# 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 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Christopher Russell' _publ_contact_author_address ;School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS ; _publ_contact_author_email Chris.Russell@bris.ac.uk _publ_contact_author_phone 01179287599 _publ_contact_author_fax 01179251295 loop_ _publ_author_name _publ_author_address C.Russell ;School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS ; N.Norman ;School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS ; 'Xiaochen Xie' ;School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS ; M.Haddow ;School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS ; S.Mansell ;School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS ; _publ_section_title ; Diborane(4) Compounds with Bidentate Diamino Groups ; # Attachment '- all.cif' #TrackingRef '- all.cif' data_2bthf _database_code_depnum_ccdc_archive 'CCDC 848882' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H32 Cl2 Li2 O4, C12 H12 B2 N4' _chemical_formula_sum 'C28 H44 B2 Cl2 Li2 N4 O4' _chemical_formula_weight 607.07 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' Li Li -0.0003 0.0001 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6702(3) _cell_length_b 9.7473(3) _cell_length_c 10.6975(3) _cell_angle_alpha 108.594(2) _cell_angle_beta 105.241(2) _cell_angle_gamma 102.205(2) _cell_volume 782.46(4) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7268 _cell_measurement_theta_min 3.55 _cell_measurement_theta_max 32.76 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 322 _exptl_absorpt_coefficient_mu 0.247 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6498 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_process_details 'SADABS-2008/1 - Bruker AXS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23240 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 32.80 _reflns_number_total 5698 _reflns_number_gt 4456 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0688P)^2^+0.1240P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5698 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1217 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 B1 B 0.49087(17) 0.91656(15) 1.00551(15) 0.0166(2) Uani 1 1 d . . . N1 N 0.38147(13) 1.08591(11) 0.88110(11) 0.0179(2) Uani 1 1 d . . . H1 H 0.3866 1.1728 0.8711 0.021 Uiso 1 1 calc R . . N2 N 0.34982(13) 0.79138(11) 0.90159(11) 0.0177(2) Uani 1 1 d . . . H2 H 0.3353 0.7006 0.9047 0.021 Uiso 1 1 calc R . . C1 C 0.24788(15) 0.95374(13) 0.78505(13) 0.0167(2) Uani 1 1 d . . . C2 C 0.23291(15) 0.80889(13) 0.79398(13) 0.0170(2) Uani 1 1 d . . . C3 C 0.09766(16) 0.68219(14) 0.69239(13) 0.0202(2) Uani 1 1 d . . . H3 H 0.0878 0.5851 0.6970 0.024 Uiso 1 1 calc R . . C4 C -0.02326(17) 0.69334(15) 0.58452(14) 0.0226(2) Uani 1 1 d . . . H4 H -0.1137 0.6050 0.5162 0.027 Uiso 1 1 calc R . . C5 C -0.01041(17) 0.83507(16) 0.57766(14) 0.0225(2) Uani 1 1 d . . . H5 H -0.0930 0.8445 0.5053 0.027 Uiso 1 1 calc R . . C6 C 0.12332(16) 0.96252(15) 0.67678(13) 0.0200(2) Uani 1 1 d . . . H6 H 0.1308 1.0589 0.6711 0.024 Uiso 1 1 calc R . . Li1 Li 0.5893(3) 0.4947(2) 0.9027(2) 0.0203(4) Uani 1 1 d . . . Cl1 Cl 0.29826(4) 0.41758(3) 0.85209(3) 0.01773(8) Uani 1 1 d . . . O1 O 0.65986(12) 0.65449(10) 0.84145(10) 0.02095(18) Uani 1 1 d . . . C7 C 0.58718(18) 0.65789(15) 0.70577(14) 0.0236(3) Uani 1 1 d . . . H7A H 0.4623 0.6193 0.6724 0.028 Uiso 1 1 calc R . . H7B H 0.6253 0.5943 0.6354 0.028 Uiso 1 1 calc R . . C8 C 0.64917(16) 0.82539(15) 0.72814(13) 0.0212(2) Uani 1 1 d . . . H8A H 0.5643 0.8757 0.7447 0.025 Uiso 1 1 calc R . . H8B H 0.6730 0.8351 0.6452 0.025 Uiso 1 1 calc R . . C9 C 0.81220(16) 0.89622(15) 0.85980(13) 0.0204(2) Uani 1 1 d . . . H9A H 0.9113 0.9346 0.8362 0.024 Uiso 1 1 calc R . . H9B H 0.8036 0.9818 0.9351 0.024 Uiso 1 1 calc R . . C10 C 0.82689(16) 0.76533(15) 0.90620(14) 0.0213(2) Uani 1 1 d . . . H10A H 0.9086 0.7201 0.8739 0.026 Uiso 1 1 calc R . . H10B H 0.8648 0.8021 1.0103 0.026 Uiso 1 1 calc R . . O2 O 0.64318(12) 0.32047(11) 0.80131(10) 0.02250(19) Uani 1 1 d . . . C11 C 0.55776(18) 0.24404(18) 0.65085(15) 0.0301(3) Uani 1 1 d . . . H11A H 0.4852 0.2995 0.6155 0.036 Uiso 1 1 calc R . . H11B H 0.4869 0.1381 0.6247 0.036 Uiso 1 1 calc R . . C12 C 0.6977(2) 0.2446(2) 0.59114(16) 0.0329(3) Uani 1 1 d . . . H12A H 0.7416 0.3435 0.5846 0.040 Uiso 1 1 calc R . . H12B H 0.6591 0.1608 0.4967 0.040 Uiso 1 1 calc R . . C13 C 0.82935(18) 0.22005(17) 0.69955(15) 0.0274(3) Uani 1 1 d . . . H13A H 0.8055 0.1101 0.6811 0.033 Uiso 1 1 calc R . . H13B H 0.9442 0.2620 0.7003 0.033 Uiso 1 1 calc R . . C14 C 0.8108(2) 0.3074(2) 0.83655(16) 0.0343(3) Uani 1 1 d . . . H14A H 0.8253 0.2521 0.8998 0.041 Uiso 1 1 calc R . . H14B H 0.8971 0.4102 0.8852 0.041 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0210(6) 0.0143(6) 0.0187(6) 0.0077(5) 0.0098(5) 0.0084(5) N1 0.0233(5) 0.0131(4) 0.0204(5) 0.0090(4) 0.0083(4) 0.0080(4) N2 0.0225(5) 0.0120(4) 0.0212(5) 0.0084(4) 0.0084(4) 0.0072(4) C1 0.0203(5) 0.0164(5) 0.0168(5) 0.0070(4) 0.0091(4) 0.0086(4) C2 0.0210(5) 0.0157(5) 0.0175(5) 0.0069(4) 0.0096(4) 0.0080(4) C3 0.0235(6) 0.0167(5) 0.0201(6) 0.0055(5) 0.0091(5) 0.0071(5) C4 0.0226(6) 0.0227(6) 0.0179(6) 0.0036(5) 0.0071(5) 0.0057(5) C5 0.0232(6) 0.0293(7) 0.0180(6) 0.0103(5) 0.0081(5) 0.0118(5) C6 0.0240(6) 0.0224(6) 0.0192(6) 0.0108(5) 0.0099(5) 0.0115(5) Li1 0.0234(10) 0.0176(10) 0.0206(10) 0.0069(9) 0.0093(9) 0.0071(8) Cl1 0.01754(13) 0.01417(13) 0.01896(14) 0.00624(10) 0.00356(10) 0.00446(10) O1 0.0210(4) 0.0187(4) 0.0207(4) 0.0090(4) 0.0050(4) 0.0028(3) C7 0.0248(6) 0.0228(6) 0.0166(6) 0.0055(5) 0.0038(5) 0.0031(5) C8 0.0211(6) 0.0236(6) 0.0188(6) 0.0101(5) 0.0060(5) 0.0059(5) C9 0.0200(5) 0.0201(6) 0.0188(6) 0.0084(5) 0.0056(5) 0.0029(5) C10 0.0171(5) 0.0236(6) 0.0224(6) 0.0106(5) 0.0055(5) 0.0049(5) O2 0.0233(4) 0.0226(5) 0.0200(4) 0.0046(4) 0.0072(4) 0.0110(4) C11 0.0211(6) 0.0334(8) 0.0217(6) -0.0031(6) 0.0033(5) 0.0091(6) C12 0.0306(7) 0.0476(9) 0.0206(6) 0.0084(6) 0.0101(6) 0.0193(7) C13 0.0234(6) 0.0305(7) 0.0288(7) 0.0090(6) 0.0104(5) 0.0125(6) C14 0.0282(7) 0.0510(10) 0.0238(7) 0.0114(7) 0.0059(6) 0.0226(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N2 1.4175(18) . ? B1 N1 1.4216(17) 2_677 ? B1 B1 1.646(2) 2_677 ? N1 C1 1.3987(16) . ? N1 B1 1.4216(17) 2_677 ? N1 H1 0.8800 . ? N2 C2 1.4025(15) . ? N2 H2 0.8800 . ? C1 C6 1.3999(17) . ? C1 C2 1.4264(16) . ? C2 C3 1.3940(18) . ? C3 C4 1.3909(18) . ? C3 H3 0.9500 . ? C4 C5 1.3893(18) . ? C4 H4 0.9500 . ? C5 C6 1.3844(19) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? Li1 O1 1.920(2) . ? Li1 O2 1.925(2) . ? Li1 Cl1 2.331(2) 2_667 ? Li1 Cl1 2.334(2) . ? Li1 Li1 2.892(4) 2_667 ? Cl1 Li1 2.331(2) 2_667 ? O1 C7 1.4366(15) . ? O1 C10 1.4416(15) . ? C7 C8 1.5244(18) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.5424(18) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.5264(17) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? O2 C11 1.4386(17) . ? O2 C14 1.4457(17) . ? C11 C12 1.512(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.517(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.512(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? 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 N2 B1 N1 127.13(11) . 2_677 ? N2 B1 B1 116.67(14) . 2_677 ? N1 B1 B1 116.20(14) 2_677 2_677 ? C1 N1 B1 121.64(10) . 2_677 ? C1 N1 H1 119.2 . . ? B1 N1 H1 119.2 2_677 . ? C2 N2 B1 121.54(10) . . ? C2 N2 H2 119.2 . . ? B1 N2 H2 119.2 . . ? N1 C1 C6 119.55(10) . . ? N1 C1 C2 122.12(11) . . ? C6 C1 C2 118.34(12) . . ? C3 C2 N2 119.68(10) . . ? C3 C2 C1 118.51(11) . . ? N2 C2 C1 121.82(11) . . ? C4 C3 C2 122.11(11) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C5 C4 C3 119.31(12) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C6 C5 C4 119.71(12) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 122.01(11) . . ? C5 C6 H6 119.0 . . ? C1 C6 H6 119.0 . . ? O1 Li1 O2 108.02(11) . . ? O1 Li1 Cl1 110.95(10) . 2_667 ? O2 Li1 Cl1 115.11(10) . 2_667 ? O1 Li1 Cl1 111.84(10) . . ? O2 Li1 Cl1 107.51(10) . . ? Cl1 Li1 Cl1 103.36(8) 2_667 . ? O1 Li1 Li1 126.05(14) . 2_667 ? O2 Li1 Li1 125.79(13) . 2_667 ? Cl1 Li1 Li1 51.72(7) 2_667 2_667 ? Cl1 Li1 Li1 51.64(7) . 2_667 ? Li1 Cl1 Li1 76.64(8) 2_667 . ? C7 O1 C10 106.50(9) . . ? C7 O1 Li1 127.34(11) . . ? C10 O1 Li1 123.25(10) . . ? O1 C7 C8 105.35(10) . . ? O1 C7 H7A 110.7 . . ? C8 C7 H7A 110.7 . . ? O1 C7 H7B 110.7 . . ? C8 C7 H7B 110.7 . . ? H7A C7 H7B 108.8 . . ? C7 C8 C9 104.38(10) . . ? C7 C8 H8A 110.9 . . ? C9 C8 H8A 110.9 . . ? C7 C8 H8B 110.9 . . ? C9 C8 H8B 110.9 . . ? H8A C8 H8B 108.9 . . ? C10 C9 C8 104.59(10) . . ? C10 C9 H9A 110.8 . . ? C8 C9 H9A 110.8 . . ? C10 C9 H9B 110.8 . . ? C8 C9 H9B 110.8 . . ? H9A C9 H9B 108.9 . . ? O1 C10 C9 105.56(10) . . ? O1 C10 H10A 110.6 . . ? C9 C10 H10A 110.6 . . ? O1 C10 H10B 110.6 . . ? C9 C10 H10B 110.6 . . ? H10A C10 H10B 108.8 . . ? C11 O2 C14 108.69(10) . . ? C11 O2 Li1 118.71(10) . . ? C14 O2 Li1 123.79(11) . . ? O2 C11 C12 104.85(11) . . ? O2 C11 H11A 110.8 . . ? C12 C11 H11A 110.8 . . ? O2 C11 H11B 110.8 . . ? C12 C11 H11B 110.8 . . ? H11A C11 H11B 108.9 . . ? C11 C12 C13 101.92(12) . . ? C11 C12 H12A 111.4 . . ? C13 C12 H12A 111.4 . . ? C11 C12 H12B 111.4 . . ? C13 C12 H12B 111.4 . . ? H12A C12 H12B 109.3 . . ? C14 C13 C12 102.71(11) . . ? C14 C13 H13A 111.2 . . ? C12 C13 H13A 111.2 . . ? C14 C13 H13B 111.2 . . ? C12 C13 H13B 111.2 . . ? H13A C13 H13B 109.1 . . ? O2 C14 C13 107.10(11) . . ? O2 C14 H14A 110.3 . . ? C13 C14 H14A 110.3 . . ? O2 C14 H14B 110.3 . . ? C13 C14 H14B 110.3 . . ? H14A C14 H14B 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 B1 N2 C2 -179.54(11) 2_677 . . . ? B1 B1 N2 C2 0.69(19) 2_677 . . . ? B1 N1 C1 C6 178.71(11) 2_677 . . . ? B1 N1 C1 C2 -0.80(17) 2_677 . . . ? B1 N2 C2 C3 178.83(11) . . . . ? B1 N2 C2 C1 -1.25(17) . . . . ? N1 C1 C2 C3 -178.77(11) . . . . ? C6 C1 C2 C3 1.71(17) . . . . ? N1 C1 C2 N2 1.31(17) . . . . ? C6 C1 C2 N2 -178.21(11) . . . . ? N2 C2 C3 C4 179.09(11) . . . . ? C1 C2 C3 C4 -0.83(18) . . . . ? C2 C3 C4 C5 -0.47(19) . . . . ? C3 C4 C5 C6 0.86(19) . . . . ? C4 C5 C6 C1 0.07(19) . . . . ? N1 C1 C6 C5 179.10(11) . . . . ? C2 C1 C6 C5 -1.37(18) . . . . ? O1 Li1 Cl1 Li1 -119.42(14) . . . 2_667 ? O2 Li1 Cl1 Li1 122.16(13) . . . 2_667 ? Cl1 Li1 Cl1 Li1 0.0 2_667 . . 2_667 ? O2 Li1 O1 C7 69.35(16) . . . . ? Cl1 Li1 O1 C7 -163.60(10) 2_667 . . . ? Cl1 Li1 O1 C7 -48.76(16) . . . . ? Li1 Li1 O1 C7 -106.40(18) 2_667 . . . ? O2 Li1 O1 C10 -88.69(14) . . . . ? Cl1 Li1 O1 C10 38.36(15) 2_667 . . . ? Cl1 Li1 O1 C10 153.20(10) . . . . ? Li1 Li1 O1 C10 95.56(18) 2_667 . . . ? C10 O1 C7 C8 -37.19(13) . . . . ? Li1 O1 C7 C8 161.85(11) . . . . ? O1 C7 C8 C9 23.48(13) . . . . ? C7 C8 C9 C10 -2.29(13) . . . . ? C7 O1 C10 C9 35.64(13) . . . . ? Li1 O1 C10 C9 -162.42(11) . . . . ? C8 C9 C10 O1 -19.57(13) . . . . ? O1 Li1 O2 C11 -65.18(15) . . . . ? Cl1 Li1 O2 C11 170.23(10) 2_667 . . . ? Cl1 Li1 O2 C11 55.68(14) . . . . ? Li1 Li1 O2 C11 110.60(17) 2_667 . . . ? O1 Li1 O2 C14 78.55(15) . . . . ? Cl1 Li1 O2 C14 -46.04(16) 2_667 . . . ? Cl1 Li1 O2 C14 -160.59(11) . . . . ? Li1 Li1 O2 C14 -105.67(18) 2_667 . . . ? C14 O2 C11 C12 -23.97(16) . . . . ? Li1 O2 C11 C12 124.76(13) . . . . ? O2 C11 C12 C13 37.14(16) . . . . ? C11 C12 C13 C14 -35.67(16) . . . . ? C11 O2 C14 C13 0.85(17) . . . . ? Li1 O2 C14 C13 -145.94(12) . . . . ? C12 C13 C14 O2 22.32(17) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 32.80 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.480 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.073 data_2bdma _database_code_depnum_ccdc_archive 'CCDC 848883' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 B2 N4, 2(C4 H9 N O)' _chemical_formula_sum 'C20 H30 B2 N6 O2' _chemical_formula_weight 408.12 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.708(3) _cell_length_b 8.5531(14) _cell_length_c 12.4561(19) _cell_angle_alpha 90.00 _cell_angle_beta 115.224(5) _cell_angle_gamma 90.00 _cell_volume 2188.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1899 _cell_measurement_theta_min 2.5785 _cell_measurement_theta_max 26.9965 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.719044 _exptl_absorpt_correction_T_max 0.999104 _exptl_absorpt_process_details 'SADABS-2008/1 - Bruker AXS' _exptl_special_details ; Crystal poorly diffracting at high angle. Cut-off at 0.90 A resolution was applied. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5649 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 23.26 _reflns_number_total 1559 _reflns_number_gt 1115 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2004)' _computing_cell_refinement 'APEX-II and SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT v7.51A (BRUKER)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0980P)^2^+7.4484P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1559 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1018 _refine_ls_R_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.2120 _refine_ls_wR_factor_gt 0.1887 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 O1 O 0.41027(12) 0.3682(3) 0.6862(2) 0.0293(7) Uani 1 1 d . A 1 B1 B 0.5014(2) -0.0670(5) 1.0485(3) 0.0268(10) Uani 1 1 d . . . N1 N 0.44150(15) -0.1197(4) 1.0432(2) 0.0281(8) Uani 1 1 d . . . H1 H 0.4354(19) -0.186(5) 1.085(3) 0.042 Uiso 1 1 d . . . N2 N 0.43544(14) 0.1169(4) 0.8717(2) 0.0280(8) Uani 1 1 d . . . H2 H 0.4280(19) 0.185(5) 0.818(4) 0.042 Uiso 1 1 d . . . C1 C 0.38182(17) -0.0590(4) 0.9599(3) 0.0256(9) Uani 1 1 d . . . C2 C 0.37890(17) 0.0561(4) 0.8761(3) 0.0268(9) Uani 1 1 d . . . C3 C 0.31822(19) 0.1110(5) 0.7971(3) 0.0351(10) Uani 1 1 d . . . H3 H 0.3159 0.1866 0.7396 0.042 Uiso 1 1 calc R . . C4 C 0.2610(2) 0.0592(5) 0.7995(3) 0.0398(11) Uani 1 1 d . . . H4 H 0.2202 0.0994 0.7449 0.048 Uiso 1 1 calc R . . C5 C 0.26412(19) -0.0519(5) 0.8824(3) 0.0365(10) Uani 1 1 d . . . H5 H 0.2254 -0.0881 0.8856 0.044 Uiso 1 1 calc R . . C6 C 0.32356(18) -0.1095(4) 0.9601(3) 0.0329(10) Uani 1 1 d . . . H6 H 0.3250 -0.1867 1.0160 0.039 Uiso 1 1 calc R . . N3 N 0.3867(2) 0.6217(5) 0.6452(4) 0.0628(12) Uani 1 1 d . A . C7 C 0.4135(2) 0.5082(7) 0.7173(4) 0.0551(13) Uani 1 1 d . . . C8 C 0.3524(2) 0.5782(6) 0.5143(3) 0.0586(14) Uani 1 1 d . . . H8A H 0.3555 0.4650 0.5055 0.088 Uiso 1 1 calc R A . H8B H 0.3731 0.6329 0.4703 0.088 Uiso 1 1 calc R . . H8C H 0.3065 0.6086 0.4829 0.088 Uiso 1 1 calc R . . C9 C 0.3884(3) 0.7881(5) 0.6772(5) 0.0743(18) Uani 1 1 d . . . H9A H 0.3912 0.7969 0.7577 0.111 Uiso 1 1 calc R A . H9B H 0.3487 0.8399 0.6211 0.111 Uiso 1 1 calc R . . H9C H 0.4264 0.8382 0.6741 0.111 Uiso 1 1 calc R . . C10 C 0.4510(2) 0.5585(6) 0.8479(3) 0.0533(13) Uani 1 1 d . A . H10A H 0.4724 0.4672 0.8963 0.080 Uiso 1 1 calc R . . H10B H 0.4206 0.6035 0.8763 0.080 Uiso 1 1 calc R . . H10C H 0.4838 0.6367 0.8540 0.080 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0428(17) 0.0206(15) 0.0264(13) -0.0026(11) 0.0166(12) 0.0042(11) B1 0.035(3) 0.029(2) 0.0198(19) 0.0010(18) 0.0146(19) 0.0028(19) N1 0.037(2) 0.0296(18) 0.0219(16) 0.0061(13) 0.0167(15) 0.0000(15) N2 0.036(2) 0.0298(18) 0.0196(16) 0.0088(13) 0.0133(15) 0.0039(15) C1 0.032(2) 0.028(2) 0.0176(18) -0.0040(15) 0.0112(17) -0.0010(16) C2 0.032(2) 0.031(2) 0.0185(18) -0.0016(15) 0.0119(17) 0.0016(16) C3 0.041(3) 0.039(2) 0.0233(19) 0.0029(17) 0.0119(18) 0.0050(19) C4 0.032(2) 0.052(3) 0.028(2) -0.0068(19) 0.0054(18) 0.002(2) C5 0.034(2) 0.044(3) 0.032(2) -0.0077(19) 0.0147(19) -0.0054(19) C6 0.040(2) 0.032(2) 0.029(2) -0.0028(17) 0.0179(19) -0.0047(18) N3 0.076(3) 0.055(3) 0.078(3) 0.019(2) 0.052(3) 0.011(2) C7 0.040(3) 0.082(4) 0.055(3) 0.015(3) 0.030(2) 0.007(3) C8 0.066(3) 0.089(4) 0.023(2) 0.020(2) 0.020(2) 0.003(3) C9 0.141(5) 0.021(3) 0.092(4) 0.009(2) 0.079(4) 0.016(3) C10 0.064(3) 0.077(3) 0.022(2) -0.018(2) 0.022(2) -0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C7 1.252(6) . ? B1 N1 1.407(5) . ? B1 N2 1.419(5) 5_657 ? B1 B1 1.648(8) 5_657 ? N1 C1 1.409(5) . ? N1 H1 0.82(4) . ? N2 C2 1.408(5) . ? N2 B1 1.419(5) 5_657 ? N2 H2 0.85(4) . ? C1 C6 1.393(5) . ? C1 C2 1.416(5) . ? C2 C3 1.390(5) . ? C3 C4 1.386(5) . ? C3 H3 0.9500 . ? C4 C5 1.382(6) . ? C4 H4 0.9500 . ? C5 C6 1.374(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? N3 C7 1.286(6) . ? N3 C9 1.474(6) . ? N3 C8 1.524(6) . ? C7 C10 1.540(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 B1 N2 127.3(3) . 5_657 ? N1 B1 B1 117.1(4) . 5_657 ? N2 B1 B1 115.7(4) 5_657 5_657 ? B1 N1 C1 121.6(3) . . ? B1 N1 H1 128(3) . . ? C1 N1 H1 111(3) . . ? C2 N2 B1 122.0(3) . 5_657 ? C2 N2 H2 114(3) . . ? B1 N2 H2 124(3) 5_657 . ? C6 C1 N1 120.0(3) . . ? C6 C1 C2 118.1(3) . . ? N1 C1 C2 121.8(3) . . ? C3 C2 N2 119.6(3) . . ? C3 C2 C1 118.5(3) . . ? N2 C2 C1 121.9(3) . . ? C4 C3 C2 122.2(4) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C5 C4 C3 119.0(4) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C6 C5 C4 119.7(4) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C1 122.4(4) . . ? C5 C6 H6 118.8 . . ? C1 C6 H6 118.8 . . ? C7 N3 C9 126.2(5) . . ? C7 N3 C8 115.9(4) . . ? C9 N3 C8 117.9(4) . . ? O1 C7 N3 123.9(5) . . ? O1 C7 C10 121.8(4) . . ? N3 C7 C10 114.3(5) . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 B1 N1 C1 179.4(3) 5_657 . . . ? B1 B1 N1 C1 -1.0(6) 5_657 . . . ? B1 N1 C1 C6 -177.5(3) . . . . ? B1 N1 C1 C2 1.1(5) . . . . ? B1 N2 C2 C3 178.9(3) 5_657 . . . ? B1 N2 C2 C1 -0.4(5) 5_657 . . . ? C6 C1 C2 C3 -1.0(5) . . . . ? N1 C1 C2 C3 -179.7(3) . . . . ? C6 C1 C2 N2 178.3(3) . . . . ? N1 C1 C2 N2 -0.3(5) . . . . ? N2 C2 C3 C4 -178.0(3) . . . . ? C1 C2 C3 C4 1.3(5) . . . . ? C2 C3 C4 C5 -0.6(6) . . . . ? C3 C4 C5 C6 -0.4(6) . . . . ? C4 C5 C6 C1 0.7(6) . . . . ? N1 C1 C6 C5 178.7(3) . . . . ? C2 C1 C6 C5 0.0(5) . . . . ? C9 N3 C7 O1 179.4(4) . . . . ? C8 N3 C7 O1 -3.2(6) . . . . ? C9 N3 C7 C10 -0.9(6) . . . . ? C8 N3 C7 C10 176.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.793 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.064 data_4 _database_code_depnum_ccdc_archive 'CCDC 848884' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H20 B2 N4' _chemical_formula_sum 'C16 H20 B2 N4' _chemical_formula_weight 289.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.3806(5) _cell_length_b 8.3655(3) _cell_length_c 26.4698(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3184.34(19) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4701 _cell_measurement_theta_min 2.833 _cell_measurement_theta_max 28.0995 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6575 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS-2008/1 - Bruker AXS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II kappa CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23345 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 24.71 _reflns_number_total 2707 _reflns_number_gt 2088 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+0.7827P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2707 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.957 _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 B1 B 0.88478(12) 0.0457(2) 0.33082(7) 0.0194(4) Uani 1 1 d . . . B2 B 0.88237(12) 0.0047(2) 0.39339(7) 0.0200(4) Uani 1 1 d . . . N1 N 0.81846(9) -0.00800(16) 0.29385(5) 0.0194(3) Uani 1 1 d . . . N2 N 0.95047(9) 0.13962(16) 0.30262(5) 0.0189(3) Uani 1 1 d . . . N3 N 0.86710(9) -0.14969(15) 0.41608(5) 0.0195(3) Uani 1 1 d . . . N4 N 0.88807(9) 0.11332(16) 0.43506(5) 0.0195(3) Uani 1 1 d . . . C1 C 0.84312(11) 0.05027(18) 0.24639(6) 0.0194(4) Uani 1 1 d . . . C2 C 0.92468(11) 0.14162(19) 0.25194(6) 0.0191(4) Uani 1 1 d . . . C3 C 0.96395(12) 0.2193(2) 0.21097(6) 0.0244(4) Uani 1 1 d . . . H3 H 1.0188 0.2815 0.2147 0.029 Uiso 1 1 calc R . . C4 C 0.92061(12) 0.2034(2) 0.16423(6) 0.0276(4) Uani 1 1 d . . . H4 H 0.9463 0.2557 0.1356 0.033 Uiso 1 1 calc R . . C5 C 0.84042(12) 0.1122(2) 0.15869(6) 0.0279(4) Uani 1 1 d . . . H5 H 0.8126 0.1028 0.1263 0.033 Uiso 1 1 calc R . . C6 C 0.80007(11) 0.0346(2) 0.19964(6) 0.0246(4) Uani 1 1 d . . . H6 H 0.7450 -0.0270 0.1958 0.030 Uiso 1 1 calc R . . C7 C 0.86336(10) -0.1326(2) 0.46848(6) 0.0195(4) Uani 1 1 d . . . C8 C 0.87638(10) 0.0295(2) 0.48022(6) 0.0196(4) Uani 1 1 d . . . C9 C 0.87489(11) 0.0812(2) 0.52991(6) 0.0233(4) Uani 1 1 d . . . H9 H 0.8847 0.1905 0.5381 0.028 Uiso 1 1 calc R . . C10 C 0.85860(12) -0.0315(2) 0.56743(6) 0.0265(4) Uani 1 1 d . . . H10 H 0.8570 0.0015 0.6018 0.032 Uiso 1 1 calc R . . C11 C 0.84471(11) -0.1911(2) 0.55574(6) 0.0266(4) Uani 1 1 d . . . H11 H 0.8333 -0.2653 0.5822 0.032 Uiso 1 1 calc R . . C12 C 0.84711(11) -0.2447(2) 0.50601(6) 0.0235(4) Uani 1 1 d . . . H12 H 0.8379 -0.3543 0.4981 0.028 Uiso 1 1 calc R . . C13 C 0.73175(11) -0.0942(2) 0.30077(6) 0.0267(4) Uani 1 1 d . . . H13A H 0.6800 -0.0288 0.2885 0.040 Uiso 1 1 calc R . . H13B H 0.7228 -0.1175 0.3367 0.040 Uiso 1 1 calc R . . H13C H 0.7340 -0.1947 0.2817 0.040 Uiso 1 1 calc R . . C14 C 1.03306(11) 0.2241(2) 0.31950(6) 0.0267(4) Uani 1 1 d . . . H14A H 1.0875 0.1838 0.3012 0.040 Uiso 1 1 calc R . . H14B H 1.0417 0.2068 0.3558 0.040 Uiso 1 1 calc R . . H14C H 1.0258 0.3387 0.3129 0.040 Uiso 1 1 calc R . . C15 C 0.85789(12) -0.3069(2) 0.39308(6) 0.0248(4) Uani 1 1 d . . . H15A H 0.9078 -0.3766 0.4053 0.037 Uiso 1 1 calc R . . H15B H 0.8621 -0.2969 0.3563 0.037 Uiso 1 1 calc R . . H15C H 0.7976 -0.3530 0.4022 0.037 Uiso 1 1 calc R . . C16 C 0.89901(12) 0.2863(2) 0.43537(6) 0.0249(4) Uani 1 1 d . . . H16A H 0.8454 0.3353 0.4522 0.037 Uiso 1 1 calc R . . H16B H 0.9030 0.3254 0.4005 0.037 Uiso 1 1 calc R . . H16C H 0.9560 0.3146 0.4536 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0202(10) 0.0097(10) 0.0282(10) -0.0023(8) 0.0012(7) 0.0037(8) B2 0.0157(9) 0.0154(10) 0.0290(10) 0.0010(8) 0.0007(7) -0.0008(8) N1 0.0197(7) 0.0146(8) 0.0240(7) -0.0016(6) 0.0029(5) -0.0012(6) N2 0.0185(7) 0.0154(8) 0.0228(7) 0.0005(6) -0.0015(5) -0.0021(6) N3 0.0226(7) 0.0132(8) 0.0226(7) -0.0017(6) 0.0017(5) -0.0007(6) N4 0.0220(7) 0.0121(8) 0.0246(8) 0.0008(6) -0.0011(5) -0.0007(6) C1 0.0206(8) 0.0124(9) 0.0253(9) -0.0031(7) 0.0009(6) 0.0035(7) C2 0.0186(8) 0.0138(9) 0.0248(9) -0.0006(7) -0.0004(6) 0.0044(7) C3 0.0221(9) 0.0216(10) 0.0295(10) 0.0041(7) 0.0017(7) 0.0012(8) C4 0.0282(10) 0.0284(11) 0.0263(9) 0.0055(8) 0.0023(7) 0.0065(8) C5 0.0290(10) 0.0311(11) 0.0237(9) -0.0006(8) -0.0035(7) 0.0084(8) C6 0.0219(9) 0.0215(10) 0.0304(10) -0.0050(8) -0.0019(7) 0.0043(7) C7 0.0156(8) 0.0194(10) 0.0235(9) -0.0003(7) -0.0001(6) 0.0012(7) C8 0.0157(8) 0.0191(9) 0.0238(9) 0.0029(7) -0.0009(6) 0.0003(7) C9 0.0225(9) 0.0208(10) 0.0267(9) -0.0019(8) -0.0028(7) 0.0008(7) C10 0.0249(9) 0.0315(11) 0.0231(9) -0.0017(8) -0.0004(7) -0.0006(8) C11 0.0229(9) 0.0308(11) 0.0261(10) 0.0071(8) 0.0002(7) -0.0035(8) C12 0.0208(9) 0.0193(10) 0.0303(10) 0.0030(8) 0.0003(7) -0.0023(7) C13 0.0243(9) 0.0207(10) 0.0351(10) -0.0054(8) 0.0028(7) -0.0078(8) C14 0.0222(9) 0.0265(11) 0.0313(10) 0.0026(8) -0.0031(7) -0.0057(8) C15 0.0294(9) 0.0156(10) 0.0293(10) -0.0015(8) 0.0036(7) -0.0038(8) C16 0.0290(9) 0.0161(10) 0.0296(10) -0.0008(8) -0.0019(7) 0.0000(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N2 1.438(2) . ? B1 N1 1.438(2) . ? B1 B2 1.692(3) . ? B2 N4 1.432(2) . ? B2 N3 1.441(2) . ? N1 C1 1.393(2) . ? N1 C13 1.452(2) . ? N2 C2 1.3918(19) . ? N2 C14 1.452(2) . ? N3 C7 1.395(2) . ? N3 C15 1.455(2) . ? N4 C8 1.3962(19) . ? N4 C16 1.455(2) . ? C1 C6 1.390(2) . ? C1 C2 1.408(2) . ? C2 C3 1.385(2) . ? C3 C4 1.392(2) . ? C3 H3 0.9500 . ? C4 C5 1.390(2) . ? C4 H4 0.9500 . ? C5 C6 1.391(2) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.386(2) . ? C7 C8 1.404(2) . ? C8 C9 1.385(2) . ? C9 C10 1.389(2) . ? C9 H9 0.9500 . ? C10 C11 1.385(3) . ? C10 H10 0.9500 . ? C11 C12 1.391(2) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 B1 N1 104.66(14) . . ? N2 B1 B2 129.24(15) . . ? N1 B1 B2 126.09(15) . . ? N4 B2 N3 104.86(14) . . ? N4 B2 B1 128.65(15) . . ? N3 B2 B1 126.36(15) . . ? C1 N1 B1 109.60(13) . . ? C1 N1 C13 120.40(13) . . ? B1 N1 C13 129.70(14) . . ? C2 N2 B1 109.38(13) . . ? C2 N2 C14 120.56(13) . . ? B1 N2 C14 130.05(14) . . ? C7 N3 B2 109.18(13) . . ? C7 N3 C15 120.32(13) . . ? B2 N3 C15 130.49(14) . . ? C8 N4 B2 109.50(14) . . ? C8 N4 C16 120.52(13) . . ? B2 N4 C16 129.91(14) . . ? C6 C1 N1 131.02(15) . . ? C6 C1 C2 121.02(15) . . ? N1 C1 C2 107.93(13) . . ? C3 C2 N2 130.68(15) . . ? C3 C2 C1 120.85(15) . . ? N2 C2 C1 108.43(13) . . ? C2 C3 C4 117.96(16) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C5 C4 C3 121.18(16) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 121.34(15) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C1 C6 C5 117.65(16) . . ? C1 C6 H6 121.2 . . ? C5 C6 H6 121.2 . . ? C12 C7 N3 130.53(15) . . ? C12 C7 C8 121.15(15) . . ? N3 C7 C8 108.29(14) . . ? C9 C8 N4 131.13(16) . . ? C9 C8 C7 120.69(15) . . ? N4 C8 C7 108.17(14) . . ? C8 C9 C10 117.99(16) . . ? C8 C9 H9 121.0 . . ? C10 C9 H9 121.0 . . ? C11 C10 C9 121.24(16) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 121.25(16) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C7 C12 C11 117.67(16) . . ? C7 C12 H12 121.2 . . ? C11 C12 H12 121.2 . . ? N1 C13 H13A 109.5 . . ? N1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 C16 H16A 109.5 . . ? N4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 B1 B2 N4 51.1(3) . . . . ? N1 B1 B2 N4 -128.46(18) . . . . ? N2 B1 B2 N3 -133.75(18) . . . . ? N1 B1 B2 N3 46.7(2) . . . . ? N2 B1 N1 C1 0.06(17) . . . . ? B2 B1 N1 C1 179.72(15) . . . . ? N2 B1 N1 C13 -173.42(14) . . . . ? B2 B1 N1 C13 6.2(3) . . . . ? N1 B1 N2 C2 0.01(17) . . . . ? B2 B1 N2 C2 -179.64(15) . . . . ? N1 B1 N2 C14 -179.74(15) . . . . ? B2 B1 N2 C14 0.6(3) . . . . ? N4 B2 N3 C7 0.39(16) . . . . ? B1 B2 N3 C7 -175.68(14) . . . . ? N4 B2 N3 C15 -178.31(14) . . . . ? B1 B2 N3 C15 5.6(3) . . . . ? N3 B2 N4 C8 -0.33(16) . . . . ? B1 B2 N4 C8 175.62(15) . . . . ? N3 B2 N4 C16 -177.15(14) . . . . ? B1 B2 N4 C16 -1.2(3) . . . . ? B1 N1 C1 C6 -178.16(16) . . . . ? C13 N1 C1 C6 -4.0(3) . . . . ? B1 N1 C1 C2 -0.10(17) . . . . ? C13 N1 C1 C2 174.08(13) . . . . ? B1 N2 C2 C3 177.64(17) . . . . ? C14 N2 C2 C3 -2.6(3) . . . . ? B1 N2 C2 C1 -0.07(17) . . . . ? C14 N2 C2 C1 179.70(14) . . . . ? C6 C1 C2 C3 0.4(2) . . . . ? N1 C1 C2 C3 -177.87(14) . . . . ? C6 C1 C2 N2 178.39(14) . . . . ? N1 C1 C2 N2 0.10(17) . . . . ? N2 C2 C3 C4 -177.83(16) . . . . ? C1 C2 C3 C4 -0.4(2) . . . . ? C2 C3 C4 C5 -0.1(3) . . . . ? C3 C4 C5 C6 0.5(3) . . . . ? N1 C1 C6 C5 177.84(16) . . . . ? C2 C1 C6 C5 0.0(2) . . . . ? C4 C5 C6 C1 -0.4(3) . . . . ? B2 N3 C7 C12 177.62(16) . . . . ? C15 N3 C7 C12 -3.5(2) . . . . ? B2 N3 C7 C8 -0.31(17) . . . . ? C15 N3 C7 C8 178.54(13) . . . . ? B2 N4 C8 C9 -178.91(16) . . . . ? C16 N4 C8 C9 -1.7(2) . . . . ? B2 N4 C8 C7 0.15(17) . . . . ? C16 N4 C8 C7 177.32(13) . . . . ? C12 C7 C8 C9 1.1(2) . . . . ? N3 C7 C8 C9 179.28(13) . . . . ? C12 C7 C8 N4 -178.06(14) . . . . ? N3 C7 C8 N4 0.10(17) . . . . ? N4 C8 C9 C10 177.89(15) . . . . ? C7 C8 C9 C10 -1.1(2) . . . . ? C8 C9 C10 C11 0.3(2) . . . . ? C9 C10 C11 C12 0.4(2) . . . . ? N3 C7 C12 C11 -178.07(15) . . . . ? C8 C7 C12 C11 -0.4(2) . . . . ? C10 C11 C12 C7 -0.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.208 _refine_diff_density_min -0.241 _refine_diff_density_rms 0.041 data_5 _database_code_depnum_ccdc_archive 'CCDC 848885' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H44 B2 N4 Sn4' _chemical_formula_sum 'C24 H44 B2 N4 Sn4' _chemical_formula_weight 885.01 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.5153(15) _cell_length_b 14.5908(14) _cell_length_c 14.6299(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.118(6) _cell_angle_gamma 90.00 _cell_volume 3311.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7899 _cell_measurement_theta_min 2.367 _cell_measurement_theta_max 27.4375 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 2.999 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84903 _exptl_absorpt_correction_T_max 0.96928 _exptl_absorpt_process_details 'SADABS-2008/1 - Bruker AXS' _exptl_special_details ; Twin law needed: -1 0 0 0 -1 0 0 0 1 with BASF: 0.58771. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa-APEX-II area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_reflns_number 15207 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3776 _reflns_number_gt 3485 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2004)' _computing_cell_refinement 'APEX-II and SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT v7.51A (BRUKER)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0104P)^2^+12.1387P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3776 _refine_ls_number_parameters 161 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0518 _refine_ls_wR_factor_gt 0.0509 _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_restrained_S_all 1.166 _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 Sn1 Sn 0.20384(2) 0.425795(18) 0.21892(2) 0.01845(7) Uani 1 1 d . . . Sn2 Sn 0.02076(2) 0.25421(2) 0.46520(2) 0.02146(7) Uani 1 1 d . . . B1 B 0.0000 0.3965(4) 0.2500 0.0160(15) Uani 1 2 d S . . B2 B 0.0000 0.2792(5) 0.2500 0.0166(15) Uani 1 2 d S . . N1 N 0.0741(2) 0.4549(2) 0.2341(3) 0.0163(8) Uani 1 1 d . . . N2 N 0.0106(2) 0.2206(2) 0.3290(3) 0.0168(8) Uani 1 1 d . . . C1 C 0.0446(3) 0.5459(3) 0.2402(3) 0.0153(10) Uani 1 1 d . . . C2 C 0.0889(3) 0.6279(3) 0.2297(3) 0.0180(10) Uani 1 1 d . . . H2 H 0.1488 0.6281 0.2163 0.022 Uiso 1 1 calc R . . C3 C 0.0436(3) 0.7105(3) 0.2392(3) 0.0213(11) Uani 1 1 d . . . H3 H 0.0728 0.7670 0.2309 0.026 Uiso 1 1 calc R . . C4 C 0.0063(3) 0.1295(2) 0.2967(3) 0.0178(10) Uani 1 1 d . . . C5 C 0.0128(3) 0.0469(3) 0.3454(3) 0.0219(10) Uani 1 1 d . . . H5 H 0.0209 0.0466 0.4098 0.026 Uiso 1 1 calc R . . C6 C 0.0069(3) -0.0347(3) 0.2960(4) 0.0315(13) Uani 1 1 d . . . H6 H 0.0125 -0.0914 0.3272 0.038 Uiso 1 1 calc R . . C7 C 0.2669(3) 0.5026(4) 0.3221(4) 0.0344(13) Uani 1 1 d . . . H7A H 0.2311 0.5553 0.3389 0.052 Uiso 1 1 calc R . . H7B H 0.3226 0.5243 0.2992 0.052 Uiso 1 1 calc R . . H7C H 0.2761 0.4638 0.3759 0.052 Uiso 1 1 calc R . . C8 C 0.2377(4) 0.4710(4) 0.0848(4) 0.0388(14) Uani 1 1 d . . . H8A H 0.2132 0.4290 0.0394 0.058 Uiso 1 1 calc R . . H8B H 0.3006 0.4719 0.0788 0.058 Uiso 1 1 calc R . . H8C H 0.2149 0.5328 0.0747 0.058 Uiso 1 1 calc R . . C9 C 0.2174(3) 0.2811(3) 0.2336(4) 0.0311(12) Uani 1 1 d . . . H9A H 0.2156 0.2649 0.2985 0.047 Uiso 1 1 calc R . . H9B H 0.2726 0.2617 0.2075 0.047 Uiso 1 1 calc R . . H9C H 0.1701 0.2503 0.2014 0.047 Uiso 1 1 calc R . . C10 C 0.0478(5) 0.3959(4) 0.4714(5) 0.063(2) Uani 1 1 d . . . H10A H 0.1021 0.4085 0.4397 0.095 Uiso 1 1 calc R . . H10B H 0.0527 0.4150 0.5354 0.095 Uiso 1 1 calc R . . H10C H 0.0010 0.4302 0.4418 0.095 Uiso 1 1 calc R . . C11 C 0.1270(3) 0.1789(4) 0.5165(4) 0.0353(13) Uani 1 1 d . . . H11A H 0.1065 0.1214 0.5435 0.053 Uiso 1 1 calc R . . H11B H 0.1568 0.2151 0.5634 0.053 Uiso 1 1 calc R . . H11C H 0.1670 0.1653 0.4665 0.053 Uiso 1 1 calc R . . C12 C -0.1011(4) 0.2166(6) 0.5222(5) 0.070(2) Uani 1 1 d . . . H12A H -0.1434 0.2649 0.5096 0.105 Uiso 1 1 calc R . . H12B H -0.0951 0.2088 0.5885 0.105 Uiso 1 1 calc R . . H12C H -0.1207 0.1590 0.4948 0.105 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.01205(12) 0.01546(13) 0.02783(16) 0.00315(13) 0.00074(16) 0.00253(12) Sn2 0.02255(14) 0.02260(15) 0.01921(14) 0.00022(14) -0.00084(17) 0.00545(13) B1 0.017(4) 0.012(3) 0.020(4) 0.000 -0.003(3) 0.000 B2 0.011(3) 0.014(3) 0.024(4) 0.000 0.000(3) 0.000 N1 0.0141(18) 0.0083(15) 0.027(2) -0.0008(15) -0.0007(17) 0.0002(13) N2 0.0195(19) 0.0093(16) 0.022(2) 0.0011(14) -0.0013(17) -0.0005(14) C1 0.014(2) 0.0085(18) 0.024(3) -0.0005(16) -0.0001(18) 0.0016(15) C2 0.014(2) 0.0140(19) 0.026(3) -0.0016(18) -0.003(2) -0.0037(16) C3 0.018(2) 0.0098(19) 0.036(3) -0.0014(18) -0.004(2) -0.0016(17) C4 0.016(2) 0.0089(18) 0.029(3) 0.0021(19) 0.0028(19) -0.0010(15) C5 0.025(2) 0.016(2) 0.024(2) 0.0015(19) -0.001(2) -0.0011(19) C6 0.034(3) 0.012(2) 0.049(3) 0.006(2) 0.001(3) 0.0008(19) C7 0.024(3) 0.034(3) 0.046(3) 0.002(3) -0.013(3) -0.001(2) C8 0.033(3) 0.046(3) 0.038(3) 0.010(3) 0.014(3) 0.009(3) C9 0.023(3) 0.020(2) 0.050(4) 0.007(2) 0.005(3) 0.009(2) C10 0.127(7) 0.028(3) 0.035(3) -0.013(3) -0.038(4) 0.013(3) C11 0.036(3) 0.038(3) 0.033(3) -0.001(2) -0.007(3) 0.017(2) C12 0.030(3) 0.146(8) 0.033(4) 0.019(4) 0.013(3) -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 Sn1 N1 2.070(4) . ? Sn1 C7 2.118(5) . ? Sn1 C9 2.132(4) . ? Sn1 C8 2.137(5) . ? Sn2 N2 2.058(4) . ? Sn2 C10 2.112(5) . ? Sn2 C11 2.118(5) . ? Sn2 C12 2.140(6) . ? B1 N1 1.449(5) . ? B1 N1 1.449(5) 2 ? B1 B2 1.712(9) . ? B2 N2 1.447(5) . ? B2 N2 1.447(5) 2 ? N1 C1 1.406(5) . ? N2 C4 1.412(5) . ? C1 C2 1.389(5) . ? C1 C1 1.415(8) 2 ? C2 C3 1.402(6) . ? C2 H2 0.9500 . ? C3 C3 1.389(9) 2 ? C3 H3 0.9500 . ? C4 C4 1.381(10) 2 ? C4 C5 1.403(6) . ? C5 C6 1.395(6) . ? C5 H5 0.9500 . ? C6 C6 1.362(11) 2 ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sn1 C7 105.23(18) . . ? N1 Sn1 C9 106.73(16) . . ? C7 Sn1 C9 114.0(2) . . ? N1 Sn1 C8 106.05(19) . . ? C7 Sn1 C8 112.1(2) . . ? C9 Sn1 C8 111.9(2) . . ? N2 Sn2 C10 106.8(2) . . ? N2 Sn2 C11 106.12(18) . . ? C10 Sn2 C11 109.8(2) . . ? N2 Sn2 C12 104.5(2) . . ? C10 Sn2 C12 114.2(3) . . ? C11 Sn2 C12 114.6(2) . . ? N1 B1 N1 108.0(5) . 2 ? N1 B1 B2 126.0(2) . . ? N1 B1 B2 126.0(2) 2 . ? N2 B2 N2 107.5(5) . 2 ? N2 B2 B1 126.2(3) . . ? N2 B2 B1 126.2(3) 2 . ? C1 N1 B1 106.7(4) . . ? C1 N1 Sn1 121.1(3) . . ? B1 N1 Sn1 131.9(3) . . ? C4 N2 B2 106.5(4) . . ? C4 N2 Sn2 123.5(3) . . ? B2 N2 Sn2 129.8(3) . . ? C2 C1 N1 130.2(4) . . ? C2 C1 C1 120.4(2) . 2 ? N1 C1 C1 109.3(2) . 2 ? C1 C2 C3 118.8(4) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C3 C3 C2 120.8(2) 2 . ? C3 C3 H3 119.6 2 . ? C2 C3 H3 119.6 . . ? C4 C4 C5 120.8(3) 2 . ? C4 C4 N2 109.7(2) 2 . ? C5 C4 N2 129.5(4) . . ? C6 C5 C4 117.7(5) . . ? C6 C5 H5 121.1 . . ? C4 C5 H5 121.1 . . ? C6 C6 C5 121.4(3) 2 . ? C6 C6 H6 119.3 2 . ? C5 C6 H6 119.3 . . ? Sn1 C7 H7A 109.5 . . ? Sn1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Sn1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Sn1 C8 H8A 109.5 . . ? Sn1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Sn1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Sn1 C9 H9A 109.5 . . ? Sn1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Sn1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Sn2 C10 H10A 109.5 . . ? Sn2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Sn2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Sn2 C11 H11A 109.5 . . ? Sn2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Sn2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Sn2 C12 H12A 109.5 . . ? Sn2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Sn2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 B1 B2 N2 93.4(3) . . . . ? N1 B1 B2 N2 -86.6(3) 2 . . . ? N1 B1 B2 N2 -86.6(3) . . . 2 ? N1 B1 B2 N2 93.4(3) 2 . . 2 ? N1 B1 N1 C1 -0.1(2) 2 . . . ? B2 B1 N1 C1 179.9(2) . . . . ? N1 B1 N1 Sn1 173.2(4) 2 . . . ? B2 B1 N1 Sn1 -6.8(4) . . . . ? C7 Sn1 N1 C1 50.0(4) . . . . ? C9 Sn1 N1 C1 171.5(3) . . . . ? C8 Sn1 N1 C1 -69.0(4) . . . . ? C7 Sn1 N1 B1 -122.5(3) . . . . ? C9 Sn1 N1 B1 -1.0(4) . . . . ? C8 Sn1 N1 B1 118.5(3) . . . . ? N2 B2 N2 C4 0.0(2) 2 . . . ? B1 B2 N2 C4 -180.0(2) . . . . ? N2 B2 N2 Sn2 -175.4(4) 2 . . . ? B1 B2 N2 Sn2 4.6(4) . . . . ? C10 Sn2 N2 C4 169.7(4) . . . . ? C11 Sn2 N2 C4 52.6(4) . . . . ? C12 Sn2 N2 C4 -68.9(4) . . . . ? C10 Sn2 N2 B2 -15.5(4) . . . . ? C11 Sn2 N2 B2 -132.6(3) . . . . ? C12 Sn2 N2 B2 105.9(4) . . . . ? B1 N1 C1 C2 -179.3(4) . . . . ? Sn1 N1 C1 C2 6.5(7) . . . . ? B1 N1 C1 C1 0.4(6) . . . 2 ? Sn1 N1 C1 C1 -173.9(4) . . . 2 ? N1 C1 C2 C3 179.9(5) . . . . ? C1 C1 C2 C3 0.3(8) 2 . . . ? C1 C2 C3 C3 1.4(9) . . . 2 ? B2 N2 C4 C4 -0.1(6) . . . 2 ? Sn2 N2 C4 C4 175.8(4) . . . 2 ? B2 N2 C4 C5 -179.9(4) . . . . ? Sn2 N2 C4 C5 -4.1(7) . . . . ? C4 C4 C5 C6 0.6(8) 2 . . . ? N2 C4 C5 C6 -179.5(5) . . . . ? C4 C5 C6 C6 -1.6(9) . . . 2 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.315 _refine_diff_density_min -0.827 _refine_diff_density_rms 0.165 data_6 _database_code_depnum_ccdc_archive 'CCDC 848886' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H84 B2 Li4 N12 O2' _chemical_formula_sum 'C40 H84 B2 Li4 N12 O2' _chemical_formula_weight 814.57 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' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 21.3933(5) _cell_length_b 14.6257(4) _cell_length_c 16.3348(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5111.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9867 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 25.93 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.059 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1852 _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.996 _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_process_details 'SADABS-2008/1 - Bruker AXS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81286 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.35 _reflns_number_total 6381 _reflns_number_gt 4637 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0852P)^2^+2.6730P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6381 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1820 _refine_ls_wR_factor_gt 0.1641 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Li1 Li 0.39918(13) 0.84456(19) 0.17199(18) 0.0317(6) Uani 1 1 d . . . Li2 Li 0.39242(13) 0.6836(2) 0.11098(19) 0.0346(6) Uani 1 1 d . . . N1 N 0.47128(6) 0.76148(9) 0.12903(8) 0.0269(3) Uani 1 1 d . . . N2 N 0.57439(6) 0.73555(9) 0.17128(9) 0.0287(3) Uani 1 1 d . . . H2A H 0.6072 0.7253 0.2024 0.034 Uiso 1 1 calc R . . N3 N 0.37125(7) 0.94807(10) 0.08729(9) 0.0349(3) Uani 1 1 d . . . N4 N 0.38434(7) 0.95591(10) 0.26535(9) 0.0333(3) Uani 1 1 d . . . N5 N 0.34758(7) 0.63110(12) -0.01085(10) 0.0417(4) Uani 1 1 d . . . N6 N 0.40314(8) 0.54373(10) 0.13378(11) 0.0422(4) Uani 1 1 d . . . O1 O 0.33748(6) 0.74992(9) 0.17984(8) 0.0377(3) Uani 1 1 d . . . B1 B 0.51022(8) 0.74721(11) 0.19981(11) 0.0266(4) Uani 1 1 d . . . C1 C 0.51178(7) 0.75925(10) 0.06262(10) 0.0279(3) Uani 1 1 d . . . C2 C 0.49957(9) 0.76947(12) -0.02065(10) 0.0349(4) Uani 1 1 d . . . H2 H 0.4580 0.7797 -0.0390 0.042 Uiso 1 1 calc R . . C3 C 0.54846(10) 0.76462(12) -0.07725(12) 0.0412(4) Uani 1 1 d . . . H3 H 0.5398 0.7713 -0.1340 0.049 Uiso 1 1 calc R . . C4 C 0.60970(9) 0.75015(12) -0.05157(12) 0.0405(4) Uani 1 1 d . . . H4 H 0.6424 0.7478 -0.0909 0.049 Uiso 1 1 calc R . . C5 C 0.62343(8) 0.73921(11) 0.03083(12) 0.0357(4) Uani 1 1 d . . . H5 H 0.6652 0.7291 0.0484 0.043 Uiso 1 1 calc R . . C6 C 0.57478(7) 0.74333(10) 0.08710(10) 0.0288(3) Uani 1 1 d . . . C7 C 0.33989(9) 1.01798(13) 0.13748(11) 0.0403(4) Uani 1 1 d . . . H7A H 0.2975 0.9964 0.1523 0.048 Uiso 1 1 calc R . . H7B H 0.3353 1.0749 0.1052 0.048 Uiso 1 1 calc R . . C8 C 0.37639(10) 1.03801(12) 0.21446(11) 0.0390(4) Uani 1 1 d . . . H8A H 0.4180 1.0624 0.1995 0.047 Uiso 1 1 calc R . . H8B H 0.3543 1.0855 0.2465 0.047 Uiso 1 1 calc R . . C9 C 0.42584(9) 0.98758(13) 0.04622(11) 0.0403(4) Uani 1 1 d . . . H9A H 0.4467 0.9403 0.0137 0.061 Uiso 1 1 calc R . . H9B H 0.4549 1.0115 0.0873 0.061 Uiso 1 1 calc R . . H9C H 0.4124 1.0374 0.0102 0.061 Uiso 1 1 calc R . . C10 C 0.32799(10) 0.91229(15) 0.02633(12) 0.0471(5) Uani 1 1 d . . . H10A H 0.3136 0.9622 -0.0090 0.071 Uiso 1 1 calc R . . H10B H 0.2920 0.8846 0.0539 0.071 Uiso 1 1 calc R . . H10C H 0.3492 0.8660 -0.0070 0.071 Uiso 1 1 calc R . . C11 C 0.32539(9) 0.93296(13) 0.30682(12) 0.0407(4) Uani 1 1 d . . . H11A H 0.3116 0.9852 0.3397 0.061 Uiso 1 1 calc R . . H11B H 0.3319 0.8800 0.3425 0.061 Uiso 1 1 calc R . . H11C H 0.2934 0.9184 0.2659 0.061 Uiso 1 1 calc R . . C12 C 0.43151(9) 0.97389(14) 0.32773(11) 0.0420(4) Uani 1 1 d . . . H12A H 0.4715 0.9875 0.3013 0.063 Uiso 1 1 calc R . . H12B H 0.4361 0.9199 0.3628 0.063 Uiso 1 1 calc R . . H12C H 0.4185 1.0263 0.3611 0.063 Uiso 1 1 calc R . . C13 C 0.35918(11) 0.53244(15) -0.00592(15) 0.0559(6) Uani 1 1 d . . . H13A H 0.4004 0.5190 -0.0306 0.067 Uiso 1 1 calc R . . H13B H 0.3271 0.5000 -0.0385 0.067 Uiso 1 1 calc R . . C14 C 0.35812(11) 0.49654(14) 0.07971(15) 0.0552(6) Uani 1 1 d . . . H14A H 0.3155 0.5038 0.1024 0.066 Uiso 1 1 calc R . . H14B H 0.3680 0.4304 0.0788 0.066 Uiso 1 1 calc R . . C15 C 0.36140(12) 0.6616(2) -0.09412(14) 0.0631(7) Uani 1 1 d . . . H15A H 0.3348 0.6284 -0.1329 0.095 Uiso 1 1 calc R . . H15B H 0.4054 0.6495 -0.1066 0.095 Uiso 1 1 calc R . . H15C H 0.3532 0.7273 -0.0986 0.095 Uiso 1 1 calc R . . C16 C 0.28198(9) 0.65155(16) 0.00749(15) 0.0528(6) Uani 1 1 d . . . H16A H 0.2746 0.7173 0.0014 0.079 Uiso 1 1 calc R . . H16B H 0.2725 0.6331 0.0638 0.079 Uiso 1 1 calc R . . H16C H 0.2550 0.6179 -0.0304 0.079 Uiso 1 1 calc R . . C17 C 0.46765(11) 0.52378(16) 0.11106(17) 0.0591(6) Uani 1 1 d . . . H17A H 0.4960 0.5509 0.1514 0.089 Uiso 1 1 calc R . . H17B H 0.4764 0.5496 0.0569 0.089 Uiso 1 1 calc R . . H17C H 0.4739 0.4574 0.1096 0.089 Uiso 1 1 calc R . . C18 C 0.39174(15) 0.51605(17) 0.21800(15) 0.0676(7) Uani 1 1 d . . . H18A H 0.3999 0.4504 0.2238 0.101 Uiso 1 1 calc R . . H18B H 0.3481 0.5288 0.2324 0.101 Uiso 1 1 calc R . . H18C H 0.4195 0.5502 0.2546 0.101 Uiso 1 1 calc R . . C19A C 0.28084(10) 0.74527(18) 0.20394(17) 0.0629(7) Uani 1 1 d . . . H19A H 0.2566 0.7273 0.1549 0.075 Uiso 1 1 calc R . . H19B H 0.2686 0.8091 0.2161 0.075 Uiso 1 1 calc R . . C20A C 0.25720(16) 0.6958(3) 0.2650(2) 0.1210(17) Uani 1 1 d . . . H20A H 0.2658 0.6309 0.2552 0.182 Uiso 1 1 calc R . . H20B H 0.2119 0.7054 0.2679 0.182 Uiso 1 1 calc R . . H20C H 0.2765 0.7146 0.3168 0.182 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.0292(14) 0.0315(14) 0.0343(15) -0.0010(11) 0.0008(11) 0.0013(11) Li2 0.0263(13) 0.0370(15) 0.0406(16) -0.0049(12) 0.0004(12) -0.0016(11) N1 0.0238(6) 0.0281(6) 0.0290(7) -0.0022(5) 0.0018(5) -0.0013(5) N2 0.0214(6) 0.0293(7) 0.0355(7) -0.0003(5) 0.0003(5) 0.0012(5) N3 0.0362(8) 0.0377(8) 0.0307(7) 0.0014(6) -0.0015(6) 0.0071(6) N4 0.0376(8) 0.0327(7) 0.0294(7) 0.0008(6) 0.0031(6) 0.0041(6) N5 0.0317(8) 0.0499(9) 0.0435(9) -0.0108(7) -0.0057(7) -0.0014(7) N6 0.0432(9) 0.0336(8) 0.0499(9) -0.0051(7) -0.0054(7) -0.0031(6) O1 0.0327(6) 0.0417(7) 0.0386(7) -0.0080(5) 0.0026(5) 0.0047(5) B1 0.0221(8) 0.0240(8) 0.0336(9) -0.0005(7) 0.0015(7) -0.0003(6) C1 0.0277(8) 0.0235(7) 0.0326(8) -0.0043(6) 0.0032(6) -0.0026(6) C2 0.0380(9) 0.0342(8) 0.0323(9) -0.0037(7) 0.0004(7) -0.0018(7) C3 0.0564(12) 0.0361(9) 0.0310(9) -0.0049(7) 0.0088(8) -0.0025(8) C4 0.0469(11) 0.0313(9) 0.0435(10) -0.0055(7) 0.0204(9) -0.0010(7) C5 0.0312(8) 0.0277(8) 0.0483(10) -0.0039(7) 0.0129(8) -0.0006(6) C6 0.0275(8) 0.0229(7) 0.0360(9) -0.0028(6) 0.0043(6) -0.0015(6) C7 0.0427(10) 0.0385(9) 0.0397(10) 0.0054(8) 0.0021(8) 0.0142(8) C8 0.0500(11) 0.0304(8) 0.0364(9) 0.0016(7) 0.0052(8) 0.0078(8) C9 0.0457(10) 0.0428(10) 0.0326(9) 0.0040(7) 0.0036(8) 0.0053(8) C10 0.0474(11) 0.0526(11) 0.0412(10) 0.0002(9) -0.0092(9) 0.0059(9) C11 0.0430(10) 0.0406(10) 0.0384(10) -0.0008(8) 0.0101(8) 0.0056(8) C12 0.0497(11) 0.0436(10) 0.0327(9) -0.0032(7) -0.0016(8) -0.0009(8) C13 0.0519(13) 0.0520(12) 0.0638(14) -0.0250(11) -0.0156(11) 0.0037(10) C14 0.0555(13) 0.0357(10) 0.0745(15) -0.0123(10) -0.0124(11) -0.0079(9) C15 0.0610(14) 0.0849(18) 0.0435(12) -0.0123(12) -0.0115(11) -0.0149(13) C16 0.0285(10) 0.0571(12) 0.0729(15) -0.0178(11) -0.0114(10) -0.0027(8) C17 0.0493(12) 0.0434(11) 0.0844(17) -0.0102(11) -0.0091(12) 0.0121(9) C18 0.095(2) 0.0464(12) 0.0620(15) 0.0074(11) -0.0050(14) -0.0139(12) C19A 0.0387(11) 0.0715(15) 0.0785(17) -0.0405(13) 0.0027(11) -0.0186(10) C20A 0.095(2) 0.149(3) 0.119(3) -0.087(3) 0.071(2) -0.089(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 Li1 O1 1.917(3) . ? Li1 N1 2.085(3) . ? Li1 N3 2.136(3) . ? Li1 N4 2.254(3) . ? Li1 Li2 2.560(4) . ? Li1 B1 2.807(3) . ? Li2 O1 1.894(3) . ? Li2 N1 2.057(3) . ? Li2 N6 2.092(3) . ? Li2 N5 2.339(3) . ? N1 C1 1.389(2) . ? N1 B1 1.440(2) . ? N2 C6 1.380(2) . ? N2 B1 1.460(2) . ? N2 H2A 0.8800 . ? N3 C10 1.457(2) . ? N3 C9 1.465(2) . ? N3 C7 1.472(2) . ? N4 C12 1.458(2) . ? N4 C11 1.470(2) . ? N4 C8 1.470(2) . ? N5 C15 1.462(3) . ? N5 C16 1.466(2) . ? N5 C13 1.466(3) . ? N6 C18 1.455(3) . ? N6 C17 1.459(3) . ? N6 C14 1.478(3) . ? O1 C19A 1.276(2) . ? B1 B1 1.697(4) 3_655 ? C1 C2 1.393(2) . ? C1 C6 1.425(2) . ? C2 C3 1.398(3) . ? C2 H2 0.9500 . ? C3 C4 1.392(3) . ? C3 H3 0.9500 . ? C4 C5 1.387(3) . ? C4 H4 0.9500 . ? C5 C6 1.390(2) . ? C5 H5 0.9500 . ? C7 C8 1.509(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.494(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19A C20A 1.332(4) . ? C19A H19A 0.9900 . ? C19A H19B 0.9900 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Li1 N1 96.38(13) . . ? O1 Li1 N3 111.25(14) . . ? N1 Li1 N3 113.69(14) . . ? O1 Li1 N4 112.31(14) . . ? N1 Li1 N4 138.85(15) . . ? N3 Li1 N4 83.50(11) . . ? O1 Li1 Li2 47.41(9) . . ? N1 Li1 Li2 51.32(9) . . ? N3 Li1 Li2 112.56(14) . . ? N4 Li1 Li2 156.91(15) . . ? O1 Li1 B1 101.87(12) . . ? N1 Li1 B1 29.86(7) . . ? N3 Li1 B1 134.52(14) . . ? N4 Li1 B1 112.10(12) . . ? Li2 Li1 B1 69.17(10) . . ? O1 Li2 N1 98.08(14) . . ? O1 Li2 N6 117.58(16) . . ? N1 Li2 N6 115.21(15) . . ? O1 Li2 N5 114.77(14) . . ? N1 Li2 N5 129.81(15) . . ? N6 Li2 N5 82.83(12) . . ? O1 Li2 Li1 48.18(10) . . ? N1 Li2 Li1 52.33(10) . . ? N6 Li2 Li1 145.44(17) . . ? N5 Li2 Li1 131.03(15) . . ? C1 N1 B1 105.24(13) . . ? C1 N1 Li2 112.76(13) . . ? B1 N1 Li2 120.62(13) . . ? C1 N1 Li1 137.57(13) . . ? B1 N1 Li1 104.01(13) . . ? Li2 N1 Li1 76.35(12) . . ? C6 N2 B1 108.32(14) . . ? C6 N2 H2A 125.8 . . ? B1 N2 H2A 125.8 . . ? C10 N3 C9 109.58(15) . . ? C10 N3 C7 109.90(15) . . ? C9 N3 C7 110.13(15) . . ? C10 N3 Li1 111.46(14) . . ? C9 N3 Li1 110.68(13) . . ? C7 N3 Li1 105.01(13) . . ? C12 N4 C11 108.23(14) . . ? C12 N4 C8 109.14(15) . . ? C11 N4 C8 110.35(14) . . ? C12 N4 Li1 120.38(13) . . ? C11 N4 Li1 105.52(13) . . ? C8 N4 Li1 102.94(12) . . ? C15 N5 C16 108.76(18) . . ? C15 N5 C13 108.48(19) . . ? C16 N5 C13 110.59(17) . . ? C15 N5 Li2 127.49(15) . . ? C16 N5 Li2 98.73(14) . . ? C13 N5 Li2 101.96(14) . . ? C18 N6 C17 110.1(2) . . ? C18 N6 C14 109.03(18) . . ? C17 N6 C14 111.78(17) . . ? C18 N6 Li2 114.97(16) . . ? C17 N6 Li2 104.72(15) . . ? C14 N6 Li2 106.19(15) . . ? C19A O1 Li2 138.19(16) . . ? C19A O1 Li1 135.49(16) . . ? Li2 O1 Li1 84.41(13) . . ? N1 B1 N2 107.73(14) . . ? N1 B1 B1 128.81(17) . 3_655 ? N2 B1 B1 123.42(18) . 3_655 ? N1 B1 Li1 46.13(9) . . ? N2 B1 Li1 143.47(13) . . ? B1 B1 Li1 86.47(12) 3_655 . ? N1 C1 C2 130.03(15) . . ? N1 C1 C6 112.01(14) . . ? C2 C1 C6 117.97(15) . . ? C1 C2 C3 120.00(17) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 120.84(18) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C5 C4 C3 120.63(17) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 118.56(17) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? N2 C6 C5 131.31(16) . . ? N2 C6 C1 106.70(14) . . ? C5 C6 C1 121.98(16) . . ? N3 C7 C8 111.28(14) . . ? N3 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? N3 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? N4 C8 C7 111.87(15) . . ? N4 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? N4 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N3 C10 H10A 109.5 . . ? N3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C11 H11A 109.5 . . ? N4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 H12A 109.5 . . ? N4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N5 C13 C14 113.24(18) . . ? N5 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? N5 C13 H13B 108.9 . . ? C14 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? N6 C14 C13 112.67(18) . . ? N6 C14 H14A 109.1 . . ? C13 C14 H14A 109.1 . . ? N6 C14 H14B 109.1 . . ? C13 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? N5 C15 H15A 109.5 . . ? N5 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N5 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N5 C16 H16A 109.5 . . ? N5 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N5 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N6 C17 H17A 109.5 . . ? N6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N6 C18 H18A 109.5 . . ? N6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 C19A C20A 128.4(3) . . ? O1 C19A H19A 105.2 . . ? C20A C19A H19A 105.2 . . ? O1 C19A H19B 105.2 . . ? C20A C19A H19B 105.2 . . ? H19A C19A H19B 105.9 . . ? C19A C20A H20A 109.5 . . ? C19A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? C19A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Li1 Li2 O1 158.31(17) . . . . ? N3 Li1 Li2 O1 -98.70(16) . . . . ? N4 Li1 Li2 O1 32.7(4) . . . . ? B1 Li1 Li2 O1 130.44(14) . . . . ? O1 Li1 Li2 N1 -158.31(17) . . . . ? N3 Li1 Li2 N1 102.99(15) . . . . ? N4 Li1 Li2 N1 -125.6(4) . . . . ? B1 Li1 Li2 N1 -27.87(7) . . . . ? O1 Li1 Li2 N6 -78.2(3) . . . . ? N1 Li1 Li2 N6 80.1(3) . . . . ? N3 Li1 Li2 N6 -176.9(2) . . . . ? N4 Li1 Li2 N6 -45.5(5) . . . . ? B1 Li1 Li2 N6 52.2(3) . . . . ? O1 Li1 Li2 N5 88.09(19) . . . . ? N1 Li1 Li2 N5 -113.6(2) . . . . ? N3 Li1 Li2 N5 -10.6(2) . . . . ? N4 Li1 Li2 N5 120.8(4) . . . . ? B1 Li1 Li2 N5 -141.47(18) . . . . ? O1 Li2 N1 C1 -152.36(13) . . . . ? N6 Li2 N1 C1 81.93(19) . . . . ? N5 Li2 N1 C1 -20.3(2) . . . . ? Li1 Li2 N1 C1 -136.21(15) . . . . ? O1 Li2 N1 B1 82.22(17) . . . . ? N6 Li2 N1 B1 -43.5(2) . . . . ? N5 Li2 N1 B1 -145.76(17) . . . . ? Li1 Li2 N1 B1 98.38(15) . . . . ? O1 Li2 N1 Li1 -16.16(13) . . . . ? N6 Li2 N1 Li1 -141.86(18) . . . . ? N5 Li2 N1 Li1 115.9(2) . . . . ? O1 Li1 N1 C1 124.82(17) . . . . ? N3 Li1 N1 C1 8.2(3) . . . . ? N4 Li1 N1 C1 -100.1(3) . . . . ? Li2 Li1 N1 C1 108.9(2) . . . . ? B1 Li1 N1 C1 -132.4(2) . . . . ? O1 Li1 N1 B1 -102.76(14) . . . . ? N3 Li1 N1 B1 140.66(14) . . . . ? N4 Li1 N1 B1 32.3(3) . . . . ? Li2 Li1 N1 B1 -118.66(14) . . . . ? O1 Li1 N1 Li2 15.89(13) . . . . ? N3 Li1 N1 Li2 -100.68(16) . . . . ? N4 Li1 N1 Li2 151.0(2) . . . . ? B1 Li1 N1 Li2 118.66(14) . . . . ? O1 Li1 N3 C10 -25.4(2) . . . . ? N1 Li1 N3 C10 82.16(18) . . . . ? N4 Li1 N3 C10 -136.80(14) . . . . ? Li2 Li1 N3 C10 25.99(19) . . . . ? B1 Li1 N3 C10 108.4(2) . . . . ? O1 Li1 N3 C9 -147.58(15) . . . . ? N1 Li1 N3 C9 -40.07(19) . . . . ? N4 Li1 N3 C9 100.98(14) . . . . ? Li2 Li1 N3 C9 -96.24(17) . . . . ? B1 Li1 N3 C9 -13.8(2) . . . . ? O1 Li1 N3 C7 93.60(17) . . . . ? N1 Li1 N3 C7 -158.89(15) . . . . ? N4 Li1 N3 C7 -17.84(14) . . . . ? Li2 Li1 N3 C7 144.94(15) . . . . ? B1 Li1 N3 C7 -132.62(18) . . . . ? O1 Li1 N4 C12 117.47(17) . . . . ? N1 Li1 N4 C12 -13.2(3) . . . . ? N3 Li1 N4 C12 -132.19(14) . . . . ? Li2 Li1 N4 C12 92.0(4) . . . . ? B1 Li1 N4 C12 3.48(19) . . . . ? O1 Li1 N4 C11 -5.16(19) . . . . ? N1 Li1 N4 C11 -135.9(2) . . . . ? N3 Li1 N4 C11 105.17(13) . . . . ? Li2 Li1 N4 C11 -30.6(4) . . . . ? B1 Li1 N4 C11 -119.16(14) . . . . ? O1 Li1 N4 C8 -120.89(16) . . . . ? N1 Li1 N4 C8 108.4(2) . . . . ? N3 Li1 N4 C8 -10.55(14) . . . . ? Li2 Li1 N4 C8 -146.4(4) . . . . ? B1 Li1 N4 C8 125.12(14) . . . . ? O1 Li2 N5 C15 111.8(2) . . . . ? N1 Li2 N5 C15 -14.1(3) . . . . ? N6 Li2 N5 C15 -131.1(2) . . . . ? Li1 Li2 N5 C15 56.6(3) . . . . ? O1 Li2 N5 C16 -10.1(2) . . . . ? N1 Li2 N5 C16 -136.0(2) . . . . ? N6 Li2 N5 C16 107.02(15) . . . . ? Li1 Li2 N5 C16 -65.2(2) . . . . ? O1 Li2 N5 C13 -123.43(18) . . . . ? N1 Li2 N5 C13 110.7(2) . . . . ? N6 Li2 N5 C13 -6.32(16) . . . . ? Li1 Li2 N5 C13 -178.54(19) . . . . ? O1 Li2 N6 C18 -26.6(2) . . . . ? N1 Li2 N6 C18 88.3(2) . . . . ? N5 Li2 N6 C18 -140.82(17) . . . . ? Li1 Li2 N6 C18 28.8(3) . . . . ? O1 Li2 N6 C17 -147.51(18) . . . . ? N1 Li2 N6 C17 -32.6(2) . . . . ? N5 Li2 N6 C17 98.24(15) . . . . ? Li1 Li2 N6 C17 -92.1(3) . . . . ? O1 Li2 N6 C14 94.1(2) . . . . ? N1 Li2 N6 C14 -151.02(17) . . . . ? N5 Li2 N6 C14 -20.17(16) . . . . ? Li1 Li2 N6 C14 149.5(3) . . . . ? N1 Li2 O1 C19A -177.9(2) . . . . ? N6 Li2 O1 C19A -53.9(3) . . . . ? N5 Li2 O1 C19A 41.0(3) . . . . ? Li1 Li2 O1 C19A 164.9(3) . . . . ? N1 Li2 O1 Li1 17.19(14) . . . . ? N6 Li2 O1 Li1 141.21(17) . . . . ? N5 Li2 O1 Li1 -123.86(17) . . . . ? N1 Li1 O1 C19A 177.5(2) . . . . ? N3 Li1 O1 C19A -64.0(3) . . . . ? N4 Li1 O1 C19A 27.6(3) . . . . ? Li2 Li1 O1 C19A -165.6(3) . . . . ? B1 Li1 O1 C19A 147.7(2) . . . . ? N1 Li1 O1 Li2 -16.88(13) . . . . ? N3 Li1 O1 Li2 101.63(16) . . . . ? N4 Li1 O1 Li2 -166.75(16) . . . . ? B1 Li1 O1 Li2 -46.63(13) . . . . ? C1 N1 B1 N2 -0.72(16) . . . . ? Li2 N1 B1 N2 128.12(14) . . . . ? Li1 N1 B1 N2 -149.64(13) . . . . ? C1 N1 B1 B1 176.93(9) . . . 3_655 ? Li2 N1 B1 B1 -54.23(16) . . . 3_655 ? Li1 N1 B1 B1 28.01(14) . . . 3_655 ? C1 N1 B1 Li1 148.92(16) . . . . ? Li2 N1 B1 Li1 -82.24(15) . . . . ? C6 N2 B1 N1 0.62(17) . . . . ? C6 N2 B1 B1 -177.19(8) . . . 3_655 ? C6 N2 B1 Li1 -37.1(3) . . . . ? O1 Li1 B1 N1 82.07(15) . . . . ? N3 Li1 B1 N1 -54.49(19) . . . . ? N4 Li1 B1 N1 -157.67(18) . . . . ? Li2 Li1 B1 N1 47.13(12) . . . . ? O1 Li1 B1 N2 136.0(2) . . . . ? N1 Li1 B1 N2 54.0(2) . . . . ? N3 Li1 B1 N2 -0.5(3) . . . . ? N4 Li1 B1 N2 -103.7(2) . . . . ? Li2 Li1 B1 N2 101.1(2) . . . . ? O1 Li1 B1 B1 -76.42(12) . . . 3_655 ? N1 Li1 B1 B1 -158.49(14) . . . 3_655 ? N3 Li1 B1 B1 147.02(18) . . . 3_655 ? N4 Li1 B1 B1 43.84(13) . . . 3_655 ? Li2 Li1 B1 B1 -111.35(11) . . . 3_655 ? B1 N1 C1 C2 -179.82(16) . . . . ? Li2 N1 C1 C2 46.8(2) . . . . ? Li1 N1 C1 C2 -47.8(3) . . . . ? B1 N1 C1 C6 0.59(17) . . . . ? Li2 N1 C1 C6 -132.78(14) . . . . ? Li1 N1 C1 C6 132.65(18) . . . . ? N1 C1 C2 C3 179.99(16) . . . . ? C6 C1 C2 C3 -0.4(2) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? C2 C3 C4 C5 0.7(3) . . . . ? C3 C4 C5 C6 -0.2(2) . . . . ? B1 N2 C6 C5 178.82(16) . . . . ? B1 N2 C6 C1 -0.25(17) . . . . ? C4 C5 C6 N2 -179.58(16) . . . . ? C4 C5 C6 C1 -0.6(2) . . . . ? N1 C1 C6 N2 -0.22(17) . . . . ? C2 C1 C6 N2 -179.87(14) . . . . ? N1 C1 C6 C5 -179.40(14) . . . . ? C2 C1 C6 C5 1.0(2) . . . . ? C10 N3 C7 C8 164.59(16) . . . . ? C9 N3 C7 C8 -74.59(18) . . . . ? Li1 N3 C7 C8 44.59(19) . . . . ? C12 N4 C8 C7 166.77(15) . . . . ? C11 N4 C8 C7 -74.41(19) . . . . ? Li1 N4 C8 C7 37.80(18) . . . . ? N3 C7 C8 N4 -59.4(2) . . . . ? C15 N5 C13 C14 169.31(19) . . . . ? C16 N5 C13 C14 -71.5(2) . . . . ? Li2 N5 C13 C14 32.7(2) . . . . ? C18 N6 C14 C13 170.4(2) . . . . ? C17 N6 C14 C13 -67.7(2) . . . . ? Li2 N6 C14 C13 46.0(2) . . . . ? N5 C13 C14 N6 -56.4(3) . . . . ? Li2 O1 C19A C20A 83.4(4) . . . . ? Li1 O1 C19A C20A -118.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.800 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.047 data_7 _database_code_depnum_ccdc_archive 'CCDC 848887' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H68 B2 N4 Sn4, 4(C4 H8 O)' _chemical_formula_sum 'C100 H100 B2 N4 O4 Sn4' _chemical_formula_weight 1918.22 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3291(5) _cell_length_b 13.4745(9) _cell_length_c 13.7149(5) _cell_angle_alpha 95.346(3) _cell_angle_beta 118.325(2) _cell_angle_gamma 94.865(3) _cell_volume 2135.36(18) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9944 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 25.77 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 970 _exptl_absorpt_coefficient_mu 1.212 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6639 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_process_details 'SADABS V2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II kappa CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41781 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 25.77 _reflns_number_total 8141 _reflns_number_gt 6525 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+21.0103P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8141 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1454 _refine_ls_wR_factor_gt 0.1365 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _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 B1 B 0.4359(6) -0.0344(5) -0.0336(7) 0.0150(15) Uani 1 1 d . . . N1 N 0.3931(4) -0.0795(4) 0.0289(4) 0.0144(11) Uani 1 1 d . . . N2 N 0.6258(4) 0.0427(4) 0.1548(4) 0.0142(11) Uani 1 1 d . . . C1 C 0.4773(5) -0.0948(5) 0.1403(5) 0.0150(13) Uani 1 1 d . . . C2 C 0.5876(6) -0.0334(5) 0.2006(5) 0.0148(13) Uani 1 1 d . . . C3 C 0.6629(6) -0.0537(5) 0.3073(5) 0.0166(13) Uani 1 1 d . . . H3 H 0.7362 -0.0131 0.3490 0.020 Uiso 1 1 calc R . . C4 C 0.6353(6) -0.1307(5) 0.3552(6) 0.0186(14) Uani 1 1 d . . . H4 H 0.6880 -0.1410 0.4289 0.022 Uiso 1 1 calc R . . C5 C 0.5303(6) -0.1920(5) 0.2942(6) 0.0181(14) Uani 1 1 d . . . H5 H 0.5115 -0.2468 0.3244 0.022 Uiso 1 1 calc R . . C6 C 0.4529(6) -0.1734(5) 0.1894(6) 0.0156(13) Uani 1 1 d . . . H6 H 0.3803 -0.2153 0.1489 0.019 Uiso 1 1 calc R . . Sn1 Sn 0.23412(4) -0.05503(3) 0.00994(4) 0.01345(13) Uani 1 1 d . . . C7 C 0.0939(6) -0.1608(5) -0.1174(6) 0.0172(14) Uani 1 1 d . . . C8 C 0.0950(6) -0.2639(6) -0.1195(6) 0.0244(16) Uani 1 1 d . . . H8 H 0.1620 -0.2880 -0.0673 0.029 Uiso 1 1 calc R . . C9 C 0.0001(7) -0.3319(6) -0.1963(7) 0.0311(18) Uani 1 1 d . . . H9 H 0.0021 -0.4023 -0.1971 0.037 Uiso 1 1 calc R . . C10 C -0.1002(6) -0.2963(7) -0.2737(7) 0.035(2) Uani 1 1 d . . . H10 H -0.1659 -0.3419 -0.3277 0.042 Uiso 1 1 calc R . . C11 C -0.0999(6) -0.1930(5) -0.2688(5) 0.0211(15) Uani 1 1 d . . . H11 H -0.1672 -0.1679 -0.3192 0.025 Uiso 1 1 calc R . . C12 C -0.0052(6) -0.1266(6) -0.1932(6) 0.0215(15) Uani 1 1 d . . . H12 H -0.0071 -0.0562 -0.1926 0.026 Uiso 1 1 calc R . . C13 C 0.2162(6) 0.0980(5) -0.0197(6) 0.0167(13) Uani 1 1 d . . . C14 C 0.2423(6) 0.1456(5) -0.0925(6) 0.0221(15) Uani 1 1 d . . . H14 H 0.2699 0.1091 -0.1352 0.027 Uiso 1 1 calc R . . C15 C 0.2287(6) 0.2450(6) -0.1034(7) 0.0246(16) Uani 1 1 d . . . H15 H 0.2481 0.2766 -0.1525 0.030 Uiso 1 1 calc R . . C16 C 0.1867(6) 0.2988(5) -0.0431(6) 0.0233(15) Uani 1 1 d . . . H16 H 0.1755 0.3667 -0.0522 0.028 Uiso 1 1 calc R . . C17 C 0.1612(6) 0.2534(5) 0.0303(6) 0.0215(15) Uani 1 1 d . . . H17 H 0.1331 0.2900 0.0726 0.026 Uiso 1 1 calc R . . C18 C 0.1769(6) 0.1536(5) 0.0419(6) 0.0186(14) Uani 1 1 d . . . H18 H 0.1604 0.1228 0.0933 0.022 Uiso 1 1 calc R . . C19 C 0.2250(6) -0.0645(5) 0.1606(6) 0.0168(13) Uani 1 1 d . . . C20 C 0.1241(6) -0.1162(5) 0.1486(6) 0.0201(14) Uani 1 1 d . . . H20 H 0.0670 -0.1501 0.0769 0.024 Uiso 1 1 calc R . . C21 C 0.1053(6) -0.1191(6) 0.2399(6) 0.0244(16) Uani 1 1 d . . . H21 H 0.0361 -0.1550 0.2305 0.029 Uiso 1 1 calc R . . C22 C 0.1877(6) -0.0696(6) 0.3440(6) 0.0234(16) Uani 1 1 d . . . H22 H 0.1749 -0.0708 0.4064 0.028 Uiso 1 1 calc R . . C23 C 0.2893(7) -0.0179(6) 0.3580(6) 0.0238(15) Uani 1 1 d . . . H23 H 0.3461 0.0159 0.4298 0.029 Uiso 1 1 calc R . . C24 C 0.3076(6) -0.0157(5) 0.2664(6) 0.0189(14) Uani 1 1 d . . . H24 H 0.3774 0.0195 0.2762 0.023 Uiso 1 1 calc R . . Sn2 Sn 0.68156(4) 0.18388(3) 0.25285(4) 0.01411(13) Uani 1 1 d . . . C25 C 0.8504(6) 0.1907(5) 0.3921(6) 0.0185(14) Uani 1 1 d . . . C26 C 0.9238(6) 0.1232(6) 0.3924(6) 0.0226(15) Uani 1 1 d . . . H26 H 0.9001 0.0740 0.3284 0.027 Uiso 1 1 calc R . . C27 C 1.0314(6) 0.1272(6) 0.4854(7) 0.0305(18) Uani 1 1 d . . . H27 H 1.0817 0.0815 0.4848 0.037 Uiso 1 1 calc R . . C28 C 1.0648(7) 0.1975(6) 0.5784(7) 0.0301(18) Uani 1 1 d . . . H28 H 1.1385 0.2003 0.6421 0.036 Uiso 1 1 calc R . . C29 C 0.9931(7) 0.2637(6) 0.5804(6) 0.0318(18) Uani 1 1 d . . . H29 H 1.0170 0.3108 0.6461 0.038 Uiso 1 1 calc R . . C30 C 0.8861(6) 0.2629(6) 0.4880(6) 0.0253(16) Uani 1 1 d . . . H30 H 0.8376 0.3102 0.4892 0.030 Uiso 1 1 calc R . . C31 C 0.6668(6) 0.3022(5) 0.1562(6) 0.0173(14) Uani 1 1 d . . . C32 C 0.7533(6) 0.3857(5) 0.2022(6) 0.0232(15) Uani 1 1 d . . . H32 H 0.8192 0.3865 0.2731 0.028 Uiso 1 1 calc R . . C33 C 0.7439(7) 0.4677(6) 0.1453(7) 0.0272(17) Uani 1 1 d . . . H33 H 0.8031 0.5242 0.1775 0.033 Uiso 1 1 calc R . . C34 C 0.6493(8) 0.4670(6) 0.0428(7) 0.0320(18) Uani 1 1 d . . . H34 H 0.6435 0.5227 0.0036 0.038 Uiso 1 1 calc R . . C35 C 0.5621(7) 0.3852(6) -0.0039(7) 0.0295(17) Uani 1 1 d . . . H35 H 0.4965 0.3853 -0.0747 0.035 Uiso 1 1 calc R . . C36 C 0.5700(6) 0.3035(5) 0.0517(6) 0.0210(15) Uani 1 1 d . . . H36 H 0.5096 0.2479 0.0192 0.025 Uiso 1 1 calc R . . C37 C 0.5666(6) 0.2016(5) 0.3188(6) 0.0193(14) Uani 1 1 d . . . C38 C 0.5939(6) 0.1749(6) 0.4236(6) 0.0233(15) Uani 1 1 d . . . H38 H 0.6607 0.1440 0.4623 0.028 Uiso 1 1 calc R . . C39 C 0.5252(6) 0.1928(6) 0.4726(6) 0.0222(15) Uani 1 1 d . . . H39 H 0.5435 0.1722 0.5428 0.027 Uiso 1 1 calc R . . C40 C 0.4299(6) 0.2407(5) 0.4181(6) 0.0234(15) Uani 1 1 d . . . H40 H 0.3844 0.2554 0.4524 0.028 Uiso 1 1 calc R . . C41 C 0.4007(6) 0.2672(6) 0.3141(6) 0.0238(16) Uani 1 1 d . . . H41 H 0.3341 0.2985 0.2763 0.029 Uiso 1 1 calc R . . C42 C 0.4684(6) 0.2482(5) 0.2643(6) 0.0229(15) Uani 1 1 d . . . H42 H 0.4480 0.2670 0.1929 0.027 Uiso 1 1 calc R . . C45 C 0.1286(11) 0.6119(9) 0.1757(14) 0.087(5) Uani 1 1 d . . . H45A H 0.0845 0.6605 0.1282 0.104 Uiso 1 1 calc R . . H45B H 0.0827 0.5782 0.2058 0.104 Uiso 1 1 calc R . . C44 C 0.1615(9) 0.5354(8) 0.1105(9) 0.050(3) Uani 1 1 d . . . H44A H 0.1055 0.4725 0.0792 0.060 Uiso 1 1 calc R . . H44B H 0.1680 0.5634 0.0492 0.060 Uiso 1 1 calc R . . C43 C 0.2751(10) 0.5186(10) 0.2000(9) 0.062(3) Uani 1 1 d . . . H43A H 0.2646 0.4678 0.2433 0.075 Uiso 1 1 calc R . . H43B H 0.3214 0.4935 0.1666 0.075 Uiso 1 1 calc R . . O1 O 0.3314(7) 0.6099(6) 0.2701(8) 0.071(2) Uani 1 1 d . . . C46 C 0.2455(9) 0.6636(8) 0.2696(8) 0.047(2) Uani 1 1 d . . . H46A H 0.2597 0.7337 0.2580 0.057 Uiso 1 1 calc R . . H46B H 0.2467 0.6657 0.3425 0.057 Uiso 1 1 calc R . . C48 C 0.7243(9) 0.5983(7) 0.3973(10) 0.052(3) Uani 1 1 d . . . H48A H 0.7297 0.6093 0.3295 0.063 Uiso 1 1 calc R . . H48B H 0.7233 0.6636 0.4360 0.063 Uiso 1 1 calc R . . C49 C 0.6184(9) 0.5213(8) 0.3686(10) 0.055(3) Uani 1 1 d . . . H49A H 0.5486 0.5540 0.3473 0.066 Uiso 1 1 calc R . . H49B H 0.6034 0.4668 0.3076 0.066 Uiso 1 1 calc R . . C50 C 0.6566(9) 0.4826(8) 0.4781(9) 0.051(3) Uani 1 1 d . . . H50A H 0.6317 0.5229 0.5247 0.061 Uiso 1 1 calc R . . H50B H 0.6214 0.4115 0.4646 0.061 Uiso 1 1 calc R . . O2 O 0.7801(6) 0.4901(5) 0.5350(7) 0.059(2) Uani 1 1 d . . . C47 C 0.8204(9) 0.5459(8) 0.4737(8) 0.047(2) Uani 1 1 d . . . H47A H 0.8430 0.4999 0.4293 0.057 Uiso 1 1 calc R . . H47B H 0.8884 0.5959 0.5258 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.013(4) 0.007(3) 0.023(4) -0.003(3) 0.007(3) 0.004(3) N1 0.010(3) 0.022(3) 0.004(2) -0.007(2) 0.000(2) 0.003(2) N2 0.014(3) 0.017(3) 0.013(3) 0.004(2) 0.008(2) 0.003(2) C1 0.014(3) 0.018(3) 0.015(3) 0.004(3) 0.008(3) 0.005(3) C2 0.017(3) 0.016(3) 0.014(3) 0.002(3) 0.010(3) 0.004(3) C3 0.016(3) 0.019(3) 0.013(3) 0.001(3) 0.006(3) 0.001(3) C4 0.021(3) 0.022(4) 0.014(3) 0.008(3) 0.008(3) 0.011(3) C5 0.027(4) 0.015(3) 0.019(3) 0.005(3) 0.016(3) 0.006(3) C6 0.017(3) 0.015(3) 0.016(3) 0.001(3) 0.010(3) 0.002(3) Sn1 0.0138(2) 0.0151(2) 0.0117(2) 0.00234(17) 0.00644(18) 0.00177(17) C7 0.017(3) 0.019(3) 0.017(3) -0.003(3) 0.011(3) -0.002(3) C8 0.027(4) 0.024(4) 0.025(4) 0.001(3) 0.015(3) 0.005(3) C9 0.038(5) 0.019(4) 0.044(5) 0.000(3) 0.028(4) 0.003(3) C10 0.017(4) 0.061(6) 0.018(4) -0.014(4) 0.008(3) -0.013(4) C11 0.023(4) 0.026(4) 0.007(3) 0.004(3) 0.001(3) 0.006(3) C12 0.020(3) 0.024(4) 0.021(4) 0.000(3) 0.011(3) 0.001(3) C13 0.021(3) 0.013(3) 0.015(3) 0.003(3) 0.007(3) 0.004(3) C14 0.021(4) 0.023(4) 0.025(4) 0.004(3) 0.013(3) 0.006(3) C15 0.030(4) 0.023(4) 0.031(4) 0.012(3) 0.020(3) 0.006(3) C16 0.029(4) 0.015(3) 0.026(4) 0.007(3) 0.012(3) 0.004(3) C17 0.024(4) 0.020(4) 0.021(4) 0.001(3) 0.011(3) 0.007(3) C18 0.021(3) 0.020(3) 0.019(4) 0.008(3) 0.012(3) 0.005(3) C19 0.022(3) 0.021(3) 0.014(3) 0.008(3) 0.012(3) 0.009(3) C20 0.023(4) 0.020(3) 0.015(3) 0.006(3) 0.007(3) 0.004(3) C21 0.020(3) 0.029(4) 0.029(4) 0.010(3) 0.016(3) 0.005(3) C22 0.032(4) 0.029(4) 0.021(4) 0.011(3) 0.020(3) 0.016(3) C23 0.031(4) 0.026(4) 0.015(4) 0.003(3) 0.011(3) 0.011(3) C24 0.019(3) 0.021(3) 0.016(3) 0.003(3) 0.009(3) 0.000(3) Sn2 0.0147(2) 0.0161(2) 0.0123(2) 0.00257(18) 0.00698(19) 0.00258(17) C25 0.018(3) 0.020(3) 0.016(3) 0.004(3) 0.007(3) 0.000(3) C26 0.024(4) 0.026(4) 0.019(4) 0.003(3) 0.011(3) 0.006(3) C27 0.018(4) 0.042(5) 0.031(4) 0.014(4) 0.009(3) 0.009(3) C28 0.020(4) 0.035(4) 0.027(4) 0.002(3) 0.006(3) 0.001(3) C29 0.030(4) 0.038(5) 0.017(4) -0.007(3) 0.006(3) 0.000(4) C30 0.023(4) 0.031(4) 0.017(4) 0.003(3) 0.006(3) 0.001(3) C31 0.026(4) 0.014(3) 0.017(3) 0.004(3) 0.014(3) 0.006(3) C32 0.028(4) 0.017(3) 0.027(4) 0.003(3) 0.015(3) 0.004(3) C33 0.038(4) 0.017(4) 0.034(4) 0.004(3) 0.023(4) 0.003(3) C34 0.052(5) 0.020(4) 0.033(5) 0.010(3) 0.025(4) 0.013(4) C35 0.040(5) 0.027(4) 0.021(4) 0.009(3) 0.012(4) 0.015(3) C36 0.023(4) 0.020(4) 0.020(4) 0.001(3) 0.011(3) 0.006(3) C37 0.021(3) 0.015(3) 0.030(4) 0.006(3) 0.018(3) 0.003(3) C38 0.019(3) 0.031(4) 0.021(4) 0.006(3) 0.009(3) 0.007(3) C39 0.028(4) 0.030(4) 0.012(3) 0.002(3) 0.013(3) 0.001(3) C40 0.025(4) 0.024(4) 0.025(4) -0.004(3) 0.018(3) 0.001(3) C41 0.022(4) 0.025(4) 0.029(4) 0.004(3) 0.014(3) 0.009(3) C42 0.021(3) 0.026(4) 0.023(4) 0.000(3) 0.012(3) 0.007(3) C45 0.058(7) 0.042(7) 0.155(15) 0.008(8) 0.046(9) 0.021(6) C44 0.055(6) 0.041(5) 0.041(6) 0.001(4) 0.013(5) 0.008(5) C43 0.053(6) 0.074(8) 0.048(6) -0.016(6) 0.019(5) 0.011(6) O1 0.050(5) 0.061(5) 0.094(7) 0.004(5) 0.028(5) 0.016(4) C46 0.052(6) 0.046(6) 0.043(6) 0.008(4) 0.021(5) 0.010(5) C48 0.060(7) 0.035(5) 0.066(7) 0.003(5) 0.036(6) 0.001(5) C49 0.051(6) 0.037(5) 0.068(7) -0.006(5) 0.025(6) -0.001(5) C50 0.050(6) 0.043(6) 0.055(6) -0.003(5) 0.025(5) -0.003(5) O2 0.055(4) 0.040(4) 0.072(5) 0.004(4) 0.024(4) 0.001(3) C47 0.046(6) 0.047(6) 0.045(6) -0.010(5) 0.023(5) -0.001(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 B1 N1 1.389(10) . ? B1 N2 1.452(9) 2_655 ? B1 B1 1.646(14) 2_655 ? N1 C1 1.452(8) . ? N1 Sn1 2.068(5) . ? N2 C2 1.428(8) . ? N2 B1 1.452(9) 2_655 ? N2 Sn2 2.077(5) . ? C1 C6 1.400(9) . ? C1 C2 1.429(9) . ? C2 C3 1.397(9) . ? C3 C4 1.392(9) . ? C3 H3 0.9500 . ? C4 C5 1.380(10) . ? C4 H4 0.9500 . ? C5 C6 1.378(9) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? Sn1 C7 2.135(7) . ? Sn1 C19 2.141(6) . ? Sn1 C13 2.150(6) . ? C7 C12 1.388(10) . ? C7 C8 1.389(10) . ? C8 C9 1.382(11) . ? C8 H8 0.9500 . ? C9 C10 1.415(12) . ? C9 H9 0.9500 . ? C10 C11 1.387(12) . ? C10 H10 0.9500 . ? C11 C12 1.365(10) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.385(10) . ? C13 C14 1.393(10) . ? C14 C15 1.379(10) . ? C14 H14 0.9500 . ? C15 C16 1.386(11) . ? C15 H15 0.9500 . ? C16 C17 1.382(10) . ? C16 H16 0.9500 . ? C17 C18 1.390(10) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.389(10) . ? C19 C24 1.390(10) . ? C20 C21 1.392(10) . ? C20 H20 0.9500 . ? C21 C22 1.378(11) . ? C21 H21 0.9500 . ? C22 C23 1.387(11) . ? C22 H22 0.9500 . ? C23 C24 1.392(10) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? Sn2 C31 2.131(6) . ? Sn2 C37 2.136(7) . ? Sn2 C25 2.139(7) . ? C25 C26 1.391(10) . ? C25 C30 1.411(10) . ? C26 C27 1.387(10) . ? C26 H26 0.9500 . ? C27 C28 1.375(12) . ? C27 H27 0.9500 . ? C28 C29 1.369(12) . ? C28 H28 0.9500 . ? C29 C30 1.385(10) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.396(10) . ? C31 C36 1.405(10) . ? C32 C33 1.392(10) . ? C32 H32 0.9500 . ? C33 C34 1.371(12) . ? C33 H33 0.9500 . ? C34 C35 1.386(12) . ? C34 H34 0.9500 . ? C35 C36 1.380(10) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.396(10) . ? C37 C42 1.402(10) . ? C38 C39 1.393(10) . ? C38 H38 0.9500 . ? C39 C40 1.384(10) . ? C39 H39 0.9500 . ? C40 C41 1.380(11) . ? C40 H40 0.9500 . ? C41 C42 1.392(10) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C45 C46 1.521(16) . ? C45 C44 1.528(16) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C44 C43 1.482(14) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C43 O1 1.392(13) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? O1 C46 1.403(12) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C48 C47 1.501(15) . ? C48 C49 1.541(14) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.500(15) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 O2 1.438(12) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? O2 C47 1.428(13) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 B1 N2 124.4(6) . 2_655 ? N1 B1 B1 118.3(8) . 2_655 ? N2 B1 B1 117.3(8) 2_655 2_655 ? B1 N1 C1 116.6(5) . . ? B1 N1 Sn1 120.1(4) . . ? C1 N1 Sn1 115.5(4) . . ? C2 N2 B1 115.6(5) . 2_655 ? C2 N2 Sn2 114.3(4) . . ? B1 N2 Sn2 119.8(4) 2_655 . ? C6 C1 C2 118.5(6) . . ? C6 C1 N1 120.0(6) . . ? C2 C1 N1 121.4(6) . . ? C3 C2 N2 119.2(6) . . ? C3 C2 C1 117.3(6) . . ? N2 C2 C1 123.4(6) . . ? C4 C3 C2 122.9(6) . . ? C4 C3 H3 118.5 . . ? C2 C3 H3 118.5 . . ? C5 C4 C3 119.1(6) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C6 C5 C4 119.7(6) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C1 122.4(6) . . ? C5 C6 H6 118.8 . . ? C1 C6 H6 118.8 . . ? N1 Sn1 C7 113.7(2) . . ? N1 Sn1 C19 111.9(2) . . ? C7 Sn1 C19 105.8(3) . . ? N1 Sn1 C13 106.9(2) . . ? C7 Sn1 C13 112.5(3) . . ? C19 Sn1 C13 105.7(3) . . ? C12 C7 C8 118.8(6) . . ? C12 C7 Sn1 119.6(5) . . ? C8 C7 Sn1 121.3(5) . . ? C9 C8 C7 121.1(7) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 119.7(7) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C11 C10 C9 118.3(7) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? C12 C11 C10 121.5(7) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C7 120.7(7) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.6 . . ? C18 C13 C14 118.1(6) . . ? C18 C13 Sn1 115.8(5) . . ? C14 C13 Sn1 126.2(5) . . ? C15 C14 C13 120.9(7) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 120.2(7) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 119.8(7) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 119.4(7) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C13 C18 C17 121.5(6) . . ? C13 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C20 C19 C24 118.5(6) . . ? C20 C19 Sn1 116.6(5) . . ? C24 C19 Sn1 124.7(5) . . ? C19 C20 C21 121.1(7) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C22 C21 C20 119.6(7) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 120.2(7) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C24 119.8(7) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C19 C24 C23 120.8(6) . . ? C19 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? N2 Sn2 C31 112.1(2) . . ? N2 Sn2 C37 106.1(2) . . ? C31 Sn2 C37 106.5(3) . . ? N2 Sn2 C25 110.9(2) . . ? C31 Sn2 C25 113.4(3) . . ? C37 Sn2 C25 107.3(3) . . ? C26 C25 C30 119.2(6) . . ? C26 C25 Sn2 121.7(5) . . ? C30 C25 Sn2 119.0(5) . . ? C27 C26 C25 120.5(7) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C28 C27 C26 119.6(7) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C29 C28 C27 120.8(7) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 120.9(7) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C29 C30 C25 119.0(7) . . ? C29 C30 H30 120.5 . . ? C25 C30 H30 120.5 . . ? C32 C31 C36 118.4(6) . . ? C32 C31 Sn2 118.6(5) . . ? C36 C31 Sn2 122.9(5) . . ? C33 C32 C31 120.6(7) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C34 C33 C32 120.1(7) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 120.1(7) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 120.4(7) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C31 120.3(7) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? C38 C37 C42 118.2(6) . . ? C38 C37 Sn2 120.0(5) . . ? C42 C37 Sn2 121.6(5) . . ? C39 C38 C37 121.2(7) . . ? C39 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? C40 C39 C38 119.5(7) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C41 C40 C39 120.3(7) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C40 C41 C42 120.3(7) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C41 C42 C37 120.5(7) . . ? C41 C42 H42 119.8 . . ? C37 C42 H42 119.8 . . ? C46 C45 C44 102.5(9) . . ? C46 C45 H45A 111.3 . . ? C44 C45 H45A 111.3 . . ? C46 C45 H45B 111.3 . . ? C44 C45 H45B 111.3 . . ? H45A C45 H45B 109.2 . . ? C43 C44 C45 100.8(9) . . ? C43 C44 H44A 111.6 . . ? C45 C44 H44A 111.6 . . ? C43 C44 H44B 111.6 . . ? C45 C44 H44B 111.6 . . ? H44A C44 H44B 109.4 . . ? O1 C43 C44 108.3(10) . . ? O1 C43 H43A 110.0 . . ? C44 C43 H43A 110.0 . . ? O1 C43 H43B 110.0 . . ? C44 C43 H43B 110.0 . . ? H43A C43 H43B 108.4 . . ? C43 O1 C46 106.6(8) . . ? O1 C46 C45 109.1(9) . . ? O1 C46 H46A 109.9 . . ? C45 C46 H46A 109.9 . . ? O1 C46 H46B 109.9 . . ? C45 C46 H46B 109.9 . . ? H46A C46 H46B 108.3 . . ? C47 C48 C49 101.1(8) . . ? C47 C48 H48A 111.6 . . ? C49 C48 H48A 111.6 . . ? C47 C48 H48B 111.6 . . ? C49 C48 H48B 111.6 . . ? H48A C48 H48B 109.4 . . ? C50 C49 C48 101.0(9) . . ? C50 C49 H49A 111.6 . . ? C48 C49 H49A 111.6 . . ? C50 C49 H49B 111.6 . . ? C48 C49 H49B 111.6 . . ? H49A C49 H49B 109.4 . . ? O2 C50 C49 108.6(9) . . ? O2 C50 H50A 110.0 . . ? C49 C50 H50A 110.0 . . ? O2 C50 H50B 110.0 . . ? C49 C50 H50B 110.0 . . ? H50A C50 H50B 108.3 . . ? C47 O2 C50 107.1(8) . . ? O2 C47 C48 107.9(8) . . ? O2 C47 H47A 110.1 . . ? C48 C47 H47A 110.1 . . ? O2 C47 H47B 110.1 . . ? C48 C47 H47B 110.1 . . ? H47A C47 H47B 108.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 B1 N1 C1 158.4(6) 2_655 . . . ? B1 B1 N1 C1 -22.5(10) 2_655 . . . ? N2 B1 N1 Sn1 -53.9(8) 2_655 . . . ? B1 B1 N1 Sn1 125.3(7) 2_655 . . . ? B1 N1 C1 C6 -152.7(6) . . . . ? Sn1 N1 C1 C6 58.0(7) . . . . ? B1 N1 C1 C2 25.0(9) . . . . ? Sn1 N1 C1 C2 -124.2(6) . . . . ? B1 N2 C2 C3 157.6(6) 2_655 . . . ? Sn2 N2 C2 C3 -57.2(7) . . . . ? B1 N2 C2 C1 -18.9(9) 2_655 . . . ? Sn2 N2 C2 C1 126.3(6) . . . . ? C6 C1 C2 C3 -2.3(9) . . . . ? N1 C1 C2 C3 179.9(6) . . . . ? C6 C1 C2 N2 174.2(6) . . . . ? N1 C1 C2 N2 -3.6(10) . . . . ? N2 C2 C3 C4 -175.9(6) . . . . ? C1 C2 C3 C4 0.8(10) . . . . ? C2 C3 C4 C5 1.8(10) . . . . ? C3 C4 C5 C6 -2.8(10) . . . . ? C4 C5 C6 C1 1.2(10) . . . . ? C2 C1 C6 C5 1.4(10) . . . . ? N1 C1 C6 C5 179.2(6) . . . . ? B1 N1 Sn1 C7 89.4(5) . . . . ? C1 N1 Sn1 C7 -122.6(4) . . . . ? B1 N1 Sn1 C19 -150.8(5) . . . . ? C1 N1 Sn1 C19 -2.7(5) . . . . ? B1 N1 Sn1 C13 -35.4(5) . . . . ? C1 N1 Sn1 C13 112.6(5) . . . . ? N1 Sn1 C7 C12 -134.6(5) . . . . ? C19 Sn1 C7 C12 102.2(6) . . . . ? C13 Sn1 C7 C12 -12.8(6) . . . . ? N1 Sn1 C7 C8 51.7(6) . . . . ? C19 Sn1 C7 C8 -71.5(6) . . . . ? C13 Sn1 C7 C8 173.5(5) . . . . ? C12 C7 C8 C9 0.8(11) . . . . ? Sn1 C7 C8 C9 174.5(6) . . . . ? C7 C8 C9 C10 -0.3(12) . . . . ? C8 C9 C10 C11 -0.7(11) . . . . ? C9 C10 C11 C12 1.4(11) . . . . ? C10 C11 C12 C7 -1.0(11) . . . . ? C8 C7 C12 C11 -0.1(10) . . . . ? Sn1 C7 C12 C11 -174.0(5) . . . . ? N1 Sn1 C13 C18 -133.6(5) . . . . ? C7 Sn1 C13 C18 100.9(5) . . . . ? C19 Sn1 C13 C18 -14.1(6) . . . . ? N1 Sn1 C13 C14 45.1(6) . . . . ? C7 Sn1 C13 C14 -80.4(6) . . . . ? C19 Sn1 C13 C14 164.5(6) . . . . ? C18 C13 C14 C15 -0.5(10) . . . . ? Sn1 C13 C14 C15 -179.1(5) . . . . ? C13 C14 C15 C16 -1.1(11) . . . . ? C14 C15 C16 C17 1.6(11) . . . . ? C15 C16 C17 C18 -0.6(11) . . . . ? C14 C13 C18 C17 1.4(10) . . . . ? Sn1 C13 C18 C17 -179.8(5) . . . . ? C16 C17 C18 C13 -0.9(11) . . . . ? N1 Sn1 C19 C20 -137.3(5) . . . . ? C7 Sn1 C19 C20 -13.0(6) . . . . ? C13 Sn1 C19 C20 106.6(5) . . . . ? N1 Sn1 C19 C24 48.6(6) . . . . ? C7 Sn1 C19 C24 173.0(6) . . . . ? C13 Sn1 C19 C24 -67.4(6) . . . . ? C24 C19 C20 C21 0.2(10) . . . . ? Sn1 C19 C20 C21 -174.2(5) . . . . ? C19 C20 C21 C22 0.3(11) . . . . ? C20 C21 C22 C23 -0.6(11) . . . . ? C21 C22 C23 C24 0.3(11) . . . . ? C20 C19 C24 C23 -0.5(10) . . . . ? Sn1 C19 C24 C23 173.5(5) . . . . ? C22 C23 C24 C19 0.3(11) . . . . ? C2 N2 Sn2 C31 -154.9(4) . . . . ? B1 N2 Sn2 C31 -11.2(5) 2_655 . . . ? C2 N2 Sn2 C37 -39.0(5) . . . . ? B1 N2 Sn2 C37 104.6(5) 2_655 . . . ? C2 N2 Sn2 C25 77.2(5) . . . . ? B1 N2 Sn2 C25 -139.1(5) 2_655 . . . ? N2 Sn2 C25 C26 20.3(6) . . . . ? C31 Sn2 C25 C26 -106.9(6) . . . . ? C37 Sn2 C25 C26 135.8(6) . . . . ? N2 Sn2 C25 C30 -157.0(5) . . . . ? C31 Sn2 C25 C30 75.8(6) . . . . ? C37 Sn2 C25 C30 -41.5(6) . . . . ? C30 C25 C26 C27 -0.5(11) . . . . ? Sn2 C25 C26 C27 -177.8(6) . . . . ? C25 C26 C27 C28 0.9(12) . . . . ? C26 C27 C28 C29 0.1(12) . . . . ? C27 C28 C29 C30 -1.4(13) . . . . ? C28 C29 C30 C25 1.7(12) . . . . ? C26 C25 C30 C29 -0.7(11) . . . . ? Sn2 C25 C30 C29 176.6(6) . . . . ? N2 Sn2 C31 C32 -141.9(5) . . . . ? C37 Sn2 C31 C32 102.5(6) . . . . ? C25 Sn2 C31 C32 -15.3(6) . . . . ? N2 Sn2 C31 C36 43.0(6) . . . . ? C37 Sn2 C31 C36 -72.7(6) . . . . ? C25 Sn2 C31 C36 169.5(5) . . . . ? C36 C31 C32 C33 -0.5(10) . . . . ? Sn2 C31 C32 C33 -175.9(6) . . . . ? C31 C32 C33 C34 -0.2(11) . . . . ? C32 C33 C34 C35 0.8(12) . . . . ? C33 C34 C35 C36 -0.5(12) . . . . ? C34 C35 C36 C31 -0.3(11) . . . . ? C32 C31 C36 C35 0.8(10) . . . . ? Sn2 C31 C36 C35 176.0(6) . . . . ? N2 Sn2 C37 C38 93.1(6) . . . . ? C31 Sn2 C37 C38 -147.3(6) . . . . ? C25 Sn2 C37 C38 -25.5(6) . . . . ? N2 Sn2 C37 C42 -92.9(6) . . . . ? C31 Sn2 C37 C42 26.8(6) . . . . ? C25 Sn2 C37 C42 148.5(6) . . . . ? C42 C37 C38 C39 0.8(11) . . . . ? Sn2 C37 C38 C39 175.0(5) . . . . ? C37 C38 C39 C40 -2.0(11) . . . . ? C38 C39 C40 C41 2.4(11) . . . . ? C39 C40 C41 C42 -1.6(11) . . . . ? C40 C41 C42 C37 0.3(11) . . . . ? C38 C37 C42 C41 0.1(11) . . . . ? Sn2 C37 C42 C41 -174.0(5) . . . . ? C46 C45 C44 C43 26.8(13) . . . . ? C45 C44 C43 O1 -36.6(13) . . . . ? C44 C43 O1 C46 31.3(13) . . . . ? C43 O1 C46 C45 -12.2(13) . . . . ? C44 C45 C46 O1 -10.3(13) . . . . ? C47 C48 C49 C50 36.4(10) . . . . ? C48 C49 C50 O2 -28.8(11) . . . . ? C49 C50 O2 C47 8.8(11) . . . . ? C50 O2 C47 C48 16.1(10) . . . . ? C49 C48 C47 O2 -33.3(10) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.77 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.332 _refine_diff_density_min -1.483 _refine_diff_density_rms 0.168 data_8 _database_code_depnum_ccdc_archive 'CCDC 848888' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 B2 N4' _chemical_formula_sum 'C12 H24 B2 N4' _chemical_formula_weight 245.97 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.7678(18) _cell_length_b 10.1822(18) _cell_length_c 27.337(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2718.9(8) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2623 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 27.60 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6685 _exptl_absorpt_correction_T_max 0.7547 _exptl_absorpt_process_details 'SADABS V2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II kappa CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27191 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3124 _reflns_number_gt 1777 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+1.0389P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3124 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1085 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1861 _refine_ls_wR_factor_gt 0.1451 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 B1 B 0.1730(2) 0.31502(18) 0.19295(7) 0.0244(4) Uani 1 1 d . . . B2 B 0.0719(2) 0.18136(18) 0.19169(8) 0.0259(4) Uani 1 1 d . A . N1A N 0.21034(16) 0.36886(13) 0.14729(5) 0.0286(4) Uani 0.50 1 d P A 1 H1 H 0.2486 0.4470 0.1458 0.034 Uiso 0.50 1 calc PR A 1 N2A N 0.03452(17) 0.13541(15) 0.14470(5) 0.0344(4) Uani 0.50 1 d P A 1 H2 H 0.0086 0.0538 0.1396 0.041 Uiso 0.50 1 calc PR A 1 C1A C 0.1854(5) 0.2944(4) 0.10256(15) 0.0289(9) Uani 0.50 1 d P A 1 H3 H 0.2552 0.2231 0.0992 0.035 Uiso 0.50 1 calc PR A 1 C2A C 0.0417(4) 0.2347(4) 0.10374(14) 0.0289(8) Uani 0.50 1 d P A 1 H4 H -0.0291 0.3047 0.1083 0.035 Uiso 0.50 1 calc PR A 1 C3A C 0.0156(2) 0.1571(2) 0.05553(7) 0.0400(5) Uani 0.50 1 d P A 1 H5 H 0.0409 0.0644 0.0617 0.048 Uiso 0.50 1 calc PR A 1 H6 H -0.0842 0.1587 0.0493 0.048 Uiso 0.50 1 calc PR A 1 C4A C 0.0869(5) 0.1993(5) 0.00825(16) 0.0403(11) Uani 0.50 1 d P A 1 H7 H 0.0306 0.1754 -0.0205 0.048 Uiso 0.50 1 calc PR A 1 H8 H 0.1771 0.1556 0.0053 0.048 Uiso 0.50 1 calc PR A 1 C5A C 0.1048(6) 0.3486(7) 0.0112(3) 0.0424(15) Uani 0.50 1 d P A 1 H9 H 0.0139 0.3913 0.0132 0.051 Uiso 0.50 1 calc PR A 1 H10 H 0.1514 0.3807 -0.0186 0.051 Uiso 0.50 1 calc PR A 1 C6A C 0.1922(2) 0.38629(18) 0.05779(7) 0.0370(5) Uani 0.50 1 d P A 1 H11 H 0.2892 0.3928 0.0476 0.044 Uiso 0.50 1 calc PR A 1 H12 H 0.1634 0.4749 0.0685 0.044 Uiso 0.50 1 calc PR A 1 N1B N 0.21034(16) 0.36886(13) 0.14729(5) 0.0286(4) Uani 0.50 1 d P A 2 H13 H 0.2825 0.4200 0.1443 0.034 Uiso 0.50 1 calc PR A 2 N2B N 0.03452(17) 0.13541(15) 0.14470(5) 0.0344(4) Uani 0.50 1 d P A 2 H14 H -0.0319 0.0776 0.1418 0.041 Uiso 0.50 1 calc PR A 2 C1B C 0.1211(5) 0.3352(4) 0.10354(14) 0.0257(8) Uani 0.50 1 d P A 2 H15 H 0.0289 0.3769 0.1071 0.031 Uiso 0.50 1 calc PR A 2 C2B C 0.1063(5) 0.1838(4) 0.10005(14) 0.0281(8) Uani 0.50 1 d P A 2 H16 H 0.1978 0.1408 0.0963 0.034 Uiso 0.50 1 calc PR A 2 C3B C 0.0156(2) 0.1571(2) 0.05553(7) 0.0400(5) Uani 0.50 1 d P A 2 H17 H -0.0805 0.1529 0.0669 0.048 Uiso 0.50 1 calc PR A 2 H18 H 0.0395 0.0692 0.0426 0.048 Uiso 0.50 1 calc PR A 2 C4B C 0.0232(5) 0.2582(5) 0.01192(16) 0.0410(11) Uani 0.50 1 d P A 2 H19 H 0.0039 0.2129 -0.0194 0.049 Uiso 0.50 1 calc PR A 2 H20 H -0.0464 0.3279 0.0165 0.049 Uiso 0.50 1 calc PR A 2 C5B C 0.1646(6) 0.3186(7) 0.0104(3) 0.0449(15) Uani 0.50 1 d P A 2 H21 H 0.2339 0.2493 0.0048 0.054 Uiso 0.50 1 calc PR A 2 H22 H 0.1703 0.3825 -0.0168 0.054 Uiso 0.50 1 calc PR A 2 C6B C 0.1922(2) 0.38629(18) 0.05779(7) 0.0370(5) Uani 0.50 1 d P A 2 H23 H 0.1670 0.4799 0.0539 0.044 Uiso 0.50 1 calc PR A 2 H24 H 0.2921 0.3831 0.0637 0.044 Uiso 0.50 1 calc PR A 2 N3A N 0.21092(16) 0.36115(13) 0.23961(5) 0.0315(4) Uani 0.50 1 d P A 1 H25 H 0.2428 0.4412 0.2438 0.038 Uiso 0.50 1 calc PR A 1 N4A N 0.03433(17) 0.12760(14) 0.23714(5) 0.0337(4) Uani 0.50 1 d P A 1 H26 H 0.0059 0.0460 0.2402 0.040 Uiso 0.50 1 calc PR A 1 C7A C 0.1949(4) 0.2686(3) 0.28158(12) 0.0211(7) Uani 0.50 1 d P A 1 H27 H 0.2620 0.1946 0.2798 0.025 Uiso 0.50 1 calc PR A 1 C8A C 0.0459(4) 0.2190(3) 0.28037(12) 0.0219(7) Uani 0.50 1 d P A 1 H28 H -0.0210 0.2931 0.2782 0.026 Uiso 0.50 1 calc PR A 1 C9A C 0.0206(2) 0.13193(18) 0.32681(7) 0.0336(5) Uani 0.50 1 d P A 1 H29 H -0.0783 0.1365 0.3345 0.040 Uiso 0.50 1 calc PR A 1 H30 H 0.0407 0.0399 0.3176 0.040 Uiso 0.50 1 calc PR A 1 C10A C 0.0997(5) 0.1614(4) 0.37460(14) 0.0303(9) Uani 0.50 1 d P A 1 H31 H 0.0447 0.1341 0.4033 0.036 Uiso 0.50 1 calc PR A 1 H32 H 0.1872 0.1124 0.3751 0.036 Uiso 0.50 1 calc PR A 1 C11A C 0.1271(5) 0.3081(4) 0.37661(16) 0.0314(10) Uani 0.50 1 d P A 1 H33 H 0.1795 0.3298 0.4065 0.038 Uiso 0.50 1 calc PR A 1 H34 H 0.0394 0.3567 0.3776 0.038 Uiso 0.50 1 calc PR A 1 C12A C 0.2119(2) 0.34985(17) 0.32965(7) 0.0321(5) Uani 0.50 1 d P A 1 H35 H 0.1882 0.4422 0.3221 0.039 Uiso 0.50 1 calc PR A 1 H36 H 0.3101 0.3483 0.3386 0.039 Uiso 0.50 1 calc PR A 1 N3B N 0.21092(16) 0.36115(13) 0.23961(5) 0.0315(4) Uani 0.50 1 d P A 2 H37 H 0.2810 0.4146 0.2432 0.038 Uiso 0.50 1 calc PR A 2 N4B N 0.03433(17) 0.12760(14) 0.23714(5) 0.0337(4) Uani 0.50 1 d P A 2 H38 H -0.0338 0.0713 0.2391 0.040 Uiso 0.50 1 calc PR A 2 C7B C 0.1275(4) 0.3161(4) 0.28369(13) 0.0247(8) Uani 0.50 1 d P A 2 H39 H 0.0362 0.3604 0.2845 0.030 Uiso 0.50 1 calc PR A 2 C8B C 0.1117(4) 0.1673(3) 0.28232(13) 0.0238(8) Uani 0.50 1 d P A 2 H40 H 0.2025 0.1223 0.2841 0.029 Uiso 0.50 1 calc PR A 2 C9B C 0.0206(2) 0.13193(18) 0.32681(7) 0.0336(5) Uani 0.50 1 d P A 2 H41 H 0.0402 0.0400 0.3363 0.040 Uiso 0.50 1 calc PR A 2 H42 H -0.0764 0.1360 0.3164 0.040 Uiso 0.50 1 calc PR A 2 C10B C 0.0384(4) 0.2203(4) 0.37271(14) 0.0300(8) Uani 0.50 1 d P A 2 H43 H -0.0238 0.2969 0.3708 0.036 Uiso 0.50 1 calc PR A 2 H44 H 0.0162 0.1700 0.4027 0.036 Uiso 0.50 1 calc PR A 2 C11B C 0.1874(4) 0.2663(4) 0.37423(16) 0.0294(9) Uani 0.50 1 d P A 2 H45 H 0.2044 0.3179 0.4043 0.035 Uiso 0.50 1 calc PR A 2 H46 H 0.2498 0.1897 0.3741 0.035 Uiso 0.50 1 calc PR A 2 C12B C 0.2119(2) 0.34985(17) 0.32965(7) 0.0321(5) Uani 0.50 1 d P A 2 H47 H 0.3101 0.3438 0.3211 0.039 Uiso 0.50 1 calc PR A 2 H48 H 0.1930 0.4424 0.3385 0.039 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0219(9) 0.0213(9) 0.0301(11) -0.0002(8) -0.0012(9) 0.0024(7) B2 0.0260(10) 0.0221(9) 0.0297(11) -0.0006(8) -0.0024(9) -0.0004(8) N1A 0.0345(9) 0.0245(7) 0.0267(9) -0.0020(6) 0.0036(6) -0.0067(6) N2A 0.0457(10) 0.0307(8) 0.0267(9) 0.0022(6) -0.0047(7) -0.0152(7) C1A 0.031(2) 0.027(2) 0.029(2) -0.0009(16) -0.0030(19) -0.0008(17) C2A 0.031(2) 0.031(2) 0.025(2) 0.0026(16) 0.0013(17) -0.0019(17) C3A 0.0467(12) 0.0464(11) 0.0269(10) -0.0014(9) -0.0049(9) -0.0119(9) C4A 0.048(3) 0.047(3) 0.026(2) -0.0034(19) -0.004(2) 0.001(2) C5A 0.055(4) 0.047(3) 0.025(3) 0.008(2) -0.001(3) -0.002(3) C6A 0.0464(12) 0.0335(9) 0.0311(11) 0.0021(8) 0.0065(10) -0.0048(9) N1B 0.0345(9) 0.0245(7) 0.0267(9) -0.0020(6) 0.0036(6) -0.0067(6) N2B 0.0457(10) 0.0307(8) 0.0267(9) 0.0022(6) -0.0047(7) -0.0152(7) C1B 0.033(2) 0.0223(19) 0.022(2) 0.0017(15) -0.0026(19) 0.0032(16) C2B 0.036(2) 0.0247(19) 0.024(2) -0.0007(15) -0.0014(18) -0.0011(17) C3B 0.0467(12) 0.0464(11) 0.0269(10) -0.0014(9) -0.0049(9) -0.0119(9) C4B 0.046(3) 0.051(3) 0.026(2) 0.004(2) -0.002(2) -0.011(2) C5B 0.051(4) 0.053(4) 0.031(3) 0.002(3) 0.004(3) -0.012(3) C6B 0.0464(12) 0.0335(9) 0.0311(11) 0.0021(8) 0.0065(10) -0.0048(9) N3A 0.0396(10) 0.0280(7) 0.0269(9) 0.0026(6) -0.0012(7) -0.0153(7) N4A 0.0431(10) 0.0301(8) 0.0279(9) -0.0003(6) -0.0025(7) -0.0178(7) C7A 0.0178(17) 0.0217(16) 0.0238(19) -0.0015(14) -0.0006(15) 0.0020(14) C8A 0.0207(18) 0.0205(16) 0.024(2) 0.0007(14) -0.0018(15) 0.0027(15) C9A 0.0387(11) 0.0359(10) 0.0264(10) 0.0034(8) 0.0009(8) -0.0140(8) C10A 0.039(2) 0.029(2) 0.023(2) 0.0020(16) 0.0042(18) -0.0025(17) C11A 0.036(3) 0.032(2) 0.027(2) -0.0017(18) 0.004(2) 0.0006(18) C12A 0.0397(11) 0.0301(9) 0.0266(10) -0.0004(8) -0.0033(9) -0.0086(8) N3B 0.0396(10) 0.0280(7) 0.0269(9) 0.0026(6) -0.0012(7) -0.0153(7) N4B 0.0431(10) 0.0301(8) 0.0279(9) -0.0003(6) -0.0025(7) -0.0178(7) C7B 0.026(2) 0.0226(17) 0.026(2) 0.0022(14) 0.0017(16) 0.0005(16) C8B 0.0248(19) 0.0212(17) 0.025(2) 0.0000(14) -0.0023(16) -0.0004(15) C9B 0.0387(11) 0.0359(10) 0.0264(10) 0.0034(8) 0.0009(8) -0.0140(8) C10B 0.031(2) 0.033(2) 0.026(2) 0.0037(17) 0.0031(17) 0.0016(17) C11B 0.027(2) 0.034(2) 0.027(2) -0.0048(18) -0.001(2) 0.0029(17) C12B 0.0397(11) 0.0301(9) 0.0266(10) -0.0004(8) -0.0033(9) -0.0086(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N3A 1.409(2) . ? B1 N1A 1.411(2) . ? B1 B2 1.681(3) . ? B2 N4A 1.407(2) . ? B2 N2A 1.415(2) . ? N1A C1A 1.459(4) . ? N1A H1 0.8800 . ? N2A C2A 1.510(4) . ? N2A H2 0.8800 . ? C1A C2A 1.530(6) . ? C1A C6A 1.542(4) . ? C1A H3 1.0000 . ? C2A C3A 1.558(4) . ? C2A H4 1.0000 . ? C3A C4A 1.530(5) . ? C3A H5 0.9900 . ? C3A H6 0.9900 . ? C4A C5A 1.533(8) . ? C4A H7 0.9900 . ? C4A H8 0.9900 . ? C5A C6A 1.580(8) . ? C5A H9 0.9900 . ? C5A H10 0.9900 . ? C6A H11 0.9900 . ? C6A H12 0.9900 . ? C1B C2B 1.551(5) . ? C1B H15 1.0000 . ? C2B H16 1.0000 . ? C4B C5B 1.513(8) . ? C4B H19 0.9900 . ? C4B H20 0.9900 . ? C5B H21 0.9900 . ? C5B H22 0.9900 . ? N3A C7A 1.493(4) . ? N3A H25 0.8800 . ? N4A C8A 1.508(4) . ? N4A H26 0.8800 . ? C7A C8A 1.541(5) . ? C7A C12A 1.561(4) . ? C7A H27 1.0000 . ? C8A C9A 1.568(4) . ? C8A H28 1.0000 . ? C9A C10A 1.547(4) . ? C9A H29 0.9900 . ? C9A H30 0.9900 . ? C10A C11A 1.518(6) . ? C10A H31 0.9900 . ? C10A H32 0.9900 . ? C11A C12A 1.586(5) . ? C11A H33 0.9900 . ? C11A H34 0.9900 . ? C12A H35 0.9900 . ? C12A H36 0.9900 . ? C7B C8B 1.524(5) . ? C7B H39 1.0000 . ? C8B H40 1.0000 . ? C10B C11B 1.529(5) . ? C10B H43 0.9900 . ? C10B H44 0.9900 . ? C11B H45 0.9900 . ? C11B H46 0.9900 . ? 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 N3A B1 N1A 127.09(16) . . ? N3A B1 B2 116.29(16) . . ? N1A B1 B2 116.62(16) . . ? N4A B2 N2A 127.27(16) . . ? N4A B2 B1 116.76(16) . . ? N2A B2 B1 115.97(16) . . ? B1 N1A C1A 119.7(2) . . ? B1 N1A H1 120.1 . . ? C1A N1A H1 120.1 . . ? B2 N2A C2A 116.07(19) . . ? B2 N2A H2 122.0 . . ? C2A N2A H2 122.0 . . ? N1A C1A C2A 110.0(3) . . ? N1A C1A C6A 110.1(3) . . ? C2A C1A C6A 107.3(3) . . ? N1A C1A H3 109.8 . . ? C2A C1A H3 109.8 . . ? C6A C1A H3 109.8 . . ? N2A C2A C1A 108.9(3) . . ? N2A C2A C3A 106.2(3) . . ? C1A C2A C3A 109.5(3) . . ? N2A C2A H4 110.7 . . ? C1A C2A H4 110.7 . . ? C3A C2A H4 110.7 . . ? C4A C3A C2A 119.9(3) . . ? C4A C3A H5 107.4 . . ? C2A C3A H5 107.4 . . ? C4A C3A H6 107.4 . . ? C2A C3A H6 107.4 . . ? H5 C3A H6 106.9 . . ? C3A C4A C5A 106.6(4) . . ? C3A C4A H7 110.4 . . ? C5A C4A H7 110.4 . . ? C3A C4A H8 110.4 . . ? C5A C4A H8 110.4 . . ? H7 C4A H8 108.6 . . ? C4A C5A C6A 110.2(4) . . ? C4A C5A H9 109.6 . . ? C6A C5A H9 109.6 . . ? C4A C5A H10 109.6 . . ? C6A C5A H10 109.6 . . ? H9 C5A H10 108.1 . . ? C1A C6A C5A 118.0(3) . . ? C1A C6A H11 107.8 . . ? C5A C6A H11 107.8 . . ? C1A C6A H12 107.8 . . ? C5A C6A H12 107.8 . . ? H11 C6A H12 107.2 . . ? C2B C1B H15 110.2 . . ? C1B C2B H16 111.0 . . ? C5B C4B H19 109.8 . . ? C5B C4B H20 109.8 . . ? H19 C4B H20 108.3 . . ? C4B C5B H21 109.8 . . ? C4B C5B H22 109.8 . . ? H21 C5B H22 108.3 . . ? B1 N3A C7A 117.25(18) . . ? B1 N3A H25 121.4 . . ? C7A N3A H25 121.4 . . ? B2 N4A C8A 115.62(18) . . ? B2 N4A H26 122.2 . . ? C8A N4A H26 122.2 . . ? N3A C7A C8A 106.8(3) . . ? N3A C7A C12A 107.5(2) . . ? C8A C7A C12A 107.0(3) . . ? N3A C7A H27 111.7 . . ? C8A C7A H27 111.7 . . ? C12A C7A H27 111.7 . . ? N4A C8A C7A 106.9(3) . . ? N4A C8A C9A 105.9(2) . . ? C7A C8A C9A 108.5(3) . . ? N4A C8A H28 111.8 . . ? C7A C8A H28 111.8 . . ? C9A C8A H28 111.8 . . ? C10A C9A C8A 119.7(2) . . ? C10A C9A H29 107.4 . . ? C8A C9A H29 107.4 . . ? C10A C9A H30 107.4 . . ? C8A C9A H30 107.4 . . ? H29 C9A H30 106.9 . . ? C11A C10A C9A 108.0(3) . . ? C11A C10A H31 110.1 . . ? C9A C10A H31 110.1 . . ? C11A C10A H32 110.1 . . ? C9A C10A H32 110.1 . . ? H31 C10A H32 108.4 . . ? C10A C11A C12A 109.0(3) . . ? C10A C11A H33 109.9 . . ? C12A C11A H33 109.9 . . ? C10A C11A H34 109.9 . . ? C12A C11A H34 109.9 . . ? H33 C11A H34 108.3 . . ? C7A C12A C11A 119.0(2) . . ? C7A C12A H35 107.6 . . ? C11A C12A H35 107.6 . . ? C7A C12A H36 107.6 . . ? C11A C12A H36 107.6 . . ? H35 C12A H36 107.0 . . ? C8B C7B H39 111.0 . . ? C7B C8B H40 111.3 . . ? C11B C10B H43 110.1 . . ? C11B C10B H44 110.1 . . ? H43 C10B H44 108.5 . . ? C10B C11B H45 110.2 . . ? C10B C11B H46 110.2 . . ? H45 C11B H46 108.5 . . ? 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 N3A B1 B2 N4A 0.0(2) . . . . ? N1A B1 B2 N4A -179.90(16) . . . . ? N3A B1 B2 N2A -179.85(16) . . . . ? N1A B1 B2 N2A 0.2(2) . . . . ? N3A B1 N1A C1A 167.7(3) . . . . ? B2 B1 N1A C1A -12.4(3) . . . . ? N4A B2 N2A C2A 157.7(2) . . . . ? B1 B2 N2A C2A -22.4(3) . . . . ? B1 N1A C1A C2A 44.7(4) . . . . ? B1 N1A C1A C6A 162.7(2) . . . . ? B2 N2A C2A C1A 54.6(4) . . . . ? B2 N2A C2A C3A 172.5(2) . . . . ? N1A C1A C2A N2A -64.9(4) . . . . ? C6A C1A C2A N2A 175.4(3) . . . . ? N1A C1A C2A C3A 179.3(3) . . . . ? C6A C1A C2A C3A 59.6(4) . . . . ? N2A C2A C3A C4A -146.7(3) . . . . ? C1A C2A C3A C4A -29.2(5) . . . . ? C2A C3A C4A C5A -31.4(5) . . . . ? C3A C4A C5A C6A 58.9(5) . . . . ? N1A C1A C6A C5A -151.7(3) . . . . ? C2A C1A C6A C5A -32.1(5) . . . . ? C4A C5A C6A C1A -28.8(6) . . . . ? N1A B1 N3A C7A -162.4(2) . . . . ? B2 B1 N3A C7A 17.7(3) . . . . ? N2A B2 N4A C8A -159.6(2) . . . . ? B1 B2 N4A C8A 20.5(3) . . . . ? B1 N3A C7A C8A -53.2(3) . . . . ? B1 N3A C7A C12A -167.74(18) . . . . ? B2 N4A C8A C7A -56.1(3) . . . . ? B2 N4A C8A C9A -171.63(18) . . . . ? N3A C7A C8A N4A 71.6(3) . . . . ? C12A C7A C8A N4A -173.5(2) . . . . ? N3A C7A C8A C9A -174.6(2) . . . . ? C12A C7A C8A C9A -59.7(3) . . . . ? N4A C8A C9A C10A 144.9(3) . . . . ? C7A C8A C9A C10A 30.5(4) . . . . ? C8A C9A C10A C11A 31.0(4) . . . . ? C9A C10A C11A C12A -58.3(4) . . . . ? N3A C7A C12A C11A 147.1(3) . . . . ? C8A C7A C12A C11A 32.6(4) . . . . ? C10A C11A C12A C7A 28.3(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.353 _refine_diff_density_min -0.180 _refine_diff_density_rms 0.042 data_10 _database_code_depnum_ccdc_archive 'CCDC 848889' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H48 B2 N4 Sn4' _chemical_formula_sum 'C32 H48 B2 N4 Sn4' _chemical_formula_weight 985.12 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.0776(9) _cell_length_b 11.7668(5) _cell_length_c 17.1289(7) _cell_angle_alpha 90.00 _cell_angle_beta 117.968(2) _cell_angle_gamma 90.00 _cell_volume 3752.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9890 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 28.04 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 2.658 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6465 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS-2008/1 - Bruker AXS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35374 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 28.36 _reflns_number_total 4639 _reflns_number_gt 3870 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+22.1188P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4639 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0917 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.026 _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 B1 B 0.0314(2) 0.8706(4) 0.2314(3) 0.0206(8) Uani 1 1 d . . . N1 N 0.08868(16) 0.9527(3) 0.2647(2) 0.0192(6) Uani 1 1 d . . . N2 N 0.02770(17) 0.7884(3) 0.1669(2) 0.0215(7) Uani 1 1 d . . . C1 C 0.1400(2) 0.9530(3) 0.2338(3) 0.0211(7) Uani 1 1 d . . . C2 C 0.1924(2) 1.0361(4) 0.2588(3) 0.0276(9) Uani 1 1 d . . . H2 H 0.1915 1.0985 0.2936 0.033 Uiso 1 1 calc R . . C3 C 0.2470(2) 1.0299(4) 0.2338(3) 0.0329(10) Uani 1 1 d . . . H3 H 0.2827 1.0874 0.2523 0.039 Uiso 1 1 calc R . . C4 C 0.2492(2) 0.9431(4) 0.1837(3) 0.0271(9) Uani 1 1 d . . . H4 H 0.2876 0.9386 0.1696 0.033 Uiso 1 1 calc R . . C5 C 0.1945(2) 0.7712(4) 0.0955(3) 0.0268(9) Uani 1 1 d . . . H5 H 0.2315 0.7665 0.0788 0.032 Uiso 1 1 calc R . . C6 C 0.1407(2) 0.6924(4) 0.0646(3) 0.0284(9) Uani 1 1 d . . . H6 H 0.1406 0.6338 0.0264 0.034 Uiso 1 1 calc R . . C7 C 0.0857(2) 0.6969(3) 0.0884(3) 0.0255(8) Uani 1 1 d . . . H7 H 0.0492 0.6406 0.0665 0.031 Uiso 1 1 calc R . . C8 C 0.08320(19) 0.7813(3) 0.1431(3) 0.0203(7) Uani 1 1 d . . . C9 C 0.13938(19) 0.8647(3) 0.1770(2) 0.0187(7) Uani 1 1 d . . . C10 C 0.1956(2) 0.8597(3) 0.1521(3) 0.0221(8) Uani 1 1 d . . . C11 C 0.2182(2) 1.0097(4) 0.4640(3) 0.0314(9) Uani 1 1 d . . . H11A H 0.2357 0.9551 0.4353 0.047 Uiso 1 1 calc R . . H11B H 0.2189 0.9746 0.5163 0.047 Uiso 1 1 calc R . . H11C H 0.2493 1.0770 0.4819 0.047 Uiso 1 1 calc R . . C12 C 0.0986(2) 1.2308(4) 0.3268(3) 0.0338(10) Uani 1 1 d . . . H12A H 0.0944 1.2316 0.2673 0.051 Uiso 1 1 calc R . . H12B H 0.1407 1.2753 0.3668 0.051 Uiso 1 1 calc R . . H12C H 0.0553 1.2640 0.3249 0.051 Uiso 1 1 calc R . . C13 C 0.0424(2) 1.0367(4) 0.4334(3) 0.0337(10) Uani 1 1 d . . . H13A H -0.0070 1.0569 0.3909 0.051 Uiso 1 1 calc R . . H13B H 0.0589 1.0859 0.4855 0.051 Uiso 1 1 calc R . . H13C H 0.0440 0.9572 0.4513 0.051 Uiso 1 1 calc R . . C14 C -0.1015(3) 0.7169(6) -0.0404(4) 0.0545(15) Uani 1 1 d . . . H14A H -0.1449 0.7636 -0.0610 0.082 Uiso 1 1 calc R . . H14B H -0.1132 0.6457 -0.0740 0.082 Uiso 1 1 calc R . . H14C H -0.0650 0.7583 -0.0492 0.082 Uiso 1 1 calc R . . C15 C -0.1460(3) 0.6992(5) 0.1293(4) 0.0579(17) Uani 1 1 d . . . H15A H -0.1288 0.6792 0.1915 0.087 Uiso 1 1 calc R . . H15B H -0.1858 0.6491 0.0918 0.087 Uiso 1 1 calc R . . H15C H -0.1625 0.7783 0.1196 0.087 Uiso 1 1 calc R . . C16 C -0.0195(4) 0.5103(4) 0.1308(5) 0.0597(17) Uani 1 1 d . . . H16A H 0.0293 0.5130 0.1803 0.090 Uiso 1 1 calc R . . H16B H -0.0185 0.4746 0.0797 0.090 Uiso 1 1 calc R . . H16C H -0.0504 0.4658 0.1478 0.090 Uiso 1 1 calc R . . Sn1 Sn 0.110663(13) 1.05894(2) 0.373464(17) 0.02087(9) Uani 1 1 d . . . Sn2 Sn -0.061078(17) 0.67996(3) 0.09681(2) 0.03450(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.022(2) 0.020(2) 0.021(2) 0.0048(17) 0.0110(17) 0.0024(16) N1 0.0210(15) 0.0234(16) 0.0180(15) 0.0001(13) 0.0131(13) 0.0010(12) N2 0.0258(16) 0.0188(15) 0.0278(17) -0.0015(13) 0.0191(14) -0.0010(12) C1 0.0198(17) 0.0276(19) 0.0176(18) 0.0044(15) 0.0102(15) 0.0026(14) C2 0.029(2) 0.032(2) 0.027(2) -0.0067(18) 0.0186(18) -0.0078(17) C3 0.027(2) 0.047(3) 0.030(2) -0.007(2) 0.0175(19) -0.0127(18) C4 0.0233(19) 0.041(2) 0.023(2) -0.0008(18) 0.0159(17) -0.0017(17) C5 0.0230(19) 0.037(2) 0.025(2) 0.0023(18) 0.0150(17) 0.0065(16) C6 0.031(2) 0.031(2) 0.029(2) -0.0022(18) 0.0193(19) 0.0057(17) C7 0.0272(19) 0.0236(19) 0.030(2) -0.0018(17) 0.0173(18) 0.0008(15) C8 0.0222(18) 0.0195(18) 0.0219(19) 0.0051(15) 0.0126(15) 0.0042(14) C9 0.0178(16) 0.0253(18) 0.0154(17) 0.0049(15) 0.0098(14) 0.0032(14) C10 0.0188(17) 0.030(2) 0.0185(18) 0.0025(16) 0.0100(15) 0.0023(15) C11 0.025(2) 0.045(3) 0.024(2) -0.0001(19) 0.0112(18) 0.0064(18) C12 0.030(2) 0.026(2) 0.042(3) 0.0005(19) 0.014(2) 0.0037(17) C13 0.036(2) 0.045(3) 0.030(2) -0.018(2) 0.024(2) -0.013(2) C14 0.041(3) 0.074(4) 0.042(3) -0.014(3) 0.014(2) -0.011(3) C15 0.048(3) 0.069(4) 0.076(4) -0.044(3) 0.044(3) -0.042(3) C16 0.098(5) 0.028(3) 0.075(4) -0.017(3) 0.059(4) -0.020(3) Sn1 0.01905(13) 0.02488(15) 0.02137(14) -0.00262(10) 0.01172(11) 0.00121(9) Sn2 0.03853(18) 0.03472(18) 0.0398(2) -0.01436(14) 0.02633(16) -0.01491(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N1 1.438(5) . ? B1 N2 1.443(5) . ? B1 B1 1.719(8) 2 ? N1 C1 1.409(5) . ? N1 Sn1 2.107(3) . ? N2 C8 1.410(5) . ? N2 Sn2 2.112(3) . ? C1 C2 1.384(5) . ? C1 C9 1.419(5) . ? C2 C3 1.406(6) . ? C2 H2 0.9500 . ? C3 C4 1.348(6) . ? C3 H3 0.9500 . ? C4 C10 1.398(6) . ? C4 H4 0.9500 . ? C5 C6 1.364(6) . ? C5 C10 1.416(6) . ? C5 H5 0.9500 . ? C6 C7 1.399(5) . ? C6 H6 0.9500 . ? C7 C8 1.383(6) . ? C7 H7 0.9500 . ? C8 C9 1.435(5) . ? C9 C10 1.437(5) . ? C11 Sn1 2.141(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 Sn1 2.146(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 Sn1 2.141(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 Sn2 2.136(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 Sn2 2.120(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 Sn2 2.148(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 B1 N2 119.3(3) . . ? N1 B1 B1 120.1(3) . 2 ? N2 B1 B1 120.6(3) . 2 ? C1 N1 B1 120.1(3) . . ? C1 N1 Sn1 116.2(2) . . ? B1 N1 Sn1 123.0(2) . . ? C8 N2 B1 120.4(3) . . ? C8 N2 Sn2 115.7(2) . . ? B1 N2 Sn2 123.8(2) . . ? C2 C1 N1 121.8(4) . . ? C2 C1 C9 118.6(3) . . ? N1 C1 C9 119.6(3) . . ? C1 C2 C3 121.1(4) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C4 C3 C2 120.7(4) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C10 121.0(4) . . ? C3 C4 H4 119.5 . . ? C10 C4 H4 119.5 . . ? C6 C5 C10 120.7(4) . . ? C6 C5 H5 119.7 . . ? C10 C5 H5 119.7 . . ? C5 C6 C7 120.8(4) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C8 C7 C6 121.7(4) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C7 C8 N2 122.6(3) . . ? C7 C8 C9 118.6(3) . . ? N2 C8 C9 118.8(3) . . ? C1 C9 C8 121.3(3) . . ? C1 C9 C10 119.3(3) . . ? C8 C9 C10 119.4(3) . . ? C4 C10 C5 122.2(3) . . ? C4 C10 C9 119.0(4) . . ? C5 C10 C9 118.8(4) . . ? Sn1 C11 H11A 109.5 . . ? Sn1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Sn1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Sn1 C12 H12A 109.5 . . ? Sn1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Sn1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Sn1 C13 H13A 109.5 . . ? Sn1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Sn1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Sn2 C14 H14A 109.5 . . ? Sn2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Sn2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Sn2 C15 H15A 109.5 . . ? Sn2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Sn2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Sn2 C16 H16A 109.5 . . ? Sn2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Sn2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 Sn1 C13 115.67(14) . . ? N1 Sn1 C11 101.49(15) . . ? C13 Sn1 C11 109.95(18) . . ? N1 Sn1 C12 106.94(16) . . ? C13 Sn1 C12 107.79(19) . . ? C11 Sn1 C12 115.14(18) . . ? N2 Sn2 C15 114.71(16) . . ? N2 Sn2 C14 107.00(18) . . ? C15 Sn2 C14 108.5(3) . . ? N2 Sn2 C16 105.5(2) . . ? C15 Sn2 C16 108.4(3) . . ? C14 Sn2 C16 112.9(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 B1 N1 C1 0.6(5) . . . . ? B1 B1 N1 C1 -179.6(3) 2 . . . ? N2 B1 N1 Sn1 -169.5(3) . . . . ? B1 B1 N1 Sn1 10.3(5) 2 . . . ? N1 B1 N2 C8 6.1(5) . . . . ? B1 B1 N2 C8 -173.7(4) 2 . . . ? N1 B1 N2 Sn2 -169.9(3) . . . . ? B1 B1 N2 Sn2 10.3(5) 2 . . . ? B1 N1 C1 C2 174.7(4) . . . . ? Sn1 N1 C1 C2 -14.5(5) . . . . ? B1 N1 C1 C9 -6.8(5) . . . . ? Sn1 N1 C1 C9 164.0(3) . . . . ? N1 C1 C2 C3 174.3(4) . . . . ? C9 C1 C2 C3 -4.2(6) . . . . ? C1 C2 C3 C4 0.8(7) . . . . ? C2 C3 C4 C10 2.8(7) . . . . ? C10 C5 C6 C7 -0.3(6) . . . . ? C5 C6 C7 C8 0.6(7) . . . . ? C6 C7 C8 N2 179.0(4) . . . . ? C6 C7 C8 C9 -1.0(6) . . . . ? B1 N2 C8 C7 173.4(4) . . . . ? Sn2 N2 C8 C7 -10.2(5) . . . . ? B1 N2 C8 C9 -6.5(5) . . . . ? Sn2 N2 C8 C9 169.9(3) . . . . ? C2 C1 C9 C8 -175.0(4) . . . . ? N1 C1 C9 C8 6.4(5) . . . . ? C2 C1 C9 C10 4.2(5) . . . . ? N1 C1 C9 C10 -174.4(3) . . . . ? C7 C8 C9 C1 -179.7(4) . . . . ? N2 C8 C9 C1 0.2(5) . . . . ? C7 C8 C9 C10 1.1(5) . . . . ? N2 C8 C9 C10 -178.9(3) . . . . ? C3 C4 C10 C5 176.5(4) . . . . ? C3 C4 C10 C9 -2.7(6) . . . . ? C6 C5 C10 C4 -178.7(4) . . . . ? C6 C5 C10 C9 0.4(6) . . . . ? C1 C9 C10 C4 -0.8(6) . . . . ? C8 C9 C10 C4 178.4(4) . . . . ? C1 C9 C10 C5 180.0(4) . . . . ? C8 C9 C10 C5 -0.8(5) . . . . ? C1 N1 Sn1 C13 -170.0(3) . . . . ? B1 N1 Sn1 C13 0.5(4) . . . . ? C1 N1 Sn1 C11 -51.0(3) . . . . ? B1 N1 Sn1 C11 119.4(3) . . . . ? C1 N1 Sn1 C12 70.0(3) . . . . ? B1 N1 Sn1 C12 -119.6(3) . . . . ? C8 N2 Sn2 C15 -176.8(3) . . . . ? B1 N2 Sn2 C15 -0.6(4) . . . . ? C8 N2 Sn2 C14 -56.5(3) . . . . ? B1 N2 Sn2 C14 119.7(3) . . . . ? C8 N2 Sn2 C16 64.0(3) . . . . ? B1 N2 Sn2 C16 -119.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.141 _refine_diff_density_min -1.420 _refine_diff_density_rms 0.133 data_11 _database_code_depnum_ccdc_archive 'CCDC 848890' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 B2 N4 Sn2' _chemical_formula_sum 'C24 H24 B2 N4 Sn2' _chemical_formula_weight 627.47 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7066(4) _cell_length_b 9.6996(3) _cell_length_c 11.9435(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.769(2) _cell_angle_gamma 90.00 _cell_volume 1204.69(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22652 _cell_measurement_theta_min 2.732 _cell_measurement_theta_max 28.291 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 2.092 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4585 _exptl_absorpt_correction_T_max 0.5369 _exptl_absorpt_process_details 'SADABS-2008/1 - Bruker AXS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '/omega and /phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30698 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0112 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 28.36 _reflns_number_total 2995 _reflns_number_gt 2798 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER APEXII' _computing_cell_refinement 'BRUKER SAINT' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELX _computing_publication_material SHELX _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^)+(0.0516P)^2^+0.7127P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2995 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_gt 0.0203 _refine_ls_wR_factor_ref 0.0722 _refine_ls_wR_factor_gt 0.0657 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.007 _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 B1 B 0.4407(2) -0.0142(2) 0.94323(19) 0.0208(4) Uani 1 1 d . . . N1 N 0.32567(16) 0.06228(16) 0.93361(15) 0.0205(3) Uani 1 1 d . . . N2 N 0.45820(16) -0.11424(17) 0.86266(15) 0.0218(3) Uani 1 1 d . . . Sn1 Sn 0.355386(12) 0.190347(12) 1.077812(11) 0.01926(7) Uani 1 1 d . . . C1 C 0.22136(18) 0.03366(18) 0.84197(16) 0.0195(3) Uani 1 1 d . . . C2 C 0.1043(2) 0.1005(2) 0.82834(18) 0.0233(4) Uani 1 1 d . . . H2 H 0.0930 0.1662 0.8841 0.028 Uiso 1 1 calc R . . C3 C 0.00265(19) 0.0723(2) 0.73342(19) 0.0254(4) Uani 1 1 d . . . H3 H -0.0765 0.1201 0.7249 0.030 Uiso 1 1 calc R . . C4 C 0.0158(2) -0.0230(2) 0.65300(18) 0.0248(4) Uani 1 1 d . . . H4 H -0.0544 -0.0407 0.5893 0.030 Uiso 1 1 calc R . . C5 C 0.1330(2) -0.09604(19) 0.66309(17) 0.0219(4) Uani 1 1 d . . . C6 C 0.1479(2) -0.19402(18) 0.5789(2) 0.0248(4) Uani 1 1 d . . . H6 H 0.0783 -0.2129 0.5149 0.030 Uiso 1 1 calc R . . C7 C 0.2627(2) -0.2614(2) 0.59014(19) 0.0280(4) Uani 1 1 d . . . H7 H 0.2719 -0.3258 0.5327 0.034 Uiso 1 1 calc R . . C8 C 0.3666(2) -0.2377(2) 0.68410(18) 0.0251(4) Uani 1 1 d . . . H8 H 0.4445 -0.2871 0.6903 0.030 Uiso 1 1 calc R . . C9 C 0.35693(19) -0.14281(18) 0.76824(17) 0.0200(4) Uani 1 1 d . . . C10 C 0.23750(18) -0.06852(18) 0.75899(16) 0.0190(3) Uani 1 1 d . . . C11 C 0.2368(2) 0.1288(2) 1.1876(2) 0.0346(5) Uani 1 1 d . . . H11A H 0.1463 0.1362 1.1461 0.052 Uiso 1 1 calc R . . H11B H 0.2528 0.1887 1.2556 0.052 Uiso 1 1 calc R . . H11C H 0.2563 0.0331 1.2118 0.052 Uiso 1 1 calc R . . C12 C 0.3637(2) 0.3987(2) 1.0266(2) 0.0308(5) Uani 1 1 d . . . H12A H 0.4252 0.4073 0.9780 0.046 Uiso 1 1 calc R . . H12B H 0.3914 0.4569 1.0951 0.046 Uiso 1 1 calc R . . H12C H 0.2784 0.4281 0.9831 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0213(10) 0.0185(9) 0.0233(10) -0.0002(8) 0.0068(8) 0.0003(7) N1 0.0226(8) 0.0160(7) 0.0245(8) -0.0034(6) 0.0086(6) 0.0004(6) N2 0.0235(8) 0.0181(7) 0.0245(8) -0.0022(6) 0.0068(7) 0.0026(6) Sn1 0.02101(11) 0.01437(10) 0.02413(11) -0.00233(4) 0.00880(7) 0.00113(4) C1 0.0224(9) 0.0147(8) 0.0226(9) 0.0010(6) 0.0080(7) -0.0011(6) C2 0.0243(9) 0.0182(8) 0.0297(10) -0.0009(7) 0.0107(8) 0.0008(7) C3 0.0210(9) 0.0240(9) 0.0322(10) 0.0025(8) 0.0087(8) 0.0019(7) C4 0.0213(9) 0.0253(9) 0.0274(10) 0.0017(7) 0.0051(8) -0.0032(7) C5 0.0244(9) 0.0166(8) 0.0249(9) 0.0007(7) 0.0066(8) -0.0020(7) C6 0.0291(11) 0.0181(10) 0.0262(11) -0.0020(6) 0.0044(9) -0.0051(7) C7 0.0375(11) 0.0180(9) 0.0280(10) -0.0039(7) 0.0068(9) -0.0006(8) C8 0.0302(10) 0.0174(9) 0.0279(10) -0.0026(7) 0.0075(8) 0.0033(8) C9 0.0241(9) 0.0133(8) 0.0240(9) 0.0012(6) 0.0082(7) -0.0006(7) C10 0.0221(9) 0.0132(8) 0.0230(9) 0.0017(6) 0.0080(7) -0.0015(6) C11 0.0418(13) 0.0289(11) 0.0413(12) -0.0038(9) 0.0261(11) -0.0009(9) C12 0.0318(11) 0.0159(9) 0.0441(13) 0.0032(8) 0.0078(10) 0.0006(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N2 1.411(3) . ? B1 N1 1.418(3) . ? B1 B1 1.646(4) 3_657 ? N1 C1 1.393(3) . ? N1 Sn1 2.0856(16) . ? N2 C9 1.394(3) . ? N2 Sn1 2.0876(17) 3_657 ? Sn1 N2 2.0877(17) 3_657 ? Sn1 C11 2.117(2) . ? Sn1 C12 2.119(2) . ? C1 C2 1.386(3) . ? C1 C10 1.441(3) . ? C2 C3 1.399(3) . ? C2 H2 0.9500 . ? C3 C4 1.364(3) . ? C3 H3 0.9500 . ? C4 C5 1.421(3) . ? C4 H4 0.9500 . ? C5 C6 1.420(3) . ? C5 C10 1.423(3) . ? C6 C7 1.370(3) . ? C6 H6 0.9500 . ? C7 C8 1.398(3) . ? C7 H7 0.9500 . ? C8 C9 1.384(3) . ? C8 H8 0.9500 . ? C9 C10 1.449(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 B1 N1 123.96(19) . . ? N2 B1 B1 118.4(2) . 3_657 ? N1 B1 B1 117.7(2) . 3_657 ? C1 N1 B1 118.53(16) . . ? C1 N1 Sn1 134.73(12) . . ? B1 N1 Sn1 106.60(13) . . ? C9 N2 B1 118.98(17) . . ? C9 N2 Sn1 134.58(13) . 3_657 ? B1 N2 Sn1 106.42(13) . 3_657 ? N1 Sn1 N2 90.93(6) . 3_657 ? N1 Sn1 C11 110.33(8) . . ? N2 Sn1 C11 110.82(9) 3_657 . ? N1 Sn1 C12 109.77(8) . . ? N2 Sn1 C12 109.45(8) 3_657 . ? C11 Sn1 C12 121.34(9) . . ? C2 C1 N1 122.19(17) . . ? C2 C1 C10 119.61(18) . . ? N1 C1 C10 118.20(16) . . ? C1 C2 C3 120.75(18) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C4 C3 C2 120.79(18) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 121.0(2) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 121.3(2) . . ? C6 C5 C10 119.77(19) . . ? C4 C5 C10 118.93(18) . . ? C7 C6 C5 120.0(2) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 121.6(2) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C9 C8 C7 120.64(19) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 N2 122.79(18) . . ? C8 C9 C10 119.48(19) . . ? N2 C9 C10 117.73(16) . . ? C5 C10 C1 118.87(17) . . ? C5 C10 C9 118.59(17) . . ? C1 C10 C9 122.53(18) . . ? Sn1 C11 H11A 109.5 . . ? Sn1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Sn1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Sn1 C12 H12A 109.5 . . ? Sn1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Sn1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 B1 N1 C1 2.8(3) . . . . ? B1 B1 N1 C1 -176.1(2) 3_657 . . . ? N2 B1 N1 Sn1 179.04(16) . . . . ? B1 B1 N1 Sn1 0.2(3) 3_657 . . . ? N1 B1 N2 C9 -1.1(3) . . . . ? B1 B1 N2 C9 177.8(2) 3_657 . . . ? N1 B1 N2 Sn1 179.90(16) . . . 3_657 ? B1 B1 N2 Sn1 -1.3(3) 3_657 . . 3_657 ? C1 N1 Sn1 N2 175.77(18) . . . 3_657 ? B1 N1 Sn1 N2 0.38(13) . . . 3_657 ? C1 N1 Sn1 C11 63.13(19) . . . . ? B1 N1 Sn1 C11 -112.26(14) . . . . ? C1 N1 Sn1 C12 -73.15(19) . . . . ? B1 N1 Sn1 C12 111.46(14) . . . . ? B1 N1 C1 C2 177.91(18) . . . . ? Sn1 N1 C1 C2 2.9(3) . . . . ? B1 N1 C1 C10 -2.4(3) . . . . ? Sn1 N1 C1 C10 -177.42(13) . . . . ? N1 C1 C2 C3 178.05(18) . . . . ? C10 C1 C2 C3 -1.6(3) . . . . ? C1 C2 C3 C4 0.9(3) . . . . ? C2 C3 C4 C5 -0.1(3) . . . . ? C3 C4 C5 C6 -179.18(19) . . . . ? C3 C4 C5 C10 0.0(3) . . . . ? C4 C5 C6 C7 179.04(19) . . . . ? C10 C5 C6 C7 -0.2(3) . . . . ? C5 C6 C7 C8 0.9(3) . . . . ? C6 C7 C8 C9 -1.1(3) . . . . ? C7 C8 C9 N2 -179.16(18) . . . . ? C7 C8 C9 C10 0.5(3) . . . . ? B1 N2 C9 C8 178.87(19) . . . . ? Sn1 N2 C9 C8 -2.4(3) 3_657 . . . ? B1 N2 C9 C10 -0.8(3) . . . . ? Sn1 N2 C9 C10 177.89(13) 3_657 . . . ? C6 C5 C10 C1 178.55(17) . . . . ? C4 C5 C10 C1 -0.7(3) . . . . ? C6 C5 C10 C9 -0.4(3) . . . . ? C4 C5 C10 C9 -179.59(17) . . . . ? C2 C1 C10 C5 1.4(3) . . . . ? N1 C1 C10 C5 -178.21(16) . . . . ? C2 C1 C10 C9 -179.68(17) . . . . ? N1 C1 C10 C9 0.7(3) . . . . ? C8 C9 C10 C5 0.2(3) . . . . ? N2 C9 C10 C5 179.89(16) . . . . ? C8 C9 C10 C1 -178.69(18) . . . . ? N2 C9 C10 C1 1.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.100 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.090 data_12 _database_code_depnum_ccdc_archive 'CCDC 848891' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H32 B2 N4 Sn2, 2(C4 H8 O)' _chemical_formula_sum 'C52 H48 B2 N4 O2 Sn2' _chemical_formula_weight 1019.94 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 25.8356(7) _cell_length_b 16.9206(4) _cell_length_c 15.1685(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.211(2) _cell_angle_gamma 90.00 _cell_volume 6630.9(3) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9937 _cell_measurement_theta_min 2.654 _cell_measurement_theta_max 29.3485 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3084 _exptl_absorpt_coefficient_mu 1.177 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6425 _exptl_absorpt_correction_T_max 0.7459 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II kappa CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 91482 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 29.66 _reflns_number_total 18633 _reflns_number_gt 14538 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+10.4147P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18633 _refine_ls_number_parameters 838 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0954 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.367365(8) 0.338072(12) 0.614731(12) 0.01567(5) Uani 1 1 d . . . Sn2 Sn 0.292344(8) 0.625018(12) 0.708755(12) 0.01533(5) Uani 1 1 d . . . Sn3 Sn 1.036701(8) 0.142325(12) 0.447287(13) 0.01572(5) Uani 1 1 d . . . B1 B 0.30189(13) 0.4706(2) 0.6384(2) 0.0177(7) Uani 1 1 d . . . B2 B 0.35427(13) 0.4873(2) 0.6979(2) 0.0178(7) Uani 1 1 d . . . B3 B 0.97273(14) 0.0083(2) 0.4732(2) 0.0188(7) Uani 1 1 d . . . C1 C 0.22069(12) 0.52176(18) 0.57985(18) 0.0169(6) Uani 1 1 d . . . C2 C 0.18373(12) 0.57925(19) 0.5704(2) 0.0198(6) Uani 1 1 d . . . H2 H 0.1868 0.6271 0.6029 0.024 Uiso 1 1 calc R . . C3 C 0.14120(13) 0.5685(2) 0.5133(2) 0.0255(7) Uani 1 1 d . . . H3 H 0.1162 0.6094 0.5070 0.031 Uiso 1 1 calc R . . C4 C 0.13555(13) 0.5001(2) 0.4672(2) 0.0257(7) Uani 1 1 d . . . H4 H 0.1066 0.4937 0.4292 0.031 Uiso 1 1 calc R . . C5 C 0.17245(12) 0.43812(19) 0.47523(19) 0.0201(6) Uani 1 1 d . . . C6 C 0.16689(13) 0.3659(2) 0.4289(2) 0.0238(7) Uani 1 1 d . . . H6 H 0.1382 0.3588 0.3903 0.029 Uiso 1 1 calc R . . C7 C 0.20209(13) 0.30637(19) 0.4388(2) 0.0226(7) Uani 1 1 d . . . H7 H 0.1970 0.2579 0.4084 0.027 Uiso 1 1 calc R . . C8 C 0.24576(12) 0.31578(19) 0.49328(19) 0.0196(6) Uani 1 1 d . . . H8 H 0.2698 0.2737 0.4996 0.023 Uiso 1 1 calc R . . C9 C 0.25388(11) 0.38611(17) 0.53773(17) 0.0157(6) Uani 1 1 d . . . C10 C 0.21645(11) 0.44865(17) 0.53150(18) 0.0160(6) Uani 1 1 d . . . C11 C 0.43917(11) 0.44407(19) 0.74359(18) 0.0180(6) Uani 1 1 d . . . C12 C 0.47906(12) 0.3901(2) 0.7471(2) 0.0240(7) Uani 1 1 d . . . H12 H 0.4759 0.3412 0.7169 0.029 Uiso 1 1 calc R . . C13 C 0.52430(13) 0.4069(2) 0.7952(2) 0.0291(8) Uani 1 1 d . . . H13 H 0.5511 0.3686 0.7975 0.035 Uiso 1 1 calc R . . C14 C 0.53069(14) 0.4766(2) 0.8384(2) 0.0310(8) Uani 1 1 d . . . H14 H 0.5617 0.4864 0.8704 0.037 Uiso 1 1 calc R . . C15 C 0.49124(12) 0.5347(2) 0.8360(2) 0.0234(7) Uani 1 1 d . . . C16 C 0.49724(14) 0.6089(2) 0.8775(2) 0.0286(8) Uani 1 1 d . . . H16 H 0.5281 0.6196 0.9096 0.034 Uiso 1 1 calc R . . C17 C 0.45998(13) 0.6653(2) 0.8727(2) 0.0265(7) Uani 1 1 d . . . H17 H 0.4655 0.7151 0.8999 0.032 Uiso 1 1 calc R . . C18 C 0.41306(13) 0.6506(2) 0.82766(19) 0.0221(6) Uani 1 1 d . . . H18 H 0.3871 0.6903 0.8257 0.027 Uiso 1 1 calc R . . C19 C 0.40462(11) 0.57873(19) 0.78628(17) 0.0177(6) Uani 1 1 d . . . C20 C 0.44413(11) 0.51909(19) 0.78872(18) 0.0177(6) Uani 1 1 d . . . C21 C 0.42287(11) 0.34122(17) 0.51192(18) 0.0157(6) Uani 1 1 d . . . C22 C 0.44249(12) 0.41496(18) 0.4869(2) 0.0201(6) Uani 1 1 d . . . H22 H 0.4309 0.4612 0.5165 0.024 Uiso 1 1 calc R . . C23 C 0.47840(13) 0.4217(2) 0.4200(2) 0.0261(7) Uani 1 1 d . . . H23 H 0.4909 0.4723 0.4031 0.031 Uiso 1 1 calc R . . C24 C 0.49615(13) 0.3544(2) 0.3775(2) 0.0283(8) Uani 1 1 d . . . H24 H 0.5205 0.3587 0.3311 0.034 Uiso 1 1 calc R . . C25 C 0.47798(13) 0.2806(2) 0.4035(2) 0.0270(7) Uani 1 1 d . . . H25 H 0.4907 0.2343 0.3756 0.032 Uiso 1 1 calc R . . C26 C 0.44150(12) 0.27435(19) 0.4697(2) 0.0207(6) Uani 1 1 d . . . H26 H 0.4291 0.2237 0.4865 0.025 Uiso 1 1 calc R . . C27 C 0.34728(12) 0.23790(17) 0.68965(18) 0.0166(6) Uani 1 1 d . . . C28 C 0.38341(13) 0.18440(19) 0.7231(2) 0.0229(6) Uani 1 1 d . . . H28 H 0.4192 0.1919 0.7120 0.027 Uiso 1 1 calc R . . C29 C 0.36692(15) 0.1200(2) 0.7727(2) 0.0298(8) Uani 1 1 d . . . H29 H 0.3916 0.0835 0.7953 0.036 Uiso 1 1 calc R . . C30 C 0.31490(15) 0.1089(2) 0.7894(2) 0.0292(8) Uani 1 1 d . . . H30 H 0.3039 0.0647 0.8231 0.035 Uiso 1 1 calc R . . C31 C 0.27866(13) 0.1619(2) 0.75723(19) 0.0242(7) Uani 1 1 d . . . H31 H 0.2429 0.1544 0.7693 0.029 Uiso 1 1 calc R . . C32 C 0.29481(12) 0.22608(18) 0.70708(19) 0.0193(6) Uani 1 1 d . . . H32 H 0.2699 0.2622 0.6845 0.023 Uiso 1 1 calc R . . C33 C 0.24045(11) 0.64680(17) 0.81264(18) 0.0156(5) Uani 1 1 d . . . C34 C 0.21140(13) 0.58502(19) 0.8483(2) 0.0243(7) Uani 1 1 d . . . H34 H 0.2150 0.5331 0.8252 0.029 Uiso 1 1 calc R . . C35 C 0.17725(14) 0.5986(2) 0.9172(2) 0.0309(8) Uani 1 1 d . . . H35 H 0.1578 0.5562 0.9414 0.037 Uiso 1 1 calc R . . C36 C 0.17168(13) 0.6743(2) 0.9505(2) 0.0286(8) Uani 1 1 d . . . H36 H 0.1486 0.6836 0.9980 0.034 Uiso 1 1 calc R . . C37 C 0.19950(13) 0.7367(2) 0.9150(2) 0.0247(7) Uani 1 1 d . . . H37 H 0.1951 0.7887 0.9374 0.030 Uiso 1 1 calc R . . C38 C 0.23392(13) 0.72263(18) 0.84667(19) 0.0203(6) Uani 1 1 d . . . H38 H 0.2533 0.7653 0.8228 0.024 Uiso 1 1 calc R . . C39 C 0.31592(12) 0.72358(18) 0.63331(18) 0.0174(6) Uani 1 1 d . . . C40 C 0.28103(13) 0.78226(19) 0.6080(2) 0.0225(6) Uani 1 1 d . . . H40 H 0.2456 0.7779 0.6239 0.027 Uiso 1 1 calc R . . C41 C 0.29793(14) 0.8477(2) 0.5591(2) 0.0286(7) Uani 1 1 d . . . H41 H 0.2740 0.8874 0.5416 0.034 Uiso 1 1 calc R . . C42 C 0.34952(14) 0.8540(2) 0.5367(2) 0.0275(7) Uani 1 1 d . . . H42 H 0.3611 0.8985 0.5041 0.033 Uiso 1 1 calc R . . C43 C 0.38465(13) 0.7955(2) 0.5613(2) 0.0245(7) Uani 1 1 d . . . H43 H 0.4200 0.8001 0.5453 0.029 Uiso 1 1 calc R . . C44 C 0.36781(12) 0.73023(19) 0.60955(19) 0.0210(6) Uani 1 1 d . . . H44 H 0.3917 0.6903 0.6262 0.025 Uiso 1 1 calc R . . C45 C 0.92146(11) 0.09556(18) 0.38183(18) 0.0168(6) Uani 1 1 d . . . C46 C 0.91259(12) 0.16483(19) 0.33606(19) 0.0207(6) Uani 1 1 d . . . H46 H 0.9387 0.2044 0.3345 0.025 Uiso 1 1 calc R . . C47 C 0.86547(13) 0.1775(2) 0.2918(2) 0.0240(7) Uani 1 1 d . . . H47 H 0.8601 0.2255 0.2605 0.029 Uiso 1 1 calc R . . C48 C 0.82717(13) 0.1218(2) 0.2931(2) 0.0250(7) Uani 1 1 d . . . H48 H 0.7958 0.1312 0.2619 0.030 Uiso 1 1 calc R . . C49 C 0.83360(12) 0.05009(19) 0.34048(19) 0.0209(6) Uani 1 1 d . . . C50 C 0.79343(13) -0.0070(2) 0.3450(2) 0.0262(7) Uani 1 1 d . . . H50 H 0.7618 0.0019 0.3145 0.031 Uiso 1 1 calc R . . C51 C 0.79997(13) -0.0746(2) 0.3928(2) 0.0250(7) Uani 1 1 d . . . H51 H 0.7725 -0.1117 0.3962 0.030 Uiso 1 1 calc R . . C52 C 0.84684(12) -0.09033(19) 0.4373(2) 0.0201(6) Uani 1 1 d . . . H52 H 0.8508 -0.1382 0.4693 0.024 Uiso 1 1 calc R . . C53 C 0.88686(11) -0.03672(18) 0.43447(18) 0.0165(6) Uani 1 1 d . . . C54 C 0.88123(12) 0.03615(18) 0.38589(18) 0.0176(6) Uani 1 1 d . . . C55 C 1.08685(11) 0.16142(17) 0.33888(18) 0.0162(6) Uani 1 1 d . . . C56 C 1.12089(13) 0.1027(2) 0.3114(2) 0.0233(7) Uani 1 1 d . . . H56 H 1.1211 0.0530 0.3407 0.028 Uiso 1 1 calc R . . C57 C 1.15445(14) 0.1157(2) 0.2421(2) 0.0302(8) Uani 1 1 d . . . H57 H 1.1773 0.0751 0.2233 0.036 Uiso 1 1 calc R . . C58 C 1.15456(13) 0.1890(2) 0.1999(2) 0.0295(8) Uani 1 1 d . . . H58 H 1.1772 0.1982 0.1518 0.035 Uiso 1 1 calc R . . C59 C 1.12180(14) 0.2482(2) 0.2279(2) 0.0264(7) Uani 1 1 d . . . H59 H 1.1224 0.2984 0.1998 0.032 Uiso 1 1 calc R . . C60 C 1.08800(13) 0.23460(18) 0.2970(2) 0.0213(6) Uani 1 1 d . . . H60 H 1.0654 0.2755 0.3159 0.026 Uiso 1 1 calc R . . C61 C 1.01669(12) 0.24175(18) 0.52425(19) 0.0194(6) Uani 1 1 d . . . C62 C 0.96666(13) 0.2458(2) 0.5603(2) 0.0256(7) Uani 1 1 d . . . H62 H 0.9429 0.2038 0.5502 0.031 Uiso 1 1 calc R . . C63 C 0.95176(15) 0.3100(2) 0.6101(2) 0.0320(8) Uani 1 1 d . . . H63 H 0.9180 0.3121 0.6345 0.038 Uiso 1 1 calc R . . C64 C 0.98623(15) 0.3717(2) 0.6243(2) 0.0346(9) Uani 1 1 d . . . H64 H 0.9758 0.4163 0.6580 0.042 Uiso 1 1 calc R . . C65 C 1.03555(15) 0.3686(2) 0.5900(2) 0.0319(8) Uani 1 1 d . . . H65 H 1.0591 0.4107 0.6004 0.038 Uiso 1 1 calc R . . C66 C 1.05084(13) 0.30375(19) 0.5401(2) 0.0231(7) Uani 1 1 d . . . H66 H 1.0849 0.3018 0.5166 0.028 Uiso 1 1 calc R . . C67 C 0.35130(14) 0.6119(2) 0.2949(2) 0.0301(8) Uani 1 1 d . . . H67A H 0.3582 0.6611 0.2617 0.036 Uiso 1 1 calc R . . H67B H 0.3605 0.5662 0.2572 0.036 Uiso 1 1 calc R . . C68 C 0.38270(17) 0.6104(3) 0.3806(2) 0.0412(10) Uani 1 1 d . . . H68A H 0.4158 0.5816 0.3729 0.049 Uiso 1 1 calc R . . H68B H 0.3900 0.6645 0.4020 0.049 Uiso 1 1 calc R . . C69 C 0.34709(16) 0.5671(2) 0.4424(2) 0.0350(9) Uani 1 1 d . . . H69A H 0.3503 0.5091 0.4355 0.042 Uiso 1 1 calc R . . H69B H 0.3540 0.5815 0.5045 0.042 Uiso 1 1 calc R . . C70 C 0.29486(17) 0.5957(3) 0.4128(2) 0.0439(11) Uani 1 1 d . . . H70A H 0.2680 0.5559 0.4263 0.053 Uiso 1 1 calc R . . H70B H 0.2859 0.6457 0.4429 0.053 Uiso 1 1 calc R . . C71 C 0.02591(15) 0.5987(2) 0.6334(2) 0.0338(8) Uani 1 1 d . . . H71A H 0.0307 0.6480 0.5992 0.041 Uiso 1 1 calc R . . H71B H 0.0323 0.5531 0.5940 0.041 Uiso 1 1 calc R . . C72 C 0.06246(17) 0.5968(3) 0.7113(3) 0.0463(11) Uani 1 1 d . . . H72A H 0.0943 0.5668 0.6973 0.056 Uiso 1 1 calc R . . H72B H 0.0721 0.6509 0.7301 0.056 Uiso 1 1 calc R . . C73 C 0.03119(17) 0.5555(3) 0.7814(3) 0.0460(11) Uani 1 1 d . . . H73A H 0.0339 0.4973 0.7760 0.055 Uiso 1 1 calc R . . H73B H 0.0424 0.5716 0.8413 0.055 Uiso 1 1 calc R . . C74 C -0.02179(17) 0.5831(3) 0.7620(2) 0.0414(10) Uani 1 1 d . . . H74A H -0.0474 0.5432 0.7811 0.050 Uiso 1 1 calc R . . H74B H -0.0288 0.6331 0.7936 0.050 Uiso 1 1 calc R . . C77 C 0.30516(16) 0.0490(2) 0.4440(2) 0.0314(8) Uani 1 1 d . . . H77A H 0.3247 0.0066 0.4139 0.038 Uiso 1 1 calc R . . H77B H 0.2736 0.0261 0.4706 0.038 Uiso 1 1 calc R . . C78 C 0.33895(15) 0.0902(2) 0.5145(2) 0.0310(8) Uani 1 1 d . . . H78A H 0.3235 0.0835 0.5736 0.037 Uiso 1 1 calc R . . H78B H 0.3742 0.0671 0.5152 0.037 Uiso 1 1 calc R . . O3 O 0.34113(10) 0.17205(14) 0.49141(14) 0.0279(5) Uani 1 1 d . . . C75 C 0.33431(15) 0.1749(2) 0.3975(2) 0.0286(8) Uani 1 1 d . . . H75A H 0.3665 0.1595 0.3668 0.034 Uiso 1 1 calc R . . H75B H 0.3240 0.2285 0.3780 0.034 Uiso 1 1 calc R . . N1 N 0.26392(10) 0.53081(15) 0.63516(16) 0.0172(5) Uani 1 1 d . . . N2 N 0.29827(9) 0.39868(15) 0.58996(15) 0.0169(5) Uani 1 1 d . . . N3 N 0.39313(10) 0.42912(15) 0.69804(16) 0.0173(5) Uani 1 1 d . . . N4 N 0.35872(10) 0.56143(15) 0.74121(15) 0.0169(5) Uani 1 1 d . . . N5 N 0.96795(10) 0.08009(16) 0.42586(16) 0.0186(5) Uani 1 1 d . . . N6 N 0.93358(10) -0.04962(15) 0.47858(16) 0.0182(5) Uani 1 1 d . . . O1 O 0.29851(10) 0.60785(16) 0.31951(16) 0.0337(6) Uani 1 1 d . . . O2 O -0.02526(10) 0.59511(17) 0.66850(16) 0.0373(6) Uani 1 1 d . . . C76 C 0.29148(15) 0.1158(2) 0.3801(2) 0.0306(8) Uani 1 1 d . . . H76A H 0.2919 0.0972 0.3182 0.037 Uiso 1 1 calc R . . H76B H 0.2571 0.1385 0.3933 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.01289(10) 0.01895(10) 0.01518(9) 0.00128(7) 0.00145(7) 0.00228(8) Sn2 0.01315(10) 0.01776(10) 0.01511(9) -0.00100(7) 0.00233(7) 0.00041(8) Sn3 0.01345(10) 0.01672(10) 0.01700(9) -0.00180(7) 0.00236(7) -0.00203(7) B1 0.0130(16) 0.0240(17) 0.0161(14) -0.0021(12) -0.0006(12) 0.0023(13) B2 0.0144(16) 0.0223(17) 0.0167(14) -0.0004(12) 0.0002(12) 0.0013(13) B3 0.0155(17) 0.0227(17) 0.0183(15) -0.0017(13) 0.0012(12) -0.0026(14) C1 0.0146(14) 0.0193(14) 0.0168(13) 0.0014(11) 0.0023(11) 0.0019(11) C2 0.0143(15) 0.0220(15) 0.0231(14) 0.0011(12) 0.0004(11) 0.0012(12) C3 0.0190(17) 0.0274(17) 0.0302(16) 0.0048(13) -0.0032(13) 0.0062(14) C4 0.0175(16) 0.0338(19) 0.0257(16) 0.0003(13) -0.0070(12) 0.0030(14) C5 0.0149(15) 0.0255(16) 0.0199(14) 0.0005(12) -0.0006(11) -0.0022(12) C6 0.0190(16) 0.0298(17) 0.0224(15) -0.0037(13) -0.0036(12) -0.0045(13) C7 0.0237(17) 0.0235(16) 0.0206(14) -0.0064(12) 0.0021(12) -0.0046(13) C8 0.0195(16) 0.0215(15) 0.0177(13) -0.0013(11) 0.0033(11) 0.0012(12) C9 0.0160(14) 0.0184(14) 0.0128(12) -0.0002(10) 0.0027(10) -0.0002(11) C10 0.0152(14) 0.0187(14) 0.0141(12) 0.0017(10) 0.0006(10) -0.0017(11) C11 0.0107(14) 0.0264(16) 0.0169(13) 0.0065(11) 0.0005(10) -0.0013(12) C12 0.0172(16) 0.0242(16) 0.0307(16) 0.0071(13) -0.0029(13) -0.0017(13) C13 0.0143(16) 0.0330(19) 0.0401(19) 0.0122(15) -0.0051(14) -0.0009(14) C14 0.0178(17) 0.037(2) 0.0383(19) 0.0079(16) -0.0089(14) -0.0055(15) C15 0.0157(16) 0.0338(18) 0.0208(14) 0.0052(13) -0.0022(12) -0.0048(13) C16 0.0221(18) 0.039(2) 0.0245(15) 0.0006(14) -0.0058(13) -0.0125(15) C17 0.0228(17) 0.0347(19) 0.0218(15) -0.0050(13) 0.0010(13) -0.0089(15) C18 0.0179(16) 0.0301(17) 0.0184(13) -0.0030(12) 0.0036(12) -0.0018(13) C19 0.0129(14) 0.0285(16) 0.0117(12) 0.0005(11) 0.0029(10) -0.0025(12) C20 0.0127(14) 0.0269(16) 0.0134(12) 0.0027(11) 0.0007(10) -0.0041(12) C21 0.0129(14) 0.0185(14) 0.0156(12) 0.0019(10) -0.0001(10) 0.0033(11) C22 0.0177(16) 0.0186(15) 0.0239(14) 0.0006(11) 0.0013(12) -0.0006(12) C23 0.0220(17) 0.0303(18) 0.0260(16) 0.0076(13) -0.0010(13) -0.0067(14) C24 0.0170(16) 0.047(2) 0.0210(15) 0.0045(14) 0.0047(12) 0.0024(15) C25 0.0198(17) 0.0367(19) 0.0246(15) -0.0067(14) 0.0012(13) 0.0090(15) C26 0.0208(16) 0.0185(15) 0.0228(14) 0.0008(11) 0.0003(12) 0.0021(12) C27 0.0188(15) 0.0178(14) 0.0133(12) -0.0045(10) -0.0004(11) 0.0003(12) C28 0.0203(16) 0.0243(16) 0.0241(15) -0.0020(12) -0.0036(12) 0.0013(13) C29 0.036(2) 0.0223(17) 0.0311(17) 0.0025(13) -0.0120(15) 0.0019(15) C30 0.038(2) 0.0246(17) 0.0249(16) 0.0054(13) -0.0054(14) -0.0108(15) C31 0.0250(17) 0.0300(17) 0.0176(14) -0.0047(12) 0.0017(12) -0.0096(14) C32 0.0202(16) 0.0186(15) 0.0191(13) -0.0033(11) -0.0002(12) 0.0000(12) C33 0.0140(14) 0.0176(14) 0.0152(12) 0.0025(10) 0.0006(10) -0.0001(11) C34 0.0274(18) 0.0208(16) 0.0248(15) 0.0001(12) 0.0054(13) -0.0048(13) C35 0.033(2) 0.036(2) 0.0245(16) 0.0013(14) 0.0085(14) -0.0142(16) C36 0.0188(17) 0.046(2) 0.0211(15) -0.0051(14) 0.0076(13) 0.0006(15) C37 0.0257(18) 0.0233(16) 0.0250(15) -0.0047(12) 0.0030(13) 0.0083(14) C38 0.0240(17) 0.0171(14) 0.0197(13) 0.0024(11) 0.0032(12) 0.0014(12) C39 0.0165(15) 0.0222(15) 0.0134(12) -0.0031(11) 0.0001(11) -0.0012(12) C40 0.0177(16) 0.0274(17) 0.0225(14) 0.0002(12) 0.0011(12) 0.0008(13) C41 0.0299(19) 0.0260(17) 0.0300(17) 0.0053(14) -0.0008(14) 0.0025(15) C42 0.032(2) 0.0273(17) 0.0228(15) 0.0080(13) 0.0015(14) -0.0072(15) C43 0.0183(16) 0.0313(18) 0.0240(15) 0.0015(13) 0.0033(12) -0.0043(14) C44 0.0177(16) 0.0242(16) 0.0210(14) -0.0012(12) 0.0019(12) -0.0001(13) C45 0.0137(14) 0.0220(15) 0.0146(12) -0.0023(11) 0.0016(10) 0.0016(12) C46 0.0187(16) 0.0230(16) 0.0204(14) 0.0006(12) 0.0019(12) 0.0014(13) C47 0.0211(17) 0.0300(17) 0.0209(14) 0.0012(13) 0.0020(12) 0.0045(14) C48 0.0181(16) 0.0342(19) 0.0226(15) -0.0017(13) -0.0035(12) 0.0069(14) C49 0.0162(15) 0.0274(16) 0.0192(13) -0.0054(12) 0.0011(11) 0.0014(13) C50 0.0156(16) 0.0323(18) 0.0309(17) -0.0073(14) -0.0058(13) 0.0020(14) C51 0.0164(16) 0.0274(17) 0.0313(17) -0.0089(13) 0.0005(13) -0.0053(13) C52 0.0172(15) 0.0220(15) 0.0211(14) -0.0045(11) 0.0013(11) -0.0033(12) C53 0.0131(14) 0.0207(14) 0.0158(12) -0.0058(11) 0.0015(10) 0.0002(11) C54 0.0156(15) 0.0205(15) 0.0167(13) -0.0049(11) 0.0014(11) 0.0009(12) C55 0.0142(14) 0.0184(14) 0.0160(12) -0.0014(11) 0.0015(10) -0.0027(11) C56 0.0252(17) 0.0227(16) 0.0220(14) -0.0010(12) 0.0043(12) 0.0056(13) C57 0.0246(18) 0.039(2) 0.0267(16) -0.0028(14) 0.0075(14) 0.0097(15) C58 0.0193(17) 0.051(2) 0.0180(14) 0.0027(14) 0.0046(12) -0.0084(16) C59 0.0300(19) 0.0278(17) 0.0213(15) 0.0052(13) 0.0021(13) -0.0097(14) C60 0.0234(17) 0.0186(15) 0.0218(14) -0.0011(11) 0.0007(12) -0.0023(13) C61 0.0186(16) 0.0215(15) 0.0181(13) -0.0016(11) 0.0016(11) 0.0035(12) C62 0.0215(17) 0.0339(18) 0.0214(15) -0.0019(13) 0.0039(13) -0.0013(14) C63 0.0285(19) 0.044(2) 0.0234(16) -0.0038(15) 0.0046(14) 0.0131(17) C64 0.037(2) 0.036(2) 0.0301(18) -0.0156(15) -0.0055(15) 0.0144(17) C65 0.033(2) 0.0244(17) 0.0386(19) -0.0091(15) -0.0078(16) 0.0007(15) C66 0.0164(16) 0.0238(16) 0.0292(16) -0.0036(13) -0.0002(12) 0.0006(13) C67 0.034(2) 0.0322(19) 0.0245(16) 0.0068(14) 0.0056(14) 0.0063(16) C68 0.043(2) 0.047(2) 0.0333(19) 0.0074(17) -0.0005(17) -0.004(2) C69 0.055(3) 0.0267(18) 0.0234(16) 0.0030(14) 0.0047(16) 0.0096(18) C70 0.049(3) 0.049(2) 0.034(2) 0.0152(18) 0.0209(18) 0.016(2) C71 0.036(2) 0.035(2) 0.0305(17) 0.0075(15) 0.0089(15) 0.0089(17) C72 0.035(2) 0.060(3) 0.043(2) 0.020(2) 0.0008(18) -0.003(2) C73 0.046(3) 0.058(3) 0.035(2) 0.0112(19) 0.0046(18) 0.007(2) C74 0.046(3) 0.046(2) 0.0323(19) 0.0101(17) 0.0093(17) 0.007(2) C77 0.041(2) 0.0290(18) 0.0247(16) 0.0004(14) -0.0001(15) 0.0019(16) C78 0.032(2) 0.035(2) 0.0264(16) 0.0113(14) -0.0023(14) 0.0014(16) O3 0.0358(14) 0.0319(13) 0.0161(10) 0.0019(9) 0.0010(9) -0.0029(11) C75 0.038(2) 0.0297(18) 0.0179(14) 0.0038(13) 0.0026(14) 0.0044(16) N1 0.0136(12) 0.0197(12) 0.0185(11) -0.0033(9) -0.0014(9) 0.0022(10) N2 0.0122(12) 0.0204(12) 0.0180(11) -0.0024(9) -0.0013(9) 0.0024(10) N3 0.0133(12) 0.0213(13) 0.0173(11) -0.0002(9) -0.0007(9) 0.0003(10) N4 0.0124(12) 0.0213(13) 0.0171(11) -0.0029(9) -0.0008(9) 0.0011(10) N5 0.0130(13) 0.0236(13) 0.0191(11) -0.0011(10) 0.0000(9) -0.0026(10) N6 0.0133(12) 0.0208(13) 0.0204(12) -0.0009(10) -0.0006(9) -0.0026(10) O1 0.0328(15) 0.0391(15) 0.0293(12) 0.0041(11) 0.0088(11) 0.0058(12) O2 0.0360(16) 0.0470(17) 0.0289(13) 0.0031(12) 0.0039(11) 0.0067(13) C76 0.036(2) 0.0321(19) 0.0235(16) 0.0003(14) -0.0018(14) 0.0063(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 Sn1 N2 2.092(2) . ? Sn1 N3 2.099(3) . ? Sn1 C27 2.107(3) . ? Sn1 C21 2.123(3) . ? Sn2 N1 2.078(2) . ? Sn2 N4 2.082(2) . ? Sn2 C33 2.105(3) . ? Sn2 C39 2.114(3) . ? Sn3 N6 2.076(3) 3_756 ? Sn3 N5 2.089(3) . ? Sn3 C61 2.113(3) . ? Sn3 C55 2.122(3) . ? B1 N1 1.415(4) . ? B1 N2 1.424(4) . ? B1 B2 1.649(5) . ? B2 N3 1.406(4) . ? B2 N4 1.420(4) . ? B3 N6 1.411(4) . ? B3 N5 1.416(4) . ? B3 B3 1.648(7) 3_756 ? C1 C2 1.370(4) . ? C1 N1 1.403(4) . ? C1 C10 1.442(4) . ? C2 C3 1.408(4) . ? C2 H2 0.9500 . ? C3 C4 1.359(5) . ? C3 H3 0.9500 . ? C4 C5 1.423(5) . ? C4 H4 0.9500 . ? C5 C6 1.416(4) . ? C5 C10 1.430(4) . ? C6 C7 1.365(5) . ? C6 H6 0.9500 . ? C7 C8 1.405(4) . ? C7 H7 0.9500 . ? C8 C9 1.383(4) . ? C8 H8 0.9500 . ? C9 N2 1.408(4) . ? C9 C10 1.436(4) . ? C11 C12 1.378(4) . ? C11 N3 1.396(4) . ? C11 C20 1.448(4) . ? C12 C13 1.404(5) . ? C12 H12 0.9500 . ? C13 C14 1.360(5) . ? C13 H13 0.9500 . ? C14 C15 1.416(5) . ? C14 H14 0.9500 . ? C15 C16 1.414(5) . ? C15 C20 1.435(4) . ? C16 C17 1.356(5) . ? C16 H16 0.9500 . ? C17 C18 1.411(5) . ? C17 H17 0.9500 . ? C18 C19 1.385(4) . ? C18 H18 0.9500 . ? C19 N4 1.398(4) . ? C19 C20 1.436(4) . ? C21 C26 1.387(4) . ? C21 C22 1.400(4) . ? C22 C23 1.383(4) . ? C22 H22 0.9500 . ? C23 C24 1.386(5) . ? C23 H23 0.9500 . ? C24 C25 1.391(5) . ? C24 H24 0.9500 . ? C25 C26 1.384(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.394(4) . ? C27 C32 1.396(4) . ? C28 C29 1.392(5) . ? C28 H28 0.9500 . ? C29 C30 1.381(5) . ? C29 H29 0.9500 . ? C30 C31 1.383(5) . ? C30 H30 0.9500 . ? C31 C32 1.391(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.394(4) . ? C33 C34 1.397(4) . ? C34 C35 1.389(4) . ? C34 H34 0.9500 . ? C35 C36 1.384(5) . ? C35 H35 0.9500 . ? C36 C37 1.386(5) . ? C36 H36 0.9500 . ? C37 C38 1.389(4) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C44 1.394(4) . ? C39 C40 1.394(4) . ? C40 C41 1.402(5) . ? C40 H40 0.9500 . ? C41 C42 1.381(5) . ? C41 H41 0.9500 . ? C42 C43 1.393(5) . ? C42 H42 0.9500 . ? C43 C44 1.395(4) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.381(4) . ? C45 N5 1.397(4) . ? C45 C54 1.448(4) . ? C46 C47 1.405(4) . ? C46 H46 0.9500 . ? C47 C48 1.367(5) . ? C47 H47 0.9500 . ? C48 C49 1.419(5) . ? C48 H48 0.9500 . ? C49 C50 1.420(5) . ? C49 C54 1.428(4) . ? C50 C51 1.364(5) . ? C50 H50 0.9500 . ? C51 C52 1.409(5) . ? C51 H51 0.9500 . ? C52 C53 1.376(4) . ? C52 H52 0.9500 . ? C53 N6 1.395(4) . ? C53 C54 1.444(4) . ? C55 C60 1.392(4) . ? C55 C56 1.392(4) . ? C56 C57 1.384(4) . ? C56 H56 0.9500 . ? C57 C58 1.395(5) . ? C57 H57 0.9500 . ? C58 C59 1.380(5) . ? C58 H58 0.9500 . ? C59 C60 1.386(4) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C66 1.391(4) . ? C61 C62 1.407(4) . ? C62 C63 1.379(5) . ? C62 H62 0.9500 . ? C63 C64 1.388(6) . ? C63 H63 0.9500 . ? C64 C65 1.379(5) . ? C64 H64 0.9500 . ? C65 C66 1.391(5) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 O1 1.417(4) . ? C67 C68 1.530(5) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.505(5) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.501(6) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 O1 1.433(4) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 O2 1.428(4) . ? C71 C72 1.511(6) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.509(5) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.475(6) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 O2 1.435(4) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C77 C76 1.529(5) . ? C77 C78 1.543(5) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 O3 1.430(4) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? O3 C75 1.435(4) . ? C75 C76 1.514(5) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? N6 Sn3 2.076(3) 3_756 ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? 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 N2 Sn1 N3 90.97(10) . . ? N2 Sn1 C27 106.24(11) . . ? N3 Sn1 C27 110.11(10) . . ? N2 Sn1 C21 115.73(10) . . ? N3 Sn1 C21 102.13(11) . . ? C27 Sn1 C21 125.79(11) . . ? N1 Sn2 N4 91.13(10) . . ? N1 Sn2 C33 108.15(11) . . ? N4 Sn2 C33 116.09(10) . . ? N1 Sn2 C39 114.60(10) . . ? N4 Sn2 C39 107.28(11) . . ? C33 Sn2 C39 116.92(11) . . ? N6 Sn3 N5 90.91(10) 3_756 . ? N6 Sn3 C61 113.15(11) 3_756 . ? N5 Sn3 C61 106.12(11) . . ? N6 Sn3 C55 108.01(11) 3_756 . ? N5 Sn3 C55 118.51(10) . . ? C61 Sn3 C55 117.27(12) . . ? N1 B1 N2 123.6(3) . . ? N1 B1 B2 117.6(3) . . ? N2 B1 B2 118.8(3) . . ? N3 B2 N4 124.1(3) . . ? N3 B2 B1 117.7(3) . . ? N4 B2 B1 118.0(3) . . ? N6 B3 N5 124.3(3) . . ? N6 B3 B3 117.7(4) . 3_756 ? N5 B3 B3 118.0(4) . 3_756 ? C2 C1 N1 122.5(3) . . ? C2 C1 C10 120.3(3) . . ? N1 C1 C10 117.2(3) . . ? C1 C2 C3 120.9(3) . . ? C1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C4 C3 C2 120.5(3) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.9(3) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 121.8(3) . . ? C6 C5 C10 118.9(3) . . ? C4 C5 C10 119.3(3) . . ? C7 C6 C5 121.1(3) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 120.9(3) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C9 C8 C7 120.3(3) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 N2 121.7(3) . . ? C8 C9 C10 120.1(3) . . ? N2 C9 C10 118.2(3) . . ? C5 C10 C9 118.7(3) . . ? C5 C10 C1 118.0(3) . . ? C9 C10 C1 123.3(3) . . ? C12 C11 N3 122.3(3) . . ? C12 C11 C20 119.8(3) . . ? N3 C11 C20 117.8(3) . . ? C11 C12 C13 120.5(3) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 121.7(3) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 120.2(3) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 121.8(3) . . ? C16 C15 C20 118.6(3) . . ? C14 C15 C20 119.6(3) . . ? C17 C16 C15 121.6(3) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C16 C17 C18 120.7(3) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 120.5(3) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 N4 122.5(3) . . ? C18 C19 C20 119.6(3) . . ? N4 C19 C20 117.9(3) . . ? C15 C20 C19 119.0(3) . . ? C15 C20 C11 118.1(3) . . ? C19 C20 C11 122.8(3) . . ? C26 C21 C22 118.4(3) . . ? C26 C21 Sn1 123.7(2) . . ? C22 C21 Sn1 117.9(2) . . ? C23 C22 C21 121.1(3) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C22 C23 C24 119.8(3) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C23 C24 C25 119.5(3) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C26 C25 C24 120.4(3) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C21 120.7(3) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? C28 C27 C32 119.2(3) . . ? C28 C27 Sn1 123.6(2) . . ? C32 C27 Sn1 117.3(2) . . ? C29 C28 C27 119.9(3) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C30 C29 C28 120.3(3) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C31 120.4(3) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C30 C31 C32 119.6(3) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C31 C32 C27 120.6(3) . . ? C31 C32 H32 119.7 . . ? C27 C32 H32 119.7 . . ? C38 C33 C34 118.6(3) . . ? C38 C33 Sn2 121.1(2) . . ? C34 C33 Sn2 120.2(2) . . ? C35 C34 C33 120.7(3) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C36 C35 C34 119.7(3) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C37 C36 C35 120.5(3) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 C38 119.6(3) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C37 C38 C33 120.9(3) . . ? C37 C38 H38 119.6 . . ? C33 C38 H38 119.6 . . ? C44 C39 C40 119.5(3) . . ? C44 C39 Sn2 118.9(2) . . ? C40 C39 Sn2 121.6(2) . . ? C39 C40 C41 120.4(3) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C42 C41 C40 119.6(3) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C41 C42 C43 120.5(3) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C42 C43 C44 119.9(3) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C39 C44 C43 120.1(3) . . ? C39 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C46 C45 N5 122.7(3) . . ? C46 C45 C54 119.5(3) . . ? N5 C45 C54 117.8(3) . . ? C45 C46 C47 120.8(3) . . ? C45 C46 H46 119.6 . . ? C47 C46 H46 119.6 . . ? C48 C47 C46 120.9(3) . . ? C48 C47 H47 119.5 . . ? C46 C47 H47 119.5 . . ? C47 C48 C49 120.9(3) . . ? C47 C48 H48 119.5 . . ? C49 C48 H48 119.5 . . ? C48 C49 C50 121.5(3) . . ? C48 C49 C54 119.0(3) . . ? C50 C49 C54 119.5(3) . . ? C51 C50 C49 120.5(3) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C50 C51 C52 121.1(3) . . ? C50 C51 H51 119.4 . . ? C52 C51 H51 119.4 . . ? C53 C52 C51 120.4(3) . . ? C53 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C52 C53 N6 122.1(3) . . ? C52 C53 C54 120.3(3) . . ? N6 C53 C54 117.6(3) . . ? C49 C54 C53 118.2(3) . . ? C49 C54 C45 118.9(3) . . ? C53 C54 C45 123.0(3) . . ? C60 C55 C56 118.9(3) . . ? C60 C55 Sn3 120.2(2) . . ? C56 C55 Sn3 120.7(2) . . ? C57 C56 C55 120.8(3) . . ? C57 C56 H56 119.6 . . ? C55 C56 H56 119.6 . . ? C56 C57 C58 119.5(3) . . ? C56 C57 H57 120.2 . . ? C58 C57 H57 120.2 . . ? C59 C58 C57 120.1(3) . . ? C59 C58 H58 119.9 . . ? C57 C58 H58 119.9 . . ? C58 C59 C60 120.1(3) . . ? C58 C59 H59 120.0 . . ? C60 C59 H59 120.0 . . ? C59 C60 C55 120.5(3) . . ? C59 C60 H60 119.7 . . ? C55 C60 H60 119.7 . . ? C66 C61 C62 118.6(3) . . ? C66 C61 Sn3 122.7(2) . . ? C62 C61 Sn3 118.7(2) . . ? C63 C62 C61 120.6(3) . . ? C63 C62 H62 119.7 . . ? C61 C62 H62 119.7 . . ? C62 C63 C64 119.8(3) . . ? C62 C63 H63 120.1 . . ? C64 C63 H63 120.1 . . ? C65 C64 C63 120.4(3) . . ? C65 C64 H64 119.8 . . ? C63 C64 H64 119.8 . . ? C64 C65 C66 120.0(3) . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C65 C66 C61 120.5(3) . . ? C65 C66 H66 119.7 . . ? C61 C66 H66 119.7 . . ? O1 C67 C68 106.4(3) . . ? O1 C67 H67A 110.4 . . ? C68 C67 H67A 110.4 . . ? O1 C67 H67B 110.4 . . ? C68 C67 H67B 110.4 . . ? H67A C67 H67B 108.6 . . ? C69 C68 C67 102.3(3) . . ? C69 C68 H68A 111.3 . . ? C67 C68 H68A 111.3 . . ? C69 C68 H68B 111.3 . . ? C67 C68 H68B 111.3 . . ? H68A C68 H68B 109.2 . . ? C70 C69 C68 102.0(3) . . ? C70 C69 H69A 111.4 . . ? C68 C69 H69A 111.4 . . ? C70 C69 H69B 111.4 . . ? C68 C69 H69B 111.4 . . ? H69A C69 H69B 109.2 . . ? O1 C70 C69 106.2(3) . . ? O1 C70 H70A 110.5 . . ? C69 C70 H70A 110.5 . . ? O1 C70 H70B 110.5 . . ? C69 C70 H70B 110.5 . . ? H70A C70 H70B 108.7 . . ? O2 C71 C72 106.5(3) . . ? O2 C71 H71A 110.4 . . ? C72 C71 H71A 110.4 . . ? O2 C71 H71B 110.4 . . ? C72 C71 H71B 110.4 . . ? H71A C71 H71B 108.6 . . ? C73 C72 C71 103.1(3) . . ? C73 C72 H72A 111.1 . . ? C71 C72 H72A 111.1 . . ? C73 C72 H72B 111.1 . . ? C71 C72 H72B 111.1 . . ? H72A C72 H72B 109.1 . . ? C74 C73 C72 102.2(3) . . ? C74 C73 H73A 111.3 . . ? C72 C73 H73A 111.3 . . ? C74 C73 H73B 111.3 . . ? C72 C73 H73B 111.3 . . ? H73A C73 H73B 109.2 . . ? O2 C74 C73 107.3(3) . . ? O2 C74 H74A 110.3 . . ? C73 C74 H74A 110.3 . . ? O2 C74 H74B 110.3 . . ? C73 C74 H74B 110.3 . . ? H74A C74 H74B 108.5 . . ? C76 C77 C78 103.6(3) . . ? C76 C77 H77A 111.0 . . ? C78 C77 H77A 111.0 . . ? C76 C77 H77B 111.0 . . ? C78 C77 H77B 111.0 . . ? H77A C77 H77B 109.0 . . ? O3 C78 C77 106.9(3) . . ? O3 C78 H78A 110.3 . . ? C77 C78 H78A 110.3 . . ? O3 C78 H78B 110.3 . . ? C77 C78 H78B 110.3 . . ? H78A C78 H78B 108.6 . . ? C78 O3 C75 105.7(3) . . ? O3 C75 C76 103.8(3) . . ? O3 C75 H75A 111.0 . . ? C76 C75 H75A 111.0 . . ? O3 C75 H75B 111.0 . . ? C76 C75 H75B 111.0 . . ? H75A C75 H75B 109.0 . . ? C1 N1 B1 119.5(3) . . ? C1 N1 Sn2 133.1(2) . . ? B1 N1 Sn2 106.9(2) . . ? C9 N2 B1 118.1(3) . . ? C9 N2 Sn1 136.1(2) . . ? B1 N2 Sn1 105.78(19) . . ? C11 N3 B2 118.7(3) . . ? C11 N3 Sn1 134.3(2) . . ? B2 N3 Sn1 106.7(2) . . ? C19 N4 B2 118.6(3) . . ? C19 N4 Sn2 134.8(2) . . ? B2 N4 Sn2 106.37(19) . . ? C45 N5 B3 118.5(3) . . ? C45 N5 Sn3 135.1(2) . . ? B3 N5 Sn3 106.3(2) . . ? C53 N6 B3 118.9(3) . . ? C53 N6 Sn3 134.1(2) . 3_756 ? B3 N6 Sn3 107.0(2) . 3_756 ? C67 O1 C70 109.5(3) . . ? C71 O2 C74 108.7(3) . . ? C75 C76 C77 102.1(3) . . ? C75 C76 H76A 111.3 . . ? C77 C76 H76A 111.3 . . ? C75 C76 H76B 111.3 . . ? C77 C76 H76B 111.3 . . ? H76A C76 H76B 109.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 B1 B2 N3 -177.2(3) . . . . ? N2 B1 B2 N3 -0.1(4) . . . . ? N1 B1 B2 N4 -1.1(4) . . . . ? N2 B1 B2 N4 176.0(3) . . . . ? N1 C1 C2 C3 179.1(3) . . . . ? C10 C1 C2 C3 -0.4(4) . . . . ? C1 C2 C3 C4 1.0(5) . . . . ? C2 C3 C4 C5 -0.3(5) . . . . ? C3 C4 C5 C6 179.0(3) . . . . ? C3 C4 C5 C10 -1.0(5) . . . . ? C4 C5 C6 C7 -178.6(3) . . . . ? C10 C5 C6 C7 1.4(5) . . . . ? C5 C6 C7 C8 -1.9(5) . . . . ? C6 C7 C8 C9 -0.2(5) . . . . ? C7 C8 C9 N2 -177.4(3) . . . . ? C7 C8 C9 C10 2.8(4) . . . . ? C6 C5 C10 C9 1.1(4) . . . . ? C4 C5 C10 C9 -178.9(3) . . . . ? C6 C5 C10 C1 -178.4(3) . . . . ? C4 C5 C10 C1 1.6(4) . . . . ? C8 C9 C10 C5 -3.2(4) . . . . ? N2 C9 C10 C5 177.0(3) . . . . ? C8 C9 C10 C1 176.3(3) . . . . ? N2 C9 C10 C1 -3.5(4) . . . . ? C2 C1 C10 C5 -0.9(4) . . . . ? N1 C1 C10 C5 179.6(3) . . . . ? C2 C1 C10 C9 179.6(3) . . . . ? N1 C1 C10 C9 0.1(4) . . . . ? N3 C11 C12 C13 -178.7(3) . . . . ? C20 C11 C12 C13 0.8(5) . . . . ? C11 C12 C13 C14 -0.9(5) . . . . ? C12 C13 C14 C15 0.0(5) . . . . ? C13 C14 C15 C16 -177.7(3) . . . . ? C13 C14 C15 C20 1.0(5) . . . . ? C14 C15 C16 C17 178.0(3) . . . . ? C20 C15 C16 C17 -0.8(5) . . . . ? C15 C16 C17 C18 1.8(5) . . . . ? C16 C17 C18 C19 -1.1(5) . . . . ? C17 C18 C19 N4 179.8(3) . . . . ? C17 C18 C19 C20 -0.5(4) . . . . ? C16 C15 C20 C19 -0.8(4) . . . . ? C14 C15 C20 C19 -179.6(3) . . . . ? C16 C15 C20 C11 177.7(3) . . . . ? C14 C15 C20 C11 -1.1(4) . . . . ? C18 C19 C20 C15 1.4(4) . . . . ? N4 C19 C20 C15 -178.8(3) . . . . ? C18 C19 C20 C11 -177.0(3) . . . . ? N4 C19 C20 C11 2.7(4) . . . . ? C12 C11 C20 C15 0.2(4) . . . . ? N3 C11 C20 C15 179.7(3) . . . . ? C12 C11 C20 C19 178.6(3) . . . . ? N3 C11 C20 C19 -1.8(4) . . . . ? N2 Sn1 C21 C26 -119.9(2) . . . . ? N3 Sn1 C21 C26 143.0(2) . . . . ? C27 Sn1 C21 C26 17.0(3) . . . . ? N2 Sn1 C21 C22 61.6(3) . . . . ? N3 Sn1 C21 C22 -35.5(2) . . . . ? C27 Sn1 C21 C22 -161.5(2) . . . . ? C26 C21 C22 C23 2.0(5) . . . . ? Sn1 C21 C22 C23 -179.4(2) . . . . ? C21 C22 C23 C24 -1.1(5) . . . . ? C22 C23 C24 C25 -0.7(5) . . . . ? C23 C24 C25 C26 1.6(5) . . . . ? C24 C25 C26 C21 -0.7(5) . . . . ? C22 C21 C26 C25 -1.1(5) . . . . ? Sn1 C21 C26 C25 -179.6(2) . . . . ? N2 Sn1 C27 C28 -176.7(2) . . . . ? N3 Sn1 C27 C28 -79.5(3) . . . . ? C21 Sn1 C27 C28 43.2(3) . . . . ? N2 Sn1 C27 C32 2.4(2) . . . . ? N3 Sn1 C27 C32 99.6(2) . . . . ? C21 Sn1 C27 C32 -137.7(2) . . . . ? C32 C27 C28 C29 0.3(4) . . . . ? Sn1 C27 C28 C29 179.4(2) . . . . ? C27 C28 C29 C30 -0.2(5) . . . . ? C28 C29 C30 C31 -0.3(5) . . . . ? C29 C30 C31 C32 0.7(5) . . . . ? C30 C31 C32 C27 -0.6(4) . . . . ? C28 C27 C32 C31 0.1(4) . . . . ? Sn1 C27 C32 C31 -179.0(2) . . . . ? N1 Sn2 C33 C38 -149.5(2) . . . . ? N4 Sn2 C33 C38 109.9(2) . . . . ? C39 Sn2 C33 C38 -18.4(3) . . . . ? N1 Sn2 C33 C34 29.9(3) . . . . ? N4 Sn2 C33 C34 -70.7(3) . . . . ? C39 Sn2 C33 C34 161.0(2) . . . . ? C38 C33 C34 C35 -0.9(5) . . . . ? Sn2 C33 C34 C35 179.6(3) . . . . ? C33 C34 C35 C36 0.4(5) . . . . ? C34 C35 C36 C37 0.6(6) . . . . ? C35 C36 C37 C38 -1.2(5) . . . . ? C36 C37 C38 C33 0.7(5) . . . . ? C34 C33 C38 C37 0.4(5) . . . . ? Sn2 C33 C38 C37 179.8(2) . . . . ? N1 Sn2 C39 C44 -94.3(2) . . . . ? N4 Sn2 C39 C44 5.2(3) . . . . ? C33 Sn2 C39 C44 137.6(2) . . . . ? N1 Sn2 C39 C40 86.5(3) . . . . ? N4 Sn2 C39 C40 -174.0(2) . . . . ? C33 Sn2 C39 C40 -41.5(3) . . . . ? C44 C39 C40 C41 -0.2(5) . . . . ? Sn2 C39 C40 C41 179.0(2) . . . . ? C39 C40 C41 C42 -0.4(5) . . . . ? C40 C41 C42 C43 0.7(5) . . . . ? C41 C42 C43 C44 -0.4(5) . . . . ? C40 C39 C44 C43 0.5(4) . . . . ? Sn2 C39 C44 C43 -178.7(2) . . . . ? C42 C43 C44 C39 -0.2(5) . . . . ? N5 C45 C46 C47 179.2(3) . . . . ? C54 C45 C46 C47 -1.5(4) . . . . ? C45 C46 C47 C48 0.2(5) . . . . ? C46 C47 C48 C49 1.1(5) . . . . ? C47 C48 C49 C50 177.7(3) . . . . ? C47 C48 C49 C54 -1.0(5) . . . . ? C48 C49 C50 C51 -178.3(3) . . . . ? C54 C49 C50 C51 0.4(5) . . . . ? C49 C50 C51 C52 -1.3(5) . . . . ? C50 C51 C52 C53 1.1(5) . . . . ? C51 C52 C53 N6 179.1(3) . . . . ? C51 C52 C53 C54 0.0(4) . . . . ? C48 C49 C54 C53 179.4(3) . . . . ? C50 C49 C54 C53 0.6(4) . . . . ? C48 C49 C54 C45 -0.2(4) . . . . ? C50 C49 C54 C45 -179.0(3) . . . . ? C52 C53 C54 C49 -0.8(4) . . . . ? N6 C53 C54 C49 -180.0(3) . . . . ? C52 C53 C54 C45 178.8(3) . . . . ? N6 C53 C54 C45 -0.4(4) . . . . ? C46 C45 C54 C49 1.4(4) . . . . ? N5 C45 C54 C49 -179.2(3) . . . . ? C46 C45 C54 C53 -178.1(3) . . . . ? N5 C45 C54 C53 1.3(4) . . . . ? N6 Sn3 C55 C60 -156.8(2) 3_756 . . . ? N5 Sn3 C55 C60 101.9(2) . . . . ? C61 Sn3 C55 C60 -27.6(3) . . . . ? N6 Sn3 C55 C56 19.9(3) 3_756 . . . ? N5 Sn3 C55 C56 -81.4(3) . . . . ? C61 Sn3 C55 C56 149.1(2) . . . . ? C60 C55 C56 C57 -1.7(5) . . . . ? Sn3 C55 C56 C57 -178.5(3) . . . . ? C55 C56 C57 C58 0.8(5) . . . . ? C56 C57 C58 C59 0.7(5) . . . . ? C57 C58 C59 C60 -1.2(5) . . . . ? C58 C59 C60 C55 0.2(5) . . . . ? C56 C55 C60 C59 1.2(5) . . . . ? Sn3 C55 C60 C59 178.0(2) . . . . ? N6 Sn3 C61 C66 92.3(3) 3_756 . . . ? N5 Sn3 C61 C66 -169.5(2) . . . . ? C55 Sn3 C61 C66 -34.5(3) . . . . ? N6 Sn3 C61 C62 -88.3(3) 3_756 . . . ? N5 Sn3 C61 C62 9.9(3) . . . . ? C55 Sn3 C61 C62 144.9(2) . . . . ? C66 C61 C62 C63 0.2(5) . . . . ? Sn3 C61 C62 C63 -179.2(3) . . . . ? C61 C62 C63 C64 0.5(5) . . . . ? C62 C63 C64 C65 -0.9(6) . . . . ? C63 C64 C65 C66 0.6(6) . . . . ? C64 C65 C66 C61 0.1(5) . . . . ? C62 C61 C66 C65 -0.5(5) . . . . ? Sn3 C61 C66 C65 178.9(3) . . . . ? O1 C67 C68 C69 26.5(4) . . . . ? C67 C68 C69 C70 -35.6(4) . . . . ? C68 C69 C70 O1 33.4(4) . . . . ? O2 C71 C72 C73 25.1(5) . . . . ? C71 C72 C73 C74 -34.1(5) . . . . ? C72 C73 C74 O2 31.9(5) . . . . ? C76 C77 C78 O3 2.1(4) . . . . ? C77 C78 O3 C75 -27.4(4) . . . . ? C78 O3 C75 C76 42.4(3) . . . . ? C2 C1 N1 B1 -176.9(3) . . . . ? C10 C1 N1 B1 2.6(4) . . . . ? C2 C1 N1 Sn2 -6.1(4) . . . . ? C10 C1 N1 Sn2 173.4(2) . . . . ? N2 B1 N1 C1 -2.0(5) . . . . ? B2 B1 N1 C1 175.0(3) . . . . ? N2 B1 N1 Sn2 -174.9(2) . . . . ? B2 B1 N1 Sn2 2.0(3) . . . . ? N4 Sn2 N1 C1 -173.5(3) . . . . ? C33 Sn2 N1 C1 68.5(3) . . . . ? C39 Sn2 N1 C1 -63.9(3) . . . . ? N4 Sn2 N1 B1 -1.9(2) . . . . ? C33 Sn2 N1 B1 -119.9(2) . . . . ? C39 Sn2 N1 B1 107.7(2) . . . . ? C8 C9 N2 B1 -175.7(3) . . . . ? C10 C9 N2 B1 4.1(4) . . . . ? C8 C9 N2 Sn1 7.4(4) . . . . ? C10 C9 N2 Sn1 -172.8(2) . . . . ? N1 B1 N2 C9 -1.6(4) . . . . ? B2 B1 N2 C9 -178.5(3) . . . . ? N1 B1 N2 Sn1 176.2(3) . . . . ? B2 B1 N2 Sn1 -0.7(3) . . . . ? N3 Sn1 N2 C9 178.1(3) . . . . ? C27 Sn1 N2 C9 -70.6(3) . . . . ? C21 Sn1 N2 C9 74.1(3) . . . . ? N3 Sn1 N2 B1 0.9(2) . . . . ? C27 Sn1 N2 B1 112.2(2) . . . . ? C21 Sn1 N2 B1 -103.1(2) . . . . ? C12 C11 N3 B2 179.8(3) . . . . ? C20 C11 N3 B2 0.3(4) . . . . ? C12 C11 N3 Sn1 -6.5(4) . . . . ? C20 C11 N3 Sn1 174.0(2) . . . . ? N4 B2 N3 C11 0.3(4) . . . . ? B1 B2 N3 C11 176.1(3) . . . . ? N4 B2 N3 Sn1 -175.0(2) . . . . ? B1 B2 N3 Sn1 0.8(3) . . . . ? N2 Sn1 N3 C11 -175.2(3) . . . . ? C27 Sn1 N3 C11 77.1(3) . . . . ? C21 Sn1 N3 C11 -58.6(3) . . . . ? N2 Sn1 N3 B2 -1.0(2) . . . . ? C27 Sn1 N3 B2 -108.7(2) . . . . ? C21 Sn1 N3 B2 115.6(2) . . . . ? C18 C19 N4 B2 177.6(3) . . . . ? C20 C19 N4 B2 -2.1(4) . . . . ? C18 C19 N4 Sn2 4.9(4) . . . . ? C20 C19 N4 Sn2 -174.8(2) . . . . ? N3 B2 N4 C19 0.7(4) . . . . ? B1 B2 N4 C19 -175.2(3) . . . . ? N3 B2 N4 Sn2 175.3(2) . . . . ? B1 B2 N4 Sn2 -0.6(3) . . . . ? N1 Sn2 N4 C19 174.7(3) . . . . ? C33 Sn2 N4 C19 -74.4(3) . . . . ? C39 Sn2 N4 C19 58.4(3) . . . . ? N1 Sn2 N4 B2 1.3(2) . . . . ? C33 Sn2 N4 B2 112.2(2) . . . . ? C39 Sn2 N4 B2 -114.9(2) . . . . ? C46 C45 N5 B3 178.1(3) . . . . ? C54 C45 N5 B3 -1.2(4) . . . . ? C46 C45 N5 Sn3 2.1(4) . . . . ? C54 C45 N5 Sn3 -177.3(2) . . . . ? N6 B3 N5 C45 0.5(4) . . . . ? B3 B3 N5 C45 -178.6(3) 3_756 . . . ? N6 B3 N5 Sn3 177.6(3) . . . . ? B3 B3 N5 Sn3 -1.5(4) 3_756 . . . ? N6 Sn3 N5 C45 178.8(3) 3_756 . . . ? C61 Sn3 N5 C45 64.3(3) . . . . ? C55 Sn3 N5 C45 -70.1(3) . . . . ? N6 Sn3 N5 B3 2.4(2) 3_756 . . . ? C61 Sn3 N5 B3 -112.0(2) . . . . ? C55 Sn3 N5 B3 113.6(2) . . . . ? C52 C53 N6 B3 -179.5(3) . . . . ? C54 C53 N6 B3 -0.4(4) . . . . ? C52 C53 N6 Sn3 3.3(4) . . . 3_756 ? C54 C53 N6 Sn3 -177.5(2) . . . 3_756 ? N5 B3 N6 C53 0.4(5) . . . . ? B3 B3 N6 C53 179.4(3) 3_756 . . . ? N5 B3 N6 Sn3 178.2(2) . . . 3_756 ? B3 B3 N6 Sn3 -2.7(4) 3_756 . . 3_756 ? C68 C67 O1 C70 -6.0(4) . . . . ? C69 C70 O1 C67 -17.3(4) . . . . ? C72 C71 O2 C74 -5.7(4) . . . . ? C73 C74 O2 C71 -16.7(5) . . . . ? O3 C75 C76 C77 -39.6(3) . . . . ? C78 C77 C76 C75 22.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 29.66 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.973 _refine_diff_density_min -1.216 _refine_diff_density_rms 0.113