# 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 'Antonio Otero' _publ_contact_author_email ANTONIO.OTERO@UCLM.ES _publ_section_title ; Synthesis, structures and ring-opening polymerization studies of new zinc chloride and amide complexes supported by amidinate heteroscorpionate ligands ; loop_ _publ_author_name 'Antonio Otero' 'Carlos Alonso-Moreno' 'Mariano Fajardo' 'Juan Fernandez-Baeza' 'Andres Garces' ; A.Lara-Sanchez ; 'Isabel Lopez-Solera' 'Ana M Rodriguez' 'Luis F Sanchez-Barba' data_2 _database_code_depnum_ccdc_archive 'CCDC 732864' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H29 Cl N6 Zn' _chemical_formula_weight 430.29 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' Cl Cl 0.1484 0.1585 '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/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 8.649(5) _cell_length_b 13.089(7) _cell_length_c 10.018(6) _cell_angle_alpha 90.00 _cell_angle_beta 113.525(8) _cell_angle_gamma 90.00 _cell_volume 1039.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 215 _cell_measurement_theta_min 2.708 _cell_measurement_theta_max 16.584 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 452 _exptl_absorpt_coefficient_mu 1.323 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6692 _exptl_absorpt_correction_T_max 0.9131 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4368 _diffrn_reflns_av_R_equivalents 0.0916 _diffrn_reflns_av_sigmaI/netI 0.2987 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.49 _reflns_number_total 1988 _reflns_number_gt 692 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT, SADABS, XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1988 _refine_ls_number_parameters 135 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1513 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.1631 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 0.852 _refine_ls_restrained_S_all 0.852 _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 Zn1 Zn 0.99427(18) 0.2500 0.67056(12) 0.0351(4) Uani 1 2 d S . . Cl1 Cl 1.0413(4) 0.2500 0.4725(3) 0.0423(8) Uani 1 2 d S . . N1 N 1.1159(8) 0.3610(4) 0.8253(6) 0.0322(16) Uani 1 1 d . . . N2 N 1.0997(8) 0.3413(4) 0.9534(6) 0.0316(16) Uani 1 1 d . . . N3 N 0.7949(12) 0.2500 0.7178(8) 0.036(2) Uani 1 2 d S . . N4 N 0.7031(11) 0.2500 0.9082(8) 0.030(2) Uani 1 2 d S . . C1 C 1.1781(10) 0.4143(6) 1.0524(8) 0.037(2) Uani 1 1 d . . . C2 C 1.2464(10) 0.4830(5) 0.9877(8) 0.037(2) Uani 1 1 d . . . H2 H 1.3108 0.5419 1.0316 0.044 Uiso 1 1 calc R . . C3 C 1.2032(10) 0.4498(5) 0.8456(8) 0.0312(18) Uani 1 1 d . . . C4 C 1.1849(11) 0.4135(5) 1.2055(7) 0.045(2) Uani 1 1 d . . . H4A H 1.1731 0.4835 1.2350 0.068 Uiso 1 1 calc R . . H4B H 1.2932 0.3853 1.2721 0.068 Uiso 1 1 calc R . . H4C H 1.0929 0.3713 1.2086 0.068 Uiso 1 1 calc R . . C5 C 1.2381(11) 0.4946(5) 0.7246(7) 0.043(2) Uani 1 1 d . . . H5A H 1.1940 0.4492 0.6398 0.065 Uiso 1 1 calc R . . H5B H 1.3601 0.5027 0.7550 0.065 Uiso 1 1 calc R . . H5C H 1.1833 0.5615 0.6988 0.065 Uiso 1 1 calc R . . C6 C 1.0125(14) 0.2500 0.9663(10) 0.032(3) Uani 1 2 d S . . H6 H 1.0157 0.2500 1.0672 0.038 Uiso 1 2 calc SR . . C7 C 0.8257(16) 0.2500 0.8621(11) 0.036(3) Uani 1 2 d S . . C10 C 0.6192(16) 0.2500 0.6066(10) 0.036(3) Uani 1 2 d S . . C11 C 0.6248(17) 0.2500 0.4586(12) 0.071(4) Uani 1 2 d S . . H11A H 0.7019 0.3035 0.4543 0.107 Uiso 0.50 1 calc P . . H11B H 0.5115 0.2631 0.3843 0.107 Uiso 0.50 1 calc P . . H11C H 0.6645 0.1834 0.4406 0.107 Uiso 0.50 1 calc P . . C12 C 0.5223(11) 0.1551(6) 0.6186(8) 0.052(2) Uani 1 1 d . . . H12A H 0.5772 0.0938 0.6020 0.078 Uiso 1 1 calc . . . H12B H 0.4061 0.1586 0.5455 0.078 Uiso 1 1 calc . . . H12C H 0.5213 0.1520 0.7160 0.078 Uiso 1 1 calc . . . C8 C 0.7420(13) 0.2500 1.0626(9) 0.028(3) Uani 1 2 d S . . H8A H 0.8082 0.3114 1.1093 0.034 Uiso 0.50 1 calc PR . . H8B H 0.8082 0.1886 1.1093 0.034 Uiso 0.50 1 calc PR . . C9 C 0.5731(16) 0.2500 1.0772(11) 0.045(3) Uani 1 2 d S . . H9A H 0.5927 0.2500 1.1805 0.067 Uiso 1 2 calc S . . H9B H 0.5091 0.1889 1.0302 0.067 Uiso 0.50 1 calc P . . H9C H 0.5091 0.3111 1.0302 0.067 Uiso 0.50 1 calc P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0280(9) 0.0458(8) 0.0288(7) 0.000 0.0084(6) 0.000 Cl1 0.033(2) 0.0609(19) 0.0342(15) 0.000 0.0148(14) 0.000 N1 0.044(5) 0.028(3) 0.024(3) -0.004(3) 0.014(3) 0.001(3) N2 0.038(5) 0.029(4) 0.029(3) 0.005(3) 0.015(3) -0.005(3) N3 0.024(6) 0.065(6) 0.021(4) 0.000 0.013(5) 0.000 N4 0.025(6) 0.043(5) 0.019(4) 0.000 0.007(4) 0.000 C1 0.025(5) 0.042(5) 0.031(4) -0.005(4) -0.002(4) 0.004(4) C2 0.023(5) 0.042(5) 0.039(4) -0.006(4) 0.006(4) -0.007(4) C3 0.020(5) 0.030(4) 0.035(4) 0.002(4) 0.002(4) 0.006(4) C4 0.043(7) 0.048(5) 0.036(5) -0.005(4) 0.008(5) 0.000(4) C5 0.040(6) 0.045(5) 0.049(5) 0.001(4) 0.022(5) -0.008(4) C6 0.035(8) 0.030(6) 0.024(6) 0.000 0.006(6) 0.000 C7 0.047(9) 0.019(6) 0.039(7) 0.000 0.014(6) 0.000 C10 0.042(9) 0.043(7) 0.018(5) 0.000 0.008(6) 0.000 C11 0.024(9) 0.158(13) 0.033(7) 0.000 0.013(6) 0.000 C12 0.034(6) 0.065(6) 0.041(5) -0.003(4) -0.001(4) -0.007(5) C8 0.021(7) 0.029(6) 0.028(5) 0.000 0.003(5) 0.000 C9 0.043(9) 0.048(7) 0.040(7) 0.000 0.015(6) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N3 1.961(9) . ? Zn1 N1 2.078(6) . ? Zn1 N1 2.078(6) 4_565 ? Zn1 Cl1 2.179(3) . ? N1 C3 1.357(8) . ? N1 N2 1.371(7) . ? N2 C1 1.349(8) . ? N2 C6 1.446(8) . ? N3 C7 1.362(12) . ? N3 C10 1.482(15) . ? N4 C7 1.314(13) . ? N4 C8 1.446(10) . ? C1 C2 1.372(9) . ? C1 C4 1.511(9) . ? C2 C3 1.389(9) . ? C3 C5 1.482(9) . ? C6 N2 1.446(8) 4_565 ? C6 C7 1.534(15) . ? C10 C11 1.503(13) . ? C10 C12 1.530(11) . ? C10 C12 1.530(11) 4_565 ? C8 C9 1.525(14) . ? 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 Zn1 N1 93.0(2) . . ? N3 Zn1 N1 93.0(2) . 4_565 ? N1 Zn1 N1 88.7(3) . 4_565 ? N3 Zn1 Cl1 136.2(3) . . ? N1 Zn1 Cl1 117.14(17) . . ? N1 Zn1 Cl1 117.14(17) 4_565 . ? C3 N1 N2 106.2(6) . . ? C3 N1 Zn1 142.9(5) . . ? N2 N1 Zn1 110.9(4) . . ? C1 N2 N1 110.3(6) . . ? C1 N2 C6 130.3(6) . . ? N1 N2 C6 119.4(6) . . ? C7 N3 C10 120.3(9) . . ? C7 N3 Zn1 116.0(8) . . ? C10 N3 Zn1 123.7(6) . . ? C7 N4 C8 120.0(9) . . ? N2 C1 C2 107.6(6) . . ? N2 C1 C4 123.1(7) . . ? C2 C1 C4 129.4(7) . . ? C1 C2 C3 106.8(7) . . ? N1 C3 C2 109.1(6) . . ? N1 C3 C5 119.9(6) . . ? C2 C3 C5 131.0(7) . . ? N2 C6 N2 111.5(9) . 4_565 ? N2 C6 C7 112.6(6) . . ? N2 C6 C7 112.6(6) 4_565 . ? N4 C7 N3 122.0(11) . . ? N4 C7 C6 122.6(10) . . ? N3 C7 C6 115.4(10) . . ? N3 C10 C11 108.3(10) . . ? N3 C10 C12 111.8(6) . . ? C11 C10 C12 108.2(6) . . ? N3 C10 C12 111.8(6) . 4_565 ? C11 C10 C12 108.2(6) . 4_565 ? C12 C10 C12 108.6(10) . 4_565 ? N4 C8 C9 106.3(8) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.587 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.114 data_3 _database_code_depnum_ccdc_archive 'CCDC 732865' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H37 N7 Zn' _chemical_formula_weight 500.99 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' 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/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 8.3079(12) _cell_length_b 19.091(3) _cell_length_c 16.587(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.208(3) _cell_angle_gamma 90.00 _cell_volume 2610.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 2162 _cell_measurement_theta_min 2.466 _cell_measurement_theta_max 21.076 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.275 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 0.967 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7346 _exptl_absorpt_correction_T_max 0.8928 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21191 _diffrn_reflns_av_R_equivalents 0.0773 _diffrn_reflns_av_sigmaI/netI 0.0886 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 28.32 _reflns_number_total 6417 _reflns_number_gt 3865 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT, SADABS, XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0762P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6417 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1053 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1509 _refine_ls_wR_factor_gt 0.1282 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _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 Zn1 Zn 0.35224(4) 0.074598(18) 0.33942(2) 0.02821(14) Uani 1 1 d . . . N1 N 0.5996(3) 0.08845(12) 0.33389(17) 0.0282(6) Uani 1 1 d . . . N2 N 0.6548(3) 0.15044(12) 0.36908(16) 0.0277(6) Uani 1 1 d . . . N3 N 0.3273(3) 0.17901(13) 0.29702(17) 0.0308(6) Uani 1 1 d . . . N4 N 0.4199(3) 0.22309(12) 0.34838(16) 0.0281(6) Uani 1 1 d . . . N5 N 0.5072(3) 0.17326(14) 0.55364(17) 0.0328(6) Uani 1 1 d . B . N6 N 0.3668(3) 0.10502(13) 0.45225(16) 0.0270(6) Uani 1 1 d . . . N7 N 0.2315(4) 0.00520(15) 0.27842(19) 0.0362(7) Uani 1 1 d . . . C1 C 0.8134(4) 0.16065(17) 0.3606(2) 0.0335(8) Uani 1 1 d . . . C2 C 0.8608(4) 0.10384(18) 0.3197(2) 0.0358(8) Uani 1 1 d . . . H2 H 0.9658 0.0955 0.3048 0.043 Uiso 1 1 calc R . . C3 C 0.7260(4) 0.06048(16) 0.3040(2) 0.0316(8) Uani 1 1 d . . . C4 C 0.9041(4) 0.22515(18) 0.3910(2) 0.0461(10) Uani 1 1 d . . . H4A H 0.8556 0.2662 0.3619 0.069 Uiso 1 1 calc R . . H4B H 1.0179 0.2209 0.3817 0.069 Uiso 1 1 calc R . . H4C H 0.8982 0.2305 0.4493 0.069 Uiso 1 1 calc R . . C5 C 0.7085(4) -0.00893(17) 0.2615(2) 0.0411(9) Uani 1 1 d . . . H5A H 0.6682 -0.0437 0.2975 0.062 Uiso 1 1 calc R . . H5B H 0.8142 -0.0239 0.2473 0.062 Uiso 1 1 calc R . . H5C H 0.6315 -0.0045 0.2119 0.062 Uiso 1 1 calc R . . C6 C 0.3757(4) 0.29096(16) 0.3344(2) 0.0332(8) Uani 1 1 d . . . C7 C 0.2532(4) 0.28976(17) 0.2711(2) 0.0396(9) Uani 1 1 d . . . H7 H 0.1965 0.3292 0.2469 0.048 Uiso 1 1 calc R . . C8 C 0.2270(4) 0.22043(17) 0.2487(2) 0.0327(8) Uani 1 1 d . . . C9 C 0.4578(5) 0.35023(18) 0.3824(3) 0.0543(11) Uani 1 1 d . . . H9A H 0.4662 0.3393 0.4405 0.081 Uiso 1 1 calc R . . H9B H 0.3942 0.3932 0.3713 0.081 Uiso 1 1 calc R . . H9C H 0.5666 0.3570 0.3668 0.081 Uiso 1 1 calc R . . C10 C 0.1124(4) 0.18935(19) 0.1825(2) 0.0424(9) Uani 1 1 d . . . H10A H 0.1423 0.1404 0.1743 0.064 Uiso 1 1 calc R . . H10B H 0.1172 0.2157 0.1322 0.064 Uiso 1 1 calc R . . H10C H 0.0019 0.1913 0.1973 0.064 Uiso 1 1 calc R . . C11 C 0.5446(4) 0.19467(15) 0.40899(19) 0.0271(7) Uani 1 1 d . . . H11 H 0.6094 0.2351 0.4339 0.032 Uiso 1 1 calc R . . C12 C 0.4725(3) 0.15655(15) 0.4779(2) 0.0263(7) Uani 1 1 d . . . C13 C 0.6329(4) 0.22246(17) 0.5860(2) 0.0382(8) Uani 1 1 d . . . H13 H 0.6668 0.2500 0.5397 0.046 Uiso 1 1 calc R A 1 C14 C 0.7767(11) 0.1792(5) 0.6230(6) 0.053(2) Uiso 0.50 1 d P B 1 H14A H 0.7416 0.1466 0.6630 0.079 Uiso 0.50 1 calc PR B 1 H14B H 0.8608 0.2103 0.6498 0.079 Uiso 0.50 1 calc PR B 1 H14C H 0.8207 0.1527 0.5801 0.079 Uiso 0.50 1 calc PR B 1 C15 C 0.5753(10) 0.2714(4) 0.6436(5) 0.037(2) Uiso 0.50 1 d P B 1 H15A H 0.4802 0.2966 0.6172 0.055 Uiso 0.50 1 calc PR B 1 H15B H 0.6615 0.3050 0.6618 0.055 Uiso 0.50 1 calc PR B 1 H15C H 0.5456 0.2455 0.6906 0.055 Uiso 0.50 1 calc PR B 1 C15A C 0.5419(12) 0.2849(5) 0.6233(7) 0.055(3) Uiso 0.50 1 d P B 2 H15D H 0.4622 0.3052 0.5812 0.082 Uiso 0.50 1 calc PR B 2 H15E H 0.6208 0.3209 0.6438 0.082 Uiso 0.50 1 calc PR B 2 H15F H 0.4864 0.2675 0.6680 0.082 Uiso 0.50 1 calc PR B 2 C14A C 0.7436(11) 0.1842(5) 0.6541(6) 0.053(2) Uiso 0.50 1 d P B 2 H14D H 0.6778 0.1666 0.6949 0.080 Uiso 0.50 1 calc PR B 2 H14E H 0.8254 0.2169 0.6799 0.080 Uiso 0.50 1 calc PR B 2 H14F H 0.7978 0.1448 0.6308 0.080 Uiso 0.50 1 calc PR B 2 C16 C 0.2945(4) 0.06758(15) 0.5162(2) 0.0286(7) Uani 1 1 d . . . H16 H 0.3808 0.0597 0.5630 0.034 Uiso 1 1 calc R . . C17 C 0.1588(4) 0.11048(18) 0.5458(2) 0.0388(9) Uani 1 1 d . . . H17A H 0.2013 0.1562 0.5652 0.058 Uiso 1 1 calc R . . H17B H 0.1163 0.0856 0.5903 0.058 Uiso 1 1 calc R . . H17C H 0.0715 0.1173 0.5010 0.058 Uiso 1 1 calc R . . C18 C 0.2323(4) -0.00290(16) 0.4846(2) 0.0362(8) Uani 1 1 d . . . H18A H 0.1429 0.0039 0.4408 0.054 Uiso 1 1 calc R . . H18B H 0.1934 -0.0295 0.5288 0.054 Uiso 1 1 calc R . . H18C H 0.3202 -0.0288 0.4637 0.054 Uiso 1 1 calc R . . C19 C 0.2222(4) -0.01223(16) 0.1982(2) 0.0311(7) Uani 1 1 d . . . C20 C 0.1236(4) -0.06701(16) 0.1633(2) 0.0368(8) Uani 1 1 d . . . H20 H 0.0629 -0.0942 0.1968 0.044 Uiso 1 1 calc R . . C21 C 0.1133(5) -0.08198(18) 0.0813(2) 0.0435(10) Uani 1 1 d . . . H21 H 0.0435 -0.1188 0.0600 0.052 Uiso 1 1 calc R . . C22 C 0.1996(5) -0.0460(2) 0.0290(2) 0.0439(9) Uani 1 1 d . . . C23 C 0.2977(4) 0.00863(18) 0.0634(2) 0.0426(9) Uani 1 1 d . . . H23 H 0.3582 0.0355 0.0295 0.051 Uiso 1 1 calc R . . C24 C 0.3093(4) 0.02474(17) 0.1451(2) 0.0340(8) Uani 1 1 d . . . H24 H 0.3783 0.0620 0.1658 0.041 Uiso 1 1 calc R . . C25 C 0.1872(6) -0.0637(2) -0.0596(3) 0.0674(14) Uani 1 1 d . . . H25A H 0.1650 -0.1139 -0.0671 0.101 Uiso 1 1 calc R . . H25B H 0.2896 -0.0522 -0.0801 0.101 Uiso 1 1 calc R . . H25C H 0.0989 -0.0367 -0.0896 0.101 Uiso 1 1 calc R . . H7A H 0.188(4) -0.0227(18) 0.303(2) 0.040(11) 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 Zn1 0.0273(2) 0.0272(2) 0.0303(2) -0.00111(17) 0.00439(15) -0.00243(15) N1 0.0288(14) 0.0261(14) 0.0303(17) -0.0023(11) 0.0061(12) 0.0008(10) N2 0.0241(14) 0.0275(14) 0.0328(17) 0.0000(12) 0.0092(11) -0.0004(10) N3 0.0279(15) 0.0279(14) 0.0372(18) 0.0016(13) 0.0059(12) -0.0002(11) N4 0.0298(14) 0.0235(13) 0.0321(17) 0.0024(12) 0.0076(12) 0.0004(11) N5 0.0288(15) 0.0384(16) 0.0325(18) -0.0057(13) 0.0089(12) -0.0098(11) N6 0.0269(14) 0.0260(13) 0.0286(16) 0.0009(12) 0.0060(11) -0.0061(11) N7 0.0419(18) 0.0345(16) 0.0329(19) -0.0003(14) 0.0069(13) -0.0106(13) C1 0.0285(17) 0.0357(18) 0.037(2) 0.0070(16) 0.0075(14) -0.0038(14) C2 0.0253(17) 0.044(2) 0.040(2) 0.0069(17) 0.0127(15) 0.0042(14) C3 0.0366(19) 0.0345(18) 0.0246(19) 0.0059(14) 0.0073(14) 0.0098(14) C4 0.0309(19) 0.047(2) 0.063(3) -0.0011(19) 0.0144(18) -0.0137(16) C5 0.044(2) 0.0384(19) 0.042(2) -0.0018(17) 0.0104(17) 0.0108(15) C6 0.0350(19) 0.0254(16) 0.041(2) 0.0028(15) 0.0104(16) -0.0003(13) C7 0.039(2) 0.0306(18) 0.050(2) 0.0061(17) 0.0082(17) 0.0103(15) C8 0.0314(18) 0.0345(18) 0.033(2) 0.0045(15) 0.0093(15) 0.0046(14) C9 0.064(3) 0.0282(19) 0.067(3) -0.0020(19) -0.004(2) 0.0027(17) C10 0.033(2) 0.045(2) 0.047(3) 0.0074(18) -0.0035(16) 0.0049(15) C11 0.0266(16) 0.0265(16) 0.0284(19) -0.0034(13) 0.0049(13) -0.0012(12) C12 0.0214(16) 0.0285(16) 0.0300(19) -0.0006(14) 0.0071(13) 0.0009(12) C13 0.038(2) 0.0373(19) 0.040(2) -0.0083(16) 0.0092(16) -0.0124(15) C16 0.0256(16) 0.0324(17) 0.0279(19) 0.0012(14) 0.0043(13) -0.0052(12) C17 0.0296(19) 0.045(2) 0.044(2) -0.0034(18) 0.0134(16) -0.0043(15) C18 0.0336(19) 0.0342(18) 0.041(2) 0.0098(16) 0.0054(15) -0.0067(14) C19 0.0315(18) 0.0284(17) 0.032(2) -0.0015(15) -0.0002(14) 0.0026(13) C20 0.037(2) 0.0318(19) 0.040(2) -0.0023(16) -0.0025(16) 0.0004(14) C21 0.046(2) 0.035(2) 0.045(3) -0.0106(18) -0.0118(18) 0.0067(16) C22 0.048(2) 0.047(2) 0.034(2) -0.0038(18) -0.0072(17) 0.0180(18) C23 0.046(2) 0.042(2) 0.039(2) 0.0088(18) 0.0055(17) 0.0110(16) C24 0.0340(19) 0.0349(18) 0.033(2) 0.0010(15) 0.0015(15) -0.0002(14) C25 0.086(4) 0.076(3) 0.036(3) -0.015(2) -0.008(2) 0.027(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 Zn1 N7 1.879(3) . ? Zn1 N6 1.949(3) . ? Zn1 N1 2.085(3) . ? Zn1 N3 2.115(3) . ? N1 C3 1.328(4) . ? N1 N2 1.373(3) . ? N2 C1 1.357(4) . ? N2 C11 1.463(4) . ? N3 C8 1.340(4) . ? N3 N4 1.364(4) . ? N4 C6 1.358(4) . ? N4 C11 1.455(4) . ? N5 C12 1.294(4) . ? N5 C13 1.456(4) . ? N6 C12 1.351(4) . ? N6 C16 1.468(4) . ? N7 C19 1.365(4) . ? C1 C2 1.363(5) . ? C1 C4 1.498(5) . ? C2 C3 1.391(5) . ? C3 C5 1.499(4) . ? C6 C7 1.368(4) . ? C6 C9 1.497(5) . ? C7 C8 1.385(4) . ? C8 C10 1.484(5) . ? C11 C12 1.538(4) . ? C13 C15 1.460(9) . ? C13 C14 1.518(9) . ? C13 C14A 1.548(10) . ? C13 C15A 1.579(10) . ? C16 C18 1.511(4) . ? C16 C17 1.525(4) . ? C19 C24 1.399(4) . ? C19 C20 1.407(4) . ? C20 C21 1.382(5) . ? C21 C22 1.377(5) . ? C22 C23 1.400(5) . ? C22 C25 1.499(5) . ? C23 C24 1.380(5) . ? 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 N7 Zn1 N6 133.78(12) . . ? N7 Zn1 N1 121.88(12) . . ? N6 Zn1 N1 93.54(10) . . ? N7 Zn1 N3 117.52(12) . . ? N6 Zn1 N3 91.73(11) . . ? N1 Zn1 N3 85.52(10) . . ? C3 N1 N2 105.5(2) . . ? C3 N1 Zn1 142.7(2) . . ? N2 N1 Zn1 111.66(17) . . ? C1 N2 N1 110.9(2) . . ? C1 N2 C11 129.4(3) . . ? N1 N2 C11 119.7(2) . . ? C8 N3 N4 105.6(3) . . ? C8 N3 Zn1 141.5(2) . . ? N4 N3 Zn1 110.47(19) . . ? C6 N4 N3 111.3(3) . . ? C6 N4 C11 128.8(3) . . ? N3 N4 C11 119.9(2) . . ? C12 N5 C13 125.4(3) . . ? C12 N6 C16 115.8(3) . . ? C12 N6 Zn1 118.6(2) . . ? C16 N6 Zn1 124.53(19) . . ? C19 N7 Zn1 131.2(2) . . ? N2 C1 C2 106.4(3) . . ? N2 C1 C4 122.5(3) . . ? C2 C1 C4 131.1(3) . . ? C1 C2 C3 106.9(3) . . ? N1 C3 C2 110.3(3) . . ? N1 C3 C5 119.8(3) . . ? C2 C3 C5 130.0(3) . . ? N4 C6 C7 105.9(3) . . ? N4 C6 C9 122.3(3) . . ? C7 C6 C9 131.7(3) . . ? C6 C7 C8 107.4(3) . . ? N3 C8 C7 109.8(3) . . ? N3 C8 C10 120.0(3) . . ? C7 C8 C10 130.2(3) . . ? N4 C11 N2 109.5(3) . . ? N4 C11 C12 112.3(2) . . ? N2 C11 C12 112.8(2) . . ? N5 C12 N6 122.8(3) . . ? N5 C12 C11 123.0(3) . . ? N6 C12 C11 114.2(3) . . ? N5 C13 C15 112.1(4) . . ? N5 C13 C14 106.8(4) . . ? C15 C13 C14 112.9(6) . . ? N5 C13 C14A 107.3(4) . . ? C15 C13 C14A 92.2(5) . . ? C14 C13 C14A 23.4(5) . . ? N5 C13 C15A 106.0(5) . . ? C15 C13 C15A 17.8(5) . . ? C14 C13 C15A 130.1(6) . . ? C14A C13 C15A 109.9(6) . . ? N6 C16 C18 109.7(3) . . ? N6 C16 C17 110.9(3) . . ? C18 C16 C17 110.8(3) . . ? N7 C19 C24 121.4(3) . . ? N7 C19 C20 122.7(3) . . ? C24 C19 C20 115.9(3) . . ? C21 C20 C19 121.3(3) . . ? C22 C21 C20 123.0(3) . . ? C21 C22 C23 115.9(4) . . ? C21 C22 C25 121.9(4) . . ? C23 C22 C25 122.3(4) . . ? C24 C23 C22 122.2(4) . . ? C23 C24 C19 121.8(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.827 _refine_diff_density_min -0.776 _refine_diff_density_rms 0.100 data_6 _database_code_depnum_ccdc_archive 'CCDC 732866' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H47 N7 Si2 Zn' _chemical_formula_weight 555.24 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' 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 8.2710(5) _cell_length_b 13.0287(8) _cell_length_c 15.1904(9) _cell_angle_alpha 96.475(4) _cell_angle_beta 96.113(4) _cell_angle_gamma 105.423(4) _cell_volume 1551.91(16) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.328 _exptl_crystal_size_mid 0.259 _exptl_crystal_size_min 0.0715 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 0.892 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.124520 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega and phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12355 _diffrn_reflns_av_R_equivalents 0.0941 _diffrn_reflns_av_sigmaI/netI 0.2563 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 29.92 _reflns_number_total 7013 _reflns_number_gt 3496 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.5564P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7013 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1882 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.2531 _refine_ls_wR_factor_gt 0.1818 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.078 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.55611(7) 0.67450(5) 0.73691(4) 0.0293(2) Uani 1 1 d . . . Si2 Si 0.6630(2) 0.88545(14) 0.65560(12) 0.0385(5) Uani 1 1 d . . . Si1 Si 0.5447(2) 0.89609(15) 0.83625(12) 0.0399(5) Uani 1 1 d . . . N3 N 0.6418(5) 0.5608(4) 0.6435(3) 0.0265(11) Uani 1 1 d . . . N7 N 0.5931(6) 0.8283(4) 0.7451(3) 0.0323(13) Uani 1 1 d . . . C24 C 0.3610(10) 0.9532(7) 0.8118(6) 0.061(2) Uani 1 1 d . . . H24A H 0.3872 1.0035 0.7703 0.092 Uiso 1 1 calc R . . H24B H 0.3404 0.9892 0.8664 0.092 Uiso 1 1 calc R . . H24C H 0.2618 0.8959 0.7864 0.092 Uiso 1 1 calc R . . N6 N 0.2510(5) 0.3686(4) 0.7442(3) 0.0361(14) Uani 1 1 d . . . C11 C 0.5617(7) 0.4538(5) 0.7645(4) 0.0308(15) Uani 1 1 d . . . H11 H 0.5610 0.3811 0.7758 0.037 Uiso 1 1 calc R . . C13 C 0.2708(7) 0.2627(5) 0.7509(4) 0.0359(17) Uani 1 1 d . . . H13 H 0.3899 0.2681 0.7705 0.043 Uiso 1 1 calc R . . C6 C 0.7216(7) 0.4073(5) 0.6420(4) 0.0295(15) Uani 1 1 d . . . C2 C 0.8334(7) 0.5996(6) 0.9664(4) 0.0440(19) Uani 1 1 d . . . H2 H 0.8970 0.6101 1.0227 0.053 Uiso 1 1 calc R . . C10 C 0.7365(7) 0.6225(5) 0.5037(4) 0.0418(18) Uani 1 1 d . . . H10A H 0.7002 0.6837 0.5249 0.063 Uiso 1 1 calc R . . H10B H 0.6677 0.5864 0.4481 0.063 Uiso 1 1 calc R . . H10C H 0.8529 0.6458 0.4945 0.063 Uiso 1 1 calc R . . C8 C 0.7187(6) 0.5464(5) 0.5717(4) 0.0327(16) Uani 1 1 d . . . C4 C 0.9236(8) 0.7938(6) 0.9274(5) 0.0475(19) Uani 1 1 d . . . H4A H 1.0422 0.7990 0.9319 0.071 Uiso 1 1 calc R . . H4B H 0.9008 0.8283 0.9821 0.071 Uiso 1 1 calc R . . H4C H 0.8921 0.8285 0.8785 0.071 Uiso 1 1 calc R . . C17 C 0.0912(7) 0.5503(5) 0.8044(4) 0.046(2) Uani 1 1 d . . . H17A H 0.0964 0.4867 0.8295 0.069 Uiso 1 1 calc R . . H17B H -0.0252 0.5481 0.7879 0.069 Uiso 1 1 calc R . . H17C H 0.1459 0.6127 0.8478 0.069 Uiso 1 1 calc R . . C3 C 0.7309(7) 0.5045(5) 0.9210(4) 0.0419(18) Uani 1 1 d . . . C19 C 0.5120(9) 0.8235(6) 0.5514(4) 0.054(2) Uani 1 1 d . . . H19A H 0.4877 0.7466 0.5453 0.081 Uiso 1 1 calc R . . H19B H 0.5615 0.8485 0.5006 0.081 Uiso 1 1 calc R . . H19C H 0.4089 0.8435 0.5545 0.081 Uiso 1 1 calc R . . C1 C 0.8245(7) 0.6792(5) 0.9117(4) 0.0360(16) Uani 1 1 d . . . C20 C 0.6787(11) 1.0328(6) 0.6634(6) 0.067(3) Uani 1 1 d . . . H20A H 0.5670 1.0421 0.6573 0.100 Uiso 1 1 calc R . . H20B H 0.7370 1.0619 0.6165 0.100 Uiso 1 1 calc R . . H20C H 0.7402 1.0696 0.7204 0.100 Uiso 1 1 calc R . . C16 C 0.1809(6) 0.5557(5) 0.7213(4) 0.0288(14) Uani 1 1 d . . . H16 H 0.1213 0.4925 0.6772 0.035 Uiso 1 1 calc R . . C14 C 0.1616(10) 0.2137(6) 0.8193(5) 0.069(3) Uani 1 1 d . . . H14A H 0.1993 0.2581 0.8766 0.104 Uiso 1 1 calc R . . H14B H 0.1716 0.1428 0.8239 0.104 Uiso 1 1 calc R . . H14C H 0.0453 0.2097 0.8003 0.104 Uiso 1 1 calc R . . N5 N 0.3572(5) 0.5541(4) 0.7423(3) 0.0270(12) Uani 1 1 d . . . N2 N 0.6611(5) 0.5271(4) 0.8414(3) 0.0289(12) Uani 1 1 d . . . N1 N 0.7189(5) 0.6339(4) 0.8363(3) 0.0308(13) Uani 1 1 d . . . N4 N 0.6437(5) 0.4722(4) 0.6853(3) 0.0291(12) Uani 1 1 d . . . C22 C 0.4833(8) 0.8056(6) 0.9214(4) 0.050(2) Uani 1 1 d . . . H22A H 0.4003 0.7405 0.8930 0.075 Uiso 1 1 calc R . . H22B H 0.4365 0.8413 0.9668 0.075 Uiso 1 1 calc R . . H22C H 0.5816 0.7885 0.9482 0.075 Uiso 1 1 calc R . . C23 C 0.7247(10) 1.0141(6) 0.8936(5) 0.060(2) Uani 1 1 d . . . H23A H 0.8305 1.0000 0.8850 0.089 Uiso 1 1 calc R . . H23B H 0.7174 1.0248 0.9565 0.089 Uiso 1 1 calc R . . H23C H 0.7179 1.0775 0.8687 0.089 Uiso 1 1 calc R . . C21 C 0.8807(8) 0.8760(6) 0.6442(5) 0.059(2) Uani 1 1 d . . . H21A H 0.9605 0.9260 0.6903 0.089 Uiso 1 1 calc R . . H21B H 0.9079 0.8928 0.5866 0.089 Uiso 1 1 calc R . . H21C H 0.8860 0.8042 0.6496 0.089 Uiso 1 1 calc R . . C12 C 0.3753(6) 0.4557(5) 0.7500(3) 0.0277(14) Uani 1 1 d . . . C7 C 0.7721(7) 0.4549(5) 0.5693(4) 0.0383(17) Uani 1 1 d . . . H7 H 0.8311 0.4300 0.5268 0.046 Uiso 1 1 calc R . . C18 C 0.1711(8) 0.6561(5) 0.6806(4) 0.0426(18) Uani 1 1 d . . . H18A H 0.2310 0.7191 0.7224 0.064 Uiso 1 1 calc R . . H18B H 0.0547 0.6553 0.6673 0.064 Uiso 1 1 calc R . . H18C H 0.2215 0.6571 0.6265 0.064 Uiso 1 1 calc R . . C9 C 0.7503(9) 0.3101(5) 0.6740(5) 0.050(2) Uani 1 1 d . . . H9A H 0.8230 0.3300 0.7304 0.075 Uiso 1 1 calc R . . H9B H 0.8027 0.2748 0.6312 0.075 Uiso 1 1 calc R . . H9C H 0.6438 0.2621 0.6811 0.075 Uiso 1 1 calc R . . C5 C 0.6893(11) 0.3904(6) 0.9421(5) 0.071(3) Uani 1 1 d . . . H5A H 0.5715 0.3664 0.9485 0.106 Uiso 1 1 calc R . . H5B H 0.7572 0.3884 0.9969 0.106 Uiso 1 1 calc R . . H5C H 0.7127 0.3442 0.8943 0.106 Uiso 1 1 calc R . . C15 C 0.2122(12) 0.1934(6) 0.6614(5) 0.067(3) Uani 1 1 d . . . H15A H 0.0976 0.1919 0.6411 0.100 Uiso 1 1 calc R . . H15B H 0.2177 0.1217 0.6667 0.100 Uiso 1 1 calc R . . H15C H 0.2840 0.2225 0.6193 0.100 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0287(3) 0.0220(4) 0.0358(4) 0.0044(3) 0.0080(3) 0.0031(3) Si2 0.0441(9) 0.0238(10) 0.0457(10) 0.0074(9) 0.0111(8) 0.0033(8) Si1 0.0396(9) 0.0305(11) 0.0481(10) -0.0002(9) 0.0115(8) 0.0080(8) N3 0.030(2) 0.019(3) 0.033(2) 0.003(2) 0.008(2) 0.0095(19) N7 0.041(3) 0.016(3) 0.035(2) 0.002(2) 0.005(2) -0.001(2) C24 0.061(5) 0.045(5) 0.080(5) -0.006(5) 0.013(4) 0.023(4) N6 0.025(2) 0.023(3) 0.058(3) 0.007(3) 0.008(2) 0.001(2) C11 0.036(3) 0.020(3) 0.031(3) 0.001(3) 0.007(2) -0.001(2) C13 0.031(3) 0.024(4) 0.052(4) 0.012(3) 0.009(3) 0.003(3) C6 0.028(3) 0.021(3) 0.039(3) -0.004(3) 0.003(2) 0.010(2) C2 0.042(3) 0.055(5) 0.028(3) 0.003(3) -0.001(3) 0.005(3) C10 0.043(3) 0.047(4) 0.037(3) 0.010(3) 0.010(3) 0.011(3) C8 0.028(3) 0.032(4) 0.034(3) -0.001(3) 0.007(2) 0.002(3) C4 0.041(4) 0.040(5) 0.051(4) -0.001(4) -0.006(3) 0.002(3) C17 0.037(3) 0.049(5) 0.049(4) -0.002(3) 0.017(3) 0.007(3) C3 0.045(3) 0.048(4) 0.032(3) 0.014(3) 0.005(3) 0.008(3) C19 0.056(4) 0.060(5) 0.047(4) 0.011(4) 0.009(3) 0.016(4) C1 0.028(3) 0.044(4) 0.035(3) 0.003(3) 0.004(3) 0.010(3) C20 0.093(6) 0.029(4) 0.079(5) 0.010(4) 0.029(5) 0.012(4) C16 0.027(3) 0.023(3) 0.036(3) -0.001(3) 0.006(2) 0.009(2) C14 0.112(6) 0.036(4) 0.069(5) 0.020(4) 0.055(5) 0.016(4) N5 0.022(2) 0.024(3) 0.036(2) 0.008(2) 0.0071(19) 0.0064(18) N2 0.030(2) 0.027(3) 0.031(2) 0.007(2) 0.006(2) 0.007(2) N1 0.032(2) 0.024(3) 0.032(3) 0.000(2) 0.006(2) 0.002(2) N4 0.031(2) 0.020(3) 0.037(3) 0.003(2) 0.009(2) 0.008(2) C22 0.055(4) 0.050(5) 0.041(4) 0.003(3) 0.016(3) 0.006(3) C23 0.070(5) 0.043(5) 0.058(4) -0.012(4) 0.015(4) 0.008(4) C21 0.044(4) 0.063(5) 0.070(5) 0.011(4) 0.021(4) 0.007(4) C12 0.026(2) 0.027(3) 0.027(3) 0.002(3) 0.005(2) 0.002(2) C7 0.036(3) 0.031(4) 0.045(4) -0.007(3) 0.012(3) 0.007(3) C18 0.037(3) 0.028(4) 0.062(4) 0.008(3) 0.002(3) 0.009(3) C9 0.053(4) 0.032(4) 0.069(5) 0.003(4) 0.017(4) 0.018(3) C5 0.083(6) 0.057(6) 0.059(5) 0.032(5) -0.014(4) -0.003(4) C15 0.123(8) 0.028(5) 0.053(5) 0.005(4) 0.020(5) 0.026(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 Zn1 N7 1.932(5) . ? Zn1 N5 1.964(3) . ? Zn1 N1 2.121(5) . ? Zn1 N3 2.237(4) . ? Si2 N7 1.705(4) . ? Si2 C21 1.862(7) . ? Si2 C19 1.864(8) . ? Si2 C20 1.878(8) . ? Si1 N7 1.699(5) . ? Si1 C22 1.867(5) . ? Si1 C24 1.882(9) . ? Si1 C23 1.882(8) . ? N3 C8 1.341(5) . ? N3 N4 1.381(6) . ? N6 C12 1.301(6) . ? N6 C13 1.446(8) . ? C11 N2 1.442(7) . ? C11 N4 1.455(5) . ? C11 C12 1.541(7) . ? C13 C15 1.499(10) . ? C13 C14 1.531(5) . ? C6 N4 1.348(7) . ? C6 C7 1.376(6) . ? C6 C9 1.473(9) . ? C2 C3 1.362(9) . ? C2 C1 1.413(9) . ? C10 C8 1.503(7) . ? C8 C7 1.375(9) . ? C4 C1 1.478(8) . ? C17 C16 1.530(6) . ? C3 N2 1.380(8) . ? C3 C5 1.513(9) . ? C1 N1 1.336(7) . ? C16 N5 1.465(7) . ? C16 C18 1.525(8) . ? N5 C12 1.346(7) . ? N2 N1 1.359(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Zn1 N5 133.4(2) . . ? N7 Zn1 N1 112.0(2) . . ? N5 Zn1 N1 95.61(17) . . ? N7 Zn1 N3 130.50(14) . . ? N5 Zn1 N3 87.44(16) . . ? N1 Zn1 N3 84.14(18) . . ? N7 Si2 C21 110.6(3) . . ? N7 Si2 C19 110.8(2) . . ? C21 Si2 C19 111.8(3) . . ? N7 Si2 C20 114.3(3) . . ? C21 Si2 C20 105.2(3) . . ? C19 Si2 C20 103.9(4) . . ? N7 Si1 C22 110.9(3) . . ? N7 Si1 C24 114.3(3) . . ? C22 Si1 C24 105.3(3) . . ? N7 Si1 C23 113.5(3) . . ? C22 Si1 C23 107.1(3) . . ? C24 Si1 C23 105.1(4) . . ? C8 N3 N4 103.7(5) . . ? C8 N3 Zn1 147.5(4) . . ? N4 N3 Zn1 107.3(3) . . ? Si1 N7 Si2 124.4(3) . . ? Si1 N7 Zn1 119.13(19) . . ? Si2 N7 Zn1 116.4(3) . . ? C12 N6 C13 124.8(5) . . ? N2 C11 N4 110.2(3) . . ? N2 C11 C12 113.4(5) . . ? N4 C11 C12 112.4(5) . . ? N6 C13 C15 109.3(5) . . ? N6 C13 C14 108.3(5) . . ? C15 C13 C14 109.6(5) . . ? N4 C6 C7 105.8(5) . . ? N4 C6 C9 124.0(4) . . ? C7 C6 C9 130.1(5) . . ? C3 C2 C1 106.7(6) . . ? N3 C8 C7 111.5(5) . . ? N3 C8 C10 121.8(6) . . ? C7 C8 C10 126.7(5) . . ? C2 C3 N2 106.6(5) . . ? C2 C3 C5 132.6(6) . . ? N2 C3 C5 120.7(6) . . ? N1 C1 C2 109.4(5) . . ? N1 C1 C4 122.7(5) . . ? C2 C1 C4 127.8(6) . . ? N5 C16 C18 111.0(4) . . ? N5 C16 C17 111.5(5) . . ? C18 C16 C17 109.6(5) . . ? C12 N5 C16 114.1(4) . . ? C12 N5 Zn1 120.1(3) . . ? C16 N5 Zn1 124.8(3) . . ? N1 N2 C3 110.4(5) . . ? N1 N2 C11 119.9(4) . . ? C3 N2 C11 129.0(5) . . ? C1 N1 N2 106.9(5) . . ? C1 N1 Zn1 139.9(4) . . ? N2 N1 Zn1 109.2(4) . . ? C6 N4 N3 112.2(4) . . ? C6 N4 C11 126.6(5) . . ? N3 N4 C11 121.2(4) . . ? N6 C12 N5 124.9(5) . . ? N6 C12 C11 121.6(5) . . ? N5 C12 C11 113.4(4) . . ? C8 C7 C6 106.8(5) . . ? _diffrn_measured_fraction_theta_max 0.779 _diffrn_reflns_theta_full 29.92 _diffrn_measured_fraction_theta_full 0.779 _refine_diff_density_max 0.971 _refine_diff_density_min -1.188 _refine_diff_density_rms 0.205