# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Polly Arnold' _publ_contact_author_email POLLY.ARNOLD@ED.AC.UK _publ_section_title ; Magnesium and zinc complexes of functionalised, saturated N-heterocyclic carbene ligands; carbene lability and functionalisation, and lactide polymerisation catalysis ; loop_ _publ_author_name 'Polly Arnold' 'Ronan Bellabarba' 'Ian J. Casely' 'Robert B. Tooze' 'Zoe R. Turner' # Attachment '8087HLpSiMe3I.cif' data_po8087 _database_code_depnum_ccdc_archive 'CCDC 727055' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H29 N2 O Si, I' _chemical_formula_sum 'C13 H29 I N2 O Si' _chemical_formula_weight 384.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.0263(5) _cell_length_b 12.5089(5) _cell_length_c 11.8971(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.656(2) _cell_angle_gamma 90.00 _cell_volume 1883.77(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9928 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.4 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 1.758 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.465 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 SMART APEX CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5197 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0152 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.64 _reflns_number_total 5197 _reflns_number_gt 5053 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemans, 1993)' _computing_cell_refinement 'SAINT (Siemans, 1995)' _computing_data_reduction 'SAINT (Siemans, 1995)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _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^)+(0.0421P)^2^+3.2124P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5197 _refine_ls_number_parameters 182 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1113 _refine_ls_wR_factor_gt 0.1094 _refine_ls_goodness_of_fit_ref 1.276 _refine_ls_restrained_S_all 1.276 _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 C1 C 0.4799(3) 0.3154(3) 0.5478(3) 0.0274(6) Uani 1 1 d . . . H1 H 0.4700 0.3808 0.5844 0.033 Uiso 1 1 calc R . . C2 C 0.2925(3) 0.2563(3) 0.5155(3) 0.0331(8) Uani 1 1 d . . . H2 H 0.2747 0.1895 0.5529 0.040 Uiso 1 1 calc R . . C3 C 0.2204(3) 0.2643(5) 0.3956(4) 0.0513(11) Uani 1 1 d . . . H3A H 0.2394 0.3275 0.3562 0.077 Uiso 1 1 calc R . . H3B H 0.1470 0.2705 0.4018 0.077 Uiso 1 1 calc R . . H3C H 0.2282 0.2001 0.3511 0.077 Uiso 1 1 calc R . . C4 C 0.2772(3) 0.3508(4) 0.5893(4) 0.0476(10) Uani 1 1 d . . . H4A H 0.3250 0.3442 0.6661 0.071 Uiso 1 1 calc R . . H4B H 0.2039 0.3523 0.5970 0.071 Uiso 1 1 calc R . . H4C H 0.2927 0.4171 0.5527 0.071 Uiso 1 1 calc R . . C5 C 0.4431(3) 0.1564(3) 0.4528(3) 0.0329(7) Uani 1 1 d . . . H5A H 0.4085 0.1509 0.3694 0.039 Uiso 1 1 calc R . . H5B H 0.4320 0.0889 0.4917 0.039 Uiso 1 1 calc R . . C6 C 0.5602(3) 0.1818(3) 0.4713(4) 0.0409(9) Uani 1 1 d . . . H6A H 0.6041 0.1252 0.5173 0.049 Uiso 1 1 calc R . . H6B H 0.5803 0.1895 0.3964 0.049 Uiso 1 1 calc R . . C7 C 0.6646(3) 0.3524(3) 0.5527(3) 0.0296(7) Uani 1 1 d . . . H7A H 0.6450 0.4244 0.5752 0.035 Uiso 1 1 calc R . . H7B H 0.6861 0.3596 0.4786 0.035 Uiso 1 1 calc R . . C8 C 0.7584(3) 0.3124(3) 0.6443(3) 0.0306(7) Uani 1 1 d . . . C9 C 0.7268(3) 0.2912(3) 0.7573(3) 0.0376(8) Uani 1 1 d . . . H9A H 0.6760 0.2321 0.7467 0.056 Uiso 1 1 calc R . . H9B H 0.6944 0.3555 0.7809 0.056 Uiso 1 1 calc R . . H9C H 0.7897 0.2721 0.8174 0.056 Uiso 1 1 calc R . . C10 C 0.8449(3) 0.3968(3) 0.6613(4) 0.0444(10) Uani 1 1 d . . . H10A H 0.9065 0.3722 0.7199 0.067 Uiso 1 1 calc R . . H10B H 0.8187 0.4638 0.6871 0.067 Uiso 1 1 calc R . . H10C H 0.8650 0.4088 0.5880 0.067 Uiso 1 1 calc R . . C11 C 0.9145(13) 0.0955(12) 0.8008(11) 0.072(4) Uani 0.75(3) 1 d PU A 1 H11A H 0.9399 0.1586 0.8480 0.108 Uiso 0.75(3) 1 calc PR A 1 H11B H 0.9679 0.0389 0.8184 0.108 Uiso 0.75(3) 1 calc PR A 1 H11C H 0.8487 0.0702 0.8181 0.108 Uiso 0.75(3) 1 calc PR A 1 C11A C 0.863(4) 0.058(4) 0.767(4) 0.080(8) Uani 0.25(3) 1 d PU A 2 H11D H 0.8797 0.1028 0.8358 0.120 Uiso 0.25(3) 1 calc PR A 2 H11E H 0.9065 -0.0071 0.7801 0.120 Uiso 0.25(3) 1 calc PR A 2 H11F H 0.7879 0.0375 0.7501 0.120 Uiso 0.25(3) 1 calc PR A 2 C12 C 1.0152(4) 0.1912(5) 0.6263(5) 0.0653(15) Uani 1 1 d . A . H12A H 1.0087 0.2118 0.5455 0.098 Uiso 1 1 calc R . . H12B H 1.0721 0.1387 0.6492 0.098 Uiso 1 1 calc R . . H12C H 1.0315 0.2545 0.6758 0.098 Uiso 1 1 calc R . . C13 C 0.8551(5) 0.0191(5) 0.5401(8) 0.088(2) Uani 1 1 d . A . H13A H 0.7857 -0.0092 0.5430 0.133 Uiso 1 1 calc R . . H13B H 0.9083 -0.0374 0.5615 0.133 Uiso 1 1 calc R . . H13C H 0.8533 0.0439 0.4615 0.133 Uiso 1 1 calc R . . N1 N 0.5723(2) 0.2837(2) 0.5346(2) 0.0270(6) Uani 1 1 d . . . N2 N 0.4026(2) 0.2493(2) 0.5064(2) 0.0274(6) Uani 1 1 d . . . O1 O 0.7914(2) 0.2154(2) 0.5995(2) 0.0336(5) Uani 1 1 d . A . Si1 Si 0.88936(10) 0.13189(10) 0.64238(11) 0.0420(3) Uani 1 1 d . . . I1 I 0.46596(2) 0.063649(19) 0.75997(2) 0.03868(9) 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 C1 0.0281(16) 0.0269(16) 0.0270(14) 0.0020(12) 0.0062(12) 0.0025(13) C2 0.0293(17) 0.0335(19) 0.0352(17) 0.0032(14) 0.0052(15) -0.0029(14) C3 0.030(2) 0.073(3) 0.044(2) 0.003(2) -0.0044(18) 0.005(2) C4 0.033(2) 0.055(3) 0.059(3) -0.013(2) 0.0205(19) 0.0012(19) C5 0.0335(18) 0.0336(18) 0.0308(16) -0.0093(14) 0.0060(14) -0.0022(14) C6 0.0333(19) 0.034(2) 0.058(2) -0.0183(18) 0.0152(17) -0.0020(15) C7 0.0298(16) 0.0259(16) 0.0347(16) 0.0011(13) 0.0113(14) -0.0010(13) C8 0.0282(16) 0.0268(17) 0.0382(17) -0.0041(14) 0.0103(14) -0.0010(14) C9 0.039(2) 0.039(2) 0.0347(17) -0.0005(15) 0.0089(15) 0.0041(16) C10 0.036(2) 0.033(2) 0.062(3) -0.0068(19) 0.0072(19) -0.0094(16) C11 0.073(8) 0.078(8) 0.070(6) 0.035(5) 0.026(6) 0.043(6) C11A 0.091(17) 0.083(17) 0.071(15) 0.045(12) 0.029(13) 0.039(14) C12 0.030(2) 0.079(4) 0.085(4) -0.023(3) 0.010(2) 0.003(2) C13 0.056(3) 0.043(3) 0.163(7) -0.039(4) 0.019(4) 0.006(2) N1 0.0278(14) 0.0242(13) 0.0304(13) -0.0022(11) 0.0094(11) -0.0011(11) N2 0.0284(14) 0.0254(14) 0.0272(13) 0.0002(10) 0.0043(12) -0.0018(11) O1 0.0279(12) 0.0265(12) 0.0462(14) -0.0063(11) 0.0080(11) 0.0023(10) Si1 0.0389(6) 0.0388(6) 0.0510(6) 0.0035(5) 0.0162(5) 0.0131(5) I1 0.05689(17) 0.02772(13) 0.02959(13) 0.00324(9) 0.00653(11) -0.00458(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.306(4) . ? C1 N1 1.311(4) . ? C1 H1 0.9500 . ? C2 N2 1.465(5) . ? C2 C4 1.515(6) . ? C2 C3 1.515(5) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N2 1.481(4) . ? C5 C6 1.523(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N1 1.470(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N1 1.452(4) . ? C7 C8 1.518(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O1 1.432(4) . ? C8 C9 1.520(5) . ? C8 C10 1.522(5) . ? 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 Si1 1.891(11) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11A Si1 1.85(3) . ? C11A H11D 0.9800 . ? C11A H11E 0.9800 . ? C11A H11F 0.9800 . ? C12 Si1 1.850(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 Si1 1.848(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? O1 Si1 1.635(3) . ? 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 C1 N1 114.3(3) . . ? N2 C1 H1 122.9 . . ? N1 C1 H1 122.9 . . ? N2 C2 C4 110.8(3) . . ? N2 C2 C3 109.5(3) . . ? C4 C2 C3 110.9(4) . . ? N2 C2 H2 108.5 . . ? C4 C2 H2 108.5 . . ? C3 C2 H2 108.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C6 102.7(3) . . ? N2 C5 H5A 111.2 . . ? C6 C5 H5A 111.2 . . ? N2 C5 H5B 111.2 . . ? C6 C5 H5B 111.2 . . ? H5A C5 H5B 109.1 . . ? N1 C6 C5 103.7(3) . . ? N1 C6 H6A 111.0 . . ? C5 C6 H6A 111.0 . . ? N1 C6 H6B 111.0 . . ? C5 C6 H6B 111.0 . . ? H6A C6 H6B 109.0 . . ? N1 C7 C8 114.2(3) . . ? N1 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? N1 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? O1 C8 C7 105.9(3) . . ? O1 C8 C9 110.4(3) . . ? C7 C8 C9 110.7(3) . . ? O1 C8 C10 111.1(3) . . ? C7 C8 C10 108.2(3) . . ? C9 C8 C10 110.5(3) . . ? 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 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? Si1 C11A H11D 109.5 . . ? Si1 C11A H11E 109.5 . . ? H11D C11A H11E 109.5 . . ? Si1 C11A H11F 109.5 . . ? H11D C11A H11F 109.5 . . ? H11E C11A H11F 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C1 N1 C7 123.7(3) . . ? C1 N1 C6 109.5(3) . . ? C7 N1 C6 125.0(3) . . ? C1 N2 C2 127.9(3) . . ? C1 N2 C5 109.8(3) . . ? C2 N2 C5 122.2(3) . . ? C8 O1 Si1 134.9(2) . . ? O1 Si1 C11A 106.9(12) . . ? O1 Si1 C13 103.5(2) . . ? C11A Si1 C13 94.7(19) . . ? O1 Si1 C12 110.9(2) . . ? C11A Si1 C12 128.5(19) . . ? C13 Si1 C12 108.7(3) . . ? O1 Si1 C11 113.8(3) . . ? C11A Si1 C11 26.1(17) . . ? C13 Si1 C11 115.5(6) . . ? C12 Si1 C11 104.5(6) . . ? 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 C5 C6 N1 1.2(4) . . . . ? N1 C7 C8 O1 66.0(4) . . . . ? N1 C7 C8 C9 -53.7(4) . . . . ? N1 C7 C8 C10 -174.9(3) . . . . ? N2 C1 N1 C7 167.3(3) . . . . ? N2 C1 N1 C6 2.1(4) . . . . ? C8 C7 N1 C1 121.1(3) . . . . ? C8 C7 N1 C6 -76.0(4) . . . . ? C5 C6 N1 C1 -2.0(4) . . . . ? C5 C6 N1 C7 -167.0(3) . . . . ? N1 C1 N2 C2 174.5(3) . . . . ? N1 C1 N2 C5 -1.3(4) . . . . ? C4 C2 N2 C1 -3.8(5) . . . . ? C3 C2 N2 C1 118.9(4) . . . . ? C4 C2 N2 C5 171.5(3) . . . . ? C3 C2 N2 C5 -65.8(4) . . . . ? C6 C5 N2 C1 -0.1(4) . . . . ? C6 C5 N2 C2 -176.1(3) . . . . ? C7 C8 O1 Si1 175.1(3) . . . . ? C9 C8 O1 Si1 -65.0(4) . . . . ? C10 C8 O1 Si1 57.9(5) . . . . ? C8 O1 Si1 C11A 72(2) . . . . ? C8 O1 Si1 C13 171.4(4) . . . . ? C8 O1 Si1 C12 -72.2(4) . . . . ? C8 O1 Si1 C11 45.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.874 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.114 # Attachment 'paed4 MgLpN.cif' data_paed4 _database_code_depnum_ccdc_archive 'CCDC 727056' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H74 Mg2 N6 O2 Si4, C6 H6' _chemical_formula_sum 'C38 H80 Mg2 N6 O2 Si4' _chemical_formula_weight 814.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.0920(18) _cell_length_b 11.541(2) _cell_length_c 11.960(3) _cell_angle_alpha 111.934(3) _cell_angle_beta 103.197(3) _cell_angle_gamma 96.862(3) _cell_volume 1225.3(4) _cell_formula_units_Z 1 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 4308 _cell_measurement_theta_min 1.9531 _cell_measurement_theta_max 28.2689 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.103 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 446 _exptl_absorpt_coefficient_mu 0.183 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8928 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'AFC7/Mercury CCD detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7882 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4343 _reflns_number_gt 3675 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _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^)+(0.0507P)^2^+0.0423P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4343 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1082 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 C1 C 0.54934(18) 0.78563(16) 0.28532(17) 0.0203(4) Uani 1 1 d . . . C2 C 0.4547(2) 0.76673(18) 0.06679(18) 0.0290(5) Uani 1 1 d . . . H2 H 0.3856 0.8120 0.1026 0.035 Uiso 1 1 calc R . . C3 C 0.3769(2) 0.63077(19) -0.02838(19) 0.0344(5) Uani 1 1 d . . . H3A H 0.4417 0.5860 -0.0682 0.052 Uiso 1 1 calc R . . H3B H 0.3005 0.6349 -0.0932 0.052 Uiso 1 1 calc R . . H3C H 0.3387 0.5843 0.0152 0.052 Uiso 1 1 calc R . . C4 C 0.5161(3) 0.8392(2) -0.0001(2) 0.0446(6) Uani 1 1 d . . . H4A H 0.5683 0.9254 0.0617 0.067 Uiso 1 1 calc R . . H4B H 0.4404 0.8459 -0.0636 0.067 Uiso 1 1 calc R . . H4C H 0.5791 0.7929 -0.0413 0.067 Uiso 1 1 calc R . . C5 C 0.6958(2) 0.7326(2) 0.15560(19) 0.0311(5) Uani 1 1 d . . . H5A H 0.7557 0.8022 0.1482 0.037 Uiso 1 1 calc R . . H5B H 0.6806 0.6516 0.0805 0.037 Uiso 1 1 calc R . . C6 C 0.7594(2) 0.7186(2) 0.27628(19) 0.0333(5) Uani 1 1 d . . . H6A H 0.7603 0.6280 0.2597 0.040 Uiso 1 1 calc R . . H6B H 0.8558 0.7716 0.3193 0.040 Uiso 1 1 calc R . . C7 C 0.68378(19) 0.76787(16) 0.47647(17) 0.0218(4) Uani 1 1 d . . . H7A H 0.7619 0.7271 0.4951 0.026 Uiso 1 1 calc R . . H7B H 0.5982 0.7159 0.4764 0.026 Uiso 1 1 calc R . . C8 C 0.71446(17) 0.90281(17) 0.58197(17) 0.0221(4) Uani 1 1 d . . . C9 C 0.84968(18) 0.98549(18) 0.5904(2) 0.0291(5) Uani 1 1 d . . . H9A H 0.8425 0.9896 0.5089 0.044 Uiso 1 1 calc R . . H9B H 0.9283 0.9477 0.6120 0.044 Uiso 1 1 calc R . . H9C H 0.8649 1.0722 0.6558 0.044 Uiso 1 1 calc R . . C10 C 0.7269(2) 0.8875(2) 0.70507(19) 0.0329(5) Uani 1 1 d . . . H10A H 0.7411 0.9717 0.7741 0.049 Uiso 1 1 calc R . . H10B H 0.8065 0.8495 0.7231 0.049 Uiso 1 1 calc R . . H10C H 0.6410 0.8314 0.6970 0.049 Uiso 1 1 calc R . . C11 C 0.3331(2) 0.88986(19) 0.67982(18) 0.0307(5) Uani 1 1 d . . . H11A H 0.4331 0.9110 0.6889 0.046 Uiso 1 1 calc R . . H11B H 0.3207 0.8886 0.7583 0.046 Uiso 1 1 calc R . . H11C H 0.2888 0.9545 0.6617 0.046 Uiso 1 1 calc R . . C12 C 0.3208(2) 0.6057(2) 0.5958(2) 0.0390(5) Uani 1 1 d . . . H12A H 0.2786 0.5200 0.5280 0.059 Uiso 1 1 calc R . . H12B H 0.2979 0.6101 0.6724 0.059 Uiso 1 1 calc R . . H12C H 0.4225 0.6229 0.6125 0.059 Uiso 1 1 calc R . . C13 C 0.0619(2) 0.7061(2) 0.5439(2) 0.0329(5) Uani 1 1 d . . . H13A H 0.0175 0.7606 0.5082 0.049 Uiso 1 1 calc R . . H13B H 0.0560 0.7300 0.6301 0.049 Uiso 1 1 calc R . . H13C H 0.0138 0.6161 0.4920 0.049 Uiso 1 1 calc R . . C14 C 0.3233(2) 0.49386(18) 0.2145(2) 0.0316(5) Uani 1 1 d . . . H14A H 0.4061 0.5461 0.2128 0.047 Uiso 1 1 calc R . . H14B H 0.2758 0.4268 0.1297 0.047 Uiso 1 1 calc R . . H14C H 0.3515 0.4541 0.2729 0.047 Uiso 1 1 calc R . . C15 C 0.0468(2) 0.48116(18) 0.25708(19) 0.0342(5) Uani 1 1 d . . . H15A H 0.0756 0.4428 0.3167 0.051 Uiso 1 1 calc R . . H15B H 0.0111 0.4135 0.1711 0.051 Uiso 1 1 calc R . . H15C H -0.0268 0.5261 0.2776 0.051 Uiso 1 1 calc R . . C16 C 0.1294(2) 0.65945(19) 0.14699(18) 0.0315(5) Uani 1 1 d . . . H16A H 0.0461 0.6908 0.1616 0.047 Uiso 1 1 calc R . . H16B H 0.1044 0.5898 0.0624 0.047 Uiso 1 1 calc R . . H16C H 0.2002 0.7296 0.1537 0.047 Uiso 1 1 calc R . . C100 C 0.9072(2) 0.9922(2) 0.0658(2) 0.0431(6) Uani 1 1 d . . . H100 H 0.8434 0.9868 0.1120 0.052 Uiso 1 1 calc R . . C101 C 0.9609(2) 0.8882(2) 0.0121(2) 0.0421(6) Uani 1 1 d . . . H101 H 0.9331 0.8108 0.0201 0.051 Uiso 1 1 calc R . . C102 C 0.9455(2) 1.1042(2) 0.0531(2) 0.0404(5) Uani 1 1 d . . . H102 H 0.9072 1.1757 0.0893 0.048 Uiso 1 1 calc R . . N1 N 0.66465(15) 0.76545(14) 0.35052(14) 0.0218(3) Uani 1 1 d . . . N2 N 0.56199(15) 0.76449(14) 0.17099(14) 0.0241(4) Uani 1 1 d . . . N3 N 0.27827(14) 0.72362(13) 0.41103(14) 0.0200(3) Uani 1 1 d . . . O1 O 0.60058(11) 0.95978(11) 0.55615(11) 0.0196(3) Uani 1 1 d . . . Mg1 Mg 0.42212(6) 0.86670(5) 0.41702(5) 0.01822(16) Uani 1 1 d . . . Si1 Si 0.25064(5) 0.72845(5) 0.54709(5) 0.02077(15) Uani 1 1 d . . . Si2 Si 0.20118(5) 0.59831(5) 0.26827(5) 0.02162(15) 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 C1 0.0239(10) 0.0116(9) 0.0193(10) 0.0020(7) 0.0047(8) 0.0008(7) C2 0.0370(11) 0.0241(10) 0.0190(10) 0.0046(8) 0.0037(9) 0.0059(9) C3 0.0401(12) 0.0293(11) 0.0227(11) 0.0031(9) 0.0062(9) 0.0005(9) C4 0.0684(16) 0.0303(12) 0.0259(12) 0.0119(10) 0.0033(11) -0.0017(11) C5 0.0330(11) 0.0293(11) 0.0304(12) 0.0066(9) 0.0179(9) 0.0079(9) C6 0.0319(11) 0.0345(12) 0.0322(12) 0.0070(10) 0.0155(9) 0.0142(9) C7 0.0222(9) 0.0183(9) 0.0250(10) 0.0089(8) 0.0064(8) 0.0065(7) C8 0.0191(9) 0.0188(9) 0.0242(10) 0.0062(8) 0.0023(8) 0.0063(7) C9 0.0193(10) 0.0222(10) 0.0382(12) 0.0066(9) 0.0047(8) 0.0050(8) C10 0.0355(11) 0.0353(12) 0.0245(11) 0.0110(9) 0.0021(9) 0.0138(9) C11 0.0363(11) 0.0297(11) 0.0206(11) 0.0056(9) 0.0092(9) 0.0023(9) C12 0.0498(13) 0.0328(12) 0.0376(14) 0.0186(11) 0.0104(11) 0.0124(10) C13 0.0322(11) 0.0307(11) 0.0335(12) 0.0089(9) 0.0148(9) 0.0040(9) C14 0.0399(12) 0.0199(10) 0.0298(12) 0.0038(9) 0.0127(9) 0.0054(9) C15 0.0381(12) 0.0233(11) 0.0280(12) 0.0014(9) 0.0062(9) -0.0028(9) C16 0.0319(11) 0.0299(11) 0.0231(11) 0.0065(9) 0.0014(9) 0.0006(9) C100 0.0411(13) 0.0429(14) 0.0442(14) 0.0173(12) 0.0161(11) 0.0007(11) C101 0.0474(13) 0.0305(12) 0.0459(15) 0.0189(11) 0.0082(11) -0.0004(10) C102 0.0401(13) 0.0297(12) 0.0410(14) 0.0088(10) 0.0043(11) 0.0057(10) N1 0.0228(8) 0.0191(8) 0.0229(9) 0.0059(7) 0.0090(7) 0.0074(6) N2 0.0271(8) 0.0228(8) 0.0190(9) 0.0045(7) 0.0078(7) 0.0057(7) N3 0.0187(7) 0.0175(8) 0.0197(8) 0.0039(6) 0.0055(6) 0.0022(6) O1 0.0179(6) 0.0169(6) 0.0203(7) 0.0047(5) 0.0033(5) 0.0056(5) Mg1 0.0187(3) 0.0142(3) 0.0170(3) 0.0025(2) 0.0038(2) 0.0026(2) Si1 0.0239(3) 0.0174(3) 0.0195(3) 0.0062(2) 0.0064(2) 0.0044(2) Si2 0.0244(3) 0.0156(3) 0.0190(3) 0.0025(2) 0.0053(2) 0.0010(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 C1 N2 1.335(2) . ? C1 N1 1.343(2) . ? C1 Mg1 2.2615(18) . ? C2 N2 1.463(2) . ? C2 C4 1.525(3) . ? C2 C3 1.529(3) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N2 1.475(2) . ? C5 C6 1.516(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N1 1.466(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N1 1.464(2) . ? C7 C8 1.533(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O1 1.421(2) . ? C8 C10 1.526(3) . ? C8 C9 1.529(3) . ? 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 Si1 1.871(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 Si1 1.875(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 Si1 1.8816(19) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 Si2 1.877(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 Si2 1.8814(19) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 Si2 1.880(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C100 C101 1.373(3) . ? C100 C102 1.378(3) . ? C100 H100 0.9500 . ? C101 C102 1.370(3) 2_775 ? C101 H101 0.9500 . ? C102 C101 1.370(3) 2_775 ? C102 H102 0.9500 . ? N3 Si1 1.6948(15) . ? N3 Si2 1.7005(15) . ? N3 Mg1 2.0324(15) . ? O1 Mg1 1.9566(13) 2_676 ? O1 Mg1 2.0001(13) . ? Mg1 O1 1.9566(13) 2_676 ? Mg1 Mg1 2.9553(12) 2_676 ? 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 C1 N1 107.22(15) . . ? N2 C1 Mg1 143.35(14) . . ? N1 C1 Mg1 108.73(12) . . ? N2 C2 C4 111.84(16) . . ? N2 C2 C3 111.05(16) . . ? C4 C2 C3 109.79(16) . . ? N2 C2 H2 108.0 . . ? C4 C2 H2 108.0 . . ? C3 C2 H2 108.0 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C6 102.51(15) . . ? N2 C5 H5A 111.3 . . ? C6 C5 H5A 111.3 . . ? N2 C5 H5B 111.3 . . ? C6 C5 H5B 111.3 . . ? H5A C5 H5B 109.2 . . ? N1 C6 C5 102.15(16) . . ? N1 C6 H6A 111.3 . . ? C5 C6 H6A 111.3 . . ? N1 C6 H6B 111.3 . . ? C5 C6 H6B 111.3 . . ? H6A C6 H6B 109.2 . . ? N1 C7 C8 114.07(14) . . ? N1 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? N1 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? O1 C8 C10 109.83(15) . . ? O1 C8 C9 109.93(14) . . ? C10 C8 C9 110.41(15) . . ? O1 C8 C7 108.48(14) . . ? C10 C8 C7 107.17(15) . . ? C9 C8 C7 110.95(15) . . ? 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 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C101 C100 C102 120.4(2) . . ? C101 C100 H100 119.8 . . ? C102 C100 H100 119.8 . . ? C102 C101 C100 120.2(2) 2_775 . ? C102 C101 H101 119.9 2_775 . ? C100 C101 H101 119.9 . . ? C101 C102 C100 119.5(2) 2_775 . ? C101 C102 H102 120.3 2_775 . ? C100 C102 H102 120.3 . . ? C1 N1 C7 123.44(14) . . ? C1 N1 C6 113.80(15) . . ? C7 N1 C6 121.95(15) . . ? C1 N2 C2 125.18(16) . . ? C1 N2 C5 113.36(15) . . ? C2 N2 C5 121.41(15) . . ? Si1 N3 Si2 123.49(8) . . ? Si1 N3 Mg1 119.40(8) . . ? Si2 N3 Mg1 116.93(8) . . ? C8 O1 Mg1 135.83(10) . 2_676 ? C8 O1 Mg1 124.09(10) . . ? Mg1 O1 Mg1 96.64(5) 2_676 . ? O1 Mg1 O1 83.36(5) 2_676 . ? O1 Mg1 N3 126.06(6) 2_676 . ? O1 Mg1 N3 124.97(6) . . ? O1 Mg1 C1 115.31(6) 2_676 . ? O1 Mg1 C1 88.78(6) . . ? N3 Mg1 C1 110.54(6) . . ? O1 Mg1 Mg1 42.24(4) 2_676 2_676 ? O1 Mg1 Mg1 41.12(4) . 2_676 ? N3 Mg1 Mg1 141.04(6) . 2_676 ? C1 Mg1 Mg1 105.59(5) . 2_676 ? N3 Si1 C11 111.03(8) . . ? N3 Si1 C12 113.03(9) . . ? C11 Si1 C12 107.83(10) . . ? N3 Si1 C13 114.51(9) . . ? C11 Si1 C13 103.12(9) . . ? C12 Si1 C13 106.64(10) . . ? N3 Si2 C14 112.74(8) . . ? N3 Si2 C16 109.87(8) . . ? C14 Si2 C16 109.89(10) . . ? N3 Si2 C15 116.66(8) . . ? C14 Si2 C15 103.19(9) . . ? C16 Si2 C15 103.94(9) . . ? 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 C5 C6 N1 -9.14(19) . . . . ? N1 C7 C8 O1 59.76(19) . . . . ? N1 C7 C8 C10 178.30(14) . . . . ? N1 C7 C8 C9 -61.1(2) . . . . ? C102 C100 C101 C102 0.9(4) . . . 2_775 ? C101 C100 C102 C101 -0.9(4) . . . 2_775 ? N2 C1 N1 C7 -174.27(14) . . . . ? Mg1 C1 N1 C7 13.01(18) . . . . ? N2 C1 N1 C6 -4.4(2) . . . . ? Mg1 C1 N1 C6 -177.15(12) . . . . ? C8 C7 N1 C1 -74.3(2) . . . . ? C8 C7 N1 C6 116.63(17) . . . . ? C5 C6 N1 C1 8.9(2) . . . . ? C5 C6 N1 C7 178.93(15) . . . . ? N1 C1 N2 C2 175.31(15) . . . . ? Mg1 C1 N2 C2 -16.3(3) . . . . ? N1 C1 N2 C5 -2.4(2) . . . . ? Mg1 C1 N2 C5 165.98(16) . . . . ? C4 C2 N2 C1 135.85(18) . . . . ? C3 C2 N2 C1 -101.1(2) . . . . ? C4 C2 N2 C5 -46.6(2) . . . . ? C3 C2 N2 C5 76.4(2) . . . . ? C6 C5 N2 C1 7.7(2) . . . . ? C6 C5 N2 C2 -170.13(15) . . . . ? C10 C8 O1 Mg1 96.76(17) . . . 2_676 ? C9 C8 O1 Mg1 -24.9(2) . . . 2_676 ? C7 C8 O1 Mg1 -146.40(12) . . . 2_676 ? C10 C8 O1 Mg1 -109.49(14) . . . . ? C9 C8 O1 Mg1 128.83(13) . . . . ? C7 C8 O1 Mg1 7.35(18) . . . . ? C8 O1 Mg1 O1 -161.93(15) . . . 2_676 ? Mg1 O1 Mg1 O1 0.0 2_676 . . 2_676 ? C8 O1 Mg1 N3 68.15(14) . . . . ? Mg1 O1 Mg1 N3 -129.92(7) 2_676 . . . ? C8 O1 Mg1 C1 -46.27(13) . . . . ? Mg1 O1 Mg1 C1 115.66(6) 2_676 . . . ? C8 O1 Mg1 Mg1 -161.93(15) . . . 2_676 ? Si1 N3 Mg1 O1 -74.97(11) . . . 2_676 ? Si2 N3 Mg1 O1 109.84(9) . . . 2_676 ? Si1 N3 Mg1 O1 34.59(12) . . . . ? Si2 N3 Mg1 O1 -140.61(8) . . . . ? Si1 N3 Mg1 C1 138.14(9) . . . . ? Si2 N3 Mg1 C1 -37.05(11) . . . . ? Si1 N3 Mg1 Mg1 -18.74(14) . . . 2_676 ? Si2 N3 Mg1 Mg1 166.06(6) . . . 2_676 ? N2 C1 Mg1 O1 -51.7(2) . . . 2_676 ? N1 C1 Mg1 O1 116.59(11) . . . 2_676 ? N2 C1 Mg1 O1 -133.8(2) . . . . ? N1 C1 Mg1 O1 34.52(11) . . . . ? N2 C1 Mg1 N3 99.1(2) . . . . ? N1 C1 Mg1 N3 -92.65(12) . . . . ? N2 C1 Mg1 Mg1 -95.8(2) . . . 2_676 ? N1 C1 Mg1 Mg1 72.50(11) . . . 2_676 ? Si2 N3 Si1 C11 -172.09(10) . . . . ? Mg1 N3 Si1 C11 13.05(12) . . . . ? Si2 N3 Si1 C12 66.59(13) . . . . ? Mg1 N3 Si1 C12 -108.27(11) . . . . ? Si2 N3 Si1 C13 -55.81(13) . . . . ? Mg1 N3 Si1 C13 129.32(10) . . . . ? Si1 N3 Si2 C14 -103.72(12) . . . . ? Mg1 N3 Si2 C14 71.26(11) . . . . ? Si1 N3 Si2 C16 133.34(11) . . . . ? Mg1 N3 Si2 C16 -51.68(11) . . . . ? Si1 N3 Si2 C15 15.44(14) . . . . ? Mg1 N3 Si2 C15 -169.58(9) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 'ACTA 50' _diffrn_measured_fraction_theta_full 'ACTA 50' _refine_diff_density_max 0.253 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.052 # Attachment 'paed6 MgLN.cif' data_paed6 _database_code_depnum_ccdc_archive 'CCDC 727057' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H70 Mg2 N6 O2 Si4' _chemical_formula_sum 'C32 H70 Mg2 N6 O2 Si4' _chemical_formula_weight 731.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.537(2) _cell_length_b 11.495(2) _cell_length_c 18.056(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.067(6) _cell_angle_gamma 90.00 _cell_volume 2174.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 7408 _cell_measurement_theta_min 2.3517 _cell_measurement_theta_max 28.1463 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 0.199 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8331 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; Tmax/Tmin(RR) < 0.90 SADABS corrects for all systematic errors that lead to disparities in the intensities of symmetry-equivalent data. These may include absorption by the mount, crystal decay, changes in the volume of the crystal illuminated, etc. ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'AFC7/Mercury CCD detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 14.7059 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13350 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.34 _reflns_number_total 3951 _reflns_number_gt 3390 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _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^)+(0.0499P)^2^+0.5370P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3951 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1029 _refine_ls_wR_factor_gt 0.0975 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 C1 C 0.27335(16) 0.05953(14) 0.58781(9) 0.0194(4) Uani 1 1 d . . . C2 C 0.30668(19) 0.16248(15) 0.71125(10) 0.0260(4) Uani 1 1 d . . . H2 H 0.3874 0.1874 0.6912 0.031 Uiso 1 1 calc R . . C3 C 0.3423(2) 0.10308(18) 0.78577(11) 0.0362(5) Uani 1 1 d . . . H3A H 0.2644 0.0799 0.8072 0.054 Uiso 1 1 calc R . . H3B H 0.3913 0.1571 0.8197 0.054 Uiso 1 1 calc R . . H3C H 0.3940 0.0340 0.7785 0.054 Uiso 1 1 calc R . . C4 C 0.2254(2) 0.27024(16) 0.71897(12) 0.0371(5) Uani 1 1 d . . . H4A H 0.2065 0.3072 0.6701 0.056 Uiso 1 1 calc R . . H4B H 0.2720 0.3251 0.7534 0.056 Uiso 1 1 calc R . . H4C H 0.1454 0.2479 0.7383 0.056 Uiso 1 1 calc R . . C5 C 0.13150(18) 0.01941(15) 0.67095(11) 0.0252(4) Uani 1 1 d . . . H5 H 0.0897 0.0216 0.7151 0.030 Uiso 1 1 calc R . . C6 C 0.09722(17) -0.04400(15) 0.60964(10) 0.0240(4) Uani 1 1 d . . . H6 H 0.0271 -0.0962 0.6022 0.029 Uiso 1 1 calc R . . C7 C 0.18226(17) -0.07253(15) 0.48596(10) 0.0219(4) Uani 1 1 d . . . H7A H 0.1777 -0.0105 0.4478 0.026 Uiso 1 1 calc R . . H7B H 0.1044 -0.1207 0.4764 0.026 Uiso 1 1 calc R . . C8 C 0.29927(16) -0.14885(14) 0.47747(9) 0.0193(4) Uani 1 1 d . . . C9 C 0.31557(18) -0.24057(14) 0.53921(10) 0.0241(4) Uani 1 1 d . . . H9A H 0.3903 -0.2888 0.5328 0.036 Uiso 1 1 calc R . . H9B H 0.2392 -0.2897 0.5366 0.036 Uiso 1 1 calc R . . H9C H 0.3276 -0.2019 0.5878 0.036 Uiso 1 1 calc R . . C10 C 0.27885(19) -0.20698(16) 0.40135(10) 0.0284(4) Uani 1 1 d . . . H10A H 0.2642 -0.1473 0.3626 0.043 Uiso 1 1 calc R . . H10B H 0.2045 -0.2586 0.3994 0.043 Uiso 1 1 calc R . . H10C H 0.3547 -0.2525 0.3930 0.043 Uiso 1 1 calc R . . C11 C 0.09881(18) 0.29950(17) 0.50839(12) 0.0322(5) Uani 1 1 d . . . H11A H 0.0357 0.2861 0.4654 0.048 Uiso 1 1 calc R . . H11B H 0.0708 0.3643 0.5380 0.048 Uiso 1 1 calc R . . H11C H 0.1073 0.2292 0.5392 0.048 Uiso 1 1 calc R . . C12 C 0.36759(19) 0.38969(17) 0.55698(11) 0.0321(5) Uani 1 1 d . . . H12A H 0.3900 0.3250 0.5912 0.048 Uiso 1 1 calc R . . H12B H 0.3247 0.4506 0.5830 0.048 Uiso 1 1 calc R . . H12C H 0.4453 0.4214 0.5394 0.048 Uiso 1 1 calc R . . C13 C 0.2207(2) 0.46759(16) 0.41489(12) 0.0393(5) Uani 1 1 d . . . H13A H 0.3005 0.5016 0.4015 0.059 Uiso 1 1 calc R . . H13B H 0.1752 0.5250 0.4423 0.059 Uiso 1 1 calc R . . H13C H 0.1673 0.4448 0.3695 0.059 Uiso 1 1 calc R . . C14 C 0.4248(2) 0.07975(16) 0.31609(11) 0.0314(5) Uani 1 1 d . . . H14A H 0.5142 0.0922 0.3355 0.047 Uiso 1 1 calc R . . H14B H 0.4185 0.0708 0.2619 0.047 Uiso 1 1 calc R . . H14C H 0.3928 0.0093 0.3384 0.047 Uiso 1 1 calc R . . C15 C 0.1641(2) 0.1840(2) 0.28957(12) 0.0372(5) Uani 1 1 d . . . H15A H 0.1272 0.1127 0.3079 0.056 Uiso 1 1 calc R . . H15B H 0.1710 0.1766 0.2361 0.056 Uiso 1 1 calc R . . H15C H 0.1092 0.2503 0.2984 0.056 Uiso 1 1 calc R . . C16 C 0.4000(2) 0.33541(16) 0.29455(11) 0.0328(5) Uani 1 1 d . . . H16A H 0.3390 0.4001 0.2901 0.049 Uiso 1 1 calc R . . H16B H 0.4207 0.3127 0.2449 0.049 Uiso 1 1 calc R . . H16C H 0.4780 0.3597 0.3249 0.049 Uiso 1 1 calc R . . N1 N 0.18344(13) -0.01874(12) 0.55948(8) 0.0197(3) Uani 1 1 d . . . N2 N 0.23977(14) 0.08113(12) 0.65735(8) 0.0213(3) Uani 1 1 d . . . N3 N 0.32450(14) 0.22134(12) 0.43377(8) 0.0214(3) Uani 1 1 d . . . O1 O 0.40850(11) -0.07540(9) 0.48058(6) 0.0186(3) Uani 1 1 d . . . Mg1 Mg 0.40728(5) 0.09604(4) 0.50219(3) 0.01770(16) Uani 1 1 d . . . Si1 Si 0.25756(5) 0.33593(4) 0.47506(3) 0.02349(15) Uani 1 1 d . . . Si2 Si 0.32720(5) 0.20785(4) 0.34020(3) 0.02254(15) 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 C1 0.0190(9) 0.0180(8) 0.0217(9) 0.0000(7) 0.0041(7) 0.0014(7) C2 0.0280(11) 0.0267(10) 0.0244(10) -0.0047(7) 0.0072(8) -0.0045(8) C3 0.0376(13) 0.0463(12) 0.0246(11) -0.0054(9) 0.0035(9) -0.0026(9) C4 0.0460(14) 0.0273(11) 0.0393(12) -0.0085(9) 0.0111(10) -0.0017(9) C5 0.0231(10) 0.0241(9) 0.0304(10) 0.0012(8) 0.0117(8) -0.0009(7) C6 0.0176(10) 0.0234(9) 0.0320(11) 0.0015(8) 0.0072(8) -0.0008(7) C7 0.0197(10) 0.0251(9) 0.0205(9) 0.0006(7) 0.0000(7) -0.0036(7) C8 0.0203(9) 0.0191(9) 0.0183(9) -0.0011(7) 0.0014(7) -0.0038(7) C9 0.0258(10) 0.0199(9) 0.0268(10) 0.0015(7) 0.0034(8) -0.0040(7) C10 0.0342(11) 0.0274(10) 0.0234(10) -0.0062(8) 0.0021(8) -0.0095(8) C11 0.0261(11) 0.0279(10) 0.0429(13) -0.0042(9) 0.0054(9) 0.0022(8) C12 0.0325(12) 0.0293(10) 0.0351(12) -0.0066(8) 0.0062(9) -0.0054(8) C13 0.0474(14) 0.0232(10) 0.0477(13) 0.0021(9) 0.0068(11) 0.0084(9) C14 0.0401(12) 0.0310(10) 0.0238(10) -0.0014(8) 0.0067(9) 0.0004(9) C15 0.0277(12) 0.0558(13) 0.0280(11) 0.0051(9) 0.0030(9) -0.0038(9) C16 0.0338(12) 0.0338(11) 0.0321(11) 0.0099(8) 0.0083(9) 0.0011(9) N1 0.0171(8) 0.0197(7) 0.0225(8) 0.0004(6) 0.0028(6) 0.0009(6) N2 0.0216(8) 0.0210(7) 0.0222(8) -0.0002(6) 0.0063(6) -0.0020(6) N3 0.0225(8) 0.0186(7) 0.0231(8) 0.0022(6) 0.0028(6) 0.0020(6) O1 0.0184(7) 0.0164(6) 0.0210(6) -0.0007(5) 0.0024(5) -0.0021(5) Mg1 0.0190(3) 0.0160(3) 0.0183(3) 0.0003(2) 0.0030(2) -0.0002(2) Si1 0.0242(3) 0.0176(3) 0.0288(3) 0.00026(19) 0.0036(2) 0.00084(19) Si2 0.0217(3) 0.0252(3) 0.0209(3) 0.00473(19) 0.0031(2) -0.0003(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 C1 N2 1.363(2) . ? C1 N1 1.366(2) . ? C1 Mg1 2.2403(18) . ? C2 N2 1.474(2) . ? C2 C4 1.521(3) . ? C2 C3 1.520(3) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.343(3) . ? C5 N2 1.387(2) . ? C5 H5 0.9500 . ? C6 N1 1.380(2) . ? C6 H6 0.9500 . ? C7 N1 1.463(2) . ? C7 C8 1.534(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O1 1.424(2) . ? C8 C10 1.523(2) . ? C8 C9 1.531(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si1 1.884(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 Si1 1.884(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 Si1 1.879(2) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 Si2 1.8735(19) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 Si2 1.879(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 Si2 1.8843(19) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? N3 Si2 1.6998(16) . ? N3 Si1 1.7028(15) . ? N3 Mg1 2.0332(15) . ? O1 Mg1 1.9476(14) 3_656 ? O1 Mg1 2.0092(12) . ? Mg1 O1 1.9476(14) 3_656 ? Mg1 Mg1 2.9549(12) 3_656 ? 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 C1 N1 103.16(14) . . ? N2 C1 Mg1 147.72(13) . . ? N1 C1 Mg1 109.11(11) . . ? N2 C2 C4 110.03(16) . . ? N2 C2 C3 110.81(15) . . ? C4 C2 C3 111.92(16) . . ? N2 C2 H2 108.0 . . ? C4 C2 H2 108.0 . . ? C3 C2 H2 108.0 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 N2 106.64(16) . . ? C6 C5 H5 126.7 . . ? N2 C5 H5 126.7 . . ? C5 C6 N1 106.77(16) . . ? C5 C6 H6 126.6 . . ? N1 C6 H6 126.6 . . ? N1 C7 C8 113.73(14) . . ? N1 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? N1 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? O1 C8 C10 109.41(14) . . ? O1 C8 C9 110.59(14) . . ? C10 C8 C9 110.45(14) . . ? O1 C8 C7 108.17(13) . . ? C10 C8 C7 107.62(14) . . ? C9 C8 C7 110.52(14) . . ? 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 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 N1 C6 111.80(14) . . ? C1 N1 C7 123.86(14) . . ? C6 N1 C7 124.30(14) . . ? C1 N2 C5 111.61(15) . . ? C1 N2 C2 124.83(15) . . ? C5 N2 C2 123.54(15) . . ? Si2 N3 Si1 123.85(9) . . ? Si2 N3 Mg1 119.21(8) . . ? Si1 N3 Mg1 116.93(8) . . ? C8 O1 Mg1 136.22(10) . 3_656 ? C8 O1 Mg1 124.58(10) . . ? Mg1 O1 Mg1 96.61(5) 3_656 . ? O1 Mg1 O1 83.39(5) 3_656 . ? O1 Mg1 N3 122.66(6) 3_656 . ? O1 Mg1 N3 126.02(6) . . ? O1 Mg1 C1 123.84(6) 3_656 . ? O1 Mg1 C1 88.15(6) . . ? N3 Mg1 C1 106.91(6) . . ? O1 Mg1 Mg1 42.49(4) 3_656 3_656 ? O1 Mg1 Mg1 40.90(4) . 3_656 ? N3 Mg1 Mg1 139.07(5) . 3_656 ? C1 Mg1 Mg1 110.18(5) . 3_656 ? N3 Si1 C13 116.08(9) . . ? N3 Si1 C11 113.01(8) . . ? C13 Si1 C11 103.16(10) . . ? N3 Si1 C12 110.39(8) . . ? C13 Si1 C12 105.19(10) . . ? C11 Si1 C12 108.40(9) . . ? N3 Si2 C14 111.71(8) . . ? N3 Si2 C15 112.72(9) . . ? C14 Si2 C15 105.58(10) . . ? N3 Si2 C16 114.46(8) . . ? C14 Si2 C16 104.55(9) . . ? C15 Si2 C16 107.11(10) . . ? 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 C5 C6 N1 -0.90(19) . . . . ? N1 C7 C8 O1 -66.89(17) . . . . ? N1 C7 C8 C10 174.99(14) . . . . ? N1 C7 C8 C9 54.30(18) . . . . ? N2 C1 N1 C6 0.29(18) . . . . ? Mg1 C1 N1 C6 -179.48(11) . . . . ? N2 C1 N1 C7 -177.41(14) . . . . ? Mg1 C1 N1 C7 2.82(19) . . . . ? C5 C6 N1 C1 0.40(19) . . . . ? C5 C6 N1 C7 178.08(15) . . . . ? C8 C7 N1 C1 63.2(2) . . . . ? C8 C7 N1 C6 -114.24(18) . . . . ? N1 C1 N2 C5 -0.87(19) . . . . ? Mg1 C1 N2 C5 178.71(18) . . . . ? N1 C1 N2 C2 -179.07(15) . . . . ? Mg1 C1 N2 C2 0.5(3) . . . . ? C6 C5 N2 C1 1.1(2) . . . . ? C6 C5 N2 C2 179.37(15) . . . . ? C4 C2 N2 C1 108.20(19) . . . . ? C3 C2 N2 C1 -127.49(18) . . . . ? C4 C2 N2 C5 -69.8(2) . . . . ? C3 C2 N2 C5 54.5(2) . . . . ? C10 C8 O1 Mg1 -80.66(18) . . . 3_656 ? C9 C8 O1 Mg1 41.2(2) . . . 3_656 ? C7 C8 O1 Mg1 162.37(11) . . . 3_656 ? C10 C8 O1 Mg1 122.19(13) . . . . ? C9 C8 O1 Mg1 -115.93(13) . . . . ? C7 C8 O1 Mg1 5.22(17) . . . . ? C8 O1 Mg1 O1 164.31(14) . . . 3_656 ? Mg1 O1 Mg1 O1 0.0 3_656 . . 3_656 ? C8 O1 Mg1 N3 -69.72(14) . . . . ? Mg1 O1 Mg1 N3 125.97(7) 3_656 . . . ? C8 O1 Mg1 C1 39.93(12) . . . . ? Mg1 O1 Mg1 C1 -124.38(6) 3_656 . . . ? C8 O1 Mg1 Mg1 164.31(14) . . . 3_656 ? Si2 N3 Mg1 O1 71.19(11) . . . 3_656 ? Si1 N3 Mg1 O1 -107.99(9) . . . 3_656 ? Si2 N3 Mg1 O1 -36.08(12) . . . . ? Si1 N3 Mg1 O1 144.74(7) . . . . ? Si2 N3 Mg1 C1 -136.41(9) . . . . ? Si1 N3 Mg1 C1 44.41(10) . . . . ? Si2 N3 Mg1 Mg1 17.90(14) . . . 3_656 ? Si1 N3 Mg1 Mg1 -161.28(6) . . . 3_656 ? N2 C1 Mg1 O1 56.6(2) . . . 3_656 ? N1 C1 Mg1 O1 -123.86(11) . . . 3_656 ? N2 C1 Mg1 O1 137.3(2) . . . . ? N1 C1 Mg1 O1 -43.09(11) . . . . ? N2 C1 Mg1 N3 -95.4(2) . . . . ? N1 C1 Mg1 N3 84.15(12) . . . . ? N2 C1 Mg1 Mg1 102.2(2) . . . 3_656 ? N1 C1 Mg1 Mg1 -78.24(11) . . . 3_656 ? Si2 N3 Si1 C13 -14.63(15) . . . . ? Mg1 N3 Si1 C13 164.51(10) . . . . ? Si2 N3 Si1 C11 104.26(12) . . . . ? Mg1 N3 Si1 C11 -76.60(11) . . . . ? Si2 N3 Si1 C12 -134.17(11) . . . . ? Mg1 N3 Si1 C12 44.97(11) . . . . ? Si1 N3 Si2 C14 173.48(10) . . . . ? Mg1 N3 Si2 C14 -5.64(12) . . . . ? Si1 N3 Si2 C15 -67.83(13) . . . . ? Mg1 N3 Si2 C15 113.05(11) . . . . ? Si1 N3 Si2 C16 54.91(14) . . . . ? Mg1 N3 Si2 C16 -124.21(10) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.251 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.055 # Attachment '8067 ZnLpN.cif' data_po8067 _database_code_depnum_ccdc_archive 'CCDC 727058' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H74 N6 O2 Si4 Zn2, C6 H6' _chemical_formula_sum 'C38 H80 N6 O2 Si4 Zn2' _chemical_formula_weight 896.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 10.0409(2) _cell_length_b 11.4568(3) _cell_length_c 11.9216(3) _cell_angle_alpha 112.0690(10) _cell_angle_beta 102.6990(10) _cell_angle_gamma 96.5540(10) _cell_volume 1210.14(5) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9861 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 30.5 _exptl_crystal_description shard _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 482 _exptl_absorpt_coefficient_mu 1.126 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7163 _exptl_absorpt_correction_T_max 0.82 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Brucker SMART APEX CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 19801 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 30.57 _reflns_number_total 6759 _reflns_number_gt 6435 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemans, 1993)' _computing_cell_refinement 'SAINT (Siemans, 1995)' _computing_data_reduction 'SAINT (Siemans, 1995)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _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^)+(0.0324P)^2^+0.4032P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6759 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0710 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.04824(14) 0.28820(12) 0.79155(12) 0.0207(2) Uani 1 1 d . . . C2 C 0.94864(18) 0.26902(14) 0.57288(13) 0.0298(3) Uani 1 1 d . . . H2 H 0.8784 0.3133 0.6099 0.036 Uiso 1 1 calc R . . C3 C 0.87364(19) 0.13226(15) 0.47666(14) 0.0343(3) Uani 1 1 d . . . H3A H 0.9393 0.0894 0.4347 0.051 Uiso 1 1 calc R . . H3B H 0.7953 0.1363 0.4136 0.051 Uiso 1 1 calc R . . H3C H 0.8382 0.0834 0.5200 0.051 Uiso 1 1 calc R . . C4 C 1.0083(3) 0.34342(18) 0.50619(17) 0.0507(5) Uani 1 1 d . . . H4A H 1.0597 0.4299 0.5684 0.076 Uiso 1 1 calc R . . H4B H 0.9317 0.3507 0.4438 0.076 Uiso 1 1 calc R . . H4C H 1.0718 0.2975 0.4635 0.076 Uiso 1 1 calc R . . C5 C 1.19130(17) 0.23333(16) 0.65778(15) 0.0330(3) Uani 1 1 d . . . H5A H 1.2505 0.3034 0.6498 0.040 Uiso 1 1 calc R . . H5B H 1.1760 0.1521 0.5820 0.040 Uiso 1 1 calc R . . C6 C 1.25675(17) 0.21813(17) 0.77783(15) 0.0344(3) Uani 1 1 d . . . H6A H 1.2571 0.1267 0.7606 0.041 Uiso 1 1 calc R . . H6B H 1.3536 0.2702 0.8191 0.041 Uiso 1 1 calc R . . C7 C 0.77283(18) 0.60841(16) 0.78945(14) 0.0336(3) Uani 1 1 d . . . H7A H 0.8586 0.6634 0.7952 0.050 Uiso 1 1 calc R . . H7B H 0.6933 0.6479 0.7731 0.050 Uiso 1 1 calc R . . H7C H 0.7573 0.5232 0.7203 0.050 Uiso 1 1 calc R . . C8 C 0.78731(14) 0.59403(12) 0.91367(13) 0.0223(3) Uani 1 1 d . . . C9 C 0.81586(14) 0.73064(12) 1.01916(13) 0.0226(3) Uani 1 1 d . . . H9A H 0.9002 0.7836 1.0179 0.027 Uiso 1 1 calc R . . H9B H 0.7360 0.7707 1.0013 0.027 Uiso 1 1 calc R . . C10 C 0.65379(15) 0.51084(14) 0.90790(16) 0.0309(3) Uani 1 1 d . . . H10A H 0.6402 0.4230 0.8437 0.046 Uiso 1 1 calc R . . H10B H 0.5737 0.5476 0.8859 0.046 Uiso 1 1 calc R . . H10C H 0.6617 0.5085 0.9904 0.046 Uiso 1 1 calc R . . C11 C 0.82740(18) -0.00319(14) 0.71407(15) 0.0328(3) Uani 1 1 d . . . H11A H 0.9091 0.0495 0.7105 0.049 Uiso 1 1 calc R . . H11B H 0.7807 -0.0718 0.6300 0.049 Uiso 1 1 calc R . . H11C H 0.8576 -0.0416 0.7736 0.049 Uiso 1 1 calc R . . C12 C 0.62357(17) 0.15984(15) 0.64594(14) 0.0324(3) Uani 1 1 d . . . H12A H 0.5382 0.1882 0.6612 0.049 Uiso 1 1 calc R . . H12B H 0.6007 0.0895 0.5616 0.049 Uiso 1 1 calc R . . H12C H 0.6909 0.2323 0.6515 0.049 Uiso 1 1 calc R . . C13 C 0.55112(18) -0.01687(15) 0.76200(16) 0.0360(4) Uani 1 1 d . . . H13A H 0.5829 -0.0540 0.8223 0.054 Uiso 1 1 calc R . . H13B H 0.5151 -0.0859 0.6766 0.054 Uiso 1 1 calc R . . H13C H 0.4768 0.0279 0.7839 0.054 Uiso 1 1 calc R . . C14 C 0.83321(18) 0.39630(14) 1.18026(14) 0.0313(3) Uani 1 1 d . . . H14A H 0.9312 0.4215 1.1838 0.047 Uiso 1 1 calc R . . H14B H 0.8286 0.3927 1.2602 0.047 Uiso 1 1 calc R . . H14C H 0.7820 0.4598 1.1663 0.047 Uiso 1 1 calc R . . C15 C 0.8269(2) 0.11068(17) 1.09558(18) 0.0411(4) Uani 1 1 d . . . H15A H 0.7837 0.0242 1.0288 0.062 Uiso 1 1 calc R . . H15B H 0.8073 0.1163 1.1742 0.062 Uiso 1 1 calc R . . H15C H 0.9283 0.1271 1.1085 0.062 Uiso 1 1 calc R . . C16 C 0.56387(17) 0.20942(16) 1.04613(16) 0.0338(3) Uani 1 1 d . . . H16A H 0.5167 0.2609 1.0073 0.051 Uiso 1 1 calc R . . H16B H 0.5578 0.2365 1.1329 0.051 Uiso 1 1 calc R . . H16C H 0.5187 0.1179 0.9973 0.051 Uiso 1 1 calc R . . C100 C 0.55507(19) 0.39445(17) 0.44633(17) 0.0397(4) Uani 1 1 d . . . H100 H 0.5933 0.3219 0.4096 0.048 Uiso 1 1 calc R . . C101 C 0.5957(2) 0.50736(19) 0.43514(19) 0.0439(4) Uani 1 1 d . . . H101 H 0.6616 0.5125 0.3901 0.053 Uiso 1 1 calc R . . C102 C 0.5411(2) 0.61307(17) 0.48900(18) 0.0429(4) Uani 1 1 d . . . H102 H 0.5700 0.6910 0.4815 0.051 Uiso 1 1 calc R . . N1 N 1.16326(12) 0.26696(11) 0.85486(11) 0.0230(2) Uani 1 1 d . . . N2 N 1.05739(13) 0.26597(11) 0.67545(11) 0.0249(2) Uani 1 1 d . . . N3 N 0.77831(12) 0.22905(10) 0.90972(10) 0.0204(2) Uani 1 1 d . . . O1 O 0.90412(10) 0.53974(8) 0.93916(9) 0.02007(18) Uani 1 1 d . . . Si1 Si 0.70220(4) 0.10127(3) 0.76807(3) 0.02260(8) Uani 1 1 d . . . Si2 Si 0.75309(4) 0.23425(3) 1.04797(3) 0.02113(8) Uani 1 1 d . . . Zn1 Zn 0.921841(15) 0.361230(13) 0.909075(13) 0.01798(5) 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 C1 0.0242(6) 0.0142(5) 0.0194(6) 0.0042(4) 0.0049(5) 0.0002(5) C2 0.0419(8) 0.0239(6) 0.0184(6) 0.0059(5) 0.0049(6) 0.0053(6) C3 0.0423(9) 0.0270(7) 0.0239(7) 0.0044(6) 0.0061(6) -0.0007(6) C4 0.0792(15) 0.0326(8) 0.0272(8) 0.0140(7) -0.0015(9) -0.0106(9) C5 0.0374(8) 0.0323(7) 0.0306(7) 0.0092(6) 0.0189(7) 0.0085(6) C6 0.0310(8) 0.0378(8) 0.0322(8) 0.0076(6) 0.0136(6) 0.0142(7) C7 0.0378(8) 0.0368(8) 0.0235(7) 0.0126(6) 0.0009(6) 0.0126(7) C8 0.0213(6) 0.0190(6) 0.0222(6) 0.0063(5) 0.0014(5) 0.0049(5) C9 0.0241(6) 0.0184(6) 0.0238(6) 0.0080(5) 0.0046(5) 0.0058(5) C10 0.0208(6) 0.0219(6) 0.0418(8) 0.0077(6) 0.0035(6) 0.0033(5) C11 0.0429(9) 0.0216(6) 0.0311(7) 0.0055(6) 0.0148(7) 0.0081(6) C12 0.0340(8) 0.0306(7) 0.0236(7) 0.0081(6) -0.0002(6) 0.0011(6) C13 0.0379(8) 0.0240(7) 0.0335(8) 0.0038(6) 0.0084(7) -0.0084(6) C14 0.0395(8) 0.0261(7) 0.0212(6) 0.0038(5) 0.0095(6) 0.0003(6) C15 0.0543(11) 0.0357(8) 0.0397(9) 0.0227(7) 0.0097(8) 0.0159(8) C16 0.0301(8) 0.0351(8) 0.0342(8) 0.0103(6) 0.0146(6) 0.0032(6) C100 0.0384(9) 0.0322(8) 0.0403(9) 0.0103(7) 0.0052(7) 0.0046(7) C101 0.0434(10) 0.0429(10) 0.0448(10) 0.0178(8) 0.0165(8) 0.0006(8) C102 0.0479(10) 0.0325(8) 0.0467(10) 0.0211(8) 0.0077(8) -0.0018(7) N1 0.0244(6) 0.0207(5) 0.0229(5) 0.0064(4) 0.0084(5) 0.0074(4) N2 0.0308(6) 0.0219(5) 0.0198(5) 0.0056(4) 0.0088(5) 0.0050(5) N3 0.0222(5) 0.0165(5) 0.0183(5) 0.0042(4) 0.0050(4) 0.0002(4) O1 0.0191(4) 0.0165(4) 0.0197(4) 0.0043(3) 0.0017(3) 0.0041(3) Si1 0.02574(19) 0.01608(16) 0.01968(17) 0.00304(13) 0.00477(14) -0.00049(14) Si2 0.02445(18) 0.01808(16) 0.02002(17) 0.00734(13) 0.00629(14) 0.00345(14) Zn1 0.01834(8) 0.01510(7) 0.01667(8) 0.00398(5) 0.00321(6) 0.00189(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.3348(18) . ? C1 N2 1.3361(17) . ? C1 Zn1 2.1017(13) . ? C2 N2 1.4637(19) . ? C2 C4 1.523(2) . ? C2 C3 1.529(2) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N2 1.474(2) . ? C5 C6 1.520(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N1 1.4664(18) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.528(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 O1 1.4165(16) . ? C8 C10 1.526(2) . ? C8 C9 1.5406(18) . ? C9 N1 1.4593(18) 2_767 ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si1 1.8835(16) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 Si1 1.8823(16) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 Si1 1.8836(16) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 Si2 1.8661(15) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 Si2 1.8802(17) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 Si2 1.8828(16) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C100 C101 1.375(3) . ? C100 C102 1.376(3) 2_666 ? C100 H100 0.9500 . ? C101 C102 1.379(3) . ? C101 H101 0.9500 . ? C102 C100 1.376(3) 2_666 ? C102 H102 0.9500 . ? N1 C9 1.4593(18) 2_767 ? N3 Si2 1.7021(12) . ? N3 Si1 1.7025(11) . ? N3 Zn1 1.9712(11) . ? O1 Zn1 1.9756(9) . ? O1 Zn1 2.0565(9) 2_767 ? Zn1 O1 2.0565(9) 2_767 ? Zn1 Zn1 3.0755(3) 2_767 ? 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 C1 N2 108.25(12) . . ? N1 C1 Zn1 111.14(9) . . ? N2 C1 Zn1 140.28(11) . . ? N2 C2 C4 111.70(14) . . ? N2 C2 C3 110.82(12) . . ? C4 C2 C3 109.45(13) . . ? N2 C2 H2 108.3 . . ? C4 C2 H2 108.3 . . ? C3 C2 H2 108.3 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C6 102.81(12) . . ? N2 C5 H5A 111.2 . . ? C6 C5 H5A 111.2 . . ? N2 C5 H5B 111.2 . . ? C6 C5 H5B 111.2 . . ? H5A C5 H5B 109.1 . . ? N1 C6 C5 101.95(12) . . ? N1 C6 H6A 111.4 . . ? C5 C6 H6A 111.4 . . ? N1 C6 H6B 111.4 . . ? C5 C6 H6B 111.4 . . ? H6A C6 H6B 109.2 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 C8 C10 110.81(11) . . ? O1 C8 C7 109.67(12) . . ? C10 C8 C7 110.47(12) . . ? O1 C8 C9 107.95(10) . . ? C10 C8 C9 110.57(12) . . ? C7 C8 C9 107.27(11) . . ? N1 C9 C8 113.73(11) 2_767 . ? N1 C9 H9A 108.8 2_767 . ? C8 C9 H9A 108.8 . . ? N1 C9 H9B 108.8 2_767 . ? C8 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? 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 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C101 C100 C102 119.72(18) . 2_666 ? C101 C100 H100 120.1 . . ? C102 C100 H100 120.1 2_666 . ? C100 C101 C102 120.34(18) . . ? C100 C101 H101 119.8 . . ? C102 C101 H101 119.8 . . ? C100 C102 C101 119.95(16) 2_666 . ? C100 C102 H102 120.0 2_666 . ? C101 C102 H102 120.0 . . ? C1 N1 C9 123.84(11) . 2_767 ? C1 N1 C6 113.45(12) . . ? C9 N1 C6 121.86(12) 2_767 . ? C1 N2 C2 125.82(13) . . ? C1 N2 C5 112.46(12) . . ? C2 N2 C5 121.70(12) . . ? Si2 N3 Si1 123.20(7) . . ? Si2 N3 Zn1 120.71(6) . . ? Si1 N3 Zn1 115.45(6) . . ? C8 O1 Zn1 132.44(8) . . ? C8 O1 Zn1 122.75(7) . 2_767 ? Zn1 O1 Zn1 99.40(4) . 2_767 ? N3 Si1 C12 109.95(6) . . ? N3 Si1 C11 112.54(7) . . ? C12 Si1 C11 110.89(8) . . ? N3 Si1 C13 116.24(7) . . ? C12 Si1 C13 103.56(8) . . ? C11 Si1 C13 103.17(8) . . ? N3 Si2 C14 111.53(6) . . ? N3 Si2 C15 112.88(7) . . ? C14 Si2 C15 107.90(8) . . ? N3 Si2 C16 113.87(7) . . ? C14 Si2 C16 103.43(7) . . ? C15 Si2 C16 106.61(9) . . ? N3 Zn1 O1 124.76(4) . . ? N3 Zn1 O1 121.82(4) . 2_767 ? O1 Zn1 O1 80.60(4) . 2_767 ? N3 Zn1 C1 114.71(5) . . ? O1 Zn1 C1 114.45(4) . . ? O1 Zn1 C1 90.85(4) 2_767 . ? N3 Zn1 Zn1 135.96(3) . 2_767 ? O1 Zn1 Zn1 41.28(3) . 2_767 ? O1 Zn1 Zn1 39.33(3) 2_767 2_767 ? C1 Zn1 Zn1 106.01(3) . 2_767 ? 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 C5 C6 N1 -9.84(15) . . . . ? O1 C8 C9 N1 -60.02(14) . . . 2_767 ? C10 C8 C9 N1 61.34(15) . . . 2_767 ? C7 C8 C9 N1 -178.14(12) . . . 2_767 ? C102 C100 C101 C102 0.4(3) 2_666 . . . ? C100 C101 C102 C100 -0.4(3) . . . 2_666 ? N2 C1 N1 C9 -173.79(12) . . . 2_767 ? Zn1 C1 N1 C9 11.44(15) . . . 2_767 ? N2 C1 N1 C6 -4.15(16) . . . . ? Zn1 C1 N1 C6 -178.92(10) . . . . ? C5 C6 N1 C1 9.16(17) . . . . ? C5 C6 N1 C9 179.03(12) . . . 2_767 ? N1 C1 N2 C2 175.29(12) . . . . ? Zn1 C1 N2 C2 -12.4(2) . . . . ? N1 C1 N2 C5 -3.18(16) . . . . ? Zn1 C1 N2 C5 169.17(12) . . . . ? C4 C2 N2 C1 134.37(15) . . . . ? C3 C2 N2 C1 -103.31(16) . . . . ? C4 C2 N2 C5 -47.30(19) . . . . ? C3 C2 N2 C5 75.02(18) . . . . ? C6 C5 N2 C1 8.59(16) . . . . ? C6 C5 N2 C2 -169.94(13) . . . . ? C10 C8 O1 Zn1 25.31(16) . . . . ? C7 C8 O1 Zn1 -96.91(13) . . . . ? C9 C8 O1 Zn1 146.52(9) . . . . ? C10 C8 O1 Zn1 -123.03(10) . . . 2_767 ? C7 C8 O1 Zn1 114.75(11) . . . 2_767 ? C9 C8 O1 Zn1 -1.82(14) . . . 2_767 ? Si2 N3 Si1 C12 132.86(9) . . . . ? Zn1 N3 Si1 C12 -56.24(9) . . . . ? Si2 N3 Si1 C11 -102.99(9) . . . . ? Zn1 N3 Si1 C11 67.91(9) . . . . ? Si2 N3 Si1 C13 15.67(12) . . . . ? Zn1 N3 Si1 C13 -173.44(7) . . . . ? Si1 N3 Si2 C14 -172.58(8) . . . . ? Zn1 N3 Si2 C14 16.98(10) . . . . ? Si1 N3 Si2 C15 65.74(11) . . . . ? Zn1 N3 Si2 C15 -104.69(9) . . . . ? Si1 N3 Si2 C16 -55.99(10) . . . . ? Zn1 N3 Si2 C16 133.58(8) . . . . ? Si2 N3 Zn1 O1 -75.18(8) . . . . ? Si1 N3 Zn1 O1 113.68(6) . . . . ? Si2 N3 Zn1 O1 26.16(9) . . . 2_767 ? Si1 N3 Zn1 O1 -144.98(6) . . . 2_767 ? Si2 N3 Zn1 C1 133.92(7) . . . . ? Si1 N3 Zn1 C1 -37.22(8) . . . . ? Si2 N3 Zn1 Zn1 -21.93(10) . . . 2_767 ? Si1 N3 Zn1 Zn1 166.93(3) . . . 2_767 ? C8 O1 Zn1 N3 -31.03(13) . . . . ? Zn1 O1 Zn1 N3 122.39(5) 2_767 . . . ? C8 O1 Zn1 O1 -153.42(13) . . . 2_767 ? Zn1 O1 Zn1 O1 0.0 2_767 . . 2_767 ? C8 O1 Zn1 C1 119.94(11) . . . . ? Zn1 O1 Zn1 C1 -86.64(5) 2_767 . . . ? C8 O1 Zn1 Zn1 -153.42(13) . . . 2_767 ? N1 C1 Zn1 N3 -91.71(10) . . . . ? N2 C1 Zn1 N3 96.08(15) . . . . ? N1 C1 Zn1 O1 114.32(9) . . . . ? N2 C1 Zn1 O1 -57.89(16) . . . . ? N1 C1 Zn1 O1 34.26(9) . . . 2_767 ? N2 C1 Zn1 O1 -137.95(15) . . . 2_767 ? N1 C1 Zn1 Zn1 71.07(9) . . . 2_767 ? N2 C1 Zn1 Zn1 -101.13(15) . . . 2_767 ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.395 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.060 # Attachment '8075 ZnLdN.cif' data_po8075 _database_code_depnum_ccdc_archive 'CCDC 727059' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H47 N3 O Si2 Zn' _chemical_formula_sum 'C25 H47 N3 O Si2 Zn' _chemical_formula_weight 527.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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/N loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.2450(4) _cell_length_b 11.7949(5) _cell_length_c 23.0602(8) _cell_angle_alpha 90.00 _cell_angle_beta 101.3390(10) _cell_angle_gamma 90.00 _cell_volume 2998.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9995 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 30.45 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.919 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.701 _exptl_absorpt_correction_T_max 0.795 _exptl_absorpt_process_details SADABS _exptl_special_details ; INCOMPLETE DATA; Reflection count < 95% completeness The data collection strategy used aimed to achieve a complete data set to 2\? = 53 deg. Some higher angle data were collected in the process and these have been included in the refinement. ; _diffrn_ambient_temperature 150(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 SMART APEX CCD area detector' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 30818 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0400 _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 -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 30.53 _reflns_number_total 8688 _reflns_number_gt 7357 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _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^)+(0.0351P)^2^+2.0169P] 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 RIDING _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8688 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1158 _refine_ls_wR_factor_gt 0.1105 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.198 _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 C1 C 0.29756(18) 0.15042(18) 0.33384(9) 0.0193(4) Uani 1 1 d . . . C5 C 0.46963(19) 0.04381(19) 0.37471(9) 0.0237(4) Uani 1 1 d . . . H5A H 0.4577 -0.0283 0.3948 0.028 Uiso 1 1 calc R . . H5B H 0.5533 0.0714 0.3894 0.028 Uiso 1 1 calc R . . C6 C 0.44298(18) 0.02992(19) 0.30744(9) 0.0237(4) Uani 1 1 d . . . H6A H 0.5092 0.0617 0.2898 0.028 Uiso 1 1 calc R . . H6B H 0.4308 -0.0507 0.2959 0.028 Uiso 1 1 calc R . . C7 C 0.2719(2) 0.1072(2) 0.22749(9) 0.0287(5) Uani 1 1 d . . . H7A H 0.1918 0.0694 0.2212 0.034 Uiso 1 1 calc R . . H7B H 0.3217 0.0671 0.2030 0.034 Uiso 1 1 calc R . . C8 C 0.2537(2) 0.2307(2) 0.20563(10) 0.0282(5) Uani 1 1 d . . . C9 C 0.1973(3) 0.2245(2) 0.13981(11) 0.0448(7) Uani 1 1 d . . . H9A H 0.1216 0.1811 0.1343 0.067 Uiso 1 1 calc R . . H9B H 0.2538 0.1870 0.1186 0.067 Uiso 1 1 calc R . . H9C H 0.1802 0.3013 0.1242 0.067 Uiso 1 1 calc R . . C10 C 0.3758(3) 0.2924(3) 0.21445(13) 0.0422(6) Uani 1 1 d . . . H10A H 0.3629 0.3708 0.2006 0.063 Uiso 1 1 calc R . . H10B H 0.4290 0.2537 0.1918 0.063 Uiso 1 1 calc R . . H10C H 0.4137 0.2921 0.2565 0.063 Uiso 1 1 calc R . . C21 C 0.36780(18) 0.16886(18) 0.44111(9) 0.0207(4) Uani 1 1 d . . . C22 C 0.44016(19) 0.26083(18) 0.46525(9) 0.0227(4) Uani 1 1 d . . . C23 C 0.4278(2) 0.2979(2) 0.52122(10) 0.0293(5) Uani 1 1 d . . . H23 H 0.4759 0.3594 0.5392 0.035 Uiso 1 1 calc R . . C24 C 0.3469(3) 0.2466(2) 0.55096(11) 0.0360(6) Uani 1 1 d . . . H24 H 0.3385 0.2743 0.5886 0.043 Uiso 1 1 calc R . . C25 C 0.2786(2) 0.1558(2) 0.52642(10) 0.0328(5) Uani 1 1 d . . . H25 H 0.2239 0.1210 0.5476 0.039 Uiso 1 1 calc R . . C26 C 0.28799(19) 0.11354(19) 0.47081(9) 0.0243(4) Uani 1 1 d . . . C27 C -0.0784(3) 0.1032(3) 0.25335(16) 0.0596(9) Uani 1 1 d . . . H27A H -0.0185 0.1183 0.2287 0.089 Uiso 1 1 calc R . . H27B H -0.1509 0.0690 0.2291 0.089 Uiso 1 1 calc R . . H27C H -0.0437 0.0510 0.2853 0.089 Uiso 1 1 calc R . . C28 C -0.1828(3) 0.3331(3) 0.22163(13) 0.0531(8) Uani 1 1 d . . . H28A H -0.2039 0.4071 0.2362 0.080 Uiso 1 1 calc R . . H28B H -0.2555 0.2982 0.1979 0.080 Uiso 1 1 calc R . . H28C H -0.1216 0.3433 0.1971 0.080 Uiso 1 1 calc R . . C29 C -0.2489(3) 0.2088(4) 0.32434(16) 0.0668(11) Uani 1 1 d . . . H29A H -0.2233 0.1521 0.3553 0.100 Uiso 1 1 calc R . . H29B H -0.3183 0.1797 0.2957 0.100 Uiso 1 1 calc R . . H29C H -0.2723 0.2787 0.3422 0.100 Uiso 1 1 calc R . . C30 C -0.1007(3) 0.5109(2) 0.36584(13) 0.0452(7) Uani 1 1 d . . . H30A H -0.0738 0.5512 0.3336 0.068 Uiso 1 1 calc R . . H30B H -0.0979 0.5624 0.3994 0.068 Uiso 1 1 calc R . . H30C H -0.1840 0.4841 0.3523 0.068 Uiso 1 1 calc R . . C31 C -0.0456(2) 0.3219(3) 0.45537(12) 0.0399(6) Uani 1 1 d . . . H31A H -0.1237 0.2835 0.4430 0.060 Uiso 1 1 calc R . . H31B H -0.0534 0.3814 0.4840 0.060 Uiso 1 1 calc R . . H31C H 0.0158 0.2669 0.4736 0.060 Uiso 1 1 calc R . . C32 C 0.1577(2) 0.4417(2) 0.41744(10) 0.0311(5) Uani 1 1 d . . . H32A H 0.2112 0.3786 0.4331 0.047 Uiso 1 1 calc R . . H32B H 0.1558 0.4971 0.4489 0.047 Uiso 1 1 calc R . . H32C H 0.1882 0.4781 0.3851 0.047 Uiso 1 1 calc R . . C220 C 0.52534(19) 0.31945(19) 0.43114(10) 0.0244(4) Uani 1 1 d . . . H220 H 0.5603 0.2597 0.4087 0.029 Uiso 1 1 calc R . . C221 C 0.4578(2) 0.4041(2) 0.38591(10) 0.0299(5) Uani 1 1 d . . . H22A H 0.3928 0.3648 0.3588 0.045 Uiso 1 1 calc R . . H22B H 0.5145 0.4375 0.3635 0.045 Uiso 1 1 calc R . . H22C H 0.4227 0.4643 0.4066 0.045 Uiso 1 1 calc R . . C222 C 0.6315(2) 0.3799(2) 0.47086(11) 0.0333(5) Uani 1 1 d . . . H22D H 0.6006 0.4432 0.4911 0.050 Uiso 1 1 calc R . . H22E H 0.6874 0.4088 0.4467 0.050 Uiso 1 1 calc R . . H22F H 0.6744 0.3264 0.5002 0.050 Uiso 1 1 calc R . . C260 C 0.2152(2) 0.0104(2) 0.44547(10) 0.0285(5) Uani 1 1 d . . . H260 H 0.2405 -0.0099 0.4076 0.034 Uiso 1 1 calc R . . C261 C 0.0790(2) 0.0338(2) 0.43142(13) 0.0406(6) Uani 1 1 d . . . H26A H 0.0516 0.0537 0.4679 0.061 Uiso 1 1 calc R . . H26B H 0.0360 -0.0340 0.4140 0.061 Uiso 1 1 calc R . . H26C H 0.0622 0.0969 0.4033 0.061 Uiso 1 1 calc R . . C262 C 0.2432(3) -0.0910(2) 0.48713(12) 0.0403(6) Uani 1 1 d . . . H26D H 0.3305 -0.1064 0.4947 0.060 Uiso 1 1 calc R . . H26E H 0.1990 -0.1576 0.4689 0.060 Uiso 1 1 calc R . . H26F H 0.2180 -0.0739 0.5245 0.060 Uiso 1 1 calc R . . N1 N 0.33009(16) 0.09549(15) 0.28972(8) 0.0234(4) Uani 1 1 d . . . N2 N 0.37860(14) 0.12982(15) 0.38336(7) 0.0187(3) Uani 1 1 d . . . N3 N 0.00298(15) 0.29461(17) 0.33249(8) 0.0241(4) Uani 1 1 d . . . O1 O 0.17334(15) 0.28956(14) 0.23391(7) 0.0297(4) Uani 1 1 d . . . Si1 Si -0.12066(6) 0.23930(6) 0.28584(3) 0.03265(16) Uani 1 1 d . . . Si2 Si 0.00151(5) 0.38686(6) 0.38925(3) 0.02437(14) Uani 1 1 d . . . Zn1 Zn 0.15121(2) 0.25248(2) 0.310719(10) 0.02033(7) 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 C1 0.0218(9) 0.0177(10) 0.0187(9) -0.0001(8) 0.0046(7) -0.0020(8) C5 0.0227(9) 0.0196(11) 0.0274(11) -0.0011(8) 0.0019(8) 0.0065(8) C6 0.0213(9) 0.0224(11) 0.0272(11) -0.0050(9) 0.0043(8) 0.0027(8) C7 0.0393(12) 0.0272(12) 0.0176(10) -0.0044(9) 0.0008(9) 0.0057(10) C8 0.0398(13) 0.0256(12) 0.0198(10) 0.0000(8) 0.0070(9) 0.0054(10) C9 0.075(2) 0.0352(15) 0.0216(12) 0.0014(10) 0.0027(12) 0.0121(14) C10 0.0455(15) 0.0417(16) 0.0441(16) 0.0021(13) 0.0202(12) -0.0020(13) C21 0.0221(9) 0.0208(11) 0.0183(9) 0.0008(8) 0.0015(7) 0.0048(8) C22 0.0235(10) 0.0217(11) 0.0211(10) 0.0008(8) -0.0002(8) 0.0054(8) C23 0.0354(12) 0.0271(12) 0.0220(10) -0.0034(9) -0.0030(9) 0.0033(10) C24 0.0499(15) 0.0375(15) 0.0204(11) -0.0039(10) 0.0066(10) 0.0052(12) C25 0.0402(13) 0.0356(14) 0.0252(11) 0.0038(10) 0.0130(10) 0.0023(11) C26 0.0276(10) 0.0233(11) 0.0221(10) 0.0039(8) 0.0049(8) 0.0028(9) C27 0.0459(17) 0.053(2) 0.073(2) -0.0279(17) -0.0065(15) -0.0100(15) C28 0.0411(15) 0.067(2) 0.0438(16) -0.0010(15) -0.0107(12) -0.0083(15) C29 0.0339(15) 0.106(3) 0.062(2) -0.008(2) 0.0130(14) -0.0339(18) C30 0.0429(15) 0.0402(16) 0.0492(16) -0.0034(13) 0.0009(12) 0.0183(13) C31 0.0395(14) 0.0472(17) 0.0377(14) 0.0005(12) 0.0192(11) 0.0010(12) C32 0.0285(11) 0.0351(13) 0.0290(12) -0.0049(10) 0.0039(9) -0.0024(10) C220 0.0213(9) 0.0211(11) 0.0306(11) -0.0044(9) 0.0045(8) -0.0008(8) C221 0.0306(11) 0.0275(12) 0.0306(12) 0.0035(10) 0.0040(9) -0.0055(10) C222 0.0254(11) 0.0271(13) 0.0435(14) -0.0025(10) -0.0031(10) -0.0024(9) C260 0.0323(11) 0.0256(12) 0.0288(11) 0.0034(9) 0.0090(9) -0.0040(9) C261 0.0326(13) 0.0369(15) 0.0516(16) 0.0104(12) 0.0065(11) -0.0046(11) C262 0.0514(16) 0.0277(14) 0.0414(15) 0.0092(11) 0.0082(12) -0.0012(12) N1 0.0291(9) 0.0200(9) 0.0204(8) -0.0020(7) 0.0037(7) 0.0061(7) N2 0.0182(7) 0.0182(9) 0.0192(8) -0.0015(7) 0.0028(6) 0.0026(7) N3 0.0166(8) 0.0275(10) 0.0274(9) -0.0034(8) 0.0025(7) -0.0008(7) O1 0.0381(9) 0.0284(9) 0.0240(8) 0.0052(7) 0.0093(7) 0.0108(7) Si1 0.0203(3) 0.0393(4) 0.0371(4) -0.0058(3) 0.0026(3) -0.0067(3) Si2 0.0196(3) 0.0270(3) 0.0268(3) -0.0008(2) 0.0051(2) 0.0032(2) Zn1 0.01849(12) 0.02008(14) 0.02157(13) -0.00081(9) 0.00185(9) 0.00146(9) _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 C1 N1 1.317(3) . ? C1 N2 1.336(2) . ? C1 Zn1 2.024(2) . ? C5 N2 1.482(3) . ? C5 C6 1.530(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N1 1.474(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N1 1.462(3) . ? C7 C8 1.541(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O1 1.398(3) . ? C8 C9 1.527(3) . ? C8 C10 1.532(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C21 C26 1.394(3) . ? C21 C22 1.404(3) . ? C21 N2 1.437(3) . ? C22 C23 1.395(3) . ? C22 C220 1.520(3) . ? C23 C24 1.382(4) . ? C23 H23 0.9500 . ? C24 C25 1.374(4) . ? C24 H24 0.9500 . ? C25 C26 1.399(3) . ? C25 H25 0.9500 . ? C26 C260 1.518(3) . ? C27 Si1 1.872(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 Si1 1.871(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 Si1 1.871(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 Si2 1.874(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 Si2 1.873(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 Si2 1.864(2) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C220 C222 1.530(3) . ? C220 C221 1.533(3) . ? C220 H220 1.0000 . ? C221 H22A 0.9800 . ? C221 H22B 0.9800 . ? C221 H22C 0.9800 . ? C222 H22D 0.9800 . ? C222 H22E 0.9800 . ? C222 H22F 0.9800 . ? C260 C261 1.526(3) . ? C260 C262 1.527(3) . ? C260 H260 1.0000 . ? C261 H26A 0.9800 . ? C261 H26B 0.9800 . ? C261 H26C 0.9800 . ? C262 H26D 0.9800 . ? C262 H26E 0.9800 . ? C262 H26F 0.9800 . ? N3 Si2 1.705(2) . ? N3 Si1 1.7110(18) . ? N3 Zn1 1.8991(18) . ? O1 Zn1 1.8878(16) . ? 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 C1 N2 108.93(18) . . ? N1 C1 Zn1 115.09(14) . . ? N2 C1 Zn1 135.73(15) . . ? N2 C5 C6 101.94(16) . . ? N2 C5 H5A 111.4 . . ? C6 C5 H5A 111.4 . . ? N2 C5 H5B 111.4 . . ? C6 C5 H5B 111.4 . . ? H5A C5 H5B 109.2 . . ? N1 C6 C5 102.21(16) . . ? N1 C6 H6A 111.3 . . ? C5 C6 H6A 111.3 . . ? N1 C6 H6B 111.3 . . ? C5 C6 H6B 111.3 . . ? H6A C6 H6B 109.2 . . ? N1 C7 C8 114.55(18) . . ? N1 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? N1 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? O1 C8 C9 107.9(2) . . ? O1 C8 C10 110.3(2) . . ? C9 C8 C10 109.9(2) . . ? O1 C8 C7 111.91(19) . . ? C9 C8 C7 106.39(19) . . ? C10 C8 C7 110.3(2) . . ? 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 . . ? C26 C21 C22 123.10(19) . . ? C26 C21 N2 119.04(19) . . ? C22 C21 N2 117.85(18) . . ? C23 C22 C21 117.0(2) . . ? C23 C22 C220 121.6(2) . . ? C21 C22 C220 121.43(19) . . ? C24 C23 C22 121.1(2) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C25 C24 C23 120.4(2) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 121.2(2) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C21 C26 C25 117.1(2) . . ? C21 C26 C260 122.48(19) . . ? C25 C26 C260 120.4(2) . . ? Si1 C27 H27A 109.5 . . ? Si1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si1 C28 H28A 109.5 . . ? Si1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si1 C29 H29A 109.5 . . ? Si1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si2 C30 H30A 109.5 . . ? Si2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si2 C31 H31A 109.5 . . ? Si2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si2 C32 H32A 109.5 . . ? Si2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C22 C220 C222 113.50(19) . . ? C22 C220 C221 111.71(17) . . ? C222 C220 C221 109.12(19) . . ? C22 C220 H220 107.4 . . ? C222 C220 H220 107.4 . . ? C221 C220 H220 107.4 . . ? C220 C221 H22A 109.5 . . ? C220 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? C220 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? C220 C222 H22D 109.5 . . ? C220 C222 H22E 109.5 . . ? H22D C222 H22E 109.5 . . ? C220 C222 H22F 109.5 . . ? H22D C222 H22F 109.5 . . ? H22E C222 H22F 109.5 . . ? C26 C260 C261 112.3(2) . . ? C26 C260 C262 110.87(19) . . ? C261 C260 C262 110.5(2) . . ? C26 C260 H260 107.7 . . ? C261 C260 H260 107.7 . . ? C262 C260 H260 107.7 . . ? C260 C261 H26A 109.5 . . ? C260 C261 H26B 109.5 . . ? H26A C261 H26B 109.5 . . ? C260 C261 H26C 109.5 . . ? H26A C261 H26C 109.5 . . ? H26B C261 H26C 109.5 . . ? C260 C262 H26D 109.5 . . ? C260 C262 H26E 109.5 . . ? H26D C262 H26E 109.5 . . ? C260 C262 H26F 109.5 . . ? H26D C262 H26F 109.5 . . ? H26E C262 H26F 109.5 . . ? C1 N1 C7 124.94(18) . . ? C1 N1 C6 113.49(17) . . ? C7 N1 C6 121.13(17) . . ? C1 N2 C21 124.50(17) . . ? C1 N2 C5 112.49(16) . . ? C21 N2 C5 122.04(16) . . ? Si2 N3 Si1 126.64(11) . . ? Si2 N3 Zn1 120.77(10) . . ? Si1 N3 Zn1 112.39(10) . . ? C8 O1 Zn1 122.61(14) . . ? N3 Si1 C28 113.77(12) . . ? N3 Si1 C29 112.44(13) . . ? C28 Si1 C29 106.64(17) . . ? N3 Si1 C27 109.87(12) . . ? C28 Si1 C27 105.98(16) . . ? C29 Si1 C27 107.76(18) . . ? N3 Si2 C32 109.77(10) . . ? N3 Si2 C31 114.26(12) . . ? C32 Si2 C31 104.81(12) . . ? N3 Si2 C30 112.04(11) . . ? C32 Si2 C30 108.20(13) . . ? C31 Si2 C30 107.36(13) . . ? O1 Zn1 N3 118.16(8) . . ? O1 Zn1 C1 97.73(7) . . ? N3 Zn1 C1 142.79(8) . . ? 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 C5 C6 N1 -8.6(2) . . . . ? N1 C7 C8 O1 -64.7(3) . . . . ? N1 C7 C8 C9 177.7(2) . . . . ? N1 C7 C8 C10 58.4(3) . . . . ? C26 C21 C22 C23 -1.2(3) . . . . ? N2 C21 C22 C23 179.63(18) . . . . ? C26 C21 C22 C220 -179.48(19) . . . . ? N2 C21 C22 C220 1.4(3) . . . . ? C21 C22 C23 C24 -0.6(3) . . . . ? C220 C22 C23 C24 177.6(2) . . . . ? C22 C23 C24 C25 1.5(4) . . . . ? C23 C24 C25 C26 -0.6(4) . . . . ? C22 C21 C26 C25 2.1(3) . . . . ? N2 C21 C26 C25 -178.76(19) . . . . ? C22 C21 C26 C260 -176.8(2) . . . . ? N2 C21 C26 C260 2.4(3) . . . . ? C24 C25 C26 C21 -1.2(3) . . . . ? C24 C25 C26 C260 177.7(2) . . . . ? C23 C22 C220 C222 26.2(3) . . . . ? C21 C22 C220 C222 -155.6(2) . . . . ? C23 C22 C220 C221 -97.6(2) . . . . ? C21 C22 C220 C221 80.5(2) . . . . ? C21 C26 C260 C261 -114.5(2) . . . . ? C25 C26 C260 C261 66.7(3) . . . . ? C21 C26 C260 C262 121.4(2) . . . . ? C25 C26 C260 C262 -57.4(3) . . . . ? N2 C1 N1 C7 -172.7(2) . . . . ? Zn1 C1 N1 C7 2.5(3) . . . . ? N2 C1 N1 C6 -0.2(3) . . . . ? Zn1 C1 N1 C6 174.98(14) . . . . ? C8 C7 N1 C1 49.0(3) . . . . ? C8 C7 N1 C6 -122.9(2) . . . . ? C5 C6 N1 C1 6.0(2) . . . . ? C5 C6 N1 C7 178.83(19) . . . . ? N1 C1 N2 C21 -175.19(19) . . . . ? Zn1 C1 N2 C21 11.1(3) . . . . ? N1 C1 N2 C5 -6.3(2) . . . . ? Zn1 C1 N2 C5 179.99(17) . . . . ? C26 C21 N2 C1 76.6(3) . . . . ? C22 C21 N2 C1 -104.2(2) . . . . ? C26 C21 N2 C5 -91.3(2) . . . . ? C22 C21 N2 C5 87.9(2) . . . . ? C6 C5 N2 C1 9.6(2) . . . . ? C6 C5 N2 C21 178.82(18) . . . . ? C9 C8 O1 Zn1 144.19(17) . . . . ? C10 C8 O1 Zn1 -95.7(2) . . . . ? C7 C8 O1 Zn1 27.5(3) . . . . ? Si2 N3 Si1 C28 84.61(18) . . . . ? Zn1 N3 Si1 C28 -90.19(16) . . . . ? Si2 N3 Si1 C29 -36.7(2) . . . . ? Zn1 N3 Si1 C29 148.45(17) . . . . ? Si2 N3 Si1 C27 -156.76(17) . . . . ? Zn1 N3 Si1 C27 28.44(18) . . . . ? Si1 N3 Si2 C32 -169.63(14) . . . . ? Zn1 N3 Si2 C32 4.78(16) . . . . ? Si1 N3 Si2 C31 72.99(17) . . . . ? Zn1 N3 Si2 C31 -112.61(14) . . . . ? Si1 N3 Si2 C30 -49.39(19) . . . . ? Zn1 N3 Si2 C30 125.02(15) . . . . ? C8 O1 Zn1 N3 -156.30(17) . . . . ? C8 O1 Zn1 C1 13.56(19) . . . . ? Si2 N3 Zn1 O1 -117.86(12) . . . . ? Si1 N3 Zn1 O1 57.28(14) . . . . ? Si2 N3 Zn1 C1 78.91(18) . . . . ? Si1 N3 Zn1 C1 -105.94(14) . . . . ? N1 C1 Zn1 O1 -30.20(17) . . . . ? N2 C1 Zn1 O1 143.3(2) . . . . ? N1 C1 Zn1 N3 134.92(16) . . . . ? N2 C1 Zn1 N3 -51.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 'ACTA 50' _diffrn_measured_fraction_theta_full 'ACTA 50' _refine_diff_density_max 0.591 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.071 # Attachment '7029 HLKN.cif' data_po7029 _database_code_depnum_ccdc_archive 'CCDC 727060' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H38 K N3 O Si2' _chemical_formula_sum 'C16 H38 K N3 O Si2' _chemical_formula_weight 383.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.9490(4) _cell_length_b 10.9970(5) _cell_length_c 12.2370(5) _cell_angle_alpha 95.194(2) _cell_angle_beta 111.793(2) _cell_angle_gamma 108.661(2) _cell_volume 1143.97(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) __cell_measurement_reflns_used 4732 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.99 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 420 _exptl_absorpt_coefficient_mu 0.344 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5843 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Brucker SMART APEX CCD area detector' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13380 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0517 _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 1.85 _diffrn_reflns_theta_max 28.99 _reflns_number_total 5406 _reflns_number_gt 4732 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemans, 1993)' _computing_cell_refinement 'SAINT (Siemans, 1995)' _computing_data_reduction 'SAINT (Siemans, 1995)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et. al., 2004)' _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^)+(0.0454P)^2^+4.2424P] 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 SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 5406 _refine_ls_number_parameters 220 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1162 _refine_ls_R_factor_gt 0.1039 _refine_ls_wR_factor_ref 0.2270 _refine_ls_wR_factor_gt 0.2216 _refine_ls_goodness_of_fit_ref 1.310 _refine_ls_restrained_S_all 1.310 _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 K1 K 0.52274(12) 0.09565(10) 0.14714(9) 0.0260(2) Uani 1 1 d . . . Si1 Si 0.29201(15) -0.26398(13) 0.03383(12) 0.0260(3) Uani 1 1 d . . . Si2 Si 0.64013(15) -0.18358(12) 0.16454(11) 0.0244(3) Uani 1 1 d . . . N1 N 0.6650(6) 0.3815(5) 0.4869(4) 0.0477(12) Uani 1 1 d . . . N2 N 0.4521(5) 0.2577(5) 0.3036(4) 0.0357(10) Uani 1 1 d . . . N3 N 0.4785(4) -0.1716(4) 0.0649(3) 0.0266(8) Uani 1 1 d . . . O1 O 0.6476(4) 0.1794(4) 0.3991(3) 0.0391(9) Uani 1 1 d . . . C1 C 0.5553(6) 0.2543(5) 0.4178(4) 0.0310(10) Uani 1 1 d . . . H1 H 0.4951 0.2111 0.4629 0.037 Uiso 1 1 calc R . . C2 C 0.2863(6) 0.2085(6) 0.2739(5) 0.0370(12) Uani 1 1 d . . . H2 H 0.2567 0.1135 0.2773 0.044 Uiso 1 1 calc R . . C3 C 0.2361(7) 0.2704(7) 0.3594(5) 0.0449(14) Uani 1 1 d . . . H3A H 0.2985 0.2691 0.4426 0.067 Uiso 1 1 calc R . . H3B H 0.1249 0.2203 0.3372 0.067 Uiso 1 1 calc R . . H3C H 0.2524 0.3620 0.3540 0.067 Uiso 1 1 calc R . . C4 C 0.1939(7) 0.2077(6) 0.1441(5) 0.0416(13) Uani 1 1 d . . . H4A H 0.2296 0.1669 0.0915 0.062 Uiso 1 1 calc R . . H4B H 0.2098 0.2987 0.1365 0.062 Uiso 1 1 calc R . . H4C H 0.0823 0.1571 0.1199 0.062 Uiso 1 1 calc R . . C5 C 0.5177(7) 0.4022(6) 0.2987(6) 0.0514(15) Uani 1 1 d . . . H5A H 0.5127 0.4092 0.2174 0.062 Uiso 1 1 calc R . . H5B H 0.4592 0.4515 0.3192 0.062 Uiso 1 1 calc R . . C6 C 0.6860(7) 0.4536(6) 0.3932(5) 0.0464(14) Uani 1 1 d . . . H6A H 0.7546 0.4297 0.3613 0.056 Uiso 1 1 calc R . . H6B H 0.7286 0.5506 0.4246 0.056 Uiso 1 1 calc R . . C7 C 0.8058(8) 0.3621(7) 0.5660(6) 0.0600(18) Uani 1 1 d . . . H7A H 0.8147 0.3702 0.6499 0.072 Uiso 1 1 calc R . . H7B H 0.9011 0.4289 0.5672 0.072 Uiso 1 1 calc R . . C8 C 0.7866(6) 0.2206(6) 0.5122(5) 0.0402(12) Uani 1 1 d . . . C9 C 0.7661(9) 0.1280(9) 0.5919(6) 0.068(2) Uani 1 1 d . . . H9A H 0.6799 0.1284 0.6123 0.102 Uiso 1 1 calc R . . H9B H 0.8630 0.1563 0.6663 0.102 Uiso 1 1 calc R . . H9C H 0.7422 0.0386 0.5493 0.102 Uiso 1 1 calc R . . C10 C 0.9209(7) 0.2212(7) 0.4791(6) 0.0556(17) Uani 1 1 d . . . H10A H 0.9333 0.2825 0.4269 0.083 Uiso 1 1 calc R . . H10B H 0.8971 0.1321 0.4361 0.083 Uiso 1 1 calc R . . H10C H 1.0182 0.2495 0.5532 0.083 Uiso 1 1 calc R . . C11 C 0.1969(7) -0.1634(6) 0.0882(6) 0.0378(12) Uani 1 1 d . . . C12 C 0.2576(6) -0.4123(5) 0.1014(6) 0.0411(13) Uani 1 1 d . . . H12A H 0.3196 -0.3843 0.1894 0.062 Uiso 1 1 calc R . . H12B H 0.2891 -0.4763 0.0667 0.062 Uiso 1 1 calc R . . H12C H 0.1462 -0.4534 0.0832 0.062 Uiso 1 1 calc R . . C13 C 0.8339(6) 0.3333(5) 0.1338(4) 0.0372(12) Uani 1 1 d . . . H13A H 0.8224 0.2616 0.1759 0.056 Uiso 1 1 calc R . . H13B H 0.8009 0.3987 0.1645 0.056 Uiso 1 1 calc R . . H13C H 0.9437 0.3756 0.1480 0.056 Uiso 1 1 calc R . . C14 C 0.6777(7) -0.3341(5) 0.1234(6) 0.0432(13) Uani 1 1 d . . . H14A H 0.5882 -0.4136 0.1113 0.065 Uiso 1 1 calc R . . H14B H 0.7724 -0.3331 0.1889 0.065 Uiso 1 1 calc R . . H14C H 0.6923 -0.3342 0.0484 0.065 Uiso 1 1 calc R . . C15 C 0.8210(6) -0.0408(5) 0.1846(5) 0.0370(12) Uani 1 1 d . . . H15A H 0.8106 0.0426 0.2064 0.055 Uiso 1 1 calc R . . H15B H 0.8333 -0.0460 0.1087 0.055 Uiso 1 1 calc R . . H15C H 0.9131 -0.0448 0.2492 0.055 Uiso 1 1 calc R . . C16 C 0.6491(7) -0.1777(6) 0.3217(5) 0.0441(13) Uani 1 1 d . . . H16A H 0.6303 -0.1004 0.3483 0.066 Uiso 1 1 calc R . . H16B H 0.7528 -0.1715 0.3777 0.066 Uiso 1 1 calc R . . H16C H 0.5689 -0.2582 0.3207 0.066 Uiso 1 1 calc R . . H11A H 0.191(7) -0.099(6) 0.049(5) 0.041(16) Uiso 1 1 d . . . H11B H 0.254(7) -0.128(6) 0.173(6) 0.046(17) Uiso 1 1 d . . . H11C H 0.106(8) -0.217(7) 0.083(6) 0.055(19) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0319(5) 0.0264(5) 0.0229(5) 0.0061(4) 0.0137(4) 0.0127(4) Si1 0.0272(6) 0.0257(6) 0.0277(6) 0.0116(5) 0.0130(5) 0.0104(5) Si2 0.0281(6) 0.0246(6) 0.0242(6) 0.0096(5) 0.0120(5) 0.0122(5) N1 0.046(3) 0.053(3) 0.042(3) 0.003(2) 0.020(2) 0.017(2) N2 0.026(2) 0.052(3) 0.029(2) 0.0053(19) 0.0118(18) 0.0177(19) N3 0.0257(19) 0.0265(19) 0.029(2) 0.0134(16) 0.0113(16) 0.0106(16) O1 0.0356(19) 0.057(2) 0.0310(19) 0.0125(17) 0.0137(16) 0.0260(18) C1 0.034(3) 0.041(3) 0.024(2) 0.006(2) 0.016(2) 0.016(2) C2 0.033(3) 0.050(3) 0.036(3) 0.015(2) 0.018(2) 0.021(2) C3 0.039(3) 0.069(4) 0.043(3) 0.017(3) 0.027(3) 0.030(3) C4 0.046(3) 0.049(3) 0.034(3) 0.014(2) 0.013(2) 0.027(3) C5 0.049(3) 0.044(3) 0.064(4) 0.024(3) 0.028(3) 0.013(3) C6 0.050(3) 0.036(3) 0.049(3) 0.002(2) 0.021(3) 0.013(3) C7 0.045(4) 0.075(5) 0.048(4) -0.008(3) 0.009(3) 0.025(3) C8 0.031(3) 0.054(3) 0.027(3) 0.001(2) 0.003(2) 0.018(2) C9 0.063(4) 0.108(6) 0.038(3) 0.027(4) 0.019(3) 0.039(4) C10 0.034(3) 0.077(5) 0.050(4) 0.000(3) 0.011(3) 0.025(3) C11 0.036(3) 0.044(3) 0.039(3) 0.014(3) 0.018(2) 0.019(3) C12 0.036(3) 0.037(3) 0.055(3) 0.025(3) 0.022(3) 0.012(2) C13 0.031(3) 0.037(3) 0.030(3) 0.001(2) 0.009(2) 0.003(2) C14 0.046(3) 0.034(3) 0.056(4) 0.012(2) 0.023(3) 0.021(2) C15 0.030(2) 0.034(3) 0.041(3) 0.012(2) 0.011(2) 0.009(2) C16 0.043(3) 0.064(4) 0.026(3) 0.015(2) 0.015(2) 0.020(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 K1 N3 2.794(4) 2_655 ? K1 O1 2.794(4) . ? K1 N3 2.855(4) . ? K1 N2 2.919(4) . ? K1 C11 3.336(6) . ? K1 C13 3.423(5) . ? K1 Si2 3.6148(15) . ? K1 Si1 3.6493(16) 2_655 ? K1 Si1 3.6969(16) . ? K1 K1 3.7958(19) 2_655 ? K1 Si2 3.8973(15) 2_655 ? K1 H11A 2.99(6) . ? Si1 N3 1.679(4) . ? Si1 C13 1.885(5) 2_655 ? Si1 C12 1.887(5) . ? Si1 K1 3.6493(16) 2_655 ? Si2 N3 1.673(4) . ? Si2 C14 1.876(5) . ? Si2 C16 1.886(5) . ? Si2 C15 1.886(5) . ? Si2 K1 3.8973(15) 2_655 ? N1 C1 1.409(7) . ? N1 C7 1.472(8) . ? N1 C6 1.492(8) . ? N2 C1 1.405(6) . ? N2 C2 1.447(6) . ? N2 C5 1.528(7) . ? N3 K1 2.794(4) 2_655 ? O1 C8 1.448(6) . ? O1 C1 1.477(6) . ? C1 H1 1.0000 . ? C2 C4 1.509(7) . ? C2 C3 1.512(7) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.516(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.556(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.491(9) . ? C8 C10 1.531(8) . ? 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 0.90(6) . ? C11 H11B 0.95(6) . ? C11 H11C 0.89(7) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 Si1 1.885(5) 2_655 ? 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 N3 K1 O1 144.83(12) 2_655 . ? N3 K1 N3 95.57(10) 2_655 . ? O1 K1 N3 113.54(11) . . ? N3 K1 N2 116.75(12) 2_655 . ? O1 K1 N2 48.20(11) . . ? N3 K1 N2 141.74(12) . . ? N3 K1 C11 111.08(13) 2_655 . ? O1 K1 C11 101.69(14) . . ? N3 K1 C11 56.23(12) . . ? N2 K1 C11 91.44(13) . . ? N3 K1 C13 55.91(12) 2_655 . ? O1 K1 C13 92.33(12) . . ? N3 K1 C13 115.94(13) . . ? N2 K1 C13 99.68(13) . . ? C11 K1 C13 165.80(14) . . ? N3 K1 Si2 107.68(9) 2_655 . ? O1 K1 Si2 92.50(8) . . ? N3 K1 Si2 26.83(8) . . ? N2 K1 Si2 135.45(10) . . ? C11 K1 Si2 75.06(10) . . ? C13 K1 Si2 102.36(10) . . ? N3 K1 Si1 26.15(8) 2_655 2_655 ? O1 K1 Si1 122.87(9) . 2_655 ? N3 K1 Si1 101.75(8) . 2_655 ? N2 K1 Si1 116.32(10) . 2_655 ? C11 K1 Si1 135.43(11) . 2_655 ? C13 K1 Si1 30.71(9) . 2_655 ? Si2 K1 Si1 101.90(4) . 2_655 ? N3 K1 Si1 101.85(9) 2_655 . ? O1 K1 Si1 112.98(9) . . ? N3 K1 Si1 25.84(8) . . ? N2 K1 Si1 120.59(10) . . ? C11 K1 Si1 30.61(10) . . ? C13 K1 Si1 139.72(10) . . ? Si2 K1 Si1 48.45(3) . . ? Si1 K1 Si1 117.78(3) 2_655 . ? N3 K1 K1 48.47(8) 2_655 2_655 ? O1 K1 K1 154.43(9) . 2_655 ? N3 K1 K1 47.10(8) . 2_655 ? N2 K1 K1 157.21(9) . 2_655 ? C11 K1 K1 81.18(11) . 2_655 ? C13 K1 K1 85.21(9) . 2_655 ? Si2 K1 K1 63.40(3) . 2_655 ? Si1 K1 K1 59.51(3) 2_655 2_655 ? Si1 K1 K1 58.28(3) . 2_655 ? N3 K1 Si2 21.97(8) 2_655 2_655 ? O1 K1 Si2 146.94(9) . 2_655 ? N3 K1 Si2 99.48(8) . 2_655 ? N2 K1 Si2 103.70(9) . 2_655 ? C11 K1 Si2 95.15(11) . 2_655 ? C13 K1 Si2 73.74(9) . 2_655 ? Si2 K1 Si2 119.44(3) . 2_655 ? Si1 K1 Si2 46.72(3) 2_655 2_655 ? Si1 K1 Si2 95.92(3) . 2_655 ? K1 K1 Si2 56.03(3) 2_655 2_655 ? N3 K1 H11A 99.2(12) 2_655 . ? O1 K1 H11A 110.5(12) . . ? N3 K1 H11A 65.1(12) . . ? N2 K1 H11A 88.8(11) . . ? C11 K1 H11A 15.1(12) . . ? C13 K1 H11A 154.9(12) . . ? Si2 K1 H11A 87.3(12) . . ? Si1 K1 H11A 125.0(12) 2_655 . ? Si1 K1 H11A 39.6(12) . . ? K1 K1 H11A 78.5(11) 2_655 . ? Si2 K1 H11A 81.3(12) 2_655 . ? N3 Si1 C13 112.5(2) . 2_655 ? N3 Si1 C12 117.0(2) . . ? C13 Si1 C12 104.4(3) 2_655 . ? N3 Si1 K1 47.17(13) . 2_655 ? C13 Si1 K1 67.99(16) 2_655 2_655 ? C12 Si1 K1 144.87(19) . 2_655 ? N3 Si1 K1 47.83(14) . . ? C13 Si1 K1 118.87(17) 2_655 . ? C12 Si1 K1 136.7(2) . . ? K1 Si1 K1 62.22(3) 2_655 . ? N3 Si2 C14 116.1(2) . . ? N3 Si2 C16 113.9(2) . . ? C14 Si2 C16 105.8(3) . . ? N3 Si2 C15 110.8(2) . . ? C14 Si2 C15 104.3(3) . . ? C16 Si2 C15 104.9(3) . . ? N3 Si2 K1 50.37(14) . . ? C14 Si2 K1 162.8(2) . . ? C16 Si2 K1 90.6(2) . . ? C15 Si2 K1 75.59(17) . . ? N3 Si2 K1 38.66(13) . 2_655 ? C14 Si2 K1 102.3(2) . 2_655 ? C16 Si2 K1 148.6(2) . 2_655 ? C15 Si2 K1 81.09(17) . 2_655 ? K1 Si2 K1 60.56(3) . 2_655 ? C1 N1 C7 105.6(5) . . ? C1 N1 C6 103.2(4) . . ? C7 N1 C6 114.1(5) . . ? C1 N2 C2 118.2(4) . . ? C1 N2 C5 103.6(4) . . ? C2 N2 C5 112.9(4) . . ? C1 N2 K1 100.0(3) . . ? C2 N2 K1 111.5(3) . . ? C5 N2 K1 109.6(3) . . ? Si2 N3 Si1 127.1(2) . . ? Si2 N3 K1 119.38(19) . 2_655 ? Si1 N3 K1 106.68(17) . 2_655 ? Si2 N3 K1 102.80(18) . . ? Si1 N3 K1 106.33(18) . . ? K1 N3 K1 84.43(10) 2_655 . ? C8 O1 C1 105.5(4) . . ? C8 O1 K1 145.9(3) . . ? C1 O1 K1 103.5(2) . . ? N2 C1 N1 112.0(4) . . ? N2 C1 O1 108.2(4) . . ? N1 C1 O1 105.9(4) . . ? N2 C1 H1 110.2 . . ? N1 C1 H1 110.2 . . ? O1 C1 H1 110.2 . . ? N2 C2 C4 110.4(4) . . ? N2 C2 C3 117.0(5) . . ? C4 C2 C3 111.8(4) . . ? N2 C2 H2 105.5 . . ? C4 C2 H2 105.5 . . ? C3 C2 H2 105.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 N2 103.7(5) . . ? C6 C5 H5A 111.0 . . ? N2 C5 H5A 111.0 . . ? C6 C5 H5B 111.0 . . ? N2 C5 H5B 111.0 . . ? H5A C5 H5B 109.0 . . ? N1 C6 C5 99.9(5) . . ? N1 C6 H6A 111.8 . . ? C5 C6 H6A 111.8 . . ? N1 C6 H6B 111.8 . . ? C5 C6 H6B 111.8 . . ? H6A C6 H6B 109.5 . . ? N1 C7 C8 106.4(5) . . ? N1 C7 H7A 110.5 . . ? C8 C7 H7A 110.5 . . ? N1 C7 H7B 110.5 . . ? C8 C7 H7B 110.5 . . ? H7A C7 H7B 108.6 . . ? O1 C8 C9 111.1(5) . . ? O1 C8 C10 106.6(4) . . ? C9 C8 C10 110.2(5) . . ? O1 C8 C7 103.0(4) . . ? C9 C8 C7 113.2(6) . . ? C10 C8 C7 112.4(5) . . ? 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 . . ? K1 C11 H11A 60(4) . . ? K1 C11 H11B 70(4) . . ? H11A C11 H11B 111(5) . . ? K1 C11 H11C 165(4) . . ? H11A C11 H11C 115(6) . . ? H11B C11 H11C 101(5) . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 K1 81.30(17) 2_655 . ? Si1 C13 H13A 109.5 2_655 . ? K1 C13 H13A 45.4 . . ? Si1 C13 H13B 109.5 2_655 . ? K1 C13 H13B 87.1 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 2_655 . ? K1 C13 H13C 154.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 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 N3 K1 Si1 N3 78.1(2) 2_655 . . . ? O1 K1 Si1 N3 -96.87(19) . . . . ? N2 K1 Si1 N3 -150.7(2) . . . . ? C11 K1 Si1 N3 -170.3(3) . . . . ? C13 K1 Si1 N3 27.8(2) . . . . ? Si2 K1 Si1 N3 -25.09(17) . . . . ? Si1 K1 Si1 N3 55.97(18) 2_655 . . . ? K1 K1 Si1 N3 55.97(18) 2_655 . . . ? Si2 K1 Si1 N3 99.55(18) 2_655 . . . ? N3 K1 Si1 C13 -17.1(2) 2_655 . . 2_655 ? O1 K1 Si1 C13 167.9(2) . . . 2_655 ? N3 K1 Si1 C13 -95.2(3) . . . 2_655 ? N2 K1 Si1 C13 114.1(2) . . . 2_655 ? C11 K1 Si1 C13 94.4(3) . . . 2_655 ? C13 K1 Si1 C13 -67.4(3) . . . 2_655 ? Si2 K1 Si1 C13 -120.3(2) . . . 2_655 ? Si1 K1 Si1 C13 -39.3(2) 2_655 . . 2_655 ? K1 K1 Si1 C13 -39.3(2) 2_655 . . 2_655 ? Si2 K1 Si1 C13 4.3(2) 2_655 . . 2_655 ? N3 K1 Si1 C12 164.3(3) 2_655 . . . ? O1 K1 Si1 C12 -10.8(3) . . . . ? N3 K1 Si1 C12 86.1(3) . . . . ? N2 K1 Si1 C12 -64.6(3) . . . . ? C11 K1 Si1 C12 -84.2(3) . . . . ? C13 K1 Si1 C12 113.9(3) . . . . ? Si2 K1 Si1 C12 61.0(3) . . . . ? Si1 K1 Si1 C12 142.1(3) 2_655 . . . ? K1 K1 Si1 C12 142.1(3) 2_655 . . . ? Si2 K1 Si1 C12 -174.3(3) 2_655 . . . ? N3 K1 Si1 K1 22.16(8) 2_655 . . 2_655 ? O1 K1 Si1 K1 -152.85(9) . . . 2_655 ? N3 K1 Si1 K1 -55.97(18) . . . 2_655 ? N2 K1 Si1 K1 153.33(11) . . . 2_655 ? C11 K1 Si1 K1 133.7(2) . . . 2_655 ? C13 K1 Si1 K1 -28.18(14) . . . 2_655 ? Si2 K1 Si1 K1 -81.06(4) . . . 2_655 ? Si1 K1 Si1 K1 0.0 2_655 . . 2_655 ? Si2 K1 Si1 K1 43.58(3) 2_655 . . 2_655 ? N3 K1 Si2 N3 -66.1(2) 2_655 . . . ? O1 K1 Si2 N3 143.09(19) . . . . ? N2 K1 Si2 N3 118.1(2) . . . . ? C11 K1 Si2 N3 41.7(2) . . . . ? C13 K1 Si2 N3 -123.97(19) . . . . ? Si1 K1 Si2 N3 -92.55(18) 2_655 . . . ? Si1 K1 Si2 N3 24.18(17) . . . . ? K1 K1 Si2 N3 -45.82(17) 2_655 . . . ? Si2 K1 Si2 N3 -45.82(17) 2_655 . . . ? N3 K1 Si2 C14 -24.3(7) 2_655 . . . ? O1 K1 Si2 C14 -175.1(6) . . . . ? N3 K1 Si2 C14 41.8(7) . . . . ? N2 K1 Si2 C14 159.9(6) . . . . ? C11 K1 Si2 C14 83.5(7) . . . . ? C13 K1 Si2 C14 -82.2(7) . . . . ? Si1 K1 Si2 C14 -50.8(6) 2_655 . . . ? Si1 K1 Si2 C14 66.0(6) . . . . ? K1 K1 Si2 C14 -4.0(6) 2_655 . . . ? Si2 K1 Si2 C14 -4.0(6) 2_655 . . . ? N3 K1 Si2 C16 172.7(2) 2_655 . . . ? O1 K1 Si2 C16 21.9(2) . . . . ? N3 K1 Si2 C16 -121.1(3) . . . . ? N2 K1 Si2 C16 -3.0(2) . . . . ? C11 K1 Si2 C16 -79.5(2) . . . . ? C13 K1 Si2 C16 114.9(2) . . . . ? Si1 K1 Si2 C16 146.30(19) 2_655 . . . ? Si1 K1 Si2 C16 -96.97(19) . . . . ? K1 K1 Si2 C16 -166.97(19) 2_655 . . . ? Si2 K1 Si2 C16 -166.97(19) 2_655 . . . ? N3 K1 Si2 C15 67.5(2) 2_655 . . . ? O1 K1 Si2 C15 -83.3(2) . . . . ? N3 K1 Si2 C15 133.6(3) . . . . ? N2 K1 Si2 C15 -108.3(2) . . . . ? C11 K1 Si2 C15 175.3(2) . . . . ? C13 K1 Si2 C15 9.6(2) . . . . ? Si1 K1 Si2 C15 41.07(18) 2_655 . . . ? Si1 K1 Si2 C15 157.79(18) . . . . ? K1 K1 Si2 C15 87.79(18) 2_655 . . . ? Si2 K1 Si2 C15 87.79(18) 2_655 . . . ? N3 K1 Si2 K1 -20.31(8) 2_655 . . 2_655 ? O1 K1 Si2 K1 -171.08(9) . . . 2_655 ? N3 K1 Si2 K1 45.82(17) . . . 2_655 ? N2 K1 Si2 K1 163.95(14) . . . 2_655 ? C11 K1 Si2 K1 87.48(11) . . . 2_655 ? C13 K1 Si2 K1 -78.15(9) . . . 2_655 ? Si1 K1 Si2 K1 -46.72(3) 2_655 . . 2_655 ? Si1 K1 Si2 K1 70.00(4) . . . 2_655 ? Si2 K1 Si2 K1 0.0 2_655 . . 2_655 ? N3 K1 N2 C1 -143.0(3) 2_655 . . . ? O1 K1 N2 C1 -2.0(3) . . . . ? N3 K1 N2 C1 72.5(4) . . . . ? C11 K1 N2 C1 102.5(3) . . . . ? C13 K1 N2 C1 -86.4(3) . . . . ? Si2 K1 N2 C1 32.5(4) . . . . ? Si1 K1 N2 C1 -113.7(3) 2_655 . . . ? Si1 K1 N2 C1 92.6(3) . . . . ? K1 K1 N2 C1 172.8(2) 2_655 . . . ? Si2 K1 N2 C1 -161.9(3) 2_655 . . . ? N3 K1 N2 C2 91.2(3) 2_655 . . . ? O1 K1 N2 C2 -127.8(4) . . . . ? N3 K1 N2 C2 -53.3(4) . . . . ? C11 K1 N2 C2 -23.3(3) . . . . ? C13 K1 N2 C2 147.8(3) . . . . ? Si2 K1 N2 C2 -93.3(3) . . . . ? Si1 K1 N2 C2 120.5(3) 2_655 . . . ? Si1 K1 N2 C2 -33.2(4) . . . . ? K1 K1 N2 C2 47.0(5) 2_655 . . . ? Si2 K1 N2 C2 72.3(3) 2_655 . . . ? N3 K1 N2 C5 -34.6(4) 2_655 . . . ? O1 K1 N2 C5 106.4(4) . . . . ? N3 K1 N2 C5 -179.1(3) . . . . ? C11 K1 N2 C5 -149.1(3) . . . . ? C13 K1 N2 C5 22.0(3) . . . . ? Si2 K1 N2 C5 140.9(3) . . . . ? Si1 K1 N2 C5 -5.3(4) 2_655 . . . ? Si1 K1 N2 C5 -159.0(3) . . . . ? K1 K1 N2 C5 -78.8(4) 2_655 . . . ? Si2 K1 N2 C5 -53.5(3) 2_655 . . . ? C14 Si2 N3 Si1 70.4(4) . . . . ? C16 Si2 N3 Si1 -52.8(4) . . . . ? C15 Si2 N3 Si1 -170.9(3) . . . . ? K1 Si2 N3 Si1 -122.2(4) . . . . ? K1 Si2 N3 Si1 147.0(4) 2_655 . . . ? C14 Si2 N3 K1 -76.6(3) . . . 2_655 ? C16 Si2 N3 K1 160.2(2) . . . 2_655 ? C15 Si2 N3 K1 42.2(3) . . . 2_655 ? K1 Si2 N3 K1 90.79(19) . . . 2_655 ? C14 Si2 N3 K1 -167.4(2) . . . . ? C16 Si2 N3 K1 69.4(3) . . . . ? C15 Si2 N3 K1 -48.6(2) . . . . ? K1 Si2 N3 K1 -90.79(19) 2_655 . . . ? C13 Si1 N3 Si2 -130.0(3) 2_655 . . . ? C12 Si1 N3 Si2 -9.1(4) . . . . ? K1 Si1 N3 Si2 -150.3(4) 2_655 . . . ? K1 Si1 N3 Si2 120.7(4) . . . . ? C13 Si1 N3 K1 20.3(3) 2_655 . . 2_655 ? C12 Si1 N3 K1 141.2(2) . . . 2_655 ? K1 Si1 N3 K1 -88.98(16) . . . 2_655 ? C13 Si1 N3 K1 109.2(2) 2_655 . . . ? C12 Si1 N3 K1 -129.9(2) . . . . ? K1 Si1 N3 K1 88.98(16) 2_655 . . . ? N3 K1 N3 Si2 118.9(2) 2_655 . . . ? O1 K1 N3 Si2 -40.9(2) . . . . ? N2 K1 N3 Si2 -92.4(2) . . . . ? C11 K1 N3 Si2 -129.4(2) . . . . ? C13 K1 N3 Si2 64.3(2) . . . . ? Si1 K1 N3 Si2 93.18(16) 2_655 . . . ? Si1 K1 N3 Si2 -135.3(3) . . . . ? K1 K1 N3 Si2 118.9(2) 2_655 . . . ? Si2 K1 N3 Si2 140.71(14) 2_655 . . . ? N3 K1 N3 Si1 -105.78(19) 2_655 . . . ? O1 K1 N3 Si1 94.44(18) . . . . ? N2 K1 N3 Si1 42.9(3) . . . . ? C11 K1 N3 Si1 5.90(17) . . . . ? C13 K1 N3 Si1 -160.42(16) . . . . ? Si2 K1 N3 Si1 135.3(3) . . . . ? Si1 K1 N3 Si1 -131.50(15) 2_655 . . . ? K1 K1 N3 Si1 -105.78(19) 2_655 . . . ? Si2 K1 N3 Si1 -83.97(16) 2_655 . . . ? N3 K1 N3 K1 0.0 2_655 . . 2_655 ? O1 K1 N3 K1 -159.78(10) . . . 2_655 ? N2 K1 N3 K1 148.65(16) . . . 2_655 ? C11 K1 N3 K1 111.68(16) . . . 2_655 ? C13 K1 N3 K1 -54.64(14) . . . 2_655 ? Si2 K1 N3 K1 -118.9(2) . . . 2_655 ? Si1 K1 N3 K1 -25.72(9) 2_655 . . 2_655 ? Si1 K1 N3 K1 105.78(19) . . . 2_655 ? Si2 K1 N3 K1 21.81(8) 2_655 . . 2_655 ? N3 K1 O1 C8 -68.3(6) 2_655 . . . ? N3 K1 O1 C8 75.0(6) . . . . ? N2 K1 O1 C8 -145.6(6) . . . . ? C11 K1 O1 C8 133.1(6) . . . . ? C13 K1 O1 C8 -44.7(6) . . . . ? Si2 K1 O1 C8 57.8(6) . . . . ? Si1 K1 O1 C8 -48.1(6) 2_655 . . . ? Si1 K1 O1 C8 103.2(6) . . . . ? K1 K1 O1 C8 39.1(7) 2_655 . . . ? Si2 K1 O1 C8 -107.9(6) 2_655 . . . ? N3 K1 O1 C1 79.1(3) 2_655 . . . ? N3 K1 O1 C1 -137.5(3) . . . . ? N2 K1 O1 C1 1.9(3) . . . . ? C11 K1 O1 C1 -79.5(3) . . . . ? C13 K1 O1 C1 102.8(3) . . . . ? Si2 K1 O1 C1 -154.7(3) . . . . ? Si1 K1 O1 C1 99.4(3) 2_655 . . . ? Si1 K1 O1 C1 -109.4(3) . . . . ? K1 K1 O1 C1 -173.4(2) 2_655 . . . ? Si2 K1 O1 C1 39.6(4) 2_655 . . . ? C2 N2 C1 N1 -119.6(5) . . . . ? C5 N2 C1 N1 6.1(5) . . . . ? K1 N2 C1 N1 119.3(4) . . . . ? C2 N2 C1 O1 124.0(5) . . . . ? C5 N2 C1 O1 -110.2(5) . . . . ? K1 N2 C1 O1 2.9(4) . . . . ? C7 N1 C1 N2 -150.6(5) . . . . ? C6 N1 C1 N2 -30.6(5) . . . . ? C7 N1 C1 O1 -32.9(6) . . . . ? C6 N1 C1 O1 87.2(5) . . . . ? C8 O1 C1 N2 158.7(4) . . . . ? K1 O1 C1 N2 -3.1(4) . . . . ? C8 O1 C1 N1 38.4(5) . . . . ? K1 O1 C1 N1 -123.3(3) . . . . ? C1 N2 C2 C4 -174.4(5) . . . . ? C5 N2 C2 C4 64.5(6) . . . . ? K1 N2 C2 C4 -59.4(5) . . . . ? C1 N2 C2 C3 56.1(7) . . . . ? C5 N2 C2 C3 -64.9(6) . . . . ? K1 N2 C2 C3 171.1(4) . . . . ? C1 N2 C5 C6 20.3(6) . . . . ? C2 N2 C5 C6 149.4(5) . . . . ? K1 N2 C5 C6 -85.6(5) . . . . ? C1 N1 C6 C5 40.8(5) . . . . ? C7 N1 C6 C5 154.9(5) . . . . ? N2 C5 C6 N1 -37.2(6) . . . . ? C1 N1 C7 C8 15.8(7) . . . . ? C6 N1 C7 C8 -96.9(6) . . . . ? C1 O1 C8 C9 94.8(6) . . . . ? K1 O1 C8 C9 -118.1(6) . . . . ? C1 O1 C8 C10 -145.1(5) . . . . ? K1 O1 C8 C10 2.0(9) . . . . ? C1 O1 C8 C7 -26.7(6) . . . . ? K1 O1 C8 C7 120.5(6) . . . . ? N1 C7 C8 O1 7.3(7) . . . . ? N1 C7 C8 C9 -112.7(6) . . . . ? N1 C7 C8 C10 121.6(6) . . . . ? N3 K1 C13 Si1 -10.58(14) 2_655 . . 2_655 ? O1 K1 C13 Si1 -174.38(18) . . . 2_655 ? N3 K1 C13 Si1 68.0(2) . . . 2_655 ? N2 K1 C13 Si1 -126.42(18) . . . 2_655 ? C11 K1 C13 Si1 14.7(7) . . . 2_655 ? Si2 K1 C13 Si1 92.55(17) . . . 2_655 ? Si1 K1 C13 Si1 54.9(3) . . . 2_655 ? K1 K1 C13 Si1 31.12(16) 2_655 . . 2_655 ? Si2 K1 C13 Si1 -24.85(14) 2_655 . . 2_655 ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.108 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.095 # Attachment 'paed5 ZnLm2.cif' data_paed5 _database_code_depnum_ccdc_archive 'CCDC 727061' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H46 N4 O2 Zn' _chemical_formula_sum 'C32 H46 N4 O2 Zn' _chemical_formula_weight 584.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' 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 45.089(4) _cell_length_b 11.2093(9) _cell_length_c 12.7221(11) _cell_angle_alpha 90.00 _cell_angle_beta 104.578(2) _cell_angle_gamma 90.00 _cell_volume 6222.9(9) _cell_formula_units_Z 8 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 5107 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 25.35 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 0.823 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.952 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(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 'SCXMini detector' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 19344 _diffrn_reflns_av_R_equivalents 0.1343 _diffrn_reflns_av_sigmaI/netI 0.0988 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4017 _reflns_number_gt 2934 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SCX-mini (Rigaku Inc., 2007)' _computing_cell_refinement 'SCX-mini (Rigaku Inc., 2007)' _computing_data_reduction 'SCX-mini (Rigaku Inc., 2007)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _refine_special_details ; Due to difficulties with the quality of the data collected; the structure was modelled using DELU and SIMU restraints and the disagreeable reflection 26 0 0 was omitted. ; _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^)+(0.0523P)^2^+12.6593P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4017 _refine_ls_number_parameters 352 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1087 _refine_ls_R_factor_gt 0.0711 _refine_ls_wR_factor_ref 0.1429 _refine_ls_wR_factor_gt 0.1299 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.030 _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 C1 C 0.86551(14) 0.1155(5) -0.0360(4) 0.0133(16) Uani 1 1 d . . . C5 C 0.84325(13) -0.0730(4) -0.0806(4) 0.0191(16) Uani 1 1 d . . . H5A H 0.8415 -0.1001 -0.1559 0.023 Uiso 1 1 calc R . . H5B H 0.8283 -0.1168 -0.0501 0.023 Uiso 1 1 calc R . . C6 C 0.87563(14) -0.0876(5) -0.0104(4) 0.0204(16) Uani 1 1 d . . . H6A H 0.8756 -0.1205 0.0618 0.024 Uiso 1 1 calc R . . H6B H 0.8879 -0.1403 -0.0457 0.024 Uiso 1 1 calc R . . C7 C 0.91865(14) 0.0664(5) 0.0549(4) 0.0177(17) Uani 1 1 d . . . H7A H 0.9284 0.1076 0.0033 0.021 Uiso 1 1 calc R . . H7B H 0.9301 -0.0085 0.0773 0.021 Uiso 1 1 calc R . . C8 C 0.92198(14) 0.1470(5) 0.1571(4) 0.0173(16) Uani 1 1 d . . . C9 C 0.90507(15) 0.0896(5) 0.2350(5) 0.0321(18) Uani 1 1 d . . . H9A H 0.9078 0.1390 0.3003 0.048 Uiso 1 1 calc R . . H9B H 0.9134 0.0098 0.2554 0.048 Uiso 1 1 calc R . . H9C H 0.8832 0.0834 0.1990 0.048 Uiso 1 1 calc R . . C10 C 0.95643(14) 0.1546(5) 0.2113(5) 0.0276(18) Uani 1 1 d . . . H10A H 0.9673 0.1841 0.1587 0.041 Uiso 1 1 calc R . . H10B H 0.9642 0.0752 0.2366 0.041 Uiso 1 1 calc R . . H10C H 0.9599 0.2093 0.2733 0.041 Uiso 1 1 calc R . . C11 C 0.88626(18) 0.4118(5) -0.1019(4) 0.0172(18) Uani 1 1 d . . . C15 C 0.90859(17) 0.5586(5) -0.1888(5) 0.031(2) Uani 1 1 d . . . H15A H 0.9116 0.5415 -0.2618 0.038 Uiso 1 1 calc R . . H15B H 0.9230 0.6219 -0.1539 0.038 Uiso 1 1 calc R . . C16 C 0.87554(16) 0.5933(5) -0.1948(4) 0.0212(18) Uani 1 1 d . . . H16A H 0.8745 0.6668 -0.1526 0.025 Uiso 1 1 calc R . . H16B H 0.8637 0.6056 -0.2709 0.025 Uiso 1 1 calc R . . C17 C 0.83318(17) 0.4800(5) -0.1339(4) 0.0197(14) Uiso 1 1 d U . . H17A H 0.8240 0.4053 -0.1692 0.024 Uiso 1 1 calc R . . H17B H 0.8210 0.5472 -0.1732 0.024 Uiso 1 1 calc R . . C18 C 0.83022(16) 0.4805(5) -0.0149(5) 0.0208(16) Uani 1 1 d U . . C19 C 0.84641(15) 0.5928(5) 0.0421(5) 0.0321(18) Uani 1 1 d U . . H19A H 0.8449 0.5943 0.1176 0.048 Uiso 1 1 calc R . . H19B H 0.8366 0.6642 0.0042 0.048 Uiso 1 1 calc R . . H19C H 0.8680 0.5913 0.0408 0.048 Uiso 1 1 calc R . . C20 C 0.79640(17) 0.4826(6) -0.0174(5) 0.0379(19) Uani 1 1 d U . . H20A H 0.7863 0.4121 -0.0561 0.057 Uiso 1 1 calc R . . H20B H 0.7870 0.5548 -0.0549 0.057 Uiso 1 1 calc R . . H20C H 0.7940 0.4824 0.0571 0.057 Uiso 1 1 calc R . . C21 C 0.81074(16) 0.1151(5) -0.1325(4) 0.0164(17) Uani 1 1 d . . . C22 C 0.78658(17) 0.1236(5) -0.0835(5) 0.0202(17) Uani 1 1 d . . . C23 C 0.75973(16) 0.1778(5) -0.1412(5) 0.0280(18) Uani 1 1 d . . . H23 H 0.7429 0.1831 -0.1091 0.034 Uiso 1 1 calc R . . C24 C 0.75672(17) 0.2245(5) -0.2442(5) 0.0272(19) Uani 1 1 d . . . C25 C 0.78157(18) 0.2144(5) -0.2910(5) 0.0277(19) Uani 1 1 d . . . H25 H 0.7797 0.2455 -0.3619 0.033 Uiso 1 1 calc R . . C26 C 0.80871(15) 0.1603(5) -0.2371(4) 0.0178(17) Uani 1 1 d . . . C31 C 0.94017(15) 0.3805(5) -0.0978(4) 0.0183(17) Uani 1 1 d . . . C32 C 0.96287(15) 0.4000(5) -0.0020(4) 0.0224(17) Uani 1 1 d . . . C33 C 0.98939(15) 0.3318(5) 0.0174(5) 0.0251(17) Uani 1 1 d . . . H33 H 1.0049 0.3448 0.0824 0.030 Uiso 1 1 calc R . . C34 C 0.99404(15) 0.2452(5) -0.0552(5) 0.0240(17) Uani 1 1 d . . . C35 C 0.97086(15) 0.2286(5) -0.1497(5) 0.0258(18) Uani 1 1 d . . . H35 H 0.9734 0.1688 -0.1995 0.031 Uiso 1 1 calc R . . C36 C 0.94423(15) 0.2960(5) -0.1740(4) 0.0218(16) Uani 1 1 d . . . C220 C 0.78978(16) 0.0792(6) 0.0314(5) 0.045(2) Uani 1 1 d . . . H22A H 0.7918 -0.0079 0.0330 0.067 Uiso 1 1 calc R . . H22B H 0.7716 0.1021 0.0557 0.067 Uiso 1 1 calc R . . H22C H 0.8080 0.1147 0.0798 0.067 Uiso 1 1 calc R . . C240 C 0.72772(15) 0.2896(6) -0.3030(5) 0.046(2) Uani 1 1 d . . . H24A H 0.7102 0.2567 -0.2805 0.069 Uiso 1 1 calc R . . H24B H 0.7245 0.2795 -0.3816 0.069 Uiso 1 1 calc R . . H24C H 0.7298 0.3747 -0.2850 0.069 Uiso 1 1 calc R . . C260 C 0.83487(15) 0.1516(5) -0.2880(4) 0.0259(18) Uani 1 1 d . . . H26A H 0.8518 0.2017 -0.2479 0.039 Uiso 1 1 calc R . . H26B H 0.8284 0.1790 -0.3635 0.039 Uiso 1 1 calc R . . H26C H 0.8417 0.0686 -0.2863 0.039 Uiso 1 1 calc R . . C320 C 0.95761(16) 0.4869(5) 0.0820(5) 0.0334(19) Uani 1 1 d . . . H32A H 0.9441 0.4505 0.1225 0.050 Uiso 1 1 calc R . . H32B H 0.9480 0.5594 0.0458 0.050 Uiso 1 1 calc R . . H32C H 0.9773 0.5072 0.1321 0.050 Uiso 1 1 calc R . . C340 C 1.02267(15) 0.1701(6) -0.0311(5) 0.038(2) Uani 1 1 d . . . H34A H 1.0242 0.1248 0.0359 0.057 Uiso 1 1 calc R . . H34B H 1.0406 0.2219 -0.0223 0.057 Uiso 1 1 calc R . . H34C H 1.0218 0.1147 -0.0913 0.057 Uiso 1 1 calc R . . C360 C 0.91974(15) 0.2724(5) -0.2760(5) 0.0312(18) Uani 1 1 d . . . H36A H 0.9165 0.3441 -0.3215 0.047 Uiso 1 1 calc R . . H36B H 0.9006 0.2512 -0.2573 0.047 Uiso 1 1 calc R . . H36C H 0.9261 0.2064 -0.3159 0.047 Uiso 1 1 calc R . . N1 N 0.88747(11) 0.0363(4) -0.0015(3) 0.0132(13) Uani 1 1 d . . . N2 N 0.83903(12) 0.0592(4) -0.0754(3) 0.0137(13) Uani 1 1 d . . . N3 N 0.86413(12) 0.4895(4) -0.1462(3) 0.0178(14) Uani 1 1 d U . . N4 N 0.91230(15) 0.4493(4) -0.1207(4) 0.0206(16) Uani 1 1 d . . . O1 O 0.91068(9) 0.2604(3) 0.1290(3) 0.0234(11) Uani 1 1 d . . . O2 O 0.84343(9) 0.3792(3) 0.0417(3) 0.0211(11) Uani 1 1 d U . . Zn1 Zn 0.876299(17) 0.29101(5) 0.00533(5) 0.0167(3) 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 C1 0.007(5) 0.021(3) 0.009(3) -0.002(2) -0.003(3) 0.002(3) C5 0.018(5) 0.010(3) 0.027(3) -0.003(2) 0.000(3) -0.002(3) C6 0.019(5) 0.022(3) 0.019(3) -0.004(3) 0.003(3) -0.003(3) C7 0.012(5) 0.018(3) 0.024(3) 0.003(3) 0.007(3) 0.004(3) C8 0.014(5) 0.016(3) 0.019(3) 0.002(2) -0.002(3) -0.002(3) C9 0.036(5) 0.034(4) 0.025(3) 0.002(3) 0.006(3) -0.007(3) C10 0.027(6) 0.027(3) 0.027(3) -0.004(3) 0.004(3) -0.003(3) C11 0.010(6) 0.021(3) 0.021(3) 0.000(3) 0.003(3) -0.002(3) C15 0.038(7) 0.025(4) 0.040(4) 0.015(3) 0.025(4) 0.004(4) C16 0.030(6) 0.017(3) 0.021(3) 0.002(2) 0.015(3) -0.002(3) C18 0.017(5) 0.013(3) 0.034(3) -0.001(3) 0.010(3) 0.010(3) C19 0.051(5) 0.021(3) 0.025(3) -0.001(3) 0.009(3) 0.000(3) C20 0.028(5) 0.034(4) 0.056(4) 0.013(3) 0.020(4) 0.015(3) C21 0.008(6) 0.016(3) 0.020(3) -0.005(3) -0.006(3) -0.006(3) C22 0.007(6) 0.019(3) 0.036(4) 0.003(3) 0.009(4) 0.006(3) C23 0.012(6) 0.030(4) 0.043(4) -0.003(3) 0.009(3) 0.002(3) C24 0.023(6) 0.015(3) 0.035(4) -0.002(3) -0.008(4) 0.003(3) C25 0.031(7) 0.020(3) 0.028(4) 0.000(3) -0.002(4) -0.002(3) C26 0.010(6) 0.017(3) 0.025(3) 0.000(3) 0.000(3) -0.001(3) C31 0.015(6) 0.020(3) 0.024(3) 0.006(3) 0.012(3) -0.002(3) C32 0.023(6) 0.026(4) 0.021(3) 0.005(3) 0.011(3) 0.003(3) C33 0.012(6) 0.038(4) 0.024(3) 0.007(3) 0.003(3) -0.001(3) C34 0.018(5) 0.027(3) 0.031(4) -0.001(3) 0.015(3) 0.004(3) C35 0.030(6) 0.021(4) 0.030(4) -0.006(3) 0.014(3) -0.003(3) C36 0.021(5) 0.020(3) 0.027(3) 0.002(3) 0.011(3) 0.000(3) C220 0.041(6) 0.061(5) 0.036(4) 0.016(4) 0.016(4) 0.017(4) C240 0.035(6) 0.036(4) 0.054(4) 0.003(4) -0.013(4) 0.007(4) C260 0.026(6) 0.029(4) 0.024(3) 0.004(3) 0.007(3) -0.002(3) C320 0.041(6) 0.030(4) 0.032(4) -0.007(3) 0.014(3) -0.006(3) C340 0.031(6) 0.047(4) 0.037(4) 0.006(3) 0.010(3) 0.015(4) C360 0.019(5) 0.035(4) 0.039(4) -0.002(3) 0.007(3) -0.004(3) N1 0.007(4) 0.009(2) 0.023(3) 0.000(2) 0.001(2) -0.003(2) N2 0.005(4) 0.013(2) 0.022(3) 0.001(2) 0.003(2) 0.004(2) N3 0.012(5) 0.018(3) 0.024(3) 0.002(2) 0.006(2) 0.001(3) N4 0.019(6) 0.016(3) 0.030(3) 0.005(2) 0.014(3) 0.001(3) O1 0.025(3) 0.015(2) 0.027(2) -0.0029(17) 0.0004(19) 0.0012(19) O2 0.019(3) 0.022(2) 0.026(2) 0.0052(17) 0.0118(19) 0.0060(19) Zn1 0.0197(6) 0.0121(3) 0.0181(3) 0.0002(3) 0.0043(3) -0.0004(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.320(7) . ? C1 N2 1.332(7) . ? C1 Zn1 2.063(5) . ? C5 N2 1.497(6) . ? C5 C6 1.516(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N1 1.482(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N1 1.448(7) . ? C7 C8 1.559(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O1 1.382(6) . ? C8 C10 1.535(8) . ? C8 C9 1.536(8) . ? 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 N4 1.324(7) . ? C11 N3 1.338(7) . ? C11 Zn1 2.051(6) . ? C15 N4 1.486(7) . ? C15 C16 1.524(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N3 1.469(7) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 N3 1.447(7) . ? C17 C18 1.553(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O2 1.395(6) . ? C18 C20 1.517(9) . ? C18 C19 1.542(8) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.388(8) . ? C21 C26 1.405(8) . ? C21 N2 1.442(7) . ? C22 C23 1.388(8) . ? C22 C220 1.517(8) . ? C23 C24 1.385(8) . ? C23 H23 0.9500 . ? C24 C25 1.400(9) . ? C24 C240 1.520(8) . ? C25 C26 1.383(8) . ? C25 H25 0.9500 . ? C26 C260 1.485(8) . ? C31 C32 1.397(8) . ? C31 C36 1.400(8) . ? C31 N4 1.440(7) . ? C32 C33 1.388(8) . ? C32 C320 1.508(8) . ? C33 C34 1.391(8) . ? C33 H33 0.9500 . ? C34 C35 1.393(8) . ? C34 C340 1.507(8) . ? C35 C36 1.386(8) . ? C35 H35 0.9500 . ? C36 C360 1.501(8) . ? C220 H22A 0.9800 . ? C220 H22B 0.9800 . ? C220 H22C 0.9800 . ? C240 H24A 0.9800 . ? C240 H24B 0.9800 . ? C240 H24C 0.9800 . ? C260 H26A 0.9800 . ? C260 H26B 0.9800 . ? C260 H26C 0.9800 . ? C320 H32A 0.9800 . ? C320 H32B 0.9800 . ? C320 H32C 0.9800 . ? C340 H34A 0.9800 . ? C340 H34B 0.9800 . ? C340 H34C 0.9800 . ? C360 H36A 0.9800 . ? C360 H36B 0.9800 . ? C360 H36C 0.9800 . ? O1 Zn1 1.941(4) . ? O2 Zn1 1.932(4) . ? 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 C1 N2 109.5(5) . . ? N1 C1 Zn1 116.6(4) . . ? N2 C1 Zn1 132.8(4) . . ? N2 C5 C6 101.3(4) . . ? N2 C5 H5A 111.5 . . ? C6 C5 H5A 111.5 . . ? N2 C5 H5B 111.5 . . ? C6 C5 H5B 111.5 . . ? H5A C5 H5B 109.3 . . ? N1 C6 C5 102.6(4) . . ? N1 C6 H6A 111.2 . . ? C5 C6 H6A 111.2 . . ? N1 C6 H6B 111.2 . . ? C5 C6 H6B 111.2 . . ? H6A C6 H6B 109.2 . . ? N1 C7 C8 115.2(5) . . ? N1 C7 H7A 108.5 . . ? C8 C7 H7A 108.5 . . ? N1 C7 H7B 108.5 . . ? C8 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? O1 C8 C10 109.3(5) . . ? O1 C8 C9 110.0(5) . . ? C10 C8 C9 110.1(5) . . ? O1 C8 C7 111.4(4) . . ? C10 C8 C7 106.3(5) . . ? C9 C8 C7 109.7(5) . . ? 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 . . ? N4 C11 N3 108.6(6) . . ? N4 C11 Zn1 133.0(5) . . ? N3 C11 Zn1 116.4(5) . . ? N4 C15 C16 101.8(5) . . ? N4 C15 H15A 111.4 . . ? C16 C15 H15A 111.4 . . ? N4 C15 H15B 111.4 . . ? C16 C15 H15B 111.4 . . ? H15A C15 H15B 109.3 . . ? N3 C16 C15 102.6(5) . . ? N3 C16 H16A 111.2 . . ? C15 C16 H16A 111.2 . . ? N3 C16 H16B 111.2 . . ? C15 C16 H16B 111.2 . . ? H16A C16 H16B 109.2 . . ? N3 C17 C18 115.3(5) . . ? N3 C17 H17A 108.5 . . ? C18 C17 H17A 108.5 . . ? N3 C17 H17B 108.5 . . ? C18 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? O2 C18 C20 108.7(5) . . ? O2 C18 C19 109.4(5) . . ? C20 C18 C19 110.5(5) . . ? O2 C18 C17 111.7(5) . . ? C20 C18 C17 108.2(5) . . ? C19 C18 C17 108.4(5) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 121.9(6) . . ? C22 C21 N2 119.9(5) . . ? C26 C21 N2 118.2(6) . . ? C21 C22 C23 118.1(6) . . ? C21 C22 C220 121.0(6) . . ? C23 C22 C220 120.8(6) . . ? C24 C23 C22 122.0(7) . . ? C24 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C23 C24 C25 118.3(6) . . ? C23 C24 C240 121.0(7) . . ? C25 C24 C240 120.7(6) . . ? C26 C25 C24 121.8(6) . . ? C26 C25 H25 119.1 . . ? C24 C25 H25 119.1 . . ? C25 C26 C21 117.8(6) . . ? C25 C26 C260 120.9(6) . . ? C21 C26 C260 121.3(6) . . ? C32 C31 C36 121.0(6) . . ? C32 C31 N4 120.3(5) . . ? C36 C31 N4 118.7(5) . . ? C33 C32 C31 118.6(5) . . ? C33 C32 C320 120.8(5) . . ? C31 C32 C320 120.5(6) . . ? C32 C33 C34 122.2(6) . . ? C32 C33 H33 118.9 . . ? C34 C33 H33 118.9 . . ? C33 C34 C35 117.4(6) . . ? C33 C34 C340 121.3(6) . . ? C35 C34 C340 121.3(6) . . ? C36 C35 C34 122.6(6) . . ? C36 C35 H35 118.7 . . ? C34 C35 H35 118.7 . . ? C35 C36 C31 118.1(5) . . ? C35 C36 C360 120.3(5) . . ? C31 C36 C360 121.5(6) . . ? C22 C220 H22A 109.5 . . ? C22 C220 H22B 109.5 . . ? H22A C220 H22B 109.5 . . ? C22 C220 H22C 109.5 . . ? H22A C220 H22C 109.5 . . ? H22B C220 H22C 109.5 . . ? C24 C240 H24A 109.5 . . ? C24 C240 H24B 109.5 . . ? H24A C240 H24B 109.5 . . ? C24 C240 H24C 109.5 . . ? H24A C240 H24C 109.5 . . ? H24B C240 H24C 109.5 . . ? C26 C260 H26A 109.5 . . ? C26 C260 H26B 109.5 . . ? H26A C260 H26B 109.5 . . ? C26 C260 H26C 109.5 . . ? H26A C260 H26C 109.5 . . ? H26B C260 H26C 109.5 . . ? C32 C320 H32A 109.5 . . ? C32 C320 H32B 109.5 . . ? H32A C320 H32B 109.5 . . ? C32 C320 H32C 109.5 . . ? H32A C320 H32C 109.5 . . ? H32B C320 H32C 109.5 . . ? C34 C340 H34A 109.5 . . ? C34 C340 H34B 109.5 . . ? H34A C340 H34B 109.5 . . ? C34 C340 H34C 109.5 . . ? H34A C340 H34C 109.5 . . ? H34B C340 H34C 109.5 . . ? C36 C360 H36A 109.5 . . ? C36 C360 H36B 109.5 . . ? H36A C360 H36B 109.5 . . ? C36 C360 H36C 109.5 . . ? H36A C360 H36C 109.5 . . ? H36B C360 H36C 109.5 . . ? C1 N1 C7 124.1(4) . . ? C1 N1 C6 112.3(5) . . ? C7 N1 C6 122.9(4) . . ? C1 N2 C21 125.4(5) . . ? C1 N2 C5 111.9(4) . . ? C21 N2 C5 120.9(4) . . ? C11 N3 C17 123.0(5) . . ? C11 N3 C16 112.9(5) . . ? C17 N3 C16 123.6(5) . . ? C11 N4 C31 124.2(5) . . ? C11 N4 C15 113.1(5) . . ? C31 N4 C15 121.6(6) . . ? C8 O1 Zn1 122.7(3) . . ? C18 O2 Zn1 123.1(4) . . ? O2 Zn1 O1 113.65(16) . . ? O2 Zn1 C11 97.5(2) . . ? O1 Zn1 C11 113.1(2) . . ? O2 Zn1 C1 113.8(2) . . ? O1 Zn1 C1 97.27(18) . . ? C11 Zn1 C1 122.5(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 C5 C6 N1 -14.6(5) . . . . ? N1 C7 C8 O1 -67.9(6) . . . . ? N1 C7 C8 C10 173.1(4) . . . . ? N1 C7 C8 C9 54.1(6) . . . . ? N4 C15 C16 N3 -9.2(5) . . . . ? N3 C17 C18 O2 -66.1(6) . . . . ? N3 C17 C18 C20 174.3(4) . . . . ? N3 C17 C18 C19 54.4(6) . . . . ? C26 C21 C22 C23 0.6(8) . . . . ? N2 C21 C22 C23 -179.9(5) . . . . ? C26 C21 C22 C220 -177.2(5) . . . . ? N2 C21 C22 C220 2.3(8) . . . . ? C21 C22 C23 C24 -1.1(8) . . . . ? C220 C22 C23 C24 176.8(6) . . . . ? C22 C23 C24 C25 1.0(9) . . . . ? C22 C23 C24 C240 -176.5(5) . . . . ? C23 C24 C25 C26 -0.5(8) . . . . ? C240 C24 C25 C26 177.0(5) . . . . ? C24 C25 C26 C21 0.0(8) . . . . ? C24 C25 C26 C260 -179.4(5) . . . . ? C22 C21 C26 C25 -0.1(8) . . . . ? N2 C21 C26 C25 -179.6(5) . . . . ? C22 C21 C26 C260 179.3(5) . . . . ? N2 C21 C26 C260 -0.2(7) . . . . ? C36 C31 C32 C33 -1.4(9) . . . . ? N4 C31 C32 C33 179.9(5) . . . . ? C36 C31 C32 C320 -177.0(5) . . . . ? N4 C31 C32 C320 4.3(8) . . . . ? C31 C32 C33 C34 0.0(9) . . . . ? C320 C32 C33 C34 175.6(5) . . . . ? C32 C33 C34 C35 0.1(9) . . . . ? C32 C33 C34 C340 -178.4(6) . . . . ? C33 C34 C35 C36 1.3(9) . . . . ? C340 C34 C35 C36 179.8(6) . . . . ? C34 C35 C36 C31 -2.7(9) . . . . ? C34 C35 C36 C360 -178.7(6) . . . . ? C32 C31 C36 C35 2.7(9) . . . . ? N4 C31 C36 C35 -178.6(5) . . . . ? C32 C31 C36 C360 178.6(5) . . . . ? N4 C31 C36 C360 -2.6(8) . . . . ? N2 C1 N1 C7 -174.3(5) . . . . ? Zn1 C1 N1 C7 -5.0(7) . . . . ? N2 C1 N1 C6 -3.9(6) . . . . ? Zn1 C1 N1 C6 165.5(3) . . . . ? C8 C7 N1 C1 53.5(7) . . . . ? C8 C7 N1 C6 -115.9(5) . . . . ? C5 C6 N1 C1 12.4(6) . . . . ? C5 C6 N1 C7 -177.0(5) . . . . ? N1 C1 N2 C21 -171.8(5) . . . . ? Zn1 C1 N2 C21 21.3(8) . . . . ? N1 C1 N2 C5 -6.9(6) . . . . ? Zn1 C1 N2 C5 -173.9(4) . . . . ? C22 C21 N2 C1 -109.8(6) . . . . ? C26 C21 N2 C1 69.7(7) . . . . ? C22 C21 N2 C5 86.6(6) . . . . ? C26 C21 N2 C5 -93.9(6) . . . . ? C6 C5 N2 C1 14.0(6) . . . . ? C6 C5 N2 C21 179.7(5) . . . . ? N4 C11 N3 C17 -175.4(4) . . . . ? Zn1 C11 N3 C17 -9.2(6) . . . . ? N4 C11 N3 C16 -3.5(6) . . . . ? Zn1 C11 N3 C16 162.7(3) . . . . ? C18 C17 N3 C11 57.9(6) . . . . ? C18 C17 N3 C16 -113.1(5) . . . . ? C15 C16 N3 C11 8.4(6) . . . . ? C15 C16 N3 C17 -179.7(5) . . . . ? N3 C11 N4 C31 -171.4(5) . . . . ? Zn1 C11 N4 C31 25.5(8) . . . . ? N3 C11 N4 C15 -3.3(6) . . . . ? Zn1 C11 N4 C15 -166.4(4) . . . . ? C32 C31 N4 C11 -97.8(7) . . . . ? C36 C31 N4 C11 83.5(7) . . . . ? C32 C31 N4 C15 95.1(7) . . . . ? C36 C31 N4 C15 -83.6(7) . . . . ? C16 C15 N4 C11 8.2(6) . . . . ? C16 C15 N4 C31 176.7(5) . . . . ? C10 C8 O1 Zn1 149.9(4) . . . . ? C9 C8 O1 Zn1 -89.1(5) . . . . ? C7 C8 O1 Zn1 32.7(6) . . . . ? C20 C18 O2 Zn1 145.7(4) . . . . ? C19 C18 O2 Zn1 -93.5(5) . . . . ? C17 C18 O2 Zn1 26.4(7) . . . . ? C18 O2 Zn1 O1 130.0(4) . . . . ? C18 O2 Zn1 C11 10.7(4) . . . . ? C18 O2 Zn1 C1 -119.9(4) . . . . ? C8 O1 Zn1 O2 125.4(4) . . . . ? C8 O1 Zn1 C11 -124.6(4) . . . . ? C8 O1 Zn1 C1 5.4(5) . . . . ? N4 C11 Zn1 O2 140.7(5) . . . . ? N3 C11 Zn1 O2 -21.4(4) . . . . ? N4 C11 Zn1 O1 20.9(6) . . . . ? N3 C11 Zn1 O1 -141.1(4) . . . . ? N4 C11 Zn1 C1 -94.8(6) . . . . ? N3 C11 Zn1 C1 103.1(4) . . . . ? N1 C1 Zn1 O2 -141.6(4) . . . . ? N2 C1 Zn1 O2 24.7(6) . . . . ? N1 C1 Zn1 O1 -21.7(4) . . . . ? N2 C1 Zn1 O1 144.5(5) . . . . ? N1 C1 Zn1 C11 101.7(5) . . . . ? N2 C1 Zn1 C11 -92.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.704 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.711 _refine_diff_density_max 0.564 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.078