# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1532 data_ms4 # SUBMISSION DETAILS _audit_creation_method 'manual editing of SHELXL template' _publ_contact_author_name 'Dr Tristram Chivers' _publ_contact_author_address ; Department of Chemistry University of Calgary Calgary Alberta T2N 1N4 Canada ; _publ_contact_author_email chivers@ucalgary.ca _publ_contact_author_fax '001 403 289 9488' _publ_contact_author_phone '001 403 220 5741' _publ_contact_letter ; To: Royal Society of Chemistry Please accept the following CIF data which is being submitted in support of an upcoming communication to be published in Chem. Commun. (No: B000357n). Please forward any questions concerning this CIF to Dr. Masood Parvez (parvez@ucalgary.ca). ; _publ_requested_journal 'Chem. Commun.' # TITLE AND AUTHOR LIST _publ_section_title ; An extended network of twenty-membered K6Se6P4N4 rings: X-ray structure of {[(THF)K[tBuN(Se)P(mu-NtBu)2P(Se)NtBu]K(THF)2]2}n ; loop_ _publ_author_name _publ_author_address 'Chivers, Tristram' ; Department of Chemistry University of Calgary 2500 University Drive, NW Calgary, Alberta T2N 1N4 Canada ; 'Krahn, Mark' ; Department of Chemistry University of Calgary 2500 University Drive, NW Calgary, Alberta T2N 1N4 Canada ; 'Parvez, Masood' ; Department of Chemistry University of Calgary 2500 University Drive, NW Calgary, Alberta T2N 1N4 Canada ; _publ_section_acknowledgements ; NSERC (Canada) ; # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H36 K2 N4 P2 Se2, 3(C4H8O)' _chemical_formula_sum 'C28 H60 K2 N4 O3 P2 Se2' _chemical_formula_weight 798.86 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' 'P' 'P' 0.1023 0.0942 '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' 'Se' 'Se' -0.0929 2.2259 '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/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.733(11) _cell_length_b 14.085(10) _cell_length_c 26.138(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.99(5) _cell_angle_gamma 90.00 _cell_volume 3951(5) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 12 _cell_measurement_theta_min 18.2 _cell_measurement_theta_max 21.05 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 2.194 _exptl_absorpt_correction_type 'empirical, psi-scans' _exptl_absorpt_correction_T_min 0.4067 _exptl_absorpt_correction_T_max 0.6680 _exptl_absorpt_process_details ; psi-scans (North, Phillips & Matthews, 1968) ; _exptl_special_details ; ? ; # EXPERIMENTAL DETAILS _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.2 _diffrn_reflns_number 6958 _diffrn_reflns_av_R_equivalents 0.120 _diffrn_reflns_av_sigmaI/netI 0.336 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.06 _reflns_number_total 6958 _reflns_number_gt 2135 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan (MSC, 1995)' _computing_publication_material 'teXsan (MSC, 1995)' # REFINEMENT DATA _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^)+(0.0744P)^2^+9.9743P] 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 0.0025(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6958 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2959 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.2380 _refine_ls_wR_factor_gt 0.1652 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Se1 Se -0.34368(14) 1.08197(10) 0.69091(5) 0.0542(5) Uani 1 1 d . . . Se2 Se -0.55397(13) 0.87818(10) 0.56062(5) 0.0506(5) Uani 1 1 d . . . K1 K -0.4473(3) 1.0951(2) 0.56932(10) 0.0534(9) Uani 1 1 d . . . K2 K -0.1933(3) 0.7009(2) 0.68594(10) 0.0600(10) Uani 1 1 d . . . P1 P -0.2847(3) 0.9385(2) 0.67314(11) 0.0437(10) Uani 1 1 d . . . P2 P -0.3921(3) 0.8333(2) 0.60475(11) 0.0416(10) Uani 1 1 d . . . O1 O -0.6626(11) 1.1692(9) 0.5994(4) 0.084(3) Uani 1 1 d . . . O2 O -0.2856(10) 1.2436(7) 0.5586(3) 0.077(3) Uani 1 1 d . . . O3 O 0.0316(11) 0.6386(10) 0.6550(5) 0.114(5) Uani 1 1 d . . . N1 N -0.2805(9) 0.9206(7) 0.6075(3) 0.043(3) Uani 1 1 d . . . N2 N -0.4052(9) 0.8589(7) 0.6681(3) 0.038(3) Uani 1 1 d . . . N3 N -0.1742(9) 0.8940(8) 0.7034(4) 0.052(3) Uani 1 1 d . . . N4 N -0.3388(10) 0.7318(7) 0.5974(3) 0.046(3) Uani 1 1 d . . . C1 C -0.1705(12) 0.9342(10) 0.5751(4) 0.046(4) Uani 1 1 d . . . C2 C -0.1117(12) 1.0308(10) 0.5841(4) 0.061(4) Uani 1 1 d . . . H2A H -0.0841 1.0357 0.6192 0.092 Uiso 1 1 calc R . . H2B H -0.1719 1.0796 0.5768 0.092 Uiso 1 1 calc R . . H2C H -0.0417 1.0383 0.5621 0.092 Uiso 1 1 calc R . . C3 C -0.0745(12) 0.8552(10) 0.5836(5) 0.065(4) Uani 1 1 d . . . H3A H -0.0354 0.8627 0.6167 0.097 Uiso 1 1 calc R . . H3B H -0.0125 0.8586 0.5577 0.097 Uiso 1 1 calc R . . H3C H -0.1154 0.7946 0.5819 0.097 Uiso 1 1 calc R . . C4 C -0.2155(12) 0.9291(10) 0.5185(4) 0.060(4) Uani 1 1 d . . . H4A H -0.1448 0.9314 0.4965 0.090 Uiso 1 1 calc R . . H4B H -0.2695 0.9818 0.5111 0.090 Uiso 1 1 calc R . . H4C H -0.2600 0.8708 0.5128 0.090 Uiso 1 1 calc R . . C5 C -0.5071(12) 0.8368(10) 0.7053(4) 0.044(4) Uani 1 1 d . . . C6 C -0.6121(12) 0.9092(10) 0.6987(4) 0.058(4) Uani 1 1 d . . . H6A H -0.6710 0.9013 0.7255 0.087 Uiso 1 1 calc R . . H6B H -0.6532 0.8997 0.6661 0.087 Uiso 1 1 calc R . . H6C H -0.5781 0.9722 0.7001 0.087 Uiso 1 1 calc R . . C7 C -0.4509(13) 0.8408(10) 0.7588(4) 0.066(5) Uani 1 1 d . . . H7A H -0.3859 0.7942 0.7620 0.099 Uiso 1 1 calc R . . H7B H -0.5143 0.8278 0.7833 0.099 Uiso 1 1 calc R . . H7C H -0.4169 0.9029 0.7650 0.099 Uiso 1 1 calc R . . C8 C -0.5543(13) 0.7379(11) 0.6926(5) 0.073(5) Uani 1 1 d . . . H8A H -0.4891 0.6926 0.6989 0.109 Uiso 1 1 calc R . . H8B H -0.5794 0.7354 0.6572 0.109 Uiso 1 1 calc R . . H8C H -0.6242 0.7233 0.7135 0.109 Uiso 1 1 calc R . . C9 C -0.0824(14) 0.9295(12) 0.7413(5) 0.068(5) Uani 1 1 d . . . C10 C -0.0069(14) 1.0113(12) 0.7215(6) 0.087(5) Uani 1 1 d . . . H10A H 0.0490 1.0334 0.7480 0.131 Uiso 1 1 calc R . . H10B H -0.0617 1.0619 0.7113 0.131 Uiso 1 1 calc R . . H10C H 0.0402 0.9907 0.6927 0.131 Uiso 1 1 calc R . . C11 C -0.1470(15) 0.9603(13) 0.7908(5) 0.104(7) Uani 1 1 d . . . H11A H -0.2003 0.9101 0.8022 0.156 Uiso 1 1 calc R . . H11B H -0.1958 1.0162 0.7842 0.156 Uiso 1 1 calc R . . H11C H -0.0852 0.9736 0.8168 0.156 Uiso 1 1 calc R . . C12 C 0.0018(16) 0.8487(12) 0.7549(7) 0.118(8) Uani 1 1 d . . . H12A H -0.0449 0.8004 0.7720 0.176 Uiso 1 1 calc R . . H12B H 0.0677 0.8708 0.7771 0.176 Uiso 1 1 calc R . . H12C H 0.0366 0.8229 0.7243 0.176 Uiso 1 1 calc R . . C13 C -0.3712(17) 0.6545(11) 0.5612(5) 0.068(5) Uani 1 1 d . . . C14 C -0.2725(17) 0.5771(11) 0.5710(6) 0.103(6) Uani 1 1 d . . . H14A H -0.1917 0.6014 0.5628 0.154 Uiso 1 1 calc R . . H14B H -0.2909 0.5230 0.5498 0.154 Uiso 1 1 calc R . . H14C H -0.2734 0.5587 0.6063 0.154 Uiso 1 1 calc R . . C15 C -0.4974(17) 0.6116(11) 0.5720(6) 0.093(6) Uani 1 1 d . . . H15A H -0.5011 0.5944 0.6074 0.140 Uiso 1 1 calc R . . H15B H -0.5095 0.5561 0.5512 0.140 Uiso 1 1 calc R . . H15C H -0.5615 0.6571 0.5641 0.140 Uiso 1 1 calc R . . C16 C -0.3658(18) 0.6815(11) 0.5048(5) 0.108(7) Uani 1 1 d . . . H16A H -0.4253 0.7308 0.4976 0.162 Uiso 1 1 calc R . . H16B H -0.3851 0.6269 0.4841 0.162 Uiso 1 1 calc R . . H16C H -0.2837 0.7037 0.4971 0.162 Uiso 1 1 calc R . . C17 C -0.653(2) 1.2559(15) 0.6275(6) 0.121(8) Uani 1 1 d . . . H17A H -0.5738 1.2599 0.6457 0.145 Uiso 1 1 calc R . . H17B H -0.6616 1.3102 0.6049 0.145 Uiso 1 1 calc R . . C18 C -0.753(2) 1.2522(19) 0.6622(11) 0.188(14) Uani 1 1 d . . . H18A H -0.7220 1.2631 0.6968 0.225 Uiso 1 1 calc R . . H18B H -0.8136 1.3010 0.6538 0.225 Uiso 1 1 calc R . . C19 C -0.807(3) 1.1633(18) 0.6586(11) 0.241(19) Uani 1 1 d . . . H19A H -0.7881 1.1266 0.6891 0.289 Uiso 1 1 calc R . . H19B H -0.8972 1.1696 0.6555 0.289 Uiso 1 1 calc R . . C20 C -0.7630(19) 1.1186(14) 0.6170(6) 0.107(7) Uani 1 1 d . . . H20A H -0.8274 1.1149 0.5905 0.129 Uiso 1 1 calc R . . H20B H -0.7376 1.0545 0.6259 0.129 Uiso 1 1 calc R . . C21 C -0.2167(19) 1.2778(14) 0.5185(6) 0.106(7) Uani 1 1 d . . . H21A H -0.2635 1.3263 0.5001 0.127 Uiso 1 1 calc R . . H21B H -0.1983 1.2268 0.4948 0.127 Uiso 1 1 calc R . . C22 C -0.1010(17) 1.3179(14) 0.5394(6) 0.103(6) Uani 1 1 d . . . H22A H -0.0839 1.3791 0.5240 0.123 Uiso 1 1 calc R . . H22B H -0.0313 1.2758 0.5333 0.123 Uiso 1 1 calc R . . C23 C -0.1235(19) 1.3280(15) 0.5958(6) 0.120(8) Uani 1 1 d . . . H23A H -0.0680 1.2872 0.6156 0.144 Uiso 1 1 calc R . . H23B H -0.1117 1.3932 0.6069 0.144 Uiso 1 1 calc R . . C24 C -0.252(2) 1.2990(12) 0.6012(5) 0.109(8) Uani 1 1 d . . . H24A H -0.2612 1.2624 0.6323 0.131 Uiso 1 1 calc R . . H24B H -0.3054 1.3543 0.6030 0.131 Uiso 1 1 calc R . . C25 C 0.095(2) 0.6351(17) 0.6078(7) 0.137(9) Uani 1 1 d . . . H25A H 0.1489 0.6902 0.6046 0.164 Uiso 1 1 calc R . . H25B H 0.0361 0.6349 0.5794 0.164 Uiso 1 1 calc R . . C26 C 0.170(2) 0.5490(16) 0.6074(7) 0.123(7) Uani 1 1 d . . . H26A H 0.2476 0.5587 0.5900 0.147 Uiso 1 1 calc R . . H26B H 0.1244 0.4971 0.5911 0.147 Uiso 1 1 calc R . . C27 C 0.1906(19) 0.5309(14) 0.6631(7) 0.111(7) Uani 1 1 d . . . H27A H 0.1707 0.4656 0.6714 0.134 Uiso 1 1 calc R . . H27B H 0.2769 0.5429 0.6726 0.134 Uiso 1 1 calc R . . C28 C 0.1069(18) 0.5970(16) 0.6903(7) 0.118(8) Uani 1 1 d . . . H28A H 0.0578 0.5625 0.7149 0.142 Uiso 1 1 calc R . . H28B H 0.1555 0.6447 0.7085 0.142 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 Se1 0.0764(12) 0.0526(9) 0.0340(7) -0.0065(7) 0.0119(7) -0.0079(9) Se2 0.0576(10) 0.0590(10) 0.0349(7) 0.0031(7) -0.0042(6) -0.0085(8) K1 0.063(2) 0.058(2) 0.0399(16) -0.0001(15) 0.0106(14) -0.0064(17) K2 0.070(2) 0.067(2) 0.0435(17) 0.0094(17) 0.0022(16) 0.0064(19) P1 0.056(3) 0.053(2) 0.0225(16) -0.0023(16) 0.0082(16) -0.015(2) P2 0.057(3) 0.049(2) 0.0188(15) -0.0008(15) 0.0074(15) -0.0084(19) O1 0.088(9) 0.105(9) 0.059(7) -0.028(7) 0.025(6) -0.009(7) O2 0.124(10) 0.080(7) 0.028(5) -0.009(5) 0.002(6) -0.039(7) O3 0.095(10) 0.173(13) 0.076(8) 0.039(9) 0.028(7) 0.058(9) N1 0.049(7) 0.055(7) 0.025(5) -0.013(5) 0.010(5) -0.012(6) N2 0.046(7) 0.046(7) 0.022(5) 0.001(5) 0.009(5) -0.003(5) N3 0.046(7) 0.070(8) 0.040(6) 0.002(6) -0.003(5) -0.014(6) N4 0.073(8) 0.031(6) 0.034(6) -0.006(5) 0.005(5) 0.003(6) C1 0.054(9) 0.065(10) 0.019(6) 0.004(6) 0.008(6) 0.005(8) C2 0.062(10) 0.086(12) 0.036(7) 0.007(8) 0.019(7) -0.026(9) C3 0.053(10) 0.076(11) 0.066(10) 0.003(8) 0.027(8) -0.003(9) C4 0.069(10) 0.089(11) 0.023(6) 0.015(7) 0.004(6) -0.007(9) C5 0.045(9) 0.067(10) 0.021(6) 0.009(6) 0.011(6) -0.012(8) C6 0.051(9) 0.085(11) 0.040(7) 0.001(8) 0.013(6) -0.013(9) C7 0.080(11) 0.100(13) 0.018(6) 0.002(7) 0.012(7) -0.028(9) C8 0.071(12) 0.082(12) 0.066(10) 0.010(9) 0.028(8) -0.025(10) C9 0.048(10) 0.100(13) 0.057(10) 0.015(9) -0.003(8) -0.013(10) C10 0.074(13) 0.111(15) 0.076(11) 0.005(10) -0.018(9) -0.025(12) C11 0.117(16) 0.157(19) 0.036(9) 0.013(10) -0.015(9) -0.048(14) C12 0.106(16) 0.107(16) 0.136(17) 0.004(13) -0.096(14) -0.025(13) C13 0.107(15) 0.050(11) 0.048(9) 0.004(8) 0.001(9) -0.007(10) C14 0.142(19) 0.058(12) 0.108(14) -0.026(11) 0.006(13) 0.012(12) C15 0.139(18) 0.057(12) 0.083(12) -0.016(9) -0.003(12) -0.007(12) C16 0.20(2) 0.069(12) 0.053(10) -0.010(9) 0.022(12) -0.031(13) C17 0.16(2) 0.133(18) 0.069(12) -0.027(12) 0.029(13) -0.081(16) C18 0.12(2) 0.17(3) 0.27(3) -0.15(2) 0.10(2) -0.057(18) C19 0.29(4) 0.15(2) 0.29(4) -0.14(3) 0.22(3) -0.12(3) C20 0.123(17) 0.129(17) 0.070(12) -0.022(12) 0.031(12) -0.029(15) C21 0.143(19) 0.122(17) 0.054(11) -0.018(11) 0.020(12) -0.047(14) C22 0.108(16) 0.144(18) 0.055(11) -0.004(11) 0.003(10) -0.024(14) C23 0.14(2) 0.15(2) 0.064(12) -0.028(12) -0.039(12) -0.052(16) C24 0.20(2) 0.088(14) 0.041(10) -0.020(9) 0.025(12) -0.071(15) C25 0.14(2) 0.20(3) 0.066(12) 0.056(15) 0.020(13) 0.067(19) C26 0.13(2) 0.15(2) 0.090(15) 0.018(14) 0.032(13) 0.022(16) C27 0.119(18) 0.130(18) 0.086(14) 0.038(13) 0.018(13) 0.023(15) C28 0.098(16) 0.18(2) 0.082(13) 0.058(15) 0.015(12) 0.032(15) # MOLECULAR GEOMETRY _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 Se1 P1 2.171(4) . ? Se1 K1 3.354(3) . ? Se1 K2 3.644(3) 2_456 ? Se2 P2 2.163(4) . ? Se2 K1 3.270(4) . ? Se2 K1 3.418(3) 3_476 ? K1 O1 2.667(11) . ? K1 O2 2.735(10) . ? K1 N1 3.191(11) . ? K1 Se2 3.418(3) 3_476 ? K1 C17 3.53(2) . ? K1 P2 3.846(5) . ? K1 K1 4.632(6) 3_476 ? K2 O3 2.705(11) . ? K2 N3 2.766(11) . ? K2 N4 2.804(10) . ? K2 N2 3.210(10) . ? K2 P1 3.502(5) . ? K2 P2 3.518(5) . ? K2 Se1 3.644(3) 2_446 ? P1 N3 1.546(10) . ? P1 N2 1.715(10) . ? P1 N1 1.735(9) . ? P1 P2 2.579(5) . ? P2 N4 1.552(10) . ? P2 N2 1.703(8) . ? P2 N1 1.717(10) . ? O1 C20 1.377(18) . ? O1 C17 1.428(18) . ? O2 C21 1.381(16) . ? O2 C24 1.402(15) . ? O3 C28 1.349(17) . ? O3 C25 1.423(18) . ? N1 C1 1.477(14) . ? N2 C5 1.509(14) . ? N3 C9 1.473(16) . ? N4 C13 1.480(16) . ? C1 C2 1.517(17) . ? C1 C3 1.531(17) . ? C1 C4 1.550(14) . ? C5 C7 1.514(15) . ? C5 C8 1.517(17) . ? C5 C6 1.528(17) . ? C9 C12 1.49(2) . ? C9 C10 1.505(19) . ? C9 C11 1.540(19) . ? C13 C15 1.51(2) . ? C13 C16 1.524(17) . ? C13 C14 1.54(2) . ? C17 C18 1.41(2) . ? C18 C19 1.39(3) . ? C19 C20 1.35(2) . ? C21 C22 1.46(2) . ? C22 C23 1.51(2) . ? C23 C24 1.45(2) . ? C25 C26 1.45(2) . ? C26 C27 1.49(2) . ? C27 C28 1.48(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 P1 Se1 K1 86.66(11) . . ? P1 Se1 K2 126.10(11) . 2_456 ? K1 Se1 K2 147.23(9) . 2_456 ? P2 Se2 K1 87.64(12) . . ? P2 Se2 K1 123.03(12) . 3_476 ? K1 Se2 K1 87.64(8) . 3_476 ? O1 K1 O2 106.6(4) . . ? O1 K1 N1 133.9(3) . . ? O2 K1 N1 105.5(3) . . ? O1 K1 Se2 94.7(3) . . ? O2 K1 Se2 158.4(3) . . ? N1 K1 Se2 59.71(19) . . ? O1 K1 Se1 91.0(2) . . ? O2 K1 Se1 86.5(2) . . ? N1 K1 Se1 59.07(16) . . ? Se2 K1 Se1 97.14(8) . . ? O1 K1 Se2 105.6(2) . 3_476 ? O2 K1 Se2 78.49(19) . 3_476 ? N1 K1 Se2 112.58(17) . 3_476 ? Se2 K1 Se2 92.36(8) . 3_476 ? Se1 K1 Se2 160.21(11) . 3_476 ? O1 K1 C17 21.4(4) . . ? O2 K1 C17 87.5(4) . . ? N1 K1 C17 135.4(3) . . ? Se2 K1 C17 114.1(3) . . ? Se1 K1 C17 80.0(3) . . ? Se2 K1 C17 111.8(3) 3_476 . ? O1 K1 P2 115.8(3) . . ? O2 K1 P2 131.5(3) . . ? N1 K1 P2 26.18(18) . . ? Se2 K1 P2 34.20(7) . . ? Se1 K1 P2 70.84(7) . . ? Se2 K1 P2 109.98(9) 3_476 . ? C17 K1 P2 127.4(3) . . ? O1 K1 K1 104.8(3) . 3_476 ? O2 K1 K1 120.6(2) . 3_476 ? N1 K1 K1 85.83(18) . 3_476 ? Se2 K1 K1 47.50(6) . 3_476 ? Se1 K1 K1 141.45(12) . 3_476 ? Se2 K1 K1 44.86(6) 3_476 3_476 ? C17 K1 K1 124.2(3) . 3_476 ? P2 K1 K1 70.62(9) . 3_476 ? O3 K2 N3 107.7(4) . . ? O3 K2 N4 106.9(3) . . ? N3 K2 N4 91.2(3) . . ? O3 K2 N2 144.6(3) . . ? N3 K2 N2 52.6(3) . . ? N4 K2 N2 52.4(2) . . ? O3 K2 P1 122.1(3) . . ? N3 K2 P1 25.2(2) . . ? N4 K2 P1 67.8(2) . . ? N2 K2 P1 29.20(18) . . ? O3 K2 P2 121.8(3) . . ? N3 K2 P2 67.7(2) . . ? N4 K2 P2 25.35(19) . . ? N2 K2 P2 28.86(15) . . ? P1 K2 P2 43.10(9) . . ? O3 K2 Se1 91.8(3) . 2_446 ? N3 K2 Se1 107.5(2) . 2_446 ? N4 K2 Se1 148.3(2) . 2_446 ? N2 K2 Se1 120.87(17) . 2_446 ? P1 K2 Se1 123.35(10) . 2_446 ? P2 K2 Se1 146.32(11) . 2_446 ? N3 P1 N2 110.2(5) . . ? N3 P1 N1 114.4(6) . . ? N2 P1 N1 82.0(4) . . ? N3 P1 Se1 119.5(4) . . ? N2 P1 Se1 113.7(4) . . ? N1 P1 Se1 111.1(4) . . ? N3 P1 P2 116.8(4) . . ? N2 P1 P2 40.8(3) . . ? N1 P1 P2 41.4(3) . . ? Se1 P1 P2 123.69(18) . . ? N3 P1 K2 49.7(4) . . ? N2 P1 K2 65.9(3) . . ? N1 P1 K2 86.8(4) . . ? Se1 P1 K2 162.11(14) . . ? P2 P1 K2 68.78(13) . . ? N4 P2 N2 110.6(5) . . ? N4 P2 N1 114.0(6) . . ? N2 P2 N1 82.9(4) . . ? N4 P2 Se2 119.8(4) . . ? N2 P2 Se2 112.2(4) . . ? N1 P2 Se2 111.5(4) . . ? N4 P2 P1 117.0(4) . . ? N2 P2 P1 41.2(3) . . ? N1 P2 P1 41.9(3) . . ? Se2 P2 P1 123.16(18) . . ? N4 P2 K2 50.7(4) . . ? N2 P2 K2 65.5(3) . . ? N1 P2 K2 86.5(4) . . ? Se2 P2 K2 161.74(16) . . ? P1 P2 K2 68.11(13) . . ? N4 P2 K1 155.3(4) . . ? N2 P2 K1 90.9(3) . . ? N1 P2 K1 55.1(4) . . ? Se2 P2 K1 58.16(10) . . ? P1 P2 K1 71.40(13) . . ? K2 P2 K1 137.97(12) . . ? C20 O1 C17 108.7(13) . . ? C20 O1 K1 125.7(12) . . ? C17 O1 K1 115.6(12) . . ? C21 O2 C24 106.0(12) . . ? C21 O2 K1 134.0(9) . . ? C24 O2 K1 120.0(9) . . ? C28 O3 C25 106.6(13) . . ? C28 O3 K2 117.7(11) . . ? C25 O3 K2 135.7(11) . . ? C1 N1 P2 129.2(8) . . ? C1 N1 P1 125.6(8) . . ? P2 N1 P1 96.7(5) . . ? C1 N1 K1 99.8(7) . . ? P2 N1 K1 98.7(4) . . ? P1 N1 K1 100.0(4) . . ? C5 N2 P2 131.0(8) . . ? C5 N2 P1 129.8(8) . . ? P2 N2 P1 98.0(5) . . ? C5 N2 K2 106.4(7) . . ? P2 N2 K2 85.7(4) . . ? P1 N2 K2 84.9(4) . . ? C9 N3 P1 134.8(11) . . ? C9 N3 K2 119.5(9) . . ? P1 N3 K2 105.1(5) . . ? C13 N4 P2 132.4(10) . . ? C13 N4 K2 122.3(8) . . ? P2 N4 K2 104.0(5) . . ? N1 C1 C2 111.2(10) . . ? N1 C1 C3 111.4(10) . . ? C2 C1 C3 110.6(11) . . ? N1 C1 C4 107.6(10) . . ? C2 C1 C4 108.2(10) . . ? C3 C1 C4 107.6(10) . . ? N2 C5 C7 107.8(10) . . ? N2 C5 C8 106.9(10) . . ? C7 C5 C8 111.3(11) . . ? N2 C5 C6 109.3(10) . . ? C7 C5 C6 111.2(11) . . ? C8 C5 C6 110.2(11) . . ? N3 C9 C12 107.2(13) . . ? N3 C9 C10 112.7(12) . . ? C12 C9 C10 109.8(13) . . ? N3 C9 C11 110.8(12) . . ? C12 C9 C11 107.1(14) . . ? C10 C9 C11 109.1(14) . . ? N4 C13 C15 112.1(13) . . ? N4 C13 C16 115.0(12) . . ? C15 C13 C16 109.2(14) . . ? N4 C13 C14 105.2(12) . . ? C15 C13 C14 107.6(13) . . ? C16 C13 C14 107.4(14) . . ? C18 C17 O1 104.5(15) . . ? C18 C17 K1 137.7(17) . . ? O1 C17 K1 43.0(9) . . ? C19 C18 C17 108.2(18) . . ? C20 C19 C18 109(2) . . ? C19 C20 O1 108.4(17) . . ? O2 C21 C22 108.3(14) . . ? C21 C22 C23 104.7(15) . . ? C24 C23 C22 103.7(13) . . ? O2 C24 C23 108.3(14) . . ? O3 C25 C26 108.0(15) . . ? C25 C26 C27 102.0(16) . . ? C28 C27 C26 106.2(16) . . ? O3 C28 C27 107.8(16) . . ? 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 P2 Se2 K1 O1 -131.0(2) . . . . ? K1 Se2 K1 O1 105.8(2) 3_476 . . . ? P2 Se2 K1 O2 59.2(6) . . . . ? K1 Se2 K1 O2 -64.0(6) 3_476 . . . ? P2 Se2 K1 N1 8.31(19) . . . . ? K1 Se2 K1 N1 -114.90(19) 3_476 . . . ? P2 Se2 K1 Se1 -39.39(11) . . . . ? K1 Se2 K1 Se1 -162.60(12) 3_476 . . . ? P2 Se2 K1 Se2 123.21(12) . . . 3_476 ? K1 Se2 K1 Se2 0.0 3_476 . . 3_476 ? P2 Se2 K1 C17 -121.6(4) . . . . ? K1 Se2 K1 C17 115.2(4) 3_476 . . . ? K1 Se2 K1 P2 -123.21(12) 3_476 . . . ? P2 Se2 K1 K1 123.21(12) . . . 3_476 ? P1 Se1 K1 O1 133.4(3) . . . . ? K2 Se1 K1 O1 -46.5(3) 2_456 . . . ? P1 Se1 K1 O2 -120.0(3) . . . . ? K2 Se1 K1 O2 60.1(3) 2_456 . . . ? P1 Se1 K1 N1 -9.6(2) . . . . ? K2 Se1 K1 N1 170.6(2) 2_456 . . . ? P1 Se1 K1 Se2 38.56(13) . . . . ? K2 Se1 K1 Se2 -141.30(14) 2_456 . . . ? P1 Se1 K1 Se2 -79.5(3) . . . 3_476 ? K2 Se1 K1 Se2 100.6(3) 2_456 . . 3_476 ? P1 Se1 K1 C17 151.9(3) . . . . ? K2 Se1 K1 C17 -28.0(3) 2_456 . . . ? P1 Se1 K1 P2 16.38(11) . . . . ? K2 Se1 K1 P2 -163.49(15) 2_456 . . . ? P1 Se1 K1 K1 17.8(2) . . . 3_476 ? K2 Se1 K1 K1 -162.02(15) 2_456 . . 3_476 ? K1 Se1 P1 N3 152.9(5) . . . . ? K2 Se1 P1 N3 -27.2(5) 2_456 . . . ? K1 Se1 P1 N2 -74.1(3) . . . . ? K2 Se1 P1 N2 105.8(3) 2_456 . . . ? K1 Se1 P1 N1 16.3(4) . . . . ? K2 Se1 P1 N1 -163.8(4) 2_456 . . . ? K1 Se1 P1 P2 -28.52(17) . . . . ? K2 Se1 P1 P2 151.39(14) 2_456 . . . ? K1 Se1 P1 K2 -159.0(5) . . . . ? K2 Se1 P1 K2 20.9(6) 2_456 . . . ? O3 K2 P1 N3 -60.8(6) . . . . ? N4 K2 P1 N3 -157.3(6) . . . . ? N2 K2 P1 N3 151.0(6) . . . . ? P2 K2 P1 N3 -164.6(5) . . . . ? Se1 K2 P1 N3 56.4(5) 2_446 . . . ? O3 K2 P1 N2 148.2(5) . . . . ? N3 K2 P1 N2 -151.0(6) . . . . ? N4 K2 P1 N2 51.6(4) . . . . ? P2 K2 P1 N2 44.3(3) . . . . ? Se1 K2 P1 N2 -94.7(3) 2_446 . . . ? O3 K2 P1 N1 65.5(5) . . . . ? N3 K2 P1 N1 126.3(6) . . . . ? N4 K2 P1 N1 -31.1(4) . . . . ? N2 K2 P1 N1 -82.7(5) . . . . ? P2 K2 P1 N1 -38.4(3) . . . . ? Se1 K2 P1 N1 -177.4(3) 2_446 . . . ? O3 K2 P1 Se1 -118.9(6) . . . . ? N3 K2 P1 Se1 -58.1(7) . . . . ? N4 K2 P1 Se1 144.6(6) . . . . ? N2 K2 P1 Se1 92.9(6) . . . . ? P2 K2 P1 Se1 137.3(6) . . . . ? Se1 K2 P1 Se1 -1.7(6) 2_446 . . . ? O3 K2 P1 P2 103.9(4) . . . . ? N3 K2 P1 P2 164.6(5) . . . . ? N4 K2 P1 P2 7.3(2) . . . . ? N2 K2 P1 P2 -44.3(3) . . . . ? Se1 K2 P1 P2 -139.00(15) 2_446 . . . ? K1 Se2 P2 N4 -151.2(5) . . . . ? K1 Se2 P2 N4 -65.6(5) 3_476 . . . ? K1 Se2 P2 N2 76.5(4) . . . . ? K1 Se2 P2 N2 162.2(4) 3_476 . . . ? K1 Se2 P2 N1 -14.4(3) . . . . ? K1 Se2 P2 N1 71.2(4) 3_476 . . . ? K1 Se2 P2 P1 31.31(17) . . . . ? K1 Se2 P2 P1 116.96(16) 3_476 . . . ? K1 Se2 P2 K2 155.3(5) . . . . ? K1 Se2 P2 K2 -119.0(4) 3_476 . . . ? K1 Se2 P2 K1 85.65(11) 3_476 . . . ? N3 P1 P2 N4 -0.7(6) . . . . ? N2 P1 P2 N4 -91.1(7) . . . . ? N1 P1 P2 N4 96.6(7) . . . . ? Se1 P1 P2 N4 -179.3(4) . . . . ? K2 P1 P2 N4 -13.8(4) . . . . ? N3 P1 P2 N2 90.4(7) . . . . ? N1 P1 P2 N2 -172.3(8) . . . . ? Se1 P1 P2 N2 -88.2(5) . . . . ? K2 P1 P2 N2 77.3(5) . . . . ? N3 P1 P2 N1 -97.3(7) . . . . ? N2 P1 P2 N1 172.3(8) . . . . ? Se1 P1 P2 N1 84.1(5) . . . . ? K2 P1 P2 N1 -110.4(5) . . . . ? N3 P1 P2 Se2 176.8(4) . . . . ? N2 P1 P2 Se2 86.5(5) . . . . ? N1 P1 P2 Se2 -85.8(5) . . . . ? Se1 P1 P2 Se2 -1.7(3) . . . . ? K2 P1 P2 Se2 163.75(18) . . . . ? N3 P1 P2 K2 13.1(4) . . . . ? N2 P1 P2 K2 -77.3(5) . . . . ? N1 P1 P2 K2 110.4(5) . . . . ? Se1 P1 P2 K2 -165.49(19) . . . . ? N3 P1 P2 K1 -155.4(5) . . . . ? N2 P1 P2 K1 114.2(5) . . . . ? N1 P1 P2 K1 -58.1(5) . . . . ? Se1 P1 P2 K1 26.02(16) . . . . ? K2 P1 P2 K1 -168.49(10) . . . . ? O3 K2 P2 N4 59.4(6) . . . . ? N3 K2 P2 N4 157.1(6) . . . . ? N2 K2 P2 N4 -151.0(6) . . . . ? P1 K2 P2 N4 164.1(5) . . . . ? Se1 K2 P2 N4 -114.7(5) 2_446 . . . ? O3 K2 P2 N2 -149.6(5) . . . . ? N3 K2 P2 N2 -51.9(4) . . . . ? N4 K2 P2 N2 151.0(6) . . . . ? P1 K2 P2 N2 -44.9(4) . . . . ? Se1 K2 P2 N2 36.3(4) 2_446 . . . ? O3 K2 P2 N1 -65.8(5) . . . . ? N3 K2 P2 N1 31.9(4) . . . . ? N4 K2 P2 N1 -125.2(6) . . . . ? N2 K2 P2 N1 83.8(5) . . . . ? P1 K2 P2 N1 38.9(3) . . . . ? Se1 K2 P2 N1 120.1(4) 2_446 . . . ? O3 K2 P2 Se2 123.8(6) . . . . ? N3 K2 P2 Se2 -138.6(5) . . . . ? N4 K2 P2 Se2 64.3(7) . . . . ? N2 K2 P2 Se2 -86.7(6) . . . . ? P1 K2 P2 Se2 -131.6(5) . . . . ? Se1 K2 P2 Se2 -50.4(6) 2_446 . . . ? O3 K2 P2 P1 -104.6(4) . . . . ? N3 K2 P2 P1 -7.0(2) . . . . ? N4 K2 P2 P1 -164.1(5) . . . . ? N2 K2 P2 P1 44.9(4) . . . . ? Se1 K2 P2 P1 81.2(2) 2_446 . . . ? O3 K2 P2 K1 -88.2(4) . . . . ? N3 K2 P2 K1 9.4(3) . . . . ? N4 K2 P2 K1 -147.7(5) . . . . ? N2 K2 P2 K1 61.3(4) . . . . ? P1 K2 P2 K1 16.41(14) . . . . ? Se1 K2 P2 K1 97.6(2) 2_446 . . . ? O1 K1 P2 N4 149.6(10) . . . . ? O2 K1 P2 N4 -62.1(11) . . . . ? N1 K1 P2 N4 -70.7(11) . . . . ? Se2 K1 P2 N4 92.9(10) . . . . ? Se1 K1 P2 N4 -128.9(10) . . . . ? Se2 K1 P2 N4 30.1(10) 3_476 . . . ? C17 K1 P2 N4 170.8(11) . . . . ? K1 K1 P2 N4 52.0(10) 3_476 . . . ? O1 K1 P2 N2 -59.0(4) . . . . ? O2 K1 P2 N2 89.3(4) . . . . ? N1 K1 P2 N2 80.7(5) . . . . ? Se2 K1 P2 N2 -115.8(4) . . . . ? Se1 K1 P2 N2 22.4(3) . . . . ? Se2 K1 P2 N2 -178.6(3) 3_476 . . . ? C17 K1 P2 N2 -37.8(5) . . . . ? K1 K1 P2 N2 -156.6(4) 3_476 . . . ? O1 K1 P2 N1 -139.7(4) . . . . ? O2 K1 P2 N1 8.6(4) . . . . ? Se2 K1 P2 N1 163.6(4) . . . . ? Se1 K1 P2 N1 -58.2(3) . . . . ? Se2 K1 P2 N1 100.8(4) 3_476 . . . ? C17 K1 P2 N1 -118.5(5) . . . . ? K1 K1 P2 N1 122.7(4) 3_476 . . . ? O1 K1 P2 Se2 56.7(3) . . . . ? O2 K1 P2 Se2 -155.0(3) . . . . ? N1 K1 P2 Se2 -163.6(4) . . . . ? Se1 K1 P2 Se2 138.19(12) . . . . ? Se2 K1 P2 Se2 -62.81(13) 3_476 . . . ? C17 K1 P2 Se2 77.9(4) . . . . ? K1 K1 P2 Se2 -40.84(9) 3_476 . . . ? O1 K1 P2 P1 -96.0(3) . . . . ? O2 K1 P2 P1 52.3(3) . . . . ? N1 K1 P2 P1 43.8(3) . . . . ? Se2 K1 P2 P1 -152.67(16) . . . . ? Se1 K1 P2 P1 -14.48(10) . . . . ? Se2 K1 P2 P1 144.52(13) 3_476 . . . ? C17 K1 P2 P1 -74.7(4) . . . . ? K1 K1 P2 P1 166.49(13) 3_476 . . . ? O1 K1 P2 K2 -112.0(3) . . . . ? O2 K1 P2 K2 36.3(3) . . . . ? N1 K1 P2 K2 27.7(4) . . . . ? Se2 K1 P2 K2 -168.7(2) . . . . ? Se1 K1 P2 K2 -30.54(16) . . . . ? Se2 K1 P2 K2 128.46(15) 3_476 . . . ? C17 K1 P2 K2 -90.8(4) . . . . ? K1 K1 P2 K2 150.43(17) 3_476 . . . ? O2 K1 O1 C20 -169.2(12) . . . . ? N1 K1 O1 C20 -36.7(13) . . . . ? Se2 K1 O1 C20 14.7(12) . . . . ? Se1 K1 O1 C20 -82.5(12) . . . . ? Se2 K1 O1 C20 108.5(12) 3_476 . . . ? C17 K1 O1 C20 -141.4(18) . . . . ? P2 K1 O1 C20 -13.4(12) . . . . ? K1 K1 O1 C20 61.9(12) 3_476 . . . ? O2 K1 O1 C17 -27.8(11) . . . . ? N1 K1 O1 C17 104.6(11) . . . . ? Se2 K1 O1 C17 156.1(10) . . . . ? Se1 K1 O1 C17 58.8(10) . . . . ? Se2 K1 O1 C17 -110.2(10) 3_476 . . . ? P2 K1 O1 C17 127.9(10) . . . . ? K1 K1 O1 C17 -156.7(10) 3_476 . . . ? O1 K1 O2 C21 -122.2(15) . . . . ? N1 K1 O2 C21 91.3(15) . . . . ? Se2 K1 O2 C21 47.3(18) . . . . ? Se1 K1 O2 C21 147.9(16) . . . . ? Se2 K1 O2 C21 -19.2(15) 3_476 . . . ? C17 K1 O2 C21 -132.0(16) . . . . ? P2 K1 O2 C21 87.4(15) . . . . ? K1 K1 O2 C21 -3.1(16) 3_476 . . . ? O1 K1 O2 C24 62.6(13) . . . . ? N1 K1 O2 C24 -83.9(13) . . . . ? Se2 K1 O2 C24 -127.9(12) . . . . ? Se1 K1 O2 C24 -27.4(13) . . . . ? Se2 K1 O2 C24 165.6(13) 3_476 . . . ? C17 K1 O2 C24 52.8(13) . . . . ? P2 K1 O2 C24 -87.8(13) . . . . ? K1 K1 O2 C24 -178.3(12) 3_476 . . . ? N3 K2 O3 C28 99.0(14) . . . . ? N4 K2 O3 C28 -164.1(14) . . . . ? N2 K2 O3 C28 148.3(13) . . . . ? P1 K2 O3 C28 121.9(14) . . . . ? P2 K2 O3 C28 173.2(13) . . . . ? Se1 K2 O3 C28 -10.0(15) 2_446 . . . ? N3 K2 O3 C25 -83(2) . . . . ? N4 K2 O3 C25 14(2) . . . . ? N2 K2 O3 C25 -34(2) . . . . ? P1 K2 O3 C25 -60(2) . . . . ? P2 K2 O3 C25 -9(2) . . . . ? Se1 K2 O3 C25 167.7(19) 2_446 . . . ? N4 P2 N1 C1 44.1(11) . . . . ? N2 P2 N1 C1 153.6(11) . . . . ? Se2 P2 N1 C1 -95.3(10) . . . . ? P1 P2 N1 C1 148.5(13) . . . . ? K2 P2 N1 C1 87.9(10) . . . . ? K1 P2 N1 C1 -110.3(11) . . . . ? N4 P2 N1 P1 -104.4(5) . . . . ? N2 P2 N1 P1 5.1(5) . . . . ? Se2 P2 N1 P1 116.2(4) . . . . ? K2 P2 N1 P1 -60.6(4) . . . . ? K1 P2 N1 P1 101.2(5) . . . . ? N4 P2 N1 K1 154.4(4) . . . . ? N2 P2 N1 K1 -96.1(4) . . . . ? Se2 P2 N1 K1 15.0(3) . . . . ? P1 P2 N1 K1 -101.2(5) . . . . ? K2 P2 N1 K1 -161.8(2) . . . . ? N3 P1 N1 C1 -46.6(12) . . . . ? N2 P1 N1 C1 -155.2(11) . . . . ? Se1 P1 N1 C1 92.4(10) . . . . ? P2 P1 N1 C1 -150.1(13) . . . . ? K2 P1 N1 C1 -89.1(10) . . . . ? N3 P1 N1 P2 103.5(6) . . . . ? N2 P1 N1 P2 -5.1(5) . . . . ? Se1 P1 N1 P2 -117.5(4) . . . . ? K2 P1 N1 P2 61.1(4) . . . . ? N3 P1 N1 K1 -156.4(5) . . . . ? N2 P1 N1 K1 95.0(4) . . . . ? Se1 P1 N1 K1 -17.4(4) . . . . ? P2 P1 N1 K1 100.1(5) . . . . ? K2 P1 N1 K1 161.2(3) . . . . ? O1 K1 N1 C1 -173.6(6) . . . . ? O2 K1 N1 C1 -40.8(7) . . . . ? Se2 K1 N1 C1 121.9(6) . . . . ? Se1 K1 N1 C1 -116.9(7) . . . . ? Se2 K1 N1 C1 42.9(7) 3_476 . . . ? C17 K1 N1 C1 -143.4(7) . . . . ? P2 K1 N1 C1 132.5(8) . . . . ? K1 K1 N1 C1 79.8(6) 3_476 . . . ? O1 K1 N1 P2 53.9(5) . . . . ? O2 K1 N1 P2 -173.3(3) . . . . ? Se2 K1 N1 P2 -10.6(2) . . . . ? Se1 K1 N1 P2 110.6(4) . . . . ? Se2 K1 N1 P2 -89.6(3) 3_476 . . . ? C17 K1 N1 P2 84.1(6) . . . . ? K1 K1 N1 P2 -52.7(3) 3_476 . . . ? O1 K1 N1 P1 -44.5(6) . . . . ? O2 K1 N1 P1 88.2(4) . . . . ? Se2 K1 N1 P1 -109.0(4) . . . . ? Se1 K1 N1 P1 12.2(3) . . . . ? Se2 K1 N1 P1 172.0(3) 3_476 . . . ? C17 K1 N1 P1 -14.3(7) . . . . ? P2 K1 N1 P1 -98.4(5) . . . . ? K1 K1 N1 P1 -151.1(4) 3_476 . . . ? N4 P2 N2 C5 -84.4(12) . . . . ? N1 P2 N2 C5 162.6(11) . . . . ? Se2 P2 N2 C5 52.2(11) . . . . ? P1 P2 N2 C5 167.7(13) . . . . ? K2 P2 N2 C5 -108.1(11) . . . . ? K1 P2 N2 C5 107.9(11) . . . . ? N4 P2 N2 P1 107.8(6) . . . . ? N1 P2 N2 P1 -5.2(5) . . . . ? Se2 P2 N2 P1 -115.5(4) . . . . ? K2 P2 N2 P1 84.2(4) . . . . ? K1 P2 N2 P1 -59.8(4) . . . . ? N4 P2 N2 K2 23.6(5) . . . . ? N1 P2 N2 K2 -89.4(4) . . . . ? Se2 P2 N2 K2 160.26(18) . . . . ? P1 P2 N2 K2 -84.2(4) . . . . ? K1 P2 N2 K2 -144.02(17) . . . . ? N3 P1 N2 C5 84.0(11) . . . . ? N1 P1 N2 C5 -162.8(11) . . . . ? Se1 P1 N2 C5 -53.3(11) . . . . ? P2 P1 N2 C5 -168.0(13) . . . . ? K2 P1 N2 C5 107.1(10) . . . . ? N3 P1 N2 P2 -108.0(5) . . . . ? N1 P1 N2 P2 5.1(5) . . . . ? Se1 P1 N2 P2 114.7(4) . . . . ? K2 P1 N2 P2 -84.9(4) . . . . ? N3 P1 N2 K2 -23.2(5) . . . . ? N1 P1 N2 K2 90.0(4) . . . . ? Se1 P1 N2 K2 -160.42(16) . . . . ? P2 P1 N2 K2 84.9(4) . . . . ? O3 K2 N2 C5 179.6(8) . . . . ? N3 K2 N2 C5 -115.0(7) . . . . ? N4 K2 N2 C5 116.4(7) . . . . ? P1 K2 N2 C5 -130.0(8) . . . . ? P2 K2 N2 C5 131.6(8) . . . . ? Se1 K2 N2 C5 -26.0(7) 2_446 . . . ? O3 K2 N2 P2 48.0(7) . . . . ? N3 K2 N2 P2 113.5(4) . . . . ? N4 K2 N2 P2 -15.2(3) . . . . ? P1 K2 N2 P2 98.4(4) . . . . ? Se1 K2 N2 P2 -157.5(3) 2_446 . . . ? O3 K2 N2 P1 -50.4(7) . . . . ? N3 K2 N2 P1 15.1(3) . . . . ? N4 K2 N2 P1 -113.6(4) . . . . ? P2 K2 N2 P1 -98.4(4) . . . . ? Se1 K2 N2 P1 104.1(3) 2_446 . . . ? N2 P1 N3 C9 -142.0(12) . . . . ? N1 P1 N3 C9 127.7(12) . . . . ? Se1 P1 N3 C9 -7.6(14) . . . . ? P2 P1 N3 C9 173.8(11) . . . . ? K2 P1 N3 C9 -170.1(14) . . . . ? N2 P1 N3 K2 28.1(6) . . . . ? N1 P1 N3 K2 -62.2(6) . . . . ? Se1 P1 N3 K2 162.6(2) . . . . ? P2 P1 N3 K2 -16.1(5) . . . . ? O3 K2 N3 C9 -58.9(9) . . . . ? N4 K2 N3 C9 -167.1(9) . . . . ? N2 K2 N3 C9 154.7(10) . . . . ? P1 K2 N3 C9 172.0(12) . . . . ? P2 K2 N3 C9 -176.7(9) . . . . ? Se1 K2 N3 C9 38.8(9) 2_446 . . . ? O3 K2 N3 P1 129.1(5) . . . . ? N4 K2 N3 P1 20.9(5) . . . . ? N2 K2 N3 P1 -17.3(4) . . . . ? P2 K2 N3 P1 11.3(4) . . . . ? Se1 K2 N3 P1 -133.2(4) 2_446 . . . ? N2 P2 N4 C13 138.4(12) . . . . ? N1 P2 N4 C13 -130.2(12) . . . . ? Se2 P2 N4 C13 5.6(14) . . . . ? P1 P2 N4 C13 -176.8(11) . . . . ? K2 P2 N4 C13 166.6(15) . . . . ? K1 P2 N4 C13 -72.3(17) . . . . ? N2 P2 N4 K2 -28.1(6) . . . . ? N1 P2 N4 K2 63.2(5) . . . . ? Se2 P2 N4 K2 -161.0(2) . . . . ? P1 P2 N4 K2 16.6(5) . . . . ? K1 P2 N4 K2 121.1(8) . . . . ? O3 K2 N4 C13 61.6(11) . . . . ? N3 K2 N4 C13 170.6(10) . . . . ? N2 K2 N4 C13 -151.1(11) . . . . ? P1 K2 N4 C13 -180.0(11) . . . . ? P2 K2 N4 C13 -168.3(13) . . . . ? Se1 K2 N4 C13 -62.0(12) 2_446 . . . ? O3 K2 N4 P2 -130.1(5) . . . . ? N3 K2 N4 P2 -21.1(5) . . . . ? N2 K2 N4 P2 17.2(4) . . . . ? P1 K2 N4 P2 -11.7(4) . . . . ? Se1 K2 N4 P2 106.2(5) 2_446 . . . ? P2 N1 C1 C2 168.7(9) . . . . ? P1 N1 C1 C2 -50.9(14) . . . . ? K1 N1 C1 C2 58.9(10) . . . . ? P2 N1 C1 C3 -67.3(13) . . . . ? P1 N1 C1 C3 73.0(13) . . . . ? K1 N1 C1 C3 -177.2(9) . . . . ? P2 N1 C1 C4 50.4(15) . . . . ? P1 N1 C1 C4 -169.3(9) . . . . ? K1 N1 C1 C4 -59.4(10) . . . . ? P2 N2 C5 C7 158.2(9) . . . . ? P1 N2 C5 C7 -37.7(15) . . . . ? K2 N2 C5 C7 59.4(11) . . . . ? P2 N2 C5 C8 38.4(15) . . . . ? P1 N2 C5 C8 -157.5(9) . . . . ? K2 N2 C5 C8 -60.4(10) . . . . ? P2 N2 C5 C6 -80.9(13) . . . . ? P1 N2 C5 C6 83.2(12) . . . . ? K2 N2 C5 C6 -179.6(8) . . . . ? P1 N3 C9 C12 -179.1(12) . . . . ? K2 N3 C9 C12 11.8(15) . . . . ? P1 N3 C9 C10 -58.2(18) . . . . ? K2 N3 C9 C10 132.7(11) . . . . ? P1 N3 C9 C11 64.3(18) . . . . ? K2 N3 C9 C11 -104.7(13) . . . . ? P2 N4 C13 C15 -69.4(16) . . . . ? K2 N4 C13 C15 95.1(14) . . . . ? P2 N4 C13 C16 56(2) . . . . ? K2 N4 C13 C16 -139.3(12) . . . . ? P2 N4 C13 C14 174.0(11) . . . . ? K2 N4 C13 C14 -21.4(15) . . . . ? C20 O1 C17 C18 0(3) . . . . ? K1 O1 C17 C18 -147.3(18) . . . . ? C20 O1 C17 K1 147.6(16) . . . . ? O1 K1 C17 C18 51(2) . . . . ? O2 K1 C17 C18 -156(2) . . . . ? N1 K1 C17 C18 -46(3) . . . . ? Se2 K1 C17 C18 25(2) . . . . ? Se1 K1 C17 C18 -69(2) . . . . ? Se2 K1 C17 C18 128(2) 3_476 . . . ? P2 K1 C17 C18 -12(3) . . . . ? K1 K1 C17 C18 78(2) 3_476 . . . ? O2 K1 C17 O1 153.4(11) . . . . ? N1 K1 C17 O1 -96.8(11) . . . . ? Se2 K1 C17 O1 -26.3(11) . . . . ? Se1 K1 C17 O1 -119.7(10) . . . . ? Se2 K1 C17 O1 76.8(10) 3_476 . . . ? P2 K1 C17 O1 -63.3(11) . . . . ? K1 K1 C17 O1 27.5(12) 3_476 . . . ? O1 C17 C18 C19 7(4) . . . . ? K1 C17 C18 C19 -26(4) . . . . ? C17 C18 C19 C20 -12(4) . . . . ? C18 C19 C20 O1 12(4) . . . . ? C17 O1 C20 C19 -7(3) . . . . ? K1 O1 C20 C19 136(2) . . . . ? C24 O2 C21 C22 28(2) . . . . ? K1 O2 C21 C22 -147.4(12) . . . . ? O2 C21 C22 C23 -15(2) . . . . ? C21 C22 C23 C24 -4(2) . . . . ? C21 O2 C24 C23 -31(2) . . . . ? K1 O2 C24 C23 145.3(13) . . . . ? C22 C23 C24 O2 21(2) . . . . ? C28 O3 C25 C26 33(2) . . . . ? K2 O3 C25 C26 -145.2(15) . . . . ? O3 C25 C26 C27 -26(2) . . . . ? C25 C26 C27 C28 11(2) . . . . ? C25 O3 C28 C27 -25(2) . . . . ? K2 O3 C28 C27 153.6(12) . . . . ? C26 C27 C28 O3 8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.625 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.128