Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _audit_creation_method SHELXL-97 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Hans Joachim Breunig' 'Mihaiela Emilia Ghesner' 'Enno Lork' _publ_contact_author_name 'Prof Hans Joachim Breunig' _publ_contact_author_address ; Fachbereich 2 Universitat Bremen Leobenerstr. Bremen D-28334 GERMANY ; _publ_contact_author_email BREUNIG@CHEMIE.UNI-BREMEN.DE _publ_contact_author_phone +49-421-2182266 _publ_contact_author_fax +49-421-2184042 _publ_requested_journal 'Chemical Communications' _publ_section_title ; Synthesis of a stibindolyl anion from trimesitylantimony and potassium. ; data_COMPOUND_1 _database_code_CSD 198210 _chemical_formula_sum 'C27 H41 K N3 Sb' _chemical_formula_weight 568.48 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' K K 0.2009 0.2494 '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' Sb Sb -0.5866 1.5461 '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 23.681(5) _cell_length_b 9.641(2) _cell_length_c 13.243(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.79(3) _cell_angle_gamma 90.00 _cell_volume 2909.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 800 _cell_measurement_theta_min 2.03 _cell_measurement_theta_max 26.13 _exptl_crystal_description blocks _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 1.109 _exptl_absorpt_correction_type refdelF _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Stuart & Walker, Acta Cryst A (1983)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Stoe IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'random variation +/-2.0' _diffrn_reflns_number 35681 _diffrn_reflns_av_R_equivalents 0.1266 _diffrn_reflns_av_sigmaI/netI 0.0684 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5123 _reflns_number_gt 3324 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE Expose' _computing_cell_refinement 'STOE Cell' _computing_data_reduction 'STOE Integrate' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL / DIAMOND' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0450P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5123 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.0965 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.262002(15) 0.69720(4) 0.30825(2) 0.05220(12) Uani 1 1 d . . . C1 C 0.2877(2) 0.8329(5) 0.4407(3) 0.0487(11) Uani 1 1 d . . . C2 C 0.23977(19) 0.8945(5) 0.4610(3) 0.0457(10) Uani 1 1 d . . . H2 H 0.2447 0.9552 0.5193 0.057(6) Uiso 1 1 calc R . . C3 C 0.18189(19) 0.8669(5) 0.3938(3) 0.0424(10) Uani 1 1 d . . . C4 C 0.17815(19) 0.7734(4) 0.3108(3) 0.0428(10) Uani 1 1 d . . . C5 C 0.1232(2) 0.7449(5) 0.2390(3) 0.0479(11) Uani 1 1 d . . . C6 C 0.0741(2) 0.8117(5) 0.2527(3) 0.0514(11) Uani 1 1 d . . . H6 H 0.0372 0.7939 0.2041 0.057(6) Uiso 1 1 calc R . . C7 C 0.0764(2) 0.9042(5) 0.3349(3) 0.0486(11) Uani 1 1 d . . . C8 C 0.1304(2) 0.9318(5) 0.4045(3) 0.0439(11) Uani 1 1 d . . . H8 H 0.1329 0.9955 0.4603 0.057(6) Uiso 1 1 calc R . . C9 C 0.0211(2) 0.9724(7) 0.3481(4) 0.0674(15) Uani 1 1 d . . . H9A H 0.0315 1.0391 0.4060 0.116(5) Uiso 1 1 calc R . . H9B H -0.0049 0.9013 0.3637 0.116(5) Uiso 1 1 calc R . . H9C H 0.0010 1.0206 0.2832 0.116(5) Uiso 1 1 calc R . . C10 C 0.1188(2) 0.6472(6) 0.1492(4) 0.0596(13) Uani 1 1 d . . . H10A H 0.0785 0.6471 0.1040 0.116(5) Uiso 1 1 d R . . H10B H 0.1295 0.5534 0.1762 0.116(5) Uiso 1 1 d R . . H10C H 0.1456 0.6773 0.1085 0.116(5) Uiso 1 1 d R . . C11 C 0.3479(2) 0.8535(5) 0.5036(4) 0.0543(12) Uani 1 1 d . . . C12 C 0.3607(2) 0.9094(6) 0.6053(4) 0.0569(13) Uani 1 1 d . . . H12 H 0.3292 0.9360 0.6328 0.057(6) Uiso 1 1 calc R . . C13 C 0.4182(2) 0.9273(6) 0.6672(4) 0.0682(15) Uani 1 1 d . . . C14 C 0.4633(3) 0.8871(7) 0.6258(5) 0.0803(18) Uani 1 1 d . . . H14 H 0.5026 0.8987 0.6671 0.057(6) Uiso 1 1 calc R . . C15 C 0.4533(2) 0.8312(7) 0.5273(5) 0.0786(18) Uani 1 1 d . . . C16 C 0.3959(2) 0.8155(6) 0.4666(5) 0.0676(14) Uani 1 1 d . . . H16 H 0.3889 0.7779 0.3980 0.036(11) Uiso 1 1 calc R . . C17 C 0.5043(3) 0.7856(8) 0.4849(7) 0.111(3) Uani 1 1 d . . . H17A H 0.5393 0.8401 0.5186 0.116(5) Uiso 1 1 calc R . . H17B H 0.4939 0.8006 0.4088 0.116(5) Uiso 1 1 calc R . . H17C H 0.5124 0.6869 0.5000 0.116(5) Uiso 1 1 calc R . . C18 C 0.4303(3) 0.9913(8) 0.7747(5) 0.0857(19) Uani 1 1 d . . . H18A H 0.4559 0.9297 0.8263 0.116(5) Uiso 1 1 calc R . . H18B H 0.3932 1.0046 0.7929 0.116(5) Uiso 1 1 calc R . . H18C H 0.4497 1.0811 0.7749 0.116(5) Uiso 1 1 calc R . . K1 K 0.23486(5) 0.59650(11) 0.55966(8) 0.0511(3) Uani 1 1 d . . . N1 N 0.1253(2) 0.4494(5) 0.4919(3) 0.0645(12) Uani 1 1 d . . . N2 N 0.2256(2) 0.3300(4) 0.6540(3) 0.0666(12) Uani 1 1 d . . . N3 N 0.3365(2) 0.4264(6) 0.6095(5) 0.0870(16) Uani 1 1 d . . . C19 C 0.1336(3) 0.3928(8) 0.3945(4) 0.0825(18) Uani 1 1 d . . . H19A H 0.1016 0.3282 0.3634 0.116(5) Uiso 1 1 calc R . . H19B H 0.1712 0.3436 0.4097 0.116(5) Uiso 1 1 calc R . . H19C H 0.1336 0.4686 0.3452 0.116(5) Uiso 1 1 calc R . . C20 C 0.0739(3) 0.5396(7) 0.4668(5) 0.0771(17) Uani 1 1 d . . . H20A H 0.0390 0.4852 0.4329 0.116(5) Uiso 1 1 calc R . . H20B H 0.0793 0.6132 0.4192 0.116(5) Uiso 1 1 calc R . . H20C H 0.0691 0.5811 0.5315 0.116(5) Uiso 1 1 calc R . . C21 C 0.1192(3) 0.3380(7) 0.5640(5) 0.0844(19) Uani 1 1 d . . . H21A H 0.0863 0.2769 0.5277 0.101(8) Uiso 1 1 calc R . . H21B H 0.1090 0.3797 0.6251 0.101(8) Uiso 1 1 calc R . . C22 C 0.1738(3) 0.2510(7) 0.6029(5) 0.0838(18) Uani 1 1 d . . . H22A H 0.1667 0.1811 0.6528 0.101(8) Uiso 1 1 calc R . . H22B H 0.1812 0.2006 0.5426 0.101(8) Uiso 1 1 calc R . . C23 C 0.2206(3) 0.3874(7) 0.7529(4) 0.091(2) Uani 1 1 d . . . H23A H 0.1842 0.4407 0.7406 0.116(5) Uiso 1 1 calc R . . H23B H 0.2542 0.4483 0.7825 0.116(5) Uiso 1 1 calc R . . H23C H 0.2202 0.3117 0.8021 0.116(5) Uiso 1 1 calc R . . C24 C 0.2788(3) 0.2462(7) 0.6689(6) 0.092(2) Uani 1 1 d . . . H24A H 0.2754 0.1900 0.6049 0.101(8) Uiso 1 1 calc R . . H24B H 0.2813 0.1813 0.7279 0.101(8) Uiso 1 1 calc R . . C25 C 0.3341(3) 0.3285(8) 0.6909(6) 0.102(2) Uani 1 1 d . . . H25A H 0.3388 0.3797 0.7575 0.101(8) Uiso 1 1 calc R . . H25B H 0.3676 0.2637 0.7011 0.101(8) Uiso 1 1 calc R . . C26 C 0.3875(3) 0.5130(10) 0.6453(8) 0.140(4) Uani 1 1 d . . . H26A H 0.3851 0.5638 0.7081 0.116(5) Uiso 1 1 calc R . . H26B H 0.3892 0.5790 0.5900 0.116(5) Uiso 1 1 calc R . . H26C H 0.4228 0.4551 0.6622 0.116(5) Uiso 1 1 calc R . . C27 C 0.3375(4) 0.3542(11) 0.5121(7) 0.134(4) Uani 1 1 d . . . H27A H 0.3411 0.4224 0.4593 0.116(5) Uiso 1 1 calc R . . H27B H 0.3011 0.3015 0.4857 0.116(5) Uiso 1 1 calc R . . H27C H 0.3711 0.2907 0.5263 0.116(5) 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 Sb1 0.05766(19) 0.05373(19) 0.04941(18) 0.00096(18) 0.02169(13) 0.00851(19) C1 0.060(3) 0.043(3) 0.046(2) 0.005(2) 0.019(2) 0.002(2) C2 0.049(3) 0.044(3) 0.044(2) 0.005(2) 0.012(2) -0.001(2) C3 0.047(3) 0.039(2) 0.041(2) 0.001(2) 0.011(2) 0.000(2) C4 0.051(2) 0.039(3) 0.040(2) 0.001(2) 0.0163(19) 0.003(2) C5 0.063(3) 0.042(2) 0.039(2) 0.000(2) 0.015(2) -0.004(2) C6 0.050(3) 0.057(3) 0.042(2) 0.001(3) 0.0045(19) 0.001(3) C7 0.048(3) 0.053(3) 0.044(2) 0.007(2) 0.011(2) 0.006(2) C8 0.049(3) 0.043(3) 0.041(2) -0.002(2) 0.015(2) 0.003(2) C9 0.054(3) 0.077(4) 0.066(3) -0.008(3) 0.009(3) 0.016(3) C10 0.064(3) 0.066(3) 0.049(3) -0.011(3) 0.016(2) -0.003(3) C11 0.052(3) 0.047(3) 0.067(3) 0.009(2) 0.021(2) 0.005(2) C12 0.052(3) 0.055(3) 0.063(3) 0.006(3) 0.014(2) 0.007(3) C13 0.054(3) 0.067(4) 0.076(4) 0.007(3) 0.003(3) 0.006(3) C14 0.048(3) 0.080(4) 0.100(5) -0.009(4) 0.000(3) 0.001(3) C15 0.050(3) 0.079(4) 0.110(5) -0.004(4) 0.025(3) -0.001(3) C16 0.058(3) 0.066(4) 0.082(4) -0.012(3) 0.024(3) -0.003(3) C17 0.056(3) 0.120(7) 0.163(7) -0.038(6) 0.038(4) -0.008(4) C18 0.065(4) 0.095(5) 0.081(4) 0.008(4) -0.010(3) 0.006(4) K1 0.0546(6) 0.0467(6) 0.0527(6) 0.0043(5) 0.0157(5) 0.0016(5) N1 0.071(3) 0.066(3) 0.061(3) -0.004(2) 0.026(2) -0.011(2) N2 0.102(4) 0.039(2) 0.059(2) -0.001(2) 0.022(2) -0.002(2) N3 0.064(3) 0.087(4) 0.107(4) 0.033(3) 0.016(3) 0.022(3) C19 0.088(4) 0.096(5) 0.065(3) -0.016(4) 0.024(3) -0.006(4) C20 0.068(4) 0.085(5) 0.081(4) -0.012(3) 0.023(3) -0.008(3) C21 0.101(5) 0.077(4) 0.084(4) -0.005(3) 0.039(4) -0.034(4) C22 0.123(6) 0.045(3) 0.083(4) 0.004(3) 0.029(4) -0.008(4) C23 0.151(7) 0.065(4) 0.066(4) -0.013(3) 0.045(4) -0.016(4) C24 0.130(6) 0.055(4) 0.088(4) 0.015(3) 0.023(4) 0.015(4) C25 0.100(5) 0.086(5) 0.105(5) 0.024(4) 0.001(4) 0.025(4) C26 0.073(5) 0.127(8) 0.207(10) 0.067(8) 0.016(6) 0.013(5) C27 0.113(6) 0.172(10) 0.128(7) 0.023(7) 0.054(5) 0.069(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 Sb1 C4 2.126(4) . ? Sb1 C1 2.139(5) . ? Sb1 K1 3.6886(13) . ? Sb1 K1 3.7490(13) 4_575 ? C1 C2 1.372(6) . ? C1 C11 1.454(7) . ? C1 K1 3.212(5) . ? C2 C3 1.442(6) . ? C2 K1 3.171(5) . ? C3 C4 1.405(6) . ? C3 C8 1.411(6) . ? C3 K1 3.419(5) . ? C4 C5 1.414(6) . ? C5 C6 1.384(6) . ? C5 C10 1.498(7) . ? C6 C7 1.396(7) . ? C7 C8 1.385(6) . ? C7 C9 1.517(7) . ? C11 C16 1.405(7) . ? C11 C12 1.405(7) . ? C12 C13 1.395(7) . ? C13 C14 1.383(8) . ? C13 C18 1.505(8) . ? C14 C15 1.371(8) . ? C15 C16 1.386(8) . ? C15 C17 1.529(8) . ? K1 N3 2.837(5) . ? K1 N1 2.878(5) . ? K1 N2 2.891(4) . ? K1 Sb1 3.7490(13) 4_576 ? N1 C20 1.457(7) . ? N1 C19 1.462(7) . ? N1 C21 1.470(7) . ? N2 C22 1.446(8) . ? N2 C23 1.456(7) . ? N2 C24 1.464(8) . ? N3 C26 1.438(9) . ? N3 C25 1.446(9) . ? N3 C27 1.472(10) . ? C21 C22 1.509(9) . ? C24 C25 1.490(10) . ? 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 C4 Sb1 C1 80.49(17) . . ? C4 Sb1 K1 71.55(11) . . ? C1 Sb1 K1 60.12(12) . . ? C4 Sb1 K1 83.86(11) . 4_575 ? C1 Sb1 K1 109.75(12) . 4_575 ? K1 Sb1 K1 154.41(3) . 4_575 ? C2 C1 C11 124.2(4) . . ? C2 C1 Sb1 111.1(3) . . ? C11 C1 Sb1 124.7(3) . . ? C2 C1 K1 75.9(3) . . ? C11 C1 K1 105.5(3) . . ? Sb1 C1 K1 84.62(15) . . ? C1 C2 C3 119.8(4) . . ? C1 C2 K1 79.3(3) . . ? C3 C2 K1 87.2(3) . . ? C4 C3 C8 119.4(4) . . ? C4 C3 C2 116.7(4) . . ? C8 C3 C2 123.9(4) . . ? C4 C3 K1 87.0(3) . . ? C8 C3 K1 116.7(3) . . ? C2 C3 K1 67.9(2) . . ? C3 C4 C5 120.1(4) . . ? C3 C4 Sb1 111.9(3) . . ? C5 C4 Sb1 127.9(3) . . ? C6 C5 C4 118.2(4) . . ? C6 C5 C10 121.2(4) . . ? C4 C5 C10 120.5(4) . . ? C5 C6 C7 123.0(4) . . ? C8 C7 C6 118.3(4) . . ? C8 C7 C9 120.7(4) . . ? C6 C7 C9 121.0(4) . . ? C7 C8 C3 121.0(4) . . ? C16 C11 C12 116.7(5) . . ? C16 C11 C1 121.6(5) . . ? C12 C11 C1 121.7(4) . . ? C13 C12 C11 122.2(5) . . ? C14 C13 C12 117.9(5) . . ? C14 C13 C18 121.4(5) . . ? C12 C13 C18 120.7(5) . . ? C15 C14 C13 122.4(5) . . ? C14 C15 C16 118.9(5) . . ? C14 C15 C17 120.9(6) . . ? C16 C15 C17 120.2(6) . . ? C15 C16 C11 121.9(5) . . ? N3 K1 N1 115.05(17) . . ? N3 K1 N2 62.94(16) . . ? N1 K1 N2 61.89(14) . . ? N3 K1 C2 119.71(15) . . ? N1 K1 C2 116.68(13) . . ? N2 K1 C2 177.04(13) . . ? N3 K1 C1 96.03(15) . . ? N1 K1 C1 129.45(13) . . ? N2 K1 C1 158.11(13) . . ? C2 K1 C1 24.82(11) . . ? N3 K1 C3 136.85(14) . . ? N1 K1 C3 91.90(12) . . ? N2 K1 C3 153.79(13) . . ? C2 K1 C3 24.91(11) . . ? C1 K1 C3 42.94(11) . . ? N3 K1 Sb1 90.97(12) . . ? N1 K1 Sb1 102.24(9) . . ? N2 K1 Sb1 132.54(9) . . ? C2 K1 Sb1 49.83(8) . . ? C1 K1 Sb1 35.27(8) . . ? C3 K1 Sb1 48.93(7) . . ? N3 K1 Sb1 99.82(13) . 4_576 ? N1 K1 Sb1 117.37(9) . 4_576 ? N2 K1 Sb1 96.16(9) . 4_576 ? C2 K1 Sb1 82.20(9) . 4_576 ? C1 K1 Sb1 93.31(9) . 4_576 ? C3 K1 Sb1 96.03(8) . 4_576 ? Sb1 K1 Sb1 128.51(3) . 4_576 ? C20 N1 C19 109.0(5) . . ? C20 N1 C21 111.2(5) . . ? C19 N1 C21 111.1(5) . . ? C20 N1 K1 113.7(3) . . ? C19 N1 K1 97.6(3) . . ? C21 N1 K1 113.4(4) . . ? C22 N2 C23 110.8(5) . . ? C22 N2 C24 111.2(5) . . ? C23 N2 C24 111.4(5) . . ? C22 N2 K1 114.8(3) . . ? C23 N2 K1 94.9(3) . . ? C24 N2 K1 112.6(4) . . ? C26 N3 C25 109.4(6) . . ? C26 N3 C27 110.5(7) . . ? C25 N3 C27 111.0(7) . . ? C26 N3 K1 108.9(5) . . ? C25 N3 K1 110.4(4) . . ? C27 N3 K1 106.6(4) . . ? N1 C21 C22 113.6(5) . . ? N2 C22 C21 114.0(5) . . ? N2 C24 C25 114.3(6) . . ? N3 C25 C24 114.3(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Sb1 C1 C2 1.5(3) . . . . ? K1 Sb1 C1 C2 -72.6(3) . . . . ? K1 Sb1 C1 C2 81.4(3) 4_575 . . . ? C4 Sb1 C1 C11 179.3(4) . . . . ? K1 Sb1 C1 C11 105.2(4) . . . . ? K1 Sb1 C1 C11 -100.8(4) 4_575 . . . ? C4 Sb1 C1 K1 74.11(14) . . . . ? K1 Sb1 C1 K1 154.01(5) 4_575 . . . ? C11 C1 C2 C3 -179.9(4) . . . . ? Sb1 C1 C2 C3 -2.0(5) . . . . ? K1 C1 C2 C3 -80.5(4) . . . . ? C11 C1 C2 K1 -99.4(4) . . . . ? Sb1 C1 C2 K1 78.4(2) . . . . ? C1 C2 C3 C4 1.5(6) . . . . ? K1 C2 C3 C4 -74.5(4) . . . . ? C1 C2 C3 C8 -175.9(4) . . . . ? K1 C2 C3 C8 108.2(4) . . . . ? C1 C2 C3 K1 76.0(4) . . . . ? C8 C3 C4 C5 -0.1(6) . . . . ? C2 C3 C4 C5 -177.6(4) . . . . ? K1 C3 C4 C5 119.1(4) . . . . ? C8 C3 C4 Sb1 177.4(3) . . . . ? C2 C3 C4 Sb1 -0.1(5) . . . . ? K1 C3 C4 Sb1 -63.4(2) . . . . ? C1 Sb1 C4 C3 -0.7(3) . . . . ? K1 Sb1 C4 C3 60.8(3) . . . . ? K1 Sb1 C4 C3 -112.0(3) 4_575 . . . ? C1 Sb1 C4 C5 176.5(4) . . . . ? K1 Sb1 C4 C5 -122.0(4) . . . . ? K1 Sb1 C4 C5 65.2(4) 4_575 . . . ? C3 C4 C5 C6 0.3(7) . . . . ? Sb1 C4 C5 C6 -176.7(3) . . . . ? C3 C4 C5 C10 179.0(4) . . . . ? Sb1 C4 C5 C10 1.9(6) . . . . ? C4 C5 C6 C7 -0.9(7) . . . . ? C10 C5 C6 C7 -179.5(5) . . . . ? C5 C6 C7 C8 1.2(7) . . . . ? C5 C6 C7 C9 -178.6(5) . . . . ? C6 C7 C8 C3 -0.9(7) . . . . ? C9 C7 C8 C3 178.8(5) . . . . ? C4 C3 C8 C7 0.4(7) . . . . ? C2 C3 C8 C7 177.7(4) . . . . ? K1 C3 C8 C7 -102.1(4) . . . . ? C2 C1 C11 C16 -164.8(5) . . . . ? Sb1 C1 C11 C16 17.7(7) . . . . ? K1 C1 C11 C16 111.9(5) . . . . ? C2 C1 C11 C12 16.8(8) . . . . ? Sb1 C1 C11 C12 -160.8(4) . . . . ? K1 C1 C11 C12 -66.5(5) . . . . ? C16 C11 C12 C13 0.2(8) . . . . ? C1 C11 C12 C13 178.7(5) . . . . ? C11 C12 C13 C14 -0.4(9) . . . . ? C11 C12 C13 C18 178.3(5) . . . . ? C12 C13 C14 C15 0.0(10) . . . . ? C18 C13 C14 C15 -178.7(6) . . . . ? C13 C14 C15 C16 0.6(10) . . . . ? C13 C14 C15 C17 -178.9(7) . . . . ? C14 C15 C16 C11 -0.8(9) . . . . ? C17 C15 C16 C11 178.7(6) . . . . ? C12 C11 C16 C15 0.4(8) . . . . ? C1 C11 C16 C15 -178.1(5) . . . . ? C1 C2 K1 N3 18.9(3) . . . . ? C3 C2 K1 N3 140.0(3) . . . . ? C1 C2 K1 N1 -127.4(3) . . . . ? C3 C2 K1 N1 -6.4(3) . . . . ? C1 C2 K1 N2 172(2) . . . . ? C3 C2 K1 N2 -67(3) . . . . ? C3 C2 K1 C1 121.0(4) . . . . ? C1 C2 K1 C3 -121.0(4) . . . . ? C1 C2 K1 Sb1 -43.9(2) . . . . ? C3 C2 K1 Sb1 77.1(2) . . . . ? C1 C2 K1 Sb1 115.8(3) . . . 4_576 ? C3 C2 K1 Sb1 -123.1(3) . . . 4_576 ? C2 C1 K1 N3 -163.6(3) . . . . ? C11 C1 K1 N3 -41.5(3) . . . . ? Sb1 C1 K1 N3 83.12(18) . . . . ? C2 C1 K1 N1 66.8(3) . . . . ? C11 C1 K1 N1 -171.1(3) . . . . ? Sb1 C1 K1 N1 -46.5(2) . . . . ? C2 C1 K1 N2 -178.9(3) . . . . ? C11 C1 K1 N2 -56.8(5) . . . . ? Sb1 C1 K1 N2 67.8(4) . . . . ? C11 C1 K1 C2 122.1(4) . . . . ? Sb1 C1 K1 C2 -113.3(3) . . . . ? C2 C1 K1 C3 32.0(3) . . . . ? C11 C1 K1 C3 154.1(4) . . . . ? Sb1 C1 K1 C3 -81.34(18) . . . . ? C2 C1 K1 Sb1 113.3(3) . . . . ? C11 C1 K1 Sb1 -124.6(4) . . . . ? C2 C1 K1 Sb1 -63.3(3) . . . 4_576 ? C11 C1 K1 Sb1 58.8(3) . . . 4_576 ? Sb1 C1 K1 Sb1 -176.63(12) . . . 4_576 ? C4 C3 K1 N3 65.7(3) . . . . ? C8 C3 K1 N3 -172.8(3) . . . . ? C2 C3 K1 N3 -54.8(3) . . . . ? C4 C3 K1 N1 -65.3(3) . . . . ? C8 C3 K1 N1 56.3(3) . . . . ? C2 C3 K1 N1 174.3(3) . . . . ? C4 C3 K1 N2 -65.7(4) . . . . ? C8 C3 K1 N2 55.9(5) . . . . ? C2 C3 K1 N2 173.8(3) . . . . ? C4 C3 K1 C2 120.4(4) . . . . ? C8 C3 K1 C2 -118.0(4) . . . . ? C4 C3 K1 C1 88.6(3) . . . . ? C8 C3 K1 C1 -149.8(4) . . . . ? C2 C3 K1 C1 -31.9(2) . . . . ? C4 C3 K1 Sb1 39.4(2) . . . . ? C8 C3 K1 Sb1 160.9(4) . . . . ? C2 C3 K1 Sb1 -81.1(3) . . . . ? C4 C3 K1 Sb1 177.0(2) . . . 4_576 ? C8 C3 K1 Sb1 -61.5(3) . . . 4_576 ? C2 C3 K1 Sb1 56.5(3) . . . 4_576 ? C4 Sb1 K1 N3 171.44(18) . . . . ? C1 Sb1 K1 N3 -99.1(2) . . . . ? K1 Sb1 K1 N3 -171.78(14) 4_575 . . . ? C4 Sb1 K1 N1 55.53(16) . . . . ? C1 Sb1 K1 N1 145.01(18) . . . . ? K1 Sb1 K1 N1 72.31(11) 4_575 . . . ? C4 Sb1 K1 N2 118.46(19) . . . . ? C1 Sb1 K1 N2 -152.1(2) . . . . ? K1 Sb1 K1 N2 135.23(14) 4_575 . . . ? C4 Sb1 K1 C2 -59.18(16) . . . . ? C1 Sb1 K1 C2 30.30(18) . . . . ? K1 Sb1 K1 C2 -42.40(12) 4_575 . . . ? C4 Sb1 K1 C1 -89.47(19) . . . . ? K1 Sb1 K1 C1 -72.70(16) 4_575 . . . ? C4 Sb1 K1 C3 -26.19(16) . . . . ? C1 Sb1 K1 C3 63.29(18) . . . . ? K1 Sb1 K1 C3 -9.41(12) 4_575 . . . ? C4 Sb1 K1 Sb1 -85.17(13) . . . 4_576 ? C1 Sb1 K1 Sb1 4.31(15) . . . 4_576 ? K1 Sb1 K1 Sb1 -68.39(9) 4_575 . . 4_576 ? N3 K1 N1 C20 -179.9(3) . . . . ? N2 K1 N1 C20 145.0(4) . . . . ? C2 K1 N1 C20 -32.1(4) . . . . ? C1 K1 N1 C20 -57.6(4) . . . . ? C3 K1 N1 C20 -34.7(4) . . . . ? Sb1 K1 N1 C20 -83.0(3) . . . . ? Sb1 K1 N1 C20 63.1(4) 4_576 . . . ? N3 K1 N1 C19 -65.2(4) . . . . ? N2 K1 N1 C19 -100.3(4) . . . . ? C2 K1 N1 C19 82.7(4) . . . . ? C1 K1 N1 C19 57.1(4) . . . . ? C3 K1 N1 C19 80.0(4) . . . . ? Sb1 K1 N1 C19 31.7(4) . . . . ? Sb1 K1 N1 C19 177.8(3) 4_576 . . . ? N3 K1 N1 C21 51.8(4) . . . . ? N2 K1 N1 C21 16.7(4) . . . . ? C2 K1 N1 C21 -160.3(4) . . . . ? C1 K1 N1 C21 174.1(3) . . . . ? C3 K1 N1 C21 -163.0(4) . . . . ? Sb1 K1 N1 C21 148.7(4) . . . . ? Sb1 K1 N1 C21 -65.2(4) 4_576 . . . ? N3 K1 N2 C22 -133.2(4) . . . . ? N1 K1 N2 C22 11.1(4) . . . . ? C2 K1 N2 C22 73(3) . . . . ? C1 K1 N2 C22 -116.0(5) . . . . ? C3 K1 N2 C22 11.6(5) . . . . ? Sb1 K1 N2 C22 -69.5(4) . . . . ? Sb1 K1 N2 C22 128.9(4) 4_576 . . . ? N3 K1 N2 C23 111.1(4) . . . . ? N1 K1 N2 C23 -104.6(4) . . . . ? C2 K1 N2 C23 -43(3) . . . . ? C1 K1 N2 C23 128.4(4) . . . . ? C3 K1 N2 C23 -104.0(4) . . . . ? Sb1 K1 N2 C23 174.9(3) . . . . ? Sb1 K1 N2 C23 13.2(4) 4_576 . . . ? N3 K1 N2 C24 -4.5(4) . . . . ? N1 K1 N2 C24 139.8(4) . . . . ? C2 K1 N2 C24 -158(2) . . . . ? C1 K1 N2 C24 12.7(6) . . . . ? C3 K1 N2 C24 140.3(4) . . . . ? Sb1 K1 N2 C24 59.2(4) . . . . ? Sb1 K1 N2 C24 -102.4(4) 4_576 . . . ? N1 K1 N3 C26 -178.0(5) . . . . ? N2 K1 N3 C26 -143.4(6) . . . . ? C2 K1 N3 C26 35.1(6) . . . . ? C1 K1 N3 C26 43.0(5) . . . . ? C3 K1 N3 C26 58.5(6) . . . . ? Sb1 K1 N3 C26 78.0(5) . . . . ? Sb1 K1 N3 C26 -51.5(5) 4_576 . . . ? N1 K1 N3 C25 -57.9(5) . . . . ? N2 K1 N3 C25 -23.3(5) . . . . ? C2 K1 N3 C25 155.2(5) . . . . ? C1 K1 N3 C25 163.1(5) . . . . ? C3 K1 N3 C25 178.6(4) . . . . ? Sb1 K1 N3 C25 -161.9(5) . . . . ? Sb1 K1 N3 C25 68.7(5) 4_576 . . . ? N1 K1 N3 C27 62.7(5) . . . . ? N2 K1 N3 C27 97.4(5) . . . . ? C2 K1 N3 C27 -84.1(5) . . . . ? C1 K1 N3 C27 -76.2(5) . . . . ? C3 K1 N3 C27 -60.8(6) . . . . ? Sb1 K1 N3 C27 -41.3(5) . . . . ? Sb1 K1 N3 C27 -170.7(5) 4_576 . . . ? C20 N1 C21 C22 -173.3(5) . . . . ? C19 N1 C21 C22 65.1(7) . . . . ? K1 N1 C21 C22 -43.7(6) . . . . ? C23 N2 C22 C21 68.0(7) . . . . ? C24 N2 C22 C21 -167.5(5) . . . . ? K1 N2 C22 C21 -38.1(6) . . . . ? N1 C21 C22 N2 56.3(7) . . . . ? C22 N2 C24 C25 162.7(6) . . . . ? C23 N2 C24 C25 -73.1(7) . . . . ? K1 N2 C24 C25 32.2(7) . . . . ? C26 N3 C25 C24 171.9(7) . . . . ? C27 N3 C25 C24 -65.9(8) . . . . ? K1 N3 C25 C24 52.0(8) . . . . ? N2 C24 C25 N3 -59.4(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.747 _refine_diff_density_min -0.929 _refine_diff_density_rms 0.072