# Copyright The Royal Society of Chemistry, 1998 data_1 _publ_contact_author 'Igor O.Fritsky' _publ_contact_author_email 'kokozay@chem.kiev.ua' loop_ _publ_author_name ; I.O.Fritsky, H.Kozlowski, P.J.Sadler, O.P.Yefetova, J.Swiatek-Kozlowska, V.A.Kalibabchuk, T.Glowiak ; _journal_name_full 'J.Chem.Soc., Dalton Trans.' _audit_creation_method SHELXL _chemical_name_systematic ; (Lithium, potassium) {8,17-dioxa-1,2,5,6,10,11,14,15-octaazatricyclo [13.3.1]eicosane-3,4,12,13-tetrone - (4-)} cuprate(III) pentahydrate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H22 Cu K0.50 Li0.50 N8 O11' _chemical_formula_weight 516.92 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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' _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 22.808(5) _cell_length_b 13.909(3) _cell_length_c 13.034(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.33(3) _cell_angle_gamma 90.00 _cell_volume 3824.8(15) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 9.8 _cell_measurement_theta_max 16.15 _exptl_crystal_description 'block' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.795 _exptl_crystal_density_method ? _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 1.328 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Enraf-Nonius FAST area detector diffractometer' _diffrn_measurement_method 'profile data from omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3929 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.56 _reflns_number_total 3929 _reflns_number_observed 2689 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Kuma KM4 software 1996' _computing_cell_refinement 'Kuma KM4 software 1996' _computing_data_reduction 'Kuma KM4 software 1996' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material 'ORTEP, 1964' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0461P)^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 'see experimental' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3929 _refine_ls_number_parameters 285 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_obs 0.0327 _refine_ls_wR_factor_all 0.0876 _refine_ls_wR_factor_obs 0.0796 _refine_ls_goodness_of_fit_all 0.974 _refine_ls_goodness_of_fit_obs 1.088 _refine_ls_restrained_S_all 0.974 _refine_ls_restrained_S_obs 1.088 _refine_ls_shift/esd_max 0.390 _refine_ls_shift/esd_mean 0.026 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu Cu 0.373421(15) 0.35699(2) 0.14715(3) 0.02495(9) Uani 1 d . . K K 0.5000 -0.00519(7) 0.2500 0.0515(3) Uani 1 d S . Li Li 0.4781(8) 0.1606(12) -0.0655(15) 0.087(5) Uani 0.50 d P . O1 O 0.25045(9) 0.55900(14) 0.1317(2) 0.0412(5) Uani 1 d . . O2 O 0.21837(9) 0.38536(15) 0.2046(2) 0.0423(5) Uani 1 d . . O3 O 0.49983(11) 0.3111(2) 0.0178(2) 0.0525(6) Uani 1 d . . O4 O 0.46923(11) 0.14318(14) 0.0950(2) 0.0461(5) Uani 1 d . . O5 O 0.34222(9) 0.48988(14) -0.0892(2) 0.0369(5) Uani 1 d . . O6 O 0.28293(10) 0.15645(14) 0.0588(2) 0.0396(5) Uani 1 d . . O7 O 0.15797(13) 0.6791(3) -0.0192(2) 0.0912(11) Uani 1 d . . O8 O 0.09236(11) 0.4494(2) 0.1359(2) 0.0607(7) Uani 1 d . . O9 O 0.17521(11) 0.2391(2) 0.3030(2) 0.0553(6) Uani 1 d . . O10 O 0.45680(15) 0.2289(3) -0.2034(3) 0.1161(14) Uani 1 d . . O11 O 0.05041(11) 0.5877(2) -0.0362(2) 0.0606(7) Uani 1 d . . N1 N 0.33976(10) 0.48140(15) 0.1344(2) 0.0284(5) Uani 1 d . . N2 N 0.31242(10) 0.32678(15) 0.2053(2) 0.0273(5) Uani 1 d . . N3 N 0.43784(10) 0.3894(2) 0.0965(2) 0.0330(5) Uani 1 d . . N4 N 0.40982(10) 0.2334(2) 0.1672(2) 0.0306(5) Uani 1 d . . N5 N 0.35894(10) 0.55981(15) 0.0868(2) 0.0301(5) Uani 1 d . . N6 N 0.44445(11) 0.4791(2) 0.0544(2) 0.0349(5) Uani 1 d . . N7 N 0.30015(10) 0.2339(2) 0.2325(2) 0.0304(5) Uani 1 d . . N8 N 0.38594(11) 0.15236(15) 0.2014(2) 0.0317(5) Uani 1 d . . C1 C 0.28533(12) 0.4878(2) 0.1484(2) 0.0279(5) Uani 1 d . . C2 C 0.26838(12) 0.3929(2) 0.1893(2) 0.0289(6) Uani 1 d . . C3 C 0.46527(14) 0.3130(2) 0.0704(2) 0.0339(6) Uani 1 d . . C4 C 0.44815(13) 0.2195(2) 0.1131(2) 0.0323(6) Uani 1 d . . C5 C 0.42665(13) 0.5562(2) 0.1144(2) 0.0369(7) Uani 1 d . . H5A H 0.44810(13) 0.5459(2) 0.1936(2) 0.044 Uiso 1 calc R . H5B H 0.44069(13) 0.6174(2) 0.0964(2) 0.044 Uiso 1 calc R . C6 C 0.32553(14) 0.5664(2) -0.0327(2) 0.0378(7) Uani 1 d . . H6A H 0.28022(14) 0.5647(2) -0.0504(2) 0.045 Uiso 1 calc R . H6B H 0.33551(14) 0.6273(2) -0.0585(2) 0.045 Uiso 1 calc R . C7 C 0.40826(13) 0.4891(2) -0.0637(2) 0.0368(6) Uani 1 d . . H7A H 0.42030(13) 0.5484(2) -0.0896(2) 0.044 Uiso 1 calc R . H7B H 0.41847(13) 0.4362(2) -0.1025(2) 0.044 Uiso 1 calc R . C8 C 0.35861(13) 0.1797(2) 0.2829(2) 0.0322(6) Uani 1 d . . H8A H 0.35025(13) 0.1222(2) 0.3170(2) 0.039 Uiso 1 calc R . H8B H 0.38910(13) 0.2183(2) 0.3407(2) 0.039 Uiso 1 calc R . C9 C 0.25617(14) 0.1812(2) 0.1384(2) 0.0372(6) Uani 1 d . . H9A H 0.24333(14) 0.1228(2) 0.1649(2) 0.045 Uiso 1 calc R . H9B H 0.21856(14) 0.2200(2) 0.1026(2) 0.045 Uiso 1 calc R . C10 C 0.33862(14) 0.1010(2) 0.1100(2) 0.0386(7) Uani 1 d . . H10A H 0.35633(14) 0.0847(2) 0.0553(2) 0.046 Uiso 1 calc R . H10B H 0.32780(14) 0.0415(2) 0.1374(2) 0.046 Uiso 1 calc R . H1 H 0.1591 0.7040 -0.0776 0.050 Uiso 1 d . . H2 H 0.1972 0.6412 0.0221 0.050 Uiso 1 d . . H3 H 0.1385 0.4377 0.1574 0.050 Uiso 1 d . . H4 H 0.0795 0.3997 0.1771 0.050 Uiso 1 d . . H5 H 0.2009 0.1820 0.3200 0.050 Uiso 1 d . . H6 H 0.1888 0.2689 0.2580 0.050 Uiso 1 d . . H7 H 0.4682 0.2965 -0.1974 0.050 Uiso 1 d . . H8 H 0.4150 0.2414 -0.2432 0.050 Uiso 1 d . . H9 H 0.0894 0.6124 -0.0210 0.050 Uiso 1 d . . H10 H 0.0595 0.5422 0.0171 0.050 Uiso 1 d . . 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 Cu 0.0277(2) 0.02185(15) 0.0269(2) 0.00269(13) 0.01223(12) 0.00087(13) K 0.0736(7) 0.0347(5) 0.0421(5) 0.000 0.0174(5) 0.000 Li 0.086(11) 0.097(12) 0.110(13) -0.037(10) 0.074(10) -0.028(9) O1 0.0390(11) 0.0379(12) 0.0526(13) 0.0104(10) 0.0241(10) 0.0149(9) O2 0.0311(10) 0.0470(12) 0.0561(13) 0.0133(10) 0.0246(10) 0.0044(9) O3 0.0634(14) 0.0437(13) 0.070(2) 0.0065(12) 0.0477(13) 0.0068(11) O4 0.0622(14) 0.0336(11) 0.0532(13) 0.0022(10) 0.0338(11) 0.0115(11) O5 0.0412(11) 0.0362(11) 0.0352(11) -0.0007(8) 0.0165(9) -0.0063(9) O6 0.0461(12) 0.0388(12) 0.0309(10) -0.0012(9) 0.0110(9) -0.0046(9) O7 0.056(2) 0.142(3) 0.077(2) 0.057(2) 0.0251(15) 0.020(2) O8 0.0551(15) 0.0545(15) 0.070(2) 0.0025(13) 0.0208(13) 0.0070(12) O9 0.0629(15) 0.0430(13) 0.075(2) 0.0171(12) 0.0427(13) 0.0073(11) O10 0.074(2) 0.169(4) 0.078(2) 0.028(2) -0.001(2) -0.033(2) O11 0.0576(15) 0.056(2) 0.0508(14) -0.0052(12) 0.0011(12) -0.0035(12) N1 0.0338(13) 0.0209(10) 0.0324(12) 0.0014(9) 0.0146(10) 0.0023(9) N2 0.0308(12) 0.0237(10) 0.0281(11) 0.0022(9) 0.0120(9) -0.0021(9) N3 0.0317(12) 0.0283(11) 0.0427(14) 0.0069(10) 0.0184(11) 0.0012(10) N4 0.0335(12) 0.0248(11) 0.0349(12) 0.0065(9) 0.0147(10) 0.0040(9) N5 0.0373(13) 0.0205(11) 0.0355(12) 0.0020(9) 0.0171(10) -0.0013(9) N6 0.0348(13) 0.0285(12) 0.0465(14) 0.0054(10) 0.0211(11) -0.0019(10) N7 0.0342(12) 0.0298(12) 0.0275(12) 0.0056(9) 0.0120(10) -0.0029(10) N8 0.0385(12) 0.0234(11) 0.0329(12) 0.0064(9) 0.0131(10) 0.0013(10) C1 0.0316(14) 0.0275(13) 0.0242(13) 0.0011(10) 0.0102(11) 0.0021(11) C2 0.0276(14) 0.0345(13) 0.0241(13) 0.0024(11) 0.0092(11) 0.0003(11) C3 0.0368(15) 0.0326(15) 0.0362(15) 0.0048(12) 0.0183(13) 0.0066(12) C4 0.0338(15) 0.0315(14) 0.0305(14) 0.0024(11) 0.0108(12) 0.0078(12) C5 0.039(2) 0.0271(14) 0.046(2) -0.0037(12) 0.0174(13) -0.0088(12) C6 0.041(2) 0.036(2) 0.038(2) 0.0074(13) 0.0166(13) 0.0025(13) C7 0.043(2) 0.0342(15) 0.039(2) 0.0076(12) 0.0218(13) -0.0015(13) C8 0.039(2) 0.0294(13) 0.0259(13) 0.0064(11) 0.0099(12) 0.0009(12) C9 0.039(2) 0.0358(15) 0.036(2) 0.0009(13) 0.0136(13) -0.0054(13) C10 0.047(2) 0.0292(14) 0.036(2) -0.0023(13) 0.0119(14) 0.0002(13) _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 Cu N2 1.868(2) . ? Cu N1 1.875(2) . ? Cu N3 1.880(2) . ? Cu N4 1.884(2) . ? K O4 2.785(2) 2_655 ? K O4 2.785(2) . ? K O11 2.824(3) 7 ? K O11 2.824(3) 8_556 ? K O8 3.071(3) 3_545 ? K O8 3.071(3) 4_545 ? K N8 3.274(2) 2_655 ? K N8 3.274(2) . ? K O10 3.387(5) 6_556 ? K O10 3.387(5) 5_655 ? K Li 3.408(14) 5_655 ? K Li 3.408(14) 6_556 ? Li O11 1.85(2) 3_545 ? Li O10 1.92(2) . ? Li O8 2.16(2) 7 ? Li O4 2.19(2) . ? Li O3 2.32(2) . ? Li C4 2.787(14) . ? Li K 3.408(14) 5_655 ? O1 C1 1.237(3) . ? O2 C2 1.234(3) . ? O3 C3 1.226(3) . ? O4 C4 1.224(3) . ? O5 C7 1.414(3) . ? O5 C6 1.426(3) . ? O6 C10 1.418(3) . ? O6 C9 1.432(3) . ? O7 H1 0.846(3) . ? O7 H2 1.001(3) . ? O8 Li 2.16(2) 7 ? O8 K 3.071(3) 3_455 ? O8 H3 0.994(2) . ? O8 H4 0.986(3) . ? O9 H5 0.961(2) . ? O9 H6 0.867(2) . ? O10 K 3.387(5) 5_655 ? O10 H7 0.971(4) . ? O10 H8 0.912(3) . ? O11 Li 1.85(2) 3_455 ? O11 K 2.824(3) 7 ? O11 H9 0.903(2) . ? O11 H10 0.903(3) . ? N1 C1 1.325(3) . ? N1 N5 1.404(3) . ? N2 C2 1.318(3) . ? N2 N7 1.396(3) . ? N3 C3 1.341(4) . ? N3 N6 1.394(3) . ? N4 C4 1.329(3) . ? N4 N8 1.397(3) . ? N5 C5 1.447(4) . ? N5 C6 1.455(4) . ? N6 C7 1.450(4) . ? N6 C5 1.472(4) . ? N7 C8 1.453(3) . ? N7 C9 1.453(4) . ? N8 C10 1.456(4) . ? N8 C8 1.471(3) . ? C1 C2 1.527(4) . ? C3 C4 1.523(4) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C10 H10A 0.97 . ? C10 H10B 0.97 . ? 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 N2 Cu N1 84.30(9) . . ? N2 Cu N3 176.83(10) . . ? N1 Cu N3 95.48(10) . . ? N2 Cu N4 95.49(9) . . ? N1 Cu N4 177.21(10) . . ? N3 Cu N4 84.57(10) . . ? O4 K O4 84.36(9) 2_655 . ? O4 K O11 155.95(8) 2_655 7 ? O4 K O11 71.89(7) . 7 ? O4 K O11 71.89(7) 2_655 8_556 ? O4 K O11 155.95(8) . 8_556 ? O11 K O11 132.04(11) 7 8_556 ? O4 K O8 118.28(7) 2_655 3_545 ? O4 K O8 80.29(6) . 3_545 ? O11 K O8 62.30(7) 7 3_545 ? O11 K O8 107.31(7) 8_556 3_545 ? O4 K O8 80.29(6) 2_655 4_545 ? O4 K O8 118.28(7) . 4_545 ? O11 K O8 107.31(7) 7 4_545 ? O11 K O8 62.30(7) 8_556 4_545 ? O8 K O8 156.25(10) 3_545 4_545 ? O4 K N8 53.20(6) 2_655 2_655 ? O4 K N8 66.86(7) . 2_655 ? O11 K N8 117.30(7) 7 2_655 ? O11 K N8 94.90(7) 8_556 2_655 ? O8 K N8 65.83(6) 3_545 2_655 ? O8 K N8 133.23(6) 4_545 2_655 ? O4 K N8 66.86(7) 2_655 . ? O4 K N8 53.20(6) . . ? O11 K N8 94.90(7) 7 . ? O11 K N8 117.30(7) 8_556 . ? O8 K N8 133.23(6) 3_545 . ? O8 K N8 65.83(6) 4_545 . ? N8 K N8 95.97(8) 2_655 . ? O4 K O10 124.12(7) 2_655 6_556 ? O4 K O10 143.16(7) . 6_556 ? O11 K O10 76.50(8) 7 6_556 ? O11 K O10 59.13(8) 8_556 6_556 ? O8 K O10 101.39(8) 3_545 6_556 ? O8 K O10 54.86(8) 4_545 6_556 ? N8 K O10 147.56(7) 2_655 6_556 ? N8 K O10 112.68(7) . 6_556 ? O4 K O10 143.16(7) 2_655 5_655 ? O4 K O10 124.12(7) . 5_655 ? O11 K O10 59.13(8) 7 5_655 ? O11 K O10 76.50(8) 8_556 5_655 ? O8 K O10 54.86(8) 3_545 5_655 ? O8 K O10 101.39(8) 4_545 5_655 ? N8 K O10 112.68(7) 2_655 5_655 ? N8 K O10 147.56(7) . 5_655 ? O10 K O10 46.58(12) 6_556 5_655 ? O4 K Li 156.6(2) 2_655 5_655 ? O4 K Li 91.3(3) . 5_655 ? O11 K Li 32.8(3) 7 5_655 ? O11 K Li 109.0(3) 8_556 5_655 ? O8 K Li 38.4(2) 3_545 5_655 ? O8 K Li 121.5(2) 4_545 5_655 ? N8 K Li 104.0(2) 2_655 5_655 ? N8 K Li 127.3(3) . 5_655 ? O10 K Li 71.0(3) 6_556 5_655 ? O10 K Li 32.9(3) 5_655 5_655 ? O4 K Li 91.3(3) 2_655 6_556 ? O4 K Li 156.6(2) . 6_556 ? O11 K Li 109.0(3) 7 6_556 ? O11 K Li 32.8(3) 8_556 6_556 ? O8 K Li 121.5(2) 3_545 6_556 ? O8 K Li 38.4(2) 4_545 6_556 ? N8 K Li 127.3(3) 2_655 6_556 ? N8 K Li 104.0(2) . 6_556 ? O10 K Li 32.9(3) 6_556 6_556 ? O10 K Li 71.0(3) 5_655 6_556 ? Li K Li 101.3(6) 5_655 6_556 ? O11 Li O10 110.7(7) 3_545 . ? O11 Li O8 99.3(7) 3_545 7 ? O10 Li O8 94.0(7) . 7 ? O11 Li O4 98.1(9) 3_545 . ? O10 Li O4 149.8(9) . . ? O8 Li O4 90.2(6) 7 . ? O11 Li O3 112.5(8) 3_545 . ? O10 Li O3 85.7(7) . . ? O8 Li O3 146.1(7) 7 . ? O4 Li O3 74.5(5) . . ? O11 Li C4 118.1(9) 3_545 . ? O10 Li C4 125.5(8) . . ? O8 Li C4 100.6(5) 7 . ? O4 Li C4 25.0(2) . . ? O3 Li C4 54.6(3) . . ? O11 Li K 55.9(4) 3_545 5_655 ? O10 Li K 73.0(5) . 5_655 ? O8 Li K 62.3(4) 7 5_655 ? O4 Li K 134.0(7) . 5_655 ? O3 Li K 147.1(6) . 5_655 ? C4 Li K 157.5(6) . 5_655 ? C3 O3 Li 102.3(4) . . ? C4 O4 Li 105.9(5) . . ? C4 O4 K 120.8(2) . . ? Li O4 K 133.3(5) . . ? C7 O5 C6 110.7(2) . . ? C10 O6 C9 110.0(2) . . ? H1 O7 H2 111.9(3) . . ? Li O8 K 79.3(4) 7 3_455 ? Li O8 H3 122.9(5) 7 . ? K O8 H3 138.1(2) 3_455 . ? Li O8 H4 53.6(5) 7 . ? K O8 H4 58.62(12) 3_455 . ? H3 O8 H4 103.5(2) . . ? H5 O9 H6 102.0(2) . . ? Li O10 K 74.1(5) . 5_655 ? Li O10 H7 115.9(5) . . ? K O10 H7 144.8(3) 5_655 . ? Li O10 H8 117.6(5) . . ? K O10 H8 112.7(3) 5_655 . ? H7 O10 H8 92.9(4) . . ? Li O11 K 91.3(5) 3_455 7 ? Li O11 H9 124.3(5) 3_455 . ? K O11 H9 111.6(2) 7 . ? Li O11 H10 118.0(6) 3_455 . ? K O11 H10 111.2(2) 7 . ? H9 O11 H10 100.3(2) . . ? C1 N1 N5 118.3(2) . . ? C1 N1 Cu 115.0(2) . . ? N5 N1 Cu 124.8(2) . . ? C2 N2 N7 118.2(2) . . ? C2 N2 Cu 114.8(2) . . ? N7 N2 Cu 124.3(2) . . ? C3 N3 N6 118.6(2) . . ? C3 N3 Cu 113.6(2) . . ? N6 N3 Cu 124.7(2) . . ? C4 N4 N8 117.8(2) . . ? C4 N4 Cu 113.8(2) . . ? N8 N4 Cu 125.2(2) . . ? N1 N5 C5 110.2(2) . . ? N1 N5 C6 113.4(2) . . ? C5 N5 C6 110.1(2) . . ? N3 N6 C7 113.6(2) . . ? N3 N6 C5 110.4(2) . . ? C7 N6 C5 109.5(2) . . ? N2 N7 C8 110.9(2) . . ? N2 N7 C9 113.2(2) . . ? C8 N7 C9 109.9(2) . . ? N4 N8 C10 113.1(2) . . ? N4 N8 C8 110.2(2) . . ? C10 N8 C8 109.4(2) . . ? N4 N8 K 102.95(14) . . ? C10 N8 K 96.7(2) . . ? C8 N8 K 123.86(15) . . ? O1 C1 N1 127.1(2) . . ? O1 C1 C2 121.5(2) . . ? N1 C1 C2 111.4(2) . . ? O2 C2 N2 127.6(3) . . ? O2 C2 C1 120.1(2) . . ? N2 C2 C1 112.3(2) . . ? O3 C3 N3 128.3(3) . . ? O3 C3 C4 119.6(2) . . ? N3 C3 C4 112.0(2) . . ? O4 C4 N4 127.9(3) . . ? O4 C4 C3 119.7(2) . . ? N4 C4 C3 112.4(2) . . ? O4 C4 Li 49.1(4) . . ? N4 C4 Li 154.9(4) . . ? C3 C4 Li 76.6(4) . . ? N5 C5 N6 112.2(2) . . ? N5 C5 H5A 109.2(2) . . ? N6 C5 H5A 109.2(2) . . ? N5 C5 H5B 109.17(14) . . ? N6 C5 H5B 109.18(14) . . ? H5A C5 H5B 107.9 . . ? O5 C6 N5 111.9(2) . . ? O5 C6 H6A 109.24(14) . . ? N5 C6 H6A 109.24(15) . . ? O5 C6 H6B 109.24(14) . . ? N5 C6 H6B 109.23(15) . . ? H6A C6 H6B 107.9 . . ? O5 C7 N6 112.1(2) . . ? O5 C7 H7A 109.19(14) . . ? N6 C7 H7A 109.18(14) . . ? O5 C7 H7B 109.18(15) . . ? N6 C7 H7B 109.2(2) . . ? H7A C7 H7B 107.9 . . ? N7 C8 N8 112.1(2) . . ? N7 C8 H8A 109.19(14) . . ? N8 C8 H8A 109.19(13) . . ? N7 C8 H8B 109.20(14) . . ? N8 C8 H8B 109.20(14) . . ? H8A C8 H8B 107.9 . . ? O6 C9 N7 112.6(2) . . ? O6 C9 H9A 109.06(15) . . ? N7 C9 H9A 109.07(14) . . ? O6 C9 H9B 109.06(15) . . ? N7 C9 H9B 109.1(2) . . ? H9A C9 H9B 107.8 . . ? O6 C10 N8 111.8(2) . . ? O6 C10 H10A 109.26(15) . . ? N8 C10 H10A 109.3(2) . . ? O6 C10 H10B 109.25(15) . . ? N8 C10 H10B 109.26(15) . . ? H10A C10 H10B 107.9 . . ? 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 O11 Li O3 C3 -125.7(7) 3_545 . . . ? O10 Li O3 C3 123.6(4) . . . . ? O8 Li O3 C3 32.7(17) 7 . . . ? O4 Li O3 C3 -33.3(5) . . . . ? C4 Li O3 C3 -16.4(3) . . . . ? K Li O3 C3 172.7(13) 5_655 . . . ? O11 Li O4 C4 145.2(5) 3_545 . . . ? O10 Li O4 C4 -17.1(17) . . . . ? O8 Li O4 C4 -115.4(5) 7 . . . ? O3 Li O4 C4 34.0(5) . . . . ? C4 Li O4 C4 0.000(2) . . . . ? K Li O4 C4 -165.3(7) 5_655 . . . ? O11 Li O4 K -31.8(9) 3_545 . . . ? O10 Li O4 K 165.8(12) . . . . ? O8 Li O4 K 67.6(8) 7 . . . ? O3 Li O4 K -143.0(3) . . . . ? C4 Li O4 K -177.0(6) . . . . ? K Li O4 K 17.7(12) 5_655 . . . ? O4 K O4 C4 -32.3(2) 2_655 . . . ? O11 K O4 C4 143.8(2) 7 . . . ? O11 K O4 C4 -41.4(3) 8_556 . . . ? O8 K O4 C4 -152.3(2) 3_545 . . . ? O8 K O4 C4 43.5(2) 4_545 . . . ? N8 K O4 C4 -84.5(2) 2_655 . . . ? N8 K O4 C4 32.9(2) . . . . ? O10 K O4 C4 111.6(2) 6_556 . . . ? O10 K O4 C4 172.9(2) 5_655 . . . ? Li K O4 C4 170.7(3) 5_655 . . . ? Li K O4 C4 47.8(9) 6_556 . . . ? O4 K O4 Li 144.4(6) 2_655 . . . ? O11 K O4 Li -39.5(6) 7 . . . ? O11 K O4 Li 135.3(6) 8_556 . . . ? O8 K O4 Li 24.4(6) 3_545 . . . ? O8 K O4 Li -139.9(6) 4_545 . . . ? N8 K O4 Li 92.1(6) 2_655 . . . ? N8 K O4 Li -150.4(6) . . . . ? O10 K O4 Li -71.7(6) 6_556 . . . ? O10 K O4 Li -10.4(6) 5_655 . . . ? Li K O4 Li -12.6(8) 5_655 . . . ? Li K O4 Li -135.5(12) 6_556 . . . ? O11 Li O10 K 42.1(6) 3_545 . . 5_655 ? O8 Li O10 K -59.4(4) 7 . . 5_655 ? O4 Li O10 K -156.7(17) . . . 5_655 ? O3 Li O10 K 154.6(5) . . . 5_655 ? C4 Li O10 K -165.4(8) . . . 5_655 ? K Li O10 K 0.0 5_655 . . 5_655 ? N2 Cu N1 C1 -12.4(2) . . . . ? N3 Cu N1 C1 170.8(2) . . . . ? N4 Cu N1 C1 -98.1(19) . . . . ? N2 Cu N1 N5 -176.6(2) . . . . ? N3 Cu N1 N5 6.6(2) . . . . ? N4 Cu N1 N5 97.7(19) . . . . ? N1 Cu N2 C2 13.7(2) . . . . ? N3 Cu N2 C2 100.0(17) . . . . ? N4 Cu N2 C2 -169.1(2) . . . . ? N1 Cu N2 N7 174.3(2) . . . . ? N3 Cu N2 N7 -99.5(17) . . . . ? N4 Cu N2 N7 -8.5(2) . . . . ? N2 Cu N3 C3 107.9(16) . . . . ? N1 Cu N3 C3 -166.2(2) . . . . ? N4 Cu N3 C3 16.6(2) . . . . ? N2 Cu N3 N6 -92.4(17) . . . . ? N1 Cu N3 N6 -6.4(2) . . . . ? N4 Cu N3 N6 176.4(2) . . . . ? N2 Cu N4 C4 166.4(2) . . . . ? N1 Cu N4 C4 -108.1(19) . . . . ? N3 Cu N4 C4 -16.7(2) . . . . ? N2 Cu N4 N8 7.3(2) . . . . ? N1 Cu N4 N8 92.7(19) . . . . ? N3 Cu N4 N8 -175.9(2) . . . . ? C1 N1 N5 C5 159.1(2) . . . . ? Cu N1 N5 C5 -37.2(3) . . . . ? C1 N1 N5 C6 -77.0(3) . . . . ? Cu N1 N5 C6 86.7(2) . . . . ? C3 N3 N6 C7 71.7(3) . . . . ? Cu N3 N6 C7 -87.1(3) . . . . ? C3 N3 N6 C5 -164.9(2) . . . . ? Cu N3 N6 C5 36.3(3) . . . . ? C2 N2 N7 C8 -160.8(2) . . . . ? Cu N2 N7 C8 39.3(3) . . . . ? C2 N2 N7 C9 75.1(3) . . . . ? Cu N2 N7 C9 -84.8(3) . . . . ? C4 N4 N8 C10 -71.6(3) . . . . ? Cu N4 N8 C10 86.8(3) . . . . ? C4 N4 N8 C8 165.5(2) . . . . ? Cu N4 N8 C8 -36.0(3) . . . . ? C4 N4 N8 K 31.6(2) . . . . ? Cu N4 N8 K -169.96(13) . . . . ? O4 K N8 N4 70.48(15) 2_655 . . . ? O4 K N8 N4 -30.25(14) . . . . ? O11 K N8 N4 -93.3(2) 7 . . . ? O11 K N8 N4 123.55(15) 8_556 . . . ? O8 K N8 N4 -37.3(2) 3_545 . . . ? O8 K N8 N4 159.9(2) 4_545 . . . ? N8 K N8 N4 24.88(12) 2_655 . . . ? O10 K N8 N4 -170.66(14) 6_556 . . . ? O10 K N8 N4 -127.7(2) 5_655 . . . ? Li K N8 N4 -87.9(4) 5_655 . . . ? Li K N8 N4 155.8(4) 6_556 . . . ? O4 K N8 C10 -173.9(2) 2_655 . . . ? O4 K N8 C10 85.4(2) . . . . ? O11 K N8 C10 22.4(2) 7 . . . ? O11 K N8 C10 -120.8(2) 8_556 . . . ? O8 K N8 C10 78.3(2) 3_545 . . . ? O8 K N8 C10 -84.4(2) 4_545 . . . ? N8 K N8 C10 140.5(2) 2_655 . . . ? O10 K N8 C10 -55.0(2) 6_556 . . . ? O10 K N8 C10 -12.0(2) 5_655 . . . ? Li K N8 C10 27.8(4) 5_655 . . . ? Li K N8 C10 -88.6(4) 6_556 . . . ? O4 K N8 C8 -55.0(2) 2_655 . . . ? O4 K N8 C8 -155.8(2) . . . . ? O11 K N8 C8 141.2(2) 7 . . . ? O11 K N8 C8 -2.0(2) 8_556 . . . ? O8 K N8 C8 -162.8(2) 3_545 . . . ? O8 K N8 C8 34.4(2) 4_545 . . . ? N8 K N8 C8 -100.6(2) 2_655 . . . ? O10 K N8 C8 63.8(2) 6_556 . . . ? O10 K N8 C8 106.8(2) 5_655 . . . ? Li K N8 C8 146.6(4) 5_655 . . . ? Li K N8 C8 30.3(4) 6_556 . . . ? N5 N1 C1 O1 -5.8(4) . . . . ? Cu N1 C1 O1 -171.1(2) . . . . ? N5 N1 C1 C2 174.0(2) . . . . ? Cu N1 C1 C2 8.7(3) . . . . ? N7 N2 C2 O2 6.8(4) . . . . ? Cu N2 C2 O2 168.6(2) . . . . ? N7 N2 C2 C1 -173.9(2) . . . . ? Cu N2 C2 C1 -12.1(3) . . . . ? O1 C1 C2 O2 1.3(4) . . . . ? N1 C1 C2 O2 -178.4(2) . . . . ? O1 C1 C2 N2 -178.0(2) . . . . ? N1 C1 C2 N2 2.2(3) . . . . ? Li O3 C3 N3 -150.0(6) . . . . ? Li O3 C3 C4 29.0(6) . . . . ? N6 N3 C3 O3 4.8(5) . . . . ? Cu N3 C3 O3 165.8(3) . . . . ? N6 N3 C3 C4 -174.3(2) . . . . ? Cu N3 C3 C4 -13.2(3) . . . . ? Li O4 C4 N4 147.5(5) . . . . ? K O4 C4 N4 -35.0(4) . . . . ? Li O4 C4 C3 -31.9(5) . . . . ? K O4 C4 C3 145.6(2) . . . . ? Li O4 C4 Li 0.0 . . . . ? K O4 C4 Li 177.5(5) . . . . ? N8 N4 C4 O4 -5.3(4) . . . . ? Cu N4 C4 O4 -166.2(2) . . . . ? N8 N4 C4 C3 174.1(2) . . . . ? Cu N4 C4 C3 13.3(3) . . . . ? N8 N4 C4 Li 67.5(11) . . . . ? Cu N4 C4 Li -93.3(11) . . . . ? O3 C3 C4 O4 0.3(4) . . . . ? N3 C3 C4 O4 179.4(3) . . . . ? O3 C3 C4 N4 -179.2(3) . . . . ? N3 C3 C4 N4 -0.1(3) . . . . ? O3 C3 C4 Li -24.0(5) . . . . ? N3 C3 C4 Li 155.2(5) . . . . ? O11 Li C4 O4 -39.8(6) 3_545 . . . ? O10 Li C4 O4 169.5(11) . . . . ? O8 Li C4 O4 66.8(6) 7 . . . ? O4 Li C4 O4 0.000(2) . . . . ? O3 Li C4 O4 -138.6(6) . . . . ? K Li C4 O4 28.4(15) 5_655 . . . ? O11 Li C4 N4 -133.6(8) 3_545 . . . ? O10 Li C4 N4 75.7(13) . . . . ? O8 Li C4 N4 -27.0(15) 7 . . . ? O4 Li C4 N4 -93.8(11) . . . . ? O3 Li C4 N4 127.6(8) . . . . ? K Li C4 N4 -65.4(24) 5_655 . . . ? O11 Li C4 C3 112.0(7) 3_545 . . . ? O10 Li C4 C3 -38.7(7) . . . . ? O8 Li C4 C3 -141.4(7) 7 . . . ? O4 Li C4 C3 151.8(5) . . . . ? O3 Li C4 C3 13.2(3) . . . . ? K Li C4 C3 -179.7(18) 5_655 . . . ? N1 N5 C5 N6 72.1(3) . . . . ? C6 N5 C5 N6 -53.7(3) . . . . ? N3 N6 C5 N5 -72.0(3) . . . . ? C7 N6 C5 N5 53.8(3) . . . . ? C7 O5 C6 N5 -57.8(3) . . . . ? N1 N5 C6 O5 -68.6(3) . . . . ? C5 N5 C6 O5 55.4(3) . . . . ? C6 O5 C7 N6 58.4(3) . . . . ? N3 N6 C7 O5 68.2(3) . . . . ? C5 N6 C7 O5 -55.8(3) . . . . ? N2 N7 C8 N8 -72.7(3) . . . . ? C9 N7 C8 N8 53.2(3) . . . . ? N4 N8 C8 N7 70.5(3) . . . . ? C10 N8 C8 N7 -54.4(3) . . . . ? K N8 C8 N7 -167.17(15) . . . . ? C10 O6 C9 N7 57.8(3) . . . . ? N2 N7 C9 O6 69.7(3) . . . . ? C8 N7 C9 O6 -54.9(3) . . . . ? C9 O6 C10 N8 -58.9(3) . . . . ? N4 N8 C10 O6 -66.1(3) . . . . ? C8 N8 C10 O6 57.2(3) . . . . ? K N8 C10 O6 -173.3(2) . . . . ? _refine_diff_density_max 0.516 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.070 #-END data_2 _publ_contact_author 'Igor O.Fritsky' _publ_contact_author_email 'kokozay@chem.kiev.ua' loop_ _publ_author_name ; I.O.Fritsky, H.Kozlowski, P.J.Sadler, O.P.Yefetova, J.Swiatek-Kozlowska, V.A.Kalibabchuk, T.Glowiak ; _journal_name_full 'J.Chem.Soc., Dalton Trans.' _audit_creation_method SHELXL _chemical_name_systematic ; Potassium {3,5-bis-(2'-hydroxyiminopropanoyl)-1,3,5-oxadiazinane (3-)}nickolate(II) sesquihydrate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C9 H16 K N6 Ni O6.50' _chemical_formula_weight 410.09 _chemical_melting_point ? _chemical_compound_source ? 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' '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0890(10) _cell_length_b 10.376(4) _cell_length_c 10.6400(10) _cell_angle_alpha 99.51(4) _cell_angle_beta 111.95(2) _cell_angle_gamma 106.86(2) _cell_volume 754.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 23.4 _cell_measurement_theta_max 38.8 _exptl_crystal_description BLOCK _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.806 _exptl_crystal_density_method ? _exptl_crystal_F_000 422 _exptl_absorpt_coefficient_mu 1.608 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Enraf-Nonius FAST area detector diffractometer' _diffrn_measurement_method 'profile data from omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3049 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.0668 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 24.82 _reflns_number_total 1559 _reflns_number_observed 1209 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material 'ORTEP, 1964' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0531P)^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 'see experimental' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1556 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_obs 0.0425 _refine_ls_wR_factor_all 0.1066 _refine_ls_wR_factor_obs 0.0977 _refine_ls_goodness_of_fit_all 1.013 _refine_ls_goodness_of_fit_obs 1.150 _refine_ls_restrained_S_all 1.079 _refine_ls_restrained_S_obs 1.150 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni -0.27197(10) -0.03729(6) 0.07539(8) 0.0272(3) Uani 1 d . . K1 K 0.3104(2) -0.19816(12) 0.3389(2) 0.0392(4) Uani 1 d . . O1 O -0.1744(6) 0.1204(4) -0.0975(5) 0.0403(11) Uani 1 d . . O2 O -0.3619(6) -0.3697(4) -0.2189(5) 0.0488(12) Uani 1 d . . O3 O -0.1464(6) 0.2592(4) 0.1232(5) 0.0413(11) Uani 1 d . . O4 O -0.3450(6) 0.0442(4) 0.4208(5) 0.0375(10) Uani 1 d . . O5 O -0.0966(5) -0.2443(4) 0.2649(5) 0.0371(11) Uani 1 d . . O1W1 O 0.1168(19) -0.4770(12) 0.1487(13) 0.056(3) Uani 0.50 d P . O1W2 O 0.1700(21) -0.4669(12) 0.2579(18) 0.083(5) Uani 0.50 d P . O1W3 O 0.4400(18) -0.4185(11) 0.4639(11) 0.085(4) Uani 0.50 d P . N1 N -0.2319(6) -0.0089(5) -0.0808(5) 0.0308(12) Uani 1 d . . N2 N -0.3309(6) -0.2238(4) -0.0141(5) 0.0297(12) Uani 1 d . . N3 N -0.2139(6) 0.1515(4) 0.1693(5) 0.0289(12) Uani 1 d . . N4 N -0.3200(6) -0.0672(4) 0.2273(5) 0.0281(12) Uani 1 d . . N5 N -0.3811(6) -0.3387(4) 0.0389(5) 0.0292(12) Uani 1 d . . N6 N -0.3784(6) -0.2025(4) 0.2527(5) 0.0292(12) Uani 1 d . . C1 C -0.2286(9) -0.1181(6) -0.3035(7) 0.046(2) Uani 1 d . . H1A H -0.3413(23) -0.1185(40) -0.3785(15) 0.068 Uiso 1 calc R . H1B H -0.2051(54) -0.2007(21) -0.3334(24) 0.068 Uiso 1 calc R . H1C H -0.1193(34) -0.0348(21) -0.2819(13) 0.068 Uiso 1 calc R . C2 C -0.2596(8) -0.1186(6) -0.1747(7) 0.0335(15) Uani 1 d . . C3 C -0.3234(8) -0.2526(6) -0.1373(7) 0.0319(15) Uani 1 d . . C4 C -0.3058(7) 0.0421(5) 0.3182(7) 0.0276(14) Uani 1 d . . C5 C -0.2347(7) 0.1759(5) 0.2829(7) 0.0301(14) Uani 1 d . . C6 C -0.1872(10) 0.3171(5) 0.3718(8) 0.049(2) Uani 1 d . . H6A H -0.0641(27) 0.3473(18) 0.4530(23) 0.074 Uiso 1 calc R . H6B H -0.2845(31) 0.3146(11) 0.4034(35) 0.074 Uiso 1 calc R . H6C H -0.1817(57) 0.3821(10) 0.3176(15) 0.074 Uiso 1 calc R . C7 C -0.4918(7) -0.3162(5) 0.1151(6) 0.0304(15) Uani 1 d . . H7A H -0.5485(7) -0.4037(5) 0.1319(6) 0.036 Uiso 1 calc R . H7B H -0.5967(7) -0.2937(5) 0.0551(6) 0.036 Uiso 1 calc R . C8 C -0.2133(9) -0.3561(6) 0.1310(8) 0.037(2) Uani 1 d . . H8A H -0.1345(9) -0.3616(6) 0.0820(8) 0.044 Uiso 1 calc R . H8B H -0.2534(9) -0.4453(6) 0.1501(8) 0.044 Uiso 1 calc R . C9 C -0.2078(8) -0.2284(6) 0.3367(7) 0.036(2) Uani 1 d . . H9A H -0.1274(8) -0.1500(6) 0.4242(7) 0.044 Uiso 1 calc R . H9B H -0.2491(8) -0.3133(6) 0.3624(7) 0.044 Uiso 1 calc R . H1 H -0.1459(81) 0.1960(60) 0.0121(74) 0.050(18) Uiso 1 d . . H1W1 H 0.0209 -0.5415 0.1600 0.080 Uiso 0.50 d P . H1W2 H 0.2263 -0.5243 0.2221 0.080 Uiso 0.50 d P . H2W2 H 0.0879 -0.5467 0.2801 0.080 Uiso 0.50 d P . 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 Ni1 0.0315(4) 0.0231(4) 0.0275(5) 0.0075(4) 0.0157(4) 0.0080(3) K1 0.0422(8) 0.0379(7) 0.0336(9) 0.0038(7) 0.0212(7) 0.0088(6) O1 0.046(3) 0.038(2) 0.044(3) 0.024(2) 0.024(2) 0.015(2) O2 0.064(3) 0.048(2) 0.039(3) 0.004(3) 0.028(3) 0.026(2) O3 0.051(3) 0.026(2) 0.047(3) 0.017(2) 0.023(2) 0.009(2) O4 0.054(3) 0.034(2) 0.028(3) 0.002(2) 0.027(2) 0.014(2) O5 0.032(2) 0.035(2) 0.043(3) 0.011(2) 0.017(2) 0.012(2) O1W1 0.056(7) 0.036(5) 0.064(9) -0.015(8) 0.035(8) 0.008(4) O1W2 0.078(10) 0.032(5) 0.142(15) -0.016(10) 0.077(12) 0.010(6) O1W3 0.146(11) 0.083(7) 0.048(8) 0.025(7) 0.047(8) 0.069(7) N1 0.030(3) 0.039(3) 0.029(3) 0.014(3) 0.017(3) 0.011(2) N2 0.036(3) 0.027(2) 0.029(3) 0.009(3) 0.018(3) 0.012(2) N3 0.023(3) 0.024(2) 0.033(3) 0.008(3) 0.009(3) 0.006(2) N4 0.039(3) 0.017(2) 0.034(3) 0.007(2) 0.024(3) 0.008(2) N5 0.032(3) 0.023(2) 0.034(3) 0.008(2) 0.016(3) 0.010(2) N6 0.036(3) 0.020(2) 0.037(3) 0.011(3) 0.021(3) 0.009(2) C1 0.058(4) 0.062(4) 0.035(4) 0.021(4) 0.030(4) 0.031(3) C2 0.032(3) 0.046(3) 0.025(4) 0.011(4) 0.013(3) 0.019(3) C3 0.029(3) 0.035(3) 0.028(4) 0.005(3) 0.012(3) 0.011(2) C4 0.024(3) 0.025(3) 0.028(4) 0.003(3) 0.008(3) 0.010(2) C5 0.025(3) 0.030(3) 0.030(4) 0.004(3) 0.012(3) 0.008(2) C6 0.066(5) 0.030(3) 0.048(5) 0.004(4) 0.025(4) 0.018(3) C7 0.030(3) 0.025(3) 0.037(4) 0.010(3) 0.017(3) 0.008(2) C8 0.038(4) 0.030(3) 0.044(5) 0.009(3) 0.019(4) 0.016(3) C9 0.043(4) 0.033(3) 0.027(4) 0.006(3) 0.014(3) 0.012(3) _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 Ni1 N2 1.843(4) . ? Ni1 N4 1.851(4) . ? Ni1 N1 1.861(4) . ? Ni1 N3 1.878(4) . ? Ni1 Ni1 3.798(2) 2_455 ? K1 O1W2 2.538(12) . ? K1 O4 2.650(4) 2_556 ? K1 O1 2.747(4) 2 ? K1 O1W1 2.826(12) . ? K1 O4 2.872(4) 1_655 ? K1 O5 2.951(4) . ? K1 N6 2.993(4) 1_655 ? K1 O1W3 3.074(9) . ? K1 C4 3.480(5) 1_655 ? K1 K1 4.270(4) 2_656 ? K1 K1 14.532(4) 2_455 ? O1 H1 1.19(7) . ? O1 N1 1.352(5) . ? O1 O3 2.436(6) . ? O1 K1 2.747(4) 2 ? O2 C3 1.249(7) . ? O3 H1 1.26(7) . ? O3 N3 1.347(5) . ? O4 C4 1.245(7) . ? O4 K1 2.650(4) 2_556 ? O4 K1 2.872(4) 1_455 ? O5 C9 1.407(7) . ? O5 C8 1.442(8) . ? O1W1 O1W2 1.05(2) . ? N1 C2 1.285(7) . ? N2 C3 1.323(8) . ? N2 N5 1.420(5) . ? N3 C5 1.276(7) . ? N4 C4 1.308(7) . ? N4 N6 1.450(5) . ? N5 C8 1.429(7) . ? N5 C7 1.455(7) . ? N6 C9 1.465(7) . ? N6 C7 1.474(7) . ? N6 K1 2.993(4) 1_455 ? C1 C2 1.483(8) . ? C2 C3 1.509(7) . ? C4 C5 1.506(6) . ? C4 K1 3.480(5) 1_455 ? C5 C6 1.460(8) . ? 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 N2 Ni1 N4 96.7(2) . . ? N2 Ni1 N1 83.0(2) . . ? N4 Ni1 N1 178.2(2) . . ? N2 Ni1 N3 178.8(2) . . ? N4 Ni1 N3 82.1(2) . . ? N1 Ni1 N3 98.2(2) . . ? N2 Ni1 Ni1 108.02(14) . 2_455 ? N4 Ni1 Ni1 89.50(14) . 2_455 ? N1 Ni1 Ni1 88.93(15) . 2_455 ? N3 Ni1 Ni1 71.85(14) . 2_455 ? O1W2 K1 O4 122.8(4) . 2_556 ? O1W2 K1 O1 106.0(4) . 2 ? O4 K1 O1 118.60(14) 2_556 2 ? O1W2 K1 O1W1 21.8(4) . . ? O4 K1 O1W1 140.9(3) 2_556 . ? O1 K1 O1W1 84.5(3) 2 . ? O1W2 K1 O4 143.0(4) . 1_655 ? O4 K1 O4 78.77(13) 2_556 1_655 ? O1 K1 O4 83.75(12) 2 1_655 ? O1W1 K1 O4 138.2(3) . 1_655 ? O1W2 K1 O5 81.5(4) . . ? O4 K1 O5 78.91(13) 2_556 . ? O1 K1 O5 73.57(11) 2 . ? O1W1 K1 O5 78.5(3) . . ? O4 K1 O5 134.97(11) 1_655 . ? O1W2 K1 N6 89.5(3) . 1_655 ? O4 K1 N6 128.37(13) 2_556 1_655 ? O1 K1 N6 82.38(13) 2 1_655 ? O1W1 K1 N6 82.9(3) . 1_655 ? O4 K1 N6 55.82(12) 1_655 1_655 ? O5 K1 N6 150.70(14) . 1_655 ? O1W2 K1 O1W3 47.0(5) . . ? O4 K1 O1W3 95.5(2) 2_556 . ? O1 K1 O1W3 145.8(2) 2 . ? O1W1 K1 O1W3 65.8(3) . . ? O4 K1 O1W3 106.7(2) 1_655 . ? O5 K1 O1W3 114.0(2) . . ? N6 K1 O1W3 77.6(2) 1_655 . ? O1W2 K1 C4 131.0(3) . 1_655 ? O4 K1 C4 98.06(14) 2_556 1_655 ? O1 K1 C4 70.39(12) 2 1_655 ? O1W1 K1 C4 120.2(3) . 1_655 ? O4 K1 C4 19.78(13) 1_655 1_655 ? O5 K1 C4 136.76(12) . 1_655 ? N6 K1 C4 41.71(11) 1_655 1_655 ? O1W3 K1 C4 109.2(2) . 1_655 ? O1W2 K1 K1 150.8(4) . 2_656 ? O4 K1 K1 41.27(8) 2_556 2_656 ? O1 K1 K1 102.94(10) 2 2_656 ? O1W1 K1 K1 169.3(3) . 2_656 ? O4 K1 K1 37.50(9) 1_655 2_656 ? O5 K1 K1 110.85(10) . 2_656 ? N6 K1 K1 90.43(9) 1_655 2_656 ? O1W3 K1 K1 104.6(2) . 2_656 ? C4 K1 K1 56.92(10) 1_655 2_656 ? O1W2 K1 K1 105.1(4) . 2_455 ? O4 K1 K1 84.55(9) 2_556 2_455 ? O1 K1 K1 45.87(9) 2 2_455 ? O1W1 K1 K1 93.0(3) . 2_455 ? O4 K1 K1 106.81(9) 1_655 2_455 ? O5 K1 K1 32.41(7) . 2_455 ? N6 K1 K1 128.18(9) 1_655 2_455 ? O1W3 K1 K1 145.8(2) . 2_455 ? C4 K1 K1 104.53(9) 1_655 2_455 ? K1 K1 K1 97.79(5) 2_656 2_455 ? H1 O1 N1 102.0(24) . . ? H1 O1 O3 5.6(26) . . ? N1 O1 O3 98.2(3) . . ? H1 O1 K1 118.1(26) . 2 ? N1 O1 K1 128.5(3) . 2 ? O3 O1 K1 118.9(2) . 2 ? H1 O3 N3 102.3(23) . . ? H1 O3 O1 5.3(25) . . ? N3 O3 O1 98.3(3) . . ? C4 O4 K1 147.3(3) . 2_556 ? C4 O4 K1 108.9(3) . 1_455 ? K1 O4 K1 101.23(13) 2_556 1_455 ? C9 O5 C8 110.6(4) . . ? C9 O5 K1 137.7(4) . . ? C8 O5 K1 107.1(3) . . ? O1W2 O1W1 K1 63.5(11) . . ? O1W1 O1W2 K1 94.7(13) . . ? C2 N1 O1 119.9(5) . . ? C2 N1 Ni1 117.3(4) . . ? O1 N1 Ni1 122.8(4) . . ? C3 N2 N5 117.4(4) . . ? C3 N2 Ni1 117.1(3) . . ? N5 N2 Ni1 125.5(4) . . ? C5 N3 O3 120.3(4) . . ? C5 N3 Ni1 117.4(3) . . ? O3 N3 Ni1 122.2(4) . . ? C4 N4 N6 116.6(4) . . ? C4 N4 Ni1 117.6(3) . . ? N6 N4 Ni1 125.7(3) . . ? N2 N5 C8 111.3(4) . . ? N2 N5 C7 110.1(4) . . ? C8 N5 C7 109.6(4) . . ? N4 N6 C9 110.1(4) . . ? N4 N6 C7 109.3(4) . . ? C9 N6 C7 108.5(4) . . ? N4 N6 K1 103.1(3) . 1_455 ? C9 N6 K1 124.4(3) . 1_455 ? C7 N6 K1 100.6(3) . 1_455 ? N1 C2 C1 125.7(5) . . ? N1 C2 C3 111.9(5) . . ? C1 C2 C3 122.3(5) . . ? O2 C3 N2 128.9(5) . . ? O2 C3 C2 120.5(6) . . ? N2 C3 C2 110.6(5) . . ? O4 C4 N4 128.2(4) . . ? O4 C4 C5 121.0(5) . . ? N4 C4 C5 110.8(5) . . ? O4 C4 K1 51.4(2) . 1_455 ? N4 C4 K1 85.0(3) . 1_455 ? C5 C4 K1 146.1(3) . 1_455 ? N3 C5 C6 124.2(5) . . ? N3 C5 C4 111.9(5) . . ? C6 C5 C4 123.9(6) . . ? N5 C7 N6 114.3(4) . . ? N5 C8 O5 114.3(4) . . ? O5 C9 N6 113.5(4) . . ? 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 H1 O1 O3 H1 0.000(14) . . . . ? N1 O1 O3 H1 133.7(269) . . . . ? K1 O1 O3 H1 -83.4(269) 2 . . . ? H1 O1 O3 N3 -138.3(269) . . . . ? N1 O1 O3 N3 -4.6(4) . . . . ? K1 O1 O3 N3 138.3(3) 2 . . . ? O1W2 K1 O5 C9 108.4(5) . . . . ? O4 K1 O5 C9 -17.5(4) 2_556 . . . ? O1 K1 O5 C9 -142.0(4) 2 . . . ? O1W1 K1 O5 C9 130.3(5) . . . . ? O4 K1 O5 C9 -79.1(4) 1_655 . . . ? N6 K1 O5 C9 -178.2(4) 1_655 . . . ? O1W3 K1 O5 C9 73.6(5) . . . . ? C4 K1 O5 C9 -107.6(4) 1_655 . . . ? K1 K1 O5 C9 -44.1(4) 2_656 . . . ? K1 K1 O5 C9 -114.9(5) 2_455 . . . ? O1W2 K1 O5 C8 -43.8(5) . . . . ? O4 K1 O5 C8 -169.7(3) 2_556 . . . ? O1 K1 O5 C8 65.8(3) 2 . . . ? O1W1 K1 O5 C8 -21.8(4) . . . . ? O4 K1 O5 C8 128.7(3) 1_655 . . . ? N6 K1 O5 C8 29.7(4) 1_655 . . . ? O1W3 K1 O5 C8 -78.5(4) . . . . ? C4 K1 O5 C8 100.3(3) 1_655 . . . ? K1 K1 O5 C8 163.7(3) 2_656 . . . ? K1 K1 O5 C8 92.9(3) 2_455 . . . ? O1W2 K1 O1W1 O1W2 0.000(2) . . . . ? O4 K1 O1W1 O1W2 -40.1(18) 2_556 . . . ? O1 K1 O1W1 O1W2 -170.2(15) 2 . . . ? O4 K1 O1W1 O1W2 115.4(14) 1_655 . . . ? O5 K1 O1W1 O1W2 -95.9(15) . . . . ? N6 K1 O1W1 O1W2 106.8(15) 1_655 . . . ? O1W3 K1 O1W1 O1W2 27.2(14) . . . . ? C4 K1 O1W1 O1W2 126.2(14) 1_655 . . . ? K1 K1 O1W1 O1W2 55.0(24) 2_656 . . . ? K1 K1 O1W1 O1W2 -125.1(15) 2_455 . . . ? K1 O1W1 O1W2 K1 0.0 . . . . ? O4 K1 O1W2 O1W1 151.1(13) 2_556 . . . ? O1 K1 O1W2 O1W1 10.1(16) 2 . . . ? O1W1 K1 O1W2 O1W1 0.000(3) . . . . ? O4 K1 O1W2 O1W1 -91.0(17) 1_655 . . . ? O5 K1 O1W2 O1W1 80.2(15) . . . . ? N6 K1 O1W2 O1W1 -71.8(15) 1_655 . . . ? O1W3 K1 O1W2 O1W1 -145.2(18) . . . . ? C4 K1 O1W2 O1W1 -67.6(17) 1_655 . . . ? K1 K1 O1W2 O1W1 -161.8(11) 2_656 . . . ? K1 K1 O1W2 O1W1 57.8(15) 2_455 . . . ? H1 O1 N1 C2 -173.8(28) . . . . ? O3 O1 N1 C2 -177.9(4) . . . . ? K1 O1 N1 C2 44.5(6) 2 . . . ? H1 O1 N1 Ni1 5.7(29) . . . . ? O3 O1 N1 Ni1 1.6(4) . . . . ? K1 O1 N1 Ni1 -136.0(3) 2 . . . ? N2 Ni1 N1 C2 0.2(4) . . . . ? N4 Ni1 N1 C2 -80.6(63) . . . . ? N3 Ni1 N1 C2 -179.6(4) . . . . ? Ni1 Ni1 N1 C2 -108.1(4) 2_455 . . . ? N2 Ni1 N1 O1 -179.2(4) . . . . ? N4 Ni1 N1 O1 99.9(62) . . . . ? N3 Ni1 N1 O1 1.0(4) . . . . ? Ni1 Ni1 N1 O1 72.5(4) 2_455 . . . ? N4 Ni1 N2 C3 177.0(4) . . . . ? N1 Ni1 N2 C3 -1.2(4) . . . . ? N3 Ni1 N2 C3 169.3(92) . . . . ? Ni1 Ni1 N2 C3 85.4(4) 2_455 . . . ? N4 Ni1 N2 N5 -3.8(4) . . . . ? N1 Ni1 N2 N5 177.9(4) . . . . ? N3 Ni1 N2 N5 -11.6(97) . . . . ? Ni1 Ni1 N2 N5 -95.5(4) 2_455 . . . ? H1 O3 N3 C5 -179.9(27) . . . . ? O1 O3 N3 C5 -176.3(4) . . . . ? H1 O3 N3 Ni1 2.3(27) . . . . ? O1 O3 N3 Ni1 5.9(4) . . . . ? N2 Ni1 N3 C5 6.1(97) . . . . ? N4 Ni1 N3 C5 -1.7(4) . . . . ? N1 Ni1 N3 C5 176.6(4) . . . . ? Ni1 Ni1 N3 C5 90.4(4) 2_455 . . . ? N2 Ni1 N3 O3 -176.1(93) . . . . ? N4 Ni1 N3 O3 176.1(4) . . . . ? N1 Ni1 N3 O3 -5.6(4) . . . . ? Ni1 Ni1 N3 O3 -91.8(4) 2_455 . . . ? N2 Ni1 N4 C4 -176.1(4) . . . . ? N1 Ni1 N4 C4 -95.5(62) . . . . ? N3 Ni1 N4 C4 3.7(4) . . . . ? Ni1 Ni1 N4 C4 -68.0(4) 2_455 . . . ? N2 Ni1 N4 N6 1.8(4) . . . . ? N1 Ni1 N4 N6 82.4(63) . . . . ? N3 Ni1 N4 N6 -178.4(4) . . . . ? Ni1 Ni1 N4 N6 109.9(4) 2_455 . . . ? C3 N2 N5 C8 92.2(6) . . . . ? Ni1 N2 N5 C8 -86.9(5) . . . . ? C3 N2 N5 C7 -146.0(5) . . . . ? Ni1 N2 N5 C7 34.9(6) . . . . ? C4 N4 N6 C9 -93.3(5) . . . . ? Ni1 N4 N6 C9 88.8(5) . . . . ? C4 N4 N6 C7 147.6(5) . . . . ? Ni1 N4 N6 C7 -30.3(5) . . . . ? C4 N4 N6 K1 41.3(5) . . . 1_455 ? Ni1 N4 N6 K1 -136.6(3) . . . 1_455 ? O1 N1 C2 C1 1.9(8) . . . . ? Ni1 N1 C2 C1 -177.6(5) . . . . ? O1 N1 C2 C3 -179.9(4) . . . . ? Ni1 N1 C2 C3 0.6(6) . . . . ? N5 N2 C3 O2 3.0(9) . . . . ? Ni1 N2 C3 O2 -177.8(5) . . . . ? N5 N2 C3 C2 -177.4(4) . . . . ? Ni1 N2 C3 C2 1.7(6) . . . . ? N1 C2 C3 O2 178.1(5) . . . . ? C1 C2 C3 O2 -3.7(8) . . . . ? N1 C2 C3 N2 -1.5(7) . . . . ? C1 C2 C3 N2 176.7(5) . . . . ? K1 O4 C4 N4 164.6(4) 2_556 . . . ? K1 O4 C4 N4 -39.5(7) 1_455 . . . ? K1 O4 C4 C5 -16.5(10) 2_556 . . . ? K1 O4 C4 C5 139.4(4) 1_455 . . . ? K1 O4 C4 K1 -155.8(8) 2_556 . . 1_455 ? K1 O4 C4 K1 0.0 1_455 . . 1_455 ? N6 N4 C4 O4 -3.8(8) . . . . ? Ni1 N4 C4 O4 174.3(5) . . . . ? N6 N4 C4 C5 177.2(4) . . . . ? Ni1 N4 C4 C5 -4.7(6) . . . . ? N6 N4 C4 K1 -33.7(4) . . . 1_455 ? Ni1 N4 C4 K1 144.4(3) . . . 1_455 ? O3 N3 C5 C6 -0.8(9) . . . . ? Ni1 N3 C5 C6 177.0(4) . . . . ? O3 N3 C5 C4 -178.2(4) . . . . ? Ni1 N3 C5 C4 -0.4(6) . . . . ? O4 C4 C5 N3 -175.9(5) . . . . ? N4 C4 C5 N3 3.2(7) . . . . ? K1 C4 C5 N3 -110.2(7) 1_455 . . . ? O4 C4 C5 C6 6.7(8) . . . . ? N4 C4 C5 C6 -174.2(5) . . . . ? K1 C4 C5 C6 72.4(9) 1_455 . . . ? N2 N5 C7 N6 -70.9(5) . . . . ? C8 N5 C7 N6 51.9(5) . . . . ? N4 N6 C7 N5 68.0(5) . . . . ? C9 N6 C7 N5 -52.0(5) . . . . ? K1 N6 C7 N5 176.0(3) 1_455 . . . ? N2 N5 C8 O5 69.2(5) . . . . ? C7 N5 C8 O5 -52.8(5) . . . . ? C9 O5 C8 N5 55.7(5) . . . . ? K1 O5 C8 N5 -143.9(3) . . . . ? C8 O5 C9 N6 -56.1(5) . . . . ? K1 O5 C9 N6 152.4(3) . . . . ? N4 N6 C9 O5 -65.4(5) . . . . ? C7 N6 C9 O5 54.1(5) . . . . ? K1 N6 C9 O5 171.8(3) 1_455 . . . ? _refine_diff_density_max 0.377 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.105