# ic0004030.cif data_as4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H27 N5 S2 Si' _chemical_formula_weight 297.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 21.216(2) _cell_length_b 11.0890(10) _cell_length_c 7.2870(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1714.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 33 _cell_measurement_theta_min 8.656 _cell_measurement_theta_max 14.992 _exptl_crystal_description blocks _exptl_crystal_colour orange _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 0.372 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7810 _exptl_absorpt_correction_T_max 0.8360 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 197 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'random variation +/-2.0' _diffrn_reflns_number 2803 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2069 _reflns_number_gt 1551 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material SHELXL-97 _refine_special_details ; The anion is disordered. S(1) and N(2) are not lying on the crystallographic mirrorplane. Therefore we get two positions for these two atoms. 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^)+(0.0526P)^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 refU _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0084(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2069 _refine_ls_number_parameters 101 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0957 _refine_ls_wR_factor_gt 0.0920 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.25779(10) 0.2500 0.2324(3) 0.0403(5) Uani 1 2 d S . . S1 S 0.32538(3) 0.2356(5) 0.19606(9) 0.0331(8) Uani 0.50 1 d P . . N2 N 0.35442(11) 0.2699(7) 0.0059(3) 0.0337(18) Uani 0.50 1 d P . . Si1 Si 0.43215(3) 0.2500 -0.05224(9) 0.03613(19) Uani 1 2 d S . . C1 C 0.48523(14) 0.2500 0.1505(5) 0.0714(11) Uani 1 2 d S . . H1A H 0.4850 0.1700 0.2075 0.0591(18) Uiso 0.50 1 calc PR . . H1B H 0.4706 0.3101 0.2394 0.0591(18) Uiso 0.50 1 calc PR . . H1C H 0.5282 0.2700 0.1115 0.0591(18) Uiso 0.50 1 calc PR . . C2 C 0.45090(10) 0.1167(2) -0.1975(4) 0.0717(7) Uani 1 1 d . . . H2A H 0.4446 0.0427 -0.1262 0.0591(18) Uiso 1 1 calc R . . H2B H 0.4949 0.1212 -0.2380 0.0591(18) Uiso 1 1 calc R . . H2C H 0.4231 0.1158 -0.3049 0.0591(18) Uiso 1 1 calc R . . S2 S 0.20464(2) 0.2500 -0.19210(7) 0.02687(16) Uani 1 2 d S . . N3 N 0.20300(6) 0.12590(13) -0.30971(17) 0.0312(3) Uani 1 1 d . . . C3 C 0.15586(8) 0.10050(16) -0.4514(2) 0.0372(4) Uani 1 1 d . . . H3A H 0.1704 0.1326 -0.5694 0.0591(18) Uiso 1 1 calc R . . H3B H 0.1158 0.1388 -0.4181 0.0591(18) Uiso 1 1 calc R . . H3C H 0.1498 0.0132 -0.4617 0.0591(18) Uiso 1 1 calc R . . C4 C 0.26542(8) 0.07342(16) -0.3440(2) 0.0389(4) Uani 1 1 d . . . H4A H 0.2623 -0.0148 -0.3426 0.0591(18) Uiso 1 1 calc R . . H4B H 0.2948 0.0999 -0.2482 0.0591(18) Uiso 1 1 calc R . . H4C H 0.2808 0.1001 -0.4641 0.0591(18) Uiso 1 1 calc R . . N4 N 0.12900(8) 0.2500 -0.1181(2) 0.0288(4) Uani 1 2 d S . . C5 C 0.11454(7) 0.14054(18) -0.0100(2) 0.0412(4) Uani 1 1 d . . . H5A H 0.1408 0.1391 0.1006 0.0591(18) Uiso 1 1 calc R . . H5B H 0.1233 0.0688 -0.0843 0.0591(18) Uiso 1 1 calc R . . H5C H 0.0700 0.1412 0.0252 0.0591(18) 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 N1 0.0398(11) 0.0488(13) 0.0321(10) 0.000 0.0098(9) 0.000 S1 0.0366(3) 0.035(3) 0.0281(3) 0.0057(6) 0.0029(2) 0.0045(6) N2 0.0250(10) 0.048(6) 0.0281(10) 0.0024(14) -0.0005(8) 0.0011(14) Si1 0.0243(3) 0.0461(4) 0.0380(4) 0.000 0.0015(3) 0.000 C1 0.0362(14) 0.119(3) 0.0592(18) 0.000 -0.0105(14) 0.000 C2 0.0576(13) 0.0689(16) 0.0886(17) -0.0229(15) 0.0318(13) -0.0138(12) S2 0.0233(3) 0.0388(3) 0.0186(2) 0.000 -0.0014(2) 0.000 N3 0.0285(6) 0.0370(7) 0.0281(6) -0.0008(6) -0.0012(5) 0.0051(6) C3 0.0402(8) 0.0373(9) 0.0340(8) -0.0073(7) -0.0071(7) 0.0000(8) C4 0.0358(9) 0.0414(9) 0.0394(9) 0.0048(8) 0.0069(7) 0.0108(8) N4 0.0232(8) 0.0415(11) 0.0216(8) 0.000 0.0025(7) 0.000 C5 0.0335(8) 0.0573(12) 0.0329(8) 0.0113(8) 0.0058(7) -0.0035(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 S1 1.467(2) . ? N1 S1 1.467(2) 7_565 ? S1 S1 0.320(11) 7_565 ? S1 N2 1.518(2) 7_565 ? S1 N2 1.564(3) . ? N2 N2 0.440(16) 7_565 ? N2 S1 1.518(2) 7_565 ? N2 Si1 1.717(3) . ? Si1 N2 1.717(3) 7_565 ? Si1 C1 1.857(3) . ? Si1 C2 1.862(2) 7_565 ? Si1 C2 1.862(2) . ? S2 N3 1.6215(14) 7_565 ? S2 N3 1.6215(14) . ? S2 N4 1.6929(17) . ? N3 C3 1.4650(19) . ? N3 C4 1.4679(19) . ? N4 C5 1.479(2) 7_565 ? N4 C5 1.479(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 S1 N1 S1 12.5(4) . 7_565 ? S1 S1 N1 83.7(2) 7_565 . ? S1 S1 N2 92.3(4) 7_565 7_565 ? N1 S1 N2 124.48(13) . 7_565 ? S1 S1 N2 75.9(3) 7_565 . ? N1 S1 N2 121.3(2) . . ? N2 S1 N2 16.3(6) 7_565 . ? N2 N2 S1 87.7(4) 7_565 7_565 ? N2 N2 S1 75.9(3) 7_565 . ? S1 N2 S1 11.8(4) 7_565 . ? N2 N2 Si1 82.6(3) 7_565 . ? S1 N2 Si1 127.60(18) 7_565 . ? S1 N2 Si1 124.5(2) . . ? N2 Si1 N2 14.7(5) . 7_565 ? N2 Si1 C1 112.72(13) . . ? N2 Si1 C1 112.72(13) 7_565 . ? N2 Si1 C2 104.1(2) . 7_565 ? N2 Si1 C2 116.6(2) 7_565 7_565 ? C1 Si1 C2 108.83(10) . 7_565 ? N2 Si1 C2 116.6(2) . . ? N2 Si1 C2 104.1(2) 7_565 . ? C1 Si1 C2 108.83(10) . . ? C2 Si1 C2 105.18(17) 7_565 . ? N3 S2 N3 116.13(10) 7_565 . ? N3 S2 N4 98.51(6) 7_565 . ? N3 S2 N4 98.51(6) . . ? C3 N3 C4 114.81(13) . . ? C3 N3 S2 123.39(11) . . ? C4 N3 S2 114.03(11) . . ? C5 N4 C5 110.29(18) 7_565 . ? C5 N4 S2 111.47(10) 7_565 . ? C5 N4 S2 111.47(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 S1 N1 S1 N2 -88.5(6) 7_565 . . 7_565 ? S1 N1 S1 N2 -69.3(5) 7_565 . . . ? S1 S1 N2 N2 180.000(2) 7_565 . . 7_565 ? N1 S1 N2 N2 -106.5(4) . . . 7_565 ? N1 S1 N2 S1 73.5(4) . . . 7_565 ? N2 S1 N2 S1 180.000(1) 7_565 . . 7_565 ? S1 S1 N2 Si1 109.4(5) 7_565 . . . ? N1 S1 N2 Si1 -177.1(4) . . . . ? N2 S1 N2 Si1 -70.6(5) 7_565 . . . ? S1 N2 Si1 N2 81.4(7) 7_565 . . 7_565 ? S1 N2 Si1 N2 67.3(6) . . . 7_565 ? N2 N2 Si1 C1 -93.10(12) 7_565 . . . ? S1 N2 Si1 C1 -11.7(8) 7_565 . . . ? S1 N2 Si1 C1 -25.8(7) . . . . ? N2 N2 Si1 C2 149.13(11) 7_565 . . 7_565 ? S1 N2 Si1 C2 -129.5(6) 7_565 . . 7_565 ? S1 N2 Si1 C2 -143.6(5) . . . 7_565 ? N2 N2 Si1 C2 33.81(13) 7_565 . . . ? S1 N2 Si1 C2 115.2(6) 7_565 . . . ? S1 N2 Si1 C2 101.1(5) . . . . ? N3 S2 N3 C3 -51.52(17) 7_565 . . . ? N4 S2 N3 C3 52.37(14) . . . . ? N3 S2 N3 C4 96.05(13) 7_565 . . . ? N4 S2 N3 C4 -160.05(11) . . . . ? N3 S2 N4 C5 -59.03(13) 7_565 . . 7_565 ? N3 S2 N4 C5 -177.24(12) . . . 7_565 ? N3 S2 N4 C5 177.24(12) 7_565 . . . ? N3 S2 N4 C5 59.03(13) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.211 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.050 #===END