# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Scott Bunge' _publ_contact_author_email SBUNGE@KENT.EDU _publ_section_title ; 1,1,3,3-Tetramethylguanidine solvated lanthanide aryloxides: Pre-catalysts for intramolecular hydroalkoxylation ; loop_ _publ_author_name 'Scott Bunge' 'Jeffrey A. Bertke' 'Christopher B. Durr' 'Thomas E. Janini' 'R.Rakosi III' # Attachment 'TotalCheckCif.cif' data_tej001 _database_code_depnum_ccdc_archive 'CCDC 722738' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Nd(OEt)(4MeDBP)2(H-TMG)2) (1)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H77 N6 Nd O3' _chemical_formula_weight 858.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.027(5) _cell_length_b 15.239(4) _cell_length_c 19.483(6) _cell_angle_alpha 90.00 _cell_angle_beta 111.427(4) _cell_angle_gamma 90.00 _cell_volume 4706(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7617 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 30.52 _exptl_crystal_description irregular _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1820 _exptl_absorpt_coefficient_mu 1.143 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7255 _exptl_absorpt_correction_T_max 0.8037 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 37397 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0163 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.05 _reflns_number_total 8345 _reflns_number_gt 7825 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.2737P] 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 8345 _refine_ls_number_parameters 492 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0203 _refine_ls_R_factor_gt 0.0185 _refine_ls_wR_factor_ref 0.0789 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 0.712 _refine_ls_restrained_S_all 0.712 _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 Nd1 Nd 0.273140(5) 0.192814(5) 0.148299(4) 0.01420(6) Uani 1 1 d . . . N1 N 0.29001(9) 0.03086(9) 0.12384(8) 0.0205(3) Uani 1 1 d . . . H1 H 0.3397 0.0147 0.1553 0.025 Uiso 1 1 calc R . . N2 N 0.18506(9) -0.03026(9) 0.02334(8) 0.0235(3) Uani 1 1 d . . . N3 N 0.28822(9) -0.12208(9) 0.10144(8) 0.0254(3) Uani 1 1 d . . . N4 N 0.25103(11) 0.30111(8) 0.23734(9) 0.0221(3) Uani 1 1 d . . . H4 H 0.1991 0.2900 0.2342 0.027 Uiso 1 1 calc R . . N5 N 0.34779(9) 0.40833(9) 0.29724(8) 0.0230(3) Uani 1 1 d . . . N6 N 0.22766(10) 0.39113(9) 0.32651(9) 0.0263(3) Uani 1 1 d . . . O1 O 0.41237(7) 0.17291(8) 0.21059(6) 0.0165(2) Uani 1 1 d . . . O2 O 0.13548(8) 0.17987(7) 0.13482(7) 0.0180(3) Uani 1 1 d . . . O3 O 0.26319(7) 0.26515(7) 0.05326(6) 0.0212(2) Uani 1 1 d . . . C1 C 0.76143(11) 0.08847(14) 0.33836(10) 0.0318(4) Uani 1 1 d . . . H1A H 0.7709 0.0350 0.3145 0.048 Uiso 1 1 calc R . . H1B H 0.7769 0.0778 0.3913 0.048 Uiso 1 1 calc R . . H1C H 0.7961 0.1361 0.3309 0.048 Uiso 1 1 calc R . . C2 C 0.66932(10) 0.11386(12) 0.30498(10) 0.0211(4) Uani 1 1 d . . . C3 C 0.63366(10) 0.14410(10) 0.23307(9) 0.0192(3) Uani 1 1 d . . . H3 H 0.6689 0.1507 0.2052 0.023 Uiso 1 1 calc R . . C4 C 0.54854(10) 0.16530(11) 0.19985(8) 0.0164(3) Uani 1 1 d . . . C5 C 0.49520(9) 0.15498(9) 0.24112(8) 0.0147(3) Uani 1 1 d . . . C6 C 0.53132(10) 0.12577(10) 0.31592(8) 0.0161(3) Uani 1 1 d . . . C7 C 0.61716(10) 0.10586(10) 0.34475(9) 0.0188(3) Uani 1 1 d . . . H7 H 0.6410 0.0858 0.3943 0.023 Uiso 1 1 calc R . . C8 C 0.47808(10) 0.11418(11) 0.36445(9) 0.0190(3) Uani 1 1 d . . . C9 C 0.43571(13) 0.20075(11) 0.37131(11) 0.0241(4) Uani 1 1 d . . . H9A H 0.4791 0.2447 0.3953 0.036 Uiso 1 1 calc R . . H9B H 0.4007 0.1914 0.4009 0.036 Uiso 1 1 calc R . . H9C H 0.4003 0.2215 0.3221 0.036 Uiso 1 1 calc R . . C10 C 0.53178(11) 0.08532(12) 0.44355(9) 0.0258(4) Uani 1 1 d . . . H10A H 0.5776 0.1275 0.4653 0.039 Uiso 1 1 calc R . . H10B H 0.5557 0.0271 0.4423 0.039 Uiso 1 1 calc R . . H10C H 0.4963 0.0830 0.4733 0.039 Uiso 1 1 calc R . . C11 C 0.41162(11) 0.04205(12) 0.33211(10) 0.0271(4) Uani 1 1 d . . . H11A H 0.3794 0.0335 0.3642 0.041 Uiso 1 1 calc R . . H11B H 0.4398 -0.0129 0.3286 0.041 Uiso 1 1 calc R . . H11C H 0.3733 0.0596 0.2829 0.041 Uiso 1 1 calc R . . C12 C 0.51521(12) 0.20183(10) 0.12027(10) 0.0183(4) Uani 1 1 d . . . C13 C 0.58419(13) 0.20883(14) 0.08741(12) 0.0295(4) Uani 1 1 d . . . H13A H 0.5596 0.2311 0.0368 0.044 Uiso 1 1 calc R . . H13B H 0.6087 0.1507 0.0871 0.044 Uiso 1 1 calc R . . H13C H 0.6283 0.2491 0.1173 0.044 Uiso 1 1 calc R . . C14 C 0.48115(12) 0.29518(11) 0.12046(10) 0.0225(4) Uani 1 1 d . . . H14A H 0.5261 0.3325 0.1532 0.034 Uiso 1 1 calc R . . H14B H 0.4340 0.2934 0.1380 0.034 Uiso 1 1 calc R . . H14C H 0.4616 0.3191 0.0703 0.034 Uiso 1 1 calc R . . C15 C 0.44553(10) 0.14288(11) 0.06758(9) 0.0219(3) Uani 1 1 d . . . H15A H 0.4016 0.1330 0.0881 0.033 Uiso 1 1 calc R . . H15B H 0.4699 0.0865 0.0617 0.033 Uiso 1 1 calc R . . H15C H 0.4207 0.1717 0.0195 0.033 Uiso 1 1 calc R . . C16 C -0.15686(14) 0.24517(15) 0.20224(14) 0.0456(6) Uani 1 1 d . . . H16A H -0.1930 0.1931 0.1927 0.068 Uiso 1 1 calc R . . H16B H -0.1886 0.2942 0.1723 0.068 Uiso 1 1 calc R . . H16C H -0.1384 0.2607 0.2546 0.068 Uiso 1 1 calc R . . C17 C -0.08050(12) 0.22591(13) 0.18241(11) 0.0294(4) Uani 1 1 d . . . C18 C -0.06252(10) 0.27576(11) 0.13051(10) 0.0244(4) Uani 1 1 d . . . H18 H -0.0998 0.3223 0.1071 0.029 Uiso 1 1 calc R . . C19 C 0.00730(10) 0.26133(10) 0.11084(9) 0.0208(3) Uani 1 1 d . . . C20 C 0.06447(11) 0.19242(9) 0.14747(10) 0.0174(4) Uani 1 1 d . . . C21 C 0.04386(10) 0.13707(11) 0.19764(9) 0.0214(3) Uani 1 1 d . . . C22 C -0.02700(12) 0.15654(12) 0.21432(11) 0.0274(4) Uani 1 1 d . . . H22 H -0.0392 0.1207 0.2491 0.033 Uiso 1 1 calc R . . C23 C 0.09729(11) 0.05556(11) 0.23258(10) 0.0242(4) Uani 1 1 d . . . C24 C 0.10001(12) -0.00661(11) 0.17123(11) 0.0303(4) Uani 1 1 d . . . H24A H 0.0425 -0.0241 0.1406 0.045 Uiso 1 1 calc R . . H24B H 0.1331 -0.0589 0.1934 0.045 Uiso 1 1 calc R . . H24C H 0.1262 0.0236 0.1406 0.045 Uiso 1 1 calc R . . C25 C 0.06058(13) 0.00267(14) 0.28126(13) 0.0407(5) Uani 1 1 d . . . H25A H 0.0035 -0.0171 0.2514 0.061 Uiso 1 1 calc R . . H25B H 0.0584 0.0399 0.3216 0.061 Uiso 1 1 calc R . . H25C H 0.0965 -0.0484 0.3018 0.061 Uiso 1 1 calc R . . C26 C 0.18717(12) 0.08044(13) 0.28279(11) 0.0318(4) Uani 1 1 d . . . H26A H 0.2188 0.0272 0.3044 0.048 Uiso 1 1 calc R . . H26B H 0.1849 0.1190 0.3223 0.048 Uiso 1 1 calc R . . H26C H 0.2152 0.1110 0.2538 0.048 Uiso 1 1 calc R . . C27 C 0.02024(12) 0.32036(11) 0.05178(11) 0.0236(4) Uani 1 1 d . . . C28 C -0.05841(12) 0.37666(14) 0.01141(12) 0.0366(5) Uani 1 1 d . . . H28A H -0.0488 0.4113 -0.0272 0.055 Uiso 1 1 calc R . . H28B H -0.0691 0.4162 0.0467 0.055 Uiso 1 1 calc R . . H28C H -0.1073 0.3383 -0.0109 0.055 Uiso 1 1 calc R . . C29 C 0.09319(11) 0.38520(12) 0.08719(11) 0.0294(4) Uani 1 1 d . . . H29A H 0.0978 0.4250 0.0493 0.044 Uiso 1 1 calc R . . H29B H 0.1461 0.3526 0.1095 0.044 Uiso 1 1 calc R . . H29C H 0.0821 0.4193 0.1253 0.044 Uiso 1 1 calc R . . C30 C 0.03803(11) 0.26717(13) -0.00804(10) 0.0285(4) Uani 1 1 d . . . H30A H -0.0083 0.2258 -0.0308 0.043 Uiso 1 1 calc R . . H30B H 0.0909 0.2346 0.0143 0.043 Uiso 1 1 calc R . . H30C H 0.0428 0.3072 -0.0457 0.043 Uiso 1 1 calc R . . C31 C 0.25645(10) -0.03834(10) 0.08462(9) 0.0198(3) Uani 1 1 d . . . C32 C 0.15410(12) 0.05730(12) -0.00213(10) 0.0262(4) Uani 1 1 d . . . H32A H 0.1278 0.0825 0.0305 0.039 Uiso 1 1 calc R . . H32B H 0.1123 0.0539 -0.0525 0.039 Uiso 1 1 calc R . . H32C H 0.2013 0.0945 -0.0016 0.039 Uiso 1 1 calc R . . C33 C 0.11863(12) -0.09762(13) 0.00277(12) 0.0331(4) Uani 1 1 d . . . H33A H 0.1377 -0.1483 0.0356 0.050 Uiso 1 1 calc R . . H33B H 0.1065 -0.1161 -0.0483 0.050 Uiso 1 1 calc R . . H33C H 0.0674 -0.0734 0.0072 0.050 Uiso 1 1 calc R . . C34 C 0.29404(16) -0.17962(14) 0.04358(13) 0.0411(5) Uani 1 1 d . . . H34A H 0.2563 -0.1581 -0.0046 0.062 Uiso 1 1 calc R . . H34B H 0.2775 -0.2393 0.0514 0.062 Uiso 1 1 calc R . . H34C H 0.3522 -0.1801 0.0452 0.062 Uiso 1 1 calc R . . C35 C 0.35346(13) -0.13709(13) 0.17331(11) 0.0352(5) Uani 1 1 d . . . H35A H 0.4063 -0.1101 0.1748 0.053 Uiso 1 1 calc R . . H35B H 0.3618 -0.2003 0.1820 0.053 Uiso 1 1 calc R . . H35C H 0.3362 -0.1109 0.2116 0.053 Uiso 1 1 calc R . . C36 C 0.27408(11) 0.36425(11) 0.28525(9) 0.0205(3) Uani 1 1 d . . . C37 C 0.40184(12) 0.43778(12) 0.37047(10) 0.0306(4) Uani 1 1 d . . . H37A H 0.3724 0.4298 0.4049 0.046 Uiso 1 1 calc R . . H37B H 0.4154 0.5000 0.3685 0.046 Uiso 1 1 calc R . . H37C H 0.4541 0.4034 0.3873 0.046 Uiso 1 1 calc R . . C38 C 0.39022(11) 0.39777(12) 0.24520(10) 0.0252(4) Uani 1 1 d . . . H38A H 0.4244 0.3442 0.2570 0.038 Uiso 1 1 calc R . . H38B H 0.4267 0.4485 0.2484 0.038 Uiso 1 1 calc R . . H38C H 0.3481 0.3934 0.1951 0.038 Uiso 1 1 calc R . . C39 C 0.21817(13) 0.48457(14) 0.33845(13) 0.0378(5) Uani 1 1 d . . . H39A H 0.2603 0.5180 0.3260 0.057 Uiso 1 1 calc R . . H39B H 0.2263 0.4946 0.3903 0.057 Uiso 1 1 calc R . . H39C H 0.1615 0.5038 0.3071 0.057 Uiso 1 1 calc R . . C40 C 0.15422(13) 0.33767(13) 0.32221(12) 0.0343(4) Uani 1 1 d . . . H40A H 0.1083 0.3481 0.2748 0.051 Uiso 1 1 calc R . . H40B H 0.1356 0.3538 0.3625 0.051 Uiso 1 1 calc R . . H40C H 0.1698 0.2754 0.3264 0.051 Uiso 1 1 calc R . . C41 C 0.25578(13) 0.31435(11) -0.00954(11) 0.0259(4) Uani 1 1 d . . . H41A H 0.1977 0.3085 -0.0462 0.031 Uiso 1 1 calc R . . H41B H 0.2951 0.2906 -0.0319 0.031 Uiso 1 1 calc R . . C42 C 0.27508(13) 0.41057(12) 0.00828(11) 0.0332(4) Uani 1 1 d . . . H42A H 0.2355 0.4346 0.0293 0.050 Uiso 1 1 calc R . . H42B H 0.2694 0.4425 -0.0369 0.050 Uiso 1 1 calc R . . H42C H 0.3329 0.4168 0.0440 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.01256(8) 0.01285(8) 0.01586(8) 0.00001(2) 0.00360(6) -0.00031(2) N1 0.0178(7) 0.0168(7) 0.0243(7) -0.0020(6) 0.0049(6) -0.0016(5) N2 0.0259(8) 0.0164(7) 0.0230(7) -0.0036(6) 0.0027(6) -0.0024(6) N3 0.0278(8) 0.0162(7) 0.0278(8) -0.0037(6) 0.0052(6) 0.0014(6) N4 0.0196(8) 0.0227(8) 0.0228(8) -0.0036(5) 0.0062(7) 0.0011(5) N5 0.0254(7) 0.0207(7) 0.0213(7) -0.0028(6) 0.0065(6) -0.0025(6) N6 0.0362(9) 0.0180(7) 0.0305(8) -0.0056(6) 0.0191(7) -0.0042(6) O1 0.0151(6) 0.0171(5) 0.0162(6) 0.0013(5) 0.0046(5) 0.0004(5) O2 0.0139(6) 0.0178(6) 0.0218(7) 0.0022(5) 0.0059(5) 0.0000(4) O3 0.0213(6) 0.0197(6) 0.0214(6) 0.0040(5) 0.0064(5) -0.0006(5) C1 0.0172(9) 0.0490(12) 0.0254(9) 0.0047(8) 0.0033(7) 0.0045(8) C2 0.0160(8) 0.0213(9) 0.0231(9) -0.0023(7) 0.0038(7) -0.0007(7) C3 0.0185(8) 0.0185(8) 0.0212(8) -0.0019(6) 0.0080(7) -0.0012(6) C4 0.0184(8) 0.0129(7) 0.0165(8) -0.0007(6) 0.0045(6) -0.0001(6) C5 0.0139(7) 0.0104(8) 0.0178(8) -0.0014(6) 0.0033(6) 0.0000(6) C6 0.0188(8) 0.0117(7) 0.0174(8) -0.0022(6) 0.0063(6) 0.0000(6) C7 0.0205(8) 0.0177(8) 0.0148(7) 0.0006(6) 0.0022(6) 0.0013(6) C8 0.0219(8) 0.0180(8) 0.0179(8) 0.0024(6) 0.0082(7) 0.0036(6) C9 0.0312(11) 0.0230(10) 0.0203(9) 0.0023(6) 0.0122(8) 0.0091(7) C10 0.0284(9) 0.0284(9) 0.0221(9) 0.0077(7) 0.0108(7) 0.0092(7) C11 0.0278(9) 0.0243(9) 0.0323(10) 0.0067(8) 0.0146(8) -0.0021(7) C12 0.0182(9) 0.0204(9) 0.0164(9) 0.0016(6) 0.0064(7) 0.0007(6) C13 0.0268(11) 0.0387(10) 0.0270(10) 0.0106(8) 0.0146(9) 0.0054(8) C14 0.0249(10) 0.0188(8) 0.0234(9) 0.0043(7) 0.0085(8) -0.0004(7) C15 0.0232(8) 0.0236(9) 0.0163(8) -0.0015(6) 0.0042(7) 0.0036(7) C16 0.0401(12) 0.0357(12) 0.0759(16) 0.0032(11) 0.0387(12) 0.0051(9) C17 0.0236(9) 0.0238(10) 0.0450(11) -0.0058(8) 0.0176(9) -0.0015(8) C18 0.0191(8) 0.0164(8) 0.0351(10) -0.0031(7) 0.0070(7) 0.0007(7) C19 0.0160(8) 0.0169(8) 0.0258(9) -0.0030(7) 0.0033(7) -0.0032(6) C20 0.0136(9) 0.0138(9) 0.0226(9) -0.0042(5) 0.0041(8) -0.0033(5) C21 0.0204(8) 0.0182(8) 0.0250(9) -0.0018(7) 0.0078(7) -0.0036(6) C22 0.0272(9) 0.0221(10) 0.0371(11) 0.0002(8) 0.0166(8) -0.0048(8) C23 0.0242(9) 0.0215(9) 0.0283(9) 0.0059(7) 0.0111(7) -0.0002(7) C24 0.0319(10) 0.0176(9) 0.0390(11) 0.0023(8) 0.0102(8) 0.0025(7) C25 0.0381(12) 0.0341(11) 0.0569(14) 0.0189(10) 0.0256(10) 0.0042(9) C26 0.0273(9) 0.0319(10) 0.0298(10) 0.0101(8) 0.0028(8) 0.0003(8) C27 0.0199(9) 0.0184(8) 0.0296(10) 0.0051(7) 0.0056(8) 0.0025(7) C28 0.0245(10) 0.0350(11) 0.0443(12) 0.0138(9) 0.0053(9) 0.0060(8) C29 0.0249(9) 0.0208(9) 0.0389(10) 0.0059(8) 0.0074(8) -0.0017(7) C30 0.0276(9) 0.0296(11) 0.0249(9) 0.0078(8) 0.0057(7) -0.0010(8) C31 0.0214(8) 0.0170(8) 0.0235(8) -0.0007(6) 0.0112(7) -0.0012(6) C32 0.0295(9) 0.0246(9) 0.0192(8) 0.0006(7) 0.0027(7) 0.0023(7) C33 0.0284(10) 0.0274(10) 0.0357(11) -0.0080(8) 0.0023(8) -0.0065(8) C34 0.0524(15) 0.0295(10) 0.0413(13) -0.0082(9) 0.0171(11) 0.0117(9) C35 0.0375(11) 0.0207(9) 0.0369(11) 0.0023(8) 0.0014(9) 0.0055(8) C36 0.0270(9) 0.0163(8) 0.0164(8) 0.0026(6) 0.0057(7) 0.0034(7) C37 0.0366(10) 0.0243(9) 0.0254(9) -0.0033(7) 0.0047(8) -0.0037(8) C38 0.0282(9) 0.0206(9) 0.0278(9) 0.0020(7) 0.0114(8) -0.0007(7) C39 0.0489(13) 0.0222(11) 0.0544(12) -0.0076(9) 0.0332(11) -0.0014(8) C40 0.0437(12) 0.0284(10) 0.0398(12) -0.0078(9) 0.0258(10) -0.0059(9) C41 0.0280(10) 0.0277(10) 0.0224(10) 0.0043(7) 0.0097(8) -0.0045(7) C42 0.0362(10) 0.0242(10) 0.0380(11) 0.0105(8) 0.0122(9) -0.0013(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 Nd1 O3 2.1079(12) . ? Nd1 O1 2.2546(13) . ? Nd1 O2 2.2699(14) . ? Nd1 N4 2.5203(16) . ? Nd1 N1 2.5497(15) . ? N1 C31 1.305(2) . ? N1 H1 0.8800 . ? N2 C31 1.363(2) . ? N2 C32 1.454(2) . ? N2 C33 1.471(2) . ? N3 C31 1.378(2) . ? N3 C35 1.453(2) . ? N3 C34 1.460(3) . ? N4 C36 1.298(2) . ? N4 H4 0.8800 . ? N5 C36 1.366(2) . ? N5 C38 1.453(2) . ? N5 C37 1.458(2) . ? N6 C36 1.379(2) . ? N6 C39 1.461(3) . ? N6 C40 1.469(2) . ? O1 C5 1.3434(19) . ? O2 C20 1.333(2) . ? O3 C41 1.401(2) . ? C1 C2 1.512(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C7 1.381(2) . ? C2 C3 1.387(2) . ? C3 C4 1.392(2) . ? C3 H3 0.9500 . ? C4 C5 1.425(2) . ? C4 C12 1.547(2) . ? C5 C6 1.430(2) . ? C6 C7 1.394(2) . ? C6 C8 1.540(2) . ? C7 H7 0.9500 . ? C8 C9 1.533(2) . ? C8 C11 1.538(2) . ? C8 C10 1.541(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.533(3) . ? C12 C14 1.537(2) . ? C12 C15 1.542(2) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.514(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.385(3) . ? C17 C22 1.386(3) . ? C18 C19 1.393(2) . ? C18 H18 0.9500 . ? C19 C20 1.433(2) . ? C19 C27 1.538(3) . ? C20 C21 1.429(2) . ? C21 C22 1.391(2) . ? C21 C23 1.543(2) . ? C22 H22 0.9500 . ? C23 C26 1.533(3) . ? C23 C24 1.539(3) . ? C23 C25 1.540(2) . ? 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 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C30 1.538(3) . ? C27 C29 1.539(3) . ? C27 C28 1.542(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? 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 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? 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 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.515(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Nd1 O1 105.93(4) . . ? O3 Nd1 O2 101.28(4) . . ? O1 Nd1 O2 152.74(5) . . ? O3 Nd1 N4 106.13(5) . . ? O1 Nd1 N4 96.30(5) . . ? O2 Nd1 N4 74.27(5) . . ? O3 Nd1 N1 108.69(5) . . ? O1 Nd1 N1 78.60(4) . . ? O2 Nd1 N1 94.38(4) . . ? N4 Nd1 N1 144.87(5) . . ? C31 N1 Nd1 146.77(12) . . ? C31 N1 H1 106.6 . . ? Nd1 N1 H1 106.6 . . ? C31 N2 C32 118.56(13) . . ? C31 N2 C33 121.78(15) . . ? C32 N2 C33 113.62(15) . . ? C31 N3 C35 118.06(14) . . ? C31 N3 C34 120.28(16) . . ? C35 N3 C34 113.95(16) . . ? C36 N4 Nd1 153.99(14) . . ? C36 N4 H4 103.0 . . ? Nd1 N4 H4 103.0 . . ? C36 N5 C38 119.09(14) . . ? C36 N5 C37 122.06(15) . . ? C38 N5 C37 114.83(15) . . ? C36 N6 C39 120.16(14) . . ? C36 N6 C40 117.34(14) . . ? C39 N6 C40 114.09(15) . . ? C5 O1 Nd1 173.28(10) . . ? C20 O2 Nd1 159.09(11) . . ? C41 O3 Nd1 179.00(12) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 117.54(15) . . ? C7 C2 C1 120.97(16) . . ? C3 C2 C1 121.48(16) . . ? C2 C3 C4 122.95(15) . . ? C2 C3 H3 118.5 . . ? C4 C3 H3 118.5 . . ? C3 C4 C5 118.83(14) . . ? C3 C4 C12 119.19(14) . . ? C5 C4 C12 121.96(14) . . ? O1 C5 C4 120.68(14) . . ? O1 C5 C6 120.38(13) . . ? C4 C5 C6 118.95(14) . . ? C7 C6 C5 118.39(14) . . ? C7 C6 C8 119.55(14) . . ? C5 C6 C8 122.05(14) . . ? C2 C7 C6 123.31(15) . . ? C2 C7 H7 118.3 . . ? C6 C7 H7 118.3 . . ? C9 C8 C11 110.58(14) . . ? C9 C8 C6 110.85(13) . . ? C11 C8 C6 109.91(13) . . ? C9 C8 C10 106.54(14) . . ? C11 C8 C10 106.55(14) . . ? C6 C8 C10 112.28(13) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C14 106.50(15) . . ? C13 C12 C15 106.44(15) . . ? C14 C12 C15 109.97(14) . . ? C13 C12 C4 112.77(15) . . ? C14 C12 C4 109.35(14) . . ? C15 C12 C4 111.64(13) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 117.48(16) . . ? C18 C17 C16 121.28(18) . . ? C22 C17 C16 121.22(18) . . ? C17 C18 C19 123.54(17) . . ? C17 C18 H18 118.2 . . ? C19 C18 H18 118.2 . . ? C18 C19 C20 118.14(16) . . ? C18 C19 C27 118.89(15) . . ? C20 C19 C27 122.97(16) . . ? O2 C20 C21 120.53(14) . . ? O2 C20 C19 120.69(15) . . ? C21 C20 C19 118.78(16) . . ? C22 C21 C20 118.99(16) . . ? C22 C21 C23 119.37(15) . . ? C20 C21 C23 121.63(15) . . ? C17 C22 C21 122.81(17) . . ? C17 C22 H22 118.6 . . ? C21 C22 H22 118.6 . . ? C26 C23 C24 109.98(15) . . ? C26 C23 C25 105.76(15) . . ? C24 C23 C25 106.86(16) . . ? C26 C23 C21 111.89(14) . . ? C24 C23 C21 109.46(14) . . ? C25 C23 C21 112.73(15) . . ? 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 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C30 C27 C19 112.36(14) . . ? C30 C27 C29 109.13(16) . . ? C19 C27 C29 110.66(15) . . ? C30 C27 C28 106.34(16) . . ? C19 C27 C28 111.83(16) . . ? C29 C27 C28 106.24(15) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N1 C31 N2 119.96(15) . . ? N1 C31 N3 124.01(15) . . ? N2 C31 N3 116.03(14) . . ? N2 C32 H32A 109.5 . . ? N2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N2 C33 H33A 109.5 . . ? N2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N3 C34 H34A 109.5 . . ? N3 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N3 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N3 C35 H35A 109.5 . . ? N3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N4 C36 N5 120.35(16) . . ? N4 C36 N6 123.52(16) . . ? N5 C36 N6 116.14(15) . . ? N5 C37 H37A 109.5 . . ? N5 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N5 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N5 C38 H38A 109.5 . . ? N5 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N5 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N6 C39 H39A 109.5 . . ? N6 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N6 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N6 C40 H40A 109.5 . . ? N6 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N6 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O3 C41 C42 112.03(16) . . ? O3 C41 H41A 109.2 . . ? C42 C41 H41A 109.2 . . ? O3 C41 H41B 109.2 . . ? C42 C41 H41B 109.2 . . ? H41A C41 H41B 107.9 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.461 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.049 #===END data_bob033 _database_code_depnum_ccdc_archive 'CCDC 722739' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(La(OEt)(DBP)2(H-TMG)2) (2)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H73 La N6 O3' _chemical_formula_weight 824.95 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' La La -0.2871 2.4523 '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' _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 10.8947(19) _cell_length_b 10.9333(19) _cell_length_c 19.216(3) _cell_angle_alpha 100.912(3) _cell_angle_beta 99.102(3) _cell_angle_gamma 92.317(3) _cell_volume 2213.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6225 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 30.52 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 1.005 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7525 _exptl_absorpt_correction_T_max 0.8243 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 17587 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 25.05 _reflns_number_total 7756 _reflns_number_gt 7246 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 7756 _refine_ls_number_parameters 472 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.1527 _refine_ls_wR_factor_gt 0.1492 _refine_ls_goodness_of_fit_ref 1.292 _refine_ls_restrained_S_all 1.292 _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 La1 La 0.517212(19) 0.467526(19) 0.278274(11) 0.02254(12) Uani 1 1 d . . . N1 N 0.4090(4) 0.6570(3) 0.3419(2) 0.0330(9) Uani 1 1 d . . . H1 H 0.4709 0.7031 0.3714 0.040 Uiso 1 1 calc R . . N2 N 0.3184(4) 0.8464(4) 0.3760(2) 0.0370(9) Uani 1 1 d . . . N3 N 0.1968(4) 0.6580(4) 0.3401(2) 0.0354(9) Uani 1 1 d . . . N4 N 0.6086(4) 0.3252(4) 0.1755(2) 0.0335(9) Uani 1 1 d . . . H4 H 0.5422 0.2884 0.1455 0.040 Uiso 1 1 calc R . . N5 N 0.6885(4) 0.2113(4) 0.0772(2) 0.0353(9) Uani 1 1 d . . . N6 N 0.8204(4) 0.3023(4) 0.1832(2) 0.0347(9) Uani 1 1 d . . . O1 O 0.6753(3) 0.6248(3) 0.31355(15) 0.0241(6) Uani 1 1 d . . . O2 O 0.3448(3) 0.3720(3) 0.19565(15) 0.0241(6) Uani 1 1 d . . . O3 O 0.5465(3) 0.3546(3) 0.35770(18) 0.0374(8) Uani 1 1 d . . . C1 C 0.8947(5) 0.9566(5) 0.3887(3) 0.0387(12) Uani 1 1 d . . . H1A H 0.9407 1.0349 0.4066 0.046 Uiso 1 1 calc R . . C2 C 0.8390(5) 0.9248(4) 0.3171(3) 0.0330(10) Uani 1 1 d . . . H2 H 0.8497 0.9809 0.2859 0.040 Uiso 1 1 calc R . . C3 C 0.7673(4) 0.8120(4) 0.2897(2) 0.0257(9) Uani 1 1 d . . . C4 C 0.7491(4) 0.7297(4) 0.3371(2) 0.0221(8) Uani 1 1 d . . . C5 C 0.8136(4) 0.7598(4) 0.4102(2) 0.0264(9) Uani 1 1 d . . . C6 C 0.8832(5) 0.8743(4) 0.4337(3) 0.0336(11) Uani 1 1 d . . . H6 H 0.9240 0.8961 0.4823 0.040 Uiso 1 1 calc R . . C7 C 0.7063(4) 0.7828(4) 0.2102(2) 0.0314(10) Uani 1 1 d . . . C8 C 0.7474(7) 0.8793(5) 0.1679(3) 0.0515(15) Uani 1 1 d . . . H8A H 0.7257 0.9624 0.1896 0.077 Uiso 1 1 calc R . . H8B H 0.7050 0.8569 0.1178 0.077 Uiso 1 1 calc R . . H8C H 0.8378 0.8800 0.1693 0.077 Uiso 1 1 calc R . . C9 C 0.5632(5) 0.7869(5) 0.2044(3) 0.0392(11) Uani 1 1 d . . . H9A H 0.5319 0.7267 0.2305 0.059 Uiso 1 1 calc R . . H9B H 0.5240 0.7655 0.1537 0.059 Uiso 1 1 calc R . . H9C H 0.5433 0.8710 0.2255 0.059 Uiso 1 1 calc R . . C10 C 0.7405(5) 0.6556(5) 0.1717(2) 0.0373(11) Uani 1 1 d . . . H10A H 0.8311 0.6563 0.1745 0.056 Uiso 1 1 calc R . . H10B H 0.7003 0.6397 0.1212 0.056 Uiso 1 1 calc R . . H10C H 0.7119 0.5898 0.1949 0.056 Uiso 1 1 calc R . . C11 C 0.8074(4) 0.6713(4) 0.4637(2) 0.0271(9) Uani 1 1 d . . . C12 C 0.6752(5) 0.6571(5) 0.4799(3) 0.0418(12) Uani 1 1 d . . . H12A H 0.6193 0.6140 0.4363 0.063 Uiso 1 1 calc R . . H12B H 0.6465 0.7398 0.4962 0.063 Uiso 1 1 calc R . . H12C H 0.6750 0.6082 0.5178 0.063 Uiso 1 1 calc R . . C13 C 0.8491(5) 0.5416(4) 0.4339(3) 0.0366(11) Uani 1 1 d . . . H13A H 0.8476 0.4885 0.4696 0.055 Uiso 1 1 calc R . . H13B H 0.9339 0.5504 0.4235 0.055 Uiso 1 1 calc R . . H13C H 0.7923 0.5033 0.3896 0.055 Uiso 1 1 calc R . . C14 C 0.8939(5) 0.7209(5) 0.5359(3) 0.0422(12) Uani 1 1 d . . . H14A H 0.8695 0.8029 0.5575 0.063 Uiso 1 1 calc R . . H14B H 0.9802 0.7286 0.5278 0.063 Uiso 1 1 calc R . . H14C H 0.8870 0.6627 0.5684 0.063 Uiso 1 1 calc R . . C15 C 0.1002(5) 0.1800(5) 0.0176(3) 0.0437(13) Uani 1 1 d . . . H15 H 0.0465 0.1346 -0.0239 0.052 Uiso 1 1 calc R . . C16 C 0.1376(5) 0.1242(4) 0.0750(3) 0.0369(11) Uani 1 1 d . . . H16 H 0.1084 0.0400 0.0722 0.044 Uiso 1 1 calc R . . C17 C 0.2165(4) 0.1854(4) 0.1372(3) 0.0289(10) Uani 1 1 d . . . C18 C 0.2623(4) 0.3113(4) 0.1396(2) 0.0235(8) Uani 1 1 d . . . C19 C 0.2199(4) 0.3708(4) 0.0809(2) 0.0251(9) Uani 1 1 d . . . C20 C 0.1409(4) 0.3021(5) 0.0205(3) 0.0331(10) Uani 1 1 d . . . H20 H 0.1146 0.3404 -0.0193 0.040 Uiso 1 1 calc R . . C21 C 0.2534(5) 0.1172(4) 0.2002(3) 0.0367(11) Uani 1 1 d . . . C22 C 0.2224(6) 0.1910(5) 0.2702(3) 0.0439(13) Uani 1 1 d . . . H22A H 0.2718 0.2714 0.2834 0.066 Uiso 1 1 calc R . . H22B H 0.2421 0.1435 0.3085 0.066 Uiso 1 1 calc R . . H22C H 0.1335 0.2055 0.2638 0.066 Uiso 1 1 calc R . . C23 C 0.3940(5) 0.0966(5) 0.2090(3) 0.0472(13) Uani 1 1 d . . . H23A H 0.4142 0.0551 0.1628 0.071 Uiso 1 1 calc R . . H23B H 0.4147 0.0443 0.2447 0.071 Uiso 1 1 calc R . . H23C H 0.4422 0.1774 0.2251 0.071 Uiso 1 1 calc R . . C24 C 0.1839(7) -0.0130(5) 0.1866(4) 0.0603(17) Uani 1 1 d . . . H24A H 0.0939 -0.0052 0.1758 0.090 Uiso 1 1 calc R . . H24B H 0.2030 -0.0494 0.2296 0.090 Uiso 1 1 calc R . . H24C H 0.2106 -0.0672 0.1458 0.090 Uiso 1 1 calc R . . C25 C 0.2622(4) 0.5072(4) 0.0818(2) 0.0263(9) Uani 1 1 d . . . C26 C 0.1949(5) 0.5551(5) 0.0165(3) 0.0384(11) Uani 1 1 d . . . H26A H 0.2271 0.6408 0.0183 0.058 Uiso 1 1 calc R . . H26B H 0.1052 0.5535 0.0175 0.058 Uiso 1 1 calc R . . H26C H 0.2097 0.5013 -0.0280 0.058 Uiso 1 1 calc R . . C27 C 0.2348(5) 0.5963(4) 0.1481(2) 0.0334(10) Uani 1 1 d . . . H27A H 0.2776 0.5719 0.1916 0.050 Uiso 1 1 calc R . . H27B H 0.1447 0.5926 0.1481 0.050 Uiso 1 1 calc R . . H27C H 0.2643 0.6817 0.1470 0.050 Uiso 1 1 calc R . . C28 C 0.4017(4) 0.5147(4) 0.0768(3) 0.0345(10) Uani 1 1 d . . . H28A H 0.4147 0.4627 0.0314 0.052 Uiso 1 1 calc R . . H28B H 0.4490 0.4847 0.1172 0.052 Uiso 1 1 calc R . . H28C H 0.4303 0.6016 0.0785 0.052 Uiso 1 1 calc R . . C29 C 0.3119(4) 0.7186(4) 0.3526(2) 0.0286(9) Uani 1 1 d . . . C30 C 0.1881(5) 0.5232(5) 0.3324(3) 0.0428(12) Uani 1 1 d . . . H30A H 0.1952 0.4843 0.2830 0.064 Uiso 1 1 calc R . . H30B H 0.1077 0.4957 0.3431 0.064 Uiso 1 1 calc R . . H30C H 0.2557 0.4986 0.3659 0.064 Uiso 1 1 calc R . . C31 C 0.0872(5) 0.7092(5) 0.3053(3) 0.0414(12) Uani 1 1 d . . . H31A H 0.1089 0.7949 0.3008 0.062 Uiso 1 1 calc R . . H31B H 0.0208 0.7093 0.3343 0.062 Uiso 1 1 calc R . . H31C H 0.0583 0.6578 0.2574 0.062 Uiso 1 1 calc R . . C32 C 0.2345(6) 0.9055(5) 0.4220(3) 0.0536(15) Uani 1 1 d . . . H32A H 0.1788 0.8413 0.4326 0.080 Uiso 1 1 calc R . . H32B H 0.1849 0.9624 0.3974 0.080 Uiso 1 1 calc R . . H32C H 0.2833 0.9527 0.4670 0.080 Uiso 1 1 calc R . . C33 C 0.4358(6) 0.9178(5) 0.3824(3) 0.0512(14) Uani 1 1 d . . . H33A H 0.4903 0.9095 0.4268 0.077 Uiso 1 1 calc R . . H33B H 0.4207 1.0059 0.3838 0.077 Uiso 1 1 calc R . . H33C H 0.4758 0.8863 0.3410 0.077 Uiso 1 1 calc R . . C34 C 0.7017(4) 0.2810(4) 0.1459(2) 0.0290(9) Uani 1 1 d . . . C35 C 0.5677(5) 0.1976(5) 0.0311(3) 0.0469(13) Uani 1 1 d . . . H35A H 0.5136 0.1354 0.0446 0.070 Uiso 1 1 calc R . . H35B H 0.5780 0.1701 -0.0191 0.070 Uiso 1 1 calc R . . H35C H 0.5300 0.2780 0.0367 0.070 Uiso 1 1 calc R . . C36 C 0.7704(6) 0.1128(5) 0.0577(3) 0.0449(13) Uani 1 1 d . . . H36A H 0.8309 0.1063 0.1001 0.067 Uiso 1 1 calc R . . H36B H 0.8147 0.1328 0.0202 0.067 Uiso 1 1 calc R . . H36C H 0.7207 0.0331 0.0397 0.067 Uiso 1 1 calc R . . C37 C 0.8363(5) 0.3529(5) 0.2601(3) 0.0431(12) Uani 1 1 d . . . H37A H 0.8271 0.4430 0.2681 0.065 Uiso 1 1 calc R . . H37B H 0.9195 0.3374 0.2832 0.065 Uiso 1 1 calc R . . H37C H 0.7731 0.3122 0.2809 0.065 Uiso 1 1 calc R . . C38 C 0.9215(5) 0.3466(5) 0.1498(3) 0.0387(11) Uani 1 1 d . . . H38A H 0.8993 0.3222 0.0973 0.058 Uiso 1 1 calc R . . H38B H 0.9985 0.3093 0.1660 0.058 Uiso 1 1 calc R . . H38C H 0.9341 0.4378 0.1636 0.058 Uiso 1 1 calc R . . C39 C 0.5663(6) 0.2727(6) 0.4056(3) 0.0537(15) Uani 1 1 d . . . H39A H 0.4875 0.2229 0.4037 0.064 Uiso 1 1 calc R . . H39B H 0.5912 0.3216 0.4552 0.064 Uiso 1 1 calc R . . C40 C 0.6642(7) 0.1872(7) 0.3883(5) 0.080(2) Uani 1 1 d . . . H40A H 0.6398 0.1385 0.3393 0.121 Uiso 1 1 calc R . . H40B H 0.6745 0.1305 0.4223 0.121 Uiso 1 1 calc R . . H40C H 0.7431 0.2361 0.3918 0.121 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.01979(17) 0.02148(17) 0.02649(18) 0.00414(11) 0.00493(11) 0.00191(10) N1 0.027(2) 0.030(2) 0.039(2) -0.0006(16) 0.0019(16) 0.0077(16) N2 0.039(2) 0.028(2) 0.042(2) -0.0001(17) 0.0079(19) 0.0066(17) N3 0.029(2) 0.033(2) 0.048(2) 0.0093(18) 0.0149(18) 0.0093(17) N4 0.028(2) 0.034(2) 0.037(2) 0.0006(17) 0.0108(17) 0.0023(16) N5 0.042(2) 0.033(2) 0.031(2) 0.0007(17) 0.0114(18) 0.0079(18) N6 0.030(2) 0.048(2) 0.029(2) 0.0077(18) 0.0118(16) 0.0077(18) O1 0.0217(15) 0.0232(14) 0.0259(15) 0.0033(11) 0.0022(12) -0.0008(11) O2 0.0232(15) 0.0222(14) 0.0268(15) 0.0048(12) 0.0047(12) 0.0002(11) O3 0.042(2) 0.0336(17) 0.0397(18) 0.0146(14) 0.0067(15) 0.0035(15) C1 0.044(3) 0.025(2) 0.040(3) -0.002(2) -0.001(2) -0.004(2) C2 0.038(3) 0.026(2) 0.034(2) 0.0065(19) 0.003(2) -0.0024(19) C3 0.024(2) 0.024(2) 0.027(2) 0.0014(17) 0.0039(17) 0.0009(17) C4 0.018(2) 0.024(2) 0.023(2) -0.0005(16) 0.0068(16) 0.0041(16) C5 0.021(2) 0.032(2) 0.026(2) 0.0011(18) 0.0085(17) 0.0066(18) C6 0.035(3) 0.029(2) 0.029(2) -0.0058(19) -0.0020(19) -0.0025(19) C7 0.037(3) 0.032(2) 0.025(2) 0.0045(18) 0.0057(19) 0.0013(19) C8 0.078(4) 0.044(3) 0.031(3) 0.011(2) 0.004(3) -0.014(3) C9 0.037(3) 0.040(3) 0.037(3) 0.008(2) -0.006(2) 0.003(2) C10 0.042(3) 0.041(3) 0.027(2) 0.002(2) 0.007(2) 0.003(2) C11 0.027(2) 0.031(2) 0.021(2) 0.0027(17) 0.0019(17) 0.0011(18) C12 0.037(3) 0.060(3) 0.033(3) 0.014(2) 0.013(2) 0.008(2) C13 0.046(3) 0.031(2) 0.032(2) 0.0067(19) 0.002(2) 0.013(2) C14 0.052(3) 0.042(3) 0.029(2) 0.003(2) 0.000(2) 0.000(2) C15 0.039(3) 0.042(3) 0.038(3) -0.018(2) 0.006(2) -0.008(2) C16 0.040(3) 0.021(2) 0.046(3) -0.009(2) 0.017(2) -0.0045(19) C17 0.028(2) 0.019(2) 0.041(3) -0.0002(18) 0.014(2) 0.0030(17) C18 0.019(2) 0.021(2) 0.030(2) 0.0005(17) 0.0107(17) -0.0021(16) C19 0.022(2) 0.025(2) 0.028(2) 0.0021(17) 0.0083(17) 0.0018(17) C20 0.029(2) 0.038(3) 0.031(2) -0.001(2) 0.0084(19) 0.003(2) C21 0.043(3) 0.021(2) 0.049(3) 0.009(2) 0.016(2) 0.002(2) C22 0.052(3) 0.036(3) 0.052(3) 0.017(2) 0.022(3) 0.007(2) C23 0.048(3) 0.036(3) 0.066(4) 0.021(3) 0.019(3) 0.018(2) C24 0.072(4) 0.030(3) 0.081(5) 0.013(3) 0.016(4) -0.010(3) C25 0.025(2) 0.027(2) 0.027(2) 0.0054(17) 0.0055(17) 0.0008(17) C26 0.041(3) 0.039(3) 0.037(3) 0.014(2) 0.004(2) 0.006(2) C27 0.039(3) 0.027(2) 0.036(2) 0.0053(19) 0.013(2) 0.0089(19) C28 0.028(2) 0.038(3) 0.042(3) 0.015(2) 0.011(2) -0.0019(19) C29 0.032(2) 0.030(2) 0.026(2) 0.0059(17) 0.0089(18) 0.0100(18) C30 0.043(3) 0.034(3) 0.058(3) 0.013(2) 0.023(3) 0.003(2) C31 0.027(3) 0.049(3) 0.048(3) 0.005(2) 0.009(2) 0.012(2) C32 0.061(4) 0.044(3) 0.053(3) -0.009(3) 0.020(3) 0.018(3) C33 0.059(4) 0.035(3) 0.055(3) -0.002(2) 0.008(3) -0.004(3) C34 0.032(2) 0.027(2) 0.030(2) 0.0069(18) 0.0115(19) 0.0059(18) C35 0.048(3) 0.045(3) 0.041(3) -0.003(2) 0.003(2) -0.002(2) C36 0.063(4) 0.031(3) 0.046(3) 0.004(2) 0.025(3) 0.014(2) C37 0.041(3) 0.062(3) 0.030(2) 0.010(2) 0.011(2) 0.014(3) C38 0.029(3) 0.044(3) 0.047(3) 0.011(2) 0.014(2) 0.008(2) C39 0.059(4) 0.054(3) 0.060(4) 0.036(3) 0.015(3) 0.009(3) C40 0.075(5) 0.076(5) 0.110(6) 0.057(5) 0.026(4) 0.024(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O3 2.132(3) . ? La1 O1 2.309(3) . ? La1 O2 2.326(3) . ? La1 N1 2.620(4) . ? La1 N4 2.626(4) . ? N1 C29 1.300(6) . ? N1 H1 0.8800 . ? N2 C29 1.379(6) . ? N2 C33 1.447(7) . ? N2 C32 1.457(6) . ? N3 C29 1.359(6) . ? N3 C30 1.451(6) . ? N3 C31 1.459(6) . ? N4 C34 1.305(6) . ? N4 H4 0.8800 . ? N5 C34 1.378(6) . ? N5 C35 1.450(7) . ? N5 C36 1.458(6) . ? N6 C34 1.364(6) . ? N6 C37 1.457(6) . ? N6 C38 1.470(6) . ? O1 C4 1.334(5) . ? O2 C18 1.335(5) . ? O3 C39 1.401(6) . ? C1 C6 1.376(8) . ? C1 C2 1.385(7) . ? C1 H1A 0.9500 . ? C2 C3 1.398(6) . ? C2 H2 0.9500 . ? C3 C4 1.426(6) . ? C3 C7 1.535(6) . ? C4 C5 1.437(6) . ? C5 C6 1.396(7) . ? C5 C11 1.546(6) . ? C6 H6 0.9500 . ? C7 C10 1.536(6) . ? C7 C8 1.543(7) . ? C7 C9 1.548(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.530(6) . ? C11 C14 1.539(6) . ? C11 C13 1.540(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.375(8) . ? C15 C20 1.378(8) . ? C15 H15 0.9500 . ? C16 C17 1.392(7) . ? C16 H16 0.9500 . ? C17 C18 1.434(6) . ? C17 C21 1.548(7) . ? C18 C19 1.431(6) . ? C19 C20 1.398(6) . ? C19 C25 1.539(6) . ? C20 H20 0.9500 . ? C21 C22 1.527(7) . ? C21 C24 1.542(7) . ? C21 C23 1.545(7) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.528(6) . ? C25 C28 1.538(6) . ? C25 C26 1.542(6) . ? 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 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? 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 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? 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 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.482(9) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 La1 O1 104.86(11) . . ? O3 La1 O2 105.78(12) . . ? O1 La1 O2 149.33(10) . . ? O3 La1 N1 102.86(13) . . ? O1 La1 N1 76.35(11) . . ? O2 La1 N1 98.02(11) . . ? O3 La1 N4 98.84(13) . . ? O1 La1 N4 99.36(11) . . ? O2 La1 N4 74.62(11) . . ? N1 La1 N4 158.27(13) . . ? C29 N1 La1 152.5(3) . . ? C29 N1 H1 103.7 . . ? La1 N1 H1 103.7 . . ? C29 N2 C33 119.1(4) . . ? C29 N2 C32 121.6(4) . . ? C33 N2 C32 114.3(4) . . ? C29 N3 C30 118.3(4) . . ? C29 N3 C31 121.9(4) . . ? C30 N3 C31 114.9(4) . . ? C34 N4 La1 152.0(3) . . ? C34 N4 H4 104.0 . . ? La1 N4 H4 104.0 . . ? C34 N5 C35 119.1(4) . . ? C34 N5 C36 122.0(4) . . ? C35 N5 C36 114.5(4) . . ? C34 N6 C37 117.6(4) . . ? C34 N6 C38 120.3(4) . . ? C37 N6 C38 112.8(4) . . ? C4 O1 La1 168.9(2) . . ? C18 O2 La1 168.6(2) . . ? C39 O3 La1 175.6(4) . . ? C6 C1 C2 119.8(4) . . ? C6 C1 H1A 120.1 . . ? C2 C1 H1A 120.1 . . ? C1 C2 C3 121.4(4) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C2 C3 C4 119.0(4) . . ? C2 C3 C7 119.0(4) . . ? C4 C3 C7 121.9(4) . . ? O1 C4 C3 120.4(4) . . ? O1 C4 C5 120.5(4) . . ? C3 C4 C5 119.1(4) . . ? C6 C5 C4 118.4(4) . . ? C6 C5 C11 119.0(4) . . ? C4 C5 C11 122.7(4) . . ? C1 C6 C5 122.1(4) . . ? C1 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? C3 C7 C10 111.4(4) . . ? C3 C7 C8 112.9(4) . . ? C10 C7 C8 106.1(4) . . ? C3 C7 C9 109.4(4) . . ? C10 C7 C9 110.9(4) . . ? C8 C7 C9 106.0(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C14 107.1(4) . . ? C12 C11 C13 109.3(4) . . ? C14 C11 C13 106.6(4) . . ? C12 C11 C5 110.7(4) . . ? C14 C11 C5 111.9(4) . . ? C13 C11 C5 111.1(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 119.6(5) . . ? C16 C15 H15 120.2 . . ? C20 C15 H15 120.2 . . ? C15 C16 C17 122.9(4) . . ? C15 C16 H16 118.5 . . ? C17 C16 H16 118.5 . . ? C16 C17 C18 117.7(4) . . ? C16 C17 C21 120.1(4) . . ? C18 C17 C21 122.2(4) . . ? O2 C18 C19 120.2(4) . . ? O2 C18 C17 120.5(4) . . ? C19 C18 C17 119.4(4) . . ? C20 C19 C18 119.0(4) . . ? C20 C19 C25 119.4(4) . . ? C18 C19 C25 121.6(4) . . ? C15 C20 C19 121.3(5) . . ? C15 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C22 C21 C24 107.0(4) . . ? C22 C21 C23 110.0(5) . . ? C24 C21 C23 106.7(4) . . ? C22 C21 C17 111.2(4) . . ? C24 C21 C17 112.0(5) . . ? C23 C21 C17 109.8(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C28 111.7(4) . . ? C27 C25 C19 112.1(4) . . ? C28 C25 C19 108.7(4) . . ? C27 C25 C26 105.8(4) . . ? C28 C25 C26 106.2(4) . . ? C19 C25 C26 112.3(4) . . ? 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 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N1 C29 N3 120.4(4) . . ? N1 C29 N2 123.0(4) . . ? N3 C29 N2 116.5(4) . . ? N3 C30 H30A 109.5 . . ? N3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N3 C31 H31A 109.5 . . ? N3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N2 C32 H32A 109.5 . . ? N2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N2 C33 H33A 109.5 . . ? N2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N4 C34 N6 120.4(4) . . ? N4 C34 N5 123.7(4) . . ? N6 C34 N5 115.9(4) . . ? N5 C35 H35A 109.5 . . ? N5 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N5 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N5 C36 H36A 109.5 . . ? N5 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N5 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N6 C37 H37A 109.5 . . ? N6 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N6 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N6 C38 H38A 109.5 . . ? N6 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N6 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O3 C39 C40 111.8(5) . . ? O3 C39 H39A 109.3 . . ? C40 C39 H39A 109.3 . . ? O3 C39 H39B 109.3 . . ? C40 C39 H39B 109.3 . . ? H39A C39 H39B 107.9 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.109 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.098 #===END data_bob018 _database_code_depnum_ccdc_archive 'CCDC 722740' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Nd(OCH2CH2CH2CCH)(4MeDBP)2(H-TMG)2) (3)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H79 N6 Nd O3' _chemical_formula_weight 896.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.133(2) _cell_length_b 15.229(2) _cell_length_c 19.850(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.079(2) _cell_angle_gamma 90.00 _cell_volume 4864.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6506 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 29.86 _exptl_crystal_description irregular _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1900 _exptl_absorpt_coefficient_mu 1.109 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6654 _exptl_absorpt_correction_T_max 0.7690 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 38000 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.05 _reflns_number_total 8625 _reflns_number_gt 6858 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 8625 _refine_ls_number_parameters 518 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.0990 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 0.088 _refine_ls_shift/su_mean 0.001 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 Nd1 Nd 0.226416(11) 0.692125(12) 0.354217(10) 0.02230(9) Uani 1 1 d . . . O1 O 0.36417(16) 0.67889(17) 0.36978(15) 0.0295(6) Uani 1 1 d . . . O2 O 0.08911(15) 0.67191(17) 0.29379(14) 0.0239(6) Uani 1 1 d . . . O3 O 0.23291(17) 0.76229(19) 0.44743(14) 0.0357(7) Uani 1 1 d . . . N1 N 0.2526(2) 0.8017(2) 0.2688(2) 0.0358(8) Uani 1 1 d . . . H1 H 0.3047 0.7915 0.2731 0.043 Uiso 1 1 calc R . . N2 N 0.1577(2) 0.9071(2) 0.2081(2) 0.0396(9) Uani 1 1 d . . . N3 N 0.2801(2) 0.8925(2) 0.1833(2) 0.0425(9) Uani 1 1 d . . . N4 N 0.2086(2) 0.5320(2) 0.38216(18) 0.0321(7) Uani 1 1 d . . . H4 H 0.1582 0.5173 0.3543 0.038 Uiso 1 1 calc R . . N5 N 0.3101(2) 0.4688(2) 0.47880(19) 0.0414(9) Uani 1 1 d . . . N6 N 0.2081(3) 0.3786(2) 0.4016(2) 0.0450(9) Uani 1 1 d . . . C1 C 0.6504(3) 0.7457(4) 0.2948(4) 0.0670(16) Uani 1 1 d . . . H1A H 0.6948 0.7034 0.3172 0.101 Uiso 1 1 calc R . . H1B H 0.6704 0.8052 0.3101 0.101 Uiso 1 1 calc R . . H1C H 0.6338 0.7414 0.2425 0.101 Uiso 1 1 calc R . . C2 C 0.5761(3) 0.7257(3) 0.3175(3) 0.0430(11) Uani 1 1 d . . . C3 C 0.5248(3) 0.6557(3) 0.2890(3) 0.0409(10) Uani 1 1 d . . . H3 H 0.5375 0.6192 0.2554 0.049 Uiso 1 1 calc R . . C4 C 0.4548(2) 0.6353(3) 0.3069(2) 0.0311(9) Uani 1 1 d . . . C5 C 0.4350(2) 0.6912(2) 0.3562(2) 0.0278(8) Uani 1 1 d . . . C6 C 0.4902(2) 0.7609(3) 0.3899(2) 0.0309(9) Uani 1 1 d . . . C7 C 0.5582(3) 0.7759(3) 0.3691(3) 0.0379(10) Uani 1 1 d . . . H7 H 0.5946 0.8228 0.3911 0.046 Uiso 1 1 calc R . . C8 C 0.4062(4) 0.4908(3) 0.3352(3) 0.0617(15) Uani 1 1 d . . . H8A H 0.3840 0.5204 0.3686 0.092 Uiso 1 1 calc R . . H8B H 0.4639 0.4731 0.3607 0.092 Uiso 1 1 calc R . . H8C H 0.3727 0.4387 0.3153 0.092 Uiso 1 1 calc R . . C9 C 0.4035(3) 0.5528(3) 0.2750(3) 0.0406(11) Uani 1 1 d . . . C10 C 0.4370(3) 0.5024(4) 0.2239(3) 0.0696(17) Uani 1 1 d . . . H10A H 0.4945 0.4843 0.2496 0.104 Uiso 1 1 calc R . . H10B H 0.4353 0.5403 0.1835 0.104 Uiso 1 1 calc R . . H10C H 0.4027 0.4502 0.2059 0.104 Uiso 1 1 calc R . . C11 C 0.3141(3) 0.5744(4) 0.2307(4) 0.0748(19) Uani 1 1 d . . . H11A H 0.2864 0.5216 0.2055 0.112 Uiso 1 1 calc R . . H11B H 0.3131 0.6201 0.1957 0.112 Uiso 1 1 calc R . . H11C H 0.2850 0.5955 0.2623 0.112 Uiso 1 1 calc R . . C12 C 0.4776(3) 0.8199(3) 0.4489(3) 0.0377(10) Uani 1 1 d . . . C13 C 0.5558(3) 0.8752(4) 0.4865(3) 0.0589(15) Uani 1 1 d . . . H13A H 0.5640 0.9176 0.4524 0.088 Uiso 1 1 calc R . . H13B H 0.6043 0.8365 0.5039 0.088 Uiso 1 1 calc R . . H13C H 0.5487 0.9067 0.5271 0.088 Uiso 1 1 calc R . . C14 C 0.4596(3) 0.7659(3) 0.5071(2) 0.0464(11) Uani 1 1 d . . . H14A H 0.4555 0.8053 0.5448 0.070 Uiso 1 1 calc R . . H14B H 0.5048 0.7238 0.5279 0.070 Uiso 1 1 calc R . . H14C H 0.4071 0.7341 0.4859 0.070 Uiso 1 1 calc R . . C15 C 0.4064(3) 0.8848(3) 0.4163(3) 0.0502(12) Uani 1 1 d . . . H15A H 0.4016 0.9239 0.4539 0.075 Uiso 1 1 calc R . . H15B H 0.3543 0.8524 0.3949 0.075 Uiso 1 1 calc R . . H15C H 0.4177 0.9197 0.3792 0.075 Uiso 1 1 calc R . . C16 C -0.2561(3) 0.5989(4) 0.1586(3) 0.0537(14) Uani 1 1 d . . . H16A H -0.2682 0.5423 0.1764 0.081 Uiso 1 1 calc R . . H16B H -0.2694 0.5955 0.1065 0.081 Uiso 1 1 calc R . . H16C H -0.2897 0.6449 0.1697 0.081 Uiso 1 1 calc R . . C17 C -0.1645(2) 0.6204(3) 0.1943(2) 0.0335(9) Uani 1 1 d . . . C18 C -0.1329(2) 0.6497(3) 0.2644(2) 0.0319(9) Uani 1 1 d . . . H18 H -0.1703 0.6577 0.2898 0.038 Uiso 1 1 calc R . . C19 C -0.0487(2) 0.6684(2) 0.2998(2) 0.0254(8) Uani 1 1 d . . . C20 C 0.0080(2) 0.6559(2) 0.26222(18) 0.0204(7) Uani 1 1 d . . . C21 C -0.0239(2) 0.6259(2) 0.18929(19) 0.0234(8) Uani 1 1 d . . . C22 C -0.1092(2) 0.6098(3) 0.1585(2) 0.0278(8) Uani 1 1 d . . . H22 H -0.1301 0.5905 0.1100 0.033 Uiso 1 1 calc R . . C23 C 0.0331(2) 0.6110(3) 0.1445(2) 0.0284(8) Uani 1 1 d . . . C24 C -0.0148(3) 0.5795(3) 0.0678(2) 0.0432(11) Uani 1 1 d . . . H24A H -0.0420 0.5234 0.0697 0.065 Uiso 1 1 calc R . . H24B H 0.0239 0.5718 0.0416 0.065 Uiso 1 1 calc R . . H24C H -0.0569 0.6233 0.0431 0.065 Uiso 1 1 calc R . . C25 C 0.0973(3) 0.5392(3) 0.1797(3) 0.0429(11) Uani 1 1 d . . . H25A H 0.1332 0.5590 0.2272 0.064 Uiso 1 1 calc R . . H25B H 0.1312 0.5276 0.1497 0.064 Uiso 1 1 calc R . . H25C H 0.0685 0.4853 0.1846 0.064 Uiso 1 1 calc R . . C26 C 0.0762(3) 0.6965(3) 0.1370(2) 0.0419(11) Uani 1 1 d . . . H26A H 0.0343 0.7405 0.1126 0.063 Uiso 1 1 calc R . . H26B H 0.1124 0.6856 0.1089 0.063 Uiso 1 1 calc R . . H26C H 0.1096 0.7181 0.1847 0.063 Uiso 1 1 calc R . . C27 C -0.0201(3) 0.7043(3) 0.3773(2) 0.0304(9) Uani 1 1 d . . . C28 C -0.0925(3) 0.7132(4) 0.4060(3) 0.0535(14) Uani 1 1 d . . . H28A H -0.0722 0.7393 0.4541 0.080 Uiso 1 1 calc R . . H28B H -0.1159 0.6551 0.4084 0.080 Uiso 1 1 calc R . . H28C H -0.1356 0.7510 0.3739 0.080 Uiso 1 1 calc R . . C29 C 0.0166(3) 0.7964(3) 0.3795(3) 0.0401(11) Uani 1 1 d . . . H29A H 0.0295 0.8212 0.4276 0.060 Uiso 1 1 calc R . . H29B H -0.0239 0.8341 0.3445 0.060 Uiso 1 1 calc R . . H29C H 0.0675 0.7929 0.3676 0.060 Uiso 1 1 calc R . . C30 C 0.0444(3) 0.6438(3) 0.4296(2) 0.0395(10) Uani 1 1 d . . . H30A H 0.0921 0.6367 0.4135 0.059 Uiso 1 1 calc R . . H30B H 0.0193 0.5864 0.4310 0.059 Uiso 1 1 calc R . . H30C H 0.0630 0.6699 0.4777 0.059 Uiso 1 1 calc R . . C31 C 0.2317(3) 0.8645(3) 0.2222(2) 0.0327(9) Uani 1 1 d . . . C32 C 0.1128(3) 0.8977(3) 0.2579(3) 0.0466(12) Uani 1 1 d . . . H32A H 0.0793 0.8439 0.2467 0.070 Uiso 1 1 calc R . . H32B H 0.0763 0.9485 0.2536 0.070 Uiso 1 1 calc R . . H32C H 0.1525 0.8942 0.3070 0.070 Uiso 1 1 calc R . . C33 C 0.1088(3) 0.9358(3) 0.1370(3) 0.0614(15) Uani 1 1 d . . . H33A H 0.1380 0.9215 0.1037 0.092 Uiso 1 1 calc R . . H33B H 0.1002 0.9994 0.1372 0.092 Uiso 1 1 calc R . . H33C H 0.0548 0.9059 0.1216 0.092 Uiso 1 1 calc R . . C34 C 0.2893(4) 0.9877(3) 0.1745(4) 0.0707(17) Uani 1 1 d . . . H34A H 0.2466 1.0193 0.1874 0.106 Uiso 1 1 calc R . . H34B H 0.2828 1.0003 0.1245 0.106 Uiso 1 1 calc R . . H34C H 0.3445 1.0066 0.2059 0.106 Uiso 1 1 calc R . . C35 C 0.3539(3) 0.8402(3) 0.1886(3) 0.0544(13) Uani 1 1 d . . . H35A H 0.3984 0.8536 0.2339 0.082 Uiso 1 1 calc R . . H35B H 0.3724 0.8545 0.1484 0.082 Uiso 1 1 calc R . . H35C H 0.3401 0.7776 0.1871 0.082 Uiso 1 1 calc R . . C36 C 0.2404(3) 0.4617(3) 0.4192(2) 0.0329(9) Uani 1 1 d . . . C37 C 0.1462(4) 0.3650(3) 0.3331(3) 0.0654(16) Uani 1 1 d . . . H37A H 0.0953 0.3960 0.3309 0.098 Uiso 1 1 calc R . . H37B H 0.1346 0.3021 0.3256 0.098 Uiso 1 1 calc R . . H37C H 0.1662 0.3877 0.2957 0.098 Uiso 1 1 calc R . . C38 C 0.2019(5) 0.3194(4) 0.4572(4) 0.079(2) Uani 1 1 d . . . H38A H 0.2417 0.3373 0.5037 0.119 Uiso 1 1 calc R . . H38B H 0.2143 0.2593 0.4463 0.119 Uiso 1 1 calc R . . H38C H 0.1454 0.3218 0.4589 0.119 Uiso 1 1 calc R . . C39 C 0.3400(3) 0.5562(3) 0.5055(2) 0.0516(13) Uani 1 1 d . . . H39A H 0.3661 0.5834 0.4738 0.077 Uiso 1 1 calc R . . H39B H 0.3809 0.5515 0.5541 0.077 Uiso 1 1 calc R . . H39C H 0.2932 0.5925 0.5066 0.077 Uiso 1 1 calc R . . C40 C 0.3754(4) 0.4015(4) 0.4992(3) 0.0658(16) Uani 1 1 d . . . H40A H 0.3553 0.3483 0.4706 0.099 Uiso 1 1 calc R . . H40B H 0.3898 0.3875 0.5503 0.099 Uiso 1 1 calc R . . H40C H 0.4248 0.4236 0.4904 0.099 Uiso 1 1 calc R . . C41 C 0.2387(4) 0.7923(5) 0.5141(3) 0.0722(19) Uani 1 1 d . . . H41A H 0.2963 0.7813 0.5464 0.087 Uiso 1 1 calc R . . H41B H 0.2022 0.7546 0.5312 0.087 Uiso 1 1 calc R . . C42 C 0.2199(7) 0.8790(9) 0.5246(6) 0.160(6) Uani 1 1 d . . . H42A H 0.1590 0.8864 0.5023 0.192 Uiso 1 1 calc R . . H42B H 0.2340 0.8880 0.5768 0.192 Uiso 1 1 calc R . . C43 C 0.2501(10) 0.9331(7) 0.5041(7) 0.202(8) Uani 1 1 d . . . H43A H 0.2253 0.9344 0.4511 0.242 Uiso 1 1 calc R . . H43B H 0.3099 0.9190 0.5165 0.242 Uiso 1 1 calc R . . C44 C 0.2424(6) 1.0272(7) 0.5335(5) 0.122(3) Uani 1 1 d . . . C45 C 0.2335(6) 1.1010(7) 0.5558(6) 0.139(4) Uani 1 1 d . . . H45 H 0.2267 1.1577 0.5730 0.167 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.01926(13) 0.02087(13) 0.02618(14) -0.00137(8) 0.00704(9) 0.00032(8) O1 0.0193(13) 0.0302(15) 0.0387(16) -0.0067(12) 0.0097(12) -0.0002(11) O2 0.0203(13) 0.0273(14) 0.0241(13) -0.0033(11) 0.0075(11) -0.0009(10) O3 0.0358(15) 0.0387(17) 0.0327(16) -0.0100(13) 0.0120(13) 0.0009(13) N1 0.0304(19) 0.036(2) 0.039(2) 0.0048(16) 0.0093(16) -0.0067(15) N2 0.046(2) 0.031(2) 0.042(2) 0.0049(16) 0.0150(17) 0.0031(16) N3 0.054(2) 0.0295(19) 0.052(2) 0.0072(17) 0.0288(19) 0.0003(17) N4 0.0302(17) 0.0271(18) 0.0384(19) 0.0013(15) 0.0112(15) 0.0013(14) N5 0.050(2) 0.0296(19) 0.038(2) 0.0070(16) 0.0064(17) 0.0048(17) N6 0.060(2) 0.0252(19) 0.049(2) 0.0065(17) 0.017(2) -0.0033(18) C1 0.053(3) 0.057(3) 0.111(5) -0.006(3) 0.054(3) -0.007(3) C2 0.033(2) 0.037(2) 0.065(3) 0.004(2) 0.025(2) 0.004(2) C3 0.038(2) 0.036(2) 0.054(3) -0.004(2) 0.023(2) 0.009(2) C4 0.0230(19) 0.027(2) 0.043(2) -0.0019(17) 0.0106(17) 0.0043(16) C5 0.0211(19) 0.027(2) 0.032(2) 0.0025(16) 0.0053(16) 0.0041(15) C6 0.0239(19) 0.023(2) 0.042(2) 0.0004(17) 0.0059(17) 0.0051(16) C7 0.029(2) 0.023(2) 0.061(3) 0.000(2) 0.015(2) -0.0024(17) C8 0.085(4) 0.031(3) 0.079(4) -0.013(3) 0.040(3) -0.019(3) C9 0.032(2) 0.036(2) 0.056(3) -0.021(2) 0.017(2) -0.0017(18) C10 0.062(3) 0.064(4) 0.093(4) -0.043(3) 0.040(3) -0.008(3) C11 0.043(3) 0.070(4) 0.092(4) -0.042(4) -0.001(3) 0.005(3) C12 0.028(2) 0.032(2) 0.049(3) -0.0123(19) 0.0073(19) -0.0037(17) C13 0.038(3) 0.058(3) 0.075(4) -0.034(3) 0.012(2) -0.015(2) C14 0.048(3) 0.048(3) 0.040(3) -0.012(2) 0.010(2) 0.003(2) C15 0.043(3) 0.033(2) 0.071(3) -0.015(2) 0.015(2) 0.004(2) C16 0.023(2) 0.089(4) 0.044(3) -0.011(3) 0.0055(19) -0.009(2) C17 0.0237(19) 0.043(2) 0.030(2) -0.0021(18) 0.0045(17) 0.0015(18) C18 0.0227(19) 0.040(2) 0.033(2) 0.0000(18) 0.0103(17) 0.0027(17) C19 0.0263(19) 0.0242(19) 0.025(2) -0.0012(15) 0.0079(16) 0.0009(15) C20 0.0215(17) 0.0146(17) 0.0247(19) 0.0000(14) 0.0075(15) -0.0022(14) C21 0.0273(19) 0.0189(18) 0.0256(19) 0.0012(15) 0.0112(15) -0.0015(15) C22 0.0257(19) 0.029(2) 0.0250(19) -0.0011(16) 0.0039(15) 0.0004(16) C23 0.033(2) 0.029(2) 0.027(2) -0.0069(16) 0.0141(17) -0.0057(17) C24 0.044(2) 0.055(3) 0.034(2) -0.019(2) 0.018(2) -0.015(2) C25 0.039(2) 0.040(3) 0.052(3) -0.014(2) 0.019(2) 0.006(2) C26 0.053(3) 0.043(3) 0.037(2) -0.0068(19) 0.025(2) -0.018(2) C27 0.031(2) 0.036(2) 0.028(2) -0.0094(17) 0.0151(17) -0.0046(17) C28 0.044(3) 0.078(4) 0.048(3) -0.028(3) 0.027(2) -0.011(3) C29 0.042(3) 0.035(2) 0.042(3) -0.0148(19) 0.013(2) -0.0018(19) C30 0.045(2) 0.046(3) 0.025(2) -0.0026(19) 0.0081(18) -0.010(2) C31 0.038(2) 0.027(2) 0.032(2) -0.0045(17) 0.0117(18) -0.0088(18) C32 0.052(3) 0.029(2) 0.064(3) -0.003(2) 0.025(2) 0.002(2) C33 0.071(4) 0.041(3) 0.066(4) 0.018(3) 0.014(3) 0.013(3) C34 0.097(5) 0.036(3) 0.104(5) 0.010(3) 0.067(4) -0.008(3) C35 0.064(3) 0.047(3) 0.066(3) 0.015(3) 0.040(3) 0.003(3) C36 0.040(2) 0.025(2) 0.040(2) 0.0042(18) 0.0216(19) 0.0055(18) C37 0.074(4) 0.037(3) 0.072(4) 0.000(3) 0.009(3) -0.011(3) C38 0.113(6) 0.047(3) 0.082(5) 0.017(3) 0.038(4) -0.017(3) C39 0.066(3) 0.045(3) 0.033(2) -0.001(2) 0.003(2) -0.001(2) C40 0.067(4) 0.049(3) 0.070(4) 0.016(3) 0.010(3) 0.023(3) C41 0.059(4) 0.114(5) 0.041(3) -0.037(3) 0.014(3) -0.001(3) C42 0.168(10) 0.196(13) 0.139(10) -0.117(10) 0.084(8) -0.092(10) C43 0.39(2) 0.112(8) 0.205(12) 0.074(8) 0.238(15) 0.122(12) C44 0.143(8) 0.125(8) 0.094(6) -0.002(6) 0.036(6) 0.040(7) C45 0.129(8) 0.129(9) 0.138(9) -0.038(7) 0.020(6) 0.028(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O3 2.106(3) . ? Nd1 O2 2.265(2) . ? Nd1 O1 2.282(3) . ? Nd1 N1 2.527(3) . ? Nd1 N4 2.542(3) . ? O1 C5 1.343(5) . ? O2 C20 1.336(4) . ? O3 C41 1.371(6) . ? N1 C31 1.291(5) . ? N1 H1 0.8800 . ? N2 C31 1.365(5) . ? N2 C33 1.440(6) . ? N2 C32 1.454(6) . ? N3 C31 1.382(5) . ? N3 C35 1.467(6) . ? N3 C34 1.474(6) . ? N4 C36 1.307(5) . ? N4 H4 0.8800 . ? N5 C36 1.366(5) . ? N5 C39 1.459(6) . ? N5 C40 1.469(6) . ? N6 C36 1.378(5) . ? N6 C37 1.423(6) . ? N6 C38 1.457(7) . ? C1 C2 1.518(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.374(7) . ? C2 C7 1.395(6) . ? C3 C4 1.397(6) . ? C3 H3 0.9500 . ? C4 C5 1.423(6) . ? C4 C9 1.540(6) . ? C5 C6 1.427(5) . ? C6 C7 1.382(6) . ? C6 C12 1.549(6) . ? C7 H7 0.9500 . ? C8 C9 1.510(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.517(7) . ? C9 C10 1.533(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C15 1.530(6) . ? C12 C14 1.534(7) . ? C12 C13 1.540(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.520(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C22 1.376(5) . ? C17 C18 1.381(6) . ? C18 C19 1.400(5) . ? C18 H18 0.9500 . ? C19 C20 1.426(5) . ? C19 C27 1.547(5) . ? C20 C21 1.435(5) . ? C21 C22 1.398(5) . ? C21 C23 1.546(5) . ? C22 H22 0.9500 . ? C23 C26 1.530(5) . ? C23 C24 1.537(5) . ? C23 C25 1.539(6) . ? 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 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.531(6) . ? C27 C30 1.535(6) . ? C27 C28 1.539(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? 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 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? 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 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.392(13) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.121(14) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.569(14) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.238(12) . ? C45 H45 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Nd1 O2 105.44(10) . . ? O3 Nd1 O1 100.70(10) . . ? O2 Nd1 O1 153.86(10) . . ? O3 Nd1 N1 106.66(12) . . ? O2 Nd1 N1 97.23(10) . . ? O1 Nd1 N1 74.65(11) . . ? O3 Nd1 N4 105.60(11) . . ? O2 Nd1 N4 78.73(10) . . ? O1 Nd1 N4 94.69(10) . . ? N1 Nd1 N4 147.37(11) . . ? C5 O1 Nd1 157.5(3) . . ? C20 O2 Nd1 175.6(2) . . ? C41 O3 Nd1 168.9(4) . . ? C31 N1 Nd1 154.0(3) . . ? C31 N1 H1 103.0 . . ? Nd1 N1 H1 103.0 . . ? C31 N2 C33 122.2(4) . . ? C31 N2 C32 119.0(4) . . ? C33 N2 C32 115.6(4) . . ? C31 N3 C35 117.4(4) . . ? C31 N3 C34 118.6(4) . . ? C35 N3 C34 114.7(4) . . ? C36 N4 Nd1 148.2(3) . . ? C36 N4 H4 105.9 . . ? Nd1 N4 H4 105.9 . . ? C36 N5 C39 118.7(4) . . ? C36 N5 C40 122.7(4) . . ? C39 N5 C40 113.4(4) . . ? C36 N6 C37 118.6(4) . . ? C36 N6 C38 120.2(4) . . ? C37 N6 C38 114.2(5) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 117.1(4) . . ? C3 C2 C1 121.2(4) . . ? C7 C2 C1 121.7(4) . . ? C2 C3 C4 123.5(4) . . ? C2 C3 H3 118.2 . . ? C4 C3 H3 118.2 . . ? C3 C4 C5 118.1(4) . . ? C3 C4 C9 119.7(4) . . ? C5 C4 C9 122.2(3) . . ? O1 C5 C4 120.0(3) . . ? O1 C5 C6 120.6(4) . . ? C4 C5 C6 119.4(4) . . ? C7 C6 C5 118.3(4) . . ? C7 C6 C12 118.7(4) . . ? C5 C6 C12 122.9(4) . . ? C6 C7 C2 123.3(4) . . ? C6 C7 H7 118.3 . . ? C2 C7 H7 118.3 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C8 C9 C11 110.2(5) . . ? C8 C9 C10 107.0(4) . . ? C11 C9 C10 104.9(4) . . ? C8 C9 C4 109.1(4) . . ? C11 C9 C4 112.4(4) . . ? C10 C9 C4 113.0(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C15 C12 C14 109.1(4) . . ? C15 C12 C13 106.7(4) . . ? C14 C12 C13 107.1(4) . . ? C15 C12 C6 110.7(4) . . ? C14 C12 C6 112.0(3) . . ? C13 C12 C6 111.1(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C17 C18 117.3(4) . . ? C22 C17 C16 121.1(4) . . ? C18 C17 C16 121.6(4) . . ? C17 C18 C19 123.4(4) . . ? C17 C18 H18 118.3 . . ? C19 C18 H18 118.3 . . ? C18 C19 C20 118.7(3) . . ? C18 C19 C27 119.4(3) . . ? C20 C19 C27 121.8(3) . . ? O2 C20 C19 121.1(3) . . ? O2 C20 C21 120.4(3) . . ? C19 C20 C21 118.5(3) . . ? C22 C21 C20 118.4(3) . . ? C22 C21 C23 119.6(3) . . ? C20 C21 C23 122.0(3) . . ? C17 C22 C21 123.7(4) . . ? C17 C22 H22 118.2 . . ? C21 C22 H22 118.2 . . ? C26 C23 C24 106.3(3) . . ? C26 C23 C25 110.7(3) . . ? C24 C23 C25 106.5(3) . . ? C26 C23 C21 110.7(3) . . ? C24 C23 C21 112.8(3) . . ? C25 C23 C21 109.7(3) . . ? 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 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C30 109.7(3) . . ? C29 C27 C28 106.5(4) . . ? C30 C27 C28 106.7(4) . . ? C29 C27 C19 109.8(3) . . ? C30 C27 C19 111.7(3) . . ? C28 C27 C19 112.3(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N1 C31 N2 120.6(4) . . ? N1 C31 N3 123.8(4) . . ? N2 C31 N3 115.6(4) . . ? N2 C32 H32A 109.5 . . ? N2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N2 C33 H33A 109.5 . . ? N2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N3 C34 H34A 109.5 . . ? N3 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N3 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N3 C35 H35A 109.5 . . ? N3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N4 C36 N5 119.6(4) . . ? N4 C36 N6 123.8(4) . . ? N5 C36 N6 116.6(4) . . ? N6 C37 H37A 109.5 . . ? N6 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N6 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N6 C38 H38A 109.5 . . ? N6 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N6 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N5 C39 H39A 109.5 . . ? N5 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N5 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N5 C40 H40A 109.5 . . ? N5 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N5 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O3 C41 C42 121.1(7) . . ? O3 C41 H41A 107.1 . . ? C42 C41 H41A 107.1 . . ? O3 C41 H41B 107.1 . . ? C42 C41 H41B 107.1 . . ? H41A C41 H41B 106.8 . . ? C43 C42 C41 118.9(11) . . ? C43 C42 H42A 107.6 . . ? C41 C42 H42A 107.6 . . ? C43 C42 H42B 107.6 . . ? C41 C42 H42B 107.6 . . ? H42A C42 H42B 107.0 . . ? C42 C43 C44 115.2(10) . . ? C42 C43 H43A 108.5 . . ? C44 C43 H43A 108.5 . . ? C42 C43 H43B 108.5 . . ? C44 C43 H43B 108.5 . . ? H43A C43 H43B 107.5 . . ? C45 C44 C43 177.9(13) . . ? C44 C45 H45 180.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.764 _refine_diff_density_min -0.828 _refine_diff_density_rms 0.081 #===END data_try1 _database_code_depnum_ccdc_archive 'CCDC 722741' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(La((OCH2CH2CH2CCH))(4MeDBP)2(H-TMG)2) (4)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H72 La N6 O3' _chemical_formula_weight 859.98 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' La La -0.2871 2.4523 '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' _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 10.108(3) _cell_length_b 13.612(4) _cell_length_c 17.232(5) _cell_angle_alpha 86.866(5) _cell_angle_beta 87.732(5) _cell_angle_gamma 76.967(5) _cell_volume 2305.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 3428 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 906 _exptl_absorpt_coefficient_mu 0.968 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7601 _exptl_absorpt_correction_T_max 0.8684 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(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 18383 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0838 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 25.05 _reflns_number_total 8103 _reflns_number_gt 6616 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. N6, C42 and C43 were disordered and were modeled in two positions. ; _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^)+(0.1000P)^2^+0.0146P] 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 8103 _refine_ls_number_parameters 526 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1056 _refine_ls_R_factor_gt 0.0871 _refine_ls_wR_factor_ref 0.2578 _refine_ls_wR_factor_gt 0.2487 _refine_ls_goodness_of_fit_ref 1.659 _refine_ls_restrained_S_all 1.659 _refine_ls_shift/su_max 0.924 _refine_ls_shift/su_mean 0.009 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.62158(6) 0.21442(4) 0.23808(3) 0.0270(2) Uani 1 1 d . . 1 O1 O 0.7061(6) 0.0404(5) 0.2434(4) 0.0286(15) Uani 1 1 d . . 1 O2 O 0.4277(7) 0.3310(5) 0.2032(4) 0.0325(16) Uani 1 1 d . . 1 O3 O 0.7654(8) 0.2925(6) 0.2797(5) 0.051(2) Uani 1 1 d . . 1 N1 N 0.7411(9) 0.1861(7) 0.1008(5) 0.035(2) Uani 1 1 d . . 1 H1 H 0.7882 0.1250 0.1019 0.042 Uiso 1 1 calc R . 1 N2 N 0.8023(9) 0.1702(6) -0.0335(5) 0.0330(19) Uani 1 1 d . . 1 N3 N 0.7391(9) 0.3288(6) 0.0207(5) 0.037(2) Uani 1 1 d . . 1 N4 N 0.5230(10) 0.1708(8) 0.3743(5) 0.055(3) Uani 1 1 d . . 1 H4 H 0.5560 0.1069 0.3797 0.066 Uiso 1 1 calc R . 1 N5 N 0.5007(19) 0.218(2) 0.5000(11) 0.225(17) Uani 1 1 d . . 1 N6A N 0.310(4) 0.202(3) 0.424(3) 0.11(2) Uani 0.63(6) 1 d P . 1 N6B N 0.355(3) 0.153(2) 0.4755(19) 0.044(11) Uani 0.37(6) 1 d P . 2 C1 C 0.8590(13) -0.2665(8) 0.2869(7) 0.049(3) Uani 1 1 d . . 1 H1A H 0.8912 -0.3347 0.2998 0.059 Uiso 1 1 calc R . 1 C2 C 0.9324(11) -0.1976(8) 0.3050(7) 0.043(3) Uani 1 1 d . . 1 H2 H 1.0172 -0.2213 0.3267 0.051 Uiso 1 1 calc R . 1 C3 C 0.8849(10) -0.0933(8) 0.2922(6) 0.031(2) Uani 1 1 d . . 1 C4 C 0.7577(9) -0.0585(7) 0.2557(6) 0.029(2) Uani 1 1 d . . 1 C5 C 0.6838(10) -0.1305(7) 0.2338(6) 0.030(2) Uani 1 1 d . . 1 C6 C 0.7372(11) -0.2341(8) 0.2495(7) 0.042(3) Uani 1 1 d . . 1 H6 H 0.6903 -0.2811 0.2346 0.051 Uiso 1 1 calc R . 1 C7 C 0.9706(10) -0.0196(9) 0.3150(6) 0.038(3) Uani 1 1 d . . 1 C8 C 1.1074(12) -0.0753(11) 0.3499(9) 0.065(4) Uani 1 1 d . . 1 H8A H 1.1532 -0.0269 0.3683 0.098 Uiso 1 1 calc R . 1 H8B H 1.1631 -0.1135 0.3107 0.098 Uiso 1 1 calc R . 1 H8C H 1.0908 -0.1200 0.3924 0.098 Uiso 1 1 calc R . 1 C9 C 1.0044(11) 0.0447(9) 0.2448(7) 0.045(3) Uani 1 1 d . . 1 H9A H 0.9222 0.0876 0.2256 0.068 Uiso 1 1 calc R . 1 H9B H 1.0479 0.0015 0.2047 0.068 Uiso 1 1 calc R . 1 H9C H 1.0642 0.0855 0.2599 0.068 Uiso 1 1 calc R . 1 C10 C 0.8954(12) 0.0465(9) 0.3788(6) 0.044(3) Uani 1 1 d . . 1 H10A H 0.9462 0.0951 0.3909 0.067 Uiso 1 1 calc R . 1 H10B H 0.8852 0.0049 0.4245 0.067 Uiso 1 1 calc R . 1 H10C H 0.8073 0.0810 0.3612 0.067 Uiso 1 1 calc R . 1 C11 C 0.5470(11) -0.0986(8) 0.1928(6) 0.034(2) Uani 1 1 d . . 1 C12 C 0.5653(13) -0.0397(9) 0.1162(6) 0.045(3) Uani 1 1 d . . 1 H12A H 0.4785 -0.0147 0.0931 0.067 Uiso 1 1 calc R . 1 H12B H 0.6240 -0.0835 0.0812 0.067 Uiso 1 1 calc R . 1 H12C H 0.6049 0.0160 0.1262 0.067 Uiso 1 1 calc R . 1 C13 C 0.4870(13) -0.1889(9) 0.1719(8) 0.053(3) Uani 1 1 d . . 1 H13A H 0.4579 -0.2205 0.2186 0.080 Uiso 1 1 calc R . 1 H13B H 0.5553 -0.2370 0.1451 0.080 Uiso 1 1 calc R . 1 H13C H 0.4109 -0.1650 0.1389 0.080 Uiso 1 1 calc R . 1 C14 C 0.4395(9) -0.0349(7) 0.2447(6) 0.029(2) Uani 1 1 d . . 1 H14A H 0.4154 -0.0766 0.2873 0.043 Uiso 1 1 calc R . 1 H14B H 0.3605 -0.0062 0.2151 0.043 Uiso 1 1 calc R . 1 H14C H 0.4749 0.0183 0.2645 0.043 Uiso 1 1 calc R . 1 C15 C 0.0574(12) 0.5311(9) 0.1608(8) 0.050(3) Uani 1 1 d . . 1 H15 H -0.0255 0.5755 0.1516 0.061 Uiso 1 1 calc R . 1 C16 C 0.0960(11) 0.4436(9) 0.1210(7) 0.043(3) Uani 1 1 d . . 1 H16 H 0.0367 0.4293 0.0855 0.051 Uiso 1 1 calc R . 1 C17 C 0.2205(10) 0.3754(8) 0.1317(6) 0.035(2) Uani 1 1 d . . 1 C18 C 0.3107(9) 0.3973(7) 0.1897(6) 0.029(2) Uani 1 1 d . . 1 C19 C 0.2711(10) 0.4892(8) 0.2305(5) 0.032(2) Uani 1 1 d . . 1 C20 C 0.1436(11) 0.5512(9) 0.2141(6) 0.042(3) Uani 1 1 d . . 1 H20 H 0.1157 0.6099 0.2412 0.050 Uiso 1 1 calc R . 1 C21 C 0.2583(12) 0.2819(9) 0.0852(8) 0.048(3) Uani 1 1 d . . 1 C22 C 0.1512(14) 0.2753(12) 0.0273(9) 0.070(4) Uani 1 1 d . . 1 H22A H 0.0715 0.2632 0.0548 0.106 Uiso 1 1 calc R . 1 H22B H 0.1864 0.2208 -0.0063 0.106 Uiso 1 1 calc R . 1 H22C H 0.1281 0.3375 -0.0033 0.106 Uiso 1 1 calc R . 1 C23 C 0.3893(12) 0.2799(11) 0.0374(7) 0.055(3) Uani 1 1 d . . 1 H23A H 0.3755 0.3362 0.0003 0.083 Uiso 1 1 calc R . 1 H23B H 0.4140 0.2181 0.0106 0.083 Uiso 1 1 calc R . 1 H23C H 0.4607 0.2840 0.0713 0.083 Uiso 1 1 calc R . 1 C24 C 0.2703(15) 0.1874(10) 0.1406(9) 0.066(4) Uani 1 1 d . . 1 H24A H 0.3509 0.1786 0.1702 0.099 Uiso 1 1 calc R . 1 H24B H 0.2754 0.1291 0.1107 0.099 Uiso 1 1 calc R . 1 H24C H 0.1922 0.1959 0.1751 0.099 Uiso 1 1 calc R . 1 C25 C 0.3657(11) 0.5186(8) 0.2880(6) 0.037(2) Uani 1 1 d . . 1 C26 C 0.5015(11) 0.5247(9) 0.2489(7) 0.045(3) Uani 1 1 d . . 1 H26A H 0.5483 0.4589 0.2337 0.068 Uiso 1 1 calc R . 1 H26B H 0.5556 0.5493 0.2847 0.068 Uiso 1 1 calc R . 1 H26C H 0.4863 0.5700 0.2038 0.068 Uiso 1 1 calc R . 1 C27 C 0.3873(15) 0.4433(9) 0.3589(7) 0.054(3) Uani 1 1 d . . 1 H27A H 0.4406 0.3794 0.3432 0.082 Uiso 1 1 calc R . 1 H27B H 0.3008 0.4348 0.3796 0.082 Uiso 1 1 calc R . 1 H27C H 0.4340 0.4687 0.3980 0.082 Uiso 1 1 calc R . 1 C28 C 0.3036(15) 0.6241(10) 0.3212(8) 0.064(4) Uani 1 1 d . . 1 H28A H 0.3582 0.6356 0.3627 0.096 Uiso 1 1 calc R . 1 H28B H 0.2128 0.6259 0.3406 0.096 Uiso 1 1 calc R . 1 H28C H 0.3017 0.6757 0.2808 0.096 Uiso 1 1 calc R . 1 C29 C 0.8837(18) 0.3207(15) 0.3021(13) 0.101(6) Uani 1 1 d . . 1 H29A H 0.9471 0.3150 0.2580 0.121 Uiso 1 1 calc R . 1 H29B H 0.9257 0.2733 0.3429 0.121 Uiso 1 1 calc R . 1 C30 C 0.862(2) 0.4202(16) 0.3292(16) 0.117(8) Uani 1 1 d . . 1 H30A H 0.8849 0.4638 0.2867 0.141 Uiso 1 1 calc R . 1 H30B H 0.7661 0.4433 0.3413 0.141 Uiso 1 1 calc R . 1 C31 C 0.921(12) 0.432(4) 0.383(3) 0.72(11) Uani 1 1 d . . 1 H31A H 0.8653 0.4939 0.4017 0.861 Uiso 1 1 calc R . 1 H31B H 1.0001 0.4517 0.3583 0.861 Uiso 1 1 calc R . 1 C32 C 0.976(9) 0.382(4) 0.452(2) 0.43(5) Uani 1 1 d . . 1 C33 C 1.025(6) 0.333(6) 0.509(2) 0.47(6) Uani 1 1 d . . 1 H33 H 1.0627 0.2957 0.5524 0.561 Uiso 1 1 calc R . 1 C34 C 0.7599(10) 0.2250(7) 0.0314(5) 0.028(2) Uani 1 1 d . . 1 C35 C 0.8952(11) 0.1995(8) -0.0923(6) 0.041(3) Uani 1 1 d . . 1 H35A H 0.9182 0.2608 -0.0784 0.061 Uiso 1 1 calc R . 1 H35B H 0.8526 0.2099 -0.1417 0.061 Uiso 1 1 calc R . 1 H35C H 0.9763 0.1469 -0.0954 0.061 Uiso 1 1 calc R . 1 C36 C 0.7997(12) 0.0649(8) -0.0295(7) 0.044(3) Uani 1 1 d . . 1 H36A H 0.8674 0.0289 0.0055 0.065 Uiso 1 1 calc R . 1 H36B H 0.8182 0.0384 -0.0803 0.065 Uiso 1 1 calc R . 1 H36C H 0.7117 0.0570 -0.0110 0.065 Uiso 1 1 calc R . 1 C37 C 0.6699(12) 0.3813(9) -0.0489(7) 0.046(3) Uani 1 1 d . . 1 H37A H 0.6762 0.3344 -0.0892 0.069 Uiso 1 1 calc R . 1 H37B H 0.7125 0.4351 -0.0667 0.069 Uiso 1 1 calc R . 1 H37C H 0.5760 0.4087 -0.0359 0.069 Uiso 1 1 calc R . 1 C38 C 0.7197(13) 0.3901(9) 0.0877(7) 0.049(3) Uani 1 1 d . . 1 H38A H 0.6281 0.3979 0.1075 0.074 Uiso 1 1 calc R . 1 H38B H 0.7367 0.4553 0.0730 0.074 Uiso 1 1 calc R . 1 H38C H 0.7816 0.3581 0.1271 0.074 Uiso 1 1 calc R . 1 C39 C 0.4525(14) 0.1893(9) 0.4393(7) 0.049(3) Uani 1 1 d . . 1 C40 C 0.421(2) 0.303(2) 0.5540(15) 0.155(12) Uani 1 1 d . . 1 H40A H 0.3268 0.3192 0.5416 0.232 Uiso 1 1 calc R . 1 H40B H 0.4578 0.3620 0.5458 0.232 Uiso 1 1 calc R . 1 H40C H 0.4309 0.2792 0.6074 0.232 Uiso 1 1 calc R . 1 C41 C 0.641(3) 0.223(4) 0.501(3) 0.40(5) Uani 1 1 d . . 1 H41A H 0.6557 0.2765 0.4653 0.596 Uiso 1 1 calc R . 1 H41B H 0.6968 0.1600 0.4850 0.596 Uiso 1 1 calc R . 1 H41C H 0.6633 0.2355 0.5522 0.596 Uiso 1 1 calc R . 1 C42A C 0.204(4) 0.280(3) 0.475(3) 0.045(15) Uani 0.25(3) 1 d P . 1 C43A C 0.257(3) 0.203(2) 0.3476(16) 0.057(10) Uani 0.49(4) 1 d P . 1 C42B C 0.374(2) 0.1112(15) 0.5600(10) 0.075(8) Uani 0.75(3) 1 d P . 2 C43B C 0.278(3) 0.107(3) 0.433(3) 0.12(2) Uani 0.51(4) 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0273(3) 0.0247(3) 0.0269(3) 0.0027(2) 0.0036(2) -0.0027(2) O1 0.029(3) 0.028(4) 0.028(4) 0.001(3) 0.000(3) -0.006(3) O2 0.032(4) 0.027(4) 0.033(4) 0.000(3) -0.003(3) 0.003(3) O3 0.044(5) 0.054(5) 0.063(5) -0.020(4) 0.011(4) -0.025(4) N1 0.037(5) 0.033(5) 0.034(5) 0.002(4) -0.002(4) -0.005(4) N2 0.039(5) 0.037(5) 0.024(4) -0.001(4) 0.005(4) -0.011(4) N3 0.046(5) 0.031(5) 0.030(5) 0.003(4) 0.007(4) -0.006(4) N4 0.052(6) 0.063(7) 0.035(5) 0.009(5) 0.009(5) 0.016(5) N5 0.112(14) 0.39(4) 0.100(14) -0.15(2) -0.045(11) 0.15(2) N6A 0.11(3) 0.15(3) 0.11(4) -0.07(3) 0.07(3) -0.10(3) N6B 0.052(18) 0.07(2) 0.014(17) 0.002(13) 0.009(12) -0.023(15) C1 0.060(8) 0.026(6) 0.049(7) 0.009(5) 0.011(6) 0.009(5) C2 0.032(6) 0.035(6) 0.054(7) 0.000(5) 0.006(5) 0.004(5) C3 0.025(5) 0.033(5) 0.031(5) -0.001(4) 0.006(4) 0.000(4) C4 0.025(5) 0.027(5) 0.030(5) -0.001(4) 0.012(4) 0.003(4) C5 0.030(5) 0.024(5) 0.034(5) 0.000(4) 0.011(4) -0.003(4) C6 0.040(6) 0.027(6) 0.055(7) -0.002(5) 0.015(5) -0.001(5) C7 0.022(5) 0.055(7) 0.038(6) -0.002(5) 0.003(4) -0.008(5) C8 0.031(7) 0.075(10) 0.085(10) 0.002(8) -0.008(7) -0.002(6) C9 0.029(6) 0.045(7) 0.063(8) -0.016(6) 0.008(5) -0.010(5) C10 0.042(6) 0.055(7) 0.037(6) -0.001(5) -0.007(5) -0.013(6) C11 0.042(6) 0.032(6) 0.033(6) 0.002(4) -0.006(5) -0.016(5) C12 0.065(8) 0.039(6) 0.034(6) -0.001(5) -0.005(6) -0.018(6) C13 0.059(8) 0.047(7) 0.062(8) 0.004(6) -0.013(7) -0.030(6) C14 0.022(5) 0.028(5) 0.036(5) 0.004(4) -0.004(4) -0.005(4) C15 0.031(6) 0.044(7) 0.067(8) 0.011(6) 0.005(6) 0.006(5) C16 0.032(6) 0.045(7) 0.050(7) 0.002(5) -0.003(5) -0.006(5) C17 0.031(5) 0.035(6) 0.041(6) 0.003(5) 0.003(5) -0.012(5) C18 0.022(5) 0.029(5) 0.034(5) 0.009(4) 0.000(4) 0.000(4) C19 0.028(5) 0.039(6) 0.024(5) 0.011(4) 0.007(4) -0.005(4) C20 0.041(6) 0.040(6) 0.039(6) 0.004(5) 0.001(5) 0.001(5) C21 0.039(6) 0.040(7) 0.064(8) 0.000(6) -0.006(6) -0.005(5) C22 0.048(8) 0.083(11) 0.086(11) -0.031(9) -0.016(8) -0.018(7) C23 0.041(7) 0.078(10) 0.048(7) -0.027(7) 0.001(6) -0.012(6) C24 0.062(9) 0.038(7) 0.099(12) 0.000(7) -0.021(8) -0.011(6) C25 0.043(6) 0.032(6) 0.036(6) -0.002(4) -0.002(5) -0.005(5) C26 0.036(6) 0.039(6) 0.062(8) -0.008(6) -0.009(6) -0.007(5) C27 0.082(10) 0.046(7) 0.034(6) -0.002(5) 0.005(6) -0.010(7) C28 0.079(10) 0.052(8) 0.049(8) -0.018(6) 0.008(7) 0.012(7) C29 0.080(12) 0.108(16) 0.137(18) -0.009(13) -0.022(12) -0.064(12) C30 0.106(15) 0.097(16) 0.16(2) 0.017(15) -0.060(15) -0.040(13) C31 1.6(3) 0.28(7) 0.16(4) -0.02(4) -0.40(11) 0.16(11) C32 0.84(15) 0.31(6) 0.09(3) 0.05(3) -0.12(5) -0.02(8) C33 0.43(8) 0.96(18) 0.10(3) 0.15(6) -0.10(4) -0.38(11) C34 0.033(5) 0.029(5) 0.024(5) 0.001(4) -0.004(4) -0.011(4) C35 0.046(6) 0.042(6) 0.035(6) -0.003(5) 0.008(5) -0.011(5) C36 0.055(7) 0.035(6) 0.042(6) -0.006(5) 0.005(5) -0.013(5) C37 0.050(7) 0.041(7) 0.041(6) 0.017(5) 0.004(5) -0.004(5) C38 0.065(8) 0.040(7) 0.044(7) -0.002(5) 0.001(6) -0.016(6) C39 0.065(8) 0.041(7) 0.036(7) 0.003(5) 0.017(6) -0.007(6) C40 0.109(18) 0.18(3) 0.17(2) -0.10(2) 0.007(17) 0.002(18) C41 0.094(19) 0.65(9) 0.38(6) -0.40(6) -0.14(3) 0.17(3) C42A 0.02(2) 0.04(3) 0.07(3) 0.00(2) 0.02(2) 0.006(18) C43A 0.052(17) 0.08(2) 0.043(17) -0.021(14) 0.017(12) -0.026(15) C42B 0.099(16) 0.071(14) 0.047(11) 0.012(9) 0.046(11) -0.014(11) C43B 0.06(2) 0.15(4) 0.19(5) -0.07(3) 0.04(2) -0.08(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O3 2.149(8) . ? La1 O2 2.304(6) . ? La1 O1 2.327(6) . ? La1 N4 2.605(9) . ? La1 N1 2.621(8) . ? O1 C4 1.339(11) . ? O2 C18 1.335(11) . ? O3 C29 1.409(16) . ? N1 C34 1.304(12) . ? N2 C34 1.379(12) . ? N2 C36 1.438(13) . ? N2 C35 1.454(13) . ? N3 C34 1.384(13) . ? N3 C38 1.444(14) . ? N3 C37 1.478(13) . ? N4 C39 1.308(14) . ? N5 C39 1.28(2) . ? N5 C41 1.43(4) . ? N5 C40 1.58(2) . ? N6A C39 1.44(4) . ? N6A C43A 1.45(6) . ? N6A C42A 1.60(5) . ? N6B C43B 1.36(4) . ? N6B C42B 1.54(4) . ? C1 C2 1.375(17) . ? C1 C6 1.382(17) . ? C2 C3 1.401(14) . ? C3 C4 1.424(14) . ? C3 C7 1.541(15) . ? C4 C5 1.433(14) . ? C5 C6 1.407(14) . ? C5 C11 1.541(14) . ? C7 C9 1.527(16) . ? C7 C10 1.527(15) . ? C7 C8 1.546(15) . ? C11 C14 1.521(14) . ? C11 C12 1.533(14) . ? C11 C13 1.553(15) . ? C15 C20 1.371(17) . ? C15 C16 1.378(17) . ? C16 C17 1.397(15) . ? C17 C18 1.465(15) . ? C17 C21 1.509(16) . ? C18 C19 1.438(15) . ? C19 C20 1.402(14) . ? C19 C25 1.531(15) . ? C21 C22 1.522(17) . ? C21 C23 1.527(17) . ? C21 C24 1.543(18) . ? C25 C26 1.522(15) . ? C25 C27 1.542(15) . ? C25 C28 1.562(15) . ? C29 C30 1.42(3) . ? C30 C31 1.15(6) . ? C31 C32 1.41(5) . ? C32 C33 1.21(6) . ? C33 C42A 1.88(7) 1_655 ? C42A C33 1.88(7) 1_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 La1 O2 108.9(3) . . ? O3 La1 O1 111.6(3) . . ? O2 La1 O1 139.5(2) . . ? O3 La1 N4 96.3(3) . . ? O2 La1 N4 94.1(3) . . ? O1 La1 N4 80.9(3) . . ? O3 La1 N1 94.5(3) . . ? O2 La1 N1 99.4(2) . . ? O1 La1 N1 78.3(2) . . ? N4 La1 N1 159.0(3) . . ? C4 O1 La1 172.9(6) . . ? C18 O2 La1 174.6(6) . . ? C29 O3 La1 165.3(10) . . ? C34 N1 La1 146.9(7) . . ? C34 N2 C36 118.0(8) . . ? C34 N2 C35 122.5(9) . . ? C36 N2 C35 115.1(9) . . ? C34 N3 C38 119.3(8) . . ? C34 N3 C37 120.5(9) . . ? C38 N3 C37 113.3(9) . . ? C39 N4 La1 156.0(9) . . ? C39 N5 C41 120.1(19) . . ? C39 N5 C40 124.8(16) . . ? C41 N5 C40 106(2) . . ? C39 N6A C43A 124(2) . . ? C39 N6A C42A 118(3) . . ? C43A N6A C42A 108(4) . . ? C43B N6B C42B 114(3) . . ? C2 C1 C6 119.9(10) . . ? C1 C2 C3 122.7(10) . . ? C2 C3 C4 117.9(10) . . ? C2 C3 C7 120.5(9) . . ? C4 C3 C7 121.6(9) . . ? O1 C4 C3 120.5(9) . . ? O1 C4 C5 120.1(8) . . ? C3 C4 C5 119.3(9) . . ? C6 C5 C4 119.5(10) . . ? C6 C5 C11 118.3(9) . . ? C4 C5 C11 122.2(8) . . ? C1 C6 C5 120.5(11) . . ? C9 C7 C10 111.1(10) . . ? C9 C7 C3 111.6(9) . . ? C10 C7 C3 109.4(8) . . ? C9 C7 C8 106.8(9) . . ? C10 C7 C8 105.6(10) . . ? C3 C7 C8 112.1(10) . . ? C14 C11 C12 110.2(9) . . ? C14 C11 C5 111.0(8) . . ? C12 C11 C5 109.7(9) . . ? C14 C11 C13 105.5(9) . . ? C12 C11 C13 106.6(9) . . ? C5 C11 C13 113.6(9) . . ? C20 C15 C16 118.7(10) . . ? C15 C16 C17 122.7(11) . . ? C16 C17 C18 118.0(10) . . ? C16 C17 C21 120.3(10) . . ? C18 C17 C21 121.8(9) . . ? O2 C18 C19 121.9(9) . . ? O2 C18 C17 118.8(9) . . ? C19 C18 C17 119.3(8) . . ? C20 C19 C18 117.0(10) . . ? C20 C19 C25 121.7(10) . . ? C18 C19 C25 121.2(8) . . ? C15 C20 C19 124.3(11) . . ? C17 C21 C22 113.0(10) . . ? C17 C21 C23 110.9(10) . . ? C22 C21 C23 106.0(11) . . ? C17 C21 C24 109.4(11) . . ? C22 C21 C24 105.7(11) . . ? C23 C21 C24 111.7(11) . . ? C26 C25 C19 111.1(9) . . ? C26 C25 C27 110.4(10) . . ? C19 C25 C27 110.7(9) . . ? C26 C25 C28 107.1(10) . . ? C19 C25 C28 111.7(9) . . ? C27 C25 C28 105.8(9) . . ? O3 C29 C30 114.9(17) . . ? C31 C30 C29 118(3) . . ? C30 C31 C32 142(8) . . ? C33 C32 C31 175(7) . . ? C32 C33 C42A 103(6) . 1_655 ? N1 C34 N2 125.0(9) . . ? N1 C34 N3 119.0(9) . . ? N2 C34 N3 116.0(8) . . ? N5 C39 N4 123.1(16) . . ? N5 C39 N6A 125.4(16) . . ? N4 C39 N6A 109.2(18) . . ? N6A C42A C33 150(4) . 1_455 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 3.507 _refine_diff_density_min -1.935 _refine_diff_density_rms 0.167 #===END data_bob025 _database_code_depnum_ccdc_archive 'CCDC 722742' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Nd(4MeDBP)3(H-TMG)) (5)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H82 N3 Nd O3' _chemical_formula_weight 917.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 '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 15.5703(11) _cell_length_b 16.6702(12) _cell_length_c 19.6340(14) _cell_angle_alpha 77.4400(10) _cell_angle_beta 86.8950(10) _cell_angle_gamma 81.8590(10) _cell_volume 4922.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8687 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 26.32 _exptl_crystal_description irregular _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1948 _exptl_absorpt_coefficient_mu 1.096 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7346 _exptl_absorpt_correction_T_max 0.8107 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 40247 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 25.05 _reflns_number_total 17405 _reflns_number_gt 12623 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.2813P] 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 17405 _refine_ls_number_parameters 1077 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.1194 _refine_ls_wR_factor_gt 0.0950 _refine_ls_goodness_of_fit_ref 0.769 _refine_ls_restrained_S_all 0.769 _refine_ls_shift/su_max 0.233 _refine_ls_shift/su_mean 0.002 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 Nd1 Nd 0.282710(13) 0.701972(13) 0.513338(11) 0.01908(7) Uani 1 1 d . . . Nd2 Nd 0.267864(14) 0.202818(13) 0.047969(11) 0.02046(7) Uani 1 1 d . . . N1 N 0.3044(2) 0.5477(2) 0.54031(19) 0.0273(8) Uani 1 1 d . . . H1 H 0.3606 0.5313 0.5430 0.033 Uiso 1 1 calc R . . N2 N 0.1838(2) 0.4851(2) 0.5287(2) 0.0280(8) Uani 1 1 d . . . N3 N 0.3012(2) 0.4051(2) 0.5889(2) 0.0296(9) Uani 1 1 d . . . N4 N 0.2887(3) 0.0502(2) 0.07805(19) 0.0328(9) Uani 1 1 d . . . H4 H 0.3231 0.0318 0.1138 0.039 Uiso 1 1 calc R . . N5 N 0.1799(3) -0.0081(2) 0.0384(2) 0.0336(9) Uani 1 1 d . . . N6 N 0.3184(3) -0.0811(2) 0.0485(2) 0.0356(9) Uani 1 1 d . . . O1 O 0.41873(18) 0.72419(16) 0.49808(14) 0.0224(6) Uani 1 1 d . . . O2 O 0.20052(18) 0.75072(17) 0.42072(14) 0.0231(6) Uani 1 1 d . . . O3 O 0.22824(18) 0.73010(17) 0.61041(14) 0.0226(6) Uani 1 1 d . . . O4 O 0.21462(19) 0.24357(17) 0.14164(14) 0.0245(6) Uani 1 1 d . . . O5 O 0.19181(18) 0.23033(18) -0.04760(14) 0.0262(7) Uani 1 1 d . . . O6 O 0.40393(18) 0.22190(17) 0.02921(15) 0.0253(6) Uani 1 1 d . . . C1 C 0.4891(3) 0.7576(2) 0.5115(2) 0.0225(9) Uani 1 1 d . . . C2 C 0.5418(3) 0.7169(3) 0.5698(2) 0.0252(9) Uani 1 1 d . . . C3 C 0.6082(3) 0.7567(3) 0.5863(2) 0.0263(10) Uani 1 1 d . . . H3 H 0.6427 0.7302 0.6253 0.032 Uiso 1 1 calc R . . C4 C 0.6264(3) 0.8329(3) 0.5485(2) 0.0314(10) Uani 1 1 d . . . C5 C 0.5773(3) 0.8689(3) 0.4898(2) 0.0290(10) Uani 1 1 d . . . H5 H 0.5904 0.9204 0.4625 0.035 Uiso 1 1 calc R . . C6 C 0.5096(3) 0.8332(3) 0.4689(2) 0.0260(10) Uani 1 1 d . . . C7 C 0.6981(3) 0.8744(3) 0.5691(3) 0.0470(14) Uani 1 1 d . . . H7A H 0.7169 0.8464 0.6162 0.070 Uiso 1 1 calc R . . H7B H 0.6767 0.9327 0.5685 0.070 Uiso 1 1 calc R . . H7C H 0.7472 0.8709 0.5360 0.070 Uiso 1 1 calc R . . C8 C 0.5278(3) 0.6308(3) 0.6142(2) 0.0288(10) Uani 1 1 d . . . C9 C 0.5316(3) 0.5686(3) 0.5661(3) 0.0344(11) Uani 1 1 d . . . H9A H 0.5195 0.5147 0.5936 0.052 Uiso 1 1 calc R . . H9B H 0.5895 0.5625 0.5441 0.052 Uiso 1 1 calc R . . H9C H 0.4882 0.5890 0.5298 0.052 Uiso 1 1 calc R . . C10 C 0.4426(3) 0.6355(3) 0.6560(2) 0.0340(11) Uani 1 1 d . . . H10A H 0.4370 0.5811 0.6859 0.051 Uiso 1 1 calc R . . H10B H 0.3941 0.6519 0.6240 0.051 Uiso 1 1 calc R . . H10C H 0.4420 0.6765 0.6851 0.051 Uiso 1 1 calc R . . C11 C 0.5996(3) 0.5961(3) 0.6684(3) 0.0426(13) Uani 1 1 d . . . H11A H 0.5981 0.6328 0.7013 0.064 Uiso 1 1 calc R . . H11B H 0.6564 0.5930 0.6443 0.064 Uiso 1 1 calc R . . H11C H 0.5898 0.5406 0.6937 0.064 Uiso 1 1 calc R . . C12 C 0.4665(3) 0.8736(3) 0.3986(2) 0.0298(10) Uani 1 1 d . . . C13 C 0.4934(3) 0.8163(3) 0.3479(3) 0.0403(12) Uani 1 1 d . . . H13A H 0.4672 0.8410 0.3026 0.060 Uiso 1 1 calc R . . H13B H 0.4736 0.7624 0.3664 0.060 Uiso 1 1 calc R . . H13C H 0.5568 0.8088 0.3421 0.060 Uiso 1 1 calc R . . C14 C 0.3668(3) 0.8897(3) 0.4042(2) 0.0323(11) Uani 1 1 d . . . H14A H 0.3495 0.9176 0.4429 0.048 Uiso 1 1 calc R . . H14B H 0.3433 0.8368 0.4128 0.048 Uiso 1 1 calc R . . H14C H 0.3441 0.9250 0.3605 0.048 Uiso 1 1 calc R . . C15 C 0.4966(4) 0.9576(3) 0.3663(3) 0.0499(15) Uani 1 1 d . . . H15A H 0.4693 0.9801 0.3211 0.075 Uiso 1 1 calc R . . H15B H 0.5598 0.9503 0.3595 0.075 Uiso 1 1 calc R . . H15C H 0.4800 0.9961 0.3974 0.075 Uiso 1 1 calc R . . C16 C 0.1463(3) 0.7319(2) 0.3765(2) 0.0219(9) Uani 1 1 d . . . C17 C 0.0553(3) 0.7490(2) 0.3849(2) 0.0234(9) Uani 1 1 d . . . C18 C 0.0030(3) 0.7153(3) 0.3464(2) 0.0296(10) Uani 1 1 d . . . H18 H -0.0582 0.7252 0.3529 0.036 Uiso 1 1 calc R . . C19 C 0.0366(3) 0.6677(3) 0.2989(2) 0.0315(11) Uani 1 1 d . . . C20 C 0.1258(3) 0.6593(3) 0.2858(2) 0.0313(11) Uani 1 1 d . . . H20 H 0.1492 0.6296 0.2514 0.038 Uiso 1 1 calc R . . C21 C 0.1822(3) 0.6928(3) 0.3213(2) 0.0265(10) Uani 1 1 d . . . C22 C -0.0225(4) 0.6304(3) 0.2586(3) 0.0445(14) Uani 1 1 d . . . H22A H -0.0718 0.6131 0.2887 0.067 Uiso 1 1 calc R . . H22B H 0.0100 0.5822 0.2436 0.067 Uiso 1 1 calc R . . H22C H -0.0439 0.6719 0.2176 0.067 Uiso 1 1 calc R . . C23 C 0.0137(3) 0.8066(3) 0.4331(2) 0.0267(10) Uani 1 1 d . . . C24 C 0.0486(3) 0.8905(3) 0.4109(2) 0.0337(11) Uani 1 1 d . . . H24A H 0.1120 0.8818 0.4145 0.051 Uiso 1 1 calc R . . H24B H 0.0234 0.9272 0.4416 0.051 Uiso 1 1 calc R . . H24C H 0.0329 0.9158 0.3626 0.051 Uiso 1 1 calc R . . C25 C 0.0312(3) 0.7691(3) 0.5102(2) 0.0309(10) Uani 1 1 d . . . H25A H 0.0107 0.7147 0.5231 0.046 Uiso 1 1 calc R . . H25B H 0.0004 0.8058 0.5389 0.046 Uiso 1 1 calc R . . H25C H 0.0936 0.7627 0.5181 0.046 Uiso 1 1 calc R . . C26 C -0.0864(3) 0.8235(3) 0.4271(3) 0.0450(13) Uani 1 1 d . . . H26A H -0.1014 0.8479 0.3785 0.067 Uiso 1 1 calc R . . H26B H -0.1102 0.8619 0.4567 0.067 Uiso 1 1 calc R . . H26C H -0.1107 0.7712 0.4423 0.067 Uiso 1 1 calc R . . C27 C 0.2772(3) 0.6938(3) 0.2972(2) 0.0296(10) Uani 1 1 d . . . C28 C 0.2922(3) 0.7847(3) 0.2699(2) 0.0351(11) Uani 1 1 d . . . H28A H 0.2538 0.8101 0.2309 0.053 Uiso 1 1 calc R . . H28B H 0.3528 0.7867 0.2540 0.053 Uiso 1 1 calc R . . H28C H 0.2796 0.8152 0.3075 0.053 Uiso 1 1 calc R . . C29 C 0.3425(3) 0.6514(3) 0.3536(3) 0.0403(12) Uani 1 1 d . . . H29A H 0.3460 0.6879 0.3860 0.060 Uiso 1 1 calc R . . H29B H 0.3997 0.6398 0.3317 0.060 Uiso 1 1 calc R . . H29C H 0.3235 0.5993 0.3792 0.060 Uiso 1 1 calc R . . C30 C 0.2985(4) 0.6492(3) 0.2368(3) 0.0500(14) Uani 1 1 d . . . H30A H 0.2916 0.5905 0.2527 0.075 Uiso 1 1 calc R . . H30B H 0.3585 0.6541 0.2204 0.075 Uiso 1 1 calc R . . H30C H 0.2590 0.6745 0.1985 0.075 Uiso 1 1 calc R . . C31 C 0.2060(2) 0.7564(2) 0.6705(2) 0.0198(9) Uani 1 1 d . . . C32 C 0.2168(3) 0.8383(3) 0.6758(2) 0.0236(9) Uani 1 1 d . . . C33 C 0.2000(3) 0.8601(3) 0.7400(2) 0.0298(10) Uani 1 1 d . . . H33 H 0.2070 0.9147 0.7436 0.036 Uiso 1 1 calc R . . C34 C 0.1739(3) 0.8072(3) 0.7982(2) 0.0326(11) Uani 1 1 d . . . C35 C 0.1595(3) 0.7297(3) 0.7919(2) 0.0309(10) Uani 1 1 d . . . H35 H 0.1393 0.6933 0.8319 0.037 Uiso 1 1 calc R . . C36 C 0.1732(3) 0.7020(3) 0.7293(2) 0.0243(9) Uani 1 1 d . . . C37 C 0.1613(4) 0.8344(4) 0.8673(3) 0.0511(15) Uani 1 1 d . . . H37A H 0.2083 0.8655 0.8731 0.077 Uiso 1 1 calc R . . H37B H 0.1620 0.7855 0.9055 0.077 Uiso 1 1 calc R . . H37C H 0.1054 0.8697 0.8680 0.077 Uiso 1 1 calc R . . C38 C 0.2485(3) 0.9019(3) 0.6132(2) 0.0254(10) Uani 1 1 d . . . C39 C 0.1891(3) 0.9148(3) 0.5506(2) 0.0342(11) Uani 1 1 d . . . H39A H 0.2106 0.9549 0.5115 0.051 Uiso 1 1 calc R . . H39B H 0.1299 0.9360 0.5637 0.051 Uiso 1 1 calc R . . H39C H 0.1888 0.8619 0.5367 0.051 Uiso 1 1 calc R . . C40 C 0.3441(3) 0.8741(3) 0.5956(2) 0.0283(10) Uani 1 1 d . . . H40A H 0.3489 0.8212 0.5807 0.042 Uiso 1 1 calc R . . H40B H 0.3790 0.8674 0.6370 0.042 Uiso 1 1 calc R . . H40C H 0.3651 0.9161 0.5579 0.042 Uiso 1 1 calc R . . C41 C 0.2458(3) 0.9878(3) 0.6311(3) 0.0395(12) Uani 1 1 d . . . H41A H 0.2868 0.9842 0.6682 0.059 Uiso 1 1 calc R . . H41B H 0.1870 1.0063 0.6470 0.059 Uiso 1 1 calc R . . H41C H 0.2619 1.0276 0.5895 0.059 Uiso 1 1 calc R . . C42 C 0.1532(3) 0.6145(3) 0.7274(2) 0.0302(10) Uani 1 1 d . . . C43 C 0.0936(3) 0.6184(3) 0.6672(3) 0.0371(12) Uani 1 1 d . . . H43A H 0.1239 0.6372 0.6228 0.056 Uiso 1 1 calc R . . H43B H 0.0411 0.6574 0.6712 0.056 Uiso 1 1 calc R . . H43C H 0.0775 0.5633 0.6691 0.056 Uiso 1 1 calc R . . C44 C 0.2374(3) 0.5571(3) 0.7202(3) 0.0390(12) Uani 1 1 d . . . H44A H 0.2238 0.5020 0.7182 0.058 Uiso 1 1 calc R . . H44B H 0.2737 0.5526 0.7604 0.058 Uiso 1 1 calc R . . H44C H 0.2687 0.5799 0.6773 0.058 Uiso 1 1 calc R . . C45 C 0.1059(4) 0.5747(3) 0.7949(3) 0.0505(15) Uani 1 1 d . . . H45A H 0.0494 0.6077 0.7994 0.076 Uiso 1 1 calc R . . H45B H 0.1410 0.5729 0.8353 0.076 Uiso 1 1 calc R . . H45C H 0.0974 0.5182 0.7927 0.076 Uiso 1 1 calc R . . C46 C 0.2648(3) 0.4808(3) 0.5522(2) 0.0254(10) Uani 1 1 d . . . C47 C 0.1482(3) 0.5580(3) 0.4784(2) 0.0318(11) Uani 1 1 d . . . H47A H 0.1238 0.6017 0.5029 0.048 Uiso 1 1 calc R . . H47B H 0.1024 0.5438 0.4526 0.048 Uiso 1 1 calc R . . H47C H 0.1942 0.5778 0.4457 0.048 Uiso 1 1 calc R . . C48 C 0.1189(3) 0.4360(3) 0.5673(3) 0.0346(11) Uani 1 1 d . . . H48A H 0.1452 0.3989 0.6089 0.052 Uiso 1 1 calc R . . H48B H 0.0983 0.4030 0.5374 0.052 Uiso 1 1 calc R . . H48C H 0.0700 0.4732 0.5814 0.052 Uiso 1 1 calc R . . C49 C 0.3766(3) 0.3995(3) 0.6308(3) 0.0376(12) Uani 1 1 d . . . H49A H 0.4294 0.3947 0.6016 0.056 Uiso 1 1 calc R . . H49B H 0.3781 0.3505 0.6691 0.056 Uiso 1 1 calc R . . H49C H 0.3733 0.4494 0.6500 0.056 Uiso 1 1 calc R . . C50 C 0.2896(3) 0.3280(3) 0.5685(3) 0.0362(11) Uani 1 1 d . . . H50A H 0.2543 0.3409 0.5267 0.054 Uiso 1 1 calc R . . H50B H 0.2603 0.2929 0.6067 0.054 Uiso 1 1 calc R . . H50C H 0.3465 0.2988 0.5585 0.054 Uiso 1 1 calc R . . C51 C 0.1946(3) 0.2772(3) 0.1983(2) 0.0223(9) Uani 1 1 d . . . C52 C 0.2093(3) 0.3594(3) 0.1967(2) 0.0243(9) Uani 1 1 d . . . C53 C 0.1910(3) 0.3908(3) 0.2575(2) 0.0275(10) Uani 1 1 d . . . H53 H 0.2008 0.4460 0.2565 0.033 Uiso 1 1 calc R . . C54 C 0.1595(3) 0.3454(3) 0.3182(2) 0.0279(10) Uani 1 1 d . . . C55 C 0.1422(3) 0.2665(3) 0.3170(2) 0.0276(10) Uani 1 1 d . . . H55 H 0.1180 0.2353 0.3581 0.033 Uiso 1 1 calc R . . C56 C 0.1582(3) 0.2301(3) 0.2594(2) 0.0238(9) Uani 1 1 d . . . C57 C 0.1423(3) 0.3811(3) 0.3828(3) 0.0419(13) Uani 1 1 d . . . H57A H 0.1797 0.4240 0.3815 0.063 Uiso 1 1 calc R . . H57B H 0.1547 0.3369 0.4244 0.063 Uiso 1 1 calc R . . H57C H 0.0814 0.4056 0.3845 0.063 Uiso 1 1 calc R . . C58 C 0.2439(3) 0.4166(3) 0.1312(2) 0.0275(10) Uani 1 1 d . . . C59 C 0.3377(3) 0.3826(3) 0.1141(2) 0.0320(11) Uani 1 1 d . . . H59A H 0.3600 0.4203 0.0736 0.048 Uiso 1 1 calc R . . H59B H 0.3389 0.3277 0.1034 0.048 Uiso 1 1 calc R . . H59C H 0.3740 0.3782 0.1543 0.048 Uiso 1 1 calc R . . C60 C 0.1842(3) 0.4258(3) 0.0692(2) 0.0324(11) Uani 1 1 d . . . H60A H 0.1260 0.4510 0.0807 0.049 Uiso 1 1 calc R . . H60B H 0.1811 0.3710 0.0596 0.049 Uiso 1 1 calc R . . H60C H 0.2077 0.4612 0.0279 0.049 Uiso 1 1 calc R . . C61 C 0.2481(3) 0.5045(3) 0.1420(3) 0.0383(12) Uani 1 1 d . . . H61A H 0.2679 0.5388 0.0986 0.057 Uiso 1 1 calc R . . H61B H 0.2888 0.5018 0.1791 0.057 Uiso 1 1 calc R . . H61C H 0.1903 0.5289 0.1554 0.057 Uiso 1 1 calc R . . C62 C 0.1329(3) 0.1431(3) 0.2642(2) 0.0295(10) Uani 1 1 d . . . C63 C 0.0649(3) 0.1486(3) 0.2088(3) 0.0365(11) Uani 1 1 d . . . H63A H 0.0127 0.1849 0.2187 0.055 Uiso 1 1 calc R . . H63B H 0.0500 0.0931 0.2100 0.055 Uiso 1 1 calc R . . H63C H 0.0887 0.1712 0.1625 0.055 Uiso 1 1 calc R . . C64 C 0.2135(3) 0.0810(3) 0.2529(3) 0.0363(11) Uani 1 1 d . . . H64A H 0.2413 0.1013 0.2076 0.054 Uiso 1 1 calc R . . H64B H 0.1956 0.0268 0.2537 0.054 Uiso 1 1 calc R . . H64C H 0.2547 0.0756 0.2901 0.054 Uiso 1 1 calc R . . C65 C 0.0915(4) 0.1076(3) 0.3342(3) 0.0455(14) Uani 1 1 d . . . H65A H 0.1322 0.1040 0.3715 0.068 Uiso 1 1 calc R . . H65B H 0.0775 0.0521 0.3342 0.068 Uiso 1 1 calc R . . H65C H 0.0383 0.1438 0.3421 0.068 Uiso 1 1 calc R . . C66 C 0.1331(3) 0.2117(3) -0.0885(2) 0.0249(9) Uani 1 1 d . . . C67 C 0.0427(3) 0.2386(3) -0.0798(2) 0.0272(10) Uani 1 1 d . . . C68 C -0.0161(3) 0.2058(3) -0.1143(2) 0.0287(10) Uani 1 1 d . . . H68 H -0.0765 0.2213 -0.1072 0.034 Uiso 1 1 calc R . . C69 C 0.0099(3) 0.1516(3) -0.1586(2) 0.0307(10) Uani 1 1 d . . . C70 C 0.0976(3) 0.1355(3) -0.1726(2) 0.0321(11) Uani 1 1 d . . . H70 H 0.1161 0.1028 -0.2060 0.039 Uiso 1 1 calc R . . C71 C 0.1609(3) 0.1651(3) -0.1399(2) 0.0257(9) Uani 1 1 d . . . C72 C -0.0557(3) 0.1188(3) -0.1952(3) 0.0387(12) Uani 1 1 d . . . H72A H -0.0754 0.1603 -0.2368 0.058 Uiso 1 1 calc R . . H72B H -0.1054 0.1070 -0.1636 0.058 Uiso 1 1 calc R . . H72C H -0.0290 0.0678 -0.2091 0.058 Uiso 1 1 calc R . . C73 C 0.0098(3) 0.3054(3) -0.0381(2) 0.0286(10) Uani 1 1 d . . . C74 C 0.0257(3) 0.2742(3) 0.0401(2) 0.0319(11) Uani 1 1 d . . . H74A H 0.0013 0.2222 0.0567 0.048 Uiso 1 1 calc R . . H74B H -0.0022 0.3158 0.0656 0.048 Uiso 1 1 calc R . . H74C H 0.0883 0.2647 0.0481 0.048 Uiso 1 1 calc R . . C75 C 0.0541(3) 0.3829(3) -0.0659(2) 0.0376(12) Uani 1 1 d . . . H75A H 0.1172 0.3671 -0.0673 0.056 Uiso 1 1 calc R . . H75B H 0.0394 0.4222 -0.0352 0.056 Uiso 1 1 calc R . . H75C H 0.0342 0.4089 -0.1131 0.056 Uiso 1 1 calc R . . C76 C -0.0886(3) 0.3312(3) -0.0445(3) 0.0431(13) Uani 1 1 d . . . H76A H -0.1033 0.3476 -0.0940 0.065 Uiso 1 1 calc R . . H76B H -0.1064 0.3780 -0.0219 0.065 Uiso 1 1 calc R . . H76C H -0.1190 0.2844 -0.0218 0.065 Uiso 1 1 calc R . . C77 C 0.2553(3) 0.1536(3) -0.1659(2) 0.0317(11) Uani 1 1 d . . . C78 C 0.3202(3) 0.1131(3) -0.1086(3) 0.0394(12) Uani 1 1 d . . . H78A H 0.3285 0.1533 -0.0806 0.059 Uiso 1 1 calc R . . H78B H 0.3759 0.0949 -0.1300 0.059 Uiso 1 1 calc R . . H78C H 0.2979 0.0651 -0.0785 0.059 Uiso 1 1 calc R . . C79 C 0.2791(3) 0.2399(3) -0.2010(2) 0.0396(12) Uani 1 1 d . . . H79A H 0.2377 0.2663 -0.2378 0.059 Uiso 1 1 calc R . . H79B H 0.3378 0.2341 -0.2216 0.059 Uiso 1 1 calc R . . H79C H 0.2767 0.2743 -0.1662 0.059 Uiso 1 1 calc R . . C80 C 0.2698(4) 0.1004(4) -0.2212(3) 0.0534(15) Uani 1 1 d . . . H80A H 0.2569 0.0442 -0.2006 0.080 Uiso 1 1 calc R . . H80B H 0.3303 0.0980 -0.2380 0.080 Uiso 1 1 calc R . . H80C H 0.2313 0.1251 -0.2603 0.080 Uiso 1 1 calc R . . C81 C 0.4747(3) 0.2581(2) 0.0363(2) 0.0238(9) Uani 1 1 d . . . C82 C 0.4966(3) 0.3270(3) -0.0155(2) 0.0274(10) Uani 1 1 d . . . C83 C 0.5659(3) 0.3661(3) -0.0035(2) 0.0305(10) Uani 1 1 d . . . H83 H 0.5799 0.4126 -0.0376 0.037 Uiso 1 1 calc R . . C84 C 0.6152(3) 0.3401(3) 0.0557(2) 0.0320(11) Uani 1 1 d . . . C85 C 0.5955(3) 0.2711(3) 0.1037(2) 0.0288(10) Uani 1 1 d . . . H85 H 0.6303 0.2518 0.1438 0.035 Uiso 1 1 calc R . . C86 C 0.5273(3) 0.2286(3) 0.0964(2) 0.0267(10) Uani 1 1 d . . . C87 C 0.6898(3) 0.3846(3) 0.0663(3) 0.0429(13) Uani 1 1 d . . . H87A H 0.6986 0.3778 0.1164 0.064 Uiso 1 1 calc R . . H87B H 0.6765 0.4437 0.0451 0.064 Uiso 1 1 calc R . . H87C H 0.7426 0.3611 0.0444 0.064 Uiso 1 1 calc R . . C88 C 0.5110(3) 0.1521(3) 0.1540(2) 0.0319(11) Uani 1 1 d . . . C89 C 0.5091(4) 0.0760(3) 0.1207(3) 0.0582(16) Uani 1 1 d . . . H89A H 0.5667 0.0603 0.1011 0.087 Uiso 1 1 calc R . . H89B H 0.4666 0.0903 0.0834 0.087 Uiso 1 1 calc R . . H89C H 0.4927 0.0295 0.1564 0.087 Uiso 1 1 calc R . . C90 C 0.4264(4) 0.1684(4) 0.1942(3) 0.0558(16) Uani 1 1 d . . . H90A H 0.4171 0.1184 0.2291 0.084 Uiso 1 1 calc R . . H90B H 0.3782 0.1832 0.1618 0.084 Uiso 1 1 calc R . . H90C H 0.4293 0.2142 0.2176 0.084 Uiso 1 1 calc R . . C91 C 0.5835(4) 0.1260(4) 0.2057(3) 0.0636(19) Uani 1 1 d . . . H91A H 0.5854 0.1698 0.2316 0.095 Uiso 1 1 calc R . . H91B H 0.6389 0.1168 0.1806 0.095 Uiso 1 1 calc R . . H91C H 0.5730 0.0747 0.2383 0.095 Uiso 1 1 calc R . . C92 C 0.4496(3) 0.3571(3) -0.0850(2) 0.0314(10) Uani 1 1 d . . . C93 C 0.3497(3) 0.3767(3) -0.0760(3) 0.0383(12) Uani 1 1 d . . . H93A H 0.3244 0.3248 -0.0630 0.057 Uiso 1 1 calc R . . H93B H 0.3253 0.4094 -0.1201 0.057 Uiso 1 1 calc R . . H93C H 0.3362 0.4084 -0.0393 0.057 Uiso 1 1 calc R . . C94 C 0.4795(3) 0.4367(3) -0.1288(3) 0.0435(13) Uani 1 1 d . . . H94A H 0.4678 0.4811 -0.1026 0.065 Uiso 1 1 calc R . . H94B H 0.4479 0.4532 -0.1725 0.065 Uiso 1 1 calc R . . H94C H 0.5419 0.4268 -0.1391 0.065 Uiso 1 1 calc R . . C95 C 0.4685(3) 0.2903(3) -0.1284(2) 0.0372(12) Uani 1 1 d . . . H95A H 0.5313 0.2786 -0.1363 0.056 Uiso 1 1 calc R . . H95B H 0.4400 0.3101 -0.1734 0.056 Uiso 1 1 calc R . . H95C H 0.4463 0.2396 -0.1033 0.056 Uiso 1 1 calc R . . C96 C 0.2636(3) -0.0125(3) 0.0564(2) 0.0274(10) Uani 1 1 d . . . C97 C 0.1557(4) -0.0424(3) -0.0188(3) 0.0456(13) Uani 1 1 d . . . H97A H 0.2082 -0.0630 -0.0430 0.068 Uiso 1 1 calc R . . H97B H 0.1205 0.0009 -0.0517 0.068 Uiso 1 1 calc R . . H97C H 0.1220 -0.0881 -0.0004 0.068 Uiso 1 1 calc R . . C98 C 0.1130(3) 0.0514(3) 0.0609(3) 0.0450(13) Uani 1 1 d . . . H98A H 0.1319 0.0666 0.1027 0.067 Uiso 1 1 calc R . . H98B H 0.0591 0.0267 0.0716 0.067 Uiso 1 1 calc R . . H98C H 0.1031 0.1011 0.0235 0.067 Uiso 1 1 calc R . . C99 C 0.2915(3) -0.1635(3) 0.0623(3) 0.0411(12) Uani 1 1 d . . . H99A H 0.2289 -0.1593 0.0723 0.062 Uiso 1 1 calc R . . H99B H 0.3225 -0.1986 0.1026 0.062 Uiso 1 1 calc R . . H99C H 0.3052 -0.1881 0.0213 0.062 Uiso 1 1 calc R . . C100 C 0.4112(3) -0.0812(3) 0.0538(3) 0.0540(15) Uani 1 1 d . . . H10D H 0.4274 -0.0279 0.0284 0.081 Uiso 1 1 calc R . . H10E H 0.4429 -0.1260 0.0336 0.081 Uiso 1 1 calc R . . H10F H 0.4259 -0.0899 0.1030 0.081 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.01949(13) 0.02025(13) 0.01811(13) -0.00502(9) -0.00116(9) -0.00297(9) Nd2 0.02090(13) 0.02242(13) 0.01904(13) -0.00756(10) -0.00045(9) -0.00123(9) N1 0.029(2) 0.025(2) 0.030(2) -0.0105(16) 0.0007(16) -0.0036(16) N2 0.028(2) 0.0214(19) 0.033(2) -0.0016(16) -0.0012(17) -0.0043(15) N3 0.035(2) 0.0225(19) 0.031(2) -0.0045(16) -0.0063(17) -0.0035(16) N4 0.043(2) 0.031(2) 0.025(2) -0.0090(17) -0.0067(18) -0.0025(18) N5 0.038(2) 0.031(2) 0.033(2) -0.0115(18) -0.0006(18) -0.0033(17) N6 0.037(2) 0.026(2) 0.045(3) -0.0120(18) 0.0038(19) -0.0052(17) O1 0.0243(15) 0.0176(14) 0.0250(16) -0.0032(12) -0.0030(12) -0.0027(12) O2 0.0239(15) 0.0240(15) 0.0218(15) -0.0059(12) -0.0001(12) -0.0039(12) O3 0.0249(16) 0.0261(16) 0.0183(15) -0.0077(12) -0.0002(12) -0.0041(12) O4 0.0325(17) 0.0215(15) 0.0204(15) -0.0076(12) 0.0025(13) -0.0030(12) O5 0.0236(16) 0.0347(17) 0.0200(15) -0.0065(13) -0.0032(12) -0.0011(13) O6 0.0225(15) 0.0257(16) 0.0280(16) -0.0045(13) -0.0014(13) -0.0057(12) C1 0.021(2) 0.020(2) 0.026(2) -0.0060(18) -0.0004(18) -0.0018(17) C2 0.023(2) 0.025(2) 0.026(2) -0.0044(19) 0.0019(18) -0.0005(18) C3 0.025(2) 0.026(2) 0.028(2) -0.0053(19) -0.0052(19) -0.0036(18) C4 0.028(2) 0.032(3) 0.035(3) -0.005(2) -0.005(2) -0.008(2) C5 0.029(2) 0.021(2) 0.037(3) -0.0024(19) -0.003(2) -0.0050(18) C6 0.022(2) 0.023(2) 0.032(2) -0.0068(19) -0.0033(19) 0.0000(17) C7 0.045(3) 0.036(3) 0.062(4) -0.004(3) -0.022(3) -0.013(2) C8 0.026(2) 0.025(2) 0.031(3) 0.0028(19) -0.008(2) -0.0013(18) C9 0.032(3) 0.023(2) 0.047(3) -0.007(2) -0.003(2) -0.0001(19) C10 0.033(3) 0.040(3) 0.026(2) 0.002(2) -0.003(2) -0.008(2) C11 0.038(3) 0.041(3) 0.043(3) 0.009(2) -0.014(2) -0.007(2) C12 0.030(2) 0.027(2) 0.030(3) 0.001(2) -0.003(2) -0.0058(19) C13 0.037(3) 0.049(3) 0.030(3) -0.003(2) -0.001(2) 0.003(2) C14 0.026(2) 0.033(3) 0.035(3) -0.002(2) -0.007(2) 0.0023(19) C15 0.052(3) 0.045(3) 0.046(3) 0.017(3) -0.018(3) -0.020(3) C16 0.028(2) 0.017(2) 0.021(2) -0.0012(17) -0.0040(18) -0.0023(17) C17 0.028(2) 0.022(2) 0.020(2) -0.0008(17) -0.0019(18) -0.0079(18) C18 0.030(2) 0.029(2) 0.027(2) 0.007(2) -0.008(2) -0.0120(19) C19 0.047(3) 0.026(2) 0.022(2) 0.0034(19) -0.012(2) -0.018(2) C20 0.047(3) 0.027(2) 0.022(2) -0.0055(19) -0.002(2) -0.011(2) C21 0.038(3) 0.020(2) 0.019(2) 0.0001(18) -0.0066(19) -0.0023(19) C22 0.061(4) 0.051(3) 0.028(3) -0.005(2) -0.013(2) -0.031(3) C23 0.020(2) 0.026(2) 0.033(3) -0.005(2) -0.0070(19) -0.0002(18) C24 0.044(3) 0.020(2) 0.036(3) -0.005(2) -0.003(2) -0.003(2) C25 0.032(3) 0.033(3) 0.029(3) -0.009(2) 0.004(2) -0.005(2) C26 0.029(3) 0.045(3) 0.058(4) -0.012(3) -0.008(3) 0.008(2) C27 0.038(3) 0.029(2) 0.023(2) -0.0094(19) 0.003(2) -0.005(2) C28 0.036(3) 0.041(3) 0.029(3) -0.006(2) 0.000(2) -0.011(2) C29 0.035(3) 0.045(3) 0.038(3) -0.008(2) 0.007(2) 0.002(2) C30 0.055(4) 0.061(4) 0.043(3) -0.030(3) 0.017(3) -0.016(3) C31 0.017(2) 0.025(2) 0.018(2) -0.0085(17) -0.0017(16) 0.0001(17) C32 0.022(2) 0.025(2) 0.025(2) -0.0090(18) 0.0006(18) -0.0014(17) C33 0.026(2) 0.035(3) 0.034(3) -0.017(2) 0.003(2) -0.0067(19) C34 0.028(3) 0.045(3) 0.031(3) -0.018(2) 0.007(2) -0.013(2) C35 0.030(2) 0.045(3) 0.020(2) -0.007(2) 0.0006(19) -0.013(2) C36 0.021(2) 0.029(2) 0.023(2) -0.0038(19) -0.0007(18) -0.0034(18) C37 0.056(4) 0.067(4) 0.046(3) -0.034(3) 0.013(3) -0.030(3) C38 0.028(2) 0.023(2) 0.028(2) -0.0110(19) -0.0036(19) -0.0028(18) C39 0.038(3) 0.027(2) 0.035(3) -0.002(2) -0.010(2) -0.002(2) C40 0.026(2) 0.029(2) 0.032(3) -0.009(2) 0.003(2) -0.0098(19) C41 0.048(3) 0.029(3) 0.044(3) -0.014(2) 0.001(2) -0.006(2) C42 0.035(3) 0.034(3) 0.022(2) -0.006(2) 0.001(2) -0.008(2) C43 0.041(3) 0.033(3) 0.041(3) -0.008(2) -0.005(2) -0.016(2) C44 0.047(3) 0.025(3) 0.041(3) 0.001(2) 0.003(2) -0.003(2) C45 0.076(4) 0.047(3) 0.035(3) -0.010(3) 0.015(3) -0.031(3) C46 0.034(3) 0.022(2) 0.021(2) -0.0069(18) 0.0071(19) -0.0065(19) C47 0.038(3) 0.025(2) 0.031(3) -0.003(2) -0.002(2) -0.005(2) C48 0.029(3) 0.032(3) 0.044(3) -0.007(2) 0.005(2) -0.017(2) C49 0.042(3) 0.031(3) 0.038(3) -0.005(2) -0.012(2) -0.001(2) C50 0.044(3) 0.021(2) 0.042(3) -0.005(2) 0.003(2) -0.003(2) C51 0.024(2) 0.024(2) 0.020(2) -0.0069(18) 0.0002(18) -0.0014(17) C52 0.022(2) 0.025(2) 0.026(2) -0.0083(19) -0.0048(18) 0.0005(17) C53 0.025(2) 0.029(2) 0.031(3) -0.015(2) -0.0013(19) 0.0008(18) C54 0.025(2) 0.036(3) 0.027(2) -0.016(2) 0.0037(19) -0.0058(19) C55 0.030(2) 0.035(3) 0.020(2) -0.0071(19) 0.0021(19) -0.008(2) C56 0.022(2) 0.025(2) 0.025(2) -0.0076(18) -0.0012(18) -0.0034(17) C57 0.051(3) 0.052(3) 0.033(3) -0.027(2) 0.007(2) -0.018(3) C58 0.035(3) 0.020(2) 0.028(2) -0.0049(18) -0.001(2) -0.0032(19) C59 0.035(3) 0.037(3) 0.029(2) -0.013(2) 0.005(2) -0.011(2) C60 0.046(3) 0.023(2) 0.028(2) -0.0009(19) -0.005(2) -0.005(2) C61 0.054(3) 0.023(2) 0.038(3) -0.008(2) -0.002(2) -0.007(2) C62 0.041(3) 0.025(2) 0.024(2) -0.0036(19) 0.000(2) -0.010(2) C63 0.039(3) 0.037(3) 0.038(3) -0.010(2) -0.003(2) -0.016(2) C64 0.045(3) 0.025(2) 0.036(3) -0.001(2) -0.002(2) -0.002(2) C65 0.070(4) 0.038(3) 0.032(3) -0.005(2) 0.009(3) -0.023(3) C66 0.026(2) 0.029(2) 0.019(2) -0.0005(18) -0.0025(18) -0.0055(18) C67 0.029(2) 0.027(2) 0.021(2) 0.0058(18) -0.0035(19) -0.0030(19) C68 0.024(2) 0.032(3) 0.027(2) 0.003(2) -0.0042(19) -0.0063(19) C69 0.039(3) 0.029(2) 0.023(2) 0.0017(19) -0.008(2) -0.011(2) C70 0.047(3) 0.025(2) 0.023(2) -0.0035(19) -0.003(2) -0.005(2) C71 0.029(2) 0.027(2) 0.020(2) -0.0033(18) -0.0033(18) -0.0038(18) C72 0.044(3) 0.035(3) 0.038(3) 0.001(2) -0.016(2) -0.015(2) C73 0.023(2) 0.033(3) 0.025(2) -0.001(2) -0.0018(19) 0.0036(19) C74 0.030(3) 0.035(3) 0.028(2) -0.007(2) 0.003(2) 0.004(2) C75 0.052(3) 0.030(3) 0.029(3) -0.004(2) -0.004(2) 0.001(2) C76 0.033(3) 0.044(3) 0.045(3) -0.006(3) -0.001(2) 0.011(2) C77 0.028(2) 0.044(3) 0.028(2) -0.018(2) 0.005(2) -0.005(2) C78 0.031(3) 0.043(3) 0.040(3) -0.006(2) -0.001(2) 0.006(2) C79 0.036(3) 0.051(3) 0.029(3) -0.001(2) 0.000(2) -0.007(2) C80 0.049(3) 0.069(4) 0.052(4) -0.035(3) 0.011(3) -0.011(3) C81 0.023(2) 0.023(2) 0.028(2) -0.0109(18) 0.0017(18) -0.0018(17) C82 0.025(2) 0.027(2) 0.027(2) -0.0030(19) 0.0046(19) -0.0003(18) C83 0.027(2) 0.027(2) 0.038(3) -0.008(2) 0.003(2) -0.0030(19) C84 0.025(2) 0.037(3) 0.034(3) -0.007(2) -0.003(2) -0.003(2) C85 0.027(2) 0.033(3) 0.028(2) -0.008(2) -0.0042(19) -0.0074(19) C86 0.025(2) 0.026(2) 0.029(2) -0.0076(19) -0.0002(19) -0.0014(18) C87 0.040(3) 0.045(3) 0.046(3) -0.006(3) -0.004(2) -0.020(2) C88 0.024(2) 0.032(3) 0.035(3) 0.004(2) -0.004(2) -0.0038(19) C89 0.064(4) 0.040(3) 0.067(4) -0.001(3) -0.012(3) -0.003(3) C90 0.047(3) 0.067(4) 0.041(3) 0.012(3) 0.004(3) -0.005(3) C91 0.049(4) 0.064(4) 0.065(4) 0.026(3) -0.024(3) -0.019(3) C92 0.029(2) 0.033(3) 0.029(3) -0.001(2) 0.000(2) -0.003(2) C93 0.035(3) 0.043(3) 0.032(3) -0.003(2) -0.006(2) 0.004(2) C94 0.046(3) 0.046(3) 0.034(3) 0.007(2) -0.005(2) -0.011(2) C95 0.036(3) 0.047(3) 0.028(3) -0.007(2) 0.004(2) -0.005(2) C96 0.040(3) 0.024(2) 0.018(2) -0.0041(18) -0.0006(19) -0.005(2) C97 0.056(4) 0.046(3) 0.038(3) -0.010(3) -0.012(3) -0.014(3) C98 0.042(3) 0.035(3) 0.051(3) -0.003(2) 0.003(3) 0.005(2) C99 0.052(3) 0.025(3) 0.044(3) -0.009(2) 0.002(3) 0.000(2) C100 0.041(3) 0.047(3) 0.074(4) -0.020(3) 0.008(3) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O3 2.162(3) . ? Nd1 O1 2.195(3) . ? Nd1 O2 2.218(3) . ? Nd1 N1 2.487(3) . ? Nd2 O4 2.179(3) . ? Nd2 O6 2.186(3) . ? Nd2 O5 2.201(3) . ? Nd2 N4 2.462(4) . ? N1 C46 1.321(5) . ? N1 H1 0.8800 . ? N2 C46 1.353(6) . ? N2 C47 1.451(5) . ? N2 C48 1.466(5) . ? N3 C46 1.370(5) . ? N3 C49 1.451(6) . ? N3 C50 1.463(6) . ? N4 C96 1.324(5) . ? N4 H4 0.8800 . ? N5 C96 1.356(6) . ? N5 C98 1.454(6) . ? N5 C97 1.454(6) . ? N6 C96 1.358(6) . ? N6 C100 1.455(6) . ? N6 C99 1.457(6) . ? O1 C1 1.360(5) . ? O2 C16 1.356(5) . ? O3 C31 1.357(5) . ? O4 C51 1.354(5) . ? O5 C66 1.358(5) . ? O6 C81 1.355(5) . ? C1 C6 1.420(6) . ? C1 C2 1.430(6) . ? C2 C3 1.391(6) . ? C2 C8 1.548(6) . ? C3 C4 1.384(6) . ? C3 H3 0.9500 . ? C4 C5 1.392(6) . ? C4 C7 1.509(6) . ? C5 C6 1.402(6) . ? C5 H5 0.9500 . ? C6 C12 1.540(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C10 1.523(6) . ? C8 C9 1.542(6) . ? C8 C11 1.546(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.529(7) . ? C12 C15 1.532(6) . ? C12 C14 1.540(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.414(6) . ? C16 C21 1.431(6) . ? C17 C18 1.389(6) . ? C17 C23 1.546(6) . ? C18 C19 1.388(7) . ? C18 H18 0.9500 . ? C19 C20 1.391(7) . ? C19 C22 1.521(6) . ? C20 C21 1.394(6) . ? C20 H20 0.9500 . ? C21 C27 1.530(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C25 1.531(6) . ? C23 C24 1.538(6) . ? C23 C26 1.550(6) . ? 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 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.528(6) . ? C27 C30 1.530(6) . ? C27 C28 1.541(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.424(6) . ? C31 C36 1.425(6) . ? C32 C33 1.388(6) . ? C32 C38 1.547(6) . ? C33 C34 1.365(6) . ? C33 H33 0.9500 . ? C34 C35 1.374(6) . ? C34 C37 1.515(6) . ? C35 C36 1.400(6) . ? C35 H35 0.9500 . ? C36 C42 1.543(6) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C40 1.538(6) . ? C38 C39 1.539(6) . ? C38 C41 1.542(6) . ? 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 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.526(6) . ? C42 C44 1.529(6) . ? C42 C45 1.544(6) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.415(6) . ? C51 C56 1.421(6) . ? C52 C53 1.404(6) . ? C52 C58 1.545(6) . ? C53 C54 1.372(6) . ? C53 H53 0.9500 . ? C54 C55 1.384(6) . ? C54 C57 1.511(6) . ? C55 C56 1.391(6) . ? C55 H55 0.9500 . ? C56 C62 1.538(6) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C61 1.537(6) . ? C58 C59 1.537(6) . ? C58 C60 1.539(6) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C65 1.521(6) . ? C62 C63 1.538(6) . ? C62 C64 1.549(6) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C71 1.416(6) . ? C66 C67 1.428(6) . ? C67 C68 1.403(6) . ? C67 C73 1.539(6) . ? C68 C69 1.391(6) . ? C68 H68 0.9500 . ? C69 C70 1.378(6) . ? C69 C72 1.507(6) . ? C70 C71 1.404(6) . ? C70 H70 0.9500 . ? C71 C77 1.530(6) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C74 1.532(6) . ? C73 C75 1.532(6) . ? C73 C76 1.536(6) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C78 1.530(6) . ? C77 C80 1.533(6) . ? C77 C79 1.542(7) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 C82 1.427(6) . ? C81 C86 1.430(6) . ? C82 C83 1.390(6) . ? C82 C92 1.535(6) . ? C83 C84 1.383(6) . ? C83 H83 0.9500 . ? C84 C85 1.380(6) . ? C84 C87 1.510(6) . ? C85 C86 1.387(6) . ? C85 H85 0.9500 . ? C86 C88 1.549(6) . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 C91 1.511(7) . ? C88 C90 1.521(7) . ? C88 C89 1.553(7) . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C92 C95 1.532(6) . ? C92 C94 1.534(6) . ? C92 C93 1.553(6) . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? C100 H10D 0.9800 . ? C100 H10E 0.9800 . ? C100 H10F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Nd1 O1 111.54(10) . . ? O3 Nd1 O2 115.70(10) . . ? O1 Nd1 O2 115.23(10) . . ? O3 Nd1 N1 102.38(11) . . ? O1 Nd1 N1 99.32(11) . . ? O2 Nd1 N1 110.58(11) . . ? O4 Nd2 O6 111.56(11) . . ? O4 Nd2 O5 120.75(10) . . ? O6 Nd2 O5 113.84(11) . . ? O4 Nd2 N4 106.30(11) . . ? O6 Nd2 N4 98.36(12) . . ? O5 Nd2 N4 102.63(12) . . ? C46 N1 Nd1 144.7(3) . . ? C46 N1 H1 107.6 . . ? Nd1 N1 H1 107.6 . . ? C46 N2 C47 119.5(4) . . ? C46 N2 C48 122.5(4) . . ? C47 N2 C48 114.6(4) . . ? C46 N3 C49 119.9(4) . . ? C46 N3 C50 121.5(4) . . ? C49 N3 C50 114.7(4) . . ? C96 N4 Nd2 138.8(3) . . ? C96 N4 H4 110.6 . . ? Nd2 N4 H4 110.6 . . ? C96 N5 C98 120.4(4) . . ? C96 N5 C97 122.5(4) . . ? C98 N5 C97 114.7(4) . . ? C96 N6 C100 118.8(4) . . ? C96 N6 C99 122.7(4) . . ? C100 N6 C99 114.1(4) . . ? C1 O1 Nd1 153.4(3) . . ? C16 O2 Nd1 145.5(2) . . ? C31 O3 Nd1 169.5(3) . . ? C51 O4 Nd2 169.0(3) . . ? C66 O5 Nd2 151.6(3) . . ? C81 O6 Nd2 153.8(3) . . ? O1 C1 C6 120.3(4) . . ? O1 C1 C2 119.6(4) . . ? C6 C1 C2 120.0(4) . . ? C3 C2 C1 118.2(4) . . ? C3 C2 C8 119.3(4) . . ? C1 C2 C8 122.5(4) . . ? C4 C3 C2 123.2(4) . . ? C4 C3 H3 118.4 . . ? C2 C3 H3 118.4 . . ? C3 C4 C5 117.3(4) . . ? C3 C4 C7 121.3(4) . . ? C5 C4 C7 121.3(4) . . ? C4 C5 C6 123.5(4) . . ? C4 C5 H5 118.3 . . ? C6 C5 H5 118.3 . . ? C5 C6 C1 117.5(4) . . ? C5 C6 C12 118.8(4) . . ? C1 C6 C12 123.5(4) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C10 C8 C9 111.8(4) . . ? C10 C8 C11 105.9(4) . . ? C9 C8 C11 106.7(4) . . ? C10 C8 C2 111.0(4) . . ? C9 C8 C2 109.2(4) . . ? C11 C8 C2 112.2(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C15 107.3(4) . . ? C13 C12 C14 109.5(4) . . ? C15 C12 C14 106.2(4) . . ? C13 C12 C6 107.9(4) . . ? C15 C12 C6 112.2(4) . . ? C14 C12 C6 113.5(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O2 C16 C17 121.0(4) . . ? O2 C16 C21 119.2(4) . . ? C17 C16 C21 119.8(4) . . ? C18 C17 C16 118.3(4) . . ? C18 C17 C23 120.1(4) . . ? C16 C17 C23 121.5(4) . . ? C19 C18 C17 122.6(4) . . ? C19 C18 H18 118.7 . . ? C17 C18 H18 118.7 . . ? C18 C19 C20 118.0(4) . . ? C18 C19 C22 121.2(5) . . ? C20 C19 C22 120.7(4) . . ? C19 C20 C21 122.5(4) . . ? C19 C20 H20 118.8 . . ? C21 C20 H20 118.8 . . ? C20 C21 C16 117.7(4) . . ? C20 C21 C27 120.3(4) . . ? C16 C21 C27 121.8(4) . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C25 C23 C24 110.4(4) . . ? C25 C23 C17 112.3(3) . . ? C24 C23 C17 108.8(4) . . ? C25 C23 C26 105.9(4) . . ? C24 C23 C26 107.6(4) . . ? C17 C23 C26 111.7(4) . . ? 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 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C30 105.7(4) . . ? C29 C27 C21 114.3(4) . . ? C30 C27 C21 111.4(4) . . ? C29 C27 C28 109.9(4) . . ? C30 C27 C28 107.2(4) . . ? C21 C27 C28 108.2(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O3 C31 C32 120.3(4) . . ? O3 C31 C36 120.4(4) . . ? C32 C31 C36 119.3(4) . . ? C33 C32 C31 118.2(4) . . ? C33 C32 C38 119.6(4) . . ? C31 C32 C38 122.2(4) . . ? C34 C33 C32 123.4(4) . . ? C34 C33 H33 118.3 . . ? C32 C33 H33 118.3 . . ? C33 C34 C35 118.1(4) . . ? C33 C34 C37 120.2(4) . . ? C35 C34 C37 121.8(4) . . ? C34 C35 C36 123.0(4) . . ? C34 C35 H35 118.5 . . ? C36 C35 H35 118.5 . . ? C35 C36 C31 117.8(4) . . ? C35 C36 C42 118.9(4) . . ? C31 C36 C42 123.3(4) . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C40 C38 C39 112.9(4) . . ? C40 C38 C41 106.1(4) . . ? C39 C38 C41 106.0(4) . . ? C40 C38 C32 109.5(3) . . ? C39 C38 C32 110.8(4) . . ? C41 C38 C32 111.5(4) . . ? 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 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C44 110.2(4) . . ? C43 C42 C36 110.4(4) . . ? C44 C42 C36 110.3(4) . . ? C43 C42 C45 106.7(4) . . ? C44 C42 C45 107.2(4) . . ? C36 C42 C45 112.0(4) . . ? 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 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 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N1 C46 N2 120.1(4) . . ? N1 C46 N3 123.2(4) . . ? N2 C46 N3 116.7(4) . . ? N2 C47 H47A 109.5 . . ? N2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N2 C48 H48A 109.5 . . ? N2 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N2 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N3 C49 H49A 109.5 . . ? N3 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N3 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N3 C50 H50A 109.5 . . ? N3 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N3 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O4 C51 C52 120.1(4) . . ? O4 C51 C56 120.0(4) . . ? C52 C51 C56 119.9(4) . . ? C53 C52 C51 118.3(4) . . ? C53 C52 C58 118.4(4) . . ? C51 C52 C58 123.2(4) . . ? C54 C53 C52 123.0(4) . . ? C54 C53 H53 118.5 . . ? C52 C53 H53 118.5 . . ? C53 C54 C55 117.1(4) . . ? C53 C54 C57 121.2(4) . . ? C55 C54 C57 121.6(4) . . ? C54 C55 C56 124.0(4) . . ? C54 C55 H55 118.0 . . ? C56 C55 H55 118.0 . . ? C55 C56 C51 117.5(4) . . ? C55 C56 C62 118.8(4) . . ? C51 C56 C62 123.7(4) . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C61 C58 C59 105.4(4) . . ? C61 C58 C60 106.8(4) . . ? C59 C58 C60 111.6(4) . . ? C61 C58 C52 112.6(4) . . ? C59 C58 C52 109.9(4) . . ? C60 C58 C52 110.5(4) . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C58 C61 H61A 109.5 . . ? C58 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C58 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C65 C62 C63 106.4(4) . . ? C65 C62 C56 113.3(4) . . ? C63 C62 C56 108.7(4) . . ? C65 C62 C64 107.1(4) . . ? C63 C62 C64 110.4(4) . . ? C56 C62 C64 110.8(4) . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C62 C65 H65A 109.5 . . ? C62 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C62 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? O5 C66 C71 120.4(4) . . ? O5 C66 C67 120.3(4) . . ? C71 C66 C67 119.4(4) . . ? C68 C67 C66 117.9(4) . . ? C68 C67 C73 120.1(4) . . ? C66 C67 C73 121.9(4) . . ? C69 C68 C67 122.9(4) . . ? C69 C68 H68 118.5 . . ? C67 C68 H68 118.5 . . ? C70 C69 C68 117.3(4) . . ? C70 C69 C72 121.3(4) . . ? C68 C69 C72 121.1(4) . . ? C69 C70 C71 123.2(4) . . ? C69 C70 H70 118.4 . . ? C71 C70 H70 118.4 . . ? C70 C71 C66 118.1(4) . . ? C70 C71 C77 119.1(4) . . ? C66 C71 C77 122.5(4) . . ? C69 C72 H72A 109.5 . . ? C69 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C69 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C74 C73 C75 110.0(4) . . ? C74 C73 C76 105.8(4) . . ? C75 C73 C76 107.8(4) . . ? C74 C73 C67 111.9(4) . . ? C75 C73 C67 109.7(4) . . ? C76 C73 C67 111.6(4) . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C73 C75 H75A 109.5 . . ? C73 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C73 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C73 C76 H76A 109.5 . . ? C73 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C73 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C78 C77 C71 114.3(4) . . ? C78 C77 C80 106.0(4) . . ? C71 C77 C80 113.0(4) . . ? C78 C77 C79 109.0(4) . . ? C71 C77 C79 107.6(4) . . ? C80 C77 C79 106.7(4) . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C77 C79 H79A 109.5 . . ? C77 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C77 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C77 C80 H80A 109.5 . . ? C77 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C77 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? O6 C81 C82 120.5(4) . . ? O6 C81 C86 120.4(4) . . ? C82 C81 C86 119.1(4) . . ? C83 C82 C81 118.5(4) . . ? C83 C82 C92 118.8(4) . . ? C81 C82 C92 122.6(4) . . ? C84 C83 C82 122.8(4) . . ? C84 C83 H83 118.6 . . ? C82 C83 H83 118.6 . . ? C85 C84 C83 117.9(4) . . ? C85 C84 C87 121.2(4) . . ? C83 C84 C87 120.9(4) . . ? C84 C85 C86 123.2(4) . . ? C84 C85 H85 118.4 . . ? C86 C85 H85 118.4 . . ? C85 C86 C81 118.3(4) . . ? C85 C86 C88 118.6(4) . . ? C81 C86 C88 123.1(4) . . ? C84 C87 H87A 109.5 . . ? C84 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C84 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C91 C88 C90 108.2(5) . . ? C91 C88 C86 112.5(4) . . ? C90 C88 C86 111.5(4) . . ? C91 C88 C89 105.0(4) . . ? C90 C88 C89 109.7(4) . . ? C86 C88 C89 109.8(4) . . ? C88 C89 H89A 109.5 . . ? C88 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C88 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C88 C90 H90A 109.5 . . ? C88 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C88 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C88 C91 H91A 109.5 . . ? C88 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C88 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C95 C92 C94 107.3(4) . . ? C95 C92 C82 109.3(4) . . ? C94 C92 C82 112.7(4) . . ? C95 C92 C93 108.1(4) . . ? C94 C92 C93 105.7(4) . . ? C82 C92 C93 113.4(4) . . ? C92 C93 H93A 109.5 . . ? C92 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C92 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C92 C94 H94A 109.5 . . ? C92 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C92 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C92 C95 H95A 109.5 . . ? C92 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C92 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? N4 C96 N5 119.5(4) . . ? N4 C96 N6 123.3(4) . . ? N5 C96 N6 117.1(4) . . ? N5 C97 H97A 109.5 . . ? N5 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? N5 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? N5 C98 H98A 109.5 . . ? N5 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? N5 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? N6 C99 H99A 109.5 . . ? N6 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? N6 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? N6 C100 H10D 109.5 . . ? N6 C100 H10E 109.5 . . ? H10D C100 H10E 109.5 . . ? N6 C100 H10F 109.5 . . ? H10D C100 H10F 109.5 . . ? H10E C100 H10F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.685 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.080 #===END data_jab023 _database_code_depnum_ccdc_archive 'CCDC 722743' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(La(DBP)3(H-TMG)) (6)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H92 La N3 O5' _chemical_formula_weight 1014.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.3312(16) _cell_length_b 19.335(2) _cell_length_c 20.493(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.958(2) _cell_angle_gamma 90.00 _cell_volume 5486.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5715 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 25.05 _exptl_crystal_description Irregular _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 0.825 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6040 _exptl_absorpt_correction_T_max 0.8394 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_reflns_number 43406 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.05 _reflns_number_total 9700 _reflns_number_gt 8172 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. The solvent electron density was modeled using PLATON/SQUEEZE (ver. 01-11-99), which located a potential solvent volume of 1218.2 \%A3 and an electron count of 302 electrons/cell, consistent with eight tetrahyrdrofuran molecules/cell.Eight molecule were added to the contents of the unit cell during the final refinement to properly calculate the crystal data. N1 was found to be disordered and was modeled in two positions. ; _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^)+(0.0784P)^2^+38.3417P] 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 9700 _refine_ls_number_parameters 519 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1503 _refine_ls_wR_factor_gt 0.1446 _refine_ls_goodness_of_fit_ref 0.886 _refine_ls_restrained_S_all 0.886 _refine_ls_shift/su_max 4.445 _refine_ls_shift/su_mean 0.033 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.60033(2) 0.202426(14) 0.748154(13) 0.02278(11) Uani 1 1 d . . . N1 N 0.7639(5) 0.2415(4) 0.7406(4) 0.041(3) Uani 0.633(15) 1 d P A 1 N1A N 0.7778(8) 0.2062(5) 0.7860(5) 0.020(4) Uani 0.367(15) 1 d P A 2 N2 N 0.9191(7) 0.2282(3) 0.8343(4) 0.088(3) Uani 1 1 d . A . N3 N 0.8873(6) 0.3072(3) 0.7507(3) 0.076(2) Uani 1 1 d . A . O1 O 0.5672(3) 0.09292(18) 0.77204(19) 0.0350(8) Uani 1 1 d . A . O2 O 0.5642(2) 0.27573(18) 0.82184(17) 0.0281(7) Uani 1 1 d . A . O3 O 0.5603(3) 0.23352(18) 0.63785(17) 0.0300(8) Uani 1 1 d . A . C1 C 0.5206(4) 0.0427(3) 0.7970(3) 0.0338(12) Uani 1 1 d . . . C2 C 0.4347(4) 0.0134(3) 0.7552(3) 0.0356(12) Uani 1 1 d . A . C3 C 0.3826(4) -0.0324(3) 0.7843(3) 0.0400(13) Uani 1 1 d . . . H3 H 0.3238 -0.0509 0.7574 0.048 Uiso 1 1 calc R A . C4 C 0.4136(5) -0.0516(4) 0.8513(4) 0.0537(17) Uani 1 1 d . A . H4 H 0.3757 -0.0818 0.8706 0.064 Uiso 1 1 calc R . . C5 C 0.5004(5) -0.0263(4) 0.8896(4) 0.0577(18) Uani 1 1 d . . . H5 H 0.5228 -0.0412 0.9351 0.069 Uiso 1 1 calc R A . C6 C 0.5565(4) 0.0199(3) 0.8643(3) 0.0433(14) Uani 1 1 d . A . C7 C 0.4002(5) 0.0283(3) 0.6796(3) 0.0469(15) Uani 1 1 d . . . C8 C 0.3071(6) -0.0113(4) 0.6455(3) 0.063(2) Uani 1 1 d . A . H8A H 0.3194 -0.0612 0.6500 0.095 Uiso 1 1 calc R . . H8B H 0.2868 0.0009 0.5975 0.095 Uiso 1 1 calc R . . H8C H 0.2560 0.0010 0.6672 0.095 Uiso 1 1 calc R . . C9 C 0.3772(6) 0.1059(3) 0.6652(3) 0.064(2) Uani 1 1 d . A . H9A H 0.3471 0.1124 0.6169 0.096 Uiso 1 1 calc R . . H9B H 0.4372 0.1327 0.6782 0.096 Uiso 1 1 calc R . . H9C H 0.3329 0.1217 0.6914 0.096 Uiso 1 1 calc R . . C10 C 0.4778(7) 0.0042(4) 0.6453(4) 0.083(3) Uani 1 1 d . A . H10A H 0.4855 -0.0461 0.6500 0.124 Uiso 1 1 calc R . . H10B H 0.5393 0.0268 0.6667 0.124 Uiso 1 1 calc R . . H10C H 0.4582 0.0164 0.5973 0.124 Uiso 1 1 calc R . . C11 C 0.6547(5) 0.0439(4) 0.9092(4) 0.0549(18) Uani 1 1 d . . . C12 C 0.6807(6) 0.0071(4) 0.9791(4) 0.077(3) Uani 1 1 d . A . H12A H 0.7413 0.0260 1.0071 0.116 Uiso 1 1 calc R . . H12B H 0.6881 -0.0426 0.9727 0.116 Uiso 1 1 calc R . . H12C H 0.6289 0.0148 1.0016 0.116 Uiso 1 1 calc R . . C13 C 0.7347(5) 0.0260(4) 0.8743(5) 0.070(2) Uani 1 1 d . A . H13A H 0.7205 0.0482 0.8299 0.106 Uiso 1 1 calc R . . H13B H 0.7374 -0.0243 0.8688 0.106 Uiso 1 1 calc R . . H13C H 0.7969 0.0426 0.9020 0.106 Uiso 1 1 calc R . . C14 C 0.6535(4) 0.1211(3) 0.9235(3) 0.0519(16) Uani 1 1 d . A . H14A H 0.6439 0.1468 0.8811 0.078 Uiso 1 1 calc R . . H14B H 0.7151 0.1346 0.9544 0.078 Uiso 1 1 calc R . . H14C H 0.6006 0.1314 0.9443 0.078 Uiso 1 1 calc R . . C15 C 0.5304(4) 0.3186(3) 0.8622(3) 0.0292(11) Uani 1 1 d . . . C16 C 0.5937(4) 0.3662(3) 0.9050(3) 0.0354(12) Uani 1 1 d . A . C17 C 0.5557(5) 0.4092(3) 0.9457(3) 0.0480(16) Uani 1 1 d . . . H17 H 0.5977 0.4403 0.9753 0.058 Uiso 1 1 calc R A . C18 C 0.4596(5) 0.4086(3) 0.9450(3) 0.0561(18) Uani 1 1 d . A . H18 H 0.4356 0.4397 0.9726 0.067 Uiso 1 1 calc R . . C19 C 0.3980(5) 0.3620(3) 0.9035(3) 0.0470(15) Uani 1 1 d . . . H19 H 0.3318 0.3607 0.9037 0.056 Uiso 1 1 calc R A . C20 C 0.4315(4) 0.3172(3) 0.8617(3) 0.0334(12) Uani 1 1 d . A . C21 C 0.7023(4) 0.3697(3) 0.9086(3) 0.0413(14) Uani 1 1 d . . . C22 C 0.7505(5) 0.3000(3) 0.9319(3) 0.0472(15) Uani 1 1 d . A . H22A H 0.7373 0.2868 0.9748 0.071 Uiso 1 1 calc R . . H22B H 0.8204 0.3041 0.9381 0.071 Uiso 1 1 calc R . . H22C H 0.7247 0.2647 0.8977 0.071 Uiso 1 1 calc R . . C23 C 0.7177(5) 0.3908(4) 0.8397(3) 0.0514(16) Uani 1 1 d . A . H23A H 0.6885 0.3561 0.8057 0.077 Uiso 1 1 calc R . . H23B H 0.7871 0.3939 0.8431 0.077 Uiso 1 1 calc R . . H23C H 0.6874 0.4358 0.8263 0.077 Uiso 1 1 calc R . . C24 C 0.7553(5) 0.4233(4) 0.9600(4) 0.0597(19) Uani 1 1 d . A . H24A H 0.7294 0.4695 0.9461 0.090 Uiso 1 1 calc R . . H24B H 0.8244 0.4224 0.9621 0.090 Uiso 1 1 calc R . . H24C H 0.7461 0.4125 1.0046 0.090 Uiso 1 1 calc R . . C25 C 0.3604(4) 0.2649(3) 0.8172(3) 0.0328(12) Uani 1 1 d . . . C26 C 0.3526(4) 0.2783(3) 0.7420(3) 0.0360(12) Uani 1 1 d . A . H26A H 0.3080 0.2447 0.7145 0.054 Uiso 1 1 calc R . . H26B H 0.4165 0.2733 0.7335 0.054 Uiso 1 1 calc R . . H26C H 0.3284 0.3252 0.7301 0.054 Uiso 1 1 calc R . . C27 C 0.3919(4) 0.1905(3) 0.8381(3) 0.0363(12) Uani 1 1 d . A . H27A H 0.3876 0.1823 0.8844 0.054 Uiso 1 1 calc R . . H27B H 0.4587 0.1836 0.8357 0.054 Uiso 1 1 calc R . . H27C H 0.3495 0.1580 0.8075 0.054 Uiso 1 1 calc R . . C28 C 0.2571(4) 0.2723(4) 0.8249(4) 0.0482(15) Uani 1 1 d . A . H28A H 0.2330 0.3188 0.8112 0.072 Uiso 1 1 calc R . . H28B H 0.2572 0.2647 0.8722 0.072 Uiso 1 1 calc R . . H28C H 0.2153 0.2380 0.7964 0.072 Uiso 1 1 calc R . . C29 C 0.5912(4) 0.2651(3) 0.5889(3) 0.0327(12) Uani 1 1 d . . . C30 C 0.6473(4) 0.2284(3) 0.5523(3) 0.0363(12) Uani 1 1 d . A . C31 C 0.6926(5) 0.2662(3) 0.5115(3) 0.0437(14) Uani 1 1 d . . . H31 H 0.7341 0.2426 0.4895 0.052 Uiso 1 1 calc R A . C32 C 0.6800(5) 0.3361(3) 0.5018(3) 0.0490(16) Uani 1 1 d . A . H32 H 0.7149 0.3610 0.4758 0.059 Uiso 1 1 calc R . . C33 C 0.6155(5) 0.3695(3) 0.5306(3) 0.0428(14) Uani 1 1 d . . . H33 H 0.6026 0.4171 0.5210 0.051 Uiso 1 1 calc R A . C34 C 0.5683(4) 0.3358(3) 0.5733(3) 0.0368(13) Uani 1 1 d . A . C35 C 0.6496(5) 0.1488(3) 0.5521(3) 0.0469(15) Uani 1 1 d . . . C36 C 0.5465(6) 0.1222(3) 0.5260(3) 0.061(2) Uani 1 1 d . A . H36A H 0.5197 0.1385 0.4797 0.091 Uiso 1 1 calc R . . H36B H 0.5069 0.1396 0.5549 0.091 Uiso 1 1 calc R . . H36C H 0.5467 0.0716 0.5266 0.091 Uiso 1 1 calc R . . C37 C 0.7073(7) 0.1221(4) 0.5038(4) 0.070(2) Uani 1 1 d . A . H37A H 0.6969 0.0723 0.4970 0.105 Uiso 1 1 calc R . . H37B H 0.7762 0.1312 0.5232 0.105 Uiso 1 1 calc R . . H37C H 0.6858 0.1460 0.4603 0.105 Uiso 1 1 calc R . . C38 C 0.6955(6) 0.1171(3) 0.6224(3) 0.0551(18) Uani 1 1 d . A . H38A H 0.6519 0.1236 0.6517 0.083 Uiso 1 1 calc R . . H38B H 0.7572 0.1400 0.6425 0.083 Uiso 1 1 calc R . . H38C H 0.7065 0.0675 0.6175 0.083 Uiso 1 1 calc R . . C39 C 0.4934(4) 0.3743(3) 0.6011(3) 0.0404(13) Uani 1 1 d . . . C40 C 0.4685(5) 0.4458(3) 0.5675(4) 0.0555(17) Uani 1 1 d . A . H40A H 0.4148 0.4662 0.5823 0.083 Uiso 1 1 calc R . . H40B H 0.4498 0.4404 0.5183 0.083 Uiso 1 1 calc R . . H40C H 0.5250 0.4761 0.5806 0.083 Uiso 1 1 calc R . . C41 C 0.5313(4) 0.3873(3) 0.6771(3) 0.0412(13) Uani 1 1 d . A . H41A H 0.4802 0.4083 0.6943 0.062 Uiso 1 1 calc R . . H41B H 0.5869 0.4186 0.6852 0.062 Uiso 1 1 calc R . . H41C H 0.5511 0.3434 0.7003 0.062 Uiso 1 1 calc R . . C42 C 0.3979(4) 0.3336(3) 0.5856(3) 0.0448(14) Uani 1 1 d . A . H42A H 0.4096 0.2873 0.6054 0.067 Uiso 1 1 calc R . . H42B H 0.3718 0.3298 0.5366 0.067 Uiso 1 1 calc R . . H42C H 0.3514 0.3579 0.6050 0.067 Uiso 1 1 calc R . . C43 C 0.8552(4) 0.2541(4) 0.7795(5) 0.064(2) Uani 1 1 d . . . C44 C 0.8847(16) 0.1658(8) 0.8592(13) 0.34(2) Uani 1 1 d . . . H44A H 0.8978 0.1261 0.8332 0.512 Uiso 1 1 calc R A . H44B H 0.8150 0.1696 0.8542 0.512 Uiso 1 1 calc R . . H44C H 0.9180 0.1596 0.9069 0.512 Uiso 1 1 calc R . . C45 C 0.9971(14) 0.2507(7) 0.8667(10) 0.275(17) Uani 1 1 d . . . H45A H 0.9893 0.2736 0.9076 0.413 Uiso 1 1 calc R A . H45B H 1.0216 0.2840 0.8391 0.413 Uiso 1 1 calc R . . H45C H 1.0431 0.2124 0.8793 0.413 Uiso 1 1 calc R . . C46 C 1.0034(6) 0.3035(5) 0.7476(5) 0.078(2) Uani 1 1 d . . . H46A H 1.0333 0.2613 0.7701 0.118 Uiso 1 1 calc R A . H46B H 1.0382 0.3440 0.7704 0.118 Uiso 1 1 calc R . . H46C H 1.0063 0.3030 0.7003 0.118 Uiso 1 1 calc R . . C47 C 0.8238(14) 0.3408(12) 0.6955(5) 0.312(17) Uani 1 1 d . . . H47A H 0.7618 0.3163 0.6835 0.468 Uiso 1 1 calc R A . H47B H 0.8521 0.3408 0.6567 0.468 Uiso 1 1 calc R . . H47C H 0.8136 0.3886 0.7079 0.468 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.02535(16) 0.02180(16) 0.02111(16) -0.00347(11) 0.00584(11) -0.00015(11) N1 0.036(4) 0.051(5) 0.038(5) -0.001(4) 0.013(3) -0.001(4) N1A 0.029(6) 0.016(6) 0.020(7) -0.002(5) 0.015(5) 0.002(4) N2 0.128(7) 0.055(4) 0.125(6) 0.058(4) 0.112(6) 0.052(4) N3 0.121(6) 0.051(4) 0.037(3) 0.001(3) -0.013(3) 0.042(4) O1 0.043(2) 0.0241(19) 0.043(2) -0.0028(16) 0.0193(18) -0.0030(16) O2 0.0292(18) 0.0281(18) 0.0268(18) -0.0073(14) 0.0070(14) 0.0025(15) O3 0.039(2) 0.0272(18) 0.0235(18) 0.0002(14) 0.0067(15) -0.0058(15) C1 0.036(3) 0.023(3) 0.046(3) -0.001(2) 0.017(2) 0.005(2) C2 0.046(3) 0.021(3) 0.043(3) -0.006(2) 0.018(3) 0.003(2) C3 0.038(3) 0.035(3) 0.049(3) 0.002(3) 0.014(3) -0.004(2) C4 0.047(4) 0.054(4) 0.060(4) 0.017(3) 0.015(3) -0.008(3) C5 0.049(4) 0.060(4) 0.058(4) 0.028(4) 0.005(3) 0.002(3) C6 0.038(3) 0.033(3) 0.056(4) 0.010(3) 0.007(3) 0.009(2) C7 0.069(4) 0.038(3) 0.038(3) -0.012(3) 0.019(3) -0.019(3) C8 0.093(6) 0.054(4) 0.041(4) -0.010(3) 0.016(4) -0.028(4) C9 0.098(6) 0.043(4) 0.036(3) 0.000(3) -0.008(4) -0.015(4) C10 0.141(8) 0.055(5) 0.078(5) -0.031(4) 0.075(6) -0.050(5) C11 0.036(3) 0.050(4) 0.070(5) 0.018(3) -0.002(3) 0.009(3) C12 0.059(5) 0.072(5) 0.084(6) 0.034(5) -0.011(4) 0.006(4) C13 0.036(4) 0.053(4) 0.118(7) 0.009(4) 0.011(4) 0.016(3) C14 0.036(3) 0.057(4) 0.054(4) 0.001(3) -0.006(3) 0.004(3) C15 0.037(3) 0.023(2) 0.027(3) -0.001(2) 0.008(2) 0.003(2) C16 0.047(3) 0.025(3) 0.030(3) -0.006(2) 0.003(2) 0.003(2) C17 0.065(4) 0.036(3) 0.037(3) -0.014(3) 0.002(3) 0.004(3) C18 0.073(5) 0.045(4) 0.049(4) -0.018(3) 0.015(3) 0.019(3) C19 0.051(4) 0.041(3) 0.051(4) -0.005(3) 0.017(3) 0.015(3) C20 0.041(3) 0.032(3) 0.029(3) 0.000(2) 0.013(2) 0.009(2) C21 0.047(3) 0.037(3) 0.034(3) -0.012(2) 0.000(3) -0.011(3) C22 0.038(3) 0.046(4) 0.048(4) -0.010(3) -0.004(3) 0.000(3) C23 0.060(4) 0.052(4) 0.041(3) -0.010(3) 0.011(3) -0.025(3) C24 0.066(5) 0.052(4) 0.053(4) -0.018(3) -0.001(3) -0.019(3) C25 0.027(3) 0.032(3) 0.040(3) -0.001(2) 0.010(2) 0.004(2) C26 0.026(3) 0.043(3) 0.035(3) 0.000(2) 0.002(2) 0.008(2) C27 0.034(3) 0.035(3) 0.043(3) 0.000(2) 0.015(2) -0.002(2) C28 0.031(3) 0.053(4) 0.064(4) -0.009(3) 0.019(3) 0.003(3) C29 0.036(3) 0.034(3) 0.025(3) -0.002(2) 0.002(2) -0.007(2) C30 0.045(3) 0.034(3) 0.028(3) -0.002(2) 0.006(2) -0.010(2) C31 0.053(4) 0.043(3) 0.037(3) -0.004(3) 0.017(3) -0.008(3) C32 0.058(4) 0.044(4) 0.045(4) 0.005(3) 0.015(3) -0.017(3) C33 0.053(4) 0.033(3) 0.043(3) 0.003(3) 0.013(3) -0.011(3) C34 0.040(3) 0.029(3) 0.037(3) 0.003(2) 0.002(2) -0.007(2) C35 0.077(5) 0.034(3) 0.035(3) -0.002(3) 0.023(3) 0.002(3) C36 0.105(6) 0.038(4) 0.037(3) -0.010(3) 0.014(4) -0.025(4) C37 0.133(8) 0.047(4) 0.046(4) 0.005(3) 0.049(5) 0.017(4) C38 0.088(5) 0.040(4) 0.042(4) 0.003(3) 0.026(4) 0.016(3) C39 0.043(3) 0.032(3) 0.043(3) 0.012(2) 0.006(3) -0.001(2) C40 0.061(4) 0.040(4) 0.065(4) 0.021(3) 0.015(4) 0.008(3) C41 0.042(3) 0.027(3) 0.052(4) 0.004(3) 0.008(3) 0.003(2) C42 0.039(3) 0.047(4) 0.045(3) 0.012(3) 0.004(3) -0.001(3) C43 0.026(3) 0.047(4) 0.119(7) -0.048(5) 0.022(4) -0.005(3) C44 0.43(3) 0.166(14) 0.63(4) 0.29(2) 0.49(3) 0.221(18) C45 0.26(2) 0.077(8) 0.31(2) 0.084(11) -0.24(2) -0.071(11) C46 0.056(5) 0.090(6) 0.084(6) 0.000(5) 0.006(4) -0.006(4) C47 0.36(2) 0.54(3) 0.043(6) 0.080(11) 0.061(10) 0.41(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O2 2.227(3) . ? La1 O1 2.251(3) . ? La1 O3 2.265(3) . ? La1 N1A 2.462(11) . ? La1 N1 2.506(8) . ? N1 C43 1.367(10) . ? N1A C43 1.477(12) . ? N2 C45 1.223(14) . ? N2 C43 1.349(12) . ? N2 C44 1.445(13) . ? N3 C43 1.324(11) . ? N3 C47 1.415(10) . ? N3 C46 1.683(11) . ? O1 C1 1.351(6) . ? O2 C15 1.346(6) . ? O3 C29 1.344(6) . ? C1 C6 1.413(8) . ? C1 C2 1.423(8) . ? C2 C3 1.388(8) . ? C2 C7 1.528(8) . ? C3 C4 1.380(9) . ? C3 H3 0.9500 . ? C4 C5 1.378(10) . ? C4 H4 0.9500 . ? C5 C6 1.388(9) . ? C5 H5 0.9500 . ? C6 C11 1.541(9) . ? C7 C10 1.534(10) . ? C7 C8 1.541(9) . ? C7 C9 1.548(9) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.522(10) . ? C11 C13 1.538(10) . ? C11 C12 1.556(10) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C20 1.416(8) . ? C15 C16 1.424(7) . ? C16 C17 1.387(8) . ? C16 C21 1.540(8) . ? C17 C18 1.373(10) . ? C17 H17 0.9500 . ? C18 C19 1.389(9) . ? C18 H18 0.9500 . ? C19 C20 1.388(8) . ? C19 H19 0.9500 . ? C20 C25 1.553(8) . ? C21 C22 1.533(8) . ? C21 C24 1.533(8) . ? C21 C23 1.539(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C28 1.535(7) . ? C25 C27 1.536(7) . ? C25 C26 1.538(8) . ? 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 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.422(8) . ? C29 C34 1.422(8) . ? C30 C31 1.392(8) . ? C30 C35 1.540(8) . ? C31 C32 1.371(9) . ? C31 H31 0.9500 . ? C32 C33 1.379(9) . ? C32 H32 0.9500 . ? C33 C34 1.398(8) . ? C33 H33 0.9500 . ? C34 C39 1.531(8) . ? C35 C36 1.524(10) . ? C35 C37 1.535(9) . ? C35 C38 1.547(9) . ? 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 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C41 1.532(8) . ? C39 C42 1.540(8) . ? C39 C40 1.544(8) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C44 H44A 0.9806 . ? C44 H44B 0.9806 . ? C44 H44C 0.9805 . ? C45 H45A 1.0087 . ? C45 H45B 1.0112 . ? C45 H45C 1.0046 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9802 . ? C47 H47B 0.9802 . ? C47 H47C 0.9802 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 La1 O1 110.60(13) . . ? O2 La1 O3 117.66(13) . . ? O1 La1 O3 116.95(13) . . ? O2 La1 N1A 99.8(2) . . ? O1 La1 N1A 102.6(3) . . ? O3 La1 N1A 106.3(3) . . ? O2 La1 N1 103.6(2) . . ? O1 La1 N1 123.4(2) . . ? O3 La1 N1 81.9(2) . . ? N1A La1 N1 26.2(3) . . ? C43 N1 La1 142.0(6) . . ? C43 N1A La1 136.8(7) . . ? C45 N2 C43 130.5(9) . . ? C45 N2 C44 116.9(15) . . ? C43 N2 C44 112.5(14) . . ? C43 N3 C47 119.1(14) . . ? C43 N3 C46 116.4(6) . . ? C47 N3 C46 115.3(10) . . ? C1 O1 La1 155.6(3) . . ? C15 O2 La1 172.7(3) . . ? C29 O3 La1 144.9(3) . . ? O1 C1 C6 120.2(5) . . ? O1 C1 C2 119.6(5) . . ? C6 C1 C2 120.2(5) . . ? C3 C2 C1 118.3(5) . . ? C3 C2 C7 119.1(5) . . ? C1 C2 C7 122.6(5) . . ? C4 C3 C2 121.9(6) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C5 C4 C3 118.8(6) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 122.7(6) . . ? C4 C5 H5 118.6 . . ? C6 C5 H5 118.6 . . ? C5 C6 C1 117.7(6) . . ? C5 C6 C11 119.9(6) . . ? C1 C6 C11 122.3(6) . . ? C2 C7 C10 108.9(6) . . ? C2 C7 C8 112.5(5) . . ? C10 C7 C8 106.6(6) . . ? C2 C7 C9 111.9(5) . . ? C10 C7 C9 110.5(6) . . ? C8 C7 C9 106.2(6) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C13 110.9(6) . . ? C14 C11 C6 110.8(5) . . ? C13 C11 C6 109.3(6) . . ? C14 C11 C12 106.4(7) . . ? C13 C11 C12 107.2(6) . . ? C6 C11 C12 112.1(6) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 C20 120.1(5) . . ? O2 C15 C16 120.2(5) . . ? C20 C15 C16 119.7(5) . . ? C17 C16 C15 118.1(5) . . ? C17 C16 C21 119.6(5) . . ? C15 C16 C21 122.2(5) . . ? C18 C17 C16 122.5(6) . . ? C18 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? C17 C18 C19 119.4(6) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C20 C19 C18 121.1(6) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C15 119.3(5) . . ? C19 C20 C25 119.3(5) . . ? C15 C20 C25 121.4(4) . . ? C22 C21 C24 106.0(5) . . ? C22 C21 C23 111.0(5) . . ? C24 C21 C23 106.7(5) . . ? C22 C21 C16 110.2(5) . . ? C24 C21 C16 112.2(5) . . ? C23 C21 C16 110.5(5) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C28 C25 C27 106.2(5) . . ? C28 C25 C26 105.4(5) . . ? C27 C25 C26 112.1(5) . . ? C28 C25 C20 112.5(5) . . ? C27 C25 C20 110.1(4) . . ? C26 C25 C20 110.3(5) . . ? 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 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C29 C30 120.4(5) . . ? O3 C29 C34 120.2(5) . . ? C30 C29 C34 119.4(5) . . ? C31 C30 C29 118.0(5) . . ? C31 C30 C35 120.6(5) . . ? C29 C30 C35 121.1(5) . . ? C32 C31 C30 122.7(6) . . ? C32 C31 H31 118.6 . . ? C30 C31 H31 118.6 . . ? C31 C32 C33 118.5(6) . . ? C31 C32 H32 120.8 . . ? C33 C32 H32 120.8 . . ? C32 C33 C34 122.4(6) . . ? C32 C33 H33 118.8 . . ? C34 C33 H33 118.8 . . ? C33 C34 C29 117.9(5) . . ? C33 C34 C39 120.3(5) . . ? C29 C34 C39 121.8(5) . . ? C36 C35 C37 107.2(6) . . ? C36 C35 C30 108.5(5) . . ? C37 C35 C30 110.7(5) . . ? C36 C35 C38 109.5(5) . . ? C37 C35 C38 107.3(6) . . ? C30 C35 C38 113.4(5) . . ? 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 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C41 C39 C34 111.0(5) . . ? C41 C39 C42 110.9(5) . . ? C34 C39 C42 110.3(5) . . ? C41 C39 C40 106.6(5) . . ? C34 C39 C40 112.0(5) . . ? C42 C39 C40 105.9(5) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N3 C43 N2 114.8(6) . . ? N3 C43 N1 105.6(9) . . ? N2 C43 N1 139.6(9) . . ? N3 C43 N1A 151.8(9) . . ? N2 C43 N1A 93.2(8) . . ? N1 C43 N1A 46.6(6) . . ? N2 C44 H44A 109.6 . . ? N2 C44 H44B 109.7 . . ? H44A C44 H44B 109.4 . . ? N2 C44 H44C 109.3 . . ? H44A C44 H44C 109.4 . . ? H44B C44 H44C 109.4 . . ? N2 C45 H45A 113.3 . . ? N2 C45 H45B 114.2 . . ? H45A C45 H45B 105.7 . . ? N2 C45 H45C 111.7 . . ? H45A C45 H45C 106.3 . . ? H45B C45 H45C 104.9 . . ? N3 C46 H46A 109.5 . . ? N3 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N3 C46 H46C 109.4 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N3 C47 H47A 109.4 . . ? N3 C47 H47B 109.5 . . ? H47A C47 H47B 109.4 . . ? N3 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.681 _refine_diff_density_min -1.439 _refine_diff_density_rms 0.117 #===END data_q006 _database_code_depnum_ccdc_archive 'CCDC 743116' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (DBP)(H-TMG) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H35 N3 O' _chemical_formula_weight 321.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.654(4) _cell_length_b 16.646(7) _cell_length_c 25.314(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4068(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9732 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 24.43 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.050 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9807 _exptl_absorpt_correction_T_max 0.9922 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_reflns_number 29508 _diffrn_reflns_av_R_equivalents 0.0821 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3596 _reflns_number_gt 2428 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.2019P] 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 3596 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1505 _refine_ls_wR_factor_gt 0.1256 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.916 _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 N1 N 0.35370(18) 0.32574(10) 0.62943(8) 0.0430(5) Uani 1 1 d . . . N2 N 0.41680(17) 0.35687(10) 0.54403(7) 0.0405(4) Uani 1 1 d . . . N3 N 0.55712(16) 0.40061(10) 0.61247(7) 0.0396(4) Uani 1 1 d . . . O1 O 0.20201(13) 0.19389(8) 0.60982(5) 0.0321(3) Uani 1 1 d . . . C1 C 0.19149(17) 0.13737(10) 0.64918(7) 0.0275(4) Uani 1 1 d . . . C2 C 0.08253(18) 0.14355(10) 0.68614(7) 0.0295(4) Uani 1 1 d . . . C3 C 0.07325(19) 0.08372(11) 0.72459(8) 0.0357(5) Uani 1 1 d . . . H3 H 0.0017 0.0867 0.7503 0.043 Uiso 1 1 calc R . . C4 C 0.16524(19) 0.02049(11) 0.72619(8) 0.0376(5) Uani 1 1 d . . . H4 H 0.1572 -0.0191 0.7530 0.045 Uiso 1 1 calc R . . C5 C 0.26859(19) 0.01456(11) 0.68910(8) 0.0346(5) Uani 1 1 d . . . H5 H 0.3307 -0.0297 0.6906 0.041 Uiso 1 1 calc R . . C6 C 0.28487(17) 0.07171(10) 0.64929(7) 0.0292(4) Uani 1 1 d . . . C7 C 0.39922(19) 0.06253(12) 0.60732(8) 0.0356(5) Uani 1 1 d . . . C8 C 0.5040(2) 0.13189(13) 0.61106(9) 0.0485(6) Uani 1 1 d . . . H8A H 0.4568 0.1829 0.6040 0.073 Uiso 1 1 calc R . . H8B H 0.5777 0.1238 0.5850 0.073 Uiso 1 1 calc R . . H8C H 0.5443 0.1331 0.6466 0.073 Uiso 1 1 calc R . . C9 C 0.3360(2) 0.05939(14) 0.55162(8) 0.0496(6) Uani 1 1 d . . . H9A H 0.2695 0.0150 0.5496 0.074 Uiso 1 1 calc R . . H9B H 0.4097 0.0510 0.5256 0.074 Uiso 1 1 calc R . . H9C H 0.2885 0.1102 0.5442 0.074 Uiso 1 1 calc R . . C10 C 0.4809(2) -0.01579(13) 0.61463(9) 0.0478(6) Uani 1 1 d . . . H10A H 0.5266 -0.0154 0.6492 0.072 Uiso 1 1 calc R . . H10B H 0.5509 -0.0204 0.5867 0.072 Uiso 1 1 calc R . . H10C H 0.4174 -0.0616 0.6126 0.072 Uiso 1 1 calc R . . C11 C -0.02387(18) 0.21270(11) 0.68496(8) 0.0340(5) Uani 1 1 d . . . C12 C 0.0468(2) 0.29390(11) 0.69362(9) 0.0428(5) Uani 1 1 d . . . H12A H -0.0237 0.3361 0.6963 0.064 Uiso 1 1 calc R . . H12B H 0.1083 0.3055 0.6638 0.064 Uiso 1 1 calc R . . H12C H 0.1009 0.2922 0.7263 0.064 Uiso 1 1 calc R . . C13 C -0.1009(2) 0.21402(14) 0.63218(10) 0.0556(6) Uani 1 1 d . . . H13A H -0.1485 0.1626 0.6270 0.083 Uiso 1 1 calc R . . H13B H -0.0346 0.2226 0.6034 0.083 Uiso 1 1 calc R . . H13C H -0.1690 0.2577 0.6323 0.083 Uiso 1 1 calc R . . C14 C -0.1313(2) 0.20451(14) 0.72899(11) 0.0659(8) Uani 1 1 d . . . H14A H -0.1825 0.1541 0.7245 0.099 Uiso 1 1 calc R . . H14B H -0.1959 0.2499 0.7274 0.099 Uiso 1 1 calc R . . H14C H -0.0844 0.2043 0.7633 0.099 Uiso 1 1 calc R . . C15 C 0.43869(19) 0.35998(11) 0.59732(8) 0.0336(5) Uani 1 1 d . . . C16 C 0.2847(2) 0.32791(13) 0.52477(9) 0.0484(6) Uani 1 1 d . . . H16A H 0.2865 0.2691 0.5229 0.073 Uiso 1 1 calc R . . H16B H 0.2673 0.3500 0.4895 0.073 Uiso 1 1 calc R . . H16C H 0.2110 0.3450 0.5489 0.073 Uiso 1 1 calc R . . C17 C 0.5317(2) 0.33903(16) 0.50874(9) 0.0602(7) Uani 1 1 d . . . H17A H 0.6193 0.3516 0.5265 0.090 Uiso 1 1 calc R . . H17B H 0.5232 0.3715 0.4766 0.090 Uiso 1 1 calc R . . H17C H 0.5299 0.2819 0.4994 0.090 Uiso 1 1 calc R . . C18 C 0.5860(2) 0.47906(14) 0.58898(12) 0.0645(7) Uani 1 1 d . . . H18A H 0.5448 0.4817 0.5536 0.097 Uiso 1 1 calc R . . H18B H 0.6864 0.4867 0.5863 0.097 Uiso 1 1 calc R . . H18C H 0.5463 0.5214 0.6112 0.097 Uiso 1 1 calc R . . C19 C 0.6074(2) 0.39100(14) 0.66566(9) 0.0520(6) Uani 1 1 d . . . H19A H 0.5550 0.4261 0.6894 0.078 Uiso 1 1 calc R . . H19B H 0.7058 0.4053 0.6671 0.078 Uiso 1 1 calc R . . H19C H 0.5957 0.3350 0.6767 0.078 Uiso 1 1 calc R . . H1 H 0.371(2) 0.3407(13) 0.6629(9) 0.052(7) Uiso 1 1 d . . . H2 H 0.259(2) 0.2364(15) 0.6180(9) 0.063(7) 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 N1 0.0453(11) 0.0455(10) 0.0381(11) -0.0040(8) 0.0086(9) -0.0120(8) N2 0.0344(9) 0.0486(10) 0.0384(10) 0.0020(8) 0.0041(8) -0.0064(7) N3 0.0328(9) 0.0384(10) 0.0477(11) -0.0009(8) -0.0006(8) -0.0040(7) O1 0.0324(7) 0.0298(7) 0.0340(8) 0.0035(6) 0.0018(6) 0.0009(6) C1 0.0233(9) 0.0264(9) 0.0326(11) -0.0015(8) -0.0024(8) -0.0040(7) C2 0.0234(9) 0.0278(10) 0.0373(11) -0.0023(8) 0.0012(8) -0.0046(7) C3 0.0328(10) 0.0334(10) 0.0408(12) -0.0012(9) 0.0045(9) -0.0080(8) C4 0.0375(11) 0.0296(10) 0.0456(12) 0.0062(9) 0.0000(9) -0.0061(8) C5 0.0302(10) 0.0272(10) 0.0463(12) -0.0007(9) -0.0053(9) 0.0009(8) C6 0.0241(9) 0.0288(9) 0.0348(11) -0.0051(8) -0.0029(8) -0.0010(7) C7 0.0278(10) 0.0398(11) 0.0391(12) -0.0027(9) -0.0005(8) 0.0071(8) C8 0.0303(11) 0.0524(13) 0.0628(15) 0.0027(11) 0.0123(10) 0.0001(9) C9 0.0494(13) 0.0578(14) 0.0418(13) -0.0070(10) 0.0004(10) 0.0194(10) C10 0.0389(12) 0.0486(13) 0.0560(15) -0.0025(10) -0.0002(10) 0.0167(10) C11 0.0263(9) 0.0335(10) 0.0421(12) 0.0026(8) 0.0061(8) 0.0021(8) C12 0.0412(12) 0.0331(11) 0.0540(14) -0.0062(9) 0.0028(10) 0.0069(9) C13 0.0392(12) 0.0599(15) 0.0677(16) -0.0153(12) -0.0144(11) 0.0182(10) C14 0.0519(14) 0.0556(15) 0.090(2) 0.0193(13) 0.0382(14) 0.0183(11) C15 0.0295(10) 0.0271(10) 0.0442(12) -0.0018(8) 0.0044(9) 0.0021(8) C16 0.0451(13) 0.0539(13) 0.0461(13) 0.0023(11) -0.0057(10) -0.0076(10) C17 0.0485(14) 0.0865(18) 0.0457(14) 0.0001(13) 0.0128(11) -0.0010(12) C18 0.0502(15) 0.0446(14) 0.099(2) 0.0086(13) -0.0032(14) -0.0176(11) C19 0.0415(12) 0.0604(15) 0.0541(15) -0.0140(11) -0.0057(11) 0.0055(10) _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 N1 C15 1.288(2) . ? N1 H2 1.77(3) . ? N1 H1 0.90(2) . ? N2 C15 1.366(3) . ? N2 C16 1.448(3) . ? N2 C17 1.455(3) . ? N3 C15 1.383(2) . ? N3 C19 1.440(3) . ? N3 C18 1.462(3) . ? O1 C1 1.374(2) . ? O1 H2 0.92(2) . ? C1 C2 1.412(2) . ? C1 C6 1.417(2) . ? C2 C3 1.395(3) . ? C2 C11 1.543(3) . ? C3 C4 1.378(3) . ? C3 H3 0.9500 . ? C4 C5 1.374(3) . ? C4 H4 0.9500 . ? C5 C6 1.395(3) . ? C5 H5 0.9500 . ? C6 C7 1.540(3) . ? C7 C10 1.535(3) . ? C7 C9 1.537(3) . ? C7 C8 1.538(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.529(3) . ? C11 C13 1.529(3) . ? C11 C12 1.530(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? 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 C15 N1 H2 126.7(7) . . ? C15 N1 H1 110.5(15) . . ? H2 N1 H1 119.0(16) . . ? C15 N2 C16 118.77(16) . . ? C15 N2 C17 119.74(17) . . ? C16 N2 C17 113.37(18) . . ? C15 N3 C19 118.92(17) . . ? C15 N3 C18 118.83(17) . . ? C19 N3 C18 114.52(18) . . ? C1 O1 H2 114.1(14) . . ? O1 C1 C2 119.07(15) . . ? O1 C1 C6 118.85(16) . . ? C2 C1 C6 121.94(16) . . ? C3 C2 C1 117.27(16) . . ? C3 C2 C11 120.21(16) . . ? C1 C2 C11 122.52(16) . . ? C4 C3 C2 121.62(18) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 120.21(18) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 121.79(17) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 117.12(17) . . ? C5 C6 C7 120.78(16) . . ? C1 C6 C7 122.10(16) . . ? C10 C7 C9 106.61(16) . . ? C10 C7 C8 106.99(16) . . ? C9 C7 C8 110.07(18) . . ? C10 C7 C6 111.68(16) . . ? C9 C7 C6 110.58(15) . . ? C8 C7 C6 110.77(15) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C13 107.95(18) . . ? C14 C11 C12 106.07(17) . . ? C13 C11 C12 109.23(17) . . ? C14 C11 C2 111.78(16) . . ? C13 C11 C2 110.57(16) . . ? C12 C11 C2 111.08(15) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 N2 120.51(18) . . ? N1 C15 N3 124.63(19) . . ? N2 C15 N3 114.84(17) . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 H18A 109.5 . . ? N3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 H19A 109.5 . . ? N3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.155 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.040 #===END data_newtry _database_code_depnum_ccdc_archive 'CCDC 743117' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (4MeDBP)(HTMG) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H37 N3 O' _chemical_formula_weight 335.53 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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.4695(18) _cell_length_b 14.576(3) _cell_length_c 15.153(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2091.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4776 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 29.24 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.066 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9907 _exptl_absorpt_correction_T_max 0.9915 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11967 _diffrn_reflns_av_R_equivalents 0.1016 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.04 _reflns_number_total 2123 _reflns_number_gt 1842 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(10) _refine_ls_number_reflns 2123 _refine_ls_number_parameters 233 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.1194 _refine_ls_wR_factor_gt 0.1040 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.926 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.7926(2) 0.74392(15) 0.23566(13) 0.0228(5) Uani 1 1 d . . . N2 N 0.5660(2) 0.80295(14) 0.22987(12) 0.0222(5) Uani 1 1 d . . . N3 N 0.6091(2) 0.68014(14) 0.32403(14) 0.0264(5) Uani 1 1 d . . . O1 O 1.00156(18) 0.87053(11) 0.21283(10) 0.0205(4) Uani 1 1 d . . . H1 H 0.9277 0.8387 0.2157 0.031 Uiso 1 1 calc R . . C10 C 0.9519(2) 1.05732(16) 0.05429(15) 0.0202(5) Uani 1 1 d . . . H10 H 0.9597 1.0682 -0.0073 0.024 Uiso 1 1 calc R . . C1 C 0.6629(3) 0.74144(16) 0.26237(15) 0.0197(5) Uani 1 1 d . . . C17 C 1.0445(3) 0.89535(16) 0.02494(15) 0.0195(5) Uani 1 1 d . . . C6 C 0.9696(2) 0.95567(15) 0.17859(14) 0.0170(5) Uani 1 1 d . . . C8 C 0.8992(3) 1.11244(17) 0.19841(16) 0.0230(5) Uani 1 1 d . . . H8 H 0.8717 1.1613 0.2361 0.028 Uiso 1 1 calc R . . C7 C 0.9307(2) 1.02757(16) 0.23532(14) 0.0185(5) Uani 1 1 d . . . C9 C 0.9068(3) 1.12819(16) 0.10767(16) 0.0230(5) Uani 1 1 d . . . C11 C 0.9864(2) 0.97049(15) 0.08649(14) 0.0168(5) Uani 1 1 d . . . C13 C 0.9297(3) 1.01469(18) 0.33736(15) 0.0254(6) Uani 1 1 d . . . C19 C 1.1916(3) 0.86421(18) 0.05664(16) 0.0250(6) Uani 1 1 d . . . H19A H 1.2553 0.9171 0.0584 0.037 Uiso 1 1 calc R . . H19B H 1.2291 0.8181 0.0158 0.037 Uiso 1 1 calc R . . H19C H 1.1837 0.8376 0.1158 0.037 Uiso 1 1 calc R . . C20 C 1.0624(3) 0.93080(18) -0.06988(15) 0.0247(5) Uani 1 1 d . . . H20A H 1.1267 0.9835 -0.0700 0.037 Uiso 1 1 calc R . . H20B H 0.9703 0.9496 -0.0932 0.037 Uiso 1 1 calc R . . H20C H 1.1017 0.8819 -0.1069 0.037 Uiso 1 1 calc R . . C16 C 1.0798(3) 0.9914(2) 0.36734(17) 0.0338(7) Uani 1 1 d . . . H16A H 1.1433 1.0422 0.3523 0.051 Uiso 1 1 calc R . . H16B H 1.1116 0.9354 0.3376 0.051 Uiso 1 1 calc R . . H16C H 1.0807 0.9818 0.4313 0.051 Uiso 1 1 calc R . . C18 C 0.9423(3) 0.81391(16) 0.02016(15) 0.0217(5) Uani 1 1 d . . . H18A H 0.9820 0.7664 -0.0182 0.033 Uiso 1 1 calc R . . H18B H 0.8516 0.8346 -0.0038 0.033 Uiso 1 1 calc R . . H18C H 0.9280 0.7888 0.0795 0.033 Uiso 1 1 calc R . . C3 C 0.4558(3) 0.84237(18) 0.28506(16) 0.0281(6) Uani 1 1 d . . . H3A H 0.4533 0.8102 0.3418 0.042 Uiso 1 1 calc R . . H3B H 0.3643 0.8359 0.2555 0.042 Uiso 1 1 calc R . . H3C H 0.4757 0.9075 0.2950 0.042 Uiso 1 1 calc R . . C15 C 0.8863(4) 1.1033(2) 0.38383(17) 0.0377(7) Uani 1 1 d . . . H15A H 0.8890 1.0941 0.4479 0.057 Uiso 1 1 calc R . . H15B H 0.7903 1.1202 0.3659 0.057 Uiso 1 1 calc R . . H15C H 0.9517 1.1526 0.3675 0.057 Uiso 1 1 calc R . . C2 C 0.6087(3) 0.86043(18) 0.15594(16) 0.0254(6) Uani 1 1 d . . . H2A H 0.6633 0.9128 0.1779 0.038 Uiso 1 1 calc R . . H2B H 0.5246 0.8828 0.1250 0.038 Uiso 1 1 calc R . . H2C H 0.6669 0.8245 0.1152 0.038 Uiso 1 1 calc R . . C14 C 0.8257(3) 0.9396(2) 0.36617(15) 0.0328(7) Uani 1 1 d . . . H14A H 0.8576 0.8802 0.3435 0.049 Uiso 1 1 calc R . . H14B H 0.7317 0.9534 0.3426 0.049 Uiso 1 1 calc R . . H14C H 0.8216 0.9374 0.4308 0.049 Uiso 1 1 calc R . . C12 C 0.8721(3) 1.22120(18) 0.06982(19) 0.0342(7) Uani 1 1 d . . . H12A H 0.9418 1.2372 0.0246 0.051 Uiso 1 1 calc R . . H12B H 0.8743 1.2672 0.1170 0.051 Uiso 1 1 calc R . . H12C H 0.7777 1.2196 0.0434 0.051 Uiso 1 1 calc R . . C5 C 0.7103(3) 0.6250(2) 0.37338(19) 0.0370(7) Uani 1 1 d . . . H5A H 0.7486 0.5769 0.3350 0.055 Uiso 1 1 calc R . . H5B H 0.6629 0.5966 0.4240 0.055 Uiso 1 1 calc R . . H5C H 0.7873 0.6642 0.3943 0.055 Uiso 1 1 calc R . . C4 C 0.4760(3) 0.6328(2) 0.30666(18) 0.0347(7) Uani 1 1 d . . . H4A H 0.4189 0.6694 0.2657 0.052 Uiso 1 1 calc R . . H4B H 0.4243 0.6247 0.3622 0.052 Uiso 1 1 calc R . . H4C H 0.4955 0.5727 0.2805 0.052 Uiso 1 1 calc R . . H2 H 0.837(4) 0.697(2) 0.254(2) 0.040(9) 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 N1 0.0216(11) 0.0213(11) 0.0254(10) 0.0015(9) 0.0012(9) 0.0010(9) N2 0.0225(10) 0.0238(10) 0.0204(9) 0.0005(8) 0.0005(9) 0.0014(9) N3 0.0222(11) 0.0271(11) 0.0300(11) 0.0064(9) 0.0038(9) -0.0009(9) O1 0.0191(8) 0.0216(8) 0.0208(7) 0.0043(6) 0.0006(7) -0.0009(7) C10 0.0189(12) 0.0251(12) 0.0167(10) 0.0020(9) -0.0007(10) -0.0001(10) C1 0.0209(12) 0.0208(12) 0.0172(10) -0.0035(9) 0.0020(10) -0.0023(10) C17 0.0203(12) 0.0193(11) 0.0189(11) -0.0019(9) 0.0020(10) 0.0002(10) C6 0.0140(11) 0.0203(11) 0.0167(10) 0.0001(9) -0.0014(9) -0.0011(9) C8 0.0188(12) 0.0244(12) 0.0259(12) -0.0086(10) 0.0029(10) -0.0007(10) C7 0.0126(10) 0.0264(12) 0.0166(11) -0.0036(9) 0.0002(9) -0.0032(9) C9 0.0194(12) 0.0211(12) 0.0286(12) 0.0006(10) -0.0016(10) 0.0009(10) C11 0.0143(11) 0.0191(11) 0.0170(10) -0.0017(9) 0.0008(9) -0.0009(9) C13 0.0262(13) 0.0354(14) 0.0145(11) -0.0068(10) -0.0001(11) -0.0075(12) C19 0.0208(13) 0.0266(13) 0.0275(12) -0.0044(11) 0.0029(11) 0.0062(10) C20 0.0256(13) 0.0289(12) 0.0196(11) -0.0016(10) 0.0051(11) 0.0001(11) C16 0.0318(15) 0.0510(17) 0.0185(11) 0.0036(12) -0.0085(11) -0.0085(13) C18 0.0238(13) 0.0215(12) 0.0197(10) -0.0029(9) 0.0013(10) -0.0013(10) C3 0.0245(14) 0.0338(14) 0.0261(12) -0.0030(11) 0.0011(11) 0.0073(11) C15 0.0466(19) 0.0443(17) 0.0224(13) -0.0145(12) 0.0060(13) -0.0071(14) C2 0.0245(13) 0.0291(13) 0.0226(12) 0.0038(10) -0.0042(10) 0.0016(11) C14 0.0336(16) 0.0481(17) 0.0167(11) -0.0050(12) 0.0060(12) -0.0131(14) C12 0.0405(16) 0.0230(13) 0.0391(14) 0.0041(11) 0.0035(14) 0.0057(12) C5 0.0358(16) 0.0369(16) 0.0382(15) 0.0171(13) 0.0104(13) 0.0109(14) C4 0.0338(15) 0.0321(15) 0.0383(15) -0.0002(12) 0.0089(13) -0.0112(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 N1 C1 1.294(3) . ? N1 H2 0.85(3) . ? N2 C1 1.374(3) . ? N2 C3 1.455(3) . ? N2 C2 1.456(3) . ? N3 C1 1.390(3) . ? N3 C5 1.458(4) . ? N3 C4 1.460(3) . ? O1 C6 1.379(3) . ? O1 H1 0.8400 . ? C10 C9 1.380(3) . ? C10 C11 1.395(3) . ? C10 H10 0.9500 . ? C17 C18 1.534(3) . ? C17 C20 1.536(3) . ? C17 C11 1.540(3) . ? C17 C19 1.541(3) . ? C6 C7 1.405(3) . ? C6 C11 1.421(3) . ? C8 C7 1.390(3) . ? C8 C9 1.396(3) . ? C8 H8 0.9500 . ? C7 C13 1.558(3) . ? C9 C12 1.508(3) . ? C13 C15 1.528(4) . ? C13 C16 1.531(4) . ? C13 C14 1.535(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? 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 C1 N1 H2 110(2) . . ? C1 N2 C3 122.03(19) . . ? C1 N2 C2 117.7(2) . . ? C3 N2 C2 114.46(19) . . ? C1 N3 C5 117.3(2) . . ? C1 N3 C4 119.9(2) . . ? C5 N3 C4 113.5(2) . . ? C6 O1 H1 109.5 . . ? C9 C10 C11 123.1(2) . . ? C9 C10 H10 118.4 . . ? C11 C10 H10 118.4 . . ? N1 C1 N2 120.2(2) . . ? N1 C1 N3 125.2(2) . . ? N2 C1 N3 114.6(2) . . ? C18 C17 C20 106.60(19) . . ? C18 C17 C11 110.70(19) . . ? C20 C17 C11 111.51(19) . . ? C18 C17 C19 110.9(2) . . ? C20 C17 C19 106.9(2) . . ? C11 C17 C19 110.09(18) . . ? O1 C6 C7 119.92(19) . . ? O1 C6 C11 118.80(19) . . ? C7 C6 C11 121.1(2) . . ? C7 C8 C9 122.1(2) . . ? C7 C8 H8 118.9 . . ? C9 C8 H8 118.9 . . ? C8 C7 C6 118.3(2) . . ? C8 C7 C13 120.4(2) . . ? C6 C7 C13 121.3(2) . . ? C10 C9 C8 118.1(2) . . ? C10 C9 C12 121.2(2) . . ? C8 C9 C12 120.7(2) . . ? C10 C11 C6 117.1(2) . . ? C10 C11 C17 121.13(19) . . ? C6 C11 C17 121.78(19) . . ? C15 C13 C16 107.5(2) . . ? C15 C13 C14 107.4(2) . . ? C16 C13 C14 110.7(2) . . ? C15 C13 C7 110.9(2) . . ? C16 C13 C7 108.4(2) . . ? C14 C13 C7 111.86(19) . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.198 _refine_diff_density_min -0.171 _refine_diff_density_rms 0.042 #===END