# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1740 data_znme #-------------------------------DATA FOR COMPOUND 3a-------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H39 Li N2 Si4 Zn' _chemical_formula_weight 408.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Zn' 'Zn' 0.2839 1.4301 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 17.040(10) _cell_length_b 6.840(8) _cell_length_c 21.558(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.47(4) _cell_angle_gamma 90.00 _cell_volume 2383(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 19.21 _cell_measurement_theta_max 20.00 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.228 _exptl_absorpt_correction_type 'psi scans' _exptl_absorpt_correction_T_min 0.911 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S diffractometer' _diffrn_measurement_method '\w/2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.64 _diffrn_reflns_number 4689 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 26.50 _reflns_number_total 2442 _reflns_number_gt 2047 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/RIGAKU Diffractometer Control' _computing_cell_refinement ' " ' _computing_data_reduction 'Texsan' _computing_structure_solution 'SIR' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II' _computing_publication_material 'SHELXL-97' _refine_special_details ; The final model included a occupancy factor for mutual substitutional disorder of the Zn and Li sites (refined to 5.1(3)%). Data collected from several crystals,from different reaction batches, all showed similar disorder, varying only in degree (ca. 2 to 10%). 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 w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+9.5667P] 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 2442 _refine_ls_number_parameters 105 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1441 _refine_ls_wR_factor_gt 0.1345 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.5000 0.02697(10) 0.7500 0.0229(2) Uani 0.949(3) d SP . . Li1 Li 0.5000 0.02697(10) 0.7500 0.0229(2) Uani 0.051(3) d SP . . Si1 Si 0.60211(7) 0.16911(19) 0.88685(5) 0.0278(3) Uani 1 d . . . Si2 Si 0.41974(7) 0.2521(2) 0.84310(5) 0.0287(3) Uani 1 d . . . N1 N 0.51022(19) 0.2120(5) 0.82460(15) 0.0232(7) Uani 1 d . . . C1 C 0.5000 -0.2592(10) 0.7500 0.0391(16) Uani 1 d S . . H1A H 0.5277 -0.3060 0.7934 0.059 Uiso 0.50 calc PR . . H1B H 0.5283 -0.3060 0.7209 0.059 Uiso 0.50 calc PR . . H1C H 0.4440 -0.3060 0.7357 0.059 Uiso 0.50 calc PR . . C2 C 0.5902(3) 0.0113(9) 0.9542(2) 0.0466(14) Uani 1 d . . . H2A H 0.5617 0.0829 0.9788 0.070 Uiso 1 calc R . . H2B H 0.6439 -0.0265 0.9825 0.070 Uiso 1 calc R . . H2C H 0.5590 -0.1034 0.9358 0.070 Uiso 1 calc R . . C3 C 0.6774(3) 0.0306(9) 0.8561(3) 0.0468(13) Uani 1 d . . . H3A H 0.6614 -0.1045 0.8503 0.070 Uiso 1 calc R . . H3B H 0.7319 0.0410 0.8872 0.070 Uiso 1 calc R . . H3C H 0.6775 0.0844 0.8150 0.070 Uiso 1 calc R . . C4 C 0.6519(3) 0.4063(8) 0.9225(3) 0.0457(13) Uani 1 d . . . H4A H 0.6649 0.4806 0.8893 0.069 Uiso 1 calc R . . H4B H 0.7017 0.3799 0.9578 0.069 Uiso 1 calc R . . H4C H 0.6144 0.4794 0.9387 0.069 Uiso 1 calc R . . C5 C 0.3677(3) 0.0180(8) 0.8522(2) 0.0426(12) Uani 1 d . . . H5A H 0.3548 -0.0552 0.8122 0.064 Uiso 1 calc R . . H5B H 0.3176 0.0463 0.8618 0.064 Uiso 1 calc R . . H5C H 0.4039 -0.0574 0.8872 0.064 Uiso 1 calc R . . C6 C 0.3439(3) 0.3965(9) 0.7756(2) 0.0434(13) Uani 1 d . . . H6A H 0.3494 0.5331 0.7862 0.065 Uiso 1 calc R . . H6B H 0.2886 0.3545 0.7709 0.065 Uiso 1 calc R . . H6C H 0.3553 0.3751 0.7352 0.065 Uiso 1 calc R . . C7 C 0.4338(3) 0.4036(8) 0.9180(2) 0.0429(12) Uani 1 d . . . H7A H 0.4684 0.3349 0.9556 0.064 Uiso 1 calc R . . H7B H 0.3808 0.4282 0.9234 0.064 Uiso 1 calc R . . H7C H 0.4593 0.5256 0.9136 0.064 Uiso 1 calc R . . Li2 Li 0.5000 0.3849(14) 0.7500 0.049(3) Uani 0.949(3) d SP . . Zn2 Zn 0.5000 0.3849(14) 0.7500 0.049(3) Uani 0.051(3) d SP . . 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 0.0235(4) 0.0248(4) 0.0245(4) 0.000 0.0136(3) 0.000 Li1 0.0235(4) 0.0248(4) 0.0245(4) 0.000 0.0136(3) 0.000 Si1 0.0189(5) 0.0424(7) 0.0236(6) 0.0045(5) 0.0086(4) 0.0019(5) Si2 0.0187(5) 0.0475(8) 0.0217(6) -0.0056(5) 0.0089(4) 0.0020(5) N1 0.0202(15) 0.0340(19) 0.0168(15) -0.0004(14) 0.0080(13) 0.0048(14) C1 0.049(4) 0.045(4) 0.028(3) 0.000 0.018(3) 0.000 C2 0.034(2) 0.075(4) 0.032(2) 0.020(3) 0.011(2) 0.002(3) C3 0.030(2) 0.068(4) 0.046(3) 0.011(3) 0.018(2) 0.017(2) C4 0.028(2) 0.058(3) 0.046(3) -0.006(3) 0.004(2) -0.008(2) C5 0.027(2) 0.065(3) 0.039(2) -0.007(2) 0.015(2) -0.010(2) C6 0.026(2) 0.071(4) 0.034(2) -0.006(2) 0.0112(19) 0.018(2) C7 0.035(2) 0.069(3) 0.025(2) -0.014(2) 0.0111(19) 0.009(2) Li2 0.036(4) 0.088(6) 0.022(3) 0.000 0.008(3) 0.000 Zn2 0.036(4) 0.088(6) 0.022(3) 0.000 0.008(3) 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 C1 1.957(7) . ? Zn1 N1 2.010(3) 2_656 ? Zn1 N1 2.010(3) . ? Zn1 Li2 2.448(10) . ? Si1 N1 1.734(3) . ? Si1 C2 1.871(5) . ? Si1 C3 1.877(5) . ? Si1 C4 1.878(6) . ? Si2 N1 1.732(3) . ? Si2 C7 1.870(5) . ? Si2 C5 1.871(6) . ? Si2 C6 1.890(5) . ? Si2 Li2 2.909(4) . ? N1 Li2 1.959(7) . ? Li2 N1 1.959(7) 2_656 ? Li2 C1 2.435(12) 1_565 ? Li2 Si2 2.909(3) 2_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 C1 Zn1 N1 129.02(10) . 2_656 ? C1 Zn1 N1 129.02(10) . . ? N1 Zn1 N1 102.0(2) 2_656 . ? C1 Zn1 Li2 180.000(6) . . ? N1 Zn1 Li2 50.98(10) 2_656 . ? N1 Zn1 Li2 50.98(10) . . ? N1 Si1 C2 113.9(2) . . ? N1 Si1 C3 111.3(2) . . ? C2 Si1 C3 103.7(3) . . ? N1 Si1 C4 110.5(2) . . ? C2 Si1 C4 109.0(3) . . ? C3 Si1 C4 108.1(3) . . ? N1 Si2 C7 114.0(2) . . ? N1 Si2 C5 112.0(2) . . ? C7 Si2 C5 108.6(2) . . ? N1 Si2 C6 110.26(18) . . ? C7 Si2 C6 104.2(2) . . ? C5 Si2 C6 107.3(2) . . ? N1 Si2 Li2 40.82(16) . . ? C7 Si2 Li2 117.6(2) . . ? C5 Si2 Li2 133.0(2) . . ? C6 Si2 Li2 70.21(18) . . ? Si2 N1 Si1 119.99(19) . . ? Si2 N1 Li2 103.86(19) . . ? Si1 N1 Li2 124.1(2) . . ? Si2 N1 Zn1 115.21(18) . . ? Si1 N1 Zn1 109.92(17) . . ? Li2 N1 Zn1 76.1(3) . . ? N1 Li2 N1 105.7(5) 2_656 . ? N1 Li2 C1 127.1(2) 2_656 1_565 ? N1 Li2 C1 127.1(2) . 1_565 ? N1 Li2 Zn1 52.9(2) 2_656 . ? N1 Li2 Zn1 52.9(2) . . ? C1 Li2 Zn1 179.999(2) 1_565 . ? N1 Li2 Si2 116.0(4) 2_656 . ? N1 Li2 Si2 35.32(10) . . ? C1 Li2 Si2 108.19(18) 1_565 . ? Zn1 Li2 Si2 71.81(18) . . ? N1 Li2 Si2 35.32(10) 2_656 2_656 ? N1 Li2 Si2 116.0(4) . 2_656 ? C1 Li2 Si2 108.20(18) 1_565 2_656 ? Zn1 Li2 Si2 71.81(18) . 2_656 ? Si2 Li2 Si2 143.6(4) . 2_656 ? 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 C7 Si2 N1 Si1 39.0(3) . . . . ? C5 Si2 N1 Si1 -84.9(3) . . . . ? C6 Si2 N1 Si1 155.7(3) . . . . ? Li2 Si2 N1 Si1 144.1(4) . . . . ? C7 Si2 N1 Li2 -105.1(3) . . . . ? C5 Si2 N1 Li2 131.0(3) . . . . ? C6 Si2 N1 Li2 11.7(3) . . . . ? C7 Si2 N1 Zn1 173.9(2) . . . . ? C5 Si2 N1 Zn1 50.0(3) . . . . ? C6 Si2 N1 Zn1 -69.3(3) . . . . ? Li2 Si2 N1 Zn1 -81.0(3) . . . . ? C2 Si1 N1 Si2 39.3(3) . . . . ? C3 Si1 N1 Si2 156.1(3) . . . . ? C4 Si1 N1 Si2 -83.8(3) . . . . ? C2 Si1 N1 Li2 175.8(4) . . . . ? C3 Si1 N1 Li2 -67.4(4) . . . . ? C4 Si1 N1 Li2 52.6(4) . . . . ? C2 Si1 N1 Zn1 -97.8(3) . . . . ? C3 Si1 N1 Zn1 19.0(3) . . . . ? C4 Si1 N1 Zn1 139.1(2) . . . . ? C1 Zn1 N1 Si2 -81.0(2) . . . . ? N1 Zn1 N1 Si2 99.0(2) 2_656 . . . ? Li2 Zn1 N1 Si2 99.0(2) . . . . ? C1 Zn1 N1 Si1 58.3(2) . . . . ? N1 Zn1 N1 Si1 -121.7(2) 2_656 . . . ? Li2 Zn1 N1 Si1 -121.7(2) . . . . ? C1 Zn1 N1 Li2 180.000(4) . . . . ? N1 Zn1 N1 Li2 -0.003(3) 2_656 . . . ? Si2 N1 Li2 N1 -113.01(19) . . . 2_656 ? Si1 N1 Li2 N1 104.9(3) . . . 2_656 ? Zn1 N1 Li2 N1 0.003(2) . . . 2_656 ? Si2 N1 Li2 C1 66.98(19) . . . 1_565 ? Si1 N1 Li2 C1 -75.1(3) . . . 1_565 ? Zn1 N1 Li2 C1 179.999(4) . . . 1_565 ? Si2 N1 Li2 Zn1 -113.02(19) . . . . ? Si1 N1 Li2 Zn1 104.9(3) . . . . ? Si1 N1 Li2 Si2 -142.1(4) . . . . ? Zn1 N1 Li2 Si2 113.02(19) . . . . ? Si2 N1 Li2 Si2 -149.33(16) . . . 2_656 ? Si1 N1 Li2 Si2 68.6(4) . . . 2_656 ? Zn1 N1 Li2 Si2 -36.3(2) . . . 2_656 ? C1 Zn1 Li2 N1 78(100) . . . 2_656 ? N1 Zn1 Li2 N1 180.004(2) . . . 2_656 ? C1 Zn1 Li2 N1 -102(100) . . . . ? N1 Zn1 Li2 N1 179.996(2) 2_656 . . . ? C1 Zn1 Li2 C1 180(100) . . . 1_565 ? N1 Zn1 Li2 C1 102(76) 2_656 . . 1_565 ? N1 Zn1 Li2 C1 -78(76) . . . 1_565 ? C1 Zn1 Li2 Si2 -136(100) . . . . ? N1 Zn1 Li2 Si2 145.93(12) 2_656 . . . ? N1 Zn1 Li2 Si2 -34.07(12) . . . . ? C1 Zn1 Li2 Si2 44(100) . . . 2_656 ? N1 Zn1 Li2 Si2 -34.07(12) 2_656 . . 2_656 ? N1 Zn1 Li2 Si2 145.93(12) . . . 2_656 ? N1 Si2 Li2 N1 80.4(4) . . . 2_656 ? C7 Si2 Li2 N1 175.9(2) . . . 2_656 ? C5 Si2 Li2 N1 7.5(4) . . . 2_656 ? C6 Si2 Li2 N1 -88.0(3) . . . 2_656 ? C7 Si2 Li2 N1 95.6(3) . . . . ? C5 Si2 Li2 N1 -72.9(3) . . . . ? C6 Si2 Li2 N1 -168.4(3) . . . . ? N1 Si2 Li2 C1 -129.4(2) . . . 1_565 ? C7 Si2 Li2 C1 -33.86(19) . . . 1_565 ? C5 Si2 Li2 C1 157.7(2) . . . 1_565 ? C6 Si2 Li2 C1 62.21(19) . . . 1_565 ? N1 Si2 Li2 Zn1 50.6(2) . . . . ? C7 Si2 Li2 Zn1 146.14(19) . . . . ? C5 Si2 Li2 Zn1 -22.3(2) . . . . ? C6 Si2 Li2 Zn1 -117.79(19) . . . . ? N1 Si2 Li2 Si2 50.6(2) . . . 2_656 ? C7 Si2 Li2 Si2 146.14(19) . . . 2_656 ? C5 Si2 Li2 Si2 -22.3(2) . . . 2_656 ? C6 Si2 Li2 Si2 -117.8(2) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.454 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.454 _refine_diff_density_max 0.857 _refine_diff_density_min -0.780 _refine_diff_density_rms 0.109 #-----------------------DATA FOR COMPOUND 1----------------------------- data_znna _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H72 N4 Na2 O Si8 Zn2' _chemical_formula_weight 834.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Zn' 'Zn' 0.2839 1.4301 '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' 'Na' 'Na' 0.0362 0.0249 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 10.711(6) _cell_length_b 12.810(6) _cell_length_c 8.970(4) _cell_angle_alpha 108.96(3) _cell_angle_beta 99.77(4) _cell_angle_gamma 96.13(4) _cell_volume 1129.6(9) _cell_formula_units_Z 1 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.51 _cell_measurement_theta_max 20.01 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 446 _exptl_absorpt_coefficient_mu 1.316 _exptl_absorpt_correction_type 'psi scans' _exptl_absorpt_correction_T_min '0.735' _exptl_absorpt_correction_T_max '1.000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method '\w/2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.470 _diffrn_reflns_number 6914 _diffrn_reflns_av_R_equivalents 0.0134 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 30.04 _reflns_number_total 6590 _reflns_number_gt 5530 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/Rigaku Diffractometer Control' _computing_cell_refinement ' " ' _computing_data_reduction 'Texsan' _computing_structure_solution 'SIR' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II' _computing_publication_material 'SHELXL-97' _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 w=1/[\s^2^(Fo^2^)+(0.0723P)^2^+0.7678P] 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 6590 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1305 _refine_ls_wR_factor_gt 0.1231 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn -0.01942(2) 0.14621(2) 0.11420(3) 0.02145(8) Uani 1 d . . . Si1 Si 0.18413(7) 0.24818(6) 0.44270(8) 0.02651(14) Uani 1 d . . . Si2 Si 0.20649(7) 0.34386(6) 0.18103(8) 0.02640(14) Uani 1 d . . . Si3 Si -0.28648(7) 0.16345(6) 0.21272(8) 0.02720(14) Uani 1 d . . . Si4 Si -0.24974(7) 0.20525(6) -0.09242(9) 0.02886(15) Uani 1 d . . . Na1 Na 0.21595(10) 0.05589(9) 0.08224(15) 0.0362(2) Uani 1 d . . . O1 O 0.0000 0.0000 0.0000 0.0340(6) Uani 1 d S . . N1 N 0.15029(19) 0.23685(16) 0.2424(2) 0.0247(4) Uani 1 d . . . N2 N -0.20388(18) 0.15761(17) 0.0632(2) 0.0247(4) Uani 1 d . . . C1 C 0.0858(3) 0.1282(3) 0.4683(4) 0.0419(6) Uani 1 d . . . H1A H -0.0042 0.1385 0.4575 0.063 Uiso 1 calc R . . H1B H 0.1181 0.1252 0.5756 0.063 Uiso 1 calc R . . H1C H 0.0920 0.0581 0.3854 0.063 Uiso 1 calc R . . C2 C 0.1506(4) 0.3813(3) 0.5829(4) 0.0466(7) Uani 1 d . . . H2A H 0.2227 0.4421 0.6055 0.070 Uiso 1 calc R . . H2B H 0.1398 0.3714 0.6841 0.070 Uiso 1 calc R . . H2C H 0.0717 0.4000 0.5324 0.070 Uiso 1 calc R . . C3 C 0.3568(3) 0.2407(3) 0.5191(4) 0.0454(7) Uani 1 d . . . H3A H 0.3775 0.1700 0.4531 0.068 Uiso 1 calc R . . H3B H 0.3695 0.2448 0.6318 0.068 Uiso 1 calc R . . H3C H 0.4134 0.3036 0.5122 0.068 Uiso 1 calc R . . C4 C 0.0901(3) 0.4434(2) 0.1827(4) 0.0412(6) Uani 1 d . . . H4A H 0.0024 0.4008 0.1376 0.062 Uiso 1 calc R . . H4B H 0.1107 0.4884 0.1174 0.062 Uiso 1 calc R . . H4C H 0.0962 0.4929 0.2940 0.062 Uiso 1 calc R . . C5 C 0.3640(3) 0.4317(3) 0.3091(4) 0.0437(7) Uani 1 d . . . H5A H 0.3537 0.4690 0.4194 0.066 Uiso 1 calc R . . H5B H 0.3913 0.4882 0.2639 0.066 Uiso 1 calc R . . H5C H 0.4292 0.3836 0.3109 0.066 Uiso 1 calc R . . C6 C 0.2376(3) 0.2827(3) -0.0271(3) 0.0391(6) Uani 1 d . . . H6A H 0.3135 0.2465 -0.0216 0.059 Uiso 1 calc R . . H6B H 0.2528 0.3426 -0.0710 0.059 Uiso 1 calc R . . H6C H 0.1628 0.2272 -0.0972 0.059 Uiso 1 calc R . . C7 C -0.2291(4) 0.2930(3) 0.3943(4) 0.0497(8) Uani 1 d . . . H7A H -0.1374 0.2980 0.4375 0.074 Uiso 1 calc R . . H7B H -0.2778 0.2904 0.4766 0.074 Uiso 1 calc R . . H7C H -0.2420 0.3587 0.3642 0.074 Uiso 1 calc R . . C8 C -0.2701(3) 0.0386(3) 0.2774(4) 0.0399(6) Uani 1 d . . . H8A H -0.3255 -0.0283 0.1956 0.060 Uiso 1 calc R . . H8B H -0.2958 0.0520 0.3809 0.060 Uiso 1 calc R . . H8C H -0.1804 0.0272 0.2893 0.060 Uiso 1 calc R . . C9 C -0.4651(3) 0.1569(3) 0.1458(4) 0.0426(6) Uani 1 d . . . H9A H -0.4801 0.2240 0.1203 0.064 Uiso 1 calc R . . H9B H -0.5078 0.1534 0.2328 0.064 Uiso 1 calc R . . H9C H -0.5000 0.0900 0.0496 0.064 Uiso 1 calc R . . C10 C -0.3043(4) 0.3448(3) -0.0285(5) 0.0539(9) Uani 1 d . . . H10A H -0.3846 0.3369 0.0085 0.081 Uiso 1 calc R . . H10B H -0.3186 0.3708 -0.1204 0.081 Uiso 1 calc R . . H10C H -0.2380 0.3992 0.0596 0.081 Uiso 1 calc R . . C11 C -0.1143(3) 0.2172(3) -0.1963(4) 0.0408(6) Uani 1 d . . . H11A H -0.0476 0.2808 -0.1261 0.061 Uiso 1 calc R . . H11B H -0.1465 0.2290 -0.2975 0.061 Uiso 1 calc R . . H11C H -0.0779 0.1481 -0.2196 0.061 Uiso 1 calc R . . C12 C -0.3833(3) 0.1030(4) -0.2547(4) 0.0538(9) Uani 1 d . . . H12A H -0.3540 0.0318 -0.2998 0.081 Uiso 1 calc R . . H12B H -0.4079 0.1334 -0.3405 0.081 Uiso 1 calc R . . H12C H -0.4578 0.0907 -0.2085 0.081 Uiso 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 0.02130(13) 0.01991(13) 0.02102(13) 0.00538(9) 0.00314(9) 0.00274(9) Si1 0.0298(3) 0.0260(3) 0.0207(3) 0.0067(2) 0.0018(2) 0.0028(2) Si2 0.0271(3) 0.0235(3) 0.0263(3) 0.0092(2) 0.0017(2) -0.0003(2) Si3 0.0270(3) 0.0298(3) 0.0255(3) 0.0086(2) 0.0080(2) 0.0074(2) Si4 0.0249(3) 0.0339(3) 0.0312(3) 0.0167(3) 0.0041(2) 0.0061(3) Na1 0.0255(5) 0.0274(5) 0.0458(6) 0.0015(4) 0.0044(4) 0.0043(4) O1 0.0277(12) 0.0219(11) 0.0400(14) -0.0020(10) 0.0025(10) 0.0015(9) N1 0.0252(9) 0.0235(9) 0.0204(8) 0.0062(7) -0.0008(7) -0.0033(7) N2 0.0199(8) 0.0292(9) 0.0268(9) 0.0109(7) 0.0053(7) 0.0085(7) C1 0.0514(17) 0.0406(15) 0.0348(13) 0.0187(12) 0.0071(12) -0.0020(13) C2 0.066(2) 0.0378(15) 0.0291(13) 0.0010(11) 0.0100(13) 0.0125(14) C3 0.0363(15) 0.064(2) 0.0366(14) 0.0225(14) -0.0011(11) 0.0099(14) C4 0.0431(15) 0.0320(13) 0.0474(16) 0.0143(12) 0.0042(12) 0.0093(11) C5 0.0367(14) 0.0365(14) 0.0486(16) 0.0154(12) -0.0054(12) -0.0106(11) C6 0.0376(14) 0.0513(17) 0.0335(13) 0.0196(12) 0.0103(11) 0.0105(12) C7 0.063(2) 0.0403(16) 0.0370(15) 0.0022(12) 0.0129(14) 0.0075(15) C8 0.0369(14) 0.0447(15) 0.0432(15) 0.0249(13) 0.0057(11) 0.0029(12) C9 0.0293(13) 0.0584(18) 0.0475(16) 0.0225(14) 0.0147(12) 0.0156(12) C10 0.059(2) 0.0499(19) 0.075(2) 0.0397(18) 0.0262(18) 0.0291(16) C11 0.0360(14) 0.0557(18) 0.0348(13) 0.0215(13) 0.0091(11) 0.0041(12) C12 0.0416(17) 0.072(2) 0.0417(16) 0.0267(16) -0.0086(13) -0.0108(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.8733(9) . ? Zn1 N2 1.983(2) . ? Zn1 N1 1.986(2) . ? Zn1 Na1 2.9033(18) . ? Zn1 Na1 2.975(2) 2 ? Si1 N1 1.726(2) . ? Si1 C1 1.868(3) . ? Si1 C2 1.873(3) . ? Si1 C3 1.884(3) . ? Si1 Na1 3.466(2) . ? Si2 N1 1.723(2) . ? Si2 C4 1.874(3) . ? Si2 C6 1.878(3) . ? Si2 C5 1.878(3) . ? Si2 Na1 3.520(2) . ? Si3 N2 1.714(2) . ? Si3 C7 1.863(3) . ? Si3 C8 1.885(3) . ? Si3 C9 1.890(3) . ? Si3 Na1 3.430(2) 2 ? Si4 N2 1.716(2) . ? Si4 C11 1.871(3) . ? Si4 C10 1.880(3) . ? Si4 C12 1.880(4) . ? Si4 Na1 3.432(2) 2 ? Na1 O1 2.2651(17) . ? Na1 N1 2.541(3) . ? Na1 N2 2.597(3) 2 ? Na1 Zn1 2.975(2) 2 ? Na1 Si3 3.430(2) 2 ? Na1 Si4 3.432(2) 2 ? O1 Zn1 1.8733(9) 2 ? O1 Na1 2.2651(17) 2 ? N2 Na1 2.597(3) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 N2 108.38(8) . . ? O1 Zn1 N1 110.03(8) . . ? N2 Zn1 N1 141.58(9) . . ? O1 Zn1 Na1 51.25(4) . . ? N2 Zn1 Na1 158.61(7) . . ? N1 Zn1 Na1 59.14(7) . . ? O1 Zn1 Na1 49.56(4) . 2 ? N2 Zn1 Na1 59.23(7) . 2 ? N1 Zn1 Na1 158.75(7) . 2 ? Na1 Zn1 Na1 100.82(5) . 2 ? N1 Si1 C1 109.53(12) . . ? N1 Si1 C2 113.57(13) . . ? C1 Si1 C2 108.01(17) . . ? N1 Si1 C3 113.18(13) . . ? C1 Si1 C3 105.68(16) . . ? C2 Si1 C3 106.45(17) . . ? N1 Si1 Na1 44.50(8) . . ? C1 Si1 Na1 86.10(11) . . ? C2 Si1 Na1 157.92(11) . . ? C3 Si1 Na1 85.05(12) . . ? N1 Si2 C4 111.66(13) . . ? N1 Si2 C6 109.28(13) . . ? C4 Si2 C6 110.12(15) . . ? N1 Si2 C5 114.37(13) . . ? C4 Si2 C5 106.07(16) . . ? C6 Si2 C5 105.09(16) . . ? N1 Si2 Na1 42.80(8) . . ? C4 Si2 Na1 141.31(11) . . ? C6 Si2 Na1 69.30(11) . . ? C5 Si2 Na1 111.37(12) . . ? N2 Si3 C7 113.22(15) . . ? N2 Si3 C8 109.53(13) . . ? C7 Si3 C8 108.31(16) . . ? N2 Si3 C9 113.36(13) . . ? C7 Si3 C9 106.29(17) . . ? C8 Si3 C9 105.74(15) . . ? N2 Si3 Na1 47.42(8) . 2 ? C7 Si3 Na1 148.99(13) . 2 ? C8 Si3 Na1 67.90(11) . 2 ? C9 Si3 Na1 104.22(12) . 2 ? N2 Si4 C11 110.31(12) . . ? N2 Si4 C10 114.07(15) . . ? C11 Si4 C10 108.15(17) . . ? N2 Si4 C12 111.73(14) . . ? C11 Si4 C12 104.58(17) . . ? C10 Si4 C12 107.5(2) . . ? N2 Si4 Na1 47.39(8) . 2 ? C11 Si4 Na1 94.85(12) . 2 ? C10 Si4 Na1 155.52(12) . 2 ? C12 Si4 Na1 73.46(14) . 2 ? O1 Na1 N1 82.09(7) . . ? O1 Na1 N2 79.75(7) . 2 ? N1 Na1 N2 158.96(8) . 2 ? O1 Na1 Zn1 40.17(3) . . ? N1 Na1 Zn1 42.14(6) . . ? N2 Na1 Zn1 119.73(7) 2 . ? O1 Na1 Zn1 39.01(4) . 2 ? N1 Na1 Zn1 120.94(7) . 2 ? N2 Na1 Zn1 40.99(5) 2 2 ? Zn1 Na1 Zn1 79.18(5) . 2 ? O1 Na1 Si3 94.82(6) . 2 ? N1 Na1 Si3 165.47(7) . 2 ? N2 Na1 Si3 29.08(5) 2 2 ? Zn1 Na1 Si3 132.10(5) . 2 ? Zn1 Na1 Si3 58.25(4) 2 2 ? O1 Na1 Si4 90.06(6) . 2 ? N1 Na1 Si4 141.28(7) . 2 ? N2 Na1 Si4 29.10(5) 2 2 ? Zn1 Na1 Si4 122.85(5) . 2 ? Zn1 Na1 Si4 58.14(4) 2 2 ? Si3 Na1 Si4 52.49(4) 2 2 ? O1 Na1 Si1 91.52(6) . . ? N1 Na1 Si1 28.43(5) . . ? N2 Na1 Si1 141.67(7) 2 . ? Zn1 Na1 Si1 58.24(5) . . ? Zn1 Na1 Si1 123.65(5) 2 . ? Si3 Na1 Si1 165.90(4) 2 . ? Si4 Na1 Si1 115.05(5) 2 . ? O1 Na1 Si2 95.26(6) . . ? N1 Na1 Si2 27.44(5) . . ? N2 Na1 Si2 165.78(7) 2 . ? Zn1 Na1 Si2 57.50(4) . . ? Zn1 Na1 Si2 131.61(5) 2 . ? Si3 Na1 Si2 140.32(5) 2 . ? Si4 Na1 Si2 165.12(4) 2 . ? Si1 Na1 Si2 51.05(3) . . ? Zn1 O1 Zn1 180.0 2 . ? Zn1 O1 Na1 88.58(6) 2 2 ? Zn1 O1 Na1 91.42(6) . 2 ? Zn1 O1 Na1 91.42(6) 2 . ? Zn1 O1 Na1 88.58(6) . . ? Na1 O1 Na1 180.0 2 . ? Si2 N1 Si1 121.58(12) . . ? Si2 N1 Zn1 115.25(11) . . ? Si1 N1 Zn1 115.24(11) . . ? Si2 N1 Na1 109.76(11) . . ? Si1 N1 Na1 107.08(10) . . ? Zn1 N1 Na1 78.72(8) . . ? Si3 N2 Si4 124.34(12) . . ? Si3 N2 Zn1 116.23(11) . . ? Si4 N2 Zn1 115.88(11) . . ? Si3 N2 Na1 103.50(10) . 2 ? Si4 N2 Na1 103.51(10) . 2 ? Zn1 N2 Na1 79.78(8) . 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 Zn1 Na1 O1 -19.92(18) . . . . ? N1 Zn1 Na1 O1 172.39(7) . . . . ? Na1 Zn1 Na1 O1 0.0 2 . . . ? O1 Zn1 Na1 N1 -172.39(7) . . . . ? N2 Zn1 Na1 N1 167.69(18) . . . . ? Na1 Zn1 Na1 N1 -172.39(7) 2 . . . ? O1 Zn1 Na1 N2 -6.27(6) . . . 2 ? N2 Zn1 Na1 N2 -26.2(2) . . . 2 ? N1 Zn1 Na1 N2 166.12(10) . . . 2 ? Na1 Zn1 Na1 N2 -6.27(6) 2 . . 2 ? O1 Zn1 Na1 Zn1 0.0 . . . 2 ? N2 Zn1 Na1 Zn1 -19.92(18) . . . 2 ? N1 Zn1 Na1 Zn1 172.39(7) . . . 2 ? Na1 Zn1 Na1 Zn1 0.0 2 . . 2 ? O1 Zn1 Na1 Si3 26.55(4) . . . 2 ? N2 Zn1 Na1 Si3 6.6(2) . . . 2 ? N1 Zn1 Na1 Si3 -161.06(9) . . . 2 ? Na1 Zn1 Na1 Si3 26.55(4) 2 . . 2 ? O1 Zn1 Na1 Si4 -40.28(4) . . . 2 ? N2 Zn1 Na1 Si4 -60.20(19) . . . 2 ? N1 Zn1 Na1 Si4 132.11(9) . . . 2 ? Na1 Zn1 Na1 Si4 -40.28(4) 2 . . 2 ? O1 Zn1 Na1 Si1 -141.42(4) . . . . ? N2 Zn1 Na1 Si1 -161.34(17) . . . . ? N1 Zn1 Na1 Si1 30.97(7) . . . . ? Na1 Zn1 Na1 Si1 -141.42(4) 2 . . . ? O1 Zn1 Na1 Si2 157.41(4) . . . . ? N2 Zn1 Na1 Si2 137.49(18) . . . . ? N1 Zn1 Na1 Si2 -30.20(7) . . . . ? Na1 Zn1 Na1 Si2 157.41(4) 2 . . . ? N1 Si1 Na1 O1 -70.23(11) . . . . ? C1 Si1 Na1 O1 52.96(12) . . . . ? C2 Si1 Na1 O1 -78.0(3) . . . . ? C3 Si1 Na1 O1 159.09(12) . . . . ? C1 Si1 Na1 N1 123.20(15) . . . . ? C2 Si1 Na1 N1 -7.8(3) . . . . ? C3 Si1 Na1 N1 -130.68(15) . . . . ? N1 Si1 Na1 N2 -145.56(14) . . . 2 ? C1 Si1 Na1 N2 -22.37(14) . . . 2 ? C2 Si1 Na1 N2 -153.4(3) . . . 2 ? C3 Si1 Na1 N2 83.76(15) . . . 2 ? N1 Si1 Na1 Zn1 -46.50(10) . . . . ? C1 Si1 Na1 Zn1 76.69(12) . . . . ? C2 Si1 Na1 Zn1 -54.3(3) . . . . ? C3 Si1 Na1 Zn1 -177.18(11) . . . . ? N1 Si1 Na1 Zn1 -93.88(11) . . . 2 ? C1 Si1 Na1 Zn1 29.31(12) . . . 2 ? C2 Si1 Na1 Zn1 -101.7(3) . . . 2 ? C3 Si1 Na1 Zn1 135.44(12) . . . 2 ? N1 Si1 Na1 Si3 172.9(2) . . . 2 ? C1 Si1 Na1 Si3 -63.9(2) . . . 2 ? C2 Si1 Na1 Si3 165.1(3) . . . 2 ? C3 Si1 Na1 Si3 42.3(2) . . . 2 ? N1 Si1 Na1 Si4 -161.01(11) . . . 2 ? C1 Si1 Na1 Si4 -37.81(12) . . . 2 ? C2 Si1 Na1 Si4 -168.8(3) . . . 2 ? C3 Si1 Na1 Si4 68.32(12) . . . 2 ? N1 Si1 Na1 Si2 25.30(10) . . . . ? C1 Si1 Na1 Si2 148.50(11) . . . . ? C2 Si1 Na1 Si2 17.5(3) . . . . ? C3 Si1 Na1 Si2 -105.37(12) . . . . ? N1 Si2 Na1 O1 61.50(11) . . . . ? C4 Si2 Na1 O1 0.13(18) . . . . ? C6 Si2 Na1 O1 -96.56(12) . . . . ? C5 Si2 Na1 O1 164.76(12) . . . . ? C4 Si2 Na1 N1 -61.4(2) . . . . ? C6 Si2 Na1 N1 -158.05(14) . . . . ? C5 Si2 Na1 N1 103.26(16) . . . . ? N1 Si2 Na1 N2 130.2(3) . . . 2 ? C4 Si2 Na1 N2 68.8(3) . . . 2 ? C6 Si2 Na1 N2 -27.9(3) . . . 2 ? C5 Si2 Na1 N2 -126.6(3) . . . 2 ? N1 Si2 Na1 Zn1 47.09(10) . . . . ? C4 Si2 Na1 Zn1 -14.28(18) . . . . ? C6 Si2 Na1 Zn1 -110.96(11) . . . . ? C5 Si2 Na1 Zn1 150.35(12) . . . . ? N1 Si2 Na1 Zn1 77.39(11) . . . 2 ? C4 Si2 Na1 Zn1 16.02(19) . . . 2 ? C6 Si2 Na1 Zn1 -80.66(12) . . . 2 ? C5 Si2 Na1 Zn1 -179.35(12) . . . 2 ? N1 Si2 Na1 Si3 165.58(12) . . . 2 ? C4 Si2 Na1 Si3 104.21(18) . . . 2 ? C6 Si2 Na1 Si3 7.53(11) . . . 2 ? C5 Si2 Na1 Si3 -91.16(14) . . . 2 ? N1 Si2 Na1 Si4 -49.03(18) . . . 2 ? C4 Si2 Na1 Si4 -110.4(2) . . . 2 ? C6 Si2 Na1 Si4 152.92(19) . . . 2 ? C5 Si2 Na1 Si4 54.2(2) . . . 2 ? N1 Si2 Na1 Si1 -26.20(10) . . . . ? C4 Si2 Na1 Si1 -87.57(18) . . . . ? C6 Si2 Na1 Si1 175.74(11) . . . . ? C5 Si2 Na1 Si1 77.06(13) . . . . ? N2 Zn1 O1 Zn1 -70.4(12) . . . 2 ? N1 Zn1 O1 Zn1 110.2(12) . . . 2 ? Na1 Zn1 O1 Zn1 117.2(12) . . . 2 ? Na1 Zn1 O1 Zn1 -62.8(12) 2 . . 2 ? N2 Zn1 O1 Na1 -7.53(7) . . . 2 ? N1 Zn1 O1 Na1 173.05(7) . . . 2 ? Na1 Zn1 O1 Na1 180.0 . . . 2 ? N2 Zn1 O1 Na1 172.47(7) . . . . ? N1 Zn1 O1 Na1 -6.95(7) . . . . ? Na1 Zn1 O1 Na1 180.0 2 . . . ? N1 Na1 O1 Zn1 -174.85(5) . . . 2 ? N2 Na1 O1 Zn1 -5.53(5) 2 . . 2 ? Zn1 Na1 O1 Zn1 180.0 . . . 2 ? Si3 Na1 O1 Zn1 19.44(3) 2 . . 2 ? Si4 Na1 O1 Zn1 -32.90(3) 2 . . 2 ? Si1 Na1 O1 Zn1 -147.96(3) . . . 2 ? Si2 Na1 O1 Zn1 161.02(3) . . . 2 ? N1 Na1 O1 Zn1 5.15(5) . . . . ? N2 Na1 O1 Zn1 174.47(5) 2 . . . ? Zn1 Na1 O1 Zn1 180.0 2 . . . ? Si3 Na1 O1 Zn1 -160.56(3) 2 . . . ? Si4 Na1 O1 Zn1 147.10(3) 2 . . . ? Si1 Na1 O1 Zn1 32.04(3) . . . . ? Si2 Na1 O1 Zn1 -18.98(3) . . . . ? N1 Na1 O1 Na1 -103(5) . . . 2 ? N2 Na1 O1 Na1 67(5) 2 . . 2 ? Zn1 Na1 O1 Na1 -108(5) . . . 2 ? Zn1 Na1 O1 Na1 72(5) 2 . . 2 ? Si3 Na1 O1 Na1 92(5) 2 . . 2 ? Si4 Na1 O1 Na1 39(5) 2 . . 2 ? Si1 Na1 O1 Na1 -76(5) . . . 2 ? Si2 Na1 O1 Na1 -127(5) . . . 2 ? C4 Si2 N1 Si1 -90.23(18) . . . . ? C6 Si2 N1 Si1 147.69(15) . . . . ? C5 Si2 N1 Si1 30.2(2) . . . . ? Na1 Si2 N1 Si1 125.95(18) . . . . ? C4 Si2 N1 Zn1 57.28(16) . . . . ? C6 Si2 N1 Zn1 -64.79(16) . . . . ? C5 Si2 N1 Zn1 177.74(14) . . . . ? Na1 Si2 N1 Zn1 -86.54(12) . . . . ? C4 Si2 N1 Na1 143.82(13) . . . . ? C6 Si2 N1 Na1 21.74(14) . . . . ? C5 Si2 N1 Na1 -95.73(16) . . . . ? C1 Si1 N1 Si2 170.49(16) . . . . ? C2 Si1 N1 Si2 49.6(2) . . . . ? C3 Si1 N1 Si2 -71.9(2) . . . . ? Na1 Si1 N1 Si2 -127.16(18) . . . . ? C1 Si1 N1 Zn1 22.98(18) . . . . ? C2 Si1 N1 Zn1 -97.86(17) . . . . ? C3 Si1 N1 Zn1 140.60(16) . . . . ? Na1 Si1 N1 Zn1 85.33(12) . . . . ? C1 Si1 N1 Na1 -62.35(16) . . . . ? C2 Si1 N1 Na1 176.81(14) . . . . ? C3 Si1 N1 Na1 55.28(16) . . . . ? O1 Zn1 N1 Si2 112.99(11) . . . . ? N2 Zn1 N1 Si2 -66.13(18) . . . . ? Na1 Zn1 N1 Si2 106.68(13) . . . . ? Na1 Zn1 N1 Si2 127.71(14) 2 . . . ? O1 Zn1 N1 Si1 -97.40(11) . . . . ? N2 Zn1 N1 Si1 83.48(17) . . . . ? Na1 Zn1 N1 Si1 -103.71(13) . . . . ? Na1 Zn1 N1 Si1 -82.7(2) 2 . . . ? O1 Zn1 N1 Na1 6.31(6) . . . . ? N2 Zn1 N1 Na1 -172.81(11) . . . . ? Na1 Zn1 N1 Na1 21.0(2) 2 . . . ? O1 Na1 N1 Si2 -117.93(10) . . . . ? N2 Na1 N1 Si2 -148.5(2) 2 . . . ? Zn1 Na1 N1 Si2 -112.99(12) . . . . ? Zn1 Na1 N1 Si2 -121.71(9) 2 . . . ? Si3 Na1 N1 Si2 -39.3(3) 2 . . . ? Si4 Na1 N1 Si2 161.95(7) 2 . . . ? Si1 Na1 N1 Si2 133.83(16) . . . . ? O1 Na1 N1 Si1 108.24(10) . . . . ? N2 Na1 N1 Si1 77.7(2) 2 . . . ? Zn1 Na1 N1 Si1 113.18(12) . . . . ? Zn1 Na1 N1 Si1 104.46(10) 2 . . . ? Si3 Na1 N1 Si1 -173.15(19) 2 . . . ? Si4 Na1 N1 Si1 28.12(15) 2 . . . ? Si2 Na1 N1 Si1 -133.83(16) . . . . ? O1 Na1 N1 Zn1 -4.95(5) . . . . ? N2 Na1 N1 Zn1 -35.5(2) 2 . . . ? Zn1 Na1 N1 Zn1 -8.72(9) 2 . . . ? Si3 Na1 N1 Zn1 73.7(3) 2 . . . ? Si4 Na1 N1 Zn1 -85.06(10) 2 . . . ? Si1 Na1 N1 Zn1 -113.18(12) . . . . ? Si2 Na1 N1 Zn1 112.99(12) . . . . ? C7 Si3 N2 Si4 -92.2(2) . . . . ? C8 Si3 N2 Si4 146.82(16) . . . . ? C9 Si3 N2 Si4 29.0(2) . . . . ? Na1 Si3 N2 Si4 117.07(18) 2 . . . ? C7 Si3 N2 Zn1 65.63(18) . . . . ? C8 Si3 N2 Zn1 -55.36(16) . . . . ? C9 Si3 N2 Zn1 -173.19(14) . . . . ? Na1 Si3 N2 Zn1 -85.11(12) 2 . . . ? C7 Si3 N2 Na1 150.74(14) . . . 2 ? C8 Si3 N2 Na1 29.75(14) . . . 2 ? C9 Si3 N2 Na1 -88.08(15) . . . 2 ? C11 Si4 N2 Si3 165.53(16) . . . . ? C10 Si4 N2 Si3 43.6(2) . . . . ? C12 Si4 N2 Si3 -78.6(2) . . . . ? Na1 Si4 N2 Si3 -117.06(18) 2 . . . ? C11 Si4 N2 Zn1 7.64(17) . . . . ? C10 Si4 N2 Zn1 -114.30(17) . . . . ? C12 Si4 N2 Zn1 123.52(18) . . . . ? Na1 Si4 N2 Zn1 85.05(12) 2 . . . ? C11 Si4 N2 Na1 -77.41(15) . . . 2 ? C10 Si4 N2 Na1 160.65(15) . . . 2 ? C12 Si4 N2 Na1 38.47(18) . . . 2 ? O1 Zn1 N2 Si3 106.77(11) . . . . ? N1 Zn1 N2 Si3 -74.10(18) . . . . ? Na1 Zn1 N2 Si3 123.04(15) . . . . ? Na1 Zn1 N2 Si3 100.11(13) 2 . . . ? O1 Zn1 N2 Si4 -93.50(11) . . . . ? N1 Zn1 N2 Si4 85.63(16) . . . . ? Na1 Zn1 N2 Si4 -77.2(2) . . . . ? Na1 Zn1 N2 Si4 -100.16(13) 2 . . . ? O1 Zn1 N2 Na1 6.66(6) . . . 2 ? N1 Zn1 N2 Na1 -174.21(10) . . . 2 ? Na1 Zn1 N2 Na1 22.9(2) . . . 2 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.113 _refine_diff_density_min -1.423 _refine_diff_density_rms 0.098 #------------------------DATA FOR COMPOUND 2---------------------------- data_rem294 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H72 K2 N4 O1.82 Si8 Zn2' _chemical_formula_weight 879.64 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' 'K' 'K' 0.2009 0.2494 '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 8.9898(4) _cell_length_b 10.9763(5) _cell_length_c 12.9529(6) _cell_angle_alpha 97.322(2) _cell_angle_beta 108.154(2) _cell_angle_gamma 101.162(2) _cell_volume 1167.11(9) _cell_formula_units_Z 1 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 9259 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 28.44 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 469 _exptl_absorpt_coefficient_mu 1.436 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.489 _exptl_absorpt_correction_T_max 0.591 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10058 _diffrn_reflns_av_R_equivalents 0.0112 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.44 _reflns_number_total 5263 _reflns_number_gt 4753 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXTL and local programs' _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^)+(0.0369P)^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 SHELXL _refine_ls_extinction_coef 0.0047(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5263 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0205 _refine_ls_R_factor_gt 0.0188 _refine_ls_wR_factor_ref 0.0549 _refine_ls_wR_factor_gt 0.0545 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.024 _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 K1 K 0.59619(4) 0.74576(3) 0.56989(2) 0.02930(8) Uani 1 1 d . . . Zn1 Zn 0.617256(17) 0.480649(12) 0.647258(11) 0.01848(5) Uani 1 1 d . . . O1 O 0.5000 0.5000 0.5000 0.018(3) Uani 0.167(7) 2 d SP . 1 O2 O 0.4243(2) 0.50474(13) 0.51744(12) 0.0225(5) Uani 0.833(7) 1 d P . 2 N1 N 0.75617(12) 0.64066(10) 0.74506(9) 0.0199(2) Uani 1 1 d . . . Si1 Si 0.69505(5) 0.69658(3) 0.85132(3) 0.02441(9) Uani 1 1 d . . . C1 C 0.49117(19) 0.73020(15) 0.79194(14) 0.0378(4) Uani 1 1 d . . . H1A H 0.5035 0.8088 0.7636 0.057 Uiso 1 1 calc R . . H1B H 0.4433 0.7394 0.8500 0.057 Uiso 1 1 calc R . . H1C H 0.4206 0.6599 0.7313 0.057 Uiso 1 1 calc R . . C2 C 0.6867(2) 0.58193(15) 0.94573(12) 0.0371(3) Uani 1 1 d . . . H2A H 0.6316 0.4965 0.9014 0.056 Uiso 1 1 calc R . . H2B H 0.6274 0.6064 0.9937 0.056 Uiso 1 1 calc R . . H2C H 0.7968 0.5829 0.9916 0.056 Uiso 1 1 calc R . . C3 C 0.8275(2) 0.85219(15) 0.94111(14) 0.0427(4) Uani 1 1 d . . . H3A H 0.9377 0.8433 0.9747 0.064 Uiso 1 1 calc R . . H3B H 0.7855 0.8773 0.9997 0.064 Uiso 1 1 calc R . . H3C H 0.8284 0.9171 0.8958 0.064 Uiso 1 1 calc R . . Si2 Si 0.95394(4) 0.68205(3) 0.75159(3) 0.02302(8) Uani 1 1 d . . . C4 C 1.10201(18) 0.66556(17) 0.88429(13) 0.0387(4) Uani 1 1 d . . . H4A H 1.1345 0.7448 0.9391 0.058 Uiso 1 1 calc R . . H4B H 1.1974 0.6471 0.8707 0.058 Uiso 1 1 calc R . . H4C H 1.0517 0.5962 0.9126 0.058 Uiso 1 1 calc R . . C5 C 1.0180(2) 0.85083(15) 0.73687(15) 0.0397(4) Uani 1 1 d . . . H5A H 0.9543 0.8609 0.6633 0.060 Uiso 1 1 calc R . . H5B H 1.1329 0.8714 0.7457 0.060 Uiso 1 1 calc R . . H5C H 1.0002 0.9080 0.7939 0.060 Uiso 1 1 calc R . . C6 C 0.98271(18) 0.58347(15) 0.63430(13) 0.0346(3) Uani 1 1 d . . . H6A H 0.9783 0.4970 0.6472 0.052 Uiso 1 1 calc R . . H6B H 1.0880 0.6201 0.6292 0.052 Uiso 1 1 calc R . . H6C H 0.8969 0.5815 0.5649 0.052 Uiso 1 1 calc R . . N2 N 0.56580(13) 0.30315(9) 0.66299(9) 0.0205(2) Uani 1 1 d . . . Si3 Si 0.40638(5) 0.25458(3) 0.70693(3) 0.02476(9) Uani 1 1 d . . . C7 C 0.30003(18) 0.38267(14) 0.71879(14) 0.0351(3) Uani 1 1 d . . . H7A H 0.3689 0.4509 0.7818 0.053 Uiso 1 1 calc R . . H7B H 0.1987 0.3482 0.7303 0.053 Uiso 1 1 calc R . . H7C H 0.2765 0.4163 0.6505 0.053 Uiso 1 1 calc R . . C8 C 0.2465(2) 0.11786(15) 0.60350(15) 0.0449(4) Uani 1 1 d . . . H8A H 0.1921 0.1477 0.5369 0.067 Uiso 1 1 calc R . . H8B H 0.1672 0.0835 0.6365 0.067 Uiso 1 1 calc R . . H8C H 0.2972 0.0515 0.5834 0.067 Uiso 1 1 calc R . . C9 C 0.4640(2) 0.20204(17) 0.84287(14) 0.0441(4) Uani 1 1 d . . . H9A H 0.5022 0.1248 0.8346 0.066 Uiso 1 1 calc R . . H9B H 0.3697 0.1848 0.8664 0.066 Uiso 1 1 calc R . . H9C H 0.5503 0.2691 0.8988 0.066 Uiso 1 1 calc R . . Si4 Si 0.71721(4) 0.22753(3) 0.67108(3) 0.02244(8) Uani 1 1 d . . . C10 C 0.89716(18) 0.29419(16) 0.79929(13) 0.0373(3) Uani 1 1 d . . . H10A H 0.9454 0.3821 0.7988 0.056 Uiso 1 1 calc R . . H10B H 0.9766 0.2437 0.8021 0.056 Uiso 1 1 calc R . . H10C H 0.8642 0.2918 0.8645 0.056 Uiso 1 1 calc R . . C11 C 0.6553(2) 0.05286(13) 0.66786(14) 0.0375(4) Uani 1 1 d . . . H11A H 0.6326 0.0402 0.7355 0.056 Uiso 1 1 calc R . . H11B H 0.7429 0.0139 0.6634 0.056 Uiso 1 1 calc R . . H11C H 0.5580 0.0135 0.6030 0.056 Uiso 1 1 calc R . . C12 C 0.78103(18) 0.23519(14) 0.54622(12) 0.0325(3) Uani 1 1 d . . . H12A H 0.7018 0.1728 0.4824 0.049 Uiso 1 1 calc R . . H12B H 0.8872 0.2165 0.5616 0.049 Uiso 1 1 calc R . . H12C H 0.7873 0.3203 0.5296 0.049 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 K1 0.03830(17) 0.01768(14) 0.02463(15) 0.00484(11) 0.00151(12) 0.00547(12) Zn1 0.01967(8) 0.01580(8) 0.01949(8) 0.00435(5) 0.00613(6) 0.00385(6) O1 0.025(8) 0.013(4) 0.014(4) 0.005(3) 0.005(4) 0.001(4) O2 0.0212(9) 0.0245(6) 0.0240(7) 0.0064(5) 0.0097(5) 0.0069(6) N1 0.0190(5) 0.0192(5) 0.0193(5) 0.0027(4) 0.0056(4) 0.0020(4) Si1 0.02616(19) 0.02265(18) 0.02263(19) 0.00067(14) 0.01024(15) 0.00147(15) C1 0.0362(8) 0.0361(8) 0.0492(10) 0.0091(7) 0.0231(7) 0.0132(7) C2 0.0424(9) 0.0410(9) 0.0269(8) 0.0081(6) 0.0142(7) 0.0035(7) C3 0.0483(10) 0.0345(8) 0.0373(9) -0.0088(7) 0.0193(8) -0.0051(7) Si2 0.01900(17) 0.02581(18) 0.02230(18) 0.00562(14) 0.00610(14) 0.00231(14) C4 0.0248(7) 0.0529(10) 0.0334(8) 0.0123(7) 0.0038(6) 0.0062(7) C5 0.0350(8) 0.0337(8) 0.0487(10) 0.0120(7) 0.0166(7) -0.0014(7) C6 0.0273(7) 0.0442(9) 0.0342(8) 0.0048(7) 0.0146(6) 0.0083(7) N2 0.0233(5) 0.0165(5) 0.0226(5) 0.0064(4) 0.0084(4) 0.0048(4) Si3 0.02701(19) 0.02144(18) 0.0288(2) 0.00753(15) 0.01380(15) 0.00415(15) C7 0.0309(8) 0.0325(8) 0.0481(9) 0.0095(7) 0.0207(7) 0.0098(6) C8 0.0389(9) 0.0348(8) 0.0559(11) -0.0012(8) 0.0222(8) -0.0057(7) C9 0.0603(11) 0.0474(10) 0.0416(9) 0.0242(8) 0.0310(9) 0.0199(9) Si4 0.02346(18) 0.02023(17) 0.02480(19) 0.00752(14) 0.00749(14) 0.00755(14) C10 0.0293(8) 0.0473(9) 0.0328(8) 0.0120(7) 0.0055(6) 0.0102(7) C11 0.0426(9) 0.0240(7) 0.0515(10) 0.0139(7) 0.0179(8) 0.0140(7) C12 0.0340(8) 0.0337(8) 0.0342(8) 0.0059(6) 0.0164(6) 0.0110(6) _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 O1 2.6136(3) . ? K1 O2 2.6746(14) . ? K1 O2 2.7848(15) 2_666 ? K1 N1 2.7970(11) . ? K1 N2 2.8382(11) 2_666 ? Zn1 O1 1.93172(16) . ? Zn1 N1 1.9614(10) . ? Zn1 N2 1.9652(10) . ? Zn1 O2 2.0809(15) 2_666 ? Zn1 O2 2.0928(14) . ? O1 Zn1 1.93172(16) 2_666 ? O1 K1 2.6136(3) 2_666 ? O2 O2 1.579(4) 2_666 ? O2 Zn1 2.0809(15) 2_666 ? O2 K1 2.7848(14) 2_666 ? N1 Si2 1.7200(11) . ? N1 Si1 1.7204(11) . ? Si1 C2 1.8701(15) . ? Si1 C3 1.8791(15) . ? Si1 C1 1.8822(16) . ? Si2 C6 1.8655(15) . ? Si2 C4 1.8724(15) . ? Si2 C5 1.8830(15) . ? N2 Si4 1.7098(11) . ? N2 Si3 1.7182(11) . ? N2 K1 2.8382(11) 2_666 ? Si3 C7 1.8631(15) . ? Si3 C9 1.8728(16) . ? Si3 C8 1.8881(16) . ? Si4 C10 1.8623(15) . ? Si4 C12 1.8832(15) . ? Si4 C11 1.8814(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 O1 K1 O2 17.12(4) . . ? O1 K1 O2 16.43(4) . 2_666 ? O2 K1 O2 33.55(8) . 2_666 ? O1 K1 N1 73.83(2) . . ? O2 K1 N1 76.54(4) . . ? O2 K1 N1 72.59(3) 2_666 . ? O1 K1 N2 72.22(2) . 2_666 ? O2 K1 N2 74.81(4) . 2_666 ? O2 K1 N2 71.24(3) 2_666 2_666 ? N1 K1 N2 143.75(3) . 2_666 ? O1 Zn1 N1 113.35(3) . . ? O1 Zn1 N2 111.32(3) . . ? N1 Zn1 N2 135.32(4) . . ? O1 Zn1 O2 22.30(5) . 2_666 ? N1 Zn1 O2 109.61(5) . 2_666 ? N2 Zn1 O2 111.80(5) . 2_666 ? O1 Zn1 O2 22.17(5) . . ? N1 Zn1 O2 113.45(5) . . ? N2 Zn1 O2 107.58(5) . . ? O2 Zn1 O2 44.47(10) 2_666 . ? Zn1 O1 Zn1 180.0 2_666 . ? Zn1 O1 K1 88.775(8) 2_666 2_666 ? Zn1 O1 K1 91.225(8) . 2_666 ? Zn1 O1 K1 91.225(8) 2_666 . ? Zn1 O1 K1 88.775(8) . . ? K1 O1 K1 180.0 2_666 . ? O2 O2 Zn1 68.17(10) 2_666 2_666 ? O2 O2 Zn1 67.37(9) 2_666 . ? Zn1 O2 Zn1 135.53(10) 2_666 . ? O2 O2 K1 77.05(10) 2_666 . ? Zn1 O2 K1 86.37(5) 2_666 . ? Zn1 O2 K1 83.91(5) . . ? O2 O2 K1 69.39(9) 2_666 2_666 ? Zn1 O2 K1 81.37(5) 2_666 2_666 ? Zn1 O2 K1 83.32(5) . 2_666 ? K1 O2 K1 146.45(8) . 2_666 ? Si2 N1 Si1 122.25(6) . . ? Si2 N1 Zn1 118.01(6) . . ? Si1 N1 Zn1 115.41(6) . . ? Si2 N1 K1 103.00(5) . . ? Si1 N1 K1 103.55(5) . . ? Zn1 N1 K1 83.07(4) . . ? N1 Si1 C2 111.78(6) . . ? N1 Si1 C3 114.35(6) . . ? C2 Si1 C3 106.66(8) . . ? N1 Si1 C1 109.51(6) . . ? C2 Si1 C1 110.09(7) . . ? C3 Si1 C1 104.13(8) . . ? N1 Si2 C6 110.50(6) . . ? N1 Si2 C4 113.62(6) . . ? C6 Si2 C4 108.18(7) . . ? N1 Si2 C5 112.56(6) . . ? C6 Si2 C5 105.14(8) . . ? C4 Si2 C5 106.36(8) . . ? Si4 N2 Si3 124.54(6) . . ? Si4 N2 Zn1 115.08(6) . . ? Si3 N2 Zn1 117.47(6) . . ? Si4 N2 K1 101.05(5) . 2_666 ? Si3 N2 K1 100.61(5) . 2_666 ? Zn1 N2 K1 84.14(4) . 2_666 ? N2 Si3 C7 110.98(6) . . ? N2 Si3 C9 114.15(7) . . ? C7 Si3 C9 108.17(8) . . ? N2 Si3 C8 111.84(7) . . ? C7 Si3 C8 104.64(8) . . ? C9 Si3 C8 106.51(8) . . ? N2 Si4 C10 113.01(6) . . ? N2 Si4 C12 110.10(6) . . ? C10 Si4 C12 109.19(7) . . ? N2 Si4 C11 113.87(6) . . ? C10 Si4 C11 106.16(7) . . ? C12 Si4 C11 104.03(7) . . ? _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.327 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.043