# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_kg_177_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common NaBA_BA_2H2O _chemical_melting_point ? _chemical_formula_moiety 'Na1 C4 H3 N2 O3, C4 H4 N2 O3, 2(H2 O)' _chemical_formula_sum 'C8 H11 N4 Na O8' _chemical_formula_weight 314.20 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' Na Na 0.0362 0.0249 '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' _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 6.419(1) _cell_length_b 10.026(2) _cell_length_c 10.326(2) _cell_angle_alpha 69.67(2) _cell_angle_beta 80.22(2) _cell_angle_gamma 80.44(1) _cell_volume 610.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4662 _cell_measurement_theta_min 3.2474 _cell_measurement_theta_max 29.2439 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 324 _exptl_absorpt_coefficient_mu 0.181 _exptl_absorpt_correction_T_min 0.97557 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.1340 _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16020 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 29.33 _reflns_number_total 16020 _reflns_number_gt 11877 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.1352P)^2^+0.0772P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16020 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0982 _refine_ls_R_factor_gt 0.0720 _refine_ls_wR_factor_ref 0.2032 _refine_ls_wR_factor_gt 0.1847 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.000 _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 H100 H 0.1795 0.5584 0.2990 0.050 Uiso 1 1 d . . . H101 H 0.1679 0.6356 0.3812 0.050 Uiso 1 1 d . . . H200 H -0.1817 0.9531 0.2002 0.050 Uiso 1 1 d . . . H201 H -0.2969 0.8996 0.1399 0.050 Uiso 1 1 d . . . O6 O 0.4210(2) 0.27163(11) -0.05878(12) 0.0425(3) Uani 1 1 d . . . O2W O -0.1905(2) 0.94898(12) 0.11954(11) 0.0376(3) Uani 1 1 d . . . C2 C 0.2087(3) 0.62891(15) -0.10638(15) 0.0251(3) Uani 1 1 d . . . C4 C 0.2859(3) 0.60220(15) -0.33480(15) 0.0249(3) Uani 1 1 d . . . C5 C 0.3223(3) 0.44450(15) -0.26876(14) 0.0270(4) Uani 1 1 d . . . H5A H 0.4497 0.4087 -0.3177 0.032 Uiso 1 1 calc R . . H5B H 0.2039 0.4032 -0.2814 0.032 Uiso 1 1 calc R . . C6 C 0.3462(3) 0.39254(15) -0.11845(15) 0.0254(3) Uani 1 1 d . . . C12 C 0.3049(3) 1.01724(15) 0.28844(15) 0.0246(3) Uani 1 1 d . . . C13 C 0.2358(3) 1.04617(15) 0.51654(14) 0.0230(3) Uani 1 1 d . . . C15 C 0.2337(3) 1.19357(15) 0.45471(15) 0.0270(4) Uani 1 1 d . . . H15 H 0.2092 1.2519 0.5101 0.032 Uiso 1 1 calc R . . C16 C 0.2678(3) 1.25420(15) 0.31159(15) 0.0250(3) Uani 1 1 d . . . N1 N 0.2716(2) 0.48681(12) -0.04713(12) 0.0255(3) Uani 1 1 d . . . H1 H 0.2638 0.4536 0.0421 0.031 Uiso 1 1 calc R . . N3 N 0.2262(2) 0.68217(13) -0.24858(12) 0.0270(3) Uani 1 1 d . . . H3 H 0.1973 0.7731 -0.2865 0.032 Uiso 1 1 calc R . . N11 N 0.3023(2) 1.16213(12) 0.23406(12) 0.0259(3) Uani 1 1 d . . . H11 H 0.3237 1.1994 0.1450 0.031 Uiso 1 1 calc R . . N13 N 0.2729(2) 0.96481(12) 0.42772(12) 0.0247(3) Uani 1 1 d . . . H13 H 0.2756 0.8735 0.4654 0.030 Uiso 1 1 calc R . . Na1 Na 0.17369(11) 0.84486(6) 0.09471(6) 0.03361(18) Uani 1 1 d . . . O2 O 0.1436(2) 0.70607(11) -0.03634(12) 0.0426(3) Uani 1 1 d . . . O1W O 0.1285(2) 0.63491(12) 0.30134(12) 0.0428(3) Uani 1 1 d . . . O4 O 0.3017(2) 0.65768(11) -0.46033(10) 0.0376(3) Uani 1 1 d . . . O12 O 0.3365(2) 0.94067(11) 0.21461(11) 0.0333(3) Uani 1 1 d . . . O14 O 0.2089(2) 0.97726(10) 0.64473(10) 0.0322(3) Uani 1 1 d . . . O16 O 0.2704(2) 1.38570(10) 0.24236(10) 0.0333(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 O6 0.0635(9) 0.0254(6) 0.0267(6) -0.0025(5) -0.0019(6) 0.0104(6) O2W 0.0390(8) 0.0440(7) 0.0332(6) -0.0167(5) 0.0025(6) -0.0123(6) C2 0.0298(9) 0.0238(8) 0.0231(8) -0.0067(6) -0.0057(7) -0.0063(7) C4 0.0271(9) 0.0223(7) 0.0242(8) -0.0045(6) -0.0038(7) -0.0056(7) C5 0.0343(10) 0.0225(7) 0.0239(8) -0.0073(6) -0.0036(7) -0.0029(7) C6 0.0257(9) 0.0257(8) 0.0208(7) -0.0033(6) 0.0017(7) -0.0066(7) C12 0.0248(9) 0.0250(8) 0.0234(8) -0.0075(6) -0.0021(7) -0.0030(6) C13 0.0239(9) 0.0258(7) 0.0199(7) -0.0068(6) -0.0063(7) -0.0027(6) C15 0.0349(10) 0.0263(8) 0.0229(8) -0.0117(6) -0.0060(7) -0.0011(7) C16 0.0271(9) 0.0213(7) 0.0258(8) -0.0065(6) -0.0040(7) -0.0031(7) N1 0.0353(8) 0.0206(6) 0.0192(6) -0.0046(5) -0.0051(6) -0.0021(6) N3 0.0354(9) 0.0234(6) 0.0201(6) -0.0041(5) -0.0056(6) -0.0018(6) N11 0.0392(9) 0.0216(6) 0.0146(6) -0.0028(5) -0.0034(6) -0.0038(6) N13 0.0346(8) 0.0175(6) 0.0207(6) -0.0039(5) -0.0061(6) -0.0022(6) Na1 0.0439(4) 0.0293(3) 0.0321(4) -0.0141(3) -0.0086(3) -0.0036(3) O2 0.0733(10) 0.0269(6) 0.0309(6) -0.0154(5) -0.0063(7) -0.0016(6) O1W 0.0540(9) 0.0370(7) 0.0422(7) -0.0175(5) -0.0128(7) -0.0016(6) O4 0.0588(9) 0.0307(6) 0.0206(6) -0.0045(4) -0.0058(6) -0.0050(6) O12 0.0488(8) 0.0291(6) 0.0277(6) -0.0167(5) -0.0031(6) -0.0057(5) O14 0.0485(8) 0.0280(6) 0.0171(5) -0.0031(4) -0.0032(6) -0.0067(5) O16 0.0542(9) 0.0193(5) 0.0225(6) -0.0026(4) -0.0038(6) -0.0037(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O6 C6 1.2116(17) . ? O6 Na1 2.6894(15) 2_665 ? O2W Na1 2.4065(15) . ? O2W Na1 2.4483(14) 2_575 ? C2 O2 1.2146(17) . ? C2 N1 1.3616(17) . ? C2 N3 1.3686(18) . ? C4 O4 1.2137(17) . ? C4 N3 1.3640(18) . ? C4 C5 1.4837(19) . ? C5 C6 1.482(2) . ? C6 N1 1.3707(19) . ? C12 O12 1.2305(17) . ? C12 N13 1.3406(18) . ? C12 N11 1.3618(17) . ? C13 O14 1.2593(17) . ? C13 C15 1.3902(19) . ? C13 N13 1.3945(18) . ? C15 C16 1.383(2) . ? C16 O16 1.2640(16) . ? C16 N11 1.3883(18) . ? Na1 O12 2.2687(13) . ? Na1 O2 2.3003(13) . ? Na1 O1W 2.4370(14) . ? Na1 O2W 2.4483(14) 2_575 ? Na1 O6 2.6894(15) 2_665 ? Na1 Na1 3.6640(15) 2_575 ? 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 C6 O6 Na1 127.15(11) . 2_665 ? Na1 O2W Na1 98.00(5) . 2_575 ? O2 C2 N1 121.54(14) . . ? O2 C2 N3 121.20(14) . . ? N1 C2 N3 117.25(13) . . ? O4 C4 N3 121.23(13) . . ? O4 C4 C5 121.49(14) . . ? N3 C4 C5 117.24(12) . . ? C4 C5 C6 115.91(13) . . ? O6 C6 N1 120.71(13) . . ? O6 C6 C5 122.57(14) . . ? N1 C6 C5 116.67(13) . . ? O12 C12 N13 122.84(13) . . ? O12 C12 N11 122.15(13) . . ? N13 C12 N11 115.01(13) . . ? O14 C13 C15 127.10(14) . . ? O14 C13 N13 116.02(13) . . ? C15 C13 N13 116.88(12) . . ? C16 C15 C13 120.56(14) . . ? O16 C16 C15 127.03(14) . . ? O16 C16 N11 115.72(12) . . ? C15 C16 N11 117.25(12) . . ? C6 N1 C2 125.19(12) . . ? C2 N3 C4 125.07(12) . . ? C12 N11 C16 124.91(12) . . ? C12 N13 C13 125.38(12) . . ? O12 Na1 O2 157.38(6) . . ? O12 Na1 O2W 102.97(5) . . ? O2 Na1 O2W 99.64(5) . . ? O12 Na1 O1W 89.69(4) . . ? O2 Na1 O1W 88.09(4) . . ? O2W Na1 O1W 94.69(5) . . ? O12 Na1 O2W 95.00(4) . 2_575 ? O2 Na1 O2W 88.46(4) . 2_575 ? O2W Na1 O2W 82.00(5) . 2_575 ? O1W Na1 O2W 174.76(5) . 2_575 ? O12 Na1 O6 78.62(5) . 2_665 ? O2 Na1 O6 78.78(5) . 2_665 ? O2W Na1 O6 178.14(4) . 2_665 ? O1W Na1 O6 86.27(5) . 2_665 ? O2W Na1 O6 96.92(5) 2_575 2_665 ? O12 Na1 Na1 101.87(4) . 2_575 ? O2 Na1 Na1 95.28(4) . 2_575 ? O2W Na1 Na1 41.43(3) . 2_575 ? O1W Na1 Na1 135.98(5) . 2_575 ? O2W Na1 Na1 40.57(3) 2_575 2_575 ? O6 Na1 Na1 137.48(4) 2_665 2_575 ? C2 O2 Na1 155.56(13) . . ? C12 O12 Na1 143.60(12) . . ? _diffrn_measured_fraction_theta_max 0.892 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.466 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.080 _database_code_depnum_ccdc_archive 'CCDC 941395' ####################################################################### # # 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_ba2_k_formii_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common KBA_BA0.5_1.5H2O _chemical_melting_point ? _chemical_formula_moiety 'K C4 H3 N2 O3, (C4 H4 N2 O3)0.5, (H2 O)1.5' _chemical_formula_sum 'C12 H16 K2 N6 O12' _chemical_formula_weight 514.51 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 14.686(5) _cell_length_b 16.190(2) _cell_length_c 10.926(3) _cell_angle_alpha 90.00 _cell_angle_beta 131.41(5) _cell_angle_gamma 90.00 _cell_volume 1948.4(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2309 _cell_measurement_theta_min 2.7685 _cell_measurement_theta_max 29.2373 _exptl_crystal_description prism _exptl_crystal_colour 'light pink' _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 0.566 _exptl_absorpt_correction_T_min 0.76684 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.1340 _diffrn_measurement_method '\w scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7363 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 29.30 _reflns_number_total 2407 _reflns_number_gt 1772 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0816P)^2^+4.3100P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2407 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1649 _refine_ls_wR_factor_gt 0.1382 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _refine_ls_shift/su_max 0.000 _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 K1 K 0.02894(8) 0.0000 0.36834(10) 0.0338(3) Uani 1 2 d S . . K2 K -0.32529(10) 0.0000 0.14065(16) 0.0684(5) Uani 1 2 d S . . O8 O -0.1623(3) 0.0000 0.0442(4) 0.0519(9) Uani 1 2 d S . . O7 O -0.4487(5) 0.0000 -0.1902(7) 0.102(2) Uani 1 2 d S . . O9 O 0.2701(4) 0.0000 0.5496(7) 0.0715(13) Uani 1 2 d S . . H130 H 0.050(3) 0.2874(19) 0.207(4) 0.034(8) Uiso 1 1 d . . . H900 H 0.313(4) 0.037(3) 0.562(6) 0.090(17) Uiso 1 1 d . . . H300 H -0.109(3) 0.202(2) 0.544(4) 0.037(9) Uiso 1 1 d . . . H100 H -0.207(3) 0.206(2) 0.131(4) 0.045(10) Uiso 1 1 d . . . H800 H -0.210(4) -0.046(3) -0.007(6) 0.090(16) Uiso 1 1 d . . . H700 H -0.474(10) -0.055(5) -0.240(14) 0.29(6) Uiso 1 1 d . . . O6 O -0.2339(3) 0.34844(13) 0.0706(3) 0.0520(7) Uani 1 1 d . . . O4 O -0.1089(2) 0.34729(12) 0.5950(2) 0.0390(5) Uani 1 1 d . . . O2 O -0.14262(19) 0.10998(12) 0.3473(2) 0.0364(5) Uani 1 1 d . . . N3 N -0.1295(2) 0.23062(14) 0.4646(3) 0.0303(5) Uani 1 1 d . . . N1 N -0.1882(2) 0.23070(14) 0.2113(3) 0.0308(5) Uani 1 1 d . . . C2 C -0.1530(2) 0.18582(17) 0.3413(3) 0.0264(5) Uani 1 1 d . . . C5 C -0.1707(3) 0.35828(18) 0.3330(3) 0.0349(7) Uani 1 1 d . . . H5 H -0.1756 0.4156 0.3303 0.042 Uiso 1 1 calc R . . C4 C -0.1352(2) 0.31602(17) 0.4696(3) 0.0288(6) Uani 1 1 d . . . C6 C -0.1990(3) 0.31625(16) 0.2005(3) 0.0316(6) Uani 1 1 d . . . O14 O 0.0560(2) 0.14119(12) 0.2584(2) 0.0405(5) Uani 1 1 d . . . O12 O 0.0000 0.37773(17) 0.0000 0.0399(7) Uani 1 2 d S . . N13 N 0.0315(2) 0.25875(14) 0.1304(3) 0.0318(5) Uani 1 1 d . . . C14 C 0.0315(2) 0.17502(16) 0.1400(3) 0.0293(6) Uani 1 1 d . . . C12 C 0.0000 0.3031(2) 0.0000 0.0275(8) Uani 1 2 d S . . C15 C 0.0000 0.1263(2) 0.0000 0.0304(8) Uani 1 2 d S . . H15A H -0.0683 0.0908 -0.0412 0.036 Uiso 0.50 1 calc PR . . H15B H 0.0683 0.0908 0.0412 0.036 Uiso 0.50 1 calc PR . . 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 K1 0.0455(5) 0.0251(4) 0.0306(5) 0.000 0.0252(4) 0.000 K2 0.0406(6) 0.0317(6) 0.0612(8) 0.000 0.0032(5) 0.000 O8 0.050(2) 0.0304(17) 0.0413(19) 0.000 0.0157(16) 0.000 O7 0.082(3) 0.054(3) 0.078(3) 0.000 0.013(3) 0.000 O9 0.063(3) 0.040(2) 0.120(4) 0.000 0.064(3) 0.000 O6 0.0972(19) 0.0298(11) 0.0294(12) 0.0086(9) 0.0421(14) 0.0149(11) O4 0.0611(14) 0.0312(11) 0.0274(11) -0.0002(8) 0.0305(11) 0.0067(9) O2 0.0527(12) 0.0218(10) 0.0323(11) 0.0008(8) 0.0271(10) 0.0011(8) N3 0.0431(13) 0.0254(12) 0.0220(12) 0.0032(9) 0.0214(11) 0.0026(9) N1 0.0464(14) 0.0226(12) 0.0209(12) 0.0001(9) 0.0212(11) 0.0045(10) C2 0.0299(12) 0.0259(13) 0.0193(13) 0.0006(9) 0.0144(11) -0.0001(10) C5 0.0559(18) 0.0227(13) 0.0269(15) 0.0026(10) 0.0277(15) 0.0055(12) C4 0.0344(13) 0.0290(14) 0.0229(13) -0.0018(10) 0.0189(12) 0.0026(11) C6 0.0440(15) 0.0242(13) 0.0245(14) 0.0047(10) 0.0218(13) 0.0056(11) O14 0.0665(14) 0.0314(11) 0.0290(11) 0.0009(8) 0.0339(11) -0.0040(10) O12 0.0609(19) 0.0242(14) 0.0338(16) 0.000 0.0309(16) 0.000 N13 0.0483(14) 0.0253(12) 0.0244(12) -0.0021(9) 0.0252(12) -0.0011(10) C14 0.0381(14) 0.0280(14) 0.0244(13) -0.0006(10) 0.0217(12) -0.0025(11) C12 0.0331(18) 0.0264(18) 0.0232(18) 0.000 0.0187(16) 0.000 C15 0.045(2) 0.0242(18) 0.0257(19) 0.000 0.0247(18) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 K1 O9 2.681(5) . ? K1 O8 2.697(4) . ? K1 O14 2.731(2) 6 ? K1 O14 2.731(2) . ? K1 O2 2.958(2) 2_556 ? K1 O2 2.958(2) 5_556 ? K1 O2 2.967(2) 6 ? K1 O2 2.967(2) . ? K1 K1 3.498(2) 5_556 ? K1 K2 4.017(3) . ? K1 K2 4.103(4) 5_556 ? K2 O2 2.730(3) . ? K2 O2 2.730(3) 6 ? K2 O12 2.765(2) 3_445 ? K2 O12 2.765(2) 7_455 ? K2 O7 2.773(7) . ? K2 O9 2.912(6) 5_556 ? K2 O8 3.190(5) . ? K2 K2 3.862(4) 5_455 ? K2 K1 4.103(4) 5_556 ? O9 K2 2.912(6) 5_556 ? O6 C6 1.260(3) . ? O4 C4 1.258(3) . ? O2 C2 1.234(3) . ? O2 K1 2.958(2) 5_556 ? N3 C2 1.358(3) . ? N3 C4 1.388(3) . ? N1 C2 1.357(3) . ? N1 C6 1.390(3) . ? C5 C6 1.391(4) . ? C5 C4 1.392(4) . ? O14 C14 1.220(3) . ? O12 C12 1.208(5) . ? O12 K2 2.765(2) 3 ? O12 K2 2.765(2) 7_455 ? N13 C14 1.360(3) . ? N13 C12 1.374(3) . ? C14 C15 1.497(3) . ? C12 N13 1.374(3) 2 ? C15 C14 1.497(3) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 K1 O8 133.60(16) . . ? O9 K1 O14 79.60(9) . 6 ? O8 K1 O14 75.56(7) . 6 ? O9 K1 O14 79.60(9) . . ? O8 K1 O14 75.56(7) . . ? O14 K1 O14 113.67(9) 6 . ? O9 K1 O2 70.86(11) . 2_556 ? O8 K1 O2 138.89(6) . 2_556 ? O14 K1 O2 145.15(7) 6 2_556 ? O14 K1 O2 79.22(6) . 2_556 ? O9 K1 O2 70.86(11) . 5_556 ? O8 K1 O2 138.89(6) . 5_556 ? O14 K1 O2 79.22(6) 6 5_556 ? O14 K1 O2 145.15(7) . 5_556 ? O2 K1 O2 74.02(9) 2_556 5_556 ? O9 K1 O2 134.14(8) . 6 ? O8 K1 O2 78.74(9) . 6 ? O14 K1 O2 80.02(6) 6 6 ? O14 K1 O2 146.24(7) . 6 ? O2 K1 O2 107.64(6) 2_556 6 ? O2 K1 O2 65.20(9) 5_556 6 ? O9 K1 O2 134.14(8) . . ? O8 K1 O2 78.74(9) . . ? O14 K1 O2 146.24(7) 6 . ? O14 K1 O2 80.02(6) . . ? O2 K1 O2 65.20(9) 2_556 . ? O2 K1 O2 107.64(6) 5_556 . ? O2 K1 O2 73.75(8) 6 . ? O9 K1 K1 108.26(13) . 5_556 ? O8 K1 K1 118.13(10) . 5_556 ? O14 K1 K1 123.16(5) 6 5_556 ? O14 K1 K1 123.16(5) . 5_556 ? O2 K1 K1 53.94(5) 2_556 5_556 ? O2 K1 K1 53.94(5) 5_556 5_556 ? O2 K1 K1 53.70(5) 6 5_556 ? O2 K1 K1 53.70(5) . 5_556 ? O9 K1 K2 174.03(12) . . ? O8 K1 K2 52.36(10) . . ? O14 K1 K2 103.49(6) 6 . ? O14 K1 K2 103.49(6) . . ? O2 K1 K2 104.50(7) 2_556 . ? O2 K1 K2 104.50(7) 5_556 . ? O2 K1 K2 42.82(4) 6 . ? O2 K1 K2 42.82(4) . . ? K1 K1 K2 65.77(6) 5_556 . ? O9 K1 K2 45.06(13) . 5_556 ? O8 K1 K2 178.66(10) . 5_556 ? O14 K1 K2 103.77(5) 6 5_556 ? O14 K1 K2 103.77(5) . 5_556 ? O2 K1 K2 41.67(5) 2_556 5_556 ? O2 K1 K2 41.67(5) 5_556 5_556 ? O2 K1 K2 102.32(6) 6 5_556 ? O2 K1 K2 102.32(6) . 5_556 ? K1 K1 K2 63.21(5) 5_556 5_556 ? K2 K1 K2 128.98(6) . 5_556 ? O2 K2 O2 81.42(10) . 6 ? O2 K2 O12 165.82(8) . 3_445 ? O2 K2 O12 92.05(8) 6 3_445 ? O2 K2 O12 92.05(8) . 7_455 ? O2 K2 O12 165.82(8) 6 7_455 ? O12 K2 O12 91.42(10) 3_445 7_455 ? O2 K2 O7 121.02(12) . . ? O2 K2 O7 121.02(12) 6 . ? O12 K2 O7 73.11(11) 3_445 . ? O12 K2 O7 73.11(11) 7_455 . ? O2 K2 O9 70.93(9) . 5_556 ? O2 K2 O9 70.93(9) 6 5_556 ? O12 K2 O9 95.07(8) 3_445 5_556 ? O12 K2 O9 95.07(8) 7_455 5_556 ? O7 K2 O9 162.69(17) . 5_556 ? O2 K2 O8 74.42(7) . . ? O2 K2 O8 74.42(7) 6 . ? O12 K2 O8 116.07(6) 3_445 . ? O12 K2 O8 116.07(6) 7_455 . ? O7 K2 O8 63.59(16) . . ? O9 K2 O8 133.72(12) 5_556 . ? O2 K2 K2 136.04(6) . 5_455 ? O2 K2 K2 136.04(6) 6 5_455 ? O12 K2 K2 45.71(5) 3_445 5_455 ? O12 K2 K2 45.71(5) 7_455 5_455 ? O7 K2 K2 65.42(16) . 5_455 ? O9 K2 K2 97.28(12) 5_556 5_455 ? O8 K2 K2 129.01(9) . 5_455 ? O2 K2 K1 47.62(6) . . ? O2 K2 K1 47.62(6) 6 . ? O12 K2 K1 133.61(5) 3_445 . ? O12 K2 K1 133.61(5) 7_455 . ? O7 K2 K1 105.61(16) . . ? O9 K2 K1 91.69(11) 5_556 . ? O8 K2 K1 42.02(7) . . ? K2 K2 K1 171.03(7) 5_455 . ? O2 K2 K1 46.09(6) . 5_556 ? O2 K2 K1 46.09(6) 6 5_556 ? O12 K2 K1 121.23(6) 3_445 5_556 ? O12 K2 K1 121.23(6) 7_455 5_556 ? O7 K2 K1 156.64(15) . 5_556 ? O9 K2 K1 40.67(9) 5_556 5_556 ? O8 K2 K1 93.05(8) . 5_556 ? K2 K2 K1 137.94(8) 5_455 5_556 ? K1 K2 K1 51.02(6) . 5_556 ? K1 O8 K2 85.61(12) . . ? K1 O9 K2 94.27(15) . 5_556 ? C2 O2 K2 125.86(17) . . ? C2 O2 K1 128.22(16) . 5_556 ? K2 O2 K1 92.24(8) . 5_556 ? C2 O2 K1 132.11(18) . . ? K2 O2 K1 89.56(7) . . ? K1 O2 K1 72.36(6) 5_556 . ? C2 N3 C4 126.0(2) . . ? C2 N1 C6 124.4(2) . . ? O2 C2 N1 122.4(2) . . ? O2 C2 N3 122.5(2) . . ? N1 C2 N3 115.0(2) . . ? C6 C5 C4 121.2(3) . . ? O4 C4 N3 117.4(2) . . ? O4 C4 C5 126.7(3) . . ? N3 C4 C5 115.9(2) . . ? O6 C6 N1 116.5(2) . . ? O6 C6 C5 126.1(3) . . ? N1 C6 C5 117.4(2) . . ? C14 O14 K1 144.67(19) . . ? C12 O12 K2 135.71(5) . 3 ? C12 O12 K2 135.71(5) . 7_455 ? K2 O12 K2 88.58(10) 3 7_455 ? C14 N13 C12 125.7(2) . . ? O14 C14 N13 121.0(2) . . ? O14 C14 C15 121.5(2) . . ? N13 C14 C15 117.6(2) . . ? O12 C12 N13 121.51(16) . 2 ? O12 C12 N13 121.51(16) . . ? N13 C12 N13 117.0(3) 2 . ? C14 C15 C14 116.3(3) . 2 ? _diffrn_measured_fraction_theta_max 0.873 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.868 _refine_diff_density_min -1.299 _refine_diff_density_rms 0.077 _database_code_depnum_ccdc_archive 'CCDC 941396' ####################################################################### # # 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_move_BA_KBA_2H2O _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common BA_KBA_2H2O _chemical_melting_point ? _chemical_formula_moiety 'K1 C4 H3 N2 O3, C4 H4 N2 O3,2(H2 O)' _chemical_formula_sum 'C8 H11 K N4 O8' _chemical_formula_weight 330.31 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' _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 51.935(7) _cell_length_b 11.828(3) _cell_length_c 12.781(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.880(10) _cell_angle_gamma 90.00 _cell_volume 7847(3) _cell_formula_units_Z 24 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2968 _cell_measurement_theta_min 2.7413 _cell_measurement_theta_max 28.9282 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4080 _exptl_absorpt_coefficient_mu 0.455 _exptl_absorpt_correction_T_min 0.49095 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.1340 _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30072 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -64 _diffrn_reflns_limit_h_max 66 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 28.99 _reflns_number_total 9044 _reflns_number_gt 7422 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0855P)^2^+18.4059P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9044 _refine_ls_number_parameters 617 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1791 _refine_ls_wR_factor_gt 0.1687 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.085 _refine_ls_shift/su_mean 0.003 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 N1 N 0.24357(4) 0.95681(18) 0.38841(18) 0.0241(5) Uani 1 1 d . . . H1 H 0.2522 0.8948 0.3871 0.029 Uiso 1 1 calc R . . O6 O 0.20680(4) 0.85681(16) 0.39079(18) 0.0345(5) Uani 1 1 d . . . O2 O 0.28042(4) 1.05783(18) 0.37981(18) 0.0345(5) Uani 1 1 d . . . N3 N 0.24312(4) 1.15536(19) 0.39035(19) 0.0271(5) Uani 1 1 d . . . H3 H 0.2515 1.2179 0.3882 0.033 Uiso 1 1 calc R . . C2 C 0.25730(5) 1.0567(2) 0.3857(2) 0.0236(5) Uani 1 1 d . . . C4 C 0.21719(5) 1.1627(2) 0.3980(2) 0.0275(6) Uani 1 1 d . . . O4 O 0.20623(4) 1.25379(17) 0.4016(2) 0.0421(6) Uani 1 1 d . . . C6 C 0.21754(5) 0.9483(2) 0.3929(2) 0.0239(5) Uani 1 1 d . . . C5 C 0.20246(5) 1.0547(2) 0.4010(2) 0.0268(6) Uani 1 1 d . . . H5A H 0.1933 1.0526 0.4660 0.032 Uiso 1 1 calc R . . H5B H 0.1896 1.0558 0.3443 0.032 Uiso 1 1 calc R . . N13 N 0.23308(4) 0.45531(19) 0.36310(19) 0.0262(5) Uani 1 1 d . . . H13 H 0.2247 0.3925 0.3614 0.031 Uiso 1 1 calc R . . O16 O 0.26998(4) 0.75085(16) 0.36975(19) 0.0360(5) Uani 1 1 d . . . O12 O 0.19551(4) 0.55102(17) 0.37581(19) 0.0353(5) Uani 1 1 d . . . N11 N 0.23316(4) 0.64835(19) 0.3709(2) 0.0283(5) Uani 1 1 d . . . H11 H 0.2248 0.7110 0.3748 0.034 Uiso 1 1 calc R . . C14 C 0.25981(5) 0.4498(2) 0.3587(2) 0.0229(5) Uani 1 1 d . . . C16 C 0.26001(5) 0.6545(2) 0.3660(2) 0.0244(5) Uani 1 1 d . . . C12 C 0.21927(5) 0.5517(2) 0.3698(2) 0.0253(5) Uani 1 1 d . . . O14 O 0.26962(4) 0.35246(16) 0.35646(18) 0.0326(5) Uani 1 1 d . . . C15 C 0.27296(5) 0.5516(2) 0.3574(2) 0.0242(5) Uani 1 1 d . . . H15 H 0.2907 0.5515 0.3505 0.029 Uiso 1 1 calc R . . O26 O 0.04305(4) 0.51619(17) 0.22833(18) 0.0353(5) Uani 1 1 d . . . O22 O 0.11771(4) 0.71098(18) 0.22188(19) 0.0393(5) Uani 1 1 d . . . N21 N 0.08020(4) 0.61341(19) 0.22706(19) 0.0268(5) Uani 1 1 d . . . H21 H 0.0886 0.5508 0.2292 0.032 Uiso 1 1 calc R . . O24 O 0.04435(4) 0.91294(18) 0.2344(2) 0.0506(7) Uani 1 1 d . . . C26 C 0.05412(5) 0.6068(2) 0.2271(2) 0.0259(5) Uani 1 1 d . . . C22 C 0.09440(5) 0.7118(2) 0.2238(2) 0.0258(5) Uani 1 1 d . . . N23 N 0.08079(4) 0.8120(2) 0.2240(2) 0.0296(5) Uani 1 1 d . . . H23 H 0.0895 0.8737 0.2209 0.035 Uiso 1 1 calc R . . C24 C 0.05463(5) 0.8214(2) 0.2287(2) 0.0297(6) Uani 1 1 d . . . C25 C 0.03937(5) 0.7149(2) 0.2266(3) 0.0321(6) Uani 1 1 d . . . H25A H 0.0281 0.7160 0.1645 0.039 Uiso 1 1 calc R . . H25B H 0.0285 0.7149 0.2867 0.039 Uiso 1 1 calc R . . O34 O 0.06150(4) 0.37689(16) 0.48943(18) 0.0340(5) Uani 1 1 d . . . N31 N 0.09926(4) 0.66878(19) 0.46876(18) 0.0257(5) Uani 1 1 d . . . H31 H 0.1078 0.7307 0.4645 0.031 Uiso 1 1 calc R . . O36 O 0.06329(4) 0.77533(16) 0.47300(19) 0.0355(5) Uani 1 1 d . . . O32 O 0.13616(4) 0.56738(17) 0.45975(19) 0.0368(5) Uani 1 1 d . . . N33 N 0.09825(4) 0.47577(19) 0.4749(2) 0.0284(5) Uani 1 1 d . . . H33 H 0.1061 0.4119 0.4737 0.034 Uiso 1 1 calc R . . C36 C 0.07269(5) 0.6771(2) 0.4763(2) 0.0251(5) Uani 1 1 d . . . C34 C 0.07181(5) 0.4735(2) 0.4840(2) 0.0245(5) Uani 1 1 d . . . C32 C 0.11275(5) 0.5705(2) 0.4677(2) 0.0258(5) Uani 1 1 d . . . C35 C 0.05905(5) 0.5768(2) 0.4856(2) 0.0270(6) Uani 1 1 d . . . H35 H 0.0413 0.5788 0.4929 0.032 Uiso 1 1 calc R . . N41 N 0.08974(4) 0.17518(19) 0.47049(19) 0.0285(5) Uani 1 1 d . . . H41 H 0.0812 0.2372 0.4760 0.034 Uiso 1 1 calc R . . O46 O 0.12678(4) 0.27406(17) 0.46911(19) 0.0370(5) Uani 1 1 d . . . O44 O 0.12583(4) -0.12156(17) 0.4373(2) 0.0416(5) Uani 1 1 d . . . N43 N 0.08924(4) -0.02260(19) 0.4551(2) 0.0286(5) Uani 1 1 d . . . H43 H 0.0805 -0.0844 0.4514 0.034 Uiso 1 1 calc R . . C46 C 0.11583(5) 0.1838(2) 0.4643(2) 0.0267(6) Uani 1 1 d . . . O42 O 0.05283(4) 0.0763(2) 0.4780(2) 0.0461(6) Uani 1 1 d . . . C42 C 0.07573(5) 0.0756(2) 0.4687(2) 0.0286(6) Uani 1 1 d . . . C44 C 0.11527(5) -0.0306(2) 0.4471(2) 0.0280(6) Uani 1 1 d . . . C45 C 0.13049(5) 0.0762(2) 0.4506(3) 0.0298(6) Uani 1 1 d . . . H45A H 0.1398 0.0818 0.3862 0.036 Uiso 1 1 calc R . . H45B H 0.1432 0.0704 0.5076 0.036 Uiso 1 1 calc R . . O54 O 0.10829(4) 0.01596(16) 0.20013(18) 0.0352(5) Uani 1 1 d . . . O56 O 0.10795(4) 0.41428(16) 0.22274(18) 0.0344(5) Uani 1 1 d . . . O52 O 0.03436(4) 0.21148(19) 0.2347(2) 0.0492(6) Uani 1 1 d . . . C54 C 0.09823(5) 0.1133(2) 0.2081(2) 0.0257(5) Uani 1 1 d . . . N51 N 0.07177(4) 0.30999(19) 0.2310(2) 0.0292(5) Uani 1 1 d . . . H51 H 0.0635 0.3721 0.2401 0.035 Uiso 1 1 calc R . . C56 C 0.09822(5) 0.3173(2) 0.2210(2) 0.0255(5) Uani 1 1 d . . . C52 C 0.05776(5) 0.2125(2) 0.2276(2) 0.0299(6) Uani 1 1 d . . . N53 N 0.07181(4) 0.11697(19) 0.2176(2) 0.0290(5) Uani 1 1 d . . . H53 H 0.0637 0.0536 0.2171 0.035 Uiso 1 1 calc R . . C55 C 0.11143(5) 0.2157(2) 0.2095(2) 0.0279(6) Uani 1 1 d . . . H55 H 0.1292 0.2163 0.2027 0.033 Uiso 1 1 calc R . . K1 K 0.171438(12) 0.60071(6) 0.03262(6) 0.03951(19) Uani 1 1 d . . . K2 K 0.162522(12) 0.73297(6) 0.36421(6) 0.03686(19) Uani 1 1 d . . . K3 K 0.0000 0.38133(8) 0.2500 0.0391(2) Uani 1 2 d S . . K4 K 0.00421(2) 1.03533(11) 0.34615(13) 0.0388(3) Uani 0.50 1 d P . . O100 O 0.32136(4) 0.2988(2) 0.3415(2) 0.0489(6) Uani 1 1 d D . . O500 O 0.00884(4) 0.3901(2) 0.4676(2) 0.0535(7) Uani 1 1 d D . . O200 O 0.32386(5) 0.7467(2) 0.4033(3) 0.0561(7) Uani 1 1 d D . . O400 O 0.16083(5) 0.4586(3) 0.2004(2) 0.0555(7) Uani 1 1 d D . . O300 O 0.16055(5) 0.0284(2) 0.1787(3) 0.0554(7) Uani 1 1 d D . . O600 O 0.01106(5) 0.8195(3) 0.4697(3) 0.0711(9) Uani 1 1 d D . . H101 H 0.3030(4) 0.309(5) 0.350(5) 0.108(19) Uiso 1 1 d D . . H102 H 0.3246(12) 0.379(3) 0.326(7) 0.20(4) Uiso 1 1 d D . . H201 H 0.3046(4) 0.746(5) 0.409(5) 0.11(2) Uiso 1 1 d D . . H202 H 0.3224(13) 0.799(7) 0.342(5) 0.22(4) Uiso 1 1 d D . . H301 H 0.1421(4) 0.024(3) 0.178(3) 0.068(13) Uiso 1 1 d D . . H302 H 0.1626(8) 0.097(3) 0.142(4) 0.085(16) Uiso 1 1 d D . . H401 H 0.1693(9) 0.486(5) 0.264(3) 0.12(2) Uiso 1 1 d D . . H402 H 0.1435(5) 0.454(5) 0.224(4) 0.105(19) Uiso 1 1 d D . . H501 H 0.0271(4) 0.392(4) 0.477(3) 0.063(13) Uiso 1 1 d D . . H601 H 0.0293(5) 0.808(6) 0.484(5) 0.15(3) Uiso 1 1 d D . . H602 H 0.0099(10) 0.769(4) 0.410(3) 0.10(2) Uiso 1 1 d 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 N1 0.0229(11) 0.0177(10) 0.0317(12) -0.0007(9) 0.0024(9) 0.0014(8) O6 0.0272(10) 0.0217(10) 0.0547(13) -0.0020(9) 0.0039(9) -0.0046(8) O2 0.0204(9) 0.0331(11) 0.0502(13) -0.0033(10) 0.0039(8) -0.0022(8) N3 0.0238(11) 0.0195(11) 0.0383(13) -0.0022(10) 0.0032(9) -0.0037(9) C2 0.0227(12) 0.0236(13) 0.0245(13) -0.0001(10) 0.0005(10) -0.0010(10) C4 0.0258(13) 0.0209(13) 0.0361(15) -0.0004(11) 0.0036(11) -0.0001(10) O4 0.0310(11) 0.0211(10) 0.0750(17) 0.0026(10) 0.0117(11) 0.0031(8) C6 0.0240(12) 0.0212(12) 0.0266(13) -0.0003(10) 0.0001(10) -0.0017(10) C5 0.0205(12) 0.0227(13) 0.0372(15) -0.0002(11) 0.0022(10) -0.0005(10) N13 0.0187(10) 0.0187(10) 0.0415(13) -0.0010(10) 0.0059(9) -0.0008(8) O16 0.0231(10) 0.0203(10) 0.0645(15) -0.0035(10) 0.0018(9) -0.0035(8) O12 0.0186(9) 0.0258(10) 0.0617(14) -0.0023(10) 0.0056(9) 0.0007(8) N11 0.0199(11) 0.0188(11) 0.0463(14) -0.0033(10) 0.0016(9) 0.0028(8) C14 0.0212(12) 0.0222(12) 0.0254(13) 0.0015(10) 0.0037(10) 0.0019(9) C16 0.0230(12) 0.0225(13) 0.0277(13) -0.0006(11) 0.0021(10) -0.0013(10) C12 0.0198(12) 0.0224(13) 0.0337(14) -0.0004(11) 0.0013(10) 0.0004(10) O14 0.0233(9) 0.0204(9) 0.0547(13) 0.0021(9) 0.0092(9) 0.0028(7) C15 0.0175(11) 0.0239(13) 0.0313(14) -0.0010(11) 0.0027(10) 0.0010(10) O26 0.0289(10) 0.0222(10) 0.0550(13) -0.0024(9) 0.0023(9) -0.0041(8) O22 0.0213(10) 0.0355(12) 0.0613(15) -0.0003(11) 0.0056(9) -0.0023(8) N21 0.0231(11) 0.0194(11) 0.0379(13) -0.0020(10) 0.0021(9) 0.0025(9) O24 0.0323(12) 0.0215(11) 0.099(2) -0.0009(12) 0.0147(12) 0.0026(9) C26 0.0264(13) 0.0210(13) 0.0302(14) -0.0035(11) -0.0002(10) -0.0021(10) C22 0.0248(13) 0.0238(13) 0.0289(13) -0.0006(11) 0.0035(10) -0.0001(10) N23 0.0249(11) 0.0203(11) 0.0439(14) -0.0009(10) 0.0064(10) -0.0036(9) C24 0.0263(13) 0.0235(13) 0.0396(16) -0.0015(12) 0.0061(11) -0.0006(11) C25 0.0236(13) 0.0239(14) 0.0489(18) -0.0046(13) 0.0010(12) 0.0005(11) O34 0.0268(10) 0.0192(9) 0.0564(13) -0.0027(9) 0.0071(9) -0.0045(8) N31 0.0236(11) 0.0170(10) 0.0368(13) 0.0009(9) 0.0034(9) -0.0039(8) O36 0.0262(10) 0.0206(10) 0.0602(14) 0.0039(9) 0.0070(9) 0.0021(8) O32 0.0218(10) 0.0266(10) 0.0623(14) 0.0055(10) 0.0054(9) -0.0014(8) N33 0.0232(11) 0.0164(11) 0.0459(14) -0.0003(10) 0.0045(10) -0.0009(8) C36 0.0244(12) 0.0222(13) 0.0288(13) 0.0008(11) 0.0025(10) 0.0009(10) C34 0.0215(12) 0.0231(13) 0.0291(13) -0.0015(11) 0.0027(10) -0.0014(10) C32 0.0233(12) 0.0226(13) 0.0317(14) 0.0027(11) 0.0021(10) -0.0012(10) C35 0.0214(12) 0.0226(13) 0.0373(15) 0.0004(11) 0.0049(11) -0.0011(10) N41 0.0234(11) 0.0198(11) 0.0424(14) -0.0025(10) 0.0037(9) 0.0036(9) O46 0.0314(11) 0.0209(10) 0.0587(14) -0.0040(9) 0.0003(10) -0.0032(8) O44 0.0325(11) 0.0216(10) 0.0710(16) 0.0009(10) 0.0071(10) 0.0045(8) N43 0.0247(11) 0.0180(11) 0.0433(14) -0.0017(10) 0.0023(10) -0.0027(9) C46 0.0269(13) 0.0217(13) 0.0314(14) -0.0003(11) -0.0017(10) 0.0003(10) O42 0.0255(11) 0.0365(12) 0.0770(17) -0.0009(12) 0.0110(11) -0.0002(9) C42 0.0251(13) 0.0266(14) 0.0343(15) 0.0009(12) 0.0022(11) -0.0003(11) C44 0.0277(13) 0.0198(13) 0.0364(15) 0.0028(11) 0.0002(11) 0.0012(10) C45 0.0216(12) 0.0216(13) 0.0460(17) 0.0009(12) 0.0001(11) 0.0020(10) O54 0.0273(10) 0.0188(9) 0.0600(14) 0.0028(9) 0.0088(9) 0.0019(8) O56 0.0266(10) 0.0195(9) 0.0573(14) -0.0020(9) 0.0055(9) -0.0025(8) O52 0.0240(11) 0.0271(11) 0.097(2) 0.0020(12) 0.0108(11) 0.0008(9) C54 0.0239(13) 0.0222(13) 0.0312(14) 0.0030(11) 0.0038(10) 0.0026(10) N51 0.0236(11) 0.0176(11) 0.0467(14) 0.0012(10) 0.0056(10) 0.0026(9) C56 0.0251(13) 0.0226(13) 0.0290(13) 0.0011(11) 0.0023(10) -0.0017(10) C52 0.0237(13) 0.0211(13) 0.0450(17) 0.0031(12) 0.0042(11) 0.0002(10) N53 0.0221(11) 0.0175(11) 0.0474(14) 0.0019(10) 0.0033(10) -0.0019(8) C55 0.0185(12) 0.0232(13) 0.0422(16) 0.0019(12) 0.0042(11) -0.0006(10) K1 0.0265(3) 0.0362(4) 0.0555(4) -0.0026(3) -0.0031(3) 0.0005(3) K2 0.0221(3) 0.0279(3) 0.0610(5) 0.0045(3) 0.0076(3) -0.0005(2) K3 0.0239(4) 0.0291(5) 0.0646(7) 0.000 0.0061(4) 0.000 K4 0.0211(6) 0.0282(6) 0.0670(9) -0.0090(6) 0.0018(6) 0.0020(5) O100 0.0294(12) 0.0518(15) 0.0658(16) 0.0106(13) 0.0065(11) 0.0067(11) O500 0.0273(12) 0.0522(15) 0.0810(19) -0.0037(14) 0.0017(12) -0.0038(11) O200 0.0350(13) 0.0503(16) 0.083(2) 0.0052(14) 0.0037(13) -0.0036(11) O400 0.0338(13) 0.0726(19) 0.0604(17) -0.0017(14) 0.0051(12) -0.0054(13) O300 0.0294(12) 0.0458(15) 0.091(2) 0.0013(15) 0.0001(12) 0.0082(11) O600 0.0360(15) 0.078(2) 0.100(3) 0.018(2) 0.0049(15) 0.0016(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 C6 1.358(3) . ? N1 C2 1.381(3) . ? O6 C6 1.217(3) . ? O6 K2 2.738(2) . ? O2 C2 1.206(3) . ? O2 K1 2.753(2) 4 ? N3 C4 1.357(3) . ? N3 C2 1.382(3) . ? C4 O4 1.220(3) . ? C4 C5 1.490(4) . ? O4 K1 3.038(2) 6_576 ? C6 C5 1.488(4) . ? N13 C12 1.351(3) . ? N13 C14 1.393(3) . ? O16 C16 1.252(3) . ? O12 C12 1.239(3) . ? O12 K2 2.752(2) . ? O12 K1 2.994(2) 6_566 ? N11 C12 1.352(3) . ? N11 C16 1.400(3) . ? C14 O14 1.259(3) . ? C14 C15 1.385(4) . ? C16 C15 1.397(4) . ? O26 C26 1.217(3) . ? O26 K3 2.768(2) . ? O22 C22 1.211(3) . ? O22 K2 2.918(2) . ? N21 C26 1.357(3) . ? N21 C22 1.379(3) . ? O24 C24 1.211(3) . ? O24 K4 2.945(3) . ? O24 K4 3.057(3) 2 ? C26 C25 1.490(4) . ? C22 N23 1.380(3) . ? N23 C24 1.367(3) . ? C24 C25 1.488(4) . ? O34 C34 1.265(3) . ? N31 C32 1.358(3) . ? N31 C36 1.390(3) . ? O36 C36 1.261(3) . ? O32 C32 1.223(3) . ? O32 K2 2.704(2) . ? O32 K1 2.840(2) 6_566 ? N33 C32 1.355(3) . ? N33 C34 1.382(3) . ? C36 C35 1.389(4) . ? C34 C35 1.391(4) . ? C32 K2 3.514(3) . ? N41 C46 1.364(3) . ? N41 C42 1.384(4) . ? O46 C46 1.210(3) . ? O46 K1 2.847(2) 6_566 ? O44 C44 1.216(3) . ? O44 K2 2.754(2) 1_545 ? N43 C44 1.362(3) . ? N43 C42 1.371(4) . ? C46 C45 1.496(4) . ? O42 C42 1.199(3) . ? O42 K4 3.028(3) 1_545 ? C44 C45 1.490(4) . ? O54 C54 1.270(3) . ? O56 C56 1.254(3) . ? O52 C52 1.222(3) . ? O52 K3 2.698(2) . ? O52 K4 2.995(3) 1_545 ? O52 K4 3.047(3) 2_545 ? C54 N53 1.382(3) . ? C54 C55 1.391(4) . ? N51 C52 1.364(4) . ? N51 C56 1.386(3) . ? C56 C55 1.394(4) . ? C52 N53 1.353(3) . ? K1 O2 2.753(2) 4_545 ? K1 O400 2.794(3) . ? K1 O32 2.840(2) 6_565 ? K1 O46 2.847(2) 6_565 ? K1 O100 2.860(3) 4 ? K1 O12 2.994(2) 6_565 ? K1 O4 3.038(2) 6_575 ? K1 K2 4.5121(13) 6_565 ? K1 K2 4.5554(14) . ? K2 O44 2.754(2) 1_565 ? K2 O100 2.893(3) 4 ? K2 O200 3.041(3) 7_566 ? K2 K1 4.5121(13) 6_566 ? K3 O52 2.698(2) 2 ? K3 O26 2.768(2) 2 ? K3 O500 2.806(3) 2 ? K3 O500 2.806(3) . ? K3 K4 4.2765(19) 2_545 ? K3 K4 4.2765(19) 1_545 ? K4 K4 2.482(3) 2 ? K4 O52 2.995(3) 1_565 ? K4 O600 3.016(4) . ? K4 O42 3.028(3) 1_565 ? K4 O600 3.040(4) 5_576 ? K4 O52 3.047(3) 2_565 ? K4 O24 3.057(3) 2 ? K4 K4 4.058(3) 5_576 ? K4 K3 4.2765(19) 1_565 ? O100 K1 2.860(3) 4_545 ? O100 K2 2.893(3) 4_545 ? O200 K2 3.041(3) 7_566 ? O600 K4 3.040(4) 5_576 ? 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 C6 N1 C2 125.5(2) . . ? C6 O6 K2 149.41(18) . . ? C2 O2 K1 150.41(19) . 4 ? C4 N3 C2 126.0(2) . . ? O2 C2 N1 121.8(2) . . ? O2 C2 N3 121.7(2) . . ? N1 C2 N3 116.4(2) . . ? O4 C4 N3 121.6(3) . . ? O4 C4 C5 121.0(2) . . ? N3 C4 C5 117.3(2) . . ? C4 O4 K1 143.9(2) . 6_576 ? O6 C6 N1 121.4(2) . . ? O6 C6 C5 120.8(2) . . ? N1 C6 C5 117.8(2) . . ? C6 C5 C4 116.8(2) . . ? C12 N13 C14 125.0(2) . . ? C12 O12 K2 127.69(18) . . ? C12 O12 K1 118.93(18) . 6_566 ? K2 O12 K1 103.41(7) . 6_566 ? C12 N11 C16 125.2(2) . . ? O14 C14 C15 126.5(2) . . ? O14 C14 N13 116.6(2) . . ? C15 C14 N13 116.9(2) . . ? O16 C16 C15 126.6(2) . . ? O16 C16 N11 117.2(2) . . ? C15 C16 N11 116.2(2) . . ? O12 C12 N13 122.1(2) . . ? O12 C12 N11 122.5(2) . . ? N13 C12 N11 115.5(2) . . ? C14 C15 C16 121.2(2) . . ? C26 O26 K3 153.21(19) . . ? C22 O22 K2 139.8(2) . . ? C26 N21 C22 125.7(2) . . ? C24 O24 K4 142.1(2) . . ? C24 O24 K4 139.8(2) . 2 ? K4 O24 K4 48.81(7) . 2 ? O26 C26 N21 121.5(3) . . ? O26 C26 C25 120.8(2) . . ? N21 C26 C25 117.6(2) . . ? O22 C22 N21 121.9(3) . . ? O22 C22 N23 121.3(3) . . ? N21 C22 N23 116.8(2) . . ? C24 N23 C22 125.5(2) . . ? O24 C24 N23 121.1(3) . . ? O24 C24 C25 121.5(3) . . ? N23 C24 C25 117.4(2) . . ? C24 C25 C26 116.9(2) . . ? C32 N31 C36 125.1(2) . . ? C32 O32 K2 122.33(18) . . ? C32 O32 K1 128.75(18) . 6_566 ? K2 O32 K1 108.92(7) . 6_566 ? C32 N33 C34 125.3(2) . . ? O36 C36 C35 126.3(2) . . ? O36 C36 N31 116.6(2) . . ? C35 C36 N31 117.1(2) . . ? O34 C34 N33 116.5(2) . . ? O34 C34 C35 126.2(2) . . ? N33 C34 C35 117.4(2) . . ? O32 C32 N33 122.5(3) . . ? O32 C32 N31 122.7(2) . . ? N33 C32 N31 114.8(2) . . ? O32 C32 K2 40.56(14) . . ? N33 C32 K2 153.55(19) . . ? N31 C32 K2 85.51(15) . . ? C36 C35 C34 120.3(2) . . ? C46 N41 C42 125.8(2) . . ? C46 O46 K1 148.25(19) . 6_566 ? C44 O44 K2 155.1(2) . 1_545 ? C44 N43 C42 125.6(2) . . ? O46 C46 N41 122.0(3) . . ? O46 C46 C45 121.1(3) . . ? N41 C46 C45 117.0(2) . . ? C42 O42 K4 139.0(2) . 1_545 ? O42 C42 N43 122.1(3) . . ? O42 C42 N41 121.0(3) . . ? N43 C42 N41 116.9(2) . . ? O44 C44 N43 121.4(3) . . ? O44 C44 C45 120.9(3) . . ? N43 C44 C45 117.8(2) . . ? C44 C45 C46 116.9(2) . . ? C52 O52 K3 131.29(19) . . ? C52 O52 K4 125.4(2) . 1_545 ? K3 O52 K4 97.25(7) . 1_545 ? C52 O52 K4 128.8(2) . 2_545 ? K3 O52 K4 96.01(7) . 2_545 ? K4 O52 K4 48.50(7) 1_545 2_545 ? O54 C54 N53 116.6(2) . . ? O54 C54 C55 125.9(2) . . ? N53 C54 C55 117.5(2) . . ? C52 N51 C56 125.4(2) . . ? O56 C56 N51 117.1(2) . . ? O56 C56 C55 126.2(2) . . ? N51 C56 C55 116.7(2) . . ? O52 C52 N53 122.7(3) . . ? O52 C52 N51 122.5(3) . . ? N53 C52 N51 114.8(2) . . ? C52 N53 C54 125.1(2) . . ? C54 C55 C56 120.5(2) . . ? O2 K1 O400 77.08(7) 4_545 . ? O2 K1 O32 124.89(7) 4_545 6_565 ? O400 K1 O32 71.90(8) . 6_565 ? O2 K1 O46 158.77(7) 4_545 6_565 ? O400 K1 O46 110.64(8) . 6_565 ? O32 K1 O46 76.11(6) 6_565 6_565 ? O2 K1 O100 79.75(7) 4_545 4 ? O400 K1 O100 94.97(9) . 4 ? O32 K1 O100 146.01(7) 6_565 4 ? O46 K1 O100 79.88(7) 6_565 4 ? O2 K1 O12 76.59(6) 4_545 6_565 ? O400 K1 O12 104.51(8) . 6_565 ? O32 K1 O12 68.90(6) 6_565 6_565 ? O46 K1 O12 118.36(7) 6_565 6_565 ? O100 K1 O12 144.87(6) 4 6_565 ? O2 K1 O4 77.28(7) 4_545 6_575 ? O400 K1 O4 154.13(8) . 6_575 ? O32 K1 O4 127.21(7) 6_565 6_575 ? O46 K1 O4 92.39(7) 6_565 6_575 ? O100 K1 O4 77.10(7) 4 6_575 ? O12 K1 O4 72.64(6) 6_565 6_575 ? O2 K1 K2 96.34(5) 4_545 6_565 ? O400 K1 K2 79.65(7) . 6_565 ? O32 K1 K2 34.53(4) 6_565 6_565 ? O46 K1 K2 104.43(5) 6_565 6_565 ? O100 K1 K2 174.00(6) 4 6_565 ? O12 K1 K2 36.39(4) 6_565 6_565 ? O4 K1 K2 106.62(5) 6_575 6_565 ? O2 K1 K2 78.68(5) 4_545 . ? O400 K1 K2 57.57(7) . . ? O32 K1 K2 117.47(5) 6_565 . ? O46 K1 K2 88.85(5) 6_565 . ? O100 K1 K2 37.89(6) 4 . ? O12 K1 K2 152.37(5) 6_565 . ? O4 K1 K2 113.50(5) 6_575 . ? K2 K1 K2 137.07(2) 6_565 . ? O32 K2 O6 140.10(7) . . ? O32 K2 O12 74.50(6) . . ? O6 K2 O12 83.85(6) . . ? O32 K2 O44 86.16(7) . 1_565 ? O6 K2 O44 102.20(7) . 1_565 ? O12 K2 O44 155.10(8) . 1_565 ? O32 K2 O100 140.49(8) . 4 ? O6 K2 O100 72.65(7) . 4 ? O12 K2 O100 93.52(7) . 4 ? O44 K2 O100 111.36(8) 1_565 4 ? O32 K2 O22 79.14(7) . . ? O6 K2 O22 140.75(7) . . ? O12 K2 O22 116.51(7) . . ? O44 K2 O22 73.77(7) 1_565 . ? O100 K2 O22 72.90(7) 4 . ? O32 K2 O200 73.79(7) . 7_566 ? O6 K2 O200 70.68(7) . 7_566 ? O12 K2 O200 83.38(8) . 7_566 ? O44 K2 O200 76.14(8) 1_565 7_566 ? O100 K2 O200 143.33(7) 4 7_566 ? O22 K2 O200 140.46(7) . 7_566 ? O32 K2 C32 17.11(6) . . ? O6 K2 C32 150.58(7) . . ? O12 K2 C32 90.94(6) . . ? O44 K2 C32 71.84(7) 1_565 . ? O100 K2 C32 136.70(7) 4 . ? O22 K2 C32 66.69(7) . . ? O200 K2 C32 79.97(7) 7_566 . ? O32 K2 K1 36.54(5) . 6_566 ? O6 K2 K1 109.64(5) . 6_566 ? O12 K2 K1 40.20(5) . 6_566 ? O44 K2 K1 116.49(5) 1_565 6_566 ? O100 K2 K1 129.87(6) 4 6_566 ? O22 K2 K1 106.66(5) . 6_566 ? O200 K2 K1 65.54(6) 7_566 6_566 ? C32 K2 K1 53.65(5) . 6_566 ? O32 K2 K1 103.88(6) . . ? O6 K2 K1 100.87(5) . . ? O12 K2 K1 72.51(5) . . ? O44 K2 K1 128.53(6) 1_565 . ? O100 K2 K1 37.39(5) 4 . ? O22 K2 K1 59.52(5) . . ? O200 K2 K1 155.31(6) 7_566 . ? C32 K2 K1 105.11(5) . . ? K1 K2 K1 97.55(2) 6_566 . ? O52 K3 O52 83.77(10) 2 . ? O52 K3 O26 83.31(6) 2 2 ? O52 K3 O26 167.07(7) . 2 ? O52 K3 O26 167.07(7) 2 . ? O52 K3 O26 83.31(6) . . ? O26 K3 O26 109.61(9) 2 . ? O52 K3 O500 90.71(8) 2 2 ? O52 K3 O500 92.44(8) . 2 ? O26 K3 O500 88.36(7) 2 2 ? O26 K3 O500 89.20(7) . 2 ? O52 K3 O500 92.44(8) 2 . ? O52 K3 O500 90.71(8) . . ? O26 K3 O500 89.20(7) 2 . ? O26 K3 O500 88.36(7) . . ? O500 K3 O500 175.77(12) 2 . ? O52 K3 K4 44.00(5) 2 2_545 ? O52 K3 K4 45.12(6) . 2_545 ? O26 K3 K4 123.12(5) 2 2_545 ? O26 K3 K4 123.83(5) . 2_545 ? O500 K3 K4 75.25(6) 2 2_545 ? O500 K3 K4 108.99(6) . 2_545 ? O52 K3 K4 45.12(6) 2 1_545 ? O52 K3 K4 44.00(6) . 1_545 ? O26 K3 K4 123.83(5) 2 1_545 ? O26 K3 K4 123.12(5) . 1_545 ? O500 K3 K4 108.99(6) 2 1_545 ? O500 K3 K4 75.25(6) . 1_545 ? K4 K3 K4 33.74(4) 2_545 1_545 ? K4 K4 O24 67.95(8) 2 . ? K4 K4 O52 66.85(7) 2 1_565 ? O24 K4 O52 73.86(7) . 1_565 ? K4 K4 O600 122.15(8) 2 . ? O24 K4 O600 76.39(9) . . ? O52 K4 O600 141.57(8) 1_565 . ? K4 K4 O42 131.89(9) 2 1_565 ? O24 K4 O42 76.00(8) . 1_565 ? O52 K4 O42 73.38(8) 1_565 1_565 ? O600 K4 O42 76.26(9) . 1_565 ? K4 K4 O600 136.45(8) 2 5_576 ? O24 K4 O600 149.30(9) . 5_576 ? O52 K4 O600 97.43(9) 1_565 5_576 ? O600 K4 O600 95.84(10) . 5_576 ? O42 K4 O600 73.30(8) 1_565 5_576 ? K4 K4 O52 64.64(7) 2 2_565 ? O24 K4 O52 129.76(10) . 2_565 ? O52 K4 O52 73.21(9) 1_565 2_565 ? O600 K4 O52 145.18(8) . 2_565 ? O42 K4 O52 127.30(8) 1_565 2_565 ? O600 K4 O52 72.00(9) 5_576 2_565 ? K4 K4 O24 63.24(7) 2 2 ? O24 K4 O24 101.13(9) . 2 ? O52 K4 O24 127.42(9) 1_565 2 ? O600 K4 O24 81.79(9) . 2 ? O42 K4 O24 157.94(9) 1_565 2 ? O600 K4 O24 107.16(8) 5_576 2 ? O52 K4 O24 71.56(7) 2_565 2 ? K4 K4 K4 159.78(8) 2 5_576 ? O24 K4 K4 117.98(8) . 5_576 ? O52 K4 K4 132.77(8) 1_565 5_576 ? O600 K4 K4 48.17(8) . 5_576 ? O42 K4 K4 66.94(6) 1_565 5_576 ? O600 K4 K4 47.68(7) 5_576 5_576 ? O52 K4 K4 112.25(7) 2_565 5_576 ? O24 K4 K4 96.59(7) 2 5_576 ? K4 K4 K3 73.13(2) 2 1_565 ? O24 K4 K3 111.19(6) . 1_565 ? O52 K4 K3 38.75(5) 1_565 1_565 ? O600 K4 K3 164.64(9) . 1_565 ? O42 K4 K3 92.32(5) 1_565 1_565 ? O600 K4 K3 70.72(7) 5_576 1_565 ? O52 K4 K3 38.87(4) 2_565 1_565 ? O24 K4 K3 108.82(6) 2 1_565 ? K4 K4 K3 118.00(5) 5_576 1_565 ? K1 O100 K2 104.72(9) 4_545 4_545 ? K4 O600 K4 84.16(10) . 5_576 ? _diffrn_measured_fraction_theta_max 0.867 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.791 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.098 _database_code_depnum_ccdc_archive 'CCDC 941397'