3(2) . . ? C29 C26 C27 107.6(2) . . ? C28 C26 C27 108.3(2) . . ? C29 C26 C20 111.13(19) . . ? C28 C26 C20 110.0(2) . . ? C27 C26 C20 110.4(2) . . ? N2 C30 C16 125.67(18) . . ? N1 C31 C32 109.23(16) . . ? N2 C32 C31 108.81(15) . . ? N2 C32 C33 110.77(16) . . ? C31 C32 C33 114.57(18) . . ? O3 C33 O4 123.1(2) . . ? O3 C33 C32 120.1(2) . . ? O4 C33 C32 116.64(17) . . ? O3 C33 La1 63.94(11) . . ? O4 C33 La1 59.72(12) . . ? C32 C33 La1 174.33(13) . . ? N2 C31F C32F 93(3) . . ? N1 C32F C31F 115(2) . . ? N1 C32F C33F 132(4) . . ? C31F C32F C33F 96(3) . . ? O4F C33F O3F 122(3) . . ? O4F C33F C32F 118(3) . . ? O3F C33F C32F 119(3) . . ? O4F C33F La1 68.5(17) . . ? O3F C33F La1 53.6(17) . . ? C32F C33F La1 169(3) . . ? N4 C34 C35 110.21(19) . . ? N4 C34 C37 122.04(19) . . ? C35 C34 C37 127.6(2) . . ? C36 C35 C34 105.80(18) . . ? N3 C36 C35 107.97(18) . . ? N3 C36 C38 124.2(2) . . ? C35 C36 C38 127.9(2) . . ? N6 C39 C40 109.87(18) . . ? N6 C39 C42 120.95(19) . . ? C40 C39 C42 129.19(19) . . ? C41 C40 C39 105.71(19) . . ? N5 C41 C40 108.31(19) . . ? N5 C41 C43 122.7(2) . . ? C40 C41 C43 129.0(2) . . ? N8 C44 C45 110.08(19) . . ? N8 C44 C47 123.06(19) . . ? C45 C44 C47 126.85(19) . . ? C46 C45 C44 105.97(18) . . ? N7 C46 C45 107.68(19) . . ? N7 C46 C48 123.2(2) . . ? C45 C46 C48 128.9(2) . . ? N10 C49 C50 109.6(2) . . ? N10 C49 C52 123.8(2) . . ? C50 C49 C52 126.7(2) . . ? C51 C50 C49 106.5(2) . . ? N9 C51 C50 108.1(2) . . ? N9 C51 C53 123.7(3) . . ? C50 C51 C53 128.2(2) . . ? N12 C54 C55 109.9(2) . . ? N12 C54 C57 122.42(19) . . ? C55 C54 C57 127.6(2) . . ? C56 C55 C54 105.9(2) . . ? N11 C56 C55 108.3(2) . . ? N11 C56 C58 123.2(3) . . ? C55 C56 C58 128.5(2) . . ? N14 C59 C60 109.81(19) . . ? N14 C59 C62 123.74(18) . . ? C60 C59 C62 126.4(2) . . ? C61 C60 C59 106.30(19) . . ? N13 C61 C60 107.76(19) . . ? N13 C61 C63 123.5(2) . . ? C60 C61 C63 128.7(2) . . ? N7 B1 N3 109.14(16) . . ? N7 B1 N5 110.78(16) . . ? N3 B1 N5 113.37(16) . . ? N9 B2 N11 112.82(18) . . ? N9 B2 N13 110.96(17) . . ? N11 B2 N13 110.42(18) . . ? C64 C65 C66 108.3(5) . . ? C67 C66 C65 102.3(5) . . ? C68 C67 C66 100.9(5) . . ? C69 C68 C67 131.9(8) . . ? data_c2131fin _database_code_depnum_ccdc_archive 'CCDC 736175' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89 H134 B2 Cr La N18 O4' _chemical_formula_weight 1732.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.8338(11) _cell_length_b 17.3435(11) _cell_length_c 20.1484(13) _cell_angle_alpha 68.7160(10) _cell_angle_beta 66.9650(10) _cell_angle_gamma 67.7940(10) _cell_volume 4849.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 6251 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 23.11 _exptl_crystal_description prism _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1834 _exptl_absorpt_coefficient_mu 0.601 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 CCD area detector' _diffrn_measurement_method '\W scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21299 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0905 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 23.30 _reflns_number_total 13764 _reflns_number_gt 8903 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Two poorly resolved hexane molecules had been removed with SQUEEZE SQUEEZE - P. v.d. Sluis and A. L. Spek, Acta Crystallogr., Sect A 1990, 46, 194-201 ; _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^)+(0.0756P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13764 _refine_ls_number_parameters 979 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1403 _refine_ls_wR_factor_gt 0.1291 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _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 La1 La 0.62850(2) 0.95226(2) 0.728614(17) 0.04641(13) Uani 1 1 d . . . Cr1 Cr 0.77631(6) 0.39041(5) 1.03234(4) 0.0421(2) Uani 1 1 d . . . O1 O 0.8936(2) 0.3154(2) 0.99082(19) 0.0464(9) Uani 1 1 d . . . O2 O 0.7493(2) 0.3064(2) 1.12694(18) 0.0452(9) Uani 1 1 d . . . O3 O 0.7055(2) 0.7998(2) 0.78259(19) 0.0516(10) Uani 1 1 d . . . O4 O 0.5667(2) 0.8529(2) 0.84741(18) 0.0485(9) Uani 1 1 d . . . N1 N 0.7932(3) 0.4832(3) 0.9359(2) 0.0415(11) Uani 1 1 d . . . N2 N 0.6638(3) 0.4749(3) 1.0605(2) 0.0416(11) Uani 1 1 d . . . N3 N 0.8461(3) 0.4362(3) 1.0709(2) 0.0483(12) Uani 1 1 d . . . N4 N 0.9363(3) 0.3947(3) 1.0565(3) 0.0515(12) Uani 1 1 d D . . N5 N 0.7178(3) 0.3305(3) 0.9962(2) 0.0460(11) Uani 1 1 d . . . N6 N 0.7202(3) 0.2488(3) 1.0390(3) 0.0483(12) Uani 1 1 d D . . N7 N 0.6130(3) 1.0407(3) 0.8647(3) 0.0524(12) Uani 1 1 d . . . N8 N 0.6758(3) 0.9749(3) 0.8333(3) 0.0568(13) Uani 1 1 d . . . N9 N 0.6155(3) 1.1553(3) 0.7427(3) 0.0567(13) Uani 1 1 d . . . N10 N 0.6578(3) 1.1076(3) 0.6906(3) 0.0563(13) Uani 1 1 d . . . N11 N 0.4728(3) 1.1110(3) 0.8217(3) 0.0583(13) Uani 1 1 d . . . N12 N 0.4759(3) 1.0530(3) 0.7875(3) 0.0525(12) Uani 1 1 d . . . N13 N 0.6346(4) 0.8438(4) 0.6092(3) 0.0673(15) Uani 1 1 d . . . N14 N 0.5812(3) 0.8542(3) 0.6789(2) 0.0578(13) Uani 1 1 d . . . N15 N 0.7677(4) 0.9081(4) 0.5570(3) 0.0753(16) Uani 1 1 d . . . N16 N 0.7720(4) 0.9180(3) 0.6201(3) 0.0678(15) Uani 1 1 d . . . N17 N 0.6156(4) 1.0029(4) 0.5451(3) 0.0753(17) Uani 1 1 d . . . N18 N 0.5814(4) 1.0434(3) 0.6022(3) 0.0664(15) Uani 1 1 d . . . C1 C 0.9303(3) 0.3974(3) 0.8640(3) 0.0442(13) Uani 1 1 d . . . C2 C 0.9437(4) 0.3197(3) 0.9203(3) 0.0446(14) Uani 1 1 d . . . C3 C 1.0145(4) 0.2472(3) 0.9017(3) 0.0501(14) Uani 1 1 d . . . C4 C 1.0692(4) 0.2564(4) 0.8302(3) 0.0592(16) Uani 1 1 d . . . H4 H 1.1164 0.2081 0.8184 0.071 Uiso 1 1 calc R . . C5 C 1.0605(4) 0.3331(4) 0.7723(3) 0.0640(17) Uani 1 1 d . . . C6 C 0.9898(4) 0.4020(4) 0.7914(3) 0.0575(16) Uani 1 1 d . . . H6 H 0.9809 0.4540 0.7546 0.069 Uiso 1 1 calc R . . C7 C 1.0323(4) 0.1617(4) 0.9606(3) 0.0582(16) Uani 1 1 d . . . C8 C 1.0694(5) 0.1721(4) 1.0137(4) 0.084(2) Uani 1 1 d . . . H8A H 1.0240 0.2127 1.0416 0.126 Uiso 1 1 calc R . . H8B H 1.1220 0.1933 0.9854 0.126 Uiso 1 1 calc R . . H8C H 1.0860 0.1169 1.0480 0.126 Uiso 1 1 calc R . . C9 C 0.9470(4) 0.1328(4) 1.0036(4) 0.076(2) Uani 1 1 d . . . H9A H 0.9044 0.1728 1.0332 0.113 Uiso 1 1 calc R . . H9B H 0.9614 0.0757 1.0361 0.113 Uiso 1 1 calc R . . H9C H 0.9210 0.1316 0.9689 0.113 Uiso 1 1 calc R . . C10 C 1.1013(5) 0.0876(4) 0.9248(4) 0.094(2) Uani 1 1 d . . . H10A H 1.1065 0.0339 0.9632 0.141 Uiso 1 1 calc R . . H10B H 1.1593 0.0995 0.9013 0.141 Uiso 1 1 calc R . . H10C H 1.0811 0.0830 0.8877 0.141 Uiso 1 1 calc R . . C11 C 1.1278(5) 0.3396(5) 0.6941(4) 0.082(2) Uani 1 1 d . . . C12 C 1.1784(7) 0.2504(7) 0.6794(5) 0.170(5) Uani 1 1 d . . . H12A H 1.2058 0.2140 0.7186 0.256 Uiso 1 1 calc R . . H12B H 1.2247 0.2559 0.6318 0.256 Uiso 1 1 calc R . . H12C H 1.1367 0.2249 0.6783 0.256 Uiso 1 1 calc R . . C13 C 1.0792(7) 0.3857(8) 0.6369(4) 0.203(7) Uani 1 1 d . . . H13A H 1.0238 0.3697 0.6537 0.305 Uiso 1 1 calc R . . H13B H 1.1165 0.3700 0.5904 0.305 Uiso 1 1 calc R . . H13C H 1.0656 0.4473 0.6292 0.305 Uiso 1 1 calc R . . C14 C 1.1952(9) 0.3749(11) 0.6896(6) 0.252(9) Uani 1 1 d . . . H14A H 1.1855 0.4338 0.6595 0.378 Uiso 1 1 calc R . . H14B H 1.2542 0.3409 0.6669 0.378 Uiso 1 1 calc R . . H14C H 1.1913 0.3737 0.7393 0.378 Uiso 1 1 calc R . . C15 C 0.8578(3) 0.4737(3) 0.8752(3) 0.0440(13) Uani 1 1 d . . . H15 H 0.8573 0.5218 0.8340 0.053 Uiso 1 1 calc R . . C16 C 0.6284(4) 0.4005(4) 1.1956(3) 0.0483(14) Uani 1 1 d . . . C17 C 0.7037(4) 0.3286(3) 1.1923(3) 0.0432(13) Uani 1 1 d . . . C18 C 0.7290(4) 0.2792(3) 1.2566(3) 0.0496(14) Uani 1 1 d . . . C19 C 0.6821(4) 0.3092(4) 1.3207(3) 0.0592(16) Uani 1 1 d . . . H19 H 0.6996 0.2771 1.3641 0.071 Uiso 1 1 calc R . . C20 C 0.6117(4) 0.3831(4) 1.3248(3) 0.0593(17) Uani 1 1 d . . . C21 C 0.5837(4) 0.4268(4) 1.2614(3) 0.0574(16) Uani 1 1 d . . . H21 H 0.5335 0.4753 1.2630 0.069 Uiso 1 1 calc R . . C22 C 0.8063(4) 0.1968(4) 1.2575(3) 0.0570(16) Uani 1 1 d . . . C23 C 0.8948(4) 0.2175(4) 1.2056(4) 0.079(2) Uani 1 1 d . . . H23A H 0.8939 0.2356 1.1542 0.119 Uiso 1 1 calc R . . H23B H 0.9446 0.1665 1.2120 0.119 Uiso 1 1 calc R . . H23C H 0.9020 0.2633 1.2176 0.119 Uiso 1 1 calc R . . C24 C 0.8203(5) 0.1509(4) 1.3354(3) 0.081(2) Uani 1 1 d . . . H24A H 0.8369 0.1878 1.3512 0.122 Uiso 1 1 calc R . . H24B H 0.8677 0.0975 1.3331 0.122 Uiso 1 1 calc R . . H24C H 0.7650 0.1386 1.3709 0.122 Uiso 1 1 calc R . . C25 C 0.7883(5) 0.1322(4) 1.2334(3) 0.0710(19) Uani 1 1 d . . . H25A H 0.7285 0.1260 1.2619 0.107 Uiso 1 1 calc R . . H25B H 0.8322 0.0769 1.2423 0.107 Uiso 1 1 calc R . . H25C H 0.7929 0.1529 1.1807 0.107 Uiso 1 1 calc R . . C26 C 0.5660(5) 0.4201(4) 1.3937(4) 0.074(2) Uani 1 1 d . . . C27 C 0.6038(6) 0.3620(5) 1.4585(4) 0.112(3) Uani 1 1 d . . . H27A H 0.5667 0.3816 1.5033 0.167 Uiso 1 1 calc R . . H27B H 0.6646 0.3641 1.4469 0.167 Uiso 1 1 calc R . . H27C H 0.6040 0.3033 1.4665 0.167 Uiso 1 1 calc R . . C28 C 0.4659(5) 0.4307(6) 1.4197(4) 0.114(3) Uani 1 1 d . . . H28A H 0.4408 0.4667 1.3789 0.170 Uiso 1 1 calc R . . H28B H 0.4377 0.4576 1.4610 0.170 Uiso 1 1 calc R . . H28C H 0.4551 0.3747 1.4356 0.170 Uiso 1 1 calc R . . C29 C 0.5847(6) 0.5067(5) 1.3736(4) 0.116(3) Uani 1 1 d . . . H29A H 0.5572 0.5471 1.3354 0.173 Uiso 1 1 calc R . . H29B H 0.6490 0.4992 1.3552 0.173 Uiso 1 1 calc R . . H29C H 0.5597 0.5288 1.4176 0.173 Uiso 1 1 calc R . . C30 C 0.5929(4) 0.4513(4) 1.1276(3) 0.0498(15) Uani 1 1 d . . . C31 C 0.7214(3) 0.5606(3) 0.9412(3) 0.0430(13) Uani 1 1 d . . . C32 C 0.6484(3) 0.5512(3) 1.0090(3) 0.0408(13) Uani 1 1 d . . . C33 C 0.5709(4) 0.6209(3) 1.0142(3) 0.0525(15) Uani 1 1 d . . . H33 H 0.5200 0.6156 1.0557 0.063 Uiso 1 1 calc R . . C34 C 0.5682(4) 0.6969(3) 0.9596(3) 0.0516(15) Uani 1 1 d . . . H34 H 0.5155 0.7426 0.9648 0.062 Uiso 1 1 calc R . . C35 C 0.6419(4) 0.7080(3) 0.8962(3) 0.0420(13) Uani 1 1 d . . . C36 C 0.7170(4) 0.6385(3) 0.8877(3) 0.0421(13) Uani 1 1 d . . . H36 H 0.7663 0.6443 0.8449 0.051 Uiso 1 1 calc R . . C37 C 0.6369(4) 0.7912(3) 0.8395(3) 0.0435(14) Uani 1 1 d . . . C38 C 0.9779(4) 0.4212(4) 1.0850(4) 0.0597(16) Uani 1 1 d . . . C39 C 0.9145(5) 0.4824(4) 1.1192(4) 0.0686(18) Uani 1 1 d . . . H39 H 0.9236 0.5132 1.1443 0.082 Uiso 1 1 calc R . . C40 C 0.8327(4) 0.4911(4) 1.1100(4) 0.0620(17) Uani 1 1 d . . . C41 C 1.0749(4) 0.3825(4) 1.0776(4) 0.083(2) Uani 1 1 d . . . H41A H 1.1011 0.3460 1.0433 0.125 Uiso 1 1 calc R . . H41B H 1.0827 0.3484 1.1260 0.125 Uiso 1 1 calc R . . H41C H 1.1045 0.4278 1.0587 0.125 Uiso 1 1 calc R . . C42 C 0.7437(5) 0.5514(5) 1.1363(4) 0.091(2) Uani 1 1 d . . . H42A H 0.7198 0.5852 1.0945 0.137 Uiso 1 1 calc R . . H42B H 0.7505 0.5896 1.1577 0.137 Uiso 1 1 calc R . . H42C H 0.7028 0.5189 1.1737 0.137 Uiso 1 1 calc R . . C43 C 0.6986(4) 0.2042(4) 1.0108(3) 0.0533(15) Uani 1 1 d . . . C44 C 0.6794(4) 0.2591(4) 0.9467(3) 0.0619(17) Uani 1 1 d . . . H44 H 0.6610 0.2468 0.9141 0.074 Uiso 1 1 calc R . . C45 C 0.6923(4) 0.3365(4) 0.9395(3) 0.0560(16) Uani 1 1 d . . . C46 C 0.6969(5) 0.1127(4) 1.0493(4) 0.0748(19) Uani 1 1 d . . . H46A H 0.7404 0.0857 1.0772 0.112 Uiso 1 1 calc R . . H46B H 0.7117 0.0818 1.0126 0.112 Uiso 1 1 calc R . . H46C H 0.6374 0.1114 1.0833 0.112 Uiso 1 1 calc R . . C47 C 0.6796(5) 0.4181(5) 0.8789(4) 0.092(2) Uani 1 1 d . . . H47A H 0.6478 0.4668 0.9009 0.138 Uiso 1 1 calc R . . H47B H 0.6451 0.4152 0.8513 0.138 Uiso 1 1 calc R . . H47C H 0.7378 0.4248 0.8453 0.138 Uiso 1 1 calc R . . C48 C 0.7176(4) 0.9212(4) 0.8843(3) 0.0567(16) Uani 1 1 d . . . C49 C 0.6817(4) 0.9513(4) 0.9481(3) 0.0616(17) Uani 1 1 d . . . H49 H 0.6991 0.9257 0.9920 0.074 Uiso 1 1 calc R . . C50 C 0.6170(4) 1.0244(4) 0.9344(3) 0.0568(16) Uani 1 1 d . . . C51 C 0.7905(5) 0.8421(4) 0.8727(4) 0.078(2) Uani 1 1 d . . . H51A H 0.8022 0.8360 0.8235 0.118 Uiso 1 1 calc R . . H51B H 0.7727 0.7927 0.9102 0.118 Uiso 1 1 calc R . . H51C H 0.8444 0.8458 0.8768 0.118 Uiso 1 1 calc R . . C52 C 0.5512(4) 1.0818(4) 0.9859(3) 0.0728(19) Uani 1 1 d . . . H52A H 0.5578 1.0552 1.0356 0.109 Uiso 1 1 calc R . . H52B H 0.4904 1.0894 0.9875 0.109 Uiso 1 1 calc R . . H52C H 0.5636 1.1374 0.9673 0.109 Uiso 1 1 calc R . . C53 C 0.6969(4) 1.1585(4) 0.6271(4) 0.0654(18) Uani 1 1 d . . . C54 C 0.6775(5) 1.2375(4) 0.6388(4) 0.076(2) Uani 1 1 d . . . H54 H 0.6961 1.2850 0.6030 0.092 Uiso 1 1 calc R . . C55 C 0.6271(5) 1.2360(4) 0.7104(4) 0.0707(19) Uani 1 1 d . . . C56 C 0.7495(5) 1.1300(4) 0.5566(4) 0.084(2) Uani 1 1 d . . . H56A H 0.8095 1.0957 0.5590 0.125 Uiso 1 1 calc R . . H56B H 0.7532 1.1801 0.5145 0.125 Uiso 1 1 calc R . . H56C H 0.7198 1.0959 0.5504 0.125 Uiso 1 1 calc R . . C57 C 0.5887(5) 1.3056(4) 0.7515(4) 0.097(2) Uani 1 1 d . . . H57A H 0.6057 1.2836 0.7971 0.145 Uiso 1 1 calc R . . H57B H 0.5237 1.3232 0.7636 0.145 Uiso 1 1 calc R . . H57C H 0.6118 1.3546 0.7203 0.145 Uiso 1 1 calc R . . C58 C 0.3915(5) 1.0671(4) 0.7905(4) 0.0668(18) Uani 1 1 d . . . C59 C 0.3343(5) 1.1317(5) 0.8265(4) 0.083(2) Uani 1 1 d . . . H59 H 0.2716 1.1527 0.8363 0.100 Uiso 1 1 calc R . . C60 C 0.3876(5) 1.1580(4) 0.8446(4) 0.074(2) Uani 1 1 d . . . C61 C 0.3712(5) 1.0185(5) 0.7536(4) 0.095(2) Uani 1 1 d . . . H61A H 0.4245 0.9736 0.7379 0.143 Uiso 1 1 calc R . . H61B H 0.3523 1.0576 0.7105 0.143 Uiso 1 1 calc R . . H61C H 0.3234 0.9928 0.7886 0.143 Uiso 1 1 calc R . . C62 C 0.3589(5) 1.2275(5) 0.8847(5) 0.115(3) Uani 1 1 d . . . H62A H 0.3814 1.2042 0.9276 0.172 Uiso 1 1 calc R . . H62B H 0.2939 1.2475 0.9011 0.172 Uiso 1 1 calc R . . H62C H 0.3830 1.2753 0.8511 0.172 Uiso 1 1 calc R . . C63 C 0.5425(4) 0.7902(4) 0.7109(3) 0.0581(16) Uani 1 1 d . . . C64 C 0.5705(4) 0.7381(5) 0.6633(4) 0.0717(19) Uani 1 1 d . . . H64 H 0.5533 0.6887 0.6727 0.086 Uiso 1 1 calc R . . C65 C 0.6291(5) 0.7737(5) 0.5991(4) 0.076(2) Uani 1 1 d . . . C66 C 0.4761(4) 0.7779(4) 0.7863(3) 0.0701(18) Uani 1 1 d . . . H66A H 0.4615 0.8263 0.8063 0.105 Uiso 1 1 calc R . . H66B H 0.5015 0.7252 0.8191 0.105 Uiso 1 1 calc R . . H66C H 0.4220 0.7741 0.7827 0.105 Uiso 1 1 calc R . . C67 C 0.6804(6) 0.7441(6) 0.5282(4) 0.110(3) Uani 1 1 d . . . H67A H 0.6646 0.6941 0.5319 0.165 Uiso 1 1 calc R . . H67B H 0.7443 0.7292 0.5209 0.165 Uiso 1 1 calc R . . H67C H 0.6651 0.7901 0.4863 0.165 Uiso 1 1 calc R . . C68 C 0.8576(6) 0.9147(5) 0.6084(4) 0.086(2) Uani 1 1 d . . . C69 C 0.9073(6) 0.9022(6) 0.5371(5) 0.115(3) Uani 1 1 d . . . H69 H 0.9689 0.8973 0.5142 0.138 Uiso 1 1 calc R . . C70 C 0.8485(7) 0.8986(6) 0.5070(4) 0.104(3) Uani 1 1 d . . . C71 C 0.8864(5) 0.9244(6) 0.6654(4) 0.106(3) Uani 1 1 d . . . H71A H 0.8349 0.9552 0.6986 0.158 Uiso 1 1 calc R . . H71B H 0.9311 0.9563 0.6408 0.158 Uiso 1 1 calc R . . H71C H 0.9121 0.8679 0.6939 0.158 Uiso 1 1 calc R . . C72 C 0.8695(6) 0.8877(8) 0.4302(5) 0.157(5) Uani 1 1 d . . . H72A H 0.8741 0.8288 0.4341 0.235 Uiso 1 1 calc R . . H72B H 0.9259 0.9006 0.3988 0.235 Uiso 1 1 calc R . . H72C H 0.8219 0.9267 0.4085 0.235 Uiso 1 1 calc R . . C73 C 0.5317(5) 1.1232(5) 0.5778(4) 0.078(2) Uani 1 1 d . . . C74 C 0.5344(6) 1.1351(6) 0.5050(4) 0.096(3) Uani 1 1 d . . . H74 H 0.5063 1.1855 0.4748 0.115 Uiso 1 1 calc R . . C75 C 0.5855(6) 1.0601(6) 0.4860(3) 0.084(2) Uani 1 1 d . . . C76 C 0.4847(5) 1.1875(5) 0.6225(4) 0.088(2) Uani 1 1 d . . . H76A H 0.4204 1.1990 0.6341 0.131 Uiso 1 1 calc R . . H76B H 0.5020 1.2403 0.5943 0.131 Uiso 1 1 calc R . . H76C H 0.5011 1.1653 0.6685 0.131 Uiso 1 1 calc R . . C77 C 0.6083(6) 1.0351(6) 0.4136(4) 0.120(3) Uani 1 1 d . . . H77A H 0.6730 1.0154 0.3934 0.180 Uiso 1 1 calc R . . H77B H 0.5844 1.0848 0.3777 0.180 Uiso 1 1 calc R . . H77C H 0.5820 0.9894 0.4240 0.180 Uiso 1 1 calc R . . B1 B 0.5592(5) 1.1226(4) 0.8216(4) 0.061(2) Uani 1 1 d . . . B2 B 0.6796(6) 0.9131(7) 0.5480(4) 0.074(2) Uani 1 1 d . . . H30B H 0.559(4) 0.409(4) 1.119(3) 0.071(18) Uiso 1 1 d . . . H30A H 0.545(4) 0.496(4) 1.140(3) 0.055(17) Uiso 1 1 d . . . H2B H 0.699(4) 0.898(4) 0.492(4) 0.11(2) Uiso 1 1 d . . . H1B H 0.536(3) 1.168(3) 0.849(2) 0.041(14) Uiso 1 1 d . . . H2N H 0.735(4) 0.240(4) 1.086(3) 0.08(2) Uiso 1 1 d D . . H1N H 0.957(8) 0.354(6) 1.024(6) 0.24(6) Uiso 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 La1 0.0601(2) 0.0416(2) 0.03417(19) -0.00095(14) -0.02019(16) -0.01220(16) Cr1 0.0426(5) 0.0338(5) 0.0410(5) -0.0031(4) -0.0131(4) -0.0063(4) O1 0.048(2) 0.034(2) 0.047(2) -0.0052(17) -0.0144(19) -0.0053(17) O2 0.053(2) 0.035(2) 0.039(2) -0.0021(17) -0.0157(18) -0.0085(17) O3 0.055(3) 0.045(2) 0.039(2) -0.0053(18) -0.009(2) -0.0079(19) O4 0.057(2) 0.035(2) 0.037(2) -0.0023(17) -0.0159(18) 0.000(2) N1 0.041(3) 0.032(2) 0.040(3) -0.008(2) -0.012(2) 0.001(2) N2 0.045(3) 0.038(3) 0.034(2) -0.002(2) -0.010(2) -0.011(2) N3 0.052(3) 0.036(3) 0.050(3) -0.002(2) -0.018(2) -0.010(2) N4 0.047(3) 0.038(3) 0.061(3) 0.001(2) -0.022(3) -0.009(2) N5 0.048(3) 0.040(3) 0.042(3) -0.004(2) -0.015(2) -0.007(2) N6 0.051(3) 0.042(3) 0.053(3) -0.008(2) -0.022(3) -0.010(2) N7 0.069(3) 0.036(3) 0.055(3) -0.012(2) -0.027(3) -0.008(2) N8 0.074(4) 0.043(3) 0.059(3) -0.007(2) -0.042(3) -0.004(3) N9 0.070(3) 0.039(3) 0.060(3) -0.004(3) -0.030(3) -0.011(3) N10 0.063(3) 0.053(3) 0.055(3) -0.003(3) -0.030(3) -0.016(3) N11 0.054(3) 0.032(3) 0.066(3) 0.000(2) -0.022(3) 0.005(3) N12 0.053(3) 0.039(3) 0.059(3) 0.003(2) -0.030(3) -0.007(2) N13 0.096(4) 0.083(4) 0.034(3) -0.012(3) -0.015(3) -0.044(3) N14 0.077(4) 0.068(3) 0.037(3) -0.004(2) -0.020(3) -0.035(3) N15 0.083(4) 0.102(5) 0.043(3) -0.023(3) 0.006(3) -0.049(4) N16 0.073(4) 0.071(4) 0.053(3) -0.011(3) -0.011(3) -0.025(3) N17 0.097(4) 0.102(5) 0.034(3) 0.014(3) -0.023(3) -0.060(4) N18 0.088(4) 0.074(4) 0.039(3) 0.008(3) -0.029(3) -0.034(3) C1 0.040(3) 0.040(3) 0.045(3) -0.013(3) -0.012(3) -0.004(3) C2 0.045(3) 0.040(3) 0.051(4) -0.016(3) -0.015(3) -0.009(3) C3 0.045(3) 0.037(3) 0.065(4) -0.016(3) -0.017(3) -0.004(3) C4 0.045(4) 0.056(4) 0.066(4) -0.029(3) -0.012(3) 0.007(3) C5 0.056(4) 0.072(5) 0.054(4) -0.023(4) -0.013(3) -0.004(4) C6 0.048(4) 0.054(4) 0.053(4) -0.011(3) -0.013(3) 0.000(3) C7 0.044(4) 0.041(3) 0.073(4) -0.014(3) -0.010(3) 0.000(3) C8 0.085(5) 0.056(4) 0.102(6) 0.008(4) -0.055(5) -0.009(4) C9 0.052(4) 0.049(4) 0.102(5) -0.009(4) -0.016(4) -0.006(3) C10 0.072(5) 0.043(4) 0.119(6) -0.012(4) -0.011(4) 0.007(4) C11 0.061(5) 0.082(5) 0.054(4) -0.015(4) 0.003(4) 0.009(4) C12 0.194(11) 0.147(10) 0.070(6) -0.051(6) 0.022(6) 0.018(8) C13 0.144(9) 0.282(16) 0.042(5) -0.017(7) -0.009(5) 0.050(10) C14 0.223(14) 0.46(3) 0.127(9) -0.143(13) 0.120(10) -0.258(17) C15 0.048(4) 0.039(3) 0.038(3) -0.005(2) -0.011(3) -0.010(3) C16 0.052(4) 0.049(4) 0.036(3) 0.001(3) -0.014(3) -0.016(3) C17 0.047(3) 0.045(3) 0.038(3) -0.003(3) -0.015(3) -0.016(3) C18 0.063(4) 0.039(3) 0.046(3) 0.002(3) -0.026(3) -0.015(3) C19 0.075(4) 0.051(4) 0.047(4) -0.003(3) -0.026(3) -0.013(3) C20 0.083(5) 0.055(4) 0.037(3) -0.001(3) -0.022(3) -0.022(4) C21 0.066(4) 0.045(4) 0.045(4) -0.007(3) -0.011(3) -0.008(3) C22 0.063(4) 0.048(4) 0.044(3) 0.005(3) -0.020(3) -0.011(3) C23 0.068(5) 0.073(5) 0.078(5) 0.006(4) -0.036(4) -0.009(4) C24 0.095(5) 0.062(4) 0.072(4) 0.009(4) -0.049(4) -0.005(4) C25 0.099(5) 0.038(4) 0.062(4) -0.002(3) -0.029(4) -0.009(4) C26 0.104(6) 0.067(5) 0.053(4) -0.019(4) -0.024(4) -0.021(4) C27 0.162(8) 0.101(6) 0.053(4) -0.030(4) -0.044(5) 0.006(6) C28 0.103(7) 0.163(9) 0.072(5) -0.059(6) -0.005(5) -0.029(6) C29 0.193(10) 0.087(6) 0.072(5) -0.035(5) -0.040(6) -0.030(6) C30 0.045(4) 0.042(4) 0.040(3) -0.001(3) -0.009(3) -0.001(3) C31 0.044(3) 0.034(3) 0.043(3) -0.007(3) -0.012(3) -0.005(3) C32 0.041(3) 0.038(3) 0.039(3) -0.008(3) -0.013(3) -0.005(3) C33 0.048(4) 0.040(3) 0.040(3) 0.001(3) -0.008(3) 0.003(3) C34 0.046(4) 0.043(3) 0.046(3) -0.013(3) -0.013(3) 0.009(3) C35 0.045(3) 0.032(3) 0.043(3) -0.006(2) -0.016(3) -0.005(3) C36 0.047(3) 0.040(3) 0.032(3) -0.003(2) -0.008(3) -0.014(3) C37 0.057(4) 0.039(3) 0.032(3) -0.008(3) -0.015(3) -0.010(3) C38 0.057(4) 0.042(4) 0.083(5) -0.002(3) -0.033(4) -0.017(3) C39 0.078(5) 0.050(4) 0.096(5) -0.015(4) -0.045(4) -0.020(4) C40 0.071(5) 0.039(4) 0.075(4) -0.017(3) -0.020(4) -0.012(3) C41 0.079(5) 0.061(4) 0.122(6) -0.007(4) -0.053(5) -0.023(4) C42 0.079(5) 0.077(5) 0.133(7) -0.063(5) -0.034(5) 0.001(4) C43 0.047(4) 0.052(4) 0.065(4) -0.019(3) -0.021(3) -0.008(3) C44 0.074(4) 0.065(4) 0.067(4) -0.020(4) -0.033(4) -0.025(4) C45 0.054(4) 0.060(4) 0.051(4) -0.005(3) -0.023(3) -0.012(3) C46 0.081(5) 0.057(4) 0.098(5) -0.017(4) -0.041(4) -0.019(4) C47 0.121(6) 0.087(5) 0.078(5) 0.020(4) -0.063(5) -0.044(5) C48 0.059(4) 0.051(4) 0.063(4) -0.009(3) -0.034(3) -0.007(3) C49 0.076(5) 0.058(4) 0.054(4) 0.001(3) -0.043(4) -0.012(4) C50 0.073(4) 0.073(5) 0.046(4) -0.019(3) -0.017(3) -0.039(4) C51 0.100(5) 0.053(4) 0.093(5) -0.007(4) -0.067(5) -0.003(4) C52 0.077(5) 0.086(5) 0.063(4) -0.025(4) -0.014(4) -0.030(4) C53 0.067(4) 0.064(5) 0.058(4) 0.007(4) -0.022(4) -0.028(4) C54 0.095(6) 0.056(5) 0.077(5) 0.009(4) -0.035(4) -0.033(4) C55 0.094(5) 0.042(4) 0.080(5) 0.001(4) -0.046(4) -0.017(4) C56 0.100(6) 0.081(5) 0.062(4) 0.008(4) -0.022(4) -0.043(4) C57 0.132(7) 0.050(4) 0.115(6) -0.010(4) -0.047(5) -0.032(5) C58 0.065(5) 0.054(4) 0.071(4) 0.016(3) -0.036(4) -0.019(4) C59 0.056(5) 0.057(5) 0.097(6) 0.012(4) -0.024(4) -0.004(4) C60 0.065(5) 0.043(4) 0.075(5) 0.007(3) -0.013(4) -0.004(4) C61 0.081(5) 0.107(6) 0.096(6) 0.007(5) -0.043(5) -0.038(5) C62 0.089(6) 0.052(5) 0.160(8) -0.028(5) -0.005(6) -0.006(4) C63 0.073(4) 0.072(4) 0.040(3) -0.009(3) -0.018(3) -0.033(4) C64 0.084(5) 0.083(5) 0.061(4) -0.019(4) -0.015(4) -0.040(4) C65 0.092(5) 0.095(6) 0.058(4) -0.038(4) -0.014(4) -0.034(5) C66 0.086(5) 0.080(5) 0.050(4) -0.005(3) -0.014(4) -0.047(4) C67 0.143(8) 0.130(7) 0.081(5) -0.050(5) -0.007(5) -0.066(6) C68 0.077(6) 0.092(6) 0.076(5) -0.017(4) -0.015(5) -0.022(5) C69 0.078(6) 0.160(9) 0.092(6) -0.059(6) 0.026(5) -0.044(6) C70 0.107(7) 0.142(8) 0.076(6) -0.050(6) 0.016(6) -0.070(6) C71 0.088(6) 0.140(8) 0.103(6) -0.047(6) -0.030(5) -0.029(5) C72 0.145(9) 0.260(14) 0.089(6) -0.103(8) 0.042(6) -0.104(9) C73 0.079(5) 0.094(6) 0.053(4) 0.029(4) -0.035(4) -0.046(5) C74 0.125(7) 0.112(7) 0.069(5) 0.031(5) -0.060(5) -0.070(6) C75 0.112(7) 0.127(7) 0.036(4) 0.017(4) -0.032(4) -0.082(6) C76 0.094(6) 0.072(5) 0.074(5) 0.029(4) -0.046(4) -0.023(4) C77 0.190(9) 0.166(9) 0.050(4) 0.021(5) -0.059(5) -0.118(8) B1 0.079(6) 0.034(4) 0.064(5) -0.014(4) -0.027(4) -0.002(4) B2 0.090(7) 0.108(8) 0.039(4) -0.020(5) -0.004(4) -0.057(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O4 2.489(3) . ? La1 O3 2.506(3) . ? La1 N16 2.588(5) . ? La1 N12 2.604(5) . ? La1 N10 2.702(5) . ? La1 N18 2.706(5) . ? La1 N8 2.718(4) . ? La1 N14 2.723(5) . ? La1 C37 2.869(5) . ? Cr1 N2 1.929(4) . ? Cr1 O2 1.942(3) . ? Cr1 O1 1.962(3) . ? Cr1 N1 2.022(4) . ? Cr1 N5 2.112(5) . ? Cr1 N3 2.117(5) . ? O1 C2 1.330(6) . ? O2 C17 1.351(6) . ? O3 C37 1.282(6) . ? O4 C37 1.260(6) . ? N1 C15 1.294(6) . ? N1 C31 1.432(6) . ? N2 C32 1.361(6) . ? N2 C30 1.457(7) . ? N3 C40 1.350(7) . ? N3 N4 1.374(6) . ? N4 C38 1.333(7) . ? N5 C45 1.329(7) . ? N5 N6 1.360(6) . ? N6 C43 1.324(7) . ? N7 C50 1.353(7) . ? N7 N8 1.382(6) . ? N7 B1 1.530(8) . ? N8 C48 1.339(7) . ? N9 C55 1.367(7) . ? N9 N10 1.376(6) . ? N9 B1 1.523(9) . ? N10 C53 1.345(7) . ? N11 C60 1.343(7) . ? N11 N12 1.387(6) . ? N11 B1 1.541(9) . ? N12 C58 1.327(7) . ? N13 C65 1.343(8) . ? N13 N14 1.373(6) . ? N13 B2 1.556(9) . ? N14 C63 1.331(7) . ? N15 C70 1.331(9) . ? N15 N16 1.376(7) . ? N15 B2 1.530(10) . ? N16 C68 1.347(9) . ? N17 C75 1.376(8) . ? N17 N18 1.384(7) . ? N17 B2 1.517(11) . ? N18 C73 1.345(8) . ? C1 C6 1.407(7) . ? C1 C2 1.420(7) . ? C1 C15 1.439(7) . ? C2 C3 1.414(7) . ? C3 C4 1.362(7) . ? C3 C7 1.536(8) . ? C4 C5 1.418(8) . ? C5 C6 1.376(8) . ? C5 C11 1.532(8) . ? C7 C9 1.522(8) . ? C7 C8 1.524(8) . ? C7 C10 1.552(8) . ? C11 C14 1.441(13) . ? C11 C13 1.488(11) . ? C11 C12 1.531(11) . ? C16 C21 1.390(7) . ? C16 C17 1.403(7) . ? C16 C30 1.542(7) . ? C17 C18 1.394(7) . ? C18 C19 1.395(7) . ? C18 C22 1.526(7) . ? C19 C20 1.381(8) . ? C20 C21 1.387(7) . ? C20 C26 1.540(8) . ? C22 C25 1.532(8) . ? C22 C23 1.534(8) . ? C22 C24 1.547(7) . ? C26 C28 1.514(10) . ? C26 C27 1.528(9) . ? C26 C29 1.528(10) . ? C31 C36 1.387(7) . ? C31 C32 1.442(7) . ? C32 C33 1.403(7) . ? C33 C34 1.375(7) . ? C34 C35 1.404(7) . ? C35 C36 1.381(7) . ? C35 C37 1.477(7) . ? C38 C39 1.356(8) . ? C38 C41 1.482(8) . ? C39 C40 1.406(8) . ? C40 C42 1.489(8) . ? C43 C44 1.372(8) . ? C43 C46 1.498(8) . ? C44 C45 1.387(8) . ? C45 C47 1.503(8) . ? C48 C49 1.390(8) . ? C48 C51 1.475(8) . ? C49 C50 1.344(8) . ? C50 C52 1.520(8) . ? C53 C54 1.368(9) . ? C53 C56 1.498(9) . ? C54 C55 1.354(9) . ? C55 C57 1.509(9) . ? C58 C59 1.392(9) . ? C58 C61 1.502(10) . ? C59 C60 1.355(10) . ? C60 C62 1.516(10) . ? C63 C64 1.382(8) . ? C63 C66 1.490(8) . ? C64 C65 1.382(9) . ? C65 C67 1.511(9) . ? C68 C69 1.400(10) . ? C68 C71 1.490(10) . ? C69 C70 1.378(11) . ? C70 C72 1.512(10) . ? C73 C74 1.389(9) . ? C73 C76 1.478(10) . ? C74 C75 1.355(11) . ? C75 C77 1.536(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 La1 O3 52.47(11) . . ? O4 La1 N16 129.08(14) . . ? O3 La1 N16 77.51(14) . . ? O4 La1 N12 77.76(13) . . ? O3 La1 N12 129.79(13) . . ? N16 La1 N12 152.68(15) . . ? O4 La1 N10 135.29(13) . . ? O3 La1 N10 135.98(13) . . ? N16 La1 N10 85.92(16) . . ? N12 La1 N10 74.22(15) . . ? O4 La1 N18 135.92(14) . . ? O3 La1 N18 137.16(15) . . ? N16 La1 N18 74.24(17) . . ? N12 La1 N18 82.03(15) . . ? N10 La1 N18 73.13(15) . . ? O4 La1 N8 74.77(13) . . ? O3 La1 N8 79.62(13) . . ? N16 La1 N8 108.18(17) . . ? N12 La1 N8 81.54(15) . . ? N10 La1 N8 67.25(14) . . ? N18 La1 N8 139.89(15) . . ? O4 La1 N14 78.41(13) . . ? O3 La1 N14 74.89(13) . . ? N16 La1 N14 80.17(16) . . ? N12 La1 N14 104.02(15) . . ? N10 La1 N14 141.99(14) . . ? N18 La1 N14 69.09(15) . . ? N8 La1 N14 150.76(14) . . ? O4 La1 C37 25.97(13) . . ? O3 La1 C37 26.50(13) . . ? N16 La1 C37 103.57(16) . . ? N12 La1 C37 103.57(15) . . ? N10 La1 C37 143.05(14) . . ? N18 La1 C37 143.78(16) . . ? N8 La1 C37 75.90(14) . . ? N14 La1 C37 74.89(14) . . ? N2 Cr1 O2 93.09(16) . . ? N2 Cr1 O1 172.45(16) . . ? O2 Cr1 O1 94.45(14) . . ? N2 Cr1 N1 82.28(16) . . ? O2 Cr1 N1 175.13(16) . . ? O1 Cr1 N1 90.17(15) . . ? N2 Cr1 N5 92.16(17) . . ? O2 Cr1 N5 85.03(16) . . ? O1 Cr1 N5 88.00(15) . . ? N1 Cr1 N5 93.62(17) . . ? N2 Cr1 N3 93.89(18) . . ? O2 Cr1 N3 91.64(15) . . ? O1 Cr1 N3 86.40(16) . . ? N1 Cr1 N3 90.17(17) . . ? N5 Cr1 N3 173.25(17) . . ? C2 O1 Cr1 129.9(3) . . ? C17 O2 Cr1 122.7(3) . . ? C37 O3 La1 92.8(3) . . ? C37 O4 La1 94.1(3) . . ? C15 N1 C31 123.3(4) . . ? C15 N1 Cr1 125.0(3) . . ? C31 N1 Cr1 111.6(3) . . ? C32 N2 C30 121.7(4) . . ? C32 N2 Cr1 116.8(3) . . ? C30 N2 Cr1 120.5(3) . . ? C40 N3 N4 104.4(5) . . ? C40 N3 Cr1 141.8(4) . . ? N4 N3 Cr1 113.6(4) . . ? C38 N4 N3 112.5(5) . . ? C45 N5 N6 104.8(5) . . ? C45 N5 Cr1 143.1(4) . . ? N6 N5 Cr1 110.8(3) . . ? C43 N6 N5 112.6(5) . . ? C50 N7 N8 108.4(5) . . ? C50 N7 B1 127.4(5) . . ? N8 N7 B1 123.7(5) . . ? C48 N8 N7 106.4(4) . . ? C48 N8 La1 133.8(4) . . ? N7 N8 La1 112.1(3) . . ? C55 N9 N10 109.2(5) . . ? C55 N9 B1 127.0(6) . . ? N10 N9 B1 123.6(5) . . ? C53 N10 N9 106.7(5) . . ? C53 N10 La1 135.2(4) . . ? N9 N10 La1 117.5(3) . . ? C60 N11 N12 109.8(6) . . ? C60 N11 B1 128.3(6) . . ? N12 N11 B1 121.5(5) . . ? C58 N12 N11 105.2(5) . . ? C58 N12 La1 133.9(5) . . ? N11 N12 La1 120.8(3) . . ? C65 N13 N14 109.9(5) . . ? C65 N13 B2 126.0(6) . . ? N14 N13 B2 123.2(5) . . ? C63 N14 N13 106.4(5) . . ? C63 N14 La1 135.2(4) . . ? N13 N14 La1 113.5(4) . . ? C70 N15 N16 109.7(6) . . ? C70 N15 B2 127.7(7) . . ? N16 N15 B2 122.5(6) . . ? C68 N16 N15 107.6(6) . . ? C68 N16 La1 131.1(5) . . ? N15 N16 La1 121.0(4) . . ? C75 N17 N18 107.7(7) . . ? C75 N17 B2 127.8(7) . . ? N18 N17 B2 124.4(5) . . ? C73 N18 N17 107.2(5) . . ? C73 N18 La1 135.9(5) . . ? N17 N18 La1 116.9(4) . . ? C6 C1 C2 119.4(5) . . ? C6 C1 C15 116.2(5) . . ? C2 C1 C15 124.4(5) . . ? O1 C2 C3 119.6(5) . . ? O1 C2 C1 120.9(4) . . ? C3 C2 C1 119.4(5) . . ? C4 C3 C2 117.9(5) . . ? C4 C3 C7 120.6(5) . . ? C2 C3 C7 121.5(5) . . ? C3 C4 C5 125.1(5) . . ? C6 C5 C4 115.9(5) . . ? C6 C5 C11 122.1(6) . . ? C4 C5 C11 122.0(5) . . ? C5 C6 C1 122.3(5) . . ? C9 C7 C8 110.2(5) . . ? C9 C7 C3 111.1(5) . . ? C8 C7 C3 109.4(5) . . ? C9 C7 C10 105.8(5) . . ? C8 C7 C10 108.2(5) . . ? C3 C7 C10 112.0(5) . . ? C14 C11 C13 116.2(10) . . ? C14 C11 C12 105.7(9) . . ? C13 C11 C12 104.8(8) . . ? C14 C11 C5 108.9(7) . . ? C13 C11 C5 109.9(6) . . ? C12 C11 C5 111.2(6) . . ? N1 C15 C1 127.1(5) . . ? C21 C16 C17 119.8(5) . . ? C21 C16 C30 118.7(5) . . ? C17 C16 C30 121.4(5) . . ? O2 C17 C18 120.7(5) . . ? O2 C17 C16 119.3(4) . . ? C18 C17 C16 120.0(5) . . ? C17 C18 C19 117.2(5) . . ? C17 C18 C22 122.3(5) . . ? C19 C18 C22 120.5(5) . . ? C20 C19 C18 124.3(5) . . ? C19 C20 C21 116.8(5) . . ? C19 C20 C26 123.8(5) . . ? C21 C20 C26 119.4(6) . . ? C20 C21 C16 121.5(6) . . ? C18 C22 C25 110.1(5) . . ? C18 C22 C23 110.0(5) . . ? C25 C22 C23 110.2(5) . . ? C18 C22 C24 113.4(5) . . ? C25 C22 C24 106.6(5) . . ? C23 C22 C24 106.4(5) . . ? C28 C26 C27 108.2(7) . . ? C28 C26 C29 110.5(7) . . ? C27 C26 C29 107.0(6) . . ? C28 C26 C20 110.6(6) . . ? C27 C26 C20 111.8(6) . . ? C29 C26 C20 108.7(6) . . ? N2 C30 C16 112.1(5) . . ? C36 C31 N1 126.1(5) . . ? C36 C31 C32 120.4(5) . . ? N1 C31 C32 113.6(4) . . ? N2 C32 C33 127.9(5) . . ? N2 C32 C31 115.2(4) . . ? C33 C32 C31 116.9(5) . . ? C34 C33 C32 121.0(5) . . ? C33 C34 C35 121.9(5) . . ? C36 C35 C34 118.1(5) . . ? C36 C35 C37 121.7(5) . . ? C34 C35 C37 120.2(5) . . ? C35 C36 C31 121.4(5) . . ? O4 C37 O3 120.6(5) . . ? O4 C37 C35 120.6(5) . . ? O3 C37 C35 118.8(5) . . ? O4 C37 La1 59.9(3) . . ? O3 C37 La1 60.7(3) . . ? C35 C37 La1 179.5(5) . . ? N4 C38 C39 106.6(5) . . ? N4 C38 C41 121.0(6) . . ? C39 C38 C41 132.3(6) . . ? C38 C39 C40 107.1(6) . . ? N3 C40 C39 109.3(5) . . ? N3 C40 C42 123.1(6) . . ? C39 C40 C42 127.5(6) . . ? N6 C43 C44 106.0(5) . . ? N6 C43 C46 121.3(5) . . ? C44 C43 C46 132.7(6) . . ? C43 C44 C45 106.5(5) . . ? N5 C45 C44 110.1(5) . . ? N5 C45 C47 122.2(6) . . ? C44 C45 C47 127.7(6) . . ? N8 C48 C49 109.8(5) . . ? N8 C48 C51 123.8(6) . . ? C49 C48 C51 126.3(5) . . ? C50 C49 C48 106.1(5) . . ? C49 C50 N7 109.3(5) . . ? C49 C50 C52 129.4(6) . . ? N7 C50 C52 121.2(6) . . ? N10 C53 C54 108.7(6) . . ? N10 C53 C56 123.1(6) . . ? C54 C53 C56 128.2(6) . . ? C55 C54 C53 108.8(6) . . ? C54 C55 N9 106.5(6) . . ? C54 C55 C57 130.1(7) . . ? N9 C55 C57 123.4(7) . . ? N12 C58 C59 110.9(7) . . ? N12 C58 C61 119.3(7) . . ? C59 C58 C61 129.6(7) . . ? C60 C59 C58 105.7(7) . . ? N11 C60 C59 108.4(7) . . ? N11 C60 C62 124.4(8) . . ? C59 C60 C62 127.2(7) . . ? N14 C63 C64 110.3(5) . . ? N14 C63 C66 124.9(6) . . ? C64 C63 C66 124.7(6) . . ? C63 C64 C65 105.9(6) . . ? N13 C65 C64 107.5(6) . . ? N13 C65 C67 123.1(7) . . ? C64 C65 C67 129.4(7) . . ? N16 C68 C69 107.9(7) . . ? N16 C68 C71 122.1(7) . . ? C69 C68 C71 130.0(8) . . ? C70 C69 C68 106.8(7) . . ? N15 C70 C69 108.1(7) . . ? N15 C70 C72 124.8(9) . . ? C69 C70 C72 127.1(8) . . ? N18 C73 C74 109.6(8) . . ? N18 C73 C76 123.8(6) . . ? C74 C73 C76 126.6(7) . . ? C75 C74 C73 106.7(7) . . ? C74 C75 N17 108.8(7) . . ? C74 C75 C77 129.5(7) . . ? N17 C75 C77 121.7(9) . . ? N9 B1 N7 112.3(5) . . ? N9 B1 N11 111.4(5) . . ? N7 B1 N11 111.8(5) . . ? N17 B2 N15 111.2(6) . . ? N17 B2 N13 111.5(6) . . ? N15 B2 N13 112.2(6) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.766 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.071 data_x0032fin _database_code_depnum_ccdc_archive 'CCDC 736176' _audit_creation_date 2006-09-25T16:08:47-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C46 H62 Cl Cr N4 O6' _chemical_formula_weight 854.45 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5249(16) _cell_length_b 15.812(3) _cell_length_c 17.539(3) _cell_angle_alpha 66.033(17) _cell_angle_beta 79.982(16) _cell_angle_gamma 76.191(17) _cell_volume 2335.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 21677 _cell_measurement_theta_min 2.5453 _cell_measurement_theta_max 31.9173 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'red brown' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 910 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.351 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET) (compiled Jun 12 2006,17:01:16) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.94822 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 0.0727249664 _diffrn_orient_matrix_ub_12 0.0067008889 _diffrn_orient_matrix_ub_13 -0.0123576283 _diffrn_orient_matrix_ub_21 0.0177011747 _diffrn_orient_matrix_ub_22 -0.02615745 _diffrn_orient_matrix_ub_23 0.0418023952 _diffrn_orient_matrix_ub_31 0.0176503517 _diffrn_orient_matrix_ub_32 -0.041890752 _diffrn_orient_matrix_ub_33 -0.0079529909 _diffrn_measurement_device_type 'ccd Xcalibur S' _diffrn_measurement_method ' \w-scans' _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_unetI/netI 0.0548 _diffrn_reflns_number 68185 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 30.51 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 14196 _reflns_number_gt 9690 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET) (compiled Jun 12 2006,17:01:16) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET) (compiled Jun 12 2006,17:01:16) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET) (compiled Jun 12 2006,17:01:16) ; _computing_structure_solution ; SHELXS-97 Program for Crystal Structure Analysis (Release 97-2) G. M. Sheldrick, Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998. ; _computing_structure_refinement ; SHELXL-97 G. M. Sheldrick, 2008, Acta Cryst., A64, 112-122 ; _computing_molecular_graphics ; ORTEP3 for Windows L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565. ; _computing_publication_material ; WINGX L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838. ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0722P)^2^+0.3478P] 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_number_reflns 14196 _refine_ls_number_parameters 545 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1392 _refine_ls_wR_factor_gt 0.1218 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.656 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.063 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cr Cr 0.3209 0.6236 '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' O O 0.0106 0.006 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cr1 Cr 0.84119(3) 0.410846(18) 0.711403(16) 0.01612(8) Uani 1 1 d . . . Cl1 Cl 1.07250(5) 0.44475(3) 0.69082(3) 0.02300(10) Uani 1 1 d . . . O1 O 0.91563(14) 0.29529(8) 0.69475(7) 0.0218(3) Uani 1 1 d . . . O2 O 0.85411(14) 0.35065(8) 0.83036(7) 0.0205(3) Uani 1 1 d . . . O3 O 0.53389(19) 0.89262(10) 0.58835(9) 0.0355(4) Uani 1 1 d . . . O4 O 0.5698(2) 0.92602(10) 0.45082(9) 0.0431(4) Uani 1 1 d . . . N1 N 0.81388(16) 0.48365(10) 0.59008(9) 0.0177(3) Uani 1 1 d . . . N2 N 0.75313(16) 0.53708(10) 0.71723(8) 0.0173(3) Uani 1 1 d . . . N3 N 0.63368(17) 0.37222(11) 0.73741(9) 0.0225(3) Uani 1 1 d . . . N4 N 0.6327(2) 0.28896(12) 0.80385(11) 0.0289(4) Uani 1 1 d . . . C1 C 0.8927(2) 0.34951(12) 0.54757(11) 0.0199(3) Uani 1 1 d . . . C2 C 0.9284(2) 0.27796(12) 0.62693(11) 0.0201(3) Uani 1 1 d . . . C3 C 0.9812(2) 0.18353(12) 0.63174(12) 0.0251(4) Uani 1 1 d . . . C4 C 0.9842(2) 0.16603(13) 0.56004(12) 0.0284(4) Uani 1 1 d . . . H4 H 1.0153 0.1027 0.5641 0.034 Uiso 1 1 calc R . . C5 C 0.9447(2) 0.23509(13) 0.48148(12) 0.0257(4) Uani 1 1 d . . . C6 C 0.9027(2) 0.32573(13) 0.47683(12) 0.0240(4) Uani 1 1 d . . . H6 H 0.8793 0.3745 0.4244 0.029 Uiso 1 1 calc R . . C7 C 1.0263(3) 0.10487(13) 0.71445(12) 0.0332(5) Uani 1 1 d . . . C8 C 0.8925(3) 0.09188(15) 0.77790(15) 0.0495(7) Uani 1 1 d . . . H8A H 0.8497 0.1516 0.7846 0.074 Uiso 1 1 calc R . . H8B H 0.9213 0.0435 0.832 0.074 Uiso 1 1 calc R . . H8C H 0.8211 0.0722 0.7577 0.074 Uiso 1 1 calc R . . C9 C 1.1437(3) 0.12720(15) 0.74886(14) 0.0432(6) Uani 1 1 d . . . H9A H 1.2341 0.1252 0.7126 0.065 Uiso 1 1 calc R . . H9B H 1.1598 0.0806 0.8056 0.065 Uiso 1 1 calc R . . H9C H 1.1125 0.1902 0.7505 0.065 Uiso 1 1 calc R . . C10 C 1.0876(3) 0.01069(14) 0.70442(14) 0.0472(7) Uani 1 1 d . . . H10A H 1.0119 -0.0091 0.6877 0.071 Uiso 1 1 calc R . . H10B H 1.1205 -0.0371 0.7578 0.071 Uiso 1 1 calc R . . H10C H 1.1697 0.0181 0.6614 0.071 Uiso 1 1 calc R . . C11 C 0.9394(2) 0.20668(14) 0.40848(13) 0.0311(4) Uani 1 1 d . . . C12 C 1.0717(3) 0.13265(16) 0.40136(15) 0.0407(5) Uani 1 1 d . . . H12A H 1.1602 0.158 0.3925 0.061 Uiso 1 1 calc R . . H12B H 1.0656 0.1163 0.354 0.061 Uiso 1 1 calc R . . H12C H 1.0743 0.0762 0.4531 0.061 Uiso 1 1 calc R . . C13 C 0.8037(3) 0.1650(2) 0.4243(2) 0.0601(8) Uani 1 1 d . . . H13A H 0.8064 0.1107 0.4777 0.09 Uiso 1 1 calc R . . H13B H 0.7998 0.1448 0.3789 0.09 Uiso 1 1 calc R . . H13C H 0.7176 0.2127 0.4265 0.09 Uiso 1 1 calc R . . C14 C 0.9367(4) 0.29104(18) 0.32485(15) 0.0559(8) Uani 1 1 d . . . H14A H 0.8486 0.3379 0.3255 0.084 Uiso 1 1 calc R . . H14B H 0.9378 0.27 0.2793 0.084 Uiso 1 1 calc R . . H14C H 1.0222 0.3193 0.3162 0.084 Uiso 1 1 calc R . . C15 C 0.8427(2) 0.44626(12) 0.53335(11) 0.0194(3) Uani 1 1 d . . . H15 H 0.8288 0.4882 0.4771 0.023 Uiso 1 1 calc R . . C16 C 0.76421(19) 0.48544(12) 0.86781(10) 0.0187(3) Uani 1 1 d . . . C17 C 0.82880(19) 0.38890(12) 0.88636(10) 0.0187(3) Uani 1 1 d . . . C18 C 0.8669(2) 0.33164(13) 0.96960(11) 0.0226(4) Uani 1 1 d . . . C19 C 0.8276(2) 0.37053(13) 1.02961(11) 0.0239(4) Uani 1 1 d . . . H19 H 0.8506 0.3314 1.0852 0.029 Uiso 1 1 calc R . . C20 C 0.7559(2) 0.46399(13) 1.01444(11) 0.0218(4) Uani 1 1 d . . . C21 C 0.7283(2) 0.51974(13) 0.93319(11) 0.0214(4) Uani 1 1 d . . . H21 H 0.6835 0.5839 0.9202 0.026 Uiso 1 1 calc R . . C22 C 0.9530(2) 0.23101(13) 0.99017(12) 0.0296(4) Uani 1 1 d . . . C23 C 1.0988(3) 0.23256(16) 0.93637(14) 0.0382(5) Uani 1 1 d . . . H23A H 1.0812 0.262 0.8769 0.057 Uiso 1 1 calc R . . H23B H 1.1524 0.1679 0.949 0.057 Uiso 1 1 calc R . . H23C H 1.1559 0.2687 0.9488 0.057 Uiso 1 1 calc R . . C24 C 0.8689(3) 0.16840(15) 0.97460(16) 0.0444(6) Uani 1 1 d . . . H24A H 0.7693 0.1761 1.0004 0.067 Uiso 1 1 calc R . . H24B H 0.9168 0.1023 0.9993 0.067 Uiso 1 1 calc R . . H24C H 0.8672 0.1869 0.9142 0.067 Uiso 1 1 calc R . . C25 C 0.9869(3) 0.18468(17) 1.08185(14) 0.0506(7) Uani 1 1 d . . . H25A H 1.0401 0.2233 1.0937 0.076 Uiso 1 1 calc R . . H25B H 1.0462 0.1218 1.0925 0.076 Uiso 1 1 calc R . . H25C H 0.896 0.1792 1.1181 0.076 Uiso 1 1 calc R . . C26 C 0.7194(2) 0.49853(14) 1.08673(11) 0.0262(4) Uani 1 1 d . . . C27 C 0.8610(2) 0.50401(17) 1.11365(14) 0.0355(5) Uani 1 1 d . . . H27A H 0.9236 0.4416 1.1312 0.053 Uiso 1 1 calc R . . H27B H 0.8387 0.5251 1.1605 0.053 Uiso 1 1 calc R . . H27C H 0.911 0.5488 1.0665 0.053 Uiso 1 1 calc R . . C28 C 0.6405(2) 0.42969(16) 1.16146(12) 0.0336(5) Uani 1 1 d . . . H28A H 0.5533 0.4227 1.1437 0.05 Uiso 1 1 calc R . . H28B H 0.6127 0.4542 1.2062 0.05 Uiso 1 1 calc R . . H28C H 0.705 0.3682 1.1822 0.05 Uiso 1 1 calc R . . C29 C 0.6196(3) 0.59510(16) 1.06185(14) 0.0391(5) Uani 1 1 d . . . H29A H 0.6706 0.6421 1.0178 0.059 Uiso 1 1 calc R . . H29B H 0.592 0.6125 1.1108 0.059 Uiso 1 1 calc R . . H29C H 0.5323 0.5926 1.041 0.059 Uiso 1 1 calc R . . C30 C 0.73227(19) 0.55289(12) 0.78600(11) 0.0188(3) Uani 1 1 d . . . H30 H 0.6917 0.6156 0.7813 0.023 Uiso 1 1 calc R . . C31 C 0.76111(19) 0.58090(11) 0.56908(10) 0.0174(3) Uani 1 1 d . . . C32 C 0.72271(19) 0.60959(11) 0.63778(10) 0.0176(3) Uani 1 1 d . . . C33 C 0.6607(2) 0.70326(12) 0.62381(11) 0.0205(3) Uani 1 1 d . . . H33 H 0.6327 0.7229 0.6697 0.025 Uiso 1 1 calc R . . C34 C 0.6398(2) 0.76797(12) 0.54253(11) 0.0225(4) Uani 1 1 d . . . C35 C 0.6817(2) 0.73923(13) 0.47497(11) 0.0267(4) Uani 1 1 d . . . H35 H 0.6693 0.784 0.4195 0.032 Uiso 1 1 calc R . . C36 C 0.7405(2) 0.64699(12) 0.48815(11) 0.0238(4) Uani 1 1 d . . . H36 H 0.7673 0.628 0.4419 0.029 Uiso 1 1 calc R . . C37 C 0.5773(2) 0.86889(13) 0.52524(12) 0.0262(4) Uani 1 1 d . . . C38 C 0.5107(2) 0.38841(15) 0.70302(13) 0.0302(4) Uani 1 1 d . . . C39 C 0.4337(2) 0.31530(16) 0.74787(15) 0.0379(5) Uani 1 1 d . . . H39 H 0.343 0.3103 0.7362 0.045 Uiso 1 1 calc R . . C40 C 0.5147(2) 0.25265(15) 0.81162(15) 0.0357(5) Uani 1 1 d . . . C41 C 0.4667(3) 0.47403(19) 0.62816(16) 0.0480(6) Uani 1 1 d . . . H41A H 0.4934 0.5284 0.6316 0.072 Uiso 1 1 calc R . . H41B H 0.3614 0.4853 0.626 0.072 Uiso 1 1 calc R . . H41C H 0.5161 0.4648 0.5775 0.072 Uiso 1 1 calc R . . C42 C 0.4931(3) 0.16129(18) 0.8807(2) 0.0631(9) Uani 1 1 d . . . H42A H 0.5852 0.1162 0.8877 0.095 Uiso 1 1 calc R . . H42B H 0.4206 0.1362 0.8668 0.095 Uiso 1 1 calc R . . H42C H 0.4594 0.1714 0.9329 0.095 Uiso 1 1 calc R . . H1N H 0.692(3) 0.2733(16) 0.8350(14) 0.029(6) Uiso 1 1 d . . . H1O H 0.487(5) 0.954(3) 0.581(3) 0.136(17) Uiso 1 1 d . . . O5 O 0.4064(3) 0.23524(17) 1.19662(17) 0.0800(7) Uani 1 1 d . . . O6 O 0.4536(4) 0.0704(2) 1.1670(2) 0.1157(11) Uani 1 1 d . . . C43 C 0.5399(4) 0.1995(3) 1.1635(4) 0.1093(17) Uani 1 1 d . . . H43A H 0.618 0.2118 1.186 0.131 Uiso 1 1 calc R . . H43B H 0.5477 0.2339 1.102 0.131 Uiso 1 1 calc R . . C44 C 0.5629(5) 0.1019(3) 1.1811(4) 0.138(2) Uani 1 1 d . . . H44A H 0.6514 0.0857 1.147 0.165 Uiso 1 1 calc R . . H44B H 0.5824 0.0673 1.2407 0.165 Uiso 1 1 calc R . . C45 C 0.3195(5) 0.1066(3) 1.2086(4) 0.1183(19) Uani 1 1 d . . . H45A H 0.2365 0.0878 1.1966 0.142 Uiso 1 1 calc R . . H45B H 0.3259 0.078 1.2699 0.142 Uiso 1 1 calc R . . C46 C 0.2946(4) 0.2046(3) 1.1821(3) 0.0912(12) Uani 1 1 d . . . H46A H 0.2817 0.2333 1.1214 0.109 Uiso 1 1 calc R . . H46B H 0.2038 0.2257 1.2119 0.109 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.02062(14) 0.01135(12) 0.01470(13) -0.00439(10) -0.00171(10) -0.00084(10) Cl1 0.0216(2) 0.0229(2) 0.0220(2) -0.00591(17) -0.00272(16) -0.00372(17) O1 0.0322(7) 0.0136(6) 0.0172(6) -0.0057(5) -0.0019(5) -0.0001(5) O2 0.0265(7) 0.0154(6) 0.0169(6) -0.0055(5) -0.0018(5) -0.0002(5) O3 0.0539(10) 0.0183(7) 0.0301(8) -0.0113(6) -0.0089(7) 0.0087(7) O4 0.0691(12) 0.0171(7) 0.0264(8) -0.0007(6) -0.0042(7) 0.0086(7) N1 0.0216(7) 0.0125(6) 0.0174(7) -0.0050(5) -0.0029(5) -0.0006(5) N2 0.0209(7) 0.0131(6) 0.0156(7) -0.0039(5) -0.0035(5) -0.0004(5) N3 0.0233(8) 0.0191(7) 0.0231(8) -0.0066(6) -0.0011(6) -0.0039(6) N4 0.0258(9) 0.0223(8) 0.0326(9) -0.0048(7) -0.0009(7) -0.0050(7) C1 0.0238(9) 0.0162(8) 0.0203(8) -0.0081(7) -0.0012(7) -0.0031(7) C2 0.0237(9) 0.0143(8) 0.0220(8) -0.0073(7) 0.0012(7) -0.0046(7) C3 0.0353(11) 0.0138(8) 0.0246(9) -0.0079(7) 0.0016(8) -0.0038(7) C4 0.0405(12) 0.0151(8) 0.0302(10) -0.0110(7) -0.0003(8) -0.0041(8) C5 0.0318(10) 0.0217(9) 0.0275(9) -0.0142(8) -0.0014(8) -0.0042(8) C6 0.0302(10) 0.0202(8) 0.0225(9) -0.0093(7) -0.0047(7) -0.0021(7) C7 0.0555(14) 0.0137(8) 0.0230(9) -0.0054(7) 0.0018(9) 0.0007(9) C8 0.0787(19) 0.0207(10) 0.0372(12) -0.0079(9) 0.0186(12) -0.0107(11) C9 0.0622(16) 0.0269(11) 0.0295(11) -0.0062(9) -0.0150(11) 0.0112(11) C10 0.083(2) 0.0155(9) 0.0320(12) -0.0076(9) -0.0001(12) 0.0057(11) C11 0.0397(12) 0.0271(10) 0.0339(11) -0.0197(9) -0.0050(9) -0.0040(9) C12 0.0530(15) 0.0379(12) 0.0388(12) -0.0264(10) -0.0064(10) 0.0006(11) C13 0.0487(16) 0.085(2) 0.080(2) -0.0633(19) 0.0021(14) -0.0219(16) C14 0.102(2) 0.0367(13) 0.0346(13) -0.0210(11) -0.0230(14) 0.0028(14) C15 0.0243(9) 0.0167(8) 0.0164(8) -0.0062(6) -0.0021(6) -0.0022(7) C16 0.0190(8) 0.0186(8) 0.0178(8) -0.0072(6) -0.0016(6) -0.0020(7) C17 0.0192(8) 0.0185(8) 0.0164(8) -0.0051(6) -0.0003(6) -0.0036(7) C18 0.0249(9) 0.0208(8) 0.0172(8) -0.0028(7) -0.0017(7) -0.0035(7) C19 0.0273(10) 0.0246(9) 0.0151(8) -0.0027(7) -0.0017(7) -0.0051(8) C20 0.0208(9) 0.0256(9) 0.0198(8) -0.0098(7) -0.0012(7) -0.0039(7) C21 0.0228(9) 0.0208(8) 0.0205(8) -0.0084(7) -0.0033(7) -0.0020(7) C22 0.0418(12) 0.0178(9) 0.0212(9) -0.0012(7) -0.0066(8) 0.0006(8) C23 0.0368(12) 0.0282(11) 0.0405(12) -0.0097(9) -0.0078(9) 0.0077(9) C24 0.0646(17) 0.0192(10) 0.0447(13) -0.0063(9) -0.0080(12) -0.0076(10) C25 0.079(2) 0.0286(11) 0.0276(11) -0.0001(9) -0.0186(12) 0.0104(12) C26 0.0279(10) 0.0338(10) 0.0182(8) -0.0120(8) 0.0003(7) -0.0061(8) C27 0.0372(12) 0.0473(13) 0.0308(11) -0.0203(10) -0.0005(9) -0.0156(10) C28 0.0313(11) 0.0459(12) 0.0235(10) -0.0151(9) 0.0053(8) -0.0093(10) C29 0.0519(14) 0.0388(12) 0.0282(11) -0.0215(10) -0.0028(10) 0.0037(11) C30 0.0216(9) 0.0145(7) 0.0196(8) -0.0070(6) -0.0029(6) -0.0004(6) C31 0.0194(8) 0.0129(7) 0.0181(8) -0.0053(6) -0.0018(6) -0.0005(6) C32 0.0203(8) 0.0142(7) 0.0167(8) -0.0047(6) -0.0030(6) -0.0014(6) C33 0.0255(9) 0.0151(8) 0.0196(8) -0.0065(6) -0.0042(7) 0.0002(7) C34 0.0295(10) 0.0121(7) 0.0225(9) -0.0048(7) -0.0052(7) 0.0015(7) C35 0.0383(11) 0.0179(8) 0.0177(8) -0.0027(7) -0.0046(7) 0.0005(8) C36 0.0347(10) 0.0167(8) 0.0177(8) -0.0061(7) -0.0035(7) -0.0002(7) C37 0.0347(11) 0.0157(8) 0.0235(9) -0.0055(7) -0.0061(8) 0.0028(7) C38 0.0240(10) 0.0317(10) 0.0351(11) -0.0135(9) -0.0022(8) -0.0042(8) C39 0.0258(11) 0.0395(12) 0.0526(14) -0.0192(11) -0.0015(9) -0.0121(9) C40 0.0247(10) 0.0281(10) 0.0506(13) -0.0140(10) 0.0081(9) -0.0083(8) C41 0.0280(12) 0.0612(16) 0.0415(13) -0.0011(12) -0.0122(10) -0.0112(11) C42 0.0405(15) 0.0330(13) 0.091(2) 0.0007(14) 0.0066(14) -0.0156(12) O5 0.0701(16) 0.0709(15) 0.114(2) -0.0541(15) -0.0270(14) 0.0081(13) O6 0.138(3) 0.0754(18) 0.162(3) -0.074(2) -0.033(2) -0.005(2) C43 0.048(2) 0.065(2) 0.218(6) -0.063(3) 0.000(3) -0.0085(18) C44 0.069(3) 0.094(3) 0.270(8) -0.108(4) -0.007(4) 0.012(3) C45 0.076(3) 0.064(3) 0.203(6) -0.032(3) -0.020(3) -0.021(2) C46 0.071(3) 0.104(3) 0.120(3) -0.063(3) 0.013(2) -0.034(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Cr1 O1 1.9157(13) . ? Cr1 O2 1.9220(13) . ? Cr1 N1 1.9951(15) . ? Cr1 N2 2.0088(14) . ? Cr1 N3 2.1270(16) . ? Cr1 Cl1 2.3242(7) . ? O1 C2 1.305(2) . ? O2 C17 1.311(2) . ? O3 C37 1.281(2) . ? O4 C37 1.252(2) . ? N1 C15 1.312(2) . ? N1 C31 1.410(2) . ? N2 C30 1.302(2) . ? N2 C32 1.423(2) . ? N3 C38 1.333(3) . ? N3 N4 1.359(2) . ? N4 C40 1.342(3) . ? C1 C6 1.418(2) . ? C1 C15 1.419(2) . ? C1 C2 1.426(2) . ? C2 C3 1.429(2) . ? C3 C4 1.388(3) . ? C3 C7 1.527(3) . ? C4 C5 1.412(3) . ? C5 C6 1.365(3) . ? C5 C11 1.531(3) . ? C7 C9 1.528(3) . ? C7 C8 1.533(3) . ? C7 C10 1.534(3) . ? C11 C13 1.521(3) . ? C11 C12 1.528(3) . ? C11 C14 1.529(3) . ? C16 C21 1.416(2) . ? C16 C17 1.426(2) . ? C16 C30 1.429(2) . ? C17 C18 1.427(2) . ? C18 C19 1.380(3) . ? C18 C22 1.532(3) . ? C19 C20 1.408(3) . ? C20 C21 1.370(2) . ? C20 C26 1.532(2) . ? C22 C25 1.529(3) . ? C22 C23 1.537(3) . ? C22 C24 1.539(3) . ? C26 C29 1.528(3) . ? C26 C28 1.535(3) . ? C26 C27 1.536(3) . ? C31 C36 1.393(2) . ? C31 C32 1.415(2) . ? C32 C33 1.393(2) . ? C33 C34 1.391(2) . ? C34 C35 1.399(3) . ? C34 C37 1.486(2) . ? C35 C36 1.369(2) . ? C38 C39 1.400(3) . ? C38 C41 1.486(3) . ? C39 C40 1.364(3) . ? C40 C42 1.493(3) . ? O5 C46 1.370(4) . ? O5 C43 1.393(4) . ? O6 C44 1.353(5) . ? O6 C45 1.469(6) . ? C43 C44 1.414(5) . ? C45 C46 1.396(5) . ? 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 Cr1 O2 92.84(5) . . ? O1 Cr1 N1 92.47(6) . . ? O2 Cr1 N1 174.36(5) . . ? O1 Cr1 N2 173.81(6) . . ? O2 Cr1 N2 92.83(6) . . ? N1 Cr1 N2 81.78(6) . . ? O1 Cr1 N3 86.75(6) . . ? O2 Cr1 N3 85.52(6) . . ? N1 Cr1 N3 92.87(6) . . ? N2 Cr1 N3 91.22(6) . . ? O1 Cr1 Cl1 91.73(5) . . ? O2 Cr1 Cl1 91.17(5) . . ? N1 Cr1 Cl1 90.58(5) . . ? N2 Cr1 Cl1 90.63(5) . . ? N3 Cr1 Cl1 176.28(4) . . ? C2 O1 Cr1 129.71(11) . . ? C17 O2 Cr1 128.91(11) . . ? C15 N1 C31 121.73(15) . . ? C15 N1 Cr1 124.08(12) . . ? C31 N1 Cr1 114.18(11) . . ? C30 N2 C32 122.71(14) . . ? C30 N2 Cr1 123.75(12) . . ? C32 N2 Cr1 113.45(11) . . ? C38 N3 N4 104.51(17) . . ? C38 N3 Cr1 142.31(14) . . ? N4 N3 Cr1 111.15(12) . . ? C40 N4 N3 112.81(18) . . ? C6 C1 C15 115.56(16) . . ? C6 C1 C2 120.23(16) . . ? C15 C1 C2 124.20(16) . . ? O1 C2 C1 122.80(15) . . ? O1 C2 C3 118.96(16) . . ? C1 C2 C3 118.24(16) . . ? C4 C3 C2 117.68(17) . . ? C4 C3 C7 121.89(16) . . ? C2 C3 C7 120.38(16) . . ? C3 C4 C5 125.03(17) . . ? C6 C5 C4 116.42(17) . . ? C6 C5 C11 122.86(18) . . ? C4 C5 C11 120.56(17) . . ? C5 C6 C1 122.22(17) . . ? C3 C7 C9 111.40(17) . . ? C3 C7 C8 108.88(19) . . ? C9 C7 C8 109.9(2) . . ? C3 C7 C10 111.74(17) . . ? C9 C7 C10 107.1(2) . . ? C8 C7 C10 107.73(18) . . ? C13 C11 C12 108.54(19) . . ? C13 C11 C14 109.9(2) . . ? C12 C11 C14 107.2(2) . . ? C13 C11 C5 108.28(18) . . ? C12 C11 C5 111.36(18) . . ? C14 C11 C5 111.52(17) . . ? N1 C15 C1 126.53(16) . . ? C21 C16 C17 119.58(15) . . ? C21 C16 C30 115.90(15) . . ? C17 C16 C30 124.51(15) . . ? O2 C17 C16 122.82(15) . . ? O2 C17 C18 118.81(15) . . ? C16 C17 C18 118.37(16) . . ? C19 C18 C17 118.08(17) . . ? C19 C18 C22 121.56(16) . . ? C17 C18 C22 120.33(16) . . ? C18 C19 C20 124.82(17) . . ? C21 C20 C19 116.34(16) . . ? C21 C20 C26 124.07(17) . . ? C19 C20 C26 119.54(16) . . ? C20 C21 C16 122.53(17) . . ? C25 C22 C18 111.20(17) . . ? C25 C22 C23 107.20(19) . . ? C18 C22 C23 109.93(16) . . ? C25 C22 C24 107.65(18) . . ? C18 C22 C24 111.73(18) . . ? C23 C22 C24 108.98(19) . . ? C29 C26 C20 111.74(16) . . ? C29 C26 C28 107.37(17) . . ? C20 C26 C28 110.04(17) . . ? C29 C26 C27 109.58(18) . . ? C20 C26 C27 108.95(16) . . ? C28 C26 C27 109.12(17) . . ? N2 C30 C16 126.63(16) . . ? C36 C31 N1 124.94(15) . . ? C36 C31 C32 119.74(15) . . ? N1 C31 C32 115.27(14) . . ? C33 C32 C31 119.51(15) . . ? C33 C32 N2 125.45(15) . . ? C31 C32 N2 115.03(14) . . ? C34 C33 C32 119.80(16) . . ? C33 C34 C35 120.13(16) . . ? C33 C34 C37 121.18(16) . . ? C35 C34 C37 118.66(16) . . ? C36 C35 C34 120.52(17) . . ? C35 C36 C31 120.27(17) . . ? O4 C37 O3 123.47(17) . . ? O4 C37 C34 119.12(17) . . ? O3 C37 C34 117.42(16) . . ? N3 C38 C39 110.34(19) . . ? N3 C38 C41 122.66(19) . . ? C39 C38 C41 127.0(2) . . ? C40 C39 C38 106.45(19) . . ? N4 C40 C39 105.89(19) . . ? N4 C40 C42 121.1(2) . . ? C39 C40 C42 133.0(2) . . ? C46 O5 C43 111.9(3) . . ? C44 O6 C45 107.3(3) . . ? O5 C43 C44 114.4(4) . . ? O6 C44 C43 116.3(4) . . ? C46 C45 O6 112.0(4) . . ? O5 C46 C45 112.1(4) . . ? #------------------------------------------------------------------------------# # END OF DATA BLOCK # #------------------------------------------------------------------------------#