# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr Roland Roesler' _publ_contact_author_address ; Chemistry University of Calgary 2500 University Drive NW Calgary Alberta T2N 1N4 CANADA ; _publ_contact_author_email ROESLER@UCALGARY.CA _publ_section_title ; -n3:n4-Lithiocene and n3:n3-Zincocene Incorporating 1,2-Diaza-3,5-diborolyl, a Cyclopentadienyl Analog ; loop_ _publ_author_name 'Roland Roesler' 'Taryn D. Forster' 'Hanh V. Ly' 'Darren Maley' 'Masood Parvez' data_r8 _database_code_depnum_ccdc_archive 'CCDC 266130' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H23 B2 Li N2' _chemical_formula_weight 199.86 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.573(5) _cell_length_b 9.925(6) _cell_length_c 14.892(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1267.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 0.058 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9885 _exptl_absorpt_correction_T_max 0.9977 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2153 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 7.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1266 _reflns_number_gt 1049 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.5000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -2(4) _refine_ls_number_reflns 1266 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 N1 N 0.3191(3) 0.2229(2) 0.60689(14) 0.0266(5) Uani 1 1 d . . . N2 N 0.3047(3) 0.1101(2) 0.54381(15) 0.0261(5) Uani 1 1 d . . . C1 C 0.2673(3) 0.3138(3) 0.46034(19) 0.0270(6) Uani 1 1 d . . . C2 C 0.2480(4) 0.4115(3) 0.3826(2) 0.0350(7) Uani 1 1 d . . . H2A H 0.3067 0.4941 0.3951 0.042 Uiso 0.50 1 calc PR . . H2B H 0.1373 0.4334 0.3752 0.042 Uiso 0.50 1 calc PR . . H2C H 0.2875 0.3700 0.3274 0.042 Uiso 0.50 1 calc PR . . H2D H 0.1809 0.3709 0.3367 0.042 Uiso 0.50 1 calc PR . . H2E H 0.3504 0.4316 0.3566 0.042 Uiso 0.50 1 calc PR . . H2F H 0.2002 0.4950 0.4044 0.042 Uiso 0.50 1 calc PR . . C3 C 0.2566(4) 0.0698(3) 0.36720(19) 0.0384(8) Uani 1 1 d . . . H3A H 0.3577 0.0288 0.3533 0.046 Uiso 1 1 calc R . . H3B H 0.2225 0.1252 0.3164 0.046 Uiso 1 1 calc R . . H3C H 0.1795 -0.0012 0.3783 0.046 Uiso 1 1 calc R . . C4 C 0.2966(4) 0.4947(3) 0.6025(2) 0.0383(8) Uani 1 1 d . . . H4A H 0.2912 0.5641 0.5558 0.046 Uiso 1 1 calc R . . H4B H 0.3945 0.5042 0.6359 0.046 Uiso 1 1 calc R . . H4C H 0.2083 0.5053 0.6437 0.046 Uiso 1 1 calc R . . C5 C 0.2810(3) 0.1998(3) 0.70265(17) 0.0293(7) Uani 1 1 d . . . H5 H 0.2873 0.1006 0.7139 0.035 Uiso 1 1 calc R . . C6 C 0.1151(3) 0.2446(4) 0.7248(2) 0.0448(8) Uani 1 1 d . . . H6A H 0.0858 0.2106 0.7842 0.054 Uiso 1 1 calc R . . H6B H 0.0430 0.2087 0.6796 0.054 Uiso 1 1 calc R . . H6C H 0.1098 0.3432 0.7247 0.054 Uiso 1 1 calc R . . C7 C 0.3995(4) 0.2677(4) 0.76335(19) 0.0435(8) Uani 1 1 d . . . H7A H 0.3698 0.2540 0.8262 0.052 Uiso 1 1 calc R . . H7B H 0.4025 0.3645 0.7502 0.052 Uiso 1 1 calc R . . H7C H 0.5028 0.2285 0.7528 0.052 Uiso 1 1 calc R . . C8 C 0.3176(4) -0.0297(3) 0.57842(19) 0.0297(7) Uani 1 1 d . . . H8 H 0.3773 -0.0257 0.6360 0.036 Uiso 1 1 calc R . . C9 C 0.1589(4) -0.0891(3) 0.5994(2) 0.0443(8) Uani 1 1 d . . . H9A H 0.1720 -0.1786 0.6261 0.053 Uiso 1 1 calc R . . H9B H 0.0981 -0.0967 0.5439 0.053 Uiso 1 1 calc R . . H9C H 0.1039 -0.0304 0.6418 0.053 Uiso 1 1 calc R . . C10 C 0.4085(4) -0.1196(3) 0.5146(2) 0.0384(7) Uani 1 1 d . . . H10A H 0.4334 -0.2048 0.5445 0.046 Uiso 1 1 calc R . . H10B H 0.5054 -0.0743 0.4969 0.046 Uiso 1 1 calc R . . H10C H 0.3454 -0.1375 0.4610 0.046 Uiso 1 1 calc R . . B1 B 0.2727(4) 0.1617(3) 0.4541(2) 0.0278(7) Uani 1 1 d . . . B2 B 0.2898(4) 0.3494(3) 0.5572(2) 0.0278(7) Uani 1 1 d . . . Li1 Li 0.5124(6) 0.2203(5) 0.5231(3) 0.0363(11) 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 N1 0.0334(12) 0.0229(11) 0.0236(10) -0.0023(10) -0.0012(10) -0.0006(10) N2 0.0281(13) 0.0224(11) 0.0280(11) -0.0043(10) -0.0026(10) 0.0012(10) C1 0.0201(14) 0.0326(14) 0.0284(13) 0.0041(12) 0.0032(12) 0.0007(11) C2 0.0288(16) 0.0393(16) 0.0368(16) 0.0080(14) 0.0013(13) 0.0057(15) C3 0.0462(18) 0.0386(16) 0.0304(16) -0.0045(14) -0.0038(14) 0.0031(16) C4 0.0447(19) 0.0269(14) 0.0434(17) -0.0033(14) -0.0066(16) 0.0013(14) C5 0.0344(15) 0.0312(15) 0.0223(13) 0.0005(12) 0.0017(11) -0.0010(13) C6 0.0416(17) 0.052(2) 0.0410(16) 0.0101(18) 0.0131(13) 0.0079(17) C7 0.0515(18) 0.0494(19) 0.0298(14) -0.0033(16) -0.0075(14) -0.0058(17) C8 0.0352(17) 0.0211(13) 0.0327(15) 0.0037(12) -0.0020(13) -0.0001(12) C9 0.0460(19) 0.0380(16) 0.0489(18) 0.0022(16) 0.0047(16) -0.0139(16) C10 0.0456(17) 0.0255(14) 0.0442(18) -0.0022(14) -0.0009(14) 0.0036(13) B1 0.0251(16) 0.0322(16) 0.0260(15) -0.0019(14) -0.0012(13) 0.0013(14) B2 0.0206(16) 0.0273(15) 0.0355(17) 0.0008(15) 0.0013(13) -0.0006(13) Li1 0.033(2) 0.036(3) 0.040(3) 0.002(2) 0.000(2) -0.001(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 N1 N2 1.466(3) . ? N1 B2 1.479(4) . ? N1 C5 1.481(3) . ? N1 Li1 2.075(5) . ? N2 B1 1.457(4) . ? N2 C8 1.485(3) . ? N2 Li1 2.112(5) . ? C1 B2 1.498(4) . ? C1 B1 1.513(4) . ? C1 C2 1.519(4) . ? C1 Li1 2.225(6) 3_456 ? C1 Li1 2.479(6) . ? C2 Li1 2.786(6) 3_456 ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C2 H2D 0.9800 . ? C2 H2E 0.9800 . ? C2 H2F 0.9800 . ? C3 B1 1.589(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 B2 1.593(4) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C7 1.518(4) . ? C5 C6 1.526(4) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.516(4) . ? C8 C10 1.519(4) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? B1 Li1 2.369(6) . ? B1 Li1 2.544(6) 3_456 ? B2 Li1 2.354(6) . ? B2 Li1 2.751(6) 3_456 ? Li1 C1 2.225(6) 3_556 ? Li1 B1 2.543(6) 3_556 ? Li1 B2 2.751(6) 3_556 ? Li1 C2 2.786(6) 3_556 ? 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 N1 B2 108.28(19) . . ? N2 N1 C5 118.7(2) . . ? B2 N1 C5 125.1(2) . . ? N2 N1 Li1 70.86(18) . . ? B2 N1 Li1 81.1(2) . . ? C5 N1 Li1 138.9(2) . . ? B1 N2 N1 109.6(2) . . ? B1 N2 C8 131.4(2) . . ? N1 N2 C8 119.0(2) . . ? B1 N2 Li1 81.0(2) . . ? N1 N2 Li1 68.15(19) . . ? C8 N2 Li1 118.2(2) . . ? B2 C1 B1 106.9(3) . . ? B2 C1 C2 126.6(3) . . ? B1 C1 C2 126.4(3) . . ? B2 C1 Li1 93.2(2) . 3_456 ? B1 C1 Li1 83.4(2) . 3_456 ? C2 C1 Li1 94.3(2) . 3_456 ? B2 C1 Li1 67.5(2) . . ? B1 C1 Li1 67.9(2) . . ? C2 C1 Li1 128.2(2) . . ? Li1 C1 Li1 137.19(13) 3_456 . ? C1 C2 Li1 52.80(17) . 3_456 ? C1 C2 H2A 109.5 . . ? Li1 C2 H2A 132.0 3_456 . ? C1 C2 H2B 109.5 . . ? Li1 C2 H2B 57.2 3_456 . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? Li1 C2 H2C 118.4 3_456 . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C2 H2D 109.5 . . ? Li1 C2 H2D 74.5 3_456 . ? H2A C2 H2D 141.1 . . ? H2B C2 H2D 56.3 . . ? H2C C2 H2D 56.3 . . ? C1 C2 H2E 109.5 . . ? Li1 C2 H2E 160.8 3_456 . ? H2A C2 H2E 56.3 . . ? H2B C2 H2E 141.1 . . ? H2C C2 H2E 56.3 . . ? H2D C2 H2E 109.5 . . ? C1 C2 H2F 109.5 . . ? Li1 C2 H2F 85.8 3_456 . ? H2A C2 H2F 56.3 . . ? H2B C2 H2F 56.3 . . ? H2C C2 H2F 141.1 . . ? H2D C2 H2F 109.5 . . ? H2E C2 H2F 109.5 . . ? B1 C3 H3A 109.5 . . ? B1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? B1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? B2 C4 H4A 109.5 . . ? B2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? B2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 C7 110.9(2) . . ? N1 C5 C6 111.6(2) . . ? C7 C5 C6 111.5(2) . . ? N1 C5 H5 107.5 . . ? C7 C5 H5 107.5 . . ? C6 C5 H5 107.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C9 111.6(2) . . ? N2 C8 C10 111.7(2) . . ? C9 C8 C10 111.2(2) . . ? N2 C8 H8 107.4 . . ? C9 C8 H8 107.4 . . ? C10 C8 H8 107.4 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 B1 C1 107.5(3) . . ? N2 B1 C3 124.2(3) . . ? C1 B1 C3 128.3(3) . . ? N2 B1 Li1 61.66(19) . . ? C1 B1 Li1 75.8(2) . . ? C3 B1 Li1 124.7(3) . . ? N2 B1 Li1 101.8(2) . 3_456 ? C1 B1 Li1 60.4(2) . 3_456 ? C3 B1 Li1 107.3(2) . 3_456 ? Li1 B1 Li1 126.16(14) . 3_456 ? N1 B2 C1 107.6(2) . . ? N1 B2 C4 123.4(3) . . ? C1 B2 C4 128.8(3) . . ? N1 B2 Li1 60.53(18) . . ? C1 B2 Li1 76.5(2) . . ? C4 B2 Li1 123.7(3) . . ? N1 B2 Li1 98.7(2) . 3_456 ? C1 B2 Li1 53.89(18) . 3_456 ? C4 B2 Li1 116.3(2) . 3_456 ? Li1 B2 Li1 118.02(13) . 3_456 ? N1 Li1 N2 41.00(13) . . ? N1 Li1 C1 136.0(3) . 3_556 ? N2 Li1 C1 137.1(3) . 3_556 ? N1 Li1 B2 38.37(13) . . ? N2 Li1 B2 64.35(17) . . ? C1 Li1 B2 148.7(3) 3_556 . ? N1 Li1 B1 64.61(17) . . ? N2 Li1 B1 37.38(13) . . ? C1 Li1 B1 149.6(3) 3_556 . ? B2 Li1 B1 61.61(17) . . ? N1 Li1 C1 62.96(16) . . ? N2 Li1 C1 62.26(16) . . ? C1 Li1 C1 158.6(2) 3_556 . ? B2 Li1 C1 36.00(13) . . ? B1 Li1 C1 36.27(12) . . ? N1 Li1 B1 127.9(2) . 3_556 ? N2 Li1 B1 163.5(3) . 3_556 ? C1 Li1 B1 36.22(13) 3_556 3_556 ? B2 Li1 B1 115.6(2) . 3_556 ? B1 Li1 B1 158.7(2) . 3_556 ? C1 Li1 B1 128.4(2) . 3_556 ? N1 Li1 B2 162.8(2) . 3_556 ? N2 Li1 B2 131.5(2) . 3_556 ? C1 Li1 B2 32.95(13) 3_556 3_556 ? B2 Li1 B2 158.7(2) . 3_556 ? B1 Li1 B2 120.0(2) . 3_556 ? C1 Li1 B2 131.5(2) . 3_556 ? B1 Li1 B2 54.21(14) 3_556 3_556 ? N1 Li1 C2 106.3(2) . 3_556 ? N2 Li1 C2 107.1(2) . 3_556 ? C1 Li1 C2 32.94(12) 3_556 3_556 ? B2 Li1 C2 137.2(2) . 3_556 ? B1 Li1 C2 137.0(2) . 3_556 ? C1 Li1 C2 168.5(2) . 3_556 ? B1 Li1 C2 60.84(15) 3_556 3_556 ? B2 Li1 C2 58.29(14) 3_556 3_556 ? 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 B2 N1 N2 B1 2.1(3) . . . . ? C5 N1 N2 B1 152.8(2) . . . . ? Li1 N1 N2 B1 -71.2(2) . . . . ? B2 N1 N2 C8 -175.6(3) . . . . ? C5 N1 N2 C8 -25.0(3) . . . . ? Li1 N1 N2 C8 111.0(3) . . . . ? B2 N1 N2 Li1 73.3(2) . . . . ? C5 N1 N2 Li1 -136.0(3) . . . . ? B2 C1 C2 Li1 -97.1(3) . . . 3_456 ? B1 C1 C2 Li1 85.0(3) . . . 3_456 ? Li1 C1 C2 Li1 174.1(3) . . . 3_456 ? N2 N1 C5 C7 137.6(2) . . . . ? B2 N1 C5 C7 -77.1(3) . . . . ? Li1 N1 C5 C7 44.2(4) . . . . ? N2 N1 C5 C6 -97.4(3) . . . . ? B2 N1 C5 C6 47.9(4) . . . . ? Li1 N1 C5 C6 169.2(3) . . . . ? B1 N2 C8 C9 -82.8(4) . . . . ? N1 N2 C8 C9 94.3(3) . . . . ? Li1 N2 C8 C9 173.6(2) . . . . ? B1 N2 C8 C10 42.3(4) . . . . ? N1 N2 C8 C10 -140.5(2) . . . . ? Li1 N2 C8 C10 -61.2(3) . . . . ? N1 N2 B1 C1 0.3(3) . . . . ? C8 N2 B1 C1 177.7(3) . . . . ? Li1 N2 B1 C1 -62.5(3) . . . . ? N1 N2 B1 C3 177.4(3) . . . . ? C8 N2 B1 C3 -5.2(5) . . . . ? Li1 N2 B1 C3 114.6(3) . . . . ? N1 N2 B1 Li1 62.8(2) . . . . ? C8 N2 B1 Li1 -119.8(3) . . . . ? N1 N2 B1 Li1 -62.1(2) . . . 3_456 ? C8 N2 B1 Li1 115.3(3) . . . 3_456 ? Li1 N2 B1 Li1 -124.89(13) . . . 3_456 ? B2 C1 B1 N2 -2.6(4) . . . . ? C2 C1 B1 N2 175.7(2) . . . . ? Li1 C1 B1 N2 -93.9(3) 3_456 . . . ? Li1 C1 B1 N2 53.6(2) . . . . ? B2 C1 B1 C3 -179.5(3) . . . . ? C2 C1 B1 C3 -1.3(6) . . . . ? Li1 C1 B1 C3 89.2(4) 3_456 . . . ? Li1 C1 B1 C3 -123.3(4) . . . . ? B2 C1 B1 Li1 -56.2(2) . . . . ? C2 C1 B1 Li1 122.0(3) . . . . ? Li1 C1 B1 Li1 -147.55(11) 3_456 . . . ? B2 C1 B1 Li1 91.3(2) . . . 3_456 ? C2 C1 B1 Li1 -90.4(3) . . . 3_456 ? Li1 C1 B1 Li1 147.55(11) . . . 3_456 ? N2 N1 B2 C1 -3.7(3) . . . . ? C5 N1 B2 C1 -152.0(2) . . . . ? Li1 N1 B2 C1 62.6(2) . . . . ? N2 N1 B2 C4 -179.3(3) . . . . ? C5 N1 B2 C4 32.4(4) . . . . ? Li1 N1 B2 C4 -113.0(3) . . . . ? N2 N1 B2 Li1 -66.3(2) . . . . ? C5 N1 B2 Li1 145.4(3) . . . . ? N2 N1 B2 Li1 51.0(2) . . . 3_456 ? C5 N1 B2 Li1 -97.3(3) . . . 3_456 ? Li1 N1 B2 Li1 117.37(12) . . . 3_456 ? B1 C1 B2 N1 3.9(3) . . . . ? C2 C1 B2 N1 -174.4(3) . . . . ? Li1 C1 B2 N1 87.9(3) 3_456 . . . ? Li1 C1 B2 N1 -52.6(2) . . . . ? B1 C1 B2 C4 179.1(3) . . . . ? C2 C1 B2 C4 0.9(5) . . . . ? Li1 C1 B2 C4 -96.8(3) 3_456 . . . ? Li1 C1 B2 C4 122.6(4) . . . . ? B1 C1 B2 Li1 56.5(3) . . . . ? C2 C1 B2 Li1 -121.7(3) . . . . ? Li1 C1 B2 Li1 140.58(12) 3_456 . . . ? B1 C1 B2 Li1 -84.1(3) . . . 3_456 ? C2 C1 B2 Li1 97.7(3) . . . 3_456 ? Li1 C1 B2 Li1 -140.58(12) . . . 3_456 ? B2 N1 Li1 N2 -113.0(2) . . . . ? C5 N1 Li1 N2 112.1(3) . . . . ? N2 N1 Li1 C1 -114.7(4) . . . 3_556 ? B2 N1 Li1 C1 132.4(4) . . . 3_556 ? C5 N1 Li1 C1 -2.6(6) . . . 3_556 ? N2 N1 Li1 B2 113.0(2) . . . . ? C5 N1 Li1 B2 -134.9(4) . . . . ? N2 N1 Li1 B1 37.36(14) . . . . ? B2 N1 Li1 B1 -75.61(18) . . . . ? C5 N1 Li1 B1 149.4(3) . . . . ? N2 N1 Li1 C1 77.92(16) . . . . ? B2 N1 Li1 C1 -35.05(16) . . . . ? C5 N1 Li1 C1 -170.0(3) . . . . ? N2 N1 Li1 B1 -162.9(3) . . . 3_556 ? B2 N1 Li1 B1 84.1(3) . . . 3_556 ? C5 N1 Li1 B1 -50.9(5) . . . 3_556 ? N2 N1 Li1 B2 -72.3(8) . . . 3_556 ? B2 N1 Li1 B2 174.7(8) . . . 3_556 ? C5 N1 Li1 B2 39.7(10) . . . 3_556 ? N2 N1 Li1 C2 -97.5(2) . . . 3_556 ? B2 N1 Li1 C2 149.6(2) . . . 3_556 ? C5 N1 Li1 C2 14.6(4) . . . 3_556 ? B1 N2 Li1 N1 115.4(2) . . . . ? C8 N2 Li1 N1 -112.2(2) . . . . ? B1 N2 Li1 C1 -132.7(4) . . . 3_556 ? N1 N2 Li1 C1 111.9(4) . . . 3_556 ? C8 N2 Li1 C1 -0.3(5) . . . 3_556 ? B1 N2 Li1 B2 76.09(18) . . . . ? N1 N2 Li1 B2 -39.34(14) . . . . ? C8 N2 Li1 B2 -151.5(2) . . . . ? N1 N2 Li1 B1 -115.4(2) . . . . ? C8 N2 Li1 B1 132.4(3) . . . . ? B1 N2 Li1 C1 35.69(16) . . . . ? N1 N2 Li1 C1 -79.74(16) . . . . ? C8 N2 Li1 C1 168.1(2) . . . . ? B1 N2 Li1 B1 169.8(9) . . . 3_556 ? N1 N2 Li1 B1 54.4(9) . . . 3_556 ? C8 N2 Li1 B1 -57.8(10) . . . 3_556 ? B1 N2 Li1 B2 -86.6(3) . . . 3_556 ? N1 N2 Li1 B2 157.9(3) . . . 3_556 ? C8 N2 Li1 B2 45.7(4) . . . 3_556 ? B1 N2 Li1 C2 -149.1(2) . . . 3_556 ? N1 N2 Li1 C2 95.4(2) . . . 3_556 ? C8 N2 Li1 C2 -16.8(3) . . . 3_556 ? C1 B2 Li1 N1 -119.5(2) . . . . ? C4 B2 Li1 N1 112.6(3) . . . . ? Li1 B2 Li1 N1 -83.98(19) 3_456 . . . ? N1 B2 Li1 N2 42.07(15) . . . . ? C1 B2 Li1 N2 -77.44(19) . . . . ? C4 B2 Li1 N2 154.6(3) . . . . ? Li1 B2 Li1 N2 -41.92(13) 3_456 . . . ? N1 B2 Li1 C1 -98.8(5) . . . 3_556 ? C1 B2 Li1 C1 141.7(5) . . . 3_556 ? C4 B2 Li1 C1 13.8(6) . . . 3_556 ? Li1 B2 Li1 C1 177.2(5) 3_456 . . 3_556 ? N1 B2 Li1 B1 84.12(19) . . . . ? C1 B2 Li1 B1 -35.39(17) . . . . ? C4 B2 Li1 B1 -163.3(3) . . . . ? Li1 B2 Li1 B1 0.14(13) 3_456 . . . ? N1 B2 Li1 C1 119.5(2) . . . . ? C4 B2 Li1 C1 -127.9(3) . . . . ? Li1 B2 Li1 C1 35.53(14) 3_456 . . . ? N1 B2 Li1 B1 -119.6(3) . . . 3_556 ? C1 B2 Li1 B1 120.9(3) . . . 3_556 ? C4 B2 Li1 B1 -7.0(4) . . . 3_556 ? Li1 B2 Li1 B1 156.4(3) 3_456 . . 3_556 ? N1 B2 Li1 B2 -175.7(7) . . . 3_556 ? C1 B2 Li1 B2 64.8(6) . . . 3_556 ? C4 B2 Li1 B2 -63.1(7) . . . 3_556 ? Li1 B2 Li1 B2 100.3(7) 3_456 . . 3_556 ? N1 B2 Li1 C2 -45.7(3) . . . 3_556 ? C1 B2 Li1 C2 -165.2(3) . . . 3_556 ? C4 B2 Li1 C2 66.8(4) . . . 3_556 ? Li1 B2 Li1 C2 -129.7(3) 3_456 . . 3_556 ? N2 B1 Li1 N1 -40.98(15) . . . . ? C1 B1 Li1 N1 78.23(19) . . . . ? C3 B1 Li1 N1 -154.7(3) . . . . ? Li1 B1 Li1 N1 42.95(16) 3_456 . . . ? C1 B1 Li1 N2 119.2(3) . . . . ? C3 B1 Li1 N2 -113.8(3) . . . . ? Li1 B1 Li1 N2 83.9(2) 3_456 . . . ? N2 B1 Li1 C1 98.9(5) . . . 3_556 ? C1 B1 Li1 C1 -141.9(5) . . . 3_556 ? C3 B1 Li1 C1 -14.8(6) . . . 3_556 ? Li1 B1 Li1 C1 -177.1(5) 3_456 . . 3_556 ? N2 B1 Li1 B2 -84.09(19) . . . . ? C1 B1 Li1 B2 35.12(18) . . . . ? C3 B1 Li1 B2 162.2(3) . . . . ? Li1 B1 Li1 B2 -0.17(16) 3_456 . . . ? N2 B1 Li1 C1 -119.2(3) . . . . ? C3 B1 Li1 C1 127.0(3) . . . . ? Li1 B1 Li1 C1 -35.29(15) 3_456 . . . ? N2 B1 Li1 B1 -172.0(7) . . . 3_556 ? C1 B1 Li1 B1 -52.8(7) . . . 3_556 ? C3 B1 Li1 B1 74.2(7) . . . 3_556 ? Li1 B1 Li1 B1 -88.1(7) 3_456 . . 3_556 ? N2 B1 Li1 B2 120.3(3) . . . 3_556 ? C1 B1 Li1 B2 -120.5(3) . . . 3_556 ? C3 B1 Li1 B2 6.5(4) . . . 3_556 ? Li1 B1 Li1 B2 -155.8(3) 3_456 . . 3_556 ? N2 B1 Li1 C2 46.0(3) . . . 3_556 ? C1 B1 Li1 C2 165.2(3) . . . 3_556 ? C3 B1 Li1 C2 -67.7(4) . . . 3_556 ? Li1 B1 Li1 C2 129.9(3) 3_456 . . 3_556 ? B2 C1 Li1 N1 37.33(18) . . . . ? B1 C1 Li1 N1 -83.2(2) . . . . ? C2 C1 Li1 N1 157.1(3) . . . . ? Li1 C1 Li1 N1 -31.56(17) 3_456 . . . ? B2 C1 Li1 N2 83.8(2) . . . . ? B1 C1 Li1 N2 -36.78(19) . . . . ? C2 C1 Li1 N2 -156.5(3) . . . . ? Li1 C1 Li1 N2 14.89(16) 3_456 . . . ? B2 C1 Li1 C1 -118.2(7) . . . 3_556 ? B1 C1 Li1 C1 121.2(7) . . . 3_556 ? C2 C1 Li1 C1 1.5(8) . . . 3_556 ? Li1 C1 Li1 C1 172.9(8) 3_456 . . 3_556 ? B1 C1 Li1 B2 -120.6(3) . . . . ? C2 C1 Li1 B2 119.7(3) . . . . ? Li1 C1 Li1 B2 -68.9(2) 3_456 . . . ? B2 C1 Li1 B1 120.6(3) . . . . ? C2 C1 Li1 B1 -119.7(3) . . . . ? Li1 C1 Li1 B1 51.7(2) 3_456 . . . ? B2 C1 Li1 B1 -81.1(3) . . . 3_556 ? B1 C1 Li1 B1 158.3(3) . . . 3_556 ? C2 C1 Li1 B1 38.6(4) . . . 3_556 ? Li1 C1 Li1 B1 -150.0(3) 3_456 . . 3_556 ? B2 C1 Li1 B2 -154.0(3) . . . 3_556 ? B1 C1 Li1 B2 85.5(3) . . . 3_556 ? C2 C1 Li1 B2 -34.2(4) . . . 3_556 ? Li1 C1 Li1 B2 137.2(3) 3_456 . . 3_556 ? B2 C1 Li1 C2 60.0(12) . . . 3_556 ? B1 C1 Li1 C2 -60.5(12) . . . 3_556 ? C2 C1 Li1 C2 179.7(10) . . . 3_556 ? Li1 C1 Li1 C2 -8.9(11) 3_456 . . 3_556 ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.155 _refine_diff_density_min -0.151 _refine_diff_density_rms 0.033 data_r20 _database_code_depnum_ccdc_archive 'CCDC 266131' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H138 B12 N12 Zn3' _chemical_formula_weight 1353.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.091(4) _cell_length_b 14.803(4) _cell_length_c 15.697(5) _cell_angle_alpha 114.889(18) _cell_angle_beta 97.115(19) _cell_angle_gamma 101.325(19) _cell_volume 2028.6(12) _cell_formula_units_Z 1 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 0.920 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8373 _exptl_absorpt_correction_T_max 0.9468 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13417 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7107 _reflns_number_gt 5182 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+1.6600P] 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 7107 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1251 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.017 _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 Zn1 Zn 0.45180(4) 0.64948(3) 0.31827(3) 0.04116(13) Uani 1 1 d . A . Zn2 Zn 0.0000 1.0000 0.0000 0.0640(2) Uani 1 2 d S . . N1 N 0.7490(3) 0.7528(2) 0.35124(18) 0.0429(6) Uani 1 1 d . A . N2 N 0.7049(3) 0.6679(2) 0.25476(18) 0.0403(6) Uani 1 1 d . A . N3 N 0.2091(4) 0.6856(3) 0.4049(2) 0.0679(10) Uani 1 1 d . . . N4 N 0.1691(3) 0.5794(3) 0.3329(3) 0.0648(9) Uani 1 1 d . A . N5 N 0.2469(3) 0.9325(2) 0.0142(2) 0.0568(8) Uani 1 1 d . . . N6 N 0.2813(3) 1.0242(2) 0.1038(2) 0.0505(7) Uani 1 1 d . . . C1 C 0.6137(3) 0.6069(3) 0.3611(2) 0.0424(7) Uani 1 1 d . A . C2 C 0.5747(4) 0.5309(3) 0.4026(3) 0.0640(10) Uani 1 1 d . . . H2A H 0.6511 0.5016 0.4090 0.077 Uiso 1 1 calc R . . H2B H 0.4926 0.4757 0.3595 0.077 Uiso 1 1 calc R . . H2C H 0.5557 0.5672 0.4655 0.077 Uiso 1 1 calc R . . C3 C 0.7301(4) 0.7947(3) 0.5303(3) 0.0680(11) Uani 1 1 d . A . H3A H 0.8271 0.8342 0.5536 0.082 Uiso 1 1 calc R . . H3B H 0.7097 0.7537 0.5642 0.082 Uiso 1 1 calc R . . H3C H 0.6720 0.8417 0.5419 0.082 Uiso 1 1 calc R . . C4 C 0.5948(4) 0.4613(3) 0.1719(3) 0.0616(10) Uani 1 1 d . A . H4A H 0.6678 0.4529 0.1368 0.074 Uiso 1 1 calc R . . H4B H 0.5089 0.4502 0.1288 0.074 Uiso 1 1 calc R . . H4C H 0.5818 0.4114 0.1971 0.074 Uiso 1 1 calc R . . C5 C 0.7934(4) 0.8613(3) 0.3692(3) 0.0557(9) Uani 1 1 d . . . H5 H 0.7946 0.9021 0.4382 0.067 Uiso 1 1 calc R . . C6 C 0.6890(4) 0.8917(3) 0.3161(3) 0.0660(11) Uani 1 1 d . . . H6A H 0.7209 0.9653 0.3357 0.079 Uiso 1 1 calc R . . H6B H 0.5997 0.8762 0.3314 0.079 Uiso 1 1 calc R . . H6C H 0.6796 0.8530 0.2471 0.079 Uiso 1 1 calc R . . C7 C 0.9424(4) 0.8976(3) 0.3622(3) 0.0769(13) Uani 1 1 d . . . H7A H 0.9726 0.9727 0.3935 0.092 Uiso 1 1 calc R . . H7B H 0.9462 0.8712 0.2948 0.092 Uiso 1 1 calc R . . H7C H 1.0030 0.8718 0.3938 0.092 Uiso 1 1 calc R . . C8 C 0.7672(3) 0.6785(3) 0.1780(2) 0.0482(8) Uani 1 1 d . . . H8 H 0.7962 0.7534 0.1965 0.058 Uiso 1 1 calc R . . C9 C 0.6611(4) 0.6268(3) 0.0830(3) 0.0690(11) Uani 1 1 d . . . H9A H 0.7017 0.6408 0.0354 0.083 Uiso 1 1 calc R . . H9B H 0.5809 0.6539 0.0914 0.083 Uiso 1 1 calc R . . H9C H 0.6324 0.5526 0.0611 0.083 Uiso 1 1 calc R . . C10 C 0.8969(4) 0.6414(4) 0.1710(3) 0.0767(12) Uani 1 1 d . . . H10A H 0.9419 0.6582 0.1263 0.092 Uiso 1 1 calc R . . H10B H 0.8718 0.5670 0.1480 0.092 Uiso 1 1 calc R . . H10C H 0.9600 0.6752 0.2342 0.092 Uiso 1 1 calc R . . C11 C 0.2852(3) 0.6806(2) 0.2656(2) 0.0390(7) Uani 1 1 d . . . C12 C 0.3061(4) 0.7124(3) 0.1864(3) 0.0604(10) Uani 1 1 d . A . H12A H 0.2193 0.7187 0.1585 0.073 Uiso 1 1 calc R . . H12B H 0.3362 0.6602 0.1367 0.073 Uiso 1 1 calc R . . H12C H 0.3763 0.7785 0.2138 0.073 Uiso 1 1 calc R . . C13 C 0.3331(5) 0.8733(3) 0.4261(3) 0.0835(14) Uani 1 1 d . . . H13A H 0.2592 0.9020 0.4503 0.100 Uiso 1 1 calc R A . H13B H 0.3655 0.9007 0.3838 0.100 Uiso 1 1 calc R . . H13C H 0.4094 0.8920 0.4799 0.100 Uiso 1 1 calc R . . C14 C 0.1505(5) 0.4719(3) 0.1449(3) 0.0813(14) Uani 1 1 d . . . H14A H 0.0534 0.4601 0.1177 0.098 Uiso 1 1 calc R A . H14B H 0.1624 0.4129 0.1541 0.098 Uiso 1 1 calc R . . H14C H 0.2058 0.4807 0.1011 0.098 Uiso 1 1 calc R . . C15 C 0.2379(9) 0.7473(6) 0.5194(5) 0.0548(14) Uani 0.50 1 d P A 1 H15 H 0.2949 0.8176 0.5360 0.066 Uiso 0.50 1 calc PR A 1 C16 C 0.1094(6) 0.7623(4) 0.5456(4) 0.1003(17) Uani 0.50 1 d P A 1 H16A H 0.0668 0.7928 0.5096 0.150 Uiso 0.50 1 calc PR A 1 H16B H 0.1277 0.8081 0.6142 0.150 Uiso 0.50 1 calc PR A 1 H16C H 0.0471 0.6959 0.5306 0.150 Uiso 0.50 1 calc PR A 1 C17 C 0.3296(5) 0.7051(4) 0.5619(3) 0.0830(14) Uani 0.50 1 d P A 1 H17A H 0.4110 0.7035 0.5348 0.125 Uiso 0.50 1 calc PR A 1 H17B H 0.2809 0.6353 0.5479 0.125 Uiso 0.50 1 calc PR A 1 H17C H 0.3582 0.7482 0.6312 0.125 Uiso 0.50 1 calc PR A 1 C15' C 0.1874(9) 0.6823(6) 0.4943(5) 0.0548(14) Uani 0.50 1 d P A 2 H15' H 0.1302 0.6122 0.4780 0.066 Uiso 0.50 1 calc PR A 2 C16' C 0.1094(6) 0.7623(4) 0.5456(4) 0.1003(17) Uani 0.50 1 d P A 2 H16D H 0.0214 0.7472 0.5026 0.150 Uiso 0.50 1 calc PR A 2 H16E H 0.1652 0.8313 0.5626 0.150 Uiso 0.50 1 calc PR A 2 H16F H 0.0927 0.7584 0.6037 0.150 Uiso 0.50 1 calc PR A 2 C17' C 0.3296(5) 0.7051(4) 0.5619(3) 0.0830(14) Uani 0.50 1 d P A 2 H17D H 0.3777 0.6547 0.5285 0.125 Uiso 0.50 1 calc PR A 2 H17E H 0.3139 0.7005 0.6198 0.125 Uiso 0.50 1 calc PR A 2 H17F H 0.3858 0.7741 0.5793 0.125 Uiso 0.50 1 calc PR A 2 C18 C 0.0879(8) 0.5278(6) 0.3778(6) 0.0508(14) Uani 0.50 1 d P A 1 H18 H 0.1081 0.5760 0.4476 0.061 Uiso 0.50 1 calc PR A 1 C19 C -0.0681(4) 0.4996(4) 0.3376(3) 0.0834(14) Uani 0.50 1 d P A 1 H19A H -0.0948 0.5616 0.3453 0.125 Uiso 0.50 1 calc PR A 1 H19B H -0.1177 0.4688 0.3722 0.125 Uiso 0.50 1 calc PR A 1 H19C H -0.0912 0.4505 0.2696 0.125 Uiso 0.50 1 calc PR A 1 C20 C 0.1351(5) 0.4298(3) 0.3670(4) 0.0891(15) Uani 0.50 1 d P A 1 H20A H 0.2344 0.4498 0.3934 0.134 Uiso 0.50 1 calc PR A 1 H20B H 0.1137 0.3803 0.2992 0.134 Uiso 0.50 1 calc PR A 1 H20C H 0.0864 0.3985 0.4016 0.134 Uiso 0.50 1 calc PR A 1 C18' C 0.0687(8) 0.4756(6) 0.3200(6) 0.0508(14) Uani 0.50 1 d P A 2 H18' H 0.0490 0.4270 0.2504 0.061 Uiso 0.50 1 calc PR A 2 C19' C -0.0681(4) 0.4996(4) 0.3376(3) 0.0834(14) Uani 0.50 1 d P A 2 H19D H -0.0973 0.5312 0.2981 0.125 Uiso 0.50 1 calc PR A 2 H19E H -0.0560 0.5470 0.4052 0.125 Uiso 0.50 1 calc PR A 2 H19F H -0.1384 0.4360 0.3206 0.125 Uiso 0.50 1 calc PR A 2 C20' C 0.1351(5) 0.4298(3) 0.3670(4) 0.0891(15) Uani 0.50 1 d P A 2 H20D H 0.2204 0.4213 0.3463 0.134 Uiso 0.50 1 calc PR A 2 H20E H 0.0747 0.3626 0.3513 0.134 Uiso 0.50 1 calc PR A 2 H20F H 0.1565 0.4736 0.4362 0.134 Uiso 0.50 1 calc PR A 2 C21 C 0.1833(4) 1.0663(4) -0.0146(3) 0.0674(12) Uani 1 1 d . . . C22 C 0.172(3) 1.153(3) -0.0448(17) 0.096(7) Uani 0.50 1 d P B 1 H22A H 0.1299 1.1213 -0.1132 0.145 Uiso 0.50 1 calc PR B 1 H22B H 0.2646 1.1974 -0.0317 0.145 Uiso 0.50 1 calc PR B 1 H22C H 0.1160 1.1935 -0.0083 0.145 Uiso 0.50 1 calc PR B 1 C23 C 0.173(2) 0.9046(12) -0.1757(15) 0.089(4) Uani 0.50 1 d P B 1 H23A H 0.1859 0.8358 -0.2002 0.134 Uiso 0.50 1 calc PR B 1 H23B H 0.2363 0.9467 -0.1949 0.134 Uiso 0.50 1 calc PR B 1 H23C H 0.0778 0.8998 -0.2018 0.134 Uiso 0.50 1 calc PR B 1 C22' C 0.180(3) 1.115(3) -0.0870(16) 0.096(7) Uani 0.50 1 d P B 2 H22D H 0.1261 1.0626 -0.1506 0.145 Uiso 0.50 1 calc PR B 2 H22E H 0.2737 1.1412 -0.0907 0.145 Uiso 0.50 1 calc PR B 2 H22F H 0.1371 1.1717 -0.0641 0.145 Uiso 0.50 1 calc PR B 2 C23' C 0.179(2) 0.8570(13) -0.1715(15) 0.089(4) Uani 0.50 1 d P B 2 H23D H 0.2070 0.8008 -0.1649 0.134 Uiso 0.50 1 calc PR B 2 H23E H 0.2350 0.8799 -0.2084 0.134 Uiso 0.50 1 calc PR B 2 H23F H 0.0818 0.8332 -0.2047 0.134 Uiso 0.50 1 calc PR B 2 C24 C 0.2798(6) 1.2204(4) 0.1751(5) 0.113(2) Uani 1 1 d . . . H24A H 0.3774 1.2456 0.2076 0.136 Uiso 1 1 calc R B . H24B H 0.2237 1.2202 0.2209 0.136 Uiso 1 1 calc R . . H24C H 0.2573 1.2654 0.1483 0.136 Uiso 1 1 calc R . . C25 C 0.2957(4) 0.8452(3) 0.0156(4) 0.0810(14) Uani 1 1 d . . . H25 H 0.3128 0.8575 0.0836 0.097 Uiso 1 1 calc R . . C26 C 0.4343(5) 0.8450(4) -0.0126(4) 0.0892(15) Uani 1 1 d . . . H26A H 0.4681 0.7914 -0.0046 0.107 Uiso 1 1 calc R . . H26B H 0.5008 0.9119 0.0283 0.107 Uiso 1 1 calc R . . H26C H 0.4226 0.8315 -0.0795 0.107 Uiso 1 1 calc R . . C27 C 0.1838(5) 0.7447(3) -0.0409(4) 0.0902(15) Uani 1 1 d . . . H27A H 0.2108 0.6912 -0.0284 0.108 Uiso 1 1 calc R . . H27B H 0.1707 0.7250 -0.1093 0.108 Uiso 1 1 calc R . . H27C H 0.0977 0.7530 -0.0214 0.108 Uiso 1 1 calc R . . C28 C 0.3076(5) 1.0266(4) 0.2000(3) 0.0819(13) Uani 1 1 d . . . H28 H 0.3073 1.0982 0.2430 0.098 Uiso 1 1 calc R . . C29 C 0.4499(5) 1.0261(4) 0.2367(3) 0.0854(14) Uani 1 1 d . . . H29A H 0.4647 1.0462 0.3052 0.103 Uiso 1 1 calc R . . H29B H 0.5171 1.0748 0.2263 0.103 Uiso 1 1 calc R . . H29C H 0.4609 0.9572 0.2026 0.103 Uiso 1 1 calc R . . C30 C 0.1903(5) 0.9650(3) 0.2178(3) 0.0710(11) Uani 1 1 d . . . H30A H 0.2169 0.9692 0.2811 0.085 Uiso 1 1 calc R . . H30B H 0.1663 0.8933 0.1690 0.085 Uiso 1 1 calc R . . H30C H 0.1108 0.9922 0.2149 0.085 Uiso 1 1 calc R . . B1 B 0.6997(4) 0.7204(3) 0.4184(3) 0.0463(9) Uani 1 1 d . . . B2 B 0.6370(4) 0.5748(3) 0.2584(3) 0.0436(9) Uani 1 1 d . . . B3 B 0.2762(4) 0.7507(3) 0.3677(3) 0.0539(11) Uani 1 1 d . A . B4 B 0.1993(4) 0.5727(3) 0.2452(3) 0.0484(10) Uani 1 1 d . A . B5 B 0.2020(5) 0.9563(5) -0.0613(3) 0.0733(15) Uani 1 1 d . B . B6 B 0.2488(4) 1.1062(3) 0.0907(4) 0.0584(11) Uani 1 1 d . B . 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 Zn1 0.0339(2) 0.0479(2) 0.0506(2) 0.02904(18) 0.01160(16) 0.01424(16) Zn2 0.0381(3) 0.0942(5) 0.0983(5) 0.0763(4) 0.0251(3) 0.0197(3) N1 0.0377(15) 0.0467(15) 0.0411(15) 0.0198(13) 0.0071(12) 0.0068(12) N2 0.0336(14) 0.0484(15) 0.0408(14) 0.0214(13) 0.0121(11) 0.0107(11) N3 0.066(2) 0.114(3) 0.0550(19) 0.051(2) 0.0294(17) 0.053(2) N4 0.0464(18) 0.087(2) 0.105(3) 0.074(2) 0.0372(18) 0.0308(17) N5 0.0399(17) 0.0504(17) 0.076(2) 0.0240(17) 0.0148(15) 0.0151(13) N6 0.0454(17) 0.0560(17) 0.0593(18) 0.0352(15) 0.0125(14) 0.0125(13) C1 0.0330(17) 0.0560(19) 0.055(2) 0.0370(17) 0.0137(14) 0.0178(14) C2 0.055(2) 0.082(3) 0.093(3) 0.067(2) 0.028(2) 0.030(2) C3 0.056(2) 0.091(3) 0.051(2) 0.030(2) 0.0115(18) 0.011(2) C4 0.058(2) 0.050(2) 0.074(3) 0.024(2) 0.0177(19) 0.0179(18) C5 0.051(2) 0.049(2) 0.055(2) 0.0192(18) 0.0122(17) -0.0007(16) C6 0.070(3) 0.052(2) 0.080(3) 0.031(2) 0.023(2) 0.0202(19) C7 0.053(2) 0.080(3) 0.080(3) 0.037(2) 0.007(2) -0.015(2) C8 0.0430(19) 0.058(2) 0.0480(19) 0.0267(17) 0.0180(15) 0.0132(16) C9 0.074(3) 0.086(3) 0.049(2) 0.034(2) 0.018(2) 0.017(2) C10 0.060(3) 0.104(3) 0.093(3) 0.056(3) 0.043(2) 0.036(2) C11 0.0302(16) 0.0475(18) 0.0485(18) 0.0288(15) 0.0115(14) 0.0128(13) C12 0.048(2) 0.086(3) 0.074(3) 0.058(2) 0.0182(19) 0.0224(19) C13 0.072(3) 0.065(3) 0.080(3) 0.002(2) -0.001(2) 0.028(2) C14 0.059(3) 0.049(2) 0.106(4) 0.014(2) 0.006(2) 0.0097(19) C15 0.065(4) 0.052(4) 0.042(3) 0.017(4) 0.014(3) 0.015(3) C16 0.131(5) 0.099(4) 0.088(3) 0.037(3) 0.069(3) 0.054(3) C17 0.090(3) 0.079(3) 0.065(3) 0.036(2) -0.010(2) 0.003(2) C15' 0.065(4) 0.052(4) 0.042(3) 0.017(4) 0.014(3) 0.015(3) C16' 0.131(5) 0.099(4) 0.088(3) 0.037(3) 0.069(3) 0.054(3) C17' 0.090(3) 0.079(3) 0.065(3) 0.036(2) -0.010(2) 0.003(2) C18 0.050(3) 0.046(4) 0.057(4) 0.027(3) 0.016(3) 0.003(3) C19 0.045(2) 0.110(4) 0.081(3) 0.037(3) 0.016(2) 0.004(2) C20 0.092(4) 0.056(3) 0.123(4) 0.046(3) 0.032(3) 0.014(2) C18' 0.050(3) 0.046(4) 0.057(4) 0.027(3) 0.016(3) 0.003(3) C19' 0.045(2) 0.110(4) 0.081(3) 0.037(3) 0.016(2) 0.004(2) C20' 0.092(4) 0.056(3) 0.123(4) 0.046(3) 0.032(3) 0.014(2) C21 0.036(2) 0.104(3) 0.103(3) 0.083(3) 0.023(2) 0.018(2) C22 0.053(4) 0.17(2) 0.141(18) 0.138(17) 0.042(10) 0.033(8) C23 0.083(4) 0.112(13) 0.056(3) 0.029(9) 0.023(3) 0.008(9) C22' 0.053(4) 0.17(2) 0.141(18) 0.138(17) 0.042(10) 0.033(8) C23' 0.083(4) 0.112(13) 0.056(3) 0.029(9) 0.023(3) 0.008(9) C24 0.107(4) 0.062(3) 0.169(6) 0.042(3) 0.060(4) 0.027(3) C25 0.053(2) 0.047(2) 0.133(4) 0.032(3) 0.024(3) 0.0127(18) C26 0.060(3) 0.080(3) 0.125(4) 0.033(3) 0.038(3) 0.035(2) C27 0.084(3) 0.055(3) 0.093(3) 0.010(2) 0.012(3) -0.002(2) C28 0.071(3) 0.096(3) 0.084(3) 0.056(3) 0.008(2) 0.007(2) C29 0.066(3) 0.089(3) 0.081(3) 0.038(3) -0.011(2) 0.001(2) C30 0.077(3) 0.080(3) 0.068(3) 0.041(2) 0.028(2) 0.023(2) B1 0.033(2) 0.065(2) 0.048(2) 0.031(2) 0.0112(17) 0.0175(18) B2 0.0323(19) 0.047(2) 0.057(2) 0.0264(19) 0.0106(17) 0.0162(16) B3 0.042(2) 0.063(3) 0.054(2) 0.022(2) 0.0053(19) 0.026(2) B4 0.030(2) 0.050(2) 0.069(3) 0.030(2) 0.0103(18) 0.0139(16) B5 0.034(2) 0.117(4) 0.053(3) 0.031(3) 0.016(2) 0.001(2) B6 0.043(2) 0.059(3) 0.088(3) 0.043(2) 0.028(2) 0.0151(19) _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 Zn1 C11 2.001(3) . ? Zn1 C1 2.002(3) . ? Zn1 B2 2.443(4) . ? Zn1 B4 2.478(4) . ? Zn1 B3 2.528(4) . ? Zn1 B1 2.537(4) . ? Zn2 C21 2.004(4) 2_575 ? Zn2 C21 2.004(4) . ? Zn2 B5 2.445(5) . ? Zn2 B5 2.445(5) 2_575 ? Zn2 B6 2.546(5) 2_575 ? Zn2 B6 2.546(5) . ? N1 B1 1.432(5) . ? N1 N2 1.443(4) . ? N1 C5 1.471(4) . ? N2 B2 1.442(5) . ? N2 C8 1.476(4) . ? N3 B3 1.429(6) . ? N3 N4 1.433(5) . ? N3 C15' 1.466(8) . ? N3 C15 1.591(8) . ? N4 B4 1.412(5) . ? N4 C18 1.451(8) . ? N4 C18' 1.583(8) . ? N5 B5 1.420(6) . ? N5 N6 1.424(4) . ? N5 C25 1.477(5) . ? N6 B6 1.406(5) . ? N6 C28 1.484(5) . ? C1 B1 1.532(5) . ? C1 C2 1.534(5) . ? C1 B2 1.539(5) . ? C3 B1 1.581(5) . ? C4 B2 1.582(5) . ? C5 C6 1.514(5) . ? C5 C7 1.527(5) . ? C8 C9 1.509(5) . ? C8 C10 1.514(5) . ? C11 B3 1.525(5) . ? C11 C12 1.527(5) . ? C11 B4 1.537(5) . ? C13 B3 1.589(6) . ? C14 B4 1.578(6) . ? C15 C16 1.438(9) . ? C15 C17 1.456(9) . ? C18 C19 1.525(9) . ? C18 C20 1.563(9) . ? C21 B6 1.507(6) . ? C21 B5 1.541(7) . ? C21 C22 1.56(3) . ? C21 C22' 1.58(3) . ? C23 B5 1.59(2) . ? C23' B5 1.68(2) . ? C24 B6 1.586(7) . ? C25 C27 1.502(5) . ? C25 C26 1.519(6) . ? C28 C30 1.477(6) . ? C28 C29 1.482(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Zn1 C1 175.21(13) . . ? C11 Zn1 B2 137.72(13) . . ? C1 Zn1 B2 38.95(13) . . ? C11 Zn1 B4 38.32(13) . . ? C1 Zn1 B4 138.32(13) . . ? B2 Zn1 B4 126.22(13) . . ? C11 Zn1 B3 37.10(13) . . ? C1 Zn1 B3 147.03(14) . . ? B2 Zn1 B3 169.02(14) . . ? B4 Zn1 B3 57.54(14) . . ? C11 Zn1 B1 147.02(13) . . ? C1 Zn1 B1 37.15(13) . . ? B2 Zn1 B1 58.15(13) . . ? B4 Zn1 B1 169.23(13) . . ? B3 Zn1 B1 120.35(13) . . ? C21 Zn2 C21 180.0(3) 2_575 . ? C21 Zn2 B5 141.05(18) 2_575 . ? C21 Zn2 B5 38.95(18) . . ? C21 Zn2 B5 38.95(18) 2_575 2_575 ? C21 Zn2 B5 141.05(18) . 2_575 ? B5 Zn2 B5 180.000(1) . 2_575 ? C21 Zn2 B6 36.27(16) 2_575 2_575 ? C21 Zn2 B6 143.73(16) . 2_575 ? B5 Zn2 B6 122.93(15) . 2_575 ? B5 Zn2 B6 57.07(15) 2_575 2_575 ? C21 Zn2 B6 143.73(16) 2_575 . ? C21 Zn2 B6 36.27(16) . . ? B5 Zn2 B6 57.07(15) . . ? B5 Zn2 B6 122.93(15) 2_575 . ? B6 Zn2 B6 180.0 2_575 . ? B1 N1 N2 110.4(3) . . ? B1 N1 C5 124.5(3) . . ? N2 N1 C5 121.9(3) . . ? B2 N2 N1 109.3(2) . . ? B2 N2 C8 128.8(3) . . ? N1 N2 C8 119.0(2) . . ? B3 N3 N4 110.1(3) . . ? B3 N3 C15' 143.4(5) . . ? N4 N3 C15' 105.1(4) . . ? B3 N3 C15 110.1(4) . . ? N4 N3 C15 137.1(4) . . ? C15' N3 C15 33.3(4) . . ? B4 N4 N3 110.0(3) . . ? B4 N4 C18 145.7(5) . . ? N3 N4 C18 102.3(4) . . ? B4 N4 C18' 112.9(4) . . ? N3 N4 C18' 134.9(4) . . ? C18 N4 C18' 33.2(3) . . ? B5 N5 N6 108.8(3) . . ? B5 N5 C25 132.9(4) . . ? N6 N5 C25 116.2(3) . . ? B6 N6 N5 110.9(3) . . ? B6 N6 C28 122.4(4) . . ? N5 N6 C28 124.5(3) . . ? B1 C1 C2 126.1(3) . . ? B1 C1 B2 104.1(3) . . ? C2 C1 B2 124.1(3) . . ? B1 C1 Zn1 90.7(2) . . ? C2 C1 Zn1 113.2(2) . . ? B2 C1 Zn1 86.18(19) . . ? N1 C5 C6 113.9(3) . . ? N1 C5 C7 115.0(3) . . ? C6 C5 C7 113.5(3) . . ? N2 C8 C9 111.0(3) . . ? N2 C8 C10 111.8(3) . . ? C9 C8 C10 112.9(3) . . ? B3 C11 C12 126.6(3) . . ? B3 C11 B4 103.8(3) . . ? C12 C11 B4 123.3(3) . . ? B3 C11 Zn1 90.6(2) . . ? C12 C11 Zn1 113.0(2) . . ? B4 C11 Zn1 87.9(2) . . ? C16 C15 C17 123.6(7) . . ? C16 C15 N3 108.7(6) . . ? C17 C15 N3 108.9(5) . . ? N4 C18 C19 112.7(6) . . ? N4 C18 C20 109.4(5) . . ? C19 C18 C20 111.1(5) . . ? B6 C21 B5 103.1(3) . . ? B6 C21 C22 114.2(11) . . ? B5 C21 C22 137.4(8) . . ? B6 C21 C22' 134.9(12) . . ? B5 C21 C22' 112.2(10) . . ? C22 C21 C22' 25.2(15) . . ? B6 C21 Zn2 91.8(2) . . ? B5 C21 Zn2 86.2(2) . . ? C22 C21 Zn2 111.5(10) . . ? C22' C21 Zn2 117.1(10) . . ? N5 C25 C27 111.0(4) . . ? N5 C25 C26 111.5(4) . . ? C27 C25 C26 114.9(4) . . ? C30 C28 C29 117.8(4) . . ? C30 C28 N6 114.8(4) . . ? C29 C28 N6 115.5(4) . . ? N1 B1 C1 107.7(3) . . ? N1 B1 C3 123.3(3) . . ? C1 B1 C3 129.0(3) . . ? N1 B1 Zn1 92.1(2) . . ? C1 B1 Zn1 52.11(16) . . ? C3 B1 Zn1 119.4(2) . . ? N2 B2 C1 107.4(3) . . ? N2 B2 C4 125.6(3) . . ? C1 B2 C4 127.0(3) . . ? N2 B2 Zn1 91.10(19) . . ? C1 B2 Zn1 54.87(16) . . ? C4 B2 Zn1 118.3(2) . . ? N3 B3 C11 107.5(3) . . ? N3 B3 C13 124.6(4) . . ? C11 B3 C13 127.9(4) . . ? N3 B3 Zn1 93.4(2) . . ? C11 B3 Zn1 52.32(16) . . ? C13 B3 Zn1 117.5(3) . . ? N4 B4 C11 107.7(3) . . ? N4 B4 C14 125.4(4) . . ? C11 B4 C14 126.9(4) . . ? N4 B4 Zn1 92.7(2) . . ? C11 B4 Zn1 53.79(16) . . ? C14 B4 Zn1 118.4(3) . . ? N5 B5 C21 107.7(3) . . ? N5 B5 C23 138.4(7) . . ? C21 B5 C23 113.8(7) . . ? N5 B5 C23' 112.5(7) . . ? C21 B5 C23' 139.7(7) . . ? C23 B5 C23' 26.3(7) . . ? N5 B5 Zn2 92.4(2) . . ? C21 B5 Zn2 54.9(2) . . ? C23 B5 Zn2 112.8(8) . . ? C23' B5 Zn2 119.8(8) . . ? N6 B6 C21 108.4(4) . . ? N6 B6 C24 123.8(4) . . ? C21 B6 C24 127.7(4) . . ? N6 B6 Zn2 92.8(2) . . ? C21 B6 Zn2 51.91(19) . . ? C24 B6 Zn2 120.4(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag B1 N1 N2 B2 -5.7(3) . . . . ? C5 N1 N2 B2 -166.3(3) . . . . ? B1 N1 N2 C8 -168.0(3) . . . . ? C5 N1 N2 C8 31.4(4) . . . . ? B3 N3 N4 B4 -4.2(4) . . . . ? C15' N3 N4 B4 -174.0(4) . . . . ? C15 N3 N4 B4 -162.8(5) . . . . ? B3 N3 N4 C18 -172.6(4) . . . . ? C15' N3 N4 C18 17.6(5) . . . . ? C15 N3 N4 C18 28.8(7) . . . . ? B3 N3 N4 C18' -165.3(5) . . . . ? C15' N3 N4 C18' 24.9(7) . . . . ? C15 N3 N4 C18' 36.1(8) . . . . ? B5 N5 N6 B6 5.2(4) . . . . ? C25 N5 N6 B6 170.9(3) . . . . ? B5 N5 N6 C28 168.3(4) . . . . ? C25 N5 N6 C28 -26.1(5) . . . . ? C11 Zn1 C1 B1 152.0(15) . . . . ? B2 Zn1 C1 B1 104.1(3) . . . . ? B4 Zn1 C1 B1 -164.6(2) . . . . ? B3 Zn1 C1 B1 -60.2(3) . . . . ? C11 Zn1 C1 C2 -77.7(16) . . . . ? B2 Zn1 C1 C2 -125.6(4) . . . . ? B4 Zn1 C1 C2 -34.3(4) . . . . ? B3 Zn1 C1 C2 70.1(4) . . . . ? B1 Zn1 C1 C2 130.3(4) . . . . ? C11 Zn1 C1 B2 47.9(16) . . . . ? B4 Zn1 C1 B2 91.4(3) . . . . ? B3 Zn1 C1 B2 -164.2(2) . . . . ? B1 Zn1 C1 B2 -104.1(3) . . . . ? B1 N1 C5 C6 -104.6(4) . . . . ? N2 N1 C5 C6 53.3(4) . . . . ? B1 N1 C5 C7 122.1(4) . . . . ? N2 N1 C5 C7 -80.1(4) . . . . ? B2 N2 C8 C9 58.3(4) . . . . ? N1 N2 C8 C9 -143.3(3) . . . . ? B2 N2 C8 C10 -68.8(4) . . . . ? N1 N2 C8 C10 89.6(4) . . . . ? C1 Zn1 C11 B3 151.3(15) . . . . ? B2 Zn1 C11 B3 -164.8(2) . . . . ? B4 Zn1 C11 B3 103.8(3) . . . . ? B1 Zn1 C11 B3 -60.1(3) . . . . ? C1 Zn1 C11 C12 -78.0(16) . . . . ? B2 Zn1 C11 C12 -34.1(3) . . . . ? B4 Zn1 C11 C12 -125.5(3) . . . . ? B3 Zn1 C11 C12 130.7(4) . . . . ? B1 Zn1 C11 C12 70.6(3) . . . . ? C1 Zn1 C11 B4 47.5(16) . . . . ? B2 Zn1 C11 B4 91.4(3) . . . . ? B3 Zn1 C11 B4 -103.8(3) . . . . ? B1 Zn1 C11 B4 -163.9(2) . . . . ? B3 N3 C15 C16 112.6(6) . . . . ? N4 N3 C15 C16 -88.8(7) . . . . ? C15' N3 C15 C16 -68.8(9) . . . . ? B3 N3 C15 C17 -110.2(6) . . . . ? N4 N3 C15 C17 48.3(9) . . . . ? C15' N3 C15 C17 68.4(8) . . . . ? B4 N4 C18 C19 -57.6(10) . . . . ? N3 N4 C18 C19 102.9(5) . . . . ? C18' N4 C18 C19 -67.6(8) . . . . ? B4 N4 C18 C20 66.5(9) . . . . ? N3 N4 C18 C20 -133.0(5) . . . . ? C18' N4 C18 C20 56.5(8) . . . . ? C21 Zn2 C21 B6 177(100) 2_575 . . . ? B5 Zn2 C21 B6 -103.0(3) . . . . ? B5 Zn2 C21 B6 77.0(3) 2_575 . . . ? B6 Zn2 C21 B6 180.0 2_575 . . . ? C21 Zn2 C21 B5 -80(100) 2_575 . . . ? B5 Zn2 C21 B5 180.0 2_575 . . . ? B6 Zn2 C21 B5 -77.0(3) 2_575 . . . ? B6 Zn2 C21 B5 103.0(3) . . . . ? C21 Zn2 C21 C22 60(100) 2_575 . . . ? B5 Zn2 C21 C22 140.1(11) . . . . ? B5 Zn2 C21 C22 -39.9(11) 2_575 . . . ? B6 Zn2 C21 C22 63.0(11) 2_575 . . . ? B6 Zn2 C21 C22 -117.0(11) . . . . ? C21 Zn2 C21 C22' 33(100) 2_575 . . . ? B5 Zn2 C21 C22' 113.0(12) . . . . ? B5 Zn2 C21 C22' -67.0(12) 2_575 . . . ? B6 Zn2 C21 C22' 36.0(12) 2_575 . . . ? B6 Zn2 C21 C22' -144.0(12) . . . . ? B5 N5 C25 C27 -62.4(6) . . . . ? N6 N5 C25 C27 136.3(4) . . . . ? B5 N5 C25 C26 67.1(6) . . . . ? N6 N5 C25 C26 -94.2(5) . . . . ? B6 N6 C28 C30 101.8(5) . . . . ? N5 N6 C28 C30 -59.4(5) . . . . ? B6 N6 C28 C29 -116.0(5) . . . . ? N5 N6 C28 C29 82.8(5) . . . . ? N2 N1 B1 C1 -1.7(4) . . . . ? C5 N1 B1 C1 158.3(3) . . . . ? N2 N1 B1 C3 179.8(3) . . . . ? C5 N1 B1 C3 -20.1(5) . . . . ? N2 N1 B1 Zn1 -52.4(2) . . . . ? C5 N1 B1 Zn1 107.6(3) . . . . ? C2 C1 B1 N1 161.8(3) . . . . ? B2 C1 B1 N1 7.8(3) . . . . ? Zn1 C1 B1 N1 -78.5(3) . . . . ? C2 C1 B1 C3 -19.9(6) . . . . ? B2 C1 B1 C3 -173.9(3) . . . . ? Zn1 C1 B1 C3 99.8(4) . . . . ? C2 C1 B1 Zn1 -119.8(4) . . . . ? B2 C1 B1 Zn1 86.2(2) . . . . ? C11 Zn1 B1 N1 -65.0(3) . . . . ? C1 Zn1 B1 N1 110.9(3) . . . . ? B2 Zn1 B1 N1 65.0(2) . . . . ? B4 Zn1 B1 N1 -177.8(6) . . . . ? B3 Zn1 B1 N1 -102.3(2) . . . . ? C11 Zn1 B1 C1 -175.9(2) . . . . ? B2 Zn1 B1 C1 -45.9(2) . . . . ? B4 Zn1 B1 C1 71.3(7) . . . . ? B3 Zn1 B1 C1 146.8(2) . . . . ? C11 Zn1 B1 C3 65.7(4) . . . . ? C1 Zn1 B1 C3 -118.5(4) . . . . ? B2 Zn1 B1 C3 -164.4(4) . . . . ? B4 Zn1 B1 C3 -47.2(8) . . . . ? B3 Zn1 B1 C3 28.4(4) . . . . ? N1 N2 B2 C1 10.5(3) . . . . ? C8 N2 B2 C1 170.6(3) . . . . ? N1 N2 B2 C4 -169.5(3) . . . . ? C8 N2 B2 C4 -9.5(5) . . . . ? N1 N2 B2 Zn1 63.9(2) . . . . ? C8 N2 B2 Zn1 -136.1(3) . . . . ? B1 C1 B2 N2 -11.1(3) . . . . ? C2 C1 B2 N2 -165.8(3) . . . . ? Zn1 C1 B2 N2 78.7(2) . . . . ? B1 C1 B2 C4 169.0(3) . . . . ? C2 C1 B2 C4 14.3(5) . . . . ? Zn1 C1 B2 C4 -101.2(3) . . . . ? B1 C1 B2 Zn1 -89.8(2) . . . . ? C2 C1 B2 Zn1 115.5(3) . . . . ? C11 Zn1 B2 N2 74.7(3) . . . . ? C1 Zn1 B2 N2 -110.6(3) . . . . ? B4 Zn1 B2 N2 124.9(2) . . . . ? B3 Zn1 B2 N2 18.5(8) . . . . ? B1 Zn1 B2 N2 -67.0(2) . . . . ? C11 Zn1 B2 C1 -174.7(2) . . . . ? B4 Zn1 B2 C1 -124.5(2) . . . . ? B3 Zn1 B2 C1 129.1(7) . . . . ? B1 Zn1 B2 C1 43.6(2) . . . . ? C11 Zn1 B2 C4 -57.5(4) . . . . ? C1 Zn1 B2 C4 117.2(4) . . . . ? B4 Zn1 B2 C4 -7.3(4) . . . . ? B3 Zn1 B2 C4 -113.7(7) . . . . ? B1 Zn1 B2 C4 160.8(3) . . . . ? N4 N3 B3 C11 -2.4(4) . . . . ? C15' N3 B3 C11 160.9(6) . . . . ? C15 N3 B3 C11 162.2(4) . . . . ? N4 N3 B3 C13 179.1(3) . . . . ? C15' N3 B3 C13 -17.6(9) . . . . ? C15 N3 B3 C13 -16.3(6) . . . . ? N4 N3 B3 Zn1 -53.9(3) . . . . ? C15' N3 B3 Zn1 109.4(7) . . . . ? C15 N3 B3 Zn1 110.7(4) . . . . ? C12 C11 B3 N3 159.9(3) . . . . ? B4 C11 B3 N3 7.4(4) . . . . ? Zn1 C11 B3 N3 -80.5(3) . . . . ? C12 C11 B3 C13 -21.7(6) . . . . ? B4 C11 B3 C13 -174.1(4) . . . . ? Zn1 C11 B3 C13 97.9(4) . . . . ? C12 C11 B3 Zn1 -119.6(3) . . . . ? B4 C11 B3 Zn1 88.0(2) . . . . ? C11 Zn1 B3 N3 109.5(3) . . . . ? C1 Zn1 B3 N3 -66.3(4) . . . . ? B2 Zn1 B3 N3 177.5(6) . . . . ? B4 Zn1 B3 N3 64.0(2) . . . . ? B1 Zn1 B3 N3 -103.6(2) . . . . ? C1 Zn1 B3 C11 -175.8(2) . . . . ? B2 Zn1 B3 C11 68.0(7) . . . . ? B4 Zn1 B3 C11 -45.5(2) . . . . ? B1 Zn1 B3 C11 146.8(2) . . . . ? C11 Zn1 B3 C13 -118.2(4) . . . . ? C1 Zn1 B3 C13 66.0(5) . . . . ? B2 Zn1 B3 C13 -50.3(8) . . . . ? B4 Zn1 B3 C13 -163.8(4) . . . . ? B1 Zn1 B3 C13 28.6(4) . . . . ? N3 N4 B4 C11 9.0(4) . . . . ? C18 N4 B4 C11 168.6(7) . . . . ? C18' N4 B4 C11 174.6(4) . . . . ? N3 N4 B4 C14 -170.1(3) . . . . ? C18 N4 B4 C14 -10.5(9) . . . . ? C18' N4 B4 C14 -4.5(6) . . . . ? N3 N4 B4 Zn1 61.7(3) . . . . ? C18 N4 B4 Zn1 -138.6(7) . . . . ? C18' N4 B4 Zn1 -132.7(4) . . . . ? B3 C11 B4 N4 -10.0(4) . . . . ? C12 C11 B4 N4 -163.6(3) . . . . ? Zn1 C11 B4 N4 80.1(3) . . . . ? B3 C11 B4 C14 169.1(3) . . . . ? C12 C11 B4 C14 15.5(5) . . . . ? Zn1 C11 B4 C14 -100.8(4) . . . . ? B3 C11 B4 Zn1 -90.1(2) . . . . ? C12 C11 B4 Zn1 116.3(3) . . . . ? C11 Zn1 B4 N4 -110.0(3) . . . . ? C1 Zn1 B4 N4 75.3(3) . . . . ? B2 Zn1 B4 N4 126.5(2) . . . . ? B3 Zn1 B4 N4 -66.0(2) . . . . ? B1 Zn1 B4 N4 16.0(8) . . . . ? C1 Zn1 B4 C11 -174.7(2) . . . . ? B2 Zn1 B4 C11 -123.5(2) . . . . ? B3 Zn1 B4 C11 44.0(2) . . . . ? B1 Zn1 B4 C11 126.0(7) . . . . ? C11 Zn1 B4 C14 116.8(4) . . . . ? C1 Zn1 B4 C14 -57.9(4) . . . . ? B2 Zn1 B4 C14 -6.8(4) . . . . ? B3 Zn1 B4 C14 160.7(4) . . . . ? B1 Zn1 B4 C14 -117.3(7) . . . . ? N6 N5 B5 C21 -10.1(4) . . . . ? C25 N5 B5 C21 -172.4(3) . . . . ? N6 N5 B5 C23 166.9(13) . . . . ? C25 N5 B5 C23 4.6(14) . . . . ? N6 N5 B5 C23' 172.4(9) . . . . ? C25 N5 B5 C23' 10.1(10) . . . . ? N6 N5 B5 Zn2 -63.9(3) . . . . ? C25 N5 B5 Zn2 133.8(4) . . . . ? B6 C21 B5 N5 10.8(4) . . . . ? C22 C21 B5 N5 161.9(17) . . . . ? C22' C21 B5 N5 162.1(12) . . . . ? Zn2 C21 B5 N5 -80.1(3) . . . . ? B6 C21 B5 C23 -167.0(9) . . . . ? C22 C21 B5 C23 -16.0(19) . . . . ? C22' C21 B5 C23 -15.7(15) . . . . ? Zn2 C21 B5 C23 102.0(9) . . . . ? B6 C21 B5 C23' -172.7(13) . . . . ? C22 C21 B5 C23' -22(2) . . . . ? C22' C21 B5 C23' -21.5(18) . . . . ? Zn2 C21 B5 C23' 96.3(13) . . . . ? B6 C21 B5 Zn2 91.0(3) . . . . ? C22 C21 B5 Zn2 -118.0(17) . . . . ? C22' C21 B5 Zn2 -117.8(12) . . . . ? C21 Zn2 B5 N5 -70.0(3) 2_575 . . . ? C21 Zn2 B5 N5 110.0(3) . . . . ? B5 Zn2 B5 N5 -89(100) 2_575 . . . ? B6 Zn2 B5 N5 -113.3(3) 2_575 . . . ? B6 Zn2 B5 N5 66.7(3) . . . . ? C21 Zn2 B5 C21 180.0 2_575 . . . ? B5 Zn2 B5 C21 161(100) 2_575 . . . ? B6 Zn2 B5 C21 136.6(2) 2_575 . . . ? B6 Zn2 B5 C21 -43.4(2) . . . . ? C21 Zn2 B5 C23 76.1(7) 2_575 . . . ? C21 Zn2 B5 C23 -103.9(7) . . . . ? B5 Zn2 B5 C23 57(100) 2_575 . . . ? B6 Zn2 B5 C23 32.8(7) 2_575 . . . ? B6 Zn2 B5 C23 -147.2(7) . . . . ? C21 Zn2 B5 C23' 47.8(8) 2_575 . . . ? C21 Zn2 B5 C23' -132.2(8) . . . . ? B5 Zn2 B5 C23' 29(100) 2_575 . . . ? B6 Zn2 B5 C23' 4.4(7) 2_575 . . . ? B6 Zn2 B5 C23' -175.6(7) . . . . ? N5 N6 B6 C21 2.1(4) . . . . ? C28 N6 B6 C21 -161.4(3) . . . . ? N5 N6 B6 C24 -177.3(4) . . . . ? C28 N6 B6 C24 19.2(6) . . . . ? N5 N6 B6 Zn2 52.7(3) . . . . ? C28 N6 B6 Zn2 -110.8(3) . . . . ? B5 C21 B6 N6 -7.8(4) . . . . ? C22 C21 B6 N6 -166.7(10) . . . . ? C22' C21 B6 N6 -148.9(12) . . . . ? Zn2 C21 B6 N6 78.7(3) . . . . ? B5 C21 B6 C24 171.6(4) . . . . ? C22 C21 B6 C24 12.6(11) . . . . ? C22' C21 B6 C24 30.5(13) . . . . ? Zn2 C21 B6 C24 -101.9(4) . . . . ? B5 C21 B6 Zn2 -86.5(3) . . . . ? C22 C21 B6 Zn2 114.6(10) . . . . ? C22' C21 B6 Zn2 132.4(12) . . . . ? C21 Zn2 B6 N6 68.7(4) 2_575 . . . ? C21 Zn2 B6 N6 -111.3(4) . . . . ? B5 Zn2 B6 N6 -64.4(3) . . . . ? B5 Zn2 B6 N6 115.6(3) 2_575 . . . ? B6 Zn2 B6 N6 -97(100) 2_575 . . . ? C21 Zn2 B6 C21 180.000(1) 2_575 . . . ? B5 Zn2 B6 C21 46.9(3) . . . . ? B5 Zn2 B6 C21 -133.1(3) 2_575 . . . ? B6 Zn2 B6 C21 14(100) 2_575 . . . ? C21 Zn2 B6 C24 -63.8(5) 2_575 . . . ? C21 Zn2 B6 C24 116.2(5) . . . . ? B5 Zn2 B6 C24 163.1(5) . . . . ? B5 Zn2 B6 C24 -16.9(5) 2_575 . . . ? B6 Zn2 B6 C24 131(100) 2_575 . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.713 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.052