# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Thomas Albrecht-Schmitt' 'Evgeny V. Alekseev' 'Wulf Depmeier' 'Shuao Wang.' _publ_contact_author_name ' Thomas Albrecht-Schmitt' _publ_contact_author_email TALBREC1@ND.EDU _publ_section_title ; Further Insights into Intermediate- and Mixed-Valency in Neptunium Oxoanion Compounds: Structure and Absorption Spectroscopy of K2[(NpO2)3B10O16(OH)2(NO3)2] ; # Attachment 'KNpBNO.cif' data_KNpBNO _database_code_depnum_ccdc_archive 'CCDC 765550' #TrackingRef 'KNpBNO.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Potassium neptunium nitratoborate' _chemical_melting_point n/a _chemical_formula_moiety 'K2[(Np(VI)O2) (Np(V)O2)2 B10 O16 (OH)2](NO3)2' _chemical_formula_sum 'B10 K2 N2 Np3 O30' _chemical_formula_weight 1405.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Np Np -11.4937 4.1493 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.599(5) _cell_length_b 16.026(12) _cell_length_c 11.053(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.922(13) _cell_angle_gamma 90.00 _cell_volume 1168.7(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2026 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 24.88 _exptl_crystal_description Tablet _exptl_crystal_colour Pink _exptl_crystal_size_max 0.047 _exptl_crystal_size_mid 0.041 _exptl_crystal_size_min 0.009 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 3.993 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1242 _exptl_absorpt_coefficient_mu 13.738 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.530 _exptl_absorpt_correction_T_max 0.884 _exptl_absorpt_process_details SHELTXPREP _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Imus microfocused' _diffrn_radiation_monochromator 'Quazar optics' _diffrn_measurement_device_type 'BRUKER apex II' _diffrn_measurement_method '0.5 wide w/ exposures' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10978 _diffrn_reflns_av_R_equivalents 0.1462 _diffrn_reflns_av_sigmaI/netI 0.0901 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 24.88 _reflns_number_total 2026 _reflns_number_gt 1447 _reflns_threshold_expression >2sigma(I) _computing_data_collection smart _computing_cell_refinement 'smart saint' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXCIF-97 (Sheldrick, 2000)' _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^)+(0.0765P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2026 _refine_ls_number_parameters 214 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0740 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1350 _refine_ls_wR_factor_gt 0.1259 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Np1 Np 0.60760(8) 0.24933(4) 0.90114(5) 0.00900(18) Uani 1 1 d . . . Np2 Np 0.5000 0.5000 1.0000 0.0173(2) Uani 1 2 d S . . B1 B 1.069(2) 0.2350(10) 0.9503(16) 0.007(4) Uani 1 1 d . . . B2 B 0.590(3) 0.4467(12) 0.6203(17) 0.016(4) Uani 1 1 d U . . B3 B 0.305(3) 0.1748(11) 1.1078(16) 0.010(3) Uani 1 1 d U . . B4 B 0.456(3) 0.3110(11) 0.6499(17) 0.013(4) Uani 1 1 d U . . B5 B 1.112(3) 0.2769(11) 0.7330(16) 0.009(4) Uani 1 1 d U . . N1 N 0.111(2) 0.4303(9) 1.0860(13) 0.022(3) Uani 1 1 d . . . K1 K 0.3592(5) 0.0116(2) 0.8408(3) 0.0193(8) Uani 1 1 d . . . O1 O 0.6234(14) 0.1393(6) 0.8676(9) 0.010(2) Uani 1 1 d U . . O2 O 0.5928(15) 0.3605(7) 0.9368(9) 0.017(3) Uani 1 1 d . . . O3 O 0.9153(14) 0.2287(6) 1.0288(9) 0.006(2) Uani 1 1 d U . . O4 O 0.2640(15) 0.2115(6) 0.9792(9) 0.010(2) Uani 1 1 d U . . O5 O 0.3241(16) 0.2736(6) 0.7409(10) 0.013(2) Uani 1 1 d . . . O6 O 0.1700(18) 0.5057(8) 1.1139(10) 0.028(3) Uani 1 1 d . . . O7 O 0.5171(15) 0.2016(7) 1.1276(9) 0.012(2) Uani 1 1 d . . . O8 O 1.0048(15) 0.2623(6) 0.8371(9) 0.010(2) Uani 1 1 d . . . O9 O 0.6613(15) 0.2868(7) 0.6892(9) 0.012(2) Uani 1 1 d . . . O10 O 0.2264(17) 0.3933(7) 1.0114(11) 0.025(3) Uani 1 1 d . . . O11 O 0.4313(15) 0.3983(6) 0.6422(9) 0.010(2) Uani 1 1 d U . . O12 O 0.7895(15) 0.4148(7) 0.6005(10) 0.015(2) Uani 1 1 d . . . O13 O 0.5619(17) 0.5316(6) 0.6199(10) 0.014(3) Uani 1 1 d . . . O14 O -0.0394(18) 0.3996(8) 1.1286(11) 0.025(3) Uani 1 1 d . . . O15 O 0.4017(18) 0.5260(8) 0.8583(11) 0.028(3) Uani 1 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 Np1 0.0109(3) 0.0154(3) 0.0007(3) 0.0003(2) 0.0000(2) 0.0000(3) Np2 0.0226(5) 0.0223(5) 0.0070(4) -0.0011(4) 0.0000(3) 0.0006(5) B1 0.004(8) 0.015(10) 0.002(8) -0.004(7) 0.000(6) -0.003(7) B2 0.020(5) 0.015(5) 0.012(5) -0.004(4) -0.003(4) 0.000(4) B3 0.009(5) 0.011(5) 0.010(5) 0.001(4) 0.001(4) 0.001(4) B4 0.014(5) 0.014(5) 0.010(5) 0.000(4) 0.000(4) 0.003(4) B5 0.009(5) 0.012(5) 0.007(5) 0.000(4) 0.001(4) 0.000(4) N1 0.018(8) 0.029(9) 0.017(8) 0.002(7) 0.001(6) 0.012(7) K1 0.0145(18) 0.026(2) 0.0175(18) 0.0027(17) -0.0012(14) -0.0039(16) O1 0.007(4) 0.014(4) 0.010(4) -0.002(3) -0.002(3) -0.004(3) O2 0.012(6) 0.029(7) 0.010(6) 0.009(5) -0.007(5) -0.001(5) O3 0.007(3) 0.007(3) 0.003(3) -0.001(2) -0.002(2) 0.001(2) O4 0.010(3) 0.012(3) 0.009(3) 0.001(2) 0.002(2) 0.000(2) O5 0.013(6) 0.017(6) 0.007(6) -0.002(4) -0.007(4) 0.002(5) O6 0.046(8) 0.019(6) 0.021(6) -0.002(6) 0.009(5) 0.005(7) O7 0.009(5) 0.024(6) 0.003(5) -0.002(4) -0.002(4) 0.000(5) O8 0.009(5) 0.013(6) 0.006(6) -0.002(4) 0.002(4) -0.001(4) O9 0.015(6) 0.018(6) 0.005(5) 0.002(4) 0.004(5) 0.007(5) O10 0.019(6) 0.036(7) 0.021(7) -0.006(6) 0.003(5) 0.007(6) O11 0.008(4) 0.013(4) 0.009(4) 0.005(3) -0.002(3) 0.001(3) O12 0.008(5) 0.024(6) 0.012(6) 0.002(5) -0.004(4) 0.004(5) O13 0.021(6) 0.010(5) 0.010(6) 0.000(4) -0.002(5) 0.007(5) O14 0.021(7) 0.038(8) 0.016(7) 0.001(6) 0.004(5) -0.004(6) O15 0.024(7) 0.046(9) 0.013(6) -0.005(5) -0.006(5) 0.001(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Np1 O1 1.805(10) . ? Np1 O2 1.828(12) . ? Np1 O9 2.449(10) . ? Np1 O3 2.476(10) . ? Np1 O4 2.513(10) . ? Np1 O5 2.585(10) . ? Np1 O7 2.694(10) . ? Np1 O8 2.734(10) . ? Np1 B1 3.091(16) . ? Np1 B4 3.098(18) . ? Np1 K1 4.196(5) . ? Np2 O15 1.736(12) . ? Np2 O15 1.736(12) 3_667 ? Np2 O2 2.424(12) 3_667 ? Np2 O2 2.424(12) . ? Np2 O10 2.491(12) 3_667 ? Np2 O10 2.491(12) . ? Np2 O6 2.534(11) . ? Np2 O6 2.534(12) 3_667 ? Np2 N1 2.970(15) 3_667 ? Np2 N1 2.970(15) . ? Np2 K1 4.422(4) 4_666 ? Np2 K1 4.422(4) 2_556 ? B1 O3 1.348(18) . ? B1 O4 1.375(19) 1_655 ? B1 O8 1.38(2) . ? B2 O11 1.33(2) . ? B2 O13 1.37(2) . ? B2 O12 1.43(2) . ? B2 K1 3.18(2) 2_556 ? B3 O12 1.44(2) 4_566 ? B3 O9 1.45(2) 4_566 ? B3 O7 1.48(2) . ? B3 O4 1.56(2) . ? B4 O11 1.41(2) . ? B4 O9 1.47(2) . ? B4 O5 1.47(2) . ? B4 O3 1.50(2) 4_565 ? B5 O7 1.36(2) 4_665 ? B5 O8 1.38(2) . ? B5 O5 1.404(19) 1_655 ? N1 O14 1.210(18) . ? N1 O10 1.277(18) . ? N1 O6 1.306(19) . ? N1 K1 3.421(15) 4_566 ? K1 O11 2.650(11) 2_546 ? K1 O1 2.701(10) . ? K1 O15 2.781(12) 2_546 ? K1 O14 2.832(12) 4_665 ? K1 O13 2.838(12) 2_546 ? K1 O12 2.856(11) 2_646 ? K1 O12 3.144(11) 4_566 ? K1 B2 3.18(2) 2_546 ? K1 O6 3.277(12) 4_665 ? K1 N1 3.421(15) 4_665 ? K1 K1 3.972(7) 3_657 ? O3 B4 1.50(2) 4_666 ? O4 B1 1.375(19) 1_455 ? O5 B5 1.404(19) 1_455 ? O6 K1 3.277(12) 4_566 ? O7 B5 1.36(2) 4_566 ? O9 B3 1.45(2) 4_665 ? O11 K1 2.650(10) 2_556 ? O12 B3 1.44(2) 4_665 ? O12 K1 2.856(11) 2_656 ? O12 K1 3.144(11) 4_665 ? O13 K1 2.838(12) 2_556 ? O14 K1 2.832(12) 4_566 ? O15 K1 2.781(12) 2_556 ? 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 O1 Np1 O2 179.3(5) . . ? O1 Np1 O9 91.9(4) . . ? O2 Np1 O9 88.7(4) . . ? O1 Np1 O3 86.4(4) . . ? O2 Np1 O3 93.1(4) . . ? O9 Np1 O3 116.6(3) . . ? O1 Np1 O4 83.7(4) . . ? O2 Np1 O4 96.3(4) . . ? O9 Np1 O4 122.2(3) . . ? O3 Np1 O4 120.6(3) . . ? O1 Np1 O5 92.9(4) . . ? O2 Np1 O5 87.7(4) . . ? O9 Np1 O5 54.7(3) . . ? O3 Np1 O5 171.2(3) . . ? O4 Np1 O5 67.9(3) . . ? O1 Np1 O7 85.9(4) . . ? O2 Np1 O7 93.6(4) . . ? O9 Np1 O7 174.8(3) . . ? O3 Np1 O7 68.0(3) . . ? O4 Np1 O7 53.0(3) . . ? O5 Np1 O7 120.7(3) . . ? O1 Np1 O8 87.8(4) . . ? O2 Np1 O8 92.1(4) . . ? O9 Np1 O8 65.2(3) . . ? O3 Np1 O8 51.4(3) . . ? O4 Np1 O8 168.9(3) . . ? O5 Np1 O8 119.8(3) . . ? O7 Np1 O8 119.3(3) . . ? O1 Np1 B1 84.5(4) . . ? O2 Np1 B1 95.2(4) . . ? O9 Np1 B1 91.7(4) . . ? O3 Np1 B1 25.0(4) . . ? O4 Np1 B1 144.4(4) . . ? O5 Np1 B1 146.2(4) . . ? O7 Np1 B1 92.8(4) . . ? O8 Np1 B1 26.6(4) . . ? O1 Np1 B4 98.4(5) . . ? O2 Np1 B4 82.2(5) . . ? O9 Np1 B4 27.7(4) . . ? O3 Np1 B4 143.4(4) . . ? O4 Np1 B4 96.0(4) . . ? O5 Np1 B4 28.1(4) . . ? O7 Np1 B4 148.2(4) . . ? O8 Np1 B4 92.3(4) . . ? B1 Np1 B4 118.9(5) . . ? O1 Np1 K1 26.4(3) . . ? O2 Np1 K1 153.8(3) . . ? O9 Np1 K1 97.6(3) . . ? O3 Np1 K1 106.5(2) . . ? O4 Np1 K1 58.9(2) . . ? O5 Np1 K1 75.6(2) . . ? O7 Np1 K1 78.4(2) . . ? O8 Np1 K1 113.7(2) . . ? B1 Np1 K1 110.0(3) . . ? B4 Np1 K1 91.6(3) . . ? O15 Np2 O15 179.999(5) . 3_667 ? O15 Np2 O2 86.9(5) . 3_667 ? O15 Np2 O2 93.1(5) 3_667 3_667 ? O15 Np2 O2 93.1(5) . . ? O15 Np2 O2 86.9(5) 3_667 . ? O2 Np2 O2 180.000(2) 3_667 . ? O15 Np2 O10 92.9(5) . 3_667 ? O15 Np2 O10 87.1(5) 3_667 3_667 ? O2 Np2 O10 64.4(4) 3_667 3_667 ? O2 Np2 O10 115.6(4) . 3_667 ? O15 Np2 O10 87.1(5) . . ? O15 Np2 O10 92.9(5) 3_667 . ? O2 Np2 O10 115.6(4) 3_667 . ? O2 Np2 O10 64.4(4) . . ? O10 Np2 O10 180.0 3_667 . ? O15 Np2 O6 97.3(5) . . ? O15 Np2 O6 82.7(5) 3_667 . ? O2 Np2 O6 66.4(4) 3_667 . ? O2 Np2 O6 113.6(4) . . ? O10 Np2 O6 129.0(4) 3_667 . ? O10 Np2 O6 51.0(4) . . ? O15 Np2 O6 82.7(5) . 3_667 ? O15 Np2 O6 97.3(5) 3_667 3_667 ? O2 Np2 O6 113.6(4) 3_667 3_667 ? O2 Np2 O6 66.4(4) . 3_667 ? O10 Np2 O6 51.0(4) 3_667 3_667 ? O10 Np2 O6 129.0(4) . 3_667 ? O6 Np2 O6 179.999(2) . 3_667 ? O15 Np2 N1 86.2(5) . 3_667 ? O15 Np2 N1 93.8(5) 3_667 3_667 ? O2 Np2 N1 88.2(4) 3_667 3_667 ? O2 Np2 N1 91.8(4) . 3_667 ? O10 Np2 N1 25.1(4) 3_667 3_667 ? O10 Np2 N1 154.9(4) . 3_667 ? O6 Np2 N1 154.1(4) . 3_667 ? O6 Np2 N1 25.9(4) 3_667 3_667 ? O15 Np2 N1 93.8(5) . . ? O15 Np2 N1 86.2(5) 3_667 . ? O2 Np2 N1 91.8(4) 3_667 . ? O2 Np2 N1 88.2(4) . . ? O10 Np2 N1 154.9(4) 3_667 . ? O10 Np2 N1 25.1(4) . . ? O6 Np2 N1 25.9(4) . . ? O6 Np2 N1 154.1(4) 3_667 . ? N1 Np2 N1 179.999(1) 3_667 . ? O15 Np2 K1 165.0(4) . 4_666 ? O15 Np2 K1 15.0(4) 3_667 4_666 ? O2 Np2 K1 85.9(2) 3_667 4_666 ? O2 Np2 K1 94.1(2) . 4_666 ? O10 Np2 K1 72.1(3) 3_667 4_666 ? O10 Np2 K1 107.9(3) . 4_666 ? O6 Np2 K1 91.8(3) . 4_666 ? O6 Np2 K1 88.2(3) 3_667 4_666 ? N1 Np2 K1 80.5(3) 3_667 4_666 ? N1 Np2 K1 99.5(3) . 4_666 ? O15 Np2 K1 15.0(4) . 2_556 ? O15 Np2 K1 165.0(4) 3_667 2_556 ? O2 Np2 K1 94.1(2) 3_667 2_556 ? O2 Np2 K1 85.9(2) . 2_556 ? O10 Np2 K1 107.9(3) 3_667 2_556 ? O10 Np2 K1 72.1(3) . 2_556 ? O6 Np2 K1 88.2(3) . 2_556 ? O6 Np2 K1 91.8(3) 3_667 2_556 ? N1 Np2 K1 99.5(3) 3_667 2_556 ? N1 Np2 K1 80.5(3) . 2_556 ? K1 Np2 K1 180.0 4_666 2_556 ? O3 B1 O4 122.7(14) . 1_655 ? O3 B1 O8 112.6(12) . . ? O4 B1 O8 124.6(14) 1_655 . ? O3 B1 Np1 51.0(7) . . ? O4 B1 Np1 167.8(11) 1_655 . ? O8 B1 Np1 62.2(7) . . ? O11 B2 O13 118.1(16) . . ? O11 B2 O12 123.3(15) . . ? O13 B2 O12 118.6(16) . . ? O11 B2 K1 55.0(8) . 2_556 ? O13 B2 K1 63.2(9) . 2_556 ? O12 B2 K1 177.8(12) . 2_556 ? O12 B3 O9 114.3(13) 4_566 4_566 ? O12 B3 O7 111.3(13) 4_566 . ? O9 B3 O7 114.3(13) 4_566 . ? O12 B3 O4 108.3(12) 4_566 . ? O9 B3 O4 107.5(12) 4_566 . ? O7 B3 O4 100.1(11) . . ? O11 B4 O9 112.7(13) . . ? O11 B4 O5 112.1(13) . . ? O9 B4 O5 104.1(13) . . ? O11 B4 O3 110.3(13) . 4_565 ? O9 B4 O3 107.6(13) . 4_565 ? O5 B4 O3 109.8(13) . 4_565 ? O11 B4 Np1 114.0(10) . . ? O9 B4 Np1 50.8(7) . . ? O5 B4 Np1 56.1(7) . . ? O3 B4 Np1 135.6(10) 4_565 . ? O7 B5 O8 121.6(14) 4_665 . ? O7 B5 O5 120.5(14) 4_665 1_655 ? O8 B5 O5 117.8(14) . 1_655 ? O14 N1 O10 124.4(15) . . ? O14 N1 O6 121.9(14) . . ? O10 N1 O6 113.8(14) . . ? O14 N1 Np2 175.0(11) . . ? O10 N1 Np2 56.0(8) . . ? O6 N1 Np2 58.1(7) . . ? O14 N1 K1 51.5(8) . 4_566 ? O10 N1 K1 163.7(10) . 4_566 ? O6 N1 K1 72.6(8) . 4_566 ? Np2 N1 K1 126.5(5) . 4_566 ? O11 K1 O1 167.9(3) 2_546 . ? O11 K1 O15 71.0(3) 2_546 2_546 ? O1 K1 O15 114.5(4) . 2_546 ? O11 K1 O14 125.8(3) 2_546 4_665 ? O1 K1 O14 63.2(3) . 4_665 ? O15 K1 O14 57.0(4) 2_546 4_665 ? O11 K1 O13 49.8(3) 2_546 2_546 ? O1 K1 O13 122.0(3) . 2_546 ? O15 K1 O13 61.1(3) 2_546 2_546 ? O14 K1 O13 108.4(3) 4_665 2_546 ? O11 K1 O12 101.3(3) 2_546 2_646 ? O1 K1 O12 82.3(3) . 2_646 ? O15 K1 O12 135.6(4) 2_546 2_646 ? O14 K1 O12 105.0(3) 4_665 2_646 ? O13 K1 O12 145.1(3) 2_546 2_646 ? O11 K1 O12 94.3(3) 2_546 4_566 ? O1 K1 O12 73.7(3) . 4_566 ? O15 K1 O12 126.4(3) 2_546 4_566 ? O14 K1 O12 127.4(3) 4_665 4_566 ? O13 K1 O12 70.1(3) 2_546 4_566 ? O12 K1 O12 97.3(3) 2_646 4_566 ? O11 K1 B2 24.3(4) 2_546 2_546 ? O1 K1 B2 146.6(4) . 2_546 ? O15 K1 B2 64.4(4) 2_546 2_546 ? O14 K1 B2 120.7(4) 4_665 2_546 ? O13 K1 B2 25.6(4) 2_546 2_546 ? O12 K1 B2 123.2(4) 2_646 2_546 ? O12 K1 B2 81.3(4) 4_566 2_546 ? O11 K1 O6 117.3(3) 2_546 4_665 ? O1 K1 O6 74.8(3) . 4_665 ? O15 K1 O6 77.8(4) 2_546 4_665 ? O14 K1 O6 41.4(3) 4_665 4_665 ? O13 K1 O6 138.9(3) 2_546 4_665 ? O12 K1 O6 67.2(3) 2_646 4_665 ? O12 K1 O6 146.4(3) 4_566 4_665 ? B2 K1 O6 132.3(4) 2_546 4_665 ? O11 K1 N1 127.3(3) 2_546 4_665 ? O1 K1 N1 64.1(3) . 4_665 ? O15 K1 N1 68.2(4) 2_546 4_665 ? O14 K1 N1 19.5(3) 4_665 4_665 ? O13 K1 N1 125.8(3) 2_546 4_665 ? O12 K1 N1 86.1(4) 2_646 4_665 ? O12 K1 N1 136.8(3) 4_566 4_665 ? B2 K1 N1 131.8(4) 2_546 4_665 ? O6 K1 N1 22.4(3) 4_665 4_665 ? O11 K1 K1 101.6(3) 2_546 3_657 ? O1 K1 K1 71.4(2) . 3_657 ? O15 K1 K1 169.7(3) 2_546 3_657 ? O14 K1 K1 131.9(3) 4_665 3_657 ? O13 K1 K1 108.7(3) 2_546 3_657 ? O12 K1 K1 51.8(2) 2_646 3_657 ? O12 K1 K1 45.5(2) 4_566 3_657 ? B2 K1 K1 105.9(4) 2_546 3_657 ? O6 K1 K1 112.4(3) 4_665 3_657 ? N1 K1 K1 121.9(3) 4_665 3_657 ? O11 K1 Np1 153.2(2) 2_546 . ? O1 K1 Np1 17.3(2) . . ? O15 K1 Np1 106.6(3) 2_546 . ? O14 K1 Np1 65.1(3) 4_665 . ? O13 K1 Np1 104.7(2) 2_546 . ? O12 K1 Np1 98.3(2) 2_646 . ? O12 K1 Np1 65.0(2) 4_566 . ? B2 K1 Np1 129.7(4) 2_546 . ? O6 K1 Np1 87.2(2) 4_665 . ? N1 K1 Np1 72.0(2) 4_665 . ? K1 K1 Np1 76.60(11) 3_657 . ? Np1 O1 K1 136.3(5) . . ? Np1 O2 Np2 167.4(6) . . ? B1 O3 B4 118.7(12) . 4_666 ? B1 O3 Np1 103.9(9) . . ? B4 O3 Np1 134.2(9) 4_666 . ? B1 O4 B3 117.6(12) 1_455 . ? B1 O4 Np1 134.5(10) 1_455 . ? B3 O4 Np1 105.1(8) . . ? B5 O5 B4 123.0(12) 1_455 . ? B5 O5 Np1 139.4(10) 1_455 . ? B4 O5 Np1 95.7(9) . . ? N1 O6 Np2 96.0(9) . . ? N1 O6 K1 85.1(8) . 4_566 ? Np2 O6 K1 158.5(5) . 4_566 ? B5 O7 B3 128.5(13) 4_566 . ? B5 O7 Np1 128.3(10) 4_566 . ? B3 O7 Np1 99.7(8) . . ? B5 O8 B1 130.9(12) . . ? B5 O8 Np1 137.3(9) . . ? B1 O8 Np1 91.2(8) . . ? B3 O9 B4 108.2(12) 4_665 . ? B3 O9 Np1 143.3(9) 4_665 . ? B4 O9 Np1 101.6(9) . . ? N1 O10 Np2 98.9(10) . . ? B2 O11 B4 119.9(13) . . ? B2 O11 K1 100.7(10) . 2_556 ? B4 O11 K1 139.3(9) . 2_556 ? B2 O12 B3 114.3(13) . 4_665 ? B2 O12 K1 121.0(9) . 2_656 ? B3 O12 K1 118.2(9) 4_665 2_656 ? B2 O12 K1 98.8(9) . 4_665 ? B3 O12 K1 114.4(9) 4_665 4_665 ? K1 O12 K1 82.7(3) 2_656 4_665 ? B2 O13 K1 91.3(10) . 2_556 ? N1 O14 K1 108.9(10) . 4_566 ? Np2 O15 K1 155.7(7) . 2_556 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.88 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.602 _refine_diff_density_min -2.555 _refine_diff_density_rms 0.477