# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address 'Jianhua Cheng' ; Organometallic Chemistry Laboratory and Advanced Catalyst Research Team, RIKEN Advanced Science Institute 2-1 Hirosawa, Wako, Saitama 351-0198 (Japan) ; 'Zhaomin Hou' ;Organometallic Chemistry Laboratory and Advanced Catalyst Research Team, RIKEN Advanced Science Institute 2-1 Hirosawa, Wako, Saitama 351-0198 (Japan) ; _publ_contact_author_name 'Dr Zhaomin Hou' _publ_contact_author_email houz@riken.jp _publ_section_title ; Cationic terminal hydrido rare earth complexes bearing an amidinate ancillary ligand ; # Attachment '- CIF.cif' data_3-Lu _database_code_depnum_ccdc_archive 'CCDC 829248' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ((Ph-NCN)LuH(THF)3)(BPh4) _chemical_formula_moiety ? _chemical_formula_sum 'C67 H84 B Lu N2 O3' _chemical_properties_physical air-sensitive _exptl_crystal_recrystallization_method THF/Hexane _chemical_melting_point ? _diffrn_ambient_temperature 163(2) _chemical_formula_weight 1151.14 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' B B 0.0013 0.0007 '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' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? _symmetry_space_group_name_Hall '-P 2ybc' 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 20.966(6) _cell_length_b 11.804(3) _cell_length_c 27.217(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.748(5) _cell_angle_gamma 90.00 _cell_volume 6728(3) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 875 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 1.508 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5700 _exptl_absorpt_correction_T_max 0.7524 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35869 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11829 _reflns_number_gt 9644 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (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. EADP and SADI have been used for following atoms: EADP C2 C3 C4 C5 EADP C2' C3' C4' C5' EADP C6' C7' C8' C9' EADP C10 C11 C12 C13 C10' C11' C12' C13' SADI C42 C43 C42 C43' EADP C43 C43' EADP C63 > C68 Termianl Hydride (H1) was located by difference Fourier syntheses, while the coordinates and isotropic parameters were constrained. ; _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^)+(0.0672P)^2^+12.2743P] 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 11829 _refine_ls_number_parameters 644 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1327 _refine_ls_wR_factor_gt 0.1270 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 C2 C 0.760(2) 1.0665(17) 0.1551(8) 0.068(4) Uani 0.38(3) 1 d PD A 2 H2A H 0.7969 1.0671 0.1338 0.081 Uiso 0.38(3) 1 calc PR A 2 H2B H 0.7206 1.0569 0.1339 0.081 Uiso 0.38(3) 1 calc PR A 2 C3 C 0.7573(15) 1.1711(13) 0.1815(8) 0.068(4) Uani 0.38(3) 1 d PD A 2 H3A H 0.7821 1.2300 0.1649 0.081 Uiso 0.38(3) 1 calc PR A 2 H3B H 0.7125 1.1971 0.1826 0.081 Uiso 0.38(3) 1 calc PR A 2 C4 C 0.7820(11) 1.1535(16) 0.2273(10) 0.068(4) Uani 0.38(3) 1 d PD A 2 H4A H 0.7571 1.1962 0.2512 0.081 Uiso 0.38(3) 1 calc PR A 2 H4B H 0.8266 1.1810 0.2300 0.081 Uiso 0.38(3) 1 calc PR A 2 C5 C 0.7801(13) 1.0238(17) 0.2396(8) 0.068(4) Uani 0.38(3) 1 d PD A 2 H5A H 0.8216 0.9977 0.2544 0.081 Uiso 0.38(3) 1 calc PR A 2 H5B H 0.7461 1.0066 0.2625 0.081 Uiso 0.38(3) 1 calc PR A 2 C2' C 0.7589(14) 1.0721(15) 0.1639(6) 0.086(3) Uani 0.62(3) 1 d PD A 1 H2'1 H 0.7132 1.0855 0.1550 0.103 Uiso 0.62(3) 1 calc PR A 1 H2'2 H 0.7824 1.0674 0.1332 0.103 Uiso 0.62(3) 1 calc PR A 1 C3' C 0.7842(11) 1.1629(11) 0.1947(6) 0.086(3) Uani 0.62(3) 1 d PD A 1 H3'1 H 0.8269 1.1858 0.1844 0.103 Uiso 0.62(3) 1 calc PR A 1 H3'2 H 0.7556 1.2297 0.1924 0.103 Uiso 0.62(3) 1 calc PR A 1 C4' C 0.7880(8) 1.1211(15) 0.2423(5) 0.086(3) Uani 0.62(3) 1 d PD A 1 H4'1 H 0.7496 1.1438 0.2598 0.103 Uiso 0.62(3) 1 calc PR A 1 H4'2 H 0.8260 1.1527 0.2604 0.103 Uiso 0.62(3) 1 calc PR A 1 C5' C 0.7927(10) 0.9906(13) 0.2404(5) 0.086(3) Uani 0.62(3) 1 d PD A 1 H5'1 H 0.8375 0.9643 0.2445 0.103 Uiso 0.62(3) 1 calc PR A 1 H5'2 H 0.7668 0.9542 0.2654 0.103 Uiso 0.62(3) 1 calc PR A 1 C6 C 0.8293(7) 0.8679(14) 0.0648(5) 0.056(4) Uani 0.67(5) 1 d PD A 2 H6A H 0.8179 0.9480 0.0581 0.068 Uiso 0.67(5) 1 calc PR A 2 H6B H 0.7991 0.8181 0.0459 0.068 Uiso 0.67(5) 1 calc PR A 2 C7 C 0.8968(10) 0.8440(14) 0.0527(7) 0.069(5) Uani 0.67(5) 1 d PD A 2 H7A H 0.9021 0.7633 0.0439 0.083 Uiso 0.67(5) 1 calc PR A 2 H7B H 0.9094 0.8915 0.0248 0.083 Uiso 0.67(5) 1 calc PR A 2 C8 C 0.9361(5) 0.8724(19) 0.0983(9) 0.080(5) Uani 0.67(5) 1 d PD A 2 H8A H 0.9671 0.8111 0.1064 0.096 Uiso 0.67(5) 1 calc PR A 2 H8B H 0.9599 0.9439 0.0939 0.096 Uiso 0.67(5) 1 calc PR A 2 C9 C 0.8907(7) 0.885(3) 0.1376(6) 0.094(5) Uani 0.67(5) 1 d PD A 2 H9A H 0.9049 0.8396 0.1668 0.113 Uiso 0.67(5) 1 calc PR A 2 H9B H 0.8872 0.9651 0.1475 0.113 Uiso 0.67(5) 1 calc PR A 2 C6' C 0.8227(12) 0.874(4) 0.0675(18) 0.103(9) Uani 0.33(5) 1 d PD A 1 H6'1 H 0.8172 0.9567 0.0647 0.124 Uiso 0.33(5) 1 calc PR A 1 H6'2 H 0.7843 0.8368 0.0521 0.124 Uiso 0.33(5) 1 calc PR A 1 C7' C 0.881(2) 0.838(4) 0.0417(15) 0.103(9) Uani 0.33(5) 1 d PD A 1 H7'1 H 0.8753 0.7605 0.0279 0.124 Uiso 0.33(5) 1 calc PR A 1 H7'2 H 0.8898 0.8908 0.0147 0.124 Uiso 0.33(5) 1 calc PR A 1 C8' C 0.9326(12) 0.840(4) 0.081(2) 0.103(9) Uani 0.33(5) 1 d PD A 1 H8'1 H 0.9582 0.7700 0.0802 0.124 Uiso 0.33(5) 1 calc PR A 1 H8'2 H 0.9611 0.9057 0.0761 0.124 Uiso 0.33(5) 1 calc PR A 1 C9' C 0.9019(18) 0.850(4) 0.1288(15) 0.103(9) Uani 0.33(5) 1 d PD A 1 H9'1 H 0.9132 0.9234 0.1448 0.124 Uiso 0.33(5) 1 calc PR A 1 H9'2 H 0.9161 0.7880 0.1512 0.124 Uiso 0.33(5) 1 calc PR A 1 C10 C 0.832(2) 0.553(3) 0.1721(10) 0.114(2) Uani 0.279(11) 1 d PD A 2 H10A H 0.8705 0.5511 0.1522 0.137 Uiso 0.279(11) 1 calc PR A 2 H10B H 0.7946 0.5362 0.1499 0.137 Uiso 0.279(11) 1 calc PR A 2 C11 C 0.838(2) 0.465(2) 0.2096(12) 0.114(2) Uani 0.279(11) 1 d PD A 2 H11A H 0.8817 0.4330 0.2113 0.137 Uiso 0.279(11) 1 calc PR A 2 H11B H 0.8071 0.4033 0.2024 0.137 Uiso 0.279(11) 1 calc PR A 2 C12 C 0.8236(19) 0.525(2) 0.2578(10) 0.114(2) Uani 0.279(11) 1 d PD A 2 H12A H 0.7788 0.5127 0.2664 0.137 Uiso 0.279(11) 1 calc PR A 2 H12B H 0.8525 0.4987 0.2853 0.137 Uiso 0.279(11) 1 calc PR A 2 C13 C 0.836(3) 0.649(2) 0.2456(12) 0.114(2) Uani 0.279(11) 1 d PD A 2 H13A H 0.8061 0.6982 0.2631 0.137 Uiso 0.279(11) 1 calc PR A 2 H13B H 0.8801 0.6701 0.2561 0.137 Uiso 0.279(11) 1 calc PR A 2 C10' C 0.8686(8) 0.6001(10) 0.1608(5) 0.114(2) Uani 0.721(11) 1 d PD A 1 H10C H 0.9135 0.6236 0.1674 0.137 Uiso 0.721(11) 1 calc PR A 1 H10D H 0.8572 0.6097 0.1253 0.137 Uiso 0.721(11) 1 calc PR A 1 C11' C 0.8581(8) 0.4812(9) 0.1769(5) 0.114(2) Uani 0.721(11) 1 d PD A 1 H11C H 0.8971 0.4353 0.1735 0.137 Uiso 0.721(11) 1 calc PR A 1 H11D H 0.8226 0.4459 0.1570 0.137 Uiso 0.721(11) 1 calc PR A 1 C12' C 0.8416(8) 0.4903(10) 0.2305(5) 0.114(2) Uani 0.721(11) 1 d PD A 1 H12C H 0.8747 0.4537 0.2522 0.137 Uiso 0.721(11) 1 calc PR A 1 H12D H 0.7998 0.4545 0.2359 0.137 Uiso 0.721(11) 1 calc PR A 1 C13' C 0.8390(10) 0.6176(9) 0.2400(5) 0.114(2) Uani 0.721(11) 1 d PD A 1 H13C H 0.8048 0.6368 0.2624 0.137 Uiso 0.721(11) 1 calc PR A 1 H13D H 0.8803 0.6459 0.2543 0.137 Uiso 0.721(11) 1 calc PR A 1 C14 C 0.6469(2) 0.7452(4) 0.09965(16) 0.0347(10) Uani 1 1 d . . . C15 C 0.5883(2) 0.7169(4) 0.06905(18) 0.0385(10) Uani 1 1 d . . . C16 C 0.5915(2) 0.6523(4) 0.02697(19) 0.0449(11) Uani 1 1 d . . . H16 H 0.6316 0.6240 0.0176 0.054 Uiso 1 1 calc R . . C17 C 0.5366(3) 0.6281(4) -0.0018(2) 0.0560(14) Uani 1 1 d . . . H17 H 0.5397 0.5847 -0.0310 0.067 Uiso 1 1 calc R . . C18 C 0.4778(3) 0.6665(5) 0.0115(3) 0.0616(16) Uani 1 1 d . . . H18 H 0.4403 0.6491 -0.0080 0.074 Uiso 1 1 calc R . . C19 C 0.4743(3) 0.7301(5) 0.0533(2) 0.0579(15) Uani 1 1 d . . . H19 H 0.4340 0.7570 0.0628 0.069 Uiso 1 1 calc R . . C20 C 0.5284(2) 0.7555(5) 0.0818(2) 0.0486(12) Uani 1 1 d . . . H20 H 0.5249 0.8000 0.1106 0.058 Uiso 1 1 calc R . . C21 C 0.6165(2) 0.9418(4) 0.11162(17) 0.0383(10) Uani 1 1 d . . . C22 C 0.6107(2) 0.9914(4) 0.06507(17) 0.0371(10) Uani 1 1 d . . . C23 C 0.6491(2) 0.9533(4) 0.02242(18) 0.0420(11) Uani 1 1 d . . . H23 H 0.6725 0.8825 0.0325 0.050 Uiso 1 1 calc R . . C24 C 0.6072(3) 0.9269(5) -0.0236(2) 0.0575(14) Uani 1 1 d . . . H24A H 0.6341 0.9021 -0.0500 0.086 Uiso 1 1 calc R . . H24B H 0.5836 0.9952 -0.0341 0.086 Uiso 1 1 calc R . . H24C H 0.5769 0.8667 -0.0163 0.086 Uiso 1 1 calc R . . C25 C 0.6985(3) 1.0432(5) 0.0109(2) 0.0540(13) Uani 1 1 d . . . H25A H 0.7235 1.0174 -0.0164 0.081 Uiso 1 1 calc R . . H25B H 0.7269 1.0559 0.0400 0.081 Uiso 1 1 calc R . . H25C H 0.6766 1.1141 0.0018 0.081 Uiso 1 1 calc R . . C26 C 0.5695(2) 1.0821(4) 0.0581(2) 0.0481(12) Uani 1 1 d . . . H26 H 0.5643 1.1148 0.0263 0.058 Uiso 1 1 calc R . . C27 C 0.5358(2) 1.1264(5) 0.0956(2) 0.0572(15) Uani 1 1 d . . . H27 H 0.5074 1.1882 0.0898 0.069 Uiso 1 1 calc R . . C28 C 0.5439(3) 1.0797(5) 0.1415(2) 0.0604(15) Uani 1 1 d . . . H28 H 0.5215 1.1114 0.1677 0.073 Uiso 1 1 calc R . . C29 C 0.5841(2) 0.9873(5) 0.15113(19) 0.0502(13) Uani 1 1 d . . . C30 C 0.5902(3) 0.9392(6) 0.2023(2) 0.0716(19) Uani 1 1 d . . . H30 H 0.6299 0.8919 0.2047 0.086 Uiso 1 1 calc R . . C31 C 0.5345(5) 0.8631(7) 0.2138(3) 0.100(3) Uani 1 1 d . . . H31A H 0.5407 0.8334 0.2473 0.149 Uiso 1 1 calc R . . H31B H 0.5321 0.7999 0.1904 0.149 Uiso 1 1 calc R . . H31C H 0.4948 0.9067 0.2111 0.149 Uiso 1 1 calc R . . C32 C 0.5973(4) 1.0321(9) 0.2415(3) 0.106(3) Uani 1 1 d . . . H32A H 0.6015 0.9973 0.2742 0.159 Uiso 1 1 calc R . . H32B H 0.5595 1.0811 0.2396 0.159 Uiso 1 1 calc R . . H32C H 0.6354 1.0774 0.2358 0.159 Uiso 1 1 calc R . . C33 C 0.6891(2) 0.5541(4) 0.09776(18) 0.0414(11) Uani 1 1 d . . . C34 C 0.6467(2) 0.4860(4) 0.1231(2) 0.0479(12) Uani 1 1 d . . . C35 C 0.6060(3) 0.5303(5) 0.1634(2) 0.0628(15) Uani 1 1 d . . . H35 H 0.6113 0.6144 0.1650 0.075 Uiso 1 1 calc R . . C36 C 0.6292(5) 0.4812(8) 0.2127(3) 0.106(3) Uani 1 1 d . . . H36A H 0.6025 0.5100 0.2385 0.159 Uiso 1 1 calc R . . H36B H 0.6737 0.5035 0.2198 0.159 Uiso 1 1 calc R . . H36C H 0.6262 0.3984 0.2114 0.159 Uiso 1 1 calc R . . C37 C 0.5351(3) 0.5044(6) 0.1527(3) 0.081(2) Uani 1 1 d . . . H37A H 0.5103 0.5346 0.1794 0.121 Uiso 1 1 calc R . . H37B H 0.5289 0.4223 0.1504 0.121 Uiso 1 1 calc R . . H37C H 0.5208 0.5399 0.1216 0.121 Uiso 1 1 calc R . . C38 C 0.6427(3) 0.3714(5) 0.1109(2) 0.0625(16) Uani 1 1 d . . . H38 H 0.6139 0.3243 0.1275 0.075 Uiso 1 1 calc R . . C39 C 0.6789(3) 0.3250(5) 0.0757(3) 0.0686(18) Uani 1 1 d . . . H39 H 0.6746 0.2470 0.0676 0.082 Uiso 1 1 calc R . . C40 C 0.7212(3) 0.3909(5) 0.0525(2) 0.0603(15) Uani 1 1 d . . . H40 H 0.7465 0.3576 0.0283 0.072 Uiso 1 1 calc R . . C41 C 0.7288(3) 0.5056(4) 0.0630(2) 0.0509(13) Uani 1 1 d . C . C42 C 0.7790(3) 0.5743(5) 0.0380(2) 0.0639(16) Uani 1 1 d D . . H42 H 0.7822 0.6562 0.0471 0.077 Uiso 1 1 calc R B 1 C43 C 0.7553(4) 0.6298(10) -0.0105(3) 0.081(3) Uani 0.824(16) 1 d PD C 2 H43A H 0.7902 0.6725 -0.0244 0.121 Uiso 0.824(16) 1 calc PR C 2 H43B H 0.7199 0.6812 -0.0043 0.121 Uiso 0.824(16) 1 calc PR C 2 H43C H 0.7406 0.5710 -0.0338 0.121 Uiso 0.824(16) 1 calc PR C 2 C43' C 0.7527(19) 0.546(5) -0.0168(9) 0.081(3) Uani 0.176(16) 1 d PD C 1 H43D H 0.7790 0.5851 -0.0403 0.121 Uiso 0.176(16) 1 calc PR C 1 H43E H 0.7084 0.5723 -0.0212 0.121 Uiso 0.176(16) 1 calc PR C 1 H43F H 0.7545 0.4643 -0.0223 0.121 Uiso 0.176(16) 1 calc PR C 1 C44 C 0.8412(3) 0.5121(6) 0.0321(3) 0.084(2) Uani 1 1 d . C . H44A H 0.8712 0.5617 0.0158 0.126 Uiso 1 1 calc R . . H44B H 0.8333 0.4440 0.0121 0.126 Uiso 1 1 calc R . . H44C H 0.8594 0.4902 0.0646 0.126 Uiso 1 1 calc R . . C45 C 0.0530(2) 0.3742(4) 0.11374(18) 0.0451(11) Uani 1 1 d . . . C46 C 0.0204(3) 0.4437(5) 0.0798(2) 0.0558(13) Uani 1 1 d . . . H46 H -0.0171 0.4152 0.0631 0.067 Uiso 1 1 calc R . . C47 C 0.0404(3) 0.5536(5) 0.0691(2) 0.0701(17) Uani 1 1 d . . . H47 H 0.0166 0.5977 0.0455 0.084 Uiso 1 1 calc R . . C48 C 0.0936(4) 0.5975(5) 0.0920(3) 0.075(2) Uani 1 1 d . . . H48 H 0.1072 0.6721 0.0846 0.090 Uiso 1 1 calc R . . C49 C 0.1277(3) 0.5326(6) 0.1263(3) 0.0757(19) Uani 1 1 d . . . H49 H 0.1652 0.5626 0.1424 0.091 Uiso 1 1 calc R . . C50 C 0.1077(3) 0.4241(5) 0.1374(2) 0.0616(15) Uani 1 1 d . . . H50 H 0.1314 0.3817 0.1617 0.074 Uiso 1 1 calc R . . C51 C 0.0078(2) 0.2426(4) 0.18490(18) 0.0408(11) Uani 1 1 d . . . C52 C 0.0121(3) 0.3322(5) 0.2161(2) 0.0664(17) Uani 1 1 d . . . H52 H 0.0296 0.4012 0.2049 0.080 Uiso 1 1 calc R . . C53 C -0.0083(4) 0.3266(6) 0.2645(2) 0.079(2) Uani 1 1 d . . . H53 H -0.0045 0.3923 0.2845 0.095 Uiso 1 1 calc R . . C54 C -0.0327(3) 0.2336(6) 0.2832(2) 0.0621(16) Uani 1 1 d . . . H54 H -0.0453 0.2304 0.3162 0.075 Uiso 1 1 calc R . . C55 C -0.0389(4) 0.1412(6) 0.2520(3) 0.088(2) Uani 1 1 d . . . H55 H -0.0563 0.0727 0.2638 0.105 Uiso 1 1 calc R . . C56 C -0.0201(4) 0.1463(5) 0.2039(3) 0.079(2) Uani 1 1 d . . . H56 H -0.0266 0.0820 0.1833 0.095 Uiso 1 1 calc R . . C57 C -0.0289(2) 0.2075(4) 0.08966(19) 0.0425(11) Uani 1 1 d . . . C58 C -0.0928(3) 0.2265(4) 0.0994(2) 0.0493(12) Uani 1 1 d . . . H58 H -0.1025 0.2572 0.1304 0.059 Uiso 1 1 calc R . . C59 C -0.1428(3) 0.2023(5) 0.0655(2) 0.0575(15) Uani 1 1 d . . . H59 H -0.1857 0.2161 0.0737 0.069 Uiso 1 1 calc R . . C60 C -0.1302(3) 0.1583(5) 0.0201(2) 0.0612(15) Uani 1 1 d . . . H60 H -0.1640 0.1422 -0.0033 0.073 Uiso 1 1 calc R . . C61 C -0.0690(3) 0.1384(6) 0.0096(2) 0.0640(15) Uani 1 1 d . . . H61 H -0.0596 0.1087 -0.0217 0.077 Uiso 1 1 calc R . . C62 C -0.0195(3) 0.1608(5) 0.0440(2) 0.0579(14) Uani 1 1 d . . . H62 H 0.0229 0.1432 0.0358 0.069 Uiso 1 1 calc R . . C63 C 0.0909(2) 0.1526(4) 0.1198(2) 0.0891(9) Uani 1 1 d G . . C64 C 0.1408(2) 0.1840(3) 0.0908(2) 0.0891(9) Uani 1 1 d G . . H64 H 0.1422 0.2583 0.0775 0.107 Uiso 1 1 calc R . . C65 C 0.1886(2) 0.1066(4) 0.08128(19) 0.0891(9) Uani 1 1 d G . . H65 H 0.2227 0.1281 0.0615 0.107 Uiso 1 1 calc R . . C66 C 0.1866(2) -0.0021(3) 0.10075(19) 0.0891(9) Uani 1 1 d G . . H66 H 0.2193 -0.0550 0.0943 0.107 Uiso 1 1 calc R . . C67 C 0.1367(2) -0.0335(3) 0.12972(19) 0.0891(9) Uani 1 1 d G . . H67 H 0.1353 -0.1078 0.1430 0.107 Uiso 1 1 calc R . . C68 C 0.0888(2) 0.0439(4) 0.13922(19) 0.0891(9) Uani 1 1 d G . . H68 H 0.0547 0.0224 0.1590 0.107 Uiso 1 1 calc R . . B1 B 0.0306(3) 0.2447(5) 0.1280(2) 0.0420(12) Uani 1 1 d . . . N1 N 0.65758(17) 0.8462(3) 0.12121(13) 0.0359(8) Uani 1 1 d . . . N2 N 0.69559(17) 0.6720(3) 0.10847(14) 0.0372(8) Uani 1 1 d . . . O1 O 0.76641(19) 0.9704(3) 0.19107(13) 0.0556(9) Uani 1 1 d . . . O2 O 0.82940(16) 0.8431(4) 0.11710(16) 0.0587(10) Uani 1 1 d . . . O3 O 0.8255(2) 0.6638(4) 0.19097(17) 0.0820(14) Uani 1 1 d . . . Lu1 Lu 0.747611(9) 0.788085(17) 0.165282(8) 0.04156(9) Uani 1 1 d . A . H1 H 0.7126 0.7475 0.2301 0.050 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 C2 0.104(8) 0.036(6) 0.062(7) -0.001(4) -0.010(5) 0.004(5) C3 0.104(8) 0.036(6) 0.062(7) -0.001(4) -0.010(5) 0.004(5) C4 0.104(8) 0.036(6) 0.062(7) -0.001(4) -0.010(5) 0.004(5) C5 0.104(8) 0.036(6) 0.062(7) -0.001(4) -0.010(5) 0.004(5) C2' 0.130(7) 0.068(5) 0.059(4) -0.005(3) -0.020(4) -0.022(4) C3' 0.130(7) 0.068(5) 0.059(4) -0.005(3) -0.020(4) -0.022(4) C4' 0.130(7) 0.068(5) 0.059(4) -0.005(3) -0.020(4) -0.022(4) C5' 0.130(7) 0.068(5) 0.059(4) -0.005(3) -0.020(4) -0.022(4) C6 0.079(8) 0.043(6) 0.048(7) 0.013(5) 0.014(5) -0.004(5) C7 0.059(10) 0.066(8) 0.084(10) 0.010(7) 0.029(8) -0.011(7) C8 0.049(6) 0.084(10) 0.111(13) -0.017(8) 0.026(7) -0.016(6) C9 0.030(6) 0.138(14) 0.115(10) -0.052(10) 0.012(6) -0.014(7) C6' 0.041(9) 0.104(14) 0.17(2) -0.070(16) 0.036(10) -0.020(8) C7' 0.041(9) 0.104(14) 0.17(2) -0.070(16) 0.036(10) -0.020(8) C8' 0.041(9) 0.104(14) 0.17(2) -0.070(16) 0.036(10) -0.020(8) C9' 0.041(9) 0.104(14) 0.17(2) -0.070(16) 0.036(10) -0.020(8) C10 0.162(6) 0.070(4) 0.104(5) -0.013(3) -0.052(5) 0.032(4) C11 0.162(6) 0.070(4) 0.104(5) -0.013(3) -0.052(5) 0.032(4) C12 0.162(6) 0.070(4) 0.104(5) -0.013(3) -0.052(5) 0.032(4) C13 0.162(6) 0.070(4) 0.104(5) -0.013(3) -0.052(5) 0.032(4) C10' 0.162(6) 0.070(4) 0.104(5) -0.013(3) -0.052(5) 0.032(4) C11' 0.162(6) 0.070(4) 0.104(5) -0.013(3) -0.052(5) 0.032(4) C12' 0.162(6) 0.070(4) 0.104(5) -0.013(3) -0.052(5) 0.032(4) C13' 0.162(6) 0.070(4) 0.104(5) -0.013(3) -0.052(5) 0.032(4) C14 0.035(2) 0.035(2) 0.035(2) 0.0006(19) 0.0028(19) -0.0027(18) C15 0.035(2) 0.032(2) 0.048(3) 0.002(2) -0.002(2) -0.0017(18) C16 0.044(3) 0.034(3) 0.056(3) -0.003(2) -0.003(2) 0.000(2) C17 0.069(4) 0.035(3) 0.062(3) -0.002(2) -0.020(3) -0.009(3) C18 0.050(3) 0.044(3) 0.088(5) 0.012(3) -0.025(3) -0.010(2) C19 0.039(3) 0.050(3) 0.084(4) 0.010(3) -0.005(3) -0.005(2) C20 0.038(3) 0.050(3) 0.058(3) 0.001(3) 0.001(2) -0.002(2) C21 0.032(2) 0.036(2) 0.046(3) -0.007(2) -0.0040(19) 0.0040(19) C22 0.034(2) 0.028(2) 0.049(3) -0.005(2) -0.001(2) -0.0011(18) C23 0.047(3) 0.034(2) 0.044(3) 0.000(2) -0.002(2) 0.003(2) C24 0.074(4) 0.047(3) 0.050(3) -0.003(3) -0.011(3) 0.001(3) C25 0.059(3) 0.048(3) 0.056(3) 0.001(3) 0.009(3) -0.006(2) C26 0.042(3) 0.037(3) 0.065(3) 0.002(2) -0.003(2) 0.003(2) C27 0.043(3) 0.041(3) 0.087(4) -0.011(3) -0.006(3) 0.014(2) C28 0.045(3) 0.062(4) 0.075(4) -0.029(3) 0.002(3) 0.013(3) C29 0.040(3) 0.059(3) 0.051(3) -0.014(3) 0.000(2) 0.007(2) C30 0.063(4) 0.106(5) 0.047(3) -0.015(3) 0.009(3) 0.030(4) C31 0.148(8) 0.091(6) 0.059(4) 0.001(4) 0.008(5) -0.015(5) C32 0.098(6) 0.166(9) 0.054(4) -0.036(5) 0.011(4) -0.033(6) C33 0.043(3) 0.032(2) 0.049(3) 0.001(2) -0.007(2) 0.002(2) C34 0.046(3) 0.039(3) 0.057(3) 0.006(2) -0.009(2) -0.005(2) C35 0.075(4) 0.055(3) 0.059(4) 0.008(3) 0.011(3) -0.019(3) C36 0.141(8) 0.116(7) 0.062(5) 0.013(5) 0.009(5) -0.027(6) C37 0.071(4) 0.071(4) 0.104(5) 0.005(4) 0.032(4) -0.018(3) C38 0.056(3) 0.043(3) 0.088(4) 0.009(3) -0.010(3) -0.011(3) C39 0.058(4) 0.040(3) 0.106(5) -0.014(3) -0.019(4) 0.004(3) C40 0.053(3) 0.048(3) 0.079(4) -0.013(3) -0.006(3) 0.011(3) C41 0.052(3) 0.039(3) 0.061(3) 0.000(2) -0.005(3) 0.010(2) C42 0.070(4) 0.046(3) 0.078(4) 0.003(3) 0.020(3) 0.011(3) C43 0.070(5) 0.092(8) 0.080(5) 0.019(6) 0.006(4) -0.004(5) C43' 0.070(5) 0.092(8) 0.080(5) 0.019(6) 0.006(4) -0.004(5) C44 0.061(4) 0.078(5) 0.115(6) -0.005(4) 0.016(4) -0.002(3) C45 0.041(3) 0.049(3) 0.046(3) -0.008(2) 0.011(2) -0.006(2) C46 0.063(3) 0.048(3) 0.057(3) 0.004(3) 0.005(3) -0.006(3) C47 0.093(5) 0.050(3) 0.069(4) 0.009(3) 0.017(4) 0.000(3) C48 0.105(5) 0.050(4) 0.074(4) -0.007(3) 0.036(4) -0.021(4) C49 0.076(4) 0.073(4) 0.079(5) -0.023(4) 0.014(4) -0.032(4) C50 0.059(3) 0.063(4) 0.063(4) -0.004(3) 0.004(3) -0.015(3) C51 0.036(2) 0.039(2) 0.047(3) -0.001(2) 0.001(2) 0.001(2) C52 0.105(5) 0.048(3) 0.048(3) -0.004(3) 0.021(3) -0.009(3) C53 0.115(6) 0.069(4) 0.055(4) -0.017(3) 0.010(4) -0.008(4) C54 0.058(3) 0.086(5) 0.043(3) 0.013(3) 0.004(3) 0.001(3) C55 0.120(6) 0.059(4) 0.088(5) 0.026(4) 0.048(5) 0.010(4) C56 0.116(6) 0.047(4) 0.077(5) 0.004(3) 0.040(4) 0.004(4) C57 0.043(3) 0.037(2) 0.048(3) 0.005(2) 0.001(2) -0.001(2) C58 0.051(3) 0.040(3) 0.057(3) 0.001(2) -0.002(2) 0.006(2) C59 0.041(3) 0.052(3) 0.078(4) 0.014(3) -0.007(3) -0.001(2) C60 0.064(4) 0.060(4) 0.057(4) 0.016(3) -0.018(3) -0.016(3) C61 0.069(4) 0.076(4) 0.047(3) 0.001(3) -0.003(3) -0.017(3) C62 0.053(3) 0.074(4) 0.046(3) -0.002(3) 0.001(2) -0.008(3) C63 0.086(2) 0.0778(19) 0.106(2) 0.0073(17) 0.0326(17) 0.0285(16) C64 0.086(2) 0.0778(19) 0.106(2) 0.0073(17) 0.0326(17) 0.0285(16) C65 0.086(2) 0.0778(19) 0.106(2) 0.0073(17) 0.0326(17) 0.0285(16) C66 0.086(2) 0.0778(19) 0.106(2) 0.0073(17) 0.0326(17) 0.0285(16) C67 0.086(2) 0.0778(19) 0.106(2) 0.0073(17) 0.0326(17) 0.0285(16) C68 0.086(2) 0.0778(19) 0.106(2) 0.0073(17) 0.0326(17) 0.0285(16) B1 0.038(3) 0.043(3) 0.044(3) -0.002(2) -0.001(2) -0.002(2) N1 0.0346(19) 0.036(2) 0.037(2) -0.0017(17) 0.0001(16) 0.0003(16) N2 0.034(2) 0.0315(19) 0.045(2) -0.0001(17) -0.0023(17) 0.0013(15) O1 0.070(2) 0.053(2) 0.043(2) -0.0062(17) -0.0037(18) -0.0095(18) O2 0.0378(19) 0.071(3) 0.068(3) -0.007(2) 0.0046(18) -0.0096(18) O3 0.101(4) 0.065(3) 0.076(3) 0.001(2) -0.032(3) 0.037(3) Lu1 0.03853(13) 0.04060(14) 0.04480(14) 0.00394(9) -0.00569(9) -0.00176(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 C2 C3 1.430(16) . ? C2 O1 1.50(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.344(17) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.568(16) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 O1 1.48(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C2' O1 1.41(2) . ? C2' C3' 1.447(14) . ? C2' H2'1 0.9900 . ? C2' H2'2 0.9900 . ? C3' C4' 1.386(14) . ? C3' H3'1 0.9900 . ? C3' H3'2 0.9900 . ? C4' C5' 1.545(14) . ? C4' H4'1 0.9900 . ? C4' H4'2 0.9900 . ? C5' O1 1.446(14) . ? C5' H5'1 0.9900 . ? C5' H5'2 0.9900 . ? C6 O2 1.452(14) . ? C6 C7 1.495(12) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.494(14) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.473(13) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O2 1.462(14) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C6' O2 1.40(5) . ? C6' C7' 1.496(18) . ? C6' H6'1 0.9900 . ? C6' H6'2 0.9900 . ? C7' C8' 1.49(2) . ? C7' H7'1 0.9900 . ? C7' H7'2 0.9900 . ? C8' C9' 1.48(2) . ? C8' H8'1 0.9900 . ? C8' H8'2 0.9900 . ? C9' O2 1.54(4) . ? C9' H9'1 0.9900 . ? C9' H9'2 0.9900 . ? C10 O3 1.41(3) . ? C10 C11 1.46(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.53(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.52(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O3 1.50(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C10' O3 1.459(14) . ? C10' C11' 1.489(18) . ? C10' H10C 0.9900 . ? C10' H10D 0.9900 . ? C11' C12' 1.518(18) . ? C11' H11C 0.9900 . ? C11' H11D 0.9900 . ? C12' C13' 1.526(15) . ? C12' H12C 0.9900 . ? C12' H12D 0.9900 . ? C13' O3 1.457(14) . ? C13' H13C 0.9900 . ? C13' H13D 0.9900 . ? C14 N1 1.343(6) . ? C14 N2 1.351(6) . ? C14 C15 1.489(6) . ? C14 Lu1 2.747(5) . ? C15 C16 1.381(7) . ? C15 C20 1.395(7) . ? C16 C17 1.391(7) . ? C16 H16 0.9500 . ? C17 C18 1.379(8) . ? C17 H17 0.9500 . ? C18 C19 1.367(9) . ? C18 H18 0.9500 . ? C19 C20 1.376(8) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.396(7) . ? C21 C29 1.406(7) . ? C21 N1 1.435(6) . ? C22 C26 1.383(6) . ? C22 C23 1.512(6) . ? C23 C25 1.525(7) . ? C23 C24 1.528(7) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.372(8) . ? C26 H26 0.9500 . ? C27 C28 1.369(8) . ? C27 H27 0.9500 . ? C28 C29 1.396(8) . ? C28 H28 0.9500 . ? C29 C30 1.505(8) . ? C30 C31 1.518(10) . ? C30 C32 1.532(10) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.405(7) . ? C33 C41 1.410(7) . ? C33 N2 1.427(6) . ? C34 C38 1.395(8) . ? C34 C35 1.513(8) . ? C35 C36 1.519(9) . ? C35 C37 1.532(9) . ? C35 H35 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.364(9) . ? C38 H38 0.9500 . ? C39 C40 1.359(9) . ? C39 H39 0.9500 . ? C40 C41 1.391(7) . ? C40 H40 0.9500 . ? C41 C42 1.516(8) . ? C42 C44 1.512(8) . ? C42 C43 1.535(10) . ? C42 C43' 1.60(2) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C43' H43D 0.9800 . ? C43' H43E 0.9800 . ? C43' H43F 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.390(8) . ? C45 C50 1.416(7) . ? C45 B1 1.652(8) . ? C46 C47 1.398(8) . ? C46 H46 0.9500 . ? C47 C48 1.354(10) . ? C47 H47 0.9500 . ? C48 C49 1.381(10) . ? C48 H48 0.9500 . ? C49 C50 1.386(9) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.357(8) . ? C51 C56 1.389(8) . ? C51 B1 1.642(8) . ? C52 C53 1.405(9) . ? C52 H52 0.9500 . ? C53 C54 1.323(9) . ? C53 H53 0.9500 . ? C54 C55 1.384(10) . ? C54 H54 0.9500 . ? C55 C56 1.387(9) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C62 1.382(7) . ? C57 C58 1.394(7) . ? C57 B1 1.648(7) . ? C58 C59 1.394(8) . ? C58 H58 0.9500 . ? C59 C60 1.376(9) . ? C59 H59 0.9500 . ? C60 C61 1.349(9) . ? C60 H60 0.9500 . ? C61 C62 1.390(8) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 C64 1.3900 . ? C63 C68 1.3900 . ? C63 B1 1.691(6) . ? C64 C65 1.3900 . ? C64 H64 0.9500 . ? C65 C66 1.3900 . ? C65 H65 0.9500 . ? C66 C67 1.3900 . ? C66 H66 0.9500 . ? C67 C68 1.3900 . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? N1 Lu1 2.293(4) . ? N2 Lu1 2.301(4) . ? O1 Lu1 2.292(4) . ? O2 Lu1 2.302(4) . ? O3 Lu1 2.279(4) . ? Lu1 H1 2.0012(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 C3 C2 O1 109.2(13) . . ? C3 C2 H2A 109.8 . . ? O1 C2 H2A 109.8 . . ? C3 C2 H2B 109.8 . . ? O1 C2 H2B 109.8 . . ? H2A C2 H2B 108.3 . . ? C4 C3 C2 108.1(14) . . ? C4 C3 H3A 110.1 . . ? C2 C3 H3A 110.1 . . ? C4 C3 H3B 110.1 . . ? C2 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? C3 C4 C5 109.6(12) . . ? C3 C4 H4A 109.7 . . ? C5 C4 H4A 109.7 . . ? C3 C4 H4B 109.7 . . ? C5 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? O1 C5 C4 103.4(12) . . ? O1 C5 H5A 111.1 . . ? C4 C5 H5A 111.1 . . ? O1 C5 H5B 111.1 . . ? C4 C5 H5B 111.1 . . ? H5A C5 H5B 109.1 . . ? O1 C2' C3' 107.2(12) . . ? O1 C2' H2'1 110.3 . . ? C3' C2' H2'1 110.3 . . ? O1 C2' H2'2 110.3 . . ? C3' C2' H2'2 110.3 . . ? H2'1 C2' H2'2 108.5 . . ? C4' C3' C2' 106.4(11) . . ? C4' C3' H3'1 110.5 . . ? C2' C3' H3'1 110.5 . . ? C4' C3' H3'2 110.5 . . ? C2' C3' H3'2 110.5 . . ? H3'1 C3' H3'2 108.6 . . ? C3' C4' C5' 108.9(10) . . ? C3' C4' H4'1 109.9 . . ? C5' C4' H4'1 109.9 . . ? C3' C4' H4'2 109.9 . . ? C5' C4' H4'2 109.9 . . ? H4'1 C4' H4'2 108.3 . . ? O1 C5' C4' 100.0(9) . . ? O1 C5' H5'1 111.8 . . ? C4' C5' H5'1 111.8 . . ? O1 C5' H5'2 111.8 . . ? C4' C5' H5'2 111.8 . . ? H5'1 C5' H5'2 109.5 . . ? O2 C6 C7 102.8(8) . . ? O2 C6 H6A 111.2 . . ? C7 C6 H6A 111.2 . . ? O2 C6 H6B 111.2 . . ? C7 C6 H6B 111.2 . . ? H6A C6 H6B 109.1 . . ? C8 C7 C6 105.4(9) . . ? C8 C7 H7A 110.7 . . ? C6 C7 H7A 110.7 . . ? C8 C7 H7B 110.7 . . ? C6 C7 H7B 110.7 . . ? H7A C7 H7B 108.8 . . ? C9 C8 C7 106.0(8) . . ? C9 C8 H8A 110.5 . . ? C7 C8 H8A 110.5 . . ? C9 C8 H8B 110.5 . . ? C7 C8 H8B 110.5 . . ? H8A C8 H8B 108.7 . . ? O2 C9 C8 106.0(9) . . ? O2 C9 H9A 110.5 . . ? C8 C9 H9A 110.5 . . ? O2 C9 H9B 110.5 . . ? C8 C9 H9B 110.5 . . ? H9A C9 H9B 108.7 . . ? O2 C6' C7' 110(3) . . ? O2 C6' H6'1 109.8 . . ? C7' C6' H6'1 109.8 . . ? O2 C6' H6'2 109.8 . . ? C7' C6' H6'2 109.8 . . ? H6'1 C6' H6'2 108.2 . . ? C8' C7' C6' 103.8(17) . . ? C8' C7' H7'1 111.0 . . ? C6' C7' H7'1 111.0 . . ? C8' C7' H7'2 111.0 . . ? C6' C7' H7'2 111.0 . . ? H7'1 C7' H7'2 109.0 . . ? C9' C8' C7' 107.5(17) . . ? C9' C8' H8'1 110.2 . . ? C7' C8' H8'1 110.2 . . ? C9' C8' H8'2 110.2 . . ? C7' C8' H8'2 110.2 . . ? H8'1 C8' H8'2 108.5 . . ? C8' C9' O2 106.2(18) . . ? C8' C9' H9'1 110.5 . . ? O2 C9' H9'1 110.5 . . ? C8' C9' H9'2 110.5 . . ? O2 C9' H9'2 110.5 . . ? H9'1 C9' H9'2 108.7 . . ? O3 C10 C11 114.3(19) . . ? O3 C10 H10A 108.7 . . ? C11 C10 H10A 108.7 . . ? O3 C10 H10B 108.7 . . ? C11 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C10 C11 C12 104.9(17) . . ? C10 C11 H11A 110.8 . . ? C12 C11 H11A 110.8 . . ? C10 C11 H11B 110.8 . . ? C12 C11 H11B 110.8 . . ? H11A C11 H11B 108.8 . . ? C13 C12 C11 102.4(19) . . ? C13 C12 H12A 111.3 . . ? C11 C12 H12A 111.3 . . ? C13 C12 H12B 111.3 . . ? C11 C12 H12B 111.3 . . ? H12A C12 H12B 109.2 . . ? O3 C13 C12 108.0(19) . . ? O3 C13 H13A 110.1 . . ? C12 C13 H13A 110.1 . . ? O3 C13 H13B 110.1 . . ? C12 C13 H13B 110.1 . . ? H13A C13 H13B 108.4 . . ? O3 C10' C11' 102.5(12) . . ? O3 C10' H10C 111.3 . . ? C11' C10' H10C 111.3 . . ? O3 C10' H10D 111.3 . . ? C11' C10' H10D 111.3 . . ? H10C C10' H10D 109.2 . . ? C10' C11' C12' 105.0(9) . . ? C10' C11' H11C 110.7 . . ? C12' C11' H11C 110.7 . . ? C10' C11' H11D 110.7 . . ? C12' C11' H11D 110.7 . . ? H11C C11' H11D 108.8 . . ? C11' C12' C13' 104.2(11) . . ? C11' C12' H12C 110.9 . . ? C13' C12' H12C 110.9 . . ? C11' C12' H12D 110.9 . . ? C13' C12' H12D 110.9 . . ? H12C C12' H12D 108.9 . . ? O3 C13' C12' 102.7(10) . . ? O3 C13' H13C 111.2 . . ? C12' C13' H13C 111.2 . . ? O3 C13' H13D 111.2 . . ? C12' C13' H13D 111.2 . . ? H13C C13' H13D 109.1 . . ? N1 C14 N2 112.4(4) . . ? N1 C14 C15 124.0(4) . . ? N2 C14 C15 123.6(4) . . ? N1 C14 Lu1 56.3(2) . . ? N2 C14 Lu1 56.7(2) . . ? C15 C14 Lu1 173.3(3) . . ? C16 C15 C20 117.8(5) . . ? C16 C15 C14 121.0(4) . . ? C20 C15 C14 121.1(4) . . ? C15 C16 C17 120.6(5) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C18 C17 C16 120.7(5) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C17 119.0(5) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 120.8(5) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C15 121.2(5) . . ? C19 C20 H20 119.4 . . ? C15 C20 H20 119.4 . . ? C22 C21 C29 120.6(4) . . ? C22 C21 N1 121.3(4) . . ? C29 C21 N1 118.0(4) . . ? C26 C22 C21 118.4(4) . . ? C26 C22 C23 118.5(4) . . ? C21 C22 C23 123.1(4) . . ? C22 C23 C25 110.0(4) . . ? C22 C23 C24 112.5(4) . . ? C25 C23 C24 110.1(4) . . ? C22 C23 H23 108.0 . . ? C25 C23 H23 108.0 . . ? C24 C23 H23 108.0 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C22 122.2(5) . . ? C27 C26 H26 118.9 . . ? C22 C26 H26 118.9 . . ? C28 C27 C26 118.7(5) . . ? C28 C27 H27 120.7 . . ? C26 C27 H27 120.7 . . ? C27 C28 C29 122.2(5) . . ? C27 C28 H28 118.9 . . ? C29 C28 H28 118.9 . . ? C28 C29 C21 117.7(5) . . ? C28 C29 C30 119.5(5) . . ? C21 C29 C30 122.8(5) . . ? C29 C30 C31 112.4(6) . . ? C29 C30 C32 112.0(6) . . ? C31 C30 C32 109.3(5) . . ? C29 C30 H30 107.6 . . ? C31 C30 H30 107.6 . . ? C32 C30 H30 107.6 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C41 120.3(4) . . ? C34 C33 N2 120.9(4) . . ? C41 C33 N2 118.7(4) . . ? C38 C34 C33 118.0(5) . . ? C38 C34 C35 118.6(5) . . ? C33 C34 C35 123.4(5) . . ? C34 C35 C36 109.9(6) . . ? C34 C35 C37 111.7(5) . . ? C36 C35 C37 110.9(6) . . ? C34 C35 H35 108.1 . . ? C36 C35 H35 108.1 . . ? C37 C35 H35 108.1 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C34 121.9(6) . . ? C39 C38 H38 119.1 . . ? C34 C38 H38 119.1 . . ? C40 C39 C38 119.6(5) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C39 C40 C41 122.1(6) . . ? C39 C40 H40 118.9 . . ? C41 C40 H40 118.9 . . ? C40 C41 C33 117.9(5) . . ? C40 C41 C42 120.2(5) . . ? C33 C41 C42 121.9(5) . . ? C44 C42 C41 114.1(5) . . ? C44 C42 C43 111.2(6) . . ? C41 C42 C43 114.3(6) . . ? C44 C42 C43' 93.6(18) . . ? C41 C42 C43' 95.3(17) . . ? C43 C42 C43' 37.2(19) . . ? C44 C42 H42 116.5 . . ? C41 C42 H42 116.5 . . ? C43 C42 H42 79.4 . . ? C43' C42 H42 116.5 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C43' H43D 109.5 . . ? C42 C43' H43E 109.5 . . ? H43D C43' H43E 109.5 . . ? C42 C43' H43F 109.5 . . ? H43D C43' H43F 109.5 . . ? H43E C43' H43F 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C50 114.8(5) . . ? C46 C45 B1 124.4(4) . . ? C50 C45 B1 120.8(5) . . ? C45 C46 C47 122.9(6) . . ? C45 C46 H46 118.6 . . ? C47 C46 H46 118.6 . . ? C48 C47 C46 120.5(6) . . ? C48 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C47 C48 C49 119.2(6) . . ? C47 C48 H48 120.4 . . ? C49 C48 H48 120.4 . . ? C48 C49 C50 120.5(6) . . ? C48 C49 H49 119.7 . . ? C50 C49 H49 119.7 . . ? C49 C50 C45 122.1(6) . . ? C49 C50 H50 118.9 . . ? C45 C50 H50 118.9 . . ? C52 C51 C56 114.9(5) . . ? C52 C51 B1 124.3(5) . . ? C56 C51 B1 120.7(5) . . ? C51 C52 C53 122.4(6) . . ? C51 C52 H52 118.8 . . ? C53 C52 H52 118.8 . . ? C54 C53 C52 122.7(6) . . ? C54 C53 H53 118.6 . . ? C52 C53 H53 118.6 . . ? C53 C54 C55 116.4(6) . . ? C53 C54 H54 121.8 . . ? C55 C54 H54 121.8 . . ? C54 C55 C56 121.5(6) . . ? C54 C55 H55 119.3 . . ? C56 C55 H55 119.3 . . ? C55 C56 C51 122.1(6) . . ? C55 C56 H56 119.0 . . ? C51 C56 H56 119.0 . . ? C62 C57 C58 114.5(5) . . ? C62 C57 B1 122.6(5) . . ? C58 C57 B1 122.8(5) . . ? C59 C58 C57 122.7(5) . . ? C59 C58 H58 118.6 . . ? C57 C58 H58 118.6 . . ? C60 C59 C58 120.0(5) . . ? C60 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? C61 C60 C59 118.8(5) . . ? C61 C60 H60 120.6 . . ? C59 C60 H60 120.6 . . ? C60 C61 C62 120.7(6) . . ? C60 C61 H61 119.6 . . ? C62 C61 H61 119.6 . . ? C57 C62 C61 123.2(6) . . ? C57 C62 H62 118.4 . . ? C61 C62 H62 118.4 . . ? C64 C63 C68 120.0 . . ? C64 C63 B1 119.5(3) . . ? C68 C63 B1 120.4(3) . . ? C65 C64 C63 120.0 . . ? C65 C64 H64 120.0 . . ? C63 C64 H64 120.0 . . ? C64 C65 C66 120.0 . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C65 C66 C67 120.0 . . ? C65 C66 H66 120.0 . . ? C67 C66 H66 120.0 . . ? C68 C67 C66 120.0 . . ? C68 C67 H67 120.0 . . ? C66 C67 H67 120.0 . . ? C67 C68 C63 120.0 . . ? C67 C68 H68 120.0 . . ? C63 C68 H68 120.0 . . ? C51 B1 C57 110.4(4) . . ? C51 B1 C45 109.6(4) . . ? C57 B1 C45 108.3(4) . . ? C51 B1 C63 111.6(4) . . ? C57 B1 C63 107.0(4) . . ? C45 B1 C63 109.9(4) . . ? C14 N1 C21 122.2(4) . . ? C14 N1 Lu1 94.5(3) . . ? C21 N1 Lu1 143.3(3) . . ? C14 N2 C33 121.6(4) . . ? C14 N2 Lu1 93.9(3) . . ? C33 N2 Lu1 139.0(3) . . ? C2' O1 C5' 112.0(7) . . ? C2' O1 C5 96.8(8) . . ? C5' O1 C5 18.5(9) . . ? C2' O1 C2 9.2(11) . . ? C5' O1 C2 120.0(9) . . ? C5 O1 C2 105.6(9) . . ? C2' O1 Lu1 128.5(6) . . ? C5' O1 Lu1 119.4(7) . . ? C5 O1 Lu1 134.1(8) . . ? C2 O1 Lu1 120.1(7) . . ? C6' O2 C6 6.7(17) . . ? C6' O2 C9 109.2(17) . . ? C6 O2 C9 105.5(9) . . ? C6' O2 C9' 103.8(17) . . ? C6 O2 C9' 98.4(16) . . ? C9 O2 C9' 20.2(12) . . ? C6' O2 Lu1 125.4(12) . . ? C6 O2 Lu1 130.5(6) . . ? C9 O2 Lu1 122.8(8) . . ? C9' O2 Lu1 130.7(15) . . ? C10 O3 C13' 88.2(11) . . ? C10 O3 C10' 40.9(17) . . ? C13' O3 C10' 102.9(8) . . ? C10 O3 C13 103.9(14) . . ? C13' O3 C13 15.7(10) . . ? C10' O3 C13 115.7(18) . . ? C10 O3 Lu1 124.4(14) . . ? C13' O3 Lu1 128.9(8) . . ? C10' O3 Lu1 127.8(5) . . ? C13 O3 Lu1 116.5(17) . . ? O3 Lu1 O1 113.60(16) . . ? O3 Lu1 N1 155.87(15) . . ? O1 Lu1 N1 90.25(13) . . ? O3 Lu1 N2 97.60(15) . . ? O1 Lu1 N2 146.49(13) . . ? N1 Lu1 N2 58.32(13) . . ? O3 Lu1 O2 79.30(18) . . ? O1 Lu1 O2 77.74(14) . . ? N1 Lu1 O2 103.57(14) . . ? N2 Lu1 O2 97.31(14) . . ? O3 Lu1 C14 126.71(16) . . ? O1 Lu1 C14 119.19(14) . . ? N1 Lu1 C14 29.17(14) . . ? N2 Lu1 C14 29.37(13) . . ? O2 Lu1 C14 104.61(14) . . ? O3 Lu1 H1 82.13(13) . . ? O1 Lu1 H1 91.14(9) . . ? N1 Lu1 H1 101.85(9) . . ? N2 Lu1 H1 105.53(10) . . ? O2 Lu1 H1 152.20(10) . . ? C14 Lu1 H1 103.06(9) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.582 _refine_diff_density_min -0.875 _refine_diff_density_rms 0.099 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.333 -0.032 0.144 367 66 ' ' 2 0.667 0.002 0.356 368 66 ' ' 3 0.333 -0.027 0.644 367 65 ' ' 4 0.667 -0.001 0.856 368 65 ' ' 5 0.559 0.234 0.713 6 0 ' ' 6 0.559 0.266 0.213 6 0 ' ' 7 0.441 0.734 0.787 6 0 ' ' 8 0.441 0.766 0.287 6 0 ' ' _platon_squeeze_details ; Two disorder THF molecule per formual unit of [(Ph-NCN)LuH(THF)3][BPh4] were not modelled and the disordered density was taken into account using the SQUEEZE/PLATON procedure. (Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194?01) as implemented in PLATON (Spek, A.L. Acta Crystallogr. 1990, A46, C34; Spek, A.L. J. Appl. Cryst. 2003, 36, 7?3. PLATON - a multipurpose crystallographic tool. Utrecht University, Utrecht, The Netherlands). ; data_5-Lu _database_code_depnum_ccdc_archive 'CCDC 829249' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((Ph-NCN)Lu(NCN)(THF)2)(BPh4) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H90 B Lu N4 O2' _chemical_formula_weight 1205.24 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' B B 0.0013 0.0007 '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' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.306(4) _cell_length_b 12.971(5) _cell_length_c 23.504(8) _cell_angle_alpha 77.098(7) _cell_angle_beta 86.501(6) _cell_angle_gamma 80.166(6) _cell_volume 3602(2) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 249 _cell_measurement_theta_min 1.63 _cell_measurement_theta_max 25 _exptl_crystal_description Fragment _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 1.411 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6022 _exptl_absorpt_correction_T_max 0.6609 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19316 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.1515 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12412 _reflns_number_gt 8161 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (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. SADI and EADP have been used for the following atoms: SADI C32 C33 C32 C34 C32 C33' C32 C34' EADP C33 C34 C33' C34' EADP C37 C38 C39 H1 was located by difference Fourier syntheses. The coordinates parameters were refined, while the displace parameter was constrained. ; _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^)+(0.0778P)^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 12412 _refine_ls_number_parameters 696 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1173 _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.1718 _refine_ls_wR_factor_gt 0.1548 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9901(7) 0.1565(8) 0.3037(4) 0.043(2) Uani 1 1 d . . . C2 C 0.9215(8) 0.0104(8) 0.2787(4) 0.055(3) Uani 1 1 d . . . H2 H 0.8453 -0.0050 0.2761 0.066 Uiso 1 1 calc R . . C3 C 0.9806(10) -0.0095(9) 0.2239(5) 0.079(3) Uani 1 1 d . . . H3A H 0.9463 0.0426 0.1904 0.118 Uiso 1 1 calc R . . H3B H 0.9761 -0.0822 0.2199 0.118 Uiso 1 1 calc R . . H3C H 1.0581 -0.0018 0.2254 0.118 Uiso 1 1 calc R . . C4 C 0.9698(8) -0.0683(8) 0.3303(5) 0.065(3) Uani 1 1 d . . . H4A H 0.9287 -0.0548 0.3656 0.097 Uiso 1 1 calc R . . H4B H 1.0472 -0.0613 0.3333 0.097 Uiso 1 1 calc R . . H4C H 0.9656 -0.1410 0.3260 0.097 Uiso 1 1 calc R . . C5 C 1.0668(8) 0.2973(8) 0.3310(4) 0.051(2) Uani 1 1 d . . . H5 H 1.0335 0.3655 0.3429 0.061 Uiso 1 1 calc R . . C6 C 1.1497(9) 0.3266(9) 0.2832(4) 0.066(3) Uani 1 1 d . . . H6A H 1.1118 0.3740 0.2493 0.099 Uiso 1 1 calc R . . H6B H 1.1890 0.2614 0.2721 0.099 Uiso 1 1 calc R . . H6C H 1.2026 0.3635 0.2971 0.099 Uiso 1 1 calc R . . C7 C 1.1213(9) 0.2249(8) 0.3841(4) 0.064(3) Uani 1 1 d . . . H7A H 1.0652 0.2081 0.4147 0.096 Uiso 1 1 calc R . . H7B H 1.1745 0.2610 0.3984 0.096 Uiso 1 1 calc R . . H7C H 1.1597 0.1585 0.3740 0.096 Uiso 1 1 calc R . . C8 C 0.6732(8) 0.0893(8) 0.3605(4) 0.055(3) Uani 1 1 d . . . H8A H 0.7346 0.0761 0.3879 0.067 Uiso 1 1 calc R . . H8B H 0.6889 0.0373 0.3348 0.067 Uiso 1 1 calc R . . C9 C 0.5649(10) 0.0792(9) 0.3934(6) 0.084(4) Uani 1 1 d . . . H9A H 0.5462 0.0067 0.3974 0.101 Uiso 1 1 calc R . . H9B H 0.5674 0.0943 0.4328 0.101 Uiso 1 1 calc R . . C10 C 0.4842(9) 0.1616(10) 0.3564(5) 0.078(3) Uani 1 1 d . . . H10A H 0.4587 0.1330 0.3248 0.094 Uiso 1 1 calc R . . H10B H 0.4195 0.1857 0.3800 0.094 Uiso 1 1 calc R . . C11 C 0.5458(8) 0.2492(8) 0.3326(5) 0.064(3) Uani 1 1 d . . . H11A H 0.5406 0.2990 0.3594 0.077 Uiso 1 1 calc R . . H11B H 0.5173 0.2899 0.2942 0.077 Uiso 1 1 calc R . . C12 C 0.7731(11) 0.3402(8) 0.4048(4) 0.069(3) Uani 1 1 d . . . H12A H 0.7420 0.2735 0.4199 0.083 Uiso 1 1 calc R . . H12B H 0.8544 0.3233 0.4079 0.083 Uiso 1 1 calc R . . C13 C 0.7283(9) 0.4209(8) 0.4380(4) 0.063(3) Uani 1 1 d . . . H13A H 0.7805 0.4230 0.4680 0.075 Uiso 1 1 calc R . . H13B H 0.6573 0.4057 0.4575 0.075 Uiso 1 1 calc R . . C14 C 0.7120(9) 0.5238(9) 0.3939(5) 0.071(3) Uani 1 1 d . . . H14A H 0.6544 0.5774 0.4070 0.085 Uiso 1 1 calc R . . H14B H 0.7814 0.5538 0.3853 0.085 Uiso 1 1 calc R . . C15 C 0.6764(9) 0.4903(8) 0.3427(5) 0.065(3) Uani 1 1 d . . . H15A H 0.5967 0.4855 0.3459 0.078 Uiso 1 1 calc R . . H15B H 0.6907 0.5416 0.3061 0.078 Uiso 1 1 calc R . . C16 C 0.7470(7) 0.4050(7) 0.1661(3) 0.037(2) Uani 1 1 d . . . C17 C 0.7224(7) 0.4683(8) 0.1056(4) 0.048(2) Uani 1 1 d . . . C18 C 0.6720(8) 0.4227(10) 0.0661(4) 0.062(3) Uani 1 1 d . . . H18 H 0.6561 0.3518 0.0774 0.075 Uiso 1 1 calc R . . C19 C 0.6468(8) 0.4845(14) 0.0108(5) 0.090(5) Uani 1 1 d . . . H19 H 0.6172 0.4540 -0.0168 0.107 Uiso 1 1 calc R . . C20 C 0.6647(10) 0.5918(14) -0.0050(6) 0.100(5) Uani 1 1 d . . . H20 H 0.6435 0.6344 -0.0422 0.120 Uiso 1 1 calc R . . C21 C 0.7115(10) 0.6335(11) 0.0327(5) 0.078(4) Uani 1 1 d . . . H21 H 0.7249 0.7054 0.0219 0.094 Uiso 1 1 calc R . . C22 C 0.7409(7) 0.5712(9) 0.0880(4) 0.060(3) Uani 1 1 d . . . H22 H 0.7747 0.6017 0.1141 0.072 Uiso 1 1 calc R . . C23 C 0.9268(7) 0.4616(7) 0.1667(4) 0.044(2) Uani 1 1 d . . . C24 C 0.9948(7) 0.4180(7) 0.1253(4) 0.044(2) Uani 1 1 d . . . C25 C 0.9793(8) 0.3176(8) 0.1070(4) 0.050(2) Uani 1 1 d . . . H25 H 0.9123 0.2926 0.1281 0.060 Uiso 1 1 calc R . . C26 C 1.0759(8) 0.2289(8) 0.1229(5) 0.062(3) Uani 1 1 d . . . H26A H 1.0624 0.1651 0.1104 0.093 Uiso 1 1 calc R . . H26B H 1.0851 0.2121 0.1652 0.093 Uiso 1 1 calc R . . H26C H 1.1429 0.2521 0.1033 0.093 Uiso 1 1 calc R . . C27 C 0.9598(9) 0.3386(9) 0.0404(4) 0.066(3) Uani 1 1 d . . . H27A H 0.9494 0.2719 0.0300 0.099 Uiso 1 1 calc R . . H27B H 1.0239 0.3646 0.0187 0.099 Uiso 1 1 calc R . . H27C H 0.8939 0.3927 0.0304 0.099 Uiso 1 1 calc R . . C28 C 1.0834(8) 0.4687(8) 0.0997(4) 0.055(3) Uani 1 1 d . . . H28 H 1.1292 0.4410 0.0708 0.066 Uiso 1 1 calc R . . C29 C 1.1041(8) 0.5590(9) 0.1167(5) 0.065(3) Uani 1 1 d . . . H29 H 1.1632 0.5940 0.0986 0.078 Uiso 1 1 calc R . . C30 C 1.0404(8) 0.5979(8) 0.1591(4) 0.056(3) Uani 1 1 d . . . H30 H 1.0569 0.6593 0.1704 0.067 Uiso 1 1 calc R . . C31 C 0.9535(8) 0.5517(7) 0.1858(4) 0.048(2) Uani 1 1 d . B . C32 C 0.8825(10) 0.5990(10) 0.2313(5) 0.084(4) Uani 1 1 d D . . H32 H 0.8237 0.5572 0.2500 0.101 Uiso 1 1 calc R A 1 C33 C 0.935(2) 0.630(2) 0.2811(10) 0.086(4) Uani 0.57(2) 1 d PD B 2 H33A H 0.8764 0.6580 0.3066 0.129 Uiso 0.57(2) 1 calc PR B 2 H33B H 0.9803 0.6851 0.2650 0.129 Uiso 0.57(2) 1 calc PR B 2 H33C H 0.9807 0.5667 0.3037 0.129 Uiso 0.57(2) 1 calc PR B 2 C34 C 0.7783(19) 0.678(2) 0.2155(10) 0.086(4) Uani 0.57(2) 1 d PD B 2 H34A H 0.7434 0.6982 0.2509 0.129 Uiso 0.57(2) 1 calc PR B 2 H34B H 0.7274 0.6446 0.1975 0.129 Uiso 0.57(2) 1 calc PR B 2 H34C H 0.7961 0.7417 0.1879 0.129 Uiso 0.57(2) 1 calc PR B 2 C33' C 0.970(2) 0.607(3) 0.2733(14) 0.086(4) Uani 0.43(2) 1 d PD B 1 H33D H 0.9343 0.6370 0.3057 0.129 Uiso 0.43(2) 1 calc PR B 1 H33E H 1.0211 0.6541 0.2523 0.129 Uiso 0.43(2) 1 calc PR B 1 H33F H 1.0118 0.5357 0.2886 0.129 Uiso 0.43(2) 1 calc PR B 1 C34' C 0.840(3) 0.7169(18) 0.1996(11) 0.086(4) Uani 0.43(2) 1 d PD B 1 H34D H 0.7921 0.7534 0.2265 0.129 Uiso 0.43(2) 1 calc PR B 1 H34E H 0.7975 0.7168 0.1655 0.129 Uiso 0.43(2) 1 calc PR B 1 H34F H 0.9025 0.7545 0.1868 0.129 Uiso 0.43(2) 1 calc PR B 1 C35 C 0.5794(7) 0.3230(8) 0.1822(3) 0.047(2) Uani 1 1 d . . . C36 C 0.5697(9) 0.2189(8) 0.1756(4) 0.057(3) Uani 1 1 d . . . C37 C 0.6650(10) 0.1312(10) 0.1813(5) 0.079(2) Uani 1 1 d . . . H37 H 0.7175 0.1442 0.2088 0.095 Uiso 1 1 calc R . . C38 C 0.7258(9) 0.1275(10) 0.1237(5) 0.079(2) Uani 1 1 d . . . H38A H 0.7876 0.0679 0.1295 0.118 Uiso 1 1 calc R . . H38B H 0.7538 0.1950 0.1088 0.118 Uiso 1 1 calc R . . H38C H 0.6753 0.1172 0.0956 0.118 Uiso 1 1 calc R . . C39 C 0.6294(10) 0.0190(9) 0.2074(5) 0.079(2) Uani 1 1 d . . . H39A H 0.6943 -0.0372 0.2101 0.118 Uiso 1 1 calc R . . H39B H 0.5755 0.0058 0.1820 0.118 Uiso 1 1 calc R . . H39C H 0.5962 0.0186 0.2464 0.118 Uiso 1 1 calc R . . C40 C 0.4623(10) 0.2025(11) 0.1649(4) 0.075(4) Uani 1 1 d . . . H40 H 0.4518 0.1333 0.1613 0.090 Uiso 1 1 calc R . . C41 C 0.3718(9) 0.2844(11) 0.1594(4) 0.069(3) Uani 1 1 d . . . H41 H 0.3017 0.2718 0.1502 0.083 Uiso 1 1 calc R . . C42 C 0.3841(8) 0.3814(12) 0.1672(4) 0.069(3) Uani 1 1 d . . . H42 H 0.3214 0.4361 0.1648 0.083 Uiso 1 1 calc R . . C43 C 0.4896(7) 0.4043(8) 0.1789(4) 0.049(2) Uani 1 1 d . . . C44 C 0.4951(8) 0.5136(9) 0.1896(4) 0.061(3) Uani 1 1 d . . . H44 H 0.5731 0.5163 0.1982 0.073 Uiso 1 1 calc R . . C45 C 0.4588(10) 0.6035(10) 0.1361(5) 0.088(4) Uani 1 1 d . . . H45A H 0.4644 0.6730 0.1445 0.133 Uiso 1 1 calc R . . H45B H 0.3823 0.6022 0.1273 0.133 Uiso 1 1 calc R . . H45C H 0.5067 0.5923 0.1024 0.133 Uiso 1 1 calc R . . C46 C 0.4229(11) 0.5325(10) 0.2419(5) 0.088(4) Uani 1 1 d . . . H46A H 0.4533 0.5808 0.2610 0.132 Uiso 1 1 calc R . . H46B H 0.4206 0.4640 0.2695 0.132 Uiso 1 1 calc R . . H46C H 0.3481 0.5648 0.2290 0.132 Uiso 1 1 calc R . . C47 C 0.5025(7) 0.7977(7) 0.3945(4) 0.044(2) Uani 1 1 d . . . C48 C 0.5399(8) 0.7767(7) 0.4521(4) 0.049(2) Uani 1 1 d . . . H48 H 0.4886 0.7622 0.4835 0.058 Uiso 1 1 calc R . . C49 C 0.6494(8) 0.7764(8) 0.4649(5) 0.057(3) Uani 1 1 d . . . H49 H 0.6707 0.7630 0.5044 0.069 Uiso 1 1 calc R . . C50 C 0.7277(10) 0.7958(8) 0.4199(6) 0.074(3) Uani 1 1 d . . . H50 H 0.8015 0.7983 0.4284 0.088 Uiso 1 1 calc R . . C51 C 0.6966(9) 0.8110(8) 0.3631(6) 0.065(3) Uani 1 1 d . . . H51 H 0.7504 0.8197 0.3325 0.078 Uiso 1 1 calc R . . C52 C 0.5858(9) 0.8139(8) 0.3497(5) 0.058(3) Uani 1 1 d . . . H52 H 0.5660 0.8269 0.3100 0.070 Uiso 1 1 calc R . . C53 C 0.3545(8) 0.6732(8) 0.3856(4) 0.047(2) Uani 1 1 d . . . C54 C 0.4150(7) 0.5855(7) 0.4208(4) 0.043(2) Uani 1 1 d . . . H54 H 0.4748 0.5971 0.4411 0.052 Uiso 1 1 calc R . . C55 C 0.3942(8) 0.4804(8) 0.4288(4) 0.048(2) Uani 1 1 d . . . H55 H 0.4376 0.4237 0.4547 0.057 Uiso 1 1 calc R . . C56 C 0.3102(9) 0.4595(8) 0.3987(4) 0.058(3) Uani 1 1 d . . . H56 H 0.2959 0.3885 0.4028 0.069 Uiso 1 1 calc R . . C57 C 0.2474(8) 0.5450(9) 0.3622(5) 0.062(3) Uani 1 1 d . . . H57 H 0.1891 0.5320 0.3415 0.074 Uiso 1 1 calc R . . C58 C 0.2677(8) 0.6491(8) 0.3554(4) 0.055(3) Uani 1 1 d . . . H58 H 0.2230 0.7057 0.3301 0.065 Uiso 1 1 calc R . . C59 C 0.3459(8) 0.8692(8) 0.3136(4) 0.048(2) Uani 1 1 d . . . C60 C 0.3736(12) 0.8260(9) 0.2636(5) 0.085(4) Uani 1 1 d . . . H60 H 0.4088 0.7535 0.2689 0.102 Uiso 1 1 calc R . . C61 C 0.3518(12) 0.8844(11) 0.2066(5) 0.089(4) Uani 1 1 d . . . H61 H 0.3707 0.8507 0.1746 0.107 Uiso 1 1 calc R . . C62 C 0.3033(9) 0.9903(10) 0.1968(5) 0.064(3) Uani 1 1 d . . . H62 H 0.2882 1.0307 0.1583 0.076 Uiso 1 1 calc R . . C63 C 0.2775(8) 1.0352(9) 0.2439(5) 0.063(3) Uani 1 1 d . . . H63 H 0.2453 1.1087 0.2381 0.075 Uiso 1 1 calc R . . C64 C 0.2975(7) 0.9755(8) 0.3008(4) 0.048(2) Uani 1 1 d . . . H64 H 0.2766 1.0101 0.3323 0.058 Uiso 1 1 calc R . . C65 C 0.2905(8) 0.8494(7) 0.4269(4) 0.048(2) Uani 1 1 d . . . C66 C 0.3121(8) 0.9332(7) 0.4501(4) 0.048(2) Uani 1 1 d . . . H66 H 0.3793 0.9598 0.4390 0.057 Uiso 1 1 calc R . . C67 C 0.2421(9) 0.9794(8) 0.4880(5) 0.063(3) Uani 1 1 d . . . H67 H 0.2624 1.0359 0.5026 0.076 Uiso 1 1 calc R . . C68 C 0.1413(9) 0.9454(8) 0.5058(4) 0.055(3) Uani 1 1 d . . . H68 H 0.0931 0.9775 0.5324 0.066 Uiso 1 1 calc R . . C69 C 0.1138(9) 0.8621(9) 0.4831(4) 0.062(3) Uani 1 1 d . . . H69 H 0.0455 0.8374 0.4935 0.074 Uiso 1 1 calc R . . C70 C 0.1877(7) 0.8162(7) 0.4452(4) 0.046(2) Uani 1 1 d . . . H70 H 0.1682 0.7592 0.4307 0.055 Uiso 1 1 calc R . . B1 B 0.3727(9) 0.7966(8) 0.3803(4) 0.044(3) Uani 1 1 d . . . N1 N 0.9762(5) 0.2572(6) 0.3098(3) 0.0415(18) Uani 1 1 d . . . N2 N 0.9075(5) 0.1227(6) 0.2829(3) 0.0400(17) Uani 1 1 d . . . N3 N 0.8377(6) 0.4104(6) 0.1960(3) 0.0432(18) Uani 1 1 d . . . N4 N 0.6865(6) 0.3353(6) 0.1980(3) 0.0420(18) Uani 1 1 d . . . O1 O 0.6597(5) 0.1967(5) 0.3269(2) 0.0460(15) Uani 1 1 d . . . O2 O 0.7424(5) 0.3856(5) 0.3440(2) 0.0482(16) Uani 1 1 d . . . Lu1 Lu 0.79965(3) 0.28473(3) 0.277326(16) 0.03505(14) Uani 1 1 d . . . H1 H 1.064(7) 0.100(6) 0.319(3) 0.050 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 C1 0.031(5) 0.061(7) 0.039(5) -0.013(5) -0.001(4) -0.010(5) C2 0.033(5) 0.076(8) 0.062(7) -0.021(6) 0.002(5) -0.021(5) C3 0.065(8) 0.084(9) 0.099(9) -0.045(7) 0.028(7) -0.022(6) C4 0.051(6) 0.046(6) 0.105(9) -0.017(6) -0.012(6) -0.025(5) C5 0.053(6) 0.055(6) 0.051(6) -0.010(5) -0.011(5) -0.023(5) C6 0.056(7) 0.081(8) 0.075(7) -0.026(6) 0.005(6) -0.042(6) C7 0.061(7) 0.077(8) 0.059(6) -0.005(6) -0.018(5) -0.035(6) C8 0.046(6) 0.071(7) 0.055(6) -0.017(5) 0.017(5) -0.025(5) C9 0.074(9) 0.045(7) 0.123(10) -0.005(7) 0.046(8) -0.013(6) C10 0.043(7) 0.093(9) 0.101(9) -0.026(8) 0.008(6) -0.015(6) C11 0.048(7) 0.061(7) 0.079(8) -0.009(6) 0.020(6) -0.010(5) C12 0.106(10) 0.062(7) 0.036(6) -0.007(5) -0.004(6) -0.008(6) C13 0.070(8) 0.071(8) 0.062(7) -0.039(6) 0.001(6) -0.021(6) C14 0.057(7) 0.060(8) 0.107(9) -0.044(7) 0.024(6) -0.018(6) C15 0.064(7) 0.048(7) 0.079(8) -0.012(6) 0.018(6) -0.009(5) C16 0.030(5) 0.044(5) 0.037(5) -0.009(4) 0.001(4) -0.007(4) C17 0.034(5) 0.071(7) 0.039(5) -0.019(5) 0.007(4) -0.005(5) C18 0.040(6) 0.099(9) 0.048(6) -0.015(6) -0.002(5) -0.013(6) C19 0.029(6) 0.207(16) 0.035(6) -0.023(8) -0.004(5) -0.031(8) C20 0.046(8) 0.170(15) 0.057(8) 0.031(9) 0.005(6) -0.018(9) C21 0.057(8) 0.108(10) 0.056(7) 0.014(7) -0.007(6) -0.014(7) C22 0.030(5) 0.082(8) 0.063(7) 0.005(6) -0.007(5) -0.020(5) C23 0.038(5) 0.056(6) 0.040(5) -0.004(4) -0.005(4) -0.022(4) C24 0.033(5) 0.058(6) 0.040(5) -0.004(5) 0.002(4) -0.017(4) C25 0.044(6) 0.061(7) 0.046(6) -0.010(5) 0.001(4) -0.012(5) C26 0.045(6) 0.063(7) 0.083(7) -0.016(6) -0.009(5) -0.018(5) C27 0.057(7) 0.093(9) 0.055(6) -0.018(6) 0.000(5) -0.024(6) C28 0.037(6) 0.076(8) 0.047(6) -0.001(5) 0.009(4) -0.012(5) C29 0.039(6) 0.071(8) 0.084(8) 0.008(6) -0.008(6) -0.039(6) C30 0.050(6) 0.058(7) 0.067(7) -0.016(6) 0.001(5) -0.023(5) C31 0.041(6) 0.045(6) 0.059(6) -0.012(5) 0.001(5) -0.011(4) C32 0.089(10) 0.101(10) 0.094(9) -0.057(8) 0.028(8) -0.061(8) C33 0.067(11) 0.114(11) 0.070(8) -0.042(7) 0.017(8) 0.028(8) C34 0.067(11) 0.114(11) 0.070(8) -0.042(7) 0.017(8) 0.028(8) C33' 0.067(11) 0.114(11) 0.070(8) -0.042(7) 0.017(8) 0.028(8) C34' 0.067(11) 0.114(11) 0.070(8) -0.042(7) 0.017(8) 0.028(8) C35 0.037(5) 0.081(7) 0.027(5) -0.011(5) -0.005(4) -0.020(5) C36 0.081(8) 0.043(6) 0.057(6) -0.005(5) -0.026(5) -0.039(5) C37 0.064(5) 0.098(5) 0.087(5) -0.027(5) -0.018(4) -0.032(4) C38 0.064(5) 0.098(5) 0.087(5) -0.027(5) -0.018(4) -0.032(4) C39 0.064(5) 0.098(5) 0.087(5) -0.027(5) -0.018(4) -0.032(4) C40 0.066(8) 0.129(11) 0.045(6) -0.003(7) -0.015(6) -0.069(8) C41 0.048(7) 0.103(10) 0.054(7) 0.010(7) -0.008(5) -0.042(7) C42 0.018(5) 0.130(11) 0.050(6) 0.000(7) -0.006(4) -0.014(6) C43 0.027(5) 0.072(7) 0.046(6) -0.006(5) 0.004(4) -0.010(5) C44 0.041(6) 0.073(8) 0.060(7) -0.006(6) 0.004(5) 0.001(5) C45 0.069(8) 0.089(9) 0.092(9) 0.014(7) -0.002(7) -0.015(7) C46 0.102(11) 0.080(9) 0.076(8) -0.026(7) 0.019(7) 0.008(7) C47 0.040(5) 0.037(5) 0.059(6) -0.018(4) 0.019(5) -0.018(4) C48 0.053(6) 0.046(6) 0.053(6) -0.011(5) -0.002(5) -0.025(5) C49 0.052(7) 0.052(6) 0.071(7) -0.009(5) -0.003(6) -0.023(5) C50 0.055(7) 0.054(7) 0.119(11) -0.020(7) -0.014(7) -0.021(6) C51 0.050(7) 0.054(7) 0.095(9) -0.020(6) 0.011(6) -0.015(5) C52 0.058(7) 0.052(6) 0.066(7) -0.017(5) 0.017(5) -0.010(5) C53 0.043(6) 0.056(6) 0.050(6) -0.018(5) 0.003(5) -0.020(5) C54 0.040(5) 0.044(6) 0.049(5) -0.009(5) 0.001(4) -0.017(4) C55 0.043(6) 0.051(6) 0.051(6) -0.007(5) 0.003(4) -0.018(5) C56 0.061(7) 0.049(6) 0.073(7) -0.023(6) 0.009(6) -0.028(5) C57 0.043(6) 0.070(8) 0.083(8) -0.031(6) 0.003(6) -0.023(5) C58 0.056(7) 0.047(6) 0.065(7) -0.019(5) -0.002(5) -0.013(5) C59 0.041(6) 0.052(6) 0.059(6) -0.021(5) 0.011(5) -0.019(5) C60 0.149(13) 0.063(8) 0.052(7) -0.024(6) 0.016(7) -0.029(8) C61 0.153(14) 0.086(10) 0.044(7) -0.024(7) 0.020(7) -0.057(9) C62 0.075(8) 0.068(8) 0.048(7) 0.008(6) -0.018(6) -0.031(6) C63 0.045(6) 0.063(7) 0.070(8) 0.008(6) 0.008(5) -0.012(5) C64 0.040(6) 0.052(6) 0.057(6) -0.021(5) 0.002(5) -0.010(5) C65 0.050(6) 0.044(6) 0.050(6) -0.011(5) 0.000(5) -0.007(5) C66 0.049(6) 0.037(5) 0.062(6) -0.024(5) 0.005(5) -0.006(4) C67 0.058(7) 0.061(7) 0.079(8) -0.028(6) -0.007(6) -0.017(6) C68 0.067(7) 0.062(7) 0.035(5) -0.015(5) 0.002(5) -0.002(5) C69 0.045(6) 0.075(8) 0.069(7) -0.025(6) 0.002(5) -0.008(5) C70 0.041(6) 0.046(6) 0.056(6) -0.019(5) -0.002(5) -0.011(4) B1 0.045(6) 0.044(6) 0.043(6) -0.003(5) 0.004(5) -0.017(5) N1 0.028(4) 0.044(5) 0.055(5) -0.011(4) -0.004(3) -0.013(3) N2 0.027(4) 0.044(5) 0.056(5) -0.015(4) -0.008(3) -0.017(3) N3 0.036(4) 0.065(5) 0.036(4) -0.018(4) 0.003(3) -0.022(4) N4 0.032(4) 0.057(5) 0.044(4) -0.016(4) 0.002(3) -0.019(4) O1 0.040(4) 0.048(4) 0.049(4) -0.001(3) 0.011(3) -0.021(3) O2 0.054(4) 0.049(4) 0.044(4) -0.010(3) -0.004(3) -0.013(3) Lu1 0.0295(2) 0.0446(2) 0.0355(2) -0.00984(15) -0.00114(14) -0.01669(15) _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 1.327(11) . ? C1 N2 1.332(10) . ? C1 Lu1 2.651(10) . ? C1 H1 1.10(8) . ? C2 N2 1.461(12) . ? C2 C4 1.480(13) . ? C2 C3 1.492(13) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N1 1.463(11) . ? C5 C6 1.500(13) . ? C5 C7 1.502(12) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 O1 1.428(11) . ? C8 C9 1.510(13) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.487(15) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.462(14) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O1 1.463(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.457(13) . ? C12 O2 1.465(10) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.488(14) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.481(14) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O2 1.454(11) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N4 1.340(10) . ? C16 N3 1.374(10) . ? C16 C17 1.494(12) . ? C16 Lu1 2.780(8) . ? C17 C22 1.360(13) . ? C17 C18 1.427(13) . ? C18 C19 1.388(15) . ? C18 H18 0.9500 . ? C19 C20 1.410(19) . ? C19 H19 0.9500 . ? C20 C21 1.339(18) . ? C20 H20 0.9500 . ? C21 C22 1.401(14) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.397(12) . ? C23 C31 1.435(12) . ? C23 N3 1.438(10) . ? C24 C28 1.404(12) . ? C24 C25 1.504(13) . ? C25 C26 1.506(13) . ? C25 C27 1.555(12) . ? 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 C29 1.385(14) . ? C28 H28 0.9500 . ? C29 C30 1.362(14) . ? C29 H29 0.9500 . ? C30 C31 1.367(13) . ? C30 H30 0.9500 . ? C31 C32 1.509(14) . ? C32 C34 1.506(15) . ? C32 C33 1.528(15) . ? C32 C33' 1.539(17) . ? C32 C34' 1.561(16) . ? C32 H32 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C33' H33D 0.9800 . ? C33' H33E 0.9800 . ? C33' H33F 0.9800 . ? C34' H34D 0.9800 . ? C34' H34E 0.9800 . ? C34' H34F 0.9800 . ? C35 C43 1.383(13) . ? C35 C36 1.419(13) . ? C35 N4 1.434(10) . ? C36 C40 1.421(13) . ? C36 C37 1.476(15) . ? C37 C38 1.513(15) . ? C37 C39 1.572(15) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.392(16) . ? C40 H40 0.9500 . ? C41 C42 1.346(16) . ? C41 H41 0.9500 . ? C42 C43 1.436(13) . ? C42 H42 0.9500 . ? C43 C44 1.508(14) . ? C44 C46 1.512(14) . ? C44 C45 1.542(14) . ? C44 H44 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.409(12) . ? C47 C52 1.430(12) . ? C47 B1 1.655(14) . ? C48 C49 1.397(13) . ? C48 H48 0.9500 . ? C49 C50 1.396(15) . ? C49 H49 0.9500 . ? C50 C51 1.372(15) . ? C50 H50 0.9500 . ? C51 C52 1.410(14) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.378(12) . ? C53 C58 1.431(13) . ? C53 B1 1.630(13) . ? C54 C55 1.398(12) . ? C54 H54 0.9500 . ? C55 C56 1.384(13) . ? C55 H55 0.9500 . ? C56 C57 1.387(14) . ? C56 H56 0.9500 . ? C57 C58 1.387(13) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C64 1.379(12) . ? C59 C60 1.411(13) . ? C59 B1 1.660(14) . ? C60 C61 1.400(15) . ? C60 H60 0.9500 . ? C61 C62 1.375(16) . ? C61 H61 0.9500 . ? C62 C63 1.361(14) . ? C62 H62 0.9500 . ? C63 C64 1.400(13) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 C66 1.389(12) . ? C65 C70 1.417(12) . ? C65 B1 1.629(14) . ? C66 C67 1.365(13) . ? C66 H66 0.9500 . ? C67 C68 1.396(14) . ? C67 H67 0.9500 . ? C68 C69 1.404(13) . ? C68 H68 0.9500 . ? C69 C70 1.389(12) . ? C69 H69 0.9500 . ? C70 H70 0.9500 . ? N1 Lu1 2.291(7) . ? N2 Lu1 2.268(7) . ? N3 Lu1 2.300(7) . ? N4 Lu1 2.304(7) . ? O1 Lu1 2.336(5) . ? O2 Lu1 2.266(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 N1 C1 N2 118.6(8) . . ? N1 C1 Lu1 59.8(5) . . ? N2 C1 Lu1 58.8(5) . . ? N1 C1 H1 121(4) . . ? N2 C1 H1 120(4) . . ? Lu1 C1 H1 174(4) . . ? N2 C2 C4 115.5(8) . . ? N2 C2 C3 112.8(8) . . ? C4 C2 C3 110.9(9) . . ? N2 C2 H2 105.6 . . ? C4 C2 H2 105.6 . . ? C3 C2 H2 105.6 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 C6 111.6(7) . . ? N1 C5 C7 114.4(8) . . ? C6 C5 C7 111.4(9) . . ? N1 C5 H5 106.3 . . ? C6 C5 H5 106.3 . . ? C7 C5 H5 106.3 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 C8 C9 105.2(8) . . ? O1 C8 H8A 110.7 . . ? C9 C8 H8A 110.7 . . ? O1 C8 H8B 110.7 . . ? C9 C8 H8B 110.7 . . ? H8A C8 H8B 108.8 . . ? C10 C9 C8 103.5(9) . . ? C10 C9 H9A 111.1 . . ? C8 C9 H9A 111.1 . . ? C10 C9 H9B 111.1 . . ? C8 C9 H9B 111.1 . . ? H9A C9 H9B 109.0 . . ? C11 C10 C9 104.2(9) . . ? C11 C10 H10A 110.9 . . ? C9 C10 H10A 110.9 . . ? C11 C10 H10B 110.9 . . ? C9 C10 H10B 110.9 . . ? H10A C10 H10B 108.9 . . ? C10 C11 O1 104.7(8) . . ? C10 C11 H11A 110.8 . . ? O1 C11 H11A 110.8 . . ? C10 C11 H11B 110.8 . . ? O1 C11 H11B 110.8 . . ? H11A C11 H11B 108.9 . . ? C13 C12 O2 106.7(8) . . ? C13 C12 H12A 110.4 . . ? O2 C12 H12A 110.4 . . ? C13 C12 H12B 110.4 . . ? O2 C12 H12B 110.4 . . ? H12A C12 H12B 108.6 . . ? C12 C13 C14 104.8(8) . . ? C12 C13 H13A 110.8 . . ? C14 C13 H13A 110.8 . . ? C12 C13 H13B 110.8 . . ? C14 C13 H13B 110.8 . . ? H13A C13 H13B 108.9 . . ? C15 C14 C13 101.9(8) . . ? C15 C14 H14A 111.4 . . ? C13 C14 H14A 111.4 . . ? C15 C14 H14B 111.4 . . ? C13 C14 H14B 111.4 . . ? H14A C14 H14B 109.2 . . ? O2 C15 C14 104.5(9) . . ? O2 C15 H15A 110.9 . . ? C14 C15 H15A 110.9 . . ? O2 C15 H15B 110.9 . . ? C14 C15 H15B 110.9 . . ? H15A C15 H15B 108.9 . . ? N4 C16 N3 111.0(7) . . ? N4 C16 C17 125.6(8) . . ? N3 C16 C17 123.4(7) . . ? N4 C16 Lu1 55.5(4) . . ? N3 C16 Lu1 55.5(4) . . ? C17 C16 Lu1 178.1(6) . . ? C22 C17 C18 118.6(9) . . ? C22 C17 C16 121.6(9) . . ? C18 C17 C16 119.7(9) . . ? C19 C18 C17 118.5(11) . . ? C19 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? C18 C19 C20 120.8(12) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C21 C20 C19 119.8(12) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C22 120.0(13) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C17 C22 C21 122.1(11) . . ? C17 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C24 C23 C31 119.8(8) . . ? C24 C23 N3 121.3(8) . . ? C31 C23 N3 118.5(8) . . ? C23 C24 C28 119.0(9) . . ? C23 C24 C25 123.3(8) . . ? C28 C24 C25 117.7(8) . . ? C24 C25 C26 112.0(8) . . ? C24 C25 C27 111.6(8) . . ? C26 C25 C27 109.3(8) . . ? C24 C25 H25 107.9 . . ? C26 C25 H25 107.9 . . ? C27 C25 H25 107.9 . . ? 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 . . ? C29 C28 C24 120.1(9) . . ? C29 C28 H28 119.9 . . ? C24 C28 H28 119.9 . . ? C30 C29 C28 120.3(9) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C31 122.3(9) . . ? C29 C30 H30 118.9 . . ? C31 C30 H30 118.9 . . ? C30 C31 C23 118.2(9) . . ? C30 C31 C32 120.8(9) . . ? C23 C31 C32 120.9(8) . . ? C34 C32 C31 121.6(11) . . ? C34 C32 C33 107.6(14) . . ? C31 C32 C33 120.8(12) . . ? C34 C32 C33' 126.1(17) . . ? C31 C32 C33' 101.2(13) . . ? C33 C32 C33' 20.0(11) . . ? C34 C32 C34' 37.6(14) . . ? C31 C32 C34' 104.4(13) . . ? C33 C32 C34' 94.8(18) . . ? C33' C32 C34' 105(2) . . ? C34 C32 H32 77.3 . . ? C31 C32 H32 114.8 . . ? C33 C32 H32 105.8 . . ? C33' C32 H32 114.8 . . ? C34' C32 H32 114.8 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C33' H33D 109.5 . . ? C32 C33' H33E 109.5 . . ? H33D C33' H33E 109.5 . . ? C32 C33' H33F 109.5 . . ? H33D C33' H33F 109.5 . . ? H33E C33' H33F 109.5 . . ? C32 C34' H34D 109.5 . . ? C32 C34' H34E 109.5 . . ? H34D C34' H34E 109.5 . . ? C32 C34' H34F 109.5 . . ? H34D C34' H34F 109.5 . . ? H34E C34' H34F 109.5 . . ? C43 C35 C36 122.3(9) . . ? C43 C35 N4 122.1(9) . . ? C36 C35 N4 115.3(8) . . ? C35 C36 C40 116.2(10) . . ? C35 C36 C37 122.2(9) . . ? C40 C36 C37 121.6(10) . . ? C36 C37 C38 112.2(10) . . ? C36 C37 C39 111.7(10) . . ? C38 C37 C39 109.0(10) . . ? C36 C37 H37 107.9 . . ? C38 C37 H37 107.9 . . ? C39 C37 H37 107.9 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C36 122.2(11) . . ? C41 C40 H40 118.9 . . ? C36 C40 H40 118.9 . . ? C42 C41 C40 119.6(10) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C41 C42 C43 121.6(11) . . ? C41 C42 H42 119.2 . . ? C43 C42 H42 119.2 . . ? C35 C43 C42 117.9(10) . . ? C35 C43 C44 123.9(8) . . ? C42 C43 C44 118.1(9) . . ? C43 C44 C46 109.9(9) . . ? C43 C44 C45 111.9(9) . . ? C46 C44 C45 109.4(9) . . ? C43 C44 H44 108.5 . . ? C46 C44 H44 108.5 . . ? C45 C44 H44 108.5 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C52 115.2(9) . . ? C48 C47 B1 122.0(8) . . ? C52 C47 B1 122.7(9) . . ? C49 C48 C47 122.7(9) . . ? C49 C48 H48 118.6 . . ? C47 C48 H48 118.6 . . ? C50 C49 C48 120.3(10) . . ? C50 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? C51 C50 C49 119.1(10) . . ? C51 C50 H50 120.4 . . ? C49 C50 H50 120.4 . . ? C50 C51 C52 120.9(11) . . ? C50 C51 H51 119.5 . . ? C52 C51 H51 119.5 . . ? C51 C52 C47 121.5(10) . . ? C51 C52 H52 119.2 . . ? C47 C52 H52 119.2 . . ? C54 C53 C58 114.7(8) . . ? C54 C53 B1 124.2(8) . . ? C58 C53 B1 121.0(9) . . ? C53 C54 C55 124.3(9) . . ? C53 C54 H54 117.8 . . ? C55 C54 H54 117.8 . . ? C56 C55 C54 119.6(9) . . ? C56 C55 H55 120.2 . . ? C54 C55 H55 120.2 . . ? C55 C56 C57 118.3(9) . . ? C55 C56 H56 120.9 . . ? C57 C56 H56 120.9 . . ? C56 C57 C58 121.6(10) . . ? C56 C57 H57 119.2 . . ? C58 C57 H57 119.2 . . ? C57 C58 C53 121.5(10) . . ? C57 C58 H58 119.3 . . ? C53 C58 H58 119.3 . . ? C64 C59 C60 113.4(9) . . ? C64 C59 B1 124.9(8) . . ? C60 C59 B1 121.7(9) . . ? C61 C60 C59 123.4(11) . . ? C61 C60 H60 118.3 . . ? C59 C60 H60 118.3 . . ? C62 C61 C60 120.4(11) . . ? C62 C61 H61 119.8 . . ? C60 C61 H61 119.8 . . ? C63 C62 C61 117.8(10) . . ? C63 C62 H62 121.1 . . ? C61 C62 H62 121.1 . . ? C62 C63 C64 121.4(10) . . ? C62 C63 H63 119.3 . . ? C64 C63 H63 119.3 . . ? C59 C64 C63 123.6(9) . . ? C59 C64 H64 118.2 . . ? C63 C64 H64 118.2 . . ? C66 C65 C70 114.2(8) . . ? C66 C65 B1 123.5(8) . . ? C70 C65 B1 122.2(8) . . ? C67 C66 C65 123.7(9) . . ? C67 C66 H66 118.2 . . ? C65 C66 H66 118.2 . . ? C66 C67 C68 121.4(9) . . ? C66 C67 H67 119.3 . . ? C68 C67 H67 119.3 . . ? C67 C68 C69 117.7(9) . . ? C67 C68 H68 121.2 . . ? C69 C68 H68 121.2 . . ? C70 C69 C68 119.3(10) . . ? C70 C69 H69 120.4 . . ? C68 C69 H69 120.4 . . ? C69 C70 C65 123.8(9) . . ? C69 C70 H70 118.1 . . ? C65 C70 H70 118.1 . . ? C65 B1 C53 109.3(7) . . ? C65 B1 C47 109.9(7) . . ? C53 B1 C47 109.2(8) . . ? C65 B1 C59 108.8(7) . . ? C53 B1 C59 111.0(8) . . ? C47 B1 C59 108.6(7) . . ? C1 N1 C5 119.7(8) . . ? C1 N1 Lu1 90.1(5) . . ? C5 N1 Lu1 150.1(6) . . ? C1 N2 C2 118.2(8) . . ? C1 N2 Lu1 91.1(6) . . ? C2 N2 Lu1 150.4(5) . . ? C16 N3 C23 121.0(7) . . ? C16 N3 Lu1 95.0(5) . . ? C23 N3 Lu1 141.5(6) . . ? C16 N4 C35 124.1(7) . . ? C16 N4 Lu1 95.8(5) . . ? C35 N4 Lu1 139.4(5) . . ? C8 O1 C11 109.9(6) . . ? C8 O1 Lu1 126.2(5) . . ? C11 O1 Lu1 123.7(5) . . ? C15 O2 C12 106.8(7) . . ? C15 O2 Lu1 135.4(6) . . ? C12 O2 Lu1 117.8(5) . . ? O2 Lu1 N2 133.1(2) . . ? O2 Lu1 N1 90.0(2) . . ? N2 Lu1 N1 60.2(2) . . ? O2 Lu1 N3 102.7(2) . . ? N2 Lu1 N3 113.2(3) . . ? N1 Lu1 N3 92.7(2) . . ? O2 Lu1 N4 110.7(2) . . ? N2 Lu1 N4 113.6(2) . . ? N1 Lu1 N4 146.7(2) . . ? N3 Lu1 N4 58.1(2) . . ? O2 Lu1 O1 78.9(2) . . ? N2 Lu1 O1 88.6(2) . . ? N1 Lu1 O1 123.8(2) . . ? N3 Lu1 O1 143.5(2) . . ? N4 Lu1 O1 86.8(2) . . ? O2 Lu1 C1 112.9(2) . . ? N2 Lu1 C1 30.2(2) . . ? N1 Lu1 C1 30.0(2) . . ? N3 Lu1 C1 105.2(3) . . ? N4 Lu1 C1 135.9(3) . . ? O1 Lu1 C1 107.6(2) . . ? O2 Lu1 C16 109.5(2) . . ? N2 Lu1 C16 116.7(2) . . ? N1 Lu1 C16 120.6(2) . . ? N3 Lu1 C16 29.5(2) . . ? N4 Lu1 C16 28.6(2) . . ? O1 Lu1 C16 115.0(2) . . ? C1 Lu1 C16 124.1(2) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 2.015 _refine_diff_density_min -2.148 _refine_diff_density_rms 0.135 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.011 0.000 0.000 640 139 ' ' 2 0.000 0.500 0.500 168 50 ' ' _platon_squeeze_details ; Two disordered THF molecules per formual unit of [(Ph-NCN)Lu(NCN)(THF)2][BPh4] were not modelled and the disordered density was taken into account using the SQUEEZE/PLATON procedure. (Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194?01) as implemented in PLATON (Spek, A.L. Acta Crystallogr. 1990, A46, C34; Spek, A.L. J. Appl. Cryst. 2003, 36, 7?3. PLATON - a multipurpose crystallographic tool. Utrecht University, Utrecht, The Netherlands). ; data_6-Lu _database_code_depnum_ccdc_archive 'CCDC 829250' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((Ph-NCN)Lu(THF)4)(BPh4)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C95 H111 B2 Lu N2 O4' _chemical_formula_weight 1541.45 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' B B 0.0013 0.0007 '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' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 14.5937(15) _cell_length_b 40.384(4) _cell_length_c 28.730(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.444(2) _cell_angle_gamma 90.00 _cell_volume 16926(3) _cell_formula_units_Z 8 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 395 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 25.0 _exptl_crystal_description fragment _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6464 _exptl_absorpt_coefficient_mu 1.217 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7507 _exptl_absorpt_correction_T_max 0.8385 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 92044 _diffrn_reflns_av_R_equivalents 0.1086 _diffrn_reflns_av_sigmaI/netI 0.1422 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 29679 _reflns_number_gt 17139 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXH-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (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. EADP has been used for the following atoms: EADP C14 C15 C14' C15' EADP C101 C102 C301 C302 ; _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^)+(0.0524P)^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 29679 _refine_ls_number_parameters 1875 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1137 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1369 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 0.903 _refine_ls_restrained_S_all 0.903 _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 C1 C 0.9929(5) 1.04680(16) 0.3553(3) 0.0438(19) Uani 1 1 d . . . H1A H 0.9542 1.0613 0.3352 0.053 Uiso 1 1 calc R . . H1B H 1.0581 1.0517 0.3495 0.053 Uiso 1 1 calc R . . C2 C 0.9722(6) 1.05221(19) 0.4057(3) 0.057(2) Uani 1 1 d . . . H2A H 1.0124 1.0695 0.4196 0.069 Uiso 1 1 calc R . . H2B H 0.9074 1.0586 0.4095 0.069 Uiso 1 1 calc R . . C3 C 0.9918(6) 1.0191(2) 0.4269(3) 0.069(3) Uani 1 1 d . . . H3A H 0.9588 1.0162 0.4563 0.083 Uiso 1 1 calc R . . H3B H 1.0583 1.0160 0.4331 0.083 Uiso 1 1 calc R . . C4 C 0.9568(5) 0.99499(17) 0.3899(2) 0.0412(18) Uani 1 1 d . . . H4A H 0.9910 0.9738 0.3916 0.049 Uiso 1 1 calc R . . H4B H 0.8907 0.9904 0.3935 0.049 Uiso 1 1 calc R . . C5 C 0.8140(5) 0.94177(18) 0.3203(3) 0.063(3) Uani 1 1 d . . . H5A H 0.7714 0.9562 0.3022 0.076 Uiso 1 1 calc R . . H5B H 0.8076 0.9468 0.3538 0.076 Uiso 1 1 calc R . . C6 C 0.7934(5) 0.90663(17) 0.3111(3) 0.049(2) Uani 1 1 d . . . H6A H 0.7622 0.9040 0.2803 0.059 Uiso 1 1 calc R . . H6B H 0.7535 0.8975 0.3353 0.059 Uiso 1 1 calc R . . C7 C 0.8864(5) 0.88895(16) 0.3119(3) 0.049(2) Uani 1 1 d . . . H7A H 0.8898 0.8720 0.3369 0.058 Uiso 1 1 calc R . . H7B H 0.8981 0.8783 0.2817 0.058 Uiso 1 1 calc R . . C8 C 0.9524(5) 0.91647(16) 0.3215(3) 0.0435(19) Uani 1 1 d . . . H8A H 0.9687 0.9175 0.3551 0.052 Uiso 1 1 calc R . . H8B H 1.0092 0.9130 0.3040 0.052 Uiso 1 1 calc R . . C9 C 1.1896(5) 1.02381(19) 0.2619(3) 0.051(2) Uani 1 1 d . . . H9A H 1.1704 1.0473 0.2637 0.061 Uiso 1 1 calc R . . H9B H 1.1920 1.0173 0.2288 0.061 Uiso 1 1 calc R . . C10 C 1.2809(5) 1.0191(2) 0.2854(3) 0.057(2) Uani 1 1 d . . . H10A H 1.2971 1.0386 0.3048 0.068 Uiso 1 1 calc R . . H10B H 1.3290 1.0159 0.2622 0.068 Uiso 1 1 calc R . . C11 C 1.2715(4) 0.98832(18) 0.3157(3) 0.045(2) Uani 1 1 d . . . H11A H 1.2891 0.9682 0.2985 0.055 Uiso 1 1 calc R . . H11B H 1.3101 0.9901 0.3444 0.055 Uiso 1 1 calc R . . C12 C 1.1728(5) 0.98769(18) 0.3267(3) 0.048(2) Uani 1 1 d . . . H12A H 1.1517 0.9647 0.3314 0.057 Uiso 1 1 calc R . . H12B H 1.1614 1.0006 0.3553 0.057 Uiso 1 1 calc R . . C13 C 1.1248(5) 0.93853(18) 0.2264(3) 0.054(2) Uani 1 1 d . . . H13A H 1.1654 0.9565 0.2156 0.065 Uiso 1 1 calc R A 1 H13B H 1.1479 0.9309 0.2572 0.065 Uiso 1 1 calc R A 1 C14 C 1.103(4) 0.9019(12) 0.207(2) 0.090(7) Uani 0.33(4) 1 d P B 2 H14A H 1.1423 0.8982 0.1797 0.107 Uiso 0.33(4) 1 calc PR B 2 H14B H 1.1219 0.8859 0.2310 0.107 Uiso 0.33(4) 1 calc PR B 2 C15 C 1.035(3) 0.8956(12) 0.196(2) 0.090(7) Uani 0.33(4) 1 d P B 2 H15A H 1.0097 0.8784 0.2165 0.107 Uiso 0.33(4) 1 calc PR B 2 H15B H 1.0337 0.8870 0.1636 0.107 Uiso 0.33(4) 1 calc PR B 2 C14' C 1.1246(14) 0.9111(8) 0.1932(12) 0.090(7) Uani 0.67(4) 1 d P B 1 H14C H 1.1705 0.9149 0.1690 0.107 Uiso 0.67(4) 1 calc PR B 1 H14D H 1.1389 0.8900 0.2093 0.107 Uiso 0.67(4) 1 calc PR B 1 C15' C 1.0337(11) 0.9104(8) 0.1730(12) 0.090(7) Uani 0.67(4) 1 d P B 1 H15C H 1.0113 0.8872 0.1722 0.107 Uiso 0.67(4) 1 calc PR B 1 H15D H 1.0353 0.9185 0.1405 0.107 Uiso 0.67(4) 1 calc PR B 1 C16 C 0.9714(5) 0.93040(19) 0.1988(3) 0.053(2) Uani 1 1 d . . . H16A H 0.9300 0.9164 0.2171 0.063 Uiso 1 1 calc R B 1 H16B H 0.9339 0.9446 0.1776 0.063 Uiso 1 1 calc R B 1 C17 C 0.8668(4) 1.03438(15) 0.2207(2) 0.0264(15) Uani 1 1 d . B . C18 C 0.8077(4) 1.05757(14) 0.1925(2) 0.0249(15) Uani 1 1 d . . . C19 C 0.7288(4) 1.07132(15) 0.2103(2) 0.0317(16) Uani 1 1 d . . . H19 H 0.7108 1.0650 0.2406 0.038 Uiso 1 1 calc R . . C20 C 0.6756(5) 1.09365(17) 0.1857(3) 0.0415(19) Uani 1 1 d . . . H20 H 0.6228 1.1031 0.1992 0.050 Uiso 1 1 calc R . . C21 C 0.6998(5) 1.10207(16) 0.1416(3) 0.0386(18) Uani 1 1 d . . . H21 H 0.6632 1.1176 0.1246 0.046 Uiso 1 1 calc R . . C22 C 0.7749(5) 1.08878(17) 0.1213(3) 0.0410(19) Uani 1 1 d . . . H22 H 0.7893 1.0945 0.0902 0.049 Uiso 1 1 calc R . . C23 C 0.8301(4) 1.06684(15) 0.1466(2) 0.0327(17) Uani 1 1 d . . . H23 H 0.8835 1.0580 0.1329 0.039 Uiso 1 1 calc R . . C24 C 1.0104(4) 1.05806(15) 0.1938(2) 0.0282(16) Uani 1 1 d . . . C25 C 1.0104(4) 1.09142(15) 0.2070(2) 0.0276(16) Uani 1 1 d . . . C26 C 0.9689(5) 1.10513(16) 0.2507(3) 0.0379(18) Uani 1 1 d . . . H26 H 0.9348 1.0867 0.2658 0.045 Uiso 1 1 calc R . . C27 C 0.9009(5) 1.13265(17) 0.2400(3) 0.057(2) Uani 1 1 d . . . H27A H 0.8750 1.1406 0.2691 0.086 Uiso 1 1 calc R . . H27B H 0.8516 1.1242 0.2195 0.086 Uiso 1 1 calc R . . H27C H 0.9323 1.1509 0.2245 0.086 Uiso 1 1 calc R . . C28 C 1.0445(5) 1.11676(18) 0.2852(3) 0.049(2) Uani 1 1 d . . . H28A H 1.0164 1.1253 0.3134 0.073 Uiso 1 1 calc R . . H28B H 1.0806 1.1343 0.2709 0.073 Uiso 1 1 calc R . . H28C H 1.0846 1.0981 0.2934 0.073 Uiso 1 1 calc R . . C29 C 1.0541(4) 1.11380(17) 0.1771(3) 0.0368(18) Uani 1 1 d . . . H29 H 1.0557 1.1366 0.1851 0.044 Uiso 1 1 calc R . . C30 C 1.0943(5) 1.10373(19) 0.1371(3) 0.0423(19) Uani 1 1 d . . . H30 H 1.1203 1.1195 0.1167 0.051 Uiso 1 1 calc R . . C31 C 1.0968(4) 1.07018(17) 0.1264(2) 0.0358(17) Uani 1 1 d . . . H31 H 1.1259 1.0630 0.0990 0.043 Uiso 1 1 calc R . . C32 C 1.0573(4) 1.04689(16) 0.1554(2) 0.0284(16) Uani 1 1 d . . . C33 C 1.0632(5) 1.01052(18) 0.1418(2) 0.0406(18) Uani 1 1 d . . . H33 H 1.0528 0.9971 0.1705 0.049 Uiso 1 1 calc R . . C34 C 0.9883(6) 1.0008(2) 0.1055(3) 0.072(3) Uani 1 1 d . . . H34A H 0.9938 0.9772 0.0981 0.107 Uiso 1 1 calc R . . H34B H 0.9957 1.0140 0.0772 0.107 Uiso 1 1 calc R . . H34C H 0.9278 1.0051 0.1183 0.107 Uiso 1 1 calc R . . C35 C 1.1574(5) 1.0011(2) 0.1239(3) 0.066(3) Uani 1 1 d . . . H35A H 1.1581 0.9774 0.1163 0.099 Uiso 1 1 calc R . . H35B H 1.2043 1.0057 0.1480 0.099 Uiso 1 1 calc R . . H35C H 1.1702 1.0140 0.0960 0.099 Uiso 1 1 calc R . . C36 C 0.7376(4) 1.00381(14) 0.2524(2) 0.0287(16) Uani 1 1 d . . . C37 C 0.6917(4) 0.98730(16) 0.2155(2) 0.0346(17) Uani 1 1 d . . . C38 C 0.7346(5) 0.97829(17) 0.1702(2) 0.0400(19) Uani 1 1 d . . . H38 H 0.7995 0.9862 0.1715 0.048 Uiso 1 1 calc R . . C39 C 0.7362(5) 0.94032(16) 0.1623(3) 0.047(2) Uani 1 1 d . . . H39A H 0.7650 0.9355 0.1327 0.071 Uiso 1 1 calc R . . H39B H 0.6733 0.9318 0.1616 0.071 Uiso 1 1 calc R . . H39C H 0.7713 0.9297 0.1878 0.071 Uiso 1 1 calc R . . C40 C 0.6867(5) 0.99497(19) 0.1288(3) 0.053(2) Uani 1 1 d . . . H40A H 0.7169 0.9885 0.1001 0.080 Uiso 1 1 calc R . . H40B H 0.6901 1.0191 0.1326 0.080 Uiso 1 1 calc R . . H40C H 0.6224 0.9881 0.1272 0.080 Uiso 1 1 calc R . . C41 C 0.5995(5) 0.97808(17) 0.2209(3) 0.0424(19) Uani 1 1 d . . . H41 H 0.5676 0.9668 0.1964 0.051 Uiso 1 1 calc R . . C42 C 0.5549(5) 0.98535(17) 0.2617(3) 0.0431(19) Uani 1 1 d . . . H42 H 0.4927 0.9790 0.2650 0.052 Uiso 1 1 calc R . . C43 C 0.5998(5) 1.00147(17) 0.2969(3) 0.046(2) Uani 1 1 d . . . H43 H 0.5679 1.0063 0.3245 0.055 Uiso 1 1 calc R . . C44 C 0.6903(4) 1.01109(15) 0.2940(2) 0.0281(15) Uani 1 1 d . . . C45 C 0.7395(4) 1.02704(16) 0.3359(2) 0.0325(16) Uani 1 1 d . . . H45 H 0.8046 1.0194 0.3355 0.039 Uiso 1 1 calc R . . C46 C 0.7005(5) 1.01585(18) 0.3827(2) 0.049(2) Uani 1 1 d . . . H46A H 0.7348 1.0266 0.4083 0.073 Uiso 1 1 calc R . . H46B H 0.7063 0.9918 0.3856 0.073 Uiso 1 1 calc R . . H46C H 0.6358 1.0221 0.3839 0.073 Uiso 1 1 calc R . . C47 C 0.7415(5) 1.06510(16) 0.3340(3) 0.045(2) Uani 1 1 d . . . H47A H 0.7744 1.0737 0.3616 0.068 Uiso 1 1 calc R . . H47B H 0.6787 1.0736 0.3332 0.068 Uiso 1 1 calc R . . H47C H 0.7728 1.0722 0.3059 0.068 Uiso 1 1 calc R . . C72 C 0.4708(4) 0.62830(15) 0.1636(2) 0.0320(17) Uani 1 1 d . . . C73 C 0.4116(5) 0.63769(16) 0.1987(3) 0.0402(18) Uani 1 1 d . . . H73 H 0.4333 0.6364 0.2301 0.048 Uiso 1 1 calc R . . C74 C 0.3232(5) 0.64874(17) 0.1902(3) 0.051(2) Uani 1 1 d . . . H74 H 0.2863 0.6550 0.2155 0.062 Uiso 1 1 calc R . . C75 C 0.2882(5) 0.65079(18) 0.1460(4) 0.056(2) Uani 1 1 d . . . H75 H 0.2274 0.6584 0.1400 0.068 Uiso 1 1 calc R . . C76 C 0.3444(6) 0.64141(17) 0.1099(3) 0.051(2) Uani 1 1 d . . . H76 H 0.3214 0.6423 0.0787 0.061 Uiso 1 1 calc R . . C77 C 0.4337(5) 0.63071(15) 0.1187(3) 0.0363(17) Uani 1 1 d . . . H77 H 0.4706 0.6249 0.0932 0.044 Uiso 1 1 calc R . . C78 C 0.6174(5) 0.59024(16) 0.1377(2) 0.0364(18) Uani 1 1 d . . . C79 C 0.7087(5) 0.58693(18) 0.1270(3) 0.045(2) Uani 1 1 d . . . H79 H 0.7523 0.6013 0.1414 0.054 Uiso 1 1 calc R . . C80 C 0.7392(6) 0.5631(2) 0.0956(3) 0.062(3) Uani 1 1 d . . . H80 H 0.8020 0.5622 0.0877 0.075 Uiso 1 1 calc R . . C81 C 0.6770(7) 0.5409(2) 0.0759(3) 0.068(3) Uani 1 1 d . . . H81 H 0.6972 0.5247 0.0545 0.082 Uiso 1 1 calc R . . C82 C 0.5877(7) 0.5423(2) 0.0872(3) 0.073(3) Uani 1 1 d . . . H82 H 0.5452 0.5266 0.0747 0.088 Uiso 1 1 calc R . . C83 C 0.5589(6) 0.56708(18) 0.1175(3) 0.054(2) Uani 1 1 d . . . H83 H 0.4957 0.5681 0.1246 0.064 Uiso 1 1 calc R . . C84 C 0.6325(4) 0.65382(16) 0.1746(2) 0.0326(17) Uani 1 1 d . . . C85 C 0.6144(5) 0.67689(18) 0.2099(3) 0.046(2) Uani 1 1 d . . . H85 H 0.5712 0.6710 0.2326 0.055 Uiso 1 1 calc R . . C86 C 0.6560(6) 0.70785(18) 0.2134(3) 0.052(2) Uani 1 1 d . . . H86 H 0.6408 0.7224 0.2380 0.062 Uiso 1 1 calc R . . C87 C 0.7190(5) 0.71726(18) 0.1812(3) 0.054(2) Uani 1 1 d . . . H87 H 0.7469 0.7385 0.1828 0.064 Uiso 1 1 calc R . . C88 C 0.7409(5) 0.6955(2) 0.1469(3) 0.059(2) Uani 1 1 d . . . H88 H 0.7867 0.7011 0.1254 0.070 Uiso 1 1 calc R . . C89 C 0.6963(5) 0.66477(17) 0.1432(3) 0.0436(19) Uani 1 1 d . . . H89 H 0.7105 0.6508 0.1178 0.052 Uiso 1 1 calc R . . C90 C 0.5950(4) 0.59998(16) 0.2260(2) 0.0319(17) Uani 1 1 d . . . C91 C 0.6766(5) 0.60417(17) 0.2515(2) 0.0379(18) Uani 1 1 d . . . H91 H 0.7216 0.6190 0.2404 0.046 Uiso 1 1 calc R . . C92 C 0.6936(5) 0.58699(19) 0.2929(3) 0.049(2) Uani 1 1 d . . . H92 H 0.7497 0.5904 0.3097 0.059 Uiso 1 1 calc R . . C93 C 0.6297(6) 0.56518(19) 0.3096(3) 0.055(2) Uani 1 1 d . . . H93 H 0.6421 0.5535 0.3377 0.066 Uiso 1 1 calc R . . C94 C 0.5488(5) 0.56035(19) 0.2859(3) 0.049(2) Uani 1 1 d . . . H94 H 0.5040 0.5455 0.2972 0.059 Uiso 1 1 calc R . . C95 C 0.5340(5) 0.57789(16) 0.2444(3) 0.0405(19) Uani 1 1 d . . . H95 H 0.4778 0.5743 0.2278 0.049 Uiso 1 1 calc R . . C96 C 0.4278(5) 0.1973(2) 0.9078(3) 0.052(2) Uani 1 1 d . . . H96A H 0.4921 0.1947 0.8982 0.062 Uiso 1 1 calc R . . H96B H 0.3990 0.2154 0.8894 0.062 Uiso 1 1 calc R . . C97 C 0.3764(7) 0.1660(3) 0.9010(4) 0.086(3) Uani 1 1 d . . . H97A H 0.3114 0.1707 0.8926 0.103 Uiso 1 1 calc R . . H97B H 0.4034 0.1527 0.8758 0.103 Uiso 1 1 calc R . . C98 C 0.3837(8) 0.1485(2) 0.9451(4) 0.100(4) Uani 1 1 d . . . H98A H 0.4394 0.1345 0.9466 0.120 Uiso 1 1 calc R . . H98B H 0.3293 0.1344 0.9498 0.120 Uiso 1 1 calc R . . C99 C 0.3893(6) 0.17576(19) 0.9811(3) 0.061(2) Uani 1 1 d . . . H99A H 0.3279 0.1803 0.9935 0.073 Uiso 1 1 calc R . . H99B H 0.4309 0.1693 1.0073 0.073 Uiso 1 1 calc R . . C100 C 0.2364(5) 0.2425(2) 0.9481(3) 0.067(3) Uani 1 1 d . . . H10U H 0.2466 0.2193 0.9385 0.081 Uiso 1 1 calc R C 1 H10V H 0.2558 0.2573 0.9227 0.081 Uiso 1 1 calc R C 1 C101 C 0.156(2) 0.2641(11) 0.9538(15) 0.068(5) Uani 0.41(3) 1 d P D 2 H10C H 0.1647 0.2852 0.9371 0.082 Uiso 0.41(3) 1 calc PR D 2 H10D H 0.1003 0.2532 0.9408 0.082 Uiso 0.41(3) 1 calc PR D 2 C102 C 0.147(2) 0.2699(11) 1.0008(16) 0.068(5) Uani 0.41(3) 1 d P D 2 H10E H 0.0885 0.2601 1.0112 0.082 Uiso 0.41(3) 1 calc PR D 2 H10F H 0.1443 0.2940 1.0065 0.082 Uiso 0.41(3) 1 calc PR D 2 C301 C 0.1359(16) 0.2482(8) 0.9586(10) 0.068(5) Uani 0.59(3) 1 d P D 1 H30A H 0.1116 0.2664 0.9387 0.082 Uiso 0.59(3) 1 calc PR D 1 H30B H 0.1007 0.2279 0.9509 0.082 Uiso 0.59(3) 1 calc PR D 1 C302 C 0.1248(16) 0.2557(8) 1.0020(11) 0.068(5) Uani 0.59(3) 1 d P D 1 H30C H 0.0845 0.2392 1.0167 0.082 Uiso 0.59(3) 1 calc PR D 1 H30D H 0.0960 0.2778 1.0044 0.082 Uiso 0.59(3) 1 calc PR D 1 C103 C 0.2219(5) 0.2558(2) 1.0271(3) 0.061(2) Uani 1 1 d . . . H10G H 0.2335 0.2774 1.0425 0.073 Uiso 1 1 calc R D 1 H10H H 0.2255 0.2381 1.0510 0.073 Uiso 1 1 calc R D 1 C104 C 0.4939(5) 0.32940(18) 1.0047(3) 0.052(2) Uani 1 1 d . . . H10I H 0.5373 0.3294 0.9787 0.063 Uiso 1 1 calc R . . H10J H 0.5273 0.3224 1.0334 0.063 Uiso 1 1 calc R . . C105 C 0.4547(5) 0.36347(18) 1.0110(3) 0.053(2) Uani 1 1 d . . . H10K H 0.4985 0.3809 1.0018 0.064 Uiso 1 1 calc R . . H10L H 0.4364 0.3673 1.0435 0.064 Uiso 1 1 calc R . . C106 C 0.3718(5) 0.36197(17) 0.9777(3) 0.051(2) Uani 1 1 d . . . H10M H 0.3255 0.3788 0.9858 0.061 Uiso 1 1 calc R . . H10N H 0.3901 0.3656 0.9451 0.061 Uiso 1 1 calc R . . C107 C 0.3352(4) 0.32736(17) 0.9843(3) 0.0401(19) Uani 1 1 d . . . H10O H 0.2927 0.3266 1.0105 0.048 Uiso 1 1 calc R . . H10P H 0.3026 0.3195 0.9557 0.048 Uiso 1 1 calc R . . C108 C 0.4888(5) 0.28235(19) 0.8946(3) 0.052(2) Uani 1 1 d . . . H10Q H 0.4878 0.3067 0.8990 0.063 Uiso 1 1 calc R . . H10R H 0.4251 0.2745 0.8895 0.063 Uiso 1 1 calc R . . C109 C 0.5474(5) 0.2732(2) 0.8534(3) 0.057(2) Uani 1 1 d . . . H10S H 0.5587 0.2928 0.8337 0.068 Uiso 1 1 calc R . . H10T H 0.5170 0.2559 0.8341 0.068 Uiso 1 1 calc R . . C110 C 0.6380(6) 0.2601(2) 0.8753(3) 0.061(2) Uani 1 1 d . . . H11U H 0.6459 0.2362 0.8685 0.073 Uiso 1 1 calc R . . H11V H 0.6910 0.2724 0.8632 0.073 Uiso 1 1 calc R . . C111 C 0.6298(5) 0.2656(2) 0.9265(3) 0.051(2) Uani 1 1 d . . . H11C H 0.6600 0.2475 0.9443 0.061 Uiso 1 1 calc R . . H11D H 0.6585 0.2869 0.9358 0.061 Uiso 1 1 calc R . . C112 C 0.5302(4) 0.23669(15) 1.0808(2) 0.0278(16) Uani 1 1 d . D . C113 C 0.5781(4) 0.22789(16) 1.1264(3) 0.0347(17) Uani 1 1 d . . . C114 C 0.5505(5) 0.24180(17) 1.1683(3) 0.0440(19) Uani 1 1 d . . . H114 H 0.5008 0.2570 1.1681 0.053 Uiso 1 1 calc R . . C115 C 0.5946(5) 0.23382(19) 1.2103(3) 0.048(2) Uani 1 1 d . . . H115 H 0.5762 0.2439 1.2384 0.058 Uiso 1 1 calc R . . C116 C 0.6652(6) 0.2112(2) 1.2108(3) 0.058(2) Uani 1 1 d . . . H116 H 0.6949 0.2053 1.2395 0.070 Uiso 1 1 calc R . . C117 C 0.6927(5) 0.1971(2) 1.1705(3) 0.059(2) Uani 1 1 d . . . H117 H 0.7422 0.1819 1.1711 0.070 Uiso 1 1 calc R . . C118 C 0.6490(4) 0.20487(17) 1.1285(3) 0.0388(18) Uani 1 1 d . . . H118 H 0.6678 0.1943 1.1007 0.047 Uiso 1 1 calc R . . C119 C 0.3785(4) 0.23916(18) 1.1137(2) 0.0359(18) Uani 1 1 d . . . C120 C 0.3366(5) 0.26815(19) 1.1314(3) 0.0427(19) Uani 1 1 d . . . C121 C 0.3616(5) 0.30259(19) 1.1144(3) 0.054(2) Uani 1 1 d . . . H121 H 0.3718 0.3009 1.0802 0.065 Uiso 1 1 calc R . . C122 C 0.2875(6) 0.3281(2) 1.1211(4) 0.089(3) Uani 1 1 d . . . H12U H 0.3079 0.3495 1.1092 0.134 Uiso 1 1 calc R . . H12V H 0.2748 0.3301 1.1543 0.134 Uiso 1 1 calc R . . H12C H 0.2316 0.3212 1.1041 0.134 Uiso 1 1 calc R . . C123 C 0.4499(6) 0.31630(19) 1.1370(3) 0.063(2) Uani 1 1 d . . . H12D H 0.4999 0.3005 1.1328 0.095 Uiso 1 1 calc R . . H12E H 0.4409 0.3198 1.1703 0.095 Uiso 1 1 calc R . . H12F H 0.4654 0.3374 1.1223 0.095 Uiso 1 1 calc R . . C124 C 0.2715(6) 0.2648(2) 1.1644(3) 0.062(2) Uani 1 1 d . . . H124 H 0.2415 0.2840 1.1755 0.074 Uiso 1 1 calc R . . C125 C 0.2477(5) 0.2338(3) 1.1825(3) 0.065(3) Uani 1 1 d . . . H125 H 0.2036 0.2322 1.2062 0.078 Uiso 1 1 calc R . . C126 C 0.2884(5) 0.2058(2) 1.1657(3) 0.055(2) Uani 1 1 d . . . H126 H 0.2712 0.1848 1.1774 0.066 Uiso 1 1 calc R . . C127 C 0.3557(5) 0.20775(18) 1.1310(3) 0.0399(18) Uani 1 1 d . . . C128 C 0.3997(5) 0.17589(17) 1.1152(3) 0.0424(19) Uani 1 1 d . . . H128 H 0.4447 0.1816 1.0907 0.051 Uiso 1 1 calc R . . C129 C 0.3281(5) 0.15235(19) 1.0932(3) 0.064(3) Uani 1 1 d . . . H12G H 0.3584 0.1320 1.0831 0.096 Uiso 1 1 calc R . . H12H H 0.2983 0.1631 1.0662 0.096 Uiso 1 1 calc R . . H12I H 0.2820 0.1469 1.1162 0.096 Uiso 1 1 calc R . . C130 C 0.4522(5) 0.15841(18) 1.1551(3) 0.052(2) Uani 1 1 d . . . H13U H 0.4801 0.1381 1.1434 0.078 Uiso 1 1 calc R . . H13V H 0.4098 0.1529 1.1798 0.078 Uiso 1 1 calc R . . H13C H 0.5003 0.1731 1.1675 0.078 Uiso 1 1 calc R . . C131 C 0.6713(4) 0.23647(17) 1.0358(2) 0.0339(17) Uani 1 1 d . . . C132 C 0.7077(5) 0.2089(2) 1.0129(3) 0.045(2) Uani 1 1 d . . . C133 C 0.6483(5) 0.1807(2) 0.9953(3) 0.062(3) Uani 1 1 d . . . H133 H 0.5829 0.1877 0.9974 0.075 Uiso 1 1 calc R . . C134 C 0.6640(7) 0.1702(2) 0.9454(3) 0.091(3) Uani 1 1 d . . . H13D H 0.6225 0.1519 0.9370 0.137 Uiso 1 1 calc R . . H13E H 0.7277 0.1628 0.9424 0.137 Uiso 1 1 calc R . . H13F H 0.6521 0.1889 0.9245 0.137 Uiso 1 1 calc R . . C135 C 0.6611(9) 0.1498(3) 1.0248(4) 0.125(5) Uani 1 1 d . . . H13G H 0.6503 0.1552 1.0575 0.187 Uiso 1 1 calc R . . H13H H 0.7238 0.1416 1.0217 0.187 Uiso 1 1 calc R . . H13I H 0.6175 0.1328 1.0142 0.187 Uiso 1 1 calc R . . C136 C 0.8017(6) 0.2073(2) 1.0070(3) 0.063(2) Uani 1 1 d . . . H136 H 0.8276 0.1886 0.9924 0.075 Uiso 1 1 calc R . . C137 C 0.8568(6) 0.2323(3) 1.0220(4) 0.075(3) Uani 1 1 d . . . H137 H 0.9207 0.2311 1.0166 0.090 Uiso 1 1 calc R . . C138 C 0.8228(5) 0.2592(2) 1.0446(3) 0.060(3) Uani 1 1 d . . . H138 H 0.8635 0.2759 1.0562 0.072 Uiso 1 1 calc R . . C139 C 0.7277(5) 0.2626(2) 1.0511(3) 0.049(2) Uani 1 1 d . . . C140 C 0.6913(5) 0.2931(2) 1.0752(3) 0.051(2) Uani 1 1 d . . . H140 H 0.6230 0.2912 1.0759 0.061 Uiso 1 1 calc R . . C141 C 0.7280(6) 0.2947(2) 1.1262(3) 0.079(3) Uani 1 1 d . . . H14U H 0.7029 0.3143 1.1414 0.119 Uiso 1 1 calc R . . H14V H 0.7950 0.2961 1.1265 0.119 Uiso 1 1 calc R . . H14W H 0.7092 0.2748 1.1429 0.119 Uiso 1 1 calc R . . C142 C 0.7152(5) 0.3260(2) 1.0497(3) 0.065(3) Uani 1 1 d . . . H14X H 0.6896 0.3448 1.0666 0.098 Uiso 1 1 calc R . . H14E H 0.6891 0.3255 1.0180 0.098 Uiso 1 1 calc R . . H14F H 0.7819 0.3284 1.0485 0.098 Uiso 1 1 calc R . . C143 C 1.0498(5) 0.1432(2) -0.0592(3) 0.046(2) Uani 1 1 d . . . C144 C 1.1179(5) 0.1341(2) -0.0903(3) 0.068(3) Uani 1 1 d . . . H144 H 1.1519 0.1144 -0.0845 0.081 Uiso 1 1 calc R . . C145 C 1.1372(7) 0.1528(4) -0.1289(4) 0.102(4) Uani 1 1 d . . . H145 H 1.1854 0.1458 -0.1483 0.122 Uiso 1 1 calc R . . C146 C 1.0912(9) 0.1807(3) -0.1406(4) 0.097(5) Uani 1 1 d . . . H146 H 1.1054 0.1929 -0.1677 0.117 Uiso 1 1 calc R . . C147 C 1.0225(7) 0.1907(2) -0.1115(4) 0.082(3) Uani 1 1 d . . . H147 H 0.9875 0.2099 -0.1190 0.099 Uiso 1 1 calc R . . C148 C 1.0040(5) 0.1728(2) -0.0713(3) 0.055(2) Uani 1 1 d . . . H148 H 0.9585 0.1809 -0.0512 0.066 Uiso 1 1 calc R . . C149 C 1.0939(6) 0.0612(2) -0.0208(4) 0.092(4) Uani 1 1 d . . . H149 H 1.0384 0.0551 -0.0367 0.110 Uiso 1 1 calc R . . C150 C 1.1617(7) 0.0372(2) -0.0147(4) 0.107(4) Uani 1 1 d . . . H150 H 1.1508 0.0152 -0.0252 0.128 Uiso 1 1 calc R . . C151 C 1.2426(6) 0.0449(2) 0.0060(3) 0.069(3) Uani 1 1 d . . . H151 H 1.2903 0.0289 0.0087 0.083 Uiso 1 1 calc R . . C152 C 1.2544(5) 0.0759(2) 0.0229(3) 0.057(2) Uani 1 1 d . . . H152 H 1.3101 0.0816 0.0387 0.068 Uiso 1 1 calc R . . C153 C 1.1855(5) 0.09931(18) 0.0172(3) 0.045(2) Uani 1 1 d . . . H153 H 1.1963 0.1208 0.0295 0.053 Uiso 1 1 calc R . . C154 C 1.1034(5) 0.09347(19) -0.0048(3) 0.0425(19) Uani 1 1 d . . . C155 C 1.0816(5) 0.17020(18) 0.0424(3) 0.048(2) Uani 1 1 d . . . H155 H 1.1328 0.1722 0.0228 0.058 Uiso 1 1 calc R . . C156 C 1.0774(6) 0.19043(18) 0.0816(3) 0.055(2) Uani 1 1 d . . . H156 H 1.1265 0.2052 0.0887 0.066 Uiso 1 1 calc R . . C157 C 1.0037(6) 0.1894(2) 0.1101(3) 0.059(2) Uani 1 1 d . . . H157 H 1.0011 0.2031 0.1369 0.071 Uiso 1 1 calc R . . C158 C 0.9329(5) 0.16775(19) 0.0989(3) 0.047(2) Uani 1 1 d . . . H158 H 0.8796 0.1671 0.1173 0.057 Uiso 1 1 calc R . . C159 C 0.9403(5) 0.14705(18) 0.0609(3) 0.045(2) Uani 1 1 d . . . H159 H 0.8921 0.1317 0.0548 0.054 Uiso 1 1 calc R . . C160 C 1.0138(5) 0.14720(15) 0.0309(2) 0.0323(17) Uani 1 1 d . . . C161 C 0.9247(4) 0.10231(16) -0.0239(2) 0.0329(17) Uani 1 1 d . . . C162 C 0.8665(4) 0.10641(17) -0.0622(2) 0.0367(18) Uani 1 1 d . . . H162 H 0.8825 0.1224 -0.0848 0.044 Uiso 1 1 calc R . . C163 C 0.7861(5) 0.08846(18) -0.0695(3) 0.045(2) Uani 1 1 d . . . H163 H 0.7489 0.0924 -0.0965 0.054 Uiso 1 1 calc R . . C164 C 0.7605(5) 0.06535(19) -0.0381(3) 0.049(2) Uani 1 1 d . . . H164 H 0.7067 0.0525 -0.0436 0.059 Uiso 1 1 calc R . . C165 C 0.8136(6) 0.06064(18) 0.0019(3) 0.057(2) Uani 1 1 d . . . H165 H 0.7946 0.0455 0.0251 0.069 Uiso 1 1 calc R . . C166 C 0.8956(6) 0.07829(18) 0.0081(3) 0.051(2) Uani 1 1 d . . . H166 H 0.9331 0.0739 0.0350 0.062 Uiso 1 1 calc R . . C167 C 0.0260(5) 0.64198(17) -0.0800(2) 0.0378(18) Uani 1 1 d . . . C168 C 0.0838(5) 0.63430(19) -0.1178(3) 0.047(2) Uani 1 1 d . . . H168 H 0.1218 0.6152 -0.1154 0.057 Uiso 1 1 calc R . . C169 C 0.0870(6) 0.6533(2) -0.1576(3) 0.059(2) Uani 1 1 d . . . H169 H 0.1269 0.6474 -0.1819 0.071 Uiso 1 1 calc R . . C170 C 0.0322(7) 0.6808(2) -0.1619(3) 0.069(3) Uani 1 1 d . . . H170 H 0.0321 0.6933 -0.1899 0.083 Uiso 1 1 calc R . . C171 C -0.0221(6) 0.6904(2) -0.1264(3) 0.061(2) Uani 1 1 d . . . H171 H -0.0573 0.7102 -0.1291 0.073 Uiso 1 1 calc R . . C172 C -0.0256(5) 0.67082(18) -0.0856(3) 0.055(2) Uani 1 1 d . . . H172 H -0.0643 0.6775 -0.0612 0.066 Uiso 1 1 calc R . . C173 C -0.0762(5) 0.59408(17) -0.0416(2) 0.0359(17) Uani 1 1 d . . . C174 C -0.1580(5) 0.60553(19) -0.0611(3) 0.047(2) Uani 1 1 d . . . H174 H -0.1587 0.6268 -0.0751 0.057 Uiso 1 1 calc R . . C175 C -0.2384(5) 0.5877(2) -0.0612(3) 0.052(2) Uani 1 1 d . . . H175 H -0.2931 0.5971 -0.0742 0.062 Uiso 1 1 calc R . . C176 C -0.2393(5) 0.5559(2) -0.0422(3) 0.048(2) Uani 1 1 d . . . H176 H -0.2941 0.5432 -0.0427 0.058 Uiso 1 1 calc R . . C177 C -0.1624(5) 0.54362(18) -0.0236(3) 0.045(2) Uani 1 1 d . . . H177 H -0.1624 0.5221 -0.0103 0.054 Uiso 1 1 calc R . . C178 C -0.0829(5) 0.56170(19) -0.0234(3) 0.047(2) Uani 1 1 d . . . H178 H -0.0291 0.5519 -0.0103 0.057 Uiso 1 1 calc R . . C179 C 0.0556(5) 0.66772(19) 0.0226(3) 0.051(2) Uani 1 1 d . . . H179 H 0.1002 0.6738 0.0006 0.061 Uiso 1 1 calc R . . C180 C 0.0491(6) 0.6860(2) 0.0630(3) 0.062(2) Uani 1 1 d . . . H180 H 0.0882 0.7045 0.0681 0.074 Uiso 1 1 calc R . . C181 C -0.0136(6) 0.6776(2) 0.0961(3) 0.062(2) Uani 1 1 d . . . H181 H -0.0174 0.6898 0.1242 0.075 Uiso 1 1 calc R . . C182 C -0.0705(6) 0.6511(2) 0.0875(3) 0.058(2) Uani 1 1 d . . . H182 H -0.1136 0.6448 0.1101 0.070 Uiso 1 1 calc R . . C183 C -0.0658(5) 0.63329(18) 0.0460(3) 0.045(2) Uani 1 1 d . . . H183 H -0.1079 0.6157 0.0402 0.054 Uiso 1 1 calc R . . C184 C -0.0011(5) 0.64071(18) 0.0129(3) 0.0383(18) Uani 1 1 d . . . C185 C 0.1084(5) 0.59441(17) -0.0247(3) 0.0386(18) Uani 1 1 d . . . C186 C 0.1289(5) 0.56833(18) -0.0553(3) 0.0450(19) Uani 1 1 d . . . H186 H 0.0886 0.5644 -0.0812 0.054 Uiso 1 1 calc R . . C187 C 0.2053(5) 0.54805(18) -0.0493(3) 0.050(2) Uani 1 1 d . . . H187 H 0.2160 0.5305 -0.0706 0.060 Uiso 1 1 calc R . . C188 C 0.2650(6) 0.55344(19) -0.0128(3) 0.054(2) Uani 1 1 d . . . H188 H 0.3169 0.5395 -0.0082 0.065 Uiso 1 1 calc R . . C189 C 0.2497(5) 0.57905(18) 0.0172(3) 0.046(2) Uani 1 1 d . . . H189 H 0.2922 0.5833 0.0421 0.055 Uiso 1 1 calc R . . C190 C 0.1725(5) 0.59872(17) 0.0115(2) 0.0415(19) Uani 1 1 d . . . H190 H 0.1629 0.6160 0.0333 0.050 Uiso 1 1 calc R . . C191 C 0.5751(4) 0.40535(16) 0.3034(3) 0.0340(17) Uani 1 1 d . . . C192 C 0.6224(4) 0.43394(17) 0.2933(3) 0.0416(19) Uani 1 1 d . . . H192 H 0.6515 0.4354 0.2641 0.050 Uiso 1 1 calc R . . C193 C 0.6299(5) 0.46065(19) 0.3233(3) 0.051(2) Uani 1 1 d . . . H193 H 0.6623 0.4799 0.3144 0.061 Uiso 1 1 calc R . . C194 C 0.5904(6) 0.4592(2) 0.3661(3) 0.059(2) Uani 1 1 d . . . H194 H 0.5959 0.4773 0.3871 0.070 Uiso 1 1 calc R . . C195 C 0.5425(6) 0.4311(2) 0.3785(3) 0.059(2) Uani 1 1 d . . . H195 H 0.5138 0.4298 0.4077 0.071 Uiso 1 1 calc R . . C196 C 0.5370(5) 0.4045(2) 0.3467(3) 0.054(2) Uani 1 1 d . . . H196 H 0.5056 0.3850 0.3557 0.065 Uiso 1 1 calc R . . C197 C 0.6594(5) 0.34879(16) 0.2803(3) 0.0375(18) Uani 1 1 d . . . C198 C 0.7064(5) 0.34900(17) 0.3224(3) 0.0398(18) Uani 1 1 d . . . H198 H 0.6879 0.3642 0.3455 0.048 Uiso 1 1 calc R . . C199 C 0.7802(5) 0.32786(19) 0.3329(3) 0.053(2) Uani 1 1 d . . . H199 H 0.8110 0.3292 0.3623 0.063 Uiso 1 1 calc R . . C200 C 0.8079(6) 0.3052(2) 0.3004(3) 0.066(3) Uani 1 1 d . . . H200 H 0.8590 0.2912 0.3068 0.079 Uiso 1 1 calc R . . C201 C 0.7602(6) 0.3032(2) 0.2584(3) 0.072(3) Uani 1 1 d . . . H201 H 0.7764 0.2869 0.2362 0.086 Uiso 1 1 calc R . . C202 C 0.6885(5) 0.32486(18) 0.2486(3) 0.051(2) Uani 1 1 d . . . H202 H 0.6577 0.3234 0.2191 0.061 Uiso 1 1 calc R . . C203 C 0.5764(5) 0.38784(17) 0.2131(3) 0.0405(19) Uani 1 1 d . . . C204 C 0.5023(6) 0.4003(2) 0.1892(3) 0.055(2) Uani 1 1 d . . . H204 H 0.4446 0.3994 0.2038 0.066 Uiso 1 1 calc R . . C205 C 0.5050(7) 0.4144(2) 0.1450(3) 0.071(3) Uani 1 1 d . . . H205 H 0.4510 0.4232 0.1306 0.086 Uiso 1 1 calc R . . C206 C 0.5861(8) 0.4152(2) 0.1228(3) 0.073(3) Uani 1 1 d . . . H206 H 0.5888 0.4238 0.0920 0.087 Uiso 1 1 calc R . . C207 C 0.6639(7) 0.4035(2) 0.1448(4) 0.077(3) Uani 1 1 d . . . H207 H 0.7210 0.4047 0.1298 0.093 Uiso 1 1 calc R . . C208 C 0.6595(6) 0.3901(2) 0.1888(3) 0.064(2) Uani 1 1 d . . . H208 H 0.7142 0.3820 0.2034 0.077 Uiso 1 1 calc R . . C209 C 0.4759(5) 0.35239(16) 0.2731(2) 0.0342(16) Uani 1 1 d . . . C210 C 0.3908(5) 0.36816(18) 0.2750(2) 0.0428(19) Uani 1 1 d . . . H210 H 0.3882 0.3917 0.2747 0.051 Uiso 1 1 calc R . . C211 C 0.3093(5) 0.3500(2) 0.2773(3) 0.058(2) Uani 1 1 d . . . H211 H 0.2529 0.3617 0.2787 0.069 Uiso 1 1 calc R . . C212 C 0.3076(6) 0.3165(3) 0.2776(3) 0.065(3) Uani 1 1 d . . . H212 H 0.2516 0.3045 0.2777 0.079 Uiso 1 1 calc R . . C213 C 0.3905(7) 0.3008(2) 0.2779(3) 0.068(3) Uani 1 1 d . . . H213 H 0.3923 0.2774 0.2802 0.082 Uiso 1 1 calc R . . C214 C 0.4721(6) 0.31815(19) 0.2748(3) 0.053(2) Uani 1 1 d . . . H214 H 0.5278 0.3060 0.2739 0.063 Uiso 1 1 calc R . . B1 B 0.5801(5) 0.61812(19) 0.1747(3) 0.034(2) Uani 1 1 d . . . B2 B 1.0233(5) 0.1217(2) -0.0141(3) 0.039(2) Uani 1 1 d . . . B3 B 0.0163(6) 0.6169(2) -0.0340(3) 0.042(2) Uani 1 1 d . . . B4 B 0.5727(6) 0.37336(19) 0.2669(3) 0.036(2) Uani 1 1 d . . . N1 N 0.9596(3) 1.03429(12) 0.22060(18) 0.0293(13) Uani 1 1 d . B . N2 N 0.8316(3) 1.01202(12) 0.24955(18) 0.0268(13) Uani 1 1 d . B . N3 N 0.4407(3) 0.24344(12) 1.07620(18) 0.0288(13) Uani 1 1 d . D . N4 N 0.5733(3) 0.23906(13) 1.0397(2) 0.0374(15) Uani 1 1 d . D . O1 O 0.9729(3) 1.01214(10) 0.34576(15) 0.0332(11) Uani 1 1 d . B . O2 O 0.9069(3) 0.94726(10) 0.30652(16) 0.0381(12) Uani 1 1 d . B . O3 O 1.1253(3) 1.00248(11) 0.28689(16) 0.0368(12) Uani 1 1 d . B . O4 O 1.0307(3) 0.95085(11) 0.22987(17) 0.0414(12) Uani 1 1 d . B . O5 O 0.4240(3) 0.20448(11) 0.95800(16) 0.0394(12) Uani 1 1 d . D . O6 O 0.2884(3) 0.24994(11) 0.99141(17) 0.0435(12) Uani 1 1 d . D . O7 O 0.4186(3) 0.30682(11) 0.99446(16) 0.0393(12) Uani 1 1 d . D . O8 O 0.5311(3) 0.26618(11) 0.93476(16) 0.0415(12) Uani 1 1 d . D . Lu1 Lu 0.972880(19) 0.992063(7) 0.272744(10) 0.02746(8) Uani 1 1 d . . . Lu2 Lu 0.445045(19) 0.252020(7) 0.997702(11) 0.03125(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.059(5) 0.031(4) 0.042(5) 0.001(4) -0.002(4) -0.006(4) C2 0.079(6) 0.050(5) 0.043(6) -0.014(4) 0.001(5) -0.004(4) C3 0.092(7) 0.078(7) 0.037(5) 0.000(5) -0.003(5) -0.025(5) C4 0.060(5) 0.039(4) 0.025(4) 0.009(3) 0.001(4) 0.001(4) C5 0.054(6) 0.044(5) 0.093(8) 0.030(5) 0.028(5) 0.011(4) C6 0.048(5) 0.043(5) 0.056(6) -0.001(4) -0.002(4) -0.011(4) C7 0.047(5) 0.027(4) 0.072(6) 0.008(4) -0.002(4) -0.002(4) C8 0.041(4) 0.041(5) 0.049(5) 0.011(4) -0.001(4) -0.003(4) C9 0.041(5) 0.062(5) 0.049(6) 0.012(4) 0.002(4) -0.006(4) C10 0.035(5) 0.064(6) 0.072(7) 0.014(5) 0.002(4) -0.004(4) C11 0.031(4) 0.053(5) 0.052(5) -0.006(4) -0.002(4) 0.001(4) C12 0.052(5) 0.045(5) 0.044(5) 0.010(4) -0.008(4) -0.004(4) C13 0.032(4) 0.049(5) 0.082(7) -0.017(5) 0.005(4) 0.010(4) C14 0.068(7) 0.070(13) 0.130(16) -0.057(11) 0.001(8) 0.014(7) C15 0.068(7) 0.070(13) 0.130(16) -0.057(11) 0.001(8) 0.014(7) C14' 0.068(7) 0.070(13) 0.130(16) -0.057(11) 0.001(8) 0.014(7) C15' 0.068(7) 0.070(13) 0.130(16) -0.057(11) 0.001(8) 0.014(7) C16 0.051(5) 0.055(5) 0.051(6) -0.008(4) -0.008(4) -0.003(4) C17 0.030(4) 0.021(4) 0.028(4) -0.004(3) -0.001(3) -0.001(3) C18 0.018(3) 0.023(3) 0.034(4) 0.004(3) 0.001(3) -0.004(3) C19 0.031(4) 0.033(4) 0.031(4) 0.005(3) 0.001(3) -0.004(3) C20 0.040(4) 0.037(4) 0.047(5) 0.004(4) 0.006(4) 0.007(3) C21 0.034(4) 0.036(4) 0.046(5) 0.019(4) -0.001(4) 0.006(3) C22 0.037(4) 0.054(5) 0.032(5) 0.014(4) 0.001(4) 0.002(4) C23 0.028(4) 0.037(4) 0.033(4) 0.008(3) 0.004(3) -0.002(3) C24 0.021(4) 0.028(4) 0.036(4) 0.011(3) -0.002(3) -0.002(3) C25 0.017(3) 0.030(4) 0.036(4) 0.010(3) 0.001(3) -0.003(3) C26 0.037(4) 0.029(4) 0.048(5) 0.007(4) 0.009(4) -0.006(3) C27 0.045(5) 0.043(5) 0.084(7) -0.009(4) 0.016(5) -0.007(4) C28 0.055(5) 0.050(5) 0.041(5) -0.016(4) 0.004(4) -0.014(4) C29 0.034(4) 0.035(4) 0.042(5) 0.006(4) 0.001(4) -0.003(3) C30 0.035(4) 0.052(5) 0.039(5) 0.018(4) -0.004(4) -0.009(4) C31 0.028(4) 0.049(5) 0.030(4) 0.005(4) 0.001(3) 0.001(3) C32 0.022(4) 0.037(4) 0.026(4) 0.003(3) -0.001(3) 0.002(3) C33 0.040(4) 0.051(5) 0.032(5) 0.004(4) 0.017(3) -0.001(4) C34 0.080(6) 0.057(6) 0.078(7) -0.023(5) -0.014(5) 0.008(5) C35 0.072(6) 0.070(6) 0.057(6) 0.001(5) 0.021(5) 0.025(5) C36 0.023(4) 0.019(3) 0.044(5) 0.008(3) 0.001(3) 0.001(3) C37 0.031(4) 0.031(4) 0.041(5) 0.002(3) -0.001(3) -0.005(3) C38 0.034(4) 0.051(5) 0.036(5) -0.008(4) 0.006(4) -0.018(3) C39 0.032(4) 0.043(5) 0.067(6) -0.014(4) 0.011(4) -0.003(3) C40 0.060(5) 0.067(6) 0.032(5) 0.002(4) -0.004(4) -0.006(4) C41 0.031(4) 0.052(5) 0.044(5) -0.002(4) 0.000(4) -0.008(3) C42 0.034(4) 0.040(5) 0.056(6) -0.004(4) 0.005(4) -0.012(3) C43 0.037(5) 0.051(5) 0.050(5) -0.003(4) 0.018(4) 0.009(4) C44 0.026(4) 0.028(4) 0.031(4) 0.009(3) 0.009(3) 0.009(3) C45 0.034(4) 0.037(4) 0.027(4) 0.000(3) -0.001(3) 0.003(3) C46 0.054(5) 0.059(5) 0.034(5) 0.004(4) 0.007(4) 0.002(4) C47 0.047(5) 0.041(5) 0.048(5) -0.005(4) -0.001(4) 0.009(4) C72 0.031(4) 0.033(4) 0.032(4) 0.000(3) 0.002(3) -0.001(3) C73 0.036(4) 0.043(5) 0.042(5) 0.001(4) -0.001(4) -0.006(3) C74 0.035(5) 0.038(5) 0.082(7) -0.005(5) 0.006(5) 0.002(4) C75 0.036(5) 0.044(5) 0.089(8) 0.003(5) -0.008(5) 0.000(4) C76 0.060(6) 0.039(5) 0.052(6) 0.013(4) -0.028(5) -0.007(4) C77 0.040(4) 0.034(4) 0.036(5) 0.006(3) 0.005(4) -0.004(3) C78 0.042(5) 0.036(4) 0.031(4) 0.005(3) 0.010(4) -0.001(3) C79 0.043(5) 0.050(5) 0.043(5) 0.008(4) 0.007(4) 0.013(4) C80 0.058(6) 0.061(6) 0.069(7) 0.026(5) 0.033(5) 0.028(5) C81 0.107(8) 0.041(5) 0.059(7) -0.002(5) 0.037(6) 0.011(5) C82 0.085(7) 0.059(6) 0.076(7) -0.015(5) 0.026(6) -0.008(5) C83 0.067(6) 0.041(5) 0.054(6) -0.018(4) 0.025(5) 0.003(4) C84 0.031(4) 0.037(4) 0.030(4) 0.003(3) 0.009(3) 0.005(3) C85 0.043(5) 0.053(5) 0.042(5) 0.007(4) 0.009(4) 0.002(4) C86 0.067(6) 0.037(5) 0.051(6) -0.010(4) -0.005(5) 0.001(4) C87 0.045(5) 0.031(5) 0.083(7) -0.003(5) -0.019(5) -0.009(4) C88 0.043(5) 0.057(6) 0.077(7) 0.004(5) 0.002(5) -0.014(4) C89 0.041(5) 0.040(5) 0.050(5) -0.001(4) 0.004(4) 0.001(4) C90 0.024(4) 0.031(4) 0.041(5) -0.001(3) 0.005(3) 0.007(3) C91 0.039(4) 0.043(4) 0.033(5) 0.001(4) 0.003(4) 0.007(3) C92 0.038(5) 0.058(5) 0.049(6) -0.020(4) -0.013(4) 0.014(4) C93 0.066(6) 0.054(6) 0.046(6) 0.007(4) 0.005(5) 0.025(5) C94 0.043(5) 0.061(5) 0.043(5) 0.016(4) 0.013(4) 0.009(4) C95 0.039(4) 0.038(4) 0.045(5) 0.002(4) 0.007(4) 0.002(3) C96 0.058(5) 0.067(6) 0.030(5) -0.012(4) -0.005(4) 0.001(4) C97 0.081(7) 0.098(8) 0.079(8) -0.051(7) 0.015(6) -0.011(6) C98 0.146(10) 0.052(6) 0.100(9) 0.011(6) -0.052(8) -0.040(6) C99 0.064(6) 0.050(5) 0.069(7) 0.003(5) 0.001(5) -0.019(4) C100 0.050(5) 0.106(8) 0.044(6) 0.002(5) -0.014(4) 0.015(5) C101 0.021(9) 0.107(19) 0.076(7) -0.010(14) -0.009(8) -0.005(8) C102 0.021(9) 0.107(19) 0.076(7) -0.010(14) -0.009(8) -0.005(8) C301 0.021(9) 0.107(19) 0.076(7) -0.010(14) -0.009(8) -0.005(8) C302 0.021(9) 0.107(19) 0.076(7) -0.010(14) -0.009(8) -0.005(8) C103 0.050(5) 0.076(6) 0.058(6) -0.001(5) 0.007(5) 0.000(4) C104 0.051(5) 0.050(5) 0.057(6) 0.010(4) 0.002(4) -0.010(4) C105 0.078(6) 0.042(5) 0.039(5) 0.000(4) -0.004(4) -0.007(4) C106 0.065(5) 0.039(5) 0.049(6) -0.002(4) 0.007(4) 0.009(4) C107 0.034(4) 0.048(5) 0.039(5) 0.009(4) 0.004(4) 0.012(4) C108 0.047(5) 0.059(5) 0.050(6) 0.024(4) -0.009(4) 0.004(4) C109 0.063(6) 0.062(6) 0.045(6) 0.006(4) -0.001(5) 0.001(4) C110 0.073(6) 0.067(6) 0.045(6) 0.016(4) 0.033(5) 0.016(5) C111 0.035(5) 0.061(5) 0.056(6) 0.006(4) 0.010(4) 0.008(4) C112 0.028(4) 0.025(4) 0.030(4) 0.003(3) 0.003(3) -0.001(3) C113 0.025(4) 0.039(4) 0.040(5) 0.006(4) 0.002(3) -0.007(3) C114 0.047(5) 0.044(5) 0.041(5) -0.001(4) 0.005(4) -0.007(4) C115 0.060(5) 0.056(5) 0.029(5) -0.006(4) -0.001(4) -0.003(4) C116 0.058(6) 0.082(7) 0.034(5) 0.021(5) -0.012(4) 0.000(5) C117 0.049(5) 0.076(6) 0.051(6) 0.018(5) 0.001(5) 0.014(4) C118 0.038(4) 0.047(5) 0.032(5) -0.001(4) -0.001(3) 0.011(4) C119 0.023(4) 0.056(5) 0.028(4) 0.001(4) 0.001(3) 0.002(3) C120 0.037(4) 0.054(5) 0.038(5) 0.006(4) 0.009(4) 0.016(4) C121 0.067(6) 0.057(6) 0.039(5) 0.000(4) 0.009(4) 0.025(5) C122 0.091(7) 0.067(7) 0.111(9) 0.002(6) 0.020(7) 0.045(6) C123 0.086(7) 0.050(5) 0.053(6) 0.006(4) -0.010(5) -0.001(5) C124 0.054(6) 0.080(7) 0.051(6) 0.003(5) 0.005(5) 0.029(5) C125 0.042(5) 0.112(8) 0.043(6) 0.012(6) 0.017(4) 0.010(5) C126 0.048(5) 0.078(6) 0.040(5) 0.012(5) 0.013(4) -0.024(5) C127 0.038(4) 0.045(5) 0.037(5) -0.001(4) 0.004(4) -0.012(4) C128 0.048(5) 0.043(5) 0.036(5) 0.002(4) 0.007(4) -0.011(4) C129 0.059(6) 0.065(6) 0.068(7) -0.001(5) 0.003(5) -0.030(5) C130 0.057(5) 0.045(5) 0.055(6) 0.019(4) 0.003(4) -0.014(4) C131 0.030(4) 0.044(4) 0.027(4) 0.010(3) 0.001(3) 0.003(3) C132 0.033(4) 0.068(6) 0.035(5) 0.014(4) 0.007(4) 0.015(4) C133 0.043(5) 0.059(6) 0.086(8) -0.012(5) 0.017(5) 0.021(4) C134 0.123(9) 0.070(7) 0.079(8) -0.007(6) -0.016(7) 0.024(6) C135 0.209(14) 0.105(10) 0.062(8) -0.002(7) 0.034(8) -0.043(9) C136 0.051(6) 0.074(7) 0.064(7) 0.015(5) 0.009(5) 0.017(5) C137 0.041(6) 0.076(7) 0.109(9) 0.019(6) 0.010(6) 0.006(5) C138 0.039(5) 0.056(6) 0.086(7) 0.027(5) -0.005(5) -0.009(4) C139 0.033(5) 0.068(6) 0.047(5) 0.004(4) 0.006(4) -0.002(4) C140 0.031(4) 0.090(7) 0.032(5) 0.003(4) 0.001(4) -0.029(4) C141 0.092(7) 0.089(7) 0.057(7) -0.007(5) -0.001(5) -0.051(6) C142 0.054(5) 0.070(6) 0.072(7) 0.007(5) -0.001(5) -0.028(5) C143 0.038(5) 0.072(6) 0.028(5) -0.011(4) 0.001(4) -0.010(4) C144 0.038(5) 0.124(8) 0.040(6) -0.001(5) 0.001(4) -0.010(5) C145 0.059(7) 0.209(15) 0.039(7) 0.002(8) 0.014(5) -0.047(8) C146 0.093(10) 0.156(12) 0.042(7) 0.039(7) -0.008(7) -0.075(8) C147 0.070(7) 0.086(8) 0.089(9) 0.031(6) -0.003(6) -0.029(6) C148 0.053(5) 0.065(6) 0.048(6) 0.015(5) 0.002(4) -0.015(5) C149 0.065(6) 0.074(7) 0.134(10) -0.061(7) -0.051(6) 0.031(5) C150 0.078(7) 0.081(7) 0.159(12) -0.078(8) -0.044(7) 0.040(6) C151 0.059(6) 0.062(6) 0.086(8) -0.024(5) -0.013(5) 0.024(5) C152 0.033(5) 0.074(6) 0.063(6) -0.001(5) -0.006(4) 0.006(4) C153 0.043(5) 0.042(5) 0.049(5) -0.005(4) 0.002(4) 0.005(4) C154 0.036(4) 0.059(5) 0.033(5) -0.007(4) -0.004(4) 0.009(4) C155 0.053(5) 0.042(5) 0.050(6) -0.001(4) 0.004(4) 0.005(4) C156 0.067(6) 0.044(5) 0.053(6) -0.007(4) -0.009(5) -0.010(4) C157 0.077(7) 0.054(6) 0.046(6) -0.011(4) 0.007(5) 0.019(5) C158 0.050(5) 0.055(5) 0.038(5) 0.001(4) 0.015(4) 0.011(4) C159 0.048(5) 0.044(5) 0.044(5) 0.000(4) 0.009(4) 0.010(4) C160 0.041(4) 0.027(4) 0.029(4) 0.004(3) -0.001(3) 0.010(3) C161 0.027(4) 0.039(4) 0.033(4) 0.003(3) 0.002(3) 0.009(3) C162 0.037(4) 0.042(4) 0.032(5) 0.003(3) 0.003(3) 0.008(3) C163 0.036(5) 0.059(5) 0.039(5) -0.004(4) 0.002(4) 0.007(4) C164 0.049(5) 0.052(5) 0.046(6) -0.011(4) 0.008(4) -0.010(4) C165 0.084(7) 0.035(5) 0.053(6) -0.001(4) 0.011(5) -0.015(4) C166 0.069(6) 0.047(5) 0.037(5) 0.000(4) -0.004(4) 0.003(4) C167 0.038(4) 0.043(5) 0.033(5) -0.004(4) 0.001(4) -0.017(4) C168 0.050(5) 0.050(5) 0.042(5) -0.007(4) 0.009(4) -0.009(4) C169 0.046(5) 0.082(7) 0.049(6) 0.002(5) 0.009(4) -0.027(5) C170 0.070(7) 0.087(8) 0.050(7) 0.014(5) -0.002(5) -0.030(6) C171 0.065(6) 0.043(5) 0.074(7) 0.017(5) -0.008(5) -0.014(4) C172 0.062(6) 0.038(5) 0.066(6) 0.009(4) 0.018(5) -0.003(4) C173 0.037(4) 0.041(4) 0.031(4) -0.004(3) 0.005(3) -0.002(3) C174 0.044(5) 0.058(5) 0.040(5) 0.003(4) 0.008(4) -0.003(4) C175 0.034(5) 0.072(6) 0.049(6) -0.009(5) 0.004(4) -0.005(4) C176 0.052(5) 0.061(6) 0.032(5) -0.019(4) 0.015(4) -0.020(4) C177 0.056(5) 0.045(5) 0.035(5) 0.001(4) 0.008(4) -0.006(4) C178 0.048(5) 0.052(5) 0.042(5) -0.001(4) 0.006(4) 0.000(4) C179 0.043(5) 0.054(5) 0.056(6) -0.020(4) 0.014(4) 0.004(4) C180 0.063(6) 0.056(6) 0.068(7) -0.019(5) 0.017(5) -0.013(5) C181 0.066(6) 0.064(6) 0.058(6) -0.026(5) 0.006(5) 0.008(5) C182 0.052(5) 0.083(7) 0.041(6) -0.001(5) 0.024(4) 0.013(5) C183 0.043(5) 0.043(5) 0.050(6) -0.001(4) 0.001(4) 0.003(4) C184 0.034(4) 0.045(5) 0.036(5) -0.001(4) 0.002(4) 0.008(4) C185 0.033(4) 0.047(5) 0.036(5) 0.003(4) 0.000(4) -0.010(3) C186 0.045(5) 0.054(5) 0.036(5) -0.010(4) 0.005(4) 0.000(4) C187 0.054(5) 0.043(5) 0.054(6) -0.007(4) 0.008(4) 0.003(4) C188 0.060(6) 0.055(5) 0.047(6) 0.001(4) 0.002(5) 0.015(4) C189 0.061(5) 0.047(5) 0.030(5) 0.003(4) -0.006(4) 0.007(4) C190 0.053(5) 0.043(5) 0.029(5) -0.002(4) 0.008(4) -0.002(4) C191 0.032(4) 0.033(4) 0.037(5) -0.001(3) -0.004(3) 0.000(3) C192 0.033(4) 0.039(4) 0.053(5) -0.005(4) 0.001(4) -0.004(3) C193 0.038(5) 0.045(5) 0.069(7) -0.007(5) -0.008(4) -0.001(4) C194 0.061(6) 0.045(5) 0.069(7) -0.025(5) -0.017(5) 0.011(4) C195 0.061(6) 0.074(7) 0.043(6) -0.014(5) -0.006(4) 0.026(5) C196 0.057(5) 0.061(6) 0.044(6) -0.011(4) 0.010(4) 0.003(4) C197 0.047(5) 0.031(4) 0.035(5) -0.004(3) 0.010(4) 0.002(3) C198 0.045(5) 0.039(4) 0.036(5) -0.002(4) 0.012(4) -0.001(4) C199 0.042(5) 0.056(5) 0.060(6) 0.009(5) -0.006(4) -0.001(4) C200 0.057(6) 0.073(6) 0.066(7) -0.008(5) -0.002(5) 0.028(5) C201 0.077(7) 0.068(6) 0.072(7) -0.013(5) 0.013(6) 0.032(5) C202 0.063(6) 0.052(5) 0.038(5) -0.004(4) -0.003(4) 0.014(4) C203 0.048(5) 0.036(4) 0.038(5) -0.007(4) 0.015(4) -0.006(4) C204 0.047(5) 0.079(6) 0.039(5) 0.017(5) 0.009(4) -0.010(4) C205 0.069(7) 0.079(7) 0.067(7) 0.027(5) 0.011(6) -0.007(5) C206 0.111(9) 0.059(6) 0.049(6) 0.004(5) 0.017(6) -0.008(6) C207 0.081(8) 0.079(7) 0.074(8) 0.013(6) 0.044(6) 0.002(6) C208 0.056(6) 0.072(6) 0.064(7) 0.011(5) 0.017(5) 0.010(5) C209 0.046(4) 0.030(4) 0.027(4) 0.001(3) 0.005(3) 0.005(3) C210 0.045(5) 0.047(5) 0.037(5) 0.013(4) 0.015(4) -0.004(4) C211 0.048(5) 0.093(7) 0.033(5) 0.019(5) 0.002(4) 0.001(5) C212 0.064(7) 0.079(7) 0.054(6) 0.007(5) 0.000(5) -0.031(6) C213 0.091(8) 0.049(6) 0.065(7) -0.005(5) 0.025(6) -0.019(5) C214 0.058(5) 0.048(5) 0.052(6) -0.002(4) 0.013(4) 0.000(4) B1 0.037(5) 0.034(5) 0.031(5) 0.010(4) 0.003(4) 0.001(4) B2 0.031(5) 0.049(6) 0.038(5) 0.001(4) 0.004(4) 0.005(4) B3 0.036(5) 0.042(5) 0.049(6) -0.005(5) 0.008(4) -0.003(4) B4 0.040(5) 0.034(5) 0.035(5) -0.004(4) 0.010(4) 0.007(4) N1 0.028(3) 0.031(3) 0.028(3) 0.003(3) -0.005(3) 0.000(2) N2 0.020(3) 0.024(3) 0.037(4) 0.009(3) -0.001(2) -0.005(2) N3 0.020(3) 0.042(4) 0.025(3) 0.001(3) 0.012(2) 0.000(2) N4 0.019(3) 0.043(4) 0.050(4) -0.011(3) 0.004(3) -0.003(3) O1 0.045(3) 0.025(3) 0.030(3) 0.000(2) 0.003(2) -0.001(2) O2 0.039(3) 0.029(3) 0.046(3) 0.009(2) 0.003(2) -0.005(2) O3 0.030(3) 0.043(3) 0.037(3) 0.003(2) -0.007(2) -0.009(2) O4 0.033(3) 0.044(3) 0.047(3) -0.010(3) -0.001(2) -0.002(2) O5 0.054(3) 0.037(3) 0.027(3) -0.005(2) 0.002(2) 0.001(2) O6 0.026(3) 0.058(3) 0.047(3) 0.000(3) 0.007(2) 0.000(2) O7 0.036(3) 0.037(3) 0.045(3) 0.003(2) 0.005(2) -0.004(2) O8 0.038(3) 0.049(3) 0.038(3) 0.008(2) 0.008(2) -0.001(2) Lu1 0.02574(15) 0.02605(15) 0.03053(18) 0.00202(14) -0.00066(12) -0.00023(13) Lu2 0.02854(16) 0.03554(18) 0.02964(18) 0.00219(14) -0.00003(12) -0.00106(13) _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 O1 1.454(7) . ? C1 C2 1.501(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.496(10) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.518(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O1 1.469(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 O2 1.440(8) . ? C5 C6 1.473(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.533(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.492(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O2 1.469(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O3 1.473(8) . ? C9 C10 1.490(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.526(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.483(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O3 1.450(8) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14' 1.46(2) . ? C13 O4 1.466(7) . ? C13 C14 1.61(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.06(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.68(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C14' C15' 1.44(3) . ? C14' H14C 0.9900 . ? C14' H14D 0.9900 . ? C15' C16 1.437(17) . ? C15' H15C 0.9900 . ? C15' H15D 0.9900 . ? C16 O4 1.480(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 N2 1.337(7) . ? C17 N1 1.354(7) . ? C17 C18 1.497(8) . ? C17 Lu1 2.726(6) . ? C18 C19 1.388(8) . ? C18 C23 1.418(8) . ? C19 C20 1.373(9) . ? C19 H19 0.9500 . ? C20 C21 1.368(9) . ? C20 H20 0.9500 . ? C21 C22 1.365(9) . ? C21 H21 0.9500 . ? C22 C23 1.391(9) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C32 1.389(9) . ? C24 C25 1.399(8) . ? C24 N1 1.446(8) . ? C25 C29 1.410(9) . ? C25 C26 1.513(9) . ? C26 C27 1.515(9) . ? C26 C28 1.539(9) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.366(9) . ? C29 H29 0.9500 . ? C30 C31 1.390(9) . ? C30 H30 0.9500 . ? C31 C32 1.391(9) . ? C31 H31 0.9500 . ? C32 C33 1.523(9) . ? C33 C35 1.528(9) . ? C33 C34 1.542(10) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.409(9) . ? C36 N2 1.415(7) . ? C36 C44 1.425(9) . ? C37 C41 1.409(9) . ? C37 C38 1.503(9) . ? C38 C40 1.520(9) . ? C38 C39 1.550(9) . ? C38 H38 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.386(10) . ? C41 H41 0.9500 . ? C42 C43 1.357(9) . ? C42 H42 0.9500 . ? C43 C44 1.382(9) . ? C43 H43 0.9500 . ? C44 C45 1.528(9) . ? C45 C47 1.539(8) . ? C45 C46 1.541(9) . ? C45 H45 1.0000 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C72 C77 1.388(9) . ? C72 C73 1.399(9) . ? C72 B1 1.670(10) . ? C73 C74 1.382(9) . ? C73 H73 0.9500 . ? C74 C75 1.359(11) . ? C74 H74 0.9500 . ? C75 C76 1.392(11) . ? C75 H75 0.9500 . ? C76 C77 1.391(9) . ? C76 H76 0.9500 . ? C77 H77 0.9500 . ? C78 C79 1.382(9) . ? C78 C83 1.385(9) . ? C78 B1 1.650(10) . ? C79 C80 1.398(10) . ? C79 H79 0.9500 . ? C80 C81 1.385(12) . ? C80 H80 0.9500 . ? C81 C82 1.352(11) . ? C81 H81 0.9500 . ? C82 C83 1.399(10) . ? C82 H82 0.9500 . ? C83 H83 0.9500 . ? C84 C89 1.386(9) . ? C84 C85 1.405(9) . ? C84 B1 1.632(10) . ? C85 C86 1.392(9) . ? C85 H85 0.9500 . ? C86 C87 1.374(10) . ? C86 H86 0.9500 . ? C87 C88 1.366(11) . ? C87 H87 0.9500 . ? C88 C89 1.403(9) . ? C88 H88 0.9500 . ? C89 H89 0.9500 . ? C90 C95 1.375(9) . ? C90 C91 1.392(9) . ? C90 B1 1.655(10) . ? C91 C92 1.394(10) . ? C91 H91 0.9500 . ? C92 C93 1.378(10) . ? C92 H92 0.9500 . ? C93 C94 1.360(10) . ? C93 H93 0.9500 . ? C94 C95 1.399(9) . ? C94 H94 0.9500 . ? C95 H95 0.9500 . ? C96 O5 1.473(8) . ? C96 C97 1.478(11) . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? C97 C98 1.455(12) . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? C98 C99 1.511(12) . ? C98 H98A 0.9900 . ? C98 H98B 0.9900 . ? C99 O5 1.435(8) . ? C99 H99A 0.9900 . ? C99 H99B 0.9900 . ? C100 O6 1.472(8) . ? C100 C101 1.47(4) . ? C100 C301 1.52(3) . ? C100 H10U 0.9900 . ? C100 H10V 0.9900 . ? C101 C102 1.38(3) . ? C101 H10C 0.9900 . ? C101 H10D 0.9900 . ? C102 C103 1.43(4) . ? C102 H10E 0.9900 . ? C102 H10F 0.9900 . ? C301 C302 1.30(2) . ? C301 H30A 0.9900 . ? C301 H30B 0.9900 . ? C302 C103 1.57(2) . ? C302 H30C 0.9900 . ? C302 H30D 0.9900 . ? C103 O6 1.449(8) . ? C103 H10G 0.9900 . ? C103 H10H 0.9900 . ? C104 O7 1.452(8) . ? C104 C105 1.503(10) . ? C104 H10I 0.9900 . ? C104 H10J 0.9900 . ? C105 C106 1.525(10) . ? C105 H10K 0.9900 . ? C105 H10L 0.9900 . ? C106 C107 1.510(9) . ? C106 H10M 0.9900 . ? C106 H10N 0.9900 . ? C107 O7 1.495(7) . ? C107 H10O 0.9900 . ? C107 H10P 0.9900 . ? C108 O8 1.451(8) . ? C108 C109 1.524(10) . ? C108 H10Q 0.9900 . ? C108 H10R 0.9900 . ? C109 C110 1.544(10) . ? C109 H10S 0.9900 . ? C109 H10T 0.9900 . ? C110 C111 1.494(10) . ? C110 H11U 0.9900 . ? C110 H11V 0.9900 . ? C111 O8 1.467(8) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 N3 1.338(7) . ? C112 N4 1.354(8) . ? C112 C113 1.512(9) . ? C112 Lu2 2.735(7) . ? C113 C118 1.392(9) . ? C113 C114 1.395(9) . ? C114 C115 1.391(10) . ? C114 H114 0.9500 . ? C115 C116 1.377(10) . ? C115 H115 0.9500 . ? C116 C117 1.359(11) . ? C116 H116 0.9500 . ? C117 C118 1.386(10) . ? C117 H117 0.9500 . ? C118 H118 0.9500 . ? C119 C127 1.406(9) . ? C119 C120 1.421(9) . ? C119 N3 1.437(8) . ? C120 C124 1.366(10) . ? C120 C121 1.522(10) . ? C121 C122 1.509(10) . ? C121 C123 1.532(10) . ? C121 H121 1.0000 . ? C122 H12U 0.9800 . ? C122 H12V 0.9800 . ? C122 H12C 0.9800 . ? C123 H12D 0.9800 . ? C123 H12E 0.9800 . ? C123 H12F 0.9800 . ? C124 C125 1.401(11) . ? C124 H124 0.9500 . ? C125 C126 1.371(11) . ? C125 H125 0.9500 . ? C126 C127 1.418(10) . ? C126 H126 0.9500 . ? C127 C128 1.513(9) . ? C128 C130 1.535(9) . ? C128 C129 1.537(9) . ? C128 H128 1.0000 . ? C129 H12G 0.9800 . ? C129 H12H 0.9800 . ? C129 H12I 0.9800 . ? C130 H13U 0.9800 . ? C130 H13V 0.9800 . ? C130 H13C 0.9800 . ? C131 C139 1.401(10) . ? C131 C132 1.404(10) . ? C131 N4 1.441(8) . ? C132 C136 1.388(10) . ? C132 C133 1.513(11) . ? C133 C135 1.515(12) . ? C133 C134 1.519(12) . ? C133 H133 1.0000 . ? C134 H13D 0.9800 . ? C134 H13E 0.9800 . ? C134 H13F 0.9800 . ? C135 H13G 0.9800 . ? C135 H13H 0.9800 . ? C135 H13I 0.9800 . ? C136 C137 1.352(11) . ? C136 H136 0.9500 . ? C137 C138 1.368(12) . ? C137 H137 0.9500 . ? C138 C139 1.411(10) . ? C138 H138 0.9500 . ? C139 C140 1.516(10) . ? C140 C141 1.548(10) . ? C140 C142 1.564(10) . ? C140 H140 1.0000 . ? C141 H14U 0.9800 . ? C141 H14V 0.9800 . ? C141 H14W 0.9800 . ? C142 H14X 0.9800 . ? C142 H14E 0.9800 . ? C142 H14F 0.9800 . ? C143 C144 1.400(10) . ? C143 C148 1.410(10) . ? C143 B2 1.615(11) . ? C144 C145 1.378(13) . ? C144 H144 0.9500 . ? C145 C146 1.347(15) . ? C145 H145 0.9500 . ? C146 C147 1.382(14) . ? C146 H146 0.9500 . ? C147 C148 1.395(11) . ? C147 H147 0.9500 . ? C148 H148 0.9500 . ? C149 C154 1.390(10) . ? C149 C150 1.394(11) . ? C149 H149 0.9500 . ? C150 C151 1.344(11) . ? C150 H150 0.9500 . ? C151 C152 1.352(10) . ? C151 H151 0.9500 . ? C152 C153 1.387(9) . ? C152 H152 0.9500 . ? C153 C154 1.360(9) . ? C153 H153 0.9500 . ? C154 B2 1.650(10) . ? C155 C160 1.391(9) . ? C155 C156 1.394(10) . ? C155 H155 0.9500 . ? C156 C157 1.370(10) . ? C156 H156 0.9500 . ? C157 C158 1.384(10) . ? C157 H157 0.9500 . ? C158 C159 1.383(10) . ? C158 H158 0.9500 . ? C159 C160 1.394(9) . ? C159 H159 0.9500 . ? C160 B2 1.660(11) . ? C161 C162 1.382(9) . ? C161 C166 1.410(9) . ? C161 B2 1.656(10) . ? C162 C163 1.392(9) . ? C162 H162 0.9500 . ? C163 C164 1.356(10) . ? C163 H163 0.9500 . ? C164 C165 1.384(10) . ? C164 H164 0.9500 . ? C165 C166 1.401(10) . ? C165 H165 0.9500 . ? C166 H166 0.9500 . ? C167 C172 1.394(10) . ? C167 C168 1.426(9) . ? C167 B3 1.673(11) . ? C168 C169 1.378(10) . ? C168 H168 0.9500 . ? C169 C170 1.373(11) . ? C169 H169 0.9500 . ? C170 C171 1.363(11) . ? C170 H170 0.9500 . ? C171 C172 1.418(10) . ? C171 H171 0.9500 . ? C172 H172 0.9500 . ? C173 C174 1.385(9) . ? C173 C178 1.413(9) . ? C173 B3 1.646(10) . ? C174 C175 1.376(9) . ? C174 H174 0.9500 . ? C175 C176 1.398(10) . ? C175 H175 0.9500 . ? C176 C177 1.327(10) . ? C176 H176 0.9500 . ? C177 C178 1.370(9) . ? C177 H177 0.9500 . ? C178 H178 0.9500 . ? C179 C180 1.383(10) . ? C179 C184 1.393(9) . ? C179 H179 0.9500 . ? C180 C181 1.378(11) . ? C180 H180 0.9500 . ? C181 C182 1.371(11) . ? C181 H181 0.9500 . ? C182 C183 1.396(10) . ? C182 H182 0.9500 . ? C183 C184 1.389(9) . ? C183 H183 0.9500 . ? C184 B3 1.679(11) . ? C185 C190 1.391(9) . ? C185 C186 1.408(9) . ? C185 B3 1.639(10) . ? C186 C187 1.391(9) . ? C186 H186 0.9500 . ? C187 C188 1.365(10) . ? C187 H187 0.9500 . ? C188 C189 1.368(10) . ? C188 H188 0.9500 . ? C189 C190 1.385(9) . ? C189 H189 0.9500 . ? C190 H190 0.9500 . ? C191 C196 1.377(10) . ? C191 C192 1.380(9) . ? C191 B4 1.663(10) . ? C192 C193 1.384(9) . ? C192 H192 0.9500 . ? C193 C194 1.371(11) . ? C193 H193 0.9500 . ? C194 C195 1.385(11) . ? C194 H194 0.9500 . ? C195 C196 1.411(10) . ? C195 H195 0.9500 . ? C196 H196 0.9500 . ? C197 C198 1.374(9) . ? C197 C202 1.402(9) . ? C197 B4 1.646(10) . ? C198 C199 1.401(9) . ? C198 H198 0.9500 . ? C199 C200 1.373(11) . ? C199 H199 0.9500 . ? C200 C201 1.382(11) . ? C200 H200 0.9500 . ? C201 C202 1.388(10) . ? C201 H201 0.9500 . ? C202 H202 0.9500 . ? C203 C204 1.363(10) . ? C203 C208 1.417(10) . ? C203 B4 1.653(11) . ? C204 C205 1.393(11) . ? C204 H204 0.9500 . ? C205 C206 1.360(11) . ? C205 H205 0.9500 . ? C206 C207 1.369(12) . ? C206 H206 0.9500 . ? C207 C208 1.379(12) . ? C207 H207 0.9500 . ? C208 H208 0.9500 . ? C209 C214 1.385(9) . ? C209 C210 1.398(9) . ? C209 B4 1.661(10) . ? C210 C211 1.399(10) . ? C210 H210 0.9500 . ? C211 C212 1.354(11) . ? C211 H211 0.9500 . ? C212 C213 1.366(11) . ? C212 H212 0.9500 . ? C213 C214 1.386(10) . ? C213 H213 0.9500 . ? C214 H214 0.9500 . ? N1 Lu1 2.275(5) . ? N2 Lu1 2.297(5) . ? N3 Lu2 2.284(5) . ? N4 Lu2 2.263(5) . ? O1 Lu1 2.249(4) . ? O2 Lu1 2.278(4) . ? O3 Lu1 2.291(4) . ? O4 Lu1 2.248(4) . ? O5 Lu2 2.250(4) . ? O6 Lu2 2.291(4) . ? O7 Lu2 2.248(4) . ? O8 Lu2 2.300(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 106.1(6) . . ? O1 C1 H1A 110.5 . . ? C2 C1 H1A 110.5 . . ? O1 C1 H1B 110.5 . . ? C2 C1 H1B 110.5 . . ? H1A C1 H1B 108.7 . . ? C3 C2 C1 102.8(6) . . ? C3 C2 H2A 111.2 . . ? C1 C2 H2A 111.2 . . ? C3 C2 H2B 111.2 . . ? C1 C2 H2B 111.2 . . ? H2A C2 H2B 109.1 . . ? C2 C3 C4 103.3(7) . . ? C2 C3 H3A 111.1 . . ? C4 C3 H3A 111.1 . . ? C2 C3 H3B 111.1 . . ? C4 C3 H3B 111.1 . . ? H3A C3 H3B 109.1 . . ? O1 C4 C3 104.1(6) . . ? O1 C4 H4A 110.9 . . ? C3 C4 H4A 110.9 . . ? O1 C4 H4B 110.9 . . ? C3 C4 H4B 110.9 . . ? H4A C4 H4B 109.0 . . ? O2 C5 C6 106.7(6) . . ? O2 C5 H5A 110.4 . . ? C6 C5 H5A 110.4 . . ? O2 C5 H5B 110.4 . . ? C6 C5 H5B 110.4 . . ? H5A C5 H5B 108.6 . . ? C5 C6 C7 105.7(6) . . ? C5 C6 H6A 110.6 . . ? C7 C6 H6A 110.6 . . ? C5 C6 H6B 110.6 . . ? C7 C6 H6B 110.6 . . ? H6A C6 H6B 108.7 . . ? C8 C7 C6 102.9(5) . . ? C8 C7 H7A 111.2 . . ? C6 C7 H7A 111.2 . . ? C8 C7 H7B 111.2 . . ? C6 C7 H7B 111.2 . . ? H7A C7 H7B 109.1 . . ? O2 C8 C7 106.9(5) . . ? O2 C8 H8A 110.3 . . ? C7 C8 H8A 110.3 . . ? O2 C8 H8B 110.3 . . ? C7 C8 H8B 110.3 . . ? H8A C8 H8B 108.6 . . ? O3 C9 C10 106.2(6) . . ? O3 C9 H9A 110.5 . . ? C10 C9 H9A 110.5 . . ? O3 C9 H9B 110.5 . . ? C10 C9 H9B 110.5 . . ? H9A C9 H9B 108.7 . . ? C9 C10 C11 105.6(6) . . ? C9 C10 H10A 110.6 . . ? C11 C10 H10A 110.6 . . ? C9 C10 H10B 110.6 . . ? C11 C10 H10B 110.6 . . ? H10A C10 H10B 108.7 . . ? C12 C11 C10 103.7(6) . . ? C12 C11 H11A 111.0 . . ? C10 C11 H11A 111.0 . . ? C12 C11 H11B 111.0 . . ? C10 C11 H11B 111.0 . . ? H11A C11 H11B 109.0 . . ? O3 C12 C11 105.8(6) . . ? O3 C12 H12A 110.6 . . ? C11 C12 H12A 110.6 . . ? O3 C12 H12B 110.6 . . ? C11 C12 H12B 110.6 . . ? H12A C12 H12B 108.7 . . ? C14' C13 O4 108.4(10) . . ? C14' C13 C14 23(3) . . ? O4 C13 C14 98.9(19) . . ? C14' C13 H13A 110.0 . . ? O4 C13 H13A 110.0 . . ? C14 C13 H13A 132.6 . . ? C14' C13 H13B 110.0 . . ? O4 C13 H13B 110.0 . . ? C14 C13 H13B 95.2 . . ? H13A C13 H13B 108.4 . . ? C15 C14 C13 120(4) . . ? C15 C14 H14A 107.3 . . ? C13 C14 H14A 107.3 . . ? C15 C14 H14B 107.3 . . ? C13 C14 H14B 107.3 . . ? H14A C14 H14B 106.9 . . ? C14 C15 C16 107(4) . . ? C14 C15 H15A 110.3 . . ? C16 C15 H15A 110.3 . . ? C14 C15 H15B 110.3 . . ? C16 C15 H15B 110.3 . . ? H15A C15 H15B 108.5 . . ? C15' C14' C13 105.5(14) . . ? C15' C14' H14C 110.6 . . ? C13 C14' H14C 110.6 . . ? C15' C14' H14D 110.6 . . ? C13 C14' H14D 110.6 . . ? H14C C14' H14D 108.8 . . ? C14' C15' C16 111.6(14) . . ? C14' C15' H15C 109.3 . . ? C16 C15' H15C 109.3 . . ? C14' C15' H15D 109.3 . . ? C16 C15' H15D 109.3 . . ? H15C C15' H15D 108.0 . . ? C15' C16 O4 104.9(9) . . ? C15' C16 C15 31.8(18) . . ? O4 C16 C15 100.6(15) . . ? C15' C16 H16A 110.8 . . ? O4 C16 H16A 110.8 . . ? C15 C16 H16A 83.7 . . ? C15' C16 H16B 110.8 . . ? O4 C16 H16B 110.8 . . ? C15 C16 H16B 138.2 . . ? H16A C16 H16B 108.8 . . ? N2 C17 N1 113.6(5) . . ? N2 C17 C18 122.1(5) . . ? N1 C17 C18 124.2(6) . . ? N2 C17 Lu1 57.3(3) . . ? N1 C17 Lu1 56.3(3) . . ? C18 C17 Lu1 179.4(5) . . ? C19 C18 C23 116.7(6) . . ? C19 C18 C17 121.6(6) . . ? C23 C18 C17 121.7(6) . . ? C20 C19 C18 122.5(7) . . ? C20 C19 H19 118.7 . . ? C18 C19 H19 118.7 . . ? C21 C20 C19 118.9(7) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C22 C21 C20 121.8(7) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C21 C22 C23 119.2(7) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C22 C23 C18 120.7(6) . . ? C22 C23 H23 119.7 . . ? C18 C23 H23 119.7 . . ? C32 C24 C25 122.0(6) . . ? C32 C24 N1 118.5(6) . . ? C25 C24 N1 119.5(6) . . ? C24 C25 C29 116.7(6) . . ? C24 C25 C26 125.4(6) . . ? C29 C25 C26 117.9(6) . . ? C25 C26 C27 111.9(6) . . ? C25 C26 C28 110.6(5) . . ? C27 C26 C28 111.2(6) . . ? C25 C26 H26 107.6 . . ? C27 C26 H26 107.6 . . ? C28 C26 H26 107.6 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C25 122.2(7) . . ? C30 C29 H29 118.9 . . ? C25 C29 H29 118.9 . . ? C29 C30 C31 119.3(7) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C30 C31 C32 120.9(7) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C24 C32 C31 118.5(6) . . ? C24 C32 C33 123.3(6) . . ? C31 C32 C33 118.1(6) . . ? C32 C33 C35 112.6(6) . . ? C32 C33 C34 112.0(6) . . ? C35 C33 C34 109.7(6) . . ? C32 C33 H33 107.4 . . ? C35 C33 H33 107.4 . . ? C34 C33 H33 107.4 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 N2 120.7(6) . . ? C37 C36 C44 119.9(6) . . ? N2 C36 C44 119.4(6) . . ? C41 C37 C36 118.6(7) . . ? C41 C37 C38 116.9(6) . . ? C36 C37 C38 124.5(6) . . ? C37 C38 C40 112.1(6) . . ? C37 C38 C39 111.9(6) . . ? C40 C38 C39 109.4(6) . . ? C37 C38 H38 107.7 . . ? C40 C38 H38 107.7 . . ? C39 C38 H38 107.7 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C37 120.5(7) . . ? C42 C41 H41 119.7 . . ? C37 C41 H41 119.7 . . ? C43 C42 C41 120.2(7) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 122.3(7) . . ? C42 C43 H43 118.8 . . ? C44 C43 H43 118.8 . . ? C43 C44 C36 118.4(6) . . ? C43 C44 C45 120.1(6) . . ? C36 C44 C45 121.3(6) . . ? C44 C45 C47 113.7(5) . . ? C44 C45 C46 112.8(5) . . ? C47 C45 C46 109.4(6) . . ? C44 C45 H45 106.8 . . ? C47 C45 H45 106.8 . . ? C46 C45 H45 106.8 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C77 C72 C73 114.7(6) . . ? C77 C72 B1 123.0(6) . . ? C73 C72 B1 122.1(6) . . ? C74 C73 C72 123.4(7) . . ? C74 C73 H73 118.3 . . ? C72 C73 H73 118.3 . . ? C75 C74 C73 120.8(8) . . ? C75 C74 H74 119.6 . . ? C73 C74 H74 119.6 . . ? C74 C75 C76 117.8(7) . . ? C74 C75 H75 121.1 . . ? C76 C75 H75 121.1 . . ? C77 C76 C75 121.0(7) . . ? C77 C76 H76 119.5 . . ? C75 C76 H76 119.5 . . ? C72 C77 C76 122.3(7) . . ? C72 C77 H77 118.9 . . ? C76 C77 H77 118.9 . . ? C79 C78 C83 115.4(7) . . ? C79 C78 B1 123.1(6) . . ? C83 C78 B1 121.4(6) . . ? C78 C79 C80 122.4(8) . . ? C78 C79 H79 118.8 . . ? C80 C79 H79 118.8 . . ? C81 C80 C79 119.4(8) . . ? C81 C80 H80 120.3 . . ? C79 C80 H80 120.3 . . ? C82 C81 C80 120.2(8) . . ? C82 C81 H81 119.9 . . ? C80 C81 H81 119.9 . . ? C81 C82 C83 118.9(9) . . ? C81 C82 H82 120.5 . . ? C83 C82 H82 120.5 . . ? C78 C83 C82 123.6(8) . . ? C78 C83 H83 118.2 . . ? C82 C83 H83 118.2 . . ? C89 C84 C85 113.6(6) . . ? C89 C84 B1 127.3(6) . . ? C85 C84 B1 119.2(6) . . ? C86 C85 C84 123.9(7) . . ? C86 C85 H85 118.0 . . ? C84 C85 H85 118.0 . . ? C87 C86 C85 119.9(7) . . ? C87 C86 H86 120.1 . . ? C85 C86 H86 120.1 . . ? C88 C87 C86 118.7(7) . . ? C88 C87 H87 120.7 . . ? C86 C87 H87 120.7 . . ? C87 C88 C89 120.5(8) . . ? C87 C88 H88 119.7 . . ? C89 C88 H88 119.7 . . ? C84 C89 C88 123.4(7) . . ? C84 C89 H89 118.3 . . ? C88 C89 H89 118.3 . . ? C95 C90 C91 115.5(7) . . ? C95 C90 B1 123.9(6) . . ? C91 C90 B1 120.3(6) . . ? C90 C91 C92 121.2(7) . . ? C90 C91 H91 119.4 . . ? C92 C91 H91 119.4 . . ? C93 C92 C91 120.5(7) . . ? C93 C92 H92 119.7 . . ? C91 C92 H92 119.7 . . ? C94 C93 C92 120.3(8) . . ? C94 C93 H93 119.9 . . ? C92 C93 H93 119.9 . . ? C93 C94 C95 117.8(8) . . ? C93 C94 H94 121.1 . . ? C95 C94 H94 121.1 . . ? C90 C95 C94 124.6(7) . . ? C90 C95 H95 117.7 . . ? C94 C95 H95 117.7 . . ? O5 C96 C97 105.5(7) . . ? O5 C96 H96A 110.6 . . ? C97 C96 H96A 110.6 . . ? O5 C96 H96B 110.6 . . ? C97 C96 H96B 110.6 . . ? H96A C96 H96B 108.8 . . ? C98 C97 C96 105.9(8) . . ? C98 C97 H97A 110.6 . . ? C96 C97 H97A 110.6 . . ? C98 C97 H97B 110.6 . . ? C96 C97 H97B 110.6 . . ? H97A C97 H97B 108.7 . . ? C97 C98 C99 104.1(8) . . ? C97 C98 H98A 110.9 . . ? C99 C98 H98A 110.9 . . ? C97 C98 H98B 110.9 . . ? C99 C98 H98B 110.9 . . ? H98A C98 H98B 109.0 . . ? O5 C99 C98 106.6(7) . . ? O5 C99 H99A 110.4 . . ? C98 C99 H99A 110.4 . . ? O5 C99 H99B 110.4 . . ? C98 C99 H99B 110.4 . . ? H99A C99 H99B 108.6 . . ? O6 C100 C101 100.4(17) . . ? O6 C100 C301 106.3(12) . . ? C101 C100 C301 27.8(14) . . ? O6 C100 H10U 110.5 . . ? C101 C100 H10U 135.8 . . ? C301 C100 H10U 110.5 . . ? O6 C100 H10V 110.5 . . ? C101 C100 H10V 88.2 . . ? C301 C100 H10V 110.5 . . ? H10U C100 H10V 108.7 . . ? C102 C101 C100 108(2) . . ? C102 C101 H10C 110.1 . . ? C100 C101 H10C 110.1 . . ? C102 C101 H10D 110.1 . . ? C100 C101 H10D 110.1 . . ? H10C C101 H10D 108.4 . . ? C101 C102 C103 111(3) . . ? C101 C102 H10E 109.5 . . ? C103 C102 H10E 109.5 . . ? C101 C102 H10F 109.5 . . ? C103 C102 H10F 109.5 . . ? H10E C102 H10F 108.1 . . ? C302 C301 C100 111.7(15) . . ? C302 C301 H30A 109.3 . . ? C100 C301 H30A 109.3 . . ? C302 C301 H30B 109.3 . . ? C100 C301 H30B 109.3 . . ? H30A C301 H30B 107.9 . . ? C301 C302 C103 108.0(17) . . ? C301 C302 H30C 110.1 . . ? C103 C302 H30C 110.1 . . ? C301 C302 H30D 110.1 . . ? C103 C302 H30D 110.1 . . ? H30C C302 H30D 108.4 . . ? C102 C103 O6 102(2) . . ? C102 C103 C302 24.7(17) . . ? O6 C103 C302 106.6(14) . . ? C102 C103 H10G 90.3 . . ? O6 C103 H10G 110.4 . . ? C302 C103 H10G 110.4 . . ? C102 C103 H10H 132.7 . . ? O6 C103 H10H 110.4 . . ? C302 C103 H10H 110.4 . . ? H10G C103 H10H 108.6 . . ? O7 C104 C105 108.1(6) . . ? O7 C104 H10I 110.1 . . ? C105 C104 H10I 110.1 . . ? O7 C104 H10J 110.1 . . ? C105 C104 H10J 110.1 . . ? H10I C104 H10J 108.4 . . ? C104 C105 C106 100.7(6) . . ? C104 C105 H10K 111.6 . . ? C106 C105 H10K 111.6 . . ? C104 C105 H10L 111.6 . . ? C106 C105 H10L 111.6 . . ? H10K C105 H10L 109.4 . . ? C107 C106 C105 103.6(6) . . ? C107 C106 H10M 111.0 . . ? C105 C106 H10M 111.0 . . ? C107 C106 H10N 111.0 . . ? C105 C106 H10N 111.0 . . ? H10M C106 H10N 109.0 . . ? O7 C107 C106 104.5(5) . . ? O7 C107 H10O 110.9 . . ? C106 C107 H10O 110.9 . . ? O7 C107 H10P 110.9 . . ? C106 C107 H10P 110.9 . . ? H10O C107 H10P 108.9 . . ? O8 C108 C109 105.8(6) . . ? O8 C108 H10Q 110.6 . . ? C109 C108 H10Q 110.6 . . ? O8 C108 H10R 110.6 . . ? C109 C108 H10R 110.6 . . ? H10Q C108 H10R 108.7 . . ? C108 C109 C110 104.9(6) . . ? C108 C109 H10S 110.8 . . ? C110 C109 H10S 110.8 . . ? C108 C109 H10T 110.8 . . ? C110 C109 H10T 110.8 . . ? H10S C109 H10T 108.8 . . ? C111 C110 C109 105.2(6) . . ? C111 C110 H11U 110.7 . . ? C109 C110 H11U 110.7 . . ? C111 C110 H11V 110.7 . . ? C109 C110 H11V 110.7 . . ? H11U C110 H11V 108.8 . . ? O8 C111 C110 105.4(6) . . ? O8 C111 H11C 110.7 . . ? C110 C111 H11C 110.7 . . ? O8 C111 H11D 110.7 . . ? C110 C111 H11D 110.7 . . ? H11C C111 H11D 108.8 . . ? N3 C112 N4 111.9(6) . . ? N3 C112 C113 124.2(6) . . ? N4 C112 C113 123.9(6) . . ? N3 C112 Lu2 56.4(3) . . ? N4 C112 Lu2 55.5(3) . . ? C113 C112 Lu2 179.3(5) . . ? C118 C113 C114 117.6(7) . . ? C118 C113 C112 121.4(6) . . ? C114 C113 C112 121.0(6) . . ? C115 C114 C113 121.1(7) . . ? C115 C114 H114 119.4 . . ? C113 C114 H114 119.4 . . ? C116 C115 C114 119.6(7) . . ? C116 C115 H115 120.2 . . ? C114 C115 H115 120.2 . . ? C117 C116 C115 120.2(7) . . ? C117 C116 H116 119.9 . . ? C115 C116 H116 119.9 . . ? C116 C117 C118 120.6(8) . . ? C116 C117 H117 119.7 . . ? C118 C117 H117 119.7 . . ? C117 C118 C113 120.8(7) . . ? C117 C118 H118 119.6 . . ? C113 C118 H118 119.6 . . ? C127 C119 C120 120.6(7) . . ? C127 C119 N3 122.3(6) . . ? C120 C119 N3 117.1(6) . . ? C124 C120 C119 118.6(8) . . ? C124 C120 C121 119.4(7) . . ? C119 C120 C121 121.9(7) . . ? C122 C121 C120 113.8(7) . . ? C122 C121 C123 107.3(7) . . ? C120 C121 C123 113.6(6) . . ? C122 C121 H121 107.2 . . ? C120 C121 H121 107.2 . . ? C123 C121 H121 107.2 . . ? C121 C122 H12U 109.5 . . ? C121 C122 H12V 109.5 . . ? H12U C122 H12V 109.5 . . ? C121 C122 H12C 109.5 . . ? H12U C122 H12C 109.5 . . ? H12V C122 H12C 109.5 . . ? C121 C123 H12D 109.5 . . ? C121 C123 H12E 109.5 . . ? H12D C123 H12E 109.5 . . ? C121 C123 H12F 109.5 . . ? H12D C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C120 C124 C125 122.0(8) . . ? C120 C124 H124 119.0 . . ? C125 C124 H124 119.0 . . ? C126 C125 C124 119.5(8) . . ? C126 C125 H125 120.2 . . ? C124 C125 H125 120.2 . . ? C125 C126 C127 121.0(8) . . ? C125 C126 H126 119.5 . . ? C127 C126 H126 119.5 . . ? C119 C127 C126 118.2(7) . . ? C119 C127 C128 123.7(7) . . ? C126 C127 C128 118.1(7) . . ? C127 C128 C130 112.0(6) . . ? C127 C128 C129 111.1(6) . . ? C130 C128 C129 110.1(6) . . ? C127 C128 H128 107.8 . . ? C130 C128 H128 107.8 . . ? C129 C128 H128 107.8 . . ? C128 C129 H12G 109.5 . . ? C128 C129 H12H 109.5 . . ? H12G C129 H12H 109.5 . . ? C128 C129 H12I 109.5 . . ? H12G C129 H12I 109.5 . . ? H12H C129 H12I 109.5 . . ? C128 C130 H13U 109.5 . . ? C128 C130 H13V 109.5 . . ? H13U C130 H13V 109.5 . . ? C128 C130 H13C 109.5 . . ? H13U C130 H13C 109.5 . . ? H13V C130 H13C 109.5 . . ? C139 C131 C132 121.0(7) . . ? C139 C131 N4 119.9(6) . . ? C132 C131 N4 118.8(6) . . ? C136 C132 C131 118.7(8) . . ? C136 C132 C133 119.0(8) . . ? C131 C132 C133 122.2(7) . . ? C132 C133 C135 111.8(8) . . ? C132 C133 C134 115.3(8) . . ? C135 C133 C134 106.2(7) . . ? C132 C133 H133 107.7 . . ? C135 C133 H133 107.7 . . ? C134 C133 H133 107.7 . . ? C133 C134 H13D 109.5 . . ? C133 C134 H13E 109.5 . . ? H13D C134 H13E 109.5 . . ? C133 C134 H13F 109.5 . . ? H13D C134 H13F 109.5 . . ? H13E C134 H13F 109.5 . . ? C133 C135 H13G 109.5 . . ? C133 C135 H13H 109.5 . . ? H13G C135 H13H 109.5 . . ? C133 C135 H13I 109.5 . . ? H13G C135 H13I 109.5 . . ? H13H C135 H13I 109.5 . . ? C137 C136 C132 120.6(9) . . ? C137 C136 H136 119.7 . . ? C132 C136 H136 119.7 . . ? C136 C137 C138 121.6(9) . . ? C136 C137 H137 119.2 . . ? C138 C137 H137 119.2 . . ? C137 C138 C139 120.5(8) . . ? C137 C138 H138 119.7 . . ? C139 C138 H138 119.7 . . ? C131 C139 C138 117.4(8) . . ? C131 C139 C140 122.9(7) . . ? C138 C139 C140 119.6(7) . . ? C139 C140 C141 110.6(7) . . ? C139 C140 C142 113.1(7) . . ? C141 C140 C142 109.3(6) . . ? C139 C140 H140 107.9 . . ? C141 C140 H140 107.9 . . ? C142 C140 H140 107.9 . . ? C140 C141 H14U 109.5 . . ? C140 C141 H14V 109.5 . . ? H14U C141 H14V 109.5 . . ? C140 C141 H14W 109.5 . . ? H14U C141 H14W 109.5 . . ? H14V C141 H14W 109.5 . . ? C140 C142 H14X 109.5 . . ? C140 C142 H14E 109.5 . . ? H14X C142 H14E 109.5 . . ? C140 C142 H14F 109.5 . . ? H14X C142 H14F 109.5 . . ? H14E C142 H14F 109.5 . . ? C144 C143 C148 113.8(8) . . ? C144 C143 B2 124.1(8) . . ? C148 C143 B2 122.1(7) . . ? C145 C144 C143 122.3(10) . . ? C145 C144 H144 118.9 . . ? C143 C144 H144 118.9 . . ? C146 C145 C144 123.1(11) . . ? C146 C145 H145 118.4 . . ? C144 C145 H145 118.4 . . ? C145 C146 C147 117.3(10) . . ? C145 C146 H146 121.3 . . ? C147 C146 H146 121.3 . . ? C146 C147 C148 120.5(10) . . ? C146 C147 H147 119.8 . . ? C148 C147 H147 119.8 . . ? C147 C148 C143 122.9(9) . . ? C147 C148 H148 118.5 . . ? C143 C148 H148 118.5 . . ? C154 C149 C150 123.1(8) . . ? C154 C149 H149 118.5 . . ? C150 C149 H149 118.5 . . ? C151 C150 C149 120.5(9) . . ? C151 C150 H150 119.8 . . ? C149 C150 H150 119.8 . . ? C150 C151 C152 118.4(8) . . ? C150 C151 H151 120.8 . . ? C152 C151 H151 120.8 . . ? C151 C152 C153 120.3(7) . . ? C151 C152 H152 119.9 . . ? C153 C152 H152 119.9 . . ? C154 C153 C152 124.3(7) . . ? C154 C153 H153 117.9 . . ? C152 C153 H153 117.9 . . ? C153 C154 C149 113.4(7) . . ? C153 C154 B2 124.6(7) . . ? C149 C154 B2 122.0(6) . . ? C160 C155 C156 122.6(8) . . ? C160 C155 H155 118.7 . . ? C156 C155 H155 118.7 . . ? C157 C156 C155 121.1(8) . . ? C157 C156 H156 119.5 . . ? C155 C156 H156 119.5 . . ? C156 C157 C158 118.3(8) . . ? C156 C157 H157 120.8 . . ? C158 C157 H157 120.8 . . ? C159 C158 C157 119.5(8) . . ? C159 C158 H158 120.3 . . ? C157 C158 H158 120.3 . . ? C158 C159 C160 124.3(7) . . ? C158 C159 H159 117.8 . . ? C160 C159 H159 117.8 . . ? C155 C160 C159 114.1(7) . . ? C155 C160 B2 121.8(7) . . ? C159 C160 B2 124.0(6) . . ? C162 C161 C166 114.4(6) . . ? C162 C161 B2 126.3(6) . . ? C166 C161 B2 119.2(6) . . ? C161 C162 C163 123.8(7) . . ? C161 C162 H162 118.1 . . ? C163 C162 H162 118.1 . . ? C164 C163 C162 120.3(7) . . ? C164 C163 H163 119.9 . . ? C162 C163 H163 119.9 . . ? C163 C164 C165 119.2(7) . . ? C163 C164 H164 120.4 . . ? C165 C164 H164 120.4 . . ? C164 C165 C166 119.7(7) . . ? C164 C165 H165 120.2 . . ? C166 C165 H165 120.2 . . ? C165 C166 C161 122.5(7) . . ? C165 C166 H166 118.8 . . ? C161 C166 H166 118.8 . . ? C172 C167 C168 115.0(7) . . ? C172 C167 B3 122.7(7) . . ? C168 C167 B3 122.3(7) . . ? C169 C168 C167 123.0(8) . . ? C169 C168 H168 118.5 . . ? C167 C168 H168 118.5 . . ? C170 C169 C168 119.5(9) . . ? C170 C169 H169 120.2 . . ? C168 C169 H169 120.2 . . ? C171 C170 C169 120.8(9) . . ? C171 C170 H170 119.6 . . ? C169 C170 H170 119.6 . . ? C170 C171 C172 119.5(8) . . ? C170 C171 H171 120.2 . . ? C172 C171 H171 120.2 . . ? C167 C172 C171 122.1(8) . . ? C167 C172 H172 119.0 . . ? C171 C172 H172 119.0 . . ? C174 C173 C178 113.0(7) . . ? C174 C173 B3 124.2(7) . . ? C178 C173 B3 122.3(6) . . ? C175 C174 C173 123.6(7) . . ? C175 C174 H174 118.2 . . ? C173 C174 H174 118.2 . . ? C174 C175 C176 119.8(7) . . ? C174 C175 H175 120.1 . . ? C176 C175 H175 120.1 . . ? C177 C176 C175 118.9(7) . . ? C177 C176 H176 120.5 . . ? C175 C176 H176 120.5 . . ? C176 C177 C178 120.7(7) . . ? C176 C177 H177 119.7 . . ? C178 C177 H177 119.7 . . ? C177 C178 C173 124.0(7) . . ? C177 C178 H178 118.0 . . ? C173 C178 H178 118.0 . . ? C180 C179 C184 122.2(8) . . ? C180 C179 H179 118.9 . . ? C184 C179 H179 118.9 . . ? C181 C180 C179 120.4(8) . . ? C181 C180 H180 119.8 . . ? C179 C180 H180 119.8 . . ? C182 C181 C180 118.7(8) . . ? C182 C181 H181 120.7 . . ? C180 C181 H181 120.7 . . ? C181 C182 C183 120.8(8) . . ? C181 C182 H182 119.6 . . ? C183 C182 H182 119.6 . . ? C184 C183 C182 121.4(7) . . ? C184 C183 H183 119.3 . . ? C182 C183 H183 119.3 . . ? C183 C184 C179 116.3(7) . . ? C183 C184 B3 123.0(7) . . ? C179 C184 B3 120.4(7) . . ? C190 C185 C186 114.2(7) . . ? C190 C185 B3 125.8(7) . . ? C186 C185 B3 119.9(6) . . ? C187 C186 C185 123.1(7) . . ? C187 C186 H186 118.5 . . ? C185 C186 H186 118.5 . . ? C188 C187 C186 119.7(7) . . ? C188 C187 H187 120.2 . . ? C186 C187 H187 120.2 . . ? C187 C188 C189 119.6(7) . . ? C187 C188 H188 120.2 . . ? C189 C188 H188 120.2 . . ? C188 C189 C190 120.2(7) . . ? C188 C189 H189 119.9 . . ? C190 C189 H189 119.9 . . ? C189 C190 C185 123.2(7) . . ? C189 C190 H190 118.4 . . ? C185 C190 H190 118.4 . . ? C196 C191 C192 115.2(7) . . ? C196 C191 B4 123.2(6) . . ? C192 C191 B4 121.4(7) . . ? C191 C192 C193 123.6(8) . . ? C191 C192 H192 118.2 . . ? C193 C192 H192 118.2 . . ? C194 C193 C192 119.8(8) . . ? C194 C193 H193 120.1 . . ? C192 C193 H193 120.1 . . ? C193 C194 C195 119.4(8) . . ? C193 C194 H194 120.3 . . ? C195 C194 H194 120.3 . . ? C194 C195 C196 118.6(8) . . ? C194 C195 H195 120.7 . . ? C196 C195 H195 120.7 . . ? C191 C196 C195 123.2(8) . . ? C191 C196 H196 118.4 . . ? C195 C196 H196 118.4 . . ? C198 C197 C202 115.1(7) . . ? C198 C197 B4 124.5(6) . . ? C202 C197 B4 120.4(7) . . ? C197 C198 C199 123.3(7) . . ? C197 C198 H198 118.4 . . ? C199 C198 H198 118.4 . . ? C200 C199 C198 119.9(8) . . ? C200 C199 H199 120.0 . . ? C198 C199 H199 120.0 . . ? C199 C200 C201 118.8(8) . . ? C199 C200 H200 120.6 . . ? C201 C200 H200 120.6 . . ? C200 C201 C202 120.0(8) . . ? C200 C201 H201 120.0 . . ? C202 C201 H201 120.0 . . ? C201 C202 C197 122.8(8) . . ? C201 C202 H202 118.6 . . ? C197 C202 H202 118.6 . . ? C204 C203 C208 114.0(7) . . ? C204 C203 B4 123.8(7) . . ? C208 C203 B4 122.1(7) . . ? C203 C204 C205 124.7(8) . . ? C203 C204 H204 117.6 . . ? C205 C204 H204 117.6 . . ? C206 C205 C204 118.9(9) . . ? C206 C205 H205 120.6 . . ? C204 C205 H205 120.6 . . ? C205 C206 C207 119.7(9) . . ? C205 C206 H206 120.1 . . ? C207 C206 H206 120.1 . . ? C206 C207 C208 120.2(9) . . ? C206 C207 H207 119.9 . . ? C208 C207 H207 119.9 . . ? C207 C208 C203 122.4(9) . . ? C207 C208 H208 118.8 . . ? C203 C208 H208 118.8 . . ? C214 C209 C210 114.7(7) . . ? C214 C209 B4 123.2(6) . . ? C210 C209 B4 122.1(6) . . ? C209 C210 C211 121.4(7) . . ? C209 C210 H210 119.3 . . ? C211 C210 H210 119.3 . . ? C212 C211 C210 122.6(8) . . ? C212 C211 H211 118.7 . . ? C210 C211 H211 118.7 . . ? C211 C212 C213 116.6(8) . . ? C211 C212 H212 121.7 . . ? C213 C212 H212 121.7 . . ? C212 C213 C214 121.9(8) . . ? C212 C213 H213 119.1 . . ? C214 C213 H213 119.1 . . ? C209 C214 C213 122.8(8) . . ? C209 C214 H214 118.6 . . ? C213 C214 H214 118.6 . . ? C84 B1 C78 116.0(6) . . ? C84 B1 C90 110.0(6) . . ? C78 B1 C90 103.5(5) . . ? C84 B1 C72 103.2(5) . . ? C78 B1 C72 111.9(6) . . ? C90 B1 C72 112.6(6) . . ? C143 B2 C154 108.5(6) . . ? C143 B2 C161 110.0(6) . . ? C154 B2 C161 108.1(6) . . ? C143 B2 C160 108.6(6) . . ? C154 B2 C160 112.0(6) . . ? C161 B2 C160 109.7(6) . . ? C185 B3 C173 112.1(6) . . ? C185 B3 C167 112.3(6) . . ? C173 B3 C167 108.6(6) . . ? C185 B3 C184 109.1(6) . . ? C173 B3 C184 106.7(6) . . ? C167 B3 C184 107.8(6) . . ? C197 B4 C203 112.9(6) . . ? C197 B4 C209 108.6(6) . . ? C203 B4 C209 109.3(6) . . ? C197 B4 C191 108.4(6) . . ? C203 B4 C191 108.2(6) . . ? C209 B4 C191 109.4(6) . . ? C17 N1 C24 121.7(5) . . ? C17 N1 Lu1 93.9(4) . . ? C24 N1 Lu1 144.3(4) . . ? C17 N2 C36 125.7(5) . . ? C17 N2 Lu1 93.4(4) . . ? C36 N2 Lu1 139.9(4) . . ? C112 N3 C119 122.4(6) . . ? C112 N3 Lu2 94.5(4) . . ? C119 N3 Lu2 142.4(4) . . ? C112 N4 C131 123.0(6) . . ? C112 N4 Lu2 94.9(4) . . ? C131 N4 Lu2 141.7(5) . . ? C1 O1 C4 109.0(5) . . ? C1 O1 Lu1 121.2(4) . . ? C4 O1 Lu1 129.7(4) . . ? C5 O2 C8 102.2(5) . . ? C5 O2 Lu1 130.6(4) . . ? C8 O2 Lu1 127.2(4) . . ? C12 O3 C9 109.1(5) . . ? C12 O3 Lu1 120.4(4) . . ? C9 O3 Lu1 130.5(4) . . ? C13 O4 C16 107.7(5) . . ? C13 O4 Lu1 130.9(4) . . ? C16 O4 Lu1 121.4(4) . . ? C99 O5 C96 108.4(6) . . ? C99 O5 Lu2 120.0(4) . . ? C96 O5 Lu2 131.0(4) . . ? C103 O6 C100 106.9(5) . . ? C103 O6 Lu2 128.6(4) . . ? C100 O6 Lu2 124.5(4) . . ? C104 O7 C107 107.4(5) . . ? C104 O7 Lu2 118.8(4) . . ? C107 O7 Lu2 133.8(4) . . ? C108 O8 C111 106.1(5) . . ? C108 O8 Lu2 120.5(4) . . ? C111 O8 Lu2 133.0(4) . . ? O4 Lu1 O1 141.88(16) . . ? O4 Lu1 N1 102.77(18) . . ? O1 Lu1 N1 110.00(17) . . ? O4 Lu1 O2 79.28(16) . . ? O1 Lu1 O2 83.07(16) . . ? N1 Lu1 O2 147.80(17) . . ? O4 Lu1 O3 81.75(16) . . ? O1 Lu1 O3 77.92(16) . . ? N1 Lu1 O3 92.58(17) . . ? O2 Lu1 O3 119.30(16) . . ? O4 Lu1 N2 116.60(17) . . ? O1 Lu1 N2 97.09(17) . . ? N1 Lu1 N2 59.03(17) . . ? O2 Lu1 N2 90.93(16) . . ? O3 Lu1 N2 147.98(16) . . ? O4 Lu1 C17 112.31(18) . . ? O1 Lu1 C17 105.80(17) . . ? N1 Lu1 C17 29.71(17) . . ? O2 Lu1 C17 119.43(17) . . ? O3 Lu1 C17 121.16(17) . . ? N2 Lu1 C17 29.32(17) . . ? O7 Lu2 O5 142.91(17) . . ? O7 Lu2 N4 112.88(17) . . ? O5 Lu2 N4 100.01(18) . . ? O7 Lu2 N3 100.45(17) . . ? O5 Lu2 N3 111.36(17) . . ? N4 Lu2 N3 58.74(19) . . ? O7 Lu2 O6 82.11(16) . . ? O5 Lu2 O6 78.77(17) . . ? N4 Lu2 O6 147.58(19) . . ? N3 Lu2 O6 91.15(17) . . ? O7 Lu2 O8 79.59(16) . . ? O5 Lu2 O8 83.33(17) . . ? N4 Lu2 O8 90.94(19) . . ? N3 Lu2 O8 147.49(17) . . ? O6 Lu2 O8 120.72(17) . . ? O7 Lu2 C112 109.44(18) . . ? O5 Lu2 C112 107.63(17) . . ? N4 Lu2 C112 29.56(18) . . ? N3 Lu2 C112 29.18(17) . . ? O6 Lu2 C112 119.44(18) . . ? O8 Lu2 C112 119.83(18) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.186 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.109 # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.000 329 107 ' ' 2 0.500 0.500 0.000 130 25 ' ' 3 0.017 0.743 0.227 263 74 ' ' 4 0.104 0.619 0.131 16 3 ' ' 5 0.983 0.243 0.273 263 74 ' ' 6 0.896 0.119 0.369 16 2 ' ' 7 0.500 0.500 0.500 329 106 ' ' 8 0.500 1.000 0.500 130 25 ' ' 9 0.017 0.757 0.727 263 75 ' ' 10 0.104 0.881 0.631 16 2 ' ' 11 0.983 0.257 0.773 263 74 ' ' 12 0.896 0.381 0.869 16 2 ' ' _platon_squeeze_details ; One disordered THF molecules per formual unit of [(Ph-NCN)Lu(THF)4][BPh4]2 were not modelled and the disordered density was taken into account using the SQUEEZE/PLATON procedure. (Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194?01) as implemented in PLATON (Spek, A.L. Acta Crystallogr. 1990, A46, C34; Spek, A.L. J. Appl. Cryst. 2003, 36, 7?3. PLATON - a multipurpose crystallographic tool. Utrecht University, Utrecht, The Netherlands). ; data_4-Y _database_code_depnum_ccdc_archive 'CCDC 829251' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (((Ph-NCN)YH(THF)2)(BPh4))2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C126 H152 B2 N4 O4 Y2' _chemical_formula_weight 1985.96 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' B B 0.0013 0.0007 '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' Y Y -2.7962 3.5667 '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 15.062(5) _cell_length_b 16.053(5) _cell_length_c 16.125(5) _cell_angle_alpha 115.236(5) _cell_angle_beta 106.900(5) _cell_angle_gamma 98.019(5) _cell_volume 3214.3(18) _cell_formula_units_Z 1 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 457 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 25.00 _exptl_crystal_description Fragment _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.026 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 0.945 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7333 _exptl_absorpt_correction_T_max 0.8713 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71069 _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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16980 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.1291 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11136 _reflns_number_gt 6141 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (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. SADI and EADP have been used for the following atoms: SADI C3 C4 C3' C4' EADP C3 C4 C3' C4' ; _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^)+(0.0613P)^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 11136 _refine_ls_number_parameters 627 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1090 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1415 _refine_ls_wR_factor_gt 0.1269 _refine_ls_goodness_of_fit_ref 0.875 _refine_ls_restrained_S_all 0.875 _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 C2 C 0.7904(4) 0.0825(4) 0.1509(4) 0.0798(16) Uani 1 1 d . . . H2A H 0.7883 0.1093 0.1055 0.096 Uiso 1 1 calc R A 1 H2B H 0.7746 0.0113 0.1129 0.096 Uiso 1 1 calc R A 1 C3 C 0.8861(10) 0.2169(9) 0.3047(9) 0.092(3) Uani 0.647(13) 1 d PD B 2 H3A H 0.8916 0.2849 0.3219 0.110 Uiso 0.647(13) 1 calc PR B 2 H3B H 0.9441 0.2158 0.3524 0.110 Uiso 0.647(13) 1 calc PR B 2 C4 C 0.8797(7) 0.1599(8) 0.2008(8) 0.092(3) Uani 0.647(13) 1 d PD B 2 H4A H 0.8783 0.2003 0.1685 0.110 Uiso 0.647(13) 1 calc PR B 2 H4B H 0.9358 0.1344 0.2004 0.110 Uiso 0.647(13) 1 calc PR B 2 C3' C 0.883(2) 0.2037(18) 0.3327(17) 0.092(3) Uani 0.353(13) 1 d PD B 1 H3'1 H 0.9235 0.2049 0.3939 0.110 Uiso 0.353(13) 1 calc PR B 1 H3'2 H 0.8994 0.2692 0.3406 0.110 Uiso 0.353(13) 1 calc PR B 1 C4' C 0.8915(13) 0.1300(16) 0.2418(15) 0.092(3) Uani 0.353(13) 1 d PD B 1 H4'1 H 0.9129 0.0794 0.2545 0.110 Uiso 0.353(13) 1 calc PR B 1 H4'2 H 0.9410 0.1612 0.2263 0.110 Uiso 0.353(13) 1 calc PR B 1 C5 C 0.7914(4) 0.1698(4) 0.3100(4) 0.0823(16) Uani 1 1 d . . . H5A H 0.7673 0.2250 0.3405 0.099 Uiso 1 1 calc R B 1 H5B H 0.7843 0.1296 0.3415 0.099 Uiso 1 1 calc R B 1 C6 C 0.6796(4) 0.3106(3) 0.1930(3) 0.0627(13) Uani 1 1 d . . . H6A H 0.7475 0.3170 0.1978 0.075 Uiso 1 1 calc R . . H6B H 0.6769 0.3180 0.2563 0.075 Uiso 1 1 calc R . . C7 C 0.6448(4) 0.3824(3) 0.1717(5) 0.0838(18) Uani 1 1 d . . . H7A H 0.6970 0.4450 0.2077 0.101 Uiso 1 1 calc R . . H7B H 0.5884 0.3927 0.1900 0.101 Uiso 1 1 calc R . . C8 C 0.6157(4) 0.3373(4) 0.0603(5) 0.0813(17) Uani 1 1 d . . . H8A H 0.5680 0.3640 0.0314 0.098 Uiso 1 1 calc R . . H8B H 0.6731 0.3469 0.0434 0.098 Uiso 1 1 calc R . . C9 C 0.5706(3) 0.2321(3) 0.0252(3) 0.0573(12) Uani 1 1 d . . . H9A H 0.4991 0.2165 0.0048 0.069 Uiso 1 1 calc R . . H9B H 0.5849 0.1903 -0.0322 0.069 Uiso 1 1 calc R . . C10 C 0.4950(3) 0.1215(3) 0.2813(3) 0.0359(9) Uani 1 1 d . B . C11 C 0.4672(3) 0.1407(3) 0.3666(3) 0.0437(10) Uani 1 1 d . . . C12 C 0.5074(3) 0.1077(3) 0.4316(3) 0.0535(12) Uani 1 1 d . . . H12 H 0.5518 0.0718 0.4202 0.064 Uiso 1 1 calc R . . C13 C 0.4830(4) 0.1268(3) 0.5126(4) 0.0712(15) Uani 1 1 d . . . H13 H 0.5104 0.1039 0.5566 0.085 Uiso 1 1 calc R . . C14 C 0.4185(4) 0.1793(3) 0.5299(4) 0.0677(14) Uani 1 1 d . . . H14 H 0.4021 0.1921 0.5858 0.081 Uiso 1 1 calc R . . C15 C 0.3786(3) 0.2125(3) 0.4681(3) 0.0549(12) Uani 1 1 d . . . H15 H 0.3341 0.2481 0.4805 0.066 Uiso 1 1 calc R . . C16 C 0.4030(3) 0.1944(3) 0.3862(3) 0.0474(11) Uani 1 1 d . . . H16 H 0.3758 0.2186 0.3435 0.057 Uiso 1 1 calc R . . C17 C 0.5163(3) 0.2862(3) 0.3034(3) 0.0380(10) Uani 1 1 d . . . C18 C 0.4495(3) 0.3140(3) 0.2462(3) 0.0434(10) Uani 1 1 d . . . C19 C 0.3770(3) 0.2430(3) 0.1413(3) 0.0474(11) Uani 1 1 d . . . H19 H 0.4108 0.1970 0.1095 0.057 Uiso 1 1 calc R . . C20 C 0.3456(3) 0.2889(3) 0.0763(4) 0.0659(14) Uani 1 1 d . . . H20A H 0.2993 0.2387 0.0096 0.099 Uiso 1 1 calc R . . H20B H 0.4028 0.3207 0.0714 0.099 Uiso 1 1 calc R . . H20C H 0.3144 0.3369 0.1062 0.099 Uiso 1 1 calc R . . C21 C 0.2878(3) 0.1826(3) 0.1378(4) 0.0683(14) Uani 1 1 d . . . H21A H 0.2440 0.1376 0.0683 0.103 Uiso 1 1 calc R . . H21B H 0.2539 0.2251 0.1712 0.103 Uiso 1 1 calc R . . H21C H 0.3077 0.1460 0.1717 0.103 Uiso 1 1 calc R . . C22 C 0.4508(4) 0.4108(3) 0.2906(4) 0.0572(13) Uani 1 1 d . . . H22 H 0.4051 0.4309 0.2547 0.069 Uiso 1 1 calc R . . C23 C 0.5170(4) 0.4774(3) 0.3854(4) 0.0619(13) Uani 1 1 d . . . H23 H 0.5169 0.5427 0.4143 0.074 Uiso 1 1 calc R . . C24 C 0.5835(3) 0.4489(3) 0.4382(4) 0.0578(12) Uani 1 1 d . . . H24 H 0.6299 0.4957 0.5029 0.069 Uiso 1 1 calc R . . C25 C 0.5844(3) 0.3537(3) 0.3990(3) 0.0475(11) Uani 1 1 d . . . C26 C 0.6610(3) 0.3291(3) 0.4623(3) 0.0553(12) Uani 1 1 d . . . H26 H 0.6527 0.2586 0.4231 0.066 Uiso 1 1 calc R . . C27 C 0.6501(4) 0.3478(3) 0.5586(4) 0.0733(15) Uani 1 1 d . . . H27A H 0.7001 0.3300 0.5963 0.110 Uiso 1 1 calc R . . H27B H 0.5854 0.3089 0.5435 0.110 Uiso 1 1 calc R . . H27C H 0.6575 0.4165 0.5983 0.110 Uiso 1 1 calc R . . C28 C 0.7643(4) 0.3856(3) 0.4852(4) 0.0802(16) Uani 1 1 d . . . H28A H 0.8123 0.3685 0.5258 0.120 Uiso 1 1 calc R . . H28B H 0.7735 0.4551 0.5218 0.120 Uiso 1 1 calc R . . H28C H 0.7727 0.3693 0.4227 0.120 Uiso 1 1 calc R . . C29 C 0.4738(3) -0.0517(3) 0.2257(3) 0.0417(10) Uani 1 1 d . . . C30 C 0.3757(3) -0.0960(3) 0.2009(3) 0.0458(11) Uani 1 1 d . . . C31 C 0.2945(3) -0.0547(3) 0.1723(3) 0.0553(12) Uani 1 1 d . . . H31 H 0.3254 0.0108 0.1840 0.066 Uiso 1 1 calc R . . C32 C 0.2293(4) -0.1163(4) 0.0630(4) 0.0906(18) Uani 1 1 d . . . H32A H 0.1780 -0.0878 0.0463 0.136 Uiso 1 1 calc R . . H32B H 0.1997 -0.1817 0.0489 0.136 Uiso 1 1 calc R . . H32C H 0.2680 -0.1192 0.0230 0.136 Uiso 1 1 calc R . . C33 C 0.2345(4) -0.0421(4) 0.2353(4) 0.0782(16) Uani 1 1 d . . . H33A H 0.1835 -0.0150 0.2144 0.117 Uiso 1 1 calc R . . H33B H 0.2768 0.0019 0.3055 0.117 Uiso 1 1 calc R . . H33C H 0.2044 -0.1050 0.2266 0.117 Uiso 1 1 calc R . . C34 C 0.3518(4) -0.1839(3) 0.1970(3) 0.0583(12) Uani 1 1 d . . . H34 H 0.2861 -0.2137 0.1828 0.070 Uiso 1 1 calc R . . C35 C 0.4196(4) -0.2298(3) 0.2128(4) 0.0666(14) Uani 1 1 d . . . H35 H 0.4004 -0.2914 0.2076 0.080 Uiso 1 1 calc R . . C36 C 0.5136(4) -0.1878(3) 0.2358(3) 0.0563(12) Uani 1 1 d . . . H36 H 0.5599 -0.2207 0.2461 0.068 Uiso 1 1 calc R . . C37 C 0.5448(3) -0.0970(3) 0.2449(3) 0.0449(11) Uani 1 1 d . . . C38 C 0.6516(3) -0.0522(3) 0.2749(3) 0.0501(11) Uani 1 1 d . . . H38 H 0.6600 0.0137 0.2820 0.060 Uiso 1 1 calc R . . C39 C 0.7151(4) -0.0390(4) 0.3770(4) 0.0876(17) Uani 1 1 d . . . H39A H 0.7837 -0.0096 0.3935 0.131 Uiso 1 1 calc R . . H39B H 0.7066 -0.1022 0.3737 0.131 Uiso 1 1 calc R . . H39C H 0.6951 0.0030 0.4286 0.131 Uiso 1 1 calc R . . C40 C 0.6891(4) -0.1072(3) 0.1978(4) 0.0686(14) Uani 1 1 d . . . H40A H 0.7586 -0.0749 0.2208 0.103 Uiso 1 1 calc R . . H40B H 0.6533 -0.1095 0.1351 0.103 Uiso 1 1 calc R . . H40C H 0.6801 -0.1732 0.1872 0.103 Uiso 1 1 calc R . . C41 C 0.1363(3) 0.2851(3) 0.5233(3) 0.0413(10) Uani 1 1 d . . . C42 C 0.1702(3) 0.3461(3) 0.4899(3) 0.0488(11) Uani 1 1 d . . . H42 H 0.1919 0.4139 0.5338 0.059 Uiso 1 1 calc R . . C43 C 0.1738(3) 0.3128(3) 0.3968(3) 0.0521(11) Uani 1 1 d . . . H43 H 0.1959 0.3574 0.3775 0.063 Uiso 1 1 calc R . . C44 C 0.1453(3) 0.2151(4) 0.3321(3) 0.0582(12) Uani 1 1 d . . . H44 H 0.1467 0.1916 0.2677 0.070 Uiso 1 1 calc R . . C45 C 0.1146(3) 0.1516(3) 0.3620(4) 0.0611(13) Uani 1 1 d . . . H45 H 0.0963 0.0838 0.3190 0.073 Uiso 1 1 calc R . . C46 C 0.1106(3) 0.1877(3) 0.4557(3) 0.0509(11) Uani 1 1 d . . . H46 H 0.0888 0.1425 0.4744 0.061 Uiso 1 1 calc R . . C47 C 0.0570(3) 0.2418(3) 0.6336(3) 0.0461(11) Uani 1 1 d . . . C48 C 0.0795(3) 0.1639(3) 0.6411(3) 0.0563(12) Uani 1 1 d . . . H48 H 0.1448 0.1623 0.6538 0.068 Uiso 1 1 calc R . . C49 C 0.0129(4) 0.0885(3) 0.6311(4) 0.0724(15) Uani 1 1 d . . . H49 H 0.0317 0.0355 0.6342 0.087 Uiso 1 1 calc R . . C50 C -0.0810(4) 0.0910(4) 0.6168(4) 0.0789(16) Uani 1 1 d . . . H50 H -0.1273 0.0404 0.6115 0.095 Uiso 1 1 calc R . . C51 C -0.1069(4) 0.1663(4) 0.6101(4) 0.0803(16) Uani 1 1 d . . . H51 H -0.1716 0.1688 0.6001 0.096 Uiso 1 1 calc R . . C52 C -0.0375(4) 0.2403(3) 0.6182(4) 0.0643(13) Uani 1 1 d . . . H52 H -0.0572 0.2921 0.6126 0.077 Uiso 1 1 calc R . . C53 C 0.1012(3) 0.4245(3) 0.6707(3) 0.0464(11) Uani 1 1 d . . . C54 C 0.1224(3) 0.4878(3) 0.7696(4) 0.0575(12) Uani 1 1 d . . . H54 H 0.1622 0.4763 0.8189 0.069 Uiso 1 1 calc R . . C55 C 0.0884(4) 0.5673(4) 0.8006(4) 0.0767(15) Uani 1 1 d . . . H55 H 0.1054 0.6087 0.8696 0.092 Uiso 1 1 calc R . . C56 C 0.0305(4) 0.5866(4) 0.7319(5) 0.0696(15) Uani 1 1 d . . . H56 H 0.0062 0.6403 0.7526 0.084 Uiso 1 1 calc R . . C57 C 0.0087(3) 0.5270(3) 0.6339(4) 0.0623(13) Uani 1 1 d . . . H57 H -0.0295 0.5402 0.5854 0.075 Uiso 1 1 calc R . . C58 C 0.0419(3) 0.4472(3) 0.6041(4) 0.0559(12) Uani 1 1 d . . . H58 H 0.0233 0.4057 0.5348 0.067 Uiso 1 1 calc R . . C59 C 0.2461(3) 0.3498(3) 0.7148(3) 0.0420(10) Uani 1 1 d . . . C60 C 0.2633(4) 0.3560(3) 0.8082(3) 0.0556(12) Uani 1 1 d . . . H60 H 0.2088 0.3389 0.8226 0.067 Uiso 1 1 calc R . . C61 C 0.3566(4) 0.3862(3) 0.8808(4) 0.0605(13) Uani 1 1 d . . . H61 H 0.3650 0.3899 0.9431 0.073 Uiso 1 1 calc R . . C62 C 0.4359(4) 0.4102(3) 0.8611(4) 0.0621(13) Uani 1 1 d . . . H62 H 0.4997 0.4320 0.9103 0.075 Uiso 1 1 calc R . . C63 C 0.4230(3) 0.4029(3) 0.7708(4) 0.0555(12) Uani 1 1 d . . . H63 H 0.4778 0.4178 0.7561 0.067 Uiso 1 1 calc R . . C64 C 0.3303(3) 0.3737(3) 0.7013(3) 0.0446(10) Uani 1 1 d . . . H64 H 0.3237 0.3698 0.6392 0.053 Uiso 1 1 calc R . . B1 B 0.1361(4) 0.3254(3) 0.6357(4) 0.0430(12) Uani 1 1 d . . . N1 N 0.5157(2) 0.1870(2) 0.2532(2) 0.0368(8) Uani 1 1 d . B . N2 N 0.5043(2) 0.0364(2) 0.2227(2) 0.0397(8) Uani 1 1 d . B . O1 O 0.7267(2) 0.1111(2) 0.2028(2) 0.0578(8) Uani 1 1 d . B . O2 O 0.61409(19) 0.21794(17) 0.10951(19) 0.0451(7) Uani 1 1 d . B . Y1 Y 0.56354(3) 0.08977(3) 0.13143(3) 0.03847(14) Uani 1 1 d . . . H1 H 0.557(2) -0.031(2) 0.003(2) 0.044(10) 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 C2 0.068(4) 0.109(4) 0.086(4) 0.059(4) 0.045(3) 0.028(3) C3 0.057(3) 0.124(5) 0.072(6) 0.043(4) 0.019(4) 0.000(3) C4 0.057(3) 0.124(5) 0.072(6) 0.043(4) 0.019(4) 0.000(3) C3' 0.057(3) 0.124(5) 0.072(6) 0.043(4) 0.019(4) 0.000(3) C4' 0.057(3) 0.124(5) 0.072(6) 0.043(4) 0.019(4) 0.000(3) C5 0.067(4) 0.065(3) 0.072(4) 0.020(3) 0.004(3) -0.005(3) C6 0.068(3) 0.047(3) 0.051(3) 0.013(2) 0.021(3) -0.002(3) C7 0.080(4) 0.036(3) 0.121(5) 0.019(3) 0.052(4) 0.013(3) C8 0.086(4) 0.073(4) 0.122(5) 0.074(4) 0.044(4) 0.033(3) C9 0.064(3) 0.062(3) 0.054(3) 0.032(3) 0.025(3) 0.024(3) C10 0.033(2) 0.038(2) 0.037(2) 0.018(2) 0.0127(19) 0.0163(19) C11 0.058(3) 0.038(2) 0.039(3) 0.019(2) 0.021(2) 0.020(2) C12 0.077(3) 0.053(3) 0.054(3) 0.031(2) 0.040(3) 0.041(3) C13 0.122(5) 0.067(3) 0.057(3) 0.043(3) 0.047(3) 0.052(3) C14 0.098(4) 0.067(3) 0.057(3) 0.032(3) 0.045(3) 0.038(3) C15 0.069(3) 0.059(3) 0.051(3) 0.030(3) 0.032(3) 0.032(3) C16 0.053(3) 0.046(3) 0.048(3) 0.025(2) 0.021(2) 0.022(2) C17 0.048(3) 0.033(2) 0.041(3) 0.019(2) 0.023(2) 0.019(2) C18 0.054(3) 0.038(2) 0.050(3) 0.024(2) 0.028(2) 0.023(2) C19 0.059(3) 0.049(3) 0.046(3) 0.029(2) 0.021(2) 0.029(2) C20 0.072(4) 0.084(4) 0.071(4) 0.048(3) 0.041(3) 0.047(3) C21 0.064(3) 0.069(3) 0.068(4) 0.037(3) 0.017(3) 0.019(3) C22 0.080(4) 0.056(3) 0.067(4) 0.042(3) 0.043(3) 0.041(3) C23 0.088(4) 0.035(3) 0.069(4) 0.021(3) 0.041(3) 0.029(3) C24 0.066(3) 0.038(3) 0.055(3) 0.012(2) 0.022(3) 0.014(2) C25 0.054(3) 0.042(3) 0.049(3) 0.020(2) 0.024(2) 0.021(2) C26 0.056(3) 0.043(3) 0.049(3) 0.014(2) 0.012(2) 0.015(2) C27 0.092(4) 0.066(3) 0.053(3) 0.025(3) 0.018(3) 0.036(3) C28 0.066(4) 0.059(3) 0.088(4) 0.023(3) 0.016(3) 0.018(3) C29 0.055(3) 0.036(2) 0.041(3) 0.019(2) 0.024(2) 0.021(2) C30 0.055(3) 0.040(2) 0.044(3) 0.018(2) 0.025(2) 0.015(2) C31 0.047(3) 0.053(3) 0.066(3) 0.029(3) 0.025(3) 0.014(2) C32 0.087(4) 0.113(5) 0.082(4) 0.051(4) 0.034(4) 0.049(4) C33 0.067(4) 0.076(4) 0.100(4) 0.042(3) 0.046(3) 0.025(3) C34 0.063(3) 0.049(3) 0.066(3) 0.029(3) 0.029(3) 0.012(3) C35 0.087(4) 0.046(3) 0.075(4) 0.035(3) 0.036(3) 0.016(3) C36 0.082(4) 0.048(3) 0.055(3) 0.032(2) 0.031(3) 0.031(3) C37 0.063(3) 0.034(2) 0.044(3) 0.020(2) 0.024(2) 0.022(2) C38 0.051(3) 0.047(3) 0.057(3) 0.030(2) 0.016(2) 0.024(2) C39 0.081(4) 0.119(5) 0.074(4) 0.051(4) 0.030(3) 0.049(4) C40 0.078(4) 0.063(3) 0.071(4) 0.031(3) 0.039(3) 0.026(3) C41 0.045(3) 0.033(2) 0.048(3) 0.022(2) 0.018(2) 0.0113(19) C42 0.058(3) 0.039(2) 0.048(3) 0.021(2) 0.019(2) 0.016(2) C43 0.051(3) 0.061(3) 0.056(3) 0.038(3) 0.020(2) 0.021(2) C44 0.053(3) 0.074(4) 0.046(3) 0.030(3) 0.018(2) 0.017(3) C45 0.067(3) 0.050(3) 0.059(3) 0.020(3) 0.026(3) 0.017(2) C46 0.050(3) 0.045(3) 0.057(3) 0.023(2) 0.021(2) 0.014(2) C47 0.054(3) 0.035(2) 0.045(3) 0.018(2) 0.018(2) 0.011(2) C48 0.051(3) 0.054(3) 0.067(3) 0.036(3) 0.019(2) 0.012(2) C49 0.074(4) 0.054(3) 0.090(4) 0.042(3) 0.025(3) 0.013(3) C50 0.078(4) 0.061(4) 0.091(4) 0.038(3) 0.035(3) -0.001(3) C51 0.063(4) 0.069(4) 0.109(5) 0.046(4) 0.034(3) 0.013(3) C52 0.057(3) 0.055(3) 0.083(4) 0.039(3) 0.024(3) 0.014(3) C53 0.039(3) 0.040(2) 0.055(3) 0.020(2) 0.018(2) 0.009(2) C54 0.066(3) 0.054(3) 0.060(3) 0.028(3) 0.029(3) 0.029(3) C55 0.079(4) 0.071(4) 0.064(4) 0.016(3) 0.027(3) 0.033(3) C56 0.064(4) 0.055(3) 0.092(4) 0.030(3) 0.040(3) 0.028(3) C57 0.055(3) 0.058(3) 0.084(4) 0.040(3) 0.027(3) 0.028(3) C58 0.059(3) 0.053(3) 0.057(3) 0.030(3) 0.019(3) 0.021(2) C59 0.052(3) 0.023(2) 0.047(3) 0.016(2) 0.016(2) 0.0086(19) C60 0.064(3) 0.047(3) 0.056(3) 0.031(2) 0.017(3) 0.015(2) C61 0.074(4) 0.045(3) 0.050(3) 0.022(2) 0.010(3) 0.017(3) C62 0.062(3) 0.039(3) 0.059(3) 0.019(2) -0.002(3) 0.013(2) C63 0.054(3) 0.038(3) 0.060(3) 0.020(2) 0.010(3) 0.016(2) C64 0.052(3) 0.032(2) 0.041(3) 0.014(2) 0.012(2) 0.015(2) B1 0.047(3) 0.030(3) 0.051(3) 0.020(2) 0.018(3) 0.012(2) N1 0.043(2) 0.0315(18) 0.041(2) 0.0191(16) 0.0179(16) 0.0164(15) N2 0.045(2) 0.0342(19) 0.049(2) 0.0230(17) 0.0225(17) 0.0204(16) O1 0.0426(18) 0.063(2) 0.066(2) 0.0306(18) 0.0204(17) 0.0192(16) O2 0.0558(18) 0.0327(15) 0.0375(17) 0.0144(14) 0.0129(14) 0.0085(14) Y1 0.0418(3) 0.0315(2) 0.0400(3) 0.01537(19) 0.01678(19) 0.01131(17) _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 C2 C4 1.431(10) . ? C2 O1 1.449(5) . ? C2 C4' 1.57(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.492(10) . ? C3 C5 1.561(13) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C3' C5 1.28(3) . ? C3' C4' 1.497(15) . ? C3' H3'1 0.9900 . ? C3' H3'2 0.9900 . ? C4' H4'1 0.9900 . ? C4' H4'2 0.9900 . ? C5 O1 1.484(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O2 1.452(5) . ? C6 C7 1.457(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.512(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.508(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O2 1.455(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N1 1.344(4) . ? C10 N2 1.344(4) . ? C10 C11 1.474(5) . ? C10 Y1 2.777(4) . ? C11 C12 1.393(5) . ? C11 C16 1.399(5) . ? C12 C13 1.379(6) . ? C12 H12 0.9500 . ? C13 C14 1.383(6) . ? C13 H13 0.9500 . ? C14 C15 1.354(6) . ? C14 H14 0.9500 . ? C15 C16 1.395(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C25 1.396(6) . ? C17 C18 1.414(5) . ? C17 N1 1.443(4) . ? C18 C22 1.402(5) . ? C18 C19 1.512(6) . ? C19 C21 1.515(6) . ? C19 C20 1.529(5) . ? 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 C23 1.377(6) . ? C22 H22 0.9500 . ? C23 C24 1.379(6) . ? C23 H23 0.9500 . ? C24 C25 1.386(5) . ? C24 H24 0.9500 . ? C25 C26 1.522(6) . ? C26 C27 1.513(6) . ? C26 C28 1.538(6) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.404(5) . ? C29 C37 1.410(5) . ? C29 N2 1.449(5) . ? C30 C34 1.377(5) . ? C30 C31 1.519(6) . ? C31 C32 1.512(7) . ? C31 C33 1.515(6) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.367(6) . ? C34 H34 0.9500 . ? C35 C36 1.347(6) . ? C35 H35 0.9500 . ? C36 C37 1.397(5) . ? C36 H36 0.9500 . ? C37 C38 1.505(6) . ? C38 C40 1.502(6) . ? C38 C39 1.550(6) . ? C38 H38 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C46 1.384(5) . ? C41 C42 1.407(5) . ? C41 B1 1.646(6) . ? C42 C43 1.383(5) . ? C42 H42 0.9500 . ? C43 C44 1.375(6) . ? C43 H43 0.9500 . ? C44 C45 1.379(6) . ? C44 H44 0.9500 . ? C45 C46 1.392(6) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C52 1.367(6) . ? C47 C48 1.384(5) . ? C47 B1 1.647(6) . ? C48 C49 1.378(6) . ? C48 H48 0.9500 . ? C49 C50 1.374(7) . ? C49 H49 0.9500 . ? C50 C51 1.358(7) . ? C50 H50 0.9500 . ? C51 C52 1.401(6) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.383(6) . ? C53 C58 1.396(6) . ? C53 B1 1.663(6) . ? C54 C55 1.389(6) . ? C54 H54 0.9500 . ? C55 C56 1.374(7) . ? C55 H55 0.9500 . ? C56 C57 1.358(6) . ? C56 H56 0.9500 . ? C57 C58 1.384(6) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C64 1.379(5) . ? C59 C60 1.408(5) . ? C59 B1 1.639(6) . ? C60 C61 1.396(6) . ? C60 H60 0.9500 . ? C61 C62 1.368(6) . ? C61 H61 0.9500 . ? C62 C63 1.361(6) . ? C62 H62 0.9500 . ? C63 C64 1.374(6) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? N1 Y1 2.310(3) . ? N2 Y1 2.307(3) . ? O1 Y1 2.294(3) . ? O2 Y1 2.297(3) . ? Y1 Y1 3.6419(13) 2_655 ? Y1 H1 2.11(3) . ? 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 C4 C2 O1 108.8(6) . . ? C4 C2 C4' 37.0(7) . . ? O1 C2 C4' 100.1(8) . . ? C4 C2 H2A 75.3 . . ? O1 C2 H2A 111.8 . . ? C4' C2 H2A 111.8 . . ? C4 C2 H2B 133.0 . . ? O1 C2 H2B 111.8 . . ? C4' C2 H2B 111.8 . . ? H2A C2 H2B 109.5 . . ? C4 C3 C5 107.6(8) . . ? C4 C3 H3A 110.2 . . ? C5 C3 H3A 110.2 . . ? C4 C3 H3B 110.2 . . ? C5 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? C2 C4 C3 104.9(7) . . ? C2 C4 H4A 110.8 . . ? C3 C4 H4A 110.8 . . ? C2 C4 H4B 110.8 . . ? C3 C4 H4B 110.8 . . ? H4A C4 H4B 108.8 . . ? C5 C3' C4' 99.4(15) . . ? C5 C3' H3'1 111.9 . . ? C4' C3' H3'1 111.9 . . ? C5 C3' H3'2 111.9 . . ? C4' C3' H3'2 111.9 . . ? H3'1 C3' H3'2 109.6 . . ? C3' C4' C2 110.0(14) . . ? C3' C4' H4'1 109.7 . . ? C2 C4' H4'1 109.7 . . ? C3' C4' H4'2 109.7 . . ? C2 C4' H4'2 109.7 . . ? H4'1 C4' H4'2 108.2 . . ? C3' C5 O1 117.8(10) . . ? C3' C5 C3 21.0(13) . . ? O1 C5 C3 101.2(6) . . ? C3' C5 H5A 107.9 . . ? O1 C5 H5A 107.9 . . ? C3 C5 H5A 103.8 . . ? C3' C5 H5B 107.9 . . ? O1 C5 H5B 107.9 . . ? C3 C5 H5B 127.7 . . ? H5A C5 H5B 107.2 . . ? O2 C6 C7 104.9(4) . . ? O2 C6 H6A 110.8 . . ? C7 C6 H6A 110.8 . . ? O2 C6 H6B 110.8 . . ? C7 C6 H6B 110.8 . . ? H6A C6 H6B 108.8 . . ? C6 C7 C8 102.8(4) . . ? C6 C7 H7A 111.2 . . ? C8 C7 H7A 111.2 . . ? C6 C7 H7B 111.2 . . ? C8 C7 H7B 111.2 . . ? H7A C7 H7B 109.1 . . ? C9 C8 C7 102.0(4) . . ? C9 C8 H8A 111.4 . . ? C7 C8 H8A 111.4 . . ? C9 C8 H8B 111.4 . . ? C7 C8 H8B 111.4 . . ? H8A C8 H8B 109.2 . . ? O2 C9 C8 105.9(4) . . ? O2 C9 H9A 110.5 . . ? C8 C9 H9A 110.5 . . ? O2 C9 H9B 110.5 . . ? C8 C9 H9B 110.5 . . ? H9A C9 H9B 108.7 . . ? N1 C10 N2 111.5(3) . . ? N1 C10 C11 124.4(3) . . ? N2 C10 C11 124.1(3) . . ? N1 C10 Y1 55.93(18) . . ? N2 C10 Y1 55.80(18) . . ? C11 C10 Y1 175.2(3) . . ? C12 C11 C16 118.5(4) . . ? C12 C11 C10 120.0(4) . . ? C16 C11 C10 121.5(4) . . ? C13 C12 C11 120.4(4) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 120.0(4) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.9(4) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 119.8(4) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C11 120.4(4) . . ? C15 C16 H16 119.8 . . ? C11 C16 H16 119.8 . . ? C25 C17 C18 121.2(3) . . ? C25 C17 N1 122.7(3) . . ? C18 C17 N1 115.8(3) . . ? C22 C18 C17 117.7(4) . . ? C22 C18 C19 120.0(4) . . ? C17 C18 C19 122.3(3) . . ? C18 C19 C21 113.1(4) . . ? C18 C19 C20 114.1(4) . . ? C21 C19 C20 109.6(4) . . ? C18 C19 H19 106.5 . . ? C21 C19 H19 106.5 . . ? C20 C19 H19 106.5 . . ? 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 . . ? C23 C22 C18 121.2(4) . . ? C23 C22 H22 119.4 . . ? C18 C22 H22 119.4 . . ? C22 C23 C24 119.9(4) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C23 C24 C25 121.6(4) . . ? C23 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? C24 C25 C17 118.4(4) . . ? C24 C25 C26 117.9(4) . . ? C17 C25 C26 123.6(4) . . ? C27 C26 C25 112.4(4) . . ? C27 C26 C28 109.8(4) . . ? C25 C26 C28 110.9(4) . . ? C27 C26 H26 107.9 . . ? C25 C26 H26 107.9 . . ? C28 C26 H26 107.9 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C37 120.5(4) . . ? C30 C29 N2 121.7(4) . . ? C37 C29 N2 117.5(3) . . ? C34 C30 C29 117.9(4) . . ? C34 C30 C31 118.7(4) . . ? C29 C30 C31 123.2(4) . . ? C32 C31 C33 110.3(4) . . ? C32 C31 C30 111.1(4) . . ? C33 C31 C30 112.5(4) . . ? C32 C31 H31 107.6 . . ? C33 C31 H31 107.6 . . ? C30 C31 H31 107.6 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C30 122.1(4) . . ? C35 C34 H34 119.0 . . ? C30 C34 H34 119.0 . . ? C36 C35 C34 120.0(4) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 121.7(4) . . ? C35 C36 H36 119.2 . . ? C37 C36 H36 119.2 . . ? C36 C37 C29 117.7(4) . . ? C36 C37 C38 119.0(4) . . ? C29 C37 C38 123.2(4) . . ? C40 C38 C37 112.9(4) . . ? C40 C38 C39 109.7(4) . . ? C37 C38 C39 112.4(4) . . ? C40 C38 H38 107.2 . . ? C37 C38 H38 107.2 . . ? C39 C38 H38 107.2 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C46 C41 C42 113.7(4) . . ? C46 C41 B1 123.0(4) . . ? C42 C41 B1 123.2(3) . . ? C43 C42 C41 123.7(4) . . ? C43 C42 H42 118.2 . . ? C41 C42 H42 118.2 . . ? C44 C43 C42 119.9(4) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 119.1(4) . . ? C43 C44 H44 120.5 . . ? C45 C44 H44 120.5 . . ? C44 C45 C46 119.5(4) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C41 C46 C45 124.2(4) . . ? C41 C46 H46 117.9 . . ? C45 C46 H46 117.9 . . ? C52 C47 C48 114.6(4) . . ? C52 C47 B1 122.9(4) . . ? C48 C47 B1 122.4(4) . . ? C49 C48 C47 123.9(4) . . ? C49 C48 H48 118.1 . . ? C47 C48 H48 118.1 . . ? C50 C49 C48 119.3(5) . . ? C50 C49 H49 120.4 . . ? C48 C49 H49 120.4 . . ? C51 C50 C49 119.4(5) . . ? C51 C50 H50 120.3 . . ? C49 C50 H50 120.3 . . ? C50 C51 C52 119.6(5) . . ? C50 C51 H51 120.2 . . ? C52 C51 H51 120.2 . . ? C47 C52 C51 123.3(5) . . ? C47 C52 H52 118.4 . . ? C51 C52 H52 118.4 . . ? C54 C53 C58 114.0(4) . . ? C54 C53 B1 121.9(4) . . ? C58 C53 B1 123.8(4) . . ? C53 C54 C55 123.2(5) . . ? C53 C54 H54 118.4 . . ? C55 C54 H54 118.4 . . ? C56 C55 C54 120.4(5) . . ? C56 C55 H55 119.8 . . ? C54 C55 H55 119.8 . . ? C57 C56 C55 118.4(5) . . ? C57 C56 H56 120.8 . . ? C55 C56 H56 120.8 . . ? C56 C57 C58 120.5(5) . . ? C56 C57 H57 119.8 . . ? C58 C57 H57 119.8 . . ? C57 C58 C53 123.4(5) . . ? C57 C58 H58 118.3 . . ? C53 C58 H58 118.3 . . ? C64 C59 C60 113.4(4) . . ? C64 C59 B1 124.4(4) . . ? C60 C59 B1 122.1(4) . . ? C61 C60 C59 123.1(4) . . ? C61 C60 H60 118.5 . . ? C59 C60 H60 118.5 . . ? C62 C61 C60 119.3(5) . . ? C62 C61 H61 120.4 . . ? C60 C61 H61 120.4 . . ? C63 C62 C61 119.8(5) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C62 C63 C64 119.5(5) . . ? C62 C63 H63 120.2 . . ? C64 C63 H63 120.2 . . ? C63 C64 C59 124.9(4) . . ? C63 C64 H64 117.6 . . ? C59 C64 H64 117.6 . . ? C59 B1 C41 109.2(3) . . ? C59 B1 C47 111.1(3) . . ? C41 B1 C47 108.3(3) . . ? C59 B1 C53 109.4(3) . . ? C41 B1 C53 111.3(3) . . ? C47 B1 C53 107.6(3) . . ? C10 N1 C17 125.1(3) . . ? C10 N1 Y1 95.3(2) . . ? C17 N1 Y1 139.1(2) . . ? C10 N2 C29 124.1(3) . . ? C10 N2 Y1 95.4(2) . . ? C29 N2 Y1 140.4(2) . . ? C2 O1 C5 105.6(4) . . ? C2 O1 Y1 126.5(3) . . ? C5 O1 Y1 127.3(3) . . ? C6 O2 C9 108.0(3) . . ? C6 O2 Y1 121.5(2) . . ? C9 O2 Y1 128.4(2) . . ? O1 Y1 O2 84.90(10) . . ? O1 Y1 N2 100.92(11) . . ? O2 Y1 N2 147.18(10) . . ? O1 Y1 N1 108.61(11) . . ? O2 Y1 N1 89.86(10) . . ? N2 Y1 N1 57.54(10) . . ? O1 Y1 C10 105.37(11) . . ? O2 Y1 C10 118.42(10) . . ? N2 Y1 C10 28.81(10) . . ? N1 Y1 C10 28.80(10) . . ? O1 Y1 Y1 116.96(8) . 2_655 ? O2 Y1 Y1 96.92(7) . 2_655 ? N2 Y1 Y1 108.53(8) . 2_655 ? N1 Y1 Y1 134.32(8) . 2_655 ? C10 Y1 Y1 126.75(8) . 2_655 ? O1 Y1 H1 88.3(9) . . ? O2 Y1 H1 103.6(8) . . ? N2 Y1 H1 108.8(8) . . ? N1 Y1 H1 159.5(9) . . ? C10 Y1 H1 136.5(8) . . ? Y1 Y1 H1 29.9(9) 2_655 . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.381 _refine_diff_density_min -0.301 _refine_diff_density_rms 0.063 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.010 0.000 810 202 ' ' 2 0.097 0.929 0.595 7 0 ' ' 3 0.903 0.071 0.405 7 0 ' ' _platon_squeeze_details ; Two disorder C6H5Cl molecule per formual unit of [(Ph-NCN)YH(THF)2][BPh4] were not modelled and the disordered density was taken into account using the SQUEEZE/PLATON procedure. (Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194?01) as implemented in PLATON (Spek, A.L. Acta Crystallogr. 1990, A46, C34; Spek, A.L. J. Appl. Cryst. 2003, 36, 7?3. PLATON - a multipurpose crystallographic tool. Utrecht University, Utrecht, The Netherlands). ; data_4-Lu _database_code_depnum_ccdc_archive 'CCDC 829252' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (((Ph-NCN)LuH(THF)2)(BPh4))2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C126 H152 B2 Lu2 N4 O4' _chemical_formula_weight 2158.08 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' B B 0.0013 0.0007 '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' Lu Lu -0.4720 5.8584 '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 15.0119(15) _cell_length_b 16.0338(16) _cell_length_c 16.0949(15) _cell_angle_alpha 115.524(2) _cell_angle_beta 106.633(2) _cell_angle_gamma 98.134(2) _cell_volume 3188.7(5) _cell_formula_units_Z 1 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 334 _cell_measurement_theta_min 1.48 _cell_measurement_theta_max 25.0 _exptl_crystal_description Fragment _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 1.586 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6068 _exptl_absorpt_correction_T_max 0.7969 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17464 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.1133 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11039 _reflns_number_gt 7961 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (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. EADP and SADI have been used for the following atoms: SADI C3 C4 C3' C4' EADP C3 C4 C3' C4' ; _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^)+(0.0502P)^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 11039 _refine_ls_number_parameters 624 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2 C 0.7814(6) 0.0756(6) 0.1415(6) 0.072(2) Uani 1 1 d . . . H2A H 0.7525 0.0656 0.0732 0.087 Uiso 1 1 calc R A 1 H2B H 0.7923 0.0147 0.1375 0.087 Uiso 1 1 calc R A 1 C3 C 0.876(2) 0.106(2) 0.1992(19) 0.094(4) Uani 0.388(14) 1 d PD B 2 H3A H 0.9149 0.1412 0.1779 0.112 Uiso 0.388(14) 1 calc PR B 2 H3B H 0.8987 0.0496 0.1954 0.112 Uiso 0.388(14) 1 calc PR B 2 C4 C 0.8847(18) 0.1702(18) 0.302(2) 0.094(4) Uani 0.388(14) 1 d PD B 2 H4A H 0.9197 0.1487 0.3473 0.112 Uiso 0.388(14) 1 calc PR B 2 H4B H 0.9227 0.2374 0.3254 0.112 Uiso 0.388(14) 1 calc PR B 2 C3' C 0.8773(12) 0.1613(12) 0.2054(11) 0.094(4) Uani 0.612(14) 1 d PD B 1 H3'1 H 0.9343 0.1365 0.2117 0.112 Uiso 0.612(14) 1 calc PR B 1 H3'2 H 0.8823 0.2014 0.1733 0.112 Uiso 0.612(14) 1 calc PR B 1 C4' C 0.8762(6) 0.2224(6) 0.3087(6) 0.094(4) Uani 0.612(14) 1 d PD B 1 H4'1 H 0.9339 0.2281 0.3620 0.112 Uiso 0.612(14) 1 calc PR B 1 H4'2 H 0.8748 0.2882 0.3213 0.112 Uiso 0.612(14) 1 calc PR B 1 C5 C 0.7865(6) 0.1678(6) 0.3031(6) 0.080(3) Uani 1 1 d R . . H5A H 0.7554 0.2129 0.3403 0.096 Uiso 1 1 d R . . H5B H 0.8009 0.1263 0.3330 0.096 Uiso 1 1 d R . . C6 C 0.6791(6) 0.3070(4) 0.1917(5) 0.057(2) Uani 1 1 d . . . H6A H 0.7467 0.3122 0.1952 0.069 Uiso 1 1 calc R . . H6B H 0.6769 0.3154 0.2556 0.069 Uiso 1 1 calc R . . C7 C 0.6422(6) 0.3809(5) 0.1679(7) 0.078(3) Uani 1 1 d . . . H7A H 0.5862 0.3921 0.1872 0.094 Uiso 1 1 calc R . . H7B H 0.6946 0.4435 0.2025 0.094 Uiso 1 1 calc R . . C8 C 0.6121(6) 0.3340(5) 0.0578(7) 0.070(2) Uani 1 1 d . . . H8A H 0.6693 0.3418 0.0398 0.084 Uiso 1 1 calc R . . H8B H 0.5653 0.3615 0.0291 0.084 Uiso 1 1 calc R . . C9 C 0.5638(6) 0.2270(5) 0.0215(5) 0.054(2) Uani 1 1 d . . . H9A H 0.4924 0.2130 0.0035 0.065 Uiso 1 1 calc R . . H9B H 0.5758 0.1839 -0.0376 0.065 Uiso 1 1 calc R . . C10 C 0.4943(4) 0.1195(4) 0.2775(4) 0.0345(15) Uani 1 1 d . B . C11 C 0.4660(5) 0.1395(4) 0.3637(5) 0.0409(16) Uani 1 1 d . . . C12 C 0.5054(6) 0.1058(5) 0.4276(5) 0.052(2) Uani 1 1 d . . . H12 H 0.5492 0.0690 0.4154 0.062 Uiso 1 1 calc R . . C13 C 0.4812(7) 0.1253(5) 0.5086(6) 0.068(2) Uani 1 1 d . . . H13 H 0.5089 0.1027 0.5525 0.082 Uiso 1 1 calc R . . C14 C 0.4168(6) 0.1776(6) 0.5266(6) 0.066(2) Uani 1 1 d . . . H14 H 0.4008 0.1913 0.5832 0.080 Uiso 1 1 calc R . . C15 C 0.3757(6) 0.2101(5) 0.4624(5) 0.0528(19) Uani 1 1 d . . . H15 H 0.3297 0.2444 0.4735 0.063 Uiso 1 1 calc R . . C16 C 0.4014(5) 0.1926(4) 0.3829(5) 0.0440(17) Uani 1 1 d . . . H16 H 0.3749 0.2170 0.3403 0.053 Uiso 1 1 calc R . . C17 C 0.5144(5) 0.2840(4) 0.3000(5) 0.0374(16) Uani 1 1 d . . . C18 C 0.4483(5) 0.3118(4) 0.2442(5) 0.0379(16) Uani 1 1 d . . . C19 C 0.3754(5) 0.2399(5) 0.1385(5) 0.0454(18) Uani 1 1 d . . . H19 H 0.4083 0.1930 0.1057 0.054 Uiso 1 1 calc R . . C20 C 0.3429(6) 0.2869(6) 0.0741(6) 0.061(2) Uani 1 1 d . . . H20A H 0.2967 0.2366 0.0070 0.091 Uiso 1 1 calc R . . H20B H 0.4000 0.3197 0.0695 0.091 Uiso 1 1 calc R . . H20C H 0.3113 0.3344 0.1048 0.091 Uiso 1 1 calc R . . C21 C 0.2852(6) 0.1813(5) 0.1368(6) 0.063(2) Uani 1 1 d . . . H21A H 0.2405 0.1358 0.0674 0.094 Uiso 1 1 calc R . . H21B H 0.2524 0.2253 0.1709 0.094 Uiso 1 1 calc R . . H21C H 0.3047 0.1450 0.1711 0.094 Uiso 1 1 calc R . . C22 C 0.4496(6) 0.4093(5) 0.2901(6) 0.0487(19) Uani 1 1 d . . . H22 H 0.4037 0.4296 0.2548 0.058 Uiso 1 1 calc R . . C23 C 0.5150(6) 0.4748(5) 0.3839(6) 0.054(2) Uani 1 1 d . . . H23 H 0.5137 0.5400 0.4139 0.065 Uiso 1 1 calc R . . C24 C 0.5822(5) 0.4478(5) 0.4351(5) 0.0502(19) Uani 1 1 d . . . H24 H 0.6291 0.4958 0.4995 0.060 Uiso 1 1 calc R . . C25 C 0.5852(5) 0.3531(4) 0.3974(5) 0.0429(17) Uani 1 1 d . . . C26 C 0.6605(5) 0.3269(5) 0.4579(5) 0.055(2) Uani 1 1 d . . . H26 H 0.6519 0.2562 0.4177 0.066 Uiso 1 1 calc R . . C27 C 0.6495(6) 0.3463(6) 0.5563(5) 0.073(2) Uani 1 1 d . . . H27A H 0.6989 0.3276 0.5932 0.110 Uiso 1 1 calc R . . H27B H 0.5842 0.3083 0.5413 0.110 Uiso 1 1 calc R . . H27C H 0.6583 0.4156 0.5968 0.110 Uiso 1 1 calc R . . C28 C 0.7650(5) 0.3856(5) 0.4816(6) 0.069(2) Uani 1 1 d . . . H28A H 0.8134 0.3674 0.5204 0.104 Uiso 1 1 calc R . . H28B H 0.7742 0.4552 0.5204 0.104 Uiso 1 1 calc R . . H28C H 0.7730 0.3711 0.4190 0.104 Uiso 1 1 calc R . . C29 C 0.4747(5) -0.0532(4) 0.2233(5) 0.0436(17) Uani 1 1 d . . . C30 C 0.3773(5) -0.0966(5) 0.1987(5) 0.0454(17) Uani 1 1 d . . . C31 C 0.2953(5) -0.0586(5) 0.1684(6) 0.0533(19) Uani 1 1 d . . . H31 H 0.3246 0.0057 0.1763 0.064 Uiso 1 1 calc R . . C32 C 0.2278(7) -0.1265(6) 0.0580(6) 0.079(3) Uani 1 1 d . . . H32A H 0.1752 -0.1001 0.0396 0.118 Uiso 1 1 calc R . . H32B H 0.1998 -0.1909 0.0477 0.118 Uiso 1 1 calc R . . H32C H 0.2655 -0.1319 0.0162 0.118 Uiso 1 1 calc R . . C33 C 0.2342(6) -0.0430(5) 0.2333(6) 0.067(2) Uani 1 1 d . . . H33A H 0.1819 -0.0184 0.2099 0.100 Uiso 1 1 calc R . . H33B H 0.2762 0.0042 0.3031 0.100 Uiso 1 1 calc R . . H33C H 0.2056 -0.1048 0.2280 0.100 Uiso 1 1 calc R . . C34 C 0.3519(6) -0.1859(5) 0.1964(6) 0.058(2) Uani 1 1 d . . . H34 H 0.2858 -0.2160 0.1815 0.069 Uiso 1 1 calc R . . C35 C 0.4208(7) -0.2297(5) 0.2154(6) 0.066(2) Uani 1 1 d . . . H35 H 0.4022 -0.2902 0.2128 0.079 Uiso 1 1 calc R . . C36 C 0.5158(6) -0.1874(5) 0.2380(5) 0.056(2) Uani 1 1 d . . . H36 H 0.5627 -0.2195 0.2491 0.067 Uiso 1 1 calc R . . C37 C 0.5452(5) -0.0980(4) 0.2449(5) 0.0430(17) Uani 1 1 d . . . C38 C 0.6518(5) -0.0520(5) 0.2751(5) 0.0501(19) Uani 1 1 d . . . H38 H 0.6594 0.0132 0.2801 0.060 Uiso 1 1 calc R . . C39 C 0.7151(7) -0.0356(7) 0.3772(6) 0.093(3) Uani 1 1 d . . . H39A H 0.7836 -0.0052 0.3933 0.139 Uiso 1 1 calc R . . H39B H 0.7078 -0.0981 0.3756 0.139 Uiso 1 1 calc R . . H39C H 0.6943 0.0070 0.4282 0.139 Uiso 1 1 calc R . . C40 C 0.6926(6) -0.1087(5) 0.1997(6) 0.071(2) Uani 1 1 d . . . H40A H 0.7620 -0.0747 0.2233 0.107 Uiso 1 1 calc R . . H40B H 0.6570 -0.1142 0.1352 0.107 Uiso 1 1 calc R . . H40C H 0.6851 -0.1737 0.1918 0.107 Uiso 1 1 calc R . . C41 C 0.1362(5) 0.2865(4) 0.5232(5) 0.0399(16) Uani 1 1 d . . . C42 C 0.1686(5) 0.3465(5) 0.4891(5) 0.0473(18) Uani 1 1 d . . . H42 H 0.1897 0.4147 0.5329 0.057 Uiso 1 1 calc R . . C43 C 0.1722(5) 0.3131(5) 0.3954(6) 0.0535(19) Uani 1 1 d . . . H43 H 0.1947 0.3579 0.3765 0.064 Uiso 1 1 calc R . . C44 C 0.1432(5) 0.2146(6) 0.3299(6) 0.055(2) Uani 1 1 d . . . H44 H 0.1448 0.1911 0.2653 0.066 Uiso 1 1 calc R . . C45 C 0.1119(6) 0.1511(5) 0.3590(6) 0.058(2) Uani 1 1 d . . . H45 H 0.0927 0.0831 0.3151 0.069 Uiso 1 1 calc R . . C46 C 0.1084(5) 0.1870(5) 0.4532(5) 0.0463(18) Uani 1 1 d . . . H46 H 0.0860 0.1415 0.4715 0.056 Uiso 1 1 calc R . . C47 C 0.0569(5) 0.2434(4) 0.6339(5) 0.0453(17) Uani 1 1 d . . . C48 C 0.0796(6) 0.1623(5) 0.6393(6) 0.060(2) Uani 1 1 d . . . H48 H 0.1439 0.1583 0.6486 0.072 Uiso 1 1 calc R . . C49 C 0.0101(7) 0.0886(5) 0.6313(6) 0.066(2) Uani 1 1 d . . . H49 H 0.0287 0.0360 0.6358 0.079 Uiso 1 1 calc R . . C50 C -0.0821(7) 0.0897(6) 0.6173(6) 0.072(2) Uani 1 1 d . . . H50 H -0.1288 0.0384 0.6110 0.086 Uiso 1 1 calc R . . C51 C -0.1070(6) 0.1667(6) 0.6124(6) 0.076(3) Uani 1 1 d . . . H51 H -0.1715 0.1697 0.6043 0.091 Uiso 1 1 calc R . . C52 C -0.0399(6) 0.2404(5) 0.6189(6) 0.060(2) Uani 1 1 d . . . H52 H -0.0609 0.2915 0.6129 0.072 Uiso 1 1 calc R . . C53 C 0.1010(5) 0.4265(4) 0.6715(5) 0.0408(16) Uani 1 1 d . . . C54 C 0.1225(5) 0.4906(5) 0.7697(6) 0.0547(19) Uani 1 1 d . . . H54 H 0.1624 0.4793 0.8190 0.066 Uiso 1 1 calc R . . C55 C 0.0900(6) 0.5701(6) 0.8013(6) 0.070(2) Uani 1 1 d . . . H55 H 0.1078 0.6120 0.8708 0.084 Uiso 1 1 calc R . . C56 C 0.0315(6) 0.5894(5) 0.7326(7) 0.062(2) Uani 1 1 d . . . H56 H 0.0086 0.6443 0.7540 0.075 Uiso 1 1 calc R . . C57 C 0.0071(6) 0.5283(5) 0.6332(6) 0.062(2) Uani 1 1 d . . . H57 H -0.0325 0.5406 0.5847 0.075 Uiso 1 1 calc R . . C58 C 0.0412(5) 0.4466(5) 0.6032(6) 0.0526(19) Uani 1 1 d . . . H58 H 0.0226 0.4037 0.5339 0.063 Uiso 1 1 calc R . . C59 C 0.2460(5) 0.3507(4) 0.7146(5) 0.0362(16) Uani 1 1 d . . . C60 C 0.2629(6) 0.3568(4) 0.8079(6) 0.0519(19) Uani 1 1 d . . . H60 H 0.2086 0.3398 0.8229 0.062 Uiso 1 1 calc R . . C61 C 0.3557(6) 0.3867(5) 0.8781(6) 0.056(2) Uani 1 1 d . . . H61 H 0.3636 0.3901 0.9403 0.068 Uiso 1 1 calc R . . C62 C 0.4368(6) 0.4115(5) 0.8612(6) 0.055(2) Uani 1 1 d . . . H62 H 0.5005 0.4334 0.9110 0.066 Uiso 1 1 calc R . . C63 C 0.4234(5) 0.4037(4) 0.7693(6) 0.0468(18) Uani 1 1 d . . . H63 H 0.4783 0.4188 0.7544 0.056 Uiso 1 1 calc R . . C64 C 0.3299(5) 0.3740(4) 0.6988(5) 0.0415(17) Uani 1 1 d . . . H64 H 0.3229 0.3693 0.6362 0.050 Uiso 1 1 calc R . . B1 B 0.1348(6) 0.3248(5) 0.6351(6) 0.0400(19) Uani 1 1 d . . . N1 N 0.5165(4) 0.1855(3) 0.2499(4) 0.0357(12) Uani 1 1 d . B . N2 N 0.5051(4) 0.0343(3) 0.2195(4) 0.0403(13) Uani 1 1 d . B . O1 O 0.7199(3) 0.1082(3) 0.1971(4) 0.0526(13) Uani 1 1 d . B . O2 O 0.6099(3) 0.2136(3) 0.1065(3) 0.0426(11) Uani 1 1 d . B . Lu1 Lu 0.56016(2) 0.087593(19) 0.12784(2) 0.03385(10) Uani 1 1 d . . . H1 H 0.441(3) 0.035(3) 0.001(3) 0.025(14) 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 C2 0.060(6) 0.095(7) 0.074(6) 0.050(5) 0.025(5) 0.032(5) C3 0.056(5) 0.059(8) 0.099(7) -0.002(8) 0.014(6) 0.002(7) C4 0.056(5) 0.059(8) 0.099(7) -0.002(8) 0.014(6) 0.002(7) C3' 0.056(5) 0.059(8) 0.099(7) -0.002(8) 0.014(6) 0.002(7) C4' 0.056(5) 0.059(8) 0.099(7) -0.002(8) 0.014(6) 0.002(7) C5 0.068(6) 0.063(5) 0.061(6) 0.007(5) 0.005(5) 0.007(5) C6 0.059(5) 0.031(4) 0.051(5) 0.004(4) 0.013(4) -0.006(4) C7 0.071(6) 0.036(4) 0.123(9) 0.026(5) 0.058(6) 0.009(4) C8 0.080(6) 0.058(5) 0.110(8) 0.065(6) 0.046(6) 0.034(5) C9 0.065(5) 0.050(4) 0.059(5) 0.033(4) 0.026(4) 0.020(4) C10 0.033(4) 0.036(3) 0.028(4) 0.010(3) 0.010(3) 0.017(3) C11 0.057(5) 0.034(3) 0.042(4) 0.022(3) 0.025(4) 0.022(3) C12 0.084(6) 0.039(4) 0.047(5) 0.022(4) 0.035(4) 0.036(4) C13 0.115(7) 0.071(5) 0.053(5) 0.045(5) 0.044(5) 0.055(6) C14 0.097(7) 0.082(6) 0.049(5) 0.040(5) 0.044(5) 0.048(5) C15 0.070(5) 0.052(4) 0.039(5) 0.018(4) 0.024(4) 0.033(4) C16 0.055(5) 0.043(4) 0.035(4) 0.017(3) 0.018(4) 0.024(4) C17 0.051(4) 0.025(3) 0.039(4) 0.013(3) 0.021(4) 0.017(3) C18 0.048(4) 0.036(3) 0.040(4) 0.022(3) 0.023(4) 0.019(3) C19 0.057(5) 0.047(4) 0.046(5) 0.028(4) 0.023(4) 0.031(4) C20 0.068(5) 0.075(5) 0.065(5) 0.047(5) 0.031(5) 0.038(5) C21 0.065(6) 0.070(5) 0.054(5) 0.036(4) 0.016(5) 0.021(5) C22 0.063(5) 0.044(4) 0.061(5) 0.036(4) 0.032(5) 0.031(4) C23 0.073(6) 0.032(4) 0.062(6) 0.020(4) 0.034(5) 0.026(4) C24 0.059(5) 0.031(4) 0.052(5) 0.013(4) 0.022(4) 0.015(4) C25 0.049(4) 0.034(4) 0.043(4) 0.016(3) 0.019(4) 0.015(3) C26 0.059(5) 0.034(4) 0.040(5) 0.005(4) 0.002(4) 0.010(4) C27 0.090(7) 0.061(5) 0.048(5) 0.017(4) 0.010(5) 0.035(5) C28 0.048(5) 0.054(5) 0.066(6) 0.011(4) -0.001(4) 0.014(4) C29 0.069(5) 0.039(4) 0.034(4) 0.022(3) 0.026(4) 0.020(4) C30 0.051(5) 0.041(4) 0.055(5) 0.027(4) 0.028(4) 0.023(4) C31 0.045(5) 0.045(4) 0.066(6) 0.028(4) 0.020(4) 0.009(4) C32 0.090(7) 0.091(7) 0.077(7) 0.053(6) 0.035(6) 0.047(6) C33 0.064(5) 0.050(4) 0.084(6) 0.024(4) 0.039(5) 0.018(4) C34 0.064(5) 0.052(4) 0.076(6) 0.042(4) 0.035(5) 0.017(4) C35 0.100(7) 0.046(4) 0.070(6) 0.038(4) 0.041(6) 0.025(5) C36 0.087(6) 0.041(4) 0.064(5) 0.039(4) 0.037(5) 0.033(4) C37 0.062(5) 0.033(4) 0.030(4) 0.012(3) 0.018(4) 0.017(4) C38 0.066(5) 0.038(4) 0.044(5) 0.020(4) 0.012(4) 0.029(4) C39 0.080(7) 0.120(8) 0.062(6) 0.029(6) 0.024(6) 0.049(6) C40 0.081(6) 0.065(5) 0.080(6) 0.035(5) 0.043(5) 0.031(5) C41 0.032(4) 0.035(4) 0.046(4) 0.019(3) 0.010(3) 0.007(3) C42 0.048(5) 0.041(4) 0.047(5) 0.021(4) 0.013(4) 0.010(4) C43 0.051(5) 0.053(5) 0.060(5) 0.032(4) 0.020(4) 0.015(4) C44 0.045(5) 0.074(6) 0.049(5) 0.030(5) 0.020(4) 0.022(4) C45 0.065(5) 0.043(4) 0.056(5) 0.012(4) 0.029(5) 0.021(4) C46 0.044(4) 0.042(4) 0.050(5) 0.022(4) 0.017(4) 0.011(3) C47 0.049(5) 0.035(4) 0.032(4) 0.010(3) 0.004(4) 0.004(3) C48 0.057(5) 0.041(4) 0.077(6) 0.027(4) 0.024(5) 0.011(4) C49 0.074(6) 0.047(4) 0.078(6) 0.042(5) 0.024(5) 0.002(4) C50 0.076(7) 0.053(5) 0.095(7) 0.047(5) 0.037(6) 0.003(5) C51 0.049(5) 0.069(6) 0.096(7) 0.035(5) 0.030(5) 0.001(5) C52 0.060(5) 0.048(4) 0.077(6) 0.035(4) 0.026(5) 0.019(4) C53 0.040(4) 0.033(4) 0.050(5) 0.021(4) 0.018(4) 0.009(3) C54 0.057(5) 0.055(5) 0.059(5) 0.032(4) 0.023(4) 0.023(4) C55 0.079(6) 0.056(5) 0.066(6) 0.017(5) 0.032(5) 0.035(5) C56 0.064(6) 0.035(4) 0.081(7) 0.021(5) 0.029(5) 0.020(4) C57 0.067(6) 0.055(5) 0.078(6) 0.042(5) 0.026(5) 0.030(4) C58 0.057(5) 0.047(4) 0.054(5) 0.025(4) 0.021(4) 0.019(4) C59 0.046(4) 0.023(3) 0.042(4) 0.020(3) 0.013(4) 0.013(3) C60 0.063(5) 0.032(4) 0.055(5) 0.022(4) 0.015(5) 0.012(4) C61 0.070(6) 0.042(4) 0.056(5) 0.032(4) 0.010(5) 0.016(4) C62 0.050(5) 0.033(4) 0.052(5) 0.013(4) -0.007(4) 0.013(3) C63 0.043(5) 0.031(4) 0.059(5) 0.021(4) 0.011(4) 0.013(3) C64 0.050(5) 0.023(3) 0.041(4) 0.013(3) 0.009(4) 0.012(3) B1 0.051(5) 0.020(3) 0.043(5) 0.013(4) 0.015(4) 0.009(4) N1 0.045(3) 0.025(3) 0.038(3) 0.016(3) 0.016(3) 0.012(2) N2 0.056(4) 0.032(3) 0.040(3) 0.018(3) 0.022(3) 0.024(3) O1 0.046(3) 0.044(3) 0.059(3) 0.019(3) 0.020(3) 0.014(2) O2 0.059(3) 0.027(2) 0.041(3) 0.019(2) 0.018(3) 0.008(2) Lu1 0.03943(18) 0.02517(14) 0.03486(18) 0.01310(12) 0.01414(13) 0.01080(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C2 C3 1.33(3) . ? C2 O1 1.460(8) . ? C2 C3' 1.547(17) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.477(18) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.48(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C3' C4' 1.530(13) . ? C3' H3'1 0.9900 . ? C3' H3'2 0.9900 . ? C4' C5 1.4550 . ? C4' H4'1 0.9900 . ? C4' H4'2 0.9900 . ? C5 O1 1.474(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O2 1.475(7) . ? C6 C7 1.520(10) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.486(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.533(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O2 1.466(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N2 1.347(7) . ? C10 N1 1.348(7) . ? C10 C11 1.483(8) . ? C10 Lu1 2.736(6) . ? C11 C12 1.386(9) . ? C11 C16 1.394(8) . ? C12 C13 1.370(9) . ? C12 H12 0.9500 . ? C13 C14 1.379(10) . ? C13 H13 0.9500 . ? C14 C15 1.382(9) . ? C14 H14 0.9500 . ? C15 C16 1.367(8) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.396(9) . ? C17 C25 1.424(9) . ? C17 N1 1.441(7) . ? C18 C22 1.407(8) . ? C18 C19 1.519(9) . ? C19 C21 1.521(9) . ? C19 C20 1.540(9) . ? 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 C23 1.356(9) . ? C22 H22 0.9500 . ? C23 C24 1.357(10) . ? C23 H23 0.9500 . ? C24 C25 1.385(8) . ? C24 H24 0.9500 . ? C25 C26 1.503(9) . ? C26 C27 1.540(10) . ? C26 C28 1.555(10) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.387(9) . ? C29 C37 1.406(9) . ? C29 N2 1.445(7) . ? C30 C34 1.409(9) . ? C30 C31 1.500(9) . ? C31 C32 1.537(10) . ? C31 C33 1.543(9) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.366(10) . ? C34 H34 0.9500 . ? C35 C36 1.358(10) . ? C35 H35 0.9500 . ? C36 C37 1.384(9) . ? C36 H36 0.9500 . ? C37 C38 1.501(10) . ? C38 C40 1.518(9) . ? C38 C39 1.528(10) . ? C38 H38 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.392(8) . ? C41 C46 1.408(8) . ? C41 B1 1.642(10) . ? C42 C43 1.387(9) . ? C42 H42 0.9500 . ? C43 C44 1.379(9) . ? C43 H43 0.9500 . ? C44 C45 1.371(9) . ? C44 H44 0.9500 . ? C45 C46 1.391(9) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C52 1.393(9) . ? C47 C48 1.420(9) . ? C47 B1 1.615(9) . ? C48 C49 1.394(9) . ? C48 H48 0.9500 . ? C49 C50 1.342(11) . ? C49 H49 0.9500 . ? C50 C51 1.367(11) . ? C50 H50 0.9500 . ? C51 C52 1.385(10) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.368(9) . ? C53 C58 1.392(9) . ? C53 B1 1.685(9) . ? C54 C55 1.372(9) . ? C54 H54 0.9500 . ? C55 C56 1.382(11) . ? C55 H55 0.9500 . ? C56 C57 1.365(10) . ? C56 H56 0.9500 . ? C57 C58 1.414(9) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C64 1.387(9) . ? C59 C60 1.407(9) . ? C59 B1 1.648(10) . ? C60 C61 1.375(10) . ? C60 H60 0.9500 . ? C61 C62 1.365(10) . ? C61 H61 0.9500 . ? C62 C63 1.381(9) . ? C62 H62 0.9500 . ? C63 C64 1.384(9) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? N1 Lu1 2.263(5) . ? N2 Lu1 2.275(5) . ? O1 Lu1 2.243(5) . ? O2 Lu1 2.254(4) . ? Lu1 Lu1 3.5263(6) 2_655 ? Lu1 H1 2.01(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 C3 C2 O1 113.7(12) . . ? C3 C2 C3' 33.3(14) . . ? O1 C2 C3' 102.2(8) . . ? C3 C2 H2A 127.4 . . ? O1 C2 H2A 111.3 . . ? C3' C2 H2A 111.3 . . ? C3 C2 H2B 78.1 . . ? O1 C2 H2B 111.3 . . ? C3' C2 H2B 111.3 . . ? H2A C2 H2B 109.2 . . ? C2 C3 C4 106.1(19) . . ? C2 C3 H3A 110.5 . . ? C4 C3 H3A 110.5 . . ? C2 C3 H3B 110.5 . . ? C4 C3 H3B 110.5 . . ? H3A C3 H3B 108.7 . . ? C5 C4 C3 109.5(19) . . ? C5 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? C5 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? C4' C3' C2 108.1(10) . . ? C4' C3' H3'1 110.1 . . ? C2 C3' H3'1 110.1 . . ? C4' C3' H3'2 110.1 . . ? C2 C3' H3'2 110.1 . . ? H3'1 C3' H3'2 108.4 . . ? C5 C4' C3' 103.1(6) . . ? C5 C4' H4'1 111.1 . . ? C3' C4' H4'1 111.1 . . ? C5 C4' H4'2 111.1 . . ? C3' C4' H4'2 111.1 . . ? H4'1 C4' H4'2 109.1 . . ? C4' C5 O1 108.1(4) . . ? C4' C5 C4 32.8(11) . . ? O1 C5 C4 104.3(12) . . ? C4' C5 H5A 110.1 . . ? O1 C5 H5A 109.5 . . ? C4 C5 H5A 137.6 . . ? C4' C5 H5B 110.1 . . ? O1 C5 H5B 110.6 . . ? C4 C5 H5B 81.9 . . ? H5A C5 H5B 108.4 . . ? O2 C6 C7 102.8(6) . . ? O2 C6 H6A 111.2 . . ? C7 C6 H6A 111.2 . . ? O2 C6 H6B 111.2 . . ? C7 C6 H6B 111.2 . . ? H6A C6 H6B 109.1 . . ? C8 C7 C6 102.9(6) . . ? C8 C7 H7A 111.2 . . ? C6 C7 H7A 111.2 . . ? C8 C7 H7B 111.2 . . ? C6 C7 H7B 111.2 . . ? H7A C7 H7B 109.1 . . ? C7 C8 C9 103.3(6) . . ? C7 C8 H8A 111.1 . . ? C9 C8 H8A 111.1 . . ? C7 C8 H8B 111.1 . . ? C9 C8 H8B 111.1 . . ? H8A C8 H8B 109.1 . . ? O2 C9 C8 104.6(6) . . ? O2 C9 H9A 110.8 . . ? C8 C9 H9A 110.8 . . ? O2 C9 H9B 110.8 . . ? C8 C9 H9B 110.8 . . ? H9A C9 H9B 108.9 . . ? N2 C10 N1 111.4(5) . . ? N2 C10 C11 124.1(6) . . ? N1 C10 C11 124.4(5) . . ? N2 C10 Lu1 56.0(3) . . ? N1 C10 Lu1 55.5(3) . . ? C11 C10 Lu1 175.9(4) . . ? C12 C11 C16 118.8(6) . . ? C12 C11 C10 119.7(6) . . ? C16 C11 C10 121.5(6) . . ? C13 C12 C11 120.2(6) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 120.5(7) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C13 C14 C15 119.9(7) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 119.7(7) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C11 120.9(6) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? C18 C17 C25 121.3(5) . . ? C18 C17 N1 116.9(6) . . ? C25 C17 N1 121.2(6) . . ? C17 C18 C22 117.6(6) . . ? C17 C18 C19 122.0(5) . . ? C22 C18 C19 120.4(6) . . ? C18 C19 C21 112.3(5) . . ? C18 C19 C20 113.7(6) . . ? C21 C19 C20 108.9(6) . . ? C18 C19 H19 107.2 . . ? C21 C19 H19 107.2 . . ? C20 C19 H19 107.2 . . ? 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 . . ? C23 C22 C18 121.2(6) . . ? C23 C22 H22 119.4 . . ? C18 C22 H22 119.4 . . ? C22 C23 C24 120.4(6) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C25 122.6(7) . . ? C23 C24 H24 118.7 . . ? C25 C24 H24 118.7 . . ? C24 C25 C17 116.6(6) . . ? C24 C25 C26 120.4(6) . . ? C17 C25 C26 123.0(5) . . ? C25 C26 C27 111.6(6) . . ? C25 C26 C28 110.2(6) . . ? C27 C26 C28 109.4(6) . . ? C25 C26 H26 108.5 . . ? C27 C26 H26 108.5 . . ? C28 C26 H26 108.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C37 120.2(6) . . ? C30 C29 N2 121.2(6) . . ? C37 C29 N2 118.4(6) . . ? C29 C30 C34 118.2(6) . . ? C29 C30 C31 124.8(6) . . ? C34 C30 C31 116.9(6) . . ? C30 C31 C32 110.8(6) . . ? C30 C31 C33 113.3(6) . . ? C32 C31 C33 109.4(6) . . ? C30 C31 H31 107.7 . . ? C32 C31 H31 107.7 . . ? C33 C31 H31 107.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C30 121.0(7) . . ? C35 C34 H34 119.5 . . ? C30 C34 H34 119.5 . . ? C36 C35 C34 120.5(7) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C37 120.8(7) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C36 C37 C29 119.3(7) . . ? C36 C37 C38 118.7(6) . . ? C29 C37 C38 122.0(6) . . ? C37 C38 C40 113.5(6) . . ? C37 C38 C39 112.9(6) . . ? C40 C38 C39 108.4(6) . . ? C37 C38 H38 107.3 . . ? C40 C38 H38 107.3 . . ? C39 C38 H38 107.3 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C46 113.2(6) . . ? C42 C41 B1 124.7(6) . . ? C46 C41 B1 122.0(6) . . ? C43 C42 C41 124.2(6) . . ? C43 C42 H42 117.9 . . ? C41 C42 H42 117.9 . . ? C44 C43 C42 119.8(7) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C45 C44 C43 119.2(7) . . ? C45 C44 H44 120.4 . . ? C43 C44 H44 120.4 . . ? C44 C45 C46 119.6(7) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C45 C46 C41 124.0(6) . . ? C45 C46 H46 118.0 . . ? C41 C46 H46 118.0 . . ? C52 C47 C48 113.6(6) . . ? C52 C47 B1 124.2(6) . . ? C48 C47 B1 121.9(6) . . ? C49 C48 C47 121.8(7) . . ? C49 C48 H48 119.1 . . ? C47 C48 H48 119.1 . . ? C50 C49 C48 122.0(7) . . ? C50 C49 H49 119.0 . . ? C48 C49 H49 119.0 . . ? C49 C50 C51 118.1(7) . . ? C49 C50 H50 121.0 . . ? C51 C50 H50 121.0 . . ? C50 C51 C52 121.2(8) . . ? C50 C51 H51 119.4 . . ? C52 C51 H51 119.4 . . ? C51 C52 C47 123.2(7) . . ? C51 C52 H52 118.4 . . ? C47 C52 H52 118.4 . . ? C54 C53 C58 115.0(6) . . ? C54 C53 B1 122.6(6) . . ? C58 C53 B1 122.1(6) . . ? C53 C54 C55 124.0(7) . . ? C53 C54 H54 118.0 . . ? C55 C54 H54 118.0 . . ? C54 C55 C56 120.2(8) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C57 C56 C55 118.8(7) . . ? C57 C56 H56 120.6 . . ? C55 C56 H56 120.6 . . ? C56 C57 C58 119.4(7) . . ? C56 C57 H57 120.3 . . ? C58 C57 H57 120.3 . . ? C53 C58 C57 122.5(7) . . ? C53 C58 H58 118.8 . . ? C57 C58 H58 118.8 . . ? C64 C59 C60 114.5(6) . . ? C64 C59 B1 123.8(6) . . ? C60 C59 B1 121.6(6) . . ? C61 C60 C59 121.9(7) . . ? C61 C60 H60 119.0 . . ? C59 C60 H60 119.0 . . ? C62 C61 C60 122.0(7) . . ? C62 C61 H61 119.0 . . ? C60 C61 H61 119.0 . . ? C61 C62 C63 117.8(7) . . ? C61 C62 H62 121.1 . . ? C63 C62 H62 121.1 . . ? C62 C63 C64 120.1(7) . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C63 C64 C59 123.6(7) . . ? C63 C64 H64 118.2 . . ? C59 C64 H64 118.2 . . ? C47 B1 C41 110.0(5) . . ? C47 B1 C59 111.7(5) . . ? C41 B1 C59 108.7(5) . . ? C47 B1 C53 107.8(5) . . ? C41 B1 C53 110.3(5) . . ? C59 B1 C53 108.3(5) . . ? C10 N1 C17 123.9(5) . . ? C10 N1 Lu1 95.1(3) . . ? C17 N1 Lu1 140.8(4) . . ? C10 N2 C29 123.6(5) . . ? C10 N2 Lu1 94.6(4) . . ? C29 N2 Lu1 141.3(4) . . ? C2 O1 C5 106.1(5) . . ? C2 O1 Lu1 125.0(4) . . ? C5 O1 Lu1 128.3(4) . . ? C9 O2 C6 109.6(5) . . ? C9 O2 Lu1 127.5(4) . . ? C6 O2 Lu1 121.0(4) . . ? O1 Lu1 O2 85.13(16) . . ? O1 Lu1 N1 107.64(18) . . ? O2 Lu1 N1 89.25(15) . . ? O1 Lu1 N2 99.48(18) . . ? O2 Lu1 N2 147.69(16) . . ? N1 Lu1 N2 58.77(16) . . ? O1 Lu1 C10 104.85(18) . . ? O2 Lu1 C10 118.45(16) . . ? N1 Lu1 C10 29.39(16) . . ? N2 Lu1 C10 29.39(16) . . ? O1 Lu1 Lu1 116.04(12) . 2_655 ? O2 Lu1 Lu1 96.70(11) . 2_655 ? N1 Lu1 Lu1 136.24(13) . 2_655 ? N2 Lu1 Lu1 109.41(13) . 2_655 ? C10 Lu1 Lu1 127.87(13) . 2_655 ? O1 Lu1 H1 147.1(13) . . ? O2 Lu1 H1 87.8(13) . . ? N1 Lu1 H1 104.3(13) . . ? N2 Lu1 H1 103.5(13) . . ? C10 Lu1 H1 106.7(13) . . ? Lu1 Lu1 H1 33.3(13) 2_655 . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.368 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.115 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.011 0.000 797 217 ' ' 2 0.097 0.928 0.601 8 1 ' ' 3 0.903 0.072 0.399 8 1 ' ' _platon_squeeze_details ; Two disorder C6H5Cl molecule per formual unit of [(Ph-NCN)LuH(THF)2][BPh4] were not modelled and the disordered density was taken into account using the SQUEEZE/PLATON procedure. (Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194?01) as implemented in PLATON (Spek, A.L. Acta Crystallogr. 1990, A46, C34; Spek, A.L. J. Appl. Cryst. 2003, 36, 7?3. PLATON - a multipurpose crystallographic tool. Utrecht University, Utrecht, The Netherlands). ;