data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'YunLong Feng' _publ_contact_author_email SKY37@ZJNU.CN _publ_section_title ; A chiral manganese-potassium heterometallic MOF with unusual (3,7) topology network ; loop_ _publ_author_name 'YunLong Feng.' 'Yao-Kang Lv.' 'Cai-Hong Zhan.' # Attachment '1.CIF' data_a _database_code_depnum_ccdc_archive 'CCDC 731529' #TrackingRef '1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H16 I3 K Mn O15' _chemical_formula_sum 'C12 H16 I3 K Mn O15' _chemical_formula_weight 874.99 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 _symmetry_space_group_name_Hall 'P1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 5.8478(3) _cell_length_b 9.1080(5) _cell_length_c 11.0349(6) _cell_angle_alpha 91.713(3) _cell_angle_beta 93.054(3) _cell_angle_gamma 97.672(3) _cell_volume 581.24(5) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3340 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 27.19 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.257 _exptl_crystal_size_mid 0.044 _exptl_crystal_size_min 0.024 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 411 _exptl_absorpt_coefficient_mu 4.799 _exptl_absorpt_correction_T_min 0.785 _exptl_absorpt_correction_T_max 0.850 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 7126 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.1396 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.19 _reflns_number_total 2511 _reflns_number_gt 1823 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEXII (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2002)' _computing_publication_material 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^)+(0.0002P)^2^+3.0000P] 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 mixed _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 0.0(6) _chemical_absolute_configuration rm _refine_ls_number_reflns 2511 _refine_ls_number_parameters 314 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1510 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0684 _refine_ls_wR_factor_gt 0.0419 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.017 _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 I1 I 0.69198(14) 0.71659(13) 0.69359(11) 0.0442(2) Uani 1 1 d . . . I2 I 1.03422(13) 0.64473(12) 0.86403(9) 0.0647(4) Uani 1 1 d . . . I3 I 0.32136(11) 0.77981(10) 0.51116(9) 0.0509(3) Uani 1 1 d . . . K1 K 0.8221(4) 1.0458(3) 0.4252(3) 0.0375(7) Uani 1 1 d . . . Mn1 Mn 0.4432(2) 0.14529(18) 0.15502(14) 0.0191(4) Uani 1 1 d D . . O1 O 0.2983(11) 0.8924(9) 0.1303(8) 0.033(2) Uani 1 1 d . . . O2 O 0.3906(10) 0.6669(8) 0.1404(8) 0.0247(18) Uani 1 1 d . . . O3 O 0.7504(10) 0.9949(9) 0.1631(7) 0.0226(17) Uani 1 1 d D . . H3 H 0.834(15) 1.063(4) 0.135(6) 0.027 Uiso 1 1 d D . . O4 O 0.8269(12) 0.7684(9) 0.3053(8) 0.0310(19) Uani 1 1 d D . . H4 H 0.884(19) 0.703(10) 0.342(10) 0.037 Uiso 1 1 d D . . O5 O 0.3718(10) 0.3769(8) 0.2094(8) 0.0258(18) Uani 1 1 d D . . H5 H 0.248(10) 0.407(12) 0.219(10) 0.031 Uiso 1 1 d D . . O6 O 0.9637(11) 0.4803(9) 0.3053(9) 0.035(2) Uani 1 1 d . . . O7 O 0.7565(10) 0.2668(9) 0.2393(7) 0.0261(18) Uani 1 1 d . . . O8 O 0.6194(13) 0.2840(11) -0.4718(8) 0.042(2) Uani 1 1 d . . . O9 O 0.5293(10) 0.2638(9) -0.2782(7) 0.030(2) Uani 1 1 d . . . O10 O 0.1528(13) 0.3040(10) -0.5282(7) 0.031(2) Uani 1 1 d D . . H10 H 0.10(2) 0.374(9) -0.561(11) 0.037 Uiso 1 1 d D . . O11 O 0.0416(11) 0.1145(10) -0.3520(7) 0.0289(19) Uani 1 1 d D . . H11 H -0.025(17) 0.063(12) -0.302(9) 0.035 Uiso 1 1 d D . . O12 O 0.5049(10) 0.1661(9) -0.0372(7) 0.0285(19) Uani 1 1 d D . . H12 H 0.623(12) 0.156(13) -0.072(10) 0.034 Uiso 1 1 d D . . O13 O 0.1080(10) 0.1392(8) 0.0588(7) 0.0231(18) Uani 1 1 d . . . O14 O -0.0969(10) 0.0974(9) -0.1176(7) 0.0299(19) Uani 1 1 d . . . O1W O 0.3133(13) 0.0908(11) 0.3324(8) 0.039(2) Uani 1 1 d D . . H1WA H 0.435(11) 0.145(10) 0.362(4) 0.047 Uiso 1 1 d D . . H1WB H 0.296(17) 0.009(7) 0.368(10) 0.047 Uiso 1 1 d D . . C1 C 0.4418(14) 0.8100(12) 0.1263(10) 0.021(2) Uani 1 1 d . . . C2 C 0.6966(15) 0.8504(12) 0.1151(10) 0.022(2) Uani 1 1 d D . . H2A H 0.7313 0.8456 0.0311 0.027 Uiso 1 1 d R . . C3 C 0.7991(14) 0.7301(12) 0.1816(10) 0.023(2) Uani 1 1 d . . . H3A H 0.9450 0.7113 0.1483 0.027 Uiso 1 1 d R . . C4 C 0.6062(14) 0.5989(12) 0.1521(10) 0.020(2) Uani 1 1 d . . . H4A H 0.6337 0.5510 0.0765 0.024 Uiso 1 1 d R . . C5 C 0.5649(14) 0.4832(13) 0.2481(11) 0.023(3) Uani 1 1 d . . . H5A H 0.5339 0.5317 0.3249 0.028 Uiso 1 1 d R . . C6 C 0.7783(15) 0.4011(14) 0.2657(10) 0.025(3) Uani 1 1 d . . . C7 C 0.4862(16) 0.2979(13) -0.3932(11) 0.025(3) Uani 1 1 d . . . C8 C 0.2483(15) 0.3422(14) -0.4083(9) 0.025(3) Uani 1 1 d . . . H8A H 0.2576 0.4495 -0.3933 0.030 Uiso 1 1 d R . . C9 C 0.1216(14) 0.2611(13) -0.3077(9) 0.022(2) Uani 1 1 d . . . H9A H -0.0049 0.3124 -0.2808 0.026 Uiso 1 1 d R . . C10 C 0.3119(14) 0.1415(13) -0.1245(9) 0.020(2) Uani 1 1 d . . . H10A H 0.3172 0.0518 -0.1715 0.024 Uiso 1 1 d R . . C11 C 0.3211(14) 0.2692(14) -0.2096(9) 0.024(3) Uani 1 1 d . . . H11A H 0.3356 0.3604 -0.1622 0.029 Uiso 1 1 d R . . C12 C 0.0893(15) 0.1250(13) -0.0551(11) 0.024(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 I1 0.0339(3) 0.0472(6) 0.0499(5) -0.0033(4) 0.0010(3) 0.0012(3) I2 0.0541(6) 0.0962(11) 0.0471(7) -0.0193(7) -0.0087(4) 0.0321(6) I3 0.0402(5) 0.0518(8) 0.0604(7) 0.0207(6) -0.0011(4) 0.0031(4) K1 0.0361(12) 0.043(2) 0.0318(16) -0.0060(14) -0.0049(9) 0.0034(10) Mn1 0.0164(6) 0.0204(10) 0.0200(8) 0.0031(7) -0.0012(5) 0.0012(5) O1 0.022(3) 0.023(5) 0.054(6) 0.005(4) -0.002(3) 0.004(3) O2 0.024(3) 0.005(5) 0.045(5) -0.002(4) -0.004(3) 0.002(3) O3 0.022(3) 0.016(5) 0.029(4) 0.002(4) 0.008(3) -0.002(3) O4 0.038(4) 0.017(5) 0.035(5) 0.001(4) -0.016(3) 0.000(3) O5 0.015(3) 0.016(5) 0.046(5) -0.001(4) 0.005(3) 0.001(3) O6 0.030(4) 0.018(5) 0.054(6) -0.001(4) -0.018(3) 0.000(3) O7 0.020(3) 0.018(5) 0.038(5) -0.001(4) -0.005(3) 0.000(3) O8 0.034(4) 0.074(8) 0.022(5) 0.010(5) 0.009(3) 0.018(4) O9 0.016(3) 0.050(6) 0.024(4) 0.010(4) 0.003(3) 0.007(3) O10 0.034(4) 0.040(6) 0.020(5) 0.007(4) -0.001(3) 0.014(4) O11 0.031(4) 0.031(6) 0.022(5) 0.002(4) -0.004(3) -0.003(3) O12 0.015(3) 0.052(6) 0.019(4) 0.005(4) 0.002(2) 0.006(3) O13 0.016(3) 0.030(5) 0.024(4) 0.007(4) 0.003(2) 0.003(3) O14 0.017(3) 0.051(6) 0.021(4) 0.002(4) -0.002(3) 0.001(3) O1W 0.051(5) 0.034(6) 0.033(5) 0.005(5) 0.013(4) 0.002(4) C1 0.018(4) 0.017(7) 0.027(6) -0.001(5) -0.006(3) -0.001(4) C2 0.026(5) 0.015(7) 0.024(6) -0.007(5) 0.008(4) -0.004(4) C3 0.015(4) 0.019(7) 0.033(6) 0.003(5) 0.000(3) 0.001(3) C4 0.018(4) 0.013(7) 0.030(6) -0.001(5) 0.000(4) 0.003(4) C5 0.018(4) 0.018(7) 0.034(7) 0.010(6) 0.004(4) 0.002(4) C6 0.021(4) 0.027(8) 0.027(6) 0.012(6) -0.003(4) 0.005(4) C7 0.024(5) 0.025(8) 0.025(6) 0.000(6) 0.005(4) 0.000(4) C8 0.028(5) 0.037(8) 0.011(5) -0.001(5) -0.004(4) 0.005(4) C9 0.014(4) 0.035(7) 0.015(5) 0.003(5) -0.002(3) 0.005(3) C10 0.016(4) 0.031(7) 0.014(5) 0.003(5) 0.003(3) 0.006(4) C11 0.016(4) 0.040(8) 0.017(6) -0.002(5) 0.004(3) 0.003(4) C12 0.018(4) 0.023(7) 0.033(7) 0.015(6) 0.006(4) 0.007(4) _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 I1 I2 2.8273(13) . ? I1 I3 3.0031(13) . ? I3 K1 3.726(3) . ? K1 O11 2.729(8) 1_666 ? K1 O4 2.821(9) . ? K1 O8 2.844(9) 1_566 ? K1 O10 2.853(10) 1_666 ? K1 O3 2.914(8) . ? K1 O7 2.962(8) 1_565 ? K1 O1W 3.081(8) 1_665 ? K1 O1W 3.177(8) 1_565 ? Mn1 O7 2.159(7) . ? Mn1 O13 2.172(6) . ? Mn1 O12 2.180(8) . ? Mn1 O1W 2.184(9) . ? Mn1 O5 2.274(8) . ? Mn1 O1 2.349(8) 1_545 ? Mn1 O3 2.400(7) 1_545 ? O1 C1 1.199(12) . ? O1 Mn1 2.349(8) 1_565 ? O2 C1 1.314(13) . ? O2 C4 1.478(10) . ? O3 C2 1.394(13) . ? O3 Mn1 2.400(7) 1_565 ? O3 H3 0.82(6) . ? O4 C3 1.395(14) . ? O4 H4 0.83(11) . ? O5 C5 1.423(12) . ? O5 H5 0.82(7) . ? O6 C6 1.269(13) . ? O7 C6 1.237(13) . ? O7 K1 2.962(8) 1_545 ? O8 C7 1.211(13) . ? O8 K1 2.844(9) 1_544 ? O9 C7 1.334(13) . ? O9 C11 1.473(11) . ? O10 C8 1.423(12) . ? O10 K1 2.853(10) 1_444 ? O10 H10 0.83(9) . ? O11 C9 1.418(13) . ? O11 K1 2.729(8) 1_444 ? O11 H11 0.82(10) . ? O12 C10 1.434(11) . ? O12 H12 0.82(8) . ? O13 C12 1.257(13) . ? O14 C12 1.249(11) . ? O1W K1 3.081(8) 1_445 ? O1W K1 3.177(8) 1_545 ? O1W H1WA 0.85(8) . ? O1W H1WB 0.85(8) . ? C1 C2 1.499(12) . ? C2 C3 1.509(14) . ? C2 H2A 0.9597 . ? C3 C4 1.544(14) . ? C3 H3A 0.9799 . ? C4 C5 1.522(14) . ? C4 H4A 0.9601 . ? C5 C6 1.545(12) . ? C5 H5A 0.9806 . ? C7 C8 1.502(13) . ? C8 C9 1.523(13) . ? C8 H8A 0.9800 . ? C9 C11 1.541(12) . ? C9 H9A 0.9800 . ? C10 C11 1.515(15) . ? C10 C12 1.537(12) . ? C10 H10A 0.9598 . ? C11 H11A 0.9601 . ? 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 I2 I1 I3 177.69(6) . . ? I1 I3 K1 78.67(5) . . ? O11 K1 O4 121.9(3) 1_666 . ? O11 K1 O8 73.1(2) 1_666 1_566 ? O4 K1 O8 156.2(2) . 1_566 ? O11 K1 O10 57.5(2) 1_666 1_666 ? O4 K1 O10 134.7(2) . 1_666 ? O8 K1 O10 68.2(2) 1_566 1_666 ? O11 K1 O3 160.3(2) 1_666 . ? O4 K1 O3 56.1(2) . . ? O8 K1 O3 116.5(2) 1_566 . ? O10 K1 O3 108.4(2) 1_666 . ? O11 K1 O7 123.9(3) 1_666 1_565 ? O4 K1 O7 108.3(2) . 1_565 ? O8 K1 O7 70.0(2) 1_566 1_565 ? O10 K1 O7 70.1(2) 1_666 1_565 ? O3 K1 O7 52.2(2) . 1_565 ? O11 K1 O1W 84.6(2) 1_666 1_665 ? O4 K1 O1W 80.0(3) . 1_665 ? O8 K1 O1W 121.9(3) 1_566 1_665 ? O10 K1 O1W 54.7(3) 1_666 1_665 ? O3 K1 O1W 75.8(2) . 1_665 ? O7 K1 O1W 80.9(2) 1_565 1_665 ? O11 K1 O1W 129.0(3) 1_666 1_565 ? O4 K1 O1W 96.7(2) . 1_565 ? O8 K1 O1W 61.2(3) 1_566 1_565 ? O10 K1 O1W 117.9(3) 1_666 1_565 ? O3 K1 O1W 68.5(2) . 1_565 ? O7 K1 O1W 60.5(2) 1_565 1_565 ? O1W K1 O1W 138.3(3) 1_665 1_565 ? O11 K1 I3 100.20(18) 1_666 . ? O4 K1 I3 70.12(18) . . ? O8 K1 I3 89.91(19) 1_566 . ? O10 K1 I3 151.83(19) 1_666 . ? O3 K1 I3 97.07(15) . . ? O7 K1 I3 120.14(14) 1_565 . ? O1W K1 I3 147.5(2) 1_665 . ? O1W K1 I3 60.38(17) 1_565 . ? O7 Mn1 O13 150.9(3) . . ? O7 Mn1 O12 101.6(3) . . ? O13 Mn1 O12 73.0(2) . . ? O7 Mn1 O1W 91.1(3) . . ? O13 Mn1 O1W 96.6(3) . . ? O12 Mn1 O1W 167.2(3) . . ? O7 Mn1 O5 71.5(3) . . ? O13 Mn1 O5 81.6(3) . . ? O12 Mn1 O5 102.2(3) . . ? O1W Mn1 O5 83.2(3) . . ? O7 Mn1 O1 134.0(3) . 1_545 ? O13 Mn1 O1 75.0(3) . 1_545 ? O12 Mn1 O1 93.0(3) . 1_545 ? O1W Mn1 O1 76.8(3) . 1_545 ? O5 Mn1 O1 147.0(2) . 1_545 ? O7 Mn1 O3 68.9(3) . 1_545 ? O13 Mn1 O3 137.1(3) . 1_545 ? O12 Mn1 O3 86.3(3) . 1_545 ? O1W Mn1 O3 96.9(3) . 1_545 ? O5 Mn1 O3 140.4(2) . 1_545 ? O1 Mn1 O3 68.9(2) 1_545 1_545 ? C1 O1 Mn1 115.3(6) . 1_565 ? C1 O2 C4 109.4(7) . . ? C2 O3 Mn1 116.3(5) . 1_565 ? C2 O3 K1 119.5(6) . . ? Mn1 O3 K1 91.5(2) 1_565 . ? C2 O3 H3 127(4) . . ? Mn1 O3 H3 89(7) 1_565 . ? K1 O3 H3 104(5) . . ? C3 O4 K1 129.5(6) . . ? C3 O4 H4 109(9) . . ? K1 O4 H4 119(9) . . ? C5 O5 Mn1 117.5(6) . . ? C5 O5 H5 113(8) . . ? Mn1 O5 H5 129(8) . . ? C6 O7 Mn1 123.2(6) . . ? C6 O7 K1 121.6(7) . 1_545 ? Mn1 O7 K1 95.3(3) . 1_545 ? C7 O8 K1 135.8(8) . 1_544 ? C7 O9 C11 109.7(7) . . ? C8 O10 K1 120.6(7) . 1_444 ? C8 O10 H10 112(10) . . ? K1 O10 H10 108(9) 1_444 . ? C9 O11 K1 124.1(6) . 1_444 ? C9 O11 H11 113(9) . . ? K1 O11 H11 109(9) 1_444 . ? C10 O12 Mn1 119.0(5) . . ? C10 O12 H12 109(8) . . ? Mn1 O12 H12 128(8) . . ? C12 O13 Mn1 120.3(6) . . ? Mn1 O1W K1 132.4(3) . 1_445 ? Mn1 O1W K1 89.0(3) . 1_545 ? K1 O1W K1 138.3(3) 1_445 1_545 ? Mn1 O1W H1WA 86(4) . . ? K1 O1W H1WA 130(6) 1_445 . ? K1 O1W H1WA 43(8) 1_545 . ? Mn1 O1W H1WB 131(9) . . ? K1 O1W H1WB 72(8) 1_445 . ? K1 O1W H1WB 76(6) 1_545 . ? H1WA O1W H1WB 110(4) . . ? O1 C1 O2 121.8(8) . . ? O1 C1 C2 127.5(10) . . ? O2 C1 C2 110.5(8) . . ? O3 C2 C1 105.8(8) . . ? O3 C2 C3 117.3(9) . . ? C1 C2 C3 103.3(8) . . ? O3 C2 H2A 110.6 . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2A 109.6 . . ? O4 C3 C2 109.4(9) . . ? O4 C3 C4 112.7(8) . . ? C2 C3 C4 99.8(7) . . ? O4 C3 H3A 111.7 . . ? C2 C3 H3A 111.3 . . ? C4 C3 H3A 111.4 . . ? O2 C4 C5 105.3(7) . . ? O2 C4 C3 104.9(8) . . ? C5 C4 C3 117.3(9) . . ? O2 C4 H4A 110.3 . . ? C5 C4 H4A 109.4 . . ? C3 C4 H4A 109.3 . . ? O5 C5 C4 109.6(8) . . ? O5 C5 C6 108.1(9) . . ? C4 C5 C6 110.0(8) . . ? O5 C5 H5A 109.4 . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5A 110.1 . . ? O7 C6 O6 125.7(9) . . ? O7 C6 C5 118.5(9) . . ? O6 C6 C5 115.8(11) . . ? O8 C7 O9 122.7(9) . . ? O8 C7 C8 127.3(10) . . ? O9 C7 C8 109.8(8) . . ? O10 C8 C7 110.1(9) . . ? O10 C8 C9 115.2(9) . . ? C7 C8 C9 102.8(8) . . ? O10 C8 H8A 109.5 . . ? C7 C8 H8A 109.3 . . ? C9 C8 H8A 109.6 . . ? O11 C9 C8 107.6(9) . . ? O11 C9 C11 113.2(8) . . ? C8 C9 C11 99.8(7) . . ? O11 C9 H9A 111.9 . . ? C8 C9 H9A 111.7 . . ? C11 C9 H9A 111.9 . . ? O12 C10 C11 109.8(8) . . ? O12 C10 C12 108.1(8) . . ? C11 C10 C12 111.7(8) . . ? O12 C10 H10A 109.9 . . ? C11 C10 H10A 108.5 . . ? C12 C10 H10A 108.9 . . ? O9 C11 C10 106.1(8) . . ? O9 C11 C9 104.7(8) . . ? C10 C11 C9 116.2(9) . . ? O9 C11 H11A 109.8 . . ? C10 C11 H11A 108.8 . . ? C9 C11 H11A 111.1 . . ? O14 C12 O13 125.2(9) . . ? O14 C12 C10 116.6(10) . . ? O13 C12 C10 118.1(8) . . ? 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 I2 I1 I3 K1 -139.4(12) . . . . ? I1 I3 K1 O11 -33.57(19) . . . 1_666 ? I1 I3 K1 O4 86.83(16) . . . . ? I1 I3 K1 O8 -106.38(17) . . . 1_566 ? I1 I3 K1 O10 -68.4(3) . . . 1_666 ? I1 I3 K1 O3 136.88(16) . . . . ? I1 I3 K1 O7 -173.0(2) . . . 1_565 ? I1 I3 K1 O1W 62.3(3) . . . 1_665 ? I1 I3 K1 O1W -162.8(2) . . . 1_565 ? I1 I3 K1 Mn1 174.75(7) . . . 1_565 ? O11 K1 O3 C2 107.3(9) 1_666 . . . ? O4 K1 O3 C2 16.5(5) . . . . ? O8 K1 O3 C2 -137.2(6) 1_566 . . . ? O10 K1 O3 C2 148.5(6) 1_666 . . . ? O7 K1 O3 C2 -166.8(6) 1_565 . . . ? O1W K1 O3 C2 103.9(6) 1_665 . . . ? O1W K1 O3 C2 -98.0(6) 1_565 . . . ? I3 K1 O3 C2 -43.8(6) . . . . ? Mn1 K1 O3 C2 -121.6(6) 1_565 . . . ? O11 K1 O3 Mn1 -131.1(7) 1_666 . . 1_565 ? O4 K1 O3 Mn1 138.1(3) . . . 1_565 ? O8 K1 O3 Mn1 -15.6(3) 1_566 . . 1_565 ? O10 K1 O3 Mn1 -89.9(2) 1_666 . . 1_565 ? O7 K1 O3 Mn1 -45.1(2) 1_565 . . 1_565 ? O1W K1 O3 Mn1 -134.5(3) 1_665 . . 1_565 ? O1W K1 O3 Mn1 23.6(2) 1_565 . . 1_565 ? I3 K1 O3 Mn1 77.82(19) . . . 1_565 ? O11 K1 O4 C3 -155.4(6) 1_666 . . . ? O8 K1 O4 C3 80.3(10) 1_566 . . . ? O10 K1 O4 C3 -81.3(7) 1_666 . . . ? O3 K1 O4 C3 1.2(6) . . . . ? O7 K1 O4 C3 -1.5(7) 1_565 . . . ? O1W K1 O4 C3 -78.3(7) 1_665 . . . ? O1W K1 O4 C3 59.7(7) 1_565 . . . ? I3 K1 O4 C3 114.8(7) . . . . ? Mn1 K1 O4 C3 26.0(7) 1_565 . . . ? O7 Mn1 O5 C5 10.3(7) . . . . ? O13 Mn1 O5 C5 -158.5(7) . . . . ? O12 Mn1 O5 C5 -88.1(7) . . . . ? O1W Mn1 O5 C5 103.7(7) . . . . ? O1 Mn1 O5 C5 156.5(7) 1_545 . . . ? O3 Mn1 O5 C5 11.0(9) 1_545 . . . ? K1 Mn1 O5 C5 50.6(7) 1_545 . . . ? O13 Mn1 O7 C6 14.8(12) . . . . ? O12 Mn1 O7 C6 90.5(9) . . . . ? O1W Mn1 O7 C6 -91.1(9) . . . . ? O5 Mn1 O7 C6 -8.6(8) . . . . ? O1 Mn1 O7 C6 -163.6(8) 1_545 . . . ? O3 Mn1 O7 C6 172.0(9) 1_545 . . . ? K1 Mn1 O7 C6 -133.6(9) 1_545 . . . ? O13 Mn1 O7 K1 148.4(5) . . . 1_545 ? O12 Mn1 O7 K1 -135.9(3) . . . 1_545 ? O1W Mn1 O7 K1 42.5(3) . . . 1_545 ? O5 Mn1 O7 K1 125.0(3) . . . 1_545 ? O1 Mn1 O7 K1 -30.1(5) 1_545 . . 1_545 ? O3 Mn1 O7 K1 -54.5(2) 1_545 . . 1_545 ? O7 Mn1 O12 C10 -160.5(7) . . . . ? O13 Mn1 O12 C10 -10.0(7) . . . . ? O1W Mn1 O12 C10 26.7(18) . . . . ? O5 Mn1 O12 C10 -87.2(8) . . . . ? O1 Mn1 O12 C10 63.3(7) 1_545 . . . ? O3 Mn1 O12 C10 131.9(8) 1_545 . . . ? K1 Mn1 O12 C10 153.1(6) 1_545 . . . ? O7 Mn1 O13 C12 94.8(10) . . . . ? O12 Mn1 O13 C12 11.5(8) . . . . ? O1W Mn1 O13 C12 -160.8(8) . . . . ? O5 Mn1 O13 C12 117.1(9) . . . . ? O1 Mn1 O13 C12 -86.4(9) 1_545 . . . ? O3 Mn1 O13 C12 -53.1(9) 1_545 . . . ? K1 Mn1 O13 C12 -142.0(7) 1_545 . . . ? O7 Mn1 O1W K1 147.3(5) . . . 1_445 ? O13 Mn1 O1W K1 -4.7(6) . . . 1_445 ? O12 Mn1 O1W K1 -39.7(18) . . . 1_445 ? O5 Mn1 O1W K1 76.1(5) . . . 1_445 ? O1 Mn1 O1W K1 -77.5(5) 1_545 . . 1_445 ? O3 Mn1 O1W K1 -143.8(5) 1_545 . . 1_445 ? K1 Mn1 O1W K1 -173.8(7) 1_545 . . 1_445 ? O7 Mn1 O1W K1 -38.9(3) . . . 1_545 ? O13 Mn1 O1W K1 169.2(3) . . . 1_545 ? O12 Mn1 O1W K1 134.1(13) . . . 1_545 ? O5 Mn1 O1W K1 -110.1(3) . . . 1_545 ? O1 Mn1 O1W K1 96.3(3) 1_545 . . 1_545 ? O3 Mn1 O1W K1 30.0(3) 1_545 . . 1_545 ? Mn1 O1 C1 O2 164.4(8) 1_565 . . . ? Mn1 O1 C1 C2 -10.7(15) 1_565 . . . ? C4 O2 C1 O1 -170.3(10) . . . . ? C4 O2 C1 C2 5.5(12) . . . . ? Mn1 O3 C2 C1 -26.4(10) 1_565 . . . ? K1 O3 C2 C1 81.8(8) . . . . ? Mn1 O3 C2 C3 -141.0(6) 1_565 . . . ? K1 O3 C2 C3 -32.7(10) . . . . ? O1 C1 C2 O3 25.8(15) . . . . ? O2 C1 C2 O3 -149.7(9) . . . . ? O1 C1 C2 C3 149.6(12) . . . . ? O2 C1 C2 C3 -25.9(12) . . . . ? K1 O4 C3 C2 -16.0(10) . . . . ? K1 O4 C3 C4 -126.0(8) . . . . ? O3 C2 C3 O4 30.6(11) . . . . ? C1 C2 C3 O4 -85.3(9) . . . . ? O3 C2 C3 C4 149.0(9) . . . . ? C1 C2 C3 C4 33.1(10) . . . . ? C1 O2 C4 C5 141.1(9) . . . . ? C1 O2 C4 C3 16.7(11) . . . . ? O4 C3 C4 O2 85.2(9) . . . . ? C2 C3 C4 O2 -30.8(10) . . . . ? O4 C3 C4 C5 -31.3(12) . . . . ? C2 C3 C4 C5 -147.2(9) . . . . ? Mn1 O5 C5 C4 109.3(8) . . . . ? Mn1 O5 C5 C6 -10.6(10) . . . . ? O2 C4 C5 O5 59.7(11) . . . . ? C3 C4 C5 O5 175.9(9) . . . . ? O2 C4 C5 C6 178.4(9) . . . . ? C3 C4 C5 C6 -65.3(13) . . . . ? Mn1 O7 C6 O6 -173.4(9) . . . . ? K1 O7 C6 O6 64.5(14) 1_545 . . . ? Mn1 O7 C6 C5 5.6(13) . . . . ? K1 O7 C6 C5 -116.5(8) 1_545 . . . ? O5 C5 C6 O7 3.8(14) . . . . ? C4 C5 C6 O7 -115.9(11) . . . . ? O5 C5 C6 O6 -177.1(10) . . . . ? C4 C5 C6 O6 63.2(13) . . . . ? K1 O8 C7 O9 59.5(16) 1_544 . . . ? K1 O8 C7 C8 -115.4(12) 1_544 . . . ? C11 O9 C7 O8 -170.8(11) . . . . ? C11 O9 C7 C8 4.9(13) . . . . ? K1 O10 C8 C7 101.4(8) 1_444 . . . ? K1 O10 C8 C9 -14.4(12) 1_444 . . . ? O8 C7 C8 O10 26.0(17) . . . . ? O9 C7 C8 O10 -149.5(9) . . . . ? O8 C7 C8 C9 149.3(12) . . . . ? O9 C7 C8 C9 -26.2(12) . . . . ? K1 O11 C9 C8 -46.3(8) 1_444 . . . ? K1 O11 C9 C11 -155.6(6) 1_444 . . . ? O10 C8 C9 O11 36.0(11) . . . . ? C7 C8 C9 O11 -83.8(9) . . . . ? O10 C8 C9 C11 154.3(9) . . . . ? C7 C8 C9 C11 34.5(11) . . . . ? Mn1 O12 C10 C11 129.8(7) . . . . ? Mn1 O12 C10 C12 7.8(11) . . . . ? C7 O9 C11 C10 141.6(9) . . . . ? C7 O9 C11 C9 18.2(12) . . . . ? O12 C10 C11 O9 65.5(10) . . . . ? C12 C10 C11 O9 -174.7(9) . . . . ? O12 C10 C11 C9 -178.7(8) . . . . ? C12 C10 C11 C9 -58.9(13) . . . . ? O11 C9 C11 O9 81.7(10) . . . . ? C8 C9 C11 O9 -32.5(11) . . . . ? O11 C9 C11 C10 -34.9(12) . . . . ? C8 C9 C11 C10 -149.0(9) . . . . ? Mn1 O13 C12 O14 168.3(9) . . . . ? Mn1 O13 C12 C10 -11.2(14) . . . . ? O12 C10 C12 O14 -177.5(9) . . . . ? C11 C10 C12 O14 61.7(14) . . . . ? O12 C10 C12 O13 2.1(14) . . . . ? C11 C10 C12 O13 -118.7(11) . . . . ? 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 O3 H3 O13 0.82(6) 1.91(5) 2.653(9) 152(8) 1_665 O4 H4 O6 0.83(11) 2.17(9) 2.843(12) 139(12) . O5 H5 O6 0.82(7) 2.13(4) 2.917(10) 161(11) 1_455 O10 H10 O6 0.83(9) 1.99(6) 2.759(11) 156(13) 1_454 O11 H11 O14 0.82(10) 2.12(10) 2.754(11) 134(12) . O12 H12 O14 0.82(8) 1.88(4) 2.679(9) 164(12) 1_655 O1W H1WA O8 0.85(8) 2.33(4) 3.081(13) 147(6) 1_556 O1W H1WA O7 0.85(8) 2.53(5) 3.101(11) 125(4) . O1W H1WB I3 0.85(8) 2.67(8) 3.504(9) 167(8) 1_545 C3 H3A O1 0.98 2.49 3.178(11) 127.4 1_655 _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.19 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 2.331 _refine_diff_density_min -4.043 _refine_diff_density_rms 0.479