# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_m091215f _database_code_depnum_ccdc_archive 'CCDC 886739' #TrackingRef 'Dy-02.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H10 Dy2 K2 N2 O20' _chemical_formula_weight 977.48 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' 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.594(2) _cell_length_b 12.467(4) _cell_length_c 14.022(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1152.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 4366 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.9 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.816 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 6.906 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6080 _exptl_absorpt_correction_T_max 0.8742 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14795 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0730 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.91 _reflns_number_total 2765 _reflns_number_gt 2483 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'CrystalStructure 3.8' _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^)+(0.0455P)^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 CONSTR _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0296(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.18(2) _refine_ls_number_reflns 2765 _refine_ls_number_parameters 201 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0952 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.003 _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 Dy1 Dy -0.09946(6) 1.15000(3) 0.27423(3) 0.00704(14) Uani 1 1 d . . . K1 K 0.0958(3) 1.36039(15) 0.02952(14) 0.0183(4) Uani 1 1 d . . . N1 N 0.1088(12) 0.7882(5) 0.1002(5) 0.0070(13) Uani 1 1 d . . . O1 O 0.1367(9) 1.0079(4) 0.2573(4) 0.0111(13) Uani 1 1 d . . . O2 O 0.1235(9) 0.8310(4) 0.2832(4) 0.0100(11) Uani 1 1 d . . . O3 O -0.0747(10) 1.1256(4) 0.1116(4) 0.0109(13) Uani 1 1 d . . . O4 O 0.2303(10) 1.1472(5) 0.0458(5) 0.0180(14) Uani 1 1 d . . . O5 O -0.0628(8) 0.8008(5) -0.2111(4) 0.0107(13) Uani 1 1 d . . . O6 O 0.2704(8) 0.7812(5) -0.2101(4) 0.0095(13) Uani 1 1 d . . . O7 O 0.0862(11) 0.5984(5) -0.0845(4) 0.0147(13) Uani 1 1 d . . . O8 O 0.1097(11) 0.5806(4) 0.0731(4) 0.0093(11) Uani 1 1 d . . . C1 C 0.1060(15) 0.8924(6) 0.1222(6) 0.0085(15) Uani 1 1 d . . . C2 C 0.0984(15) 0.9714(6) 0.0533(6) 0.0102(16) Uani 1 1 d . . . C3 C 0.1068(14) 0.9390(6) -0.0419(5) 0.0086(15) Uani 1 1 d . . . H3 H 0.1140 0.9914 -0.0909 0.010 Uiso 1 1 calc R . . C4 C 0.1046(13) 0.8315(6) -0.0653(5) 0.0075(14) Uani 1 1 d . . . C5 C 0.1057(14) 0.7568(6) 0.0084(6) 0.0087(15) Uani 1 1 d . . . C6 C 0.1208(12) 0.9129(6) 0.2296(6) 0.0084(14) Uani 1 1 d . . . C7 C 0.0885(17) 1.0922(6) 0.0731(6) 0.0107(16) Uani 1 1 d . . . C8 C 0.1033(14) 0.8010(6) -0.1697(6) 0.0067(14) Uani 1 1 d U . . C9 C 0.1011(14) 0.6360(6) -0.0041(6) 0.0092(15) Uani 1 1 d . . . O9 O -0.2921(9) 0.9905(5) 0.2499(4) 0.0167(14) Uani 1 1 d . . . H9A H -0.3320 0.9817 0.1928 0.020 Uiso 1 1 d R . . H9B H -0.3631 0.9534 0.2883 0.020 Uiso 1 1 d R . . O10 O 0.4571(10) 1.3342(5) 0.1324(5) 0.0185(15) Uani 1 1 d . . . H10A H 0.4404 1.2715 0.1547 0.022 Uiso 1 1 d R . . H10B H 0.5790 1.3438 0.1146 0.022 Uiso 1 1 d 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 Dy1 0.0081(2) 0.00716(19) 0.00584(19) -0.00065(15) 0.00023(15) -0.00023(15) K1 0.0152(9) 0.0149(8) 0.0248(10) -0.0024(8) -0.0017(9) -0.0005(10) N1 0.005(3) 0.007(3) 0.008(3) 0.001(2) 0.000(3) 0.002(3) O1 0.011(3) 0.009(2) 0.014(3) -0.009(2) 0.003(2) -0.004(2) O2 0.012(3) 0.012(3) 0.007(2) -0.003(2) -0.001(2) -0.003(2) O3 0.014(3) 0.013(3) 0.006(3) -0.004(2) -0.001(2) 0.003(2) O4 0.020(3) 0.011(3) 0.024(3) 0.002(3) 0.009(3) -0.002(3) O5 0.009(3) 0.011(3) 0.012(3) 0.001(2) 0.001(2) -0.005(2) O6 0.008(3) 0.009(3) 0.011(3) -0.004(2) 0.004(2) -0.003(2) O7 0.024(4) 0.012(3) 0.009(3) -0.002(2) 0.000(3) 0.001(3) O8 0.013(3) 0.011(3) 0.004(2) 0.000(2) 0.000(3) 0.001(3) C1 0.007(4) 0.011(3) 0.007(4) 0.000(3) 0.000(4) -0.004(4) C2 0.007(4) 0.014(4) 0.010(4) 0.002(3) -0.002(4) -0.003(4) C3 0.009(4) 0.010(4) 0.006(3) 0.000(3) 0.001(4) 0.002(4) C4 0.003(3) 0.010(3) 0.010(3) -0.001(3) -0.003(3) 0.000(4) C5 0.006(4) 0.011(3) 0.009(3) -0.003(3) 0.000(4) -0.005(4) C6 0.007(4) 0.009(3) 0.009(3) -0.001(3) -0.001(4) 0.002(3) C7 0.020(5) 0.008(3) 0.005(3) 0.000(3) -0.005(4) 0.003(4) C8 0.0069(16) 0.0063(16) 0.0068(16) 0.0006(10) 0.0002(10) -0.0004(10) C9 0.008(4) 0.007(3) 0.012(4) 0.002(3) 0.004(3) 0.001(4) O9 0.021(3) 0.017(3) 0.012(3) -0.004(2) 0.001(3) -0.009(3) O10 0.020(4) 0.021(3) 0.014(3) 0.007(3) -0.003(3) -0.004(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 Dy1 O3 2.307(6) . ? Dy1 O8 2.310(5) 3 ? Dy1 O5 2.319(6) 2_475 ? Dy1 O6 2.344(6) 2_575 ? Dy1 O1 2.370(6) . ? Dy1 O9 2.384(6) . ? Dy1 O2 2.401(5) 3 ? Dy1 N1 2.464(6) 3 ? Dy1 K1 4.507(2) . ? K1 O4 2.633(7) 4_475 ? K1 O10 2.804(7) . ? K1 O4 2.812(7) . ? K1 O8 2.814(6) 1_565 ? K1 O3 2.944(7) 4_575 ? K1 O2 3.020(6) 3 ? K1 O3 3.339(6) . ? K1 O7 3.372(6) 1_565 ? K1 C7 3.399(8) . ? K1 C9 3.469(8) 1_565 ? K1 K1 4.374(3) 4_575 ? K1 K1 4.374(3) 4_475 ? K1 H10A 3.0780 . ? N1 C1 1.335(9) . ? N1 C5 1.346(10) . ? N1 Dy1 2.464(6) 3_545 ? O1 C6 1.251(9) . ? O2 C6 1.268(10) . ? O2 Dy1 2.401(5) 3_545 ? O2 K1 3.020(6) 3_545 ? O3 C7 1.274(12) . ? O3 K1 2.944(7) 4_475 ? O4 C7 1.221(11) . ? O4 K1 2.633(7) 4_575 ? O5 C8 1.239(10) . ? O5 Dy1 2.319(6) 2_474 ? O6 C8 1.263(10) . ? O6 Dy1 2.344(6) 2_574 ? O7 C9 1.225(10) . ? O7 K1 3.372(6) 1_545 ? O8 C9 1.286(9) . ? O8 Dy1 2.310(5) 3_545 ? O8 K1 2.814(6) 1_545 ? C1 C2 1.381(11) . ? C1 C6 1.530(11) . ? C2 C3 1.395(10) . ? C2 C7 1.533(11) . ? C3 C4 1.380(10) . ? C3 H3 0.9500 . ? C4 C5 1.390(11) . ? C4 C8 1.513(10) . ? C5 C9 1.517(10) . ? C9 K1 3.469(8) 1_545 ? O9 H9A 0.8500 . ? O9 H9B 0.8500 . ? O10 H10A 0.8501 . ? O10 H10B 0.8498 . ? 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 O3 Dy1 O8 150.3(2) . 3 ? O3 Dy1 O5 101.0(2) . 2_475 ? O8 Dy1 O5 89.3(2) 3 2_475 ? O3 Dy1 O6 94.3(2) . 2_575 ? O8 Dy1 O6 94.4(2) 3 2_575 ? O5 Dy1 O6 141.62(19) 2_475 2_575 ? O3 Dy1 O1 75.9(2) . . ? O8 Dy1 O1 80.3(2) 3 . ? O5 Dy1 O1 146.8(2) 2_475 . ? O6 Dy1 O1 71.04(19) 2_575 . ? O3 Dy1 O9 77.7(2) . . ? O8 Dy1 O9 78.7(2) 3 . ? O5 Dy1 O9 73.8(2) 2_475 . ? O6 Dy1 O9 144.3(2) 2_575 . ? O1 Dy1 O9 73.3(2) . . ? O3 Dy1 O2 78.3(2) . 3 ? O8 Dy1 O2 131.37(19) 3 3 ? O5 Dy1 O2 73.6(2) 2_475 3 ? O6 Dy1 O2 75.43(19) 2_575 3 ? O1 Dy1 O2 135.4(2) . 3 ? O9 Dy1 O2 134.5(2) . 3 ? O3 Dy1 N1 143.2(2) . 3 ? O8 Dy1 N1 66.4(2) 3 3 ? O5 Dy1 N1 74.2(2) 2_475 3 ? O6 Dy1 N1 72.5(2) 2_575 3 ? O1 Dy1 N1 127.6(2) . 3 ? O9 Dy1 N1 132.2(2) . 3 ? O2 Dy1 N1 65.2(2) 3 3 ? O3 Dy1 K1 45.86(14) . . ? O8 Dy1 K1 158.74(16) 3 . ? O5 Dy1 K1 100.85(15) 2_475 . ? O6 Dy1 K1 66.04(14) 2_575 . ? O1 Dy1 K1 99.86(15) . . ? O9 Dy1 K1 121.92(15) . . ? O2 Dy1 K1 38.43(14) 3 . ? N1 Dy1 K1 98.28(16) 3 . ? O4 K1 O10 168.5(2) 4_475 . ? O4 K1 O4 106.71(17) 4_475 . ? O10 K1 O4 65.2(2) . . ? O4 K1 O8 98.7(2) 4_475 1_565 ? O10 K1 O8 88.5(2) . 1_565 ? O4 K1 O8 153.4(2) . 1_565 ? O4 K1 O3 114.1(2) 4_475 4_575 ? O10 K1 O3 74.05(19) . 4_575 ? O4 K1 O3 82.97(18) . 4_575 ? O8 K1 O3 93.68(19) 1_565 4_575 ? O4 K1 O2 84.6(2) 4_475 3 ? O10 K1 O2 86.88(19) . 3 ? O4 K1 O2 88.05(17) . 3 ? O8 K1 O2 86.85(16) 1_565 3 ? O3 K1 O2 160.90(18) 4_575 3 ? O4 K1 O3 78.39(19) 4_475 . ? O10 K1 O3 90.40(18) . . ? O4 K1 O3 41.38(18) . . ? O8 K1 O3 142.29(17) 1_565 . ? O3 K1 O3 122.13(13) 4_575 . ? O2 K1 O3 55.46(15) 3 . ? O4 K1 O7 79.9(2) 4_475 1_565 ? O10 K1 O7 111.23(18) . 1_565 ? O4 K1 O7 151.24(19) . 1_565 ? O8 K1 O7 40.96(14) 1_565 1_565 ? O3 K1 O7 69.09(16) 4_575 1_565 ? O2 K1 O7 120.66(15) 3 1_565 ? O3 K1 O7 158.19(18) . 1_565 ? O4 K1 C7 91.4(2) 4_475 . ? O10 K1 C7 78.8(2) . . ? O4 K1 C7 19.9(2) . . ? O8 K1 C7 157.09(18) 1_565 . ? O3 K1 C7 100.9(2) 4_575 . ? O2 K1 C7 73.61(19) 3 . ? O3 K1 C7 21.8(2) . . ? O7 K1 C7 161.94(18) 1_565 . ? O4 K1 C9 89.4(2) 4_475 1_565 ? O10 K1 C9 100.2(2) . 1_565 ? O4 K1 C9 160.8(2) . 1_565 ? O8 K1 C9 20.40(18) 1_565 1_565 ? O3 K1 C9 80.94(18) 4_575 1_565 ? O2 K1 C9 104.07(17) 3 1_565 ? O3 K1 C9 156.70(19) . 1_565 ? O7 K1 C9 20.56(17) 1_565 1_565 ? C7 K1 C9 177.5(2) . 1_565 ? O4 K1 K1 126.26(17) 4_475 4_575 ? O10 K1 K1 51.95(14) . 4_575 ? O4 K1 K1 35.17(14) . 4_575 ? O8 K1 K1 129.09(16) 1_565 4_575 ? O3 K1 K1 49.73(12) 4_575 4_575 ? O2 K1 K1 116.69(13) 3 4_575 ? O3 K1 K1 76.55(13) . 4_575 ? O7 K1 K1 118.58(14) 1_565 4_575 ? C7 K1 K1 54.95(19) . 4_575 ? C9 K1 K1 126.16(16) 1_565 4_575 ? O4 K1 K1 37.96(15) 4_475 4_475 ? O10 K1 K1 131.66(15) . 4_475 ? O4 K1 K1 70.02(16) . 4_475 ? O8 K1 K1 132.81(16) 1_565 4_475 ? O3 K1 K1 117.81(14) 4_575 4_475 ? O2 K1 K1 74.18(12) 3 4_475 ? O3 K1 K1 42.27(12) . 4_475 ? O7 K1 K1 116.74(13) 1_565 4_475 ? C7 K1 K1 53.44(18) . 4_475 ? C9 K1 K1 127.25(16) 1_565 4_475 ? K1 K1 K1 97.84(8) 4_575 4_475 ? O4 K1 H10A 153.1 4_475 . ? O10 K1 H10A 15.7 . . ? O4 K1 H10A 51.7 . . ? O8 K1 H10A 101.7 1_565 . ? O3 K1 H10A 81.9 4_575 . ? O2 K1 H10A 79.3 3 . ? O3 K1 H10A 74.7 . . ? O7 K1 H10A 127.0 1_565 . ? C7 K1 H10A 63.5 . . ? C9 K1 H10A 115.3 1_565 . ? K1 K1 H10A 47.5 4_575 . ? K1 K1 H10A 116.0 4_475 . ? C1 N1 C5 120.2(7) . . ? C1 N1 Dy1 121.0(5) . 3_545 ? C5 N1 Dy1 118.7(5) . 3_545 ? C6 O1 Dy1 133.1(5) . . ? C6 O2 Dy1 123.8(5) . 3_545 ? C6 O2 K1 114.3(5) . 3_545 ? Dy1 O2 K1 111.9(2) 3_545 3_545 ? C7 O3 Dy1 121.5(5) . . ? C7 O3 K1 111.0(5) . 4_475 ? Dy1 O3 K1 127.2(3) . 4_475 ? C7 O3 K1 81.8(5) . . ? Dy1 O3 K1 104.42(19) . . ? K1 O3 K1 88.00(15) 4_475 . ? C7 O4 K1 143.8(6) . 4_575 ? C7 O4 K1 108.3(6) . . ? K1 O4 K1 106.9(2) 4_575 . ? C8 O5 Dy1 152.9(6) . 2_474 ? C8 O6 Dy1 141.1(5) . 2_574 ? C9 O7 K1 84.2(5) . 1_545 ? C9 O8 Dy1 125.3(5) . 3_545 ? C9 O8 K1 109.9(5) . 1_545 ? Dy1 O8 K1 124.5(2) 3_545 1_545 ? N1 C1 C2 122.2(7) . . ? N1 C1 C6 112.9(7) . . ? C2 C1 C6 124.9(7) . . ? C1 C2 C3 117.5(7) . . ? C1 C2 C7 125.2(7) . . ? C3 C2 C7 117.3(7) . . ? C4 C3 C2 120.5(7) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 118.2(7) . . ? C3 C4 C8 118.3(7) . . ? C5 C4 C8 123.4(6) . . ? N1 C5 C4 121.1(7) . . ? N1 C5 C9 113.6(7) . . ? C4 C5 C9 125.3(7) . . ? O1 C6 O2 125.2(8) . . ? O1 C6 C1 118.0(7) . . ? O2 C6 C1 116.7(7) . . ? O4 C7 O3 126.6(8) . . ? O4 C7 C2 117.5(9) . . ? O3 C7 C2 115.7(9) . . ? O4 C7 K1 51.7(4) . . ? O3 C7 K1 76.5(5) . . ? C2 C7 K1 159.0(5) . . ? O5 C8 O6 124.1(7) . . ? O5 C8 C4 117.3(8) . . ? O6 C8 C4 118.5(8) . . ? O7 C9 O8 124.9(7) . . ? O7 C9 C5 119.2(7) . . ? O8 C9 C5 115.8(7) . . ? O7 C9 K1 75.2(5) . 1_545 ? O8 C9 K1 49.7(4) . 1_545 ? C5 C9 K1 165.5(5) . 1_545 ? Dy1 O9 H9A 114.1 . . ? Dy1 O9 H9B 131.0 . . ? H9A O9 H9B 110.8 . . ? K1 O10 H10A 100.7 . . ? K1 O10 H10B 129.6 . . ? H10A O10 H10B 111.1 . . ? 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 O3 Dy1 O1 C6 -68.5(7) . . . . ? O8 Dy1 O1 C6 93.7(8) 3 . . . ? O5 Dy1 O1 C6 20.1(9) 2_475 . . . ? O6 Dy1 O1 C6 -168.2(8) 2_575 . . . ? O9 Dy1 O1 C6 12.7(7) . . . . ? O2 Dy1 O1 C6 -124.9(7) 3 . . . ? N1 Dy1 O1 C6 143.5(7) 3 . . . ? K1 Dy1 O1 C6 -107.9(7) . . . . ? O8 Dy1 O3 C7 -67.9(8) 3 . . . ? O5 Dy1 O3 C7 -176.4(6) 2_475 . . . ? O6 Dy1 O3 C7 38.9(7) 2_575 . . . ? O1 Dy1 O3 C7 -30.3(6) . . . . ? O9 Dy1 O3 C7 -105.9(7) . . . . ? O2 Dy1 O3 C7 113.1(7) 3 . . . ? N1 Dy1 O3 C7 105.3(7) 3 . . . ? K1 Dy1 O3 C7 89.1(6) . . . . ? O8 Dy1 O3 K1 104.4(5) 3 . . 4_475 ? O5 Dy1 O3 K1 -4.1(3) 2_475 . . 4_475 ? O6 Dy1 O3 K1 -148.8(3) 2_575 . . 4_475 ? O1 Dy1 O3 K1 142.0(3) . . . 4_475 ? O9 Dy1 O3 K1 66.5(3) . . . 4_475 ? O2 Dy1 O3 K1 -74.6(3) 3 . . 4_475 ? N1 Dy1 O3 K1 -82.4(5) 3 . . 4_475 ? K1 Dy1 O3 K1 -98.6(3) . . . 4_475 ? O8 Dy1 O3 K1 -156.9(4) 3 . . . ? O5 Dy1 O3 K1 94.5(2) 2_475 . . . ? O6 Dy1 O3 K1 -50.1(2) 2_575 . . . ? O1 Dy1 O3 K1 -119.3(2) . . . . ? O9 Dy1 O3 K1 165.1(3) . . . . ? O2 Dy1 O3 K1 24.0(2) 3 . . . ? N1 Dy1 O3 K1 16.2(5) 3 . . . ? O4 K1 O3 C7 125.5(5) 4_475 . . . ? O10 K1 O3 C7 -57.2(5) . . . . ? O4 K1 O3 C7 -7.2(4) . . . . ? O8 K1 O3 C7 -145.2(5) 1_565 . . . ? O3 K1 O3 C7 14.2(5) 4_575 . . . ? O2 K1 O3 C7 -143.1(5) 3 . . . ? O7 K1 O3 C7 130.0(5) 1_565 . . . ? C9 K1 O3 C7 -174.7(6) 1_565 . . . ? K1 K1 O3 C7 -6.6(4) 4_575 . . . ? K1 K1 O3 C7 111.5(5) 4_475 . . . ? O4 K1 O3 Dy1 -114.0(3) 4_475 . . . ? O10 K1 O3 Dy1 63.3(2) . . . . ? O4 K1 O3 Dy1 113.3(3) . . . . ? O8 K1 O3 Dy1 -24.8(4) 1_565 . . . ? O3 K1 O3 Dy1 134.66(12) 4_575 . . . ? O2 K1 O3 Dy1 -22.61(19) 3 . . . ? O7 K1 O3 Dy1 -109.5(4) 1_565 . . . ? C7 K1 O3 Dy1 120.5(5) . . . . ? C9 K1 O3 Dy1 -54.2(6) 1_565 . . . ? K1 K1 O3 Dy1 113.9(2) 4_575 . . . ? K1 K1 O3 Dy1 -128.0(3) 4_475 . . . ? O4 K1 O3 K1 13.93(19) 4_475 . . 4_475 ? O10 K1 O3 K1 -168.69(19) . . . 4_475 ? O4 K1 O3 K1 -118.7(3) . . . 4_475 ? O8 K1 O3 K1 103.2(3) 1_565 . . 4_475 ? O3 K1 O3 K1 -97.4(3) 4_575 . . 4_475 ? O2 K1 O3 K1 105.4(2) 3 . . 4_475 ? O7 K1 O3 K1 18.4(5) 1_565 . . 4_475 ? C7 K1 O3 K1 -111.5(5) . . . 4_475 ? C9 K1 O3 K1 73.8(5) 1_565 . . 4_475 ? K1 K1 O3 K1 -118.14(15) 4_575 . . 4_475 ? O4 K1 O4 C7 -41.0(5) 4_475 . . . ? O10 K1 O4 C7 130.2(6) . . . . ? O8 K1 O4 C7 121.7(6) 1_565 . . . ? O3 K1 O4 C7 -154.1(6) 4_575 . . . ? O2 K1 O4 C7 42.8(6) 3 . . . ? O3 K1 O4 C7 7.8(5) . . . . ? O7 K1 O4 C7 -140.5(5) 1_565 . . . ? C9 K1 O4 C7 172.7(6) 1_565 . . . ? K1 K1 O4 C7 -171.3(7) 4_575 . . . ? K1 K1 O4 C7 -31.1(5) 4_475 . . . ? O4 K1 O4 K1 130.3(3) 4_475 . . 4_575 ? O10 K1 O4 K1 -58.5(2) . . . 4_575 ? O8 K1 O4 K1 -67.0(5) 1_565 . . 4_575 ? O3 K1 O4 K1 17.1(2) 4_575 . . 4_575 ? O2 K1 O4 K1 -146.0(2) 3 . . 4_575 ? O3 K1 O4 K1 179.1(4) . . . 4_575 ? O7 K1 O4 K1 30.7(5) 1_565 . . 4_575 ? C7 K1 O4 K1 171.3(7) . . . 4_575 ? C9 K1 O4 K1 -16.0(8) 1_565 . . 4_575 ? K1 K1 O4 K1 140.2(2) 4_475 . . 4_575 ? C5 N1 C1 C2 0.5(17) . . . . ? Dy1 N1 C1 C2 -175.9(7) 3_545 . . . ? C5 N1 C1 C6 -177.2(8) . . . . ? Dy1 N1 C1 C6 6.5(12) 3_545 . . . ? N1 C1 C2 C3 -4.0(16) . . . . ? C6 C1 C2 C3 173.3(9) . . . . ? N1 C1 C2 C7 178.1(10) . . . . ? C6 C1 C2 C7 -4.5(17) . . . . ? C1 C2 C3 C4 5.6(15) . . . . ? C7 C2 C3 C4 -176.4(9) . . . . ? C2 C3 C4 C5 -3.7(14) . . . . ? C2 C3 C4 C8 177.0(9) . . . . ? C1 N1 C5 C4 1.6(15) . . . . ? Dy1 N1 C5 C4 178.1(7) 3_545 . . . ? C1 N1 C5 C9 -177.7(9) . . . . ? Dy1 N1 C5 C9 -1.3(11) 3_545 . . . ? C3 C4 C5 N1 0.0(14) . . . . ? C8 C4 C5 N1 179.3(9) . . . . ? C3 C4 C5 C9 179.2(9) . . . . ? C8 C4 C5 C9 -1.4(15) . . . . ? Dy1 O1 C6 O2 -105.3(9) . . . . ? Dy1 O1 C6 C1 77.5(10) . . . . ? Dy1 O2 C6 O1 -178.7(6) 3_545 . . . ? K1 O2 C6 O1 38.6(10) 3_545 . . . ? Dy1 O2 C6 C1 -1.4(10) 3_545 . . . ? K1 O2 C6 C1 -144.2(6) 3_545 . . . ? N1 C1 C6 O1 174.1(8) . . . . ? C2 C1 C6 O1 -3.5(15) . . . . ? N1 C1 C6 O2 -3.4(13) . . . . ? C2 C1 C6 O2 179.1(9) . . . . ? K1 O4 C7 O3 177.2(6) 4_575 . . . ? K1 O4 C7 O3 -17.0(10) . . . . ? K1 O4 C7 C2 -7.4(14) 4_575 . . . ? K1 O4 C7 C2 158.4(6) . . . . ? K1 O4 C7 K1 -165.8(11) 4_575 . . . ? Dy1 O3 C7 O4 -88.2(10) . . . . ? K1 O3 C7 O4 98.3(9) 4_475 . . . ? K1 O3 C7 O4 13.7(8) . . . . ? Dy1 O3 C7 C2 96.3(7) . . . . ? K1 O3 C7 C2 -77.1(7) 4_475 . . . ? K1 O3 C7 C2 -161.8(7) . . . . ? Dy1 O3 C7 K1 -101.9(4) . . . . ? K1 O3 C7 K1 84.6(3) 4_475 . . . ? C1 C2 C7 O4 116.7(11) . . . . ? C3 C2 C7 O4 -61.2(12) . . . . ? C1 C2 C7 O3 -67.5(13) . . . . ? C3 C2 C7 O3 114.7(9) . . . . ? C1 C2 C7 K1 170.5(14) . . . . ? C3 C2 C7 K1 -7(3) . . . . ? O4 K1 C7 O4 141.0(5) 4_475 . . . ? O10 K1 C7 O4 -44.9(6) . . . . ? O8 K1 C7 O4 -102.4(7) 1_565 . . . ? O3 K1 C7 O4 26.2(6) 4_575 . . . ? O2 K1 C7 O4 -135.0(6) 3 . . . ? O3 K1 C7 O4 -166.0(8) . . . . ? O7 K1 C7 O4 80.7(9) 1_565 . . . ? C9 K1 C7 O4 -110(6) 1_565 . . . ? K1 K1 C7 O4 6.1(5) 4_575 . . . ? K1 K1 C7 O4 142.8(6) 4_475 . . . ? O4 K1 C7 O3 -52.9(5) 4_475 . . . ? O10 K1 C7 O3 121.1(5) . . . . ? O4 K1 C7 O3 166.0(8) . . . . ? O8 K1 C7 O3 63.6(8) 1_565 . . . ? O3 K1 C7 O3 -167.8(4) 4_575 . . . ? O2 K1 C7 O3 31.0(4) 3 . . . ? O7 K1 C7 O3 -113.3(7) 1_565 . . . ? C9 K1 C7 O3 56(6) 1_565 . . . ? K1 K1 C7 O3 172.2(5) 4_575 . . . ? K1 K1 C7 O3 -51.2(4) 4_475 . . . ? O4 K1 C7 C2 75.3(19) 4_475 . . . ? O10 K1 C7 C2 -110.7(19) . . . . ? O4 K1 C7 C2 -65.8(19) . . . . ? O8 K1 C7 C2 -168.2(17) 1_565 . . . ? O3 K1 C7 C2 -40(2) 4_575 . . . ? O2 K1 C7 C2 159(2) 3 . . . ? O3 K1 C7 C2 128(2) . . . . ? O7 K1 C7 C2 15(2) 1_565 . . . ? C9 K1 C7 C2 -176(5) 1_565 . . . ? K1 K1 C7 C2 -59.6(19) 4_575 . . . ? K1 K1 C7 C2 77.1(19) 4_475 . . . ? Dy1 O5 C8 O6 -158.1(8) 2_474 . . . ? Dy1 O5 C8 C4 19.2(15) 2_474 . . . ? Dy1 O6 C8 O5 130.6(8) 2_574 . . . ? Dy1 O6 C8 C4 -46.7(11) 2_574 . . . ? C3 C4 C8 O5 -83.0(10) . . . . ? C5 C4 C8 O5 97.7(10) . . . . ? C3 C4 C8 O6 94.5(10) . . . . ? C5 C4 C8 O6 -84.9(11) . . . . ? K1 O7 C9 O8 -0.8(10) 1_545 . . . ? K1 O7 C9 C5 -179.3(8) 1_545 . . . ? Dy1 O8 C9 O7 -172.3(7) 3_545 . . . ? K1 O8 C9 O7 1.0(12) 1_545 . . . ? Dy1 O8 C9 C5 6.3(12) 3_545 . . . ? K1 O8 C9 C5 179.6(6) 1_545 . . . ? Dy1 O8 C9 K1 -173.3(9) 3_545 . . 1_545 ? N1 C5 C9 O7 175.8(9) . . . . ? C4 C5 C9 O7 -3.5(15) . . . . ? N1 C5 C9 O8 -2.9(13) . . . . ? C4 C5 C9 O8 177.8(9) . . . . ? N1 C5 C9 K1 -2(3) . . . 1_545 ? C4 C5 C9 K1 179.1(19) . . . 1_545 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9A O7 0.85 1.90 2.693(8) 155.6 4_465 O9 H9B O10 0.85 1.96 2.776(9) 161.3 3_545 O10 H10A O5 0.85 2.24 2.853(9) 129.4 2_575 O10 H10A O6 0.85 2.44 3.033(8) 127.5 2_575 O10 H10A O4 0.85 2.58 3.025(10) 113.8 . O10 H10B O2 0.85 2.43 3.008(9) 125.5 3_655 O10 H10B O4 0.85 2.46 3.089(10) 131.0 4_575 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.930 _refine_diff_density_min -3.474 _refine_diff_density_rms 0.489 data_sa _database_code_depnum_ccdc_archive 'CCDC 886740' #TrackingRef 'Er-03.cif' _audit_creation_method SHELXL-97 _audit_creation_date 2012-05-23 _audit_update_record 2012-05-23 _chemical_formula_sum 'C9 H5 Er K N O10' _chemical_formula_weight 493.500 _refine_ls_R_factor_all 0.022 _cell_length_a 6.5710(13) _cell_length_b 12.445(3) _cell_length_c 14.012(3) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 1145.8(4) _cell_formula_units_Z 4 _symmetry_int_tables_number 19 _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall P_2ac_2ab loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 0.500-x,-y,0.500+z 3 0.500+x,0.500-y,-z 4 -x,0.500+y,0.500-z loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_radius_bond Er ? 1.200 K ? 1.200 O ? 1.200 H ? 1.200 N ? 1.200 C ? 1.200 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_Wyckoff_symbol _atom_site_attached_hydrogens _atom_site_calc_flag _atom_site_thermal_displace_type _atom_site_u_iso_or_equiv Er1 Er 0.0991(0) -0.1494(0) -0.7244(0) 1.000 4 a ? d Uani 0.00538(5) K1 K 0.0953(2) 0.1397(1) -0.5280(1) 1.000 4 a ? d Uani 0.01657(19) O1 O 0.1088(6) -0.0804(2) -0.5725(2) 1.000 4 a ? d Uani 0.0090(6) O2 O 0.0869(5) -0.0992(2) -0.4139(2) 1.000 4 a ? d Uani 0.0112(6) O3 O 0.2706(4) -0.2846(2) -0.2891(2) 1.000 4 a ? d Uani 0.0076(6) O4 O -0.0652(4) -0.3018(2) -0.2890(2) 1.000 4 a ? d Uani 0.0090(7) O5 O 0.2294(5) -0.6485(3) -0.5488(2) 1.000 4 a ? d Uani 0.0159(7) O6 O -0.0778(5) -0.6250(2) -0.6142(2) 1.000 4 a ? d Uani 0.0096(7) O7 O 0.1343(4) -0.5063(2) -0.7593(2) 1.000 4 a ? d Uani 0.0071(7) O8 O 0.1228(4) -0.3290(2) -0.7840(2) 1.000 4 a ? d Uani 0.0079(6) O9 O 0.2939(5) 0.0084(3) -0.7484(2) 1.000 4 a ? d Uani 0.0140(8) H9A H 0.362(6) 0.044(3) -0.707(3) 1.000 4 a ? d Uiso 0.02100 H9B H 0.335(7) 0.034(4) -0.8013(18) 1.000 4 a ? d Uiso 0.02100 O10 O 0.4572(5) 0.1667(3) -0.6318(2) 1.000 4 a ? d Uani 0.0162(7) H10A H 0.5849(19) 0.159(4) -0.629(4) 1.000 4 a ? d Uiso 0.02400 H10B H 0.431(8) 0.215(3) -0.672(3) 1.000 4 a ? d Uiso 0.02400 N1 N 0.1084(6) -0.2870(3) -0.6007(2) 1.000 4 a ? d Uani 0.0050(6) C1 C 0.1067(7) -0.2572(3) -0.5085(3) 1.000 4 a ? d Uani 0.0059(8) C2 C 0.1047(7) -0.3312(3) -0.4349(3) 1.000 4 a ? d Uani 0.0063(8) C3 C 0.1060(7) -0.4395(3) -0.4594(3) 1.000 4 a ? d Uani 0.0082(8) H3 H 0.1128 -0.4923 -0.4106 1.000 4 a ? calc Uiso 0.01000 C4 C 0.0974(7) -0.4718(3) -0.5545(3) 1.000 4 a ? d Uani 0.0075(8) C5 C 0.1041(8) -0.3913(3) -0.6239(3) 1.000 4 a ? d Uani 0.0071(8) C6 C 0.1022(7) -0.1355(3) -0.4954(3) 1.000 4 a ? d Uani 0.0077(8) C7 C 0.1044(7) -0.3018(3) -0.3291(3) 1.000 4 a ? d Uani 0.0054(7) C8 C 0.0872(8) -0.5919(3) -0.5749(3) 1.000 4 a ? d Uani 0.0095(9) C9 C 0.1188(6) -0.4112(3) -0.7309(3) 1.000 4 a ? d Uani 0.0060(7) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Er1 0.00618(8) 0.00464(7) 0.00532(8) -0.00004(8) -0.00019(8) 0.00057(8) K1 0.0140(4) 0.0136(4) 0.0221(5) -0.0004(5) 0.0019(5) -0.0016(4) O1 0.0141(15) 0.0062(13) 0.0066(14) 0.0001(15) -0.0013(15) -0.0005(11) O2 0.0172(16) 0.0081(13) 0.0082(15) -0.0029(15) -0.0033(15) -0.0033(11) O3 0.0073(15) 0.0099(14) 0.0057(17) 0.0034(12) -0.0028(12) -0.0007(12) O4 0.0074(17) 0.0114(14) 0.0082(17) 0.0019(11) 0.0011(13) -0.0015(12) O5 0.0180(16) 0.0077(14) 0.0222(18) 0.0042(16) -0.0076(13) -0.0029(15) O6 0.0124(17) 0.0081(14) 0.0082(16) -0.0049(13) -0.0006(13) -0.0011(11) O7 0.0104(16) 0.0048(13) 0.0061(16) -0.0014(11) 0.0010(12) -0.0039(11) O8 0.0122(15) 0.0055(13) 0.0059(14) 0.0024(11) -0.0001(13) 0.0001(11) O9 0.0187(18) 0.0132(16) 0.010(2) -0.0099(14) -0.0001(14) 0.0032(12) O10 0.0192(18) 0.0151(18) 0.0145(18) 0.0013(14) 0.0023(13) 0.0068(14) N1 0.0028(15) 0.0061(15) 0.0061(17) 0.0002(16) 0.0007(17) -0.0001(12) C1 0.0053(11) 0.0062(10) 0.0063(11) 0.0007(9) -0.0002(9) -0.0002(8) C2 0.0024(16) 0.0094(19) 0.0073(19) 0.000(2) 0.0015(18) -0.0023(14) C3 0.0096(19) 0.0081(18) 0.007(2) 0.000(2) 0.001(2) 0.0020(15) C4 0.0057(18) 0.0083(19) 0.009(2) 0.000(2) -0.001(2) 0.0021(15) C5 0.0070(19) 0.0060(17) 0.008(2) 0.002(2) 0.002(2) -0.0015(15) C6 0.0049(17) 0.0089(19) 0.010(2) 0.000(2) 0.0000(18) 0.0012(15) C7 0.0063(11) 0.0039(10) 0.0058(11) 0.0002(9) -0.0001(9) 0.0011(8) C8 0.014(2) 0.0092(19) 0.005(2) -0.003(2) 0.006(2) 0.0009(16) C9 0.0028(18) 0.0090(17) 0.0063(19) -0.0023(16) 0.002(2) -0.0008(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Er1 O6 . 4_553 2.286(3) no Er1 O4 . 3_544 2.296(3) no Er1 O1 . . 2.296(3) no Er1 O3 . 3_444 2.317(3) no Er1 O7 . 4_553 2.361(3) no Er1 O9 . . 2.368(3) no Er1 O8 . . 2.391(2) no Er1 N1 . . 2.437(3) no K1 O5 . 3_444 2.637(3) no K1 O5 . 1_565 2.794(4) no K1 O10 . . 2.807(3) no K1 O1 . . 2.811(3) no K1 O6 . 3_544 2.936(3) no K1 O8 . 4_553 3.024(3) no K1 O6 . 1_565 3.365(3) no K1 O2 . . 3.377(3) no K1 C8 . 1_565 3.404(4) no K1 O10 . 3_454 3.411(4) no K1 C6 . . 3.456(4) no K1 K1 . 3_554 4.3523(14) no O1 C6 . . 1.280(5) no O2 C6 . . 1.232(5) no O3 C7 . . 1.246(5) no O3 Er1 . 3_544 2.317(3) no O4 C7 . . 1.248(5) no O4 Er1 . 3_444 2.296(3) no O5 C8 . . 1.226(6) no O5 K1 . 3_544 2.637(3) no O5 K1 . 1_545 2.794(4) no O6 C8 . . 1.284(6) no O6 Er1 . 4_543 2.286(3) no O6 K1 . 3_444 2.936(3) no O6 K1 . 1_545 3.365(3) no O7 C9 . . 1.253(4) no O7 Er1 . 4_543 2.361(3) no O8 C9 . . 1.266(5) no O8 K1 . 4_543 3.024(3) no O9 H9A . . 0.856(10) no O9 H9B . . 0.85(1) no O10 K1 . 3_554 3.411(4) no O10 H10A . . 0.845(10) no O10 H10B . . 0.847(10) no N1 C5 . . 1.339(5) no N1 C1 . . 1.345(5) no C1 C2 . . 1.383(5) no C1 C6 . . 1.526(5) no C2 C3 . . 1.391(5) no C2 C7 . . 1.527(5) no C3 C4 . . 1.392(5) no C3 H3 . . 0.9500 no C4 C5 . . 1.396(5) no C4 C8 . . 1.524(5) no C5 C9 . . 1.522(6) no C8 K1 . 1_545 3.404(4) no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O6 Er1 O4 4_553 . 3_544 100.07(11) no O6 Er1 O1 4_553 . . 150.34(10) no O4 Er1 O1 3_544 . . 89.80(12) no O6 Er1 O3 4_553 . 3_444 94.07(11) no O4 Er1 O3 3_544 . 3_444 142.60(9) no O1 Er1 O3 . . 3_444 94.75(12) no O6 Er1 O7 4_553 . 4_553 76.36(10) no O4 Er1 O7 3_544 . 4_553 146.27(10) no O1 Er1 O7 . . 4_553 79.97(11) no O3 Er1 O7 3_444 . 4_553 70.75(9) no O6 Er1 O9 4_553 . . 77.45(10) no O4 Er1 O9 3_544 . . 73.25(11) no O1 Er1 O9 . . . 78.82(11) no O3 Er1 O9 3_444 . . 144.01(11) no O7 Er1 O9 4_553 . . 73.26(11) no O6 Er1 O8 4_553 . . 77.45(9) no O4 Er1 O8 3_544 . . 73.65(10) no O1 Er1 O8 . . . 132.19(10) no O3 Er1 O8 3_444 . . 75.98(10) no O7 Er1 O8 4_553 . . 135.51(10) no O9 Er1 O8 . . . 133.67(11) no O6 Er1 N1 4_553 . . 142.98(10) no O4 Er1 N1 3_544 . . 74.44(12) no O1 Er1 N1 . . . 66.6(1) no O3 Er1 N1 3_444 . . 73.51(12) no O7 Er1 N1 4_553 . . 127.95(11) no O9 Er1 N1 . . . 132.06(12) no O8 Er1 N1 . . . 65.79(10) no O5 K1 O5 3_444 . 1_565 106.93(8) no O5 K1 O10 3_444 . . 168.22(11) no O5 K1 O10 1_565 . . 64.29(10) no O5 K1 O1 3_444 . . 99.17(11) no O5 K1 O1 1_565 . . 152.41(10) no O10 K1 O1 . . . 88.57(11) no O5 K1 O6 3_444 . 3_544 113.13(10) no O5 K1 O6 1_565 . 3_544 84.20(9) no O10 K1 O6 . . 3_544 74.88(9) no O1 K1 O6 . . 3_544 93.82(9) no O5 K1 O8 3_444 . 4_553 85.3(1) no O5 K1 O8 1_565 . 4_553 86.40(8) no O10 K1 O8 . . 4_553 86.27(9) no O1 K1 O8 . . 4_553 86.98(8) no O6 K1 O8 3_544 . 4_553 161.10(9) no O5 K1 O6 3_444 . 1_565 78.6(1) no O5 K1 O6 1_565 . 1_565 41.28(8) no O10 K1 O6 . . 1_565 89.80(9) no O1 K1 O6 . . 1_565 141.17(9) no O6 K1 O6 3_544 . 1_565 123.04(7) no O8 K1 O6 4_553 . 1_565 54.21(7) no O5 K1 O2 3_444 . . 80.1(1) no O5 K1 O2 1_565 . . 152.27(9) no O10 K1 O2 . . . 111.37(9) no O1 K1 O2 . . . 41.17(7) no O6 K1 O2 3_544 . . 68.63(8) no O8 K1 O2 4_553 . . 121.20(7) no O6 K1 O2 1_565 . . 158.52(9) no O5 K1 C8 3_444 . 1_565 91.38(11) no O5 K1 C8 1_565 . 1_565 19.85(10) no O10 K1 C8 . . 1_565 78.23(11) no O1 K1 C8 . . 1_565 156.04(9) no O6 K1 C8 3_544 . 1_565 101.75(10) no O8 K1 C8 4_553 . 1_565 72.43(9) no O6 K1 C8 1_565 . 1_565 21.86(10) no O2 K1 C8 . . 1_565 162.76(9) no O5 K1 O10 3_444 . 3_454 57.35(9) no O5 K1 O10 1_565 . 3_454 59.08(9) no O10 K1 O10 . . 3_454 118.73(9) no O1 K1 O10 . . 3_454 147.36(9) no O6 K1 O10 3_544 . 3_454 78.07(8) no O8 K1 O10 4_553 . 3_454 110.77(8) no O6 K1 O10 1_565 . 3_454 62.04(8) no O2 K1 O10 . . 3_454 107.86(8) no C8 K1 O10 1_565 . 3_454 55.23(9) no O5 K1 C6 3_444 . . 89.93(10) no O5 K1 C6 1_565 . . 160.84(10) no O10 K1 C6 . . . 100.13(10) no O1 K1 C6 . . . 20.44(9) no O6 K1 C6 3_544 . . 80.73(9) no O8 K1 C6 4_553 . . 104.41(9) no O6 K1 C6 1_565 . . 156.09(10) no O2 K1 C6 . . . 20.74(8) no C8 K1 C6 1_565 . . 176.47(10) no O10 K1 C6 3_454 . . 128.07(9) no O5 K1 K1 3_444 . 3_554 126.07(8) no O5 K1 K1 1_565 . 3_554 35.51(7) no O10 K1 K1 . . 3_554 51.58(7) no O1 K1 K1 . . 3_554 129.11(8) no O6 K1 K1 3_544 . 3_554 50.55(6) no O8 K1 K1 4_553 . 3_554 115.70(6) no O6 K1 K1 1_565 . 3_554 76.78(6) no O2 K1 K1 . . 3_554 118.84(6) no C8 K1 K1 1_565 . 3_554 55.11(9) no O10 K1 K1 3_454 . 3_554 68.73(6) no C6 K1 K1 . . 3_554 126.25(8) no C6 O1 Er1 . . . 125.5(2) no C6 O1 K1 . . . 109.5(2) no Er1 O1 K1 . . . 124.70(11) no C6 O2 K1 . . . 83.2(2) no C7 O3 Er1 . . 3_544 142.4(3) no C7 O4 Er1 . . 3_444 153.5(3) no C8 O5 K1 . . 3_544 142.5(3) no C8 O5 K1 . . 1_545 109.4(3) no K1 O5 K1 3_544 . 1_545 106.49(11) no C8 O6 Er1 . . 4_543 121.2(3) no C8 O6 K1 . . 3_444 110.3(2) no Er1 O6 K1 4_543 . 3_444 128.20(13) no C8 O6 K1 . . 1_545 80.8(2) no Er1 O6 K1 4_543 . 1_545 105.07(9) no K1 O6 K1 3_444 . 1_545 87.10(7) no C9 O7 Er1 . . 4_543 133.7(3) no C9 O8 Er1 . . . 123.3(3) no C9 O8 K1 . . 4_543 113.5(2) no Er1 O8 K1 . . 4_543 113.18(9) no Er1 O9 H9A . . . 128.(3) no Er1 O9 H9B . . . 127.(3) no H9A O9 H9B . . . 103.(4) no K1 O10 K1 . . 3_554 88.28(9) no K1 O10 H10A . . . 143.(4) no K1 O10 H10A 3_554 . . 78.(4) no K1 O10 H10B . . . 105.(4) no K1 O10 H10B 3_554 . . 90.(4) no H10A O10 H10B . . . 109.(5) no C5 N1 C1 . . . 120.0(3) no C5 N1 Er1 . . . 120.6(3) no C1 N1 Er1 . . . 119.3(2) no N1 C1 C2 . . . 122.2(3) no N1 C1 C6 . . . 112.9(3) no C2 C1 C6 . . . 124.9(3) no C1 C2 C3 . . . 117.4(3) no C1 C2 C7 . . . 124.3(3) no C3 C2 C7 . . . 118.2(3) no C2 C3 C4 . . . 121.1(4) no C2 C3 H3 . . . 119.50 no C4 C3 H3 . . . 119.50 no C3 C4 C5 . . . 117.3(4) no C3 C4 C8 . . . 117.7(3) no C5 C4 C8 . . . 125.1(4) no N1 C5 C4 . . . 121.8(4) no N1 C5 C9 . . . 113.3(3) no C4 C5 C9 . . . 124.8(3) no O2 C6 O1 . . . 126.1(4) no O2 C6 C1 . . . 118.4(4) no O1 C6 C1 . . . 115.5(3) no O2 C6 K1 . . . 76.0(2) no O1 C6 K1 . . . 50.06(19) no C1 C6 K1 . . . 165.5(3) no O3 C7 O4 . . . 125.5(4) no O3 C7 C2 . . . 118.5(4) no O4 C7 C2 . . . 116.0(4) no O5 C8 O6 . . . 126.0(4) no O5 C8 C4 . . . 118.3(4) no O6 C8 C4 . . . 115.6(4) no O5 C8 K1 . . 1_545 50.7(2) no O6 C8 K1 . . 1_545 77.4(2) no C4 C8 K1 . . 1_545 157.8(3) no O7 C9 O8 . . . 125.1(4) no O7 C9 C5 . . . 118.1(3) no O8 C9 C5 . . . 116.7(3) no 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O6 Er1 O1 C6 4_553 . . . 172.2(3) no O4 Er1 O1 C6 3_544 . . . -77.5(4) no O3 Er1 O1 C6 3_444 . . . 65.3(4) no O7 Er1 O1 C6 4_553 . . . 134.8(4) no O9 Er1 O1 C6 . . . . -150.5(4) no O8 Er1 O1 C6 . . . . -10.0(5) no N1 Er1 O1 C6 . . . . -4.4(4) no O6 Er1 O1 K1 4_553 . . . -1.0(3) no O4 Er1 O1 K1 3_544 . . . 109.33(17) no O3 Er1 O1 K1 3_444 . . . -107.83(17) no O7 Er1 O1 K1 4_553 . . . -38.36(16) no O9 Er1 O1 K1 . . . . 36.38(17) no O8 Er1 O1 K1 . . . . 176.81(12) no N1 Er1 O1 K1 . . . . -177.6(2) no O5 K1 O1 C6 3_444 . . . -64.1(3) no O5 K1 O1 C6 1_565 . . . 134.9(3) no O10 K1 O1 C6 . . . . 124.8(3) no O6 K1 O1 C6 3_544 . . . 50.1(3) no O8 K1 O1 C6 4_553 . . . -148.8(3) no O6 K1 O1 C6 1_565 . . . -147.3(3) no O2 K1 O1 C6 . . . . -0.8(3) no C8 K1 O1 C6 1_565 . . . -179.1(3) no O10 K1 O1 C6 3_454 . . . -23.7(4) no K1 K1 O1 C6 3_554 . . . 90.1(3) no O5 K1 O1 Er1 3_444 . . . 110.00(18) no O5 K1 O1 Er1 1_565 . . . -51.0(3) no O10 K1 O1 Er1 . . . . -61.08(18) no O6 K1 O1 Er1 3_544 . . . -135.82(17) no O8 K1 O1 Er1 4_553 . . . 25.26(17) no O6 K1 O1 Er1 1_565 . . . 26.8(3) no O2 K1 O1 Er1 . . . . 173.3(3) no C8 K1 O1 Er1 1_565 . . . -5.1(4) no O10 K1 O1 Er1 3_454 . . . 150.43(13) no C6 K1 O1 Er1 . . . . 174.1(4) no K1 K1 O1 Er1 3_554 . . . -95.85(17) no O5 K1 O2 C6 3_444 . . . 117.2(3) no O5 K1 O2 C6 1_565 . . . -135.1(3) no O10 K1 O2 C6 . . . . -60.0(3) no O1 K1 O2 C6 . . . . 0.8(3) no O6 K1 O2 C6 3_544 . . . -123.0(3) no O8 K1 O2 C6 4_553 . . . 38.9(3) no O6 K1 O2 C6 1_565 . . . 109.8(3) no C8 K1 O2 C6 1_565 . . . 178.5(4) no O10 K1 O2 C6 3_454 . . . 168.0(3) no K1 K1 O2 C6 3_554 . . . -116.9(3) no O6 Er1 O8 C9 4_553 . . . -171.7(3) no O4 Er1 O8 C9 3_544 . . . 83.7(3) no O1 Er1 O8 C9 . . . . 9.4(4) no O3 Er1 O8 C9 3_444 . . . -74.2(3) no O7 Er1 O8 C9 4_553 . . . -116.5(3) no O9 Er1 O8 C9 . . . . 129.6(3) no N1 Er1 O8 C9 . . . . 3.8(3) no O6 Er1 O8 K1 4_553 . . 4_543 -28.56(12) no O4 Er1 O8 K1 3_544 . . 4_543 -133.15(13) no O1 Er1 O8 K1 . . . 4_543 152.56(13) no O3 Er1 O8 K1 3_444 . . 4_543 68.94(12) no O7 Er1 O8 K1 4_553 . . 4_543 26.60(19) no O9 Er1 O8 K1 . . . 4_543 -87.21(16) no N1 Er1 O8 K1 . . . 4_543 146.90(16) no O5 K1 O10 K1 3_444 . . 3_554 83.0(5) no O5 K1 O10 K1 1_565 . . 3_554 39.53(8) no O1 K1 O10 K1 . . . 3_554 -145.61(8) no O6 K1 O10 K1 3_544 . . 3_554 -51.26(7) no O8 K1 O10 K1 4_553 . . 3_554 127.33(8) no O6 K1 O10 K1 1_565 . . 3_554 73.19(8) no O2 K1 O10 K1 . . . 3_554 -110.53(8) no C8 K1 O10 K1 1_565 . . 3_554 54.51(9) no O10 K1 O10 K1 3_454 . . 3_554 15.64(8) no C6 K1 O10 K1 . . . 3_554 -128.68(9) no O6 Er1 N1 C5 4_553 . . . 1.7(5) no O4 Er1 N1 C5 3_544 . . . -84.4(4) no O1 Er1 N1 C5 . . . . 178.9(4) no O3 Er1 N1 C5 3_444 . . . 76.0(4) no O7 Er1 N1 C5 4_553 . . . 124.2(4) no O9 Er1 N1 C5 . . . . -133.6(4) no O8 Er1 N1 C5 . . . . -5.7(4) no O6 Er1 N1 C1 4_553 . . . -174.7(3) no O4 Er1 N1 C1 3_544 . . . 99.1(4) no O1 Er1 N1 C1 . . . . 2.5(3) no O3 Er1 N1 C1 3_444 . . . -100.4(4) no O7 Er1 N1 C1 4_553 . . . -52.2(4) no O9 Er1 N1 C1 . . . . 50.0(4) no O8 Er1 N1 C1 . . . . 177.9(4) no C5 N1 C1 C2 . . . . 1.3(8) no Er1 N1 C1 C2 . . . . 177.7(3) no C5 N1 C1 C6 . . . . -177.3(4) no Er1 N1 C1 C6 . . . . -0.9(5) no N1 C1 C2 C3 . . . . 0.5(7) no C6 C1 C2 C3 . . . . 178.9(4) no N1 C1 C2 C7 . . . . 179.5(4) no C6 C1 C2 C7 . . . . -2.1(7) no C1 C2 C3 C4 . . . . -3.7(7) no C7 C2 C3 C4 . . . . 177.2(4) no C2 C3 C4 C5 . . . . 5.0(7) no C2 C3 C4 C8 . . . . -176.6(4) no C1 N1 C5 C4 . . . . 0.1(8) no Er1 N1 C5 C4 . . . . -176.2(4) no C1 N1 C5 C9 . . . . -176.7(4) no Er1 N1 C5 C9 . . . . 6.9(6) no C3 C4 C5 N1 . . . . -3.2(8) no C8 C4 C5 N1 . . . . 178.5(5) no C3 C4 C5 C9 . . . . 173.3(4) no C8 C4 C5 C9 . . . . -5.0(8) no K1 O2 C6 O1 . . . . -1.4(5) no K1 O2 C6 C1 . . . . -179.1(4) no Er1 O1 C6 O2 . . . . -172.3(4) no K1 O1 C6 O2 . . . . 1.8(6) no Er1 O1 C6 C1 . . . . 5.5(6) no K1 O1 C6 C1 . . . . 179.6(3) no Er1 O1 C6 K1 . . . . -174.0(4) no N1 C1 C6 O2 . . . . 175.3(4) no C2 C1 C6 O2 . . . . -3.2(7) no N1 C1 C6 O1 . . . . -2.7(6) no C2 C1 C6 O1 . . . . 178.8(4) no N1 C1 C6 K1 . . . . -1.3(14) no C2 C1 C6 K1 . . . . -179.9(9) no O5 K1 C6 O2 3_444 . . . -61.2(3) no O5 K1 C6 O2 1_565 . . . 90.9(4) no O10 K1 C6 O2 . . . . 125.0(3) no O1 K1 C6 O2 . . . . -178.5(5) no O6 K1 C6 O2 3_544 . . . 52.3(3) no O8 K1 C6 O2 4_553 . . . -146.3(3) no O6 K1 C6 O2 1_565 . . . -121.8(3) no C8 K1 C6 O2 1_565 . . . -172.9(19) no O10 K1 C6 O2 3_454 . . . -14.5(3) no K1 K1 C6 O2 3_554 . . . 75.7(3) no O5 K1 C6 O1 3_444 . . . 117.4(3) no O5 K1 C6 O1 1_565 . . . -90.6(4) no O10 K1 C6 O1 . . . . -56.5(3) no O6 K1 C6 O1 3_544 . . . -129.2(3) no O8 K1 C6 O1 4_553 . . . 32.2(3) no O6 K1 C6 O1 1_565 . . . 56.8(4) no O2 K1 C6 O1 . . . . 178.5(5) no C8 K1 C6 O1 1_565 . . . 6.(2) no O10 K1 C6 O1 3_454 . . . 164.0(3) no K1 K1 C6 O1 3_554 . . . -105.8(3) no O5 K1 C6 C1 3_444 . . . 115.8(12) no O5 K1 C6 C1 1_565 . . . -92.2(12) no O10 K1 C6 C1 . . . . -58.0(12) no O1 K1 C6 C1 . . . . -1.6(10) no O6 K1 C6 C1 3_544 . . . -130.7(12) no O8 K1 C6 C1 4_553 . . . 30.7(12) no O6 K1 C6 C1 1_565 . . . 55.2(13) no O2 K1 C6 C1 . . . . 177.0(14) no C8 K1 C6 C1 1_565 . . . 4.(3) no O10 K1 C6 C1 3_454 . . . 162.5(11) no K1 K1 C6 C1 3_554 . . . -107.4(12) no Er1 O3 C7 O4 3_544 . . . 132.5(4) no Er1 O3 C7 C2 3_544 . . . -44.2(6) no Er1 O4 C7 O3 3_444 . . . -155.8(4) no Er1 O4 C7 C2 3_444 . . . 20.9(8) no C1 C2 C7 O3 . . . . -85.5(5) no C3 C2 C7 O3 . . . . 93.5(5) no C1 C2 C7 O4 . . . . 97.5(5) no C3 C2 C7 O4 . . . . -83.5(5) no K1 O5 C8 O6 3_544 . . . 178.0(3) no K1 O5 C8 O6 1_545 . . . -19.5(5) no K1 O5 C8 C4 3_544 . . . -5.9(7) no K1 O5 C8 C4 1_545 . . . 156.6(3) no K1 O5 C8 K1 3_544 . . 1_545 -162.5(5) no Er1 O6 C8 O5 4_543 . . . -86.8(5) no K1 O6 C8 O5 3_444 . . . 98.8(4) no K1 O6 C8 O5 1_545 . . . 15.3(4) no Er1 O6 C8 C4 4_543 . . . 97.0(4) no K1 O6 C8 C4 3_444 . . . -77.5(4) no K1 O6 C8 C4 1_545 . . . -160.9(3) no Er1 O6 C8 K1 4_543 . . 1_545 -102.1(2) no K1 O6 C8 K1 3_444 . . 1_545 83.42(14) no C3 C4 C8 O5 . . . . -61.6(6) no C5 C4 C8 O5 . . . . 116.7(5) no C3 C4 C8 O6 . . . . 114.9(5) no C5 C4 C8 O6 . . . . -66.8(6) no C3 C4 C8 K1 . . . 1_545 -7.3(12) no C5 C4 C8 K1 . . . 1_545 171.0(6) no Er1 O7 C9 O8 4_543 . . . -106.6(4) no Er1 O7 C9 C5 4_543 . . . 76.5(5) no Er1 O8 C9 O7 . . . . -178.7(3) no K1 O8 C9 O7 4_543 . . . 38.2(5) no Er1 O8 C9 C5 . . . . -1.7(5) no K1 O8 C9 C5 4_543 . . . -144.8(3) no N1 C5 C9 O7 . . . . 173.8(4) no C4 C5 C9 O7 . . . . -3.0(7) no N1 C5 C9 O8 . . . . -3.4(6) no C4 C5 C9 O8 . . . . 179.8(4) no data_r91114e _database_code_depnum_ccdc_archive 'CCDC 886741' #TrackingRef 'Nd-01.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H5 K N Nd O10' _chemical_formula_weight 470.48 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' 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ORTHORHOMBIC, _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 14.120(3) _cell_length_b 12.545(3) _cell_length_c 6.6886(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1184.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 4544 _cell_measurement_theta_min 2.171 _cell_measurement_theta_max 27.880 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 4.795 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7003 _exptl_absorpt_correction_T_max 0.8314 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9641 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.85 _reflns_number_total 2811 _reflns_number_gt 2665 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalclear(Rigaku/MSC Inc., 2005)' _computing_cell_refinement crystalclear _computing_data_reduction crystalclear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0401P)^2^+1.6641P] 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 CONATR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.489(19) _refine_ls_number_reflns 2811 _refine_ls_number_parameters 199 _refine_ls_number_restraints 136 _refine_ls_R_factor_all 0.0279 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0703 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.002 _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 Nd1 Nd 0.978612(16) 0.600294(18) 1.35138(3) 0.00201(8) Uani 1 1 d U . . K1 K 0.78144(8) 0.89000(9) 0.34687(18) 0.0147(2) Uani 1 1 d U . . O1 O 0.9578(2) 0.5268(3) 1.0219(5) 0.0049(7) Uani 1 1 d U . . O2 O 0.9626(2) 0.5539(3) 0.6956(5) 0.0075(7) Uani 1 1 d U . . O3 O 0.8356(2) 0.3510(3) 0.8334(6) 0.0090(7) Uani 1 1 d U . . O4 O 0.6793(2) 0.3320(3) 0.8620(6) 0.0062(6) Uani 1 1 d U . . O5 O 0.4693(2) 0.5858(3) 0.8814(5) 0.0071(6) Uani 1 1 d U . . O6 O 0.4985(2) 0.7596(3) 0.8974(4) 0.0048(7) Uani 1 1 d U . . O7 O 0.6453(2) 0.8749(3) 0.6798(5) 0.0086(7) Uani 1 1 d U . . O8 O 0.7108(3) 0.8953(4) 0.9800(6) 0.0153(8) Uani 1 1 d U . . O9 O 1.0020(3) 0.7660(3) 1.5414(5) 0.0117(8) Uani 1 1 d DU . . H9A H 0.9591 0.7839 1.6238 0.014 Uiso 1 1 d RD . . H9B H 1.0524 0.8030 1.5406 0.014 Uiso 1 1 d RD . . O10 O 0.8826(3) 0.9175(3) 0.7048(6) 0.0153(8) Uani 1 1 d DU . . H10A H 0.8537 0.9154 0.8162 0.018 Uiso 1 1 d RD . . H10B H 0.9420 0.9280 0.7018 0.018 Uiso 1 1 d R . . N1 N 0.6517(3) 0.5386(3) 0.8653(7) 0.0043(7) Uani 1 1 d U . . C1 C 0.9199(3) 0.5486(4) 0.8612(8) 0.0045(8) Uani 1 1 d U . . C2 C 0.8159(3) 0.5791(4) 0.8596(7) 0.0045(8) Uani 1 1 d U . . C3 C 0.7418(3) 0.5069(4) 0.8602(7) 0.0034(8) Uani 1 1 d U . . C4 C 0.6303(3) 0.6428(4) 0.8626(8) 0.0042(8) Uani 1 1 d U . . C5 C 0.6996(3) 0.7210(4) 0.8540(8) 0.0039(8) Uani 1 1 d U . . C6 C 0.7944(3) 0.6868(4) 0.8562(8) 0.0051(8) Uani 1 1 d U . . H6 H 0.8431 0.7368 0.8554 0.006 Uiso 1 1 calc R . . C7 C 0.7549(3) 0.3867(4) 0.8531(7) 0.0048(8) Uani 1 1 d U . . C8 C 0.5243(3) 0.6649(4) 0.8797(6) 0.0047(8) Uani 1 1 d U . . C9 C 0.6827(3) 0.8392(4) 0.8409(8) 0.0074(9) Uani 1 1 d U . . 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 Nd1 0.00177(11) 0.00132(11) 0.00295(11) 0.00009(9) 0.00022(9) -0.00068(9) K1 0.0212(5) 0.0109(5) 0.0119(4) -0.0009(5) -0.0018(4) 0.0012(4) O1 0.0047(10) 0.0049(10) 0.0052(10) 0.0001(8) -0.0011(8) 0.0007(8) O2 0.0069(10) 0.0091(10) 0.0065(10) 0.0003(8) 0.0016(8) 0.0011(8) O3 0.0077(10) 0.0087(10) 0.0107(10) -0.0010(9) -0.0005(8) 0.0019(8) O4 0.0055(9) 0.0047(10) 0.0083(9) 0.0012(9) -0.0001(8) 0.0000(8) O5 0.0066(10) 0.0062(10) 0.0085(10) -0.0001(8) -0.0003(8) -0.0010(8) O6 0.0048(10) 0.0039(10) 0.0058(10) 0.0017(8) 0.0021(8) -0.0005(8) O7 0.0084(10) 0.0083(11) 0.0090(11) 0.0010(8) -0.0002(8) -0.0001(8) O8 0.0178(11) 0.0128(11) 0.0152(11) -0.0008(9) -0.0024(8) -0.0004(9) O9 0.0107(11) 0.0120(11) 0.0125(10) -0.0018(9) 0.0009(8) -0.0021(8) O10 0.0145(11) 0.0153(12) 0.0160(11) 0.0011(9) -0.0005(8) -0.0017(9) N1 0.0045(10) 0.0044(11) 0.0041(10) 0.0005(9) -0.0003(9) -0.0004(8) C1 0.0042(11) 0.0042(11) 0.0050(11) -0.0002(9) 0.0006(9) -0.0003(9) C2 0.0045(11) 0.0046(11) 0.0044(11) 0.0006(9) 0.0000(9) 0.0003(9) C3 0.0026(11) 0.0036(11) 0.0040(11) 0.0006(9) -0.0006(9) -0.0003(9) C4 0.0043(11) 0.0042(11) 0.0040(11) 0.0002(9) 0.0002(9) 0.0004(9) C5 0.0042(11) 0.0037(11) 0.0038(11) -0.0001(9) -0.0003(9) 0.0006(9) C6 0.0044(11) 0.0057(11) 0.0053(11) -0.0008(9) 0.0001(9) -0.0005(9) C7 0.0047(11) 0.0057(11) 0.0039(11) 0.0001(9) -0.0001(9) 0.0003(9) C8 0.0049(11) 0.0049(11) 0.0042(11) 0.0003(9) -0.0001(9) -0.0001(9) C9 0.0072(12) 0.0068(12) 0.0081(12) 0.0005(9) 0.0002(9) 0.0000(9) _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 Nd1 O7 2.383(4) 3_567 ? Nd1 O2 2.386(3) 1_556 ? Nd1 O4 2.387(3) 2_665 ? Nd1 O1 2.407(3) . ? Nd1 O6 2.436(3) 3_567 ? Nd1 O5 2.456(3) 2_665 ? Nd1 O9 2.458(4) . ? Nd1 N1 2.536(4) 2_665 ? Nd1 K1 4.4942(14) 4_746 ? Nd1 K1 4.5783(14) 1_556 ? K1 O8 2.650(4) 1_554 ? K1 O10 2.809(4) . ? K1 O8 2.839(5) 2_674 ? K1 O4 2.841(4) 2_664 ? K1 O7 2.947(4) . ? K1 O5 3.076(4) 3_566 ? K1 O7 3.319(4) 2_674 ? K1 C9 3.435(5) 2_674 ? K1 C7 3.509(5) 2_664 ? K1 K1 4.4261(16) 2_675 ? K1 K1 4.4261(16) 2_674 ? K1 Nd1 4.4942(14) 4_756 ? O1 C1 1.231(6) . ? O2 C1 1.264(6) . ? O2 Nd1 2.386(3) 1_554 ? O3 C7 1.231(6) . ? O4 C7 1.270(6) . ? O4 Nd1 2.387(3) 2_664 ? O4 K1 2.841(4) 2_665 ? O5 C8 1.260(6) . ? O5 Nd1 2.456(3) 2_664 ? O5 K1 3.076(4) 3_466 ? O6 C8 1.248(6) . ? O6 Nd1 2.436(3) 3_467 ? O7 C9 1.281(6) . ? O7 Nd1 2.383(4) 3_467 ? O7 K1 3.319(4) 2_675 ? O8 C9 1.232(7) . ? O8 K1 2.650(4) 1_556 ? O8 K1 2.839(5) 2_675 ? O9 H9A 0.8488 . ? O9 H9B 0.8494 . ? O10 H10A 0.8500 . ? O10 H10B 0.8501 . ? N1 C3 1.334(6) . ? N1 C4 1.341(6) . ? N1 Nd1 2.536(4) 2_664 ? C1 C2 1.518(6) . ? C2 C3 1.383(6) . ? C2 C6 1.384(6) . ? C3 C7 1.520(6) . ? C4 C5 1.387(6) . ? C4 C8 1.526(6) . ? C5 C6 1.406(6) . ? C5 C9 1.505(6) . ? C6 H6 0.9300 . ? C7 K1 3.509(5) 2_665 ? C9 K1 3.435(5) 2_675 ? 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 O7 Nd1 O2 102.10(12) 3_567 1_556 ? O7 Nd1 O4 151.49(12) 3_567 2_665 ? O2 Nd1 O4 88.26(13) 1_556 2_665 ? O7 Nd1 O1 95.19(11) 3_567 . ? O2 Nd1 O1 141.14(12) 1_556 . ? O4 Nd1 O1 92.84(12) 2_665 . ? O7 Nd1 O6 74.47(11) 3_567 3_567 ? O2 Nd1 O6 147.80(12) 1_556 3_567 ? O4 Nd1 O6 82.63(12) 2_665 3_567 ? O1 Nd1 O6 70.42(11) . 3_567 ? O7 Nd1 O5 80.53(12) 3_567 2_665 ? O2 Nd1 O5 73.58(11) 1_556 2_665 ? O4 Nd1 O5 127.98(11) 2_665 2_665 ? O1 Nd1 O5 75.36(11) . 2_665 ? O6 Nd1 O5 134.98(11) 3_567 2_665 ? O7 Nd1 O9 78.60(12) 3_567 . ? O2 Nd1 O9 73.75(13) 1_556 . ? O4 Nd1 O9 79.00(12) 2_665 . ? O1 Nd1 O9 144.44(12) . . ? O6 Nd1 O9 74.20(12) 3_567 . ? O5 Nd1 O9 136.16(12) 2_665 . ? O7 Nd1 N1 144.03(12) 3_567 2_665 ? O2 Nd1 N1 74.22(13) 1_556 2_665 ? O4 Nd1 N1 64.26(12) 2_665 2_665 ? O1 Nd1 N1 71.46(13) . 2_665 ? O6 Nd1 N1 127.20(12) 3_567 2_665 ? O5 Nd1 N1 63.95(12) 2_665 2_665 ? O9 Nd1 N1 131.26(13) . 2_665 ? O7 Nd1 K1 46.06(9) 3_567 4_746 ? O2 Nd1 K1 102.28(9) 1_556 4_746 ? O4 Nd1 K1 157.20(9) 2_665 4_746 ? O1 Nd1 K1 66.24(8) . 4_746 ? O6 Nd1 K1 97.75(8) 3_567 4_746 ? O5 Nd1 K1 40.57(8) 2_665 4_746 ? O9 Nd1 K1 123.20(9) . 4_746 ? N1 Nd1 K1 98.88(9) 2_665 4_746 ? O7 Nd1 K1 119.77(9) 3_567 1_556 ? O2 Nd1 K1 98.20(9) 1_556 1_556 ? O4 Nd1 K1 31.76(8) 2_665 1_556 ? O1 Nd1 K1 102.92(8) . 1_556 ? O6 Nd1 K1 59.55(8) 3_567 1_556 ? O5 Nd1 K1 159.58(8) 2_665 1_556 ? O9 Nd1 K1 54.12(9) . 1_556 ? N1 Nd1 K1 96.00(9) 2_665 1_556 ? K1 Nd1 K1 157.294(17) 4_746 1_556 ? O8 K1 O10 167.86(13) 1_554 . ? O8 K1 O8 106.33(10) 1_554 2_674 ? O10 K1 O8 66.21(12) . 2_674 ? O8 K1 O4 97.53(13) 1_554 2_664 ? O10 K1 O4 89.47(12) . 2_664 ? O8 K1 O4 155.67(12) 2_674 2_664 ? O8 K1 O7 117.13(12) 1_554 . ? O10 K1 O7 72.27(11) . . ? O8 K1 O7 81.31(11) 2_674 . ? O4 K1 O7 92.15(11) 2_664 . ? O8 K1 O5 82.09(11) 1_554 3_566 ? O10 K1 O5 88.42(11) . 3_566 ? O8 K1 O5 91.66(10) 2_674 3_566 ? O4 K1 O5 86.91(10) 2_664 3_566 ? O7 K1 O5 160.68(10) . 3_566 ? O8 K1 O7 77.48(11) 1_554 2_674 ? O10 K1 O7 91.12(11) . 2_674 ? O8 K1 O7 41.46(10) 2_674 2_674 ? O4 K1 O7 145.30(10) 2_664 2_674 ? O7 K1 O7 120.96(8) . 2_674 ? O5 K1 O7 58.43(9) 3_566 2_674 ? O8 K1 C9 91.15(13) 1_554 2_674 ? O10 K1 C9 79.25(13) . 2_674 ? O8 K1 C9 19.89(12) 2_674 2_674 ? O4 K1 C9 160.21(11) 2_664 2_674 ? O7 K1 C9 99.69(11) . 2_674 ? O5 K1 C9 76.67(11) 3_566 2_674 ? O7 K1 C9 21.77(11) 2_674 2_674 ? O8 K1 C7 88.90(12) 1_554 2_664 ? O10 K1 C7 100.70(12) . 2_664 ? O8 K1 C7 160.12(11) 2_674 2_664 ? O4 K1 C7 19.71(10) 2_664 2_664 ? O7 K1 C7 80.35(11) . 2_664 ? O5 K1 C7 103.27(10) 3_566 2_664 ? O7 K1 C7 158.20(11) 2_674 2_664 ? C9 K1 C7 179.92(12) 2_674 2_664 ? O8 K1 K1 127.50(10) 1_554 2_675 ? O10 K1 K1 51.79(9) . 2_675 ? O8 K1 K1 34.83(8) 2_674 2_675 ? O4 K1 K1 128.56(9) 2_664 2_675 ? O7 K1 K1 48.57(7) . 2_675 ? O5 K1 K1 119.11(8) 3_566 2_675 ? O7 K1 K1 76.28(7) 2_674 2_675 ? C9 K1 K1 54.67(10) 2_674 2_675 ? C7 K1 K1 125.34(8) 2_664 2_675 ? O8 K1 K1 37.73(10) 1_554 2_674 ? O10 K1 K1 132.02(10) . 2_674 ? O8 K1 K1 69.70(9) 2_674 2_674 ? O4 K1 K1 132.63(9) 2_664 2_674 ? O7 K1 K1 118.68(9) . 2_674 ? O5 K1 K1 74.72(7) 3_566 2_674 ? O7 K1 K1 41.75(7) 2_674 2_674 ? C9 K1 K1 53.42(9) 2_674 2_674 ? C7 K1 K1 126.62(8) 2_664 2_674 ? K1 K1 K1 98.15(5) 2_675 2_674 ? O8 K1 Nd1 89.76(9) 1_554 4_756 ? O10 K1 Nd1 78.24(9) . 4_756 ? O8 K1 Nd1 60.44(8) 2_674 4_756 ? O4 K1 Nd1 116.03(8) 2_664 4_756 ? O7 K1 Nd1 138.77(8) . 4_756 ? O5 K1 Nd1 31.29(6) 3_566 4_756 ? O7 K1 Nd1 31.14(6) 2_674 4_756 ? C9 K1 Nd1 45.95(9) 2_674 4_756 ? C7 K1 Nd1 133.98(8) 2_664 4_756 ? K1 K1 Nd1 90.46(4) 2_675 4_756 ? K1 K1 Nd1 64.04(3) 2_674 4_756 ? C1 O1 Nd1 140.1(3) . . ? C1 O2 Nd1 154.7(3) . 1_554 ? C7 O4 Nd1 126.2(3) . 2_664 ? C7 O4 K1 111.3(3) . 2_665 ? Nd1 O4 K1 122.00(13) 2_664 2_665 ? C8 O5 Nd1 124.3(3) . 2_664 ? C8 O5 K1 116.7(3) . 3_466 ? Nd1 O5 K1 108.14(12) 2_664 3_466 ? C8 O6 Nd1 131.0(3) . 3_467 ? C9 O7 Nd1 121.7(3) . 3_467 ? C9 O7 K1 112.9(3) . . ? Nd1 O7 K1 124.72(14) 3_467 . ? C9 O7 K1 84.2(3) . 2_675 ? Nd1 O7 K1 102.79(12) 3_467 2_675 ? K1 O7 K1 89.67(9) . 2_675 ? C9 O8 K1 143.8(4) . 1_556 ? C9 O8 K1 108.5(3) . 2_675 ? K1 O8 K1 107.44(14) 1_556 2_675 ? Nd1 O9 H9A 117.6 . . ? Nd1 O9 H9B 124.8 . . ? H9A O9 H9B 117.2 . . ? K1 O10 H10A 119.9 . . ? K1 O10 H10B 120.1 . . ? H10A O10 H10B 120.0 . . ? C3 N1 C4 120.3(4) . . ? C3 N1 Nd1 119.1(3) . 2_664 ? C4 N1 Nd1 120.4(3) . 2_664 ? O1 C1 O2 124.7(4) . . ? O1 C1 C2 118.9(4) . . ? O2 C1 C2 116.3(4) . . ? C3 C2 C6 118.3(4) . . ? C3 C2 C1 124.5(4) . . ? C6 C2 C1 117.2(4) . . ? N1 C3 C2 121.8(4) . . ? N1 C3 C7 114.3(4) . . ? C2 C3 C7 123.9(4) . . ? N1 C4 C5 122.1(4) . . ? N1 C4 C8 113.4(4) . . ? C5 C4 C8 124.5(4) . . ? C4 C5 C6 117.1(4) . . ? C4 C5 C9 126.0(4) . . ? C6 C5 C9 116.9(4) . . ? C2 C6 C5 120.4(4) . . ? C2 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? O3 C7 O4 125.9(5) . . ? O3 C7 C3 118.5(4) . . ? O4 C7 C3 115.6(4) . . ? O3 C7 K1 76.9(3) . 2_665 ? O4 C7 K1 49.0(2) . 2_665 ? C3 C7 K1 164.6(3) . 2_665 ? O6 C8 O5 124.7(4) . . ? O6 C8 C4 117.8(4) . . ? O5 C8 C4 117.5(4) . . ? O8 C9 O7 124.7(5) . . ? O8 C9 C5 117.8(5) . . ? O7 C9 C5 117.4(5) . . ? O8 C9 K1 51.6(3) . 2_675 ? O7 C9 K1 74.0(3) . 2_675 ? C5 C9 K1 161.9(3) . 2_675 ? 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 O7 Nd1 O1 C1 -113.5(5) 3_567 . . . ? O2 Nd1 O1 C1 129.9(5) 1_556 . . . ? O4 Nd1 O1 C1 39.1(5) 2_665 . . . ? O6 Nd1 O1 C1 -42.0(5) 3_567 . . . ? O5 Nd1 O1 C1 167.7(5) 2_665 . . . ? O9 Nd1 O1 C1 -35.9(5) . . . . ? N1 Nd1 O1 C1 100.7(5) 2_665 . . . ? K1 Nd1 O1 C1 -150.3(5) 4_746 . . . ? K1 Nd1 O1 C1 8.7(5) 1_556 . . . ? O8 K1 O7 C9 159.0(3) 1_554 . . . ? O10 K1 O7 C9 -29.3(3) . . . . ? O8 K1 O7 C9 -97.0(3) 2_674 . . . ? O4 K1 O7 C9 59.4(3) 2_664 . . . ? O5 K1 O7 C9 -27.3(5) 3_566 . . . ? O7 K1 O7 C9 -109.6(3) 2_674 . . . ? C9 K1 O7 C9 -104.6(4) 2_674 . . . ? C7 K1 O7 C9 75.3(3) 2_664 . . . ? K1 K1 O7 C9 -83.6(3) 2_675 . . . ? K1 K1 O7 C9 -158.1(3) 2_674 . . . ? Nd1 K1 O7 C9 -75.7(4) 4_756 . . . ? O8 K1 O7 Nd1 -12.0(2) 1_554 . . 3_467 ? O10 K1 O7 Nd1 159.7(2) . . . 3_467 ? O8 K1 O7 Nd1 91.96(18) 2_674 . . 3_467 ? O4 K1 O7 Nd1 -111.59(17) 2_664 . . 3_467 ? O5 K1 O7 Nd1 161.6(2) 3_566 . . 3_467 ? O7 K1 O7 Nd1 79.33(19) 2_674 . . 3_467 ? C9 K1 O7 Nd1 84.33(18) 2_674 . . 3_467 ? C7 K1 O7 Nd1 -95.74(17) 2_664 . . 3_467 ? K1 K1 O7 Nd1 105.39(18) 2_675 . . 3_467 ? K1 K1 O7 Nd1 30.89(19) 2_674 . . 3_467 ? Nd1 K1 O7 Nd1 113.25(15) 4_756 . . 3_467 ? O8 K1 O7 K1 -117.40(13) 1_554 . . 2_675 ? O10 K1 O7 K1 54.26(10) . . . 2_675 ? O8 K1 O7 K1 -13.43(10) 2_674 . . 2_675 ? O4 K1 O7 K1 143.02(10) 2_664 . . 2_675 ? O5 K1 O7 K1 56.2(3) 3_566 . . 2_675 ? O7 K1 O7 K1 -26.07(12) 2_674 . . 2_675 ? C9 K1 O7 K1 -21.06(11) 2_674 . . 2_675 ? C7 K1 O7 K1 158.86(11) 2_664 . . 2_675 ? K1 K1 O7 K1 -74.50(9) 2_674 . . 2_675 ? Nd1 K1 O7 K1 7.86(15) 4_756 . . 2_675 ? Nd1 O1 C1 O2 123.1(5) . . . . ? Nd1 O1 C1 C2 -52.4(7) . . . . ? Nd1 O2 C1 O1 -166.0(5) 1_554 . . . ? Nd1 O2 C1 C2 9.7(10) 1_554 . . . ? O1 C1 C2 C3 -82.6(6) . . . . ? O2 C1 C2 C3 101.5(6) . . . . ? O1 C1 C2 C6 97.7(6) . . . . ? O2 C1 C2 C6 -78.2(6) . . . . ? C4 N1 C3 C2 2.4(8) . . . . ? Nd1 N1 C3 C2 177.5(4) 2_664 . . . ? C4 N1 C3 C7 -176.9(5) . . . . ? Nd1 N1 C3 C7 -1.9(6) 2_664 . . . ? C6 C2 C3 N1 -2.6(7) . . . . ? C1 C2 C3 N1 177.8(5) . . . . ? C6 C2 C3 C7 176.8(5) . . . . ? C1 C2 C3 C7 -2.9(8) . . . . ? C3 N1 C4 C5 0.2(8) . . . . ? Nd1 N1 C4 C5 -174.8(4) 2_664 . . . ? C3 N1 C4 C8 -177.1(4) . . . . ? Nd1 N1 C4 C8 7.9(6) 2_664 . . . ? N1 C4 C5 C6 -2.5(8) . . . . ? C8 C4 C5 C6 174.5(5) . . . . ? N1 C4 C5 C9 177.0(5) . . . . ? C8 C4 C5 C9 -6.0(8) . . . . ? C3 C2 C6 C5 0.2(8) . . . . ? C1 C2 C6 C5 179.8(5) . . . . ? C4 C5 C6 C2 2.2(8) . . . . ? C9 C5 C6 C2 -177.3(5) . . . . ? Nd1 O4 C7 O3 -170.3(4) 2_664 . . . ? K1 O4 C7 O3 2.4(6) 2_665 . . . ? Nd1 O4 C7 C3 7.4(6) 2_664 . . . ? K1 O4 C7 C3 -180.0(3) 2_665 . . . ? Nd1 O4 C7 K1 -172.6(5) 2_664 . . 2_665 ? N1 C3 C7 O3 174.8(5) . . . . ? C2 C3 C7 O3 -4.6(7) . . . . ? N1 C3 C7 O4 -3.0(7) . . . . ? C2 C3 C7 O4 177.6(5) . . . . ? N1 C3 C7 K1 -3.1(14) . . . 2_665 ? C2 C3 C7 K1 177.5(9) . . . 2_665 ? Nd1 O6 C8 O5 -102.1(5) 3_467 . . . ? Nd1 O6 C8 C4 80.3(5) 3_467 . . . ? Nd1 O5 C8 O6 -179.1(3) 2_664 . . . ? K1 O5 C8 O6 41.0(5) 3_466 . . . ? Nd1 O5 C8 C4 -1.4(6) 2_664 . . . ? K1 O5 C8 C4 -141.3(3) 3_466 . . . ? N1 C4 C8 O6 173.4(4) . . . . ? C5 C4 C8 O6 -3.8(7) . . . . ? N1 C4 C8 O5 -4.4(7) . . . . ? C5 C4 C8 O5 178.4(5) . . . . ? K1 O8 C9 O7 174.9(3) 1_556 . . . ? K1 O8 C9 O7 -13.0(6) 2_675 . . . ? K1 O8 C9 C5 -9.8(8) 1_556 . . . ? K1 O8 C9 C5 162.4(3) 2_675 . . . ? K1 O8 C9 K1 -172.1(7) 1_556 . . 2_675 ? Nd1 O7 C9 O8 -90.9(5) 3_467 . . . ? K1 O7 C9 O8 97.7(5) . . . . ? K1 O7 C9 O8 10.5(5) 2_675 . . . ? Nd1 O7 C9 C5 93.7(5) 3_467 . . . ? K1 O7 C9 C5 -77.6(4) . . . . ? K1 O7 C9 C5 -164.8(4) 2_675 . . . ? Nd1 O7 C9 K1 -101.5(3) 3_467 . . 2_675 ? K1 O7 C9 K1 87.19(19) . . . 2_675 ? C4 C5 C9 O8 117.1(6) . . . . ? C6 C5 C9 O8 -63.4(7) . . . . ? C4 C5 C9 O7 -67.2(7) . . . . ? C6 C5 C9 O7 112.2(5) . . . . ? C4 C5 C9 K1 167.0(9) . . . 2_675 ? C6 C5 C9 K1 -13.6(14) . . . 2_675 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.700 _refine_diff_density_min -1.657 _refine_diff_density_rms 0.161