# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ; Syntheses and Structures of Lanthanide Borohydride Supported by a Bridged Bis(amidinate) and Their High Activity for Control Polymerization of -Caprolactone, L-Lactide and rac-Lactide ; _publ_section_title_footnote ; ? ; loop_ _publ_author_address ; Department of Chemistry and Chemical Engineering Dushu Lake Campus Suzhou University Suzhou, 215123 P. R. China ; ; Department of Chemistry and Chemical Engineering Dushu Lake Campus Suzhou University Suzhou, 215123 P. R. China ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_contact_author_email wenbo860407@163.com _publ_contact_author_name 'Wenbo Li' _publ_author_name 'Qi Shen' #============================================================================== data_shelxl _database_code_depnum_ccdc_archive 'CCDC 843489' #TrackingRef 'shelxl (1).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H48 B N4 O2 Si2 Y, C4 H10 O2' _chemical_formula_sum 'C31 H58 B N4 O4 Si2 Y' _chemical_formula_weight 706.71 _chemical_absolute_configuration ad 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' Si Si 0.0817 0.0704 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 8.683(2) _cell_length_b 19.888(6) _cell_length_c 23.197(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4005.9(18) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7754 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 1.550 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.330 _exptl_absorpt_correction_T_max 0.581 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8666 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.1533 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6724 _reflns_number_gt 3844 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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. ; _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^)+(0.0348P)^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 -0.030(8) _refine_ls_number_reflns 6724 _refine_ls_number_parameters 344 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1130 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 0.843 _refine_ls_restrained_S_all 0.850 _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 Y1 Y 0.54953(7) 0.37647(3) 0.69643(2) 0.03766(16) Uani 1 1 d . A . Si1 Si 0.5846(3) 0.42117(13) 0.86165(8) 0.0726(8) Uani 1 1 d D . . Si2 Si 0.6454(3) 0.44309(12) 0.53935(8) 0.0621(6) Uani 1 1 d . . . O1 O 0.3208(5) 0.4429(2) 0.6946(2) 0.0623(13) Uani 1 1 d D . . O2 O 0.5996(5) 0.5003(2) 0.7005(2) 0.0570(12) Uani 1 1 d . . . O3 O 0.1959(7) 0.6459(4) 0.6433(3) 0.134(3) Uiso 1 1 d . . . O4 O 0.0618(7) 0.6018(3) 0.7495(2) 0.110(2) Uiso 1 1 d . . . N1 N 0.5101(6) 0.3820(3) 0.8021(2) 0.0520(15) Uani 1 1 d . A . N2 N 0.4027(6) 0.3002(3) 0.7489(2) 0.0476(15) Uani 1 1 d . A . N3 N 0.5546(7) 0.3964(3) 0.59153(19) 0.0524(15) Uani 1 1 d . A . N4 N 0.4360(8) 0.3071(3) 0.62935(18) 0.0536(16) Uani 1 1 d . A . C1 C 0.4247(7) 0.3269(3) 0.8001(3) 0.0460(16) Uani 1 1 d . . . C2 C 0.4603(9) 0.3454(4) 0.5845(3) 0.0507(18) Uani 1 1 d . . . C3 C 0.3080(7) 0.2413(3) 0.7376(2) 0.0470(18) Uani 1 1 d . . . H3A H 0.1995 0.2548 0.7366 0.056 Uiso 1 1 calc R A . H3B H 0.3208 0.2092 0.7693 0.056 Uiso 1 1 calc R . . C4 C 0.3471(9) 0.2074(3) 0.6823(2) 0.066(2) Uani 1 1 d . A . H4A H 0.2825 0.1672 0.6786 0.079 Uiso 1 1 calc R . . H4B H 0.4544 0.1923 0.6843 0.079 Uiso 1 1 calc R . . C5 C 0.3281(9) 0.2488(4) 0.6291(3) 0.072(3) Uani 1 1 d . . . H5A H 0.3480 0.2209 0.5951 0.086 Uiso 1 1 calc R A . H5B H 0.2219 0.2652 0.6268 0.086 Uiso 1 1 calc R . . C6 C 0.3533(12) 0.2964(5) 0.8517(3) 0.0946(14) Uani 1 1 d D A . C7 C 0.2171(11) 0.3222(5) 0.8736(3) 0.0946(14) Uani 1 1 d . . . H7 H 0.1698 0.3581 0.8540 0.113 Uiso 1 1 calc R A . C8 C 0.1471(11) 0.2973(5) 0.9233(3) 0.0946(14) Uani 1 1 d D A . H8 H 0.0566 0.3165 0.9382 0.113 Uiso 1 1 calc R . . C9 C 0.2160(11) 0.2440(5) 0.9490(3) 0.0946(14) Uani 1 1 d D . . H9 H 0.1696 0.2261 0.9823 0.113 Uiso 1 1 calc R A . C10 C 0.3444(11) 0.2155(5) 0.9304(3) 0.0946(14) Uani 1 1 d D A . H10 H 0.3878 0.1786 0.9497 0.113 Uiso 1 1 calc R . . C11 C 0.4156(11) 0.2430(5) 0.8792(3) 0.0946(14) Uani 1 1 d D . . H11 H 0.5064 0.2234 0.8649 0.113 Uiso 1 1 calc R A . C12 C 0.3798(8) 0.3308(4) 0.5270(3) 0.052(2) Uani 1 1 d . A . C13 C 0.4243(9) 0.2756(4) 0.4929(3) 0.062(2) Uani 1 1 d . . . H13 H 0.4998 0.2456 0.5062 0.074 Uiso 1 1 calc R A . C14 C 0.3567(11) 0.2659(5) 0.4397(3) 0.082(3) Uani 1 1 d . A . H14 H 0.3906 0.2305 0.4161 0.098 Uiso 1 1 calc R . . C15 C 0.2420(11) 0.3067(6) 0.4211(4) 0.087(3) Uani 1 1 d . . . H15 H 0.1944 0.2984 0.3855 0.104 Uiso 1 1 calc R A . C16 C 0.1959(10) 0.3593(6) 0.4536(4) 0.098(4) Uani 1 1 d . A . H16 H 0.1170 0.3876 0.4401 0.117 Uiso 1 1 calc R . . C17 C 0.2655(8) 0.3723(5) 0.5080(3) 0.073(2) Uani 1 1 d . . . H17 H 0.2332 0.4090 0.5305 0.088 Uiso 1 1 calc R A . C18 C 0.589(2) 0.3726(10) 0.9306(5) 0.118(3) Uani 0.50 1 d PD A 1 H18A H 0.4847 0.3620 0.9423 0.176 Uiso 0.50 1 calc PR A 1 H18B H 0.6385 0.3993 0.9603 0.176 Uiso 0.50 1 calc PR A 1 H18C H 0.6465 0.3313 0.9249 0.176 Uiso 0.50 1 calc PR A 1 C18' C 0.462(2) 0.4296(10) 0.9282(5) 0.118(3) Uani 0.50 1 d PD A 2 H18D H 0.4423 0.4768 0.9358 0.176 Uiso 0.50 1 calc PR A 2 H18E H 0.5148 0.4098 0.9608 0.176 Uiso 0.50 1 calc PR A 2 H18F H 0.3645 0.4065 0.9223 0.176 Uiso 0.50 1 calc PR A 2 C19 C 0.8012(16) 0.4355(11) 0.8480(7) 0.118(3) Uani 0.50 1 d PD A 1 H19A H 0.8493 0.3933 0.8374 0.176 Uiso 0.50 1 calc PR A 1 H19B H 0.8490 0.4528 0.8828 0.176 Uiso 0.50 1 calc PR A 1 H19C H 0.8142 0.4677 0.8170 0.176 Uiso 0.50 1 calc PR A 1 C19' C 0.7540(19) 0.3729(10) 0.8877(7) 0.118(3) Uani 0.50 1 d PD A 2 H19D H 0.7667 0.3328 0.8644 0.176 Uiso 0.50 1 calc PR A 2 H19E H 0.7381 0.3601 0.9276 0.176 Uiso 0.50 1 calc PR A 2 H19F H 0.8456 0.4006 0.8847 0.176 Uiso 0.50 1 calc PR A 2 C20 C 0.488(2) 0.5025(8) 0.8711(7) 0.118(3) Uani 0.50 1 d PD A 1 H20A H 0.5239 0.5338 0.8420 0.176 Uiso 0.50 1 calc PR A 1 H20B H 0.5105 0.5201 0.9091 0.176 Uiso 0.50 1 calc PR A 1 H20C H 0.3773 0.4965 0.8671 0.176 Uiso 0.50 1 calc PR A 1 C20' C 0.614(3) 0.5116(8) 0.8436(6) 0.118(3) Uani 0.50 1 d PD A 2 H20D H 0.7038 0.5163 0.8192 0.176 Uiso 0.50 1 calc PR A 2 H20E H 0.6286 0.5371 0.8788 0.176 Uiso 0.50 1 calc PR A 2 H20F H 0.5239 0.5285 0.8234 0.176 Uiso 0.50 1 calc PR A 2 C21 C 0.6749(10) 0.3995(4) 0.4686(3) 0.114(4) Uani 1 1 d . . . H21A H 0.7024 0.3529 0.4755 0.172 Uiso 1 1 calc R . . H21B H 0.7570 0.4215 0.4475 0.172 Uiso 1 1 calc R . . H21C H 0.5805 0.4014 0.4463 0.172 Uiso 1 1 calc R . . C22 C 0.5494(12) 0.5237(5) 0.5261(4) 0.146(5) Uani 1 1 d . . . H22A H 0.4406 0.5160 0.5194 0.219 Uiso 1 1 calc R . . H22B H 0.5946 0.5450 0.4925 0.219 Uiso 1 1 calc R . . H22C H 0.5623 0.5526 0.5594 0.219 Uiso 1 1 calc R . . C23 C 0.8404(10) 0.4615(6) 0.5636(3) 0.146(5) Uani 1 1 d . . . H23A H 0.8601 0.4380 0.5995 0.219 Uiso 1 1 calc R . . H23B H 0.8514 0.5095 0.5695 0.219 Uiso 1 1 calc R . . H23C H 0.9134 0.4466 0.5346 0.219 Uiso 1 1 calc R . . C24 C 0.3335(9) 0.5078(4) 0.6795(4) 0.094(2) Uani 1 1 d D . . H24A H 0.2430 0.5314 0.6945 0.113 Uiso 1 1 calc R . . H24B H 0.3283 0.5102 0.6374 0.113 Uiso 1 1 calc R . . C25 C 0.4689(9) 0.5447(4) 0.6977(4) 0.094(2) Uani 1 1 d . . . H25A H 0.4897 0.5811 0.6704 0.113 Uiso 1 1 calc R . . H25B H 0.4505 0.5646 0.7358 0.113 Uiso 1 1 calc R . . C26 C 0.1694(7) 0.4163(4) 0.6926(4) 0.100(3) Uani 1 1 d . . . H26A H 0.1027 0.4472 0.6720 0.150 Uiso 1 1 calc R . . H26B H 0.1312 0.4103 0.7316 0.150 Uiso 1 1 calc R . . H26C H 0.1707 0.3733 0.6729 0.150 Uiso 1 1 calc R . . C27 C 0.7404(7) 0.5369(4) 0.7064(4) 0.084(3) Uani 1 1 d . . . H27A H 0.7571 0.5641 0.6723 0.126 Uiso 1 1 calc R . . H27B H 0.8251 0.5055 0.7109 0.126 Uiso 1 1 calc R . . H27C H 0.7345 0.5658 0.7400 0.126 Uiso 1 1 calc R . . C28 C 0.0911(10) 0.6806(5) 0.6780(3) 0.115(4) Uiso 1 1 d D . . H28A H -0.0142 0.6682 0.6671 0.139 Uiso 1 1 calc R . . H28B H 0.1031 0.7291 0.6720 0.139 Uiso 1 1 calc R . . C29 C 0.1163(11) 0.6648(5) 0.7374(4) 0.115(4) Uiso 1 1 d D . . H29A H 0.2267 0.6668 0.7460 0.138 Uiso 1 1 calc R . . H29B H 0.0637 0.6979 0.7617 0.138 Uiso 1 1 calc R . . C30 C 0.1650(14) 0.6497(7) 0.5836(4) 0.181(5) Uiso 1 1 d . . . H30A H 0.0731 0.6240 0.5748 0.271 Uiso 1 1 calc R . . H30B H 0.2515 0.6316 0.5622 0.271 Uiso 1 1 calc R . . H30C H 0.1491 0.6963 0.5727 0.271 Uiso 1 1 calc R . . C31 C 0.0820(12) 0.5840(5) 0.8078(4) 0.147(4) Uiso 1 1 d . . . H31A H 0.1891 0.5901 0.8185 0.220 Uiso 1 1 calc R . . H31B H 0.0531 0.5373 0.8132 0.220 Uiso 1 1 calc R . . H31C H 0.0176 0.6124 0.8318 0.220 Uiso 1 1 calc R . . B1 B 0.8210(8) 0.3354(5) 0.7054(4) 0.078(3) Uani 1 1 d D . . H1A H 0.731(5) 0.2996(19) 0.7206(17) 0.094 Uiso 1 1 d D . . H1B H 0.846(6) 0.3747(18) 0.7380(14) 0.094 Uiso 1 1 d D . . H1C H 0.791(5) 0.358(2) 0.6627(11) 0.094 Uiso 1 1 d D . . H1D H 0.935(4) 0.310(3) 0.705(2) 0.094 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0382(3) 0.0353(3) 0.0395(3) -0.0035(3) 0.0008(3) -0.0049(4) Si1 0.107(2) 0.0633(17) 0.0479(12) -0.0085(11) -0.0112(13) -0.0214(16) Si2 0.0820(16) 0.0542(15) 0.0499(12) 0.0061(11) 0.0141(12) -0.0180(13) O1 0.044(3) 0.046(3) 0.097(3) 0.020(3) 0.000(3) 0.005(2) O2 0.051(3) 0.041(3) 0.079(3) -0.005(3) 0.001(3) -0.008(2) N1 0.085(4) 0.044(3) 0.028(2) -0.008(3) -0.008(3) -0.014(3) N2 0.056(4) 0.050(4) 0.036(3) -0.006(3) 0.001(3) -0.018(3) N3 0.068(4) 0.049(4) 0.040(3) 0.002(3) 0.002(3) -0.021(4) N4 0.082(4) 0.052(4) 0.028(3) 0.005(3) -0.012(3) -0.035(4) C1 0.042(4) 0.059(4) 0.038(3) 0.009(4) 0.010(4) 0.010(3) C2 0.061(5) 0.048(4) 0.043(4) -0.001(3) -0.002(4) -0.004(5) C3 0.052(4) 0.044(4) 0.045(4) -0.008(3) -0.002(3) -0.020(4) C4 0.106(6) 0.031(4) 0.061(5) -0.011(4) 0.014(5) -0.030(4) C5 0.112(7) 0.054(5) 0.048(4) 0.007(4) -0.010(4) -0.045(5) C6 0.128(4) 0.096(4) 0.059(2) 0.002(2) 0.004(2) -0.022(3) C7 0.128(4) 0.096(4) 0.059(2) 0.002(2) 0.004(2) -0.022(3) C8 0.128(4) 0.096(4) 0.059(2) 0.002(2) 0.004(2) -0.022(3) C9 0.128(4) 0.096(4) 0.059(2) 0.002(2) 0.004(2) -0.022(3) C10 0.128(4) 0.096(4) 0.059(2) 0.002(2) 0.004(2) -0.022(3) C11 0.128(4) 0.096(4) 0.059(2) 0.002(2) 0.004(2) -0.022(3) C12 0.060(5) 0.058(5) 0.037(4) -0.006(4) 0.005(3) -0.005(4) C13 0.077(6) 0.062(5) 0.047(4) -0.011(4) -0.004(4) 0.000(5) C14 0.105(7) 0.097(8) 0.043(5) -0.002(5) 0.002(5) -0.039(7) C15 0.083(7) 0.110(10) 0.068(6) 0.006(6) -0.018(6) -0.025(7) C16 0.071(6) 0.121(11) 0.101(7) 0.042(7) -0.022(6) -0.002(7) C17 0.064(5) 0.084(7) 0.072(5) 0.014(5) -0.006(4) 0.010(6) C18 0.170(10) 0.112(8) 0.071(5) -0.042(5) -0.027(6) -0.049(7) C18' 0.170(10) 0.112(8) 0.071(5) -0.042(5) -0.027(6) -0.049(7) C19 0.170(10) 0.112(8) 0.071(5) -0.042(5) -0.027(6) -0.049(7) C19' 0.170(10) 0.112(8) 0.071(5) -0.042(5) -0.027(6) -0.049(7) C20 0.170(10) 0.112(8) 0.071(5) -0.042(5) -0.027(6) -0.049(7) C20' 0.170(10) 0.112(8) 0.071(5) -0.042(5) -0.027(6) -0.049(7) C21 0.177(9) 0.078(8) 0.088(6) 0.005(5) 0.086(6) -0.012(7) C22 0.173(10) 0.087(8) 0.178(9) 0.075(7) 0.088(9) 0.042(9) C23 0.134(9) 0.204(16) 0.100(7) 0.020(8) 0.031(7) -0.089(10) C24 0.063(4) 0.054(4) 0.164(6) 0.002(5) -0.001(5) 0.015(4) C25 0.063(4) 0.054(4) 0.164(6) 0.002(5) -0.001(5) 0.015(4) C26 0.034(4) 0.076(7) 0.191(9) 0.003(7) 0.011(6) -0.007(4) C27 0.057(5) 0.060(6) 0.135(7) -0.031(6) 0.016(5) -0.034(4) B1 0.030(5) 0.063(7) 0.142(9) 0.031(7) -0.015(6) 0.002(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 Y1 N4 2.302(5) . ? Y1 N2 2.325(5) . ? Y1 O1 2.386(4) . ? Y1 N3 2.466(5) . ? Y1 N1 2.477(5) . ? Y1 B1 2.503(8) . ? Y1 O2 2.503(4) . ? Y1 C2 2.780(6) . ? Y1 C1 2.816(6) . ? Y1 H1A 2.27(5) . ? Y1 H1C 2.27(4) . ? Si1 N1 1.713(5) . ? Si1 C20 1.836(15) . ? Si1 C19' 1.858(15) . ? Si1 C20' 1.865(14) . ? Si1 C18 1.868(13) . ? Si1 C18' 1.885(13) . ? Si1 C19 1.929(14) . ? Si2 N3 1.717(5) . ? Si2 C23 1.821(9) . ? Si2 C22 1.832(9) . ? Si2 C21 1.873(7) . ? O1 C24 1.341(8) . ? O1 C26 1.418(7) . ? O2 C27 1.428(6) . ? O2 C25 1.439(7) . ? O3 C28 1.396(9) . ? O3 C30 1.412(10) . ? O4 C29 1.367(10) . ? O4 C31 1.410(9) . ? N1 C1 1.324(8) . ? N2 C1 1.315(7) . ? N2 C3 1.455(7) . ? N3 C2 1.314(8) . ? N4 C2 1.307(7) . ? N4 C5 1.490(8) . ? C1 C6 1.477(10) . ? C2 C12 1.532(8) . ? C3 C4 1.489(7) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.493(8) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C11 1.353(10) . ? C6 C7 1.386(11) . ? C7 C8 1.394(10) . ? C7 H7 0.9400 . ? C8 C9 1.357(10) . ? C8 H8 0.9400 . ? C9 C10 1.322(10) . ? C9 H9 0.9400 . ? C10 C11 1.445(9) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C17 1.364(9) . ? C12 C13 1.408(9) . ? C13 C14 1.379(8) . ? C13 H13 0.9400 . ? C14 C15 1.355(12) . ? C14 H14 0.9400 . ? C15 C16 1.349(12) . ? C15 H15 0.9400 . ? C16 C17 1.423(10) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C18' H18D 0.9700 . ? C18' H18E 0.9700 . ? C18' H18F 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C19' H19D 0.9700 . ? C19' H19E 0.9700 . ? C19' H19F 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C20' H20D 0.9700 . ? C20' H20E 0.9700 . ? C20' H20F 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C25 1.448(9) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 C29 1.431(8) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? B1 H1A 1.112(10) . ? B1 H1B 1.109(10) . ? B1 H1C 1.114(9) . ? B1 H1D 1.106(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Y1 N2 74.20(18) . . ? N4 Y1 O1 87.9(2) . . ? N2 Y1 O1 85.09(18) . . ? N4 Y1 N3 55.73(17) . . ? N2 Y1 N3 129.13(18) . . ? O1 Y1 N3 84.70(19) . . ? N4 Y1 N1 129.52(18) . . ? N2 Y1 N1 55.63(17) . . ? O1 Y1 N1 83.02(18) . . ? N3 Y1 N1 166.33(18) . . ? N4 Y1 B1 105.3(3) . . ? N2 Y1 B1 105.1(3) . . ? O1 Y1 B1 165.0(3) . . ? N3 Y1 B1 96.8(3) . . ? N1 Y1 B1 93.6(3) . . ? N4 Y1 O2 133.62(17) . . ? N2 Y1 O2 135.84(17) . . ? O1 Y1 O2 66.43(15) . . ? N3 Y1 O2 82.86(17) . . ? N1 Y1 O2 86.74(17) . . ? B1 Y1 O2 98.9(2) . . ? N4 Y1 C2 27.83(18) . . ? N2 Y1 C2 101.0(2) . . ? O1 Y1 C2 82.8(2) . . ? N3 Y1 C2 28.21(18) . . ? N1 Y1 C2 153.6(2) . . ? B1 Y1 C2 105.5(3) . . ? O2 Y1 C2 107.60(19) . . ? N4 Y1 C1 101.7(2) . . ? N2 Y1 C1 27.60(17) . . ? O1 Y1 C1 83.62(17) . . ? N3 Y1 C1 154.9(2) . . ? N1 Y1 C1 28.04(17) . . ? B1 Y1 C1 100.2(2) . . ? O2 Y1 C1 112.28(18) . . ? C2 Y1 C1 127.8(2) . . ? N4 Y1 H1A 93.5(10) . . ? N2 Y1 H1A 79.2(4) . . ? O1 Y1 H1A 163.2(7) . . ? N3 Y1 H1A 109.9(10) . . ? N1 Y1 H1A 83.2(10) . . ? B1 Y1 H1A 26.4(3) . . ? O2 Y1 H1A 122.2(6) . . ? C2 Y1 H1A 106.0(11) . . ? C1 Y1 H1A 79.7(8) . . ? N4 Y1 H1C 93.6(11) . . ? N2 Y1 H1C 125.3(8) . . ? O1 Y1 H1C 148.7(6) . . ? N3 Y1 H1C 70.8(4) . . ? N1 Y1 H1C 118.4(5) . . ? B1 Y1 H1C 26.4(2) . . ? O2 Y1 H1C 90.9(11) . . ? C2 Y1 H1C 84.2(8) . . ? C1 Y1 H1C 126.3(4) . . ? H1A Y1 H1C 47.9(6) . . ? N1 Si1 C20 108.9(5) . . ? N1 Si1 C19' 109.0(6) . . ? C20 Si1 C19' 141.2(8) . . ? N1 Si1 C20' 108.0(5) . . ? C20 Si1 C20' 40.5(7) . . ? C19' Si1 C20' 117.7(9) . . ? N1 Si1 C18 117.6(6) . . ? C20 Si1 C18 111.3(8) . . ? C19' Si1 C18 55.8(8) . . ? C20' Si1 C18 133.5(7) . . ? N1 Si1 C18' 119.2(5) . . ? C20 Si1 C18' 64.2(8) . . ? C19' Si1 C18' 103.2(8) . . ? C20' Si1 C18' 100.1(8) . . ? C18 Si1 C18' 50.0(8) . . ? N1 Si1 C19 107.6(5) . . ? C20 Si1 C19 109.7(9) . . ? C19' Si1 C19 50.0(7) . . ? C20' Si1 C19 71.8(9) . . ? C18 Si1 C19 101.3(9) . . ? C18' Si1 C19 132.4(7) . . ? N3 Si2 C23 108.5(4) . . ? N3 Si2 C22 112.5(4) . . ? C23 Si2 C22 107.4(5) . . ? N3 Si2 C21 115.5(3) . . ? C23 Si2 C21 103.7(4) . . ? C22 Si2 C21 108.7(4) . . ? C24 O1 C26 115.3(6) . . ? C24 O1 Y1 118.0(5) . . ? C26 O1 Y1 124.5(4) . . ? C27 O2 C25 111.6(6) . . ? C27 O2 Y1 130.7(4) . . ? C25 O2 Y1 117.7(4) . . ? C28 O3 C30 114.5(8) . . ? C29 O4 C31 112.5(8) . . ? C1 N1 Si1 128.0(5) . . ? C1 N1 Y1 90.4(4) . . ? Si1 N1 Y1 140.0(3) . . ? C1 N2 C3 124.8(5) . . ? C1 N2 Y1 97.4(4) . . ? C3 N2 Y1 137.8(4) . . ? C2 N3 Si2 128.0(5) . . ? C2 N3 Y1 89.3(4) . . ? Si2 N3 Y1 142.3(3) . . ? C2 N4 C5 123.5(6) . . ? C2 N4 Y1 96.9(4) . . ? C5 N4 Y1 137.6(4) . . ? N2 C1 N1 116.6(6) . . ? N2 C1 C6 120.3(6) . . ? N1 C1 C6 123.1(7) . . ? N2 C1 Y1 55.0(3) . . ? N1 C1 Y1 61.6(3) . . ? C6 C1 Y1 175.3(6) . . ? N4 C2 N3 116.8(6) . . ? N4 C2 C12 120.6(7) . . ? N3 C2 C12 122.6(6) . . ? N4 C2 Y1 55.3(3) . . ? N3 C2 Y1 62.5(3) . . ? C12 C2 Y1 169.0(5) . . ? N2 C3 C4 113.0(5) . . ? N2 C3 H3A 109.0 . . ? C4 C3 H3A 109.0 . . ? N2 C3 H3B 109.0 . . ? C4 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C3 C4 C5 115.9(6) . . ? C3 C4 H4A 108.3 . . ? C5 C4 H4A 108.3 . . ? C3 C4 H4B 108.3 . . ? C5 C4 H4B 108.3 . . ? H4A C4 H4B 107.4 . . ? N4 C5 C4 110.9(6) . . ? N4 C5 H5A 109.5 . . ? C4 C5 H5A 109.5 . . ? N4 C5 H5B 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 108.0 . . ? C11 C6 C7 117.3(9) . . ? C11 C6 C1 122.5(9) . . ? C7 C6 C1 120.2(9) . . ? C6 C7 C8 122.9(10) . . ? C6 C7 H7 118.5 . . ? C8 C7 H7 118.5 . . ? C9 C8 C7 116.7(9) . . ? C9 C8 H8 121.6 . . ? C7 C8 H8 121.6 . . ? C10 C9 C8 124.2(10) . . ? C10 C9 H9 117.9 . . ? C8 C9 H9 117.9 . . ? C9 C10 C11 117.9(9) . . ? C9 C10 H10 121.0 . . ? C11 C10 H10 121.0 . . ? C6 C11 C10 120.9(10) . . ? C6 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C17 C12 C13 119.3(7) . . ? C17 C12 C2 120.0(7) . . ? C13 C12 C2 120.8(7) . . ? C14 C13 C12 119.7(8) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C15 C14 C13 120.8(9) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C16 C15 C14 120.3(10) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 120.7(10) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C12 C17 C16 119.1(9) . . ? C12 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C18' H18D 109.5 . . ? Si1 C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? Si1 C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? Si1 C19' H19D 109.5 . . ? Si1 C19' H19E 109.5 . . ? H19D C19' H19E 109.5 . . ? Si1 C19' H19F 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? Si1 C20' H20D 109.5 . . ? Si1 C20' H20E 109.5 . . ? H20D C20' H20E 109.5 . . ? Si1 C20' H20F 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O1 C24 C25 118.6(7) . . ? O1 C24 H24A 107.7 . . ? C25 C24 H24A 107.7 . . ? O1 C24 H24B 107.7 . . ? C25 C24 H24B 107.7 . . ? H24A C24 H24B 107.1 . . ? O2 C25 C24 110.0(6) . . ? O2 C25 H25A 109.7 . . ? C24 C25 H25A 109.7 . . ? O2 C25 H25B 109.7 . . ? C24 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? O1 C26 H26A 109.5 . . ? O1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O2 C27 H27A 109.5 . . ? O2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O3 C28 C29 110.3(9) . . ? O3 C28 H28A 109.6 . . ? C29 C28 H28A 109.6 . . ? O3 C28 H28B 109.6 . . ? C29 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? O4 C29 C28 110.2(9) . . ? O4 C29 H29A 109.6 . . ? C28 C29 H29A 109.6 . . ? O4 C29 H29B 109.6 . . ? C28 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? O3 C30 H30A 109.5 . . ? O3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O4 C31 H31A 109.5 . . ? O4 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O4 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Y1 B1 H1A 65(3) . . ? Y1 B1 H1B 91(3) . . ? H1A B1 H1B 112.0(14) . . ? Y1 B1 H1C 65(2) . . ? H1A B1 H1C 111.8(13) . . ? H1B B1 H1C 111.9(13) . . ? Y1 B1 H1D 170(3) . . ? H1A B1 H1D 110(4) . . ? H1B B1 H1D 99(4) . . ? H1C B1 H1D 111.8(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Y1 O1 C24 -120.9(6) . . . . ? N2 Y1 O1 C24 164.8(6) . . . . ? N3 Y1 O1 C24 -65.1(6) . . . . ? N1 Y1 O1 C24 108.9(6) . . . . ? B1 Y1 O1 C24 31.3(13) . . . . ? O2 Y1 O1 C24 19.4(6) . . . . ? C2 Y1 O1 C24 -93.4(6) . . . . ? C1 Y1 O1 C24 137.1(7) . . . . ? N4 Y1 O1 C26 41.0(6) . . . . ? N2 Y1 O1 C26 -33.3(6) . . . . ? N3 Y1 O1 C26 96.8(6) . . . . ? N1 Y1 O1 C26 -89.2(6) . . . . ? B1 Y1 O1 C26 -166.8(9) . . . . ? O2 Y1 O1 C26 -178.7(7) . . . . ? C2 Y1 O1 C26 68.5(6) . . . . ? C1 Y1 O1 C26 -61.0(6) . . . . ? N4 Y1 O2 C27 -121.4(6) . . . . ? N2 Y1 O2 C27 122.4(6) . . . . ? O1 Y1 O2 C27 176.7(6) . . . . ? N3 Y1 O2 C27 -96.0(6) . . . . ? N1 Y1 O2 C27 92.9(6) . . . . ? B1 Y1 O2 C27 -0.2(7) . . . . ? C2 Y1 O2 C27 -109.7(6) . . . . ? C1 Y1 O2 C27 104.7(6) . . . . ? N4 Y1 O2 C25 60.0(6) . . . . ? N2 Y1 O2 C25 -56.2(6) . . . . ? O1 Y1 O2 C25 -1.9(5) . . . . ? N3 Y1 O2 C25 85.4(6) . . . . ? N1 Y1 O2 C25 -85.7(6) . . . . ? B1 Y1 O2 C25 -178.9(6) . . . . ? C2 Y1 O2 C25 71.7(6) . . . . ? C1 Y1 O2 C25 -73.9(6) . . . . ? C20 Si1 N1 C1 -111.8(9) . . . . ? C19' Si1 N1 C1 76.5(9) . . . . ? C20' Si1 N1 C1 -154.5(9) . . . . ? C18 Si1 N1 C1 15.9(10) . . . . ? C18' Si1 N1 C1 -41.4(10) . . . . ? C19 Si1 N1 C1 129.4(9) . . . . ? C20 Si1 N1 Y1 87.4(9) . . . . ? C19' Si1 N1 Y1 -84.3(8) . . . . ? C20' Si1 N1 Y1 44.6(9) . . . . ? C18 Si1 N1 Y1 -144.9(9) . . . . ? C18' Si1 N1 Y1 157.7(8) . . . . ? C19 Si1 N1 Y1 -31.4(9) . . . . ? N4 Y1 N1 C1 8.1(5) . . . . ? N2 Y1 N1 C1 0.7(4) . . . . ? O1 Y1 N1 C1 89.5(4) . . . . ? N3 Y1 N1 C1 115.8(8) . . . . ? B1 Y1 N1 C1 -105.1(4) . . . . ? O2 Y1 N1 C1 156.2(4) . . . . ? C2 Y1 N1 C1 31.7(7) . . . . ? N4 Y1 N1 Si1 173.1(4) . . . . ? N2 Y1 N1 Si1 165.7(6) . . . . ? O1 Y1 N1 Si1 -105.4(5) . . . . ? N3 Y1 N1 Si1 -79.2(9) . . . . ? B1 Y1 N1 Si1 59.9(5) . . . . ? O2 Y1 N1 Si1 -38.8(5) . . . . ? C2 Y1 N1 Si1 -163.3(4) . . . . ? C1 Y1 N1 Si1 165.0(8) . . . . ? N4 Y1 N2 C1 -174.8(5) . . . . ? O1 Y1 N2 C1 -85.6(4) . . . . ? N3 Y1 N2 C1 -164.7(4) . . . . ? N1 Y1 N2 C1 -0.7(4) . . . . ? B1 Y1 N2 C1 83.2(5) . . . . ? O2 Y1 N2 C1 -37.3(5) . . . . ? C2 Y1 N2 C1 -167.3(4) . . . . ? N4 Y1 N2 C3 3.9(6) . . . . ? O1 Y1 N2 C3 93.1(7) . . . . ? N3 Y1 N2 C3 14.0(8) . . . . ? N1 Y1 N2 C3 178.0(7) . . . . ? B1 Y1 N2 C3 -98.1(7) . . . . ? O2 Y1 N2 C3 141.4(6) . . . . ? C2 Y1 N2 C3 11.4(7) . . . . ? C1 Y1 N2 C3 178.7(9) . . . . ? C23 Si2 N3 C2 -140.5(7) . . . . ? C22 Si2 N3 C2 100.8(8) . . . . ? C21 Si2 N3 C2 -24.7(8) . . . . ? C23 Si2 N3 Y1 29.0(7) . . . . ? C22 Si2 N3 Y1 -89.6(7) . . . . ? C21 Si2 N3 Y1 144.9(5) . . . . ? N4 Y1 N3 C2 6.5(4) . . . . ? N2 Y1 N3 C2 -5.3(6) . . . . ? O1 Y1 N3 C2 -84.6(5) . . . . ? N1 Y1 N3 C2 -110.7(8) . . . . ? B1 Y1 N3 C2 110.4(5) . . . . ? O2 Y1 N3 C2 -151.4(5) . . . . ? C1 Y1 N3 C2 -22.1(7) . . . . ? N4 Y1 N3 Si2 -165.3(6) . . . . ? N2 Y1 N3 Si2 -177.1(4) . . . . ? O1 Y1 N3 Si2 103.6(5) . . . . ? N1 Y1 N3 Si2 77.5(10) . . . . ? B1 Y1 N3 Si2 -61.4(6) . . . . ? O2 Y1 N3 Si2 36.8(5) . . . . ? C2 Y1 N3 Si2 -171.8(9) . . . . ? C1 Y1 N3 Si2 166.1(4) . . . . ? N2 Y1 N4 C2 163.9(6) . . . . ? O1 Y1 N4 C2 78.4(5) . . . . ? N3 Y1 N4 C2 -6.6(4) . . . . ? N1 Y1 N4 C2 157.6(4) . . . . ? B1 Y1 N4 C2 -94.4(5) . . . . ? O2 Y1 N4 C2 24.4(6) . . . . ? C1 Y1 N4 C2 161.5(5) . . . . ? N2 Y1 N4 C5 1.1(8) . . . . ? O1 Y1 N4 C5 -84.4(8) . . . . ? N3 Y1 N4 C5 -169.4(9) . . . . ? N1 Y1 N4 C5 -5.2(9) . . . . ? B1 Y1 N4 C5 102.8(8) . . . . ? O2 Y1 N4 C5 -138.4(7) . . . . ? C2 Y1 N4 C5 -162.9(12) . . . . ? C1 Y1 N4 C5 -1.4(8) . . . . ? C3 N2 C1 N1 -177.7(6) . . . . ? Y1 N2 C1 N1 1.3(7) . . . . ? C3 N2 C1 C6 1.1(11) . . . . ? Y1 N2 C1 C6 -179.9(6) . . . . ? C3 N2 C1 Y1 -179.0(8) . . . . ? Si1 N1 C1 N2 -169.0(5) . . . . ? Y1 N1 C1 N2 -1.2(6) . . . . ? Si1 N1 C1 C6 12.2(11) . . . . ? Y1 N1 C1 C6 -180.0(7) . . . . ? Si1 N1 C1 Y1 -167.8(6) . . . . ? N4 Y1 C1 N2 5.1(5) . . . . ? O1 Y1 C1 N2 91.6(4) . . . . ? N3 Y1 C1 N2 28.9(7) . . . . ? N1 Y1 C1 N2 178.7(7) . . . . ? B1 Y1 C1 N2 -103.0(5) . . . . ? O2 Y1 C1 N2 152.9(4) . . . . ? C2 Y1 C1 N2 15.9(5) . . . . ? N4 Y1 C1 N1 -173.6(4) . . . . ? N2 Y1 C1 N1 -178.7(7) . . . . ? O1 Y1 C1 N1 -87.1(4) . . . . ? N3 Y1 C1 N1 -149.8(4) . . . . ? B1 Y1 C1 N1 78.3(4) . . . . ? O2 Y1 C1 N1 -25.8(4) . . . . ? C2 Y1 C1 N1 -162.8(4) . . . . ? N4 Y1 C1 C6 6(7) . . . . ? N2 Y1 C1 C6 1(7) . . . . ? O1 Y1 C1 C6 92(7) . . . . ? N3 Y1 C1 C6 30(7) . . . . ? N1 Y1 C1 C6 180(100) . . . . ? B1 Y1 C1 C6 -102(7) . . . . ? O2 Y1 C1 C6 154(7) . . . . ? C2 Y1 C1 C6 17(7) . . . . ? C5 N4 C2 N3 177.7(7) . . . . ? Y1 N4 C2 N3 11.5(8) . . . . ? C5 N4 C2 C12 -1.6(12) . . . . ? Y1 N4 C2 C12 -167.8(6) . . . . ? C5 N4 C2 Y1 166.2(9) . . . . ? Si2 N3 C2 N4 163.0(6) . . . . ? Y1 N3 C2 N4 -10.6(7) . . . . ? Si2 N3 C2 C12 -17.7(11) . . . . ? Y1 N3 C2 C12 168.7(6) . . . . ? Si2 N3 C2 Y1 173.6(7) . . . . ? N2 Y1 C2 N4 -15.7(5) . . . . ? O1 Y1 C2 N4 -99.3(5) . . . . ? N3 Y1 C2 N4 168.5(8) . . . . ? N1 Y1 C2 N4 -41.4(8) . . . . ? B1 Y1 C2 N4 93.5(5) . . . . ? O2 Y1 C2 N4 -161.7(5) . . . . ? C1 Y1 C2 N4 -23.2(6) . . . . ? N4 Y1 C2 N3 -168.5(8) . . . . ? N2 Y1 C2 N3 175.8(4) . . . . ? O1 Y1 C2 N3 92.3(4) . . . . ? N1 Y1 C2 N3 150.2(4) . . . . ? B1 Y1 C2 N3 -75.0(5) . . . . ? O2 Y1 C2 N3 29.8(5) . . . . ? C1 Y1 C2 N3 168.4(4) . . . . ? N4 Y1 C2 C12 71(3) . . . . ? N2 Y1 C2 C12 56(3) . . . . ? O1 Y1 C2 C12 -28(3) . . . . ? N3 Y1 C2 C12 -120(3) . . . . ? N1 Y1 C2 C12 30(3) . . . . ? B1 Y1 C2 C12 165(3) . . . . ? O2 Y1 C2 C12 -90(3) . . . . ? C1 Y1 C2 C12 48(3) . . . . ? C1 N2 C3 C4 -158.8(6) . . . . ? Y1 N2 C3 C4 22.7(10) . . . . ? N2 C3 C4 C5 -60.8(9) . . . . ? C2 N4 C5 C4 169.2(7) . . . . ? Y1 N4 C5 C4 -31.4(12) . . . . ? C3 C4 C5 N4 64.0(9) . . . . ? N2 C1 C6 C11 81.8(11) . . . . ? N1 C1 C6 C11 -99.5(11) . . . . ? Y1 C1 C6 C11 81(7) . . . . ? N2 C1 C6 C7 -97.9(10) . . . . ? N1 C1 C6 C7 80.8(11) . . . . ? Y1 C1 C6 C7 -99(7) . . . . ? C11 C6 C7 C8 2.7(14) . . . . ? C1 C6 C7 C8 -177.6(7) . . . . ? C6 C7 C8 C9 -2.3(14) . . . . ? C7 C8 C9 C10 0.9(15) . . . . ? C8 C9 C10 C11 -0.1(14) . . . . ? C7 C6 C11 C10 -1.8(14) . . . . ? C1 C6 C11 C10 178.5(7) . . . . ? C9 C10 C11 C6 0.5(13) . . . . ? N4 C2 C12 C17 108.7(9) . . . . ? N3 C2 C12 C17 -70.5(10) . . . . ? Y1 C2 C12 C17 44(3) . . . . ? N4 C2 C12 C13 -72.6(10) . . . . ? N3 C2 C12 C13 108.2(9) . . . . ? Y1 C2 C12 C13 -137(2) . . . . ? C17 C12 C13 C14 2.7(11) . . . . ? C2 C12 C13 C14 -176.0(7) . . . . ? C12 C13 C14 C15 -3.5(12) . . . . ? C13 C14 C15 C16 2.5(15) . . . . ? C14 C15 C16 C17 -0.7(15) . . . . ? C13 C12 C17 C16 -0.9(11) . . . . ? C2 C12 C17 C16 177.8(7) . . . . ? C15 C16 C17 C12 -0.1(14) . . . . ? C26 O1 C24 C25 160.0(8) . . . . ? Y1 O1 C24 C25 -36.4(11) . . . . ? C27 O2 C25 C24 167.8(7) . . . . ? Y1 O2 C25 C24 -13.4(10) . . . . ? O1 C24 C25 O2 32.0(12) . . . . ? C30 O3 C28 C29 170.4(9) . . . . ? C31 O4 C29 C28 -179.2(7) . . . . ? O3 C28 C29 O4 -75.0(10) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.699 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.068 # Attachment 'shelxl (2).cif' data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 843490' #TrackingRef 'shelxl (2).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H48 B N4 Nd O2 Si2, C4 H10 O2' _chemical_formula_sum 'C31 H58 B N4 Nd O4 Si2' _chemical_formula_weight 762.04 _chemical_absolute_configuration ad 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' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 8.7384(7) _cell_length_b 20.0777(19) _cell_length_c 23.162(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4063.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 14872 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1588 _exptl_absorpt_coefficient_mu 1.371 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.589 _exptl_absorpt_correction_T_max 0.872 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20514 _diffrn_reflns_av_R_equivalents 0.0828 _diffrn_reflns_av_sigmaI/netI 0.1282 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.47 _reflns_number_total 9028 _reflns_number_gt 6042 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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. ; _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^)+(0.0433P)^2^+5.1760P] 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 0.05(3) _refine_ls_number_reflns 9028 _refine_ls_number_parameters 377 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.1293 _refine_ls_R_factor_gt 0.0861 _refine_ls_wR_factor_ref 0.1632 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Nd1 Nd 0.55740(7) 0.37956(3) 0.69629(2) 0.04600(15) Uani 1 1 d . A . Si1 Si 0.5779(7) 0.41988(19) 0.86483(15) 0.0908(15) Uani 1 1 d D . . Si2 Si 0.6416(5) 0.44275(18) 0.53486(15) 0.0725(10) Uani 1 1 d D . . O1 O 0.3243(8) 0.4518(3) 0.6929(4) 0.072(2) Uani 1 1 d D . . O2 O 0.6043(8) 0.5075(3) 0.6984(4) 0.071(2) Uani 1 1 d D . . O3 O 0.1982(15) 0.6483(6) 0.6422(6) 0.142(5) Uani 1 1 d . . . O4 O 0.0595(15) 0.6043(6) 0.7494(5) 0.124(4) Uani 1 1 d . . . N1 N 0.5051(10) 0.3799(5) 0.8048(4) 0.071(3) Uani 1 1 d . A . N2 N 0.4007(11) 0.3019(5) 0.7491(4) 0.062(3) Uani 1 1 d . . . N3 N 0.5529(12) 0.3956(4) 0.5878(4) 0.064(3) Uani 1 1 d . A . N4 N 0.4383(15) 0.3073(5) 0.6281(3) 0.069(3) Uani 1 1 d . . . C1 C 0.4237(14) 0.3262(6) 0.7999(5) 0.060(3) Uani 1 1 d . A . C2 C 0.4574(16) 0.3441(6) 0.5825(4) 0.063(3) Uani 1 1 d . A . C3 C 0.3043(15) 0.2429(6) 0.7374(5) 0.068(4) Uani 1 1 d . C . H3A H 0.3177 0.2106 0.7687 0.082 Uiso 1 1 calc R . . H3B H 0.1966 0.2564 0.7370 0.082 Uiso 1 1 calc R . . C4 C 0.3417(16) 0.2103(6) 0.6818(4) 0.071(4) Uani 1 1 d . . . H4A H 0.4472 0.1940 0.6839 0.085 Uiso 1 1 calc R C . H4B H 0.2749 0.1715 0.6774 0.085 Uiso 1 1 calc R . . C5 C 0.3270(17) 0.2519(7) 0.6296(5) 0.082(4) Uani 1 1 d . C . H5A H 0.2232 0.2702 0.6279 0.098 Uiso 1 1 calc R . . H5B H 0.3419 0.2238 0.5955 0.098 Uiso 1 1 calc R . . C6 C 0.351(2) 0.2953(9) 0.8513(7) 0.108(2) Uani 1 1 d . . . C7 C 0.220(2) 0.3186(9) 0.8737(6) 0.108(2) Uani 1 1 d . C . H7 H 0.1739 0.3544 0.8544 0.130 Uiso 1 1 calc R . . C8 C 0.146(2) 0.2943(9) 0.9238(6) 0.108(2) Uani 1 1 d . . . H8 H 0.0545 0.3124 0.9387 0.130 Uiso 1 1 calc R C . C9 C 0.221(2) 0.2417(9) 0.9480(7) 0.108(2) Uani 1 1 d . C . H9 H 0.1753 0.2229 0.9809 0.130 Uiso 1 1 calc R . . C10 C 0.342(2) 0.2156(9) 0.9318(6) 0.108(2) Uani 1 1 d . . . H10 H 0.3880 0.1805 0.9523 0.130 Uiso 1 1 calc R C . C11 C 0.411(2) 0.2422(8) 0.8794(6) 0.108(2) Uani 1 1 d . C . H11 H 0.4996 0.2220 0.8645 0.130 Uiso 1 1 calc R . . C12 C 0.3798(14) 0.3298(6) 0.5256(5) 0.060(3) Uani 1 1 d . . . C13 C 0.4256(18) 0.2759(7) 0.4921(5) 0.082(4) Uani 1 1 d . C . H13 H 0.5001 0.2462 0.5061 0.098 Uiso 1 1 calc R . . C14 C 0.361(2) 0.2659(8) 0.4377(6) 0.100(5) Uani 1 1 d . . . H14 H 0.3993 0.2326 0.4132 0.119 Uiso 1 1 calc R C . C15 C 0.242(2) 0.3041(11) 0.4202(7) 0.104(6) Uani 1 1 d . C . H15 H 0.1925 0.2946 0.3851 0.124 Uiso 1 1 calc R . . C16 C 0.1954(19) 0.3555(9) 0.4527(7) 0.107(6) Uani 1 1 d . . . H16 H 0.1162 0.3832 0.4395 0.129 Uiso 1 1 calc R C . C17 C 0.2636(17) 0.3678(8) 0.5058(5) 0.085(4) Uani 1 1 d . C . H17 H 0.2280 0.4034 0.5285 0.102 Uiso 1 1 calc R . . C18 C 0.592(4) 0.3736(17) 0.9317(10) 0.129(5) Uiso 0.50 1 d PD A 1 H18A H 0.4902 0.3668 0.9475 0.193 Uiso 0.50 1 calc PR A 1 H18B H 0.6533 0.3984 0.9591 0.193 Uiso 0.50 1 calc PR A 1 H18C H 0.6394 0.3308 0.9244 0.193 Uiso 0.50 1 calc PR A 1 C18' C 0.446(4) 0.4352(17) 0.9255(11) 0.129(5) Uiso 0.50 1 d PD A 2 H18D H 0.3673 0.4664 0.9135 0.193 Uiso 0.50 1 calc PR A 2 H18E H 0.5025 0.4537 0.9578 0.193 Uiso 0.50 1 calc PR A 2 H18F H 0.3988 0.3936 0.9370 0.193 Uiso 0.50 1 calc PR A 2 C19 C 0.784(2) 0.4436(18) 0.8501(15) 0.129(5) Uiso 0.50 1 d PD A 1 H19A H 0.8488 0.4049 0.8551 0.193 Uiso 0.50 1 calc PR A 1 H19B H 0.8151 0.4782 0.8769 0.193 Uiso 0.50 1 calc PR A 1 H19C H 0.7931 0.4599 0.8108 0.193 Uiso 0.50 1 calc PR A 1 C19' C 0.735(3) 0.3696(17) 0.8936(14) 0.129(5) Uiso 0.50 1 d PD A 2 H19D H 0.7325 0.3256 0.8763 0.193 Uiso 0.50 1 calc PR A 2 H19E H 0.7240 0.3655 0.9352 0.193 Uiso 0.50 1 calc PR A 2 H19F H 0.8318 0.3909 0.8848 0.193 Uiso 0.50 1 calc PR A 2 C20 C 0.479(4) 0.4998(12) 0.8735(15) 0.129(5) Uiso 0.50 1 d PD A 1 H20A H 0.3752 0.4959 0.8591 0.193 Uiso 0.50 1 calc PR A 1 H20B H 0.5329 0.5339 0.8520 0.193 Uiso 0.50 1 calc PR A 1 H20C H 0.4766 0.5117 0.9141 0.193 Uiso 0.50 1 calc PR A 1 C20' C 0.615(4) 0.5075(10) 0.8446(15) 0.129(5) Uiso 0.50 1 d PD A 2 H20D H 0.7193 0.5119 0.8311 0.193 Uiso 0.50 1 calc PR A 2 H20E H 0.5993 0.5359 0.8780 0.193 Uiso 0.50 1 calc PR A 2 H20F H 0.5448 0.5206 0.8141 0.193 Uiso 0.50 1 calc PR A 2 C21 C 0.648(3) 0.4032(17) 0.4617(9) 0.095(4) Uiso 0.50 1 d PD B 1 H21A H 0.6809 0.3573 0.4653 0.142 Uiso 0.50 1 calc PR B 1 H21B H 0.7187 0.4273 0.4373 0.142 Uiso 0.50 1 calc PR B 1 H21C H 0.5464 0.4044 0.4446 0.142 Uiso 0.50 1 calc PR B 1 C21' C 0.712(3) 0.3938(16) 0.4728(10) 0.095(4) Uiso 0.50 1 d PD B 2 H21D H 0.7462 0.3506 0.4861 0.142 Uiso 0.50 1 calc PR B 2 H21E H 0.7959 0.4172 0.4546 0.142 Uiso 0.50 1 calc PR B 2 H21F H 0.6293 0.3880 0.4451 0.142 Uiso 0.50 1 calc PR B 2 C22 C 0.567(4) 0.5280(9) 0.5366(12) 0.095(4) Uiso 0.50 1 d PD B 1 H22A H 0.4643 0.5286 0.5203 0.142 Uiso 0.50 1 calc PR B 1 H22B H 0.6327 0.5569 0.5141 0.142 Uiso 0.50 1 calc PR B 1 H22C H 0.5630 0.5436 0.5762 0.142 Uiso 0.50 1 calc PR B 1 C22' C 0.519(3) 0.5124(12) 0.5087(12) 0.095(4) Uiso 0.50 1 d PD B 2 H22D H 0.4430 0.4952 0.4822 0.142 Uiso 0.50 1 calc PR B 2 H22E H 0.5825 0.5450 0.4890 0.142 Uiso 0.50 1 calc PR B 2 H22F H 0.4689 0.5333 0.5413 0.142 Uiso 0.50 1 calc PR B 2 C23 C 0.847(2) 0.4496(16) 0.5548(13) 0.095(4) Uiso 0.50 1 d PD B 1 H23A H 0.8560 0.4618 0.5952 0.142 Uiso 0.50 1 calc PR B 1 H23B H 0.8957 0.4835 0.5312 0.142 Uiso 0.50 1 calc PR B 1 H23C H 0.8974 0.4072 0.5484 0.142 Uiso 0.50 1 calc PR B 1 C23' C 0.811(3) 0.4860(14) 0.5657(13) 0.095(4) Uiso 0.50 1 d PD B 2 H23D H 0.7840 0.5049 0.6029 0.142 Uiso 0.50 1 calc PR B 2 H23E H 0.8427 0.5213 0.5397 0.142 Uiso 0.50 1 calc PR B 2 H23F H 0.8937 0.4544 0.5705 0.142 Uiso 0.50 1 calc PR B 2 C24 C 0.338(4) 0.5149(10) 0.6654(12) 0.086(6) Uani 0.50 1 d PD C 1 H24A H 0.2436 0.5407 0.6696 0.103 Uiso 0.50 1 calc PR C 1 H24B H 0.3608 0.5095 0.6242 0.103 Uiso 0.50 1 calc PR C 1 C24' C 0.337(4) 0.5155(11) 0.7174(14) 0.086(6) Uani 0.50 1 d PD C 2 H24C H 0.3450 0.5116 0.7594 0.103 Uiso 0.50 1 calc PR C 2 H24D H 0.2441 0.5412 0.7086 0.103 Uiso 0.50 1 calc PR C 2 C25 C 0.468(3) 0.5485(16) 0.696(2) 0.087(4) Uani 0.50 1 d PD C 1 H25A H 0.4923 0.5902 0.6758 0.104 Uiso 0.50 1 calc PR C 1 H25B H 0.4362 0.5597 0.7353 0.104 Uiso 0.50 1 calc PR C 1 C25' C 0.473(3) 0.5515(16) 0.695(2) 0.087(4) Uani 0.50 1 d PD C 2 H25C H 0.4560 0.5645 0.6543 0.104 Uiso 0.50 1 calc PR C 2 H25D H 0.4918 0.5919 0.7172 0.104 Uiso 0.50 1 calc PR C 2 C26 C 0.1767(14) 0.4262(7) 0.6899(9) 0.118(6) Uani 1 1 d . C . H26A H 0.1371 0.4198 0.7286 0.177 Uiso 1 1 calc R . . H26B H 0.1784 0.3838 0.6698 0.177 Uiso 1 1 calc R . . H26C H 0.1114 0.4572 0.6692 0.177 Uiso 1 1 calc R . . C27 C 0.7429(13) 0.5443(6) 0.7040(8) 0.096(5) Uani 1 1 d . C . H27A H 0.7509 0.5760 0.6725 0.143 Uiso 1 1 calc R . . H27B H 0.8293 0.5140 0.7028 0.143 Uiso 1 1 calc R . . H27C H 0.7428 0.5680 0.7405 0.143 Uiso 1 1 calc R . . C28 C 0.092(2) 0.6852(8) 0.6797(9) 0.131(7) Uani 1 1 d . . . H28A H 0.1101 0.7331 0.6755 0.157 Uiso 1 1 calc R . . H28B H -0.0134 0.6757 0.6683 0.157 Uiso 1 1 calc R . . C29 C 0.116(2) 0.6655(8) 0.7394(8) 0.110(6) Uani 1 1 d . . . H29A H 0.2258 0.6660 0.7482 0.132 Uiso 1 1 calc R . . H29B H 0.0656 0.6977 0.7650 0.132 Uiso 1 1 calc R . . C30 C 0.164(3) 0.6530(14) 0.5834(9) 0.211(14) Uani 1 1 d . . . H30A H 0.0595 0.6389 0.5769 0.317 Uiso 1 1 calc R . . H30B H 0.2331 0.6246 0.5617 0.317 Uiso 1 1 calc R . . H30C H 0.1765 0.6988 0.5709 0.317 Uiso 1 1 calc R . . C31 C 0.086(2) 0.5863(11) 0.8102(7) 0.176(10) Uani 1 1 d . . . H31A H 0.1864 0.6023 0.8220 0.264 Uiso 1 1 calc R . . H31B H 0.0825 0.5382 0.8143 0.264 Uiso 1 1 calc R . . H31C H 0.0082 0.6065 0.8342 0.264 Uiso 1 1 calc R . . B1 B 0.8437(13) 0.3395(6) 0.7053(8) 0.077(5) Uani 1 1 d D . . H1A H 0.761(8) 0.301(3) 0.719(3) 0.092 Uiso 1 1 d D . . H1B H 0.833(10) 0.386(2) 0.731(3) 0.092 Uiso 1 1 d D . . H1C H 0.841(8) 0.348(3) 0.6581(10) 0.092 Uiso 1 1 d D . . H1D H 0.951(6) 0.317(5) 0.721(3) 0.092 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0491(3) 0.0419(2) 0.0470(3) -0.0027(3) 0.0004(3) -0.0061(3) Si1 0.151(4) 0.070(2) 0.0512(19) -0.0085(17) -0.016(3) -0.037(3) Si2 0.098(3) 0.064(2) 0.055(2) 0.0021(18) 0.0186(19) -0.017(2) O1 0.053(4) 0.054(4) 0.111(6) 0.010(5) 0.007(5) 0.000(3) O2 0.064(5) 0.046(4) 0.103(6) -0.001(5) 0.010(5) -0.005(3) O3 0.143(11) 0.132(11) 0.151(12) 0.028(9) 0.002(9) 0.060(9) O4 0.127(9) 0.111(9) 0.134(10) -0.027(7) -0.015(9) -0.014(8) N1 0.106(7) 0.062(5) 0.044(4) -0.011(7) -0.002(5) -0.012(6) N2 0.093(8) 0.051(5) 0.043(5) 0.001(4) -0.001(5) -0.027(5) N3 0.081(6) 0.064(6) 0.048(4) -0.003(4) 0.013(5) -0.047(6) N4 0.098(7) 0.077(6) 0.032(4) 0.009(4) -0.012(6) -0.039(7) C1 0.071(8) 0.079(7) 0.032(5) 0.015(6) 0.006(7) 0.009(7) C2 0.062(7) 0.087(8) 0.040(5) 0.000(6) -0.002(6) -0.007(8) C3 0.084(9) 0.071(8) 0.051(7) -0.018(6) 0.013(6) -0.044(7) C4 0.102(10) 0.069(8) 0.042(7) -0.011(6) 0.009(6) -0.038(7) C5 0.101(10) 0.089(10) 0.055(7) 0.001(7) -0.009(7) -0.051(9) C6 0.122(6) 0.130(6) 0.074(4) 0.004(4) -0.002(4) -0.031(5) C7 0.122(6) 0.130(6) 0.074(4) 0.004(4) -0.002(4) -0.031(5) C8 0.122(6) 0.130(6) 0.074(4) 0.004(4) -0.002(4) -0.031(5) C9 0.122(6) 0.130(6) 0.074(4) 0.004(4) -0.002(4) -0.031(5) C10 0.122(6) 0.130(6) 0.074(4) 0.004(4) -0.002(4) -0.031(5) C11 0.122(6) 0.130(6) 0.074(4) 0.004(4) -0.002(4) -0.031(5) C12 0.075(8) 0.059(7) 0.045(6) -0.001(6) -0.001(6) -0.017(6) C13 0.101(10) 0.095(10) 0.049(6) -0.012(7) -0.029(8) -0.010(9) C14 0.137(15) 0.108(13) 0.054(8) -0.012(8) 0.002(9) -0.042(11) C15 0.105(13) 0.142(17) 0.064(10) 0.007(11) -0.011(10) -0.052(13) C16 0.102(12) 0.116(15) 0.104(13) 0.038(11) -0.044(10) -0.009(11) C17 0.112(11) 0.075(10) 0.069(8) -0.011(8) -0.005(8) 0.002(9) C24 0.077(11) 0.073(11) 0.108(16) -0.035(16) -0.006(17) -0.005(9) C24' 0.077(11) 0.073(11) 0.108(16) -0.035(16) -0.006(17) -0.005(9) C25 0.088(10) 0.051(7) 0.123(10) 0.011(9) 0.018(11) 0.016(7) C25' 0.088(10) 0.051(7) 0.123(10) 0.011(9) 0.018(11) 0.016(7) C26 0.052(7) 0.101(11) 0.201(18) -0.013(13) 0.005(12) -0.008(7) C27 0.064(8) 0.072(8) 0.150(14) -0.008(11) -0.007(10) -0.032(7) C28 0.105(13) 0.079(11) 0.21(2) 0.023(13) 0.003(15) 0.038(10) C29 0.116(14) 0.072(11) 0.142(17) -0.022(12) -0.019(12) 0.027(10) C30 0.22(3) 0.30(4) 0.111(16) 0.07(2) -0.019(17) 0.03(2) C31 0.165(19) 0.29(3) 0.074(11) 0.015(15) -0.002(13) -0.037(18) B1 0.036(6) 0.049(7) 0.144(15) 0.011(9) -0.025(9) 0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 N4 2.384(9) . ? Nd1 N2 2.409(8) . ? Nd1 O1 2.502(7) . ? Nd1 N3 2.534(8) . ? Nd1 N1 2.554(9) . ? Nd1 O2 2.601(7) . ? Nd1 B1 2.636(11) . ? Nd1 C2 2.867(11) . ? Nd1 C1 2.877(11) . ? Nd1 H1A 2.44(9) . ? Nd1 H1B 2.54(9) . ? Si1 N1 1.727(10) . ? Si1 C18 1.811(17) . ? Si1 C19' 1.830(18) . ? Si1 C20 1.833(18) . ? Si1 C18' 1.843(18) . ? Si1 C20' 1.848(18) . ? Si1 C19 1.892(18) . ? Si2 N3 1.732(8) . ? Si2 C22 1.834(16) . ? Si2 C21' 1.845(17) . ? Si2 C23' 1.857(17) . ? Si2 C22' 1.861(17) . ? Si2 C23 1.861(17) . ? Si2 C21 1.872(17) . ? O1 C26 1.390(13) . ? O1 C24' 1.404(16) . ? O1 C24 1.423(17) . ? O2 C27 1.425(11) . ? O2 C25 1.450(17) . ? O2 C25' 1.450(17) . ? O3 C30 1.40(2) . ? O3 C28 1.467(19) . ? O4 C29 1.345(18) . ? O4 C31 1.472(18) . ? N1 C1 1.297(13) . ? N2 C1 1.290(13) . ? N2 C3 1.479(12) . ? N3 C2 1.335(14) . ? N4 C2 1.300(13) . ? N4 C5 1.477(14) . ? C1 C6 1.485(19) . ? C2 C12 1.511(15) . ? C3 C4 1.480(14) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.474(15) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C7 1.33(2) . ? C6 C11 1.36(2) . ? C7 C8 1.419(19) . ? C7 H7 0.9400 . ? C8 C9 1.36(2) . ? C8 H8 0.9400 . ? C9 C10 1.24(2) . ? C9 H9 0.9400 . ? C10 C11 1.455(19) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C17 1.350(17) . ? C12 C13 1.390(16) . ? C13 C14 1.398(16) . ? C13 H13 0.9400 . ? C14 C15 1.35(2) . ? C14 H14 0.9400 . ? C15 C16 1.34(2) . ? C15 H15 0.9400 . ? C16 C17 1.390(18) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C18' H18D 0.9700 . ? C18' H18E 0.9700 . ? C18' H18F 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C19' H19D 0.9700 . ? C19' H19E 0.9700 . ? C19' H19F 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C20' H20D 0.9700 . ? C20' H20E 0.9700 . ? C20' H20F 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C21' H21D 0.9700 . ? C21' H21E 0.9700 . ? C21' H21F 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C22' H22D 0.9700 . ? C22' H22E 0.9700 . ? C22' H22F 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C23' H23D 0.9700 . ? C23' H23E 0.9700 . ? C23' H23F 0.9700 . ? C24 C25 1.50(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24' C25' 1.49(2) . ? C24' H24C 0.9800 . ? C24' H24D 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25' H25C 0.9800 . ? C25' H25D 0.9800 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 C29 1.45(2) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? B1 H1A 1.111(10) . ? B1 H1B 1.107(10) . ? B1 H1C 1.106(10) . ? B1 H1D 1.101(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Nd1 N2 72.2(3) . . ? N4 Nd1 O1 88.7(4) . . ? N2 Nd1 O1 85.9(3) . . ? N4 Nd1 N3 54.1(3) . . ? N2 Nd1 N3 125.3(3) . . ? O1 Nd1 N3 83.3(3) . . ? N4 Nd1 N1 125.1(3) . . ? N2 Nd1 N1 53.1(3) . . ? O1 Nd1 N1 83.3(3) . . ? N3 Nd1 N1 166.5(3) . . ? N4 Nd1 O2 133.0(3) . . ? N2 Nd1 O2 136.0(3) . . ? O1 Nd1 O2 63.7(2) . . ? N3 Nd1 O2 84.0(3) . . ? N1 Nd1 O2 90.4(3) . . ? N4 Nd1 B1 106.3(5) . . ? N2 Nd1 B1 107.6(4) . . ? O1 Nd1 B1 162.2(3) . . ? N3 Nd1 B1 97.6(5) . . ? N1 Nd1 B1 95.4(5) . . ? O2 Nd1 B1 98.6(3) . . ? N4 Nd1 C2 26.7(3) . . ? N2 Nd1 C2 97.6(3) . . ? O1 Nd1 C2 82.4(3) . . ? N3 Nd1 C2 27.8(3) . . ? N1 Nd1 C2 148.3(4) . . ? O2 Nd1 C2 108.1(3) . . ? B1 Nd1 C2 106.6(5) . . ? N4 Nd1 C1 98.6(3) . . ? N2 Nd1 C1 26.4(3) . . ? O1 Nd1 C1 84.9(3) . . ? N3 Nd1 C1 150.3(3) . . ? N1 Nd1 C1 26.8(3) . . ? O2 Nd1 C1 114.6(3) . . ? B1 Nd1 C1 101.9(5) . . ? C2 Nd1 C1 123.4(4) . . ? N4 Nd1 H1A 93.8(15) . . ? N2 Nd1 H1A 83.4(6) . . ? O1 Nd1 H1A 167.7(12) . . ? N3 Nd1 H1A 107.9(15) . . ? N1 Nd1 H1A 85.4(15) . . ? O2 Nd1 H1A 121.5(9) . . ? B1 Nd1 H1A 24.9(3) . . ? C2 Nd1 H1A 105.0(17) . . ? C1 Nd1 H1A 82.8(11) . . ? N4 Nd1 H1B 130.7(6) . . ? N2 Nd1 H1B 114.2(15) . . ? O1 Nd1 H1B 138.8(6) . . ? N3 Nd1 H1B 108.7(15) . . ? N1 Nd1 H1B 81.9(14) . . ? O2 Nd1 H1B 78.2(10) . . ? B1 Nd1 H1B 24.6(4) . . ? C2 Nd1 H1B 126.2(12) . . ? C1 Nd1 H1B 98.1(16) . . ? H1A Nd1 H1B 43.4(8) . . ? N1 Si1 C18 118.4(12) . . ? N1 Si1 C19' 108.3(12) . . ? C18 Si1 C19' 49.8(14) . . ? N1 Si1 C20 108.7(12) . . ? C18 Si1 C20 112.7(16) . . ? C19' Si1 C20 142.8(17) . . ? N1 Si1 C18' 117.4(12) . . ? C18 Si1 C18' 58.3(15) . . ? C19' Si1 C18' 106.5(16) . . ? C20 Si1 C18' 58.3(15) . . ? N1 Si1 C20' 107.6(12) . . ? C18 Si1 C20' 133.9(16) . . ? C19' Si1 C20' 119.2(17) . . ? C20 Si1 C20' 43.7(14) . . ? C18' Si1 C20' 98.2(16) . . ? N1 Si1 C19 108.8(11) . . ? C18 Si1 C19 102.7(15) . . ? C19' Si1 C19 59.4(15) . . ? C20 Si1 C19 104.4(17) . . ? C18' Si1 C19 133.6(16) . . ? C20' Si1 C19 63.2(16) . . ? N3 Si2 C22 109.6(11) . . ? N3 Si2 C21' 114.1(12) . . ? C22 Si2 C21' 129.2(14) . . ? N3 Si2 C23' 109.9(11) . . ? C22 Si2 C23' 80.8(14) . . ? C21' Si2 C23' 106.6(14) . . ? N3 Si2 C22' 112.6(10) . . ? C22 Si2 C22' 25.9(11) . . ? C21' Si2 C22' 109.7(13) . . ? C23' Si2 C22' 103.3(13) . . ? N3 Si2 C23 107.3(11) . . ? C22 Si2 C23 105.7(14) . . ? C21' Si2 C23 85.0(14) . . ? C23' Si2 C23 26.0(11) . . ? C22' Si2 C23 125.4(14) . . ? N3 Si2 C21 114.9(12) . . ? C22 Si2 C21 115.2(14) . . ? C21' Si2 C21 19.9(13) . . ? C23' Si2 C21 121.6(15) . . ? C22' Si2 C21 92.3(14) . . ? C23 Si2 C21 103.2(13) . . ? C26 O1 C24' 115.4(15) . . ? C26 O1 C24 112.7(15) . . ? C24' O1 C24 50.4(14) . . ? C26 O1 Nd1 122.9(7) . . ? C24' O1 Nd1 116.9(14) . . ? C24 O1 Nd1 117.4(14) . . ? C27 O2 C25 114.0(16) . . ? C27 O2 C25' 111.1(17) . . ? C25 O2 C25' 3(3) . . ? C27 O2 Nd1 130.4(7) . . ? C25 O2 Nd1 115.5(15) . . ? C25' O2 Nd1 118.5(15) . . ? C30 O3 C28 114.1(16) . . ? C29 O4 C31 109.3(14) . . ? C1 N1 Si1 131.1(9) . . ? C1 N1 Nd1 90.6(7) . . ? Si1 N1 Nd1 136.7(5) . . ? C1 N2 C3 124.1(9) . . ? C1 N2 Nd1 97.5(7) . . ? C3 N2 Nd1 138.5(6) . . ? C2 N3 Si2 129.7(8) . . ? C2 N3 Nd1 90.1(6) . . ? Si2 N3 Nd1 139.9(5) . . ? C2 N4 C5 122.1(10) . . ? C2 N4 Nd1 97.8(7) . . ? C5 N4 Nd1 136.9(7) . . ? N2 C1 N1 118.6(11) . . ? N2 C1 C6 120.3(12) . . ? N1 C1 C6 121.0(12) . . ? N2 C1 Nd1 56.1(6) . . ? N1 C1 Nd1 62.6(6) . . ? C6 C1 Nd1 176.5(10) . . ? N4 C2 N3 116.5(10) . . ? N4 C2 C12 123.0(11) . . ? N3 C2 C12 120.5(10) . . ? N4 C2 Nd1 55.5(6) . . ? N3 C2 Nd1 62.1(6) . . ? C12 C2 Nd1 170.7(9) . . ? C4 C3 N2 112.8(9) . . ? C4 C3 H3A 109.0 . . ? N2 C3 H3A 109.0 . . ? C4 C3 H3B 109.0 . . ? N2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C3 116.4(11) . . ? C5 C4 H4A 108.2 . . ? C3 C4 H4A 108.2 . . ? C5 C4 H4B 108.2 . . ? C3 C4 H4B 108.2 . . ? H4A C4 H4B 107.3 . . ? C4 C5 N4 112.8(10) . . ? C4 C5 H5A 109.0 . . ? N4 C5 H5A 109.0 . . ? C4 C5 H5B 109.0 . . ? N4 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C7 C6 C11 114.8(17) . . ? C7 C6 C1 122.1(17) . . ? C11 C6 C1 123.1(17) . . ? C6 C7 C8 126.2(19) . . ? C6 C7 H7 116.9 . . ? C8 C7 H7 116.9 . . ? C9 C8 C7 112.3(18) . . ? C9 C8 H8 123.9 . . ? C7 C8 H8 123.9 . . ? C10 C9 C8 127.9(19) . . ? C10 C9 H9 116.0 . . ? C8 C9 H9 116.0 . . ? C9 C10 C11 116.7(19) . . ? C9 C10 H10 121.7 . . ? C11 C10 H10 121.7 . . ? C6 C11 C10 122.0(18) . . ? C6 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? C17 C12 C13 117.9(11) . . ? C17 C12 C2 121.8(12) . . ? C13 C12 C2 120.3(12) . . ? C12 C13 C14 119.8(14) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 120.1(16) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 120.1(16) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 120.2(16) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C12 C17 C16 121.5(14) . . ? C12 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? Si1 C18' H18D 109.5 . . ? Si1 C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? Si1 C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? Si1 C19' H19D 109.5 . . ? Si1 C19' H19E 109.5 . . ? H19D C19' H19E 109.5 . . ? Si1 C19' H19F 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? Si1 C20' H20D 109.5 . . ? Si1 C20' H20E 109.5 . . ? H20D C20' H20E 109.5 . . ? Si1 C20' H20F 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? Si2 C21' H21D 109.5 . . ? Si2 C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? Si2 C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? Si2 C22' H22D 109.5 . . ? Si2 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? Si2 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? Si2 C23' H23D 109.5 . . ? Si2 C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? Si2 C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? O1 C24 C25 105(2) . . ? O1 C24 H24A 110.8 . . ? C25 C24 H24A 110.8 . . ? O1 C24 H24B 110.8 . . ? C25 C24 H24B 110.8 . . ? H24A C24 H24B 108.9 . . ? O1 C24' C25' 111(3) . . ? O1 C24' H24C 109.4 . . ? C25' C24' H24C 109.4 . . ? O1 C24' H24D 109.4 . . ? C25' C24' H24D 109.4 . . ? H24C C24' H24D 108.0 . . ? O2 C25 C24 113(3) . . ? O2 C25 H25A 109.1 . . ? C24 C25 H25A 109.1 . . ? O2 C25 H25B 109.1 . . ? C24 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? O2 C25' C24' 108(3) . . ? O2 C25' H25C 110.0 . . ? C24' C25' H25C 110.0 . . ? O2 C25' H25D 110.0 . . ? C24' C25' H25D 110.0 . . ? H25C C25' H25D 108.4 . . ? O1 C26 H26A 109.5 . . ? O1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O2 C27 H27A 109.5 . . ? O2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 O3 109.7(14) . . ? C29 C28 H28A 109.7 . . ? O3 C28 H28A 109.7 . . ? C29 C28 H28B 109.7 . . ? O3 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? O4 C29 C28 111.0(16) . . ? O4 C29 H29A 109.4 . . ? C28 C29 H29A 109.4 . . ? O4 C29 H29B 109.4 . . ? C28 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? O3 C30 H30A 109.5 . . ? O3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O4 C31 H31A 109.5 . . ? O4 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O4 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Nd1 B1 H1A 68(5) . . ? Nd1 B1 H1B 73(5) . . ? H1A B1 H1B 112.4(14) . . ? Nd1 B1 H1C 82(4) . . ? H1A B1 H1C 112.6(14) . . ? H1B B1 H1C 113.1(14) . . ? Nd1 B1 H1D 164(4) . . ? H1A B1 H1D 100(6) . . ? H1B B1 H1D 104(6) . . ? H1C B1 H1D 113.6(15) . . ? 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 N4 Nd1 O1 C26 39.2(12) . . . . ? N2 Nd1 O1 C26 -33.1(12) . . . . ? N3 Nd1 O1 C26 93.2(12) . . . . ? N1 Nd1 O1 C26 -86.4(12) . . . . ? O2 Nd1 O1 C26 179.8(13) . . . . ? B1 Nd1 O1 C26 -173.0(17) . . . . ? C2 Nd1 O1 C26 65.2(12) . . . . ? C1 Nd1 O1 C26 -59.5(12) . . . . ? N4 Nd1 O1 C24' -166.5(17) . . . . ? N2 Nd1 O1 C24' 121.3(17) . . . . ? N3 Nd1 O1 C24' -112.5(17) . . . . ? N1 Nd1 O1 C24' 67.9(17) . . . . ? O2 Nd1 O1 C24' -25.9(17) . . . . ? B1 Nd1 O1 C24' -19(2) . . . . ? C2 Nd1 O1 C24' -140.5(17) . . . . ? C1 Nd1 O1 C24' 94.8(17) . . . . ? N4 Nd1 O1 C24 -109.3(15) . . . . ? N2 Nd1 O1 C24 178.4(15) . . . . ? N3 Nd1 O1 C24 -55.3(15) . . . . ? N1 Nd1 O1 C24 125.1(15) . . . . ? O2 Nd1 O1 C24 31.3(14) . . . . ? B1 Nd1 O1 C24 38(2) . . . . ? C2 Nd1 O1 C24 -83.3(15) . . . . ? C1 Nd1 O1 C24 152.0(15) . . . . ? N4 Nd1 O2 C27 -123.3(12) . . . . ? N2 Nd1 O2 C27 125.4(12) . . . . ? O1 Nd1 O2 C27 176.6(13) . . . . ? N3 Nd1 O2 C27 -98.0(13) . . . . ? N1 Nd1 O2 C27 94.2(12) . . . . ? B1 Nd1 O2 C27 -1.2(13) . . . . ? C2 Nd1 O2 C27 -112.0(13) . . . . ? C1 Nd1 O2 C27 106.1(12) . . . . ? N4 Nd1 O2 C25 60(2) . . . . ? N2 Nd1 O2 C25 -52(2) . . . . ? O1 Nd1 O2 C25 -1(2) . . . . ? N3 Nd1 O2 C25 85(2) . . . . ? N1 Nd1 O2 C25 -83(2) . . . . ? B1 Nd1 O2 C25 -178(2) . . . . ? C2 Nd1 O2 C25 71(2) . . . . ? C1 Nd1 O2 C25 -71(2) . . . . ? N4 Nd1 O2 C25' 58(3) . . . . ? N2 Nd1 O2 C25' -53(3) . . . . ? O1 Nd1 O2 C25' -2(3) . . . . ? N3 Nd1 O2 C25' 83(3) . . . . ? N1 Nd1 O2 C25' -84(3) . . . . ? B1 Nd1 O2 C25' -180(3) . . . . ? C2 Nd1 O2 C25' 69(3) . . . . ? C1 Nd1 O2 C25' -72(3) . . . . ? C18 Si1 N1 C1 18.3(19) . . . . ? C19' Si1 N1 C1 71.8(17) . . . . ? C20 Si1 N1 C1 -112.0(17) . . . . ? C18' Si1 N1 C1 -48.7(17) . . . . ? C20' Si1 N1 C1 -158.2(16) . . . . ? C19 Si1 N1 C1 134.9(16) . . . . ? C18 Si1 N1 Nd1 -143.0(15) . . . . ? C19' Si1 N1 Nd1 -89.5(14) . . . . ? C20 Si1 N1 Nd1 86.6(15) . . . . ? C18' Si1 N1 Nd1 150.0(13) . . . . ? C20' Si1 N1 Nd1 40.5(15) . . . . ? C19 Si1 N1 Nd1 -26.4(14) . . . . ? N4 Nd1 N1 C1 8.4(9) . . . . ? N2 Nd1 N1 C1 2.1(7) . . . . ? O1 Nd1 N1 C1 92.0(7) . . . . ? N3 Nd1 N1 C1 90.3(14) . . . . ? O2 Nd1 N1 C1 155.4(7) . . . . ? B1 Nd1 N1 C1 -105.9(7) . . . . ? C2 Nd1 N1 C1 28.4(11) . . . . ? N4 Nd1 N1 Si1 174.4(7) . . . . ? N2 Nd1 N1 Si1 168.1(9) . . . . ? O1 Nd1 N1 Si1 -102.0(7) . . . . ? N3 Nd1 N1 Si1 -103.6(13) . . . . ? O2 Nd1 N1 Si1 -38.5(7) . . . . ? B1 Nd1 N1 Si1 60.2(8) . . . . ? C2 Nd1 N1 Si1 -165.6(6) . . . . ? C1 Nd1 N1 Si1 166.0(12) . . . . ? N4 Nd1 N2 C1 -176.8(9) . . . . ? O1 Nd1 N2 C1 -86.8(8) . . . . ? N3 Nd1 N2 C1 -165.6(7) . . . . ? N1 Nd1 N2 C1 -2.1(7) . . . . ? O2 Nd1 N2 C1 -42.4(10) . . . . ? B1 Nd1 N2 C1 81.3(9) . . . . ? C2 Nd1 N2 C1 -168.6(7) . . . . ? N4 Nd1 N2 C3 4.3(12) . . . . ? O1 Nd1 N2 C3 94.3(12) . . . . ? N3 Nd1 N2 C3 15.5(14) . . . . ? N1 Nd1 N2 C3 179.0(14) . . . . ? O2 Nd1 N2 C3 138.7(11) . . . . ? B1 Nd1 N2 C3 -97.6(13) . . . . ? C2 Nd1 N2 C3 12.5(13) . . . . ? C1 Nd1 N2 C3 -178.9(17) . . . . ? C22 Si2 N3 C2 113.4(14) . . . . ? C21' Si2 N3 C2 -40.0(16) . . . . ? C23' Si2 N3 C2 -159.6(14) . . . . ? C22' Si2 N3 C2 85.8(15) . . . . ? C23 Si2 N3 C2 -132.3(15) . . . . ? C21 Si2 N3 C2 -18.1(17) . . . . ? C22 Si2 N3 Nd1 -75.4(14) . . . . ? C21' Si2 N3 Nd1 131.2(12) . . . . ? C23' Si2 N3 Nd1 11.6(14) . . . . ? C22' Si2 N3 Nd1 -103.0(13) . . . . ? C23 Si2 N3 Nd1 38.9(14) . . . . ? C21 Si2 N3 Nd1 153.0(12) . . . . ? N4 Nd1 N3 C2 6.8(7) . . . . ? N2 Nd1 N3 C2 -6.3(9) . . . . ? O1 Nd1 N3 C2 -86.4(7) . . . . ? N1 Nd1 N3 C2 -84.7(14) . . . . ? O2 Nd1 N3 C2 -150.5(7) . . . . ? B1 Nd1 N3 C2 111.5(8) . . . . ? C1 Nd1 N3 C2 -19.2(11) . . . . ? N4 Nd1 N3 Si2 -166.4(11) . . . . ? N2 Nd1 N3 Si2 -179.5(7) . . . . ? O1 Nd1 N3 Si2 100.4(9) . . . . ? N1 Nd1 N3 Si2 102.0(16) . . . . ? O2 Nd1 N3 Si2 36.3(8) . . . . ? B1 Nd1 N3 Si2 -61.7(9) . . . . ? C2 Nd1 N3 Si2 -173.2(14) . . . . ? C1 Nd1 N3 Si2 167.5(6) . . . . ? N2 Nd1 N4 C2 161.7(10) . . . . ? O1 Nd1 N4 C2 75.6(9) . . . . ? N3 Nd1 N4 C2 -7.1(8) . . . . ? N1 Nd1 N4 C2 156.4(8) . . . . ? O2 Nd1 N4 C2 24.5(11) . . . . ? B1 Nd1 N4 C2 -94.7(10) . . . . ? C1 Nd1 N4 C2 160.2(9) . . . . ? N2 Nd1 N4 C5 3.0(13) . . . . ? O1 Nd1 N4 C5 -83.1(14) . . . . ? N3 Nd1 N4 C5 -165.8(16) . . . . ? N1 Nd1 N4 C5 -2.3(16) . . . . ? O2 Nd1 N4 C5 -134.2(12) . . . . ? B1 Nd1 N4 C5 106.7(14) . . . . ? C2 Nd1 N4 C5 -159(2) . . . . ? C1 Nd1 N4 C5 1.5(14) . . . . ? C3 N2 C1 N1 -177.0(11) . . . . ? Nd1 N2 C1 N1 3.9(13) . . . . ? C3 N2 C1 C6 -0.6(19) . . . . ? Nd1 N2 C1 C6 -179.7(12) . . . . ? C3 N2 C1 Nd1 179.1(14) . . . . ? Si1 N1 C1 N2 -170.9(9) . . . . ? Nd1 N1 C1 N2 -3.6(12) . . . . ? Si1 N1 C1 C6 12.6(19) . . . . ? Nd1 N1 C1 C6 180.0(12) . . . . ? Si1 N1 C1 Nd1 -167.3(11) . . . . ? N4 Nd1 C1 N2 3.1(9) . . . . ? O1 Nd1 C1 N2 91.0(8) . . . . ? N3 Nd1 C1 N2 24.2(12) . . . . ? N1 Nd1 C1 N2 176.2(12) . . . . ? O2 Nd1 C1 N2 149.0(7) . . . . ? B1 Nd1 C1 N2 -105.7(8) . . . . ? C2 Nd1 C1 N2 13.6(9) . . . . ? N4 Nd1 C1 N1 -173.1(7) . . . . ? N2 Nd1 C1 N1 -176.2(12) . . . . ? O1 Nd1 C1 N1 -85.2(7) . . . . ? N3 Nd1 C1 N1 -152.0(7) . . . . ? O2 Nd1 C1 N1 -27.2(8) . . . . ? B1 Nd1 C1 N1 78.2(7) . . . . ? C2 Nd1 C1 N1 -162.6(7) . . . . ? N4 Nd1 C1 C6 8(17) . . . . ? N2 Nd1 C1 C6 4(17) . . . . ? O1 Nd1 C1 C6 95(17) . . . . ? N3 Nd1 C1 C6 29(17) . . . . ? N1 Nd1 C1 C6 -179(100) . . . . ? O2 Nd1 C1 C6 153(17) . . . . ? B1 Nd1 C1 C6 -101(17) . . . . ? C2 Nd1 C1 C6 18(17) . . . . ? C5 N4 C2 N3 175.2(12) . . . . ? Nd1 N4 C2 N3 12.3(13) . . . . ? C5 N4 C2 C12 -6(2) . . . . ? Nd1 N4 C2 C12 -169.0(10) . . . . ? C5 N4 C2 Nd1 162.9(16) . . . . ? Si2 N3 C2 N4 162.9(10) . . . . ? Nd1 N3 C2 N4 -11.4(12) . . . . ? Si2 N3 C2 C12 -15.9(18) . . . . ? Nd1 N3 C2 C12 169.8(11) . . . . ? Si2 N3 C2 Nd1 174.3(12) . . . . ? N2 Nd1 C2 N4 -17.6(10) . . . . ? O1 Nd1 C2 N4 -102.4(9) . . . . ? N3 Nd1 C2 N4 167.6(14) . . . . ? N1 Nd1 C2 N4 -38.6(12) . . . . ? O2 Nd1 C2 N4 -161.4(9) . . . . ? B1 Nd1 C2 N4 93.4(10) . . . . ? C1 Nd1 C2 N4 -23.7(10) . . . . ? N4 Nd1 C2 N3 -167.6(14) . . . . ? N2 Nd1 C2 N3 174.8(7) . . . . ? O1 Nd1 C2 N3 90.0(7) . . . . ? N1 Nd1 C2 N3 153.8(6) . . . . ? O2 Nd1 C2 N3 31.0(8) . . . . ? B1 Nd1 C2 N3 -74.2(8) . . . . ? C1 Nd1 C2 N3 168.7(7) . . . . ? N4 Nd1 C2 C12 83(5) . . . . ? N2 Nd1 C2 C12 66(5) . . . . ? O1 Nd1 C2 C12 -19(5) . . . . ? N3 Nd1 C2 C12 -109(5) . . . . ? N1 Nd1 C2 C12 45(5) . . . . ? O2 Nd1 C2 C12 -78(5) . . . . ? B1 Nd1 C2 C12 177(5) . . . . ? C1 Nd1 C2 C12 60(5) . . . . ? C1 N2 C3 C4 -158.2(13) . . . . ? Nd1 N2 C3 C4 20.5(19) . . . . ? N2 C3 C4 C5 -59.0(16) . . . . ? C3 C4 C5 N4 65.8(16) . . . . ? C2 N4 C5 C4 170.8(13) . . . . ? Nd1 N4 C5 C4 -34(2) . . . . ? N2 C1 C6 C7 -96.7(18) . . . . ? N1 C1 C6 C7 80(2) . . . . ? Nd1 C1 C6 C7 -101(17) . . . . ? N2 C1 C6 C11 84(2) . . . . ? N1 C1 C6 C11 -99.6(18) . . . . ? Nd1 C1 C6 C11 80(17) . . . . ? C11 C6 C7 C8 2(3) . . . . ? C1 C6 C7 C8 -177.2(14) . . . . ? C6 C7 C8 C9 -1(2) . . . . ? C7 C8 C9 C10 1(3) . . . . ? C8 C9 C10 C11 -3(3) . . . . ? C7 C6 C11 C10 -3(2) . . . . ? C1 C6 C11 C10 175.9(13) . . . . ? C9 C10 C11 C6 4(2) . . . . ? N4 C2 C12 C17 107.4(16) . . . . ? N3 C2 C12 C17 -73.8(16) . . . . ? Nd1 C2 C12 C17 30(6) . . . . ? N4 C2 C12 C13 -71.7(17) . . . . ? N3 C2 C12 C13 107.0(14) . . . . ? Nd1 C2 C12 C13 -149(5) . . . . ? C17 C12 C13 C14 5.4(19) . . . . ? C2 C12 C13 C14 -175.4(12) . . . . ? C12 C13 C14 C15 -7(2) . . . . ? C13 C14 C15 C16 6(2) . . . . ? C14 C15 C16 C17 -3(3) . . . . ? C13 C12 C17 C16 -3(2) . . . . ? C2 C12 C17 C16 178.2(12) . . . . ? C15 C16 C17 C12 1(2) . . . . ? C26 O1 C24 C25 153(2) . . . . ? C24' O1 C24 C25 48(3) . . . . ? Nd1 O1 C24 C25 -55(3) . . . . ? C26 O1 C24' C25' -153(3) . . . . ? C24 O1 C24' C25' -53(3) . . . . ? Nd1 O1 C24' C25' 51(3) . . . . ? C27 O2 C25 C24 155(3) . . . . ? C25' O2 C25 C24 128(72) . . . . ? Nd1 O2 C25 C24 -27(4) . . . . ? O1 C24 C25 O2 52(4) . . . . ? C27 O2 C25' C24' -153(3) . . . . ? C25 O2 C25' C24' 1(67) . . . . ? Nd1 O2 C25' C24' 26(4) . . . . ? O1 C24' C25' O2 -49(4) . . . . ? C30 O3 C28 C29 167.5(18) . . . . ? C31 O4 C29 C28 179.7(14) . . . . ? O3 C28 C29 O4 -74(2) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.675 _refine_diff_density_min -0.675 _refine_diff_density_rms 0.104 # Attachment 'shelxl (3).cif' data_shelxl3 _database_code_depnum_ccdc_archive 'CCDC 843491' #TrackingRef 'shelxl (3).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H48 B N4 O2 Si2 Sm, C4 H10 O2' _chemical_formula_sum 'C31 H58 B N4 O4 Si2 Sm' _chemical_formula_weight 768.15 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 8.6970(5) _cell_length_b 19.9369(11) _cell_length_c 23.1964(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4022.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 13115 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 1.554 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.474 _exptl_absorpt_correction_T_max 0.733 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27690 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9171 _reflns_number_gt 8568 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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. ; _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^)+(0.0587P)^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 -0.018(15) _refine_ls_number_reflns 9171 _refine_ls_number_parameters 377 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1133 _refine_ls_wR_factor_gt 0.1105 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.44325(3) 0.622054(12) 0.304243(11) 0.04068(8) Uani 1 1 d . A . Si1 Si 0.4119(3) 0.58057(10) 0.13710(9) 0.0790(7) Uani 1 1 d D . . Si2 Si 0.3583(2) 0.55711(9) 0.46395(8) 0.0659(5) Uani 1 1 d D . . O1 O 0.6759(4) 0.54964(19) 0.3057(2) 0.0714(12) Uani 1 1 d D . . O2 O 0.3950(4) 0.49528(17) 0.3022(2) 0.0640(11) Uani 1 1 d D . . O3 O 0.7965(9) 0.3511(4) 0.3574(4) 0.134(3) Uani 1 1 d . . . O4 O 0.9354(8) 0.3943(4) 0.2516(3) 0.116(2) Uani 1 1 d . . . N1 N 0.4881(7) 0.6219(3) 0.1966(2) 0.0679(13) Uani 1 1 d . A . N2 N 0.5941(6) 0.7006(3) 0.2515(2) 0.0618(14) Uani 1 1 d . . . N3 N 0.4489(7) 0.6048(2) 0.4114(2) 0.0602(12) Uani 1 1 d . A . N4 N 0.5673(8) 0.6928(2) 0.3712(2) 0.0647(14) Uani 1 1 d . . . C1 C 0.5742(7) 0.6755(3) 0.2001(3) 0.0562(13) Uani 1 1 d . A . C2 C 0.5443(8) 0.6557(3) 0.4176(2) 0.0556(13) Uani 1 1 d . A . C3 C 0.6956(7) 0.7577(3) 0.2617(3) 0.0590(15) Uani 1 1 d . C . H3A H 0.6841 0.7903 0.2304 0.071 Uiso 1 1 calc R . . H3B H 0.8027 0.7425 0.2623 0.071 Uiso 1 1 calc R . . C4 C 0.6568(8) 0.7905(3) 0.3184(3) 0.0626(16) Uani 1 1 d . . . H4A H 0.7205 0.8308 0.3224 0.075 Uiso 1 1 calc R C . H4B H 0.5493 0.8051 0.3169 0.075 Uiso 1 1 calc R . . C5 C 0.6779(11) 0.7486(3) 0.3711(3) 0.081(2) Uani 1 1 d . C . H5A H 0.7829 0.7308 0.3721 0.098 Uiso 1 1 calc R . . H5B H 0.6625 0.7762 0.4056 0.098 Uiso 1 1 calc R . . C6 C 0.6491(13) 0.7053(5) 0.1486(4) 0.0970(11) Uani 1 1 d . . . C7 C 0.7828(12) 0.6757(5) 0.1278(4) 0.0970(11) Uani 1 1 d . C . H7 H 0.8262 0.6395 0.1481 0.116 Uiso 1 1 calc R . . C8 C 0.8531(12) 0.6981(5) 0.0783(4) 0.0970(11) Uani 1 1 d . . . H8 H 0.9410 0.6769 0.0634 0.116 Uiso 1 1 calc R C . C9 C 0.7923(12) 0.7503(5) 0.0529(4) 0.0970(11) Uani 1 1 d . C . H9 H 0.8429 0.7663 0.0199 0.116 Uiso 1 1 calc R . . C10 C 0.6694(12) 0.7822(5) 0.0686(4) 0.0970(11) Uani 1 1 d . . . H10 H 0.6317 0.8189 0.0474 0.116 Uiso 1 1 calc R C . C11 C 0.5928(12) 0.7588(5) 0.1204(4) 0.0970(11) Uani 1 1 d . C . H11 H 0.5045 0.7809 0.1340 0.116 Uiso 1 1 calc R . . C12 C 0.6231(7) 0.6693(3) 0.4744(3) 0.0574(14) Uani 1 1 d . . . C13 C 0.5775(9) 0.7231(4) 0.5081(3) 0.078(2) Uani 1 1 d . C . H13 H 0.5005 0.7523 0.4948 0.093 Uiso 1 1 calc R . . C14 C 0.6450(11) 0.7339(5) 0.5612(3) 0.094(3) Uani 1 1 d . . . H14 H 0.6092 0.7692 0.5845 0.113 Uiso 1 1 calc R C . C15 C 0.7581(10) 0.6959(5) 0.5799(4) 0.090(3) Uani 1 1 d . C . H15 H 0.8050 0.7054 0.6155 0.109 Uiso 1 1 calc R . . C16 C 0.8080(10) 0.6421(5) 0.5473(4) 0.098(3) Uani 1 1 d . . . H16 H 0.8872 0.6142 0.5609 0.118 Uiso 1 1 calc R C . C17 C 0.7384(9) 0.6298(4) 0.4934(4) 0.084(2) Uani 1 1 d . C . H17 H 0.7725 0.5937 0.4706 0.101 Uiso 1 1 calc R . . C18 C 0.425(3) 0.6190(11) 0.0677(8) 0.131(3) Uiso 0.50 1 d PD A 1 H18A H 0.4081 0.6669 0.0714 0.197 Uiso 0.50 1 calc PR A 1 H18B H 0.3483 0.5999 0.0424 0.197 Uiso 0.50 1 calc PR A 1 H18C H 0.5268 0.6111 0.0518 0.197 Uiso 0.50 1 calc PR A 1 C18' C 0.581(2) 0.5512(11) 0.0864(10) 0.131(3) Uiso 0.50 1 d PD A 2 H18D H 0.6397 0.5900 0.0739 0.197 Uiso 0.50 1 calc PR A 2 H18E H 0.5391 0.5284 0.0530 0.197 Uiso 0.50 1 calc PR A 2 H18F H 0.6480 0.5208 0.1073 0.197 Uiso 0.50 1 calc PR A 2 C19 C 0.1946(18) 0.5670(12) 0.1517(11) 0.131(3) Uiso 0.50 1 d PD A 1 H19A H 0.1808 0.5494 0.1904 0.197 Uiso 0.50 1 calc PR A 1 H19B H 0.1536 0.5353 0.1239 0.197 Uiso 0.50 1 calc PR A 1 H19C H 0.1408 0.6094 0.1481 0.197 Uiso 0.50 1 calc PR A 1 C19' C 0.305(2) 0.6361(10) 0.0912(10) 0.131(3) Uiso 0.50 1 d PD A 2 H19D H 0.2047 0.6444 0.1080 0.197 Uiso 0.50 1 calc PR A 2 H19E H 0.2926 0.6157 0.0536 0.197 Uiso 0.50 1 calc PR A 2 H19F H 0.3601 0.6782 0.0873 0.197 Uiso 0.50 1 calc PR A 2 C20 C 0.500(3) 0.4986(9) 0.1320(11) 0.131(3) Uiso 0.50 1 d PD A 1 H20A H 0.6104 0.5030 0.1347 0.197 Uiso 0.50 1 calc PR A 1 H20B H 0.4728 0.4784 0.0953 0.197 Uiso 0.50 1 calc PR A 1 H20C H 0.4625 0.4705 0.1632 0.197 Uiso 0.50 1 calc PR A 1 C20' C 0.329(3) 0.4996(9) 0.1607(10) 0.131(3) Uiso 0.50 1 d PD A 2 H20D H 0.3867 0.4630 0.1437 0.197 Uiso 0.50 1 calc PR A 2 H20E H 0.2225 0.4969 0.1484 0.197 Uiso 0.50 1 calc PR A 2 H20F H 0.3340 0.4965 0.2024 0.197 Uiso 0.50 1 calc PR A 2 C21 C 0.349(2) 0.5965(9) 0.5363(7) 0.087(2) Uiso 0.50 1 d PD B 1 H21A H 0.4475 0.5913 0.5555 0.131 Uiso 0.50 1 calc PR B 1 H21B H 0.2695 0.5750 0.5589 0.131 Uiso 0.50 1 calc PR B 1 H21C H 0.3258 0.6439 0.5322 0.131 Uiso 0.50 1 calc PR B 1 C21' C 0.291(2) 0.6051(9) 0.5273(7) 0.087(2) Uiso 0.50 1 d PD B 2 H21D H 0.3784 0.6182 0.5506 0.131 Uiso 0.50 1 calc PR B 2 H21E H 0.2222 0.5774 0.5500 0.131 Uiso 0.50 1 calc PR B 2 H21F H 0.2366 0.6449 0.5144 0.131 Uiso 0.50 1 calc PR B 2 C22 C 0.431(2) 0.4726(7) 0.4656(8) 0.087(2) Uiso 0.50 1 d PD B 1 H22A H 0.3982 0.4489 0.4313 0.131 Uiso 0.50 1 calc PR B 1 H22B H 0.3927 0.4497 0.4995 0.131 Uiso 0.50 1 calc PR B 1 H22C H 0.5429 0.4736 0.4668 0.131 Uiso 0.50 1 calc PR B 1 C22' C 0.4787(19) 0.4837(8) 0.4857(8) 0.087(2) Uiso 0.50 1 d PD B 2 H22D H 0.5329 0.4665 0.4523 0.131 Uiso 0.50 1 calc PR B 2 H22E H 0.4132 0.4488 0.5014 0.131 Uiso 0.50 1 calc PR B 2 H22F H 0.5526 0.4976 0.5147 0.131 Uiso 0.50 1 calc PR B 2 C23 C 0.1503(15) 0.5514(9) 0.4430(8) 0.087(2) Uiso 0.50 1 d PD B 1 H23A H 0.1070 0.5961 0.4405 0.131 Uiso 0.50 1 calc PR B 1 H23B H 0.0948 0.5257 0.4718 0.131 Uiso 0.50 1 calc PR B 1 H23C H 0.1416 0.5293 0.4058 0.131 Uiso 0.50 1 calc PR B 1 C23' C 0.1768(17) 0.5209(8) 0.4343(8) 0.087(2) Uiso 0.50 1 d PD B 2 H23D H 0.1167 0.5562 0.4163 0.131 Uiso 0.50 1 calc PR B 2 H23E H 0.1178 0.5008 0.4653 0.131 Uiso 0.50 1 calc PR B 2 H23F H 0.2015 0.4869 0.4058 0.131 Uiso 0.50 1 calc PR B 2 C24 C 0.6597(18) 0.4873(6) 0.3314(8) 0.076(3) Uani 0.50 1 d PD C 1 H24A H 0.6363 0.4923 0.3725 0.091 Uiso 0.50 1 calc PR C 1 H24B H 0.7546 0.4613 0.3274 0.091 Uiso 0.50 1 calc PR C 1 C24' C 0.6593(17) 0.4858(6) 0.2846(8) 0.076(3) Uani 0.50 1 d PD C 2 H24C H 0.7515 0.4600 0.2944 0.091 Uiso 0.50 1 calc PR C 2 H24D H 0.6534 0.4882 0.2424 0.091 Uiso 0.50 1 calc PR C 2 C25 C 0.5295(19) 0.4532(11) 0.3007(15) 0.080(3) Uani 0.50 1 d PD C 1 H25A H 0.5585 0.4444 0.2605 0.096 Uiso 0.50 1 calc PR C 1 H25B H 0.5071 0.4102 0.3192 0.096 Uiso 0.50 1 calc PR C 1 C25' C 0.5211(19) 0.4486(11) 0.3063(15) 0.080(3) Uani 0.50 1 d PD C 2 H25C H 0.5014 0.4088 0.2826 0.096 Uiso 0.50 1 calc PR C 2 H25D H 0.5365 0.4344 0.3463 0.096 Uiso 0.50 1 calc PR C 2 C26 C 0.8248(7) 0.5760(4) 0.3084(6) 0.113(3) Uani 1 1 d . C . H26A H 0.8942 0.5477 0.2865 0.170 Uiso 1 1 calc R . . H26B H 0.8582 0.5776 0.3483 0.170 Uiso 1 1 calc R . . H26C H 0.8253 0.6209 0.2924 0.170 Uiso 1 1 calc R . . C27 C 0.2511(8) 0.4592(3) 0.2960(5) 0.092(3) Uani 1 1 d . C . H27A H 0.2480 0.4377 0.2585 0.138 Uiso 1 1 calc R . . H27B H 0.1659 0.4903 0.2994 0.138 Uiso 1 1 calc R . . H27C H 0.2434 0.4254 0.3259 0.138 Uiso 1 1 calc R . . C28 C 0.9037(14) 0.3159(5) 0.3205(6) 0.128(4) Uani 1 1 d . . . H28A H 1.0092 0.3275 0.3315 0.153 Uiso 1 1 calc R . . H28B H 0.8908 0.2674 0.3256 0.153 Uiso 1 1 calc R . . C29 C 0.8796(12) 0.3327(5) 0.2613(6) 0.117(4) Uani 1 1 d . . . H29A H 0.9319 0.3002 0.2364 0.141 Uiso 1 1 calc R . . H29B H 0.7695 0.3316 0.2524 0.141 Uiso 1 1 calc R . . C30 C 0.8337(19) 0.3470(9) 0.4163(6) 0.188(7) Uani 1 1 d . . . H30A H 0.7821 0.3087 0.4333 0.282 Uiso 1 1 calc R . . H30B H 0.8006 0.3877 0.4357 0.282 Uiso 1 1 calc R . . H30C H 0.9440 0.3419 0.4206 0.282 Uiso 1 1 calc R . . C31 C 0.9171(16) 0.4122(8) 0.1933(5) 0.169(6) Uani 1 1 d . . . H31A H 0.9510 0.3755 0.1689 0.254 Uiso 1 1 calc R . . H31B H 0.9781 0.4518 0.1850 0.254 Uiso 1 1 calc R . . H31C H 0.8096 0.4216 0.1856 0.254 Uiso 1 1 calc R . . B1 B 0.1538(5) 0.6600(2) 0.3007(3) 0.0454(13) Uani 1 1 d D . . H1A H 0.173(5) 0.6581(19) 0.2543(6) 0.055 Uiso 1 1 d D . . H1B H 0.142(5) 0.6106(10) 0.3213(14) 0.055 Uiso 1 1 d D . . H1C H 0.234(4) 0.6936(14) 0.3240(15) 0.055 Uiso 1 1 d D . . H1D H 0.043(3) 0.6828(19) 0.291(2) 0.055 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.04190(12) 0.03876(13) 0.04138(13) -0.00209(11) -0.00008(11) -0.00638(10) Si1 0.1227(19) 0.0673(11) 0.0468(10) -0.0092(8) -0.0172(11) -0.0265(12) Si2 0.0882(13) 0.0580(10) 0.0515(10) 0.0037(8) 0.0156(9) -0.0172(9) O1 0.0443(18) 0.058(2) 0.112(4) -0.006(3) 0.001(3) 0.0061(16) O2 0.057(2) 0.0418(19) 0.093(3) -0.006(2) 0.004(2) -0.0080(15) O3 0.139(6) 0.137(6) 0.127(6) 0.036(5) 0.004(5) 0.050(5) O4 0.120(5) 0.128(5) 0.099(5) -0.019(4) -0.019(4) -0.022(4) N1 0.108(4) 0.057(3) 0.039(2) -0.002(3) -0.004(2) -0.015(3) N2 0.083(4) 0.062(3) 0.040(3) -0.007(2) 0.008(2) -0.036(3) N3 0.080(3) 0.054(3) 0.047(2) -0.006(2) 0.000(3) -0.027(2) N4 0.096(4) 0.059(3) 0.040(2) 0.002(2) -0.006(3) -0.036(3) C1 0.078(4) 0.050(3) 0.041(3) -0.003(2) 0.004(3) -0.012(3) C2 0.076(4) 0.057(3) 0.033(3) -0.003(2) 0.002(3) -0.022(3) C3 0.071(4) 0.060(3) 0.046(3) -0.002(3) 0.005(3) -0.031(3) C4 0.087(4) 0.046(3) 0.054(4) -0.012(2) 0.009(3) -0.020(3) C5 0.127(6) 0.072(4) 0.046(4) -0.001(3) -0.007(4) -0.052(4) C6 0.129(3) 0.100(3) 0.062(2) -0.0007(17) -0.001(2) -0.022(2) C7 0.129(3) 0.100(3) 0.062(2) -0.0007(17) -0.001(2) -0.022(2) C8 0.129(3) 0.100(3) 0.062(2) -0.0007(17) -0.001(2) -0.022(2) C9 0.129(3) 0.100(3) 0.062(2) -0.0007(17) -0.001(2) -0.022(2) C10 0.129(3) 0.100(3) 0.062(2) -0.0007(17) -0.001(2) -0.022(2) C11 0.129(3) 0.100(3) 0.062(2) -0.0007(17) -0.001(2) -0.022(2) C12 0.078(4) 0.052(3) 0.042(3) 0.000(3) 0.001(3) -0.009(3) C13 0.100(5) 0.091(5) 0.043(3) -0.005(3) -0.015(4) -0.015(4) C14 0.119(7) 0.113(7) 0.051(4) -0.013(4) -0.005(4) -0.028(6) C15 0.090(5) 0.119(7) 0.062(5) 0.023(5) -0.024(4) -0.035(5) C16 0.086(5) 0.110(7) 0.100(7) 0.046(6) -0.032(5) -0.003(5) C17 0.089(5) 0.078(5) 0.085(5) 0.004(4) -0.010(4) 0.012(4) C24 0.066(5) 0.064(5) 0.098(8) -0.007(7) 0.014(8) 0.020(4) C24' 0.066(5) 0.064(5) 0.098(8) -0.007(7) 0.014(8) 0.020(4) C25 0.083(5) 0.042(4) 0.115(7) 0.004(5) 0.012(5) 0.006(3) C25' 0.083(5) 0.042(4) 0.115(7) 0.004(5) 0.012(5) 0.006(3) C26 0.040(3) 0.100(5) 0.200(11) -0.016(7) -0.002(6) -0.012(3) C27 0.070(4) 0.067(4) 0.139(8) -0.001(5) -0.009(5) -0.033(3) C28 0.126(8) 0.072(5) 0.185(13) 0.024(7) 0.009(9) 0.036(5) C29 0.101(7) 0.090(7) 0.160(12) -0.047(7) 0.003(7) 0.021(5) C30 0.193(14) 0.243(18) 0.127(12) 0.047(12) -0.004(11) 0.054(14) C31 0.163(11) 0.256(17) 0.088(8) -0.009(10) -0.026(9) -0.039(11) B1 0.0204(18) 0.031(2) 0.085(4) -0.003(3) -0.006(3) 0.0031(16) _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 Sm1 N4 2.358(5) . ? Sm1 N2 2.381(5) . ? Sm1 O1 2.486(4) . ? Sm1 N3 2.510(5) . ? Sm1 N1 2.527(5) . ? Sm1 O2 2.562(3) . ? Sm1 B1 2.630(4) . ? Sm1 C2 2.852(5) . ? Sm1 C1 2.875(6) . ? Sm1 H1C 2.36(4) . ? Si1 N1 1.739(5) . ? Si1 C18 1.786(16) . ? Si1 C19' 1.795(14) . ? Si1 C20 1.806(15) . ? Si1 C20' 1.851(14) . ? Si1 C19 1.939(16) . ? Si1 C18' 1.973(15) . ? Si2 N3 1.735(5) . ? Si2 C22 1.802(13) . ? Si2 C21' 1.848(14) . ? Si2 C21 1.854(14) . ? Si2 C23' 1.867(13) . ? Si2 C22' 1.869(13) . ? Si2 C23 1.877(13) . ? O1 C24' 1.371(12) . ? O1 C24 1.385(13) . ? O1 C26 1.399(7) . ? O2 C25 1.440(16) . ? O2 C25' 1.442(16) . ? O2 C27 1.451(7) . ? O3 C30 1.407(15) . ? O3 C28 1.449(13) . ? O4 C29 1.338(12) . ? O4 C31 1.408(14) . ? N1 C1 1.308(8) . ? N2 C1 1.305(7) . ? N2 C3 1.459(7) . ? N3 C2 1.319(7) . ? N4 C2 1.322(7) . ? N4 C5 1.471(8) . ? C1 C6 1.486(10) . ? C2 C12 1.509(8) . ? C3 C4 1.507(8) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.492(9) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C11 1.344(13) . ? C6 C7 1.390(14) . ? C7 C8 1.375(12) . ? C7 H7 0.9400 . ? C8 C9 1.307(12) . ? C8 H8 0.9400 . ? C9 C10 1.296(13) . ? C9 H9 0.9400 . ? C10 C11 1.450(12) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C17 1.350(10) . ? C12 C13 1.384(9) . ? C13 C14 1.382(10) . ? C13 H13 0.9400 . ? C14 C15 1.315(12) . ? C14 H14 0.9400 . ? C15 C16 1.382(13) . ? C15 H15 0.9400 . ? C16 C17 1.412(12) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C18' H18D 0.9700 . ? C18' H18E 0.9700 . ? C18' H18F 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C19' H19D 0.9700 . ? C19' H19E 0.9700 . ? C19' H19F 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C20' H20D 0.9700 . ? C20' H20E 0.9700 . ? C20' H20F 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C21' H21D 0.9700 . ? C21' H21E 0.9700 . ? C21' H21F 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C22' H22D 0.9700 . ? C22' H22E 0.9700 . ? C22' H22F 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C23' H23D 0.9700 . ? C23' H23E 0.9700 . ? C23' H23F 0.9700 . ? C24 C25 1.501(14) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24' C25' 1.499(14) . ? C24' H24C 0.9800 . ? C24' H24D 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25' H25C 0.9800 . ? C25' H25D 0.9800 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 C29 1.429(16) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? B1 H1A 1.089(10) . ? B1 H1B 1.100(9) . ? B1 H1C 1.109(9) . ? B1 H1D 1.093(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Sm1 N2 72.10(17) . . ? N4 Sm1 O1 88.1(2) . . ? N2 Sm1 O1 86.59(18) . . ? N4 Sm1 N3 54.64(15) . . ? N2 Sm1 N3 126.02(15) . . ? O1 Sm1 N3 83.74(19) . . ? N4 Sm1 N1 125.49(18) . . ? N2 Sm1 N1 53.74(16) . . ? O1 Sm1 N1 83.51(19) . . ? N3 Sm1 N1 167.23(18) . . ? N4 Sm1 O2 132.59(17) . . ? N2 Sm1 O2 136.86(17) . . ? O1 Sm1 O2 63.94(12) . . ? N3 Sm1 O2 83.45(16) . . ? N1 Sm1 O2 90.34(17) . . ? N4 Sm1 B1 106.7(2) . . ? N2 Sm1 B1 108.8(2) . . ? O1 Sm1 B1 161.18(14) . . ? N3 Sm1 B1 95.1(2) . . ? N1 Sm1 B1 96.7(2) . . ? O2 Sm1 B1 97.25(13) . . ? N4 Sm1 C2 27.34(15) . . ? N2 Sm1 C2 98.57(17) . . ? O1 Sm1 C2 82.72(19) . . ? N3 Sm1 C2 27.53(14) . . ? N1 Sm1 C2 149.7(2) . . ? O2 Sm1 C2 107.41(16) . . ? B1 Sm1 C2 104.9(2) . . ? N4 Sm1 C1 98.63(16) . . ? N2 Sm1 C1 26.68(15) . . ? O1 Sm1 C1 84.50(18) . . ? N3 Sm1 C1 151.05(17) . . ? N1 Sm1 C1 27.05(16) . . ? O2 Sm1 C1 114.53(16) . . ? B1 Sm1 C1 104.2(2) . . ? C2 Sm1 C1 124.41(17) . . ? N4 Sm1 H1C 82.1(3) . . ? N2 Sm1 H1C 97.3(8) . . ? O1 Sm1 H1C 167.7(7) . . ? N3 Sm1 H1C 84.6(8) . . ? N1 Sm1 H1C 108.2(8) . . ? O2 Sm1 H1C 118.3(6) . . ? B1 Sm1 H1C 24.9(2) . . ? C2 Sm1 H1C 85.2(6) . . ? C1 Sm1 H1C 104.2(9) . . ? N1 Si1 C18 119.2(8) . . ? N1 Si1 C19' 112.1(8) . . ? C18 Si1 C19' 40.1(9) . . ? N1 Si1 C20 108.7(9) . . ? C18 Si1 C20 107.6(11) . . ? C19' Si1 C20 137.5(11) . . ? N1 Si1 C20' 109.1(8) . . ? C18 Si1 C20' 131.8(11) . . ? C19' Si1 C20' 120.7(10) . . ? C20 Si1 C20' 52.8(10) . . ? N1 Si1 C19 107.4(8) . . ? C18 Si1 C19 106.3(11) . . ? C19' Si1 C19 71.6(10) . . ? C20 Si1 C19 107.2(11) . . ? C20' Si1 C19 56.4(10) . . ? N1 Si1 C18' 109.3(8) . . ? C18 Si1 C18' 62.7(10) . . ? C19' Si1 C18' 102.5(10) . . ? C20 Si1 C18' 51.5(10) . . ? C20' Si1 C18' 102.1(9) . . ? C19 Si1 C18' 142.2(10) . . ? N3 Si2 C22 111.5(6) . . ? N3 Si2 C21' 114.8(6) . . ? C22 Si2 C21' 125.4(8) . . ? N3 Si2 C21 115.0(6) . . ? C22 Si2 C21 113.1(8) . . ? C21' Si2 C21 17.9(7) . . ? N3 Si2 C23' 109.7(6) . . ? C22 Si2 C23' 86.8(8) . . ? C21' Si2 C23' 103.0(8) . . ? C21 Si2 C23' 117.5(8) . . ? N3 Si2 C22' 111.3(6) . . ? C22 Si2 C22' 20.6(7) . . ? C21' Si2 C22' 111.6(8) . . ? C21 Si2 C22' 96.4(8) . . ? C23' Si2 C22' 105.7(8) . . ? N3 Si2 C23 106.8(6) . . ? C22 Si2 C23 106.8(8) . . ? C21' Si2 C23 86.1(8) . . ? C21 Si2 C23 102.7(8) . . ? C23' Si2 C23 20.9(7) . . ? C22' Si2 C23 124.2(8) . . ? C24' O1 C24 46.4(9) . . ? C24' O1 C26 117.5(8) . . ? C24 O1 C26 114.3(9) . . ? C24' O1 Sm1 116.6(7) . . ? C24 O1 Sm1 116.4(7) . . ? C26 O1 Sm1 122.4(4) . . ? C25 O2 C25' 7(2) . . ? C25 O2 C27 114.2(10) . . ? C25' O2 C27 110.0(10) . . ? C25 O2 Sm1 116.2(9) . . ? C25' O2 Sm1 120.7(9) . . ? C27 O2 Sm1 129.3(4) . . ? C30 O3 C28 113.5(10) . . ? C29 O4 C31 110.7(10) . . ? C1 N1 Si1 130.9(5) . . ? C1 N1 Sm1 91.5(4) . . ? Si1 N1 Sm1 136.6(3) . . ? C1 N2 C3 121.8(5) . . ? C1 N2 Sm1 98.3(3) . . ? C3 N2 Sm1 139.7(4) . . ? C2 N3 Si2 129.1(4) . . ? C2 N3 Sm1 90.8(3) . . ? Si2 N3 Sm1 139.6(3) . . ? C2 N4 C5 121.5(5) . . ? C2 N4 Sm1 97.6(3) . . ? C5 N4 Sm1 138.7(4) . . ? N2 C1 N1 116.5(5) . . ? N2 C1 C6 121.6(6) . . ? N1 C1 C6 121.9(6) . . ? N2 C1 Sm1 55.0(3) . . ? N1 C1 Sm1 61.5(3) . . ? C6 C1 Sm1 176.4(5) . . ? N3 C2 N4 115.9(5) . . ? N3 C2 C12 121.3(5) . . ? N4 C2 C12 122.8(5) . . ? N3 C2 Sm1 61.6(3) . . ? N4 C2 Sm1 55.0(3) . . ? C12 C2 Sm1 170.6(5) . . ? N2 C3 C4 110.1(5) . . ? N2 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? N2 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? C5 C4 C3 116.4(6) . . ? C5 C4 H4A 108.2 . . ? C3 C4 H4A 108.2 . . ? C5 C4 H4B 108.2 . . ? C3 C4 H4B 108.2 . . ? H4A C4 H4B 107.3 . . ? N4 C5 C4 110.1(6) . . ? N4 C5 H5A 109.6 . . ? C4 C5 H5A 109.6 . . ? N4 C5 H5B 109.6 . . ? C4 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? C11 C6 C7 118.3(9) . . ? C11 C6 C1 123.3(9) . . ? C7 C6 C1 118.4(8) . . ? C8 C7 C6 121.5(10) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C9 C8 C7 117.1(10) . . ? C9 C8 H8 121.5 . . ? C7 C8 H8 121.5 . . ? C10 C9 C8 126.7(10) . . ? C10 C9 H9 116.6 . . ? C8 C9 H9 116.6 . . ? C9 C10 C11 116.9(10) . . ? C9 C10 H10 121.5 . . ? C11 C10 H10 121.5 . . ? C6 C11 C10 119.4(10) . . ? C6 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C17 C12 C13 118.7(7) . . ? C17 C12 C2 121.1(6) . . ? C13 C12 C2 120.2(6) . . ? C14 C13 C12 120.2(8) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 121.5(9) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 120.0(8) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 119.1(7) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C12 C17 C16 120.4(8) . . ? C12 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? Si1 C18' H18D 109.5 . . ? Si1 C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? Si1 C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? Si1 C19' H19D 109.5 . . ? Si1 C19' H19E 109.5 . . ? H19D C19' H19E 109.5 . . ? Si1 C19' H19F 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? Si1 C20' H20D 109.5 . . ? Si1 C20' H20E 109.5 . . ? H20D C20' H20E 109.5 . . ? Si1 C20' H20F 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? Si2 C21' H21D 109.5 . . ? Si2 C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? Si2 C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? Si2 C22' H22D 109.5 . . ? Si2 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? Si2 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? Si2 C23' H23D 109.5 . . ? Si2 C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? Si2 C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? O1 C24 C25 106.2(15) . . ? O1 C24 H24A 110.5 . . ? C25 C24 H24A 110.5 . . ? O1 C24 H24B 110.5 . . ? C25 C24 H24B 110.5 . . ? H24A C24 H24B 108.7 . . ? O1 C24' C25' 115.1(15) . . ? O1 C24' H24C 108.5 . . ? C25' C24' H24C 108.5 . . ? O1 C24' H24D 108.5 . . ? C25' C24' H24D 108.5 . . ? H24C C24' H24D 107.5 . . ? O2 C25 C24 109.7(16) . . ? O2 C25 H25A 109.7 . . ? C24 C25 H25A 109.7 . . ? O2 C25 H25B 109.7 . . ? C24 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? O2 C25' C24' 105.6(15) . . ? O2 C25' H25C 110.6 . . ? C24' C25' H25C 110.6 . . ? O2 C25' H25D 110.6 . . ? C24' C25' H25D 110.6 . . ? H25C C25' H25D 108.8 . . ? O1 C26 H26A 109.5 . . ? O1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O2 C27 H27A 109.5 . . ? O2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 O3 111.1(8) . . ? C29 C28 H28A 109.4 . . ? O3 C28 H28A 109.4 . . ? C29 C28 H28B 109.4 . . ? O3 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? O4 C29 C28 108.9(10) . . ? O4 C29 H29A 109.9 . . ? C28 C29 H29A 109.9 . . ? O4 C29 H29B 109.9 . . ? C28 C29 H29B 109.9 . . ? H29A C29 H29B 108.3 . . ? O3 C30 H30A 109.5 . . ? O3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O4 C31 H31A 109.5 . . ? O4 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O4 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Sm1 B1 H1A 83(3) . . ? Sm1 B1 H1B 80(2) . . ? H1A B1 H1B 114.4(13) . . ? Sm1 B1 H1C 63.6(19) . . ? H1A B1 H1C 113.8(13) . . ? H1B B1 H1C 112.8(13) . . ? Sm1 B1 H1D 167(3) . . ? H1A B1 H1D 87(4) . . ? H1B B1 H1D 112(3) . . ? H1C B1 H1D 114.1(14) . . ? 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 N4 Sm1 O1 C24' 162.8(10) . . . . ? N2 Sm1 O1 C24' -125.0(10) . . . . ? N3 Sm1 O1 C24' 108.2(10) . . . . ? N1 Sm1 O1 C24' -71.1(10) . . . . ? O2 Sm1 O1 C24' 22.4(10) . . . . ? B1 Sm1 O1 C24' 20.6(12) . . . . ? C2 Sm1 O1 C24' 135.9(10) . . . . ? C1 Sm1 O1 C24' -98.3(10) . . . . ? N4 Sm1 O1 C24 110.6(9) . . . . ? N2 Sm1 O1 C24 -177.3(9) . . . . ? N3 Sm1 O1 C24 55.9(9) . . . . ? N1 Sm1 O1 C24 -123.4(9) . . . . ? O2 Sm1 O1 C24 -29.8(9) . . . . ? B1 Sm1 O1 C24 -31.6(12) . . . . ? C2 Sm1 O1 C24 83.6(9) . . . . ? C1 Sm1 O1 C24 -150.6(9) . . . . ? N4 Sm1 O1 C26 -38.6(7) . . . . ? N2 Sm1 O1 C26 33.6(7) . . . . ? N3 Sm1 O1 C26 -93.2(7) . . . . ? N1 Sm1 O1 C26 87.5(8) . . . . ? O2 Sm1 O1 C26 -179.0(8) . . . . ? B1 Sm1 O1 C26 179.3(8) . . . . ? C2 Sm1 O1 C26 -65.5(7) . . . . ? C1 Sm1 O1 C26 60.3(7) . . . . ? N4 Sm1 O2 C25 -62.4(16) . . . . ? N2 Sm1 O2 C25 49.3(16) . . . . ? O1 Sm1 O2 C25 -2.5(15) . . . . ? N3 Sm1 O2 C25 -88.7(16) . . . . ? N1 Sm1 O2 C25 80.1(16) . . . . ? B1 Sm1 O2 C25 177.0(16) . . . . ? C2 Sm1 O2 C25 -74.9(16) . . . . ? C1 Sm1 O2 C25 67.6(16) . . . . ? N4 Sm1 O2 C25' -56.3(17) . . . . ? N2 Sm1 O2 C25' 55.4(17) . . . . ? O1 Sm1 O2 C25' 3.6(17) . . . . ? N3 Sm1 O2 C25' -82.6(17) . . . . ? N1 Sm1 O2 C25' 86.3(17) . . . . ? B1 Sm1 O2 C25' -176.9(17) . . . . ? C2 Sm1 O2 C25' -68.8(17) . . . . ? C1 Sm1 O2 C25' 73.7(17) . . . . ? N4 Sm1 O2 C27 125.2(7) . . . . ? N2 Sm1 O2 C27 -123.1(7) . . . . ? O1 Sm1 O2 C27 -174.9(8) . . . . ? N3 Sm1 O2 C27 98.9(7) . . . . ? N1 Sm1 O2 C27 -92.2(7) . . . . ? B1 Sm1 O2 C27 4.6(7) . . . . ? C2 Sm1 O2 C27 112.7(7) . . . . ? C1 Sm1 O2 C27 -104.7(7) . . . . ? C18 Si1 N1 C1 -9.5(13) . . . . ? C19' Si1 N1 C1 -53.5(11) . . . . ? C20 Si1 N1 C1 114.1(11) . . . . ? C20' Si1 N1 C1 170.2(10) . . . . ? C19 Si1 N1 C1 -130.2(10) . . . . ? C18' Si1 N1 C1 59.4(10) . . . . ? C18 Si1 N1 Sm1 155.4(10) . . . . ? C19' Si1 N1 Sm1 111.4(9) . . . . ? C20 Si1 N1 Sm1 -81.0(10) . . . . ? C20' Si1 N1 Sm1 -25.0(9) . . . . ? C19 Si1 N1 Sm1 34.6(9) . . . . ? C18' Si1 N1 Sm1 -135.8(8) . . . . ? N4 Sm1 N1 C1 -7.7(5) . . . . ? N2 Sm1 N1 C1 -0.1(4) . . . . ? O1 Sm1 N1 C1 -90.6(4) . . . . ? N3 Sm1 N1 C1 -93.7(8) . . . . ? O2 Sm1 N1 C1 -154.3(4) . . . . ? B1 Sm1 N1 C1 108.3(4) . . . . ? C2 Sm1 N1 C1 -27.2(6) . . . . ? N4 Sm1 N1 Si1 -176.3(4) . . . . ? N2 Sm1 N1 Si1 -168.7(6) . . . . ? O1 Sm1 N1 Si1 100.8(5) . . . . ? N3 Sm1 N1 Si1 97.7(9) . . . . ? O2 Sm1 N1 Si1 37.0(5) . . . . ? B1 Sm1 N1 Si1 -60.3(5) . . . . ? C2 Sm1 N1 Si1 164.2(4) . . . . ? C1 Sm1 N1 Si1 -168.6(8) . . . . ? N4 Sm1 N2 C1 173.6(5) . . . . ? O1 Sm1 N2 C1 84.5(4) . . . . ? N3 Sm1 N2 C1 164.3(4) . . . . ? N1 Sm1 N2 C1 0.1(4) . . . . ? O2 Sm1 N2 C1 39.5(6) . . . . ? B1 Sm1 N2 C1 -84.4(5) . . . . ? C2 Sm1 N2 C1 166.6(4) . . . . ? N4 Sm1 N2 C3 -1.3(7) . . . . ? O1 Sm1 N2 C3 -90.3(7) . . . . ? N3 Sm1 N2 C3 -10.6(8) . . . . ? N1 Sm1 N2 C3 -174.8(8) . . . . ? O2 Sm1 N2 C3 -135.3(6) . . . . ? B1 Sm1 N2 C3 100.8(7) . . . . ? C2 Sm1 N2 C3 -8.2(7) . . . . ? C1 Sm1 N2 C3 -174.9(10) . . . . ? C22 Si2 N3 C2 -111.5(8) . . . . ? C21' Si2 N3 C2 38.7(9) . . . . ? C21 Si2 N3 C2 19.0(9) . . . . ? C23' Si2 N3 C2 154.1(8) . . . . ? C22' Si2 N3 C2 -89.3(8) . . . . ? C23 Si2 N3 C2 132.2(8) . . . . ? C22 Si2 N3 Sm1 78.2(8) . . . . ? C21' Si2 N3 Sm1 -131.6(7) . . . . ? C21 Si2 N3 Sm1 -151.3(7) . . . . ? C23' Si2 N3 Sm1 -16.2(8) . . . . ? C22' Si2 N3 Sm1 100.4(7) . . . . ? C23 Si2 N3 Sm1 -38.1(7) . . . . ? N4 Sm1 N3 C2 -5.8(4) . . . . ? N2 Sm1 N3 C2 5.1(5) . . . . ? O1 Sm1 N3 C2 86.3(4) . . . . ? N1 Sm1 N3 C2 89.3(9) . . . . ? O2 Sm1 N3 C2 150.6(4) . . . . ? B1 Sm1 N3 C2 -112.6(4) . . . . ? C1 Sm1 N3 C2 19.7(6) . . . . ? N4 Sm1 N3 Si2 166.7(6) . . . . ? N2 Sm1 N3 Si2 177.6(4) . . . . ? O1 Sm1 N3 Si2 -101.3(5) . . . . ? N1 Sm1 N3 Si2 -98.2(10) . . . . ? O2 Sm1 N3 Si2 -36.9(4) . . . . ? B1 Sm1 N3 Si2 59.9(5) . . . . ? C2 Sm1 N3 Si2 172.5(7) . . . . ? C1 Sm1 N3 Si2 -167.8(4) . . . . ? N2 Sm1 N4 C2 -164.9(5) . . . . ? O1 Sm1 N4 C2 -77.9(5) . . . . ? N3 Sm1 N4 C2 5.8(4) . . . . ? N1 Sm1 N4 C2 -158.5(4) . . . . ? O2 Sm1 N4 C2 -26.8(6) . . . . ? B1 Sm1 N4 C2 90.2(5) . . . . ? C1 Sm1 N4 C2 -162.0(5) . . . . ? N2 Sm1 N4 C5 -2.9(8) . . . . ? O1 Sm1 N4 C5 84.2(8) . . . . ? N3 Sm1 N4 C5 167.9(9) . . . . ? N1 Sm1 N4 C5 3.5(9) . . . . ? O2 Sm1 N4 C5 135.2(7) . . . . ? B1 Sm1 N4 C5 -107.8(8) . . . . ? C2 Sm1 N4 C5 162.0(11) . . . . ? C1 Sm1 N4 C5 0.0(8) . . . . ? C3 N2 C1 N1 175.9(6) . . . . ? Sm1 N2 C1 N1 -0.2(7) . . . . ? C3 N2 C1 C6 -2.4(11) . . . . ? Sm1 N2 C1 C6 -178.5(7) . . . . ? C3 N2 C1 Sm1 176.1(7) . . . . ? Si1 N1 C1 N2 169.8(5) . . . . ? Sm1 N1 C1 N2 0.1(6) . . . . ? Si1 N1 C1 C6 -11.8(11) . . . . ? Sm1 N1 C1 C6 178.5(7) . . . . ? Si1 N1 C1 Sm1 169.7(7) . . . . ? N4 Sm1 C1 N2 -6.2(5) . . . . ? O1 Sm1 C1 N2 -93.4(5) . . . . ? N3 Sm1 C1 N2 -26.9(6) . . . . ? N1 Sm1 C1 N2 -179.8(7) . . . . ? O2 Sm1 C1 N2 -151.4(4) . . . . ? B1 Sm1 C1 N2 103.6(4) . . . . ? C2 Sm1 C1 N2 -16.1(5) . . . . ? N4 Sm1 C1 N1 173.7(4) . . . . ? N2 Sm1 C1 N1 179.8(7) . . . . ? O1 Sm1 C1 N1 86.5(4) . . . . ? N3 Sm1 C1 N1 152.9(4) . . . . ? O2 Sm1 C1 N1 28.4(4) . . . . ? B1 Sm1 C1 N1 -76.6(4) . . . . ? C2 Sm1 C1 N1 163.8(4) . . . . ? N4 Sm1 C1 C6 14(9) . . . . ? N2 Sm1 C1 C6 20(9) . . . . ? O1 Sm1 C1 C6 -73(9) . . . . ? N3 Sm1 C1 C6 -6(9) . . . . ? N1 Sm1 C1 C6 -159(9) . . . . ? O2 Sm1 C1 C6 -131(9) . . . . ? B1 Sm1 C1 C6 124(9) . . . . ? C2 Sm1 C1 C6 4(9) . . . . ? Si2 N3 C2 N4 -164.3(6) . . . . ? Sm1 N3 C2 N4 9.4(6) . . . . ? Si2 N3 C2 C12 16.5(9) . . . . ? Sm1 N3 C2 C12 -169.8(6) . . . . ? Si2 N3 C2 Sm1 -173.7(6) . . . . ? C5 N4 C2 N3 -176.3(7) . . . . ? Sm1 N4 C2 N3 -10.1(7) . . . . ? C5 N4 C2 C12 2.9(11) . . . . ? Sm1 N4 C2 C12 169.0(6) . . . . ? C5 N4 C2 Sm1 -166.2(9) . . . . ? N4 Sm1 C2 N3 169.7(7) . . . . ? N2 Sm1 C2 N3 -175.8(4) . . . . ? O1 Sm1 C2 N3 -90.4(4) . . . . ? N1 Sm1 C2 N3 -154.0(4) . . . . ? O2 Sm1 C2 N3 -30.7(4) . . . . ? B1 Sm1 C2 N3 72.0(4) . . . . ? C1 Sm1 C2 N3 -168.6(4) . . . . ? N2 Sm1 C2 N4 14.5(5) . . . . ? O1 Sm1 C2 N4 99.9(5) . . . . ? N3 Sm1 C2 N4 -169.7(7) . . . . ? N1 Sm1 C2 N4 36.3(7) . . . . ? O2 Sm1 C2 N4 159.7(5) . . . . ? B1 Sm1 C2 N4 -97.6(5) . . . . ? C1 Sm1 C2 N4 21.7(5) . . . . ? N4 Sm1 C2 C12 -80(2) . . . . ? N2 Sm1 C2 C12 -65(2) . . . . ? O1 Sm1 C2 C12 20(2) . . . . ? N3 Sm1 C2 C12 111(2) . . . . ? N1 Sm1 C2 C12 -43(3) . . . . ? O2 Sm1 C2 C12 80(2) . . . . ? B1 Sm1 C2 C12 -177(2) . . . . ? C1 Sm1 C2 C12 -58(2) . . . . ? C1 N2 C3 C4 160.7(7) . . . . ? Sm1 N2 C3 C4 -25.3(10) . . . . ? N2 C3 C4 C5 62.9(8) . . . . ? C2 N4 C5 C4 -167.9(7) . . . . ? Sm1 N4 C5 C4 33.2(12) . . . . ? C3 C4 C5 N4 -66.6(9) . . . . ? N2 C1 C6 C11 -82.0(11) . . . . ? N1 C1 C6 C11 99.7(10) . . . . ? Sm1 C1 C6 C11 -102(9) . . . . ? N2 C1 C6 C7 99.2(9) . . . . ? N1 C1 C6 C7 -79.1(11) . . . . ? Sm1 C1 C6 C7 79(9) . . . . ? C11 C6 C7 C8 -2.8(13) . . . . ? C1 C6 C7 C8 176.0(8) . . . . ? C6 C7 C8 C9 2.8(13) . . . . ? C7 C8 C9 C10 -2.1(14) . . . . ? C8 C9 C10 C11 1.4(14) . . . . ? C7 C6 C11 C10 2.1(13) . . . . ? C1 C6 C11 C10 -176.7(7) . . . . ? C9 C10 C11 C6 -1.4(13) . . . . ? N3 C2 C12 C17 72.9(9) . . . . ? N4 C2 C12 C17 -106.2(8) . . . . ? Sm1 C2 C12 C17 -33(3) . . . . ? N3 C2 C12 C13 -107.0(7) . . . . ? N4 C2 C12 C13 73.9(9) . . . . ? Sm1 C2 C12 C13 147(2) . . . . ? C17 C12 C13 C14 -2.7(11) . . . . ? C2 C12 C13 C14 177.2(7) . . . . ? C12 C13 C14 C15 3.3(12) . . . . ? C13 C14 C15 C16 -2.6(13) . . . . ? C14 C15 C16 C17 1.5(13) . . . . ? C13 C12 C17 C16 1.6(11) . . . . ? C2 C12 C17 C16 -178.2(7) . . . . ? C15 C16 C17 C12 -1.0(12) . . . . ? C24' O1 C24 C25 -46.7(16) . . . . ? C26 O1 C24 C25 -152.4(13) . . . . ? Sm1 O1 C24 C25 56.0(15) . . . . ? C24 O1 C24' C25' 54.8(19) . . . . ? C26 O1 C24' C25' 153.1(16) . . . . ? Sm1 O1 C24' C25' -47.2(19) . . . . ? C25' O2 C25 C24 -101(19) . . . . ? C27 O2 C25 C24 -156.0(15) . . . . ? Sm1 O2 C25 C24 30(3) . . . . ? O1 C24 C25 O2 -55(2) . . . . ? C25 O2 C25' C24' 26(16) . . . . ? C27 O2 C25' C24' 153.7(16) . . . . ? Sm1 O2 C25' C24' -25(3) . . . . ? O1 C24' C25' O2 46(3) . . . . ? C30 O3 C28 C29 -168.1(12) . . . . ? C31 O4 C29 C28 178.6(10) . . . . ? O3 C28 C29 O4 75.0(12) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.106 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.091 # Attachment 'shelxl (4).cif' data_shelxl4 _database_code_depnum_ccdc_archive 'CCDC 843492' #TrackingRef 'shelxl (4).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H48 B N4 O2 Si2 Yb, C4 H10 O2' _chemical_formula_sum 'C31 H58 B N4 O4 Si2 Yb' _chemical_formula_weight 790.84 _chemical_absolute_configuration ad 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 8.6469(12) _cell_length_b 19.790(3) _cell_length_c 23.214(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3972.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 13975 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 2.450 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.295 _exptl_absorpt_correction_T_max 0.504 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16387 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0998 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.47 _reflns_number_total 8853 _reflns_number_gt 7566 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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. ; _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^)+(0.0268P)^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 0.027(11) _refine_ls_number_reflns 8853 _refine_ls_number_parameters 369 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.0823 _refine_ls_wR_factor_gt 0.0776 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.959 _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 Yb1 Yb 0.54798(3) 0.374625(15) 0.695825(11) 0.03353(7) Uani 1 1 d . A . Si1 Si 0.5969(3) 0.42124(12) 0.85927(8) 0.0605(7) Uani 1 1 d D . . Si2 Si 0.6454(3) 0.44314(11) 0.54047(8) 0.0544(5) Uani 1 1 d . . . O1 O 0.3208(4) 0.4411(2) 0.6946(2) 0.0549(12) Uani 1 1 d . . . O2 O 0.5985(5) 0.4969(2) 0.7008(2) 0.0529(12) Uani 1 1 d . . . O3 O 0.1985(10) 0.6444(4) 0.6420(3) 0.128(3) Uani 1 1 d . . . O4 O 0.0637(8) 0.6020(4) 0.7485(3) 0.106(2) Uani 1 1 d . . . N1 N 0.5167(6) 0.3798(3) 0.8009(2) 0.0494(13) Uani 1 1 d . A . N2 N 0.4059(6) 0.2985(3) 0.74882(19) 0.0462(15) Uani 1 1 d . A . N3 N 0.5523(7) 0.3954(2) 0.59228(19) 0.0405(12) Uani 1 1 d . A . N4 N 0.4335(8) 0.3064(3) 0.6297(2) 0.0497(15) Uani 1 1 d . A . C1 C 0.4278(7) 0.3258(3) 0.7993(3) 0.0411(14) Uani 1 1 d . . . C2 C 0.4579(9) 0.3445(3) 0.5847(2) 0.0462(16) Uani 1 1 d . . . C3 C 0.3075(8) 0.2402(4) 0.7375(3) 0.0539(19) Uani 1 1 d . . . H3A H 0.1994 0.2551 0.7365 0.065 Uiso 1 1 calc R A . H3B H 0.3185 0.2080 0.7693 0.065 Uiso 1 1 calc R . . C4 C 0.3442(9) 0.2056(3) 0.6829(3) 0.060(2) Uani 1 1 d . A . H4A H 0.2799 0.1650 0.6798 0.071 Uiso 1 1 calc R . . H4B H 0.4525 0.1911 0.6838 0.071 Uiso 1 1 calc R . . C5 C 0.3191(9) 0.2484(4) 0.6305(3) 0.058(2) Uani 1 1 d . . . H5A H 0.2134 0.2663 0.6306 0.070 Uiso 1 1 calc R A . H5B H 0.3322 0.2209 0.5957 0.070 Uiso 1 1 calc R . . C6 C 0.3559(12) 0.2974(5) 0.8511(3) 0.0823(12) Uani 1 1 d . A . C7 C 0.2226(11) 0.3263(5) 0.8728(3) 0.0823(12) Uani 1 1 d . . . H7 H 0.1782 0.3625 0.8524 0.099 Uiso 1 1 calc R A . C8 C 0.1492(11) 0.3044(5) 0.9240(3) 0.0823(12) Uani 1 1 d . A . H8 H 0.0635 0.3268 0.9401 0.099 Uiso 1 1 calc R . . C9 C 0.2127(11) 0.2486(5) 0.9480(3) 0.0823(12) Uani 1 1 d . . . H9 H 0.1620 0.2300 0.9801 0.099 Uiso 1 1 calc R A . C10 C 0.3392(11) 0.2179(5) 0.9302(3) 0.0823(12) Uani 1 1 d . A . H10 H 0.3811 0.1814 0.9510 0.099 Uiso 1 1 calc R . . C11 C 0.4098(11) 0.2412(5) 0.8793(3) 0.0823(12) Uani 1 1 d . . . H11 H 0.4956 0.2179 0.8644 0.099 Uiso 1 1 calc R A . C12 C 0.3771(8) 0.3297(4) 0.5283(3) 0.0474(17) Uani 1 1 d . A . C13 C 0.4222(10) 0.2750(4) 0.4941(3) 0.064(2) Uani 1 1 d . . . H13 H 0.4979 0.2447 0.5074 0.077 Uiso 1 1 calc R A . C14 C 0.3536(11) 0.2656(5) 0.4397(3) 0.076(3) Uani 1 1 d . A . H14 H 0.3873 0.2301 0.4159 0.091 Uiso 1 1 calc R . . C15 C 0.2390(11) 0.3074(6) 0.4211(4) 0.084(3) Uani 1 1 d . . . H15 H 0.1897 0.2997 0.3857 0.101 Uiso 1 1 calc R A . C16 C 0.1972(10) 0.3605(6) 0.4548(4) 0.084(3) Uani 1 1 d . A . H16 H 0.1195 0.3898 0.4414 0.101 Uiso 1 1 calc R . . C17 C 0.2646(8) 0.3737(5) 0.5086(3) 0.065(2) Uani 1 1 d . . . H17 H 0.2343 0.4113 0.5306 0.078 Uiso 1 1 calc R A . C18 C 0.621(2) 0.3717(11) 0.9257(7) 0.103(3) Uiso 0.50 1 d PD A 1 H18A H 0.5216 0.3542 0.9379 0.155 Uiso 0.50 1 calc PR A 1 H18B H 0.6634 0.4004 0.9557 0.155 Uiso 0.50 1 calc PR A 1 H18C H 0.6914 0.3344 0.9185 0.155 Uiso 0.50 1 calc PR A 1 C18' C 0.532(3) 0.4016(11) 0.9300(6) 0.103(3) Uiso 0.50 1 d PD A 2 H18D H 0.4281 0.4190 0.9354 0.155 Uiso 0.50 1 calc PR A 2 H18E H 0.6008 0.4221 0.9580 0.155 Uiso 0.50 1 calc PR A 2 H18F H 0.5317 0.3530 0.9353 0.155 Uiso 0.50 1 calc PR A 2 C19 C 0.8065(17) 0.4467(11) 0.8379(9) 0.103(3) Uiso 0.50 1 d PD A 1 H19A H 0.8665 0.4064 0.8299 0.155 Uiso 0.50 1 calc PR A 1 H19B H 0.8540 0.4714 0.8694 0.155 Uiso 0.50 1 calc PR A 1 H19C H 0.8036 0.4751 0.8039 0.155 Uiso 0.50 1 calc PR A 1 C19' C 0.8076(17) 0.4110(11) 0.8625(8) 0.103(3) Uiso 0.50 1 d PD A 2 H19D H 0.8322 0.3660 0.8764 0.155 Uiso 0.50 1 calc PR A 2 H19E H 0.8509 0.4444 0.8885 0.155 Uiso 0.50 1 calc PR A 2 H19F H 0.8511 0.4171 0.8244 0.155 Uiso 0.50 1 calc PR A 2 C20 C 0.485(2) 0.4966(9) 0.8765(8) 0.103(3) Uiso 0.50 1 d PD A 1 H20A H 0.4995 0.5300 0.8464 0.155 Uiso 0.50 1 calc PR A 1 H20B H 0.5205 0.5149 0.9130 0.155 Uiso 0.50 1 calc PR A 1 H20C H 0.3767 0.4849 0.8794 0.155 Uiso 0.50 1 calc PR A 1 C20' C 0.571(3) 0.5152(7) 0.8506(8) 0.103(3) Uiso 0.50 1 d PD A 2 H20D H 0.4646 0.5272 0.8588 0.155 Uiso 0.50 1 calc PR A 2 H20E H 0.5965 0.5281 0.8114 0.155 Uiso 0.50 1 calc PR A 2 H20F H 0.6390 0.5386 0.8772 0.155 Uiso 0.50 1 calc PR A 2 C21 C 0.6713(11) 0.4007(5) 0.4694(3) 0.089(3) Uani 1 1 d . . . H21A H 0.6943 0.3533 0.4754 0.133 Uiso 1 1 calc R . . H21B H 0.7559 0.4219 0.4488 0.133 Uiso 1 1 calc R . . H21C H 0.5769 0.4050 0.4471 0.133 Uiso 1 1 calc R . . C22 C 0.5450(14) 0.5267(4) 0.5299(4) 0.110(3) Uani 1 1 d . . . H22A H 0.4415 0.5190 0.5151 0.165 Uiso 1 1 calc R . . H22B H 0.6030 0.5539 0.5026 0.165 Uiso 1 1 calc R . . H22C H 0.5387 0.5502 0.5664 0.165 Uiso 1 1 calc R . . C23 C 0.8457(11) 0.4609(6) 0.5645(4) 0.119(4) Uani 1 1 d . . . H23A H 0.8516 0.4569 0.6061 0.178 Uiso 1 1 calc R . . H23B H 0.8745 0.5063 0.5531 0.178 Uiso 1 1 calc R . . H23C H 0.9158 0.4287 0.5469 0.178 Uiso 1 1 calc R . . C24 C 0.3318(9) 0.5054(4) 0.6782(4) 0.0783(17) Uani 1 1 d . . . H24A H 0.2401 0.5295 0.6921 0.094 Uiso 1 1 calc R . . H24B H 0.3298 0.5069 0.6360 0.094 Uiso 1 1 calc R . . C25 C 0.4687(9) 0.5415(4) 0.6980(4) 0.0783(17) Uani 1 1 d . . . H25A H 0.4914 0.5788 0.6716 0.094 Uiso 1 1 calc R . . H25B H 0.4490 0.5606 0.7363 0.094 Uiso 1 1 calc R . . C26 C 0.1702(7) 0.4141(4) 0.6947(5) 0.096(3) Uani 1 1 d . . . H26A H 0.0996 0.4463 0.7121 0.144 Uiso 1 1 calc R . . H26B H 0.1690 0.3724 0.7166 0.144 Uiso 1 1 calc R . . H26C H 0.1382 0.4051 0.6554 0.144 Uiso 1 1 calc R . . C27 C 0.7421(8) 0.5335(4) 0.7075(4) 0.070(2) Uani 1 1 d . . . H27A H 0.7607 0.5608 0.6735 0.106 Uiso 1 1 calc R . . H27B H 0.8264 0.5017 0.7125 0.106 Uiso 1 1 calc R . . H27C H 0.7355 0.5625 0.7411 0.106 Uiso 1 1 calc R . . C28 C 0.0923(14) 0.6820(6) 0.6769(6) 0.124(5) Uani 1 1 d . . . H28A H 0.1083 0.7305 0.6711 0.149 Uiso 1 1 calc R . . H28B H -0.0143 0.6711 0.6660 0.149 Uiso 1 1 calc R . . C29 C 0.1174(13) 0.6650(6) 0.7361(6) 0.119(5) Uani 1 1 d . . . H29A H 0.2284 0.6672 0.7446 0.143 Uiso 1 1 calc R . . H29B H 0.0649 0.6981 0.7607 0.143 Uiso 1 1 calc R . . C30 C 0.1676(16) 0.6488(7) 0.5836(5) 0.175(7) Uani 1 1 d . . . H30A H 0.1499 0.6957 0.5733 0.263 Uiso 1 1 calc R . . H30B H 0.0763 0.6224 0.5746 0.263 Uiso 1 1 calc R . . H30C H 0.2551 0.6315 0.5620 0.263 Uiso 1 1 calc R . . C31 C 0.0881(14) 0.5850(7) 0.8077(4) 0.166(6) Uani 1 1 d . . . H31A H 0.1959 0.5733 0.8136 0.249 Uiso 1 1 calc R . . H31B H 0.0234 0.5468 0.8180 0.249 Uiso 1 1 calc R . . H31C H 0.0616 0.6234 0.8317 0.249 Uiso 1 1 calc R . . B1 B 0.8264(6) 0.3361(3) 0.7002(3) 0.0331(15) Uani 1 1 d D . . H1A H 0.774(5) 0.3132(19) 0.7386(11) 0.040 Uiso 1 1 d D . . H1B H 0.834(5) 0.3916(6) 0.7030(16) 0.040 Uiso 1 1 d D . . H1C H 0.772(4) 0.3186(18) 0.6596(10) 0.040 Uiso 1 1 d D . . H1D H 0.945(2) 0.318(2) 0.7062(16) 0.040 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.03368(12) 0.03272(12) 0.03419(11) -0.00272(14) 0.00081(12) -0.00556(14) Si1 0.0832(19) 0.0583(15) 0.0399(10) -0.0122(10) -0.0082(10) -0.0147(12) Si2 0.0658(13) 0.0511(14) 0.0464(11) 0.0052(9) 0.0110(10) -0.0116(11) O1 0.033(2) 0.043(3) 0.089(3) 0.015(3) 0.005(3) 0.0082(19) O2 0.050(3) 0.036(3) 0.073(3) -0.001(3) -0.001(3) -0.013(2) O3 0.151(7) 0.114(8) 0.121(6) 0.035(5) 0.020(5) 0.042(6) O4 0.115(5) 0.107(7) 0.096(5) -0.017(4) -0.003(5) -0.037(5) N1 0.079(4) 0.042(3) 0.028(2) -0.005(3) -0.004(3) -0.016(3) N2 0.065(4) 0.043(3) 0.030(3) 0.000(2) 0.001(3) -0.033(3) N3 0.048(3) 0.040(3) 0.034(2) -0.002(2) 0.000(3) -0.011(3) N4 0.082(4) 0.036(3) 0.031(3) -0.003(2) -0.001(3) -0.025(3) C1 0.044(4) 0.051(4) 0.028(3) 0.001(3) -0.001(3) -0.002(3) C2 0.051(4) 0.056(4) 0.032(3) -0.003(3) 0.005(4) -0.010(4) C3 0.064(5) 0.048(5) 0.050(4) 0.000(4) -0.007(4) -0.029(4) C4 0.081(5) 0.034(4) 0.064(5) -0.009(3) 0.011(4) -0.030(4) C5 0.073(5) 0.060(5) 0.042(4) 0.001(3) -0.005(4) -0.033(4) C6 0.102(3) 0.089(3) 0.056(2) 0.008(2) -0.001(2) -0.014(2) C7 0.102(3) 0.089(3) 0.056(2) 0.008(2) -0.001(2) -0.014(2) C8 0.102(3) 0.089(3) 0.056(2) 0.008(2) -0.001(2) -0.014(2) C9 0.102(3) 0.089(3) 0.056(2) 0.008(2) -0.001(2) -0.014(2) C10 0.102(3) 0.089(3) 0.056(2) 0.008(2) -0.001(2) -0.014(2) C11 0.102(3) 0.089(3) 0.056(2) 0.008(2) -0.001(2) -0.014(2) C12 0.056(4) 0.053(5) 0.033(3) -0.002(3) -0.007(3) -0.004(4) C13 0.096(7) 0.058(5) 0.038(3) -0.006(3) -0.004(4) -0.010(5) C14 0.114(7) 0.084(7) 0.030(4) -0.003(4) -0.001(4) -0.028(6) C15 0.085(7) 0.112(9) 0.055(5) 0.026(6) -0.024(5) -0.031(6) C16 0.067(5) 0.100(9) 0.085(6) 0.040(6) -0.028(5) -0.011(6) C17 0.060(4) 0.069(5) 0.066(4) 0.003(5) -0.017(4) 0.016(5) C21 0.122(8) 0.079(7) 0.067(5) -0.007(5) 0.044(5) -0.019(6) C22 0.161(9) 0.057(6) 0.112(7) 0.035(5) 0.030(8) 0.007(7) C23 0.114(8) 0.143(12) 0.099(7) 0.024(7) 0.028(6) -0.055(8) C24 0.061(4) 0.049(4) 0.125(5) -0.007(4) 0.005(4) 0.009(3) C25 0.061(4) 0.049(4) 0.125(5) -0.007(4) 0.005(4) 0.009(3) C26 0.026(4) 0.077(6) 0.185(9) 0.012(7) -0.005(6) -0.003(4) C27 0.053(4) 0.055(5) 0.103(7) -0.025(5) -0.001(4) -0.019(4) C28 0.126(11) 0.069(8) 0.177(13) 0.021(8) -0.016(10) 0.033(7) C29 0.088(8) 0.080(9) 0.190(13) -0.070(10) -0.009(9) 0.009(7) C30 0.206(14) 0.22(2) 0.096(8) 0.055(10) 0.017(9) 0.058(13) C31 0.167(13) 0.250(18) 0.080(7) -0.011(9) -0.021(8) -0.060(11) B1 0.008(3) 0.031(3) 0.060(4) 0.005(4) -0.010(3) 0.000(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 Yb1 N4 2.272(5) . ? Yb1 N2 2.300(5) . ? Yb1 O1 2.364(4) . ? Yb1 N3 2.439(4) . ? Yb1 N1 2.455(5) . ? Yb1 O2 2.461(4) . ? Yb1 B1 2.527(5) . ? Yb1 C2 2.760(6) . ? Yb1 C1 2.790(6) . ? Yb1 H1A 2.50(5) . ? Yb1 H1B 2.50(4) . ? Yb1 H1C 2.39(4) . ? Si1 N1 1.730(5) . ? Si1 C18' 1.779(14) . ? Si1 C20 1.820(14) . ? Si1 C19' 1.835(14) . ? Si1 C18 1.839(14) . ? Si1 C20' 1.883(14) . ? Si1 C19 1.946(14) . ? Si2 N3 1.728(5) . ? Si2 C23 1.853(10) . ? Si2 C21 1.864(8) . ? Si2 C22 1.884(9) . ? O1 C24 1.331(8) . ? O1 C26 1.408(7) . ? O2 C25 1.430(8) . ? O2 C27 1.446(7) . ? O3 C30 1.384(11) . ? O3 C28 1.434(12) . ? O4 C29 1.362(12) . ? O4 C31 1.431(11) . ? N1 C1 1.318(7) . ? N2 C1 1.303(7) . ? N2 C3 1.457(8) . ? N3 C2 1.309(8) . ? N4 C2 1.305(7) . ? N4 C5 1.515(8) . ? C1 C6 1.466(10) . ? C2 C12 1.511(9) . ? C3 C4 1.477(9) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.499(9) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C11 1.372(12) . ? C6 C7 1.381(13) . ? C7 C8 1.417(10) . ? C7 H7 0.9400 . ? C8 C9 1.353(12) . ? C8 H8 0.9400 . ? C9 C10 1.317(12) . ? C9 H9 0.9400 . ? C10 C11 1.409(10) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C17 1.384(10) . ? C12 C13 1.397(9) . ? C13 C14 1.409(9) . ? C13 H13 0.9400 . ? C14 C15 1.361(13) . ? C14 H14 0.9400 . ? C15 C16 1.359(13) . ? C15 H15 0.9400 . ? C16 C17 1.403(10) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C18' H18D 0.9700 . ? C18' H18E 0.9700 . ? C18' H18F 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C19' H19D 0.9700 . ? C19' H19E 0.9700 . ? C19' H19F 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C20' H20D 0.9700 . ? C20' H20E 0.9700 . ? C20' H20F 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C25 1.457(10) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 C29 1.431(14) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? B1 H1A 1.099(10) . ? B1 H1B 1.102(9) . ? B1 H1C 1.107(9) . ? B1 H1D 1.092(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Yb1 N2 74.91(18) . . ? N4 Yb1 O1 87.8(2) . . ? N2 Yb1 O1 85.79(18) . . ? N4 Yb1 N3 55.99(17) . . ? N2 Yb1 N3 130.22(17) . . ? O1 Yb1 N3 84.69(19) . . ? N4 Yb1 N1 130.39(18) . . ? N2 Yb1 N1 55.75(17) . . ? O1 Yb1 N1 84.08(19) . . ? N3 Yb1 N1 166.75(17) . . ? N4 Yb1 O2 133.87(18) . . ? N2 Yb1 O2 135.51(18) . . ? O1 Yb1 O2 66.49(14) . . ? N3 Yb1 O2 82.96(16) . . ? N1 Yb1 O2 86.12(17) . . ? N4 Yb1 B1 105.3(2) . . ? N2 Yb1 B1 106.9(2) . . ? O1 Yb1 B1 163.68(18) . . ? N3 Yb1 B1 94.4(2) . . ? N1 Yb1 B1 94.4(2) . . ? O2 Yb1 B1 97.20(17) . . ? N4 Yb1 C2 27.96(18) . . ? N2 Yb1 C2 101.98(19) . . ? O1 Yb1 C2 82.8(2) . . ? N3 Yb1 C2 28.31(17) . . ? N1 Yb1 C2 155.0(2) . . ? O2 Yb1 C2 107.84(18) . . ? B1 Yb1 C2 104.0(2) . . ? N4 Yb1 C1 102.33(19) . . ? N2 Yb1 C1 27.58(17) . . ? O1 Yb1 C1 83.88(17) . . ? N3 Yb1 C1 155.86(19) . . ? N1 Yb1 C1 28.18(16) . . ? O2 Yb1 C1 111.52(18) . . ? B1 Yb1 C1 102.5(2) . . ? C2 Yb1 C1 128.6(2) . . ? N4 Yb1 H1A 108.6(9) . . ? N2 Yb1 H1A 83.5(5) . . ? O1 Yb1 H1A 157.2(7) . . ? N3 Yb1 H1A 117.4(6) . . ? N1 Yb1 H1A 73.3(6) . . ? O2 Yb1 H1A 108.7(8) . . ? B1 Yb1 H1A 25.2(3) . . ? C2 Yb1 H1A 119.0(8) . . ? C1 Yb1 H1A 77.3(4) . . ? N4 Yb1 H1B 123.8(7) . . ? N2 Yb1 H1B 125.5(7) . . ? O1 Yb1 H1B 138.4(4) . . ? N3 Yb1 H1B 91.6(9) . . ? N1 Yb1 H1B 92.1(9) . . ? O2 Yb1 H1B 71.9(4) . . ? B1 Yb1 H1B 25.3(3) . . ? C2 Yb1 H1B 111.7(8) . . ? C1 Yb1 H1B 111.0(8) . . ? H1A Yb1 H1B 43.0(5) . . ? N4 Yb1 H1C 80.8(4) . . ? N2 Yb1 H1C 108.6(10) . . ? O1 Yb1 H1C 158.4(7) . . ? N3 Yb1 H1C 73.7(6) . . ? N1 Yb1 H1C 117.3(6) . . ? O2 Yb1 H1C 109.2(9) . . ? B1 Yb1 H1C 25.8(2) . . ? C2 Yb1 H1C 78.5(4) . . ? C1 Yb1 H1C 116.4(8) . . ? H1A Yb1 H1C 44.0(5) . . ? H1B Yb1 H1C 44.1(5) . . ? N1 Si1 C18' 119.6(8) . . ? N1 Si1 C20 110.4(7) . . ? C18' Si1 C20 79.0(9) . . ? N1 Si1 C19' 112.2(7) . . ? C18' Si1 C19' 104.5(10) . . ? C20 Si1 C19' 127.4(10) . . ? N1 Si1 C18 116.8(7) . . ? C18' Si1 C18 31.3(8) . . ? C20 Si1 C18 108.2(9) . . ? C19' Si1 C18 78.0(8) . . ? N1 Si1 C20' 109.7(6) . . ? C18' Si1 C20' 106.1(9) . . ? C20 Si1 C20' 32.0(8) . . ? C19' Si1 C20' 103.4(10) . . ? C18 Si1 C20' 129.0(9) . . ? N1 Si1 C19 107.3(7) . . ? C18' Si1 C19 125.8(10) . . ? C20 Si1 C19 109.7(10) . . ? C19' Si1 C19 27.6(8) . . ? C18 Si1 C19 104.2(9) . . ? C20' Si1 C19 80.0(10) . . ? N3 Si2 C23 109.2(4) . . ? N3 Si2 C21 115.2(3) . . ? C23 Si2 C21 103.9(4) . . ? N3 Si2 C22 110.8(4) . . ? C23 Si2 C22 107.7(5) . . ? C21 Si2 C22 109.6(4) . . ? C24 O1 C26 115.4(6) . . ? C24 O1 Yb1 118.4(4) . . ? C26 O1 Yb1 123.9(4) . . ? C25 O2 C27 111.7(5) . . ? C25 O2 Yb1 117.7(4) . . ? C27 O2 Yb1 130.5(4) . . ? C30 O3 C28 113.4(9) . . ? C29 O4 C31 111.6(9) . . ? C1 N1 Si1 129.8(5) . . ? C1 N1 Yb1 90.2(4) . . ? Si1 N1 Yb1 138.9(3) . . ? C1 N2 C3 125.0(5) . . ? C1 N2 Yb1 97.6(4) . . ? C3 N2 Yb1 137.2(4) . . ? C2 N3 Si2 128.1(4) . . ? C2 N3 Yb1 89.6(4) . . ? Si2 N3 Yb1 141.7(3) . . ? C2 N4 C5 123.5(6) . . ? C2 N4 Yb1 97.3(4) . . ? C5 N4 Yb1 136.6(4) . . ? N2 C1 N1 116.4(6) . . ? N2 C1 C6 121.2(6) . . ? N1 C1 C6 122.3(6) . . ? N2 C1 Yb1 54.8(3) . . ? N1 C1 Yb1 61.7(3) . . ? C6 C1 Yb1 175.8(5) . . ? N4 C2 N3 115.9(6) . . ? N4 C2 C12 120.4(6) . . ? N3 C2 C12 123.7(6) . . ? N4 C2 Yb1 54.7(3) . . ? N3 C2 Yb1 62.1(3) . . ? C12 C2 Yb1 168.8(5) . . ? N2 C3 C4 113.4(6) . . ? N2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? N2 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C3 C4 C5 113.8(6) . . ? C3 C4 H4A 108.8 . . ? C5 C4 H4A 108.8 . . ? C3 C4 H4B 108.8 . . ? C5 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C4 C5 N4 110.1(5) . . ? C4 C5 H5A 109.6 . . ? N4 C5 H5A 109.6 . . ? C4 C5 H5B 109.6 . . ? N4 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? C11 C6 C7 116.4(9) . . ? C11 C6 C1 123.9(9) . . ? C7 C6 C1 119.6(9) . . ? C6 C7 C8 123.6(9) . . ? C6 C7 H7 118.2 . . ? C8 C7 H7 118.2 . . ? C9 C8 C7 114.4(9) . . ? C9 C8 H8 122.8 . . ? C7 C8 H8 122.8 . . ? C10 C9 C8 125.8(9) . . ? C10 C9 H9 117.1 . . ? C8 C9 H9 117.1 . . ? C9 C10 C11 118.1(10) . . ? C9 C10 H10 121.0 . . ? C11 C10 H10 121.0 . . ? C6 C11 C10 121.3(10) . . ? C6 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C17 C12 C13 119.7(6) . . ? C17 C12 C2 119.3(7) . . ? C13 C12 C2 120.9(7) . . ? C12 C13 C14 119.7(8) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 120.6(9) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C16 C15 C14 118.9(8) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C15 C16 C17 123.0(9) . . ? C15 C16 H16 118.5 . . ? C17 C16 H16 118.5 . . ? C12 C17 C16 118.0(8) . . ? C12 C17 H17 121.0 . . ? C16 C17 H17 121.0 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? Si1 C18' H18D 109.5 . . ? Si1 C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? Si1 C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? Si1 C19' H19D 109.5 . . ? Si1 C19' H19E 109.5 . . ? H19D C19' H19E 109.5 . . ? Si1 C19' H19F 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? Si1 C20' H20D 109.5 . . ? Si1 C20' H20E 109.5 . . ? H20D C20' H20E 109.5 . . ? Si1 C20' H20F 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O1 C24 C25 115.9(7) . . ? O1 C24 H24A 108.3 . . ? C25 C24 H24A 108.3 . . ? O1 C24 H24B 108.3 . . ? C25 C24 H24B 108.3 . . ? H24A C24 H24B 107.4 . . ? O2 C25 C24 110.4(6) . . ? O2 C25 H25A 109.6 . . ? C24 C25 H25A 109.6 . . ? O2 C25 H25B 109.6 . . ? C24 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? O1 C26 H26A 109.5 . . ? O1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O2 C27 H27A 109.5 . . ? O2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 O3 108.9(9) . . ? C29 C28 H28A 109.9 . . ? O3 C28 H28A 109.9 . . ? C29 C28 H28B 109.9 . . ? O3 C28 H28B 109.9 . . ? H28A C28 H28B 108.3 . . ? O4 C29 C28 111.5(11) . . ? O4 C29 H29A 109.3 . . ? C28 C29 H29A 109.3 . . ? O4 C29 H29B 109.3 . . ? C28 C29 H29B 109.3 . . ? H29A C29 H29B 108.0 . . ? O3 C30 H30A 109.5 . . ? O3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O4 C31 H31A 109.5 . . ? O4 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O4 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Yb1 B1 H1A 76(2) . . ? Yb1 B1 H1B 76(2) . . ? H1A B1 H1B 113.0(13) . . ? Yb1 B1 H1C 70.0(19) . . ? H1A B1 H1C 112.6(12) . . ? H1B B1 H1C 112.8(12) . . ? Yb1 B1 H1D 175(2) . . ? H1A B1 H1D 99(3) . . ? H1B B1 H1D 105(3) . . ? H1C B1 H1D 113.5(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Yb1 O1 C24 -118.8(6) . . . . ? N2 Yb1 O1 C24 166.1(6) . . . . ? N3 Yb1 O1 C24 -62.8(6) . . . . ? N1 Yb1 O1 C24 110.2(6) . . . . ? O2 Yb1 O1 C24 21.8(6) . . . . ? B1 Yb1 O1 C24 24.6(11) . . . . ? C2 Yb1 O1 C24 -91.2(6) . . . . ? C1 Yb1 O1 C24 138.5(6) . . . . ? N4 Yb1 O1 C26 43.0(7) . . . . ? N2 Yb1 O1 C26 -32.0(7) . . . . ? N3 Yb1 O1 C26 99.1(7) . . . . ? N1 Yb1 O1 C26 -88.0(7) . . . . ? O2 Yb1 O1 C26 -176.3(7) . . . . ? B1 Yb1 O1 C26 -173.5(8) . . . . ? C2 Yb1 O1 C26 70.6(7) . . . . ? C1 Yb1 O1 C26 -59.6(7) . . . . ? N4 Yb1 O2 C25 59.1(6) . . . . ? N2 Yb1 O2 C25 -58.5(6) . . . . ? O1 Yb1 O2 C25 -2.4(5) . . . . ? N3 Yb1 O2 C25 84.8(6) . . . . ? N1 Yb1 O2 C25 -87.6(6) . . . . ? B1 Yb1 O2 C25 178.4(6) . . . . ? C2 Yb1 O2 C25 71.2(6) . . . . ? C1 Yb1 O2 C25 -75.2(6) . . . . ? N4 Yb1 O2 C27 -122.6(6) . . . . ? N2 Yb1 O2 C27 119.8(6) . . . . ? O1 Yb1 O2 C27 176.0(6) . . . . ? N3 Yb1 O2 C27 -96.8(6) . . . . ? N1 Yb1 O2 C27 90.8(6) . . . . ? B1 Yb1 O2 C27 -3.2(6) . . . . ? C2 Yb1 O2 C27 -110.5(6) . . . . ? C1 Yb1 O2 C27 103.2(6) . . . . ? C18' Si1 N1 C1 -12.4(11) . . . . ? C20 Si1 N1 C1 -101.1(9) . . . . ? C19' Si1 N1 C1 110.5(9) . . . . ? C18 Si1 N1 C1 23.0(10) . . . . ? C20' Si1 N1 C1 -135.2(9) . . . . ? C19 Si1 N1 C1 139.4(9) . . . . ? C18' Si1 N1 Yb1 -176.9(9) . . . . ? C20 Si1 N1 Yb1 94.5(8) . . . . ? C19' Si1 N1 Yb1 -54.0(9) . . . . ? C18 Si1 N1 Yb1 -141.4(8) . . . . ? C20' Si1 N1 Yb1 60.3(9) . . . . ? C19 Si1 N1 Yb1 -25.0(9) . . . . ? N4 Yb1 N1 C1 6.1(5) . . . . ? N2 Yb1 N1 C1 -0.8(4) . . . . ? O1 Yb1 N1 C1 88.1(4) . . . . ? N3 Yb1 N1 C1 120.3(8) . . . . ? O2 Yb1 N1 C1 154.8(4) . . . . ? B1 Yb1 N1 C1 -108.2(4) . . . . ? C2 Yb1 N1 C1 29.3(7) . . . . ? N4 Yb1 N1 Si1 174.2(4) . . . . ? N2 Yb1 N1 Si1 167.3(6) . . . . ? O1 Yb1 N1 Si1 -103.8(5) . . . . ? N3 Yb1 N1 Si1 -71.6(9) . . . . ? O2 Yb1 N1 Si1 -37.1(5) . . . . ? B1 Yb1 N1 Si1 59.9(5) . . . . ? C2 Yb1 N1 Si1 -162.6(4) . . . . ? C1 Yb1 N1 Si1 168.1(8) . . . . ? N4 Yb1 N2 C1 -173.6(5) . . . . ? O1 Yb1 N2 C1 -84.8(4) . . . . ? N3 Yb1 N2 C1 -164.2(4) . . . . ? N1 Yb1 N2 C1 0.9(4) . . . . ? O2 Yb1 N2 C1 -35.1(5) . . . . ? B1 Yb1 N2 C1 84.6(4) . . . . ? C2 Yb1 N2 C1 -166.6(4) . . . . ? N4 Yb1 N2 C3 1.8(7) . . . . ? O1 Yb1 N2 C3 90.6(7) . . . . ? N3 Yb1 N2 C3 11.2(8) . . . . ? N1 Yb1 N2 C3 176.3(8) . . . . ? O2 Yb1 N2 C3 140.4(6) . . . . ? B1 Yb1 N2 C3 -99.9(7) . . . . ? C2 Yb1 N2 C3 8.9(7) . . . . ? C1 Yb1 N2 C3 175.5(10) . . . . ? C23 Si2 N3 C2 -139.6(7) . . . . ? C21 Si2 N3 C2 -23.2(8) . . . . ? C22 Si2 N3 C2 101.9(7) . . . . ? C23 Si2 N3 Yb1 29.5(6) . . . . ? C21 Si2 N3 Yb1 145.8(5) . . . . ? C22 Si2 N3 Yb1 -89.0(6) . . . . ? N4 Yb1 N3 C2 6.1(4) . . . . ? N2 Yb1 N3 C2 -4.8(5) . . . . ? O1 Yb1 N3 C2 -84.7(4) . . . . ? N1 Yb1 N3 C2 -116.9(8) . . . . ? O2 Yb1 N3 C2 -151.6(4) . . . . ? B1 Yb1 N3 C2 111.6(4) . . . . ? C1 Yb1 N3 C2 -22.7(7) . . . . ? N4 Yb1 N3 Si2 -165.3(6) . . . . ? N2 Yb1 N3 Si2 -176.2(4) . . . . ? O1 Yb1 N3 Si2 103.9(5) . . . . ? N1 Yb1 N3 Si2 71.7(10) . . . . ? O2 Yb1 N3 Si2 36.9(5) . . . . ? B1 Yb1 N3 Si2 -59.8(5) . . . . ? C2 Yb1 N3 Si2 -171.4(8) . . . . ? C1 Yb1 N3 Si2 165.9(4) . . . . ? N2 Yb1 N4 C2 165.1(6) . . . . ? O1 Yb1 N4 C2 78.9(5) . . . . ? N3 Yb1 N4 C2 -6.2(4) . . . . ? N1 Yb1 N4 C2 159.2(4) . . . . ? O2 Yb1 N4 C2 25.2(6) . . . . ? B1 Yb1 N4 C2 -91.1(5) . . . . ? C1 Yb1 N4 C2 162.1(5) . . . . ? N2 Yb1 N4 C5 4.0(7) . . . . ? O1 Yb1 N4 C5 -82.3(8) . . . . ? N3 Yb1 N4 C5 -167.4(9) . . . . ? N1 Yb1 N4 C5 -2.0(9) . . . . ? O2 Yb1 N4 C5 -136.0(7) . . . . ? B1 Yb1 N4 C5 107.7(8) . . . . ? C2 Yb1 N4 C5 -161.2(11) . . . . ? C1 Yb1 N4 C5 1.0(8) . . . . ? C3 N2 C1 N1 -177.7(6) . . . . ? Yb1 N2 C1 N1 -1.5(7) . . . . ? C3 N2 C1 C6 2.0(11) . . . . ? Yb1 N2 C1 C6 178.2(6) . . . . ? C3 N2 C1 Yb1 -176.2(8) . . . . ? Si1 N1 C1 N2 -168.5(5) . . . . ? Yb1 N1 C1 N2 1.4(6) . . . . ? Si1 N1 C1 C6 11.9(11) . . . . ? Yb1 N1 C1 C6 -178.3(7) . . . . ? Si1 N1 C1 Yb1 -169.8(6) . . . . ? N4 Yb1 C1 N2 6.3(5) . . . . ? O1 Yb1 C1 N2 92.6(4) . . . . ? N3 Yb1 C1 N2 30.5(7) . . . . ? N1 Yb1 C1 N2 -178.5(7) . . . . ? O2 Yb1 C1 N2 154.4(4) . . . . ? B1 Yb1 C1 N2 -102.6(4) . . . . ? C2 Yb1 C1 N2 16.9(5) . . . . ? N4 Yb1 C1 N1 -175.2(4) . . . . ? N2 Yb1 C1 N1 178.5(7) . . . . ? O1 Yb1 C1 N1 -88.9(4) . . . . ? N3 Yb1 C1 N1 -151.0(4) . . . . ? O2 Yb1 C1 N1 -27.1(4) . . . . ? B1 Yb1 C1 N1 75.9(4) . . . . ? C2 Yb1 C1 N1 -164.6(4) . . . . ? N4 Yb1 C1 C6 -15(8) . . . . ? N2 Yb1 C1 C6 -21(8) . . . . ? O1 Yb1 C1 C6 71(8) . . . . ? N3 Yb1 C1 C6 9(8) . . . . ? N1 Yb1 C1 C6 160(8) . . . . ? O2 Yb1 C1 C6 133(8) . . . . ? B1 Yb1 C1 C6 -124(8) . . . . ? C2 Yb1 C1 C6 -4(8) . . . . ? C5 N4 C2 N3 175.3(7) . . . . ? Yb1 N4 C2 N3 10.7(7) . . . . ? C5 N4 C2 C12 -3.5(11) . . . . ? Yb1 N4 C2 C12 -168.1(6) . . . . ? C5 N4 C2 Yb1 164.6(9) . . . . ? Si2 N3 C2 N4 163.4(5) . . . . ? Yb1 N3 C2 N4 -9.9(7) . . . . ? Si2 N3 C2 C12 -17.9(11) . . . . ? Yb1 N3 C2 C12 168.8(7) . . . . ? Si2 N3 C2 Yb1 173.3(6) . . . . ? N2 Yb1 C2 N4 -14.7(6) . . . . ? O1 Yb1 C2 N4 -98.8(5) . . . . ? N3 Yb1 C2 N4 169.1(8) . . . . ? N1 Yb1 C2 N4 -39.8(8) . . . . ? O2 Yb1 C2 N4 -161.2(5) . . . . ? B1 Yb1 C2 N4 96.3(5) . . . . ? C1 Yb1 C2 N4 -22.6(6) . . . . ? N4 Yb1 C2 N3 -169.1(8) . . . . ? N2 Yb1 C2 N3 176.2(4) . . . . ? O1 Yb1 C2 N3 92.1(4) . . . . ? N1 Yb1 C2 N3 151.1(4) . . . . ? O2 Yb1 C2 N3 29.7(5) . . . . ? B1 Yb1 C2 N3 -72.8(4) . . . . ? C1 Yb1 C2 N3 168.3(4) . . . . ? N4 Yb1 C2 C12 67(2) . . . . ? N2 Yb1 C2 C12 53(3) . . . . ? O1 Yb1 C2 C12 -31(3) . . . . ? N3 Yb1 C2 C12 -124(3) . . . . ? N1 Yb1 C2 C12 28(3) . . . . ? O2 Yb1 C2 C12 -94(3) . . . . ? B1 Yb1 C2 C12 164(2) . . . . ? C1 Yb1 C2 C12 45(3) . . . . ? C1 N2 C3 C4 -159.8(7) . . . . ? Yb1 N2 C3 C4 25.7(10) . . . . ? N2 C3 C4 C5 -63.3(9) . . . . ? C3 C4 C5 N4 66.7(8) . . . . ? C2 N4 C5 C4 167.1(7) . . . . ? Yb1 N4 C5 C4 -35.5(10) . . . . ? N2 C1 C6 C11 78.2(11) . . . . ? N1 C1 C6 C11 -102.2(10) . . . . ? Yb1 C1 C6 C11 98(8) . . . . ? N2 C1 C6 C7 -99.3(10) . . . . ? N1 C1 C6 C7 80.3(11) . . . . ? Yb1 C1 C6 C7 -79(8) . . . . ? C11 C6 C7 C8 5.3(14) . . . . ? C1 C6 C7 C8 -177.0(8) . . . . ? C6 C7 C8 C9 -5.4(14) . . . . ? C7 C8 C9 C10 5.5(15) . . . . ? C8 C9 C10 C11 -5.3(15) . . . . ? C7 C6 C11 C10 -4.8(14) . . . . ? C1 C6 C11 C10 177.6(8) . . . . ? C9 C10 C11 C6 4.8(14) . . . . ? N4 C2 C12 C17 110.8(9) . . . . ? N3 C2 C12 C17 -67.9(10) . . . . ? Yb1 C2 C12 C17 50(3) . . . . ? N4 C2 C12 C13 -73.9(10) . . . . ? N3 C2 C12 C13 107.5(9) . . . . ? Yb1 C2 C12 C13 -135(2) . . . . ? C17 C12 C13 C14 0.5(11) . . . . ? C2 C12 C13 C14 -174.8(7) . . . . ? C12 C13 C14 C15 -2.9(12) . . . . ? C13 C14 C15 C16 3.3(14) . . . . ? C14 C15 C16 C17 -1.3(15) . . . . ? C13 C12 C17 C16 1.4(12) . . . . ? C2 C12 C17 C16 176.8(7) . . . . ? C15 C16 C17 C12 -1.0(13) . . . . ? C26 O1 C24 C25 157.4(8) . . . . ? Yb1 O1 C24 C25 -39.2(10) . . . . ? C27 O2 C25 C24 167.0(7) . . . . ? Yb1 O2 C25 C24 -14.3(9) . . . . ? O1 C24 C25 O2 34.0(11) . . . . ? C30 O3 C28 C29 170.3(11) . . . . ? C31 O4 C29 C28 -179.8(10) . . . . ? O3 C28 C29 O4 -73.1(13) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.844 _refine_diff_density_min -0.855 _refine_diff_density_rms 0.095