# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address P.W.Roesky ; Universit\"at Karlsruhe Institut f\"ur Anorganische Chemie Engesserst. 15 76128 Karllsruhe Germany ; 'Nils Meyer' ; Freie Universit\"at Berlin Fabeckstr. 34-36 14195 Berlin Bundesrepublik Deutschland ; _publ_contact_author ; Prof. Dr. Peter Roesky Freie Universitaet Berlin Fabeckstr. 34-36 14195 Berlin Bundesrepublik Deutschland ; _publ_contact_author_email roesky@chemie.fu-berlin.de _publ_contact_author_fax +49/(0)3083852440 _publ_contact_author_phone +49/(0)3083854004 _publ_contact_letter ; ; _publ_requested_coeditor_name ? _publ_section_title ; ; _publ_contact_author_name 'Prof. Dr. Peter Roesky' data_f:\meyer\pyrlabh4\mk1 _database_code_depnum_ccdc_archive 'CCDC 689078' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C 38 H 62 N 3 O 2 B 2 LA 1' _chemical_formula_sum 'C38 H62 B2 La N3 O2' _chemical_formula_weight 753.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 16.0927(8) _cell_length_b 25.1371(17) _cell_length_c 19.9083(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8053.4(8) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.432 _exptl_crystal_size_mid 0.289 _exptl_crystal_size_min 0.204 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3152 _exptl_absorpt_coefficient_mu 1.094 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7507 _exptl_absorpt_correction_T_max 0.8509 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28300 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7100 _reflns_number_gt 4451 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.0363P)^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 7100 _refine_ls_number_parameters 434 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0723 _refine_ls_wR_factor_gt 0.0652 _refine_ls_goodness_of_fit_ref 0.864 _refine_ls_restrained_S_all 0.867 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3849(2) -0.02751(15) 0.12521(18) 0.0378(9) Uani 1 1 d . . . H1 H 0.3900 -0.0647 0.1329 0.045 Uiso 1 1 calc R . . C2 C 0.4555(2) 0.00170(14) 0.10229(17) 0.0354(8) Uani 1 1 d . . . C3 C 0.5370(2) -0.01430(16) 0.0866(2) 0.0435(10) Uani 1 1 d . . . H3 H 0.5591 -0.0493 0.0889 0.052 Uiso 1 1 calc R . . C4 C 0.5783(2) 0.03145(16) 0.0672(2) 0.0448(10) Uani 1 1 d . . . H4 H 0.6347 0.0340 0.0534 0.054 Uiso 1 1 calc R . . C5 C 0.5212(2) 0.07326(15) 0.07167(19) 0.0379(9) Uani 1 1 d . . . C6 C 0.5283(2) 0.12817(15) 0.0559(2) 0.0419(9) Uani 1 1 d . . . H6 H 0.5802 0.1417 0.0409 0.050 Uiso 1 1 calc R . . C7 C 0.2507(2) -0.03754(15) 0.1647(2) 0.0392(9) Uani 1 1 d . . . C8 C 0.1860(2) -0.05665(15) 0.1242(2) 0.0467(9) Uani 1 1 d . . . C9 C 0.1245(3) -0.08721(19) 0.1534(3) 0.0637(13) Uani 1 1 d . . . H9 H 0.0805 -0.1007 0.1265 0.076 Uiso 1 1 calc R . . C10 C 0.1265(3) -0.0983(2) 0.2215(3) 0.0690(14) Uani 1 1 d . . . H10 H 0.0830 -0.1186 0.2411 0.083 Uiso 1 1 calc R . . C11 C 0.1904(3) -0.08043(18) 0.2607(2) 0.0603(12) Uani 1 1 d . . . H11 H 0.1912 -0.0890 0.3071 0.072 Uiso 1 1 calc R . . C12 C 0.2548(2) -0.04971(16) 0.2336(2) 0.0477(10) Uani 1 1 d . . . C13 C 0.4818(2) 0.21506(16) 0.0462(2) 0.0503(11) Uani 1 1 d . . . C14 C 0.5234(3) 0.24702(17) 0.0939(3) 0.0615(13) Uani 1 1 d . . . C15 C 0.5371(4) 0.2998(2) 0.0766(4) 0.090(2) Uani 1 1 d . . . H15 H 0.5663 0.3224 0.1067 0.108 Uiso 1 1 calc R . . C16 C 0.5091(4) 0.3198(2) 0.0168(4) 0.106(3) Uani 1 1 d . . . H16 H 0.5176 0.3565 0.0072 0.127 Uiso 1 1 calc R . . C17 C 0.4695(4) 0.2888(2) -0.0294(4) 0.0880(19) Uani 1 1 d . . . H17 H 0.4520 0.3036 -0.0709 0.106 Uiso 1 1 calc R . . C18 C 0.4546(3) 0.23527(18) -0.0156(3) 0.0650(13) Uani 1 1 d . . . C19 C 0.1849(3) -0.04603(19) 0.0481(2) 0.0596(11) Uani 1 1 d . . . H19 H 0.2221 -0.0149 0.0394 0.072 Uiso 1 1 calc R . . C20 C 0.0989(3) -0.0319(3) 0.0213(3) 0.0888(18) Uani 1 1 d . . . H20A H 0.0786 0.0001 0.0440 0.107 Uiso 1 1 calc R . . H20B H 0.0607 -0.0615 0.0298 0.107 Uiso 1 1 calc R . . H20C H 0.1023 -0.0254 -0.0271 0.107 Uiso 1 1 calc R . . C21 C 0.2205(3) -0.0931(2) 0.0108(3) 0.0831(17) Uani 1 1 d . . . H21A H 0.1863 -0.1246 0.0194 0.100 Uiso 1 1 calc R . . H21B H 0.2774 -0.0997 0.0262 0.100 Uiso 1 1 calc R . . H21C H 0.2210 -0.0855 -0.0375 0.100 Uiso 1 1 calc R . . C22 C 0.3255(3) -0.03199(19) 0.2781(2) 0.0585(11) Uani 1 1 d . . . H22 H 0.3611 -0.0072 0.2514 0.070 Uiso 1 1 calc R . . C23 C 0.2962(3) -0.0019(2) 0.3407(3) 0.0813(16) Uani 1 1 d . . . H23A H 0.2603 -0.0251 0.3676 0.098 Uiso 1 1 calc R . . H23B H 0.2650 0.0298 0.3270 0.098 Uiso 1 1 calc R . . H23C H 0.3445 0.0088 0.3674 0.098 Uiso 1 1 calc R . . C24 C 0.3790(3) -0.0793(2) 0.2982(3) 0.0854(17) Uani 1 1 d . . . H24A H 0.4010 -0.0965 0.2577 0.102 Uiso 1 1 calc R . . H24B H 0.3453 -0.1049 0.3235 0.102 Uiso 1 1 calc R . . H24C H 0.4253 -0.0670 0.3263 0.102 Uiso 1 1 calc R . . C25 C 0.5555(3) 0.2255(2) 0.1601(3) 0.0726(14) Uani 1 1 d . . . H25 H 0.5329 0.1888 0.1658 0.087 Uiso 1 1 calc R . . C26 C 0.5264(4) 0.2587(3) 0.2200(3) 0.104(2) Uani 1 1 d . . . H26A H 0.4656 0.2591 0.2214 0.124 Uiso 1 1 calc R . . H26B H 0.5471 0.2952 0.2154 0.124 Uiso 1 1 calc R . . H26C H 0.5480 0.2432 0.2616 0.124 Uiso 1 1 calc R . . C27 C 0.6500(3) 0.2216(3) 0.1597(4) 0.113(2) Uani 1 1 d . . . H27A H 0.6739 0.2571 0.1528 0.136 Uiso 1 1 calc R . . H27B H 0.6677 0.1980 0.1233 0.136 Uiso 1 1 calc R . . H27C H 0.6692 0.2073 0.2028 0.136 Uiso 1 1 calc R . . C28 C 0.4163(3) 0.1985(3) -0.0675(3) 0.0846(18) Uani 1 1 d . . . H28 H 0.3867 0.1698 -0.0423 0.101 Uiso 1 1 calc R . . C29 C 0.3523(5) 0.2255(3) -0.1118(4) 0.134(3) Uiso 1 1 d . . . H29A H 0.3787 0.2546 -0.1366 0.160 Uiso 1 1 calc R . . H29B H 0.3074 0.2397 -0.0838 0.160 Uiso 1 1 calc R . . H29C H 0.3295 0.1996 -0.1436 0.160 Uiso 1 1 calc R . . C30 C 0.4800(4) 0.1718(2) -0.1112(3) 0.0950(18) Uani 1 1 d . . . H30A H 0.5180 0.1510 -0.0831 0.114 Uiso 1 1 calc R . . H30B H 0.5115 0.1988 -0.1359 0.114 Uiso 1 1 calc R . . H30C H 0.4520 0.1481 -0.1431 0.114 Uiso 1 1 calc R . . C31A C 0.2283(8) 0.2318(5) 0.0509(7) 0.090(4) Uiso 0.50 1 d P A 1 H31A H 0.2659 0.2323 0.0115 0.107 Uiso 0.50 1 calc PR A 1 H31B H 0.1801 0.2093 0.0390 0.107 Uiso 0.50 1 calc PR A 1 C31B C 0.1905(7) 0.2203(5) 0.0753(7) 0.084(3) Uiso 0.50 1 d P A 2 H31C H 0.1927 0.2165 0.0259 0.100 Uiso 0.50 1 calc PR A 2 H31D H 0.1455 0.1974 0.0931 0.100 Uiso 0.50 1 calc PR A 2 C32A C 0.2026(8) 0.2781(6) 0.0602(7) 0.094(4) Uiso 0.50 1 d P A 1 H32A H 0.1413 0.2790 0.0636 0.113 Uiso 0.50 1 calc PR A 1 H32B H 0.2207 0.3022 0.0236 0.113 Uiso 0.50 1 calc PR A 1 C32B C 0.1778(10) 0.2746(6) 0.0942(8) 0.105(4) Uiso 0.50 1 d P A 2 H32C H 0.1948 0.2979 0.0565 0.126 Uiso 0.50 1 calc PR A 2 H32D H 0.1179 0.2806 0.1025 0.126 Uiso 0.50 1 calc PR A 2 C33A C 0.2439(11) 0.2932(7) 0.1278(9) 0.118(6) Uiso 0.50 1 d P A 1 H33A H 0.2702 0.3287 0.1253 0.141 Uiso 0.50 1 calc PR A 1 H33B H 0.2029 0.2930 0.1649 0.141 Uiso 0.50 1 calc PR A 1 C33B C 0.2210(8) 0.2883(5) 0.1497(7) 0.069(3) Uiso 0.50 1 d P A 2 H33C H 0.1838 0.2902 0.1892 0.083 Uiso 0.50 1 calc PR A 2 H33D H 0.2479 0.3234 0.1436 0.083 Uiso 0.50 1 calc PR A 2 C34A C 0.3054(6) 0.2519(4) 0.1369(6) 0.058(3) Uiso 0.50 1 d P A 1 H34A H 0.3585 0.2621 0.1152 0.069 Uiso 0.50 1 calc PR A 1 H34B H 0.3157 0.2456 0.1852 0.069 Uiso 0.50 1 calc PR A 1 C34B C 0.2848(8) 0.2460(6) 0.1591(7) 0.083(4) Uiso 0.50 1 d P A 2 H34C H 0.3412 0.2614 0.1558 0.099 Uiso 0.50 1 calc PR A 2 H34D H 0.2786 0.2295 0.2040 0.099 Uiso 0.50 1 calc PR A 2 C35A C 0.1507(6) 0.0732(4) 0.2306(5) 0.046(2) Uiso 0.50 1 d P B 1 H35A H 0.1913 0.0453 0.2430 0.055 Uiso 0.50 1 calc PR B 1 H35B H 0.1559 0.1024 0.2637 0.055 Uiso 0.50 1 calc PR B 1 C35B C 0.1508(10) 0.0945(7) 0.2349(8) 0.106(6) Uiso 0.50 1 d P B 2 H35C H 0.1876 0.0704 0.2606 0.127 Uiso 0.50 1 calc PR B 2 H35D H 0.1558 0.1309 0.2534 0.127 Uiso 0.50 1 calc PR B 2 C36A C 0.0702(8) 0.0519(6) 0.2344(6) 0.081(4) Uiso 0.50 1 d PD B 1 H36A H 0.0726 0.0148 0.2510 0.097 Uiso 0.50 1 calc PR B 1 H36B H 0.0360 0.0730 0.2660 0.097 Uiso 0.50 1 calc PR B 1 C36B C 0.0652(10) 0.0763(7) 0.2372(8) 0.104(5) Uiso 0.50 1 d PD B 2 H36C H 0.0327 0.0976 0.2697 0.124 Uiso 0.50 1 calc PR B 2 H36D H 0.0627 0.0384 0.2507 0.124 Uiso 0.50 1 calc PR B 2 C37A C 0.0365(6) 0.0530(5) 0.1740(5) 0.066(3) Uiso 0.50 1 d PD B 1 H37A H -0.0207 0.0674 0.1765 0.079 Uiso 0.50 1 calc PR B 1 H37B H 0.0337 0.0165 0.1553 0.079 Uiso 0.50 1 calc PR B 1 C37B C 0.0309(10) 0.0834(7) 0.1667(8) 0.119(5) Uiso 0.50 1 d PD B 2 H37C H 0.0245 0.0488 0.1433 0.143 Uiso 0.50 1 calc PR B 2 H37D H -0.0230 0.1023 0.1670 0.143 Uiso 0.50 1 calc PR B 2 C38A C 0.0911(7) 0.0888(5) 0.1284(6) 0.069(3) Uiso 0.50 1 d P B 1 H38A H 0.0991 0.0722 0.0838 0.083 Uiso 0.50 1 calc PR B 1 H38B H 0.0652 0.1242 0.1224 0.083 Uiso 0.50 1 calc PR B 1 C38B C 0.0962(7) 0.1153(5) 0.1370(7) 0.083(4) Uiso 0.50 1 d P B 2 H38C H 0.0954 0.1123 0.0874 0.100 Uiso 0.50 1 calc PR B 2 H38D H 0.0899 0.1532 0.1495 0.100 Uiso 0.50 1 calc PR B 2 N1 N 0.31437(18) -0.00465(11) 0.13568(14) 0.0351(7) Uani 1 1 d . . . N2 N 0.44610(17) 0.05503(11) 0.09363(14) 0.0347(7) Uani 1 1 d . . . N3 N 0.46550(19) 0.16040(12) 0.06137(16) 0.0399(7) Uani 1 1 d . . . O1 O 0.17122(16) 0.09366(12) 0.16400(15) 0.0617(8) Uani 1 1 d . . . O2 O 0.27237(19) 0.20626(12) 0.10648(18) 0.0706(9) Uani 1 1 d . . . B1 B 0.2553(4) 0.0961(2) -0.0108(3) 0.0519(14) Uani 1 1 d . . . HB1 H 0.303(3) 0.077(2) -0.008(3) 0.091(18) Uiso 1 1 d . . . HB2 H 0.230(3) 0.0983(17) -0.060(2) 0.070(13) Uiso 1 1 d . . . HB3 H 0.275(3) 0.131(2) 0.000(3) 0.104(19) Uiso 1 1 d . . . HB4 H 0.216(3) 0.088(2) 0.022(3) 0.092(18) Uiso 1 1 d . . . B2 B 0.3628(4) 0.1334(3) 0.2418(3) 0.0582(14) Uani 1 1 d . . . HB5 H 0.358(2) 0.0893(15) 0.2341(18) 0.035(10) Uiso 1 1 d . . . HB6 H 0.379(3) 0.1432(18) 0.290(3) 0.078(15) Uiso 1 1 d . . . HB7 H 0.300(3) 0.1501(18) 0.227(2) 0.082(15) Uiso 1 1 d . . . HB8 H 0.403(2) 0.1477(16) 0.206(2) 0.053(12) Uiso 1 1 d . . . La1 La 0.320145(12) 0.107473(8) 0.114241(10) 0.03639(7) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.048(2) 0.0329(19) 0.033(2) 0.0019(17) -0.0026(17) 0.0013(17) C2 0.0398(18) 0.034(2) 0.032(2) -0.0008(16) -0.0007(16) 0.0029(16) C3 0.041(2) 0.039(2) 0.051(2) -0.0004(19) 0.0041(18) 0.0067(18) C4 0.0331(19) 0.052(3) 0.050(3) 0.000(2) 0.0064(17) 0.0066(19) C5 0.0365(19) 0.041(2) 0.036(2) -0.0035(18) 0.0000(16) -0.0016(18) C6 0.038(2) 0.043(2) 0.044(2) -0.0031(18) 0.0086(18) -0.0088(18) C7 0.0381(19) 0.037(2) 0.042(2) 0.0061(18) 0.0099(18) 0.0025(17) C8 0.0444(19) 0.052(2) 0.044(2) 0.0077(18) 0.003(2) -0.010(2) C9 0.050(2) 0.078(3) 0.064(3) 0.015(3) 0.002(2) -0.022(2) C10 0.059(3) 0.080(4) 0.069(3) 0.021(3) 0.021(2) -0.013(3) C11 0.061(3) 0.069(3) 0.051(3) 0.017(2) 0.015(2) -0.001(2) C12 0.052(2) 0.047(2) 0.043(2) 0.010(2) 0.009(2) 0.005(2) C13 0.055(2) 0.035(2) 0.062(3) 0.003(2) 0.024(2) 0.001(2) C14 0.065(3) 0.036(2) 0.083(4) -0.020(2) 0.033(2) -0.013(2) C15 0.112(4) 0.051(3) 0.108(5) -0.025(3) 0.061(4) -0.026(3) C16 0.137(6) 0.041(3) 0.141(7) 0.005(4) 0.082(5) 0.009(4) C17 0.095(4) 0.064(4) 0.105(5) 0.031(4) 0.046(4) 0.023(3) C18 0.064(3) 0.051(3) 0.080(4) 0.017(3) 0.029(3) 0.008(2) C19 0.052(2) 0.071(3) 0.056(3) 0.014(2) -0.006(2) -0.019(3) C20 0.072(3) 0.131(5) 0.063(4) 0.031(4) -0.020(3) -0.014(3) C21 0.085(3) 0.105(5) 0.059(3) 0.002(3) 0.011(3) -0.022(3) C22 0.065(3) 0.073(3) 0.038(2) 0.014(2) -0.002(2) -0.006(3) C23 0.101(4) 0.095(4) 0.048(3) 0.004(3) -0.010(3) 0.003(3) C24 0.071(3) 0.119(5) 0.066(4) 0.022(3) 0.000(3) 0.019(3) C25 0.081(3) 0.063(3) 0.075(4) -0.020(3) 0.010(3) -0.025(3) C26 0.104(4) 0.118(5) 0.088(4) -0.053(4) 0.013(3) -0.025(4) C27 0.080(4) 0.122(6) 0.136(6) -0.038(5) 0.007(4) -0.019(4) C28 0.075(3) 0.096(5) 0.082(4) 0.047(4) -0.011(3) -0.007(3) C30 0.129(5) 0.079(4) 0.076(4) 0.007(4) -0.014(4) -0.008(4) N1 0.0359(15) 0.0353(16) 0.0341(16) 0.0055(12) 0.0031(14) 0.0036(15) N2 0.0345(15) 0.0346(17) 0.0351(18) -0.0006(13) 0.0041(12) 0.0005(13) N3 0.0434(17) 0.0351(18) 0.0411(19) -0.0013(15) 0.0032(15) -0.0040(15) O1 0.0452(15) 0.082(2) 0.0574(18) 0.0157(16) 0.0080(14) 0.0164(16) O2 0.076(2) 0.0484(17) 0.087(3) -0.0034(19) -0.0246(19) 0.0208(16) B1 0.063(3) 0.054(4) 0.038(3) 0.000(2) -0.014(3) -0.006(3) B2 0.075(4) 0.062(4) 0.037(3) -0.011(3) -0.010(3) 0.002(3) La1 0.03642(10) 0.03824(11) 0.03452(10) -0.00158(12) -0.00019(11) 0.00622(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.289(4) . ? C1 C2 1.428(5) . ? C1 H1 0.9500 . ? C2 N2 1.360(4) . ? C2 C3 1.407(5) . ? C3 C4 1.384(5) . ? C3 H3 0.9500 . ? C4 C5 1.399(5) . ? C4 H4 0.9500 . ? C5 N2 1.365(4) . ? C5 C6 1.420(5) . ? C6 N3 1.300(5) . ? C6 H6 0.9500 . ? C7 C8 1.402(5) . ? C7 C12 1.406(5) . ? C7 N1 1.438(4) . ? C8 C9 1.382(5) . ? C8 C19 1.537(6) . ? C9 C10 1.384(7) . ? C9 H9 0.9500 . ? C10 C11 1.368(6) . ? C10 H10 0.9500 . ? C11 C12 1.401(5) . ? C11 H11 0.9500 . ? C12 C22 1.509(6) . ? C13 C18 1.402(6) . ? C13 C14 1.412(6) . ? C13 N3 1.431(5) . ? C14 C15 1.389(7) . ? C14 C25 1.515(7) . ? C15 C16 1.367(9) . ? C15 H15 0.9500 . ? C16 C17 1.365(9) . ? C16 H16 0.9500 . ? C17 C18 1.394(7) . ? C17 H17 0.9500 . ? C18 C28 1.517(8) . ? C19 C21 1.511(7) . ? C19 C20 1.524(6) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.522(6) . ? C22 C23 1.531(7) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.523(7) . ? C25 C26 1.529(7) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.503(8) . ? C28 C29 1.516(8) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31A C32A 1.248(16) . ? C31A O2 1.463(12) . ? C31A H31A 0.9900 . ? C31A H31B 0.9900 . ? C31B C32B 1.431(17) . ? C31B O2 1.498(12) . ? C31B H31C 0.9900 . ? C31B H31D 0.9900 . ? C32A C33A 1.55(2) . ? C32A H32A 0.9900 . ? C32A H32B 0.9900 . ? C32B C33B 1.351(18) . ? C32B H32C 0.9900 . ? C32B H32D 0.9900 . ? C33A C34A 1.45(2) . ? C33A H33A 0.9900 . ? C33A H33B 0.9900 . ? C33B C34B 1.489(18) . ? C33B H33C 0.9900 . ? C33B H33D 0.9900 . ? C34A O2 1.402(11) . ? C34A H34A 0.9900 . ? C34A H34B 0.9900 . ? C34B O2 1.462(13) . ? C34B H34C 0.9900 . ? C34B H34D 0.9900 . ? C35A C36A 1.405(15) . ? C35A O1 1.460(10) . ? C35A H35A 0.9900 . ? C35A H35B 0.9900 . ? C35B C36B 1.45(2) . ? C35B O1 1.450(16) . ? C35B H35C 0.9900 . ? C35B H35D 0.9900 . ? C36A C37A 1.319(12) . ? C36A H36A 0.9900 . ? C36A H36B 0.9900 . ? C36B C37B 1.517(14) . ? C36B H36C 0.9900 . ? C36B H36D 0.9900 . ? C37A C38A 1.552(15) . ? C37A H37A 0.9900 . ? C37A H37B 0.9900 . ? C37B C38B 1.448(19) . ? C37B H37C 0.9900 . ? C37B H37D 0.9900 . ? C38A O1 1.475(11) . ? C38A H38A 0.9900 . ? C38A H38B 0.9900 . ? C38B O1 1.430(12) . ? C38B H38C 0.9900 . ? C38B H38D 0.9900 . ? N1 La1 2.852(3) . ? N2 La1 2.453(3) . ? N3 La1 2.890(3) . ? O1 La1 2.616(3) . ? O2 La1 2.604(3) . ? B1 La1 2.714(5) . ? B1 HB1 0.90(5) . ? B1 HB2 1.06(5) . ? B1 HB3 0.95(6) . ? B1 HB4 0.94(6) . ? B2 La1 2.711(6) . ? B2 HB5 1.12(4) . ? B2 HB6 1.03(5) . ? B2 HB7 1.14(5) . ? B2 HB8 1.02(4) . ? La1 HB1 2.58(5) . ? La1 HB3 2.46(6) . ? La1 HB4 2.53(5) . ? La1 HB5 2.50(3) . ? La1 HB7 2.52(5) . ? La1 HB8 2.48(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 121.5(3) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? N2 C2 C3 110.9(3) . . ? N2 C2 C1 117.3(3) . . ? C3 C2 C1 131.7(3) . . ? C4 C3 C2 105.8(3) . . ? C4 C3 H3 127.1 . . ? C2 C3 H3 127.1 . . ? C3 C4 C5 106.9(3) . . ? C3 C4 H4 126.5 . . ? C5 C4 H4 126.5 . . ? N2 C5 C4 110.5(3) . . ? N2 C5 C6 117.9(3) . . ? C4 C5 C6 131.5(3) . . ? N3 C6 C5 121.6(3) . . ? N3 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C8 C7 C12 121.5(3) . . ? C8 C7 N1 119.6(3) . . ? C12 C7 N1 118.9(3) . . ? C9 C8 C7 118.7(4) . . ? C9 C8 C19 120.1(4) . . ? C7 C8 C19 121.1(3) . . ? C8 C9 C10 120.5(4) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C11 C10 C9 120.7(4) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 121.2(4) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C7 117.4(4) . . ? C11 C12 C22 119.6(4) . . ? C7 C12 C22 123.0(4) . . ? C18 C13 C14 122.1(4) . . ? C18 C13 N3 118.4(4) . . ? C14 C13 N3 119.5(4) . . ? C15 C14 C13 116.8(5) . . ? C15 C14 C25 120.2(5) . . ? C13 C14 C25 122.9(4) . . ? C16 C15 C14 121.1(6) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C17 C16 C15 122.0(6) . . ? C17 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C16 C17 C18 120.0(6) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 118.0(5) . . ? C17 C18 C28 121.6(5) . . ? C13 C18 C28 120.3(4) . . ? C21 C19 C20 110.7(4) . . ? C21 C19 C8 110.1(4) . . ? C20 C19 C8 113.3(4) . . ? C21 C19 H19 107.5 . . ? C20 C19 H19 107.5 . . ? C8 C19 H19 107.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C12 C22 C24 110.5(4) . . ? C12 C22 C23 113.1(4) . . ? C24 C22 C23 110.3(4) . . ? C12 C22 H22 107.6 . . ? C24 C22 H22 107.6 . . ? C23 C22 H22 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C14 C25 C27 111.0(5) . . ? C14 C25 C26 112.3(5) . . ? C27 C25 C26 110.2(5) . . ? C14 C25 H25 107.7 . . ? C27 C25 H25 107.7 . . ? C26 C25 H25 107.7 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C29 109.0(5) . . ? C30 C28 C18 113.0(4) . . ? C29 C28 C18 113.6(6) . . ? C30 C28 H28 107.0 . . ? C29 C28 H28 107.0 . . ? C18 C28 H28 107.0 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32A C31A O2 117.2(12) . . ? C32A C31A H31A 108.0 . . ? O2 C31A H31A 108.0 . . ? C32A C31A H31B 108.0 . . ? O2 C31A H31B 108.0 . . ? H31A C31A H31B 107.2 . . ? C32B C31B O2 104.0(10) . . ? C32B C31B H31C 111.0 . . ? O2 C31B H31C 111.0 . . ? C32B C31B H31D 111.0 . . ? O2 C31B H31D 111.0 . . ? H31C C31B H31D 109.0 . . ? C31A C32A C33A 102.4(13) . . ? C31A C32A H32A 111.3 . . ? C33A C32A H32A 111.3 . . ? C31A C32A H32B 111.3 . . ? C33A C32A H32B 111.3 . . ? H32A C32A H32B 109.2 . . ? C33B C32B C31B 112.6(12) . . ? C33B C32B H32C 109.1 . . ? C31B C32B H32C 109.1 . . ? C33B C32B H32D 109.1 . . ? C31B C32B H32D 109.1 . . ? H32C C32B H32D 107.8 . . ? C34A C33A C32A 103.1(13) . . ? C34A C33A H33A 111.1 . . ? C32A C33A H33A 111.1 . . ? C34A C33A H33B 111.1 . . ? C32A C33A H33B 111.1 . . ? H33A C33A H33B 109.1 . . ? C32B C33B C34B 106.1(12) . . ? C32B C33B H33C 110.5 . . ? C34B C33B H33C 110.5 . . ? C32B C33B H33D 110.5 . . ? C34B C33B H33D 110.5 . . ? H33C C33B H33D 108.7 . . ? O2 C34A C33A 105.9(10) . . ? O2 C34A H34A 110.6 . . ? C33A C34A H34A 110.6 . . ? O2 C34A H34B 110.6 . . ? C33A C34A H34B 110.6 . . ? H34A C34A H34B 108.7 . . ? O2 C34B C33B 107.7(10) . . ? O2 C34B H34C 110.2 . . ? C33B C34B H34C 110.2 . . ? O2 C34B H34D 110.2 . . ? C33B C34B H34D 110.2 . . ? H34C C34B H34D 108.5 . . ? C36A C35A O1 113.0(8) . . ? C36A C35A H35A 109.0 . . ? O1 C35A H35A 109.0 . . ? C36A C35A H35B 109.0 . . ? O1 C35A H35B 109.0 . . ? H35A C35A H35B 107.8 . . ? C36B C35B O1 103.9(12) . . ? C36B C35B H35C 111.0 . . ? O1 C35B H35C 111.0 . . ? C36B C35B H35D 111.0 . . ? O1 C35B H35D 111.0 . . ? H35C C35B H35D 109.0 . . ? C37A C36A C35A 108.8(11) . . ? C37A C36A H36A 109.9 . . ? C35A C36A H36A 109.9 . . ? C37A C36A H36B 109.9 . . ? C35A C36A H36B 109.9 . . ? H36A C36A H36B 108.3 . . ? C35B C36B C37B 106.2(14) . . ? C35B C36B H36C 110.5 . . ? C37B C36B H36C 110.5 . . ? C35B C36B H36D 110.5 . . ? C37B C36B H36D 110.5 . . ? H36C C36B H36D 108.7 . . ? C36A C37A C38A 108.2(10) . . ? C36A C37A H37A 110.1 . . ? C38A C37A H37A 110.1 . . ? C36A C37A H37B 110.1 . . ? C38A C37A H37B 110.1 . . ? H37A C37A H37B 108.4 . . ? C38B C37B C36B 100.4(12) . . ? C38B C37B H37C 111.7 . . ? C36B C37B H37C 111.7 . . ? C38B C37B H37D 111.7 . . ? C36B C37B H37D 111.7 . . ? H37C C37B H37D 109.5 . . ? O1 C38A C37A 105.2(8) . . ? O1 C38A H38A 110.7 . . ? C37A C38A H38A 110.7 . . ? O1 C38A H38B 110.7 . . ? C37A C38A H38B 110.7 . . ? H38A C38A H38B 108.8 . . ? O1 C38B C37B 104.3(10) . . ? O1 C38B H38C 110.9 . . ? C37B C38B H38C 110.9 . . ? O1 C38B H38D 110.9 . . ? C37B C38B H38D 110.9 . . ? H38C C38B H38D 108.9 . . ? C1 N1 C7 115.9(3) . . ? C1 N1 La1 112.8(2) . . ? C7 N1 La1 130.7(2) . . ? C2 N2 C5 105.9(3) . . ? C2 N2 La1 126.9(2) . . ? C5 N2 La1 127.2(2) . . ? C6 N3 C13 116.0(3) . . ? C6 N3 La1 111.9(2) . . ? C13 N3 La1 131.9(2) . . ? C38B O1 C35B 99.7(8) . . ? C38B O1 C35A 106.5(7) . . ? C35B O1 C35A 21.5(7) . . ? C38B O1 C38A 27.5(6) . . ? C35B O1 C38A 105.7(8) . . ? C35A O1 C38A 102.1(6) . . ? C38B O1 La1 125.5(5) . . ? C35B O1 La1 125.1(6) . . ? C35A O1 La1 126.7(4) . . ? C38A O1 La1 129.0(5) . . ? C34A O2 C31A 98.7(7) . . ? C34A O2 C34B 23.0(6) . . ? C31A O2 C34B 108.0(8) . . ? C34A O2 C31B 108.6(6) . . ? C31A O2 C31B 32.6(6) . . ? C34B O2 C31B 104.8(7) . . ? C34A O2 La1 130.0(4) . . ? C31A O2 La1 127.4(5) . . ? C34B O2 La1 124.7(6) . . ? C31B O2 La1 120.6(5) . . ? La1 B1 HB1 72(3) . . ? La1 B1 HB2 171(2) . . ? HB1 B1 HB2 114(4) . . ? La1 B1 HB3 64(3) . . ? HB1 B1 HB3 102(4) . . ? HB2 B1 HB3 107(4) . . ? La1 B1 HB4 69(3) . . ? HB1 B1 HB4 115(5) . . ? HB2 B1 HB4 113(4) . . ? HB3 B1 HB4 105(4) . . ? La1 B2 HB5 67.4(18) . . ? La1 B2 HB6 180(3) . . ? HB5 B2 HB6 113(3) . . ? La1 B2 HB7 68(2) . . ? HB5 B2 HB7 106(3) . . ? HB6 B2 HB7 112(4) . . ? La1 B2 HB8 66(2) . . ? HB5 B2 HB8 107(3) . . ? HB6 B2 HB8 113(3) . . ? HB7 B2 HB8 105(3) . . ? N2 La1 O2 138.30(10) . . ? N2 La1 O1 138.51(9) . . ? O2 La1 O1 83.03(10) . . ? N2 La1 B2 94.40(15) . . ? O2 La1 B2 84.31(16) . . ? O1 La1 B2 84.79(16) . . ? N2 La1 B1 96.19(16) . . ? O2 La1 B1 86.11(15) . . ? O1 La1 B1 88.93(16) . . ? B2 La1 B1 169.1(2) . . ? N2 La1 N1 61.37(9) . . ? O2 La1 N1 160.32(10) . . ? O1 La1 N1 77.43(9) . . ? B2 La1 N1 96.07(15) . . ? B1 La1 N1 91.21(14) . . ? N2 La1 N3 61.15(9) . . ? O2 La1 N3 77.20(10) . . ? O1 La1 N3 160.14(9) . . ? B2 La1 N3 91.46(16) . . ? B1 La1 N3 91.45(15) . . ? N1 La1 N3 122.40(8) . . ? N2 La1 HB1 76.8(13) . . ? O2 La1 HB1 101.3(13) . . ? O1 La1 HB1 102.6(11) . . ? B2 La1 HB1 171.1(12) . . ? B1 La1 HB1 19.4(12) . . ? N1 La1 HB1 81.0(12) . . ? N3 La1 HB1 83.2(11) . . ? N2 La1 HB3 102.8(13) . . ? O2 La1 HB3 68.1(14) . . ? O1 La1 HB3 96.2(13) . . ? B2 La1 HB3 152.0(14) . . ? B1 La1 HB3 20.5(14) . . ? N1 La1 HB3 111.5(15) . . ? N3 La1 HB3 78.2(13) . . ? HB1 La1 HB3 33.2(16) . . ? N2 La1 HB4 108.9(12) . . ? O2 La1 HB4 86.9(12) . . ? O1 La1 HB4 68.9(13) . . ? B2 La1 HB4 153.1(13) . . ? B1 La1 HB4 20.3(13) . . ? N1 La1 HB4 84.0(12) . . ? N3 La1 HB4 111.3(13) . . ? HB1 La1 HB4 35.4(15) . . ? HB3 La1 HB4 35.0(16) . . ? N2 La1 HB5 82.0(8) . . ? O2 La1 HB5 107.6(9) . . ? O1 La1 HB5 80.7(7) . . ? B2 La1 HB5 24.5(8) . . ? B1 La1 HB5 161.5(9) . . ? N1 La1 HB5 71.6(9) . . ? N3 La1 HB5 103.5(8) . . ? HB1 La1 HB5 151.1(15) . . ? HB3 La1 HB5 175.1(15) . . ? HB4 La1 HB5 144.5(15) . . ? N2 La1 HB7 119.2(11) . . ? O2 La1 HB7 66.9(11) . . ? O1 La1 HB7 66.3(10) . . ? B2 La1 HB7 24.8(11) . . ? B1 La1 HB7 144.6(11) . . ? N1 La1 HB7 106.4(11) . . ? N3 La1 HB7 103.6(10) . . ? HB1 La1 HB7 164.0(17) . . ? HB3 La1 HB7 133.2(17) . . ? HB4 La1 HB7 129.9(17) . . ? HB5 La1 HB7 42.0(13) . . ? N2 La1 HB8 84.2(9) . . ? O2 La1 HB8 79.3(9) . . ? O1 La1 HB8 105.4(10) . . ? B2 La1 HB8 22.1(9) . . ? B1 La1 HB8 158.0(10) . . ? N1 La1 HB8 108.0(9) . . ? N3 La1 HB8 69.4(10) . . ? HB1 La1 HB8 151.8(15) . . ? HB3 La1 HB8 138.2(17) . . ? HB4 La1 HB8 165.7(14) . . ? HB5 La1 HB8 40.5(12) . . ? HB7 La1 HB8 40.1(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 1.7(5) . . . . ? N1 C1 C2 C3 -178.9(4) . . . . ? N2 C2 C3 C4 -0.5(4) . . . . ? C1 C2 C3 C4 -179.9(4) . . . . ? C2 C3 C4 C5 0.1(4) . . . . ? C3 C4 C5 N2 0.4(5) . . . . ? C3 C4 C5 C6 -177.5(4) . . . . ? N2 C5 C6 N3 -0.6(6) . . . . ? C4 C5 C6 N3 177.2(4) . . . . ? C12 C7 C8 C9 1.3(6) . . . . ? N1 C7 C8 C9 -178.6(4) . . . . ? C12 C7 C8 C19 -176.2(4) . . . . ? N1 C7 C8 C19 3.9(6) . . . . ? C7 C8 C9 C10 0.5(7) . . . . ? C19 C8 C9 C10 178.0(4) . . . . ? C8 C9 C10 C11 -1.7(8) . . . . ? C9 C10 C11 C12 1.1(7) . . . . ? C10 C11 C12 C7 0.7(6) . . . . ? C10 C11 C12 C22 -178.4(4) . . . . ? C8 C7 C12 C11 -1.9(6) . . . . ? N1 C7 C12 C11 178.0(3) . . . . ? C8 C7 C12 C22 177.1(4) . . . . ? N1 C7 C12 C22 -3.0(6) . . . . ? C18 C13 C14 C15 -0.6(6) . . . . ? N3 C13 C14 C15 -179.7(4) . . . . ? C18 C13 C14 C25 -178.1(4) . . . . ? N3 C13 C14 C25 2.8(6) . . . . ? C13 C14 C15 C16 1.9(7) . . . . ? C25 C14 C15 C16 179.5(5) . . . . ? C14 C15 C16 C17 -2.5(9) . . . . ? C15 C16 C17 C18 1.6(9) . . . . ? C16 C17 C18 C13 -0.3(7) . . . . ? C16 C17 C18 C28 -175.6(5) . . . . ? C14 C13 C18 C17 -0.2(6) . . . . ? N3 C13 C18 C17 178.9(4) . . . . ? C14 C13 C18 C28 175.2(4) . . . . ? N3 C13 C18 C28 -5.8(6) . . . . ? C9 C8 C19 C21 -80.8(5) . . . . ? C7 C8 C19 C21 96.6(5) . . . . ? C9 C8 C19 C20 43.8(6) . . . . ? C7 C8 C19 C20 -138.7(4) . . . . ? C11 C12 C22 C24 69.5(5) . . . . ? C7 C12 C22 C24 -109.5(5) . . . . ? C11 C12 C22 C23 -54.7(5) . . . . ? C7 C12 C22 C23 126.3(4) . . . . ? C15 C14 C25 C27 -69.8(6) . . . . ? C13 C14 C25 C27 107.6(5) . . . . ? C15 C14 C25 C26 54.1(6) . . . . ? C13 C14 C25 C26 -128.5(5) . . . . ? C17 C18 C28 C30 89.7(6) . . . . ? C13 C18 C28 C30 -85.5(6) . . . . ? C17 C18 C28 C29 -35.1(7) . . . . ? C13 C18 C28 C29 149.7(5) . . . . ? O2 C31A C32A C33A 9.6(18) . . . . ? O2 C31B C32B C33B -23.0(17) . . . . ? C31A C32A C33A C34A 13.2(18) . . . . ? C31B C32B C33B C34B 16.1(19) . . . . ? C32A C33A C34A O2 -31.3(15) . . . . ? C32B C33B C34B O2 -2.2(16) . . . . ? O1 C35A C36A C37A 4.3(15) . . . . ? O1 C35B C36B C37B -18.7(17) . . . . ? C35A C36A C37A C38A -12.9(15) . . . . ? C35B C36B C37B C38B -11.7(18) . . . . ? C36A C37A C38A O1 17.1(13) . . . . ? C36B C37B C38B O1 38.7(15) . . . . ? C2 C1 N1 C7 -174.3(3) . . . . ? C2 C1 N1 La1 -2.7(4) . . . . ? C8 C7 N1 C1 -104.2(4) . . . . ? C12 C7 N1 C1 75.9(4) . . . . ? C8 C7 N1 La1 86.1(4) . . . . ? C12 C7 N1 La1 -93.9(4) . . . . ? C3 C2 N2 C5 0.7(4) . . . . ? C1 C2 N2 C5 -179.8(3) . . . . ? C3 C2 N2 La1 -178.9(2) . . . . ? C1 C2 N2 La1 0.6(5) . . . . ? C4 C5 N2 C2 -0.6(4) . . . . ? C6 C5 N2 C2 177.6(3) . . . . ? C4 C5 N2 La1 178.9(2) . . . . ? C6 C5 N2 La1 -2.9(5) . . . . ? C5 C6 N3 C13 177.8(4) . . . . ? C5 C6 N3 La1 2.8(5) . . . . ? C18 C13 N3 C6 103.6(4) . . . . ? C14 C13 N3 C6 -77.3(5) . . . . ? C18 C13 N3 La1 -82.7(4) . . . . ? C14 C13 N3 La1 96.4(4) . . . . ? C37B C38B O1 C35B -51.4(13) . . . . ? C37B C38B O1 C35A -30.5(12) . . . . ? C37B C38B O1 C38A 53.9(16) . . . . ? C37B C38B O1 La1 161.7(8) . . . . ? C36B C35B O1 C38B 42.1(13) . . . . ? C36B C35B O1 C35A -69(2) . . . . ? C36B C35B O1 C38A 14.5(14) . . . . ? C36B C35B O1 La1 -170.7(8) . . . . ? C36A C35A O1 C38B 34.7(12) . . . . ? C36A C35A O1 C35B 109(3) . . . . ? C36A C35A O1 C38A 6.7(11) . . . . ? C36A C35A O1 La1 -157.6(8) . . . . ? C37A C38A O1 C38B -116(2) . . . . ? C37A C38A O1 C35B -35.1(11) . . . . ? C37A C38A O1 C35A -13.3(10) . . . . ? C37A C38A O1 La1 150.4(6) . . . . ? C33A C34A O2 C31A 34.6(12) . . . . ? C33A C34A O2 C34B -81(2) . . . . ? C33A C34A O2 C31B 2.6(13) . . . . ? C33A C34A O2 La1 -167.1(8) . . . . ? C32A C31A O2 C34A -28.9(15) . . . . ? C32A C31A O2 C34B -7.3(16) . . . . ? C32A C31A O2 C31B 82.3(17) . . . . ? C32A C31A O2 La1 172.0(10) . . . . ? C33B C34B O2 C34A 92(2) . . . . ? C33B C34B O2 C31A 22.7(13) . . . . ? C33B C34B O2 C31B -11.2(13) . . . . ? C33B C34B O2 La1 -156.6(7) . . . . ? C32B C31B O2 C34A -3.9(13) . . . . ? C32B C31B O2 C31A -80.5(15) . . . . ? C32B C31B O2 C34B 19.8(13) . . . . ? C32B C31B O2 La1 166.9(8) . . . . ? C2 N2 La1 O2 179.6(3) . . . . ? C5 N2 La1 O2 0.1(4) . . . . ? C2 N2 La1 O1 6.1(4) . . . . ? C5 N2 La1 O1 -173.4(3) . . . . ? C2 N2 La1 B2 93.2(3) . . . . ? C5 N2 La1 B2 -86.3(3) . . . . ? C2 N2 La1 B1 -89.3(3) . . . . ? C5 N2 La1 B1 91.2(3) . . . . ? C2 N2 La1 N1 -1.3(3) . . . . ? C5 N2 La1 N1 179.2(3) . . . . ? C2 N2 La1 N3 -177.6(3) . . . . ? C5 N2 La1 N3 3.0(3) . . . . ? C34A O2 La1 N2 -56.5(7) . . . . ? C31A O2 La1 N2 96.2(7) . . . . ? C34B O2 La1 N2 -84.7(7) . . . . ? C31B O2 La1 N2 134.9(6) . . . . ? C34A O2 La1 O1 119.2(7) . . . . ? C31A O2 La1 O1 -88.2(7) . . . . ? C34B O2 La1 O1 90.9(7) . . . . ? C31B O2 La1 O1 -49.4(6) . . . . ? C34A O2 La1 B2 33.8(7) . . . . ? C31A O2 La1 B2 -173.6(7) . . . . ? C34B O2 La1 B2 5.5(7) . . . . ? C31B O2 La1 B2 -134.8(7) . . . . ? C34A O2 La1 B1 -151.4(7) . . . . ? C31A O2 La1 B1 1.2(7) . . . . ? C34B O2 La1 B1 -179.7(7) . . . . ? C31B O2 La1 B1 40.0(7) . . . . ? C34A O2 La1 N1 125.9(7) . . . . ? C31A O2 La1 N1 -81.5(8) . . . . ? C34B O2 La1 N1 97.7(7) . . . . ? C31B O2 La1 N1 -42.7(8) . . . . ? C34A O2 La1 N3 -59.0(7) . . . . ? C31A O2 La1 N3 93.6(7) . . . . ? C34B O2 La1 N3 -87.3(7) . . . . ? C31B O2 La1 N3 132.3(7) . . . . ? C38B O1 La1 N2 -138.6(7) . . . . ? C35B O1 La1 N2 82.4(8) . . . . ? C35A O1 La1 N2 55.9(6) . . . . ? C38A O1 La1 N2 -104.1(7) . . . . ? C38B O1 La1 O2 45.7(7) . . . . ? C35B O1 La1 O2 -93.3(8) . . . . ? C35A O1 La1 O2 -119.7(6) . . . . ? C38A O1 La1 O2 80.2(7) . . . . ? C38B O1 La1 B2 130.6(7) . . . . ? C35B O1 La1 B2 -8.4(8) . . . . ? C35A O1 La1 B2 -34.9(6) . . . . ? C38A O1 La1 B2 165.1(7) . . . . ? C38B O1 La1 B1 -40.5(7) . . . . ? C35B O1 La1 B1 -179.5(8) . . . . ? C35A O1 La1 B1 154.0(6) . . . . ? C38A O1 La1 B1 -6.0(7) . . . . ? C38B O1 La1 N1 -132.0(7) . . . . ? C35B O1 La1 N1 89.1(8) . . . . ? C35A O1 La1 N1 62.6(6) . . . . ? C38A O1 La1 N1 -97.5(7) . . . . ? C38B O1 La1 N3 50.8(8) . . . . ? C35B O1 La1 N3 -88.2(9) . . . . ? C35A O1 La1 N3 -114.7(6) . . . . ? C38A O1 La1 N3 85.3(7) . . . . ? C1 N1 La1 N2 2.0(2) . . . . ? C7 N1 La1 N2 172.0(3) . . . . ? C1 N1 La1 O2 -179.8(3) . . . . ? C7 N1 La1 O2 -9.8(5) . . . . ? C1 N1 La1 O1 -172.9(3) . . . . ? C7 N1 La1 O1 -3.0(3) . . . . ? C1 N1 La1 B2 -89.7(3) . . . . ? C7 N1 La1 B2 80.3(3) . . . . ? C1 N1 La1 B1 98.4(3) . . . . ? C7 N1 La1 B1 -91.6(3) . . . . ? C1 N1 La1 N3 5.9(3) . . . . ? C7 N1 La1 N3 175.9(3) . . . . ? C6 N3 La1 N2 -2.8(2) . . . . ? C13 N3 La1 N2 -176.7(4) . . . . ? C6 N3 La1 O2 175.2(3) . . . . ? C13 N3 La1 O2 1.3(3) . . . . ? C6 N3 La1 O1 170.0(3) . . . . ? C13 N3 La1 O1 -3.8(5) . . . . ? C6 N3 La1 B2 91.4(3) . . . . ? C13 N3 La1 B2 -82.5(4) . . . . ? C6 N3 La1 B1 -99.1(3) . . . . ? C13 N3 La1 B1 87.0(4) . . . . ? C6 N3 La1 N1 -6.7(3) . . . . ? C13 N3 La1 N1 179.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.469 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.058 _publ_section_abstract ; ; _publ_section_experimental ; ; _publ_section_comment ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; #============================================================================== #============================================================================== # Attachment 'compound_3.cif' # CIF-file generated for roesky R = 0.02 #============================================================================== data_roesky _database_code_depnum_ccdc_archive 'CCDC 689232' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H62 B2 Lu N3 O2, 2(C4 H8 O)' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural ? _chemical_formula_sum 'C46 H78 B2 Lu N3 O4' _chemical_formula_iupac ? _chemical_formula_weight 933.70 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Lu Lu -0.4720 5.8584 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall 'P -2yac' _symmetry_space_group_name_H-M 'P n' _symmetry_Int_Tables_number 7 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2+x,-y,1/2+z _cell_length_a 9.5587(9) _cell_length_b 15.1757(17) _cell_length_c 16.1030(19) _cell_angle_alpha 90 _cell_angle_beta 100.420(9) _cell_angle_gamma 90 _cell_volume 2297.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 6(2) _cell_measurement_reflns_used 10940 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 30.42 _cell_special_details ; ; _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 2.192 _exptl_absorpt_correction_type empirical # Example: '(North et al., 1968)' _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.688 _exptl_absorpt_correction_T_max 0.814 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 6(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating Anode FR591 BRUKER' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '4 circle euler goniometer HUBER' _diffrn_measurement_method 'rotation method' _diffrn_detector 'image plate' _diffrn_detector_type 'MAR345 MARRESEARCH' _diffrn_detector_area_resol_mean 6.67 # number of measured reflections (redundant set) _diffrn_reflns_number 13834 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 30.23 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_max 0.779 _diffrn_measured_fraction_theta_full 0.986 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 8265 # number of observed reflections (> n sig(I)) _reflns_number_gt 8047 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'FD345 (Weber, 2004)' _computing_cell_refinement 'EVAL14 (Duisenberg, 2003)' _computing_data_reduction 'EVAL14 (Duisenberg, 2003)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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. Hydrogen atoms except those of the BH4 group (which have been refined freely) have been put at calculated positions. For the hydrogen atoms of the BH3 group a search for the optimal dihedral angle was performed employing the SHELX command HFIX 137. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0)^2^+6.1344P] 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_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(7) # Permitted for _chemical_absolute_configuration: # Absolute configuration details # rm = Det. by chiral ref. mol. with known abs.conf # ad = Det. by anomalous dispersion # rmad = Det. by 'rm' and 'ad' # syn = Det. with reference to synthesis # unk = Unknown/Arbitrary _chemical_absolute_configuration ? _refine_ls_number_reflns 8265 _refine_ls_number_parameters 526 _refine_ls_number_restraints 2 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0618 _refine_ls_wR_factor_gt 0.0592 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.091 _refine_diff_density_min -0.848 _refine_diff_density_rms 0.095 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Lu1 Lu Uani 0.26964(1) 0.73646(1) 0.19960(1) 1.000 0.0068(1) . . O1 O Uani 0.0551(3) 0.67712(19) 0.12567(18) 1.000 0.0110(7) . . O2 O Uani 0.4605(3) 0.8118(2) 0.28327(18) 1.000 0.0115(8) . . N1 N Uani 0.0917(3) 0.9669(2) 0.1858(2) 1.000 0.0101(8) . . N2 N Uani 0.1442(3) 0.7948(2) 0.2944(2) 1.000 0.0083(8) . . N3 N Uani 0.2844(4) 0.6368(2) 0.2973(2) 1.000 0.0084(8) . . C1 C Uani 0.0492(4) 0.9470(3) 0.2569(2) 1.000 0.0104(10) . . C2 C Uani 0.0685(4) 0.8710(2) 0.3066(2) 1.000 0.0097(10) . . C3 C Uani 0.0141(4) 0.8619(3) 0.3829(3) 1.000 0.0109(10) . . C4 C Uani 0.0577(4) 0.7803(3) 0.4167(2) 1.000 0.0109(10) . . C5 C Uani 0.1377(4) 0.7412(2) 0.3609(2) 1.000 0.0082(9) . . C6 C Uani 0.2119(4) 0.6540(2) 0.3684(2) 1.000 0.0092(9) . . C7 C Uani 0.0488(4) 1.0530(2) 0.1513(2) 1.000 0.0091(9) . . C8 C Uani 0.1494(4) 1.1217(3) 0.1612(2) 1.000 0.0098(10) . . C9 C Uani 0.1056(4) 1.2046(3) 0.1306(2) 1.000 0.0120(10) . . C10 C Uani -0.0350(4) 1.2213(3) 0.0931(3) 1.000 0.0139(10) . . C11 C Uani -0.1320(4) 1.1521(3) 0.0824(3) 1.000 0.0133(10) . . C12 C Uani -0.0923(4) 1.0670(3) 0.1108(2) 1.000 0.0120(10) . . C13 C Uani -0.1987(4) 0.9922(3) 0.0922(2) 1.000 0.0122(10) . . C14 C Uani -0.3495(4) 1.0192(3) 0.1020(3) 1.000 0.0162(11) . . C15 C Uani -0.1984(5) 0.9573(3) 0.0035(3) 1.000 0.0165(11) . . C16 C Uani 0.3013(4) 1.1066(3) 0.2073(3) 1.000 0.0118(13) . . C17 C Uani 0.4104(5) 1.1676(3) 0.1783(3) 1.000 0.0174(11) . . C18 C Uani 0.3079(4) 1.1174(3) 0.3031(3) 1.000 0.0151(11) . . C19 C Uani 0.3470(4) 0.5509(2) 0.3051(2) 1.000 0.0089(10) . . C20 C Uani 0.4951(4) 0.5392(3) 0.3334(2) 1.000 0.0097(10) . . C21 C Uani 0.5512(4) 0.4540(3) 0.3434(2) 1.000 0.0113(10) . . C22 C Uani 0.4674(4) 0.3803(3) 0.3256(2) 1.000 0.0123(10) . . C23 C Uani 0.3214(4) 0.3914(3) 0.2967(3) 1.000 0.0118(10) . . C24 C Uani 0.2600(4) 0.4747(3) 0.2856(2) 1.000 0.0095(10) . . C25 C Uani 0.1049(4) 0.4825(3) 0.2456(3) 1.000 0.0108(10) . . C26 C Uani 0.0879(4) 0.4619(3) 0.1512(3) 1.000 0.0124(10) . . C27 C Uani 0.0070(6) 0.4231(4) 0.2879(4) 1.000 0.0171(16) . . C28 C Uani 0.5933(4) 0.6171(2) 0.3564(2) 1.000 0.0100(10) . . C29 C Uani 0.7235(4) 0.6143(3) 0.3137(3) 1.000 0.0146(11) . . C30 C Uani 0.6383(4) 0.6235(3) 0.4529(3) 1.000 0.0146(11) . . C31 C Uani -0.0765(4) 0.6745(3) 0.1581(3) 1.000 0.0121(10) . . C32 C Uani -0.1788(4) 0.7299(3) 0.0962(3) 1.000 0.0143(10) . . C33 C Uani -0.1364(4) 0.7065(3) 0.0110(3) 1.000 0.0163(11) . . C34 C Uani 0.0156(4) 0.6707(3) 0.0346(3) 1.000 0.0137(11) . . C35 C Uani 0.4601(4) 0.8416(3) 0.3694(3) 1.000 0.0137(11) . . C36 C Uani 0.6004(4) 0.8910(3) 0.3957(3) 1.000 0.0151(11) . . C37 C Uani 0.6253(4) 0.9284(3) 0.3123(3) 1.000 0.0144(10) . . C38 C Uani 0.5793(4) 0.8527(3) 0.2520(3) 1.000 0.0131(10) . . B1 B Uani 0.4093(5) 0.6872(3) 0.0920(3) 1.000 0.0127(11) . . B2 B Uani 0.1746(5) 0.9051(3) 0.1341(3) 1.000 0.0119(11) . . O3 O Uani 0.7278(3) 0.4071(2) 0.0847(2) 1.000 0.0199(9) . . C39 C Uani 0.6325(4) 0.3679(3) 0.1333(3) 1.000 0.0159(11) . . C40 C Uani 0.4853(6) 0.4103(4) 0.1041(4) 1.000 0.0158(14) . . C41 C Uani 0.5026(4) 0.4587(3) 0.0231(3) 1.000 0.0146(11) . . C42 C Uani 0.6592(4) 0.4834(3) 0.0432(3) 1.000 0.0158(11) . . O4 O Uani 0.9459(3) 0.0978(2) 0.3727(2) 1.000 0.0168(8) . . C43 C Uani 0.8580(5) 0.1013(3) 0.4352(3) 1.000 0.0163(11) . . C44 C Uani 0.7344(4) 0.1594(3) 0.3972(3) 1.000 0.0157(11) . . C45 C Uani 0.8036(5) 0.2286(3) 0.3483(3) 1.000 0.0186(11) . . C46 C Uani 0.9490(5) 0.1864(3) 0.3420(3) 1.000 0.0171(11) . . H1 H Uiso -0.00360 0.99220 0.27810 1.000 0.0120 calc R H1A H Uiso 0.469(7) 0.675(4) 0.046(4) 1.000 0.0150 . . H1B H Uiso 0.327(7) 0.753(4) 0.072(4) 1.000 0.0150 . . H1C H Uiso 0.319(8) 0.634(4) 0.101(4) 1.000 0.0150 . . H1D H Uiso 0.472(7) 0.691(4) 0.147(4) 1.000 0.0150 . . H2A H Uiso 0.195(7) 0.931(4) 0.080(4) 1.000 0.0140 . . H2B H Uiso 0.117(7) 0.840(5) 0.106(4) 1.000 0.0140 . . H2C H Uiso 0.296(7) 0.889(4) 0.173(4) 1.000 0.0140 . . H3 H Uiso -0.04170 0.90380 0.40620 1.000 0.0130 calc R H4 H Uiso 0.03780 0.75560 0.46750 1.000 0.0130 calc R H6A H Uiso 0.28250 0.65260 0.42160 1.000 0.0110 calc R H6B H Uiso 0.14150 0.60680 0.37120 1.000 0.0110 calc R H9 H Uiso 0.17320 1.25100 0.13530 1.000 0.0140 calc R H10 H Uiso -0.06410 1.27920 0.07510 1.000 0.0170 calc R H11 H Uiso -0.22720 1.16280 0.05520 1.000 0.0160 calc R H13 H Uiso -0.16690 0.94350 0.13320 1.000 0.0150 calc R H14A H Uiso -0.41370 0.96870 0.08930 1.000 0.0250 calc R H14B H Uiso -0.38260 1.06740 0.06280 1.000 0.0250 calc R H14C H Uiso -0.34870 1.03890 0.16000 1.000 0.0250 calc R H15A H Uiso -0.26710 0.90900 -0.00880 1.000 0.0250 calc R H15B H Uiso -0.10310 0.93560 -0.00030 1.000 0.0250 calc R H15C H Uiso -0.22470 1.00480 -0.03760 1.000 0.0250 calc R H16 H Uiso 0.32800 1.04450 0.19660 1.000 0.0140 calc R H17A H Uiso 0.50540 1.15440 0.21030 1.000 0.0260 calc R H17B H Uiso 0.38620 1.22900 0.18800 1.000 0.0260 calc R H17C H Uiso 0.40950 1.15840 0.11790 1.000 0.0260 calc R H18A H Uiso 0.23810 1.07830 0.32170 1.000 0.0220 calc R H18B H Uiso 0.28650 1.17870 0.31560 1.000 0.0220 calc R H18C H Uiso 0.40350 1.10220 0.33310 1.000 0.0220 calc R H21 H Uiso 0.65040 0.44680 0.36300 1.000 0.0140 calc R H22 H Uiso 0.50790 0.32300 0.33270 1.000 0.0150 calc R H23 H Uiso 0.26280 0.34080 0.28420 1.000 0.0140 calc R H25 H Uiso 0.07520 0.54510 0.25160 1.000 0.0130 calc R H26A H Uiso -0.01260 0.46680 0.12490 1.000 0.0190 calc R H26B H Uiso 0.12130 0.40190 0.14370 1.000 0.0190 calc R H26C H Uiso 0.14400 0.50390 0.12460 1.000 0.0190 calc R H27A H Uiso -0.09180 0.43090 0.25940 1.000 0.0260 calc R H27B H Uiso 0.01580 0.43930 0.34750 1.000 0.0260 calc R H27C H Uiso 0.03490 0.36130 0.28350 1.000 0.0260 calc R H28 H Uiso 0.53850 0.67170 0.33670 1.000 0.0120 calc R H29A H Uiso 0.78320 0.66610 0.33070 1.000 0.0220 calc R H29B H Uiso 0.69260 0.61440 0.25230 1.000 0.0220 calc R H29C H Uiso 0.77820 0.56070 0.33090 1.000 0.0220 calc R H30A H Uiso 0.70170 0.67420 0.46710 1.000 0.0220 calc R H30B H Uiso 0.68820 0.56950 0.47440 1.000 0.0220 calc R H30C H Uiso 0.55370 0.63100 0.47870 1.000 0.0220 calc R H31A H Uiso -0.06340 0.69980 0.21560 1.000 0.0150 calc R H31B H Uiso -0.11160 0.61330 0.15970 1.000 0.0150 calc R H32A H Uiso -0.16560 0.79360 0.10880 1.000 0.0170 calc R H32B H Uiso -0.27880 0.71370 0.09690 1.000 0.0170 calc R H33A H Uiso -0.20100 0.66130 -0.01910 1.000 0.0200 calc R H33B H Uiso -0.13910 0.75930 -0.02530 1.000 0.0200 calc R H34A H Uiso 0.01950 0.60870 0.01620 1.000 0.0160 calc R H34B H Uiso 0.08140 0.70600 0.00690 1.000 0.0160 calc R H35A H Uiso 0.45460 0.79080 0.40720 1.000 0.0160 calc R H35B H Uiso 0.37820 0.88100 0.37120 1.000 0.0160 calc R H36A H Uiso 0.59150 0.93840 0.43660 1.000 0.0180 calc R H36B H Uiso 0.67800 0.85060 0.42060 1.000 0.0180 calc R H37A H Uiso 0.72680 0.94330 0.31450 1.000 0.0170 calc R H37B H Uiso 0.56660 0.98150 0.29630 1.000 0.0170 calc R H38A H Uiso 0.54860 0.87460 0.19360 1.000 0.0160 calc R H38B H Uiso 0.65790 0.81010 0.25270 1.000 0.0160 calc R H39A H Uiso 0.66620 0.37900 0.19420 1.000 0.0190 calc R H39B H Uiso 0.62710 0.30350 0.12390 1.000 0.0190 calc R H40A H Uiso 0.40990 0.36490 0.09260 1.000 0.0190 calc R H40B H Uiso 0.46210 0.45190 0.14700 1.000 0.0190 calc R H41A H Uiso 0.48150 0.41970 -0.02680 1.000 0.0170 calc R H41B H Uiso 0.44110 0.51160 0.01370 1.000 0.0170 calc R H42A H Uiso 0.69590 0.49650 -0.00920 1.000 0.0190 calc R H42B H Uiso 0.67440 0.53550 0.08070 1.000 0.0190 calc R H43A H Uiso 0.91030 0.12710 0.48840 1.000 0.0200 calc R H43B H Uiso 0.82460 0.04170 0.44720 1.000 0.0200 calc R H44A H Uiso 0.69000 0.18720 0.44160 1.000 0.0190 calc R H44B H Uiso 0.66120 0.12530 0.35890 1.000 0.0190 calc R H45A H Uiso 0.81650 0.28520 0.37930 1.000 0.0220 calc R H45B H Uiso 0.74600 0.23890 0.29160 1.000 0.0220 calc R H46A H Uiso 0.96360 0.18630 0.28270 1.000 0.0200 calc R H46B H Uiso 1.02750 0.21980 0.37660 1.000 0.0200 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 Lu1 0.0075(1) 0.0051(1) 0.0082(1) 0.0005(1) 0.0023(1) 0.0001(1) O1 0.0102(12) 0.0118(13) 0.0119(13) 0.0009(9) 0.0043(10) -0.0003(9) O2 0.0119(13) 0.0107(15) 0.0116(13) 0.0013(10) 0.0016(10) -0.0026(9) N1 0.0105(14) 0.0080(15) 0.0124(15) 0.0004(11) 0.0038(12) 0.0010(11) N2 0.0087(13) 0.0056(14) 0.0109(14) -0.0018(11) 0.0023(11) -0.0008(11) N3 0.0103(14) 0.0058(15) 0.0099(14) 0.0017(10) 0.0039(12) -0.0012(11) C1 0.0092(16) 0.0080(17) 0.0136(17) -0.0033(13) 0.0012(13) -0.0008(12) C2 0.0087(16) 0.0059(17) 0.0143(17) -0.0022(12) 0.0017(13) 0.0024(12) C3 0.0092(16) 0.0098(18) 0.0139(17) 0.0001(13) 0.0025(13) 0.0000(12) C4 0.0120(16) 0.0098(18) 0.0118(16) 0.0035(13) 0.0045(13) -0.0007(12) C5 0.0077(15) 0.0063(17) 0.0101(15) -0.0003(12) 0.0000(12) -0.0025(12) C6 0.0124(16) 0.0065(17) 0.0095(16) 0.0008(12) 0.0041(13) 0.0008(12) C7 0.0100(16) 0.0075(17) 0.0109(16) -0.0004(12) 0.0049(13) -0.0002(12) C8 0.0109(18) 0.0095(18) 0.0091(16) 0.0019(12) 0.0023(14) 0.0020(13) C9 0.0145(17) 0.0088(18) 0.0132(17) -0.0008(13) 0.0042(14) -0.0013(13) C10 0.0196(18) 0.0082(19) 0.0134(17) 0.0021(13) 0.0020(14) 0.0012(13) C11 0.0137(17) 0.0141(19) 0.0118(17) 0.0024(13) 0.0013(14) 0.0024(13) C12 0.0168(18) 0.0099(18) 0.0101(16) -0.0027(13) 0.0043(14) 0.0006(13) C13 0.0151(18) 0.0111(19) 0.0098(16) -0.0003(13) 0.0003(14) 0.0013(13) C14 0.0140(18) 0.016(2) 0.019(2) 0.0034(15) 0.0040(15) -0.0008(14) C15 0.021(2) 0.012(2) 0.0152(19) -0.0037(14) -0.0002(15) -0.0025(14) C16 0.013(3) 0.0083(17) 0.015(2) 0.0004(14) 0.005(2) 0.0018(11) C17 0.0164(19) 0.014(2) 0.023(2) -0.0008(15) 0.0068(16) -0.0015(14) C18 0.0132(18) 0.016(2) 0.0157(19) -0.0007(14) 0.0014(15) 0.0003(14) C19 0.0119(16) 0.0077(18) 0.0078(16) 0.0008(12) 0.0037(13) 0.0003(12) C20 0.0100(16) 0.0106(18) 0.0088(16) 0.0007(12) 0.0022(13) 0.0001(12) C21 0.0108(16) 0.0122(19) 0.0115(17) 0.0010(13) 0.0038(13) 0.0049(13) C22 0.0184(19) 0.0077(18) 0.0121(17) 0.0002(12) 0.0063(14) 0.0036(13) C23 0.0156(18) 0.0061(18) 0.0138(17) -0.0009(13) 0.0029(14) -0.0012(13) C24 0.0109(16) 0.0104(18) 0.0084(16) 0.0000(12) 0.0049(13) 0.0014(12) C25 0.0071(15) 0.0088(18) 0.0166(18) 0.0004(13) 0.0026(13) -0.0014(12) C26 0.0114(17) 0.0121(19) 0.0138(17) 0.0001(13) 0.0025(14) 0.0005(13) C27 0.015(3) 0.015(2) 0.023(3) 0.0031(17) 0.008(2) -0.0008(19) C28 0.0086(16) 0.0093(18) 0.0113(16) 0.0018(12) 0.0001(13) 0.0012(12) C29 0.0118(17) 0.0129(19) 0.0197(19) -0.0019(14) 0.0047(15) -0.0005(13) C30 0.0161(18) 0.014(2) 0.0140(18) -0.0015(13) 0.0032(15) 0.0014(14) C31 0.0083(16) 0.0165(19) 0.0125(17) -0.0003(13) 0.0045(13) -0.0002(13) C32 0.0154(17) 0.0110(19) 0.0169(18) 0.0009(14) 0.0044(14) 0.0017(13) C33 0.0168(18) 0.018(2) 0.0132(17) 0.0023(14) 0.0003(14) 0.0055(15) C34 0.0142(18) 0.018(2) 0.0095(17) 0.0005(13) 0.0037(14) -0.0014(14) C35 0.0146(18) 0.016(2) 0.0116(17) -0.0024(13) 0.0052(14) -0.0033(14) C36 0.0113(17) 0.016(2) 0.0179(19) -0.0033(14) 0.0022(15) -0.0009(13) C37 0.0095(16) 0.0134(19) 0.0201(19) 0.0012(14) 0.0025(14) -0.0025(13) C38 0.0127(17) 0.0122(19) 0.0151(18) 0.0010(13) 0.0044(14) -0.0014(13) B1 0.0132(19) 0.012(2) 0.014(2) -0.0005(15) 0.0056(16) 0.0013(14) B2 0.020(2) 0.0042(19) 0.0120(19) 0.0014(14) 0.0041(16) 0.0023(14) O3 0.0115(13) 0.0304(18) 0.0183(15) 0.0055(12) 0.0038(11) 0.0035(11) C39 0.0139(18) 0.020(2) 0.0139(18) 0.0020(14) 0.0030(14) 0.0025(14) C40 0.013(2) 0.021(3) 0.014(2) 0.0032(17) 0.0037(18) 0.0020(19) C41 0.0159(18) 0.0129(19) 0.0139(18) 0.0004(13) 0.0000(14) 0.0019(14) C42 0.0129(18) 0.015(2) 0.020(2) -0.0019(14) 0.0040(15) -0.0003(14) O4 0.0183(14) 0.0145(15) 0.0192(15) -0.0006(11) 0.0075(12) 0.0026(11) C43 0.0164(18) 0.015(2) 0.0186(19) -0.0011(14) 0.0060(15) 0.0000(14) C44 0.0129(18) 0.017(2) 0.0181(19) 0.0017(14) 0.0049(15) 0.0027(14) C45 0.0171(18) 0.014(2) 0.025(2) 0.0048(15) 0.0045(16) 0.0030(14) C46 0.0177(19) 0.011(2) 0.024(2) 0.0036(15) 0.0077(16) 0.0020(14) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 O1 2.356(3) . . yes Lu1 O2 2.358(3) . . yes Lu1 N2 2.284(3) . . yes Lu1 N3 2.168(3) . . yes Lu1 B1 2.486(5) . . yes Lu1 B2 2.853(5) . . yes Lu1 H1B 2.24(6) . . no O1 C34 1.450(6) . . yes O1 C31 1.447(5) . . yes O2 C38 1.461(5) . . yes O2 C35 1.460(6) . . yes O3 C39 1.433(5) . . yes O3 C42 1.435(5) . . yes O4 C46 1.435(6) . . yes O4 C43 1.424(6) . . yes N1 C7 1.450(4) . . yes N1 C1 1.317(5) . . yes N1 B2 1.562(6) . . yes N2 C2 1.397(4) . . yes N2 C5 1.355(4) . . yes N3 C19 1.430(5) . . yes N3 C6 1.465(5) . . yes C1 C2 1.397(5) . . no C2 C3 1.425(6) . . no C3 C4 1.386(6) . . no C4 C5 1.412(5) . . no C5 C6 1.496(5) . . no C7 C12 1.404(5) . . no C7 C8 1.408(5) . . no C8 C9 1.388(6) . . no C8 C16 1.524(6) . . no C9 C10 1.393(6) . . no C10 C11 1.391(6) . . no C11 C12 1.399(6) . . no C12 C13 1.517(6) . . no C13 C14 1.534(6) . . no C13 C15 1.524(6) . . no C16 C18 1.541(7) . . no C16 C17 1.529(6) . . no C19 C24 1.426(5) . . no C19 C20 1.418(5) . . no C20 C21 1.398(6) . . no C20 C28 1.513(5) . . no C21 C22 1.375(6) . . no C22 C23 1.399(6) . . no C23 C24 1.392(6) . . no C24 C25 1.510(6) . . no C25 C26 1.532(7) . . no C25 C27 1.544(7) . . no C28 C29 1.527(6) . . no C28 C30 1.539(6) . . no C31 C32 1.518(6) . . no C32 C33 1.541(7) . . no C33 C34 1.533(6) . . no C35 C36 1.528(6) . . no C36 C37 1.516(7) . . no C37 C38 1.517(7) . . no C1 H1 0.9500 . . no C3 H3 0.9500 . . no C4 H4 0.9500 . . no C6 H6B 0.9900 . . no C6 H6A 0.9900 . . no C9 H9 0.9500 . . no C10 H10 0.9500 . . no C11 H11 0.9500 . . no C13 H13 1.0000 . . no C14 H14C 0.9800 . . no C14 H14B 0.9800 . . no C14 H14A 0.9800 . . no C15 H15B 0.9800 . . no C15 H15C 0.9800 . . no C15 H15A 0.9800 . . no C16 H16 1.0000 . . no C17 H17C 0.9800 . . no C17 H17A 0.9800 . . no C17 H17B 0.9800 . . no C18 H18B 0.9800 . . no C18 H18C 0.9800 . . no C18 H18A 0.9800 . . no C21 H21 0.9500 . . no C22 H22 0.9500 . . no C23 H23 0.9500 . . no C25 H25 1.0000 . . no C26 H26B 0.9800 . . no C26 H26C 0.9800 . . no C26 H26A 0.9800 . . no C27 H27C 0.9800 . . no C27 H27A 0.9800 . . no C27 H27B 0.9800 . . no C28 H28 1.0000 . . no C29 H29C 0.9800 . . no C29 H29B 0.9800 . . no C29 H29A 0.9800 . . no C30 H30A 0.9800 . . no C30 H30C 0.9800 . . no C30 H30B 0.9800 . . no C31 H31A 0.9900 . . no C31 H31B 0.9900 . . no C32 H32B 0.9900 . . no C32 H32A 0.9900 . . no C33 H33A 0.9900 . . no C33 H33B 0.9900 . . no C34 H34B 0.9900 . . no C34 H34A 0.9900 . . no C35 H35B 0.9900 . . no C35 H35A 0.9900 . . no C36 H36B 0.9900 . . no C36 H36A 0.9900 . . no C37 H37A 0.9900 . . no C37 H37B 0.9900 . . no C38 H38A 0.9900 . . no C38 H38B 0.9900 . . no C39 C40 1.541(7) . . no C40 C41 1.532(8) . . no C41 C42 1.520(6) . . no C39 H39B 0.9900 . . no C39 H39A 0.9900 . . no C40 H40A 0.9900 . . no C40 H40B 0.9900 . . no C41 H41A 0.9900 . . no C41 H41B 0.9900 . . no C42 H42A 0.9900 . . no C42 H42B 0.9900 . . no C43 C44 1.512(6) . . no C44 C45 1.533(6) . . no C45 C46 1.550(7) . . no C43 H43A 0.9900 . . no C43 H43B 0.9900 . . no C44 H44A 0.9900 . . no C44 H44B 0.9900 . . no C45 H45B 0.9900 . . no C45 H45A 0.9900 . . no C46 H46A 0.9900 . . no C46 H46B 0.9900 . . no B1 H1D 0.98(7) . . no B1 H1C 1.21(7) . . no B1 H1A 1.03(7) . . no B1 H1B 1.28(6) . . no B2 H2B 1.18(7) . . no B2 H2C 1.24(7) . . no B2 H2A 1.01(6) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Lu1 O2 170.65(10) . . . yes O1 Lu1 N2 88.38(10) . . . yes O1 Lu1 N3 92.09(12) . . . yes O1 Lu1 B1 93.50(13) . . . yes O1 Lu1 B2 88.06(12) . . . yes O2 Lu1 N2 82.85(10) . . . yes O2 Lu1 N3 88.94(12) . . . yes O2 Lu1 B1 94.96(13) . . . yes O2 Lu1 B2 86.45(12) . . . yes N2 Lu1 N3 76.03(12) . . . yes N2 Lu1 B1 174.67(13) . . . yes N2 Lu1 B2 74.26(12) . . . yes N3 Lu1 B1 108.86(14) . . . yes N3 Lu1 B2 150.27(13) . . . yes B1 Lu1 B2 100.79(14) . . . yes O1 Lu1 H1B 85.1(17) . . . no O2 Lu1 H1B 100.2(17) . . . no N2 Lu1 H1B 144.8(16) . . . no N3 Lu1 H1B 138.7(16) . . . no B1 Lu1 H1B 30.8(16) . . . no B2 Lu1 H1B 71.0(16) . . . no C31 O1 C34 106.2(3) . . . yes Lu1 O1 C31 124.2(2) . . . yes Lu1 O1 C34 125.5(2) . . . yes C35 O2 C38 109.4(3) . . . yes Lu1 O2 C35 124.0(2) . . . yes Lu1 O2 C38 125.3(2) . . . yes C39 O3 C42 107.9(3) . . . yes C43 O4 C46 105.1(3) . . . yes C1 N1 C7 115.4(3) . . . yes C1 N1 B2 126.3(3) . . . yes C7 N1 B2 118.2(3) . . . yes Lu1 N2 C2 139.7(2) . . . yes C2 N2 C5 106.7(3) . . . yes Lu1 N2 C5 113.6(2) . . . yes Lu1 N3 C6 117.7(2) . . . yes C6 N3 C19 110.1(3) . . . yes Lu1 N3 C19 132.1(2) . . . yes N1 C1 C2 131.1(4) . . . yes N2 C2 C1 128.4(3) . . . yes C1 C2 C3 122.9(3) . . . no N2 C2 C3 108.7(3) . . . yes C2 C3 C4 107.1(3) . . . no C3 C4 C5 106.5(3) . . . no N2 C5 C4 111.0(3) . . . yes C4 C5 C6 128.6(3) . . . no N2 C5 C6 120.4(3) . . . yes N3 C6 C5 112.3(3) . . . yes N1 C7 C8 119.0(3) . . . yes N1 C7 C12 119.7(3) . . . yes C8 C7 C12 121.3(3) . . . no C9 C8 C16 120.6(4) . . . no C7 C8 C16 121.0(4) . . . no C7 C8 C9 118.4(3) . . . no C8 C9 C10 121.6(4) . . . no C9 C10 C11 119.0(4) . . . no C10 C11 C12 121.4(4) . . . no C7 C12 C11 118.2(4) . . . no C11 C12 C13 119.6(3) . . . no C7 C12 C13 122.1(4) . . . no C12 C13 C14 112.9(4) . . . no C12 C13 C15 109.3(3) . . . no C14 C13 C15 110.5(3) . . . no C8 C16 C18 109.5(3) . . . no C8 C16 C17 113.7(4) . . . no C17 C16 C18 109.5(4) . . . no N3 C19 C24 120.1(3) . . . yes N3 C19 C20 121.3(3) . . . yes C20 C19 C24 118.6(3) . . . no C19 C20 C28 121.3(4) . . . no C21 C20 C28 119.1(3) . . . no C19 C20 C21 119.5(4) . . . no C20 C21 C22 122.1(4) . . . no C21 C22 C23 118.7(4) . . . no C22 C23 C24 121.6(4) . . . no C19 C24 C23 119.5(3) . . . no C23 C24 C25 119.0(4) . . . no C19 C24 C25 121.3(4) . . . no C26 C25 C27 110.8(4) . . . no C24 C25 C27 113.1(4) . . . no C24 C25 C26 109.1(3) . . . no C20 C28 C29 112.8(3) . . . no C20 C28 C30 110.1(3) . . . no C29 C28 C30 110.8(3) . . . no O1 C31 C32 104.3(3) . . . yes C31 C32 C33 102.4(3) . . . no C32 C33 C34 104.5(4) . . . no O1 C34 C33 106.8(3) . . . yes O2 C35 C36 105.2(3) . . . yes C35 C36 C37 102.1(4) . . . no C36 C37 C38 102.1(4) . . . no O2 C38 C37 104.7(3) . . . yes C2 C1 H1 114.00 . . . no N1 C1 H1 114.00 . . . no C4 C3 H3 126.00 . . . no C2 C3 H3 126.00 . . . no C3 C4 H4 127.00 . . . no C5 C4 H4 127.00 . . . no C5 C6 H6A 109.00 . . . no N3 C6 H6B 109.00 . . . no N3 C6 H6A 109.00 . . . no H6A C6 H6B 108.00 . . . no C5 C6 H6B 109.00 . . . no C10 C9 H9 119.00 . . . no C8 C9 H9 119.00 . . . no C9 C10 H10 120.00 . . . no C11 C10 H10 121.00 . . . no C12 C11 H11 119.00 . . . no C10 C11 H11 119.00 . . . no C15 C13 H13 108.00 . . . no C12 C13 H13 108.00 . . . no C14 C13 H13 108.00 . . . no H14A C14 H14C 110.00 . . . no C13 C14 H14B 109.00 . . . no C13 C14 H14A 110.00 . . . no H14B C14 H14C 109.00 . . . no C13 C14 H14C 110.00 . . . no H14A C14 H14B 109.00 . . . no H15B C15 H15C 109.00 . . . no C13 C15 H15C 109.00 . . . no H15A C15 H15B 109.00 . . . no C13 C15 H15B 110.00 . . . no C13 C15 H15A 110.00 . . . no H15A C15 H15C 109.00 . . . no C8 C16 H16 108.00 . . . no C18 C16 H16 108.00 . . . no C17 C16 H16 108.00 . . . no C16 C17 H17B 109.00 . . . no H17A C17 H17C 109.00 . . . no C16 C17 H17A 109.00 . . . no H17B C17 H17C 109.00 . . . no C16 C17 H17C 109.00 . . . no H17A C17 H17B 109.00 . . . no H18B C18 H18C 109.00 . . . no C16 C18 H18C 110.00 . . . no H18A C18 H18B 109.00 . . . no C16 C18 H18B 110.00 . . . no H18A C18 H18C 109.00 . . . no C16 C18 H18A 110.00 . . . no C22 C21 H21 119.00 . . . no C20 C21 H21 119.00 . . . no C23 C22 H22 121.00 . . . no C21 C22 H22 121.00 . . . no C24 C23 H23 119.00 . . . no C22 C23 H23 119.00 . . . no C24 C25 H25 108.00 . . . no C27 C25 H25 108.00 . . . no C26 C25 H25 108.00 . . . no H26A C26 H26B 109.00 . . . no C25 C26 H26A 109.00 . . . no H26A C26 H26C 109.00 . . . no H26B C26 H26C 110.00 . . . no C25 C26 H26C 109.00 . . . no C25 C26 H26B 109.00 . . . no C25 C27 H27B 110.00 . . . no C25 C27 H27A 109.00 . . . no H27A C27 H27B 109.00 . . . no C25 C27 H27C 109.00 . . . no H27B C27 H27C 110.00 . . . no H27A C27 H27C 109.00 . . . no C20 C28 H28 108.00 . . . no C30 C28 H28 108.00 . . . no C29 C28 H28 108.00 . . . no H29A C29 H29B 110.00 . . . no C28 C29 H29A 109.00 . . . no H29A C29 H29C 109.00 . . . no H29B C29 H29C 110.00 . . . no C28 C29 H29B 109.00 . . . no C28 C29 H29C 109.00 . . . no C28 C30 H30B 109.00 . . . no C28 C30 H30A 109.00 . . . no H30A C30 H30C 109.00 . . . no H30A C30 H30B 109.00 . . . no C28 C30 H30C 110.00 . . . no H30B C30 H30C 109.00 . . . no H31A C31 H31B 109.00 . . . no C32 C31 H31A 111.00 . . . no O1 C31 H31A 111.00 . . . no O1 C31 H31B 111.00 . . . no C32 C31 H31B 111.00 . . . no C31 C32 H32A 111.00 . . . no C33 C32 H32A 111.00 . . . no C33 C32 H32B 111.00 . . . no H32A C32 H32B 109.00 . . . no C31 C32 H32B 111.00 . . . no C32 C33 H33B 111.00 . . . no C34 C33 H33A 111.00 . . . no C32 C33 H33A 111.00 . . . no H33A C33 H33B 109.00 . . . no C34 C33 H33B 111.00 . . . no H34A C34 H34B 109.00 . . . no C33 C34 H34A 110.00 . . . no O1 C34 H34A 110.00 . . . no O1 C34 H34B 110.00 . . . no C33 C34 H34B 110.00 . . . no O2 C35 H35A 111.00 . . . no C36 C35 H35A 111.00 . . . no C36 C35 H35B 111.00 . . . no H35A C35 H35B 109.00 . . . no O2 C35 H35B 111.00 . . . no H36A C36 H36B 109.00 . . . no C37 C36 H36A 111.00 . . . no C35 C36 H36B 111.00 . . . no C37 C36 H36B 111.00 . . . no C35 C36 H36A 111.00 . . . no H37A C37 H37B 109.00 . . . no C38 C37 H37A 111.00 . . . no C38 C37 H37B 111.00 . . . no C36 C37 H37A 111.00 . . . no C36 C37 H37B 111.00 . . . no O2 C38 H38B 111.00 . . . no C37 C38 H38A 111.00 . . . no O2 C38 H38A 111.00 . . . no H38A C38 H38B 109.00 . . . no C37 C38 H38B 111.00 . . . no O3 C39 C40 107.2(4) . . . yes C39 C40 C41 103.1(4) . . . no C40 C41 C42 101.0(4) . . . no O3 C42 C41 104.5(3) . . . yes O3 C39 H39A 110.00 . . . no O3 C39 H39B 110.00 . . . no H39A C39 H39B 109.00 . . . no C40 C39 H39A 110.00 . . . no C40 C39 H39B 110.00 . . . no C41 C40 H40A 111.00 . . . no C41 C40 H40B 111.00 . . . no H40A C40 H40B 109.00 . . . no C39 C40 H40A 111.00 . . . no C39 C40 H40B 111.00 . . . no C40 C41 H41A 112.00 . . . no C40 C41 H41B 111.00 . . . no C42 C41 H41A 112.00 . . . no C42 C41 H41B 112.00 . . . no H41A C41 H41B 109.00 . . . no O3 C42 H42B 111.00 . . . no C41 C42 H42A 111.00 . . . no O3 C42 H42A 111.00 . . . no C41 C42 H42B 111.00 . . . no H42A C42 H42B 109.00 . . . no O4 C43 C44 104.7(4) . . . yes C43 C44 C45 103.3(3) . . . no C44 C45 C46 103.1(4) . . . no O4 C46 C45 106.9(4) . . . yes O4 C43 H43A 111.00 . . . no O4 C43 H43B 111.00 . . . no H43A C43 H43B 109.00 . . . no C44 C43 H43A 111.00 . . . no C44 C43 H43B 111.00 . . . no C43 C44 H44A 111.00 . . . no H44A C44 H44B 109.00 . . . no C43 C44 H44B 111.00 . . . no C45 C44 H44A 111.00 . . . no C45 C44 H44B 111.00 . . . no H45A C45 H45B 109.00 . . . no C44 C45 H45B 111.00 . . . no C44 C45 H45A 111.00 . . . no C46 C45 H45B 111.00 . . . no C46 C45 H45A 111.00 . . . no C45 C46 H46A 110.00 . . . no H46A C46 H46B 109.00 . . . no O4 C46 H46B 110.00 . . . no O4 C46 H46A 110.00 . . . no C45 C46 H46B 110.00 . . . no Lu1 B2 N1 120.0(3) . . . yes Lu1 B1 H1B 64(3) . . . no Lu1 B1 H1A 173(3) . . . no H1A B1 H1D 110(5) . . . no H1B B1 H1C 98(5) . . . no H1B B1 H1D 116(5) . . . no H1C B1 H1D 105(5) . . . no Lu1 B1 H1D 71(4) . . . no H1A B1 H1B 111(5) . . . no Lu1 B1 H1C 68(3) . . . no H1A B1 H1C 118(5) . . . no Lu1 B2 H2A 125(4) . . . no Lu1 B2 H2B 59(3) . . . no H2A B2 H2B 98(5) . . . no H2A B2 H2C 102(5) . . . no H2B B2 H2C 111(5) . . . no Lu1 B2 H2C 55(3) . . . no N1 B2 H2A 115(4) . . . no N1 B2 H2B 117(3) . . . no N1 B2 H2C 112(3) . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Lu1 O1 C31 -11.4(3) . . . . no N2 Lu1 O1 C34 142.6(3) . . . . no N3 Lu1 O1 C31 64.6(3) . . . . no N3 Lu1 O1 C34 -141.5(3) . . . . no B1 Lu1 O1 C31 173.6(3) . . . . no B1 Lu1 O1 C34 -32.4(3) . . . . no B2 Lu1 O1 C31 -85.7(3) . . . . no B2 Lu1 O1 C34 68.3(3) . . . . no N2 Lu1 O2 C35 19.1(3) . . . . no N2 Lu1 O2 C38 -146.2(3) . . . . no N3 Lu1 O2 C35 -57.0(3) . . . . no N3 Lu1 O2 C38 137.8(3) . . . . no B1 Lu1 O2 C35 -165.8(3) . . . . no B1 Lu1 O2 C38 29.0(3) . . . . no B2 Lu1 O2 C35 93.6(3) . . . . no B2 Lu1 O2 C38 -71.6(3) . . . . no O1 Lu1 N2 C2 -88.5(4) . . . . no O1 Lu1 N2 C5 91.3(2) . . . . no O2 Lu1 N2 C2 88.2(4) . . . . no O2 Lu1 N2 C5 -91.9(2) . . . . no N3 Lu1 N2 C2 178.9(4) . . . . no N3 Lu1 N2 C5 -1.2(2) . . . . no B2 Lu1 N2 C2 -0.1(4) . . . . no B2 Lu1 N2 C5 179.8(3) . . . . no O1 Lu1 N3 C6 -87.1(3) . . . . no O1 Lu1 N3 C19 88.7(4) . . . . no O2 Lu1 N3 C6 83.7(3) . . . . no O2 Lu1 N3 C19 -100.6(4) . . . . no N2 Lu1 N3 C6 0.8(3) . . . . no N2 Lu1 N3 C19 176.5(4) . . . . no B1 Lu1 N3 C6 178.5(3) . . . . no B1 Lu1 N3 C19 -5.7(4) . . . . no B2 Lu1 N3 C6 2.7(4) . . . . no B2 Lu1 N3 C19 178.5(3) . . . . no O1 Lu1 B2 N1 92.4(3) . . . . no O2 Lu1 B2 N1 -80.0(3) . . . . no N2 Lu1 B2 N1 3.6(3) . . . . no N3 Lu1 B2 N1 1.6(5) . . . . no B1 Lu1 B2 N1 -174.4(3) . . . . no Lu1 O1 C31 C32 118.3(3) . . . . no C34 O1 C31 C32 -39.8(4) . . . . no Lu1 O1 C34 C33 -132.0(3) . . . . no C31 O1 C34 C33 25.8(4) . . . . no Lu1 O2 C35 C36 -176.8(2) . . . . no C38 O2 C35 C36 -9.5(4) . . . . no Lu1 O2 C38 C37 151.0(3) . . . . no C35 O2 C38 C37 -16.0(4) . . . . no C42 O3 C39 C40 13.3(5) . . . . no C39 O3 C42 C41 -34.3(4) . . . . no C43 O4 C46 C45 -31.5(4) . . . . no C46 O4 C43 C44 42.5(4) . . . . no C7 N1 C1 C2 179.0(4) . . . . no B2 N1 C7 C12 101.0(4) . . . . no C1 N1 B2 Lu1 -5.5(5) . . . . no C7 N1 B2 Lu1 178.3(2) . . . . no B2 N1 C1 C2 2.7(7) . . . . no C1 N1 C7 C8 102.8(4) . . . . no C1 N1 C7 C12 -75.5(4) . . . . no B2 N1 C7 C8 -80.6(4) . . . . no C5 N2 C2 C1 177.4(4) . . . . no Lu1 N2 C5 C6 1.6(4) . . . . no C2 N2 C5 C4 0.6(4) . . . . no C2 N2 C5 C6 -178.5(3) . . . . no Lu1 N2 C2 C1 -2.8(6) . . . . no Lu1 N2 C2 C3 179.4(3) . . . . no C5 N2 C2 C3 -0.5(4) . . . . no Lu1 N2 C5 C4 -179.4(2) . . . . no C6 N3 C19 C20 -102.9(4) . . . . no C6 N3 C19 C24 76.1(4) . . . . no Lu1 N3 C19 C24 -99.9(4) . . . . no Lu1 N3 C6 C5 -0.2(4) . . . . no C19 N3 C6 C5 -176.9(3) . . . . no Lu1 N3 C19 C20 81.1(4) . . . . no N1 C1 C2 N2 2.1(7) . . . . no N1 C1 C2 C3 179.7(4) . . . . no C1 C2 C3 C4 -177.7(4) . . . . no N2 C2 C3 C4 0.2(4) . . . . no C2 C3 C4 C5 0.1(4) . . . . no C3 C4 C5 N2 -0.4(4) . . . . no C3 C4 C5 C6 178.6(4) . . . . no C4 C5 C6 N3 -179.8(4) . . . . no N2 C5 C6 N3 -1.0(5) . . . . no N1 C7 C8 C9 -177.7(3) . . . . no N1 C7 C8 C16 0.0(5) . . . . no C8 C7 C12 C11 -1.8(5) . . . . no C8 C7 C12 C13 174.2(3) . . . . no C12 C7 C8 C9 0.7(5) . . . . no C12 C7 C8 C16 178.4(3) . . . . no N1 C7 C12 C11 176.5(3) . . . . no N1 C7 C12 C13 -7.5(5) . . . . no C7 C8 C9 C10 1.9(5) . . . . no C7 C8 C16 C18 -84.6(4) . . . . no C16 C8 C9 C10 -175.8(4) . . . . no C7 C8 C16 C17 152.5(4) . . . . no C9 C8 C16 C17 -29.9(5) . . . . no C9 C8 C16 C18 93.1(4) . . . . no C8 C9 C10 C11 -3.2(6) . . . . no C9 C10 C11 C12 2.0(7) . . . . no C10 C11 C12 C7 0.5(6) . . . . no C10 C11 C12 C13 -175.6(4) . . . . no C11 C12 C13 C14 -40.5(5) . . . . no C11 C12 C13 C15 82.9(5) . . . . no C7 C12 C13 C14 143.5(4) . . . . no C7 C12 C13 C15 -93.1(4) . . . . no N3 C19 C20 C28 -0.1(5) . . . . no N3 C19 C24 C23 -177.4(3) . . . . no N3 C19 C24 C25 8.2(5) . . . . no N3 C19 C20 C21 177.4(3) . . . . no C24 C19 C20 C21 -1.6(5) . . . . no C24 C19 C20 C28 -179.1(3) . . . . no C20 C19 C24 C23 1.6(5) . . . . no C20 C19 C24 C25 -172.8(3) . . . . no C28 C20 C21 C22 178.4(3) . . . . no C19 C20 C28 C29 -129.9(4) . . . . no C19 C20 C21 C22 0.8(5) . . . . no C19 C20 C28 C30 105.8(4) . . . . no C21 C20 C28 C29 52.6(4) . . . . no C21 C20 C28 C30 -71.8(4) . . . . no C20 C21 C22 C23 -0.1(5) . . . . no C21 C22 C23 C24 0.1(6) . . . . no C22 C23 C24 C25 173.6(4) . . . . no C22 C23 C24 C19 -0.9(6) . . . . no C23 C24 C25 C26 -72.4(5) . . . . no C19 C24 C25 C26 102.0(4) . . . . no C19 C24 C25 C27 -134.3(4) . . . . no C23 C24 C25 C27 51.4(5) . . . . no O1 C31 C32 C33 37.2(4) . . . . no C31 C32 C33 C34 -21.1(4) . . . . no C32 C33 C34 O1 -1.9(4) . . . . no O2 C35 C36 C37 31.1(4) . . . . no C35 C36 C37 C38 -40.1(4) . . . . no C36 C37 C38 O2 35.1(4) . . . . no O3 C39 C40 C41 12.6(5) . . . . no C39 C40 C41 C42 -31.6(5) . . . . no C40 C41 C42 O3 40.7(4) . . . . no O4 C43 C44 C45 -36.1(4) . . . . no C43 C44 C45 C46 16.2(4) . . . . no C44 C45 C46 O4 8.3(5) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Lu1 C25 4.278(4) . . no Lu1 C28 4.050(3) . . no Lu1 H25 3.6300 . . no Lu1 H26C 3.8500 . . no Lu1 H28 3.2200 . . no O1 N2 3.234(4) . . no O1 N3 3.260(4) . . no O1 C26 3.300(5) . . no O2 C28 3.345(4) . . no O2 N2 3.072(4) . . no O2 N3 3.174(4) . . no O4 C1 3.218(5) . 1_645 no O1 H2B 2.58(8) . . no O1 H25 2.8300 . . no O1 H1C 2.70(8) . . no O1 H26C 2.7600 . . no O2 H1D 2.88(6) . . no O2 H28 2.3600 . . no O2 H2C 2.45(6) . . no O3 H26A 2.6100 . 1_655 no O3 H10 2.8000 . 1_645 no O3 H6A 2.9100 . 2_564 no O4 H1 2.3200 . 1_645 no N1 N2 3.133(4) . . no N1 C18 3.412(5) . . no N2 O2 3.072(4) . . no N2 O1 3.234(4) . . no N2 B2 3.134(6) . . no N2 N1 3.133(4) . . no N2 C31 3.305(5) . . no N2 N3 2.743(4) . . no N2 C35 3.124(5) . . no N2 C6 2.475(4) . . no N3 N2 2.743(4) . . no N3 O2 3.174(4) . . no N3 C5 2.459(5) . . no N3 O1 3.260(4) . . no N1 H18A 2.9200 . . no N1 H16 2.5300 . . no N1 H13 2.4900 . . no N2 H31A 2.5900 . . no N2 H35B 2.6900 . . no N3 H25 2.4400 . . no N3 H28 2.4500 . . no C1 C13 3.293(5) . . no C1 O4 3.218(5) . 1_465 no C1 C18 3.562(6) . . no C5 C35 3.418(6) . . no C6 C25 3.316(6) . . no C13 C1 3.293(5) . . no C14 C17 3.587(6) . 1_455 no C15 C18 3.431(7) . 2_474 no C16 B2 3.419(6) . . no C17 C14 3.587(6) . 1_655 no C18 C1 3.562(6) . . no C18 N1 3.412(5) . . no C18 C15 3.431(7) . 2_575 no C22 C33 3.564(6) . 2_565 no C22 C34 3.403(6) . 2_565 no C25 Lu1 4.278(4) . . no C25 C6 3.316(6) . . no C25 C31 3.549(6) . . no C26 C31 3.599(6) . . no C26 O1 3.300(5) . . no C26 C30 3.559(7) . 2_464 no C28 O2 3.345(4) . . no C28 Lu1 4.050(3) . . no C29 C31 3.536(6) . 1_655 no C30 C26 3.559(7) . 2_565 no C31 C25 3.549(6) . . no C31 C29 3.536(6) . 1_455 no C31 C26 3.599(6) . . no C33 C22 3.564(6) . 2_464 no C34 C22 3.403(6) . 2_464 no C35 C5 3.418(6) . . no C1 H13 2.6000 . . no C1 H18A 2.7600 . . no C2 H35B 2.9600 . . no C3 H14B 3.0800 . 2_575 no C3 H37A 3.0300 . 1_455 no C4 H11 2.8800 . 2_575 no C5 H35A 3.0800 . . no C5 H31A 2.8200 . . no C6 H42A 3.0400 . 2_465 no C6 H25 2.6600 . . no C6 H35A 3.0900 . . no C7 H18A 3.0300 . . no C8 H46A 3.0300 . 1_465 no C9 H26B 3.0000 . 1_565 no C9 H46A 3.0200 . 1_465 no C9 H17B 2.7000 . . no C9 H17C 3.0300 . . no C10 H35A 2.9800 . 2_474 no C11 H15C 2.9800 . . no C11 H14B 2.6900 . . no C12 H1 2.9000 . . no C13 H32A 3.0400 . . no C14 H38A 2.9100 . 1_455 no C14 H11 2.6500 . . no C15 H32A 2.9900 . . no C15 H18A 2.9300 . 2_474 no C17 H9 2.5800 . . no C17 H14C 3.0700 . 1_655 no C21 H34A 3.0100 . 2_565 no C21 H29C 2.7400 . . no C21 H39A 3.0400 . . no C21 H30B 2.8700 . . no C22 H34A 3.0200 . 2_565 no C22 H39A 3.0900 . . no C22 H40B 3.0700 . . no C23 H26B 2.8400 . . no C23 H27C 2.7500 . . no C24 H6B 2.7900 . . no C25 H31B 3.0200 . . no C25 H6B 2.7400 . . no C26 H30C 3.0800 . 2_464 no C26 H23 3.0800 . . no C26 H34A 3.1000 . . no C26 H31B 3.0000 . . no C27 H23 2.7600 . . no C29 H31A 3.0800 . 1_655 no C29 H21 2.7900 . . no C30 H21 3.0600 . . no C30 H35A 3.1000 . . no C31 H29B 3.0400 . 1_455 no C31 H25 2.7300 . . no C34 H26C 3.0600 . . no C34 H1C 2.96(8) . . no C34 H2B 2.91(7) . . no C35 H28 2.7600 . . no C37 H44B 3.0800 . 1_565 no C37 H14C 3.0200 . 1_655 no C38 H1D 3.05(6) . . no C38 H2C 2.83(7) . . no C41 H30B 3.0000 . 2_464 no C42 H6B 3.0700 . 2_564 no C43 H2A 3.07(7) . 2_565 no C44 H1B 3.09(6) . 2_565 no C46 H27C 2.9800 . 1_655 no B2 N2 3.134(6) . . no B2 C16 3.419(6) . . no B2 C2 3.167(6) . . no B1 H41B 2.9900 . . no B1 H32B 3.0000 . 1_655 no B2 H1B 3.00(6) . . no B2 H16 2.6700 . . no H1 H3 2.5400 . . no H1 C12 2.9000 . . no H1 O4 2.3200 . 1_465 no H1A H41B 2.5400 . . no H1A H32B 2.4700 . 1_655 no H1B H34B 2.5000 . . no H1B H2B 2.54(10) . . no H1B H1C 1.87(9) . . no H1B H1D 1.91(9) . . no H1B H43A 2.4800 . 2_464 no H1B H1A 1.90(9) . . no H1B C44 3.09(6) . 2_464 no H1B B2 3.00(6) . . no H1B H44A 2.4400 . 2_464 no H1C C34 2.96(8) . . no H1D C38 3.05(6) . . no H2A C43 3.07(7) . 2_464 no H2B C34 2.91(7) . . no H2B H34B 2.5700 . . no H2C H16 2.4000 . . no H2C H38A 2.3900 . . no H2C C38 2.83(7) . . no H3 H1 2.5400 . . no H3 H37A 2.5000 . 1_455 no H3 H43B 2.6000 . 1_465 no H6A O3 2.9100 . 2_465 no H6B H25 2.1300 . . no H6B C25 2.7400 . . no H6B C24 2.7900 . . no H6B H42A 2.4600 . 2_465 no H6B C42 3.0700 . 2_465 no H6B H41A 2.4700 . 2_465 no H9 H17B 2.0900 . . no H9 H26B 2.3500 . 1_565 no H9 C17 2.5800 . . no H10 H30C 2.4800 . 2_474 no H10 O3 2.8000 . 1_465 no H11 C14 2.6500 . . no H11 C4 2.8800 . 2_474 no H11 H14B 2.0900 . . no H13 H32A 2.3100 . . no H13 C1 2.6000 . . no H13 N1 2.4900 . . no H14A H43A 2.5700 . 2_364 no H14A H38A 2.2800 . 1_455 no H14A H15A 2.4700 . . no H14B H15C 2.5800 . . no H14B C11 2.6900 . . no H14B H11 2.0900 . . no H14B C3 3.0800 . 2_474 no H14C C37 3.0200 . 1_455 no H14C H17A 2.4700 . 1_455 no H14C C17 3.0700 . 1_455 no H15A H14A 2.4700 . . no H15C C11 2.9800 . . no H15C H14B 2.5800 . . no H15C H35B 2.5800 . 2_474 no H15C H18A 2.5600 . 2_474 no H16 B2 2.6700 . . no H16 H2C 2.4000 . . no H16 N1 2.5300 . . no H17A H14C 2.4700 . 1_655 no H17A H18C 2.4900 . . no H17B H18B 2.5300 . . no H17B C9 2.7000 . . no H17B H9 2.0900 . . no H17C C9 3.0300 . . no H18A C15 2.9300 . 2_575 no H18A C7 3.0300 . . no H18A H15C 2.5600 . 2_575 no H18A N1 2.9200 . . no H18A C1 2.7600 . . no H18B H23 2.5100 . 1_565 no H18B H17B 2.5300 . . no H18C H17A 2.4900 . . no H18C H37B 2.5400 . . no H18C H44B 2.4500 . 1_565 no H21 H29C 2.2300 . . no H21 C29 2.7900 . . no H21 C30 3.0600 . . no H21 H30B 2.5700 . . no H23 C26 3.0800 . . no H23 H26B 2.5900 . . no H23 C27 2.7600 . . no H23 H27C 2.2000 . . no H23 H18B 2.5100 . 1_545 no H25 C6 2.6600 . . no H25 C31 2.7300 . . no H25 N3 2.4400 . . no H25 Lu1 3.6300 . . no H25 H31B 2.3400 . . no H25 H6B 2.1300 . . no H25 O1 2.8300 . . no H26A H31B 2.5200 . . no H26A O3 2.6100 . 1_455 no H26A H27A 2.4800 . . no H26B C23 2.8400 . . no H26B H23 2.5900 . . no H26B C9 3.0000 . 1_545 no H26B H9 2.3500 . 1_545 no H26C O1 2.7600 . . no H26C H34A 2.5000 . . no H26C Lu1 3.8500 . . no H26C C34 3.0600 . . no H27A H39A 2.4900 . 1_455 no H27A H26A 2.4800 . . no H27C C23 2.7500 . . no H27C C46 2.9800 . 1_455 no H27C H23 2.2000 . . no H28 C35 2.7600 . . no H28 Lu1 3.2200 . . no H28 O2 2.3600 . . no H28 N3 2.4500 . . no H28 H35A 2.3500 . . no H29A H30A 2.4600 . . no H29B C31 3.0400 . 1_655 no H29B H31B 2.6000 . 1_655 no H29C H21 2.2300 . . no H29C C21 2.7400 . . no H30A H29A 2.4600 . . no H30B C41 3.0000 . 2_565 no H30B H21 2.5700 . . no H30B C21 2.8700 . . no H30C H10 2.4800 . 2_575 no H30C C26 3.0800 . 2_565 no H31A C29 3.0800 . 1_455 no H31A N2 2.5900 . . no H31A C5 2.8200 . . no H31B C26 3.0000 . . no H31B H42B 2.5000 . 1_455 no H31B C25 3.0200 . . no H31B H29B 2.6000 . 1_455 no H31B H25 2.3400 . . no H31B H26A 2.5200 . . no H32A H13 2.3100 . . no H32A C15 2.9900 . . no H32A C13 3.0400 . . no H32B B1 3.0000 . 1_455 no H32B H1A 2.4700 . 1_455 no H34A C26 3.1000 . . no H34A C22 3.0200 . 2_464 no H34A H26C 2.5000 . . no H34A C21 3.0100 . 2_464 no H34B H2B 2.5700 . . no H34B H1B 2.5000 . . no H34B H44A 2.2800 . 2_464 no H35A H28 2.3500 . . no H35A C10 2.9800 . 2_575 no H35A C30 3.1000 . . no H35A C5 3.0800 . . no H35A C6 3.0900 . . no H35B H15C 2.5800 . 2_575 no H35B C2 2.9600 . . no H35B N2 2.6900 . . no H37A H3 2.5000 . 1_655 no H37A C3 3.0300 . 1_655 no H37B H18C 2.5400 . . no H37B H44B 2.5000 . 1_565 no H38A H14A 2.2800 . 1_655 no H38A H2C 2.3900 . . no H38A C14 2.9100 . 1_655 no H39A C22 3.0900 . . no H39A H27A 2.4900 . 1_655 no H39A C21 3.0400 . . no H40B C22 3.0700 . . no H41A H6B 2.4700 . 2_564 no H41B B1 2.9900 . . no H41B H1A 2.5400 . . no H42A H6B 2.4600 . 2_564 no H42A C6 3.0400 . 2_564 no H42B H31B 2.5000 . 1_655 no H43A H1B 2.4800 . 2_565 no H43A H14A 2.5700 . 2_665 no H43B H3 2.6000 . 1_645 no H44A H1B 2.4400 . 2_565 no H44A H34B 2.2800 . 2_565 no H44B C37 3.0800 . 1_545 no H44B H18C 2.4500 . 1_545 no H44B H37B 2.5000 . 1_545 no H46A C8 3.0300 . 1_645 no H46A C9 3.0200 . 1_645 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C1 H1 O4 0.9500 2.3200 3.218(5) 157.00 1_465 yes C13 H13 N1 1.0000 2.4900 2.935(5) 106.00 . yes C16 H16 N1 1.0000 2.5300 2.894(5) 101.00 . yes C25 H25 N3 1.0000 2.4400 2.933(6) 110.00 . yes C28 H28 O2 1.0000 2.3600 3.345(4) 167.00 . yes C28 H28 N3 1.0000 2.4500 2.949(5) 110.00 . yes C31 H31A N2 0.9900 2.5900 3.305(5) 129.00 . yes # Loop Mechanism for Extra Tables(s) #loop_ #_publ_manuscript_incl_extra_item #'_geom_extra_tableA_col_1' #'_geom_extra_tableA_col_2' #'_geom_extra_tableA_col_3' #'_geom_extra_table_head_A' #'_geom_table_footnote_A' #'_geom_extra_tableB_col_1' #'_geom_extra_tableB_col_2' #'_geom_extra_tableB_col_3' #'_geom_extra_table_head_B' #'_geom_table_footnote_B' # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 # ? ? ? # #loop_ #_geom_extra_tableB_col_1 #_geom_extra_tableB_col_2 #_geom_extra_tableB_col_3 # ? ? ? # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; #===END