Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #============================================================================== _audit_creation_date ? _audit_creation_method SHELXL-97 _audit_update_record ; ? ; #========================================================================== # 1. Submission Details _publ_contact_author_name 'Prof. Jun Okuda' _publ_contact_author_address ; Institut f\"ur Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; _publ_contact_author_email jun.okuda@ac.rwth-aachen.de _publ_contact_author_fax 0049-241-8094645 _publ_contact_author_phone 0049-241-8092644 _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #========================================================================== # 3. Title and Author List _publ_section_title ; Cationic Rare-Earth Metal Bis(tetrahydridoborato) Complexes: Direct Synthesis, Structure and Ring Opening Polymerisation Activtiy Toward Cyclic Esters ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address D.Robert ; Institute of Inorganic Chemistry RWTH Aachen University Landoltweg 1 D-52056 Aachen Germany ; M.Kondracka ; Institute of Inorganic Chemistry RWTH Aachen University Landoltweg 1 D-52056 Aachen Germany ; J.Okuda ; Institut fuer Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; #========================================================================== _publ_section_references ; Bruker (1999). SAINT+. Version 6.02. Bruker AXS Inc., Madison, Wisconson, USA. Bruker (2001). SMART. Version 5.624. Bruker AXS Inc., Madison, Wisconson, USA. Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXS-97. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G. M. (1998). SHELXTL. Version 5.1. Bruker AXS Inc., Madison, Wisconson, USA. Spek, A. L. (1990). Acta Cryst. A46, C-34. ; _publ_section_acknowledgements ; Support from the DFG is gratefully acknowledged. ; #========================================================================== data_dr1440 _database_code_depnum_ccdc_archive 'CCDC 674068' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H48 B2 O5 Y, C24 H20 B' _chemical_formula_sum 'C44 H68 B3 O5 Y' _chemical_formula_weight 798.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc 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 13.516(2) _cell_length_b 13.118(2) _cell_length_c 24.745(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.817(4) _cell_angle_gamma 90.00 _cell_volume 4386.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 905 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 21.64 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 1.371 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6839 _exptl_absorpt_correction_T_max 0.8105 _exptl_absorpt_process_details Platon _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59767 _diffrn_reflns_av_R_equivalents 0.0919 _diffrn_reflns_av_sigmaI/netI 0.0840 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 28.34 _reflns_number_total 10938 _reflns_number_gt 7098 _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^)+(0.0163P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10938 _refine_ls_number_parameters 510 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0708 _refine_ls_wR_factor_gt 0.0669 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Y Y 0.202055(15) 0.321463(15) 0.752817(8) 0.01954(6) Uani 1 1 d . . . O1 O 0.06734(10) 0.29374(10) 0.81579(5) 0.0245(3) Uani 1 1 d . . . O2 O 0.26601(9) 0.33049(10) 0.84389(5) 0.0216(3) Uani 1 1 d . . . O3 O 0.38286(10) 0.33702(10) 0.74891(5) 0.0237(3) Uani 1 1 d . . . O4 O 0.23915(10) 0.34576(10) 0.65858(5) 0.0267(4) Uani 1 1 d . . . O5 O 0.04719(10) 0.30748(11) 0.70305(5) 0.0322(4) Uani 1 1 d . . . B1 B 0.2279(2) 0.1266(2) 0.74722(12) 0.0308(7) Uani 1 1 d . . . H1A H 0.2376(14) 0.0396(16) 0.7446(8) 0.043(6) Uiso 1 1 d . . . H1B H 0.2639(16) 0.1729(17) 0.7188(9) 0.055(7) Uiso 1 1 d . . . H1C H 0.155(2) 0.1506(18) 0.7419(9) 0.070(9) Uiso 1 1 d . . . H1D H 0.2484(17) 0.1602(17) 0.7818(10) 0.065(8) Uiso 1 1 d . . . B2 B 0.1795(2) 0.5158(2) 0.75608(11) 0.0233(6) Uani 1 1 d . . . H1E H 0.1360(14) 0.4833(14) 0.7244(8) 0.034(6) Uiso 1 1 d . . . H1F H 0.1539(15) 0.4790(16) 0.7899(9) 0.054(7) Uiso 1 1 d . . . H1G H 0.2557(15) 0.4859(15) 0.7511(7) 0.039(6) Uiso 1 1 d . . . H1H H 0.1786(14) 0.5940(16) 0.7557(8) 0.039(6) Uiso 1 1 d . . . B3 B 0.68891(17) 0.23809(18) 0.50641(9) 0.0200(5) Uani 1 1 d . . . C1 C 0.00726(15) 0.20107(16) 0.81883(9) 0.0318(6) Uani 1 1 d . . . H1I H 0.0483 0.1423 0.8304 0.038 Uiso 1 1 calc R . . H1J H -0.0234 0.1854 0.7832 0.038 Uiso 1 1 calc R . . C2 C -0.07151(17) 0.22355(19) 0.86017(9) 0.0420(7) Uani 1 1 d . . . H2A H -0.1306 0.2552 0.8431 0.050 Uiso 1 1 calc R . . H2B H -0.0916 0.1609 0.8794 0.050 Uiso 1 1 calc R . . C3 C -0.01924(17) 0.29742(17) 0.89800(9) 0.0370(6) Uani 1 1 d . . . H3A H -0.0671 0.3384 0.9187 0.044 Uiso 1 1 calc R . . H3B H 0.0257 0.2613 0.9235 0.044 Uiso 1 1 calc R . . C4 C 0.03767(16) 0.36268(16) 0.85914(9) 0.0323(6) Uani 1 1 d . . . H4A H -0.0045 0.4183 0.8447 0.039 Uiso 1 1 calc R . . H4B H 0.0965 0.3930 0.8772 0.039 Uiso 1 1 calc R . . C5 C 0.26192(16) 0.25034(15) 0.88469(8) 0.0268(5) Uani 1 1 d . . . H5A H 0.3100 0.1956 0.8768 0.032 Uiso 1 1 calc R . . H5B H 0.1948 0.2203 0.8860 0.032 Uiso 1 1 calc R . . C6 C 0.28790(18) 0.30229(17) 0.93748(8) 0.0375(6) Uani 1 1 d . . . H6A H 0.3188 0.2540 0.9634 0.045 Uiso 1 1 calc R . . H6B H 0.2288 0.3332 0.9540 0.045 Uiso 1 1 calc R . . C7 C 0.36061(18) 0.38299(19) 0.92000(9) 0.0428(7) Uani 1 1 d . . . H7A H 0.3646 0.4393 0.9466 0.051 Uiso 1 1 calc R . . H7B H 0.4274 0.3538 0.9152 0.051 Uiso 1 1 calc R . . C8 C 0.31713(17) 0.41893(16) 0.86707(8) 0.0331(6) Uani 1 1 d . . . H8A H 0.2701 0.4756 0.8729 0.040 Uiso 1 1 calc R . . H8B H 0.3699 0.4427 0.8428 0.040 Uiso 1 1 calc R . . C9 C 0.45389(15) 0.26648(17) 0.77300(9) 0.0316(6) Uani 1 1 d . . . H9A H 0.4583 0.2036 0.7511 0.038 Uiso 1 1 calc R . . H9B H 0.4339 0.2478 0.8100 0.038 Uiso 1 1 calc R . . C10 C 0.55210(16) 0.32154(19) 0.77426(9) 0.0409(6) Uani 1 1 d . . . H10A H 0.6080 0.2732 0.7713 0.049 Uiso 1 1 calc R . . H10B H 0.5604 0.3622 0.8077 0.049 Uiso 1 1 calc R . . C11 C 0.54399(16) 0.38992(18) 0.72452(9) 0.0380(6) Uani 1 1 d . . . H11A H 0.5891 0.4492 0.7275 0.046 Uiso 1 1 calc R . . H11B H 0.5586 0.3517 0.6911 0.046 Uiso 1 1 calc R . . C12 C 0.43693(15) 0.42263(16) 0.72579(9) 0.0300(5) Uani 1 1 d . . . H12A H 0.4294 0.4843 0.7484 0.036 Uiso 1 1 calc R . . H12B H 0.4120 0.4378 0.6888 0.036 Uiso 1 1 calc R . . C13 C 0.19801(17) 0.42544(18) 0.62297(8) 0.0376(6) Uani 1 1 d . . . H13A H 0.2232 0.4934 0.6338 0.045 Uiso 1 1 calc R . . H13B H 0.1249 0.4261 0.6246 0.045 Uiso 1 1 calc R . . C14 C 0.23175(18) 0.3986(2) 0.56643(9) 0.0493(7) Uani 1 1 d . . . H14A H 0.1840 0.3526 0.5480 0.059 Uiso 1 1 calc R . . H14B H 0.2409 0.4606 0.5442 0.059 Uiso 1 1 calc R . . C15 C 0.32896(18) 0.34578(19) 0.57751(9) 0.0434(7) Uani 1 1 d . . . H15A H 0.3477 0.3016 0.5469 0.052 Uiso 1 1 calc R . . H15B H 0.3825 0.3957 0.5846 0.052 Uiso 1 1 calc R . . C16 C 0.30784(16) 0.28354(17) 0.62714(8) 0.0332(6) Uani 1 1 d . . . H16A H 0.2772 0.2175 0.6171 0.040 Uiso 1 1 calc R . . H16B H 0.3695 0.2703 0.6481 0.040 Uiso 1 1 calc R . . C17 C -0.03808(16) 0.37437(18) 0.70900(10) 0.0404(6) Uani 1 1 d . . . H17A H -0.0344 0.4322 0.6834 0.048 Uiso 1 1 calc R . . H17B H -0.0404 0.4019 0.7462 0.048 Uiso 1 1 calc R . . C18 C -0.12760(18) 0.3108(2) 0.69713(11) 0.0567(8) Uani 1 1 d . . . H18A H -0.1488 0.2726 0.7295 0.068 Uiso 1 1 calc R . . H18B H -0.1834 0.3529 0.6835 0.068 Uiso 1 1 calc R . . C19 C -0.0903(2) 0.2409(2) 0.65446(10) 0.0583(9) Uani 1 1 d . . . H19A H -0.1077 0.2678 0.6182 0.070 Uiso 1 1 calc R . . H19B H -0.1206 0.1726 0.6583 0.070 Uiso 1 1 calc R . . C20 C 0.0216(2) 0.2335(2) 0.66119(11) 0.0683(9) Uani 1 1 d . . . H20A H 0.0414 0.1640 0.6724 0.082 Uiso 1 1 calc R . . H20B H 0.0547 0.2505 0.6269 0.082 Uiso 1 1 calc R . . C21 C 0.61760(14) 0.18953(15) 0.55306(8) 0.0204(5) Uani 1 1 d . . . C22 C 0.53267(15) 0.13568(15) 0.53784(9) 0.0276(5) Uani 1 1 d . . . H22 H 0.5172 0.1297 0.5004 0.033 Uiso 1 1 calc R . . C23 C 0.46976(16) 0.09051(16) 0.57456(10) 0.0359(6) Uani 1 1 d . . . H23 H 0.4122 0.0555 0.5622 0.043 Uiso 1 1 calc R . . C24 C 0.49092(17) 0.09657(16) 0.62917(10) 0.0367(6) Uani 1 1 d . . . H24 H 0.4478 0.0667 0.6547 0.044 Uiso 1 1 calc R . . C25 C 0.57523(17) 0.14643(15) 0.64604(9) 0.0314(6) Uani 1 1 d . . . H25 H 0.5913 0.1497 0.6835 0.038 Uiso 1 1 calc R . . C26 C 0.63723(15) 0.19205(15) 0.60891(8) 0.0250(5) Uani 1 1 d . . . H26 H 0.6949 0.2262 0.6217 0.030 Uiso 1 1 calc R . . C27 C 0.62160(14) 0.30121(14) 0.46185(8) 0.0198(5) Uani 1 1 d . . . C28 C 0.53291(15) 0.34815(15) 0.47623(9) 0.0260(5) Uani 1 1 d . . . H28 H 0.5107 0.3397 0.5122 0.031 Uiso 1 1 calc R . . C29 C 0.47557(16) 0.40628(16) 0.44112(9) 0.0301(5) Uani 1 1 d . . . H29 H 0.4162 0.4369 0.4532 0.036 Uiso 1 1 calc R . . C30 C 0.50548(17) 0.41929(16) 0.38847(9) 0.0323(6) Uani 1 1 d . . . H30 H 0.4657 0.4568 0.3635 0.039 Uiso 1 1 calc R . . C31 C 0.59394(18) 0.37709(16) 0.37264(9) 0.0325(6) Uani 1 1 d . . . H31 H 0.6159 0.3866 0.3367 0.039 Uiso 1 1 calc R . . C32 C 0.65111(15) 0.32082(16) 0.40887(8) 0.0267(5) Uani 1 1 d . . . H32 H 0.7127 0.2946 0.3972 0.032 Uiso 1 1 calc R . . C33 C 0.74824(14) 0.13972(15) 0.48156(8) 0.0209(5) Uani 1 1 d . . . C34 C 0.73159(15) 0.09476(15) 0.43080(8) 0.0261(5) Uani 1 1 d . . . H34 H 0.6832 0.1241 0.4074 0.031 Uiso 1 1 calc R . . C35 C 0.78264(16) 0.00919(17) 0.41317(9) 0.0340(6) Uani 1 1 d . . . H35 H 0.7697 -0.0175 0.3781 0.041 Uiso 1 1 calc R . . C36 C 0.85194(17) -0.03690(17) 0.44652(10) 0.0381(6) Uani 1 1 d . . . H36 H 0.8871 -0.0953 0.4347 0.046 Uiso 1 1 calc R . . C37 C 0.86932(16) 0.00337(17) 0.49748(9) 0.0327(6) Uani 1 1 d . . . H37 H 0.9163 -0.0280 0.5211 0.039 Uiso 1 1 calc R . . C38 C 0.81873(15) 0.08902(16) 0.51422(9) 0.0273(5) Uani 1 1 d . . . H38 H 0.8322 0.1149 0.5494 0.033 Uiso 1 1 calc R . . C39 C 0.76615(14) 0.32392(15) 0.53061(7) 0.0193(4) Uani 1 1 d . . . C40 C 0.73442(16) 0.40068(15) 0.56599(8) 0.0249(5) Uani 1 1 d . . . H40 H 0.6677 0.3998 0.5776 0.030 Uiso 1 1 calc R . . C41 C 0.79629(17) 0.47763(16) 0.58464(8) 0.0302(6) Uani 1 1 d . . . H41 H 0.7718 0.5273 0.6090 0.036 Uiso 1 1 calc R . . C42 C 0.89308(17) 0.48248(16) 0.56810(9) 0.0321(6) Uani 1 1 d . . . H42 H 0.9355 0.5355 0.5805 0.038 Uiso 1 1 calc R . . C43 C 0.92723(16) 0.40893(17) 0.53314(9) 0.0309(6) Uani 1 1 d . . . H43 H 0.9938 0.4109 0.5214 0.037 Uiso 1 1 calc R . . C44 C 0.86462(15) 0.33226(16) 0.51507(8) 0.0257(5) Uani 1 1 d . . . H44 H 0.8900 0.2828 0.4909 0.031 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 Y 0.02182(11) 0.01998(10) 0.01679(10) -0.00020(10) -0.00073(7) 0.00012(11) O1 0.0225(8) 0.0275(9) 0.0235(8) -0.0010(6) 0.0028(6) -0.0023(7) O2 0.0283(8) 0.0196(8) 0.0168(7) 0.0022(6) -0.0036(6) -0.0067(7) O3 0.0245(8) 0.0243(9) 0.0224(8) 0.0077(6) 0.0000(6) -0.0012(7) O4 0.0302(9) 0.0327(9) 0.0171(8) -0.0010(6) 0.0011(7) 0.0090(7) O5 0.0324(9) 0.0358(10) 0.0281(9) -0.0015(7) -0.0083(7) -0.0038(8) B1 0.0370(19) 0.0233(16) 0.0320(17) -0.0026(13) 0.0001(15) -0.0007(13) B2 0.0312(18) 0.0178(14) 0.0208(14) -0.0003(12) -0.0039(13) 0.0025(12) B3 0.0163(14) 0.0227(14) 0.0212(13) 0.0003(10) 0.0013(11) 0.0002(11) C1 0.0262(13) 0.0331(15) 0.0360(14) 0.0055(11) -0.0005(11) -0.0086(11) C2 0.0291(15) 0.0519(17) 0.0453(16) 0.0119(13) 0.0081(12) -0.0039(13) C3 0.0326(14) 0.0466(17) 0.0322(14) 0.0044(12) 0.0104(11) 0.0080(12) C4 0.0317(14) 0.0351(14) 0.0303(13) -0.0032(11) 0.0074(11) 0.0081(11) C5 0.0312(13) 0.0248(12) 0.0244(13) 0.0112(10) 0.0003(10) 0.0020(10) C6 0.0528(16) 0.0397(16) 0.0198(12) 0.0054(11) -0.0040(11) 0.0128(13) C7 0.0478(17) 0.0493(17) 0.0308(15) -0.0081(12) -0.0149(12) -0.0027(14) C8 0.0431(15) 0.0287(13) 0.0272(13) -0.0028(11) -0.0066(11) -0.0150(11) C9 0.0293(14) 0.0341(14) 0.0314(14) 0.0109(11) 0.0020(11) 0.0064(11) C10 0.0284(14) 0.0489(16) 0.0451(15) 0.0144(14) -0.0072(11) -0.0002(13) C11 0.0294(14) 0.0409(15) 0.0438(16) 0.0094(12) 0.0014(12) -0.0071(12) C12 0.0298(14) 0.0307(13) 0.0295(13) 0.0068(10) 0.0018(11) -0.0068(11) C13 0.0424(16) 0.0470(16) 0.0233(13) 0.0118(11) -0.0008(11) 0.0106(13) C14 0.0515(18) 0.077(2) 0.0198(14) 0.0068(13) 0.0016(12) 0.0052(16) C15 0.0425(16) 0.067(2) 0.0210(13) -0.0098(12) 0.0094(12) -0.0059(14) C16 0.0313(14) 0.0402(14) 0.0281(13) -0.0126(11) 0.0057(11) 0.0068(11) C17 0.0278(14) 0.0528(17) 0.0404(16) 0.0133(13) -0.0085(12) 0.0023(13) C18 0.0369(16) 0.067(2) 0.066(2) 0.0356(17) -0.0172(14) -0.0084(15) C19 0.061(2) 0.086(2) 0.0279(15) 0.0217(15) -0.0176(14) -0.0509(17) C20 0.084(2) 0.059(2) 0.061(2) -0.0268(16) -0.0369(17) 0.0030(17) C21 0.0176(11) 0.0173(11) 0.0263(12) 0.0009(10) 0.0017(9) 0.0042(9) C22 0.0242(13) 0.0279(13) 0.0307(13) 0.0034(10) 0.0006(10) -0.0003(10) C23 0.0230(13) 0.0258(13) 0.0589(18) 0.0054(12) 0.0022(12) -0.0024(11) C24 0.0358(15) 0.0249(14) 0.0502(17) 0.0134(12) 0.0241(13) 0.0063(12) C25 0.0391(15) 0.0267(13) 0.0287(13) 0.0057(10) 0.0096(11) 0.0099(11) C26 0.0263(12) 0.0216(13) 0.0272(12) 0.0029(10) 0.0013(10) 0.0016(10) C27 0.0171(11) 0.0200(12) 0.0223(11) -0.0027(9) -0.0018(9) -0.0048(9) C28 0.0242(13) 0.0267(13) 0.0270(12) 0.0043(10) 0.0016(10) 0.0004(10) C29 0.0213(12) 0.0268(13) 0.0421(15) 0.0056(11) -0.0018(11) -0.0007(10) C30 0.0352(15) 0.0242(13) 0.0369(15) 0.0097(11) -0.0158(11) -0.0049(11) C31 0.0479(16) 0.0297(14) 0.0198(12) 0.0043(10) -0.0016(11) -0.0055(12) C32 0.0290(12) 0.0257(12) 0.0256(12) 0.0006(11) 0.0022(9) -0.0014(11) C33 0.0164(12) 0.0222(12) 0.0244(12) 0.0016(9) 0.0040(9) -0.0041(9) C34 0.0211(12) 0.0259(13) 0.0313(13) -0.0036(10) 0.0012(10) -0.0050(10) C35 0.0333(15) 0.0315(14) 0.0375(15) -0.0124(12) 0.0072(12) -0.0073(12) C36 0.0340(15) 0.0240(13) 0.0567(18) -0.0055(12) 0.0166(13) 0.0016(11) C37 0.0233(13) 0.0320(14) 0.0431(16) 0.0112(12) 0.0077(11) 0.0056(11) C38 0.0245(13) 0.0335(14) 0.0242(12) 0.0039(10) 0.0056(10) 0.0019(11) C39 0.0213(11) 0.0201(11) 0.0165(10) 0.0057(10) -0.0017(8) 0.0020(10) C40 0.0251(13) 0.0216(12) 0.0280(13) 0.0033(10) -0.0010(10) 0.0025(10) C41 0.0417(15) 0.0198(12) 0.0289(13) -0.0014(10) -0.0044(11) 0.0025(11) C42 0.0428(16) 0.0218(13) 0.0312(14) 0.0044(10) -0.0127(12) -0.0103(11) C43 0.0241(13) 0.0350(14) 0.0336(14) 0.0045(11) 0.0002(11) -0.0096(11) C44 0.0272(13) 0.0276(13) 0.0224(12) 0.0003(10) -0.0010(9) -0.0037(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y O2 2.4051(13) . ? Y O4 2.4134(13) . ? Y O5 2.4203(14) . ? Y O1 2.4406(13) . ? Y O3 2.4556(13) . ? Y B2 2.569(3) . ? Y B1 2.584(3) . ? Y H1B 2.29(2) . ? Y H1C 2.34(2) . ? Y H1D 2.32(2) . ? Y H1E 2.404(18) . ? Y H1F 2.36(2) . ? Y H1G 2.276(19) . ? O1 C4 1.464(2) . ? O1 C1 1.464(2) . ? O2 C5 1.459(2) . ? O2 C8 1.463(2) . ? O3 C9 1.455(2) . ? O3 C12 1.461(2) . ? O4 C16 1.468(2) . ? O4 C13 1.471(2) . ? O5 C20 1.457(3) . ? O5 C17 1.458(2) . ? B1 H1A 1.15(2) . ? B1 H1B 1.05(2) . ? B1 H1C 1.04(3) . ? B1 H1D 1.00(2) . ? B2 H1E 1.063(19) . ? B2 H1F 1.03(2) . ? B2 H1G 1.11(2) . ? B2 H1H 1.03(2) . ? B3 C39 1.643(3) . ? B3 C21 1.643(3) . ? B3 C33 1.643(3) . ? B3 C27 1.643(3) . ? C1 C2 1.516(3) . ? C1 H1I 0.9900 . ? C1 H1J 0.9900 . ? C2 C3 1.515(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.507(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.510(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.512(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.504(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.511(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.526(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.510(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.519(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.507(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.505(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.495(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.492(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.522(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.395(3) . ? C21 C26 1.404(3) . ? C22 C23 1.386(3) . ? C22 H22 0.9500 . ? C23 C24 1.379(3) . ? C23 H23 0.9500 . ? C24 C25 1.374(3) . ? C24 H24 0.9500 . ? C25 C26 1.388(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.398(3) . ? C27 C32 1.400(3) . ? C28 C29 1.385(3) . ? C28 H28 0.9500 . ? C29 C30 1.380(3) . ? C29 H29 0.9500 . ? C30 C31 1.379(3) . ? C30 H30 0.9500 . ? C31 C32 1.388(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.403(3) . ? C33 C38 1.408(3) . ? C34 C35 1.391(3) . ? C34 H34 0.9500 . ? C35 C36 1.379(3) . ? C35 H35 0.9500 . ? C36 C37 1.384(3) . ? C36 H36 0.9500 . ? C37 C38 1.382(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C44 1.395(3) . ? C39 C40 1.405(3) . ? C40 C41 1.386(3) . ? C40 H40 0.9500 . ? C41 C42 1.378(3) . ? C41 H41 0.9500 . ? C42 C43 1.380(3) . ? C42 H42 0.9500 . ? C43 C44 1.384(3) . ? C43 H43 0.9500 . ? C44 H44 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 O2 Y O4 145.29(5) . . ? O2 Y O5 141.00(5) . . ? O4 Y O5 73.05(5) . . ? O2 Y O1 70.77(4) . . ? O4 Y O1 143.49(5) . . ? O5 Y O1 70.48(5) . . ? O2 Y O3 71.83(4) . . ? O4 Y O3 74.36(4) . . ? O5 Y O3 147.16(5) . . ? O1 Y O3 142.14(4) . . ? O2 Y B2 87.88(7) . . ? O4 Y B2 85.74(7) . . ? O5 Y B2 89.36(7) . . ? O1 Y B2 92.16(7) . . ? O3 Y B2 92.16(7) . . ? O2 Y B1 92.97(8) . . ? O4 Y B1 92.80(7) . . ? O5 Y B1 90.82(8) . . ? O1 Y B1 89.39(7) . . ? O3 Y B1 86.83(8) . . ? B2 Y B1 178.41(10) . . ? O2 Y H1B 105.0(5) . . ? O4 Y H1B 71.0(6) . . ? O5 Y H1B 93.8(5) . . ? O1 Y H1B 112.8(6) . . ? O3 Y H1B 71.7(5) . . ? B2 Y H1B 154.4(6) . . ? B1 Y H1B 24.0(6) . . ? O2 Y H1C 104.4(6) . . ? O4 Y H1C 94.3(6) . . ? O5 Y H1C 68.8(6) . . ? O1 Y H1C 74.2(6) . . ? O3 Y H1C 110.1(6) . . ? B2 Y H1C 157.0(7) . . ? B1 Y H1C 23.7(6) . . ? H1B Y H1C 40.8(8) . . ? O2 Y H1D 70.3(6) . . ? O4 Y H1D 111.1(6) . . ? O5 Y H1D 108.4(6) . . ? O1 Y H1D 82.4(6) . . ? O3 Y H1D 79.8(6) . . ? B2 Y H1D 158.1(6) . . ? B1 Y H1D 22.7(6) . . ? H1B Y H1D 40.2(8) . . ? H1C Y H1D 40.0(8) . . ? O2 Y H1E 111.0(5) . . ? O4 Y H1E 71.5(4) . . ? O5 Y H1E 66.6(5) . . ? O1 Y H1E 92.3(4) . . ? O3 Y H1E 106.3(5) . . ? B2 Y H1E 24.4(5) . . ? B1 Y H1E 155.2(5) . . ? H1B Y H1E 141.4(7) . . ? H1C Y H1E 135.3(8) . . ? H1D Y H1E 173.9(7) . . ? O2 Y H1F 71.9(5) . . ? O4 Y H1F 108.9(6) . . ? O5 Y H1F 91.3(5) . . ? O1 Y H1F 70.7(5) . . ? O3 Y H1F 102.9(5) . . ? B2 Y H1F 23.7(5) . . ? B1 Y H1F 157.9(6) . . ? H1B Y H1F 174.6(7) . . ? H1C Y H1F 143.8(8) . . ? H1D Y H1F 139.0(8) . . ? H1E Y H1F 40.2(7) . . ? O2 Y H1G 82.0(5) . . ? O4 Y H1G 77.6(5) . . ? O5 Y H1G 109.6(5) . . ? O1 Y H1G 113.2(5) . . ? O3 Y H1G 66.6(5) . . ? B2 Y H1G 25.6(5) . . ? B1 Y H1G 153.3(5) . . ? H1B Y H1G 133.1(8) . . ? H1C Y H1G 171.8(7) . . ? H1D Y H1G 141.8(8) . . ? H1E Y H1G 43.5(7) . . ? H1F Y H1G 42.8(7) . . ? C4 O1 C1 108.50(15) . . ? C4 O1 Y 126.20(11) . . ? C1 O1 Y 125.15(11) . . ? C5 O2 C8 108.81(14) . . ? C5 O2 Y 126.59(11) . . ? C8 O2 Y 124.59(11) . . ? C9 O3 C12 108.57(15) . . ? C9 O3 Y 125.61(11) . . ? C12 O3 Y 125.66(11) . . ? C16 O4 C13 108.32(15) . . ? C16 O4 Y 125.48(12) . . ? C13 O4 Y 126.20(11) . . ? C20 O5 C17 106.99(17) . . ? C20 O5 Y 127.39(14) . . ? C17 O5 Y 125.61(13) . . ? Y B1 H1A 178.8(10) . . ? Y B1 H1B 61.9(12) . . ? H1A B1 H1B 118.7(15) . . ? Y B1 H1C 65.1(13) . . ? H1A B1 H1C 113.7(16) . . ? H1B B1 H1C 100.8(17) . . ? Y B1 H1D 63.5(13) . . ? H1A B1 H1D 117.1(17) . . ? H1B B1 H1D 101.1(18) . . ? H1C B1 H1D 103.0(18) . . ? Y B2 H1E 69.1(10) . . ? Y B2 H1F 66.5(12) . . ? H1E B2 H1F 102.9(16) . . ? Y B2 H1G 62.3(10) . . ? H1E B2 H1G 106.3(14) . . ? H1F B2 H1G 104.3(15) . . ? Y B2 H1H 173.4(11) . . ? H1E B2 H1H 112.9(15) . . ? H1F B2 H1H 118.1(16) . . ? H1G B2 H1H 111.3(15) . . ? C39 B3 C21 112.68(17) . . ? C39 B3 C33 111.33(16) . . ? C21 B3 C33 104.64(16) . . ? C39 B3 C27 104.01(16) . . ? C21 B3 C27 110.01(16) . . ? C33 B3 C27 114.40(17) . . ? O1 C1 C2 105.57(17) . . ? O1 C1 H1I 110.6 . . ? C2 C1 H1I 110.6 . . ? O1 C1 H1J 110.6 . . ? C2 C1 H1J 110.6 . . ? H1I C1 H1J 108.8 . . ? C3 C2 C1 102.46(18) . . ? C3 C2 H2A 111.3 . . ? C1 C2 H2A 111.3 . . ? C3 C2 H2B 111.3 . . ? C1 C2 H2B 111.3 . . ? H2A C2 H2B 109.2 . . ? C4 C3 C2 101.94(18) . . ? C4 C3 H3A 111.4 . . ? C2 C3 H3A 111.4 . . ? C4 C3 H3B 111.4 . . ? C2 C3 H3B 111.4 . . ? H3A C3 H3B 109.2 . . ? O1 C4 C3 105.33(17) . . ? O1 C4 H4A 110.7 . . ? C3 C4 H4A 110.7 . . ? O1 C4 H4B 110.7 . . ? C3 C4 H4B 110.7 . . ? H4A C4 H4B 108.8 . . ? O2 C5 C6 105.22(16) . . ? O2 C5 H5A 110.7 . . ? C6 C5 H5A 110.7 . . ? O2 C5 H5B 110.7 . . ? C6 C5 H5B 110.7 . . ? H5A C5 H5B 108.8 . . ? C5 C6 C7 102.29(17) . . ? C5 C6 H6A 111.3 . . ? C7 C6 H6A 111.3 . . ? C5 C6 H6B 111.3 . . ? C7 C6 H6B 111.3 . . ? H6A C6 H6B 109.2 . . ? C8 C7 C6 102.77(18) . . ? C8 C7 H7A 111.2 . . ? C6 C7 H7A 111.2 . . ? C8 C7 H7B 111.2 . . ? C6 C7 H7B 111.2 . . ? H7A C7 H7B 109.1 . . ? O2 C8 C7 105.62(17) . . ? O2 C8 H8A 110.6 . . ? C7 C8 H8A 110.6 . . ? O2 C8 H8B 110.6 . . ? C7 C8 H8B 110.6 . . ? H8A C8 H8B 108.7 . . ? O3 C9 C10 106.19(17) . . ? O3 C9 H9A 110.5 . . ? C10 C9 H9A 110.5 . . ? O3 C9 H9B 110.5 . . ? C10 C9 H9B 110.5 . . ? H9A C9 H9B 108.7 . . ? C9 C10 C11 102.20(18) . . ? C9 C10 H10A 111.3 . . ? C11 C10 H10A 111.3 . . ? C9 C10 H10B 111.3 . . ? C11 C10 H10B 111.3 . . ? H10A C10 H10B 109.2 . . ? C12 C11 C10 102.01(17) . . ? C12 C11 H11A 111.4 . . ? C10 C11 H11A 111.4 . . ? C12 C11 H11B 111.4 . . ? C10 C11 H11B 111.4 . . ? H11A C11 H11B 109.2 . . ? O3 C12 C11 105.93(17) . . ? O3 C12 H12A 110.5 . . ? C11 C12 H12A 110.5 . . ? O3 C12 H12B 110.5 . . ? C11 C12 H12B 110.5 . . ? H12A C12 H12B 108.7 . . ? O4 C13 C14 105.75(18) . . ? O4 C13 H13A 110.6 . . ? C14 C13 H13A 110.6 . . ? O4 C13 H13B 110.6 . . ? C14 C13 H13B 110.6 . . ? H13A C13 H13B 108.7 . . ? C15 C14 C13 102.19(18) . . ? C15 C14 H14A 111.3 . . ? C13 C14 H14A 111.3 . . ? C15 C14 H14B 111.3 . . ? C13 C14 H14B 111.3 . . ? H14A C14 H14B 109.2 . . ? C16 C15 C14 102.89(18) . . ? C16 C15 H15A 111.2 . . ? C14 C15 H15A 111.2 . . ? C16 C15 H15B 111.2 . . ? C14 C15 H15B 111.2 . . ? H15A C15 H15B 109.1 . . ? O4 C16 C15 105.04(18) . . ? O4 C16 H16A 110.7 . . ? C15 C16 H16A 110.7 . . ? O4 C16 H16B 110.7 . . ? C15 C16 H16B 110.7 . . ? H16A C16 H16B 108.8 . . ? O5 C17 C18 106.4(2) . . ? O5 C17 H17A 110.4 . . ? C18 C17 H17A 110.4 . . ? O5 C17 H17B 110.4 . . ? C18 C17 H17B 110.4 . . ? H17A C17 H17B 108.6 . . ? C19 C18 C17 101.6(2) . . ? C19 C18 H18A 111.4 . . ? C17 C18 H18A 111.4 . . ? C19 C18 H18B 111.4 . . ? C17 C18 H18B 111.4 . . ? H18A C18 H18B 109.3 . . ? C18 C19 C20 107.8(2) . . ? C18 C19 H19A 110.1 . . ? C20 C19 H19A 110.1 . . ? C18 C19 H19B 110.1 . . ? C20 C19 H19B 110.1 . . ? H19A C19 H19B 108.5 . . ? O5 C20 C19 105.2(2) . . ? O5 C20 H20A 110.7 . . ? C19 C20 H20A 110.7 . . ? O5 C20 H20B 110.7 . . ? C19 C20 H20B 110.7 . . ? H20A C20 H20B 108.8 . . ? C22 C21 C26 114.89(18) . . ? C22 C21 B3 119.69(18) . . ? C26 C21 B3 125.32(18) . . ? C23 C22 C21 123.3(2) . . ? C23 C22 H22 118.3 . . ? C21 C22 H22 118.3 . . ? C24 C23 C22 119.8(2) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C25 C24 C23 119.0(2) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C24 C25 C26 120.7(2) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C21 122.3(2) . . ? C25 C26 H26 118.9 . . ? C21 C26 H26 118.9 . . ? C28 C27 C32 114.46(18) . . ? C28 C27 B3 121.31(18) . . ? C32 C27 B3 123.97(18) . . ? C29 C28 C27 123.9(2) . . ? C29 C28 H28 118.1 . . ? C27 C28 H28 118.1 . . ? C30 C29 C28 119.4(2) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C31 C30 C29 119.0(2) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C30 C31 C32 120.5(2) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C27 122.6(2) . . ? C31 C32 H32 118.7 . . ? C27 C32 H32 118.7 . . ? C34 C33 C38 114.46(19) . . ? C34 C33 B3 126.31(19) . . ? C38 C33 B3 119.09(19) . . ? C35 C34 C33 123.1(2) . . ? C35 C34 H34 118.5 . . ? C33 C34 H34 118.5 . . ? C36 C35 C34 120.1(2) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C37 118.9(2) . . ? C35 C36 H36 120.6 . . ? C37 C36 H36 120.6 . . ? C38 C37 C36 120.3(2) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C37 C38 C33 123.1(2) . . ? C37 C38 H38 118.5 . . ? C33 C38 H38 118.5 . . ? C44 C39 C40 114.60(19) . . ? C44 C39 B3 123.86(18) . . ? C40 C39 B3 121.35(17) . . ? C41 C40 C39 122.8(2) . . ? C41 C40 H40 118.6 . . ? C39 C40 H40 118.6 . . ? C42 C41 C40 120.4(2) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C41 C42 C43 118.8(2) . . ? C41 C42 H42 120.6 . . ? C43 C42 H42 120.6 . . ? C42 C43 C44 120.1(2) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C39 123.3(2) . . ? C43 C44 H44 118.3 . . ? C39 C44 H44 118.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Y O1 C4 56.17(14) . . . . ? O4 Y O1 C4 -116.59(15) . . . . ? O5 Y O1 C4 -119.38(15) . . . . ? O3 Y O1 C4 65.48(17) . . . . ? B2 Y O1 C4 -30.83(15) . . . . ? B1 Y O1 C4 149.53(16) . . . . ? O2 Y O1 C1 -119.03(15) . . . . ? O4 Y O1 C1 68.21(16) . . . . ? O5 Y O1 C1 65.42(14) . . . . ? O3 Y O1 C1 -109.72(15) . . . . ? B2 Y O1 C1 153.97(15) . . . . ? B1 Y O1 C1 -25.67(16) . . . . ? O4 Y O2 C5 -128.41(14) . . . . ? O5 Y O2 C5 65.82(16) . . . . ? O1 Y O2 C5 59.15(14) . . . . ? O3 Y O2 C5 -114.85(14) . . . . ? B2 Y O2 C5 152.18(15) . . . . ? B1 Y O2 C5 -29.17(16) . . . . ? O4 Y O2 C8 50.83(17) . . . . ? O5 Y O2 C8 -114.94(15) . . . . ? O1 Y O2 C8 -121.61(15) . . . . ? O3 Y O2 C8 64.39(14) . . . . ? B2 Y O2 C8 -28.57(15) . . . . ? B1 Y O2 C8 150.08(16) . . . . ? O2 Y O3 C9 59.04(14) . . . . ? O4 Y O3 C9 -128.93(15) . . . . ? O5 Y O3 C9 -121.73(15) . . . . ? O1 Y O3 C9 49.79(17) . . . . ? B2 Y O3 C9 146.10(15) . . . . ? B1 Y O3 C9 -35.13(16) . . . . ? O2 Y O3 C12 -115.77(15) . . . . ? O4 Y O3 C12 56.26(14) . . . . ? O5 Y O3 C12 63.46(17) . . . . ? O1 Y O3 C12 -125.02(14) . . . . ? B2 Y O3 C12 -28.71(15) . . . . ? B1 Y O3 C12 150.06(16) . . . . ? O2 Y O4 C16 67.86(17) . . . . ? O5 Y O4 C16 -121.45(15) . . . . ? O1 Y O4 C16 -124.20(14) . . . . ? O3 Y O4 C16 54.48(14) . . . . ? B2 Y O4 C16 147.92(16) . . . . ? B1 Y O4 C16 -31.44(16) . . . . ? O2 Y O4 C13 -111.51(16) . . . . ? O5 Y O4 C13 59.18(16) . . . . ? O1 Y O4 C13 56.43(18) . . . . ? O3 Y O4 C13 -124.89(16) . . . . ? B2 Y O4 C13 -31.45(16) . . . . ? B1 Y O4 C13 149.18(17) . . . . ? O2 Y O5 C20 -127.67(19) . . . . ? O4 Y O5 C20 60.75(19) . . . . ? O1 Y O5 C20 -121.0(2) . . . . ? O3 Y O5 C20 53.5(2) . . . . ? B2 Y O5 C20 146.5(2) . . . . ? B1 Y O5 C20 -31.9(2) . . . . ? O2 Y O5 C17 53.74(18) . . . . ? O4 Y O5 C17 -117.85(16) . . . . ? O1 Y O5 C17 60.41(15) . . . . ? O3 Y O5 C17 -125.09(15) . . . . ? B2 Y O5 C17 -32.11(16) . . . . ? B1 Y O5 C17 149.48(16) . . . . ? C4 O1 C1 C2 8.9(2) . . . . ? Y O1 C1 C2 -175.19(12) . . . . ? O1 C1 C2 C3 -30.4(2) . . . . ? C1 C2 C3 C4 39.7(2) . . . . ? C1 O1 C4 C3 16.5(2) . . . . ? Y O1 C4 C3 -159.35(13) . . . . ? C2 C3 C4 O1 -35.0(2) . . . . ? C8 O2 C5 C6 14.5(2) . . . . ? Y O2 C5 C6 -166.13(12) . . . . ? O2 C5 C6 C7 -33.1(2) . . . . ? C5 C6 C7 C8 38.9(2) . . . . ? C5 O2 C8 C7 10.2(2) . . . . ? Y O2 C8 C7 -169.14(13) . . . . ? C6 C7 C8 O2 -30.7(2) . . . . ? C12 O3 C9 C10 11.4(2) . . . . ? Y O3 C9 C10 -164.12(13) . . . . ? O3 C9 C10 C11 -31.2(2) . . . . ? C9 C10 C11 C12 38.4(2) . . . . ? C9 O3 C12 C11 13.5(2) . . . . ? Y O3 C12 C11 -170.99(12) . . . . ? C10 C11 C12 O3 -32.4(2) . . . . ? C16 O4 C13 C14 8.9(2) . . . . ? Y O4 C13 C14 -171.64(14) . . . . ? O4 C13 C14 C15 -30.1(2) . . . . ? C13 C14 C15 C16 39.4(2) . . . . ? C13 O4 C16 C15 16.1(2) . . . . ? Y O4 C16 C15 -163.41(13) . . . . ? C14 C15 C16 O4 -34.7(2) . . . . ? C20 O5 C17 C18 32.1(2) . . . . ? Y O5 C17 C18 -149.09(15) . . . . ? O5 C17 C18 C19 -34.5(2) . . . . ? C17 C18 C19 C20 24.6(3) . . . . ? C17 O5 C20 C19 -15.6(3) . . . . ? Y O5 C20 C19 165.60(14) . . . . ? C18 C19 C20 O5 -6.2(3) . . . . ? C39 B3 C21 C22 164.05(18) . . . . ? C33 B3 C21 C22 -74.8(2) . . . . ? C27 B3 C21 C22 48.5(2) . . . . ? C39 B3 C21 C26 -19.8(3) . . . . ? C33 B3 C21 C26 101.3(2) . . . . ? C27 B3 C21 C26 -135.39(19) . . . . ? C26 C21 C22 C23 2.1(3) . . . . ? B3 C21 C22 C23 178.58(19) . . . . ? C21 C22 C23 C24 -0.9(3) . . . . ? C22 C23 C24 C25 -0.9(3) . . . . ? C23 C24 C25 C26 1.4(3) . . . . ? C24 C25 C26 C21 -0.2(3) . . . . ? C22 C21 C26 C25 -1.5(3) . . . . ? B3 C21 C26 C25 -177.80(19) . . . . ? C39 B3 C27 C28 -91.5(2) . . . . ? C21 B3 C27 C28 29.4(3) . . . . ? C33 B3 C27 C28 146.80(18) . . . . ? C39 B3 C27 C32 82.3(2) . . . . ? C21 B3 C27 C32 -156.77(18) . . . . ? C33 B3 C27 C32 -39.3(3) . . . . ? C32 C27 C28 C29 2.4(3) . . . . ? B3 C27 C28 C29 176.84(19) . . . . ? C27 C28 C29 C30 0.6(3) . . . . ? C28 C29 C30 C31 -2.4(3) . . . . ? C29 C30 C31 C32 1.2(3) . . . . ? C30 C31 C32 C27 2.1(3) . . . . ? C28 C27 C32 C31 -3.7(3) . . . . ? B3 C27 C32 C31 -177.96(19) . . . . ? C39 B3 C33 C34 -131.0(2) . . . . ? C21 B3 C33 C34 107.0(2) . . . . ? C27 B3 C33 C34 -13.4(3) . . . . ? C39 B3 C33 C38 53.5(2) . . . . ? C21 B3 C33 C38 -68.5(2) . . . . ? C27 B3 C33 C38 171.09(17) . . . . ? C38 C33 C34 C35 -2.1(3) . . . . ? B3 C33 C34 C35 -177.75(19) . . . . ? C33 C34 C35 C36 1.4(3) . . . . ? C34 C35 C36 C37 0.1(3) . . . . ? C35 C36 C37 C38 -0.7(3) . . . . ? C36 C37 C38 C33 -0.1(3) . . . . ? C34 C33 C38 C37 1.4(3) . . . . ? B3 C33 C38 C37 177.42(18) . . . . ? C21 B3 C39 C44 139.30(19) . . . . ? C33 B3 C39 C44 22.1(3) . . . . ? C27 B3 C39 C44 -101.6(2) . . . . ? C21 B3 C39 C40 -45.9(3) . . . . ? C33 B3 C39 C40 -163.16(18) . . . . ? C27 B3 C39 C40 73.2(2) . . . . ? C44 C39 C40 C41 -1.0(3) . . . . ? B3 C39 C40 C41 -176.17(18) . . . . ? C39 C40 C41 C42 1.0(3) . . . . ? C40 C41 C42 C43 -0.6(3) . . . . ? C41 C42 C43 C44 0.3(3) . . . . ? C42 C43 C44 C39 -0.3(3) . . . . ? C40 C39 C44 C43 0.6(3) . . . . ? B3 C39 C44 C43 175.71(19) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.984 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.060 #==END #========================================================================== data_dr1870 _database_code_depnum_ccdc_archive 'CCDC 674069' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H48 B2 Nd O5, C24 H20 B' _chemical_formula_sum 'C44 H68 B3 Nd O5' _chemical_formula_weight 853.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21/c _symmetry_space_group_name_Hall -P2ybc 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 13.033(2) _cell_length_b 13.516(2) _cell_length_c 24.968(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.071(9) _cell_angle_gamma 90.00 _cell_volume 4398.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 8451 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 28.91 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1788 _exptl_absorpt_coefficient_mu 1.221 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7108 _exptl_absorpt_correction_T_max 0.7922 _exptl_absorpt_process_details Platon _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31868 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 0.82 _diffrn_reflns_theta_max 31.70 _reflns_number_total 12299 _reflns_number_gt 10062 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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. Only a part of hydrogen atoms could be refined. B-H bonds were restrained to a value of 1.2 A, inter hydrogen atoms were constrained to common isotropic displacement parameters. Crystals of dr1870 show monoclinic angles very close to 90 degrees, are pseudo-merohedral twins with apparent Laue symmetry mmm. ; _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^)+(0.0354P)^2^+1.9582P] 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 12299 _refine_ls_number_parameters 497 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0867 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd Nd 0.797389(11) 0.822000(10) 0.750948(18) 0.01616(4) Uani 1 1 d . . . B1 B 0.8174(2) 1.0227(2) 0.7551(2) 0.0122(7) Uani 1 1 d D . . H1D H 0.8578 0.9933 0.7250 0.015 Uiso 1 1 calc R . . H1A H 0.812(2) 1.1083(13) 0.7546(17) 0.015 Uiso 1 1 d D . . H1B H 0.837(3) 0.991(3) 0.7970(9) 0.015 Uiso 1 1 d D . . H1C H 0.7329(15) 0.995(2) 0.7583(15) 0.015 Uiso 1 1 d D . . B2 B 0.7725(3) 0.6210(3) 0.7456(3) 0.0254(9) Uani 1 1 d . . . H2E H 0.7634 0.5477 0.7423 0.030 Uiso 1 1 calc R . . H1F H 0.729(4) 0.666(3) 0.7140(19) 0.030 Uiso 1 1 d . . . H1G H 0.840(3) 0.643(3) 0.7393(18) 0.030 Uiso 1 1 d . . . H1H H 0.744(4) 0.648(3) 0.7774(19) 0.030 Uiso 1 1 d . . . B3 B 0.3109(3) 0.7631(3) 1.0055(2) 0.0169(9) Uani 1 1 d . . . O1 O 0.61063(15) 0.83719(14) 0.7505(2) 0.0211(4) Uani 1 1 d . . . O2 O 0.7318(2) 0.8295(2) 0.84411(13) 0.0210(7) Uani 1 1 d . . . O3 O 0.9352(2) 0.7962(2) 0.81582(12) 0.0247(7) Uani 1 1 d . . . O4 O 0.9586(2) 0.8102(2) 0.70100(13) 0.0297(8) Uani 1 1 d . . . O5 O 0.7599(2) 0.8467(2) 0.65452(13) 0.0252(7) Uani 1 1 d . . . C1 C 0.5565(3) 0.9236(3) 0.72501(17) 0.0301(9) Uani 1 1 d . . . H1I H 0.5642 0.9843 0.7469 0.036 Uiso 1 1 calc R . . H1J H 0.5828 0.9365 0.6885 0.036 Uiso 1 1 calc R . . C2 C 0.4497(3) 0.8902(4) 0.7237(2) 0.0396(11) Uani 1 1 d . . . H2A H 0.4346 0.8541 0.6901 0.048 Uiso 1 1 calc R . . H2B H 0.4018 0.9468 0.7270 0.048 Uiso 1 1 calc R . . C3 C 0.4421(3) 0.8217(4) 0.7723(2) 0.0431(12) Uani 1 1 d . . . H3A H 0.4342 0.8603 0.8057 0.052 Uiso 1 1 calc R . . H3B H 0.3831 0.7760 0.7686 0.052 Uiso 1 1 calc R . . C4 C 0.5409(3) 0.7661(3) 0.77227(18) 0.0318(9) Uani 1 1 d . . . H4A H 0.5611 0.7465 0.8090 0.038 Uiso 1 1 calc R . . H4B H 0.5367 0.7063 0.7495 0.038 Uiso 1 1 calc R . . C5 C 0.6800(3) 0.9174(3) 0.86747(17) 0.0302(9) Uani 1 1 d . . . H5A H 0.6235 0.9403 0.8440 0.036 Uiso 1 1 calc R . . H5B H 0.7293 0.9724 0.8726 0.036 Uiso 1 1 calc R . . C6 C 0.6392(4) 0.8817(4) 0.9204(2) 0.0433(13) Uani 1 1 d . . . H6A H 0.5683 0.8563 0.9166 0.052 Uiso 1 1 calc R . . H6B H 0.6396 0.9356 0.9473 0.052 Uiso 1 1 calc R . . C7 C 0.7121(4) 0.7996(3) 0.93648(17) 0.0366(10) Uani 1 1 d . . . H7A H 0.7751 0.8269 0.9531 0.044 Uiso 1 1 calc R . . H7B H 0.6791 0.7535 0.9620 0.044 Uiso 1 1 calc R . . C8 C 0.7365(3) 0.7482(3) 0.88416(16) 0.0258(8) Uani 1 1 d . . . H8A H 0.8056 0.7179 0.8852 0.031 Uiso 1 1 calc R . . H8B H 0.6851 0.6963 0.8761 0.031 Uiso 1 1 calc R . . C9 C 0.9636(3) 0.8653(3) 0.85933(16) 0.0291(9) Uani 1 1 d . . . H9A H 0.9018 0.8949 0.8759 0.035 Uiso 1 1 calc R . . H9B H 1.0083 0.9190 0.8458 0.035 Uiso 1 1 calc R . . C10 C 1.0198(3) 0.8009(3) 0.89854(17) 0.0327(10) Uani 1 1 d . . . H10A H 0.9719 0.7676 0.9235 0.039 Uiso 1 1 calc R . . H10B H 1.0708 0.8393 0.9194 0.039 Uiso 1 1 calc R . . C11 C 1.0724(3) 0.7261(4) 0.8611(2) 0.0432(14) Uani 1 1 d . . . H11A H 1.1346 0.7553 0.8447 0.052 Uiso 1 1 calc R . . H11B H 1.0922 0.6656 0.8809 0.052 Uiso 1 1 calc R . . C12 C 0.9955(4) 0.7034(4) 0.8200(2) 0.0318(11) Uani 1 1 d . . . H12A H 0.9515 0.6474 0.8312 0.038 Uiso 1 1 calc R . . H12B H 1.0286 0.6869 0.7855 0.038 Uiso 1 1 calc R . . C13 C 1.0422(3) 0.8803(3) 0.70787(18) 0.0314(9) Uani 1 1 d . . . H13A H 1.0438 0.9075 0.7447 0.038 Uiso 1 1 calc R . . H13B H 1.0375 0.9353 0.6819 0.038 Uiso 1 1 calc R . . C14 C 1.1323(3) 0.8169(4) 0.6972(2) 0.0396(11) Uani 1 1 d . . . H14A H 1.1533 0.7812 0.7301 0.048 Uiso 1 1 calc R . . H14B H 1.1909 0.8573 0.6846 0.048 Uiso 1 1 calc R . . C15 C 1.0990(4) 0.7445(4) 0.6542(2) 0.0385(12) Uani 1 1 d . . . H15A H 1.1139 0.7708 0.6181 0.046 Uiso 1 1 calc R . . H15B H 1.1344 0.6801 0.6586 0.046 Uiso 1 1 calc R . . C16 C 0.9879(4) 0.7336(5) 0.6623(3) 0.0595(19) Uani 1 1 d . . . H16A H 0.9507 0.7430 0.6281 0.071 Uiso 1 1 calc R . . H16B H 0.9717 0.6670 0.6765 0.071 Uiso 1 1 calc R . . C17 C 0.8031(3) 0.9250(3) 0.61909(16) 0.0350(9) Uani 1 1 d . . . H17A H 0.8789 0.9257 0.6211 0.042 Uiso 1 1 calc R . . H17B H 0.7770 0.9911 0.6295 0.042 Uiso 1 1 calc R . . C18 C 0.7678(4) 0.8984(4) 0.5639(2) 0.0485(13) Uani 1 1 d . . . H18A H 0.7569 0.9581 0.5416 0.058 Uiso 1 1 calc R . . H18B H 0.8176 0.8542 0.5458 0.058 Uiso 1 1 calc R . . C19 C 0.6698(4) 0.8465(4) 0.5747(2) 0.0398(13) Uani 1 1 d . . . H19A H 0.6502 0.8039 0.5441 0.048 Uiso 1 1 calc R . . H19B H 0.6139 0.8946 0.5814 0.048 Uiso 1 1 calc R . . C20 C 0.6907(3) 0.7852(3) 0.62401(16) 0.0313(9) Uani 1 1 d . . . H20A H 0.6267 0.7721 0.6441 0.038 Uiso 1 1 calc R . . H20B H 0.7232 0.7214 0.6145 0.038 Uiso 1 1 calc R . . C21 C 0.2512(3) 0.8615(3) 0.98080(17) 0.0205(8) Uani 1 1 d . . . C22 C 0.2671(4) 0.9060(3) 0.9322(2) 0.0238(11) Uani 1 1 d . . . H22 H 0.3153 0.8759 0.9087 0.029 Uiso 1 1 calc R . . C23 C 0.2173(4) 0.9935(3) 0.9139(2) 0.0273(11) Uani 1 1 d . . . H23 H 0.2314 1.0197 0.8794 0.033 Uiso 1 1 calc R . . C24 C 0.1480(3) 1.0394(3) 0.9476(2) 0.0379(11) Uani 1 1 d . . . H24 H 0.1131 1.0977 0.9366 0.045 Uiso 1 1 calc R . . C25 C 0.1304(3) 0.9992(3) 0.99765(19) 0.0324(9) Uani 1 1 d . . . H25 H 0.0836 1.0306 1.0213 0.039 Uiso 1 1 calc R . . C26 C 0.1810(3) 0.9122(3) 1.01401(17) 0.0253(8) Uani 1 1 d . . . H26 H 0.1675 0.8867 1.0487 0.030 Uiso 1 1 calc R . . C27 C 0.2339(3) 0.6762(3) 1.02960(16) 0.0185(7) Uani 1 1 d . . . C28 C 0.1348(3) 0.6690(3) 1.01466(16) 0.0244(8) Uani 1 1 d . . . H28 H 0.1067 0.7174 0.9913 0.029 Uiso 1 1 calc R . . C29 C 0.0719(3) 0.5913(3) 1.03286(17) 0.0284(9) Uani 1 1 d . . . H29 H 0.0026 0.5893 1.0211 0.034 Uiso 1 1 calc R . . C30 C 0.1064(3) 0.5175(3) 1.06726(16) 0.0291(9) Uani 1 1 d . . . H30 H 0.0624 0.4656 1.0786 0.035 Uiso 1 1 calc R . . C31 C 0.2033(5) 0.5224(3) 1.0836(2) 0.0321(11) Uani 1 1 d . . . H31 H 0.2300 0.4742 1.1075 0.039 Uiso 1 1 calc R . . C32 C 0.2652(4) 0.5990(3) 1.06507(19) 0.0253(12) Uani 1 1 d . . . H32 H 0.3344 0.6000 1.0771 0.030 Uiso 1 1 calc R . . C33 C 0.3778(4) 0.7002(3) 0.96115(18) 0.0187(9) Uani 1 1 d . . . C34 C 0.3483(3) 0.6799(3) 0.90895(19) 0.0243(10) Uani 1 1 d . . . H34 H 0.2849 0.7063 0.8967 0.029 Uiso 1 1 calc R . . C35 C 0.4057(4) 0.6233(3) 0.87351(18) 0.0289(9) Uani 1 1 d . . . H35 H 0.3821 0.6148 0.8378 0.035 Uiso 1 1 calc R . . C36 C 0.4939(4) 0.5805(3) 0.88882(19) 0.0296(10) Uani 1 1 d . . . H36 H 0.5345 0.5430 0.8646 0.036 Uiso 1 1 calc R . . C37 C 0.5223(4) 0.5937(3) 0.9411(2) 0.0297(11) Uani 1 1 d . . . H37 H 0.5823 0.5617 0.9539 0.036 Uiso 1 1 calc R . . C38 C 0.4664(4) 0.6522(3) 0.97586(19) 0.0234(10) Uani 1 1 d . . . H38 H 0.4904 0.6596 1.0116 0.028 Uiso 1 1 calc R . . C39 C 0.3810(4) 0.8114(3) 1.0515(2) 0.0219(10) Uani 1 1 d . . . C40 C 0.3640(3) 0.8080(3) 1.10705(18) 0.0244(10) Uani 1 1 d . . . H40 H 0.3064 0.7718 1.1196 0.029 Uiso 1 1 calc R . . C41 C 0.4250(3) 0.8536(3) 1.1443(2) 0.0308(10) Uani 1 1 d . . . H41 H 0.4088 0.8504 1.1814 0.037 Uiso 1 1 calc R . . C42 C 0.5108(4) 0.9045(3) 1.1266(2) 0.0328(12) Uani 1 1 d . . . H42 H 0.5554 0.9351 1.1517 0.039 Uiso 1 1 calc R . . C43 C 0.5316(4) 0.9107(4) 1.0728(2) 0.0391(14) Uani 1 1 d . . . H43 H 0.5903 0.9460 1.0607 0.047 Uiso 1 1 calc R . . C44 C 0.4673(4) 0.8656(4) 1.0362(2) 0.0279(11) Uani 1 1 d . . . H44 H 0.4823 0.8717 0.9991 0.033 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 Nd 0.01450(6) 0.01656(7) 0.01741(8) -0.00023(12) -0.0004(3) -0.00119(6) B1 0.0198(14) 0.0088(12) 0.0081(18) -0.0012(17) 0.0036(17) -0.0040(10) B2 0.0207(15) 0.0215(17) 0.034(3) -0.003(3) -0.001(2) -0.0015(12) B3 0.0144(15) 0.013(2) 0.023(2) 0.0005(17) 0.0040(17) 0.0009(15) O1 0.0175(9) 0.0280(11) 0.0178(10) -0.004(2) -0.006(2) 0.0002(8) O2 0.0226(15) 0.0197(14) 0.0207(15) 0.0039(11) 0.0032(12) 0.0049(11) O3 0.0165(14) 0.0275(15) 0.0300(17) -0.0025(13) -0.0056(12) 0.0010(11) O4 0.0178(14) 0.0317(17) 0.040(2) -0.0016(14) 0.0119(14) -0.0013(12) O5 0.0223(15) 0.0306(16) 0.0226(16) 0.0011(13) -0.0032(12) -0.0075(12) C1 0.0271(19) 0.030(2) 0.033(2) 0.0134(18) -0.0044(16) 0.0073(16) C2 0.0201(19) 0.043(3) 0.056(3) 0.013(2) 0.0026(19) 0.0064(19) C3 0.0226(19) 0.057(3) 0.050(3) 0.014(2) 0.0107(18) 0.006(2) C4 0.0212(17) 0.039(2) 0.035(2) 0.0119(19) -0.0014(16) -0.0043(17) C5 0.034(2) 0.028(2) 0.029(2) -0.0018(17) 0.0096(17) 0.0108(16) C6 0.044(3) 0.049(3) 0.037(3) -0.008(2) 0.020(2) 0.001(2) C7 0.045(3) 0.045(3) 0.020(2) 0.0058(18) 0.005(2) -0.011(2) C8 0.0227(17) 0.0240(19) 0.031(2) 0.0129(17) -0.0008(16) -0.0030(15) C9 0.0256(19) 0.032(2) 0.030(2) -0.0033(18) -0.0059(17) -0.0050(16) C10 0.0235(19) 0.043(3) 0.031(2) 0.0031(19) -0.0110(17) -0.0060(17) C11 0.020(2) 0.056(3) 0.054(4) 0.011(3) -0.008(2) 0.010(2) C12 0.0201(19) 0.039(3) 0.036(3) 0.005(2) -0.0031(18) 0.0100(17) C13 0.0202(17) 0.040(2) 0.034(2) 0.0066(19) 0.0024(16) -0.0062(17) C14 0.0228(19) 0.045(3) 0.051(3) 0.018(2) 0.0069(19) 0.0017(19) C15 0.027(2) 0.053(3) 0.035(3) 0.017(2) 0.009(2) 0.020(2) C16 0.045(3) 0.066(4) 0.068(4) -0.041(3) 0.027(3) -0.013(3) C17 0.033(2) 0.049(3) 0.023(2) 0.0101(18) -0.0002(19) -0.010(2) C18 0.045(3) 0.071(4) 0.030(3) 0.006(3) 0.006(2) -0.004(3) C19 0.032(3) 0.060(4) 0.028(3) -0.008(2) -0.012(2) 0.004(2) C20 0.028(2) 0.040(2) 0.026(2) -0.0086(18) -0.0053(18) -0.0053(18) C21 0.0100(15) 0.0172(19) 0.034(2) -0.0020(17) -0.0026(15) -0.0044(14) C22 0.015(2) 0.020(2) 0.036(3) 0.002(2) 0.0008(19) -0.0043(18) C23 0.025(2) 0.025(2) 0.031(2) 0.0119(19) -0.0074(19) -0.0052(18) C24 0.029(2) 0.023(2) 0.061(3) 0.007(2) -0.017(2) 0.0043(17) C25 0.0212(18) 0.029(2) 0.047(3) -0.0089(19) -0.0091(18) 0.0064(15) C26 0.0176(17) 0.0264(19) 0.032(2) -0.0031(17) -0.0030(15) 0.0034(14) C27 0.0168(16) 0.0190(19) 0.0197(19) -0.0003(16) 0.0037(13) 0.0000(14) C28 0.0229(17) 0.027(2) 0.023(2) -0.0007(16) 0.0007(15) -0.0023(15) C29 0.0189(17) 0.033(2) 0.033(2) -0.0050(18) -0.0011(16) -0.0111(15) C30 0.034(2) 0.0210(19) 0.032(2) -0.0034(17) 0.0094(18) -0.0114(17) C31 0.037(2) 0.020(2) 0.039(3) 0.0033(19) 0.006(3) 0.005(2) C32 0.024(3) 0.022(3) 0.029(3) -0.002(2) 0.003(2) 0.000(2) C33 0.0180(19) 0.0156(18) 0.023(2) 0.0026(16) -0.0013(16) -0.0040(15) C34 0.0189(19) 0.026(2) 0.028(2) -0.0037(18) -0.0031(18) -0.0001(16) C35 0.041(2) 0.026(2) 0.020(2) -0.0032(17) 0.0013(18) -0.0056(18) C36 0.027(2) 0.021(2) 0.040(3) -0.014(2) 0.014(2) -0.0037(17) C37 0.013(2) 0.025(2) 0.050(3) -0.008(2) 0.0044(19) 0.0038(17) C38 0.0180(19) 0.024(2) 0.029(2) -0.0005(18) 0.0012(17) -0.0008(15) C39 0.0116(17) 0.0148(19) 0.039(3) -0.0025(17) -0.0036(18) 0.0048(15) C40 0.021(2) 0.022(2) 0.030(3) -0.0001(18) -0.0023(18) 0.0046(15) C41 0.035(2) 0.023(2) 0.035(3) -0.0070(19) -0.011(2) 0.0083(17) C42 0.024(2) 0.028(2) 0.047(3) -0.015(2) -0.015(2) 0.0066(18) C43 0.017(2) 0.030(3) 0.070(4) -0.014(3) -0.008(2) -0.0020(19) C44 0.019(2) 0.027(2) 0.038(3) -0.004(2) 0.0049(19) -0.0007(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd O3 2.442(3) . ? Nd O1 2.4428(19) . ? Nd O4 2.450(3) . ? Nd O5 2.479(3) . ? Nd O2 2.481(3) . ? Nd B1 2.727(3) . ? Nd B2 2.740(4) . ? Nd H1B 2.61(4) . ? Nd H1C 2.49(3) . ? Nd H1F 2.47(4) . ? Nd H1G 2.51(4) . ? Nd H1H 2.54(5) . ? B1 H1B 1.157(18) . ? B1 H1A 1.160(17) . ? B1 H1C 1.167(17) . ? B1 H1D 1.0000 . ? B1 H1A 1.160(17) . ? B1 H1B 1.157(18) . ? B1 H1C 1.167(17) . ? B2 H1G 0.94(4) . ? B2 H1H 0.95(5) . ? B2 H1F 1.14(5) . ? B2 H2E 1.0000 . ? B2 H1F 1.14(5) . ? B2 H1G 0.94(4) . ? B2 H1H 0.95(5) . ? B3 C39 1.606(6) . ? B3 C33 1.647(6) . ? B3 C27 1.659(6) . ? B3 C21 1.660(6) . ? O1 C4 1.431(5) . ? O1 C1 1.505(5) . ? O2 C5 1.486(4) . ? O2 C8 1.487(5) . ? O3 C9 1.479(5) . ? O3 C12 1.485(5) . ? O4 C13 1.454(5) . ? O4 C16 1.466(6) . ? O5 C20 1.444(5) . ? O5 C17 1.490(5) . ? C1 C2 1.463(6) . ? C1 H1I 0.9900 . ? C1 H1J 0.9900 . ? C2 C3 1.530(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.490(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.505(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.514(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.513(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.501(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.538(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.465(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.478(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.516(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.469(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.497(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.483(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.509(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.371(6) . ? C21 C26 1.413(5) . ? C22 C23 1.424(6) . ? C22 H22 0.9500 . ? C23 C24 1.383(7) . ? C23 H23 0.9500 . ? C24 C25 1.381(7) . ? C24 H24 0.9500 . ? C25 C26 1.408(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.348(5) . ? C27 C32 1.427(6) . ? C28 C29 1.407(5) . ? C28 H28 0.9500 . ? C29 C30 1.391(6) . ? C29 H29 0.9500 . ? C30 C31 1.328(8) . ? C30 H30 0.9500 . ? C31 C32 1.392(7) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.374(7) . ? C33 C34 1.386(6) . ? C34 C35 1.389(6) . ? C34 H34 0.9500 . ? C35 C36 1.342(6) . ? C35 H35 0.9500 . ? C36 C37 1.367(7) . ? C36 H36 0.9500 . ? C37 C38 1.382(6) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C44 1.396(7) . ? C39 C40 1.405(6) . ? C40 C41 1.369(6) . ? C40 H40 0.9500 . ? C41 C42 1.387(7) . ? C41 H41 0.9500 . ? C42 C43 1.373(8) . ? C42 H42 0.9500 . ? C43 C44 1.382(7) . ? C43 H43 0.9500 . ? C44 H44 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 Nd O1 138.37(17) . . ? O3 Nd O4 72.40(11) . . ? O1 Nd O4 149.11(18) . . ? O3 Nd O5 143.84(11) . . ? O1 Nd O5 77.79(16) . . ? O4 Nd O5 71.49(11) . . ? O3 Nd O2 68.79(10) . . ? O1 Nd O2 69.93(16) . . ? O4 Nd O2 140.95(11) . . ? O5 Nd O2 146.85(9) . . ? O3 Nd B1 92.66(12) . . ? O1 Nd B1 90.68(8) . . ? O4 Nd B1 90.12(10) . . ? O5 Nd B1 85.50(13) . . ? O2 Nd B1 87.52(12) . . ? O3 Nd B2 88.72(14) . . ? O1 Nd B2 88.01(9) . . ? O4 Nd B2 90.70(12) . . ? O5 Nd B2 93.63(17) . . ? O2 Nd B2 92.59(16) . . ? B1 Nd B2 178.56(13) . . ? O3 Nd H1B 71.9(6) . . ? O1 Nd H1B 97.1(8) . . ? O4 Nd H1B 96.5(8) . . ? O5 Nd H1B 110.4(4) . . ? O2 Nd H1B 67.6(6) . . ? B1 Nd H1B 24.9(4) . . ? B2 Nd H1B 156.0(4) . . ? O3 Nd H1C 109.5(7) . . ? O1 Nd H1C 65.5(4) . . ? O4 Nd H1C 112.9(5) . . ? O5 Nd H1C 83.1(9) . . ? O2 Nd H1C 77.0(8) . . ? B1 Nd H1C 25.3(4) . . ? B2 Nd H1C 153.4(4) . . ? H1B Nd H1C 38.0(9) . . ? O3 Nd H1F 113.0(11) . . ? O1 Nd H1F 73.1(11) . . ? O4 Nd H1F 93.7(11) . . ? O5 Nd H1F 71.5(11) . . ? O2 Nd H1F 105.0(11) . . ? B1 Nd H1F 154.0(11) . . ? B2 Nd H1F 24.7(11) . . ? H1B Nd H1F 169.7(14) . . ? H1C Nd H1F 135.0(12) . . ? O3 Nd H1G 77.0(9) . . ? O1 Nd H1G 107.6(9) . . ? O4 Nd H1G 71.7(10) . . ? O5 Nd H1G 93.5(10) . . ? O2 Nd H1G 103.0(10) . . ? B1 Nd H1G 161.1(10) . . ? B2 Nd H1G 20.1(9) . . ? H1B Nd H1G 148.8(11) . . ? H1C Nd H1G 172.8(10) . . ? H1F Nd H1G 37.8(13) . . ? O3 Nd H1H 84.0(11) . . ? O1 Nd H1H 78.9(11) . . ? O4 Nd H1H 107.8(10) . . ? O5 Nd H1H 108.9(11) . . ? O2 Nd H1H 72.5(11) . . ? B1 Nd H1H 159.6(11) . . ? B2 Nd H1H 20.2(10) . . ? H1B Nd H1H 138.6(12) . . ? H1C Nd H1H 139.3(12) . . ? H1F Nd H1H 37.5(13) . . ? H1G Nd H1H 36.3(13) . . ? H1B B1 H1A 113(3) . . ? H1B B1 H1C 91(3) . . ? H1A B1 H1C 105(2) . . ? H1B B1 Nd 72.1(18) . . ? H1A B1 Nd 170.5(15) . . ? H1C B1 Nd 65.8(15) . . ? H1B B1 H1D 114.9 . . ? H1A B1 H1D 114.9 . . ? H1C B1 H1D 114.9 . . ? Nd B1 H1D 68.1 . . ? H1B B1 H1A 113(3) . . ? H1C B1 H1A 105(2) . . ? Nd B1 H1A 170.5(15) . . ? H1D B1 H1A 114.9 . . ? H1A B1 H1B 113(3) . . ? H1C B1 H1B 91(3) . . ? Nd B1 H1B 72.1(18) . . ? H1D B1 H1B 114.9 . . ? H1A B1 H1B 113(3) . . ? H1B B1 H1C 91(3) . . ? H1A B1 H1C 105(2) . . ? Nd B1 H1C 65.8(15) . . ? H1D B1 H1C 114.9 . . ? H1A B1 H1C 105(2) . . ? H1B B1 H1C 91(3) . . ? H1G B2 H1H 112(4) . . ? H1G B2 H1F 101(3) . . ? H1H B2 H1F 100(3) . . ? H1G B2 Nd 66(2) . . ? H1H B2 Nd 68(3) . . ? H1F B2 Nd 65(2) . . ? H1G B2 H2E 113.9 . . ? H1H B2 H2E 113.9 . . ? H1F B2 H2E 113.9 . . ? Nd B2 H2E 178.1 . . ? H1G B2 H1F 101(3) . . ? H1H B2 H1F 100(3) . . ? Nd B2 H1F 65(2) . . ? H2E B2 H1F 113.9 . . ? H1H B2 H1G 112(4) . . ? H1F B2 H1G 101(3) . . ? Nd B2 H1G 66(2) . . ? H2E B2 H1G 113.9 . . ? H1F B2 H1G 101(3) . . ? H1G B2 H1H 112(4) . . ? H1F B2 H1H 100(3) . . ? Nd B2 H1H 68(3) . . ? H2E B2 H1H 113.9 . . ? H1F B2 H1H 100(3) . . ? H1G B2 H1H 112(4) . . ? C39 B3 C33 112.9(3) . . ? C39 B3 C27 111.9(4) . . ? C33 B3 C27 101.5(3) . . ? C39 B3 C21 101.9(3) . . ? C33 B3 C21 114.3(4) . . ? C27 B3 C21 114.8(3) . . ? C4 O1 C1 112.6(3) . . ? C4 O1 Nd 125.1(2) . . ? C1 O1 Nd 122.3(2) . . ? C5 O2 C8 110.2(3) . . ? C5 O2 Nd 123.9(2) . . ? C8 O2 Nd 125.9(2) . . ? C9 O3 C12 110.5(3) . . ? C9 O3 Nd 125.4(2) . . ? C12 O3 Nd 123.8(3) . . ? C13 O4 C16 110.0(3) . . ? C13 O4 Nd 122.7(2) . . ? C16 O4 Nd 127.3(3) . . ? C20 O5 C17 109.4(3) . . ? C20 O5 Nd 123.9(3) . . ? C17 O5 Nd 126.7(2) . . ? C2 C1 O1 102.4(3) . . ? C2 C1 H1I 111.3 . . ? O1 C1 H1I 111.3 . . ? C2 C1 H1J 111.3 . . ? O1 C1 H1J 111.3 . . ? H1I C1 H1J 109.2 . . ? C1 C2 C3 103.4(4) . . ? C1 C2 H2A 111.1 . . ? C3 C2 H2A 111.1 . . ? C1 C2 H2B 111.1 . . ? C3 C2 H2B 111.1 . . ? H2A C2 H2B 109.0 . . ? C4 C3 C2 104.4(4) . . ? C4 C3 H3A 110.9 . . ? C2 C3 H3A 110.9 . . ? C4 C3 H3B 110.9 . . ? C2 C3 H3B 110.9 . . ? H3A C3 H3B 108.9 . . ? O1 C4 C3 102.2(3) . . ? O1 C4 H4A 111.3 . . ? C3 C4 H4A 111.3 . . ? O1 C4 H4B 111.3 . . ? C3 C4 H4B 111.3 . . ? H4A C4 H4B 109.2 . . ? O2 C5 C6 104.4(3) . . ? O2 C5 H5A 110.9 . . ? C6 C5 H5A 110.9 . . ? O2 C5 H5B 110.9 . . ? C6 C5 H5B 110.9 . . ? H5A C5 H5B 108.9 . . ? C5 C6 C7 104.2(4) . . ? C5 C6 H6A 110.9 . . ? C7 C6 H6A 110.9 . . ? C5 C6 H6B 110.9 . . ? C7 C6 H6B 110.9 . . ? H6A C6 H6B 108.9 . . ? C8 C7 C6 103.9(4) . . ? C8 C7 H7A 111.0 . . ? C6 C7 H7A 111.0 . . ? C8 C7 H7B 111.0 . . ? C6 C7 H7B 111.0 . . ? H7A C7 H7B 109.0 . . ? O2 C8 C7 103.5(3) . . ? O2 C8 H8A 111.1 . . ? C7 C8 H8A 111.1 . . ? O2 C8 H8B 111.1 . . ? C7 C8 H8B 111.1 . . ? H8A C8 H8B 109.0 . . ? O3 C9 C10 103.5(3) . . ? O3 C9 H9A 111.1 . . ? C10 C9 H9A 111.1 . . ? O3 C9 H9B 111.1 . . ? C10 C9 H9B 111.1 . . ? H9A C9 H9B 109.0 . . ? C9 C10 C11 101.7(4) . . ? C9 C10 H10A 111.4 . . ? C11 C10 H10A 111.4 . . ? C9 C10 H10B 111.4 . . ? C11 C10 H10B 111.4 . . ? H10A C10 H10B 109.3 . . ? C12 C11 C10 105.0(3) . . ? C12 C11 H11A 110.7 . . ? C10 C11 H11A 110.7 . . ? C12 C11 H11B 110.7 . . ? C10 C11 H11B 110.7 . . ? H11A C11 H11B 108.8 . . ? C11 C12 O3 103.5(4) . . ? C11 C12 H12A 111.1 . . ? O3 C12 H12A 111.1 . . ? C11 C12 H12B 111.1 . . ? O3 C12 H12B 111.1 . . ? H12A C12 H12B 109.0 . . ? O4 C13 C14 101.4(3) . . ? O4 C13 H13A 111.5 . . ? C14 C13 H13A 111.5 . . ? O4 C13 H13B 111.5 . . ? C14 C13 H13B 111.5 . . ? H13A C13 H13B 109.3 . . ? C13 C14 C15 105.9(4) . . ? C13 C14 H14A 110.5 . . ? C15 C14 H14A 110.5 . . ? C13 C14 H14B 110.5 . . ? C15 C14 H14B 110.5 . . ? H14A C14 H14B 108.7 . . ? C16 C15 C14 104.4(4) . . ? C16 C15 H15A 110.9 . . ? C14 C15 H15A 110.9 . . ? C16 C15 H15B 110.9 . . ? C14 C15 H15B 110.9 . . ? H15A C15 H15B 108.9 . . ? O4 C16 C15 106.1(4) . . ? O4 C16 H16A 110.5 . . ? C15 C16 H16A 110.5 . . ? O4 C16 H16B 110.5 . . ? C15 C16 H16B 110.5 . . ? H16A C16 H16B 108.7 . . ? O5 C17 C18 105.1(4) . . ? O5 C17 H17A 110.7 . . ? C18 C17 H17A 110.7 . . ? O5 C17 H17B 110.7 . . ? C18 C17 H17B 110.7 . . ? H17A C17 H17B 108.8 . . ? C19 C18 C17 102.1(4) . . ? C19 C18 H18A 111.4 . . ? C17 C18 H18A 111.4 . . ? C19 C18 H18B 111.4 . . ? C17 C18 H18B 111.4 . . ? H18A C18 H18B 109.2 . . ? C18 C19 C20 104.7(4) . . ? C18 C19 H19A 110.8 . . ? C20 C19 H19A 110.8 . . ? C18 C19 H19B 110.8 . . ? C20 C19 H19B 110.8 . . ? H19A C19 H19B 108.9 . . ? O5 C20 C19 103.1(4) . . ? O5 C20 H20A 111.2 . . ? C19 C20 H20A 111.2 . . ? O5 C20 H20B 111.2 . . ? C19 C20 H20B 111.2 . . ? H20A C20 H20B 109.1 . . ? C22 C21 C26 113.9(4) . . ? C22 C21 B3 127.6(4) . . ? C26 C21 B3 118.3(4) . . ? C21 C22 C23 125.4(5) . . ? C21 C22 H22 117.3 . . ? C23 C22 H22 117.3 . . ? C24 C23 C22 118.4(4) . . ? C24 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? C25 C24 C23 118.9(4) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C24 C25 C26 120.8(4) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C25 C26 C21 122.6(4) . . ? C25 C26 H26 118.7 . . ? C21 C26 H26 118.7 . . ? C28 C27 C32 113.1(4) . . ? C28 C27 B3 122.1(3) . . ? C32 C27 B3 124.7(4) . . ? C27 C28 C29 121.5(4) . . ? C27 C28 H28 119.2 . . ? C29 C28 H28 119.2 . . ? C30 C29 C28 123.1(4) . . ? C30 C29 H29 118.5 . . ? C28 C29 H29 118.5 . . ? C31 C30 C29 117.4(4) . . ? C31 C30 H30 121.3 . . ? C29 C30 H30 121.3 . . ? C30 C31 C32 119.1(5) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C31 C32 C27 125.7(5) . . ? C31 C32 H32 117.1 . . ? C27 C32 H32 117.1 . . ? C38 C33 C34 113.0(4) . . ? C38 C33 B3 120.6(4) . . ? C34 C33 B3 126.0(4) . . ? C33 C34 C35 123.9(4) . . ? C33 C34 H34 118.0 . . ? C35 C34 H34 118.0 . . ? C36 C35 C34 121.2(4) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C35 C36 C37 116.5(4) . . ? C35 C36 H36 121.8 . . ? C37 C36 H36 121.8 . . ? C36 C37 C38 122.2(5) . . ? C36 C37 H37 118.9 . . ? C38 C37 H37 118.9 . . ? C33 C38 C37 123.0(5) . . ? C33 C38 H38 118.5 . . ? C37 C38 H38 118.5 . . ? C44 C39 C40 114.6(4) . . ? C44 C39 B3 118.3(4) . . ? C40 C39 B3 127.1(4) . . ? C41 C40 C39 124.3(4) . . ? C41 C40 H40 117.8 . . ? C39 C40 H40 117.8 . . ? C40 C41 C42 118.3(5) . . ? C40 C41 H41 120.9 . . ? C42 C41 H41 120.9 . . ? C43 C42 C41 120.2(4) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 120.0(5) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C43 C44 C39 122.6(5) . . ? C43 C44 H44 118.7 . . ? C39 C44 H44 118.7 . . ? _diffrn_measured_fraction_theta_max 0.826 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.484 _refine_diff_density_min -0.988 _refine_diff_density_rms 0.114 #==END #========================================================================== data_dr1460 _database_code_depnum_ccdc_archive 'CCDC 674070' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H48 B2 O5 Sm, C24 H20 B' _chemical_formula_sum 'C44 H68 B3 O5 Sm' _chemical_formula_weight 859.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall -P2ybc 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 13.070(6) _cell_length_b 13.534(6) _cell_length_c 24.936(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.071(9) _cell_angle_gamma 90.00 _cell_volume 4411(3) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 976 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 22.44 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1796 _exptl_absorpt_coefficient_mu 1.372 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6836 _exptl_absorpt_correction_T_max 0.8103 _exptl_absorpt_process_details Platon _exptl_special_details ? _diffrn_ambient_temperature 130(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 54897 _diffrn_reflns_av_R_equivalents 0.0843 _diffrn_reflns_av_sigmaI/netI 0.0843 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 0.82 _diffrn_reflns_theta_max 29.40 _reflns_number_total 11001 _reflns_number_gt 7937 _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 SHELXT' _computing_publication_material 'Bruker SHELXT' _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. Only a part of hydrogen atoms could be refined. B-H bonds were restrained to a value of 1.2 A, inter hydrogen atoms were constrained to common isotropic displacement parameters. Only a part of hydrogen atoms could be refined. Crystal of dr1460 shows monoclinic angles very close to 90 degrees, is pseudo-merohedral twin with apparent Laue symmetry mmm. ; _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^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11001 _refine_ls_number_parameters 503 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.008 _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 Sm Sm 0.797727(17) 0.821827(15) 0.75154(3) 0.02155(6) Uani 1 1 d . . . B1 B 0.8186(3) 1.0193(3) 0.7553(4) 0.0168(12) Uani 1 1 d D . . H1A H 0.814(3) 1.1042(13) 0.756(2) 0.020 Uiso 1 1 d D . . H1B H 0.842(3) 0.987(3) 0.7958(11) 0.020 Uiso 1 1 d D . . H1C H 0.862(3) 0.981(3) 0.7198(13) 0.020 Uiso 1 1 d D . . H1D H 0.7378(16) 0.987(3) 0.7591(18) 0.020 Uiso 1 1 d D . . B2 B 0.7729(3) 0.6218(4) 0.7482(5) 0.0340(14) Uani 1 1 d D . . H1E H 0.851(2) 0.647(3) 0.7321(18) 0.041 Uiso 1 1 d D . . H1F H 0.753(3) 0.5377(16) 0.740(2) 0.041 Uiso 1 1 d D . . H1G H 0.762(4) 0.659(4) 0.7915(11) 0.041 Uiso 1 1 d D . . H1H H 0.724(3) 0.668(3) 0.7162(15) 0.041 Uiso 1 1 d D . . B3 B 0.3110(4) 0.7636(5) 1.0065(3) 0.0179(14) Uani 1 1 d . . . O1 O 0.6137(2) 0.8384(2) 0.7502(3) 0.0294(8) Uani 1 1 d . . . O2 O 0.7322(3) 0.8291(3) 0.84406(18) 0.0221(10) Uani 1 1 d . . . O3 O 0.9344(3) 0.7954(3) 0.81623(17) 0.0277(11) Uani 1 1 d . . . O4 O 0.9579(3) 0.8086(3) 0.70196(18) 0.0293(11) Uani 1 1 d . . . O5 O 0.7606(3) 0.8473(3) 0.65628(19) 0.0274(11) Uani 1 1 d . . . C1 C 0.5587(4) 0.9229(4) 0.7250(2) 0.0346(15) Uani 1 1 d . . . H1I H 0.5666 0.9838 0.7467 0.042 Uiso 1 1 calc R . . H1J H 0.5842 0.9355 0.6883 0.042 Uiso 1 1 calc R . . C2 C 0.4506(4) 0.8900(5) 0.7240(3) 0.0409(17) Uani 1 1 d . . . H2A H 0.4348 0.8540 0.6905 0.049 Uiso 1 1 calc R . . H2B H 0.4033 0.9467 0.7276 0.049 Uiso 1 1 calc R . . C3 C 0.4437(4) 0.8215(5) 0.7726(3) 0.0448(17) Uani 1 1 d . . . H3A H 0.4353 0.8601 0.8061 0.054 Uiso 1 1 calc R . . H3B H 0.3853 0.7754 0.7690 0.054 Uiso 1 1 calc R . . C4 C 0.5436(4) 0.7661(4) 0.7730(2) 0.0372(15) Uani 1 1 d . . . H4A H 0.5640 0.7476 0.8099 0.045 Uiso 1 1 calc R . . H4B H 0.5398 0.7058 0.7506 0.045 Uiso 1 1 calc R . . C5 C 0.6806(4) 0.9174(4) 0.8674(2) 0.0330(14) Uani 1 1 d . . . H5A H 0.6243 0.9405 0.8440 0.040 Uiso 1 1 calc R . . H5B H 0.7298 0.9722 0.8727 0.040 Uiso 1 1 calc R . . C6 C 0.6402(6) 0.8815(6) 0.9200(3) 0.046(2) Uani 1 1 d . . . H6A H 0.5696 0.8561 0.9160 0.056 Uiso 1 1 calc R . . H6B H 0.6402 0.9353 0.9469 0.056 Uiso 1 1 calc R . . C7 C 0.7120(5) 0.7999(4) 0.9367(2) 0.0366(15) Uani 1 1 d . . . H7A H 0.6783 0.7540 0.9621 0.044 Uiso 1 1 calc R . . H7B H 0.7744 0.8270 0.9538 0.044 Uiso 1 1 calc R . . C8 C 0.7373(4) 0.7485(4) 0.8844(2) 0.0293(14) Uani 1 1 d . . . H8A H 0.8065 0.7189 0.8857 0.035 Uiso 1 1 calc R . . H8B H 0.6868 0.6960 0.8763 0.035 Uiso 1 1 calc R . . C9 C 0.9633(4) 0.8645(4) 0.8593(2) 0.0347(14) Uani 1 1 d . . . H9A H 0.9020 0.8942 0.8761 0.042 Uiso 1 1 calc R . . H9B H 1.0079 0.9178 0.8455 0.042 Uiso 1 1 calc R . . C10 C 1.0198(4) 0.7994(5) 0.8982(2) 0.0389(16) Uani 1 1 d . . . H10A H 0.9722 0.7665 0.9233 0.047 Uiso 1 1 calc R . . H10B H 1.0710 0.8375 0.9189 0.047 Uiso 1 1 calc R . . C11 C 1.0715(5) 0.7245(6) 0.8611(3) 0.045(2) Uani 1 1 d . . . H11A H 1.1345 0.7528 0.8453 0.054 Uiso 1 1 calc R . . H11B H 1.0896 0.6637 0.8810 0.054 Uiso 1 1 calc R . . C12 C 0.9961(5) 0.7028(5) 0.8191(3) 0.0346(17) Uani 1 1 d . . . H12A H 0.9528 0.6457 0.8291 0.042 Uiso 1 1 calc R . . H12B H 1.0299 0.6889 0.7845 0.042 Uiso 1 1 calc R . . C13 C 1.0417(4) 0.8795(4) 0.7090(2) 0.0355(14) Uani 1 1 d . . . H13A H 1.0441 0.9059 0.7460 0.043 Uiso 1 1 calc R . . H13B H 1.0367 0.9350 0.6832 0.043 Uiso 1 1 calc R . . C14 C 1.1317(4) 0.8145(5) 0.6973(3) 0.0452(17) Uani 1 1 d . . . H14A H 1.1525 0.7778 0.7298 0.054 Uiso 1 1 calc R . . H14B H 1.1904 0.8545 0.6848 0.054 Uiso 1 1 calc R . . C15 C 1.0976(5) 0.7442(5) 0.6541(3) 0.0393(19) Uani 1 1 d . . . H15A H 1.1127 0.7712 0.6181 0.047 Uiso 1 1 calc R . . H15B H 1.1322 0.6795 0.6580 0.047 Uiso 1 1 calc R . . C16 C 0.9843(6) 0.7340(6) 0.6623(3) 0.058(2) Uani 1 1 d . . . H16A H 0.9470 0.7457 0.6283 0.069 Uiso 1 1 calc R . . H16B H 0.9672 0.6671 0.6756 0.069 Uiso 1 1 calc R . . C17 C 0.8034(5) 0.9243(4) 0.6197(2) 0.0380(14) Uani 1 1 d . . . H17A H 0.8790 0.9248 0.6216 0.046 Uiso 1 1 calc R . . H17B H 0.7778 0.9905 0.6298 0.046 Uiso 1 1 calc R . . C18 C 0.7687(4) 0.8981(6) 0.5642(3) 0.0511(19) Uani 1 1 d . . . H18A H 0.7574 0.9578 0.5420 0.061 Uiso 1 1 calc R . . H18B H 0.8184 0.8542 0.5460 0.061 Uiso 1 1 calc R . . C19 C 0.6707(5) 0.8458(6) 0.5757(3) 0.044(2) Uani 1 1 d . . . H19A H 0.6506 0.8034 0.5451 0.052 Uiso 1 1 calc R . . H19B H 0.6151 0.8938 0.5826 0.052 Uiso 1 1 calc R . . C20 C 0.6914(4) 0.7839(4) 0.6249(2) 0.0344(14) Uani 1 1 d . . . H20A H 0.6275 0.7700 0.6449 0.041 Uiso 1 1 calc R . . H20B H 0.7246 0.7206 0.6154 0.041 Uiso 1 1 calc R . . C21 C 0.2507(4) 0.8619(4) 0.9806(3) 0.0211(13) Uani 1 1 d . . . C22 C 0.2680(5) 0.9055(5) 0.9316(3) 0.0271(18) Uani 1 1 d . . . H22 H 0.3163 0.8753 0.9084 0.033 Uiso 1 1 calc R . . C23 C 0.2181(5) 0.9930(5) 0.9133(3) 0.0304(17) Uani 1 1 d . . . H23 H 0.2332 1.0197 0.8789 0.036 Uiso 1 1 calc R . . C24 C 0.1470(4) 1.0384(5) 0.9467(3) 0.0408(17) Uani 1 1 d . . . H24 H 0.1105 1.0954 0.9351 0.049 Uiso 1 1 calc R . . C25 C 0.1304(4) 0.9980(4) 0.9978(3) 0.0362(15) Uani 1 1 d . . . H25 H 0.0839 1.0296 1.0215 0.043 Uiso 1 1 calc R . . C26 C 0.1807(4) 0.9124(4) 1.0144(2) 0.0304(13) Uani 1 1 d . . . H26 H 0.1678 0.8872 1.0493 0.036 Uiso 1 1 calc R . . C27 C 0.2346(4) 0.6764(4) 1.0304(3) 0.0244(13) Uani 1 1 d . . . C28 C 0.1347(4) 0.6683(4) 1.0143(2) 0.0305(13) Uani 1 1 d . . . H28 H 0.1073 0.7156 0.9900 0.037 Uiso 1 1 calc R . . C29 C 0.0720(4) 0.5917(4) 1.0330(2) 0.0338(14) Uani 1 1 d . . . H29 H 0.0026 0.5903 1.0217 0.041 Uiso 1 1 calc R . . C30 C 0.1066(4) 0.5170(4) 1.0674(2) 0.0356(14) Uani 1 1 d . . . H30 H 0.0634 0.4644 1.0785 0.043 Uiso 1 1 calc R . . C31 C 0.2022(6) 0.5237(5) 1.0836(3) 0.0338(17) Uani 1 1 d . . . H31 H 0.2287 0.4763 1.1080 0.041 Uiso 1 1 calc R . . C32 C 0.2647(6) 0.5995(5) 1.0652(3) 0.032(2) Uani 1 1 d . . . H32 H 0.3338 0.5996 1.0771 0.038 Uiso 1 1 calc R . . C33 C 0.3785(5) 0.7002(5) 0.9617(3) 0.0238(16) Uani 1 1 d . . . C34 C 0.3487(5) 0.6782(5) 0.9088(3) 0.0327(18) Uani 1 1 d . . . H34 H 0.2848 0.7034 0.8967 0.039 Uiso 1 1 calc R . . C35 C 0.4048(5) 0.6232(5) 0.8734(3) 0.0353(16) Uani 1 1 d . . . H35 H 0.3815 0.6150 0.8376 0.042 Uiso 1 1 calc R . . C36 C 0.4945(5) 0.5801(5) 0.8894(3) 0.0328(17) Uani 1 1 d . . . H36 H 0.5351 0.5422 0.8654 0.039 Uiso 1 1 calc R . . C37 C 0.5228(6) 0.5944(5) 0.9415(3) 0.0320(18) Uani 1 1 d . . . H37 H 0.5834 0.5636 0.9542 0.038 Uiso 1 1 calc R . . C38 C 0.4660(5) 0.6525(5) 0.9768(3) 0.0228(15) Uani 1 1 d . . . H38 H 0.4891 0.6591 1.0127 0.027 Uiso 1 1 calc R . . C39 C 0.3799(5) 0.8110(5) 1.0523(3) 0.0244(16) Uani 1 1 d . . . C40 C 0.3629(5) 0.8071(5) 1.1068(3) 0.0284(16) Uani 1 1 d . . . H40 H 0.3053 0.7710 1.1193 0.034 Uiso 1 1 calc R . . C41 C 0.4253(5) 0.8528(4) 1.1447(3) 0.0325(16) Uani 1 1 d . . . H41 H 0.4097 0.8486 1.1819 0.039 Uiso 1 1 calc R . . C42 C 0.5094(5) 0.9038(5) 1.1275(3) 0.0371(19) Uani 1 1 d . . . H42 H 0.5538 0.9340 1.1528 0.045 Uiso 1 1 calc R . . C43 C 0.5299(6) 0.9116(6) 1.0733(3) 0.039(2) Uani 1 1 d . . . H43 H 0.5871 0.9488 1.0613 0.046 Uiso 1 1 calc R . . C44 C 0.4674(5) 0.8653(5) 1.0372(3) 0.0285(17) Uani 1 1 d . . . H44 H 0.4836 0.8699 1.0001 0.034 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 Sm 0.01575(9) 0.01838(10) 0.03051(12) 0.0003(2) -0.0031(4) -0.00096(10) B1 0.017(2) 0.006(2) 0.028(3) -0.003(3) 0.004(3) -0.0031(16) B2 0.019(2) 0.032(3) 0.050(4) -0.006(5) -0.017(5) -0.005(2) B3 0.014(2) 0.011(4) 0.028(4) -0.008(3) 0.002(3) 0.000(3) O1 0.0256(14) 0.0317(19) 0.0309(19) -0.008(3) -0.010(4) -0.0008(13) O2 0.020(2) 0.014(2) 0.032(2) 0.0030(17) 0.0034(17) 0.0031(17) O3 0.017(2) 0.030(3) 0.036(3) -0.003(2) -0.0040(18) 0.0012(18) O4 0.018(2) 0.029(3) 0.041(3) -0.002(2) 0.0111(19) -0.0023(18) O5 0.019(2) 0.035(3) 0.028(2) -0.0043(18) 0.0016(17) -0.0122(17) C1 0.027(3) 0.033(4) 0.044(4) 0.011(3) -0.011(2) 0.006(3) C2 0.018(3) 0.048(4) 0.056(4) 0.015(3) -0.005(3) -0.001(3) C3 0.027(3) 0.056(4) 0.051(4) 0.017(4) 0.008(2) 0.002(3) C4 0.024(3) 0.039(4) 0.049(4) 0.011(3) 0.003(2) 0.005(3) C5 0.033(3) 0.025(3) 0.042(4) -0.001(3) 0.010(3) 0.010(2) C6 0.045(4) 0.058(5) 0.036(4) -0.008(4) 0.013(3) 0.002(4) C7 0.041(4) 0.036(4) 0.033(3) 0.004(3) 0.006(3) -0.005(3) C8 0.027(3) 0.024(3) 0.037(4) 0.012(3) -0.001(3) -0.004(2) C9 0.024(3) 0.036(3) 0.044(4) 0.001(3) -0.010(3) -0.009(2) C10 0.025(3) 0.054(4) 0.037(4) 0.006(3) -0.008(3) -0.009(3) C11 0.019(3) 0.071(5) 0.046(5) 0.016(4) 0.000(3) 0.007(3) C12 0.017(3) 0.035(4) 0.052(4) 0.001(3) -0.003(3) 0.011(3) C13 0.019(3) 0.048(4) 0.040(4) -0.001(3) -0.001(2) -0.002(3) C14 0.022(3) 0.052(4) 0.062(5) 0.017(4) 0.009(3) -0.004(3) C15 0.024(3) 0.064(5) 0.030(4) 0.011(3) 0.009(3) 0.026(3) C16 0.045(5) 0.054(6) 0.075(6) -0.032(5) 0.023(4) -0.010(4) C17 0.038(3) 0.048(4) 0.028(3) 0.010(3) 0.001(3) -0.014(3) C18 0.033(3) 0.075(5) 0.046(5) 0.000(4) 0.002(3) -0.002(3) C19 0.034(4) 0.054(5) 0.043(5) -0.011(4) -0.007(3) 0.006(3) C20 0.026(3) 0.033(3) 0.044(4) -0.012(3) -0.003(3) -0.007(3) C21 0.011(2) 0.012(3) 0.039(4) 0.000(3) -0.002(2) -0.003(2) C22 0.014(4) 0.019(4) 0.048(5) 0.003(3) -0.002(3) -0.007(3) C23 0.018(3) 0.021(4) 0.052(4) 0.012(3) -0.011(3) -0.009(3) C24 0.033(3) 0.020(3) 0.069(5) 0.007(3) -0.022(3) 0.003(3) C25 0.024(3) 0.029(3) 0.056(4) -0.011(3) -0.011(3) 0.003(2) C26 0.021(3) 0.027(3) 0.043(4) -0.005(3) -0.005(2) 0.002(2) C27 0.019(3) 0.014(3) 0.040(4) -0.004(3) -0.002(2) 0.001(2) C28 0.021(3) 0.035(4) 0.035(4) -0.006(3) -0.002(2) -0.002(3) C29 0.020(3) 0.032(3) 0.049(4) -0.006(3) -0.002(3) -0.012(2) C30 0.035(3) 0.023(3) 0.049(4) -0.007(3) 0.007(3) -0.011(3) C31 0.034(4) 0.021(3) 0.046(4) 0.005(3) 0.005(4) 0.008(3) C32 0.026(4) 0.028(5) 0.042(5) -0.004(4) -0.003(3) 0.000(3) C33 0.016(3) 0.018(3) 0.037(4) 0.001(3) -0.008(3) -0.007(3) C34 0.019(3) 0.032(4) 0.047(5) -0.004(3) -0.003(3) -0.003(3) C35 0.041(4) 0.032(4) 0.033(4) 0.006(3) -0.004(3) -0.017(3) C36 0.021(3) 0.020(3) 0.058(5) -0.012(3) 0.012(3) -0.001(3) C37 0.021(4) 0.024(4) 0.051(5) -0.011(3) 0.002(3) -0.001(3) C38 0.017(3) 0.022(4) 0.029(4) -0.008(3) 0.002(2) 0.004(2) C39 0.017(3) 0.019(3) 0.038(4) -0.003(3) -0.004(3) 0.005(3) C40 0.025(3) 0.018(4) 0.043(4) -0.002(3) 0.002(3) 0.004(3) C41 0.034(3) 0.022(4) 0.041(4) -0.007(3) -0.012(3) 0.008(3) C42 0.038(4) 0.024(4) 0.049(5) -0.008(3) -0.023(3) 0.011(3) C43 0.013(3) 0.034(4) 0.068(6) -0.015(4) -0.007(3) -0.001(3) C44 0.020(3) 0.028(4) 0.038(4) -0.010(3) 0.001(3) 0.002(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 Sm O1 2.416(3) . ? Sm O3 2.432(4) . ? Sm O4 2.439(4) . ? Sm O5 2.448(5) . ? Sm O2 2.464(5) . ? Sm B1 2.688(5) . ? Sm B2 2.728(6) . ? Sm H1B 2.56(5) . ? Sm H1C 2.45(5) . ? Sm H1D 2.38(4) . ? Sm H1E 2.51(4) . ? Sm H1G 2.46(5) . ? Sm H1H 2.46(5) . ? B1 H1A 1.150(18) . ? B1 H1B 1.143(18) . ? B1 H1C 1.169(18) . ? B1 H1D 1.146(17) . ? B2 H1E 1.148(19) . ? B2 H1F 1.184(18) . ? B2 H1G 1.201(19) . ? B2 H1H 1.199(18) . ? B3 C39 1.588(8) . ? B3 C27 1.657(9) . ? B3 C33 1.663(8) . ? B3 C21 1.676(9) . ? O1 C4 1.456(7) . ? O1 C1 1.490(6) . ? O2 C8 1.486(7) . ? O2 C5 1.492(6) . ? O3 C9 1.472(7) . ? O3 C12 1.491(7) . ? O4 C16 1.455(8) . ? O4 C13 1.466(7) . ? O5 C20 1.472(6) . ? O5 C17 1.494(7) . ? C1 C2 1.481(7) . ? C1 H1I 0.9900 . ? C1 H1J 0.9900 . ? C2 C3 1.528(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.505(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.495(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.507(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.515(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.504(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.530(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.466(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.498(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.504(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.501(9) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.498(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.492(9) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.511(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.377(9) . ? C21 C26 1.419(8) . ? C22 C23 1.426(9) . ? C22 H22 0.9500 . ? C23 C24 1.393(10) . ? C23 H23 0.9500 . ? C24 C25 1.404(9) . ? C24 H24 0.9500 . ? C25 C26 1.396(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.371(7) . ? C27 C32 1.410(9) . ? C28 C29 1.402(7) . ? C28 H28 0.9500 . ? C29 C30 1.400(8) . ? C29 H29 0.9500 . ? C30 C31 1.316(10) . ? C30 H30 0.9500 . ? C31 C32 1.390(10) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.365(9) . ? C33 C34 1.408(9) . ? C34 C35 1.369(9) . ? C34 H34 0.9500 . ? C35 C36 1.369(9) . ? C35 H35 0.9500 . ? C36 C37 1.365(9) . ? C36 H36 0.9500 . ? C37 C38 1.395(8) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.381(9) . ? C39 C44 1.410(10) . ? C40 C41 1.392(9) . ? C40 H40 0.9500 . ? C41 C42 1.368(9) . ? C41 H41 0.9500 . ? C42 C43 1.381(10) . ? C42 H42 0.9500 . ? C43 C44 1.368(9) . ? C43 H43 0.9500 . ? C44 H44 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 O1 Sm O3 138.9(2) . . ? O1 Sm O4 148.8(3) . . ? O3 Sm O4 72.25(15) . . ? O1 Sm O5 77.2(2) . . ? O3 Sm O5 143.96(14) . . ? O4 Sm O5 71.79(15) . . ? O1 Sm O2 70.2(2) . . ? O3 Sm O2 68.94(14) . . ? O4 Sm O2 140.99(14) . . ? O5 Sm O2 146.54(11) . . ? O1 Sm B1 90.55(11) . . ? O3 Sm B1 92.81(18) . . ? O4 Sm B1 90.17(16) . . ? O5 Sm B1 85.0(2) . . ? O2 Sm B1 87.9(2) . . ? O1 Sm B2 88.45(12) . . ? O3 Sm B2 87.8(2) . . ? O4 Sm B2 90.80(19) . . ? O5 Sm B2 95.0(3) . . ? O2 Sm B2 91.5(3) . . ? B1 Sm B2 178.97(16) . . ? O1 Sm H1B 98.6(9) . . ? O3 Sm H1B 71.1(6) . . ? O4 Sm H1B 95.1(10) . . ? O5 Sm H1B 109.9(5) . . ? O2 Sm H1B 68.9(8) . . ? B1 Sm H1B 25.0(4) . . ? B2 Sm H1B 155.1(5) . . ? O1 Sm H1C 104.8(8) . . ? O3 Sm H1C 95.3(10) . . ? O4 Sm H1C 66.8(6) . . ? O5 Sm H1C 68.2(8) . . ? O2 Sm H1C 112.8(5) . . ? B1 Sm H1C 25.8(4) . . ? B2 Sm H1C 155.0(5) . . ? H1B Sm H1C 44.9(8) . . ? O1 Sm H1D 65.6(5) . . ? O3 Sm H1D 109.1(9) . . ? O4 Sm H1D 113.1(6) . . ? O5 Sm H1D 83.1(11) . . ? O2 Sm H1D 76.9(10) . . ? B1 Sm H1D 25.2(4) . . ? B2 Sm H1D 153.8(5) . . ? H1B Sm H1D 38.6(10) . . ? H1C Sm H1D 46.2(7) . . ? O1 Sm H1E 111.1(6) . . ? O3 Sm H1E 77.7(10) . . ? O4 Sm H1E 66.1(5) . . ? O5 Sm H1E 90.0(11) . . ? O2 Sm H1E 108.4(9) . . ? B1 Sm H1E 156.1(5) . . ? B2 Sm H1E 24.9(4) . . ? H1B Sm H1E 147.5(12) . . ? H1C Sm H1E 132.3(7) . . ? H1D Sm H1E 172.8(14) . . ? O1 Sm H1G 84.3(11) . . ? O3 Sm H1G 74.8(10) . . ? O4 Sm H1G 107.5(9) . . ? O5 Sm H1G 118.8(6) . . ? O2 Sm H1G 65.9(6) . . ? B1 Sm H1G 153.5(5) . . ? B2 Sm H1G 26.1(4) . . ? H1B Sm H1G 130.5(8) . . ? H1C Sm H1G 169.9(14) . . ? H1D Sm H1G 138.4(11) . . ? H1E Sm H1G 44.6(10) . . ? O1 Sm H1H 71.5(10) . . ? O3 Sm H1H 113.7(5) . . ? O4 Sm H1H 95.4(11) . . ? O5 Sm H1H 72.2(7) . . ? O2 Sm H1H 103.4(10) . . ? B1 Sm H1H 153.4(5) . . ? B2 Sm H1H 26.1(4) . . ? H1B Sm H1H 169.4(14) . . ? H1C Sm H1H 140.0(11) . . ? H1D Sm H1H 134.1(10) . . ? H1E Sm H1H 40.7(11) . . ? H1G Sm H1H 46.6(8) . . ? Sm B1 H1A 171.3(17) . . ? Sm B1 H1B 71(2) . . ? H1A B1 H1B 112(3) . . ? Sm B1 H1C 65(2) . . ? H1A B1 H1C 118(3) . . ? H1B B1 H1C 112(3) . . ? Sm B1 H1D 62.2(18) . . ? H1A B1 H1D 109(3) . . ? H1B B1 H1D 92(3) . . ? H1C B1 H1D 110(3) . . ? Sm B2 H1E 67(2) . . ? Sm B2 H1F 170(3) . . ? H1E B2 H1F 115(3) . . ? Sm B2 H1G 65(3) . . ? H1E B2 H1G 107(4) . . ? H1F B2 H1G 122(4) . . ? Sm B2 H1H 65(2) . . ? H1E B2 H1H 95(3) . . ? H1F B2 H1H 106(4) . . ? H1G B2 H1H 109(3) . . ? C39 B3 C27 111.8(6) . . ? C39 B3 C33 113.0(4) . . ? C27 B3 C33 101.3(4) . . ? C39 B3 C21 102.8(4) . . ? C27 B3 C21 114.9(4) . . ? C33 B3 C21 113.6(6) . . ? C4 O1 C1 112.2(4) . . ? C4 O1 Sm 124.0(3) . . ? C1 O1 Sm 123.8(3) . . ? C8 O2 C5 110.1(4) . . ? C8 O2 Sm 126.2(3) . . ? C5 O2 Sm 123.8(3) . . ? C9 O3 C12 111.1(4) . . ? C9 O3 Sm 125.2(3) . . ? C12 O3 Sm 123.5(3) . . ? C16 O4 C13 110.9(5) . . ? C16 O4 Sm 126.9(4) . . ? C13 O4 Sm 122.2(3) . . ? C20 O5 C17 108.2(5) . . ? C20 O5 Sm 123.6(4) . . ? C17 O5 Sm 128.1(3) . . ? C2 C1 O1 103.6(4) . . ? C2 C1 H1I 111.0 . . ? O1 C1 H1I 111.0 . . ? C2 C1 H1J 111.0 . . ? O1 C1 H1J 111.0 . . ? H1I C1 H1J 109.0 . . ? C1 C2 C3 103.1(5) . . ? C1 C2 H2A 111.2 . . ? C3 C2 H2A 111.2 . . ? C1 C2 H2B 111.2 . . ? C3 C2 H2B 111.2 . . ? H2A C2 H2B 109.1 . . ? C4 C3 C2 104.8(5) . . ? C4 C3 H3A 110.8 . . ? C2 C3 H3A 110.8 . . ? C4 C3 H3B 110.8 . . ? C2 C3 H3B 110.8 . . ? H3A C3 H3B 108.9 . . ? O1 C4 C3 102.0(4) . . ? O1 C4 H4A 111.4 . . ? C3 C4 H4A 111.4 . . ? O1 C4 H4B 111.4 . . ? C3 C4 H4B 111.4 . . ? H4A C4 H4B 109.2 . . ? O2 C5 C6 104.0(5) . . ? O2 C5 H5A 111.0 . . ? C6 C5 H5A 111.0 . . ? O2 C5 H5B 111.0 . . ? C6 C5 H5B 111.0 . . ? H5A C5 H5B 109.0 . . ? C5 C6 C7 105.1(5) . . ? C5 C6 H6A 110.7 . . ? C7 C6 H6A 110.7 . . ? C5 C6 H6B 110.7 . . ? C7 C6 H6B 110.7 . . ? H6A C6 H6B 108.8 . . ? C6 C7 C8 103.6(5) . . ? C6 C7 H7A 111.0 . . ? C8 C7 H7A 111.0 . . ? C6 C7 H7B 111.0 . . ? C8 C7 H7B 111.0 . . ? H7A C7 H7B 109.0 . . ? O2 C8 C7 103.7(5) . . ? O2 C8 H8A 111.0 . . ? C7 C8 H8A 111.0 . . ? O2 C8 H8B 111.0 . . ? C7 C8 H8B 111.0 . . ? H8A C8 H8B 109.0 . . ? O3 C9 C10 102.9(5) . . ? O3 C9 H9A 111.2 . . ? C10 C9 H9A 111.2 . . ? O3 C9 H9B 111.2 . . ? C10 C9 H9B 111.2 . . ? H9A C9 H9B 109.1 . . ? C9 C10 C11 102.4(5) . . ? C9 C10 H10A 111.3 . . ? C11 C10 H10A 111.3 . . ? C9 C10 H10B 111.3 . . ? C11 C10 H10B 111.3 . . ? H10A C10 H10B 109.2 . . ? C12 C11 C10 105.5(5) . . ? C12 C11 H11A 110.6 . . ? C10 C11 H11A 110.6 . . ? C12 C11 H11B 110.6 . . ? C10 C11 H11B 110.6 . . ? H11A C11 H11B 108.8 . . ? C11 C12 O3 103.2(5) . . ? C11 C12 H12A 111.1 . . ? O3 C12 H12A 111.1 . . ? C11 C12 H12B 111.1 . . ? O3 C12 H12B 111.1 . . ? H12A C12 H12B 109.1 . . ? O4 C13 C14 100.3(5) . . ? O4 C13 H13A 111.7 . . ? C14 C13 H13A 111.7 . . ? O4 C13 H13B 111.7 . . ? C14 C13 H13B 111.7 . . ? H13A C13 H13B 109.5 . . ? C13 C14 C15 106.2(5) . . ? C13 C14 H14A 110.5 . . ? C15 C14 H14A 110.5 . . ? C13 C14 H14B 110.5 . . ? C15 C14 H14B 110.5 . . ? H14A C14 H14B 108.7 . . ? C16 C15 C14 104.6(6) . . ? C16 C15 H15A 110.8 . . ? C14 C15 H15A 110.8 . . ? C16 C15 H15B 110.8 . . ? C14 C15 H15B 110.8 . . ? H15A C15 H15B 108.9 . . ? O4 C16 C15 105.3(6) . . ? O4 C16 H16A 110.7 . . ? C15 C16 H16A 110.7 . . ? O4 C16 H16B 110.7 . . ? C15 C16 H16B 110.7 . . ? H16A C16 H16B 108.8 . . ? O5 C17 C18 106.6(5) . . ? O5 C17 H17A 110.4 . . ? C18 C17 H17A 110.4 . . ? O5 C17 H17B 110.4 . . ? C18 C17 H17B 110.4 . . ? H17A C17 H17B 108.6 . . ? C19 C18 C17 101.1(5) . . ? C19 C18 H18A 111.5 . . ? C17 C18 H18A 111.5 . . ? C19 C18 H18B 111.5 . . ? C17 C18 H18B 111.5 . . ? H18A C18 H18B 109.4 . . ? C18 C19 C20 105.5(5) . . ? C18 C19 H19A 110.6 . . ? C20 C19 H19A 110.6 . . ? C18 C19 H19B 110.6 . . ? C20 C19 H19B 110.6 . . ? H19A C19 H19B 108.8 . . ? O5 C20 C19 102.6(5) . . ? O5 C20 H20A 111.3 . . ? C19 C20 H20A 111.3 . . ? O5 C20 H20B 111.3 . . ? C19 C20 H20B 111.3 . . ? H20A C20 H20B 109.2 . . ? C22 C21 C26 115.3(6) . . ? C22 C21 B3 127.2(6) . . ? C26 C21 B3 117.2(5) . . ? C21 C22 C23 124.4(7) . . ? C21 C22 H22 117.8 . . ? C23 C22 H22 117.8 . . ? C24 C23 C22 118.7(7) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C25 118.3(6) . . ? C23 C24 H24 120.8 . . ? C25 C24 H24 120.8 . . ? C26 C25 C24 121.4(6) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C25 C26 C21 121.8(6) . . ? C25 C26 H26 119.1 . . ? C21 C26 H26 119.1 . . ? C28 C27 C32 112.7(6) . . ? C28 C27 B3 121.7(5) . . ? C32 C27 B3 125.4(5) . . ? C27 C28 C29 121.2(6) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C30 C29 C28 123.3(5) . . ? C30 C29 H29 118.3 . . ? C28 C29 H29 118.3 . . ? C31 C30 C29 116.3(6) . . ? C31 C30 H30 121.8 . . ? C29 C30 H30 121.8 . . ? C30 C31 C32 120.6(7) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C31 C32 C27 125.7(7) . . ? C31 C32 H32 117.1 . . ? C27 C32 H32 117.1 . . ? C38 C33 C34 112.9(6) . . ? C38 C33 B3 120.2(6) . . ? C34 C33 B3 126.3(6) . . ? C35 C34 C33 124.9(7) . . ? C35 C34 H34 117.6 . . ? C33 C34 H34 117.6 . . ? C36 C35 C34 120.2(7) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C37 C36 C35 116.6(6) . . ? C37 C36 H36 121.7 . . ? C35 C36 H36 121.7 . . ? C36 C37 C38 122.5(7) . . ? C36 C37 H37 118.8 . . ? C38 C37 H37 118.8 . . ? C33 C38 C37 122.6(7) . . ? C33 C38 H38 118.7 . . ? C37 C38 H38 118.7 . . ? C40 C39 C44 114.5(6) . . ? C40 C39 B3 126.9(6) . . ? C44 C39 B3 118.6(6) . . ? C39 C40 C41 123.9(7) . . ? C39 C40 H40 118.1 . . ? C41 C40 H40 118.1 . . ? C42 C41 C40 118.7(7) . . ? C42 C41 H41 120.6 . . ? C40 C41 H41 120.6 . . ? C41 C42 C43 120.2(7) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C44 C43 C42 119.5(8) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C43 C44 C39 123.1(7) . . ? C43 C44 H44 118.4 . . ? C39 C44 H44 118.4 . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.448 _refine_diff_density_min -2.868 _refine_diff_density_rms 0.114