data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H52 K N2 Ni Si2' _chemical_formula_weight 594.73 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' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 13.3749(9) _cell_length_b 13.3774(9) _cell_length_c 18.2349(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3262.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9871 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 25.38 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1284 _exptl_absorpt_coefficient_mu 0.816 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9084 _exptl_absorpt_correction_T_max 0.9156 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'QUAZAR multilayer mirros' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 40859 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.38 _reflns_number_total 2999 _reflns_number_gt 2482 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP32 _computing_publication_material WinGX _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^)+(0.0230P)^2^+3.3081P] 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 2999 _refine_ls_number_parameters 171 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0676 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 C1 C 0.36816(13) 0.11653(13) 0.11068(10) 0.0101(4) Uani 1 1 d . . . C2 C 0.31810(13) 0.03794(14) 0.07267(10) 0.0129(4) Uani 1 1 d . . . C3 C 0.33951(14) 0.02109(14) -0.00108(11) 0.0171(4) Uani 1 1 d . . . H3 H 0.3040 -0.0297 -0.0266 0.021 Uiso 1 1 calc R . . C4 C 0.41104(14) 0.07625(15) -0.03820(11) 0.0184(4) Uani 1 1 d . . . H4 H 0.4232 0.0649 -0.0888 0.022 Uiso 1 1 calc R . . C5 C 0.46434(14) 0.14796(14) -0.00030(10) 0.0161(4) Uani 1 1 d . . . H5 H 0.5154 0.1840 -0.0250 0.019 Uiso 1 1 calc R . . C6 C 0.44516(13) 0.16891(14) 0.07335(10) 0.0130(4) Uani 1 1 d . . . C7 C 0.50430(14) 0.25117(15) 0.11093(11) 0.0180(4) Uani 1 1 d . . . H7 H 0.4869 0.2498 0.1643 0.022 Uiso 1 1 calc R . . C8 C 0.61771(14) 0.23612(16) 0.10423(13) 0.0256(5) Uani 1 1 d . . . H8A H 0.6360 0.1710 0.1248 0.038 Uiso 1 1 calc R . . H8B H 0.6524 0.2892 0.1312 0.038 Uiso 1 1 calc R . . H8C H 0.6371 0.2386 0.0524 0.038 Uiso 1 1 calc R . . C9 C 0.47288(16) 0.35316(15) 0.08061(13) 0.0256(5) Uani 1 1 d . . . H9A H 0.4853 0.3551 0.0277 0.038 Uiso 1 1 calc R . . H9B H 0.5117 0.4059 0.1048 0.038 Uiso 1 1 calc R . . H9C H 0.4015 0.3638 0.0900 0.038 Uiso 1 1 calc R . . C10 C 0.24549(14) -0.02981(14) 0.11331(11) 0.0173(4) Uani 1 1 d . . . H10 H 0.2117 0.0106 0.1522 0.021 Uiso 1 1 calc R . . C11 C 0.30436(17) -0.11420(16) 0.15091(13) 0.0294(5) Uani 1 1 d . . . H11A H 0.3332 -0.1583 0.1135 0.044 Uiso 1 1 calc R . . H11B H 0.2593 -0.1528 0.1824 0.044 Uiso 1 1 calc R . . H11C H 0.3581 -0.0853 0.1807 0.044 Uiso 1 1 calc R . . C12 C 0.16461(16) -0.07631(17) 0.06461(13) 0.0287(5) Uani 1 1 d . . . H12A H 0.1311 -0.0236 0.0365 0.043 Uiso 1 1 calc R . . H12B H 0.1155 -0.1109 0.0954 0.043 Uiso 1 1 calc R . . H12C H 0.1954 -0.1242 0.0308 0.043 Uiso 1 1 calc R . . C13 C 0.30271(18) 0.0290(2) 0.31929(13) 0.0413(7) Uani 1 1 d . . . H13A H 0.2384 0.0634 0.3244 0.062 Uiso 1 1 calc R . . H13B H 0.3315 0.0174 0.3680 0.062 Uiso 1 1 calc R . . H13C H 0.2925 -0.0352 0.2945 0.062 Uiso 1 1 calc R . . C14 C 0.4167(2) 0.2191(2) 0.32320(13) 0.0453(7) Uani 1 1 d . . . H14A H 0.4692 0.2600 0.3007 0.068 Uiso 1 1 calc R . . H14B H 0.4389 0.1962 0.3716 0.068 Uiso 1 1 calc R . . H14C H 0.3557 0.2590 0.3285 0.068 Uiso 1 1 calc R . . C15 C 0.51141(15) 0.04008(16) 0.24897(11) 0.0224(5) Uani 1 1 d . . . H15A H 0.4996 -0.0185 0.2178 0.034 Uiso 1 1 calc R . . H15B H 0.5381 0.0184 0.2964 0.034 Uiso 1 1 calc R . . H15C H 0.5596 0.0846 0.2250 0.034 Uiso 1 1 calc R . . N1 N 0.33901(11) 0.14480(11) 0.18225(8) 0.0114(3) Uani 1 1 d . . . Si1 Si 0.39055(4) 0.10847(4) 0.26354(3) 0.01856(14) Uani 1 1 d . . . K1 K 0.2500 0.2500 -0.00483(3) 0.01890(15) Uani 1 2 d S . . Ni1 Ni 0.2500 0.2500 0.183971(17) 0.01027(10) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0103(9) 0.0098(9) 0.0104(9) 0.0014(7) -0.0022(7) 0.0046(7) C2 0.0107(9) 0.0122(9) 0.0157(10) -0.0005(8) -0.0021(7) 0.0047(7) C3 0.0192(10) 0.0146(10) 0.0176(10) -0.0054(8) -0.0064(8) 0.0083(8) C4 0.0223(10) 0.0220(11) 0.0109(9) -0.0007(8) -0.0004(8) 0.0114(9) C5 0.0147(10) 0.0188(10) 0.0149(10) 0.0060(8) 0.0051(8) 0.0075(8) C6 0.0106(9) 0.0132(9) 0.0151(10) 0.0021(8) 0.0001(7) 0.0033(7) C7 0.0135(9) 0.0182(10) 0.0222(10) 0.0001(9) 0.0023(8) -0.0026(8) C8 0.0149(10) 0.0246(12) 0.0372(13) 0.0001(10) 0.0012(9) -0.0038(9) C9 0.0206(11) 0.0171(11) 0.0391(13) -0.0014(10) 0.0046(10) -0.0010(9) C10 0.0156(9) 0.0130(9) 0.0233(11) -0.0049(8) 0.0015(9) -0.0027(8) C11 0.0303(12) 0.0183(11) 0.0398(14) 0.0085(10) 0.0026(10) -0.0039(10) C12 0.0219(11) 0.0259(12) 0.0381(14) -0.0131(10) 0.0000(10) -0.0072(9) C13 0.0355(14) 0.0609(18) 0.0274(13) 0.0223(12) 0.0148(11) 0.0254(13) C14 0.0645(18) 0.0454(16) 0.0260(13) -0.0182(11) -0.0246(13) 0.0293(14) C15 0.0222(11) 0.0253(11) 0.0198(11) 0.0029(9) -0.0020(8) 0.0080(9) N1 0.0122(8) 0.0113(8) 0.0107(8) -0.0003(6) 0.0005(6) 0.0018(6) Si1 0.0222(3) 0.0238(3) 0.0097(3) -0.0004(2) -0.0011(2) 0.0120(2) K1 0.0184(3) 0.0213(3) 0.0170(3) 0.000 0.000 0.0085(3) Ni1 0.00997(16) 0.01134(17) 0.00951(17) 0.000 0.000 0.00282(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.414(2) . ? C1 C6 1.420(3) . ? C1 C2 1.426(3) . ? C1 K1 3.1815(17) . ? C2 C3 1.393(3) . ? C2 C10 1.521(3) . ? C2 K1 3.2976(18) . ? C3 C4 1.385(3) . ? C3 K1 3.2886(18) . ? C3 H3 0.9500 . ? C4 C5 1.381(3) . ? C4 K1 3.2268(19) . ? C4 H4 0.9500 . ? C5 C6 1.396(3) . ? C5 K1 3.1762(18) . ? C5 H5 0.9500 . ? C6 C7 1.519(3) . ? C6 K1 3.1659(18) . ? C7 C9 1.531(3) . ? C7 C8 1.535(3) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.532(3) . ? C10 C11 1.538(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 Si1 1.883(2) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 Si1 1.869(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 Si1 1.876(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? N1 Si1 1.7054(16) . ? N1 Ni1 1.8436(15) . ? K1 C6 3.1659(18) 2 ? K1 C5 3.1762(18) 2 ? K1 C1 3.1815(17) 2 ? K1 C4 3.2268(19) 2 ? K1 C3 3.2886(18) 2 ? K1 C2 3.2976(18) 2 ? Ni1 N1 1.8436(15) 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 N1 C1 C6 120.71(16) . . ? N1 C1 C2 121.09(16) . . ? C6 C1 C2 118.13(16) . . ? N1 C1 K1 108.91(10) . . ? C6 C1 K1 76.46(10) . . ? C2 C1 K1 81.88(10) . . ? C3 C2 C1 119.46(17) . . ? C3 C2 C10 120.33(17) . . ? C1 C2 C10 120.14(16) . . ? C3 C2 K1 77.43(11) . . ? C1 C2 K1 72.77(10) . . ? C10 C2 K1 123.03(11) . . ? C4 C3 C2 121.84(18) . . ? C4 C3 K1 75.24(11) . . ? C2 C3 K1 78.15(11) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? K1 C3 H3 118.3 . . ? C5 C4 C3 118.83(18) . . ? C5 C4 K1 75.50(11) . . ? C3 C4 K1 80.24(11) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? K1 C4 H4 114.4 . . ? C4 C5 C6 121.76(18) . . ? C4 C5 K1 79.61(11) . . ? C6 C5 K1 76.87(10) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? K1 C5 H5 114.7 . . ? C5 C6 C1 119.71(17) . . ? C5 C6 C7 118.95(17) . . ? C1 C6 C7 121.28(17) . . ? C5 C6 K1 77.70(11) . . ? C1 C6 K1 77.69(10) . . ? C7 C6 K1 112.60(11) . . ? C6 C7 C9 109.88(16) . . ? C6 C7 C8 112.56(17) . . ? C9 C7 C8 111.06(17) . . ? C6 C7 H7 107.7 . . ? C9 C7 H7 107.7 . . ? C8 C7 H7 107.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 C12 114.23(17) . . ? C2 C10 C11 109.13(16) . . ? C12 C10 C11 108.79(17) . . ? C2 C10 H10 108.2 . . ? C12 C10 H10 108.2 . . ? C11 C10 H10 108.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C1 N1 Si1 127.93(12) . . ? C1 N1 Ni1 113.46(11) . . ? Si1 N1 Ni1 117.63(8) . . ? N1 Si1 C14 110.85(10) . . ? N1 Si1 C15 111.36(8) . . ? C14 Si1 C15 107.88(11) . . ? N1 Si1 C13 112.21(10) . . ? C14 Si1 C13 104.45(13) . . ? C15 Si1 C13 109.79(10) . . ? C6 K1 C6 126.48(7) . 2 ? C6 K1 C5 25.42(5) . . ? C6 K1 C5 151.61(5) 2 . ? C6 K1 C5 151.61(5) . 2 ? C6 K1 C5 25.42(5) 2 2 ? C5 K1 C5 177.02(7) . 2 ? C6 K1 C1 107.68(5) . 2 ? C6 K1 C1 25.85(5) 2 2 ? C5 K1 C1 132.25(5) . 2 ? C5 K1 C1 45.03(5) 2 2 ? C6 K1 C1 25.85(5) . . ? C6 K1 C1 107.68(5) 2 . ? C5 K1 C1 45.03(5) . . ? C5 K1 C1 132.25(5) 2 . ? C1 K1 C1 97.09(6) 2 . ? C6 K1 C4 44.58(5) . . ? C6 K1 C4 151.90(5) 2 . ? C5 K1 C4 24.89(5) . . ? C5 K1 C4 156.48(5) 2 . ? C1 K1 C4 149.39(5) 2 . ? C1 K1 C4 52.34(5) . . ? C6 K1 C4 151.90(5) . 2 ? C6 K1 C4 44.58(5) 2 2 ? C5 K1 C4 156.48(5) . 2 ? C5 K1 C4 24.89(5) 2 2 ? C1 K1 C4 52.34(5) 2 2 ? C1 K1 C4 149.39(5) . 2 ? C4 K1 C4 158.26(7) . 2 ? C6 K1 C3 51.05(5) . . ? C6 K1 C3 127.58(5) 2 . ? C5 K1 C3 43.17(5) . . ? C5 K1 C3 136.73(5) 2 . ? C1 K1 C3 133.60(5) 2 . ? C1 K1 C3 44.18(5) . . ? C4 K1 C3 24.52(5) . . ? C4 K1 C3 156.58(5) 2 . ? C6 K1 C3 127.58(5) . 2 ? C6 K1 C3 51.05(5) 2 2 ? C5 K1 C3 136.73(5) . 2 ? C5 K1 C3 43.17(5) 2 2 ? C1 K1 C3 44.18(5) 2 2 ? C1 K1 C3 133.60(5) . 2 ? C4 K1 C3 156.58(5) . 2 ? C4 K1 C3 24.52(5) 2 2 ? C3 K1 C3 177.62(7) . 2 ? C6 K1 C2 109.24(5) . 2 ? C6 K1 C2 44.32(5) 2 2 ? C5 K1 C2 127.44(5) . 2 ? C5 K1 C2 50.94(5) 2 2 ? C1 K1 C2 25.35(5) 2 2 ? C1 K1 C2 109.65(5) . 2 ? C4 K1 C2 152.23(5) . 2 ? C4 K1 C2 43.68(5) 2 2 ? C3 K1 C2 153.21(5) . 2 ? C3 K1 C2 24.42(5) 2 2 ? C6 K1 C2 44.32(5) . . ? C6 K1 C2 109.24(5) 2 . ? C5 K1 C2 50.94(5) . . ? C5 K1 C2 127.44(5) 2 . ? C1 K1 C2 109.65(5) 2 . ? C1 K1 C2 25.35(5) . . ? C4 K1 C2 43.68(5) . . ? C4 K1 C2 152.23(5) 2 . ? C3 K1 C2 24.42(5) . . ? C3 K1 C2 153.21(5) 2 . ? C2 K1 C2 129.25(7) 2 . ? N1 Ni1 N1 178.05(9) 2 . ? N1 Ni1 K1 89.02(5) 2 . ? N1 Ni1 K1 89.02(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.336 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.055